# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PhaseIV
_database_code_depnum_ccdc_archive 'CCDC 1976838'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2020-01-10 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT987_PhaseIV             
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: the compound was refined as two component twin using hklf 5
;
# Added during the CSD deposition process: Friday 10 January 2020 02:53 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H25 Br11 N10 Sb2'
_chemical_formula_weight         1347.86

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'
N N 0.0061 0.0033 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   16.2118(7)
_cell_length_b                   14.1972(4)
_cell_length_c                   14.9780(9)
_cell_angle_alpha                90
_cell_angle_beta                 112.787(5)
_cell_angle_gamma                90
_cell_volume                     3178.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    99.9(6)
_cell_measurement_reflns_used    5953
_cell_measurement_theta_min      3.2410
_cell_measurement_theta_max      28.9830

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.817
_exptl_crystal_F_000             2448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    15.544
_exptl_absorpt_correction_T_min  0.71035
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.679
_oxdiff_exptl_absorpt_empirical_full_max 1.595
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      99.9(6)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            10037
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.364
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.584
_diffrn_reflns_point_group_measured_fraction_full 0.584
_reflns_number_total             10037
_reflns_number_gt                7613
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.122
_reflns_Friedel_fraction_max     0.133
_reflns_Friedel_fraction_full    0.132

