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_4335075
_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, C34 H31 B N9 O Ru, 0.58(C H2 Cl2)'
_chemical_formula_sum            'C66.58 H44.17 B2 Cl1.17 F24 N9 O Ru'
_chemical_formula_weight         1606.30
_chemical_name_systematic
;
(2,3-diphenyl-prop-1-en-3-one-ylidene)-{\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 
0.52 dichloromethane solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                110.90(3)
_cell_angle_beta                 106.52(3)
_cell_angle_gamma                91.96(3)
_cell_formula_units_Z            2
_cell_length_a                   13.444(3)
_cell_length_b                   16.053(3)
_cell_length_c                   18.075(4)
_cell_measurement_reflns_used    5946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.469
_cell_measurement_theta_min      2.200
_cell_volume                     3453.5(17)
_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 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28776
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.20
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0013
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       prism
_exptl_crystal_F_000             1609.0
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.585
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         15300
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0725P)^2^+5.7540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1490
_reflns_number_gt                14172
_reflns_number_total             15300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400433z_si_002_1.cif
_cod_data_source_block           pv1104
_cod_database_code               4335075