#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:15:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179101 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/63/4306342.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_4306342
loop_
_publ_author_name
'Lucas Vandenburgh'
'Matthew R. Buck'
'Daniel A. Freedman'
_publ_section_title
;
Preparation, Separation, and Characterization of Ruthenium(II) Thiocyanate
Linkage Isomers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9134
_journal_page_last               9136
_journal_paper_doi               10.1021/ic801194j
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C21 H22 F6 N3 P Ru S'
_chemical_formula_weight         594.52
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 111.7720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.3255(10)
_cell_length_b                   21.8263(12)
_cell_length_c                   12.2195(7)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      30.28
_cell_measurement_theta_min      2.59
_cell_volume                     4538.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      115(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  '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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31739
_diffrn_reflns_theta_full        30.43
_diffrn_reflns_theta_max         30.43
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  0.9302
_exptl_absorpt_correction_T_min  0.7964
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         6539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0222
_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)+(0.0282P)²+5.6180P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0581
_reflns_number_gt                5943
_reflns_number_total             6539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801194j_si_001_1.cif
_cod_data_source_block           df527ru_0m
_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               4306342
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.213381(6) 0.101136(5) 0.228373(9) 0.01400(4) Uani 1 1 d . . .
N1 N 0.06789(10) 0.13951(8) 0.41450(15) 0.0367(3) Uani 1 1 d . . .
N2 N 0.19150(7) 0.19117(5) 0.26292(10) 0.0174(2) Uani 1 1 d . . .
N3 N 0.32369(7) 0.13194(6) 0.33588(10) 0.0170(2) Uani 1 1 d . . .
S1 S 0.19988(2) 0.073095(19) 0.41148(3) 0.02485(8) Uani 1 1 d . . .
C21 C 0.12128(10) 0.11250(7) 0.41120(14) 0.0242(3) Uani 1 1 d . . .
C1 C 0.24608(9) 0.08785(7) 0.07197(12) 0.0195(3) Uani 1 1 d . . .
C2 C 0.17086(8) 0.11487(7) 0.03623(12) 0.0180(3) Uani 1 1 d . . .
H2 H 0.1613 0.1514 -0.0060 0.022 Uiso 1 1 calc R . .
C3 C 0.10914(8) 0.08712(7) 0.06376(12) 0.0192(3) Uani 1 1 d . . .
H3 H 0.0600 0.1057 0.0387 0.023 Uiso 1 1 calc R . .
C4 C 0.12151(9) 0.03223(7) 0.12801(13) 0.0226(3) Uani 1 1 d . . .
C5 C 0.19781(10) 0.00524(7) 0.16517(13) 0.0238(3) Uani 1 1 d . . .
H5 H 0.2076 -0.0308 0.2087 0.029 Uiso 1 1 calc R . .
C6 C 0.25818(9) 0.03204(7) 0.13728(13) 0.0224(3) Uani 1 1 d . . .
H23 H 0.3071 0.0131 0.1618 0.027 Uiso 1 1 calc R . .
C7 C 0.05830(11) 0.00278(9) 0.15962(16) 0.0340(4) Uani 1 1 d . . .
H6 H 0.0171 0.0319 0.1500 0.051 Uiso 1 1 calc R . .
H7 H 0.0798 -0.0107 0.2401 0.051 Uiso 1 1 calc R . .
H5 H 0.0374 -0.0318 0.1091 0.051 Uiso 1 1 calc R . .
C8 C 0.31334(9) 0.11526(8) 0.04488(14) 0.0249(3) Uani 1 1 d . . .
H8 H 0.3627 0.1030 0.1075 0.030 Uiso 1 1 calc R . .
C9 C 0.31139(12) 0.18466(9) 0.03777(18) 0.0369(4) Uani 1 1 d . . .
H10 H 0.2664 0.1974 -0.0288 0.055 Uiso 1 1 calc R . .
H9 H 0.3584 0.1992 0.0291 0.055 Uiso 1 1 calc R . .
