#------------------------------------------------------------------------------
#$Date: 2025-07-06 20:00:15 +0200 (Sun 06 de Jul de 2025) $
#$Revision: 301176 $
#$URL: svn://www.crystallography.net/cod/cif/7/16/04/7160441.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_7160441
loop_
_publ_author_name
'Ozturk, Sena'
'Davis, Alexander R.'
'Seaton, Colin C.'
'Male, Louise'
'Pike, Sarah J.'
_publ_section_title
;
 Solvatomorphism of a 2,6-pyridyldicarboxamide-based foldamer.
;
_journal_issue                   23
_journal_name_full               'Organic & biomolecular chemistry'
_journal_page_first              5590
_journal_page_last               5599
_journal_paper_doi               10.1039/d5ob00342c
_journal_volume                  23
_journal_year                    2025
_chemical_formula_moiety         'C31 H25 N9 O2'
_chemical_formula_sum            'C31 H25 N9 O2'
_chemical_formula_weight         555.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2025-02-24 deposited with the CCDC.	2025-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.4570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.56410(10)
_cell_length_b                   38.6957(4)
_cell_length_c                   12.34340(10)
_cell_measurement_reflns_used    25567
_cell_measurement_temperature    103(6)
_cell_measurement_theta_max      78.6570
_cell_measurement_theta_min      3.8530
_cell_volume                     5348.54(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      103(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     85.00 111.00   0.50    0.80    --  111.50 169.00 100.00   52
  2  ω     96.00 133.00   0.50    0.80    --  111.50 125.00  30.00   74
  3  ω    151.00 178.00   0.50    0.80    --  111.50 125.00  30.00   54
  4  ω     95.00 156.00   0.50    0.80    --  111.50 125.00 -30.00  122
  5  ω    103.00 143.00   0.50    0.80    --  111.50 115.00 -43.00   80
  6  ω    109.00 173.00   0.50    0.80    --  111.50  57.00 120.00  128
  7  ω    -25.00  24.00   0.50    0.20    --  -49.04  19.00 -30.00   98
  8  ω    -25.00  25.00   0.50    0.20    --  -49.04  19.00 -90.00  100
  9  ω     -9.00  22.00   0.50    0.20    --  -49.04  38.00  90.00   62
 10  ω    -65.00 -29.00   0.50    0.80    --  -90.00  57.00 150.00   72
 11  ω    -63.00 -23.00   0.50    0.80    --  -90.00  57.00  90.00   80
 12  ω    -45.00 -10.00   0.50    0.20    --  -49.04 115.00 -43.00   70
 13  ω   -100.00 -75.00   0.50    0.80    --  -90.00 169.00 100.00   50
 14  ω    -83.00 -55.00   0.50    0.80    --  -90.00 115.00 -43.00   56
 15  ω   -156.00 -77.00   0.50    0.80    --  -90.00 -57.00 -90.00  158
 16  ω   -121.00 -85.00   0.50    0.80    --  -90.00-115.00-132.00   72
 17  ω    -98.00 -73.00   0.50    0.80    --  -90.00-125.00 -90.00   50
 18  ω   -161.00-104.00   0.50    0.80    --  -90.00-125.00 -90.00  114
 19  ω   -120.00 -47.00   0.50    0.20    --  -49.04-169.00  83.00  146
 20  ω   -114.00 -88.00   0.50    0.80    --  -90.00 -38.00  60.00   52
 21  ω     65.00  90.00   0.50    0.20    --   49.04-169.00  83.00   50
 22  ω    117.00 142.00   0.50    0.80    --  111.50-169.00  83.00   50
 23  ω     40.00 106.00   0.50    0.80    --  111.50 -99.00 -30.00  132
 24  ω     35.00  60.00   0.50    0.20    --   49.04-115.00-132.00   50
 25  ω     68.00 108.00   0.50    0.80    --  111.50-115.00-132.00   80
 26  ω     43.00  76.00   0.50    0.80    --  111.50 -77.00-120.00   66
 27  ω     41.00  91.00   0.50    0.80    --  111.50 -77.00-150.00  100
 28  ω     40.00  65.00   0.50    0.80    --  111.50 -57.00 -90.00   50
 29  ω    -23.00   7.00   0.50    0.20    --   49.04 -19.00 -60.00   60
 30  ω    -22.00  21.00   0.50    0.20    --   49.04 -19.00 120.00   86
 31  ω     41.00  66.00   0.50    0.80    --  111.50 -57.00   0.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0202451000
_diffrn_orient_matrix_UB_12      0.0000923000
_diffrn_orient_matrix_UB_13      -0.1282087000
_diffrn_orient_matrix_UB_21      0.0308820000
_diffrn_orient_matrix_UB_22      -0.0387790000
_diffrn_orient_matrix_UB_23      0.0028098000
_diffrn_orient_matrix_UB_31      -0.1324859000
_diffrn_orient_matrix_UB_32      -0.0090455000
_diffrn_orient_matrix_UB_33      -0.0132083000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39445
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.501
_diffrn_reflns_theta_min         3.871
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.168
_refine_diff_density_max         1.339
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         10243
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0581P)²+3.9271P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9045
_reflns_number_total             10243
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ob00342c2.cif
_cod_data_source_block           SP031_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7160437--7160444.cif.'
_cod_database_code               7160441
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H30 N5 O5'
_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.
;
_reflns_odcompleteness_completeness 98.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N1-H1A = N1-H1B
 0.86 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28),
  C29(H29), C30(H30), C31(H31), C103(H103), C104(H104), C105(H105), C106(H106),
 C109(H109), C110(H110), C111(H111), C112(H112), C115(H115), C116(H116),
 C117(H117), C122(H122), C123(H123), C124(H124), C125(H125), C128(H128),
 C129(H129), C130(H130), C131(H131)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.211
_oxdiff_exptl_absorpt_empirical_full_min 0.815
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.26519(16) 0.02572(5) 0.24821(17) 0.0286(4) Uani 1 1 d . . . . .
C2 C 0.24083(15) 0.06023(5) 0.27234(16) 0.0254(4) Uani 1 1 d . . . . .
