#------------------------------------------------------------------------------
#$Date: 2025-03-04 22:21:00 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298278 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/76/7717686.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_7717686
loop_
_publ_author_name
'Galiev, R. R.'
'Komarov, V. Y.'
'Ryzhikov, M. R.'
'Kozlova, S. G.'
'Kuznetsov, V. A.'
'Grayfer, E. D.'
'Artemkina, S. B.'
'Fedorov, V. E.'
_publ_section_title
;
 Extended chains in vanadium O-centered complex
 [V₄OSe₈I₅]<sub>∞</sub>: synthesis
 and structure.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2147
_journal_page_last               2155
_journal_paper_doi               10.1039/d4dt02758b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'I5 O Se8 V4'
_chemical_formula_sum            'I5 O Se8 V4'
_chemical_formula_weight         1485.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-07-12 deposited with the CCDC.	2024-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 123.649(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.1319(13)
_cell_length_b                   5.8841(3)
_cell_length_c                   18.0933(9)
_cell_measurement_reflns_used    3774
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.32
_cell_measurement_theta_min      2.32
_cell_volume                     1872.81(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
 Data collection was performed by Dr. V.Yu. Komarov in XRD Facility
 of NIIC SB RAS
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture, PHOTON-III CMOS'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11066
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.503
_diffrn_reflns_theta_min         2.316
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    25.707
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1089 before and 0.0521 after correction.
The Ratio of minimum to maximum transmission is 0.6940.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.270
_exptl_crystal_description       needle
_exptl_crystal_F_000             2548
_exptl_crystal_size_max          0.062
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.004
_refine_diff_density_max         1.368
_refine_diff_density_min         -4.266
_refine_diff_density_rms         0.366
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         2859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0445P)²+40.6730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2268
_reflns_number_total             2859
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02758b3.cif
_cod_data_source_block           sp387_s2_150k
_cod_depositor_comments          'Adding full bibliography for 7717686.cif.'
_cod_database_code               7717686
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.299
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.34845(3) 0.31965(10) 0.48794(3) 0.01878(14) Uani 1 1 d . . . . .
I2 I 0.33208(3) 1.09207(10) 0.78999(4) 0.01921(14) Uani 1 1 d . . . . .
I3 I 0.5000 0.20463(14) 0.7500 0.02060(18) Uani 1 2 d S T P A 1
Se11 Se 0.52919(5) 0.86527(17) 0.93593(5) 0.0204(2) Uani 1 1 d . . . . .
Se12 Se 0.45420(5) 0.54182(17) 0.88276(5) 0.02003(19) Uani 1 1 d . . . . .
Se21 Se 0.33221(5) 0.86934(17) 0.59760(5) 0.0201(2) Uani 1 1 d . . . . .
Se22 Se 0.32721(5) 0.54453(17) 0.66644(5) 0.0202(2) Uani 1 1 d . . . . .
V1 V 0.43125(8) 0.5796(3) 0.63276(9) 0.0193(3) Uani 1 1 d . . . . .
V2 V 0.42435(8) 0.8312(3) 0.76794(9) 0.0190(3) Uani 1 1 d . . . . .
O1 O 0.5000 0.7027(14) 0.7500 0.0134(15) Uani 1 2 d S T P A .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 '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'
Se Se -0.0929 2.2259 '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
V1 I3 V1 78.02(6) . 2_656 ?
V1 I3 V2 126.81(4) 2_656 2_646 ?
V1 I3 V2 126.81(4) . 1_545 ?
V1 I3 V2 127.10(4) 2_656 1_545 ?
V1 I3 V2 127.10(4) . 2_646 ?
V2 I3 V2 78.62(6) 1_545 2_646 ?
Se12 Se11 V1 65.20(5) . 2_656 ?
Se12 Se11 V2 60.42(5) . . ?
V1 Se11 V2 70.63(5) 2_656 . ?
Se11 Se12 V1 60.69(5) . 2_656 ?
Se11 Se12 V2 65.30(5) . . ?
V2 Se12 V1 70.76(5) . 2_656 ?
Se22 Se21 V1 65.19(5) . . ?
Se22 Se21 V2 61.05(5) . . ?
V1 Se21 V2 70.45(5) . . ?
Se21 Se22 V1 60.72(5) . . ?
Se21 Se22 V2 64.83(5) . . ?
V2 Se22 V1 70.20(5) . . ?
I1 V1 I3 94.22(5) . . ?
I1 V1 V2 142.80(6) . . ?
I1 V1 V2 141.12(6) . 2_656 ?
I3 V1 V2 90.61(5) . . ?
I3 V1 V2 90.38(5) . 2_656 ?
Se11 V1 I1 96.60(5) 2_656 . ?
Se11 V1 I3 136.21(6) 2_656 . ?
Se11 V1 Se12 54.11(4) 2_656 2_656 ?
Se11 V1 Se22 137.07(7) 2_656 . ?
Se11 V1 V2 56.26(5) 2_656 2_656 ?
Se11 V1 V2 105.12(7) 2_656 . ?
Se12 V1 I1 89.32(5) 2_656 . ?
