Trinuclear Nickel Complexes with Triplesalen Ligands: Simultaneous Occurrence of Mixed Valence and Valence Tautomerism in the Oxidized Species
Thorsten Glaser; Maik Heidemeier; Roland Fröhlich; Peter Hildebrandt; Eberhart Bothe; Eckhard Bill; Inorganic Chemistry 44 (2005) 5467–5482; doi:10.1021/ic050268x

data_4309266
_publ_section_title
;
Trinuclear Nickel Complexes with Triplesalen Ligands: Simultaneous
Occurrence of Mixed Valence and Valence Tautomerism in the Oxidized Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5467
_journal_page_last               5482
_journal_paper_doi               10.1021/ic050268x
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C54 H66 N12 Ni3 O15'
_chemical_formula_weight         1299.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                112.06(1)
_cell_angle_beta                 109.85(1)
_cell_angle_gamma                91.59(1)
_cell_formula_units_Z            2
_cell_length_a                   14.489(1)
_cell_length_b                   14.606(1)
_cell_length_c                   15.744(1)
_cell_measurement_temperature    198(2)
_cell_volume                     2858.0(5)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode Nonius FF591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30042
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.9491
_exptl_absorpt_correction_T_min  0.6202
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995 & 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         9989
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1125P)^2^+7.4461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2045
_reflns_number_gt                7214
_reflns_number_total             9989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050268xsi20050221_061712.cif
_cod_data_source_block           han2510
_cod_database_code               4309266