#------------------------------------------------------------------------------
#$Date: 2020-08-06 15:50:10 +0300 (Thu, 06 Aug 2020) $
#$Revision: 254872 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/58/7125899.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_7125899
loop_
_publ_author_name
'Marczenko, Katherine M.'
'Chitnis, Saurabh S.'
_publ_section_title
;
 Bismuthanylstibanes.
;
_journal_issue                   58
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8015
_journal_page_last               8018
_journal_paper_doi               10.1039/d0cc00254b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C44 H72 Bi N4 Sb Si4'
_chemical_formula_sum            'C44 H72 Bi N4 Sb Si4'
_chemical_formula_weight         1100.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-29 deposited with the CCDC.	2020-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.6560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.5482(4)
_cell_length_b                   12.2644(5)
_cell_length_c                   19.2011(8)
_cell_measurement_reflns_used    4778
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      72.17
_cell_measurement_theta_min      2.80
_cell_volume                     2432.77(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      115.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'D8 Quest Photon II'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1761
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            130846
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.237
_diffrn_reflns_theta_min         4.304
_exptl_absorpt_coefficient_mu    12.609
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0435 before and 0.0381 after correction. The Ratio of minimum to maximum transmission is 0.9410. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.056
_refine_diff_density_max         3.260
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0492P)²+5.8005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4774
_reflns_number_total             4778
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc00254b2.cif
_cod_data_source_block           p21c
_cod_depositor_comments
'Adding full bibliography for 7125895--7125899.cif.'
_cod_database_code               7125899
_shelx_shelxl_version_number     2018/3
_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.
;
_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. Shared sites
{Bi01, Sb01}
3. Uiso/Uaniso restraints and constraints
Uanis(Bi01) = Uanis(Sb01)
4. Others
 Fixed Sof: Bi01(0.5) Sb01(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C009(H00A,H00B), C00D(H00D,H00E), C00E(H00F,H00G), C00J(H00N,H00O), C00M(H00T,
 H00U), C00N(H00V,H00W)
5.b Aromatic/amide H refined with riding coordinates:
 C008(H008), C00A(H00C), C00F(H00H), C00G(H00I), C00H(H00J), C00L(H00S)
5.c Idealised Me refined as rotating group:
 C00I(H00K,H00L,H00M), C00K(H00P,H00Q,H00R), C00O(H00X,H00Y,H), C00P(H00Z,HA,
 HB), C00Q(H00,HC,HD), C00R(H0AA,HE,HF)
;
_olex2_submission_special_instructions 'No special instructions were received'
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'
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_occupancy
Bi01 Bi 0.36178(2) 0.53636(2) 0.49124(2) 0.01986(9) Uani 0.5 1 d . P
Sb01 Sb 0.36178(2) 0.53636(2) 0.49124(2) 0.01986(9) Uani 0.5 1 d . P
Si02 Si 0.31781(10) 0.80810(8) 0.49908(5) 0.0214(2) Uani 1 1 d . .
Si03 Si 0.18419(12) 0.45867(8) 0.33286(6) 0.0252(3) Uani 1 1 d . .
N004 N 0.4020(3) 0.7006(2) 0.46883(16) 0.0216(6) Uani 1 1 d . .
N005 N 0.3276(3) 0.5172(3) 0.37982(16) 0.0219(6) Uani 1 1 d . .
C006 C 0.4993(4) 0.7142(3) 0.42891(18) 0.0208(7) Uani 1 1 d . .
C007 C 0.4308(4) 0.5483(3) 0.3475(2) 0.0226(8) Uani 1 1 d . .
C008 C 0.4555(4) 0.4878(3) 0.2904(2) 0.0283(8) Uani 1 1 d . .
H008 H 0.400368 0.428067 0.273738 0.034 Uiso 1 1 calc R .
C009 C 0.3918(4) 0.8503(3) 0.5922(2) 0.0289(8) Uani 1 1 d . .
H00A H 0.479408 0.879906 0.593056 0.035 Uiso 1 1 calc R .
H00B H 0.338865 0.909333 0.606942 0.035 Uiso 1 1 calc R .
C00A C 0.5846(4) 0.8010(3) 0.4455(2) 0.0278(8) Uani 1 1 d . .
H00C H 0.573370 0.849995 0.482129 0.033 Uiso 1 1 calc R .
