#------------------------------------------------------------------------------
#$Date: 2024-07-05 19:46:21 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293119 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/57/7715776.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_7715776
loop_
_publ_author_name
'Beckmann, J. Louis'
'Neumann, Beate'
'Stammler, Hans-Georg'
'Lamm, Jan-Hendrik'
'Mitzel, Norbert W.'
_publ_section_title
;
 Bidentate boron Lewis acids: synthesis by tin boron exchange reaction and
 host-guest complex formation.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7958
_journal_page_last               7964
_journal_paper_doi               10.1039/d4dt00782d
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C44 H34 B2 N2'
_chemical_formula_sum            'C44 H34 B2 N2'
_chemical_formula_weight         612.35
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-04
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-03-04 deposited with the CCDC.	2024-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.4546(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.17085(16)
_cell_length_b                   18.4947(2)
_cell_length_c                   16.5929(2)
_cell_measurement_reflns_used    37804
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.1320
_cell_measurement_theta_min      3.5810
_cell_volume                     3359.84(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -15.00   1.00    7.50    --  -38.50 -19.00-120.00  101
  2  ω    -53.00  33.00   1.00    7.50    --  -38.50  37.00 -60.00   86
  3  ω    -57.00  19.00   1.00    7.50    --  -38.50  37.00-120.00   76
  4  ω    -58.00  31.00   1.00    7.50    --  -38.50  37.00  60.00   89
  5  ω     12.00  39.00   1.00    7.50    --   42.70  80.00 -17.54   27
  6  ω     13.00  40.00   1.00    7.50    --   42.70  77.00 -77.86   27
  7  ω     14.00 112.00   1.00    7.50    --   42.70  70.00 131.72   98
  8  ω     28.00  97.00   1.00    7.50    --   42.70-125.00 -30.00   69
  9  ω     21.00  92.00   1.00    7.50    --   42.70  51.00  10.00   71
 10  ω     13.00  38.00   1.00    7.50    --   42.70  77.00-165.55   25
 11  ω     12.00  42.00   1.00    7.50    --   42.70  82.00 103.72   30
 12  ω     13.00  42.00   1.00    7.50    --   42.70  80.00-136.67   29
 13  ω     75.00 103.00   1.00    7.50    --   42.70  57.00  90.00   28
 14  ω     22.00  75.00   1.00    7.50    --   42.70  37.00 -90.00   53
 15  ω     22.00  64.00   1.00    7.50    --   42.70  57.00 -60.00   42
 16  ω     11.00  38.00   1.00    7.50    --   42.70  81.00  34.29   27
 17  ω      7.00  67.00   1.00    7.50    --   42.70 -99.00 120.00   60
 18  ω     18.00  59.00   1.00    7.50    --   42.70  57.00  90.00   41
 19  ω     84.00 178.00   1.00   31.50    --  111.00  66.00 121.95   94
 20  ω     85.00 113.00   1.00   31.50    --  111.00  61.00 -65.58   28
 21  ω     85.00 112.00   1.00   31.50    --  111.00  62.00 141.26   27
 22  ω    128.00 155.00   1.00   31.50    --  111.00  61.00 -10.95   27
 23  ω     84.00 110.00   1.00   31.50    --  111.00  64.00  74.93   26
 24  ω     89.00 116.00   1.00   31.50    --  111.00  45.00 -30.00   27
 25  ω    134.00 176.00   1.00   31.50    --  111.00  64.00  74.93   42
 26  ω     87.00 154.00   1.00   31.50    --  111.00  53.00 -67.43   67
 27  ω     42.00  74.00   1.00   31.50    --  111.00-137.00 -92.37   32
 28  ω     95.00 122.00   1.00   31.50    --  111.00-137.00 -92.37   27
 29  ω     54.00 124.00   1.00   31.50    --  111.00-140.00 -36.18   70
 30  ω     59.00 113.00   1.00   31.50    --  111.00-125.00  30.00   54
 31  ω    125.00 176.00   1.00   31.50    --  111.00  65.00 -41.29   51
 32  ω     85.00 112.00   1.00   31.50    --  111.00  61.00 -10.95   27
 33  ω     86.00 113.00   1.00   31.50    --  111.00  58.00 -92.10   27
 34  ω     84.00 111.00   1.00   31.50    --  111.00  65.00 -41.29   27
 35  ω    117.00 145.00   1.00   31.50    --  111.00  58.00 168.29   28
 36  ω     86.00 174.00   1.00   31.50    --  111.00  55.00 178.69   88
 37  ω     86.00 114.00   1.00   31.50    --  111.00  58.00 168.29   28
 38  ω     56.00 137.00   1.00   31.50    --  111.00 -61.00   0.00   81
 39  ω     83.00 109.00   1.00   31.50    --  111.00  68.00  30.98   26
 40  ω     86.00 112.00   1.00   31.50    --  111.00  56.00  28.72   26
 41  ω     86.00 114.00   1.00   31.50    --  111.00  55.00  73.93   28
 42  ω     58.00 137.00   1.00   31.50    --  111.00 -61.00 120.00   79
 43  ω     86.00 176.00   1.00   31.50    --  111.00  61.00 -60.00   90
 44  ω     89.00 118.00   1.00   31.50    --  111.00  45.00 -90.00   29
 45  ω     85.00 112.00   1.00   31.50    --  111.00  61.00   0.00   27
 46  ω     90.00 115.00   1.00   31.50    --  111.00  45.00-150.00   25
 47  ω     44.00 113.00   1.00   31.50    --  111.00-125.00   0.00   69
 48  ω     85.00 111.00   1.00   31.50    --  111.00  61.00-120.00   26
 49  ω    121.00 177.00   1.00   31.50    --  111.00  61.00-120.00   56
 50  ω     85.00 115.00   1.00   31.50    --  111.00  61.00 120.00   30
 51  ω     85.00 178.00   1.00   31.50    --  111.00  61.00  60.00   93
 52  ω     85.00 112.00   1.00   31.50    --  111.00  61.00 -30.00   27
 53  ω     85.00 112.00   1.00   31.50    --  111.00  61.00  90.00   27
 54  ω     90.00 178.00   1.00   31.50    --  111.00  45.00  30.00   88
 55  ω     85.00 123.00   1.00   31.50    --  111.00  61.00 150.00   38
 56  ω     86.00 143.00   1.00   31.50    --  111.00  61.00 -90.00   57
 57  ω     83.00 175.00   1.00   31.50    --  111.00  70.00-160.15   92
 58  ω    151.00 176.00   1.00   31.50    --  111.00  71.00-146.18   25
 59  ω     83.00 110.00   1.00   31.50    --  111.00  69.00 175.00   27
 60  ω     82.00 108.00   1.00   31.50    --  111.00  71.00-146.18   26
 61  ω     42.00 112.00   1.00   31.50    --  111.00-125.00  60.00   70
 62  ω     36.00  61.00   1.00   31.50    --  111.00 -94.00  60.00   25
 63  ω     41.00 113.00   1.00   31.50    --  111.00-125.00-180.00   72
 64  ω     78.00 106.00   1.00   31.50    --  111.00 -94.00  60.00   28
 65  ω     84.00 114.00   1.00   31.50    --  111.00  64.00 -22.39   30
 66  ω     87.00 113.00   1.00   31.50    --  111.00  52.00  60.34   26
 67  ω     86.00 143.00   1.00   31.50    --  111.00  58.00 108.90   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1297677000
_diffrn_orient_matrix_UB_12      -0.0242056000
_diffrn_orient_matrix_UB_13      0.0063614000
_diffrn_orient_matrix_UB_21      0.0080896000
_diffrn_orient_matrix_UB_22      0.0458966000
_diffrn_orient_matrix_UB_23      0.0783473000
_diffrn_orient_matrix_UB_31      -0.0539496000
_diffrn_orient_matrix_UB_32      0.0651270000
_diffrn_orient_matrix_UB_33      -0.0528932000
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            65174
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.326
_diffrn_reflns_theta_min         2.717
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_exptl_crystal_size_rad          0.050
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.4(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         13796
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0880P)²+3.0439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1791
_refine_ls_wR_factor_ref         0.1800
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                13520
_reflns_number_total             13796
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00782d2.cif
_cod_data_source_block           3ax2Py
_cod_depositor_comments
'Adding full bibliography for 7715770--7715781.cif.'
