#------------------------------------------------------------------------------
#$Date: 2024-10-06 10:10:37 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295194 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/23/1572335.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_1572335
loop_
_publ_author_name
'Scholes, Abbie M.'
'Kershaw Cook, Laurence J.'
'Szczypiński, Filip T'
'Luzyanin, Konstantin V.'
'Egleston, Benjamin D.'
'Greenaway, Rebecca L.'
'Slater, Anna G.'
_publ_section_title
;
 Dynamic and solid-state behaviour of bromoisotrianglimine.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              14254
_journal_page_last               14263
_journal_paper_doi               10.1039/d4sc04207g
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C42 H45 Br3 N6, 1.5(H2 O), 0.786(O)'
_chemical_formula_sum            'C42 H48 Br3 N6 O2.29'
_chemical_formula_weight         913.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-01-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-12-07 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.547(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5590(4)
_cell_length_b                   23.3781(6)
_cell_length_c                   16.2798(5)
_cell_measurement_reflns_used    16908
_cell_measurement_temperature    100.01(13)
_cell_measurement_theta_max      25.0480
_cell_measurement_theta_min      1.5380
_cell_volume                     4665.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_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    -34.00  -8.00   1.00   50.00    --   -8.70  66.00 163.00   26
  2  ω    -70.00  14.00   1.00   50.00    --   -8.70 -66.00  28.00   84
  3  ω    -45.00  17.00   1.00   50.00    --   -8.70 -38.00  30.00   62
  4  ω    -80.00  19.00   1.00   50.00    --   -8.70 -57.00-120.00   99
  5  ω    -46.00  58.00   1.00   50.00    --   -8.70  68.00-150.00  104
  6  ω     18.00  68.00   1.00   50.00    --   -8.70  66.00 163.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0144307000
_diffrn_orient_matrix_UB_12      0.0022981000
_diffrn_orient_matrix_UB_13      0.0444928000
_diffrn_orient_matrix_UB_21      0.0376460000
_diffrn_orient_matrix_UB_22      -0.0228001000
_diffrn_orient_matrix_UB_23      0.0015958000
_diffrn_orient_matrix_UB_31      0.0415063000
_diffrn_orient_matrix_UB_32      0.0198682000
_diffrn_orient_matrix_UB_33      -0.0033829000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0559
_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       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55071
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.422
_diffrn_reflns_theta_min         1.549
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku 007HF (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.632
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       needle
_exptl_crystal_F_000             1861
_exptl_crystal_preparation
'Slow vapour diffusion of n-heptane into a THF solution.'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.661
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 5735 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         18957
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0795P)²+2.6105P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                14728
_reflns_number_total             18957
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc04207g2.cif
_cod_data_source_block           33-rr_h2o_w0154_sq_ams502_thfhept_100k_1
_cod_depositor_comments
'Adding full bibliography for 1572326--1572335.cif.'
_cod_database_code               1572335
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H45 N6 Br3'
_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   0.880
_shelx_estimated_absorpt_t_min   0.663
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O103(H10C,H10D), O104(H10E,H10F), O106(H10G,H10H)
2.b Ternary CH refined with riding coordinates:
 C79(H79), C10(H10), C28(H28), C78(H78), C11(H11), C44(H44), C95(H95),
 C96(H96), C45(H45), C27(H27), C62(H62), C61(H61)
2.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C97(H97A,H97B), C15(H15A,H15B), C83(H83A,
 H83B), C46(H46A,H46B), C13(H13A,H13B), C100(H10A,H10B), C99(H99A,H99B),
 C98(H98A,H98B), C29(H29A,H29B), C47(H47A,H47B), C48(H48A,H48B), C63(H63A,H63B),
  C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C82(H82A,H82B), C80(H80A,
 H80B), C49(H49A,H49B), C66(H66A,H66B), C64(H64A,H64B), C65(H65A,H65B),
 C81(H81A,H81B)
2.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C93(H93), C42(H42), C39(H39), C17(H17), C3(H3), C51(H51),
 C92(H92), C90(H90), C76(H76), C71(H71), C5(H5), C24(H24), C88(H88), C85(H85),
 C34(H34), C56(H56), C22(H22), C73(H73), C20(H20), C59(H59), C68(H68), C75(H75),
  C41(H41), C37(H37), C25(H25), C102(H102), C58(H58), C54(H54)
;
_olex2_date_sample_data_collection 2022-06-08
_olex2_submission_original_sample_id 'AMS502 THF nHept 100 K'
_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 1.132
_oxdiff_exptl_absorpt_empirical_full_min 0.885
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
Br1 Br -0.00139(6) 0.54241(3) 0.30396(5) 0.03448(18) Uani 1 1 d . . . . .
Br18 Br 0.43188(6) 0.37486(3) 0.73266(6) 0.0455(2) Uani 1 1 d . . . . .
Br69 Br -0.08238(7) 0.44717(4) 0.64983(6) 0.0523(2) Uani 1 1 d . . . . .
Br86 Br 0.29474(8) 0.12863(7) 0.79136(7) 0.0808(4) Uani 1 1 d . . . . .
Br35 Br 0.04553(14) 0.72678(5) 0.79859(8) 0.0953(5) Uani 1 1 d . . . . .
Br52 Br 0.34439(15) 0.33629(7) 1.04812(12) 0.1256(8) Uani 1 1 d . . . . .
N9 N -0.1073(5) 0.2987(3) 0.4551(4) 0.0371(15) Uani 1 1 d . . . . .
N16 N 0.0594(5) 0.2556(2) 0.5932(4) 0.0312(14) Uani 1 1 d . . . . .
N43 N -0.3794(6) 0.5971(3) 0.5866(4) 0.0412(16) Uani 1 1 d . . . . .
N50 N -0.3734(5) 0.5367(3) 0.4318(4) 0.0339(14) Uani 1 1 d . . . . .
N94 N 0.7174(5) 0.1948(3) 0.8019(4) 0.0386(15) Uani 1 1 d . . . . .
N77 N 0.2235(5) 0.3913(3) 0.4611(4) 0.0405(16) Uani 1 1 d . . . . .
N33 N -0.0623(6) 0.5218(3) 0.9334(4) 0.0442(17) Uani 1 1 d . . . . .
C8 C -0.0672(6) 0.3359(3) 0.4157(5) 0.0325(16) Uani 1 1 d . . . . .
H8 H -0.007279 0.325368 0.391972 0.039 Uiso 1 1 calc R U . . .
N84 N 0.3591(5) 0.2882(3) 0.4807(5) 0.0485(18) Uani 1 1 d . . . . .
C2 C -0.0835(6) 0.4906(3) 0.3564(5) 0.0302(16) Uani 1 1 d . . . . .
C7 C -0.1755(6) 0.5097(3) 0.3812(5) 0.0292(15) Uani 1 1 d . . . . .
H7 H -0.198685 0.548379 0.372510 0.035 Uiso 1 1 calc R U . . .
C6 C -0.2341(6) 0.4704(3) 0.4196(5) 0.0331(16) Uani 1 1 d . . . . .
N101 N 0.7914(6) 0.2777(3) 0.9295(4) 0.0424(16) Uani 1 1 d . . . . .
C4 C -0.1075(6) 0.3953(3) 0.4037(4) 0.0293(15) Uani 1 1 d . . . . .
N26 N 0.0308(6) 0.4079(3) 0.9227(4) 0.0435(16) Uani 1 1 d . . . . .
N67 N 0.3994(7) 0.5562(3) 0.7716(5) 0.0503(18) Uani 1 1 d . . . . .
C79 C 0.2921(7) 0.3064(4) 0.4020(6) 0.046(2) Uani 1 1 d . . . . .
H79 H 0.217101 0.290368 0.396338 0.056 Uiso 1 1 calc R U . . .
N60 N 0.5410(8) 0.5204(3) 0.9264(5) 0.061(2) Uani 1 1 d . . . . .
