#------------------------------------------------------------------------------
#$Date: 2024-04-05 00:40:10 +0200 (Fri 05 de Apr de 2024) $
#$Revision: 290832 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/12/1571239.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_1571239
loop_
_publ_author_name
'Suating, Paolo'
'Ewe, Marc B.'
'Kimberly, Lauren B.'
'Arman, Hadi D.'
'Wherritt, Daniel J.'
'Urbach, Adam R.'
_publ_section_title
;
 Peptide recognition by a synthetic receptor at subnanomolar
 concentrations
;
_journal_issue                   14
_journal_name_full               'Chemical Science'
_journal_page_first              5133
_journal_page_last               5142
_journal_paper_doi               10.1039/D4SC01122H
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H48 N32 O16, C21 H31 N5 O7, 18(H2 O), H O'
_chemical_formula_sum            'C69 H116 N37 O42'
_chemical_formula_weight         2135.98
_chemical_name_common            'H-YLGGG-OH Q8 complex hydrate'
_chemical_name_systematic
'L-tyrosyl-L-leucylglycylglycylglycine cucurbit[8]uril complex octadecahydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-22
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-12-08 deposited with the CCDC.	2024-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.2330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.11250(10)
_cell_length_b                   21.09440(10)
_cell_length_c                   18.85710(10)
_cell_measurement_reflns_used    80756
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.5650
_cell_measurement_theta_min      2.4460
_cell_volume                     4981.73(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (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_pressure         100
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -51.00 -19.00   0.50    0.36    --  -91.75  45.00-180.00   64
  2  ω    -51.00 -19.00   0.50    0.36    --  -91.75  45.00-150.00   64
  3  ω    -51.00 -19.00   0.50    0.36    --  -91.75  45.00-120.00   64
  4  ω    -51.00 -19.00   0.50    0.36    --  -91.75  45.00 -90.00   64
  5  ω    -51.00 -19.00   0.50    0.36    --  -91.75  45.00 -60.00   64
  6  ω    -51.00 -19.00   0.50    0.36    --  -91.75  45.00 -30.00   64
  7  ω    -51.00 -19.00   0.50    0.36    --  -91.75  45.00  30.00   64
  8  ω    -51.00 -19.00   0.50    0.36    --  -91.75  45.00  60.00   64
  9  ω    -51.00 -19.00   0.50    0.36    --  -91.75  45.00  90.00   64
 10  ω    -30.00  29.00   0.50    0.09    --  -46.89  19.00  30.00  118
 11  ω    -43.00  27.00   0.50    0.09    --  -46.89  37.00  60.00  140
 12  ω     27.00  88.00   0.50    0.09    --   46.89-115.00   4.00  122
 13  ω     34.00  94.00   0.50    0.09    --   46.89-125.00 120.00  120
 14  ω     37.00 112.00   0.50    0.36    --  106.92-125.00 -60.00  150
 15  ω     55.00 140.00   0.50    0.36    --  106.92-166.00-141.00  170
 16  ω     37.00 112.00   0.50    0.36    --  106.92-125.00-180.00  150
 17  ω     55.00 122.00   0.50    0.09    --   46.89-166.00-141.00  134
 18  ω     37.00 112.00   0.50    0.36    --  106.92-125.00 -30.00  150
 19  ω     38.00 109.00   0.50    0.36    --  106.92-115.00   4.00  142
 20  ω     37.00 112.00   0.50    0.36    --  106.92-125.00 120.00  150
 21  ω     36.00 106.00   0.50    0.36    --  106.92-102.00 129.76  140
 22  ω     37.00 112.00   0.50    0.36    --  106.92-125.00  30.00  150
 23  ω     34.00 106.00   0.50    0.36    --  106.92 -94.00  30.00  144
 24  ω     34.00 106.00   0.50    0.36    --  106.92 -94.00-180.00  144
 25  ω     34.00 101.00   0.50    0.36    --  106.92 -77.00-180.00  134
 26  ω     34.00  71.00   0.50    0.36    --  106.92 -61.00 -90.00   74
 27  ω     34.00 101.00   0.50    0.36    --  106.92 -77.00  30.00  134
 28  ω     34.00  71.00   0.50    0.36    --  106.92 -61.00  90.00   74
 29  ω     83.00 119.00   0.50    0.09    --   46.89  57.00  60.00   72
 30  ω     69.00 154.00   0.50    0.36    --  106.92 166.00-119.00  170
 31  ω    101.00 178.00   0.50    0.36    --  106.92  77.00-180.00  154
 32  ω     69.00 119.00   0.50    0.09    --   46.89 166.00-119.00  100
 33  ω    101.00 176.00   0.50    0.36    --  106.92 115.00  94.00  150
 34  ω    -83.00 -23.00   0.50    0.36    --  -91.75 115.00  94.00  120
 35  ω    -82.00  -6.00   0.50    0.09    --  -46.89 115.00  94.00  152
 36  ω   -114.00 -33.00   0.50    0.09    --  -46.89 166.00-119.00  162
 37  ω   -114.00 -33.00   0.50    0.36    --  -91.75 166.00-119.00  162
 38  ω   -119.00 -31.00   0.50    0.09    --  -46.89 -53.00 -44.10  176
 39  ω   -119.00 -83.00   0.50    0.09    --  -46.89 -57.00 -90.00   72
 40  ω   -119.00 -83.00   0.50    0.09    --  -46.89 -57.00-120.00   72
 41  ω   -119.00 -83.00   0.50    0.09    --  -46.89 -57.00  90.00   72
 42  ω   -119.00 -83.00   0.50    0.09    --  -46.89 -57.00 120.00   72
 43  ω   -119.00 -83.00   0.50    0.09    --  -46.89 -57.00 150.00   72
 44  ω   -167.00 -74.00   0.50    0.36    --  -91.75 -15.00  60.00  186
 45  ω   -164.00 -77.00   0.50    0.36    --  -91.75 -48.00  17.13  174
 46  ω   -164.00 -91.00   0.50    0.36    --  -91.75 -61.00 -60.00  146
 47  ω   -164.00 -91.00   0.50    0.36    --  -91.75 -61.00 -90.00  146
 48  ω   -164.00 -77.00   0.50    0.36    --  -91.75 -50.00-153.28  174
 49  ω   -164.00-100.00   0.50    0.36    --  -91.75 -94.00 -30.00  128
 50  ω   -161.00 -80.00   0.50    0.36    --  -91.75-115.00   4.00  162
 51  ω   -119.00 -47.00   0.50    0.09    --  -46.89-166.00-141.00  144
 52  ω   -137.00 -47.00   0.50    0.36    --  -91.75-166.00-141.00  180
;
_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      0.0609446000
_diffrn_orient_matrix_UB_12      0.0465715000
_diffrn_orient_matrix_UB_13      0.0607833000
_diffrn_orient_matrix_UB_21      -0.0690658000
_diffrn_orient_matrix_UB_22      0.0550065000
_diffrn_orient_matrix_UB_23      -0.0421976000
_diffrn_orient_matrix_UB_31      -0.0816160000
_diffrn_orient_matrix_UB_32      -0.0118094000
