#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:57:49 +0100 (vie 25 de mar de 2016) $
#$Revision: 179820 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/16/7011687.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_7011687
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            'C13 H11 N4 O3 V'
_chemical_formula_weight         322.20
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 106.507(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.280(5)
_cell_length_b                   6.834(2)
_cell_length_c                   14.297(5)
_cell_measurement_reflns_used    1097
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.281
_cell_measurement_theta_min      2.924
_cell_volume                     1337.7(8)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1061
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3777
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.801392
_exptl_absorpt_correction_T_min  0.530563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Sadabs'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0782P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1442
_reflns_number_gt                957
_reflns_number_total             1299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202852m.txt
_cod_data_source_block           3vinh
_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.

'_refine_ls_hydrogen_treatment' value 'Constr' changed to
'constr' 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/m
_cod_database_code               7011687
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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 0.11748(5) 0.0000 0.19612(5) 0.0429(4) Uani 1 2 d S . .
O1 O 0.05500(17) 0.1938(4) 0.15405(17) 0.0599(8) Uani 1 1 d . . .
O2 O 0.1198(2) 0.0000 0.3339(2) 0.0652(12) Uani 1 2 d S . .
N1 N 0.2002(3) 0.0000 0.0953(3) 0.0389(9) Uani 1 2 d S . .
N2 N 0.2658(3) 0.0000 0.2775(3) 0.0469(11) Uani 1 2 d S . .
N3 N 0.2885(3) 0.0000 0.3783(3) 0.0606(13) Uani 1 2 d S . .
N4 N 0.2071(4) 0.0000 0.6996(4) 0.0842(18) Uani 1 2 d S . .
C1 C 0.1591(4) 0.0000 -0.0005(3) 0.0467(12) Uani 1 2 d S . .
H1A H 0.0914 0.0000 -0.0240 0.056 Uiso 1 2 calc SR . .
C2 C 0.2142(4) 0.0000 -0.0673(4) 0.0538(14) Uani 1 2 d S . .
H2A H 0.1835 0.0000 -0.1340 0.065 Uiso 1 2 calc SR . .
C3 C 0.3135(5) 0.0000 -0.0330(4) 0.0548(15) Uani 1 2 d S . .
H3A H 0.3515 0.0000 -0.0762 0.066 Uiso 1 2 calc SR . .
C4 C 0.3577(4) 0.0000 0.0673(4) 0.0479(13) Uani 1 2 d S . .
H4A H 0.4254 0.0000 0.0923 0.057 Uiso 1 2 calc SR . .
C5 C 0.2981(3) 0.0000 0.1294(3) 0.0406(11) Uani 1 2 d S . .
C6 C 0.3350(4) 0.0000 0.2355(4) 0.0464(13) Uani 1 2 d S . .
C7 C 0.4419(4) 0.0000 0.2888(4) 0.0675(18) Uani 1 2 d S . .
H7A H 0.4502 0.0000 0.3578 0.101 Uiso 1 2 calc SR . .
H7B H 0.4719 0.1147 0.2713 0.101 Uiso 0.50 1 calc PR . .
H7C H 0.4719 -0.1147 0.2713 0.101 Uiso 0.50 1 calc PR . .
C8 C 0.2045(4) 0.0000 0.3984(4) 0.0639(17) Uani 1 2 d S . .
C9 C 0.2068(4) 0.0000 0.5032(4) 0.0723(19) Uani 1 2 d S . .
C10 C 0.2931(4) 0.0000 0.5783(4) 0.0579(15) Uani 1 2 d S A .
H10A H 0.3530 0.0000 0.5646 0.070 Uiso 1 2 calc SR . .
C11 C 0.2890(4) 0.0000 0.6732(4) 0.0652(16) Uani 1 2 d S A .
H11A H 0.3479 0.0000 0.7224 0.078 Uiso 1 2 calc SR . .
C12 C 0.1271(6) -0.0576(11) 0.6279(5) 0.058(3) Uani 0.50 1 d P A -1
H12A H 0.0724 -0.0970 0.6462 0.069 Uiso 0.50 1 calc PR A -1
C13 C 0.1211(5) -0.0616(10) 0.5290(5) 0.054(3) Uani 0.50 1 d P A -1
H13A H 0.0648 -0.1019 0.4822 0.065 Uiso 0.50 1 calc PR A -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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O1 110.22(19) 6 . ?
