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_7242850
_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         'Cl5 Sb, 2(C4 H6 N3)'
_chemical_formula_sum            'C8 H12 Cl5 N6 Sb'
_chemical_formula_weight         491.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2020-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-26 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.65(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.713(3)
_cell_length_b                   14.125(5)
_cell_length_c                   10.254(4)
_cell_measurement_reflns_used    12171
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.0020
_cell_measurement_theta_min      3.5370
_cell_volume                     796.8(6)
_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 8.3359
_diffrn_detector_type            'Sapphire2, large Be window'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -71.00  70.62   0.73   10.00    --   30.00 -79.00   0.00  194
  2  \w    -71.00  70.62   0.73   10.00    --   30.00 -79.00  90.00  194
  3  \w    -71.00  70.62   0.73   10.00    --   30.00 -79.00 180.00  194
  4  \w    -71.00  70.62   0.73   10.00    --   30.00 -79.00 270.00  194
  5  \w    -54.00  60.61   0.73   16.00    --   48.00 -79.00  45.00  157
  6  \w    -54.00  60.61   0.73   16.00    --   48.00 -79.00 135.00  157
  7  \w    -54.00  60.61   0.73   16.00    --   48.00 -79.00 225.00  157
  8  \w    -54.00   5.86   0.73   16.00    --   48.00 -79.00 315.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0664068000
_diffrn_orient_matrix_UB_12      0.0341153000
_diffrn_orient_matrix_UB_13      0.0461142000
_diffrn_orient_matrix_UB_21      -0.0096713000
_diffrn_orient_matrix_UB_22      -0.0286905000
_diffrn_orient_matrix_UB_23      0.0551001000
_diffrn_orient_matrix_UB_31      0.1099808000
_diffrn_orient_matrix_UB_32      -0.0231659000
_diffrn_orient_matrix_UB_33      -0.0003563000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14833
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.801
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.962
_diffrn_reflns_theta_min         2.884
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.567
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.649
_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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.048
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.402
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 2564 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.396(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         6494
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0257P)^2^+0.1531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0531
_reflns_Friedel_coverage         0.738
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.702
_reflns_number_gt                6240
_reflns_number_total             6494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra10151f2.cif
_cod_data_source_block           2aprmsbcl_acentro
_cod_database_code               7242850
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C8 H12 N6 Sb1 Cl5'
_shelx_estimated_absorpt_t_max   0.748
_shelx_estimated_absorpt_t_min   0.602
_reflns_odcompleteness_completeness 99.82
_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, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3B(H3B), N1A(H1A), C6A(H6A), C4A(H4A), C5A(H5A), C6B(H6B), N1B(H1B), C4B(H4B)
2.b X=CH2 refined with riding coordinates:
 N2B(H2BA,H2BB), N2A(H2AA,H2AB)
;
_shelx_res_checksum              63667
_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 1.125
_oxdiff_exptl_absorpt_empirical_full_min 0.923