#------------------------------------------------------------------------------
#$Date: 2023-04-04 12:46:11 +0300 (Tue, 04 Apr 2023) $
#$Revision: 282266 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/14/7131436.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_7131436
loop_
_publ_author_name
'Muang-Non, Phonlakrit'
'Markwell-Heys, Adrian W'
'Doonan, Christian J.'
'White, Nicholas G.'
_publ_section_title
;
 Charge "mis-matched" hydrogen bonded frameworks for cation exchange and
 dye sorption.
;
_journal_issue                   27
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4059
_journal_page_last               4062
_journal_paper_doi               10.1039/d3cc00553d
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C28 H16 B O8, 5(H2 O), 2.5(C14 H16 N4)'
_chemical_formula_sum            'C63 H66 B N10 O13'
_chemical_formula_weight         1182.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-31 deposited with the CCDC.	2023-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                110.045(3)
_cell_angle_beta                 110.898(3)
_cell_angle_gamma                96.920(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1697(4)
_cell_length_b                   14.5406(4)
_cell_length_c                   16.0657(5)
_cell_measurement_reflns_used    14684
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      60.9630
_cell_measurement_theta_min      3.5720
_cell_volume                     2791.70(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -107.00  -7.00   1.00    1.00    --  -36.03 -19.00 -90.00  100
  2  ω    -86.00  -6.00   1.00    1.00    --  -36.03 125.00   0.00   80
  3  ω   -103.00 -19.00   1.00    1.00    --  -36.03 -57.00-150.00   84
  4  ω    103.00 153.00   1.00    6.00    --   85.19  77.00 -30.00   50
  5  ω     17.00 103.00   1.00    6.00    --   85.19 -45.00-120.00   86
  6  ω     18.00 103.00   1.00    6.00    --   85.19 -61.00  60.00   85
  7  ω     16.00 106.00   1.00    6.00    --   85.19 -95.00 -90.00   90
  8  ω     16.00 106.00   1.00    6.00    --   85.19 -95.00-180.00   90
  9  ω     15.00 107.00   1.00    6.00    --   85.19 -30.00 -60.00   92
 10  ω     18.00 112.00   1.00    6.00    --   85.19 -77.00-150.00   94
 11  ω     16.00 106.00   1.00    6.00    --   85.19 -95.00  30.00   90
 12  ω     16.00 154.00   1.00    6.00    --   85.19   0.00 -30.00  138
 13  ω   -103.00 -19.00   1.00    1.00    --  -36.03 -57.00 120.00   84
 14  ω   -103.00 -19.00   1.00    1.00    --  -36.03 -57.00  60.00   84
 15  ω    -53.00  31.00   1.00    1.00    --  -36.03  57.00-120.00   84
 16  ω     67.00 152.00   1.00    6.00    --   85.19  61.00   0.00   85
 17  ω     67.00 152.00   1.00    6.00    --   85.19  61.00 150.00   85
 18  ω     67.00 152.00   1.00    6.00    --   85.19  61.00-180.00   85
 19  ω     64.00 155.00   1.00    6.00    --   85.19  30.00 150.00   91
 20  ω     67.00 152.00   1.00    6.00    --   85.19  61.00  90.00   85
 21  ω     68.00 154.00   1.00    6.00    --   85.19  45.00-120.00   86
 22  ω     68.00 154.00   1.00    6.00    --   85.19  45.00 -30.00   86
 23  ω     67.00 152.00   1.00    6.00    --   85.19  61.00 -90.00   85
 24  ω     68.00 154.00   1.00    6.00    --   85.19  45.00  60.00   86
 25  ω   -103.00 -19.00   1.00    1.00    --  -36.03 -57.00 150.00   84
 26  ω   -103.00 -19.00   1.00    1.00    --  -36.03 -57.00   0.00   84
 27  ω   -103.00 -19.00   1.00    1.00    --  -36.03 -57.00 -60.00   84
 28  ω     67.00 152.00   1.00    6.00    --   85.19  61.00  60.00   85
 29  ω     67.00 152.00   1.00    6.00    --   85.19  61.00-120.00   85
 30  ω     67.00 152.00   1.00    6.00    --   85.19  61.00 -30.00   85
 31  ω     67.00 152.00   1.00    6.00    --   85.19  61.00 120.00   85
 32  ω     67.00 152.00   1.00    6.00    --   85.19  61.00  30.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0648795000
_diffrn_orient_matrix_UB_12      0.0649099000
_diffrn_orient_matrix_UB_13      -0.0296206000
_diffrn_orient_matrix_UB_21      0.0423661000
_diffrn_orient_matrix_UB_22      0.0878169000
_diffrn_orient_matrix_UB_23      0.1025652000
_diffrn_orient_matrix_UB_31      0.0930676000
_diffrn_orient_matrix_UB_32      -0.0429877000
_diffrn_orient_matrix_UB_33      0.0366383000
_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  0.0417
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40019
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        58.935
_diffrn_reflns_theta_max         58.935
_diffrn_reflns_theta_min         3.474
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             1246
_exptl_crystal_recrystallization_method
'Crystallised using diphenylbisamidinium.2Cl with TBA5.tetraboratecarboxylate in H2O. Final concentration = 2 mM.'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         8003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0488P)²+1.5095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6891
_reflns_number_total             8003
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc00553d2.cif
_cod_data_source_block           2_B
_cod_depositor_comments
'Adding full bibliography for 7131429--7131437.cif.'
_cod_original_cell_volume        2791.70(16)
_cod_database_code               7131436
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H50N50O50B25
_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   0.908
_shelx_estimated_absorpt_t_min   0.828
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O100(H10C,H10D), O130(H13C,H13D), O140(H14A,H14B), O120(H12C,H12D), O110(H11C,
 H11D)
2.b Aromatic/amide H refined with riding coordinates:
 C53(H53), C70(H70), C62(H62), C52(H52), C59(H59), C76(H76), C73(H73),
 C66(H66), C67(H67), C60(H60), C55(H55), C32(H32), C74(H74), C77(H77), C56(H56),
  C69(H69), C63(H63), C45(H45), C31(H31), C25(H25), C46(H46), C9(H9), C3(H3),
 C22(H22), C12(H12), C4(H4), C26(H26), C10(H10), C6(H6), C29(H29), C28(H28),
 C43(H43), C13(H13), C23(H23), C42(H42), C7(H7)
2.c X=CH2 refined with riding coordinates:
 N20(H20A,H20B), N21(H21A,H21B), N12(H12A,H12B), N13(H13A,H13B), N3(H3A,H3B),
 N4(H4A,H4B), N11(H11A,H11B), N10(H10A,H10B), N2(H2A,H2B), N1(H1A,H1B)
;
_ins_header
;
TITL PMN-C-21-H2O-repro in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  14.169663  14.540633  16.065734 110.0445 110.8977  96.9201
ZERR    1.00   0.000397   0.000406   0.000456   0.0026   0.0026   0.0023
LATT  1
SFAC C H B N O
UNIT 50.00 50.00 25.00 50.00 50.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.12 0.18 0.24
TREF
HKLF 4
END
;
_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 1.227
_oxdiff_exptl_absorpt_empirical_full_min 0.763
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
O1 O 0.28629(10) 0.07331(10) 1.01991(9) 0.0196(3) Uani 1 1 d . . . . .
