# Electronic Supplementary Material (ESI) for Dalton Transactions.
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_TMA-MnNb9

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'Tetramethylammonium nonaniobomanganate'
_chemical_melting_point          ?
_chemical_formula_moiety         'Mn Nb9 O28 8(C4 H12 N) 29(H2 O)'
_chemical_formula_sum            'C33 H60 Mn N8 Nb9 O57'
_chemical_formula_weight         2372.02

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'
Mn Mn 0.3368 0.7283 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   22.846(6)
_cell_length_b                   13.767(4)
_cell_length_c                   17.970(5)
_cell_angle_alpha                90
_cell_angle_beta                 129.353(3)
_cell_angle_gamma                90
_cell_volume                     4370(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    6920
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      27.51

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_F_000             2328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.447
_exptl_crystal_size_mid          0.423
_exptl_crystal_size_min          0.236
_exptl_absorpt_coefficient_mu    1.374
_shelx_estimated_absorpt_T_min   0.579
_shelx_estimated_absorpt_T_max   0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5855
_exptl_absorpt_correction_T_max  0.7426
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            23936
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.795
_diffrn_reflns_theta_max         27.543
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5199
_reflns_number_gt                5048
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0359P)²+53.9487P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5199
_refine_ls_number_parameters     313
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1285
_refine_ls_wR_factor_gt          0.1279
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_restrained_S_all      1.242
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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
Nb1 Nb 0.43887(3) 0.26705(3) 0.37775(3) 0.02656(13) Uani 1 1 d . . . . .
Mn2 Mn 0.44092(4) 0.5000 0.38183(5) 0.0203(3) Uani 0.519(10) 2 d S T P A 1
Nb2 Nb 0.44092(4) 0.5000 0.38183(5) 0.0203(3) Uani 0.481(10) 2 d S T P A 2
Nb3 Nb 0.39203(2) 0.38191(3) 0.49998(3) 0.02287(12) Uani 1 1 d . . . . .
O1 O 0.3951(2) 0.1743(3) 0.2901(3) 0.0408(10) Uani 1 1 d . . . . .
O2 O 0.40018(19) 0.3944(2) 0.3004(2) 0.0241(7) Uani 1 1 d . . . . .
O3 O 0.36464(19) 0.2951(3) 0.3982(2) 0.0278(7) Uani 1 1 d . . . . .
O4 O 0.5000 0.1958(3) 0.5000 0.0289(10) Uani 1 2 d S T P A .
O5 O 0.4664(2) 0.2950(3) 0.6017(2) 0.0279(7) Uani 1 1 d . . . . .
O6 O 0.5000 0.4010(3) 0.5000 0.0217(9) Uani 1 2 d S T P A .
O7 O 0.3634(3) 0.5000 0.4098(3) 0.0292(11) Uani 1 2 d S T P A .
O8 O 0.5464(3) 0.5000 0.4098(3) 0.0294(11) Uani 1 2 d S T P . .
O9 O 0.3153(2) 0.3691(3) 0.5001(3) 0.0387(9) Uani 1 1 d . . . . .
O10 O 0.5000 0.2500(10) 0.0000 0.149(6) Uani 1 2 d S T P . .
O11 O 0.4556(8) 0.1582(13) 0.0912(10) 0.226(8) Uani 1 1 d . . . . .
O12 O 0.5434(4) 0.1900(6) 0.2737(5) 0.088(2) Uani 1 1 d . . . . .
O13 O 0.3475(4) 0.0000 0.1951(4) 0.0433(14) Uani 1 2 d S T P . .
O14 O 0.1353(7) 0.1581(14) 0.0911(10) 0.226(8) Uani 1 1 d . . . . .
O15 O 0.2304(3) 0.1902(6) 0.2737(5) 0.087(2) Uani 1 1 d . . . . .
O16 O 0.1903(3) 0.2500(4) 0.3804(4) 0.0634(14) Uani 1 1 d . . . . .
O17 O 0.3128(17) 0.5000 0.126(2) 0.144(19) Uani 0.45(4) 2 d S T . . .
O18 O 0.1904(9) 0.0000 0.0590(13) 0.114(10) Uani 0.66(3) 2 d S T . . .
O19 O 0.200(2) 0.0000 0.156(4) 0.17(3) Uani 0.34(4) 2 d S T . . .
O20 O 0.3685(14) 0.0000 0.0591(13) 0.115(10) Uani 0.67(3) 2 d S T . . .
O21 O 0.455(3) 0.0000 0.156(4) 0.17(3) Uani 0.33(4) 2 d S T . . .
N1 N 0.3773(4) 0.0000 0.5001(5) 0.0326(14) Uani 1 2 d S T P . .
N2 N 0.1630(5) 0.5000 0.1911(6) 0.053(2) Uani 1 2 d S T P . .
N3 N 0.5281(6) 0.5000 0.1910(6) 0.053(2) Uani 1 2 d S T P . .
N4 N 0.2500 0.2500 0.0000 0.198(14) Uani 1 2 d S . P . .
C1 C 0.3729(8) 0.0000 0.4138(9) 0.065(3) Uani 1 2 d S T P . .
H1A H 0.4104 0.0454 0.4238 0.098 Uiso 0.5 1 calc R U P . .
H1B H 0.3221 0.0200 0.3572 0.098 Uiso 0.5 1 calc R U P . .
H1C H 0.3834 -0.0655 0.4034 0.098 Uiso 0.5 1 calc R U P . .
C2 C 0.3400(4) 0.0885(5) 0.4999(5) 0.0464(15) Uani 1 1 d . . . . .
H2A H 0.3435 0.0885 0.5571 0.070 Uiso 1 1 calc R U . . .
H2B H 0.2866 0.0890 0.4419 0.070 Uiso 1 1 calc R U . . .
H2C H 0.3653 0.1464 0.5005 0.070 Uiso 1 1 calc R U . . .
C3 C 0.4591(6) 0.0000 0.5861(9) 0.066(3) Uani 1 2 d S T P . .
H3A H 0.4800 -0.0653 0.5956 0.099 Uiso 0.5 1 calc R U P . .
H3C H 0.4649 0.0190 0.6430 0.099 Uiso 0.5 1 calc R U P . .
H3B H 0.4862 0.0462 0.5762 0.099 Uiso 0.5 1 calc R U P . .
C4 C 0.1706(8) 0.5000 0.2801(10) 0.088(4) Uani 1 2 d S T P . .
H4A H 0.1322 0.5429 0.2708 0.132 Uiso 0.5 1 calc R U P . .
H4B H 0.2211 0.5233 0.3346 0.132 Uiso 0.5 1 calc R U P . .
H4C H 0.1635 0.4338 0.2932 0.132 Uiso 0.5 1 calc R U P . .
C5 C 0.2058(7) 0.4167(10) 0.1956(8) 0.135(6) Uani 1 1 d . . . . .
H5A H 0.1766 0.3569 0.1794 0.202 Uiso 1 1 calc R U . . .
H5B H 0.2544 0.4113 0.2607 0.202 Uiso 1 1 calc R U . . .
H5C H 0.2148 0.4265 0.1496 0.202 Uiso 1 1 calc R U . . .
C6 C 0.0865(8) 0.5000 0.1026(14) 0.151(9) Uani 1 2 d S T P . .
C7 C 0.4899(9) 0.4169(10) 0.1957(8) 0.133(6) Uani 1 1 d . . . . .
H7A H 0.4350 0.4274 0.1508 0.199 Uiso 1 1 calc R U . . .
H7B H 0.5072 0.4107 0.2612 0.199 Uiso 1 1 calc R U . . .
H7C H 0.5019 0.3573 0.1781 0.199 Uiso 1 1 calc R U . . .
C8 C 0.6092(8) 0.5000 0.2800(10) 0.088(4) Uani 1 2 d S T P . .
H8A H 0.6290 0.4335 0.2942 0.132 Uiso 0.5 1 calc R U P . .
H8B H 0.6131 0.5251 0.3341 0.132 Uiso 0.5 1 calc R U P . .
H8C H 0.6386 0.5414 0.2701 0.132 Uiso 0.5 1 calc R U P . .
C9 C 0.5155(15) 0.5000 0.1021(14) 0.151(9) Uani 1 2 d S T P . .
C10 C 0.2271(15) 0.203(2) 0.0609(18) 0.111(12) Uiso 0.54(4) 1 d . . . . .
C11 C 0.2891(14) 0.3541(19) 0.079(2) 0.217(17) Uani 0.96(5) 1 d . . . . .
C12 C 0.292(2) 0.234(3) 0.0874(14) 0.085(17) Uani 0.33(4) 1 d . . . . .
C13 C 0.3352(11) 0.203(2) 0.0623(19) 0.143(16) Uani 0.57(4) 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Nb1 O1 1.764(4) . ?
Nb1 O4 1.962(2) . ?
Nb1 O3 1.988(4) . ?
Nb1 O5 1.989(4) 2_656 ?
Nb1 O2 2.056(3) . ?
Nb1 O6 2.507(4) . ?
Nb1 Mn2 3.2074(10) . ?
Mn2 O2 1.843(3) 6_565 ?
Mn2 O2 1.843(3) . ?
Mn2 O7 2.125(6) . ?
Mn2 O8 2.127(6) . ?
Mn2 O6 2.134(3) . ?
Mn2 O6 2.134(3) 5_666 ?
Mn2 Nb1 3.2074(10) 6_565 ?
Nb3 O9 1.762(4) . ?
Nb3 O3 1.927(3) . ?
Nb3 O5 1.929(3) . ?
Nb3 O7 2.087(3) . ?
Nb3 O8 2.087(3) 5_666 ?
Nb3 O6 2.4805(9) . ?
Nb3 Nb3 3.2513(12) 6_565 ?
O4 Nb1 1.962(2) 2_656 ?
O5 Nb1 1.989(4) 2_656 ?
O6 Nb2 2.134(3) 5_666 ?
O6 Mn2 2.134(3) 5_666 ?
O6 Nb3 2.4805(9) 2_656 ?
O6 Nb1 2.507(4) 2_656 ?
O7 Nb3 2.087(3) 6_565 ?
O8 Nb3 2.087(3) 5_666 ?
O8 Nb3 2.087(3) 2_656 ?
O18 O19 1.62(5) . ?
O20 O21 1.60(6) . ?
N1 C2 1.486(7) 6 ?
N1 C2 1.486(7) . ?
N1 C3 1.489(12) . ?
N1 C1 1.489(12) . ?
N2 C6 1.435(16) . ?
N2 C4 1.494(16) . ?
N2 C5 1.476(12) 6_565 ?
N2 C5 1.476(12) . ?
N3 C9 1.432(16) . ?
N3 C7 1.474(12) 6_565 ?
N3 C7 1.474(12) . ?
N3 C8 1.494(16) . ?
N4 C12 1.23(2) . ?
N4 C12 1.23(2) 7 ?
N4 C10 1.62(3) 7 ?
N4 C10 1.62(3) . ?
N4 C13 1.641(19) . ?
N4 C13 1.641(19) 7 ?
N4 C11 1.81(2) . ?
N4 C11 1.81(2) 7 ?
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 H3C 0.9800 . ?
C3 H3B 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 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 C12 1.32(5) . ?
C11 C12 1.66(4) . ?
C12 C13 1.38(5) . ?

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
O1 Nb1 O4 103.62(18) . . ?
O1 Nb1 O3 103.79(18) . . ?
O4 Nb1 O3 88.56(10) . . ?
O1 Nb1 O5 103.87(18) . 2_656 ?
O4 Nb1 O5 88.32(10) . 2_656 ?
O3 Nb1 O5 152.11(14) . 2_656 ?
O1 Nb1 O2 104.84(16) . . ?
O4 Nb1 O2 151.54(15) . . ?
O3 Nb1 O2 84.73(14) . . ?
O5 Nb1 O2 84.92(14) 2_656 . ?
O1 Nb1 O6 179.02(15) . . ?
O4 Nb1 O6 77.36(14) . . ?
O3 Nb1 O6 76.20(10) . . ?
O5 Nb1 O6 76.08(10) 2_656 . ?
O2 Nb1 O6 74.18(12) . . ?
O1 Nb1 Mn2 137.38(13) . . ?
O4 Nb1 Mn2 119.00(12) . . ?
O3 Nb1 Mn2 78.66(10) . . ?
O5 Nb1 Mn2 78.71(10) 2_656 . ?
O2 Nb1 Mn2 32.54(9) . . ?
O6 Nb1 Mn2 41.64(7) . . ?
O2 Mn2 O2 104.2(2) 6_565 . ?
O2 Mn2 O7 96.36(13) 6_565 . ?
O2 Mn2 O7 96.36(13) . . ?
O2 Mn2 O8 96.53(13) 6_565 . ?
O2 Mn2 O8 96.53(13) . . ?
O7 Mn2 O8 158.94(18) . . ?
O2 Mn2 O6 167.59(14) 6_565 . ?
O2 Mn2 O6 88.22(14) . . ?
O7 Mn2 O6 82.01(10) . . ?
O8 Mn2 O6 81.83(10) . . ?
O2 Mn2 O6 88.22(14) 6_565 5_666 ?
O2 Mn2 O6 167.59(14) . 5_666 ?
O7 Mn2 O6 82.01(10) . 5_666 ?
O8 Mn2 O6 81.83(10) . 5_666 ?
O6 Mn2 O6 79.4(2) . 5_666 ?
O2 Mn2 Nb1 141.08(10) 6_565 . ?
O2 Mn2 Nb1 36.89(10) . . ?
O7 Mn2 Nb1 90.180(16) . . ?
O8 Mn2 Nb1 90.191(16) . . ?
