#------------------------------------------------------------------------------
#$Date: 2024-10-06 10:10:37 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295194 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/23/1572331.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_1572331
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, 0.65(C7 H8), C2.45 H2.45'
_chemical_formula_sum            'C49 H52.65 Br3 N6'
_chemical_formula_weight         965.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-12-07 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.692(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0041(2)
_cell_length_b                   14.3125(2)
_cell_length_c                   15.5247(3)
_cell_measurement_reflns_used    25294
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      28.1570
_cell_measurement_theta_min      1.9330
_cell_volume                     2302.09(7)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(11)
_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 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00  40.00   1.00   10.00    --    5.00 -57.00-180.00  124
  2  ω    -46.00  80.00   1.00   10.00    --   -8.90  68.00  90.00  126
  3  ω    -44.00  80.00   1.00   10.00    --   -8.90  57.00 -90.00  124
  4  ω    -44.00  80.00   1.00   10.00    --   -8.90  57.00 -30.00  124
  5  ω    -46.00  80.00   1.00   10.00    --   -8.90  68.00  30.00  126
  6  ω    -98.00   8.00   1.00   10.00    --   -8.90 -57.00 -30.00  106
;
_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      0.0190579000
_diffrn_orient_matrix_UB_12      -0.0006181000
_diffrn_orient_matrix_UB_13      0.0484478000
_diffrn_orient_matrix_UB_21      0.0354265000
_diffrn_orient_matrix_UB_22      -0.0416733000
_diffrn_orient_matrix_UB_23      0.0011003000
_diffrn_orient_matrix_UB_31      0.0553579000
_diffrn_orient_matrix_UB_32      0.0268354000
_diffrn_orient_matrix_UB_33      0.0028620000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47561
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.297
_diffrn_reflns_theta_min         1.966
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku 007HF (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.668
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88133
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             987
_exptl_crystal_preparation
'Slow vapour diffusion of toluene into an acetonitrile solution.'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 4342 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         11043
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0303
_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)+(0.0291P)²+1.1077P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0634
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.945
_reflns_number_gt                10218
_reflns_number_total             11043
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc04207g2.cif
_cod_data_source_block           33-rr_tol_w0002_ams384-1_mecntol_100k_1
_cod_depositor_comments
'Adding full bibliography for 1572326--1572335.cif.'
_cod_database_code               1572331
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C49 H53 Br3 N6'
_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   0.776
_shelx_estimated_absorpt_t_min   0.617
_reflns_odcompleteness_completeness 99.96
