Reactivity of the palladium dimer [Pd2(μ-SO2)(μ-dba)(PBz3)2]. Syntheses and structural characterisation of [Pd3(μ-SO2)3(PBz3)3], [Pd2(μ-SO2)(μ-dppm)(PBz3)2], [Pd(SO2)(PBz3)2], [Pd3(μ-CO)2(μ-SO2)(PBz3)3] and [Pd3(μ-SO2)2(CNBut )2(PBz3)3] (Bz = benzyl) †
Arifhodzic-Radojevic, Sanja; Burrows, Andrew D.; Choi, Nick; McPartlin, Mary; Mingos, D. Michael P.; Tarlton, Stephen V.; Vilar, Ramón; Journal of the Chemical Society, Dalton Transactions  (1999) 3981–; doi:10.1039/a906444c

data_7027755
_publ_section_title
;
 Reactivity of the palladium dimer [Pd2(\m-SO2)(\m-dba)(PBz3)2]. Syntheses
 and structural characterisation of [Pd3(\m-SO2)3(PBz3)3],
 [Pd2(\m-SO2)(\m-dppm)(PBz3)2], [Pd(SO2)(PBz3)2],
 [Pd3(\m-CO)2(\m-SO2)(PBz3)3] and [Pd3(\m-SO2)2(CNBut&#x200A;)2(PBz3)3]
 (Bz&#x2005;=&#x2005;benzyl)&#x200A;&#x2020;
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3981
_journal_paper_doi               10.1039/a906444c
_journal_year                    1999
_chemical_formula_sum            'C63 H63 O6 P3 Pd3 S3'
_chemical_formula_weight         1424.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   24.985(2)
_cell_length_b                   24.985(2)
_cell_length_c                   16.219(3)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      12.46
_cell_measurement_theta_min      4.88
_cell_volume                     8768.3(19)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'Theta/2 theta'
_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  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0750
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4121
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  -
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  0.755360
_exptl_absorpt_correction_T_min  0.325522
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   -
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.366
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+74.1161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                2219
_reflns_number_total             3354
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906444csup1.cif
_cod_data_source_block           ab347
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value '-' 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 
;
_cod_original_cell_volume        8768.0(19)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7027755