#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/10/95/4109567.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_4109567
loop_
_publ_author_name
'Soon Hyeok Hong'
'Anna G. Wenzel'
'Tina T. Salguero'
'Michael W. Day'
'Robert H. Grubbs'
_publ_section_title
;
 Decomposition of Ruthenium Olefin Metathesis Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7961
_journal_page_last               7968
_journal_paper_doi               10.1021/ja0713577
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C46 H58 Cl2 N4 Ru2'
_chemical_formula_sum            'C46 H58 Cl2 N4 Ru2'
_chemical_formula_weight         940.00
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.828(2)
_cell_angle_beta                 98.018(2)
_cell_angle_gamma                116.4470(10)
_cell_formula_units_Z            1
_cell_length_a                   9.8735(6)
_cell_length_b                   10.7053(7)
_cell_length_c                   11.8315(7)
_cell_measurement_reflns_used    8556
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.51
_cell_measurement_theta_min      2.21
_cell_volume                     1063.77(12)
_computing_cell_refinement       'Bruker SAINT v6.45A'
_computing_data_collection       'Bruker SMART v5.630'
_computing_data_reduction        'Bruker SAINT v6.45A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF v6.12'
_computing_structure_refinement  'Bruker XL v6.12'
_computing_structure_solution    'Bruker XS v6.12'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.841
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       'ω scans at 6 φ settings'
_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  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0889
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19483
_diffrn_reflns_theta_full        34.93
_diffrn_reflns_theta_max         34.93
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_T_max  0.9415
_exptl_absorpt_correction_T_min  0.8380
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dichroic - Red/brown'
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_meas      0
_exptl_crystal_description       Plate
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.257
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    Unrestrained
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     360
_refine_ls_number_reflns         7835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s²(Fo²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                5514
_reflns_number_total             7835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0713577si20070226_014637.cif
_cod_data_source_block           compound21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Difference Fourier map' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1063.77(11)
_cod_database_code               4109567
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
Ru1 Ru 0.55804(2) 0.68828(2) 0.587948(15) 0.01807(6) Uani 1 1 d
Cl1 Cl 0.36346(6) 0.43684(6) 0.57292(4) 0.02225(12) Uani 1 1 d
N1 N 0.5407(2) 0.8846(2) 0.80791(15) 0.0226(4) Uani 1 1 d
N2 N 0.3784(2) 0.8212(2) 0.63593(15) 0.0259(5) Uani 1 1 d
C1 C 0.4919(2) 0.7991(2) 0.69301(18) 0.0204(5) Uani 1 1 d
C2 C 0.4490(4) 0.9596(4) 0.8297(2) 0.0410(8) Uani 1 1 d
C3 C 0.3580(4) 0.9368(3) 0.7075(2) 0.0315(6) Uani 1 1 d