_diffrn_orient_matrix_UB_33      0.0428473000
_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  0.0504
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            112702
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.955
_diffrn_reflns_theta_min         2.453
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       plate
_exptl_crystal_F_000             2250
_exptl_crystal_recrystallization_method
'phosphate-buffered D2O; heating and cooling cycles'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.14(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1401
_refine_ls_number_reflns         20089
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0552P)²+2.5221P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.900
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.929
_reflns_number_gt                19374
_reflns_number_total             20089
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc01122h2.cif
_cod_data_source_block           hpd814c
_cod_depositor_comments
'Adding full bibliography for 1571239--1571240.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1571239
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O'
_chemical_oxdiff_usercomment     'Trinity H-YLGGG-OH/08 PO4 buffer D2O'
_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_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.792
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.86(10)
 0.14(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 HE-O31
 0.95 with sigma of 0.02
4.a Free rotating group:
 O30(H,HA), O24(HB,HC), O31(HD,HE), O32(HG,HH), O36(HI,HJ), O37(HK,HL), O28(HM,
 HN), O38(HO,HP), O49(HQ,HR), O26(HS,HT), O35(HU,HV), O40(HW,HX), O39(HY,HZ),
 O25(H1,H4), O50(H5,H6), O27(H10,H11), O33(H12,H13), O34(H22,H23), O29(H24)
4.b Ternary CH refined with riding coordinates:
 C39(H39), C8(H8), C9(H9), C3(H3), C14(H14), C32(H32), C62(H25), C26(H26),
 C44(H44), C45(H45), C33(H33), C2(H2), C27(H27), C58(H30), C56(H31), C15(H15),
 C21(H21), C38(H38), C20(H20)
4.c Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C12(H12A,H12B), C17(H17A,H17B), C36(H36A,H36B), C23(H23A,
 H23B), C57(H28,H29), C18(H18A,H18B), C6(H6A,H6B), C41(H41A,H41B), C42(H42A,
 H42B), C29(H29A,H29B), C24(H24A,H24B), C35(H35A,H35B), C30(H30A,H30B),
 C11(H11A,H11B), C63(H35,H36), C5(H5A,H5B), C48(H48A,H48B), C52(H40,H41),
 C54(H43,H46), C50(H47,H48)
4.d Aromatic/amide H refined with riding coordinates:
 N34(H7), N33(H19), C68(H34), C69(H37), C65(H42), C66(H49)
4.e Idealised Me refined as rotating group:
 N37(H16,H17,H18), C60(H50,H51,H52), C59(H53,H54,H55)
4.f Idealised tetrahedral OH refined as rotating group:
 O23(HF)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method 'nylon loop'
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.366
_oxdiff_exptl_absorpt_empirical_full_min 0.621
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
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
O16 O 0.65819(16) 0.99023(10) 1.00124(11) 0.0173(4) Uani 1 1 d . . . . .
O1 O 0.22011(16) 0.76154(10) 0.91948(11) 0.0168(4) Uani 1 1 d . . . . .
O14 O 0.90233(16) 0.96514(10) 1.14863(11) 0.0165(4) Uani 1 1 d . . . . .
O12 O 1.04044(17) 0.85379(10) 1.09981(12) 0.0187(4) Uani 1 1 d . . . . .
O4 O 0.42284(16) 0.84232(10) 0.59879(12) 0.0201(4) Uani 1 1 d . . . . .
O2 O 0.46445(17) 0.94492(10) 0.77614(11) 0.0187(4) Uani 1 1 d . . . . .
O10 O 0.98659(16) 0.75221(10) 0.91331(12) 0.0202(4) Uani 1 1 d . . . . .
O5 O 0.41567(16) 0.52458(10) 0.70716(11) 0.0190(4) Uani 1 1 d . . . . .
O15 O 0.37306(16) 0.81499(10) 1.12588(12) 0.0192(4) Uani 1 1 d . . . . .
O6 O 0.59331(17) 0.73722(10) 0.56147(12) 0.0198(4) Uani 1 1 d . . . . .
O9 O 0.82051(16) 0.52415(10) 1.02583(11) 0.0181(4) Uani 1 1 d . . . . .
O7 O 0.66585(16) 0.46685(11) 0.81458(12) 0.0203(4) Uani 1 1 d . . . . .
O8 O 0.83902(17) 0.70235(10) 0.69884(12) 0.0194(4) Uani 1 1 d . . . . .
O11 O 0.82329(17) 0.63224(10) 1.21024(12) 0.0208(4) Uani 1 1 d . . . . .
O3 O 0.21699(16) 0.64048(10) 0.74858(11) 0.0163(4) Uani 1 1 d . . . . .
O22 O 0.34196(17) 0.37758(11) 0.11530(12) 0.0234(5) Uani 1 1 d . . . . .
O13 O 0.64418(17) 0.75577(10) 1.23481(12) 0.0206(4) Uani 1 1 d . . . . .
O21 O 0.19461(17) 0.37581(11) 0.24250(12) 0.0233(5) Uani 1 1 d . . . . .
O30 O 0.24927(19) 0.48454(12) 0.52017(14) 0.0270(5) Uani 1 1 d G . . . .
H H 0.289533 0.482596 0.490997 0.040 Uiso 1 1 d G U . . .
HA H 0.186436 0.494565 0.491076 0.040 Uiso 1 1 d G U . . .
O24 O 0.26990(18) 0.63475(10) 0.90438(12) 0.0218(4) Uani 1 1 d G . . . .
HB H 0.248705 0.672385 0.912750 0.033 Uiso 1 1 d G U . . .
HC H 0.268265 0.635546 0.857956 0.033 Uiso 1 1 d G U . . .
O31 O -0.01650(17) 0.36473(11) 0.15815(13) 0.0237(5) Uani 1 1 d DG . . . .
HD H 0.042685 0.371833 0.193166 0.036 Uiso 1 1 d G U . . .
HE H -0.030429 0.342018 0.128267 0.036 Uiso 1 1 d DG U . . .
O23 O 0.51860(18) 0.10769(10) 0.02157(13) 0.0243(5) Uani 1 1 d . . . . .
HF H 0.582822 0.117908 0.040665 0.036 Uiso 1 1 calc R U . . .
O18 O 0.76371(18) 0.66427(11) 0.42365(13) 0.0250(5) Uani 1 1 d . . . . .
O32 O 0.06152(19) 0.46319(11) 0.08943(13) 0.0249(5) Uani 1 1 d G . . . .
HG H 0.123348 0.466956 0.122808 0.037 Uiso 1 1 d G U . . .
HH H 0.026040 0.437324 0.109163 0.037 Uiso 1 1 d G U . . .
O36 O 0.60306(19) 0.60914(12) 0.18844(13) 0.0260(5) Uani 1 1 d G . . . .
HI H 0.663278 0.628606 0.193451 0.039 Uiso 1 1 d G U . . .
HJ H 0.555409 0.639135 0.178514 0.039 Uiso 1 1 d G U . . .
O37 O 0.4163(2) 0.68546(12) 0.15452(14) 0.0298(5) Uani 1 1 d G . . . .
HK H 0.413217 0.724287 0.138360 0.045 Uiso 1 1 d G U . . .
HL H 0.387441 0.687127 0.190484 0.045 Uiso 1 1 d G U . . .
O28 O 0.52809(18) 0.80647(12) 0.43102(13) 0.0258(5) Uani 1 1 d G . . . .
HM H 0.545642 0.776703 0.405001 0.039 Uiso 1 1 d G U . . .
HN H 0.539990 0.790163 0.475131 0.039 Uiso 1 1 d G U . . .
O17 O 0.92557(18) 0.62104(11) 0.44654(13) 0.0258(5) Uani 1 1 d . . . . .
O20 O 0.37620(19) 0.50051(12) 0.43204(13) 0.0278(5) Uani 1 1 d . . . . .
