# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1840551'
_audit_update_record             
;
2018-08-30 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H100 O52 Rh4 W8'
_chemical_formula_weight         3295.63

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'
W W -0.8490 6.8722 '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/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   12.461(2)
_cell_length_b                   15.509(3)
_cell_length_c                   22.269(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.352(3)
_cell_angle_gamma                90
_cell_volume                     4246.3(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    25416
_cell_measurement_theta_min      1.607
_cell_measurement_theta_max      27.497

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.578
_exptl_crystal_F_000             3056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    11.632
_shelx_estimated_absorpt_T_min   0.110
_shelx_estimated_absorpt_T_max   0.242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4117
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25416
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.607
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9603
_reflns_number_gt                7495
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL-2016/6, PLATON, WINGX (Ferrugia, 2012)'
_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)+(0.0520P)²+31.7187P] 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         9603
_refine_ls_number_parameters     480
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.1086
_refine_ls_wR_factor_gt          0.1017
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
W1 W 0.53260(3) 0.33782(2) 0.07394(2) 0.02318(10) Uani 1 1 d . . . . .
W2 W 0.46200(3) 0.70486(2) 0.08861(2) 0.02133(9) Uani 1 1 d . . . . .
W3 W 0.49496(3) 0.52360(2) 0.17119(2) 0.02162(9) Uani 1 1 d . . . . .
W4 W 0.33640(3) 0.52105(2) 0.03127(2) 0.01969(9) Uani 1 1 d . . . . .
Rh6 Rh 0.26513(6) 0.61944(5) 0.14271(3) 0.02525(16) Uani 1 1 d . . . . .
Rh5 Rh 0.70846(6) 0.68634(5) 0.20073(3) 0.02649(17) Uani 1 1 d . . . . .
O1 O 0.3177(5) 0.6425(4) 0.0593(3) 0.0217(13) Uani 1 1 d . . . . .
O2 O 0.4000(6) 0.8024(4) 0.0983(3) 0.0331(16) Uani 1 1 d . . . . .
O3 O 0.5348(6) 0.4184(4) 0.1405(3) 0.0278(15) Uani 1 1 d . . . . .
O4 O 0.4347(5) 0.6440(4) 0.1636(3) 0.0223(13) Uani 1 1 d . . . . .
O5 O 0.2013(6) 0.4971(5) 0.0072(3) 0.0320(16) Uani 1 1 d . . . . .
O6 O 0.4408(7) 0.2667(5) 0.0970(3) 0.0424(19) Uani 1 1 d . . . . .
O7 O 0.5015(5) 0.5687(4) 0.0778(3) 0.0206(13) Uani 1 1 d . . . . .
O8 O 0.3426(5) 0.5050(4) 0.1217(3) 0.0230(13) Uani 1 1 d . . . . .
O9 O 0.3791(5) 0.5647(4) -0.0361(3) 0.0242(14) Uani 1 1 d . . . . .
O10 O 0.4009(5) 0.4160(4) 0.0306(3) 0.0216(13) Uani 1 1 d . . . . .
O11 O 0.6258(5) 0.5678(4) 0.1922(3) 0.0288(15) Uani 1 1 d . . . . .
O12 O 0.5993(5) 0.7226(4) 0.1220(3) 0.0280(15) Uani 1 1 d . . . . .
O13 O 0.6530(6) 0.2886(5) 0.1011(3) 0.0382(18) Uani 1 1 d D . . . .
O14 O 0.8082(6) 0.6332(5) 0.1389(3) 0.042(2) Uani 1 1 d . . . . .
O15 O 0.4799(5) 0.7115(4) 0.0079(3) 0.0252(14) Uani 1 1 d . . . . .
O16 O 0.4580(6) 0.4951(5) 0.2402(3) 0.0347(17) Uani 1 1 d . . . . .
C20 C 0.1865(9) 0.7164(7) 0.1861(5) 0.036(3) Uani 1 1 d . . . . .
C21 C 0.2051(10) 0.6437(8) 0.2250(5) 0.044(3) Uani 1 1 d . . . . .
C23 C 0.7413(12) 0.8093(7) 0.2383(5) 0.046(3) Uani 1 1 d . . . . .
C24 C 0.0973(9) 0.6018(9) 0.1377(7) 0.056(4) Uani 1 1 d . . . . .
C25 C 0.1487(12) 0.5746(9) 0.1941(8) 0.062(4) Uani 1 1 d . . . . .
C26 C 0.6602(10) 0.7683(10) 0.2671(6) 0.051(4) Uani 1 1 d . . . . .
C30 C 0.8158(11) 0.6884(8) 0.2830(5) 0.046(3) Uani 1 1 d . . . . .
C32 C 0.8359(10) 0.7587(8) 0.2505(5) 0.044(3) Uani 1 1 d . . . . .
C33 C 0.2730(15) 0.6428(12) 0.2859(6) 0.084(6) Uani 1 1 d . . . . .
H33A H 0.227922 0.652680 0.316325 0.126 Uiso 1 1 calc R U . . .
H33B H 0.326934 0.687424 0.288153 0.126 Uiso 1 1 calc R U . . .
H33C H 0.308219 0.587850 0.292773 0.126 Uiso 1 1 calc R U . . .
C35 C 0.7077(13) 0.6935(10) 0.2943(5) 0.058(4) Uani 1 1 d . . . . .
C36 C 0.9441(15) 0.7784(14) 0.2319(8) 0.101(7) Uani 1 1 d . . . . .
H36A H 0.968324 0.729301 0.211480 0.151 Uiso 1 1 calc R U . . .
H36B H 0.996314 0.791371 0.267395 0.151 Uiso 1 1 calc R U . . .
H36C H 0.936811 0.827102 0.204911 0.151 Uiso 1 1 calc R U . . .
C38 C 0.6498(18) 0.6342(14) 0.3290(8) 0.106(7) Uani 1 1 d . U . . .
H38A H 0.683130 0.578266 0.330143 0.159 Uiso 1 1 calc R U . . .
H38B H 0.575176 0.629918 0.309874 0.159 Uiso 1 1 calc R U . . .
H38C H 0.653139 0.655444 0.369755 0.159 Uiso 1 1 calc R U . . .
C39 C 0.1188(10) 0.6915(9) 0.1335(5) 0.050(3) Uani 1 1 d . . . . .
C40 C 0.8947(15) 0.6197(11) 0.3069(7) 0.091(6) Uani 1 1 d . U . . .
H40A H 0.920664 0.629544 0.349288 0.136 Uiso 1 1 calc R U . . .
H40B H 0.954956 0.620610 0.284888 0.136 Uiso 1 1 calc R U . . .
