#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:29:14 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178567 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/76/4067672.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_4067672
loop_
_publ_author_name
'Hill, Anthony F.'
'Neumann, Horst'
'Wagler, Jörg'
_publ_section_title
;
 Bis(methimazolyl)silyl Complexes of Ruthenium
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1026
_journal_paper_doi               10.1021/om901067t
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C39 H30 O3 P2 Ru'
_chemical_formula_sum            'C39 H30 O3 P2 Ru'
_chemical_formula_weight         709.64
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.67490(10)
_cell_length_b                   15.67490(10)
_cell_length_c                   23.0971(3)
_cell_measurement_reflns_used    130393
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      42.106
_cell_measurement_theta_min      2.546
_cell_volume                     4914.71(8)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Scalepack
_computing_molecular_graphics    'ORTEP32 for windows (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            107567
_diffrn_reflns_theta_full        38.00
_diffrn_reflns_theta_max         38.00
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         8918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0387P)²+1.8179P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                6235
_reflns_number_total             8918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om901067t_si_001.cif
_cod_data_source_block           ks00201
_cod_original_sg_symbol_H-M      P-3c1
_cod_database_code               4067672
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-y, -x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x-y, -y, -z-1/2'
'-x, -x+y, -z-1/2'
'y, x, -z-1/2'
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 0.2500 0.01256(4) Uani 1 6 d S
Ru2 Ru 0.3333 0.6667 0.521792(6) 0.01298(4) Uani 1 3 d S
P1 P 0.0000 0.0000 0.14793(2) 0.01361(7) Uani 1 3 d S
P2 P 0.3333 0.6667 0.623177(19) 0.01278(7) Uani 1 3 d S
P3 P 0.3333 0.6667 0.419797(19) 0.01242(7) Uani 1 3 d S
O1 O 0.19622(8) 0.0000 0.2500 0.0269(3) Uani 1 2 d S
O2 O 0.52221(8) 0.65289(8) 0.52403(4) 0.0318(2) Uani 1 1 d .
C1 C 0.12294(10) 0.0000 0.2500 0.0183(3) Uani 1 2 d S
C2 C -0.06852(8) -0.12155(8) 0.11450(4) 0.01619(17) Uani 1 1 d .
C3 C -0.13600(9) -0.14345(9) 0.06964(5) 0.0214(2) Uani 1 1 d .
H3 H -0.1481 -0.0938 0.0550 0.026 Uiso 1 1 calc R
C4 C -0.18579(10) -0.23833(10) 0.04619(5) 0.0278(3) Uani 1 1 d .
H4 H -0.2323 -0.2532 0.0160 0.033 Uiso 1 1 calc R
C5 C -0.16760(11) -0.31071(10) 0.06678(6) 0.0309(3) Uani 1 1 d .
H5 H -0.2014 -0.3750 0.0506 0.037 Uiso 1 1 calc R
C6 C -0.09970(11) -0.28919(9) 0.11121(6) 0.0302(3) Uani 1 1 d .
H6 H -0.0865 -0.3385 0.1251 0.036 Uiso 1 1 calc R
C7 C -0.05153(9) -0.19559(9) 0.13511(5) 0.0233(2) Uani 1 1 d .
H7 H -0.0063 -0.1815 0.1659 0.028 Uiso 1 1 calc R
C8 C 0.45177(9) 0.65804(9) 0.52264(5) 0.0217(2) Uani 1 1 d .
C9 C 0.45175(7) 0.70337(8) 0.65786(4) 0.01473(16) Uani 1 1 d .
C10 C 0.53674(8) 0.78713(8) 0.63729(5) 0.01949(19) Uani 1 1 d .
H10 H 0.5325 0.8215 0.6045 0.023 Uiso 1 1 calc R
C11 C 0.62694(8) 0.82001(9) 0.66456(5) 0.0228(2) Uani 1 1 d .
H11 H 0.6839 0.8773 0.6508 0.027 Uiso 1 1 calc R
C12 C 0.63376(8) 0.76901(9) 0.71202(5) 0.0217(2) Uani 1 1 d .
