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_4072095
_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_sum            'C38.5 H33 Cl2 N Ni P2'
_chemical_formula_weight         701.21
_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                 115.807(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.647(2)
_cell_length_b                   17.098(3)
_cell_length_c                   15.666(3)
_cell_measurement_reflns_used    1705
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18.442
_cell_measurement_theta_min      2.612
_cell_volume                     3532.0(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0905
_diffrn_reflns_av_sigmaI/netI    0.1491
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17296
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.8870
_exptl_absorpt_correction_T_min  0.8341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6140
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1607
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0236P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                2420
_reflns_number_total             6140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800580p_si_003.cif
_cod_data_source_block           070323f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3532.1(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C38.50 H33 Cl2 N Ni P2'
_cod_database_code               4072095