#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:06:34 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178549 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/56/4065661.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_4065661
loop_
_publ_author_name
'Cheung, Wai-Man'
'Chiu, Wai-Hang'
'Yi, Xiao-Yi'
'Zhang, Qian-Feng'
'Williams, Ian D.'
'Leung, Wa-Hung'
_publ_section_title
;
 Formation of a Ruthenium(II) Dicyclohexyl(η2-cyclohex-3-enyl)phosphine
 Hydride Complex from an Alkylidene Precursor
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1981
_journal_paper_doi               10.1021/om100054n
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C30 H60 N P3 Ru S2'
_chemical_formula_weight         692.89
_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                95.7840(10)
_cell_angle_beta                 102.7490(10)
_cell_angle_gamma                108.0770(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6266(10)
_cell_length_b                   11.5208(12)
_cell_length_c                   16.9307(18)
_cell_measurement_reflns_used    8627
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.30
_cell_volume                     1711.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17612
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0239
_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/[σ²(Fo²)+(0.0348P)²+0.0380P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                5950
_reflns_number_total             6629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100054n_si_001.cif
_cod_data_source_block           cpd4_wai101
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065661
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 0.176342(15) 0.272032(12) 0.225954(8) 0.01366(5) Uani 1 1 d .
H1 H 0.1559 0.2537 0.1367 0.046(7) Uiso 1 1 d R
S1 S 0.23165(5) 0.08296(4) 0.22260(3) 0.01749(10) Uani 1 1 d .
S2 S -0.08246(5) 0.19820(4) 0.24522(3) 0.02166(11) Uani 1 1 d .
P1 P 0.05631(5) -0.07131(4) 0.22123(3) 0.01661(10) Uani 1 1 d .
P2 P -0.11446(5) 0.05067(4) 0.30177(3) 0.01747(10) Uani 1 1 d .
P3 P 0.41627(5) 0.38099(4) 0.22917(3) 0.01389(10) Uani 1 1 d .
N1 N -0.06573(17) -0.06108(13) 0.26852(10) 0.0199(3) Uani 1 1 d .
C1 C 0.1414(2) -0.17865(17) 0.26778(12) 0.0217(4) Uani 1 1 d .
H1A H 0.2085 -0.1969 0.2345 0.026 Uiso 1 1 calc R
C2 C 0.2376(2) -0.11946(19) 0.35529(12) 0.0287(5) Uani 1 1 d .
H2A H 0.1751 -0.0950 0.3876 0.043 Uiso 1 1 calc R
H2B H 0.3218 -0.0459 0.3541 0.043 Uiso 1 1 calc R
H2C H 0.2778 -0.1793 0.3805 0.043 Uiso 1 1 calc R
C3 C 0.0168(2) -0.30069(18) 0.26624(15) 0.0336(5) Uani 1 1 d .
H3A H 0.0616 -0.3535 0.2973 0.050 Uiso 1 1 calc R
H3B H -0.0322 -0.3437 0.2091 0.050 Uiso 1 1 calc R
H3C H -0.0587 -0.2829 0.2913 0.050 Uiso 1 1 calc R
C4 C -0.0413(2) -0.14620(18) 0.11422(12) 0.0260(4) Uani 1 1 d .
H4 H -0.1250 -0.2234 0.1148 0.031 Uiso 1 1 calc R
C5 C -0.1138(2) -0.0613(2) 0.07022(12) 0.0305(5) Uani 1 1 d .
H5A H -0.0345 0.0163 0.0700 0.046 Uiso 1 1 calc R
H5B H -0.1844 -0.0430 0.0991 0.046 Uiso 1 1 calc R
H5C H -0.1689 -0.1029 0.0134 0.046 Uiso 1 1 calc R
C6 C 0.0622(2) -0.1846(2) 0.06821(13) 0.0321(5) Uani 1 1 d .
