#------------------------------------------------------------------------------
#$Date: 2024-04-05 01:40:10 +0300 (Fri, 05 Apr 2024) $
#$Revision: 290832 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/12/1571240.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_1571240
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_compound_source        synthetic
_chemical_formula_moiety
'4(C21 H32 N5 O7), 23.2(H2 O), 4(C48 H48 N32 O16), 15(H O), 2(O)'
_chemical_formula_sum            'C276 H381.4 N148 O132.2'
_chemical_formula_weight         7887.87
_chemical_name_common            'LYGGG Q8 complex'
_chemical_name_systematic
'L-leucyl-L-tyrosylglycylglycylglycine cucurbit[8]uril complex hydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-16 deposited with the CCDC.	2024-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.7510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   34.6961(3)
_cell_length_b                   14.63880(10)
_cell_length_c                   18.86300(10)
_cell_measurement_reflns_used    43860
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.9140
_cell_measurement_theta_min      2.5410
_cell_volume                     9579.87(12)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00   0.00   0.50    1.35    --  -46.89 108.00 131.00  164
  2  ω     21.00  84.00   0.50    1.35    --   46.89-108.00  34.00  126
  3  ω   -162.00 -82.00   0.50    5.38    --  -91.75-108.00  34.00  160
  4  ω    -82.00 -22.00   0.50    5.38    --  -91.75 108.00 131.00  120
  5  ω    104.00 177.00   0.50    5.38    --  106.92 108.00 131.00  146
  6  ω     37.00 107.00   0.50    5.38    --  106.92-108.00  34.00  140
  7  ω   -119.00 -30.00   0.50    1.35    --  -46.89 -54.00 114.49  178
  8  ω    -30.00  29.00   0.50    1.35    --  -46.89  19.00   0.00  118
  9  ω   -119.00 -83.00   0.50    1.35    --  -46.89 -57.00-120.00   72
 10  ω   -119.00 -83.00   0.50    1.35    --  -46.89 -57.00-150.00   72
 11  ω    -43.00  27.00   0.50    1.35    --  -46.89  37.00  90.00  140
 12  ω     83.00 119.00   0.50    1.35    --   46.89  57.00-150.00   72
 13  ω     83.00 119.00   0.50    1.35    --   46.89  57.00-180.00   72
 14  ω    -51.00 -19.00   0.50    5.38    --  -91.75  45.00 -90.00   64
 15  ω    -71.00 -19.00   0.50    5.38    --  -91.75  61.00  90.00  104
 16  ω   -164.00 -77.00   0.50    5.38    --  -91.75 -45.00  63.98  174
 17  ω    -51.00 -19.00   0.50    5.38    --  -91.75  45.00 120.00   64
 18  ω    -51.00 -19.00   0.50    5.38    --  -91.75  45.00 -60.00   64
 19  ω   -162.00 -88.00   0.50    5.38    --  -91.75-125.00-150.00  148
 20  ω   -164.00 -83.00   0.50    5.38    --  -91.75 -57.00-162.59  162
 21  ω   -164.00-100.00   0.50    5.38    --  -91.75 -94.00 -90.00  128
 22  ω    -51.00 -19.00   0.50    5.38    --  -91.75  45.00  90.00   64
 23  ω    -51.00 -19.00   0.50    5.38    --  -91.75  45.00 -30.00   64
 24  ω   -164.00 -91.00   0.50    5.38    --  -91.75 -61.00 -30.00  146
 25  ω   -164.00 -91.00   0.50    5.38    --  -91.75 -61.00 -60.00  146
 26  ω     37.00 112.00   0.50    5.38    --  106.92-125.00   0.00  150
 27  ω     34.00 106.00   0.50    5.38    --  106.92 -94.00 -90.00  144
 28  ω     37.00 112.00   0.50    5.38    --  106.92-125.00 120.00  150
 29  ω     34.00  71.00   0.50    5.38    --  106.92 -61.00  90.00   74
 30  ω     36.00 107.00   0.50    5.38    --  106.92-105.00-111.01  142
 31  ω     34.00  71.00   0.50    5.38    --  106.92 -61.00 -60.00   74
 32  ω     34.00  71.00   0.50    5.38    --  106.92 -61.00   0.00   74
 33  ω     37.00 112.00   0.50    5.38    --  106.92-125.00-120.00  150
 34  ω     37.00 112.00   0.50    5.38    --  106.92-125.00 150.00  150
 35  ω     93.00 178.00   0.50    5.38    --  106.92  45.00-150.00  170
 36  ω     34.00 106.00   0.50    5.38    --  106.92 -94.00  30.00  144
 37  ω     95.00 177.00   0.50    5.38    --  106.92 125.00 -30.00  164
 38  ω     34.00  71.00   0.50    5.38    --  106.92 -61.00-120.00   74
 39  ω   -119.00 -32.00   0.50    1.35    --  -46.89 -48.00 -95.05  174
 40  ω   -119.00 -32.00   0.50    1.35    --  -46.89 -48.00  33.66  174
 41  ω   -119.00 -32.00   0.50    1.35    --  -46.89 -52.00-159.34  174
 42  ω   -119.00 -71.00   0.50    1.35    --  -46.89 -55.00 -36.40   96
 43  ω   -119.00 -30.00   0.50    1.35    --  -46.89 -54.00  -4.10  178
;
_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      -0.0435630000
_diffrn_orient_matrix_UB_12      0.0117996000
_diffrn_orient_matrix_UB_13      0.0117671000
_diffrn_orient_matrix_UB_21      0.0031903000
_diffrn_orient_matrix_UB_22      0.1017859000
_diffrn_orient_matrix_UB_23      -0.0198646000
_diffrn_orient_matrix_UB_31      -0.0079289000
_diffrn_orient_matrix_UB_32      -0.0239635000
_diffrn_orient_matrix_UB_33      -0.0783742000
_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  0.0443
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            88713
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.000
_diffrn_reflns_theta_min         4.020
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
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    1.367
_exptl_crystal_description       plank
_exptl_crystal_F_000             4131
_exptl_crystal_recrystallization_method 'pH 7 10 mM phosphate-buffered D2O'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1317
_refine_ls_number_reflns         17957
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0560
_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)+(0.0350P)²+25.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1324
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                16856
_reflns_number_total             17957
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc01122h2.cif
_cod_data_source_block           hpd817c
_cod_depositor_comments
'Adding full bibliography for 1571239--1571240.cif.'
