Anionic Nickel(II) Complexes with Doubly Deprotonated PNP Pincer-Type Ligands and Their Reactivity toward CO2
Vogt, Matthias; Rivada-Wheelaghan, Orestes; Iron, Mark A.; Leitus, Gregory; Diskin-Posner, Yael; Shimon, Linda J. W.; Ben-David, Yehoshoa; Milstein, David; Organometallics 32 (2013) 300–; doi:10.1021/om3010838

data_4079956
_publ_section_title
;
 Anionic Nickel(II) Complexes with Doubly Deprotonated PNP Pincer-Type
 Ligands and Their Reactivity toward CO2
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              300
_journal_paper_doi               10.1021/om3010838
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C20 H36 N Ni P2, C12 H30 Li O6'
_chemical_formula_sum            'C32 H66 Li N Ni O6 P2'
_chemical_formula_weight         688.45
_chemical_name_systematic
; 
 ? 
;
_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                 103.460(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1865(7)
_cell_length_b                   16.1597(13)
_cell_length_c                   21.9789(16)
_cell_measurement_reflns_used    48057
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.58
_cell_volume                     3864.0(5)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker Apex2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker KappaApex2 CCD'
_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  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            48057
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.9755
_exptl_absorpt_correction_T_min  0.8548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         8861
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0325P)^2^+1.1218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                6392
_reflns_number_total             8861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3010838_si_002.cif
_cod_data_source_block           m1318_complex_9
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4079956