#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:57:49 +0100 (vie 25 de mar de 2016) $
#$Revision: 179820 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/16/7011686.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_7011686
loop_
_publ_author_name
'Maurya, Mannar R.'
'Khurana, Shilpa'
'Zhang, Wenjian'
'Rehder, Dieter'
_publ_section_title
;
 Biomimetic oxo-, dioxo- and oxo-peroxo-hydrazonato-vanadium(iv/v)
 complexes
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3015
_journal_paper_doi               10.1039/b202852m
_journal_year                    2002
_chemical_formula_sum            'C14 H12 N3 O3 V'
_chemical_formula_weight         321.21
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 119.7930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.2827(15)
_cell_length_b                   12.6396(12)
_cell_length_c                   14.7731(14)
_cell_measurement_reflns_used    4511
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.050
_cell_measurement_theta_min      2.161
_cell_volume                     2638.5(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15407
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.765980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Sadabs'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       nadel
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0767P)²+1.0418P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                2571
_reflns_number_total             3097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202852m.txt
_cod_data_source_block           2vbhz
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi_scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7011686
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.57183(3) 0.27996(3) 0.52758(3) 0.02176(15) Uani 1 1 d . . .
O1 O 0.58966(13) 0.15835(14) 0.56621(15) 0.0342(4) Uani 1 1 d . . .
O2 O 0.58882(13) 0.29497(15) 0.42933(14) 0.0331(4) Uani 1 1 d . . .
O3 O 0.43453(11) 0.29462(13) 0.46272(13) 0.0249(4) Uani 1 1 d . . .
N1 N 0.70558(13) 0.33673(16) 0.64190(15) 0.0218(4) Uani 1 1 d . . .
N2 N 0.54754(13) 0.40342(15) 0.60691(14) 0.0204(4) Uani 1 1 d . . .
N3 N 0.45502(13) 0.42868(16) 0.57728(15) 0.0230(4) Uani 1 1 d . . .
C1 C 0.78689(18) 0.2949(2) 0.6571(2) 0.0272(5) Uani 1 1 d . . .
H1A H 0.7847 0.2394 0.6126 0.033 Uiso 1 1 calc R . .
C2 C 0.87348(17) 0.3293(2) 0.7349(2) 0.0325(6) Uani 1 1 d . . .
H2A H 0.9299 0.2965 0.7450 0.039 Uiso 1 1 calc R . .
C3 C 0.87778(17) 0.4116(2) 0.7983(2) 0.0313(6) Uani 1 1 d . . .
H3A H 0.9371 0.4361 0.8525 0.038 Uiso 1 1 calc R . .
C4 C 0.79432(17) 0.4579(2) 0.78154(19) 0.0262(5) Uani 1 1 d . . .
H4A H 0.7956 0.5160 0.8231 0.031 Uiso 1 1 calc R . .
C5 C 0.70910(16) 0.41842(18) 0.70348(17) 0.0218(5) Uani 1 1 d . . .
C6 C 0.61598(16) 0.45671(18) 0.68053(18) 0.0212(5) Uani 1 1 d . . .
C7 C 0.60276(17) 0.5468(2) 0.7365(2) 0.0284(5) Uani 1 1 d . . .
H7A H 0.5350 0.5591 0.7087 0.043 Uiso 1 1 calc R . .
H7B H 0.6318 0.6105 0.7267 0.043 Uiso 1 1 calc R . .
H7C H 0.6328 0.5303 0.8110 0.043 Uiso 1 1 calc R . .
C8 C 0.40104(16) 0.36526(18) 0.49978(17) 0.0208(5) Uani 1 1 d . . .
C9 C 0.29743(15) 0.37410(18) 0.45314(17) 0.0208(5) Uani 1 1 d . . .
C10 C 0.25775(17) 0.45637(19) 0.48216(18) 0.0246(5) Uani 1 1 d . . .
