Formation, characterization, and structural studies of novel thiosemicarbazone palladium(II) complexes. Crystal structures of [{Pd[C6H4C(Et)NNC(S)NH2]}4], [Pd{C6H4C(Et)NN C(S)NH2}(PMePh2)] and [{Pd[C6H4C(Et)NNC(S)NH2]}2(μ-Ph2PCH2PPh2)]
Vila, José M.; Pereira, Ma Teresa; Ortigueira, Juan M.; Graña, María; Lata, Darío; Suárez, Antonio; Fernández, Jesús J.; Fernández, Alberto; López-Torres, Margarita; Adams, Harry; Journal of the Chemical Society, Dalton Transactions  (1999) 4193–; doi:10.1039/a906276i

data_7027747
_publ_section_title
;
 Formation, characterization, and structural studies of novel
 thiosemicarbazone palladium(II) complexes. Crystal structures of
 [{Pd[C6H4C(Et)&#xE006;NN&#xE006;C(S)NH2]}4],
 [Pd{C6H4C(Et)&#xE006;NN&#xE006; C(S)NH2}(PMePh2)] and
 [{Pd[C6H4C(Et)&#xE006;NN&#xE006;C(S)NH2]}2(\m-Ph2PCH2PPh2)]
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4193
_journal_paper_doi               10.1039/a906276i
_journal_year                    1999
_chemical_formula_sum            'C51 H56 N6 O2 P2 Pd2 S2'
_chemical_formula_weight         1123.88
_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-97
_cell_angle_alpha                93.9370(10)
_cell_angle_beta                 90.9930(10)
_cell_angle_gamma                92.30
_cell_formula_units_Z            4
_cell_length_a                   13.8547(2)
_cell_length_b                   17.8565(2)
_cell_length_c                   21.11840(10)
_cell_measurement_temperature    293(2)
_cell_volume                     5207.03(10)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  '\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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.1136
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27248
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.97
_diffrn_standards_decay_%        '< 1'
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7589
_exptl_absorpt_correction_type   'empirical using SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         17986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+3.2609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1424
_reflns_number_gt                10201
_reflns_number_total             17986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906276isup1.cif
_cod_data_source_block           7b'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+3.2609P] 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^)+(0.0418P)^2^+3.2609P] 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        5207.02(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027747