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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/1/56/41/1564154.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_1564154
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_formula_moiety         'Bi2 Cl10, 2(C6 H10 N2), 2(H2 O)'
_chemical_formula_sum            'C12 H24 Bi2 Cl10 N4 O2'
_chemical_formula_weight         1028.81
_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                107.9200(10)
_cell_angle_beta                 103.4700(10)
_cell_angle_gamma                103.6630(10)
_cell_formula_units_Z            1
_cell_length_a                   7.42560(10)
_cell_length_b                   10.4710(2)
_cell_length_c                   10.6081(2)
_cell_measurement_reflns_used    9672
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      2.39
_cell_volume                     719.73(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 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.0245
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_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            11514
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_min         3.055
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    13.154
_exptl_absorpt_correction_T_max  0.1496
_exptl_absorpt_correction_T_min  0.0979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.374
_exptl_crystal_density_meas      2.373
_exptl_crystal_density_method    NONE
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0185(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2810
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0147
_refine_ls_R_factor_gt           0.0136
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0148P)²+0.3880P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0331
_refine_ls_wR_factor_ref         0.0335
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2712
_reflns_number_total             2810
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2020-511-119754.cif
_cod_data_source_block           1
_cod_database_code               1564154
_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   0.213
_shelx_estimated_absorpt_t_max   0.301
_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 0.3133(4) 0.2452(3) 1.2020(3) 0.0344(6) Uani 1 1 d . . . . .
H1 H 0.3345 0.3268 1.2786 0.041 Uiso 1 1 calc R U . . .
C2 C 0.2498(4) 0.2389(3) 1.0673(3) 0.0335(6) Uani 1 1 d . . . . .
C3 C 0.2158(4) 0.1186(3) 0.9523(3) 0.0389(6) Uani 1 1 d . . . . .
H3 H 0.1722 0.1166 0.8619 0.047 Uiso 1 1 calc R U . . .
C4 C 0.2474(5) 0.0017(3) 0.9733(3) 0.0433(7) Uani 1 1 d . . . . .
H4 H 0.2247 -0.0801 0.8965 0.052 Uiso 1 1 calc R U . . .
C5 C 0.3127(4) 0.0043(3) 1.1079(3) 0.0398(7) Uani 1 1 d . . . . .
H5 H 0.3344 -0.0749 1.1221 0.048 Uiso 1 1 calc R U . . .
C6 C 0.3448(4) 0.1261(3) 1.2200(3) 0.0330(6) Uani 1 1 d . . . . .
N1 N 0.2149(4) 0.3650(3) 1.0468(3) 0.0449(6) Uani 1 1 d . . . . .
H1A H 0.3186 0.4419 1.1020 0.067 Uiso 1 1 calc R U . . .
H1B H 0.1090 0.3753 1.0685 0.067 Uiso 1 1 calc R U . . .
H1C H 0.1960 0.3538 0.9576 0.067 Uiso 1 1 calc R U . . .
N2 N 0.4105(4) 0.1308(3) 1.3631(2) 0.0424(6) Uani 1 1 d . . . . .
H2A H 0.3087 0.1184 1.3942 0.064 Uiso 1 1 calc R U . . .
H2B H 0.5012 0.2148 1.4189 0.064 Uiso 1 1 calc R U . . .
H2C H 0.4614 0.0619 1.3633 0.064 Uiso 1 1 calc R U . . .
Cl1 Cl -0.25993(10) 0.44444(8) 1.51834(9) 0.04344(17) Uani 1 1 d . . . . .
Cl2 Cl -0.12439(12) 0.24298(9) 1.73194(9) 0.0515(2) Uani 1 1 d . . . . .
Cl3 Cl 0.01370(13) 0.16607(9) 1.41569(9) 0.0537(2) Uani 1 1 d . . . . .
Cl4 Cl 0.40323(11) 0.36227(9) 1.77452(10) 0.0518(2) Uani 1 1 d . . . . .
Cl5 Cl 0.17238(14) 0.61768(9) 1.88425(10) 0.0608(2) Uani 1 1 d . . . . .
Bi1 Bi 0.08109(2) 0.39995(2) 1.64157(2) 0.03019(6) Uani 1 1 d . . . . .
O1' O 0.6178(4) -0.0496(3) 1.3931(3) 0.0546(6) Uani 1 1 d D . . . .
H1'' H 0.745(3) -0.002(4) 1.411(4) 0.077(13) Uiso 1 1 d D . . . .
H1' H 0.598(7) -0.130(3) 1.321(3) 0.090(15) 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'
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'
O O 0.0106 0.0060 '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
C2 C1 C6 117.7(3) . .
C2 C1 H1 121.1 . .
C6 C1 H1 121.1 . .
C1 C2 C3 122.1(3) . .
C1 C2 N1 118.2(2) . .
C3 C2 N1 119.7(3) . .
C4 C3 C2 118.9(3) . .
C4 C3 H3 120.5 . .
C2 C3 H3 120.5 . .
