Enormous lattice distortion through an isomorphous phase transition in an organic‒inorganic hybrid based on haloantimonate(iii)
Wojciechowska, Martyna; Szklarz, Przemysław; Białońska, Agata; Baran, Jan; Janicki, Rafał; Medycki, Wojciech; Durlak, Piotr; Piecha-Bisiorek, Anna; Jakubas, Ryszard; CrystEngComm 18 (2016) 6184–; doi:10.1039/C6CE01008C

data_7225712
_publ_section_title
;
 Enormous lattice distortion through an isomorphous phase transition in an
 organic--inorganic hybrid based on haloantimonate(iii)
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              6184
_journal_paper_doi               10.1039/C6CE01008C
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C8 H20 N, Br4 Sb'
_chemical_formula_sum            'C8 H20 Br4 N Sb'
_chemical_formula_weight         571.64
_chemical_name_systematic
;
Bis(diisobutylammonium) octabromodiantimonate(III)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2016-04-20 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.25(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.964(2)
_cell_length_b                   20.098(8)
_cell_length_c                   14.385(8)
_cell_measurement_reflns_used    3373
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      28.6414
_cell_measurement_theta_min      3.0346
_cell_volume                     1701.8(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.918
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7558
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.043
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.987
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35463
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28c (release 15-05-2013 CrysAlis171 .NET)
(compiled May 15 2013,09:16:53)
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)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.231
_exptl_crystal_description       needle
_exptl_crystal_F_000             1064
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.894
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.191
_refine_ls_extinction_coef       0.0028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         2824
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0810P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1210
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1934
_reflns_number_total             2824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01008c3.cif
_cod_data_source_block           SbBrDIBA250K
_cod_depositor_comments
'Adding full bibliography for 7225712--7225715.cif.'
_cod_database_code               7225712
_shelx_estimated_absorpt_t_min   0.073
_shelx_estimated_absorpt_t_max   0.242
_shelxl_version_number           2014-3
_shelx_res_checksum              76008
_solvent_exptl_crystal_recrystallization_method water