Synthesis and investigation of the thermal properties of [Co(NH~3~)~6~][Co(C~2~O~4~)~3~]·3H~2~O and [Ir(NH~3~)~6~][Ir(C~2~O~4~)~3~]
Filatov, Evgeny; Lagunova, Varvara; Kochetygov, Ilia; Plyusnin, Pavel; Kuratieva, Natalia; Kostin, Gennadiy; Korenev, Sergey; Acta Crystallographica Section B 78 (2022) –; doi:10.1107/S205252062200405X

data_2108983
_publ_section_title
;
 Synthesis and investigation of the thermal properties of
 [Co(NH~3~)~6~][Co(C~2~O~4~)~3~]&#x00B7;3H~2~O and
 [Ir(NH~3~)~6~][Ir(C~2~O~4~)~3~]
;
_journal_coeditor_code           YH5018
_journal_issue                   '3 Part 2'
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205252062200405X
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          'K3 [Co (N H3)6] [Ir (C2 O4)3]2, 6H2 O'
_chemical_formula_moiety
'3(K +), Co H18 N6 3+, 2(C6 Ir O12 3-), 6(H2 O)'
_chemical_formula_sum            'C12 H30 Co Ir2 K3 N6 O30'
_chemical_formula_weight         1299.05
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.2003(8)
_cell_length_b                   10.2003(8)
_cell_length_c                   29.408(4)
_cell_measurement_reflns_used    3992
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.41
_cell_volume                     2649.9(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker--Nonius X8 APEX CCD area-detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            7274
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         26.380
_diffrn_reflns_theta_min         2.690
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.442
_exptl_crystal_description       plate
_exptl_crystal_F_000             1866
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_transmission_factor_max   0.745
_exptl_transmission_factor_min   0.590
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1200
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0184
_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^)+(0.0141P)^2^+7.2472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1135
_reflns_number_total             1200
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            yh5018sup1.cif
_cod_data_source_block           lav147_K3CoNH36IrOx32
_cod_original_cell_volume        2649.8(5)
_cod_database_code               2108983
_publcif_datablock.id            {97a2415b-431c-45a0-96a0-a3e8a6ea8d71}
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.431
_shelx_estimated_absorpt_t_max   0.729
_shelx_res_checksum              24833
_shelx_hkl_checksum              87146
_publcif_info_exptl_table_max_cols 5
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
'<span class="funder"><span class="fundref-name" data-id="501100006769">Russian Science Foundation</span><span class="fundref-subname" data-id=""></span> (<span class="fundref-grant-group"><span class="fundref-grant-type">grant</span> No. <span class="fundref-grant-id">21-73-20203</span> to <span class="fundref-grant-recipient">Evgeny Filatov</span></span>); </span><span class="funder"><span class="fundref-name" data-id="">Ministry of Science and Higher Education of the Russian Federation</span><span class="fundref-subname" data-id=""></span> (<span class="fundref-grant-group"><span class="fundref-grant-type">contract</span> No. <span class="fundref-grant-id">121031700315-2</span></span>; <span class="fundref-grant-group"><span class="fundref-grant-type">contract</span> No. <span class="fundref-grant-id">121031700313-8</span></span>).</span>'
_cod_database_fobs_code 2108983