H11 H 0.3081 0.2013 0.1086 0.055 Uiso 1 1 calc R . .
C10 C 0.31163(11) 0.08750(9) -0.07131(16) 0.0322(4) Uani 1 1 d . . .
H12 H 0.2641 0.0996 -0.1342 0.048 Uiso 1 1 calc R . .
H14 H 0.3136 0.0436 -0.0651 0.048 Uiso 1 1 calc R . .
H13 H 0.3561 0.1019 -0.0874 0.048 Uiso 1 1 calc R . .
C11 C 0.25474(9) 0.22475(6) 0.33008(12) 0.0188(3) Uani 1 1 d . . .
C12 C 0.24674(10) 0.28512(7) 0.36073(14) 0.0261(3) Uani 1 1 d . . .
H15 H 0.2906 0.3074 0.4067 0.031 Uiso 1 1 calc R . .
C13 C 0.17302(11) 0.31154(7) 0.32230(15) 0.0289(3) Uani 1 1 d . . .
H16 H 0.1666 0.3518 0.3419 0.035 Uiso 1 1 calc R . .
C14 C 0.10875(10) 0.27709(7) 0.25405(15) 0.0272(3) Uani 1 1 d . . .
H17 H 0.0586 0.2941 0.2271 0.033 Uiso 1 1 calc R . .
C15 C 0.11966(9) 0.21709(7) 0.22626(14) 0.0222(3) Uani 1 1 d . . .
H18 H 0.0762 0.1941 0.1811 0.027 Uiso 1 1 calc R . .
C16 C 0.32957(8) 0.19180(7) 0.36892(12) 0.0182(3) Uani 1 1 d . . .
C17 C 0.40169(9) 0.21796(7) 0.43425(14) 0.0242(3) Uani 1 1 d . . .
H19 H 0.4049 0.2590 0.4563 0.029 Uiso 1 1 calc R . .
C18 C 0.46876(9) 0.18222(8) 0.46615(14) 0.0277(3) Uani 1 1 d . . .
H20 H 0.5178 0.1993 0.5077 0.033 Uiso 1 1 calc R . .
C19 C 0.46225(9) 0.12095(8) 0.43570(14) 0.0265(3) Uani 1 1 d . . .
H21 H 0.5065 0.0960 0.4583 0.032 Uiso 1 1 calc R . .
C20 C 0.38886(9) 0.09727(7) 0.37108(14) 0.0225(3) Uani 1 1 d . . .
H22 H 0.3845 0.0559 0.3513 0.027 Uiso 1 1 calc R . .
P1 P 0.5000 0.96157(2) 0.2500 0.02270(11) Uani 1 2 d S . .
P2 P 0.5000 0.30827(3) 0.2500 0.02632(12) Uani 1 2 d S . .
F1 F 0.42544(8) 0.96278(10) 0.13160(13) 0.0751(5) Uani 1 1 d . . .
F2 F 0.44274(7) 0.96138(5) 0.32229(11) 0.0394(3) Uani 1 1 d . . .
F3 F 0.5000 0.88964(7) 0.2500 0.0739(8) Uani 1 2 d S . .
F4 F 0.5000 1.03440(8) 0.2500 0.0728(8) Uani 1 2 d S . .
F5 F 0.5000 0.38096(8) 0.2500 0.0644(6) Uani 1 2 d S . .
F6 F 0.47778(7) 0.30777(6) 0.10951(10) 0.0400(3) Uani 1 1 d . . .
F7 F 0.40836(7) 0.30795(6) 0.22936(11) 0.0445(3) Uani 1 1 d . . .
F8 F 0.5000 0.23545(7) 0.2500 0.0373(3) Uani 1 2 d S . .
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'
F F 0.0171 0.0103 '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
N3 Ru1 N2 77.34(5) . . ?
N3 Ru1 C2 120.52(5) . . ?
N2 Ru1 C2 93.96(5) . . ?
N3 Ru1 C6 94.80(5) . . ?
N2 Ru1 C6 152.16(5) . . ?
