#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:07:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180223 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/09/7110941.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7110941
loop_
_publ_author_name
'van der Schaaf, Paul A.'
'Kolly, Roman'
'Hafner, Andreas'
_publ_section_title
;
 A 14-electron ruthenium hydride: the key intermediate in the synthesis of
 ruthenium carbene complexes; X-ray structure of [RuHCl(PPri3)2]
;
_journal_issue                   12
_journal_name_full               'Chemical Communications'
_journal_page_first              1045
_journal_paper_doi               10.1039/b002298p
_journal_year                    2000
_chemical_formula_sum            'C36 H67 Cl P2 Ru'
_chemical_formula_weight         698.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.290(9)
_cell_angle_beta                 108.475(9)
_cell_angle_gamma                90.824(10)
_cell_formula_units_Z            1
_cell_length_a                   9.8438(8)
_cell_length_b                   10.2011(8)
_cell_length_c                   10.8356(9)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      2.21
_cell_volume                     927.37(17)
_computing_cell_refinement       'CELL (Stoe & Cie GmbH, Darmstadt, 1997)'
_computing_data_collection       'EXPOSE (Stoe & Cie GmbH, Darmstadt, 1997)'
_computing_data_reduction
'INTEGRATE (Stoe & Cie GmbH, Darmstadt, 1997)'
_computing_molecular_graphics    'PLATON/PLUTON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.886
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'STOE Image Plate Diffraction System'
_diffrn_measurement_method       'phi oscillation'
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6747
_diffrn_reflns_theta_full        25.85
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   empirical_DIFABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             374
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.634
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0412
_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)+(0.0813P)²+1.3096P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1277
_reflns_number_gt                2953
_reflns_number_total             3181
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002298psup1.cif
_cod_data_source_block           cpd1Cy
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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        927.37(13)
_cod_database_code               7110941
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Ru1 Ru 0.0000 0.0000 0.0000 0.02174(16) Uani 1 2 d S
H1RU H 0.1179 0.0473 -0.0654 0.033 Uiso 0.50 1 d P
Cl1 Cl 0.1512(2) 0.0825(2) -0.09629(19) 0.0389(5) Uani 0.50 1 d P
P1 P 0.20266(9) 0.02805(9) 0.20439(9) 0.0219(2) Uani 1 1 d .
C1 C 0.2581(4) -0.1475(4) 0.1979(4) 0.0259(7) Uani 1 1 d .
H1 H 0.3492 -0.1244 0.2812 0.031 Uiso 1 1 calc R
C2 C 0.1458(5) -0.2433(5) 0.2091(5) 0.0367(9) Uani 1 1 d .
H2A H 0.1289 -0.1899 0.3001 0.044 Uiso 1 1 calc R
H2B H 0.0536 -0.2657 0.1291 0.044 Uiso 1 1 calc R
C3 C 0.1974(5) -0.3853(5) 0.2040(5) 0.0417(10) Uani 1 1 d .
H3A H 0.1228 -0.4455 0.2092 0.050 Uiso 1 1 calc R
H3B H 0.2861 -0.3634 0.2877 0.050 Uiso 1 1 calc R
C4 C 0.2278(5) -0.4699(5) 0.0644(5) 0.0413(10) Uani 1 1 d .
H4A H 0.2641 -0.5588 0.0644 0.050 Uiso 1 1 calc R
H4B H 0.1375 -0.4984 -0.0193 0.050 Uiso 1 1 calc R
C5 C 0.3398(5) -0.3755(5) 0.0526(5) 0.0414(10) Uani 1 1 d .
H5A H 0.4323 -0.3539 0.1322 0.050 Uiso 1 1 calc R
H5B H 0.3560 -0.4293 -0.0387 0.050 Uiso 1 1 calc R
C6 C 0.2906(5) -0.2342(4) 0.0582(4) 0.0356(9) Uani 1 1 d .
H6A H 0.2029 -0.2555 -0.0262 0.043 Uiso 1 1 calc R
H6B H 0.3664 -0.1746 0.0540 0.043 Uiso 1 1 calc R
C7 C 0.1665(4) 0.1103(4) 0.3768(4) 0.0268(7) Uani 1 1 d .
