#------------------------------------------------------------------------------
#$Date: 2022-04-06 01:50:27 +0300 (Wed, 06 Apr 2022) $
#$Revision: 274362 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/47/7244716.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_7244716
loop_
_publ_author_name
'Korobeynikov, Nikita A.'
'Usoltsev, Andrey N.'
'Kolesov, Boris A.'
'Abramov, Pavel A.'
'Plyusnin, Pavel E.'
'Sokolov, Maksim Nailyevich'
'Adonin, Sergey A.'
_publ_section_title
;
 Dichlorine-containing chlorobismuthate(III) supramolecular hybrid:
 structure and experimental studies of stability
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00210H
_journal_year                    2022
_chemical_formula_sum            'C12 H36 Bi2 Cl11 N3'
_chemical_formula_weight         1030.35
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-01-13 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   9.1792(3)
_cell_length_b                   9.1792(3)
_cell_length_c                   21.9776(10)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.5495
_cell_measurement_theta_min      2.5622
_cell_volume                     1603.69(10)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2016)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1101
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16530
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.661
_diffrn_reflns_theta_min         2.562
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    11.882
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.134
_exptl_crystal_description       plate
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.758
_refine_diff_density_min         -2.463
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.449
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         621
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.343
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0609
_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)+50.5902P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                615
_reflns_number_total             621
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00210h2.cif
_cod_data_source_block           NK693_pl
_cod_original_cell_volume        1603.69(13)
_cod_database_code               7244716
_shelx_shelxl_version_number     2017/1
_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_min   0.330
_shelx_estimated_absorpt_t_max   0.648
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-y, -x, -z+1/2'
'x-y, -y, -z'
'x, x-y, -z+1/2'
'y, x, -z'
'-x+y, y, -z+1/2'
'-x, -x+y, -z'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'y, x, z-1/2'
'-x+y, y, z'
'-x, -x+y, z-1/2'
'-y, -x, z'
'x-y, -y, z-1/2'
'x, x-y, 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
Bi1 Bi 0.333333 0.666667 0.16278(6) 0.0339(4) Uani 1 6 d S T P . .
Cl1 Cl 0.0519(8) 0.1038(16) 0.0260(5) 0.035(3) Uani 0.3334 2 d S T P . .
Cl3 Cl 0.0600(10) 0.5300(5) 0.250000 0.078(3) Uani 1 4 d S T P . .
Cl2A Cl 0.189(2) 0.379(5) 0.1108(15) 0.053(9) Uiso 0.2 2 d S . P . .
Cl2B Cl 0.2449(12) 0.4071(12) 0.0959(4) 0.042(2) Uiso 0.4 1 d . . P . .
N1 N -0.333333 0.333333 0.0883(9) 0.036(5) Uani 1 6 d DS T P . .
C11 C -0.184(3) 0.318(4) 0.068(3) 0.036(5) Uani 0.1667 1 d D . P A -1
H11A H -0.084261 0.395399 0.091645 0.054 Uiso 0.1667 1 calc R U P A -1
H11B H -0.207747 0.202307 0.074391 0.054 Uiso 0.1667 1 calc R U P A -1
H11C H -0.162104 0.346122 0.024632 0.054 Uiso 0.1667 1 calc R U P A -1
C12 C -0.487(4) 0.213(4) 0.052(2) 0.036(5) Uani 0.1667 1 d D . P A -1
H12A H -0.465565 0.241507 0.008231 0.054 Uiso 0.1667 1 calc R U P A -1
H12B H -0.511326 0.097758 0.058029 0.054 Uiso 0.1667 1 calc R U P A -1
H12C H -0.583793 0.223412 0.064623 0.054 Uiso 0.1667 1 calc R U P A -1
C13 C -0.367(7) 0.290(5) 0.1553(13) 0.036(5) Uani 0.1667 1 d D . P A -1
H13A H -0.267216 0.367402 0.178997 0.054 Uiso 0.1667 1 calc R U P A -1
H13B H -0.463245 0.299926 0.168409 0.054 Uiso 0.1667 1 calc R U P A -1
H13C H -0.390778 0.174271 0.161815 0.054 Uiso 0.1667 1 calc R U P A -1
C14 C -0.296(4) 0.512(3) 0.078(3) 0.036(5) Uani 0.1667 1 d D . P A -1
H14A H -0.196477 0.589843 0.101933 0.054 Uiso 0.1667 1 calc R U P A -1
H14B H -0.274252 0.540540 0.034910 0.054 Uiso 0.1667 1 calc R U P A -1
H14C H -0.392478 0.522433 0.091304 0.054 Uiso 0.1667 1 calc R U P A -1
N2 N 0.000000 0.000000 0.250000 0.038(8) Uani 1 12 d DS T P . .
