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_4341517
_publ_section_title
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 Homoleptic Nickel(II) Complexes of Redox-Tunable Pincer-type Ligands.
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_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'
_chemical_formula_sum            'C40 H36 N10 Ni'
_chemical_formula_weight         715.50
_chemical_name_systematic
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 ? 
;
_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     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                79.7090(10)
_cell_angle_beta                 84.0790(10)
_cell_angle_gamma                75.7380(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7592(2)
_cell_length_b                   12.8293(3)
_cell_length_c                   16.0382(3)
_cell_measurement_reflns_used    9389
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67
_cell_measurement_theta_min      3
_cell_volume                     1715.33(7)
_computing_cell_refinement       'SAINT v7.56A (Bruker, 2008)'
_computing_data_collection       'APEX2-2008.5-0 (Bruker, 2008)'
_computing_data_reduction        'SADABS-2008/1 (Bruker, 2008)'
_computing_molecular_graphics
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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.
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_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-2008/4(Bruker, 2008)'
_computing_structure_solution    'XS/SHELXTL-2008/1 (Bruker, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker APEX2 CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14299
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.98
_diffrn_reflns_theta_min         2.81
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_T_max  0.9034
_exptl_absorpt_correction_T_min  0.6603
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 Numerical (based on real shape of the crystal) absorption
 correction followed by:
 SADABS. Program for empirical absorption correction of
 area-detector data. University of Goetingen. Germany. 
 Sheldrick, G. M. 1996
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0403P)^2^+1.2177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                5444
_reflns_number_total             5860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500657e_si_002.cif
_cod_data_source_block           NiMeMe2_1
_cod_original_cell_volume        1715.33(6)
_cod_database_code               4341517
_olex2_refinement_description
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1. Others
 Fixed Sof: H77a(0.5) H77b(0.5) H77c(0.5) H77d(0.5) H77e(0.5) H77f(0.5)
 Fixed Uiso: H11(0.025) H12(0.028) H13(0.026) H3(0.023) H5(0.028) H6(0.024)
 H7a(0.051) H7b(0.051) H7c(0.051) H21(0.025) H22(0.026) H23(0.025) H33(0.023)
 H35(0.024) H36(0.022) H37a(0.047) H37b(0.047) H37c(0.047) H41(0.026)
 H42(0.029) H43(0.026) H53(0.026) H55(0.03) H56(0.027) H57a(0.05) H57b(0.05)
 H57c(0.05) H61(0.026) H62(0.032) H63(0.03) H73(0.025) H75(0.028) H76(0.026)
 H77a(0.041) H77b(0.041) H77c(0.041) H77d(0.041) H77e(0.041) H77f(0.041)
 Fixed X: H11(0.1583) H12(0.4232) H13(0.5364) H3(0.4807) H5(0.4252) H6(0.2629)
 H7a(0.6332) H7b(0.6453) H7c(0.5054) H21(-0.366) H22(-0.4765) H23(-0.2618) H33(-
 0.087) H35(0.3882) H36(0.3974) H37a(0.0399) H37b(0.2254) H37c(0.1628) H41(-
 0.0485) H42(-0.186) H43(-0.2383) H53(-0.1089) H55(-0.1947) H56(-0.2045) H57a(-
 0.1886) H57b(-0.0127) H57c(-0.157) H61(0.3137) H62(0.3178) H63(0.0406) H73(-
 0.2259) H75(-0.6028) H76(-0.4444) H77a(-0.6369) H77b(-0.5579) H77c(-0.484)
 H77d(-0.4823) H77e(-0.5613) H77f(-0.6352)
 Fixed Y: H11(0.8802) H12(0.8194) H13(0.6298) H3(0.4638) H5(0.2729) H6(0.419)
 H7a(0.2788) H7b(0.2105) H7c(0.2096) H21(0.7563) H22(0.6483) H23(0.5864)
 H33(0.6859) H35(0.6023) H36(0.582) H37a(0.6606) H37b(0.6081) H37c(0.7365)
 H41(0.4877) H42(0.4225) H43(0.5754) H53(0.694) H55(1.0218) H56(1.0224)
 H57a(0.9235) H57b(0.8509) H57c(0.7934) H61(0.8107) H62(1.0039) H63(1.1133)
 H73(1.1016) H75(1.0804) H76(0.9545) H77a(1.2177) H77b(1.15) H77c(1.2447)
 H77d(1.1906) H77e(1.2582) H77f(1.1636)
 Fixed Z: H11(0.3541) H12(0.4163) H13(0.3849) H3(0.3976) H5(0.2346) H6(0.1583)
 H7a(0.4144) H7b(0.3388) H7c(0.4113) H21(0.2446) H22(0.16) H23(0.0509) H33(-
 0.0548) H35(-0.0779) H36(0.0665) H37a(-0.193) H37b(-0.2014) H37c(-0.2026)
 H41(0.2992) H42(0.4373) H43(0.5221) H53(0.5678) H55(0.525) H56(0.3825)
 H57a(0.6721) H57b(0.6621) H57c(0.6889) H61(0.1289) H62(0.067) H63(0.0881)
 H73(0.0599) H75(0.223) H76(0.3173) H77a(0.0976) H77b(0.0232) H77c(0.0429)
 H77d(0.0115) H77e(0.086) H77f(0.0662)
;