C2 Ru1 C6 66.79(6) . . ?
N3 Ru1 C5 119.83(5) . . ?
N2 Ru1 C5 162.75(5) . . ?
C2 Ru1 C5 78.92(5) . . ?
C6 Ru1 C5 36.97(6) . . ?
N3 Ru1 C3 158.03(5) . . ?
N2 Ru1 C3 98.51(5) . . ?
C2 Ru1 C3 37.67(5) . . ?
C6 Ru1 C3 78.76(5) . . ?
C5 Ru1 C3 66.27(6) . . ?
N3 Ru1 C1 94.40(5) . . ?
N2 Ru1 C1 115.55(5) . . ?
C2 Ru1 C1 37.18(5) . . ?
C6 Ru1 C1 37.61(6) . . ?
C5 Ru1 C1 67.52(6) . . ?
C3 Ru1 C1 67.62(5) . . ?
N3 Ru1 C4 156.72(5) . . ?
N2 Ru1 C4 125.47(5) . . ?
C2 Ru1 C4 67.23(5) . . ?
C6 Ru1 C4 67.14(6) . . ?
C5 Ru1 C4 37.28(6) . . ?
C3 Ru1 C4 36.57(5) . . ?
C1 Ru1 C4 80.22(5) . . ?
N3 Ru1 S1 84.61(3) . . ?
N2 Ru1 S1 87.58(3) . . ?
C2 Ru1 S1 154.57(4) . . ?
C6 Ru1 S1 118.60(4) . . ?
C5 Ru1 S1 92.25(4) . . ?
C3 Ru1 S1 116.99(4) . . ?
C1 Ru1 S1 156.13(4) . . ?
C4 Ru1 S1 91.29(4) . . ?
C15 N2 C11 118.90(13) . . ?
C15 N2 Ru1 124.55(10) . . ?
C11 N2 Ru1 116.52(9) . . ?
C20 N3 C16 118.90(13) . . ?
C20 N3 Ru1 124.25(10) . . ?
C16 N3 Ru1 116.82(9) . . ?
C21 S1 Ru1 104.53(6) . . ?
N1 C21 S1 178.03(16) . . ?
C2 C1 C6 117.45(13) . . ?
C2 C1 C8 123.26(14) . . ?
C6 C1 C8 119.30(14) . . ?
C2 C1 Ru1 70.60(8) . . ?
C6 C1 Ru1 70.52(8) . . ?
C8 C1 Ru1 129.60(10) . . ?
C1 C2 C3 121.17(13) . . ?
C1 C2 Ru1 72.21(8) . . ?
C3 C2 Ru1 71.90(8) . . ?
C4 C3 C2 121.04(13) . . ?
C4 C3 Ru1 72.84(8) . . ?
C2 C3 Ru1 70.42(8) . . ?
C3 C4 C5 117.78(14) . . ?
C3 C4 C7 122.10(15) . . ?
C5 C4 C7 120.11(14) . . ?
C3 C4 Ru1 70.58(8) . . ?
C5 C4 Ru1 69.88(8) . . ?
C7 C4 Ru1 129.86(11) . . ?
C6 C5 C4 121.28(14) . . ?
C6 C5 Ru1 71.25(8) . . ?
C4 C5 Ru1 72.84(8) . . ?
C5 C6 C1 121.28(14) . . ?
C5 C6 Ru1 71.78(9) . . ?
C1 C6 Ru1 71.88(8) . . ?
C1 C8 C9 113.81(14) . . ?
C1 C8 C10 107.93(13) . . ?
C9 C8 C10 110.47(15) . . ?
N2 C11 C12 121.42(14) . . ?
N2 C11 C16 114.67(12) . . ?
C12 C11 C16 123.89(14) . . ?
C13 C12 C11 119.41(15) . . ?
C12 C13 C14 118.95(14) . . ?
C13 C14 C15 119.51(15) . . ?
N2 C15 C14 121.81(15) . . ?
N3 C16 C17 121.31(14) . . ?
