Synthesis, Structure, and Reactivity of Dinuclear Nickel Amino-Thiophenolate Complexes Bearing Bridging VO2(OH)2- and VO2(OR)2- Coligands
Vasile Lozan; Jochen Lach; Berthold Kersting; Inorganic Chemistry 51 (2012) 5213–5223; doi:10.1021/ic300085f

data_4329088
_publ_contact_author_address
; Institut fuer Anorganische Chemie
  Universitaet Leipzig, Johannisallee 29
  04103 Leipzig
  Germany
;
_publ_contact_author_email       b.kersting@uni-leipzig.de
_publ_contact_author_fax         '+49/(0)341/973 6199'
_publ_contact_author_name        'Prof. Dr Berthold Kersting'
_publ_contact_author_phone       '+49/(0)341/973 6143'
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Dinuclear Nickel
 Amino-Thiophenolate Complexes Bearing Bridging VO2(OH)2- and VO2(OR)2-
 Coligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5213
_journal_page_last               5223
_journal_paper_doi               10.1021/ic300085f
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source
;
 Crystals were grown by recystallization from acetonitrile 
;
_chemical_formula_structural
; 
 [Ni2L(u-O2V(OEt)2)][BPh4].xCH3CN 
;
_chemical_formula_sum            'C66 H94 B N6 Ni2 O4 S2 V'
_chemical_formula_weight         1278.76
_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
_cell_angle_alpha                72.01(3)
_cell_angle_beta                 64.20(3)
_cell_angle_gamma                66.63(3)
_cell_formula_units_Z            2
_cell_length_a                   16.184(3)
_cell_length_b                   16.065(3)
_cell_length_c                   16.414(3)
_cell_measurement_temperature    213(2)
_cell_volume                     3478.7(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  BRUKER-AXS
_diffrn_measurement_method       hemisphere
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0642
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26191
_diffrn_reflns_theta_full        25.44
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.8926
_exptl_absorpt_correction_T_min  0.8299
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         1.370
_refine_diff_density_min         -1.966
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         12010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0593
_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^)+(0.1293P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1714
_refine_ls_wR_factor_ref         0.1795
_reflns_number_gt                8286
_reflns_number_total             12010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300085f_si_001_2.cif
_cod_data_source_block           voets
_cod_original_cell_volume        3478.7(12)
_cod_database_code               4329088