#------------------------------------------------------------------------------
#$Date: 2024-08-05 22:43:21 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293884 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/32/7063299.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_7063299
loop_
_publ_author_name
'Guseinov, Firudin I.'
'Ovsyannikov, Viacheslav O.'
'Shuvalova, Elena V.'
'Kustov, Leonid M.'
'Kobrakov, Konstantin I.'
'Samigullina, Aida I.'
'Mahmudov, Kamran T.'
_publ_section_title
;
 Unexpected 20-membered macrocycles obtained by the condensation of
 α,α-dihalo-β-oxoaldehydes with diaminofurazan
;
_journal_issue                   29
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12869
_journal_page_last               12872
_journal_paper_doi               10.1039/D4NJ01789G
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety
'C48 H40 Br8 N16 O12, 3.117(C3 H7 N O), 0.883(C2 H6 O S) '
_chemical_formula_sum            'C59.12 H67.12 Br8 N19.12 O16 S0.88'
_chemical_formula_weight         1969.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-02-07
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2024-03-06 deposited with the CCDC.	2024-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.326(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8694(4)
_cell_length_b                   29.3492(6)
_cell_length_c                   19.4086(5)
_cell_measurement_reflns_used    27196
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.1900
_cell_measurement_theta_min      2.7800
_cell_volume                     7455.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.104a 64-bit (release 22-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -75.00  24.00   0.50    3.00    --  -42.41  86.00  -0.00  198
  2  ω    -75.00  24.00   0.50    3.00    --  -42.41  86.00  -0.00  198
  3  ω      4.00  64.00   0.50    3.00    --   42.41 -86.00-118.00  120
  4  ω   -100.00 -74.00   0.50   22.00    --  -96.00  86.00  -0.00   52
  5  ω     57.00 122.00   0.50   22.00    --  117.50 -86.00-118.00  130
  6  ω    101.00 178.00   0.50   22.00    --  117.50  86.00  -0.00  154
  7  ω    -16.00  38.00   0.50    3.00    --  -42.41  19.00  90.00  108
  8  ω    -27.00  34.00   0.50    3.00    --  -42.41  38.00 120.00  122
  9  ω     35.00  94.00   0.50    3.00    --   42.41-125.00  90.00  118
 10  ω     49.00  75.00   0.50    3.00    --   42.41-125.00 120.00   52
 11  ω   -104.00 -67.00   0.50   22.00    --  -96.00 -77.00 -60.00   74
 12  ω   -149.00-123.00   0.50   22.00    --  -96.00 -77.00 -60.00   52
 13  ω    -50.00 -21.00   0.50   22.00    --  -96.00  45.00-150.00   58
 14  ω   -155.00-110.00   0.50   22.00    --  -96.00 -86.00-118.00   90
 15  ω     54.00 104.00   0.50   22.00    --  117.50 -77.00 120.00  100
 16  ω     48.00  77.00   0.50   22.00    --  117.50-125.00 120.00   58
 17  ω     46.00 104.00   0.50   22.00    --  117.50-125.00  90.00  116
 18  ω     81.00 111.00   0.50   22.00    --  117.50-125.00 120.00   60
 19  ω     65.00 103.00   0.50   22.00    --  117.50 -95.00  90.00   76
 20  ω     92.00 178.00   0.50   22.00    --  117.50  77.00 -90.00  172
 21  ω     44.00  97.00   0.50   22.00    --  117.50 -77.00  60.00  106
 22  ω     44.00  69.00   0.50   22.00    --  117.50 -61.00  90.00   50
 23  ω     46.00  93.00   0.50   22.00    --  117.50 -77.00 -90.00   94
 24  ω     44.00  69.00   0.50   22.00    --  117.50 -61.00 150.00   50
 25  ω     44.00  88.00   0.50   22.00    --  117.50 -77.00 150.00   88
 26  ω     94.00 128.00   0.50   22.00    --  117.50  77.00  30.00   68
 27  ω    140.00 175.00   0.50   22.00    --  117.50  77.00  30.00   70
 28  ω     45.00 103.00   0.50   22.00    --  117.50 -77.00 -60.00  116
 29  ω     50.00  84.00   0.50   22.00    --  117.50 -77.00   0.00   68
 30  ω    103.00 129.00   0.50   22.00    --  117.50  45.00 -90.00   52
 31  ω    135.00 161.00   0.50   22.00    --  117.50  45.00 -90.00   52
 32  ω     55.00 108.00   0.50   22.00    --  117.50-125.00-120.00  106
 33  ω     98.00 160.00   0.50   22.00    --  117.50  61.00 -30.00  124
 34  ω     95.00 121.00   0.50   22.00    --  117.50 125.00   0.00   52
 35  ω     45.00  70.00   0.50   22.00    --  117.50 -61.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0513918000
_diffrn_orient_matrix_UB_12      0.0239404000
_diffrn_orient_matrix_UB_13      -0.0493663000
_diffrn_orient_matrix_UB_21      0.0744117000
_diffrn_orient_matrix_UB_22      -0.0403713000
_diffrn_orient_matrix_UB_23      0.0098667000
_diffrn_orient_matrix_UB_31      -0.0754312000
_diffrn_orient_matrix_UB_32      -0.0235162000
_diffrn_orient_matrix_UB_33      -0.0673216000
_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  0.0615
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60350
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.331
_diffrn_reflns_theta_min         2.844
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.026
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3911
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.594
_refine_diff_density_min         -1.937
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         15830
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.1193
_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)+(0.0268P)²+171.4857P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2430
_refine_ls_wR_factor_ref         0.2458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14317
_reflns_number_total             15830
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4nj01789g2.cif
_cod_data_source_block           G-29
_cod_depositor_comments
'Adding full bibliography for 7063299--7063301.cif.'
_cod_database_code               7063299
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H20N8O12Br
_chemical_oxdiff_usercomment     G-29
_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   0.840
_shelx_estimated_absorpt_t_min   0.314
_reflns_odcompleteness_completeness 98.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C46-C47 \\sim C46A-C47A
 with sigma of 0.02
 C47-C48 \\sim C47A-C48A
 with sigma of 0.02
 C48-C49 \\sim C48A-C49A
 with sigma of 0.02
 C49-C47 \\sim C47A-C49A
 with sigma of 0.04
 C45-C46 \\sim C45A-C46A
 with sigma of 0.02
 C47A-C45A \\sim C45-C47
 with sigma of 0.04
 C47-O50 \\sim C47A-O50A
 with sigma of 0.02
 O50-C50 \\sim O50A-C50A
 with sigma of 0.02
 N73-C75 \\sim N73A-C75A
 with sigma of 0.02
 O73A-N73A \\sim O73-N73
 with sigma of 0.04
 N73-C74 \\sim N73A-C74A
 with sigma of 0.02
 O73A-C73A \\sim O73-C73
 with sigma of 0.02
 C73A-C75A \\sim C73-C75
 with sigma of 0.04
 C73A-C74A \\sim C73-C74
 with sigma of 0.04
 C73A-N73A \\sim C73-N73
 with sigma of 0.02
3. Restrained planarity
 C75A, C74A, N73A, C73A, O73A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
Uanis(C73) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C80) \\sim Ueq, Uanis(C80A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C47) = Uanis(C46)
Uanis(C48) = Uanis(C48A) = Uanis(C47A) = Uanis(C47) = Uanis(C46A) = Uanis(C46)
Uanis(C50) = Uanis(C50A)
Uanis(C19) = Uanis(C20)
Uanis(C49) = Uanis(C49A) = Uanis(C45A) = Uanis(C45)
Uanis(O50) = Uanis(O50A)
Uanis(C75A) = Uanis(C75)
Uanis(O73A) = Uanis(O73)
Uanis(N73A) = Uanis(N73)
Uanis(C74A) = Uanis(C74) = Uanis(C73A) = Uanis(C73)
Uanis(O76) = Uanis(O76A)
Uanis(C77A) = Uanis(C77)
Uanis(C78) = Uanis(C78A)
Uanis(C80) = Uanis(C80A)
Uanis(C81) = Uanis(C81A)
Uanis(C79A) = Uanis(S79)
Uanis(O79) = Uanis(O79A)
5. Others
 Sof(S76A)=Sof(O76A)=Sof(C77A)=Sof(H77D)=Sof(H77E)=Sof(H77F)=Sof(C78A)=
 Sof(H78D)=Sof(H78E)=Sof(H78F)=1-FVAR(1)
 Sof(O76)=Sof(N76)=Sof(C76)=Sof(H76)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=
 Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=FVAR(1)
 Sof(O79A)=Sof(N79A)=Sof(C79A)=Sof(H79A)=Sof(C80A)=Sof(H80A)=Sof(H80B)=
 Sof(H80C)=Sof(C81A)=Sof(H81A)=Sof(H81B)=Sof(H81C)=1-FVAR(2)
 Sof(S79)=Sof(O79)=Sof(C80)=Sof(H80D)=Sof(H80E)=Sof(H80F)=Sof(C81)=Sof(H81D)=
 Sof(H81E)=Sof(H81F)=FVAR(2)
 Sof(O50A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(C48A)=
 Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(C50A)=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(3)
 Sof(O50)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(C48)=Sof(H48)=
 Sof(C49)=Sof(H49)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(3)
 Sof(O73A)=Sof(N73A)=Sof(C73A)=Sof(H73A)=Sof(C74A)=Sof(H74D)=Sof(H74E)=
 Sof(H74F)=Sof(C75A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=1-FVAR(4)
 Sof(O73)=Sof(N73)=Sof(C73)=Sof(H73)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=FVAR(4)
6.a Free rotating group:
 S76A(O76A,C77A,C78A), S79(O79,C80,C81), O76(N76,C76,C77,C78), O79A(N79A,C79A,
 C80A,C81A)
6.b Ternary CH refined with riding coordinates:
 C7(H7), C15(H15), C23(H23), C31(H31)
6.c Me refined with riding coordinates:
 C77A(H77D,H77E,H77F), C78A(H78D,H78E,H78F), C80(H80D,H80E,H80F), C81(H81D,
 H81E,H81F), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C),
 C74A(H74D,H74E,H74F), C75(H75A,H75B,H75C), C75A(H75D,H75E,H75F), C77(H77A,H77B,
 H77C), C78(H78A,H78B,H78C), C80A(H80A,H80B,H80C), C81A(H81A,H81B,H81C)
6.d Aromatic/amide H refined with riding coordinates:
 N6(H6), N8(H8), N14(H14), N16(H16), N22(H22), N24(H24), N30(H30), N32(H32),
 C36(H36), C37(H37), C39(H39), C40(H40), C45(H45), C45A(H45A), C46(H46),
 C46A(H46A), C48(H48), C48A(H48A), C49(H49), C49A(H49A), C54(H54), C55(H55),
 C57(H57), C58(H58), C63(H63), C64(H64), C66(H66), C67(H67), C70(H70), C73(H73),
  C73A(H73A), C76(H76), C79A(H79A)
6.e Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C50(H50A,H50B,H50C), C50A(H50D,H50E,H50F), C59(H59A,H59B,
 H59C), C68(H68A,H68B,H68C)
;
_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 1.493
_oxdiff_exptl_absorpt_empirical_full_min 0.637
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.79738(10) 0.59736(4) 0.11160(7) 0.0435(3) Uani 1 1 d . . . . .
