Synthesis, Molecular Structure, and Reactivity of the Tetranuclear Complex [NBu4]2[Pd4(μ-PPh2)2(μ-Cl)4(C6F5)4]. Molecular Structure of [Pd2(μ-PPh2)(C6F5)2(bipy)2]ClO4.C6H14
Ester Alonso; Juan Forniés; Consuelo Fortuño; Antonio Martín; Georgina M. Rosair; Alan J. Welch; Inorganic Chemistry 36 (1997) 4426–4431; doi:10.1021/ic9701930

data_4323590
_publ_section_title
;
 Synthesis, Molecular Structure, and Reactivity of the Tetranuclear
 Complex [NBu4]2[Pd4(\m-PPh2)2(\m-Cl)4(C6F5)4]. Molecular Structure of
 [Pd2(\m-PPh2)(C6F5)2(bipy)2]ClO4.C6H14
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4426
_journal_page_last               4431
_journal_paper_doi               10.1021/ic9701930
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C50 H40 Cl F10 N4 O4 P Pd2'
_chemical_formula_weight         1230.08
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.214(3)
_cell_length_b                   10.311(2)
_cell_length_c                   28.380(6)
_cell_measurement_reflns_used    247
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2.51
_cell_volume                     4660.3(17)
_computing_cell_refinement       'MADNES (1991)'
_computing_data_collection       'MADNES (1991)'
_computing_data_reduction        'MADNES (1991)'
_computing_molecular_graphics    'SHELXTL (Siemens, Sheldrick 1994)'
_computing_publication_material  'SHELXTL (Siemens, Sheldrick 1994)'
_computing_structure_refinement  'SHELXTL (Siemens, Sheldrick 1994)'
_computing_structure_solution    'SHELXTL (Siemens, Sheldrick 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius FAST diffractometer'
_diffrn_measurement_method       'MADNES (1991) 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  0.0765
_diffrn_reflns_av_sigmaI/netI    0.1351
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18297
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.955
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.846
_refine_ls_goodness_of_fit_obs   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         7104
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      0.848
_refine_ls_restrained_S_obs      1.001
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_obs          0.0398
_refine_ls_shift/esd_max         -0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0875
_refine_ls_wR_factor_obs         0.0829
_reflns_number_observed          4782
_reflns_number_total             7104
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9701930.cif
_cod_data_source_block           Complex7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.0000P] 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^)+(0.0304P)^2^+0.0000P] 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        4660.3(16)
_cod_database_code               4323590