# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_TMA-RhNb9
_database_code_depnum_ccdc_archive 'CCDC 1417431'
_audit_update_record             
;
2015-08-07 deposited with the CCDC.
2015-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'tetramethylammonium rhodium nonaniobate'
_chemical_melting_point          ?
_chemical_formula_moiety         'Nb8.88 O28 Rh1.12, 6(C4 H12 N), 14(H2 O)'
_chemical_formula_sum            'C24 H100 N6 Nb8.88 O42 Rh1.12'
_chemical_formula_weight         2084.19

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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   11.1230(8)
_cell_length_b                   12.1932(9)
_cell_length_c                   13.3388(10)
_cell_angle_alpha                85.9610(10)
_cell_angle_beta                 68.0040(10)
_cell_angle_gamma                87.8620(10)
_cell_volume                     1673.1(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    7553
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      27.49

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_F_000             1036
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.096
_exptl_absorpt_coefficient_mu    1.816
_shelx_estimated_absorpt_T_min   0.496
_shelx_estimated_absorpt_T_max   0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6039
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19423
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.047
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7620
_reflns_number_gt                7099
_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 SMART 1000'
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0290P)²+6.5947P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7620
_refine_ls_number_parameters     438
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0840
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.001
_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 0.26131(3) 0.36794(2) 0.27754(2) 0.01371(8) Uani 1 1 d . . . . .
Nb2 Nb 0.12942(4) 0.46748(2) 0.51932(2) 0.02644(13) Uani 0.438(13) 1 d . . P A
2
Nb3 Nb 0.15217(3) 0.62912(2) 0.30288(2) 0.01192(7) Uani 1 1 d . . . . .
Nb4 Nb -0.01361(3) 0.43800(3) 0.23769(2) 0.01423(8) Uani 1 1 d . . . . .
Nb5 Nb 0.02628(3) 0.72544(2) 0.54324(2) 0.01225(7) Uani 1 1 d . . . . .
Rh2 Rh 0.12942(4) 0.46748(2) 0.51932(2) 0.02644(13) Uani 0.562(13) 1 d . . P A
1
O1 O 0.4082(2) 0.3067(2) 0.1999(2) 0.0215(5) Uani 1 1 d . . . . .
O2 O 0.2865(2) 0.3968(2) 0.4243(2) 0.0153(5) Uani 1 1 d . . . . .
O3 O 0.2942(2) 0.5266(2) 0.24741(19) 0.0160(5) Uani 1 1 d . . . . .
O4 O 0.1601(2) 0.3723(2) 0.1863(2) 0.0171(5) Uani 1 1 d . . . . .
O5 O -0.1540(2) 0.75546(19) 0.6309(2) 0.0165(5) Uani 1 1 d . . . . .
O6 O 0.1739(2) 0.4860(2) 0.6447(2) 0.0160(5) Uani 1 1 d . . . . .
O7 O 0.1770(2) 0.62161(19) 0.45186(19) 0.0138(5) Uani 1 1 d . . . . .
O8 O 0.2202(2) 0.7572(2) 0.2483(2) 0.0192(5) Uani 1 1 d . . . . .
O9 O 0.0627(2) 0.5868(2) 0.21204(19) 0.0157(5) Uani 1 1 d . . . . .
O10 O -0.0708(3) 0.4241(2) 0.1343(2) 0.0233(6) Uani 1 1 d . . . . .
O11 O 0.0784(2) 0.6948(2) 0.6650(2) 0.0163(5) Uani 1 1 d . . . . .
O12 O 0.0853(3) 0.8572(2) 0.4933(2) 0.0198(5) Uani 1 1 d . . . . .
O13 O 0.0306(2) 0.32632(19) 0.58028(19) 0.0152(5) Uani 1 1 d . . . . .
O14 O -0.0542(2) 0.54194(18) 0.60442(19) 0.0133(5) Uani 1 1 d . . . . .
O15 O 0.7771(3) 0.9558(3) 0.5521(3) 0.0286(6) Uani 1 1 d . . . . .
O16 O 0.7847(5) 0.8165(4) 0.3820(5) 0.0702(14) Uani 1 1 d . . . . .
O17 O 0.8047(4) 0.9085(5) 0.1772(5) 0.0676(14) Uani 1 1 d . . . . .
O18 O 0.3813(3) 0.8969(3) 0.2940(3) 0.0392(8) Uani 1 1 d . . . . .
O19 O 0.5942(4) -0.0265(4) 0.1295(4) 0.0570(11) Uani 1 1 d . . . . .
O20 O 0.3820(5) 0.8059(4) 0.9309(5) 0.084(2) Uani 1 1 d . . . . .
O21 O 0.8640(3) 0.2979(3) 0.9957(3) 0.0306(7) Uani 1 1 d . . . . .
C1 C 0.7765(4) 0.6561(4) 0.0730(4) 0.0327(9) Uani 1 1 d . . . . .
H1A H 0.8327 0.6019 0.0923 0.049 Uiso 1 1 calc R U . . .
H1B H 0.7796 0.7260 0.1040 0.049 Uiso 1 1 calc R U . . .
H1C H 0.8065 0.6672 -0.0060 0.049 Uiso 1 1 calc R U . . .
C2 C 0.6387(5) 0.5052(4) 0.0771(5) 0.0423(12) Uani 1 1 d . . . . .
H2A H 0.5499 0.4775 0.1064 0.063 Uiso 1 1 calc R U . . .
H2B H 0.6947 0.4548 0.1009 0.063 Uiso 1 1 calc R U . . .
H2C H 0.6704 0.5105 -0.0022 0.063 Uiso 1 1 calc R U . . .
C3 C 0.5559(5) 0.6929(4) 0.0797(4) 0.0372(10) Uani 1 1 d . . . . .
H3A H 0.5883 0.6980 0.0004 0.056 Uiso 1 1 calc R U . . .
H3B H 0.5575 0.7658 0.1058 0.056 Uiso 1 1 calc R U . . .
H3C H 0.4668 0.6658 0.1086 0.056 Uiso 1 1 calc R U . . .
C4 C 0.5893(5) 0.6098(5) 0.2388(4) 0.0461(13) Uani 1 1 d . . . . .
H4A H 0.5000 0.5832 0.2675 0.069 Uiso 1 1 calc R U . . .
H4B H 0.5911 0.6832 0.2637 0.069 Uiso 1 1 calc R U . . .
H4C H 0.6437 0.5593 0.2645 0.069 Uiso 1 1 calc R U . . .
C5 C 0.9673(5) 0.8846(4) 0.8809(4) 0.0382(11) Uani 1 1 d . . . . .
H5A H 0.9760 0.8190 0.8402 0.057 Uiso 1 1 calc R U . . .
H5B H 0.9238 0.8652 0.9585 0.057 Uiso 1 1 calc R U . . .
H5C H 1.0535 0.9135 0.8670 0.057 Uiso 1 1 calc R U . . .
C6 C 0.9563(5) 1.0013(4) 0.7280(3) 0.0308(9) Uani 1 1 d . . . . .
H6A H 0.9654 0.9364 0.6862 0.046 Uiso 1 1 calc R U . . .
H6B H 1.0424 1.0298 0.7152 0.046 Uiso 1 1 calc R U . . .
H6C H 0.9055 1.0581 0.7052 0.046 Uiso 1 1 calc R U . . .
C7 C 0.7578(5) 0.9267(4) 0.8657(4) 0.0418(11) Uani 1 1 d . . . . .
H7A H 0.7091 0.9812 0.8380 0.063 Uiso 1 1 calc R U . . .
H7B H 0.7112 0.9116 0.9437 0.063 Uiso 1 1 calc R U . . .
H7C H 0.7671 0.8585 0.8285 0.063 Uiso 1 1 calc R U . . .
C8 C 0.8760(4) 1.0699(3) 0.9090(3) 0.0257(8) Uani 1 1 d . . . . .
H8A H 0.9622 1.0999 0.8931 0.039 Uiso 1 1 calc R U . . .
H8B H 0.8354 1.0496 0.9866 0.039 Uiso 1 1 calc R U . . .
H8C H 0.8222 1.1256 0.8884 0.039 Uiso 1 1 calc R U . . .
C10 C 0.5210(5) 0.8509(5) 0.6088(6) 0.0581(18) Uani 1 1 d . . . . .
H10A H 0.4993 0.8951 0.6720 0.087 Uiso 1 1 calc R U . . .
H10B H 0.5561 0.8986 0.5424 0.087 Uiso 1 1 calc R U . . .
H10C H 0.5859 0.7949 0.6102 0.087 Uiso 1 1 calc R U . . .
C11 C 0.2971(6) 0.8752(5) 0.6293(9) 0.092(3) Uani 1 1 d . . . . .
H11A H 0.2201 0.8389 0.6290 0.138 Uiso 1 1 calc R U . . .
H11B H 0.3234 0.9338 0.5714 0.138 Uiso 1 1 calc R U . . .
H11C H 0.2770 0.9068 0.6994 0.138 Uiso 1 1 calc R U . . .
C12 C 0.3723(9) 0.7070(9) 0.6893(9) 0.146(6) Uani 1 1 d . . . . .