H40C H 0.859509 0.564496 0.301734 0.136 Uiso 1 1 calc R U . . .
C42 C 0.2298(12) 0.8039(8) 0.2012(7) 0.059(4) Uani 1 1 d . . . . .
H42A H 0.212105 0.840712 0.166383 0.089 Uiso 1 1 calc R U . . .
H42B H 0.307408 0.801066 0.212795 0.089 Uiso 1 1 calc R U . . .
H42C H 0.198121 0.826743 0.234405 0.089 Uiso 1 1 calc R U . . .
C43 C 0.1443(19) 0.4849(12) 0.2199(10) 0.112(7) Uani 1 1 d . U . . .
H43A H 0.216812 0.465218 0.234736 0.168 Uiso 1 1 calc R U . . .
H43B H 0.110213 0.446550 0.188671 0.168 Uiso 1 1 calc R U . . .
H43C H 0.103054 0.485808 0.252772 0.168 Uiso 1 1 calc R U . . .
C47 C 0.5485(13) 0.8000(13) 0.2669(8) 0.096(6) Uani 1 1 d . U . . .
H47A H 0.545086 0.830012 0.304217 0.144 Uiso 1 1 calc R U . . .
H47B H 0.499100 0.752127 0.263036 0.144 Uiso 1 1 calc R U . . .
H47C H 0.528764 0.838605 0.233170 0.144 Uiso 1 1 calc R U . . .
C49 C 0.0781(15) 0.7468(13) 0.0832(7) 0.096(6) Uani 1 1 d . U . . .
H49A H 0.065243 0.713413 0.046395 0.145 Uiso 1 1 calc R U . . .
H49B H 0.130645 0.790948 0.079473 0.145 Uiso 1 1 calc R U . . .
H49C H 0.011309 0.772904 0.089994 0.145 Uiso 1 1 calc R U . . .
C50 C 0.7337(17) 0.8923(10) 0.2069(7) 0.089(6) Uani 1 1 d . U . . .
H50A H 0.761882 0.936879 0.234992 0.134 Uiso 1 1 calc R U . . .
H50B H 0.658983 0.904373 0.190768 0.134 Uiso 1 1 calc R U . . .
H50C H 0.775259 0.890305 0.174166 0.134 Uiso 1 1 calc R U . . .
C51 C 0.0253(14) 0.5482(14) 0.0923(10) 0.109(7) Uani 1 1 d . U . . .
H51A H -0.043136 0.539450 0.105952 0.164 Uiso 1 1 calc R U . . .
H51B H 0.059256 0.493492 0.088142 0.164 Uiso 1 1 calc R U . . .
H51C H 0.013412 0.577235 0.053747 0.164 Uiso 1 1 calc R U . . .
O1W O 0.7612(8) 0.7021(6) 0.0238(4) 0.060(3) Uani 1 1 d . . . A 1
O2W O 0.2651(9) 0.3413(6) 0.1402(5) 0.065(3) Uani 1 1 d . . . B 1
O3W O 0.7961(8) 0.4624(6) 0.1500(4) 0.061(3) Uani 1 1 d . . . C 1
O4W O 0.4800(19) 0.4685(15) 0.3654(10) 0.061(6) Uiso 0.5 1 d . . P D 1
O5W O -0.0898(13) 0.7141(11) -0.0637(7) 0.046(4) Uiso 0.5 1 d . . P E 1
O6W O 0.139(2) 0.6549(17) -0.0671(11) 0.077(7) Uiso 0.5 1 d . . P F 1
O7W O 0.7870(16) 0.2405(15) 0.0250(9) 0.082(6) Uiso 0.5 1 d D . P G 2
O8W O 0.6809(14) 0.8405(12) 0.0475(8) 0.051(4) Uiso 0.5 1 d . . P H 2
O9W O 0.650(2) 0.4080(17) 0.4383(11) 0.092(7) Uiso 0.5 1 d . . P I 1
O10W O 0.329(2) 1.1183(18) 0.0683(12) 0.088(8) Uiso 0.5 1 d . . P J 1
O11W O 0.390(3) 1.102(2) 0.0600(16) 0.136(13) Uiso 0.5 1 d . . P K 2
O12W O 0.091(2) 0.6287(17) -0.0643(11) 0.082(7) Uiso 0.5 1 d . . P L 2
O13W O 0.418(2) 0.6165(18) 0.4501(12) 0.100(8) Uiso 0.5 1 d . . P M 1
O14W O 0.659(3) 0.581(3) 0.4888(17) 0.098(12) Uiso 0.3333 1 d . . P N 1
O15W O 0.631(6) 0.980(4) 0.054(3) 0.17(2) Uiso 0.3333 1 d . . P O 1
O16W O 0.685(3) 1.133(2) 0.0229(16) 0.089(11) Uiso 0.3333 1 d . . P P 2
O17W O 0.564(4) 0.944(3) 0.072(2) 0.111(14) Uiso 0.3333 1 d . . P Q 2
O18W O 0.437(3) 0.970(2) 0.1284(17) 0.091(11) Uiso 0.3333 1 d . . P R 1
O19W O 0.439(3) 0.487(2) 0.3657(13) 0.049(7) Uiso 0.3333 1 d . . P S 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O13 1.704(7) . ?
W1 O6 1.726(8) . ?
W1 O3 1.935(6) . ?
W1 O15 1.960(6) 3_665 ?
W1 O9 2.123(6) 3_665 ?
W1 O10 2.140(6) . ?
W2 O2 1.728(7) . ?
W2 O12 1.773(7) . ?
W2 O15 1.849(6) . ?
W2 O4 1.995(6) . ?
W2 O1 2.052(6) . ?
W2 O7 2.190(6) . ?
W2 Rh6 3.1913(9) . ?
W3 O16 1.731(6) . ?
W3 O11 1.760(7) . ?
W3 O3 1.867(7) . ?
W3 O4 2.009(6) . ?
W3 O8 2.055(6) . ?
W3 O7 2.208(6) . ?
W3 Rh6 3.1972(10) . ?
W4 O5 1.722(7) . ?
W4 O9 1.803(6) . ?
W4 O10 1.818(6) . ?
W4 O1 2.010(6) . ?
W4 O8 2.018(6) . ?
W4 O7 2.272(6) . ?
W4 Rh6 3.1611(9) . ?
Rh6 C24 2.094(11) . ?
Rh6 O1 2.098(6) . ?
Rh6 C25 2.107(12) . ?
Rh6 O8 2.110(6) . ?
Rh6 C20 2.112(10) . ?
Rh6 C39 2.120(11) . ?
Rh6 C21 2.122(10) . ?
Rh6 O4 2.123(6) . ?
Rh5 C30 2.087(10) . ?
