#------------------------------------------------------------------------------
#$Date: 2016-10-07 10:37:42 +0300 (Fri, 07 Oct 2016) $
#$Revision: 187017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/02/05/7020524.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_7020524
loop_
_publ_author_name
'Son, Jung-Ho'
'Ohlin, C André'
'Casey, William H.'
_publ_section_title
;
 A new class of soluble and stable transition-metal-substituted
 polyoxoniobate: [Cr(2)(OH)(4)Nb(10)O(30)](8-).
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12674
_journal_page_last               12677
_journal_paper_doi               10.1039/c2dt31760e
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'Cr2 H12 K2 Nb10 O389, 6(C4 H12 N), 10(H2 O)'
_chemical_formula_sum            'C24 H104 Cr2 K2 N6 Nb10 O48'
_chemical_formula_weight         2356.44
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.0920(10)
_cell_angle_beta                 100.7010(10)
_cell_angle_gamma                102.2830(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8564(4)
_cell_length_b                   14.0354(5)
_cell_length_c                   14.0485(5)
_cell_measurement_reflns_used    9239
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.68
_cell_volume                     1818.12(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      90(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23575
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    2.012
_exptl_absorpt_correction_T_max  0.8090
_exptl_absorpt_correction_T_min  0.7134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    2.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1170
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.00015(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         8325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0076P)²+4.8287P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0557
_reflns_number_gt                7722
_reflns_number_total             8325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31760e.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1818.12(11)
_cod_database_code               7020524
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Nb1 Nb 1.04820(2) 0.74971(2) 0.86299(2) 0.00887(6) Uani 1 1 d .
Nb2 Nb 0.97964(2) 0.485058(19) 0.686251(19) 0.00769(6) Uani 1 1 d .
Nb3 Nb 1.18543(2) 0.698363(19) 0.661295(19) 0.00752(6) Uani 1 1 d .
Nb4 Nb 0.94281(2) 0.808349(19) 0.66011(2) 0.00811(6) Uani 1 1 d .
Nb5 Nb 0.74406(2) 0.60461(2) 0.68357(2) 0.00868(6) Uani 1 1 d .
Cr1 Cr 0.89147(4) 0.55113(3) 0.49751(3) 0.00705(9) Uani 1 1 d .
K1 K 0.39440(6) 0.36191(5) 0.57310(5) 0.01506(13) Uani 1 1 d .
O1 O 1.1131(2) 0.82754(16) 1.00653(16) 0.0142(4) Uani 1 1 d .
O2 O 1.04785(19) 0.59696(16) 0.83357(16) 0.0107(4) Uani 1 1 d .
O3 O 1.20960(19) 0.76384(16) 0.81407(16) 0.0107(4) Uani 1 1 d .
O4 O 1.01241(19) 0.85768(16) 0.81311(16) 0.0107(4) Uani 1 1 d .
O5 O 0.85303(19) 0.69186(16) 0.83202(16) 0.0112(4) Uani 1 1 d .
O6 O 0.95935(18) 0.63947(15) 0.65838(15) 0.0088(4) Uani 1 1 d .
O7 O 0.9966(2) 0.36369(16) 0.68810(16) 0.0131(4) Uani 1 1 d .
O8 O 1.15460(18) 0.54524(15) 0.65906(15) 0.0086(4) Uani 1 1 d .
O9 O 0.79672(19) 0.47321(16) 0.67614(16) 0.0099(4) Uani 1 1 d .
O10 O 1.34578(19) 0.72457(16) 0.64590(16) 0.0117(4) Uani 1 1 d .
O11 O 1.11875(19) 0.80560(15) 0.63816(16) 0.0098(4) Uani 1 1 d .
O12 O 0.92297(18) 0.42057(15) 0.50933(15) 0.0084(4) Uani 1 1 d .
O13 O 0.9269(2) 0.92525(16) 0.64655(16) 0.0130(4) Uani 1 1 d .
O14 O 0.76313(19) 0.73164(16) 0.65262(16) 0.0104(4) Uani 1 1 d .
O15 O 0.8736(2) 0.68582(16) 0.48837(17) 0.0101(4) Uani 1 1 d .
O16 O 0.5818(2) 0.57064(17) 0.69046(17) 0.0144(4) Uani 1 1 d .
O17 O 0.7093(2) 0.51801(18) 0.50864(17) 0.0100(4) Uani 1 1 d .
O18 O 0.3815(3) 0.3573(2) 0.7740(2) 0.0314(6) Uani 1 1 d .
O19 O 0.3937(2) 0.5628(2) 0.79487(19) 0.0189(5) Uani 1 1 d .
O20 O 0.5999(2) 0.27813(19) 0.5481(2) 0.0170(4) Uani 1 1 d .
O21 O 0.5972(2) 0.86309(19) 0.69030(19) 0.0182(5) Uani 1 1 d .
O22 O 0.8542(3) 0.6998(3) 0.1864(2) 0.0299(6) Uani 1 1 d .