O2 O 0.12892(10) 0.09424(10) 1.00410(10) 0.0203(3) Uani 1 1 d . . . . .
O6 O 0.46381(11) 0.14327(10) 0.54000(10) 0.0246(3) Uani 1 1 d . . . . .
O5 O 0.57083(11) 0.29550(10) 0.59130(10) 0.0242(3) Uani 1 1 d . . . . .
O4 O 0.47821(11) 0.92581(10) 1.10553(11) 0.0273(3) Uani 1 1 d . . . . .
O8 O -0.18056(11) 0.35828(10) 0.46633(10) 0.0247(3) Uani 1 1 d . . . . .
O7 O -0.20215(11) 0.46782(11) 0.58907(10) 0.0259(3) Uani 1 1 d . . . . .
O3 O 0.45120(11) 0.87950(11) 1.21550(10) 0.0282(3) Uani 1 1 d . . . . .
O100 O 0.46779(12) 0.11181(11) 0.19818(11) 0.0323(4) Uani 1 1 d G . . . .
H10C H 0.469599 0.049076 0.172866 0.049 Uiso 1 1 d G U . . .
H10D H 0.419679 0.118672 0.150540 0.049 Uiso 1 1 d G U . . .
O130 O 0.66884(13) 0.60630(12) 0.83626(11) 0.0349(4) Uani 1 1 d G . . . .
H13C H 0.699227 0.562591 0.811963 0.052 Uiso 1 1 d G U . . .
H13D H 0.608877 0.569121 0.824702 0.052 Uiso 1 1 d G U . . .
O140 O 0.72301(12) 0.46736(13) 0.37093(12) 0.0369(4) Uani 1 1 d G . . . .
H14A H 0.763267 0.436412 0.399617 0.055 Uiso 1 1 d G U . . .
H14B H 0.763134 0.503641 0.356695 0.055 Uiso 1 1 d G U . . .
O120 O 0.73824(12) 0.45782(12) 0.72998(11) 0.0336(4) Uani 1 1 d G . . . .
H12C H 0.761540 0.469122 0.690063 0.050 Uiso 1 1 d G U . . .
H12D H 0.679431 0.410065 0.691911 0.050 Uiso 1 1 d G U . . .
N20 N 0.77635(13) 0.12806(13) 0.98876(12) 0.0219(4) Uani 1 1 d . . . . .
H20A H 0.753255 0.066157 0.982841 0.026 Uiso 1 1 calc R U . . .
H20B H 0.736085 0.169628 0.990241 0.026 Uiso 1 1 calc R U . . .
N21 N 0.93071(13) 0.09649(12) 0.99314(12) 0.0218(4) Uani 1 1 d . . . . .
H21A H 0.907462 0.034628 0.987226 0.026 Uiso 1 1 calc R U . . .
H21B H 0.994092 0.116661 0.997561 0.026 Uiso 1 1 calc R U . . .
N12 N -0.33400(13) 0.05282(12) 0.13507(12) 0.0225(4) Uani 1 1 d . . . . .
H12A H -0.401176 0.032964 0.120747 0.027 Uiso 1 1 calc R U . . .
H12B H -0.307429 0.015829 0.098026 0.027 Uiso 1 1 calc R U . . .
N13 N -0.31201(13) 0.19388(13) 0.26787(12) 0.0236(4) Uani 1 1 d . . . . .
H13A H -0.379094 0.174623 0.254121 0.028 Uiso 1 1 calc R U . . .
H13B H -0.270802 0.250619 0.319083 0.028 Uiso 1 1 calc R U . . .
N3 N 0.67932(14) 0.20556(13) 0.48719(13) 0.0271(4) Uani 1 1 d . . . . .
H3A H 0.631189 0.227676 0.504620 0.033 Uiso 1 1 calc R U . . .
H3B H 0.730550 0.248613 0.489578 0.033 Uiso 1 1 calc R U . . .
N4 N 0.59790(14) 0.04480(13) 0.45437(13) 0.0263(4) Uani 1 1 d . . . . .
H4A H 0.550051 0.067482 0.471917 0.032 Uiso 1 1 calc R U . . .
H4B H 0.594290 -0.020472 0.434637 0.032 Uiso 1 1 calc R U . . .
N11 N 0.57013(13) 0.38824(13) 0.46684(13) 0.0272(4) Uani 1 1 d . . . . .
H11A H 0.635127 0.417041 0.480168 0.033 Uiso 1 1 calc R U . . .
H11B H 0.556290 0.373980 0.510974 0.033 Uiso 1 1 calc R U . . .
N10 N 0.51047(14) 0.38628(14) 0.31311(14) 0.0288(4) Uani 1 1 d . . . . .
H10A H 0.574618 0.415060 0.324221 0.035 Uiso 1 1 calc R U . . .
H10B H 0.457636 0.370814 0.256348 0.035 Uiso 1 1 calc R U . . .
N2 N 1.34011(15) 0.01879(15) 0.29283(14) 0.0345(5) Uani 1 1 d . . . . .
H2A H 1.391610 0.005443 0.276536 0.041 Uiso 1 1 calc R U . . .
H2B H 1.329231 0.079371 0.304763 0.041 Uiso 1 1 calc R U . . .
C51 C 0.23082(15) 0.19704(13) 0.96157(13) 0.0158(4) Uani 1 1 d . . . . .
C61 C 0.33304(14) 0.54148(14) 0.91908(14) 0.0159(4) Uani 1 1 d . . . . .
N1 N 1.29627(16) -0.14134(15) 0.28150(15) 0.0373(5) Uani 1 1 d . . . . .
H1A H 1.347884 -0.154282 0.265231 0.045 Uiso 1 1 calc R U . . .
