#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:00:57 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178764 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/18/4101886.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_4101886
loop_
_publ_author_name
'Brian L. Conley'
'Travis J. Williams'
_publ_contact_author_address
;
Loker Hydrocarbon Research Institute and Department of Chemistry, 
University of Southern California, Los Angeles, CA 90089-1661
;
_publ_contact_author_email       travisw@usc.edu
_publ_contact_author_name        'Travis J. Williams'
_publ_section_title
;
 Thermochemistry and Molecular Structure of a Remarkable Agostic
 Interaction in a Heterobifunctional Ruthenium-Boron Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1764
_journal_page_last               1765
_journal_paper_doi               10.1021/ja909858a
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C18 H20 B F3 N5 O6 Ru S'
_chemical_formula_weight         603.33
_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                 110.535(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.644(8)
_cell_length_b                   8.032(3)
_cell_length_c                   29.052(9)
_cell_measurement_reflns_used    5811
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      1.50
_cell_volume                     5167(3)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0871
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            15109
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.9288
_exptl_absorpt_correction_T_min  0.7147
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing,R.H.,Acta Crystallogr.1995,A51,33'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_meas      calculated
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0695P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1421
_reflns_number_gt                3618
_reflns_number_total             5811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909858a_si_002.cif
_cod_data_source_block           Williams1
_cod_database_code               4101886
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 0.321528(17) 0.58057(5) 0.894718(13) 0.03448(14) Uani 1 1 d . . .
B1 B 0.3623(3) 0.4406(7) 0.8225(2) 0.0408(14) Uani 1 1 d . . .
N1 N 0.26151(17) 0.5016(5) 0.82863(13) 0.0353(9) Uani 1 1 d . . .
N2 N 0.35930(17) 0.3491(5) 0.90343(14) 0.0377(9) Uani 1 1 d . . .
N3 N 0.38710(18) 0.6474(5) 0.95887(15) 0.0383(9) Uani 1 1 d . . .
N4 N 0.28275(18) 0.8102(5) 0.87965(13) 0.0371(9) Uani 1 1 d . . .
N5 N 0.26855(18) 0.5359(5) 0.93385(15) 0.0395(10) Uani 1 1 d . . .
O1 O 0.37467(14) 0.6074(4) 0.85052(11) 0.0376(8) Uani 1 1 d . . .
C1 C 0.2012(2) 0.5082(6) 0.81392(18) 0.0415(12) Uani 1 1 d . . .
H1 H 0.1831 0.5561 0.8353 0.050 Uiso 1 1 calc R . .
C2 C 0.1647(2) 0.4486(7) 0.76932(19) 0.0495(14) Uani 1 1 d . . .
H2 H 0.1220 0.4545 0.7598 0.059 Uiso 1 1 calc R . .
C3 C 0.1914(3) 0.3795(7) 0.7384(2) 0.0543(15) Uani 1 1 d . . .
H3 H 0.1672 0.3355 0.7074 0.065 Uiso 1 1 calc R . .
C4 C 0.2533(3) 0.3754(6) 0.75317(18) 0.0476(14) Uani 1 1 d . . .
H4 H 0.2719 0.3278 0.7321 0.057 Uiso 1 1 calc R . .
C5 C 0.2888(2) 0.4393(6) 0.79819(17) 0.0406(12) Uani 1 1 d . . .
C6 C 0.3977(3) 0.4219(8) 0.7843(2) 0.0592(15) Uani 1 1 d . . .
H6A H 0.3880 0.5168 0.7617 0.089 Uiso 1 1 calc R . .
H6B H 0.3853 0.3184 0.7656 0.089 Uiso 1 1 calc R . .
H6C H 0.4413 0.4191 0.8025 0.089 Uiso 1 1 calc R . .
C7 C 0.3761(2) 0.2992(6) 0.86524(18) 0.0403(12) Uani 1 1 d . . .
C8 C 0.4014(2) 0.1429(7) 0.86658(19) 0.0444(13) Uani 1 1 d . . .
H8 H 0.4129 0.1076 0.8399 0.053 Uiso 1 1 calc R . .