O23 O 0.3711(3) 0.9213(2) 0.1607(3) 0.0303(6) Uani 1 1 d .
O24 O -0.0023(3) 0.8730(2) 0.1719(2) 0.0277(6) Uani 1 1 d .
N1 N 0.3257(3) 0.1255(2) 0.0023(2) 0.0144(5) Uani 1 1 d .
N2 N 0.2595(3) 0.6173(2) 0.0988(2) 0.0163(5) Uani 1 1 d .
N3 N 0.7388(2) 0.0065(2) 0.4671(2) 0.0143(5) Uani 1 1 d .
C1 C 0.4547(3) 0.1474(3) 0.0814(3) 0.0258(7) Uani 1 1 d .
H1A H 0.4559 0.0802 0.0870 0.039 Uiso 1 1 calc R
H1B H 0.4647 0.2063 0.1536 0.039 Uiso 1 1 calc R
H1C H 0.5278 0.1699 0.0553 0.039 Uiso 1 1 calc R
C2 C 0.2128(3) 0.0859(3) 0.0383(3) 0.0178(6) Uani 1 1 d .
H2A H 0.2141 0.0169 0.0398 0.027 Uiso 1 1 calc R
H2B H 0.1291 0.0732 -0.0130 0.027 Uiso 1 1 calc R
H2C H 0.2212 0.1416 0.1118 0.027 Uiso 1 1 calc R
C3 C 0.3142(4) 0.0401(3) -0.1091(3) 0.0279(8) Uani 1 1 d .
H3A H 0.3899 0.0653 -0.1314 0.042 Uiso 1 1 calc R
H3B H 0.2319 0.0283 -0.1615 0.042 Uiso 1 1 calc R
H3C H 0.3134 -0.0291 -0.1074 0.042 Uiso 1 1 calc R
C4 C 0.3226(3) 0.2297(3) -0.0013(3) 0.0224(7) Uani 1 1 d .
H4A H 0.3318 0.2862 0.0720 0.034 Uiso 1 1 calc R
H4B H 0.2382 0.2164 -0.0522 0.034 Uiso 1 1 calc R
H4C H 0.3957 0.2551 -0.0260 0.034 Uiso 1 1 calc R
C5 C 0.3411(4) 0.6994(3) 0.2138(3) 0.0288(8) Uani 1 1 d .
H5A H 0.3529 0.7742 0.2229 0.043 Uiso 1 1 calc R
H5B H 0.4278 0.6893 0.2291 0.043 Uiso 1 1 calc R
H5C H 0.2960 0.6887 0.2647 0.043 Uiso 1 1 calc R
C6 C 0.2466(4) 0.5032(3) 0.0836(3) 0.0240(7) Uani 1 1 d .
H6A H 0.1993 0.4890 0.1319 0.036 Uiso 1 1 calc R
H6B H 0.3349 0.4965 0.1016 0.036 Uiso 1 1 calc R
H6C H 0.1971 0.4496 0.0072 0.036 Uiso 1 1 calc R
C7 C 0.1261(3) 0.6318(3) 0.0802(3) 0.0221(7) Uani 1 1 d .
H7A H 0.1362 0.7080 0.0947 0.033 Uiso 1 1 calc R
H7B H 0.0826 0.6156 0.1296 0.033 Uiso 1 1 calc R
H7C H 0.0722 0.5813 0.0041 0.033 Uiso 1 1 calc R
C8 C 0.3233(4) 0.6358(3) 0.0193(3) 0.0252(7) Uani 1 1 d .
H8A H 0.2663 0.5843 -0.0556 0.038 Uiso 1 1 calc R
H8B H 0.4093 0.6237 0.0301 0.038 Uiso 1 1 calc R
H8C H 0.3360 0.7116 0.0316 0.038 Uiso 1 1 calc R
C9 C 0.6625(3) -0.0436(3) 0.5227(3) 0.0216(7) Uani 1 1 d .
H9A H 0.5925 -0.1118 0.4675 0.032 Uiso 1 1 calc R
H9B H 0.6228 0.0083 0.5664 0.032 Uiso 1 1 calc R
H9C H 0.7222 -0.0603 0.5707 0.032 Uiso 1 1 calc R
C10 C 0.8075(3) -0.0692(3) 0.4070(3) 0.0239(7) Uani 1 1 d .
H10A H 0.8630 -0.0338 0.3753 0.036 Uiso 1 1 calc R
H10B H 0.7415 -0.1379 0.3483 0.036 Uiso 1 1 calc R
H10C H 0.8631 -0.0856 0.4579 0.036 Uiso 1 1 calc R
C11 C 0.8398(3) 0.1144(3) 0.5520(3) 0.0218(7) Uani 1 1 d .
H11A H 0.8986 0.1021 0.6047 0.033 Uiso 1 1 calc R
H11B H 0.7948 0.1646 0.5903 0.033 Uiso 1 1 calc R
H11C H 0.8919 0.1468 0.5163 0.033 Uiso 1 1 calc R
C12 C 0.6485(3) 0.0271(3) 0.3889(3) 0.0190(6) Uani 1 1 d .
