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_4341521
_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         '0.5(C40 H30 N12 Ni), 0.65(C H2 Cl2)'
_chemical_formula_sum            'C41.29 H32.59 Cl2.59 N12 Ni'
_chemical_formula_weight         847.49
_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     direct
_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                 102.7148(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.3591(3)
_cell_length_b                   27.8741(5)
_cell_length_c                   17.7477(3)
_cell_measurement_reflns_used    51210
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.7228
_cell_measurement_theta_min      3.4576
_cell_volume                     8377.0(3)
_computing_cell_refinement
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
;
_computing_data_collection
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
;
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
 1 omega -9.00 96.00 1.0000 63.8000
 omega____ theta____ kappa____ phi______ frames
 - 19.7376 77.0000 -180.0000 105
 2 omega -15.00 100.00 1.0000 63.8000
 omega____ theta____ kappa____ phi______ frames
 - 19.7376 22.0000 159.0000 115
 3 omega 6.00 32.00 1.0000 63.8000
 omega____ theta____ kappa____ phi______ frames
 - -19.8939 22.0000 6.0000 26
 4 omega -56.00 46.00 1.0000 63.8000
 omega____ theta____ kappa____ phi______ frames
 - 19.7376 -37.0000 30.0000 102
 5 omega -59.00 53.00 1.0000 63.8000
 omega____ theta____ kappa____ phi______ frames
 - 19.7376 -77.0000 150.0000 112
 6 omega -14.00 98.00 1.0000 63.8000
 omega____ theta____ kappa____ phi______ frames
 - 19.7376 77.0000 -30.0000 112
 7 omega -99.00 14.00 1.0000 63.8000
 omega____ theta____ kappa____ phi______ frames
 - -19.8939 -77.0000 30.0000 113
 8 omega -54.00 59.00 1.0000 63.8000
 omega____ theta____ kappa____ phi______ frames
 - -19.8939 77.0000 -60.0000 113
 9 omega -28.00 56.00 1.0000 63.8000
 omega____ theta____ kappa____ phi______ frames
 - -19.8939 37.0000 -90.0000 84
 10 omega -59.00 17.00 1.0000 63.8000
 omega____ theta____ kappa____ phi______ frames
 - 19.7376 -77.0000 -120.0000 76
 11 omega -54.00 59.00 1.0000 63.8000
 omega____ theta____ kappa____ phi______ frames
 - -19.8939 77.0000 60.0000 113
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0318003
_diffrn_orient_matrix_UB_12      -0.0017097
_diffrn_orient_matrix_UB_13      0.0327041
_diffrn_orient_matrix_UB_21      0.0267596
_diffrn_orient_matrix_UB_22      0.0067836
_diffrn_orient_matrix_UB_23      -0.0230758
_diffrn_orient_matrix_UB_31      -0.0051688
_diffrn_orient_matrix_UB_32      0.0244762
_diffrn_orient_matrix_UB_33      0.0087018
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1322
_diffrn_reflns_av_unetI/netI     0.1372
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            268199
_diffrn_reflns_theta_full        32.80
_diffrn_reflns_theta_max         32.80
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
 Analytical numeric absorption correction using a multifaceted crystal
 model based on expressions derived by R.C. Clark & J.S. Reid.
 (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3491