C3 C4 C5 120.7(3) . .
C3 C4 H4 119.7 . .
C5 C4 H4 119.7 . .
C6 C5 C4 118.8(3) . .
C6 C5 H5 120.6 . .
C4 C5 H5 120.6 . .
C5 C6 C1 121.8(3) . .
C5 C6 N2 119.8(3) . .
C1 C6 N2 118.3(2) . .
C2 N1 H1A 109.5 . .
C2 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
C2 N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
C6 N2 H2A 109.5 . .
C6 N2 H2B 109.5 . .
H2A N2 H2B 109.5 . .
C6 N2 H2C 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
Bi1 Cl1 Bi1 95.11(2) . 2_568
Cl2 Bi1 Cl4 90.56(3) . .
Cl2 Bi1 Cl5 88.61(3) . .
Cl4 Bi1 Cl5 83.59(3) . .
Cl2 Bi1 Cl3 88.44(3) . .
Cl4 Bi1 Cl3 90.01(3) . .
Cl5 Bi1 Cl3 172.93(3) . .
Cl2 Bi1 Cl1 87.30(3) . .
Cl4 Bi1 Cl1 176.46(2) . .
Cl5 Bi1 Cl1 93.53(3) . .
Cl3 Bi1 Cl1 92.75(3) . .
Cl2 Bi1 Cl1 168.88(2) . 2_568
Cl4 Bi1 Cl1 97.62(3) . 2_568
Cl5 Bi1 Cl1 99.74(3) . 2_568
Cl3 Bi1 Cl1 84.05(3) . 2_568
Cl1 Bi1 Cl1 84.89(2) . 2_568
H1'' O1' H1' 101(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.372(4) .
C1 C6 1.382(4) .
C1 H1 0.9300 .
C2 C3 1.379(4) .
C2 N1 1.473(4) .
C3 C4 1.372(4) .
C3 H3 0.9300 .
C4 C5 1.386(4) .
C4 H4 0.9300 .
C5 C6 1.375(4) .
C5 H5 0.9300 .
C6 N2 1.464(3) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
Cl1 Bi1 2.7800(7) .
Cl1 Bi1 3.0041(8) 2_568
Cl2 Bi1 2.5328(8) .
Cl3 Bi1 2.6909(8) .
Cl4 Bi1 2.6614(7) .
Cl5 Bi1 2.6702(8) .
Bi1 Cl1 3.0041(8) 2_568
O1' H1'' 0.904(15) .
O1' H1' 0.898(15) .
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 Cl1 0.93 2.95 3.839(3) 161.1 2_568
N1 H1A Cl4 0.89 2.30 3.183(3) 174.3 2_668
N1 H1B Cl5 0.89 2.27 3.160(3) 175.4 2_568
N1 H1C Cl2 0.89 2.66 3.327(3) 132.7 1_554
N1 H1C Cl4 0.89 2.75 3.486(3) 140.5 1_554
N2 H2A Cl3 0.89 2.40 3.206(3) 150.1 .
N2 H2A O1' 0.89 2.55 2.996(4) 111.5 2_658
N2 H2B Cl1 0.89 2.36 3.238(3) 167.0 1_655
N2 H2C O1' 0.89 1.87 2.748(4) 167.3 .
O1' H1'' Cl3 0.904(15) 2.30(2) 3.163(3) 159(4) 1_655
O1' H1' Cl4 0.898(15) 2.32(2) 3.154(3) 154(4) 2_658
C1 H1 Cl1 0.93 2.95 3.839(3) 161.1 2_568
N1 H1A Cl4 0.89 2.30 3.183(3) 174.3 2_668
N1 H1B Cl5 0.89 2.27 3.160(3) 175.4 2_568
N1 H1C Cl2 0.89 2.66 3.327(3) 132.7 1_554
N1 H1C Cl4 0.89 2.75 3.486(3) 140.5 1_554
N2 H2A Cl3 0.89 2.40 3.206(3) 150.1 .
N2 H2A O1' 0.89 2.55 2.996(4) 111.5 2_658
N2 H2B Cl1 0.89 2.36 3.238(3) 167.0 1_655
N2 H2C O1' 0.89 1.87 2.748(4) 167.3 .
O1' H1'' Cl3 0.904(15) 2.30(2) 3.163(3) 159(4) 1_655
O1' H1' Cl4 0.898(15) 2.32(2) 3.154(3) 154(4) 2_658
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 0.6(4) . . . .
C6 C1 C2 N1 179.7(3) . . . .
C1 C2 C3 C4 -0.3(4) . . . .
N1 C2 C3 C4 -179.4(3) . . . .
C2 C3 C4 C5 -0.1(5) . . . .
C3 C4 C5 C6 0.2(5) . . . .
C4 C5 C6 C1 0.2(4) . . . .
C4 C5 C6 N2 178.9(3) . . . .
C2 C1 C6 C5 -0.5(4) . . . .
C2 C1 C6 N2 -179.3(2) . . . .
