# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_43
_database_code_depnum_ccdc_archive 'CCDC 1423580'
_audit_update_record             
;
2015-09-11 deposited with the CCDC.
2016-01-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT043_43                  
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      24.71 Check
RESPONSE: H-atoms of the solvate water molecules and disordered MeOH were not localized
;

# Added during the CSD deposition process: Friday 11th of September 2015 08:10:04 AM
# end Validation Reply Form

#complex 1
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26.12 H72.50 Na4 Nb6 O35.12 Ru2'
_chemical_formula_weight         1800.40

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   30.105(3)
_cell_length_b                   30.105(3)
_cell_length_c                   14.0549(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12738(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7727
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      26.35

_exptl_crystal_description       rhombohedra
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_F_000             7106
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.012
_exptl_crystal_size_min          0.012
_exptl_absorpt_coefficient_mu    1.608
_shelx_estimated_absorpt_T_min   0.910
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean 25
_diffrn_reflns_number            26872
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.353
_diffrn_reflns_theta_max         26.394
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6515
_reflns_number_gt                5049
_reflns_threshold_expression     >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       'APEX2 (Bruker-AXS, 2004)'
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXLE (Sheldrick, 2011)'
_computing_publication_material  'CIFTAB-97 (Sheldrick, 1998)'
_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)+(0.0528P)²+99.6420P] 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         6515
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.1093
_refine_ls_wR_factor_gt          0.0971
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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
C2 C -0.0086(2) 0.67492(19) 0.1315(5) 0.0362(16) Uani 1 1 d . . . . .
H2A H -0.0332 0.6680 0.1768 0.043 Uiso 1 1 calc R U . . .
C1M C 0.1740(3) 0.6147(3) -0.4382(6) 0.068(3) Uani 1 1 d . . . . .
H1MA H 0.1770 0.6312 -0.4979 0.102 Uiso 1 1 calc R U . . .
H1MB H 0.2024 0.6148 -0.4043 0.102 Uiso 1 1 calc R U . . .
H1MC H 0.1653 0.5840 -0.4521 0.102 Uiso 1 1 calc R U . . .
C3 C -0.01909(19) 0.68402(18) 0.0355(5) 0.0301(15) Uani 1 1 d . . . . .
H3A H -0.0508 0.6836 0.0142 0.036 Uiso 1 1 calc R U . . .
C2M C 0.0259(2) 0.6123(3) -0.3139(5) 0.0433(18) Uani 1 1 d . . . . .
H2MA H -0.0049 0.6227 -0.3108 0.065 Uiso 1 1 calc R U . . .
H2MB H 0.0404 0.6248 -0.3702 0.065 Uiso 1 1 calc R U . . .
H2MC H 0.0262 0.5798 -0.3180 0.065 Uiso 1 1 calc R U . . .
C4 C 0.0153(2) 0.68424(17) -0.0325(5) 0.0259(13) Uani 1 1 d . . . . .
H4A H 0.0072 0.6835 -0.1015 0.031 Uiso 1 1 calc R U . . .
C3M C 0.1005(3) 0.5120(3) -0.3843(5) 0.052(2) Uani 1 1 d . . . . .
H3MA H 0.0954 0.4802 -0.3743 0.078 Uiso 1 1 calc R U . . .
H3MB H 0.0741 0.5254 -0.4133 0.078 Uiso 1 1 calc R U . . .
H3MC H 0.1261 0.5160 -0.4266 0.078 Uiso 1 1 calc R U . . .
C5 C 0.05985(19) 0.67651(18) -0.0065(5) 0.0280(14) Uani 1 1 d . . . . .
H5A H 0.0825 0.6706 -0.0570 0.034 Uiso 1 1 calc R U . . .
C4M C 0.2196(3) 0.5423(2) -0.2169(7) 0.062(2) Uani 1 1 d . . . . .
H4MA H 0.2498 0.5390 -0.1917 0.092 Uiso 1 1 calc R U . . .
H4MB H 0.2015 0.5170 -0.1967 0.092 Uiso 1 1 calc R U . . .
H4MC H 0.2208 0.5433 -0.2866 0.092 Uiso 1 1 calc R U . . .
C6 C 0.0700(2) 0.66759(18) 0.0889(5) 0.0304(15) Uani 1 1 d . . . . .
H6A H 0.0999 0.6554 0.1050 0.036 Uiso 1 1 calc R U . . .
C5M C 0.2734(5) 0.5609(5) 0.1007(10) 0.138(6) Uani 1 1 d . . . . .
H5MA H 0.3046 0.5539 0.0875 0.207 Uiso 1 1 calc R U . . .
H5MB H 0.2718 0.5840 0.1497 0.207 Uiso 1 1 calc R U . . .
H5MC H 0.2581 0.5341 0.1232 0.207 Uiso 1 1 calc R U . . .
C7 C 0.0357(2) 0.6669(2) 0.1603(5) 0.0378(16) Uani 1 1 d . . . . .
H7A H 0.0420 0.6549 0.2252 0.045 Uiso 1 1 calc R U . . .
C6M C 0.2143(3) 0.6728(4) 0.1520(7) 0.079(3) Uani 1 1 d . . . . .
H6MA H 0.2139 0.7041 0.1709 0.119 Uiso 1 1 calc R U . . .
H6MB H 0.2014 0.6546 0.2028 0.119 Uiso 1 1 calc R U . . .
H6MC H 0.2451 0.6635 0.1407 0.119 Uiso 1 1 calc R U . . .
C7M C 0.0931(6) 0.6068(6) 0.3678(12) 0.077(5) Uani 0.6 1 d . . P . .
O2 O -0.01601(11) 0.41740(11) 0.0788(3) 0.0166(8) Uani 1 1 d . . . . .
O3 O 0.0000 0.5000 0.0000 0.0150(11) Uani 1 2 d S . P . .
O2W O 0.04881(13) 0.62584(13) -0.2316(3) 0.0279(9) Uani 1 1 d . . . . .
O4 O 0.05198(11) 0.56377(11) 0.0886(3) 0.0172(8) Uani 1 1 d . . . . .
O3W O 0.10908(16) 0.53239(14) -0.2969(3) 0.0368(11) Uani 1 1 d . . . . .
O5 O 0.05332(11) 0.50489(11) -0.1600(3) 0.0177(8) Uani 1 1 d . . . . .
O4W O 0.14010(15) 0.63549(14) -0.3793(3) 0.0357(11) Uani 1 1 d . . . . .
O6 O -0.00099(13) 0.55981(13) 0.2680(3) 0.0243(9) Uani 1 1 d . . . . .
O5W O 0.20074(15) 0.58222(13) -0.1820(4) 0.0388(12) Uani 1 1 d . . . . .
O7 O 0.11270(12) 0.56981(12) -0.0762(3) 0.0209(8) Uani 1 1 d . . . . .
O6W O 0.14055(18) 0.57510(19) 0.1496(5) 0.0632(16) Uani 1 1 d . . . . .
O8 O 0.09083(11) 0.48545(11) 0.0159(3) 0.0172(8) Uani 1 1 d . . . . .
O7W O 0.18914(18) 0.66725(18) 0.0671(4) 0.0504(14) Uani 1 1 d . . . . .
O8M O 0.1265(3) 0.6272(3) 0.3074(6) 0.055(2) Uani 0.6 1 d . . P . .
O8W O 0.2518(2) 0.5770(2) 0.0126(5) 0.081(2) Uani 1 1 d . . . . .
O10M O -0.0379(4) 0.6220(4) 0.3746(8) 0.035(3) Uiso 0.4 1 d . . P . .
C10M C -0.0145(7) 0.6282(7) 0.4440(17) 0.061(6) Uiso 0.4 1 d . . P . .
C11M C 0.031(3) 0.708(3) 0.399(6) 0.017(17) Uiso 0.0622 1 d . . P . .
O11M O 0.0000 0.7500 0.3750 0.082(16) Uiso 0.2488 4 d S . P . .
O11 O 0.08142(12) 0.40057(12) 0.1077(3) 0.0205(8) Uani 1 1 d . . . . .
O9 O 0.03422(11) 0.42237(11) -0.0737(3) 0.0164(8) Uani 1 1 d . . . . .
O12 O 0.03712(11) 0.48010(11) 0.1768(3) 0.0166(8) Uani 1 1 d . . . . .
Na1 Na 0.12544(7) 0.60237(7) -0.22906(16) 0.0226(5) Uani 1 1 d . . . . .
Na2 Na 0.17649(9) 0.60106(9) -0.0170(2) 0.0444(7) Uani 1 1 d . . . . .
Nb1 Nb 0.04674(2) 0.44289(2) 0.06429(4) 0.01443(12) Uani 1 1 d . . . . .
Nb2 Nb 0.06596(2) 0.53801(2) -0.04431(4) 0.01419(12) Uani 1 1 d . . . . .
Nb3 Nb -0.00003(2) 0.53277(2) 0.15783(3) 0.01484(12) Uani 1 1 d . . . . .
Ru1 Ru 0.01806(2) 0.62224(2) 0.04496(3) 0.01646(12) 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
C2 C7 1.413(10) . ?
C2 C3 1.413(10) . ?
C2 Ru1 2.154(6) . ?
C2 H2A 1.0000 . ?
C1M O4W 1.455(10) . ?
C1M H1MA 0.9800 . ?
C1M H1MB 0.9800 . ?
C1M H1MC 0.9800 . ?
C3 C4 1.408(9) . ?
C3 Ru1 2.174(5) . ?
C3 H3A 1.0000 . ?
C2M O2W 1.408(8) . ?
C2M H2MA 0.9800 . ?
C2M H2MB 0.9800 . ?
C2M H2MC 0.9800 . ?
C4 C5 1.410(8) . ?
C4 Ru1 2.162(5) . ?
C4 H4A 1.0000 . ?
C3M O3W 1.398(8) . ?
C3M H3MA 0.9800 . ?
C3M H3MB 0.9800 . ?
C3M H3MC 0.9800 . ?
C5 C6 1.402(9) . ?
C5 Ru1 2.185(5) . ?
C5 H5A 1.0000 . ?
C4M O5W 1.417(8) . ?
C4M H4MA 0.9800 . ?
C4M H4MB 0.9800 . ?
C4M H4MC 0.9800 . ?
C6 C7 1.440(10) . ?
C6 Ru1 2.165(5) . ?
C6 H6A 1.0000 . ?
C5M O8W 1.480(12) . ?
C5M H5MA 0.9800 . ?
C5M H5MB 0.9800 . ?
C5M H5MC 0.9800 . ?
C7 Ru1 2.172(6) . ?
C7 H7A 1.0000 . ?
C6M O7W 1.424(10) . ?
C6M H6MA 0.9800 . ?
C6M H6MB 0.9800 . ?
C6M H6MC 0.9800 . ?
C7M O8M 1.453(19) . ?
O2 Nb1 2.049(3) . ?
O2 Nb2 2.073(3) 9_565 ?
O2 Ru1 2.111(4) 9_565 ?
O3 Nb2 2.3749(5) 9_565 ?
O3 Nb2 2.3749(5) . ?
O3 Nb1 2.3986(5) . ?
O3 Nb1 2.3986(5) 9_565 ?
O3 Nb3 2.4278(5) . ?
O3 Nb3 2.4278(5) 9_565 ?
O2W Na1 2.413(5) . ?
O4 Nb2 2.066(4) . ?
O4 Nb3 2.066(4) . ?
O4 Ru1 2.126(3) . ?
O3W Na1 2.364(5) . ?
O5 Nb2 1.945(4) . ?
O5 Nb3 1.965(3) 9_565 ?
O4W Na1 2.376(5) . ?
O6 Nb3 1.750(4) . ?
O5W Na1 2.438(5) . ?
O5W Na2 2.496(6) . ?
O7 Nb2 1.760(4) . ?
O7 Na2 2.295(4) . ?
O7 Na1 2.393(4) . ?
O6W Na2 2.696(7) . ?
O8 Nb2 1.945(3) . ?
O8 Nb1 1.966(3) . ?
O7W Na2 2.348(6) . ?
O8W Na2 2.416(7) . ?
O10M C10M 1.22(2) . ?
C11M O11M 1.61(8) . ?
O11M C11M 1.61(8) 11_566 ?
O11M C11M 1.61(8) 16_666 ?
O11M C11M 1.61(8) 6_464 ?
O11 Nb1 1.756(4) . ?
O11 Na1 2.456(4) 3 ?
O11 Na2 2.801(5) 3 ?
O9 Nb3 2.069(4) 9_565 ?
O9 Nb1 2.070(4) . ?
O9 Ru1 2.108(3) 9_565 ?
O12 Nb3 1.959(3) . ?
O12 Nb1 1.959(4) . ?
Na1 O11 2.456(4) 4_454 ?
Na1 Na2 3.354(4) . ?
Na1 Nb2 3.702(2) . ?
Na1 Nb1 3.704(2) 4_454 ?
Na2 O11 2.801(5) 4_454 ?
Nb1 Ru1 3.1637(6) 9_565 ?
Nb1 Nb2 3.2963(7) . ?
Nb1 Nb3 3.3217(7) . ?
Nb1 Na1 3.704(2) 3 ?
Nb2 O2 2.073(3) 9_565 ?
Nb2 Ru1 3.1755(6) . ?
Nb2 Nb3 3.3206(7) 9_565 ?
Nb3 O5 1.965(3) 9_565 ?
Nb3 O9 2.069(4) 9_565 ?
Nb3 Ru1 3.1731(7) . ?
Nb3 Nb2 3.3204(7) 9_565 ?
Ru1 O9 2.108(3) 9_565 ?
Ru1 O2 2.111(4) 9_565 ?
Ru1 Nb1 3.1636(6) 9_565 ?

