#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/04/7010432.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_7010432
loop_
_publ_author_name
'Agustín Caballero'
'Felipe Gómezde la Torre'
'Félix A. Jalón'
'Blanca R. Manzano'
'Ana M. Rodríguez'
'Swiatoslaw Trofimenko'
'Michael P. Sigalas'
_publ_section_title
;
 Synthesis and characterisation of a series of ruthenium scorpionate
 complexes with B--HM agostic interactions. Crystal structure of
 [RuH(κ2-N,BH TpTn)(PMe3)(cod)]
 (TpTn = hydrotris[3-(2-thienyl)pyrazol-1-yl]borate)
;
_journal_issue                   4
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              427
_journal_page_last               433
_journal_paper_doi               10.1039/b008986i
_journal_year                    2001
_chemical_formula_sum            'C32 H38 B N6 P Ru S3'
_chemical_formula_weight         745.71
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.020(5)
_cell_angle_beta                 105.600(5)
_cell_angle_gamma                94.070(5)
_cell_formula_units_Z            2
_cell_length_a                   10.682(5)
_cell_length_b                   11.427(5)
_cell_length_c                   14.375(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     1667.4(12)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XRAY80 (Stewart, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       'ω/2\2q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0882
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8005
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         2.12
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         8005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[σ²(Fo²)+(0.0624P)²+0.0000P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1503
_reflns_number_gt                5254
_reflns_number_total             8005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008986i.txt
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010432
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 0.75950(4) -0.85606(4) 0.71042(3) 0.02460(12) Uani 1 1 d . . .
HA H 0.766(4) -0.949(4) 0.758(3) 0.019(12) Uiso 1 1 d . . .
HB H 0.760(5) -0.689(4) 0.669(4) 0.027(13) Uiso 1 1 d . . .
P1 P 0.82047(13) -0.77484(12) 0.87477(9) 0.0276(3) Uani 1 1 d . . .
S2 S 0.53681(14) -1.04310(14) 0.81303(14) 0.0479(4) Uani 1 1 d . . .
S4 S 0.62512(17) -0.39428(16) 0.98032(12) 0.0504(4) Uani 1 1 d . . .
S3 S 0.9239(11) -0.5281(9) 0.3831(7) 0.067(3) Uani 0.50 1 d P A 1
S3A S 0.9237(10) -0.5761(9) 0.3602(6) 0.062(2) Uani 0.50 1 d P A 2
N21 N 0.5641(4) -0.8193(3) 0.6961(3) 0.0247(8) Uani 1 1 d . . .
N22 N 0.5504(4) -0.7100(3) 0.6648(3) 0.0262(9) Uani 1 1 d . . .
N31 N 0.6431(4) -0.6417(4) 0.5353(3) 0.0258(9) Uani 1 1 d . . .
N32 N 0.7411(4) -0.6037(4) 0.4977(3) 0.0292(9) Uani 1 1 d . . .
N41 N 0.6982(4) -0.5208(4) 0.7017(3) 0.0268(9) Uani 1 1 d . . .
N42 N 0.6728(4) -0.4961(4) 0.7893(3) 0.0266(9) Uani 1 1 d . . .
B1 B 0.6665(5) -0.6451(5) 0.6436(4) 0.0281(12) Uani 1 1 d . . .
C1 C 0.9385(5) -0.9448(5) 0.7223(4) 0.0323(12) Uani 1 1 d . . .
H1 H 0.9407 -0.9458 0.7873 0.039 Uiso 1 1 calc . . .
C2 C 0.9560(5) -0.8355(5) 0.6921(4) 0.0350(12) Uani 1 1 d . . .
H2 H 0.9735 -0.7685 0.7392 0.042 Uiso 1 1 calc . . .
C3 C 0.9488(5) -0.8174(5) 0.5901(4) 0.0394(13) Uani 1 1 d . . .
H3A H 1.0291 -0.8382 0.5762 0.047 Uiso 1 1 calc . . .
H3B H 0.9438 -0.7338 0.5853 0.047 Uiso 1 1 calc . . .
C4 C 0.8337(6) -0.8887(5) 0.5124(4) 0.0386(13) Uani 1 1 d . . .
H4A H 0.8121 -0.8470 0.4562 0.046 Uiso 1 1 calc . . .
H4B H 0.8601 -0.9647 0.4915 0.046 Uiso 1 1 calc . . .
C5 C 0.7131(5) -0.9100(4) 0.5459(4) 0.0284(11) Uani 1 1 d . . .
H5 H 0.6533 -0.8542 0.5375 0.034 Uiso 1 1 calc . . .
