#------------------------------------------------------------------------------
#$Date: 2016-02-21 01:03:34 +0100 (dom 21 de feb de 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/42/2234229.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2234229
loop_
_publ_author_name
'Sun, Xin-Zhi'
_publ_section_title
;
 {2-[(2-Aminocyclohexyl)iminomethyl]phenolato}dioxidovanadium(V)
;
_journal_coeditor_code           HB6676
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m476
_journal_paper_doi               10.1107/S1600536812011592
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[V (C13 H17 N2 O) O2]'
_chemical_formula_moiety         'C13 H17 N2 O3 V'
_chemical_formula_sum            'C13 H17 N2 O3 V'
_chemical_formula_weight         300.23
_chemical_name_systematic
;
{2-[(2-Aminocyclohexyl)iminomethyl]phenolato}dioxidovanadium(V)
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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            16
_cell_length_a                   19.120(9)
_cell_length_b                   19.120(9)
_cell_length_c                   15.421(3)
_cell_measurement_reflns_used    1125
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      2.7
_cell_volume                     5638(4)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1717
_diffrn_reflns_av_sigmaI/netI    0.1120
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19404
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         1.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.8713
_exptl_absorpt_correction_T_min  0.8540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1798
_refine_ls_R_factor_gt           0.0992
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0708P)²+16.0234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.2025
_reflns_number_gt                1487
_reflns_number_total             2537
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb6676.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2234229
_cod_database_fobs_code          2234229
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
V V1 0.04762(6) 0.08630(6) 0.66104(7) 0.0417(4) Uani d . 1 1
N N1 0.1074(3) 0.0188(3) 0.5792(4) 0.0574(17) Uani d . 1 1
N N2 0.0524(3) 0.1379(3) 0.5413(3) 0.0424(14) Uani d . 1 1
H H2A 0.0122 0.1616 0.5337 0.051 Uiso calc R 1 1
H H2B 0.0872 0.1695 0.5436 0.051 Uiso calc R 1 1
O O1 0.0854(3) 0.0299(3) 0.7510(3) 0.0589(14) Uani d . 1 1
O O2 -0.0330(2) 0.0631(2) 0.6543(3) 0.0581(14) Uani d . 1 1
O O3 0.0526(3) 0.1602(2) 0.7122(3) 0.0596(14) Uani d . 1 1
C C1 0.1142(4) -0.0770(4) 0.6803(5) 0.062(2) Uani d . 1 1
C C2 0.0962(4) -0.0379(4) 0.7536(5) 0.057(2) Uani d . 1 1
C C3 0.0907(5) -0.0727(5) 0.8315(6) 0.078(3) Uani d . 1 1
H H3 0.0788 -0.0477 0.8811 0.093 Uiso calc R 1 1
C C4 0.1022(6) -0.1422(6) 0.8374(7) 0.109(4) Uani d . 1 1
H H4 0.0984 -0.1643 0.8909 0.130 Uiso calc R 1 1
C C5 0.1195(6) -0.1808(5) 0.7646(8) 0.111(4) Uani d . 1 1
H H5 0.1271 -0.2287 0.7692 0.133 Uiso calc R 1 1
C C6 0.1251(5) -0.1488(5) 0.6875(7) 0.094(3) Uani d . 1 1
H H6 0.1365 -0.1748 0.6384 0.112 Uiso calc R 1 1
C C7 0.1238(4) -0.0435(5) 0.5984(5) 0.073(3) Uani d . 1 1
H H7 0.1441 -0.0701 0.5546 0.087 Uiso calc R 1 1
