Synthesis and Characterization of Zinc and Cadmium Compounds with Arenephosphinothiol Ligands. Crystal and Molecular Structures of [Cd2{2-(Ph2PO)C6H4S}4], [Zn{2-(Ph2P)-6-(Me3Si)C6H3S}2], [Cd{2-(Ph2PO)-6-(Me3Si)C6H3S}2(CH3OH)], and [Zn{PhPO(C6H4S-2)2}(bipy)]
Paulo Pérez-Lourido; Jaime Romero; José A. García-Vázquez; Antonio Sousa; Kevin P. Maresca; Jon Zubieta; Inorganic Chemistry 38 (1999) 3709–3715; doi:10.1021/ic981405b

data_4322173
_publ_section_title
;
 Synthesis and Characterization of Zinc and Cadmium Compounds with
 Arenephosphinothiol Ligands. Crystal and Molecular Structures of
 [Cd2{2-(Ph2PO)C6H4S}4], [Zn{2-(Ph2P)-6-(Me3Si)C6H3S}2],
 [Cd{2-(Ph2PO)-6-(Me3Si)C6H3S}2(CH3OH)], and [Zn{PhPO(C6H4S-2)2}(bipy)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3709
_journal_page_last               3715
_journal_paper_doi               10.1021/ic981405b
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C46 H50 N2 P2 S2 Si2 Zn'
_chemical_formula_weight         878.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 113.84(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.332(4)
_cell_length_b                   9.391(2)
_cell_length_c                   25.938(5)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     4753(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nicolet P3'
_diffrn_measurement_method       theta/2theta
_diffrn_radiation_monochromator  beta-filter
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            4546
_diffrn_reflns_theta_max         57.46
_diffrn_reflns_theta_min         4.53
_diffrn_standards_decay_%        1.3
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.899
_exptl_absorpt_correction_T_max  .663
_exptl_absorpt_correction_T_min  .439
_exptl_absorpt_correction_type   numeric
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.00062(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.029
_refine_ls_goodness_of_fit_obs   1.030
_refine_ls_hydrogen_treatment    refined
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         2564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_restrained_S_obs      1.030
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_obs          0.0377
_refine_ls_shift/esd_max         -0.627
_refine_ls_shift/esd_mean        0.173
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+5.5423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0953
_refine_ls_wR_factor_obs         0.0949
_reflns_number_observed          2540
_reflns_number_total             2564
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981405b_2.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+5.5423P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+5.5423P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4752.8(16)
_cod_database_code               4322173