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_7063408
_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         'C4 O9 V, 2(C16 H36 N)'
_chemical_formula_sum            'C36 H72 N2 O9 V'
_chemical_formula_weight         727.89
_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     iterative
_audit_creation_date             2024-06-24
_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                 120.899(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9092(19)
_cell_length_b                   13.9416(12)
_cell_length_c                   18.272(3)
_cell_measurement_reflns_used    4100
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.81
_cell_measurement_theta_min      2.51
_cell_volume                     4133.3(9)
_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(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
'Data collection was performed by Kochelakov D.V. 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  0.0738
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25901
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         2.511
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.'
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       block
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         5125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0400P)^2^+2.5035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3772
_reflns_number_total             5125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03084b2.cif
_cod_data_source_block           voc2o4
_cod_depositor_comments
'Adding full bibliography for 7063408--7063411.cif.'
_cod_original_cell_volume        4133.4(8)
_cod_database_code               7063408
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.974
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B)
1.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              13334
_olex2_submission_special_instructions 'No special instructions were received'