#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:21:57 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301837 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/95/4319502.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_4319502
loop_
_publ_author_name
'H. Nakano'
'T. Ozeki'
'A. Yagasaki'
_publ_section_title
;
 Synthesis and Structural Characterization of a New Series of
 Vanadoselenites, [SexV4-xO12-x](4-x)- (x = 1, 2)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1816
_journal_page_last               1819
_journal_paper_doi               10.1021/ic0010508
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C36 H30 N O5 P2 Se V'
_chemical_formula_weight         748.45
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.3070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2931(3)
_cell_length_b                   13.5101(3)
_cell_length_c                   20.9793(5)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_volume                     3344.09(14)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23375
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.524
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.757659
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         4794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0487P)²+0.4918P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                3414
_reflns_number_total             4794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0010508_2.cif
_cod_data_source_block           sev
_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.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319502
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_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
Se Se 0.12623(3) -0.13172(3) 0.07445(2) 0.05243(15) Uani 1 1 d . . .
V V -0.02715(6) 0.05909(5) 0.08269(3) 0.0477(2) Uani 1 1 d . . .
O1 O 0.0929(3) -0.2473(2) 0.06978(17) 0.0824(10) Uani 1 1 d . . .
O2 O -0.0838(3) 0.0774(2) 0.14227(15) 0.0695(9) Uani 1 1 d . . .
O3 O 0.0908(3) 0.1168(2) 0.09890(16) 0.0753(9) Uani 1 1 d . . .
O4 O 0.0006(2) -0.07430(18) 0.07594(14) 0.0521(7) Uani 1 1 d . . .
O5 O -0.1330(3) 0.0990(2) 0.00377(15) 0.0700(9) Uani 1 1 d . . .
N N 0.2966(2) -0.1250(2) 0.69546(13) 0.0331(7) Uani 1 1 d . . .
P1 P 0.19790(7) -0.09154(7) 0.63247(4) 0.0293(2) Uani 1 1 d . . .
P2 P 0.42418(7) -0.09107(7) 0.72902(4) 0.0297(2) Uani 1 1 d . . .
C1 C 0.2054(3) 0.0371(3) 0.60982(17) 0.0317(8) Uani 1 1 d . . .
C2 C 0.2305(3) 0.0650(3) 0.55206(19) 0.0427(10) Uani 1 1 d . . .
H2 H 0.2395 0.0171 0.5221 0.051 Uiso 1 1 calc R . .
C3 C 0.2424(3) 0.1651(3) 0.5389(2) 0.0544(11) Uani 1 1 d . . .
H3 H 0.2592 0.1840 0.5001 0.065 Uiso 1 1 calc R . .
C4 C 0.2294(3) 0.2356(3) 0.5831(2) 0.0574(12) Uani 1 1 d . . .
H4 H 0.2369 0.3022 0.5740 0.069 Uiso 1 1 calc R . .
C5 C 0.2051(3) 0.2084(3) 0.6411(2) 0.0538(11) Uani 1 1 d . . .
H5 H 0.1971 0.2567 0.6711 0.065 Uiso 1 1 calc R . .
C6 C 0.1927(3) 0.1092(3) 0.65478(19) 0.0429(9) Uani 1 1 d . . .
H6 H 0.1761 0.0909 0.6937 0.052 Uiso 1 1 calc R . .
C7 C 0.0630(3) -0.1073(2) 0.64956(16) 0.0310(8) Uani 1 1 d . . .
C8 C -0.0275(3) -0.0464(3) 0.62036(19) 0.0458(10) Uani 1 1 d . . .
H8 H -0.0173 0.0067 0.5945 0.055 Uiso 1 1 calc R . .
C9 C -0.1331(3) -0.0638(3) 0.6293(2) 0.0507(11) Uani 1 1 d . . .
H9 H -0.1934 -0.0223 0.6093 0.061 Uiso 1 1 calc R . .
