#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:01:31 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180244 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/30/7113036.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7113036
loop_
_publ_author_name
'Hall, Justin W.'
'Yang, Xiaoping'
'Jones, Richard A.'
_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
'φ-scans and ω-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/[σ²(Fo²)+(0.0120P)²+0.9560P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x+1/2, z+1/2'
'-x, -y, z'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'-y, -x, -z'
'-x, -y, -z'
'y-1/2, -x-1/2, -z-1/2'
'x, y, -z'
'-y-1/2, x-1/2, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'-y, -x, z'
'x-1/2, -y-1/2, z-1/2'
'y, x, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.5000 0.5000 0.0000 0.02333(14) Uani 1 8 d SD . .
Cl1 Cl 0.23727(19) 0.23727(19) 0.0000 0.0367(4) Uani 1 4 d S . .
P1 P 0.32129(14) 0.67871(14) 0.13659(12) 0.0327(3) Uani 1 2 d SD . .
H1 H 0.3565(19) 0.6435(19) 0.2474(12) 0.050(14) Uiso 0.76(5) 2 d SPD A 1
H2 H 0.3345(17) 0.882(2) 0.1405(12) 0.050(14) Uiso 0.76(5) 1 d PD A 1
H2Z H 0.421(3) 0.7953(14) 0.2117(10) 0.050(14) Uiso 0.24(5) 1 d PD A 2
H1Z H 0.1827(15) 0.8173(15) 0.1048(15) 0.050(14) Uiso 0.24(5) 2 d SPD A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os1 0.02466(16) 0.02466(16) 0.0207(2) 0.000 0.000 0.00181(16)
Cl1 0.0360(6) 0.0360(6) 0.0382(9) 0.000 0.000 -0.0096(7)
P1 0.0353(4) 0.0353(4) 0.0277(6) -0.0034(4) 0.0034(4) 0.0053(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
P1 Os1 P1 92.03(7) 9_665 11
P1 Os1 P1 87.97(7) 9_665 3_665
P1 Os1 P1 180.00(5) 11 3_665
P1 Os1 P1 180.00(4) 9_665 .
P1 Os1 P1 87.97(7) 11 .
P1 Os1 P1 92.03(7) 3_665 .
P1 Os1 Cl1 90.0 9_665 9_665
P1 Os1 Cl1 90.0 11 9_665
P1 Os1 Cl1 90.0 3_665 9_665
P1 Os1 Cl1 90.0 . 9_665
P1 Os1 Cl1 90.0 9_665 .
P1 Os1 Cl1 90.0 11 .
P1 Os1 Cl1 90.0 3_665 .
P1 Os1 Cl1 90.0 . .
Cl1 Os1 Cl1 180.0 9_665 .
Os1 P1 H1 119.9(8) . .
Os1 P1 H2 119.9(8) . .
H1 P1 H2 97.4(10) . .
Os1 P1 H2Z 119.9(8) . .
H1 P1 H2Z 51.4(4) . .
H2 P1 H2Z 51.4(4) . .
Os1 P1 H1Z 119.9(8) . .
H1 P1 H1Z 120.3(15) . .
H2 P1 H1Z 51.4(4) . .
H2Z P1 H1Z 97.4(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os1 P1 2.3099(13) 9_665
Os1 P1 2.3099(13) 11
Os1 P1 2.3099(13) 3_665
Os1 P1 2.3099(13) .
Os1 Cl1 2.4433(18) 9_665
Os1 Cl1 2.4433(18) .
P1 H1 1.342(14) .
P1 H2 1.342(14) .
P1 H2Z 1.342(14) .
P1 H1Z 1.342(14) .
