#------------------------------------------------------------------------------
#$Date: 2016-01-29 09:36:48 +0200 (Fri, 29 Jan 2016) $
#$Revision: 175271 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/40/7224055.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7224055
loop_
_publ_author_name
'Abramov, Pavel A.'
'Vicent, Cristian'
'Kompankov, Nikolay B.'
'Laricheva, Yuliya A.'
'Sokolov, Maksim Nailyevich'
_publ_section_title
;
 Unique solubility of polyoxoniobate salts in methanol: coordination to
 cations and POM methylation
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA23918D
_journal_year                    2016
_chemical_formula_structural     K4[{C10H15Ir}2Nb6O19]*10CH3OH*4H2O
_chemical_formula_sum            'C30 H78 Ir2 K4 Nb6 O33'
_chemical_formula_weight         2065.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-11 deposited with the CCDC.
2016-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                113.102(3)
_cell_angle_beta                 92.519(3)
_cell_angle_gamma                111.051(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7760(6)
_cell_length_b                   11.8756(7)
_cell_length_c                   14.1839(9)
_cell_measurement_reflns_used    6620
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      3.10
_cell_volume                     1521.58(17)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2004)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_computing_molecular_graphics    'SHELXLE (Sheldrick, 2011)'
_computing_publication_material  'CIFTAB-97 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18012
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_min         1.598
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.800
_exptl_absorpt_correction_T_max  0.722
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    2.254
_exptl_crystal_description       yellow
_exptl_crystal_F_000             998
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.697
_refine_diff_density_min         -2.619
_refine_diff_density_rms         0.628
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6901
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0333
_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)+(0.0764P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5935
_reflns_number_total             6901
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c5ra23918d2.cif
_cod_data_source_block           18
_cod_original_cell_volume        1521.58(16)
_cod_database_code               7224055
_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   0.477
_shelx_estimated_absorpt_t_max   0.722
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
C1 C 0.3736(8) 0.0031(8) 0.0819(6) 0.0157(12) Uani 1 1 d . U .
H1A H 0.4549 0.0388 0.0563 0.024 Uiso 1 1 calc R U .
H1B H 0.4012 0.0111 0.1519 0.024 Uiso 1 1 calc R U .
H1C H 0.3201 -0.0915 0.0337 0.024 Uiso 1 1 calc R U .
C2 C 0.2891(8) 0.0811(8) 0.0880(6) 0.0149(12) Uani 1 1 d . U .
C3 C 0.1633(8) 0.0568(7) 0.1222(6) 0.0137(12) Uani 1 1 d . U .
C5 C 0.1130(7) 0.1534(7) 0.1165(6) 0.0099(14) Uani 1 1 d . . .
C6 C 0.2118(8) 0.2381(7) 0.0800(6) 0.0135(16) Uani 1 1 d . . .
C7 C -0.0131(8) 0.1648(9) 0.1503(6) 0.0208(19) Uani 1 1 d . . .
H7A H -0.0596 0.0932 0.1709 0.031 Uiso 1 1 calc R U .
H7B H 0.0114 0.2522 0.2102 0.031 Uiso 1 1 calc R U .
H7C H -0.0737 0.1565 0.0921 0.031 Uiso 1 1 calc R U .
C8 C 0.2022(9) 0.3521(8) 0.0635(7) 0.0210(18) Uani 1 1 d . . .
H8A H 0.2820 0.3929 0.0386 0.032 Uiso 1 1 calc R U .
H8B H 0.1193 0.3185 0.0112 0.032 Uiso 1 1 calc R U .
H8C H 0.1990 0.4195 0.1300 0.032 Uiso 1 1 calc R U .
C9 C 0.3211(7) 0.1938(8) 0.0614(6) 0.0122(15) Uani 1 1 d . . .
C10 C 0.4430(9) 0.2478(10) 0.0207(7) 0.0239(19) Uani 1 1 d . . .
H10A H 0.4991 0.1975 0.0165 0.036 Uiso 1 1 calc R U .
H10B H 0.4137 0.2386 -0.0493 0.036 Uiso 1 1 calc R U .
H10C H 0.4964 0.3428 0.0682 0.036 Uiso 1 1 calc R U .
C11 C 0.0926(8) -0.0535(7) 0.1509(6) 0.0147(12) Uani 1 1 d . U .
H11A H 0.0086 -0.0481 0.1716 0.022 Uiso 1 1 calc R U .
H11B H 0.0704 -0.1399 0.0905 0.022 Uiso 1 1 calc R U .
