Unusual Reactivity of the Bis(pyrazolyl)borate Chelate: B−H for B−X (X = F, Cl, OH) Substitution in Complexes of Ruthenium
Page, Michael J.; Messerle, Barbara A.; Wagler, Jörg; Organometallics 28 (2009) 6145–; doi:10.1021/om900660k

data_4070218
_publ_section_title
;
 Unusual Reactivity of the Bis(pyrazolyl)borate Chelate: B&#x2212;H for
 B&#x2212;X (X = F, Cl, OH) Substitution in Complexes of Ruthenium
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6145
_journal_paper_doi               10.1021/om900660k
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C33 H32 B2 N10 O P Ru, C F3 O3 S'
_chemical_formula_sum            'C34 H32 B2 F3 N10 O4 P Ru S'
_chemical_formula_weight         887.42
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.7270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.35060(10)
_cell_length_b                   22.9442(3)
_cell_length_c                   15.5326(2)
_cell_measurement_reflns_used    52239
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      2.546
_cell_volume                     3807.76(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius Collect, KappaCCD'
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP32 for windows (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa 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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            58514
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         9147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+1.7112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                7205
_reflns_number_total             9147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900660k_si_002.cif
_cod_data_source_block           compd_9
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4070218