Br2 Br 0.65599(10) 0.52507(4) 0.15861(7) 0.0432(3) Uani 1 1 d . . . . .
Br3 Br 0.25905(11) 0.53583(4) 0.28800(7) 0.0448(3) Uani 1 1 d . . . . .
Br4 Br 0.12231(11) 0.61488(4) 0.32219(8) 0.0490(3) Uani 1 1 d . . . . .
Br5 Br 0.12643(13) 0.86125(6) 0.27031(11) 0.0774(5) Uani 1 1 d . . . . .
Br6 Br 0.28183(14) 0.91932(4) 0.21834(7) 0.0595(4) Uani 1 1 d . . . . .
Br7 Br 0.64603(10) 0.91153(4) 0.10762(7) 0.0472(3) Uani 1 1 d . . . . .
Br8 Br 0.79709(11) 0.83902(5) 0.07493(8) 0.0532(3) Uani 1 1 d . . . . .
O1 O 0.4222(9) 0.7102(3) -0.0124(6) 0.081(4) Uani 1 1 d . . . . .
O9 O 0.3123(6) 0.5554(3) 0.0667(4) 0.0467(19) Uani 1 1 d . . . . .
O17 O 0.1401(12) 0.7135(3) 0.0637(5) 0.091(4) Uani 1 1 d . . . . .
O25 O 0.3009(7) 0.8629(3) 0.0008(4) 0.053(2) Uani 1 1 d . . . . .
O34 O 0.7339(6) 0.6338(2) 0.2703(4) 0.0422(18) Uani 1 1 d . . . . .
O41 O 1.0778(7) 0.4983(3) 0.4437(5) 0.057(2) Uani 1 1 d . . . . .
O43 O 0.3873(7) 0.6480(3) 0.3761(5) 0.052(2) Uani 1 1 d . . . . .
O50 O 0.463(2) 0.4991(9) 0.6290(13) 0.053(5) Uani 0.53(3) 1 d D . P A 1
O50A O 0.496(2) 0.5126(10) 0.6325(15) 0.053(5) Uani 0.47(3) 1 d D . P A 2
O52 O 0.3941(7) 0.8184(3) 0.3364(4) 0.047(2) Uani 1 1 d . . . . .
O59 O 0.4526(6) 0.9783(2) 0.5642(4) 0.0403(17) Uani 1 1 d . . . . .
O61 O 0.7242(7) 0.8115(3) 0.2366(4) 0.048(2) Uani 1 1 d . . . . .
O68 O 1.0562(7) 0.9604(3) 0.3855(4) 0.0469(19) Uani 1 1 d . . . . .
N2 N 0.4804(11) 0.7503(4) 0.0106(7) 0.077(4) Uani 1 1 d . . . . .
N5 N 0.4767(10) 0.6733(4) 0.0283(7) 0.063(3) Uani 1 1 d . . . . .
N6 N 0.6337(7) 0.6652(3) 0.1250(5) 0.042(2) Uani 1 1 d . . . . .
H6 H 0.692977 0.676642 0.151603 0.050 Uiso 1 1 calc R U . . .
N8 N 0.5333(7) 0.6122(3) 0.1712(5) 0.039(2) Uani 1 1 d . . . . .
H8 H 0.550212 0.621750 0.216633 0.047 Uiso 1 1 calc R U . . .
N10 N 0.4151(7) 0.5692(3) 0.0793(5) 0.041(2) Uani 1 1 d . . . . .
N13 N 0.2784(8) 0.5717(3) 0.1226(5) 0.044(2) Uani 1 1 d . . . . .
N14 N 0.3543(7) 0.6165(3) 0.2275(5) 0.038(2) Uani 1 1 d . . . . .
H14 H 0.412206 0.624628 0.260741 0.046 Uiso 1 1 calc R U . . .
N16 N 0.2394(8) 0.6747(3) 0.2441(6) 0.045(2) Uani 1 1 d . . . . .
H16 H 0.252928 0.688598 0.286448 0.054 Uiso 1 1 calc R U . . .
N18 N 0.1665(12) 0.6779(4) 0.1153(6) 0.071(4) Uani 1 1 d . . . . .
N21 N 0.1610(11) 0.7557(4) 0.0977(6) 0.068(4) Uani 1 1 d . . . . .
N22 N 0.2341(8) 0.7795(3) 0.2214(5) 0.041(2) Uani 1 1 d . . . . .
H22 H 0.243030 0.773649 0.267543 0.050 Uiso 1 1 calc R U . . .
N24 N 0.3485(8) 0.8254(3) 0.1809(5) 0.039(2) Uani 1 1 d . . . . .
H24 H 0.406596 0.817127 0.213707 0.047 Uiso 1 1 calc R U . . .
N26 N 0.2667(9) 0.8545(3) 0.0597(6) 0.049(2) Uani 1 1 d . . . . .
N29 N 0.4053(9) 0.8540(3) 0.0198(5) 0.048(2) Uani 1 1 d . . . . .
N30 N 0.5284(8) 0.8252(3) 0.1274(5) 0.040(2) Uani 1 1 d . . . . .
H30 H 0.543218 0.820889 0.174678 0.047 Uiso 1 1 calc R U . . .
N32 N 0.6389(9) 0.7695(3) 0.1002(6) 0.048(2) Uani 1 1 d . . . . .
H32 H 0.701747 0.761046 0.124835 0.058 Uiso 1 1 calc R U . . .
C3 C 0.5636(11) 0.7387(4) 0.0646(7) 0.051(3) Uani 1 1 d . . . . .
C4 C 0.5615(10) 0.6899(4) 0.0752(6) 0.045(3) Uani 1 1 d . . . . .
C7 C 0.6055(8) 0.6181(3) 0.1308(6) 0.035(2) Uani 1 1 d . . . . .
H7 H 0.571518 0.606464 0.080173 0.042 Uiso 1 1 calc R U . . .
C11 C 0.4415(9) 0.5925(3) 0.1394(6) 0.037(2) Uani 1 1 d . . . . .
C12 C 0.3540(9) 0.5947(4) 0.1650(6) 0.038(2) Uani 1 1 d . . . . .
C15 C 0.2558(9) 0.6261(3) 0.2381(7) 0.039(2) Uani 1 1 d . . . . .
H15 H 0.199333 0.613587 0.195686 0.047 Uiso 1 1 calc R U . . .
C19 C 0.2008(10) 0.6976(4) 0.1782(6) 0.0451(19) Uani 1 1 d . . . . .
C20 C 0.2010(10) 0.7464(4) 0.1679(6) 0.0451(19) Uani 1 1 d . . . . .
C23 C 0.2533(9) 0.8245(3) 0.1975(7) 0.040(2) Uani 1 1 d . . . . .
H23 H 0.195537 0.833086 0.152740 0.048 Uiso 1 1 calc R U . . .
C27 C 0.3446(9) 0.8397(4) 0.1122(6) 0.040(2) Uani 1 1 d . . . . .
C28 C 0.4332(9) 0.8394(4) 0.0873(6) 0.039(2) Uani 1 1 d . . . . .
C31 C 0.6064(9) 0.8168(3) 0.0939(7) 0.041(3) Uani 1 1 d . . . . .
H31 H 0.575513 0.823797 0.040723 0.049 Uiso 1 1 calc R U . . .
C33 C 0.7029(8) 0.5876(4) 0.1672(6) 0.038(2) Uani 1 1 d . . . . .
C34 C 0.7608(8) 0.5994(3) 0.2472(6) 0.035(2) Uani 1 1 d . . . . .
C35 C 0.8448(8) 0.5711(3) 0.2933(6) 0.035(2) Uani 1 1 d . . . . .