O1 V1 O2 102.95(10) 6 . ?
O1 V1 O2 102.95(10) . . ?
O1 V1 N2 124.62(10) 6 . ?
O1 V1 N2 124.62(10) . . ?
O2 V1 N2 73.59(14) . . ?
O1 V1 N1 95.92(11) 6 . ?
O1 V1 N1 95.92(11) . . ?
O2 V1 N1 146.55(15) . . ?
N2 V1 N1 72.97(15) . . ?
C8 O2 V1 117.4(3) . . ?
C1 N1 C5 118.9(4) . . ?
C1 N1 V1 122.4(3) . . ?
C5 N1 V1 118.7(3) . . ?
C6 N2 N3 119.9(4) . . ?
C6 N2 V1 121.6(3) . . ?
N3 N2 V1 118.5(3) . . ?
C8 N3 N2 105.6(4) . . ?
C11 N4 C12 114.0(5) . . ?
C11 N4 C12 114.0(5) . 6 ?
C12 N4 C12 33.6(6) . 6 ?
N1 C1 C2 122.3(5) . . ?
N1 C1 H1A 118.8 . . ?
C2 C1 H1A 118.8 . . ?
C3 C2 C1 119.0(5) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C2 C3 C4 119.4(4) . . ?
C2 C3 H3A 120.3 . . ?
C4 C3 H3A 120.3 . . ?
C5 C4 C3 118.4(5) . . ?
C5 C4 H4A 120.8 . . ?
C3 C4 H4A 120.8 . . ?
N1 C5 C4 122.0(4) . . ?
N1 C5 C6 114.1(3) . . ?
C4 C5 C6 123.9(4) . . ?
N2 C6 C5 112.7(4) . . ?
N2 C6 C7 124.4(4) . . ?
C5 C6 C7 122.9(4) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C8 N3 124.9(5) . . ?
O2 C8 C9 117.7(4) . . ?
N3 C8 C9 117.4(5) . . ?
C10 C9 C13 115.8(5) . 6 ?
C10 C9 C13 115.8(5) . . ?
C13 C9 C13 34.0(6) 6 . ?
C10 C9 C8 122.7(5) . . ?
C13 C9 C8 118.8(5) 6 . ?
C13 C9 C8 118.8(5) . . ?
C11 C10 C9 119.2(5) . . ?
C11 C10 H10A 120.4 . . ?
C9 C10 H10A 120.4 . . ?
N4 C11 C10 124.6(6) . . ?
N4 C11 H11A 117.7 . . ?
C10 C11 H11A 117.7 . . ?
N4 C12 C13 124.5(6) . . ?
N4 C12 H12A 117.7 . . ?
C13 C12 H12A 117.7 . . ?
C12 C13 C9 116.4(6) . . ?
C12 C13 H13A 121.8 . . ?
C9 C13 H13A 121.8 . . ?
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 1.615(3) 6 ?
V1 O1 1.615(3) . ?
V1 O2 1.961(3) . ?
V1 N2 2.107(4) . ?
V1 N1 2.107(3) . ?
O2 C8 1.296(6) . ?
N1 C1 1.328(6) . ?
N1 C5 1.344(6) . ?
N2 C6 1.294(5) . ?
N2 N3 1.384(5) . ?
N3 C8 1.311(6) . ?
N4 C11 1.327(7) . ?
N4 C12 1.359(9) . ?
N4 C12 1.359(9) 6 ?
C1 C2 1.399(6) . ?
C1 H1A 0.9300 . ?
C2 C3 1.362(8) . ?
C2 H2A 0.9300 . ?
C3 C4 1.393(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.392(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.458(6) . ?
C6 C7 1.500(7) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.490(6) . ?
C9 C10 1.385(8) . ?
C9 C13 1.438(8) 6 ?
C9 C13 1.438(8) . ?
C10 C11 1.375(7) . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9300 . ?
C12 C13 1.392(9) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
