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_7012979
_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            'C29 H45 N4 P V'
_chemical_formula_weight         531.60
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 93.55(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.740(3)
_cell_length_b                   14.466(3)
_cell_length_c                   15.247(3)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.5
_cell_measurement_theta_min      3.5
_cell_volume                     2804.6(10)
_computing_cell_refinement       'Bruker AXS SAINT (V. 6.31a, Bruker 2002)'
_computing_data_collection       'Proteum (Version 1.35)'
_computing_data_reduction        'Bruker AXS SAINT (V. 6.31a, Bruker 2002)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean '5.602 pixels/mm'
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker three circle diffractometer'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  'mirror system'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17902
_diffrn_reflns_theta_full        59.67
_diffrn_reflns_theta_max         59.67
_diffrn_reflns_theta_min         3.48
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.667
_exptl_absorpt_correction_T_max  0.7106
_exptl_absorpt_correction_T_min  0.5275
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.503(3)
_refine_ls_extinction_coef       0.0121(3)
_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   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         7400
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.3970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                7386
_reflns_number_total             7400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303196a.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7012979