_cod_original_formula_sum        'C276 H381.40 N148 O132.20'
_cod_database_code               1571240
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O'
_chemical_oxdiff_usercomment     'H-LYGGG-OH Q8'
_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   0.963
_shelx_estimated_absorpt_t_min   0.895
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.84081
 0.15919
2. Restrained distances
 H31B-O32
 1.95 with sigma of 0.02
 H26A-O21A
 2.1 with sigma of 0.02
 H26A-O22A
 2.05 with sigma of 0.02
 O19_$1-H34D
 2.2 with sigma of 0.02
 H35C-O10
 2.1 with sigma of 0.02
 H31A-O21B
 2.15 with sigma of 0.02
 H36-N36
 0.85 with sigma of 0.02
 H34E-O13_$1
 2.05 with sigma of 0.02
 H25-O24
 2 with sigma of 0.02
 O20-H28B
 2 with sigma of 0.02
 H27A-O22B
 1.7 with sigma of 0.02
 H27C-O23A
 1.95 with sigma of 0.02
 H27C-O27A
 1.05 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C69B) = Uanis(O23B) = Uanis(O23A) = Uanis(C69A) = Uanis(O22A) = Uanis(C68)
Uanis(O22B) = Uanis(C69B) = Uanis(O23B)
Uanis(O27B) = Uanis(O27A)
4. Others
 Fixed Sof: O21A(0.6) O35(0.75) H35C(0.75) O31(0.5) H31A(0.5) H31B(0.5)
 O22A(0.6) O23A(0.6) H68A(0.6) H68B(0.6) H68C(0.4) H68D(0.4) O26(0.5) H26A(0.5)
 O32(0.5) C69A(0.6) C69B(0.4) O23B(0.4) O21B(0.4) O22B(0.4) O27A(0.5) O27B(0.3)
 H27C(0.5) H27A(0.3) H27B(0.3)
5.a Free rotating group:
 O33(H33B,H33C), O34(H34D,H34E), O29(H29C,H29D), O24(H24C,H24D), O30(H30),
 O28(H28A,H28B), O25(H25), O35(H35C), O31(H31A,H31B), O26(H26A), O27B(H27C,H27A,
 H27B)
5.b Ternary CH refined with riding coordinates:
 C60(H60), C49(H49), C20(H20), C2(H2), C14(H14), C27(H27), C33(H33), C3(H3),
 C15(H15), C45(H45), C9(H9), C44(H44), C26(H26), C21(H21), C8(H8), C58(H58),
 C39(H39), C32(H32), C38(H38)
5.c Secondary CH2 refined with riding coordinates:
 N37(H37A,H37B), C59(H59A,H59B), C24(H24A,H24B), C64(H64A,H64B), C11(H11A,
 H11B), C6(H6A,H6B), C5(H5A,H5B), C42(H42A,H42B), C66(H66A,H66B), C50(H50A,
 H50B), C48(H48A,H48B), C12(H12A,H12B), C35(H35A,H35B), C41(H41A,H41B),
 C23(H23A,H23B), C18(H18A,H18B), C29(H29A,H29B), C47(H47A,H47B), C17(H17A,H17B),
  C30(H30A,H30B), C36(H36A,H36B), C68(H68A,H68B), C68(H68C,H68D)
5.d Aromatic/amide H refined with riding coordinates:
 N35(H35), C56(H56), C55(H55), C52(H52), C53(H53)
5.e Idealised Me refined as rotating group:
 N34(H34A,H34B,H34C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C)
5.f Idealised tetrahedral OH refined as rotating group:
 O17(H17)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.387
_oxdiff_exptl_absorpt_empirical_full_min 0.659
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, 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
O19 O 0.33128(10) 0.4434(2) 0.92263(16) 0.0320(7) Uani 1 1 d . . . . .
O33 O 0.35032(9) 0.2039(2) 0.71209(17) 0.0332(7) Uani 1 1 d G . . . .
H33B H 0.334648 0.162665 0.728448 0.050 Uiso 1 1 d G U . . .
H33C H 0.335357 0.241957 0.689461 0.050 Uiso 1 1 d G U . . .
O3 O 0.11832(11) 0.6147(3) 0.85460(18) 0.0395(8) Uani 1 1 d . . . . .
O5 O 0.11291(10) 0.4538(2) 0.71209(17) 0.0363(8) Uani 1 1 d . . . . .
O17 O 0.29924(12) 0.9317(2) 0.69203(17) 0.0420(9) Uani 1 1 d . . . . .
H17 H 0.301371 0.977833 0.718297 0.063 Uiso 1 1 calc R U . . .
O6 O 0.12914(10) 0.7591(2) 0.49501(17) 0.0375(8) Uani 1 1 d . . . . .
O4 O 0.13128(10) 0.9331(3) 0.64084(17) 0.0402(8) Uani 1 1 d . . . . .
O9 O 0.30812(12) 0.3750(3) 0.66882(17) 0.0424(9) Uani 1 1 d . . . . .
O16 O 0.31138(12) 1.0676(2) 0.79175(17) 0.0404(9) Uani 1 1 d . . . . .
O18 O 0.23648(11) 0.5382(3) 0.87250(18) 0.0454(9) Uani 1 1 d . . . . .
O11 O 0.39778(10) 0.4841(3) 0.7834(2) 0.0420(9) Uani 1 1 d . . . . .
O1 O 0.20817(11) 0.7366(3) 0.96652(18) 0.0407(8) Uani 1 1 d . . . . .
O7 O 0.19919(13) 0.3529(3) 0.63784(17) 0.0453(9) Uani 1 1 d . . . . .
O8 O 0.20800(11) 0.6442(2) 0.40524(18) 0.0400(8) Uani 1 1 d . . . . .
O20 O 0.37823(11) 0.1915(2) 0.91973(19) 0.0424(9) Uani 1 1 d D . . . .
O14 O 0.39541(13) 0.9494(3) 0.6933(2) 0.0537(10) Uani 1 1 d . . . . .
O15 O 0.32119(11) 0.7632(3) 1.00363(19) 0.0449(9) Uani 1 1 d . . . . .
N35 N 0.31698(11) 0.3556(3) 0.82862(19) 0.0281(8) Uani 1 1 d . . . . .
H35 H 0.309408 0.352665 0.783971 0.034 Uiso 1 1 calc R U . . .
O13 O 0.40399(11) 0.6611(3) 0.9315(2) 0.0491(10) Uani 1 1 d . . . . .
O2 O 0.20992(12) 1.0763(3) 0.77142(19) 0.0512(10) Uani 1 1 d . . . . .
N17 N 0.29579(13) 0.3962(3) 0.55014(19) 0.0346(9) Uani 1 1 d . . . . .
N9 N 0.08152(12) 0.5797(3) 0.6684(2) 0.0375(10) Uani 1 1 d . . . . .
N1 N 0.22651(12) 0.8887(3) 0.9551(2) 0.0362(9) Uani 1 1 d . . . . .
N4 N 0.17199(13) 0.9731(3) 0.8319(2) 0.0352(9) Uani 1 1 d . . . . .
N6 N 0.08621(12) 0.6906(3) 0.7639(2) 0.0369(10) Uani 1 1 d . . . . .
N13 N 0.16481(14) 0.4120(3) 0.5413(2) 0.0398(10) Uani 1 1 d . . . . .
N10 N 0.10995(13) 0.4858(3) 0.5937(2) 0.0367(9) Uani 1 1 d . . . . .
N2 N 0.16850(13) 0.8447(3) 0.9138(2) 0.0366(9) Uani 1 1 d . . . . .
N8 N 0.09312(12) 0.8146(3) 0.6785(2) 0.0330(9) Uani 1 1 d . . . . .
N33 N 0.27440(13) 0.5115(3) 0.7775(2) 0.0333(9) Uani 1 1 d . . . . .
N15 N 0.23179(13) 0.5052(3) 0.4419(2) 0.0367(9) Uani 1 1 d . . . . .
O34 O 0.59368(12) 0.4795(3) 1.0313(2) 0.0558(11) Uani 1 1 d G . . . .
H34D H 0.607853 0.440455 1.052092 0.084 Uiso 1 1 d DG U . . .
H34E H 0.607672 0.535024 1.030659 0.084 Uiso 1 1 d DG U . . .
N36 N 0.39342(12) 0.3102(3) 0.8484(2) 0.0319(9) Uani 1 1 d D . . . .