Rh5 C35 2.088(10) . ?
Rh5 C23 2.096(11) . ?
Rh5 O11 2.101(7) . ?
Rh5 C32 2.106(11) . ?
Rh5 C26 2.110(10) . ?
Rh5 O12 2.113(6) . ?
Rh5 O14 2.162(7) . ?
C20 C39 1.381(16) . ?
C20 C21 1.418(16) . ?
C20 C42 1.480(16) . ?
C21 C25 1.400(19) . ?
C21 C33 1.477(18) . ?
C23 C32 1.406(18) . ?
C23 C26 1.432(19) . ?
C23 C50 1.461(19) . ?
C24 C25 1.38(2) . ?
C24 C39 1.423(19) . ?
C24 C51 1.49(2) . ?
C25 C43 1.51(2) . ?
C26 C35 1.39(2) . ?
C26 C47 1.475(19) . ?
C30 C32 1.355(18) . ?
C30 C35 1.41(2) . ?
C30 C40 1.488(18) . ?
C32 C36 1.505(19) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C35 C38 1.47(2) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C49 1.44(2) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?

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
O13 W1 O6 101.3(4) . . ?
O13 W1 O3 96.6(3) . . ?
O6 W1 O3 96.5(3) . . ?
O13 W1 O15 95.0(3) . 3_665 ?
O6 W1 O15 94.1(3) . 3_665 ?
O3 W1 O15 162.4(3) . 3_665 ?
O13 W1 O9 88.7(3) . 3_665 ?
O6 W1 O9 169.8(3) . 3_665 ?
O3 W1 O9 84.2(3) . 3_665 ?
O15 W1 O9 82.9(3) 3_665 3_665 ?
O13 W1 O10 168.6(3) . . ?
O6 W1 O10 90.0(3) . . ?
O3 W1 O10 83.9(3) . . ?
O15 W1 O10 82.1(2) 3_665 . ?
O9 W1 O10 80.0(2) 3_665 . ?
O2 W2 O12 103.4(3) . . ?
O2 W2 O15 101.5(3) . . ?
O12 W2 O15 97.9(3) . . ?
O2 W2 O4 99.8(3) . . ?
O12 W2 O4 90.4(3) . . ?
O15 W2 O4 154.6(3) . . ?
O2 W2 O1 93.8(3) . . ?
O12 W2 O1 160.5(3) . . ?
O15 W2 O1 87.4(3) . . ?
O4 W2 O1 77.5(2) . . ?
O2 W2 O7 166.1(3) . . ?
O12 W2 O7 88.7(3) . . ?
O15 W2 O7 83.2(2) . . ?
O4 W2 O7 73.0(2) . . ?
O1 W2 O7 73.2(2) . . ?
O2 W2 Rh6 86.0(2) . . ?
O12 W2 Rh6 130.9(2) . . ?
O15 W2 Rh6 127.7(2) . . ?
O4 W2 Rh6 40.68(17) . . ?
O1 W2 Rh6 40.27(17) . . ?
O7 W2 Rh6 80.89(16) . . ?
O16 W3 O11 103.4(3) . . ?
O16 W3 O3 103.1(3) . . ?
O11 W3 O3 98.5(3) . . ?
O16 W3 O4 99.4(3) . . ?
O11 W3 O4 88.7(3) . . ?
O3 W3 O4 154.0(2) . . ?
O16 W3 O8 94.8(3) . . ?
O11 W3 O8 158.8(3) . . ?
O3 W3 O8 87.6(3) . . ?
O4 W3 O8 77.6(2) . . ?
O16 W3 O7 166.5(3) . . ?
O11 W3 O7 87.3(3) . . ?
O3 W3 O7 83.1(2) . . ?
O4 W3 O7 72.4(2) . . ?
O8 W3 O7 73.2(2) . . ?
O16 W3 Rh6 86.3(2) . . ?
O11 W3 Rh6 129.3(2) . . ?
O3 W3 Rh6 128.1(2) . . ?
O4 W3 Rh6 40.63(18) . . ?
O8 W3 Rh6 40.48(17) . . ?
O7 W3 Rh6 80.50(15) . . ?
O5 W4 O9 103.1(3) . . ?
O5 W4 O10 102.4(3) . . ?
O9 W4 O10 98.0(3) . . ?
O5 W4 O1 98.2(3) . . ?
O9 W4 O1 88.4(3) . . ?
O10 W4 O1 156.4(3) . . ?
O5 W4 O8 99.3(3) . . ?
O9 W4 O8 155.2(3) . . ?
O10 W4 O8 87.2(3) . . ?
O1 W4 O8 78.1(2) . . ?
O5 W4 O7 168.3(3) . . ?
O9 W4 O7 83.7(3) . . ?
O10 W4 O7 85.8(2) . . ?
O1 W4 O7 72.3(2) . . ?
O8 W4 O7 72.5(2) . . ?
O5 W4 Rh6 87.9(2) . . ?
O9 W4 Rh6 129.1(2) . . ?
O10 W4 Rh6 128.31(19) . . ?
O1 W4 Rh6 40.73(17) . . ?
O8 W4 Rh6 41.10(18) . . ?
O7 W4 Rh6 80.44(15) . . ?
C24 Rh6 O1 115.3(5) . . ?
C24 Rh6 C25 38.4(6) . . ?
O1 Rh6 C25 151.5(5) . . ?
C24 Rh6 O8 111.6(4) . . ?
O1 Rh6 O8 74.1(2) . . ?
C25 Rh6 O8 102.9(4) . . ?
C24 Rh6 C20 65.4(5) . . ?
O1 Rh6 C20 121.2(3) . . ?
C25 Rh6 C20 64.9(5) . . ?
O8 Rh6 C20 164.5(4) . . ?
C24 Rh6 C39 39.5(5) . . ?
O1 Rh6 C39 102.3(4) . . ?
C25 Rh6 C39 64.5(6) . . ?
O8 Rh6 C39 147.1(4) . . ?
C20 Rh6 C39 38.1(4) . . ?
C24 Rh6 C21 65.2(5) . . ?
O1 Rh6 C21 159.8(4) . . ?
C25 Rh6 C21 38.7(5) . . ?
O8 Rh6 C21 125.4(4) . . ?
C20 Rh6 C21 39.1(4) . . ?
C39 Rh6 C21 64.6(5) . . ?
C24 Rh6 O4 170.1(4) . . ?
O1 Rh6 O4 73.8(2) . . ?
C25 Rh6 O4 133.6(5) . . ?
O8 Rh6 O4 74.0(2) . . ?
C20 Rh6 O4 106.9(4) . . ?
C39 Rh6 O4 137.4(4) . . ?