_cod_original_cell_volume        3359.85(8)
_cod_database_code               7715776
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C44H34B2N2
_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   0.984
_shelx_estimated_absorpt_t_min   0.921
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     42.10
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6(7)
 0.4(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C62B) = Uanis(C62A)
Uanis(C67B) = Uanis(C67A)
Uanis(C68A) = Uanis(C68B)
Uanis(C61A) = Uanis(C61B)
Uanis(C63A) = Uanis(C63B)
Uanis(C64A) = Uanis(C64B)
Uanis(C65B) = Uanis(C65A)
Uanis(C66B) = Uanis(C66A)
4. Others
 Sof(C61B)=Sof(H61C)=Sof(H61D)=Sof(C62B)=Sof(C63B)=Sof(H63B)=Sof(C64B)=
 Sof(H64B)=Sof(C65B)=Sof(H65B)=Sof(C66B)=Sof(H66B)=Sof(C67B)=Sof(C68B)=
 Sof(H68C)=Sof(H68D)=1-FVAR(1)
 Sof(C61A)=Sof(H61A)=Sof(H61B)=Sof(C62A)=Sof(C63A)=Sof(H63A)=Sof(C64A)=
 Sof(H64A)=Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(H66A)=Sof(C67A)=Sof(C68A)=
 Sof(H68A)=Sof(H68B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C24(H24A,H24B), C32(H32A,H32B), C39(H39A,H39B), C61A(H61A,
 H61B), C61B(H61C,H61D), C68A(H68A,H68B), C68B(H68C,H68D), C76(H76A,H76B),
 C83(H83A,H83B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14),
 C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C41(H41),
 C42(H42), C43(H43), C44(H44), C47(H47), C50(H50), C51(H51), C52(H52), C54(H54),
  C56(H56), C57(H57), C58(H58), C63A(H63A), C63B(H63B), C64A(H64A), C64B(H64B),
 C65A(H65A), C65B(H65B), C66A(H66A), C66B(H66B), C69(H69), C70(H70), C71(H71),
 C72(H72), C73(H73), C78(H78), C79(H79), C80(H80), C81(H81), C84(H84), C85(H85),
  C86(H86), C87(H87), C88(H88)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.121
_oxdiff_exptl_absorpt_empirical_full_min 0.870
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
N1 N 0.2714(3) 0.7084(2) 0.2751(2) 0.0226(7) Uani 1 1 d . . . . .
N2 N 0.7046(3) 0.68405(18) 0.6524(2) 0.0200(6) Uani 1 1 d . . . . .
N3 N 0.4188(3) 0.2874(2) -0.0840(2) 0.0270(8) Uani 1 1 d . . . . .
N4 N 0.8615(3) 0.30866(19) 0.3000(2) 0.0218(7) Uani 1 1 d . . . . .
C1 C 0.0169(4) 0.5822(2) 0.4372(3) 0.0290(9) Uani 1 1 d . . . . .
C2 C 0.0595(4) 0.5524(2) 0.5178(3) 0.0262(9) Uani 1 1 d . . . . .
C3 C 0.1742(4) 0.5703(2) 0.5659(3) 0.0252(8) Uani 1 1 d . . . . .
H3 H 0.223245 0.605646 0.546450 0.030 Uiso 1 1 calc R . . . .
C4 C 0.2174(4) 0.5370(2) 0.6415(3) 0.0244(8) Uani 1 1 d . . . . .
C5 C 0.3408(4) 0.5472(2) 0.6865(3) 0.0259(9) Uani 1 1 d . . . . .
C6 C 0.3782(4) 0.5139(3) 0.7607(3) 0.0323(10) Uani 1 1 d . . . . .
H6 H 0.459042 0.521569 0.790373 0.039 Uiso 1 1 calc R . . . .
C7 C 0.2990(4) 0.4682(3) 0.7943(3) 0.0338(10) Uani 1 1 d . . . . .
H7 H 0.326635 0.446508 0.846579 0.041 Uiso 1 1 calc R . . . .
C8 C 0.1830(4) 0.4549(3) 0.7519(3) 0.0329(10) Uani 1 1 d . . . . .
H8 H 0.131146 0.423564 0.774700 0.039 Uiso 1 1 calc R . . . .
C9 C 0.1392(4) 0.4876(2) 0.6741(3) 0.0281(9) Uani 1 1 d . . . . .
C10 C 0.0250(4) 0.4705(2) 0.6259(3) 0.0305(9) Uani 1 1 d . . . . .
H10 H -0.027309 0.438604 0.647503 0.037 Uiso 1 1 calc R . . . .
C11 C -0.0146(4) 0.4989(2) 0.5469(3) 0.0280(9) Uani 1 1 d . . . . .
C12 C -0.1240(4) 0.4744(3) 0.4942(3) 0.0344(10) Uani 1 1 d . . . . .
H12 H -0.174256 0.439936 0.514011 0.041 Uiso 1 1 calc R . . . .
C13 C -0.1570(4) 0.5000(3) 0.4157(3) 0.0356(11) Uani 1 1 d . . . . .
H13 H -0.227204 0.480896 0.380170 0.043 Uiso 1 1 calc R . . . .
C14 C -0.0879(4) 0.5543(3) 0.3871(3) 0.0342(10) Uani 1 1 d . . . . .
H14 H -0.113079 0.572272 0.332765 0.041 Uiso 1 1 calc R . . . .
C15 C 0.0789(4) 0.6406(2) 0.4060(3) 0.0293(9) Uani 1 1 d . . . . .
C16 C 0.1263(4) 0.6894(3) 0.3740(3) 0.0300(9) Uani 1 1 d . . . . .
C17 C 0.0775(4) 0.7976(3) 0.2644(3) 0.0327(10) Uani 1 1 d . . . . .
H17A H 0.052585 0.773433 0.210423 0.039 Uiso 1 1 calc R . . . .
H17B H 0.004387 0.805457 0.288569 0.039 Uiso 1 1 calc R . . . .
C18 C 0.1415(4) 0.8677(3) 0.2558(2) 0.0282(9) Uani 1 1 d . . . . .
C19 C 0.1100(4) 0.9206(3) 0.1958(3) 0.0351(10) Uani 1 1 d . . . . .
H19 H 0.043518 0.912713 0.151155 0.042 Uiso 1 1 calc R . . . .
C20 C 0.1752(5) 0.9845(3) 0.2010(3) 0.0381(11) Uani 1 1 d . . . . .
H20 H 0.151867 1.020881 0.160457 0.046 Uiso 1 1 calc R . . . .
C21 C 0.2753(5) 0.9962(3) 0.2654(3) 0.0382(11) Uani 1 1 d . . . . .
H21 H 0.320959 1.039765 0.268236 0.046 Uiso 1 1 calc R . . . .
C22 C 0.3068(4) 0.9425(3) 0.3255(3) 0.0301(9) Uani 1 1 d . . . . .
H22 H 0.373908 0.950149 0.369775 0.036 Uiso 1 1 calc R . . . .
C23 C 0.2408(4) 0.8780(2) 0.3212(3) 0.0264(9) Uani 1 1 d . . . . .
C24 C 0.2598(4) 0.8149(2) 0.3796(2) 0.0234(8) Uani 1 1 d . . . . .
H24A H 0.228568 0.825618 0.430061 0.028 Uiso 1 1 calc R . . . .
H24B H 0.347339 0.801796 0.394919 0.028 Uiso 1 1 calc R . . . .
C25 C 0.2448(4) 0.7001(3) 0.1929(3) 0.0329(10) Uani 1 1 d . . . . .
H25 H 0.173228 0.722070 0.162294 0.039 Uiso 1 1 calc R . . . .
C26 C 0.3186(5) 0.6604(3) 0.1518(3) 0.0372(11) Uani 1 1 d . . . . .
H26 H 0.297555 0.654813 0.093751 0.045 Uiso 1 1 calc R . . . .
C27 C 0.4227(4) 0.6292(3) 0.1957(3) 0.0316(9) Uani 1 1 d . . . . .
H27 H 0.475460 0.602621 0.168236 0.038 Uiso 1 1 calc R . . . .
C28 C 0.4501(4) 0.6366(3) 0.2796(3) 0.0313(9) Uani 1 1 d . . . . .
H28 H 0.521115 0.614581 0.310997 0.038 Uiso 1 1 calc R . . . .
C29 C 0.3723(4) 0.6768(3) 0.3180(3) 0.0295(9) Uani 1 1 d . . . . .
H29 H 0.391095 0.682073 0.376144 0.035 Uiso 1 1 calc R . . . .
C30 C 0.4235(4) 0.5909(2) 0.6511(3) 0.0259(8) Uani 1 1 d . . . . .
C31 C 0.4944(4) 0.6244(2) 0.6187(3) 0.0252(8) Uani 1 1 d . . . . .
C32 C 0.5300(4) 0.7507(2) 0.5463(3) 0.0262(8) Uani 1 1 d . . . . .
H32A H 0.441706 0.747528 0.522084 0.031 Uiso 1 1 calc R . . . .
