#------------------------------------------------------------------------------
#$Date: 2024-10-06 07:02:01 +0200 (Sun 06 de Oct de 2024) $
#$Revision: 295095 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/34/7133462.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7133462
loop_
_publ_author_name
'Maestri, Claudio'
'Minazzi, Paolo'
'Grell, Toni'
'Colombo, Valentina'
'Lattuada, Luciano'
'Giovenzana, Giovanni B.'
'Travagin, Fabio'
_publ_section_title
;
 A serendipitous one-pot synthesis of the
 octahydro-2H-pyrazino[1,2-a]pyrazine core.
;
_journal_issue                   70
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9428
_journal_page_last               9431
_journal_paper_doi               10.1039/d4cc03596h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C22 H29 N3 O'
_chemical_formula_sum            'C22 H29 N3 O'
_chemical_formula_weight         351.48
_chemical_melting_point          ?
_chemical_name_common            n/a
_chemical_name_systematic        n/a
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-01-24 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.011(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2333(3)
_cell_length_b                   10.3310(2)
_cell_length_c                   18.6080(4)
_cell_measurement_reflns_used    16981
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.5860
_cell_measurement_theta_min      1.9870
_cell_volume                     1966.94(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0098
_diffrn_reflns_av_unetI/netI     0.0078
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21745
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.466
_diffrn_reflns_theta_min         2.189
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.290
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         6066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0654P)²+0.4127P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5524
_reflns_number_total             6066
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc03596h2.cif
_cod_data_source_block           116PAAZTA
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'Not measured' was changed
to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7133462.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7133462
_shelx_shelxl_version_number     2019/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_res_file
;
TITL 116PAAZTA
    shelx.res
    created by SHELXL-2019/3 at 15:52:38 on 24-Jan-2024
CELL  0.71073  10.2333  10.3310  18.6080   90.000   91.011   90.000
ZERR     4.00   0.0003   0.0002   0.0004    0.000    0.002    0.000
LATT   1
SYMM  1/2 - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    N    O
UNIT  88 116 12 4
MERG   2
OMIT     0   2   0
EQIV $1 -x+1, -y+1, -z+1
HTAB O1 N3_$1
FMAP   2
PLAN   20
ACTA
BOND   $H
CONF
LIST   4
L.S.  10
TEMP  -123.00
WGHT    0.065400    0.412700
FVAR       4.59149
C1    1    0.429437    0.436061    0.413925    11.00000    0.02091    0.01771 =
         0.01950   -0.00078   -0.00086   -0.00065
AFIX  23
H1A   2    0.388850    0.470365    0.369149    11.00000   -1.20000
H1B   2    0.390061    0.481119    0.455208    11.00000   -1.20000
AFIX   0
C2    1    0.404468    0.289256    0.419444    11.00000    0.01628    0.01744 =
         0.01698   -0.00131   -0.00074   -0.00067
C3    1    0.462337    0.220435    0.354225    11.00000    0.02147    0.02036 =
         0.01666   -0.00208   -0.00146    0.00202
AFIX  23
H3A   2    0.556547    0.241232    0.351423    11.00000   -1.20000
H3B   2    0.453827    0.125642    0.360380    11.00000   -1.20000
AFIX   0
C4    1    0.469643    0.232608    0.487066    11.00000    0.01908    0.01932 =
         0.01666   -0.00003    0.00080    0.00157
AFIX  23
H4A   2    0.468422    0.136997    0.483541    11.00000   -1.20000
H4B   2    0.562195    0.260483    0.489054    11.00000   -1.20000
AFIX   0
C5    1    0.257941    0.224144    0.290415    11.00000    0.02454    0.03588 =
         0.02223   -0.00514   -0.00588   -0.00386
AFIX  23
H5A   2    0.249585    0.129016    0.294813    11.00000   -1.20000
H5B   2    0.212698    0.251258    0.245422    11.00000   -1.20000
AFIX   0
C6    1    0.194257    0.289228    0.354296    11.00000    0.01865    0.03843 =
         0.02508   -0.00431   -0.00533    0.00010
AFIX  23
H6A   2    0.195104    0.384308    0.347683    11.00000   -1.20000
H6B   2    0.102134    0.260837    0.357430    11.00000   -1.20000
AFIX   0
C7    1    0.200173    0.294734    0.486455    11.00000    0.01731    0.03212 =
         0.02424   -0.00312    0.00170   -0.00036
AFIX  23
H7A   2    0.107385    0.267652    0.484350    11.00000   -1.20000
H7B   2    0.203058    0.390155    0.491117    11.00000   -1.20000
AFIX   0
C8    1    0.268038    0.232840    0.551178    11.00000    0.02055    0.02584 =
         0.02242   -0.00077    0.00353   -0.00466
AFIX  23
H8A   2    0.224368    0.260303    0.595715    11.00000   -1.20000
H8B   2    0.261574    0.137439    0.547571    11.00000   -1.20000