C9 C 0.4100(2) 0.0386(7) 0.9057(2) 0.0524(15) Uani 1 1 d . . .
H9 H 0.4264 -0.0696 0.9060 0.063 Uiso 1 1 calc R . .
C10 C 0.3944(2) 0.0930(7) 0.9453(2) 0.0519(14) Uani 1 1 d . . .
H10 H 0.4009 0.0241 0.9732 0.062 Uiso 1 1 calc R . .
C11 C 0.3693(2) 0.2485(6) 0.94282(19) 0.0436(12) Uani 1 1 d . . .
H11 H 0.3586 0.2866 0.9697 0.052 Uiso 1 1 calc R . .
C12 C 0.4230(2) 0.6691(6) 0.9959(2) 0.0452(13) Uani 1 1 d . . .
C13 C 0.4698(3) 0.6966(8) 1.0438(2) 0.081(2) Uani 1 1 d . . .
H13A H 0.4547 0.7741 1.0629 0.121 Uiso 1 1 calc R . .
H13B H 0.5057 0.7438 1.0393 0.121 Uiso 1 1 calc R . .
H13C H 0.4802 0.5904 1.0614 0.121 Uiso 1 1 calc R . .
C14 C 0.2572(2) 0.9320(7) 0.86914(18) 0.0422(12) Uani 1 1 d . . .
C15 C 0.2251(3) 1.0893(7) 0.8557(2) 0.0643(17) Uani 1 1 d . . .
H15A H 0.1911 1.0909 0.8675 0.096 Uiso 1 1 calc R . .
H15B H 0.2101 1.1016 0.8199 0.096 Uiso 1 1 calc R . .
H15C H 0.2527 1.1813 0.8707 0.096 Uiso 1 1 calc R . .
C16 C 0.2411(3) 0.5201(7) 0.9585(2) 0.0516(14) Uani 1 1 d . . .
C17 C 0.2059(3) 0.5027(10) 0.9912(2) 0.090(2) Uani 1 1 d . . .
H17A H 0.2282 0.4326 1.0194 0.135 Uiso 1 1 calc R . .
H17B H 0.1669 0.4510 0.9732 0.135 Uiso 1 1 calc R . .
H17C H 0.1993 0.6128 1.0030 0.135 Uiso 1 1 calc R . .
C18 C 0.4543(5) 0.2256(18) 0.1549(4) 0.126(4) Uani 1 1 d . . .
F1 F 0.4525(3) 0.3771(14) 0.1736(2) 0.202(4) Uani 1 1 d . . .
F2 F 0.5055(3) 0.1584(11) 0.1812(2) 0.195(4) Uani 1 1 d . . .
F3 F 0.4081(3) 0.1627(14) 0.1618(3) 0.225(4) Uani 1 1 d . . .
S1 S 0.44625(7) 0.2433(2) 0.09237(7) 0.0693(5) Uani 1 1 d . . .
O2 O 0.3911(2) 0.3322(7) 0.06986(19) 0.0993(17) Uani 1 1 d . . .
O3 O 0.4430(3) 0.0769(8) 0.0763(3) 0.145(3) Uani 1 1 d . . .
O4 O 0.49975(19) 0.3286(6) 0.09429(17) 0.0787(13) Uani 1 1 d . . .
O5 O 0.3417(6) 0.6398(18) 0.0736(5) 0.301(7) Uani 1 1 d . . .
O6 O 0.4135(12) 0.841(7) 0.1496(9) 0.78(4) Uani 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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 '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'
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
N5 Ru1 N3 87.39(16) . . ?
N5 Ru1 N4 87.70(16) . . ?
N3 Ru1 N4 95.68(15) . . ?
N5 Ru1 N2 95.77(16) . . ?
N3 Ru1 N2 88.11(15) . . ?
N4 Ru1 N2 174.98(15) . . ?
N5 Ru1 N1 96.39(16) . . ?
N3 Ru1 N1 174.75(16) . . ?
N4 Ru1 N1 88.13(15) . . ?