H6A H 0.0061 -0.2200 0.0106 0.048 Uiso 1 1 calc R
H6B H 0.0968 -0.2467 0.0940 0.048 Uiso 1 1 calc R
H6C H 0.1500 -0.1116 0.0706 0.048 Uiso 1 1 calc R
C7 C -0.3177(2) -0.01415(17) 0.29323(13) 0.0240(4) Uani 1 1 d .
H7 H -0.3501 0.0541 0.3153 0.029 Uiso 1 1 calc R
C8 C -0.3518(2) -0.11649(19) 0.34456(14) 0.0330(5) Uani 1 1 d .
H8A H -0.4617 -0.1557 0.3340 0.049 Uiso 1 1 calc R
H8B H -0.3073 -0.0803 0.4032 0.049 Uiso 1 1 calc R
H8C H -0.3080 -0.1790 0.3293 0.049 Uiso 1 1 calc R
C9 C -0.4076(2) -0.0623(2) 0.20320(14) 0.0325(5) Uani 1 1 d .
H9A H -0.3862 -0.1354 0.1819 0.049 Uiso 1 1 calc R
H9B H -0.3781 0.0027 0.1709 0.049 Uiso 1 1 calc R
H9C H -0.5162 -0.0852 0.1990 0.049 Uiso 1 1 calc R
C10 C -0.0205(2) 0.10008(18) 0.41229(12) 0.0235(4) Uani 1 1 d .
H10 H -0.0292 0.0232 0.4365 0.028 Uiso 1 1 calc R
C11 C 0.1477(2) 0.17192(19) 0.42723(12) 0.0276(4) Uani 1 1 d .
H11A H 0.1606 0.2516 0.4088 0.041 Uiso 1 1 calc R
H11B H 0.1927 0.1237 0.3964 0.041 Uiso 1 1 calc R
H11C H 0.1980 0.1867 0.4862 0.041 Uiso 1 1 calc R
C12 C -0.0925(2) 0.1760(2) 0.45831(13) 0.0324(5) Uani 1 1 d .
H12A H -0.0337 0.2031 0.5161 0.049 Uiso 1 1 calc R
H12B H -0.1967 0.1248 0.4551 0.049 Uiso 1 1 calc R
H12C H -0.0932 0.2489 0.4332 0.049 Uiso 1 1 calc R
C21 C 0.56469(18) 0.37869(16) 0.32072(10) 0.0159(4) Uani 1 1 d .
H21 H 0.6104 0.3174 0.3020 0.019 Uiso 1 1 calc R
C22 C 0.6965(2) 0.50200(17) 0.35707(11) 0.0204(4) Uani 1 1 d .
H22A H 0.7429 0.5328 0.3132 0.024 Uiso 1 1 calc R
H22B H 0.6574 0.5648 0.3790 0.024 Uiso 1 1 calc R
C23 C 0.8162(2) 0.48440(19) 0.42591(12) 0.0249(4) Uani 1 1 d .
H23A H 0.8994 0.5648 0.4489 0.030 Uiso 1 1 calc R
H23B H 0.8594 0.4252 0.4032 0.030 Uiso 1 1 calc R
C24 C 0.7484(2) 0.4353(2) 0.49456(12) 0.0280(5) Uani 1 1 d .
H24A H 0.8266 0.4194 0.5365 0.034 Uiso 1 1 calc R
H24B H 0.7160 0.4988 0.5216 0.034 Uiso 1 1 calc R
C25 C 0.6127(2) 0.31568(19) 0.46078(11) 0.0244(4) Uani 1 1 d .
H25A H 0.6482 0.2487 0.4416 0.029 Uiso 1 1 calc R
H25B H 0.5651 0.2909 0.5055 0.029 Uiso 1 1 calc R
C26 C 0.4951(2) 0.33041(18) 0.38973(11) 0.0198(4) Uani 1 1 d .
