#------------------------------------------------------------------------------
#$Date: 2024-10-06 10:10:37 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295194 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/23/1572334.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_1572334
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'
_chemical_formula_sum            'C42 H45 Br3 N6'
_chemical_formula_weight         873.57
_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             2022-09-11
_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                 91.9080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5723(3)
_cell_length_b                   18.9659(3)
_cell_length_c                   14.9238(2)
_cell_measurement_reflns_used    44387
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      27.7610
_cell_measurement_theta_min      1.7200
_cell_volume                     4122.31(12)
_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(10)
_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    -98.00  80.00   1.00    4.00    --   -8.90  23.00-158.00  178
  2  ω    -98.00  26.00   1.00    4.00    --   -8.90 -57.00 -30.00  124
  3  ω    -44.00  80.00   1.00    4.00    --   -8.90  57.00 -60.00  124
  4  ω    -98.00  26.00   1.00    4.00    --   -8.90 -57.00-120.00  124
  5  ω    -46.00  80.00   1.00    4.00    --   -8.90  68.00   0.00  126
  6  ω    -98.00  80.00   1.00    4.00    --   -8.90   0.00-180.00  178
  7  ω    -54.00  80.00   1.00    4.00    --   -8.90  38.00-120.00  134
  8  ω    -98.00  24.00   1.00    4.00    --   -8.90 -68.00-180.00  122
  9  ω    -98.00  26.00   1.00    4.00    --   -8.90 -57.00  90.00  124
;
_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      -0.0481981000
_diffrn_orient_matrix_UB_12      0.0053996000
_diffrn_orient_matrix_UB_13      -0.0011447000
_diffrn_orient_matrix_UB_21      -0.0014500000
_diffrn_orient_matrix_UB_22      -0.0099322000
_diffrn_orient_matrix_UB_23      0.0457806000
_diffrn_orient_matrix_UB_31      0.0068937000
_diffrn_orient_matrix_UB_32      0.0356355000
_diffrn_orient_matrix_UB_33      0.0128463000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            145655
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.321
_diffrn_reflns_theta_min         1.737
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku 007HF (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.972
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.171
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_preparation
'Slow evaporation of a methanol solution followed by annealing under the cryostream at 375 K for 15 minutes.'
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.126
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.002(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         20267
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1138P)²+10.3415P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                17354
_reflns_number_total             20267
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc04207g2.cif
_cod_data_source_block           33-rr_desolv_w0077_ams337-3_meoh_100k_1
_cod_depositor_comments
'Adding full bibliography for 1572326--1572335.cif.'
_cod_database_code               1572334
_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   0.706
_shelx_estimated_absorpt_t_min   0.400
_reflns_odcompleteness_completeness 99.97
_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
2.a Ternary CH refined with riding coordinates:
 C28(H28), C44(H44), C10(H10), C96(H96), C79(H79), C27(H27), C95(H95),
 C78(H78), C11(H11), C45(H45), C62(H62), C61(H61)
2.b Secondary CH2 refined with riding coordinates:
 C98(H98A,H98B), C13(H13A,H13B), C15(H15A,H15B), C100(H10A,H10B), C99(H99A,
 H99B), C83(H83A,H83B), C97(H97A,H97B), C12(H12A,H12B), C29(H29A,H29B),
 C14(H14A,H14B), C32(H32A,H32B), C81(H81A,H81B), C82(H82A,H82B), C46(H46A,H46B),
  C31(H31A,H31B), C80(H80A,H80B), C30(H30A,H30B), C49(H49A,H49B), C47(H47A,
 H47B), C48(H48A,H48B), C64(H64A,H64B), C63(H63A,H63B), C66(H66A,H66B),
 C65(H65A,H65B)
2.c Aromatic/amide H refined with riding coordinates:
 C102(H102), C17(H17), C8(H8), C24(H24), C90(H90), C76(H76), C93(H93),
 C25(H25), C68(H68), C20(H20), C39(H39), C92(H92), C34(H34), C71(H71), C75(H75),
  C37(H37), C56(H56), C59(H59), C85(H85), C58(H58), C88(H88), C5(H5), C41(H41),
 C51(H51), C22(H22), C42(H42), C54(H54), C7(H7), C73(H73), C3(H3)
;
_olex2_date_sample_data_collection 2022-04-26
_olex2_submission_original_sample_id 'AMS337-1 MeOH Desolv 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 1.712
_oxdiff_exptl_absorpt_empirical_full_min 0.630
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 1.16484(6) 0.56945(5) 0.84985(6) 0.0262(2) Uani 1 1 d . . . . .
Br86 Br -0.00920(6) 0.38651(5) 1.15979(6) 0.0248(2) Uani 1 1 d . . . . .
Br35 Br 0.60830(7) 0.65236(5) 0.80473(6) 0.0277(2) Uani 1 1 d . . . . .
Br1 Br 0.91331(7) 0.63457(5) 0.29137(7) 0.0297(2) Uani 1 1 d . . . . .
