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_2108981
_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          '[Co (N H3)6], [Co (C2 O4)3], 3(H2 O)'
_chemical_formula_moiety         'Co H18 N6 2+, C6 Co O12 2-, 3(H2 O)'
_chemical_formula_sum            'C6 H24 Co2 N6 O15'
_chemical_formula_weight         538.17
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   mixed
_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            6
_cell_length_a                   12.3686(2)
_cell_length_b                   12.3686(2)
_cell_length_c                   21.1962(4)
_cell_measurement_reflns_used    6138
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.70
_cell_volume                     2808.21(8)
_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 0.998
_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  0.0409
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23212
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         28.265
_diffrn_reflns_theta_min         2.130
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_description       prism
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_exptl_transmission_factor_max   0.745
_exptl_transmission_factor_min   0.646
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4663
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0390P)^2^+0.7848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3638
_reflns_number_total             4663
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            yh5018sup1.cif
_cod_data_source_block           fil002_CoNH36CoOx33H2O
_cod_original_cell_volume        2808.21(11)
_cod_database_code               2108981
_publcif_datablock.id            {feb1bbdb-9c86-43f6-924a-605af9f4c6de}
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.707
_shelx_estimated_absorpt_t_max   0.755
_shelx_res_checksum              57667
_shelx_hkl_checksum              88635
_cod_database_fobs_code 2108981