C6 C 0.6862(5) -1.0069(4) 0.5880(4) 0.0289(11) Uani 1 1 d . . .
H6 H 0.6100 -1.0119 0.6075 0.035 Uiso 1 1 calc . . .
C7 C 0.7718(5) -1.1049(5) 0.6044(4) 0.0385(13) Uani 1 1 d . . .
H7A H 0.7650 -1.1513 0.5417 0.046 Uiso 1 1 calc . . .
H7B H 0.7390 -1.1566 0.6433 0.046 Uiso 1 1 calc . . .
C8 C 0.9157(5) -1.0644(5) 0.6552(4) 0.0360(12) Uani 1 1 d . . .
H8A H 0.9617 -1.0579 0.6060 0.043 Uiso 1 1 calc . . .
H8B H 0.9526 -1.1242 0.6936 0.043 Uiso 1 1 calc . . .
C9 C 0.8888(6) -0.8741(5) 0.9612(4) 0.0411(13) Uani 1 1 d . . .
H9A H 0.8303 -0.9456 0.9488 0.062 Uiso 1 1 calc . . .
H9B H 0.8999 -0.8357 1.0266 0.062 Uiso 1 1 calc . . .
H9C H 0.9719 -0.8931 0.9537 0.062 Uiso 1 1 calc . . .
C10 C 0.6893(6) -0.7258(5) 0.9222(4) 0.0383(13) Uani 1 1 d . . .
H10A H 0.6184 -0.7881 0.9054 0.057 Uiso 1 1 calc . . .
H10B H 0.6591 -0.6571 0.8944 0.057 Uiso 1 1 calc . . .
H10C H 0.7206 -0.7060 0.9920 0.057 Uiso 1 1 calc . . .
C11 C 0.9427(6) -0.6469(5) 0.9134(4) 0.0411(14) Uani 1 1 d . . .
H11A H 1.0178 -0.6642 0.8917 0.062 Uiso 1 1 calc . . .
H11B H 0.9681 -0.6288 0.9834 0.062 Uiso 1 1 calc . . .
H11C H 0.9070 -0.5801 0.8856 0.062 Uiso 1 1 calc . . .
C21 C 0.4281(5) -0.6821(5) 0.6575(4) 0.0308(11) Uani 1 1 d . . .
H21 H 0.3951 -0.6132 0.6378 0.037 Uiso 1 1 calc . . .
C22 C 0.3612(5) -0.7716(5) 0.6838(4) 0.0306(11) Uani 1 1 d . . .
H22 H 0.2747 -0.7755 0.6858 0.037 Uiso 1 1 calc . . .
C23 C 0.4485(5) -0.8583(5) 0.7079(3) 0.0274(10) Uani 1 1 d . . .
C24 C 0.4201(5) -0.9666(5) 0.7447(4) 0.0305(11) Uani 1 1 d . . .
C25 C 0.2989(5) -1.0165(5) 0.7396(4) 0.0373(13) Uani 1 1 d . . .
H25 H 0.2225 -0.9885 0.7060 0.045 Uiso 1 1 calc . . .
C26 C 0.3000(6) -1.1151(5) 0.7902(5) 0.0432(15) Uani 1 1 d . . .
H26 H 0.2243 -1.1582 0.7932 0.052 Uiso 1 1 calc . . .
C27 C 0.4204(6) -1.1405(5) 0.8334(5) 0.0445(15) Uani 1 1 d . . .
H27 H 0.4386 -1.2025 0.8696 0.053 Uiso 1 1 calc . . .
C31 C 0.5303(4) -0.6678(5) 0.4628(4) 0.0299(11) Uani 1 1 d . . .
H31 H 0.4499 -0.6932 0.4711 0.036 Uiso 1 1 calc . . .
C32 C 0.5514(5) -0.6514(6) 0.3769(4) 0.0400(14) Uani 1 1 d . . .
H32 H 0.4915 -0.6640 0.3153 0.048 Uiso 1 1 calc . . .
C33 C 0.6860(5) -0.6105(4) 0.4023(4) 0.0263(10) Uani 1 1 d . A .
C34 C 0.7591(5) -0.5736(4) 0.3360(4) 0.0277(11) Uani 1 1 d . . .
C35 C 0.7081(5) -0.5552(4) 0.2381(4) 0.0287(11) Uani 1 1 d . A .
H35 H 0.6202 -0.5670 0.2031 0.034 Uiso 1 1 calc . . .
C36 C 0.8117(6) -0.5159(6) 0.2014(4) 0.0474(15) Uani 1 1 d . . .