C10 C -0.1491(3) -0.1403(4) 0.6667(2) 0.0608(12) Uani 1 1 d . . .
H10 H -0.2203 -0.1520 0.6723 0.073 Uiso 1 1 calc R . .
C11 C -0.0604(4) -0.2003(4) 0.6961(3) 0.109(2) Uani 1 1 d . . .
H11 H -0.0711 -0.2530 0.7222 0.131 Uiso 1 1 calc R . .
C12 C 0.0458(4) -0.1836(4) 0.6874(3) 0.0804(17) Uani 1 1 d . . .
H12 H 0.1058 -0.2252 0.7077 0.096 Uiso 1 1 calc R . .
C13 C 0.1937(3) -0.1663(2) 0.56087(16) 0.0309(8) Uani 1 1 d . . .
C14 C 0.0976(3) -0.1684(3) 0.50575(18) 0.0479(10) Uani 1 1 d . . .
H14 H 0.0337 -0.1318 0.5061 0.057 Uiso 1 1 calc R . .
C15 C 0.0981(4) -0.2248(3) 0.45106(19) 0.0566(11) Uani 1 1 d . . .
H15 H 0.0345 -0.2253 0.4144 0.068 Uiso 1 1 calc R . .
C16 C 0.1909(4) -0.2802(3) 0.4499(2) 0.0536(11) Uani 1 1 d . . .
H16 H 0.1900 -0.3184 0.4129 0.064 Uiso 1 1 calc R . .
C17 C 0.2857(3) -0.2791(3) 0.50393(19) 0.0505(11) Uani 1 1 d . . .
H17 H 0.3490 -0.3162 0.5032 0.061 Uiso 1 1 calc R . .
C18 C 0.2868(3) -0.2232(3) 0.55888(18) 0.0402(9) Uani 1 1 d . . .
H18 H 0.3508 -0.2235 0.5953 0.048 Uiso 1 1 calc R . .
C19 C 0.4331(3) -0.0278(3) 0.80621(18) 0.0389(9) Uani 1 1 d . . .
C20 C 0.3367(3) -0.0180(3) 0.8278(2) 0.0485(10) Uani 1 1 d . . .
H20 H 0.2684 -0.0451 0.8030 0.058 Uiso 1 1 calc R . .
C21 C 0.3423(4) 0.0324(3) 0.8866(2) 0.0676(13) Uani 1 1 d . . .
H21 H 0.2772 0.0401 0.9004 0.081 Uiso 1 1 calc R . .
C22 C 0.4432(5) 0.0709(4) 0.9241(2) 0.0827(16) Uani 1 1 d . . .
H22 H 0.4467 0.1042 0.9634 0.099 Uiso 1 1 calc R . .
C23 C 0.5379(5) 0.0602(4) 0.9037(2) 0.0869(17) Uani 1 1 d . . .
H23 H 0.6062 0.0865 0.9292 0.104 Uiso 1 1 calc R . .
C24 C 0.5341(4) 0.0106(4) 0.8452(2) 0.0689(14) Uani 1 1 d . . .
H24 H 0.6000 0.0032 0.8322 0.083 Uiso 1 1 calc R . .
C25 C 0.4842(3) -0.0107(3) 0.67923(16) 0.0322(8) Uani 1 1 d . . .
C26 C 0.4766(3) 0.0916(3) 0.68364(19) 0.0431(10) Uani 1 1 d . . .
H26 H 0.4484 0.1193 0.7164 0.052 Uiso 1 1 calc R . .
C27 C 0.5101(3) 0.1520(3) 0.6403(2) 0.0594(12) Uani 1 1 d . . .
H27 H 0.5044 0.2204 0.6435 0.071 Uiso 1 1 calc R . .
C28 C 0.5523(4) 0.1112(4) 0.5919(2) 0.0703(15) Uani 1 1 d . . .
H28 H 0.5747 0.1524 0.5624 0.084 Uiso 1 1 calc R . .