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
C7 C2 C3 121.2(6) . . ?
C7 C2 Ru1 71.6(4) . . ?
C3 C2 Ru1 71.7(3) . . ?
C7 C2 H2A 118.8 . . ?
C3 C2 H2A 118.8 . . ?
Ru1 C2 H2A 118.8 . . ?
O4W C1M H1MA 109.5 . . ?
O4W C1M H1MB 109.5 . . ?
H1MA C1M H1MB 109.5 . . ?
O4W C1M H1MC 109.5 . . ?
H1MA C1M H1MC 109.5 . . ?
H1MB C1M H1MC 109.5 . . ?
C4 C3 C2 119.0(6) . . ?
C4 C3 Ru1 70.6(3) . . ?
C2 C3 Ru1 70.2(3) . . ?
C4 C3 H3A 119.8 . . ?
C2 C3 H3A 119.8 . . ?
Ru1 C3 H3A 119.8 . . ?
O2W C2M H2MA 109.5 . . ?
O2W C2M H2MB 109.5 . . ?
H2MA C2M H2MB 109.5 . . ?
O2W C2M H2MC 109.5 . . ?
H2MA C2M H2MC 109.5 . . ?
H2MB C2M H2MC 109.5 . . ?
C3 C4 C5 121.5(6) . . ?
C3 C4 Ru1 71.5(3) . . ?
C5 C4 Ru1 72.0(3) . . ?
C3 C4 H4A 118.6 . . ?
C5 C4 H4A 118.6 . . ?
Ru1 C4 H4A 118.6 . . ?
O3W C3M H3MA 109.5 . . ?
O3W C3M H3MB 109.5 . . ?
H3MA C3M H3MB 109.5 . . ?
O3W C3M H3MC 109.5 . . ?
H3MA C3M H3MC 109.5 . . ?
H3MB C3M H3MC 109.5 . . ?
C6 C5 C4 119.1(6) . . ?
C6 C5 Ru1 70.4(3) . . ?
C4 C5 Ru1 70.2(3) . . ?
C6 C5 H5A 119.7 . . ?
C4 C5 H5A 119.7 . . ?
Ru1 C5 H5A 119.7 . . ?
O5W C4M H4MA 109.5 . . ?
O5W C4M H4MB 109.5 . . ?
H4MA C4M H4MB 109.5 . . ?
O5W C4M H4MC 109.5 . . ?
H4MA C4M H4MC 109.5 . . ?
H4MB C4M H4MC 109.5 . . ?
C5 C6 C7 120.9(6) . . ?
C5 C6 Ru1 72.0(3) . . ?
C7 C6 Ru1 70.8(3) . . ?
C5 C6 H6A 118.9 . . ?
C7 C6 H6A 118.9 . . ?
Ru1 C6 H6A 118.9 . . ?
O8W C5M H5MA 109.5 . . ?
O8W C5M H5MB 109.5 . . ?
H5MA C5M H5MB 109.5 . . ?
O8W C5M H5MC 109.5 . . ?
H5MA C5M H5MC 109.5 . . ?
H5MB C5M H5MC 109.5 . . ?
C2 C7 C6 118.3(6) . . ?
C2 C7 Ru1 70.3(4) . . ?
C6 C7 Ru1 70.4(3) . . ?
C2 C7 H7A 120.2 . . ?
C6 C7 H7A 120.2 . . ?
Ru1 C7 H7A 120.2 . . ?
O7W C6M H6MA 109.5 . . ?
O7W C6M H6MB 109.5 . . ?
H6MA C6M H6MB 109.5 . . ?
O7W C6M H6MC 109.5 . . ?
H6MA C6M H6MC 109.5 . . ?
H6MB C6M H6MC 109.5 . . ?
Nb1 O2 Nb2 113.75(16) . 9_565 ?
Nb1 O2 Ru1 99.00(15) . 9_565 ?
Nb2 O2 Ru1 98.74(15) 9_565 9_565 ?
Nb2 O3 Nb2 180.0 9_565 . ?
Nb2 O3 Nb1 92.656(15) 9_565 . ?
Nb2 O3 Nb1 87.346(15) . . ?
Nb2 O3 Nb1 87.344(15) 9_565 9_565 ?
Nb2 O3 Nb1 92.654(15) . 9_565 ?
Nb1 O3 Nb1 180.0 . 9_565 ?
Nb2 O3 Nb3 87.472(16) 9_565 . ?
Nb2 O3 Nb3 92.528(16) . . ?
Nb1 O3 Nb3 86.980(16) . . ?
Nb1 O3 Nb3 93.019(16) 9_565 . ?
Nb2 O3 Nb3 92.527(16) 9_565 9_565 ?
Nb2 O3 Nb3 87.473(16) . 9_565 ?
Nb1 O3 Nb3 93.019(16) . 9_565 ?
Nb1 O3 Nb3 86.982(16) 9_565 9_565 ?
Nb3 O3 Nb3 180.0 . 9_565 ?
C2M O2W Na1 113.3(4) . . ?
Nb2 O4 Nb3 114.23(16) . . ?
Nb2 O4 Ru1 98.49(15) . . ?
Nb3 O4 Ru1 98.39(14) . . ?
C3M O3W Na1 141.7(4) . . ?
Nb2 O5 Nb3 116.25(18) . 9_565 ?
C1M O4W Na1 117.1(5) . . ?
C4M O5W Na1 119.4(5) . . ?
C4M O5W Na2 129.2(5) . . ?
Na1 O5W Na2 85.62(16) . . ?
Nb2 O7 Na2 143.2(2) . . ?
Nb2 O7 Na1 125.4(2) . . ?
Na2 O7 Na1 91.33(15) . . ?
Nb2 O8 Nb1 114.90(16) . . ?
C6M O7W Na2 127.4(6) . . ?
C5M O8W Na2 130.9(8) . . ?
C11M O11M C11M 156(6) 11_566 16_666 ?
C11M O11M C11M 92.5(13) 11_566 6_464 ?
C11M O11M C11M 92.5(13) 16_666 6_464 ?
C11M O11M C11M 92.5(13) 11_566 . ?
C11M O11M C11M 92.5(13) 16_666 . ?
C11M O11M C11M 156(6) 6_464 . ?
Nb1 O11 Na1 122.26(19) . 3 ?
Nb1 O11 Na2 116.59(17) . 3 ?
Na1 O11 Na2 78.98(12) 3 3 ?
Nb3 O9 Nb1 115.56(16) 9_565 . ?
Nb3 O9 Ru1 98.85(14) 9_565 9_565 ?
Nb1 O9 Ru1 98.44(15) . 9_565 ?
Nb3 O12 Nb1 115.94(18) . . ?
O3W Na1 O4W 93.12(17) . . ?
O3W Na1 O7 87.91(16) . . ?
O4W Na1 O7 178.34(17) . . ?
O3W Na1 O2W 93.20(17) . . ?
O4W Na1 O2W 92.39(17) . . ?
O7 Na1 O2W 88.85(15) . . ?
O3W Na1 O5W 94.66(18) . . ?
O4W Na1 O5W 99.95(18) . . ?
O7 Na1 O5W 78.66(16) . . ?
O2W Na1 O5W 164.96(19) . . ?
O3W Na1 O11 170.93(18) . 4_454 ?
O4W Na1 O11 92.47(15) . 4_454 ?
O7 Na1 O11 86.34(14) . 4_454 ?
O2W Na1 O11 93.69(15) . 4_454 ?
O5W Na1 O11 77.34(15) . 4_454 ?
O3W Na1 Na2 116.31(15) . . ?
O4W Na1 Na2 135.19(14) . . ?
O7 Na1 Na2 43.16(10) . . ?
O2W Na1 Na2 117.04(14) . . ?
O5W Na1 Na2 47.92(13) . . ?
O11 Na1 Na2 55.06(11) 4_454 . ?
O3W Na1 Nb2 73.48(12) . . ?
O4W Na1 Nb2 158.87(13) . . ?
O7 Na1 Nb2 22.80(9) . . ?
O2W Na1 Nb2 72.60(11) . . ?
O5W Na1 Nb2 97.42(13) . . ?
O11 Na1 Nb2 103.05(11) 4_454 . ?
Na2 Na1 Nb2 65.93(6) . . ?
O3W Na1 Nb1 155.67(13) . 4_454 ?
O4W Na1 Nb1 72.56(11) . 4_454 ?
O7 Na1 Nb1 106.03(11) . 4_454 ?
O2W Na1 Nb1 106.65(11) . 4_454 ?
O5W Na1 Nb1 69.49(11) . 4_454 ?
O11 Na1 Nb1 23.64(9) 4_454 4_454 ?
Na2 Na1 Nb1 67.18(6) . 4_454 ?
Nb2 Na1 Nb1 125.38(6) . 4_454 ?
O7 Na2 O7W 131.8(2) . . ?
O7 Na2 O8W 136.5(2) . . ?
O7W Na2 O8W 90.9(2) . . ?
O7 Na2 O5W 79.34(16) . . ?
O7W Na2 O5W 127.8(2) . . ?
O8W Na2 O5W 79.5(2) . . ?
O7 Na2 O6W 81.94(17) . . ?
O7W Na2 O6W 82.75(19) . . ?
O8W Na2 O6W 98.0(2) . . ?
O5W Na2 O6W 149.15(19) . . ?
O7 Na2 O11 80.59(14) . 4_454 ?
O7W Na2 O11 75.27(17) . 4_454 ?
O8W Na2 O11 126.0(2) . 4_454 ?
O5W Na2 O11 70.26(15) . 4_454 ?
O6W Na2 O11 130.17(18) . 4_454 ?
O7 Na2 Na1 45.51(11) . . ?
O7W Na2 Na1 120.78(17) . . ?
O8W Na2 Na1 125.9(2) . . ?
O5W Na2 Na1 46.47(12) . . ?
O6W Na2 Na1 126.26(15) . . ?
O11 Na2 Na1 45.96(10) 4_454 . ?
O11 Nb1 O12 102.86(17) . . ?
O11 Nb1 O8 101.04(15) . . ?
O12 Nb1 O8 90.36(15) . . ?
O11 Nb1 O2 103.99(15) . . ?
O12 Nb1 O2 89.84(14) . . ?
O8 Nb1 O2 154.27(14) . . ?
O11 Nb1 O9 102.53(16) . . ?
O12 Nb1 O9 154.13(14) . . ?
O8 Nb1 O9 89.63(15) . . ?
O2 Nb1 O9 79.27(14) . . ?
O11 Nb1 O3 178.18(13) . . ?
O12 Nb1 O3 78.90(10) . . ?
O8 Nb1 O3 78.38(10) . . ?
O2 Nb1 O3 76.42(10) . . ?
O9 Nb1 O3 75.77(9) . . ?
O11 Nb1 Ru1 94.90(12) . 9_565 ?
O12 Nb1 Ru1 130.91(10) . 9_565 ?
O8 Nb1 Ru1 130.73(11) . 9_565 ?
O2 Nb1 Ru1 41.22(10) . 9_565 ?
O9 Nb1 Ru1 41.24(10) . 9_565 ?
O3 Nb1 Ru1 84.241(15) . 9_565 ?
O11 Nb1 Nb2 133.36(12) . . ?
O12 Nb1 Nb2 84.43(10) . . ?
O8 Nb1 Nb2 32.35(10) . . ?
O2 Nb1 Nb2 122.23(10) . . ?
O9 Nb1 Nb2 81.80(10) . . ?
O3 Nb1 Nb2 46.030(11) . . ?
Ru1 Nb1 Nb2 114.956(19) 9_565 . ?
O11 Nb1 Nb3 134.87(13) . . ?
O12 Nb1 Nb3 32.02(10) . . ?
O8 Nb1 Nb3 83.80(10) . . ?
O2 Nb1 Nb3 82.81(10) . . ?
O9 Nb1 Nb3 122.46(10) . . ?
O3 Nb1 Nb3 46.875(12) . . ?
Ru1 Nb1 Nb3 115.823(17) 9_565 . ?
Nb2 Nb1 Nb3 63.251(14) . . ?
O11 Nb1 Na1 34.11(13) . 3 ?
O12 Nb1 Na1 124.58(11) . 3 ?
O8 Nb1 Na1 75.34(10) . 3 ?
O2 Nb1 Na1 124.54(10) . 3 ?
O9 Nb1 Na1 80.30(10) . 3 ?
O3 Nb1 Na1 144.30(4) . 3 ?
Ru1 Nb1 Na1 94.93(4) 9_565 3 ?
Nb2 Nb1 Na1 104.85(4) . 3 ?
Nb3 Nb1 Na1 149.24(4) . 3 ?
O7 Nb2 O8 104.21(15) . . ?
O7 Nb2 O5 102.86(17) . . ?
O8 Nb2 O5 91.28(15) . . ?
O7 Nb2 O4 100.87(16) . . ?
O8 Nb2 O4 89.43(15) . . ?
O5 Nb2 O4 155.31(14) . . ?
O7 Nb2 O2 99.69(15) . 9_565 ?
O8 Nb2 O2 155.23(14) . 9_565 ?
O5 Nb2 O2 89.68(15) . 9_565 ?
O4 Nb2 O2 79.68(14) . 9_565 ?
O7 Nb2 O3 175.85(12) . . ?
O8 Nb2 O3 79.37(10) . . ?
O5 Nb2 O3 78.97(10) . . ?
O4 Nb2 O3 76.91(9) . . ?
O2 Nb2 O3 76.53(9) 9_565 . ?
O7 Nb2 Ru1 91.68(12) . . ?
O8 Nb2 Ru1 130.73(11) . . ?
O5 Nb2 Ru1 130.61(10) . . ?
O4 Nb2 Ru1 41.46(10) . . ?
O2 Nb2 Ru1 41.07(10) 9_565 . ?
O3 Nb2 Ru1 84.349(15) . . ?
O7 Nb2 Nb1 136.94(12) . . ?
O8 Nb2 Nb1 32.75(10) . . ?
O5 Nb2 Nb1 84.69(10) . . ?
O4 Nb2 Nb1 82.63(10) . . ?
O2 Nb2 Nb1 122.93(10) 9_565 . ?
O3 Nb2 Nb1 46.624(11) . . ?
Ru1 Nb2 Nb1 115.538(18) . . ?
O7 Nb2 Nb3 134.82(13) . 9_565 ?
O8 Nb2 Nb3 85.25(10) . 9_565 ?
O5 Nb2 Nb3 32.05(10) . 9_565 ?
O4 Nb2 Nb3 123.62(10) . 9_565 ?
O2 Nb2 Nb3 82.51(10) 9_565 9_565 ?
O3 Nb2 Nb3 46.923(12) . 9_565 ?
Ru1 Nb2 Nb3 115.528(17) . 9_565 ?
Nb1 Nb2 Nb3 63.899(15) . 9_565 ?
O7 Nb2 Na1 31.80(13) . . ?
O8 Nb2 Na1 123.04(11) . . ?
O5 Nb2 Na1 77.08(11) . . ?
O4 Nb2 Na1 122.43(10) . . ?
O2 Nb2 Na1 81.25(10) 9_565 . ?
O3 Nb2 Na1 147.21(4) . . ?
Ru1 Nb2 Na1 94.52(4) . . ?
Nb1 Nb2 Na1 149.82(4) . . ?
Nb3 Nb2 Na1 106.74(4) 9_565 . ?
O6 Nb3 O12 105.40(17) . . ?
O6 Nb3 O5 103.95(17) . 9_565 ?
O12 Nb3 O5 89.81(14) . 9_565 ?
O6 Nb3 O4 102.65(16) . . ?
O12 Nb3 O4 89.84(14) . . ?
O5 Nb3 O4 152.49(15) 9_565 . ?
O6 Nb3 O9 101.19(16) . 9_565 ?
O12 Nb3 O9 152.90(15) . 9_565 ?
O5 Nb3 O9 88.82(14) 9_565 9_565 ?
O4 Nb3 O9 79.23(14) . 9_565 ?
O6 Nb3 O3 176.14(13) . . ?
O12 Nb3 O3 78.18(11) . . ?
O5 Nb3 O3 77.30(11) 9_565 . ?
O4 Nb3 O3 75.71(10) . . ?
O9 Nb3 O3 75.12(10) 9_565 . ?
O6 Nb3 Ru1 92.89(13) . . ?
O12 Nb3 Ru1 131.10(10) . . ?
O5 Nb3 Ru1 129.64(11) 9_565 . ?
O4 Nb3 Ru1 41.51(10) . . ?
O9 Nb3 Ru1 41.03(9) 9_565 . ?
O3 Nb3 Ru1 83.576(17) . . ?
O6 Nb3 Nb2 135.56(13) . 9_565 ?
O12 Nb3 Nb2 83.52(10) . 9_565 ?
O5 Nb3 Nb2 31.70(11) 9_565 9_565 ?
O4 Nb3 Nb2 121.11(10) . 9_565 ?
O9 Nb3 Nb2 81.19(10) 9_565 9_565 ?
O3 Nb3 Nb2 45.605(11) . 9_565 ?
Ru1 Nb3 Nb2 114.025(19) . 9_565 ?
O6 Nb3 Nb1 137.41(13) . . ?
O12 Nb3 Nb1 32.04(11) . . ?
O5 Nb3 Nb1 83.24(10) 9_565 . ?
O4 Nb3 Nb1 81.98(10) . . ?
O9 Nb3 Nb1 121.09(10) 9_565 . ?
O3 Nb3 Nb1 46.145(11) . . ?
Ru1 Nb3 Nb1 114.893(18) . . ?
Nb2 Nb3 Nb1 62.640(14) 9_565 . ?
O9 Ru1 O2 77.04(14) 9_565 9_565 ?
O9 Ru1 O4 77.05(13) 9_565 . ?
O2 Ru1 O4 77.51(14) 9_565 . ?
O9 Ru1 C2 94.8(2) 9_565 . ?
O2 Ru1 C2 150.6(2) 9_565 . ?
O4 Ru1 C2 128.7(2) . . ?
O9 Ru1 C4 128.12(18) 9_565 . ?
O2 Ru1 C4 94.12(19) 9_565 . ?
O4 Ru1 C4 151.50(19) . . ?
C2 Ru1 C4 68.6(2) . . ?
O9 Ru1 C6 152.4(2) 9_565 . ?
O2 Ru1 C6 127.8(2) 9_565 . ?
O4 Ru1 C6 95.33(18) . . ?
C2 Ru1 C6 69.1(2) . . ?
C4 Ru1 C6 68.1(2) . . ?
O9 Ru1 C7 115.7(2) 9_565 . ?
O2 Ru1 C7 166.5(2) 9_565 . ?
O4 Ru1 C7 100.4(2) . . ?
C2 Ru1 C7 38.1(3) . . ?
C4 Ru1 C7 81.4(3) . . ?
C6 Ru1 C7 38.8(3) . . ?
O9 Ru1 C3 99.95(18) 9_565 . ?
O2 Ru1 C3 114.7(2) 9_565 . ?
O4 Ru1 C3 166.7(2) . . ?
C2 Ru1 C3 38.1(3) . . ?
C4 Ru1 C3 37.9(2) . . ?
C6 Ru1 C3 81.3(2) . . ?
C7 Ru1 C3 69.0(3) . . ?
O9 Ru1 C5 165.82(19) 9_565 . ?
O2 Ru1 C5 99.6(2) 9_565 . ?
O4 Ru1 C5 115.98(18) . . ?
C2 Ru1 C5 81.4(2) . . ?
C4 Ru1 C5 37.9(2) . . ?
C6 Ru1 C5 37.6(2) . . ?
C7 Ru1 C5 69.1(3) . . ?
C3 Ru1 C5 68.7(2) . . ?
O9 Ru1 Nb1 40.33(10) 9_565 9_565 ?
O2 Ru1 Nb1 39.78(9) 9_565 9_565 ?
O4 Ru1 Nb1 85.59(9) . 9_565 ?
C2 Ru1 Nb1 120.07(19) . 9_565 ?
C4 Ru1 Nb1 105.46(16) . 9_565 ?
C6 Ru1 Nb1 167.00(19) . 9_565 ?
C7 Ru1 Nb1 153.7(2) . 9_565 ?
C3 Ru1 Nb1 100.56(16) . 9_565 ?
C5 Ru1 Nb1 131.12(18) . 9_565 ?
O9 Ru1 Nb3 40.12(10) 9_565 . ?
O2 Ru1 Nb3 85.82(9) 9_565 . ?
O4 Ru1 Nb3 40.11(9) . . ?
C2 Ru1 Nb3 106.18(18) . . ?
C4 Ru1 Nb3 167.88(16) . . ?
C6 Ru1 Nb3 121.10(18) . . ?
C7 Ru1 Nb3 101.20(19) . . ?
C3 Ru1 Nb3 131.95(17) . . ?
C5 Ru1 Nb3 154.03(17) . . ?
Nb1 Ru1 Nb3 67.089(15) 9_565 . ?
O9 Ru1 Nb2 84.60(9) 9_565 . ?
O2 Ru1 Nb2 40.19(9) 9_565 . ?
O4 Ru1 Nb2 40.06(10) . . ?
C2 Ru1 Nb2 168.6(2) . . ?
C4 Ru1 Nb2 120.53(17) . . ?
C6 Ru1 Nb2 106.76(16) . . ?
C7 Ru1 Nb2 132.72(19) . . ?
C3 Ru1 Nb2 153.18(19) . . ?
C5 Ru1 Nb2 101.81(16) . . ?
Nb1 Ru1 Nb2 66.003(14) 9_565 . ?
Nb3 Ru1 Nb2 66.271(15) . . ?

