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_4341522
_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, 2(C3 H6 O)'
_chemical_formula_sum            'C46 H36 N14 Ni O2'
_chemical_formula_weight         875.60
_chemical_name_systematic
;
 ? 
;
_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     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                100.8347(18)
_cell_angle_beta                 98.0479(18)
_cell_angle_gamma                91.2391(18)
_cell_formula_units_Z            2
_cell_length_a                   9.8514(2)
_cell_length_b                   13.9696(3)
_cell_length_c                   16.7096(4)
_cell_measurement_reflns_used    15532
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.3710
_cell_measurement_theta_min      3.4450
_cell_volume                     2233.62(9)
_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 0.9984
_diffrn_measured_fraction_theta_max 0.8773
_diffrn_measurement_details
;
  1 omega   34.00   76.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -       18.0909 -178.0000 -180.0000 42

  2 omega   68.00   95.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -       18.0909 -178.0000  -90.0000 27

  3 omega  -54.00   41.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -37.0000  150.0000 95

  4 omega    5.00   84.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -       18.0909   37.0000  -30.0000 79

  5 omega  -19.00   59.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -99.0000   60.0000 78

  6 omega    5.00   49.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -       18.0909   57.0000  -60.0000 44

  7 omega  -17.00   15.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -      -18.4034  -84.0000  -74.0000 32

  8 omega  -85.00  -57.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -      -18.4034  142.0000  109.6333 28

  9 omega   34.00   95.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -       18.0909 -178.0000   30.0000 61

 10 omega   -3.00   87.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -       18.0909   57.0000   60.0000 90

 11 omega   -3.00   87.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -       18.0909   57.0000 -120.0000 90

 12 omega   34.00   95.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -       18.0909 -178.0000  120.0000 61

 13 omega  -20.00   43.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -99.0000 -120.0000 63