H12 H 0.6954 0.7915 0.7307 0.026 Uiso 1 1 calc R
C13 C 0.55054(8) 0.68536(9) 0.73205(5) 0.01915(19) Uani 1 1 d .
H13 H 0.5555 0.6498 0.7640 0.023 Uiso 1 1 calc R
C14 C 0.45976(8) 0.65336(8) 0.70548(4) 0.01597(17) Uani 1 1 d .
H14 H 0.4028 0.5969 0.7200 0.019 Uiso 1 1 calc R
C15 C 0.41527(7) 0.62974(8) 0.38578(4) 0.01418(16) Uani 1 1 d .
C16 C 0.41289(9) 0.54348(8) 0.40450(5) 0.01979(19) Uani 1 1 d .
H16 H 0.3700 0.5059 0.4351 0.024 Uiso 1 1 calc R
C17 C 0.47287(9) 0.51244(9) 0.37864(5) 0.0238(2) Uani 1 1 d .
H17 H 0.4696 0.4530 0.3909 0.029 Uiso 1 1 calc R
C18 C 0.53764(9) 0.56843(9) 0.33476(5) 0.0230(2) Uani 1 1 d .
H18 H 0.5792 0.5477 0.3174 0.028 Uiso 1 1 calc R
C19 C 0.54142(9) 0.65430(9) 0.31645(5) 0.0218(2) Uani 1 1 d .
H19 H 0.5861 0.6928 0.2868 0.026 Uiso 1 1 calc R
C20 C 0.47987(8) 0.68447(8) 0.34140(5) 0.01747(18) Uani 1 1 d .
H20 H 0.4820 0.7428 0.3281 0.021 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'
O O 0.0106 0.0060 '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
C1 Ru1 C1 120.0 2 3
C1 Ru1 C1 120.0 2 .
C1 Ru1 C1 120.0 3 .
C1 Ru1 P1 90.0 2 .
C1 Ru1 P1 90.0 3 .
C1 Ru1 P1 90.0 . .
C1 Ru1 P1 90.0 2 10_556
C1 Ru1 P1 90.0 3 10_556
C1 Ru1 P1 90.0 . 10_556
P1 Ru1 P1 180.0 . 10_556
C8 Ru2 C8 119.990(1) 2_665 3_565
C8 Ru2 C8 119.990(2) 2_665 .
C8 Ru2 C8 119.990(1) 3_565 .
C8 Ru2 P2 89.41(3) 2_665 .
C8 Ru2 P2 89.41(3) 3_565 .
C8 Ru2 P2 89.42(3) . .
C8 Ru2 P3 90.59(3) 2_665 .
C8 Ru2 P3 90.59(3) 3_565 .
C8 Ru2 P3 90.58(3) . .
P2 Ru2 P3 180.0 . .
C2 P1 C2 103.40(4) . 2
C2 P1 C2 103.40(4) . 3
C2 P1 C2 103.40(4) 2 3
C2 P1 Ru1 115.02(3) . .
C2 P1 Ru1 115.02(3) 2 .
C2 P1 Ru1 115.02(3) 3 .
C9 P2 C9 102.28(4) 2_665 3_565
C9 P2 C9 102.28(4) 2_665 .
C9 P2 C9 102.28(4) 3_565 .
C9 P2 Ru2 115.96(3) 2_665 .
C9 P2 Ru2 115.96(3) 3_565 .
C9 P2 Ru2 115.95(3) . .
C15 P3 C15 102.90(4) 2_665 3_565
C15 P3 C15 102.90(4) 2_665 .
C15 P3 C15 102.90(4) 3_565 .
C15 P3 Ru2 115.44(3) 2_665 .
C15 P3 Ru2 115.44(3) 3_565 .
C15 P3 Ru2 115.44(3) . .
O1 C1 Ru1 180.0 . .
C3 C2 C7 118.96(10) . .
C3 C2 P1 123.29(8) . .
C7 C2 P1 117.74(8) . .
C2 C3 C4 120.06(11) . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C5 C4 C3 120.29(12) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C4 C5 C6 120.00(12) . .