C36 C 0.8911(9) 0.5350(3) 0.2683(7) 0.040(2) Uani 1 1 d . . . . .
H36 H 0.869067 0.527984 0.217628 0.048 Uiso 1 1 calc R U . . .
C37 C 0.9688(9) 0.5093(3) 0.3167(6) 0.040(2) Uani 1 1 d . . . . .
H37 H 0.998892 0.484654 0.299336 0.048 Uiso 1 1 calc R U . . .
C38 C 1.0021(9) 0.5201(4) 0.3908(7) 0.044(3) Uani 1 1 d . . . . .
C39 C 0.9563(11) 0.5564(4) 0.4155(7) 0.052(3) Uani 1 1 d . . . . .
H39 H 0.978087 0.563891 0.465931 0.063 Uiso 1 1 calc R U . . .
C40 C 0.8809(9) 0.5807(4) 0.3672(6) 0.042(3) Uani 1 1 d . . . . .
H40 H 0.851494 0.605425 0.384882 0.050 Uiso 1 1 calc R U . . .
C41 C 1.1268(11) 0.4605(5) 0.4214(9) 0.062(4) Uani 1 1 d . . . . .
H41A H 1.162336 0.471462 0.388578 0.093 Uiso 1 1 calc R U . . .
H41B H 1.075208 0.437979 0.395960 0.093 Uiso 1 1 calc R U . . .
H41C H 1.176149 0.446492 0.464552 0.093 Uiso 1 1 calc R U . . .
C42 C 0.2542(10) 0.6014(4) 0.3104(6) 0.041(3) Uani 1 1 d . . . . .
C43 C 0.3388(10) 0.6136(4) 0.3793(7) 0.049(3) Uani 1 1 d . . . . .
C44 C 0.3692(10) 0.5849(4) 0.4461(6) 0.046(3) Uani 1 1 d . . . . .
C45 C 0.293(3) 0.552(3) 0.460(3) 0.047(5) Uani 0.53(3) 1 d D . P A 1
H45 H 0.224410 0.551239 0.427398 0.057 Uiso 0.53(3) 1 calc R U P A 1
C45A C 0.308(4) 0.557(3) 0.463(3) 0.047(5) Uani 0.47(3) 1 d D . P A 2
H45A H 0.239513 0.552356 0.431683 0.057 Uiso 0.47(3) 1 calc R U P A 2
C46 C 0.325(3) 0.5243(14) 0.5216(19) 0.046(5) Uani 0.53(3) 1 d D . P A 1
H46 H 0.277418 0.504271 0.531309 0.056 Uiso 0.53(3) 1 calc R U P A 1
C46A C 0.347(3) 0.5328(16) 0.529(2) 0.046(5) Uani 0.47(3) 1 d D . P A 2
H46A H 0.303748 0.513475 0.544516 0.056 Uiso 0.47(3) 1 calc R U P A 2
C47 C 0.424(2) 0.5250(11) 0.5682(15) 0.046(5) Uani 0.53(3) 1 d D . P A 1
C47A C 0.448(3) 0.5369(12) 0.5711(17) 0.046(5) Uani 0.47(3) 1 d D . P A 2
C48 C 0.496(3) 0.5553(10) 0.5554(15) 0.046(5) Uani 0.53(3) 1 d D . P A 1
H48 H 0.564816 0.555952 0.587728 0.056 Uiso 0.53(3) 1 calc R U P A 1
C48A C 0.509(3) 0.5708(11) 0.5534(17) 0.046(5) Uani 0.47(3) 1 d D . P A 2
H48A H 0.577620 0.575749 0.584301 0.056 Uiso 0.47(3) 1 calc R U P A 2
C49 C 0.466(3) 0.5837(11) 0.4957(18) 0.047(5) Uani 0.53(3) 1 d D . P A 1
H49 H 0.514938 0.603910 0.488456 0.057 Uiso 0.53(3) 1 calc R U P A 1
C49A C 0.469(4) 0.5964(13) 0.491(2) 0.047(5) Uani 0.47(3) 1 d D . P A 2
H49A H 0.505739 0.620674 0.479576 0.057 Uiso 0.47(3) 1 calc R U P A 2
C50 C 0.394(3) 0.4645(14) 0.641(2) 0.067(8) Uani 0.53(3) 1 d D . P A 1
H50A H 0.379468 0.441872 0.601390 0.101 Uiso 0.53(3) 1 calc R U P A 1
H50B H 0.330698 0.478955 0.640579 0.101 Uiso 0.53(3) 1 calc R U P A 1
H50C H 0.427109 0.449528 0.687708 0.101 Uiso 0.53(3) 1 calc R U P A 1
C50A C 0.438(4) 0.4743(15) 0.646(3) 0.067(8) Uani 0.47(3) 1 d D . P A 2
H50D H 0.430102 0.451119 0.608108 0.101 Uiso 0.47(3) 1 calc R U P A 2
H50E H 0.370667 0.484865 0.644929 0.101 Uiso 0.47(3) 1 calc R U P A 2
H50F H 0.474575 0.461094 0.693938 0.101 Uiso 0.47(3) 1 calc R U P A 2
C51 C 0.2619(9) 0.8606(4) 0.2589(6) 0.042(3) Uani 1 1 d . . . . .
C52 C 0.3442(9) 0.8531(3) 0.3324(6) 0.039(2) Uani 1 1 d . . . . .
C53 C 0.3675(9) 0.8859(3) 0.3925(6) 0.037(2) Uani 1 1 d . . . . .
C54 C 0.3098(10) 0.9259(4) 0.3938(7) 0.042(3) Uani 1 1 d . . . . .
H54 H 0.249444 0.932169 0.354126 0.050 Uiso 1 1 calc R U . . .
C55 C 0.3406(10) 0.9554(4) 0.4517(7) 0.044(3) Uani 1 1 d . . . . .
H55 H 0.302097 0.982126 0.451751 0.053 Uiso 1 1 calc R U . . .
C56 C 0.4292(9) 0.9460(3) 0.5111(6) 0.038(2) Uani 1 1 d . . . . .
C57 C 0.4853(9) 0.9066(4) 0.5117(7) 0.044(3) Uani 1 1 d . . . . .
H57 H 0.545016 0.900181 0.551966 0.052 Uiso 1 1 calc R U . . .
C58 C 0.4529(10) 0.8764(4) 0.4524(6) 0.043(3) Uani 1 1 d . . . . .
H58 H 0.489964 0.849033 0.453372 0.052 Uiso 1 1 calc R U . . .
C59 C 0.5384(10) 0.9695(4) 0.6292(7) 0.048(3) Uani 1 1 d . . . . .
H59A H 0.598604 0.962064 0.615623 0.072 Uiso 1 1 calc R U . . .
H59B H 0.522361 0.943770 0.655817 0.072 Uiso 1 1 calc R U . . .
H59C H 0.552469 0.996592 0.660434 0.072 Uiso 1 1 calc R U . . .
C60 C 0.6992(9) 0.8487(4) 0.1255(6) 0.041(2) Uani 1 1 d . . . . .
C61 C 0.7550(9) 0.8429(4) 0.2091(6) 0.041(3) Uani 1 1 d . . . . .
C62 C 0.8353(9) 0.8732(4) 0.2518(6) 0.041(2) Uani 1 1 d . . . . .
C63 C 0.8791(9) 0.9098(4) 0.2241(7) 0.042(3) Uani 1 1 d . . . . .
H63 H 0.856874 0.915213 0.172953 0.050 Uiso 1 1 calc R U . . .
C64 C 0.9529(10) 0.9374(4) 0.2699(7) 0.047(3) Uani 1 1 d . . . . .
H64 H 0.982542 0.960915 0.249865 0.056 Uiso 1 1 calc R U . . .
C65 C 0.9843(8) 0.9312(4) 0.3447(6) 0.038(2) Uani 1 1 d . . . . .
C66 C 0.9430(10) 0.8954(4) 0.3741(7) 0.046(3) Uani 1 1 d . . . . .
H66 H 0.964103 0.891025 0.425458 0.055 Uiso 1 1 calc R U . . .
C67 C 0.8720(9) 0.8669(4) 0.3282(6) 0.041(2) Uani 1 1 d . . . . .
H67 H 0.846669 0.842038 0.348551 0.049 Uiso 1 1 calc R U . . .
C68 C 1.0851(10) 0.9571(4) 0.4626(6) 0.047(3) Uani 1 1 d . . . . .
H68A H 1.023864 0.957942 0.477117 0.071 Uiso 1 1 calc R U . . .
H68B H 1.129716 0.982766 0.484987 0.071 Uiso 1 1 calc R U . . .
H68C H 1.121663 0.928430 0.478848 0.071 Uiso 1 1 calc R U . . .
