#------------------------------------------------------------------------------
#$Date: 2022-05-07 01:39:13 +0200 (Sat 07 de May de 2022) $
#$Revision: 275158 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/21/7012141.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_7012141
loop_
_publ_author_name
'Watanabe, Masanobu'
'Sato, Masaru'
'Kai, Masahiro'
_publ_section_title
;
 Synthesis of the first non-carbonyl cisoid fulvalene complexes with an
 Ru--Ru bond bridged by thiolate ligands
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              651
_journal_paper_doi               10.1039/b207928n
_journal_year                    2003
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C54 H50 F12 N4 P4 Ru2 '
_chemical_formula_sum            'C54 H50 F12 N4 P4 Ru2'
_chemical_formula_weight         1309.034
_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_primary     vecmap
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                83.319(6)
_cell_angle_beta                 103.008(7)
_cell_angle_gamma                104.474(8)
_cell_formula_units_Z            1
_cell_length_a                   9.1510(8)
_cell_length_b                   10.180(2)
_cell_length_c                   15.852(2)
_cell_measurement_temperature    298
_cell_volume                     1390.3(4)
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Buerskens et al., 1992)'
_diffrn_measured_fraction_theta_full 0.615
_diffrn_measured_fraction_theta_max 0.615
_diffrn_measurement_device       KappaCCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01663
_diffrn_orient_matrix_UB_12      0.10117
_diffrn_orient_matrix_UB_13      -0.00516
_diffrn_orient_matrix_UB_21      0.10473
_diffrn_orient_matrix_UB_22      0.00649
_diffrn_orient_matrix_UB_23      -0.01137
_diffrn_orient_matrix_UB_31      -0.04735
_diffrn_orient_matrix_UB_32      -0.01445
_diffrn_orient_matrix_UB_33      -0.06421
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6567
_diffrn_reflns_theta_full        32.17
_diffrn_reflns_theta_max         32.17
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.051
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0892
_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)+(0.0180P)²+13.6800P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1845
_refine_ls_wR_factor_ref         0.1876
_reflns_number_gt                5731
_reflns_number_total             6024
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207928n.txt
_cod_data_source_block           compond_2b
_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_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_cell_volume        1390.3(3)
_cod_original_sg_symbol_H-M      'P -1          '
_cod_original_formula_sum        'C54 H50 F12 N4 P4 Ru2 '
_cod_database_code               7012141
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.17609(7) 0.93038(6) 0.14353(4) 0.03467(17) Uani 1 1 d . . .
P1 P 0.2824(2) 0.95547(18) 0.29113(11) 0.0348(4) Uani 1 1 d . . .
N1 N -0.0473(8) 0.8359(7) 0.1534(4) 0.0453(16) Uani 1 1 d . . .
N2 N 0.2185(8) 0.7403(6) 0.1426(4) 0.0448(15) Uani 1 1 d . . .
C1 C 0.0806(9) 1.0226(7) 0.0241(4) 0.0413(18) Uani 1 1 d . . .
C2 C 0.2044(10) 0.9713(8) 0.0099(5) 0.048(2) Uani 1 1 d . . .
C3 C 0.3434(10) 1.0381(9) 0.0725(5) 0.049(2) Uani 1 1 d . . .
C4 C 0.3026(10) 1.1337(8) 0.1220(5) 0.052(2) Uani 1 1 d . . .
C5 C 0.1403(9) 1.1211(7) 0.0949(5) 0.0441(18) Uani 1 1 d . . .
C6 C -0.1755(10) 0.7907(9) 0.1420(6) 0.054(2) Uani 1 1 d . . .
C7 C -0.3441(12) 0.7310(12) 0.1243(8) 0.084(4) Uani 1 1 d . . .
C8 C 0.2370(11) 0.6378(9) 0.1350(6) 0.055(2) Uani 1 1 d . . .
