Chemical Pathways Connecting Lead(II) Iodide and Perovskite via Polymeric Plumbate(II) Fiber.
Guo, Yunlong; Shoyama, Kazutaka; Sato, Wataru; Matsuo, Yutaka; Inoue, Kento; Harano, Koji; Liu, Chao; Tanaka, Hideyuki; Nakamura, Eiichi; Journal of the American Chemical Society 137 (2015) 15907–15914; doi:10.1021/jacs.5b10599

data_4129809
_publ_section_title
;
 Chemical Pathways Connecting Lead(II) Iodide and Perovskite via Polymeric
 Plumbate(II) Fiber.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15907
_journal_page_last               15914
_journal_paper_doi               10.1021/jacs.5b10599
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'I8 Pb3, 2(C2 O S), 2(C N)'
_chemical_formula_sum            'C6 I8 N2 O2 Pb3 S2'
_chemical_formula_weight         1832.97
_chemical_name_common            INT-3
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.59140(10)
_cell_length_b                   27.2463(5)
_cell_length_c                   26.7574(5)
_cell_measurement_reflns_used    18021
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      68.227
_cell_measurement_theta_min      3.244
_cell_volume                     3347.31(11)
_computing_cell_refinement       'Rapid Auto (Rigaku)'
_computing_data_collection       'Rapid Auto (Rigaku)'
_computing_data_reduction        'Rapid Auto (Rigaku)'
_computing_molecular_graphics    Mercury
_computing_publication_material  Mercury
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1022
_diffrn_reflns_av_unetI/netI     0.1053
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            18021
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.227
_diffrn_reflns_theta_min         3.244
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    88.003
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.1973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Empirical Absorption Correction March 2001 T Higashi'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    3.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         4.354
_refine_diff_density_min         -3.250
_refine_diff_density_rms         0.498
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.000019(7)
_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   1.150
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         3472
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0745P)^2^+12.7796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1714
_reflns_Friedel_coverage         0.955
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2740
_reflns_number_total             3472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10599_si_005.cif
_cod_data_source_block           (CH3NH3)2Pb3I8DMSO2
_cod_original_cell_volume        3347.32(11)
_cod_database_code               4129809
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.013
_shelx_estimated_absorpt_t_max   0.473
_shelx_res_checksum              94572
_shelx_hkl_checksum              60619