_refine_diff_density_max         1.979
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.149

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeOH'
####################################################################### 
# 
# 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_18
_database_code_depnum_ccdc_archive 'CCDC 1423581'
_audit_update_record             
;
2015-09-11 deposited with the CCDC.
2016-01-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT043_18                  
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      24.15 Check
RESPONSE: H-atoms of the solvate water and MeOH molecules were not localized
;

# Added during the CSD deposition process: Friday 11th of September 2015 08:10:04 AM
# end Validation Reply Form

#complex 2
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_structural     K4[{C10H15Ir}2Nb6O19]*10CH3OH*4H2O
_chemical_formula_sum            'C30 H78 Ir2 K4 Nb6 O33'
_chemical_formula_weight         2065.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   10.7760(6)
_cell_length_b                   11.8756(7)
_cell_length_c                   14.1839(9)
_cell_angle_alpha                113.102(3)
_cell_angle_beta                 92.519(3)
_cell_angle_gamma                111.051(2)
_cell_volume                     1521.58(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6620
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      27.57

_exptl_crystal_description       yellow
_exptl_crystal_colour            plate
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.254
_exptl_crystal_F_000             998
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    5.800
_shelx_estimated_absorpt_T_min   0.477
_shelx_estimated_absorpt_T_max   0.722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_T_max  0.722
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean 25
_diffrn_reflns_number            18012
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.598
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             6901
_reflns_number_gt                5935
_reflns_threshold_expression     >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       'APEX2 (Bruker-AXS, 2004)'
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXLE (Sheldrick, 2011)'
_computing_publication_material  'CIFTAB-97 (Sheldrick, 1998)'
_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)+(0.0764P)²] 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         6901
_refine_ls_number_parameters     344
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.1341
_refine_ls_wR_factor_gt          0.0942
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.156
_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
C1 C 0.3736(8) 0.0031(8) 0.0819(6) 0.0157(12) Uani 1 1 d . U . . .
H1A H 0.4549 0.0388 0.0563 0.024 Uiso 1 1 calc R U . . .
H1B H 0.4012 0.0111 0.1519 0.024 Uiso 1 1 calc R U . . .
H1C H 0.3201 -0.0915 0.0337 0.024 Uiso 1 1 calc R U . . .
C2 C 0.2891(8) 0.0811(8) 0.0880(6) 0.0149(12) Uani 1 1 d . U . . .
C3 C 0.1633(8) 0.0568(7) 0.1222(6) 0.0137(12) Uani 1 1 d . U . . .
C5 C 0.1130(7) 0.1534(7) 0.1165(6) 0.0099(14) Uani 1 1 d . . . . .
C6 C 0.2118(8) 0.2381(7) 0.0800(6) 0.0135(16) Uani 1 1 d . . . . .
C7 C -0.0131(8) 0.1648(9) 0.1503(6) 0.0208(19) Uani 1 1 d . . . . .
H7A H -0.0596 0.0932 0.1709 0.031 Uiso 1 1 calc R U . . .
H7B H 0.0114 0.2522 0.2102 0.031 Uiso 1 1 calc R U . . .
H7C H -0.0737 0.1565 0.0921 0.031 Uiso 1 1 calc R U . . .
C8 C 0.2022(9) 0.3521(8) 0.0635(7) 0.0210(18) Uani 1 1 d . . . . .
H8A H 0.2820 0.3929 0.0386 0.032 Uiso 1 1 calc R U . . .
H8B H 0.1193 0.3185 0.0112 0.032 Uiso 1 1 calc R U . . .
H8C H 0.1990 0.4195 0.1300 0.032 Uiso 1 1 calc R U . . .
C9 C 0.3211(7) 0.1938(8) 0.0614(6) 0.0122(15) Uani 1 1 d . . . . .
C10 C 0.4430(9) 0.2478(10) 0.0207(7) 0.0239(19) Uani 1 1 d . . . . .
H10A H 0.4991 0.1975 0.0165 0.036 Uiso 1 1 calc R U . . .
H10B H 0.4137 0.2386 -0.0493 0.036 Uiso 1 1 calc R U . . .
H10C H 0.4964 0.3428 0.0682 0.036 Uiso 1 1 calc R U . . .
C11 C 0.0926(8) -0.0535(7) 0.1509(6) 0.0147(12) Uani 1 1 d . U . . .
H11A H 0.0086 -0.0481 0.1716 0.022 Uiso 1 1 calc R U . . .
H11B H 0.0704 -0.1399 0.0905 0.022 Uiso 1 1 calc R U . . .
H11C H 0.1521 -0.0455 0.2097 0.022 Uiso 1 1 calc R U . . .
C12 C 0.3169(9) 0.2878(9) 0.7750(7) 0.025(2) Uani 1 1 d . . . . .
H12A H 0.2771 0.3534 0.8036 0.037 Uiso 1 1 calc R U . . .
H12B H 0.3061 0.2363 0.8160 0.037 Uiso 1 1 calc R U . . .
H12C H 0.4139 0.3348 0.7787 0.037 Uiso 1 1 calc R U . . .
C13 C 0.3095(9) -0.1112(9) 0.7175(7) 0.0215(18) Uani 1 1 d . . . . .
H5 H 0.244(10) -0.139(9) 0.764(8) 0.026 Uiso 1 1 d . U . . .
H6 H 0.408(10) -0.051(9) 0.739(7) 0.026 Uiso 1 1 d . U . . .
H4 H 0.287(10) -0.015(9) 0.745(7) 0.026 Uiso 1 1 d . U . . .
C14 C 0.8096(10) 0.3878(10) 0.0184(7) 0.028(2) Uani 1 1 d . . . . .
O1 O 0.2490(5) 0.3318(5) 0.3678(4) 0.0055(10) Uani 1 1 d . . . . .
O2 O 0.4494(5) 0.4624(5) 0.2964(4) 0.0078(10) Uani 1 1 d . . . . .
O3 O 0.4595(5) 0.2638(5) 0.3312(4) 0.0069(10) Uani 1 1 d . . . . .
O4 O 0.7101(5) 0.6392(5) 0.4288(4) 0.0071(10) Uani 1 1 d . . . . .
O5 O 0.6946(5) 0.3977(5) 0.2520(4) 0.0093(10) Uani 1 1 d . . . . .
O6 O 0.5000 0.5000 0.5000 0.0053(13) Uiso 1 2 d S . P . .
O7 O 0.2202(5) 0.5484(5) 0.3248(4) 0.0099(10) Uani 1 1 d . . . . .
O8 O 0.2842(5) 0.5719(5) 0.5349(4) 0.0068(10) Uani 1 1 d . . . . .
O9 O 0.2421(5) 0.1012(5) 0.4065(4) 0.0106(11) Uani 1 1 d . . . . .
O10 O 0.4905(5) 0.7091(5) 0.4608(4) 0.0082(10) Uani 1 1 d . . . . .
O11 O -0.0412(5) 0.4350(5) 0.3566(4) 0.0127(11) Uani 1 1 d . . . . .
O12 O 0.2507(6) 0.2011(5) 0.6709(4) 0.0172(12) Uani 1 1 d . . . . .
O13 O 0.2529(5) -0.1908(5) 0.6084(4) 0.0152(12) Uani 1 1 d . . . . .
O14 O 0.0359(6) -0.0502(6) 0.6086(5) 0.0242(14) Uani 1 1 d . . . . .
O15 O 0.5547(6) 0.1309(5) 0.6201(4) 0.0172(12) Uani 1 1 d . . . . .
C15 C -0.0139(9) 0.3079(9) 0.7254(7) 0.0230(19) Uani 1 1 d . . . . .
H15A H 0.0362 0.4057 0.7603 0.035 Uiso 1 1 calc R U . . .
H15B H -0.0644 0.2779 0.7730 0.035 Uiso 1 1 calc R U . . .
H15C H 0.0503 0.2659 0.7065 0.035 Uiso 1 1 calc R U . . .
O16 O -0.1073(5) 0.2704(5) 0.6325(4) 0.0148(11) Uani 1 1 d . . . . .
C16 C 0.6119(9) 0.1875(9) 0.7291(7) 0.0229(19) Uani 1 1 d . . . . .
H16A H 0.7103 0.2392 0.7423 0.034 Uiso 1 1 calc R U . . .
H16B H 0.5700 0.2469 0.7692 0.034 Uiso 1 1 calc R U . . .
H16C H 0.5948 0.1155 0.7509 0.034 Uiso 1 1 calc R U . . .
O17 O 0.8163(7) 0.3270(6) 0.0873(5) 0.0247(14) Uani 1 1 d . . . . .
K1 K 0.02590(15) 0.32423(16) 0.47579(13) 0.0107(3) Uani 1 1 d . . . . .
K2 K 0.28654(17) -0.02846(16) 0.51320(13) 0.0142(3) Uani 1 1 d . . . . .
Nb1 Nb 0.34060(6) 0.53053(6) 0.40010(5) 0.00503(14) Uani 1 1 d . . . . .
Nb3 Nb 0.61265(6) 0.44375(6) 0.35673(5) 0.00519(14) Uani 1 1 d . . . . .
Nb4 Nb 0.35459(6) 0.26874(6) 0.44599(5) 0.00513(14) Uani 1 1 d . . . . .
Ir1 Ir 0.30904(3) 0.25583(3) 0.22260(2) 0.00611(10) Uani 1 1 d . . . . .


