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

####################################################################### 
# 
# 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 1402553'
_audit_update_record             
;
2015-05-24 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H30 N5 Nb O13'
_chemical_formula_weight         809.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9340(12)
_cell_length_b                   11.3774(10)
_cell_length_c                   17.883(2)
_cell_angle_alpha                78.587(9)
_cell_angle_beta                 78.363(11)
_cell_angle_gamma                70.115(10)
_cell_volume                     1657.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3237
_cell_measurement_theta_min      2.4440
_cell_measurement_theta_max      22.3230

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_F_000             828
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.442
_shelx_estimated_absorpt_T_min   0.909
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95299
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
'Mon May 04 20:58:25 2015'
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported S'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17278
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.581
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6757
_reflns_number_gt                5150
_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       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'CysAlisPro 171.37.34b'
_computing_data_reduction        'CysAlisPro 171.37.34b'
_computing_structure_solution    'SuperFlip (Palatinus & Chapius, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0487P)²+0.0789P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6757
_refine_ls_number_parameters     494
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1086
_refine_ls_wR_factor_gt          0.0985
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.240
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.75795(4) 0.23547(2) 0.16565(2) 0.02810(11) Uani 1 1 d . . . . .
O1 O 0.8879(3) 0.30969(19) 0.10930(13) 0.0424(6) Uani 1 1 d . . . . .
O2 O 0.5802(3) 0.30088(18) 0.09156(12) 0.0405(6) Uani 1 1 d . . . . .
O3 O 0.3575(3) 0.4467(2) 0.05732(16) 0.0629(8) Uani 1 1 d . . . . .
O4 O 0.3491(3) 0.5544(2) 0.18685(14) 0.0495(7) Uani 1 1 d . . . . .
C1 C 0.4602(4) 0.4030(3) 0.09908(19) 0.0354(8) Uani 1 1 d . . . . .
C2 C 0.4585(4) 0.4620(3) 0.16875(18) 0.0323(7) Uani 1 1 d . . . . .
O5 O 0.5805(3) 0.40182(18) 0.20371(12) 0.0379(6) Uani 1 1 d . . . . .
O6 O 0.8143(3) 0.25444(18) 0.26947(11) 0.0307(5) Uani 1 1 d . . . . .
O7 O 0.8114(3) 0.1847(2) 0.39454(12) 0.0437(6) Uani 1 1 d . . . . .
O8 O 0.5764(3) 0.0803(2) 0.38671(13) 0.0444(6) Uani 1 1 d . . . . .
O9 O 0.6125(3) 0.13951(18) 0.25845(12) 0.0317(5) Uani 1 1 d . . . . .
C3 C 0.7656(4) 0.1945(3) 0.33327(18) 0.0300(7) Uani 1 1 d . . . . .
C4 C 0.6397(4) 0.1313(3) 0.32806(18) 0.0309(7) Uani 1 1 d . . . . .
O10 O 0.9472(3) 0.06685(18) 0.19936(12) 0.0332(5) Uani 1 1 d . . . . .
O11 O 1.0950(3) -0.12958(18) 0.17746(12) 0.0373(6) Uani 1 1 d . . . . .
O12 O 0.9055(3) -0.08941(19) 0.06026(13) 0.0391(6) Uani 1 1 d . . . . .
O13 O 0.7799(3) 0.10052(18) 0.09507(12) 0.0346(5) Uani 1 1 d . . . . .
C5 C 0.9884(4) -0.0307(3) 0.16380(17) 0.0286(7) Uani 1 1 d . . . . .
C6 C 0.8863(4) -0.0097(3) 0.10023(17) 0.0276(7) Uani 1 1 d . . . . .
C7 C 0.7668(5) 0.5928(4) 0.6214(2) 0.0588(11) Uani 1 1 d . . . . .
H7A H 0.8783 0.5878 0.6125 0.088 Uiso 1 1 calc R U . . .
H7B H 0.7507 0.5250 0.6603 0.088 Uiso 1 1 calc R U . . .
H7C H 0.7026 0.6721 0.6384 0.088 Uiso 1 1 calc R U . . .
C8 C 0.7183(4) 0.5827(3) 0.5482(2) 0.0416(9) Uani 1 1 d . . . . .
N1 N 0.6039(3) 0.6794(2) 0.51958(15) 0.0359(7) Uani 1 1 d . . . . .
H1 H 0.5617 0.7462 0.5417 0.043 Uiso 0.5 1 calc R U P . .
C9 C 0.7893(5) 0.4739(3) 0.5124(2) 0.0534(10) Uani 1 1 d . . . . .
H9 H 0.8702 0.4072 0.5336 0.064 Uiso 1 1 calc R U . . .
C10 C 0.7411(5) 0.4649(3) 0.4469(2) 0.0522(10) Uani 1 1 d . . . . .
H10 H 0.7891 0.3927 0.4231 0.063 Uiso 1 1 calc R U . . .
C11 C 0.6182(5) 0.5657(3) 0.4154(2) 0.0423(9) Uani 1 1 d . . . . .
C12 C 0.5568(5) 0.5656(4) 0.3478(2) 0.0553(11) Uani 1 1 d . . . . .
H12 H 0.5996 0.4955 0.3218 0.066 Uiso 1 1 calc R U . . .
C13 C 0.4385(5) 0.6645(4) 0.3209(2) 0.0541(11) Uani 1 1 d . . . . .
H13 H 0.4000 0.6617 0.2769 0.065 Uiso 1 1 calc R U . . .