H11C H 0.1521 -0.0455 0.2097 0.022 Uiso 1 1 calc R U .
C12 C 0.3169(9) 0.2878(9) 0.7750(7) 0.025(2) Uani 1 1 d . . .
H12A H 0.2771 0.3534 0.8036 0.037 Uiso 1 1 calc R U .
H12B H 0.3061 0.2363 0.8160 0.037 Uiso 1 1 calc R U .
H12C H 0.4139 0.3348 0.7787 0.037 Uiso 1 1 calc R U .
C13 C 0.3095(9) -0.1112(9) 0.7175(7) 0.0215(18) Uani 1 1 d . . .
H5 H 0.244(10) -0.139(9) 0.764(8) 0.026 Uiso 1 1 d . U .
H6 H 0.408(10) -0.051(9) 0.739(7) 0.026 Uiso 1 1 d . U .
H4 H 0.287(10) -0.015(9) 0.745(7) 0.026 Uiso 1 1 d . U .
C14 C 0.8096(10) 0.3878(10) 0.0184(7) 0.028(2) Uani 1 1 d . . .
O1 O 0.2490(5) 0.3318(5) 0.3678(4) 0.0055(10) Uani 1 1 d . . .
O2 O 0.4494(5) 0.4624(5) 0.2964(4) 0.0078(10) Uani 1 1 d . . .
O3 O 0.4595(5) 0.2638(5) 0.3312(4) 0.0069(10) Uani 1 1 d . . .
O4 O 0.7101(5) 0.6392(5) 0.4288(4) 0.0071(10) Uani 1 1 d . . .
O5 O 0.6946(5) 0.3977(5) 0.2520(4) 0.0093(10) Uani 1 1 d . . .
O6 O 0.5000 0.5000 0.5000 0.0053(13) Uiso 1 2 d S . P
O7 O 0.2202(5) 0.5484(5) 0.3248(4) 0.0099(10) Uani 1 1 d . . .
O8 O 0.2842(5) 0.5719(5) 0.5349(4) 0.0068(10) Uani 1 1 d . . .
O9 O 0.2421(5) 0.1012(5) 0.4065(4) 0.0106(11) Uani 1 1 d . . .
O10 O 0.4905(5) 0.7091(5) 0.4608(4) 0.0082(10) Uani 1 1 d . . .
O11 O -0.0412(5) 0.4350(5) 0.3566(4) 0.0127(11) Uani 1 1 d . . .
O12 O 0.2507(6) 0.2011(5) 0.6709(4) 0.0172(12) Uani 1 1 d . . .
O13 O 0.2529(5) -0.1908(5) 0.6084(4) 0.0152(12) Uani 1 1 d . . .
O14 O 0.0359(6) -0.0502(6) 0.6086(5) 0.0242(14) Uani 1 1 d . . .
O15 O 0.5547(6) 0.1309(5) 0.6201(4) 0.0172(12) Uani 1 1 d . . .
C15 C -0.0139(9) 0.3079(9) 0.7254(7) 0.0230(19) Uani 1 1 d . . .
H15A H 0.0362 0.4057 0.7603 0.035 Uiso 1 1 calc R U .
H15B H -0.0644 0.2779 0.7730 0.035 Uiso 1 1 calc R U .
H15C H 0.0503 0.2659 0.7065 0.035 Uiso 1 1 calc R U .
O16 O -0.1073(5) 0.2704(5) 0.6325(4) 0.0148(11) Uani 1 1 d . . .
C16 C 0.6119(9) 0.1875(9) 0.7291(7) 0.0229(19) Uani 1 1 d . . .
H16A H 0.7103 0.2392 0.7423 0.034 Uiso 1 1 calc R U .
H16B H 0.5700 0.2469 0.7692 0.034 Uiso 1 1 calc R U .
H16C H 0.5948 0.1155 0.7509 0.034 Uiso 1 1 calc R U .
O17 O 0.8163(7) 0.3270(6) 0.0873(5) 0.0247(14) Uani 1 1 d . . .
K1 K 0.02590(15) 0.32423(16) 0.47579(13) 0.0107(3) Uani 1 1 d . . .
K2 K 0.28654(17) -0.02846(16) 0.51320(13) 0.0142(3) Uani 1 1 d . . .
Nb1 Nb 0.34060(6) 0.53053(6) 0.40010(5) 0.00503(14) Uani 1 1 d . . .