C93 C 0.6619(6) 0.2239(4) 0.7423(5) 0.0396(18) Uani 1 1 d . . . . .
H93 H 0.697652 0.251914 0.715619 0.048 Uiso 1 1 calc R U . . .
C10 C -0.0606(6) 0.2406(3) 0.4552(5) 0.0326(16) Uani 1 1 d . . . . .
H10 H 0.003238 0.241589 0.427691 0.039 Uiso 1 1 calc R U . . .
C12 C 0.0255(6) 0.1582(3) 0.5403(5) 0.0347(17) Uani 1 1 d . . . . .
H12A H 0.089432 0.161038 0.514080 0.042 Uiso 1 1 calc R U . . .
H12B H 0.050910 0.143123 0.598047 0.042 Uiso 1 1 calc R U . . .
C91 C 0.3786(6) 0.2332(3) 0.6095(5) 0.0339(16) Uani 1 1 d . . . . .
C42 C -0.2939(8) 0.6266(3) 0.5997(6) 0.045(2) Uani 1 1 d . . . . .
H42 H -0.284061 0.652353 0.556836 0.054 Uiso 1 1 calc R U . . .
C23 C 0.1137(6) 0.3199(3) 0.7113(5) 0.0335(16) Uani 1 1 d . . . . .
C28 C -0.0794(7) 0.4727(4) 0.9841(5) 0.0426(19) Uani 1 1 d . . . . .
H28 H -0.143928 0.450934 0.952451 0.051 Uiso 1 1 calc R U . . .
C78 C 0.2854(6) 0.3716(4) 0.3981(5) 0.0395(18) Uani 1 1 d . . . . .
H78 H 0.360436 0.388342 0.411192 0.047 Uiso 1 1 calc R U . . .
C14 C -0.1065(9) 0.1402(4) 0.4038(7) 0.059(3) Uani 1 1 d . . . . .
H14A H -0.167419 0.115056 0.376457 0.071 Uiso 1 1 calc R U . . .
H14B H -0.050684 0.139221 0.369283 0.071 Uiso 1 1 calc R U . . .
C39 C -0.2022(7) 0.5770(3) 0.7319(6) 0.043(2) Uani 1 1 d . . . . .
H39 H -0.253162 0.546632 0.718593 0.051 Uiso 1 1 calc R U . . .
C11 C -0.0241(6) 0.2185(3) 0.5446(5) 0.0325(16) Uani 1 1 d . . . . .
H11 H -0.087950 0.216251 0.572040 0.039 Uiso 1 1 calc R U . . .
C17 C 0.0358(6) 0.2817(3) 0.6552(5) 0.0341(17) Uani 1 1 d . . . . .
H17 H -0.034894 0.276537 0.666156 0.041 Uiso 1 1 calc R U . . .
C3 C -0.0486(6) 0.4344(3) 0.3668(4) 0.0288(15) Uani 1 1 d . . . . .
H3 H 0.015089 0.422603 0.348957 0.035 Uiso 1 1 calc R U . . .
C51 C -0.3336(6) 0.4881(3) 0.4455(5) 0.0342(17) Uani 1 1 d . . . . .
H51 H -0.369275 0.461306 0.474140 0.041 Uiso 1 1 calc R U . . .
C44 C -0.4620(7) 0.6049(3) 0.5079(6) 0.042(2) Uani 1 1 d . . . . .
H44 H -0.435723 0.635105 0.473645 0.050 Uiso 1 1 calc R U . . .
C92 C 0.3207(6) 0.2000(4) 0.6546(6) 0.045(2) Uani 1 1 d . . . . .
H92 H 0.244510 0.194211 0.634843 0.055 Uiso 1 1 calc R U . . .
C89 C 0.5436(6) 0.2157(3) 0.7130(5) 0.0388(18) Uani 1 1 d . . . . .
C95 C 0.8330(6) 0.2089(3) 0.8288(5) 0.0383(18) Uani 1 1 d . . . . .
H95 H 0.850895 0.241687 0.794774 0.046 Uiso 1 1 calc R U . . .
C90 C 0.4895(6) 0.2408(3) 0.6380(5) 0.0385(18) Uani 1 1 d . . . . .
H90 H 0.529144 0.263244 0.606307 0.046 Uiso 1 1 calc R U . . .
C76 C 0.2687(7) 0.4275(3) 0.5146(5) 0.0385(18) Uani 1 1 d . . . . .
H76 H 0.341264 0.438892 0.514344 0.046 Uiso 1 1 calc R U . . .
C38 C -0.2082(8) 0.6241(4) 0.6769(5) 0.046(2) Uani 1 1 d . . . . .
C97 C 0.9743(6) 0.2378(4) 0.9551(6) 0.045(2) Uani 1 1 d . . . . .
H97A H 0.988036 0.246918 1.015873 0.054 Uiso 1 1 calc R U . . .
H97B H 0.996285 0.271258 0.925425 0.054 Uiso 1 1 calc R U . . .
C71 C 0.1078(7) 0.4404(3) 0.5826(5) 0.0406(18) Uani 1 1 d . . . . .
H71 H 0.065219 0.415004 0.543230 0.049 Uiso 1 1 calc R U . . .
C15 C -0.1488(7) 0.2009(3) 0.4053(6) 0.047(2) Uani 1 1 d . . . . .
H15A H -0.213111 0.201145 0.431317 0.056 Uiso 1 1 calc R U . . .
H15B H -0.172112 0.215237 0.346959 0.056 Uiso 1 1 calc R U . . .
C5 C -0.2013(6) 0.4143(3) 0.4306(5) 0.0307(16) Uani 1 1 d . . . . .
H5 H -0.241835 0.388116 0.456422 0.037 Uiso 1 1 calc R U . . .
C24 C 0.2173(6) 0.3301(3) 0.6961(5) 0.0360(17) Uani 1 1 d . . . . .
H24 H 0.237511 0.313997 0.648173 0.043 Uiso 1 1 calc R U . . .
C19 C 0.2896(6) 0.3636(3) 0.7510(6) 0.0389(18) Uani 1 1 d . . . . .
C70 C 0.0650(7) 0.4642(3) 0.6435(5) 0.0400(19) Uani 1 1 d . . . . .
C88 C 0.4850(6) 0.1822(4) 0.7599(5) 0.0427(19) Uani 1 1 d . . . . .
H88 H 0.521038 0.165036 0.811312 0.051 Uiso 1 1 calc R U . . .
C83 C 0.2230(7) 0.3929(4) 0.3129(5) 0.046(2) Uani 1 1 d . . . . .
H83A H 0.224410 0.435196 0.311827 0.056 Uiso 1 1 calc R U . . .
H83B H 0.145960 0.380449 0.303655 0.056 Uiso 1 1 calc R U . . .
C85 C 0.3184(6) 0.2578(3) 0.5289(5) 0.0368(18) Uani 1 1 d . . . . .
H85 H 0.242607 0.249783 0.512600 0.044 Uiso 1 1 calc R U . . .
C46 C -0.5670(6) 0.5550(4) 0.3805(6) 0.046(2) Uani 1 1 d . . . . .
H46A H -0.545294 0.582352 0.340680 0.056 Uiso 1 1 calc R U . . .
H46B H -0.578837 0.517281 0.352382 0.056 Uiso 1 1 calc R U . . .
C34 C -0.1241(7) 0.5256(3) 0.8616(6) 0.045(2) Uani 1 1 d . . . . .
H34 H -0.174029 0.495282 0.843084 0.054 Uiso 1 1 calc R U . . .
C96 C 0.8549(6) 0.2261(3) 0.9226(5) 0.0379(17) Uani 1 1 d . . . . .
H96 H 0.831236 0.194523 0.956045 0.045 Uiso 1 1 calc R U . . .
C72 C 0.2152(6) 0.4532(3) 0.5774(5) 0.0368(17) Uani 1 1 d . . . . .
C13 C -0.0578(7) 0.1169(3) 0.4893(5) 0.0427(19) Uani 1 1 d . . . . .