O19 O 0.6391(2) 0.51868(13) 0.43694(13) 0.0295(5) Uani 1 1 d . . . . .
O38 O 0.3028(2) 0.37416(12) 0.59493(13) 0.0293(5) Uani 1 1 d G . . . .
HO H 0.288534 0.419775 0.571956 0.044 Uiso 1 1 d G U . . .
HP H 0.355236 0.356706 0.584768 0.044 Uiso 1 1 d G U . . .
O49 O 0.56603(18) 0.70740(12) 0.34572(13) 0.0271(5) Uani 1 1 d G . . . .
HQ H 0.624464 0.687816 0.369766 0.041 Uiso 1 1 d G U . . .
HR H 0.578872 0.721879 0.306022 0.041 Uiso 1 1 d G U . . .
O26 O 0.99672(19) 0.66842(13) 0.58835(14) 0.0327(5) Uani 1 1 d G . . . .
HS H 0.972024 0.660442 0.541080 0.049 Uiso 1 1 d G U . . .
HT H 0.959830 0.700820 0.595267 0.049 Uiso 1 1 d G U . . .
O35 O 0.29177(19) 0.59141(12) 0.07818(15) 0.0292(5) Uani 1 1 d G . . . .
HU H 0.333135 0.622413 0.099750 0.044 Uiso 1 1 d G U . . .
HV H 0.323048 0.569644 0.051347 0.044 Uiso 1 1 d G U . . .
N26 N 0.66344(19) 0.86455(12) 1.23689(13) 0.0151(5) Uani 1 1 d . . . . .
N10 N 0.51982(19) 0.53888(12) 0.62840(13) 0.0169(5) Uani 1 1 d . . . . .
O40 O 0.1584(2) 0.28409(13) 0.53190(14) 0.0342(6) Uani 1 1 d G . . . .
HW H 0.179644 0.248596 0.543302 0.051 Uiso 1 1 d G U . . .
HX H 0.212555 0.314564 0.552380 0.051 Uiso 1 1 d G U . . .
N7 N 0.28526(19) 0.82386(12) 0.64983(13) 0.0156(5) Uani 1 1 d . . . . .
N2 N 0.26789(19) 0.86648(12) 0.92005(13) 0.0154(5) Uani 1 1 d . . . . .
N5 N 0.19814(19) 0.74437(12) 0.70666(13) 0.0152(5) Uani 1 1 d . . . . .
N32 N 0.48412(19) 0.96000(12) 0.99199(13) 0.0157(5) Uani 1 1 d . . . . .
N6 N 0.24755(19) 0.67125(12) 0.63884(13) 0.0155(5) Uani 1 1 d . . . . .
O39 O 0.0880(2) 0.29492(13) 0.37995(14) 0.0338(6) Uani 1 1 d G . . . .
HY H 0.125544 0.292652 0.426453 0.051 Uiso 1 1 d G U . . .
HZ H 0.121240 0.275007 0.352879 0.051 Uiso 1 1 d G U . . .
N16 N 0.88769(19) 0.61381(12) 0.77364(13) 0.0167(5) Uani 1 1 d . . . . .
O25 O 1.0351(2) 0.56354(13) 0.67664(14) 0.0310(5) Uani 1 1 d G . . . .
H1 H 1.014833 0.595520 0.646600 0.046 Uiso 1 1 d G U . . .
H4 H 1.097216 0.574721 0.705836 0.046 Uiso 1 1 d G U . . .
O50 O 1.0301(2) 0.50383(13) 0.46270(15) 0.0327(5) Uani 1 1 d G . . . .
H5 H 1.004421 0.490383 0.497537 0.049 Uiso 1 1 d G U . . .
H6 H 1.003208 0.533820 0.453338 0.049 Uiso 1 1 d G U . . .
N18 N 0.95820(19) 0.59726(12) 1.05631(13) 0.0161(5) Uani 1 1 d . . . . .
N27 N 0.91582(19) 0.89323(12) 1.24340(14) 0.0164(5) Uani 1 1 d . . . . .
N36 N 0.23582(19) 0.29838(12) 0.13501(13) 0.0157(5) Uani 1 1 d . . . . .
N15 N 0.77023(19) 0.60249(12) 0.66176(13) 0.0157(5) Uani 1 1 d . . . . .
N35 N 0.3561(2) 0.35589(12) 0.32295(14) 0.0169(5) Uani 1 1 d . . . . .
N29 N 0.49764(19) 0.89614(11) 1.14940(13) 0.0146(5) Uani 1 1 d . . . . .
N31 N 0.60244(19) 0.97246(12) 1.10424(13) 0.0148(5) Uani 1 1 d . . . . .
N1 N 0.22240(18) 0.81475(12) 0.81195(13) 0.0150(5) Uani 1 1 d . . . . .
N34 N 0.4387(2) 0.47809(12) 0.33519(14) 0.0187(5) Uani 1 1 d . . . . .
H7 H 0.444498 0.449138 0.302990 0.022 Uiso 1 1 calc R U . . .
O27 O 0.9819(2) 0.45847(13) 0.58628(15) 0.0326(5) Uani 1 1 d G . . . .
H10 H 0.912946 0.457802 0.577606 0.049 Uiso 1 1 d G U . . .
H11 H 1.003504 0.489311 0.617760 0.049 Uiso 1 1 d G U . . .
O33 O 0.2688(2) 0.49377(13) 0.16909(15) 0.0339(5) Uani 1 1 d G . . . .
H12 H 0.285182 0.528448 0.150040 0.051 Uiso 1 1 d G U . . .
H13 H 0.310689 0.465118 0.159474 0.051 Uiso 1 1 d G U . . .
N8 N 0.32123(19) 0.75131(12) 0.57506(13) 0.0160(5) Uani 1 1 d . . . . .
N19 N 0.98361(19) 0.64322(12) 0.89982(13) 0.0164(5) Uani 1 1 d . . . . .
N30 N 0.36658(19) 0.89712(12) 1.04407(13) 0.0153(5) Uani 1 1 d . . . . .
N23 N 1.0480(2) 0.74494(12) 1.12157(14) 0.0177(5) Uani 1 1 d . . . . .
N9 N 0.37491(19) 0.59888(12) 0.61234(13) 0.0153(5) Uani 1 1 d . . . . .
N24 N 1.01510(19) 0.80980(12) 1.20573(14) 0.0160(5) Uani 1 1 d . . . . .
N28 N 0.76637(19) 0.94850(12) 1.20104(13) 0.0156(5) Uani 1 1 d . . . . .
N37 N 0.1606(2) 0.41165(12) -0.00324(14) 0.0171(5) Uani 1 1 d . . . . .
H16 H 0.119595 0.415446 -0.051304 0.021 Uiso 1 1 calc R U . . .
H17 H 0.218841 0.437184 0.004838 0.021 Uiso 1 1 calc R U . . .
H18 H 0.121795 0.423306 0.027448 0.021 Uiso 1 1 calc R U . . .
N20 N 1.0442(2) 0.68413(12) 1.01264(14) 0.0175(5) Uani 1 1 d . . . . .
N3 N 0.37726(19) 0.93333(12) 0.86655(13) 0.0168(5) Uani 1 1 d . . . . .
N14 N 0.82245(19) 0.51865(12) 0.81922(13) 0.0165(5) Uani 1 1 d . . . . .
N33 N 0.6679(2) 0.56220(13) 0.33458(15) 0.0223(5) Uani 1 1 d . . . . .
