#------------------------------------------------------------------------------
#$Date: 2022-06-02 05:14:52 +0300 (Thu, 02 Jun 2022) $
#$Revision: 275738 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/89/2108983.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2108983
loop_
_publ_author_name
'Filatov, Evgeny'
'Lagunova, Varvara'
'Kochetygov, Ilia'
'Plyusnin, Pavel'
'Kuratieva, Natalia'
'Kostin, Gennadiy'
'Korenev, Sergey'
_publ_section_title
;
 Synthesis and investigation of the thermal properties of
 [Co(NH₃)₆][Co(C₂O₄)₃]·3H₂O and
 [Ir(NH₃)₆][Ir(C₂O₄)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       'φ 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/[σ²(Fo²)+(0.0141P)²+7.2472P] where P=(Fo²+2Fc²)/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     >2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.431
_shelx_estimated_absorpt_t_max   0.729
_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>'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.6667 0.3333 0.08004(2) 0.01547(8) Uani 1 3 d S T P . .
Co1 Co 0.0000 0.0000 0.0000 0.0172(2) Uani 1 6 d S T P . .
K1 K 0.3333 0.6667 0.03822(4) 0.0217(3) Uani 1 3 d S T P . .
K2 K 0.3333 0.6667 0.1667 0.0283(4) Uani 1 6 d S T P . .
O1 O 0.5179(3) 0.3765(3) 0.11451(8) 0.0234(5) Uani 1 1 d . . . . .
O2 O 0.6966(2) 0.5142(2) 0.04310(8) 0.0208(5) Uani 1 1 d . . . . .
O3 O 0.4024(3) 0.5104(3) 0.10575(9) 0.0377(6) Uani 1 1 d . . . . .
O4 O 0.5980(3) 0.6627(3) 0.03424(9) 0.0304(6) Uani 1 1 d . . . . .
N1 N 0.1590(3) 0.1575(3) 0.03811(11) 0.0283(7) Uani 1 1 d . . . . .
H1A H 0.2479 0.2028 0.0225 0.042 Uiso 1 1 calc R U . . .
H1B H 0.1700 0.1148 0.0639 0.042 Uiso 1 1 calc R U . . .
H1C H 0.1326 0.2279 0.0455 0.042 Uiso 1 1 calc R U . . .
C1 C 0.4974(4) 0.4780(4) 0.09466(11) 0.0217(7) Uani 1 1 d . . . . .
C2 C 0.6043(4) 0.5605(3) 0.05389(11) 0.0193(7) Uani 1 1 d . . . . .
O1W O 0.2420(9) 0.0704(9) 0.1268(2) 0.068(2) Uani 0.5 1 d . U P . .
O2W O 0.1778(12) -0.0544(12) 0.1227(3) 0.104(3) Uani 0.5 1 d . U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ir1 O2 94.01(9) 3_665 . ?
O2 Ir1 O2 94.00(9) 3_665 2_655 ?
O2 Ir1 O2 94.01(9) . 2_655 ?
O2 Ir1 O1 86.43(9) 3_665 2_655 ?
O2 Ir1 O1 175.97(8) . 2_655 ?
O2 Ir1 O1 81.97(8) 2_655 2_655 ?
O2 Ir1 O1 81.97(8) 3_665 3_665 ?
O2 Ir1 O1 86.43(9) . 3_665 ?
O2 Ir1 O1 175.97(8) 2_655 3_665 ?
O1 Ir1 O1 97.60(8) 2_655 3_665 ?
O2 Ir1 O1 175.97(8) 3_665 . ?
O2 Ir1 O1 81.97(8) . . ?
O2 Ir1 O1 86.43(9) 2_655 . ?
O1 Ir1 O1 97.60(8) 2_655 . ?
O1 Ir1 O1 97.60(8) 3_665 . ?
O2 Ir1 K1 57.62(6) 3_665 10_665 ?
O2 Ir1 K1 57.62(6) . 10_665 ?
O2 Ir1 K1 57.62(6) 2_655 10_665 ?
O1 Ir1 K1 119.68(6) 2_655 10_665 ?
O1 Ir1 K1 119.68(6) 3_665 10_665 ?
O1 Ir1 K1 119.68(6) . 10_665 ?
N1 Co1 N1 180.0 . 10 ?
N1 Co1 N1 89.31(13) . 12 ?
N1 Co1 N1 90.69(13) 10 12 ?
N1 Co1 N1 90.69(13) . 2 ?
N1 Co1 N1 89.31(13) 10 2 ?
N1 Co1 N1 89.31(13) 12 2 ?
N1 Co1 N1 89.31(13) . 11 ?
N1 Co1 N1 90.69(13) 10 11 ?
N1 Co1 N1 90.69(13) 12 11 ?
N1 Co1 N1 180.00(18) 2 11 ?
N1 Co1 N1 90.69(13) . 3 ?