H13A H -0.021699 0.079950 0.483450 0.051 Uiso 1 1 calc R U . . .
H13B H -0.116528 0.109764 0.519938 0.051 Uiso 1 1 calc R U . . .
C56 C 0.6486(7) 0.3757(4) 0.9413(6) 0.051(2) Uani 1 1 d . . . . .
H56 H 0.709735 0.383111 0.917269 0.062 Uiso 1 1 calc R U . . .
C21 C 0.1551(7) 0.3808(3) 0.8339(5) 0.0406(18) Uani 1 1 d . . . . .
C40 C -0.1230(8) 0.5750(3) 0.8044(5) 0.044(2) Uani 1 1 d . . . . .
C22 C 0.0844(6) 0.3451(3) 0.7790(5) 0.0370(17) Uani 1 1 d . . . . .
H22 H 0.013675 0.337973 0.788813 0.044 Uiso 1 1 calc R U . . .
C73 C 0.2759(7) 0.4892(3) 0.6368(5) 0.044(2) Uani 1 1 d . . . . .
H73 H 0.348692 0.498252 0.633706 0.052 Uiso 1 1 calc R U . . .
C20 C 0.2598(7) 0.3895(3) 0.8184(5) 0.0403(19) Uani 1 1 d . . . . .
H20 H 0.310279 0.413406 0.854788 0.048 Uiso 1 1 calc R U . . .
C45 C -0.4751(6) 0.5501(3) 0.4588(5) 0.0372(17) Uani 1 1 d . . . . .
H45 H -0.492109 0.518406 0.495162 0.045 Uiso 1 1 calc R U . . .
C100 C 0.9012(7) 0.1569(4) 0.8163(6) 0.045(2) Uani 1 1 d . . . . .
H10A H 0.888668 0.147721 0.755614 0.054 Uiso 1 1 calc R U . . .
H10B H 0.878496 0.123517 0.845701 0.054 Uiso 1 1 calc R U . . .
C59 C 0.5894(8) 0.4758(4) 0.9125(7) 0.053(2) Uani 1 1 d . . . . .
H59 H 0.637900 0.478880 0.875316 0.064 Uiso 1 1 calc R U . . .
C99 C 1.0226(7) 0.1687(4) 0.8507(6) 0.045(2) Uani 1 1 d . . . . .
H99A H 1.065378 0.134073 0.844247 0.053 Uiso 1 1 calc R U . . .
H99B H 1.046811 0.199997 0.818021 0.053 Uiso 1 1 calc R U . . .
C98 C 1.0432(7) 0.1851(4) 0.9414(6) 0.047(2) Uani 1 1 d . . . . .
H98A H 1.121546 0.194010 0.961773 0.056 Uiso 1 1 calc R U . . .
H98B H 1.024978 0.152521 0.974598 0.056 Uiso 1 1 calc R U . . .
C29 C -0.1073(8) 0.4957(4) 1.0666(5) 0.045(2) Uani 1 1 d . . . . .
H29A H -0.047028 0.520145 1.096828 0.055 Uiso 1 1 calc R U . . .
H29B H -0.174386 0.519153 1.052942 0.055 Uiso 1 1 calc R U . . .
C87 C 0.3761(7) 0.1748(4) 0.7303(6) 0.051(2) Uani 1 1 d . . . . .
C47 C -0.6724(7) 0.5749(4) 0.4015(7) 0.061(3) Uani 1 1 d . . . . .
H47A H -0.728136 0.580325 0.348874 0.073 Uiso 1 1 calc R U . . .
H47B H -0.699236 0.545347 0.435516 0.073 Uiso 1 1 calc R U . . .
C48 C -0.6561(8) 0.6299(4) 0.4495(8) 0.065(3) Uani 1 1 d . . . . .
H48A H -0.635674 0.660339 0.413466 0.078 Uiso 1 1 calc R U . . .
H48B H -0.725436 0.641279 0.464471 0.078 Uiso 1 1 calc R U . . .
C27 C 0.0169(7) 0.4335(4) 1.0000(6) 0.047(2) Uani 1 1 d . . . . .
H27 H 0.083861 0.455838 1.025440 0.056 Uiso 1 1 calc R U . . .
C68 C 0.2974(8) 0.5489(3) 0.7657(5) 0.048(2) Uani 1 1 d . . . . .
H68 H 0.262948 0.567852 0.804545 0.057 Uiso 1 1 calc R U . . .
C75 C 0.1246(8) 0.5007(3) 0.7045(5) 0.045(2) Uani 1 1 d . . . . .
H75 H 0.092480 0.516975 0.746784 0.055 Uiso 1 1 calc R U . . .
C62 C 0.4562(8) 0.5974(3) 0.8338(6) 0.053(2) Uani 1 1 d . . . . .
H62 H 0.409400 0.606772 0.874442 0.063 Uiso 1 1 calc R U . . .
C55 C 0.5780(9) 0.4205(4) 0.9477(7) 0.063(3) Uani 1 1 d . . . . .
C63 C 0.4762(10) 0.6518(4) 0.7868(7) 0.068(3) Uani 1 1 d . . . . .
H63A H 0.405636 0.668106 0.756952 0.082 Uiso 1 1 calc R U . . .
H63B H 0.519575 0.642429 0.744554 0.082 Uiso 1 1 calc R U . . .
C30 C -0.1242(8) 0.4454(4) 1.1227(5) 0.050(2) Uani 1 1 d . . . . .
H30A H -0.139630 0.460084 1.175931 0.060 Uiso 1 1 calc R U . . .
H30B H -0.187915 0.422571 1.093907 0.060 Uiso 1 1 calc R U . . .
C74 C 0.2323(8) 0.5127(3) 0.7017(6) 0.047(2) Uani 1 1 d . . . . .
C61 C 0.5616(9) 0.5723(4) 0.8804(7) 0.061(3) Uani 1 1 d . . . . .
H61 H 0.607100 0.561893 0.839295 0.074 Uiso 1 1 calc R U . . .
C41 C -0.0468(9) 0.6198(4) 0.8277(6) 0.055(2) Uani 1 1 d . . . . .
H41 H 0.006787 0.619333 0.878833 0.066 Uiso 1 1 calc R U . . .
C37 C -0.1360(9) 0.6679(4) 0.6975(6) 0.056(2) Uani 1 1 d . . . . .
H37 H -0.140419 0.700560 0.662135 0.067 Uiso 1 1 calc R U . . .
C31 C -0.0233(8) 0.4073(4) 1.1421(6) 0.052(2) Uani 1 1 d . . . . .
H31A H -0.036118 0.374809 1.177719 0.063 Uiso 1 1 calc R U . . .
H31B H 0.039603 0.429474 1.173508 0.063 Uiso 1 1 calc R U . . .
C25 C 0.1262(8) 0.4086(4) 0.9059(6) 0.047(2) Uani 1 1 d . . . . .
H25 H 0.182117 0.428828 0.943401 0.056 Uiso 1 1 calc R U . . .
C32 C 0.0024(8) 0.3846(4) 1.0602(5) 0.050(2) Uani 1 1 d . . . . .
H32A H -0.057674 0.359294 1.031832 0.060 Uiso 1 1 calc R U . . .
H32B H 0.070026 0.361527 1.073616 0.060 Uiso 1 1 calc R U . . .
C82 C 0.2749(9) 0.3689(5) 0.2412(7) 0.067(3) Uani 1 1 d . . . . .
H82A H 0.231956 0.381626 0.185863 0.081 Uiso 1 1 calc R U . . .
H82B H 0.350235 0.383525 0.247814 0.081 Uiso 1 1 calc R U . . .
C36 C -0.0561(10) 0.6643(4) 0.7707(6) 0.063(3) Uani 1 1 d . . . . .
C80 C 0.3414(11) 0.2836(5) 0.3305(7) 0.076(4) Uani 1 1 d . . . . .
H80A H 0.417536 0.297249 0.338045 0.091 Uiso 1 1 calc R U . . .