_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 C(H,H,H) groups
2. Restrained distances
 C58B-C52B = C58C-C56B
 1.5 with sigma of 0.02
 C57B-C52B \\sim C52B-C53B \\sim C53B-C54B \\sim C54B-C55B \\sim C55B-C56B
\\sim C57B-C56B
 with sigma of 0.02
 C58B-C53B \\sim C58B-C57B \\sim C58C-C55B \\sim C58C-C57B
 with sigma of 0.02
3. Restrained planarity
 C53B, C57B, C56B, C52B, C55B, C54B, C58B, C58C
 with sigma of 0.1
4. Others
 Fixed Sof: C57A(0.65) H57A(0.65) C55A(0.65) H55A(0.65) C56A(0.65) H56A(0.65)
 C52A(0.65) C54A(0.65) H54A(0.65) C53A(0.65) H53A(0.65) C58A(0.65) H58G(0.65)
 H58H(0.65) H58I(0.65) C52B(0.35) C57B(0.35) H57B(0.35) C54B(0.35) H54B(0.35)
 C53B(0.35) H53B(0.35) C56B(0.35) C55B(0.35) H55B(0.35) C58B(0.18) H58A(0.18)
 H58B(0.18) H58C(0.18) C58C(0.17) H58D(0.17) H58E(0.17) H58F(0.17)
5.a Ternary CH refined with riding coordinates:
 C27(H27), C44(H44), C28(H28), C11(H11), C49(H49), C10(H10)
5.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C15(H15A,H15B), C14(H14A,H14B), C30(H30A,H30B), C48(H48A,
 H48B), C29(H29A,H29B), C32(H32A,H32B), C47(H47A,H47B), C13(H13A,H13B),
 C31(H31A,H31B), C45(H45A,H45B), C46(H46A,H46B)
5.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C17(H17), C8(H8), C51(H51), C20(H20), C22(H22), C37(H37), C39(H39),
 C25(H25), C24(H24), C41(H41), C3(H3), C42(H42), C5(H5), C7(H7), C57A(H57A),
 C55A(H55A), C56A(H56A), C54A(H54A), C53A(H53A), C57B(H57B), C54B(H54B),
 C53B(H53B), C55B(H55B)
5.d Idealised Me refined as rotating group:
 C58A(H58G,H58H,H58I), C58B(H58A,H58B,H58C), C58C(H58D,H58E,H58F)
;
_olex2_date_sample_data_collection 2022-03-03
_olex2_submission_original_sample_id 'AMS384-1 MeCN Tol 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 1.220
_oxdiff_exptl_absorpt_empirical_full_min 0.845
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
Br18 Br 1.25218(3) 0.70065(2) 0.79342(2) 0.02668(9) Uani 1 1 d . . . . .
Br1 Br 0.97228(4) 0.76098(2) 0.21224(2) 0.02946(9) Uani 1 1 d . . . . .
Br35 Br 0.34011(4) 0.87198(3) 0.56873(3) 0.03492(10) Uani 1 1 d . . . . .
N16 N 1.1642(2) 0.3713(2) 0.58992(18) 0.0195(5) Uani 1 1 d . . . . .
N33 N 0.4710(3) 0.5156(2) 0.69210(18) 0.0187(6) Uani 1 1 d . . . . .
N50 N 0.5342(3) 0.5538(2) 0.15996(18) 0.0195(6) Uani 1 1 d . . . . .
N26 N 0.7425(3) 0.4618(2) 0.76791(18) 0.0196(6) Uani 1 1 d . . . . .
N43 N 0.3447(3) 0.5765(2) 0.25574(18) 0.0194(6) Uani 1 1 d . . . . .
C34 C 0.4479(3) 0.5078(2) 0.6070(2) 0.0167(6) Uani 1 1 d . . . . .
H34 H 0.457120 0.448518 0.582331 0.020 Uiso 1 1 calc R . . . .
N9 N 1.0676(2) 0.35057(19) 0.39456(18) 0.0186(6) Uani 1 1 d . . . . .
C4 C 0.9852(3) 0.4938(2) 0.3157(2) 0.0193(7) Uani 1 1 d . . . . .
C19 C 1.1236(3) 0.6070(2) 0.7481(2) 0.0178(6) Uani 1 1 d . . . . .
C17 C 1.0591(3) 0.3914(2) 0.6023(2) 0.0189(7) Uani 1 1 d . . . . .
H17 H 0.986408 0.352386 0.575227 0.023 Uiso 1 1 calc R . . . .
C27 C 0.6507(3) 0.4548(2) 0.8175(2) 0.0180(6) Uani 1 1 d . . . . .
H27 H 0.649293 0.515219 0.849489 0.022 Uiso 1 1 calc R . . . .
C8 C 1.0886(3) 0.4316(2) 0.3721(2) 0.0193(6) Uani 1 1 d . . . . .
H8 H 1.174870 0.453987 0.392360 0.023 Uiso 1 1 calc R . . . .
C51 C 0.6237(3) 0.4977(2) 0.1997(2) 0.0185(6) Uani 1 1 d . . . . .
H51 H 0.602559 0.435120 0.209322 0.022 Uiso 1 1 calc R . . . .
C20 C 1.0200(3) 0.6059(2) 0.7804(2) 0.0177(6) Uani 1 1 d . . . . .
H20 H 1.013307 0.651553 0.822986 0.021 Uiso 1 1 calc R . . . .
C44 C 0.3135(3) 0.5822(2) 0.1562(2) 0.0174(6) Uani 1 1 d . . . . .
