Thermally Induced Reversible Double Phase Transitions in an Organic-Inorganic Hybrid Iodoplumbate C4H12NPbI3 with Symmetry Breaking.
Liu, Guangfeng; Liu, Jie; Sun, Zhihua; Zhang, Zhenyi; Chang, Lei; Wang, Junling; Tao, Xutang; Zhang, Qichun; Inorganic chemistry 55 (2016) 8025–8030; doi:10.1021/acs.inorgchem.6b01143

data_4348366
_publ_section_title
;
 Thermally Induced Reversible Double Phase Transitions in an
 Organic-Inorganic Hybrid Iodoplumbate C4H12NPbI3 with Symmetry Breaking.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8025
_journal_page_last               8030
_journal_paper_doi               10.1021/acs.inorgchem.6b01143
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C4 H12 I3 N Pb'
_chemical_formula_weight         662.04
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
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_cell_angle_beta                 90
_cell_angle_gamma                120
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_cell_length_a                   9.616(3)
_cell_length_b                   9.616(3)
_cell_length_c                   23.734(6)
_cell_measurement_reflns_used    8443
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.45
_cell_volume                     1900.6(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
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_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10822
_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.457
_diffrn_reflns_theta_min         0.858
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    20.572
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.471
_exptl_crystal_description       prism
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.495
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.234
_refine_diff_density_max         4.119
_refine_diff_density_min         -3.888
_refine_diff_density_rms         0.548
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         2814
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0509
_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^)+(0.1200P)^2^+0.2418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1442
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2782
_reflns_number_total             2814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01143_si_002.cif
_cod_data_source_block           liujie20151211_1_0m_a
_cod_original_cell_volume        1900.5(11)
_cod_database_code               4348366
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.035
_shelx_estimated_absorpt_t_max   0.086
_shelx_res_checksum              93016
_shelx_hkl_checksum              72344