C14 C 0.3703(4) 0.7749(3) 0.35902(18) 0.0398(8) Uani 1 1 d . . . . .
C15 C 0.2473(5) 0.8809(4) 0.3333(2) 0.0517(10) Uani 1 1 d . . . . .
H15 H 0.2069 0.8823 0.2889 0.062 Uiso 1 1 calc R U . . .
C16 C 0.1863(5) 0.9817(4) 0.3725(2) 0.0500(10) Uani 1 1 d . . . . .
H16 H 0.1038 1.0513 0.3551 0.060 Uiso 1 1 calc R U . . .
C17 C 0.2467(4) 0.9818(3) 0.43893(19) 0.0384(8) Uani 1 1 d . . . . .
N2 N 0.3649(3) 0.8807(2) 0.46254(14) 0.0325(6) Uani 1 1 d . . . . .
H2 H 0.4025 0.8809 0.5032 0.039 Uiso 0.5 1 calc R U P . .
C18 C 0.1862(5) 1.0880(3) 0.4848(2) 0.0539(10) Uani 1 1 d . . . . .
H18A H 0.1600 1.0566 0.5381 0.081 Uiso 1 1 calc R U . . .
H18B H 0.0917 1.1484 0.4664 0.081 Uiso 1 1 calc R U . . .
H18C H 0.2677 1.1276 0.4797 0.081 Uiso 1 1 calc R U . . .
C19 C 0.4291(4) 0.7769(3) 0.42517(17) 0.0318(7) Uani 1 1 d . . . . .
C20 C 0.5544(4) 0.6714(3) 0.45457(18) 0.0346(8) Uani 1 1 d . . . . .
C21 C 0.8937(5) 0.7619(4) 0.3392(2) 0.0564(11) Uani 1 1 d . . . . .
H21A H 0.8412 0.8483 0.3472 0.085 Uiso 1 1 calc R U . . .
H21B H 1.0080 0.7464 0.3280 0.085 Uiso 1 1 calc R U . . .
H21C H 0.8692 0.7074 0.3850 0.085 Uiso 1 1 calc R U . . .
C22 C 0.8363(4) 0.7365(3) 0.2734(2) 0.0409(8) Uani 1 1 d . . . . .
N3 N 0.7132(3) 0.8254(2) 0.24574(15) 0.0347(6) Uani 1 1 d . . . . .
H3 H 0.6686 0.8945 0.2654 0.042 Uiso 0.5 1 calc R U P . .
C23 C 0.9086(5) 0.6226(3) 0.2425(2) 0.0561(11) Uani 1 1 d . . . . .
H23 H 0.9952 0.5616 0.2631 0.067 Uiso 1 1 calc R U . . .
C24 C 0.8539(5) 0.6007(4) 0.1831(2) 0.0575(11) Uani 1 1 d . . . . .
H24 H 0.9018 0.5246 0.1633 0.069 Uiso 1 1 calc R U . . .
C25 C 0.7252(5) 0.6930(3) 0.1516(2) 0.0428(9) Uani 1 1 d . . . . .
C26 C 0.6632(6) 0.6811(4) 0.0875(2) 0.0578(11) Uani 1 1 d . . . . .
H26 H 0.7083 0.6076 0.0648 0.069 Uiso 1 1 calc R U . . .
C27 C 0.5410(5) 0.7736(4) 0.0590(2) 0.0550(11) Uani 1 1 d . . . . .
H27 H 0.5030 0.7637 0.0167 0.066 Uiso 1 1 calc R U . . .
C28 C 0.4680(5) 0.8877(4) 0.0928(2) 0.0465(9) Uani 1 1 d . . . . .
C29 C 0.3401(5) 0.9861(4) 0.0658(2) 0.0588(12) Uani 1 1 d . . . . .
H29 H 0.2998 0.9796 0.0233 0.071 Uiso 1 1 calc R U . . .
C30 C 0.2722(5) 1.0931(4) 0.1011(2) 0.0575(12) Uani 1 1 d . . . . .
H30 H 0.1870 1.1582 0.0822 0.069 Uiso 1 1 calc R U . . .
C31 C 0.3311(4) 1.1042(3) 0.1655(2) 0.0457(9) Uani 1 1 d . . . . .
N4 N 0.4581(3) 1.0108(3) 0.18862(16) 0.0378(7) Uani 1 1 d . . . . .
H4 H 0.4982 1.0192 0.2264 0.045 Uiso 0.5 1 calc R U P . .
C32 C 0.2541(5) 1.2125(4) 0.2092(3) 0.0627(12) Uani 1 1 d . . . . .
H32A H 0.1500 1.2095 0.2351 0.094 Uiso 1 1 calc R U . . .
H32B H 0.2425 1.2899 0.1744 0.094 Uiso 1 1 calc R U . . .
H32C H 0.3199 1.2083 0.2466 0.094 Uiso 1 1 calc R U . . .
C33 C 0.5288(4) 0.9016(3) 0.15538(18) 0.0351(8) Uani 1 1 d . . . . .
C34 C 0.6595(4) 0.8048(3) 0.18572(18) 0.0349(8) Uani 1 1 d . . . . .
N5 N 0.1785(2) 0.70125(14) 0.05930(9) 0.0446(8) Uani 1 1 d D . . . .
H5B H 0.1110(3) 0.6743(3) 0.0402(2) 0.067 Uiso 1 1 d D U . . .
