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_7242853
_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 H6 N3)'
_chemical_formula_sum            'C8 H12 Bi Br5 N6'
_chemical_formula_weight         800.77
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-08-17
_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                115.801(5)
_cell_angle_beta                 96.295(3)
_cell_angle_gamma                98.857(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8733(3)
_cell_length_b                   11.4038(5)
_cell_length_c                   11.6180(5)
_cell_measurement_reflns_used    5859
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.5440
_cell_measurement_theta_min      3.3250
_cell_volume                     909.46(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.567
_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    -70.00  69.50   0.75   30.00    --   28.00 -79.00   0.00  186
  2  \w    -70.00  69.50   0.75   30.00    --   28.00 -79.00  90.00  186
  3  \w    -70.00  69.50   0.75   30.00    --   28.00 -79.00 180.00  186
  4  \w    -70.00  69.50   0.75   30.00    --   28.00 -79.00 270.00  186
  5  \w    -54.00  60.00   0.75   50.00    --   48.00 -79.00  45.00  152
;
_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      -0.0342251000
_diffrn_orient_matrix_UB_12      -0.0588107000
_diffrn_orient_matrix_UB_13      -0.0598369000
_diffrn_orient_matrix_UB_21      -0.0087018000
_diffrn_orient_matrix_UB_22      0.0395608000
_diffrn_orient_matrix_UB_23      -0.0325141000
_diffrn_orient_matrix_UB_31      0.0860660000
_diffrn_orient_matrix_UB_32      -0.0021123000
_diffrn_orient_matrix_UB_33      -0.0122301000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.567
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9692
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.567
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.673
_diffrn_reflns_theta_min         2.972
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    20.675
_exptl_absorpt_correction_T_max  0.481
_exptl_absorpt_correction_T_min  0.035
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.924
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.038
_refine_diff_density_max         2.716
_refine_diff_density_min         -2.757
_refine_diff_density_rms         0.400
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         5132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0546
_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/[\s^2^(Fo^2^)+(0.0756P)^2^+5.6399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4358
_reflns_number_total             5132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra10151f2.cif
_cod_data_source_block           2apyrimabs
_cod_original_cell_volume        909.46(7)
_cod_database_code               7242853
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C8 H12 Bi Br5 N6'
_reflns_odcompleteness_completeness 99.22
_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:
 N1A(H1A), C5A(H5A), N1B(H1B), C6A(H6A), C4A(H4A), C6B(H6B), C4B(H4B), C5B(H5B)
2.b X=CH2 refined with riding coordinates:
 N2A(H2AA,H2AB), N2B(H2BA,H2BB)
;
_shelx_res_checksum              62390
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.572
_oxdiff_exptl_absorpt_empirical_full_min 0.655