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1300P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.50(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10037
_refine_ls_number_parameters     488
_refine_ls_number_restraints     201
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0660
_refine_ls_wR_factor_ref         0.1931
_refine_ls_wR_factor_gt          0.1843
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Sb1 Sb 0.17512(17) 0.6708(2) 0.56691(18) 0.0164(6) Uani 1 1 d . . . . .
Br1 Br 0.2533(3) 0.5071(3) 0.5078(3) 0.0246(10) Uani 1 1 d . . . . .
Br2 Br 0.3377(3) 0.7496(3) 0.6378(3) 0.0239(10) Uani 1 1 d . . . . .
Br3 Br 0.2256(3) 0.5605(3) 0.7561(3) 0.0234(10) Uani 1 1 d . . . . .
Br4 Br 0.1087(3) 0.8083(3) 0.6426(3) 0.0227(10) Uani 1 1 d . . . . .
Br5 Br -0.0017(3) 0.5819(3) 0.4832(3) 0.0310(11) Uani 1 1 d . . . . .
Br6 Br 0.1341(3) 0.7601(3) 0.4021(3) 0.0254(10) Uani 1 1 d . . . . .
Sb2 Sb 0.33406(17) 0.33797(19) 0.43811(18) 0.0156(6) Uani 1 1 d . . . . .
Br7 Br 0.1839(3) 0.2385(3) 0.4098(3) 0.0247(10) Uani 1 1 d . . . . .
Br8 Br 0.2587(3) 0.4138(3) 0.2316(3) 0.0187(9) Uani 1 1 d . . . . .
Br9 Br 0.4095(3) 0.2022(3) 0.3817(3) 0.0213(9) Uani 1 1 d . . . . .
Br10 Br 0.4888(2) 0.4574(3) 0.4706(3) 0.0211(9) Uani 1 1 d . . . . .
Br11 Br 0.4090(3) 0.2809(3) 0.6183(3) 0.0196(9) Uani 1 1 d . . . . .
Sb1A Sb 0.17104(17) 0.8414(2) 0.07319(18) 0.0152(6) Uani 1 1 d . . . . .
Br1A Br 0.2298(3) 1.0121(3) -0.0041(3) 0.0191(9) Uani 1 1 d . . . . .
Br2A Br 0.3386(3) 0.7647(3) 0.1316(3) 0.0224(10) Uani 1 1 d . . . . .
Br3A Br 0.2341(3) 0.9481(3) 0.2605(3) 0.0249(10) Uani 1 1 d . . . . .
Br4A Br 0.1157(3) 0.6975(3) 0.1492(3) 0.0238(10) Uani 1 1 d . . . . .
Br5A Br -0.0020(3) 0.9216(3) 0.0154(3) 0.0253(10) Uani 1 1 d . . . . .
Br6A Br 0.1207(3) 0.7559(3) -0.0960(3) 0.0226(10) Uani 1 1 d . . . . .
Sb2A Sb 0.33048(16) 1.17622(19) -0.05558(18) 0.0139(6) Uani 1 1 d . . . . .
Br7A Br 0.1861(3) 1.2830(3) -0.0994(3) 0.0244(10) Uani 1 1 d . . . . .
Br8A Br 0.2682(3) 1.0940(3) -0.2579(3) 0.0188(9) Uani 1 1 d . . . . .
Br9A Br 0.4185(3) 1.2966(3) -0.1158(3) 0.0198(9) Uani 1 1 d . . . . .
Br13 Br 0.4835(2) 1.0396(3) 0.0022(3) 0.0203(9) Uani 1 1 d . . . . .
Br14 Br 0.4023(3) 1.2430(3) 0.1225(3) 0.0207(9) Uani 1 1 d . . . . .
N1 N 0.376(2) 0.7751(17) 0.401(2) 0.018(5) Uani 1 1 d D U . . .
H1A H 0.341392 0.806342 0.352137 0.022 Uiso 1 1 calc R U . . .
H1B H 0.414683 0.804371 0.450225 0.022 Uiso 1 1 calc R U . . .
C1 C 0.371(2) 0.6836(17) 0.402(2) 0.011(7) Uani 1 1 d D U . . .
H1 H 0.410130 0.652043 0.456912 0.014 Uiso 1 1 calc R U . . .
N2 N 0.3158(17) 0.634(2) 0.3324(18) 0.018(5) Uani 1 1 d D U . . .
H2A H 0.279074 0.660701 0.281082 0.022 Uiso 1 1 calc R U . . .
H2B H 0.315699 0.573190 0.337352 0.022 Uiso 1 1 calc R U . . .
N3 N 0.453(2) -0.055(2) 0.757(2) 0.041(9) Uani 1 1 d D U . . .
H3A H 0.408063 -0.037286 0.768772 0.049 Uiso 1 1 calc R U . . .
H3B H 0.459450 -0.113231 0.744718 0.049 Uiso 1 1 calc R U . . .
C2 C 0.513(2) 0.006(2) 0.756(3) 0.028(9) Uani 1 1 d D U . . .
H2 H 0.561829 -0.011662 0.742747 0.034 Uiso 1 1 calc R U . . .
N4 N 0.501(2) 0.094(2) 0.774(2) 0.030(8) Uani 1 1 d D U . . .
H4A H 0.455258 0.109978 0.786115 0.036 Uiso 1 1 calc R U . . .
H4B H 0.539360 0.136008 0.774064 0.036 Uiso 1 1 calc R U . . .
N5 N 0.4214(18) -0.008(3) 0.212(2) 0.042(10) Uani 1 1 d D U . . .
H5A H 0.410670 -0.007002 0.150628 0.051 Uiso 1 1 calc R U . . .
H5B H 0.378527 -0.018317 0.230675 0.051 Uiso 1 1 calc R U . . .
C3 C 0.5019(16) 0.004(3) 0.274(2) 0.021(8) Uani 1 1 d D U . . .
H3 H 0.509758 0.001874 0.339034 0.025 Uiso 1 1 calc R U . . .
N6 N 0.573(2) 0.020(3) 0.257(3) 0.038(9) Uani 1 1 d D U . . .
H6A H 0.569119 0.022379 0.197760 0.046 Uiso 1 1 calc R U . . .
H6B H 0.623804 0.027160 0.303702 0.046 Uiso 1 1 calc R U . . .
N7 N 0.6696(19) -0.036(2) -0.028(2) 0.024(8) Uani 1 1 d D U . . .
H7A H 0.684557 -0.086000 -0.050306 0.029 Uiso 1 1 calc R U . . .
H7B H 0.619103 -0.033624 -0.021537 0.029 Uiso 1 1 calc R U . . .
C4 C 0.7230(18) 0.036(2) -0.004(2) 0.012(8) Uani 1 1 d D U . . .
H4 H 0.704082 0.088512 0.020180 0.014 Uiso 1 1 calc R U . . .
N8 N 0.8005(18) 0.041(3) -0.010(2) 0.030(9) Uani 1 1 d D U . . .
H8A H 0.820386 -0.006220 -0.031631 0.037 Uiso 1 1 calc R U . . .
H8B H 0.831958 0.091420 0.007738 0.037 Uiso 1 1 calc R U . . .
N9 N -0.0652(17) 0.539(2) 0.240(2) 0.022(7) Uani 1 1 d D U . . .
H9A H -0.058608 0.554067 0.297528 0.027 Uiso 1 1 calc R U . . .
H9B H -0.115430 0.548900 0.192152 0.027 Uiso 1 1 calc R U . . .
C5 C 0.0005(18) 0.501(3) 0.224(2) 0.031(10) Uani 1 1 d D U . . .
H5 H -0.008896 0.484998 0.160190 0.038 Uiso 1 1 calc R U . . .
N10 N 0.079(2) 0.483(3) 0.291(2) 0.049(11) Uani 1 1 d D U . . .
H10A H 0.089669 0.496273 0.350187 0.059 Uiso 1 1 calc R U . . .
H10B H 0.119819 0.457169 0.275584 0.059 Uiso 1 1 calc R U . . .
N11 N 0.1909(17) 0.978(2) 0.5127(19) 0.019(7) Uani 1 1 d D U . . .
H11A H 0.169185 1.027734 0.528927 0.023 Uiso 1 1 calc R U . . .
H11B H 0.160328 0.927170 0.498270 0.023 Uiso 1 1 calc R U . . .
C6 C 0.2705(19) 0.981(2) 0.510(3) 0.021(9) Uani 1 1 d D U . . .
H6 H 0.291016 0.926282 0.492106 0.025 Uiso 1 1 calc R U . . .
N12 N 0.324(2) 1.054(2) 0.530(2) 0.027(8) Uani 1 1 d D U . . .
H12A H 0.307648 1.106156 0.546905 0.032 Uiso 1 1 calc R U . . .
H12B H 0.375259 1.049014 0.526212 0.032 Uiso 1 1 calc R U . . .
N13 N 0.030(3) 0.459(3) 0.770(3) 0.064(13) Uani 1 1 d D U . . .
H13A H 0.085098 0.468053 0.780588 0.077 Uiso 1 1 calc R U . . .
H13B H 0.012323 0.404496 0.781499 0.077 Uiso 1 1 calc R U . . .
C7 C -0.028(4) 0.527(3) 0.736(4) 0.08(2) Uani 1 1 d D U . . .
H7 H -0.088015 0.517398 0.724570 0.097 Uiso 1 1 calc R U . . .
N14 N 0.001(3) 0.607(3) 0.720(3) 0.063(12) Uani 1 1 d D U . . .
H14A H 0.056378 0.615112 0.731001 0.075 Uiso 1 1 calc R U . . .
H14B H -0.036245 0.653415 0.697575 0.075 Uiso 1 1 calc R U . . .
N15 N 0.923(2) 0.651(2) 0.946(2) 0.028(5) Uani 1 1 d D U . . .
H15A H 0.912764 0.591047 0.945382 0.034 Uiso 1 1 calc R U . . .
H15B H 0.973387 0.673075 0.984414 0.034 Uiso 1 1 calc R U . . .
C8 C 0.862(2) 0.706(2) 0.888(2) 0.028(5) Uani 1 1 d D U . . .
H8 H 0.873881 0.770480 0.888504 0.034 Uiso 1 1 calc R U . . .
N16 N 0.7861(19) 0.674(3) 0.829(2) 0.028(5) Uani 1 1 d D U . . .
H16A H 0.774857 0.614849 0.827717 0.034 Uiso 1 1 calc R U . . .
H16B H 0.746667 0.711995 0.791002 0.034 Uiso 1 1 calc R U . . .
N17 N -0.218(2) -0.168(3) 0.325(2) 0.032(8) Uani 1 1 d D U . . .
H17A H -0.227533 -0.108445 0.315193 0.039 Uiso 1 1 calc R U . . .
H17B H -0.259343 -0.207551 0.294243 0.039 Uiso 1 1 calc R U . . .
C9 C -0.141(2) -0.198(3) 0.386(3) 0.034(10) Uani 1 1 d D U . . .
H9 H -0.132607 -0.262141 0.394762 0.041 Uiso 1 1 calc R U . . .
N18 N -0.0760(19) -0.142(2) 0.434(2) 0.026(8) Uani 1 1 d D U . . .
H18A H -0.082673 -0.081542 0.426699 0.031 Uiso 1 1 calc R U . . .
H18B H -0.026171 -0.164385 0.473732 0.031 Uiso 1 1 calc R U . . .
N19 N 0.372(2) 0.7254(19) 0.893(2) 0.030(8) Uani 1 1 d D U . . .
H19A H 0.333009 0.696040 0.845633 0.036 Uiso 1 1 calc R U . . .
H19B H 0.418008 0.695670 0.933187 0.036 Uiso 1 1 calc R U . . .
C10 C 0.363(2) 0.8149(19) 0.906(2) 0.018(9) Uani 1 1 d D U . . .
H10 H 0.406835 0.843636 0.958468 0.022 Uiso 1 1 calc R U . . .
N20 N 0.2971(16) 0.868(2) 0.8514(19) 0.018(7) Uani 1 1 d D U . . .
H20A H 0.254817 0.844169 0.801846 0.022 Uiso 1 1 calc R U . . .
H20B H 0.296052 0.926603 0.864869 0.022 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Sb1 Br6 2.621(5) . ?
Sb1 Br2 2.676(5) . ?
Sb1 Br4 2.683(5) . ?
Sb1 Br5 2.932(5) . ?
Sb1 Br1 2.943(5) . ?
Sb1 Br3 3.059(5) . ?
Br1 Sb2 3.103(5) . ?
Sb2 Br9 2.594(5) . ?
Sb2 Br11 2.622(4) . ?
Sb2 Br7 2.702(5) . ?
Sb2 Br10 2.908(5) . ?
Sb2 Br8 3.048(5) . ?
Sb1A Br6A 2.639(5) . ?
Sb1A Br4A 2.658(5) . ?
Sb1A Br2A 2.737(5) . ?
Sb1A Br5A 2.835(5) . ?
Sb1A Br1A 2.995(5) . ?
Sb1A Br3A 2.999(5) . ?
Br1A Sb2A 3.109(5) . ?
Sb2A Br9A 2.601(5) . ?
Sb2A Br14 2.638(4) . ?
Sb2A Br7A 2.650(5) . ?
Sb2A Br13 3.000(5) . ?
Sb2A Br8A 3.033(5) . ?
N1 C1 1.302(13) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
C1 N2 1.298(12) . ?
C1 H1 0.9300 . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N3 C2 1.300(13) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
C2 N4 1.301(13) . ?
C2 H2 0.9300 . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N5 C3 1.291(13) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
C3 N6 1.295(13) . ?
C3 H3 0.9300 . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
N7 C4 1.296(13) . ?
N7 H7A 0.8600 . ?
N7 H7B 0.8600 . ?
C4 N8 1.297(13) . ?
C4 H4 0.9300 . ?
N8 H8A 0.8600 . ?
N8 H8B 0.8600 . ?
N9 C5 1.297(13) . ?
N9 H9A 0.8600 . ?
N9 H9B 0.8600 . ?
C5 N10 1.304(13) . ?
C5 H5 0.9300 . ?
N10 H10A 0.8600 . ?
N10 H10B 0.8600 . ?
N11 C6 1.306(13) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
C6 N12 1.300(13) . ?
C6 H6 0.9300 . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
N13 C7 1.299(13) . ?
N13 H13A 0.8600 . ?
N13 H13B 0.8600 . ?
C7 N14 1.297(13) . ?
C7 H7 0.9300 . ?
N14 H14A 0.8600 . ?
N14 H14B 0.8600 . ?
N15 C8 1.299(13) . ?
N15 H15A 0.8600 . ?
N15 H15B 0.8600 . ?
C8 N16 1.290(13) . ?
C8 H8 0.9300 . ?
N16 H16A 0.8600 . ?
N16 H16B 0.8600 . ?
N17 C9 1.292(13) . ?
N17 H17A 0.8600 . ?
N17 H17B 0.8600 . ?
C9 N18 1.299(13) . ?
C9 H9 0.9300 . ?
N18 H18A 0.8600 . ?
N18 H18B 0.8600 . ?
N19 C10 1.302(13) . ?
N19 H19A 0.8600 . ?
N19 H19B 0.8600 . ?
C10 N20 1.299(12) . ?
C10 H10 0.9300 . ?
N20 H20A 0.8600 . ?
N20 H20B 0.8600 . ?

