# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pa300-2
#complex 1
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_structural     K4[(C10H15Rh)2Nb6O19]*20H2O
_chemical_formula_sum            'C20 H70 K4 Nb6 O39 Rh2'
_chemical_formula_weight         1854.44

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  ?

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

_cell_length_a                   14.8711(17)
_cell_length_b                   9.5972(11)
_cell_length_c                   19.615(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.761(3)
_cell_angle_gamma                90.00
_cell_volume                     2798.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(2)
_cell_measurement_reflns_used    2671
_cell_measurement_theta_min      2.5238
_cell_measurement_theta_max      28.9379

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1828
_exptl_absorpt_coefficient_mu    2.152
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6026
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'based on intensities (SADABS, Bruker, 2005)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex2 Duo CCD detector'
_diffrn_measurement_method       'combined omega- and phi-scans'
_diffrn_detector_area_resol_mean 25
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            19444
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0895
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         30.66
_reflns_number_total             8599
_reflns_number_gt                6081
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2 V.1.27 (Bruker, 2005)'
_computing_cell_refinement       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_reduction        'Apex2 V.1.27 (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V6.22 (Bruker, 2000-2005)'
_computing_publication_material  'local programs'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0218P)²+45.4204P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8599
_refine_ls_number_parameters     327
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0659
_refine_ls_wR_factor_ref         0.1425
_refine_ls_wR_factor_gt          0.1302
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.52252(14) 1.00412(19) 0.12469(9) 0.0233(4) Uani 1 1 d . . .
K2 K 0.63315(14) 0.3441(2) 0.20324(9) 0.0254(4) Uani 1 1 d . . .
Rh1 Rh 0.24809(4) 0.51296(6) 0.01165(3) 0.01002(12) Uani 1 1 d . . .
Nb1 Nb 0.41299(4) 0.70447(6) -0.01789(3) 0.00909(13) Uani 1 1 d . . .
Nb2 Nb 0.39929(4) 0.36240(6) -0.06908(3) 0.00891(13) Uani 1 1 d . . .
Nb3 Nb 0.42201(4) 0.44253(6) 0.10185(3) 0.00843(13) Uani 1 1 d . . .
C11 C 0.1389(5) 0.6486(9) 0.0316(4) 0.0162(15) Uani 1 1 d U . .
C12 C 0.1385(5) 0.5309(8) 0.0783(4) 0.0155(15) Uani 1 1 d . . .
C13 C 0.1281(5) 0.4060(8) 0.0388(4) 0.0166(15) Uani 1 1 d . . .
C14 C 0.1230(5) 0.4452(8) -0.0320(4) 0.0152(15) Uani 1 1 d . . .
C15 C 0.1287(5) 0.5944(9) -0.0355(4) 0.0176(16) Uani 1 1 d . . .
C16 C 0.1509(6) 0.7954(9) 0.0532(5) 0.0225(18) Uani 1 1 d . . .
H16A H 0.0926 0.8348 0.0648 0.034 Uiso 1 1 calc R . .
H16B H 0.1762 0.8491 0.0158 0.034 Uiso 1 1 calc R . .
H16C H 0.1920 0.7995 0.0932 0.034 Uiso 1 1 calc R . .
C17 C 0.1467(6) 0.5409(10) 0.1549(4) 0.0253(19) Uani 1 1 d . . .
H17A H 0.0925 0.5850 0.1723 0.038 Uiso 1 1 calc R . .
H17B H 0.1995 0.5971 0.1679 0.038 Uiso 1 1 calc R . .
H17C H 0.1532 0.4473 0.1744 0.038 Uiso 1 1 calc R . .
C18 C 0.1287(6) 0.2596(9) 0.0647(5) 0.027(2) Uani 1 1 d . . .
H18A H 0.0691 0.2180 0.0569 0.041 Uiso 1 1 calc R . .
H18B H 0.1439 0.2595 0.1137 0.041 Uiso 1 1 calc R . .
H18C H 0.1736 0.2052 0.0406 0.041 Uiso 1 1 calc R . .
C19 C 0.1076(6) 0.3515(9) -0.0917(4) 0.0232(18) Uani 1 1 d . . .
H19A H 0.0436 0.3527 -0.1054 0.035 Uiso 1 1 calc R . .
H19B H 0.1254 0.2563 -0.0792 0.035 Uiso 1 1 calc R . .
H19C H 0.1434 0.3836 -0.1297 0.035 Uiso 1 1 calc R . .
C20 C 0.1287(6) 0.6770(9) -0.1003(4) 0.0215(18) Uani 1 1 d . . .
H20A H 0.0665 0.6939 -0.1163 0.032 Uiso 1 1 calc R . .
H20B H 0.1605 0.6247 -0.1351 0.032 Uiso 1 1 calc R . .
H20C H 0.1591 0.7662 -0.0920 0.032 Uiso 1 1 calc R . .
O1I O 0.5000 0.5000 0.0000 0.0104(14) Uani 1 2 d S . .
O1 O 0.3487(4) 0.8558(5) -0.0340(3) 0.0151(11) Uani 1 1 d . . .
O2 O 0.3245(4) 0.2608(5) -0.1193(3) 0.0149(11) Uani 1 1 d . . .
O3 O 0.3633(4) 0.3993(6) 0.1758(3) 0.0153(11) Uani 1 1 d . . .
O11 O 0.3401(3) 0.5536(5) -0.0681(2) 0.0106(10) Uani 1 1 d . . .
O12 O 0.3574(3) 0.6156(5) 0.0659(3) 0.0110(10) Uani 1 1 d . . .
O13 O 0.3465(3) 0.3511(5) 0.0258(2) 0.0095(9) Uani 1 1 d . . .
O14 O 0.5200(4) 0.5614(5) 0.1372(2) 0.0116(10) Uani 1 1 d . . .
O15 O 0.5106(3) 0.7751(5) 0.0411(3) 0.0094(10) Uani 1 1 d . . .
O16 O 0.4915(3) 0.7100(5) -0.0962(2) 0.0115(10) Uani 1 1 d . . .
O1W O 0.7781(4) 0.9746(6) 0.0949(3) 0.0228(13) Uani 1 1 d . . .
O2W O 0.9630(4) 0.9992(7) 0.0675(3) 0.0294(15) Uani 1 1 d . . .
O3W O 0.7553(4) 0.7446(6) 0.2472(3) 0.0223(13) Uani 1 1 d . . .
O4W O 0.3463(5) 1.0603(6) 0.0684(3) 0.0284(15) Uani 1 1 d . . .
O5W O 0.9662(5) 0.4691(7) 0.2994(4) 0.0354(17) Uani 1 1 d . . .
O6W O 0.9457(5) 0.7514(7) 0.2588(4) 0.0367(17) Uani 1 1 d . . .
O7W O 0.7839(6) 0.4617(7) 0.2659(4) 0.048(2) Uani 1 1 d . . .
O8W O 0.6367(8) 0.3393(8) 0.3404(4) 0.062(3) Uani 1 1 d . . .
O9W O 0.6750(5) 0.0717(7) 0.2098(3) 0.0288(15) Uani 1 1 d . . .
O10W O 0.4723(6) 1.1621(11) 0.2335(4) 0.064(3) 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
K1 K2 3.946(3) 1_565 ?
K1 K2 4.426(3) 2_655 ?
K1 Nb1 3.640(2) 3_675 ?
K1 Nb2 3.872(2) 3_665 ?
K1 O1 2.975(6) 3_675 ?
K1 O2 3.416(6) 3_665 ?
K1 O15 2.744(5) . ?
K1 O16 2.807(5) 3_675 ?
K1 O4W 2.864(7) . ?
K1 O8W 2.946(10) 2_655 ?
K1 O9W 2.849(7) 1_565 ?
K1 O10W 2.740(9) . ?
K2 K1 3.946(3) 1_545 ?
K2 K1 4.426(3) 2_645 ?
K2 Nb1 3.7082(19) 3_665 ?
K2 Nb2 3.8748(19) 3_665 ?
K2 Nb3 3.785(2) . ?
K2 O11 2.867(5) 3_665 ?
K2 O14 2.954(5) . ?
K2 O16 2.806(5) 3_665 ?
K2 O7W 2.764(8) . ?
K2 O8W 2.690(8) . ?
K2 O9W 2.689(7) . ?
K2 O10W 3.036(11) 1_545 ?
Rh1 Nb1 3.1329(9) . ?
