Crystal structure of {2,2'-[ethylenebis(nitrilomethanylylidene)]diphenolato-κ^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>'}oxidovanadium(IV) methanol monosolvate
Hsuan, Rachel E.; Hughes, Jemma E.; Miller, Thomas H.; Shaikh, Nabila; Cunningham, Phoebe H. M.; O'Connor, Alice E.; Tidey, Jeremiah P.; Blake, Alexander J.; Acta Crystallographica Section E 70 (2014) m380–m381; doi:10.1107/S1600536814023332

data_2240132
_publ_section_title
;
 Crystal structure of
 {2,2'-[ethylenebis(nitrilomethanylylidene)]diphenolato-\k^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>'}oxidovanadium(IV)
 methanol monosolvate
;
_journal_coeditor_code           GG2143
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m380
_journal_page_last               m381
_journal_paper_doi               10.1107/S1600536814023332
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[V (C16 H14 N2 O2) O], C H4 O'
_chemical_formula_moiety         'C16 H14 N2 O3 V, C H4 O'
_chemical_formula_sum            'C17 H18 N2 O4 V'
_chemical_formula_weight         365.27
_chemical_name_systematic
;{2,2'-[Ethylenebis(nitrilomethanylylidene)]diphenolato-\k^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>'}oxidovanadium(IV) methanol
monosolvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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
_audit_creation_method
;
OLEX2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.9597(4)
_cell_length_b                   8.8616(2)
_cell_length_c                   28.5426(7)
_cell_measurement_reflns_used    3840
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.28
_cell_measurement_theta_min      5.20
_cell_volume                     3277.94(15)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2013)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3271
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type
'Agilent GV1000 diffractometer with an Atlas CCD detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            7416
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         74.358
_diffrn_reflns_theta_min         5.226
_exptl_absorpt_coefficient_mu    5.272
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.29
_refine_ls_abs_structure_details
;
Flack (1983), 1395 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.066(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         4634
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.065P)^2^+1.252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.100
_refine_ls_wR_factor_ref         0.105
_reflns_number_gt                4350
_reflns_number_total             4634
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg2143sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        3277.92(15)
_cod_database_code               2240132
_cod_database_fobs_code          2240132
_shelx_hkl_checksum              66642
_shelx_res_checksum              93246
_shelxl_version_number           2014-3