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#$Date: 2024-10-06 12:05:32 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295311 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/34/7063410.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_7063410
loop_
_publ_author_name
'Vorobyeva, Sofia N.'
'Rudzis, Zakhar V.'
'Sukhikh, Taisiya S.'
'Filatov, Evgeny Yu.'
'Plusnin, Pavel E.'
'Nadolinny, Vladimir A.'
'Bogomyakov, Artem S.'
'Korenev, Sergey V.'
_publ_section_title
;
 Double complex salts based on tetraamminplatinum(ii) and vanadyl(iv)
 bisoxalate for the preparation of bimetallic Pt--V alloys
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15894
_journal_page_last               15903
_journal_paper_doi               10.1039/D4NJ03084B
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         '2(H6 N2 Pt0.5), C4 H2 O10 V, 2(H2 O)'
_chemical_formula_sum            'C4 H18 N4 O12 Pt V'
_chemical_formula_weight         560.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-06-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-08-09 deposited with the CCDC.	2024-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                108.1350(10)
_cell_angle_beta                 97.3040(10)
_cell_angle_gamma                95.7430(10)
_cell_formula_units_Z            2
_cell_length_a                   7.27950(10)
_cell_length_b                   8.24340(10)
_cell_length_c                   12.9863(2)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      33.12
_cell_measurement_theta_min      2.61
_cell_volume                     726.456(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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
'Data collection was performed by Sukhikh A.S. in XRD Facility of NIIC SB RAS'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15497
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.132
_diffrn_reflns_theta_min         1.674
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.331
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0681 before and 0.0359 after correction.
The Ratio of minimum to maximum transmission is 0.8040.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.561
_exptl_crystal_description       plate
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.611
_refine_diff_density_min         -1.578
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         5492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0192
_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)+(0.0143P)²+0.3056P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0414
_refine_ls_wR_factor_ref         0.0433
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4682
_reflns_number_total             5492
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4nj03084b2.cif
_cod_data_source_block           rzv-7
_cod_depositor_comments
'Adding full bibliography for 7063408--7063411.cif.'
_cod_original_cell_volume        726.455(18)
_cod_database_code               7063410
_shelx_shelxl_version_number     2017/1
_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   0.683
_shelx_estimated_absorpt_t_min   0.425
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O4(H4D,H4E), O5(H5A,H5B)
2.b Rotating group:
 O2(H2A,H2B)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_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
Pt1 Pt 1.000000 1.000000 0.500000 0.01062(3) Uani 1 2 d S . P . .
N1 N 1.0053(3) 0.7568(2) 0.50907(15) 0.0163(4) Uani 1 1 d . . . . .
H1A H 1.098572 0.709701 0.475108 0.020 Uiso 1 1 calc R U . . .
H1B H 0.893473 0.689937 0.475315 0.020 Uiso 1 1 calc R U . . .
H1C H 1.026356 0.762704 0.580829 0.020 Uiso 1 1 calc R U . . .
N2 N 0.9024(3) 1.0761(3) 0.64637(16) 0.0197(4) Uani 1 1 d . . . . .
H2C H 0.775011 1.062418 0.633198 0.024 Uiso 1 1 calc R U . . .
H2D H 0.948164 1.189156 0.683272 0.024 Uiso 1 1 calc R U . . .
H2E H 0.940559 1.010630 0.687620 0.024 Uiso 1 1 calc R U . . .
Pt2 Pt 0.500000 1.000000 1.000000 0.01358(3) Uani 1 2 d S . P . .
N3 N 0.6789(3) 1.0525(2) 0.90135(17) 0.0194(4) Uani 1 1 d . . . . .
H3A H 0.619662 1.013203 0.830246 0.023 Uiso 1 1 calc R U . . .
H3B H 0.781251 0.999176 0.907732 0.023 Uiso 1 1 calc R U . . .
H3C H 0.715325 1.168524 0.922182 0.023 Uiso 1 1 calc R U . . .
N4 N 0.2923(3) 0.8922(3) 0.86798(17) 0.0234(4) Uani 1 1 d . . . . .
H4A H 0.343502 0.854264 0.805974 0.028 Uiso 1 1 calc R U . . .
H4B H 0.218264 0.972355 0.861625 0.028 Uiso 1 1 calc R U . . .
H4C H 0.222133 0.801597 0.877287 0.028 Uiso 1 1 calc R U . . .