Rh1 Nb2 3.1416(9) . ?
Rh1 Nb3 3.1615(9) . ?
Rh1 C11 2.127(7) . ?
Rh1 C12 2.127(7) . ?
Rh1 C13 2.140(8) . ?
Rh1 C14 2.126(8) . ?
Rh1 C15 2.126(8) . ?
Rh1 O11 2.145(5) . ?
Rh1 O12 2.155(5) . ?
Rh1 O13 2.147(5) . ?
Nb1 K1 3.640(2) 3_675 ?
Nb1 K2 3.7082(19) 3_665 ?
Nb1 Nb2 3.2896(9) 3_665 ?
Nb1 Nb3 3.3123(10) 3_665 ?
Nb1 O1I 2.3707(7) . ?
Nb1 O1 1.762(5) . ?
Nb1 O11 2.043(5) . ?
Nb1 O12 2.048(5) . ?
Nb1 O15 1.951(5) . ?
Nb1 O16 1.958(5) . ?
Nb2 K1 3.872(2) 3_665 ?
Nb2 K2 3.8748(19) 3_665 ?
Nb2 Nb1 3.2897(9) 3_665 ?
Nb2 Nb3 3.3295(9) 3_665 ?
Nb2 O1I 2.3870(6) . ?
Nb2 O2 1.758(5) . ?
Nb2 O11 2.036(5) . ?
Nb2 O13 2.044(5) . ?
Nb2 O14 1.964(5) 3_665 ?
Nb2 O15 1.947(5) 3_665 ?
Nb3 Nb1 3.3123(10) 3_665 ?
Nb3 Nb2 3.3293(10) 3_665 ?
Nb3 O1I 2.4047(7) . ?
Nb3 O3 1.766(5) . ?
Nb3 O12 2.034(5) . ?
Nb3 O13 2.038(5) . ?
Nb3 O14 1.961(5) . ?
Nb3 O16 1.954(5) 3_665 ?
C11 C12 1.453(11) . ?
C11 C15 1.420(11) . ?
C11 C16 1.481(11) . ?
C12 C13 1.434(11) . ?
C12 C17 1.507(11) . ?
C13 C14 1.438(11) . ?
C13 C18 1.495(12) . ?
C14 C15 1.436(11) . ?
C14 C19 1.489(11) . ?
C15 C20 1.498(11) . ?
O1I Nb1 2.3707(7) 3_665 ?
O1I Nb2 2.3870(6) 3_665 ?
O1I Nb3 2.4048(7) 3_665 ?
O1 K1 2.975(6) 3_675 ?
O2 K1 3.416(6) 3_665 ?
O11 K2 2.866(5) 3_665 ?
O14 Nb2 1.964(5) 3_665 ?
O15 Nb2 1.947(5) 3_665 ?
O16 K1 2.807(5) 3_675 ?
O16 K2 2.806(5) 3_665 ?
O16 Nb3 1.954(5) 3_665 ?
O8W K1 2.946(10) 2_645 ?
O9W K1 2.849(7) 1_545 ?
O10W K2 3.036(11) 1_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
K2 K1 K2 102.17(5) 1_565 2_655 ?
Nb1 K1 K2 58.36(4) 3_675 1_565 ?
Nb1 K1 K2 149.16(6) 3_675 2_655 ?
Nb1 K1 Nb2 116.69(5) 3_675 3_665 ?
Nb2 K1 K2 137.39(7) 3_665 1_565 ?
Nb2 K1 K2 93.91(5) 3_665 2_655 ?
O1 K1 K2 65.90(11) 3_675 1_565 ?
O1 K1 K2 166.99(12) 3_675 2_655 ?
O1 K1 Nb1 28.71(10) 3_675 3_675 ?
O1 K1 Nb2 92.14(12) 3_675 3_665 ?
O1 K1 O2 82.88(14) 3_675 3_665 ?
O2 K1 K2 110.94(11) 3_665 1_565 ?
O2 K1 K2 97.46(10) 3_665 2_655 ?
O2 K1 Nb1 111.50(11) 3_665 3_675 ?
O2 K1 Nb2 27.00(9) 3_665 3_665 ?
O15 K1 K2 156.05(13) . 1_565 ?
O15 K1 K2 98.74(12) . 2_655 ?
O15 K1 Nb1 106.55(12) . 3_675 ?
O15 K1 Nb2 28.18(10) . 3_665 ?
O15 K1 O1 92.03(16) . 3_675 ?
O15 K1 O2 54.27(14) . 3_665 ?
O15 K1 O16 131.38(16) . 3_675 ?
O15 K1 O4W 83.05(17) . . ?
O15 K1 O8W 70.80(18) . 2_655 ?
O15 K1 O9W 124.60(19) . 1_565 ?
O16 K1 K2 45.32(11) 3_675 1_565 ?
O16 K1 K2 116.99(12) 3_675 2_655 ?
O16 K1 Nb1 32.18(10) 3_675 3_675 ?
O16 K1 Nb2 148.55(12) 3_675 3_665 ?
O16 K1 O1 58.96(15) 3_675 3_675 ?
O16 K1 O2 140.08(15) 3_675 3_665 ?
O16 K1 O4W 71.20(16) 3_675 . ?
O16 K1 O8W 121.1(2) 3_675 2_655 ?
O16 K1 O9W 86.96(18) 3_675 1_565 ?
O4W K1 K2 111.14(13) . 1_565 ?
O4W K1 K2 82.28(14) . 2_655 ?
O4W K1 Nb1 83.54(13) . 3_675 ?
O4W K1 Nb2 109.97(13) . 3_665 ?
O4W K1 O1 106.41(17) . 3_675 ?
O4W K1 O2 136.95(16) . 3_665 ?
O4W K1 O8W 57.2(2) . 2_655 ?
O8W K1 K2 132.99(16) 2_655 1_565 ?
O8W K1 K2 36.24(16) 2_655 2_655 ?
O8W K1 Nb1 140.7(2) 2_655 3_675 ?
O8W K1 Nb2 80.10(17) 2_655 3_665 ?
O8W K1 O1 156.7(2) 2_655 3_675 ?
O8W K1 O2 98.5(2) 2_655 3_665 ?
O9W K1 K2 42.96(14) 1_565 1_565 ?
O9W K1 K2 93.31(14) 1_565 2_655 ?
O9W K1 Nb1 86.75(14) 1_565 3_675 ?
O9W K1 Nb2 97.55(15) 1_565 3_665 ?
O9W K1 O1 74.47(17) 1_565 3_675 ?
O9W K1 O2 70.65(17) 1_565 3_665 ?
O9W K1 O4W 152.3(2) 1_565 . ?
O9W K1 O8W 128.1(2) 1_565 2_655 ?
O10W K1 K2 50.1(2) . 1_565 ?
O10W K1 K2 55.7(2) . 2_655 ?
O10W K1 Nb1 96.1(2) . 3_675 ?
O10W K1 Nb2 144.43(18) . 3_665 ?
O10W K1 O1 114.3(3) . 3_675 ?
O10W K1 O2 129.32(19) . 3_665 ?
O10W K1 O15 153.4(3) . . ?
O10W K1 O16 66.0(2) . 3_675 ?
O10W K1 O4W 85.9(2) . . ?
O10W K1 O8W 82.9(3) . 2_655 ?
O10W K1 O9W 69.4(2) . 1_565 ?
K1 K2 K1 111.29(5) 1_545 2_645 ?
Nb1 K2 K1 56.69(4) 3_665 1_545 ?
Nb1 K2 K1 134.90(6) 3_665 2_645 ?
Nb1 K2 Nb2 53.85(3) 3_665 3_665 ?
Nb1 K2 Nb3 52.46(3) 3_665 . ?
Nb2 K2 K1 107.11(5) 3_665 1_545 ?
Nb2 K2 K1 102.04(5) 3_665 2_645 ?
Nb3 K2 K1 70.85(5) . 1_545 ?
Nb3 K2 K1 82.48(5) . 2_645 ?
Nb3 K2 Nb2 51.51(3) . 3_665 ?
O11 K2 K1 89.42(11) 3_665 1_545 ?
O11 K2 K1 132.63(12) 3_665 2_645 ?
O11 K2 Nb1 33.17(10) 3_665 3_665 ?
O11 K2 Nb2 30.77(10) 3_665 3_665 ?
O11 K2 Nb3 64.21(11) 3_665 . ?