C29 C 0.5615(3) 0.0103(4) 0.5867(2) 0.0583(12) Uani 1 1 d . . .
H29 H 0.5903 -0.0164 0.5539 0.070 Uiso 1 1 calc R . .
C30 C 0.5279(3) -0.0519(3) 0.63052(17) 0.0410(9) Uani 1 1 d . . .
H30 H 0.5345 -0.1202 0.6274 0.049 Uiso 1 1 calc R . .
C31 C 0.5133(3) -0.1991(3) 0.74544(16) 0.0324(8) Uani 1 1 d . . .
C32 C 0.4663(3) -0.2934(3) 0.73221(17) 0.0426(10) Uani 1 1 d . . .
H32 H 0.3881 -0.3010 0.7166 0.051 Uiso 1 1 calc R . .
C33 C 0.5370(4) -0.3765(3) 0.7425(2) 0.0591(12) Uani 1 1 d . . .
H33 H 0.5062 -0.4396 0.7337 0.071 Uiso 1 1 calc R . .
C34 C 0.6521(5) -0.3639(4) 0.7657(2) 0.0715(15) Uani 1 1 d . . .
H34 H 0.6990 -0.4193 0.7724 0.086 Uiso 1 1 calc R . .
C35 C 0.6995(4) -0.2725(4) 0.7791(2) 0.0670(14) Uani 1 1 d . . .
H35 H 0.7777 -0.2658 0.7952 0.080 Uiso 1 1 calc R . .
C36 C 0.6309(3) -0.1897(3) 0.76891(19) 0.0503(11) Uani 1 1 d . . .
H36 H 0.6633 -0.1272 0.7777 0.060 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'
P P 0.1023 0.0942 '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'
Se Se -0.0929 2.2259 '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 Se O5 105.66(16) . 3 ?
O1 Se O4 102.84(14) . . ?
O5 Se O4 100.56(13) 3 . ?
O3 V O2 108.91(17) . . ?
O3 V O4 108.45(14) . . ?
O2 V O4 109.79(14) . . ?
O3 V O5 114.28(16) . . ?
O2 V O5 107.29(14) . . ?
O4 V O5 108.08(13) . . ?
Se O4 V 128.44(15) . . ?
Se O5 V 135.04(17) 3 . ?
P1 N P2 135.42(18) . . ?
N P1 C13 111.77(15) . . ?
N P1 C7 109.34(15) . . ?
C13 P1 C7 106.69(15) . . ?
N P1 C1 114.07(15) . . ?
C13 P1 C1 108.14(16) . . ?
C7 P1 C1 106.45(15) . . ?
N P2 C31 108.77(16) . . ?
N P2 C25 115.41(15) . . ?
C31 P2 C25 105.86(16) . . ?
N P2 C19 109.66(16) . . ?
C31 P2 C19 109.36(16) . . ?
C25 P2 C19 107.62(16) . . ?
C2 C1 C6 119.8(3) . . ?
C2 C1 P1 122.1(3) . . ?
C6 C1 P1 118.0(3) . . ?
C1 C2 C3 119.9(4) . . ?
C4 C3 C2 120.0(4) . . ?
C3 C4 C5 120.5(4) . . ?
C4 C5 C6 120.1(4) . . ?
C5 C6 C1 119.7(4) . . ?
C12 C7 C8 118.3(3) . . ?
C12 C7 P1 120.7(3) . . ?
C8 C7 P1 120.8(3) . . ?
C7 C8 C9 120.6(4) . . ?
C10 C9 C8 120.4(4) . . ?
C9 C10 C11 119.5(4) . . ?
C10 C11 C12 120.5(4) . . ?
C7 C12 C11 120.6(4) . . ?
C18 C13 C14 118.3(3) . . ?
C18 C13 P1 120.4(3) . . ?
C14 C13 P1 121.3(3) . . ?
C15 C14 C13 119.9(4) . . ?
C16 C15 C14 121.0(4) . . ?
