Towards ferroelectricity-inducing chains of halogenoantimonates(iii) and halogenobismuthates(iii)
Owczarek, Magdalena; Szklarz, Przemysław; Jakubas, Ryszard; RSC Advances 11 (2021) 17574–17586; doi:10.1039/D0RA10151F

data_7242844
_publ_section_title
;
 Towards ferroelectricity-inducing chains of halogenoantimonates(iii) and
 halogenobismuthates(iii)
;
_journal_issue                   29
_journal_name_full               'RSC Advances'
_journal_page_first              17574
_journal_page_last               17586
_journal_paper_doi               10.1039/D0RA10151F
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'Bi Br5, 2(C4 H5 N2 S)'
_chemical_formula_sum            'C8 H10 Bi Br5 N4 S2'
_chemical_formula_weight         834.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2020-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-15 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.77(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.752(4)
_cell_length_b                   15.263(5)
_cell_length_c                   10.633(4)
_cell_measurement_reflns_used    2826
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.0420
_cell_measurement_theta_min      5.2930
_cell_volume                     902.7(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1956
_diffrn_detector_type            Onyx
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f      0.00 245.00   1.00   30.00   0.00  29.00 -25.00    --   245
  2  \w     25.00  50.00   1.00   55.00    --   40.00 -79.00   0.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0602712000
_diffrn_orient_matrix_UB_12      -0.0050906000
_diffrn_orient_matrix_UB_13      0.0666687000
_diffrn_orient_matrix_UB_21      -0.1116728000
_diffrn_orient_matrix_UB_22      -0.0079513000
_diffrn_orient_matrix_UB_23      0.0147375000
_diffrn_orient_matrix_UB_31      0.0127361000
_diffrn_orient_matrix_UB_32      -0.0454858000
_diffrn_orient_matrix_UB_33      -0.0100169000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5070
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.692
_diffrn_reflns_theta_min         4.781
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.058
_exptl_absorpt_correction_T_max  0.223
_exptl_absorpt_correction_T_min  0.167
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.072
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.921
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         2247
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0266
_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/[\s^2^(Fo^2^)+(0.0187P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1902
_reflns_number_total             2247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra10151f2.cif
_cod_data_source_block           2shprmbibr
_cod_database_code               7242844
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C8 H10 N4 S2 Bi Br5'
_shelx_estimated_absorpt_t_max   0.187
_shelx_estimated_absorpt_t_min   0.171
_reflns_odcompleteness_completeness 97.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 N1-H1 = N3-H3
 0.88 with sigma of 0.02
3.a Riding coordinates:
 N1(H1), N3(H3)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C5(H5)
;
_shelx_res_checksum              80034
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.812