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_4313073
_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            'C44 H86 Cl8 N2 P6 V2'
_chemical_formula_weight         1214.44
_chemical_name_systematic
;
 ?
;
_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                90.000(5)
_cell_angle_beta                 90.660(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   10.769(5)
_cell_length_b                   15.902(5)
_cell_length_c                   18.413(5)
_cell_measurement_temperature    180(2)
_cell_volume                     3153(2)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0982
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11812
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         3.36
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  'every frame'
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.504
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0005(5)
_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   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+16.5390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                2702
_reflns_number_total             3289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026089m_s1_3.cif
_cod_data_source_block           (3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4313073
_computing_corr_abs              DIFABS