C9 C 0.2598(15) 0.5020(10) 0.1240(9) 0.086(4) Uani 1 1 d . . .
C10 C 0.1795(9) 0.8500(7) 0.3645(4) 0.0399(16) Uani 1 1 d . . .
C11 C 0.1877(11) 0.8948(10) 0.4487(5) 0.055(2) Uani 1 1 d . . .
C12 C 0.1141(12) 0.8091(10) 0.5030(6) 0.064(3) Uani 1 1 d . . .
C13 C 0.0289(12) 0.6814(10) 0.4740(6) 0.065(3) Uani 1 1 d . . .
C14 C 0.0194(11) 0.6350(8) 0.3914(6) 0.054(2) Uani 1 1 d . . .
C15 C 0.0925(10) 0.7189(8) 0.3356(5) 0.0445(18) Uani 1 1 d . . .
C16 C 0.3164(9) 1.1294(7) 0.3351(4) 0.0412(17) Uani 1 1 d . . .
C17 C 0.4595(11) 1.2051(9) 0.3798(6) 0.057(2) Uani 1 1 d . . .
C18 C 0.4802(15) 1.3404(11) 0.4039(8) 0.080(3) Uani 1 1 d . . .
C19 C 0.3547(17) 1.3958(11) 0.3880(7) 0.082(4) Uani 1 1 d . . .
C20 C 0.2110(15) 1.3205(11) 0.3454(7) 0.075(3) Uani 1 1 d . . .
C21 C 0.1921(11) 1.1876(9) 0.3192(6) 0.055(2) Uani 1 1 d . . .
C22 C 0.4729(9) 0.9204(7) 0.3186(4) 0.0385(16) Uani 1 1 d . . .
C23 C 0.5098(11) 0.8229(10) 0.3746(6) 0.060(2) Uani 1 1 d . . .
C24 C 0.6549(13) 0.7980(11) 0.3895(7) 0.076(3) Uani 1 1 d . . .
C25 C 0.7654(12) 0.8710(11) 0.3497(7) 0.070(3) Uani 1 1 d . . .
C26 C 0.7314(11) 0.9697(10) 0.2938(6) 0.061(2) Uani 1 1 d . . .
C27 C 0.5852(10) 0.9946(9) 0.2786(5) 0.052(2) Uani 1 1 d . . .
P2 P 0.7744(4) 0.3600(3) 0.1495(3) 0.0815(9) Uani 1 1 d . . .
F1 F 0.6920(14) 0.2092(10) 0.1302(10) 0.190(6) Uani 1 1 d . . .
F2 F 0.8717(15) 0.4957(11) 0.1857(9) 0.198(6) Uani 1 1 d . . .
F3 F 0.866(3) 0.316(2) 0.2282(17) 0.395(18) Uani 1 1 d . . .
F4 F 0.8913(17) 0.3375(15) 0.1006(15) 0.252(9) Uani 1 1 d . . .
F5 F 0.699(3) 0.402(3) 0.0724(9) 0.367(14) Uani 1 1 d . . .
F6 F 0.6494(17) 0.3740(15) 0.1894(12) 0.244(8) Uani 1 1 d . . .
H2 H 0.1954 0.8981 -0.0256 0.058 Uiso 1 1 d R . .
H3 H 0.4681 1.0349 0.0622 0.058 Uiso 1 1 d R . .
H4 H 0.3805 1.1913 0.1640 0.062 Uiso 1 1 d R . .
H5 H 0.1070 1.1784 0.1137 0.053 Uiso 1 1 d R . .
H7A H -0.3926 0.7578 0.1652 0.101 Uiso 1 1 d R . .
H7B H -0.3596 0.6339 0.1286 0.101 Uiso 1 1 d R . .
H7C H -0.3885 0.7606 0.0666 0.101 Uiso 1 1 d R . .
H9A H 0.2639 0.4905 0.0654 0.104 Uiso 1 1 d R . .