C4 C5 H5 120.0 . .
C6 C5 H5 120.0 . .
C7 C6 C5 119.72(12) . .
C7 C6 H6 120.1 . .
C5 C6 H6 120.1 . .
C6 C7 C2 120.96(11) . .
C6 C7 H7 119.5 . .
C2 C7 H7 119.5 . .
O2 C8 Ru2 178.99(10) . .
C14 C9 C10 118.87(10) . .
C14 C9 P2 122.11(8) . .
C10 C9 P2 118.97(8) . .
C11 C10 C9 120.43(10) . .
C11 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
C10 C11 C12 119.99(11) . .
C10 C11 H11 120.0 . .
C12 C11 H11 120.0 . .
C13 C12 C11 119.96(10) . .
C13 C12 H12 120.0 . .
C11 C12 H12 120.0 . .
C12 C13 C14 120.14(10) . .
C12 C13 H13 119.9 . .
C14 C13 H13 119.9 . .
C9 C14 C13 120.59(10) . .
C9 C14 H14 119.7 . .
C13 C14 H14 119.7 . .
C20 C15 C16 118.75(10) . .
C20 C15 P3 122.01(8) . .
C16 C15 P3 119.23(8) . .
C17 C16 C15 120.54(10) . .
C17 C16 H16 119.7 . .
C15 C16 H16 119.7 . .
C16 C17 C18 119.98(11) . .
C16 C17 H17 120.0 . .
C18 C17 H17 120.0 . .
C19 C18 C17 119.93(10) . .
C19 C18 H18 120.0 . .
C17 C18 H18 120.0 . .
C18 C19 C20 120.22(11) . .
C18 C19 H19 119.9 . .
C20 C19 H19 119.9 . .
C15 C20 C19 120.55(10) . .
C15 C20 H20 119.7 . .
C19 C20 H20 119.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 C1 1.9270(16) 2
Ru1 C1 1.9270(16) 3
Ru1 C1 1.9270(16) .
Ru1 P1 2.3575(5) .
Ru1 P1 2.3575(5) 10_556
Ru2 C8 1.9277(12) 2_665
Ru2 C8 1.9277(12) 3_565
Ru2 C8 1.9277(12) .
Ru2 P2 2.3417(5) .
Ru2 P3 2.3558(4) .
P1 C2 1.8258(10) .
P1 C2 1.8258(10) 2
P1 C2 1.8258(10) 3
P2 C9 1.8303(10) 2_665
P2 C9 1.8303(10) 3_565
P2 C9 1.8303(10) .
P3 C15 1.8290(10) 2_665
P3 C15 1.8290(10) 3_565
P3 C15 1.8290(10) .
O1 C1 1.149(2) .
O2 C8 1.1471(15) .
C2 C3 1.3953(15) .
C2 C7 1.3977(16) .
C3 C4 1.3977(17) .
C3 H3 0.9500 .
C4 C5 1.385(2) .
C4 H4 0.9500 .
C5 C6 1.3930(19) .
C5 H5 0.9500 .
C6 C7 1.3855(17) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C9 C14 1.3922(14) .
C9 C10 1.4054(15) .
C10 C11 1.3902(16) .
C10 H10 0.9500 .
C11 C12 1.3918(17) .
C11 H11 0.9500 .
C12 C13 1.3872(17) .
C12 H12 0.9500 .
C13 C14 1.3926(15) .
C13 H13 0.9500 .
C14 H14 0.9500 .
C15 C20 1.3939(15) .
C15 C16 1.4022(15) .
C16 C17 1.3910(16) .
C16 H16 0.9500 .
C17 C18 1.3917(18) .
C17 H17 0.9500 .
C18 C19 1.3836(17) .
C18 H18 0.9500 .
C19 C20 1.3940(15) .
C19 H19 0.9500 .
C20 H20 0.9500 .
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
_geom_torsion_site_symmetry_4
C1 Ru1 P1 C2 -145.79(4) 2 .
C1 Ru1 P1 C2 -25.79(4) 3 .
C1 Ru1 P1 C2 94.21(4) . .