Br69 Br 0.42123(8) 0.29056(5) 0.76577(7) 0.0310(2) Uani 1 1 d . . . . .
Br52 Br -0.14165(7) 0.41544(6) 0.60757(7) 0.0309(2) Uani 1 1 d . . . . .
N9 N 1.0770(5) 0.3379(4) 0.4388(5) 0.0217(16) Uani 1 1 d . . . . .
N101 N -0.1276(5) 0.6878(4) 0.8672(5) 0.0226(16) Uani 1 1 d . . . . .
N26 N 0.8630(5) 0.3326(4) 0.9381(5) 0.0203(15) Uani 1 1 d . . . . .
N94 N -0.0738(5) 0.6586(4) 1.0509(5) 0.0208(15) Uani 1 1 d . . . . .
N50 N 0.6617(5) 0.4243(4) 0.3392(5) 0.0226(16) Uani 1 1 d . . . . .
N77 N 0.4704(5) 0.5241(4) 0.9773(5) 0.0229(16) Uani 1 1 d . . . . .
N43 N 0.5455(5) 0.4207(5) 0.4925(5) 0.0243(16) Uani 1 1 d . . . . .
N16 N 1.1535(5) 0.3338(4) 0.6218(5) 0.0187(15) Uani 1 1 d . . . . .
N67 N 0.3197(6) 0.5882(5) 0.5748(6) 0.0277(18) Uani 1 1 d . . . . .
N60 N 0.1264(6) 0.6150(5) 0.5353(6) 0.0268(17) Uani 1 1 d . . . . .
C102 C -0.1461(6) 0.6265(5) 0.8394(6) 0.0223(18) Uani 1 1 d . . . . .
H102 H -0.190260 0.599424 0.869772 0.027 Uiso 1 1 calc R . . . .
N84 N 0.3561(5) 0.5760(4) 1.1213(5) 0.0226(15) Uani 1 1 d . . . . .
N33 N 0.6789(5) 0.3800(5) 0.9020(5) 0.0234(16) Uani 1 1 d . . . . .
C17 C 1.0850(6) 0.3303(5) 0.6706(6) 0.0187(17) Uani 1 1 d . . . . .
H17 H 1.042951 0.292764 0.659950 0.022 Uiso 1 1 calc R . . . .
C8 C 1.0763(6) 0.4017(5) 0.4137(6) 0.0223(19) Uani 1 1 d . . . . .
H8 H 1.132443 0.427084 0.412533 0.027 Uiso 1 1 calc R . . . .
C57 C -0.1015(7) 0.5952(5) 0.7613(6) 0.0235(19) Uani 1 1 d . . . . .
C28 C 0.6984(6) 0.3153(5) 0.9521(6) 0.0209(18) Uani 1 1 d . . . . .
H28 H 0.702278 0.274673 0.909728 0.025 Uiso 1 1 calc R . . . .
C91 C 0.2018(6) 0.5296(5) 1.1270(6) 0.0202(17) Uani 1 1 d . . . . .
C24 C 1.1174(6) 0.4422(5) 0.7576(6) 0.0198(17) Uani 1 1 d . . . . .
H24 H 1.166182 0.453661 0.719570 0.024 Uiso 1 1 calc R . . . .
C87 C 0.0562(6) 0.4706(5) 1.1386(6) 0.0204(17) Uani 1 1 d . . . . .
C90 C 0.1551(6) 0.5916(5) 1.1055(6) 0.0215(18) Uani 1 1 d . . . . .
H90 H 0.188839 0.633575 1.095342 0.026 Uiso 1 1 calc R . . . .
C76 C 0.4355(6) 0.5482(5) 0.9050(6) 0.0206(18) Uani 1 1 d . . . . .
H76 H 0.426735 0.597674 0.899644 0.025 Uiso 1 1 calc R . . . .
C93 C 0.0117(6) 0.6589(5) 1.0698(6) 0.0219(18) Uani 1 1 d . . . . .
H93 H 0.045451 0.701556 1.065616 0.026 Uiso 1 1 calc R . . . .
C25 C 0.9009(6) 0.3929(5) 0.9337(5) 0.0187(16) Uani 1 1 d . . . . .
H25 H 0.880841 0.429256 0.972229 0.022 Uiso 1 1 calc R . . . .
C68 C 0.3181(6) 0.5224(5) 0.5898(6) 0.0222(18) Uani 1 1 d . . . . .
H68 H 0.293854 0.492049 0.544204 0.027 Uiso 1 1 calc R . . . .
C23 C 1.0652(6) 0.3806(5) 0.7434(6) 0.0183(16) Uani 1 1 d . . . . .
C19 C 1.0961(6) 0.4857(5) 0.8283(6) 0.0209(17) Uani 1 1 d . . . . .
C20 C 1.0255(6) 0.4710(5) 0.8846(6) 0.0199(17) Uani 1 1 d . . . . .
H20 H 1.011582 0.502518 0.931667 0.024 Uiso 1 1 calc R . . . .