N1 Co1 N1 89.31(13) 10 3 ?
N1 Co1 N1 180.0(2) 12 3 ?
N1 Co1 N1 90.69(13) 2 3 ?
N1 Co1 N1 89.31(13) 11 3 ?
O4 K1 O4 119.817(9) 2_665 3_565 ?
O4 K1 O4 119.816(9) 2_665 . ?
O4 K1 O4 119.817(9) 3_565 . ?
O4 K1 O3 83.27(8) 2_665 3_565 ?
O4 K1 O3 59.80(7) 3_565 3_565 ?
O4 K1 O3 135.26(8) . 3_565 ?
O4 K1 O3 59.80(7) 2_665 2_665 ?
O4 K1 O3 135.25(8) 3_565 2_665 ?
O4 K1 O3 83.28(8) . 2_665 ?
O3 K1 O3 76.70(8) 3_565 2_665 ?
O4 K1 O3 135.25(8) 2_665 . ?
O4 K1 O3 83.27(8) 3_565 . ?
O4 K1 O3 59.80(7) . . ?
O3 K1 O3 76.70(8) 3_565 . ?
O3 K1 O3 76.70(8) 2_665 . ?
O4 K1 O2 66.78(7) 2_665 12 ?
O4 K1 O2 75.43(7) 3_565 12 ?
O4 K1 O2 122.74(8) . 12 ?
O3 K1 O2 101.13(7) 3_565 12 ?
O3 K1 O2 126.46(6) 2_665 12 ?
O3 K1 O2 156.09(7) . 12 ?
O4 K1 O2 75.43(7) 2_665 11_565 ?
O4 K1 O2 122.75(8) 3_565 11_565 ?
O4 K1 O2 66.78(7) . 11_565 ?
O3 K1 O2 156.09(7) 3_565 11_565 ?
O3 K1 O2 101.13(7) 2_665 11_565 ?
O3 K1 O2 126.46(7) . 11_565 ?
O2 K1 O2 60.57(7) 12 11_565 ?
O4 K1 O2 122.75(8) 2_665 10_665 ?
O4 K1 O2 66.78(7) 3_565 10_665 ?
O4 K1 O2 75.43(7) . 10_665 ?
O3 K1 O2 126.46(7) 3_565 10_665 ?
O3 K1 O2 156.09(7) 2_665 10_665 ?
O3 K1 O2 101.13(7) . 10_665 ?
O2 K1 O2 60.57(7) 12 10_665 ?
O2 K1 O2 60.57(7) 11_565 10_665 ?
O4 K1 C2 18.14(7) 2_665 2_665 ?
O4 K1 C2 135.00(7) 3_565 2_665 ?
O4 K1 C2 105.09(7) . 2_665 ?
O3 K1 C2 86.98(8) 3_565 2_665 ?
O3 K1 C2 43.38(7) 2_665 2_665 ?
O3 K1 C2 120.08(8) . 2_665 ?
O2 K1 C2 83.23(7) 12 2_665 ?
O2 K1 C2 76.18(7) 11_565 2_665 ?
O2 K1 C2 132.92(7) 10_665 2_665 ?
O4 K1 C2 105.09(7) 2_665 3_565 ?
O4 K1 C2 18.14(7) 3_565 3_565 ?
O4 K1 C2 135.00(7) . 3_565 ?
O3 K1 C2 43.38(7) 3_565 3_565 ?
O3 K1 C2 120.08(8) 2_665 3_565 ?
O3 K1 C2 86.98(8) . 3_565 ?
O2 K1 C2 76.18(7) 12 3_565 ?
O2 K1 C2 132.92(7) 11_565 3_565 ?
O2 K1 C2 83.23(7) 10_665 3_565 ?
C2 K1 C2 118.26(2) 2_665 3_565 ?
O4 K1 C2 135.00(7) 2_665 . ?
O4 K1 C2 105.09(7) 3_565 . ?
O4 K1 C2 18.14(7) . . ?
O3 K1 C2 120.08(8) 3_565 . ?
O3 K1 C2 86.98(8) 2_665 . ?
O3 K1 C2 43.38(7) . . ?
O2 K1 C2 132.92(7) 12 . ?
O2 K1 C2 83.23(7) 11_565 . ?
O2 K1 C2 76.18(7) 10_665 . ?
C2 K1 C2 118.26(2) 2_665 . ?
C2 K1 C2 118.26(2) 3_565 . ?
O3 K2 O3 81.18(8) 13_565 14_455 ?
O3 K2 O3 81.18(8) 13_565 15 ?
O3 K2 O3 81.18(8) 14_455 15 ?
O3 K2 O3 98.81(8) 13_565 3_565 ?
O3 K2 O3 98.81(8) 14_455 3_565 ?
O3 K2 O3 180.0 15 3_565 ?
O3 K2 O3 98.82(8) 13_565 2_665 ?