C4 C 0.6160(3) 0.8616(3) 0.90833(17) 0.0209(5) Uani 1 1 d
C5 C 0.5372(3) 0.7352(2) 0.94236(18) 0.0221(5) Uani 1 1 d
C6 C 0.6097(3) 0.7212(3) 1.0440(2) 0.0256(5) Uani 1 1 d
C7 C 0.7571(3) 0.8289(3) 1.11447(19) 0.0245(5) Uani 1 1 d
C8 C 0.8293(3) 0.9536(3) 1.0795(2) 0.0242(5) Uani 1 1 d
C9 C 0.7632(3) 0.9748(3) 0.97894(18) 0.0221(5) Uani 1 1 d
C10 C 0.3759(3) 0.6167(3) 0.8701(2) 0.0305(6) Uani 1 1 d
C11 C 0.8331(4) 0.8104(4) 1.2243(3) 0.0359(6) Uani 1 1 d
C12 C 0.8429(3) 1.1170(3) 0.9504(2) 0.0283(6) Uani 1 1 d
C13 C 0.3288(3) 0.7659(3) 0.50889(19) 0.0261(5) Uani 1 1 d
C14 C 0.1697(3) 0.6957(3) 0.4507(2) 0.0385(7) Uani 1 1 d
C15 C 0.1288(3) 0.6341(4) 0.3282(2) 0.0419(8) Uani 1 1 d
C16 C 0.2360(3) 0.6342(3) 0.2644(2) 0.0332(6) Uani 1 1 d
C17 C 0.3906(3) 0.7047(3) 0.3241(2) 0.0277(6) Uani 1 1 d
C18 C 0.4427(3) 0.7775(3) 0.44638(19) 0.0243(5) Uani 1 1 d
C19 C 0.0482(4) 0.6844(6) 0.5159(4) 0.0687(13) Uani 1 1 d
C20 C 0.1827(4) 0.5558(4) 0.1328(2) 0.0445(8) Uani 1 1 d
C21 C 0.6105(3) 0.8574(3) 0.5118(2) 0.0249(5) Uani 1 1 d
C22 C 0.7925(3) 0.8196(3) 0.6807(2) 0.0257(6) Uani 1 1 d
C23 C 0.7314(3) 0.6891(3) 0.7123(2) 0.0265(6) Uani 1 1 d
H2A H 0.517(3) 1.050(3) 0.870(2) 0.035(8) Uiso 1 1 d
H2B H 0.388(4) 0.920(4) 0.882(3) 0.082(13) Uiso 1 1 d
H3A H 0.258(4) 0.905(3) 0.701(3) 0.054(9) Uiso 1 1 d
H3B H 0.420(3) 1.028(3) 0.683(2) 0.033(7) Uiso 1 1 d
H6 H 0.563(3) 0.647(3) 1.064(2) 0.017(6) Uiso 1 1 d
H8 H 0.917(3) 1.025(3) 1.121(2) 0.022(6) Uiso 1 1 d
H10A H 0.383(3) 0.577(3) 0.795(2) 0.031(7) Uiso 1 1 d
H10B H 0.313(3) 0.656(3) 0.856(2) 0.026(7) Uiso 1 1 d
H10C H 0.326(3) 0.544(3) 0.913(2) 0.028(7) Uiso 1 1 d
H11A H 0.761(3) 0.745(3) 1.252(2) 0.046(9) Uiso 1 1 d
H11B H 0.889(4) 0.904(4) 1.288(3) 0.064(10) Uiso 1 1 d
H11C H 0.898(4) 0.780(3) 1.204(3) 0.056(10) Uiso 1 1 d
H12A H 0.812(3) 1.184(3) 0.987(2) 0.041(8) Uiso 1 1 d
H12B H 0.818(3) 1.109(3) 0.873(2) 0.025(6) Uiso 1 1 d
H12C H 0.947(3) 1.159(3) 0.976(2) 0.039(8) Uiso 1 1 d
H15 H 0.031(3) 0.589(3) 0.291(2) 0.029(7) Uiso 1 1 d
H17 H 0.457(3) 0.701(3) 0.289(2) 0.027(7) Uiso 1 1 d
H19A H 0.062(3) 0.645(3) 0.582(3) 0.047(9) Uiso 1 1 d
H19B H -0.060(4) 0.618(4) 0.476(3) 0.067(10) Uiso 1 1 d
H19C H 0.043(4) 0.777(4) 0.533(3) 0.082(13) Uiso 1 1 d
H20A H 0.084(5) 0.532(4) 0.105(4) 0.098(15) Uiso 1 1 d
H20B H 0.185(4) 0.473(4) 0.121(3) 0.078(13) Uiso 1 1 d
H20C H 0.248(4) 0.617(4) 0.084(3) 0.086(13) Uiso 1 1 d
H21A H 0.660(3) 0.966(3) 0.570(2) 0.032(7) Uiso 1 1 d
H21B H 0.673(3) 0.867(3) 0.465(3) 0.049(9) Uiso 1 1 d
H22A H 0.865(3) 0.832(3) 0.628(2) 0.031(7) Uiso 1 1 d
H22B H 0.820(3) 0.914(3) 0.737(2) 0.039(7) Uiso 1 1 d
H23A H 0.715(3) 0.688(3) 0.794(2) 0.041(8) Uiso 1 1 d
H23B H 0.758(2) 0.617(2) 0.6823(18) 0.011(5) Uiso 1 1 d
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'
Cl Cl 0.1484 0.1585 '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_3
_geom_angle_publ_flag
C1 Ru1 C21 82.08(10) . yes
C1 Ru1 C22 92.40(9) . yes
C21 Ru1 C22 81.43(10) . yes
C1 Ru1 C23 99.58(9) . yes
C21 Ru1 C23 120.55(10) . yes
C22 Ru1 C23 39.21(10) . yes
C1 Ru1 Cl1 101.39(7) . yes
C21 Ru1 Cl1 144.76(6) . yes
C22 Ru1 Cl1 132.79(8) . yes
C23 Ru1 Cl1 93.71(8) . yes
C1 Ru1 Cl1 170.94(7) 2_666 yes
C21 Ru1 Cl1 89.68(7) 2_666 yes
C22 Ru1 Cl1 90.07(6) 2_666 yes
C23 Ru1 Cl1 87.82(6) 2_666 yes
Cl1 Ru1 Cl1 83.190(19) 2_666 yes
Ru1 Cl1 Ru1 96.809(19) 2_666 yes
C1 N1 C4 125.42(18) . ?