H19 H 0.638687 0.576143 0.289098 0.027 Uiso 1 1 calc R U . . .
N13 N 0.69525(19) 0.51238(12) 0.71108(13) 0.0167(5) Uani 1 1 d . . . . .
N12 N 0.59548(19) 0.62860(12) 0.57998(14) 0.0172(5) Uani 1 1 d . . . . .
N21 N 0.96779(19) 0.65644(12) 1.16859(14) 0.0177(5) Uani 1 1 d . . . . .
N25 N 0.80943(19) 0.80492(12) 1.26784(13) 0.0169(5) Uani 1 1 d . . . . .
N17 N 0.91863(19) 0.54950(12) 0.94602(13) 0.0161(5) Uani 1 1 d . . . . .
N11 N 0.43929(19) 0.67724(12) 0.53981(14) 0.0163(5) Uani 1 1 d . . . . .
N4 N 0.2994(2) 0.89646(12) 0.75223(13) 0.0183(5) Uani 1 1 d . . . . .
N22 N 0.9260(2) 0.72257(12) 1.24698(14) 0.0183(5) Uani 1 1 d . . . . .
O34 O 1.0114(3) 0.42303(15) 0.34013(17) 0.0483(8) Uani 1 1 d G . . . .
H22 H 1.007494 0.441233 0.380680 0.072 Uiso 1 1 d G U . . .
H23 H 1.031887 0.384473 0.353591 0.072 Uiso 1 1 d G U . . .
C7 C 0.2212(2) 0.68134(14) 0.70275(15) 0.0145(5) Uani 1 1 d . . . . .
C40 C 0.8645(2) 0.93805(13) 1.19311(15) 0.0144(5) Uani 1 1 d . . . . .
C43 C 0.4094(2) 0.86424(13) 1.10816(15) 0.0141(5) Uani 1 1 d . . . . .
C46 C 0.5884(2) 0.97588(13) 1.02916(16) 0.0148(5) Uani 1 1 d . . . . .
C61 C 0.2653(2) 0.34142(14) 0.09312(17) 0.0163(5) Uani 1 1 d . . . . .
C1 C 0.2359(2) 0.80919(14) 0.88713(15) 0.0141(5) Uani 1 1 d . . . . .
C28 C 1.0041(2) 0.69853(14) 0.93974(16) 0.0154(5) Uani 1 1 d . . . . .
C4 C 0.3897(2) 0.92703(14) 0.79622(15) 0.0158(5) Uani 1 1 d . . . . .
C34 C 1.0356(2) 0.80770(14) 1.13864(16) 0.0161(5) Uani 1 1 d . . . . .
C39 C 0.8502(2) 0.86896(13) 1.28719(15) 0.0148(5) Uani 1 1 d . . . . .
H39 H 0.886148 0.873532 1.341675 0.018 Uiso 1 1 calc R U . . .
C47 C 0.2632(2) 0.88134(14) 0.99368(15) 0.0159(5) Uani 1 1 d . . . . .
H47A H 0.233729 0.844485 1.013575 0.019 Uiso 1 1 calc R U . . .
H47B H 0.214064 0.917538 0.990768 0.019 Uiso 1 1 calc R U . . .
C10 C 0.3514(2) 0.80960(14) 0.60754(15) 0.0161(5) Uani 1 1 d . . . . .
C19 C 0.7214(2) 0.49625(14) 0.78509(16) 0.0153(5) Uani 1 1 d . . . . .
C13 C 0.4350(2) 0.55120(14) 0.65513(16) 0.0163(5) Uani 1 1 d . . . . .
C8 C 0.2272(2) 0.72630(14) 0.59117(15) 0.0150(5) Uani 1 1 d . . . . .
H8 H 0.167253 0.718854 0.544803 0.018 Uiso 1 1 calc R U . . .
C12 C 0.3623(2) 0.72723(14) 0.51694(16) 0.0170(5) Uani 1 1 d . . . . .
H12A H 0.301620 0.711464 0.475764 0.020 Uiso 1 1 calc R U . . .
H12B H 0.395485 0.762700 0.497428 0.020 Uiso 1 1 calc R U . . .
C9 C 0.1995(2) 0.77846(14) 0.64014(15) 0.0153(5) Uani 1 1 d . . . . .
H9 H 0.128493 0.798132 0.615183 0.018 Uiso 1 1 calc R U . . .
C17 C 0.5978(2) 0.49013(14) 0.65804(16) 0.0160(5) Uani 1 1 d . . . . .
H17A H 0.616110 0.469366 0.616348 0.019 Uiso 1 1 calc R U . . .
H17B H 0.565067 0.457641 0.682354 0.019 Uiso 1 1 calc R U . . .
C37 C 0.6997(2) 0.80357(14) 1.24514(15) 0.0161(5) Uani 1 1 d . . . . .
C51 C 0.6049(3) 0.53932(15) 0.37290(17) 0.0216(6) Uani 1 1 d . . . . .
C25 C 0.8915(2) 0.55330(14) 1.01140(16) 0.0158(5) Uani 1 1 d . . . . .
C3 C 0.2700(2) 0.91528(13) 0.86671(15) 0.0151(5) Uani 1 1 d . . . . .
H3 H 0.226316 0.952959 0.871602 0.018 Uiso 1 1 calc R U . . .
C31 C 0.8974(2) 0.66667(14) 1.20858(16) 0.0168(5) Uani 1 1 d . . . . .
C36 C 1.0197(2) 0.86861(14) 1.24638(16) 0.0159(5) Uani 1 1 d . . . . .
H36A H 1.061016 0.861480 1.298934 0.019 Uiso 1 1 calc R U . . .
H36B H 1.058223 0.900697 1.225809 0.019 Uiso 1 1 calc R U . . .
C49 C 0.8252(2) 0.62149(15) 0.41599(17) 0.0203(6) Uani 1 1 d . . . . .
C14 C 0.5185(2) 0.57684(13) 0.56451(15) 0.0145(5) Uani 1 1 d . . . . .
H14 H 0.523646 0.550243 0.521797 0.017 Uiso 1 1 calc R U . . .
C64 C 0.3254(2) 0.26859(14) -0.02677(16) 0.0174(6) Uani 1 1 d . . . . .
C22 C 0.8322(2) 0.64545(14) 0.70990(15) 0.0150(5) Uani 1 1 d . . . . .
C16 C 0.5473(2) 0.68641(14) 0.56130(15) 0.0161(5) Uani 1 1 d . . . . .
C32 C 1.0246(2) 0.74811(14) 1.24078(16) 0.0166(5) Uani 1 1 d . . . . .
H32 H 1.081726 0.747685 1.289605 0.020 Uiso 1 1 calc R U . . .
C67 C 0.4574(2) 0.16101(15) 0.00524(16) 0.0194(6) Uani 1 1 d . . . . .
O29 O 0.7681(3) 0.4399(2) 0.53817(18) 0.0598(10) Uani 1 1 d G . . . .
H24 H 0.727984 0.453093 0.495292 0.090 Uiso 1 1 d G U . . .
C23 C 0.8822(2) 0.49817(14) 0.89329(15) 0.0154(5) Uani 1 1 d . . . . .
H23A H 0.945041 0.473607 0.890169 0.018 Uiso 1 1 calc R U . . .
H23B H 0.836678 0.469406 0.912326 0.018 Uiso 1 1 calc R U . . .
C62 C 0.1958(2) 0.34439(14) 0.01204(16) 0.0165(6) Uani 1 1 d . . . . .