S76A S 0.6109(13) 0.6852(5) 0.3566(8) 0.075(5) Uani 0.303(9) 1 d G . P B -2
O76A O 0.5307(15) 0.6809(9) 0.2825(9) 0.051(3) Uani 0.303(9) 1 d G . P B -2
C77A C 0.559(3) 0.7227(12) 0.4099(16) 0.077(6) Uani 0.303(9) 1 d G . P B -2
H77D H 0.609294 0.726450 0.458872 0.116 Uiso 0.303(9) 1 calc R U P B -2
H77E H 0.544067 0.752499 0.385892 0.116 Uiso 0.303(9) 1 calc R U P B -2
H77F H 0.496301 0.709513 0.413788 0.116 Uiso 0.303(9) 1 calc R U P B -2
C78A C 0.706(2) 0.7248(12) 0.3471(18) 0.076(6) Uani 0.303(9) 1 d G . P B -2
H78D H 0.760110 0.728526 0.394430 0.114 Uiso 0.303(9) 1 calc R U P B -2
H78E H 0.735814 0.712835 0.311435 0.114 Uiso 0.303(9) 1 calc R U P B -2
H78F H 0.673960 0.754294 0.330403 0.114 Uiso 0.303(9) 1 calc R U P B -2
S79 S 0.9074(6) 0.7038(2) 0.2546(4) 0.072(3) Uani 0.580(13) 1 d G . P C -1
O79 O 0.8052(14) 0.7198(11) 0.2047(12) 0.058(3) Uani 0.580(13) 1 d G . P C -1
C80 C 0.912(2) 0.7164(12) 0.3471(7) 0.143(14) Uani 0.580(13) 1 d G U P C -1
H80D H 0.977684 0.706443 0.381527 0.214 Uiso 0.580(13) 1 calc R U P C -1
H80E H 0.903986 0.749250 0.352315 0.214 Uiso 0.580(13) 1 calc R U P C -1
H80F H 0.856405 0.700208 0.357487 0.214 Uiso 0.580(13) 1 calc R U P C -1
C81 C 1.001(3) 0.7460(11) 0.2507(18) 0.108(8) Uani 0.580(13) 1 d G . P C -1
H81D H 1.068525 0.736686 0.282714 0.162 Uiso 0.580(13) 1 calc R U P C -1
H81E H 1.000883 0.748547 0.200411 0.162 Uiso 0.580(13) 1 calc R U P C -1
H81F H 0.982911 0.775511 0.266797 0.162 Uiso 0.580(13) 1 calc R U P C -1
O70 O 0.5484(9) 0.8620(4) 0.2692(6) 0.074(3) Uani 1 1 d . . . . .
N70 N 0.6534(8) 0.8821(3) 0.3792(6) 0.047(2) Uani 1 1 d . . . . .
C70 C 0.6031(12) 0.8527(6) 0.3292(9) 0.067(4) Uani 1 1 d . . . . .
H70 H 0.610966 0.821331 0.341937 0.081 Uiso 1 1 calc R U . . .
C71 C 0.6515(18) 0.9299(5) 0.3706(11) 0.100(7) Uani 1 1 d . . . . .
H71A H 0.695355 0.944106 0.415790 0.150 Uiso 1 1 calc R U . . .
H71B H 0.676414 0.937890 0.330395 0.150 Uiso 1 1 calc R U . . .
H71C H 0.581286 0.941000 0.359490 0.150 Uiso 1 1 calc R U . . .
C72 C 0.7159(13) 0.8642(6) 0.4500(8) 0.074(5) Uani 1 1 d . . . . .
H72A H 0.749101 0.889467 0.482124 0.110 Uiso 1 1 calc R U . . .
H72B H 0.672464 0.847309 0.472013 0.110 Uiso 1 1 calc R U . . .
H72C H 0.768088 0.843757 0.443520 0.110 Uiso 1 1 calc R U . . .
O73 O 0.2646(11) 0.7382(4) 0.3639(6) 0.064(3) Uani 0.867(16) 1 d D . P D 1
O73A O 0.233(5) 0.743(3) 0.329(3) 0.064(3) Uani 0.133(16) 1 d D . P D 2
N73 N 0.311(2) 0.7717(6) 0.4726(10) 0.097(7) Uani 0.867(16) 1 d D . P D 1
N73A N 0.358(4) 0.7433(16) 0.435(3) 0.097(7) Uani 0.133(16) 1 d D . P D 2
C73 C 0.315(2) 0.7413(7) 0.4278(12) 0.094(5) Uani 0.867(16) 1 d D U P D 1
H73 H 0.363162 0.717652 0.446669 0.113 Uiso 0.867(16) 1 calc R U P D 1
C73A C 0.314(5) 0.730(2) 0.371(3) 0.094(5) Uani 0.133(16) 1 d D . P D 2
H73A H 0.347525 0.706854 0.353620 0.113 Uiso 0.133(16) 1 calc R U P D 2
C74 C 0.222(2) 0.8014(7) 0.4564(11) 0.094(5) Uani 0.867(16) 1 d D U P D 1
H74A H 0.231858 0.823004 0.496640 0.141 Uiso 0.867(16) 1 calc R U P D 1
H74B H 0.214013 0.818163 0.411177 0.141 Uiso 0.867(16) 1 calc R U P D 1
H74C H 0.161234 0.782939 0.450608 0.141 Uiso 0.867(16) 1 calc R U P D 1
C74A C 0.313(11) 0.778(4) 0.468(7) 0.094(5) Uani 0.133(16) 1 d D . P D 2
H74D H 0.358055 0.784473 0.517911 0.141 Uiso 0.133(16) 1 calc R U P D 2
H74E H 0.304231 0.806485 0.439049 0.141 Uiso 0.133(16) 1 calc R U P D 2
H74F H 0.246192 0.768182 0.469054 0.141 Uiso 0.133(16) 1 calc R U P D 2
C75 C 0.380(2) 0.7777(8) 0.5444(11) 0.103(8) Uani 0.867(16) 1 d D U P D 1
H75A H 0.358789 0.804107 0.566860 0.154 Uiso 0.867(16) 1 calc R U P D 1
H75B H 0.379357 0.750367 0.573330 0.154 Uiso 0.867(16) 1 calc R U P D 1
H75C H 0.448955 0.782715 0.542847 0.154 Uiso 0.867(16) 1 calc R U P D 1
C75A C 0.452(5) 0.729(3) 0.485(4) 0.103(8) Uani 0.133(16) 1 d D . P D 2
H75D H 0.465381 0.746065 0.531146 0.154 Uiso 0.133(16) 1 calc R U P D 2
H75E H 0.448380 0.696390 0.495114 0.154 Uiso 0.133(16) 1 calc R U P D 2
H75F H 0.506425 0.734690 0.465110 0.154 Uiso 0.133(16) 1 calc R U P D 2
O76 O 0.5545(8) 0.6344(3) 0.3145(6) 0.051(3) Uani 0.697(9) 1 d G . P B -1
N76 N 0.6064(9) 0.7067(3) 0.3562(5) 0.059(5) Uani 0.697(9) 1 d G . P B -1
C76 C 0.5984(8) 0.6608(3) 0.3632(5) 0.054(5) Uani 0.697(9) 1 d G . P B -1
H76 H 0.629944 0.648175 0.410371 0.064 Uiso 0.697(9) 1 calc R U P B -1
C77 C 0.6604(15) 0.7352(4) 0.4179(7) 0.077(6) Uani 0.697(9) 1 d G . P B -1
H77A H 0.657633 0.766993 0.401947 0.116 Uiso 0.697(9) 1 calc R U P B -1
H77B H 0.628145 0.732534 0.455703 0.116 Uiso 0.697(9) 1 calc R U P B -1
H77C H 0.731776 0.725363 0.437812 0.116 Uiso 0.697(9) 1 calc R U P B -1
C78 C 0.5604(17) 0.7287(4) 0.2859(7) 0.076(6) Uani 0.697(9) 1 d G . P B -1
H78A H 0.573636 0.761522 0.291035 0.114 Uiso 0.697(9) 1 calc R U P B -1
H78B H 0.590024 0.716103 0.250643 0.114 Uiso 0.697(9) 1 calc R U P B -1
H78C H 0.486509 0.723281 0.268687 0.114 Uiso 0.697(9) 1 calc R U P B -1
O79A O 0.797(2) 0.7158(14) 0.1999(17) 0.058(3) Uani 0.420(13) 1 d G . P C -2
N79A N 0.9472(19) 0.7316(8) 0.2919(10) 0.076(10) Uani 0.420(13) 1 d G . P C -2
C79A C 0.8480(16) 0.7178(11) 0.2642(14) 0.072(3) Uani 0.420(13) 1 d G . P C -2
H79A H 0.815715 0.708970 0.298324 0.086 Uiso 0.420(13) 1 calc R U P C -2
C80A C 1.002(3) 0.7327(16) 0.3699(12) 0.143(14) Uani 0.420(13) 1 d G U P C -2
H80A H 1.071493 0.743535 0.378759 0.214 Uiso 0.420(13) 1 calc R U P C -2
H80B H 0.966438 0.753423 0.393368 0.214 Uiso 0.420(13) 1 calc R U P C -2
H80C H 1.003422 0.702053 0.390175 0.214 Uiso 0.420(13) 1 calc R U P C -2
C81A C 1.002(4) 0.746(2) 0.2436(19) 0.108(8) Uani 0.420(13) 1 d G . P C -2
H81A H 1.072159 0.754478 0.272650 0.162 Uiso 0.420(13) 1 calc R U P C -2
H81B H 1.004460 0.720509 0.211076 0.162 Uiso 0.420(13) 1 calc R U P C -2
H81C H 0.967474 0.771869 0.214368 0.162 Uiso 0.420(13) 1 calc R U P C -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'
Br Br -0.6763 1.2805 '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'
S S 0.3331 0.5567 '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
0 1 0 0.0153
0 -1 0 0.0150
1 0 -1 0.0231
-1 0 1 0.0365
-1 0 0 0.0578
1 0 0 0.0605
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
N5 O1 N2 108.6(10) . . ?
N13 O9 N10 110.1(7) . . ?
N21 O17 N18 111.1(9) . . ?
N29 O25 N26 110.6(9) . . ?
C38 O41 C41 117.3(11) . . ?