Nb3 Nb 0.61265(6) 0.44375(6) 0.35673(5) 0.00519(14) Uani 1 1 d . . .
Nb4 Nb 0.35459(6) 0.26874(6) 0.44599(5) 0.00513(14) Uani 1 1 d . . .
Ir1 Ir 0.30904(3) 0.25583(3) 0.22260(2) 0.00611(10) 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'
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'
Nb Nb -2.0727 0.6215 '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
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C3 C2 C9 108.9(6) . .
C3 C2 C1 124.9(7) . .
C9 C2 C1 126.2(7) . .
C3 C2 Ir1 70.8(4) . .
C9 C2 Ir1 70.2(4) . .
C1 C2 Ir1 124.6(5) . .
C2 C3 C5 108.0(7) . .
C2 C3 C11 125.4(7) . .
C5 C3 C11 126.4(7) . .
C2 C3 Ir1 70.0(4) . .
C5 C3 Ir1 70.7(4) . .
C11 C3 Ir1 128.1(5) . .
C6 C5 C3 107.4(7) . .
C6 C5 C7 128.0(7) . .
C3 C5 C7 124.4(7) . .
C6 C5 Ir1 69.5(4) . .
C3 C5 Ir1 69.5(4) . .
C7 C5 Ir1 123.0(5) . .
C5 C6 C9 108.7(7) . .
C5 C6 C8 125.7(7) . .
C9 C6 C8 125.6(7) . .
C5 C6 Ir1 71.0(4) . .
C9 C6 Ir1 70.2(4) . .
C8 C6 Ir1 125.0(5) . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C6 C9 C2 107.0(6) . .
C6 C9 C10 128.1(8) . .
C2 C9 C10 124.9(7) . .
C6 C9 Ir1 70.1(4) . .
C2 C9 Ir1 69.7(4) . .
C10 C9 Ir1 126.2(5) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C3 C11 H11A 109.5 . .
C3 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C3 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
O12 C12 H12A 109.5 . .
O12 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
O12 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
O13 C13 K2 47.9(4) . .
O13 C13 H5 113(5) . .
K2 C13 H5 136(5) . .
O13 C13 H6 118(6) . .
K2 C13 H6 89(6) . .
H5 C13 H6 128(8) . .
O13 C13 H4 109(5) . .
K2 C13 H4 70(5) . .
H5 C13 H4 86(7) . .
H6 C13 H4 88(7) . .
Nb1 O1 Nb4 115.3(2) . .
Nb1 O1 Ir1 96.8(2) . .
Nb4 O1 Ir1 96.18(19) . .
Nb1 O1 K1 101.97(18) . .
Nb4 O1 K1 100.13(18) . .
Ir1 O1 K1 146.8(2) . .
Nb1 O2 Nb3 115.8(2) . .
Nb1 O2 Ir1 97.3(2) . .
Nb3 O2 Ir1 99.4(2) . .
Nb4 O3 Nb3 115.6(2) . .
Nb4 O3 Ir1 97.4(2) . .
Nb3 O3 Ir1 99.1(2) . .
Nb3 O4 Nb4 115.6(2) . 2_666
Nb3 O4 K1 102.67(19) . 2_666
Nb4 O4 K1 101.73(18) 2_666 2_666
Nb1 O6 Nb1 180.0 2_666 .
Nb1 O6 Nb4 87.18(2) 2_666 .
Nb1 O6 Nb4 92.82(2) . .
Nb1 O6 Nb4 92.82(2) 2_666 2_666
Nb1 O6 Nb4 87.17(2) . 2_666
Nb4 O6 Nb4 180.0 . 2_666
Nb1 O6 Nb3 88.22(2) 2_666 .
Nb1 O6 Nb3 91.77(2) . .
Nb4 O6 Nb3 91.78(2) . .
Nb4 O6 Nb3 88.22(2) 2_666 .
Nb1 O6 Nb3 91.78(2) 2_666 2_666
Nb1 O6 Nb3 88.23(2) . 2_666
Nb4 O6 Nb3 88.22(2) . 2_666
Nb4 O6 Nb3 91.78(2) 2_666 2_666
Nb3 O6 Nb3 180.0 . 2_666
Nb1 O8 Nb3 116.6(2) . 2_666
Nb1 O8 K1 100.45(19) . .
Nb3 O8 K1 98.81(18) 2_666 .
Nb4 O9 K2 118.5(2) . .
Nb4 O10 Nb1 115.1(2) 2_666 .