H25 H 0.132234 0.316171 0.004562 0.020 Uiso 1 1 calc R U . . .
C26 C 1.0435(2) 0.61650(14) 1.02697(16) 0.0163(5) Uani 1 1 d . . . . .
H26 H 1.114792 0.600658 1.057754 0.020 Uiso 1 1 calc R U . . .
C57 C 0.4081(2) 0.26530(14) 0.22677(16) 0.0175(6) Uani 1 1 d . . . . .
H28 H 0.451296 0.301313 0.218046 0.021 Uiso 1 1 calc R U . . .
H29 H 0.437462 0.252579 0.279444 0.021 Uiso 1 1 calc R U . . .
C18 C 0.7075(2) 0.61921(15) 0.58704(16) 0.0173(6) Uani 1 1 d . . . . .
H18A H 0.736630 0.658625 0.572106 0.021 Uiso 1 1 calc R U . . .
H18B H 0.714345 0.585155 0.552617 0.021 Uiso 1 1 calc R U . . .
C55 C 0.2773(2) 0.34460(14) 0.26010(16) 0.0158(5) Uani 1 1 d . . . . .
C6 C 0.2768(2) 0.88896(14) 0.67314(16) 0.0180(6) Uani 1 1 d . . . . .
H6A H 0.326927 0.915710 0.656046 0.022 Uiso 1 1 calc R U . . .
H6B H 0.203608 0.904545 0.648560 0.022 Uiso 1 1 calc R U . . .
C44 C 0.4191(2) 0.95763(13) 1.04341(15) 0.0140(5) Uani 1 1 d . . . . .
H44 H 0.368083 0.993996 1.035999 0.017 Uiso 1 1 calc R U . . .
C41 C 0.5523(2) 0.87953(14) 1.22563(16) 0.0165(5) Uani 1 1 d . . . . .
H41A H 0.547143 0.915380 1.258268 0.020 Uiso 1 1 calc R U . . .
H41B H 0.516452 0.842509 1.240015 0.020 Uiso 1 1 calc R U . . .
C42 C 0.6958(2) 0.99702(13) 1.15924(15) 0.0149(5) Uani 1 1 d . . . . .
H42A H 0.672351 1.024224 1.194246 0.018 Uiso 1 1 calc R U . . .
H42B H 0.736228 1.024010 1.134027 0.018 Uiso 1 1 calc R U . . .
C29 C 0.9768(3) 0.59482(14) 1.13657(16) 0.0180(6) Uani 1 1 d . . . . .
H29A H 0.924479 0.565500 1.147558 0.022 Uiso 1 1 calc R U . . .
H29B H 1.049076 0.577573 1.160344 0.022 Uiso 1 1 calc R U . . .
C45 C 0.5036(2) 0.95930(13) 1.12071(16) 0.0145(5) Uani 1 1 d . . . . .
H45 H 0.486918 0.992595 1.153381 0.017 Uiso 1 1 calc R U . . .
C24 C 0.9829(2) 0.64151(15) 0.82295(16) 0.0180(6) Uani 1 1 d . . . . .
H24A H 0.990406 0.685315 0.806321 0.022 Uiso 1 1 calc R U . . .
H24B H 1.045595 0.617001 0.819375 0.022 Uiso 1 1 calc R U . . .
C33 C 1.0521(2) 0.70335(14) 1.18389(16) 0.0170(6) Uani 1 1 d . . . . .
H33 H 1.124137 0.683614 1.204547 0.020 Uiso 1 1 calc R U . . .
C2 C 0.2241(2) 0.88167(14) 0.79117(15) 0.0160(5) Uani 1 1 d . . . . .
H2 H 0.150981 0.897493 0.764166 0.019 Uiso 1 1 calc R U . . .
C35 C 0.8708(2) 0.74805(14) 1.29611(16) 0.0180(6) Uani 1 1 d . . . . .
H35A H 0.923684 0.758005 1.344399 0.022 Uiso 1 1 calc R U . . .
H35B H 0.821967 0.715275 1.305030 0.022 Uiso 1 1 calc R U . . .
C27 C 1.0098(2) 0.58778(14) 0.94740(16) 0.0157(5) Uani 1 1 d . . . . .
H27 H 1.068347 0.562194 0.937569 0.019 Uiso 1 1 calc R U . . .
C58 C 0.4198(2) 0.20969(14) 0.17752(16) 0.0172(6) Uani 1 1 d . . . . .
H30 H 0.397183 0.224359 0.124720 0.021 Uiso 1 1 calc R U . . .
C56 C 0.2923(2) 0.28773(14) 0.21320(15) 0.0154(5) Uani 1 1 d . . . . .
H31 H 0.254451 0.251580 0.228783 0.018 Uiso 1 1 calc R U . . .
C68 C 0.5019(2) 0.22142(15) 0.00886(17) 0.0199(6) Uani 1 1 d . . . . .
H34 H 0.577164 0.226304 0.021597 0.024 Uiso 1 1 calc R U . . .
C15 C 0.4099(2) 0.61199(13) 0.54716(15) 0.0140(5) Uani 1 1 d . . . . .
H15 H 0.357606 0.595927 0.500560 0.017 Uiso 1 1 calc R U . . .
C21 C 0.7851(2) 0.53800(14) 0.69020(15) 0.0148(5) Uani 1 1 d . . . . .
H21 H 0.809009 0.508794 0.656481 0.018 Uiso 1 1 calc R U . . .
C30 C 1.1019(2) 0.72968(14) 1.06748(16) 0.0177(6) Uani 1 1 d . . . . .
H30A H 1.173386 0.712351 1.093394 0.021 Uiso 1 1 calc R U . . .
H30B H 1.112124 0.769042 1.041821 0.021 Uiso 1 1 calc R U . . .
C38 C 0.7477(2) 0.91065(14) 1.26084(15) 0.0148(5) Uani 1 1 d . . . . .
H38 H 0.738191 0.937882 1.301834 0.018 Uiso 1 1 calc R U . . .
C20 C 0.8718(2) 0.54601(14) 0.76662(15) 0.0150(5) Uani 1 1 d . . . . .
H20 H 0.939270 0.523425 0.767730 0.018 Uiso 1 1 calc R U . . .
C11 C 0.2651(2) 0.60875(13) 0.61262(16) 0.0143(5) Uani 1 1 d . . . . .
H11A H 0.216932 0.602825 0.561610 0.017 Uiso 1 1 calc R U . . .
H11B H 0.246600 0.576373 0.644750 0.017 Uiso 1 1 calc R U . . .
C53 C 0.3878(2) 0.46334(15) 0.38399(17) 0.0186(6) Uani 1 1 d . . . . .
C63 C 0.2565(2) 0.32719(14) -0.04426(16) 0.0186(6) Uani 1 1 d . . . . .
H35 H 0.203534 0.321481 -0.093622 0.022 Uiso 1 1 calc R U . . .
H36 H 0.302344 0.363560 -0.048001 0.022 Uiso 1 1 calc R U . . .
C69 C 0.4362(2) 0.27445(14) -0.00614(17) 0.0189(6) Uani 1 1 d . . . . .
H37 H 0.467335 0.315454 -0.002279 0.023 Uiso 1 1 calc R U . . .
C5 C 0.1523(2) 0.77051(14) 0.76147(16) 0.0150(5) Uani 1 1 d . . . . .
H5A H 0.134875 0.735325 0.790626 0.018 Uiso 1 1 calc R U . . .