H12A H 0.7004 0.0625 0.3552 0.028 Uiso 1 1 calc R
H12B H 0.6023 0.0754 0.4285 0.028 Uiso 1 1 calc R
H12C H 0.5836 -0.0431 0.3319 0.028 Uiso 1 1 calc R
H1 H 0.910(4) 0.691(3) 0.452(3) 0.028(12) Uiso 1 1 d .
H2 H 0.679(4) 0.468(3) 0.485(3) 0.016(11) Uiso 1 1 d .
H3 H 0.319(5) 0.332(4) 0.792(4) 0.042(14) Uiso 1 1 d .
H4 H 0.379(6) 0.432(6) 0.795(5) 0.10(2) Uiso 1 1 d .
H5 H 0.324(4) 0.556(3) 0.757(3) 0.013(9) Uiso 1 1 d .
H6 H 0.444(4) 0.572(3) 0.764(3) 0.021(10) Uiso 1 1 d .
H7 H 0.607(4) 0.268(4) 0.492(4) 0.035(13) Uiso 1 1 d .
H8 H 0.667(4) 0.336(3) 0.592(3) 0.020(10) Uiso 1 1 d .
H9 H 0.531(4) 0.820(3) 0.684(3) 0.023(10) Uiso 1 1 d .
H10 H 0.646(4) 0.831(3) 0.684(3) 0.022(11) Uiso 1 1 d .
H11 H 0.902(5) 0.689(4) 0.227(4) 0.056(16) Uiso 1 1 d .
H12 H 0.899(5) 0.754(4) 0.197(4) 0.044(15) Uiso 1 1 d .
H13 H 0.368(5) 0.976(4) 0.208(4) 0.045(14) Uiso 1 1 d .
H14 H 0.299(4) 0.895(3) 0.115(4) 0.026(11) Uiso 1 1 d .
H15 H 0.068(5) 0.877(4) 0.195(4) 0.032(14) Uiso 1 1 d .
H16 H 0.037(5) 0.951(5) 0.233(5) 0.067(17) Uiso 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'
Cr Cr 0.3209 0.6236 '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'
K K 0.2009 0.2494 '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
O1 Nb1 O4 104.32(9) . .
O1 Nb1 O5 105.38(9) . .
O4 Nb1 O5 86.48(8) . .
O1 Nb1 O3 103.03(9) . .
O4 Nb1 O3 86.93(8) . .
O5 Nb1 O3 151.59(8) . .
O1 Nb1 O2 103.91(9) . .
O4 Nb1 O2 151.77(8) . .
O5 Nb1 O2 85.98(8) . .
O3 Nb1 O2 86.89(8) . .
O1 Nb1 O6 179.10(8) . .
O4 Nb1 O6 75.73(7) . .
O5 Nb1 O6 75.52(7) . .
O3 Nb1 O6 76.07(7) . .
O2 Nb1 O6 76.05(7) . .
O1 Nb1 Nb2 134.13(7) . .
O4 Nb1 Nb2 121.54(6) . .
O5 Nb1 Nb2 78.28(6) . .
O3 Nb1 Nb2 81.77(6) . .
O2 Nb1 Nb2 30.24(5) . .
O6 Nb1 Nb2 45.85(4) . .
O1 Nb1 Nb3 133.16(7) . .
O4 Nb1 Nb3 78.60(6) . .
O5 Nb1 Nb3 121.43(6) . .
O3 Nb1 Nb3 30.20(6) . .
O2 Nb1 Nb3 82.28(6) . .
O6 Nb1 Nb3 45.94(4) . .
Nb2 Nb1 Nb3 63.665(7) . .
O1 Nb1 Nb4 134.27(7) . .
O4 Nb1 Nb4 29.96(6) . .
O5 Nb1 Nb4 80.02(6) . .
O3 Nb1 Nb4 80.53(6) . .
O2 Nb1 Nb4 121.82(6) . .
O6 Nb1 Nb4 45.77(4) . .
Nb2 Nb1 Nb4 91.598(9) . .
Nb3 Nb1 Nb4 59.661(7) . .
O1 Nb1 Nb5 135.23(7) . .
O4 Nb1 Nb5 79.43(6) . .
O5 Nb1 Nb5 29.86(6) . .
O3 Nb1 Nb5 121.74(6) . .
O2 Nb1 Nb5 80.54(6) . .
O6 Nb1 Nb5 45.67(4) . .
Nb2 Nb1 Nb5 60.022(7) . .
Nb3 Nb1 Nb5 91.572(9) . .
Nb4 Nb1 Nb5 60.329(7) . .
O7 Nb2 O2 106.20(9) . .
O7 Nb2 O9 105.02(9) . .
O2 Nb2 O9 95.06(8) . .
O7 Nb2 O8 101.26(8) . .
O2 Nb2 O8 89.58(8) . .
O9 Nb2 O8 150.81(8) . .