H5A H 0.2393(3) 0.7353(3) 0.01972(16) 0.067 Uiso 1 1 d D U . . .
H5D H 0.1201(4) 0.7605(2) 0.09022(16) 0.067 Uiso 1 1 d D U . . .
H5C H 0.2437(4) 0.6349(2) 0.08704(17) 0.067 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O1 1.713(2) . ?
Nb1 O6 2.087(2) . ?
Nb1 O13 2.1098(19) . ?
Nb1 O2 2.118(2) . ?
Nb1 O5 2.143(2) . ?
Nb1 O10 2.156(2) . ?
Nb1 O9 2.239(2) . ?
O2 C1 1.294(4) . ?
O3 C1 1.211(4) . ?
O4 C2 1.214(4) . ?
C1 C2 1.523(4) . ?
C2 O5 1.283(4) . ?
O6 C3 1.284(4) . ?
O7 C3 1.217(3) . ?
O8 C4 1.225(4) . ?
O9 C4 1.295(3) . ?
C3 C4 1.552(5) . ?
O10 C5 1.296(3) . ?
O11 C5 1.220(3) . ?
O12 C6 1.210(3) . ?
O13 C6 1.289(3) . ?
C5 C6 1.530(4) . ?
C7 C8 1.495(5) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N1 1.320(4) . ?
C8 C9 1.400(5) . ?
N1 C20 1.354(4) . ?
N1 H1 0.8600 . ?
C9 C10 1.360(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.405(5) . ?
C10 H10 0.9300 . ?
C11 C20 1.404(4) . ?
C11 C12 1.425(5) . ?
C12 C13 1.341(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.437(5) . ?
C13 H13 0.9300 . ?
C14 C19 1.395(4) . ?
C14 C15 1.399(5) . ?
C15 C16 1.358(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.401(5) . ?
C16 H16 0.9300 . ?
C17 N2 1.333(4) . ?
C17 C18 1.481(5) . ?
N2 C19 1.366(4) . ?
N2 H2 0.8600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.430(4) . ?
C21 C22 1.487(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 N3 1.320(4) . ?
C22 C23 1.404(5) . ?
N3 C34 1.349(4) . ?
N3 H3 0.8600 . ?
C23 C24 1.352(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.396(5) . ?
C24 H24 0.9300 . ?
C25 C34 1.410(5) . ?
C25 C26 1.417(5) . ?
C26 C27 1.338(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.432(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.389(5) . ?
C28 C33 1.395(4) . ?
C29 C30 1.376(6) . ?
C29 H29 0.9300 . ?
C30 C31 1.401(5) . ?
C30 H30 0.9300 . ?
C31 N4 1.336(4) . ?
C31 C32 1.481(5) . ?
N4 C33 1.379(4) . ?
N4 H4 0.8600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.420(5) . ?
N5 H5B 0.90816(13) . ?
N5 H5A 0.90815(15) . ?
N5 H5D 0.90815(16) . ?
N5 H5C 0.90816(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nb1 O6 94.42(10) . . ?
O1 Nb1 O13 99.35(10) . . ?
O6 Nb1 O13 142.58(8) . . ?
O1 Nb1 O2 96.31(10) . . ?
O6 Nb1 O2 144.53(8) . . ?
O13 Nb1 O2 68.11(7) . . ?
O1 Nb1 O5 96.53(10) . . ?
O6 Nb1 O5 73.34(8) . . ?
O13 Nb1 O5 138.21(8) . . ?
O2 Nb1 O5 71.90(8) . . ?
O1 Nb1 O10 93.99(10) . . ?
O6 Nb1 O10 72.32(8) . . ?
O13 Nb1 O10 72.14(7) . . ?
O2 Nb1 O10 140.03(8) . . ?
O5 Nb1 O10 144.70(8) . . ?
O1 Nb1 O9 168.59(9) . . ?
O6 Nb1 O9 74.35(8) . . ?
O13 Nb1 O9 88.82(8) . . ?
O2 Nb1 O9 94.13(8) . . ?
O5 Nb1 O9 82.33(8) . . ?
O10 Nb1 O9 80.87(8) . . ?
C1 O2 Nb1 121.92(19) . . ?
O3 C1 O2 124.9(3) . . ?
O3 C1 C2 122.8(3) . . ?
O2 C1 C2 112.3(3) . . ?
O4 C2 O5 126.8(3) . . ?
O4 C2 C1 120.9(3) . . ?
O5 C2 C1 112.3(3) . . ?
C2 O5 Nb1 121.50(19) . . ?
C3 O6 Nb1 120.35(19) . . ?
C4 O9 Nb1 115.71(19) . . ?
O7 C3 O6 124.9(3) . . ?
O7 C3 C4 120.2(3) . . ?
O6 C3 C4 114.9(3) . . ?
O8 C4 O9 126.3(3) . . ?
O8 C4 C3 120.0(3) . . ?
O9 C4 C3 113.7(3) . . ?
C5 O10 Nb1 120.72(18) . . ?
C6 O13 Nb1 122.48(18) . . ?
O11 C5 O10 125.9(3) . . ?
O11 C5 C6 121.9(3) . . ?
O10 C5 C6 112.2(2) . . ?
O12 C6 O13 125.0(3) . . ?
O12 C6 C5 122.6(3) . . ?
O13 C6 C5 112.5(2) . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C9 121.4(3) . . ?
N1 C8 C7 117.3(3) . . ?
C9 C8 C7 121.3(3) . . ?
