#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:26:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179110 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/72/4307253.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_4307253
loop_
_publ_author_name
'Elaine Phuay Leng Tay'
'Seah Ling Kuan'
'Weng Kee Leong'
'Lai Yoong Goh'
_publ_section_title
;
Synthetic and X-ray Structural and Reactivity Studies of Cp*RuIV Complexes
Containing Bidentate Dithiocarbonate, Xanthate, Carbonate, and Phosphinate
Ligands (Cp* = η5-C5Me5)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1440
_journal_page_last               1450
_journal_paper_doi               10.1021/ic061781t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C32 H37 O P Ru S2'
_chemical_formula_weight         633.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.6760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6555(2)
_cell_length_b                   11.1636(2)
_cell_length_c                   18.7075(3)
_cell_measurement_reflns_used    8883
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.31
_cell_volume                     2997.37(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω 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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24465
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.8426
_exptl_absorpt_correction_T_min  0.7872
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         7316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0459
_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)+(0.0466P)²+2.3876P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1052
_reflns_number_gt                6754
_reflns_number_total             7316
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061781tsi20060920_065925_09.cif
_cod_data_source_block           et14
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4307253
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.931289(14) 0.183289(19) 0.210615(11) 0.02538(8) Uani 1 1 d . . .
P1 P 1.02143(5) 0.23579(6) 0.32167(4) 0.02610(14) Uani 1 1 d . . .
S1 S 1.05059(5) 0.25301(6) 0.14897(4) 0.03031(15) Uani 1 1 d . . .
S2 S 0.89930(5) 0.38847(6) 0.17677(4) 0.03005(15) Uani 1 1 d . . .
O1 O 1.03116(15) 0.47693(18) 0.10835(12) 0.0378(5) Uani 1 1 d . . .
C1 C 0.99557(19) 0.3868(2) 0.13986(14) 0.0289(5) Uani 1 1 d . . .
C2 C 0.9925(2) 0.5983(3) 0.10972(18) 0.0402(7) Uani 1 1 d . . .
H2 H 0.9795 0.6146 0.1587 0.048 Uiso 1 1 calc R . .
C3 C 1.0705(3) 0.6782(3) 0.0969(3) 0.0675(12) Uani 1 1 d . . .
H3A H 1.1248 0.6658 0.1354 0.101 Uiso 1 1 calc R . .
H3B H 1.0510 0.7613 0.0969 0.101 Uiso 1 1 calc R . .
H3C H 1.0857 0.6590 0.0502 0.101 Uiso 1 1 calc R . .
C4 C 0.9045(3) 0.6116(3) 0.0535(2) 0.0537(9) Uani 1 1 d . . .
H4A H 0.9180 0.6013 0.0052 0.081 Uiso 1 1 calc R . .
H4B H 0.8785 0.6907 0.0573 0.081 Uiso 1 1 calc R . .
H4C H 0.8600 0.5514 0.0615 0.081 Uiso 1 1 calc R . .
C11 C 0.9594(2) 0.2868(2) 0.39204(15) 0.0310(6) Uani 1 1 d . . .
C12 C 1.0053(2) 0.3130(3) 0.46301(18) 0.0422(7) Uani 1 1 d . . .
H12 H 1.0700 0.3010 0.4768 0.051 Uiso 1 1 calc R . .
C13 C 0.9560(3) 0.3566(3) 0.51362(19) 0.0506(9) Uani 1 1 d . . .
H13 H 0.9872 0.3731 0.5616 0.061 Uiso 1 1 calc R . .
C14 C 0.8618(3) 0.3755(3) 0.4936(2) 0.0519(9) Uani 1 1 d . . .
H14 H 0.8286 0.4047 0.5280 0.062 Uiso 1 1 calc R . .
C15 C 0.8158(3) 0.3522(3) 0.4236(2) 0.0471(8) Uani 1 1 d . . .
H15 H 0.7513 0.3661 0.4100 0.056 Uiso 1 1 calc R . .
C16 C 0.8645(2) 0.3078(3) 0.37254(17) 0.0365(6) Uani 1 1 d . . .