O7 Nb2 O12 96.80(8) . .
O2 Nb2 O12 155.17(8) . .
O9 Nb2 O12 87.72(8) . .
O8 Nb2 O12 76.68(7) . .
O7 Nb2 O6 171.98(8) . .
O2 Nb2 O6 80.87(7) . .
O9 Nb2 O6 77.67(7) . .
O8 Nb2 O6 74.64(7) . .
O12 Nb2 O6 75.63(7) . .
O7 Nb2 Cr1 91.33(7) . 2_766
O2 Nb2 Cr1 128.10(6) . 2_766
O9 Nb2 Cr1 127.49(6) . 2_766
O8 Nb2 Cr1 38.65(5) . 2_766
O12 Nb2 Cr1 40.33(5) . 2_766
O6 Nb2 Cr1 81.18(5) . 2_766
O7 Nb2 Nb1 138.53(7) . .
O2 Nb2 Nb1 32.34(6) . .
O9 Nb2 Nb1 85.85(6) . .
O8 Nb2 Nb1 82.80(5) . .
O12 Nb2 Nb1 123.91(5) . .
O6 Nb2 Nb1 48.57(5) . .
Cr1 Nb2 Nb1 113.806(11) 2_766 .
O7 Nb2 Nb5 137.58(7) . .
O2 Nb2 Nb5 82.30(6) . .
O9 Nb2 Nb5 32.70(6) . .
O8 Nb2 Nb5 120.58(5) . .
O12 Nb2 Nb5 87.01(5) . .
O6 Nb2 Nb5 45.94(4) . .
Cr1 Nb2 Nb5 116.339(11) 2_766 .
Nb1 Nb2 Nb5 60.291(7) . .
O10 Nb3 O3 106.49(9) . .
O10 Nb3 O11 105.00(9) . .
O3 Nb3 O11 95.36(8) . .
O10 Nb3 O8 101.40(8) . .
O3 Nb3 O8 88.78(8) . .
O11 Nb3 O8 150.84(8) . .
O10 Nb3 O12 97.33(8) . 2_766
O3 Nb3 O12 153.83(8) . 2_766
O11 Nb3 O12 88.68(8) . 2_766
O8 Nb3 O12 75.79(7) . 2_766
O10 Nb3 O6 171.95(8) . .
O3 Nb3 O6 80.48(7) . .
O11 Nb3 O6 77.89(7) . .
O8 Nb3 O6 74.35(7) . .
O12 Nb3 O6 75.10(7) 2_766 .
O10 Nb3 Cr1 91.91(6) . 2_766
O3 Nb3 Cr1 126.75(6) . 2_766
O11 Nb3 Cr1 127.98(6) . 2_766
O8 Nb3 Cr1 38.14(5) . 2_766
O12 Nb3 Cr1 39.89(5) 2_766 2_766
O6 Nb3 Cr1 80.54(5) . 2_766
O10 Nb3 Nb4 137.41(7) . .
O3 Nb3 Nb4 82.49(6) . .
O11 Nb3 Nb4 32.53(6) . .
O8 Nb3 Nb4 120.64(5) . .
O12 Nb3 Nb4 87.34(5) 2_766 .
O6 Nb3 Nb4 46.29(4) . .
Cr1 Nb3 Nb4 116.296(11) 2_766 .
O10 Nb3 Nb1 138.49(6) . .
O3 Nb3 Nb1 32.00(6) . .
O11 Nb3 Nb1 85.73(6) . .
O8 Nb3 Nb1 82.64(5) . .
O12 Nb3 Nb1 123.30(5) 2_766 .
O6 Nb3 Nb1 48.56(5) . .
Cr1 Nb3 Nb1 113.072(11) 2_766 .
Nb4 Nb3 Nb1 60.369(7) . .
O13 Nb4 O4 106.08(9) . .
O13 Nb4 O14 104.15(9) . .
O4 Nb4 O14 93.31(8) . .
O13 Nb4 O11 102.13(9) . .
O4 Nb4 O11 91.80(8) . .
O14 Nb4 O11 150.64(8) . .
O13 Nb4 O15 99.81(8) . .
O4 Nb4 O15 154.09(8) . .
O14 Nb4 O15 81.14(8) . .
O11 Nb4 O15 81.72(8) . .
O13 Nb4 O6 174.09(8) . .
O4 Nb4 O6 79.75(7) . .
O14 Nb4 O6 76.09(7) . .
O11 Nb4 O6 76.43(7) . .
O15 Nb4 O6 74.35(7) . .
O13 Nb4 Nb3 132.96(7) . .
O4 Nb4 Nb3 79.88(6) . .
O14 Nb4 Nb3 122.32(6) . .
O11 Nb4 Nb3 31.07(5) . .
O15 Nb4 Nb3 81.85(5) . .
O6 Nb4 Nb3 46.25(5) . .
O13 Nb4 Nb1 137.49(7) . .
O4 Nb4 Nb1 31.42(6) . .
