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_7012868
_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            'C92.5 H101 N O5.5 P4 Pd4 S3'
_chemical_formula_weight         1960.40
_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                71.32(2)
_cell_angle_beta                 85.57(2)
_cell_angle_gamma                87.920(14)
_cell_formula_units_Z            2
_cell_length_a                   13.822(3)
_cell_length_b                   15.464(4)
_cell_length_c                   23.567(7)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      11.11
_cell_volume                     4757(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      293(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  0.0909
_diffrn_reflns_av_sigmaI/netI    0.1128
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14632
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         1.98
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.628
_exptl_absorpt_correction_T_max  0.4643
_exptl_absorpt_correction_T_min  0.0465
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Orange/red
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       rhombs
_exptl_crystal_F_000             1998
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.309
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.00134(12)
_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   1.033
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         12361
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.078
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_obs          0.0890
_refine_ls_shift/esd_max         0.024
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1401P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2663
_refine_ls_wR_factor_obs         0.2158
_reflns_number_observed          8535
_reflns_number_total             13957
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b302034g.txt
_cod_data_source_block           Compound_7
_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^)+(0.1401P)^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^)+(0.1401P)^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        4757.3(20)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C92.50 H101 N O5.50 P4 S3 Pd4'
_cod_database_code               7012868