H44 H 0.325401 0.647995 0.138733 0.021 Uiso 1 1 calc R . . . .
C28 C 0.5159(3) 0.4344(2) 0.7503(2) 0.0175(6) Uani 1 1 d . . . . .
H28 H 0.519461 0.379103 0.711856 0.021 Uiso 1 1 calc R . . . .
C22 C 0.9378(3) 0.4718(2) 0.6859(2) 0.0183(6) Uani 1 1 d . . . . .
H22 H 0.871933 0.426393 0.662272 0.022 Uiso 1 1 calc R . . . .
C11 C 1.1671(3) 0.2822(2) 0.5458(2) 0.0183(7) Uani 1 1 d . . . . .
H11 H 1.085276 0.247682 0.538626 0.022 Uiso 1 1 calc R . . . .
C36 C 0.3600(3) 0.7525(2) 0.5224(2) 0.0215(7) Uani 1 1 d . . . . .
C37 C 0.3481(3) 0.7452(2) 0.4301(2) 0.0200(7) Uani 1 1 d . . . . .
H37 H 0.329554 0.798776 0.391734 0.024 Uiso 1 1 calc R . . . .
C39 C 0.3936(3) 0.5803(2) 0.4528(2) 0.0163(6) Uani 1 1 d . . . . .
H39 H 0.404688 0.521136 0.428737 0.020 Uiso 1 1 calc R . . . .
C25 C 0.8201(3) 0.5299(2) 0.7874(2) 0.0179(6) Uani 1 1 d . . . . .
H25 H 0.810101 0.577470 0.827204 0.022 Uiso 1 1 calc R . . . .
C12 C 1.2809(3) 0.2243(2) 0.6053(2) 0.0193(7) Uani 1 1 d . . . . .
H12A H 1.272666 0.215001 0.666308 0.023 Uiso 1 1 calc R . . . .
H12B H 1.362186 0.258681 0.613839 0.023 Uiso 1 1 calc R . . . .
C24 C 1.1384(3) 0.5414(2) 0.6878(2) 0.0182(6) Uani 1 1 d . . . . .
H24 H 1.210999 0.542939 0.667861 0.022 Uiso 1 1 calc R . . . .
C41 C 0.3881(3) 0.6759(2) 0.5795(2) 0.0200(7) Uani 1 1 d . . . . .
H41 H 0.394637 0.682118 0.641860 0.024 Uiso 1 1 calc R . . . .
C15 C 1.1824(3) 0.2026(3) 0.4071(2) 0.0184(6) Uani 1 1 d . . . . .
H15A H 1.099896 0.169474 0.397632 0.022 Uiso 1 1 calc R . . . .
H15B H 1.191726 0.212198 0.346534 0.022 Uiso 1 1 calc R . . . .
C3 C 1.0183(3) 0.5819(3) 0.2941(2) 0.0216(7) Uani 1 1 d . . . . .
H3 H 1.105794 0.601802 0.315653 0.026 Uiso 1 1 calc R . . . .
C42 C 0.3470(3) 0.6529(2) 0.2970(2) 0.0176(6) Uani 1 1 d . . . . .
H42 H 0.337344 0.709378 0.263203 0.021 Uiso 1 1 calc R . . . .
C40 C 0.4070(3) 0.5889(2) 0.5447(2) 0.0162(6) Uani 1 1 d . . . . .
C14 C 1.2936(3) 0.1427(2) 0.4662(2) 0.0194(7) Uani 1 1 d . . . . .
H14A H 1.376448 0.172880 0.470766 0.023 Uiso 1 1 calc R . . . .
H14B H 1.290675 0.080916 0.436833 0.023 Uiso 1 1 calc R . . . .
C49 C 0.4022(3) 0.5174(2) 0.1260(2) 0.0181(6) Uani 1 1 d . . . . .
H49 H 0.400036 0.453250 0.150916 0.022 Uiso 1 1 calc R . . . .
C23 C 1.0437(3) 0.4720(2) 0.6564(2) 0.0183(6) Uani 1 1 d . . . . .
