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_7225713
_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   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-04-20 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.32(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.046(2)
_cell_length_b                   18.186(3)
_cell_length_c                   14.839(3)
_cell_measurement_reflns_used    11923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.8817
_cell_measurement_theta_min      2.9750
_cell_volume                     1621.7(7)
_computing_cell_refinement
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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)
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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)
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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)
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.779
_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  0.0455
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.779
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21768
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         36.972
_diffrn_reflns_theta_min         2.981
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.530
_exptl_absorpt_correction_T_max  0.274
_exptl_absorpt_correction_T_min  0.077
_exptl_absorpt_correction_type   analytical
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CrysAlisPro, Agilent Technologies,
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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    2.341
_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         1.359
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         6414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4633
_reflns_number_total             6414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01008c3.cif
_cod_data_source_block           SbBrDIBA100K
_cod_depositor_comments
'Adding full bibliography for 7225712--7225715.cif.'
_cod_database_code               7225713
_shelx_estimated_absorpt_t_min   0.069
_shelx_estimated_absorpt_t_max   0.231
_shelxl_version_number           2014-3
_shelx_res_checksum              78709
_solvent_exptl_crystal_recrystallization_method water