K1 O11 K1 97.73(17) . 2_566
C12 O12 K2 132.3(5) . .
C13 O13 K2 109.1(5) . .
C13 O13 K1 123.3(5) . 2_556
K2 O13 K1 92.60(16) . 2_556
K1 O14 K2 85.33(16) 2_556 .
C16 O15 K2 129.3(5) . .
C16 O15 K2 114.4(5) . 2_656
K2 O15 K2 105.81(19) . 2_656
O16 C15 H15A 109.5 . .
O16 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
O16 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C15 O16 K2 131.4(5) . 2_556
C15 O16 K1 112.9(5) . .
K2 O16 K1 91.02(17) 2_556 .
O15 C16 H16A 109.5 . .
O15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
O15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
O11 K1 O13 71.40(16) . 2_556
O11 K1 O14 121.15(18) . 2_556
O13 K1 O14 73.26(16) 2_556 2_556
O11 K1 O16 126.77(16) . .
O13 K1 O16 71.94(16) 2_556 .
O14 K1 O16 82.24(18) 2_556 .
O11 K1 O11 82.27(17) . 2_566
O13 K1 O11 101.22(16) 2_556 2_566
O14 K1 O11 150.45(18) 2_556 2_566
O16 K1 O11 68.65(15) . 2_566
O11 K1 O1 83.94(15) . .
O13 K1 O1 128.80(16) 2_556 .
O14 K1 O1 83.33(16) 2_556 .
O16 K1 O1 149.15(15) . .
O11 K1 O1 119.44(15) 2_566 .
O11 K1 O4 130.72(16) . 2_666
O13 K1 O4 156.19(16) 2_556 2_666
O14 K1 O4 85.60(16) 2_556 2_666
O16 K1 O4 94.87(15) . 2_666
O11 K1 O4 91.73(15) 2_566 2_666
O1 K1 O4 56.88(14) . 2_666
O11 K1 O8 78.49(15) . .
O13 K1 O8 147.98(15) 2_556 .
O14 K1 O8 134.11(16) 2_556 .
O16 K1 O8 121.00(15) . .
O11 K1 O8 63.42(14) 2_566 .
O1 K1 O8 56.07(14) . .
O4 K1 O8 55.82(14) 2_666 .
O11 K1 Nb3 108.76(12) . 2_666
O13 K1 Nb3 167.41(13) 2_556 2_666
O14 K1 Nb3 115.38(13) 2_556 2_666
O16 K1 Nb3 99.42(11) . 2_666
O11 K1 Nb3 66.65(11) 2_566 2_666
O1 K1 Nb3 63.02(10) . 2_666
O4 K1 Nb3 29.81(10) 2_666 2_666
O8 K1 Nb3 30.35(9) . 2_666
O11 K1 Nb4 115.62(12) . .
O13 K1 Nb4 140.35(13) 2_556 .
O14 K1 Nb4 70.38(12) 2_556 .
O16 K1 Nb4 117.32(11) . .
O11 K1 Nb4 118.22(11) 2_566 .
O1 K1 Nb4 31.84(9) . .
O4 K1 Nb4 30.53(10) 2_666 .
O8 K1 Nb4 63.81(9) . .
Nb3 K1 Nb4 51.57(2) 2_666 .
O11 K1 Nb1 67.70(12) . .
O13 K1 Nb1 135.44(13) 2_556 .
O14 K1 Nb1 114.38(14) 2_556 .
O16 K1 Nb1 149.87(12) . .
O11 K1 Nb1 90.22(11) 2_566 .
O1 K1 Nb1 31.07(10) . .
O4 K1 Nb1 63.44(10) 2_666 .
O8 K1 Nb1 29.79(10) . .
Nb3 K1 Nb1 51.25(2) 2_666 .
Nb4 K1 Nb1 53.37(2) . .
O11 K1 K2 114.21(12) . 2_556
O13 K1 K2 42.81(11) 2_556 2_556
O14 K1 K2 50.08(13) 2_556 2_556
O16 K1 K2 42.87(11) . 2_556
O11 K1 K2 105.97(12) 2_566 2_556
O1 K1 K2 133.23(11) . 2_556
O4 K1 K2 114.45(11) 2_666 2_556
O8 K1 K2 163.20(11) . 2_556
Nb3 K1 K2 134.96(5) 2_666 2_556
Nb4 K1 K2 115.86(5) . 2_556
Nb1 K1 K2 163.80(5) . 2_556
O9 K2 O16 93.37(16) . 2_556
O9 K2 O13 163.58(17) . .
