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_7012869
_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            'C94 H97 N O5 P4 Pd4 S3'
_chemical_formula_weight         1966.39
_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                83.375(5)
_cell_angle_beta                 67.888(5)
_cell_angle_gamma                72.737(7)
_cell_formula_units_Z            2
_cell_length_a                   15.8551(8)
_cell_length_b                   16.7489(9)
_cell_length_c                   18.9814(8)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      10.58
_cell_volume                     4459.5(4)
_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      193(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  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13799
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         2.51
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.137
_exptl_absorpt_correction_T_max  0.4845
_exptl_absorpt_correction_T_min  0.0551
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Deep red'
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       rhombs
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.211
_refine_diff_density_min         -4.949
_refine_diff_density_rms         0.203
_refine_ls_extinction_coef       0.00021(4)
_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   1.054
_refine_ls_goodness_of_fit_obs   1.115
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         12259
_refine_ls_number_restraints     1300
_refine_ls_restrained_S_all      1.049
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_all          0.1714
_refine_ls_R_factor_obs          0.1332
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+166.4998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3408
_refine_ls_wR_factor_obs         0.3034
_reflns_number_observed          9944
_reflns_number_total             13214
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b302034g.txt
_cod_data_source_block           Compound_8
_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.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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^)+(0.0917P)^2^+166.4998P] 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^)+(0.0917P)^2^+166.4998P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012869