#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:51:58 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178758 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/12/4101288.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_4101288
loop_
_publ_author_name
'Feng, Yuee'
'Lail, Marty'
'Foley, Nicholas A'
'Gunnoe, T Brent'
'Barakat, Khaldoon A'
'Cundari, Thomas R'
'Petersen, Jeffrey L'
_publ_section_title
;
 Hydrogen-deuterium exchange between TpRu(PMe3)(L)X (L = PMe3 and X =
 OH, OPh, Me, Ph, or NHPh; L = NCMe and X = Ph) and deuterated arene
 solvents: evidence for metal-mediated processes.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7982
_journal_page_last               7994
_journal_paper_doi               10.1021/ja0615775
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C21 H33 B N6 O P2 Ru'
_chemical_formula_weight         559.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0881(15)
_cell_length_b                   12.9815(12)
_cell_length_c                   12.2632(11)
_cell_measurement_temperature    295(2)
_cell_volume                     2561.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17304
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         3054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0278P)²+1.2325P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                2606
_reflns_number_total             3054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0615775si20060307_085253.cif
_cod_data_source_block           compound_5
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4101288
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Ru1 Ru 0.346610(12) 0.2500 0.627240(16) 0.03214(8) Uani 1 2 d S
P1 P 0.28289(4) 0.11054(5) 0.54746(4) 0.04680(14) Uani 1 1 d .
O1 O 0.45069(12) 0.2500 0.52364(15) 0.0469(5) Uani 1 2 d S
N1 N 0.25660(14) 0.2500 0.74775(17) 0.0372(5) Uani 1 2 d S
N2 N 0.28054(15) 0.2500 0.85393(17) 0.0396(5) Uani 1 2 d S
N3 N 0.41675(10) 0.14304(13) 0.72373(13) 0.0401(4) Uani 1 1 d .
N4 N 0.41544(10) 0.15512(14) 0.83415(14) 0.0433(4) Uani 1 1 d .
C1 C 0.17320(18) 0.2500 0.7491(2) 0.0461(7) Uani 1 2 d S
H1 H 0.1398 0.2500 0.6872 0.055 Uiso 1 2 calc SR
C2 C 0.14340(18) 0.2500 0.8552(3) 0.0479(7) Uani 1 2 d S
H2 H 0.0882 0.2500 0.8779 0.057 Uiso 1 2 calc SR
C3 C 0.21263(19) 0.2500 0.9186(2) 0.0465(7) Uani 1 2 d S
H3 H 0.2132 0.2500 0.9944 0.056 Uiso 1 2 calc SR
C4 C 0.47036(14) 0.06806(18) 0.7038(2) 0.0548(6) Uani 1 1 d .
H4 H 0.4836 0.0435 0.6347 0.066 Uiso 1 1 calc R
C5 C 0.50410(16) 0.0312(2) 0.8005(3) 0.0687(8) Uani 1 1 d .
H5 H 0.5430 -0.0213 0.8087 0.082 Uiso 1 1 calc R
C6 C 0.46853(14) 0.0876(2) 0.8797(2) 0.0584(6) Uani 1 1 d .
H6 H 0.4789 0.0810 0.9539 0.070 Uiso 1 1 calc R
C7 C 0.45913(18) 0.2500 0.4182(2) 0.0433(6) Uani 1 2 d S
C8 C 0.3943(2) 0.2500 0.3420(3) 0.0518(8) Uani 1 2 d S
H8 H 0.3396 0.2500 0.3667 0.062 Uiso 1 2 calc SR
C9 C 0.4095(2) 0.2500 0.2299(3) 0.0603(9) Uani 1 2 d S
H9 H 0.3648 0.2500 0.1817 0.072 Uiso 1 2 calc SR
C10 C 0.4888(2) 0.2500 0.1892(3) 0.0593(9) Uani 1 2 d S
H10 H 0.4988 0.2500 0.1145 0.071 Uiso 1 2 calc SR
C11 C 0.5532(3) 0.2500 0.2632(3) 0.0773(12) Uani 1 2 d S
H11 H 0.6076 0.2500 0.2376 0.093 Uiso 1 2 calc SR
C12 C 0.5395(2) 0.2500 0.3737(3) 0.0652(10) Uani 1 2 d S
H12 H 0.5849 0.2500 0.4206 0.078 Uiso 1 2 calc SR
C13 C 0.19000(18) 0.1178(3) 0.4621(3) 0.0826(9) Uani 1 1 d .
H13A H 0.1729 0.0495 0.4421 0.124 Uiso 1 1 calc R
H13B H 0.2022 0.1567 0.3974 0.124 Uiso 1 1 calc R
H13C H 0.1461 0.1510 0.5019 0.124 Uiso 1 1 calc R
C14 C 0.34856(18) 0.0274(2) 0.4634(2) 0.0741(8) Uani 1 1 d .