C1 N1 C2 111.87(19) . ?
C4 N1 C2 117.47(17) . ?
C1 N2 C13 117.14(17) . ?
C1 N2 C3 114.08(18) . ?
C13 N2 C3 125.8(2) . ?
N2 C1 N1 106.28(18) . ?
N2 C1 Ru1 113.79(14) . ?
N1 C1 Ru1 138.88(16) . ?
N1 C2 C3 104.26(19) . ?
N1 C2 H2A 105.9(18) . ?
C3 C2 H2A 116.6(19) . ?
N1 C2 H2B 109(2) . ?
C3 C2 H2B 115(2) . ?
H2A C2 H2B 106(3) . ?
N2 C3 C2 101.3(2) . ?
N2 C3 H3A 109(2) . ?
C2 C3 H3A 114(2) . ?
N2 C3 H3B 106.7(14) . ?
C2 C3 H3B 106.2(14) . ?
H3A C3 H3B 119(3) . ?
C5 C4 C9 120.7(2) . ?
C5 C4 N1 120.10(19) . ?
C9 C4 N1 118.8(2) . ?
C6 C5 C4 118.4(2) . ?
C6 C5 C10 120.7(2) . ?
C4 C5 C10 120.9(2) . ?
C5 C6 C7 122.6(2) . ?
C5 C6 H6 118.5(17) . ?
C7 C6 H6 118.9(17) . ?
C8 C7 C6 117.3(2) . ?
C8 C7 C11 121.4(2) . ?
C6 C7 C11 121.4(2) . ?
C7 C8 C9 123.1(2) . ?
C7 C8 H8 121.7(17) . ?
C9 C8 H8 115.1(17) . ?
C8 C9 C4 117.8(2) . ?
C8 C9 C12 120.5(2) . ?
C4 C9 C12 121.6(2) . ?
C5 C10 H10A 108.8(15) . ?
C5 C10 H10B 109.9(16) . ?
H10A C10 H10B 105(2) . ?
C5 C10 H10C 111.9(14) . ?
H10A C10 H10C 114(2) . ?
H10B C10 H10C 107(2) . ?
C7 C11 H11A 111.0(19) . ?
C7 C11 H11B 110.3(19) . ?
H11A C11 H11B 108(3) . ?
C7 C11 H11C 107(2) . ?
H11A C11 H11C 110(3) . ?
H11B C11 H11C 111(3) . ?
C9 C12 H12A 111.1(17) . ?
C9 C12 H12B 113.0(16) . ?
H12A C12 H12B 105(2) . ?
C9 C12 H12C 111.4(19) . ?
H12A C12 H12C 107(2) . ?
H12B C12 H12C 109(2) . ?
C14 C13 C18 121.6(2) . ?
C14 C13 N2 120.1(2) . ?
C18 C13 N2 118.20(19) . ?
C15 C14 C13 117.0(2) . ?
C15 C14 C19 120.9(3) . ?
C13 C14 C19 122.1(2) . ?
C16 C15 C14 123.2(2) . ?
C16 C15 H15 118.0(16) . ?
C14 C15 H15 118.6(16) . ?
C17 C16 C15 118.1(2) . ?
C17 C16 C20 121.2(3) . ?
C15 C16 C20 120.7(3) . ?
C16 C17 C18 122.3(2) . ?
C16 C17 H17 120.1(17) . ?
C18 C17 H17 117.5(17) . ?