H16 H 0.8327 0.2921 0.3246 0.044 Uiso 1 1 calc R . .
C21 C 1.09511(19) 0.1111(3) 0.36363(15) 0.0309(6) Uani 1 1 d . . .
C22 C 1.0857(2) 0.0533(3) 0.42776(17) 0.0417(7) Uani 1 1 d . . .
H22 H 1.0435 0.0829 0.4552 0.050 Uiso 1 1 calc R . .
C23 C 1.1386(3) -0.0482(3) 0.4512(2) 0.0536(9) Uani 1 1 d . . .
H23 H 1.1308 -0.0877 0.4940 0.064 Uiso 1 1 calc R . .
C24 C 1.2019(3) -0.0913(3) 0.4126(2) 0.0522(9) Uani 1 1 d . . .
H24 H 1.2377 -0.1594 0.4293 0.063 Uiso 1 1 calc R . .
C25 C 1.2130(2) -0.0348(3) 0.34950(19) 0.0433(7) Uani 1 1 d . . .
H25 H 1.2572 -0.0631 0.3235 0.052 Uiso 1 1 calc R . .
C26 C 1.1585(2) 0.0646(3) 0.32439(16) 0.0366(6) Uani 1 1 d . . .
H26 H 1.1645 0.1009 0.2802 0.044 Uiso 1 1 calc R . .
C31 C 1.10400(19) 0.3626(3) 0.32780(14) 0.0295(5) Uani 1 1 d . . .
C32 C 1.2001(2) 0.3517(3) 0.3439(2) 0.0457(8) Uani 1 1 d . . .
H32 H 1.2275 0.2758 0.3537 0.055 Uiso 1 1 calc R . .
C33 C 1.2564(2) 0.4529(4) 0.3456(2) 0.0570(10) Uani 1 1 d . . .
H33 H 1.3215 0.4440 0.3570 0.068 Uiso 1 1 calc R . .
C34 C 1.2192(3) 0.5646(3) 0.33124(19) 0.0487(9) Uani 1 1 d . . .
H34 H 1.2581 0.6316 0.3316 0.058 Uiso 1 1 calc R . .
C35 C 1.1237(3) 0.5776(3) 0.31609(17) 0.0436(7) Uani 1 1 d . . .
H35 H 1.0970 0.6539 0.3066 0.052 Uiso 1 1 calc R . .
C36 C 1.0672(2) 0.4779(3) 0.31489(16) 0.0369(6) Uani 1 1 d . . .
H36 H 1.0022 0.4881 0.3051 0.044 Uiso 1 1 calc R . .
C41 C 0.8532(2) 0.0356(3) 0.24990(18) 0.0364(6) Uani 1 1 d . . .
C42 C 0.7897(2) 0.1106(3) 0.2021(2) 0.0424(7) Uani 1 1 d . . .
C43 C 0.8145(2) 0.1084(3) 0.13198(19) 0.0432(7) Uani 1 1 d . . .
C44 C 0.8929(2) 0.0314(3) 0.13631(17) 0.0374(6) Uani 1 1 d . . .
C45 C 0.91781(19) -0.0134(3) 0.20900(16) 0.0330(6) Uani 1 1 d . . .
C46 C 0.8465(3) 0.0019(3) 0.3266(2) 0.0497(9) Uani 1 1 d . . .
H46A H 0.8274 0.0712 0.3512 0.075 Uiso 1 1 calc R . .
H46B H 0.9069 -0.0256 0.3529 0.075 Uiso 1 1 calc R . .
H46C H 0.8011 -0.0617 0.3252 0.075 Uiso 1 1 calc R . .
C47 C 0.7016(2) 0.1639(3) 0.2189(3) 0.0621(11) Uani 1 1 d . . .
H47A H 0.6494 0.1118 0.2001 0.093 Uiso 1 1 calc R . .
H47B H 0.6908 0.2421 0.1961 0.093 Uiso 1 1 calc R . .
H47C H 0.7083 0.1722 0.2714 0.093 Uiso 1 1 calc R . .
