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_4322195
_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            'C42 H37 Cd N3 O2 P2 S2'
_chemical_formula_weight         854.10
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                106.622(1)
_cell_angle_beta                 109.693(1)
_cell_angle_gamma                107.137(1)
_cell_formula_units_Z            2
_cell_length_a                   13.5780(2)
_cell_length_b                   13.8505(2)
_cell_length_c                   13.9526(2)
_cell_measurement_reflns_used    '60 frames'
_cell_measurement_temperature    298(2)
_cell_volume                     2133.30(7)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'Siemens XCIF'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13594
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.5963
_exptl_absorpt_correction_T_min  0.7081
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.449
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.082
_refine_ls_hydrogen_treatment    idealized
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9556
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_obs          0.0483
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(?P)^2^+?P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1613
_refine_ls_wR_factor_obs         0.1460
_reflns_number_total             9560
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981405b_1.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(?P)^2^+?P] 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^)+(?P)^2^+?P] 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        2133.30(5)
_cod_original_formula_sum        'C42 H37 N3 O2 P2 S2 Cd'
_cod_database_code               4322195