H1B H 1.255884 -0.188852 0.285756 0.045 Uiso 1 1 calc R U . . .
C50 C 0.21456(15) 0.11691(13) 0.99848(13) 0.0158(4) Uani 1 1 d . . . . .
C44 C 0.98074(15) 0.45070(14) 1.00158(13) 0.0166(4) Uani 1 1 d . . . . .
C54 C 0.25683(15) 0.34536(13) 0.88546(13) 0.0156(4) Uani 1 1 d . . . . .
C65 C 0.44002(15) 0.28667(14) 0.65066(13) 0.0167(4) Uani 1 1 d . . . . .
C33 C -0.27330(15) 0.13780(14) 0.21183(14) 0.0186(4) Uani 1 1 d . . . . .
C58 C 0.41661(14) 0.74921(14) 1.06040(14) 0.0174(4) Uani 1 1 d . . . . .
C53 C 0.16359(15) 0.31112(14) 0.89038(13) 0.0175(4) Uani 1 1 d . . . . .
H53 H 0.106647 0.338109 0.867674 0.021 Uiso 1 1 calc R U . . .
C70 C 0.47391(15) 0.39061(14) 0.70998(14) 0.0177(4) Uani 1 1 d . . . . .
H70 H 0.530979 0.432191 0.709919 0.021 Uiso 1 1 calc R U . . .
C71 C -0.14758(15) 0.41769(14) 0.55627(14) 0.0189(4) Uani 1 1 d . . . . .
C40 C 0.87109(15) 0.15845(14) 0.99538(13) 0.0177(4) Uani 1 1 d . . . . .
C62 C 0.36757(15) 0.56894(14) 1.01975(14) 0.0176(4) Uani 1 1 d . . . . .
H62 H 0.364090 0.516472 1.041987 0.021 Uiso 1 1 calc R U . . .
C57 C 0.45298(15) 0.85956(15) 1.13333(14) 0.0193(4) Uani 1 1 d . . . . .
C64 C 0.49400(15) 0.23772(14) 0.58975(14) 0.0186(4) Uani 1 1 d . . . . .
C72 C -0.03972(15) 0.42440(14) 0.62486(14) 0.0178(4) Uani 1 1 d . . . . .
C75 C 0.16046(15) 0.42402(13) 0.75652(13) 0.0156(4) Uani 1 1 d . . . . .
C52 C 0.15032(15) 0.23894(14) 0.92719(13) 0.0169(4) Uani 1 1 d . . . . .
H52 H 0.085045 0.218081 0.928776 0.020 Uiso 1 1 calc R U . . .
C59 C 0.38726(15) 0.72433(14) 0.96061(14) 0.0186(4) Uani 1 1 d . . . . .
H59 H 0.396064 0.776881 0.939337 0.022 Uiso 1 1 calc R U . . .
C41 C 0.90903(15) 0.26173(14) 1.00266(14) 0.0182(4) Uani 1 1 d . . . . .
C76 C 0.09671(15) 0.48073(14) 0.78904(14) 0.0191(4) Uani 1 1 d . . . . .
H76 H 0.121246 0.520464 0.857296 0.023 Uiso 1 1 calc R U . . .
C30 C -0.16023(15) 0.17016(15) 0.23641(14) 0.0188(4) Uani 1 1 d . . . . .
C73 C 0.02295(15) 0.37083(14) 0.59017(14) 0.0192(4) Uani 1 1 d . . . . .
H73 H -0.000531 0.333795 0.521613 0.023 Uiso 1 1 calc R U . . .
C27 C 0.05644(15) 0.22591(15) 0.28807(14) 0.0195(4) Uani 1 1 d . . . . .
C66 C 0.35562(15) 0.22857(14) 0.65224(14) 0.0183(4) Uani 1 1 d . . . . .
H66 H 0.330424 0.157350 0.612535 0.022 Uiso 1 1 calc R U . . .
C67 C 0.30822(15) 0.27354(14) 0.71099(14) 0.0187(4) Uani 1 1 d . . . . .
H67 H 0.250785 0.231641 0.710266 0.022 Uiso 1 1 calc R U . . .
C24 C 0.17042(15) 0.25541(14) 0.31533(14) 0.0197(4) Uani 1 1 d . . . . .
O110 O 0.84339(17) 0.30638(15) 0.72617(16) 0.0556(5) Uani 1 1 d G . . . .
H11C H 0.811476 0.353960 0.726990 0.083 Uiso 1 1 d G U . . .
H11D H 0.906137 0.334183 0.735114 0.083 Uiso 1 1 d G U . . .
C11 C 0.76016(16) 0.07635(14) 0.43282(14) 0.0196(4) Uani 1 1 d . . . . .
C60 C 0.34557(15) 0.62383(14) 0.89292(14) 0.0176(4) Uani 1 1 d . . . . .
H60 H 0.324351 0.609564 0.825598 0.021 Uiso 1 1 calc R U . . .
C68 C 0.34073(15) 0.37829(14) 0.77188(13) 0.0162(4) Uani 1 1 d . . . . .
C55 C 0.33838(15) 0.30477(15) 0.92465(14) 0.0196(4) Uani 1 1 d . . . . .
H55 H 0.404874 0.328359 0.926428 0.024 Uiso 1 1 calc R U . . .
C32 C -0.00446(16) 0.12507(15) 0.22855(14) 0.0202(4) Uani 1 1 d . . . . .
H32 H 0.027544 0.074942 0.204029 0.024 Uiso 1 1 calc R U . . .
C74 C 0.11952(15) 0.37063(14) 0.65430(14) 0.0188(4) Uani 1 1 d . . . . .
H74 H 0.159798 0.332540 0.627733 0.023 Uiso 1 1 calc R U . . .
C77 C 0.00023(16) 0.48119(15) 0.72624(14) 0.0211(4) Uani 1 1 d . . . . .
H77 H -0.039595 0.520588 0.752193 0.025 Uiso 1 1 calc R U . . .
C56 C 0.32695(15) 0.23204(14) 0.96092(14) 0.0189(4) Uani 1 1 d . . . . .
H56 H 0.384267 0.206120 0.985223 0.023 Uiso 1 1 calc R U . . .
C69 C 0.42599(15) 0.43485(14) 0.76931(13) 0.0167(4) Uani 1 1 d . . . . .
H69 H 0.452025 0.505950 0.809525 0.020 Uiso 1 1 calc R U . . .