_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
C1 C2 1.498(10) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.430(11) . ?
C2 C9 1.460(11) . ?
C2 Ir1 2.129(8) . ?
C3 C5 1.460(11) . ?
C3 C11 1.480(11) . ?
C3 Ir1 2.139(7) . ?
C5 C6 1.449(11) . ?
C5 C7 1.495(11) . ?
C5 Ir1 2.155(7) . ?
C6 C9 1.448(11) . ?
C6 C8 1.498(11) . ?
C6 Ir1 2.134(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.491(11) . ?
C9 Ir1 2.135(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 O12 1.391(10) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 O13 1.419(10) . ?
C13 K2 3.431(9) . ?
C13 H5 1.04(10) . ?
C13 H6 1.00(10) . ?
C13 H4 1.17(10) . ?
C14 O17 1.437(11) . ?
O1 Nb1 2.048(5) . ?
O1 Nb4 2.058(5) . ?
O1 Ir1 2.133(5) . ?
O1 K1 2.900(5) . ?
O2 Nb1 2.023(5) . ?
O2 Nb3 2.043(5) . ?
O2 Ir1 2.141(5) . ?
O3 Nb4 2.016(5) . ?
O3 Nb3 2.056(5) . ?
O3 Ir1 2.137(5) . ?
O4 Nb3 1.957(5) . ?
O4 Nb4 1.993(5) 2_666 ?
O4 K1 2.903(5) 2_666 ?
O5 Nb3 1.763(5) . ?
O6 Nb1 2.3930(6) 2_666 ?
O6 Nb1 2.3930(6) . ?
O6 Nb4 2.3951(6) . ?
O6 Nb4 2.3951(6) 2_666 ?
O6 Nb3 2.4050(6) . ?
O6 Nb3 2.4050(6) 2_666 ?
O7 Nb1 1.767(5) . ?
O8 Nb1 1.961(5) . ?
O8 Nb3 1.964(5) 2_666 ?
O8 K1 3.013(5) . ?
O9 Nb4 1.754(5) . ?
O9 K2 2.680(5) . ?
O10 Nb4 1.954(5) 2_666 ?
O10 Nb1 1.958(5) . ?
O11 K1 2.725(6) . ?
O11 K1 2.855(6) 2_566 ?
O12 K2 2.938(6) . ?
O13 K2 2.694(6) . ?
O13 K1 2.783(5) 2_556 ?
O14 K1 2.789(6) 2_556 ?
O14 K2 3.047(6) . ?
O15 C16 1.423(10) . ?
O15 K2 2.769(6) . ?
O15 K2 2.821(6) 2_656 ?
C15 O16 1.430(10) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O16 K2 2.694(5) 2_556 ?
O16 K1 2.854(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
K1 O13 2.783(5) 2_556 ?
K1 O14 2.789(6) 2_556 ?
K1 O11 2.855(6) 2_566 ?
K1 O4 2.903(5) 2_666 ?
K1 Nb3 3.8401(16) 2_666 ?
K1 Nb4 3.8403(17) . ?
K1 Nb1 3.8820(17) . ?
K1 K2 3.960(2) 2_556 ?
K2 O16 2.694(5) 2_556 ?
K2 O15 2.821(6) 2_656 ?
K2 Nb4 3.8400(17) . ?
K2 K1 3.960(2) 2_556 ?
K2 K2 4.458(3) 2_656 ?
Nb1 Ir1 3.1270(7) . ?
Nb1 Nb4 3.3013(8) 2_666 ?
Nb1 Nb3 3.3398(9) 2_666 ?
Nb3 O8 1.964(5) 2_666 ?
Nb3 Ir1 3.1905(7) . ?
Nb3 Nb1 3.3397(9) 2_666 ?
Nb3 Nb4 3.3410(9) 2_666 ?
Nb3 K1 3.8401(17) 2_666 ?
Nb4 O10 1.954(5) 2_666 ?
Nb4 O4 1.993(5) 2_666 ?
Nb4 Ir1 3.1196(7) . ?
Nb4 Nb1 3.3013(8) 2_666 ?
Nb4 Nb3 3.3411(9) 2_666 ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C9 108.9(6) . . ?
C3 C2 C1 124.9(7) . . ?
C9 C2 C1 126.2(7) . . ?
C3 C2 Ir1 70.8(4) . . ?
C9 C2 Ir1 70.2(4) . . ?
C1 C2 Ir1 124.6(5) . . ?
C2 C3 C5 108.0(7) . . ?
C2 C3 C11 125.4(7) . . ?
C5 C3 C11 126.4(7) . . ?
C2 C3 Ir1 70.0(4) . . ?
C5 C3 Ir1 70.7(4) . . ?
C11 C3 Ir1 128.1(5) . . ?
C6 C5 C3 107.4(7) . . ?
C6 C5 C7 128.0(7) . . ?
C3 C5 C7 124.4(7) . . ?
C6 C5 Ir1 69.5(4) . . ?
C3 C5 Ir1 69.5(4) . . ?
C7 C5 Ir1 123.0(5) . . ?
C5 C6 C9 108.7(7) . . ?
C5 C6 C8 125.7(7) . . ?
C9 C6 C8 125.6(7) . . ?
C5 C6 Ir1 71.0(4) . . ?
C9 C6 Ir1 70.2(4) . . ?
C8 C6 Ir1 125.0(5) . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 C2 107.0(6) . . ?
C6 C9 C10 128.1(8) . . ?
C2 C9 C10 124.9(7) . . ?
C6 C9 Ir1 70.1(4) . . ?
C2 C9 Ir1 69.7(4) . . ?
C10 C9 Ir1 126.2(5) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O12 C12 H12A 109.5 . . ?
O12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O12 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O13 C13 K2 47.9(4) . . ?
O13 C13 H5 113(5) . . ?
K2 C13 H5 136(5) . . ?
O13 C13 H6 118(6) . . ?
K2 C13 H6 89(6) . . ?
H5 C13 H6 128(8) . . ?
O13 C13 H4 109(5) . . ?
K2 C13 H4 70(5) . . ?
H5 C13 H4 86(7) . . ?
H6 C13 H4 88(7) . . ?
Nb1 O1 Nb4 115.3(2) . . ?
Nb1 O1 Ir1 96.8(2) . . ?
Nb4 O1 Ir1 96.18(19) . . ?
Nb1 O1 K1 101.97(18) . . ?
Nb4 O1 K1 100.13(18) . . ?
Ir1 O1 K1 146.8(2) . . ?
Nb1 O2 Nb3 115.8(2) . . ?
Nb1 O2 Ir1 97.3(2) . . ?
Nb3 O2 Ir1 99.4(2) . . ?
Nb4 O3 Nb3 115.6(2) . . ?
Nb4 O3 Ir1 97.4(2) . . ?
Nb3 O3 Ir1 99.1(2) . . ?
Nb3 O4 Nb4 115.6(2) . 2_666 ?
Nb3 O4 K1 102.67(19) . 2_666 ?
Nb4 O4 K1 101.73(18) 2_666 2_666 ?
Nb1 O6 Nb1 180.0 2_666 . ?
Nb1 O6 Nb4 87.18(2) 2_666 . ?
Nb1 O6 Nb4 92.82(2) . . ?
Nb1 O6 Nb4 92.82(2) 2_666 2_666 ?
Nb1 O6 Nb4 87.17(2) . 2_666 ?
Nb4 O6 Nb4 180.0 . 2_666 ?
Nb1 O6 Nb3 88.22(2) 2_666 . ?
Nb1 O6 Nb3 91.77(2) . . ?
Nb4 O6 Nb3 91.78(2) . . ?
Nb4 O6 Nb3 88.22(2) 2_666 . ?
Nb1 O6 Nb3 91.78(2) 2_666 2_666 ?
Nb1 O6 Nb3 88.23(2) . 2_666 ?
Nb4 O6 Nb3 88.22(2) . 2_666 ?
Nb4 O6 Nb3 91.78(2) 2_666 2_666 ?
Nb3 O6 Nb3 180.0 . 2_666 ?
Nb1 O8 Nb3 116.6(2) . 2_666 ?
Nb1 O8 K1 100.45(19) . . ?
Nb3 O8 K1 98.81(18) 2_666 . ?
Nb4 O9 K2 118.5(2) . . ?
Nb4 O10 Nb1 115.1(2) 2_666 . ?
K1 O11 K1 97.73(17) . 2_566 ?
C12 O12 K2 132.3(5) . . ?
C13 O13 K2 109.1(5) . . ?
C13 O13 K1 123.3(5) . 2_556 ?
K2 O13 K1 92.60(16) . 2_556 ?
K1 O14 K2 85.33(16) 2_556 . ?
C16 O15 K2 129.3(5) . . ?
C16 O15 K2 114.4(5) . 2_656 ?
K2 O15 K2 105.81(19) . 2_656 ?
O16 C15 H15A 109.5 . . ?
O16 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O16 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C15 O16 K2 131.4(5) . 2_556 ?
C15 O16 K1 112.9(5) . . ?
K2 O16 K1 91.02(17) 2_556 . ?
O15 C16 H16A 109.5 . . ?
O15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O11 K1 O13 71.40(16) . 2_556 ?
O11 K1 O14 121.15(18) . 2_556 ?
O13 K1 O14 73.26(16) 2_556 2_556 ?
O11 K1 O16 126.77(16) . . ?
O13 K1 O16 71.94(16) 2_556 . ?
O14 K1 O16 82.24(18) 2_556 . ?
O11 K1 O11 82.27(17) . 2_566 ?
O13 K1 O11 101.22(16) 2_556 2_566 ?
O14 K1 O11 150.45(18) 2_556 2_566 ?
O16 K1 O11 68.65(15) . 2_566 ?
O11 K1 O1 83.94(15) . . ?
O13 K1 O1 128.80(16) 2_556 . ?
O14 K1 O1 83.33(16) 2_556 . ?
O16 K1 O1 149.15(15) . . ?
O11 K1 O1 119.44(15) 2_566 . ?
O11 K1 O4 130.72(16) . 2_666 ?
O13 K1 O4 156.19(16) 2_556 2_666 ?
O14 K1 O4 85.60(16) 2_556 2_666 ?
O16 K1 O4 94.87(15) . 2_666 ?
O11 K1 O4 91.73(15) 2_566 2_666 ?
O1 K1 O4 56.88(14) . 2_666 ?
O11 K1 O8 78.49(15) . . ?
O13 K1 O8 147.98(15) 2_556 . ?
O14 K1 O8 134.11(16) 2_556 . ?
O16 K1 O8 121.00(15) . . ?
O11 K1 O8 63.42(14) 2_566 . ?
O1 K1 O8 56.07(14) . . ?
O4 K1 O8 55.82(14) 2_666 . ?
O11 K1 Nb3 108.76(12) . 2_666 ?
O13 K1 Nb3 167.41(13) 2_556 2_666 ?
O14 K1 Nb3 115.38(13) 2_556 2_666 ?
O16 K1 Nb3 99.42(11) . 2_666 ?
O11 K1 Nb3 66.65(11) 2_566 2_666 ?
O1 K1 Nb3 63.02(10) . 2_666 ?
O4 K1 Nb3 29.81(10) 2_666 2_666 ?
O8 K1 Nb3 30.35(9) . 2_666 ?
O11 K1 Nb4 115.62(12) . . ?
O13 K1 Nb4 140.35(13) 2_556 . ?
O14 K1 Nb4 70.38(12) 2_556 . ?
O16 K1 Nb4 117.32(11) . . ?
O11 K1 Nb4 118.22(11) 2_566 . ?
O1 K1 Nb4 31.84(9) . . ?
O4 K1 Nb4 30.53(10) 2_666 . ?
O8 K1 Nb4 63.81(9) . . ?
Nb3 K1 Nb4 51.57(2) 2_666 . ?
O11 K1 Nb1 67.70(12) . . ?
O13 K1 Nb1 135.44(13) 2_556 . ?
O14 K1 Nb1 114.38(14) 2_556 . ?
O16 K1 Nb1 149.87(12) . . ?
O11 K1 Nb1 90.22(11) 2_566 . ?
O1 K1 Nb1 31.07(10) . . ?
O4 K1 Nb1 63.44(10) 2_666 . ?
O8 K1 Nb1 29.79(10) . . ?
Nb3 K1 Nb1 51.25(2) 2_666 . ?
Nb4 K1 Nb1 53.37(2) . . ?
O11 K1 K2 114.21(12) . 2_556 ?
O13 K1 K2 42.81(11) 2_556 2_556 ?
O14 K1 K2 50.08(13) 2_556 2_556 ?
O16 K1 K2 42.87(11) . 2_556 ?
O11 K1 K2 105.97(12) 2_566 2_556 ?
O1 K1 K2 133.23(11) . 2_556 ?
O4 K1 K2 114.45(11) 2_666 2_556 ?
O8 K1 K2 163.20(11) . 2_556 ?
Nb3 K1 K2 134.96(5) 2_666 2_556 ?
Nb4 K1 K2 115.86(5) . 2_556 ?
Nb1 K1 K2 163.80(5) . 2_556 ?
O9 K2 O16 93.37(16) . 2_556 ?
O9 K2 O13 163.58(17) . . ?
O16 K2 O13 75.83(17) 2_556 . ?
O9 K2 O15 102.50(16) . . ?
