Functionalized N-Heterocyclic Carbene Nonspectator Ligands upon Internal Alkyne Activation Reactions
Francys E. Fernández; María del Carmen Puerta; Pedro Valerga; Inorganic Chemistry 52 (2013) 6502–6509; doi:10.1021/ic400433z

data_4335077
_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) 012798'
_publ_section_title
;
 Functionalized N-Heterocyclic Carbene Nonspectator Ligands upon Internal
 Alkyne Activation Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6502
_journal_page_last               6509
_journal_paper_doi               10.1021/ic400433z
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C32 H12 B F24, C30 H28 B F3 N9 O2 Ru'
_chemical_formula_sum            'C62 H40 B2 F27 N9 O2 Ru'
_chemical_formula_weight         1578.72
_chemical_name_systematic
;
{Hydrotris(pyrazolyl)borate-\k^3^ <i>N</i>,<i>N</i>',<i>N</i>''}-
{1-(4-trifluoromethylphenyl)-2-(1-methyl-1H-imidazol-2-yl)-3-pyridyl-prop-1-
ylidene-2-carboxylic acid methyl ester-\k^3^ <i>C</i>,<i>N</i>,<i>N</i>'}
-ruthenium(II)  <i>tetrakis</i>{3,5-<i>bis</i>(trifluoromethyl)phenyl}borate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.955(3)
_cell_length_b                   20.205(4)
_cell_length_c                   37.714(8)
_cell_measurement_reflns_used    6900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.671
_cell_measurement_theta_min      2.286
_cell_volume                     12920(4)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0831
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            72446
_diffrn_reflns_theta_full        24.07
_diffrn_reflns_theta_max         24.07
_diffrn_reflns_theta_min         2.09
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0027
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       prism
_exptl_crystal_F_000             6304
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         10172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0797
_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^)+(0.0156P)^2^+89.1424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1406
_reflns_number_gt                9401
_reflns_number_total             10172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400433z_si_002_3.cif
_cod_data_source_block           pv1222
_cod_database_code               4335077