C8 N1 C20 118.6(3) . . ?
C8 N1 H1 120.7 . . ?
C20 N1 H1 120.7 . . ?
C10 C9 C8 120.6(4) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 119.5(3) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C20 C11 C10 116.3(3) . . ?
C20 C11 C12 119.5(3) . . ?
C10 C11 C12 124.2(3) . . ?
C13 C12 C11 121.3(3) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 120.9(3) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C19 C14 C15 118.1(3) . . ?
C19 C14 C13 118.6(3) . . ?
C15 C14 C13 123.3(3) . . ?
C16 C15 C14 120.5(3) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 120.6(3) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
N2 C17 C16 118.4(3) . . ?
N2 C17 C18 118.0(3) . . ?
C16 C17 C18 123.7(3) . . ?
C17 N2 C19 123.0(3) . . ?
C17 N2 H2 118.5 . . ?
C19 N2 H2 118.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C19 C14 119.4(3) . . ?
N2 C19 C20 119.8(3) . . ?
C14 C19 C20 120.8(3) . . ?
N1 C20 C11 123.7(3) . . ?
N1 C20 C19 117.5(3) . . ?
C11 C20 C19 118.8(3) . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N3 C22 C23 121.4(3) . . ?
N3 C22 C21 117.0(3) . . ?
C23 C22 C21 121.6(3) . . ?
C22 N3 C34 118.1(3) . . ?
C22 N3 H3 121.0 . . ?
C34 N3 H3 121.0 . . ?
C24 C23 C22 120.8(4) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C25 119.5(4) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C24 C25 C34 116.2(3) . . ?
C24 C25 C26 123.8(4) . . ?
C34 C25 C26 120.0(4) . . ?
C27 C26 C25 121.2(4) . . ?
C27 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C26 C27 C28 120.9(4) . . ?
C26 C27 H27 119.5 . . ?
C28 C27 H27 119.5 . . ?
C29 C28 C33 118.2(4) . . ?
C29 C28 C27 123.2(4) . . ?
C33 C28 C27 118.6(4) . . ?
C30 C29 C28 121.0(4) . . ?
C30 C29 H29 119.5 . . ?
C28 C29 H29 119.5 . . ?
C29 C30 C31 120.3(4) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
N4 C31 C30 117.8(4) . . ?
N4 C31 C32 119.8(4) . . ?
C30 C31 C32 122.3(4) . . ?
C31 N4 C33 123.7(3) . . ?
C31 N4 H4 118.1 . . ?
C33 N4 H4 118.1 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N4 C33 C28 118.9(3) . . ?
N4 C33 C34 120.0(3) . . ?
C28 C33 C34 121.1(3) . . ?
N3 C34 C25 124.0(3) . . ?
N3 C34 C33 117.8(3) . . ?
C25 C34 C33 118.2(3) . . ?
H5B N5 H5A 109.47(2) . . ?
H5B N5 H5D 109.47(2) . . ?
H5A N5 H5D 109.47(2) . . ?
H5B N5 H5C 109.47(2) . . ?
H5A N5 H5C 109.47(3) . . ?
H5D N5 H5C 109.47(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5C O3 0.9082(2) 2.156(4) 2.795(3) 126.6(2) .
N5 H5C O4 0.9082(2) 2.087(3) 2.912(3) 150.5(3) .
N2 H2 O7 0.86 2.56 2.826(3) 98.8 2_666
N1 H1 O8 0.86 2.40 3.256(3) 173.3 2_666
N2 H2 O8 0.86 2.16 2.990(3) 162.5 2_666
N3 H3 O9 0.86 2.64 3.418(3) 150.9 1_565
N4 H4 O9 0.86 2.18 2.898(3) 141.1 1_565
N5 H5D O11 0.9082(2) 2.118(3) 2.954(3) 152.4(3) 1_465
N5 H5D O12 0.9082(2) 2.169(4) 2.770(3) 122.9(2) 1_465
N5 H5C O3 0.9082(2) 2.156(4) 2.795(3) 126.6(2) .
N5 H5C O4 0.9082(2) 2.087(3) 2.912(3) 150.5(3) .
N5 H5B O1 0.9082(1) 2.642(4) 3.221(3) 122.4(2) 2_665
N5 H5A O2 0.9082(2) 2.304(3) 3.093(3) 145.2(3) 2_665
N5 H5A O13 0.9082(2) 2.478(3) 3.246(3) 142.5(2) 2_665

_refine_diff_density_max         0.997
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.110



_exptl_crystal_recrystallization_method 'Slow diffusion'
####################################################################### 
# 
# 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 1402554'
_audit_update_record             
;
2015-05-24 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H60 Cr2 Nb2 O30 S10'
_chemical_formula_weight         1487.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4285(7)
_cell_length_b                   12.1741(9)
_cell_length_c                   12.1850(10)
_cell_angle_alpha                98.122(6)
_cell_angle_beta                 116.838(7)
_cell_angle_gamma                94.962(5)
_cell_volume                     1475.7(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2232
_cell_measurement_theta_min      2.3710
_cell_measurement_theta_max      25.5810

_exptl_crystal_description       Tabular
_exptl_crystal_colour            'Emerald Green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_F_000             758
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.171
_shelx_estimated_absorpt_T_min   0.835
_shelx_estimated_absorpt_T_max   0.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
'Sun May 03 19:25:34 2015'
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported S'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9435
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.630
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             5834
_reflns_number_gt                4357
_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       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'CysAlisPro 171.37.34b'
_computing_data_reduction        'CysAlisPro 171.37.34b'
_computing_structure_solution    'SuperFlip (Palatinus & Chapius, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0689P)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         5834
_refine_ls_number_parameters     361
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0538
_refine_ls_wR_factor_ref         0.1532
_refine_ls_wR_factor_gt          0.1363
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
Nb1 Nb 0.36408(3) 0.12906(3) 0.37404(3) 0.03553(16) Uani 1 1 d . . . . .