H12A H 0.3304 0.7342 0.7618 0.219 Uiso 1 1 calc R U . . .
H12B H 0.4526 0.6676 0.6842 0.219 Uiso 1 1 calc R U . . .
H12C H 0.3137 0.6569 0.6759 0.219 Uiso 1 1 calc R U . . .
C13 C 0.4277(9) 0.7494(13) 0.5019(10) 0.166(7) Uani 1 1 d . . . . .
H13A H 0.5193 0.7281 0.4692 0.249 Uiso 1 1 calc R U . . .
H13B H 0.4071 0.8054 0.4541 0.249 Uiso 1 1 calc R U . . .
H13C H 0.3736 0.6848 0.5119 0.249 Uiso 1 1 calc R U . . .
H4 H 0.721(4) 0.807(4) 0.454(4) 0.015(7) Uiso 1 1 d . . . . .
H5 H 0.955(6) 0.298(5) 0.952(5) 0.045(16) Uiso 1 1 d . . . . .
H6 H 0.887(5) 0.340(5) 1.028(4) 0.038(15) Uiso 1 1 d . . . . .
H7 H 0.509(10) -0.051(8) 0.182(8) 0.12(3) Uiso 1 1 d . . . . .
H8 H 0.331(9) 0.929(8) 0.325(8) 0.11(4) Uiso 1 1 d . . . . .
H9 H 0.335(5) 0.854(5) 0.282(4) 0.031(13) Uiso 1 1 d . . . . .
H10 H 0.463(7) 0.765(6) 0.903(6) 0.07(2) Uiso 1 1 d . . . . .
H11 H 0.313(9) 0.762(7) 0.957(7) 0.11(3) Uiso 1 1 d . . . . .
H12 H 0.755(11) 0.887(9) 0.238(9) 0.14(5) Uiso 1 1 d . . . . .
H13 H 0.803(5) 0.908(5) 0.584(4) 0.036(15) Uiso 1 1 d . . . . .
H14 H 0.716(7) 0.922(6) 0.175(6) 0.07(2) Uiso 1 1 d . . . . .
H15 H 0.833(5) 1.001(4) 0.530(4) 0.022(12) Uiso 1 1 d . . . . .
H16 H 0.608(9) 0.034(8) 0.178(8) 0.12(3) Uiso 1 1 d . . . . .
H17 H 0.780(4) 0.734(4) 0.355(3) 0.015(7) Uiso 1 1 d . . . . .
N1 N 0.6402(3) 0.6154(3) 0.1168(3) 0.0248(7) Uani 1 1 d . . . . .
N2 N 0.8886(3) 0.9702(3) 0.8459(3) 0.0252(7) Uani 1 1 d . . . . .
N3 N 0.4011(4) 0.7960(4) 0.6117(4) 0.0443(11) Uani 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
Nb1 O1 1.747(3) . ?
Nb1 O4 1.940(2) . ?
Nb1 O3 1.967(2) . ?
Nb1 O5 1.991(2) 2_566 ?
Nb1 O2 2.133(2) . ?
Nb1 O14 2.516(2) 2_566 ?
Nb1 Nb2 3.3016(5) . ?
Nb1 Nb3 3.3594(5) . ?
Nb2 O6 1.943(2) . ?
Nb2 O2 1.946(2) . ?
Nb2 O7 2.025(2) . ?
Nb2 O13 2.026(2) . ?
Nb2 O14 2.123(2) 2_566 ?
Nb2 O14 2.134(2) . ?
Nb2 Nb2 3.1728(8) 2_566 ?
Nb2 Nb4 3.2835(5) 2_566 ?
Nb2 Nb5 3.3003(5) 2_566 ?
Nb2 Nb5 3.3029(5) . ?
Nb2 Nb3 3.3123(5) . ?
Nb3 O8 1.748(2) . ?
Nb3 O3 1.927(2) . ?
Nb3 O9 1.938(2) . ?
Nb3 O7 2.102(2) . ?
Nb3 O13 2.126(2) 2_566 ?
Nb3 O14 2.422(2) 2_566 ?
Nb3 Nb5 3.2655(5) . ?
Nb3 Nb2 3.3376(5) 2_566 ?
Nb4 O10 1.742(3) . ?
Nb4 O4 1.953(3) . ?
Nb4 O11 1.980(2) 2_566 ?
Nb4 O9 1.985(2) . ?
Nb4 O6 2.118(2) 2_566 ?
Nb4 O14 2.518(2) 2_566 ?
Nb4 Nb2 3.2835(5) 2_566 ?
Nb5 O12 1.748(2) . ?
Nb5 O11 1.928(2) . ?
Nb5 O5 1.942(2) . ?
Nb5 O7 2.104(2) . ?
Nb5 O13 2.115(2) 2_566 ?
Nb5 O14 2.412(2) . ?
Nb5 Nb2 3.3003(5) 2_566 ?
Rh2 O6 1.943(2) . ?
Rh2 O2 1.946(2) . ?
Rh2 O7 2.025(2) . ?
Rh2 O13 2.026(2) . ?
Rh2 O14 2.123(2) 2_566 ?
Rh2 O14 2.134(2) . ?
Rh2 Rh2 3.1728(8) 2_566 ?
O5 Nb1 1.991(2) 2_566 ?
O6 Nb4 2.118(2) 2_566 ?
O11 Nb4 1.980(2) 2_566 ?
O13 Nb5 2.115(2) 2_566 ?
O13 Nb3 2.126(2) 2_566 ?
O14 Rh2 2.123(2) 2_566 ?
O14 Nb2 2.123(2) 2_566 ?
O14 Nb3 2.421(2) 2_566 ?
O14 Nb1 2.516(2) 2_566 ?
O14 Nb4 2.518(2) 2_566 ?
O15 H13 0.80(6) . ?
O15 H15 0.80(5) . ?
O16 H4 0.95(4) . ?
O16 H17 1.10(4) . ?
O17 H12 0.82(11) . ?
O17 H14 1.01(8) . ?
O18 H8 0.68(10) . ?
O18 H9 0.82(6) . ?
O19 H7 0.98(10) . ?
O19 H16 1.06(10) . ?
O20 H10 0.97(7) . ?
O20 H11 0.89(10) . ?
O21 H5 0.96(6) . ?
O21 H6 0.80(6) . ?
C1 N1 1.496(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.481(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 N1 1.494(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 N1 1.507(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 N2 1.498(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N2 1.496(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.490(6) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 N2 1.500(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 N3 1.501(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N3 1.439(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N3 1.404(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N3 1.529(11) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 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
O1 Nb1 O4 104.24(12) . . ?
O1 Nb1 O3 104.00(11) . . ?
O4 Nb1 O3 90.97(10) . . ?
O1 Nb1 O5 104.89(11) . 2_566 ?
O4 Nb1 O5 89.98(10) . 2_566 ?
O3 Nb1 O5 149.91(10) . 2_566 ?
O1 Nb1 O2 103.29(11) . . ?
O4 Nb1 O2 152.46(10) . . ?
O3 Nb1 O2 83.10(10) . . ?
O5 Nb1 O2 82.28(10) 2_566 . ?
O1 Nb1 O14 177.36(11) . 2_566 ?
O4 Nb1 O14 78.37(9) . 2_566 ?
O3 Nb1 O14 75.43(9) . 2_566 ?
O5 Nb1 O14 75.32(9) 2_566 2_566 ?
O2 Nb1 O14 74.10(8) . 2_566 ?
O1 Nb1 Nb2 137.38(9) . . ?
O4 Nb1 Nb2 118.38(7) . . ?
O3 Nb1 Nb2 76.71(7) . . ?
O5 Nb1 Nb2 76.44(7) 2_566 . ?
O2 Nb1 Nb2 34.09(6) . . ?
O14 Nb1 Nb2 40.01(5) 2_566 . ?
O1 Nb1 Nb3 133.74(9) . . ?
O4 Nb1 Nb3 80.04(7) . . ?
O3 Nb1 Nb3 30.04(7) . . ?
O5 Nb1 Nb3 121.28(7) 2_566 . ?
O2 Nb1 Nb3 81.56(6) . . ?
O14 Nb1 Nb3 45.96(5) 2_566 . ?
Nb2 Nb1 Nb3 59.633(9) . . ?
O6 Nb2 O2 100.86(10) . . ?
O6 Nb2 O7 95.95(10) . . ?
O2 Nb2 O7 95.86(10) . . ?
O6 Nb2 O13 94.96(10) . . ?
O2 Nb2 O13 95.62(10) . . ?
O7 Nb2 O13 162.37(10) . . ?
O6 Nb2 O14 171.58(10) . 2_566 ?
O2 Nb2 O14 87.56(10) . 2_566 ?
O7 Nb2 O14 83.19(9) . 2_566 ?
O13 Nb2 O14 83.98(9) . 2_566 ?
O6 Nb2 O14 87.96(10) . . ?
O2 Nb2 O14 171.17(10) . . ?
O7 Nb2 O14 83.56(9) . . ?
O13 Nb2 O14 83.05(9) . . ?
O14 Nb2 O14 83.62(9) 2_566 . ?
O6 Nb2 Nb2 129.64(7) . 2_566 ?