H32B H 0.542695 0.786663 0.591414 0.031 Uiso 1 1 calc R . . . .
C33 C 0.6037(4) 0.7696(2) 0.4817(2) 0.0250(8) Uani 1 1 d . . . . .
C34 C 0.6194(4) 0.8364(3) 0.4482(3) 0.0310(9) Uani 1 1 d . . . . .
H34 H 0.578673 0.877504 0.464249 0.037 Uiso 1 1 calc R . . . .
C35 C 0.6943(4) 0.8440(3) 0.3915(3) 0.0356(10) Uani 1 1 d . . . . .
H35 H 0.704359 0.890201 0.368801 0.043 Uiso 1 1 calc R . . . .
C36 C 0.7543(4) 0.7849(3) 0.3676(3) 0.0358(11) Uani 1 1 d . . . . .
H36 H 0.807041 0.790522 0.329595 0.043 Uiso 1 1 calc R . . . .
C37 C 0.7368(4) 0.7167(3) 0.3998(3) 0.0318(10) Uani 1 1 d . . . . .
H37 H 0.776715 0.675624 0.383068 0.038 Uiso 1 1 calc R . . . .
C38 C 0.6612(4) 0.7089(2) 0.4562(2) 0.0236(8) Uani 1 1 d . . . . .
C39 C 0.6271(4) 0.6401(2) 0.4968(3) 0.0260(8) Uani 1 1 d . . . . .
H39A H 0.697876 0.607165 0.511621 0.031 Uiso 1 1 calc R . . . .
H39B H 0.559206 0.614242 0.460858 0.031 Uiso 1 1 calc R . . . .
C40 C 0.8154(4) 0.6579(2) 0.6494(3) 0.0278(9) Uani 1 1 d . . . . .
H40 H 0.827780 0.634037 0.601088 0.033 Uiso 1 1 calc R . . . .
C41 C 0.9124(4) 0.6651(3) 0.7155(3) 0.0374(11) Uani 1 1 d . . . . .
H41 H 0.990010 0.645312 0.712842 0.045 Uiso 1 1 calc R . . . .
C42 C 0.8954(5) 0.7012(3) 0.7852(3) 0.0383(11) Uani 1 1 d . . . . .
H42 H 0.961163 0.707116 0.830709 0.046 Uiso 1 1 calc R . . . .
C43 C 0.7809(4) 0.7286(3) 0.7875(3) 0.0343(10) Uani 1 1 d . . . . .
H43 H 0.766967 0.753841 0.834617 0.041 Uiso 1 1 calc R . . . .
C44 C 0.6880(4) 0.7187(2) 0.7210(2) 0.0254(8) Uani 1 1 d . . . . .
H44 H 0.609131 0.736903 0.723107 0.030 Uiso 1 1 calc R . . . .
C45 C 0.1483(4) 0.4116(3) 0.0738(3) 0.0299(9) Uani 1 1 d . . . . .
C46 C 0.2016(4) 0.4397(2) 0.1549(2) 0.0239(8) Uani 1 1 d . . . . .
C47 C 0.3148(4) 0.4182(2) 0.1992(2) 0.0233(8) Uani 1 1 d . . . . .
H47 H 0.361843 0.385116 0.174621 0.028 Uiso 1 1 calc R . . . .
C48 C 0.3620(4) 0.4434(2) 0.2784(3) 0.0218(8) Uani 1 1 d . . . . .
C49 C 0.4801(4) 0.4226(2) 0.3252(3) 0.0237(8) Uani 1 1 d . . . . .
C50 C 0.5168(4) 0.4465(2) 0.4051(3) 0.0276(9) Uani 1 1 d . . . . .
H50 H 0.594643 0.432527 0.435436 0.033 Uiso 1 1 calc R . . . .
C51 C 0.4416(4) 0.4911(3) 0.4426(3) 0.0327(10) Uani 1 1 d . . . . .
H51 H 0.467267 0.504897 0.498553 0.039 Uiso 1 1 calc R . . . .
C52 C 0.3324(4) 0.5145(3) 0.3991(3) 0.0310(9) Uani 1 1 d . . . . .
H52 H 0.284086 0.546313 0.424359 0.037 Uiso 1 1 calc R . . . .
C53 C 0.2889(4) 0.4920(2) 0.3161(3) 0.0241(8) Uani 1 1 d . . . . .
C54 C 0.1772(4) 0.5155(2) 0.2712(3) 0.0269(9) Uani 1 1 d . . . . .
H54 H 0.130741 0.549160 0.295502 0.032 Uiso 1 1 calc R . . . .
C55 C 0.1315(4) 0.4911(2) 0.1917(3) 0.0255(8) Uani 1 1 d . . . . .
C56 C 0.0164(4) 0.5153(3) 0.1458(3) 0.0312(9) Uani 1 1 d . . . . .
H56 H -0.028783 0.550203 0.169352 0.037 Uiso 1 1 calc R . . . .
C57 C -0.0292(5) 0.4897(3) 0.0699(3) 0.0358(10) Uani 1 1 d . . . . .
H57 H -0.105041 0.507380 0.040059 0.043 Uiso 1 1 calc R . . . .
C58 C 0.0358(5) 0.4364(3) 0.0346(3) 0.0380(11) Uani 1 1 d . . . . .
H58 H 0.000432 0.417258 -0.017889 0.046 Uiso 1 1 calc R . . . .
C59 C 0.2113(5) 0.3573(3) 0.0370(3) 0.0337(10) Uani 1 1 d . . . . .
C60 C 0.2602(4) 0.3094(3) 0.0056(3) 0.0339(10) Uani 1 1 d . . . . .
C61A C 0.2396(8) 0.1859(5) -0.0907(5) 0.0342(19) Uani 0.816(11) 1 d . . P A 1
H61A H 0.164200 0.176088 -0.069657 0.041 Uiso 0.816(11) 1 calc R . P A 1
H61B H 0.216810 0.202192 -0.148552 0.041 Uiso 0.816(11) 1 calc R . P A 1
C61B C 0.222(4) 0.208(3) -0.106(3) 0.0342(19) Uani 0.184(11) 1 d . . P A 2
H61C H 0.141507 0.203891 -0.090807 0.041 Uiso 0.184(11) 1 calc R . P A 2
H61D H 0.214463 0.232721 -0.159853 0.041 Uiso 0.184(11) 1 calc R . P A 2
C62A C 0.3214(7) 0.1185(4) -0.0834(5) 0.0281(15) Uani 0.816(11) 1 d . . P A 1
C62B C 0.285(3) 0.139(2) -0.104(2) 0.0281(15) Uani 0.184(11) 1 d . . P A 2
C63A C 0.3125(7) 0.0581(5) -0.1350(5) 0.0419(19) Uani 0.816(11) 1 d . . P A 1
H63A H 0.248041 0.055145 -0.181771 0.050 Uiso 0.816(11) 1 calc R . P A 1
C63B C 0.263(4) 0.083(2) -0.166(2) 0.0419(19) Uani 0.184(11) 1 d . . P A 2
H63B H 0.203921 0.087479 -0.215551 0.050 Uiso 0.184(11) 1 calc R . P A 2
C64A C 0.3970(9) 0.0029(4) -0.1184(8) 0.047(3) Uani 0.816(11) 1 d . . P A 1
H64A H 0.387823 -0.038931 -0.152363 0.056 Uiso 0.816(11) 1 calc R . P A 1
C64B C 0.341(4) 0.018(2) -0.146(3) 0.047(3) Uani 0.184(11) 1 d . . P A 2
H64B H 0.324406 -0.021014 -0.183522 0.056 Uiso 0.184(11) 1 calc R . P A 2
C65A C 0.4959(10) 0.0078(4) -0.0519(5) 0.0434(19) Uani 0.816(11) 1 d . . P A 1
H65A H 0.555917 -0.029276 -0.042424 0.052 Uiso 0.816(11) 1 calc R . P A 1
C65B C 0.431(6) 0.009(2) -0.083(3) 0.0434(19) Uani 0.184(11) 1 d . . P A 2
H65B H 0.484098 -0.032253 -0.077779 0.052 Uiso 0.184(11) 1 calc R . P A 2
C66A C 0.5056(7) 0.0672(3) -0.0001(4) 0.0326(15) Uani 0.816(11) 1 d . . P A 1
H66A H 0.571718 0.070679 0.045599 0.039 Uiso 0.816(11) 1 calc R . P A 1
C66B C 0.444(3) 0.0660(17) -0.020(2) 0.0326(15) Uani 0.184(11) 1 d . . P A 2
H66B H 0.496427 0.060739 0.032041 0.039 Uiso 0.184(11) 1 calc R . P A 2
C67A C 0.4179(7) 0.1221(4) -0.0154(4) 0.0264(15) Uani 0.816(11) 1 d . . P A 1
C67B C 0.379(4) 0.125(2) -0.040(2) 0.0264(15) Uani 0.184(11) 1 d . . P A 2
C68A C 0.4117(12) 0.1944(6) 0.0301(8) 0.0297(19) Uani 0.816(11) 1 d . . P A 1
H68A H 0.494207 0.215684 0.046638 0.036 Uiso 0.816(11) 1 calc R . P A 1
H68B H 0.377148 0.186846 0.079999 0.036 Uiso 0.816(11) 1 calc R . P A 1
C68B C 0.398(7) 0.181(3) 0.036(4) 0.0297(19) Uani 0.184(11) 1 d . . P A 2
H68C H 0.484215 0.191412 0.059946 0.036 Uiso 0.184(11) 1 calc R . P A 2
H68D H 0.351968 0.167560 0.079470 0.036 Uiso 0.184(11) 1 calc R . P A 2
C69 C 0.4183(4) 0.2792(3) -0.1648(2) 0.0298(9) Uani 1 1 d . . . . .