O11 K2 O14 56.35(14) 3_665 . ?
O11 K2 O10W 120.69(19) 3_665 1_545 ?
O14 K2 K1 100.81(11) . 1_545 ?
O14 K2 K1 77.59(11) . 2_645 ?
O14 K2 Nb1 64.73(10) . 3_665 ?
O14 K2 Nb2 29.72(10) . 3_665 ?
O14 K2 Nb3 30.81(10) . . ?
O14 K2 O10W 92.89(18) . 1_545 ?
O16 K2 K1 45.33(11) 3_665 1_545 ?
O16 K2 K1 106.61(12) 3_665 2_645 ?
O16 K2 Nb1 31.25(10) 3_665 3_665 ?
O16 K2 Nb2 63.94(11) 3_665 3_665 ?
O16 K2 Nb3 30.09(11) 3_665 . ?
O16 K2 O11 58.56(15) 3_665 3_665 ?
O16 K2 O14 56.51(15) 3_665 . ?
O16 K2 O10W 62.19(19) 3_665 1_545 ?
O7W K2 K1 146.52(17) . 1_545 ?
O7W K2 K1 87.4(2) . 2_645 ?
O7W K2 Nb1 127.6(2) . 3_665 ?
O7W K2 Nb2 95.03(17) . 3_665 ?
O7W K2 Nb3 141.27(17) . . ?
O7W K2 O11 97.9(2) . 3_665 ?
O7W K2 O14 110.48(19) . . ?
O7W K2 O16 156.4(2) . 3_665 ?
O7W K2 O10W 141.4(2) . 1_545 ?
O8W K2 K1 111.80(19) . 1_545 ?
O8W K2 K1 40.3(2) . 2_645 ?
O8W K2 Nb1 167.4(2) . 3_665 ?
O8W K2 Nb2 133.64(17) . 3_665 ?
O8W K2 Nb3 121.4(2) . . ?
O8W K2 O11 158.8(2) . 3_665 ?
O8W K2 O14 116.4(2) . . ?
O8W K2 O16 137.5(3) . 3_665 ?
O8W K2 O7W 64.6(3) . . ?
O8W K2 O10W 77.6(3) . 1_545 ?
O9W K2 K1 46.21(15) . 1_545 ?
O9W K2 K1 115.24(15) . 2_645 ?
O9W K2 Nb1 87.72(14) . 3_665 ?
O9W K2 Nb2 139.72(15) . 3_665 ?
O9W K2 Nb3 117.05(15) . . ?
O9W K2 O11 109.79(18) . 3_665 ?
O9W K2 O14 146.63(19) . . ?
O9W K2 O16 90.14(18) . 3_665 ?
O9W K2 O7W 101.1(2) . . ?
O9W K2 O8W 86.4(2) . . ?
O9W K2 O10W 67.3(2) . 1_545 ?
O10W K2 K1 43.85(17) 1_545 1_545 ?
O10W K2 K1 67.46(17) 1_545 2_645 ?
O10W K2 Nb1 89.78(16) 1_545 3_665 ?
O10W K2 Nb2 117.95(15) 1_545 3_665 ?
O10W K2 Nb3 66.44(15) 1_545 . ?
Nb1 Rh1 Nb2 66.43(2) . . ?
Nb1 Rh1 Nb3 66.26(2) . . ?
Nb2 Rh1 Nb3 66.29(2) . . ?
C11 Rh1 Nb1 106.4(2) . . ?
C11 Rh1 Nb2 159.5(2) . . ?
C11 Rh1 Nb3 130.1(2) . . ?
C11 Rh1 C13 66.4(3) . . ?
C11 Rh1 O11 122.1(3) . . ?
C11 Rh1 O12 101.4(3) . . ?
C11 Rh1 O13 160.1(3) . . ?
C12 Rh1 Nb1 133.2(2) . . ?
C12 Rh1 Nb2 157.0(2) . . ?
C12 Rh1 Nb3 107.6(2) . . ?
C12 Rh1 C11 40.0(3) . . ?
C12 Rh1 C13 39.3(3) . . ?
C12 Rh1 O11 162.0(3) . . ?
C12 Rh1 O12 103.9(3) . . ?
C12 Rh1 O13 120.8(3) . . ?
C13 Rh1 Nb1 172.2(2) . . ?
C13 Rh1 Nb2 121.3(2) . . ?
C13 Rh1 Nb3 115.6(2) . . ?
C13 Rh1 O11 145.5(3) . . ?
C13 Rh1 O12 136.0(3) . . ?
C13 Rh1 O13 101.0(3) . . ?
C14 Rh1 Nb1 141.7(2) . . ?
C14 Rh1 Nb2 106.7(2) . . ?
C14 Rh1 Nb3 148.3(2) . . ?
C14 Rh1 C11 66.3(3) . . ?
C14 Rh1 C12 66.1(3) . . ?
C14 Rh1 C13 39.4(3) . . ?
C14 Rh1 C15 39.5(3) . . ?
C14 Rh1 O11 109.4(3) . . ?
C14 Rh1 O12 167.6(2) . . ?
C14 Rh1 O13 114.6(2) . . ?
C15 Rh1 Nb1 110.6(2) . . ?
C15 Rh1 Nb2 123.4(2) . . ?
C15 Rh1 Nb3 168.6(2) . . ?
C15 Rh1 C11 39.0(3) . . ?
C15 Rh1 C12 65.9(3) . . ?
C15 Rh1 C13 66.0(3) . . ?
C15 Rh1 O11 99.1(3) . . ?
C15 Rh1 O12 130.9(3) . . ?
C15 Rh1 O13 151.6(3) . . ?
O11 Rh1 Nb1 40.35(13) . . ?
O11 Rh1 Nb2 39.99(14) . . ?
O11 Rh1 Nb3 85.27(13) . . ?
O11 Rh1 O12 77.77(19) . . ?
O11 Rh1 O13 77.17(19) . . ?
O12 Rh1 Nb1 40.53(13) . . ?
O12 Rh1 Nb2 85.32(14) . . ?
O12 Rh1 Nb3 39.58(13) . . ?
O13 Rh1 Nb1 85.05(14) . . ?
O13 Rh1 Nb2 40.22(13) . . ?
O13 Rh1 Nb3 39.65(13) . . ?
O13 Rh1 O12 76.45(19) . . ?
K1 Nb1 K2 64.95(4) 3_675 3_665 ?
Rh1 Nb1 K1 141.14(4) . 3_675 ?
Rh1 Nb1 K2 89.16(4) . 3_665 ?
Rh1 Nb1 Nb2 116.50(3) . 3_665 ?
Rh1 Nb1 Nb3 115.98(3) . 3_665 ?
Nb2 Nb1 K1 102.35(4) 3_665 3_675 ?
Nb2 Nb1 K2 127.76(4) 3_665 3_665 ?
Nb2 Nb1 Nb3 62.93(2) 3_665 3_665 ?
Nb3 Nb1 K1 80.15(4) 3_665 3_675 ?
Nb3 Nb1 K2 64.95(4) 3_665 3_665 ?
O1I Nb1 K1 124.67(4) . 3_675 ?
O1I Nb1 K2 97.17(4) . 3_665 ?
O1I Nb1 Rh1 85.05(2) . . ?
O1I Nb1 Nb2 46.461(16) . 3_665 ?
O1I Nb1 Nb3 46.510(16) . 3_665 ?
O1 Nb1 K1 54.20(18) . 3_675 ?
O1 Nb1 K2 81.10(18) . 3_665 ?
O1 Nb1 Rh1 95.34(18) . . ?
O1 Nb1 Nb2 134.48(18) . 3_665 ?
O1 Nb1 Nb3 131.95(18) . 3_665 ?
O1 Nb1 O1I 178.22(18) . . ?
O1 Nb1 O11 102.8(2) . . ?
O1 Nb1 O12 104.9(2) . . ?
O1 Nb1 O15 102.1(2) . . ?
O1 Nb1 O16 99.8(2) . . ?
O11 Nb1 K1 114.36(14) . 3_675 ?
O11 Nb1 K2 50.15(14) . 3_665 ?
O11 Nb1 Rh1 42.83(14) . . ?
O11 Nb1 Nb2 122.73(14) . 3_665 ?
O11 Nb1 Nb3 81.31(14) . 3_665 ?
O11 Nb1 O1I 76.34(14) . . ?
O11 Nb1 O12 82.56(19) . . ?