H26A H 0.4494 0.3891 0.4106 0.024 Uiso 1 1 calc R
H26B H 0.4133 0.2492 0.3670 0.024 Uiso 1 1 calc R
C31 C 0.49363(19) 0.36061(16) 0.13999(11) 0.0162(4) Uani 1 1 d .
H31 H 0.4248 0.3775 0.0925 0.019 Uiso 1 1 calc R
C32 C 0.4873(2) 0.22709(17) 0.11462(11) 0.0211(4) Uani 1 1 d .
H32A H 0.5582 0.2065 0.1582 0.025 Uiso 1 1 calc R
H32B H 0.3837 0.1689 0.1085 0.025 Uiso 1 1 calc R
C33 C 0.5297(2) 0.21161(18) 0.03336(11) 0.0238(4) Uani 1 1 d .
H33A H 0.5293 0.1259 0.0195 0.029 Uiso 1 1 calc R
H33B H 0.4531 0.2245 -0.0112 0.029 Uiso 1 1 calc R
C34 C 0.6858(2) 0.30351(18) 0.03835(12) 0.0238(4) Uani 1 1 d .
H34A H 0.7640 0.2837 0.0778 0.029 Uiso 1 1 calc R
H34B H 0.7062 0.2955 -0.0164 0.029 Uiso 1 1 calc R
C35 C 0.6957(2) 0.43620(18) 0.06591(12) 0.0247(4) Uani 1 1 d .
H35A H 0.6268 0.4596 0.0229 0.030 Uiso 1 1 calc R
H35B H 0.8003 0.4930 0.0728 0.030 Uiso 1 1 calc R
C36 C 0.6527(2) 0.45127(17) 0.14728(11) 0.0214(4) Uani 1 1 d .
H36A H 0.6557 0.5375 0.1622 0.026 Uiso 1 1 calc R
H36B H 0.7272 0.4356 0.1916 0.026 Uiso 1 1 calc R
C41 C 0.4225(2) 0.54420(16) 0.24042(11) 0.0174(4) Uani 1 1 d .
H41 H 0.5295 0.6026 0.2614 0.021 Uiso 1 1 calc R
C42 C 0.3335(2) 0.55336(16) 0.30365(11) 0.0184(4) Uani 1 1 d .
H42A H 0.3867 0.5403 0.3573 0.022 Uiso 1 1 calc R
H42B H 0.3243 0.6367 0.3114 0.022 Uiso 1 1 calc R
C43 C 0.1772(2) 0.45418(16) 0.27196(11) 0.0192(4) Uani 1 1 d .
H43 H 0.1074 0.4548 0.3077 0.023 Uiso 1 1 calc R
C44 C 0.1066(2) 0.42357(16) 0.18708(12) 0.0200(4) Uani 1 1 d .
H44 H -0.0057 0.4038 0.1741 0.024 Uiso 1 1 calc R
C45 C 0.1766(2) 0.49111(18) 0.12528(12) 0.0249(4) Uani 1 1 d .
H45A H 0.1165 0.5423 0.1035 0.030 Uiso 1 1 calc R
H45B H 0.1699 0.4288 0.0785 0.030 Uiso 1 1 calc R
C46 C 0.3426(2) 0.57499(17) 0.16045(11) 0.0213(4) Uani 1 1 d .
