Vanadium complexes incorporating the ?-diketiminato ligand L. Syntheses and structures of LV(OSO2CF3)2 and LVPPh2
Neculai, Dante; Mirela Neculai, Ana; Roesky, Herbert W.; Herbst-Irmer, Regine; Walfort, Bernhard; Stalke, Dietmar; Dalton Transactions  (2003) 2831–; doi:10.1039/b303196a

data_7012978
_publ_section_title
;
 Vanadium complexes incorporating the ?-diketiminato ligand L.
 Syntheses and structures of LV(OSO2CF3)2 and LVPPh2
;
_journal_issue                   14
_journal_name_full               'Dalton Transactions'
_journal_page_first              2831
_journal_paper_doi               10.1039/b303196a
_journal_year                    2003
_chemical_formula_sum            'C33 H51 F6 N4 O6 S2 V'
_chemical_formula_weight         828.84
_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                90.00
_cell_angle_beta                 97.774(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.329(2)
_cell_length_b                   13.388(2)
_cell_length_c                   19.652(3)
_cell_measurement_reflns_used    9666
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.16
_cell_volume                     3996.0(10)
_computing_cell_refinement       'SAINT-NT V5/6.0'
_computing_data_collection       'SMART-NT V5.6'
_computing_data_reduction        'SAINT-NT V5/6.0'
_computing_molecular_graphics    'XP in SHELXTL-97'
_computing_publication_material  'XP in SHELXTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'omega scans'
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30036
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  0.9586
_exptl_absorpt_correction_T_min  0.8480
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs2
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         9058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+1.6935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                6850
_reflns_number_total             9058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303196a.txt
_cod_data_source_block           2
_cod_original_cell_volume        3995.8(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7012978