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_2108982
_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          '[Ir (N H3)6] [Ir (C2 O4)4]'
_chemical_formula_moiety         'H18 Ir N6 3+, C6 Ir O12 3-'
_chemical_formula_sum            'C6 H18 Ir2 N6 O12'
_chemical_formula_weight         750.66
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                84.3680(10)
_cell_angle_beta                 87.5790(10)
_cell_angle_gamma                70.5340(10)
_cell_formula_units_Z            2
_cell_length_a                   7.5600(2)
_cell_length_b                   9.7304(3)
_cell_length_c                   11.9386(3)
_cell_measurement_reflns_used    4768
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.23
_cell_volume                     823.99(4)
_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      293(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.0340
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7770
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         28.320
_diffrn_reflns_theta_min         1.714
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.026
_exptl_crystal_description       plate
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.541
_refine_diff_density_max         1.454
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0221
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3532
_reflns_number_total             4063
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            yh5018sup1.cif
_cod_data_source_block           ko123_IrNH36IrOx3
_cod_database_code               2108982
_publcif_datablock.id            {12bd4438-1f6e-4751-a664-4d34bdfd928f}
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.294
_shelx_estimated_absorpt_t_max   0.563
_shelx_res_checksum              65721
_shelx_hkl_checksum              47693
_cod_database_fobs_code 2108982