O12 Nb1 K1 154.35(14) . 3_675 ?
O12 Nb1 K2 131.87(14) . 3_665 ?
O12 Nb1 Rh1 43.12(14) . . ?
O12 Nb1 Nb2 81.91(14) . 3_665 ?
O12 Nb1 Nb3 123.02(14) . 3_665 ?
O12 Nb1 O1I 76.61(14) . . ?
O15 Nb1 K1 82.54(15) . 3_675 ?
O15 Nb1 K2 137.52(16) . 3_665 ?
O15 Nb1 Rh1 131.81(15) . . ?
O15 Nb1 Nb2 32.40(14) . 3_665 ?
O15 Nb1 Nb3 83.91(15) . 3_665 ?
O15 Nb1 O1I 78.86(14) . . ?
O15 Nb1 O11 155.0(2) . . ?
O15 Nb1 O12 88.8(2) . . ?
O15 Nb1 O16 90.3(2) . . ?
O16 Nb1 K1 49.76(15) . 3_675 ?
O16 Nb1 K2 48.03(15) . 3_665 ?
O16 Nb1 Rh1 130.52(16) . . ?
O16 Nb1 Nb2 83.99(15) . 3_665 ?
O16 Nb1 Nb3 32.11(15) . 3_665 ?
O16 Nb1 O1I 78.62(15) . . ?
O16 Nb1 O11 87.8(2) . . ?
O16 Nb1 O12 154.9(2) . . ?
K1 Nb2 K2 120.09(4) 3_665 3_665 ?
Rh1 Nb2 K1 141.77(4) . 3_665 ?
Rh1 Nb2 K2 86.09(4) . 3_665 ?
Rh1 Nb2 Nb1 115.94(3) . 3_665 ?
Rh1 Nb2 Nb3 115.25(3) . 3_665 ?
Nb1 Nb2 K1 73.23(3) 3_665 3_665 ?
Nb1 Nb2 K2 125.45(4) 3_665 3_665 ?
Nb1 Nb2 Nb3 62.63(2) 3_665 3_665 ?
Nb3 Nb2 K1 102.01(4) 3_665 3_665 ?
Nb3 Nb2 K2 62.84(3) 3_665 3_665 ?
O1I Nb2 K1 118.29(4) . 3_665 ?
O1I Nb2 K2 92.65(3) . 3_665 ?
O1I Nb2 Rh1 84.59(2) . . ?
O1I Nb2 Nb1 46.051(16) . 3_665 ?
O1I Nb2 Nb3 46.207(16) . 3_665 ?
O2 Nb2 K1 61.88(18) . 3_665 ?
O2 Nb2 K2 87.66(18) . 3_665 ?
O2 Nb2 Rh1 95.00(18) . . ?
O2 Nb2 Nb1 133.99(18) . 3_665 ?
O2 Nb2 Nb3 134.32(18) . 3_665 ?
O2 Nb2 O1I 179.47(19) . . ?
O2 Nb2 O11 103.8(2) . . ?
O2 Nb2 O13 103.1(2) . . ?
O2 Nb2 O14 102.4(2) . 3_665 ?
O2 Nb2 O15 101.5(2) . 3_665 ?
O11 Nb2 K1 162.83(14) . 3_665 ?
O11 Nb2 K2 46.09(14) . 3_665 ?
O11 Nb2 Rh1 42.61(14) . . ?
O11 Nb2 Nb1 122.07(14) . 3_665 ?
O11 Nb2 Nb3 80.96(15) . 3_665 ?
O11 Nb2 O1I 76.09(14) . . ?
O11 Nb2 O13 81.99(19) . . ?
O13 Nb2 K1 109.59(14) . 3_665 ?
O13 Nb2 K2 127.83(14) . 3_665 ?
O13 Nb2 Rh1 42.69(13) . . ?
O13 Nb2 Nb1 82.01(14) . 3_665 ?
O13 Nb2 Nb3 122.44(14) . 3_665 ?
O13 Nb2 O1I 76.37(14) . . ?
O14 Nb2 K1 87.21(15) 3_665 3_665 ?
O14 Nb2 K2 48.20(16) 3_665 3_665 ?
O14 Nb2 Rh1 129.31(15) 3_665 . ?
O14 Nb2 Nb1 84.19(15) 3_665 3_665 ?
O14 Nb2 Nb3 31.94(14) 3_665 3_665 ?
O14 Nb2 O1I 78.14(15) 3_665 . ?
O14 Nb2 O11 86.8(2) 3_665 . ?
O14 Nb2 O13 154.0(2) 3_665 . ?
O15 Nb2 K1 41.72(14) 3_665 3_665 ?
O15 Nb2 K2 138.95(16) 3_665 3_665 ?
O15 Nb2 Rh1 131.81(15) 3_665 . ?
O15 Nb2 Nb1 32.47(14) 3_665 3_665 ?
O15 Nb2 Nb3 83.64(15) 3_665 3_665 ?
O15 Nb2 O1I 78.52(14) 3_665 . ?
O15 Nb2 O11 154.4(2) 3_665 . ?
O15 Nb2 O13 89.3(2) 3_665 . ?
O15 Nb2 O14 90.8(2) 3_665 3_665 ?
Rh1 Nb3 K2 177.07(4) . . ?
Rh1 Nb3 Nb1 114.75(3) . 3_665 ?
Rh1 Nb3 Nb2 114.57(3) . 3_665 ?
Nb1 Nb3 K2 62.59(4) 3_665 . ?
Nb1 Nb3 Nb2 62.33(2) 3_665 3_665 ?
Nb2 Nb3 K2 65.64(3) 3_665 . ?
O1I Nb3 K2 94.60(4) . . ?
O1I Nb3 Rh1 83.87(2) . . ?
O1I Nb3 Nb1 45.662(16) . 3_665 ?
O1I Nb3 Nb2 45.768(16) . 3_665 ?
O3 Nb3 K2 86.12(18) . . ?
O3 Nb3 Rh1 95.39(18) . . ?
O3 Nb3 Nb1 134.49(18) . 3_665 ?
O3 Nb3 Nb2 135.10(18) . 3_665 ?
O3 Nb3 O1I 179.11(18) . . ?
O3 Nb3 O12 103.7(2) . . ?
O3 Nb3 O13 103.0(2) . . ?
O3 Nb3 O14 103.1(2) . . ?
O3 Nb3 O16 102.3(2) . 3_665 ?
O12 Nb3 K2 139.57(15) . . ?
O12 Nb3 Rh1 42.45(14) . . ?
O12 Nb3 Nb1 121.65(15) . 3_665 ?
O12 Nb3 Nb2 81.08(15) . 3_665 ?
O12 Nb3 O1I 76.08(14) . . ?
O12 Nb3 O13 81.63(19) . . ?
O13 Nb3 K2 134.96(14) . . ?
O13 Nb3 Rh1 42.24(13) . . ?
O13 Nb3 Nb1 81.51(14) . 3_665 ?
O13 Nb3 Nb2 121.71(14) . 3_665 ?
O13 Nb3 O1I 76.07(14) . . ?
O14 Nb3 K2 50.50(15) . . ?
O14 Nb3 Rh1 131.28(15) . . ?
O14 Nb3 Nb1 82.52(15) . 3_665 ?
O14 Nb3 Nb2 32.01(15) . 3_665 ?
O14 Nb3 O1I 77.76(15) . . ?
O14 Nb3 O12 89.1(2) . . ?
O14 Nb3 O13 153.6(2) . . ?
O16 Nb3 K2 46.04(15) 3_665 . ?
O16 Nb3 Rh1 131.07(15) 3_665 . ?
O16 Nb3 Nb1 32.18(14) 3_665 3_665 ?
O16 Nb3 Nb2 83.07(15) 3_665 3_665 ?
O16 Nb3 O1I 77.84(15) 3_665 . ?
O16 Nb3 O12 153.7(2) 3_665 . ?
O16 Nb3 O13 89.1(2) 3_665 . ?
O16 Nb3 O14 88.4(2) 3_665 . ?
C12 C11 Rh1 70.0(4) . . ?
C12 C11 C16 124.2(7) . . ?
C15 C11 Rh1 70.4(4) . . ?
C15 C11 C12 107.3(7) . . ?
C15 C11 C16 128.4(8) . . ?
C16 C11 Rh1 123.3(6) . . ?
C11 C12 Rh1 70.0(4) . . ?
C11 C12 C17 125.2(7) . . ?