C30 C 0.4707(3) 0.3344(2) 0.8710(2) 0.0225(7) Uani 1 1 d . . . . .
H30A H 0.409723 0.324936 0.904753 0.027 Uiso 1 1 calc R . . . .
H30B H 0.473640 0.275913 0.837642 0.027 Uiso 1 1 calc R . . . .
C2 C 0.9226(3) 0.6406(2) 0.2407(2) 0.0214(7) Uani 1 1 d . . . . .
C48 C 0.3602(3) 0.5134(2) 0.0218(2) 0.0211(7) Uani 1 1 d . . . . .
H48A H 0.370555 0.575938 -0.002025 0.025 Uiso 1 1 calc R . . . .
H48B H 0.416667 0.469320 0.003717 0.025 Uiso 1 1 calc R . . . .
C29 C 0.4224(3) 0.4143(2) 0.8023(2) 0.0198(7) Uani 1 1 d . . . . .
H29A H 0.412136 0.471327 0.835270 0.024 Uiso 1 1 calc R . . . .
H29B H 0.336735 0.397702 0.758102 0.024 Uiso 1 1 calc R . . . .
C10 C 1.1787(3) 0.2971(2) 0.4512(2) 0.0164(6) Uani 1 1 d . . . . .
H10 H 1.259764 0.332312 0.457600 0.020 Uiso 1 1 calc R . . . .
C21 C 0.9263(3) 0.5367(2) 0.7493(2) 0.0181(6) Uani 1 1 d . . . . .
C38 C 0.3639(3) 0.6586(2) 0.3955(2) 0.0181(6) Uani 1 1 d . . . . .
C32 C 0.6991(3) 0.3774(3) 0.8883(2) 0.0214(7) Uani 1 1 d . . . . .
H32A H 0.782868 0.396368 0.933462 0.026 Uiso 1 1 calc R . . . .
H32B H 0.713710 0.320105 0.857378 0.026 Uiso 1 1 calc R . . . .
C5 C 0.8551(3) 0.4658(2) 0.2843(2) 0.0189(6) Uani 1 1 d . . . . .
H5 H 0.831755 0.405492 0.299029 0.023 Uiso 1 1 calc R . . . .
C47 C 0.2209(3) 0.4823(3) -0.0206(2) 0.0236(7) Uani 1 1 d . . . . .
H47A H 0.211109 0.418104 -0.000230 0.028 Uiso 1 1 calc R . . . .
H47B H 0.196438 0.481854 -0.088101 0.028 Uiso 1 1 calc R . . . .
C13 C 1.2866(3) 0.1293(2) 0.5620(2) 0.0216(7) Uani 1 1 d . . . . .
H13A H 1.363548 0.094461 0.600444 0.026 Uiso 1 1 calc R . . . .
H13B H 1.208974 0.092382 0.558403 0.026 Uiso 1 1 calc R . . . .
C31 C 0.6045(3) 0.3553(3) 0.9386(2) 0.0231(7) Uani 1 1 d . . . . .
H31A H 0.636134 0.300681 0.979116 0.028 Uiso 1 1 calc R . . . .
H31B H 0.599634 0.409231 0.977241 0.028 Uiso 1 1 calc R . . . .
C45 C 0.1723(3) 0.5541(3) 0.1117(2) 0.0216(7) Uani 1 1 d . . . . .
H45A H 0.116977 0.600075 0.128541 0.026 Uiso 1 1 calc R . . . .
H45B H 0.158465 0.492393 0.135796 0.026 Uiso 1 1 calc R . . . .
C46 C 0.1323(3) 0.5487(3) 0.0077(2) 0.0254(8) Uani 1 1 d . . . . .
H46A H 0.136519 0.611768 -0.017327 0.030 Uiso 1 1 calc R . . . .
H46B H 0.042038 0.526352 -0.017924 0.030 Uiso 1 1 calc R . . . .
C6 C 0.7608(3) 0.5265(2) 0.2317(2) 0.0185(6) Uani 1 1 d . . . . .