C21 Rh6 O4 104.9(4) . . ?
C24 Rh6 W4 107.5(3) . . ?
O1 Rh6 W4 38.68(16) . . ?
C25 Rh6 W4 125.0(4) . . ?
O8 Rh6 W4 38.95(16) . . ?
C20 Rh6 W4 155.9(3) . . ?
C39 Rh6 W4 121.7(3) . . ?
C21 Rh6 W4 161.2(4) . . ?
O4 Rh6 W4 82.07(16) . . ?
C24 Rh6 W2 148.9(5) . . ?
O1 Rh6 W2 39.22(17) . . ?
C25 Rh6 W2 169.0(5) . . ?
O8 Rh6 W2 81.83(17) . . ?
C20 Rh6 W2 108.6(3) . . ?
C39 Rh6 W2 116.5(4) . . ?
C21 Rh6 W2 130.7(4) . . ?
O4 Rh6 W2 37.77(16) . . ?
W4 Rh6 W2 64.707(19) . . ?
C24 Rh6 W3 143.6(4) . . ?
O1 Rh6 W3 81.73(17) . . ?
C25 Rh6 W3 114.4(4) . . ?
O8 Rh6 W3 39.22(17) . . ?
C20 Rh6 W3 135.0(3) . . ?
C39 Rh6 W3 173.1(3) . . ?
C21 Rh6 W3 109.9(3) . . ?
O4 Rh6 W3 38.03(17) . . ?
W4 Rh6 W3 64.814(19) . . ?
W2 Rh6 W3 63.20(2) . . ?
C30 Rh5 C35 39.5(6) . . ?
C30 Rh5 C23 65.2(4) . . ?
C35 Rh5 C23 65.5(5) . . ?
C30 Rh5 O11 109.1(4) . . ?
C35 Rh5 O11 93.1(4) . . ?
C23 Rh5 O11 153.3(4) . . ?
C30 Rh5 C32 37.7(5) . . ?
C35 Rh5 C32 64.7(5) . . ?
C23 Rh5 C32 39.1(5) . . ?
O11 Rh5 C32 146.1(4) . . ?
C30 Rh5 C26 65.8(5) . . ?
C35 Rh5 C26 38.8(6) . . ?
C23 Rh5 C26 39.8(5) . . ?
O11 Rh5 C26 113.5(4) . . ?
C32 Rh5 C26 65.6(5) . . ?
C30 Rh5 O12 163.6(4) . . ?
C35 Rh5 O12 135.0(5) . . ?
C23 Rh5 O12 98.4(4) . . ?
O11 Rh5 O12 85.3(2) . . ?
C32 Rh5 O12 128.5(4) . . ?
C26 Rh5 O12 101.7(4) . . ?
C30 Rh5 O14 102.3(4) . . ?
C35 Rh5 O14 138.8(5) . . ?
C23 Rh5 O14 120.4(5) . . ?
O11 Rh5 O14 86.2(3) . . ?
C32 Rh5 O14 94.3(4) . . ?
C26 Rh5 O14 159.2(4) . . ?
O12 Rh5 O14 86.1(3) . . ?
W4 O1 W2 113.6(3) . . ?
W4 O1 Rh6 100.6(3) . . ?
W2 O1 Rh6 100.5(2) . . ?
W3 O3 W1 150.8(4) . . ?
W2 O4 W3 113.5(3) . . ?
W2 O4 Rh6 101.5(2) . . ?
W3 O4 Rh6 101.3(3) . . ?
W2 O7 W3 99.1(2) . . ?
W2 O7 W4 99.3(2) . . ?
W3 O7 W4 99.0(2) . . ?
W4 O8 W3 113.6(3) . . ?
W4 O8 Rh6 99.9(3) . . ?
W3 O8 Rh6 100.3(3) . . ?
W4 O9 W1 147.1(3) . 3_665 ?
W4 O10 W1 144.3(3) . . ?
W3 O11 Rh5 141.6(4) . . ?
W2 O12 Rh5 138.9(4) . . ?
W2 O15 W1 151.5(4) . 3_665 ?
C39 C20 C21 108.2(11) . . ?
C39 C20 C42 126.8(12) . . ?
C21 C20 C42 124.9(12) . . ?
C39 C20 Rh6 71.3(6) . . ?
C21 C20 Rh6 70.8(6) . . ?
C42 C20 Rh6 125.3(8) . . ?
C25 C21 C20 106.8(12) . . ?
C25 C21 C33 127.7(14) . . ?
C20 C21 C33 125.5(13) . . ?
C25 C21 Rh6 70.1(7) . . ?
C20 C21 Rh6 70.1(6) . . ?
C33 C21 Rh6 124.2(9) . . ?
C32 C23 C26 107.2(11) . . ?
C32 C23 C50 124.9(15) . . ?
C26 C23 C50 127.7(14) . . ?
C32 C23 Rh5 70.8(6) . . ?
C26 C23 Rh5 70.6(7) . . ?
C50 C23 Rh5 128.2(9) . . ?
C25 C24 C39 107.1(12) . . ?
C25 C24 C51 125.8(17) . . ?
C39 C24 C51 127.0(17) . . ?
C25 C24 Rh6 71.3(7) . . ?
C39 C24 Rh6 71.3(7) . . ?
C51 C24 Rh6 126.5(9) . . ?
C24 C25 C21 109.6(12) . . ?
C24 C25 C43 126.1(17) . . ?
C21 C25 C43 124.4(17) . . ?
C24 C25 Rh6 70.3(7) . . ?
C21 C25 Rh6 71.3(7) . . ?
C43 C25 Rh6 125.6(10) . . ?
C35 C26 C23 106.5(11) . . ?
C35 C26 C47 127.8(16) . . ?
C23 C26 C47 125.7(15) . . ?
C35 C26 Rh5 69.8(7) . . ?
C23 C26 Rh5 69.6(6) . . ?
C47 C26 Rh5 125.1(9) . . ?
C32 C30 C35 108.3(12) . . ?
C32 C30 C40 126.8(15) . . ?
C35 C30 C40 124.8(15) . . ?
C32 C30 Rh5 71.9(6) . . ?
C35 C30 Rh5 70.3(6) . . ?
C40 C30 Rh5 126.4(9) . . ?
C30 C32 C23 109.3(11) . . ?
C30 C32 C36 124.2(15) . . ?
C23 C32 C36 126.5(15) . . ?
C30 C32 Rh5 70.4(6) . . ?
C23 C32 Rh5 70.1(6) . . ?
C36 C32 Rh5 126.6(9) . . ?
C21 C33 H33A 109.5 . . ?
C21 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C21 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C26 C35 C30 108.6(11) . . ?