C63 C 0.40684(15) 0.66998(14) 1.08874(14) 0.0185(4) Uani 1 1 d . . . . .
H63 H 0.427169 0.684694 1.156052 0.022 Uiso 1 1 calc R U . . .
C45 C 1.04858(16) 0.40972(15) 1.05594(14) 0.0208(4) Uani 1 1 d . . . . .
H45 H 1.120686 0.446639 1.093701 0.025 Uiso 1 1 calc R U . . .
C5 C 1.02226(16) 0.00793(15) 0.37194(14) 0.0207(4) Uani 1 1 d . . . . .
C31 C -0.11003(15) 0.09748(15) 0.20501(14) 0.0197(4) Uani 1 1 d . . . . .
H31 H -0.149349 0.028020 0.166864 0.024 Uiso 1 1 calc R U . . .
C25 C 0.20845(16) 0.21852(15) 0.24515(14) 0.0221(4) Uani 1 1 d . . . . .
H25 H 0.161561 0.169257 0.181283 0.027 Uiso 1 1 calc R U . . .
C46 C 1.01442(16) 0.31711(15) 1.05672(14) 0.0208(4) Uani 1 1 d . . . . .
H46 H 1.062957 0.291116 1.094247 0.025 Uiso 1 1 calc R U . . .
C8 C 0.93116(16) 0.02962(14) 0.39322(14) 0.0192(4) Uani 1 1 d . . . . .
C14 C 0.67472(16) 0.10838(15) 0.45764(14) 0.0205(4) Uani 1 1 d . . . . .
C9 C 0.94676(16) 0.10874(15) 0.48016(15) 0.0217(4) Uani 1 1 d . . . . .
H9 H 1.016424 0.146767 0.527405 0.026 Uiso 1 1 calc R U . . .
C3 C 1.20255(16) 0.06313(15) 0.39600(15) 0.0232(5) Uani 1 1 d . . . . .
H3 H 1.267492 0.114619 0.428870 0.028 Uiso 1 1 calc R U . . .
C22 C 0.34824(16) 0.35357(15) 0.43384(15) 0.0228(4) Uani 1 1 d . . . . .
H22 H 0.396672 0.397034 0.499361 0.027 Uiso 1 1 calc R U . . .
C12 C 0.74256(16) -0.00459(15) 0.34612(14) 0.0214(4) Uani 1 1 d . . . . .
H12 H 0.672909 -0.044612 0.300608 0.026 Uiso 1 1 calc R U . . .
C4 C 1.11933(16) 0.08157(15) 0.41861(14) 0.0226(4) Uani 1 1 d . . . . .
H4 H 1.128241 0.145995 0.467173 0.027 Uiso 1 1 calc R U . . .
C26 C 0.31334(16) 0.25245(15) 0.26697(15) 0.0230(5) Uani 1 1 d . . . . .
H26 H 0.337390 0.228449 0.217457 0.028 Uiso 1 1 calc R U . . .
C2 C 1.19140(16) -0.03098(16) 0.32495(15) 0.0238(5) Uani 1 1 d . . . . .
C21 C 0.38390(16) 0.32161(15) 0.36113(15) 0.0213(4) Uani 1 1 d . . . . .
C10 C 0.86332(16) 0.13307(15) 0.49913(15) 0.0222(4) Uani 1 1 d . . . . .
H10 H 0.876159 0.189019 0.557949 0.027 Uiso 1 1 calc R U . . .
C20 C 0.49367(16) 0.36650(15) 0.38096(16) 0.0235(5) Uani 1 1 d . . . . .
C6 C 1.01278(17) -0.08592(16) 0.30185(15) 0.0256(5) Uani 1 1 d . . . . .
H6 H 0.948253 -0.137882 0.269538 0.031 Uiso 1 1 calc R U . . .
C29 C -0.10067(16) 0.27150(15) 0.29339(15) 0.0227(4) Uani 1 1 d . . . . .
H29 H -0.133766 0.322295 0.314105 0.027 Uiso 1 1 calc R U . . .
C28 C 0.00600(16) 0.29843(15) 0.31986(15) 0.0233(5) Uani 1 1 d . . . . .
H28 H 0.045881 0.367416 0.360360 0.028 Uiso 1 1 calc R U . . .
C43 C 0.87472(16) 0.39629(16) 0.95127(16) 0.0249(5) Uani 1 1 d . . . . .
H43 H 0.825644 0.423356 0.915641 0.030 Uiso 1 1 calc R U . . .
C13 C 0.82681(16) -0.02648(15) 0.32650(14) 0.0210(4) Uani 1 1 d . . . . .
H13 H 0.813844 -0.080725 0.266505 0.025 Uiso 1 1 calc R U . . .
C23 C 0.24256(16) 0.32223(15) 0.41094(15) 0.0215(4) Uani 1 1 d . . . . .
H23 H 0.218593 0.346240 0.460518 0.026 Uiso 1 1 calc R U . . .
C42 C 0.83941(16) 0.30384(15) 0.95208(15) 0.0235(5) Uani 1 1 d . . . . .
H42 H 0.766630 0.268770 0.917596 0.028 Uiso 1 1 calc R U . . .
C1 C 1.27959(17) -0.05156(16) 0.29934(15) 0.0266(5) Uani 1 1 d . . . . .
C7 C 1.09551(17) -0.10485(16) 0.27842(15) 0.0281(5) Uani 1 1 d . . . . .
H7 H 1.086670 -0.169244 0.229852 0.034 Uiso 1 1 calc R U . . .
B1 B 0.27439(17) 0.42381(16) 0.83491(15) 0.0161(5) 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'
B B 0.0090 0.0039 '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
6 -7 1 0.0902
5 -1 5 0.0911
0 6 4 0.0648
-5 -1 -5 0.1292
1 -7 -4 0.0938
-3 -7 9 0.0867
4 7 -9 0.0286
-9 0 4 0.0820
-6 -6 8 0.0883
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
H10C O100 H10D 104.5 . . ?
H13C O130 H13D 104.5 . . ?
H14A O140 H14B 104.5 . . ?
H12C O120 H12D 104.5 . . ?
H20A N20 H20B 120.0 . . ?
C40 N20 H20A 120.0 . . ?
C40 N20 H20B 120.0 . . ?
H21A N21 H21B 120.0 . . ?
C40 N21 H21A 120.0 . . ?
C40 N21 H21B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
C33 N12 H12A 120.0 . . ?
C33 N12 H12B 120.0 . . ?
H13A N13 H13B 120.0 . . ?
