Synthesis and catalytic activity of nickel(II) complexes containing NCN pincer ligands
Ashwin G. Nair; Roy T. McBurney; Mark R.D. Gatus; D.Barney Walker; Mohan Bhadbhade; Barbara A. Messerle; Journal of Organometallic Chemistry 845 (2017) 63–70; doi:10.1016/j.jorganchem.2017.02.025

data_4032690
_publ_section_title
;
 Synthesis and catalytic activity of nickel(II) complexes containing NCN
 pincer ligands
;
_journal_name_full               'Journal of Organometallic Chemistry'
_journal_page_first              63
_journal_page_last               70
_journal_paper_doi               10.1016/j.jorganchem.2017.02.025
_journal_volume                  845
_journal_year                    2017
_chemical_formula_moiety         'C11 H12 Cl N6 Ni, F6 P'
_chemical_formula_sum            'C11 H12 Cl F6 N6 Ni P'
_chemical_formula_weight         467.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                91.69(3)
_cell_angle_beta                 104.13(3)
_cell_angle_gamma                104.66(3)
_cell_formula_units_Z            2
_cell_length_a                   7.9770(16)
_cell_length_b                   8.7170(17)
_cell_length_c                   12.200(2)
_cell_measurement_reflns_used    4992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      2.5
_cell_measurement_theta_min      22.5
_cell_volume                     792.1(3)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16062
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.056
_diffrn_reflns_theta_min         1.729
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.570
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_description       plate
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.9530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3991
_reflns_number_total             4211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            J-Org-Chem-2017-845-63-70-3.cif
_cod_data_source_block           3
_cod_database_code               4032690
_shelx_res_checksum              20177
_shelx_hkl_checksum              10201
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id Ni_2a
_olex2_submission_special_instructions 'No special instructions were received'