O16 K2 O15 146.54(17) 2_556 . ?
O13 K2 O15 93.11(16) . . ?
O9 K2 O15 93.74(17) . 2_656 ?
O16 K2 O15 75.56(17) 2_556 2_656 ?
O13 K2 O15 95.43(17) . 2_656 ?
O15 K2 O15 74.19(19) . 2_656 ?
O9 K2 O12 75.54(16) . . ?
O16 K2 O12 132.32(17) 2_556 . ?
O13 K2 O12 102.40(17) . . ?
O15 K2 O12 80.60(17) . . ?
O15 K2 O12 149.78(17) 2_656 . ?
O9 K2 O14 95.80(17) . . ?
O16 K2 O14 80.30(17) 2_556 . ?
O13 K2 O14 70.47(17) . . ?
O15 K2 O14 126.18(18) . . ?
O15 K2 O14 154.49(17) 2_656 . ?
O12 K2 O14 55.73(16) . . ?
O9 K2 C13 158.9(2) . . ?
O16 K2 C13 98.3(2) 2_556 . ?
O13 K2 C13 23.02(19) . . ?
O15 K2 C13 76.93(19) . . ?
O15 K2 C13 106.2(2) 2_656 . ?
O12 K2 C13 83.62(19) . . ?
O14 K2 C13 69.1(2) . . ?
O9 K2 Nb4 23.67(11) . . ?
O16 K2 Nb4 116.44(13) 2_556 . ?
O13 K2 Nb4 166.08(13) . . ?
O15 K2 Nb4 79.86(11) . . ?
O15 K2 Nb4 94.18(12) 2_656 . ?
O12 K2 Nb4 64.76(11) . . ?
O14 K2 Nb4 103.94(12) . . ?
C13 K2 Nb4 143.33(16) . . ?
O9 K2 K1 119.18(12) . 2_556 ?
O16 K2 K1 46.11(13) 2_556 2_556 ?
O13 K2 K1 44.59(12) . 2_556 ?
O15 K2 K1 137.07(12) . 2_556 ?
O15 K2 K1 110.53(12) 2_656 2_556 ?
O12 K2 K1 99.24(12) . 2_556 ?
O14 K2 K1 44.60(11) . 2_556 ?
C13 K2 K1 60.56(15) . 2_556 ?
Nb4 K2 K1 139.13(5) . 2_556 ?
O9 K2 K2 100.11(12) . 2_656 ?
O16 K2 K2 111.12(13) 2_556 2_656 ?
O13 K2 K2 95.37(13) . 2_656 ?
O15 K2 K2 37.50(12) . 2_656 ?
O15 K2 K2 36.69(11) 2_656 2_656 ?
O12 K2 K2 116.44(13) . 2_656 ?
O14 K2 K2 159.65(14) . 2_656 ?
C13 K2 K2 92.04(16) . 2_656 ?
Nb4 K2 K2 86.38(5) . 2_656 ?
K1 K2 K2 132.58(6) 2_556 2_656 ?
O7 Nb1 O10 102.7(2) . . ?
O7 Nb1 O8 102.4(2) . . ?
O10 Nb1 O8 89.8(2) . . ?
O7 Nb1 O2 103.5(2) . . ?
O10 Nb1 O2 89.3(2) . . ?
O8 Nb1 O2 153.6(2) . . ?
O7 Nb1 O1 102.4(2) . . ?
O10 Nb1 O1 154.7(2) . . ?
O8 Nb1 O1 87.8(2) . . ?
O2 Nb1 O1 81.9(2) . . ?
O7 Nb1 O6 178.47(17) . . ?
O10 Nb1 O6 78.84(14) . . ?
O8 Nb1 O6 77.74(14) . . ?
O2 Nb1 O6 76.23(14) . . ?
O1 Nb1 O6 76.02(13) . . ?
O7 Nb1 Ir1 93.87(17) . . ?
O10 Nb1 Ir1 131.98(15) . . ?
O8 Nb1 Ir1 130.32(14) . . ?
O2 Nb1 Ir1 42.76(14) . . ?
O1 Nb1 Ir1 42.64(14) . . ?
O6 Nb1 Ir1 84.890(19) . . ?
O7 Nb1 Nb4 135.08(17) . 2_666 ?
O10 Nb1 Nb4 32.42(14) . 2_666 ?
O8 Nb1 Nb4 82.35(14) . 2_666 ?
O2 Nb1 Nb4 82.86(14) . 2_666 ?
O1 Nb1 Nb4 122.44(13) . 2_666 ?
O6 Nb1 Nb4 46.439(15) . 2_666 ?
Ir1 Nb1 Nb4 117.11(2) . 2_666 ?
O7 Nb1 Nb3 134.11(17) . 2_666 ?
O10 Nb1 Nb3 84.44(15) . 2_666 ?
O8 Nb1 Nb3 31.71(14) . 2_666 ?
O2 Nb1 Nb3 122.08(14) . 2_666 ?
O1 Nb1 Nb3 80.35(13) . 2_666 ?
O6 Nb1 Nb3 46.035(15) . 2_666 ?
Ir1 Nb1 Nb3 114.92(2) . 2_666 ?
Nb4 Nb1 Nb3 62.525(18) 2_666 2_666 ?
O7 Nb1 K1 84.69(17) . . ?
O10 Nb1 K1 139.26(15) . . ?
O8 Nb1 K1 49.76(14) . . ?
O2 Nb1 K1 128.38(14) . . ?
O1 Nb1 K1 46.96(14) . . ?
O6 Nb1 K1 94.33(3) . . ?
Ir1 Nb1 K1 86.39(3) . . ?
Nb4 Nb1 K1 126.24(3) 2_666 . ?
Nb3 Nb1 K1 63.73(3) 2_666 . ?
O5 Nb3 O4 103.2(2) . . ?
O5 Nb3 O8 101.5(2) . 2_666 ?
O4 Nb3 O8 89.9(2) . 2_666 ?
O5 Nb3 O2 105.4(2) . . ?
O4 Nb3 O2 90.21(19) . . ?
O8 Nb3 O2 152.4(2) 2_666 . ?
O5 Nb3 O3 103.0(2) . . ?
O4 Nb3 O3 153.6(2) . . ?
O8 Nb3 O3 88.00(19) 2_666 . ?
O2 Nb3 O3 79.79(19) . . ?
O5 Nb3 O6 178.16(17) . . ?
O4 Nb3 O6 78.30(15) . . ?
O8 Nb3 O6 77.41(14) 2_666 . ?
O2 Nb3 O6 75.59(14) . . ?
O3 Nb3 O6 75.56(14) . . ?
O5 Nb3 Ir1 96.38(16) . . ?
O4 Nb3 Ir1 131.40(14) . . ?
O8 Nb3 Ir1 129.12(14) 2_666 . ?
O2 Nb3 Ir1 41.46(14) . . ?
O3 Nb3 Ir1 41.40(13) . . ?
O6 Nb3 Ir1 83.296(18) . . ?
O5 Nb3 Nb1 133.14(16) . 2_666 ?
O4 Nb3 Nb1 83.13(14) . 2_666 ?
O8 Nb3 Nb1 31.67(14) 2_666 2_666 ?
O2 Nb3 Nb1 121.15(15) . 2_666 ?
O3 Nb3 Nb1 81.37(13) . 2_666 ?
O6 Nb3 Nb1 45.741(15) . 2_666 ?
Ir1 Nb3 Nb1 114.05(2) . 2_666 ?
O5 Nb3 Nb4 135.75(17) . 2_666 ?
O4 Nb3 Nb4 32.55(15) . 2_666 ?
O8 Nb3 Nb4 83.85(14) 2_666 2_666 ?
O2 Nb3 Nb4 81.54(14) . 2_666 ?
O3 Nb3 Nb4 121.16(14) . 2_666 ?
O6 Nb3 Nb4 45.770(15) . 2_666 ?
Ir1 Nb3 Nb4 114.21(2) . 2_666 ?
Nb1 Nb3 Nb4 62.547(19) 2_666 2_666 ?
O5 Nb3 K1 85.16(16) . 2_666 ?
O4 Nb3 K1 47.52(14) . 2_666 ?
O8 Nb3 K1 50.84(14) 2_666 2_666 ?
O2 Nb3 K1 137.61(14) . 2_666 ?
O3 Nb3 K1 138.74(13) . 2_666 ?
O6 Nb3 K1 95.18(3) . 2_666 ?
Ir1 Nb3 K1 178.38(3) . 2_666 ?
Nb1 Nb3 K1 65.02(3) 2_666 2_666 ?
Nb4 Nb3 K1 64.22(3) 2_666 2_666 ?
O9 Nb4 O10 103.1(2) . 2_666 ?
O9 Nb4 O4 100.6(2) . 2_666 ?
O10 Nb4 O4 89.4(2) 2_666 2_666 ?
O9 Nb4 O3 104.8(2) . . ?
O10 Nb4 O3 91.5(2) 2_666 . ?
O4 Nb4 O3 153.7(2) 2_666 . ?
O9 Nb4 O1 102.2(2) . . ?
O10 Nb4 O1 154.6(2) 2_666 . ?
O4 Nb4 O1 86.03(19) 2_666 . ?
O3 Nb4 O1 82.04(19) . . ?
O9 Nb4 O6 177.55(17) . . ?
O10 Nb4 O6 78.86(14) 2_666 . ?
O4 Nb4 O6 77.89(14) 2_666 . ?
O3 Nb4 O6 76.50(14) . . ?
O1 Nb4 O6 75.80(13) . . ?
O9 Nb4 Ir1 94.51(17) . . ?
O10 Nb4 Ir1 134.09(15) 2_666 . ?
O4 Nb4 Ir1 128.77(14) 2_666 . ?
O3 Nb4 Ir1 42.79(13) . . ?
O1 Nb4 Ir1 42.83(14) . . ?
O6 Nb4 Ir1 85.022(19) . . ?
O9 Nb4 Nb1 135.61(16) . 2_666 ?
O10 Nb4 Nb1 32.49(14) 2_666 2_666 ?
O4 Nb4 Nb1 83.77(13) 2_666 2_666 ?
O3 Nb4 Nb1 82.92(13) . 2_666 ?
O1 Nb4 Nb1 122.16(13) . 2_666 ?
O6 Nb4 Nb1 46.385(15) . 2_666 ?
Ir1 Nb4 Nb1 117.12(2) . 2_666 ?
O9 Nb4 Nb3 132.49(18) . 2_666 ?
O10 Nb4 Nb3 82.79(15) 2_666 2_666 ?
O4 Nb4 Nb3 31.89(14) 2_666 2_666 ?
O3 Nb4 Nb3 122.33(14) . 2_666 ?
O1 Nb4 Nb3 80.19(14) . 2_666 ?
O6 Nb4 Nb3 46.012(16) . 2_666 ?
Ir1 Nb4 Nb3 115.08(2) . 2_666 ?
Nb1 Nb4 Nb3 62.477(19) 2_666 2_666 ?
O9 Nb4 K2 37.84(16) . . ?
O10 Nb4 K2 66.45(14) 2_666 . ?
O4 Nb4 K2 90.84(14) 2_666 . ?
O3 Nb4 K2 113.52(14) . . ?
O1 Nb4 K2 138.44(14) . . ?
O6 Nb4 K2 143.67(3) . . ?
Ir1 Nb4 K2 126.91(3) . . ?
Nb1 Nb4 K2 98.55(3) 2_666 . ?
Nb3 Nb4 K2 115.99(3) 2_666 . ?
O9 Nb4 K1 82.22(17) . . ?
O10 Nb4 K1 136.57(15) 2_666 . ?
O4 Nb4 K1 47.74(13) 2_666 . ?
O3 Nb4 K1 129.40(13) . . ?
O1 Nb4 K1 48.03(14) . . ?
O6 Nb4 K1 95.34(3) . . ?
Ir1 Nb4 K1 87.22(3) . . ?
Nb1 Nb4 K1 126.64(3) 2_666 . ?
Nb3 Nb4 K1 64.21(3) 2_666 . ?
K2 Nb4 K1 102.30(4) . . ?
C2 Ir1 O1 145.9(3) . . ?
C2 Ir1 C6 66.5(3) . . ?
O1 Ir1 C6 122.8(3) . . ?
C2 Ir1 C9 40.0(3) . . ?
O1 Ir1 C9 162.4(2) . . ?
C6 Ir1 C9 39.6(3) . . ?
C2 Ir1 O3 100.1(2) . . ?
O1 Ir1 O3 77.54(18) . . ?
C6 Ir1 O3 159.1(3) . . ?
C9 Ir1 O3 119.9(2) . . ?
C2 Ir1 C3 39.2(3) . . ?
O1 Ir1 C3 110.2(3) . . ?
C6 Ir1 C3 66.6(3) . . ?
C9 Ir1 C3 66.7(3) . . ?
O3 Ir1 C3 113.8(2) . . ?
C2 Ir1 O2 135.9(3) . . ?
O1 Ir1 O2 77.22(19) . . ?
C6 Ir1 O2 102.2(2) . . ?
C9 Ir1 O2 103.5(2) . . ?
O3 Ir1 O2 75.86(18) . . ?
C3 Ir1 O2 168.5(2) . . ?
C2 Ir1 C5 66.2(3) . . ?
O1 Ir1 C5 99.6(2) . . ?
C6 Ir1 C5 39.5(3) . . ?
C9 Ir1 C5 66.5(3) . . ?
O3 Ir1 C5 151.2(2) . . ?
C3 Ir1 C5 39.7(3) . . ?
O2 Ir1 C5 132.0(2) . . ?
C2 Ir1 Nb4 120.1(2) . . ?
O1 Ir1 Nb4 40.98(12) . . ?
C6 Ir1 Nb4 160.8(2) . . ?
C9 Ir1 Nb4 156.0(2) . . ?
O3 Ir1 Nb4 39.86(14) . . ?
C3 Ir1 Nb4 106.3(2) . . ?
O2 Ir1 Nb4 85.09(14) . . ?
C5 Ir1 Nb4 123.7(2) . . ?
C2 Ir1 Nb1 172.4(2) . . ?
O1 Ir1 Nb1 40.56(13) . . ?
C6 Ir1 Nb1 106.9(2) . . ?
C9 Ir1 Nb1 132.4(2) . . ?
O3 Ir1 Nb1 85.18(13) . . ?
C3 Ir1 Nb1 143.1(2) . . ?
O2 Ir1 Nb1 39.90(14) . . ?
C5 Ir1 Nb1 111.5(2) . . ?
Nb4 Ir1 Nb1 67.449(17) . . ?
C2 Ir1 Nb3 114.7(2) . . ?
O1 Ir1 Nb3 85.32(12) . . ?
C6 Ir1 Nb3 129.7(2) . . ?
C9 Ir1 Nb3 106.53(19) . . ?
O3 Ir1 Nb3 39.53(13) . . ?
C3 Ir1 Nb3 147.2(2) . . ?
O2 Ir1 Nb3 39.19(13) . . ?
C5 Ir1 Nb3 168.9(2) . . ?
Nb4 Ir1 Nb3 66.199(17) . . ?
Nb1 Ir1 Nb3 66.078(17) . . ?