C47 O50 C50 116(3) . . ?
C47A O50A C50A 115(3) . . ?
C56 O59 C59 117.4(9) . . ?
C65 O68 C68 118.1(9) . . ?
C3 N2 O1 107.1(11) . . ?
C4 N5 O1 107.2(10) . . ?
C4 N6 H6 122.8 . . ?
C4 N6 C7 114.3(10) . . ?
C7 N6 H6 122.8 . . ?
C7 N8 H8 119.6 . . ?
C11 N8 H8 119.6 . . ?
C11 N8 C7 120.9(9) . . ?
C11 N10 O9 105.8(8) . . ?
C12 N13 O9 105.2(9) . . ?
C12 N14 H14 120.6 . . ?
C12 N14 C15 118.7(9) . . ?
C15 N14 H14 120.6 . . ?
C15 N16 H16 122.4 . . ?
C19 N16 H16 122.4 . . ?
C19 N16 C15 115.1(10) . . ?
C19 N18 O17 105.5(10) . . ?
C20 N21 O17 104.9(10) . . ?
C20 N22 H22 121.6 . . ?
C20 N22 C23 116.7(9) . . ?
C23 N22 H22 121.6 . . ?
C23 N24 H24 121.0 . . ?
C27 N24 H24 121.0 . . ?
C27 N24 C23 118.0(10) . . ?
C27 N26 O25 106.4(10) . . ?
C28 N29 O25 105.4(9) . . ?
C28 N30 H30 119.3 . . ?
C28 N30 C31 121.4(9) . . ?
C31 N30 H30 119.3 . . ?
C3 N32 H32 122.5 . . ?
C3 N32 C31 114.9(11) . . ?
C31 N32 H32 122.5 . . ?
N2 C3 N32 123.1(12) . . ?
N2 C3 C4 108.3(11) . . ?
N32 C3 C4 128.6(12) . . ?
N5 C4 N6 125.3(11) . . ?
N5 C4 C3 108.8(11) . . ?
N6 C4 C3 126.0(11) . . ?
N6 C7 N8 113.8(8) . . ?
N6 C7 H7 107.5 . . ?
N6 C7 C33 111.2(9) . . ?
N8 C7 H7 107.5 . . ?
N8 C7 C33 109.1(9) . . ?
C33 C7 H7 107.5 . . ?
N8 C11 C12 126.3(10) . . ?
N10 C11 N8 125.5(10) . . ?
N10 C11 C12 108.2(10) . . ?
N13 C12 N14 125.0(10) . . ?
N13 C12 C11 110.6(9) . . ?
N14 C12 C11 124.3(10) . . ?
N14 C15 H15 108.9 . . ?
N14 C15 C42 108.7(9) . . ?
N16 C15 N14 112.0(8) . . ?
N16 C15 H15 108.9 . . ?
N16 C15 C42 109.3(9) . . ?
C42 C15 H15 108.9 . . ?
N16 C19 C20 126.1(10) . . ?
N18 C19 N16 124.3(11) . . ?
N18 C19 C20 109.3(11) . . ?
N21 C20 N22 123.4(11) . . ?
N21 C20 C19 109.1(10) . . ?
N22 C20 C19 127.4(11) . . ?
N22 C23 N24 111.2(8) . . ?
N22 C23 H23 109.1 . . ?
N22 C23 C51 110.3(9) . . ?
N24 C23 H23 109.1 . . ?
N24 C23 C51 108.0(9) . . ?
C51 C23 H23 109.1 . . ?
N24 C27 C28 123.3(11) . . ?
N26 C27 N24 128.2(11) . . ?
N26 C27 C28 108.5(10) . . ?
N29 C28 N30 125.8(10) . . ?
N29 C28 C27 109.0(11) . . ?
N30 C28 C27 125.2(10) . . ?
N30 C31 H31 107.4 . . ?
N30 C31 C60 111.4(9) . . ?
N32 C31 N30 112.4(9) . . ?
N32 C31 H31 107.4 . . ?
N32 C31 C60 110.6(10) . . ?
C60 C31 H31 107.4 . . ?
Br2 C33 Br1 110.8(5) . . ?
C7 C33 Br1 107.3(7) . . ?
C7 C33 Br2 106.6(7) . . ?
C34 C33 Br1 107.5(7) . . ?
C34 C33 Br2 110.5(7) . . ?
C34 C33 C7 114.1(8) . . ?
O34 C34 C33 116.1(10) . . ?
O34 C34 C35 121.6(10) . . ?
C35 C34 C33 122.3(9) . . ?
C36 C35 C34 125.1(10) . . ?
C40 C35 C34 117.3(9) . . ?
C40 C35 C36 117.5(11) . . ?
C35 C36 H36 119.5 . . ?
C37 C36 C35 120.9(11) . . ?
C37 C36 H36 119.5 . . ?
C36 C37 H37 120.3 . . ?
C36 C37 C38 119.3(10) . . ?
C38 C37 H37 120.3 . . ?
O41 C38 C37 125.4(11) . . ?
O41 C38 C39 115.1(11) . . ?
C37 C38 C39 119.5(11) . . ?
C38 C39 H39 120.1 . . ?
C40 C39 C38 119.8(11) . . ?
C40 C39 H39 120.1 . . ?
C35 C40 H40 118.6 . . ?
C39 C40 C35 122.8(11) . . ?
C39 C40 H40 118.6 . . ?
O41 C41 H41A 109.5 . . ?
O41 C41 H41B 109.5 . . ?
O41 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
Br4 C42 Br3 108.8(6) . . ?
C15 C42 Br3 103.8(7) . . ?
C15 C42 Br4 107.4(8) . . ?
C43 C42 Br3 110.7(8) . . ?
C43 C42 Br4 109.4(7) . . ?
C43 C42 C15 116.3(10) . . ?
O43 C43 C42 115.5(11) . . ?
O43 C43 C44 120.6(13) . . ?
C44 C43 C42 123.7(11) . . ?
C43 C44 C45 119.8(15) . . ?
C45A C44 C43 123.9(18) . . ?
C45A C44 C49A 126(2) . . ?
C49 C44 C43 123.9(16) . . ?
C49 C44 C45 116(2) . . ?
C49A C44 C43 110.1(15) . . ?
C44 C45 H45 120.8 . . ?
C46 C45 C44 118(2) . . ?
C46 C45 H45 120.8 . . ?
C44 C45A H45A 121.4 . . ?
C44 C45A C46A 117(3) . . ?
C46A C45A H45A 121.4 . . ?
C45 C46 H46 119.2 . . ?
C47 C46 C45 122(2) . . ?
C47 C46 H46 119.2 . . ?
C45A C46A H46A 119.5 . . ?
C47A C46A C45A 121(2) . . ?
C47A C46A H46A 119.5 . . ?
O50 C47 C46 126(2) . . ?
O50 C47 C48 114(2) . . ?
C46 C47 C48 120.2(19) . . ?
O50A C47A C46A 126(2) . . ?
O50A C47A C48A 115(2) . . ?
C46A C47A C48A 119(2) . . ?
C47 C48 H48 120.5 . . ?
C49 C48 C47 119(2) . . ?
C49 C48 H48 120.5 . . ?
C47A C48A H48A 120.3 . . ?
C49A C48A C47A 119(2) . . ?
C49A C48A H48A 120.3 . . ?
C44 C49 C48 124(3) . . ?
C44 C49 H49 117.8 . . ?
C48 C49 H49 117.8 . . ?
C44 C49A H49A 121.7 . . ?
C48A C49A C44 117(3) . . ?
C48A C49A H49A 121.7 . . ?
O50 C50 H50A 109.5 . . ?
O50 C50 H50B 109.5 . . ?
O50 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O50A C50A H50D 109.5 . . ?
O50A C50A H50E 109.5 . . ?
O50A C50A H50F 109.5 . . ?
H50D C50A H50E 109.5 . . ?
H50D C50A H50F 109.5 . . ?
H50E C50A H50F 109.5 . . ?
Br6 C51 Br5 107.8(5) . . ?
C23 C51 Br5 104.9(8) . . ?
C23 C51 Br6 105.9(7) . . ?
C52 C51 Br5 110.2(7) . . ?
C52 C51 Br6 110.1(8) . . ?
C52 C51 C23 117.4(9) . . ?
O52 C52 C51 114.5(10) . . ?
O52 C52 C53 121.8(11) . . ?
C53 C52 C51 123.6(9) . . ?
C54 C53 C52 125.3(11) . . ?
C58 C53 C52 116.0(9) . . ?
C58 C53 C54 118.7(10) . . ?
C53 C54 H54 119.7 . . ?
C55 C54 C53 120.7(12) . . ?
C55 C54 H54 119.7 . . ?
C54 C55 H55 120.0 . . ?
C54 C55 C56 120.0(10) . . ?
C56 C55 H55 120.0 . . ?
O59 C56 C55 114.2(9) . . ?
O59 C56 C57 125.5(11) . . ?
C57 C56 C55 120.3(11) . . ?
C56 C57 H57 120.3 . . ?
C56 C57 C58 119.4(11) . . ?
C58 C57 H57 120.3 . . ?
C53 C58 C57 120.9(10) . . ?
C53 C58 H58 119.6 . . ?
C57 C58 H58 119.6 . . ?
O59 C59 H59A 109.5 . . ?
O59 C59 H59B 109.5 . . ?
O59 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
Br8 C60 Br7 109.4(5) . . ?
C31 C60 Br7 106.5(8) . . ?
