Synthesis and Crystal Structure of Unprecedented Phosphine Adducts of d1-Aryl Imido-Vanadium(IV) Complexes
Christian Lorber; Robert Choukroun; Bruno Donnadieu; Inorganic Chemistry 42 (2003) 673–675; doi:10.1021/ic026089m

data_4313071
_publ_contact_author             'Dr Christian Lorber'
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
UPR-CNRS 8241
205, route de Narbonne
31077 Toulouse cedex, France                                               
;
_publ_contact_author_email       ' lorber@lcc-toulouse.fr '
_publ_section_title
;
 Synthesis and Crystal Structure of Unprecedented Phosphine Adducts of
 d1-Aryl Imido-Vanadium(IV) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              673
_journal_page_last               675
_journal_paper_doi               10.1021/ic026089m
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C76 H78 Cl8 N2 P4 V2'
_chemical_formula_weight         1528.76
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.70(3)
_cell_angle_beta                 111.31(3)
_cell_angle_gamma                92.33(3)
_cell_formula_units_Z            1
_cell_length_a                   11.745(2)
_cell_length_b                   13.517(3)
_cell_length_c                   13.862(3)
_cell_measurement_temperature    180(2)
_cell_volume                     1910.9(9)
_computing_cell_refinement
'Crysalis RED version beta 169(Oxford Diffraction)'
_computing_data_collection
'Crysalis CCD version beta 169(Oxford Diffraction)'
_computing_data_reduction
'Crysalis RED version beta 169(Oxford Diffraction)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device       'Crysalis Oxford Diffraction'
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12495
_diffrn_reflns_theta_full        22.21
_diffrn_reflns_theta_max         22.21
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  'every frame'
_exptl_absorpt_coefficient_mu    0.650
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         4576
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0982P)^2^+0.8905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                3701
_reflns_number_total             4576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026089m_s1_1.cif
_cod_data_source_block           (4)
_cod_original_cell_volume        1910.9(7)
_cod_database_code               4313071
_computing_corr_abs              DIFABS