C26 C35 C38 122.7(17) . . ?
C30 C35 C38 128.6(17) . . ?
C26 C35 Rh5 71.5(6) . . ?
C30 C35 Rh5 70.2(6) . . ?
C38 C35 Rh5 125.1(9) . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C20 C39 C24 108.3(12) . . ?
C20 C39 C49 125.8(15) . . ?
C24 C39 C49 125.9(15) . . ?
C20 C39 Rh6 70.7(6) . . ?
C24 C39 Rh6 69.3(7) . . ?
C49 C39 Rh6 125.4(10) . . ?
C30 C40 H40A 109.5 . . ?
C30 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C30 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C20 C42 H42A 109.5 . . ?
C20 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C20 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C25 C43 H43A 109.5 . . ?
C25 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C25 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C26 C47 H47A 109.5 . . ?
C26 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C26 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C39 C49 H49A 109.5 . . ?
C39 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C39 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C23 C50 H50A 109.5 . . ?
C23 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C23 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C24 C51 H51A 109.5 . . ?
C24 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C24 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?

_refine_diff_density_max         1.862
_refine_diff_density_min         -1.467
_refine_diff_density_rms         0.297

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1840552'
_audit_update_record             
;
2018-08-30 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H104 Ir4 O55 W8'
_chemical_formula_weight         3704.83

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   12.685(3)
_cell_length_b                   15.825(4)
_cell_length_c                   22.113(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.964(4)
_cell_angle_gamma                90
_cell_volume                     4422.2(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    22662
_cell_measurement_theta_min      1.584
_cell_measurement_theta_max      25.249

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.782
_exptl_crystal_F_000             3368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    16.440
_shelx_estimated_absorpt_T_min   0.053
_shelx_estimated_absorpt_T_max   0.559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4214
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22662
_diffrn_reflns_av_unetI/netI     0.1340
_diffrn_reflns_av_R_equivalents  0.1124
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.584
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7976
_reflns_number_gt                4701
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL-2016/6, PLATON, WINGX (Ferrugia, 2012)'

_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)+(0.0730P)²] 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         7976
_refine_ls_number_parameters     488
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0595
_refine_ls_wR_factor_ref         0.1543
_refine_ls_wR_factor_gt          0.1325
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_restrained_S_all      0.914
_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_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
W1 W 0.51893(7) 0.33878(6) 0.07496(4) 0.0271(2) Uani 1 1 d . . . . .
W2 W 0.45579(7) 0.70485(6) 0.08864(4) 0.0264(2) Uani 1 1 d . . . . .
W3 W 0.47527(7) 0.52525(6) 0.17172(4) 0.0269(2) Uani 1 1 d . . . . .
W4 W 0.33482(7) 0.52419(6) 0.03155(4) 0.0243(2) Uani 1 1 d . . . . .
Ir6 Ir 0.25114(7) 0.62223(6) 0.14608(4) 0.0297(2) Uani 1 1 d . . . . .
Ir5 Ir 0.68620(7) 0.68369(6) 0.20052(4) 0.0319(2) Uani 1 1 d . . . . .
O1 O 0.3157(10) 0.6462(9) 0.0616(6) 0.026(3) Uani 1 1 d . . . . .
O2 O 0.3980(11) 0.8003(8) 0.0998(7) 0.036(4) Uani 1 1 d . . . . .
O3 O 0.5138(11) 0.4194(8) 0.1410(5) 0.024(3) Uani 1 1 d . . . . .
O4 O 0.4177(11) 0.6443(9) 0.1642(6) 0.030(3) Uani 1 1 d . . . . .
O5 O 0.2039(11) 0.5025(9) 0.0100(6) 0.033(4) Uani 1 1 d . . . . .
O6 O 0.4221(11) 0.2744(8) 0.0973(6) 0.033(4) Uani 1 1 d D U . . .
O7 O 0.4919(10) 0.5684(8) 0.0764(6) 0.024(3) Uani 1 1 d . . . . .
O8 O 0.3293(10) 0.5085(9) 0.1234(6) 0.032(4) Uani 1 1 d . . . . .
O9 O 0.3846(11) 0.5679(9) -0.0366(6) 0.030(3) Uani 1 1 d . . . . .
O10 O 0.3966(11) 0.4220(9) 0.0283(7) 0.036(4) Uani 1 1 d . . . . .
O11 O 0.6023(11) 0.5688(9) 0.1892(6) 0.035(4) Uani 1 1 d . . . . .
O12 O 0.5868(11) 0.7166(9) 0.1223(6) 0.035(4) Uani 1 1 d . . . . .
O13 O 0.6321(12) 0.2873(9) 0.1037(6) 0.037(4) Uani 1 1 d . . . . .
O14 O 0.7833(11) 0.6283(10) 0.1350(6) 0.039(4) Uani 1 1 d . . . . .
O15 O 0.4809(11) 0.7101(9) 0.0066(6) 0.034(4) Uani 1 1 d . . . . .
O16 O 0.4326(13) 0.4987(11) 0.2425(6) 0.047(4) Uani 1 1 d . . . . .
C20 C 0.1668(18) 0.7189(14) 0.1889(9) 0.034(6) Uani 1 1 d . . . . .
C21 C 0.1834(17) 0.6458(15) 0.2314(9) 0.034(6) Uani 1 1 d . . . . .
C23 C 0.684(2) 0.8002(16) 0.2436(11) 0.050(7) Uani 1 1 d . . . . .
C24 C 0.0846(16) 0.6023(16) 0.1438(11) 0.039(6) Uani 1 1 d . . . . .
C25 C 0.1308(19) 0.5765(15) 0.2029(11) 0.041(6) Uani 1 1 d . U . . .
C26 C 0.629(2) 0.741(2) 0.2772(11) 0.057(8) Uani 1 1 d . . . . .
C30 C 0.8046(18) 0.7000(15) 0.2738(10) 0.036(6) Uani 1 1 d . U . . .
C32 C 0.792(2) 0.7768(19) 0.2423(11) 0.053(7) Uani 1 1 d . . . . .
C33 C 0.244(2) 0.6551(17) 0.2914(10) 0.054(7) Uani 1 1 d . U . . .
H33A H 0.195696 0.665030 0.321835 0.081 Uiso 1 1 calc R U . . .
H33B H 0.291673 0.701929 0.290265 0.081 Uiso 1 1 calc R U . . .
H33C H 0.283192 0.604316 0.300923 0.081 Uiso 1 1 calc R U . . .
C35 C 0.708(2) 0.6783(19) 0.2965(10) 0.057(8) Uani 1 1 d . . . . .
C36 C 0.874(2) 0.8246(19) 0.2132(13) 0.074(10) Uani 1 1 d . . . . .
