Double complex salts based on tetraamminplatinum(ii) and vanadyl(iv) bisoxalate for the preparation of bimetallic Pt–V alloys
Vorobyeva, Sofia N.; Rudzis, Zakhar V.; Sukhikh, Taisiya S.; Filatov, Evgeny Yu.; Plusnin, Pavel E.; Nadolinny, Vladimir A.; Bogomyakov, Artem S.; Korenev, Sergey V.; New Journal of Chemistry 48 (2024) 15894–15903; doi:10.1039/D4NJ03084B

data_7063411
_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 O9 V'
_chemical_formula_sum            'C4 H12 N4 O9 Pt V'
_chemical_formula_weight         506.21
_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_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 97.242(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.603(8)
_cell_length_b                   7.945(3)
_cell_length_c                   15.358(6)
_cell_measurement_reflns_used    175
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      17.27
_cell_measurement_theta_min      2.67
_cell_volume                     2372.9(16)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'Data collection was performed by Kochelakov D. in XRD Facility of NIIC SB RAS'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1196
_diffrn_reflns_av_unetI/netI     0.1500
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4516
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        23.261
_diffrn_reflns_theta_max         23.261
_diffrn_reflns_theta_min         2.674
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.618
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0868 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.7848.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.834
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.332
_refine_diff_density_min         -1.555
_refine_diff_density_rms         0.369
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         1703
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1070
_reflns_number_total             1703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03084b2.cif
_cod_data_source_block           bch-337-2
_cod_depositor_comments
'Adding full bibliography for 7063408--7063411.cif.'
_cod_original_cell_volume        2372.8(16)
_cod_database_code               7063411
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.571
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 O11, O12, O13, O14, C1, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O21, O22, O23, O24, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C)
;
_shelx_res_checksum              78576
_olex2_submission_special_instructions 'No special instructions were received'