H14A H 0.3926 -0.0006 0.5073 0.111 Uiso 1 1 calc R
H14B H 0.3719 0.0668 0.4047 0.111 Uiso 1 1 calc R
H14C H 0.3157 -0.0279 0.4342 0.111 Uiso 1 1 calc R
C15 C 0.24738(19) 0.0176(2) 0.6498(2) 0.0720(8) Uani 1 1 d .
H15A H 0.2249 -0.0419 0.6139 0.108 Uiso 1 1 calc R
H15B H 0.2052 0.0487 0.6943 0.108 Uiso 1 1 calc R
H15C H 0.2934 -0.0027 0.6947 0.108 Uiso 1 1 calc R
B1 B 0.3731(2) 0.2500 0.8838(3) 0.0460(8) Uani 1 2 d S
H1A H 0.3799 0.2500 0.9632 0.055 Uiso 1 2 calc SR
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'
P P 0.1023 0.0942 '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
N1 Ru1 O1 171.60(8) . .
N1 Ru1 N3 88.52(6) . 7_565
O1 Ru1 N3 85.09(6) . 7_565
N1 Ru1 N3 88.52(6) . .
O1 Ru1 N3 85.09(6) . .
N3 Ru1 N3 80.67(9) 7_565 .
N1 Ru1 P1 89.54(4) . .
O1 Ru1 P1 95.62(4) . .
N3 Ru1 P1 168.24(5) 7_565 .
N3 Ru1 P1 87.69(5) . .
N1 Ru1 P1 89.54(4) . 7_565
O1 Ru1 P1 95.62(4) . 7_565
N3 Ru1 P1 87.69(5) 7_565 7_565
N3 Ru1 P1 168.24(5) . 7_565
P1 Ru1 P1 103.89(3) . 7_565
C13 P1 C14 100.38(14) . .
C13 P1 C15 99.86(14) . .
C14 P1 C15 100.21(15) . .
C13 P1 Ru1 124.61(11) . .
C14 P1 Ru1 116.56(9) . .
C15 P1 Ru1 111.48(9) . .
C7 O1 Ru1 133.19(19) . .
C1 N1 N2 105.8(2) . .
C1 N1 Ru1 135.14(19) . .
N2 N1 Ru1 119.11(17) . .
C3 N2 N1 109.5(2) . .
C3 N2 B1 130.2(2) . .
N1 N2 B1 120.3(2) . .
C4 N3 N4 106.17(17) . .
C4 N3 Ru1 135.80(16) . .
N4 N3 Ru1 117.73(12) . .
C6 N4 N3 109.10(19) . .
C6 N4 B1 129.8(2) . .
N3 N4 B1 119.59(17) . .
N1 C1 C2 111.0(3) . .
C3 C2 C1 104.7(3) . .
N2 C3 C2 109.1(3) . .
N3 C4 C5 110.5(2) . .
C6 C5 C4 105.2(2) . .
C5 C6 N4 109.0(2) . .
O1 C7 C8 125.9(3) . .
O1 C7 C12 118.9(3) . .
C8 C7 C12 115.2(3) . .
C9 C8 C7 121.7(3) . .
C10 C9 C8 121.5(3) . .
C9 C10 C11 117.4(3) . .
C12 C11 C10 122.0(4) . .
C11 C12 C7 122.2(3) . .
N4 B1 N4 106.9(2) . 7_565
N4 B1 N2 109.66(17) . .
N4 B1 N2 109.66(17) 7_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N1 2.069(2) .
Ru1 O1 2.1019(19) .
Ru1 N3 2.1451(16) 7_565
Ru1 N3 2.1451(16) .
Ru1 P1 2.2991(6) .
Ru1 P1 2.2991(6) 7_565
P1 C13 1.827(3) .
P1 C14 1.829(3) .
P1 C15 1.832(3) .
O1 C7 1.300(3) .
N1 C1 1.342(4) .
N1 N2 1.358(3) .
N2 C3 1.350(4) .
N2 B1 1.534(4) .
N3 C4 1.323(3) .
N3 N4 1.363(2) .
N4 C6 1.345(3) .
N4 B1 1.533(3) .
C1 C2 1.386(4) .
C2 C3 1.358(4) .
C4 C5 1.390(4) .
C5 C6 1.344(4) .
C7 C8 1.401(4) .
C7 C12 1.403(4) .
C8 C9 1.397(4) .
C9 C10 1.370(5) .
C10 C11 1.378(5) .
C11 C12 1.373(4) .
B1 N4 1.533(3) 7_565
