#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:23:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179325 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/22/4322234.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4322234
loop_
_publ_author_name
'Henk Hagen'
'Antonio Barbon'
'Ernst E. van Faassen'
'Bert T. G. Lutz'
'Jaap Boersma'
'Anthony L. Spek'
'Gerard van Koten'
_publ_contact_author_address
;
    Bijvoet Center for Biomolecular Research
    Department of Crystal and Structural Chemistry
    Utrecht University
    Padualaan 8
    3584 CH Utrecht
    The Netherlands
;
_publ_contact_author_email       spea@chem.uu.nl
_publ_contact_author_fax         '+31 30 2533940'
_publ_contact_author_name        '   Dr. A.L. Spek'
_publ_contact_author_phone       '+31 30 2532538'
_publ_section_title
;
 Synthesis and Characterization of O,N-Chelated Vanadium(IV) Oxo Phenolate
 Complexes: Electronic Effect of Meta and Para Substituents on the
 Vanadium Center
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4079
_journal_page_last               4086
_journal_paper_doi               10.1021/ic9901564
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         'C18 H24 N2 O3 V'
_chemical_formula_sum            'C18 H24 N2 O3 V'
_chemical_formula_weight         367.34
_chemical_name_systematic
;                                                                               
 ?                                                                              
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.4321(7)
_cell_length_b                   14.1919(14)
_cell_length_c                   26.5484(14)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.5
_cell_volume                     3553.8(5)
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    DIRDIF
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       CAD4T
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_sigmaI/netI    0.1260
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            9417
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.973
_refine_ls_goodness_of_fit_obs   1.115
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_restrained_S_obs      1.115
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_obs          0.0565
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0300P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1049
_refine_ls_wR_factor_obs         0.0829
_reflns_number_observed          2037
_reflns_number_total             4071
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            ic9901564_1.cif
_cod_data_source_block           s1536a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322234
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, -z'
'-x, y-1/2, -z-1/2'
'x-1/2, y, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
V1 V 0.20661(6) 0.19393(4) 0.13930(2) 0.02180(15) Uani 1 d . .
O1 O 0.2783(3) 0.14030(15) 0.18576(9) 0.0279(6) Uani 1 d . .
O2 O 0.1916(3) 0.12381(16) 0.07872(9) 0.0305(6) Uani 1 d . .
O3 O 0.1464(2) 0.31733(15) 0.15415(8) 0.0240(6) Uani 1 d . .
N1 N 0.3959(3) 0.25821(19) 0.10951(11) 0.0224(7) Uani 1 d . .
N2 N -0.0072(3) 0.14890(19) 0.15303(10) 0.0233(7) Uani 1 d . .
C1 C 0.2755(4) 0.1139(2) 0.03825(13) 0.0267(9) Uani 1 d . .
C2 C 0.4162(4) 0.1442(2) 0.03756(13) 0.0264(9) Uani 1 d . .
C3 C 0.4951(4) 0.1329(3) -0.00561(13) 0.0345(10) Uani 1 d . .
H3 H 0.5882 0.1544 -0.0060 0.041 Uiso 1 calc R .
C4 C 0.4414(5) 0.0908(3) -0.04847(15) 0.0420(11) Uani 1 d . .
H4 H 0.4975 0.0829 -0.0770 0.050 Uiso 1 calc R .
C5 C 0.3018(5) 0.0606(3) -0.04796(14) 0.0392(11) Uani 1 d . .
H5 H 0.2628 0.0330 -0.0765 0.047 Uiso 1 calc R .
C6 C 0.2204(4) 0.0715(2) -0.00521(13) 0.0345(10) Uani 1 d . .
H6 H 0.1272 0.0502 -0.0052 0.041 Uiso 1 calc R .
C7 C 0.4829(3) 0.1842(3) 0.08411(13) 0.0284(9) Uani 1 d . .
H7A H 0.4997 0.1333 0.1078 0.034 Uiso 1 calc R .
H7B H 0.5742 0.2110 0.0753 0.034 Uiso 1 calc R .
C8 C 0.4797(4) 0.2977(3) 0.15193(12) 0.0317(10) Uani 1 d . .
H8A H 0.5627 0.3285 0.1390 0.048 Uiso 1 calc R .
H8B H 0.5077 0.2477 0.1742 0.048 Uiso 1 calc R .
H8C H 0.4230 0.3424 0.1701 0.048 Uiso 1 calc R .
C9 C 0.3660(4) 0.3355(2) 0.07331(13) 0.0311(10) Uani 1 d . .
H9A H 0.3117 0.3837 0.0898 0.047 Uiso 1 calc R .
H9B H 0.3133 0.3111 0.0453 0.047 Uiso 1 calc R .
H9C H 0.4538 0.3616 0.0615 0.047 Uiso 1 calc R .
C10 C 0.0325(4) 0.3530(2) 0.17821(12) 0.0219(8) Uani 1 d . .
C11 C -0.0700(4) 0.2953(2) 0.20118(12) 0.0218(8) Uani 1 d . .
C12 C -0.1847(4) 0.3376(2) 0.22534(12) 0.0282(9) Uani 1 d . .