H9B H 0.1768 0.4336 0.1413 0.104 Uiso 1 1 d R . .
H9C H 0.3554 0.4934 0.1617 0.104 Uiso 1 1 d R . .
H11 H 0.2524 0.9755 0.4665 0.066 Uiso 1 1 d R . .
H12 H 0.1161 0.8518 0.5615 0.077 Uiso 1 1 d R . .
H13 H -0.0234 0.6341 0.5105 0.078 Uiso 1 1 d R . .
H14 H -0.0238 0.5642 0.3693 0.065 Uiso 1 1 d R . .
H15 H 0.0840 0.6855 0.2790 0.053 Uiso 1 1 d R . .
H17 H 0.5384 1.1786 0.3785 0.069 Uiso 1 1 d R . .
H18 H 0.5952 1.4024 0.4403 0.096 Uiso 1 1 d R . .
H19 H 0.3540 1.4685 0.4034 0.098 Uiso 1 1 d R . .
H20 H 0.1231 1.3600 0.3339 0.090 Uiso 1 1 d R . .
H21 H 0.1022 1.1408 0.2913 0.066 Uiso 1 1 d R . .
H23 H 0.4169 0.7612 0.4001 0.072 Uiso 1 1 d R . .
H24 H 0.6830 0.7248 0.4335 0.092 Uiso 1 1 d R . .
H25 H 0.8648 0.8500 0.3604 0.084 Uiso 1 1 d R . .
H26 H 0.8075 1.0245 0.2635 0.073 Uiso 1 1 d R . .
H27 H 0.5625 1.0685 0.2385 0.062 Uiso 1 1 d 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'
P P 0.1023 0.0942 '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'
Ru Ru -1.2594 0.8363 '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'
loop_
_diffrn_radiation_wavelength
0.71073
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
N1 Ru1 N2 88.4(3) . . ?
N1 Ru1 C5 98.4(3) . . ?
N2 Ru1 C5 157.7(3) . . ?
N1 Ru1 C3 152.3(3) . . ?
N2 Ru1 C3 96.9(3) . . ?
C5 Ru1 C3 67.6(3) . . ?
N1 Ru1 C1 86.8(3) . . ?
N2 Ru1 C1 118.0(3) . . ?
C5 Ru1 C1 42.1(3) . . ?
C3 Ru1 C1 66.7(3) . . ?
N1 Ru1 C4 136.5(3) . . ?
N2 Ru1 C4 134.3(3) . . ?
C5 Ru1 C4 39.6(3) . . ?
C3 Ru1 C4 40.8(3) . . ?
C1 Ru1 C4 68.0(3) . . ?
N1 Ru1 C2 112.7(3) . . ?
N2 Ru1 C2 89.1(3) . . ?
C5 Ru1 C2 68.7(3) . . ?
C3 Ru1 C2 40.7(3) . . ?
C1 Ru1 C2 38.9(3) . . ?
C4 Ru1 C2 68.8(3) . . ?
N1 Ru1 P1 98.57(18) . . ?
N2 Ru1 P1 95.16(19) . . ?
C5 Ru1 P1 104.6(2) . . ?
C3 Ru1 P1 108.0(2) . . ?
C1 Ru1 P1 146.7(2) . . ?
C4 Ru1 P1 86.6(2) . . ?
C2 Ru1 P1 148.6(2) . . ?
C10 P1 C22 105.2(3) . . ?
C10 P1 C16 101.4(4) . . ?
C22 P1 C16 102.9(3) . . ?
C10 P1 Ru1 116.5(3) . . ?
C22 P1 Ru1 110.7(2) . . ?
C16 P1 Ru1 118.4(2) . . ?
C6 N1 Ru1 166.6(7) . . ?
C8 N2 Ru1 174.4(7) . . ?
C2 C1 C1 122.6(9) . 2_575 ?
C2 C1 C5 109.6(6) . . ?
C1 C1 C5 127.8(9) 2_575 . ?