C44 C 0.5092(6) 0.4184(5) 0.3999(6) 0.0242(18) Uani 1 1 d . . . . .
H44 H 0.499115 0.467493 0.377215 0.029 Uiso 1 1 calc R . . . .
C39 C 0.6140(6) 0.4295(5) 0.6734(6) 0.0217(18) Uani 1 1 d . . . . .
H39 H 0.614433 0.384072 0.646519 0.026 Uiso 1 1 calc R . . . .
C4 C 0.9897(7) 0.4372(5) 0.3860(6) 0.0221(18) Uani 1 1 d . . . . .
C10 C 1.1648(6) 0.3054(5) 0.4613(6) 0.0214(18) Uani 1 1 d . . . . .
H10 H 1.215437 0.340648 0.456220 0.026 Uiso 1 1 calc R . . . .
C92 C 0.1508(6) 0.4688(5) 1.1446(6) 0.0215(18) Uani 1 1 d . . . . .
H92 H 0.181448 0.426200 1.160817 0.026 Uiso 1 1 calc R . . . .
C34 C 0.6612(6) 0.3752(5) 0.8188(6) 0.0214(18) Uani 1 1 d . . . . .
H34 H 0.662841 0.330241 0.790869 0.026 Uiso 1 1 calc R . . . .
C71 C 0.4197(6) 0.4291(5) 0.8344(6) 0.0213(18) Uani 1 1 d . . . . .
H71 H 0.441998 0.407861 0.888458 0.026 Uiso 1 1 calc R . . . .
C55 C 0.0112(7) 0.5989(5) 0.6453(6) 0.0246(19) Uani 1 1 d . . . . .
C98 C -0.2797(7) 0.8145(5) 0.9914(7) 0.027(2) Uani 1 1 d . . . . .
H98A H -0.306429 0.860231 0.972218 0.033 Uiso 1 1 calc R . . . .
H98B H -0.330565 0.782666 1.007085 0.033 Uiso 1 1 calc R . . . .
C13 C 1.2641(7) 0.1743(5) 0.5134(7) 0.029(2) Uani 1 1 d . . . . .
H13A H 1.322773 0.149756 0.527582 0.034 Uiso 1 1 calc R . . . .
H13B H 1.213503 0.140180 0.520685 0.034 Uiso 1 1 calc R . . . .
C15 C 1.1776(7) 0.2445(6) 0.3948(6) 0.027(2) Uani 1 1 d . . . . .
H15A H 1.122870 0.213661 0.395058 0.033 Uiso 1 1 calc R . . . .
H15B H 1.182375 0.264134 0.333683 0.033 Uiso 1 1 calc R . . . .
C100 C -0.1688(6) 0.7570(5) 1.1010(7) 0.0242(19) Uani 1 1 d . . . . .
H10A H -0.215468 0.722406 1.119140 0.029 Uiso 1 1 calc R . . . .
H10B H -0.126688 0.765840 1.153235 0.029 Uiso 1 1 calc R . . . .
C75 C 0.3635(6) 0.4180(5) 0.6803(6) 0.0222(18) Uani 1 1 d . . . . .
H75 H 0.347421 0.388737 0.630505 0.027 Uiso 1 1 calc R . . . .
C96 C -0.1788(6) 0.7132(5) 0.9425(6) 0.0201(17) Uani 1 1 d . . . . .
H96 H -0.226069 0.677431 0.958439 0.024 Uiso 1 1 calc R . . . .
C79 C 0.4537(6) 0.5607(5) 1.1324(6) 0.0216(18) Uani 1 1 d . . . . .
H79 H 0.461639 0.509935 1.149072 0.026 Uiso 1 1 calc R . . . .
C99 C -0.2158(7) 0.8254(5) 1.0732(7) 0.029(2) Uani 1 1 d . . . . .
H99A H -0.168828 0.861114 1.059189 0.035 Uiso 1 1 calc R . . . .
H99B H -0.251598 0.843478 1.123557 0.035 Uiso 1 1 calc R . . . .
C70 C 0.3985(6) 0.3887(5) 0.7600(6) 0.0210(17) Uani 1 1 d . . . . .
C27 C 0.7906(6) 0.3249(5) 1.0033(6) 0.0210(18) Uani 1 1 d . . . . .
H27 H 0.788006 0.368703 1.040321 0.025 Uiso 1 1 calc R . . . .
C38 C 0.5893(6) 0.4885(5) 0.6225(6) 0.0215(18) Uani 1 1 d . . . . .
C53 C -0.0942(6) 0.5025(5) 0.6517(6) 0.0239(19) Uani 1 1 d . . . . .
C74 C 0.3524(6) 0.4907(5) 0.6750(6) 0.0198(17) Uani 1 1 d . . . . .
C89 C 0.0595(6) 0.5929(5) 1.0986(6) 0.0210(18) Uani 1 1 d . . . . .
C83 C 0.6070(6) 0.5640(5) 1.0590(7) 0.027(2) Uani 1 1 d . . . . .
