Diphenyllead(IV) chloride complexes with benzilthiosemicarbazones. The first bis(thiosemicarbazone) derivatives.
Calatayud, David G.; López-Torres, Elena; Mendiola, M. Antonia; Inorganic chemistry 46 (2007) 10434–10443; doi:10.1021/ic701490j

data_4339363
_publ_section_title
;
 Diphenyllead(IV) chloride complexes with benzilthiosemicarbazones. The
 first bis(thiosemicarbazone) derivatives.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10434
_journal_page_last               10443
_journal_paper_doi               10.1021/ic701490j
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         'C30 H28 N6 Pb S2, H2 O'
_chemical_formula_sum            'C30 H30 N6 O Pb S2'
_chemical_formula_weight         761.94
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.1671(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8952(2)
_cell_length_b                   9.6592(2)
_cell_length_c                   24.3891(5)
_cell_measurement_reflns_used    33974
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     2957.98(10)
_computing_cell_refinement
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
KappaCCD software 'Collect' (Nonius, 2000) 
;
_computing_data_reduction
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_publication_material
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_refinement
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
; 
Nonius KappaCCD 
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            33974
_diffrn_reflns_theta_full        27.475
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         5.151
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.879
_exptl_absorpt_correction_T_max  0.49
_exptl_absorpt_correction_T_min  0.19
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' brown-yellow '
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_thermal_history
; 
The material was crystallised at ambient temperature. A suitable crystal 
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. 
;
_refine_diff_density_max         1.27
_refine_diff_density_min         -1.34
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0618
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4888
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.018113
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.632 0.180 0.432 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0462
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0357
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                4888
_reflns_number_total             6719
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic701490j-file003.cif
_cod_data_source_block           arc1537
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

2021-09-13
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1523.88
_cod_original_formula_moiety         ' C60 H56 N12 Pb2 S4, 2 (H2 O) '
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C60 H60 N12 O2 Pb2 S4 '
_cod_database_code               4339363