C15 C16 C17 119.7(4) . . ?
C18 C17 C16 120.2(4) . . ?
C17 C18 C13 121.0(3) . . ?
C24 C19 C20 118.6(4) . . ?
C24 C19 P2 121.8(3) . . ?
C20 C19 P2 119.7(3) . . ?
C19 C20 C21 120.0(4) . . ?
C22 C21 C20 120.3(4) . . ?
C23 C22 C21 119.8(4) . . ?
C22 C23 C24 120.8(5) . . ?
C19 C24 C23 120.5(4) . . ?
C26 C25 C30 119.5(3) . . ?
C26 C25 P2 120.9(3) . . ?
C30 C25 P2 119.2(3) . . ?
C27 C26 C25 120.7(4) . . ?
C26 C27 C28 119.8(4) . . ?
C29 C28 C27 120.8(4) . . ?
C28 C29 C30 120.0(4) . . ?
C29 C30 C25 119.2(4) . . ?
C32 C31 C36 118.9(3) . . ?
C32 C31 P2 120.5(3) . . ?
C36 C31 P2 120.6(3) . . ?
C31 C32 C33 119.8(4) . . ?
C34 C33 C32 119.3(4) . . ?
C35 C34 C33 121.6(4) . . ?
C34 C35 C36 119.7(4) . . ?
C35 C36 C31 120.6(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
Se O1 1.610(3) . ?
Se O5 1.724(3) 3 ?
Se O4 1.736(3) . ?
V O3 1.597(3) . ?
V O2 1.612(3) . ?
V O4 1.847(3) . ?
V O5 1.875(3) . ?
O5 Se 1.724(3) 3 ?
N P1 1.588(3) . ?
N P2 1.595(3) . ?
P1 C13 1.799(3) . ?
P1 C7 1.805(3) . ?
P1 C1 1.811(3) . ?
P2 C31 1.799(3) . ?
P2 C25 1.803(3) . ?
P2 C19 1.807(4) . ?
C1 C2 1.384(5) . ?
C1 C6 1.395(5) . ?
C2 C3 1.397(5) . ?
C3 C4 1.370(6) . ?
C4 C5 1.382(6) . ?
C5 C6 1.388(5) . ?
C7 C12 1.353(5) . ?
C7 C8 1.381(5) . ?
C8 C9 1.382(5) . ?
C9 C10 1.345(6) . ?
C10 C11 1.360(6) . ?
C11 C12 1.387(6) . ?
C13 C18 1.389(5) . ?
C13 C14 1.402(5) . ?
C14 C15 1.379(5) . ?
C15 C16 1.370(5) . ?
C16 C17 1.379(5) . ?
C17 C18 1.375(5) . ?
C19 C24 1.382(5) . ?
C19 C20 1.389(5) . ?
C20 C21 1.393(6) . ?
C21 C22 1.371(6) . ?
C22 C23 1.356(7) . ?
C23 C24 1.386(6) . ?
C25 C26 1.390(5) . ?
C25 C30 1.397(5) . ?
C26 C27 1.368(5) . ?
C27 C28 1.378(6) . ?
C28 C29 1.375(6) . ?
C29 C30 1.391(5) . ?
C31 C32 1.394(5) . ?
C31 C36 1.396(5) . ?
C32 C33 1.399(5) . ?
C33 C34 1.372(6) . ?
C34 C35 1.360(7) . ?
C35 C36 1.381(6) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 Se O4 V -72.5(2) 3 . . . ?
Se O4 V O5 115.4(2) . . . . ?
O4 V O5 Se -81.3(3) . . . 3 ?
V O5 Se O4 22.4(3) . . 3 3 ?
O5 Se O4 V 72.5(2) . 3 3 3 ?
Se O4 V O5 -115.4(2) 3 3 3 3 ?
O4 V O5 Se 81.3(3) 3 3 3 . ?
V O5 Se O4 -22.4(3) 3 3 . . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139133572