C3 C 0.23341(16) 0.08592(5) 0.19062(16) 0.0294(4) Uani 1 1 d . . . . .
H3 H 0.218091 0.108648 0.207229 0.035 Uiso 1 1 calc R U . . .
C4 C 0.24847(18) 0.07801(6) 0.08626(18) 0.0375(5) Uani 1 1 d . . . . .
H4 H 0.243767 0.095245 0.032819 0.045 Uiso 1 1 calc R U . . .
C5 C 0.27059(18) 0.04425(6) 0.06187(18) 0.0385(5) Uani 1 1 d . . . . .
H5 H 0.280081 0.038872 -0.008837 0.046 Uiso 1 1 calc R U . . .
C6 C 0.27891(17) 0.01840(6) 0.13956(19) 0.0365(5) Uani 1 1 d . . . . .
H6 H 0.293710 -0.004153 0.120744 0.044 Uiso 1 1 calc R U . . .
C7 C 0.19268(15) 0.10153(4) 0.51458(15) 0.0229(4) Uani 1 1 d . . . . .
C8 C 0.14264(15) 0.13301(4) 0.53683(15) 0.0223(4) Uani 1 1 d . . . . .
C9 C 0.14144(16) 0.14141(5) 0.64682(15) 0.0254(4) Uani 1 1 d . . . . .
H9 H 0.106990 0.161964 0.662128 0.030 Uiso 1 1 calc R U . . .
C10 C 0.19194(17) 0.11887(5) 0.73257(16) 0.0272(4) Uani 1 1 d . . . . .
H10 H 0.191988 0.124554 0.805786 0.033 Uiso 1 1 calc R U . . .
C11 C 0.24264(18) 0.08786(5) 0.71100(16) 0.0289(4) Uani 1 1 d . . . . .
H11 H 0.276189 0.072960 0.769534 0.035 Uiso 1 1 calc R U . . .
C12 C 0.24314(17) 0.07919(5) 0.60267(16) 0.0275(4) Uani 1 1 d . . . . .
H12 H 0.277111 0.058455 0.588262 0.033 Uiso 1 1 calc R U . . .
C13 C 0.07067(15) 0.18863(4) 0.44604(15) 0.0232(4) Uani 1 1 d . . . . .
C14 C 0.03002(15) 0.20447(4) 0.33145(15) 0.0230(4) Uani 1 1 d . . . . .
C15 C 0.00230(17) 0.23954(5) 0.32128(16) 0.0272(4) Uani 1 1 d . . . . .
H15 H 0.007721 0.253211 0.384329 0.033 Uiso 1 1 calc R U . . .
C16 C -0.03351(17) 0.25353(5) 0.21493(17) 0.0290(4) Uani 1 1 d . . . . .
H16 H -0.054387 0.276742 0.205231 0.035 Uiso 1 1 calc R U . . .
C17 C -0.03786(16) 0.23256(5) 0.12331(17) 0.0273(4) Uani 1 1 d . . . . .
H17 H -0.061274 0.241444 0.051130 0.033 Uiso 1 1 calc R U . . .
C18 C -0.00647(15) 0.19783(4) 0.14113(15) 0.0236(4) Uani 1 1 d . . . . .
C19 C -0.00734(15) 0.17473(5) 0.04276(15) 0.0242(4) Uani 1 1 d . . . . .
C20 C -0.03068(15) 0.11214(5) -0.00496(15) 0.0234(4) Uani 1 1 d . . . . .
C21 C -0.05693(15) 0.08042(5) 0.03938(15) 0.0233(4) Uani 1 1 d . . . . .
C22 C -0.07536(17) 0.05096(5) -0.02790(17) 0.0289(4) Uani 1 1 d . . . . .
H22 H -0.092368 0.029957 0.001341 0.035 Uiso 1 1 calc R U . . .
C23 C -0.06844(18) 0.05290(5) -0.13751(17) 0.0328(4) Uani 1 1 d . . . . .
H23 H -0.081774 0.033301 -0.182527 0.039 Uiso 1 1 calc R U . . .
C24 C -0.04142(18) 0.08428(5) -0.18087(17) 0.0323(4) Uani 1 1 d . . . . .
H24 H -0.036001 0.085364 -0.254710 0.039 Uiso 1 1 calc R U . . .
C25 C -0.02246(17) 0.11393(5) -0.11560(16) 0.0282(4) Uani 1 1 d . . . . .
H25 H -0.004490 0.134754 -0.145309 0.034 Uiso 1 1 calc R U . . .
C26 C -0.10197(15) 0.05360(4) 0.30066(15) 0.0228(4) Uani 1 1 d . . . . .
C27 C -0.11257(15) 0.02087(5) 0.34820(16) 0.0248(4) Uani 1 1 d . . . . .
C28 C -0.13037(16) 0.01955(5) 0.45661(16) 0.0275(4) Uani 1 1 d . . . . .
H28 H -0.137464 -0.001718 0.489422 0.033 Uiso 1 1 calc R U . . .
C29 C -0.13740(17) 0.04968(5) 0.51484(16) 0.0290(4) Uani 1 1 d . . . . .
H29 H -0.148583 0.048436 0.586776 0.035 Uiso 1 1 calc R U . . .
C30 C -0.12791(18) 0.08206(5) 0.46697(16) 0.0297(4) Uani 1 1 d . . . . .
H30 H -0.133369 0.102211 0.506463 0.036 Uiso 1 1 calc R U . . .
C31 C -0.11048(17) 0.08369(5) 0.36119(16) 0.0275(4) Uani 1 1 d . . . . .
H31 H -0.104208 0.105136 0.329135 0.033 Uiso 1 1 calc R U . . .
N1 N 0.27036(17) 0.00064(5) 0.32490(17) 0.0378(4) Uani 1 1 d D . . . .
H1A H 0.320(3) -0.0183(7) 0.320(3) 0.095(12) Uiso 1 1 d D . . . .
H1B H 0.283(3) 0.0100(8) 0.3977(18) 0.082(11) Uiso 1 1 d D . . . .
N2 N 0.23103(13) 0.06600(4) 0.38279(13) 0.0252(3) Uani 1 1 d . . . . .