N30 N 0.29469(13) 0.9054(3) 0.9813(2) 0.0399(10) Uani 1 1 d . . . . .
O29 O 0.53868(13) 0.2494(4) 0.9102(2) 0.0632(12) Uani 1 1 d G . . . .
H29C H 0.527563 0.216952 0.942796 0.095 Uiso 1 1 d G U . . .
H29D H 0.524409 0.240975 0.872397 0.095 Uiso 1 1 d G U . . .
N37 N 0.43048(12) 0.2161(4) 0.7452(2) 0.0462(11) Uani 1 1 d . . . . .
H37A H 0.415325 0.262941 0.729707 0.055 Uiso 1 1 calc R U . . .
H37B H 0.414549 0.175635 0.766764 0.055 Uiso 1 1 calc R U . . .
N29 N 0.35740(13) 0.8886(3) 0.9719(2) 0.0434(11) Uani 1 1 d . . . . .
N11 N 0.09006(11) 0.7029(3) 0.5833(2) 0.0338(9) Uani 1 1 d . . . . .
N18 N 0.35228(13) 0.4421(3) 0.5947(2) 0.0367(9) Uani 1 1 d . . . . .
N7 N 0.12293(12) 0.9004(3) 0.7594(2) 0.0350(9) Uani 1 1 d . . . . .
N12 N 0.11407(12) 0.6066(3) 0.5046(2) 0.0365(9) Uani 1 1 d . . . . .
N5 N 0.11975(12) 0.7723(3) 0.8420(2) 0.0338(9) Uani 1 1 d . . . . .
N21 N 0.40394(13) 0.5106(3) 0.6627(2) 0.0415(10) Uani 1 1 d . . . . .
C13 C 0.10263(14) 0.5014(3) 0.6635(3) 0.0337(11) Uani 1 1 d . . . . .
O24 O 0.25063(17) 0.2443(3) 0.7447(2) 0.0662(13) Uani 1 1 d DG . . . .
H24C H 0.260345 0.264401 0.705382 0.099 Uiso 1 1 d G U . . .
H24D H 0.244072 0.188146 0.735253 0.099 Uiso 1 1 d G U . . .
N3 N 0.22433(13) 1.0285(3) 0.8855(2) 0.0417(10) Uani 1 1 d . . . . .
N14 N 0.22678(14) 0.3829(3) 0.5302(2) 0.0381(10) Uani 1 1 d . . . . .
N22 N 0.43488(13) 0.6010(3) 0.7391(3) 0.0431(11) Uani 1 1 d . . . . .
N32 N 0.29288(14) 1.0409(3) 0.9066(2) 0.0378(10) Uani 1 1 d . . . . .
N25 N 0.43368(13) 0.7174(3) 0.8311(3) 0.0453(11) Uani 1 1 d . . . . .
N27 N 0.40399(15) 0.9254(3) 0.8146(2) 0.0452(11) Uani 1 1 d . . . . .
O10 O 0.32214(14) 0.6584(4) 0.4351(3) 0.0785(17) Uani 1 1 d D . . . .
N23 N 0.40701(14) 0.6279(3) 0.5714(3) 0.0468(11) Uani 1 1 d . . . . .
O12 O 0.39942(15) 0.7832(3) 0.5577(2) 0.0706(15) Uani 1 1 d . . . . .
N16 N 0.16907(13) 0.5310(3) 0.4521(2) 0.0361(9) Uani 1 1 d . . . . .
N31 N 0.35173(14) 0.9989(3) 0.8748(2) 0.0396(10) Uani 1 1 d . . . . .
C63 C 0.32022(13) 0.4366(3) 0.8604(2) 0.0282(10) Uani 1 1 d . . . . .
C56 C 0.28573(14) 0.7607(3) 0.8315(2) 0.0300(10) Uani 1 1 d . . . . .
H56 H 0.270635 0.751344 0.872569 0.036 Uiso 1 1 calc R U . . .
C43 C 0.32418(17) 0.8441(4) 0.9871(3) 0.0415(13) Uani 1 1 d . . . . .
C55 C 0.28130(15) 0.8412(3) 0.7928(2) 0.0339(11) Uani 1 1 d . . . . .
H55 H 0.263679 0.886731 0.807801 0.041 Uiso 1 1 calc R U . . .
C7 C 0.10897(15) 0.6850(4) 0.8233(3) 0.0392(12) Uani 1 1 d . . . . .
N19 N 0.30049(13) 0.5134(3) 0.4576(2) 0.0421(11) Uani 1 1 d . . . . .
C65 C 0.36870(15) 0.2553(3) 0.8812(2) 0.0309(10) Uani 1 1 d . . . . .
N26 N 0.41013(14) 0.8144(3) 0.9098(3) 0.0449(11) Uani 1 1 d . . . . .
C51 C 0.31174(13) 0.6940(3) 0.8114(2) 0.0284(9) Uani 1 1 d . . . . .
N24 N 0.43455(15) 0.7208(3) 0.6488(3) 0.0485(12) Uani 1 1 d . . . . .
C54 C 0.30291(16) 0.8541(3) 0.7322(2) 0.0339(11) Uani 1 1 d . . . . .
C57 C 0.24011(14) 0.5232(3) 0.8091(2) 0.0333(10) Uani 1 1 d . . . . .
C16 C 0.11321(14) 0.6974(4) 0.5245(2) 0.0337(11) Uani 1 1 d . . . . .
C37 C 0.41458(15) 0.7239(4) 0.8946(3) 0.0422(13) Uani 1 1 d . . . . .
C1 C 0.20209(15) 0.8143(4) 0.9471(2) 0.0371(12) Uani 1 1 d . . . . .
C25 C 0.31758(16) 0.4018(3) 0.6102(2) 0.0353(11) Uani 1 1 d . . . . .
N34 N 0.17286(12) 0.4792(3) 0.8045(2) 0.0426(10) Uani 1 1 d . . . . .
H34A H 0.151652 0.470609 0.776442 0.051 Uiso 1 1 calc R U . . .
H34B H 0.166984 0.517873 0.840575 0.051 Uiso 1 1 calc R U . . .
H34C H 0.180668 0.424563 0.822764 0.051 Uiso 1 1 calc R U . . .
C19 C 0.19703(17) 0.3787(3) 0.5764(3) 0.0385(12) Uani 1 1 d . . . . .
C59 C 0.19228(15) 0.6148(4) 0.7363(3) 0.0380(11) Uani 1 1 d . . . . .
H59A H 0.167095 0.609498 0.711342 0.046 Uiso 1 1 calc R U . . .
H59B H 0.188457 0.653902 0.778423 0.046 Uiso 1 1 calc R U . . .
C60 C 0.22048(14) 0.6628(3) 0.6870(2) 0.0331(10) Uani 1 1 d . . . . .
H60 H 0.245798 0.669480 0.712466 0.040 Uiso 1 1 calc R U . . .
N20 N 0.35733(14) 0.5555(3) 0.5013(2) 0.0481(12) Uani 1 1 d . . . . .
C31 C 0.41101(14) 0.5267(4) 0.7331(3) 0.0376(11) Uani 1 1 d . . . . .
C10 C 0.11705(14) 0.8873(4) 0.6876(3) 0.0358(11) Uani 1 1 d . . . . .
C24 C 0.26838(16) 0.5138(4) 0.4084(3) 0.0434(13) Uani 1 1 d . . . . .
H24A H 0.268771 0.571457 0.381052 0.052 Uiso 1 1 calc R U . . .