H7 H 0.0900 0.0378 0.3655 0.032 Uiso 1 1 calc R
C8 C 0.2916(4) 0.1310(5) 0.5142(4) 0.0363(9) Uani 1 1 d .
H8A H 0.3316 0.0403 0.4975 0.044 Uiso 1 1 calc R
H8B H 0.3692 0.2078 0.5373 0.044 Uiso 1 1 calc R
C9 C 0.2389(5) 0.1722(5) 0.6403(4) 0.0426(10) Uani 1 1 d .
H9A H 0.1673 0.0916 0.6203 0.051 Uiso 1 1 calc R
H9B H 0.3210 0.1883 0.7278 0.051 Uiso 1 1 calc R
C10 C 0.1714(5) 0.3077(5) 0.6663(4) 0.0437(10) Uani 1 1 d .
H10A H 0.2461 0.3909 0.6979 0.052 Uiso 1 1 calc R
H10B H 0.1326 0.3274 0.7439 0.052 Uiso 1 1 calc R
C11 C 0.0499(5) 0.2920(5) 0.5304(5) 0.0441(10) Uani 1 1 d .
H11A H 0.0137 0.3848 0.5490 0.053 Uiso 1 1 calc R
H11B H -0.0306 0.2178 0.5067 0.053 Uiso 1 1 calc R
C12 C 0.0998(4) 0.2491(5) 0.4019(4) 0.0365(9) Uani 1 1 d .
H12A H 0.1718 0.3285 0.4201 0.044 Uiso 1 1 calc R
H12B H 0.0168 0.2328 0.3150 0.044 Uiso 1 1 calc R
C13 C 0.3743(4) 0.1305(4) 0.2258(4) 0.0278(7) Uani 1 1 d .
H13 H 0.3765 0.0928 0.1265 0.033 Uiso 1 1 calc R
C14 C 0.5188(4) 0.1077(5) 0.3150(5) 0.0393(9) Uani 1 1 d .
H14A H 0.5287 0.1499 0.4172 0.047 Uiso 1 1 calc R
H14B H 0.5214 0.0030 0.2820 0.047 Uiso 1 1 calc R
C15 C 0.6440(4) 0.1803(6) 0.2980(6) 0.0519(12) Uani 1 1 d .
H15A H 0.7362 0.1676 0.3578 0.062 Uiso 1 1 calc R
H15B H 0.6377 0.1318 0.1968 0.062 Uiso 1 1 calc R
C16 C 0.6427(5) 0.3395(6) 0.3410(7) 0.0584(14) Uani 1 1 d .
H16A H 0.7208 0.3797 0.3222 0.070 Uiso 1 1 calc R
H16B H 0.6606 0.3903 0.4450 0.070 Uiso 1 1 calc R
C17 C 0.4986(5) 0.3652(6) 0.2578(6) 0.0517(12) Uani 1 1 d .
H17A H 0.4871 0.3263 0.1553 0.062 Uiso 1 1 calc R
H17B H 0.4977 0.4704 0.2943 0.062 Uiso 1 1 calc R
C18 C 0.3717(4) 0.2927(5) 0.2723(5) 0.0366(9) Uani 1 1 d .
H18A H 0.3768 0.3395 0.3732 0.044 Uiso 1 1 calc R
H18B H 0.2801 0.3061 0.2123 0.044 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'
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 180.00(4) 2 .
P1 Ru1 Cl1 91.62(4) 2 2
P1 Ru1 Cl1 88.38(4) . 2
P1 Ru1 Cl1 88.38(4) 2 .
P1 Ru1 Cl1 91.62(4) . .
Cl1 Ru1 Cl1 180.00(11) 2 .
C7 P1 C1 102.95(16) . .
C7 P1 C13 109.51(17) . .
C1 P1 C13 102.12(16) . .
C7 P1 Ru1 113.08(11) . .
C1 P1 Ru1 113.66(11) . .
C13 P1 Ru1 114.41(11) . .
C2 C1 C6 109.5(3) . .
C2 C1 P1 113.4(3) . .
C6 C1 P1 110.5(2) . .
C3 C2 C1 111.1(3) . .
C2 C3 C4 110.7(3) . .
C5 C4 C3 110.0(4) . .
C6 C5 C4 111.4(3) . .
C5 C6 C1 111.4(3) . .
C12 C7 C8 110.4(3) . .
C12 C7 P1 114.6(2) . .