N3 N 0.19417(13) 0.09573(4) 0.40123(13) 0.0234(3) Uani 1 1 d . . . . .
N4 N 0.09439(13) 0.15445(4) 0.44506(13) 0.0236(3) Uani 1 1 d . . . . .
H4A H 0.092(2) 0.1458(6) 0.380(2) 0.031(6) Uiso 1 1 d . . . . .
N5 N 0.02494(13) 0.18373(4) 0.24358(13) 0.0223(3) Uani 1 1 d . . . . .
N6 N -0.01478(14) 0.14074(4) 0.06679(13) 0.0243(3) Uani 1 1 d . . . . .
H6A H -0.018(2) 0.1359(6) 0.135(2) 0.031(6) Uiso 1 1 d . . . . .
N7 N -0.06721(13) 0.08169(4) 0.15148(13) 0.0229(3) Uani 1 1 d . . . . .
N8 N -0.08575(13) 0.05263(4) 0.19140(13) 0.0236(3) Uani 1 1 d . . . . .
N9 N -0.10744(16) -0.00878(4) 0.28910(16) 0.0330(4) Uani 1 1 d . . . . .
H9A H -0.101(2) -0.0285(7) 0.323(2) 0.041(7) Uiso 1 1 d . . . . .
H9B H -0.092(2) -0.0067(7) 0.220(2) 0.052(8) Uiso 1 1 d . . . . .
O1 O 0.08021(12) 0.20628(3) 0.53056(11) 0.0295(3) Uani 1 1 d . . . . .
O2 O -0.00309(12) 0.18683(3) -0.04788(11) 0.0308(3) Uani 1 1 d . . . . .
C101 C 0.62313(19) 0.27604(5) 0.8589(2) 0.0391(5) Uani 1 1 d . . . . .
C102 C 0.68106(17) 0.30558(5) 0.83032(19) 0.0330(4) Uani 1 1 d . . . . .
C103 C 0.74334(19) 0.32767(6) 0.91293(19) 0.0377(5) Uani 1 1 d . . . . .
H103 H 0.781566 0.346901 0.892929 0.045 Uiso 1 1 calc R U . . .
C104 C 0.7495(2) 0.32155(6) 1.0245(2) 0.0428(5) Uani 1 1 d . . . . .
H104 H 0.792493 0.336272 1.079501 0.051 Uiso 1 1 calc R U . . .
C105 C 0.6903(2) 0.29300(6) 1.0531(2) 0.0462(6) Uani 1 1 d . . . . .
H105 H 0.692977 0.288942 1.127949 0.055 Uiso 1 1 calc R U . . .
C106 C 0.6283(2) 0.27076(6) 0.9732(2) 0.0412(5) Uani 1 1 d . . . . .
H106 H 0.589010 0.251936 0.994468 0.049 Uiso 1 1 calc R U . . .
C107 C 0.68770(16) 0.34398(5) 0.57058(17) 0.0291(4) Uani 1 1 d . . . . .
C108 C 0.66777(16) 0.37759(5) 0.52494(17) 0.0285(4) Uani 1 1 d . . . . .
C109 C 0.67138(17) 0.38325(6) 0.41446(17) 0.0333(4) Uani 1 1 d . . . . .
H109 H 0.658272 0.405242 0.383465 0.040 Uiso 1 1 calc R U . . .
C110 C 0.69476(18) 0.35572(7) 0.35104(18) 0.0400(5) Uani 1 1 d . . . . .
H110 H 0.698622 0.359582 0.277660 0.048 Uiso 1 1 calc R U . . .
C111 C 0.71246(18) 0.32259(6) 0.3947(2) 0.0422(5) Uani 1 1 d . . . . .
H111 H 0.726592 0.304391 0.350514 0.051 Uiso 1 1 calc R U . . .
C112 C 0.70901(17) 0.31674(6) 0.50413(19) 0.0359(5) Uani 1 1 d . . . . .
H112 H 0.720951 0.294544 0.533696 0.043 Uiso 1 1 calc R U . . .
C113 C 0.61274(16) 0.43690(5) 0.57232(16) 0.0279(4) Uani 1 1 d . . . . .
C114 C 0.59149(15) 0.45622(5) 0.67107(16) 0.0249(4) Uani 1 1 d . . . . .
C115 C 0.58225(16) 0.49206(5) 0.66775(17) 0.0285(4) Uani 1 1 d . . . . .
H115 H 0.586864 0.504307 0.604135 0.034 Uiso 1 1 calc R U . . .
C116 C 0.56607(16) 0.50898(5) 0.76127(18) 0.0302(4) Uani 1 1 d . . . . .
H116 H 0.559650 0.532938 0.761605 0.036 Uiso 1 1 calc R U . . .
C117 C 0.55947(16) 0.48997(5) 0.85466(17) 0.0281(4) Uani 1 1 d . . . . .
H117 H 0.552199 0.500886 0.919762 0.034 Uiso 1 1 calc R U . . .
C118 C 0.56401(15) 0.45408(4) 0.84841(16) 0.0237(4) Uani 1 1 d . . . . .
C119 C 0.54391(16) 0.43247(4) 0.94404(16) 0.0246(4) Uani 1 1 d . . . . .
C120 C 0.47795(15) 0.37313(4) 0.97753(15) 0.0226(4) Uani 1 1 d . . . . .
C121 C 0.42420(15) 0.34353(4) 0.91944(15) 0.0221(4) Uani 1 1 d . . . . .
C122 C 0.38441(16) 0.31701(5) 0.97758(16) 0.0268(4) Uani 1 1 d . . . . .
H122 H 0.349546 0.297414 0.939370 0.032 Uiso 1 1 calc R U . . .
C123 C 0.39637(17) 0.31961(5) 1.09138(16) 0.0285(4) Uani 1 1 d . . . . .
H123 H 0.369360 0.301910 1.129761 0.034 Uiso 1 1 calc R U . . .
C124 C 0.44882(17) 0.34874(5) 1.14791(16) 0.0285(4) Uani 1 1 d . . . . .
H124 H 0.456487 0.350423 1.224539 0.034 Uiso 1 1 calc R U . . .