H24B H 0.271484 0.462748 0.374524 0.052 Uiso 1 1 calc R U . . .
O30 O 0.53195(16) 0.4200(4) 0.9610(3) 0.0798(15) Uani 1 1 d G . . . .
H30 H 0.536187 0.466184 0.933801 0.120 Uiso 1 1 d G U . . .
C49 C 0.31156(13) 0.5194(3) 0.8142(2) 0.0305(10) Uani 1 1 d . . . . .
H49 H 0.331488 0.519438 0.776416 0.037 Uiso 1 1 calc R U . . .
C22 C 0.20308(16) 0.5676(3) 0.4307(2) 0.0348(11) Uani 1 1 d . . . . .
C64 C 0.32587(14) 0.2720(3) 0.8672(2) 0.0313(10) Uani 1 1 d . . . . .
H64A H 0.315337 0.219590 0.839998 0.038 Uiso 1 1 calc R U . . .
H64B H 0.312525 0.273764 0.913243 0.038 Uiso 1 1 calc R U . . .
C11 C 0.06608(15) 0.6123(4) 0.7350(3) 0.0395(12) Uani 1 1 d . . . . .
H11A H 0.038623 0.628510 0.727532 0.047 Uiso 1 1 calc R U . . .
H11B H 0.067231 0.561985 0.770018 0.047 Uiso 1 1 calc R U . . .
C67 C 0.45273(16) 0.2499(5) 0.7952(3) 0.0503(15) Uani 1 1 d . . . . .
C20 C 0.17205(16) 0.4351(3) 0.4687(2) 0.0355(11) Uani 1 1 d . . . . .
H20 H 0.156246 0.396978 0.435220 0.043 Uiso 1 1 calc R U . . .
C2 C 0.20633(16) 0.9735(4) 0.9404(3) 0.0381(11) Uani 1 1 d . . . . .
H2 H 0.201729 1.009517 0.984467 0.046 Uiso 1 1 calc R U . . .
C14 C 0.07125(14) 0.6189(4) 0.5990(3) 0.0359(11) Uani 1 1 d . . . . .
H14 H 0.042699 0.623220 0.591964 0.043 Uiso 1 1 calc R U . . .
N28 N 0.43471(16) 0.8354(3) 0.7388(3) 0.0521(13) Uani 1 1 d . . . . .
C46 C 0.31791(17) 1.0374(3) 0.8519(3) 0.0385(12) Uani 1 1 d . . . . .
C27 C 0.35520(17) 0.4599(4) 0.5188(3) 0.0407(12) Uani 1 1 d . . . . .
H27 H 0.376884 0.424863 0.497467 0.049 Uiso 1 1 calc R U . . .
C33 C 0.44847(15) 0.6315(4) 0.6711(3) 0.0454(14) Uani 1 1 d . . . . .
H33 H 0.477165 0.627071 0.668101 0.055 Uiso 1 1 calc R U . . .
C4 C 0.20284(16) 1.0306(4) 0.8244(3) 0.0400(12) Uani 1 1 d . . . . .
C52 C 0.33251(15) 0.7076(4) 0.7493(3) 0.0369(11) Uani 1 1 d . . . . .
H52 H 0.350121 0.662077 0.734263 0.044 Uiso 1 1 calc R U . . .
C3 C 0.16841(16) 0.9427(4) 0.9047(2) 0.0384(12) Uani 1 1 d . . . . .
H3 H 0.145624 0.971200 0.927927 0.046 Uiso 1 1 calc R U . . .
C15 C 0.08969(15) 0.5493(4) 0.5472(2) 0.0370(11) Uani 1 1 d . . . . .
H15 H 0.069671 0.517541 0.517556 0.044 Uiso 1 1 calc R U . . .
C6 C 0.13792(16) 0.9852(4) 0.7866(3) 0.0399(12) Uani 1 1 d . . . . .
H6A H 0.117604 1.016164 0.814103 0.048 Uiso 1 1 calc R U . . .
H6B H 0.144583 1.025327 0.746354 0.048 Uiso 1 1 calc R U . . .
C5 C 0.13424(15) 0.7915(4) 0.9139(3) 0.0372(11) Uani 1 1 d . . . . .
H5A H 0.114154 0.824439 0.940537 0.045 Uiso 1 1 calc R U . . .
H5B H 0.139422 0.733028 0.938613 0.045 Uiso 1 1 calc R U . . .
C42 C 0.38717(17) 1.0105(4) 0.8362(3) 0.0440(13) Uani 1 1 d . . . . .
H42A H 0.381911 1.048159 0.793536 0.053 Uiso 1 1 calc R U . . .
H42B H 0.405954 1.043919 0.866392 0.053 Uiso 1 1 calc R U . . .
C66 C 0.43502(15) 0.3015(4) 0.8548(3) 0.0381(11) Uani 1 1 d . . . . .
H66A H 0.441405 0.270176 0.899932 0.046 Uiso 1 1 calc R U . . .
H66B H 0.446528 0.363360 0.856866 0.046 Uiso 1 1 calc R U . . .
C50 C 0.31732(14) 0.6089(3) 0.8559(3) 0.0334(10) Uani 1 1 d . . . . .
H50A H 0.298910 0.610334 0.895504 0.040 Uiso 1 1 calc R U . . .
H50B H 0.343685 0.609533 0.876584 0.040 Uiso 1 1 calc R U . . .
C48 C 0.25616(17) 1.0875(4) 0.9011(3) 0.0426(12) Uani 1 1 d . . . . .
H48A H 0.251265 1.119317 0.946423 0.051 Uiso 1 1 calc R U . . .
H48B H 0.257741 1.134463 0.863518 0.051 Uiso 1 1 calc R U . . .
C45 C 0.30837(17) 0.9979(4) 0.9695(3) 0.0412(12) Uani 1 1 d . . . . .
H45 H 0.305346 1.037230 1.012414 0.049 Uiso 1 1 calc R U . . .
C9 C 0.07695(15) 0.7823(4) 0.7442(3) 0.0367(11) Uani 1 1 d . . . . .
H9 H 0.048543 0.793578 0.745766 0.044 Uiso 1 1 calc R U . . .
C12 C 0.07674(14) 0.7906(4) 0.6096(3) 0.0357(11) Uani 1 1 d . . . . .
H12A H 0.048300 0.788990 0.613174 0.043 Uiso 1 1 calc R U . . .
H12B H 0.083449 0.838697 0.575042 0.043 Uiso 1 1 calc R U . . .
C35 C 0.45037(17) 0.6326(4) 0.8061(3) 0.0497(15) Uani 1 1 d . . . . .
H35A H 0.478531 0.641103 0.801534 0.060 Uiso 1 1 calc R U . . .
H35B H 0.446210 0.584689 0.842277 0.060 Uiso 1 1 calc R U . . .
C41 C 0.39542(17) 0.8456(4) 0.9762(3) 0.0463(14) Uani 1 1 d . . . . .
H41A H 0.413899 0.889917 0.997025 0.056 Uiso 1 1 calc R U . . .
H41B H 0.394004 0.792826 1.008956 0.056 Uiso 1 1 calc R U . . .
C44 C 0.35102(17) 0.9827(4) 0.9514(3) 0.0415(13) Uani 1 1 d . . . . .
H44 H 0.368422 1.025496 0.977948 0.050 Uiso 1 1 calc R U . . .