C33 N13 H13A 120.0 . . ?
C33 N13 H13B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C14 N3 H3A 120.0 . . ?
C14 N3 H3B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C14 N4 H4A 120.0 . . ?
C14 N4 H4B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C20 N11 H11A 120.0 . . ?
C20 N11 H11B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C20 N10 H10A 120.0 . . ?
C20 N10 H10B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
C52 C51 C50 120.67(16) . . ?
C52 C51 C56 117.76(17) . . ?
C56 C51 C50 121.57(17) . . ?
C62 C61 C60 114.83(17) . . ?
C62 C61 B1 123.91(16) . . ?
C60 C61 B1 121.13(16) . . ?
H1A N1 H1B 120.0 . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
O1 C50 C51 118.57(16) . . ?
O2 C50 O1 122.97(17) . . ?
O2 C50 C51 118.44(17) . . ?
C45 C44 C44 121.7(2) . 2_767 ?
C45 C44 C43 116.88(18) . . ?
C43 C44 C44 121.4(2) . 2_767 ?
C53 C54 C55 114.72(17) . . ?
C53 C54 B1 125.05(17) . . ?
C55 C54 B1 120.19(16) . . ?
C70 C65 C64 121.67(17) . . ?
C70 C65 C66 117.54(17) . . ?
C66 C65 C64 120.76(17) . . ?
N12 C33 N13 120.64(18) . . ?
N12 C33 C30 119.83(17) . . ?
N13 C33 C30 119.53(17) . . ?
C59 C58 C57 120.41(17) . . ?
C63 C58 C57 121.67(17) . . ?
C63 C58 C59 117.86(17) . . ?
C54 C53 H53 118.6 . . ?
C54 C53 C52 122.80(18) . . ?
C52 C53 H53 118.6 . . ?
C65 C70 H70 119.3 . . ?
C69 C70 C65 121.33(17) . . ?
C69 C70 H70 119.3 . . ?
O8 C71 C72 117.48(17) . . ?
O7 C71 O8 122.78(18) . . ?
O7 C71 C72 119.71(17) . . ?
N20 C40 C41 120.06(17) . . ?
N21 C40 N20 119.85(17) . . ?
N21 C40 C41 120.07(17) . . ?
C61 C62 H62 118.6 . . ?
C63 C62 C61 122.81(18) . . ?
C63 C62 H62 118.6 . . ?
O4 C57 O3 124.26(18) . . ?
O4 C57 C58 117.16(17) . . ?
O3 C57 C58 118.48(17) . . ?
O6 C64 O5 122.44(17) . . ?
O6 C64 C65 119.95(16) . . ?
O5 C64 C65 117.61(16) . . ?
C73 C72 C71 120.84(17) . . ?
C73 C72 C77 117.37(18) . . ?
C77 C72 C71 121.74(18) . . ?
C76 C75 B1 121.29(16) . . ?
C74 C75 C76 114.40(18) . . ?
C74 C75 B1 124.30(17) . . ?
C51 C52 C53 121.14(17) . . ?
C51 C52 H52 119.4 . . ?
C53 C52 H52 119.4 . . ?
C58 C59 H59 119.8 . . ?
C60 C59 C58 120.43(18) . . ?
C60 C59 H59 119.8 . . ?
C46 C41 C40 121.66(18) . . ?
C42 C41 C40 119.86(17) . . ?
C42 C41 C46 118.45(18) . . ?
C75 C76 H76 118.5 . . ?
C77 C76 C75 123.06(17) . . ?
C77 C76 H76 118.5 . . ?
C31 C30 C33 119.61(17) . . ?
C29 C30 C33 121.77(18) . . ?
C29 C30 C31 118.58(18) . . ?
C72 C73 H73 119.5 . . ?
C72 C73 C74 120.94(18) . . ?
C74 C73 H73 119.5 . . ?
C32 C27 C24 121.04(18) . . ?
C32 C27 C28 118.03(18) . . ?
C28 C27 C24 120.93(17) . . ?
C65 C66 H66 119.7 . . ?
C67 C66 C65 120.58(18) . . ?
C67 C66 H66 119.7 . . ?
C66 C67 H67 118.4 . . ?
C66 C67 C68 123.25(17) . . ?
C68 C67 H67 118.4 . . ?
C25 C24 C27 120.20(18) . . ?
C25 C24 C23 118.31(18) . . ?
C23 C24 C27 121.48(17) . . ?
H11C O110 H11D 104.5 . . ?
C12 C11 C14 123.56(18) . . ?
C12 C11 C10 118.96(18) . . ?
C10 C11 C14 117.44(17) . . ?
C61 C60 H60 118.4 . . ?
C59 C60 C61 123.12(17) . . ?
C59 C60 H60 118.4 . . ?
C67 C68 B1 118.69(16) . . ?
C69 C68 C67 115.04(17) . . ?
C69 C68 B1 126.22(16) . . ?
C54 C55 H55 118.2 . . ?
C56 C55 C54 123.58(17) . . ?
C56 C55 H55 118.2 . . ?
C27 C32 H32 119.6 . . ?
C31 C32 C27 120.90(19) . . ?
C31 C32 H32 119.6 . . ?
C75 C74 H74 118.4 . . ?
C73 C74 C75 123.18(18) . . ?
C73 C74 H74 118.4 . . ?
C72 C77 H77 119.5 . . ?
C76 C77 C72 120.97(18) . . ?
C76 C77 H77 119.5 . . ?
C51 C56 H56 120.1 . . ?
C55 C56 C51 119.90(18) . . ?
C55 C56 H56 120.1 . . ?
C70 C69 C68 122.26(17) . . ?
C70 C69 H69 118.9 . . ?
C68 C69 H69 118.9 . . ?
C58 C63 C62 120.85(17) . . ?
C58 C63 H63 119.6 . . ?
C62 C63 H63 119.6 . . ?
C44 C45 H45 119.0 . . ?
C46 C45 C44 122.10(18) . . ?
C46 C45 H45 119.0 . . ?
C4 C5 C8 121.70(18) . . ?
C6 C5 C8 120.99(18) . . ?
C6 C5 C4 117.28(18) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 C30 120.88(18) . . ?
C32 C31 H31 119.6 . . ?
C24 C25 H25 119.5 . . ?
C26 C25 C24 121.00(18) . . ?
C26 C25 H25 119.5 . . ?
C41 C46 H46 119.9 . . ?
C45 C46 C41 120.19(19) . . ?
C45 C46 H46 119.9 . . ?
