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_4348367
_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            'C8 H24 I6 N2 Pb2'
_chemical_formula_weight         1324.07
_space_group_IT_number           6
_space_group_name_Hall           'P -2y'
_space_group_name_H-M_alt        'P 1 m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2y'
_symmetry_space_group_name_H-M   'P 1 m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.980(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6621(16)
_cell_length_b                   15.840(3)
_cell_length_c                   9.6626(16)
_cell_measurement_reflns_used    6171
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      28.76
_cell_measurement_theta_min      2.43
_cell_volume                     1281.0(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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6158
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    20.348
_exptl_absorpt_correction_T_max  0.0999
_exptl_absorpt_correction_T_min  0.0350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    3.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.689
_refine_diff_density_min         -2.580
_refine_diff_density_rms         0.426
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3433
_refine_ls_number_restraints     243
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+46.0204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1816
_refine_ls_wR_factor_ref         0.1821
_reflns_number_gt                3413
_reflns_number_total             3433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01143_si_003.cif
_cod_data_source_block           new
_cod_original_sg_symbol_H-M      'P m'
_cod_database_code               4348367