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_4079954
_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         'C19 H35 Cl N Ni P2, C H2 CL2, Cl'
_chemical_formula_sum            'C20 H37 Cl4 N Ni P2'
_chemical_formula_weight         553.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 108.2250(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.85360(10)
_cell_length_b                   11.12400(10)
_cell_length_c                   16.0637(2)
_cell_measurement_reflns_used    6494
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     2690.81(5)
_computing_cell_refinement       HKL
_computing_data_collection       HKL
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altmore et al, 1994)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'omega and phi scan'
_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  0.1382
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49975
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_T_max  0.9404
_exptl_absorpt_correction_T_min  0.7888
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
;
Cylinder (Maslen, 1992)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         12180
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0283P)^2^+2.9684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                10753
_reflns_number_total             12180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3010838_si_002.cif
_cod_data_source_block           m1305_complex_3
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2690.81(4)
_cod_original_sg_symbol_Hall     P2yb
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4079954