Phosphonium-Templated Iodoplumbates.
Omahen, Emily H.; Binder, Justin F.; Jacobs, Brad F.; Swidan, Ala'aeddeen; Macdonald, Charles L. B.; ACS omega 3 (2018) 17077–17082; doi:10.1021/acsomega.8b02240

data_4516156
_publ_section_title
;
 Phosphonium-Templated Iodoplumbates.
;
_journal_issue                   12
_journal_name_full               'ACS omega'
_journal_page_first              17077
_journal_page_last               17082
_journal_paper_doi               10.1021/acsomega.8b02240
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C12 H28 P,  Pb I3'
_chemical_formula_sum            'C12 H28 I3 P Pb'
_chemical_formula_weight         791.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 107.066(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.0770(7)
_cell_length_b                   16.3313(9)
_cell_length_c                   16.9952(9)
_cell_measurement_reflns_used    9376
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.10
_cell_measurement_theta_min      2.93
_cell_volume                     4265.7(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-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0807
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            208613
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.568
_diffrn_reflns_theta_min         2.864
_exptl_absorpt_coefficient_mu    12.313
_exptl_absorpt_correction_T_max  0.085
_exptl_absorpt_correction_T_min  0.050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Burker 2016'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.464
_exptl_crystal_description       prism
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.763
_refine_diff_density_min         -4.029
_refine_diff_density_rms         0.356
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.260(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         25712
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0343P)^2^+91.7134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1364
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                18928
_reflns_number_total             25712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b02240_si_004.cif
_cod_data_source_block           eo131_p21
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4516156
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.079
_shelx_estimated_absorpt_t_max   0.192
_shelx_res_checksum              70764
_shelx_hkl_checksum              62911