C C8 0.1201(5) 0.0398(6) 0.4903(6) 0.094(3) Uani d . 1 1
H H8 0.1107 -0.0015 0.4546 0.112 Uiso calc R 1 1
C C9 0.0635(4) 0.0936(4) 0.4666(5) 0.063(2) Uani d . 1 1
H H9 0.0202 0.0670 0.4586 0.075 Uiso calc R 1 1
C C10 0.0774(7) 0.1306(6) 0.3813(6) 0.110(4) Uani d . 1 1
H H10A 0.0630 0.0998 0.3346 0.132 Uiso calc R 1 1
H H10B 0.0478 0.1717 0.3788 0.132 Uiso calc R 1 1
C C11 0.1431(8) 0.1505(8) 0.3664(10) 0.167(7) Uani d . 1 1
H H11A 0.1534 0.1903 0.4032 0.200 Uiso calc R 1 1
H H11B 0.1465 0.1661 0.3067 0.200 Uiso calc R 1 1
C C12 0.1999(6) 0.0933(7) 0.3823(7) 0.115(4) Uani d . 1 1
H H12A 0.1972 0.0579 0.3373 0.137 Uiso calc R 1 1
H H12B 0.2461 0.1141 0.3804 0.137 Uiso calc R 1 1
C C13 0.1873(5) 0.0597(7) 0.4717(8) 0.134(5) Uani d . 1 1
H H13A 0.2170 0.0187 0.4764 0.161 Uiso calc R 1 1
H H13B 0.2023 0.0926 0.5158 0.161 Uiso calc R 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O2 V1 O3 109.2(3)
O2 V1 O1 104.8(2)
O3 V1 O1 96.7(2)
O2 V1 N2 96.6(2)
O3 V1 N2 90.9(2)
O1 V1 N2 153.4(2)
O2 V1 N1 108.0(2)
O3 V1 N1 141.5(3)
O1 V1 N1 83.4(2)
N2 V1 N1 75.0(2)
C7 N1 C8 116.1(7)
C7 N1 V1 124.2(5)
C8 N1 V1 118.8(5)
C9 N2 V1 115.6(4)
C9 N2 H2A 108.4
V1 N2 H2A 108.4
C9 N2 H2B 108.4
V1 N2 H2B 108.4
H2A N2 H2B 107.4
C2 O1 V1 129.9(5)
C6 C1 C2 119.9(8)
C6 C1 C7 119.5(8)
C2 C1 C7 120.5(7)
O1 C2 C3 119.4(7)
O1 C2 C1 122.8(7)
C3 C2 C1 117.9(8)
C4 C3 C2 121.4(9)
C4 C3 H3 119.3
C2 C3 H3 119.3
C3 C4 C5 120.7(10)
C3 C4 H4 119.7
C5 C4 H4 119.7
C6 C5 C4 119.7(9)
C6 C5 H5 120.1
C4 C5 H5 120.1
C5 C6 C1 120.4(9)
C5 C6 H6 119.8
C1 C6 H6 119.8
N1 C7 C1 126.6(7)
N1 C7 H7 116.7
C1 C7 H7 116.7
C13 C8 N1 115.6(9)
C13 C8 C9 115.2(9)
N1 C8 C9 107.0(6)
C13 C8 H8 106.1
N1 C8 H8 106.1
C9 C8 H8 106.1
N2 C9 C10 116.3(7)
N2 C9 C8 107.8(6)
C10 C9 C8 113.3(7)
N2 C9 H9 106.2
C10 C9 H9 106.2
C8 C9 H9 106.2
C11 C10 C9 116.6(11)
C11 C10 H10A 108.1
C9 C10 H10A 108.1
C11 C10 H10B 108.1
C9 C10 H10B 108.1
H10A C10 H10B 107.3
C10 C11 C12 115.4(11)
C10 C11 H11A 108.4
C12 C11 H11A 108.4
C10 C11 H11B 108.4
C12 C11 H11B 108.4
H11A C11 H11B 107.5
C13 C12 C11 108.9(10)
C13 C12 H12A 109.9
C11 C12 H12A 109.9
C13 C12 H12B 109.9
C11 C12 H12B 109.9
H12A C12 H12B 108.3
C8 C13 C12 116.7(9)
C8 C13 H13A 108.1
C12 C13 H13A 108.1
C8 C13 H13B 108.1
C12 C13 H13B 108.1
H13A C13 H13B 107.3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
V1 O2 1.607(5) y
V1 O3 1.621(5) y
V1 O1 1.900(5) y
V1 N2 2.095(5) y
V1 N1 2.137(6) y
N1 C7 1.267(9) ?
N1 C8 1.448(10) ?
N2 C9 1.447(8) ?
N2 H2A 0.9000 ?
N2 H2B 0.9000 ?
O1 C2 1.314(8) ?
C1 C6 1.394(11) ?
C1 C2 1.398(10) ?
C1 C7 1.428(11) ?
C2 C3 1.377(11) ?
C3 C4 1.350(12) ?
C3 H3 0.9300 ?
C4 C5 1.383(13) ?
C4 H4 0.9300 ?
C5 C6 1.342(13) ?
C5 H5 0.9300 ?
C6 H6 0.9300 ?
C7 H7 0.9300 ?
C8 C13 1.370(12) ?
C8 C9 1.536(11) ?
C8 H8 0.9800 ?
C9 C10 1.517(11) ?
C9 H9 0.9800 ?
C10 C11 1.332(15) ?
C10 H10A 0.9700 ?
C10 H10B 0.9700 ?
C11 C12 1.561(17) ?
C11 H11A 0.9700 ?
C11 H11B 0.9700 ?
C12 C13 1.541(13) ?
C12 H12A 0.9700 ?
C12 H12B 0.9700 ?
C13 H13A 0.9700 ?
C13 H13B 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N2 H2B O2 12_667 0.90 2.26 3.099(7) 155
N2 H2B O3 12_667 0.90 2.55 3.229(7) 133
N2 H2A O3 14_556 0.90 2.07 2.948(7) 166
