#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:41:08 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179984 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/78/7027825.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7027825
loop_
_publ_author_name
'Choudhary, Nosheen F.'
'Connelly, Neil G.'
'Hitchcock, Peter B.'
'Leigh, G. Jeffery'
_publ_section_title
;
 New compounds of tetradentate Schiff bases with vanadium(IV) and
 vanadium(V) †
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4437
_journal_paper_doi               10.1039/a908337e
_journal_year                    1999
_chemical_formula_sum            'C21 H24 N2 O5 V'
_chemical_formula_weight         435.36
_chemical_name_common            '[(salen????)VO]'
_chemical_name_systematic
; 
  ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 107.35(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.682(3)
_cell_length_b                   17.520(3)
_cell_length_c                   13.600(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     1974.6(9)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       ω--2θ
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3703
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.087
_refine_ls_goodness_of_fit_obs   1.113
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_restrained_S_obs      1.113
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_obs          0.0683
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1290P)²+1.3635P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2026
_refine_ls_wR_factor_obs         0.1809
_reflns_number_observed          2757
_reflns_number_total             3470
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            908337esup1.cif
_cod_data_source_block           jan1497
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1290P)^2^+1.3635P] 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^)+(0.1290P)^2^+1.3635P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027825
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, -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
V V 0.19369(8) 0.81161(4) 0.42690(5) 0.0269(3) Uani 1 d .
O1 O 0.0615(4) 0.7655(2) 0.4611(2) 0.0474(8) Uani 1 d .
O2 O 0.3301(3) 0.8608(2) 0.5510(2) 0.0313(6) Uani 1 d .
O3 O 0.3816(3) 0.7485(2) 0.4335(2) 0.0316(7) Uani 1 d .
O4 O 0.5244(4) 0.8897(2) 0.7381(2) 0.0427(8) Uani 1 d .
O5 O 0.6657(4) 0.6799(2) 0.4961(2) 0.0433(8) Uani 1 d .
N1 N 0.0906(4) 0.9184(2) 0.3874(3) 0.0330(8) Uani 1 d .
N2 N 0.1170(4) 0.7879(2) 0.2695(3) 0.0306(8) Uani 1 d .
C1 C 0.3637(5) 0.9318(2) 0.5759(3) 0.0267(8) Uani 1 d .
C2 C 0.4731(5) 0.9504(2) 0.6743(3) 0.0299(9) Uani 1 d .
C3 C 0.5214(5) 1.0239(2) 0.6987(3) 0.0348(10) Uani 1 d .
H3 H 0.5962(5) 1.0344(2) 0.7621(3) 0.042 Uiso 1 calc R
C4 C 0.4600(6) 1.0838(3) 0.6299(4) 0.0403(10) Uani 1 d .
H4 H 0.4958(6) 1.1335(3) 0.6466(4) 0.048 Uiso 1 calc R
C5 C 0.3472(6) 1.0684(2) 0.5379(3) 0.0391(10) Uani 1 d .
H5 H 0.3047(6) 1.1081(2) 0.4926(3) 0.047 Uiso 1 calc R
C6 C 0.2948(5) 0.9937(2) 0.5112(3) 0.0312(9) Uani 1 d .
C7 C 0.1555(5) 0.9822(3) 0.4242(3) 0.0360(10) Uani 1 d .
H7 H 0.1063(5) 1.0260(3) 0.3904(3) 0.043 Uiso 1 calc R
C8 C -0.0737(5) 0.9230(3) 0.3131(3) 0.0442(12) Uani 1 d .
H8A H -0.1067(5) 0.9761(3) 0.3057(3) 0.053 Uiso 1 calc R
H8B H -0.1477(5) 0.8960(3) 0.3420(3) 0.053 Uiso 1 calc R
C9 C -0.0905(5) 0.8905(3) 0.2057(3) 0.0391(11) Uani 1 d .
C10 C -0.0524(6) 0.8058(3) 0.2124(3) 0.0412(11) Uani 1 d .
H10A H -0.1226(6) 0.7803(3) 0.2457(3) 0.049 Uiso 1 calc R
H10B H -0.0762(6) 0.7855(3) 0.1432(3) 0.049 Uiso 1 calc R
C11 C 0.1986(5) 0.7535(2) 0.2177(3) 0.0339(10) Uani 1 d .
H11 H 0.1466(5) 0.7461(2) 0.1480(3) 0.041 Uiso 1 calc R
C12 C 0.3608(5) 0.7254(2) 0.2555(3) 0.0307(9) Uani 1 d .
C13 C 0.4358(6) 0.6995(2) 0.1840(3) 0.0389(10) Uani 1 d .
H13 H 0.3812(6) 0.7030(2) 0.1140(3) 0.047 Uiso 1 calc R
C14 C 0.5864(6) 0.6693(3) 0.2147(4) 0.0438(11) Uani 1 d .
H14 H 0.6360(6) 0.6538(3) 0.1661(4) 0.053 Uiso 1 calc R
C15 C 0.6672(6) 0.6615(3) 0.3206(4) 0.0416(11) Uani 1 d .