_refine_diff_density_max         1.697
_refine_diff_density_min         -2.619
_refine_diff_density_rms         0.628

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeOH'
####################################################################### 
# 
# 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_18k
_database_code_depnum_ccdc_archive 'CCDC 1423582'
_audit_update_record             
;
2015-09-11 deposited with the CCDC.
2016-01-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT043_18k                 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      30.23 Check
RESPONSE: H-atoms of the water and MeOH molecules were not localized
;

# Added during the CSD deposition process: Friday 11th of September 2015 08:10:04 AM
# end Validation Reply Form

#complex 3
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_structural     K4[{C10H15Rh}2Nb6O19]*4MeOH*10H2O
_chemical_formula_sum            'C24 H66 K4 Nb6 O33 Rh2'
_chemical_formula_weight         1802.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   14.6139(5)
_cell_length_b                   9.3769(3)
_cell_length_c                   19.9504(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.9640(10)
_cell_angle_gamma                90
_cell_volume                     2719.07(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5309
_cell_measurement_theta_min      3.39
_cell_measurement_theta_max      27.44

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.202
_exptl_crystal_F_000             1772
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.012
_exptl_absorpt_coefficient_mu    2.203
_shelx_estimated_absorpt_T_min   0.778
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean 25
_diffrn_reflns_number            17988
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.401
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6205
_reflns_number_gt                4923
_reflns_threshold_expression     >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       'APEX2 (Bruker-AXS, 2004)'
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXLE (Sheldrick, 2011)'
_computing_publication_material  'CIFTAB-97 (Sheldrick, 1998)'
_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)+(0.0897P)²+1.2721P] 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         6205
_refine_ls_number_parameters     311
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.1570
_refine_ls_wR_factor_gt          0.1143
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_restrained_S_all      1.143
_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 0.39473(4) 0.63966(6) 0.42841(3) 0.01358(15) Uani 1 1 d . . . . .
Nb2 Nb 0.41250(4) 0.28853(6) 0.47716(3) 0.01362(15) Uani 1 1 d . . . . .
Nb3 Nb 0.42158(4) 0.55394(6) 0.59773(2) 0.01297(15) Uani 1 1 d . . . . .
Rh4 Rh 0.24302(3) 0.48022(5) 0.50168(2) 0.01659(15) Uani 1 1 d . . . . .
C10 C 0.1180(4) 0.4062(8) 0.4500(3) 0.0223(14) Uani 1 1 d . . . . .
C9 C 0.1309(5) 0.3436(8) 0.5152(4) 0.0255(15) Uani 1 1 d . . . . .
C8 C 0.1139(5) 0.5583(8) 0.4570(4) 0.0290(16) Uani 1 1 d . . . . .
C7 C 0.1142(5) 0.3286(9) 0.3843(4) 0.0348(19) Uani 1 1 d . . . . .
H7A H 0.1047 0.3972 0.3471 0.052 Uiso 1 1 calc R U . . .
H7B H 0.1722 0.2775 0.3815 0.052 Uiso 1 1 calc R U . . .
H7C H 0.0632 0.2603 0.3811 0.052 Uiso 1 1 calc R U . . .
C6 C 0.1346(5) 0.4569(9) 0.5634(4) 0.0287(17) Uani 1 1 d . . . . .
C5 C 0.1379(5) 0.1864(9) 0.5306(4) 0.038(2) Uani 1 1 d . . . . .
H5A H 0.1466 0.1724 0.5795 0.057 Uiso 1 1 calc R U . . .
H5B H 0.0812 0.1387 0.5120 0.057 Uiso 1 1 calc R U . . .
H5C H 0.1903 0.1459 0.5103 0.057 Uiso 1 1 calc R U . . .
C4 C 0.1275(6) 0.7337(10) 0.5570(6) 0.055(3) Uani 1 1 d . . . . .
H4A H 0.1338 0.7265 0.6062 0.083 Uiso 1 1 calc R U . . .
H4B H 0.1806 0.7846 0.5425 0.083 Uiso 1 1 calc R U . . .
H4C H 0.0710 0.7858 0.5417 0.083 Uiso 1 1 calc R U . . .
C3 C 0.1230(4) 0.5886(8) 0.5273(4) 0.0278(16) Uani 1 1 d . . . . .
C2 C 0.0993(5) 0.6645(10) 0.4015(5) 0.044(2) Uani 1 1 d . . . . .
H2A H 0.0954 0.6150 0.3580 0.067 Uiso 1 1 calc R U . . .
H2B H 0.0420 0.7166 0.4053 0.067 Uiso 1 1 calc R U . . .
H2C H 0.1509 0.7316 0.4045 0.067 Uiso 1 1 calc R U . . .
C1 C 0.1502(6) 0.4400(11) 0.6385(4) 0.048(2) Uani 1 1 d . . . . .
H1A H 0.1559 0.3385 0.6499 0.073 Uiso 1 1 calc R U . . .
H1B H 0.2068 0.4897 0.6557 0.073 Uiso 1 1 calc R U . . .
H1C H 0.0981 0.4809 0.6591 0.073 Uiso 1 1 calc R U . . .
C1A C 0.252(2) 0.724(4) 0.2438(17) 0.059(9) Uiso 0.3 1 d . . P A 1
H1AA H 0.1958 0.7797 0.2448 0.089 Uiso 0.3 1 calc R U P A 1
H1AB H 0.3030 0.7714 0.2710 0.089 Uiso 0.3 1 calc R U P A 1
H1AC H 0.2672 0.7153 0.1971 0.089 Uiso 0.3 1 calc R U P A 1
C1B C 0.2113(8) 0.6346(11) 0.2177(5) 0.029(2) Uiso 0.7 1 d . . P A 2
H1BA H 0.1634 0.7035 0.2261 0.044 Uiso 0.7 1 calc R U P A 2
H1BB H 0.2652 0.6855 0.2044 0.044 Uiso 0.7 1 calc R U P A 2
H1BC H 0.1877 0.5697 0.1814 0.044 Uiso 0.7 1 calc R U P A 2
C2A C -0.0003(15) 0.935(2) 0.2913(10) 0.055(5) Uiso 0.6 1 d . . P B 3
C2B C 0.025(3) 0.974(4) 0.289(2) 0.078(12) Uiso 0.4 1 d . . P B 4
O10 O 0.5150(3) 0.2182(4) 0.5404(2) 0.0154(9) Uani 1 1 d . . . . .
O9 O 0.4916(3) 0.2874(4) 0.4041(2) 0.0161(9) Uani 1 1 d . . . . .
O8 O 0.3454(3) 0.1323(5) 0.4579(2) 0.0201(10) Uani 1 1 d . . . . .
O7 O 0.5000 0.5000 0.5000 0.0140(12) Uani 1 2 d S . P . .
O6 O 0.3404(3) 0.6488(4) 0.5196(2) 0.0156(9) Uani 1 1 d . . . . .
O5 O 0.3558(3) 0.3754(4) 0.5585(2) 0.0148(9) Uani 1 1 d . . . . .
O4 O 0.3337(3) 0.4440(4) 0.4266(2) 0.0150(9) Uani 1 1 d . . . . .
O3 O 0.5243(3) 0.4340(5) 0.6363(2) 0.0152(9) Uani 1 1 d . . . . .
O2 O 0.3622(3) 0.5942(5) 0.6679(2) 0.0205(10) Uani 1 1 d . . . . .
O1 O 0.3141(3) 0.7390(5) 0.3747(2) 0.0208(10) Uani 1 1 d . . . . .
O4W O 0.6680(4) 1.0632(5) 0.4403(2) 0.0311(12) Uani 1 1 d . . . . .
O3W O 0.3249(4) 0.0666(6) 0.2796(2) 0.0341(13) Uani 1 1 d . . . . .
O2W O 0.3468(5) 0.3484(6) 0.1535(3) 0.0436(15) Uani 1 1 d . . . . .
O1W O 0.5285(5) 1.1799(7) 0.2638(3) 0.0507(17) Uani 1 1 d . . . . .
O1M O 0.2364(5) 0.5568(7) 0.2759(3) 0.0561(17) Uani 1 1 d . . . . .
O1X O 0.2140(3) 0.9804(5) 0.3804(3) 0.0312(12) Uani 1 1 d . . . . .
O2M O 0.0234(6) 0.9850(8) 0.3604(5) 0.080(2) Uani 1 1 d . . . . .
K5 K 0.48240(12) 1.00283(16) 0.36920(7) 0.0256(3) Uani 1 1 d . . . . .
K6 K 0.36565(12) 0.34795(18) 0.28755(8) 0.0298(4) 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 1.773(4) . ?
Nb1 O10 1.932(4) 3_666 ?
Nb1 O3 1.966(4) 3_666 ?
Nb1 O4 2.039(4) . ?
Nb1 O6 2.061(4) . ?
Nb1 O7 2.3801(5) . ?
Nb1 Rh4 3.1560(7) . ?
Nb1 Nb2 3.2917(8) 3_666 ?
Nb1 Nb3 3.3263(8) 3_666 ?
Nb1 K5 3.8662(16) . ?
Nb1 K6 3.9130(16) . ?
Nb2 O8 1.783(4) . ?
Nb2 O9 1.952(4) . ?
Nb2 O10 1.970(4) . ?
Nb2 O4 2.056(4) . ?
Nb2 O5 2.065(4) . ?
Nb2 O7 2.3778(5) . ?
Nb2 Rh4 3.1394(7) . ?
Nb2 Nb1 3.2918(8) 3_666 ?
Nb2 Nb3 3.3237(7) 3_666 ?
Nb2 K5 3.6492(16) 1_545 ?
Nb2 K6 3.8145(16) . ?
Nb3 O2 1.763(4) . ?
Nb3 O9 1.958(4) 3_666 ?
Nb3 O3 1.967(4) . ?
Nb3 O5 2.046(4) . ?
Nb3 O6 2.060(4) . ?
Nb3 O7 2.4156(5) . ?
Nb3 Rh4 3.1497(7) . ?
Nb3 Nb2 3.3237(7) 3_666 ?
Nb3 Nb1 3.3263(8) 3_666 ?
Nb3 K6 3.7779(18) 3_666 ?
Rh4 C6 2.116(7) . ?
Rh4 C10 2.118(6) . ?
Rh4 C9 2.119(7) . ?
Rh4 O4 2.128(4) . ?
Rh4 C8 2.131(7) . ?
Rh4 O6 2.132(4) . ?
Rh4 C3 2.134(7) . ?
Rh4 O5 2.140(4) . ?
C10 C9 1.421(10) . ?
C10 C8 1.435(11) . ?
C10 C7 1.496(9) . ?
C9 C6 1.430(10) . ?
C9 C5 1.507(11) . ?
C8 C3 1.423(10) . ?
C8 C2 1.489(11) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C6 C3 1.431(11) . ?
C6 C1 1.501(10) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C4 C3 1.482(11) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1A O1M 1.72(3) . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C1B O1M 1.388(12) . ?
C1B H1BA 0.9800 . ?
C1B H1BB 0.9800 . ?
C1B H1BC 0.9800 . ?
C2A O2M 1.46(2) . ?
C2B O2M 1.44(4) . ?
O10 Nb1 1.932(4) 3_666 ?
O10 K5 2.744(4) 3_666 ?
O9 Nb3 1.958(4) 3_666 ?
O9 K5 2.757(4) 1_545 ?
O9 K6 2.868(4) . ?
O8 K5 3.058(5) 1_545 ?
O7 Nb2 2.3778(5) 3_666 ?
O7 Nb1 2.3801(5) 3_666 ?
O7 Nb3 2.4157(5) 3_666 ?
O4 K6 2.999(4) . ?
O3 Nb1 1.966(4) 3_666 ?
O3 K6 2.927(5) 3_666 ?
O4W K5 2.982(6) . ?
O3W K6 2.706(6) . ?
O3W K5 2.828(6) 1_545 ?
O2W K6 2.660(5) . ?
O2W K5 2.960(7) 2_645 ?
O1W K5 2.816(6) . ?
O1W K6 2.934(7) 1_565 ?
O1M K6 2.715(7) . ?
K5 O10 2.744(4) 3_666 ?
K5 O9 2.757(4) 1_565 ?
K5 O3W 2.828(6) 1_565 ?
K5 O2W 2.960(7) 2_655 ?
K5 O8 3.058(5) 1_565 ?
K5 Nb2 3.6493(16) 1_565 ?
K5 K6 3.932(2) 1_565 ?
K5 K6 4.274(2) 2_655 ?
K6 O3 2.927(5) 3_666 ?
K6 O1W 2.934(7) 1_545 ?
K6 Nb3 3.7779(18) 3_666 ?
K6 K5 3.932(2) 1_545 ?
K6 K5 4.274(2) 2_645 ?