H36A H 0.844382 0.846561 0.174925 0.112 Uiso 1 1 calc R U . . .
H36B H 0.931935 0.787700 0.206621 0.112 Uiso 1 1 calc R U . . .
H36C H 0.898691 0.870429 0.239029 0.112 Uiso 1 1 calc R U . . .
C38 C 0.686(2) 0.603(2) 0.3326(13) 0.085(11) Uani 1 1 d . . . . .
H38A H 0.723009 0.555323 0.317728 0.127 Uiso 1 1 calc R U . . .
H38B H 0.611773 0.592182 0.329206 0.127 Uiso 1 1 calc R U . . .
H38C H 0.710555 0.612944 0.374337 0.127 Uiso 1 1 calc R U . . .
C39 C 0.104(2) 0.6871(17) 0.1373(12) 0.050(7) Uani 1 1 d . . . . .
C40 C 0.9037(18) 0.651(2) 0.2801(11) 0.065(9) Uani 1 1 d . . . . .
H40A H 0.899482 0.609064 0.310909 0.097 Uiso 1 1 calc R U . . .
H40B H 0.961747 0.688746 0.291456 0.097 Uiso 1 1 calc R U . . .
H40C H 0.914643 0.624716 0.242196 0.097 Uiso 1 1 calc R U . . .
C42 C 0.207(2) 0.8063(15) 0.2022(13) 0.068(9) Uani 1 1 d . . . . .
H42A H 0.229987 0.830897 0.165984 0.102 Uiso 1 1 calc R U . . .
H42B H 0.265095 0.804037 0.232949 0.102 Uiso 1 1 calc R U . . .
H42C H 0.151145 0.840117 0.216405 0.102 Uiso 1 1 calc R U . . .
C43 C 0.129(3) 0.488(2) 0.2308(16) 0.096(12) Uani 1 1 d . U . . .
H43A H 0.199801 0.471166 0.244762 0.144 Uiso 1 1 calc R U . . .
H43B H 0.100479 0.448347 0.200622 0.144 Uiso 1 1 calc R U . . .
H43C H 0.085793 0.488055 0.264298 0.144 Uiso 1 1 calc R U . . .
C47 C 0.521(2) 0.741(3) 0.2940(13) 0.099(14) Uani 1 1 d . . . . .
H47A H 0.516438 0.707374 0.329677 0.148 Uiso 1 1 calc R U . . .
H47B H 0.475006 0.718188 0.261247 0.148 Uiso 1 1 calc R U . . .
H47C H 0.499402 0.798061 0.302011 0.148 Uiso 1 1 calc R U . . .
C49 C 0.064(2) 0.743(2) 0.0860(11) 0.079(11) Uani 1 1 d . . . . .
H49A H 0.054985 0.710155 0.049258 0.118 Uiso 1 1 calc R U . . .
H49B H 0.113098 0.787621 0.081293 0.118 Uiso 1 1 calc R U . . .
H49C H -0.003413 0.766150 0.094385 0.118 Uiso 1 1 calc R U . . .
C50 C 0.637(3) 0.8801(19) 0.2163(13) 0.096(13) Uani 1 1 d . . . . .
H50A H 0.690054 0.923064 0.217066 0.145 Uiso 1 1 calc R U . . .
H50B H 0.580020 0.898676 0.239301 0.145 Uiso 1 1 calc R U . . .
H50C H 0.609423 0.869657 0.175092 0.145 Uiso 1 1 calc R U . . .
C51 C 0.020(2) 0.547(3) 0.0989(16) 0.111(15) Uani 1 1 d . . . . .
H51A H -0.037023 0.522309 0.118240 0.166 Uiso 1 1 calc R U . . .
H51B H 0.064410 0.503649 0.084709 0.166 Uiso 1 1 calc R U . . .
H51C H -0.007649 0.581148 0.065190 0.166 Uiso 1 1 calc R U . . .
O1W O 0.7577(12) 0.6943(10) 0.0232(7) 0.048(4) Uani 1 1 d . . . . .
O2W O 0.2428(14) 0.3518(10) 0.1400(7) 0.055(5) Uani 1 1 d . . . . .
O3W O 0.7750(15) 0.4581(12) 0.1505(8) 0.063(5) Uani 1 1 d . . . . .
O4W O 0.4311(17) 0.4984(13) 0.3692(8) 0.077(6) Uani 1 1 d . . . . .
O5W O -0.0842(17) 0.6997(14) -0.0585(8) 0.084(7) Uani 1 1 d . . . . .
O6W O 0.1076(17) 0.6302(13) -0.0644(10) 0.083(7) Uani 1 1 d . . . . .
O7W O 0.7685(17) 0.2427(16) 0.0275(9) 0.097(8) Uani 1 1 d . . . A 1
O8W O 0.694(2) 0.8663(17) 0.0618(12) 0.027(7) Uiso 0.5 1 d . . P B 1
O9W O 0.605(2) 0.4429(17) 0.4407(12) 0.030(7) Uiso 0.5 1 d . . P . .
O10W O 0.309(2) 1.1676(16) 0.0324(12) 0.037(8) Uiso 0.5 1 d . . P C 2
O11W O 0.403(2) 1.0786(19) 0.0712(14) 0.040(8) Uiso 0.5 1 d . . P D 1
O12W O 0.271(3) 0.954(2) 0.0908(16) 0.061(10) Uiso 0.5 1 d . . P . .
O13W O 0.372(3) 0.639(2) 0.4451(16) 0.064(11) Uiso 0.5 1 d . . P E 1
O14W O 0.681(2) 0.590(2) 0.4830(14) 0.046(9) Uiso 0.5 1 d . . P F 2
O15W O 0.516(4) 0.962(3) 0.081(2) 0.116(18) Uiso 0.5 1 d . . P G 2
O16W O 0.590(4) 1.069(3) 0.048(2) 0.118(18) Uiso 0.5 1 d . . P H 3


_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
W1 O6 1.702(14) . ?
W1 O13 1.724(14) . ?
W1 O3 1.944(12) . ?
W1 O15 1.961(14) 3_665 ?
W1 O9 2.139(14) 3_665 ?
W1 O10 2.220(14) . ?
W2 O2 1.706(13) . ?
W2 O12 1.771(14) . ?
W2 O15 1.872(14) . ?
W2 O4 2.022(13) . ?
W2 O1 2.047(13) . ?
W2 O7 2.229(14) . ?
W3 O16 1.751(14) . ?
W3 O11 1.764(14) . ?
W3 O3 1.888(13) . ?
W3 O4 2.022(13) . ?
W3 O8 2.074(13) . ?
