Synthesis and structural characterisation of the palladium cluster compounds [Pd3(μ-SO2)2(μ-PPh2py)2(PBz3)2] and [Pd4(μ-SO2)2(μ3-S)(CNR)(PBz3)4] (R =tBu, 2,6-dimethylphenyl and cyclohexyl)
Anna M. Williamson; Gareth R. Owen; D. Michael P. Mingos; Ramón Vilar; Andrew J. P. White; David J. Williams; Dalton Trans.  (2003) 2526–2532; doi:10.1039/b302034g

data_7012866
_publ_section_title
;
 Synthesis and structural characterisation of the palladium cluster
 compounds [Pd3(\m-SO2)2(\m-PPh2py)2(PBz3)2] and
 [Pd4(\m-SO2)2(\m3-S)(CNR)(PBz3)4]&#x00A0;(R =tBu, 2,6-dimethylphenyl
 and cyclohexyl)
;
_journal_issue                   12
_journal_name_full               'Dalton Trans.'
_journal_page_first              2526
_journal_page_last               2532
_journal_paper_doi               10.1039/b302034g
_journal_year                    2003
_chemical_formula_sum            'C79 H76 Cl6 N2 O4 P4 Pd3 S2'
_chemical_formula_weight         1837.32
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                95.190(9)
_cell_angle_beta                 100.051(8)
_cell_angle_gamma                97.313(7)
_cell_formula_units_Z            2
_cell_length_a                   13.9578(11)
_cell_length_b                   14.4750(12)
_cell_length_c                   20.1575(15)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      11.28
_cell_volume                     3950.9(6)
_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      203(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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12271
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         2.24
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.971
_exptl_absorpt_correction_T_max  0.4395
_exptl_absorpt_correction_T_min  0.3205
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.926
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.00054(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.036
_refine_ls_goodness_of_fit_obs   1.065
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         10994
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.093
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_obs          0.0526
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+6.6648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1424
_refine_ls_wR_factor_obs         0.1235
_reflns_number_observed          9349
_reflns_number_total             11712
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b302034g.txt
_cod_data_source_block           Compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+6.6648P] 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^)+(0.0707P)^2^+6.6648P] 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        3950.9(5)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C79 H76 N2 O4 P4 S2 Cl6 Pd3'
_cod_database_code               7012866