O6 Mn2 Nb1 51.33(10) . . ?
O6 Mn2 Nb1 130.70(10) 5_666 . ?
O2 Mn2 Nb1 36.89(10) 6_565 6_565 ?
O2 Mn2 Nb1 141.08(10) . 6_565 ?
O7 Mn2 Nb1 90.179(16) . 6_565 ?
O8 Mn2 Nb1 90.191(16) . 6_565 ?
O6 Mn2 Nb1 130.70(10) . 6_565 ?
O6 Mn2 Nb1 51.33(10) 5_666 6_565 ?
Nb1 Mn2 Nb1 177.97(3) . 6_565 ?
O9 Nb3 O3 102.37(17) . . ?
O9 Nb3 O5 102.45(18) . . ?
O3 Nb3 O5 94.33(15) . . ?
O9 Nb3 O7 104.9(2) . . ?
O3 Nb3 O7 89.57(15) . . ?
O5 Nb3 O7 150.88(18) . . ?
O9 Nb3 O8 104.9(2) . 5_666 ?
O3 Nb3 O8 150.86(17) . 5_666 ?
O5 Nb3 O8 89.57(15) . 5_666 ?
O7 Nb3 O8 73.83(15) . 5_666 ?
O9 Nb3 O6 179.64(18) . . ?
O3 Nb3 O6 77.90(13) . . ?
O5 Nb3 O6 77.76(13) . . ?
O7 Nb3 O6 74.89(17) . . ?
O8 Nb3 O6 74.75(17) 5_666 . ?
O9 Nb3 Nb3 95.73(14) . 6_565 ?
O3 Nb3 Nb3 128.33(10) . 6_565 ?
O5 Nb3 Nb3 128.35(11) . 6_565 ?
O7 Nb3 Nb3 38.83(11) . 6_565 ?
O8 Nb3 Nb3 38.85(11) 5_666 6_565 ?
O6 Nb3 Nb3 83.91(11) . 6_565 ?
Mn2 O2 Nb1 110.57(15) . . ?
Nb3 O3 Nb1 119.63(17) . . ?
Nb1 O4 Nb1 120.0(2) 2_656 . ?
Nb3 O5 Nb1 119.75(17) . 2_656 ?
Mn2 O6 Mn2 100.6(2) . 5_666 ?
Mn2 O6 Nb3 93.80(7) . . ?
Nb2 O6 Nb3 93.97(7) 5_666 . ?
Mn2 O6 Nb3 93.97(7) 5_666 . ?
Mn2 O6 Nb3 93.97(7) . 2_656 ?
Nb2 O6 Nb3 93.80(7) 5_666 2_656 ?
Mn2 O6 Nb3 93.80(7) 5_666 2_656 ?
Nb3 O6 Nb3 167.8(2) . 2_656 ?
Mn2 O6 Nb1 87.04(4) . . ?
Nb2 O6 Nb1 172.33(17) 5_666 . ?
Mn2 O6 Nb1 172.33(17) 5_666 . ?
Nb3 O6 Nb1 85.45(9) . . ?
Nb3 O6 Nb1 85.61(9) 2_656 . ?
Mn2 O6 Nb1 172.33(17) . 2_656 ?
Nb2 O6 Nb1 87.04(4) 5_666 2_656 ?
Mn2 O6 Nb1 87.04(4) 5_666 2_656 ?
Nb3 O6 Nb1 85.61(9) . 2_656 ?
Nb3 O6 Nb1 85.45(9) 2_656 2_656 ?
Nb1 O6 Nb1 85.30(15) . 2_656 ?
Nb3 O7 Nb3 102.3(2) . 6_565 ?
Nb3 O7 Mn2 106.61(17) . . ?
Nb3 O7 Mn2 106.61(17) 6_565 . ?
Nb3 O8 Nb3 102.3(2) 5_666 2_656 ?
Nb3 O8 Mn2 106.75(17) 5_666 . ?
Nb3 O8 Mn2 106.75(17) 2_656 . ?
C2 N1 C2 110.1(7) 6 . ?
C2 N1 C3 110.1(5) 6 . ?
C2 N1 C3 110.1(5) . . ?
C2 N1 C1 109.8(5) 6 . ?
C2 N1 C1 109.8(5) . . ?
C3 N1 C1 107.0(9) . . ?
C6 N2 C4 114.8(13) . . ?
C6 N2 C5 111.1(8) . 6_565 ?
C4 N2 C5 108.6(8) . 6_565 ?
C6 N2 C5 111.1(8) . . ?
C4 N2 C5 108.6(8) . . ?
C5 N2 C5 102.0(15) 6_565 . ?
C9 N3 C7 110.9(8) . 6_565 ?
C9 N3 C7 110.9(8) . . ?
C7 N3 C7 101.8(15) 6_565 . ?
C9 N3 C8 115.5(13) . . ?
C7 N3 C8 108.4(8) 6_565 . ?
C7 N3 C8 108.4(8) . . ?
C12 N4 C12 180.0 . 7 ?
C12 N4 C10 127(2) . 7 ?
C12 N4 C10 53(2) 7 7 ?
C12 N4 C10 53(2) . . ?
C12 N4 C10 127(2) 7 . ?
C10 N4 C10 180.0 7 . ?
C12 N4 C13 55(2) . . ?
C12 N4 C13 125(2) 7 . ?
C10 N4 C13 82.4(13) 7 . ?
C10 N4 C13 97.6(13) . . ?
C12 N4 C13 125(2) . 7 ?
C12 N4 C13 55(2) 7 7 ?
C10 N4 C13 97.6(13) 7 7 ?
C10 N4 C13 82.4(13) . 7 ?
C13 N4 C13 180.0 . 7 ?
C12 N4 C11 62.8(19) . . ?
C12 N4 C11 117.2(19) 7 . ?
C10 N4 C11 90.4(13) 7 . ?
C10 N4 C11 89.6(13) . . ?
C13 N4 C11 89.7(15) . . ?
C13 N4 C11 90.3(15) 7 . ?
C12 N4 C11 117.2(19) . 7 ?
C12 N4 C11 62.8(19) 7 7 ?
C10 N4 C11 89.6(13) 7 7 ?
C10 N4 C11 90.4(13) . 7 ?
C13 N4 C11 90.3(15) . 7 ?
C13 N4 C11 89.7(15) 7 7 ?
C11 N4 C11 180.0 . 7 ?
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 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3C C3 H3B 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 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 . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C12 C10 N4 48.4(13) . . ?
C12 C11 N4 41.5(9) . . ?
N4 C12 C10 79(2) . . ?
N4 C12 C13 78(2) . . ?
C10 C12 C13 131(3) . . ?
N4 C12 C11 75.7(19) . . ?
C10 C12 C11 108(3) . . ?
C13 C12 C11 106(3) . . ?
C12 C13 N4 47.3(10) . . ?

_refine_diff_density_max         0.928
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.129

_database_code_depnum_ccdc_archive 'CCDC 990476'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_TMA-CrNb9

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            'Tetramethylammonium nonaniobochromate'
_chemical_melting_point          ?
_chemical_formula_moiety         'H2 Cr Nb9 O28, 6 (C4 H12 N), 14 (H2 O)'
_chemical_formula_sum            'C24 H93 Cr N6 Nb9 O42.50'
_chemical_formula_weight         2034.23

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   16.6016(8)
_cell_length_b                   17.2436(8)
_cell_length_c                   24.0263(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.1210(10)
_cell_angle_gamma                90.00
_cell_volume                     6607.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    9049
_cell_measurement_theta_min      2.81
_cell_measurement_theta_max      27.52

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4048
_exptl_absorpt_coefficient_mu    1.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4515
_exptl_absorpt_correction_T_max  0.6062
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            66308
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.81
_diffrn_reflns_theta_max         26.37
_reflns_number_total             13488
_reflns_number_gt                12337
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+26.7566P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13488
_refine_ls_number_parameters     884
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0656
_refine_ls_wR_factor_gt          0.0643
_refine_ls_goodness_of_fit_ref   1.301
_refine_ls_restrained_S_all      1.301
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr2 Cr 0.57866(3) 0.91109(3) 0.74305(2) 0.0188(2) Uani 0.701(5) 1 d P A 1
Cr9 Cr 0.41350(2) 0.82376(2) 0.762222(16) 0.01295(16) Uani 0.324(5) 1 d P A 3
Nb1 Nb 0.70151(2) 0.832365(19) 0.859323(14) 0.01128(7) Uani 1 1 d . . .
Nb2 Nb 0.57866(3) 0.91109(3) 0.74305(2) 0.0188(2) Uani 0.299(5) 1 d P A 2
Nb3 Nb 0.58289(2) 0.719132(18) 0.754829(13) 0.01032(7) Uani 1 1 d . A .
Nb4 Nb 0.53108(2) 0.744574(18) 0.880103(13) 0.01059(7) Uani 1 1 d . . .
Nb5 Nb 0.53590(2) 0.939635(18) 0.866767(13) 0.01051(7) Uani 1 1 d . A .
Nb6 Nb 0.41734(2) 1.018619(18) 0.748998(13) 0.01024(7) Uani 1 1 d . . .
Nb7 Nb 0.46850(2) 0.993285(18) 0.624191(13) 0.01053(7) Uani 1 1 d . . .
Nb8 Nb 0.463030(19) 0.798271(18) 0.637652(13) 0.00974(7) Uani 1 1 d . . .
Nb9 Nb 0.41350(2) 0.82376(2) 0.762222(16) 0.01295(16) Uani 0.676(5) 1 d P A 4
Nb10 Nb 0.297416(19) 0.906200(18) 0.643761(13) 0.01027(7) Uani 1 1 d . A .
O1 O 0.80800(16) 0.83312(15) 0.89707(11) 0.0168(5) Uani 1 1 d . A .
O2 O 0.69209(18) 0.90485(17) 0.78836(12) 0.0145(6) Uani 1 1 d . A .
O3 O 0.69146(15) 0.74849(15) 0.80158(11) 0.0134(5) Uani 1 1 d . A .
O4 O 0.65161(15) 0.76404(14) 0.90526(10) 0.0130(5) Uani 1 1 d . A .
O5 O 0.65464(15) 0.92274(15) 0.89091(10) 0.0132(5) Uani 1 1 d . A .
O6 O 0.58907(18) 0.97753(18) 0.68187(13) 0.0141(6) Uani 1 1 d . A .
O7 O 0.58258(15) 0.81111(14) 0.69828(10) 0.0121(5) Uani 1 1 d . A .
O8 O 0.60056(17) 0.63681(15) 0.71625(11) 0.0167(5) Uani 1 1 d . . .
O9 O 0.54736(16) 0.67594(14) 0.81824(11) 0.0135(5) Uani 1 1 d . A .
O10 O 0.51232(16) 0.68065(15) 0.93163(11) 0.0166(5) Uani 1 1 d . A .
O11 O 0.51084(15) 0.84973(15) 0.90785(10) 0.0130(5) Uani 1 1 d . A .
O12 O 0.52247(16) 1.01770(15) 0.91055(11) 0.0162(5) Uani 1 1 d . . .
O13 O 0.54270(15) 0.99184(14) 0.79062(10) 0.0112(5) Uani 1 1 d . A .
O14 O 0.54914(15) 0.83500(14) 0.80237(10) 0.0104(5) Uani 1 1 d . A .
O15 O 0.39892(17) 1.10012(15) 0.78780(11) 0.0168(5) Uani 1 1 d . A .
O16 O 0.45289(15) 1.06187(14) 0.68563(11) 0.0127(5) Uani 1 1 d . A .
O17 O 0.48833(16) 1.05662(15) 0.57270(11) 0.0166(5) Uani 1 1 d . A .
O18 O 0.48762(15) 0.88756(15) 0.59702(10) 0.0128(5) Uani 1 1 d . A .
O19 O 0.47663(17) 0.72009(15) 0.59390(11) 0.0162(5) Uani 1 1 d . A .
O20 O 0.45470(15) 0.74581(14) 0.71445(10) 0.0113(5) Uani 1 1 d . A .
O21 O 0.41052(16) 0.75949(15) 0.82291(11) 0.0139(5) Uani 1 1 d . A .
O22 O 0.41462(15) 0.92515(14) 0.80588(10) 0.0114(5) Uani 1 1 d . A .
O23 O 0.44936(15) 0.90286(14) 0.70206(10) 0.0103(5) Uani 1 1 d . A .
O24 O 0.30751(15) 0.98971(14) 0.70185(11) 0.0128(5) Uani 1 1 d . A .
O25 O 0.34797(15) 0.97437(14) 0.59802(10) 0.0124(5) Uani 1 1 d . A .
O26 O 0.34374(15) 0.81474(14) 0.61386(10) 0.0126(5) Uani 1 1 d . A .
O27 O 0.30514(15) 0.83285(15) 0.71519(11) 0.0131(5) Uani 1 1 d . . .
O28 O 0.19161(16) 0.90561(15) 0.60502(11) 0.0158(5) Uani 1 1 d . . .
O29 O 0.41689(19) 0.89674(19) 0.98456(14) 0.0221(6) Uani 1 1 d . . .
O30 O 0.9319(2) 0.3367(2) 0.98359(15) 0.0291(7) Uani 1 1 d . . .
O31 O 0.0290(2) 0.8857(2) 0.53971(14) 0.0249(7) Uani 1 1 d . . .
O32 O 0.4494(2) 0.6339(2) 0.48700(15) 0.0292(7) Uani 1 1 d . . .
O33 O 0.9693(2) 0.9327(2) 0.13081(16) 0.0278(7) Uani 1 1 d . . .
O34 O 0.8436(2) 0.1544(2) 0.11853(18) 0.0393(9) Uani 1 1 d . . .
