Mass spectrometry-directed synthesis of 'early–late' sulfide-bridged heterobimetallic complexes from the metalloligand [Pt2(PPh3)4(µ-S)2] and oxo compounds of vanadium(v), molybdenum(vi) and uranium(vi)
Fong, S.-W. Audi; Yap, Woon Teck; Vittal, Jagadese J.; Henderson, William; Hor, T. S. Andy; Journal of the Chemical Society, Dalton Transactions  (2002) 1826–; doi:10.1039/b107939p

data_7011137
_publ_section_title
;
 Mass spectrometry-directed synthesis of 'early--late' sulfide-bridged
 heterobimetallic complexes from the metalloligand
 [Pt2(PPh3)4(&#x00B5;-S)2] and oxo compounds of vanadium(v),
 molybdenum(vi) and uranium(vi)
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1826
_journal_paper_doi               10.1039/b107939p
_journal_year                    2002
_chemical_formula_sum            'C72 H60 N2 O8 P4 Pt2 S2 U'
_chemical_formula_weight         1897.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 115.2910(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.5463(9)
_cell_length_b                   14.2378(6)
_cell_length_c                   23.8747(10)
_cell_measurement_reflns_used    6710
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.6
_cell_measurement_theta_min      2.3
_cell_volume                     6929.4(5)
_computing_cell_refinement       'Bruker AXS, SAINT'
_computing_data_collection       'Bruker AXS, SMART'
_computing_data_reduction        'Bruker AXS, SAINT'
_computing_molecular_graphics    'Bruker AXS, SHELXTL'
_computing_publication_material  'Bruker AXS, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_method       '\w 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  0.0659
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39879
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    6.567
_exptl_absorpt_correction_T_max  0.5454
_exptl_absorpt_correction_T_min  0.4493
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'long rod cut'
_exptl_crystal_F_000             3640
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.306
_refine_diff_density_min         -1.422
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         12198
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0484
_reflns_number_gt                8557
_reflns_number_total             12198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b107939p.txt
_cod_data_source_block           1141
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7011137