H83A H 0.619693 0.513852 1.072987 0.032 Uiso 1 1 calc R . . . .
H83B H 0.638051 0.575910 1.003029 0.032 Uiso 1 1 calc R . . . .
C40 C 0.6380(6) 0.4375(5) 0.7641(6) 0.0206(18) Uani 1 1 d . . . . .
C97 C -0.2266(6) 0.7823(5) 0.9145(7) 0.0230(18) Uani 1 1 d . . . . .
H97A H -0.179933 0.816477 0.894868 0.028 Uiso 1 1 calc R . . . .
H97B H -0.269494 0.773148 0.862968 0.028 Uiso 1 1 calc R . . . .
C37 C 0.5892(6) 0.5550(5) 0.6614(6) 0.0237(19) Uani 1 1 d . . . . .
H37 H 0.572686 0.595361 0.626761 0.028 Uiso 1 1 calc R . . . .
C56 C -0.0283(6) 0.6286(5) 0.7202(6) 0.0221(18) Uani 1 1 d . . . . .
H56 H -0.005377 0.672002 0.743608 0.026 Uiso 1 1 calc R . . . .
C59 C 0.0881(6) 0.6363(5) 0.6049(6) 0.0257(19) Uani 1 1 d . . . . .
H59 H 0.109868 0.678509 0.632578 0.031 Uiso 1 1 calc R . . . .
C85 C 0.3028(6) 0.5245(5) 1.1321(6) 0.0216(18) Uani 1 1 d . . . . .
H85 H 0.329329 0.479588 1.144350 0.026 Uiso 1 1 calc R . . . .
C95 C -0.1142(6) 0.7265(5) 1.0237(6) 0.0210(18) Uani 1 1 d . . . . .
H95 H -0.064703 0.760100 1.007168 0.025 Uiso 1 1 calc R . . . .
C21 C 0.9744(6) 0.4089(5) 0.8716(6) 0.0187(16) Uani 1 1 d . . . . .
C58 C -0.1336(6) 0.5315(5) 0.7265(6) 0.0233(18) Uani 1 1 d . . . . .
H58 H -0.182691 0.507836 0.754025 0.028 Uiso 1 1 calc R . . . .
C88 C 0.0102(6) 0.5314(5) 1.1158(6) 0.0198(17) Uani 1 1 d . . . . .
H88 H -0.054998 0.531721 1.111762 0.024 Uiso 1 1 calc R . . . .
C12 C 1.2529(7) 0.2359(5) 0.5786(6) 0.0251(19) Uani 1 1 d . . . . .
H12A H 1.305827 0.268334 0.574471 0.030 Uiso 1 1 calc R . . . .
H12B H 1.251802 0.217775 0.640711 0.030 Uiso 1 1 calc R . . . .
C5 C 0.9062(6) 0.4010(5) 0.3856(6) 0.0235(19) Uani 1 1 d . . . . .
H5 H 0.905006 0.352917 0.403319 0.028 Uiso 1 1 calc R . . . .
C78 C 0.5027(6) 0.5746(5) 1.0449(6) 0.0204(17) Uani 1 1 d . . . . .
H78 H 0.489734 0.623744 1.023725 0.024 Uiso 1 1 calc R . . . .
C29 C 0.6212(7) 0.3028(5) 1.0170(6) 0.027(2) Uani 1 1 d . . . . .
H29A H 0.563492 0.292862 0.982421 0.032 Uiso 1 1 calc R . . . .
H29B H 0.611842 0.346042 1.052706 0.032 Uiso 1 1 calc R . . . .
C11 C 1.1631(6) 0.2766(5) 0.5565(6) 0.0205(18) Uani 1 1 d . . . . .
H11 H 1.109908 0.243612 0.561156 0.025 Uiso 1 1 calc R . . . .
C41 C 0.6368(6) 0.5045(5) 0.8038(6) 0.0208(18) Uani 1 1 d . . . . .
H41 H 0.651828 0.510133 0.865867 0.025 Uiso 1 1 calc R . . . .
C14 C 1.2633(7) 0.2003(6) 0.4174(7) 0.031(2) Uani 1 1 d . . . . .
H14A H 1.265084 0.159353 0.376311 0.037 Uiso 1 1 calc R . . . .
H14B H 1.318877 0.229105 0.408115 0.037 Uiso 1 1 calc R . . . .
C32 C 0.8109(6) 0.2623(5) 1.0647(6) 0.0220(18) Uani 1 1 d . . . . .
H32A H 0.869733 0.270258 1.098277 0.026 Uiso 1 1 calc R . . . .
H32B H 0.817057 0.219074 1.028296 0.026 Uiso 1 1 calc R . . . .
C81 C 0.5973(7) 0.5962(6) 1.2223(7) 0.029(2) Uani 1 1 d . . . . .
H81A H 0.621142 0.628544 1.269617 0.034 Uiso 1 1 calc R . . . .
H81B H 0.609879 0.547206 1.242199 0.034 Uiso 1 1 calc R . . . .
