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#$Date: 2022-06-02 05:14:52 +0300 (Thu, 02 Jun 2022) $
#$Revision: 275738 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/89/2108982.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_2108982
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          '[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       '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  0.0340
_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/[σ²(Fo²)] where P=(Fo²+2Fc²)/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     >2σ(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_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   0.294
_shelx_estimated_absorpt_t_max   0.563
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.09273(2) 0.77320(2) 0.26275(2) 0.01794(5) Uani 1 1 d . . . . .
Ir2 Ir 0.53618(2) 0.24648(2) 0.23156(2) 0.02161(6) Uani 1 1 d . . . . .
O11 O 0.2861(5) 0.3030(4) 0.1528(3) 0.0311(8) Uani 1 1 d . . . . .
O12 O 0.6343(5) 0.1664(4) 0.0801(3) 0.0283(8) Uani 1 1 d . . . . .
O13 O 0.1646(5) 0.2229(5) 0.0159(3) 0.0395(10) Uani 1 1 d . . . . .
O14 O 0.5240(5) 0.1352(5) -0.0800(3) 0.0395(10) Uani 1 1 d . . . . .
O21 O 0.4276(5) 0.3222(4) 0.3817(3) 0.0277(8) Uani 1 1 d . . . . .
O22 O 0.4705(5) 0.0665(4) 0.2969(3) 0.0286(8) Uani 1 1 d . . . . .
O23 O 0.2916(5) 0.2561(4) 0.5359(3) 0.0338(9) Uani 1 1 d . . . . .
O24 O 0.3180(5) -0.0023(4) 0.4421(3) 0.0324(8) Uani 1 1 d . . . . .
O31 O 0.5988(5) 0.4303(4) 0.1756(3) 0.0294(8) Uani 1 1 d . . . . .
O32 O 0.7924(5) 0.1922(4) 0.3072(3) 0.0280(8) Uani 1 1 d . . . . .
O33 O 0.8078(6) 0.5377(5) 0.2054(4) 0.0539(12) Uani 1 1 d . . . . .
O34 O 0.9707(6) 0.3096(5) 0.3658(4) 0.0565(13) Uani 1 1 d . . . . .
N1 N 0.0973(7) 0.9646(5) 0.1678(4) 0.0476(14) Uani 1 1 d . . . . .
H1A H -0.0054 1.0007 0.1259 0.071 Uiso 1 1 calc R U . . .
H1B H 0.1984 0.9443 0.1232 0.071 Uiso 1 1 calc R U . . .
H1C H 0.1009 1.0303 0.2138 0.071 Uiso 1 1 calc R U . . .
N2 N 0.0129(6) 0.8884(5) 0.4022(3) 0.0271(9) Uani 1 1 d . . . . .
H2A H 0.1144 0.8848 0.4391 0.041 Uiso 0.5 1 calc R U P . .
H2B H -0.0525 0.9812 0.3808 0.041 Uiso 0.5 1 calc R U P . .
H2C H -0.0580 0.8492 0.4471 0.041 Uiso 0.5 1 calc R U P . .
H2D H -0.1118 0.9253 0.4056 0.041 Uiso 0.5 1 calc R U P . .
H2E H 0.0551 0.8289 0.4639 0.041 Uiso 0.5 1 calc R U P . .
H2F H 0.0606 0.9610 0.3976 0.041 Uiso 0.5 1 calc R U P . .
N3 N 0.0806(6) 0.5871(5) 0.3600(4) 0.0310(10) Uani 1 1 d . . . . .
H3A H 0.0180 0.6129 0.4236 0.047 Uiso 1 1 calc R U . . .
H3B H 0.1964 0.5279 0.3760 0.047 Uiso 1 1 calc R U . . .
H3C H 0.0221 0.5410 0.3220 0.047 Uiso 1 1 calc R U . . .
N4 N 0.1711(6) 0.6527(5) 0.1226(3) 0.0325(10) Uani 1 1 d . . . . .
H4A H 0.1468 0.5691 0.1360 0.049 Uiso 1 1 calc R U . . .
H4B H 0.2933 0.6334 0.1091 0.049 Uiso 1 1 calc R U . . .
H4C H 0.1067 0.7043 0.0630 0.049 Uiso 1 1 calc R U . . .
N5 N 0.3761(6) 0.7266(6) 0.3012(4) 0.0360(11) Uani 1 1 d . . . . .
H5A H 0.4440 0.7169 0.2380 0.054 Uiso 1 1 calc R U . . .
H5B H 0.4155 0.6437 0.3459 0.054 Uiso 1 1 calc R U . . .
H5C H 0.3889 0.7993 0.3362 0.054 Uiso 1 1 calc R U . . .
N6 N -0.1858(5) 0.8258(5) 0.2256(3) 0.0267(9) Uani 1 1 d . . . . .
H6A H -0.2523 0.9045 0.2597 0.040 Uiso 1 1 calc R U . . .
H6B H -0.2248 0.7511 0.2495 0.040 Uiso 1 1 calc R U . . .
