#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:00:57 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178764 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/18/4101887.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_4101887
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            'C22 H28 B Cl N2 Ru'
_chemical_formula_weight         467.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.424(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9877(8)
_cell_length_b                   13.6367(13)
_cell_length_c                   17.3641(16)
_cell_measurement_reflns_used    6393
_cell_measurement_temperature    144(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.77
_cell_volume                     2070.0(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      144(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12497
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  0.9938
_exptl_absorpt_correction_T_min  0.6600
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0322
_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)+(0.0424P)²+0.0518P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0800
_reflns_number_gt                3834
_reflns_number_total             4645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909858a_si_003.cif
_cod_data_source_block           Williams4
_cod_database_code               4101887
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.59555(2) 0.397373(13) 0.177091(11) 0.02036(8) Uani 1 1 d . . .
B1 B 0.9390(3) 0.4488(2) 0.30716(17) 0.0257(6) Uani 1 1 d . . .
Cl1 Cl 0.45216(7) 0.54567(4) 0.13402(4) 0.02989(15) Uani 1 1 d . . .
N1 N 0.7862(2) 0.47574(14) 0.16004(12) 0.0218(4) Uani 1 1 d . . .
N2 N 0.6423(2) 0.46323(14) 0.29058(12) 0.0230(4) Uani 1 1 d . . .
C1 C 0.7720(3) 0.51231(18) 0.08633(15) 0.0261(5) Uani 1 1 d . . .
H1 H 0.6748 0.5090 0.0503 0.031 Uiso 1 1 calc R . .
C2 C 0.8910(3) 0.5540(2) 0.06103(16) 0.0327(6) Uani 1 1 d . . .
H2 H 0.8772 0.5788 0.0087 0.039 Uiso 1 1 calc R . .
C3 C 1.0319(3) 0.5588(2) 0.11407(18) 0.0381(7) Uani 1 1 d . . .
H3 H 1.1179 0.5859 0.0986 0.046 Uiso 1 1 calc R . .
C4 C 1.0452(3) 0.52394(19) 0.18943(16) 0.0307(6) Uani 1 1 d . . .
H4 H 1.1417 0.5282 0.2260 0.037 Uiso 1 1 calc R . .
C5 C 0.9213(3) 0.48189(17) 0.21493(15) 0.0239(5) Uani 1 1 d . . .
C6 C 0.9605(3) 0.3295(2) 0.32366(16) 0.0325(6) Uani 1 1 d . . .
H6A H 1.0229 0.3019 0.2896 0.049 Uiso 1 1 calc R . .
H6B H 0.8599 0.2977 0.3119 0.049 Uiso 1 1 calc R . .
H6C H 1.0113 0.3182 0.3793 0.049 Uiso 1 1 calc R . .
C7 C 1.0928(3) 0.4997(2) 0.36113(16) 0.0375(7) Uani 1 1 d . . .
H7A H 1.1833 0.4727 0.3463 0.056 Uiso 1 1 calc R . .
H7B H 1.0988 0.4861 0.4172 0.056 Uiso 1 1 calc R . .
H7C H 1.0887 0.5707 0.3523 0.056 Uiso 1 1 calc R . .
C8 C 0.7846(3) 0.48563(17) 0.33429(14) 0.0235(5) Uani 1 1 d . . .
C9 C 0.7942(3) 0.53850(19) 0.40443(15) 0.0300(6) Uani 1 1 d . . .
H9 H 0.8922 0.5575 0.4346 0.036 Uiso 1 1 calc R . .
C10 C 0.6667(3) 0.5640(2) 0.43141(15) 0.0315(6) Uani 1 1 d . . .
H10 H 0.6763 0.5995 0.4794 0.038 Uiso 1 1 calc R . .
C11 C 0.5246(3) 0.53654(19) 0.38685(15) 0.0299(6) Uani 1 1 d . . .
H11 H 0.4343 0.5511 0.4042 0.036 Uiso 1 1 calc R . .
C12 C 0.5171(3) 0.48788(18) 0.31705(15) 0.0271(6) Uani 1 1 d . . .
H12 H 0.4193 0.4706 0.2857 0.033 Uiso 1 1 calc R . .
C13 C 0.6378(3) 0.28406(17) 0.09124(15) 0.0273(6) Uani 1 1 d . . .
C14 C 0.6925(3) 0.25107(17) 0.17048(15) 0.0262(5) Uani 1 1 d . . .