C2 C 0.9098(7) 0.5398(5) 0.3315(6) 0.0228(18) Uani 1 1 d . . . . .
C51 C 0.7373(6) 0.3958(5) 0.3613(6) 0.0229(18) Uani 1 1 d . . . . .
H51 H 0.737851 0.347819 0.379787 0.027 Uiso 1 1 calc R . . . .
C45 C 0.5790(6) 0.3811(5) 0.3424(6) 0.0212(17) Uani 1 1 d . . . . .
H45 H 0.594384 0.333861 0.368630 0.025 Uiso 1 1 calc R . . . .
C22 C 0.9942(6) 0.3646(5) 0.8001(6) 0.0187(17) Uani 1 1 d . . . . .
H22 H 0.958792 0.323102 0.790002 0.022 Uiso 1 1 calc R . . . .
C72 C 0.4077(6) 0.5029(5) 0.8287(6) 0.0203(17) Uani 1 1 d . . . . .
C42 C 0.5575(6) 0.4809(5) 0.5277(6) 0.0229(18) Uani 1 1 d . . . . .
H42 H 0.545901 0.521919 0.492659 0.027 Uiso 1 1 calc R . . . .
C54 C -0.0229(7) 0.5350(6) 0.6104(6) 0.026(2) Uani 1 1 d . . . . .
H54 H 0.003086 0.514527 0.558970 0.031 Uiso 1 1 calc R . . . .
C36 C 0.6137(6) 0.5615(5) 0.7520(6) 0.0215(18) Uani 1 1 d . . . . .
C82 C 0.6458(7) 0.6104(5) 1.1357(7) 0.029(2) Uani 1 1 d . . . . .
H82A H 0.712209 0.600818 1.144843 0.034 Uiso 1 1 calc R . . . .
H82B H 0.638283 0.660642 1.119293 0.034 Uiso 1 1 calc R . . . .
C46 C 0.5398(7) 0.3723(5) 0.2466(6) 0.026(2) Uani 1 1 d . . . . .
H46A H 0.532511 0.419347 0.218553 0.031 Uiso 1 1 calc R . . . .
H46B H 0.583803 0.345051 0.211145 0.031 Uiso 1 1 calc R . . . .
C31 C 0.7342(7) 0.2525(5) 1.1304(7) 0.028(2) Uani 1 1 d . . . . .
H31A H 0.748122 0.211436 1.169485 0.034 Uiso 1 1 calc R . . . .
H31B H 0.730128 0.294819 1.169003 0.034 Uiso 1 1 calc R . . . .
C80 C 0.4938(6) 0.6067(5) 1.2086(6) 0.0252(19) Uani 1 1 d . . . . .
H80A H 0.481241 0.656927 1.194806 0.030 Uiso 1 1 calc R . . . .
H80B H 0.463120 0.594985 1.264912 0.030 Uiso 1 1 calc R . . . .
C62 C 0.2847(7) 0.6138(5) 0.4877(7) 0.027(2) Uani 1 1 d . . . . .
H62 H 0.267541 0.572894 0.448331 0.033 Uiso 1 1 calc R . . . .
C7 C 0.8272(7) 0.5052(5) 0.3315(6) 0.0234(19) Uani 1 1 d . . . . .
H7 H 0.772245 0.528700 0.312859 0.028 Uiso 1 1 calc R . . . .
C6 C 0.8249(6) 0.4345(5) 0.3595(6) 0.0238(19) Uani 1 1 d . . . . .
C30 C 0.6431(8) 0.2410(6) 1.0803(7) 0.031(2) Uani 1 1 d . . . . .
H30A H 0.593658 0.236163 1.123802 0.038 Uiso 1 1 calc R . . . .
H30B H 0.645763 0.196734 1.045279 0.038 Uiso 1 1 calc R . . . .
C61 C 0.2003(7) 0.6598(5) 0.5020(7) 0.028(2) Uani 1 1 d . . . . .
H61 H 0.215941 0.697064 0.547410 0.034 Uiso 1 1 calc R . . . .
C49 C 0.4180(7) 0.3788(6) 0.3984(7) 0.032(2) Uani 1 1 d . . . . .
H49A H 0.427272 0.331432 0.425025 0.038 Uiso 1 1 calc R . . . .
H49B H 0.373609 0.404616 0.434967 0.038 Uiso 1 1 calc R . . . .
C73 C 0.3751(6) 0.5329(5) 0.7494(6) 0.0208(18) Uani 1 1 d . . . . .
H73 H 0.367972 0.582653 0.745437 0.025 Uiso 1 1 calc R . . . .
C47 C 0.4477(8) 0.3348(7) 0.2438(7) 0.038(3) Uani 1 1 d . . . . .
H47A H 0.456368 0.285508 0.264305 0.045 Uiso 1 1 calc R . . . .
H47B H 0.422967 0.333586 0.181247 0.045 Uiso 1 1 calc R . . . .
C3 C 0.9913(7) 0.5074(5) 0.3588(6) 0.0242(19) Uani 1 1 d . . . . .