O35 O 0.1818(2) 1.0097(2) 0.24116(16) 0.0297(7) Uani 1 1 d . . .
O36 O 0.9395(2) 0.0669(2) 0.06622(19) 0.0381(9) Uani 1 1 d . . .
O37 O 0.1995(2) 0.4237(3) 0.62550(15) 0.0498(11) Uani 1 1 d . . .
O38 O 0.3325(3) 0.2493(3) 0.7670(3) 0.0852(19) Uani 1 1 d . . .
O39 O 0.0332(3) 0.3292(2) 0.36803(17) 0.0360(8) Uani 1 1 d . . .
O40 O 0.0633(5) 0.1731(3) 0.3918(3) 0.053(3) Uani 0.85(2) 1 d P . .
O41 O 0.1654(3) 0.0867(3) 0.3440(2) 0.0344(17) Uani 0.769(14) 1 d P . .
O42 O 0.2519(12) 0.1509(13) 0.3221(9) 0.062(8) Uani 0.218(14) 1 d P . .
O43 O 0.3180(2) 0.1503(3) 0.36930(17) 0.0431(15) Uani 0.908(13) 1 d P . .
O44 O 0.0015(14) 0.1859(10) 0.3708(7) 0.053(7) Uani 0.30(2) 1 d P . .
O45 O 0.1653(15) 0.1300(17) 0.3979(13) 0.21(2) Uani 0.39(2) 1 d P . .
N1 N 0.7826(2) 0.5793(2) 0.93838(14) 0.0183(7) Uani 1 1 d . . .
N2 N 0.2915(2) 0.4039(2) 0.41687(16) 0.0236(8) Uani 1 1 d . . .
N3 N 0.0554(2) 0.2464(2) 0.19592(16) 0.0222(7) Uani 1 1 d . . .
N4 N 0.9187(2) 0.9992(2) 0.28477(14) 0.0191(7) Uani 1 1 d . . .
N5 N 0.6987(2) 0.8506(2) 0.06614(14) 0.0202(7) Uani 1 1 d . . .
N6 N 0.7181(2) 0.3314(2) 0.06458(15) 0.0212(7) Uani 1 1 d . . .
C1 C 0.8341(3) 0.6461(3) 0.96814(19) 0.0287(10) Uani 1 1 d . . .
H1A H 0.8419 0.6421 1.0100 0.043 Uiso 1 1 calc R . .
H1B H 0.8052 0.6947 0.9538 0.043 Uiso 1 1 calc R . .
H1C H 0.8888 0.6452 0.9601 0.043 Uiso 1 1 calc R . .
C2 C 0.8292(3) 0.5057(2) 0.95845(17) 0.0215(8) Uani 1 1 d . . .
H2A H 0.8839 0.5076 0.9505 0.032 Uiso 1 1 calc R . .
H2B H 0.7969 0.4617 0.9378 0.032 Uiso 1 1 calc R . .
H2C H 0.8372 0.4995 1.0002 0.032 Uiso 1 1 calc R . .
C3 C 0.7677(3) 0.5871(3) 0.87441(18) 0.0325(11) Uani 1 1 d . . .
H3A H 0.8216 0.5872 0.8651 0.049 Uiso 1 1 calc R . .
H3B H 0.7381 0.6358 0.8613 0.049 Uiso 1 1 calc R . .
H3C H 0.7336 0.5434 0.8548 0.049 Uiso 1 1 calc R . .
C4 C 0.7005(3) 0.5783(3) 0.9525(2) 0.0316(10) Uani 1 1 d . . .
H4A H 0.6674 0.5337 0.9335 0.047 Uiso 1 1 calc R . .
H4B H 0.6699 0.6263 0.9386 0.047 Uiso 1 1 calc R . .
H4C H 0.7104 0.5741 0.9945 0.047 Uiso 1 1 calc R . .
C5 C 0.2411(3) 0.4174(3) 0.45901(19) 0.0291(10) Uani 1 1 d . . .
H5A H 0.2024 0.3740 0.4572 0.044 Uiso 1 1 calc R . .
H5B H 0.2091 0.4656 0.4491 0.044 Uiso 1 1 calc R . .
H5C H 0.2789 0.4214 0.4983 0.044 Uiso 1 1 calc R . .
C6 C 0.3508(3) 0.4703(3) 0.4192(2) 0.0356(11) Uani 1 1 d . . .
H6A H 0.3191 0.5189 0.4114 0.053 Uiso 1 1 calc R . .
H6B H 0.3812 0.4627 0.3900 0.053 Uiso 1 1 calc R . .
H6C H 0.3909 0.4726 0.4578 0.053 Uiso 1 1 calc R . .
C7 C 0.3404(3) 0.3303(3) 0.4323(3) 0.0400(13) Uani 1 1 d . . .
H7A H 0.3746 0.3328 0.4727 0.060 Uiso 1 1 calc R . .
H7B H 0.3769 0.3235 0.4069 0.060 Uiso 1 1 calc R . .
H7C H 0.3016 0.2863 0.4275 0.060 Uiso 1 1 calc R . .
C8 C 0.2328(3) 0.3986(3) 0.3573(2) 0.0349(11) Uani 1 1 d . . .
H8A H 0.1927 0.3565 0.3559 0.052 Uiso 1 1 calc R . .
H8B H 0.2648 0.3882 0.3294 0.052 Uiso 1 1 calc R . .
H8C H 0.2025 0.4477 0.3474 0.052 Uiso 1 1 calc R . .
C9 C 0.1226(3) 0.2999(3) 0.2276(2) 0.0359(11) Uani 1 1 d . . .
H9A H 0.1717 0.2943 0.2127 0.054 Uiso 1 1 calc R . .
H9B H 0.1384 0.2873 0.2690 0.054 Uiso 1 1 calc R . .
H9C H 0.1022 0.3535 0.2220 0.054 Uiso 1 1 calc R . .
C10 C 0.0857(3) 0.1639(3) 0.2033(2) 0.0349(12) Uani 1 1 d . . .
H10A H 0.1332 0.1578 0.1869 0.052 Uiso 1 1 calc R . .
H10B H 0.0402 0.1291 0.1833 0.052 Uiso 1 1 calc R . .
H10C H 0.1035 0.1509 0.2447 0.052 Uiso 1 1 calc R . .
C11 C 0.0299(3) 0.2660(3) 0.13296(19) 0.0298(10) Uani 1 1 d . . .
H11A H 0.0089 0.3194 0.1278 0.045 Uiso 1 1 calc R . .
H11B H -0.0145 0.2304 0.1123 0.045 Uiso 1 1 calc R . .
H11C H 0.0783 0.2610 0.1174 0.045 Uiso 1 1 calc R . .
C12 C -0.0183(3) 0.2537(2) 0.22022(19) 0.0229(9) Uani 1 1 d . . .
H12A H -0.0013 0.2397 0.2614 0.034 Uiso 1 1 calc R . .
H12B H -0.0632 0.2190 0.1992 0.034 Uiso 1 1 calc R . .
H12C H -0.0386 0.3074 0.2160 0.034 Uiso 1 1 calc R . .
C13 C 0.9316(4) 0.9854(3) 0.34751(19) 0.0364(12) Uani 1 1 d . . .
H13A H 0.9588 0.9350 0.3582 0.055 Uiso 1 1 calc R . .
H13B H 0.8772 0.9857 0.3561 0.055 Uiso 1 1 calc R . .
H13C H 0.9672 1.0265 0.3697 0.055 Uiso 1 1 calc R . .
C14 C 1.0008(3) 1.0024(3) 0.2722(2) 0.0356(12) Uani 1 1 d . . .
H14A H 1.0340 1.0451 0.2940 0.053 Uiso 1 1 calc R . .
H14B H 0.9923 1.0107 0.2306 0.053 Uiso 1 1 calc R . .
H14C H 1.0307 0.9533 0.2837 0.053 Uiso 1 1 calc R . .
C15 C 0.8692(4) 0.9331(4) 0.2525(2) 0.0512(15) Uani 1 1 d . . .
H15A H 0.8665 0.9373 0.2114 0.077 Uiso 1 1 calc R . .
H15B H 0.8123 0.9345 0.2570 0.077 Uiso 1 1 calc R . .
H15C H 0.8963 0.8841 0.2680 0.077 Uiso 1 1 calc R . .
C16 C 0.8740(3) 1.0740(3) 0.2673(2) 0.0381(13) Uani 1 1 d . . .
H16A H 0.9057 1.1161 0.2910 0.057 Uiso 1 1 calc R . .
H16B H 0.8180 1.0711 0.2731 0.057 Uiso 1 1 calc R . .
H16C H 0.8691 1.0841 0.2264 0.057 Uiso 1 1 calc R . .
C17 C 0.7425(3) 0.8660(3) 0.12837(18) 0.0312(10) Uani 1 1 d . . .
H17A H 0.7808 0.9100 0.1312 0.047 Uiso 1 1 calc R . .
H17B H 0.7744 0.8200 0.1455 0.047 Uiso 1 1 calc R . .
H17C H 0.7010 0.8782 0.1492 0.047 Uiso 1 1 calc R . .
C18 C 0.7627(3) 0.8377(3) 0.03383(19) 0.0300(10) Uani 1 1 d . . .
H18A H 0.7344 0.8277 -0.0071 0.045 Uiso 1 1 calc R . .
H18B H 0.7977 0.7930 0.0503 0.045 Uiso 1 1 calc R . .
H18C H 0.7981 0.8839 0.0371 0.045 Uiso 1 1 calc R . .
C19 C 0.6443(3) 0.7806(3) 0.0608(2) 0.0379(12) Uani 1 1 d . . .
H19A H 0.6034 0.7886 0.0828 0.057 Uiso 1 1 calc R . .
H19B H 0.6790 0.7353 0.0760 0.057 Uiso 1 1 calc R . .
H19C H 0.6146 0.7720 0.0199 0.057 Uiso 1 1 calc R . .
C20 C 0.6457(3) 0.9186(3) 0.0409(2) 0.0289(10) Uani 1 1 d . . .
H20A H 0.6179 0.9089 -0.0001 0.043 Uiso 1 1 calc R . .
H20B H 0.6810 0.9649 0.0446 0.043 Uiso 1 1 calc R . .
H20C H 0.6033 0.9269 0.0618 0.043 Uiso 1 1 calc R . .
C21 C 0.7414(3) 0.3283(3) 0.12951(19) 0.0308(10) Uani 1 1 d . . .
H21A H 0.7720 0.3755 0.1455 0.046 Uiso 1 1 calc R . .
H21B H 0.7770 0.2829 0.1431 0.046 Uiso 1 1 calc R . .
H21C H 0.6904 0.3243 0.1423 0.046 Uiso 1 1 calc R . .
C22 C 0.7962(3) 0.3322(3) 0.0455(2) 0.0289(10) Uani 1 1 d . . .
H22A H 0.7816 0.3338 0.0031 0.043 Uiso 1 1 calc R . .
H22B H 0.8290 0.2854 0.0595 0.043 Uiso 1 1 calc R . .
H22C H 0.8295 0.3781 0.0614 0.043 Uiso 1 1 calc R . .
C23 C 0.6675(3) 0.2610(2) 0.0400(2) 0.0267(10) Uani 1 1 d . . .
H23A H 0.6167 0.2595 0.0531 0.040 Uiso 1 1 calc R . .
H23B H 0.7009 0.2143 0.0531 0.040 Uiso 1 1 calc R . .
H23C H 0.6519 0.2634 -0.0024 0.040 Uiso 1 1 calc R . .
C24 C 0.6684(3) 0.4025(2) 0.0434(2) 0.0293(10) Uani 1 1 d . . .
H24A H 0.7011 0.4484 0.0601 0.044 Uiso 1 1 calc R . .
H24B H 0.6163 0.4012 0.0550 0.044 Uiso 1 1 calc R . .
H24C H 0.6550 0.4048 0.0010 0.044 Uiso 1 1 calc R . .
H1 H 0.716(4) 0.925(4) 0.782(3) 0.04(2) Uiso 1 1 d . . .
H2 H 0.605(4) 0.957(4) 0.669(3) 0.04(2) Uiso 1 1 d . . .
H3 H 0.451(3) 0.883(3) 0.970(2) 0.036(16) Uiso 1 1 d . . .
H4 H 0.440(3) 0.927(3) 1.010(2) 0.036(15) Uiso 1 1 d . . .
H5 H 0.966(4) 0.345(4) 0.968(3) 0.07(2) Uiso 1 1 d . . .
H6 H 0.946(5) 0.365(4) 1.010(3) 0.08(3) Uiso 1 1 d . . .
H7 H 0.028(3) 0.870(3) 0.507(3) 0.037(15) Uiso 1 1 d . . .
H8 H 0.074(4) 0.888(3) 0.555(2) 0.033(16) Uiso 1 1 d . . .
H9 H 0.412(3) 0.644(3) 0.464(2) 0.027(15) Uiso 1 1 d . . .
H10 H 0.462(3) 0.668(3) 0.513(2) 0.031(14) Uiso 1 1 d . . .
H11 H 1.006(4) 0.924(4) 0.155(3) 0.05(2) Uiso 1 1 d . . .
H12 H 0.967(3) 0.898(3) 0.114(2) 0.021(14) Uiso 1 1 d . . .
H13 H 0.875(5) 0.122(4) 0.111(3) 0.07(2) Uiso 1 1 d . . .
H14 H 0.801(4) 0.133(4) 0.123(3) 0.049(18) Uiso 1 1 d . . .
H15 H 0.157(4) 0.963(4) 0.235(3) 0.06(2) Uiso 1 1 d . . .