C31 C60 Br8 109.9(7) . . ?
C31 C60 C61 114.0(9) . . ?
C61 C60 Br7 108.2(7) . . ?
C61 C60 Br8 108.7(8) . . ?
O61 C61 C60 114.6(11) . . ?
O61 C61 C62 122.0(11) . . ?
C62 C61 C60 123.4(9) . . ?
C63 C62 C61 126.1(11) . . ?
C67 C62 C61 117.5(10) . . ?
C67 C62 C63 116.4(11) . . ?
C62 C63 H63 119.3 . . ?
C64 C63 C62 121.3(11) . . ?
C64 C63 H63 119.3 . . ?
C63 C64 H64 119.7 . . ?
C63 C64 C65 120.7(11) . . ?
C65 C64 H64 119.7 . . ?
O68 C65 C64 116.6(10) . . ?
O68 C65 C66 123.7(11) . . ?
C64 C65 C66 119.7(11) . . ?
C65 C66 H66 120.2 . . ?
C67 C66 C65 119.6(11) . . ?
C67 C66 H66 120.2 . . ?
C62 C67 H67 118.9 . . ?
C66 C67 C62 122.2(10) . . ?
C66 C67 H67 118.9 . . ?
O68 C68 H68A 109.5 . . ?
O68 C68 H68B 109.5 . . ?
O68 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
O76A S76A C77A 106.8 . . ?
O76A S76A C78A 106.8 . . ?
C78A S76A C77A 96.2 . . ?
S76A C77A H77D 109.5 . . ?
S76A C77A H77E 109.5 . . ?
S76A C77A H77F 109.5 . . ?
H77D C77A H77E 109.5 . . ?
H77D C77A H77F 109.5 . . ?
H77E C77A H77F 109.5 . . ?
S76A C78A H78D 109.5 . . ?
S76A C78A H78E 109.5 . . ?
S76A C78A H78F 109.5 . . ?
H78D C78A H78E 109.5 . . ?
H78D C78A H78F 109.5 . . ?
H78E C78A H78F 109.5 . . ?
O79 S79 C80 106.9 . . ?
O79 S79 C81 107.1 . . ?
C81 S79 C80 96.5 . . ?
S79 C80 H80D 109.5 . . ?
S79 C80 H80E 109.5 . . ?
S79 C80 H80F 109.5 . . ?
H80D C80 H80E 109.5 . . ?
H80D C80 H80F 109.5 . . ?
H80E C80 H80F 109.5 . . ?
S79 C81 H81D 109.5 . . ?
S79 C81 H81E 109.5 . . ?
S79 C81 H81F 109.5 . . ?
H81D C81 H81E 109.5 . . ?
H81D C81 H81F 109.5 . . ?
H81E C81 H81F 109.5 . . ?
C70 N70 C71 125.5(14) . . ?
C70 N70 C72 117.6(13) . . ?
C71 N70 C72 116.9(13) . . ?
O70 C70 N70 125.5(17) . . ?
O70 C70 H70 117.2 . . ?
N70 C70 H70 117.2 . . ?
N70 C71 H71A 109.5 . . ?
N70 C71 H71B 109.5 . . ?
N70 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
N70 C72 H72A 109.5 . . ?
N70 C72 H72B 109.5 . . ?
N70 C72 H72C 109.5 . . ?
H72A C72 H72B 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C73 N73 C74 120(2) . . ?
C73 N73 C75 127(3) . . ?
C75 N73 C74 112.6(18) . . ?
C73A N73A C74A 121(5) . . ?
C73A N73A C75A 129(4) . . ?
C75A N73A C74A 110(6) . . ?
O73 C73 N73 128(3) . . ?
O73 C73 H73 115.8 . . ?
N73 C73 H73 115.8 . . ?
O73A C73A N73A 127(5) . . ?
O73A C73A H73A 116.3 . . ?
N73A C73A H73A 116.3 . . ?
N73 C74 H74A 109.5 . . ?
N73 C74 H74B 109.5 . . ?
N73 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
N73A C74A H74D 109.5 . . ?
N73A C74A H74E 109.5 . . ?
N73A C74A H74F 109.5 . . ?
H74D C74A H74E 109.5 . . ?
H74D C74A H74F 109.5 . . ?
H74E C74A H74F 109.5 . . ?
N73 C75 H75A 109.5 . . ?
N73 C75 H75B 109.5 . . ?
N73 C75 H75C 109.5 . . ?
H75A C75 H75B 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
N73A C75A H75D 109.5 . . ?
N73A C75A H75E 109.5 . . ?
N73A C75A H75F 109.5 . . ?
H75D C75A H75E 109.5 . . ?
H75D C75A H75F 109.5 . . ?
H75E C75A H75F 109.5 . . ?
C76 N76 C77 121.7 . . ?
C76 N76 C78 120.5 . . ?
C77 N76 C78 117.7 . . ?
O76 C76 N76 126.0 . . ?
O76 C76 H76 117.0 . . ?
N76 C76 H76 117.0 . . ?
N76 C77 H77A 109.5 . . ?
N76 C77 H77B 109.5 . . ?
N76 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
N76 C78 H78A 109.5 . . ?
N76 C78 H78B 109.5 . . ?
N76 C78 H78C 109.5 . . ?
H78A C78 H78B 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C79A N79A C80A 121.8 . . ?
C79A N79A C81A 120.5 . . ?
C80A N79A C81A 117.7 . . ?
O79A C79A N79A 126.0 . . ?
O79A C79A H79A 117.0 . . ?
N79A C79A H79A 117.0 . . ?
N79A C80A H80A 109.5 . . ?
N79A C80A H80B 109.5 . . ?
N79A C80A H80C 109.5 . . ?
H80A C80A H80B 109.5 . . ?
H80A C80A H80C 109.5 . . ?
H80B C80A H80C 109.5 . . ?
N79A C81A H81A 109.5 . . ?
N79A C81A H81B 109.5 . . ?
N79A C81A H81C 109.5 . . ?
H81A C81A H81B 109.5 . . ?
H81A C81A H81C 109.5 . . ?
H81B C81A H81C 109.5 . . ?
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
Br1 C33 1.975(10) . ?
Br2 C33 1.936(11) . ?
Br3 C42 1.979(11) . ?
Br4 C42 1.958(12) . ?
Br5 C51 1.963(11) . ?
Br6 C51 1.952(12) . ?
Br7 C60 1.973(11) . ?
Br8 C60 1.941(11) . ?
O1 N2 1.414(15) . ?
O1 N5 1.403(14) . ?
O9 N10 1.423(12) . ?
O9 N13 1.402(11) . ?
O17 N18 1.408(14) . ?
O17 N21 1.388(14) . ?
O25 N26 1.398(12) . ?
O25 N29 1.396(14) . ?
O34 C34 1.214(12) . ?
O41 C38 1.361(14) . ?
O41 C41 1.439(15) . ?
O43 C43 1.225(14) . ?
O50 C47 1.36(2) . ?
O50 C50 1.46(3) . ?
O50A C47A 1.36(2) . ?
O50A C50A 1.46(3) . ?
O52 C52 1.219(13) . ?
O59 C56 1.357(13) . ?
O59 C59 1.443(15) . ?
O61 C61 1.212(13) . ?
O68 C65 1.353(14) . ?
O68 C68 1.418(13) . ?
N2 C3 1.321(18) . ?
N5 C4 1.318(17) . ?
N6 H6 0.8800 . ?
N6 C4 1.351(15) . ?
N6 C7 1.449(13) . ?
N8 H8 0.8800 . ?
N8 C7 1.471(13) . ?
N8 C11 1.349(14) . ?
N10 C11 1.296(14) . ?
N13 C12 1.288(14) . ?
N14 H14 0.8800 . ?
N14 C12 1.371(13) . ?
N14 C15 1.474(13) . ?
N16 H16 0.8800 . ?
N16 C15 1.457(13) . ?
N16 C19 1.386(15) . ?
N18 C19 1.291(15) . ?
N21 C20 1.320(16) . ?
N22 H22 0.8800 . ?
N22 C20 1.384(14) . ?
N22 C23 1.452(12) . ?
N24 H24 0.8800 . ?
N24 C23 1.458(14) . ?
N24 C27 1.383(13) . ?
N26 C27 1.290(16) . ?
N29 C28 1.307(14) . ?
N30 H30 0.8800 . ?
N30 C28 1.358(15) . ?
N30 C31 1.455(13) . ?
N32 H32 0.8800 . ?
N32 C3 1.380(16) . ?
N32 C31 1.452(14) . ?
C3 C4 1.449(16) . ?
C7 H7 1.0000 . ?
C7 C33 1.579(15) . ?
C11 C12 1.457(14) . ?
C15 H15 1.0000 . ?
C15 C42 1.585(15) . ?
C19 C20 1.445(16) . ?
C23 H23 1.0000 . ?
C23 C51 1.570(15) . ?
C27 C28 1.462(15) . ?
C31 H31 1.0000 . ?
C31 C60 1.547(16) . ?
C33 C34 1.532(16) . ?
C34 C35 1.469(16) . ?
C35 C36 1.407(14) . ?
C35 C40 1.383(15) . ?
C36 H36 0.9500 . ?
C36 C37 1.394(16) . ?
C37 H37 0.9500 . ?
C37 C38 1.395(17) . ?
C38 C39 1.403(17) . ?
C39 H39 0.9500 . ?
C39 C40 1.353(18) . ?
C40 H40 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.502(18) . ?
C43 C44 1.486(17) . ?