AFIX   0
C9    1    0.459507    0.197864    0.226023    11.00000    0.03293    0.02533 =
         0.01723   -0.00268   -0.00216    0.00587
AFIX  23
H9A   2    0.442717    0.103538    0.227529    11.00000   -1.20000
H9B   2    0.555142    0.211108    0.230303    11.00000   -1.20000
AFIX   0
C10   1    0.411642    0.250536    0.154552    11.00000    0.02675    0.02212 =
         0.01752   -0.00145   -0.00185    0.00011
C11   1    0.388958    0.168424    0.096369    11.00000    0.03574    0.02162 =
         0.01920   -0.00233    0.00038   -0.00194
AFIX  43
H11   2    0.401759    0.077882    0.101969    11.00000   -1.20000
AFIX   0
C12   1    0.347664    0.217464    0.029952    11.00000    0.03765    0.03078 =
         0.01799   -0.00341   -0.00151   -0.00242
AFIX  43
H12   2    0.332463    0.160375   -0.009336    11.00000   -1.20000
AFIX   0
C13   1    0.328832    0.348979    0.021219    11.00000    0.03823    0.03385 =
         0.02128    0.00336   -0.00387    0.00223
AFIX  43
H13   2    0.301919    0.382542   -0.024212    11.00000   -1.20000
AFIX   0
C14   1    0.349332    0.431939    0.078981    11.00000    0.06156    0.02374 =
         0.03095    0.00202   -0.00955    0.00581
AFIX  43
H14   2    0.335066    0.522260    0.073337    11.00000   -1.20000
AFIX   0
C15   1    0.390777    0.382800    0.145155    11.00000    0.05549    0.02230 =
         0.02604   -0.00442   -0.01071    0.00307
AFIX  43
H15   2    0.405035    0.440134    0.184431    11.00000   -1.20000
AFIX   0
C16   1    0.478585    0.205730    0.613917    11.00000    0.02663    0.02781 =
         0.01834    0.00362    0.00248    0.00666
AFIX  23
H16A  2    0.568891    0.240067    0.616003    11.00000   -1.20000
H16B  2    0.484131    0.112284    0.602583    11.00000   -1.20000
AFIX   0
C17   1    0.419320    0.220629    0.687320    11.00000    0.02315    0.02550 =
         0.01786    0.00311    0.00070    0.00355
C18   1    0.360631    0.114231    0.719687    11.00000    0.03484    0.02771 =
         0.02480    0.00305    0.00355   -0.00240
AFIX  43
H18   2    0.355601    0.034366    0.694484    11.00000   -1.20000
AFIX   0
C19   1    0.309192    0.123045    0.788419    11.00000    0.03460    0.04131 =
         0.02590    0.00810    0.00516   -0.00564
AFIX  43
H19   2    0.269279    0.049823    0.809761    11.00000   -1.20000
AFIX   0
C20   1    0.316692    0.239282    0.825353    11.00000    0.02205    0.05099 =
         0.01794    0.00225    0.00081    0.00460
AFIX  43
H20   2    0.282390    0.245773    0.872324    11.00000   -1.20000
AFIX   0
C21   1    0.374282    0.346285    0.793796    11.00000    0.03125    0.03639 =
         0.02172   -0.00378   -0.00228    0.00608
AFIX  43
H21   2    0.378720    0.426032    0.819142    11.00000   -1.20000
AFIX   0
C22   1    0.425628    0.337298    0.725105    11.00000    0.03100    0.02654 =
         0.02215    0.00195    0.00006    0.00105
AFIX  43
H22   2    0.465099    0.410883    0.703891    11.00000   -1.20000
AFIX   0
N1    3    0.396392    0.259421    0.287377    11.00000    0.02258    0.02427 =
         0.01627   -0.00312   -0.00269    0.00150
N2    3    0.264804    0.255497    0.420635    11.00000    0.01612    0.02630 =
         0.02013   -0.00307   -0.00136   -0.00236
N3    3    0.406425    0.271473    0.554451    11.00000    0.01839    0.01928 =
         0.01622    0.00028    0.00077   -0.00037
O1    4    0.567151    0.458298    0.413819    11.00000    0.02273    0.02060 =
         0.02796   -0.00244    0.00095   -0.00579
AFIX 148
H1    2    0.582589    0.536996    0.424099    11.00000   -1.50000
AFIX   0
HKLF    4




REM  116PAAZTA
REM wR2 = 0.1143, GooF = S = 1.032, Restrained GooF = 1.032 for all data
REM R1 = 0.0409 for 5524 Fo > 4sig(Fo) and 0.0447 for all 6066 data
REM 237 parameters refined using 0 restraints

END

WGHT      0.0654      0.4127

REM Highest difference peak  0.385,  deepest hole -0.260,  1-sigma level  0.059
Q1    1   0.2239  0.2593  0.3210  11.00000  0.05    0.38
Q2    1   0.2303  0.2653  0.5190  11.00000  0.05    0.36
Q3    1   0.4191  0.3628  0.4169  11.00000  0.05    0.33
Q4    1   0.2326  0.2748  0.4530  11.00000  0.05    0.33
Q5    1   0.4346  0.2590  0.3872  11.00000  0.05    0.33
Q6    1   0.3335  0.1201  0.7542  11.00000  0.05    0.31
Q7    1   0.4487  0.2139  0.6509  11.00000  0.05    0.30
Q8    1   0.4365  0.2651  0.4530  11.00000  0.05    0.30
Q9    1   0.4022  0.3361  0.7599  11.00000  0.05    0.30
Q10   1   0.4040  0.2149  0.1252  11.00000  0.05    0.29
Q11   1   0.2322  0.2764  0.3896  11.00000  0.05    0.28
Q12   1   0.3967  0.1650  0.7045  11.00000  0.05    0.28
Q13   1   0.4348  0.2314  0.1887  11.00000  0.05    0.27
Q14   1   0.4179  0.2777  0.7058  11.00000  0.05    0.27
Q15   1   0.4398  0.2541  0.5213  11.00000  0.05    0.26
Q16   1   0.2951  0.1869  0.7995  11.00000  0.05    0.25
Q17   1   0.4071  0.3156  0.1471  11.00000  0.05    0.24
Q18   1   0.3683  0.4049  0.1109  11.00000  0.05    0.23
Q19   1   0.4232  0.2335  0.2592  11.00000  0.05    0.23