H69 H 0.359621 0.248010 -0.196444 0.036 Uiso 1 1 calc R . . . .
C70 C 0.5007(4) 0.3150(3) -0.2030(3) 0.0331(10) Uani 1 1 d . . . . .
H70 H 0.497749 0.308565 -0.260174 0.040 Uiso 1 1 calc R . . . .
C71 C 0.5856(5) 0.3592(3) -0.1583(3) 0.0344(10) Uani 1 1 d . . . . .
H71 H 0.643663 0.382921 -0.183882 0.041 Uiso 1 1 calc R . . . .
C72 C 0.5876(5) 0.3699(3) -0.0748(3) 0.0376(11) Uani 1 1 d . . . . .
H72 H 0.645454 0.401287 -0.042630 0.045 Uiso 1 1 calc R . . . .
C73 C 0.5019(5) 0.3329(3) -0.0406(3) 0.0338(10) Uani 1 1 d . . . . .
H73 H 0.501669 0.339905 0.016053 0.041 Uiso 1 1 calc R . . . .
C74 C 0.5609(4) 0.3778(2) 0.2896(3) 0.0260(8) Uani 1 1 d . . . . .
C75 C 0.6359(4) 0.3427(2) 0.2629(3) 0.0265(8) Uani 1 1 d . . . . .
C76 C 0.7148(4) 0.2141(3) 0.2092(3) 0.0301(9) Uani 1 1 d . . . . .
H76A H 0.747832 0.185085 0.258767 0.036 Uiso 1 1 calc R . . . .
H76B H 0.626654 0.203538 0.191316 0.036 Uiso 1 1 calc R . . . .
C77 C 0.7832(4) 0.1990(3) 0.1412(3) 0.0293(9) Uani 1 1 d . . . . .
C78 C 0.8209(5) 0.1318(3) 0.1173(3) 0.0380(11) Uani 1 1 d . . . . .
H78 H 0.801332 0.088838 0.143267 0.046 Uiso 1 1 calc R . . . .
C79 C 0.8873(5) 0.1285(3) 0.0550(3) 0.0384(11) Uani 1 1 d . . . . .
H79 H 0.913837 0.083001 0.038457 0.046 Uiso 1 1 calc R . . . .
C80 C 0.9150(4) 0.1909(3) 0.0168(3) 0.0402(12) Uani 1 1 d . . . . .
H80 H 0.960919 0.188074 -0.025505 0.048 Uiso 1 1 calc R . . . .
C81 C 0.8762(4) 0.2580(3) 0.0397(3) 0.0362(11) Uani 1 1 d . . . . .
H81 H 0.894363 0.300750 0.012655 0.043 Uiso 1 1 calc R . . . .
C82 C 0.8106(4) 0.2620(3) 0.1026(3) 0.0292(9) Uani 1 1 d . . . . .
C83 C 0.7618(4) 0.3286(3) 0.1386(3) 0.0283(9) Uani 1 1 d . . . . .
H83A H 0.684968 0.345500 0.103080 0.034 Uiso 1 1 calc R . . . .
H83B H 0.822283 0.368359 0.145567 0.034 Uiso 1 1 calc R . . . .
C84 C 0.9639(4) 0.3435(2) 0.2904(3) 0.0291(9) Uani 1 1 d . . . . .
H84 H 0.965078 0.365650 0.238863 0.035 Uiso 1 1 calc R . . . .
C85 C 1.0656(4) 0.3485(3) 0.3510(3) 0.0361(10) Uani 1 1 d . . . . .
H85 H 1.136763 0.372320 0.341308 0.043 Uiso 1 1 calc R . . . .
C86 C 1.0633(5) 0.3186(3) 0.4261(3) 0.0384(11) Uani 1 1 d . . . . .
H86 H 1.132361 0.322577 0.469739 0.046 Uiso 1 1 calc R . . . .
C87 C 0.9589(4) 0.2824(3) 0.4383(3) 0.0348(10) Uani 1 1 d . . . . .
H87 H 0.955904 0.260722 0.489765 0.042 Uiso 1 1 calc R . . . .
C88 C 0.8601(4) 0.2789(3) 0.3736(3) 0.0290(9) Uani 1 1 d . . . . .
H88 H 0.788418 0.254462 0.381441 0.035 Uiso 1 1 calc R . . . .
B1 B 0.1804(4) 0.7502(3) 0.3260(3) 0.0263(9) Uani 1 1 d . . . . .
B2 B 0.5852(4) 0.6723(3) 0.5785(3) 0.0219(9) Uani 1 1 d . . . . .
B3 B 0.3249(5) 0.2464(3) -0.0337(3) 0.0324(11) Uani 1 1 d . . . . .
B4 B 0.7379(4) 0.3007(3) 0.2273(3) 0.0255(9) 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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0140
1 0 0 0.0140
-1 5 -5 0.0617
-1 5 5 0.0685
1 -5 3 0.0623
1 -4 -5 0.0705
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
C25 N1 B1 122.9(4) . . ?
C29 N1 C25 118.7(4) . . ?
C29 N1 B1 118.2(3) . . ?
C40 N2 C44 119.0(4) . . ?
C40 N2 B2 123.1(3) . . ?
C44 N2 B2 117.8(3) . . ?
C69 N3 C73 117.8(4) . . ?
C69 N3 B3 125.1(4) . . ?
C73 N3 B3 117.1(3) . . ?
C84 N4 B4 124.2(3) . . ?
C88 N4 C84 117.8(4) . . ?
C88 N4 B4 118.0(4) . . ?
C14 C1 C2 119.8(4) . . ?
C14 C1 C15 118.2(4) . . ?
C15 C1 C2 122.0(4) . . ?
C3 C2 C1 122.3(4) . . ?
C3 C2 C11 119.5(4) . . ?
C11 C2 C1 118.1(4) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 C2 121.3(4) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 122.1(4) . . ?
C3 C4 C9 119.3(4) . . ?
C9 C4 C5 118.4(4) . . ?
C6 C5 C4 119.8(4) . . ?
C6 C5 C30 121.1(4) . . ?
C30 C5 C4 119.1(4) . . ?
C5 C6 H6 119.3 . . ?
C5 C6 C7 121.4(4) . . ?
C7 C6 H6 119.3 . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.4(5) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.7(4) . . ?
C9 C8 H8 119.6 . . ?
C8 C9 C4 119.0(4) . . ?
C10 C9 C4 118.7(4) . . ?
C10 C9 C8 122.2(4) . . ?
C9 C10 H10 118.9 . . ?
C11 C10 C9 122.2(4) . . ?
C11 C10 H10 118.9 . . ?
C10 C11 C2 118.5(4) . . ?
C10 C11 C12 121.8(4) . . ?
C12 C11 C2 119.6(4) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 C11 120.7(4) . . ?
C13 C12 H12 119.7 . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C14 120.4(4) . . ?
C14 C13 H13 119.8 . . ?
C1 C14 C13 121.1(5) . . ?
C1 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C16 C15 C1 175.3(5) . . ?
C15 C16 B1 175.3(5) . . ?
H17A C17 H17B 109.0 . . ?
C18 C17 H17A 111.1 . . ?
C18 C17 H17B 111.1 . . ?
C18 C17 B1 103.5(4) . . ?
B1 C17 H17A 111.1 . . ?
B1 C17 H17B 111.1 . . ?
C19 C18 C17 128.1(4) . . ?
C19 C18 C23 120.6(5) . . ?
C23 C18 C17 111.3(4) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 120.1(5) . . ?
C20 C19 H19 120.0 . . ?
C19 C20 H20 119.7 . . ?