H5B H 0.084839 0.792422 0.735520 0.018 Uiso 1 1 calc R U . . .
C48 C 0.4371(2) 0.98206(14) 0.91588(16) 0.0170(6) Uani 1 1 d . . . . .
H48A H 0.388959 1.018164 0.916156 0.020 Uiso 1 1 calc R U . . .
H48B H 0.494738 0.997635 0.896362 0.020 Uiso 1 1 calc R U . . .
C52 C 0.4854(3) 0.54011(15) 0.33272(18) 0.0231(6) Uani 1 1 d . . . . .
H40 H 0.450014 0.571671 0.356366 0.028 Uiso 1 1 calc R U . . .
H41 H 0.473509 0.552858 0.280366 0.028 Uiso 1 1 calc R U . . .
C65 C 0.2813(2) 0.20784(15) -0.03201(16) 0.0196(6) Uani 1 1 d . . . . .
H42 H 0.205946 0.202905 -0.046773 0.024 Uiso 1 1 calc R U . . .
C54 C 0.3414(2) 0.39733(15) 0.38061(16) 0.0188(6) Uani 1 1 d . . . . .
H43 H 0.373496 0.376574 0.429197 0.023 Uiso 1 1 calc R U . . .
H46 H 0.263796 0.401331 0.373719 0.023 Uiso 1 1 calc R U . . .
C50 C 0.7821(3) 0.56462(16) 0.36571(19) 0.0231(6) Uani 1 1 d . . . . .
H47 H 0.814447 0.564961 0.324463 0.028 Uiso 1 1 calc R U . . .
H48 H 0.805971 0.525366 0.394646 0.028 Uiso 1 1 calc R U . . .
C66 C 0.3463(3) 0.15461(15) -0.01592(17) 0.0219(6) Uani 1 1 d . . . . .
H49 H 0.315190 0.113637 -0.019306 0.026 Uiso 1 1 calc R U . . .
C60 C 0.3499(3) 0.15298(15) 0.18405(19) 0.0242(6) Uani 1 1 d . . . . .
H50 H 0.366605 0.140256 0.236225 0.036 Uiso 1 1 calc R U . . .
H51 H 0.364023 0.117493 0.154755 0.036 Uiso 1 1 calc R U . . .
H52 H 0.274479 0.164984 0.165348 0.036 Uiso 1 1 calc R U . . .
C59 C 0.5368(2) 0.18989(16) 0.19765(18) 0.0232(6) Uani 1 1 d . . . . .
H53 H 0.579762 0.225590 0.189463 0.035 Uiso 1 1 calc R U . . .
H54 H 0.544209 0.154085 0.166434 0.035 Uiso 1 1 calc R U . . .
H55 H 0.561480 0.177264 0.249982 0.035 Uiso 1 1 calc R U . . .
H56 H 0.174(4) 0.282(2) 0.116(2) 0.028 Uiso 1 1 d . U . . .
H57 H 0.418(4) 0.332(2) 0.335(2) 0.028 Uiso 1 1 d . U . . .
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
-8 -1 9 0.0752
-1 12 -5 0.0745
8 0 -9 0.0830
1 -12 4 0.1357
0 5 11 0.0560
1 -4 -11 0.0411
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
C37 N26 C41 121.7(2) . . ?
C37 N26 C38 113.1(2) . . ?
C38 N26 C41 123.0(2) . . ?
C13 N10 C17 123.4(2) . . ?
C13 N10 C14 113.0(2) . . ?
C17 N10 C14 123.5(2) . . ?
C10 N7 C9 112.5(2) . . ?
C10 N7 C6 119.9(2) . . ?
C9 N7 C6 122.4(2) . . ?
C1 N2 C47 122.3(2) . . ?
C1 N2 C3 112.4(2) . . ?
C47 N2 C3 122.0(2) . . ?
C7 N5 C9 112.0(2) . . ?
C7 N5 C5 123.5(2) . . ?
C5 N5 C9 122.8(2) . . ?
C46 N32 C44 110.8(2) . . ?
C46 N32 C48 119.2(2) . . ?
C48 N32 C44 120.0(2) . . ?
C7 N6 C8 112.1(2) . . ?
C7 N6 C11 123.4(2) . . ?
C8 N6 C11 122.5(2) . . ?
C22 N16 C24 119.9(2) . . ?
C22 N16 C20 112.0(2) . . ?
C24 N16 C20 122.3(2) . . ?
C25 N18 C26 112.1(2) . . ?
C25 N18 C29 119.5(2) . . ?
C26 N18 C29 119.7(2) . . ?
C40 N27 C39 112.7(2) . . ?
C40 N27 C36 122.8(2) . . ?
C36 N27 C39 124.3(2) . . ?
C61 N36 C56 123.7(2) . . ?
C22 N15 C18 122.6(2) . . ?
C22 N15 C21 112.8(2) . . ?
C18 N15 C21 124.2(2) . . ?
C55 N35 C54 122.0(2) . . ?
C43 N29 C41 122.3(2) . . ?
C43 N29 C45 111.8(2) . . ?
C41 N29 C45 121.9(2) . . ?
C46 N31 C42 123.1(2) . . ?
C46 N31 C45 112.1(2) . . ?
C42 N31 C45 122.5(2) . . ?
C1 N1 C2 110.4(2) . . ?
C1 N1 C5 118.9(2) . . ?
C5 N1 C2 120.0(2) . . ?
C53 N34 C52 122.6(3) . . ?
C10 N8 C8 112.4(2) . . ?
C10 N8 C12 121.8(2) . . ?
C12 N8 C8 124.0(2) . . ?
C28 N19 C24 120.9(2) . . ?
C28 N19 C27 112.0(2) . . ?
C24 N19 C27 121.9(2) . . ?
C43 N30 C47 121.7(2) . . ?
C43 N30 C44 112.5(2) . . ?
C47 N30 C44 123.5(2) . . ?
C34 N23 C33 111.6(2) . . ?
C34 N23 C30 119.7(2) . . ?
C30 N23 C33 122.0(2) . . ?
C13 N9 C15 111.3(2) . . ?
C13 N9 C11 119.7(2) . . ?
C11 N9 C15 122.2(2) . . ?
C34 N24 C36 121.8(2) . . ?
C34 N24 C32 112.2(2) . . ?
C32 N24 C36 122.9(2) . . ?
C40 N28 C42 122.0(2) . . ?
C40 N28 C38 112.2(2) . . ?
C42 N28 C38 125.5(2) . . ?
C28 N20 C26 112.8(2) . . ?
C28 N20 C30 122.7(2) . . ?
C30 N20 C26 123.3(2) . . ?
C4 N3 C3 111.3(2) . . ?
C4 N3 C48 119.1(2) . . ?
C48 N3 C3 121.5(2) . . ?
C19 N14 C23 121.3(2) . . ?
C19 N14 C20 112.3(2) . . ?
C23 N14 C20 123.6(2) . . ?
C51 N33 C50 121.8(3) . . ?
C19 N13 C17 121.6(2) . . ?
C19 N13 C21 112.8(2) . . ?
C17 N13 C21 123.7(2) . . ?
C16 N12 C14 112.1(2) . . ?
C16 N12 C18 121.5(2) . . ?
C18 N12 C14 122.6(2) . . ?
C31 N21 C29 121.4(2) . . ?
C31 N21 C33 112.4(2) . . ?
C33 N21 C29 122.9(2) . . ?
C37 N25 C39 111.7(2) . . ?
C37 N25 C35 120.8(2) . . ?