Q20   1   0.3539  0.2851  0.0259  11.00000  0.05    0.21
;
_shelx_res_checksum              2013
_shelx_hkl_file
;
   0   0  -2 371.839 5.00289   1
   0   0   2 355.361 4.87190   2
   0   0  -3 21.5817 4.43544   1
   0   0   3 16.5118 4.59643   2
   0   0   4 3298.64 10.5563   3
   0   0  -4 3325.16 19.4258   1
   0   0   4 3283.61 18.4882   2
   0   0   5 25.7008 3.49367   3
   0   0  -5 20.6084 6.60672   1
   0   0   5 31.9646 6.51247   2
   0   0   6 16099.8 27.4556   3
   0   0  -6 16098.7 50.6366   1
   0   0   6 16102.7 49.2994   2
   0   0   7 26.8239 4.06205   3
   0   0  -7 14.7876 8.13912   1
   0   0   7 27.6059 8.15723   2
   0   0   8 25334.3 39.1876   3
   0   0  -8 25299.4 73.1547   1
   0   0   9 10.2331 5.08035   3
   0   0  -9 15.4251 10.4755   1
   0   0   9-0.02337 9.86168   2
   0   0  10 39504.0 53.1891   3
   0   0 -10 39285.9 104.835   1
   0   0  10 39560.9 100.106   2
   0   0  11 34.6864 5.51069   3
   0   0 -11 21.9258 11.1131   1
   0   0  11 18.7092 10.8786   2
   0   0  12 75.3430 5.99618   3
   0   0 -12 61.1714 12.9578   1
   0   0  12 54.7155 12.3944   2
   0   0  13 12.0008 6.16141   3
   0   0  13-1.54029 12.8324   2
   0   0 -13 4.15082 12.6918   1
   0   0  14 67282.9 158.349   2
   0   0 -14 67714.0 164.031   1
   0   0  15 411.988 24.8882   2
   0   0 -15 267.450 25.3817   1
   0   0  16 43495.5 138.465   2
   0   0 -16 44780.4 144.220   1
   0   0  17 226.125 20.5729   2
   0   0 -17 161.002 21.6962   1
   0   0  18 2226.03 37.6754   2
   0   0 -18 2278.39 39.2242   1
   0   0  19 11.1820 18.9789   2
   0   0 -19 24.0949 19.7188   1
   0   0  20 486.390 24.4480   2
   0   0 -20 554.703 27.4972   1
   0   0  21-11.2999 19.7673   2
   0   0 -21-9.51055 21.5159   1
   0   0  22 526.822 27.9319   2
   0   0 -22 510.068 29.7011   1
   0   0  23-36.2269 21.5856   2
   0   0 -23 10.7325 22.6472   1
   0   0  24 92.2565 23.5472   2
   0   0 -24 98.1233 25.9170   1
   0   0  25 27.9560 22.9516   2
   0   0 -25-41.2807 26.1524   1
   0   0 -26 449.668 33.5653   1
   0  -1   0 911.539 6.40798   1
   0   1   0 919.198 6.67822   3
   0   1   1 11116.0 22.1742   3
   0  -1   1 11061.4 22.2668   3
   0  -1  -1 11115.1 23.7805   1
   0  -1   1 11171.8 22.4029   1
   0  -1   2 2037.38 10.3946   3
   0   1   2 1974.04 9.88003   3
   0  -1   2 2013.82 11.7178   1
   0  -1   2 2049.99 10.5774   2
   0   1   2 1989.94 10.0076   2
   0  -1  -2 2020.76 12.4955   1
   0  -1   3 2653.23 12.4520   3
   0  -1   3 2705.18 15.5374   1
   0   1   3 2589.26 12.0347   3
   0  -1   3 2586.66 14.4205   2
   0   1   3 2603.53 14.2827   2
   0  -1  -3 2730.18 16.3087   1
   0  -1   4 68604.5 62.2260   3
   0  -1   4 68639.4 83.4895   1
   0   1   4 68785.2 81.6607   2
   0  -1   4 69065.5 82.5530   2
   0   1   4 68984.4 59.4395   3
   0  -1  -4 68400.4 88.9545   1
   0   1   5 30649.2 41.9264   3
   0  -1   5 30579.3 62.4306   2
   0   1   5 31293.0 61.3336   2
   0   1  -5 30913.8 63.9300   1
   0  -1  -5 31615.8 66.6939   1
   0  -1   5 31037.2 44.0334   3
   0   1   6 749.953 8.01071   3
   0  -1   6 766.097 12.4258   2
   0   1   6 756.926 12.7491   2
   0   1  -6 739.026 13.2419   1
   0  -1  -6 730.940 13.0726   1
   0  -1   6 754.742 8.39164   3
   0   1   7 24751.9 40.7217   3
   0  -1   7 24642.2 65.9274   2
   0   1   7 24541.4 65.5220   2
   0  -1  -7 24860.3 68.9925   1
   0  -1   7 24925.1 43.1634   3
   0   1   8 5601.65 20.4533   3
   0  -1   8 5593.82 34.5959   2
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   8   7  -6 1814.11 37.0013   2
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   8   7  -5 106.399 22.5605   2
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   8   7  -3 349.577 27.4845   2
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 -13  -3   2 46.8080 24.8906   3
  13  -3  -2 13.0810 40.5663   2
  13   3  -2 6.08418 41.6160   2
 -13   3   2-5.86580 25.6935   3
 -13  -3   1 2923.50 51.1599   3
  13   3  -1 2932.29 67.7513   2
  13  -3  -1 3082.99 63.9879   2
 -13   3   1 2900.01 52.0888   3
 -13  -3   0 613.136 31.3051   3
  13   3   0 609.354 51.8902   2
 -13   3   0 665.079 33.8459   3
 -13  -3  -1 730.993 32.4930   3
  13  -3   1 715.191 50.0937   2
  13   3   1 713.044 52.4709   2
 -13   3  -1 619.323 32.8757   3
 -13  -3  -2 45.3132 23.7473   3
  13  -3   2-43.5341 40.3816   2
  13   3   2 69.7554 44.0129   2
 -13   3  -2 11.2463 24.6919   3
 -13  -3  -3 5.35570 23.3208   3
  13  -3   3 43.8050 40.3541   2
  13   3   3 48.5244 45.7456   2
 -13   3  -3 21.2535 24.3116   3
  13  -3   4 19.8507 40.4470   2
  13   3   4-13.3040 43.5221   2
 -13   3  -4 52.3802 24.5037   3
  13  -3   5 787.608 45.4960   2
  13   3   5 783.042 49.8751   2
  13  -3   6 1883.04 53.5217   2
  13   3   6 1790.98 60.1118   2
  13  -3   7 2547.89 59.9805   2
  13   3   7 2583.91 65.0903   2
  13  -3   8 3070.89 62.3292   2
  13   3   8 3132.49 68.3375   2
  13  -3   9 2255.03 56.1548   2
  13  -3  10 92.3944 34.6769   2
  13  -3  11 734.060 42.3060   2