C2 C1 Ru1 72.6(4) . . ?
C1 C1 Ru1 124.7(7) 2_575 . ?
C5 C1 Ru1 67.6(3) . . ?
C1 C2 C3 105.5(7) . . ?
C1 C2 Ru1 68.5(4) . . ?
C3 C2 Ru1 67.6(4) . . ?
C4 C3 C2 109.9(7) . . ?
C4 C3 Ru1 70.4(5) . . ?
C2 C3 Ru1 71.7(4) . . ?
C5 C4 C3 106.8(7) . . ?
C5 C4 Ru1 68.2(4) . . ?
C3 C4 Ru1 68.8(4) . . ?
C4 C5 C1 108.1(7) . . ?
C4 C5 Ru1 72.3(4) . . ?
C1 C5 Ru1 70.2(4) . . ?
N1 C6 C7 178.4(11) . . ?
N2 C8 C9 179.2(12) . . ?
C15 C10 C11 123.6(7) . . ?
C15 C10 P1 116.0(6) . . ?
C11 C10 P1 120.3(6) . . ?
C12 C11 C10 117.9(9) . . ?
C11 C12 C13 118.0(9) . . ?
C12 C13 C14 125.1(8) . . ?
C15 C14 C13 118.2(9) . . ?
C14 C15 C10 117.2(8) . . ?
C21 C16 C17 117.6(8) . . ?
C21 C16 P1 116.6(6) . . ?
C17 C16 P1 125.7(6) . . ?
C16 C17 C18 122.8(9) . . ?
C19 C18 C17 118.4(10) . . ?
C18 C19 C20 119.3(10) . . ?
C19 C20 C21 122.0(10) . . ?
C16 C21 C20 119.7(9) . . ?
C23 C22 C27 116.1(8) . . ?
C23 C22 P1 123.9(7) . . ?
C27 C22 P1 120.0(5) . . ?
C22 C23 C24 120.9(9) . . ?
C25 C24 C23 122.9(9) . . ?
C26 C25 C24 117.4(9) . . ?
C25 C26 C27 119.8(9) . . ?
C22 C27 C26 123.0(8) . . ?
F5 P2 F3 174.8(18) . . ?
F5 P2 F6 89.6(12) . . ?
F3 P2 F6 95.6(16) . . ?
F5 P2 F4 86.3(13) . . ?
F3 P2 F4 88.5(14) . . ?
F6 P2 F4 174.0(10) . . ?
F5 P2 F2 101.8(13) . . ?
F3 P2 F2 77.8(10) . . ?
F6 P2 F2 89.1(8) . . ?
F4 P2 F2 96.1(7) . . ?
F5 P2 F1 89.8(13) . . ?
F3 P2 F1 90.7(10) . . ?
F6 P2 F1 91.3(7) . . ?
F4 P2 F1 84.3(7) . . ?
F2 P2 F1 168.4(9) . . ?
C1 C2 H2 126.4 . . ?
C3 C2 H2 127.4 . . ?
Ru1 C2 H2 120.7 . . ?
C4 C3 H3 128.5 . . ?
C2 C3 H3 118.8 . . ?
Ru1 C3 H3 139.5 . . ?
C5 C4 H4 131.4 . . ?
C3 C4 H4 121.8 . . ?
Ru1 C4 H4 128.0 . . ?
C4 C5 H5 114.6 . . ?
C1 C5 H5 135.9 . . ?
Ru1 C5 H5 133.1 . . ?
C6 C7 H7A 111.3 . . ?
C6 C7 H7B 108.0 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.1 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C8 C9 H9A 112.6 . . ?
C8 C9 H9B 108.7 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 107.0 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C11 H11 121.0 . . ?
C10 C11 H11 120.6 . . ?
C11 C12 H12 113.9 . . ?
C13 C12 H12 127.6 . . ?
C12 C13 H13 113.0 . . ?
