# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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. 
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data_1
_database_code_depnum_ccdc_archive 'CCDC 1417629'
_audit_update_record             
;
2015-11-18 deposited with the CCDC.
2015-12-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H156 Er4 N18 O49'
_chemical_formula_weight         3015.42

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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'

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

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

_cell_length_a                   29.881(5)
_cell_length_b                   29.881(5)
_cell_length_c                   29.881(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     26680(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9827
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.44

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_F_000             12176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    2.577
_shelx_estimated_absorpt_T_min   0.554
_shelx_estimated_absorpt_T_max   0.640
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_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            57009
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.180
_diffrn_reflns_theta_max         25.494
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8282
_reflns_number_gt                6849
_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.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.001 -0.009 -0.005 17160.0 5473.8
_platon_squeeze_details          
;
In order to subtract the contribution from the disordered solvent molecules,
the SQUEEZE command was applied.
SQUEEZE removed disordered solvent molecules per formula unit. This valueis calculated based upon volume/count_electrons analysis.
See ref. P. van der Sluis and A. L. Spek, Acta Crystallogr., 1990, A46, 194.

CHEMW03_ALERT_2_A ALERT: The ratio of given/expected molecular weight as
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for two disordered nitrate ions, thirteen disordered DMF and ten disordered H2O omitted by SQUEEZE.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    diamond
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0553P)²+5.8825P] 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         8282
_refine_ls_number_parameters     255
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0951
_refine_ls_wR_factor_gt          0.0930
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.104
_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
Er1 Er 0.24316(2) 0.18123(2) 0.14139(2) 0.03741(8) Uani 1 1 d . . . . .
Er2 Er 0.24763(2) 0.24763(2) 0.24763(2) 0.03665(9) Uani 1 3 d S T P . .
O2 O 0.31556(11) 0.20182(15) 0.15652(12) 0.0975(13) Uani 1 1 d . U . . .
O1 O 0.31787(13) 0.24746(19) 0.21811(19) 0.153(3) Uani 1 1 d . . . . .
O3 O 0.64100(11) 0.25869(11) -0.10580(10) 0.0696(9) Uani 1 1 d . . . . .
O4 O 0.69875(10) 0.29889(12) -0.08033(9) 0.0725(9) Uani 1 1 d . . . . .
O5 O 0.29453(13) 0.29453(13) 0.29453(13) 0.161(4) Uani 1 3 d S T P . .
H5B H 0.3175 0.2800 0.3029 0.242 Uiso 0.3333 1 d R U P . .
H5C H 0.3027 0.3176 0.2800 0.242 Uiso 0.3333 1 d R U P . .
O6 O 0.24750(7) 0.17303(7) 0.22105(7) 0.0333(5) Uani 1 1 d . . . . .
H6A H 0.2737 0.1620 0.2298 0.040 Uiso 1 1 d R U . . .