 -13  -4   8 9233.99 91.9671   3
  13   4  -8 8968.27 92.6653   2
 -13   4   8 9183.63 93.6863   3
 -13  -4   7 1510.43 44.4722   3
  13   4  -7 1440.45 51.4655   2
 -13   4   7 1458.32 46.9712   3
 -13  -4   6 209.374 30.2287   3
  13   4  -6 206.228 40.0857   2
 -13  -4   5 902.336 36.9412   3
  13   4  -5 827.829 48.0272   2
 -13   4   5 930.082 39.5531   3
 -13  -4   4 3.47415 26.7825   3
  13   4  -4 29.8757 41.0599   2
 -13   4   4 82.5759 29.0147   3
 -13  -4   3 128.403 27.4656   3
  13   4  -3 57.3021 43.3491   2
 -13   4   3 124.416 27.4251   3
 -13  -4   2 230.227 28.7275   3
  13   4  -2 185.955 45.7791   2
 -13   4   2 202.758 29.1447   3
 -13  -4   1 372.779 31.6947   3
  13   4  -1 381.987 49.8399   2
  13  -4  -1 339.410 44.0435   2
 -13   4   1 376.307 31.9281   3
 -13  -4   0 168.201 26.8122   3
  13   4   0 196.931 50.2186   2
  13  -4   0 156.970 42.0625   2
 -13   4   0 134.469 29.0555   3
 -13  -4  -1 149.251 28.0000   3
  13  -4   1 86.8407 40.1100   2
  13   4   1 159.284 48.1268   2
 -13   4  -1 32.9252 26.1988   3
 -13  -4  -2 299.240 28.3314   3
  13  -4   2 307.318 41.6019   2
  13   4   2 366.514 49.0612   2
 -13   4  -2 332.052 30.4107   3
 -13  -4  -3 108.071 25.4377   3
  13   4   3 85.6185 49.5790   2
  13  -4   3 196.827 41.7792   2
 -13   4  -3 153.135 27.5294   3
  13   4   4-3.07963 48.3526   2
  13  -4   4-46.0278 38.5511   2
 -13   4  -4 59.5125 24.5614   3
  13  -4   5 568.111 41.8790   2
  13   4   5 526.473 51.2983   2
  13  -4   6 839.851 44.4914   2
  13   4   6 925.389 55.0064   2
  13  -4   7 79.9181 36.9976   2
  13   4   7 162.481 47.5261   2
 -13   5   6-31.7353 28.4879   3
  13   5  -6-12.7271 39.3569   2
 -13  -5   6 8.45316 26.7460   3
 -13   5   5-21.6862 26.9426   3
  13   5  -5 71.7363 40.9662   2
 -13  -5   5-6.35227 28.0987   3
 -13   5   4 65.0759 28.3560   3
  13   5  -4 22.6777 42.8557   2
 -13  -5   4 55.7276 28.9801   3
 -13   5   3 135.457 29.4947   3
  13   5  -3 183.279 47.1845   2
 -13  -5   3 138.642 29.1460   3
 -13   5   2 624.217 34.7957   3
 -13  -5   2 671.355 35.0926   3
 -13   5   1 393.283 32.3988   3
  13   5  -1 453.303 51.9277   2
 -13  -5   1 475.275 31.9856   3
 -13   5   0 905.219 37.8131   3
  13   5   0 906.630 55.2728   2
 -13  -5   0 884.339 36.0496   3
 -13   5  -1 3131.66 54.9403   3
  13   5   1 3111.31 73.6367   2
 -13  -5  -1 3067.92 53.4372   3
 -13   5  -2 453.233 31.8676   3
  13   5   2 448.030 54.5751   2
 -13  -5  -2 490.008 31.3747   3
 -13   5  -3 3286.98 54.8512   3
  13   5   3 3292.56 72.8749   2
 -13  -5  -3 3151.80 53.0004   3
 -13   5  -4 400.931 31.8782   3
  13   5   4 550.243 50.8848   2
  13   5   5 12.3836 46.3512   2
 -13  -6   4 1007.08 39.9280   3
 -13   6   3 91.3691 29.7970   3
  13   6  -3 177.190 45.4661   2
 -13  -6   3 83.4139 30.0043   3
 -13   6   2 747.137 37.4981   3
  13   6  -2 764.931 54.9320   2
 -13  -6   2 810.690 37.9578   3
 -13   6   1 392.674 32.6978   3
  13   6  -1 354.822 52.8372   2
 -13  -6   1 307.867 31.9790   3
 -13   6   0-34.6845 28.7833   3
  13   6   0-52.3323 49.5350   2
 -13  -6   0-2.42379 27.6868   3
 -13   6  -1-3.68298 27.5961   3
  13   6   1 1.71764 50.3502   2
 -13  -6  -1 14.8655 27.5579   3
 -13   6  -2 2578.71 52.2068   3
 -13  -6  -2 2558.11 51.1206   3
 -13   6  -3 510.268 33.0765   3
  13   6   3 547.432 52.3207   2
 -13  -6  -3 453.344 32.0800   3
 -13   6  -4 77.0080 27.8775   3
 -13  -7   0 1124.57 41.8399   3
 -13  -7  -1 162.906 30.8580   3
 -13   7  -2 48.8433 29.6053   3
 -13  -7  -2 113.723 29.9244   3
 -13   7  -3 148.866 30.5684   3
 -13   7  -4 451.368 32.9395   3
  14   0  -6 2498.07 62.1186   2
 -14   0   6 2522.43 54.1311   3
 -14   0   5-27.2611 28.7414   3
  14   0  -5-28.9634 41.6200   2
  14   0  -4 169.245 44.9563   2
 -14   0   4 183.330 29.4542   3
 -14   0   3-31.4583 26.4315   3
  14   0  -3-29.7365 45.1471   2
 -14   0   2 31.7899 28.7976   3
  14   0  -2-4.72778 44.9680   2
 -14   0   1 9.63433 28.8671   3
  14   0  -1-9.34180 49.2732   2
  14   0   0 1849.30 62.1883   2
 -14   0   0 1902.95 47.4190   3
 -14   0  -1-6.86408 27.7587   3
  14   0   1-7.31299 49.2192   2
  14   0   2 259.960 50.7914   2
 -14   0  -2 264.771 28.9110   3
  14   0   3 47.2088 47.0205   2
 -14   0  -3 48.0867 25.2067   3
  14   0   4 177.762 47.4429   2
  14   0   5 7.28654 43.4265   2
  14  -1  -7 33.6407 37.4726   2
  14  -1  -6 569.010 44.8614   2
  14  -1  -5 364.540 45.0914   2
  14   1  -5 313.872 46.0127   2
 -14   1   5 348.076 33.1301   3
 -14  -1   5 293.010 33.0897   3
  14  -1  -4 2595.51 63.8926   2
  14   1  -4 2605.30 65.2372   2
 -14   1   4 2718.91 54.9214   3
 -14  -1   4 2721.69 54.5393   3
  14  -1  -3 574.238 49.5711   2
  14   1  -3 469.569 50.4773   2
 -14   1   3 503.770 35.4885   3
 -14  -1   3 504.638 35.7086   3
  14  -1  -2 7507.47 94.9421   2
  14   1  -2 7715.97 94.8353   2
 -14   1   2 7747.74 82.3805   3
 -14  -1   2 7775.89 81.5218   3
  14   1  -1 794.253 57.1915   2
 -14   1   1 904.198 40.2092   3
 -14  -1   1 882.999 39.7738   3