C21 C -0.080(10) -0.137(7) 0.298(2) 0.038(8) Uani 0.0833 1 d D . P B -1
H21A H -0.065004 -0.231680 0.286533 0.057 Uiso 0.0833 1 calc R U P B -1
H21B H -0.025792 -0.091930 0.337357 0.057 Uiso 0.0833 1 calc R U P B -1
H21C H -0.200097 -0.174675 0.300971 0.057 Uiso 0.0833 1 calc R U P B -1
C22 C -0.023(8) 0.147(5) 0.268(3) 0.038(8) Uani 0.0833 1 d D . P B -1
H22A H -0.143140 0.109137 0.270702 0.057 Uiso 0.0833 1 calc R U P B -1
H22B H 0.031243 0.191961 0.307040 0.057 Uiso 0.0833 1 calc R U P B -1
H22C H 0.028628 0.235321 0.236660 0.057 Uiso 0.0833 1 calc R U P B -1
C23 C -0.084(9) -0.069(9) 0.1890(19) 0.038(8) Uani 0.0833 1 d D . P B -1
H23A H -0.069004 -0.164440 0.177584 0.057 Uiso 0.0833 1 calc R U P B -1
H23B H -0.204046 -0.107375 0.192033 0.057 Uiso 0.0833 1 calc R U P B -1
H23C H -0.032255 0.018813 0.158004 0.057 Uiso 0.0833 1 calc R U P B -1
C24 C 0.186(3) 0.059(8) 0.245(4) 0.038(8) Uani 0.0833 1 d D . P B -1
H24A H 0.200936 -0.036342 0.233877 0.057 Uiso 0.0833 1 calc R U P B -1
H24B H 0.237734 0.146917 0.214281 0.057 Uiso 0.0833 1 calc R U P B -1
H24C H 0.240349 0.103557 0.284661 0.057 Uiso 0.0833 1 calc R U P B -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2A Bi1 Cl2A 101.6(10) 5_565 . ?
Cl2A Bi1 Cl2A 101.6(10) 5_565 3_665 ?
Cl2A Bi1 Cl2A 101.6(10) . 3_665 ?
Cl2A Bi1 Cl2B 102.7(6) 5_565 . ?
Cl2A Bi1 Cl2B 12.3(6) . . ?
Cl2A Bi1 Cl2B 89.4(6) 3_665 . ?
Cl2A Bi1 Cl2B 12.3(6) 5_565 5_565 ?
Cl2A Bi1 Cl2B 89.4(6) . 5_565 ?
Cl2A Bi1 Cl2B 102.7(6) 3_665 5_565 ?
Cl2B Bi1 Cl2B 90.4(3) . 5_565 ?
Cl2A Bi1 Cl2B 12.3(6) 5_565 24_565 ?
Cl2A Bi1 Cl2B 102.7(6) . 24_565 ?
Cl2A Bi1 Cl2B 89.4(6) 3_665 24_565 ?
Cl2B Bi1 Cl2B 101.0(3) . 24_565 ?
Cl2B Bi1 Cl2B 17.0(4) 5_565 24_565 ?
Cl2A Bi1 Cl2B 89.4(6) 5_565 20 ?
Cl2A Bi1 Cl2B 12.3(6) . 20 ?
Cl2A Bi1 Cl2B 102.7(6) 3_665 20 ?
Cl2B Bi1 Cl2B 17.0(4) . 20 ?
Cl2B Bi1 Cl2B 77.2(5) 5_565 20 ?
Cl2B Bi1 Cl2B 90.4(3) 24_565 20 ?
Cl2A Bi1 Cl2B 89.4(6) 5_565 3_665 ?
Cl2A Bi1 Cl2B 102.7(6) . 3_665 ?
Cl2A Bi1 Cl2B 12.3(6) 3_665 3_665 ?
Cl2B Bi1 Cl2B 90.4(3) . 3_665 ?
Cl2B Bi1 Cl2B 90.4(3) 5_565 3_665 ?
Cl2B Bi1 Cl2B 77.2(5) 24_565 3_665 ?
Cl2B Bi1 Cl2B 101.0(3) 20 3_665 ?
Cl2A Bi1 Cl2B 102.7(6) 5_565 22_665 ?
Cl2A Bi1 Cl2B 89.4(6) . 22_665 ?
Cl2A Bi1 Cl2B 12.3(6) 3_665 22_665 ?
Cl2B Bi1 Cl2B 77.2(5) . 22_665 ?
Cl2B Bi1 Cl2B 101.0(3) 5_565 22_665 ?
Cl2B Bi1 Cl2B 90.4(3) 24_565 22_665 ?
Cl2B Bi1 Cl2B 90.4(3) 20 22_665 ?
Cl2B Bi1 Cl2B 17.0(4) 3_665 22_665 ?
Cl2A Bi1 Cl3 165.1(8) 5_565 3_665 ?
Cl2A Bi1 Cl3 87.7(6) . 3_665 ?
Cl2A Bi1 Cl3 87.7(6) 3_665 3_665 ?
Cl2B Bi1 Cl3 88.93(19) . 3_665 ?
Cl2B Bi1 Cl3 169.62(19) 5_565 3_665 ?
Cl2B Bi1 Cl3 169.62(19) 24_565 3_665 ?
Cl2B Bi1 Cl3 100.0(2) 20 3_665 ?