C13 C18 C17 117.5(2) . ?
C13 C18 C21 119.49(19) . ?
C17 C18 C21 122.9(2) . ?
C14 C19 H19A 108.4(18) . ?
C14 C19 H19B 118.9(19) . ?
H19A C19 H19B 101(3) . ?
C14 C19 H19C 111(2) . ?
H19A C19 H19C 119(3) . ?
H19B C19 H19C 99(3) . ?
C16 C20 H20A 109(3) . ?
C16 C20 H20B 110(2) . ?
H20A C20 H20B 106(3) . ?
C16 C20 H20C 113(2) . ?
H20A C20 H20C 108(3) . ?
H20B C20 H20C 110(3) . ?
C18 C21 Ru1 86.08(15) . ?
C18 C21 H21A 119.9(13) . ?
Ru1 C21 H21A 118.2(13) . ?
C18 C21 H21B 112.9(19) . ?
Ru1 C21 H21B 116(2) . ?
H21A C21 H21B 104(2) . ?
C23 C22 Ru1 70.58(13) . ?
C23 C22 H22A 116.7(15) . ?
Ru1 C22 H22A 112.9(14) . ?
C23 C22 H22B 121.8(16) . ?
Ru1 C22 H22B 116.4(15) . ?
H22A C22 H22B 112(2) . ?
C22 C23 Ru1 70.20(13) . ?
C22 C23 H23A 120.7(16) . ?
Ru1 C23 H23A 117.0(15) . ?
C22 C23 H23B 120.0(13) . ?
Ru1 C23 H23B 112.3(12) . ?
H23A C23 H23B 111(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 C1 1.935(2) . yes
Ru1 C21 2.065(3) . yes
Ru1 C22 2.086(2) . yes
Ru1 C23 2.091(2) . yes
Ru1 Cl1 2.4671(6) . yes
Ru1 Cl1 2.5289(5) 2_666 yes
Cl1 Ru1 2.5290(5) 2_666 yes
N1 C1 1.369(2) . ?
N1 C4 1.432(3) . ?
N1 C2 1.471(3) . ?
N2 C1 1.361(3) . ?
N2 C13 1.432(3) . ?
N2 C3 1.470(3) . ?
C2 C3 1.506(4) . ?
C2 H2A 0.88(3) . ?
C2 H2B 0.94(4) . ?
C3 H3A 0.88(3) . ?
C3 H3B 1.02(3) . ?
C4 C5 1.398(3) . ?
C4 C9 1.411(3) . ?
C5 C6 1.380(3) . ?
C5 C10 1.513(3) . ?
C6 C7 1.396(3) . ?
C6 H6 0.82(2) . ?
C7 C8 1.379(3) . ?
C7 C11 1.499(4) . ?
C8 C9 1.383(3) . ?
C8 H8 0.85(2) . ?
C9 C12 1.500(4) . ?
C10 H10A 0.93(3) . ?
C10 H10B 0.91(3) . ?
C10 H10C 0.99(3) . ?
C11 H11A 0.91(3) . ?
C11 H11B 0.99(3) . ?
C11 H11C 0.89(3) . ?
C12 H12A 0.96(3) . ?
C12 H12B 0.90(2) . ?
C12 H12C 0.89(3) . ?
C13 C14 1.400(3) . ?
C13 C18 1.403(3) . ?
C14 C15 1.392(3) . ?
C14 C19 1.487(4) . ?
C15 C16 1.383(4) . ?
C15 H15 0.86(3) . ?
C16 C17 1.368(3) . ?
C16 C20 1.514(3) . ?
C17 C18 1.406(3) . ?
C17 H17 0.84(2) . ?
C18 C21 1.485(3) . ?
C19 H19A 0.98(3) . ?
C19 H19B 0.96(4) . ?
C19 H19C 1.00(4) . ?
C20 H20A 0.89(4) . ?
C20 H20B 0.89(4) . ?
C20 H20C 1.03(4) . ?
C21 H21A 1.07(3) . ?
C21 H21B 0.88(3) . ?
C22 C23 1.402(4) . ?
C22 H22A 0.99(2) . ?
C22 H22B 0.99(3) . ?
C23 H23A 1.00(3) . ?
C23 H23B 0.94(2) . ?
