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#$Date: 2021-07-15 10:49:38 +0300 (Thu, 15 Jul 2021) $
#$Revision: 267548 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/41/1564156.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_1564156
loop_
_publ_author_name
'Pandey, Souvik'
'Pradeep, Prajisha'
'Venugopal M, Anjali'
'Aswanth, A.A.'
'Andrews, Alex P.'
'Venugopal, Ajay'
_publ_section_title
;
 Incorporation of nitrate ions into halobismuthates
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119754
_journal_paper_doi               10.1016/j.ica.2020.119754
_journal_volume                  511
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         'Bi2 Cl8 N2 O6, 2(C6 H10 N2), 2(H2 O)'
_chemical_formula_sum            'C12 H24 Bi2 Cl8 N6 O8'
_chemical_formula_weight         1081.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                103.7960(10)
_cell_angle_beta                 107.5400(10)
_cell_angle_gamma                97.2160(10)
_cell_formula_units_Z            1
_cell_length_a                   7.43460(10)
_cell_length_b                   10.4198(2)
_cell_length_c                   10.6765(2)
_cell_measurement_reflns_used    8309
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.94
_cell_volume                     748.25(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11955
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.966
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    12.503
_exptl_absorpt_correction_T_max  0.368
_exptl_absorpt_correction_T_min  0.256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.401
_exptl_crystal_density_meas      2.400
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2913
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0173
_refine_ls_R_factor_gt           0.0153
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0164P)²+0.2717P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0331
_refine_ls_wR_factor_ref         0.0336
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2736
_reflns_number_total             2913
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2020-511-119754.cif
_cod_data_source_block           3
_cod_database_code               1564156
_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   0.256
_shelx_estimated_absorpt_t_max   0.368
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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
C1 C 0.8235(4) 1.2161(3) 0.7429(3) 0.0321(7) Uani 1 1 d . . . . .
H1 H 0.8484 1.2929 0.8163 0.039 Uiso 1 1 calc R U . . .
C2 C 0.8585(4) 1.2245(3) 0.6244(3) 0.0339(7) Uani 1 1 d . . . . .
C3 C 0.8234(5) 1.1122(3) 0.5164(3) 0.0398(8) Uani 1 1 d . . . . .
H3 H 0.8482 1.1197 0.4378 0.048 Uiso 1 1 calc R U . . .
C4 C 0.7503(5) 0.9869(3) 0.5254(3) 0.0448(8) Uani 1 1 d . . . . .
H4 H 0.7253 0.9100 0.4522 0.054 Uiso 1 1 calc R U . . .
C5 C 0.7143(5) 0.9754(3) 0.6417(3) 0.0381(7) Uani 1 1 d . . . . .
H5 H 0.6664 0.8914 0.6484 0.046 Uiso 1 1 calc R U . . .
C6 C 0.7511(4) 1.0912(3) 0.7478(3) 0.0299(6) Uani 1 1 d . . . . .
N1 N 0.5140(4) 0.5601(3) 0.3687(3) 0.0384(6) Uani 1 1 d . . . . .
N2 N 0.9361(4) 1.3583(3) 0.6190(3) 0.0468(7) Uani 1 1 d . . . . .
H2A H 0.9504 1.4200 0.6970 0.070 Uiso 1 1 calc R U . . .
H2B H 1.0501 1.3592 0.6079 0.070 Uiso 1 1 calc R U . . .
H2C H 0.8549 1.3773 0.5489 0.070 Uiso 1 1 calc R U . . .
N3 N 0.7139(4) 1.0807(3) 0.8735(3) 0.0374(6) Uani 1 1 d . . . . .
H3A H 0.6673 0.9946 0.8640 0.056 Uiso 1 1 calc R U . . .
H3B H 0.8236 1.1112 0.9450 0.056 Uiso 1 1 calc R U . . .
H3C H 0.6284 1.1299 0.8874 0.056 Uiso 1 1 calc R U . . .
O1 O 0.6444(4) 0.5145(3) 0.3316(3) 0.0589(7) Uani 1 1 d . . . . .
O1' O 1.0347(4) 1.3549(3) 0.3882(3) 0.0577(7) Uani 1 1 d D . . . .
O2 O 0.3419(3) 0.5117(2) 0.2900(2) 0.0462(6) Uani 1 1 d . . . . .
O3 O 0.5520(4) 0.6465(2) 0.4792(3) 0.0597(7) Uani 1 1 d . . . . .
Cl1 Cl 0.32929(13) 0.19971(10) -0.16695(8) 0.0548(2) Uani 1 1 d . . . . .
Cl2 Cl 0.61867(11) 0.17730(8) 0.16524(9) 0.04132(18) Uani 1 1 d . . . . .
Cl3 Cl 0.12305(11) 0.19938(8) 0.10327(9) 0.04274(19) Uani 1 1 d . . . . .
Cl4 Cl 0.76169(12) 0.46318(9) 0.04775(9) 0.04157(18) Uani 1 1 d . . . . .
Bi1 Bi 0.42218(2) 0.34801(2) 0.08226(2) 0.02908(5) Uani 1 1 d . . . . .
H1B H 1.163(2) 1.362(7) 0.418(6) 0.18(3) Uiso 1 1 d D . . . .
H1A H 0.970(6) 1.293(4) 0.308(3) 0.107(19) Uiso 1 1 d D . . . .
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'
O O 0.0106 0.0060 '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'
Bi Bi -4.1077 10.2566 '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
C6 C1 C2 117.5(3) . .
C6 C1 H1 121.2 . .
C2 C1 H1 121.2 . .
C3 C2 C1 121.6(3) . .
C3 C2 N2 120.8(3) . .
C1 C2 N2 117.6(3) . .
C2 C3 C4 119.1(3) . .