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 O10 102.7(2) . 3_666 ?
O1 Nb1 O3 101.28(19) . 3_666 ?
O10 Nb1 O3 90.92(18) 3_666 3_666 ?
O1 Nb1 O4 101.5(2) . . ?
O10 Nb1 O4 155.43(17) 3_666 . ?
O3 Nb1 O4 87.96(17) 3_666 . ?
O1 Nb1 O6 102.62(19) . . ?
O10 Nb1 O6 90.01(17) 3_666 . ?
O3 Nb1 O6 155.25(17) 3_666 . ?
O4 Nb1 O6 81.09(17) . . ?
O1 Nb1 O7 178.23(16) . . ?
O10 Nb1 O7 79.01(12) 3_666 . ?
O3 Nb1 O7 78.76(12) 3_666 . ?
O4 Nb1 O7 76.69(12) . . ?
O6 Nb1 O7 77.15(12) . . ?
O1 Nb1 Rh4 94.24(15) . . ?
O10 Nb1 Rh4 131.82(12) 3_666 . ?
O3 Nb1 Rh4 129.63(13) 3_666 . ?
O4 Nb1 Rh4 41.82(11) . . ?
O6 Nb1 Rh4 42.03(12) . . ?
O7 Nb1 Rh4 84.422(18) . . ?
O1 Nb1 Nb2 135.56(15) . 3_666 ?
O10 Nb1 Nb2 32.82(12) 3_666 3_666 ?
O3 Nb1 Nb2 84.83(12) 3_666 3_666 ?
O4 Nb1 Nb2 122.76(12) . 3_666 ?
O6 Nb1 Nb2 82.63(12) . 3_666 ?
O7 Nb1 Nb2 46.194(13) . 3_666 ?
Rh4 Nb1 Nb2 115.62(2) . 3_666 ?
O1 Nb1 Nb3 133.54(14) . 3_666 ?
O10 Nb1 Nb3 83.79(13) 3_666 3_666 ?
O3 Nb1 Nb3 32.25(12) 3_666 3_666 ?
O4 Nb1 Nb3 82.23(12) . 3_666 ?
O6 Nb1 Nb3 123.53(12) . 3_666 ?
O7 Nb1 Nb3 46.528(13) . 3_666 ?
Rh4 Nb1 Nb3 115.55(2) . 3_666 ?
Nb2 Nb1 Nb3 62.921(16) 3_666 3_666 ?
O1 Nb1 K5 64.72(15) . . ?
O10 Nb1 K5 41.73(12) 3_666 . ?
O3 Nb1 K5 82.38(13) 3_666 . ?
O4 Nb1 K5 160.99(12) . . ?
O6 Nb1 K5 113.79(12) . . ?
O7 Nb1 K5 117.00(3) . . ?
Rh4 Nb1 K5 146.08(3) . . ?
Nb2 Nb1 K5 72.76(3) 3_666 . ?
Nb3 Nb1 K5 97.72(3) 3_666 . ?
O1 Nb1 K6 85.28(15) . . ?
O10 Nb1 K6 137.13(13) 3_666 . ?
O3 Nb1 K6 46.40(13) 3_666 . ?
O4 Nb1 K6 48.97(11) . . ?
O6 Nb1 K6 129.78(12) . . ?
O7 Nb1 K6 93.53(3) . . ?
Rh4 Nb1 K6 88.42(3) . . ?
Nb2 Nb1 K6 125.21(3) 3_666 . ?
Nb3 Nb1 K6 62.29(3) 3_666 . ?
K5 Nb1 K6 114.27(3) . . ?
O8 Nb2 O9 100.94(19) . . ?
O8 Nb2 O10 103.17(19) . . ?
O9 Nb2 O10 90.39(17) . . ?
O8 Nb2 O4 102.07(19) . . ?
O9 Nb2 O4 89.00(17) . . ?
O10 Nb2 O4 154.40(17) . . ?
O8 Nb2 O5 103.69(19) . . ?
O9 Nb2 O5 154.99(17) . . ?
O10 Nb2 O5 88.24(17) . . ?
O4 Nb2 O5 81.71(16) . . ?
O8 Nb2 O7 178.36(15) . . ?
O9 Nb2 O7 78.42(12) . . ?
O10 Nb2 O7 78.38(12) . . ?
O4 Nb2 O7 76.44(12) . . ?
O5 Nb2 O7 76.84(12) . . ?
O8 Nb2 Rh4 94.51(15) . . ?
O9 Nb2 Rh4 131.10(13) . . ?
O10 Nb2 Rh4 130.67(12) . . ?
O4 Nb2 Rh4 42.25(11) . . ?
O5 Nb2 Rh4 42.61(12) . . ?
O7 Nb2 Rh4 84.833(18) . . ?
O8 Nb2 Nb1 135.28(15) . 3_666 ?
O9 Nb2 Nb1 83.71(13) . 3_666 ?
O10 Nb2 Nb1 32.13(12) . 3_666 ?
O4 Nb2 Nb1 122.56(12) . 3_666 ?
O5 Nb2 Nb1 81.91(12) . 3_666 ?
O7 Nb2 Nb1 46.251(13) . 3_666 ?
Rh4 Nb2 Nb1 115.84(2) . 3_666 ?
O8 Nb2 Nb3 132.78(14) . 3_666 ?
O9 Nb2 Nb3 31.84(12) . 3_666 ?
O10 Nb2 Nb3 83.98(12) . 3_666 ?
O4 Nb2 Nb3 82.06(12) . 3_666 ?
O5 Nb2 Nb3 123.32(12) . 3_666 ?
O7 Nb2 Nb3 46.573(13) . 3_666 ?
Rh4 Nb2 Nb3 116.09(2) . 3_666 ?
Nb1 Nb2 Nb3 62.963(16) 3_666 3_666 ?
O8 Nb2 K5 56.70(15) . 1_545 ?
O9 Nb2 K5 48.05(13) . 1_545 ?
O10 Nb2 K5 83.77(12) . 1_545 ?
O4 Nb2 K5 114.06(12) . 1_545 ?
O5 Nb2 K5 155.96(12) . 1_545 ?
O7 Nb2 K5 123.19(3) . 1_545 ?
Rh4 Nb2 K5 141.81(3) . 1_545 ?
Nb1 Nb2 K5 102.27(3) 3_666 1_545 ?
Nb3 Nb2 K5 78.40(3) 3_666 1_545 ?
O8 Nb2 K6 82.42(14) . . ?
O9 Nb2 K6 47.12(13) . . ?
O10 Nb2 K6 136.94(12) . . ?
O4 Nb2 K6 51.41(11) . . ?
O5 Nb2 K6 132.56(12) . . ?
O7 Nb2 K6 96.07(3) . . ?
Rh4 Nb2 K6 90.44(3) . . ?
Nb1 Nb2 K6 126.33(3) 3_666 . ?
Nb3 Nb2 K6 63.47(3) 3_666 . ?
K5 Nb2 K6 63.53(3) 1_545 . ?
O2 Nb3 O9 103.0(2) . 3_666 ?
O2 Nb3 O3 103.31(19) . . ?
O9 Nb3 O3 88.41(18) 3_666 . ?
O2 Nb3 O5 103.20(19) . . ?
O9 Nb3 O5 153.44(17) 3_666 . ?
O3 Nb3 O5 89.48(18) . . ?
O2 Nb3 O6 102.45(19) . . ?
O9 Nb3 O6 88.93(17) 3_666 . ?
O3 Nb3 O6 154.03(16) . . ?
O5 Nb3 O6 81.54(17) . . ?
O2 Nb3 O7 178.75(15) . . ?
O9 Nb3 O7 77.37(12) 3_666 . ?
O3 Nb3 O7 77.85(11) . . ?
O5 Nb3 O7 76.31(11) . . ?
O6 Nb3 O7 76.36(11) . . ?
O2 Nb3 Rh4 94.87(16) . . ?
O9 Nb3 Rh4 130.76(13) 3_666 . ?
O3 Nb3 Rh4 131.51(13) . . ?
O5 Nb3 Rh4 42.33(12) . . ?
O6 Nb3 Rh4 42.16(12) . . ?
O7 Nb3 Rh4 84.000(17) . . ?
O2 Nb3 Nb2 134.77(16) . 3_666 ?
O9 Nb3 Nb2 31.74(12) 3_666 3_666 ?
O3 Nb3 Nb2 82.39(12) . 3_666 ?
O5 Nb3 Nb2 121.84(11) . 3_666 ?
O6 Nb3 Nb2 81.83(12) . 3_666 ?
O7 Nb3 Nb2 45.632(13) . 3_666 ?
Rh4 Nb3 Nb2 114.896(19) . 3_666 ?
O2 Nb3 Nb1 135.51(15) . 3_666 ?
O9 Nb3 Nb1 82.92(13) 3_666 3_666 ?
O3 Nb3 Nb1 32.23(11) . 3_666 ?
O5 Nb3 Nb1 81.27(12) . 3_666 ?
O6 Nb3 Nb1 121.86(11) . 3_666 ?
O7 Nb3 Nb1 45.645(13) . 3_666 ?
Rh4 Nb3 Nb1 114.58(2) . 3_666 ?
Nb2 Nb3 Nb1 62.208(17) 3_666 3_666 ?
O2 Nb3 K6 84.78(16) . 3_666 ?
O9 Nb3 K6 48.10(13) 3_666 3_666 ?
O3 Nb3 K6 49.89(13) . 3_666 ?
O5 Nb3 K6 139.09(12) . 3_666 ?
O6 Nb3 K6 136.58(12) . 3_666 ?
O7 Nb3 K6 96.34(3) . 3_666 ?
Rh4 Nb3 K6 178.58(3) . 3_666 ?
Nb2 Nb3 K6 64.61(3) 3_666 3_666 ?
Nb1 Nb3 K6 66.49(3) 3_666 3_666 ?
C6 Rh4 C10 65.8(3) . . ?
C6 Rh4 C9 39.5(3) . . ?
C10 Rh4 C9 39.2(3) . . ?
C6 Rh4 O4 162.1(2) . . ?
C10 Rh4 O4 100.0(2) . . ?
C9 Rh4 O4 122.6(2) . . ?
C6 Rh4 C8 66.1(3) . . ?
C10 Rh4 C8 39.5(3) . . ?
C9 Rh4 C8 66.3(3) . . ?
O4 Rh4 C8 110.5(2) . . ?
C6 Rh4 O6 120.4(2) . . ?
C10 Rh4 O6 148.3(2) . . ?
C9 Rh4 O6 159.8(2) . . ?
O4 Rh4 O6 77.47(16) . . ?
C8 Rh4 O6 111.2(2) . . ?
C6 Rh4 C3 39.3(3) . . ?
C10 Rh4 C3 65.4(3) . . ?
C9 Rh4 C3 65.9(3) . . ?
O4 Rh4 C3 146.3(2) . . ?
C8 Rh4 C3 39.0(3) . . ?
O6 Rh4 C3 99.0(2) . . ?
C6 Rh4 O5 103.1(2) . . ?
C10 Rh4 O5 133.2(2) . . ?
C9 Rh4 O5 102.6(2) . . ?
O4 Rh4 O5 78.34(16) . . ?
C8 Rh4 O5 168.3(2) . . ?
O6 Rh4 O5 77.77(16) . . ?
C3 Rh4 O5 134.3(2) . . ?
C6 Rh4 Nb2 133.0(2) . . ?
C10 Rh4 Nb2 113.02(19) . . ?
C9 Rh4 Nb2 107.8(2) . . ?
O4 Rh4 Nb2 40.52(11) . . ?
C8 Rh4 Nb2 144.1(2) . . ?
O6 Rh4 Nb2 85.83(12) . . ?
C3 Rh4 Nb2 172.3(2) . . ?
O5 Rh4 Nb2 40.79(11) . . ?
C6 Rh4 Nb3 107.0(2) . . ?
C10 Rh4 Nb3 170.31(19) . . ?
C9 Rh4 Nb3 131.1(2) . . ?
O4 Rh4 Nb3 85.77(11) . . ?
C8 Rh4 Nb3 145.1(2) . . ?
O6 Rh4 Nb3 40.44(11) . . ?
C3 Rh4 Nb3 113.52(19) . . ?
O5 Rh4 Nb3 40.08(11) . . ?
Nb2 Rh4 Nb3 66.628(17) . . ?
C6 Rh4 Nb1 157.3(2) . . ?
C10 Rh4 Nb1 122.79(18) . . ?
C9 Rh4 Nb1 159.22(19) . . ?
O4 Rh4 Nb1 39.72(11) . . ?
C8 Rh4 Nb1 106.1(2) . . ?
O6 Rh4 Nb1 40.35(11) . . ?
C3 Rh4 Nb1 121.3(2) . . ?
O5 Rh4 Nb1 85.62(11) . . ?
Nb2 Rh4 Nb1 66.143(17) . . ?
Nb3 Rh4 Nb1 66.445(17) . . ?
C9 C10 C8 109.0(6) . . ?
C9 C10 C7 126.2(7) . . ?
C8 C10 C7 124.8(7) . . ?
C9 C10 Rh4 70.4(4) . . ?
C8 C10 Rh4 70.7(4) . . ?
C7 C10 Rh4 122.5(5) . . ?
C10 C9 C6 107.5(6) . . ?
C10 C9 C5 126.2(7) . . ?
C6 C9 C5 126.3(7) . . ?
C10 C9 Rh4 70.4(4) . . ?
C6 C9 Rh4 70.2(4) . . ?
C5 C9 Rh4 125.5(5) . . ?
C3 C8 C10 107.1(6) . . ?
C3 C8 C2 126.3(8) . . ?
C10 C8 C2 126.6(7) . . ?
C3 C8 Rh4 70.6(4) . . ?
C10 C8 Rh4 69.8(4) . . ?
