Double complex salts based on [Rh(NH3)6]3+ as precursors for Rh–Nb and Rh–V alloy systems: synthesis, structure, and thermal properties
Bautina, Sofia; Vorobyeva, Sofia; Rudzis, Zakhar; Rudneva, Yuliya; Nadolinny, Vladimir; Plusnin, Pavel; Sukhikh, Taisiya; Zhurenok, Angelina; Kozlova, Ekaterina; Korenev, Sergey; New Journal of Chemistry 49 (2025) 18753–18766; doi:10.1039/D5NJ03210E

data_7064044
_publ_section_title
;
 Double complex salts based on [Rh(NH3)6]3+ as precursors for Rh--Nb and
 Rh--V alloy systems: synthesis, structure, and thermal properties
;
_journal_issue                   43
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18753
_journal_page_last               18766
_journal_paper_doi               10.1039/D5NJ03210E
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'H18 N6 Rh, C6 Nb O13, 4(H2 O)'
_chemical_formula_sum            'C6 H26 N6 Nb O17 Rh'
_chemical_formula_weight         650.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-09-19
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-09-19 deposited with the CCDC.	2025-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.1610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2150(3)
_cell_length_b                   13.8259(5)
_cell_length_c                   16.4926(6)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      78.93
_cell_measurement_theta_min      4.21
_cell_volume                     2061.51(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16543
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.920
_diffrn_reflns_theta_min         4.206
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    11.906
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.5160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0814 before and 0.0392 after correction.
The Ratio of minimum to maximum transmission is 0.6842.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.458
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+1.2148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3888
_reflns_number_total             4318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03210e2.cif
_cod_data_source_block           bsa-59_rh_nb
_cod_depositor_comments
'Adding full bibliography for 7064043--7064045.cif.'
_cod_database_code               7064044
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.797
_shelx_estimated_absorpt_t_min   0.329
_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:
 O15(H15A,H15B), O17(H17A,H17B), O14(H14A,H14B), O16(H16A,H16B)
2.b Idealised Me refined as rotating group:
 N6(H6A,H6B,H6C), N2(H2A,H2B,H2C), N4(H4A,H4B,H4C), N3(H3A,H3B,H3C), N1(H1A,
 H1B,H1C), N5(H5A,H5B,H5C)
;
_shelx_res_checksum              64846
_olex2_submission_special_instructions 'No special instructions were received'