H16 H 0.175(6) 1.026(5) 0.269(4) 0.11(3) Uiso 1 1 d . . .
H17 H 0.979(5) 0.084(5) 0.059(4) 0.09(3) Uiso 1 1 d . . .
H18 H 0.957(6) 0.036(6) 0.089(4) 0.11(3) Uiso 1 1 d . . .
H19 H 0.282(3) 0.222(3) 0.754(2) 0.021(12) Uiso 1 1 d . . .
H20 H 0.037(4) 0.363(4) 0.392(3) 0.05(2) Uiso 1 1 d . . .
H21 H -0.006(4) 0.341(4) 0.344(3) 0.05(2) Uiso 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Cr2 O2 1.898(3) . ?
Cr2 O6 1.909(3) . ?
Cr2 O13 1.995(2) . ?
Cr2 O7 2.043(3) . ?
Cr2 O14 2.093(2) . ?
Cr2 O23 2.103(2) . ?
Cr9 O21 1.843(3) . ?
Cr9 O27 1.846(3) . ?
Cr9 O20 2.007(2) . ?
Cr9 O22 2.036(3) . ?
Cr9 O23 2.187(2) . ?
Cr9 O14 2.198(2) . ?
Nb1 O1 1.749(3) . ?
Nb1 O4 1.949(3) . ?
Nb1 O3 1.979(3) . ?
Nb1 O5 1.984(3) . ?
Nb1 O2 2.085(3) . ?
Nb1 O14 2.520(2) . ?
Nb1 Nb3 3.3538(5) . ?
Nb1 Nb5 3.3594(5) . ?
Nb3 O8 1.764(3) . ?
Nb3 O3 1.908(3) . ?
Nb3 O9 1.930(2) . ?
Nb3 O7 2.088(2) . ?
Nb3 O20 2.130(2) . ?
Nb3 O14 2.443(2) . ?
Nb3 Nb8 3.2614(4) . ?
Nb4 O10 1.749(3) . ?
Nb4 O4 1.952(3) . ?
Nb4 O9 1.976(3) . ?
Nb4 O11 1.992(3) . ?
Nb4 O21 2.105(3) . ?
Nb4 O14 2.514(2) . ?
Nb5 O12 1.760(3) . ?
Nb5 O5 1.916(3) . ?
Nb5 O11 1.944(3) . ?
Nb5 O13 2.070(2) . ?
Nb5 O22 2.150(2) . ?
Nb5 O14 2.426(2) . ?
Nb5 Nb6 3.2623(5) . ?
Nb6 O15 1.760(3) . ?
Nb6 O24 1.926(2) . ?
Nb6 O16 1.929(2) . ?
Nb6 O13 2.095(2) . ?
Nb6 O22 2.122(2) . ?
Nb6 O23 2.423(2) . ?
Nb7 O17 1.749(3) . ?
Nb7 O25 1.951(3) . ?
Nb7 O16 1.964(3) . ?
Nb7 O18 1.991(3) . ?
Nb7 O6 2.112(3) . ?
Nb7 O23 2.523(2) . ?
Nb7 Nb10 3.3594(5) . ?
Nb8 O19 1.762(3) . ?
Nb8 O26 1.924(2) . ?
Nb8 O18 1.927(3) . ?
Nb8 O20 2.094(2) . ?
Nb8 O7 2.122(3) . ?
Nb8 O23 2.428(2) . ?
Nb8 Nb10 3.3569(5) . ?
Nb10 O28 1.745(3) . ?
Nb10 O25 1.951(2) . ?
Nb10 O26 1.975(2) . ?
Nb10 O24 1.980(3) . ?
Nb10 O27 2.107(2) . ?
Nb10 O23 2.523(2) . ?
O2 H1 0.58(6) . ?
O6 H2 0.58(6) . ?
O29 H3 0.77(6) . ?
O29 H4 0.81(6) . ?
O30 H5 0.77(7) . ?
O30 H6 0.78(8) . ?
O31 H7 0.83(6) . ?
O31 H8 0.74(6) . ?
O32 H9 0.72(5) . ?
O32 H10 0.84(6) . ?
O33 H11 0.74(7) . ?
O33 H12 0.72(5) . ?
O34 H13 0.82(8) . ?
O34 H14 0.84(7) . ?
O35 H15 0.90(7) . ?
O35 H16 0.76(9) . ?
O36 H17 0.78(9) . ?
O36 H18 0.76(9) . ?
O38 H19 0.93(5) . ?
O39 H20 0.81(7) . ?
O39 H21 0.77(7) . ?
O40 O44 1.034(19) . ?
O40 O45 1.82(2) . ?
O41 O45 1.49(3) . ?
O42 O43 1.341(19) . ?
N1 C4 1.492(5) . ?
N1 C1 1.493(5) . ?
N1 C3 1.494(5) . ?
N1 C2 1.495(5) . ?
N2 C8 1.494(6) . ?
N2 C7 1.497(5) . ?
N2 C5 1.499(5) . ?
N2 C6 1.501(6) . ?
N3 C9 1.485(6) . ?
N3 C11 1.492(5) . ?
N3 C12 1.500(5) . ?
N3 C10 1.502(5) . ?
N4 C14 1.478(5) . ?
N4 C13 1.482(5) . ?
N4 C16 1.489(5) . ?
N4 C15 1.490(6) . ?
N5 C20 1.490(5) . ?
N5 C19 1.491(6) . ?
N5 C17 1.494(5) . ?
N5 C18 1.497(5) . ?
N6 C24 1.487(6) . ?
N6 C22 1.490(5) . ?
N6 C21 1.500(6) . ?
N6 C23 1.501(5) . ?
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 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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 Cr2 O6 100.84(13) . . ?
O2 Cr2 O13 96.78(11) . . ?
O6 Cr2 O13 97.33(12) . . ?
O2 Cr2 O7 94.74(11) . . ?
O6 Cr2 O7 94.48(12) . . ?
O13 Cr2 O7 161.64(10) . . ?
O2 Cr2 O14 87.51(11) . . ?
O6 Cr2 O14 171.46(11) . . ?
O13 Cr2 O14 83.32(10) . . ?
O7 Cr2 O14 82.95(10) . . ?
O2 Cr2 O23 170.24(12) . . ?
O6 Cr2 O23 88.78(11) . . ?
O13 Cr2 O23 83.48(10) . . ?
O7 Cr2 O23 82.77(10) . . ?
O14 Cr2 O23 82.82(9) . . ?
O21 Cr9 O27 107.44(11) . . ?
O21 Cr9 O20 97.93(11) . . ?
O27 Cr9 O20 97.80(11) . . ?
O21 Cr9 O22 96.16(10) . . ?
O27 Cr9 O22 96.34(10) . . ?
O20 Cr9 O22 156.03(10) . . ?
O21 Cr9 O23 165.93(10) . . ?
O27 Cr9 O23 86.58(10) . . ?
O20 Cr9 O23 80.86(9) . . ?
O22 Cr9 O23 80.77(9) . . ?
O21 Cr9 O14 87.42(10) . . ?
O27 Cr9 O14 165.10(10) . . ?
O20 Cr9 O14 80.78(9) . . ?
O22 Cr9 O14 80.59(9) . . ?
O23 Cr9 O14 78.54(9) . . ?
O1 Nb1 O4 103.78(11) . . ?
O1 Nb1 O3 104.21(11) . . ?
O4 Nb1 O3 89.36(10) . . ?
O1 Nb1 O5 104.07(11) . . ?
O4 Nb1 O5 89.12(10) . . ?
O3 Nb1 O5 151.21(10) . . ?
O1 Nb1 O2 104.78(12) . . ?
O4 Nb1 O2 151.43(11) . . ?
O3 Nb1 O2 83.81(11) . . ?
O5 Nb1 O2 83.89(11) . . ?
O1 Nb1 O14 177.86(11) . . ?
O4 Nb1 O14 78.35(9) . . ?
O3 Nb1 O14 75.87(9) . . ?
O5 Nb1 O14 75.67(9) . . ?
O2 Nb1 O14 73.09(10) . . ?
O1 Nb1 Nb3 133.75(9) . . ?
O4 Nb1 Nb3 79.54(7) . . ?
O3 Nb1 Nb3 29.77(7) . . ?
O5 Nb1 Nb3 122.17(7) . . ?
O2 Nb1 Nb3 80.89(8) . . ?
O14 Nb1 Nb3 46.51(5) . . ?
O1 Nb1 Nb5 133.85(9) . . ?
O4 Nb1 Nb5 79.63(7) . . ?
O3 Nb1 Nb5 121.92(7) . . ?
O5 Nb1 Nb5 29.96(7) . . ?
O2 Nb1 Nb5 80.60(8) . . ?
O14 Nb1 Nb5 46.06(5) . . ?
Nb3 Nb1 Nb5 92.367(11) . . ?
O8 Nb3 O3 104.78(12) . . ?
O8 Nb3 O9 103.66(11) . . ?
O3 Nb3 O9 94.79(11) . . ?
O8 Nb3 O7 103.89(11) . . ?
O3 Nb3 O7 90.73(10) . . ?
O9 Nb3 O7 149.45(10) . . ?
O8 Nb3 O20 103.03(11) . . ?
O3 Nb3 O20 150.67(10) . . ?
O9 Nb3 O20 87.55(10) . . ?
O7 Nb3 O20 73.61(9) . . ?
O8 Nb3 O14 175.76(10) . . ?
O3 Nb3 O14 79.02(9) . . ?
O9 Nb3 O14 77.67(9) . . ?
O7 Nb3 O14 73.95(9) . . ?
O20 Nb3 O14 72.92(9) . . ?
O8 Nb3 Nb8 91.93(9) . . ?
O3 Nb3 Nb8 130.33(8) . . ?
O9 Nb3 Nb8 126.59(8) . . ?
O7 Nb3 Nb8 39.61(7) . . ?
O20 Nb3 Nb8 39.05(6) . . ?
O14 Nb3 Nb8 84.10(6) . . ?
O8 Nb3 Nb1 135.49(9) . . ?
O3 Nb3 Nb1 30.98(8) . . ?
O9 Nb3 Nb1 83.01(8) . . ?
O7 Nb3 Nb1 86.54(7) . . ?
O20 Nb3 Nb1 121.33(7) . . ?
O14 Nb3 Nb1 48.47(6) . . ?
Nb8 Nb3 Nb1 119.557(12) . . ?
O10 Nb4 O4 104.95(11) . . ?
O10 Nb4 O9 104.08(11) . . ?
O4 Nb4 O9 89.61(10) . . ?
O10 Nb4 O11 104.89(11) . . ?
O4 Nb4 O11 89.63(10) . . ?
O9 Nb4 O11 150.19(10) . . ?
O10 Nb4 O21 102.42(11) . . ?
O4 Nb4 O21 152.63(10) . . ?
O9 Nb4 O21 83.46(10) . . ?
O11 Nb4 O21 83.64(10) . . ?
O10 Nb4 O14 176.54(10) . . ?
O4 Nb4 O14 78.46(9) . . ?
O9 Nb4 O14 75.13(9) . . ?
O11 Nb4 O14 75.53(9) . . ?
O21 Nb4 O14 74.17(9) . . ?
O12 Nb5 O5 103.04(11) . . ?
O12 Nb5 O11 103.06(11) . . ?
O5 Nb5 O11 94.14(11) . . ?
O12 Nb5 O13 104.04(11) . . ?
O5 Nb5 O13 91.71(10) . . ?
O11 Nb5 O13 150.17(10) . . ?
O12 Nb5 O22 104.21(11) . . ?
O5 Nb5 O22 151.49(10) . . ?
O11 Nb5 O22 87.76(10) . . ?
O13 Nb5 O22 73.72(9) . . ?
O12 Nb5 O14 177.11(10) . . ?
O5 Nb5 O14 79.18(9) . . ?
O11 Nb5 O14 78.51(9) . . ?
O13 Nb5 O14 73.92(9) . . ?
O22 Nb5 O14 73.33(9) . . ?
O12 Nb5 Nb6 93.04(9) . . ?
O5 Nb5 Nb6 130.41(8) . . ?
O11 Nb5 Nb6 127.64(7) . . ?
O13 Nb5 Nb6 38.71(7) . . ?
O22 Nb5 Nb6 39.89(7) . . ?
O14 Nb5 Nb6 84.09(6) . . ?
O12 Nb5 Nb1 133.97(9) . . ?
O5 Nb5 Nb1 31.14(8) . . ?
O11 Nb5 Nb1 83.20(7) . . ?
O13 Nb5 Nb1 86.91(7) . . ?
O22 Nb5 Nb1 121.70(7) . . ?
O14 Nb5 Nb1 48.41(6) . . ?
Nb6 Nb5 Nb1 119.296(12) . . ?
O15 Nb6 O24 104.06(12) . . ?
O15 Nb6 O16 104.22(11) . . ?
O24 Nb6 O16 94.76(10) . . ?
O15 Nb6 O13 102.64(11) . . ?
O24 Nb6 O13 151.22(10) . . ?
O16 Nb6 O13 88.90(10) . . ?
O15 Nb6 O22 103.15(11) . . ?
O24 Nb6 O22 89.79(10) . . ?
O16 Nb6 O22 150.21(10) . . ?
O13 Nb6 O22 73.81(9) . . ?
O15 Nb6 O23 175.86(11) . . ?
O24 Nb6 O23 78.89(9) . . ?
O16 Nb6 O23 78.26(9) . . ?
O13 Nb6 O23 73.94(9) . . ?
O22 Nb6 O23 73.78(9) . . ?
O15 Nb6 Nb5 91.47(9) . . ?
O24 Nb6 Nb5 130.30(8) . . ?
O16 Nb6 Nb5 127.07(7) . . ?