Cr1 Cr 0.61469(6) 0.16945(6) 0.70664(6) 0.0342(2) Uani 1 1 d . . . . .
S1 S 0.61264(13) 0.41468(10) 0.67203(12) 0.0506(3) Uani 1 1 d . . . . .
S3 S 0.88059(12) 0.15427(12) 0.93095(12) 0.0520(3) Uani 1 1 d . . . . .
S2 S 0.79411(12) 0.17664(12) 0.57432(12) 0.0528(3) Uani 1 1 d . . . . .
O10 O 0.3046(3) 0.2912(3) 0.3989(3) 0.0548(9) Uani 1 1 d . . . . .
O7 O 0.1895(3) 0.0972(3) 0.3820(3) 0.0527(9) Uani 1 1 d . . . . .
O9 O 0.1585(5) 0.3806(5) 0.4314(6) 0.1172(19) Uani 1 1 d . . . . .
O13 O 0.7422(3) 0.1865(3) 0.8883(3) 0.0518(9) Uani 1 1 d . . . . .
O11 O 0.5909(3) 0.3288(3) 0.7451(3) 0.0507(8) Uani 1 1 d . . . . .
O3 O 0.4953(3) 0.2035(3) 0.3235(4) 0.0576(9) Uani 1 1 d . . . . .
O4 O 0.5337(6) 0.2470(5) 0.1710(6) 0.135(2) Uani 1 1 d . . . . .
O2 O 0.4867(3) 0.1578(3) 0.5355(3) 0.0521(9) Uani 1 1 d . . . . .
O6 O 0.2467(3) 0.1393(3) 0.1773(3) 0.0579(10) Uani 1 1 d . . . . .
O1 O 0.3606(3) -0.0172(3) 0.3247(3) 0.0512(9) Uani 1 1 d . . . . .
O12 O 0.7644(3) 0.2280(3) 0.6798(3) 0.0456(8) Uani 1 1 d . . . . .
O5 O 0.2600(6) 0.1759(5) 0.0104(4) 0.1125(19) Uani 1 1 d . . . . .
O14 O 0.4734(4) 0.1244(4) 0.7477(5) 0.0875(14) Uani 1 1 d . . . . .
C6 C 0.7625(6) 0.5062(5) 0.7840(6) 0.081(2) Uani 1 1 d . . . . .
H6A H 0.7572 0.5306 0.8598 0.122 Uiso 1 1 calc R U . . .
H6B H 0.7748 0.5705 0.7505 0.122 Uiso 1 1 calc R U . . .
H6C H 0.8364 0.4669 0.8020 0.122 Uiso 1 1 calc R U . . .
O8 O 0.0290(5) 0.1658(5) 0.4128(5) 0.1158(19) Uani 1 1 d . . . . .
C8 C 0.9614(5) 0.1559(6) 0.6576(6) 0.0787(19) Uani 1 1 d . . . . .
H8A H 1.0160 0.2256 0.7114 0.118 Uiso 1 1 calc R U . . .
H8B H 0.9927 0.1305 0.5989 0.118 Uiso 1 1 calc R U . . .
H8C H 0.9658 0.1004 0.7074 0.118 Uiso 1 1 calc R U . . .
C5 C 0.4971(6) 0.5041(5) 0.6659(6) 0.0729(18) Uani 1 1 d . . . . .
H5A H 0.4086 0.4614 0.6212 0.109 Uiso 1 1 calc R U . . .
H5B H 0.5044 0.5630 0.6234 0.109 Uiso 1 1 calc R U . . .
H5C H 0.5156 0.5367 0.7497 0.109 Uiso 1 1 calc R U . . .
C7 C 0.8203(7) 0.2945(6) 0.5132(6) 0.0819(19) Uani 1 1 d . . . . .
H7A H 0.7378 0.3212 0.4710 0.123 Uiso 1 1 calc R U . . .
H7B H 0.8531 0.2730 0.4547 0.123 Uiso 1 1 calc R U . . .
H7C H 0.8842 0.3532 0.5806 0.123 Uiso 1 1 calc R U . . .
C9 C 0.9899(6) 0.2853(5) 0.9940(6) 0.085(2) Uani 1 1 d . . . . .
H9A H 0.9884 0.3189 0.9267 0.128 Uiso 1 1 calc R U . . .
H9B H 1.0787 0.2737 1.0464 0.128 Uiso 1 1 calc R U . . .
H9C H 0.9620 0.3344 1.0431 0.128 Uiso 1 1 calc R U . . .
C10 C 0.9130(6) 0.1068(6) 1.0710(5) 0.080(2) Uani 1 1 d . . . . .
H10A H 0.8924 0.1597 1.1232 0.121 Uiso 1 1 calc R U . . .
H10B H 1.0053 0.1003 1.1149 0.121 Uiso 1 1 calc R U . . .
H10C H 0.8590 0.0347 1.0509 0.121 Uiso 1 1 calc R U . . .