C48 C 0.7623(3) 0.1698(3) 0.0639(2) 0.0675(13) Uani 1 1 d . . .
H48A H 0.8061 0.1954 0.0344 0.101 Uiso 1 1 calc R . .
H48B H 0.7296 0.2391 0.0775 0.101 Uiso 1 1 calc R . .
H48C H 0.7178 0.1145 0.0361 0.101 Uiso 1 1 calc R . .
C49 C 0.9387(3) -0.0004(3) 0.07425(18) 0.0513(9) Uani 1 1 d . . .
H49A H 0.9102 -0.0724 0.0505 0.077 Uiso 1 1 calc R . .
H49B H 1.0045 -0.0145 0.0926 0.077 Uiso 1 1 calc R . .
H49C H 0.9309 0.0649 0.0394 0.077 Uiso 1 1 calc R . .
C50 C 0.9869(2) -0.1111(3) 0.23517(19) 0.0409(7) Uani 1 1 d . . .
H50A H 0.9583 -0.1884 0.2215 0.061 Uiso 1 1 calc R . .
H50B H 1.0061 -0.1068 0.2879 0.061 Uiso 1 1 calc R . .
H50C H 1.0408 -0.1014 0.2130 0.061 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C43 Ru1 C44 38.00(12) . . ?
C43 Ru1 C42 38.05(13) . . ?
C44 Ru1 C42 63.43(12) . . ?
C43 Ru1 C45 63.51(11) . . ?
C44 Ru1 C45 37.82(11) . . ?
C42 Ru1 C45 63.38(11) . . ?
C43 Ru1 C41 63.37(12) . . ?
C44 Ru1 C41 63.33(11) . . ?
C42 Ru1 C41 37.63(12) . . ?
C45 Ru1 C41 38.03(10) . . ?
C43 Ru1 P1 159.04(10) . . ?
C44 Ru1 P1 142.76(8) . . ?
C42 Ru1 P1 121.28(10) . . ?
C45 Ru1 P1 107.43(8) . . ?
C41 Ru1 P1 97.52(8) . . ?
C43 Ru1 S2 95.91(9) . . ?
C44 Ru1 S2 124.07(8) . . ?
C42 Ru1 S2 101.63(8) . . ?
C45 Ru1 S2 159.38(8) . . ?
C41 Ru1 S2 135.42(8) . . ?
P1 Ru1 S2 92.35(2) . . ?
C43 Ru1 S1 110.29(10) . . ?
C44 Ru1 S1 93.68(8) . . ?
C42 Ru1 S1 148.00(10) . . ?
C45 Ru1 S1 112.75(8) . . ?
C41 Ru1 S1 150.74(8) . . ?
P1 Ru1 S1 90.59(2) . . ?
S2 Ru1 S1 71.77(2) . . ?
C11 P1 C21 105.21(13) . . ?
C11 P1 C31 97.50(12) . . ?
C21 P1 C31 103.45(13) . . ?
C11 P1 Ru1 116.70(10) . . ?
C21 P1 Ru1 111.91(9) . . ?
C31 P1 Ru1 119.97(9) . . ?
C1 S1 Ru1 87.48(9) . . ?
C1 S2 Ru1 87.85(10) . . ?
C1 O1 C2 120.3(2) . . ?
O1 C1 S1 119.6(2) . . ?
O1 C1 S2 127.5(2) . . ?
S1 C1 S2 112.90(16) . . ?
O1 C2 C4 111.0(3) . . ?
O1 C2 C3 103.6(3) . . ?
C4 C2 C3 113.7(3) . . ?
C16 C11 C12 118.8(3) . . ?
C16 C11 P1 118.7(2) . . ?
C12 C11 P1 122.3(2) . . ?
C13 C12 C11 120.3(3) . . ?
C14 C13 C12 120.1(3) . . ?
C15 C14 C13 120.3(3) . . ?
C14 C15 C16 120.1(3) . . ?
C11 C16 C15 120.4(3) . . ?
C22 C21 C26 118.2(3) . . ?
C22 C21 P1 124.5(2) . . ?
C26 C21 P1 117.0(2) . . ?