C26 C 0.31617(16) 0.4293(4) 0.4885(3) 0.0390(12) Uani 1 1 d . . . . .
H26 H 0.319136 0.380372 0.451952 0.047 Uiso 1 1 calc R U . . .
C40 C 0.40970(18) 0.9088(4) 0.7437(3) 0.0483(14) Uani 1 1 d . . . . .
C21 C 0.21546(16) 0.4163(3) 0.4609(2) 0.0367(11) Uani 1 1 d . . . . .
H21 H 0.220330 0.369643 0.423306 0.044 Uiso 1 1 calc R U . . .
C23 C 0.26306(17) 0.3357(4) 0.5438(3) 0.0411(12) Uani 1 1 d . . . . .
H23A H 0.260851 0.300040 0.588188 0.049 Uiso 1 1 calc R U . . .
H23B H 0.267668 0.292013 0.504759 0.049 Uiso 1 1 calc R U . . .
C8 C 0.09906(15) 0.8403(4) 0.8013(2) 0.0343(11) Uani 1 1 d . . . . .
H8 H 0.080894 0.875617 0.831559 0.041 Uiso 1 1 calc R U . . .
O28 O 0.4427(2) 0.1229(4) 0.9867(4) 0.098(2) Uani 1 1 d G . . . .
H28A H 0.446400 0.074977 1.013179 0.147 Uiso 1 1 d G U . . .
H28B H 0.423824 0.123710 0.960369 0.147 Uiso 1 1 d DG U . . .
C58 C 0.20456(15) 0.5194(4) 0.7616(3) 0.0396(11) Uani 1 1 d . . . . .
H58 H 0.209675 0.479504 0.719698 0.047 Uiso 1 1 calc R U . . .
C39 C 0.42951(17) 0.8725(4) 0.8601(3) 0.0488(14) Uani 1 1 d . . . . .
H39 H 0.449142 0.912121 0.884268 0.059 Uiso 1 1 calc R U . . .
C18 C 0.13238(16) 0.5753(4) 0.4397(3) 0.0410(12) Uani 1 1 d . . . . .
H18A H 0.114858 0.531987 0.415047 0.049 Uiso 1 1 calc R U . . .
H18B H 0.136234 0.628274 0.408017 0.049 Uiso 1 1 calc R U . . .
C29 C 0.38603(17) 0.4259(4) 0.6384(3) 0.0425(12) Uani 1 1 d . . . . .
H29A H 0.404998 0.390443 0.610909 0.051 Uiso 1 1 calc R U . . .
H29B H 0.378718 0.388912 0.679996 0.051 Uiso 1 1 calc R U . . .
C47 C 0.25640(16) 0.8854(4) 1.0089(3) 0.0422(12) Uani 1 1 d . . . . .
H47A H 0.256712 0.823782 1.030606 0.051 Uiso 1 1 calc R U . . .
H47B H 0.250355 0.929994 1.046591 0.051 Uiso 1 1 calc R U . . .
C53 C 0.32789(16) 0.7860(4) 0.7096(3) 0.0394(12) Uani 1 1 d . . . . .
H53 H 0.341729 0.793561 0.666841 0.047 Uiso 1 1 calc R U . . .
C17 C 0.12593(17) 0.4008(4) 0.5694(3) 0.0429(13) Uani 1 1 d . . . . .
H17A H 0.108894 0.375049 0.531935 0.051 Uiso 1 1 calc R U . . .
H17B H 0.126803 0.356840 0.609275 0.051 Uiso 1 1 calc R U . . .
O21A O 0.4888(2) 0.2216(7) 0.8034(4) 0.056(2) Uani 0.6 1 d D . P A 1
C34 C 0.41217(17) 0.7168(4) 0.5893(3) 0.0518(16) Uani 1 1 d . . . . .
O25 O 0.2065(2) 0.3184(4) 0.8459(3) 0.096(2) Uani 1 1 d G . . . .
H25 H 0.206283 0.295348 0.800158 0.144 Uiso 1 1 d DG U . . .
C32 C 0.42831(16) 0.5672(4) 0.6179(3) 0.0456(13) Uani 1 1 d . . . . .
H32 H 0.447305 0.529603 0.591209 0.055 Uiso 1 1 calc R U . . .
C30 C 0.39320(18) 0.6026(5) 0.5006(3) 0.0573(17) Uani 1 1 d . . . . .
H30A H 0.390337 0.658589 0.471511 0.069 Uiso 1 1 calc R U . . .
H30B H 0.412703 0.563322 0.477839 0.069 Uiso 1 1 calc R U . . .
C28 C 0.32614(19) 0.5845(5) 0.4624(3) 0.0554(16) Uani 1 1 d . . . . .
C38 C 0.44838(18) 0.8059(4) 0.8077(4) 0.0536(15) Uani 1 1 d . . . . .
H38 H 0.477146 0.808443 0.811279 0.064 Uiso 1 1 calc R U . . .
C61 C 0.20443(15) 0.7579(4) 0.6717(3) 0.0438(13) Uani 1 1 d . . . . .
H61A H 0.180158 0.752478 0.644872 0.066 Uiso 1 1 calc R U . . .
H61B H 0.223049 0.792621 0.643864 0.066 Uiso 1 1 calc R U . . .
H61C H 0.199767 0.789667 0.716508 0.066 Uiso 1 1 calc R U . . .
C36 C 0.4507(2) 0.8045(4) 0.6734(4) 0.0615(18) Uani 1 1 d . . . . .
H36A H 0.446410 0.852044 0.636814 0.074 Uiso 1 1 calc R U . . .
H36B H 0.478824 0.796696 0.679848 0.074 Uiso 1 1 calc R U . . .
C62 C 0.22703(19) 0.6129(5) 0.6180(3) 0.0508(14) Uani 1 1 d . . . . .
H62A H 0.237666 0.552152 0.628026 0.076 Uiso 1 1 calc R U . . .
H62B H 0.245200 0.647538 0.589142 0.076 Uiso 1 1 calc R U . . .
H62C H 0.202481 0.606630 0.592210 0.076 Uiso 1 1 calc R U . . .
O35 O 0.3491(3) 0.7174(5) 0.2975(4) 0.105(3) Uani 0.75 1 d G . P . .
H35C H 0.352395 0.695263 0.342457 0.157 Uiso 0.75 1 d DG U P . .
O31 O 0.4935(3) 0.4283(6) 0.6974(6) 0.069(3) Uani 0.5 1 d G . P . .
H31A H 0.483954 0.414501 0.738362 0.103 Uiso 0.5 1 d DG U P . .
H31B H 0.517304 0.453551 0.697610 0.103 Uiso 0.5 1 d DG U P . .
O22A O 0.4705(2) 0.0561(7) 0.7328(5) 0.0753(12) Uani 0.6 1 d D . P B 1
O23A O 0.4734(2) 0.0671(7) 0.6147(4) 0.0753(12) Uani 0.6 1 d D . P B 1
C68 C 0.4444(2) 0.1708(6) 0.6822(4) 0.0753(12) Uani 1 1 d . . . . .
H68A H 0.421006 0.160566 0.652559 0.090 Uiso 0.6 1 calc R U P C 1
H68B H 0.459473 0.217958 0.657268 0.090 Uiso 0.6 1 calc R U P C 1
H68C H 0.460923 0.120538 0.700132 0.090 Uiso 0.4 1 calc R U P D 2
H68D H 0.421335 0.141011 0.660985 0.090 Uiso 0.4 1 calc R U P D 2
O26 O 0.4856(3) 0.0644(12) 0.8646(9) 0.134(7) Uani 0.5 1 d G . P . .
