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_4341518
_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         'C36 H28 N10 Ni, C H2 Cl2'
_chemical_formula_sum            'C37 H30 Cl2 N10 Ni'
_chemical_formula_weight         744.32
_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                 93.2065(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.55338(11)
_cell_length_b                   17.50145(18)
_cell_length_c                   40.5845(5)
_cell_measurement_reflns_used    28800
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.5364
_cell_measurement_theta_min      3.2693
_cell_volume                     6775.02(13)
_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      100.0
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
1 omega  -65.00   35.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      -40.7737   37.0000   90.0000 100

2 omega    9.00   34.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      -40.7737   37.0000    0.0000 25

3 omega  -67.00  -40.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      -40.7737   37.0000    0.0000 27

4 omega   57.00   84.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-       40.7737 -125.0000 -150.0000 27

5 omega   25.00   86.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-       40.7737 -125.0000  -30.0000 61

6 omega  102.00  150.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      100.5756  125.0000    0.0000 48

7 omega   23.00   87.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      100.5756  -77.0000 -180.0000 64

8 omega   43.00   77.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      100.5756  -45.0000   90.0000 34

9 omega   86.00  113.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      100.5756 -110.0000  151.0000 27

10 omega  102.00  174.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      100.5756   45.0000 -150.0000 72

11 omega   23.00   94.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      100.5756  -77.0000   90.0000 71

12 omega   60.00  175.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      100.5756   15.0000 -180.0000 115

13 omega -119.00   -7.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      -40.7737  -77.0000 -150.0000 112

14 omega -117.00  -14.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      -40.7737  -37.0000  -60.0000 103

15 omega -119.00   -7.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      -40.7737  -77.0000   90.0000 112

16 omega   21.00  113.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      100.5756 -106.0000   18.0000 92

17 omega   39.00  178.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      100.5756   15.0000    0.0000 139

18 omega   73.00  168.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      100.5756   45.0000   60.0000 95

