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_4516159
_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         'C4 H12 P, I'
_chemical_formula_sum            'C4 H12 I P'
_chemical_formula_weight         218.01
_space_group_crystal_system      tetragonal
_space_group_IT_number           129
_space_group_name_Hall           '-P 4a 2a'
_space_group_name_H-M_alt        'P 4/n m m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2018-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.1978(10)
_cell_length_b                   8.1978(10)
_cell_length_c                   6.0037(8)
_cell_measurement_reflns_used    5087
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      31.829
_cell_measurement_theta_min      3.515
_cell_volume                     403.47(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX3 Photon 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7940
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.518
_diffrn_reflns_theta_min         3.393
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.061
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.3871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1448 before and 0.0885 after correction. The Ratio of minimum to maximum transmission is 0.5186. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_description       prism
_exptl_crystal_F_000             208
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.015
_refine_diff_density_max         2.899
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     13
_refine_ls_number_reflns         448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.232
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0220P)^2^+2.5021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                399
_reflns_number_total             448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b02240_si_002.cif
_cod_data_source_block           mo_eo36_0m
_cod_original_cell_volume        403.47(11)
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_database_code               4516159
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.497
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H1A(0.5) H1C(0.5) H1B(0.5)
3.a Idealised Me refined as rotating group:
 C1(H1A,H1C,H1B)
;
_shelx_res_checksum              1903
_shelx_hkl_checksum              60157
_olex2_submission_special_instructions 'No special instructions were received'