#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:32:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179115 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/77/4307752.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_4307752
loop_
_publ_author_name
'Manas Sutradhar'
'Gurunath Mukherjee'
'Michael G. B. Drew'
'Saktiprosad Ghosh'
_publ_section_title
;
Simple General Method of Generating Non-oxo, Non-amavadine Model
Octacoordinated Vanadium(IV) Complexes of Some Tetradentate ONNO Chelating
Ligands from Various Oxovanadium(IV/V) Compounds and Structural
Characterization of One of Them
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5069
_journal_page_last               5075
_journal_paper_doi               10.1021/ic062242r
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C56 H44 N12 O4 V'
_chemical_formula_weight         999.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           118
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 -2n'
_symmetry_space_group_name_H-M   'P -4 n 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.437(12)
_cell_length_b                   11.438(12)
_cell_length_c                   18.720(19)
_cell_measurement_temperature    293(2)
_cell_volume                     2449(4)
_computing_cell_refinement       XDS
_computing_data_collection       'XDS (Kabsch, 1988)'
_computing_data_reduction        XDS
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Marresearch Image Plate'
_diffrn_measurement_method
'95 frames at 2^o intervals, counting time 2 min.'
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14796
_diffrn_reflns_theta_full        25.75
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.264
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1038
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_coef       0.0089(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details 
  w=1/[σ²(Fo²)+(0.0477P)²+1.1992P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                2241
_reflns_number_total             2343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062242r-file002.cif
_cod_data_source_block           x
_cod_database_code               4307752
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, -z'
'y, -x, -z'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+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 0.5000 0.0000 0.2500 0.02170(18) Uani 1 4 d S . .
O11 O 0.55142(14) 0.12365(14) 0.17816(9) 0.0312(4) Uani 1 1 d . . .
C12 C 0.64977(18) 0.11143(19) 0.14518(12) 0.0262(5) Uani 1 1 d . . .
N13 N 0.28342(16) -0.01817(16) 0.15386(11) 0.0299(4) Uani 1 1 d . . .
N14 N 0.33662(15) 0.05314(16) 0.20307(10) 0.0253(4) Uani 1 1 d . . .
C15 C 0.28538(19) 0.14871(19) 0.22298(13) 0.0280(5) Uani 1 1 d . . .
C16 C 0.1699(2) 0.1939(2) 0.19812(14) 0.0318(5) Uani 1 1 d . . .
C17 C 0.0687(2) 0.1550(3) 0.22865(19) 0.0605(9) Uani 1 1 d . . .
H17 H 0.0696 0.0900 0.2585 0.073 Uiso 1 1 calc R . .
C18 C -0.0371(3) 0.2136(4) 0.2147(2) 0.0725(11) Uani 1 1 d . . .
H18 H -0.1060 0.1880 0.2360 0.087 Uiso 1 1 calc R . .
C19 C -0.0389(3) 0.3067(3) 0.1706(2) 0.0634(10) Uani 1 1 d . . .
H19 H -0.1085 0.3470 0.1630 0.076 Uiso 1 1 calc R . .
C20 C 0.0594(3) 0.3419(3) 0.1373(2) 0.0712(11) Uani 1 1 d . . .
H20 H 0.0565 0.4035 0.1049 0.085 Uiso 1 1 calc R . .
C21 C 0.1652(3) 0.2865(3) 0.15100(18) 0.0548(8) Uani 1 1 d . . .
H21 H 0.2330 0.3120 0.1284 0.066 Uiso 1 1 calc R . .
C31 C 0.6906(2) 0.2079(2) 0.09801(12) 0.0293(5) Uani 1 1 d . . .
C32 C 0.6291(2) 0.3142(2) 0.10104(16) 0.0391(6) Uani 1 1 d . . .
H32 H 0.5640 0.3199 0.1305 0.047 Uiso 1 1 calc R . .
C33 C 0.6629(3) 0.4103(2) 0.06149(18) 0.0539(8) Uani 1 1 d . . .
H33 H 0.6220 0.4803 0.0650 0.065 Uiso 1 1 calc R . .
C34 C 0.7591(3) 0.4007(3) 0.01631(18) 0.0580(9) Uani 1 1 d . . .
H34 H 0.7821 0.4648 -0.0108 0.070 Uiso 1 1 calc R . .
C35 C 0.8206(3) 0.2971(3) 0.01130(16) 0.0511(8) Uani 1 1 d . . .
H35 H 0.8832 0.2918 -0.0203 0.061 Uiso 1 1 calc R . .
C36 C 0.7904(2) 0.1992(2) 0.05311(13) 0.0380(6) Uani 1 1 d . . .