H3 H 1.047567 0.532791 0.358931 0.029 Uiso 1 1 calc R . . . .
C48 C 0.3792(8) 0.3713(7) 0.3028(7) 0.038(3) Uani 1 1 d . . . . .
H48A H 0.321591 0.343638 0.303096 0.046 Uiso 1 1 calc R . . . .
H48B H 0.364560 0.418594 0.278051 0.046 Uiso 1 1 calc R . . . .
C64 C 0.3270(8) 0.6919(7) 0.3572(8) 0.042(3) Uani 1 1 d . . . . .
H64A H 0.311205 0.655110 0.312215 0.050 Uiso 1 1 calc R . . . .
H64B H 0.376655 0.721411 0.333353 0.050 Uiso 1 1 calc R . . . .
C63 C 0.3602(8) 0.6573(7) 0.4444(8) 0.038(3) Uani 1 1 d . . . . .
H63A H 0.381851 0.694251 0.486879 0.046 Uiso 1 1 calc R . . . .
H63B H 0.412931 0.626169 0.432262 0.046 Uiso 1 1 calc R . . . .
C66 C 0.1671(8) 0.6944(7) 0.4148(8) 0.038(3) Uani 1 1 d . . . . .
H66A H 0.114338 0.725523 0.426719 0.046 Uiso 1 1 calc R . . . .
H66B H 0.145879 0.657554 0.372002 0.046 Uiso 1 1 calc R . . . .
C65 C 0.2429(9) 0.7376(7) 0.3731(9) 0.044(3) Uani 1 1 d . . . . .
H65A H 0.260300 0.777142 0.413468 0.053 Uiso 1 1 calc R . . . .
H65B H 0.219853 0.757678 0.315407 0.053 Uiso 1 1 calc R . . . .
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 25 -1 0.1431
-10 11 17 0.1034
-9 -24 3 0.1460
8 -15 -16 0.1184
2 26 5 0.1603
15 -4 13 0.0471
-15 6 -13 0.0722
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 118.2(8) . . ?
C102 N101 C96 116.8(8) . . ?
C25 N26 C27 116.6(7) . . ?
C93 N94 C95 116.1(8) . . ?
C51 N50 C45 117.8(8) . . ?
C76 N77 C78 117.7(8) . . ?
C42 N43 C44 117.4(8) . . ?
C17 N16 C11 116.1(8) . . ?
C68 N67 C62 118.4(9) . . ?
C59 N60 C61 116.2(9) . . ?
N101 C102 C57 122.4(9) . . ?
C85 N84 C79 115.8(8) . . ?
C34 N33 C28 118.3(8) . . ?
N16 C17 C23 124.7(8) . . ?
N9 C8 C4 121.1(8) . . ?
C56 C57 C102 121.6(9) . . ?
C58 C57 C102 119.5(9) . . ?
C58 C57 C56 118.8(9) . . ?
N33 C28 C27 108.0(7) . . ?
N33 C28 C29 108.7(8) . . ?
C29 C28 C27 110.7(7) . . ?
C90 C91 C92 118.7(8) . . ?
C90 C91 C85 123.2(8) . . ?
C92 C91 C85 118.1(8) . . ?
C19 C24 C23 118.4(8) . . ?
C92 C87 Br86 118.5(7) . . ?
C88 C87 Br86 120.4(7) . . ?
C88 C87 C92 121.1(8) . . ?
C91 C90 C89 120.8(9) . . ?
N77 C76 C72 122.8(8) . . ?
N94 C93 C89 120.5(9) . . ?
N26 C25 C21 122.9(8) . . ?
N67 C68 C74 123.0(9) . . ?
C24 C23 C17 121.8(8) . . ?
C22 C23 C17 118.3(8) . . ?
C22 C23 C24 119.9(8) . . ?
C24 C19 Br18 119.8(7) . . ?
C20 C19 Br18 117.8(7) . . ?
C20 C19 C24 122.4(8) . . ?
C19 C20 C21 119.3(8) . . ?
N43 C44 C45 108.5(8) . . ?
N43 C44 C49 108.4(8) . . ?
C45 C44 C49 111.1(8) . . ?
C38 C39 C40 119.5(9) . . ?
C5 C4 C8 120.8(8) . . ?
C3 C4 C8 119.6(9) . . ?
C3 C4 C5 119.5(9) . . ?
N9 C10 C15 107.2(7) . . ?
N9 C10 C11 109.1(7) . . ?
C11 C10 C15 109.8(8) . . ?
C87 C92 C91 120.2(8) . . ?
N33 C34 C40 121.7(9) . . ?
C70 C71 C72 118.7(8) . . ?
C56 C55 C59 118.3(9) . . ?
C56 C55 C54 119.8(9) . . ?
C54 C55 C59 121.9(9) . . ?
C99 C98 C97 110.1(8) . . ?
C14 C13 C12 110.8(8) . . ?
C14 C15 C10 112.7(8) . . ?
C99 C100 C95 110.9(8) . . ?