H80B H 0.342817 0.241245 0.332446 0.091 Uiso 1 1 calc R U . . .
C49 C -0.5698(8) 0.6245(4) 0.5272(7) 0.060(3) Uani 1 1 d . . . . .
H49A H -0.593349 0.596664 0.565500 0.072 Uiso 1 1 calc R U . . .
H49B H -0.559164 0.661960 0.556304 0.072 Uiso 1 1 calc R U . . .
C102 C 0.7137(9) 0.2746(4) 0.9638(8) 0.071(3) Uani 1 1 d . . . . .
H102 H 0.703292 0.239428 0.990119 0.085 Uiso 1 1 calc R U . . .
C66 C 0.6246(10) 0.6156(4) 0.9443(9) 0.083(4) Uani 1 1 d . . . . .
H66A H 0.694334 0.598680 0.974616 0.100 Uiso 1 1 calc R U . . .
H66B H 0.581000 0.625823 0.986052 0.100 Uiso 1 1 calc R U . . .
C64 C 0.5377(12) 0.6954(5) 0.8499(9) 0.094(4) Uani 1 1 d . . . . .
H64A H 0.493373 0.705583 0.891155 0.113 Uiso 1 1 calc R U . . .
H64B H 0.550930 0.730687 0.819967 0.113 Uiso 1 1 calc R U . . .
C57 C 0.6339(11) 0.3217(5) 0.9679(8) 0.084(4) Uani 1 1 d . . . . .
C65 C 0.6469(11) 0.6696(5) 0.8958(10) 0.097(5) Uani 1 1 d . . . . .
H65A H 0.688067 0.697993 0.935489 0.116 Uiso 1 1 calc R U . . .
H65B H 0.691209 0.659397 0.854536 0.116 Uiso 1 1 calc R U . . .
C58 C 0.5435(10) 0.3106(5) 0.9974(7) 0.072(3) Uani 1 1 d . . . . .
H58 H 0.531272 0.272685 1.014351 0.087 Uiso 1 1 calc R U . . .
C54 C 0.4883(10) 0.4084(5) 0.9813(7) 0.069(3) Uani 1 1 d . . . . .
H54 H 0.440340 0.438343 0.989024 0.083 Uiso 1 1 calc R U . . .
C53 C 0.4676(11) 0.3529(6) 1.0038(8) 0.082(4) Uani 1 1 d . . . . .
C81 C 0.2762(13) 0.3030(5) 0.2454(8) 0.092(4) Uani 1 1 d . . . . .
H81A H 0.200627 0.288428 0.236720 0.111 Uiso 1 1 calc R U . . .
H81B H 0.309384 0.287451 0.200207 0.111 Uiso 1 1 calc R U . . .
O103 O 0.8296(5) 0.3678(3) 0.8187(4) 0.0505(14) Uani 1 1 d G . . . .
H10C H 0.887444 0.382504 0.847891 0.076 Uiso 1 1 d G U . . .
H10D H 0.810809 0.342907 0.850875 0.076 Uiso 1 1 d G U . . .
O104 O 0.5595(6) 0.5044(3) 0.6849(5) 0.0654(19) Uani 1 1 d G . . . .
H10E H 0.517294 0.485285 0.646894 0.098 Uiso 1 1 d G U . . .
H10F H 0.568750 0.535916 0.661354 0.098 Uiso 1 1 d G U . . .
O106 O 0.6734(10) 0.4024(4) 0.6794(6) 0.104(3) Uani 1 1 d G . . . .
H10G H 0.619511 0.379895 0.676051 0.156 Uiso 1 1 d G U . . .
H10H H 0.659424 0.420958 0.633370 0.156 Uiso 1 1 d G U . . .
O107 O 0.7391(8) 0.2962(7) 0.5702(8) 0.131(7) Uani 0.89(3) 1 d . . . . .
O105 O 0.5651(8) 0.3606(4) 0.5241(8) 0.071(5) Uani 0.68(3) 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 0.0033 0.0016 '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 -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C8 N9 C10 115.9(6) . . ?
C17 N16 C11 116.9(6) . . ?
C42 N43 C44 119.6(7) . . ?
C51 N50 C45 118.9(6) . . ?
C93 N94 C95 117.1(7) . . ?
C76 N77 C78 117.4(7) . . ?
C34 N33 C28 116.3(7) . . ?
N9 C8 H8 118.0 . . ?
N9 C8 C4 123.9(7) . . ?
C4 C8 H8 118.0 . . ?
C85 N84 C79 119.3(7) . . ?
C7 C2 Br1 119.6(5) . . ?
C7 C2 C3 122.4(7) . . ?
C3 C2 Br1 118.0(5) . . ?
C2 C7 H7 121.0 . . ?
C2 C7 C6 118.1(6) . . ?
C6 C7 H7 121.0 . . ?
C7 C6 C51 120.3(6) . . ?
C5 C6 C7 120.7(7) . . ?
C5 C6 C51 118.9(7) . . ?
C102 N101 C96 119.2(8) . . ?
C3 C4 C8 118.4(6) . . ?
C3 C4 C5 118.9(6) . . ?
C5 C4 C8 122.6(6) . . ?
C25 N26 C27 118.5(7) . . ?
C68 N67 C62 118.1(8) . . ?
N84 C79 H79 109.2 . . ?
N84 C79 C78 110.5(8) . . ?
N84 C79 C80 108.6(7) . . ?
C78 C79 H79 109.2 . . ?
C78 C79 C80 110.2(7) . . ?
C80 C79 H79 109.2 . . ?
C59 N60 C61 116.5(9) . . ?
N94 C93 H93 119.1 . . ?
N94 C93 C89 121.9(8) . . ?
C89 C93 H93 119.1 . . ?
N9 C10 H10 109.5 . . ?
N9 C10 C11 110.5(6) . . ?
N9 C10 C15 108.3(6) . . ?
C11 C10 H10 109.5 . . ?
C11 C10 C15 109.6(6) . . ?
C15 C10 H10 109.5 . . ?
H12A C12 H12B 108.0 . . ?
C11 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
C13 C12 H12A 109.3 . . ?
C13 C12 H12B 109.3 . . ?
C13 C12 C11 111.4(6) . . ?
C92 C91 C90 120.2(7) . . ?
C92 C91 C85 117.6(7) . . ?
C90 C91 C85 122.1(7) . . ?
N43 C42 H42 117.8 . . ?
N43 C42 C38 124.3(8) . . ?
C38 C42 H42 117.8 . . ?
C24 C23 C17 120.6(7) . . ?
C22 C23 C17 119.9(7) . . ?
C22 C23 C24 119.6(7) . . ?
N33 C28 H28 108.2 . . ?
N33 C28 C29 107.8(6) . . ?
N33 C28 C27 111.6(7) . . ?
C29 C28 H28 108.2 . . ?
C27 C28 H28 108.2 . . ?
C27 C28 C29 112.8(7) . . ?
N77 C78 C79 108.2(6) . . ?
N77 C78 H78 109.9 . . ?
N77 C78 C83 106.6(6) . . ?
C79 C78 H78 109.9 . . ?
C83 C78 C79 112.2(7) . . ?
C83 C78 H78 109.9 . . ?
H14A C14 H14B 107.7 . . ?
C15 C14 H14A 108.9 . . ?
C15 C14 H14B 108.9 . . ?
C13 C14 H14A 108.9 . . ?
C13 C14 H14B 108.9 . . ?
C13 C14 C15 113.5(8) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C40 C39 C38 120.2(8) . . ?
N16 C11 C10 110.5(6) . . ?
N16 C11 C12 108.5(6) . . ?
N16 C11 H11 110.0 . . ?
C10 C11 C12 107.8(6) . . ?
C10 C11 H11 110.0 . . ?
C12 C11 H11 110.0 . . ?
N16 C17 C23 122.8(7) . . ?
N16 C17 H17 118.6 . . ?
C23 C17 H17 118.6 . . ?
