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_7701493
_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, H2 O, 6(C4 H10 N)'
_chemical_formula_sum            'C24 H62 Br18 In4 N6 O'
_chemical_formula_weight         2348.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-05-29
_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                   14.9084(4)
_cell_length_b                   20.8427(7)
_cell_length_c                   19.5727(5)
_cell_measurement_reflns_used    4674
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.9470
_cell_measurement_theta_min      4.2310
_cell_volume                     6081.9(3)
_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      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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    -30.00  24.00   1.00    3.00    --  -39.95  57.00  90.00   54
  2  \w   -106.00 -50.00   1.00    3.00    --  -39.95 -57.00   0.00   56
  3  \w     43.00  94.00   1.00    3.00    --   39.95-125.00 -30.00   51
  4  \w     87.00 164.00   1.00    6.00    --  105.48  45.00 120.00   77
  5  \w    101.00 178.00   1.00    6.00    --  105.48 125.00 -90.00   77
  6  \w     95.00 178.00   1.00    6.00    --  105.48 125.00-180.00   83
;
_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      0.0477687000
_diffrn_orient_matrix_UB_12      0.0589957000
_diffrn_orient_matrix_UB_13      0.0302628000
_diffrn_orient_matrix_UB_21      0.0891900000
_diffrn_orient_matrix_UB_22      -0.0374939000
_diffrn_orient_matrix_UB_23      0.0009353000
_diffrn_orient_matrix_UB_31      0.0210203000
_diffrn_orient_matrix_UB_32      0.0240611000
_diffrn_orient_matrix_UB_33      -0.0726362000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12124
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        65.997
_diffrn_reflns_theta_max         65.997
_diffrn_reflns_theta_min         3.645
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    26.041
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22727
_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    2.565
_exptl_crystal_description       block
_exptl_crystal_F_000             4328
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.708
_refine_diff_density_min         -1.803
_refine_diff_density_rms         0.310
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         7688
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0810
_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^)+(0.0997P)^2^+191.0617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2069
_refine_ls_wR_factor_ref         0.2131
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                6977
_reflns_number_total             7688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03970h2.cif
_cod_data_source_block           03083
_cod_original_cell_volume        6081.8(3)
_cod_database_code               7701493
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     C4A-C3-CSCl
_shelx_estimated_absorpt_t_max   0.096
_shelx_estimated_absorpt_t_min   0.083
_reflns_odcompleteness_completeness 99.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(2)
 0.49(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 N1-C4
 1.47 with sigma of 0.02
 C4-N1
 1.55 with sigma of 0.02
 C4-C3
 1.55 with sigma of 0.02
 C19-C18
 1.55 with sigma of 0.02
 C2-C3
 1.55 with sigma of 0.02
 C9-C10
 1.55 with sigma of 0.02
 C15-C14
 1.55 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C9) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(N2) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C15) \\sim
Ueq, Uanis(N4) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C14) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5.a Riding coordinates:
 O1W(H1WA,H1WB)
5.b 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), N4(H4C,H4D), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), N5(H5C,H5D), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), N6(H6C,H6D), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
;
_shelx_res_checksum              56652
_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 2.559
_oxdiff_exptl_absorpt_empirical_full_min 0.445