C125 C 0.49017(16) 0.37543(5) 1.09301(16) 0.0260(4) Uani 1 1 d . . . . .
H125 H 0.525755 0.394735 1.132529 0.031 Uiso 1 1 calc R U . . .
C126 C 0.35225(15) 0.31494(5) 0.63749(15) 0.0235(4) Uani 1 1 d . . . . .
C127 C 0.29640(16) 0.28471(5) 0.58466(17) 0.0265(4) Uani 1 1 d . . . . .
C128 C 0.28531(17) 0.28083(5) 0.46948(17) 0.0319(4) Uani 1 1 d . . . . .
H128 H 0.249020 0.261135 0.433067 0.038 Uiso 1 1 calc R U . . .
C129 C 0.32742(18) 0.30578(6) 0.40971(17) 0.0346(5) Uani 1 1 d . . . . .
H129 H 0.318712 0.302777 0.333341 0.041 Uiso 1 1 calc R U . . .
C130 C 0.38295(18) 0.33551(5) 0.46193(17) 0.0323(4) Uani 1 1 d . . . . .
H130 H 0.411660 0.352146 0.420914 0.039 Uiso 1 1 calc R U . . .
C131 C 0.39489(16) 0.34000(5) 0.57527(16) 0.0271(4) Uani 1 1 d . . . . .
H131 H 0.431522 0.359819 0.610520 0.033 Uiso 1 1 calc R U . . .
N101 N 0.5635(2) 0.25366(5) 0.7782(2) 0.0494(5) Uani 1 1 d . . . . .
H10A H 0.546(3) 0.2624(9) 0.704(3) 0.079(11) Uiso 1 1 d . . . . .
H10B H 0.508(4) 0.2390(11) 0.805(3) 0.110(14) Uiso 1 1 d . . . . .
N102 N 0.67104(14) 0.30985(4) 0.71384(16) 0.0330(4) Uani 1 1 d . . . . .
N103 N 0.69004(14) 0.34038(4) 0.68512(14) 0.0291(4) Uani 1 1 d . . . . .
N104 N 0.64257(14) 0.40333(4) 0.59543(14) 0.0272(3) Uani 1 1 d . . . . .
H10C H 0.647(2) 0.3963(6) 0.664(2) 0.039(6) Uiso 1 1 d . . . . .
N105 N 0.57998(12) 0.43726(4) 0.75888(13) 0.0229(3) Uani 1 1 d . . . . .
N106 N 0.51596(14) 0.39910(4) 0.91505(13) 0.0234(3) Uani 1 1 d . . . . .
H10D H 0.512(2) 0.3940(6) 0.846(2) 0.032(6) Uiso 1 1 d . . . . .
N107 N 0.41732(13) 0.34267(4) 0.80301(13) 0.0228(3) Uani 1 1 d . . . . .
N108 N 0.35935(13) 0.31710(4) 0.75296(13) 0.0243(3) Uani 1 1 d . . . . .
N109 N 0.25863(16) 0.25924(4) 0.64617(16) 0.0322(4) Uani 1 1 d . . . . .
H10E H 0.252(2) 0.2668(7) 0.713(2) 0.042(7) Uiso 1 1 d . . . . .
H10F H 0.202(2) 0.2442(7) 0.612(2) 0.049(7) Uiso 1 1 d . . . . .
O101 O 0.60379(14) 0.45119(4) 0.48180(12) 0.0395(4) Uani 1 1 d . . . . .
O102 O 0.54989(13) 0.44524(3) 1.03620(11) 0.0324(3) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 7 -7 0.0864
1 -7 7 0.0864
-7 -6 2 0.0935
7 6 -1 0.2021
6 1 2 0.1895
1 -25 0 0.1065
-1 25 0 0.0930
-6 -13 1 0.1119
1 -18 -5 0.1155
0 19 5 0.0475
-7 4 4 0.0896
-7 0 1 0.0906
3 -23 -1 0.1107
4 -20 -2 0.1461
0 19 -5 0.0934
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
C2 C1 C6 117.62(19) . . ?
N1 C1 C2 120.63(19) . . ?
N1 C1 C6 121.69(18) . . ?
C1 C2 N2 114.90(17) . . ?
C3 C2 C1 119.87(18) . . ?
C3 C2 N2 125.17(16) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.04(19) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.3(2) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.5(2) . . ?
C6 C5 H5 119.3 . . ?
C1 C6 H6 119.6 . . ?
C5 C6 C1 120.71(19) . . ?
C5 C6 H6 119.6 . . ?
C8 C7 N3 115.87(15) . . ?
C12 C7 C8 119.77(17) . . ?
C12 C7 N3 124.25(16) . . ?
C9 C8 C7 119.69(16) . . ?
C9 C8 N4 123.23(16) . . ?
N4 C8 C7 117.07(16) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.44(17) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 H10 119.5 . . ?
C9 C10 C11 121.02(18) . . ?
C11 C10 H10 119.5 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 119.95(18) . . ?
C12 C11 H11 120.0 . . ?
C7 C12 H12 119.9 . . ?
C11 C12 C7 120.11(17) . . ?
C11 C12 H12 119.9 . . ?
N4 C13 C14 113.99(15) . . ?
O1 C13 C14 120.82(16) . . ?
O1 C13 N4 125.19(17) . . ?
C15 C14 C13 119.49(16) . . ?
N5 C14 C13 117.23(15) . . ?
N5 C14 C15 123.27(17) . . ?
C14 C15 H15 120.9 . . ?
C16 C15 C14 118.29(17) . . ?
C16 C15 H15 120.9 . . ?
C15 C16 H16 120.4 . . ?
C17 C16 C15 119.17(17) . . ?
C17 C16 H16 120.4 . . ?
C16 C17 H17 120.6 . . ?
C16 C17 C18 118.79(18) . . ?
C18 C17 H17 120.6 . . ?
C17 C18 C19 119.71(16) . . ?
N5 C18 C17 122.62(17) . . ?
N5 C18 C19 117.67(15) . . ?
N6 C19 C18 112.79(16) . . ?
O2 C19 C18 121.07(16) . . ?