C74 C75 C70 118.8(8) . . ?
N101 C96 C97 108.2(7) . . ?
N101 C96 C95 110.4(7) . . ?
C95 C96 C97 109.6(7) . . ?
N84 C79 C78 110.6(7) . . ?
N84 C79 C80 108.5(7) . . ?
C78 C79 C80 110.9(8) . . ?
C100 C99 C98 111.1(8) . . ?
C71 C70 Br69 118.5(7) . . ?
C71 C70 C75 122.2(9) . . ?
C75 C70 Br69 119.3(7) . . ?
N26 C27 C28 108.6(7) . . ?
N26 C27 C32 110.3(7) . . ?
C32 C27 C28 111.0(8) . . ?
C39 C38 C42 120.6(8) . . ?
C37 C38 C39 120.4(8) . . ?
C37 C38 C42 118.9(9) . . ?
C58 C53 Br52 118.0(7) . . ?
C54 C53 Br52 120.5(7) . . ?
C54 C53 C58 121.6(9) . . ?
C75 C74 C68 119.1(9) . . ?
C75 C74 C73 119.9(8) . . ?
C73 C74 C68 120.9(8) . . ?
C90 C89 C93 119.6(8) . . ?
C90 C89 C88 119.3(9) . . ?
C88 C89 C93 121.1(8) . . ?
C82 C83 C78 111.4(8) . . ?
C39 C40 C34 119.8(8) . . ?
C39 C40 C41 120.2(9) . . ?
C41 C40 C34 120.0(8) . . ?
C98 C97 C96 111.7(8) . . ?
C38 C37 C36 118.8(9) . . ?
C55 C56 C57 120.6(9) . . ?
N60 C59 C55 123.1(10) . . ?
N84 C85 C91 124.1(8) . . ?
N94 C95 C100 109.6(8) . . ?
N94 C95 C96 107.8(7) . . ?
C96 C95 C100 109.7(7) . . ?
C20 C21 C25 118.7(8) . . ?
C22 C21 C25 122.1(8) . . ?
C22 C21 C20 119.2(8) . . ?
C53 C58 C57 120.2(9) . . ?
C87 C88 C89 119.9(8) . . ?
C13 C12 C11 110.7(8) . . ?
C6 C5 C4 120.7(9) . . ?
N77 C78 C79 109.1(7) . . ?
N77 C78 C83 107.7(7) . . ?
C79 C78 C83 110.3(8) . . ?
C28 C29 C30 111.6(8) . . ?
N16 C11 C10 111.0(7) . . ?
N16 C11 C12 109.0(7) . . ?
C10 C11 C12 109.7(7) . . ?
C36 C41 C40 118.9(8) . . ?
C13 C14 C15 111.5(8) . . ?
C27 C32 C31 110.6(8) . . ?
C82 C81 C80 110.4(8) . . ?
C7 C2 Br1 119.2(7) . . ?
C7 C2 C3 122.1(9) . . ?
C3 C2 Br1 118.7(8) . . ?
N50 C51 C6 122.1(9) . . ?
N50 C45 C44 108.9(7) . . ?
N50 C45 C46 108.3(7) . . ?
C44 C45 C46 109.9(7) . . ?
C23 C22 C21 120.7(8) . . ?
C71 C72 C76 120.1(8) . . ?
C73 C72 C76 119.9(8) . . ?
C73 C72 C71 119.8(9) . . ?
N43 C42 C38 121.3(9) . . ?
C53 C54 C55 119.0(9) . . ?
C37 C36 Br35 118.0(7) . . ?
C41 C36 Br35 119.8(7) . . ?
C41 C36 C37 122.1(8) . . ?
C81 C82 C83 111.3(8) . . ?
C47 C46 C45 112.2(8) . . ?
C30 C31 C32 110.4(8) . . ?
C81 C80 C79 112.0(8) . . ?
N67 C62 C61 108.8(8) . . ?
N67 C62 C63 108.7(9) . . ?
C61 C62 C63 110.1(8) . . ?
C2 C7 C6 119.1(9) . . ?
C5 C6 C51 119.9(9) . . ?
C5 C6 C7 119.4(9) . . ?
C7 C6 C51 120.7(9) . . ?
C31 C30 C29 110.7(8) . . ?
N60 C61 C62 108.6(8) . . ?
N60 C61 C66 108.8(9) . . ?
C66 C61 C62 111.2(8) . . ?
C48 C49 C44 110.8(8) . . ?
C72 C73 C74 120.5(8) . . ?
C46 C47 C48 111.6(9) . . ?
C2 C3 C4 119.1(9) . . ?
C47 C48 C49 110.7(9) . . ?
C63 C64 C65 110.2(10) . . ?
C64 C63 C62 112.3(10) . . ?
C61 C66 C65 111.5(10) . . ?
C66 C65 C64 110.8(10) . . ?
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 1.900(9) . ?
Br86 C87 1.889(9) . ?
Br35 C36 1.898(9) . ?
Br1 C2 1.896(9) . ?
