Synthesis and Characterization of Amido Pincer Complexes of Lithium and Nickel and Catalysis of the Nickel Complexes in the Kumada Cross-Coupling
Sun, Kai; Wang, Li; Wang, Zhong-Xia; Organometallics 27 (2008) 5649–; doi:10.1021/om800580p

data_4072093
_publ_section_title
;
 Synthesis and Characterization of Amido Pincer Complexes of Lithium and
 Nickel and Catalysis of the Nickel Complexes in the Kumada Cross-Coupling
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5649
_journal_paper_doi               10.1021/om800580p
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C25 H20 N P'
_chemical_formula_sum            'C25 H20 N P'
_chemical_formula_weight         365.39
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 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                 98.395(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.108(3)
_cell_length_b                   13.258(3)
_cell_length_c                   20.346(4)
_cell_measurement_reflns_used    4383
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.4
_cell_volume                     4031.7(14)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30031
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  0.9744
_exptl_absorpt_correction_T_min  0.9661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.28(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         11604
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1658
_reflns_number_gt                5411
_reflns_number_total             11604
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800580p_si_001.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        4031.6(15)
_cod_database_code               4072093