C00B C 0.6208(4) 0.6606(3) 0.3371(2) 0.0252(8) Uani 1 1 d . .
C00C C 0.5148(4) 0.6406(3) 0.37273(18) 0.0212(7) Uani 1 1 d . .
C00D C 0.3035(4) 0.9282(3) 0.4374(2) 0.0304(9) Uani 1 1 d . .
H00D H 0.258717 0.987999 0.457262 0.037 Uiso 1 1 calc R .
H00E H 0.391556 0.954094 0.435239 0.037 Uiso 1 1 calc R .
C00E C 0.1489(4) 0.7587(4) 0.4981(2) 0.0301(9) Uani 1 1 d . .
H00F H 0.111175 0.729940 0.450216 0.036 Uiso 1 1 calc R .
H00G H 0.152457 0.698194 0.532521 0.036 Uiso 1 1 calc R .
C00F C 0.6868(4) 0.8189(3) 0.4099(2) 0.0311(9) Uani 1 1 d . .
H00H H 0.742735 0.879681 0.422316 0.037 Uiso 1 1 calc R .
C00G C 0.5578(5) 0.5111(4) 0.2565(2) 0.0331(9) Uani 1 1 d . .
H00I H 0.570092 0.468332 0.217177 0.040 Uiso 1 1 calc R .
C00H C 0.7057(4) 0.7498(4) 0.3581(2) 0.0313(9) Uani 1 1 d . .
H00J H 0.776760 0.761107 0.335487 0.038 Uiso 1 1 calc R .
C00I C 0.2302(5) 0.9038(4) 0.3617(2) 0.0396(11) Uani 1 1 d . .
H00K H 0.223331 0.970623 0.333149 0.059 Uiso 1 1 calc GR .
H00L H 0.143246 0.877038 0.363206 0.059 Uiso 1 1 calc GR .
H00M H 0.277002 0.848232 0.340247 0.059 Uiso 1 1 calc GR .
C00J C 0.1969(5) 0.3075(3) 0.3209(2) 0.0344(9) Uani 1 1 d . .
H00N H 0.111272 0.278970 0.297138 0.041 Uiso 1 1 calc R .
H00O H 0.258468 0.293036 0.289263 0.041 Uiso 1 1 calc R .
C00K C 0.4018(5) 0.7572(4) 0.6451(2) 0.0429(12) Uani 1 1 d . .
H00P H 0.447109 0.695702 0.628448 0.064 Uiso 1 1 calc GR .
H00Q H 0.314804 0.734227 0.649455 0.064 Uiso 1 1 calc GR .
H00R H 0.450130 0.781527 0.691542 0.064 Uiso 1 1 calc GR .
C00L C 0.6393(4) 0.5944(4) 0.2797(2) 0.0327(9) Uani 1 1 d . .
H00S H 0.709874 0.608645 0.257184 0.039 Uiso 1 1 calc R .
C00M C 0.0572(5) 0.4848(4) 0.3866(3) 0.0366(10) Uani 1 1 d . .
H00T H 0.085677 0.451968 0.434302 0.044 Uiso 1 1 calc R .
H00U H 0.049515 0.564467 0.393005 0.044 Uiso 1 1 calc R .
C00N C 0.1358(5) 0.5238(4) 0.2431(3) 0.0388(11) Uani 1 1 d . .
H00V H 0.196933 0.500332 0.213063 0.047 Uiso 1 1 calc R .
H00W H 0.048595 0.497317 0.220262 0.047 Uiso 1 1 calc R .
C00O C 0.2419(6) 0.2468(4) 0.3906(3) 0.0545(14) Uani 1 1 d . .
H00X H 0.246284 0.168554 0.381112 0.082 Uiso 1 1 calc GR .
H00Y H 0.180578 0.259676 0.421874 0.082 Uiso 1 1 calc GR .
H H 0.327811 0.273166 0.413776 0.082 Uiso 1 1 calc GR .
C00P C 0.0604(5) 0.8495(4) 0.5170(3) 0.0488(12) Uani 1 1 d . .
H00Z H 0.055435 0.909155 0.482612 0.073 Uiso 1 1 calc GR .
HA H 0.096028 0.876910 0.564869 0.073 Uiso 1 1 calc GR .