W3 O7 2.243(13) . ?
W4 O5 1.722(14) . ?
W4 O10 1.801(14) . ?
W4 O9 1.821(13) . ?
W4 O8 2.053(13) . ?
W4 O1 2.063(14) . ?
W4 O7 2.259(12) . ?
W4 Ir6 3.2269(13) . ?
Ir6 C39 2.12(2) . ?
Ir6 C24 2.13(2) . ?
Ir6 C20 2.13(2) . ?
Ir6 O8 2.135(14) . ?
Ir6 O1 2.138(12) . ?
Ir6 O4 2.145(14) . ?
Ir6 C21 2.173(19) . ?
Ir6 C25 2.18(2) . ?
Ir5 C23 2.08(2) . ?
Ir5 C26 2.11(2) . ?
Ir5 O11 2.111(15) . ?
Ir5 O12 2.116(15) . ?
Ir5 C35 2.12(2) . ?
Ir5 C30 2.13(2) . ?
Ir5 C32 2.15(3) . ?
Ir5 O14 2.167(13) . ?
C20 C39 1.42(3) . ?
C20 C21 1.50(3) . ?
C20 C42 1.49(3) . ?
C21 C25 1.40(3) . ?
C21 C33 1.48(3) . ?
C23 C26 1.41(4) . ?
C23 C32 1.42(3) . ?
C23 C50 1.50(4) . ?
C24 C39 1.37(3) . ?
C24 C25 1.44(3) . ?
C24 C51 1.51(3) . ?
C25 C43 1.54(4) . ?
C26 C35 1.45(4) . ?
C26 C47 1.46(4) . ?
C30 C32 1.40(3) . ?
C30 C35 1.41(3) . ?
C30 C40 1.47(3) . ?
C32 C36 1.48(4) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C35 C38 1.47(4) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C49 1.49(3) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?

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
O6 W1 O13 102.1(7) . . ?
O6 W1 O3 95.9(6) . . ?
O13 W1 O3 96.6(6) . . ?
O6 W1 O15 95.1(6) . 3_665 ?
O13 W1 O15 94.9(6) . 3_665 ?
O3 W1 O15 162.1(5) . 3_665 ?
O6 W1 O9 168.6(6) . 3_665 ?
O13 W1 O9 89.2(6) . 3_665 ?
O3 W1 O9 84.4(5) . 3_665 ?
O15 W1 O9 82.1(5) 3_665 3_665 ?
O6 W1 O10 89.8(6) . . ?
O13 W1 O10 168.0(6) . . ?
O3 W1 O10 83.8(5) . . ?
O15 W1 O10 82.1(6) 3_665 . ?
O9 W1 O10 78.9(5) 3_665 . ?
O2 W2 O12 104.2(7) . . ?
O2 W2 O15 102.3(7) . . ?
O12 W2 O15 99.8(6) . . ?
O2 W2 O4 99.4(6) . . ?
O12 W2 O4 89.2(6) . . ?
O15 W2 O4 153.6(6) . . ?
O2 W2 O1 94.0(6) . . ?
O12 W2 O1 158.4(6) . . ?
O15 W2 O1 87.3(5) . . ?
O4 W2 O1 76.3(5) . . ?
O2 W2 O7 166.1(6) . . ?
O12 W2 O7 87.6(6) . . ?
O15 W2 O7 82.6(6) . . ?
O4 W2 O7 73.0(5) . . ?
O1 W2 O7 73.0(5) . . ?
O16 W3 O11 104.2(7) . . ?
O16 W3 O3 102.6(7) . . ?
O11 W3 O3 99.5(6) . . ?
O16 W3 O4 99.2(7) . . ?
O11 W3 O4 88.3(6) . . ?
O3 W3 O4 154.1(5) . . ?
O16 W3 O8 95.7(6) . . ?
O11 W3 O8 157.0(6) . . ?
O3 W3 O8 87.0(6) . . ?
O4 W3 O8 77.1(6) . . ?
O16 W3 O7 167.1(6) . . ?
O11 W3 O7 85.9(5) . . ?
O3 W3 O7 83.3(5) . . ?
O4 W3 O7 72.7(5) . . ?
O8 W3 O7 73.0(5) . . ?
O5 W4 O10 102.8(6) . . ?
O5 W4 O9 104.0(6) . . ?
O10 W4 O9 97.2(7) . . ?
O5 W4 O8 97.7(6) . . ?
O10 W4 O8 89.0(6) . . ?
O9 W4 O8 155.4(6) . . ?
O5 W4 O1 98.0(6) . . ?
O10 W4 O1 156.5(6) . . ?
O9 W4 O1 88.3(6) . . ?
O8 W4 O1 77.3(5) . . ?
O5 W4 O7 167.5(6) . . ?
O10 W4 O7 85.7(6) . . ?
O9 W4 O7 83.7(5) . . ?
O8 W4 O7 73.0(5) . . ?
O1 W4 O7 72.1(5) . . ?
O5 W4 Ir6 86.5(5) . . ?
O10 W4 Ir6 129.6(5) . . ?
O9 W4 Ir6 128.9(4) . . ?
O8 W4 Ir6 40.5(4) . . ?
O1 W4 Ir6 40.7(3) . . ?
O7 W4 Ir6 81.0(3) . . ?
C39 Ir6 C24 37.7(9) . . ?
C39 Ir6 C20 39.1(8) . . ?
C24 Ir6 C20 65.4(9) . . ?
C39 Ir6 O8 143.9(8) . . ?
C24 Ir6 O8 110.4(7) . . ?
C20 Ir6 O8 165.7(6) . . ?
C39 Ir6 O1 103.6(8) . . ?
C24 Ir6 O1 117.4(7) . . ?
C20 Ir6 O1 120.3(6) . . ?
O8 Ir6 O1 73.9(5) . . ?
C39 Ir6 O4 141.4(8) . . ?
C24 Ir6 O4 170.5(7) . . ?
C20 Ir6 O4 108.9(7) . . ?
O8 Ir6 O4 73.2(5) . . ?
O1 Ir6 O4 71.9(5) . . ?
C39 Ir6 C21 65.5(9) . . ?
C24 Ir6 C21 65.2(9) . . ?
C20 Ir6 C21 40.6(7) . . ?
O8 Ir6 C21 125.1(7) . . ?
O1 Ir6 C21 159.9(7) . . ?
O4 Ir6 C21 105.5(7) . . ?
C39 Ir6 C25 63.9(10) . . ?
C24 Ir6 C25 39.1(9) . . ?
C20 Ir6 C25 65.2(9) . . ?
O8 Ir6 C25 102.6(7) . . ?
O1 Ir6 C25 154.4(7) . . ?
