Lead(II) complexes with phosphorylthiolato and thiophosphorylthiolato ligands
Pérez-Lourido, Paulo; Romero, Jaime; García-Vázquez, José A.; Sousa, Antonio; Zheng, Yifan; Dilworth, Jonathan R.; Zubieta, Jon; Journal of the Chemical Society, Dalton Transactions  (2000) 769–; doi:10.1039/a908496g

data_7009080
_publ_section_title
;
 Lead(II) complexes with phosphorylthiolato and thiophosphorylthiolato
 ligands
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              769
_journal_paper_doi               10.1039/a908496g
_journal_year                    2000
_chemical_formula_sum            'C64 H54 P4 Pb S6'
_chemical_formula_weight         1346.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.014(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.212(3)
_cell_length_b                   14.4198(10)
_cell_length_c                   25.146(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      16
_cell_volume                     5874.8(14)
_computing_cell_refinement       'CAD-4 (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 (Enraf-Nonius, 1989)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1994)'
_computing_publication_material  'SHELXL-96 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 '
_diffrn_measurement_method       \w-2\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            5678
_diffrn_reflns_theta_max         25.52
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.234
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       brick
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.358
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.037(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.035
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         5678
_refine_ls_number_restraints     2
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_refine_ls_restrained_S_obs      1.125
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_obs          0.0362
_refine_ls_shift/esd_max         0.108
_refine_ls_shift/esd_mean        0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.3420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1003
_refine_ls_wR_factor_obs         0.0849
_reflns_number_observed          3702
_reflns_number_total             5678
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908496g.txt
_cod_data_source_block           compound6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Psi-scan' changed to 'psi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.3420P] 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^)+(0.0583P)^2^+0.3420P] 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        5874.9(14)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7009080