Picolyl-NHC Hydrotris(pyrazolyl)borate Ruthenium(II) Complexes: Synthesis, Characterization, and Reactivity with Small Molecules
Francys E. Fernández; M. Carmen Puerta; Pedro Valerga; Inorganic Chemistry 52 (2013) 4396–4410; doi:10.1021/ic302553z

data_4334463
_publ_contact_author_address
;
Departamento de CMIM y Qu\'imica Inorg\'anica
Universidad de C\'adiz
Facultad de Ciencias
Campus Universitario del R\'io San Pedro
11510. Puerto Real. SPAIN.
;
_publ_contact_author_email       pedro.valerga@uca.es
_publ_contact_author_fax         '34 (956) 016288'
_publ_contact_author_name        'Pedro Valerga'
_publ_contact_author_phone       '34 (956) 016340'
_publ_section_title
;
 Picolyl-NHC Hydrotris(pyrazolyl)borate Ruthenium(II) Complexes:
 Synthesis, Characterization, and Reactivity with Small Molecules
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4396
_journal_page_last               4410
_journal_paper_doi               10.1021/ic302553z
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C21 H25 B Cl N9 Ru, 0.35(Ag Br)'
_chemical_formula_sum            'C21 H25 Ag0.35 B Br0.35 Cl N9 Ru'
_chemical_formula_weight         616.36
_chemical_name_systematic
;(chlorido)-{\k^2^  C,N-3-isopropyl-1-(pyrid-2-ylmethyl)-2,3-dihydro-
imidazole-2-ylidene}-{\k^3^ N,N',N''-tris(pirazolyl)borate}-ruthenium(II)
0.35 silver bromide
;
_space_group_IT_number           161
_symmetry_cell_setting           rhombohedral
_symmetry_Int_Tables_number      161
_symmetry_space_group_name_Hall  'P 3* -2n'
_symmetry_space_group_name_H-M   'R 3 c :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.046(17)
_cell_angle_beta                 97.046(17)
_cell_angle_gamma                97.046(17)
_cell_formula_units_Z            6
_cell_length_a                   16.0514(19)
_cell_length_b                   16.0514(19)
_cell_length_c                   16.0514(19)
_cell_measurement_reflns_used    9784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.020
_cell_measurement_theta_min      2.580
_cell_volume                     4033.4(9)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-3 vers. 1.08 (Farrugia, 2005)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '1700 omega scan frames, 0.3 deg, 10 sec'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25515
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         1.69
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0083
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.474
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       prism
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.013
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4740
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+2.4161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                4661
_reflns_number_total             4740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302553z_si_002_1.cif
_cod_data_source_block           pv1216
_cod_original_cell_volume        4033.4(8)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4334463