Three-Coordinate Nickel(II) and Nickel(I) Thiolate Complexes Based on the β-Diketiminate Ligand System.
Horn, Bettina; Limberg, Christian; Herwig, Christian; Braun, Beatrice; Inorganic chemistry 53 (2014) 6867–6874; doi:10.1021/ic500698v

data_4338807
_publ_section_title
;
 Three-Coordinate Nickel(II) and Nickel(I) Thiolate Complexes Based on the
 \b-Diketiminate Ligand System.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6867
_journal_page_last               6874
_journal_paper_doi               10.1021/ic500698v
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C37 H58 N2 Ni S'
_chemical_formula_sum            'C37 H58 N2 Ni S'
_chemical_formula_weight         621.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_method           SHELXL-97
_cell_angle_alpha                95.973(2)
_cell_angle_beta                 90.744(2)
_cell_angle_gamma                113.835(2)
_cell_formula_units_Z            4
_cell_length_a                   9.6736(3)
_cell_length_b                   9.7346(3)
_cell_length_c                   41.7577(11)
_cell_measurement_reflns_used    45791
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.66
_cell_measurement_theta_min      2.30
_cell_volume                     3570.81(19)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      ' 660 frames, detector distance = 125 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0931
_diffrn_reflns_av_unetI/netI     0.1051
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            45193
_diffrn_reflns_theta_full        26.60
_diffrn_reflns_theta_max         26.60
_diffrn_reflns_theta_min         2.30
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           45
_diffrn_source_power             2.25
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  0.9097
_exptl_absorpt_correction_T_min  0.8429
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0061(3)
_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   0.847
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         14924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.847
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0449P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0963
_reflns_d_resolution_high        0.794
_reflns_d_resolution_low         8.865
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              52
_reflns_limit_l_min              0
_reflns_number_gt                9202
_reflns_number_total             14924
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500698v_si_001.cif
_cod_data_source_block           c:bh230_complex1
_cod_depositor_comments
'Adding full bibliography for 4338807--4338810.cif.'
_cod_original_cell_volume        3570.81(18)
_cod_database_code               4338807