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_4516160
_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_sum            'C4 H12 I3 P Pb'
_chemical_formula_weight         679.00
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   10.0382(8)
_cell_length_b                   10.0382(8)
_cell_length_c                   23.738(2)
_cell_measurement_reflns_used    9597
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.90
_cell_volume                     2071.5(3)
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0620
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            36416
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.568
_diffrn_reflns_theta_min         2.904
_exptl_absorpt_coefficient_mu    18.987
_exptl_absorpt_correction_T_max  0.058
_exptl_absorpt_correction_T_min  0.022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2016'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.266
_exptl_crystal_description       prism
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.150
_refine_diff_density_max         4.445
_refine_diff_density_min         -4.158
_refine_diff_density_rms         0.421
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.491(10)
_refine_ls_extinction_coef       0.00157(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         4194
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0549P)^2^+44.8752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.958
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4059
_reflns_number_total             4194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b02240_si_003.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        2071.5(4)
_cod_database_code               4516160
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.031
_shelx_estimated_absorpt_t_max   0.163
_shelx_res_checksum              17258
_shelx_hkl_checksum              34582