H26A H 0.468301 0.093892 0.836991 0.201 Uiso 0.5 1 d DG U P . .
O32 O 0.5458(4) 0.5517(11) 0.7452(9) 0.122(5) Uani 0.5 1 d D . P . .
C69A C 0.4649(3) 0.0944(11) 0.6756(7) 0.0753(12) Uani 0.6 1 d . . P B 1
C69B C 0.4630(5) 0.2049(17) 0.6285(10) 0.0753(12) Uani 0.4 1 d . . P B 2
O23B O 0.4676(3) 0.2867(11) 0.6322(7) 0.0753(12) Uani 0.4 1 d . . P B 2
O21B O 0.4868(3) 0.2780(9) 0.7802(7) 0.055(3) Uani 0.4 1 d D . P A 2
O22B O 0.4693(3) 0.1537(11) 0.5763(7) 0.0753(12) Uani 0.4 1 d D . P B 2
H33A H 0.278(2) 0.482(6) 0.741(4) 0.090 Uiso 1 1 d . U . . .
H36 H 0.387(2) 0.353(4) 0.821(4) 0.090 Uiso 1 1 d D U . . .
O27A O 0.4847(5) 0.1983(10) 0.5256(7) 0.111(4) Uani 0.5 1 d D . P E 1
O27B O 0.4775(8) -0.0035(13) 0.5856(12) 0.111(4) Uani 0.3 1 d G . P F 2
H27C H 0.475945 0.190974 0.578944 0.166 Uiso 0.5 1 d DG U P F 1
H27A H 0.464129 0.039702 0.565802 0.166 Uiso 0.3 1 d DG U P F 2
H27B H 0.501916 0.002337 0.595770 0.166 Uiso 0.3 1 d G U P F 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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 0 -12 0.0254
-11 -8 0 0.0763
0 0 12 0.0296
11 8 -1 0.0400
-7 -1 -11 0.0209
20 -5 -1 0.0300
7 1 11 0.0191
-20 5 1 0.0468
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
C63 N35 C64 120.5(4) . . ?
C25 N17 C26 112.1(4) . . ?
C25 N17 C23 122.4(4) . . ?
C23 N17 C26 122.0(4) . . ?
C13 N9 C11 122.6(4) . . ?
C13 N9 C14 113.1(4) . . ?
C11 N9 C14 123.7(4) . . ?
C1 N1 C2 111.0(4) . . ?
C1 N1 C47 118.9(4) . . ?
C47 N1 C2 120.4(4) . . ?
C4 N4 C3 111.3(4) . . ?
C4 N4 C6 119.5(4) . . ?
C3 N4 C6 120.8(4) . . ?
C7 N6 C11 122.3(5) . . ?
C7 N6 C9 113.3(4) . . ?
C9 N6 C11 122.8(4) . . ?
C19 N13 C20 113.0(4) . . ?
C19 N13 C17 122.1(4) . . ?
C20 N13 C17 123.0(5) . . ?
C13 N10 C15 112.4(4) . . ?
C13 N10 C17 122.0(4) . . ?
C17 N10 C15 123.0(4) . . ?
C1 N2 C3 111.9(4) . . ?
C1 N2 C5 121.3(4) . . ?
C5 N2 C3 123.0(5) . . ?
C10 N8 C9 113.0(4) . . ?
C10 N8 C12 122.2(4) . . ?
C9 N8 C12 122.3(4) . . ?
C57 N33 C49 124.0(4) . . ?
C24 N15 C21 122.3(4) . . ?
C22 N15 C24 121.5(4) . . ?
C22 N15 C21 110.4(4) . . ?
C65 N36 C66 123.6(4) . . ?
C43 N30 C45 112.3(4) . . ?
C43 N30 C47 121.5(4) . . ?
C45 N30 C47 122.8(5) . . ?
C67 N37 C68 124.4(5) . . ?
C43 N29 C41 123.3(5) . . ?
C43 N29 C44 112.7(5) . . ?
C44 N29 C41 124.0(4) . . ?
C16 N11 C14 112.9(4) . . ?
C16 N11 C12 121.2(4) . . ?
C14 N11 C12 122.8(4) . . ?
C25 N18 C27 110.9(4) . . ?
C25 N18 C29 121.0(4) . . ?
C29 N18 C27 121.5(4) . . ?
C10 N7 C6 121.2(4) . . ?
C10 N7 C8 111.9(4) . . ?
C6 N7 C8 122.4(4) . . ?
C16 N12 C15 113.2(4) . . ?
C16 N12 C18 122.8(4) . . ?
C15 N12 C18 123.3(5) . . ?
C7 N5 C5 120.2(4) . . ?
C7 N5 C8 111.9(4) . . ?
C8 N5 C5 121.4(4) . . ?
C31 N21 C29 121.6(4) . . ?
C31 N21 C32 111.5(5) . . ?
C29 N21 C32 123.2(5) . . ?
O5 C13 N9 126.1(5) . . ?
O5 C13 N10 125.6(5) . . ?
N10 C13 N9 108.3(4) . . ?
C4 N3 C2 112.2(4) . . ?
C4 N3 C48 125.0(4) . . ?
C48 N3 C2 121.6(4) . . ?
C19 N14 C21 113.3(5) . . ?
C19 N14 C23 121.8(4) . . ?
C21 N14 C23 123.0(4) . . ?
C31 N22 C33 112.0(5) . . ?
C31 N22 C35 123.0(5) . . ?
C35 N22 C33 123.9(5) . . ?
C46 N32 C48 122.3(4) . . ?
C46 N32 C45 111.9(5) . . ?
C45 N32 C48 125.6(4) . . ?
C37 N25 C35 122.7(5) . . ?
C37 N25 C38 112.0(5) . . ?
C35 N25 C38 121.1(5) . . ?
C42 N27 C39 122.9(5) . . ?
C40 N27 C42 119.5(5) . . ?
C40 N27 C39 112.7(5) . . ?
C34 N23 C32 112.0(5) . . ?
C34 N23 C30 120.7(5) . . ?
C32 N23 C30 123.9(5) . . ?
C22 N16 C20 112.8(4) . . ?
C22 N16 C18 122.8(4) . . ?
C20 N16 C18 122.2(5) . . ?
C46 N31 C42 121.7(4) . . ?
C46 N31 C44 110.6(5) . . ?
C42 N31 C44 122.7(5) . . ?
O19 C63 N35 121.6(4) . . ?
O19 C63 C49 122.5(4) . . ?
N35 C63 C49 115.8(4) . . ?
C51 C56 C55 121.3(4) . . ?
O15 C43 N30 126.1(5) . . ?
O15 C43 N29 126.1(6) . . ?
N29 C43 N30 107.8(5) . . ?
C54 C55 C56 119.3(5) . . ?
O3 C7 N6 126.3(5) . . ?
O3 C7 N5 125.9(5) . . ?
N6 C7 N5 107.9(5) . . ?
C24 N19 C26 122.7(5) . . ?
C28 N19 C24 122.3(5) . . ?
C28 N19 C26 112.0(5) . . ?
O20 C65 N36 124.3(5) . . ?
O20 C65 C64 118.6(4) . . ?
N36 C65 C64 117.0(4) . . ?
C37 N26 C41 122.3(5) . . ?
C37 N26 C39 112.5(5) . . ?