 14 omega   -8.00    3.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -       18.0909   37.0000 -180.0000 11
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0267048000
_diffrn_orient_matrix_UB_12      0.0321284000
_diffrn_orient_matrix_UB_13      0.0373105000
_diffrn_orient_matrix_UB_21      0.0675803000
_diffrn_orient_matrix_UB_22      -0.0072885000
_diffrn_orient_matrix_UB_23      -0.0092216000
_diffrn_orient_matrix_UB_31      -0.0045003000
_diffrn_orient_matrix_UB_32      0.0399202000
_diffrn_orient_matrix_UB_33      -0.0207814000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35371
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.834
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.5976
_exptl_crystal_size_mid          0.3608
_exptl_crystal_size_min          0.1433
_refine_diff_density_max         1.821
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         10555
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0663
_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^)+(0.1102P)^2^+4.2694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1963
_refine_ls_wR_factor_ref         0.2108
_reflns_number_gt                8534
_reflns_number_total             10555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500657e_si_002.cif
_cod_data_source_block           NiCNCN_10_2acetone
_cod_original_cell_volume        2233.64(8)
_cod_database_code               4341522
_chemical_oxdiff_formula         'Ni (C20 N7 H12)2 (C3 H6 O)2'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Sof: O1S(0.5) C1S(0.5) C2S(0.5) H2Sa(0.5) H2Sb(0.5) H2Sc(0.5) C3S(0.5)
 H3Sa(0.5) H3Sb(0.5) H3Sc(0.5) O1Q(0.5) C1Q(0.5) C2Q(0.5) H2Qa(0.5) H2Qb(0.5)
 H2Qc(0.5) C3Q(0.5) H3Qa(0.5) H3Qb(0.5) H3Qc(0.5) O2S(0.5) C4S(0.5) C5S(0.5)
 H5Sa(0.5) H5Sb(0.5) H5Sc(0.5) C6S(0.5) H6Sa(0.5) H6Sb(0.5) H6Sc(0.5) O2Q(0.5)
 C4Q(0.5) C5Q(0.5) H5Qa(0.5) H5Qb(0.5) H5Qc(0.5) C6Q(0.5) H6Qa(0.5) H6Qb(0.5)
 H6Qc(0.5)
 Fixed Uiso: H11(0.036) H12(0.04) H13(0.038) H3(0.033) H5(0.036) H6(0.035)
 H21(0.041) H22(0.046) H23(0.045) H33(0.039) H35(0.036) H36(0.032) H41(0.039)
 H42(0.049) H43(0.045) H53(0.039) H55(0.053) H56(0.048) H61(0.031) H62(0.036)
 H63(0.035) H73(0.04) H75(0.048) H76(0.043) H2Sa(0.099) H2Sb(0.099) H2Sc(0.099)
 H3Sa(0.158) H3Sb(0.158) H3Sc(0.158) H2Qa(0.158) H2Qb(0.158) H2Qc(0.158)
 H3Qa(0.099) H3Qb(0.099) H3Qc(0.099) H5Sa(0.167) H5Sb(0.167) H5Sc(0.167)
 H6Sa(0.172) H6Sb(0.172) H6Sc(0.172) H5Qa(0.32) H5Qb(0.32) H5Qc(0.32)
 H6Qa(0.256) H6Qb(0.256) H6Qc(0.256)
 Fixed X: H11(0.4834) H12(0.3255) H13(0.4243) H3(0.6572) H5(0.8716) H6(0.8333)
 H21(0.9712) H22(1.1353) H23(1.0366) H33(0.8158) H35(0.54) H36(0.5666)
 H41(1.0027) H42(1.2041) H43(1.1295) H53(0.9409) H55(0.6612) H56(0.627)
 H61(0.438) H62(0.2541) H63(0.3495) H73(0.5409) H75(0.823) H76(0.847)
 H2Sa(0.1265) H2Sb(0.1018) H2Sc(0.1725) H3Sa(0.364) H3Sb(0.2999) H3Sc(0.4512)
 H2Qa(0.3693) H2Qb(0.3769) H2Qc(0.4254) H3Qa(0.0616) H3Qb(0.2033) H3Qc(0.1795)
 H5Sa(0.3746) H5Sb(0.4477) H5Sc(0.3061) H6Sa(0.4208) H6Sb(0.4316) H6Sc(0.3081)
 H5Qa(0.0304) H5Qb(0.1148) H5Qc(-0.0096) H6Qa(0.3355) H6Qb(0.3103) H6Qc(0.3652)
 Fixed Y: H11(0.8814) H12(0.8322) H13(0.6847) H3(0.6461) H5(0.4125) H6(0.448)
 H21(0.8295) H22(0.7228) H23(0.5514) H33(0.4702) H35(0.3191) H36(0.4379)
 H41(0.6508) H42(0.7517) H43(0.9229) H53(1.0081) H55(1.1737) H56(1.0576)
 H61(0.6145) H62(0.6548) H63(0.797) H73(0.8455) H75(1.0706) H76(1.0332)
 H2Sa(0.2271) H2Sb(0.1111) H2Sc(0.1709) H3Sa(0.0464) H3Sb(0.0046) H3Sc(0.0554)
 H2Qa(0.0279) H2Qb(0.144) H2Qc(0.0761) H3Qa(0.1501) H3Qb(0.1692) H3Qc(0.2217)
 H5Sa(0.4369) H5Sb(0.5007) H5Sc(0.5332) H6Sa(0.4077) H6Sb(0.3254) H6Sc(0.3191)
 H5Qa(0.2318) H5Qb(0.2361) H5Qc(0.3062) H6Qa(0.3911) H6Qb(0.275) H6Qc(0.3341)
 Fixed Z: H11(0.1859) H12(0.052) H13(-0.026) H3(-0.0637) H5(-0.0167)
 H6(0.1183) H21(0.4032) H22(0.4698) H23(0.4203) H33(0.4207) H35(0.2342)
 H36(0.1573) H41(0.186) H42(0.1659) H43(0.1803) H53(0.1227) H55(0.2324)
 H56(0.3095) H61(0.2302) H62(0.3195) H63(0.4297) H73(0.5259) H75(0.5593)
 H76(0.4228) H2Sa(0.0674) H2Sb(0.0409) H2Sc(-0.0164) H3Sa(-0.0007) H3Sb(0.0694)
 H3Sc(0.0889) H2Qa(0.1246) H2Qb(0.1333) H2Qc(0.0552) H3Qa(-0.0007) H3Qb(-0.033)
 H3Qc(0.0573) H5Sa(0.3564) H5Sb(0.442) H5Sc(0.3978) H6Sa(0.5519) H6Sb(0.4726)
 H6Sc(0.5246) H5Qa(0.3505) H5Qb(0.276) H5Qc(0.29) H6Qa(0.331) H6Qb(0.3149)
 H6Qc(0.4058)
;