C2 C3 C4 119.6(6) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
N50 C51 C6 122.9(7) . . ?
N50 C51 H51 118.5 . . ?
C6 C51 H51 118.5 . . ?
N43 C44 H44 108.5 . . ?
N43 C44 C45 109.4(6) . . ?
N43 C44 C49 110.3(7) . . ?
C45 C44 H44 108.5 . . ?
C45 C44 C49 111.6(7) . . ?
C49 C44 H44 108.5 . . ?
C91 C92 H92 120.5 . . ?
C91 C92 C87 118.9(7) . . ?
C87 C92 H92 120.5 . . ?
C90 C89 C93 119.7(8) . . ?
C90 C89 C88 119.8(7) . . ?
C88 C89 C93 120.5(8) . . ?
N94 C95 H95 109.6 . . ?
N94 C95 C96 107.9(6) . . ?
N94 C95 C100 109.3(6) . . ?
C96 C95 H95 109.6 . . ?
C100 C95 H95 109.6 . . ?
C100 C95 C96 110.8(7) . . ?
C91 C90 C89 120.4(8) . . ?
C91 C90 H90 119.8 . . ?
C89 C90 H90 119.8 . . ?
N77 C76 H76 118.3 . . ?
N77 C76 C72 123.4(7) . . ?
C72 C76 H76 118.3 . . ?
C39 C38 C42 120.3(8) . . ?
C37 C38 C42 120.4(8) . . ?
C37 C38 C39 119.3(9) . . ?
H97A C97 H97B 108.1 . . ?
C96 C97 H97A 109.5 . . ?
C96 C97 H97B 109.5 . . ?
C96 C97 C98 110.5(7) . . ?
C98 C97 H97A 109.5 . . ?
C98 C97 H97B 109.5 . . ?
C70 C71 H71 120.0 . . ?
C70 C71 C72 120.0(8) . . ?
C72 C71 H71 120.0 . . ?
C10 C15 H15A 109.4 . . ?
C10 C15 H15B 109.4 . . ?
C14 C15 C10 111.0(7) . . ?
C14 C15 H15A 109.4 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C6 C5 C4 120.3(7) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C23 C24 H24 120.2 . . ?
C19 C24 C23 119.5(7) . . ?
C19 C24 H24 120.2 . . ?
C24 C19 Br18 119.4(6) . . ?
C24 C19 C20 120.9(7) . . ?
C20 C19 Br18 119.7(6) . . ?
C71 C70 Br69 119.8(6) . . ?
C71 C70 C75 122.5(8) . . ?
C75 C70 Br69 117.6(7) . . ?
C89 C88 H88 120.5 . . ?
C87 C88 C89 118.9(8) . . ?
C87 C88 H88 120.5 . . ?
C78 C83 H83A 109.6 . . ?
C78 C83 H83B 109.6 . . ?
C78 C83 C82 110.4(7) . . ?
H83A C83 H83B 108.1 . . ?
C82 C83 H83A 109.6 . . ?
C82 C83 H83B 109.6 . . ?
N84 C85 C91 125.4(7) . . ?
N84 C85 H85 117.3 . . ?
C91 C85 H85 117.3 . . ?
H46A C46 H46B 107.9 . . ?
C45 C46 H46A 109.2 . . ?
C45 C46 H46B 109.2 . . ?
C47 C46 H46A 109.2 . . ?
C47 C46 H46B 109.2 . . ?
C47 C46 C45 112.0(8) . . ?
N33 C34 H34 118.4 . . ?
N33 C34 C40 123.2(8) . . ?
C40 C34 H34 118.4 . . ?
N101 C96 C95 107.9(6) . . ?
N101 C96 C97 110.0(7) . . ?
N101 C96 H96 109.6 . . ?
C95 C96 H96 109.6 . . ?
C97 C96 C95 110.2(6) . . ?
C97 C96 H96 109.6 . . ?
C71 C72 C76 123.3(7) . . ?
C73 C72 C76 118.0(7) . . ?
C73 C72 C71 118.6(8) . . ?
C12 C13 H13A 109.3 . . ?
C12 C13 H13B 109.3 . . ?
C14 C13 C12 111.6(7) . . ?
C14 C13 H13A 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 108.0 . . ?
C55 C56 H56 118.6 . . ?
C57 C56 H56 118.6 . . ?
C57 C56 C55 122.7(9) . . ?
C22 C21 C20 117.5(7) . . ?
C22 C21 C25 123.3(7) . . ?
C20 C21 C25 119.1(7) . . ?
C39 C40 C34 117.6(7) . . ?
C39 C40 C41 122.0(8) . . ?
C41 C40 C34 120.3(8) . . ?
C23 C22 C21 121.9(7) . . ?
C23 C22 H22 119.0 . . ?
C21 C22 H22 119.0 . . ?
C72 C73 H73 119.4 . . ?
C72 C73 C74 121.3(8) . . ?
C74 C73 H73 119.4 . . ?
C19 C20 C21 120.5(8) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
N50 C45 C44 109.8(6) . . ?
N50 C45 C46 108.3(6) . . ?
N50 C45 H45 109.3 . . ?
C44 C45 C46 110.9(6) . . ?
C44 C45 H45 109.3 . . ?
C46 C45 H45 109.3 . . ?
C95 C100 H10A 109.5 . . ?
C95 C100 H10B 109.5 . . ?
C95 C100 C99 110.6(7) . . ?
H10A C100 H10B 108.1 . . ?
C99 C100 H10A 109.5 . . ?
C99 C100 H10B 109.5 . . ?
N60 C59 H59 117.2 . . ?
N60 C59 C55 125.7(10) . . ?
C55 C59 H59 117.2 . . ?
C100 C99 H99A 109.5 . . ?
C100 C99 H99B 109.5 . . ?
H99A C99 H99B 108.1 . . ?
C98 C99 C100 110.6(7) . . ?
C98 C99 H99A 109.5 . . ?
C98 C99 H99B 109.5 . . ?
C97 C98 H98A 109.3 . . ?
C97 C98 H98B 109.3 . . ?
C99 C98 C97 111.4(7) . . ?
C99 C98 H98A 109.3 . . ?
C99 C98 H98B 109.3 . . ?
H98A C98 H98B 108.0 . . ?
C28 C29 H29A 109.7 . . ?
C28 C29 H29B 109.7 . . ?
H29A C29 H29B 108.2 . . ?
C30 C29 C28 109.6(7) . . ?
C30 C29 H29A 109.7 . . ?
C30 C29 H29B 109.7 . . ?
C92 C87 Br86 118.3(6) . . ?
C88 C87 Br86 120.0(7) . . ?
C88 C87 C92 121.7(8) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 108.0 . . ?
C48 C47 C46 110.9(8) . . ?
C48 C47 H47A 109.5 . . ?
C48 C47 H47B 109.5 . . ?
C47 C48 H48A 109.4 . . ?
C47 C48 H48B 109.4 . . ?
H48A C48 H48B 108.0 . . ?
C49 C48 C47 111.4(8) . . ?
C49 C48 H48A 109.4 . . ?
C49 C48 H48B 109.4 . . ?
N26 C27 C28 110.6(7) . . ?
N26 C27 H27 109.2 . . ?
N26 C27 C32 107.5(7) . . ?
C28 C27 H27 109.2 . . ?
C28 C27 C32 111.2(7) . . ?
C32 C27 H27 109.2 . . ?
N67 C68 H68 118.9 . . ?
N67 C68 C74 122.2(9) . . ?
C74 C68 H68 118.9 . . ?
C70 C75 H75 120.8 . . ?
C74 C75 C70 118.3(8) . . ?
C74 C75 H75 120.8 . . ?
N67 C62 H62 109.4 . . ?
N67 C62 C63 108.0(8) . . ?
N67 C62 C61 109.7(7) . . ?
C63 C62 H62 109.4 . . ?
C61 C62 H62 109.4 . . ?
C61 C62 C63 110.9(9) . . ?