19 omega   26.00   77.00   1.0000   23.7900
omega____ theta____ kappa____ phi______ frames
-      100.5756  -45.0000 -120.0000 51
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0139569
_diffrn_orient_matrix_UB_12      0.0815657
_diffrn_orient_matrix_UB_13      -0.0137425
_diffrn_orient_matrix_UB_21      -0.0570227
_diffrn_orient_matrix_UB_22      -0.0277554
_diffrn_orient_matrix_UB_23      -0.0341843
_diffrn_orient_matrix_UB_31      -0.1503667
_diffrn_orient_matrix_UB_32      0.0181796
_diffrn_orient_matrix_UB_33      0.0094124
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            53167
_diffrn_reflns_theta_full        70.67
_diffrn_reflns_theta_max         70.67
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.635
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.63724
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.000036(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         12822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+5.9038P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                10793
_reflns_number_total             12822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500657e_si_002.cif
_cod_data_source_block           NiHH_3_CH2Cl2
_cod_database_code               4341518
_olex2_refinement_description
;
1. Others
 Fixed Sof: Ni1(0.5) N11(0.5) N12(0.5) N21(0.5) N22(0.5) N1(0.5) N41(0.5)
 N42(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) H4(0.5) C5(0.5) H5(0.5)
 C6(0.5) H6(0.5) C1(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) H34(0.5) C35(0.5) H35(0.5) C36(0.5)
 H36(0.5) C31(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) H54(0.5) C55(0.5) H55(0.5) C56(0.5)
 H56(0.5) C51(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) H74(0.5) C75(0.5) H75(0.5) C76(0.5)
 H76(0.5) C71(0.5) Ni2(0.5) N11A(0.5) N12A(0.5) N21A(0.5) N22A(0.5) N1A(0.5)
 N41A(0.5) N42A(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) H4A(0.5)
 C5A(0.5) H5A(0.5) C6A(0.5) H6A(0.5) C1A(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)
 H34A(0.5) C35A(0.5) H35A(0.5) C36A(0.5) H36A(0.5) C31A(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) H54A(0.5) C55A(0.5) H55A(0.5) C56A(0.5) H56A(0.5)
 C51A(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) H74A(0.5) C75A(0.5) H75A(0.5)
 C76A(0.5) H76A(0.5) C71A(0.5) Cl1(0.5) Cl2(0.5) C1S(0.5) H1Sa(0.5) H1Sb(0.5)
 Cl3(0.5) Cl4(0.5) C2S(0.5) H2Sa(0.5) H2Sb(0.5)
 Fixed Uiso: H11(0.024) H12(0.026) H13(0.023) H3(0.022) H4(0.024) H5(0.026)
 H6(0.023) H21(0.023) H22(0.028) H23(0.026) H33(0.024) H34(0.027) H35(0.026)
 H36(0.022) H41(0.023) H42(0.03) H43(0.029) H53(0.029) H54(0.036) H55(0.034)
 H56(0.027) H61(0.023) H62(0.028) H63(0.025) H73(0.023) H74(0.024) H75(0.025)
 H76(0.023) H11A(0.023) H12A(0.028) H13A(0.027) H3A(0.026) H4A(0.03) H5A(0.027)
 H6A(0.023) H21A(0.02) H22A(0.024) H23A(0.024) H33A(0.024) H34A(0.028)
 H35A(0.027) H36A(0.022) H41A(0.021) H42A(0.024) H43A(0.023) H53A(0.02)
 H54A(0.024) H55A(0.026) H56A(0.023) H61A(0.025) H62A(0.033) H63A(0.029)
 H73A(0.024) H74A(0.028) H75A(0.027) H76A(0.023) H1Sa(0.043) H1Sb(0.043)
 H2Sa(0.054) H2Sb(0.054)
 Fixed X: H11(0.6814) H12(0.855) H13(0.8831) H3(0.7462) H4(0.7464) H5(0.7187)
 H6(0.6847) H21(0.2753) H22(0.2193) H23(0.4416) H33(0.6945) H34(0.92)
 H35(1.0327) H36(0.9249) H41(0.3976) H42(0.1464) H43(0.0814) H53(0.1814)
 H54(0.1819) H55(0.3025) H56(0.4226) H61(0.9056) H62(1.0197) H63(0.8266)
 H73(0.613) H74(0.4016) H75(0.2165) H76(0.2421) H11A(0.6545) H12A(0.5209)
 H13A(0.3868) H3A(0.4227) H4A(0.3149) H5A(0.2662) H6A(0.3239) H21A(0.8274)
 H22A(0.7778) H23A(0.5252) H33A(0.311) H34A(0.0754) H35A(0.0032) H36A(0.1586)
 H41A(0.6213) H42A(0.8379) H43A(1.0146) H53A(1.0276) H54A(1.1585) H55A(1.1249)
 H56A(0.9597) H61A(0.303) H62A(0.2779) H63A(0.5079) H73A(0.6575) H74A(0.8797)
 H75A(1.0632) H76A(1.0244) H1Sa(0.0605) H1Sb(-0.0683) H2Sa(0.2244) H2Sb(0.2811)
 Fixed Y: H11(0.1244) H12(0.0208) H13(-0.0461) H3(-0.1027) H4(-0.1426) H5(-
 0.0519) H6(0.0738) H21(0.2734) H22(0.326) H23(0.3204) H33(0.3656) H34(0.3459)
 H35(0.2312) H36(0.1405) H41(0.0944) H42(0.0585) H43(0.0634) H53(0.0049)
 H54(0.0118) H55(0.1101) H56(0.1994) H61(0.2158) H62(0.3192) H63(0.3887)
 H73(0.4501) H74(0.4976) H75(0.4135) H76(0.2862) H11A(0.8137) H12A(0.9357)
 H13A(0.9453) H3A(0.9371) H4A(0.9218) H5A(0.7988) H6A(0.6951) H21A(0.5378)
 H22A(0.4183) H23A(0.4232) H33A(0.4403) H34A(0.4631) H35A(0.5881) H36A(0.6866)
 H41A(0.6617) H42A(0.6798) H43A(0.7361) H53A(0.8435) H54A(0.8953) H55A(0.85)
 H56A(0.7586) H61A(0.6945) H62A(0.6772) H63A(0.63) H73A(0.5216) H74A(0.4704)
 H75A(0.5219) H76A(0.6197) H1Sa(0.1796) H1Sb(0.2146) H2Sa(0.4772) H2Sb(0.5445)
 Fixed Z: H11(0.0551) H12(0.0476) H13(0.1018) H3(0.1425) H4(0.197) H5(0.2381)
 H6(0.2249) H21(0.1384) H22(0.1931) H23(0.228) H33(0.2205) H34(0.2429)
 H35(0.2324) H36(0.1994) H41(0.1853) H42(0.1793) H43(0.1191) H53(0.0693)
 H54(0.0123) H55(-0.0119) H56(0.0201) H61(0.1323) H62(0.1014) H63(0.0707)
 H73(0.0804) H74(0.0588) H75(0.0473) H76(0.059) H11A(0.0641) H12A(0.059)
 H13A(0.1094) H3A(0.1673) H4A(0.2164) H5A(0.2344) H6A(0.2036) H21A(0.127)
 H22A(0.1574) H23A(0.1682) H33A(0.1354) H34A(0.1419) H35A(0.1513) H36A(0.15)
 H41A(0.2003) H42A(0.2366) H43A(0.2012) H53A(0.1651) H54A(0.1244) H55A(0.0706)
 H56A(0.0578) H61A(0.0764) H62A(0.0154) H63A(-0.0015) H73A(0.0157) H74A(0.013)
 H75A(0.046) H76A(0.0816) H1Sa(0.0304) H1Sb(0.0474) H2Sa(0.2246) H2Sb(0.2035)
;