C1 Ru1 P1 C2 94.21(4) 2 2
C1 Ru1 P1 C2 -145.79(4) 3 2
C1 Ru1 P1 C2 -25.79(4) . 2
C1 Ru1 P1 C2 -25.79(4) 2 3
C1 Ru1 P1 C2 94.21(4) 3 3
C1 Ru1 P1 C2 -145.79(4) . 3
C8 Ru2 P2 C9 21.11(5) 2_665 2_665
C8 Ru2 P2 C9 -98.89(5) 3_565 2_665
C8 Ru2 P2 C9 141.11(5) . 2_665
C8 Ru2 P2 C9 141.11(5) 2_665 3_565
C8 Ru2 P2 C9 21.11(5) 3_565 3_565
C8 Ru2 P2 C9 -98.89(5) . 3_565
C8 Ru2 P2 C9 -98.89(5) 2_665 .
C8 Ru2 P2 C9 141.11(5) 3_565 .
C8 Ru2 P2 C9 21.11(5) . .
C8 Ru2 P3 C15 14.18(5) 2_665 2_665
C8 Ru2 P3 C15 134.18(5) 3_565 2_665
C8 Ru2 P3 C15 -105.82(5) . 2_665
C8 Ru2 P3 C15 -105.82(5) 2_665 3_565
C8 Ru2 P3 C15 14.18(5) 3_565 3_565
C8 Ru2 P3 C15 134.18(5) . 3_565
C8 Ru2 P3 C15 134.18(5) 2_665 .
C8 Ru2 P3 C15 -105.82(5) 3_565 .
C8 Ru2 P3 C15 14.18(5) . .
C2 P1 C2 C3 -101.42(7) 2 .
C2 P1 C2 C3 6.14(11) 3 .
Ru1 P1 C2 C3 132.36(9) . .
C2 P1 C2 C7 78.30(12) 2 .
C2 P1 C2 C7 -174.15(9) 3 .
Ru1 P1 C2 C7 -47.92(10) . .
C7 C2 C3 C4 0.31(17) . .
P1 C2 C3 C4 -179.97(9) . .
C2 C3 C4 C5 -0.8(2) . .
C3 C4 C5 C6 0.2(2) . .
C4 C5 C6 C7 0.8(2) . .
C5 C6 C7 C2 -1.3(2) . .
C3 C2 C7 C6 0.75(18) . .
P1 C2 C7 C6 -178.98(11) . .
C9 P2 C9 C14 95.80(6) 2_665 .
C9 P2 C9 C14 -9.87(10) 3_565 .
Ru2 P2 C9 C14 -137.04(8) . .
C9 P2 C9 C10 -81.52(11) 2_665 .
C9 P2 C9 C10 172.81(9) 3_565 .
Ru2 P2 C9 C10 45.64(10) . .
C14 C9 C10 C11 -0.79(17) . .
P2 C9 C10 C11 176.62(9) . .
C9 C10 C11 C12 0.98(18) . .
C10 C11 C12 C13 0.04(18) . .
C11 C12 C13 C14 -1.26(17) . .
C10 C9 C14 C13 -0.43(15) . .
P2 C9 C14 C13 -177.76(8) . .
C12 C13 C14 C9 1.46(16) . .
C15 P3 C15 C20 -4.87(11) 2_665 .
C15 P3 C15 C20 101.83(7) 3_565 .
Ru2 P3 C15 C20 -131.52(8) . .
C15 P3 C15 C16 175.54(8) 2_665 .
C15 P3 C15 C16 -77.76(11) 3_565 .
Ru2 P3 C15 C16 48.89(9) . .
C20 C15 C16 C17 -0.94(17) . .
P3 C15 C16 C17 178.67(9) . .
C15 C16 C17 C18 1.57(18) . .
C16 C17 C18 C19 -0.78(19) . .
C17 C18 C19 C20 -0.63(18) . .
C16 C15 C20 C19 -0.48(16) . .
P3 C15 C20 C19 179.93(9) . .
C18 C19 C20 C15 1.26(18) . .