HB H -0.026429 0.819945 0.515475 0.073 Uiso 1 1 calc GR .
C00Q C -0.0756(5) 0.4392(5) 0.3530(3) 0.0463(12) Uani 1 1 d . .
H00 H -0.100702 0.465286 0.303935 0.069 Uiso 1 1 calc GR .
HC H -0.139435 0.463741 0.380329 0.069 Uiso 1 1 calc GR .
HD H -0.072088 0.359381 0.353303 0.069 Uiso 1 1 calc GR .
C00R C 0.1337(7) 0.6482(5) 0.2455(4) 0.0692(19) Uani 1 1 d . .
H0AA H 0.101936 0.676825 0.197462 0.104 Uiso 1 1 calc GR .
HE H 0.221447 0.675482 0.263749 0.104 Uiso 1 1 calc GR .
HF H 0.076356 0.672220 0.276773 0.104 Uiso 1 1 calc GR .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.0111 8.9310 '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_3
N004 Bi01 Bi01 94.33(9) 3_666
N005 Bi01 Bi01 92.49(10) 3_666
N005 Bi01 N004 84.27(12) .
N004 Si02 C009 112.52(17) .
N004 Si02 C00D 111.24(17) .
N004 Si02 C00E 107.30(18) .
C009 Si02 C00D 110.51(19) .
C009 Si02 C00E 108.08(19) .
C00D Si02 C00E 106.9(2) .
N005 Si03 C00J 113.12(19) .
N005 Si03 C00M 106.58(18) .
N005 Si03 C00N 110.2(2) .
C00J Si03 C00M 108.3(2) .
C00N Si03 C00J 108.7(2) .
C00N Si03 C00M 109.9(2) .
Si02 N004 Bi01 120.78(16) .
C006 N004 Bi01 114.8(2) .
C006 N004 Si02 124.4(2) .
Si03 N005 Bi01 121.37(18) .
C007 N005 Bi01 115.3(2) .
C007 N005 Si03 123.2(3) .
N004 C006 C00C 122.6(3) .
C00A C006 N004 118.3(3) .
C00A C006 C00C 119.1(3) .
N005 C007 C00C 122.3(3) .
C008 C007 N005 119.1(4) .
C008 C007 C00C 118.6(4) .
C007 C008 H008 118.6 .
C007 C008 C00G 122.9(4) .
C00G C008 H008 118.6 .
Si02 C009 H00A 109.0 .
Si02 C009 H00B 109.0 .
H00A C009 H00B 107.8 .
C00K C009 Si02 113.0(3) .
C00K C009 H00A 109.0 .
C00K C009 H00B 109.0 .
C006 C00A H00C 118.9 .
C006 C00A C00F 122.2(4) .
C00F C00A H00C 118.9 .
C00H C00B C00C 120.0(4) .
C00L C00B C00C 120.9(4) .
C00L C00B C00H 119.1(4) .
C006 C00C C007 125.6(3) .
C006 C00C C00B 117.6(3) .
C00B C00C C007 116.7(3) .
Si02 C00D H00D 108.8 .
Si02 C00D H00E 108.8 .
H00D C00D H00E 107.6 .
C00I C00D Si02 114.0(3) .
C00I C00D H00D 108.8 .
C00I C00D H00E 108.8 .
Si02 C00E H00F 109.1 .
Si02 C00E H00G 109.1 .
H00F C00E H00G 107.8 .
C00P C00E Si02 112.5(3) .
C00P C00E H00F 109.1 .
C00P C00E H00G 109.1 .
C00A C00F H00H 120.0 .
C00H C00F C00A 120.1(4) .
C00H C00F H00H 120.0 .
C008 C00G H00I 120.0 .
C00L C00G C008 120.0(4) .
C00L C00G H00I 120.0 .
C00B C00H H00J 119.5 .
C00F C00H C00B 121.0(4) .
C00F C00H H00J 119.5 .
C00D C00I H00K 109.5 .
C00D C00I H00L 109.5 .
C00D C00I H00M 109.5 .
H00K C00I H00L 109.5 .
H00K C00I H00M 109.5 .
H00L C00I H00M 109.5 .
Si03 C00J H00N 109.0 .
Si03 C00J H00O 109.0 .
H00N C00J H00O 107.8 .
C00O C00J Si03 113.1(3) .
C00O C00J H00N 109.0 .