O16 K2 O13 75.83(17) 2_556 .
O9 K2 O15 102.50(16) . .
O16 K2 O15 146.54(17) 2_556 .
O13 K2 O15 93.11(16) . .
O9 K2 O15 93.74(17) . 2_656
O16 K2 O15 75.56(17) 2_556 2_656
O13 K2 O15 95.43(17) . 2_656
O15 K2 O15 74.19(19) . 2_656
O9 K2 O12 75.54(16) . .
O16 K2 O12 132.32(17) 2_556 .
O13 K2 O12 102.40(17) . .
O15 K2 O12 80.60(17) . .
O15 K2 O12 149.78(17) 2_656 .
O9 K2 O14 95.80(17) . .
O16 K2 O14 80.30(17) 2_556 .
O13 K2 O14 70.47(17) . .
O15 K2 O14 126.18(18) . .
O15 K2 O14 154.49(17) 2_656 .
O12 K2 O14 55.73(16) . .
O9 K2 C13 158.9(2) . .
O16 K2 C13 98.3(2) 2_556 .
O13 K2 C13 23.02(19) . .
O15 K2 C13 76.93(19) . .
O15 K2 C13 106.2(2) 2_656 .
O12 K2 C13 83.62(19) . .
O14 K2 C13 69.1(2) . .
O9 K2 Nb4 23.67(11) . .
O16 K2 Nb4 116.44(13) 2_556 .
O13 K2 Nb4 166.08(13) . .
O15 K2 Nb4 79.86(11) . .
O15 K2 Nb4 94.18(12) 2_656 .
O12 K2 Nb4 64.76(11) . .
O14 K2 Nb4 103.94(12) . .
C13 K2 Nb4 143.33(16) . .
O9 K2 K1 119.18(12) . 2_556
O16 K2 K1 46.11(13) 2_556 2_556
O13 K2 K1 44.59(12) . 2_556
O15 K2 K1 137.07(12) . 2_556
O15 K2 K1 110.53(12) 2_656 2_556
O12 K2 K1 99.24(12) . 2_556
O14 K2 K1 44.60(11) . 2_556
C13 K2 K1 60.56(15) . 2_556
Nb4 K2 K1 139.13(5) . 2_556
O9 K2 K2 100.11(12) . 2_656
O16 K2 K2 111.12(13) 2_556 2_656
O13 K2 K2 95.37(13) . 2_656
O15 K2 K2 37.50(12) . 2_656
O15 K2 K2 36.69(11) 2_656 2_656
O12 K2 K2 116.44(13) . 2_656
O14 K2 K2 159.65(14) . 2_656
C13 K2 K2 92.04(16) . 2_656
Nb4 K2 K2 86.38(5) . 2_656
K1 K2 K2 132.58(6) 2_556 2_656
O7 Nb1 O10 102.7(2) . .
O7 Nb1 O8 102.4(2) . .
O10 Nb1 O8 89.8(2) . .
O7 Nb1 O2 103.5(2) . .
O10 Nb1 O2 89.3(2) . .
O8 Nb1 O2 153.6(2) . .
O7 Nb1 O1 102.4(2) . .
O10 Nb1 O1 154.7(2) . .
O8 Nb1 O1 87.8(2) . .
O2 Nb1 O1 81.9(2) . .
O7 Nb1 O6 178.47(17) . .
O10 Nb1 O6 78.84(14) . .
O8 Nb1 O6 77.74(14) . .
O2 Nb1 O6 76.23(14) . .
O1 Nb1 O6 76.02(13) . .
O7 Nb1 Ir1 93.87(17) . .
O10 Nb1 Ir1 131.98(15) . .
O8 Nb1 Ir1 130.32(14) . .
O2 Nb1 Ir1 42.76(14) . .
O1 Nb1 Ir1 42.64(14) . .
O6 Nb1 Ir1 84.890(19) . .
O7 Nb1 Nb4 135.08(17) . 2_666
O10 Nb1 Nb4 32.42(14) . 2_666
O8 Nb1 Nb4 82.35(14) . 2_666
O2 Nb1 Nb4 82.86(14) . 2_666
O1 Nb1 Nb4 122.44(13) . 2_666
O6 Nb1 Nb4 46.439(15) . 2_666
Ir1 Nb1 Nb4 117.11(2) . 2_666
O7 Nb1 Nb3 134.11(17) . 2_666
O10 Nb1 Nb3 84.44(15) . 2_666
O8 Nb1 Nb3 31.71(14) . 2_666
O2 Nb1 Nb3 122.08(14) . 2_666
O1 Nb1 Nb3 80.35(13) . 2_666
O6 Nb1 Nb3 46.035(15) . 2_666
Ir1 Nb1 Nb3 114.92(2) . 2_666
Nb4 Nb1 Nb3 62.525(18) 2_666 2_666
O7 Nb1 K1 84.69(17) . .
