Homoleptic Nickel(II) Complexes of Redox-Tunable Pincer-type Ligands.
Hewage, Jeewantha S.; Wanniarachchi, Sarath; Morin, Tyler J.; Liddle, Brendan J.; Banaszynski, Megan; Lindeman, Sergey V.; Bennett, Brian; Gardinier, James R.; Inorganic chemistry 53 (2014) 10070–10084; doi:10.1021/ic500657e

data_4341523
_publ_section_title
;
 Homoleptic Nickel(II) Complexes of Redox-Tunable Pincer-type Ligands.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10070
_journal_page_last               10084
_journal_paper_doi               10.1021/ic500657e
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C40 H24 N14 Ni, C3 H6 O'
_chemical_formula_sum            'C43 H30 N14 Ni O'
_chemical_formula_weight         817.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-18
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.6602(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.21320(17)
_cell_length_b                   15.60318(16)
_cell_length_c                   17.3945(2)
_cell_measurement_reflns_used    18121
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.8510
_cell_measurement_theta_min      3.3560
_cell_volume                     3748.48(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 16.1500
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.9022
_diffrn_measurement_details
;
  1 omega   54.00   83.00   1.0000   25.7000
omega____ theta____ kappa____ phi______ frames
    -       18.0909 -178.0000 -120.0000 29

  2 omega  -44.00   56.00   1.0000   25.7000
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -19.0000  -90.0000 100

  3 omega   15.00   88.00   1.0000   25.7000
omega____ theta____ kappa____ phi______ frames
    -       18.0909   37.0000   90.0000 73

  4 omega    4.00   30.00   1.0000   25.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.4034   77.0000 -180.0000 26

  5 omega  -47.00  -20.00   1.0000   25.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.4034   77.0000 -180.0000 27

  6 omega   34.00   95.00   1.0000   25.7000
omega____ theta____ kappa____ phi______ frames
    -       18.0909 -178.0000 -180.0000 61

  7 omega  -12.00   88.00   1.0000   25.7000
omega____ theta____ kappa____ phi______ frames
    -       18.0909   77.0000  -90.0000 100

  8 omega   -8.00   91.00   1.0000   25.7000
omega____ theta____ kappa____ phi______ frames
    -       18.0909   37.0000   30.0000 99

  9 omega  -80.00  -27.00   1.0000   25.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.4034  131.0000 -146.3391 53
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0277306000
_diffrn_orient_matrix_UB_12      0.0196603000
_diffrn_orient_matrix_UB_13      0.0240960000
_diffrn_orient_matrix_UB_21      0.0254571000
_diffrn_orient_matrix_UB_22      -0.0241016000
_diffrn_orient_matrix_UB_23      0.0329524000
_diffrn_orient_matrix_UB_31      0.0349651000
_diffrn_orient_matrix_UB_32      0.0331415000
_diffrn_orient_matrix_UB_33      0.0096935000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42291
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.1934
_exptl_crystal_size_mid          0.1583
_exptl_crystal_size_min          0.0894
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         9159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0394P)^2^+6.3322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1201
_reflns_number_gt                7659
_reflns_number_total             9159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500657e_si_002.cif
_cod_data_source_block           NiCNCN_10_1acetone
_cod_original_cell_volume        3748.49(8)
_cod_database_code               4341523
_chemical_oxdiff_formula         'Ni (C20 N7 H12)2 C3 H6 O'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H11(0.029) H12(0.039) H13(0.046) H3(0.044) H5(0.035) H6(0.028)
 H21(0.034) H22(0.039) H23(0.036) H33(0.028) H35(0.03) H36(0.026) H41(0.035)
 H42(0.034) H43(0.029) H53(0.024) H55(0.026) H56(0.026) H61(0.029) H62(0.034)
 H63(0.035) H73(0.037) H75(0.037) H76(0.028) H2Sa(0.156) H2Sb(0.156)
 H2Sc(0.156) H3Sa(0.352) H3Sb(0.352) H3Sc(0.352)
 Fixed X: H11(0.662) H12(0.5913) H13(0.4448) H3(0.3058) H5(0.2127) H6(0.3591)
 H21(0.6096) H22(0.5736) H23(0.552) H33(0.6503) H35(0.5811) H36(0.5151)
 H41(0.363) H42(0.2643) H43(0.3484) H53(0.4012) H55(0.6642) H56(0.7319)
 H61(0.6753) H62(0.8437) H63(0.926) H73(0.951) H75(0.8802) H76(0.7274)
 H2Sa(0.3223) H2Sb(0.3486) H2Sc(0.3949) H3Sa(0.1861) H3Sb(0.1397) H3Sc(0.1243)
 Fixed Y: H11(0.5395) H12(0.6462) H13(0.5764) H3(0.5021) H5(0.2605) H6(0.2079)
 H21(0.2447) H22(0.0885) H23(0.0279) H33(0.0313) H35(0.1094) H36(0.2332)
 H41(0.2623) H42(0.288) H43(0.4054) H53(0.5461) H55(0.6617) H56(0.5458)
 H61(0.3342) H62(0.3827) H63(0.4028) H73(0.3131) H75(0.3438) H76(0.3878)
 H2Sa(0.6168) H2Sb(0.5297) H2Sc(0.6184) H3Sa(0.4952) H3Sb(0.5788) H3Sc(0.5606)
 Fixed Z: H11(0.342) H12(0.4199) H13(0.4486) H3(0.3934) H5(0.4185) H6(0.4051)
 H21(0.1409) H22(0.116) H23(0.2441) H33(0.3796) H35(0.5814) H36(0.5187)
 H41(0.2298) H42(0.0919) H43(0.0363) H53(0.0762) H55(0.1171) H56(0.1916)
 H61(0.491) H62(0.5533) H63(0.4419) H73(0.336) H75(0.0979) H76(0.1037)
 H2Sa(0.1857) H2Sb(0.2346) H2Sc(0.2714) H3Sa(0.2343) H3Sb(0.1868) H3Sc(0.2735)
;