C19 C20 C21 120.6(4) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 120.6 . . ?
C20 C21 C22 118.9(5) . . ?
C22 C21 H21 120.6 . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.8(4) . . ?
C23 C22 H22 119.6 . . ?
C18 C23 C24 112.4(4) . . ?
C22 C23 C18 118.9(4) . . ?
C22 C23 C24 128.6(4) . . ?
C23 C24 H24A 111.2 . . ?
C23 C24 H24B 111.2 . . ?
C23 C24 B1 103.0(3) . . ?
H24A C24 H24B 109.1 . . ?
B1 C24 H24A 111.2 . . ?
B1 C24 H24B 111.2 . . ?
N1 C25 H25 119.0 . . ?
N1 C25 C26 122.0(4) . . ?
C26 C25 H25 119.0 . . ?
C25 C26 H26 120.4 . . ?
C27 C26 C25 119.2(4) . . ?
C27 C26 H26 120.4 . . ?
C26 C27 H27 120.3 . . ?
C26 C27 C28 119.5(4) . . ?
C28 C27 H27 120.3 . . ?
C27 C28 H28 120.5 . . ?
C27 C28 C29 119.0(4) . . ?
C29 C28 H28 120.5 . . ?
N1 C29 C28 121.6(4) . . ?
N1 C29 H29 119.2 . . ?
C28 C29 H29 119.2 . . ?
C31 C30 C5 176.5(5) . . ?
C30 C31 B2 176.9(5) . . ?
H32A C32 H32B 109.2 . . ?
C33 C32 H32A 111.3 . . ?
C33 C32 H32B 111.3 . . ?
C33 C32 B2 102.4(3) . . ?
B2 C32 H32A 111.3 . . ?
B2 C32 H32B 111.3 . . ?
C34 C33 C32 128.4(4) . . ?
C34 C33 C38 119.5(4) . . ?
C38 C33 C32 112.1(4) . . ?
C33 C34 H34 119.8 . . ?
C33 C34 C35 120.4(5) . . ?
C35 C34 H34 119.8 . . ?
C34 C35 H35 119.7 . . ?
C36 C35 C34 120.6(5) . . ?
C36 C35 H35 119.7 . . ?
C35 C36 H36 120.3 . . ?
C35 C36 C37 119.4(4) . . ?
C37 C36 H36 120.3 . . ?
C36 C37 H37 120.0 . . ?
C38 C37 C36 120.1(5) . . ?
C38 C37 H37 120.0 . . ?
C33 C38 C39 111.4(3) . . ?
C37 C38 C33 120.0(4) . . ?
C37 C38 C39 128.6(4) . . ?
C38 C39 H39A 111.5 . . ?
C38 C39 H39B 111.5 . . ?
C38 C39 B2 101.6(3) . . ?
H39A C39 H39B 109.3 . . ?
B2 C39 H39A 111.5 . . ?
B2 C39 H39B 111.5 . . ?
N2 C40 H40 119.3 . . ?
N2 C40 C41 121.3(4) . . ?
C41 C40 H40 119.3 . . ?
C40 C41 H41 120.3 . . ?
C42 C41 C40 119.5(5) . . ?
C42 C41 H41 120.3 . . ?
C41 C42 H42 120.6 . . ?
C41 C42 C43 118.8(4) . . ?
C43 C42 H42 120.6 . . ?
C42 C43 H43 120.5 . . ?
C44 C43 C42 119.1(5) . . ?
C44 C43 H43 120.5 . . ?
N2 C44 C43 122.2(4) . . ?
N2 C44 H44 118.9 . . ?
C43 C44 H44 118.9 . . ?
C58 C45 C46 119.1(4) . . ?
C58 C45 C59 120.9(4) . . ?
C59 C45 C46 120.0(4) . . ?
C47 C46 C45 123.4(4) . . ?
C47 C46 C55 118.6(4) . . ?
C55 C46 C45 118.0(4) . . ?
C46 C47 H47 118.8 . . ?
C46 C47 C48 122.5(4) . . ?
C48 C47 H47 118.8 . . ?
C47 C48 C49 123.5(4) . . ?
C47 C48 C53 118.5(4) . . ?
C53 C48 C49 118.0(4) . . ?
C50 C49 C48 119.8(4) . . ?
C50 C49 C74 119.3(4) . . ?
C74 C49 C48 121.0(4) . . ?
C49 C50 H50 119.2 . . ?
C49 C50 C51 121.5(4) . . ?
C51 C50 H50 119.2 . . ?
C50 C51 H51 119.9 . . ?
C52 C51 C50 120.2(4) . . ?
C52 C51 H51 119.9 . . ?
C51 C52 H52 119.4 . . ?
C51 C52 C53 121.2(4) . . ?
C53 C52 H52 119.4 . . ?
C52 C53 C48 119.2(4) . . ?
C54 C53 C48 119.2(4) . . ?
C54 C53 C52 121.6(4) . . ?
C53 C54 H54 119.1 . . ?
C53 C54 C55 121.9(4) . . ?
C55 C54 H54 119.1 . . ?
C54 C55 C46 119.1(4) . . ?
C54 C55 C56 121.6(4) . . ?
C56 C55 C46 119.2(4) . . ?
C55 C56 H56 119.3 . . ?
C57 C56 C55 121.4(4) . . ?
C57 C56 H56 119.3 . . ?
C56 C57 H57 120.0 . . ?
C56 C57 C58 120.0(4) . . ?
C58 C57 H57 120.0 . . ?
C45 C58 C57 122.1(5) . . ?
C45 C58 H58 119.0 . . ?
C57 C58 H58 119.0 . . ?
C60 C59 C45 177.1(5) . . ?
C59 C60 B3 179.0(5) . . ?
H61A C61A H61B 109.0 . . ?
C62A C61A H61A 111.0 . . ?
C62A C61A H61B 111.0 . . ?
C62A C61A B3 103.9(5) . . ?
B3 C61A H61A 111.0 . . ?
B3 C61A H61B 111.0 . . ?
H61C C61B H61D 110.0 . . ?
C62B C61B H61C 112.5 . . ?
C62B C61B H61D 112.5 . . ?
C62B C61B B3 96(3) . . ?
B3 C61B H61C 112.5 . . ?
B3 C61B H61D 112.5 . . ?
C63A C62A C61A 129.1(7) . . ?
C63A C62A C67A 118.8(7) . . ?
C67A C62A C61A 112.1(6) . . ?
C63B C62B C61B 127(3) . . ?
C67B C62B C61B 118(3) . . ?
C67B C62B C63B 115(3) . . ?
C62A C63A H63A 119.8 . . ?
C64A C63A C62A 120.4(8) . . ?
C64A C63A H63A 119.8 . . ?
C62B C63B H63B 122.9 . . ?
C62B C63B C64B 114(3) . . ?
C64B C63B H63B 122.9 . . ?
C63A C64A H64A 119.7 . . ?
C63A C64A C65A 120.6(8) . . ?
C65A C64A H64A 119.7 . . ?
C63B C64B H64B 116.1 . . ?
C65B C64B C63B 128(4) . . ?
C65B C64B H64B 116.1 . . ?
C64A C65A H65A 120.3 . . ?
C66A C65A C64A 119.5(8) . . ?
C66A C65A H65A 120.3 . . ?
C64B C65B H65B 122.8 . . ?
C64B C65B C66B 114(4) . . ?
C66B C65B H65B 122.8 . . ?
C65A C66A H66A 120.1 . . ?
C65A C66A C67A 119.8(7) . . ?
C67A C66A H66A 120.1 . . ?
C65B C66B H66B 121.5 . . ?
C67B C66B C65B 117(4) . . ?
C67B C66B H66B 121.5 . . ?
C62A C67A C68A 109.5(8) . . ?
C66A C67A C62A 120.7(6) . . ?
C66A C67A C68A 129.6(8) . . ?
C62B C67B C68B 118(4) . . ?
C66B C67B C62B 130(4) . . ?
C66B C67B C68B 111(4) . . ?
C67A C68A H68A 110.5 . . ?
C67A C68A H68B 110.5 . . ?
C67A C68A B3 106.0(9) . . ?
H68A C68A H68B 108.7 . . ?
B3 C68A H68A 110.5 . . ?
B3 C68A H68B 110.5 . . ?
C67B C68B H68C 114.1 . . ?
C67B C68B H68D 114.1 . . ?
C67B C68B B3 87(4) . . ?
H68C C68B H68D 111.3 . . ?
B3 C68B H68C 114.1 . . ?
B3 C68B H68D 114.1 . . ?
N3 C69 H69 119.0 . . ?
N3 C69 C70 122.0(4) . . ?
C70 C69 H69 119.0 . . ?