_exptl_crystal_size_max          0.517
_exptl_crystal_size_mid          0.1184
_exptl_crystal_size_min          0.0509
_refine_diff_density_max         1.930
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         29874
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1939
_refine_ls_R_factor_gt           0.1005
_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^)+(0.1101P)^2^+25.4857P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2599
_refine_ls_wR_factor_ref         0.2906
_reflns_number_gt                14244
_reflns_number_total             29874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500657e_si_002.cif
_cod_data_source_block           NiMeCN_8_1p29CH2Cl2
_cod_original_cell_volume        8376.9(3)
_cod_database_code               4341521
_olex2_refinement_description
;
1. Others
 Fixed Sof: Ni1(0.5) N11(0.5) N12(0.5) N7(0.5) N21(0.5) N22(0.5) N1(0.5)
 N41(0.5) N42(0.5) N57(0.5) N61(0.5) N62(0.5) N2(0.5) C11(0.5) H11(0.5)
 C12(0.5) H12(0.5) C13(0.5) H13(0.5) C2(0.5) C3(0.5) H3(0.5) C4(0.5) C5(0.5)
 H5(0.5) C6(0.5) H6(0.5) C1(0.5) C7(0.5) C21(0.5) H21(0.5) C22(0.5) H22(0.5)
 C23(0.5) H23(0.5) C32(0.5) C33(0.5) H33(0.5) C34(0.5) C35(0.5) H35(0.5)
 C36(0.5) H36(0.5) C31(0.5) C37(0.5) H37a(0.5) H37b(0.5) H37c(0.5) C41(0.5)
 H41(0.5) C42(0.5) H42(0.5) C43(0.5) H43(0.5) C52(0.5) C53(0.5) H53(0.5)
 C54(0.5) C55(0.5) H55(0.5) C56(0.5) H56(0.5) C51(0.5) C57(0.5) C61(0.5)
 H61(0.5) C62(0.5) H62(0.5) C63(0.5) H63(0.5) C72(0.5) C73(0.5) H73(0.5)
 C74(0.5) C75(0.5) H75(0.5) C76(0.5) H76(0.5) C71(0.5) C77(0.5) H77a(0.5)
 H77b(0.5) H77c(0.5) Ni1A(0.5) N11A(0.5) N12A(0.5) N7A(0.5) N21A(0.5) N22A(0.5)
 N1A(0.5) N41A(0.5) N42A(0.5) N57A(0.5) N61A(0.5) N62A(0.5) N2A(0.5) C11A(0.5)
 H11A(0.5) C12A(0.5) H12A(0.5) C13A(0.5) H13A(0.5) C2A(0.5) C3A(0.5) H3A(0.5)
 C4A(0.5) C5A(0.5) H5A(0.5) C6A(0.5) H6A(0.5) C1A(0.5) C7A(0.5) C21A(0.5)
 H21A(0.5) C22A(0.5) H22A(0.5) C23A(0.5) H23A(0.5) C32A(0.5) C33A(0.5)
 H33A(0.5) C34A(0.5) C35A(0.5) H35A(0.5) C36A(0.5) H36A(0.5) C31A(0.5)
 C37A(0.5) H37d(0.5) H37e(0.5) H37f(0.5) C41A(0.5) H41A(0.5) C42A(0.5)
 H42A(0.5) C43A(0.5) H43A(0.5) C52A(0.5) C53A(0.5) H53A(0.5) C54A(0.5)
 C55A(0.5) H55A(0.5) C56A(0.5) H56A(0.5) C51A(0.5) C57A(0.5) C61A(0.5)
 H61A(0.5) C62A(0.5) H62A(0.5) C63A(0.5) H63A(0.5) C72A(0.5) C73A(0.5)
 H73A(0.5) C74A(0.5) C75A(0.5) H75A(0.5) C76A(0.5) H76A(0.5) C71A(0.5)
 C77A(0.5) H77d(0.5) H77e(0.5) H77f(0.5)
 Fixed Uiso: H11(0.042) H12(0.053) H13(0.05) H3(0.049) H5(0.047) H6(0.042)
 H21(0.06) H22(0.08) H23(0.069) H33(0.045) H35(0.047) H36(0.038) H37a(0.098)
 H37b(0.098) H37c(0.098) H41(0.046) H42(0.055) H43(0.054) H53(0.055) H55(0.065)
 H56(0.059) H61(0.033) H62(0.038) H63(0.036) H73(0.05) H75(0.068) H76(0.064)
 H77a(0.1) H77b(0.1) H77c(0.1) H11A(0.041) H12A(0.051) H13A(0.048) H3A(0.048)
 H5A(0.052) H6A(0.046) H21A(0.045) H22A(0.053) H23A(0.048) H33A(0.043)
 H35A(0.052) H36A(0.042) H37d(0.088) H37e(0.088) H37f(0.088) H41A(0.038)
 H42A(0.04) H43A(0.034) H53A(0.031) H55A(0.045) H56A(0.043) H61A(0.043)
 H62A(0.055) H63A(0.063) H73A(0.059) H75A(0.058) H76A(0.047) H77d(0.11)