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
Br6 Sb1 Br2 91.33(16) . . ?
Br6 Sb1 Br4 92.80(16) . . ?
Br2 Sb1 Br4 91.32(16) . . ?
Br6 Sb1 Br5 87.48(15) . . ?
Br2 Sb1 Br5 177.91(17) . . ?
Br4 Sb1 Br5 90.46(15) . . ?
Br6 Sb1 Br1 94.60(15) . . ?
Br2 Sb1 Br1 88.66(15) . . ?
Br4 Sb1 Br1 172.59(16) . . ?
Br5 Sb1 Br1 89.73(15) . . ?
Br6 Sb1 Br3 177.87(17) . . ?
Br2 Sb1 Br3 88.73(14) . . ?
Br4 Sb1 Br3 89.33(14) . . ?
Br5 Sb1 Br3 92.40(15) . . ?
Br1 Sb1 Br3 83.27(13) . . ?
Sb1 Br1 Sb2 177.92(17) . . ?
Br9 Sb2 Br11 90.94(15) . . ?
Br9 Sb2 Br7 94.05(16) . . ?
Br11 Sb2 Br7 91.73(15) . . ?
Br9 Sb2 Br10 90.17(14) . . ?
Br11 Sb2 Br10 88.97(13) . . ?
Br7 Sb2 Br10 175.71(17) . . ?
Br9 Sb2 Br8 89.22(14) . . ?
Br11 Sb2 Br8 175.80(17) . . ?
Br7 Sb2 Br8 92.44(14) . . ?
Br10 Sb2 Br8 86.84(13) . . ?
Br9 Sb2 Br1 176.80(17) . . ?
Br11 Sb2 Br1 88.91(14) . . ?
Br7 Sb2 Br1 89.15(14) . . ?
Br10 Sb2 Br1 86.63(14) . . ?
Br8 Sb2 Br1 90.70(13) . . ?
Br6A Sb1A Br4A 91.57(16) . . ?
Br6A Sb1A Br2A 91.34(16) . . ?
Br4A Sb1A Br2A 90.87(16) . . ?
Br6A Sb1A Br5A 89.42(15) . . ?
Br4A Sb1A Br5A 88.91(15) . . ?
Br2A Sb1A Br5A 179.22(17) . . ?
Br6A Sb1A Br1A 91.58(14) . . ?
Br4A Sb1A Br1A 176.19(17) . . ?
Br2A Sb1A Br1A 91.18(14) . . ?
Br5A Sb1A Br1A 89.00(14) . . ?
Br6A Sb1A Br3A 176.27(17) . . ?
Br4A Sb1A Br3A 92.11(15) . . ?
Br2A Sb1A Br3A 88.04(14) . . ?
Br5A Sb1A Br3A 91.22(15) . . ?
Br1A Sb1A Br3A 84.76(14) . . ?
Sb1A Br1A Sb2A 168.06(16) . . ?
Br9A Sb2A Br14 91.59(15) . . ?
Br9A Sb2A Br7A 95.10(16) . . ?
Br14 Sb2A Br7A 92.65(16) . . ?
Br9A Sb2A Br13 91.22(14) . . ?
Br14 Sb2A Br13 87.07(14) . . ?
Br7A Sb2A Br13 173.68(16) . . ?
Br9A Sb2A Br8A 85.48(13) . . ?
Br14 Sb2A Br8A 173.82(15) . . ?
Br7A Sb2A Br8A 93.03(13) . . ?
Br13 Sb2A Br8A 87.55(13) . . ?
Br9A Sb2A Br1A 171.77(16) . . ?
Br14 Sb2A Br1A 94.99(14) . . ?
Br7A Sb2A Br1A 89.54(14) . . ?
Br13 Sb2A Br1A 84.20(13) . . ?
Br8A Sb2A Br1A 87.49(12) . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
N2 C1 N1 124(3) . . ?
N2 C1 H1 117.8 . . ?
N1 C1 H1 117.8 . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C2 N3 H3A 120.0 . . ?
C2 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
N3 C2 N4 118(3) . . ?
C2 N4 H4A 120.0 . . ?
C2 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C3 N5 H5A 120.0 . . ?
C3 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
N5 C3 N6 127(3) . . ?
N5 C3 H3 116.5 . . ?
N6 C3 H3 116.5 . . ?
C3 N6 H6A 120.0 . . ?
C3 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C4 N7 H7A 120.0 . . ?
C4 N7 H7B 120.0 . . ?
H7A N7 H7B 120.0 . . ?
N7 C4 N8 126(3) . . ?
N7 C4 H4 117.1 . . ?
N8 C4 H4 117.1 . . ?
C4 N8 H8A 120.0 . . ?
C4 N8 H8B 120.0 . . ?
H8A N8 H8B 120.0 . . ?
C5 N9 H9A 120.0 . . ?
C5 N9 H9B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
N9 C5 N10 124(3) . . ?
N9 C5 H5 117.8 . . ?
N10 C5 H5 117.8 . . ?
C5 N10 H10A 120.0 . . ?
C5 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C6 N11 H11A 120.0 . . ?
C6 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
N12 C6 N11 127(3) . . ?
N12 C6 H6 116.7 . . ?
N11 C6 H6 116.7 . . ?
C6 N12 H12A 120.0 . . ?
C6 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
C7 N13 H13A 120.0 . . ?
C7 N13 H13B 120.0 . . ?
H13A N13 H13B 120.0 . . ?
N14 C7 N13 118(5) . . ?
N13 C7 H7 120.8 . . ?
C7 N14 H14A 120.0 . . ?
C7 N14 H14B 120.0 . . ?
H14A N14 H14B 120.0 . . ?
C8 N15 H15A 120.0 . . ?
C8 N15 H15B 120.0 . . ?
H15A N15 H15B 120.0 . . ?
N16 C8 N15 121(3) . . ?
N16 C8 H8 119.4 . . ?
N15 C8 H8 119.4 . . ?
C8 N16 H16A 120.0 . . ?
C8 N16 H16B 120.0 . . ?
H16A N16 H16B 120.0 . . ?
C9 N17 H17A 120.0 . . ?
C9 N17 H17B 120.0 . . ?
H17A N17 H17B 120.0 . . ?
N17 C9 N18 123(3) . . ?
N17 C9 H9 118.4 . . ?
N18 C9 H9 118.4 . . ?
C9 N18 H18A 120.0 . . ?
C9 N18 H18B 120.0 . . ?
H18A N18 H18B 120.0 . . ?
C10 N19 H19A 120.0 . . ?
C10 N19 H19B 120.0 . . ?
H19A N19 H19B 120.0 . . ?
N20 C10 N19 126(3) . . ?
N20 C10 H10 116.9 . . ?
C10 N20 H20A 120.0 . . ?
C10 N20 H20B 120.0 . . ?
H20A N20 H20B 120.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag














N1 H1A Br3A 0.86 2.67 3.47(3) 155.9 . yes
N1 H1B Br10 0.86 2.67 3.45(3) 151.1 2_656 yes
N2 H2A Br4A 0.86 2.67 3.46(3) 153.3 . yes
N2 H2B Br8 0.86 2.71 3.43(3) 142.5 . yes
N3 H3A Br8A 0.86 2.84 3.61(4) 149.5 1_546 yes
N3 H3B Br2 0.86 2.79 3.43(3) 132.6 1_545 yes
N4 H4A Br8A 0.86 2.85 3.62(3) 149.1 1_546 yes
N4 H4B Br2A 0.86 2.66 3.43(3) 149.7 2_646 yes
N9 H9A Br5 0.86 2.60 3.44(3) 166.4 . yes
N9 H9B Br1A 0.86 2.76 3.52(3) 149.2 2_545 yes
N10 H10A Br1 0.86 2.79 3.40(3) 129.3 . yes
N10 H10B Br8 0.86 2.65 3.50(4) 168.4 . yes
N11 H11A Br5 0.86 2.76 3.42(3) 135.1 2_556 yes
N11 H11B Br6 0.86 2.72 3.47(3) 145.8 . yes
N12 H12B Br10 0.86 2.54 3.33(4) 153.3 2_656 yes
N13 H13A Br3 0.86 2.77 3.57(5) 154.3 . yes
C7 H7 Br3A 0.93 2.65 3.54(5) 160.1 2_546 yes
N14 H14A Br3 0.86 2.73 3.54(4) 156.1 . yes
N14 H14B Br7 0.86 2.61 3.42(4) 157.7 2_556 yes
N15 H15A Br5A 0.86 2.75 3.46(3) 140.6 2_646 yes
N15 H15B Br4A 0.86 2.67 3.48(3) 158.0 1_656 yes
N16 H16A Br3A 0.86 2.69 3.44(4) 147.5 2_646 yes
N16 H16B Br8 0.86 2.88 3.52(4) 132.8 2_656 yes
N16 H16B Br9 0.86 2.84 3.52(3) 138.1 2_656 yes
N19 H19A Br3 0.86 2.59 3.40(3) 157.4 . yes
N19 H19B Br13 0.86 2.68 3.47(3) 152.6 2_646 yes
N20 H20A Br4 0.86 2.68 3.53(3) 167.6 . yes
N20 H20B Br1A 0.86 2.85 3.45(3) 128.5 1_556 yes
N17 H17A Br3 0.86 2.63 3.45(4) 158.9 2_546 yes
N17 H17B Br8A 0.86 2.86 3.53(4) 135.9 2_535 yes
N17 H17B Br9A 0.86 2.91 3.57(3) 135.1 2_535 yes
N18 H18A Br5 0.86 2.77 3.46(3) 139.0 2_546 yes
N18 H18B Br4 0.86 2.65 3.46(3) 156.9 1_545 yes
N5 H5B Br3A 0.86 2.59 3.44(4) 171.2 1_545 yes
C3 H3 Br10 0.93 2.91 3.82(3) 167.5 2_646 yes
N6 H6A Br13 0.86 2.72 3.52(3) 155.5 1_545 yes
N6 H6B Br1 0.86 2.77 3.57(3) 155.1 2_646 yes
N7 H7A Br14 0.86 2.80 3.45(3) 133.6 2_635 yes
N7 H7B Br13 0.86 2.58 3.39(3) 158.3 1_545 yes
N8 H8A Br5A 0.86 2.88 3.51(3) 132.2 1_645 yes
N8 H8B Br6A 0.86 2.65 3.45(4) 155.7 2_645 yes