C35 N25 C39 123.4(2) . . ?
C25 N17 C23 122.3(2) . . ?
C25 N17 C27 112.6(2) . . ?
C27 N17 C23 122.3(2) . . ?
C12 N11 C15 123.0(2) . . ?
C16 N11 C12 124.1(3) . . ?
C16 N11 C15 112.9(2) . . ?
C4 N4 C6 123.2(2) . . ?
C4 N4 C2 113.1(2) . . ?
C2 N4 C6 123.1(2) . . ?
C31 N22 C32 112.9(2) . . ?
C31 N22 C35 123.3(2) . . ?
C32 N22 C35 123.3(2) . . ?
O3 C7 N5 125.7(3) . . ?
O3 C7 N6 125.8(3) . . ?
N6 C7 N5 108.4(2) . . ?
O14 C40 N27 125.3(3) . . ?
O14 C40 N28 125.8(3) . . ?
N28 C40 N27 108.9(2) . . ?
O15 C43 N29 126.4(3) . . ?
O15 C43 N30 125.5(3) . . ?
N30 C43 N29 108.2(2) . . ?
O16 C46 N32 126.7(3) . . ?
O16 C46 N31 124.6(3) . . ?
N31 C46 N32 108.7(2) . . ?
O22 C61 N36 124.8(3) . . ?
O22 C61 C62 119.8(3) . . ?
N36 C61 C62 115.4(2) . . ?
O1 C1 N2 125.0(3) . . ?
O1 C1 N1 126.3(3) . . ?
N2 C1 N1 108.7(2) . . ?
O10 C28 N19 125.3(3) . . ?
O10 C28 N20 126.0(3) . . ?
N20 C28 N19 108.7(2) . . ?
O2 C4 N3 127.1(3) . . ?
O2 C4 N4 125.8(3) . . ?
N4 C4 N3 107.1(2) . . ?
O12 C34 N23 126.0(3) . . ?
O12 C34 N24 125.7(3) . . ?
N24 C34 N23 108.3(2) . . ?
N27 C39 N25 114.8(2) . . ?
N27 C39 C38 102.7(2) . . ?
N25 C39 C38 103.0(2) . . ?
N2 C47 N30 112.6(2) . . ?
O4 C10 N7 126.8(3) . . ?
O4 C10 N8 125.4(3) . . ?
N7 C10 N8 107.8(2) . . ?
O7 C19 N14 126.1(3) . . ?
O7 C19 N13 126.1(3) . . ?
N14 C19 N13 107.8(2) . . ?
O5 C13 N10 126.2(3) . . ?
O5 C13 N9 125.9(3) . . ?
N10 C13 N9 107.9(2) . . ?
N6 C8 N8 114.2(2) . . ?
N6 C8 C9 103.5(2) . . ?
N8 C8 C9 103.3(2) . . ?
N11 C12 N8 114.6(2) . . ?
N7 C9 N5 115.3(2) . . ?
N7 C9 C8 103.6(2) . . ?
N5 C9 C8 103.2(2) . . ?
N10 C17 N13 114.6(2) . . ?
O13 C37 N26 125.9(3) . . ?
O13 C37 N25 125.8(3) . . ?
N26 C37 N25 108.3(2) . . ?
O19 C51 N33 123.4(3) . . ?
O19 C51 C52 120.7(3) . . ?
N33 C51 C52 115.8(3) . . ?
O9 C25 N18 126.3(3) . . ?
O9 C25 N17 126.0(3) . . ?
N18 C25 N17 107.6(2) . . ?
N2 C3 N3 113.9(2) . . ?
N2 C3 C2 103.4(2) . . ?
N3 C3 C2 103.4(2) . . ?
O11 C31 N21 126.2(3) . . ?
O11 C31 N22 126.2(3) . . ?
N21 C31 N22 107.6(2) . . ?
N27 C36 N24 113.3(2) . . ?
O18 C49 O17 124.8(3) . . ?
O18 C49 C50 120.5(3) . . ?
O17 C49 C50 114.7(3) . . ?
N10 C14 N12 114.4(2) . . ?
N10 C14 C15 102.9(2) . . ?
N12 C14 C15 102.8(2) . . ?
C69 C64 C63 119.7(3) . . ?
C69 C64 C65 118.4(3) . . ?
C65 C64 C63 121.9(3) . . ?
O8 C22 N16 125.2(3) . . ?
O8 C22 N15 126.5(3) . . ?
N15 C22 N16 108.3(2) . . ?
O6 C16 N12 125.9(3) . . ?
O6 C16 N11 126.1(3) . . ?
N11 C16 N12 108.0(2) . . ?
N24 C32 C33 103.8(2) . . ?
N22 C32 N24 114.6(2) . . ?
N22 C32 C33 103.1(2) . . ?
O23 C67 C68 122.2(3) . . ?
O23 C67 C66 118.6(3) . . ?
C68 C67 C66 119.2(3) . . ?
N14 C23 N17 114.3(2) . . ?
N37 C62 C61 106.9(2) . . ?
N37 C62 C63 106.5(2) . . ?
C61 C62 C63 113.7(2) . . ?
N18 C26 N20 113.3(2) . . ?
N18 C26 C27 103.2(2) . . ?
N20 C26 C27 102.6(2) . . ?
C58 C57 C56 114.0(2) . . ?
N12 C18 N15 113.0(2) . . ?
O21 C55 N35 122.0(3) . . ?
O21 C55 C56 121.1(3) . . ?
N35 C55 C56 116.8(2) . . ?
N4 C6 N7 113.9(2) . . ?
N32 C44 C45 103.1(2) . . ?
N30 C44 N32 113.9(2) . . ?
N30 C44 C45 102.8(2) . . ?
N26 C41 N29 112.4(2) . . ?
N31 C42 N28 114.0(2) . . ?
N21 C29 N18 113.0(2) . . ?
N29 C45 C44 103.2(2) . . ?
N31 C45 N29 114.0(2) . . ?
N31 C45 C44 103.8(2) . . ?
N16 C24 N19 113.8(2) . . ?
N23 C33 C32 103.4(2) . . ?
N21 C33 N23 114.1(2) . . ?
N21 C33 C32 103.6(2) . . ?
N1 C2 C3 103.2(2) . . ?
N4 C2 N1 114.5(2) . . ?
N4 C2 C3 103.5(2) . . ?
N22 C35 N25 113.7(2) . . ?
N19 C27 C26 103.3(2) . . ?
N17 C27 N19 113.5(2) . . ?
N17 C27 C26 103.5(2) . . ?
C57 C58 C60 112.2(2) . . ?
C59 C58 C57 109.5(2) . . ?
C59 C58 C60 110.3(3) . . ?
N36 C56 C57 113.3(2) . . ?
N36 C56 C55 110.4(2) . . ?
C55 C56 C57 115.6(2) . . ?
C69 C68 C67 120.1(3) . . ?
N9 C15 C14 103.3(2) . . ?
N11 C15 N9 114.8(2) . . ?
N11 C15 C14 102.7(2) . . ?
N15 C21 C20 102.8(2) . . ?
N13 C21 N15 114.6(2) . . ?
N13 C21 C20 102.6(2) . . ?
N23 C30 N20 113.1(2) . . ?
N26 C38 N28 114.5(2) . . ?
N26 C38 C39 103.2(2) . . ?
N28 C38 C39 103.2(2) . . ?
N16 C20 N14 114.3(2) . . ?
N16 C20 C21 103.8(2) . . ?