Se12 V1 I3 83.83(5) 2_656 . ?
Se12 V1 V2 127.88(6) 2_656 . ?
Se12 V1 V2 52.81(4) 2_656 2_656 ?
Se21 V1 I1 98.03(5) . . ?
Se21 V1 I3 137.02(6) . . ?
Se21 V1 Se11 82.98(6) . 2_656 ?
Se21 V1 Se12 137.06(7) . 2_656 ?
Se21 V1 Se22 54.10(4) . . ?
Se21 V1 V2 104.58(7) . 2_656 ?
Se21 V1 V2 56.26(5) . . ?
Se22 V1 I1 90.29(5) . . ?
Se22 V1 I3 84.96(5) . . ?
Se22 V1 Se12 168.72(8) . 2_656 ?
Se22 V1 V2 128.59(6) . 2_656 ?
Se22 V1 V2 53.40(4) . . ?
V2 V1 V2 75.55(6) . 2_656 ?
O1 V1 I1 167.2(2) . . ?
O1 V1 I3 73.1(2) . . ?
O1 V1 Se11 92.22(18) . 2_656 ?
O1 V1 Se12 88.39(6) . 2_656 ?
O1 V1 Se21 92.18(18) . . ?
O1 V1 Se22 89.51(6) . . ?
O1 V1 V2 40.98(9) . 2_656 ?
O1 V1 V2 41.23(9) . . ?
I2 V2 I3 94.36(5) . 1_565 ?
I2 V2 V1 142.23(6) . . ?
I2 V2 V1 142.32(6) . 2_656 ?
I3 V2 V1 90.23(5) 1_565 . ?
I3 V2 V1 90.01(5) 1_565 2_656 ?
Se11 V2 I2 90.05(5) . . ?
Se11 V2 I3 84.54(5) . 1_565 ?
Se11 V2 V1 53.11(4) . 2_656 ?
Se11 V2 V1 127.73(6) . . ?
Se12 V2 I2 97.86(5) . . ?
Se12 V2 I3 136.75(6) . 1_565 ?
Se12 V2 Se11 54.28(4) . . ?
Se12 V2 Se21 136.99(7) . . ?
Se12 V2 Se22 82.90(6) . . ?
Se12 V2 V1 104.17(7) . . ?
Se12 V2 V1 56.43(5) . 2_656 ?
Se21 V2 I2 89.90(5) . . ?
Se21 V2 I3 84.06(5) . 1_565 ?
Se21 V2 Se11 168.55(8) . . ?
Se21 V2 V1 127.77(6) . 2_656 ?
Se21 V2 V1 53.28(4) . . ?
Se22 V2 I2 97.29(5) . . ?
Se22 V2 I3 136.30(6) . 1_565 ?
Se22 V2 Se11 137.17(7) . . ?
Se22 V2 Se21 54.11(4) . . ?
Se22 V2 V1 105.10(7) . 2_656 ?
Se22 V2 V1 56.40(5) . . ?
V1 V2 V1 74.99(6) . 2_656 ?
O1 V2 I2 167.8(2) . . ?
O1 V2 I3 73.5(2) . 1_565 ?
O1 V2 Se11 88.76(6) . . ?
O1 V2 Se12 91.24(18) . . ?
O1 V2 Se21 88.89(6) . . ?
O1 V2 Se22 91.79(18) . . ?
O1 V2 V1 40.40(9) . 2_656 ?
O1 V2 V1 40.65(9) . . ?
V1 O1 V1 135.9(5) . 2_656 ?
V1 O1 V2 98.12(6) 2_656 2_656 ?
V1 O1 V2 98.62(6) 2_656 . ?
V1 O1 V2 98.12(6) . . ?
V1 O1 V2 98.62(6) . 2_656 ?
V2 O1 V2 134.4(4) . 2_656 ?
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
I1 V1 2.6808(16) . ?
I2 V2 2.6793(16) . ?
I3 V1 2.8395(18) . ?
I3 V1 2.8395(18) 2_656 ?
I3 V2 2.8396(18) 1_545 ?
I3 V2 2.8396(17) 2_646 ?
Se11 Se12 2.3172(14) . ?
Se11 V1 2.4940(18) 2_656 ?
Se11 V2 2.5931(16) . ?
Se12 V1 2.5963(16) 2_656 ?
Se12 V2 2.4822(18) . ?
Se21 Se22 2.3154(14) . ?
Se21 V1 2.4933(18) . ?
Se21 V2 2.5866(16) . ?
Se22 V1 2.5946(16) . ?
Se22 V2 2.5009(18) . ?
V1 Se11 2.4940(18) 2_656 ?
V1 Se12 2.5963(16) 2_656 ?
V1 V2 2.942(2) 2_656 ?
V1 V2 2.931(2) . ?
V1 O1 1.929(3) . ?
V2 I3 2.8396(17) 1_565 ?
V2 V1 2.942(2) 2_656 ?
V2 O1 1.951(3) . ?
O1 V1 1.929(3) 2_656 ?
O1 V2 1.951(3) 2_656 ?