C9 C8 C5 120.57(18) . . ?
C9 C8 C13 117.38(18) . . ?
C13 C8 C5 122.03(17) . . ?
N3 C14 N4 119.48(18) . . ?
N3 C14 C11 117.50(17) . . ?
N4 C14 C11 122.98(18) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 C8 121.44(19) . . ?
C10 C9 H9 119.3 . . ?
C4 C3 H3 119.9 . . ?
C4 C3 C2 120.15(19) . . ?
C2 C3 H3 119.9 . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C23 C22 C21 120.22(18) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.87(18) . . ?
C13 C12 H12 120.1 . . ?
C5 C4 H4 119.1 . . ?
C3 C4 C5 121.82(19) . . ?
C3 C4 H4 119.1 . . ?
C25 C26 H26 119.9 . . ?
C25 C26 C21 120.29(18) . . ?
C21 C26 H26 119.9 . . ?
C3 C2 C1 120.77(18) . . ?
C7 C2 C3 118.54(19) . . ?
C7 C2 C1 120.69(18) . . ?
C22 C21 C20 120.83(18) . . ?
C26 C21 C22 119.24(18) . . ?
C26 C21 C20 119.75(18) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 C11 120.67(18) . . ?
C9 C10 H10 119.7 . . ?
N11 C20 C21 119.26(18) . . ?
N10 C20 N11 122.16(19) . . ?
N10 C20 C21 118.55(19) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.28(19) . . ?
C7 C6 H6 119.4 . . ?
C30 C29 H29 119.8 . . ?
C28 C29 C30 120.42(19) . . ?
C28 C29 H29 119.8 . . ?
C27 C28 H28 119.4 . . ?
C29 C28 C27 121.13(18) . . ?
C29 C28 H28 119.4 . . ?
C44 C43 H43 119.3 . . ?
C42 C43 C44 121.49(19) . . ?
C42 C43 H43 119.3 . . ?
C8 C13 H13 119.2 . . ?
C12 C13 C8 121.64(18) . . ?
C12 C13 H13 119.2 . . ?
C24 C23 H23 119.7 . . ?
C22 C23 C24 120.70(18) . . ?
C22 C23 H23 119.7 . . ?
C41 C42 H42 119.6 . . ?
C43 C42 C41 120.76(19) . . ?
C43 C42 H42 119.6 . . ?
N2 C1 C2 120.7(2) . . ?
N1 C1 N2 119.6(2) . . ?
N1 C1 C2 119.66(19) . . ?
C2 C7 H7 119.5 . . ?
C6 C7 C2 120.93(19) . . ?
C6 C7 H7 119.5 . . ?
C61 B1 C54 110.69(15) . . ?
C61 B1 C75 107.43(15) . . ?
C61 B1 C68 113.91(15) . . ?
C54 B1 C75 111.04(15) . . ?
C68 B1 C54 106.32(15) . . ?
C68 B1 C75 107.45(15) . . ?
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
O1 C50 1.268(2) . ?
O2 C50 1.262(2) . ?
O6 C64 1.253(2) . ?
O5 C64 1.280(2) . ?
O4 C57 1.257(2) . ?
O8 C71 1.272(2) . ?
O7 C71 1.253(2) . ?
O3 C57 1.261(2) . ?
O100 H10C 0.8701 . ?
O100 H10D 0.8700 . ?
O130 H13C 0.8703 . ?
O130 H13D 0.8698 . ?
O140 H14A 0.8700 . ?
O140 H14B 0.8701 . ?
O120 H12C 0.8702 . ?
O120 H12D 0.8698 . ?
N20 H20A 0.8800 . ?
N20 H20B 0.8800 . ?
N20 C40 1.316(3) . ?
N21 H21A 0.8800 . ?
N21 H21B 0.8800 . ?
N21 C40 1.307(3) . ?
N12 H12A 0.8800 . ?
N12 H12B 0.8800 . ?
N12 C33 1.315(3) . ?
N13 H13A 0.8800 . ?
N13 H13B 0.8800 . ?
N13 C33 1.316(3) . ?
N3 H3A 0.8800 . ?
N3 H3B 0.8800 . ?
N3 C14 1.312(3) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N4 C14 1.314(3) . ?
N11 H11A 0.8800 . ?
N11 H11B 0.8800 . ?
N11 C20 1.315(3) . ?
N10 H10A 0.8800 . ?
N10 H10B 0.8800 . ?
N10 C20 1.308(3) . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
N2 C1 1.311(3) . ?
C51 C50 1.506(3) . ?
C51 C52 1.388(3) . ?
C51 C56 1.401(3) . ?
C61 C62 1.400(3) . ?
C61 C60 1.410(3) . ?
C61 B1 1.648(3) . ?
N1 H1A 0.8800 . ?
N1 H1B 0.8800 . ?
N1 C1 1.307(3) . ?
C44 C44 1.496(4) 2_767 ?
C44 C45 1.392(3) . ?
C44 C43 1.395(3) . ?
C54 C53 1.394(3) . ?
C54 C55 1.407(3) . ?
C54 B1 1.653(3) . ?
C65 C70 1.391(3) . ?
C65 C64 1.496(3) . ?
C65 C66 1.392(3) . ?
C33 C30 1.478(3) . ?
C58 C57 1.515(3) . ?
C58 C59 1.402(3) . ?
C58 C63 1.386(3) . ?
C53 H53 0.9500 . ?
C53 C52 1.394(3) . ?
C70 H70 0.9500 . ?
C70 C69 1.389(3) . ?
C71 C72 1.500(3) . ?
C40 C41 1.483(3) . ?
C62 H62 0.9500 . ?
C62 C63 1.394(3) . ?
C72 C73 1.389(3) . ?
C72 C77 1.401(3) . ?
C75 C76 1.411(3) . ?
C75 C74 1.405(3) . ?
C75 B1 1.657(3) . ?
C52 H52 0.9500 . ?
C59 H59 0.9500 . ?
C59 C60 1.383(3) . ?
C41 C46 1.392(3) . ?
C41 C42 1.387(3) . ?
C76 H76 0.9500 . ?
C76 C77 1.382(3) . ?
C30 C31 1.396(3) . ?
C30 C29 1.395(3) . ?
C73 H73 0.9500 . ?
C73 C74 1.390(3) . ?
C27 C24 1.478(3) . ?
C27 C32 1.398(3) . ?
C27 C28 1.399(3) . ?
C66 H66 0.9500 . ?
C66 C67 1.380(3) . ?