C41 N26 C39 123.8(5) . . ?
C56 C51 C52 118.3(4) . . ?
C56 C51 C50 120.5(4) . . ?
C52 C51 C50 121.2(4) . . ?
C34 N24 C33 112.7(5) . . ?
C34 N24 C36 121.7(5) . . ?
C36 N24 C33 123.5(5) . . ?
O17 C54 C55 121.4(5) . . ?
O17 C54 C53 118.6(4) . . ?
C55 C54 C53 120.0(4) . . ?
O18 C57 N33 123.9(4) . . ?
O18 C57 C58 119.4(4) . . ?
N33 C57 C58 116.7(4) . . ?
O6 C16 N11 127.2(5) . . ?
O6 C16 N12 125.9(5) . . ?
N11 C16 N12 106.9(4) . . ?
O13 C37 N25 126.8(6) . . ?
O13 C37 N26 125.4(6) . . ?
N26 C37 N25 107.8(5) . . ?
O1 C1 N1 126.9(5) . . ?
O1 C1 N2 125.3(5) . . ?
N1 C1 N2 107.7(4) . . ?
O9 C25 N17 125.7(5) . . ?
O9 C25 N18 125.1(5) . . ?
N17 C25 N18 109.2(4) . . ?
O7 C19 N13 127.2(5) . . ?
O7 C19 N14 125.8(5) . . ?
N14 C19 N13 107.0(4) . . ?
C60 C59 C58 115.5(4) . . ?
C61 C60 C59 107.4(4) . . ?
C62 C60 C59 113.9(5) . . ?
C62 C60 C61 109.7(4) . . ?
C30 N20 C27 121.4(5) . . ?
C28 N20 C27 112.5(5) . . ?
C28 N20 C30 122.0(5) . . ?
O11 C31 N21 126.7(5) . . ?
O11 C31 N22 124.7(5) . . ?
N21 C31 N22 108.6(4) . . ?
O4 C10 N8 126.4(5) . . ?
O4 C10 N7 125.3(5) . . ?
N8 C10 N7 108.3(4) . . ?
N15 C24 N19 113.4(4) . . ?
N33 C49 C63 112.1(4) . . ?
N33 C49 C50 114.7(4) . . ?
C63 C49 C50 111.3(4) . . ?
O8 C22 N15 124.4(5) . . ?
O8 C22 N16 126.7(5) . . ?
N16 C22 N15 108.9(4) . . ?
N35 C64 C65 114.9(4) . . ?
N6 C11 N9 113.9(4) . . ?
N37 C67 C66 119.3(5) . . ?
N37 C67 O21A 120.9(6) . . ?
O21A C67 C66 117.9(5) . . ?
O21B C67 N37 119.8(8) . . ?
O21B C67 C66 113.1(7) . . ?
N13 C20 N16 115.0(4) . . ?
N13 C20 C21 103.4(4) . . ?
N16 C20 C21 102.7(4) . . ?
N1 C2 N3 113.5(4) . . ?
N1 C2 C3 104.0(4) . . ?
N3 C2 C3 102.9(4) . . ?
N9 C14 C15 102.0(4) . . ?
N11 C14 N9 114.6(4) . . ?
N11 C14 C15 104.0(4) . . ?
C40 N28 C38 111.8(5) . . ?
C40 N28 C36 123.5(5) . . ?
C36 N28 C38 123.7(6) . . ?
O16 C46 N32 124.9(5) . . ?
O16 C46 N31 125.7(5) . . ?
N32 C46 N31 109.4(4) . . ?
N18 C27 C26 104.0(4) . . ?
N20 C27 N18 113.8(4) . . ?
N20 C27 C26 104.3(4) . . ?
N22 C33 N24 115.1(5) . . ?
N22 C33 C32 103.9(4) . . ?
N24 C33 C32 102.3(5) . . ?
O2 C4 N4 125.6(5) . . ?
O2 C4 N3 125.8(5) . . ?
N3 C4 N4 108.5(4) . . ?
C53 C52 C51 121.1(5) . . ?
N4 C3 C2 103.9(4) . . ?
N2 C3 N4 114.7(4) . . ?
N2 C3 C2 103.8(4) . . ?
N10 C15 C14 103.8(4) . . ?
N12 C15 N10 115.2(4) . . ?
N12 C15 C14 102.6(4) . . ?
N7 C6 N4 113.0(4) . . ?
N2 C5 N5 112.4(4) . . ?
N27 C42 N31 113.1(4) . . ?
N36 C66 C67 113.6(4) . . ?
C51 C50 C49 113.8(4) . . ?
N3 C48 N32 114.0(5) . . ?
N30 C45 C44 102.4(4) . . ?
N32 C45 N30 114.4(4) . . ?
N32 C45 C44 103.3(4) . . ?
N6 C9 N8 116.2(4) . . ?
N6 C9 C8 102.9(4) . . ?
N8 C9 C8 102.7(4) . . ?
N11 C12 N8 113.4(4) . . ?
N22 C35 N25 114.4(5) . . ?
N26 C41 N29 114.8(4) . . ?
N29 C44 N31 114.4(4) . . ?
N29 C44 C45 102.9(4) . . ?
N31 C44 C45 102.9(4) . . ?
N17 C26 N19 114.6(4) . . ?
N17 C26 C27 103.7(4) . . ?
N19 C26 C27 102.9(4) . . ?
O14 C40 N27 127.5(6) . . ?
O14 C40 N28 125.1(6) . . ?
N27 C40 N28 107.5(5) . . ?
N15 C21 C20 104.3(4) . . ?
N14 C21 N15 114.8(4) . . ?
N14 C21 C20 103.2(4) . . ?
N17 C23 N14 113.6(4) . . ?
N7 C8 C9 103.4(4) . . ?
N5 C8 N7 115.1(4) . . ?
N5 C8 C9 103.2(4) . . ?
C57 C58 C59 111.8(4) . . ?
N34 C58 C57 107.0(4) . . ?
N34 C58 C59 108.9(4) . . ?
N27 C39 C38 102.7(5) . . ?
N26 C39 N27 114.5(5) . . ?
N26 C39 C38 104.5(5) . . ?
N16 C18 N12 113.4(4) . . ?
N18 C29 N21 112.4(4) . . ?
N1 C47 N30 113.0(4) . . ?
C52 C53 C54 119.9(5) . . ?
N10 C17 N13 112.3(4) . . ?
N23 C34 N24 108.6(5) . . ?
O12 C34 N23 126.7(7) . . ?
O12 C34 N24 124.7(7) . . ?
N21 C32 C33 103.3(4) . . ?
N23 C32 N21 113.9(4) . . ?
N23 C32 C33 104.2(5) . . ?
N20 C30 N23 112.9(5) . . ?
O10 C28 N19 125.6(6) . . ?
O10 C28 N20 126.4(6) . . ?
N20 C28 N19 107.9(5) . . ?
N25 C38 C39 102.4(5) . . ?
N28 C38 N25 115.2(5) . . ?
N28 C38 C39 104.5(5) . . ?
N24 C36 N28 113.6(5) . . ?
C69A C68 N37 130.2(10) . . ?
C69B C68 N37 129.3(12) . . ?
O22A C69A O23A 128.4(15) . . ?
O22A C69A C68 112.3(10) . . ?
O23A C69A C68 119.1(14) . . ?
O23B C69B C68 113.5(15) . . ?
O23B C69B O22B 128(2) . . ?