C13 C12 Rh1 70.9(4) . . ?
C13 C12 C11 108.2(7) . . ?
C13 C12 C17 126.6(7) . . ?
C17 C12 Rh1 125.4(6) . . ?
C12 C13 Rh1 69.9(4) . . ?
C12 C13 C14 107.7(7) . . ?
C12 C13 C18 127.1(8) . . ?
C14 C13 Rh1 69.7(4) . . ?
C14 C13 C18 125.1(8) . . ?
C18 C13 Rh1 122.6(6) . . ?
C13 C14 Rh1 70.9(4) . . ?
C13 C14 C19 127.1(7) . . ?
C15 C14 Rh1 70.3(4) . . ?
C15 C14 C13 107.8(7) . . ?
C15 C14 C19 124.9(8) . . ?
C19 C14 Rh1 127.8(5) . . ?
C11 C15 Rh1 70.5(4) . . ?
C11 C15 C14 109.0(7) . . ?
C11 C15 C20 126.2(8) . . ?
C14 C15 Rh1 70.3(4) . . ?
C14 C15 C20 124.7(8) . . ?
C20 C15 Rh1 122.8(6) . . ?
Nb1 O1I Nb1 180.0 . 3_665 ?
Nb1 O1I Nb2 87.49(2) . 3_665 ?
Nb1 O1I Nb2 92.51(2) 3_665 3_665 ?
Nb1 O1I Nb2 92.51(2) . . ?
Nb1 O1I Nb2 87.49(2) 3_665 . ?
Nb1 O1I Nb3 92.17(2) . . ?
Nb1 O1I Nb3 87.83(2) 3_665 . ?
Nb1 O1I Nb3 87.83(2) . 3_665 ?
Nb1 O1I Nb3 92.17(2) 3_665 3_665 ?
Nb2 O1I Nb2 180.00(2) 3_665 . ?
Nb2 O1I Nb3 88.02(2) 3_665 . ?
Nb2 O1I Nb3 91.98(2) . . ?
Nb2 O1I Nb3 91.97(2) 3_665 3_665 ?
Nb2 O1I Nb3 88.03(2) . 3_665 ?
Nb3 O1I Nb3 180.0 . 3_665 ?
Nb1 O1 K1 97.1(2) . 3_675 ?
Nb2 O2 K1 91.1(2) . 3_665 ?
Rh1 O11 K2 147.8(2) . 3_665 ?
Nb1 O11 K2 96.68(19) . 3_665 ?
Nb1 O11 Rh1 96.8(2) . . ?
Nb2 O11 K2 103.14(19) . 3_665 ?
Nb2 O11 Rh1 97.4(2) . . ?
Nb2 O11 Nb1 114.9(2) . . ?
Nb1 O12 Rh1 96.4(2) . . ?
Nb3 O12 Rh1 98.0(2) . . ?
Nb3 O12 Nb1 114.9(2) . . ?
Nb2 O13 Rh1 97.1(2) . . ?
Nb3 O13 Rh1 98.1(2) . . ?
Nb3 O13 Nb2 115.2(2) . . ?
Nb2 O14 K2 102.1(2) 3_665 . ?
Nb3 O14 K2 98.7(2) . . ?
Nb3 O14 Nb2 116.0(2) . 3_665 ?
Nb1 O15 K1 131.8(2) . . ?
Nb2 O15 K1 110.1(2) 3_665 . ?
Nb2 O15 Nb1 115.1(2) 3_665 . ?
K2 O16 K1 89.34(15) 3_665 3_675 ?
Nb1 O16 K1 98.1(2) . 3_675 ?
Nb1 O16 K2 100.7(2) . 3_665 ?
Nb3 O16 K1 140.0(2) 3_665 3_675 ?
Nb3 O16 K2 103.9(2) 3_665 3_665 ?
Nb3 O16 Nb1 115.7(2) 3_665 . ?
K2 O8W K1 103.4(3) . 2_645 ?
K2 O9W K1 90.8(2) . 1_545 ?
K1 O10W K2 86.0(2) . 1_565 ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.936
_refine_diff_density_min         -1.700
_refine_diff_density_rms         0.274
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: H2O/acetone'
_chemical_properties_physical    Moisture-sensitive
_database_code_depnum_ccdc_archive 'CCDC 1016219'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_308
#complex 2
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_sum            'C20 H66 Cs4 O37 Rh2 Ta6'
_chemical_formula_weight         2721.89

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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5851(10)
_cell_length_b                   10.5155(11)
_cell_length_c                   14.6458(15)
_cell_angle_alpha                95.814(3)
_cell_angle_beta                 99.365(3)
_cell_angle_gamma                98.708(3)
_cell_volume                     1427.7(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150.0(2)
_cell_measurement_reflns_used    1484
_cell_measurement_theta_min      2.3817
_cell_measurement_theta_max      27.2436

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    3.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1230
_exptl_absorpt_coefficient_mu    14.609
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5958
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'based on intensities (SADABS, Bruker, 2005)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex2 Duo CCD detector'
_diffrn_measurement_method       'combined omega- and phi-scans'
_diffrn_detector_area_resol_mean 25
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8488
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         27.51
_reflns_number_total             6435
_reflns_number_gt                4679
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2 V.1.27 (Bruker, 2005)'
_computing_cell_refinement       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_reduction        'Apex2 V.1.27 (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V6.22 (Bruker, 2000-2005)'
_computing_publication_material  'local programs'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0387P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6435
_refine_ls_number_parameters     327
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1061
_refine_ls_wR_factor_gt          0.0937
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.040
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 0.76443(10) 0.93594(8) 0.18570(7) 0.0295(2) Uani 1 1 d . . .
Cs2 Cs 0.04449(10) 0.77403(10) -0.00065(8) 0.0399(3) Uani 1 1 d . . .
Ta1 Ta 0.39765(5) 0.63938(4) 0.10014(3) 0.00899(12) Uani 1 1 d . . .
Ta2 Ta 0.42936(6) 0.31461(4) 0.07602(3) 0.01327(12) Uani 1 1 d . . .
Ta3 Ta 0.72793(5) 0.54954(5) 0.09885(3) 0.01421(13) Uani 1 1 d . . .
O1M O 0.5000 0.5000 0.0000 0.007(2) Uani 1 2 d SU . .
Rh1 Rh 0.55176(14) 0.50788(10) 0.26097(6) 0.0254(3) Uani 1 1 d . . .
O1 O 0.3225(9) 0.7453(7) 0.1767(6) 0.0158(19) Uani 1 1 d . . .
O2 O 0.3768(12) 0.1782(8) 0.1339(6) 0.029(2) Uani 1 1 d U . .
O3 O 0.8975(10) 0.5911(10) 0.1757(6) 0.034(3) Uani 1 1 d . . .
O4 O 0.3684(9) 0.4650(7) 0.1505(6) 0.0160(19) Uani 1 1 d . . .
O5 O 0.6005(9) 0.6461(7) 0.1700(5) 0.0141(18) Uani 1 1 d . . .
O6 O 0.6236(9) 0.3962(7) 0.1521(5) 0.0139(18) Uani 1 1 d U . .
O11 O 0.7647(9) 0.4296(8) 0.0002(6) 0.0153(18) Uani 1 1 d U . .
O12 O 0.7385(8) 0.6886(7) 0.0211(6) 0.0135(18) Uani 1 1 d . . .
O13 O 0.4747(9) 0.7595(7) 0.0200(5) 0.0109(17) Uani 1 1 d . . .
C11 C 0.472(2) 0.5681(15) 0.3826(10) 0.041(4) Uani 1 1 d U . .
C12 C 0.613(2) 0.6313(15) 0.3903(9) 0.038(4) Uani 1 1 d U . .
C13 C 0.701(2) 0.5331(15) 0.3874(9) 0.038(4) Uani 1 1 d U . .
C14 C 0.608(2) 0.4057(14) 0.3762(9) 0.041(4) Uani 1 1 d U . .
C15 C 0.473(2) 0.4277(15) 0.3726(10) 0.037(4) Uani 1 1 d U . .
C16 C 0.337(2) 0.6293(19) 0.3809(12) 0.067(6) Uani 1 1 d U . .
H16A H 0.3270 0.6573 0.4450 0.101 Uiso 1 1 calc R . .
H16B H 0.2532 0.5654 0.3503 0.101 Uiso 1 1 calc R . .
