Vanadium(IV) and Vanadium(V) Complexes of Salicyladimine Ligands
Kathryn I. Smith; Londa L. Borer; Marilyn M. Olmstead; Inorganic Chemistry 42 (2003) 7410–7415; doi:10.1021/ic034640p

data_4312495
_publ_section_title
;
 Vanadium(IV) and Vanadium(V) Complexes of Salicyladimine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7410
_journal_page_last               7415
_journal_paper_doi               10.1021/ic034640p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C19 H22 N2 O7 V, 2(C2 H4 Cl2)'
_chemical_formula_sum            'C23 H30 Cl4 N2 O7 V'
_chemical_formula_weight         639.23
_chemical_name_common            VO(H~2~O)(C~19~H~20~N~2~O~5~)^.^2dichloroethane
_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                66.003(6)
_cell_angle_beta                 74.842(7)
_cell_angle_gamma                88.338(7)
_cell_formula_units_Z            2
_cell_length_a                   10.6789(10)
_cell_length_b                   11.7717(8)
_cell_length_c                   12.6972(12)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.5
_cell_measurement_theta_min      4.0
_cell_volume                     1402.0(2)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL Plus, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       2\q-\w
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_source         'Siemens rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3536
_diffrn_reflns_theta_full        55.06
_diffrn_reflns_theta_max         55.06
_diffrn_reflns_theta_min         3.96
_diffrn_standards_decay_%        4.2
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.850
_exptl_absorpt_correction_T_max  0.4936
_exptl_absorpt_correction_T_min  0.3412
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;XABS2: an empirical absorption correction program. Parkin, S.; Moezzi,
   B.; Hope, H. J. Appl. Cryst. 1995, 28, 53-56.
;
_exptl_crystal_colour            'green-brown dichroic'
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.00013(13)
_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   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+1.6415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                3086
_reflns_number_total             3531
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic034640p_s1_2.cif
_cod_data_source_block           mn846
_cod_database_code               4312495