#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:40:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179256 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/76/4317699.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_4317699
loop_
_publ_author_name
'Rupam Dinda'
'Parbati Sengupta'
'Saktiprosad Ghosh'
'Thomas C. W. Mak'
_publ_section_title
;
 Valence Delocalization in a Mixed-Oxidation Divanadium (IV, V) Complex
 Electrogenerated from Its Structurally Characterized Divanadium (V)
 Analogue with a Tridentate (ONO) Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1684
_journal_page_last               1688
_journal_paper_doi               10.1021/ic010865t
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C30 H26 N6 O7 V2'
_chemical_formula_weight         684.45
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.145(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9240(18)
_cell_length_b                   16.211(4)
_cell_length_c                   23.381(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2986.2(12)
_computing_cell_refinement       'Bruker SMART CCD Diffractometer'
_computing_data_collection       'Bruker SMART CCD Diffractometer'
_computing_data_reduction        'Bruker SMART CCD Diffractometer'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens 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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD Diffractometer'
_diffrn_measurement_method       'omega 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  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20687
_diffrn_reflns_theta_full        28.10
_diffrn_reflns_theta_max         28.10
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7621
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Dark blue'
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.93
_exptl_crystal_size_mid          0.68
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0000(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          3.069
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0837P)²+1.7533P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1712
_reflns_number_gt                4880
_reflns_number_total             7242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010865t.cif
_cod_data_source_block           r06
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2986.1(12)
_cod_database_code               4317699
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.57067(8) 0.56186(4) 0.35362(2) 0.03272(18) Uani 1 1 d . . .
V2 V 0.21456(8) 0.59103(4) 0.30173(3) 0.03427(18) Uani 1 1 d . . .
O1 O 0.5335(3) 0.60740(14) 0.27616(10) 0.0361(6) Uani 1 1 d . . .
O2 O 0.5858(3) 0.57939(16) 0.43065(11) 0.0419(6) Uani 1 1 d . . .
O3 O 0.3214(3) 0.67638(14) 0.35058(10) 0.0366(6) Uani 1 1 d . . .
O4 O 0.1925(4) 0.54323(16) 0.23119(11) 0.0468(7) Uani 1 1 d . . .
O5 O 0.3599(3) 0.51981(14) 0.34027(10) 0.0354(6) Uani 1 1 d . . .
O6 O 0.0354(3) 0.57923(17) 0.32425(13) 0.0528(7) Uani 1 1 d . . .
O7 O 0.7014(3) 0.49019(16) 0.34688(12) 0.0485(7) Uani 1 1 d . . .
N1 N 0.7237(4) 0.66586(17) 0.35475(12) 0.0335(6) Uani 1 1 d . . .
N2 N 0.7092(4) 0.71400(18) 0.30525(12) 0.0361(7) Uani 1 1 d . . .
N3 N 0.7135(5) 0.8446(2) 0.23142(15) 0.0589(10) Uani 1 1 d . . .
H3A H 0.7423 0.8284 0.2661 0.071 Uiso 1 1 calc R . .
H3B H 0.7423 0.8929 0.2207 0.071 Uiso 1 1 calc R . .
N4 N 0.1731(4) 0.69987(18) 0.25493(12) 0.0355(7) Uani 1 1 d . . .
N5 N 0.2419(4) 0.77107(18) 0.28116(12) 0.0389(7) Uani 1 1 d . . .
N6 N 0.3777(7) 0.9244(2) 0.29646(16) 0.0781(15) Uani 1 1 d . . .
H6B H 0.3219 0.8920 0.2722 0.094 Uiso 1 1 calc R . .
H6C H 0.3983 0.9743 0.2869 0.094 Uiso 1 1 calc R . .
C1 C 0.6085(5) 0.6784(2) 0.26553(15) 0.0336(8) Uani 1 1 d . . .
C2 C 0.5714(5) 0.7141(2) 0.20797(14) 0.0347(8) Uani 1 1 d . . .
C3 C 0.4765(5) 0.6667(2) 0.16648(15) 0.0428(9) Uani 1 1 d . . .
