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_4032689
_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, C3 H6 O, C24 H20 B'
_chemical_formula_sum            'C38 H38 B Cl N6 Ni O'
_chemical_formula_weight         699.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 109.158(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0883(12)
_cell_length_b                   12.3222(8)
_cell_length_c                   18.5299(15)
_cell_measurement_reflns_used    1881
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.492
_cell_measurement_theta_min      2.272
_cell_volume                     3470.0(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1099
_diffrn_reflns_av_unetI/netI     0.1223
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23797
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.628
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1184 before and 0.0785 after correction.
The Ratio of minimum to maximum transmission is 0.8131.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.094
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         6092
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0290P)^2^+2.3197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1313
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3657
_reflns_number_total             6092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            J-Org-Chem-2017-845-63-70-2.cif
_cod_data_source_block           2
_cod_database_code               4032689
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 O1AC, C1AC, C2AC, C3AC
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: O1AC(0.7) C3AC(0.7) H3AA(0.7) H3AB(0.7) H3AC(0.7) C1(0.3) H1B(0.3)
 H1D(0.3) H1E(0.3) O2(0.3)
4.a Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1C(H1C), C2A(H2AA), C2B(H2BA), C2C(H2C), C3A(H3A), C3B(H3B),
 C3C(H3C), C12B(H12B), C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B),
 C22B(H22B), C23B(H23B), C24B(H24B), C25B(H25B), C26B(H26B), C32B(H32B),
 C33B(H33B), C34B(H34B), C35B(H35B), C36B(H36B), C42B(H42B), C43B(H43B),
 C44B(H44B), C45B(H45B), C46B(H46B)
4.c Idealised Me refined as rotating group:
 C1AC(H1AA,H1AB,H1AC), C3AC(H3AA,H3AB,H3AC), C1(H1B,H1D,H1E)
;
_shelx_res_checksum              59806
_shelx_hkl_checksum              70984
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'