C56 C55 C59 121.8(9) . . ?
C54 C55 C56 117.6(10) . . ?
C54 C55 C59 120.2(9) . . ?
C62 C63 H63A 109.8 . . ?
C62 C63 H63B 109.8 . . ?
C62 C63 C64 109.3(9) . . ?
H63A C63 H63B 108.3 . . ?
C64 C63 H63A 109.8 . . ?
C64 C63 H63B 109.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 108.1 . . ?
C31 C30 C29 110.8(8) . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C73 C74 C68 121.2(9) . . ?
C75 C74 C73 119.2(8) . . ?
C75 C74 C68 119.7(9) . . ?
N60 C61 C62 110.3(9) . . ?
N60 C61 H61 109.1 . . ?
N60 C61 C66 108.6(9) . . ?
C62 C61 H61 109.1 . . ?
C62 C61 C66 110.6(8) . . ?
C66 C61 H61 109.1 . . ?
C40 C41 H41 122.5 . . ?
C36 C41 C40 115.0(9) . . ?
C36 C41 H41 122.5 . . ?
C38 C37 H37 120.5 . . ?
C38 C37 C36 119.1(8) . . ?
C36 C37 H37 120.5 . . ?
C30 C31 H31A 109.6 . . ?
C30 C31 H31B 109.6 . . ?
C30 C31 C32 110.2(7) . . ?
H31A C31 H31B 108.1 . . ?
C32 C31 H31A 109.6 . . ?
C32 C31 H31B 109.6 . . ?
N26 C25 C21 125.0(8) . . ?
N26 C25 H25 117.5 . . ?
C21 C25 H25 117.5 . . ?
C27 C32 H32A 109.2 . . ?
C27 C32 H32B 109.2 . . ?
C31 C32 C27 111.8(7) . . ?
C31 C32 H32A 109.2 . . ?
C31 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
C83 C82 H82A 109.8 . . ?
C83 C82 H82B 109.8 . . ?
H82A C82 H82B 108.3 . . ?
C81 C82 C83 109.2(8) . . ?
C81 C82 H82A 109.8 . . ?
C81 C82 H82B 109.8 . . ?
C41 C36 Br35 117.2(8) . . ?
C37 C36 Br35 118.4(7) . . ?
C37 C36 C41 124.3(8) . . ?
C79 C80 H80A 109.4 . . ?
C79 C80 H80B 109.4 . . ?
H80A C80 H80B 108.0 . . ?
C81 C80 C79 111.3(8) . . ?
C81 C80 H80A 109.4 . . ?
C81 C80 H80B 109.4 . . ?
C44 C49 H49A 109.3 . . ?
C44 C49 H49B 109.3 . . ?
C48 C49 C44 111.5(8) . . ?
C48 C49 H49A 109.3 . . ?
C48 C49 H49B 109.3 . . ?
H49A C49 H49B 108.0 . . ?
N101 C102 H102 117.2 . . ?
N101 C102 C57 125.7(9) . . ?
C57 C102 H102 117.2 . . ?
C61 C66 H66A 110.0 . . ?
C61 C66 H66B 110.0 . . ?
C61 C66 C65 108.4(10) . . ?
H66A C66 H66B 108.4 . . ?
C65 C66 H66A 110.0 . . ?
C65 C66 H66B 110.0 . . ?
C63 C64 H64A 109.8 . . ?
C63 C64 H64B 109.8 . . ?
C63 C64 C65 109.4(11) . . ?
H64A C64 H64B 108.2 . . ?
C65 C64 H64A 109.8 . . ?
C65 C64 H64B 109.8 . . ?
C56 C57 C102 121.9(10) . . ?
C58 C57 C56 118.4(10) . . ?
C58 C57 C102 119.8(11) . . ?
C66 C65 H65A 109.9 . . ?
C66 C65 H65B 109.9 . . ?
C64 C65 C66 109.1(11) . . ?
C64 C65 H65A 109.9 . . ?
C64 C65 H65B 109.9 . . ?
H65A C65 H65B 108.3 . . ?
C57 C58 H58 119.0 . . ?
C57 C58 C53 122.1(11) . . ?
C53 C58 H58 119.0 . . ?
C55 C54 H54 119.7 . . ?
C55 C54 C53 120.7(10) . . ?
C53 C54 H54 119.7 . . ?
C58 C53 Br52 121.0(10) . . ?
C54 C53 Br52 120.6(9) . . ?
C54 C53 C58 118.3(11) . . ?
C82 C81 H81A 109.7 . . ?
C82 C81 H81B 109.7 . . ?
C80 C81 C82 109.8(12) . . ?
C80 C81 H81A 109.7 . . ?
C80 C81 H81B 109.7 . . ?
H81A C81 H81B 108.2 . . ?
H10C O103 H10D 104.5 . . ?
H10E O104 H10F 104.5 . . ?
H10G O106 H10H 104.5 . . ?
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 C2 1.908(7) . ?
Br18 C19 1.893(8) . ?
Br69 C70 1.918(9) . ?
Br86 C87 1.907(9) . ?
Br35 C36 1.928(9) . ?
Br52 C53 1.885(12) . ?
N9 C8 1.250(10) . ?
N9 C10 1.479(9) . ?
N16 C11 1.456(10) . ?
N16 C17 1.268(10) . ?
N43 C42 1.255(11) . ?
N43 C44 1.474(12) . ?
N50 C51 1.241(9) . ?
N50 C45 1.472(9) . ?
N94 C93 1.264(10) . ?
N94 C95 1.460(10) . ?
N77 C78 1.488(10) . ?
N77 C76 1.258(10) . ?
N33 C28 1.457(11) . ?
N33 C34 1.258(11) . ?
C8 H8 0.9500 . ?
C8 C4 1.475(10) . ?
N84 C79 1.436(12) . ?
N84 C85 1.248(11) . ?
C2 C7 1.378(10) . ?
C2 C3 1.384(10) . ?
C7 H7 0.9500 . ?
C7 C6 1.407(10) . ?
C6 C51 1.463(11) . ?
C6 C5 1.375(10) . ?
N101 C96 1.463(10) . ?
N101 C102 1.227(12) . ?
C4 C3 1.391(10) . ?
C4 C5 1.414(10) . ?
N26 C27 1.437(11) . ?
N26 C25 1.286(11) . ?
N67 C68 1.275(12) . ?
N67 C62 1.466(11) . ?
C79 H79 1.0000 . ?
C79 C78 1.526(12) . ?
C79 C80 1.529(12) . ?
N60 C59 1.252(12) . ?
N60 C61 1.479(13) . ?
C93 H93 0.9500 . ?
C93 C89 1.471(11) . ?
C10 H10 1.0000 . ?
C10 C11 1.518(11) . ?
C10 C15 1.535(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.549(9) . ?
C12 C13 1.529(11) . ?
C91 C92 1.380(12) . ?
C91 C90 1.381(11) . ?
C91 C85 1.481(11) . ?
C42 H42 0.9500 . ?
C42 C38 1.467(14) . ?
C23 C17 1.484(11) . ?
C23 C24 1.397(11) . ?
C23 C22 1.368(11) . ?
C28 H28 1.0000 . ?
C28 C29 1.555(11) . ?
C28 C27 1.494(13) . ?
C78 H78 1.0000 . ?
C78 C83 1.521(12) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.518(13) . ?
C14 C13 1.496(13) . ?
C39 H39 0.9500 . ?
C39 C38 1.409(11) . ?
C39 C40 1.368(13) . ?
C11 H11 1.0000 . ?
C17 H17 0.9500 . ?
C3 H3 0.9500 . ?
C51 H51 0.9500 . ?
C44 H44 1.0000 . ?
C44 C45 1.500(11) . ?
C44 C49 1.526(11) . ?
C92 H92 0.9500 . ?
C92 C87 1.406(13) . ?
C89 C90 1.390(12) . ?
C89 C88 1.408(12) . ?
C95 H95 1.0000 . ?