O2 C19 N6 126.13(17) . . ?
C25 C20 C21 119.89(16) . . ?
C25 C20 N6 123.35(17) . . ?
N6 C20 C21 116.75(16) . . ?
C20 C21 N7 115.34(15) . . ?
C22 C21 C20 119.79(17) . . ?
C22 C21 N7 124.83(17) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.17(18) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 120.1 . . ?
C22 C23 C24 119.90(18) . . ?
C24 C23 H23 120.1 . . ?
C23 C24 H24 119.5 . . ?
C25 C24 C23 121.04(19) . . ?
C25 C24 H24 119.5 . . ?
C20 C25 H25 120.4 . . ?
C24 C25 C20 119.21(18) . . ?
C24 C25 H25 120.4 . . ?
C31 C26 C27 119.90(17) . . ?
C31 C26 N8 125.26(16) . . ?
N8 C26 C27 114.83(15) . . ?
C28 C27 C26 118.45(17) . . ?
N9 C27 C26 120.65(18) . . ?
N9 C27 C28 120.89(17) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 C27 120.42(17) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 H29 119.5 . . ?
C28 C29 C30 120.92(18) . . ?
C30 C29 H29 119.5 . . ?
C29 C30 H30 120.4 . . ?
C31 C30 C29 119.21(18) . . ?
C31 C30 H30 120.4 . . ?
C26 C31 H31 119.5 . . ?
C30 C31 C26 121.10(17) . . ?
C30 C31 H31 119.5 . . ?
C1 N1 H1A 116(2) . . ?
C1 N1 H1B 111(2) . . ?
H1A N1 H1B 114(3) . . ?
N3 N2 C2 115.35(15) . . ?
N2 N3 C7 114.05(15) . . ?
C8 N4 H4A 115.8(15) . . ?
C13 N4 C8 127.76(16) . . ?
C13 N4 H4A 115.3(15) . . ?
C14 N5 C18 117.81(15) . . ?
C19 N6 C20 129.32(16) . . ?
C19 N6 H6A 116.1(15) . . ?
C20 N6 H6A 114.1(15) . . ?
N8 N7 C21 114.34(14) . . ?
N7 N8 C26 115.15(14) . . ?
C27 N9 H9A 119.3(17) . . ?
C27 N9 H9B 117.8(17) . . ?
H9A N9 H9B 121(2) . . ?
C106 C101 C102 117.5(2) . . ?
N101 C101 C102 120.9(2) . . ?
N101 C101 C106 121.6(2) . . ?
C101 C102 N102 115.0(2) . . ?
C103 C102 C101 120.4(2) . . ?
C103 C102 N102 124.61(18) . . ?
C102 C103 H103 119.5 . . ?
C104 C103 C102 121.0(2) . . ?
C104 C103 H103 119.5 . . ?
C103 C104 H104 120.5 . . ?
C103 C104 C105 118.9(2) . . ?
C105 C104 H104 120.5 . . ?
C104 C105 H105 119.4 . . ?
C106 C105 C104 121.2(2) . . ?
C106 C105 H105 119.4 . . ?
C101 C106 H106 119.6 . . ?
C105 C106 C101 120.8(2) . . ?
C105 C106 H106 119.6 . . ?
C108 C107 N103 116.73(17) . . ?
C112 C107 C108 119.8(2) . . ?
C112 C107 N103 123.45(18) . . ?
C109 C108 C107 119.56(19) . . ?
C109 C108 N104 123.98(18) . . ?
N104 C108 C107 116.45(18) . . ?
C108 C109 H109 120.3 . . ?
C110 C109 C108 119.3(2) . . ?
C110 C109 H109 120.3 . . ?
C109 C110 H110 119.3 . . ?
C111 C110 C109 121.4(2) . . ?
C111 C110 H110 119.3 . . ?
C110 C111 H111 120.2 . . ?
C112 C111 C110 119.7(2) . . ?
C112 C111 H111 120.2 . . ?
C107 C112 H112 119.9 . . ?
C111 C112 C107 120.3(2) . . ?
C111 C112 H112 119.9 . . ?
N104 C113 C114 113.00(16) . . ?
O101 C113 C114 121.39(17) . . ?
O101 C113 N104 125.61(19) . . ?
C115 C114 C113 119.97(17) . . ?
N105 C114 C113 116.92(16) . . ?
N105 C114 C115 123.10(18) . . ?
C114 C115 H115 120.9 . . ?
C116 C115 C114 118.30(18) . . ?
C116 C115 H115 120.9 . . ?
C115 C116 H116 120.3 . . ?
C115 C116 C117 119.42(17) . . ?
C117 C116 H116 120.3 . . ?
C116 C117 H117 120.9 . . ?
C116 C117 C118 118.21(18) . . ?
C118 C117 H117 120.9 . . ?
C117 C118 C119 119.55(17) . . ?
N105 C118 C117 123.17(18) . . ?
N105 C118 C119 117.21(15) . . ?
N106 C119 C118 113.17(16) . . ?
O102 C119 C118 121.18(16) . . ?
O102 C119 N106 125.62(18) . . ?
C125 C120 C121 119.28(16) . . ?
C125 C120 N106 123.27(16) . . ?
N106 C120 C121 117.45(16) . . ?
C120 C121 N107 116.10(15) . . ?
C122 C121 C120 119.75(17) . . ?
C122 C121 N107 124.13(16) . . ?
C121 C122 H122 119.7 . . ?
C123 C122 C121 120.52(17) . . ?
C123 C122 H122 119.7 . . ?
C122 C123 H123 120.2 . . ?
C122 C123 C124 119.51(17) . . ?
C124 C123 H123 120.2 . . ?
C123 C124 H124 119.2 . . ?
C123 C124 C125 121.50(18) . . ?
C125 C124 H124 119.2 . . ?
C120 C125 H125 120.3 . . ?
C124 C125 C120 119.44(17) . . ?
C124 C125 H125 120.3 . . ?
C131 C126 C127 120.16(17) . . ?
C131 C126 N108 125.02(16) . . ?
N108 C126 C127 114.82(16) . . ?
