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_4348372
_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_formula_sum            'C4 H12 I3 N Pb'
_chemical_formula_weight         662.04
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   9.798(3)
_cell_length_b                   9.798(3)
_cell_length_c                   7.953(3)
_cell_measurement_reflns_used    5523
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.40
_cell_volume                     661.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7502
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.583
_diffrn_reflns_theta_min         2.400
_exptl_absorpt_coefficient_mu    19.710
_exptl_absorpt_correction_T_max  0.0182
_exptl_absorpt_correction_T_min  0.0042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.325
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.495
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.214
_refine_diff_density_max         2.580
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       0.0059(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         557
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0584P)^2^+2.5940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                544
_reflns_number_total             557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01143_si_004.cif
_cod_data_source_block           02_a
_cod_original_cell_volume        661.2(5)
_cod_database_code               4348372
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.037
_shelx_estimated_absorpt_t_max   0.101
_shelx_res_checksum              18783
_shelx_hkl_checksum              9837