C2 C3 H3 120.4 . .
C4 C3 H3 120.4 . .
C5 C4 C3 120.6(3) . .
C5 C4 H4 119.7 . .
C3 C4 H4 119.7 . .
C4 C5 C6 118.3(3) . .
C4 C5 H5 120.8 . .
C6 C5 H5 120.8 . .
C1 C6 C5 122.8(3) . .
C1 C6 N3 118.2(3) . .
C5 C6 N3 119.1(3) . .
O3 N1 O1 121.4(3) . .
O3 N1 O2 120.9(3) . .
O1 N1 O2 117.6(3) . .
C2 N2 H2A 109.5 . .
C2 N2 H2B 109.5 . .
H2A N2 H2B 109.5 . .
C2 N2 H2C 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
C6 N3 H3A 109.5 . .
C6 N3 H3B 109.5 . .
H3A N3 H3B 109.5 . .
C6 N3 H3C 109.5 . .
H3A N3 H3C 109.5 . .
H3B N3 H3C 109.5 . .
N1 O1 Bi1 98.57(19) . .
H1B O1' H1A 115(3) . .
N1 O2 Bi1 96.88(16) . .
Bi1 Cl4 Bi1 93.34(2) . 2_665
Cl1 Bi1 Cl2 89.44(3) . .
Cl1 Bi1 Cl3 88.91(3) . .
Cl2 Bi1 Cl3 86.57(3) . .
Cl1 Bi1 O1 159.25(6) . .
Cl2 Bi1 O1 82.70(6) . .
Cl3 Bi1 O1 109.64(6) . .
Cl1 Bi1 O2 152.38(5) . .
Cl2 Bi1 O2 111.81(5) . .
Cl3 Bi1 O2 75.55(5) . .
O1 Bi1 O2 46.78(7) . .
Cl1 Bi1 Cl4 85.65(3) . .
Cl2 Bi1 Cl4 84.91(2) . .
Cl3 Bi1 Cl4 169.93(2) . .
O1 Bi1 Cl4 74.57(6) . .
O2 Bi1 Cl4 112.69(5) . .
Cl1 Bi1 Cl4 83.46(3) . 2_665
Cl2 Bi1 Cl4 169.36(2) . 2_665
Cl3 Bi1 Cl4 101.14(2) . 2_665
O1 Bi1 Cl4 101.29(6) . 2_665
O2 Bi1 Cl4 77.50(5) . 2_665
Cl4 Bi1 Cl4 86.66(2) . 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.364(4) .
C1 C2 1.386(4) .
C1 H1 0.9300 .
C2 C3 1.366(4) .
C2 N2 1.462(4) .
C3 C4 1.386(5) .
C3 H3 0.9300 .
C4 C5 1.375(5) .
C4 H4 0.9300 .
C5 C6 1.376(4) .
C5 H5 0.9300 .
C6 N3 1.475(4) .
N1 O3 1.229(3) .
N1 O1 1.257(3) .
N1 O2 1.259(3) .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
N3 H3A 0.8900 .
N3 H3B 0.8900 .
N3 H3C 0.8900 .
O1 Bi1 2.693(2) .
O1' H1B 0.898(15) .
O1' H1A 0.890(15) .
O2 Bi1 2.727(2) .
Cl1 Bi1 2.5705(8) .
Cl2 Bi1 2.5898(8) .
Cl3 Bi1 2.6449(8) .
Cl4 Bi1 2.8210(8) .
Cl4 Bi1 2.9155(8) 2_665
Bi1 Cl4 2.9155(8) 2_665
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
C1 H1 Cl4 0.93 2.97 3.825(3) 153.5 1_566
C5 H5 O3 0.93 2.61 3.328(4) 134.0 .
N2 H2A O2 0.89 2.40 2.887(4) 114.5 2_676
N2 H2A Cl4 0.89 2.78 3.484(3) 136.9 2_776
N2 H2B O1 0.89 2.30 3.066(4) 144.9 2_776
N2 H2B O1' 0.89 2.30 2.770(4) 112.5 .
N3 H3A Cl2 0.89 2.49 3.270(3) 146.6 2_666
N3 H3A Cl3 0.89 2.73 3.331(3) 126.2 2_666
N3 H3B Cl3 0.89 2.27 3.148(3) 170.9 1_666
N3 H3C Cl1 0.89 2.38 3.210(3) 156.3 1_566
N3 H3C Cl2 0.89 2.91 3.351(3) 112.1 1_566
O1' H1B N1 0.898(15) 2.63(3) 3.419(4) 147(5) 2_776
O1' H1B O1 0.898(15) 2.53(5) 3.072(4) 119(4) 2_776
O1' H1B O3 0.898(15) 2.10(2) 2.974(4) 166(7) 2_776
O1' H1A Cl2 0.890(15) 2.56(3) 3.268(3) 137(4) 1_565
O1' H1A Cl3 0.890(15) 2.79(4) 3.381(3) 125(4) 1_665
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C6 C1 C2 C3 -0.4(5) . . . .
C6 C1 C2 N2 -180.0(3) . . . .
C1 C2 C3 C4 0.2(5) . . . .
N2 C2 C3 C4 179.8(3) . . . .
C2 C3 C4 C5 -0.3(5) . . . .
C3 C4 C5 C6 0.6(5) . . . .
C2 C1 C6 C5 0.6(5) . . . .
C2 C1 C6 N3 179.7(3) . . . .
C4 C5 C6 C1 -0.7(5) . . . .
C4 C5 C6 N3 -179.8(3) . . . .
O3 N1 O1 Bi1 -177.5(2) . . . .
O2 N1 O1 Bi1 4.1(3) . . . .
O3 N1 O2 Bi1 177.6(2) . . . .
O1 N1 O2 Bi1 -4.0(3) . . . .