V1 V 0.81360(5) 0.60867(5) 0.76397(3) 0.01133(7) Uani 1 1 d . . . . .
O1 O 0.9015(2) 0.7563(2) 0.72006(13) 0.0180(3) Uani 1 1 d . . . . .
O2 O 1.0436(2) 0.4873(2) 0.76959(13) 0.0155(3) Uani 1 1 d . . . . .
H2A H 1.122268 0.521470 0.732526 0.023 Uiso 1 1 d R U . . .
H2B H 1.104137 0.521259 0.836836 0.023 Uiso 1 1 d R U . . .
O11 O 0.5459(2) 0.6466(2) 0.75061(12) 0.0154(3) Uani 1 1 d . . . . .
O12 O 0.7088(2) 0.4104(2) 0.62901(12) 0.0153(3) Uani 1 1 d . . . . .
O13 O 0.2708(2) 0.5510(2) 0.63802(13) 0.0189(3) Uani 1 1 d . . . . .
O14 O 0.4446(2) 0.2966(2) 0.50672(14) 0.0226(4) Uani 1 1 d . . . . .
O21 O 0.8897(2) 0.76538(19) 0.92351(12) 0.0142(3) Uani 1 1 d . . . . .
O22 O 0.7303(2) 0.44678(19) 0.85906(12) 0.0150(3) Uani 1 1 d . . . . .
O23 O 0.8926(2) 0.7908(2) 1.10065(13) 0.0178(3) Uani 1 1 d . . . . .
O24 O 0.7640(2) 0.4381(2) 1.03029(13) 0.0195(3) Uani 1 1 d . . . . .
C00K C 0.5335(3) 0.4025(3) 0.59054(17) 0.0143(4) Uani 1 1 d . . . . .
C00L C 0.8603(3) 0.7078(3) 1.00168(17) 0.0124(4) Uani 1 1 d . . . . .
C00M C 0.7770(3) 0.5142(3) 0.96226(17) 0.0127(4) Uani 1 1 d . . . . .
C00N C 0.4389(3) 0.5446(3) 0.66396(17) 0.0144(4) Uani 1 1 d . . . . .
O4 O 0.3632(3) 0.2685(2) 0.76107(15) 0.0260(4) Uani 1 1 d G . . . .
H4D H 0.279519 0.248409 0.799546 0.039 Uiso 1 1 d G U . . .
H4E H 0.467648 0.320090 0.804864 0.039 Uiso 1 1 d G U . . .
O5 O 0.4934(4) -0.0330(3) 0.66993(18) 0.0523(7) Uani 1 1 d G . . . .
H5A H 0.429141 0.048365 0.664751 0.078 Uiso 1 1 d G U . . .
H5B H 0.489541 -0.107028 0.604844 0.078 Uiso 1 1 d G U . . .
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'
Pt Pt -1.7033 8.3905 '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
N1 Pt1 N1 180.0 . 2_776 ?
N1 Pt1 N2 90.58(8) 2_776 2_776 ?
N1 Pt1 N2 90.58(8) . . ?
N1 Pt1 N2 89.42(8) . 2_776 ?
N1 Pt1 N2 89.42(8) 2_776 . ?
N2 Pt1 N2 180.0 . 2_776 ?
Pt1 N1 H1A 109.5 . . ?
Pt1 N1 H1B 109.5 . . ?
Pt1 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Pt1 N2 H2C 109.5 . . ?
Pt1 N2 H2D 109.5 . . ?
Pt1 N2 H2E 109.5 . . ?
H2C N2 H2D 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
N3 Pt2 N3 180.0 2_677 . ?
N4 Pt2 N3 89.14(9) 2_677 . ?
N4 Pt2 N3 90.86(8) 2_677 2_677 ?
N4 Pt2 N3 89.14(9) . 2_677 ?
N4 Pt2 N3 90.86(8) . . ?
N4 Pt2 N4 180.0 . 2_677 ?
Pt2 N3 H3A 109.5 . . ?
Pt2 N3 H3B 109.5 . . ?
Pt2 N3 H3C 109.5 . . ?
H3A N3 H3B 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
Pt2 N4 H4A 109.5 . . ?
Pt2 N4 H4B 109.5 . . ?
Pt2 N4 H4C 109.5 . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
O1 V1 O2 97.32(7) . . ?
