Syntheses of Selenolato-Bridged Dinuclear Hydridoplatinum Complexes [Pt2H2(μ-SetBu)2(PPh3)2] and [Pt2H(SetBu)(μ-SetBu)2(PPh3)2]: Unusual Thermal Reaction of Hydrido(1,1-Dimethylethaneselenolato) Platinum Complex cis-[PtH(SetBu)(PPh3)2]
Norio Nakata; Takashige Ikeda; Akihiko Ishii; Inorganic Chemistry 49 (2010) 8112–8116; doi:10.1021/ic1011742

data_4316447
_publ_section_title
;
 Syntheses of Selenolato-Bridged Dinuclear Hydridoplatinum Complexes
 [Pt2H2(\m-SetBu)2(PPh3)2] and [Pt2H(SetBu)(\m-SetBu)2(PPh3)2]: Unusual
 Thermal Reaction of Hydrido(1,1-Dimethylethaneselenolato) Platinum
 Complex cis-[PtH(SetBu)(PPh3)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8112
_journal_page_last               8116
_journal_paper_doi               10.1021/ic1011742
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C44 H50 P2 Pt2 Se2, C H2 Cl2'
_chemical_formula_sum            'C45 H52 Cl2 P2 Pt2 Se2'
_chemical_formula_weight         1273.81
_chemical_name_common            '[Pt2H2(SetBu)2(PPh3)2]_CH2Cl2'
_chemical_name_systematic
; 
 [Pt2H2(SetBu)2(PPh3)2]_CH2Cl2 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 105.471(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.169(3)
_cell_length_b                   10.802(2)
_cell_length_c                   26.764(5)
_cell_measurement_temperature    103(2)
_cell_volume                     4505.2(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            24786
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    8.040
_exptl_absorpt_correction_T_max  0.3255
_exptl_absorpt_correction_T_min  0.2118
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            paleyellow
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.877
_refine_diff_density_min         -1.566
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         8365
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0575P)^2^+14.1512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                6453
_reflns_number_total             8365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1011742_si_003.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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        4505.0(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4316447