  14  -1   0 12056.2 115.538   2
  14   1   0 11577.1 113.923   2
 -14   1   0 12171.9 99.2979   3
 -14  -1   0 11795.2 97.0095   3
 -14   1  -1 174.089 29.3504   3
  14  -1   1 136.235 48.8810   2
 -14  -1  -1 103.461 28.4181   3
  14  -1   2 463.815 50.8458   2
  14   1   2 508.880 54.2529   2
 -14   1  -2 513.408 32.0319   3
 -14   1  -3 109.641 26.6546   3
  14  -1   3 123.660 46.3068   2
  14   1   3 119.126 45.0954   2
 -14  -1  -3 156.695 27.2158   3
  14  -1   4 1609.61 59.1178   2
  14   1   4 1640.67 61.6917   2
  14  -1   5 338.682 46.9439   2
  14  -1   6 1234.76 53.8212   2
  14  -2  -7 202.829 40.2632   2
  14  -2  -6 79.6929 39.6991   2
 -14   2   5 16.4892 29.8600   3
 -14  -2   5-33.6865 29.3963   3
  14  -2  -4 344.719 45.6722   2
 -14   2   4 415.098 33.9332   3
 -14  -2   4 351.092 32.4122   3
  14  -2  -3 72.1053 45.9694   2
  14   2  -3 93.8582 48.6750   2
 -14   2   3 135.812 29.4833   3
 -14  -2   3 78.2824 28.8311   3
  14  -2  -2 62.2976 45.8093   2
  14   2  -2 161.726 49.0197   2
 -14   2   2 203.621 31.1882   3
 -14  -2   2 120.317 30.4923   3
 -14   2   1-6.40559 30.1276   3
  14  -2  -1-14.3299 48.4597   2
  14   2  -1 50.5870 49.3562   2
 -14  -2   1-36.3388 30.7375   3
  14  -2   0 6925.81 92.2274   2
  14   2   0 6806.22 96.9077   2
 -14   2   0 7001.50 79.3215   3
 -14  -2   0 6900.67 77.4020   3
  14  -2   1 501.532 50.9870   2
  14   2   1 380.168 52.4223   2
 -14  -2  -1 430.797 32.6839   3
 -14   2  -1 383.814 33.2330   3
 -14   2  -2 24.7222 26.7030   3
  14  -2   2-17.9754 43.1257   2
  14   2   2-72.5882 51.0601   2
 -14  -2  -2 14.5518 25.5243   3
  14  -2   3 317.114 46.0886   2
 -14   2  -3 272.138 29.3227   3
  14  -2   4 40.7181 43.3238   2
  14  -2   5 113.586 43.0567   2
  14  -2   6 891.014 50.0104   2
  14  -3  -7 1255.23 50.7078   2
  14  -3  -6-49.3714 40.0946   2
  14  -3  -5 337.049 44.6145   2
  14  -3  -4 50.6384 42.9424   2
 -14  -3   4-29.7353 29.3973   3
  14  -3  -3 736.938 50.5016   2
 -14   3   3 777.319 39.4673   3
 -14  -3   3 752.911 37.8237   3
  14  -3  -2 5883.88 84.5895   2
 -14   3   2 6036.47 77.1398   3
 -14  -3   2 6134.11 74.3307   3
 -14   3   1 77.2482 32.7872   3
 -14  -3   1 104.730 30.6694   3
  14  -3   0 10186.5 105.965   2
 -14  -3   0 10177.0 91.3563   3
  14  -3   1 662.746 51.0374   2
 -14   3  -1 596.382 37.1792   3
 -14  -3  -1 541.599 33.6259   3
  14  -3   2 993.364 52.8055   2
 -14   3  -2 1068.01 39.3060   3
 -14   3  -3 5.34372 26.4898   3
  14  -3   3-49.1631 45.0057   2
  14  -3   4 61.1154 42.7045   2
  14  -3   5 981.633 50.2195   2
  14  -3   6 163.520 41.4541   2
 -14  -4   2 430.082 33.9589   3
 -14   4   1 576.486 37.5070   3
 -14  -4   1 579.221 35.7747   3
 -14   4   0 1707.39 47.2961   3
 -14  -4   0 1769.82 47.1135   3
 -14   4  -1 109.748 30.9956   3
 -14  -4  -1 137.198 29.5809   3
 -14   4  -2 348.328 31.0755   3
 -14  -4  -2 350.612 31.3390   3
 -14   4  -3 276.326 30.8244   3
 -14  -5  -1 830.549 38.2524   3
 -14   5  -2-3.73920 29.5502   3
 -14  -5  -2 7.74290 28.2513   3
 -14   5  -3 164.918 30.5411   3
   0   0   0    0.00    0.00   0

data_xcalibur
_audit_creation_date           2022-03-04
_audit_creation_method         'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection     'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_cell_refinement     'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction      'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_cell_length_a                  10.2344(2)
_cell_length_b                  10.3325(2)
_cell_length_c                  18.6144(4)
_cell_angle_alpha               90.0
_cell_angle_beta                91.001(2)
_cell_angle_gamma               90.0
_cell_volume                    1968.11(8)
_cell_measurement_temperature   296.15(10)
_cell_measurement_reflns_used   16981
_cell_measurement_theta_min     1.9870
_cell_measurement_theta_max     31.5860
_cell_oxdiff_length_a                  10.2366(2)
_cell_oxdiff_length_b                  10.3301(2)
_cell_oxdiff_length_c                  18.6147(4)
_cell_oxdiff_angle_alpha               89.9933(16)
_cell_oxdiff_angle_beta                91.0128(16)
_cell_oxdiff_angle_gamma               89.9969(17)
_cell_oxdiff_volume                    1968.11(7)
_cell_oxdiff_measurement_reflns_used   16981
_exptl_absorpt_correction_T_min                   0.87431
_exptl_absorpt_correction_T_max                   1.00000
_exptl_crystal_description                prism
_exptl_crystal_colour                     'clear colourless'
_exptl_crystal_size_max                             0.370
_exptl_crystal_size_mid                             0.350
_exptl_crystal_size_min                             0.290
_exptl_absorpt_correction_type            multi-scan
_exptl_absorpt_process_details
)
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
)
_oxdiff_exptl_absorpt_empirical_full_min           0.873
_oxdiff_exptl_absorpt_empirical_full_max           1.196
_oxdiff_exptl_absorpt_empirical_details
)