O1 V1 O11 99.97(8) . . ?
O1 V1 O12 104.86(8) . . ?
O1 V1 O21 91.55(7) . . ?
O1 V1 O22 166.99(7) . . ?
O2 V1 O21 92.83(6) . . ?
O2 V1 O22 80.51(6) . . ?
O11 V1 O2 160.46(7) . . ?
O11 V1 O21 95.73(6) . . ?
O11 V1 O22 84.60(6) . . ?
O12 V1 O2 85.77(6) . . ?
O12 V1 O11 81.07(6) . . ?
O12 V1 O21 163.59(6) . . ?
O12 V1 O22 87.83(6) . . ?
O21 V1 O22 75.82(6) . . ?
V1 O2 H2A 109.5 . . ?
V1 O2 H2B 109.5 . . ?
H2A O2 H2B 104.4 . . ?
C00N O11 V1 114.99(13) . . ?
C00K O12 V1 115.72(13) . . ?
C00L O21 V1 120.06(13) . . ?
C00M O22 V1 115.36(13) . . ?
O12 C00K C00N 113.02(18) . . ?
O14 C00K O12 126.3(2) . . ?
O14 C00K C00N 120.7(2) . . ?
O21 C00L C00M 113.76(18) . . ?
O23 C00L O21 126.3(2) . . ?
O23 C00L C00M 119.90(18) . . ?
O22 C00M C00L 114.47(18) . . ?
O24 C00M O22 125.7(2) . . ?
O24 C00M C00L 119.80(19) . . ?
O11 C00N C00K 114.84(18) . . ?
O13 C00N O11 125.1(2) . . ?
O13 C00N C00K 120.0(2) . . ?
H4D O4 H4E 109.4 . . ?
H5A O5 H5B 109.5 . . ?
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
Pt1 N1 2.0485(18) . ?
Pt1 N1 2.0485(18) 2_776 ?
Pt1 N2 2.0500(18) . ?
Pt1 N2 2.0500(18) 2_776 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N2 H2C 0.9100 . ?
N2 H2D 0.9100 . ?
N2 H2E 0.9100 . ?
Pt2 N3 2.0446(19) 2_677 ?
Pt2 N3 2.0446(19) . ?
Pt2 N4 2.0345(19) . ?
Pt2 N4 2.035(2) 2_677 ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 H4C 0.9100 . ?
V1 O1 1.6080(16) . ?
V1 O2 2.0395(15) . ?
V1 O11 1.9985(15) . ?
V1 O12 1.9881(16) . ?
V1 O21 2.0413(15) . ?
V1 O22 2.1743(15) . ?
O2 H2A 0.8724 . ?
O2 H2B 0.8720 . ?
O11 C00N 1.279(3) . ?
O12 C00K 1.297(3) . ?
O13 C00N 1.238(3) . ?
O14 C00K 1.217(3) . ?
O21 C00L 1.279(2) . ?
O22 C00M 1.266(2) . ?
O23 C00L 1.232(2) . ?
O24 C00M 1.240(2) . ?
C00K C00N 1.546(3) . ?
C00L C00M 1.548(3) . ?
O4 H4D 0.8701 . ?
O4 H4E 0.8700 . ?
O5 H5A 0.8698 . ?
O5 H5B 0.8700 . ?
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
V1 O11 C00N O13 -176.96(17) . . . . ?
V1 O11 C00N C00K 4.5(2) . . . . ?
V1 O12 C00K O14 176.68(18) . . . . ?
V1 O12 C00K C00N -4.1(2) . . . . ?
V1 O21 C00L O23 -176.86(17) . . . . ?
V1 O21 C00L C00M 3.4(2) . . . . ?
V1 O22 C00M O24 -170.63(17) . . . . ?
V1 O22 C00M C00L 8.0(2) . . . . ?
O12 C00K C00N O11 -0.3(3) . . . . ?
O12 C00K C00N O13 -178.93(19) . . . . ?
O14 C00K C00N O11 179.0(2) . . . . ?
O14 C00K C00N O13 0.4(3) . . . . ?
O21 C00L C00M O22 -7.7(3) . . . . ?
O21 C00L C00M O24 171.01(19) . . . . ?
O23 C00L C00M O22 172.56(19) . . . . ?
O23 C00L C00M O24 -8.7(3) . . . . ?