C4 C 0.2006(6) 0.2954(6) 0.4128(5) 0.0694(17) Uani 1 1 d . . . . .
C1 C 0.4590(7) 0.2119(5) 0.2081(7) 0.0726(17) Uani 1 1 d . . . . .
C2 C 0.3092(7) 0.1727(5) 0.1205(6) 0.0671(16) Uani 1 1 d . . . . .
C3 C 0.1299(6) 0.1791(6) 0.4031(5) 0.0662(17) Uani 1 1 d . . . . .
O15 O 1.0813(8) 0.4467(7) 0.8335(7) 0.171(3) Uani 1 1 d . . . . .
C13 C 1.1581(11) 0.5384(10) 0.6948(10) 0.177(5) Uani 1 1 d . . . . .
H13A H 1.0698 0.5152 0.6261 0.266 Uiso 1 1 calc R U . A 1
H13B H 1.2105 0.4810 0.6943 0.266 Uiso 1 1 calc R U . A 1
H13C H 1.1981 0.6072 0.6864 0.266 Uiso 1 1 calc R U . A 1
C12 C 1.3265(12) 0.5590(18) 0.9384(12) 0.271(9) Uani 1 1 d . . . . .
H12A H 1.3378 0.5653 1.0222 0.407 Uiso 1 1 calc R U . B 1
H12B H 1.3812 0.6217 0.9353 0.407 Uiso 1 1 calc R U . B 1
H12C H 1.3521 0.4902 0.9147 0.407 Uiso 1 1 calc R U . B 1
S5B S 1.1512(5) 0.5588(7) 0.8292(5) 0.099(3) Uani 0.491(13) 1 d . . P C 1
S5A S 1.1928(8) 0.4820(9) 0.8258(7) 0.146(4) Uani 0.509(13) 1 d . . P C 2
S4A S 0.3473(5) 0.1185(5) 0.7056(5) 0.071(2) Uiso 0.321(5) 1 d . . P . .
C11A C 0.269(2) 0.024(2) 0.748(2) 0.047(5) Uiso 0.321(5) 1 d . . P . .
H11A H 0.2503 -0.0486 0.6945 0.070 Uiso 0.321(5) 1 calc R U P . .
H11B H 0.1878 0.0460 0.7398 0.070 Uiso 0.321(5) 1 calc R U P . .
H11C H 0.3255 0.0192 0.8335 0.070 Uiso 0.321(5) 1 calc R U P . .
C12A C 0.326(3) 0.228(3) 0.772(3) 0.109(9) Uiso 0.321(5) 1 d . . P . .
H12D H 0.3963 0.2491 0.8568 0.163 Uiso 0.321(5) 1 calc R U P . .
H12E H 0.2420 0.2144 0.7721 0.163 Uiso 0.321(5) 1 calc R U P . .
H12F H 0.3262 0.2869 0.7277 0.163 Uiso 0.321(5) 1 calc R U P . .
S4B S 0.4106(4) 0.0334(4) 0.7617(4) 0.0715(17) Uiso 0.394(6) 1 d . . P . .
C12B C 0.237(2) 0.050(2) 0.710(2) 0.104(9) Uiso 0.394(6) 1 d . . P . .
H12G H 0.2318 0.1027 0.7739 0.155 Uiso 0.394(6) 1 calc R U P . .
H12H H 0.1845 -0.0213 0.6962 0.155 Uiso 0.394(6) 1 calc R U P . .
H12I H 0.2038 0.0781 0.6337 0.155 Uiso 0.394(6) 1 calc R U P . .
C11B C 0.4686(19) 0.0364(17) 0.9221(16) 0.098(6) Uiso 0.394(6) 1 d . . P . .
H11D H 0.5094 0.1118 0.9688 0.147 Uiso 0.394(6) 1 calc R U P . .
H11E H 0.5328 -0.0129 0.9493 0.147 Uiso 0.394(6) 1 calc R U P . .
H11F H 0.3953 0.0119 0.9363 0.147 Uiso 0.394(6) 1 calc R U P . .
S4C S 0.4328(5) 0.1305(5) 0.8269(5) 0.062(2) Uiso 0.273(5) 1 d . . P . .
C12C C 0.292(4) -0.002(3) 0.772(3) 0.103(14) Uiso 0.273(5) 1 d . . P . .
H12J H 0.2570 -0.0306 0.6833 0.154 Uiso 0.273(5) 1 calc R U P . .
H12K H 0.2211 0.0195 0.7878 0.154 Uiso 0.273(5) 1 calc R U P . .
H12L H 0.3281 -0.0597 0.8170 0.154 Uiso 0.273(5) 1 calc R U P . .
C11C C 0.362(3) 0.256(2) 0.840(3) 0.083(8) Uiso 0.273(5) 1 d . . P . .
H11G H 0.4198 0.3203 0.8450 0.125 Uiso 0.273(5) 1 calc R U P . .
H11H H 0.3514 0.2649 0.9147 0.125 Uiso 0.273(5) 1 calc R U P . .
H11I H 0.2765 0.2486 0.7680 0.125 Uiso 0.273(5) 1 calc R U 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
Nb1 O2 1.786(3) . ?
Nb1 O1 1.789(3) . ?
Nb1 O7 2.048(3) . ?
Nb1 O3 2.051(4) . ?
Nb1 O10 2.168(3) . ?
Nb1 O6 2.184(3) . ?
Cr1 O2 1.906(3) . ?