C44 C45 1.51(6) . ?
C44 C45A 1.30(6) . ?
C44 C49 1.37(4) . ?
C44 C49A 1.41(5) . ?
C45 H45 0.9500 . ?
C45 C46 1.40(2) . ?
C45A H45A 0.9500 . ?
C45A C46A 1.40(2) . ?
C46 H46 0.9500 . ?
C46 C47 1.37(2) . ?
C46A H46A 0.9500 . ?
C46A C47A 1.37(2) . ?
C47 C48 1.42(3) . ?
C47A C48A 1.42(3) . ?
C48 H48 0.9500 . ?
C48 C49 1.38(2) . ?
C48A H48A 0.9500 . ?
C48A C49A 1.37(2) . ?
C49 H49 0.9500 . ?
C49A H49A 0.9500 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C50A H50D 0.9800 . ?
C50A H50E 0.9800 . ?
C50A H50F 0.9800 . ?
C51 C52 1.519(17) . ?
C52 C53 1.463(15) . ?
C53 C54 1.425(14) . ?
C53 C58 1.386(17) . ?
C54 H54 0.9500 . ?
C54 C55 1.369(16) . ?
C55 H55 0.9500 . ?
C55 C56 1.406(17) . ?
C56 C57 1.391(15) . ?
C57 H57 0.9500 . ?
C57 C58 1.404(17) . ?
C58 H58 0.9500 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 C61 1.558(16) . ?
C61 C62 1.451(17) . ?
C62 C63 1.423(15) . ?
C62 C67 1.412(15) . ?
C63 H63 0.9500 . ?
C63 C64 1.376(18) . ?
C64 H64 0.9500 . ?
C64 C65 1.383(16) . ?
C65 C66 1.405(15) . ?
C66 H66 0.9500 . ?
C66 C67 1.373(17) . ?
C67 H67 0.9500 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
S76A O76A 1.5046 . ?
S76A C77A 1.8142 . ?
S76A C78A 1.8135 . ?
C77A H77D 0.9800 . ?
C77A H77E 0.9800 . ?
C77A H77F 0.9800 . ?
C78A H78D 0.9800 . ?
C78A H78E 0.9800 . ?
C78A H78F 0.9800 . ?
S79 O79 1.5027 . ?
S79 C80 1.8129 . ?
S79 C81 1.8083 . ?
C80 H80D 0.9800 . ?
C80 H80E 0.9800 . ?
C80 H80F 0.9800 . ?
C81 H81D 0.9800 . ?
C81 H81E 0.9800 . ?
C81 H81F 0.9800 . ?
O70 C70 1.192(18) . ?
N70 C70 1.314(18) . ?
N70 C71 1.412(17) . ?
N70 C72 1.459(18) . ?
C70 H70 0.9500 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
O73 C73 1.21(2) . ?
O73A C73A 1.21(3) . ?
N73 C73 1.26(2) . ?
N73 C74 1.46(3) . ?
N73 C75 1.41(3) . ?
N73A C73A 1.25(3) . ?
N73A C74A 1.46(4) . ?
N73A C75A 1.41(3) . ?
C73 H73 0.9500 . ?
C73A H73A 0.9500 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C74A H74D 0.9800 . ?
C74A H74E 0.9800 . ?
C74A H74F 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C75A H75D 0.9800 . ?
C75A H75E 0.9800 . ?
C75A H75F 0.9800 . ?
O76 C76 1.2167 . ?
N76 C76 1.3618 . ?
N76 C77 1.4502 . ?
N76 C78 1.4523 . ?
C76 H76 0.9500 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
O79A C79A 1.2164 . ?
N79A C79A 1.3623 . ?
N79A C80A 1.4501 . ?
N79A C81A 1.4535 . ?
C79A H79A 0.9500 . ?
C80A H80A 0.9800 . ?
C80A H80B 0.9800 . ?
C80A H80C 0.9800 . ?
C81A H81A 0.9800 . ?
C81A H81B 0.9800 . ?
C81A H81C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N6 H6 O79 0.88 2.01 2.86(3) 163.3 . yes
N6 H6 O79A 0.88 1.84 2.70(3) 163.8 . yes
N8 H8 O34 0.88 2.44 2.881(13) 111.6 . yes
N8 H8 O76A 0.88 2.22 2.96(2) 141.3 . yes
N8 H8 O76 0.88 1.92 2.776(13) 164.9 . yes
N14 H14 O43 0.88 2.47 2.916(12) 111.8 . yes
N14 H14 O76A 0.88 2.27 2.99(2) 139.7 . yes
N14 H14 O76 0.88 1.92 2.781(14) 164.0 . yes
N16 H16 O73 0.88 2.06 2.909(15) 161.6 . yes
N16 H16 O73A 0.88 1.86 2.62(7) 142.8 . yes
N22 H22 O73 0.88 2.07 2.920(14) 161.2 . yes
N22 H22 O73A 0.88 1.55 2.36(7) 152.6 . yes
N24 H24 O52 0.88 2.45 2.879(12) 110.9 . yes
N24 H24 O70 0.88 2.32 2.939(15) 127.8 . yes
N30 H30 O61 0.88 2.41 2.867(13) 112.4 . yes
N30 H30 O70 0.88 2.18 2.884(13) 136.9 . yes
N32 H32 O79 0.88 2.11 2.910(16) 150.5 . yes
N32 H32 O79A 0.88 2.09 2.87(3) 147.4 . yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C33 C34 O34 109.7(9) . . . . ?
Br1 C33 C34 C35 -69.5(10) . . . . ?
Br2 C33 C34 O34 -129.3(8) . . . . ?
Br2 C33 C34 C35 51.5(11) . . . . ?
Br3 C42 C43 O43 133.2(10) . . . . ?
Br3 C42 C43 C44 -42.1(13) . . . . ?
Br4 C42 C43 O43 -106.9(10) . . . . ?
Br4 C42 C43 C44 77.9(12) . . . . ?
Br5 C51 C52 O52 118.1(9) . . . . ?
Br5 C51 C52 C53 -65.8(12) . . . . ?
Br6 C51 C52 O52 -123.1(9) . . . . ?
Br6 C51 C52 C53 53.0(12) . . . . ?
Br7 C60 C61 O61 124.8(9) . . . . ?
Br7 C60 C61 C62 -53.5(12) . . . . ?
Br8 C60 C61 O61 -116.5(9) . . . . ?
Br8 C60 C61 C62 65.2(12) . . . . ?
O1 N2 C3 N32 179.5(12) . . . . ?
O1 N2 C3 C4 2.1(17) . . . . ?
O1 N5 C4 N6 178.9(12) . . . . ?
O1 N5 C4 C3 -0.7(15) . . . . ?
O9 N10 C11 N8 -179.7(10) . . . . ?
O9 N10 C11 C12 -1.5(12) . . . . ?
O9 N13 C12 N14 -179.4(10) . . . . ?
O9 N13 C12 C11 -2.3(12) . . . . ?
O17 N18 C19 N16 -177.2(13) . . . . ?
O17 N18 C19 C20 -2.4(17) . . . . ?
O17 N21 C20 N22 179.1(13) . . . . ?
O17 N21 C20 C19 -2.6(16) . . . . ?
O25 N26 C27 N24 -177.8(10) . . . . ?
O25 N26 C27 C28 1.3(12) . . . . ?
O25 N29 C28 N30 177.6(10) . . . . ?
O25 N29 C28 C27 -0.8(12) . . . . ?
O34 C34 C35 C36 -169.6(10) . . . . ?
O34 C34 C35 C40 10.7(15) . . . . ?
O41 C38 C39 C40 179.3(11) . . . . ?
O43 C43 C44 C45 160(4) . . . . ?
O43 C43 C44 C45A 159(5) . . . . ?
O43 C43 C44 C49 -24(2) . . . . ?
O43 C43 C44 C49A -15(2) . . . . ?
O50 C47 C48 C49 -180(3) . . . . ?
O50A C47A C48A C49A 178(4) . . . . ?
O52 C52 C53 C54 -176.4(10) . . . . ?
O52 C52 C53 C58 3.5(15) . . . . ?
O59 C56 C57 C58 -179.1(10) . . . . ?
O61 C61 C62 C63 177.4(11) . . . . ?
O61 C61 C62 C67 -4.6(16) . . . . ?
O68 C65 C66 C67 -178.4(10) . . . . ?
N2 O1 N5 C4 2.0(16) . . . . ?
N2 C3 C4 N5 -0.9(17) . . . . ?
N2 C3 C4 N6 179.4(13) . . . . ?
N5 O1 N2 C3 -2.6(17) . . . . ?
N6 C7 C33 Br1 -53.1(10) . . . . ?
N6 C7 C33 Br2 -171.9(7) . . . . ?
N6 C7 C33 C34 65.9(11) . . . . ?
N8 C7 C33 Br1 -179.4(7) . . . . ?
N8 C7 C33 Br2 61.8(9) . . . . ?
N8 C7 C33 C34 -60.4(11) . . . . ?
N8 C11 C12 N13 -179.3(11) . . . . ?
N8 C11 C12 N14 -2.2(18) . . . . ?
N10 O9 N13 C12 1.4(12) . . . . ?
N10 C11 C12 N13 2.6(14) . . . . ?
N10 C11 C12 N14 179.6(10) . . . . ?
N13 O9 N10 C11 0.1(12) . . . . ?
N14 C15 C42 Br3 -64.7(9) . . . . ?
N14 C15 C42 Br4 -179.9(7) . . . . ?