H3C H 0.4408 0.6144 0.1763 0.051 Uiso 1 1 calc R . .
C4 C 0.4343(6) 0.6952(3) 0.11127(17) 0.0521(11) Uani 1 1 d . . .
H4A H 0.3701 0.6630 0.0841 0.062 Uiso 1 1 calc R . .
C5 C 0.4897(6) 0.7728(3) 0.09705(17) 0.0551(12) Uani 1 1 d . . .
H5B H 0.4651 0.7920 0.0596 0.066 Uiso 1 1 calc R . .
C6 C 0.5786(6) 0.8212(2) 0.13647(17) 0.0513(11) Uani 1 1 d . . .
H6D H 0.6115 0.8735 0.1258 0.062 Uiso 1 1 calc R . .
C7 C 0.6231(5) 0.7940(2) 0.19365(16) 0.0398(9) Uani 1 1 d . . .
C8 C 0.7299(5) 0.5909(2) 0.46607(15) 0.0384(8) Uani 1 1 d . . .
C9 C 0.7499(5) 0.5497(2) 0.51873(16) 0.0459(9) Uani 1 1 d . . .
H9A H 0.6639 0.5160 0.5296 0.055 Uiso 1 1 calc R . .
C10 C 0.8982(6) 0.5594(3) 0.55450(17) 0.0539(11) Uani 1 1 d . . .
H10A H 0.9124 0.5317 0.5895 0.065 Uiso 1 1 calc R . .
C11 C 1.0256(6) 0.6097(3) 0.53902(17) 0.0530(11) Uani 1 1 d . . .
H11A H 1.1265 0.6144 0.5630 0.064 Uiso 1 1 calc R . .
C12 C 1.0045(5) 0.6528(3) 0.48852(17) 0.0472(10) Uani 1 1 d . . .
H12A H 1.0902 0.6880 0.4792 0.057 Uiso 1 1 calc R . .
C13 C 0.8552(5) 0.6450(2) 0.45026(15) 0.0383(8) Uani 1 1 d . . .
C14 C 0.8304(5) 0.6918(2) 0.39677(16) 0.0384(8) Uani 1 1 d . . .
C15 C 0.9258(6) 0.7705(3) 0.39105(18) 0.0534(11) Uani 1 1 d . . .
H15A H 0.8949 0.7937 0.3536 0.080 Uiso 1 1 calc R . .
H15B H 1.0455 0.7595 0.3959 0.080 Uiso 1 1 calc R . .
H15C H 0.8982 0.8088 0.4199 0.080 Uiso 1 1 calc R . .
C21 C 0.3170(5) 0.7529(2) 0.33149(14) 0.0342(8) Uani 1 1 d . . .
C22 C 0.4039(5) 0.8156(2) 0.36861(14) 0.0367(8) Uani 1 1 d . . .
C23 C 0.4642(5) 0.7931(2) 0.42485(16) 0.0453(9) Uani 1 1 d . . .
H23A H 0.4450 0.7398 0.4372 0.054 Uiso 1 1 calc R . .
C24 C 0.5500(7) 0.8470(3) 0.46198(18) 0.0583(12) Uani 1 1 d . . .
H24A H 0.5876 0.8309 0.4994 0.070 Uiso 1 1 calc R . .
C25 C 0.5803(8) 0.9256(3) 0.4433(2) 0.0737(16) Uani 1 1 d . . .
H25A H 0.6390 0.9627 0.4684 0.088 Uiso 1 1 calc R . .
C26 C 0.5265(8) 0.9497(3) 0.3893(2) 0.0785(17) Uani 1 1 d . . .
H26A H 0.5515 1.0027 0.3777 0.094 Uiso 1 1 calc R . .
C27 C 0.4332(7) 0.8966(2) 0.35008(18) 0.0549(11) Uani 1 1 d . . .
C28 C 0.0801(5) 0.5573(3) 0.18543(18) 0.0474(10) Uani 1 1 d . . .
C29 C 0.0229(6) 0.4900(3) 0.1525(2) 0.0718(14) Uani 1 1 d . . .
H29A H 0.0588 0.4370 0.1630 0.086 Uiso 1 1 calc R . .