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
)
_diffrn_ambient_temperature 296.15(10)
_diffrn_ambient_environment air
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device 'abstract diffractometer'
_diffrn_measurement_device_type
)
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
)
_diffrn_detector 'CCD plate'
_diffrn_reflns_number 22377
_diffrn_reflns_av_R_equivalents 0.0098
_diffrn_reflns_av_sigmaI/netI 0.0084
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_theta_min 1.9710
_diffrn_reflns_theta_max 31.4612
_diffrn_measured_fraction_theta_max 0.9294
_diffrn_reflns_theta_full 31.3907
_diffrn_measured_fraction_theta_full 0.9292
_diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11       0.0066703000
_diffrn_orient_matrix_UB_12       0.0496914000
_diffrn_orient_matrix_UB_13       0.0261009000
_diffrn_orient_matrix_UB_21      -0.0678629000
_diffrn_orient_matrix_UB_22       0.0131788000
_diffrn_orient_matrix_UB_23      -0.0031484000
_diffrn_orient_matrix_UB_31      -0.0123608000
_diffrn_orient_matrix_UB_32      -0.0455164000
_diffrn_orient_matrix_UB_33       0.0275901000
_diffrn_measurement_details
)
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
#--------------------------------------------------------------------------
  1  \w      4.25 184.25   0.50   15.00    --   30.00  73.76 -25.75  360
  2  \w      4.25 184.25   0.50   15.00    --   30.00  73.76  94.25  360
  3  \w      4.25 184.25   0.50   15.00    --   30.00  73.76-145.75  360
)
_diffrn_measurement_method '\w scans'
_space_group_IT_number 14
_space_group_crystal_system monoclinic
_space_group_name_H-M_alt 'P 1 21/n 1'
_reflns_odcompleteness_completeness		92.92
_reflns_odcompleteness_theta		31.39
_reflns_odcompleteness_iscentric		1

_chemical_name_systematic         'n/a'
_chemical_name_common             'n/a'
_chemical_melting_point           'Not measured'
_chemical_formula_moiety          'C22 H29 N3 O'

_diffrn_detector_type 'APEX II CCD Detector'
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Bruker APEX II'
computing_data_collection     'APEX-II (Bruker, 2004)'

_diffrn_ambient_temperature             150.0(2)
_cell_measurement_temperature   	150.0(2)
_diffrn_detector_area_resol_mean        8.3333

_atom_sites_solution_primary            dual
_atom_sites_solution_primary            difmap
_refine_ls_hydrogen_treatment		refxyz
_computing_structure_solution   'SHELXT 2015 (Sheldrick, 2015)'
_chemical_absolute_configuration        .

_publ_contact_author_name       'Toni Grell'
_publ_contact_author_email       'toni.grell@unimi.it'
_publ_contact_author_address
)
Via Camillo Golgi 19, 20133 Milan, Italy
)
;
_shelx_hkl_checksum              59761
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.42944(7) 0.43606(7) 0.41392(4) 0.01939(14) Uani 1 1 d . . . . .
H1A H 0.388850 0.470365 0.369149 0.023 Uiso 1 1 calc R U . . .
H1B H 0.390061 0.481119 0.455208 0.023 Uiso 1 1 calc R U . . .
C2 C 0.40447(7) 0.28926(7) 0.41944(4) 0.01691(13) Uani 1 1 d . . . . .
C3 C 0.46234(7) 0.22044(7) 0.35422(4) 0.01952(14) Uani 1 1 d . . . . .
H3A H 0.556547 0.241232 0.351423 0.023 Uiso 1 1 calc R U . . .
H3B H 0.453827 0.125642 0.360380 0.023 Uiso 1 1 calc R U . . .
C4 C 0.46964(7) 0.23261(7) 0.48707(4) 0.01835(14) Uani 1 1 d . . . . .
H4A H 0.468422 0.136997 0.483541 0.022 Uiso 1 1 calc R U . . .
H4B H 0.562195 0.260483 0.489054 0.022 Uiso 1 1 calc R U . . .
C5 C 0.25794(8) 0.22414(9) 0.29042(5) 0.02762(17) Uani 1 1 d . . . . .
H5A H 0.249585 0.129016 0.294813 0.033 Uiso 1 1 calc R U . . .
H5B H 0.212698 0.251258 0.245422 0.033 Uiso 1 1 calc R U . . .
C6 C 0.19426(8) 0.28923(9) 0.35430(5) 0.02745(17) Uani 1 1 d . . . . .
H6A H 0.195104 0.384308 0.347683 0.033 Uiso 1 1 calc R U . . .
H6B H 0.102134 0.260837 0.357430 0.033 Uiso 1 1 calc R U . . .
C7 C 0.20017(8) 0.29473(9) 0.48645(4) 0.02454(16) Uani 1 1 d . . . . .
H7A H 0.107385 0.267652 0.484350 0.029 Uiso 1 1 calc R U . . .
H7B H 0.203058 0.390155 0.491117 0.029 Uiso 1 1 calc R U . . .
C8 C 0.26804(8) 0.23284(8) 0.55118(4) 0.02290(15) Uani 1 1 d . . . . .
H8A H 0.224368 0.260303 0.595715 0.027 Uiso 1 1 calc R U . . .
H8B H 0.261574 0.137439 0.547571 0.027 Uiso 1 1 calc R U . . .
C9 C 0.45951(9) 0.19786(8) 0.22602(4) 0.02519(16) Uani 1 1 d . . . . .
H9A H 0.442717 0.103538 0.227529 0.030 Uiso 1 1 calc R U . . .
H9B H 0.555142 0.211108 0.230303 0.030 Uiso 1 1 calc R U . . .
C10 C 0.41164(8) 0.25054(8) 0.15455(4) 0.02216(15) Uani 1 1 d . . . . .
C11 C 0.38896(9) 0.16842(8) 0.09637(4) 0.02552(16) Uani 1 1 d . . . . .
H11 H 0.401759 0.077882 0.101969 0.031 Uiso 1 1 calc R U . . .
C12 C 0.34766(9) 0.21746(9) 0.02995(4) 0.02883(18) Uani 1 1 d . . . . .
H12 H 0.332463 0.160375 -0.009336 0.035 Uiso 1 1 calc R U . . .
C13 C 0.32883(10) 0.34898(10) 0.02122(5) 0.03117(18) Uani 1 1 d . . . . .
H13 H 0.301919 0.382542 -0.024212 0.037 Uiso 1 1 calc R U . . .
C14 C 0.34933(12) 0.43194(9) 0.07898(5) 0.0389(2) Uani 1 1 d . . . . .
H14 H 0.335066 0.522260 0.073337 0.047 Uiso 1 1 calc R U . . .