C67 H67 0.9500 . ?
C67 C68 1.406(3) . ?
C24 C25 1.392(3) . ?
C24 C23 1.402(3) . ?
O110 H11C 0.8699 . ?
O110 H11D 0.8700 . ?
C11 C14 1.482(3) . ?
C11 C12 1.395(3) . ?
C11 C10 1.396(3) . ?
C60 H60 0.9500 . ?
C68 C69 1.399(3) . ?
C68 B1 1.648(3) . ?
C55 H55 0.9500 . ?
C55 C56 1.390(3) . ?
C32 H32 0.9500 . ?
C32 C31 1.374(3) . ?
C74 H74 0.9500 . ?
C77 H77 0.9500 . ?
C56 H56 0.9500 . ?
C69 H69 0.9500 . ?
C63 H63 0.9500 . ?
C45 H45 0.9500 . ?
C45 C46 1.381(3) . ?
C5 C8 1.490(3) . ?
C5 C4 1.400(3) . ?
C5 C6 1.394(3) . ?
C31 H31 0.9500 . ?
C25 H25 0.9500 . ?
C25 C26 1.381(3) . ?
C46 H46 0.9500 . ?
C8 C9 1.393(3) . ?
C8 C13 1.407(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.378(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.382(3) . ?
C3 C2 1.396(3) . ?
C22 H22 0.9500 . ?
C22 C21 1.393(3) . ?
C22 C23 1.383(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.385(3) . ?
C4 H4 0.9500 . ?
C26 H26 0.9500 . ?
C26 C21 1.391(3) . ?
C2 C1 1.481(3) . ?
C2 C7 1.390(3) . ?
C21 C20 1.485(3) . ?
C10 H10 0.9500 . ?
C6 H6 0.9500 . ?
C6 C7 1.383(3) . ?
C29 H29 0.9500 . ?
C29 C28 1.380(3) . ?
C28 H28 0.9500 . ?
C43 H43 0.9500 . ?
C43 C42 1.383(3) . ?
C13 H13 0.9500 . ?
C23 H23 0.9500 . ?
C42 H42 0.9500 . ?
C7 H7 0.9500 . ?
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
O8 C71 C72 C73 2.7(3) . . . . ?
O8 C71 C72 C77 -174.74(17) . . . . ?
O7 C71 C72 C73 -179.02(17) . . . . ?
O7 C71 C72 C77 3.6(3) . . . . ?
N20 C40 C41 C46 146.70(19) . . . . ?
N20 C40 C41 C42 -35.5(3) . . . . ?
N21 C40 C41 C46 -34.9(3) . . . . ?
N21 C40 C41 C42 142.81(19) . . . . ?
N12 C33 C30 C31 -24.4(3) . . . . ?
N12 C33 C30 C29 157.92(19) . . . . ?
N13 C33 C30 C31 154.82(19) . . . . ?
N13 C33 C30 C29 -22.9(3) . . . . ?
C61 C62 C63 C58 -2.0(3) . . . . ?
C50 C51 C52 C53 -178.23(16) . . . . ?
C50 C51 C56 C55 178.85(17) . . . . ?
C44 C44 C45 C46 -177.8(2) 2_767 . . . ?
C44 C44 C43 C42 178.3(2) 2_767 . . . ?
C44 C45 C46 C41 -0.5(3) . . . . ?
C44 C43 C42 C41 -0.5(3) . . . . ?
C54 C53 C52 C51 0.1(3) . . . . ?
C54 C55 C56 C51 -1.4(3) . . . . ?
C65 C70 C69 C68 -0.9(3) . . . . ?
C65 C66 C67 C68 0.0(3) . . . . ?
C33 C30 C31 C32 -178.61(18) . . . . ?
C33 C30 C29 C28 176.22(18) . . . . ?
C58 C59 C60 C61 -2.0(3) . . . . ?
C53 C54 C55 C56 3.4(3) . . . . ?
C53 C54 B1 C61 98.4(2) . . . . ?
C53 C54 B1 C75 -20.9(2) . . . . ?
C53 C54 B1 C68 -137.43(18) . . . . ?
C70 C65 C64 O6 177.32(18) . . . . ?
C70 C65 C64 O5 -2.4(3) . . . . ?
C70 C65 C66 C67 -0.1(3) . . . . ?
C71 C72 C73 C74 -174.98(17) . . . . ?
C71 C72 C77 C76 175.36(17) . . . . ?
C40 C41 C46 C45 175.03(18) . . . . ?
C40 C41 C42 C43 -174.56(18) . . . . ?
C62 C61 C60 C59 -0.9(3) . . . . ?
C62 C61 B1 C54 3.0(3) . . . . ?
C62 C61 B1 C75 124.43(19) . . . . ?
C62 C61 B1 C68 -116.7(2) . . . . ?
C57 C58 C59 C60 -174.43(17) . . . . ?
C57 C58 C63 C62 176.31(17) . . . . ?
C64 C65 C70 C69 -177.40(18) . . . . ?
C64 C65 C66 C67 177.88(18) . . . . ?
C72 C73 C74 C75 -0.6(3) . . . . ?
C75 C76 C77 C72 -0.3(3) . . . . ?
C52 C51 C50 O1 172.98(16) . . . . ?
C52 C51 C50 O2 -5.1(2) . . . . ?
C52 C51 C56 C55 -1.4(3) . . . . ?
C59 C58 C57 O4 -15.7(3) . . . . ?
C59 C58 C57 O3 160.90(18) . . . . ?
C59 C58 C63 C62 -0.9(3) . . . . ?
C76 C75 C74 C73 -1.8(3) . . . . ?
C76 C75 B1 C61 -41.3(2) . . . . ?
C76 C75 B1 C54 79.9(2) . . . . ?
C76 C75 B1 C68 -164.24(16) . . . . ?
C30 C29 C28 C27 1.9(3) . . . . ?
C73 C72 C77 C76 -2.2(3) . . . . ?
C27 C24 C25 C26 174.01(19) . . . . ?
C27 C24 C23 C22 -176.30(19) . . . . ?
C27 C32 C31 C30 2.8(3) . . . . ?
C66 C65 C70 C69 0.5(3) . . . . ?
C66 C65 C64 O6 -0.6(3) . . . . ?
C66 C65 C64 O5 179.76(18) . . . . ?
C66 C67 C68 C69 -0.3(3) . . . . ?
C66 C67 C68 B1 177.28(18) . . . . ?
C67 C68 C69 C70 0.7(3) . . . . ?