H36 H 0.8012 -0.5091 0.1360 0.057 Uiso 1 1 calc . B 1
C37 C 0.932(2) -0.4882(15) 0.2738(18) 0.042(5) Uani 0.50 1 d P A 1
H37 H 1.0068 -0.4524 0.2635 0.050 Uiso 0.50 1 calc P C 1
C37A C 0.926(3) -0.5374(17) 0.2487(18) 0.051(5) Uani 0.50 1 d P A 2
H37A H 0.9991 -0.5327 0.2259 0.061 Uiso 0.50 1 calc P D 2
C41 C 0.7659(5) -0.4255(5) 0.6845(4) 0.0355(12) Uani 1 1 d . . .
H41 H 0.7947 -0.4217 0.6293 0.043 Uiso 1 1 calc . . .
C42 C 0.7856(5) -0.3355(5) 0.7603(4) 0.0388(13) Uani 1 1 d . . .
H42 H 0.8296 -0.2603 0.7678 0.047 Uiso 1 1 calc . . .
C43 C 0.7244(5) -0.3824(5) 0.8243(4) 0.0309(11) Uani 1 1 d . . .
C44 C 0.7090(5) -0.3230(5) 0.9141(4) 0.0333(12) Uani 1 1 d . . .
C45 C 0.7508(5) -0.2062(5) 0.9607(4) 0.0328(12) Uani 1 1 d . . .
H45 H 0.7972 -0.1506 0.9369 0.039 Uiso 1 1 calc . . .
C46 C 0.7156(7) -0.1835(6) 1.0446(6) 0.062(2) Uani 1 1 d . . .
H46 H 0.7368 -0.1102 1.0843 0.075 Uiso 1 1 calc . . .
C47 C 0.6488(7) -0.2738(7) 1.0652(4) 0.0577(19) Uani 1 1 d . . .
H47 H 0.6185 -0.2710 1.1203 0.069 Uiso 1 1 calc . . .
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'
P P 0.1023 0.0942 '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
N21 Ru1 C2 157.24(19) . . ?
N21 Ru1 C1 164.15(17) . . ?
C2 Ru1 C1 36.9(2) . . ?
N21 Ru1 C6 89.33(17) . . ?
C2 Ru1 C6 94.49(19) . . ?
C1 Ru1 C6 79.64(19) . . ?
N21 Ru1 C5 90.78(16) . . ?
C2 Ru1 C5 79.75(19) . . ?
C1 Ru1 C5 86.79(18) . . ?
C6 Ru1 C5 35.41(18) . . ?
N21 Ru1 P1 90.84(11) . . ?
C2 Ru1 P1 95.76(14) . . ?
C1 Ru1 P1 93.83(14) . . ?
C6 Ru1 P1 152.82(14) . . ?
C5 Ru1 P1 171.64(14) . . ?
C11 P1 C10 102.8(3) . . ?
C11 P1 C9 101.8(3) . . ?
C10 P1 C9 100.6(3) . . ?
C11 P1 Ru1 117.57(19) . . ?
C10 P1 Ru1 115.55(19) . . ?
C9 P1 Ru1 116.1(2) . . ?
C27 S2 C24 92.4(3) . . ?
C47 S4 C44 92.1(3) . . ?
C37 S3 C34 91.0(10) . . ?
C34 S3A C37A 92.8(10) . . ?
C23 N21 N22 106.9(4) . . ?
C23 N21 Ru1 145.0(4) . . ?
N22 N21 Ru1 108.0(3) . . ?
C21 N22 N21 109.6(4) . . ?
C21 N22 B1 131.8(4) . . ?
N21 N22 B1 118.6(4) . . ?
C31 N31 N32 109.4(4) . . ?
C31 N31 B1 128.8(4) . . ?
N32 N31 B1 121.7(4) . . ?
C33 N32 N31 105.4(4) . . ?
N42 N41 C41 109.6(4) . . ?
N42 N41 B1 121.4(4) . . ?
C41 N41 B1 128.5(4) . . ?
C43 N42 N41 105.7(4) . . ?
N31 B1 N22 111.5(4) . . ?
N31 B1 N41 111.4(4) . . ?
N22 B1 N41 110.3(4) . . ?
C2 C1 C8 124.2(5) . . ?
C2 C1 Ru1 70.8(3) . . ?
C8 C1 Ru1 113.3(3) . . ?
C1 C2 C3 125.0(5) . . ?
C1 C2 Ru1 72.3(3) . . ?
C3 C2 Ru1 110.1(3) . . ?
C2 C3 C4 114.8(5) . . ?
C5 C4 C3 114.1(4) . . ?
C6 C5 C4 124.0(5) . . ?