O14 Nb4 Nb1 85.26(6) . .
O11 Nb4 Nb1 84.18(5) . .
O15 Nb4 Nb1 122.68(5) . .
O6 Nb4 Nb1 48.34(5) . .
Nb3 Nb4 Nb1 59.970(7) . .
O13 Nb4 K1 87.52(7) . 2_666
O4 Nb4 K1 138.72(6) . 2_666
O14 Nb4 K1 45.41(6) . 2_666
O11 Nb4 K1 123.87(6) . 2_666
O15 Nb4 K1 42.26(6) . 2_666
O6 Nb4 K1 88.59(5) . 2_666
Nb3 Nb4 K1 119.026(12) . 2_666
Nb1 Nb4 K1 123.929(12) . 2_666
O16 Nb5 O5 105.05(9) . .
O16 Nb5 O14 104.47(9) . .
O5 Nb5 O14 94.05(8) . .
O16 Nb5 O9 102.46(9) . .
O5 Nb5 O9 90.91(8) . .
O14 Nb5 O9 150.27(8) . .
O16 Nb5 O17 100.83(9) . .
O5 Nb5 O17 154.05(8) . .
O14 Nb5 O17 81.18(8) . .
O9 Nb5 O17 81.64(8) . .
O16 Nb5 O6 175.21(8) . .
O5 Nb5 O6 79.60(7) . .
O14 Nb5 O6 76.05(7) . .
O9 Nb5 O6 76.07(7) . .
O17 Nb5 O6 74.48(7) . .
O16 Nb5 Nb2 133.31(7) . .
O5 Nb5 Nb2 79.00(6) . .
O14 Nb5 Nb2 121.83(6) . .
O9 Nb5 Nb2 31.20(5) . .
O17 Nb5 Nb2 81.96(5) . .
O6 Nb5 Nb2 45.80(4) . .
O16 Nb5 Nb1 136.44(7) . .
O5 Nb5 Nb1 31.39(6) . .
O14 Nb5 Nb1 85.05(6) . .
O9 Nb5 Nb1 84.07(6) . .
O17 Nb5 Nb1 122.70(6) . .
O6 Nb5 Nb1 48.22(5) . .
Nb2 Nb5 Nb1 59.687(8) . .
O16 Nb5 K1 88.11(7) . 2_666
O5 Nb5 K1 139.89(6) . 2_666
O14 Nb5 K1 45.85(6) . 2_666
O9 Nb5 K1 123.61(6) . 2_666
O17 Nb5 K1 42.08(6) . 2_666
O6 Nb5 K1 88.97(5) . 2_666
Nb2 Nb5 K1 118.996(12) . 2_666
Nb1 Nb5 K1 124.217(12) . 2_666
O16 Nb5 K1 34.09(7) . .
O5 Nb5 K1 126.26(6) . .
O14 Nb5 K1 122.56(6) . .
O9 Nb5 K1 75.98(6) . .
O17 Nb5 K1 76.11(6) . .
O6 Nb5 K1 141.78(5) . .
Nb2 Nb5 K1 106.273(12) . .
Nb1 Nb5 K1 150.403(12) . .
K1 Nb5 K1 85.272(15) 2_666 .
O8 Cr1 O6 171.55(8) 2_766 .
O8 Cr1 O17 96.97(9) 2_766 .
O6 Cr1 O17 88.94(8) . .
O8 Cr1 O15 97.36(8) 2_766 .
O6 Cr1 O15 88.76(8) . .
O17 Cr1 O15 88.91(9) . .
O8 Cr1 O12 84.01(8) 2_766 2_766
O6 Cr1 O12 89.76(8) . 2_766
O17 Cr1 O12 176.73(8) . 2_766
O15 Cr1 O12 94.07(8) . 2_766
O8 Cr1 O12 83.40(8) 2_766 .
O6 Cr1 O12 90.10(8) . .
O17 Cr1 O12 94.87(8) . .
O15 Cr1 O12 176.03(8) . .
O12 Cr1 O12 82.13(8) 2_766 .
O8 Cr1 Nb2 41.79(6) 2_766 2_766
O6 Cr1 Nb2 133.57(6) . 2_766
O17 Cr1 Nb2 136.94(6) . 2_766
O15 Cr1 Nb2 86.06(6) . 2_766
O12 Cr1 Nb2 44.84(5) 2_766 2_766
O12 Cr1 Nb2 91.98(5) . 2_766
O8 Cr1 Nb3 41.50(6) 2_766 2_766
O6 Cr1 Nb3 133.51(6) . 2_766
O17 Cr1 Nb3 86.47(7) . 2_766
O15 Cr1 Nb3 137.28(6) . 2_766
O12 Cr1 Nb3 92.25(5) 2_766 2_766
O12 Cr1 Nb3 44.46(5) . 2_766
Nb2 Cr1 Nb3 69.444(11) 2_766 2_766
O8 Cr1 K1 85.94(6) 2_766 2_666
O6 Cr1 K1 102.52(6) . 2_666
O17 Cr1 K1 45.92(6) . 2_666
O15 Cr1 K1 46.47(6) . 2_666
O12 Cr1 K1 137.34(6) 2_766 2_666
O12 Cr1 K1 137.49(6) . 2_666
Nb2 Cr1 K1 106.679(16) 2_766 2_666
Nb3 Cr1 K1 106.847(16) 2_766 2_666
O17 K1 O15 61.69(6) 2_666 2_666
O17 K1 O20 133.02(7) 2_666 .