O7 O 0.17074(8) 0.17074(8) 0.17074(8) 0.0435(10) Uani 1 3 d DS T P . .
H7A H 0.15427(17) 0.1543(2) 0.1543(2) 0.052 Uiso 1 3 d DR U P . .
O8 O 0.28615(13) 0.16532(18) 0.07392(12) 0.1276(18) Uani 1 1 d . U . . .
H8A H 0.2716 0.1471 0.0576 0.191 Uiso 1 1 d R U . . .
H8B H 0.2905 0.1895 0.0596 0.191 Uiso 1 1 d R U . . .
N1 N 0.60501(14) 0.24403(16) 0.18525(12) 0.0838(14) Uani 1 1 d . U . . .
C1 C 0.33628(17) 0.2267(2) 0.18531(19) 0.0919(19) Uani 1 1 d . . . . .
C2 C 0.38596(16) 0.2300(2) 0.17903(16) 0.0796(16) Uani 1 1 d . . . . .
C7 C 0.40616(16) 0.2133(2) 0.14008(16) 0.0877(17) Uani 1 1 d . U . . .
H3 H 0.3889 0.1986 0.1188 0.105 Uiso 1 1 calc R U . . .
C3 C 0.41357(18) 0.2497(2) 0.21113(19) 0.105(2) Uani 1 1 d . . . . .
H4 H 0.4007 0.2593 0.2378 0.126 Uiso 1 1 calc R U . . .
C6 C 0.45209(15) 0.2185(2) 0.13311(16) 0.092(2) Uani 1 1 d . . . . .
H5 H 0.4647 0.2078 0.1067 0.111 Uiso 1 1 calc R U . . .
C4 C 0.45908(17) 0.2556(2) 0.20522(19) 0.112(3) Uani 1 1 d . . . . .
H6 H 0.4762 0.2697 0.2270 0.135 Uiso 1 1 calc R U . . .
C5 C 0.47953(15) 0.2394(2) 0.16457(16) 0.0844(18) Uani 1 1 d . . . . .
C8 C 0.56083(16) 0.2413(2) 0.19107(16) 0.089(2) Uani 1 1 d . . . . .
H8 H 0.5503 0.2366 0.2200 0.107 Uiso 1 1 calc R U . . .
C9 C 0.52887(15) 0.24481(19) 0.15652(15) 0.0764(16) Uani 1 1 d . . . . .
C10 C 0.54512(15) 0.25245(18) 0.11384(16) 0.0814(17) Uani 1 1 d . . . . .
H10 H 0.5252 0.2554 0.0901 0.098 Uiso 1 1 calc R U . . .
C11 C 0.59190(14) 0.25587(19) 0.10589(15) 0.0778(16) Uani 1 1 d . . . . .
C12 C 0.61960(15) 0.2505(2) 0.14276(16) 0.089(2) Uani 1 1 d . . . . .
H12 H 0.6503 0.2514 0.1380 0.106 Uiso 1 1 calc R U . . .
C17 C 0.61008(16) 0.2608(2) 0.05978(15) 0.0794(16) Uani 1 1 d . . . . .
C18 C 0.58807(19) 0.2435(2) 0.02251(18) 0.0961(19) Uani 1 1 d . U . . .
H14 H 0.5617 0.2274 0.0265 0.115 Uiso 1 1 calc R U . . .
C16 C 0.65052(17) 0.2831(3) 0.05184(16) 0.108(2) Uani 1 1 d . . . . .
H15 H 0.6665 0.2943 0.0761 0.130 Uiso 1 1 calc R U . . .
C19 C 0.60462(19) 0.2498(2) -0.02040(16) 0.100(2) Uani 1 1 d . . . . .
H16 H 0.5887 0.2388 -0.0448 0.120 Uiso 1 1 calc R U . . .
C15 C 0.66757(17) 0.2891(2) 0.00923(15) 0.096(2) Uani 1 1 d . . . . .
H17 H 0.6944 0.3044 0.0053 0.115 Uiso 1 1 calc R U . . .
C14 C 0.64509(15) 0.2725(2) -0.02744(15) 0.0761(15) Uani 1 1 d . . . . .
C13 C 0.66282(16) 0.27707(18) -0.07523(14) 0.0640(12) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O3 2.255(3) 10_554 ?
Er1 O6 2.292(2) 5 ?
Er1 O2 2.294(3) . ?
Er1 O4 2.333(3) 3_455 ?
Er1 O7 2.3559(17) . ?
Er1 O6 2.397(2) . ?
Er1 O8 2.437(3) . ?
Er1 Er1 3.7537(7) 6 ?
Er1 Er1 3.7538(7) 5 ?
Er2 O1 2.277(4) . ?
Er2 O1 2.277(4) 5 ?
Er2 O1 2.277(4) 6 ?
Er2 O6 2.366(2) 5 ?
Er2 O6 2.366(2) 6 ?
Er2 O6 2.366(2) . ?
Er2 O5 2.427(7) . ?
Er2 Er1 3.7461(7) 6 ?
Er2 Er1 3.7461(7) 5 ?
O2 C1 1.295(6) . ?
O1 C1 1.283(7) . ?
O3 C13 1.249(5) . ?
O3 Er1 2.255(3) 9 ?
O4 C13 1.265(5) . ?
O4 Er1 2.333(3) 3 ?
O6 Er1 2.292(2) 6 ?
O7 Er1 2.3560(17) 6 ?
O7 Er1 2.3560(17) 5 ?
N1 C8 1.334(6) . ?
N1 C12 1.356(6) . ?
C1 C2 1.499(7) . ?
C2 C3 1.395(7) . ?
C2 C7 1.403(6) . ?
C7 C6 1.397(6) . ?
C3 C4 1.383(7) . ?
C6 C5 1.394(7) . ?
C4 C5 1.443(7) . ?
C5 C9 1.503(6) . ?
C8 C9 1.410(6) . ?
C9 C10 1.384(6) . ?
C10 C11 1.422(6) . ?
C11 C12 1.387(6) . ?
C11 C17 1.488(6) . ?
C17 C18 1.393(7) . ?
C17 C16 1.400(7) . ?
C18 C19 1.387(7) . ?
C16 C15 1.383(6) . ?
C19 C14 1.403(7) . ?
C15 C14 1.377(7) . ?
C14 C13 1.529(6) . ?