_refine_diff_density_max         3.355
_refine_diff_density_min         -2.125
_refine_diff_density_rms         0.413

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_phaseII
_database_code_depnum_ccdc_archive 'CCDC 1976841'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2020-01-10 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT043_phaseII             
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      15.21 Check
RESPONSE: H atoms in disordered moleculaes are not identified
;
# Added during the CSD deposition process: Friday 10 January 2020 02:53 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H25 Br11 N10 Sb2'
_chemical_formula_weight         1347.86

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'
N N 0.0061 0.0033 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.5603(6)
_cell_length_b                   14.3249(12)
_cell_length_c                   13.2890(13)
_cell_angle_alpha                90
_cell_angle_beta                 93.542(7)
_cell_angle_gamma                90
_cell_volume                     1626.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    219.8(4)
_cell_measurement_reflns_used    2237
_cell_measurement_theta_min      3.1090
_cell_measurement_theta_max      23.2360

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.752
_exptl_crystal_F_000             1224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    15.188
_exptl_absorpt_correction_T_min  0.62695
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.739
_oxdiff_exptl_absorpt_empirical_full_max 1.519
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      219.8(4)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            6105
_diffrn_reflns_av_unetI/netI     0.1171
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.755
_diffrn_reflns_theta_max         29.503
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6105
_reflns_number_gt                2981
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'

_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0704P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6105
_refine_ls_number_parameters     93
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1296
_refine_ls_wR_factor_gt          0.1185
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_restrained_S_all      0.878
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.002

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
Sb1 Sb -0.01309(8) 0.65901(5) 0.65128(5) 0.0425(2) Uani 1 1 d . . . . .
Br1 Br 0.000000 0.500000 0.500000 0.0775(6) Uani 1 2 d S . P . .
Br2 Br 0.20740(15) 0.75373(10) 0.54977(11) 0.0784(4) Uani 1 1 d . . . . .
Br3 Br 0.24207(14) 0.56827(11) 0.77433(10) 0.0799(5) Uani 1 1 d . . . . .
Br4 Br -0.02359(15) 0.79014(9) 0.78741(10) 0.0763(4) Uani 1 1 d . . . . .
Br5 Br -0.23409(15) 0.55044(11) 0.75196(11) 0.0835(5) Uani 1 1 d . . . . .
Br6 Br -0.24598(15) 0.73865(10) 0.54105(11) 0.0788(5) Uani 1 1 d . . . . .
N1 N 0.5546(12) 0.4559(8) 0.9370(8) 0.095(3) Uiso 1 1 d D . . . .
C1 C 0.512(3) 0.5314(14) 0.9796(15) 0.095(3) Uiso 0.5 1 d D . P . .
C2 C 0.0260(19) 0.6763(12) 0.2952(17) 0.172(4) Uiso 1 1 d D . . . .
H2 H 0.111268 0.636782 0.307154 0.206 Uiso 1 1 calc R U . . .
N2 N 0.0336(16) 0.7640(11) 0.2733(12) 0.172(4) Uiso 1 1 d D . . . .
H2A H -0.050910 0.796062 0.263271 0.206 Uiso 1 1 calc R U . . .
H2B H 0.123161 0.790414 0.268877 0.206 Uiso 1 1 calc R U . . .
N3 N -0.1227(18) 0.6520(10) 0.2977(12) 0.172(4) Uiso 1 1 d D . . . .
H3A H -0.195178 0.692774 0.285725 0.206 Uiso 1 1 calc R U . . .
H3B H -0.146989 0.595291 0.311353 0.206 Uiso 1 1 calc R U . . .
N4 N 0.445(3) 0.5189(19) 0.5836(12) 0.123(6) Uiso 0.5 1 d D . P . .
N5 N 0.383(2) 0.5453(18) 0.523(2) 0.123(6) Uiso 0.5 1 d D . P . .
C3 C 0.500000 0.500000 0.500000 0.123(6) Uiso 1 2 d DS . P . .
C4 C 0.431(4) 1.0148(12) 0.551(3) 0.134(5) Uiso 0.5 1 d D . P . .
N6 N 0.4722(16) 0.9400(9) 0.5034(11) 0.134(5) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Sb1 Br4 2.6133(13) . ?
Sb1 Br6 2.6572(13) . ?
Sb1 Br2 2.7455(14) . ?
Sb1 Br5 2.8462(14) . ?
Sb1 Br3 2.9485(13) . ?
Sb1 Br1 3.0447(7) . ?