O2 Nb2 Nb2 129.51(7) . 2_566 ?
O7 Nb2 Nb2 81.10(7) . 2_566 ?
O13 Nb2 Nb2 81.28(7) . 2_566 ?
O14 Nb2 Nb2 41.95(6) 2_566 2_566 ?
O14 Nb2 Nb2 41.67(6) . 2_566 ?
O6 Nb2 Nb4 37.89(7) . 2_566 ?
O2 Nb2 Nb4 138.75(7) . 2_566 ?
O7 Nb2 Nb4 90.58(7) . 2_566 ?
O13 Nb2 Nb4 89.57(7) . 2_566 ?
O14 Nb2 Nb4 133.69(6) 2_566 2_566 ?
O14 Nb2 Nb4 50.07(6) . 2_566 ?
Nb2 Nb2 Nb4 91.744(15) 2_566 2_566 ?
O6 Nb2 Nb5 132.98(7) . 2_566 ?
O2 Nb2 Nb5 85.56(7) . 2_566 ?
O7 Nb2 Nb5 130.01(7) . 2_566 ?
O13 Nb2 Nb5 38.09(7) . 2_566 ?
O14 Nb2 Nb5 46.87(6) 2_566 2_566 ?
O14 Nb2 Nb5 88.09(6) . 2_566 ?
Nb2 Nb2 Nb5 61.322(12) 2_566 2_566 ?
Nb4 Nb2 Nb5 120.200(13) 2_566 2_566 ?
O6 Nb2 Nb1 138.77(7) . . ?
O2 Nb2 Nb1 37.91(7) . . ?
O7 Nb2 Nb1 90.06(7) . . ?
O13 Nb2 Nb1 90.81(7) . . ?
O14 Nb2 Nb1 49.65(6) 2_566 . ?
O14 Nb2 Nb1 133.27(6) . . ?
Nb2 Nb2 Nb1 91.597(14) 2_566 . ?
Nb4 Nb2 Nb1 176.657(15) 2_566 . ?
Nb5 Nb2 Nb1 61.530(9) 2_566 . ?
O6 Nb2 Nb5 86.07(7) . . ?
O2 Nb2 Nb5 133.51(7) . . ?
O7 Nb2 Nb5 37.71(7) . . ?
O13 Nb2 Nb5 129.85(7) . . ?
O14 Nb2 Nb5 88.20(6) 2_566 . ?
O14 Nb2 Nb5 46.83(6) . . ?
Nb2 Nb2 Nb5 61.242(11) 2_566 . ?
Nb4 Nb2 Nb5 61.746(9) 2_566 . ?
Nb5 Nb2 Nb5 122.564(14) 2_566 . ?
Nb1 Nb2 Nb5 120.205(12) . . ?
O6 Nb2 Nb3 133.26(7) . . ?
O2 Nb2 Nb3 85.43(7) . . ?
O7 Nb2 Nb3 37.41(7) . . ?
O13 Nb2 Nb3 130.82(7) . . ?
O14 Nb2 Nb3 46.87(6) 2_566 . ?
O14 Nb2 Nb3 88.84(6) . . ?
Nb2 Nb2 Nb3 61.904(11) 2_566 . ?
Nb4 Nb2 Nb3 120.868(13) 2_566 . ?
Nb5 Nb2 Nb3 93.456(12) 2_566 . ?
Nb1 Nb2 Nb3 61.051(10) . . ?
Nb5 Nb2 Nb3 59.159(10) . . ?
O8 Nb3 O3 104.07(11) . . ?
O8 Nb3 O9 105.89(11) . . ?
O3 Nb3 O9 94.94(10) . . ?
O8 Nb3 O7 100.30(11) . . ?
O3 Nb3 O7 90.13(10) . . ?
O9 Nb3 O7 151.17(10) . . ?
O8 Nb3 O13 102.26(11) . 2_566 ?
O3 Nb3 O13 151.39(10) . 2_566 ?
O9 Nb3 O13 88.43(10) . 2_566 ?
O7 Nb3 O13 74.26(9) . 2_566 ?
O8 Nb3 O14 174.47(10) . 2_566 ?
O3 Nb3 O14 78.46(9) . 2_566 ?
O9 Nb3 O14 78.59(9) . 2_566 ?
O7 Nb3 O14 74.66(8) . 2_566 ?
O13 Nb3 O14 74.38(9) 2_566 2_566 ?
O8 Nb3 Nb5 90.27(8) . . ?
O3 Nb3 Nb5 129.20(7) . . ?
O9 Nb3 Nb5 127.94(7) . . ?
O7 Nb3 Nb5 39.09(7) . . ?
O13 Nb3 Nb5 39.52(6) 2_566 . ?
O14 Nb3 Nb5 84.37(6) 2_566 . ?
O8 Nb3 Nb2 135.58(9) . . ?
O3 Nb3 Nb2 76.86(7) . . ?
O9 Nb3 Nb2 118.37(7) . . ?
O7 Nb3 Nb2 35.83(6) . . ?
O13 Nb3 Nb2 76.58(6) 2_566 . ?
O14 Nb3 Nb2 39.77(5) 2_566 . ?
Nb5 Nb3 Nb2 60.276(10) . . ?
O8 Nb3 Nb2 137.55(9) . 2_566 ?
O3 Nb3 Nb2 118.09(7) . 2_566 ?
O9 Nb3 Nb2 76.53(7) . 2_566 ?
O7 Nb3 Nb2 76.07(6) . 2_566 ?
O13 Nb3 Nb2 35.50(7) 2_566 2_566 ?
O14 Nb3 Nb2 39.63(5) 2_566 2_566 ?
Nb5 Nb3 Nb2 59.964(9) . 2_566 ?
Nb2 Nb3 Nb2 56.994(14) . 2_566 ?
O8 Nb3 Nb1 134.65(9) . . ?
O3 Nb3 Nb1 30.72(7) . . ?
O9 Nb3 Nb1 82.95(7) . . ?
O7 Nb3 Nb1 87.21(6) . . ?
O13 Nb3 Nb1 122.67(7) 2_566 . ?
O14 Nb3 Nb1 48.32(6) 2_566 . ?
Nb5 Nb3 Nb1 119.586(11) . . ?
Nb2 Nb3 Nb1 59.316(9) . . ?
Nb2 Nb3 Nb1 87.766(11) 2_566 . ?
O10 Nb4 O4 105.19(12) . . ?
O10 Nb4 O11 103.60(11) . 2_566 ?
O4 Nb4 O11 89.27(10) . 2_566 ?
O10 Nb4 O9 105.99(11) . . ?
O4 Nb4 O9 90.11(10) . . ?
O11 Nb4 O9 149.49(10) 2_566 . ?
O10 Nb4 O6 101.86(11) . 2_566 ?
O4 Nb4 O6 152.91(10) . 2_566 ?
O11 Nb4 O6 82.89(10) 2_566 2_566 ?
O9 Nb4 O6 83.92(10) . 2_566 ?
O10 Nb4 O14 176.33(11) . 2_566 ?
O4 Nb4 O14 78.10(9) . 2_566 ?
O11 Nb4 O14 74.62(9) 2_566 2_566 ?
O9 Nb4 O14 75.41(9) . 2_566 ?
O6 Nb4 O14 74.82(8) 2_566 2_566 ?
O10 Nb4 Nb2 136.13(10) . 2_566 ?
O4 Nb4 Nb2 118.63(7) . 2_566 ?
O11 Nb4 Nb2 76.19(7) 2_566 2_566 ?
O9 Nb4 Nb2 77.41(7) . 2_566 ?
O6 Nb4 Nb2 34.29(6) 2_566 2_566 ?
O14 Nb4 Nb2 40.53(5) 2_566 2_566 ?
O12 Nb5 O11 104.06(11) . . ?
O12 Nb5 O5 102.17(11) . . ?
O11 Nb5 O5 94.90(10) . . ?
O12 Nb5 O7 103.34(11) . . ?
O11 Nb5 O7 89.20(10) . . ?
O5 Nb5 O7 152.32(10) . . ?
O12 Nb5 O13 102.33(11) . 2_566 ?
O11 Nb5 O13 151.54(10) . 2_566 ?
O5 Nb5 O13 89.77(10) . 2_566 ?
O7 Nb5 O13 74.46(9) . 2_566 ?
O12 Nb5 O14 177.55(10) . . ?
O11 Nb5 O14 78.08(9) . . ?
O5 Nb5 O14 78.71(9) . . ?
O7 Nb5 O14 75.39(8) . . ?
O13 Nb5 O14 75.34(9) 2_566 . ?
O12 Nb5 Nb3 92.23(8) . . ?
O11 Nb5 Nb3 128.23(7) . . ?
O5 Nb5 Nb3 129.55(7) . . ?
O7 Nb5 Nb3 39.04(6) . . ?
O13 Nb5 Nb3 39.78(7) 2_566 . ?
O14 Nb5 Nb3 85.48(6) . . ?
O12 Nb5 Nb2 137.87(9) . 2_566 ?
O11 Nb5 Nb2 118.04(7) . 2_566 ?
O5 Nb5 Nb2 77.00(7) . 2_566 ?