C15 C 0.39078(11) 0.38280(9) 0.14515(5) 0.0347(2) Uani 1 1 d . . . . .
H15 H 0.405035 0.440134 0.184431 0.042 Uiso 1 1 calc R U . . .
C16 C 0.47858(8) 0.20573(8) 0.61392(4) 0.02423(16) Uani 1 1 d . . . . .
H16A H 0.568891 0.240067 0.616003 0.029 Uiso 1 1 calc R U . . .
H16B H 0.484131 0.112284 0.602583 0.029 Uiso 1 1 calc R U . . .
C17 C 0.41932(8) 0.22063(8) 0.68732(4) 0.02217(15) Uani 1 1 d . . . . .
C18 C 0.36063(9) 0.11423(9) 0.71969(5) 0.02908(18) Uani 1 1 d . . . . .
H18 H 0.355601 0.034366 0.694484 0.035 Uiso 1 1 calc R U . . .
C19 C 0.30919(10) 0.12305(10) 0.78842(5) 0.0339(2) Uani 1 1 d . . . . .
H19 H 0.269279 0.049823 0.809761 0.041 Uiso 1 1 calc R U . . .
C20 C 0.31669(8) 0.23928(10) 0.82535(4) 0.03032(19) Uani 1 1 d . . . . .
H20 H 0.282390 0.245773 0.872324 0.036 Uiso 1 1 calc R U . . .
C21 C 0.37428(9) 0.34628(10) 0.79380(5) 0.02982(18) Uani 1 1 d . . . . .
H21 H 0.378720 0.426032 0.819142 0.036 Uiso 1 1 calc R U . . .
C22 C 0.42563(9) 0.33730(8) 0.72510(4) 0.02657(16) Uani 1 1 d . . . . .
H22 H 0.465099 0.410883 0.703891 0.032 Uiso 1 1 calc R U . . .
N1 N 0.39639(7) 0.25942(7) 0.28738(3) 0.02107(13) Uani 1 1 d . . . . .
N2 N 0.26480(6) 0.25550(7) 0.42063(4) 0.02087(13) Uani 1 1 d . . . . .
N3 N 0.40643(6) 0.27147(6) 0.55445(3) 0.01796(12) Uani 1 1 d . . . . .
O1 O 0.56715(6) 0.45830(6) 0.41382(3) 0.02376(13) Uani 1 1 d . . . . .
H1 H 0.5826(3) 0.5370(13) 0.4241(7) 0.036 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0209(3) 0.0177(3) 0.0195(3) -0.0008(2) -0.0009(2) -0.0007(2)
C2 0.0163(3) 0.0174(3) 0.0170(3) -0.0013(2) -0.0007(2) -0.0007(2)
C3 0.0215(3) 0.0204(3) 0.0167(3) -0.0021(2) -0.0015(2) 0.0020(2)
C4 0.0191(3) 0.0193(3) 0.0167(3) 0.0000(2) 0.0008(2) 0.0016(2)
C5 0.0245(4) 0.0359(4) 0.0222(4) -0.0051(3) -0.0059(3) -0.0039(3)
C6 0.0186(3) 0.0384(4) 0.0251(4) -0.0043(3) -0.0053(3) 0.0001(3)
C7 0.0173(3) 0.0321(4) 0.0242(4) -0.0031(3) 0.0017(3) -0.0004(3)
C8 0.0205(3) 0.0258(4) 0.0224(3) -0.0008(3) 0.0035(3) -0.0047(3)
C9 0.0329(4) 0.0253(4) 0.0172(3) -0.0027(3) -0.0022(3) 0.0059(3)
C10 0.0267(4) 0.0221(3) 0.0175(3) -0.0014(3) -0.0019(3) 0.0001(3)
C11 0.0357(4) 0.0216(3) 0.0192(3) -0.0023(3) 0.0004(3) -0.0019(3)
C12 0.0377(5) 0.0308(4) 0.0180(3) -0.0034(3) -0.0015(3) -0.0024(3)
C13 0.0382(5) 0.0338(4) 0.0213(4) 0.0034(3) -0.0039(3) 0.0022(4)
C14 0.0616(7) 0.0237(4) 0.0310(4) 0.0020(3) -0.0096(4) 0.0058(4)
C15 0.0555(6) 0.0223(4) 0.0260(4) -0.0044(3) -0.0107(4) 0.0031(4)
C16 0.0266(4) 0.0278(4) 0.0183(3) 0.0036(3) 0.0025(3) 0.0067(3)
C17 0.0232(3) 0.0255(4) 0.0179(3) 0.0031(3) 0.0007(3) 0.0035(3)
C18 0.0348(4) 0.0277(4) 0.0248(4) 0.0031(3) 0.0036(3) -0.0024(3)
C19 0.0346(4) 0.0413(5) 0.0259(4) 0.0081(4) 0.0052(3) -0.0056(4)
C20 0.0221(4) 0.0510(5) 0.0179(3) 0.0023(3) 0.0008(3) 0.0046(3)
C21 0.0313(4) 0.0364(5) 0.0217(4) -0.0038(3) -0.0023(3) 0.0061(3)
C22 0.0310(4) 0.0265(4) 0.0221(4) 0.0020(3) 0.0001(3) 0.0010(3)
N1 0.0226(3) 0.0243(3) 0.0163(3) -0.0031(2) -0.0027(2) 0.0015(2)
N2 0.0161(3) 0.0263(3) 0.0201(3) -0.0031(2) -0.0014(2) -0.0024(2)
N3 0.0184(3) 0.0193(3) 0.0162(3) 0.0003(2) 0.0008(2) -0.0004(2)
O1 0.0227(3) 0.0206(3) 0.0280(3) -0.0024(2) 0.0009(2) -0.0058(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 108.85(6) . . ?
O1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
O1 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
N2 C2 C4 107.84(6) . . ?
N2 C2 C3 106.89(6) . . ?
C4 C2 C3 107.73(6) . . ?
N2 C2 C1 113.34(6) . . ?
C4 C2 C1 111.14(6) . . ?
C3 C2 C1 109.66(6) . . ?
N1 C3 C2 111.51(6) . . ?
N1 C3 H3A 109.3 . . ?
C2 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
N3 C4 C2 113.78(6) . . ?
N3 C4 H4A 108.8 . . ?
C2 C4 H4A 108.8 . . ?
N3 C4 H4B 108.8 . . ?
C2 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
N1 C5 C6 110.36(6) . . ?
N1 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
N1 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
N2 C6 C5 110.02(7) . . ?
N2 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
N2 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N2 C7 C8 109.90(6) . . ?