C67 C68 B1 C61 168.55(17) . . . . ?
C67 C68 B1 C54 46.4(2) . . . . ?
C67 C68 B1 C75 -72.6(2) . . . . ?
C24 C27 C32 C31 178.63(18) . . . . ?
C24 C27 C28 C29 179.03(18) . . . . ?
C24 C25 C26 C21 2.5(3) . . . . ?
C11 C12 C13 C8 1.5(3) . . . . ?
C60 C61 C62 C63 2.8(3) . . . . ?
C60 C61 B1 C54 -172.58(16) . . . . ?
C60 C61 B1 C75 -51.2(2) . . . . ?
C60 C61 B1 C68 67.7(2) . . . . ?
C55 C54 C53 C52 -2.7(3) . . . . ?
C55 C54 B1 C61 -84.0(2) . . . . ?
C55 C54 B1 C75 156.74(16) . . . . ?
C55 C54 B1 C68 40.2(2) . . . . ?
C32 C27 C24 C25 43.9(3) . . . . ?
C32 C27 C24 C23 -137.4(2) . . . . ?
C32 C27 C28 C29 0.0(3) . . . . ?
C74 C75 C76 C77 2.2(3) . . . . ?
C74 C75 B1 C61 137.88(17) . . . . ?
C74 C75 B1 C54 -101.0(2) . . . . ?
C74 C75 B1 C68 14.9(2) . . . . ?
C77 C72 C73 C74 2.6(3) . . . . ?
C56 C51 C50 O1 -7.2(3) . . . . ?
C56 C51 C50 O2 174.69(17) . . . . ?
C56 C51 C52 C53 2.0(3) . . . . ?
C69 C68 B1 C61 -14.2(3) . . . . ?
C69 C68 B1 C54 -136.37(18) . . . . ?
C69 C68 B1 C75 104.7(2) . . . . ?
C63 C58 C57 O4 167.14(18) . . . . ?
C63 C58 C57 O3 -16.3(3) . . . . ?
C63 C58 C59 C60 2.8(3) . . . . ?
C45 C44 C43 C42 -2.6(3) . . . . ?
C5 C8 C9 C10 176.89(18) . . . . ?
C5 C8 C13 C12 -178.80(18) . . . . ?
C5 C6 C7 C2 0.7(3) . . . . ?
C31 C30 C29 C28 -1.5(3) . . . . ?
C25 C24 C23 C22 2.4(3) . . . . ?
C25 C26 C21 C22 2.1(3) . . . . ?
C25 C26 C21 C20 -173.04(19) . . . . ?
C46 C41 C42 C43 3.3(3) . . . . ?
C8 C5 C4 C3 -177.19(19) . . . . ?
C8 C5 C6 C7 176.9(2) . . . . ?
C8 C9 C10 C11 2.3(3) . . . . ?
C14 C11 C12 C13 176.93(18) . . . . ?
C14 C11 C10 C9 -178.95(18) . . . . ?
C9 C8 C13 C12 -0.2(3) . . . . ?
C3 C2 C1 N2 -39.8(3) . . . . ?
C3 C2 C1 N1 141.3(2) . . . . ?
C3 C2 C7 C6 -0.1(3) . . . . ?
C22 C21 C20 N11 38.1(3) . . . . ?
C22 C21 C20 N10 -139.6(2) . . . . ?
C12 C11 C14 N3 -130.6(2) . . . . ?
C12 C11 C14 N4 51.7(3) . . . . ?
C12 C11 C10 C9 -1.0(3) . . . . ?
C4 C5 C8 C9 -21.1(3) . . . . ?
C4 C5 C8 C13 157.40(19) . . . . ?
C4 C5 C6 C7 -0.9(3) . . . . ?
C4 C3 C2 C1 179.48(19) . . . . ?
C4 C3 C2 C7 -0.2(3) . . . . ?
C26 C21 C20 N11 -146.8(2) . . . . ?
C26 C21 C20 N10 35.5(3) . . . . ?
C2 C3 C4 C5 -0.1(3) . . . . ?
C21 C22 C23 C24 2.1(3) . . . . ?
C10 C11 C14 N3 47.3(3) . . . . ?
C10 C11 C14 N4 -130.4(2) . . . . ?
C10 C11 C12 C13 -0.9(3) . . . . ?
C6 C5 C8 C9 161.1(2) . . . . ?
C6 C5 C8 C13 -20.3(3) . . . . ?
C6 C5 C4 C3 0.6(3) . . . . ?
C29 C30 C31 C32 -0.8(3) . . . . ?
C28 C27 C24 C25 -135.1(2) . . . . ?
C28 C27 C24 C23 43.6(3) . . . . ?
C28 C27 C32 C31 -2.4(3) . . . . ?
C43 C44 C45 C46 3.2(3) . . . . ?
C13 C8 C9 C10 -1.7(3) . . . . ?
C23 C24 C25 C26 -4.7(3) . . . . ?
C23 C22 C21 C26 -4.4(3) . . . . ?
C23 C22 C21 C20 170.72(19) . . . . ?
C42 C41 C46 C45 -2.7(3) . . . . ?
C1 C2 C7 C6 -179.8(2) . . . . ?
C7 C2 C1 N2 139.9(2) . . . . ?
C7 C2 C1 N1 -39.0(3) . . . . ?
B1 C61 C62 C63 -173.02(18) . . . . ?
B1 C61 C60 C59 175.14(18) . . . . ?
B1 C54 C53 C52 175.00(17) . . . . ?
B1 C54 C55 C56 -174.47(17) . . . . ?
B1 C75 C76 C77 -178.57(17) . . . . ?
B1 C75 C74 C73 179.01(17) . . . . ?
B1 C68 C69 C70 -176.61(18) . . . . ?
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
6.4603 -7.4629 0.5206 -0.0807 -0.3283 0.9411
5.3236 -0.5065 5.0049 0.1643 0.6944 0.7006
-0.3364 5.9337 4.4692 0.2309 0.9652 -0.1226
-4.5029 -0.7864 -5.2184 -0.1886 -0.7951 -0.5765
1.4894 -6.7319 -3.9436 -0.2235 -0.9326 0.2835
-3.4389 -7.1223 8.7279 -0.9440 0.1240 0.3059
3.7858 6.9506 -8.7380 0.9556 -0.1255 -0.2666
-9.1642 0.3958 4.3163 -0.6967 0.0892 -0.7118
-5.8177 -5.5999 8.4604 -0.9915 0.1295 0.0093