O7 Nb5 Nb2 76.93(6) . 2_566 ?
O13 Nb5 Nb2 36.24(7) 2_566 2_566 ?
O14 Nb5 Nb2 39.96(5) . 2_566 ?
Nb3 Nb5 Nb2 61.102(10) . 2_566 ?
O12 Nb5 Nb2 138.87(9) . . ?
O11 Nb5 Nb2 76.25(7) . . ?
O5 Nb5 Nb2 118.89(7) . . ?
O7 Nb5 Nb2 36.06(6) . . ?
O13 Nb5 Nb2 76.93(6) 2_566 . ?
O14 Nb5 Nb2 40.18(6) . . ?
Nb3 Nb5 Nb2 60.564(9) . . ?
Nb2 Nb5 Nb2 57.435(14) 2_566 . ?
O6 Rh2 O2 100.86(10) . . ?
O6 Rh2 O7 95.95(10) . . ?
O2 Rh2 O7 95.86(10) . . ?
O6 Rh2 O13 94.96(10) . . ?
O2 Rh2 O13 95.62(10) . . ?
O7 Rh2 O13 162.37(10) . . ?
O6 Rh2 O14 171.58(10) . 2_566 ?
O2 Rh2 O14 87.56(10) . 2_566 ?
O7 Rh2 O14 83.19(9) . 2_566 ?
O13 Rh2 O14 83.98(9) . 2_566 ?
O6 Rh2 O14 87.96(10) . . ?
O2 Rh2 O14 171.17(10) . . ?
O7 Rh2 O14 83.56(9) . . ?
O13 Rh2 O14 83.05(9) . . ?
O14 Rh2 O14 83.62(9) 2_566 . ?
O6 Rh2 Rh2 129.64(7) . 2_566 ?
O2 Rh2 Rh2 129.51(7) . 2_566 ?
O7 Rh2 Rh2 81.10(7) . 2_566 ?
O13 Rh2 Rh2 81.28(7) . 2_566 ?
O14 Rh2 Rh2 41.95(6) 2_566 2_566 ?
O14 Rh2 Rh2 41.67(6) . 2_566 ?
Rh2 O2 Nb1 108.00(11) . . ?
Nb2 O2 Nb1 108.00(11) . . ?
Nb3 O3 Nb1 119.24(12) . . ?
Nb1 O4 Nb4 119.62(12) . . ?
Nb5 O5 Nb1 118.33(12) . 2_566 ?
Rh2 O6 Nb4 107.82(11) . 2_566 ?
Nb2 O6 Nb4 107.82(11) . 2_566 ?
Rh2 O7 Nb3 106.76(10) . . ?
Nb2 O7 Nb3 106.76(10) . . ?
Rh2 O7 Nb5 106.23(10) . . ?
Nb2 O7 Nb5 106.23(10) . . ?
Nb3 O7 Nb5 101.88(10) . . ?
Nb3 O9 Nb4 118.76(12) . . ?
Nb5 O11 Nb4 119.75(12) . 2_566 ?
Rh2 O13 Nb5 105.67(10) . 2_566 ?
Nb2 O13 Nb5 105.67(10) . 2_566 ?
Rh2 O13 Nb3 106.95(10) . 2_566 ?
Nb2 O13 Nb3 106.95(10) . 2_566 ?
Nb5 O13 Nb3 100.70(10) 2_566 2_566 ?
Nb2 O14 Nb2 96.38(9) 2_566 . ?
Rh2 O14 Rh2 96.38(9) 2_566 . ?
Rh2 O14 Nb5 93.18(8) 2_566 . ?
Nb2 O14 Nb5 93.18(8) 2_566 . ?
Nb2 O14 Nb5 92.99(9) . . ?
Rh2 O14 Nb5 92.99(9) . . ?
Rh2 O14 Nb3 93.36(9) 2_566 2_566 ?
Nb2 O14 Nb3 93.36(9) 2_566 2_566 ?
Nb2 O14 Nb3 94.00(8) . 2_566 ?
Rh2 O14 Nb3 94.00(8) . 2_566 ?
Nb5 O14 Nb3 169.85(11) . 2_566 ?
Rh2 O14 Nb1 90.34(8) 2_566 2_566 ?
Nb2 O14 Nb1 90.34(8) 2_566 2_566 ?
Nb2 O14 Nb1 173.28(11) . 2_566 ?
Rh2 O14 Nb1 173.28(11) . 2_566 ?
Nb5 O14 Nb1 86.48(7) . 2_566 ?
Nb3 O14 Nb1 85.72(7) 2_566 2_566 ?
Rh2 O14 Nb4 174.22(12) 2_566 2_566 ?
Nb2 O14 Nb4 174.22(12) 2_566 2_566 ?
Nb2 O14 Nb4 89.40(8) . 2_566 ?
Rh2 O14 Nb4 89.40(8) . 2_566 ?
Nb5 O14 Nb4 86.52(7) . 2_566 ?
Nb3 O14 Nb4 86.20(7) 2_566 2_566 ?
Nb1 O14 Nb4 83.88(7) 2_566 2_566 ?
H13 O15 H15 106(5) . . ?
H4 O16 H17 98(4) . . ?
H12 O17 H14 76(8) . . ?
H8 O18 H9 94(8) . . ?
H7 O19 H16 96(7) . . ?
H10 O20 H11 112(7) . . ?
H5 O21 H6 82(5) . . ?
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 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 . . ?
N3 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C2 N1 C3 109.7(4) . . ?
C2 N1 C1 109.0(3) . . ?
C3 N1 C1 109.8(3) . . ?
C2 N1 C4 110.5(4) . . ?
C3 N1 C4 108.4(4) . . ?
C1 N1 C4 109.4(4) . . ?
C7 N2 C6 109.7(3) . . ?
C7 N2 C5 109.9(4) . . ?
C6 N2 C5 109.4(3) . . ?
C7 N2 C8 110.0(3) . . ?
C6 N2 C8 108.9(3) . . ?
C5 N2 C8 108.9(3) . . ?
C12 N3 C11 114.1(7) . . ?
C12 N3 C10 108.9(4) . . ?
C11 N3 C10 110.2(5) . . ?
C12 N3 C13 107.3(9) . . ?
C11 N3 C13 107.1(7) . . ?
C10 N3 C13 109.2(6) . . ?

_refine_diff_density_max         1.553
_refine_diff_density_min         -2.307
_refine_diff_density_rms         0.118

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TMA-Rh2Nb10
_database_code_depnum_ccdc_archive 'CCDC 1417432'
_audit_update_record             
;
2015-08-07 deposited with the CCDC.
2015-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'tetramethylammonium bis-rhodium decaniobate'
_chemical_melting_point          ?
_chemical_formula_moiety         'H4 Nb10 O34 Rh2, 8(C4 H12 N), 18(H2 O)'
_chemical_formula_sum            'C32 H136 N8 Nb10 O52 Rh2'
_chemical_formula_weight         2600.40

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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.0911(15)
_cell_length_b                   15.379(2)
_cell_length_c                   24.327(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.748(2)
_cell_angle_gamma                90
_cell_volume                     4140.6(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    9151
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      27.53

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_F_000             2600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.443
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.244
_exptl_absorpt_coefficient_mu    1.815
_shelx_estimated_absorpt_T_min   0.500
_shelx_estimated_absorpt_T_max   0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6654
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44814
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.844
_diffrn_reflns_theta_max         27.541
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9483
_reflns_number_gt                9099
_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-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0152P)²+6.8050P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9483
_refine_ls_number_parameters     565
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_ref         0.0460
_refine_ls_wR_factor_gt          0.0454
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.004
_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 0.55507(2) 0.72820(2) -0.08708(2) 0.00786(4) Uani 1 1 d . . . . .
Nb2 Nb 0.50628(2) 1.06209(2) 0.10842(2) 0.00718(4) Uani 1 1 d . . . . .
Nb3 Nb 0.66862(2) 0.86729(2) 0.00849(2) 0.00721(4) Uani 1 1 d . . . . .
Nb4 Nb 0.44359(2) 0.73379(2) 0.03719(2) 0.00815(4) Uani 1 1 d . . . . .
Nb5 Nb 0.27428(2) 0.80428(2) -0.07405(2) 0.00841(4) Uani 1 1 d . . . . .
Rh1 Rh 0.39882(2) 0.93848(2) 0.01441(2) 0.00638(4) Uani 1 1 d . . . . .
O1 O 0.61779(13) 0.64421(9) -0.12590(6) 0.0128(3) Uani 1 1 d . . . . .
O2 O 0.43870(12) 1.16595(9) 0.13530(6) 0.0101(3) Uani 1 1 d . . . . .
O3 O 0.70118(12) 0.77857(9) -0.04445(6) 0.0095(3) Uani 1 1 d . . . . .
O4 O 0.51852(12) 0.66741(9) -0.01864(6) 0.0105(3) Uani 1 1 d . . . . .
O5 O 0.37859(12) 0.72325(9) -0.10997(6) 0.0107(3) Uani 1 1 d . . . . .
O6 O 0.46774(12) 0.84103(9) -0.03243(5) 0.0082(3) Uani 1 1 d . . . . .
