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)
Agustín Caballero; Felipe Gómezde la Torre; Félix A. Jalón; Blanca R. Manzano; Ana M. Rodríguez; Swiatoslaw Trofimenko; Michael P. Sigalas; J. Chem. Soc., Dalton Trans.  (2001) 427–433; doi:10.1039/b008986i

data_7010432
_publ_section_title
;
 Synthesis and characterisation of a series of ruthenium scorpionate
 complexes with B--HM agostic interactions. Crystal structure of
 [RuH(\k2-N,BH TpTn)(PMe3)(cod)]
 (TpTn&#x00A0;=&#x00A0;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       '\w/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/[\s^2^(Fo^2^)+(0.0624P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/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