O13 Nb6 Nb5 38.17(7) . . ?
O22 Nb6 Nb5 40.52(7) . . ?
O23 Nb6 Nb5 84.39(6) . . ?
O17 Nb7 O25 104.72(11) . . ?
O17 Nb7 O16 104.22(11) . . ?
O25 Nb7 O16 90.30(10) . . ?
O17 Nb7 O18 105.15(11) . . ?
O25 Nb7 O18 89.08(10) . . ?
O16 Nb7 O18 149.76(10) . . ?
O17 Nb7 O6 102.37(12) . . ?
O25 Nb7 O6 152.90(10) . . ?
O16 Nb7 O6 83.29(11) . . ?
O18 Nb7 O6 83.63(11) . . ?
O17 Nb7 O23 176.42(10) . . ?
O25 Nb7 O23 78.84(9) . . ?
O16 Nb7 O23 75.20(9) . . ?
O18 Nb7 O23 75.03(9) . . ?
O6 Nb7 O23 74.06(9) . . ?
O17 Nb7 Nb10 135.30(9) . . ?
O25 Nb7 Nb10 30.58(7) . . ?
O16 Nb7 Nb10 82.58(7) . . ?
O18 Nb7 Nb10 81.64(7) . . ?
O6 Nb7 Nb10 122.33(8) . . ?
O23 Nb7 Nb10 48.27(5) . . ?
O19 Nb8 O26 103.15(11) . . ?
O19 Nb8 O18 103.23(11) . . ?
O26 Nb8 O18 94.42(11) . . ?
O19 Nb8 O20 104.24(11) . . ?
O26 Nb8 O20 90.64(10) . . ?
O18 Nb8 O20 150.11(10) . . ?
O19 Nb8 O7 103.82(11) . . ?
O26 Nb8 O7 151.39(10) . . ?
O18 Nb8 O7 88.57(10) . . ?
O20 Nb8 O7 73.63(9) . . ?
O19 Nb8 O23 177.09(10) . . ?
O26 Nb8 O23 78.99(9) . . ?
O18 Nb8 O23 78.45(9) . . ?
O20 Nb8 O23 73.65(9) . . ?
O7 Nb8 O23 73.75(9) . . ?
O19 Nb8 Nb3 92.65(9) . . ?
O26 Nb8 Nb3 130.49(7) . . ?
O18 Nb8 Nb3 127.41(7) . . ?
O20 Nb8 Nb3 39.85(7) . . ?
O7 Nb8 Nb3 38.84(7) . . ?
O23 Nb8 Nb3 84.44(6) . . ?
O19 Nb8 Nb10 133.82(9) . . ?
O26 Nb8 Nb10 31.03(7) . . ?
O18 Nb8 Nb10 82.56(7) . . ?
O20 Nb8 Nb10 86.89(7) . . ?
O7 Nb8 Nb10 122.23(7) . . ?
O23 Nb8 Nb10 48.52(6) . . ?
Nb3 Nb8 Nb10 120.334(12) . . ?
O28 Nb10 O25 103.29(11) . . ?
O28 Nb10 O26 103.73(11) . . ?
O25 Nb10 O26 90.25(10) . . ?
O28 Nb10 O24 104.83(11) . . ?
O25 Nb10 O24 89.62(10) . . ?
O26 Nb10 O24 150.67(10) . . ?
O28 Nb10 O27 104.81(11) . . ?
O25 Nb10 O27 151.90(10) . . ?
O26 Nb10 O27 82.83(10) . . ?
O24 Nb10 O27 83.59(10) . . ?
O28 Nb10 O23 177.84(11) . . ?
O25 Nb10 O23 78.84(9) . . ?
O26 Nb10 O23 75.73(9) . . ?
O24 Nb10 O23 75.48(9) . . ?
O27 Nb10 O23 73.06(9) . . ?
O28 Nb10 Nb8 133.55(9) . . ?
O25 Nb10 Nb8 79.85(7) . . ?
O26 Nb10 Nb8 30.13(7) . . ?
O24 Nb10 Nb8 121.60(7) . . ?
O27 Nb10 Nb8 80.64(7) . . ?
O23 Nb10 Nb8 46.13(5) . . ?
O28 Nb10 Nb7 133.87(9) . . ?
O25 Nb10 Nb7 30.59(7) . . ?
O26 Nb10 Nb7 82.89(7) . . ?
O24 Nb10 Nb7 82.19(7) . . ?
O27 Nb10 Nb7 121.31(7) . . ?
O23 Nb10 Nb7 48.25(5) . . ?
Nb8 Nb10 Nb7 60.469(10) . . ?
Cr2 O2 Nb1 109.88(14) . . ?
Cr2 O2 H1 118(6) . . ?
Nb1 O2 H1 132(6) . . ?
Nb3 O3 Nb1 119.25(12) . . ?
Nb1 O4 Nb4 119.27(12) . . ?
Nb5 O5 Nb1 118.90(12) . . ?
Cr2 O6 Nb7 108.09(13) . . ?
Cr2 O6 H2 101(7) . . ?
Nb7 O6 H2 103(7) . . ?
Cr2 O7 Nb3 107.05(11) . . ?
Cr2 O7 Nb8 106.80(11) . . ?
Nb3 O7 Nb8 101.55(10) . . ?
Nb3 O9 Nb4 119.89(13) . . ?
Nb5 O11 Nb4 118.43(12) . . ?
Cr2 O13 Nb5 107.53(11) . . ?
Cr2 O13 Nb6 107.22(11) . . ?
Nb5 O13 Nb6 103.12(10) . . ?
Cr2 O14 Cr9 99.29(10) . . ?
Cr2 O14 Nb5 92.74(9) . . ?
Cr9 O14 Nb5 94.72(9) . . ?
Cr2 O14 Nb3 93.83(9) . . ?
Cr9 O14 Nb3 93.60(9) . . ?
Nb5 O14 Nb3 168.44(11) . . ?
Cr2 O14 Nb4 173.43(12) . . ?
Cr9 O14 Nb4 87.27(8) . . ?
Nb5 O14 Nb4 86.38(7) . . ?
Nb3 O14 Nb4 86.00(8) . . ?
Cr2 O14 Nb1 89.52(9) . . ?
Cr9 O14 Nb1 171.16(12) . . ?
Nb5 O14 Nb1 85.54(7) . . ?
Nb3 O14 Nb1 85.02(8) . . ?
Nb4 O14 Nb1 83.93(7) . . ?
Nb6 O16 Nb7 119.57(13) . . ?
Nb8 O18 Nb7 119.34(12) . . ?
Cr9 O20 Nb8 109.33(11) . . ?
Cr9 O20 Nb3 109.90(11) . . ?
Nb8 O20 Nb3 101.10(10) . . ?
Cr9 O21 Nb4 111.12(12) . . ?
Cr9 O22 Nb6 108.62(11) . . ?
Cr9 O22 Nb5 108.86(11) . . ?
Nb6 O22 Nb5 99.59(10) . . ?
Cr2 O23 Cr9 99.35(10) . . ?
Cr2 O23 Nb6 93.08(9) . . ?
Cr9 O23 Nb6 94.07(9) . . ?
Cr2 O23 Nb8 94.86(9) . . ?
Cr9 O23 Nb8 92.80(9) . . ?
Nb6 O23 Nb8 168.52(11) . . ?
Cr2 O23 Nb7 89.04(8) . . ?
Cr9 O23 Nb7 171.61(12) . . ?
Nb6 O23 Nb7 85.70(8) . . ?
Nb8 O23 Nb7 86.16(7) . . ?
Cr2 O23 Nb10 172.49(12) . . ?
Cr9 O23 Nb10 88.14(8) . . ?
Nb6 O23 Nb10 85.69(7) . . ?
Nb8 O23 Nb10 85.36(8) . . ?
Nb7 O23 Nb10 83.49(7) . . ?
Nb6 O24 Nb10 118.94(12) . . ?
Nb10 O25 Nb7 118.84(12) . . ?
Nb8 O26 Nb10 118.84(12) . . ?
Cr9 O27 Nb10 112.22(12) . . ?
H3 O29 H4 106(5) . . ?
H5 O30 H6 101(7) . . ?
H7 O31 H8 104(5) . . ?
H9 O32 H10 113(5) . . ?
H11 O33 H12 101(6) . . ?
H13 O34 H14 110(6) . . ?
H15 O35 H16 108(8) . . ?
H17 O36 H18 104(8) . . ?
H20 O39 H21 103(6) . . ?
O44 O40 O45 154.5(15) . . ?
O41 O45 O40 111.1(18) . . ?
C4 N1 C1 109.7(3) . . ?
C4 N1 C3 109.5(3) . . ?
C1 N1 C3 109.4(3) . . ?
C4 N1 C2 109.9(3) . . ?
C1 N1 C2 108.9(3) . . ?
C3 N1 C2 109.4(3) . . ?
C8 N2 C7 110.5(4) . . ?
C8 N2 C5 108.6(3) . . ?
C7 N2 C5 109.3(4) . . ?
C8 N2 C6 109.2(4) . . ?
C7 N2 C6 109.4(3) . . ?
C5 N2 C6 109.8(4) . . ?
C9 N3 C11 109.9(3) . . ?
C9 N3 C12 109.0(3) . . ?
C11 N3 C12 110.0(3) . . ?
C9 N3 C10 110.4(4) . . ?
C11 N3 C10 109.1(3) . . ?
C12 N3 C10 108.4(3) . . ?
C14 N4 C13 109.4(4) . . ?
C14 N4 C16 109.0(3) . . ?
C13 N4 C16 110.2(3) . . ?
C14 N4 C15 109.2(4) . . ?
C13 N4 C15 108.1(4) . . ?
C16 N4 C15 110.9(4) . . ?
C20 N5 C19 109.1(3) . . ?
C20 N5 C17 109.6(3) . . ?
C19 N5 C17 110.2(4) . . ?
C20 N5 C18 109.3(3) . . ?
C19 N5 C18 109.6(4) . . ?
C17 N5 C18 109.1(3) . . ?
C24 N6 C22 109.6(3) . . ?
C24 N6 C21 110.1(3) . . ?
C22 N6 C21 109.0(3) . . ?
C24 N6 C23 109.6(3) . . ?
C22 N6 C23 109.1(3) . . ?
C21 N6 C23 109.6(3) . . ?
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 . . ?
N4 C13 H13A 109.5 . . ?
N4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N4 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 C16 H16A 109.5 . . ?
N4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N5 C17 H17A 109.5 . . ?
N5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N5 C18 H18A 109.5 . . ?
N5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N5 C19 H19A 109.5 . . ?
N5 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N5 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N5 C20 H20A 109.5 . . ?
N5 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N5 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N6 C21 H21A 109.5 . . ?
N6 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N6 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N6 C22 H22A 109.5 . . ?
N6 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N6 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N6 C23 H23A 109.5 . . ?
N6 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N6 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N6 C24 H24A 109.5 . . ?
N6 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N6 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.402
_refine_diff_density_min         -1.567
_refine_diff_density_rms         0.099
_database_code_depnum_ccdc_archive 'CCDC 990475'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_TMA-CoNb9

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            'Tetramethylammonium nonaniobocobaltate'
_chemical_melting_point          ?
_chemical_formula_moiety         'Co Nb9 O28, 7(C4 H12 N), 25 (H2O)'
_chemical_formula_sum            'C28 H72 Co N7 Nb9 O53'
_chemical_formula_weight         2250.05

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'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   25.543(2)
_cell_length_b                   13.8124(12)
_cell_length_c                   23.383(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.0260(10)
_cell_angle_gamma                90.00
_cell_volume                     8003.9(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9070
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      30.51

_exptl_crystal_description       block
_exptl_crystal_colour            violet
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4436
_exptl_absorpt_coefficient_mu    1.540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5403
_exptl_absorpt_correction_T_max  0.8650
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            126087
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         30.54
_reflns_number_total             24416
_reflns_number_gt                17592
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0554P)²+83.1099P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         24416
_refine_ls_number_parameters     905
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1700
_refine_ls_wR_factor_gt          0.1559
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.155561(18) 0.75913(3) 0.16244(2) 0.0209(4) Uani 1 1 d . . .
Nb3 Nb 0.221026(18) 0.88368(3) 0.28090(2) 0.0185(4) Uani 1 1 d . . .
Nb4 Nb 0.291314(17) 0.76224(3) 0.19883(2) 0.0182(4) Uani 1 1 d . . .
Nb5 Nb 0.222847(18) 0.87507(3) 0.07566(2) 0.0195(4) Uani 1 1 d . . .
Nb6 Nb 0.222646(18) 1.11044(3) 0.072260(19) 0.0195(4) Uani 1 1 d . . .
Nb7 Nb 0.155830(18) 1.23398(3) 0.15508(2) 0.0221(4) Uani 1 1 d . . .
Nb8 Nb 0.221960(19) 1.11825(3) 0.27807(2) 0.0199(4) Uani 1 1 d . . .
Nb9 Nb 0.292065(16) 0.99698(3) 0.195564(17) 0.0138(4) Uani 1 1 d . . .
Nb10 Nb 0.291596(18) 1.23191(3) 0.19227(2) 0.0189(4) Uani 1 1 d . . .
Co2 Co 0.16046(3) 0.99664(5) 0.15977(3) 0.0171(4) Uani 1 1 d . . .
O1 O 0.10775(16) 0.6655(3) 0.1511(2) 0.0312(10) Uani 1 1 d . . .
O2 O 0.10692(15) 0.8831(3) 0.14558(17) 0.0234(8) Uani 1 1 d . . .
O3 O 0.16474(15) 0.7945(3) 0.24612(17) 0.0233(8) Uani 1 1 d . . .