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
Br4 Sb1 Br6 90.93(5) . . ?
Br4 Sb1 Br2 92.23(5) . . ?
Br6 Sb1 Br2 91.84(5) . . ?
Br4 Sb1 Br5 90.86(5) . . ?
Br6 Sb1 Br5 89.77(5) . . ?
Br2 Sb1 Br5 176.49(5) . . ?
Br4 Sb1 Br3 89.36(5) . . ?
Br6 Sb1 Br3 179.12(5) . . ?
Br2 Sb1 Br3 88.98(5) . . ?
Br5 Sb1 Br3 89.40(4) . . ?
Br4 Sb1 Br1 177.51(4) . . ?
Br6 Sb1 Br1 90.81(4) . . ?
Br2 Sb1 Br1 89.48(4) . . ?
Br5 Sb1 Br1 87.38(4) . . ?
Br3 Sb1 Br1 88.86(3) . . ?
Sb1 Br1 Sb1 180.00(2) . 3_566 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2A Br3 0.86 2.64 3.464(16) 160.9 4_575 yes
N2 H2B Br5 0.86 2.60 3.342(14) 144.7 4_675 yes
N3 H3A Br4 0.86 2.82 3.525(16) 139.9 4_575 yes
N3 H3B Br3 0.86 2.71 3.434(14) 143.0 3_566 yes

_refine_diff_density_max         1.561
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.186

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PhaseIII
_database_code_depnum_ccdc_archive 'CCDC 1976839'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2020-01-10 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H25 Br11 N10 Sb2'
_chemical_formula_weight         1347.86

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'
N N 0.0061 0.0033 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.2457(12)
_cell_length_b                   14.2267(8)
_cell_length_c                   15.1237(11)
_cell_angle_alpha                90
_cell_angle_beta                 113.536(9)
_cell_angle_gamma                90
_cell_volume                     3204.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    179.7(5)
_cell_measurement_reflns_used    6460
_cell_measurement_theta_min      3.0890
_cell_measurement_theta_max      28.5480

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.794
_exptl_crystal_F_000             2448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    15.416
_exptl_absorpt_correction_T_min  0.66817
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.746
_oxdiff_exptl_absorpt_empirical_full_max 1.564
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      179.7(5)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            9778
_diffrn_reflns_av_unetI/netI     0.0971
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.701
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9778
_reflns_number_gt                5896
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component perfect twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0593P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9775
_refine_ls_number_parameters     238
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.1019
_refine_ls_wR_factor_gt          0.0946
_refine_ls_goodness_of_fit_ref   0.815
_refine_ls_restrained_S_all      0.821
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000