H14 H 0.8049 0.2410 0.1913 0.031 Uiso 1 1 calc R . .
C15 C 0.5954(3) 0.24844(17) 0.22354(15) 0.0264(5) Uani 1 1 d . . .
H15 H 0.6405 0.2363 0.2810 0.032 Uiso 1 1 calc R . .
C16 C 0.4389(3) 0.27746(18) 0.19892(17) 0.0295(6) Uani 1 1 d . . .
C17 C 0.3891(3) 0.31393(18) 0.12281(16) 0.0306(6) Uani 1 1 d . . .
H17 H 0.2888 0.3492 0.1087 0.037 Uiso 1 1 calc R . .
C18 C 0.4871(3) 0.31735(18) 0.06851(15) 0.0295(6) Uani 1 1 d . . .
H18 H 0.4533 0.3543 0.0177 0.035 Uiso 1 1 calc R . .
C19 C 0.7355(3) 0.2844(2) 0.03034(16) 0.0342(6) Uani 1 1 d . . .
H19 H 0.7125 0.3460 -0.0015 0.041 Uiso 1 1 calc R . .
C20 C 0.6850(4) 0.1974(2) -0.02558(18) 0.0473(8) Uani 1 1 d . . .
H20A H 0.7064 0.1360 0.0042 0.071 Uiso 1 1 calc R . .
H20B H 0.7412 0.1984 -0.0676 0.071 Uiso 1 1 calc R . .
H20C H 0.5750 0.2023 -0.0491 0.071 Uiso 1 1 calc R . .
C21 C 0.9086(3) 0.2806(2) 0.06529(17) 0.0391(7) Uani 1 1 d . . .
H21A H 0.9352 0.2184 0.0934 0.059 Uiso 1 1 calc R . .
H21B H 0.9386 0.3352 0.1023 0.059 Uiso 1 1 calc R . .
H21C H 0.9627 0.2858 0.0225 0.059 Uiso 1 1 calc R . .
C22 C 0.3331(3) 0.2685(2) 0.25484(19) 0.0428(7) Uani 1 1 d . . .
H22A H 0.2471 0.3140 0.2384 0.064 Uiso 1 1 calc R . .
H22B H 0.3894 0.2847 0.3088 0.064 Uiso 1 1 calc R . .
H22C H 0.2944 0.2012 0.2536 0.064 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'
B B 0.0013 0.0007 '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'
N N 0.0061 0.0033 '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
N1 Ru1 N2 85.60(8) . . ?
N1 Ru1 C15 126.59(8) . . ?
N2 Ru1 C15 93.88(9) . . ?
N1 Ru1 C14 96.24(8) . . ?
N2 Ru1 C14 116.09(9) . . ?
C15 Ru1 C14 37.57(9) . . ?
N1 Ru1 C17 147.19(9) . . ?
N2 Ru1 C17 125.81(9) . . ?
C15 Ru1 C17 66.65(10) . . ?
C14 Ru1 C17 79.18(9) . . ?
N1 Ru1 C18 110.21(9) . . ?
N2 Ru1 C18 163.86(9) . . ?
C15 Ru1 C18 79.47(10) . . ?
C14 Ru1 C18 66.79(10) . . ?
C17 Ru1 C18 38.05(9) . . ?
N1 Ru1 C13 89.27(8) . . ?
N2 Ru1 C13 152.19(9) . . ?
C15 Ru1 C13 67.62(9) . . ?
C14 Ru1 C13 37.43(9) . . ?
C17 Ru1 C13 67.27(10) . . ?
C18 Ru1 C13 36.63(9) . . ?
N1 Ru1 C16 163.51(8) . . ?
N2 Ru1 C16 98.54(9) . . ?
C15 Ru1 C16 37.54(9) . . ?
C14 Ru1 C16 67.57(9) . . ?
C17 Ru1 C16 36.34(10) . . ?
C18 Ru1 C16 67.25(10) . . ?
C13 Ru1 C16 79.62(9) . . ?
N1 Ru1 Cl1 85.67(5) . . ?
N2 Ru1 Cl1 84.81(5) . . ?
C15 Ru1 Cl1 147.59(7) . . ?
C14 Ru1 Cl1 159.09(7) . . ?
C17 Ru1 Cl1 87.94(7) . . ?