N14 C20 C21 103.8(2) . . ?
N6 C11 N9 112.9(2) . . ?
O20 C53 N34 123.7(3) . . ?
O20 C53 C54 118.5(3) . . ?
N34 C53 C54 117.8(3) . . ?
C64 C63 C62 116.0(2) . . ?
C68 C69 C64 121.2(3) . . ?
N5 C5 N1 113.4(2) . . ?
N3 C48 N32 113.3(2) . . ?
N34 C52 C51 110.8(3) . . ?
C66 C65 C64 120.8(3) . . ?
N35 C54 C53 116.4(2) . . ?
N33 C50 C49 115.4(3) . . ?
C65 C66 C67 120.3(3) . . ?
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
O16 C46 1.221(4) . ?
O1 C1 1.225(4) . ?
O14 C40 1.234(4) . ?
O12 C34 1.230(4) . ?
O4 C10 1.213(4) . ?
O2 C4 1.211(4) . ?
O10 C28 1.231(4) . ?
O5 C13 1.220(4) . ?
O15 C43 1.230(4) . ?
O6 C16 1.229(4) . ?
O9 C25 1.212(4) . ?
O7 C19 1.210(4) . ?
O8 C22 1.226(4) . ?
O11 C31 1.221(4) . ?
O3 C7 1.233(4) . ?
O22 C61 1.233(4) . ?
O13 C37 1.225(4) . ?
O21 C55 1.228(4) . ?
O23 C67 1.363(4) . ?
O18 C49 1.246(4) . ?
O17 C49 1.271(4) . ?
O20 C53 1.241(4) . ?
O19 C51 1.236(4) . ?
N26 C37 1.364(4) . ?
N26 C41 1.444(4) . ?
N26 C38 1.440(4) . ?
N10 C13 1.375(4) . ?
N10 C17 1.441(4) . ?
N10 C14 1.443(4) . ?
N7 C10 1.375(4) . ?
N7 C9 1.447(4) . ?
N7 C6 1.456(4) . ?
N2 C1 1.367(4) . ?
N2 C47 1.442(4) . ?
N2 C3 1.445(4) . ?
N5 C7 1.370(4) . ?
N5 C9 1.450(4) . ?
N5 C5 1.449(4) . ?
N32 C46 1.380(4) . ?
N32 C44 1.470(3) . ?
N32 C48 1.460(4) . ?
N6 C7 1.365(4) . ?
N6 C8 1.444(4) . ?
N6 C11 1.450(4) . ?
N16 C22 1.379(4) . ?
N16 C24 1.441(4) . ?
N16 C20 1.446(4) . ?
N18 C25 1.380(4) . ?
N18 C26 1.446(4) . ?
N18 C29 1.461(4) . ?
N27 C40 1.367(4) . ?
N27 C39 1.451(4) . ?
N27 C36 1.443(4) . ?
N36 C61 1.333(4) . ?
N36 C56 1.458(4) . ?
N15 C22 1.367(4) . ?
N15 C18 1.449(4) . ?
N15 C21 1.454(4) . ?
N35 C55 1.342(4) . ?
N35 C54 1.452(4) . ?
N29 C43 1.365(4) . ?
N29 C41 1.446(4) . ?
N29 C45 1.449(4) . ?
N31 C46 1.374(4) . ?
N31 C42 1.446(4) . ?
N31 C45 1.447(3) . ?
N1 C1 1.381(4) . ?
N1 C2 1.467(4) . ?
N1 C5 1.450(3) . ?
N34 C53 1.324(4) . ?
N34 C52 1.451(4) . ?
N8 C10 1.378(4) . ?
N8 C8 1.453(4) . ?
N8 C12 1.448(4) . ?
N19 C28 1.371(4) . ?
N19 C24 1.447(4) . ?
N19 C27 1.452(4) . ?
N30 C43 1.362(4) . ?
N30 C47 1.445(4) . ?
N30 C44 1.452(4) . ?
N23 C34 1.383(4) . ?
N23 C33 1.455(4) . ?
N23 C30 1.439(4) . ?
N9 C13 1.381(4) . ?
N9 C15 1.460(3) . ?
N9 C11 1.456(3) . ?
N24 C34 1.370(4) . ?
N24 C36 1.450(4) . ?
N24 C32 1.448(4) . ?
N28 C40 1.357(4) . ?
N28 C42 1.447(4) . ?
N28 C38 1.460(4) . ?
N37 C62 1.494(4) . ?
N20 C28 1.353(4) . ?
N20 C26 1.453(4) . ?
N20 C30 1.449(4) . ?
N3 C4 1.390(4) . ?
N3 C3 1.458(4) . ?
N3 C48 1.451(4) . ?
N14 C19 1.374(4) . ?
N14 C23 1.450(4) . ?
N14 C20 1.454(4) . ?
N33 C51 1.338(4) . ?
N33 C50 1.438(4) . ?
N13 C19 1.378(4) . ?
N13 C17 1.448(4) . ?
N13 C21 1.453(4) . ?
N12 C14 1.456(4) . ?
N12 C16 1.371(4) . ?
N12 C18 1.449(4) . ?
N21 C31 1.371(4) . ?
N21 C29 1.453(4) . ?
N21 C33 1.447(4) . ?
N25 C39 1.459(4) . ?
N25 C37 1.374(4) . ?
N25 C35 1.455(4) . ?
N17 C25 1.383(4) . ?
N17 C23 1.452(4) . ?
N17 C27 1.436(4) . ?
N11 C12 1.435(4) . ?
N11 C16 1.367(4) . ?
N11 C15 1.447(4) . ?
N4 C4 1.387(4) . ?
N4 C6 1.440(4) . ?
N4 C2 1.429(4) . ?
N22 C31 1.376(4) . ?
N22 C32 1.437(4) . ?
N22 C35 1.438(4) . ?
C61 C62 1.532(4) . ?
C39 C38 1.559(4) . ?
C8 C9 1.548(4) . ?
C51 C52 1.525(4) . ?
C3 C2 1.545(4) . ?
C49 C50 1.530(4) . ?
C14 C15 1.553(4) . ?
C64 C63 1.509(4) . ?
C64 C69 1.394(4) . ?
C64 C65 1.397(4) . ?
C32 C33 1.549(4) . ?
C67 C68 1.395(4) . ?
C67 C66 1.398(4) . ?
C62 C63 1.547(4) . ?
C26 C27 1.556(4) . ?
C57 C58 1.532(4) . ?
C57 C56 1.538(4) . ?
C55 C56 1.537(4) . ?
C44 C45 1.548(4) . ?
C58 C60 1.534(4) . ?
C58 C59 1.525(4) . ?
C68 C69 1.389(4) . ?
C21 C20 1.557(4) . ?
C53 C54 1.514(4) . ?
C65 C66 1.388(5) . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.86(10)
2 0.14(10)
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
-7.5085 -0.8799 8.6562 0.0276 0.1049 0.9941
-0.6168 12.1600 -5.0513 0.2217 0.9246 -0.3097
7.5826 0.4406 -8.5305 -0.0359 -0.1395 -0.9896
1.3745 -12.2624 4.2679 -0.2279 -0.9495 0.2155
-0.0657 4.5381 11.0596 0.8796 -0.2125 0.4256
0.6701 -4.1745 -11.3843 -0.8456 0.2045 -0.4932
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.200 0.203 0.656 219.7 81.7 '8 H2O'
2 0.200 0.703 0.344 219.7 81.7 '8 H2O'