O15 K1 O20 145.24(7) 2_666 .
O17 K1 O16 76.59(7) 2_666 .
O15 K1 O16 126.49(6) 2_666 .
O20 K1 O16 87.79(7) . .
O17 K1 O18 125.91(7) 2_666 .
O15 K1 O18 88.51(7) 2_666 .
O20 K1 O18 97.73(8) . .
O16 K1 O18 90.43(8) . .
O17 K1 O14 57.58(6) 2_666 2_666
O15 K1 O14 57.56(6) 2_666 2_666
O20 K1 O14 100.68(7) . 2_666
O16 K1 O14 124.33(6) . 2_666
O18 K1 O14 140.88(8) . 2_666
O17 K1 O19 78.90(6) 2_666 .
O15 K1 O19 85.35(6) 2_666 .
O20 K1 O19 125.40(7) . .
O16 K1 O19 53.39(6) . .
O18 K1 O19 53.00(7) . .
O14 K1 O19 131.82(6) 2_666 .
O17 K1 Cr1 31.76(5) 2_666 2_666
O15 K1 Cr1 32.03(4) 2_666 2_666
O20 K1 Cr1 159.16(6) . 2_666
O16 K1 Cr1 97.17(5) . 2_666
O18 K1 Cr1 102.45(6) . 2_666
O14 K1 Cr1 59.89(4) 2_666 2_666
O19 K1 Cr1 72.32(4) . 2_666
O17 K1 Nb5 32.37(5) 2_666 2_666
O15 K1 Nb5 66.44(5) 2_666 2_666
O20 K1 Nb5 109.13(5) . 2_666
O16 K1 Nb5 95.70(5) . 2_666
O18 K1 Nb5 152.62(6) . 2_666
O14 K1 Nb5 29.47(4) 2_666 2_666
O19 K1 Nb5 111.27(4) . 2_666
Cr1 K1 Nb5 50.348(11) 2_666 2_666
O17 K1 Nb4 66.24(5) 2_666 2_666
O15 K1 Nb4 32.47(4) 2_666 2_666
O20 K1 Nb4 116.45(5) . 2_666
O16 K1 Nb4 142.81(5) . 2_666
O18 K1 Nb4 111.94(6) . 2_666
O14 K1 Nb4 29.21(4) 2_666 2_666
O19 K1 Nb4 117.25(5) . 2_666
Cr1 K1 Nb4 50.427(11) 2_666 2_666
Nb5 K1 Nb4 51.167(10) 2_666 2_666
O17 K1 Nb5 85.80(5) 2_666 .
O15 K1 Nb5 144.12(5) 2_666 .
O20 K1 Nb5 68.45(5) . .
O16 K1 Nb5 20.76(4) . .
O18 K1 Nb5 100.13(6) . .
O14 K1 Nb5 118.69(4) 2_666 .
O19 K1 Nb5 73.06(5) . .
Cr1 K1 Nb5 112.457(17) 2_666 .
Nb5 K1 Nb5 94.728(14) 2_666 .
Nb4 K1 Nb5 145.839(18) 2_666 .
O17 K1 H4 108.6(14) 2_666 .
O15 K1 H4 85.8(13) 2_666 .
O20 K1 H4 110.4(13) . .
O16 K1 H4 76.9(13) . .
O18 K1 H4 19.3(14) . .
O14 K1 H4 143.4(13) 2_666 .
O19 K1 H4 33.8(14) . .
Cr1 K1 H4 90.4(13) 2_666 .
Nb5 K1 H4 139.3(13) 2_666 .
Nb4 K1 H4 115.5(13) 2_666 .
Nb5 K1 H4 91.1(13) . .
O17 K1 H6 75.3(8) 2_666 .
O15 K1 H6 94.6(8) 2_666 .
O20 K1 H6 118.7(8) . .
O16 K1 H6 40.5(8) . .
O18 K1 H6 62.5(8) . .
O14 K1 H6 132.2(8) 2_666 .
O19 K1 H6 13.1(8) . .
Cr1 K1 H6 76.1(8) 2_666 .
Nb5 K1 H6 106.8(8) 2_666 .
Nb4 K1 H6 124.9(8) 2_666 .
Nb5 K1 H6 60.5(8) . .
H4 K1 H6 44.0(16) . .
O17 K1 H7 120.7(9) 2_666 .
O15 K1 H7 139.5(9) 2_666 .
O20 K1 H7 13.7(9) . .
O16 K1 H7 89.6(8) . .