C69 C70 H70 120.2 . . ?
C71 C70 C69 119.6(4) . . ?
C71 C70 H70 120.2 . . ?
C70 C71 H71 120.0 . . ?
C70 C71 C72 120.0(5) . . ?
C72 C71 H71 120.0 . . ?
C71 C72 H72 121.3 . . ?
C73 C72 C71 117.4(5) . . ?
C73 C72 H72 121.3 . . ?
N3 C73 C72 123.2(4) . . ?
N3 C73 H73 118.4 . . ?
C72 C73 H73 118.4 . . ?
C75 C74 C49 175.4(5) . . ?
C74 C75 B4 176.9(5) . . ?
H76A C76 H76B 109.0 . . ?
C77 C76 H76A 111.1 . . ?
C77 C76 H76B 111.1 . . ?
C77 C76 B4 103.4(4) . . ?
B4 C76 H76A 111.1 . . ?
B4 C76 H76B 111.1 . . ?
C78 C77 C76 127.2(4) . . ?
C82 C77 C76 112.3(4) . . ?
C82 C77 C78 120.5(4) . . ?
C77 C78 H78 120.4 . . ?
C79 C78 C77 119.2(5) . . ?
C79 C78 H78 120.4 . . ?
C78 C79 H79 119.8 . . ?
C80 C79 C78 120.4(5) . . ?
C80 C79 H79 119.8 . . ?
C79 C80 H80 119.7 . . ?
C79 C80 C81 120.7(4) . . ?
C81 C80 H80 119.7 . . ?
C80 C81 H81 120.3 . . ?
C82 C81 C80 119.3(5) . . ?
C82 C81 H81 120.3 . . ?
C77 C82 C83 111.6(4) . . ?
C81 C82 C77 119.9(5) . . ?
C81 C82 C83 128.4(5) . . ?
C82 C83 H83A 111.0 . . ?
C82 C83 H83B 111.0 . . ?
C82 C83 B4 103.6(4) . . ?
H83A C83 H83B 109.0 . . ?
B4 C83 H83A 111.0 . . ?
B4 C83 H83B 111.0 . . ?
N4 C84 H84 118.4 . . ?
N4 C84 C85 123.2(4) . . ?
C85 C84 H84 118.4 . . ?
C84 C85 H85 120.6 . . ?
C84 C85 C86 118.8(5) . . ?
C86 C85 H85 120.6 . . ?
C85 C86 H86 120.2 . . ?
C85 C86 C87 119.6(4) . . ?
C87 C86 H86 120.2 . . ?
C86 C87 H87 120.9 . . ?
C88 C87 C86 118.2(4) . . ?
C88 C87 H87 120.9 . . ?
N4 C88 C87 122.4(4) . . ?
N4 C88 H88 118.8 . . ?
C87 C88 H88 118.8 . . ?
N1 B1 C24 107.4(3) . . ?
C16 B1 N1 105.4(4) . . ?
C16 B1 C17 114.1(4) . . ?
C16 B1 C24 118.0(4) . . ?
C17 B1 N1 111.2(3) . . ?
C17 B1 C24 100.6(4) . . ?
C31 B2 N2 104.6(3) . . ?
C31 B2 C32 113.8(3) . . ?
C31 B2 C39 117.2(3) . . ?
C32 B2 N2 109.1(3) . . ?
C32 B2 C39 101.8(3) . . ?
C39 B2 N2 110.2(3) . . ?
N3 B3 C68B 113(2) . . ?
C60 B3 N3 105.1(4) . . ?
C60 B3 C61A 118.7(5) . . ?
C60 B3 C61B 108.2(17) . . ?
C60 B3 C68A 115.8(6) . . ?
C60 B3 C68B 115(2) . . ?
C61A B3 N3 112.1(4) . . ?
C61B B3 N3 104.4(17) . . ?
C61B B3 C68B 110(3) . . ?
C68A B3 N3 104.3(5) . . ?
C68A B3 C61A 100.1(6) . . ?
C75 B4 N4 104.1(3) . . ?
C75 B4 C76 116.5(4) . . ?
C75 B4 C83 116.1(4) . . ?
C76 B4 N4 107.4(3) . . ?
C83 B4 N4 111.7(3) . . ?
C83 B4 C76 101.1(4) . . ?
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
N1 C25 1.345(5) . ?
N1 C29 1.342(6) . ?
N1 B1 1.638(6) . ?
N2 C40 1.339(5) . ?
N2 C44 1.350(5) . ?
N2 B2 1.638(5) . ?
N3 C69 1.347(5) . ?
N3 C73 1.351(6) . ?
N3 B3 1.649(6) . ?
N4 C84 1.350(6) . ?
N4 C88 1.343(5) . ?
N4 B4 1.650(6) . ?
C1 C2 1.437(7) . ?
C1 C14 1.393(7) . ?
C1 C15 1.435(6) . ?
C2 C3 1.408(6) . ?
C2 C11 1.434(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.394(6) . ?
C4 C5 1.444(6) . ?
C4 C9 1.442(5) . ?
C5 C6 1.365(7) . ?
C5 C30 1.438(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.415(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.368(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.421(7) . ?
C9 C10 1.400(7) . ?
C10 H10 0.9500 . ?
C10 C11 1.399(7) . ?
C11 C12 1.427(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.367(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.406(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.220(7) . ?
C16 B1 1.567(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.501(7) . ?
C17 B1 1.634(7) . ?
C18 C19 1.390(7) . ?
C18 C23 1.401(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.383(8) . ?
C20 H20 0.9500 . ?
C20 C21 1.402(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.402(7) . ?
C22 H22 0.9500 . ?
C22 C23 1.397(7) . ?
C23 C24 1.505(6) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 B1 1.642(6) . ?
C25 H25 0.9500 . ?
C25 C26 1.381(7) . ?
C26 H26 0.9500 . ?
C26 C27 1.371(7) . ?
C27 H27 0.9500 . ?
C27 C28 1.372(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.391(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.212(6) . ?
C31 B2 1.589(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.516(6) . ?
C32 B2 1.624(6) . ?
C33 C34 1.382(6) . ?
C33 C38 1.399(6) . ?
C34 H34 0.9500 . ?
C34 C35 1.385(7) . ?
C35 H35 0.9500 . ?
C35 C36 1.381(8) . ?
C36 H36 0.9500 . ?
C36 C37 1.399(8) . ?
C37 H37 0.9500 . ?
C37 C38 1.387(6) . ?
C38 C39 1.524(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 B2 1.632(6) . ?
C40 H40 0.9500 . ?
C40 C41 1.386(7) . ?
C41 H41 0.9500 . ?
C41 C42 1.380(8) . ?
C42 H42 0.9500 . ?
C42 C43 1.383(8) . ?
C43 H43 0.9500 . ?
C43 C44 1.369(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.455(6) . ?
C45 C58 1.375(7) . ?
C45 C59 1.431(6) . ?
C46 C47 1.388(6) . ?
C46 C55 1.442(6) . ?
C47 H47 0.9500 . ?
C47 C48 1.396(6) . ?
C48 C49 1.444(6) . ?
C48 C53 1.439(5) . ?
C49 C50 1.380(6) . ?
C49 C74 1.435(6) . ?
C50 H50 0.9500 . ?
C50 C51 1.408(6) . ?
C51 H51 0.9500 . ?
C51 C52 1.359(7) . ?
C52 H52 0.9500 . ?
C52 C53 1.427(6) . ?
C53 C54 1.389(6) . ?
C54 H54 0.9500 . ?
C54 C55 1.393(6) . ?
C55 C56 1.430(6) . ?
C56 H56 0.9500 . ?
C56 C57 1.347(7) . ?
C57 H57 0.9500 . ?
C57 C58 1.419(7) . ?
C58 H58 0.9500 . ?
C59 C60 1.211(7) . ?
C60 B3 1.578(7) . ?
C61A H61A 0.9900 . ?
C61A H61B 0.9900 . ?
C61A C62A 1.536(10) . ?
C61A B3 1.643(10) . ?
C61B H61C 0.9900 . ?
C61B H61D 0.9900 . ?
C61B C62B 1.46(5) . ?
C61B B3 1.65(5) . ?
C62A C63A 1.398(9) . ?
C62A C67A 1.399(8) . ?
C62B C63B 1.44(5) . ?
C62B C67B 1.36(4) . ?
C63A H63A 0.9500 . ?
C63A C64A 1.381(13) . ?
C63B H63B 0.9500 . ?
C63B C64B 1.48(6) . ?
C64A H64A 0.9500 . ?
C64A C65A 1.401(13) . ?
C64B H64B 0.9500 . ?
C64B C65B 1.31(7) . ?