C7 C 0.7951(3) 0.6154(2) 0.2089(2) 0.0194(7) Uani 1 1 d . . . . .
H7 H 0.731262 0.657053 0.172350 0.023 Uiso 1 1 calc R . . . .
C57A C 0.7619(9) 0.8028(5) 0.8061(5) 0.0294(17) Uani 0.65 1 d . . P A 1
H57A H 0.756856 0.836408 0.752173 0.035 Uiso 0.65 1 calc R . P A 1
C55A C 0.6522(12) 0.7171(7) 0.8918(11) 0.058(4) Uani 0.65 1 d . . P A 1
H55A H 0.574127 0.693257 0.896627 0.070 Uiso 0.65 1 calc R . P A 1
C56A C 0.6547(7) 0.7648(6) 0.8146(6) 0.0386(16) Uani 0.65 1 d . . P A 1
H56A H 0.576133 0.771005 0.764820 0.046 Uiso 0.65 1 calc R . P A 1
C52A C 0.8833(6) 0.7928(5) 0.8776(6) 0.0319(15) Uani 0.65 1 d . . P A 1
C54A C 0.7695(15) 0.7061(7) 0.9615(7) 0.056(3) Uani 0.65 1 d . . P A 1
H54A H 0.771968 0.672127 1.014615 0.067 Uiso 0.65 1 calc R . P A 1
C53A C 0.8849(8) 0.7435(5) 0.9562(5) 0.0435(19) Uani 0.65 1 d . . P A 1
H53A H 0.963545 0.735383 1.005522 0.052 Uiso 0.65 1 calc R . P A 1
C58A C 1.0073(7) 0.8336(5) 0.8778(6) 0.0482(18) Uani 0.65 1 d . . P A 1
H58G H 1.006441 0.839474 0.814728 0.072 Uiso 0.65 1 calc GR . P A 1
H58H H 1.078568 0.792750 0.912289 0.072 Uiso 0.65 1 calc GR . P A 1
H58I H 1.018732 0.895416 0.906539 0.072 Uiso 0.65 1 calc GR . P A 1
C52B C 0.6865(17) 0.7050(16) 0.9123(14) 0.042(6) Uiso 0.35 1 d D . P B 2
C57B C 0.8113(17) 0.7206(13) 0.9598(15) 0.047(7) Uiso 0.35 1 d D . P B 2
H57B H 0.853232 0.700120 1.020870 0.057 Uiso 0.35 1 calc R . P B 2
C54B C 0.6803(19) 0.7772(14) 0.7804(15) 0.063(6) Uiso 0.35 1 d D . P B 2
H54B H 0.637913 0.795724 0.718744 0.076 Uiso 0.35 1 calc R . P B 2
C53B C 0.616(2) 0.7319(12) 0.8265(12) 0.058(5) Uiso 0.35 1 d D . P B 2
H53B H 0.526379 0.719173 0.800657 0.070 Uiso 0.35 1 calc R . P B 2
C56B C 0.8703(17) 0.7691(12) 0.9103(13) 0.060(6) Uiso 0.35 1 d D . P B 2
C55B C 0.8081(17) 0.7965(12) 0.8232(12) 0.038(5) Uiso 0.35 1 d D . P B 2
H55B H 0.854127 0.829914 0.791133 0.045 Uiso 0.35 1 calc R . P B 2
C58B C 0.6032(18) 0.6589(14) 0.9572(13) 0.031(5) Uiso 0.18 1 d D . P B 2
H58A H 0.655962 0.617965 1.006147 0.046 Uiso 0.18 1 calc GR . P B 2
H58B H 0.537079 0.621753 0.912030 0.046 Uiso 0.18 1 calc GR . P B 2
H58C H 0.561591 0.706482 0.983130 0.046 Uiso 0.18 1 calc GR . P B 2
C58C C 0.9999(18) 0.8011(16) 0.9545(16) 0.047(7) Uani 0.17 1 d D . P B 2
H58D H 1.000487 0.849746 0.999039 0.070 Uiso 0.17 1 calc GR . P B 2
H58E H 1.033960 0.826718 0.908665 0.070 Uiso 0.17 1 calc GR . P B 2
H58F H 1.053985 0.748652 0.986027 0.070 Uiso 0.17 1 calc GR . P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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
C17 N16 C11 116.0(3) . . ?
