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_4341525
_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_absolute_configuration ad
_chemical_formula_moiety         'C40 H36 N10 Ni, 2(B F4), 2(C6 H6)'
_chemical_formula_sum            'C52 H48 B2 F8 N10 Ni'
_chemical_formula_weight         1045.33
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 98.748(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2835(2)
_cell_length_b                   25.5403(7)
_cell_length_c                   20.4839(6)
_cell_measurement_reflns_used    8870
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.0890
_cell_measurement_theta_min      4.0490
_cell_volume                     4800.3(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      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9239
_diffrn_measurement_details
;
  1 omega  -96.00   -2.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7892  125.0000   60.0000 94

  2 omega -110.00  -11.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7892  -57.0000  150.0000 99

  3 omega -114.00  -76.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000 -125.0000  -90.0000 38

  4 omega   29.00   54.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -94.0000 -150.0000 25

  5 omega   24.00   93.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -94.0000  -60.0000 69

  6 omega   65.00  107.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -94.0000 -150.0000 42

  7 omega   37.00   79.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -30.0000  -90.0000 42

  8 omega   32.00   89.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -45.0000 -180.0000 57

  9 omega  102.00  144.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0222  125.0000  -90.0000 42

 10 omega   25.00  171.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0222    0.0000  120.0000 146

 11 omega  -49.00   35.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7892   37.0000  -60.0000 84

 12 omega -115.00  -11.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7892  -57.0000 -120.0000 104

 13 omega -120.00   -7.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7892  -77.0000    0.0000 113

 14 omega   23.00  109.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -94.0000   30.0000 86

 15 omega   76.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0222   30.0000  -30.0000 102

 16 omega   46.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0222   15.0000 -120.0000 132

 17 omega   23.00   45.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -94.0000  120.0000 22
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1647162000
_diffrn_orient_matrix_UB_12      0.0088925000
_diffrn_orient_matrix_UB_13      0.0017801000
_diffrn_orient_matrix_UB_21      0.0143530000
_diffrn_orient_matrix_UB_22      0.0156959000
_diffrn_orient_matrix_UB_23      0.0733036000
_diffrn_orient_matrix_UB_31      0.0293453000
_diffrn_orient_matrix_UB_32      -0.0575740000
_diffrn_orient_matrix_UB_33      0.0202037000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17439
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.78
_diffrn_reflns_theta_min         4.09
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.738
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.623
_exptl_crystal_size_mid          0.0503
_exptl_crystal_size_min          0.0364
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_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     662
_refine_ls_number_reflns         8984
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0596
_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^)+(0.1192P)^2^+1.6885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1672
_reflns_number_gt                8380
_reflns_number_total             8984
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500657e_si_002.cif
_cod_data_source_block           NiMeMediBF4_1_2BF4_2C6H6
_cod_database_code               4341525
_chemical_oxdiff_formula         'Ni C40 N10 H36 B2 F8 C12 H12'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H11(0.049) H12(0.054) H13(0.052) H3(0.048) H5(0.049) H6(0.045)
 H7a(0.076) H7b(0.076) H7c(0.076) H21(0.049) H22(0.052) H23(0.058) H33(0.049)
 H35(0.051) H36(0.046) H37a(0.087) H37b(0.087) H37c(0.087) H61(0.05) H62(0.062)
 H63(0.06) H73(0.059) H75(0.064) H76(0.059) H77a(0.095) H77b(0.095) H77c(0.095)
 H41(0.046) H42(0.053) H43(0.056) H53(0.055) H55(0.063) H56(0.058) H57a(0.088)
 H57b(0.088) H57c(0.088) H1S(0.065) H2S(0.063) H3S(0.062) H4S(0.066) H5S(0.066)
 H6S(0.069) H7S(0.078) H8S(0.091) H9S(0.1) H10S(0.084) H11S(0.075) H12S(0.071)
 Fixed X: H11(0.8181) H12(0.9504) H13(0.8295) H3(0.5819) H5(0.3749) H6(0.4459)
 H7a(0.316) H7b(0.4301) H7c(0.477) H21(0.2857) H22(0.1834) H23(0.3387)
 H33(0.5755) H35(0.7889) H36(0.7219) H37a(0.714) H37b(0.8441) H37c(0.689)
 H61(0.8794) H62(1.0522) H63(0.9401) H73(0.7518) H75(0.4245) H76(0.4042)
 H77a(0.6521) H77b(0.5224) H77c(0.6862) H41(0.2694) H42(0.097) H43(0.1805)
 H53(0.3435) H55(0.624) H56(0.6562) H57a(0.4003) H57b(0.5436) H57c(0.3895)
 H1S(0.2908) H2S(0.1149) H3S(0.0451) H4S(0.1461) H5S(0.3175) H6S(0.3924)
 H7S(0.0833) H8S(0.2102) H9S(0.1994) H10S(0.0768) H11S(-0.0447) H12S(-0.0439)
 Fixed Y: H11(0.5661) H12(0.6042) H13(0.6896) H3(0.7239) H5(0.8366) H6(0.7987)
 H7a(0.8001) H7b(0.8469) H7c(0.7951) H21(0.5801) H22(0.6187) H23(0.6959)
 H33(0.7296) H35(0.8382) H36(0.796) H37a(0.7937) H37b(0.8209) H37c(0.8492)
 H61(0.6806) H62(0.6453) H63(0.5652) H73(0.5178) H75(0.4238) H76(0.4697)
 H77a(0.4528) H77b(0.4152) H77c(0.4035) H41(0.6944) H42(0.6654) H43(0.5772)
 H53(0.5185) H55(0.4103) H56(0.4604) H57a(0.4456) H57b(0.4125) H57c(0.3952)
 H1S(0.9072) H2S(0.8605) H3S(0.777) H4S(0.7419) H5S(0.7893) H6S(0.8719)
 H7S(0.4189) H8S(0.3765) H9S(0.4105) H10S(0.4868) H11S(0.5303) H12S(0.4945)
 Fixed Z: H11(0.7007) H12(0.8058) H13(0.8219) H3(0.8203) H5(0.7038) H6(0.6125)
 H7a(0.8312) H7b(0.8299) H7c(0.8718) H21(0.5021) H22(0.3917) H23(0.3762)
 H33(0.3863) H35(0.5086) H36(0.5978) H37a(0.3395) H37b(0.3878) H37c(0.3721)
 H61(0.5886) H62(0.5172) H63(0.4638) H73(0.4165) H75(0.4513) H76(0.5461)
 H77a(0.3347) H77b(0.349) H77c(0.3828) H41(0.6265) H42(0.7028) H43(0.7431)
 H53(0.7769) H55(0.7252) H56(0.6348) H57a(0.8465) H57b(0.8397) H57c(0.7995)
 H1S(0.5652) H2S(0.6107) H3S(0.5714) H4S(0.4834) H5S(0.4358) H6S(0.4769)
 H7S(0.7579) H8S(0.6809) H9S(0.5759) H10S(0.5469) H11S(0.6222) H12S(0.7282)
;