B(C6F5)3Adducts of TCNE− and TCNQ−Vanadium Complexes as New Building Blocks for Molecule-Based Magnets
Choukroun, Robert; Lorber, Christian; de Caro, Dominique; Vendier, Laure; Organometallics 25 (2006) 4243–; doi:10.1021/om060433w

data_4074136
_publ_section_title
;
 B(C6F5)3Adducts of TCNE&#x2212; and TCNQ&#x2212;Vanadium Complexes as New
 Building Blocks for Molecule-Based Magnets
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4243
_journal_paper_doi               10.1021/om060433w
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C48 H4 B2 F30 N4'
_chemical_formula_sum            'C48 H4 B2 F30 N4'
_chemical_formula_weight         1228.17
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.250(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0537(11)
_cell_length_b                   14.0758(15)
_cell_length_c                   14.7110(14)
_cell_measurement_reflns_used    2731
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.2222
_cell_measurement_theta_min      2.7066
_cell_measurement_wavelength     0.71073
_cell_volume                     2265.2(4)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.1065
_diffrn_reflns_av_unetI/netI     0.1049
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14118
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  0.9752
_exptl_absorpt_correction_T_min  0.9510
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.073
_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   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         3259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.132
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0899P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1895
_reflns_number_gt                1601
_reflns_number_total             3259
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om060433wsi20060518_105049.cif
_cod_data_source_block           (2)
_cod_database_code               4074136