H10A H 0.2972 0.5102 0.5281 0.030 Uiso 1 1 calc R . .
C11 C 0.16140(17) 0.4594(2) 0.44417(19) 0.0289(6) Uani 1 1 d . . .
H11A H 0.1346 0.5153 0.4641 0.035 Uiso 1 1 calc R . .
C12 C 0.10358(17) 0.3812(2) 0.37710(19) 0.0293(6) Uani 1 1 d . . .
H12A H 0.0375 0.3823 0.3529 0.035 Uiso 1 1 calc R . .
C13 C 0.14175(18) 0.3015(2) 0.3452(2) 0.0295(6) Uani 1 1 d . . .
H13A H 0.1016 0.2494 0.2973 0.035 Uiso 1 1 calc R . .
C14 C 0.23897(18) 0.29769(19) 0.38328(19) 0.0253(5) Uani 1 1 d . . .
H14A H 0.2652 0.2429 0.3615 0.030 Uiso 1 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 O2 110.35(10) . . ?
O1 V1 O3 102.97(9) . . ?
O2 V1 O3 102.29(8) . . ?
O1 V1 N2 124.03(9) . . ?
O2 V1 N2 125.17(9) . . ?
O3 V1 N2 73.56(7) . . ?
O1 V1 N1 96.19(9) . . ?
O2 V1 N1 96.29(9) . . ?
O3 V1 N1 146.51(7) . . ?
N2 V1 N1 72.96(7) . . ?
C8 O3 V1 118.39(15) . . ?
C1 N1 C5 118.7(2) . . ?
C1 N1 V1 122.81(17) . . ?
C5 N1 V1 118.54(15) . . ?
C6 N2 N3 119.62(19) . . ?
C6 N2 V1 122.19(15) . . ?
N3 N2 V1 118.18(14) . . ?
C8 N3 N2 106.70(18) . . ?
N1 C1 C2 122.3(2) . . ?
C1 C2 C3 119.5(2) . . ?
C2 C3 C4 119.0(2) . . ?
C5 C4 C3 119.0(2) . . ?
N1 C5 C4 121.6(2) . . ?
N1 C5 C6 113.7(2) . . ?
C4 C5 C6 124.7(2) . . ?
N2 C6 C5 112.5(2) . . ?
N2 C6 C7 124.4(2) . . ?
C5 C6 C7 123.1(2) . . ?
O3 C8 N3 123.1(2) . . ?
O3 C8 C9 118.5(2) . . ?
N3 C8 C9 118.4(2) . . ?
C14 C9 C10 119.6(2) . . ?
C14 C9 C8 119.8(2) . . ?
C10 C9 C8 120.5(2) . . ?
C11 C10 C9 120.1(2) . . ?
C10 C11 C12 120.2(2) . . ?
C13 C12 C11 120.2(2) . . ?
C12 C13 C14 120.0(2) . . ?
C9 C14 C13 119.9(2) . . ?
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 1.6150(19) . ?
V1 O2 1.6181(18) . ?
V1 O3 1.9548(17) . ?
V1 N2 2.1037(19) . ?
V1 N1 2.111(2) . ?
O3 C8 1.300(3) . ?
N1 C1 1.337(3) . ?
N1 C5 1.358(3) . ?
N2 C6 1.294(3) . ?
N2 N3 1.381(3) . ?
N3 C8 1.314(3) . ?
C1 C2 1.374(4) . ?
C2 C3 1.377(4) . ?
C3 C4 1.385(4) . ?
C4 C5 1.384(3) . ?
C5 C6 1.462(3) . ?
C6 C7 1.485(3) . ?
C8 C9 1.476(3) . ?
C9 C14 1.388(3) . ?
C9 C10 1.399(3) . ?
C10 C11 1.379(3) . ?
C11 C12 1.385(4) . ?
C12 C13 1.384(4) . ?
C13 C14 1.393(3) . ?
