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_4338810
_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         'C90 H136 K2 N4 Ni2 O2 S2'
_chemical_formula_sum            'C90 H136 K2 N4 Ni2 O2 S2'
_chemical_formula_weight         1565.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.5970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.7088(4)
_cell_length_b                   18.3156(6)
_cell_length_c                   19.4283(6)
_cell_measurement_reflns_used    4268
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.42
_cell_volume                     4413.5(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker D8 Venture'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            152169
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.9758
_exptl_absorpt_correction_T_min  0.8665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Spek, 2003'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         10977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0326
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                9866
_reflns_number_total             10977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500698v_si_001.cif
_cod_data_source_block           bh456_complex4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4338807--4338810.cif.
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4338810