C23 C22 C21 120.1(3) . . ?
C24 C23 C22 120.8(3) . . ?
C23 C24 C25 120.0(3) . . ?
C24 C25 C26 119.7(3) . . ?
C25 C26 C21 121.1(3) . . ?
C32 C31 C36 117.3(3) . . ?
C32 C31 P1 124.7(2) . . ?
C36 C31 P1 118.0(2) . . ?
C31 C32 C33 120.3(3) . . ?
C34 C33 C32 121.6(3) . . ?
C33 C34 C35 119.0(3) . . ?
C34 C35 C36 119.9(3) . . ?
C35 C36 C31 121.9(3) . . ?
C42 C41 C45 107.8(3) . . ?
C42 C41 C46 125.8(3) . . ?
C45 C41 C46 126.0(3) . . ?
C42 C41 Ru1 70.73(17) . . ?
C45 C41 Ru1 70.56(16) . . ?
C46 C41 Ru1 129.8(2) . . ?
C41 C42 C43 108.1(3) . . ?
C41 C42 C47 125.3(3) . . ?
C43 C42 C47 125.7(3) . . ?
C41 C42 Ru1 71.63(16) . . ?
C43 C42 Ru1 70.26(17) . . ?
C47 C42 Ru1 132.2(2) . . ?
C44 C43 C42 108.1(3) . . ?
C44 C43 C48 125.9(4) . . ?
C42 C43 C48 125.9(3) . . ?
C44 C43 Ru1 71.30(17) . . ?
C42 C43 Ru1 71.69(17) . . ?
C48 C43 Ru1 126.0(2) . . ?
C43 C44 C45 108.3(3) . . ?
C43 C44 C49 125.6(3) . . ?
C45 C44 C49 126.1(3) . . ?
C43 C44 Ru1 70.70(17) . . ?
C45 C44 Ru1 71.53(16) . . ?
C49 C44 Ru1 125.3(2) . . ?
C44 C45 C41 107.8(3) . . ?
C44 C45 C50 126.3(3) . . ?
C41 C45 C50 125.1(3) . . ?
C44 C45 Ru1 70.65(16) . . ?
C41 C45 Ru1 71.41(16) . . ?
C50 C45 Ru1 131.8(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C43 2.185(3) . ?
Ru1 C44 2.193(3) . ?
Ru1 C42 2.204(3) . ?
Ru1 C45 2.205(3) . ?
Ru1 C41 2.216(3) . ?
Ru1 P1 2.3009(7) . ?
Ru1 S2 2.3974(7) . ?
Ru1 S1 2.4102(7) . ?
P1 C11 1.836(3) . ?
P1 C21 1.838(3) . ?
P1 C31 1.851(3) . ?
S1 C1 1.689(3) . ?
S2 C1 1.692(3) . ?
O1 C1 1.325(3) . ?
O1 C2 1.471(3) . ?
C2 C4 1.497(5) . ?
C2 C3 1.506(5) . ?
C11 C16 1.385(4) . ?
C11 C12 1.393(4) . ?
C12 C13 1.390(4) . ?
C13 C14 1.372(6) . ?
C14 C15 1.371(5) . ?
C15 C16 1.394(4) . ?
C21 C22 1.394(4) . ?
C21 C26 1.396(4) . ?
C22 C23 1.394(5) . ?
C23 C24 1.373(5) . ?
C24 C25 1.378(5) . ?
C25 C26 1.392(4) . ?
C31 C32 1.384(4) . ?
C31 C36 1.398(4) . ?
C32 C33 1.396(5) . ?
C33 C34 1.365(6) . ?
C34 C35 1.378(5) . ?
C35 C36 1.384(4) . ?
C41 C42 1.426(5) . ?
C41 C45 1.440(4) . ?
C41 C46 1.506(5) . ?
C42 C43 1.431(5) . ?
C42 C47 1.510(5) . ?
C43 C44 1.425(4) . ?
C43 C48 1.510(5) . ?
C44 C45 1.425(4) . ?
C44 C49 1.496(4) . ?
C45 C50 1.501(4) . ?