C8 C7 P1 116.4(3) . .
C9 C8 C7 110.5(3) . .
C10 C9 C8 111.5(4) . .
C9 C10 C11 111.4(3) . .
C10 C11 C12 112.2(3) . .
C11 C12 C7 110.4(3) . .
C18 C13 C14 110.0(3) . .
C18 C13 P1 113.2(2) . .
C14 C13 P1 118.3(3) . .
C15 C14 C13 109.7(3) . .
C16 C15 C14 112.4(4) . .
C15 C16 C17 111.1(4) . .
C16 C17 C18 111.6(4) . .
C13 C18 C17 111.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 P1 2.3724(8) 2
Ru1 P1 2.3724(8) .
Ru1 Cl1 2.384(2) 2
Ru1 Cl1 2.384(2) .
P1 C7 1.860(3) .
P1 C1 1.860(4) .
P1 C13 1.871(3) .
C1 C2 1.531(5) .
C1 C6 1.545(5) .
C2 C3 1.528(6) .
C3 C4 1.531(6) .
C4 C5 1.524(6) .
C5 C6 1.511(6) .
C7 C12 1.528(5) .
C7 C8 1.533(5) .
C8 C9 1.516(5) .
C9 C10 1.503(7) .
C10 C11 1.520(7) .
C11 C12 1.520(5) .
C13 C18 1.522(6) .
C13 C14 1.528(5) .
C14 C15 1.527(6) .
C15 C16 1.496(7) .
C16 C17 1.513(7) .
C17 C18 1.525(5) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
P1 Ru1 P1 C7 -151(35) 2
Cl1 Ru1 P1 C7 -42.18(14) 2
Cl1 Ru1 P1 C7 137.82(14) .
P1 Ru1 P1 C1 -34(35) 2
Cl1 Ru1 P1 C1 74.73(13) 2
Cl1 Ru1 P1 C1 -105.27(13) .
P1 Ru1 P1 C13 83(37) 2
Cl1 Ru1 P1 C13 -168.48(14) 2
Cl1 Ru1 P1 C13 11.52(14) .
C7 P1 C1 C2 55.6(3) .
C13 P1 C1 C2 169.1(3) .
Ru1 P1 C1 C2 -67.1(3) .
C7 P1 C1 C6 179.0(3) .
C13 P1 C1 C6 -67.4(3) .
Ru1 P1 C1 C6 56.3(3) .
C6 C1 C2 C3 56.3(4) .
P1 C1 C2 C3 -179.7(3) .
C1 C2 C3 C4 -57.9(5) .
C2 C3 C4 C5 57.2(5) .
C3 C4 C5 C6 -57.1(5) .
C4 C5 C6 C1 56.9(5) .
C2 C1 C6 C5 -55.9(4) .
P1 C1 C6 C5 178.5(3) .
C1 P1 C7 C12 -172.7(3) .
C13 P1 C7 C12 79.3(3) .
Ru1 P1 C7 C12 -49.6(3) .
C1 P1 C7 C8 56.4(3) .
C13 P1 C7 C8 -51.7(3) .
Ru1 P1 C7 C8 179.5(2) .
C12 C7 C8 C9 57.6(4) .
P1 C7 C8 C9 -169.6(3) .
C7 C8 C9 C10 -57.0(5) .
C8 C9 C10 C11 55.1(5) .
C9 C10 C11 C12 -54.4(5) .
C10 C11 C12 C7 54.9(5) .
C8 C7 C12 C11 -56.3(4) .
P1 C7 C12 C11 169.9(3) .
C7 P1 C13 C18 -56.7(3) .
C1 P1 C13 C18 -165.3(3) .
Ru1 P1 C13 C18 71.4(3) .
C7 P1 C13 C14 74.1(3) .
C1 P1 C13 C14 -34.5(3) .
Ru1 P1 C13 C14 -157.8(3) .
C18 C13 C14 C15 -57.2(5) .
P1 C13 C14 C15 170.6(3) .
C13 C14 C15 C16 57.1(6) .
C14 C15 C16 C17 -55.4(6) .
C15 C16 C17 C18 54.0(6) .
C14 C13 C18 C17 57.1(5) .
P1 C13 C18 C17 -168.1(3) .
C16 C17 C18 C13 -55.4(6) .