O3 K2 O3 180.0 14_455 2_665 ?
O3 K2 O3 98.82(8) 15 2_665 ?
O3 K2 O3 81.19(8) 3_565 2_665 ?
O3 K2 O3 180.00(9) 13_565 . ?
O3 K2 O3 98.82(8) 14_455 . ?
O3 K2 O3 98.82(8) 15 . ?
O3 K2 O3 81.19(8) 3_565 . ?
O3 K2 O3 81.19(8) 2_665 . ?
O3 K2 K1 48.71(6) 13_565 13_565 ?
O3 K2 K1 48.71(6) 14_455 13_565 ?
O3 K2 K1 48.70(6) 15 13_565 ?
O3 K2 K1 131.29(6) 3_565 13_565 ?
O3 K2 K1 131.29(6) 2_665 13_565 ?
O3 K2 K1 131.29(6) . 13_565 ?
O3 K2 K1 131.29(6) 13_565 . ?
O3 K2 K1 131.29(6) 14_455 . ?
O3 K2 K1 131.30(6) 15 . ?
O3 K2 K1 48.71(6) 3_565 . ?
O3 K2 K1 48.71(6) 2_665 . ?
O3 K2 K1 48.71(6) . . ?
K1 K2 K1 180.0 13_565 . ?
C1 O1 Ir1 112.50(19) . . ?
C2 O2 Ir1 113.40(19) . . ?
C2 O2 K1 124.42(19) . 10_665 ?
Ir1 O2 K1 86.77(7) . 10_665 ?
C1 O3 K2 144.4(2) . . ?
C1 O3 K1 114.8(2) . . ?
K2 O3 K1 85.53(7) . . ?
C2 O4 K1 117.9(2) . . ?
Co1 N1 H1A 109.5 . . ?
Co1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
Co1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
O3 C1 O1 124.6(3) . . ?
O3 C1 C2 119.9(3) . . ?
O1 C1 C2 115.5(3) . . ?
O3 C1 K1 47.02(18) . . ?
O1 C1 K1 163.4(2) . . ?
C2 C1 K1 74.81(17) . . ?
O4 C2 O2 123.9(3) . . ?
O4 C2 C1 120.3(3) . . ?
O2 C2 C1 115.8(3) . . ?
O4 C2 K1 43.94(16) . . ?
O2 C2 K1 157.8(2) . . ?
C1 C2 K1 79.54(17) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 O2 2.028(2) 3_665 ?
Ir1 O2 2.028(2) . ?
Ir1 O2 2.028(2) 2_655 ?
Ir1 O1 2.048(2) 2_655 ?
Ir1 O1 2.048(2) 3_665 ?
Ir1 O1 2.048(2) . ?
Ir1 K1 3.4778(13) 10_665 ?
Co1 N1 1.965(3) . ?
Co1 N1 1.965(3) 10 ?
Co1 N1 1.965(3) 12 ?
Co1 N1 1.965(3) 2 ?
Co1 N1 1.965(3) 11 ?
Co1 N1 1.965(3) 3 ?
K1 O4 2.722(2) 2_665 ?
K1 O4 2.722(2) 3_565 ?
K1 O4 2.722(2) . ?
K1 O3 2.847(3) 3_565 ?
K1 O3 2.847(3) 2_665 ?
K1 O3 2.847(3) . ?
K1 O2 2.942(2) 12 ?
K1 O2 2.942(2) 11_565 ?
K1 O2 2.942(2) 10_665 ?
K1 C2 3.467(3) 2_665 ?
K1 C2 3.467(3) 3_565 ?
K1 C2 3.466(3) . ?
K2 O3 2.715(2) 13_565 ?
K2 O3 2.715(3) 14_455 ?
K2 O3 2.715(2) 15 ?
K2 O3 2.714(2) 3_565 ?
K2 O3 2.714(3) 2_665 ?
K2 O3 2.715(2) . ?
K2 K1 3.7773(13) 13_565 ?
O1 C1 1.294(4) . ?
O2 C2 1.286(4) . ?
O2 K1 2.942(2) 10_665 ?
O3 C1 1.214(4) . ?
O4 C2 1.221(4) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
C1 C2 1.555(4) . ?
O1W O2W 1.109(11) . ?
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{c66c15df-ec9e-491c-a855-34bbc8e35f57} ? ? ?
{feb1bbdb-9c86-43f6-924a-605af9f4c6de} y y y
{12bd4438-1f6e-4751-a664-4d34bdfd928f} y y y
{97a2415b-431c-45a0-96a0-a3e8a6ea8d71} y y y
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
loop_
_publcif_info_exptl_table_header_item
?
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
{c66c15df-ec9e-491c-a855-34bbc8e35f57} '_publcif_info_datablock.publ_exptl'
loop_
_publcif_info_cif.paper_type
CB

_cod_database_fobs_code 2108983
