Synthesis and Ligand Non-Innocence of Thiolate-Ligated (N4S) Iron(II) and Nickel(II) Bis(imino)pyridine Complexes
Leland R. Widger; Yunbo Jiang; Maxime A. Siegler; Devesh Kumar; Reza Latifi; Sam P. de Visser; Guy N. L. Jameson; David P. Goldberg; Inorganic Chemistry 52 (2013) 10467–10480; doi:10.1021/ic4013558

data_4335957
_publ_section_title
;
 Synthesis and Ligand Non-Innocence of Thiolate-Ligated (N4S) Iron(II) and
 Nickel(II) Bis(imino)pyridine Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10467
_journal_page_last               10480
_journal_paper_doi               10.1021/ic4013558
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C27 H30 N3 Ni S, C H2 Cl2, B F4'
_chemical_formula_sum            'C28 H32 B Cl2 F4 N3 Ni S'
_chemical_formula_weight         659.05
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           14
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_symmetry_space_group_name_Hall  '-P 2ybc'
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_cell_angle_alpha                90.00
_cell_angle_beta                 95.0548(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.13933(17)
_cell_length_b                   13.80648(15)
_cell_length_c                   13.94752(16)
_cell_measurement_reflns_used    19778
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.06
_cell_measurement_theta_min      1.90
_cell_volume                     2903.98(6)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
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_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
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_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
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_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 15.9890
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39899
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         7712
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0601P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                5909
_reflns_number_total             7712
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic4013558_si_005.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4335957