Catalytic Alkenylation of Phenylpyridines with Terminal Alkynes by a [12]Metallacrown-6 Ruthenium(II) Compound
Ming-Hua Xie; Miao Wang; Chuan-De Wu; Inorganic Chemistry 48 (2009) 10477–10479; doi:10.1021/ic901309b

data_4303587
_publ_section_title
;
Catalytic Alkenylation of Phenylpyridines with Terminal Alkynes by a
[12]Metallacrown-6 Ruthenium(II) Compound
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10477
_journal_page_last               10479
_journal_paper_doi               10.1021/ic901309b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C12 H36 S12 Zn6'
_chemical_formula_weight         957.35
_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                 94.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.030(2)
_cell_length_b                   13.156(3)
_cell_length_c                   12.529(3)
_cell_measurement_reflns_used    15652
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      3.10
_cell_volume                     1647.4(6)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens XPREP'
_computing_molecular_graphics    'Siemens SHELX-97'
_computing_publication_material  'Siemens SHELX-97'
_computing_structure_refinement  'Siemens SHELX-97'
_computing_structure_solution    'Siemens SHELX-97'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15652
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.063
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Bloc
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.039
_refine_diff_density_max         1.721
_refine_diff_density_min         -1.560
_refine_diff_density_rms         0.280
_refine_ls_extinction_coef       0.0036(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0763
_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^)+(0.1563P)^2^+14.1200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2358
_refine_ls_wR_factor_ref         0.2752
_reflns_number_gt                2618
_reflns_number_total             3740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901309b_si_002_2.cif
_cod_data_source_block           ZnRing
_cod_original_cell_volume        1647.5(6)
_cod_database_code               4303587