C00O C00J H00O 109.0 .
C009 C00K H00P 109.5 .
C009 C00K H00Q 109.5 .
C009 C00K H00R 109.5 .
H00P C00K H00Q 109.5 .
H00P C00K H00R 109.5 .
H00Q C00K H00R 109.5 .
C00B C00L H00S 119.6 .
C00G C00L C00B 120.8(4) .
C00G C00L H00S 119.6 .
Si03 C00M H00T 108.8 .
Si03 C00M H00U 108.8 .
H00T C00M H00U 107.7 .
C00Q C00M Si03 113.7(3) .
C00Q C00M H00T 108.8 .
C00Q C00M H00U 108.8 .
Si03 C00N H00V 108.8 .
Si03 C00N H00W 108.8 .
H00V C00N H00W 107.7 .
C00R C00N Si03 113.6(4) .
C00R C00N H00V 108.8 .
C00R C00N H00W 108.8 .
C00J C00O H00X 109.5 .
C00J C00O H00Y 109.5 .
C00J C00O H 109.5 .
H00X C00O H00Y 109.5 .
H00X C00O H 109.5 .
H00Y C00O H 109.5 .
C00E C00P H00Z 109.5 .
C00E C00P HA 109.5 .
C00E C00P HB 109.5 .
H00Z C00P HA 109.5 .
H00Z C00P HB 109.5 .
HA C00P HB 109.5 .
C00M C00Q H00 109.5 .
C00M C00Q HC 109.5 .
C00M C00Q HD 109.5 .
H00 C00Q HC 109.5 .
H00 C00Q HD 109.5 .
HC C00Q HD 109.5 .
C00N C00R H0AA 109.5 .
C00N C00R HE 109.5 .
C00N C00R HF 109.5 .
H0AA C00R HE 109.5 .
H0AA C00R HF 109.5 .
HE C00R HF 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Bi01 Bi01 3.0024(3) 3_666
Bi01 N004 2.121(3) .
Bi01 N005 2.110(3) .
Si02 N004 1.752(3) .
Si02 C009 1.873(4) .
Si02 C00D 1.877(4) .
Si02 C00E 1.878(4) .
Si03 N005 1.751(4) .
Si03 C00J 1.876(4) .
Si03 C00M 1.876(5) .
Si03 C00N 1.875(5) .
N004 C006 1.410(5) .
N005 C007 1.410(5) .
C006 C00A 1.389(6) .
C006 C00C 1.440(5) .
C007 C008 1.390(6) .
C007 C00C 1.458(6) .
C008 H008 0.9500 .
C008 C00G 1.398(6) .
C009 H00A 0.9900 .
C009 H00B 0.9900 .
C009 C00K 1.518(6) .
C00A H00C 0.9500 .
C00A C00F 1.406(6) .
C00B C00C 1.445(5) .
C00B C00H 1.420(6) .
C00B C00L 1.413(6) .
C00D H00D 0.9900 .
C00D H00E 0.9900 .
C00D C00I 1.532(6) .
C00E H00F 0.9900 .
C00E H00G 0.9900 .
C00E C00P 1.542(6) .
C00F H00H 0.9500 .
C00F C00H 1.352(6) .
C00G H00I 0.9500 .
C00G C00L 1.351(7) .
C00H H00J 0.9500 .
C00I H00K 0.9800 .
C00I H00L 0.9800 .
C00I H00M 0.9800 .
C00J H00N 0.9900 .
C00J H00O 0.9900 .
C00J C00O 1.522(7) .
C00K H00P 0.9800 .
C00K H00Q 0.9800 .
C00K H00R 0.9800 .
C00L H00S 0.9500 .
C00M H00T 0.9900 .
C00M H00U 0.9900 .
C00M C00Q 1.525(7) .
C00N H00V 0.9900 .
C00N H00W 0.9900 .
C00N C00R 1.527(8) .
C00O H00X 0.9800 .
C00O H00Y 0.9800 .
C00O H 0.9800 .
C00P H00Z 0.9800 .
C00P HA 0.9800 .
C00P HB 0.9800 .
C00Q H00 0.9800 .
C00Q HC 0.9800 .
C00Q HD 0.9800 .
C00R H0AA 0.9800 .
C00R HE 0.9800 .
C00R HF 0.9800 .