H12 H -0.2538 0.2998 0.2401 0.034 Uiso 1 calc R .
C13 C -0.1980(4) 0.4341(3) 0.22783(12) 0.0304(9) Uani 1 d . .
H13 H -0.2743 0.4611 0.2447 0.036 Uiso 1 calc R .
C14 C -0.0974(4) 0.4902(3) 0.20512(13) 0.0277(9) Uani 1 d . .
H14 H -0.1068 0.5554 0.2062 0.033 Uiso 1 calc R .
C15 C 0.0173(4) 0.4505(2) 0.18074(12) 0.0244(9) Uani 1 d . .
H15 H 0.0850 0.4892 0.1659 0.029 Uiso 1 calc R .
C16 C -0.0558(4) 0.1899(2) 0.20168(12) 0.0266(8) Uani 1 d . .
H16A H 0.0109 0.1723 0.2278 0.032 Uiso 1 calc R .
H16B H -0.1469 0.1626 0.2103 0.032 Uiso 1 calc R .
C17 C -0.0082(4) 0.0447(2) 0.15709(14) 0.0320(10) Uani 1 d . .
H17A H 0.0513 0.0256 0.1846 0.048 Uiso 1 calc R .
H17B H 0.0267 0.0178 0.1263 0.048 Uiso 1 calc R .
H17C H -0.1034 0.0233 0.1630 0.048 Uiso 1 calc R .
C18 C -0.1061(4) 0.1768(2) 0.11205(13) 0.0307(9) Uani 1 d . .
H18A H -0.2000 0.1552 0.1200 0.046 Uiso 1 calc R .
H18B H -0.0756 0.1490 0.0809 0.046 Uiso 1 calc R .
H18C H -0.1066 0.2442 0.1088 0.046 Uiso 1 calc R .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O3 114.13(11) . . ?
O1 V1 O2 115.83(11) . . ?
O3 V1 O2 130.03(11) . . ?
O1 V1 N2 97.17(11) . . ?
O3 V1 N2 87.58(10) . . ?
O2 V1 N2 85.29(11) . . ?
O1 V1 N1 97.71(12) . . ?
O3 V1 N1 86.17(10) . . ?
O2 V1 N1 88.43(11) . . ?
N2 V1 N1 165.12(11) . . ?
C1 O2 V1 133.6(2) . . ?
C10 O3 V1 133.6(2) . . ?
C9 N1 C8 108.2(3) . . ?
C9 N1 C7 109.4(3) . . ?
C8 N1 C7 108.4(3) . . ?
C9 N1 V1 113.2(2) . . ?
C8 N1 V1 108.8(2) . . ?
C7 N1 V1 108.8(2) . . ?
C17 N2 C18 108.3(3) . . ?
C17 N2 C16 109.0(3) . . ?
C18 N2 C16 109.7(3) . . ?
C17 N2 V1 108.4(2) . . ?
C18 N2 V1 112.7(2) . . ?
C16 N2 V1 108.7(2) . . ?
O2 C1 C2 122.6(3) . . ?
O2 C1 C6 119.0(3) . . ?
C2 C1 C6 118.3(3) . . ?
C3 C2 C1 119.3(4) . . ?
C3 C2 C7 120.3(3) . . ?
C1 C2 C7 120.4(3) . . ?
C2 C3 C4 122.6(4) . . ?
C3 C4 C5 118.3(4) . . ?
C6 C5 C4 120.2(4) . . ?
C5 C6 C1 121.3(4) . . ?
N1 C7 C2 114.1(3) . . ?
O3 C10 C15 118.6(3) . . ?
O3 C10 C11 122.3(3) . . ?
C15 C10 C11 119.1(3) . . ?
C12 C11 C10 118.8(3) . . ?
C12 C11 C16 119.6(3) . . ?
C10 C11 C16 121.5(3) . . ?
C13 C12 C11 121.4(4) . . ?
C12 C13 C14 119.4(4) . . ?
C13 C14 C15 120.6(3) . . ?
C14 C15 C10 120.6(3) . . ?
N2 C16 C11 114.1(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.599(2) . ?
V1 O3 1.883(2) . ?
V1 O2 1.897(2) . ?
V1 N2 2.147(3) . ?
V1 N1 2.155(3) . ?
O2 C1 1.342(4) . ?
O3 C10 1.348(4) . ?
N1 C9 1.485(4) . ?
N1 C8 1.486(4) . ?
N1 C7 1.494(4) . ?
N2 C17 1.482(4) . ?
N2 C18 1.487(4) . ?
N2 C16 1.489(4) . ?
C1 C2 1.395(5) . ?
C1 C6 1.401(4) . ?
C2 C3 1.376(4) . ?
C2 C7 1.498(5) . ?
C3 C4 1.381(5) . ?
C4 C5 1.385(5) . ?
C5 C6 1.379(5) . ?
C10 C15 1.393(4) . ?
C10 C11 1.407(5) . ?
C11 C12 1.394(4) . ?
C11 C16 1.501(4) . ?
C12 C13 1.376(4) . ?
C13 C14 1.378(5) . ?
C14 C15 1.381(4) . ?