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
O3 Er1 O6 149.19(9) 10_554 5 ?
O3 Er1 O2 106.99(14) 10_554 . ?
O6 Er1 O2 87.64(12) 5 . ?
O3 Er1 O4 103.69(13) 10_554 3_455 ?
O6 Er1 O4 86.48(10) 5 3_455 ?
O2 Er1 O4 128.48(13) . 3_455 ?
O3 Er1 O7 81.16(10) 10_554 . ?
O6 Er1 O7 72.34(9) 5 . ?
O2 Er1 O7 145.94(13) . . ?
O4 Er1 O7 78.61(10) 3_455 . ?
O3 Er1 O6 84.50(10) 10_554 . ?
O6 Er1 O6 72.19(11) 5 . ?
O2 Er1 O6 77.32(10) . . ?
O4 Er1 O6 146.48(9) 3_455 . ?
O7 Er1 O6 70.51(9) . . ?
O3 Er1 O8 79.27(15) 10_554 . ?
O6 Er1 O8 131.43(14) 5 . ?
O2 Er1 O8 73.64(13) . . ?
O4 Er1 O8 72.70(12) 3_455 . ?
O7 Er1 O8 140.01(14) . . ?
O6 Er1 O8 140.63(10) . . ?
O3 Er1 Er1 71.03(8) 10_554 6 ?
O6 Er1 Er1 78.33(5) 5 6 ?
O2 Er1 Er1 112.97(9) . 6 ?
O4 Er1 Er1 115.72(8) 3_455 6 ?
O7 Er1 Er1 37.19(5) . 6 ?
O6 Er1 Er1 35.86(5) . 6 ?
O8 Er1 Er1 150.24(13) . 6 ?
O3 Er1 Er1 118.33(8) 10_554 5 ?
O6 Er1 Er1 37.78(6) 5 5 ?
O2 Er1 Er1 124.70(10) . 5 ?
O4 Er1 Er1 70.22(8) 3_455 5 ?
O7 Er1 Er1 37.19(5) . 5 ?
O6 Er1 Er1 77.25(5) . 5 ?
O8 Er1 Er1 141.77(10) . 5 ?
Er1 Er1 Er1 60.0 6 5 ?
O1 Er2 O1 111.00(10) . 5 ?
O1 Er2 O1 111.00(10) . 6 ?
O1 Er2 O1 110.99(10) 5 6 ?
O1 Er2 O6 86.81(15) . 5 ?
O1 Er2 O6 82.50(13) 5 5 ?
O1 Er2 O6 150.13(11) 6 5 ?
O1 Er2 O6 150.12(11) . 6 ?
O1 Er2 O6 86.82(15) 5 6 ?
O1 Er2 O6 82.50(13) 6 6 ?
O6 Er2 O6 71.45(8) 5 6 ?
O1 Er2 O6 82.50(13) . . ?
O1 Er2 O6 150.13(11) 5 . ?
O1 Er2 O6 86.82(15) 6 . ?
O6 Er2 O6 71.45(8) 5 . ?
O6 Er2 O6 71.45(8) 6 . ?
O1 Er2 O5 72.10(10) . . ?
O1 Er2 O5 72.10(10) 5 . ?
O1 Er2 O5 72.10(10) 6 . ?
O6 Er2 O5 137.61(5) 5 . ?
O6 Er2 O5 137.61(5) 6 . ?