N3 C16 C11 114.49(12) . . ?
C17 C16 C11 124.21(14) . . ?
C18 C17 C16 119.12(15) . . ?
C19 C18 C17 119.39(14) . . ?
C18 C19 C20 118.96(15) . . ?
N3 C20 C19 122.24(15) . . ?
F3 P1 F1 90.96(8) . . ?
F3 P1 F1 90.96(8) . 2_655 ?
F1 P1 F1 178.09(16) . 2_655 ?
F3 P1 F4 180.0 . . ?
F1 P1 F4 89.04(8) . . ?
F1 P1 F4 89.04(8) 2_655 . ?
F3 P1 F2 89.86(4) . . ?
F1 P1 F2 89.09(7) . . ?
F1 P1 F2 90.91(7) 2_655 . ?
F4 P1 F2 90.14(4) . . ?
F3 P1 F2 89.86(4) . 2_655 ?
F1 P1 F2 90.91(7) . 2_655 ?
F1 P1 F2 89.09(7) 2_655 2_655 ?
F4 P1 F2 90.14(4) . 2_655 ?
F2 P1 F2 179.71(9) . 2_655 ?
F5 P2 F8 180.0 . . ?
F5 P2 F7 90.26(5) . 2_655 ?
F8 P2 F7 89.74(5) . 2_655 ?
F5 P2 F7 90.26(5) . . ?
F8 P2 F7 89.74(5) . . ?
F7 P2 F7 179.49(11) 2_655 . ?
F5 P2 F6 90.39(5) . . ?
F8 P2 F6 89.61(5) . . ?
F7 P2 F6 90.21(6) 2_655 . ?
F7 P2 F6 89.79(6) . . ?
F5 P2 F6 90.39(5) . 2_655 ?
F8 P2 F6 89.61(5) . 2_655 ?
F7 P2 F6 89.79(6) 2_655 2_655 ?
F7 P2 F6 90.21(6) . 2_655 ?
F6 P2 F6 179.22(10) . 2_655 ?
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 N3 2.0722(12) . ?
Ru1 N2 2.0800(12) . ?
Ru1 C2 2.2028(14) . ?
Ru1 C6 2.2058(14) . ?
Ru1 C5 2.2126(15) . ?
Ru1 C3 2.2222(14) . ?
Ru1 C1 2.2237(14) . ?
Ru1 C4 2.2514(14) . ?
Ru1 S1 2.4193(4) . ?
N1 C21 1.156(2) . ?
N2 C15 1.3478(18) . ?
N2 C11 1.3594(19) . ?
N3 C20 1.3428(18) . ?
N3 C16 1.3598(18) . ?
S1 C21 1.6766(17) . ?
C1 C2 1.411(2) . ?
C1 C6 1.428(2) . ?
C1 C8 1.513(2) . ?
C2 C3 1.429(2) . ?
C3 C4 1.404(2) . ?
C4 C5 1.427(2) . ?
C4 C7 1.495(2) . ?
C5 C6 1.401(2) . ?
C8 C9 1.517(3) . ?
C8 C10 1.533(2) . ?
C11 C12 1.392(2) . ?
C11 C16 1.463(2) . ?
C12 C13 1.381(2) . ?
C13 C14 1.385(3) . ?
C14 C15 1.386(2) . ?
C16 C17 1.388(2) . ?
C17 C18 1.384(2) . ?
C18 C19 1.381(2) . ?
C19 C20 1.383(2) . ?
P1 F3 1.5699(17) . ?
P1 F1 1.5793(14) . ?
P1 F1 1.5793(14) 2_655 ?
P1 F4 1.5896(17) . ?
P1 F2 1.6029(10) . ?
P1 F2 1.6029(10) 2_655 ?
P2 F5 1.5866(18) . ?
P2 F8 1.5895(15) . ?
P2 F7 1.6030(11) 2_655 ?
P2 F7 1.6030(11) . ?
P2 F6 1.6107(11) . ?
P2 F6 1.6107(11) 2_655 ?