C34 N33 C28 119.1(3) . . ?
C51 N50 C49 117.8(3) . . ?
C25 N26 C27 117.2(3) . . ?
C42 N43 C44 116.3(3) . . ?
N33 C34 C40 121.6(3) . . ?
C8 N9 C10 117.2(3) . . ?
C3 C4 C8 118.7(3) . . ?
C3 C4 C5 119.8(3) . . ?
C5 C4 C8 121.6(3) . . ?
C20 C19 Br18 118.1(2) . . ?
C24 C19 Br18 119.4(2) . . ?
C24 C19 C20 122.5(3) . . ?
N16 C17 C23 123.5(3) . . ?
N26 C27 C28 109.7(2) . . ?
N26 C27 C32 107.1(3) . . ?
C32 C27 C28 112.1(3) . . ?
N9 C8 C4 123.1(3) . . ?
N50 C51 C6 121.8(3) . . ?
C19 C20 C21 118.9(3) . . ?
N43 C44 C49 110.0(2) . . ?
N43 C44 C45 107.6(2) . . ?
C45 C44 C49 111.0(3) . . ?
N33 C28 C27 108.7(3) . . ?
N33 C28 C29 109.3(3) . . ?
C27 C28 C29 110.3(3) . . ?
C23 C22 C21 121.2(3) . . ?
N16 C11 C12 109.6(3) . . ?
N16 C11 C10 110.6(3) . . ?
C12 C11 C10 109.9(3) . . ?
C37 C36 Br35 118.2(3) . . ?
C41 C36 Br35 120.2(2) . . ?
C41 C36 C37 121.6(3) . . ?
C38 C37 C36 118.9(3) . . ?
C40 C39 C38 120.2(3) . . ?
N26 C25 C21 121.0(3) . . ?
C11 C12 C13 111.4(3) . . ?
C19 C24 C23 118.5(3) . . ?
C36 C41 C40 119.3(3) . . ?
C14 C15 C10 111.6(2) . . ?
C2 C3 C4 119.2(3) . . ?
N43 C42 C38 123.1(3) . . ?
C39 C40 C34 120.3(3) . . ?
C39 C40 C41 119.7(3) . . ?
C41 C40 C34 119.9(3) . . ?
C15 C14 C13 111.3(3) . . ?
N50 C49 C44 109.3(3) . . ?
N50 C49 C48 107.7(3) . . ?
C48 C49 C44 110.6(3) . . ?
C22 C23 C17 117.2(3) . . ?
C22 C23 C24 119.7(3) . . ?
C24 C23 C17 122.6(3) . . ?
C31 C30 C29 111.2(3) . . ?
C3 C2 Br1 117.9(3) . . ?
C7 C2 Br1 119.6(3) . . ?
C7 C2 C3 122.4(3) . . ?
C47 C48 C49 111.8(3) . . ?
C30 C29 C28 111.7(3) . . ?
N9 C10 C11 109.1(3) . . ?
N9 C10 C15 109.8(2) . . ?
C15 C10 C11 109.3(3) . . ?
C20 C21 C25 120.0(3) . . ?
C22 C21 C20 119.2(3) . . ?
C22 C21 C25 120.8(3) . . ?
C37 C38 C39 120.2(3) . . ?
C37 C38 C42 117.5(3) . . ?
C39 C38 C42 122.2(3) . . ?
C27 C32 C31 112.7(3) . . ?
C6 C5 C4 119.8(3) . . ?
C48 C47 C46 110.0(3) . . ?
C14 C13 C12 109.9(3) . . ?
C30 C31 C32 110.8(3) . . ?
C44 C45 C46 112.3(3) . . ?
C45 C46 C47 110.5(3) . . ?
C5 C6 C51 119.9(3) . . ?