O4 O 0.22377(14) 0.6888(3) 0.18173(17) 0.0224(8) Uani 1 1 d . . .
O5 O 0.16666(15) 0.7864(3) 0.08245(17) 0.0254(8) Uani 1 1 d . . .
O6 O 0.10772(15) 1.1101(3) 0.14374(18) 0.0249(8) Uani 1 1 d . . .
O7 O 0.17331(14) 1.0011(3) 0.25327(16) 0.0201(7) Uani 1 1 d . . .
O8 O 0.22199(17) 0.8799(3) 0.35680(17) 0.0285(9) Uani 1 1 d . . .
O9 O 0.27986(14) 0.7952(3) 0.27764(16) 0.0207(8) Uani 1 1 d . . .
O10 O 0.34042(15) 0.6702(3) 0.21351(19) 0.0274(9) Uani 1 1 d . . .
O11 O 0.28150(14) 0.7882(3) 0.11338(17) 0.0227(8) Uani 1 1 d . . .
O12 O 0.22499(17) 0.8644(3) 0.00075(17) 0.0293(9) Uani 1 1 d . . .
O13 O 0.17430(14) 0.9930(3) 0.07339(16) 0.0203(7) Uani 1 1 d . . .
O14 O 0.22545(13) 0.8919(2) 0.17902(14) 0.0169(7) Uani 1 1 d . . .
O15 O 0.22463(17) 1.1147(3) -0.00342(17) 0.0299(9) Uani 1 1 d . . .
O16 O 0.16700(15) 1.2010(3) 0.07632(17) 0.0241(8) Uani 1 1 d . . .
O17 O 0.10793(16) 1.3270(3) 0.1407(2) 0.0317(10) Uani 1 1 d . . .
O18 O 0.16591(16) 1.2075(3) 0.24066(18) 0.0264(9) Uani 1 1 d . . .
O19 O 0.22317(18) 1.1290(3) 0.35343(18) 0.0294(9) Uani 1 1 d . . .
O20 O 0.27491(14) 1.0000(2) 0.27542(15) 0.0179(7) Uani 1 1 d . . .
O21 O 0.33691(14) 0.8902(2) 0.20931(15) 0.0180(7) Uani 1 1 d . . .
O22 O 0.27599(13) 0.9935(2) 0.10698(15) 0.0180(7) Uani 1 1 d . . .
O23 O 0.22603(14) 1.1022(2) 0.17608(15) 0.0178(7) Uani 1 1 d . . .
O24 O 0.28152(15) 1.1985(3) 0.10772(16) 0.0226(8) Uani 1 1 d . . .
O25 O 0.22427(15) 1.3046(3) 0.17279(18) 0.0256(9) Uani 1 1 d . . .
O26 O 0.28067(15) 1.2051(3) 0.27222(16) 0.0228(8) Uani 1 1 d . . .
O27 O 0.33710(14) 1.1035(2) 0.20632(15) 0.0179(7) Uani 1 1 d . . .
O28 O 0.34065(16) 1.3236(3) 0.20449(19) 0.0281(9) Uani 1 1 d . . .
O29 O 0.0760(4) 0.9266(8) 1.0084(5) 0.129(4) Uani 1 1 d . . .
O30 O 0.0462(2) 0.4941(4) 0.1206(4) 0.086(3) Uani 1 1 d . . .
O31 O 0.0276(4) 0.9861(7) 0.1834(5) 0.118(4) Uani 1 1 d . . .
O32 O 0.1436(3) 0.9981(4) 0.3907(3) 0.0601(16) Uani 1 1 d . . .
O33 O 0.0581(4) 0.9435(9) 0.4408(5) 0.122(4) Uani 1 1 d . . .
O34 O 0.2754(2) 0.7537(4) 0.44034(19) 0.0387(11) Uani 1 1 d . . .
O35 O 0.3414(2) 0.6914(4) 0.3705(2) 0.0486(13) Uani 1 1 d . . .
O36 O 0.4455(3) 0.6594(8) 0.3961(4) 0.115(4) Uani 1 1 d . . .
O37 O 0.5013(2) 0.7515(4) 0.4987(3) 0.0581(15) Uani 1 1 d . . .
O38 O 0.3433(2) 0.8032(4) 0.5490(2) 0.0511(14) Uani 1 1 d . . .
O39 O 0.4463(4) 0.8390(9) 0.5749(5) 0.133(4) Uani 1 1 d . . .
O40 O 0.4620(3) 0.4988(5) 0.3371(4) 0.078(2) Uani 1 1 d . . .
O41 O 0.39429(16) 0.4974(3) 0.2227(2) 0.0350(11) Uani 1 1 d . . .
O42 O 0.4622(3) 0.5003(5) 0.1444(4) 0.083(2) Uani 1 1 d . . .
O43 O 0.4413(4) 0.3499(9) 0.0666(6) 0.162(6) Uani 1 1 d . . .
O44 O 0.0242(8) 0.0230(14) 0.0610(8) 0.251(10) Uani 1 1 d . . .
O45 O 0.0803(3) 0.2614(7) 0.2810(4) 0.091(3) Uani 1 1 d . . .
O46 O 0.3424(2) 0.2973(5) 0.3697(2) 0.0578(17) Uani 1 1 d . . .
O47 O 0.5575(4) 0.6555(10) 0.5972(4) 0.166(6) Uani 1 1 d . . .
O48 O 0.0773(5) 0.0640(10) 0.2817(7) 0.172(6) Uani 1 1 d . . .
O49 O 0.2722(2) 0.2518(3) 0.43972(19) 0.0355(10) Uani 1 1 d . . .
O50 O 0.3425(2) 0.2031(6) 0.5455(2) 0.073(2) Uani 1 1 d . . .
O51 O 0.0762(5) 0.0619(10) 0.8286(5) 0.139(4) Uani 1 1 d . . .
O52 O 0.0762(3) 0.7281(7) 1.0003(4) 0.097(3) Uani 1 1 d . . .
O53 O 0.1484(3) 0.9960(4) 0.9246(3) 0.0636(18) Uani 1 1 d . . .
N1 N 0.3952(2) 0.9947(5) 0.4018(3) 0.0452(15) Uani 1 1 d . . .
N2 N 0.2214(2) 0.4950(3) 0.2943(2) 0.0294(10) Uani 1 1 d . . .
N3 N 0.0573(3) 0.7439(6) 0.3224(4) 0.0592(19) Uani 1 1 d . . .
N4 N 0.2219(2) 0.5009(3) 0.0570(2) 0.0311(11) Uani 1 1 d . . .
N5 N 0.3954(2) 0.5071(5) 0.5425(3) 0.0456(15) Uani 1 1 d . . .
N6 N 0.0592(3) 0.2586(6) 0.9484(4) 0.066(2) Uani 1 1 d . . .
C1 C 0.4468(6) 0.9989(12) 0.4462(7) 0.143(8) Uani 1 1 d . . .
H1A H 0.4765 0.9920 0.4268 0.215 Uiso 1 1 calc R . .
H1B H 0.4483 0.9462 0.4746 0.215 Uiso 1 1 calc R . .
H1C H 0.4498 1.0612 0.4668 0.215 Uiso 1 1 calc R . .
C2 C 0.3959(5) 1.0777(11) 0.3595(7) 0.113(5) Uani 1 1 d . . .
H2A H 0.3953 1.1394 0.3800 0.170 Uiso 1 1 calc R . .
H2B H 0.3641 1.0733 0.3263 0.170 Uiso 1 1 calc R . .
H2C H 0.4286 1.0738 0.3448 0.170 Uiso 1 1 calc R . .
C3 C 0.3433(5) 1.0021(11) 0.4223(5) 0.098(5) Uani 1 1 d . . .
H3A H 0.3465 0.9634 0.4581 0.147 Uiso 1 1 calc R . .
H3B H 0.3132 0.9778 0.3913 0.147 Uiso 1 1 calc R . .
H3C H 0.3367 1.0699 0.4307 0.147 Uiso 1 1 calc R . .
C4 C 0.3942(5) 0.9125(10) 0.3610(7) 0.131(7) Uani 1 1 d . . .
H4A H 0.4188 0.9257 0.3356 0.196 Uiso 1 1 calc R . .
H4B H 0.3575 0.9041 0.3365 0.196 Uiso 1 1 calc R . .
H4C H 0.4056 0.8533 0.3837 0.196 Uiso 1 1 calc R . .
C5 C 0.2721(3) 0.4958(5) 0.2738(3) 0.0397(15) Uani 1 1 d . . .
H5A H 0.2720 0.5517 0.2479 0.059 Uiso 1 1 calc R . .
H5B H 0.2746 0.4360 0.2520 0.059 Uiso 1 1 calc R . .
H5C H 0.3030 0.5002 0.3079 0.059 Uiso 1 1 calc R . .
C6 C 0.2178(3) 0.5848(4) 0.3278(3) 0.0391(15) Uani 1 1 d . . .
H6A H 0.1839 0.5849 0.3404 0.059 Uiso 1 1 calc R . .
H6B H 0.2188 0.6412 0.3027 0.059 Uiso 1 1 calc R . .
H6C H 0.2483 0.5877 0.3625 0.059 Uiso 1 1 calc R . .
C7 C 0.1738(3) 0.4907(5) 0.2414(3) 0.0482(18) Uani 1 1 d . . .
H7A H 0.1403 0.4887 0.2546 0.072 Uiso 1 1 calc R . .
H7B H 0.1765 0.4324 0.2183 0.072 Uiso 1 1 calc R . .
H7C H 0.1738 0.5482 0.2168 0.072 Uiso 1 1 calc R . .
C8 C 0.2204(3) 0.4085(4) 0.3312(3) 0.0365(14) Uani 1 1 d . . .
H8A H 0.2506 0.4112 0.3661 0.055 Uiso 1 1 calc R . .
H8B H 0.2235 0.3501 0.3084 0.055 Uiso 1 1 calc R . .
H8C H 0.1863 0.4067 0.3434 0.055 Uiso 1 1 calc R . .
C9 C 0.0139(3) 0.7249(9) 0.3567(5) 0.075(3) Uani 1 1 d . . .
H9A H 0.0194 0.7691 0.3905 0.113 Uiso 1 1 calc R . .
H9B H 0.0166 0.6579 0.3708 0.113 Uiso 1 1 calc R . .
H9C H -0.0220 0.7358 0.3308 0.113 Uiso 1 1 calc R . .
C10 C 0.0494(4) 0.8417(8) 0.2930(5) 0.074(3) Uani 1 1 d . . .
H10A H 0.0795 0.8550 0.2748 0.111 Uiso 1 1 calc R . .
H10B H 0.0483 0.8916 0.3225 0.111 Uiso 1 1 calc R . .
H10C H 0.0154 0.8422 0.2626 0.111 Uiso 1 1 calc R . .
C11 C 0.1113(3) 0.7419(7) 0.3670(5) 0.064(2) Uani 1 1 d . . .
H11A H 0.1387 0.7720 0.3499 0.095 Uiso 1 1 calc R . .
H11B H 0.1215 0.6747 0.3776 0.095 Uiso 1 1 calc R . .
H11C H 0.1086 0.7777 0.4023 0.095 Uiso 1 1 calc R . .
C12 C 0.0570(6) 0.6700(11) 0.2747(5) 0.102(5) Uani 1 1 d . . .
H12A H 0.0212 0.6686 0.2474 0.153 Uiso 1 1 calc R . .
H12B H 0.0653 0.6059 0.2926 0.153 Uiso 1 1 calc R . .
H12C H 0.0841 0.6875 0.2532 0.153 Uiso 1 1 calc R . .
C13 C 0.1718(4) 0.5015(6) 0.0810(4) 0.053(2) Uani 1 1 d . . .
H13A H 0.1709 0.5612 0.1033 0.080 Uiso 1 1 calc R . .
H13B H 0.1725 0.4455 0.1069 0.080 Uiso 1 1 calc R . .
H13C H 0.1396 0.4981 0.0482 0.080 Uiso 1 1 calc R . .
C14 C 0.2213(3) 0.5891(5) 0.0210(3) 0.0434(17) Uani 1 1 d . . .
H14A H 0.2523 0.5881 0.0032 0.065 Uiso 1 1 calc R . .
H14B H 0.2234 0.6465 0.0461 0.065 Uiso 1 1 calc R . .
H14C H 0.1879 0.5912 -0.0102 0.065 Uiso 1 1 calc R . .
C15 C 0.2704(3) 0.5008(5) 0.1079(3) 0.0447(17) Uani 1 1 d . . .
H15A H 0.3031 0.4963 0.0931 0.067 Uiso 1 1 calc R . .
H15B H 0.2686 0.4452 0.1334 0.067 Uiso 1 1 calc R . .
H15C H 0.2712 0.5608 0.1304 0.067 Uiso 1 1 calc R . .
C16 C 0.2218(3) 0.4110(5) 0.0221(3) 0.0432(17) Uani 1 1 d . . .
H16A H 0.1917 0.4130 -0.0131 0.065 Uiso 1 1 calc R . .
H16B H 0.2177 0.3547 0.0461 0.065 Uiso 1 1 calc R . .
H16C H 0.2559 0.4060 0.0101 0.065 Uiso 1 1 calc R . .
C17 C 0.4432(6) 0.4992(17) 0.5218(7) 0.181(12) Uani 1 1 d . . .
H17A H 0.4477 0.5579 0.4999 0.272 Uiso 1 1 calc R . .
H17B H 0.4405 0.4428 0.4958 0.272 Uiso 1 1 calc R . .
H17C H 0.4744 0.4915 0.5554 0.272 Uiso 1 1 calc R . .