Br69 C70 1.892(9) . ?
Br52 C53 1.899(10) . ?
N9 C8 1.266(13) . ?
N9 C10 1.449(12) . ?
N101 C102 1.260(13) . ?
N101 C96 1.452(11) . ?
N26 C25 1.273(12) . ?
N26 C27 1.466(11) . ?
N94 C93 1.267(12) . ?
N94 C95 1.468(12) . ?
N50 C51 1.262(12) . ?
N50 C45 1.459(12) . ?
N77 C76 1.264(12) . ?
N77 C78 1.458(12) . ?
N43 C44 1.464(11) . ?
N43 C42 1.266(13) . ?
N16 C17 1.257(11) . ?
N16 C11 1.468(11) . ?
N67 C68 1.269(13) . ?
N67 C62 1.463(13) . ?
N60 C59 1.263(12) . ?
N60 C61 1.471(12) . ?
C102 C57 1.478(13) . ?
N84 C79 1.455(11) . ?
N84 C85 1.262(13) . ?
N33 C28 1.458(12) . ?
N33 C34 1.264(12) . ?
C17 C23 1.482(12) . ?
C8 C4 1.478(13) . ?
C57 C56 1.400(13) . ?
C57 C58 1.389(14) . ?
C28 C27 1.534(13) . ?
C28 C29 1.527(12) . ?
C91 C90 1.391(13) . ?
C91 C92 1.402(13) . ?
C91 C85 1.473(13) . ?
C24 C23 1.407(13) . ?
C24 C19 1.382(13) . ?
C87 C92 1.379(13) . ?
C87 C88 1.371(13) . ?
C90 C89 1.395(13) . ?
C76 C72 1.472(13) . ?
C93 C89 1.488(13) . ?
C25 C21 1.470(11) . ?
C68 C74 1.478(13) . ?
C23 C22 1.391(12) . ?
C19 C20 1.378(13) . ?
C20 C21 1.404(13) . ?
C44 C45 1.526(13) . ?
C44 C49 1.526(13) . ?
C39 C38 1.394(14) . ?
C39 C40 1.395(13) . ?
C4 C5 1.397(13) . ?
C4 C3 1.392(14) . ?
C10 C15 1.538(13) . ?
C10 C11 1.523(12) . ?
C34 C40 1.469(13) . ?
C71 C70 1.375(13) . ?
C71 C72 1.412(13) . ?
C55 C56 1.393(13) . ?
C55 C59 1.472(13) . ?
C55 C54 1.403(15) . ?
C98 C99 1.524(15) . ?
C98 C97 1.532(14) . ?
C13 C12 1.532(14) . ?
C13 C14 1.516(15) . ?
C15 C14 1.533(15) . ?
C100 C99 1.519(14) . ?
C100 C95 1.536(13) . ?
C75 C70 1.394(13) . ?
C75 C74 1.391(14) . ?
C96 C97 1.537(12) . ?
C96 C95 1.530(13) . ?
C79 C78 1.532(12) . ?
C79 C80 1.535(13) . ?
C27 C32 1.522(13) . ?
C38 C37 1.388(14) . ?
C38 C42 1.480(12) . ?
C53 C58 1.385(13) . ?
C53 C54 1.373(14) . ?
C74 C73 1.400(14) . ?
C89 C88 1.399(13) . ?
C83 C78 1.540(12) . ?
C83 C82 1.536(14) . ?
C40 C41 1.403(13) . ?
C37 C36 1.394(13) . ?
C21 C22 1.396(12) . ?
C12 C11 1.544(13) . ?
C5 C6 1.388(13) . ?
C29 C30 1.533(15) . ?
C41 C36 1.364(14) . ?
C32 C31 1.523(12) . ?
C81 C82 1.517(15) . ?
C81 C80 1.528(13) . ?
C2 C7 1.371(14) . ?
C2 C3 1.387(14) . ?
C51 C6 1.473(13) . ?
C45 C46 1.530(12) . ?
C72 C73 1.383(13) . ?
C46 C47 1.518(15) . ?
C31 C30 1.518(16) . ?
C62 C61 1.528(13) . ?
C62 C63 1.535(14) . ?
C7 C6 1.406(14) . ?
C61 C66 1.522(14) . ?
C49 C48 1.523(14) . ?
C47 C48 1.521(18) . ?
C64 C63 1.522(16) . ?
C64 C65 1.527(16) . ?
C66 C65 1.524(15) . ?
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
7.4634 24.9145 -0.6523 -0.2244 -0.2881 0.9309
-10.0884 10.6055 16.6665 0.5244 0.6723 0.5225
-9.1744 -23.6228 3.2983 0.3109 0.3989 -0.8627
7.9828 -15.1256 -15.5882 -0.4486 -0.5750 -0.6842
2.2278 25.7310 5.2303 0.0256 -0.0194 0.9995
15.4504 -4.4571 12.8699 -0.7835 0.6111 0.1130
-15.3989 5.5008 -12.6915 0.7864 -0.6133 -0.0732
