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_4312426
_publ_section_title
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 Reactions of Palladium Germylene Complexes: Formation of Sulfide Bridges
;
_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 H108 Ge2 N4 P2 Pd2 S2 Si8'
_chemical_formula_weight         1378.08
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.478(2)
_cell_angle_beta                 112.702(2)
_cell_angle_gamma                90.475(2)
_cell_formula_units_Z            1
_cell_length_a                   11.2870(13)
_cell_length_b                   12.7506(15)
_cell_length_c                   13.1569(15)
_cell_measurement_reflns_used    7856
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      3.42
_cell_volume                     1670.2(3)
_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_detector_area_resol_mean 0.75
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21115
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    1.705
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   multi.scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.6641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                7375
_reflns_number_total             8130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034613zsi20030603_125230_4.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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               4312426