Cl2B Bi1 Cl3 100.0(2) 3_665 3_665 ?
Cl2B Bi1 Cl3 88.93(19) 22_665 3_665 ?
Cl2A Bi1 Cl3 87.7(6) 5_565 . ?
Cl2A Bi1 Cl3 87.7(6) . . ?
Cl2A Bi1 Cl3 165.1(8) 3_665 . ?
Cl2B Bi1 Cl3 100.0(2) . . ?
Cl2B Bi1 Cl3 88.93(19) 5_565 . ?
Cl2B Bi1 Cl3 100.0(2) 24_565 . ?
Cl2B Bi1 Cl3 88.93(19) 20 . ?
Cl2B Bi1 Cl3 169.62(19) 3_665 . ?
Cl2B Bi1 Cl3 169.62(19) 22_665 . ?
Cl3 Bi1 Cl3 80.99(17) 3_665 . ?
Cl2A Bi1 Cl3 87.7(6) 5_565 14_566 ?
Cl2A Bi1 Cl3 165.1(8) . 14_566 ?
Cl2A Bi1 Cl3 87.7(6) 3_665 14_566 ?
Cl2B Bi1 Cl3 169.62(19) . 14_566 ?
Cl2B Bi1 Cl3 100.0(2) 5_565 14_566 ?
Cl2B Bi1 Cl3 88.93(19) 24_565 14_566 ?
Cl2B Bi1 Cl3 169.62(19) 20 14_566 ?
Cl2B Bi1 Cl3 88.93(19) 3_665 14_566 ?
Cl2B Bi1 Cl3 100.0(2) 22_665 14_566 ?
Cl3 Bi1 Cl3 81.00(17) 3_665 14_566 ?
Cl3 Bi1 Cl3 81.00(17) . 14_566 ?
Cl1 Cl1 Cl1 60.9(12) 17 15 ?
Cl1 Cl1 Cl1 59.6(6) 17 3 ?
Cl1 Cl1 Cl1 89.996(1) 15 3 ?
Cl1 Cl1 Cl1 89.996(1) 17 5 ?
Cl1 Cl1 Cl1 59.6(6) 15 5 ?
Cl1 Cl1 Cl1 59.999(1) 3 5 ?
Cl1 Cl1 Cl1 45.4(5) 17 13 ?
Cl1 Cl1 Cl1 45.4(5) 15 13 ?
Cl1 Cl1 Cl1 44.6(5) 3 13 ?
Cl1 Cl1 Cl1 44.6(5) 5 13 ?
Bi1 Cl3 Bi1 82.8(2) 14_566 . ?
Cl2B Cl2A Cl2B 87(6) . 20 ?
Cl2B Cl2A Bi1 84(4) . . ?
Cl2B Cl2A Bi1 84(4) 20 . ?
Cl2A Cl2B Cl2B 46(3) . 20 ?
Cl2A Cl2B Bi1 84(4) . . ?
Cl2B Cl2B Bi1 81.5(2) 20 . ?
C12 N1 C13 109.5(6) . . ?
C12 N1 C14 109.5(6) . . ?
C13 N1 C14 109.4(6) . . ?
C12 N1 C11 109.5(6) . . ?
C13 N1 C11 109.5(6) . . ?
C14 N1 C11 109.4(6) . . ?
C22 N2 C24 109.5(6) . . ?
C22 N2 C21 109.5(6) . . ?
C24 N2 C21 109.5(6) . . ?
C22 N2 C23 109.5(6) . . ?
C24 N2 C23 109.5(6) . . ?
C21 N2 C23 109.4(6) . . ?
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
Bi1 Cl2A 2.56(3) 5_565 ?
Bi1 Cl2A 2.56(3) . ?
Bi1 Cl2A 2.56(3) 3_665 ?
Bi1 Cl2B 2.562(9) . ?
Bi1 Cl2B 2.562(9) 5_565 ?
Bi1 Cl2B 2.562(9) 24_565 ?
Bi1 Cl2B 2.562(9) 20 ?
Bi1 Cl2B 2.562(9) 3_665 ?
Bi1 Cl2B 2.562(9) 22_665 ?
Bi1 Cl3 2.897(6) 3_665 ?
Bi1 Cl3 2.897(6) . ?
Bi1 Cl3 2.898(6) 14_566 ?
Cl1 Cl1 1.41(2) 17 ?
Cl1 Cl1 1.41(2) 15 ?
Cl1 Cl1 1.43(2) 3 ?
Cl1 Cl1 1.43(2) 5 ?
Cl1 Cl1 2.01(2) 13 ?
Cl2A Cl2B 0.55(3) . ?
Cl2A Cl2B 0.55(3) 20 ?
Cl2B Cl2B 0.759(19) 20 ?
N1 C12 1.52(2) . ?
N1 C13 1.52(2) . ?
N1 C14 1.52(2) . ?
N1 C11 1.52(2) . ?
N2 C22 1.52(2) . ?
N2 C24 1.52(2) . ?
N2 C21 1.52(2) . ?
N2 C23 1.52(2) . ?