O10 Nb1 K1 139.26(15) . .
O8 Nb1 K1 49.76(14) . .
O2 Nb1 K1 128.38(14) . .
O1 Nb1 K1 46.96(14) . .
O6 Nb1 K1 94.33(3) . .
Ir1 Nb1 K1 86.39(3) . .
Nb4 Nb1 K1 126.24(3) 2_666 .
Nb3 Nb1 K1 63.73(3) 2_666 .
O5 Nb3 O4 103.2(2) . .
O5 Nb3 O8 101.5(2) . 2_666
O4 Nb3 O8 89.9(2) . 2_666
O5 Nb3 O2 105.4(2) . .
O4 Nb3 O2 90.21(19) . .
O8 Nb3 O2 152.4(2) 2_666 .
O5 Nb3 O3 103.0(2) . .
O4 Nb3 O3 153.6(2) . .
O8 Nb3 O3 88.00(19) 2_666 .
O2 Nb3 O3 79.79(19) . .
O5 Nb3 O6 178.16(17) . .
O4 Nb3 O6 78.30(15) . .
O8 Nb3 O6 77.41(14) 2_666 .
O2 Nb3 O6 75.59(14) . .
O3 Nb3 O6 75.56(14) . .
O5 Nb3 Ir1 96.38(16) . .
O4 Nb3 Ir1 131.40(14) . .
O8 Nb3 Ir1 129.12(14) 2_666 .
O2 Nb3 Ir1 41.46(14) . .
O3 Nb3 Ir1 41.40(13) . .
O6 Nb3 Ir1 83.296(18) . .
O5 Nb3 Nb1 133.14(16) . 2_666
O4 Nb3 Nb1 83.13(14) . 2_666
O8 Nb3 Nb1 31.67(14) 2_666 2_666
O2 Nb3 Nb1 121.15(15) . 2_666
O3 Nb3 Nb1 81.37(13) . 2_666
O6 Nb3 Nb1 45.741(15) . 2_666
Ir1 Nb3 Nb1 114.05(2) . 2_666
O5 Nb3 Nb4 135.75(17) . 2_666
O4 Nb3 Nb4 32.55(15) . 2_666
O8 Nb3 Nb4 83.85(14) 2_666 2_666
O2 Nb3 Nb4 81.54(14) . 2_666
O3 Nb3 Nb4 121.16(14) . 2_666
O6 Nb3 Nb4 45.770(15) . 2_666
Ir1 Nb3 Nb4 114.21(2) . 2_666
Nb1 Nb3 Nb4 62.547(19) 2_666 2_666
O5 Nb3 K1 85.16(16) . 2_666
O4 Nb3 K1 47.52(14) . 2_666
O8 Nb3 K1 50.84(14) 2_666 2_666
O2 Nb3 K1 137.61(14) . 2_666
O3 Nb3 K1 138.74(13) . 2_666
O6 Nb3 K1 95.18(3) . 2_666
Ir1 Nb3 K1 178.38(3) . 2_666
Nb1 Nb3 K1 65.02(3) 2_666 2_666
Nb4 Nb3 K1 64.22(3) 2_666 2_666
O9 Nb4 O10 103.1(2) . 2_666
O9 Nb4 O4 100.6(2) . 2_666
O10 Nb4 O4 89.4(2) 2_666 2_666
O9 Nb4 O3 104.8(2) . .
O10 Nb4 O3 91.5(2) 2_666 .
O4 Nb4 O3 153.7(2) 2_666 .
O9 Nb4 O1 102.2(2) . .
O10 Nb4 O1 154.6(2) 2_666 .
O4 Nb4 O1 86.03(19) 2_666 .
O3 Nb4 O1 82.04(19) . .
O9 Nb4 O6 177.55(17) . .
O10 Nb4 O6 78.86(14) 2_666 .
O4 Nb4 O6 77.89(14) 2_666 .
O3 Nb4 O6 76.50(14) . .
O1 Nb4 O6 75.80(13) . .
O9 Nb4 Ir1 94.51(17) . .