C65A H65A 0.9500 . ?
C65A C66A 1.386(10) . ?
C65B H65B 0.9500 . ?
C65B C66B 1.47(6) . ?
C66A H66A 0.9500 . ?
C66A C67A 1.399(9) . ?
C66B H66B 0.9500 . ?
C66B C67B 1.32(5) . ?
C67A C68A 1.543(14) . ?
C67B C68B 1.61(8) . ?
C68A H68A 0.9900 . ?
C68A H68B 0.9900 . ?
C68A B3 1.607(15) . ?
C68B H68C 0.9900 . ?
C68B H68D 0.9900 . ?
C68B B3 1.76(8) . ?
C69 H69 0.9500 . ?
C69 C70 1.386(7) . ?
C70 H70 0.9500 . ?
C70 C71 1.356(7) . ?
C71 H71 0.9500 . ?
C71 C72 1.396(7) . ?
C72 H72 0.9500 . ?
C72 C73 1.386(7) . ?
C73 H73 0.9500 . ?
C74 C75 1.211(6) . ?
C75 B4 1.587(6) . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C76 C77 1.510(6) . ?
C76 B4 1.640(7) . ?
C77 C78 1.395(7) . ?
C77 C82 1.392(7) . ?
C78 H78 0.9500 . ?
C78 C79 1.388(8) . ?
C79 H79 0.9500 . ?
C79 C80 1.382(8) . ?
C80 H80 0.9500 . ?
C80 C81 1.392(8) . ?
C81 H81 0.9500 . ?
C81 C82 1.391(6) . ?
C82 C83 1.517(6) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C83 B4 1.630(6) . ?
C84 H84 0.9500 . ?
C84 C85 1.363(7) . ?
C85 H85 0.9500 . ?
C85 C86 1.369(7) . ?
C86 H86 0.9500 . ?
C86 C87 1.393(7) . ?
C87 H87 0.9500 . ?
C87 C88 1.380(7) . ?
C88 H88 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
N1 C25 C26 C27 -0.7(8) . . . . ?
N2 C40 C41 C42 -1.4(7) . . . . ?
N3 C69 C70 C71 0.6(7) . . . . ?
N4 C84 C85 C86 -1.9(7) . . . . ?
C1 C2 C3 C4 -175.5(4) . . . . ?
C1 C2 C11 C10 -178.9(4) . . . . ?
C1 C2 C11 C12 3.0(6) . . . . ?
C2 C1 C14 C13 3.5(7) . . . . ?
C2 C3 C4 C5 171.5(4) . . . . ?
C2 C3 C4 C9 -4.9(6) . . . . ?
C2 C11 C12 C13 1.8(7) . . . . ?
C3 C2 C11 C10 5.5(6) . . . . ?
C3 C2 C11 C12 -172.5(4) . . . . ?
C3 C4 C5 C6 179.4(4) . . . . ?
C3 C4 C5 C30 -2.3(6) . . . . ?
C3 C4 C9 C8 -178.8(4) . . . . ?
C3 C4 C9 C10 4.4(6) . . . . ?
C4 C5 C6 C7 1.2(7) . . . . ?
C4 C9 C10 C11 1.1(7) . . . . ?
C5 C4 C9 C8 4.7(6) . . . . ?
C5 C4 C9 C10 -172.1(4) . . . . ?
C5 C6 C7 C8 1.5(7) . . . . ?
C6 C7 C8 C9 -0.9(7) . . . . ?
C7 C8 C9 C4 -2.2(7) . . . . ?
C7 C8 C9 C10 174.5(5) . . . . ?
C8 C9 C10 C11 -175.6(4) . . . . ?
C9 C4 C5 C6 -4.2(6) . . . . ?
C9 C4 C5 C30 174.1(4) . . . . ?
C9 C10 C11 C2 -6.0(7) . . . . ?
C9 C10 C11 C12 171.9(4) . . . . ?
C10 C11 C12 C13 -176.2(4) . . . . ?
C11 C2 C3 C4 -0.1(6) . . . . ?
C11 C12 C13 C14 -4.0(7) . . . . ?
C12 C13 C14 C1 1.4(8) . . . . ?
C14 C1 C2 C3 169.8(4) . . . . ?
C14 C1 C2 C11 -5.6(6) . . . . ?
C15 C1 C2 C3 -10.6(6) . . . . ?
C15 C1 C2 C11 174.1(4) . . . . ?
C15 C1 C14 C13 -176.2(4) . . . . ?
C17 C18 C19 C20 175.4(4) . . . . ?
C17 C18 C23 C22 -176.5(4) . . . . ?
C17 C18 C23 C24 2.7(5) . . . . ?
C18 C17 B1 N1 -84.8(4) . . . . ?
C18 C17 B1 C16 156.1(4) . . . . ?
C18 C17 B1 C24 28.7(4) . . . . ?
C18 C19 C20 C21 1.5(7) . . . . ?
C18 C23 C24 B1 16.7(4) . . . . ?
C19 C18 C23 C22 0.7(6) . . . . ?
C19 C18 C23 C24 179.8(4) . . . . ?
C19 C20 C21 C22 -1.3(7) . . . . ?
C20 C21 C22 C23 0.7(7) . . . . ?
C21 C22 C23 C18 -0.5(6) . . . . ?
C21 C22 C23 C24 -179.4(4) . . . . ?
C22 C23 C24 B1 -164.3(4) . . . . ?
C23 C18 C19 C20 -1.3(7) . . . . ?
C23 C24 B1 N1 89.3(4) . . . . ?
C23 C24 B1 C16 -151.9(4) . . . . ?
C23 C24 B1 C17 -27.1(4) . . . . ?
C25 N1 C29 C28 0.7(7) . . . . ?
C25 N1 B1 C16 108.7(5) . . . . ?
C25 N1 B1 C17 -15.6(6) . . . . ?
C25 N1 B1 C24 -124.8(4) . . . . ?
C25 C26 C27 C28 1.4(8) . . . . ?
C26 C27 C28 C29 -1.1(7) . . . . ?
C27 C28 C29 N1 0.0(7) . . . . ?
C29 N1 C25 C26 -0.4(7) . . . . ?
C29 N1 B1 C16 -66.4(5) . . . . ?
C29 N1 B1 C17 169.4(4) . . . . ?
C29 N1 B1 C24 60.2(5) . . . . ?
C30 C5 C6 C7 -177.1(4) . . . . ?
C32 C33 C34 C35 177.6(4) . . . . ?
C32 C33 C38 C37 -177.3(4) . . . . ?
C32 C33 C38 C39 3.5(5) . . . . ?
C33 C32 B2 N2 87.1(4) . . . . ?
C33 C32 B2 C31 -156.5(3) . . . . ?
C33 C32 B2 C39 -29.4(4) . . . . ?
C33 C34 C35 C36 -0.1(7) . . . . ?
C33 C38 C39 B2 -22.6(4) . . . . ?
C34 C33 C38 C37 2.2(6) . . . . ?
C34 C33 C38 C39 -177.0(4) . . . . ?
C34 C35 C36 C37 1.5(7) . . . . ?
C35 C36 C37 C38 -1.0(7) . . . . ?
C36 C37 C38 C33 -0.8(6) . . . . ?
C36 C37 C38 C39 178.2(4) . . . . ?
C37 C38 C39 B2 158.3(4) . . . . ?
C38 C33 C34 C35 -1.8(6) . . . . ?
C38 C39 B2 N2 -84.6(4) . . . . ?
C38 C39 B2 C31 156.0(4) . . . . ?
C38 C39 B2 C32 31.1(4) . . . . ?
C40 N2 C44 C43 0.4(6) . . . . ?
C40 N2 B2 C31 115.5(4) . . . . ?
C40 N2 B2 C32 -122.4(4) . . . . ?
C40 N2 B2 C39 -11.4(5) . . . . ?
C40 C41 C42 C43 0.8(7) . . . . ?
C41 C42 C43 C44 0.3(7) . . . . ?
C42 C43 C44 N2 -1.0(7) . . . . ?
C44 N2 C40 C41 0.8(6) . . . . ?
C44 N2 B2 C31 -61.2(4) . . . . ?
C44 N2 B2 C32 60.9(4) . . . . ?
C44 N2 B2 C39 172.0(4) . . . . ?
C45 C46 C47 C48 -177.1(4) . . . . ?
C45 C46 C55 C54 176.2(4) . . . . ?
C45 C46 C55 C56 -3.5(6) . . . . ?
C46 C45 C58 C57 1.3(8) . . . . ?
C46 C47 C48 C49 -179.1(4) . . . . ?
C46 C47 C48 C53 1.7(6) . . . . ?
C46 C55 C56 C57 1.8(7) . . . . ?