C18 Ru1 Cl1 92.95(7) . . ?
C13 Ru1 Cl1 122.07(7) . . ?
C16 Ru1 Cl1 110.53(7) . . ?
C7 B1 C5 108.8(2) . . ?
C7 B1 C8 111.4(2) . . ?
C5 B1 C8 107.5(2) . . ?
C7 B1 C6 105.6(2) . . ?
C5 B1 C6 114.9(2) . . ?
C8 B1 C6 108.8(2) . . ?
C1 N1 C5 120.9(2) . . ?
C1 N1 Ru1 114.89(16) . . ?
C5 N1 Ru1 123.89(16) . . ?
C12 N2 C8 120.2(2) . . ?
C12 N2 Ru1 114.88(16) . . ?
C8 N2 Ru1 124.88(15) . . ?
N1 C1 C2 123.2(2) . . ?
C1 C2 C3 117.9(2) . . ?
C4 C3 C2 118.8(2) . . ?
C3 C4 C5 122.7(3) . . ?
N1 C5 C4 116.5(2) . . ?
N1 C5 B1 122.5(2) . . ?
C4 C5 B1 121.0(2) . . ?
N2 C8 C9 117.4(2) . . ?
N2 C8 B1 121.2(2) . . ?
C9 C8 B1 121.4(2) . . ?
C10 C9 C8 122.5(3) . . ?
C9 C10 C11 118.3(2) . . ?
C12 C11 C10 118.4(2) . . ?
N2 C12 C11 123.2(2) . . ?
C18 C13 C14 118.1(2) . . ?
C18 C13 C19 118.7(2) . . ?
C14 C13 C19 123.2(2) . . ?
C18 C13 Ru1 70.15(14) . . ?
C14 C13 Ru1 69.41(14) . . ?
C19 C13 Ru1 132.38(17) . . ?
C15 C14 C13 120.9(2) . . ?
C15 C14 Ru1 71.01(13) . . ?
C13 C14 Ru1 73.16(14) . . ?
C14 C15 C16 120.9(2) . . ?
C14 C15 Ru1 71.43(13) . . ?
C16 C15 Ru1 73.56(14) . . ?
C17 C16 C15 117.6(2) . . ?
C17 C16 C22 121.9(2) . . ?
C15 C16 C22 120.5(3) . . ?
C17 C16 Ru1 69.78(14) . . ?
C15 C16 Ru1 68.90(14) . . ?
C22 C16 Ru1 132.71(19) . . ?
C16 C17 C18 121.8(2) . . ?
C16 C17 Ru1 73.88(15) . . ?
C18 C17 Ru1 71.20(14) . . ?
C13 C18 C17 120.5(2) . . ?
C13 C18 Ru1 73.22(14) . . ?
C17 C18 Ru1 70.74(14) . . ?
C13 C19 C21 114.9(2) . . ?
C13 C19 C20 107.7(2) . . ?
C21 C19 C20 110.4(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 N1 2.0982(19) . ?
Ru1 N2 2.117(2) . ?
Ru1 C15 2.185(2) . ?
Ru1 C14 2.191(2) . ?
Ru1 C17 2.194(2) . ?
Ru1 C18 2.200(2) . ?
Ru1 C13 2.240(2) . ?
Ru1 C16 2.247(2) . ?
Ru1 Cl1 2.4212(6) . ?
B1 C7 1.634(4) . ?
B1 C5 1.636(4) . ?
B1 C8 1.644(4) . ?
B1 C6 1.656(4) . ?
N1 C1 1.352(3) . ?
N1 C5 1.361(3) . ?
N2 C12 1.353(3) . ?
N2 C8 1.362(3) . ?
C1 C2 1.370(3) . ?
C2 C3 1.384(4) . ?
C3 C4 1.371(4) . ?
C4 C5 1.412(3) . ?
C8 C9 1.401(3) . ?
C9 C10 1.379(4) . ?
C10 C11 1.383(4) . ?
C11 C12 1.370(4) . ?
C13 C18 1.396(3) . ?
C13 C14 1.422(3) . ?
C13 C19 1.523(3) . ?
C14 C15 1.409(3) . ?
C15 C16 1.427(3) . ?
C16 C17 1.386(4) . ?
C16 C22 1.513(3) . ?
C17 C18 1.433(3) . ?
C19 C21 1.534(4) . ?
C19 C20 1.533(4) . ?
