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_4341519
_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         'C38 H30 Br2 N10 Ni'
_chemical_formula_sum            'C38 H30 Br2 N10 Ni'
_chemical_formula_weight         845.25
_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                80.012(2)
_cell_angle_beta                 83.860(2)
_cell_angle_gamma                76.027(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7709(3)
_cell_length_b                   12.8252(4)
_cell_length_c                   16.1692(5)
_cell_measurement_reflns_used    6900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67
_cell_measurement_theta_min      3
_cell_volume                     1734.24(10)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_collection       'APEX2-2009.5-1 (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.
;
_computing_publication_material
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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.
;
_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 0.990
_diffrn_measured_fraction_theta_max 0.940
_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  0.0208
_diffrn_reflns_av_unetI/netI     0.0239
_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       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14217
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.55
_diffrn_reflns_theta_min         2.78
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.866
_exptl_absorpt_correction_T_max  0.8995
_exptl_absorpt_correction_T_min  0.3161
_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    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5894
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.244
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0197P)^2^+3.8620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                5488
_reflns_number_total             5894
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500657e_si_002.cif
_cod_data_source_block           NeMeBr_4
_cod_database_code               4341519
_olex2_refinement_description
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1. Others
 Fixed Uiso: H37a(0.044) H37b(0.044) H37c(0.044) H7a(0.036) H7b(0.036)
 H7c(0.036) H40a(0.061) H40b(0.061) H40c(0.061) H40d(0.048) H40e(0.048)
 H40f(0.048) H11(0.025) H12(0.031) H13(0.032) H3(0.024) H5(0.027) H6(0.027)
 H23(0.027) H22(0.03) H21(0.028) H33(0.026) H35(0.03) H36(0.027) H41(0.025)
 H42(0.026) H43(0.026) H53(0.024) H55(0.025) H56(0.024) H61(0.027) H62(0.029)
 H63(0.027) H73(0.023) H75(0.031) H76(0.026)
 Fixed X: H37a(-0.1622) H37b(-0.2024) H37c(-0.0231) H7a(-0.5336) H7b(-0.4996)
 H7c(-0.6431) H40a(0.6798) H40b(0.5447) H40c(0.5462) H40d(0.0436) H40e(0.2293)
 H40f(0.164) H11(0.3121) H12(0.3189) H13(0.0439) H3(-0.2238) H5(-0.6003) H6(-
 0.4406) H23(-0.2405) H22(-0.1872) H21(-0.049) H33(-0.1023) H35(-0.1905) H36(-
 0.203) H41(-0.3661) H42(-0.4752) H43(-0.2601) H53(-0.0841) H55(0.3911)
 H56(0.3986) H61(0.1582) H62(0.4197) H63(0.5312) H73(0.4748) H75(0.4257)
 H76(0.2648)
 Fixed Y: H37a(0.7895) H37b(0.9195) H37c(0.853) H7a(1.157) H7b(1.2534)
 H7c(1.1989) H40a(0.2614) H40b(0.1951) H40c(0.2715) H40d(0.6615) H40e(0.6117)
 H40f(0.7392) H11(0.8113) H12(1.0034) H13(1.1137) H3(1.1008) H5(1.0831)
 H6(0.9571) H23(0.5777) H22(0.4246) H21(0.4903) H33(0.6946) H35(1.0223)
 H36(1.0235) H41(0.7585) H42(0.6499) H43(0.5841) H53(0.685) H55(0.6026)
 H56(0.5806) H61(0.8876) H62(0.828) H63(0.6378) H73(0.4708) H75(0.2748)
 H76(0.4193)
 Fixed Z: H37a(0.6813) H37b(0.6683) H37c(0.6614) H7a(0.0222) H7b(0.063)
 H7c(0.101) H40a(0.3635) H40b(0.371) H40c(0.4392) H40d(-0.1891) H40e(-0.1982)
 H40f(-0.1965) H11(0.1238) H12(0.0654) H13(0.0899) H3(0.0614) H5(0.2264)
 H6(0.3184) H23(0.5178) H22(0.4326) H21(0.2959) H33(0.5641) H35(0.5237)
 H36(0.3817) H41(0.2437) H42(0.1597) H43(0.0536) H53(-0.0527) H55(-0.0759)
 H56(0.068) H61(0.3471) H62(0.4113) H63(0.3846) H73(0.3984) H75(0.2382)
 H76(0.1607)
;