H16C H 0.3452 0.7044 0.3464 0.101 Uiso 1 1 calc R . .
C17 C 0.666(2) 0.7728(15) 0.3979(10) 0.056(5) Uani 1 1 d U . .
H17A H 0.7631 0.7876 0.3837 0.084 Uiso 1 1 calc R . .
H17B H 0.6676 0.8131 0.4615 0.084 Uiso 1 1 calc R . .
H17C H 0.6019 0.8112 0.3536 0.084 Uiso 1 1 calc R . .
C18 C 0.858(2) 0.5554(18) 0.3972(13) 0.071(6) Uani 1 1 d U . .
H18A H 0.8892 0.6289 0.3648 0.106 Uiso 1 1 calc R . .
H18B H 0.8889 0.4775 0.3698 0.106 Uiso 1 1 calc R . .
H18C H 0.9020 0.5745 0.4635 0.106 Uiso 1 1 calc R . .
C19 C 0.659(2) 0.2800(14) 0.3702(12) 0.055(5) Uani 1 1 d U . .
H19A H 0.6304 0.2321 0.4201 0.083 Uiso 1 1 calc R . .
H19B H 0.7638 0.2951 0.3771 0.083 Uiso 1 1 calc R . .
H19C H 0.6166 0.2294 0.3095 0.083 Uiso 1 1 calc R . .
C20 C 0.341(2) 0.3272(17) 0.3614(11) 0.055(5) Uani 1 1 d U . .
H20A H 0.3650 0.2408 0.3485 0.082 Uiso 1 1 calc R . .
H20B H 0.2694 0.3424 0.3094 0.082 Uiso 1 1 calc R . .
H20C H 0.3009 0.3327 0.4190 0.082 Uiso 1 1 calc R . .
O1W O 0.4046(11) 0.0151(11) 0.4231(6) 0.037(3) Uani 1 1 d . . .
O2W O 0.4652(10) 0.9898(8) 0.2415(6) 0.022(2) Uani 1 1 d . . .
O3W O 0.0997(12) 0.0463(9) 0.1391(7) 0.036(3) Uani 1 1 d . . .
O4W O 0.3228(11) 0.9572(9) -0.0080(7) 0.030(2) Uani 1 1 d . . .
O5W O 1.0845(13) 0.8017(11) 0.2428(8) 0.050(3) Uani 1 1 d . . .
O6W O 1.0830(12) 0.4175(11) 0.1916(10) 0.059(4) Uani 1 1 d . . .
O7W O 0.8762(14) 1.0828(14) 0.5771(10) 0.075(5) Uani 1 1 d . . .
O8W O 0.9448(17) 1.0962(16) 0.3981(11) 0.096(6) Uani 1 1 d . . .
O9WA O 0.850(2) 0.2487(18) 0.2256(13) 0.028(5) Uani 0.50 1 d P . .
O9WB O 0.9756(19) 0.195(2) 0.2541(12) 0.029(5) Uani 0.50 1 d P . .


_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
Cs1 Cs2 4.5143(15) 1_655 ?
Cs1 Cs2 4.6475(14) 2_675 ?
Cs1 O5 3.178(8) . ?
Cs1 O2W 3.222(9) . ?
Cs1 O4W 2.984(10) 2_675 ?
Cs1 O9WA 3.235(18) 1_565 ?
Cs1 O9WB 3.10(2) 1_565 ?
Cs2 Cs1 4.5144(14) 1_455 ?
Cs2 Cs1 4.6475(14) 2_675 ?
Cs2 Ta1 3.9864(11) . ?
Cs2 O11 3.019(8) 2_665 ?
Cs2 O12 3.013(8) 1_455 ?
Cs2 O3W 3.201(10) 2_565 ?
Cs2 O4W 3.069(10) . ?
Cs2 O6W 3.221(15) 2_665 ?
Ta1 Ta2 3.3229(7) 2_665 ?
Ta1 Ta3 3.2939(7) 2_665 ?
Ta1 O1M 2.3936(5) . ?
Ta1 Rh1 3.1287(11) . ?
Ta1 O1 1.808(8) . ?
Ta1 O4 2.043(8) . ?
Ta1 O5 2.032(8) . ?
Ta1 O11 1.950(8) 2_665 ?
Ta1 O13 1.954(8) . ?
Ta2 Ta1 3.3229(7) 2_665 ?
Ta2 Ta3 3.3181(8) 2_665 ?
Ta2 O1M 2.4050(5) . ?
Ta2 Rh1 3.1579(11) . ?
Ta2 O2 1.788(9) . ?
Ta2 O4 2.042(8) . ?
Ta2 O6 2.022(8) . ?
Ta2 O12 1.960(8) 2_665 ?
Ta2 O13 1.962(8) 2_665 ?
Ta3 Ta1 3.2939(7) 2_665 ?
Ta3 Ta2 3.3180(8) 2_665 ?
Ta3 O1M 2.3693(5) . ?
Ta3 Rh1 3.1581(13) . ?
Ta3 O3 1.786(9) . ?
Ta3 O5 2.045(8) . ?
Ta3 O6 2.057(9) . ?
Ta3 O11 1.933(7) . ?
Ta3 O12 1.943(8) . ?
O1M Ta1 2.3937(5) 2_665 ?
O1M Ta2 2.4050(5) 2_665 ?
O1M Ta3 2.3693(5) 2_665 ?
Rh1 O4 2.144(8) . ?
Rh1 O5 2.121(8) . ?
Rh1 O6 2.149(7) . ?
Rh1 C11 2.125(14) . ?
Rh1 C12 2.128(13) . ?
Rh1 C13 2.112(14) . ?
Rh1 C14 2.131(14) . ?
Rh1 C15 2.107(15) . ?
O11 Cs2 3.019(8) 2_665 ?
O11 Ta1 1.950(8) 2_665 ?
O12 Cs2 3.013(8) 1_655 ?
O12 Ta2 1.960(8) 2_665 ?
O13 Ta2 1.962(8) 2_665 ?
C11 C12 1.40(2) . ?
C11 C15 1.47(2) . ?
C11 C16 1.53(2) . ?
C12 C13 1.42(2) . ?
C12 C17 1.48(2) . ?
C13 C14 1.47(2) . ?
C13 C18 1.48(3) . ?
C14 C15 1.34(2) . ?
C14 C19 1.476(18) . ?
C15 C20 1.50(2) . ?
O3W Cs2 3.201(10) 2_565 ?
O4W Cs1 2.984(10) 2_675 ?
O6W Cs2 3.221(15) 2_665 ?
O9WA Cs1 3.235(18) 1_545 ?
O9WA O9WB 1.42(3) . ?
O9WB Cs1 3.10(2) 1_545 ?

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
Cs2 Cs1 Cs2 65.42(3) 1_655 2_675 ?
O5 Cs1 Cs2 86.19(15) . 1_655 ?
O5 Cs1 Cs2 140.32(14) . 2_675 ?
O5 Cs1 O2W 80.0(2) . . ?
O5 Cs1 O9WA 163.4(4) . 1_565 ?
O2W Cs1 Cs2 155.17(15) . 1_655 ?
O2W Cs1 Cs2 114.38(16) . 2_675 ?
O2W Cs1 O9WA 83.5(4) . 1_565 ?
O4W Cs1 Cs2 77.56(18) 2_675 1_655 ?
O4W Cs1 Cs2 40.51(19) 2_675 2_675 ?
O4W Cs1 O5 109.1(2) 2_675 . ?
O4W Cs1 O2W 87.5(2) 2_675 . ?
O4W Cs1 O9WA 72.0(4) 2_675 1_565 ?
O4W Cs1 O9WB 87.8(4) 2_675 1_565 ?
O9WA Cs1 Cs2 109.9(3) 1_565 1_655 ?
O9WA Cs1 Cs2 50.4(3) 1_565 2_675 ?
O9WB Cs1 Cs2 94.6(3) 1_565 1_655 ?
O9WB Cs1 Cs2 53.2(3) 1_565 2_675 ?
O9WB Cs1 O5 162.8(4) 1_565 . ?
O9WB Cs1 O2W 104.6(4) 1_565 . ?
O9WB Cs1 O9WA 25.9(5) 1_565 1_565 ?
Cs1 Cs2 Cs1 114.58(3) 1_455 2_675 ?
Ta1 Cs2 Cs1 122.39(3) . 1_455 ?
Ta1 Cs2 Cs1 99.57(2) . 2_675 ?