O18 K1 H7 111.3(9) . .
O14 K1 H7 88.5(9) 2_666 .
O19 K1 H7 134.9(9) . .
Cr1 K1 H7 145.5(9) 2_666 .
Nb5 K1 H7 95.5(9) 2_666 .
Nb4 K1 H7 107.8(9) 2_666 .
Nb5 K1 H7 69.0(8) . .
H4 K1 H7 124.0(16) . .
H6 K1 H7 125.7(12) . .
O17 K1 H8 128.1(7) 2_666 .
O15 K1 H8 161.5(8) 2_666 .
O20 K1 H8 16.3(8) . .
O16 K1 H8 71.8(8) . .
O18 K1 H8 94.7(7) . .
O14 K1 H8 111.8(7) 2_666 .
O19 K1 H8 111.1(8) . .
Cr1 K1 H8 159.8(7) 2_666 .
Nb5 K1 H8 112.6(7) 2_666 .
Nb4 K1 H8 131.6(8) 2_666 .
Nb5 K1 H8 53.1(8) . .
H4 K1 H8 103.0(15) . .
H6 K1 H8 103.1(11) . .
H7 K1 H8 24.1(10) . .
Nb2 O2 Nb1 117.42(10) . .
Nb3 O3 Nb1 117.80(10) . .
Nb4 O4 Nb1 118.62(10) . .
Nb5 O5 Nb1 118.75(10) . .
Cr1 O6 Nb2 93.60(7) . .
Cr1 O6 Nb3 93.99(7) . .
Nb2 O6 Nb3 94.16(7) . .
Cr1 O6 Nb4 94.95(7) . .
Nb2 O6 Nb4 171.17(9) . .
Nb3 O6 Nb4 87.46(6) . .
Cr1 O6 Nb5 94.45(7) . .
Nb2 O6 Nb5 88.26(6) . .
Nb3 O6 Nb5 171.06(9) . .
Nb4 O6 Nb5 88.88(6) . .
Cr1 O6 Nb1 178.99(10) . .
Nb2 O6 Nb1 85.58(6) . .
Nb3 O6 Nb1 85.50(6) . .
Nb4 O6 Nb1 85.89(6) . .
Nb5 O6 Nb1 86.10(6) . .
Cr1 O8 Nb2 99.56(8) 2_766 .
Cr1 O8 Nb3 100.36(8) 2_766 .
Nb2 O8 Nb3 115.18(9) . .
Nb2 O9 Nb5 116.11(9) . .
Nb3 O11 Nb4 116.39(9) . .
Cr1 O12 Cr1 97.87(8) 2_766 .
Cr1 O12 Nb2 94.83(8) 2_766 .
Cr1 O12 Nb2 100.06(8) . .
Cr1 O12 Nb3 100.43(8) 2_766 2_766
Cr1 O12 Nb3 95.65(8) . 2_766
Nb2 O12 Nb3 156.35(10) . 2_766
Nb4 O14 Nb5 116.68(9) . .
Nb4 O14 K1 105.38(8) . 2_666
Nb5 O14 K1 104.68(8) . 2_666
Cr1 O15 Nb4 101.94(9) . .
Cr1 O15 K1 101.50(8) . 2_666
Nb4 O15 K1 105.27(8) . 2_666
Cr1 O15 H1 104(3) . .
Nb4 O15 H1 120(3) . .
K1 O15 H1 120(3) 2_666 .
Nb5 O16 K1 125.16(10) . .
Cr1 O17 Nb5 102.12(9) . .
Cr1 O17 K1 102.32(9) . 2_666
Nb5 O17 K1 105.54(8) . 2_666
Cr1 O17 H2 112(4) . .
Nb5 O17 H2 118(4) . .
K1 O17 H2 115(4) 2_666 .
K1 O18 H3 132(3) . .
K1 O18 H4 82(4) . .
H3 O18 H4 101(5) . .
K1 O19 H5 84(3) . .
K1 O19 H6 59(3) . .
H5 O19 H6 105(4) . .
K1 O20 H7 108(3) . .
K1 O20 H8 101(2) . .
H7 O20 H8 103(4) . .
H9 O21 H10 103(4) . .
H11 O22 H12 98(5) . .
H13 O23 H14 105(4) . .
H15 O24 H16 77(4) . .
C4 N1 C3 109.4(3) . .
C4 N1 C2 109.4(2) . .
C3 N1 C2 109.7(2) . .
C4 N1 C1 108.9(2) . .
C3 N1 C1 109.4(3) . .
C2 N1 C1 110.1(2) . .
C7 N2 C5 107.9(3) . .
C7 N2 C8 109.7(2) . .
C5 N2 C8 110.4(3) . .
C7 N2 C6 110.2(3) . .
C5 N2 C6 109.4(3) . .
C8 N2 C6 109.2(3) . .
C9 N3 C12 110.4(2) . .
C9 N3 C10 109.6(2) . .
C12 N3 C10 109.8(2) . .