O7 O 0.48164(13) 0.98132(9) 0.15849(6) 0.0125(3) Uani 1 1 d . . . . .
O8 O 0.35279(12) 1.04594(9) 0.05626(5) 0.0084(3) Uani 1 1 d . . . . .
O9 O 0.67219(12) 1.09730(9) 0.11999(5) 0.0099(3) Uani 1 1 d . . . . .
O10 O 0.81073(12) 0.89697(9) 0.03959(6) 0.0122(3) Uani 1 1 d . . . . .
O11 O 0.60095(12) 0.78989(9) 0.05950(6) 0.0103(3) Uani 1 1 d . . . . .
O12 O 0.56771(12) 0.97266(9) 0.04490(5) 0.0079(3) Uani 1 1 d . . . . .
O13 O 0.42637(13) 0.65671(9) 0.08975(6) 0.0135(3) Uani 1 1 d . . . . .
O14 O 0.28644(12) 0.73666(9) -0.00493(6) 0.0108(3) Uani 1 1 d . . . . .
O15 O 0.37456(13) 0.84862(9) 0.07520(6) 0.0102(3) Uani 1 1 d . . . . .
O16 O 0.12676(13) 0.78278(10) -0.10231(6) 0.0141(3) Uani 1 1 d . . . . .
O17 O 0.23113(13) 0.90847(10) -0.01983(6) 0.0104(3) Uani 1 1 d . . . . .
O18 O 0.08276(18) 0.68489(14) 0.04426(8) 0.0283(4) Uani 1 1 d . . . . .
O19 O 0.9460(2) 0.78636(13) 0.11142(8) 0.0315(4) Uani 1 1 d . . . . .
O20 O 0.43560(15) 0.52339(11) 0.16251(7) 0.0168(3) Uani 1 1 d . . . . .
O21 O 0.13698(17) 0.40388(12) 0.12945(8) 0.0234(4) Uani 1 1 d . . . . .
O22 O 0.97690(19) 0.41500(13) 0.21206(8) 0.0267(4) Uani 1 1 d . . . . .
O23 O 0.06474(16) 0.28433(11) 0.05081(7) 0.0182(3) Uani 1 1 d . . . . .
O24 O 0.16014(19) 0.06975(13) 0.29088(9) 0.0333(4) Uani 1 1 d . . . . .
O25 O 0.38078(16) 0.00483(12) 0.25860(8) 0.0223(4) Uani 1 1 d . . . . .
O26 O 0.26315(16) 0.64338(13) 0.79938(8) 0.0213(3) Uani 1 1 d . . . . .
N1 N 0.07192(15) 0.02202(11) 0.12681(7) 0.0122(3) Uani 1 1 d . . . . .
N2 N 0.18313(16) 0.66947(12) 0.20872(7) 0.0149(4) Uani 1 1 d . . . . .
N3 N 0.75826(16) 0.51874(11) 0.04564(7) 0.0135(3) Uani 1 1 d . . . . .
N4 N 0.67003(19) 0.79894(15) 0.22757(8) 0.0254(4) Uani 1 1 d . . . . .
C1 C 0.1537(2) -0.05366(15) 0.14002(11) 0.0224(5) Uani 1 1 d . . . . .
H1A H 0.2293 -0.0460 0.1219 0.034 Uiso 1 1 calc R U . . .
H1B H 0.1140 -0.1074 0.1269 0.034 Uiso 1 1 calc R U . . .
H1C H 0.1711 -0.0572 0.1800 0.034 Uiso 1 1 calc R U . . .
C2 C 0.1324(2) 0.10343(15) 0.14761(9) 0.0189(4) Uani 1 1 d . . . . .
H2A H 0.0779 0.1529 0.1406 0.028 Uiso 1 1 calc R U . . .
H2B H 0.2066 0.1126 0.1286 0.028 Uiso 1 1 calc R U . . .
H2C H 0.1524 0.0982 0.1873 0.028 Uiso 1 1 calc R U . . .
C3 C 0.0477(2) 0.02785(15) 0.06562(8) 0.0172(4) Uani 1 1 d . . . . .
H3A H -0.0014 0.0795 0.0565 0.026 Uiso 1 1 calc R U . . .
H3B H 0.0042 -0.0242 0.0522 0.026 Uiso 1 1 calc R U . . .
H3C H 0.1245 0.0321 0.0480 0.026 Uiso 1 1 calc R U . . .
C4 C -0.04479(19) 0.00993(15) 0.15340(9) 0.0176(4) Uani 1 1 d . . . . .
H4A H -0.0285 0.0019 0.1932 0.026 Uiso 1 1 calc R U . . .
H4B H -0.0866 -0.0414 0.1378 0.026 Uiso 1 1 calc R U . . .
H4C H -0.0957 0.0614 0.1467 0.026 Uiso 1 1 calc R U . . .
C5 C 0.2683(2) 0.63743(16) 0.25452(9) 0.0218(5) Uani 1 1 d . . . . .
H5A H 0.3378 0.6093 0.2391 0.033 Uiso 1 1 calc R U . . .
H5B H 0.2266 0.5954 0.2769 0.033 Uiso 1 1 calc R U . . .
H5C H 0.2962 0.6866 0.2776 0.033 Uiso 1 1 calc R U . . .
C6 C 0.2455(2) 0.73666(14) 0.17622(9) 0.0183(4) Uani 1 1 d . . . . .
H6A H 0.2685 0.7861 0.2001 0.027 Uiso 1 1 calc R U . . .
H6B H 0.1908 0.7566 0.1455 0.027 Uiso 1 1 calc R U . . .
H6C H 0.3181 0.7113 0.1618 0.027 Uiso 1 1 calc R U . . .
C7 C 0.1449(2) 0.59578(15) 0.17145(10) 0.0227(5) Uani 1 1 d . . . . .
H7A H 0.0882 0.6171 0.1419 0.034 Uiso 1 1 calc R U . . .
H7B H 0.1054 0.5510 0.1926 0.034 Uiso 1 1 calc R U . . .
H7C H 0.2160 0.5709 0.1554 0.034 Uiso 1 1 calc R U . . .
C8 C 0.0742(2) 0.70885(16) 0.23218(11) 0.0234(5) Uani 1 1 d . . . . .
H8A H 0.0996 0.7551 0.2581 0.035 Uiso 1 1 calc R U . . .
H8B H 0.0306 0.6640 0.2515 0.035 Uiso 1 1 calc R U . . .
H8C H 0.0210 0.7332 0.2023 0.035 Uiso 1 1 calc R U . . .
C9 C 0.7961(2) 0.60984(15) 0.05880(11) 0.0253(5) Uani 1 1 d . . . . .
H9A H 0.8714 0.6227 0.0415 0.038 Uiso 1 1 calc R U . . .
H9B H 0.8088 0.6166 0.0988 0.038 Uiso 1 1 calc R U . . .
H9C H 0.7328 0.6501 0.0447 0.038 Uiso 1 1 calc R U . . .
C10 C 0.6441(2) 0.49985(16) 0.07274(11) 0.0262(5) Uani 1 1 d . . . . .
H10A H 0.5809 0.5403 0.0589 0.039 Uiso 1 1 calc R U . . .
H10B H 0.6580 0.5069 0.1127 0.039 Uiso 1 1 calc R U . . .
H10C H 0.6186 0.4400 0.0644 0.039 Uiso 1 1 calc R U . . .
C11 C 0.8542(2) 0.45685(16) 0.06672(10) 0.0252(5) Uani 1 1 d . . . . .
H11A H 0.8283 0.3971 0.0583 0.038 Uiso 1 1 calc R U . . .
H11B H 0.8679 0.4637 0.1067 0.038 Uiso 1 1 calc R U . . .
H11C H 0.9292 0.4691 0.0490 0.038 Uiso 1 1 calc R U . . .
C12 C 0.7363(3) 0.50831(18) -0.01517(10) 0.0285(6) Uani 1 1 d . . . . .
H12A H 0.6726 0.5486 -0.0287 0.043 Uiso 1 1 calc R U . . .
H12B H 0.7110 0.4484 -0.0235 0.043 Uiso 1 1 calc R U . . .
H12C H 0.8108 0.5210 -0.0332 0.043 Uiso 1 1 calc R U . . .
C13 C 0.5437(3) 0.8093(3) 0.24199(15) 0.0493(9) Uani 1 1 d . . . . .
H13A H 0.4987 0.8427 0.2131 0.074 Uiso 1 1 calc R U . . .
H13B H 0.5419 0.8402 0.2772 0.074 Uiso 1 1 calc R U . . .
H13C H 0.5065 0.7519 0.2453 0.074 Uiso 1 1 calc R U . . .
C14 C 0.6749(8) 0.7572(7) 0.17589(19) 0.228(7) Uani 1 1 d . . . . .
H14A H 0.6411 0.6985 0.1780 0.342 Uiso 1 1 calc R U . . .
H14B H 0.7591 0.7535 0.1662 0.342 Uiso 1 1 calc R U . . .
H14C H 0.6280 0.7907 0.1477 0.342 Uiso 1 1 calc R U . . .
C15 C 0.7402(2) 0.74870(17) 0.27057(10) 0.0237(5) Uani 1 1 d . . . . .
