Bioinspired Catalytic Conjugate Additions of Thiophenols to α,β-Enones by a Disubstituted Benzoate-Bridged Nickel Mimic for the Active Site of Urease
Lee, Way-Zen; Tseng, Huan-Sheng; Wang, Tzu-Li; Tsai, Hui-Lien; Kuo, Ting-Shen; Organometallics 29 (2010) 2874–; doi:10.1021/om100103u

data_4065731
_publ_contact_author             'Way-Zen Lee'
_publ_section_title
;
 Bioinspired Catalytic Conjugate Additions of Thiophenols to \a,\b-Enones
 by a Disubstituted Benzoate-Bridged Nickel Mimic for the Active Site of
 Urease
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2874
_journal_paper_doi               10.1021/om100103u
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C116 H123 Cl4 N17 Ni4 O30'
_chemical_formula_sum            'C116 H123 Cl4 N17 Ni4 O30'
_chemical_formula_weight         2611.95
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 96.57
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.8448(2)
_cell_length_b                   20.2926(2)
_cell_length_c                   24.8296(2)
_cell_measurement_reflns_used    129248
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     11935.47(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            96235
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.9564
_exptl_absorpt_correction_T_min  0.7109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5432
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.758
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1431
_refine_ls_number_reflns         21656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.758
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1503P)^2^+49.9280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.1962
_reflns_number_gt                15895
_reflns_number_total             21656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100103u_si_004.cif
_cod_data_source_block           737502
_cod_original_cell_volume        11935.50(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4065731