C9 N3 C11 109.0(2) . .
C12 N3 C11 108.7(2) . .
C10 N3 C11 109.4(2) . .
N1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N1 C3 H3A 109.5 . .
N1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N1 C4 H4A 109.5 . .
N1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N2 C5 H5A 109.5 . .
N2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
N2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
N2 C6 H6A 109.5 . .
N2 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
N2 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N2 C7 H7A 109.5 . .
N2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N2 C8 H8A 109.5 . .
N2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
N2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N3 C9 H9A 109.5 . .
N3 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N3 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N3 C10 H10A 109.5 . .
N3 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
N3 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N3 C11 H11A 109.5 . .
N3 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N3 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N3 C12 H12A 109.5 . .
N3 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N3 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 O1 1.761(2) .
Nb1 O4 1.9886(19) .
Nb1 O5 1.994(2) .
Nb1 O3 1.998(2) .
Nb1 O2 2.0100(19) .
Nb1 O6 2.5082(19) .
Nb1 Nb2 3.3353(4) .
Nb1 Nb3 3.3354(4) .
Nb1 Nb4 3.3488(4) .
Nb1 Nb5 3.3557(4) .
Nb2 O7 1.762(2) .
Nb2 O2 1.8923(19) .
Nb2 O9 1.9304(19) .
Nb2 O8 2.0779(19) .
Nb2 O12 2.1757(19) .
Nb2 O6 2.4005(19) .
Nb2 Cr1 3.0748(5) 2_766
Nb2 Nb5 3.3467(4) .
Nb3 O10 1.773(2) .
Nb3 O3 1.8968(19) .
Nb3 O11 1.9158(19) .
Nb3 O8 2.0896(19) .
Nb3 O12 2.1834(19) 2_766
Nb3 O6 2.4043(19) .
Nb3 Cr1 3.1021(5) 2_766
Nb3 Nb4 3.3250(3) .
Nb4 O13 1.767(2) .
Nb4 O4 1.9052(19) .
Nb4 O14 1.9782(19) .
Nb4 O11 1.9962(19) .
Nb4 O15 2.175(2) .
Nb4 O6 2.4056(19) .
Nb4 K1 3.9088(7) 2_666
Nb5 O16 1.756(2) .
Nb5 O5 1.906(2) .
Nb5 O14 1.9798(19) .
Nb5 O9 2.0132(19) .
Nb5 O17 2.163(2) .
Nb5 O6 2.4062(19) .
Nb5 K1 3.8927(7) 2_666
Nb5 K1 4.0518(7) .
Cr1 O8 1.9474(19) 2_766
Cr1 O6 1.9731(19) .
Cr1 O17 1.984(2) .
Cr1 O15 1.993(2) .
Cr1 O12 1.9970(19) 2_766
Cr1 O12 1.9991(19) .
Cr1 Nb2 3.0748(5) 2_766
Cr1 Nb3 3.1021(5) 2_766
Cr1 K1 3.6826(8) 2_666
K1 O17 2.708(2) 2_666
K1 O15 2.725(2) 2_666
K1 O20 2.749(2) .
K1 O16 2.777(2) .
K1 O18 2.878(3) .
K1 O14 2.887(2) 2_666
K1 O19 3.241(3) .
K1 Cr1 3.6826(7) 2_666
K1 Nb5 3.8927(7) 2_666
K1 Nb4 3.9088(7) 2_666
K1 H4 2.91(6) .
K1 H6 2.92(4) .
K1 H7 3.06(5) .
K1 H8 3.03(4) .
O8 Cr1 1.9474(19) 2_766
O12 Cr1 1.9970(19) 2_766
O12 Nb3 2.1834(19) 2_766
O14 K1 2.887(2) 2_666
O15 K1 2.725(2) 2_666
O15 H1 0.72(4) .
O17 K1 2.708(2) 2_666
O17 H2 0.62(4) .
O18 H3 0.82(5) .
O18 H4 0.97(7) .
O19 H5 0.81(4) .
O19 H6 0.77(4) .
O20 H7 0.76(5) .
O20 H8 0.86(4) .
O21 H9 0.80(4) .
O21 H10 0.76(4) .
O22 H11 0.79(6) .
O22 H12 0.75(5) .
O23 H13 0.80(5) .
O23 H14 0.81(4) .
O24 H15 0.75(5) .
O24 H16 1.01(6) .
N1 C4 1.492(4) .
N1 C3 1.494(4) .
N1 C2 1.496(4) .
N1 C1 1.501(4) .
N2 C7 1.494(4) .
N2 C5 1.496(4) .
N2 C8 1.497(4) .
N2 C6 1.498(4) .
N3 C9 1.494(4) .
N3 C12 1.494(4) .
N3 C10 1.496(4) .
N3 C11 1.500(4) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
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 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
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 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O17 H2 O10 0.62(4) 2.49(4) 3.046(3) 151(5) 2_766
O15 H1 O7 0.72(4) 2.30(4) 2.987(3) 159(4) 2_766
