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_7027746
_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            'C24 H26 Cl2 N3 P Pd S'
_chemical_formula_weight         596.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.20(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.366(3)
_cell_length_b                   9.174(2)
_cell_length_c                   18.525(3)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.949
_cell_measurement_theta_min      9.366
_cell_volume                     2531.6(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5653
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        9.92
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.107
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.273
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.150
_refine_ls_goodness_of_fit_obs   1.189
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4446
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.153
_refine_ls_restrained_S_obs      1.189
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_obs          0.0500
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+2.7320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1468
_refine_ls_wR_factor_obs         0.1393
_reflns_number_observed          3794
_reflns_number_total             4448
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            906276isup1.cif
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+2.7320P] 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^)+(0.0822P)^2^+2.7320P] 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        2531.6(8)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027746