O4 Ir6 C25 132.3(7) . . ?
C21 Ir6 C25 37.6(8) . . ?
C39 Ir6 W4 120.5(7) . . ?
C24 Ir6 W4 107.6(6) . . ?
C20 Ir6 W4 154.7(5) . . ?
O8 Ir6 W4 38.7(4) . . ?
O1 Ir6 W4 39.0(4) . . ?
O4 Ir6 W4 80.8(4) . . ?
C21 Ir6 W4 161.1(6) . . ?
C25 Ir6 W4 125.9(6) . . ?
C23 Ir5 C26 39.2(10) . . ?
C23 Ir5 O11 142.3(10) . . ?
C26 Ir5 O11 105.4(9) . . ?
C23 Ir5 O12 97.2(8) . . ?
C26 Ir5 O12 109.3(9) . . ?
O11 Ir5 O12 81.7(5) . . ?
C23 Ir5 C35 65.3(10) . . ?
C26 Ir5 C35 40.2(10) . . ?
O11 Ir5 C35 96.0(9) . . ?
O12 Ir5 C35 147.9(9) . . ?
C23 Ir5 C30 65.3(9) . . ?
C26 Ir5 C30 66.6(10) . . ?
O11 Ir5 C30 120.7(8) . . ?
O12 Ir5 C30 157.6(8) . . ?
C35 Ir5 C30 38.7(9) . . ?
C23 Ir5 C32 39.4(10) . . ?
C26 Ir5 C32 66.4(10) . . ?
O11 Ir5 C32 158.8(9) . . ?
O12 Ir5 C32 119.3(9) . . ?
C35 Ir5 C32 64.7(11) . . ?
C30 Ir5 C32 38.3(9) . . ?
C23 Ir5 O14 134.3(10) . . ?
C26 Ir5 O14 165.3(8) . . ?
O11 Ir5 O14 83.2(6) . . ?
O12 Ir5 O14 83.4(5) . . ?
C35 Ir5 O14 128.4(9) . . ?
C30 Ir5 O14 98.8(7) . . ?
C32 Ir5 O14 101.3(8) . . ?
W2 O1 W4 113.3(6) . . ?
W2 O1 Ir6 102.3(5) . . ?
W4 O1 Ir6 100.4(6) . . ?
W3 O3 W1 151.6(7) . . ?
W3 O4 W2 113.5(6) . . ?
W3 O4 Ir6 101.9(6) . . ?
W2 O4 Ir6 103.0(6) . . ?
W2 O7 W3 98.3(5) . . ?
W2 O7 W4 99.8(5) . . ?
W3 O7 W4 99.6(5) . . ?
W4 O8 W3 112.9(6) . . ?
W4 O8 Ir6 100.8(6) . . ?
W3 O8 Ir6 100.5(6) . . ?
W4 O9 W1 147.3(8) . 3_665 ?
W4 O10 W1 143.4(8) . . ?
W3 O11 Ir5 143.5(8) . . ?
W2 O12 Ir5 142.0(8) . . ?
W2 O15 W1 152.6(8) . 3_665 ?
C39 C20 C21 106(2) . . ?
C39 C20 C42 130(2) . . ?
C21 C20 C42 124(2) . . ?
C39 C20 Ir6 70.0(13) . . ?
C21 C20 Ir6 71.1(11) . . ?
C42 C20 Ir6 125.2(18) . . ?
C25 C21 C33 132(2) . . ?
C25 C21 C20 106.6(19) . . ?
C33 C21 C20 121(2) . . ?
C25 C21 Ir6 71.6(13) . . ?
C33 C21 Ir6 125.6(16) . . ?
C20 C21 Ir6 68.3(11) . . ?
C26 C23 C32 111(2) . . ?
C26 C23 C50 125(3) . . ?
C32 C23 C50 124(3) . . ?
C26 C23 Ir5 71.6(15) . . ?
C32 C23 Ir5 72.9(15) . . ?
C50 C23 Ir5 125.8(17) . . ?
C39 C24 C25 108(2) . . ?
C39 C24 C51 126(3) . . ?
C25 C24 C51 126(3) . . ?
C39 C24 Ir6 70.8(14) . . ?
C25 C24 Ir6 72.4(13) . . ?
C51 C24 Ir6 125.5(18) . . ?
C21 C25 C24 109(2) . . ?
C21 C25 C43 124(2) . . ?
C24 C25 C43 127(2) . . ?
C21 C25 Ir6 70.8(12) . . ?
C24 C25 Ir6 68.5(13) . . ?
C43 C25 Ir6 124.7(19) . . ?
C23 C26 C35 105(2) . . ?
C23 C26 C47 131(3) . . ?
C35 C26 C47 124(3) . . ?
C23 C26 Ir5 69.1(14) . . ?
C35 C26 Ir5 70.2(14) . . ?
C47 C26 Ir5 127(2) . . ?
C32 C30 C35 109(2) . . ?
C32 C30 C40 124(2) . . ?
C35 C30 C40 127(3) . . ?
C32 C30 Ir5 71.5(14) . . ?
C35 C30 Ir5 70.3(13) . . ?
C40 C30 Ir5 123.5(16) . . ?
C30 C32 C23 107(2) . . ?
C30 C32 C36 127(2) . . ?
C23 C32 C36 126(3) . . ?
C30 C32 Ir5 70.1(15) . . ?
C23 C32 Ir5 67.7(14) . . ?
C36 C32 Ir5 126.8(17) . . ?
C21 C33 H33A 109.5 . . ?
C21 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C21 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C35 C26 109(2) . . ?
C30 C35 C38 127(3) . . ?
C26 C35 C38 124(3) . . ?
C30 C35 Ir5 71.0(14) . . ?
C26 C35 Ir5 69.6(13) . . ?
C38 C35 Ir5 124(2) . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C24 C39 C20 111(2) . . ?
C24 C39 C49 127(3) . . ?
C20 C39 C49 122(2) . . ?
C24 C39 Ir6 71.5(14) . . ?
C20 C39 Ir6 70.9(14) . . ?
C49 C39 Ir6 126.6(18) . . ?
C30 C40 H40A 109.5 . . ?
C30 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C30 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C20 C42 H42A 109.5 . . ?
C20 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C20 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C25 C43 H43A 109.5 . . ?
C25 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C25 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C26 C47 H47A 109.5 . . ?
C26 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C26 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C39 C49 H49A 109.5 . . ?
C39 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C39 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C23 C50 H50A 109.5 . . ?
C23 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C23 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C24 C51 H51A 109.5 . . ?
C24 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C24 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?

_refine_diff_density_max         2.465
_refine_diff_density_min         -2.704
_refine_diff_density_rms         0.406