O11 Cs2 Cs1 137.79(17) 2_665 1_455 ?
O11 Cs2 Cs1 103.34(17) 2_665 2_675 ?
O11 Cs2 Ta1 28.26(15) 2_665 . ?
O11 Cs2 O3W 139.9(2) 2_665 2_565 ?
O11 Cs2 O4W 83.3(2) 2_665 . ?
O11 Cs2 O6W 75.4(2) 2_665 2_665 ?
O12 Cs2 Cs1 47.20(14) 1_455 1_455 ?
O12 Cs2 Cs1 130.56(16) 1_455 2_675 ?
O12 Cs2 Ta1 129.55(16) 1_455 . ?
O12 Cs2 O11 117.2(2) 1_455 2_665 ?
O12 Cs2 O3W 82.7(3) 1_455 2_565 ?
O12 Cs2 O4W 159.0(2) 1_455 . ?
O12 Cs2 O6W 78.2(2) 1_455 2_665 ?
O3W Cs2 Cs1 81.76(18) 2_565 1_455 ?
O3W Cs2 Cs1 47.9(2) 2_565 2_675 ?
O3W Cs2 Ta1 147.3(2) 2_565 . ?
O3W Cs2 O6W 75.5(2) 2_565 2_665 ?
O4W Cs2 Cs1 114.86(17) . 1_455 ?
O4W Cs2 Cs1 39.17(19) . 2_675 ?
O4W Cs2 Ta1 66.68(19) . . ?
O4W Cs2 O3W 83.7(3) . 2_565 ?
O4W Cs2 O6W 113.6(3) . 2_665 ?
O6W Cs2 Cs1 123.03(19) 2_665 1_455 ?
O6W Cs2 Cs1 86.45(18) 2_665 2_675 ?
O6W Cs2 Ta1 103.09(18) 2_665 . ?
Ta2 Ta1 Cs2 97.84(2) 2_665 . ?
Ta3 Ta1 Cs2 76.66(2) 2_665 . ?
Ta3 Ta1 Ta2 62.507(16) 2_665 2_665 ?
O1M Ta1 Cs2 120.02(2) . . ?
O1M Ta1 Ta2 46.315(12) . 2_665 ?
O1M Ta1 Ta3 45.941(12) . 2_665 ?
O1M Ta1 Rh1 84.83(2) . . ?
Rh1 Ta1 Cs2 146.11(3) . . ?
Rh1 Ta1 Ta2 115.96(3) . 2_665 ?
Rh1 Ta1 Ta3 115.74(3) . 2_665 ?
O1 Ta1 Cs2 60.6(3) . . ?
O1 Ta1 Ta2 133.6(3) . 2_665 ?
O1 Ta1 Ta3 134.8(3) . 2_665 ?
O1 Ta1 O1M 179.3(3) . . ?
O1 Ta1 Rh1 94.7(3) . . ?
O1 Ta1 O4 104.2(3) . . ?
O1 Ta1 O5 103.4(3) . . ?
O1 Ta1 O11 103.0(3) . 2_665 ?
O1 Ta1 O13 101.6(3) . . ?
O4 Ta1 Cs2 116.7(2) . . ?
O4 Ta1 Ta2 122.1(2) . 2_665 ?
O4 Ta1 Ta3 81.2(2) . 2_665 ?
O4 Ta1 O1M 75.9(2) . . ?
O4 Ta1 Rh1 42.9(2) . . ?
O5 Ta1 Cs2 157.4(2) . . ?
O5 Ta1 Ta2 81.8(2) . 2_665 ?
O5 Ta1 Ta3 121.7(2) . 2_665 ?
O5 Ta1 O1M 75.9(2) . . ?
O5 Ta1 Rh1 42.2(2) . . ?
O5 Ta1 O4 81.4(3) . . ?
O11 Ta1 Cs2 47.1(2) 2_665 . ?
O11 Ta1 Ta2 83.1(2) 2_665 2_665 ?
O11 Ta1 Ta3 31.8(2) 2_665 2_665 ?
O11 Ta1 O1M 77.8(2) 2_665 . ?
O11 Ta1 Rh1 131.0(3) 2_665 . ?
O11 Ta1 O4 88.3(3) 2_665 . ?
O11 Ta1 O5 153.3(3) 2_665 . ?
O11 Ta1 O13 89.7(3) 2_665 . ?
O13 Ta1 Cs2 79.7(2) . . ?
O13 Ta1 Ta2 32.0(2) . 2_665 ?
O13 Ta1 Ta3 83.5(2) . 2_665 ?
O13 Ta1 O1M 78.3(2) . . ?
O13 Ta1 Rh1 131.0(2) . . ?
O13 Ta1 O4 153.9(3) . . ?
O13 Ta1 O5 89.0(3) . . ?
Ta3 Ta2 Ta1 62.405(17) 2_665 2_665 ?
O1M Ta2 Ta1 46.034(12) . 2_665 ?
O1M Ta2 Ta3 45.533(13) . 2_665 ?
O1M Ta2 Rh1 84.00(3) . . ?
Rh1 Ta2 Ta1 115.37(3) . 2_665 ?
Rh1 Ta2 Ta3 114.25(3) . 2_665 ?
O2 Ta2 Ta1 134.7(3) . 2_665 ?
O2 Ta2 Ta3 134.7(3) . 2_665 ?
O2 Ta2 O1M 179.2(3) . . ?
O2 Ta2 Rh1 95.3(3) . . ?
O2 Ta2 O4 103.7(3) . . ?
O2 Ta2 O6 103.3(4) . . ?
O2 Ta2 O12 103.1(4) . 2_665 ?
O2 Ta2 O13 102.8(3) . 2_665 ?
O4 Ta2 Ta1 121.6(2) . 2_665 ?
O4 Ta2 Ta3 80.6(2) . 2_665 ?
O4 Ta2 O1M 75.6(2) . . ?
O4 Ta2 Rh1 42.3(2) . . ?
O6 Ta2 Ta1 82.1(2) . 2_665 ?
O6 Ta2 Ta3 121.8(2) . 2_665 ?
O6 Ta2 O1M 76.4(2) . . ?
O6 Ta2 Rh1 42.3(2) . . ?
O6 Ta2 O4 81.4(3) . . ?
O12 Ta2 Ta1 82.2(2) 2_665 2_665 ?
O12 Ta2 Ta3 31.6(2) 2_665 2_665 ?
O12 Ta2 O1M 77.1(2) 2_665 . ?
O12 Ta2 Rh1 130.6(2) 2_665 . ?
O12 Ta2 O4 88.6(3) 2_665 . ?
O12 Ta2 O6 153.3(3) 2_665 . ?
O12 Ta2 O13 88.6(3) 2_665 2_665 ?
O13 Ta2 Ta1 31.9(2) 2_665 2_665 ?
O13 Ta2 Ta3 83.2(2) 2_665 2_665 ?
O13 Ta2 O1M 77.9(2) 2_665 . ?
O13 Ta2 Rh1 131.4(2) 2_665 . ?
O13 Ta2 O4 153.3(3) 2_665 . ?
O13 Ta2 O6 89.4(3) 2_665 . ?
Ta1 Ta3 Ta2 63.146(16) 2_665 2_665 ?
O1M Ta3 Ta1 46.552(12) . 2_665 ?
O1M Ta3 Ta2 46.418(13) . 2_665 ?
O1M Ta3 Rh1 84.56(3) . . ?
Rh1 Ta3 Ta1 116.19(3) . 2_665 ?
Rh1 Ta3 Ta2 115.28(3) . 2_665 ?
O3 Ta3 Ta1 135.4(3) . 2_665 ?
O3 Ta3 Ta2 133.2(4) . 2_665 ?
O3 Ta3 O1M 178.0(3) . . ?
O3 Ta3 Rh1 94.2(3) . . ?
O3 Ta3 O5 101.9(4) . . ?
O3 Ta3 O6 103.6(4) . . ?
O3 Ta3 O11 103.3(4) . . ?
O3 Ta3 O12 101.3(4) . . ?
O5 Ta3 Ta1 122.6(2) . 2_665 ?
O5 Ta3 Ta2 81.7(2) . 2_665 ?
O5 Ta3 O1M 76.2(2) . . ?
O5 Ta3 Rh1 41.6(2) . . ?
O5 Ta3 O6 80.9(3) . . ?
O6 Ta3 Ta1 82.4(2) . 2_665 ?