C5 C6 C7 120.3(3) . . ?
C7 C6 C51 119.8(3) . . ?
C2 C7 C6 118.5(3) . . ?
C56A C57A C52A 120.3(8) . . ?
C54A C55A C56A 116.4(9) . . ?
C57A C56A C55A 123.9(8) . . ?
C57A C52A C58A 125.5(8) . . ?
C53A C52A C57A 117.4(7) . . ?
C53A C52A C58A 117.0(7) . . ?
C55A C54A C53A 122.3(9) . . ?
C52A C53A C54A 119.7(7) . . ?
C57B C52B C53B 129.5(19) . . ?
C57B C52B C58B 119.8(15) . . ?
C53B C52B C58B 110.5(15) . . ?
C52B C57B C56B 111.8(18) . . ?
C53B C54B C55B 118.9(19) . . ?
C54B C53B C52B 116(2) . . ?
C57B C56B C58C 118.8(16) . . ?
C55B C56B C57B 122.6(17) . . ?
C55B C56B C58C 118.3(15) . . ?
C56B C55B C54B 121.3(17) . . ?
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
Br18 C19 1.903(3) . ?
Br1 C2 1.904(3) . ?
Br35 C36 1.897(3) . ?
N16 C17 1.268(4) . ?
N16 C11 1.452(4) . ?
N33 C34 1.264(4) . ?
N33 C28 1.453(4) . ?
N50 C51 1.260(4) . ?
N50 C49 1.464(4) . ?
N26 C27 1.466(4) . ?
N26 C25 1.263(4) . ?
N43 C44 1.468(4) . ?
N43 C42 1.264(4) . ?
C34 C40 1.480(4) . ?
N9 C8 1.254(4) . ?
N9 C10 1.458(4) . ?
C4 C8 1.478(5) . ?
C4 C3 1.384(5) . ?
C4 C5 1.407(5) . ?
C19 C20 1.392(5) . ?
C19 C24 1.373(5) . ?
C17 C23 1.469(5) . ?
C27 C28 1.527(4) . ?
C27 C32 1.525(5) . ?
C51 C6 1.480(5) . ?
C20 C21 1.393(5) . ?
C44 C49 1.530(4) . ?
C44 C45 1.526(4) . ?
C28 C29 1.534(4) . ?
C22 C23 1.388(4) . ?
C22 C21 1.390(5) . ?
C11 C12 1.525(4) . ?
C11 C10 1.532(4) . ?
C36 C37 1.399(4) . ?
C36 C41 1.377(5) . ?
C37 C38 1.384(5) . ?
C39 C40 1.391(4) . ?
C39 C38 1.399(5) . ?
C25 C21 1.481(4) . ?
C12 C13 1.528(5) . ?
C24 C23 1.402(5) . ?
C41 C40 1.401(5) . ?
C15 C14 1.522(5) . ?
C15 C10 1.523(5) . ?
C3 C2 1.383(5) . ?
C42 C38 1.478(4) . ?
C14 C13 1.528(5) . ?
C49 C48 1.526(4) . ?
C30 C29 1.531(5) . ?
C30 C31 1.523(5) . ?
C2 C7 1.370(5) . ?
C48 C47 1.516(5) . ?
C32 C31 1.530(5) . ?
C5 C6 1.388(5) . ?
C47 C46 1.528(5) . ?
C45 C46 1.526(4) . ?
C6 C7 1.405(5) . ?
C57A C56A 1.346(13) . ?
C57A C52A 1.428(10) . ?
C55A C56A 1.388(17) . ?
C55A C54A 1.386(18) . ?
C52A C53A 1.405(12) . ?
C52A C58A 1.482(10) . ?
C54A C53A 1.406(16) . ?
C52B C57B 1.341(19) . ?
C52B C53B 1.351(18) . ?
C52B C58B 1.48(2) . ?
C57B C56B 1.354(18) . ?
C54B C53B 1.331(17) . ?
C54B C55B 1.366(17) . ?
C56B C55B 1.351(17) . ?
C56B C58C 1.43(2) . ?