C128 C127 C126 118.11(18) . . ?
N109 C127 C126 120.53(18) . . ?
N109 C127 C128 121.31(17) . . ?
C127 C128 H128 119.6 . . ?
C129 C128 C127 120.88(18) . . ?
C129 C128 H128 119.6 . . ?
C128 C129 H129 119.5 . . ?
C128 C129 C130 120.98(19) . . ?
C130 C129 H129 119.5 . . ?
C129 C130 H130 120.3 . . ?
C131 C130 C129 119.32(19) . . ?
C131 C130 H130 120.3 . . ?
C126 C131 H131 119.7 . . ?
C130 C131 C126 120.54(17) . . ?
C130 C131 H131 119.7 . . ?
C101 N101 H10A 115(2) . . ?
C101 N101 H10B 112(2) . . ?
H10A N101 H10B 123(3) . . ?
N103 N102 C102 114.49(17) . . ?
N102 N103 C107 114.21(17) . . ?
C108 N104 H10C 113.9(16) . . ?
C113 N104 C108 129.21(18) . . ?
C113 N104 H10C 116.9(16) . . ?
C118 N105 C114 117.66(16) . . ?
C119 N106 C120 128.56(16) . . ?
C119 N106 H10D 115.4(15) . . ?
C120 N106 H10D 115.4(15) . . ?
N108 N107 C121 113.67(15) . . ?
N107 N108 C126 115.45(15) . . ?
C127 N109 H10E 112.6(16) . . ?
C127 N109 H10F 119.8(17) . . ?
H10E N109 H10F 115(2) . . ?
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 C2 1.412(3) . ?
C1 C6 1.418(3) . ?
C1 N1 1.346(3) . ?
C2 C3 1.403(3) . ?
C2 N2 1.414(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.377(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.379(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.372(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.405(2) . ?
C7 C12 1.398(3) . ?
C7 N3 1.421(2) . ?
C8 C9 1.399(3) . ?
C8 N4 1.403(2) . ?
C9 H9 0.9300 . ?
C9 C10 1.383(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.390(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.380(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.505(3) . ?
C13 N4 1.352(2) . ?
C13 O1 1.229(2) . ?
C14 C15 1.393(2) . ?
C14 N5 1.339(2) . ?
C15 H15 0.9300 . ?
C15 C16 1.384(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.383(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.395(3) . ?
C18 C19 1.506(3) . ?
C18 N5 1.342(2) . ?
C19 N6 1.356(2) . ?
C19 O2 1.225(2) . ?
C20 C21 1.407(3) . ?
C20 C25 1.394(3) . ?
C20 N6 1.401(2) . ?
C21 C22 1.395(2) . ?
C21 N7 1.419(2) . ?
C22 H22 0.9300 . ?
C22 C23 1.377(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.393(3) . ?
C24 H24 0.9300 . ?
C24 C25 1.388(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.414(2) . ?
C26 C31 1.400(3) . ?
C26 N8 1.408(2) . ?
C27 C28 1.405(3) . ?
C27 N9 1.369(2) . ?
C28 H28 0.9300 . ?
C28 C29 1.382(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.401(3) . ?
C30 H30 0.9300 . ?
C30 C31 1.371(3) . ?
C31 H31 0.9300 . ?
N1 H1A 0.943(18) . ?
N1 H1B 0.946(18) . ?
N2 N3 1.267(2) . ?
N4 H4A 0.86(2) . ?
N6 H6A 0.87(2) . ?
N7 N8 1.267(2) . ?
N9 H9A 0.87(3) . ?
N9 H9B 0.92(3) . ?
C101 C102 1.414(3) . ?
C101 C106 1.412(3) . ?
C101 N101 1.369(3) . ?
C102 C103 1.386(3) . ?
C102 N102 1.423(3) . ?
C103 H103 0.9300 . ?
C103 C104 1.381(3) . ?
C104 H104 0.9300 . ?
C104 C105 1.391(3) . ?
C105 H105 0.9300 . ?
C105 C106 1.370(4) . ?
C106 H106 0.9300 . ?
C107 C108 1.413(3) . ?
C107 C112 1.395(3) . ?
C107 N103 1.414(3) . ?
C108 C109 1.392(3) . ?
C108 N104 1.400(3) . ?
C109 H109 0.9300 . ?
C109 C110 1.388(3) . ?
C110 H110 0.9300 . ?
C110 C111 1.386(4) . ?
C111 H111 0.9300 . ?
C111 C112 1.380(3) . ?
C112 H112 0.9300 . ?
C113 C114 1.501(3) . ?
C113 N104 1.356(2) . ?
C113 O101 1.228(2) . ?
C114 C115 1.391(3) . ?
C114 N105 1.343(2) . ?
C115 H115 0.9300 . ?
C115 C116 1.380(3) . ?
C116 H116 0.9300 . ?
C116 C117 1.386(3) . ?
C117 H117 0.9300 . ?
C117 C118 1.393(2) . ?
C118 C119 1.511(3) . ?
C118 N105 1.334(2) . ?
C119 N106 1.357(2) . ?
C119 O102 1.226(2) . ?
C120 C121 1.410(2) . ?
C120 C125 1.400(3) . ?
C120 N106 1.403(2) . ?
C121 C122 1.395(3) . ?
C121 N107 1.420(2) . ?
C122 H122 0.9300 . ?
C122 C123 1.380(3) . ?
C123 H123 0.9300 . ?
C123 C124 1.384(3) . ?
C124 H124 0.9300 . ?
C124 C125 1.384(3) . ?
C125 H125 0.9300 . ?
C126 C127 1.414(2) . ?
C126 C131 1.401(3) . ?
C126 N108 1.410(2) . ?
C127 C128 1.403(3) . ?
C127 N109 1.380(3) . ?
C128 H128 0.9300 . ?
C128 C129 1.376(3) . ?
C129 H129 0.9300 . ?
C129 C130 1.394(3) . ?
C130 H130 0.9300 . ?
C130 C131 1.382(3) . ?
C131 H131 0.9300 . ?
N101 H10A 0.95(4) . ?
N101 H10B 0.97(4) . ?
N102 N103 1.268(2) . ?