H15A H 0.7021 0.6919 0.2750 0.036 Uiso 1 1 calc R U . . .
H15B H 0.7420 0.7805 0.3055 0.036 Uiso 1 1 calc R U . . .
H15C H 0.8229 0.7405 0.2596 0.036 Uiso 1 1 calc R U . . .
C16 C 0.7179(4) 0.8879(4) 0.2284(4) 0.174(5) Uani 1 1 d . . . . .
H16A H 0.8064 0.8860 0.2303 0.261 Uiso 1 1 calc R U . . .
H16B H 0.6910 0.9188 0.2607 0.261 Uiso 1 1 calc R U . . .
H16C H 0.6883 0.9184 0.1948 0.261 Uiso 1 1 calc R U . . .
H1 H 0.413(3) 0.868(2) 0.1012(13) 0.028(8) Uiso 1 1 d . . . . .
H2 H 0.214(3) 0.950(2) -0.0333(12) 0.023(8) Uiso 1 1 d . . . . .
H3 H 0.144(3) 0.702(2) 0.0360(14) 0.043(10) Uiso 1 1 d . . . . .
H4 H 0.038(3) 0.6932(19) 0.0189(13) 0.024(8) Uiso 1 1 d . . . . .
H5 H 0.905(3) 0.814(2) 0.0920(15) 0.044(10) Uiso 1 1 d . . . . .
H6 H 0.992(3) 0.761(2) 0.0911(14) 0.037(9) Uiso 1 1 d . . . . .
H7 H 0.437(3) 0.559(2) 0.1407(14) 0.032(9) Uiso 1 1 d . . . . .
H8 H 0.420(3) 0.479(2) 0.1482(12) 0.020(7) Uiso 1 1 d . . . . .
H9 H 0.208(3) 0.395(2) 0.1303(13) 0.034(9) Uiso 1 1 d . . . . .
H10 H 0.112(3) 0.372(2) 0.1052(13) 0.030(8) Uiso 1 1 d . . . . .
H11 H 0.916(4) 0.390(3) 0.2037(15) 0.051(11) Uiso 1 1 d . . . . .
H12 H 1.018(3) 0.406(2) 0.1890(15) 0.040(10) Uiso 1 1 d . . . . .
H13 H 0.121(4) 0.261(2) 0.0511(15) 0.045(11) Uiso 1 1 d . . . . .
H14 H 0.017(3) 0.255(2) 0.0643(13) 0.033(9) Uiso 1 1 d . . . . .
H15 H 0.237(3) 0.048(2) 0.2810(15) 0.052(11) Uiso 1 1 d . . . . .
H16 H 0.108(4) 0.012(3) 0.2920(17) 0.075(13) Uiso 1 1 d . . . . .
H17 H 0.407(3) 0.001(2) 0.2286(13) 0.027(8) Uiso 1 1 d . . . . .
H18 H 0.435(3) 0.011(2) 0.2811(14) 0.037(9) Uiso 1 1 d . . . . .
H19 H 0.298(3) 0.663(2) 0.8254(13) 0.027(8) Uiso 1 1 d . . . . .
H20 H 0.299(3) 0.608(2) 0.7905(13) 0.031(9) 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
Nb1 O1 1.7692(14) . ?
Nb1 O4 1.9744(14) . ?
Nb1 O5 2.0012(14) . ?
Nb1 O2 2.0104(14) 3_675 ?
Nb1 O3 2.0203(14) . ?
Nb1 O6 2.4259(13) . ?
Nb1 Nb2 3.3299(5) 3_675 ?
Nb1 Nb4 3.3413(5) . ?
Nb1 Nb3 3.3443(4) . ?
Nb2 O7 1.7734(14) . ?
Nb2 O2 1.8987(14) . ?
Nb2 O9 1.9211(14) . ?
Nb2 O8 2.0707(14) . ?
Nb2 O12 2.2093(13) . ?
Nb2 O6 2.4061(13) 3_675 ?
Nb2 Rh1 3.1476(4) . ?
Nb2 Rh1 3.2323(4) 3_675 ?
Nb2 Nb1 3.3299(5) 3_675 ?
Nb2 Nb5 3.3334(4) 3_675 ?
Nb3 O10 1.7632(14) . ?
Nb3 O11 1.9085(14) . ?
Nb3 O3 1.9266(14) . ?
Nb3 O8 2.0662(14) 3_675 ?
Nb3 O12 2.1892(13) . ?
Nb3 O6 2.4142(13) . ?
Nb3 Rh1 3.1205(4) 3_675 ?
Nb3 Rh1 3.1985(4) . ?
Nb3 Nb4 3.3407(4) . ?
Nb4 O13 1.7630(14) . ?
Nb4 O4 1.9302(14) . ?
Nb4 O14 1.9638(14) . ?
Nb4 O11 1.9902(14) . ?
Nb4 O15 2.1569(14) . ?
Nb4 O6 2.3916(13) . ?
Nb4 Rh1 3.2290(5) . ?
Nb5 O16 1.7641(14) . ?
Nb5 O5 1.9460(14) . ?
Nb5 O14 1.9742(14) . ?
Nb5 O9 1.9948(14) 3_675 ?
Nb5 O17 2.1492(15) . ?
Nb5 O6 2.3800(13) . ?
Nb5 Rh1 3.2265(3) . ?
Nb5 Nb2 3.3334(4) 3_675 ?
Rh1 O8 2.0239(13) . ?
Rh1 O12 2.0380(13) . ?
Rh1 O12 2.0390(13) 3_675 ?
Rh1 O17 2.0405(14) . ?
Rh1 O15 2.0543(14) . ?
Rh1 O6 2.0598(13) . ?
Rh1 Rh1 3.0522(4) 3_675 ?
Rh1 Nb3 3.1206(4) 3_675 ?
O2 Nb1 2.0104(14) 3_675 ?
O6 Nb2 2.4061(13) 3_675 ?
O8 Nb3 2.0662(14) 3_675 ?
O9 Nb5 1.9948(14) 3_675 ?
O12 Rh1 2.0390(13) 3_675 ?
O15 H1 0.80(3) . ?
O17 H2 0.74(3) . ?
O18 H3 0.76(4) . ?
O18 H4 0.78(3) . ?
O19 H5 0.77(4) . ?
O19 H6 0.84(4) . ?
O20 H7 0.76(3) . ?
O20 H8 0.78(3) . ?
O21 H9 0.79(3) . ?
O21 H10 0.80(3) . ?
O22 H11 0.79(4) . ?
O22 H12 0.76(4) . ?
O23 H13 0.72(4) . ?
O23 H14 0.78(4) . ?
O24 H15 0.96(4) . ?
O24 H16 1.06(5) . ?
O25 H17 0.80(3) . ?
O25 H18 0.79(4) . ?
O26 H19 0.78(3) . ?
O26 H20 0.72(3) . ?
N1 C2 1.493(3) . ?
N1 C4 1.496(3) . ?
N1 C1 1.497(3) . ?
N1 C3 1.498(3) . ?
N2 C7 1.495(3) . ?
N2 C5 1.496(3) . ?
N2 C6 1.498(3) . ?
N2 C8 1.498(3) . ?
N3 C9 1.491(3) . ?
N3 C12 1.492(3) . ?
N3 C11 1.493(3) . ?
N3 C10 1.493(3) . ?
N4 C14 1.416(5) . ?
N4 C16 1.468(5) . ?
N4 C13 1.475(4) . ?
N4 C15 1.480(3) . ?
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 . ?

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 102.36(6) . . ?
O1 Nb1 O5 103.61(6) . . ?
O4 Nb1 O5 88.03(6) . . ?
O1 Nb1 O2 104.47(6) . 3_675 ?
O4 Nb1 O2 153.16(6) . 3_675 ?
O5 Nb1 O2 86.49(6) . 3_675 ?
O1 Nb1 O3 102.93(6) . . ?
O4 Nb1 O3 87.18(6) . . ?
O5 Nb1 O3 153.45(6) . . ?
O2 Nb1 O3 86.10(6) 3_675 . ?
O1 Nb1 O6 178.76(6) . . ?
O4 Nb1 O6 76.43(5) . . ?
O5 Nb1 O6 76.20(5) . . ?
O2 Nb1 O6 76.75(5) 3_675 . ?
O3 Nb1 O6 77.30(5) . . ?
O1 Nb1 Nb2 135.02(5) . 3_675 ?
O4 Nb1 Nb2 122.61(4) . 3_675 ?
O5 Nb1 Nb2 78.89(4) . 3_675 ?
O2 Nb1 Nb2 30.60(4) 3_675 3_675 ?
O3 Nb1 Nb2 81.81(4) . 3_675 ?
O6 Nb1 Nb2 46.19(3) . 3_675 ?
O1 Nb1 Nb4 133.11(5) . . ?
O4 Nb1 Nb4 30.77(4) . . ?
O5 Nb1 Nb4 80.78(4) . . ?
O2 Nb1 Nb4 122.42(4) 3_675 . ?
O3 Nb1 Nb4 81.81(4) . . ?
O6 Nb1 Nb4 45.66(3) . . ?