C30 C -0.0866(8) 0.5026(4) 0.1043(3) 0.109(3) Uani 1 1 d . . .
H30A H -0.1258 0.4578 0.0818 0.131 Uiso 1 1 calc R . .
C31 C -0.1396(9) 0.5805(4) 0.0888(3) 0.122(3) Uani 1 1 d . . .
H31A H -0.2140 0.5884 0.0557 0.146 Uiso 1 1 calc R . .
C32 C -0.0843(7) 0.6463(4) 0.1212(2) 0.0833(18) Uani 1 1 d . . .
H32A H -0.1234 0.6986 0.1103 0.100 Uiso 1 1 calc R . .
C33 C 0.0293(5) 0.6378(3) 0.17051(18) 0.0495(10) Uani 1 1 d . . .
C34 C 0.0974(5) 0.7093(3) 0.20278(16) 0.0423(9) Uani 1 1 d . . .
C35 C 0.0886(6) 0.7939(3) 0.17642(18) 0.0599(12) Uani 1 1 d . . .
H35A H 0.1381 0.8332 0.2040 0.090 Uiso 1 1 calc R . .
H35B H -0.0279 0.8083 0.1653 0.090 Uiso 1 1 calc R . .
H35C H 0.1498 0.7943 0.1431 0.090 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
O7 V1 O5 108.13(13) . . ?
O7 V1 O2 103.91(14) . . ?
O5 V1 O2 101.14(11) . . ?
O7 V1 O1 102.82(12) . . ?
O5 V1 O1 86.39(10) . . ?
O2 V1 O1 148.27(11) . . ?
O7 V1 N1 102.16(13) . . ?
O5 V1 N1 147.14(11) . . ?
O2 V1 N1 83.31(11) . . ?
O1 V1 N1 74.58(11) . . ?
O7 V1 V2 132.74(11) . . ?
O5 V1 V2 34.00(7) . . ?
O2 V1 V2 109.74(9) . . ?
O1 V1 V2 61.34(8) . . ?
N1 V1 V2 113.70(8) . . ?
O6 V2 O5 107.78(13) . . ?
O6 V2 O4 104.42(15) . . ?
O5 V2 O4 100.09(12) . . ?
O6 V2 O3 104.05(14) . . ?
O5 V2 O3 86.96(11) . . ?
O4 V2 O3 146.87(12) . . ?
O6 V2 N4 100.43(13) . . ?
O5 V2 N4 149.45(12) . . ?
O4 V2 N4 83.67(12) . . ?
O3 V2 N4 74.83(11) . . ?
O6 V2 V1 133.62(11) . . ?
O5 V2 V1 33.94(7) . . ?
O4 V2 V1 107.26(9) . . ?
O3 V2 V1 62.48(8) . . ?
N4 V2 V1 115.87(9) . . ?
C1 O1 V1 118.3(2) . . ?
C8 O2 V1 126.3(2) . . ?
C21 O3 V2 118.7(2) . . ?
C28 O4 V2 130.3(3) . . ?
V1 O5 V2 112.06(12) . . ?
C14 N1 N2 116.0(3) . . ?
C14 N1 V1 127.3(2) . . ?
N2 N1 V1 116.7(2) . . ?
C1 N2 N1 109.7(3) . . ?
C34 N4 N5 115.7(3) . . ?
C34 N4 V2 128.2(3) . . ?
N5 N4 V2 116.0(2) . . ?
C21 N5 N4 109.4(3) . . ?
N2 C1 O1 120.3(3) . . ?
N2 C1 C2 122.1(3) . . ?
O1 C1 C2 117.6(3) . . ?
C3 C2 C7 119.4(3) . . ?
C3 C2 C1 117.5(3) . . ?
C7 C2 C1 123.1(3) . . ?
C4 C3 C2 121.7(4) . . ?
C3 C4 C5 118.6(4) . . ?
C6 C5 C4 121.3(4) . . ?
C5 C6 C7 121.6(4) . . ?
N3 C7 C2 123.3(3) . . ?
N3 C7 C6 119.3(4) . . ?
C2 C7 C6 117.4(4) . . ?
