Identification of [MII(Arene)2]2+ (M = V, Cr) as the Key Intermediate in the Formation of V[TCNE]x.ySolvent Magnets and Cr[TCNE]x.Solvent
Douglas C. Gordon; Laura Deakin; Atta M. Arif; Joel S. Miller; Journal of the American Chemical Society 122 (2000) 290–299; doi:10.1021/ja9929741

data_4115881
_publ_section_title
;
 Identification of [MII(Arene)2]2+ (M = V, Cr) as the Key Intermediate in
 the Formation of V[TCNE]x.ySolvent Magnets and Cr[TCNE]x.Solvent
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              290
_journal_page_last               299
_journal_paper_doi               10.1021/ja9929741
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C64 H84 B O V'
_chemical_formula_weight         931.06
_chemical_name_systematic
;
 bis(1,3,5-tri-tert-butylbenzene)vanadium(1+) tetraphenylborate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.6430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.23960(10)
_cell_length_b                   20.2835(4)
_cell_length_c                   26.6935(4)
_cell_measurement_temperature    200(1)
_cell_volume                     6065.57(16)
_computing_cell_refinement       Denzo
_computing_data_collection       collect
_computing_data_reduction        denzo
_computing_molecular_graphics    Ortep3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Kappaccd
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            9919
_diffrn_reflns_theta_full        24.41
_diffrn_reflns_theta_max         24.41
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_type   scalepack
_exptl_crystal_density_diffrn    1.020
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.0136(13)
_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   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         9919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+4.5811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1921
_reflns_number_gt                8070
_reflns_number_total             9919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9929741_1.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4115881