O10 Nb4 Ir1 134.09(15) 2_666 .
O4 Nb4 Ir1 128.77(14) 2_666 .
O3 Nb4 Ir1 42.79(13) . .
O1 Nb4 Ir1 42.83(14) . .
O6 Nb4 Ir1 85.022(19) . .
O9 Nb4 Nb1 135.61(16) . 2_666
O10 Nb4 Nb1 32.49(14) 2_666 2_666
O4 Nb4 Nb1 83.77(13) 2_666 2_666
O3 Nb4 Nb1 82.92(13) . 2_666
O1 Nb4 Nb1 122.16(13) . 2_666
O6 Nb4 Nb1 46.385(15) . 2_666
Ir1 Nb4 Nb1 117.12(2) . 2_666
O9 Nb4 Nb3 132.49(18) . 2_666
O10 Nb4 Nb3 82.79(15) 2_666 2_666
O4 Nb4 Nb3 31.89(14) 2_666 2_666
O3 Nb4 Nb3 122.33(14) . 2_666
O1 Nb4 Nb3 80.19(14) . 2_666
O6 Nb4 Nb3 46.012(16) . 2_666
Ir1 Nb4 Nb3 115.08(2) . 2_666
Nb1 Nb4 Nb3 62.477(19) 2_666 2_666
O9 Nb4 K2 37.84(16) . .
O10 Nb4 K2 66.45(14) 2_666 .
O4 Nb4 K2 90.84(14) 2_666 .
O3 Nb4 K2 113.52(14) . .
O1 Nb4 K2 138.44(14) . .
O6 Nb4 K2 143.67(3) . .
Ir1 Nb4 K2 126.91(3) . .
Nb1 Nb4 K2 98.55(3) 2_666 .
Nb3 Nb4 K2 115.99(3) 2_666 .
O9 Nb4 K1 82.22(17) . .
O10 Nb4 K1 136.57(15) 2_666 .
O4 Nb4 K1 47.74(13) 2_666 .
O3 Nb4 K1 129.40(13) . .
O1 Nb4 K1 48.03(14) . .
O6 Nb4 K1 95.34(3) . .
Ir1 Nb4 K1 87.22(3) . .
Nb1 Nb4 K1 126.64(3) 2_666 .
Nb3 Nb4 K1 64.21(3) 2_666 .
K2 Nb4 K1 102.30(4) . .
C2 Ir1 O1 145.9(3) . .
C2 Ir1 C6 66.5(3) . .
O1 Ir1 C6 122.8(3) . .
C2 Ir1 C9 40.0(3) . .
O1 Ir1 C9 162.4(2) . .
C6 Ir1 C9 39.6(3) . .
C2 Ir1 O3 100.1(2) . .
O1 Ir1 O3 77.54(18) . .
C6 Ir1 O3 159.1(3) . .
C9 Ir1 O3 119.9(2) . .
C2 Ir1 C3 39.2(3) . .
O1 Ir1 C3 110.2(3) . .
C6 Ir1 C3 66.6(3) . .
C9 Ir1 C3 66.7(3) . .
O3 Ir1 C3 113.8(2) . .
C2 Ir1 O2 135.9(3) . .
O1 Ir1 O2 77.22(19) . .
C6 Ir1 O2 102.2(2) . .
C9 Ir1 O2 103.5(2) . .
O3 Ir1 O2 75.86(18) . .
C3 Ir1 O2 168.5(2) . .
C2 Ir1 C5 66.2(3) . .
O1 Ir1 C5 99.6(2) . .
C6 Ir1 C5 39.5(3) . .
C9 Ir1 C5 66.5(3) . .
O3 Ir1 C5 151.2(2) . .
C3 Ir1 C5 39.7(3) . .
O2 Ir1 C5 132.0(2) . .
C2 Ir1 Nb4 120.1(2) . .
O1 Ir1 Nb4 40.98(12) . .
C6 Ir1 Nb4 160.8(2) . .
C9 Ir1 Nb4 156.0(2) . .
O3 Ir1 Nb4 39.86(14) . .
C3 Ir1 Nb4 106.3(2) . .
O2 Ir1 Nb4 85.09(14) . .
C5 Ir1 Nb4 123.7(2) . .
C2 Ir1 Nb1 172.4(2) . .
O1 Ir1 Nb1 40.56(13) . .
C6 Ir1 Nb1 106.9(2) . .
C9 Ir1 Nb1 132.4(2) . .