O2 C8 C9 119.0(3) . . ?
O2 C8 C13 120.0(3) . . ?
C9 C8 C13 121.0(4) . . ?
C10 C9 C8 119.4(4) . . ?
C11 C10 C9 120.7(4) . . ?
C12 C11 C10 120.3(4) . . ?
C11 C12 C13 121.2(4) . . ?
C8 C13 C12 117.3(3) . . ?
C8 C13 C14 121.1(3) . . ?
C12 C13 C14 121.6(4) . . ?
N1 C14 C13 119.9(3) . . ?
N1 C14 C15 120.3(3) . . ?
C13 C14 C15 119.8(3) . . ?
N5 C21 O3 121.0(3) . . ?
N5 C21 C22 121.5(3) . . ?
O3 C21 C22 117.4(3) . . ?
C23 C22 C27 118.7(4) . . ?
C23 C22 C21 118.0(3) . . ?
C27 C22 C21 123.3(3) . . ?
C24 C23 C22 122.0(4) . . ?
C23 C24 C25 118.9(4) . . ?
C26 C25 C24 121.2(4) . . ?
C25 C26 C27 121.7(4) . . ?
N6 C27 C22 122.9(4) . . ?
N6 C27 C26 119.6(4) . . ?
C22 C27 C26 117.4(4) . . ?
O4 C28 C29 117.5(4) . . ?
O4 C28 C33 120.6(4) . . ?
C29 C28 C33 121.9(4) . . ?
C30 C29 C28 118.9(5) . . ?
C29 C30 C31 120.6(5) . . ?
C32 C31 C30 120.4(5) . . ?
C31 C32 C33 121.9(5) . . ?
C32 C33 C28 116.3(4) . . ?
C32 C33 C34 121.4(4) . . ?
C28 C33 C34 122.2(4) . . ?
N4 C34 C33 119.8(4) . . ?
N4 C34 C35 119.0(4) . . ?
C33 C34 C35 121.1(4) . . ?
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 O7 1.576(3) . ?
V1 O5 1.800(2) . ?
V1 O2 1.814(3) . ?
V1 O1 1.949(2) . ?
V1 N1 2.075(3) . ?
V1 V2 2.9875(10) . ?
V2 O6 1.578(3) . ?
V2 O5 1.803(2) . ?
V2 O4 1.814(3) . ?
V2 O3 1.931(2) . ?
V2 N4 2.084(3) . ?
O1 C1 1.331(4) . ?
O2 C8 1.350(5) . ?
O3 C21 1.317(4) . ?
O4 C28 1.336(4) . ?
N1 C14 1.295(5) . ?
N1 N2 1.390(4) . ?
N2 C1 1.293(5) . ?
N3 C7 1.353(5) . ?
N4 C34 1.309(5) . ?
N4 N5 1.391(4) . ?
N5 C21 1.295(4) . ?
N6 C27 1.360(5) . ?
C1 C2 1.465(5) . ?
C2 C3 1.393(5) . ?
C2 C7 1.410(5) . ?
C3 C4 1.378(5) . ?
C4 C5 1.384(6) . ?
C5 C6 1.350(6) . ?
C6 C7 1.416(5) . ?
C8 C9 1.395(5) . ?
C8 C13 1.403(5) . ?
C9 C10 1.376(6) . ?
C10 C11 1.376(6) . ?
C11 C12 1.367(6) . ?
C12 C13 1.411(5) . ?
C13 C14 1.458(5) . ?
C14 C15 1.496(5) . ?
C21 C22 1.460(5) . ?
C22 C23 1.398(5) . ?
C22 C27 1.410(5) . ?
C23 C24 1.361(6) . ?
C24 C25 1.377(6) . ?
C25 C26 1.345(7) . ?
C26 C27 1.408(6) . ?
C28 C29 1.384(6) . ?
C28 C33 1.398(6) . ?
C29 C30 1.361(7) . ?
C30 C31 1.368(9) . ?
C31 C32 1.354(8) . ?
C32 C33 1.391(6) . ?
C33 C34 1.455(6) . ?
C34 C35 1.503(6) . ?
