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_4341520
_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 H30 F6 N10 Ni'
_chemical_formula_sum            'C40 H30 F6 N10 Ni'
_chemical_formula_weight         823.45
_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                79.7450(10)
_cell_angle_beta                 84.0600(10)
_cell_angle_gamma                74.1850(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9877(2)
_cell_length_b                   13.0879(2)
_cell_length_c                   16.3390(3)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67
_cell_measurement_theta_min      3
_cell_volume                     1816.60(6)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_collection       'APEX2-2009.3-0 (Bruker, 2009)'
_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-2008/4 (Bruker, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.933
_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  0.0000
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6167
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.91
_diffrn_reflns_theta_min         2.75
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_T_max  0.8021
_exptl_absorpt_correction_T_min  0.6492
_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            red
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.00074(12)
_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   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         6167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0453P)^2^+1.8208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                5883
_reflns_number_total             6167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500657e_si_002.cif
_cod_data_source_block           NiMeCF3_6
_cod_database_code               4341520
_olex2_refinement_description
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1. Shared sites
{C10, C7}
{C20, C37}
{C77, C30}
{C57, C40}
2. Others
 Fixed Uiso: H11(0.053) H12(0.057) H13(0.05) H3(0.044) H5(0.055) H6(0.054)
 H7a(0.081) H7b(0.081) H7c(0.081) H21(0.053) H22(0.065) H23(0.059) H33(0.047)
 H35(0.058) H36(0.058) H20a(0.092) H20b(0.092) H20c(0.092) H61(0.047)
 H62(0.051) H63(0.048) H73(0.045) H75(0.054) H76(0.056) H77a(0.083) H77b(0.083)
 H77c(0.083) H41(0.044) H42(0.047) H43(0.043) H53(0.039) H55(0.054) H56(0.055)
 H40a(0.078) H40b(0.078) H40c(0.078)
 Fixed X: H11(-0.0464) H12(-0.1864) H13(-0.238) H3(-0.0978) H5(-0.1837) H6(-
 0.1974) H7a(-0.2069) H7b(-0.0383) H7c(-0.0606) H21(0.2928) H22(0.285)
 H23(0.0132) H33(-0.2492) H35(-0.6033) H36(-0.4377) H20a(-0.621) H20b(-0.4909)
 H20c(-0.6121) H61(-0.363) H62(-0.4716) H63(-0.2572) H73(-0.0805) H75(0.3863)
 H76(0.3923) H77a(0.1623) H77b(0.2296) H77c(0.0464) H41(0.1477) H42(0.4103)
 H43(0.5267) H53(0.4718) H55(0.4294) H56(0.2664) H40a(0.6759) H40b(0.5351)
 H40c(0.5583)
 Fixed Y: H11(0.4929) H12(0.4323) H13(0.5807) H3(0.6899) H5(1.0132) H6(1.0169)
 H7a(0.8727) H7b(0.8909) H7c(0.7716) H21(0.8102) H22(1.0003) H23(1.1072)
 H33(1.0927) H35(1.0805) H36(0.9556) H20a(1.1405) H20b(1.204) H20c(1.2362)
 H61(0.7606) H62(0.6617) H63(0.595) H73(0.6839) H75(0.5909) H76(0.5765)
 H77a(0.5843) H77b(0.6873) H77c(0.7012) H41(0.8873) H42(0.8319) H43(0.642)
 H53(0.4764) H55(0.2784) H56(0.4196) H40a(0.2595) H40b(0.2042) H40c(0.2836)
 Fixed Z: H11(0.2963) H12(0.4287) H13(0.5143) H3(0.5617) H5(0.5239) H6(0.3843)
 H7a(0.6772) H7b(0.6512) H7c(0.6716) H21(0.1228) H22(0.0618) H23(0.0901)
 H33(0.0659) H35(0.2373) H36(0.3258) H20a(0.0637) H20b(0.0343) H20c(0.1103)
 H61(0.2434) H62(0.1559) H63(0.0521) H73(-0.0478) H75(-0.0668) H76(0.0748)
 H77a(-0.1826) H77b(-0.1909) H77c(-0.182) H41(0.3434) H42(0.4008) H43(0.3767)
 H53(0.3995) H55(0.2456) H56(0.1673) H40a(0.3627) H40b(0.3827) H40c(0.4416)
;