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_4073073
_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         'C30 B2 F25 O, C12 H12 V'
_chemical_formula_sum            'C42 H12 B2 F25 O V'
_chemical_formula_weight         1080.08
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                97.186(13)
_cell_angle_beta                 108.126(14)
_cell_angle_gamma                111.383(15)
_cell_formula_units_Z            2
_cell_length_a                   11.9438(19)
_cell_length_b                   12.909(2)
_cell_length_c                   15.175(2)
_cell_measurement_reflns_used    1470
_cell_measurement_temperature    180
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      3.3
_cell_measurement_wavelength     0.71073
_cell_volume                     1993.9(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0555
_diffrn_reflns_av_unetI/netI     0.1605
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15516
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         3.3
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.861
_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    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.73
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         8130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.73
_refine_ls_R_factor_all          0.1574
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0659
_reflns_number_gt                2863
_reflns_number_total             8130
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om070052y-file001.cif
_cod_data_source_block           (4)
_cod_original_cell_volume        1993.9(5)
_cod_database_code               4073073