O6 Ta3 Ta2 122.8(2) . 2_665 ?
O6 Ta3 O1M 76.6(2) . . ?
O6 Ta3 Rh1 42.4(2) . . ?
O11 Ta3 Ta1 32.1(2) . 2_665 ?
O11 Ta3 Ta2 83.9(3) . 2_665 ?
O11 Ta3 O1M 78.7(2) . . ?
O11 Ta3 Rh1 131.8(3) . . ?
O11 Ta3 O5 154.6(3) . . ?
O11 Ta3 O6 89.5(3) . . ?
O11 Ta3 O12 91.0(3) . . ?
O12 Ta3 Ta1 84.5(2) . 2_665 ?
O12 Ta3 Ta2 31.9(2) . 2_665 ?
O12 Ta3 O1M 78.3(2) . . ?
O12 Ta3 Rh1 129.3(2) . . ?
O12 Ta3 O5 87.8(3) . . ?
O12 Ta3 O6 154.3(3) . . ?
Ta1 O1M Ta1 180.0 . 2_665 ?
Ta1 O1M Ta2 87.651(17) . 2_665 ?
Ta1 O1M Ta2 92.348(18) 2_665 2_665 ?
Ta1 O1M Ta2 92.348(17) . . ?
Ta1 O1M Ta2 87.652(17) 2_665 . ?
Ta2 O1M Ta2 180.000(13) 2_665 . ?
Ta3 O1M Ta1 92.493(17) . . ?
Ta3 O1M Ta1 87.507(18) 2_665 . ?
Ta3 O1M Ta1 87.508(18) . 2_665 ?
Ta3 O1M Ta1 92.493(18) 2_665 2_665 ?
Ta3 O1M Ta2 88.049(19) . 2_665 ?
Ta3 O1M Ta2 91.952(19) 2_665 2_665 ?
Ta3 O1M Ta2 91.951(19) . . ?
Ta3 O1M Ta2 88.049(19) 2_665 . ?
Ta3 O1M Ta3 180.0 . 2_665 ?
Ta1 Rh1 Ta2 66.83(2) . . ?
Ta1 Rh1 Ta3 66.35(2) . . ?
Ta2 Rh1 Ta3 65.85(2) . . ?
O4 Rh1 Ta1 40.4(2) . . ?
O4 Rh1 Ta2 39.8(2) . . ?
O4 Rh1 Ta3 84.6(2) . . ?
O4 Rh1 O6 76.3(3) . . ?
O5 Rh1 Ta1 40.1(2) . . ?
O5 Rh1 Ta2 85.0(2) . . ?
O5 Rh1 Ta3 39.8(2) . . ?
O5 Rh1 O4 77.1(3) . . ?
O5 Rh1 O6 77.1(3) . . ?
O5 Rh1 C11 118.7(5) . . ?
O5 Rh1 C12 99.0(5) . . ?
O5 Rh1 C14 152.5(6) . . ?
O6 Rh1 Ta1 85.5(2) . . ?
O6 Rh1 Ta2 39.3(2) . . ?
O6 Rh1 Ta3 40.2(2) . . ?
C11 Rh1 Ta1 106.2(4) . . ?
C11 Rh1 Ta2 135.6(5) . . ?
C11 Rh1 Ta3 154.6(5) . . ?
C11 Rh1 O4 105.5(6) . . ?
C11 Rh1 O6 164.2(5) . . ?
C11 Rh1 C12 38.4(7) . . ?
C11 Rh1 C14 65.5(6) . . ?
C12 Rh1 Ta1 113.4(4) . . ?
C12 Rh1 Ta2 173.9(5) . . ?
C12 Rh1 Ta3 120.1(5) . . ?
C12 Rh1 O4 136.5(5) . . ?
C12 Rh1 O6 146.0(5) . . ?
C12 Rh1 C14 67.0(5) . . ?
C13 Rh1 Ta1 147.1(4) . . ?
C13 Rh1 Ta2 142.7(4) . . ?
C13 Rh1 Ta3 107.5(5) . . ?
C13 Rh1 O4 167.5(6) . . ?
C13 Rh1 O5 113.9(5) . . ?
C13 Rh1 O6 111.1(5) . . ?
C13 Rh1 C11 64.7(7) . . ?
C13 Rh1 C12 39.3(6) . . ?
C13 Rh1 C14 40.5(6) . . ?
C14 Rh1 Ta1 166.8(6) . . ?
C14 Rh1 Ta2 111.2(4) . . ?
C14 Rh1 Ta3 125.6(5) . . ?
C14 Rh1 O4 129.7(5) . . ?
C14 Rh1 O6 101.0(5) . . ?
C15 Rh1 Ta1 130.3(5) . . ?
C15 Rh1 Ta2 108.6(4) . . ?
C15 Rh1 Ta3 160.5(5) . . ?
C15 Rh1 O4 102.9(5) . . ?
C15 Rh1 O5 159.1(5) . . ?
C15 Rh1 O6 123.5(5) . . ?
C15 Rh1 C11 40.7(6) . . ?
C15 Rh1 C12 66.3(6) . . ?
C15 Rh1 C13 64.7(7) . . ?
C15 Rh1 C14 36.9(7) . . ?
Ta1 O4 Rh1 96.7(3) . . ?
Ta2 O4 Ta1 115.9(4) . . ?
Ta2 O4 Rh1 97.9(4) . . ?
Ta1 O5 Cs1 107.5(3) . . ?
Ta1 O5 Ta3 115.1(3) . . ?
Ta1 O5 Rh1 97.8(4) . . ?
Ta3 O5 Cs1 100.4(3) . . ?
Ta3 O5 Rh1 98.6(3) . . ?
Rh1 O5 Cs1 137.9(3) . . ?
Ta2 O6 Ta3 114.6(4) . . ?
Ta2 O6 Rh1 98.4(3) . . ?
Ta3 O6 Rh1 97.3(3) . . ?
Ta1 O11 Cs2 104.6(3) 2_665 2_665 ?
Ta3 O11 Cs2 132.2(4) . 2_665 ?
Ta3 O11 Ta1 116.0(4) . 2_665 ?
Ta2 O12 Cs2 124.4(4) 2_665 1_655 ?
Ta3 O12 Cs2 110.1(3) . 1_655 ?
Ta3 O12 Ta2 116.4(4) . 2_665 ?
Ta1 O13 Ta2 116.1(4) . 2_665 ?
C12 C11 Rh1 70.9(9) . . ?
C12 C11 C15 107.7(15) . . ?
C12 C11 C16 127.7(15) . . ?
C15 C11 Rh1 69.0(8) . . ?
C15 C11 C16 124.6(18) . . ?
C16 C11 Rh1 123.9(11) . . ?
C11 C12 Rh1 70.7(8) . . ?
C11 C12 C13 106.8(15) . . ?
C11 C12 C17 127.7(16) . . ?
C13 C12 Rh1 69.8(8) . . ?
C13 C12 C17 125.4(18) . . ?
C17 C12 Rh1 123.5(11) . . ?
C12 C13 Rh1 71.0(8) . . ?
C12 C13 C14 108.8(16) . . ?
C12 C13 C18 125.7(16) . . ?
C14 C13 Rh1 70.4(8) . . ?
C14 C13 C18 125.5(16) . . ?
C18 C13 Rh1 126.1(12) . . ?
C13 C14 Rh1 69.1(8) . . ?
C13 C14 C19 124.9(18) . . ?
C15 C14 Rh1 70.6(9) . . ?
C15 C14 C13 106.8(14) . . ?
C15 C14 C19 128.3(17) . . ?
C19 C14 Rh1 125.2(11) . . ?
C11 C15 Rh1 70.3(9) . . ?
C11 C15 C20 123.6(16) . . ?
C14 C15 Rh1 72.5(10) . . ?
C14 C15 C11 109.9(16) . . ?
C14 C15 C20 126.5(15) . . ?
C20 C15 Rh1 124.2(11) . . ?
Cs1 O4W Cs2 100.3(3) 2_675 . ?
O9WB O9WA Cs1 71.8(11) . 1_545 ?
O9WA O9WB Cs1 82.3(11) . 1_545 ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         2.096
_refine_diff_density_min         -3.680
_refine_diff_density_rms         0.383



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: H2O/acetone'
_chemical_properties_physical    Moisture-sensitive
_database_code_depnum_ccdc_archive 'CCDC 1016220'