C18 C 0.3969(6) 0.5818(12) 0.5871(10) 0.158(9) Uani 1 1 d . . .
H18A H 0.4272 0.5694 0.6211 0.237 Uiso 1 1 calc R . .
H18B H 0.3631 0.5808 0.5998 0.237 Uiso 1 1 calc R . .
H18C H 0.4015 0.6454 0.5704 0.237 Uiso 1 1 calc R . .
C19 C 0.3441(5) 0.5122(11) 0.4958(5) 0.096(5) Uani 1 1 d . . .
H19A H 0.3423 0.5741 0.4749 0.144 Uiso 1 1 calc R . .
H19B H 0.3134 0.5068 0.5139 0.144 Uiso 1 1 calc R . .
H19C H 0.3430 0.4589 0.4678 0.144 Uiso 1 1 calc R . .
C20 C 0.3941(5) 0.4220(12) 0.5807(8) 0.125(6) Uani 1 1 d . . .
H20A H 0.3924 0.3626 0.5575 0.188 Uiso 1 1 calc R . .
H20B H 0.3622 0.4259 0.5970 0.188 Uiso 1 1 calc R . .
H20C H 0.4267 0.4213 0.6130 0.188 Uiso 1 1 calc R . .
C21 C 0.0584(5) 0.3324(10) 0.9952(5) 0.093(4) Uani 1 1 d . . .
H21A H 0.0880 0.3195 1.0297 0.139 Uiso 1 1 calc R . .
H21B H 0.0239 0.3287 1.0065 0.139 Uiso 1 1 calc R . .
H21C H 0.0627 0.3973 0.9800 0.139 Uiso 1 1 calc R . .
C22 C 0.1136(3) 0.2594(8) 0.9317(5) 0.075(3) Uani 1 1 d . . .
H22A H 0.1230 0.3260 0.9238 0.113 Uiso 1 1 calc R . .
H22B H 0.1112 0.2198 0.8964 0.113 Uiso 1 1 calc R . .
H22C H 0.1415 0.2328 0.9644 0.113 Uiso 1 1 calc R . .
C23 C 0.0518(5) 0.1582(9) 0.9753(6) 0.094(4) Uani 1 1 d . . .
H23A H 0.0808 0.1479 1.0108 0.141 Uiso 1 1 calc R . .
H23B H 0.0532 0.1074 0.9465 0.141 Uiso 1 1 calc R . .
H23C H 0.0169 0.1561 0.9856 0.141 Uiso 1 1 calc R . .
C24 C 0.0163(4) 0.2769(10) 0.8904(5) 0.097(4) Uani 1 1 d . . .
H24A H -0.0198 0.2723 0.8978 0.146 Uiso 1 1 calc R . .
H24B H 0.0200 0.2283 0.8611 0.146 Uiso 1 1 calc R . .
H24C H 0.0214 0.3417 0.8755 0.146 Uiso 1 1 calc R . .
C25 C 0.4649(6) 0.2913(12) 0.2925(7) 0.052(4) Uiso 0.542(10) 1 d P A 1
C26 C 0.4660(6) 0.2939(12) 0.1879(7) 0.052(4) Uiso 0.542(10) 1 d P A 1
C27 C 0.5484(6) 0.2388(11) 0.2625(6) 0.046(3) Uiso 0.542(10) 1 d P A 1
C28 C 0.4663(8) 0.1367(14) 0.2388(9) 0.067(5) Uiso 0.542(10) 1 d P A 1
N7 N 0.4870(5) 0.2395(9) 0.2456(5) 0.042(3) Uiso 0.542(10) 1 d P A 1
C27A C 0.5349(7) 0.2060(14) 0.3108(8) 0.051(4) Uiso 0.458(10) 1 d P A 2
C26A C 0.5341(8) 0.2083(14) 0.2065(9) 0.055(5) Uiso 0.458(10) 1 d P A 2
C25A C 0.4522(8) 0.2633(14) 0.2386(8) 0.052(4) Uiso 0.458(10) 1 d P A 2
C28A C 0.5346(10) 0.3616(19) 0.2596(11) 0.076(7) Uiso 0.458(10) 1 d P A 2
N7A N 0.5145(7) 0.2636(11) 0.2534(6) 0.047(3) Uiso 0.458(10) 1 d P A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Nb1 O1 1.754(4) . ?
Nb1 O4 1.950(4) . ?
Nb1 O3 1.975(4) . ?
Nb1 O5 1.994(4) . ?
Nb1 O2 2.096(4) . ?
Nb1 O14 2.523(3) . ?
Nb1 Nb3 3.3441(7) . ?
Nb3 O8 1.770(4) . ?
Nb3 O3 1.918(4) . ?
Nb3 O9 1.952(4) . ?
Nb3 O7 2.037(3) . ?
Nb3 O20 2.139(3) . ?
Nb3 O14 2.415(3) . ?
Nb3 Nb8 3.2409(7) . ?
Nb4 O10 1.760(4) . ?
Nb4 O4 1.957(3) . ?
Nb4 O11 1.985(4) . ?
Nb4 O9 1.988(4) . ?
Nb4 O21 2.099(3) . ?
Nb4 O14 2.424(3) . ?
Nb4 Nb9 3.2434(7) . ?
Nb5 O12 1.772(4) . ?
Nb5 O5 1.922(4) . ?
Nb5 O11 1.955(4) . ?
Nb5 O13 2.040(4) . ?
Nb5 O22 2.138(3) . ?
Nb5 O14 2.413(3) . ?
Nb5 Nb6 3.2519(7) . ?
Nb6 O15 1.784(4) . ?
Nb6 O16 1.913(4) . ?
Nb6 O24 1.956(4) . ?
Nb6 O13 2.043(4) . ?
Nb6 O22 2.143(3) . ?
Nb6 O23 2.411(3) . ?
Nb6 Nb7 3.3431(7) . ?
Nb7 O17 1.750(4) . ?
Nb7 O25 1.957(4) . ?
Nb7 O16 1.984(4) . ?
Nb7 O18 1.989(4) . ?
Nb7 O6 2.085(4) . ?
Nb7 O23 2.519(3) . ?
Nb8 O19 1.761(4) . ?
Nb8 O18 1.930(4) . ?
Nb8 O26 1.951(4) . ?
Nb8 O7 2.037(4) . ?
Nb8 O20 2.131(3) . ?
Nb8 O23 2.422(3) . ?
Nb9 O27 1.846(3) . ?
Nb9 O21 1.847(3) . ?
Nb9 O22 2.012(3) . ?
Nb9 O20 2.019(3) . ?
Nb9 O23 2.189(3) . ?
Nb9 O14 2.198(3) . ?
Nb9 Nb10 3.2458(7) . ?
Nb10 O28 1.755(4) . ?
Nb10 O25 1.948(4) . ?
Nb10 O24 1.985(4) . ?
Nb10 O26 1.991(4) . ?
Nb10 O27 2.103(3) . ?
Nb10 O23 2.419(3) . ?
Co2 O6 2.042(4) . ?
Co2 O2 2.054(4) . ?
Co2 O7 2.131(4) . ?
Co2 O13 2.134(4) . ?
Co2 O14 2.165(3) . ?
Co2 O23 2.183(3) . ?
N1 C1 1.466(12) . ?
N1 C4 1.481(13) . ?
N1 C2 1.517(14) . ?
N1 C3 1.519(13) . ?
N2 C8 1.478(7) . ?
N2 C6 1.483(7) . ?
N2 C5 1.485(8) . ?
N2 C7 1.511(9) . ?
N3 C10 1.507(12) . ?
N3 C12 1.509(13) . ?
N3 C11 1.515(11) . ?
N3 C9 1.541(11) . ?
N4 C14 1.480(8) . ?
N4 C16 1.487(8) . ?
N4 C15 1.494(8) . ?
N4 C13 1.515(9) . ?
N5 C17 1.423(13) . ?
N5 C18 1.462(15) . ?
N5 C20 1.482(15) . ?
N5 C19 1.490(12) . ?
N6 C21 1.500(13) . ?
N6 C22 1.533(12) . ?
N6 C24 1.544(12) . ?
N6 C23 1.553(14) . ?
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 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 N7 1.527(19) . ?
C26 N7 1.523(19) . ?
C27 N7 1.522(19) . ?
C28 N7 1.51(2) . ?
C27A N7A 1.54(2) . ?
C26A N7A 1.52(2) . ?
C25A N7A 1.55(2) . ?
C28A N7A 1.44(3) . ?

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
O1 Nb1 O4 102.59(17) . . ?
O1 Nb1 O3 104.11(19) . . ?
O4 Nb1 O3 90.53(16) . . ?
O1 Nb1 O5 104.42(19) . . ?
O4 Nb1 O5 89.36(16) . . ?
O3 Nb1 O5 150.78(15) . . ?
O1 Nb1 O2 102.40(17) . . ?
O4 Nb1 O2 154.97(14) . . ?
O3 Nb1 O2 84.66(15) . . ?
O5 Nb1 O2 83.21(16) . . ?
O1 Nb1 O14 179.13(15) . . ?
O4 Nb1 O14 76.54(13) . . ?
O3 Nb1 O14 76.01(13) . . ?
O5 Nb1 O14 75.56(13) . . ?
O2 Nb1 O14 78.47(13) . . ?
O1 Nb1 Nb3 134.01(15) . . ?
O4 Nb1 Nb3 79.93(11) . . ?
O3 Nb1 Nb3 30.30(11) . . ?
O5 Nb1 Nb3 121.56(11) . . ?
O2 Nb1 Nb3 83.69(11) . . ?
O14 Nb1 Nb3 46.02(8) . . ?
O8 Nb3 O3 103.48(18) . . ?
O8 Nb3 O9 101.36(17) . . ?
O3 Nb3 O9 94.97(15) . . ?
O8 Nb3 O7 101.74(17) . . ?
O3 Nb3 O7 92.71(15) . . ?
O9 Nb3 O7 153.19(14) . . ?
O8 Nb3 O20 103.26(16) . . ?
O3 Nb3 O20 152.11(14) . . ?
O9 Nb3 O20 87.42(14) . . ?
O7 Nb3 O20 74.19(13) . . ?
O8 Nb3 O14 176.48(16) . . ?
O3 Nb3 O14 79.72(14) . . ?
O9 Nb3 O14 76.73(13) . . ?
O7 Nb3 O14 79.45(13) . . ?
O20 Nb3 O14 73.79(12) . . ?
O8 Nb3 Nb8 92.96(14) . . ?
O3 Nb3 Nb8 129.93(11) . . ?
O9 Nb3 Nb8 127.96(10) . . ?
O7 Nb3 Nb8 37.31(10) . . ?
O20 Nb3 Nb8 40.54(9) . . ?
O14 Nb3 Nb8 86.01(8) . . ?
O8 Nb3 Nb1 134.28(14) . . ?
O3 Nb3 Nb1 31.29(11) . . ?
O9 Nb3 Nb1 83.16(11) . . ?
O7 Nb3 Nb1 90.35(10) . . ?
O20 Nb3 Nb1 122.44(9) . . ?
O14 Nb3 Nb1 48.75(8) . . ?
Nb8 Nb3 Nb1 120.136(18) . . ?
O10 Nb4 O4 102.53(16) . . ?
O10 Nb4 O11 103.71(18) . . ?
O4 Nb4 O11 89.89(16) . . ?
O10 Nb4 O9 104.07(18) . . ?
O4 Nb4 O9 89.30(15) . . ?
O11 Nb4 O9 151.71(15) . . ?
O10 Nb4 O21 103.67(15) . . ?
O4 Nb4 O21 153.80(14) . . ?
O11 Nb4 O21 84.04(14) . . ?
O9 Nb4 O21 84.30(14) . . ?
O10 Nb4 O14 178.58(15) . . ?
O4 Nb4 O14 78.89(13) . . ?
O11 Nb4 O14 76.20(13) . . ?
O9 Nb4 O14 75.90(13) . . ?
O21 Nb4 O14 74.91(12) . . ?
O10 Nb4 Nb9 135.92(13) . . ?
O4 Nb4 Nb9 121.54(10) . . ?
O11 Nb4 Nb9 78.20(11) . . ?
O9 Nb4 Nb9 78.20(10) . . ?
O21 Nb4 Nb9 32.25(9) . . ?
O14 Nb4 Nb9 42.66(8) . . ?
O12 Nb5 O5 103.37(18) . . ?
O12 Nb5 O11 101.01(18) . . ?
O5 Nb5 O11 94.47(16) . . ?
O12 Nb5 O13 101.83(18) . . ?
O5 Nb5 O13 92.82(15) . . ?
O11 Nb5 O13 153.68(14) . . ?
O12 Nb5 O22 103.48(17) . . ?
O5 Nb5 O22 152.10(15) . . ?
O11 Nb5 O22 87.77(14) . . ?
O13 Nb5 O22 74.33(13) . . ?
O12 Nb5 O14 176.66(16) . . ?
O5 Nb5 O14 79.55(14) . . ?
O11 Nb5 O14 77.01(13) . . ?
O13 Nb5 O14 79.52(13) . . ?
O22 Nb5 O14 73.86(12) . . ?
O12 Nb5 Nb6 93.40(14) . . ?
O5 Nb5 Nb6 129.95(12) . . ?
O11 Nb5 Nb6 128.39(11) . . ?
O13 Nb5 Nb6 37.24(10) . . ?
O22 Nb5 Nb6 40.62(9) . . ?
O14 Nb5 Nb6 85.85(8) . . ?
O15 Nb6 O16 103.16(18) . . ?
O15 Nb6 O24 101.32(18) . . ?
O16 Nb6 O24 94.39(16) . . ?
O15 Nb6 O13 101.64(17) . . ?