O3 Ir1 Nb1 85.18(13) . .
C3 Ir1 Nb1 143.1(2) . .
O2 Ir1 Nb1 39.90(14) . .
C5 Ir1 Nb1 111.5(2) . .
Nb4 Ir1 Nb1 67.449(17) . .
C2 Ir1 Nb3 114.7(2) . .
O1 Ir1 Nb3 85.32(12) . .
C6 Ir1 Nb3 129.7(2) . .
C9 Ir1 Nb3 106.53(19) . .
O3 Ir1 Nb3 39.53(13) . .
C3 Ir1 Nb3 147.2(2) . .
O2 Ir1 Nb3 39.19(13) . .
C5 Ir1 Nb3 168.9(2) . .
Nb4 Ir1 Nb3 66.199(17) . .
Nb1 Ir1 Nb3 66.078(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.498(10) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.430(11) .
C2 C9 1.460(11) .
C2 Ir1 2.129(8) .
C3 C5 1.460(11) .
C3 C11 1.480(11) .
C3 Ir1 2.139(7) .
C5 C6 1.449(11) .
C5 C7 1.495(11) .
C5 Ir1 2.155(7) .
C6 C9 1.448(11) .
C6 C8 1.498(11) .
C6 Ir1 2.134(7) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.491(11) .
C9 Ir1 2.135(7) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 O12 1.391(10) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 O13 1.419(10) .
C13 K2 3.431(9) .
C13 H5 1.04(10) .
C13 H6 1.00(10) .
C13 H4 1.17(10) .
C14 O17 1.437(11) .
O1 Nb1 2.048(5) .
O1 Nb4 2.058(5) .
O1 Ir1 2.133(5) .
O1 K1 2.900(5) .
O2 Nb1 2.023(5) .
O2 Nb3 2.043(5) .
O2 Ir1 2.141(5) .
O3 Nb4 2.016(5) .
O3 Nb3 2.056(5) .
O3 Ir1 2.137(5) .
O4 Nb3 1.957(5) .
O4 Nb4 1.993(5) 2_666
O4 K1 2.903(5) 2_666
O5 Nb3 1.763(5) .
O6 Nb1 2.3930(6) 2_666
O6 Nb1 2.3930(6) .
O6 Nb4 2.3951(6) .
O6 Nb4 2.3951(6) 2_666
O6 Nb3 2.4050(6) .
O6 Nb3 2.4050(6) 2_666
O7 Nb1 1.767(5) .
O8 Nb1 1.961(5) .
O8 Nb3 1.964(5) 2_666
O8 K1 3.013(5) .
O9 Nb4 1.754(5) .
O9 K2 2.680(5) .
O10 Nb4 1.954(5) 2_666
O10 Nb1 1.958(5) .
O11 K1 2.725(6) .
O11 K1 2.855(6) 2_566
O12 K2 2.938(6) .
O13 K2 2.694(6) .
O13 K1 2.783(5) 2_556
O14 K1 2.789(6) 2_556
O14 K2 3.047(6) .
O15 C16 1.423(10) .
O15 K2 2.769(6) .
O15 K2 2.821(6) 2_656
C15 O16 1.430(10) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
O16 K2 2.694(5) 2_556
O16 K1 2.854(6) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
K1 O13 2.783(5) 2_556
K1 O14 2.789(6) 2_556
K1 O11 2.855(6) 2_566
K1 O4 2.903(5) 2_666
K1 Nb3 3.8401(16) 2_666
K1 Nb4 3.8403(17) .
K1 Nb1 3.8820(17) .
K1 K2 3.960(2) 2_556
K2 O16 2.694(5) 2_556
K2 O15 2.821(6) 2_656
K2 Nb4 3.8400(17) .
K2 K1 3.960(2) 2_556
K2 K2 4.458(3) 2_656
Nb1 Ir1 3.1270(7) .
Nb1 Nb4 3.3013(8) 2_666
Nb1 Nb3 3.3398(9) 2_666
Nb3 O8 1.964(5) 2_666
Nb3 Ir1 3.1905(7) .
Nb3 Nb1 3.3397(9) 2_666
Nb3 Nb4 3.3410(9) 2_666
Nb3 K1 3.8401(17) 2_666
Nb4 O10 1.954(5) 2_666
Nb4 O4 1.993(5) 2_666
Nb4 Ir1 3.1196(7) .
Nb4 Nb1 3.3013(8) 2_666
Nb4 Nb3 3.3411(9) 2_666