O6 Er2 O5 137.61(5) . . ?
O1 Er2 Er1 118.20(12) . 6 ?
O1 Er2 Er1 125.17(14) 5 6 ?
O1 Er2 Er1 72.75(11) 6 6 ?
O6 Er2 Er1 77.72(5) 5 6 ?
O6 Er2 Er1 38.43(5) 6 6 ?
O6 Er2 Er1 35.79(5) . 6 ?
O5 Er2 Er1 144.653(3) . 6 ?
O1 Er2 Er1 125.17(14) . 5 ?
O1 Er2 Er1 72.75(11) 5 5 ?
O1 Er2 Er1 118.21(12) 6 5 ?
O6 Er2 Er1 38.43(5) 5 5 ?
O6 Er2 Er1 35.79(5) 6 5 ?
O6 Er2 Er1 77.72(5) . 5 ?
O5 Er2 Er1 144.653(3) . 5 ?
Er1 Er2 Er1 60.135(6) 6 5 ?
C1 O2 Er1 137.4(3) . . ?
C1 O1 Er2 133.8(4) . . ?
C13 O3 Er1 137.6(3) . 9 ?
C13 O4 Er1 135.1(3) . 3 ?
Er1 O6 Er2 107.06(8) 6 . ?
Er1 O6 Er1 106.36(8) 6 . ?
Er2 O6 Er1 103.72(8) . . ?
Er1 O7 Er1 105.62(11) . 6 ?
Er1 O7 Er1 105.62(11) . 5 ?
Er1 O7 Er1 105.62(11) 6 5 ?
C8 N1 C12 116.7(4) . . ?
O1 C1 O2 125.4(5) . . ?
O1 C1 C2 119.3(5) . . ?
O2 C1 C2 115.3(5) . . ?
C3 C2 C7 117.8(4) . . ?
C3 C2 C1 121.8(5) . . ?
C7 C2 C1 120.5(5) . . ?
C6 C7 C2 120.4(5) . . ?
C4 C3 C2 123.2(5) . . ?
C5 C6 C7 121.8(5) . . ?
C3 C4 C5 118.7(5) . . ?
C6 C5 C4 117.9(4) . . ?
C6 C5 C9 121.2(5) . . ?
C4 C5 C9 120.9(5) . . ?
N1 C8 C9 124.7(4) . . ?
C10 C9 C8 116.7(4) . . ?
C10 C9 C5 120.7(4) . . ?
C8 C9 C5 122.6(4) . . ?
C9 C10 C11 120.7(4) . . ?
C12 C11 C10 116.5(4) . . ?
C12 C11 C17 121.9(4) . . ?
C10 C11 C17 121.4(4) . . ?
N1 C12 C11 124.6(4) . . ?
C18 C17 C16 116.7(4) . . ?
C18 C17 C11 122.1(4) . . ?
C16 C17 C11 121.3(4) . . ?
C19 C18 C17 121.4(5) . . ?
C15 C16 C17 122.4(5) . . ?
C18 C19 C14 120.7(5) . . ?
C14 C15 C16 120.4(5) . . ?
C15 C14 C19 118.4(4) . . ?
C15 C14 C13 122.8(4) . . ?
C19 C14 C13 118.8(4) . . ?
O3 C13 O4 125.5(4) . . ?
O3 C13 C14 117.6(4) . . ?
O4 C13 C14 116.9(4) . . ?