N14 C15 C42 C43 57.3(12) . . . . ?
N16 C15 C42 Br3 172.8(8) . . . . ?
N16 C15 C42 Br4 57.6(10) . . . . ?
N16 C15 C42 C43 -65.3(13) . . . . ?
N16 C19 C20 N21 178.0(13) . . . . ?
N16 C19 C20 N22 -4(2) . . . . ?
N18 O17 N21 C20 1.2(18) . . . . ?
N18 C19 C20 N21 3.3(17) . . . . ?
N18 C19 C20 N22 -178.5(13) . . . . ?
N21 O17 N18 C19 0.8(18) . . . . ?
N22 C23 C51 Br5 -63.8(10) . . . . ?
N22 C23 C51 Br6 -177.7(8) . . . . ?
N22 C23 C51 C52 58.9(13) . . . . ?
N24 C23 C51 Br5 174.5(7) . . . . ?
N24 C23 C51 Br6 60.5(10) . . . . ?
N24 C23 C51 C52 -62.8(12) . . . . ?
N24 C27 C28 N29 178.8(10) . . . . ?
N24 C27 C28 N30 0.4(17) . . . . ?
N26 O25 N29 C28 1.6(12) . . . . ?
N26 C27 C28 N29 -0.4(13) . . . . ?
N26 C27 C28 N30 -178.7(10) . . . . ?
N29 O25 N26 C27 -1.9(12) . . . . ?
N30 C31 C60 Br7 -58.0(10) . . . . ?
N30 C31 C60 Br8 -176.4(7) . . . . ?
N30 C31 C60 C61 61.3(12) . . . . ?
N32 C3 C4 N5 -178.2(13) . . . . ?
N32 C3 C4 N6 2(2) . . . . ?
N32 C31 C60 Br7 176.3(7) . . . . ?
N32 C31 C60 Br8 57.9(11) . . . . ?
N32 C31 C60 C61 -64.5(12) . . . . ?
C3 N32 C31 N30 63.4(14) . . . . ?
C3 N32 C31 C60 -171.4(10) . . . . ?
C4 N6 C7 N8 -76.4(12) . . . . ?
C4 N6 C7 C33 159.9(9) . . . . ?
C7 N6 C4 N5 -8.0(17) . . . . ?
C7 N6 C4 C3 171.5(11) . . . . ?
C7 N8 C11 N10 14.5(17) . . . . ?
C7 N8 C11 C12 -163.4(10) . . . . ?
C7 C33 C34 O34 -9.2(13) . . . . ?
C7 C33 C34 C35 171.6(9) . . . . ?
C11 N8 C7 N6 121.1(11) . . . . ?
C11 N8 C7 C33 -114.1(11) . . . . ?
C12 N14 C15 N16 -118.9(11) . . . . ?
C12 N14 C15 C42 120.3(10) . . . . ?
C15 N14 C12 N13 -18.2(16) . . . . ?
C15 N14 C12 C11 165.1(10) . . . . ?
C15 N16 C19 N18 10.2(18) . . . . ?
C15 N16 C19 C20 -163.7(12) . . . . ?
C15 C42 C43 O43 15.0(15) . . . . ?
C15 C42 C43 C44 -160.3(10) . . . . ?
C19 N16 C15 N14 82.9(13) . . . . ?
C19 N16 C15 C42 -156.5(10) . . . . ?
C20 N22 C23 N24 -75.0(13) . . . . ?
C20 N22 C23 C51 165.2(10) . . . . ?
C23 N22 C20 N21 -18.7(19) . . . . ?
C23 N22 C20 C19 163.4(12) . . . . ?
C23 N24 C27 N26 3.0(17) . . . . ?
C23 N24 C27 C28 -176.0(9) . . . . ?
C23 C51 C52 O52 -1.9(14) . . . . ?
C23 C51 C52 C53 174.2(9) . . . . ?
C27 N24 C23 N22 124.1(10) . . . . ?
C27 N24 C23 C51 -114.8(11) . . . . ?
C28 N30 C31 N32 -117.2(12) . . . . ?
C28 N30 C31 C60 118.0(11) . . . . ?
C31 N30 C28 N29 -11.5(17) . . . . ?
C31 N30 C28 C27 166.6(10) . . . . ?
C31 N32 C3 N2 21.2(19) . . . . ?
C31 N32 C3 C4 -161.9(12) . . . . ?
C31 C60 C61 O61 6.5(14) . . . . ?
C31 C60 C61 C62 -171.7(10) . . . . ?
C33 C34 C35 C36 9.7(15) . . . . ?
C33 C34 C35 C40 -170.1(9) . . . . ?
C34 C35 C36 C37 -178.3(10) . . . . ?
C34 C35 C40 C39 178.4(11) . . . . ?
C35 C36 C37 C38 -1.0(16) . . . . ?
C36 C35 C40 C39 -1.4(16) . . . . ?
C36 C37 C38 O41 -179.2(10) . . . . ?
C36 C37 C38 C39 0.5(16) . . . . ?
C37 C38 C39 C40 -0.4(18) . . . . ?
C38 C39 C40 C35 0.9(18) . . . . ?
C40 C35 C36 C37 1.4(15) . . . . ?
C41 O41 C38 C37 -0.8(17) . . . . ?
C41 O41 C38 C39 179.5(11) . . . . ?
C42 C43 C44 C45 -25(4) . . . . ?
C42 C43 C44 C45A -26(5) . . . . ?
C42 C43 C44 C49 151(2) . . . . ?
C42 C43 C44 C49A 160(2) . . . . ?
C43 C44 C45 C46 177(5) . . . . ?
C43 C44 C45A C46A -178(4) . . . . ?
C43 C44 C49 C48 -176(2) . . . . ?
C43 C44 C49A C48A -176(3) . . . . ?
C44 C45 C46 C47 -1(9) . . . . ?
C44 C45A C46A C47A -4(10) . . . . ?
C45 C44 C49 C48 0(6) . . . . ?
C45 C46 C47 O50 -180(6) . . . . ?
C45 C46 C47 C48 1(6) . . . . ?
C45A C44 C49A C48A 10(8) . . . . ?
C45A C46A C47A O50A -174(6) . . . . ?
C45A C46A C47A C48A 10(7) . . . . ?
C46 C47 C48 C49 0(4) . . . . ?
C46A C47A C48A C49A -5(5) . . . . ?
C47 C48 C49 C44 -1(5) . . . . ?
C47A C48A C49A C44 -4(5) . . . . ?
C49 C44 C45 C46 1(9) . . . . ?
C49A C44 C45A C46A -6(11) . . . . ?
C50 O50 C47 C46 6(5) . . . . ?
C50 O50 C47 C48 -174(3) . . . . ?
C50A O50A C47A C46A 11(5) . . . . ?
C50A O50A C47A C48A -173(3) . . . . ?
C51 C52 C53 C54 7.7(16) . . . . ?
C51 C52 C53 C58 -172.4(10) . . . . ?
C52 C53 C54 C55 -177.3(10) . . . . ?
C52 C53 C58 C57 176.9(10) . . . . ?
C53 C54 C55 C56 -0.8(16) . . . . ?
C54 C53 C58 C57 -3.2(16) . . . . ?
C54 C55 C56 O59 178.7(9) . . . . ?
C54 C55 C56 C57 -0.7(16) . . . . ?
C55 C56 C57 C58 0.3(16) . . . . ?
C56 C57 C58 C53 1.8(16) . . . . ?
C58 C53 C54 C55 2.8(16) . . . . ?
C59 O59 C56 C55 175.7(9) . . . . ?
C59 O59 C56 C57 -4.9(15) . . . . ?
C60 C61 C62 C63 -4.5(17) . . . . ?
C60 C61 C62 C67 173.6(10) . . . . ?
C61 C62 C63 C64 177.9(11) . . . . ?
C61 C62 C67 C66 -175.7(11) . . . . ?
C62 C63 C64 C65 -2.1(17) . . . . ?
C63 C62 C67 C66 2.6(17) . . . . ?
C63 C64 C65 O68 -179.1(10) . . . . ?
C63 C64 C65 C66 2.2(17) . . . . ?
C64 C65 C66 C67 0.1(17) . . . . ?
C65 C66 C67 C62 -2.6(17) . . . . ?
C67 C62 C63 C64 -0.2(16) . . . . ?
C68 O68 C65 C64 175.7(10) . . . . ?
C68 O68 C65 C66 -5.7(16) . . . . ?
C71 N70 C70 O70 0(2) . . . . ?
C72 N70 C70 O70 179.3(14) . . . . ?
C74 N73 C73 O73 18(4) . . . . ?
C74A N73A C73A O73A 0.0(7) . . . . ?
C75 N73 C73 O73 -171(2) . . . . ?
C75A N73A C73A O73A -180.0(4) . . . . ?
C77 N76 C76 O76 179.9 . . . . ?
C78 N76 C76 O76 0.0 . . . . ?
C80A N79A C79A O79A -180.0 . . . . ?
C81A N79A C79A O79A 0.1 . . . . ?
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
-0.0000 1.0000 -0.0001 0.0239 -0.0404 -0.0235
0.0000 -1.0000 0.0001 -0.0239 0.0404 0.0235
0.9999 0.0011 -1.0002 0.1008 0.0645 -0.0081
-0.9999 -0.0011 1.0002 -0.1008 -0.0645 0.0081
-0.9996 -0.0013 -0.0003 -0.0514 -0.0743 0.0754
0.9996 0.0013 0.0003 0.0514 0.0743 -0.0754
