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_4341524
_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 H36 N10 Ni, 2(C H2 Cl2), 2(B F4)'
_chemical_formula_sum            'C42 H40 B2 Cl4 F8 N10 Ni'
_chemical_formula_weight         1058.97
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.734(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.8291(6)
_cell_length_b                   9.5433(2)
_cell_length_c                   20.5730(5)
_cell_measurement_reflns_used    15224
_cell_measurement_temperature    99.95(10)
_cell_measurement_theta_max      73.7110
_cell_measurement_theta_min      4.2880
_cell_volume                     4616.5(2)
_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      99.95(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9836
_diffrn_measurement_details
;
  1 omega -114.00  -11.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7892  -57.0000 -120.0000 103

  2 omega  -49.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7892   37.0000   30.0000 80

  3 omega   67.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7892 -125.0000 -180.0000 28

  4 omega -101.00  -73.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      -55.5000 -125.0000    0.0000 28

  5 omega   23.00  109.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -94.0000    0.0000 86

  6 omega   50.00   90.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -30.0000   60.0000 40

  7 omega   23.00   93.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -94.0000   60.0000 70

  8 omega   29.00   76.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -94.0000 -150.0000 47

  9 omega   29.00   85.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -30.0000   30.0000 56

 10 omega   54.00   92.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -45.0000 -120.0000 38

 11 omega   76.00  177.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      107.0222   30.0000 -150.0000 101

 12 omega -120.00   -7.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7892  -77.0000   60.0000 113

 13 omega  -49.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7892   37.0000  -30.0000 84

 14 omega  -49.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7892   37.0000 -180.0000 84

 15 omega -134.00  -43.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -77.0000 -180.0000 91

 16 omega   94.00  178.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      107.0222  125.0000   30.0000 84

 17 omega   77.00  178.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      107.0222   61.0000  -60.0000 101

 18 omega   76.00  178.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      107.0222   30.0000  120.0000 102

 19 omega   73.00  178.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      107.0222   77.0000 -120.0000 105

 20 omega   76.00  125.00   1.0000   39.9900
omega____ theta____ kappa____ phi______ frames
    -      107.0222   30.0000   30.0000 49
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0494685000
_diffrn_orient_matrix_UB_12      -0.0368596000
_diffrn_orient_matrix_UB_13      -0.0652164000
_diffrn_orient_matrix_UB_21      0.0403495000
_diffrn_orient_matrix_UB_22      0.0121019000
_diffrn_orient_matrix_UB_23      -0.0431043000
_diffrn_orient_matrix_UB_31      0.0148127000
_diffrn_orient_matrix_UB_32      -0.1566315000
_diffrn_orient_matrix_UB_33      0.0119540000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38581
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.76
_diffrn_reflns_theta_min         3.76
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.407
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.336
_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            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.1002
_exptl_crystal_size_min          0.0509
_refine_diff_density_max         1.254
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         9154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0639
_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^)+(0.1133P)^2^+5.8254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1830
_refine_ls_wR_factor_ref         0.1949
_reflns_number_gt                7713
_reflns_number_total             9154
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500657e_si_002.cif
_cod_data_source_block           NiMeM2diBF4_1_2BF4_2CH2Cl2
_cod_original_cell_volume        4616.52(19)
_cod_database_code               4341524
_chemical_oxdiff_formula         'Ni C40 H36 N10 B2 F8 C2 H4 Cl4'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H41(0.044) H42(0.05) H43(0.05) H53(0.046) H55(0.046) H56(0.042)
 H57a(0.075) H57b(0.075) H57c(0.075) H61(0.051) H62(0.064) H63(0.059)
 H73(0.052) H75(0.052) H76(0.046) H77a(0.093) H77b(0.093) H77c(0.093)
 H11(0.047) H12(0.052) H13(0.052) H3(0.059) H5(0.069) H6(0.056) H7a(0.112)
 H7b(0.112) H7c(0.112) H21(0.046) H22(0.055) H23(0.057) H33(0.061) H35(0.07)
 H36(0.059) H37a(0.12) H37b(0.12) H37c(0.12) H1sa(0.063) H1sb(0.063)
 H2sa(0.116) H2sb(0.116)
 Fixed X: H41(0.8065) H42(0.7642) H43(0.6658) H53(0.6028) H55(0.487)
 H56(0.5538) H57a(0.5157) H57b(0.4673) H57c(0.4774) H61(0.803) H62(0.7703)
 H63(0.692) H73(0.6661) H75(0.55) H76(0.5794) H77a(0.5441) H77b(0.6059)
 H77c(0.592) H11(0.6644) H12(0.6856) H13(0.7683) H3(0.7952) H5(0.9321)
 H6(0.9155) H7a(0.8687) H7b(0.9141) H7c(0.8483) H21(0.7067) H22(0.766)
 H23(0.8566) H33(0.8992) H35(0.991) H36(0.9239) H37a(1.0294) H37b(0.9782)
 H37c(0.9995) H1sa(0.4956) H1sb(0.5362) H2sa(0.9627) H2sb(0.924)
 Fixed Y: H41(0.3417) H42(0.1527) H43(0.2311) H53(0.3933) H55(0.6394)
 H56(0.7019) H57a(0.4662) H57b(0.5491) H57c(0.3858) H61(0.9525) H62(1.1438)
 H63(1.0431) H73(0.853) H75(0.542) H76(0.5053) H77a(0.7454) H77b(0.8029)
 H77c(0.6392) H11(0.8845) H12(0.9831) H13(0.8454) H3(0.5941) H5(0.3968)
 H6(0.4993) H7a(0.3141) H7b(0.4328) H7c(0.4542) H21(0.4096) H22(0.3442)
 H23(0.4813) H33(0.6897) H35(0.8505) H36(0.7724) H37a(0.7889) H37b(0.8281)
 H37c(0.9391) H1sa(1.1255) H1sb(1.1824) H2sa(0.0945) H2sb(0.177)
 Fixed Z: H41(0.4701) H42(0.3832) H43(0.319) H53(0.2686) H55(0.313)
 H56(0.4156) H57a(0.1769) H57b(0.1971) H57c(0.2145) H61(0.5074) H62(0.5707)
 H63(0.6073) H73(0.6611) H75(0.5971) H76(0.5028) H77a(0.6835) H77b(0.7264)
 H77c(0.7271) H11(0.3765) H12(0.2745) H13(0.2638) H3(0.2619) H5(0.39)
 H6(0.4839) H7a(0.2565) H7b(0.2558) H7c(0.2127) H21(0.576) H22(0.6954)
 H23(0.7206) H33(0.7158) H35(0.6034) H36(0.5036) H37a(0.745) H37b(0.773)
 H37c(0.7283) H1sa(0.4329) H1sb(0.5054) H2sa(0.5689) H2sb(0.5026)
;