_refine_diff_density_max         1.658
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.078

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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 
# 
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# Please retain this information to preserve the provenance of 
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data_2
_database_code_depnum_ccdc_archive 'CCDC 1417630'
_audit_update_record             
;
2015-11-18 deposited with the CCDC.
2015-12-18 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            'C93 H149 N17 O48 Yb4'
_chemical_formula_weight         2965.44

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'
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'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'

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

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

_cell_length_a                   29.311(5)
_cell_length_b                   29.311(5)
_cell_length_c                   29.311(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     25182(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7228
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      23.78

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_F_000             11920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    3.032
_shelx_estimated_absorpt_T_min   0.506
_shelx_estimated_absorpt_T_max   0.597
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_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            86295
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.203
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7833
_reflns_number_gt                5068
_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.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.003 -0.013 -0.005 15605 5146 ' '
_platon_squeeze_details          
;
In order to subtract the contribution from the disordered solvent molecules,
the SQUEEZE command was applied.
SQUEEZE removed disordered solvent molecules per formula unit. This valueis calculated based upon volume/count_electrons analysis.
See ref. P. van der Sluis and A. L. Spek, Acta Crystallogr., 1990, A46, 194.

CHEMW03_ALERT_2_A ALERT: The ratio of given/expected molecular weight as
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for two disordered nitrate ions, twelve disordered DMF and ten disordered H2O omitted by SQUEEZE.
;


_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    diamond
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0602P)²+461.7501P] 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         7833
_refine_ls_number_parameters     253
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.0862
_refine_ls_wR_factor_ref         0.2120
_refine_ls_wR_factor_gt          0.1918
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.14433(2) 0.24537(2) 1.18293(2) 0.04954(8) Uani 1 1 d . . . . .
Yb2 Yb -0.25046(2) 0.25046(2) 0.75046(2) 0.04606(11) Uani 1 3 d S T P . .
N1 N 0.1076(2) 0.2498(4) 0.8132(2) 0.104(3) Uani 1 1 d . . . . .
O1 O -0.1806(2) 0.2501(4) 0.7802(3) 0.169(4) Uani 1 1 d . . . . .
O2 O -0.18479(19) 0.2925(2) 0.8426(2) 0.087(2) Uani 1 1 d . . . . .
O3 O 0.14366(19) 0.2439(2) 1.10805(18) 0.0683(17) Uani 1 1 d . . . . .
O4 O 0.20330(18) 0.2033(2) 1.08211(18) 0.0741(19) Uani 1 1 d . . . . .
O5 O -0.2029(2) 0.2029(2) 0.7029(2) 0.132(4) Uani 1 3 d S TU P . .
H5A H -0.1943 0.1795 0.7178 0.199 Uiso 0.3333 1 d R U P . .
H5B H -0.2180 0.1941 0.6795 0.199 Uiso 0.3333 1 d R U P . .
O6 O 0.22326(14) 0.24900(13) 1.17526(14) 0.0401(11) Uani 1 1 d . . . . .
H6L H 0.2321 0.2721 1.1600 0.048 Uiso 1 1 d R U . . .