Nb2 Nb1 Nb4 91.842(6) 3_675 . ?
O1 Nb1 Nb3 134.01(5) . . ?
O4 Nb1 Nb3 78.78(4) . . ?
O5 Nb1 Nb3 122.33(4) . . ?
O2 Nb1 Nb3 82.07(4) 3_675 . ?
O3 Nb1 Nb3 31.24(4) . . ?
O6 Nb1 Nb3 46.15(3) . . ?
Nb2 Nb1 Nb3 63.427(9) 3_675 . ?
Nb4 Nb1 Nb3 59.958(9) . . ?
O7 Nb2 O2 105.70(6) . . ?
O7 Nb2 O9 106.61(6) . . ?
O2 Nb2 O9 96.22(6) . . ?
O7 Nb2 O8 100.34(6) . . ?
O2 Nb2 O8 89.12(6) . . ?
O9 Nb2 O8 149.87(6) . . ?
O7 Nb2 O12 96.48(6) . . ?
O2 Nb2 O12 155.70(5) . . ?
O9 Nb2 O12 86.66(5) . . ?
O8 Nb2 O12 77.03(5) . . ?
O7 Nb2 O6 173.21(6) . 3_675 ?
O2 Nb2 O6 79.26(5) . 3_675 ?
O9 Nb2 O6 77.08(5) . 3_675 ?
O8 Nb2 O6 74.84(5) . 3_675 ?
O12 Nb2 O6 77.89(5) . 3_675 ?
O7 Nb2 Rh1 90.46(5) . . ?
O2 Nb2 Rh1 128.25(4) . . ?
O9 Nb2 Rh1 126.17(4) . . ?
O8 Nb2 Rh1 39.22(4) . . ?
O12 Nb2 Rh1 40.12(3) . . ?
O6 Nb2 Rh1 82.79(3) 3_675 . ?
O7 Nb2 Rh1 135.01(5) . 3_675 ?
O2 Nb2 Rh1 118.72(4) . 3_675 ?
O9 Nb2 Rh1 76.68(4) . 3_675 ?
O8 Nb2 Rh1 74.78(4) . 3_675 ?
O12 Nb2 Rh1 38.54(3) . 3_675 ?
O6 Nb2 Rh1 39.54(3) 3_675 3_675 ?
Rh1 Nb2 Rh1 57.144(8) . 3_675 ?
O7 Nb2 Nb1 138.28(5) . 3_675 ?
O2 Nb2 Nb1 32.61(4) . 3_675 ?
O9 Nb2 Nb1 86.21(4) . 3_675 ?
O8 Nb2 Nb1 82.48(4) . 3_675 ?
O12 Nb2 Nb1 124.27(4) . 3_675 ?
O6 Nb2 Nb1 46.69(3) 3_675 3_675 ?
Rh1 Nb2 Nb1 114.074(10) . 3_675 ?
Rh1 Nb2 Nb1 86.221(6) 3_675 3_675 ?
O7 Nb2 Nb5 138.76(5) . 3_675 ?
O2 Nb2 Nb5 83.04(4) . 3_675 ?
O9 Nb2 Nb5 32.32(4) . 3_675 ?
O8 Nb2 Nb5 120.32(4) . 3_675 ?
O12 Nb2 Nb5 86.84(4) . 3_675 ?
O6 Nb2 Nb5 45.53(3) 3_675 3_675 ?
Rh1 Nb2 Nb5 115.986(10) . 3_675 ?
Rh1 Nb2 Nb5 58.843(6) 3_675 3_675 ?
Nb1 Nb2 Nb5 60.585(9) 3_675 3_675 ?
O10 Nb3 O11 105.13(6) . . ?
O10 Nb3 O3 105.60(6) . . ?
O11 Nb3 O3 95.27(6) . . ?
O10 Nb3 O8 102.41(6) . 3_675 ?
O11 Nb3 O8 150.23(6) . 3_675 ?
O3 Nb3 O8 87.99(6) . 3_675 ?
O10 Nb3 O12 95.80(6) . . ?
O11 Nb3 O12 88.02(5) . . ?
O3 Nb3 O12 156.61(5) . . ?
O8 Nb3 O12 78.12(5) 3_675 . ?
O10 Nb3 O6 174.39(6) . . ?
O11 Nb3 O6 76.83(5) . . ?
O3 Nb3 O6 79.29(5) . . ?
O8 Nb3 O6 74.74(5) 3_675 . ?
O12 Nb3 O6 78.94(5) . . ?
O10 Nb3 Rh1 91.49(5) . 3_675 ?
O11 Nb3 Rh1 127.83(4) . 3_675 ?
O3 Nb3 Rh1 127.72(4) . 3_675 ?
O8 Nb3 Rh1 39.78(4) 3_675 3_675 ?
O12 Nb3 Rh1 40.61(3) . 3_675 ?
O6 Nb3 Rh1 83.25(3) . 3_675 ?
O10 Nb3 Rh1 134.81(5) . . ?
O11 Nb3 Rh1 77.02(4) . . ?
O3 Nb3 Rh1 119.30(4) . . ?
O8 Nb3 Rh1 75.65(4) 3_675 . ?
O12 Nb3 Rh1 39.09(3) . . ?
O6 Nb3 Rh1 40.08(3) . . ?
Rh1 Nb3 Rh1 57.749(5) 3_675 . ?
O10 Nb3 Nb4 136.76(5) . . ?
O11 Nb3 Nb4 31.76(4) . . ?
O3 Nb3 Nb4 83.09(4) . . ?
O8 Nb3 Nb4 120.40(4) 3_675 . ?
O12 Nb3 Nb4 87.80(4) . . ?
O6 Nb3 Nb4 45.68(3) . . ?
Rh1 Nb3 Nb4 116.869(10) 3_675 . ?
Rh1 Nb3 Nb4 59.133(10) . . ?
O10 Nb3 Nb1 138.53(5) . . ?
O11 Nb3 Nb1 84.65(4) . . ?
O3 Nb3 Nb1 32.94(4) . . ?
O8 Nb3 Nb1 82.18(4) 3_675 . ?
O12 Nb3 Nb1 125.13(4) . . ?
O6 Nb3 Nb1 46.44(3) . . ?
Rh1 Nb3 Nb1 114.405(9) 3_675 . ?
Rh1 Nb3 Nb1 86.522(8) . . ?
Nb4 Nb3 Nb1 59.977(8) . . ?
O13 Nb4 O4 103.10(6) . . ?
O13 Nb4 O14 105.01(6) . . ?
O4 Nb4 O14 93.04(6) . . ?
O13 Nb4 O11 103.20(6) . . ?
O4 Nb4 O11 90.63(6) . . ?
O14 Nb4 O11 149.90(6) . . ?
O13 Nb4 O15 100.45(6) . . ?
O4 Nb4 O15 156.34(6) . . ?
O14 Nb4 O15 82.96(6) . . ?
O11 Nb4 O15 81.82(6) . . ?
O13 Nb4 O6 178.61(6) . . ?
O4 Nb4 O6 78.06(5) . . ?
O14 Nb4 O6 75.62(5) . . ?
O11 Nb4 O6 75.96(5) . . ?
O15 Nb4 O6 78.36(5) . . ?
O13 Nb4 Rh1 139.22(5) . . ?
O4 Nb4 Rh1 117.60(4) . . ?
O14 Nb4 Rh1 76.54(4) . . ?
O11 Nb4 Rh1 75.32(4) . . ?
O15 Nb4 Rh1 38.78(4) . . ?
O6 Nb4 Rh1 39.58(3) . . ?
O13 Nb4 Nb3 133.05(5) . . ?
O4 Nb4 Nb3 79.40(4) . . ?
O14 Nb4 Nb3 121.79(4) . . ?
O11 Nb4 Nb3 30.32(4) . . ?
O15 Nb4 Nb3 82.96(4) . . ?
O6 Nb4 Nb3 46.24(3) . . ?
Rh1 Nb4 Nb3 58.238(8) . . ?
O13 Nb4 Nb1 134.65(5) . . ?
O4 Nb4 Nb1 31.55(4) . . ?
O14 Nb4 Nb1 84.08(4) . . ?
O11 Nb4 Nb1 83.58(4) . . ?
O15 Nb4 Nb1 124.86(4) . . ?
O6 Nb4 Nb1 46.51(3) . . ?
Rh1 Nb4 Nb1 86.083(6) . . ?
Nb3 Nb4 Nb1 60.066(6) . . ?
O16 Nb5 O5 105.57(6) . . ?
O16 Nb5 O14 104.07(6) . . ?
O5 Nb5 O14 92.05(6) . . ?
O16 Nb5 O9 103.08(6) . 3_675 ?
O5 Nb5 O9 91.54(6) . 3_675 ?
O14 Nb5 O9 150.53(6) . 3_675 ?
O16 Nb5 O17 98.09(6) . . ?
O5 Nb5 O17 156.32(6) . . ?
O14 Nb5 O17 82.85(6) . . ?
O9 Nb5 O17 82.21(6) 3_675 . ?
O16 Nb5 O6 176.12(6) . . ?
O5 Nb5 O6 78.30(5) . . ?
O14 Nb5 O6 75.72(5) . . ?