N2 C7 H7A 109.7 . . ?
C8 C7 H7A 109.7 . . ?
N2 C7 H7B 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
N3 C8 C7 110.15(6) . . ?
N3 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
N3 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
N1 C9 C10 112.88(7) . . ?
N1 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
N1 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C11 C10 C15 118.49(8) . . ?
C11 C10 C9 120.82(7) . . ?
C15 C10 C9 120.68(7) . . ?
C10 C11 C12 120.79(8) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C13 C12 C11 120.07(8) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 119.83(8) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C13 C14 C15 119.98(9) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 C10 120.83(8) . . ?
C14 C15 H15 119.6 . . ?
C10 C15 H15 119.6 . . ?
N3 C16 C17 115.13(6) . . ?
N3 C16 H16A 108.5 . . ?
C17 C16 H16A 108.5 . . ?
N3 C16 H16B 108.5 . . ?
C17 C16 H16B 108.5 . . ?
H16A C16 H16B 107.5 . . ?
C18 C17 C22 118.65(7) . . ?
C18 C17 C16 119.51(8) . . ?
C22 C17 C16 121.80(7) . . ?
C17 C18 C19 121.13(9) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C20 C19 C18 119.55(9) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C21 120.06(8) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C20 C21 C22 120.32(9) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C21 C22 C17 120.30(8) . . ?
C21 C22 H22 119.9 . . ?
C17 C22 H22 119.9 . . ?
C3 N1 C5 109.33(6) . . ?
C3 N1 C9 109.88(6) . . ?
C5 N1 C9 111.20(6) . . ?
C7 N2 C6 114.72(6) . . ?
C7 N2 C2 113.66(6) . . ?
C6 N2 C2 113.34(6) . . ?
C8 N3 C4 109.08(6) . . ?
C8 N3 C16 111.87(6) . . ?
C4 N3 C16 106.80(6) . . ?
C1 O1 H1 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.4279(9) . ?
C1 C2 1.5417(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N2 1.4717(9) . ?
C2 C4 1.5300(10) . ?
C2 C3 1.5344(10) . ?
C3 N1 1.4613(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N3 1.4767(9) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N1 1.4650(11) . ?
C5 C6 1.5222(12) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N2 1.4612(10) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N2 1.4596(10) . ?
C7 C8 1.5206(12) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 N3 1.4716(10) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N1 1.4666(10) . ?
C9 C10 1.5106(11) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.3917(11) . ?
C10 C15 1.3935(12) . ?
C11 C12 1.3944(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.3815(13) . ?
C12 H12 0.9500 . ?
C13 C14 1.3878(13) . ?
C13 H13 0.9500 . ?
C14 C15 1.3912(13) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 N3 1.4840(10) . ?
C16 C17 1.5121(11) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.3944(12) . ?
C17 C22 1.3963(12) . ?
C18 C19 1.3946(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.3851(15) . ?
C19 H19 0.9500 . ?
C20 C21 1.3879(14) . ?
C20 H20 0.9500 . ?
C21 C22 1.3936(12) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
O1 H1 0.849(14) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 N3 0.85 2.02 2.8653(9) 172.3 3_666 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N2 179.49(6) . . . . ?
O1 C1 C2 C4 57.84(8) . . . . ?
O1 C1 C2 C3 -61.16(7) . . . . ?
N2 C2 C3 N1 58.70(8) . . . . ?
C4 C2 C3 N1 174.37(6) . . . . ?
C1 C2 C3 N1 -64.54(8) . . . . ?
N2 C2 C4 N3 -54.01(8) . . . . ?
C3 C2 C4 N3 -169.05(6) . . . . ?
C1 C2 C4 N3 70.80(8) . . . . ?
N1 C5 C6 N2 -56.13(10) . . . . ?
N2 C7 C8 N3 58.80(8) . . . . ?
N1 C9 C10 C11 -139.43(8) . . . . ?
N1 C9 C10 C15 41.39(12) . . . . ?
C15 C10 C11 C12 0.69(13) . . . . ?
C9 C10 C11 C12 -178.51(8) . . . . ?
C10 C11 C12 C13 0.04(14) . . . . ?
C11 C12 C13 C14 -0.91(15) . . . . ?
C12 C13 C14 C15 1.04(17) . . . . ?
C13 C14 C15 C10 -0.29(18) . . . . ?
C11 C10 C15 C14 -0.56(15) . . . . ?
C9 C10 C15 C14 178.64(10) . . . . ?
N3 C16 C17 C18 109.36(9) . . . . ?
N3 C16 C17 C22 -72.96(10) . . . . ?
C22 C17 C18 C19 -0.12(13) . . . . ?
C16 C17 C18 C19 177.64(8) . . . . ?
C17 C18 C19 C20 -0.16(14) . . . . ?
C18 C19 C20 C21 0.44(14) . . . . ?
C19 C20 C21 C22 -0.44(13) . . . . ?
C20 C21 C22 C17 0.16(13) . . . . ?
C18 C17 C22 C21 0.12(13) . . . . ?
C16 C17 C22 C21 -177.58(8) . . . . ?
C2 C3 N1 C5 -61.15(8) . . . . ?
C2 C3 N1 C9 176.55(6) . . . . ?
C6 C5 N1 C3 58.63(9) . . . . ?
C6 C5 N1 C9 -179.86(7) . . . . ?
C10 C9 N1 C3 -170.39(7) . . . . ?
C10 C9 N1 C5 68.43(9) . . . . ?
C8 C7 N2 C6 169.21(7) . . . . ?
C8 C7 N2 C2 -58.09(9) . . . . ?
C5 C6 N2 C7 -170.33(7) . . . . ?
C5 C6 N2 C2 56.83(9) . . . . ?
C4 C2 N2 C7 54.25(8) . . . . ?
C3 C2 N2 C7 169.84(6) . . . . ?
C1 C2 N2 C7 -69.23(8) . . . . ?
C4 C2 N2 C6 -172.40(6) . . . . ?
C3 C2 N2 C6 -56.80(8) . . . . ?
C1 C2 N2 C6 64.12(8) . . . . ?
C7 C8 N3 C4 -58.01(8) . . . . ?
C7 C8 N3 C16 -175.94(6) . . . . ?
C2 C4 N3 C8 57.30(8) . . . . ?
C2 C4 N3 C16 178.37(6) . . . . ?
C17 C16 N3 C8 -53.96(9) . . . . ?
C17 C16 N3 C4 -173.24(7) . . . . ?