Cr1 O1 1.910(3) 2_656 ?
Cr1 O14 1.952(4) . ?
Cr1 O12 1.976(3) . ?
Cr1 O13 1.993(3) . ?
Cr1 O11 2.002(3) . ?
S1 O11 1.538(3) . ?
S1 C5 1.765(5) . ?
S1 C6 1.780(5) . ?
S3 O13 1.532(3) . ?
S3 C10 1.768(6) . ?
S3 C9 1.772(6) . ?
S2 O12 1.536(3) . ?
S2 C7 1.770(6) . ?
S2 C8 1.775(5) . ?
O10 C4 1.278(7) . ?
O7 C3 1.314(7) . ?
O9 C4 1.216(7) . ?
O3 C1 1.296(7) . ?
O4 C1 1.206(7) . ?
O6 C2 1.277(7) . ?
O1 Cr1 1.910(3) 2_656 ?
O5 C2 1.206(7) . ?
O14 S4C 1.242(7) . ?
O14 S4A 1.284(6) . ?
O14 S4B 1.341(6) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
O8 C3 1.212(7) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C4 C3 1.530(9) . ?
C1 C2 1.537(9) . ?
O15 S5A 1.357(10) . ?
O15 S5B 1.540(10) . ?
C13 S5B 1.660(11) . ?
C13 S5A 1.721(11) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C12 S5A 1.610(14) . ?
C12 S5B 1.837(14) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
S4A S4C 1.330(7) . ?
S4A S4B 1.395(6) . ?
S4A C12A 1.55(3) . ?
S4A C11A 1.67(2) . ?
C11A H11A 0.9600 . ?
C11A H11B 0.9600 . ?
C11A H11C 0.9600 . ?
C12A H12D 0.9600 . ?
C12A H12E 0.9600 . ?
C12A H12F 0.9600 . ?
S4B S4C 1.262(7) . ?
S4B C11B 1.752(17) . ?
S4B C12B 1.83(2) . ?
C12B H12G 0.9600 . ?
C12B H12H 0.9600 . ?
C12B H12I 0.9600 . ?
C11B H11D 0.9600 . ?
C11B H11E 0.9600 . ?
C11B H11F 0.9600 . ?
S4C C11C 1.81(3) . ?
S4C C12C 1.98(4) . ?
C12C H12J 0.9600 . ?
C12C H12K 0.9600 . ?
C12C H12L 0.9600 . ?
C11C H11G 0.9600 . ?
C11C H11H 0.9600 . ?
C11C H11I 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
O2 Nb1 O1 102.74(14) . . ?
O2 Nb1 O7 102.94(14) . . ?
O1 Nb1 O7 92.28(15) . . ?
O2 Nb1 O3 91.77(16) . . ?
O1 Nb1 O3 101.82(15) . . ?
O7 Nb1 O3 156.91(14) . . ?
O2 Nb1 O10 90.52(13) . . ?
O1 Nb1 O10 162.82(14) . . ?
O7 Nb1 O10 73.90(14) . . ?
O3 Nb1 O10 88.46(14) . . ?
O2 Nb1 O6 163.26(15) . . ?
O1 Nb1 O6 89.03(14) . . ?
O7 Nb1 O6 88.23(13) . . ?
O3 Nb1 O6 73.99(14) . . ?
O10 Nb1 O6 80.54(13) . . ?
O2 Cr1 O1 91.97(13) . 2_656 ?
O2 Cr1 O14 90.50(18) . . ?
O1 Cr1 O14 91.79(18) 2_656 . ?
O2 Cr1 O12 93.24(14) . . ?
O1 Cr1 O12 92.52(14) 2_656 . ?
O14 Cr1 O12 174.19(17) . . ?
O2 Cr1 O13 176.82(14) . . ?
O1 Cr1 O13 90.46(14) 2_656 . ?
O14 Cr1 O13 87.37(18) . . ?
O12 Cr1 O13 88.70(14) . . ?
O2 Cr1 O11 89.67(13) . . ?
O1 Cr1 O11 178.21(13) 2_656 . ?
O14 Cr1 O11 87.49(18) . . ?
O12 Cr1 O11 88.09(14) . . ?
O13 Cr1 O11 87.87(14) . . ?
O11 S1 C5 102.7(3) . . ?
O11 S1 C6 104.2(2) . . ?
C5 S1 C6 99.4(3) . . ?
O13 S3 C10 103.3(3) . . ?
O13 S3 C9 104.0(3) . . ?
C10 S3 C9 100.1(3) . . ?
O12 S2 C7 103.2(3) . . ?
O12 S2 C8 102.9(2) . . ?
C7 S2 C8 99.2(3) . . ?
C4 O10 Nb1 118.7(4) . . ?
C3 O7 Nb1 121.5(4) . . ?
S3 O13 Cr1 121.17(19) . . ?
S1 O11 Cr1 119.96(19) . . ?
C1 O3 Nb1 121.3(4) . . ?
Nb1 O2 Cr1 173.1(2) . . ?
C2 O6 Nb1 117.7(4) . . ?
Nb1 O1 Cr1 170.85(19) . 2_656 ?
S2 O12 Cr1 125.70(18) . . ?
S4C O14 S4A 63.5(4) . . ?
S4C O14 S4B 58.4(4) . . ?
S4A O14 S4B 64.2(3) . . ?
S4C O14 Cr1 148.1(4) . . ?
S4A O14 Cr1 141.0(4) . . ?