O16 Nb6 O13 93.43(15) . . ?
O24 Nb6 O13 153.34(14) . . ?
O15 Nb6 O22 103.45(17) . . ?
O16 Nb6 O22 152.41(15) . . ?
O24 Nb6 O22 87.45(14) . . ?
O13 Nb6 O22 74.16(13) . . ?
O15 Nb6 O23 176.33(16) . . ?
O16 Nb6 O23 80.02(14) . . ?
O24 Nb6 O23 76.49(13) . . ?
O13 Nb6 O23 79.84(13) . . ?
O22 Nb6 O23 73.64(12) . . ?
O15 Nb6 Nb5 93.27(14) . . ?
O16 Nb6 Nb5 130.48(11) . . ?
O24 Nb6 Nb5 127.96(11) . . ?
O13 Nb6 Nb5 37.17(10) . . ?
O22 Nb6 Nb5 40.51(9) . . ?
O23 Nb6 Nb5 85.90(8) . . ?
O15 Nb6 Nb7 134.35(14) . . ?
O16 Nb6 Nb7 31.54(11) . . ?
O24 Nb6 Nb7 83.39(11) . . ?
O13 Nb6 Nb7 90.16(10) . . ?
O22 Nb6 Nb7 122.17(9) . . ?
O23 Nb6 Nb7 48.68(8) . . ?
Nb5 Nb6 Nb7 119.610(18) . . ?
O17 Nb7 O25 102.80(17) . . ?
O17 Nb7 O16 103.99(19) . . ?
O25 Nb7 O16 89.36(16) . . ?
O17 Nb7 O18 104.03(19) . . ?
O25 Nb7 O18 89.29(16) . . ?
O16 Nb7 O18 151.53(15) . . ?
O17 Nb7 O6 102.41(17) . . ?
O25 Nb7 O6 154.78(15) . . ?
O16 Nb7 O6 84.63(16) . . ?
O18 Nb7 O6 84.58(16) . . ?
O17 Nb7 O23 179.03(16) . . ?
O25 Nb7 O23 76.22(13) . . ?
O16 Nb7 O23 76.06(13) . . ?
O18 Nb7 O23 76.01(13) . . ?
O6 Nb7 O23 78.56(13) . . ?
O17 Nb7 Nb6 134.03(16) . . ?
O25 Nb7 Nb6 79.73(12) . . ?
O16 Nb7 Nb6 30.29(10) . . ?
O18 Nb7 Nb6 121.94(11) . . ?
O6 Nb7 Nb6 82.85(11) . . ?
O23 Nb7 Nb6 45.95(8) . . ?
O19 Nb8 O18 103.35(18) . . ?
O19 Nb8 O26 101.01(18) . . ?
O18 Nb8 O26 94.24(16) . . ?
O19 Nb8 O7 102.32(17) . . ?
O18 Nb8 O7 92.52(15) . . ?
O26 Nb8 O7 153.46(15) . . ?
O19 Nb8 O20 103.67(17) . . ?
O18 Nb8 O20 151.92(15) . . ?
O26 Nb8 O20 88.00(14) . . ?
O7 Nb8 O20 74.36(13) . . ?
O19 Nb8 O23 176.61(17) . . ?
O18 Nb8 O23 79.42(14) . . ?
O26 Nb8 O23 76.71(13) . . ?
O7 Nb8 O23 79.38(13) . . ?
O20 Nb8 O23 73.87(12) . . ?
O19 Nb8 Nb3 93.57(14) . . ?
O18 Nb8 Nb3 129.73(12) . . ?
O26 Nb8 Nb3 128.73(11) . . ?
O7 Nb8 Nb3 37.30(10) . . ?
O20 Nb8 Nb3 40.73(9) . . ?
O23 Nb8 Nb3 86.03(8) . . ?
O27 Nb9 O21 105.82(15) . . ?
O27 Nb9 O22 97.15(14) . . ?
O21 Nb9 O22 97.07(14) . . ?
O27 Nb9 O20 97.20(14) . . ?
O21 Nb9 O20 96.88(14) . . ?
O22 Nb9 O20 156.43(14) . . ?
O27 Nb9 O23 85.57(14) . . ?
O21 Nb9 O23 168.61(14) . . ?
O22 Nb9 O23 81.21(13) . . ?
O20 Nb9 O23 81.37(13) . . ?
O27 Nb9 O14 168.50(14) . . ?
O21 Nb9 O14 85.68(14) . . ?
O22 Nb9 O14 81.19(13) . . ?
O20 Nb9 O14 81.03(13) . . ?
O23 Nb9 O14 82.93(12) . . ?
O27 Nb9 Nb4 143.14(11) . . ?
O21 Nb9 Nb4 37.33(11) . . ?
O22 Nb9 Nb4 89.95(10) . . ?
O20 Nb9 Nb4 89.71(10) . . ?
O23 Nb9 Nb4 131.28(9) . . ?
O14 Nb9 Nb4 48.35(9) . . ?
O27 Nb9 Nb10 37.39(11) . . ?
O21 Nb9 Nb10 143.21(11) . . ?
O22 Nb9 Nb10 90.06(10) . . ?
O20 Nb9 Nb10 90.06(10) . . ?
O23 Nb9 Nb10 48.18(9) . . ?
O14 Nb9 Nb10 131.11(9) . . ?
Nb4 Nb9 Nb10 179.452(17) . . ?
O28 Nb10 O25 102.78(17) . . ?
O28 Nb10 O24 104.17(18) . . ?
O25 Nb10 O24 89.59(16) . . ?
O28 Nb10 O26 103.79(18) . . ?
O25 Nb10 O26 89.93(16) . . ?
O24 Nb10 O26 151.43(15) . . ?
O28 Nb10 O27 103.73(16) . . ?
O25 Nb10 O27 153.49(14) . . ?
O24 Nb10 O27 83.86(14) . . ?
O26 Nb10 O27 83.93(14) . . ?
O28 Nb10 O23 178.36(16) . . ?
O25 Nb10 O23 78.87(13) . . ?
O24 Nb10 O23 75.78(13) . . ?
O26 Nb10 O23 76.10(13) . . ?
O27 Nb10 O23 74.62(12) . . ?
O28 Nb10 Nb9 135.96(13) . . ?
O25 Nb10 Nb9 121.27(11) . . ?
O24 Nb10 Nb9 77.90(11) . . ?
O26 Nb10 Nb9 78.01(10) . . ?
O27 Nb10 Nb9 32.22(9) . . ?
O23 Nb10 Nb9 42.40(8) . . ?
O6 Co2 O2 99.95(15) . . ?
O6 Co2 O7 95.57(15) . . ?
O2 Co2 O7 96.81(15) . . ?
O6 Co2 O13 95.61(15) . . ?
O2 Co2 O13 94.90(15) . . ?
O7 Co2 O13 162.16(13) . . ?
O6 Co2 O14 171.75(14) . . ?
O2 Co2 O14 88.31(14) . . ?
O7 Co2 O14 83.46(13) . . ?
O13 Co2 O14 83.48(13) . . ?
O6 Co2 O23 87.91(14) . . ?
O2 Co2 O23 172.10(14) . . ?
O7 Co2 O23 83.15(13) . . ?
O13 Co2 O23 83.40(13) . . ?
O14 Co2 O23 83.83(13) . . ?
Co2 O2 Nb1 104.61(16) . . ?
Nb3 O3 Nb1 118.41(18) . . ?
Nb1 O4 Nb4 118.90(18) . . ?
Nb5 O5 Nb1 118.45(18) . . ?
Co2 O6 Nb7 105.32(17) . . ?
Nb3 O7 Nb8 105.38(16) . . ?
Nb3 O7 Co2 103.54(15) . . ?
Nb8 O7 Co2 104.27(15) . . ?
Nb3 O9 Nb4 117.87(18) . . ?
Nb5 O11 Nb4 117.46(17) . . ?
Nb5 O13 Nb6 105.59(16) . . ?
Nb5 O13 Co2 103.50(15) . . ?
Nb6 O13 Co2 103.45(15) . . ?
Co2 O14 Nb9 96.74(13) . . ?
Co2 O14 Nb5 91.29(12) . . ?
Nb9 O14 Nb5 94.14(12) . . ?
Co2 O14 Nb3 91.14(12) . . ?
Nb9 O14 Nb3 94.41(12) . . ?
Nb5 O14 Nb3 170.78(16) . . ?
Co2 O14 Nb4 174.27(16) . . ?
Nb9 O14 Nb4 88.99(11) . . ?
Nb5 O14 Nb4 88.25(11) . . ?
Nb3 O14 Nb4 88.45(11) . . ?
Co2 O14 Nb1 88.59(11) . . ?
Nb9 O14 Nb1 174.66(16) . . ?
Nb5 O14 Nb1 85.94(10) . . ?
Nb3 O14 Nb1 85.23(10) . . ?
Nb4 O14 Nb1 85.68(10) . . ?
Nb6 O16 Nb7 118.17(18) . . ?
Nb8 O18 Nb7 118.33(19) . . ?
Nb9 O20 Nb8 108.91(15) . . ?
Nb9 O20 Nb3 109.08(15) . . ?
Nb8 O20 Nb3 98.73(14) . . ?
Nb9 O21 Nb4 110.42(16) . . ?
Nb9 O22 Nb5 108.99(15) . . ?
Nb9 O22 Nb6 108.91(15) . . ?
Nb5 O22 Nb6 98.87(14) . . ?
Co2 O23 Nb9 96.49(13) . . ?
Co2 O23 Nb6 90.97(12) . . ?
Nb9 O23 Nb6 94.52(12) . . ?
Co2 O23 Nb10 174.09(17) . . ?
Nb9 O23 Nb10 89.42(12) . . ?
Nb6 O23 Nb10 88.68(11) . . ?
Co2 O23 Nb8 91.09(12) . . ?
Nb9 O23 Nb8 94.06(12) . . ?
Nb6 O23 Nb8 170.89(16) . . ?
Nb10 O23 Nb8 88.36(11) . . ?
Co2 O23 Nb7 88.21(12) . . ?
Nb9 O23 Nb7 175.30(16) . . ?
Nb6 O23 Nb7 85.37(11) . . ?
Nb10 O23 Nb7 85.88(11) . . ?
Nb8 O23 Nb7 85.83(11) . . ?
Nb6 O24 Nb10 117.87(18) . . ?
Nb10 O25 Nb7 119.03(18) . . ?
Nb8 O26 Nb10 117.73(18) . . ?
Nb9 O27 Nb10 110.39(16) . . ?
C1 N1 C4 111.1(9) . . ?
C1 N1 C2 106.4(10) . . ?
C4 N1 C2 99.1(12) . . ?
C1 N1 C3 118.5(11) . . ?
C4 N1 C3 112.0(9) . . ?
C2 N1 C3 107.6(9) . . ?
C8 N2 C6 110.8(5) . . ?
C8 N2 C5 109.6(5) . . ?
C6 N2 C5 109.6(5) . . ?
C8 N2 C7 108.8(5) . . ?
C6 N2 C7 109.0(5) . . ?
C5 N2 C7 109.1(6) . . ?
C10 N3 C12 107.1(9) . . ?
C10 N3 C11 109.2(7) . . ?
C12 N3 C11 109.7(8) . . ?
C10 N3 C9 110.9(8) . . ?
C12 N3 C9 113.2(9) . . ?
C11 N3 C9 106.7(7) . . ?
C14 N4 C16 112.1(5) . . ?
C14 N4 C15 110.2(5) . . ?
C16 N4 C15 109.1(5) . . ?
C14 N4 C13 108.3(6) . . ?
C16 N4 C13 108.6(6) . . ?
C15 N4 C13 108.5(6) . . ?
C17 N5 C18 114.9(12) . . ?
C17 N5 C20 107.0(10) . . ?
C18 N5 C20 97.4(13) . . ?
C17 N5 C19 115.4(10) . . ?
C18 N5 C19 110.9(10) . . ?
C20 N5 C19 109.5(9) . . ?
C21 N6 C22 110.7(8) . . ?
C21 N6 C24 113.4(9) . . ?
C22 N6 C24 105.7(9) . . ?
C21 N6 C23 106.7(10) . . ?
C22 N6 C23 108.4(8) . . ?
C24 N6 C23 111.9(9) . . ?
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 . . ?
N4 C13 H13A 109.5 . . ?
N4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N4 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 C16 H16A 109.5 . . ?
N4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N5 C17 H17A 109.5 . . ?
N5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N5 C18 H18A 109.5 . . ?
N5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N5 C19 H19A 109.5 . . ?
N5 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N5 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N5 C20 H20A 109.5 . . ?
N5 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N5 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N6 C21 H21A 109.5 . . ?
N6 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N6 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N6 C22 H22A 109.5 . . ?
N6 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N6 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N6 C23 H23A 109.5 . . ?
N6 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N6 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N6 C24 H24A 109.5 . . ?
N6 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N6 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C28 N7 C27 109.5(12) . . ?
C28 N7 C25 109.6(12) . . ?
C27 N7 C25 110.7(11) . . ?
C28 N7 C26 109.4(12) . . ?
C27 N7 C26 110.6(11) . . ?
C25 N7 C26 107.0(11) . . ?
C28A N7A C26A 111.9(16) . . ?
C28A N7A C27A 111.2(16) . . ?
C26A N7A C27A 105.7(14) . . ?
C28A N7A C25A 110.2(16) . . ?
C26A N7A C25A 109.8(14) . . ?
C27A N7A C25A 107.9(14) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        30.54
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.481
_refine_diff_density_min         -2.144
_refine_diff_density_rms         0.171
_database_code_depnum_ccdc_archive 'CCDC 990477'