C6 C5 Ru1 70.7(3) . . ?
C4 C5 Ru1 110.5(3) . . ?
C5 C6 C7 124.1(5) . . ?
C5 C6 Ru1 73.9(3) . . ?
C7 C6 Ru1 109.9(3) . . ?
C6 C7 C8 114.9(5) . . ?
C7 C8 C1 113.4(4) . . ?
N22 C21 C22 108.4(4) . . ?
C21 C22 C23 106.8(4) . . ?
N21 C23 C22 108.2(4) . . ?
N21 C23 C24 125.9(5) . . ?
C22 C23 C24 125.7(4) . . ?
C25 C24 C23 125.4(5) . . ?
C25 C24 S2 109.7(4) . . ?
C23 C24 S2 124.6(4) . . ?
C24 C25 C26 113.5(5) . . ?
C27 C26 C25 113.5(5) . . ?
C26 C27 S2 110.8(4) . . ?
N31 C31 C32 110.0(4) . . ?
C31 C32 C33 103.7(4) . . ?
N32 C33 C32 111.4(4) . . ?
N32 C33 C34 122.1(4) . . ?
C32 C33 C34 126.4(5) . . ?
C35 C34 C33 127.6(4) . . ?
C35 C34 S3A 108.9(5) . . ?
C33 C34 S3A 122.4(5) . . ?
C35 C34 S3 113.5(5) . . ?
C33 C34 S3 118.4(5) . . ?
S3A C34 S3 20.3(4) . . ?
C36 C35 C34 109.5(5) . . ?
C37A C36 C37 26.1(11) . . ?
C37A C36 C35 115.3(12) . . ?
C37 C36 C35 113.1(11) . . ?
C36 C37 S3 112.2(16) . . ?
C36 C37A S3A 110.6(16) . . ?
N41 C41 C42 109.8(5) . . ?
C41 C42 C43 104.1(5) . . ?
N42 C43 C42 110.9(5) . . ?
N42 C43 C44 121.3(5) . . ?
C42 C43 C44 127.7(5) . . ?
C45 C44 C43 130.1(5) . . ?
C45 C44 S4 109.0(4) . . ?
C43 C44 S4 120.8(4) . . ?
C46 C45 C44 112.2(5) . . ?
C47 C46 C45 114.6(6) . . ?
C46 C47 S4 112.0(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 N21 2.119(4) . ?
Ru1 C2 2.184(5) . ?
Ru1 C1 2.204(5) . ?
Ru1 C6 2.237(5) . ?
Ru1 C5 2.278(5) . ?
Ru1 P1 2.3276(15) . ?
P1 C11 1.814(5) . ?
P1 C10 1.810(6) . ?
P1 C9 1.827(6) . ?
S2 C27 1.718(5) . ?
S2 C24 1.729(5) . ?
S4 C47 1.680(7) . ?
S4 C44 1.708(6) . ?
S3 C37 1.71(3) . ?
S3 C34 1.723(12) . ?
S3A C34 1.701(11) . ?
S3A C37A 1.72(3) . ?
N21 C23 1.345(6) . ?
N21 N22 1.383(5) . ?
N22 C21 1.347(6) . ?
N22 B1 1.519(7) . ?
N31 C31 1.350(6) . ?
N31 N32 1.369(5) . ?
N31 B1 1.515(7) . ?
N32 C33 1.329(6) . ?
N41 N42 1.360(5) . ?
N41 C41 1.348(7) . ?
N41 B1 1.522(7) . ?
N42 C43 1.354(6) . ?
C1 C2 1.388(8) . ?
C1 C8 1.536(7) . ?
C2 C3 1.489(8) . ?
C3 C4 1.523(8) . ?
C4 C5 1.506(7) . ?
C5 C6 1.374(7) . ?
C6 C7 1.496(7) . ?
C7 C8 1.524(7) . ?
C21 C22 1.355(7) . ?
C22 C23 1.419(7) . ?
C23 C24 1.447(7) . ?
C24 C25 1.356(7) . ?
C25 C26 1.413(8) . ?
C26 C27 1.339(8) . ?
C31 C32 1.346(7) . ?
C32 C33 1.414(7) . ?
C33 C34 1.466(7) . ?
C34 C35 1.414(7) . ?
C35 C36 1.416(8) . ?
C36 C37A 1.28(3) . ?
C36 C37 1.40(2) . ?
C41 C42 1.365(7) . ?
C42 C43 1.397(8) . ?
C43 C44 1.439(7) . ?
C44 C45 1.402(7) . ?
C45 C46 1.357(9) . ?
C46 C47 1.322(10) . ?