N37 N 0.8606(2) 0.1009(2) 0.04814(13) 0.0470(6) Uani 1 1 d . . .
H37A H 0.9203 0.1010 0.0202 0.056 Uiso 1 1 calc R . .
H37B H 0.8444 0.0397 0.0730 0.056 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
O11 V1 O11 97.43(13) 7_545 8 ?
O11 V1 O11 92.00(12) 7_545 . ?
O11 V1 O11 146.69(9) 8 . ?
O11 V1 O11 146.69(9) 7_545 2_655 ?
O11 V1 O11 92.00(12) 8 2_655 ?
O11 V1 O11 97.43(13) . 2_655 ?
O11 V1 N14 75.43(9) 7_545 2_655 ?
O11 V1 N14 142.20(6) 8 2_655 ?
O11 V1 N14 71.10(7) . 2_655 ?
O11 V1 N14 77.60(8) 2_655 2_655 ?
O11 V1 N14 142.20(6) 7_545 . ?
O11 V1 N14 75.43(9) 8 . ?
O11 V1 N14 77.60(8) . . ?
O11 V1 N14 71.10(7) 2_655 . ?
N14 V1 N14 131.82(12) 2_655 . ?
O11 V1 N14 71.10(7) 7_545 8 ?
O11 V1 N14 77.61(8) 8 8 ?
O11 V1 N14 75.42(9) . 8 ?
O11 V1 N14 142.20(6) 2_655 8 ?
N14 V1 N14 131.06(10) 2_655 8 ?
N14 V1 N14 71.11(11) . 8 ?
O11 V1 N14 77.61(8) 7_545 7_545 ?
O11 V1 N14 71.10(7) 8 7_545 ?
O11 V1 N14 142.20(6) . 7_545 ?
O11 V1 N14 75.42(9) 2_655 7_545 ?
N14 V1 N14 71.11(11) 2_655 7_545 ?
N14 V1 N14 131.06(10) . 7_545 ?
N14 V1 N14 131.83(12) 8 7_545 ?
C12 O11 V1 119.47(14) . . ?
O11 C12 N13 122.2(2) . 2_655 ?
O11 C12 C31 118.46(19) . . ?
N13 C12 C31 119.3(2) 2_655 . ?
C12 N13 N14 107.80(18) 2_655 . ?
C15 N14 N13 119.61(18) . . ?
C15 N14 V1 120.91(16) . . ?
N13 N14 V1 119.40(13) . . ?
N14 C15 C15 113.51(13) . 8 ?
N14 C15 C16 127.1(2) . . ?
C15 C15 C16 119.39(12) 8 . ?
C17 C16 C21 119.0(2) . . ?
C17 C16 C15 120.4(2) . . ?
C21 C16 C15 120.0(2) . . ?
C16 C17 C18 119.7(3) . . ?
C19 C18 C17 120.2(3) . . ?
C20 C19 C18 120.4(3) . . ?
C19 C20 C21 120.4(3) . . ?
C16 C21 C20 120.2(3) . . ?
C32 C31 C36 119.1(2) . . ?
C32 C31 C12 117.4(2) . . ?
C36 C31 C12 123.4(2) . . ?
C33 C32 C31 121.8(3) . . ?
C32 C33 C34 119.0(3) . . ?
C35 C34 C33 120.8(3) . . ?
C34 C35 C36 121.2(3) . . ?
N37 C36 C35 117.7(3) . . ?
N37 C36 C31 124.2(2) . . ?
C35 C36 C31 118.0(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 O11 2.038(2) 7_545 ?
V1 O11 2.038(2) 8 ?
V1 O11 2.038(2) . ?
V1 O11 2.038(2) 2_655 ?
V1 N14 2.152(3) 2_655 ?
V1 N14 2.152(3) . ?
V1 N14 2.152(3) 8 ?
V1 N14 2.153(3) 7_545 ?
O11 C12 1.291(3) . ?
C12 N13 1.322(3) 2_655 ?
C12 C31 1.488(3) . ?
N13 C12 1.322(3) 2_655 ?
N13 N14 1.373(3) . ?
N14 C15 1.295(3) . ?
C15 C15 1.470(5) 8 ?
C15 C16 1.493(3) . ?
C16 C17 1.366(4) . ?
C16 C21 1.380(4) . ?
C17 C18 1.408(5) . ?
C18 C19 1.348(5) . ?
C19 C20 1.347(6) . ?
C20 C21 1.389(4) . ?
C31 C32 1.405(4) . ?
C31 C36 1.421(4) . ?
C32 C33 1.380(4) . ?
C33 C34 1.392(5) . ?
C34 C35 1.382(5) . ?
C35 C36 1.409(4) . ?
C36 N37 1.385(4) . ?