O22B C69B C68 118(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
O19 C63 1.234(6) . ?
O3 C7 1.227(7) . ?
O5 C13 1.202(6) . ?
O17 C54 1.370(6) . ?
O6 C16 1.200(6) . ?
O4 C10 1.218(6) . ?
O9 C25 1.223(6) . ?
O16 C46 1.236(6) . ?
O18 C57 1.223(6) . ?
O11 C31 1.229(6) . ?
O1 C1 1.212(6) . ?
O7 C19 1.220(6) . ?
O8 C22 1.233(6) . ?
O20 C65 1.227(6) . ?
O14 C40 1.221(7) . ?
O15 C43 1.230(7) . ?
N35 C63 1.333(6) . ?
N35 C64 1.455(6) . ?
O13 C37 1.211(6) . ?
O2 C4 1.231(6) . ?
N17 C25 1.356(6) . ?
N17 C26 1.452(6) . ?
N17 C23 1.444(7) . ?
N9 C13 1.364(7) . ?
N9 C11 1.452(6) . ?
N9 C14 1.468(7) . ?
N1 C1 1.387(7) . ?
N1 C2 1.450(7) . ?
N1 C47 1.442(7) . ?
N4 C4 1.370(7) . ?
N4 C3 1.451(6) . ?
N4 C6 1.460(7) . ?
N6 C7 1.365(7) . ?
N6 C11 1.446(7) . ?
N6 C9 1.429(7) . ?
N13 C19 1.381(7) . ?
N13 C20 1.437(6) . ?
N13 C17 1.465(7) . ?
N10 C13 1.363(6) . ?
N10 C15 1.454(7) . ?
N10 C17 1.439(7) . ?
N2 C1 1.390(7) . ?
N2 C3 1.444(7) . ?
N2 C5 1.422(7) . ?
N8 C10 1.358(7) . ?
N8 C9 1.447(6) . ?
N8 C12 1.454(6) . ?
N33 C57 1.348(7) . ?
N33 C49 1.460(6) . ?
N15 C24 1.431(7) . ?
N15 C22 1.366(7) . ?
N15 C21 1.465(7) . ?
N36 C65 1.333(6) . ?
N36 C66 1.452(7) . ?
N30 C43 1.364(8) . ?
N30 C45 1.453(7) . ?
N30 C47 1.463(7) . ?
N37 C67 1.309(7) . ?
N37 C68 1.448(8) . ?
N29 C43 1.358(7) . ?
N29 C41 1.463(8) . ?
N29 C44 1.447(7) . ?
N11 C16 1.380(6) . ?
N11 C14 1.426(7) . ?
N11 C12 1.454(7) . ?
N18 C25 1.375(7) . ?
N18 C27 1.460(6) . ?
N18 C29 1.442(7) . ?
N7 C10 1.382(6) . ?
N7 C6 1.439(7) . ?
N7 C8 1.449(6) . ?
N12 C16 1.381(7) . ?
N12 C15 1.443(7) . ?
N12 C18 1.461(6) . ?
N5 C7 1.376(7) . ?
N5 C5 1.467(6) . ?
N5 C8 1.442(7) . ?
N21 C31 1.367(7) . ?
N21 C29 1.458(7) . ?
N21 C32 1.462(7) . ?
N3 C2 1.459(6) . ?
N3 C4 1.364(7) . ?
N3 C48 1.430(7) . ?
N14 C19 1.361(7) . ?
N14 C21 1.446(6) . ?
N14 C23 1.456(7) . ?
N22 C31 1.371(7) . ?
N22 C33 1.443(7) . ?
N22 C35 1.443(8) . ?
N32 C46 1.357(7) . ?
N32 C48 1.448(7) . ?
N32 C45 1.441(6) . ?
N25 C37 1.379(8) . ?
N25 C35 1.450(8) . ?
N25 C38 1.463(7) . ?
N27 C42 1.436(7) . ?
N27 C40 1.377(7) . ?
N27 C39 1.449(8) . ?
O10 C28 1.205(8) . ?
N23 C34 1.355(9) . ?
N23 C32 1.445(7) . ?
N23 C30 1.462(9) . ?
O12 C34 1.220(7) . ?
N16 C22 1.362(7) . ?
N16 C20 1.442(7) . ?
N16 C18 1.444(7) . ?
N31 C46 1.366(7) . ?
N31 C42 1.447(7) . ?
N31 C44 1.466(6) . ?
C63 C49 1.520(6) . ?
C56 C55 1.394(7) . ?
C56 C51 1.386(7) . ?
C55 C54 1.389(7) . ?
N19 C24 1.441(7) . ?
N19 C26 1.464(7) . ?
N19 C28 1.372(8) . ?
C65 C64 1.525(7) . ?
N26 C37 1.366(8) . ?
N26 C41 1.434(8) . ?
N26 C39 1.439(7) . ?
C51 C52 1.397(7) . ?
C51 C50 1.513(6) . ?
N24 C33 1.455(7) . ?
N24 C34 1.358(8) . ?
N24 C36 1.423(9) . ?
C54 C53 1.391(8) . ?
C57 C58 1.517(7) . ?
N34 C58 1.496(7) . ?
C59 C60 1.529(7) . ?
C59 C58 1.535(8) . ?
C60 C61 1.525(7) . ?
C60 C62 1.513(7) . ?
N20 C27 1.439(7) . ?
N20 C30 1.423(8) . ?
N20 C28 1.368(8) . ?
C49 C50 1.540(7) . ?
C67 C66 1.493(7) . ?
C67 O21A 1.324(9) . ?
C67 O21B 1.288(13) . ?
C20 C21 1.540(8) . ?
C2 C3 1.537(7) . ?
C14 C15 1.556(7) . ?
N28 C40 1.385(8) . ?
N28 C38 1.444(8) . ?
N28 C36 1.432(8) . ?
C27 C26 1.531(8) . ?
C33 C32 1.537(9) . ?
C52 C53 1.380(7) . ?
C45 C44 1.539(8) . ?
C9 C8 1.564(7) . ?
C39 C38 1.541(10) . ?
O22A C69A 1.230(17) . ?
O23A C69A 1.255(14) . ?
C68 C69A 1.332(17) . ?
C68 C69B 1.31(2) . ?
C69B O23B 1.21(3) . ?
C69B O22B 1.26(2) . ?
O27A O27A 1.44(3) 2_656 ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.84081
2 0.15919
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
-0.6944 0.2198 -12.2253 -0.1110 0.2630 0.9584
-10.6656 -8.3694 -0.0043 0.3658 -0.8858 0.2855
0.4462 -0.4143 12.2219 0.1195 -0.2835 -0.9515
10.5244 8.3427 -1.3411 -0.3758 0.9094 -0.1783
-7.0485 -1.3545 -11.4460 0.1564 0.0670 0.9854
19.5948 -4.6086 -1.2558 -0.9228 -0.3816 0.0535
7.3789 1.2701 11.3984 -0.1723 -0.0736 -0.9823
-19.6972 4.5646 0.9935 0.9236 0.3820 -0.0311
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 0.000 0.235 -0.514 639.0 238.0 '22 H2O'
2 0.189 0.112 0.381 9.2 0.0 ?
3 0.311 0.612 0.619 9.2 0.0 ?
4 0.500 0.735 -0.349 639.0 237.5 '22 H2O'
5 0.689 0.612 0.381 9.2 0.0 ?
6 0.811 0.112 0.619 9.2 0.0 ?
