Reactions of {[Pd(μ-SC6F5)(μ-dppm)Pd](μ-SC6F5)}4.2O(C2H5)2. Crystal Structures of the Complexes [(Ph3P)Pd(μ-SC6F5)(μ-dppm)Pd(SC6F5)].1.4CH2Cl2 and [(Ph3P)Pd(μ-SC6F5)(μ-dppm)Pd(PPh3)]SO3CF3.2CH2Cl2 and ab Initio MO Calculations on the Model Systems [(H3P)Pd(μ-H2PCH2PH2)(μ-SH)Pd(PH3)]+ and [(H3P)Pd(μ-H2PCH2PH2)Pd(PH3)]2+
Rafael Usón; Juan Forniés; Javier Fernández Sanz; Miguel A. Usón; Isabel Usón; Santiago Herrero; Inorganic Chemistry 36 (1997) 1912–1922; doi:10.1021/ic960818e

data_4323390
_publ_section_title
;
 Reactions of {[Pd(\m-SC6F5)(\m-dppm)Pd](\m-SC6F5)}4.2O(C2H5)2. Crystal
 Structures of the Complexes
 [(Ph3P)Pd(\m-SC6F5)(\m-dppm)Pd(SC6F5)].1.4CH2Cl2 and
 [(Ph3P)Pd(\m-SC6F5)(\m-dppm)Pd(PPh3)]SO3CF3.2CH2Cl2 and ab Initio MO
 Calculations on the Model Systems [(H3P)Pd(\m-H2PCH2PH2)(\m-SH)Pd(PH3)]+
 and [(H3P)Pd(\m-H2PCH2PH2)Pd(PH3)]2+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1912
_journal_page_last               1922
_journal_paper_doi               10.1021/ic960818e
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C70 H56 Cl4 F8 O3 P4 Pd2 S2'
_chemical_formula_weight         '1489.88 + 149.87'
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.804(2)
_cell_length_b                   17.659(2)
_cell_length_c                   27.795(3)
_cell_measurement_reflns_used    72
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     13647(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_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      153(2)
_diffrn_measurement_device       'Siemens-Stoe AED2'
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            15938
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        <3
_diffrn_standards_interval_count 90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  0.9449
_exptl_absorpt_correction_T_min  0.6486
_exptl_absorpt_correction_type   'psi-scans,laminar correction'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       plates
_exptl_crystal_F_000             6592
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.005
_refine_ls_goodness_of_fit_obs   1.026
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1757
_refine_ls_number_reflns         15768
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.007
_refine_ls_restrained_S_obs      1.028
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_obs          0.0555
_refine_ls_shift/esd_max         2.588
_refine_ls_shift/esd_mean        0.053
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+43.3824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1341
_refine_ls_wR_factor_obs         0.1222
_reflns_number_observed          12873
_reflns_number_total             15768
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960818e_1.cif
_cod_data_source_block           5c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+43.3824P] 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^)+(0.0625P)^2^+43.3824P] 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        13646.8(20)
_cod_original_formula_sum        'C68 H52 F8 O3 P4 Pd2 S2 C2 Cl4 H4'
_cod_database_code               4323390