C14 C13 H13 121.8 . . ?
C15 C14 H14 109.2 . . ?
C13 C14 H14 132.6 . . ?
C14 C15 H15 117.1 . . ?
C10 C15 H15 125.8 . . ?
C16 C17 H17 117.0 . . ?
C18 C17 H17 117.7 . . ?
C19 C18 H18 118.1 . . ?
C17 C18 H18 123.4 . . ?
C18 C19 H19 125.1 . . ?
C20 C19 H19 115.5 . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 118.9 . . ?
C16 C21 H21 118.1 . . ?
C20 C21 H21 122.1 . . ?
C22 C23 H23 114.1 . . ?
C24 C23 H23 124.7 . . ?
C25 C24 H24 116.8 . . ?
C23 C24 H24 120.3 . . ?
C26 C25 H25 121.6 . . ?
C24 C25 H25 121.0 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.2 . . ?
C22 C27 H27 118.0 . . ?
C26 C27 H27 119.0 . . ?
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 N1 2.063(7) . ?
Ru1 N2 2.069(6) . ?
Ru1 C5 2.080(7) . ?
Ru1 C3 2.113(8) . ?
Ru1 C1 2.117(6) . ?
Ru1 C4 2.135(7) . ?
Ru1 C2 2.171(7) . ?
Ru1 P1 2.3402(18) . ?
P1 C10 1.757(8) . ?
P1 C22 1.813(8) . ?
P1 C16 1.906(8) . ?
N1 C6 1.129(10) . ?
N2 C8 1.122(10) . ?
C1 C2 1.429(12) . ?
C1 C1 1.486(14) 2_575 ?
C1 C5 1.509(10) . ?
C2 C3 1.491(11) . ?
C3 C4 1.481(13) . ?
C4 C5 1.427(11) . ?
C6 C7 1.485(13) . ?
C8 C9 1.484(13) . ?
C10 C15 1.439(11) . ?
C10 C11 1.441(11) . ?
C11 C12 1.322(12) . ?
C12 C13 1.407(14) . ?
C13 C14 1.420(13) . ?
C14 C15 1.328(11) . ?
C16 C21 1.372(11) . ?
C16 C17 1.420(11) . ?
C17 C18 1.427(14) . ?
C18 C19 1.364(16) . ?
C19 C20 1.410(16) . ?
C20 C21 1.419(13) . ?
C22 C23 1.311(10) . ?
C22 C27 1.350(11) . ?
C23 C24 1.377(13) . ?
C24 C25 1.333(15) . ?
C25 C26 1.310(13) . ?
C26 C27 1.386(12) . ?
P2 F5 1.339(13) . ?
P2 F3 1.431(15) . ?
P2 F6 1.468(11) . ?
P2 F4 1.528(13) . ?
P2 F2 1.540(9) . ?
P2 F1 1.563(10) . ?
C2 H2 0.9617 . ?
C3 H3 1.1973 . ?
C4 H4 0.9816 . ?
C5 H5 0.8319 . ?
C7 H7A 0.9601 . ?
C7 H7B 0.9599 . ?
C7 H7C 0.9601 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9599 . ?
C9 H9C 0.9600 . ?
C11 H11 0.9168 . ?
C12 H12 1.0637 . ?
C13 H13 0.8604 . ?
C14 H14 0.8077 . ?
C15 H15 0.9765 . ?
C17 H17 0.8366 . ?
C18 H18 1.1482 . ?
C19 H19 0.8082 . ?
C20 H20 0.9595 . ?
C21 H21 0.8880 . ?
C23 H23 1.0529 . ?
C24 H24 1.0010 . ?
C25 H25 0.9598 . ?
C26 H26 0.9597 . ?
C27 H27 0.9595 . ?
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2022-05-07T02:35:00+03:00
;
 Replaced the '&#x00A5;' sequences with backslash symbols ('\')
 in multiple data values.
;