S4B O14 Cr1 141.2(4) . . ?
S1 C6 H6A 109.5 . . ?
S1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
S1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
S2 C8 H8A 109.5 . . ?
S2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
S2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
S1 C5 H5A 109.5 . . ?
S1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
S1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
S2 C7 H7A 109.5 . . ?
S2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
S2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
S3 C9 H9A 109.5 . . ?
S3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
S3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
S3 C10 H10A 109.5 . . ?
S3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
S3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O9 C4 O10 125.6(7) . . ?
O9 C4 C3 121.5(6) . . ?
O10 C4 C3 112.8(5) . . ?
O4 C1 O3 124.3(7) . . ?
O4 C1 C2 122.2(7) . . ?
O3 C1 C2 113.5(5) . . ?
O5 C2 O6 125.7(6) . . ?
O5 C2 C1 121.4(6) . . ?
O6 C2 C1 112.9(5) . . ?
O8 C3 O7 124.6(7) . . ?
O8 C3 C4 122.6(6) . . ?
O7 C3 C4 112.9(5) . . ?
S5B C13 H13A 109.5 . . ?
S5B C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
S5B C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
S5B C12 H12A 109.5 . . ?
S5B C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
S5B C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O15 S5B C13 106.4(6) . . ?
O15 S5B C12 102.4(8) . . ?
C13 S5B C12 99.4(7) . . ?
O15 S5A C12 125.4(10) . . ?
O15 S5A C13 112.3(7) . . ?
C12 S5A C13 106.4(9) . . ?
O14 S4A S4C 56.7(4) . . ?
O14 S4A S4B 59.9(3) . . ?
S4C S4A S4B 55.1(3) . . ?
O14 S4A C12A 106.9(12) . . ?
S4C S4A C12A 74.5(11) . . ?
S4B S4A C12A 127.1(12) . . ?
O14 S4A C11A 117.8(10) . . ?
S4C S4A C11A 78.9(9) . . ?
S4B S4A C11A 59.3(9) . . ?
C12A S4A C11A 99.0(15) . . ?
S4A C11A H11A 109.5 . . ?
S4A C11A H11B 109.5 . . ?
H11A C11A H11B 109.5 . . ?
S4A C11A H11C 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?
S4A C12A H12D 109.5 . . ?
S4A C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
S4A C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
S4C S4B O14 56.9(4) . . ?
S4C S4B S4A 59.8(4) . . ?
O14 S4B S4A 55.9(3) . . ?
S4C S4B C11B 65.9(7) . . ?
O14 S4B C11B 109.2(8) . . ?
S4A S4B C11B 121.4(7) . . ?
S4C S4B C12B 82.4(8) . . ?
O14 S4B C12B 108.0(9) . . ?
S4A S4B C12B 52.3(8) . . ?
C11B S4B C12B 101.7(10) . . ?
S4B C12B H12G 109.5 . . ?
S4B C12B H12H 109.5 . . ?
H12G C12B H12H 109.5 . . ?
S4B C12B H12I 109.5 . . ?
H12G C12B H12I 109.5 . . ?
H12H C12B H12I 109.5 . . ?
S4B C11B H11D 109.5 . . ?
S4B C11B H11E 109.5 . . ?
H11D C11B H11E 109.5 . . ?
S4B C11B H11F 109.5 . . ?
H11D C11B H11F 109.5 . . ?
H11E C11B H11F 109.5 . . ?
O14 S4C S4B 64.7(4) . . ?
O14 S4C S4A 59.8(4) . . ?
S4B S4C S4A 65.1(4) . . ?
O14 S4C C11C 113.3(11) . . ?
S4B S4C C11C 144.1(10) . . ?
S4A S4C C11C 82.8(9) . . ?
O14 S4C C12C 106.9(11) . . ?
S4B S4C C12C 47.1(11) . . ?
S4A S4C C12C 69.5(10) . . ?
C11C S4C C12C 108.0(15) . . ?
S4C C12C H12J 109.5 . . ?
S4C C12C H12K 109.5 . . ?
H12J C12C H12K 109.5 . . ?
S4C C12C H12L 109.5 . . ?
H12J C12C H12L 109.5 . . ?
H12K C12C H12L 109.5 . . ?
S4C C11C H11G 109.5 . . ?
S4C C11C H11H 109.5 . . ?
H11G C11C H11H 109.5 . . ?
S4C C11C H11I 109.5 . . ?
H11G C11C H11I 109.5 . . ?
H11H C11C H11I 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C6 H6B O10 0.96 2.57 3.460(7) 154.1 2_666
C8 H8B O8 0.96 2.57 3.416(9) 147.5 1_655
C8 H8C O7 0.96 2.63 3.257(8) 123.6 2_656
C9 H9A O15 0.96 2.48 3.369(9) 154.2 .
C9 H9B O5 0.96 2.65 3.402(9) 135.8 1_656
C9 H9C S5B 0.96 2.71 3.654(10) 169.8 2_767
C10 H10B O6 0.96 2.49 3.393(7) 156.9 1_656
C10 H10C O5 0.96 2.63 3.582(9) 171.0 2_656
C12 H12A O11 0.96 2.66 3.553(14) 155.5 2_767
C12 H12B O4 0.96 2.58 3.474(17) 155.9 2_766

_refine_diff_density_max         0.980
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.116



_exptl_crystal_recrystallization_method 'Slow Diffusion'
_exptl_crystal_preparation       'Magnetic properties'