N2 Ru1 N1 87.89(15) . . ?
N5 Ru1 O1 174.98(15) . . ?
N3 Ru1 O1 96.09(14) . . ?
N4 Ru1 O1 95.54(14) . . ?
N2 Ru1 O1 80.76(14) . . ?
N1 Ru1 O1 79.91(14) . . ?
O1 B1 C6 113.3(4) . . ?
O1 B1 C7 104.6(4) . . ?
C6 B1 C7 116.4(4) . . ?
O1 B1 C5 102.1(4) . . ?
C6 B1 C5 115.7(4) . . ?
C7 B1 C5 102.9(4) . . ?
C1 N1 C5 120.2(4) . . ?
C1 N1 Ru1 126.7(3) . . ?
C5 N1 Ru1 113.1(3) . . ?
C11 N2 C7 119.9(4) . . ?
C11 N2 Ru1 126.0(3) . . ?
C7 N2 Ru1 114.0(3) . . ?
C12 N3 Ru1 173.3(4) . . ?
C14 N4 Ru1 174.8(4) . . ?
C16 N5 Ru1 174.6(4) . . ?
B1 O1 Ru1 101.0(3) . . ?
N1 C1 C2 122.4(5) . . ?
C1 C2 C3 118.4(5) . . ?
C4 C3 C2 119.1(5) . . ?
C3 C4 C5 120.9(5) . . ?
N1 C5 C4 118.9(5) . . ?
N1 C5 B1 113.2(4) . . ?
C4 C5 B1 127.8(5) . . ?
N2 C7 C8 119.3(5) . . ?
N2 C7 B1 112.2(4) . . ?
C8 C7 B1 128.5(5) . . ?
C9 C8 C7 121.0(5) . . ?
C8 C9 C10 119.1(5) . . ?
C11 C10 C9 118.5(5) . . ?
N2 C11 C10 122.1(5) . . ?
N3 C12 C13 179.8(7) . . ?
N4 C14 C15 179.3(6) . . ?
N5 C16 C17 178.8(6) . . ?
F3 C18 F2 114.4(10) . . ?
F3 C18 F1 98.2(11) . . ?
F2 C18 F1 107.1(11) . . ?
F3 C18 S1 113.7(9) . . ?
F2 C18 S1 112.4(9) . . ?
F1 C18 S1 109.8(9) . . ?
O3 S1 O4 114.5(4) . . ?
O3 S1 O2 112.8(4) . . ?
O4 S1 O2 115.7(3) . . ?
O3 S1 C18 103.7(6) . . ?
O4 S1 C18 103.0(4) . . ?
O2 S1 C18 105.3(5) . . ?
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 N5 1.997(4) . ?
Ru1 N3 2.034(4) . ?
Ru1 N4 2.038(4) . ?
Ru1 N2 2.040(4) . ?
Ru1 N1 2.047(4) . ?
Ru1 O1 2.099(3) . ?
B1 O1 1.542(6) . ?
B1 C6 1.614(7) . ?
B1 C7 1.630(8) . ?
B1 C5 1.630(8) . ?
N1 C1 1.339(6) . ?
N1 C5 1.360(6) . ?
N2 C11 1.352(6) . ?
N2 C7 1.363(6) . ?
N3 C12 1.126(6) . ?
N4 C14 1.134(6) . ?
N5 C16 1.129(6) . ?
C1 C2 1.367(7) . ?
C2 C3 1.381(8) . ?
C3 C4 1.374(8) . ?
C4 C5 1.382(7) . ?
C7 C8 1.385(7) . ?
C8 C9 1.370(7) . ?
C9 C10 1.394(8) . ?
C10 C11 1.374(7) . ?
C12 C13 1.459(7) . ?
C14 C15 1.455(7) . ?
C16 C17 1.474(8) . ?
C18 F3 1.284(10) . ?
C18 F2 1.300(12) . ?
C18 F1 1.339(14) . ?
C18 S1 1.765(11) . ?
S1 O3 1.409(6) . ?
S1 O4 1.422(4) . ?
S1 O2 1.428(5) . ?
