Crystal structure of tris(<i>N</i>-methylsalicylaldiminato-κ^2^<i>N</i>,<i>O</i>)vanadium(III)
Hilbert, Jessica; Kabus, Sven; Näther, Christian; Bensch, Wolfgang; Acta Crystallographica Section E 71 (2015) m225–; doi:10.1107/S2056989015021453

data_2241330
_publ_section_title
;
 Crystal structure of
 tris(<i>N</i>-methylsalicylaldiminato-\k^2^<i>N</i>,<i>O</i>)vanadium(III)
;
_journal_coeditor_code           TK5408
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m225
_journal_paper_doi               10.1107/S2056989015021453
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[V (C8 H8 N O)3]'
_chemical_formula_moiety         'C24 H24 N3 O3 V'
_chemical_formula_sum            'C24 H24 N3 O3 V'
_chemical_formula_weight         453.40
_chemical_name_systematic
;
Tris(<i>N</i>-methylsalicylaldiminato-\k^2^<i>N</i>,<i>O</i>)vanadium(III)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 103.265(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7414(3)
_cell_length_b                   26.0018(7)
_cell_length_c                   11.1004(4)
_cell_measurement_reflns_used    18648
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.000
_cell_measurement_theta_min      1.566
_cell_volume                     2174.79(13)
_computing_cell_refinement
;
X-AREA (Stoe, 2008)
;
_computing_data_collection
;
X-AREA (Stoe, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe, 2008)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       \f-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18648
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.566
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-SHAPE and X-RED32; Stoe, 2008)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.416
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.6659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                4054
_reflns_number_total             4741
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tk5408sup1.cif
_cod_data_source_block           I
_cod_database_code               2241330
_cod_database_fobs_code          2241330
_shelx_hkl_checksum              42409
_shelx_res_checksum              43123
_shelxl_version_number           2.014