H15 H 0.7695(6) 0.6398(3) 0.3419(4) 0.050 Uiso 1 calc R
C16 C 0.5963(5) 0.6858(2) 0.3923(3) 0.0315(9) Uani 1 d .
C17 C 0.4414(5) 0.7208(2) 0.3626(3) 0.0272(8) Uani 1 d .
C18 C 0.6202(7) 0.9063(3) 0.8400(4) 0.0517(14) Uani 1 d .
H18A H 0.6494(7) 0.8596(3) 0.8779(4) 0.078 Uiso 1 calc R
H18B H 0.5600(7) 0.9379(3) 0.8730(4) 0.078 Uiso 1 calc R
H18C H 0.7161(7) 0.9327(3) 0.8380(4) 0.078 Uiso 1 calc R
C19 C -0.2700(6) 0.8973(4) 0.1430(4) 0.061(2) Uani 1 d .
H19A H -0.3345(6) 0.8690(4) 0.1767(4) 0.091 Uiso 1 calc R
H19B H -0.2857(6) 0.8771(4) 0.0751(4) 0.091 Uiso 1 calc R
H19C H -0.3016(6) 0.9500(4) 0.1382(4) 0.091 Uiso 1 calc R
C20 C 0.0116(6) 0.9348(3) 0.1531(4) 0.0539(13) Uani 1 d .
H20A H -0.0168(6) 0.9879(3) 0.1507(4) 0.081 Uiso 1 calc R
H20B H -0.0069(6) 0.9160(3) 0.0842(4) 0.081 Uiso 1 calc R
H20C H 0.1235(6) 0.9288(3) 0.1909(4) 0.081 Uiso 1 calc R
C21 C 0.8109(6) 0.6379(3) 0.5301(4) 0.0471(12) Uani 1 d .
H21A H 0.8481(6) 0.6377(3) 0.6040(4) 0.071 Uiso 1 calc R
H21B H 0.8910(6) 0.6610(3) 0.5040(4) 0.071 Uiso 1 calc R
H21C H 0.7921(6) 0.5864(3) 0.5053(4) 0.071 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
O1 V O2 106.11(15)
O1 V O3 111.5(2)
O2 V O3 85.78(12)
O1 V N1 104.0(2)
O2 V N1 85.96(13)
O3 V N1 144.44(14)
O1 V N2 99.4(2)
O2 V N2 154.46(14)
O3 V N2 86.61(13)
N1 V N2 86.17(13)
C1 O2 V 132.8(2)
C17 O3 V 133.0(2)
C2 O4 C18 116.6(3)
C16 O5 C21 117.0(4)
C7 N1 C8 116.0(4)
C7 N1 V 125.4(3)
C8 N1 V 118.6(3)
C11 N2 C10 115.8(4)
C11 N2 V 126.5(3)
C10 N2 V 117.4(3)
O2 C1 C6 123.6(4)
O2 C1 C2 119.8(3)
C6 C1 C2 116.6(4)
O4 C2 C3 124.3(4)
O4 C2 C1 114.7(3)
C3 C2 C1 120.9(4)
C2 C3 C4 121.0(4)
C5 C4 C3 119.3(4)
C4 C5 C6 120.8(4)
C5 C6 C1 120.8(4)
C5 C6 C7 118.4(4)
C1 C6 C7 120.2(4)
N1 C7 C6 127.5(4)
N1 C8 C9 115.3(4)
C20 C9 C10 112.5(4)
C20 C9 C8 110.9(4)
C10 C9 C8 110.5(4)
C20 C9 C19 109.7(4)
C10 C9 C19 106.0(4)
C8 C9 C19 106.9(4)
N2 C10 C9 113.9(4)
N2 C11 C12 127.3(4)
C13 C12 C17 120.5(4)
C13 C12 C11 118.2(4)
C17 C12 C11 121.2(4)
C14 C13 C12 121.3(4)
C13 C14 C15 119.5(4)
C16 C15 C14 120.5(4)
O5 C16 C15 124.1(4)
O5 C16 C17 114.6(4)
C15 C16 C17 121.3(4)
O3 C17 C12 123.4(4)
O3 C17 C16 119.8(3)
C12 C17 C16 116.8(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
V O1 1.583(3)
V O2 1.950(3)
V O3 1.951(3)
V N1 2.075(4)
V N2 2.085(3)
O2 C1 1.300(5)
O3 C17 1.317(5)
O4 C2 1.362(5)
O4 C18 1.417(5)
O5 C16 1.364(5)
O5 C21 1.413(5)
N1 C7 1.284(6)
N1 C8 1.484(5)
N2 C11 1.288(5)
N2 C10 1.478(5)
C1 C6 1.413(6)
C1 C2 1.429(5)
C2 C3 1.364(6)
C3 C4 1.402(6)
C4 C5 1.366(6)
C5 C6 1.398(6)
C6 C7 1.432(6)
C8 C9 1.534(6)
C9 C20 1.511(7)
C9 C10 1.516(7)
C9 C19 1.541(6)
C11 C12 1.435(6)
C12 C13 1.397(6)
C12 C17 1.417(5)
C13 C14 1.356(7)
C14 C15 1.408(7)
C15 C16 1.367(6)
C16 C17 1.423(6)
