#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:01:31 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180244 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/30/7113037.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_7113037
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 P4 Ru'
_chemical_formula_sum            'Cl2 H12 P4 Ru'
_chemical_formula_weight         307.97
_chemical_name_systematic        trans-dichloridotetraphosphaneruthenium
_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                   6.5817(9)
_cell_length_b                   6.5817(9)
_cell_length_c                   11.726(2)
_cell_measurement_reflns_used    593
_cell_measurement_temperature    153(1)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     507.96(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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            996
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.55
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Nonius KappaCCD'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.616
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinoski and Minor, 1997)'
_exptl_crystal_colour            'intense yellow'
_exptl_crystal_density_diffrn    2.013
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'clear tetragonal crystals'
_exptl_crystal_F_000             300
_exptl_crystal_recrystallization_method
'crystallized from methanol at -50 °C'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     26
_refine_ls_number_reflns         339
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0160
_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)+(0.0000P)²+0.1820P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0364
_refine_ls_wR_factor_ref         0.0373
_reflns_number_gt                313
_reflns_number_total             339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc01231a.txt
_cod_data_source_block           trans-RuCl2(PH3)4
_cod_database_code               7113037
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
Ru1 Ru 0.5000 0.5000 0.0000 0.02161(14) Uani 1 8 d SD . .
Cl1 Cl 0.23920(9) 0.23920(9) 0.0000 0.0365(2) Uani 1 4 d S . .
P1 P 0.67916(7) 0.32084(7) 0.13618(5) 0.03079(19) Uani 1 2 d SD . .
H1 H 0.6471(15) 0.3529(15) 0.2405(9) 0.053(8) Uiso 0.77(3) 2 d SPD A 1
H2 H 0.8699(16) 0.3328(13) 0.1398(9) 0.053(8) Uiso 0.77(3) 1 d PD A 1
H1Z H 0.8090(11) 0.1910(11) 0.1063(12) 0.053(8) Uiso 0.23(3) 2 d SPD A 2
H2Z H 0.7890(10) 0.414(2) 0.2069(7) 0.053(8) Uiso 0.23(3) 1 d PD 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
Ru1 0.02218(16) 0.02218(16) 0.0205(2) 0.000 0.000 0.00075(13)
Cl1 0.0340(3) 0.0340(3) 0.0414(5) 0.000 0.000 -0.0105(4)
P1 0.0324(2) 0.0324(2) 0.0276(3) 0.00396(19) -0.00396(19) 0.0028(2)
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 '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 Ru1 P1 92.48(3) . 3_665
P1 Ru1 P1 180.0 . 9_665
P1 Ru1 P1 87.52(3) 3_665 9_665
P1 Ru1 P1 87.52(3) . 11
P1 Ru1 P1 180.0 3_665 11
P1 Ru1 P1 92.48(3) 9_665 11
P1 Ru1 Cl1 90.0 . .
P1 Ru1 Cl1 90.0 3_665 .
P1 Ru1 Cl1 90.0 9_665 .
P1 Ru1 Cl1 90.0 11 .
P1 Ru1 Cl1 90.0 . 9_665
P1 Ru1 Cl1 90.0 3_665 9_665
P1 Ru1 Cl1 90.0 9_665 9_665
P1 Ru1 Cl1 90.0 11 9_665
Cl1 Ru1 Cl1 180.0 . 9_665
Ru1 P1 H1 120.1(6) . .
Ru1 P1 H2 120.1(6) . .
H1 P1 H2 97.1(8) . .
Ru1 P1 H1Z 120.1(6) . .
H1 P1 H1Z 119.9(12) . .
H2 P1 H1Z 51.3(3) . .
Ru1 P1 H2Z 120.1(6) . .
H1 P1 H2Z 51.3(3) . .
H2 P1 H2Z 51.3(4) . .
H1Z P1 H2Z 97.1(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 P1 2.3088(7) .
Ru1 P1 2.3088(7) 3_665
Ru1 P1 2.3088(7) 9_665
Ru1 P1 2.3088(7) 11
Ru1 Cl1 2.4275(9) .
Ru1 Cl1 2.4275(9) 9_665
P1 H1 1.259(10) .
P1 H2 1.259(10) .
P1 H1Z 1.259(10) .
P1 H2Z 1.259(10) .