C95 C96 1.545(11) . ?
C95 C100 1.526(11) . ?
C90 H90 0.9500 . ?
C76 H76 0.9500 . ?
C76 C72 1.467(12) . ?
C38 C37 1.362(13) . ?
C97 H97A 0.9900 . ?
C97 H97B 0.9900 . ?
C97 C96 1.502(11) . ?
C97 C98 1.548(11) . ?
C71 H71 0.9500 . ?
C71 C70 1.346(12) . ?
C71 C72 1.401(11) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C5 H5 0.9500 . ?
C24 H24 0.9500 . ?
C24 C19 1.372(11) . ?
C19 C20 1.374(12) . ?
C70 C75 1.396(12) . ?
C88 H88 0.9500 . ?
C88 C87 1.359(12) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C83 C82 1.559(12) . ?
C85 H85 0.9500 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C45 1.527(12) . ?
C46 C47 1.510(12) . ?
C34 H34 0.9500 . ?
C34 C40 1.488(12) . ?
C96 H96 1.0000 . ?
C72 C73 1.381(11) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C56 H56 0.9500 . ?
C56 C55 1.391(13) . ?
C56 C57 1.360(15) . ?
C21 C22 1.394(11) . ?
C21 C20 1.406(12) . ?
C21 C25 1.453(12) . ?
C40 C41 1.413(12) . ?
C22 H22 0.9500 . ?
C73 H73 0.9500 . ?
C73 C74 1.404(13) . ?
C20 H20 0.9500 . ?
C45 H45 1.0000 . ?
C100 H10A 0.9900 . ?
C100 H10B 0.9900 . ?
C100 C99 1.530(12) . ?
C59 H59 0.9500 . ?
C59 C55 1.435(14) . ?
C99 H99A 0.9900 . ?
C99 H99B 0.9900 . ?
C99 C98 1.493(12) . ?
C98 H98A 0.9900 . ?
C98 H98B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.532(13) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.495(16) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.482(16) . ?
C27 H27 1.0000 . ?
C27 C32 1.543(12) . ?
C68 H68 0.9500 . ?
C68 C74 1.450(12) . ?
C75 H75 0.9500 . ?
C75 C74 1.391(14) . ?
C62 H62 1.0000 . ?
C62 C63 1.532(14) . ?
C62 C61 1.495(15) . ?
C55 C54 1.384(16) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.533(15) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.524(13) . ?
C61 H61 1.0000 . ?
C61 C66 1.541(13) . ?
C41 H41 0.9500 . ?
C41 C36 1.383(14) . ?
C37 H37 0.9500 . ?
C37 C36 1.383(15) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.532(13) . ?
C25 H25 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C82 C81 1.541(17) . ?
C80 H80A 0.9900 . ?
C80 H80B 0.9900 . ?
C80 C81 1.517(18) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C102 H102 0.9500 . ?
C102 C57 1.500(14) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C66 C65 1.547(19) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C64 C65 1.535(18) . ?
C57 C58 1.350(16) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C58 H58 0.9500 . ?
C58 C53 1.393(15) . ?
C54 H54 0.9500 . ?
C54 C53 1.387(17) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
O103 H10C 0.8500 . ?
O103 H10D 0.8501 . ?
O104 H10E 0.8496 . ?
O104 H10F 0.8504 . ?
O106 H10G 0.8492 . ?
O106 H10H 0.8507 . ?
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 C2 C7 C6 180.0(5) . . . . ?
Br1 C2 C3 C4 -179.1(5) . . . . ?
Br18 C19 C20 C21 -178.8(6) . . . . ?
Br69 C70 C75 C74 178.8(6) . . . . ?
N9 C8 C4 C3 173.0(7) . . . . ?
N9 C8 C4 C5 -5.0(12) . . . . ?
N9 C10 C11 N16 -60.6(8) . . . . ?
N9 C10 C11 C12 -179.1(6) . . . . ?
N9 C10 C15 C14 -179.3(7) . . . . ?
N43 C42 C38 C39 17.6(12) . . . . ?
N43 C42 C38 C37 -160.2(8) . . . . ?
N43 C44 C45 N50 -65.2(7) . . . . ?
N43 C44 C45 C46 175.1(6) . . . . ?
N43 C44 C49 C48 -177.1(7) . . . . ?
N94 C93 C89 C90 -168.3(7) . . . . ?
N94 C93 C89 C88 11.2(11) . . . . ?
N94 C95 C96 N101 -63.2(8) . . . . ?
N94 C95 C96 C97 176.7(6) . . . . ?
N94 C95 C100 C99 -175.3(7) . . . . ?
N77 C78 C83 C82 -174.1(8) . . . . ?
N77 C76 C72 C71 -1.2(12) . . . . ?
N77 C76 C72 C73 175.2(7) . . . . ?
N33 C28 C29 C30 -179.1(7) . . . . ?
N33 C28 C27 N26 -65.7(9) . . . . ?
N33 C28 C27 C32 174.9(7) . . . . ?
N33 C34 C40 C39 -173.0(8) . . . . ?
N33 C34 C40 C41 2.9(13) . . . . ?
C8 N9 C10 C11 126.8(7) . . . . ?
C8 N9 C10 C15 -113.2(8) . . . . ?
C8 C4 C3 C2 -178.8(7) . . . . ?
C8 C4 C5 C6 178.6(7) . . . . ?
N84 C79 C78 N77 -67.5(8) . . . . ?
N84 C79 C78 C83 175.2(7) . . . . ?
N84 C79 C80 C81 -178.2(10) . . . . ?
C2 C7 C6 C51 -178.7(7) . . . . ?
C2 C7 C6 C5 -1.2(11) . . . . ?
C7 C2 C3 C4 -0.1(11) . . . . ?
C7 C6 C51 N50 3.4(12) . . . . ?
C7 C6 C5 C4 0.3(11) . . . . ?
N101 C102 C57 C56 -8(2) . . . . ?
N101 C102 C57 C58 171.0(13) . . . . ?
N26 C27 C32 C31 -174.9(8) . . . . ?
N67 C68 C74 C73 -7.7(13) . . . . ?
N67 C68 C74 C75 172.2(8) . . . . ?
N67 C62 C63 C64 -178.8(10) . . . . ?
N67 C62 C61 N60 -61.7(10) . . . . ?
N67 C62 C61 C66 178.2(9) . . . . ?
C79 N84 C85 C91 176.4(7) . . . . ?
C79 C78 C83 C82 -55.8(10) . . . . ?
C79 C80 C81 C82 59.8(14) . . . . ?
N60 C59 C55 C56 -168.2(10) . . . . ?
N60 C59 C55 C54 19.0(17) . . . . ?
N60 C61 C66 C65 179.5(10) . . . . ?
C93 N94 C95 C96 120.5(8) . . . . ?
C93 N94 C95 C100 -119.0(8) . . . . ?
C93 C89 C90 C91 179.7(7) . . . . ?
C93 C89 C88 C87 -179.1(8) . . . . ?
C10 N9 C8 C4 176.0(7) . . . . ?
C91 C92 C87 Br86 -179.6(6) . . . . ?
C91 C92 C87 C88 -0.3(13) . . . . ?
C42 N43 C44 C45 118.1(8) . . . . ?
C42 N43 C44 C49 -118.8(8) . . . . ?
C42 C38 C37 C36 179.9(9) . . . . ?
C23 C24 C19 Br18 177.5(5) . . . . ?
C23 C24 C19 C20 -3.2(11) . . . . ?
C28 N33 C34 C40 175.5(7) . . . . ?
C28 C29 C30 C31 57.4(10) . . . . ?
C28 C27 C32 C31 -53.7(10) . . . . ?
C78 N77 C76 C72 176.4(7) . . . . ?
C78 C79 C80 C81 -57.0(13) . . . . ?
C78 C83 C82 C81 57.1(13) . . . . ?
C39 C38 C37 C36 2.1(14) . . . . ?
C39 C40 C41 C36 -2.2(13) . . . . ?
