Synthesis and Characterization of a New Organic-inorganic Hybrid Ferroelectric: (C4H10N)6[InBr6][InBr4]3•H2O
Xin, Wen-Bo; Xu, Guan-Cheng; Li, Min; Dalton Transactions  (2019) –; doi:10.1039/C9DT03970H

data_7701494
_publ_section_title
;
 Synthesis and Characterization of a New Organic-inorganic Hybrid
 Ferroelectric: (C4H10N)6[InBr6][InBr4]3&#x2022;H2O
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03970H
_journal_year                    2019
_chemical_formula_moiety         '3(Br4 In), Br6 In, 6(C4 H10 N)'
_chemical_formula_sum            'C24 H60 Br18 In4 N6'
_chemical_formula_weight         2330.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-04-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-16 deposited with the CCDC.	2019-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2507(17)
_cell_length_b                   19.9219(14)
_cell_length_c                   14.9429(10)
_cell_measurement_reflns_used    1455
_cell_measurement_temperature    300.01(10)
_cell_measurement_theta_max      41.5780
_cell_measurement_theta_min      4.1250
_cell_volume                     6326.1(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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -92.00  -2.00   1.00   10.00    --  -39.95 125.00  90.00   90
  2  \w     25.00  57.00   1.00   10.00    --   39.95-125.00 -60.00   32
  3  \w     60.00  95.00   1.00   10.00    --   39.95-125.00 -60.00   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0113277000
_diffrn_orient_matrix_UB_12      0.0249732000
_diffrn_orient_matrix_UB_13      0.0964776000
_diffrn_orient_matrix_UB_21      0.0566659000
_diffrn_orient_matrix_UB_22      -0.0480591000
_diffrn_orient_matrix_UB_23      0.0085107000
_diffrn_orient_matrix_UB_31      0.0439726000
_diffrn_orient_matrix_UB_32      0.0554311000
_diffrn_orient_matrix_UB_33      -0.0358129000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11954
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.588
_diffrn_reflns_theta_max         66.588
_diffrn_reflns_theta_min         4.161
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.447
_exptl_crystal_description       block
_exptl_crystal_F_000             4288
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.704
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         5561
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1441
_refine_ls_R_factor_gt           0.0873
_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^)+(0.1630P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2380
_refine_ls_wR_factor_ref         0.2835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2825
_reflns_number_total             5561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03970h2.cif
_cod_data_source_block           03083_CCDC1
_cod_database_code               7701494
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     C4A-C3-CSCl
_shelx_estimated_absorpt_t_max   0.100
_shelx_estimated_absorpt_t_min   0.087
_reflns_odcompleteness_completeness 35.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C4-N1
 1.45 with sigma of 0.02
 C1-N1
 1.45 with sigma of 0.02
 C1-C2
 1.5 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.02
 C3-C4
 1.5 with sigma of 0.02
 N3-C9
 1.45 with sigma of 0.02
 C9-C10
 1.52 with sigma of 0.02
 C10-C11
 1.52 with sigma of 0.02
 C11-C12
 1.52 with sigma of 0.02
 C12-N3
 1.45 with sigma of 0.02
 C6-C7
 1.5 with sigma of 0.02
3. Rigid bond restraints
 N1, C1, C2, C3, C4, N3, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim N2 \\sim C5 \\sim C6 \\sim C7
\\sim C8 \\sim N3 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Fixed Sof: Br5(0.5) Br6(0.5) Br7(0.5) Br8(0.5)
6.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), N2(H2C,H2D),
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), N3(H3C,H3D), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
;
_shelx_res_checksum              63312
_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 1.761
_oxdiff_exptl_absorpt_empirical_full_min 0.647