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_7063410
_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       '\f and \w 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 \l/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/[\s^2^(Fo^2^)+(0.0143P)^2^+0.3056P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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)
;
_shelx_res_checksum              12951
_olex2_submission_special_instructions 'No special instructions were received'