Crystal structure of formamidinium–lead–chloride–dimethyl sulfoxide and phase relationship of related crystalline systems
Saito, Noriko; Matsushita, Yoshitaka; Ohsawa, Takeo; Segawa, Hiroyo; Ohashi, Naoki; CrystEngComm  (2022) –; doi:10.1039/D2CE00889K

data_7245751
_publ_section_title
;
 Crystal structure of formamidinium--lead--chloride--dimethyl sulfoxide
 and phase relationship of related crystalline systems
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00889K
_journal_year                    2022
_chemical_formula_sum            'C3 H11 Cl3 N2 O Pb S'
_chemical_formula_weight         436.74
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2022-05-27 deposited with the CCDC.	2022-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.211(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8864(4)
_cell_length_b                   14.1043(4)
_cell_length_c                   9.0106(3)
_cell_measurement_reflns_used    7938
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3460
_cell_measurement_theta_min      2.6480
_cell_volume                     1154.75(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19267
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.648
_diffrn_reflns_theta_min         2.667
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    15.442
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'Clear white'
_exptl_crystal_density_diffrn    2.512
_exptl_crystal_F_000             800
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMSO'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.00248(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         3452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0101P)^2^+0.7560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0402
_refine_ls_wR_factor_ref         0.0422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2848
_reflns_number_total             3452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00889k3.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7245751
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.119
_shelx_estimated_absorpt_t_max   0.543
_shelx_res_checksum              4283
_shelx_hkl_checksum              98519