C2 C8 Rh4 126.4(5) . . ?
C10 C7 H7A 109.5 . . ?
C10 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C10 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C6 C9 108.0(6) . . ?
C3 C6 C1 126.2(8) . . ?
C9 C6 C1 125.8(8) . . ?
C3 C6 Rh4 71.0(4) . . ?
C9 C6 Rh4 70.4(4) . . ?
C1 C6 Rh4 123.2(5) . . ?
C9 C5 H5A 109.5 . . ?
C9 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C9 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C8 C3 C6 108.5(6) . . ?
C8 C3 C4 124.9(8) . . ?
C6 C3 C4 126.4(8) . . ?
C8 C3 Rh4 70.4(4) . . ?
C6 C3 Rh4 69.6(4) . . ?
C4 C3 Rh4 122.0(5) . . ?
C8 C2 H2A 109.5 . . ?
C8 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C8 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C6 C1 H1A 109.5 . . ?
C6 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C6 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1M C1A H1AA 109.5 . . ?
O1M C1A H1AB 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
O1M C1A H1AC 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
O1M C1B H1BA 109.5 . . ?
O1M C1B H1BB 109.5 . . ?
H1BA C1B H1BB 109.5 . . ?
O1M C1B H1BC 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
Nb1 O10 Nb2 115.1(2) 3_666 . ?
Nb1 O10 K5 110.31(18) 3_666 3_666 ?
Nb2 O10 K5 129.17(19) . 3_666 ?
Nb2 O9 Nb3 116.4(2) . 3_666 ?
Nb2 O9 K5 100.18(16) . 1_545 ?
Nb3 O9 K5 138.2(2) 3_666 1_545 ?
Nb2 O9 K6 102.96(17) . . ?
Nb3 O9 K6 101.35(16) 3_666 . ?
K5 O9 K6 88.65(13) 1_545 . ?
Nb2 O8 K5 94.14(17) . 1_545 ?
Nb2 O7 Nb2 180.0 3_666 . ?
Nb2 O7 Nb1 87.553(19) 3_666 . ?
Nb2 O7 Nb1 92.445(19) . . ?
Nb2 O7 Nb1 92.446(19) 3_666 3_666 ?
Nb2 O7 Nb1 87.556(19) . 3_666 ?
Nb1 O7 Nb1 180.0 . 3_666 ?
Nb2 O7 Nb3 87.796(18) 3_666 . ?
Nb2 O7 Nb3 92.205(18) . . ?
Nb1 O7 Nb3 92.172(18) . . ?
Nb1 O7 Nb3 87.828(18) 3_666 . ?
Nb2 O7 Nb3 92.205(18) 3_666 3_666 ?
Nb2 O7 Nb3 87.794(18) . 3_666 ?
Nb1 O7 Nb3 87.827(18) . 3_666 ?
Nb1 O7 Nb3 92.172(18) 3_666 3_666 ?
Nb3 O7 Nb3 180.0 . 3_666 ?
Nb3 O6 Nb1 113.9(2) . . ?
Nb3 O6 Rh4 97.40(17) . . ?
Nb1 O6 Rh4 97.62(17) . . ?
Nb3 O5 Nb2 114.35(19) . . ?
Nb3 O5 Rh4 97.59(17) . . ?
Nb2 O5 Rh4 96.60(17) . . ?
Nb1 O4 Nb2 114.0(2) . . ?
Nb1 O4 Rh4 98.46(17) . . ?
Nb2 O4 Rh4 97.23(17) . . ?
Nb1 O4 K6 100.18(15) . . ?
Nb2 O4 K6 96.19(15) . . ?
Rh4 O4 K6 150.16(19) . . ?
Nb1 O3 Nb3 115.52(19) 3_666 . ?
Nb1 O3 K6 104.49(17) 3_666 3_666 ?
Nb3 O3 K6 99.18(17) . 3_666 ?
K6 O3W K5 90.53(16) . 1_545 ?
K6 O2W K5 98.8(2) . 2_645 ?
K5 O1W K6 86.27(17) . 1_565 ?
C1B O1M K6 124.9(6) . . ?
C1A O1M K6 124.7(13) . . ?
O10 K5 O9 124.60(14) 3_666 1_565 ?
O10 K5 O1W 161.41(18) 3_666 . ?
O9 K5 O1W 66.97(15) 1_565 . ?
O10 K5 O3W 121.99(15) 3_666 1_565 ?
O9 K5 O3W 88.29(14) 1_565 1_565 ?
O1W K5 O3W 69.23(17) . 1_565 ?
O10 K5 O2W 77.10(14) 3_666 2_655 ?
O9 K5 O2W 119.48(15) 1_565 2_655 ?
O1W K5 O2W 84.45(18) . 2_655 ?
O3W K5 O2W 130.59(15) 1_565 2_655 ?
O10 K5 O4W 83.16(14) 3_666 . ?
O9 K5 O4W 71.22(14) 1_565 . ?
O1W K5 O4W 88.11(17) . . ?
O3W K5 O4W 154.30(16) 1_565 . ?
O2W K5 O4W 54.97(15) 2_655 . ?
O10 K5 O8 83.39(13) 3_666 1_565 ?
O9 K5 O8 59.16(12) 1_565 1_565 ?
O1W K5 O8 114.84(17) . 1_565 ?
O3W K5 O8 75.09(14) 1_565 1_565 ?
O2W K5 O8 153.60(14) 2_655 1_565 ?
O4W K5 O8 105.50(13) . 1_565 ?
O10 K5 Nb2 98.76(10) 3_666 1_565 ?
O9 K5 Nb2 31.77(9) 1_565 1_565 ?
O1W K5 Nb2 96.40(13) . 1_565 ?
O3W K5 Nb2 87.62(11) 1_565 1_565 ?
O2W K5 Nb2 137.85(12) 2_655 1_565 ?
O4W K5 Nb2 82.89(10) . 1_565 ?
O8 K5 Nb2 29.16(8) 1_565 1_565 ?
O10 K5 Nb1 27.95(9) 3_666 . ?
O9 K5 Nb1 141.65(10) 1_565 . ?
O1W K5 Nb1 149.34(13) . . ?
O3W K5 Nb1 96.06(12) 1_565 . ?
O2W K5 Nb1 85.83(11) 2_655 . ?
O4W K5 Nb1 109.62(10) . . ?
O8 K5 Nb1 85.13(9) 1_565 . ?
Nb2 K5 Nb1 110.14(4) 1_565 . ?
O10 K5 K6 150.40(11) 3_666 1_565 ?
O9 K5 K6 46.83(9) 1_565 1_565 ?
O1W K5 K6 48.12(14) . 1_565 ?
O3W K5 K6 43.48(11) 1_565 1_565 ?
O2W K5 K6 132.50(11) 2_655 1_565 ?
O4W K5 K6 112.02(11) . 1_565 ?
O8 K5 K6 68.34(9) 1_565 1_565 ?
Nb2 K5 K6 60.28(3) 1_565 1_565 ?
Nb1 K5 K6 135.09(5) . 1_565 ?
O10 K5 K6 104.56(10) 3_666 2_655 ?
O9 K5 K6 119.88(10) 1_565 2_655 ?
O1W K5 K6 58.06(14) . 2_655 ?
O3W K5 K6 93.44(11) 1_565 2_655 ?
O2W K5 K6 37.96(11) 2_655 2_655 ?
O4W K5 K6 84.07(10) . 2_655 ?
O8 K5 K6 168.42(10) 1_565 2_655 ?
Nb2 K5 K6 151.64(5) 1_565 2_655 ?
Nb1 K5 K6 97.94(4) . 2_655 ?
K6 K5 K6 102.28(4) 1_565 2_655 ?
O2W K6 O3W 86.76(17) . . ?
O2W K6 O1M 85.08(19) . . ?
O3W K6 O1M 123.5(2) . . ?
O2W K6 O9 143.70(18) . . ?
O3W K6 O9 88.48(15) . . ?
O1M K6 O9 126.49(17) . . ?
O2W K6 O3 120.95(16) . 3_666 ?
O3W K6 O3 144.82(15) . 3_666 ?
O1M K6 O3 83.14(17) . 3_666 ?
O9 K6 O3 56.35(12) . 3_666 ?
O2W K6 O1W 80.75(18) . 1_545 ?
O3W K6 O1W 69.16(17) . 1_545 ?
O1M K6 O1W 160.5(2) . 1_545 ?
O9 K6 O1W 64.00(14) . 1_545 ?
O3 K6 O1W 92.74(15) 3_666 1_545 ?
O2W K6 O4 156.89(17) . . ?
O3W K6 O4 107.01(14) . . ?
O1M K6 O4 71.86(16) . . ?
O9 K6 O4 57.19(12) . . ?
O3 K6 O4 55.97(11) 3_666 . ?
O1W K6 O4 121.18(15) 1_545 . ?
O2W K6 Nb3 126.96(16) . 3_666 ?
O3W K6 Nb3 115.81(13) . 3_666 ?
O1M K6 Nb3 113.45(15) . 3_666 ?
O9 K6 Nb3 30.54(9) . 3_666 ?
O3 K6 Nb3 30.93(9) 3_666 3_666 ?
O1W K6 Nb3 66.32(12) 1_545 3_666 ?
O4 K6 Nb3 64.16(9) . 3_666 ?
O2W K6 Nb2 170.57(14) . . ?
O3W K6 Nb2 86.07(11) . . ?
O1M K6 Nb2 104.01(15) . . ?
O9 K6 Nb2 29.92(8) . . ?
O3 K6 Nb2 63.59(8) 3_666 . ?
O1W K6 Nb2 90.96(12) 1_545 . ?
O4 K6 Nb2 32.40(8) . . ?
Nb3 K6 Nb2 51.92(2) 3_666 . ?
O2W K6 Nb1 135.48(13) . . ?
O3W K6 Nb1 136.93(12) . . ?
O1M K6 Nb1 65.16(14) . . ?
O9 K6 Nb1 62.84(9) . . ?
O3 K6 Nb1 29.10(8) 3_666 . ?
O1W K6 Nb1 117.53(12) 1_545 . ?
O4 K6 Nb1 30.85(8) . . ?
Nb3 K6 Nb1 51.22(2) 3_666 . ?
Nb2 K6 Nb1 52.77(2) . . ?
O2W K6 K5 114.39(13) . 1_545 ?
O3W K6 K5 45.99(12) . 1_545 ?
O1M K6 K5 153.85(16) . 1_545 ?
O9 K6 K5 44.52(9) . 1_545 ?
O3 K6 K5 99.70(10) 3_666 1_545 ?
O1W K6 K5 45.61(13) 1_545 1_545 ?
O4 K6 K5 88.08(9) . 1_545 ?
Nb3 K6 K5 69.82(4) 3_666 1_545 ?
Nb2 K6 K5 56.19(3) . 1_545 ?
Nb1 K6 K5 105.53(4) . 1_545 ?
O2W K6 K5 43.19(15) . 2_645 ?
O3W K6 K5 114.61(12) . 2_645 ?
O1M K6 K5 95.85(16) . 2_645 ?
O9 K6 K5 108.79(10) . 2_645 ?
O3 K6 K5 80.96(9) 3_666 2_645 ?
O1W K6 K5 64.68(13) 1_545 2_645 ?
O4 K6 K5 135.86(10) . 2_645 ?
Nb3 K6 K5 84.43(4) 3_666 2_645 ?
Nb2 K6 K5 136.22(5) . 2_645 ?
Nb1 K6 K5 105.19(4) . 2_645 ?
K5 K6 K5 110.29(4) 1_545 2_645 ?

_refine_diff_density_max         1.575
_refine_diff_density_min         -2.811
_refine_diff_density_rms         0.771

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         0
_diffrn_standards_decay_%        0



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeOH'
