Syntheses and structures of the tetra-phosphine complexes trans-MCl2(PH3)4 (M = Ru, Os).
Hall, Justin W.; Yang, Xiaoping; Jones, Richard A.; Chemical communications (Cambridge, England) 46 (2010) 6168–6170; doi:10.1039/c0cc01231a

data_7113036
_publ_section_title
;
 Syntheses and structures of the tetra-phosphine complexes
 trans-MCl2(PH3)4 (M = Ru, Os).
;
_journal_issue                   33
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6168
_journal_page_last               6170
_journal_paper_doi               10.1039/c0cc01231a
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'Cl2 H12 Os P4'
_chemical_formula_sum            'Cl2 H12 Os P4'
_chemical_formula_weight         397.10
_chemical_name_systematic        trans-dichloridotetraphosphaneosmium
_space_group_IT_number           136
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      136
_symmetry_space_group_name_Hall  '-P 4n 2n'
_symmetry_space_group_name_H-M   'P 42/m n m'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.5759(9)
_cell_length_b                   6.5759(9)
_cell_length_c                   11.744(2)
_cell_measurement_reflns_used    1165
_cell_measurement_temperature    153(1)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     507.84(13)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction        'Denzo (Otwinoski and Minor, 1997)'
_computing_molecular_graphics    'XP SHELXTL/PC v5.1, Bruker AXS'
_computing_structure_refinement  'XL SHELXTL/PC v5.1, Bruker AXS'
_computing_structure_solution    'XS SHELXTL/PC v5.1, Bruker AXS'
_diffrn_ambient_temperature      153(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
'\f-scans and \w-scans to fill asymmetric unit'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2954
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Nonius KappaCCD'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.628
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinoski and Minor, 1997)'
_exptl_crystal_colour            'intense yellow'
_exptl_crystal_density_diffrn    2.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'clear tetragonal crystals'
_exptl_crystal_F_000             364
_exptl_crystal_recrystallization_method
'crystallized from methanol at -50 \%C'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.173
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     26
_refine_ls_number_reflns         344
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+0.9560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0375
_refine_ls_wR_factor_ref         0.0393
_reflns_number_gt                302
_reflns_number_total             344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc01231a.txt
_cod_data_source_block           trans-OsCl2(PH3)4
_cod_database_code               7113036