H6C H -0.2010 0.8446 0.1515 0.040 Uiso 1 1 calc R U . . .
C11 C 0.2980(7) 0.2357(6) 0.0635(4) 0.0255(10) Uani 1 1 d . . . . .
C12 C 0.5002(7) 0.1724(6) 0.0155(4) 0.0258(10) Uani 1 1 d . . . . .
C21 C 0.3637(6) 0.2307(5) 0.4442(4) 0.0233(10) Uani 1 1 d . . . . .
C22 C 0.3825(6) 0.0862(6) 0.3927(4) 0.0234(10) Uani 1 1 d . . . . .
C31 C 0.7473(8) 0.4361(6) 0.2231(4) 0.0306(11) Uani 1 1 d . . . . .
C32 C 0.8479(7) 0.3037(6) 0.3063(5) 0.0291(11) Uani 1 1 d . . . . .
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'
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
N6 Ir1 N2 88.43(16) . . ?
N6 Ir1 N3 89.42(17) . . ?
N2 Ir1 N3 88.87(17) . . ?
N6 Ir1 N4 91.04(17) . . ?
N2 Ir1 N4 178.71(16) . . ?
N3 Ir1 N4 89.95(18) . . ?
N6 Ir1 N1 89.42(19) . . ?
N2 Ir1 N1 89.62(19) . . ?
N3 Ir1 N1 178.13(18) . . ?
N4 Ir1 N1 91.55(19) . . ?
N6 Ir1 N5 178.15(18) . . ?
N2 Ir1 N5 90.40(17) . . ?
N3 Ir1 N5 91.98(18) . . ?
N4 Ir1 N5 90.16(18) . . ?
N1 Ir1 N5 89.1(2) . . ?
O11 Ir2 O21 95.91(14) . . ?
O11 Ir2 O31 96.78(14) . . ?
O21 Ir2 O31 94.33(14) . . ?
O11 Ir2 O22 84.27(15) . . ?
O21 Ir2 O22 82.35(14) . . ?
O31 Ir2 O22 176.61(13) . . ?
O11 Ir2 O12 81.90(14) . . ?
O21 Ir2 O12 177.12(13) . . ?
O31 Ir2 O12 87.81(14) . . ?
O22 Ir2 O12 95.54(14) . . ?
O11 Ir2 O32 178.26(13) . . ?
O21 Ir2 O32 85.24(14) . . ?
O31 Ir2 O32 81.82(14) . . ?
O22 Ir2 O32 97.18(14) . . ?
O12 Ir2 O32 96.99(14) . . ?
C11 O11 Ir2 112.1(3) . . ?
C12 O12 Ir2 111.8(3) . . ?
C21 O21 Ir2 112.9(3) . . ?
C22 O22 Ir2 112.5(3) . . ?
C31 O31 Ir2 112.3(3) . . ?
C32 O32 Ir2 111.5(3) . . ?
O13 C11 O11 125.0(5) . . ?
O13 C11 C12 120.5(5) . . ?
O11 C11 C12 114.5(4) . . ?
O14 C12 O12 123.7(5) . . ?
O14 C12 C11 119.9(5) . . ?
O12 C12 C11 116.4(4) . . ?
O23 C21 O21 123.0(5) . . ?
O23 C21 C22 121.3(4) . . ?
O21 C21 C22 115.7(4) . . ?
O24 C22 O22 123.4(5) . . ?
O24 C22 C21 120.3(4) . . ?
O22 C22 C21 116.3(4) . . ?
O33 C31 O31 123.9(5) . . ?
O33 C31 C32 120.1(5) . . ?
O31 C31 C32 115.9(4) . . ?
O34 C32 O32 124.2(5) . . ?
O34 C32 C31 119.9(5) . . ?
O32 C32 C31 115.9(4) . . ?
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 N6 2.051(4) . ?
Ir1 N2 2.056(4) . ?
Ir1 N3 2.079(4) . ?
Ir1 N4 2.089(4) . ?
Ir1 N1 2.093(4) . ?
Ir1 N5 2.098(4) . ?
Ir2 O11 2.029(3) . ?
Ir2 O21 2.041(3) . ?
Ir2 O31 2.043(3) . ?
Ir2 O22 2.050(3) . ?
Ir2 O12 2.051(3) . ?
Ir2 O32 2.053(3) . ?
O11 C11 1.289(6) . ?
O12 C12 1.283(6) . ?
O13 C11 1.226(6) . ?
O14 C12 1.217(6) . ?
O21 C21 1.308(6) . ?
O22 C22 1.296(6) . ?
O23 C21 1.212(5) . ?
O24 C22 1.218(6) . ?
O31 C31 1.298(6) . ?
O32 C32 1.287(6) . ?
O33 C31 1.219(6) . ?
O34 C32 1.211(6) . ?
C11 C12 1.553(7) . ?
C21 C22 1.550(7) . ?
C31 C32 1.545(7) . ?

_cod_database_fobs_code 2108982
