Lead(IV) complexes with phosphinoyldithioformates, R2P(O)CS2− (R = Ph or PhCH2). Syntheses and characterization. Crystal structures of [PPh4][S2CP(O)Ph2]·0.5H2O, [PbPh2{S2CP(O)Ph2}2] and [PbPh2Cl{S2CP(O)Ph2}]
Ólafsson, Sigurjón Norberg; Flensburg, Claus; Andersen, Peter; Journal of the Chemical Society, Dalton Transactions  (2000) 4360–; doi:10.1039/b006672i

data_7010182
_publ_section_title
;
 Lead(IV) complexes with phosphinoyldithioformates, R2P(O)CS2&#x2212;
 (R&#x2005;=&#x2005;Ph or PhCH2). Syntheses and characterization.
 Crystal structures of [PPh4][S2CP(O)Ph2]&#x00B7;0.5H2O,
 [PbPh2{S2CP(O)Ph2}2] and [PbPh2Cl{S2CP(O)Ph2}]
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4360
_journal_paper_doi               10.1039/b006672i
_journal_year                    2000
_chemical_formula_sum            'C74 H62 O3 P4 S4'
_chemical_formula_weight         1251.36
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.221(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1216(14)
_cell_length_b                   41.242(8)
_cell_length_c                   9.3324(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    122(1)
_cell_measurement_theta_max      40.28
_cell_measurement_theta_min      37.37
_cell_volume                     3122.0(9)
_computing_cell_refinement       'NONIUS CAD4'
_computing_data_collection       'NONIUS CAD4'
_computing_data_reduction        'DREADD (Blessing, 1989)'
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14683
_diffrn_reflns_theta_full        74.93
_diffrn_reflns_theta_max         74.93
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        4.9
_diffrn_standards_interval_time  '10000 seconds'
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    2.755
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.436
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'ABSORB (DeTitta, 1985)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.887
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         12808
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.887
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                12598
_reflns_number_total             12808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006672i.txt
_cod_data_source_block           L
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        3121.9(8)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7010182