H46A H 0.3469 0.6623 0.1711 0.026 Uiso 1 1 calc R
H46B H 0.3983 0.5677 0.1187 0.026 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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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
C43 Ru1 C44 37.85(7)
C43 Ru1 P3 81.93(5)
C44 Ru1 P3 89.62(5)
C43 Ru1 S1 159.89(5)
C44 Ru1 S1 161.76(5)
P3 Ru1 S1 91.197(17)
C43 Ru1 S2 84.66(5)
C44 Ru1 S2 82.31(5)
P3 Ru1 S2 165.940(17)
S1 Ru1 S2 100.076(16)
P1 S1 Ru1 115.49(2)
P2 S2 Ru1 111.42(2)
N1 P1 C4 108.92(9)
N1 P1 C1 106.12(8)
C4 P1 C1 106.27(9)
N1 P1 S1 119.88(6)
C4 P1 S1 108.64(7)
C1 P1 S1 106.17(6)
N1 P2 C7 106.67(8)
N1 P2 C10 107.72(9)
C7 P2 C10 105.98(9)
N1 P2 S2 118.34(6)
C7 P2 S2 107.09(6)
C10 P2 S2 110.31(7)
C31 P3 C41 104.11(8)
C31 P3 C21 105.17(8)
C41 P3 C21 104.64(8)
C31 P3 Ru1 121.55(6)
C41 P3 Ru1 104.01(6)
C21 P3 Ru1 115.53(6)
P1 N1 P2 134.06(10)
C2 C1 C3 111.14(17)
C2 C1 P1 110.26(13)
C3 C1 P1 109.85(13)
C5 C4 C6 111.50(17)
C5 C4 P1 109.66(13)
C6 C4 P1 112.76(14)
C9 C7 C8 110.98(17)
C9 C7 P2 110.57(14)
C8 C7 P2 111.27(13)
C11 C10 C12 109.87(16)
C11 C10 P2 111.03(13)
C12 C10 P2 113.73(14)
C22 C21 C26 109.13(14)
C22 C21 P3 116.00(12)
C26 C21 P3 111.61(12)
C23 C22 C21 110.61(15)
C22 C23 C24 111.12(15)
C25 C24 C23 111.13(16)
C26 C25 C24 112.02(16)
C25 C26 C21 111.91(15)
C36 C31 C32 109.68(14)
C36 C31 P3 115.73(12)
C32 C31 P3 113.28(12)
C33 C32 C31 110.77(15)
C34 C33 C32 111.52(15)
C35 C34 C33 111.22(15)
C34 C35 C36 111.48(16)
C35 C36 C31 110.75(15)
C42 C41 C46 108.17(15)
C42 C41 P3 103.62(11)
C46 C41 P3 112.88(12)
C43 C42 C41 108.16(14)
C44 C43 C42 119.45(16)
C44 C43 Ru1 71.34(10)
C42 C43 Ru1 114.90(11)
C43 C44 C45 122.37(16)
C43 C44 Ru1 70.81(10)
C45 C44 Ru1 118.49(13)
C44 C45 C46 114.21(15)
C45 C46 C41 113.80(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ru1 C43 2.1604(17)
Ru1 C44 2.1671(17)
Ru1 P3 2.2460(5)
Ru1 S1 2.3957(5)
Ru1 S2 2.4771(5)
S1 P1 2.0301(6)
S2 P2 2.0084(7)
P1 N1 1.5866(15)
P1 C4 1.828(2)
P1 C1 1.8337(19)
P2 N1 1.5936(15)
P2 C7 1.8313(19)
P2 C10 1.834(2)
P3 C31 1.8501(18)
P3 C41 1.8514(18)
P3 C21 1.8707(17)
C1 C2 1.522(3)
C1 C3 1.532(3)
C4 C5 1.529(3)
C4 C6 1.531(3)
C7 C9 1.526(3)
C7 C8 1.531(3)
C10 C11 1.521(3)
C10 C12 1.527(3)
C21 C22 1.539(2)
C21 C26 1.539(2)
C22 C23 1.526(3)
C23 C24 1.528(3)
C24 C25 1.525(3)
C25 C26 1.522(2)
C31 C36 1.533(2)
C31 C32 1.533(2)
C32 C33 1.528(2)
C33 C34 1.524(3)
C34 C35 1.520(3)
C35 C36 1.532(2)
C41 C42 1.526(2)
C41 C46 1.536(2)
C42 C43 1.520(2)
C43 C44 1.404(3)
C44 C45 1.518(3)
C45 C46 1.532(3)