C11 N16 C17 C23 178.6(6) . . . . ?
C11 C10 C15 C14 -58.7(9) . . . . ?
C11 C12 C13 C14 53.9(10) . . . . ?
C17 N16 C11 C10 116.1(7) . . . . ?
C17 N16 C11 C12 -125.9(7) . . . . ?
C17 C23 C24 C19 -177.2(7) . . . . ?
C17 C23 C22 C21 179.3(7) . . . . ?
C3 C2 C7 C6 1.1(11) . . . . ?
C3 C4 C5 C6 0.6(11) . . . . ?
C51 N50 C45 C44 129.9(8) . . . . ?
C51 N50 C45 C46 -108.9(8) . . . . ?
C51 C6 C5 C4 177.9(7) . . . . ?
C44 N43 C42 C38 177.6(7) . . . . ?
C92 C91 C90 C89 -0.8(11) . . . . ?
C92 C91 C85 N84 -179.4(8) . . . . ?
C89 C88 C87 Br86 178.9(6) . . . . ?
C89 C88 C87 C92 -0.4(13) . . . . ?
C95 N94 C93 C89 -176.6(7) . . . . ?
C95 C100 C99 C98 56.8(10) . . . . ?
C90 C91 C92 C87 0.9(12) . . . . ?
C90 C91 C85 N84 -1.9(12) . . . . ?
C90 C89 C88 C87 0.4(12) . . . . ?
C76 N77 C78 C79 125.3(8) . . . . ?
C76 N77 C78 C83 -113.9(8) . . . . ?
C76 C72 C73 C74 -176.3(7) . . . . ?
C38 C39 C40 C34 177.3(7) . . . . ?
C38 C39 C40 C41 1.4(13) . . . . ?
C38 C37 C36 Br35 179.8(7) . . . . ?
C38 C37 C36 C41 -3.2(16) . . . . ?
C71 C70 C75 C74 0.0(12) . . . . ?
C71 C72 C73 C74 0.3(11) . . . . ?
C15 C10 C11 N16 -179.8(6) . . . . ?
C15 C10 C11 C12 61.7(8) . . . . ?
C15 C14 C13 C12 -50.1(11) . . . . ?
C5 C6 C51 N50 -174.2(8) . . . . ?
C5 C4 C3 C2 -0.7(11) . . . . ?
C24 C23 C17 N16 1.9(11) . . . . ?
C24 C23 C22 C21 -0.2(11) . . . . ?
C24 C19 C20 C21 1.8(12) . . . . ?
C70 C71 C72 C76 177.9(7) . . . . ?
C70 C71 C72 C73 1.6(11) . . . . ?
C70 C75 C74 C73 1.9(11) . . . . ?
C70 C75 C74 C68 -178.0(7) . . . . ?
C88 C89 C90 C91 0.2(11) . . . . ?
C83 C82 C81 C80 -59.1(13) . . . . ?
C85 N84 C79 C78 119.0(8) . . . . ?
C85 N84 C79 C80 -120.0(10) . . . . ?
C85 C91 C92 C87 178.4(7) . . . . ?
C85 C91 C90 C89 -178.3(7) . . . . ?
C46 C47 C48 C49 -56.8(10) . . . . ?
C34 N33 C28 C29 -120.5(8) . . . . ?
C34 N33 C28 C27 115.1(8) . . . . ?
C34 C40 C41 C36 -177.9(9) . . . . ?
C96 N101 C102 C57 -173.2(12) . . . . ?
C96 C95 C100 C99 -56.5(10) . . . . ?
C96 C97 C98 C99 57.5(10) . . . . ?
C72 C71 C70 Br69 179.5(6) . . . . ?
C72 C71 C70 C75 -1.7(12) . . . . ?
C72 C73 C74 C68 177.9(7) . . . . ?
C72 C73 C74 C75 -2.0(12) . . . . ?
C13 C12 C11 N16 -179.5(6) . . . . ?
C13 C12 C11 C10 -59.8(8) . . . . ?
C13 C14 C15 C10 52.7(11) . . . . ?
C56 C55 C54 C53 -3.0(18) . . . . ?
C56 C57 C58 C53 -2(2) . . . . ?
C40 C39 C38 C42 -179.2(8) . . . . ?
C40 C39 C38 C37 -1.3(12) . . . . ?
C40 C41 C36 Br35 -179.9(7) . . . . ?
C40 C41 C36 C37 3.1(15) . . . . ?
C22 C23 C17 N16 -177.6(7) . . . . ?
C22 C23 C24 C19 2.3(11) . . . . ?
C22 C21 C20 C19 0.3(11) . . . . ?
C22 C21 C25 N26 -6.7(13) . . . . ?
C20 C21 C22 C23 -1.2(12) . . . . ?
C20 C21 C25 N26 173.9(8) . . . . ?
C45 N50 C51 C6 178.7(7) . . . . ?
C45 C44 C49 C48 -55.3(9) . . . . ?
C45 C46 C47 C48 54.9(10) . . . . ?
C100 C95 C96 N101 177.2(7) . . . . ?
C100 C95 C96 C97 57.0(9) . . . . ?
C100 C99 C98 C97 -56.9(10) . . . . ?
C59 N60 C61 C62 125.8(10) . . . . ?
C59 N60 C61 C66 -112.8(11) . . . . ?
C59 C55 C54 C53 170.1(11) . . . . ?
C98 C97 C96 N101 -175.3(7) . . . . ?
C98 C97 C96 C95 -56.5(9) . . . . ?
C29 C28 C27 N26 172.7(7) . . . . ?
C29 C28 C27 C32 53.4(9) . . . . ?
C29 C30 C31 C32 -58.6(10) . . . . ?
C47 C46 C45 N50 -173.9(7) . . . . ?
C47 C46 C45 C44 -53.3(9) . . . . ?
C47 C48 C49 C44 56.9(10) . . . . ?
C27 N26 C25 C21 175.0(8) . . . . ?
C27 C28 C29 C30 -55.5(10) . . . . ?
C68 N67 C62 C63 -103.7(10) . . . . ?
C68 N67 C62 C61 135.4(9) . . . . ?
C62 N67 C68 C74 174.9(7) . . . . ?
C62 C63 C64 C65 59.5(15) . . . . ?
C62 C61 C66 C65 -59.4(13) . . . . ?
C55 C56 C57 C102 -177.2(12) . . . . ?
C55 C56 C57 C58 4(2) . . . . ?
C55 C54 C53 Br52 -179.2(9) . . . . ?
C55 C54 C53 C58 4.6(19) . . . . ?
C63 C62 C61 N60 179.2(8) . . . . ?
C63 C62 C61 C66 59.1(12) . . . . ?
C63 C64 C65 C66 -61.1(16) . . . . ?
C30 C31 C32 C27 56.2(11) . . . . ?
C61 N60 C59 C55 -177.5(10) . . . . ?
C61 C62 C63 C64 -58.7(13) . . . . ?
C61 C66 C65 C64 60.1(14) . . . . ?
C25 N26 C27 C28 131.4(8) . . . . ?
C25 N26 C27 C32 -107.0(9) . . . . ?
C25 C21 C22 C23 179.4(7) . . . . ?
C25 C21 C20 C19 179.8(7) . . . . ?
C80 C79 C78 N77 172.4(8) . . . . ?
C80 C79 C78 C83 55.1(10) . . . . ?
C49 C44 C45 N50 172.5(7) . . . . ?
C49 C44 C45 C46 52.8(9) . . . . ?
C102 N101 C96 C95 110.9(10) . . . . ?
C102 N101 C96 C97 -128.8(10) . . . . ?
C102 C57 C58 C53 178.9(13) . . . . ?
C57 C56 C55 C59 -174.3(11) . . . . ?
C57 C56 C55 C54 -1.3(18) . . . . ?
C57 C58 C53 Br52 -178.3(11) . . . . ?
C57 C58 C53 C54 -2(2) . . . . ?