 H77e(0.11) H77f(0.11) H1Sa(0.064) H1Sb(0.064) H1Sc(0.064) H1Sd(0.064)
 H2Sa(0.131) H2Sb(0.131) H2Sc(0.131) H2Sd(0.131) H3Sa(0.087) H3Sb(0.087)
 H3Sc(0.087) H3Sd(0.087) H4Sa(0.087) H4Sb(0.087) H4Sc(0.087) H4Sd(0.087)
 Fixed X: H11(0.3491) H12(0.2585) H13(0.1313) H3(0.0989) H5(-0.0425)
 H6(0.0317) H21(0.3957) H22(0.3487) H23(0.228) H33(0.1847) H35(0.0034)
 H36(0.0434) H37a(0.0683) H37b(0.0965) H37c(0.0096) H41(0.1914) H42(0.2411)
 H43(0.3629) H53(0.4047) H55(0.5806) H56(0.5335) H61(0.1891) H62(0.2521)
 H63(0.3963) H73(0.4738) H75(0.6322) H76(0.5531) H77a(0.6429) H77b(0.6585)
 H77c(0.5879) H11A(0.4786) H12A(0.5773) H13A(0.5343) H3A(0.4152) H5A(0.3093)
 H6A(0.3128) H21A(0.173) H22A(0.086) H23A(0.164) H33A(0.2941) H35A(0.4739)
 H36A(0.4604) H37d(0.3534) H37e(0.4031) H37f(0.445) H41A(0.5146) H42A(0.5988)
 H43A(0.517) H53A(0.3856) H55A(0.2149) H56A(0.2297) H61A(0.1989) H62A(0.0773)
 H63A(0.1042) H73A(0.2133) H75A(0.3467) H76A(0.3673) H77d(0.2173) H77e(0.3089)
 H77f(0.2708) H1Sa(-0.1573) H1Sb(-0.1811) H1Sc(-0.3434) H1Sd(-0.2667)
 H2Sa(0.3655) H2Sb(0.3757) H2Sc(0.3904) H2Sd(0.3499) H3Sa(0.4386) H3Sb(0.429)
 H3Sc(0.4069) H3Sd(0.4739) H4Sa(0.23) H4Sb(0.1782) H4Sc(0.1077) H4Sd(0.1723)
 Fixed Y: H11(0.0359) H12(-0.0335) H13(-0.0078) H3(0.0356) H5(0.1523)
 H6(0.1855) H21(0.235) H22(0.3198) H23(0.3197) H33(0.2873) H35(0.2003)
 H36(0.1502) H37a(0.2652) H37b(0.3098) H37c(0.2912) H41(0.1956) H42(0.2025)
 H43(0.1525) H53(0.0758) H55(0.0302) H56(0.0771) H61(0.1088) H62(0.0677)
 H63(0.0844) H73(0.1553) H75(0.1979) H76(0.1722) H77a(0.1674) H77b(0.2156)
 H77c(0.2117) H11A(0.0705) H12A(0.1111) H13A(0.1968) H3A(0.242) H5A(0.3397)
 H6A(0.2872) H21A(0.0828) H22A(0.124) H23A(0.192) H33A(0.2048) H35A(0.2867)
 H36A(0.259) H37d(0.258) H37e(0.3012) H37f(0.2528) H41A(0.1532) H42A(0.0941)
 H43A(0.0215) H53A(0.002) H55A(-0.0707) H56A(-0.0213) H61A(0.2033) H62A(0.1816)
 H63A(0.104) H73A(0.0704) H75A(-0.0452) H76A(-0.021) H77d(-0.0205) H77e(-
 0.0274) H77f(0.0225) H1Sa(0.15) H1Sb(0.0959) H1Sc(0.1252) H1Sd(0.0933)
 H2Sa(0.3878) H2Sb(0.4429) H2Sc(0.4341) H2Sd(0.3834) H3Sa(0.4893) H3Sb(0.4342)
 H3Sc(0.4329) H3Sd(0.4318) H4Sa(0.2932) H4Sb(0.3399) H4Sc(0.3567) H4Sd(0.3359)
 Fixed Z: H11(0.3459) H12(0.3176) H13(0.3479) H3(0.4705) H5(0.4418) H6(0.364)
 H21(0.4494) H22(0.4359) H23(0.3322) H33(0.2004) H35(0.1198) H36(0.223)
 H37a(0.0332) H37b(0.0858) H37c(0.0753) H41(0.4909) H42(0.633) H43(0.6629)
 H53(0.6424) H55(0.547) H56(0.4406) H61(0.2041) H62(0.1097) H63(0.1516)
 H73(0.1814) H75(0.3667) H76(0.4434) H77a(0.1953) H77b(0.2416) H77c(0.1696)
 H11A(0.825) H12A(0.7651) H13A(0.7506) H3A(0.6955) H5A(0.8039) H6A(0.9044)
 H21A(0.9208) H22A(0.9938) H23A(1.0617) H33A(1.1467) H35A(1.1186) H36A(0.9965)
 H37d(1.2502) H37e(1.23) H37f(1.2597) H41A(1.0038) H42A(1.089) H43A(1.0879)
 H53A(1.109) H55A(0.9614) H56A(0.8637) H61A(0.8256) H62A(0.7278) H63A(0.6724)
 H73A(0.6155) H75A(0.6806) H76A(0.8071) H77d(0.5324) H77e(0.5453) H77f(0.5186)
 H1Sa(0.5836) H1Sb(0.5744) H1Sc(0.5215) H1Sd(0.5402) H2Sa(0.3286) H2Sb(0.3163)
 H2Sc(0.3081) H2Sd(0.2952) H3Sa(0.643) H3Sb(0.6504) H3Sc(0.7038) H3Sd(0.7804)
 H4Sa(0.4943) H4Sb(0.4837) H4Sc(0.4536) H4Sd(0.4134)
;