Reactions of Palladium Germylene Complexes: Formation of Sulfide Bridges
Zuzanna T. Cygan; Jeff W. Kampf; Mark M. Banaszak Holl; Inorganic Chemistry 42 (2003) 7219–7226; doi:10.1021/ic034613z

data_4312425
_publ_section_title
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 Reactions of Palladium Germylene Complexes: Formation of Sulfide Bridges
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7219
_journal_page_last               7226
_journal_paper_doi               10.1021/ic034613z
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C42 H68 Ge N2 O P2 Pd S Si4'
_chemical_formula_weight         1002.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.421(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.3831(19)
_cell_length_b                   12.1176(5)
_cell_length_c                   22.3611(11)
_cell_measurement_temperature    158(2)
_cell_volume                     9976.2(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            126271
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_T_max  0.706
_exptl_absorpt_correction_T_min  0.584
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.58
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         12351
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+11.9786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                10918
_reflns_number_total             12351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034613zsi20030603_125230_3.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4312425