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_4334465
_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         'C20 H21 B N9 O Ru, C32 H12 B F24'
_chemical_formula_sum            'C52 H33 B2 F24 N9 O Ru'
_chemical_formula_weight         1378.56
_chemical_name_common
;
Carbonyl-{\k^2^ <i>C</i>,<i>N</i>-3-methyl-1-(pyrid-2-ylmethyl)-
2,3-dihydro-imidazole-2-ylidene}-{\k^3^ <i>N</i>,<i>N</i>',<i>N</i>''-
<i>tris</i>(pirazolyl)borate}- ruthenium(II)
<i>tetrakis</i>{3,5-<i>bis</i>(trifluoromethyl)phenyl}borate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.180(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0569(15)
_cell_length_b                   12.0298(14)
_cell_length_c                   35.729(4)
_cell_measurement_reflns_used    8543
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.117
_cell_measurement_theta_min      2.304
_cell_volume                     5603.4(11)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            37535
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.14
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0252
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.385
_refine_diff_density_min         -1.457
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         9940
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+14.6303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1495
_reflns_number_gt                9038
_reflns_number_total             9940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302553z_si_002_3.cif
_cod_data_source_block           pv1202t
_cod_original_sg_symbol_Hall     'P 2ybc'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4334465