Mononuclear Platinum(II) and Palladium(II) Dithiolate Complexes as Chelate Metalloligands for Preparation of Heterobimetallic d8-d8 Complexes
Jorge Forniés-Cámer; Anna M. Masdeu-Bultó; Carmen Claver; Christine J. Cardin; Inorganic Chemistry 37 (1998) 2626–2632; doi:10.1021/ic970557o

data_4322808
_publ_section_title
;
 Mononuclear Platinum(II) and Palladium(II) Dithiolate Complexes as
 Chelate Metalloligands for Preparation of Heterobimetallic d8-d8
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2626
_journal_page_last               2632
_journal_paper_doi               10.1021/ic970557o
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'C40.50 H48 Cl2 O4 P2 Pd Rh S2'
_chemical_formula_structural     '[(dppb)Pd(BDT)Rh(COD)]ClO4'
_chemical_formula_sum            'C40.5 H48 Cl2 O4 P2 Pd Rh S2'
_chemical_formula_weight         1005.06
_chemical_name_systematic
; 
(1,4-bis(diphenylphosphino)buthane)palladium(II)(m-buthanodithiolate)
 (1,5-cyclooctadiene)rhodium(I)perchlorate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.04(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.365(6)
_cell_length_b                   14.186(6)
_cell_length_c                   14.592(6)
_cell_measurement_reflns_used    543
_cell_measurement_temperature    293
_cell_measurement_theta_max      28
_cell_measurement_theta_min      0
_cell_volume                     4138(3)
_computing_cell_refinement       'XDS package'
_computing_data_collection       'XDS package'
_computing_data_reduction        'XDS package'
_computing_molecular_graphics    PLATON
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Mar Research image plate scanner'
_diffrn_measurement_method       'prophile data from theta/2theta 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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9279
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  3
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.181
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       prism
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.288
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.0025(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   1.027
_refine_ls_goodness_of_fit_obs   1.056
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         5702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_obs          0.0507
_refine_ls_shift/esd_max         0.156
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1209P)^2^+4.4971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1745
_refine_ls_wR_factor_obs         0.1500
_reflns_number_observed          4452
_reflns_number_total             18274
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970557o_6.cif
_cod_data_source_block           12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1209P)^2^+4.4971P] 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^)+(0.1209P)^2^+4.4971P] 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        4137.6
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_original_formula_sum        'C40.50 H48 Cl2 O4 P2 Pd Rh S2'
_cod_database_code               4322808