C47 C46 C55 C54 -2.2(6) . . . . ?
C47 C46 C55 C56 178.2(4) . . . . ?
C47 C48 C49 C50 -176.0(4) . . . . ?
C47 C48 C49 C74 4.6(6) . . . . ?
C47 C48 C53 C52 175.9(4) . . . . ?
C47 C48 C53 C54 -3.6(6) . . . . ?
C48 C49 C50 C51 0.0(6) . . . . ?
C48 C53 C54 C55 2.6(6) . . . . ?
C49 C48 C53 C52 -3.4(6) . . . . ?
C49 C48 C53 C54 177.2(4) . . . . ?
C49 C50 C51 C52 -3.1(7) . . . . ?
C50 C51 C52 C53 2.8(7) . . . . ?
C51 C52 C53 C48 0.4(7) . . . . ?
C51 C52 C53 C54 179.8(4) . . . . ?
C52 C53 C54 C55 -176.8(4) . . . . ?
C53 C48 C49 C50 3.2(6) . . . . ?
C53 C48 C49 C74 -176.2(4) . . . . ?
C53 C54 C55 C46 0.3(6) . . . . ?
C53 C54 C55 C56 179.9(4) . . . . ?
C54 C55 C56 C57 -177.8(5) . . . . ?
C55 C46 C47 C48 1.2(6) . . . . ?
C55 C56 C57 C58 1.4(8) . . . . ?
C56 C57 C58 C45 -3.0(8) . . . . ?
C58 C45 C46 C47 -179.8(4) . . . . ?
C58 C45 C46 C55 1.9(7) . . . . ?
C59 C45 C46 C47 2.1(7) . . . . ?
C59 C45 C46 C55 -176.2(4) . . . . ?
C59 C45 C58 C57 179.4(5) . . . . ?
C61A C62A C63A C64A 179.1(7) . . . . ?
C61A C62A C67A C66A -177.3(6) . . . . ?
C61A C62A C67A C68A -0.8(8) . . . . ?
C61B C62B C63B C64B -180(4) . . . . ?
C61B C62B C67B C66B 175(4) . . . . ?
C61B C62B C67B C68B 11(5) . . . . ?
C62A C61A B3 N3 83.2(6) . . . . ?
C62A C61A B3 C60 -153.9(5) . . . . ?
C62A C61A B3 C68A -26.9(7) . . . . ?
C62A C63A C64A C65A -3.0(11) . . . . ?
C62A C67A C68A B3 -17.8(7) . . . . ?
C62B C61B B3 N3 92(2) . . . . ?
C62B C61B B3 C60 -156(2) . . . . ?
C62B C61B B3 C68B -29(4) . . . . ?
C62B C63B C64B C65B -5(6) . . . . ?
C62B C67B C68B B3 -26(4) . . . . ?
C63A C62A C67A C66A 1.4(9) . . . . ?
C63A C62A C67A C68A 177.8(6) . . . . ?
C63A C64A C65A C66A 3.1(11) . . . . ?
C63B C62B C67B C66B -9(5) . . . . ?
C63B C62B C67B C68B -173(3) . . . . ?
C63B C64B C65B C66B 8(6) . . . . ?
C64A C65A C66A C67A -1.0(9) . . . . ?
C64B C65B C66B C67B -11(5) . . . . ?
C65A C66A C67A C62A -1.2(9) . . . . ?
C65A C66A C67A C68A -176.9(7) . . . . ?
C65B C66B C67B C62B 12(6) . . . . ?
C65B C66B C67B C68B 177(4) . . . . ?
C66A C67A C68A B3 158.3(6) . . . . ?
C66B C67B C68B B3 167(3) . . . . ?
C67A C62A C63A C64A 0.7(9) . . . . ?
C67A C68A B3 N3 -89.2(6) . . . . ?
C67A C68A B3 C60 155.9(5) . . . . ?
C67A C68A B3 C61A 26.9(7) . . . . ?
C67B C62B C63B C64B 4(4) . . . . ?
C67B C68B B3 N3 -84(3) . . . . ?
C67B C68B B3 C60 155(2) . . . . ?
C67B C68B B3 C61B 32(4) . . . . ?
C69 N3 C73 C72 -1.5(7) . . . . ?
C69 N3 B3 C60 -123.2(4) . . . . ?
C69 N3 B3 C61A 7.1(7) . . . . ?
C69 N3 B3 C61B -9.5(18) . . . . ?
C69 N3 B3 C68A 114.5(6) . . . . ?
C69 N3 B3 C68B 110(2) . . . . ?
C69 C70 C71 C72 -1.6(7) . . . . ?
C70 C71 C72 C73 1.1(8) . . . . ?
C71 C72 C73 N3 0.5(8) . . . . ?
C73 N3 C69 C70 0.9(7) . . . . ?
C73 N3 B3 C60 56.4(5) . . . . ?
C73 N3 B3 C61A -173.4(5) . . . . ?
C73 N3 B3 C61B 170.1(18) . . . . ?
C73 N3 B3 C68A -65.9(7) . . . . ?
C73 N3 B3 C68B -70(3) . . . . ?
C74 C49 C50 C51 179.4(4) . . . . ?
C76 C77 C78 C79 -177.6(4) . . . . ?
C76 C77 C82 C81 178.4(4) . . . . ?
C76 C77 C82 C83 -1.1(5) . . . . ?
C77 C76 B4 N4 -91.2(4) . . . . ?
C77 C76 B4 C75 152.6(4) . . . . ?
C77 C76 B4 C83 25.9(4) . . . . ?
C77 C78 C79 C80 -0.4(7) . . . . ?
C77 C82 C83 B4 18.5(5) . . . . ?
C78 C77 C82 C81 -0.1(6) . . . . ?
C78 C77 C82 C83 -179.6(4) . . . . ?
C78 C79 C80 C81 -0.4(7) . . . . ?
C79 C80 C81 C82 1.0(7) . . . . ?
C80 C81 C82 C77 -0.7(6) . . . . ?
C80 C81 C82 C83 178.7(4) . . . . ?
C81 C82 C83 B4 -160.9(4) . . . . ?
C82 C77 C78 C79 0.7(7) . . . . ?
C82 C83 B4 N4 87.4(4) . . . . ?
C82 C83 B4 C75 -153.5(4) . . . . ?
C82 C83 B4 C76 -26.5(4) . . . . ?
C84 N4 C88 C87 -0.5(7) . . . . ?
C84 N4 B4 C75 -116.8(4) . . . . ?
C84 N4 B4 C76 119.1(4) . . . . ?
C84 N4 B4 C83 9.2(6) . . . . ?
C84 C85 C86 C87 1.6(8) . . . . ?
C85 C86 C87 C88 -0.9(8) . . . . ?
C86 C87 C88 N4 0.3(7) . . . . ?
C88 N4 C84 C85 1.3(7) . . . . ?
C88 N4 B4 C75 62.8(5) . . . . ?
C88 N4 B4 C76 -61.3(5) . . . . ?
C88 N4 B4 C83 -171.2(4) . . . . ?
B1 N1 C25 C26 -175.4(5) . . . . ?
B1 N1 C29 C28 176.0(4) . . . . ?
B1 C17 C18 C19 162.2(4) . . . . ?
B1 C17 C18 C23 -20.9(4) . . . . ?
B2 N2 C40 C41 -175.8(4) . . . . ?
B2 N2 C44 C43 177.2(4) . . . . ?
B2 C32 C33 C34 -162.0(4) . . . . ?
B2 C32 C33 C38 17.4(4) . . . . ?
B3 N3 C69 C70 -179.5(4) . . . . ?
B3 N3 C73 C72 178.9(5) . . . . ?
B3 C61A C62A C63A -160.0(6) . . . . ?
B3 C61A C62A C67A 18.5(7) . . . . ?
B3 C61B C62B C63B -163(3) . . . . ?
B3 C61B C62B C67B 13(4) . . . . ?
B4 N4 C84 C85 -179.1(4) . . . . ?
B4 N4 C88 C87 179.9(4) . . . . ?
B4 C76 C77 C78 161.7(4) . . . . ?
B4 C76 C77 C82 -16.7(5) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6(7)
2 0.4(7)
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
-1.0042 0.0091 0.0106 0.1302 -0.0069 0.0542
1.0042 -0.0091 -0.0106 -0.1302 0.0069 -0.0542
-1.0109 5.0383 -5.0014 -0.0226 -0.1688 0.6472
-0.9754 5.0208 5.0264 0.0370 0.6163 0.1138
1.0038 -5.0348 2.9959 0.0107 0.0118 -0.5405
0.9776 -4.0167 -5.0260 -0.0616 -0.5702 -0.0485
