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_4115882
_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            'C48 H72 N4 O1.5 V'
_chemical_formula_weight         780.04
_chemical_name_systematic
;
bis(1,3,5-tri-tert-butylbenzene)vanadium(1+) tetracyanoethanide
;
_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                 92.8691(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0332(3)
_cell_length_b                   18.3389(5)
_cell_length_c                   22.7485(7)
_cell_measurement_temperature    200(1)
_cell_volume                     4597.1(2)
_computing_cell_refinement       Denzo-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'WInGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      200(1)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi Scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0817
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
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_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_description       prism
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8937
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0733
_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^)+(0.0861P)^2^+4.0407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1992
_reflns_number_gt                5875
_reflns_number_total             8937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9929741_2.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C48 H72 N4 O1.50 V'
_cod_database_code               4115882