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
Sb1 Sb 0.17177(5) -0.16284(5) 0.81968(5) 0.02476(19) Uani 1 1 d . . . . .
Sb2 Sb 0.33222(5) 0.16540(5) 0.68772(5) 0.02387(19) Uani 1 1 d . . . . .
Br1 Br 0.23988(9) 0.00328(9) 0.74938(9) 0.0446(3) Uani 1 1 d . . . . .
Br3 Br 0.22916(8) -0.05661(9) 1.00521(8) 0.0428(3) Uani 1 1 d . . . . .
Br2 Br 0.33733(7) -0.24303(9) 0.88510(9) 0.0394(3) Uani 1 1 d . . . . .
Br4 Br 0.11071(8) -0.30198(9) 0.89367(8) 0.0411(3) Uani 1 1 d . . . . .
Br5 Br -0.00194(8) -0.07707(10) 0.75058(10) 0.0517(4) Uani 1 1 d . . . . .
Br6 Br 0.12317(9) -0.25040(9) 0.65237(8) 0.0427(4) Uani 1 1 d . . . . .
Br7 Br 0.18294(8) 0.26788(9) 0.64627(10) 0.0456(4) Uani 1 1 d . . . . .
Br8 Br 0.26337(7) 0.08626(8) 0.48656(8) 0.0342(3) Uani 1 1 d . . . . .
Br9 Br 0.41426(8) 0.29277(8) 0.63007(8) 0.0358(3) Uani 1 1 d . . . . .
Br10 Br 0.48600(8) 0.03880(8) 0.73606(8) 0.0389(3) Uani 1 1 d . . . . .
Br11 Br 0.40465(8) 0.23075(9) 0.86527(8) 0.0379(3) Uani 1 1 d . . . . .
C1 C 0.8603(8) 0.7033(8) 0.6372(9) 0.048(3) Uani 1 1 d D . . . .
H1 H 0.872624 0.767280 0.638508 0.057 Uiso 1 1 calc R U . . .
N1 N 0.7819(6) 0.6749(7) 0.5815(7) 0.051(3) Uani 1 1 d D . . . .
H1A H 0.768789 0.616166 0.579013 0.061 Uiso 1 1 calc R U . . .
H1B H 0.742343 0.714628 0.546609 0.061 Uiso 1 1 calc R U . . .
N2 N 0.9222(7) 0.6490(8) 0.6909(8) 0.074(4) Uani 1 1 d D . . . .
H2A H 0.912414 0.589545 0.690990 0.088 Uiso 1 1 calc R U . . .
H2B H 0.973772 0.671574 0.727062 0.088 Uiso 1 1 calc R U . . .
C2 C 0.3644(8) 0.6886(8) 0.1568(8) 0.046(3) Uani 1 1 d D . . . .
H2 H 0.403808 0.659150 0.212558 0.055 Uiso 1 1 calc R U . . .
N3 N 0.3752(6) 0.7778(7) 0.1487(7) 0.049(3) Uani 1 1 d D . . . .
H3A H 0.340096 0.807476 0.098145 0.058 Uiso 1 1 calc R U . . .
H3B H 0.417402 0.807347 0.193791 0.058 Uiso 1 1 calc R U . . .
N4 N 0.3041(7) 0.6373(7) 0.0945(7) 0.058(3) Uani 1 1 d D . . . .
H4A H 0.266414 0.661900 0.041965 0.069 Uiso 1 1 calc R U . . .
H4B H 0.301269 0.578232 0.105163 0.069 Uiso 1 1 calc R U . . .
C3 C 0.7278(8) 0.4723(8) 0.2452(8) 0.037(3) Uani 1 1 d D . . . .
H3 H 0.708193 0.418585 0.266093 0.044 Uiso 1 1 calc R U . . .
N5 N 0.6775(7) 0.5455(7) 0.2269(7) 0.056(3) Uani 1 1 d D . . . .
H5A H 0.693647 0.596250 0.207421 0.067 Uiso 1 1 calc R U . . .
H5B H 0.627555 0.543678 0.234011 0.067 Uiso 1 1 calc R U . . .
N6 N 0.8042(7) 0.4679(7) 0.2367(8) 0.058(3) Uani 1 1 d D . . . .
H6A H 0.824221 0.516376 0.217538 0.070 Uiso 1 1 calc R U . . .
H6B H 0.834729 0.416637 0.250168 0.070 Uiso 1 1 calc R U . . .
C4 C 0.500000 0.500000 0.000000 0.077(7) Uiso 1 2 d DS . P . .
N7 N 0.5026(12) 0.4123(10) 0.0138(13) 0.035(5) Uiso 0.5 1 d D . P . .
N8 N 0.4441(13) 0.5651(11) -0.0056(14) 0.047(6) Uiso 0.5 1 d D . P . .
N9 N 0.4193(10) 0.528(2) 0.4494(19) 0.045(5) Uiso 0.3333 1 d D . P . .
N91 N 0.4201(10) 0.506(3) 0.493(2) 0.045(5) Uiso 0.3333 1 d D . P . .
N10 N 0.5645(13) 0.480(3) 0.473(2) 0.045(5) Uiso 0.3333 1 d D . P . .
C5 C 0.500000 0.500000 0.500000 0.094(8) Uiso 1 2 d DS . P . .
N12 N 0.0013(15) 0.0863(9) 0.0226(15) 0.059(5) Uiso 0.5 1 d D . P . .
C7 C 0.000000 0.000000 0.000000 0.111(9) Uiso 1 2 d DS . P . .
N13 N 0.0596(12) 0.0594(13) 0.0304(16) 0.059(5) Uiso 0.5 1 d D . P . .
N11 N -0.0689(14) -0.023(2) 0.4218(12) 0.049(5) Uiso 0.3333 1 d D . P . .
N21 N -0.0594(15) -0.037(2) 0.5266(18) 0.049(5) Uiso 0.3333 1 d D . P . .
N31 N -0.0773(12) -0.032(2) 0.481(2) 0.049(5) Uiso 0.3333 1 d D . P . .
C6 C 0.000000 0.000000 0.500000 0.105(9) Uiso 1 2 d DS . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Sb1 Br6 2.6425(13) . ?
Sb1 Br4 2.6535(13) . ?
Sb1 Br2 2.7184(13) . ?
Sb1 Br5 2.8618(14) . ?
Sb1 Br1 2.9799(14) . ?
Sb1 Br3 2.9894(14) . ?
Sb2 Br9 2.5978(13) . ?
Sb2 Br11 2.6336(13) . ?
Sb2 Br7 2.6806(14) . ?
Sb2 Br10 2.9259(13) . ?
Sb2 Br8 3.0095(13) . ?
Sb2 Br1 3.0913(14) . ?


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
Br6 Sb1 Br4 91.89(4) . . ?
Br6 Sb1 Br2 91.41(5) . . ?
Br4 Sb1 Br2 90.89(4) . . ?
Br6 Sb1 Br5 88.70(4) . . ?
Br4 Sb1 Br5 89.53(5) . . ?
Br2 Sb1 Br5 179.56(5) . . ?
Br6 Sb1 Br1 92.51(4) . . ?
Br4 Sb1 Br1 175.36(5) . . ?
Br2 Sb1 Br1 90.48(4) . . ?
Br5 Sb1 Br1 89.09(5) . . ?
Br6 Sb1 Br3 177.51(5) . . ?
Br4 Sb1 Br3 90.59(4) . . ?
Br2 Sb1 Br3 88.75(4) . . ?
Br5 Sb1 Br3 91.13(4) . . ?
Br1 Sb1 Br3 85.00(4) . . ?
Br9 Sb2 Br11 90.90(4) . . ?
Br9 Sb2 Br7 94.57(5) . . ?
Br11 Sb2 Br7 92.33(5) . . ?
Br9 Sb2 Br10 90.68(4) . . ?
Br11 Sb2 Br10 88.47(4) . . ?
Br7 Sb2 Br10 174.68(5) . . ?
Br9 Sb2 Br8 87.42(4) . . ?
Br11 Sb2 Br8 175.69(5) . . ?
Br7 Sb2 Br8 91.76(4) . . ?
Br10 Sb2 Br8 87.59(4) . . ?
Br9 Sb2 Br1 175.93(5) . . ?
Br11 Sb2 Br1 91.66(4) . . ?
Br7 Sb2 Br1 88.49(4) . . ?
Br10 Sb2 Br1 86.22(4) . . ?
Br8 Sb2 Br1 89.80(4) . . ?
Sb1 Br1 Sb2 173.41(6) . . ?


loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag

N1 H1A Br3 0.86 2.77 3.524(11) 146.5 2_656 yes
N1 H1B Br8 0.86 2.87 3.541(10) 136.0 3_666 yes
N1 H1B Br9 0.86 2.86 3.530(10) 135.8 3_666 yes
N2 H2A Br5 0.86 2.74 3.448(11) 141.0 2_656 yes
N2 H2B Br4 0.86 2.64 3.431(11) 153.8 1_665 yes
N3 H3A Br3 0.86 2.63 3.432(10) 154.7 1_564 yes
N3 H3B Br10 0.86 2.66 3.435(9) 151.3 3_666 yes
N4 H4A Br4 0.86 2.68 3.496(10) 159.7 1_564 yes
N4 H4B Br8 0.86 2.86 3.514(10) 134.0 4_565 yes
N5 H5A Br11 0.86 2.90 3.518(11) 130.2 3_666 yes
N5 H5B Br10 0.86 2.59 3.388(11) 154.1 4_565 yes
N6 H6A Br5 0.86 2.80 3.442(10) 132.6 4_665 yes
N6 H6B Br6 0.86 2.73 3.494(10) 149.4 3_656 yes

_refine_diff_density_max         1.730
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.209

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PhaseI
_database_code_depnum_ccdc_archive 'CCDC 1976840'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2020-01-10 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT043_PhaseI              
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      25.29 Check
RESPONSE: H atoms in disordered moleculaes are not identified
;
# Added during the CSD deposition process: Friday 10 January 2020 02:53 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H25 Br11 N10 Sb2'
_chemical_formula_weight         1347.86

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'
N N 0.0061 0.0033 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_H-M_alt        'P m n n'
_space_group_name_Hall           ?

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x-1/2, -y-1/2, z-1/2'
'-x, y, z'

_cell_length_a                   8.5458(4)
_cell_length_b                   14.2043(7)
_cell_length_c                   13.6227(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1653.61(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    249.94(13)
_cell_measurement_reflns_used    1698
_cell_measurement_theta_min      4.0800
_cell_measurement_theta_max      21.1960

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.707
_exptl_crystal_F_000             1224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    14.938
_exptl_absorpt_correction_T_min  0.51901
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.731
_oxdiff_exptl_absorpt_empirical_full_max 1.722
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      249.94(13)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            6789
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.782
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1682
_reflns_number_gt                962
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1061P)²+3.3546P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1682
_refine_ls_number_parameters     62
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1908
_refine_ls_wR_factor_gt          0.1575
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Sb1 Sb 0.000000 0.35013(7) 0.16011(7) 0.0757(5) Uani 1 2 d S T P . .
Br1 Br 0.000000 0.500000 0.000000 0.1286(12) Uani 1 4 d S T P . .
Br2 Br 0.23013(19) 0.25601(12) 0.06017(13) 0.1234(7) Uani 1 1 d . . . . .
Br3 Br 0.23486(17) 0.45464(13) 0.26278(11) 0.1211(7) Uani 1 1 d . . . . .
Br4 Br 0.000000 0.22324(17) 0.29928(19) 0.1297(9) Uani 1 2 d S T P . .
C1 C 0.000000 0.000000 0.500000 0.210(13) Uiso 1 4 d DS . P . .
N2 N 0.000000 0.017(4) 0.6000(9) 0.210(13) Uiso 0.5 2 d DS . P . .
N3 N 0.1625(10) 0.000000 0.500000 0.210(13) Uiso 0.5 2 d DS . P . .
N4 N 0.531(6) 0.0845(12) 0.026(2) 0.141(10) Uiso 0.3333 1 d D . P . .
C2 C 0.500000 0.000000 0.000000 0.141(10) Uiso 1 4 d DS . P . .
N5 N 0.500000 0.0859(17) -0.033(4) 0.141(10) Uiso 0.3333 2 d DS . P . .
C3 C 0.000000 0.729(2) 0.207(5) 0.219(9) Uiso 0.78(3) 2 d DS . P . .
N6 N -0.11116(6) 0.6691(15) 0.1883(19) 0.219(9) Uiso 0.78(3) 1 d D . P . .
C4 C 0.000000 0.714(3) 0.196(13) 0.219(9) Uiso 0.22(3) 2 d DS . P . .
N7 N -0.11116(6) 0.775(3) 0.212(7) 0.219(9) Uiso 0.22(3) 1 d D . P . .
NC N 0.500000 0.5503(14) 0.4449(14) 0.208(10) Uiso 1 2 d DS . P . .
C8 C 0.500000 0.5400(15) 0.5398(15) 0.208(10) Uiso 0.5 2 d DS . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Sb1 Br4 2.616(2) . ?
Sb1 Br2 2.7402(15) . ?
Sb1 Br2 2.7402(15) 8 ?
Sb1 Br3 2.8615(15) . ?
Sb1 Br3 2.8615(15) 8 ?
Sb1 Br1 3.0478(10) . ?


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
Br4 Sb1 Br2 91.37(6) . . ?
Br4 Sb1 Br2 91.37(6) . 8 ?
Br2 Sb1 Br2 91.73(8) . 8 ?
Br4 Sb1 Br3 90.18(6) . . ?
Br2 Sb1 Br3 89.57(5) . . ?
Br2 Sb1 Br3 177.94(6) 8 . ?
Br4 Sb1 Br3 90.18(6) . 8 ?
Br2 Sb1 Br3 177.94(6) . 8 ?
Br2 Sb1 Br3 89.57(5) 8 8 ?
Br3 Sb1 Br3 89.08(7) . 8 ?
Br4 Sb1 Br1 179.25(8) . . ?
Br2 Sb1 Br1 89.15(4) . . ?
Br2 Sb1 Br1 89.15(4) 8 . ?
Br3 Sb1 Br1 89.28(4) . . ?
Br3 Sb1 Br1 89.28(4) 8 . ?
Sb1 Br1 Sb1 180.0 . 5_565 ?


_refine_diff_density_max         0.900
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.132

