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_4309265
_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            'C69 H96 N6 Ni3 O6'
_chemical_formula_weight         1281.65
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            4
_cell_length_a                   19.6170(8)
_cell_length_b                   19.6170(8)
_cell_length_c                   23.2168(14)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     7737.5(6)
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            59630
_diffrn_reflns_theta_full        25.13
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_T_max  0.9848
_exptl_absorpt_correction_T_min  0.9134
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
; 
Integration and final cell refinement were done with SAINT.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Transparent hexagon'
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                3164
_reflns_number_total             4578
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050268xsi20050221_061656.cif
_cod_data_source_block           noabs
_cod_database_code               4309265