Reaction of V(C6H6)2with the Borane Adducts of Malononitrile [(C6F5)3B·NCCH2CN·B(C6F5)3] and Water [H2O·B(C6F5)3]
Choukroun, Robert; Lorber, Christian; Vendier, Laure; Organometallics 26 (2007) 3604–; doi:10.1021/om070052y

data_4073070
_publ_section_title
;
 Reaction of V(C6H6)2with the Borane Adducts of Malononitrile
 [(C6F5)3B&#x00B7;NCCH2CN&#x00B7;B(C6F5)3] and Water [H2O&#x00B7;B(C6F5)3]
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3604
_journal_paper_doi               10.1021/om070052y
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C39 H B2 F30 N2, C14 H16 V'
_chemical_formula_sum            'C53 H17 B2 F30 N2 V'
_chemical_formula_weight         1324.25
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.329(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5441(13)
_cell_length_b                   19.9770(16)
_cell_length_c                   15.0623(12)
_cell_measurement_reflns_used    1659
_cell_measurement_temperature    180
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_measurement_wavelength     0.71073
_cell_volume                     5429.6(7)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_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 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \f
_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  0.0452
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21571
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  5
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.325
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.62
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parralellepiped
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.03
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         5298
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0464
_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^)+(0.1026P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1468
_reflns_number_gt                4182
_reflns_number_total             5298
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om070052y-file001.cif
_cod_data_source_block           (1)
_cod_database_code               4073070