O9 Nb5 O6 76.41(5) 3_675 . ?
O17 Nb5 O6 78.03(5) . . ?
O16 Nb5 Rh1 136.51(5) . . ?
O5 Nb5 Rh1 117.90(4) . . ?
O14 Nb5 Rh1 76.49(4) . . ?
O9 Nb5 Rh1 76.01(4) 3_675 . ?
O17 Nb5 Rh1 38.42(4) . . ?
O6 Nb5 Rh1 39.61(3) . . ?
O16 Nb5 Nb2 133.76(5) . 3_675 ?
O5 Nb5 Nb2 79.46(4) . 3_675 ?
O14 Nb5 Nb2 121.87(4) . 3_675 ?
O9 Nb5 Nb2 30.99(4) 3_675 3_675 ?
O17 Nb5 Nb2 83.67(4) . 3_675 ?
O6 Nb5 Nb2 46.18(3) . 3_675 ?
Rh1 Nb5 Nb2 59.013(8) . 3_675 ?
O8 Rh1 O12 82.10(5) . . ?
O8 Rh1 O12 82.66(5) . 3_675 ?
O12 Rh1 O12 83.06(6) . 3_675 ?
O8 Rh1 O17 97.87(6) . . ?
O12 Rh1 O17 176.82(6) . . ?
O12 Rh1 O17 93.78(6) 3_675 . ?
O8 Rh1 O15 97.94(6) . . ?
O12 Rh1 O15 94.13(6) . . ?
O12 Rh1 O15 177.03(5) 3_675 . ?
O17 Rh1 O15 89.02(6) . . ?
O8 Rh1 O6 170.87(5) . . ?
O12 Rh1 O6 91.35(5) . . ?
O12 Rh1 O6 90.28(5) 3_675 . ?
O17 Rh1 O6 88.33(6) . . ?
O15 Rh1 O6 88.83(6) . . ?
O8 Rh1 Rh1 79.79(4) . 3_675 ?
O12 Rh1 Rh1 41.54(4) . 3_675 ?
O12 Rh1 Rh1 41.52(4) 3_675 3_675 ?
O17 Rh1 Rh1 135.30(4) . 3_675 ?
O15 Rh1 Rh1 135.67(4) . 3_675 ?
O6 Rh1 Rh1 91.08(4) . 3_675 ?
O8 Rh1 Nb3 40.78(4) . 3_675 ?
O12 Rh1 Nb3 91.26(4) . 3_675 ?
O12 Rh1 Nb3 44.33(4) 3_675 3_675 ?
O17 Rh1 Nb3 86.68(4) . 3_675 ?
O15 Rh1 Nb3 136.99(4) . 3_675 ?
O6 Rh1 Nb3 133.70(4) . 3_675 ?
Rh1 Rh1 Nb3 62.407(10) 3_675 3_675 ?
O8 Rh1 Nb2 40.31(4) . . ?
O12 Rh1 Nb2 44.31(4) . . ?
O12 Rh1 Nb2 91.81(4) 3_675 . ?
O17 Rh1 Nb2 136.47(4) . . ?
O15 Rh1 Nb2 86.82(4) . . ?
O6 Rh1 Nb2 134.81(4) . . ?
Rh1 Rh1 Nb2 62.824(9) 3_675 . ?
Nb3 Rh1 Nb2 68.074(10) 3_675 . ?
O8 Rh1 Nb3 124.73(4) . . ?
O12 Rh1 Nb3 42.63(4) . . ?
O12 Rh1 Nb3 89.05(4) 3_675 . ?
O17 Rh1 Nb3 137.28(4) . . ?
O15 Rh1 Nb3 88.23(4) . . ?
O6 Rh1 Nb3 49.00(4) . . ?
Rh1 Rh1 Nb3 59.844(11) 3_675 . ?
Nb3 Rh1 Nb3 122.251(5) 3_675 . ?
Nb2 Rh1 Nb3 85.900(8) . . ?
O8 Rh1 Nb5 138.31(4) . . ?
O12 Rh1 Nb5 138.67(4) . . ?
O12 Rh1 Nb5 92.67(4) 3_675 . ?
O17 Rh1 Nb5 40.88(4) . . ?
O15 Rh1 Nb5 88.82(4) . . ?
O6 Rh1 Nb5 47.45(4) . . ?
Rh1 Rh1 Nb5 122.174(10) 3_675 . ?
Nb3 Rh1 Nb5 113.955(10) 3_675 . ?
Nb2 Rh1 Nb5 174.989(7) . . ?
Nb3 Rh1 Nb5 96.430(9) . . ?
O8 Rh1 Nb4 138.66(4) . . ?
O12 Rh1 Nb4 93.53(4) . . ?
O12 Rh1 Nb4 137.88(4) 3_675 . ?
O17 Rh1 Nb4 88.59(4) . . ?
O15 Rh1 Nb4 41.12(4) . . ?
O6 Rh1 Nb4 47.72(4) . . ?
Rh1 Rh1 Nb4 122.459(10) 3_675 . ?
Nb3 Rh1 Nb4 174.981(7) 3_675 . ?
Nb2 Rh1 Nb4 114.671(10) . . ?
Nb3 Rh1 Nb4 62.629(6) . . ?
Nb5 Rh1 Nb4 62.949(8) . . ?
Nb2 O2 Nb1 116.79(7) . 3_675 ?
Nb3 O3 Nb1 115.82(7) . . ?
Nb4 O4 Nb1 117.68(7) . . ?
Nb5 O5 Nb1 116.75(7) . . ?
Rh1 O6 Nb5 92.94(5) . . ?
Rh1 O6 Nb4 92.70(5) . . ?
Nb5 O6 Nb4 89.88(5) . . ?
Rh1 O6 Nb2 92.40(5) . 3_675 ?
Nb5 O6 Nb2 88.29(4) . 3_675 ?
Nb4 O6 Nb2 174.66(6) . 3_675 ?
Rh1 O6 Nb3 90.92(5) . . ?
Nb5 O6 Nb3 175.72(6) . . ?
Nb4 O6 Nb3 88.07(4) . . ?
Nb2 O6 Nb3 93.41(5) 3_675 . ?
Rh1 O6 Nb1 178.23(7) . . ?
Nb5 O6 Nb1 88.75(4) . . ?
Nb4 O6 Nb1 87.83(4) . . ?
Nb2 O6 Nb1 87.12(4) 3_675 . ?
Nb3 O6 Nb1 87.41(4) . . ?
Rh1 O8 Nb3 99.45(6) . 3_675 ?
Rh1 O8 Nb2 100.47(6) . . ?
Nb3 O8 Nb2 116.02(6) 3_675 . ?
Nb2 O9 Nb5 116.68(7) . 3_675 ?
Nb3 O11 Nb4 117.92(7) . . ?
Rh1 O12 Rh1 96.95(6) . 3_675 ?
Rh1 O12 Nb3 98.28(6) . . ?
Rh1 O12 Nb3 95.06(5) 3_675 . ?
Rh1 O12 Nb2 95.56(5) . . ?
Rh1 O12 Nb2 99.00(6) 3_675 . ?
Nb3 O12 Nb2 158.90(7) . . ?
Nb4 O14 Nb5 117.72(7) . . ?
Rh1 O15 Nb4 100.10(6) . . ?
Rh1 O15 H1 103(2) . . ?
Nb4 O15 H1 117(2) . . ?
Rh1 O17 Nb5 100.70(6) . . ?
Rh1 O17 H2 101(2) . . ?
Nb5 O17 H2 116(2) . . ?
H3 O18 H4 105(3) . . ?
H5 O19 H6 105(3) . . ?
H7 O20 H8 109(3) . . ?
H9 O21 H10 102(3) . . ?
H11 O22 H12 105(4) . . ?
H13 O23 H14 109(4) . . ?
H15 O24 H16 102(3) . . ?
H17 O25 H18 110(3) . . ?
H19 O26 H20 107(3) . . ?
C2 N1 C4 109.88(17) . . ?
C2 N1 C1 109.08(17) . . ?
C4 N1 C1 109.84(17) . . ?
C2 N1 C3 109.51(17) . . ?
C4 N1 C3 109.47(16) . . ?
C1 N1 C3 109.05(17) . . ?
C7 N2 C5 110.01(18) . . ?
C7 N2 C6 108.99(17) . . ?
C5 N2 C6 109.25(17) . . ?
C7 N2 C8 109.50(18) . . ?
C5 N2 C8 109.57(18) . . ?
C6 N2 C8 109.52(17) . . ?
C9 N3 C12 109.84(19) . . ?
C9 N3 C11 109.95(18) . . ?
C12 N3 C11 109.79(18) . . ?
C9 N3 C10 108.81(18) . . ?
C12 N3 C10 109.18(19) . . ?
C11 N3 C10 109.25(18) . . ?
C14 N4 C16 113.6(6) . . ?
C14 N4 C13 110.6(4) . . ?
C16 N4 C13 104.2(4) . . ?
C14 N4 C15 110.0(3) . . ?
C16 N4 C15 107.7(3) . . ?
C13 N4 C15 110.6(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 . . ?
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 . . ?

_refine_diff_density_max         1.628
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.078