N104 H10C 0.88(3) . ?
N106 H10D 0.87(2) . ?
N107 N108 1.266(2) . ?
N109 H10E 0.90(3) . ?
N109 H10F 0.90(3) . ?
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
N1 H1A O102 0.943(18) 2.46(3) 3.175(2) 132(3) 2_646 yes
N4 H4A N5 0.86(2) 2.22(2) 2.668(2) 111.8(18) . yes
N6 H6A N7 0.87(2) 2.19(2) 2.645(2) 111.8(18) . yes
N104 H10C N103 0.88(3) 2.22(2) 2.675(2) 112(2) . yes
N106 H10D N105 0.87(2) 2.24(2) 2.675(2) 111.1(18) . yes
N109 H10F O1 0.90(3) 2.11(3) 3.004(2) 176(2) . 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
C1 C2 C3 C4 0.6(3) . . . . ?
C1 C2 N2 N3 -171.27(15) . . . . ?
C2 C1 C6 C5 1.0(3) . . . . ?
C2 C3 C4 C5 0.3(3) . . . . ?
C2 N2 N3 C7 -176.09(14) . . . . ?
C3 C2 N2 N3 11.6(2) . . . . ?
C3 C4 C5 C6 -0.5(3) . . . . ?
C4 C5 C6 C1 -0.2(3) . . . . ?
C6 C1 C2 C3 -1.3(3) . . . . ?
C6 C1 C2 N2 -178.52(15) . . . . ?
C7 C8 C9 C10 1.4(3) . . . . ?
C7 C8 N4 C13 -161.12(17) . . . . ?
C8 C7 C12 C11 0.7(3) . . . . ?
C8 C7 N3 N2 -174.63(15) . . . . ?
C8 C9 C10 C11 -0.7(3) . . . . ?
C9 C8 N4 C13 19.7(3) . . . . ?
C9 C10 C11 C12 0.1(3) . . . . ?
C10 C11 C12 C7 -0.1(3) . . . . ?
C12 C7 C8 C9 -1.4(3) . . . . ?
C12 C7 C8 N4 179.42(16) . . . . ?
C12 C7 N3 N2 9.2(2) . . . . ?
C13 C14 C15 C16 179.25(17) . . . . ?
C13 C14 N5 C18 -177.33(15) . . . . ?
C14 C13 N4 C8 174.41(16) . . . . ?
C14 C15 C16 C17 -1.5(3) . . . . ?
C15 C14 N5 C18 1.2(3) . . . . ?
C15 C16 C17 C18 0.3(3) . . . . ?
C16 C17 C18 C19 -178.36(16) . . . . ?
C16 C17 C18 N5 1.7(3) . . . . ?
C17 C18 C19 N6 -159.25(16) . . . . ?
C17 C18 C19 O2 19.9(3) . . . . ?
C17 C18 N5 C14 -2.5(3) . . . . ?
C18 C19 N6 C20 172.36(17) . . . . ?
C19 C18 N5 C14 177.62(15) . . . . ?
C20 C21 C22 C23 -0.3(3) . . . . ?
C20 C21 N7 N8 -177.11(15) . . . . ?
C21 C20 C25 C24 0.5(3) . . . . ?
C21 C20 N6 C19 -168.71(17) . . . . ?
C21 C22 C23 C24 0.8(3) . . . . ?
C21 N7 N8 C26 -177.05(14) . . . . ?
C22 C21 N7 N8 5.5(2) . . . . ?
C22 C23 C24 C25 -0.7(3) . . . . ?
C23 C24 C25 C20 0.0(3) . . . . ?
C25 C20 C21 C22 -0.4(3) . . . . ?
C25 C20 C21 N7 -177.96(15) . . . . ?
C25 C20 N6 C19 10.9(3) . . . . ?
C26 C27 C28 C29 0.1(3) . . . . ?
C27 C26 C31 C30 0.6(3) . . . . ?
C27 C26 N8 N7 -174.92(15) . . . . ?
C27 C28 C29 C30 0.5(3) . . . . ?
C28 C29 C30 C31 -0.5(3) . . . . ?
C29 C30 C31 C26 -0.1(3) . . . . ?
C31 C26 C27 C28 -0.6(3) . . . . ?
C31 C26 C27 N9 178.36(17) . . . . ?
C31 C26 N8 N7 6.5(3) . . . . ?
N1 C1 C2 C3 -178.73(17) . . . . ?
N1 C1 C2 N2 4.0(3) . . . . ?
N1 C1 C6 C5 178.49(19) . . . . ?
N2 C2 C3 C4 177.56(17) . . . . ?
N3 C7 C8 C9 -177.69(15) . . . . ?
N3 C7 C8 N4 3.1(2) . . . . ?
N3 C7 C12 C11 176.71(17) . . . . ?
N4 C8 C9 C10 -179.47(17) . . . . ?
N4 C13 C14 C15 179.73(16) . . . . ?
N4 C13 C14 N5 -1.7(2) . . . . ?
N5 C14 C15 C16 0.7(3) . . . . ?
N5 C18 C19 N6 20.7(2) . . . . ?
N5 C18 C19 O2 -160.16(17) . . . . ?
N6 C20 C21 C22 179.19(16) . . . . ?
N6 C20 C21 N7 1.6(2) . . . . ?
N6 C20 C25 C24 -179.03(17) . . . . ?
N7 C21 C22 C23 177.02(17) . . . . ?
N8 C26 C27 C28 -179.27(15) . . . . ?
N8 C26 C27 N9 -0.3(2) . . . . ?
N8 C26 C31 C30 179.11(17) . . . . ?
N9 C27 C28 C29 -178.91(17) . . . . ?
O1 C13 C14 C15 -0.3(3) . . . . ?
O1 C13 C14 N5 178.27(16) . . . . ?
O1 C13 N4 C8 -5.5(3) . . . . ?
O2 C19 N6 C20 -6.7(3) . . . . ?
C101 C102 C103 C104 -0.5(3) . . . . ?
C101 C102 N102 N103 159.77(17) . . . . ?
C102 C101 C106 C105 -1.9(3) . . . . ?
