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_4312494
_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         'C10 H13 N2 O4 V, 2(H2 O)'
_chemical_formula_sum            'C10 H17 N2 O6 V'
_chemical_formula_weight         312.20
_chemical_name_common            VO~2~(C~10~H~13~N~2~O~2~)^.^2H~2~O
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.9004(5)
_cell_length_b                   26.628(2)
_cell_length_c                   7.2583(6)
_cell_measurement_reflns_used    3491
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.6
_cell_measurement_theta_min      2.9
_cell_volume                     1333.67(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5.03, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12137
_diffrn_reflns_theta_full        31.46
_diffrn_reflns_theta_max         31.46
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        <0.1
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  0.9626
_exptl_absorpt_correction_T_min  0.8080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.0'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.40(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4148
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.5643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                3549
_reflns_number_total             4148
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic034640p_s1_1.cif
_cod_data_source_block           djn170
_cod_original_cell_volume        1333.65(18)
_cod_database_code               4312494