C102 C103 C104 C105 -1.0(3) . . . . ?
C102 N102 N103 C107 176.05(15) . . . . ?
C103 C102 N102 N103 -21.2(3) . . . . ?
C103 C104 C105 C106 1.1(3) . . . . ?
C104 C105 C106 C101 0.4(3) . . . . ?
C106 C101 C102 C103 2.0(3) . . . . ?
C106 C101 C102 N102 -178.94(17) . . . . ?
C107 C108 C109 C110 -0.1(3) . . . . ?
C107 C108 N104 C113 -175.44(18) . . . . ?
C108 C107 C112 C111 1.0(3) . . . . ?
C108 C107 N103 N102 159.27(16) . . . . ?
C108 C109 C110 C111 1.2(3) . . . . ?
C109 C108 N104 C113 3.1(3) . . . . ?
C109 C110 C111 C112 -1.2(3) . . . . ?
C110 C111 C112 C107 0.1(3) . . . . ?
C112 C107 C108 C109 -0.9(3) . . . . ?
C112 C107 C108 N104 177.67(17) . . . . ?
C112 C107 N103 N102 -23.6(3) . . . . ?
C113 C114 C115 C116 -178.21(16) . . . . ?
C113 C114 N105 C118 178.38(15) . . . . ?
C114 C113 N104 C108 179.50(17) . . . . ?
C114 C115 C116 C117 -0.1(3) . . . . ?
C115 C114 N105 C118 -2.9(2) . . . . ?
C115 C116 C117 C118 -2.9(3) . . . . ?
C116 C117 C118 C119 -173.53(16) . . . . ?
C116 C117 C118 N105 3.2(3) . . . . ?
C117 C118 C119 N106 161.74(16) . . . . ?
C117 C118 C119 O102 -16.3(3) . . . . ?
C117 C118 N105 C114 -0.3(2) . . . . ?
C118 C119 N106 C120 -171.61(16) . . . . ?
C119 C118 N105 C114 176.50(15) . . . . ?
C120 C121 C122 C123 0.5(3) . . . . ?
C120 C121 N107 N108 -174.23(15) . . . . ?
C121 C120 C125 C124 -0.3(3) . . . . ?
C121 C120 N106 C119 163.37(17) . . . . ?
C121 C122 C123 C124 -0.3(3) . . . . ?
C121 N107 N108 C126 -178.90(14) . . . . ?
C122 C121 N107 N108 7.4(2) . . . . ?
C122 C123 C124 C125 -0.2(3) . . . . ?
C123 C124 C125 C120 0.5(3) . . . . ?
C125 C120 C121 C122 -0.2(3) . . . . ?
C125 C120 C121 N107 -178.63(15) . . . . ?
C125 C120 N106 C119 -16.2(3) . . . . ?
C126 C127 C128 C129 -0.1(3) . . . . ?
C127 C126 C131 C130 0.0(3) . . . . ?
C127 C126 N108 N107 174.70(15) . . . . ?
C127 C128 C129 C130 0.4(3) . . . . ?
C128 C129 C130 C131 -0.5(3) . . . . ?
C129 C130 C131 C126 0.3(3) . . . . ?
C131 C126 C127 C128 -0.1(3) . . . . ?
C131 C126 C127 N109 177.29(17) . . . . ?
C131 C126 N108 N107 -5.6(2) . . . . ?
N101 C101 C102 C103 -178.6(2) . . . . ?
N101 C101 C102 N102 0.5(3) . . . . ?
N101 C101 C106 C105 178.7(2) . . . . ?
N102 C102 C103 C104 -179.52(19) . . . . ?
N103 C107 C108 C109 176.26(16) . . . . ?
N103 C107 C108 N104 -5.1(2) . . . . ?
N103 C107 C112 C111 -176.04(17) . . . . ?
N104 C108 C109 C110 -178.62(18) . . . . ?
N104 C113 C114 C115 167.97(16) . . . . ?
N104 C113 C114 N105 -13.3(2) . . . . ?
N105 C114 C115 C116 3.1(3) . . . . ?
N105 C118 C119 N106 -15.2(2) . . . . ?
N105 C118 C119 O102 166.75(17) . . . . ?
N106 C120 C121 C122 -179.75(16) . . . . ?
N106 C120 C121 N107 1.8(2) . . . . ?
N106 C120 C125 C124 179.23(17) . . . . ?
N107 C121 C122 C123 178.81(16) . . . . ?
N108 C126 C127 C128 179.58(15) . . . . ?
N108 C126 C127 N109 -3.0(2) . . . . ?
N108 C126 C131 C130 -179.63(17) . . . . ?
N109 C127 C128 C129 -177.47(18) . . . . ?
O101 C113 C114 C115 -11.5(3) . . . . ?
O101 C113 C114 N105 167.19(17) . . . . ?
O101 C113 N104 C108 -1.0(3) . . . . ?
O102 C119 N106 C120 6.3(3) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.8321 7.3235 -7.1472 0.9339 -0.3298 0.1384
0.8321 -7.3235 7.1472 -0.9339 0.3298 -0.1384
-7.2610 -6.4041 1.8778 -0.0943 0.0294 0.9951
7.2802 5.9575 -1.4592 0.0402 -0.0103 -0.9991
6.3871 1.2453 2.3577 -0.4315 0.1556 -0.8886
1.0723 -24.8533 -0.3823 0.0250 0.9958 0.0878
-0.6882 25.0030 0.3221 -0.0251 -0.9899 -0.1392
-6.3891 -12.9481 0.9130 0.0111 0.3074 0.9515
0.7528 -18.3367 -5.4448 0.6811 0.7190 0.1381
-0.2445 18.5081 5.3034 -0.6733 -0.7104 -0.2051
-7.1959 3.8944 3.7815 -0.3388 -0.3626 0.8682
-7.4855 -0.1021 1.3808 -0.0255 -0.2233 0.9744
2.6242 -23.4106 -1.4283 0.1278 0.9849 -0.1170
4.3743 -20.3555 -1.6291 0.1184 0.9199 -0.3739
-0.1297 19.0467 -5.0176 0.6477 -0.7567 -0.0888