O7 O 0.17257(14) 0.17257(14) 1.17257(14) 0.051(2) Uani 1 3 d S T P . .
H7L H 0.1558 0.1559 1.1559 0.061 Uiso 1 3 d R U P . .
O8 O 0.0775(2) 0.2883(2) 1.1673(3) 0.122(3) Uani 1 1 d . . . . .
H8M H 0.0848 0.3122 1.1528 0.183 Uiso 1 1 d R U . . .
H8N H 0.0595 0.2723 1.1512 0.183 Uiso 1 1 d R U . . .
C1 C -0.1593(3) 0.2628(3) 0.8162(2) 0.060(2) Uani 1 1 d . U . . .
C2 C -0.1128(3) 0.2664(4) 0.8195(3) 0.095(4) Uani 1 1 d . . . . .
C3 C -0.0859(3) 0.2426(4) 0.7880(3) 0.100(4) Uani 1 1 d . . . . .
H3 H -0.0992 0.2311 0.7616 0.120 Uiso 1 1 calc R U . . .
C4 C -0.0382(3) 0.2358(5) 0.7958(3) 0.117(5) Uani 1 1 d . . . . .
H4 H -0.0209 0.2189 0.7753 0.141 Uiso 1 1 calc R U . . .
C5 C -0.0186(3) 0.2542(4) 0.8333(2) 0.076(3) Uani 1 1 d . . . . .
C6 C -0.0459(3) 0.2769(5) 0.8640(3) 0.115(5) Uani 1 1 d . . . . .
H6 H -0.0328 0.2885 0.8904 0.138 Uiso 1 1 calc R U . . .
C7 C -0.0924(3) 0.2831(4) 0.8570(3) 0.112(4) Uani 1 1 d . . . . .
H7 H -0.1095 0.2990 0.8785 0.134 Uiso 1 1 calc R U . . .
C8 C 0.0622(3) 0.2529(4) 0.8092(3) 0.091(3) Uani 1 1 d . . . . .
H8 H 0.0508 0.2580 0.7800 0.109 Uiso 1 1 calc R U . . .
C9 C 0.0303(3) 0.2494(4) 0.8442(3) 0.088(3) Uani 1 1 d . . . . .
C10 C 0.0478(3) 0.2450(4) 0.8873(3) 0.096(4) Uani 1 1 d . . . . .
H10 H 0.0282 0.2443 0.9122 0.115 Uiso 1 1 calc R U . . .
C11 C 0.0939(2) 0.2417(4) 0.8943(3) 0.080(3) Uani 1 1 d . . . . .
C12 C 0.1228(3) 0.2446(4) 0.8575(3) 0.106(4) Uani 1 1 d . . . . .
H12 H 0.1540 0.2428 0.8627 0.128 Uiso 1 1 calc R U . . .
C13 C 0.1664(3) 0.2243(4) 1.0781(3) 0.075(3) Uani 1 1 d . . . . .
C14 C 0.1487(3) 0.2282(4) 1.0292(3) 0.088(3) Uani 1 1 d . . . . .
C15 C 0.1720(3) 0.2105(5) 0.9913(3) 0.106(4) Uani 1 1 d . . . . .
H15 H 0.1999 0.1959 0.9955 0.128 Uiso 1 1 calc R U . . .
C16 C 0.1544(3) 0.2146(5) 0.9484(3) 0.120(5) Uani 1 1 d . . . . .
H16 H 0.1704 0.2025 0.9238 0.144 Uiso 1 1 calc R U . . .
C17 C 0.1136(3) 0.2363(4) 0.9408(3) 0.092(4) Uani 1 1 d . . . . .
C18 C 0.0905(4) 0.2551(5) 0.9766(4) 0.115(4) Uani 1 1 d . . . . .
H18 H 0.0641 0.2720 0.9717 0.138 Uiso 1 1 calc R U . . .
C19 C 0.1076(3) 0.2485(5) 1.0212(3) 0.113(5) Uani 1 1 d . . . . .
H19 H 0.0902 0.2582 1.0459 0.135 Uiso 1 1 calc R 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
Yb1 O3 2.195(5) . ?
Yb1 O2 2.203(6) 11_656 ?
Yb1 O6 2.234(4) 5_456 ?
Yb1 O4 2.282(5) 5_456 ?
Yb1 O7 2.309(3) . ?
Yb1 O6 2.327(4) . ?
Yb1 O8 2.372(7) . ?
Yb1 Yb2 3.6519(8) 3_557 ?
Yb1 Yb1 3.6607(8) 6_546 ?
Yb1 Yb1 3.6608(8) 5_456 ?
Yb2 O1 2.226(7) 7 ?
Yb2 O1 2.226(7) 8_545 ?
Yb2 O1 2.226(7) . ?
Yb2 O6 2.310(4) 12_466 ?
Yb2 O6 2.310(4) 9_356 ?
Yb2 O6 2.310(4) 3_457 ?
Yb2 O5 2.413(11) . ?
Yb2 Yb1 3.6521(8) 12_466 ?
Yb2 Yb1 3.6521(8) 9_356 ?
Yb2 Yb1 3.6521(8) 3_457 ?
N1 C8 1.339(11) . ?
N1 C12 1.381(12) . ?
O1 C1 1.282(11) . ?
O2 C1 1.385(10) . ?
O2 Yb1 2.203(6) 12_466 ?
O3 C13 1.243(10) . ?
O4 C13 1.250(10) . ?
O4 Yb1 2.281(5) 6_546 ?
O6 Yb1 2.234(4) 6_546 ?
O6 Yb2 2.309(4) 3_557 ?
O7 Yb1 2.309(3) 5_456 ?
O7 Yb1 2.309(3) 6_546 ?
C1 C2 1.368(11) . ?
C2 C7 1.345(14) . ?
C2 C3 1.402(14) . ?
C3 C4 1.429(13) . ?
C4 C5 1.353(13) . ?
C5 C6 1.377(13) . ?
C5 C9 1.474(12) . ?
C6 C7 1.388(13) . ?
C8 C9 1.393(12) . ?
C9 C10 1.369(13) . ?
C10 C11 1.369(11) . ?
C11 C12 1.373(12) . ?
C11 C17 1.491(12) . ?
C13 C14 1.529(12) . ?
C14 C19 1.363(13) . ?
C14 C15 1.404(14) . ?
C15 C16 1.364(13) . ?
C16 C17 1.372(14) . ?
C17 C18 1.365(14) . ?
C18 C19 1.413(14) . ?

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
O3 Yb1 O2 110.3(2) . 11_656 ?
O3 Yb1 O6 149.80(18) . 5_456 ?
O2 Yb1 O6 85.2(2) 11_656 5_456 ?
O3 Yb1 O4 104.1(2) . 5_456 ?
O2 Yb1 O4 123.7(2) 11_656 5_456 ?
O6 Yb1 O4 86.58(19) 5_456 5_456 ?
O3 Yb1 O7 81.55(18) . . ?
O2 Yb1 O7 147.1(2) 11_656 . ?
O6 Yb1 O7 72.57(17) 5_456 . ?
O4 Yb1 O7 79.72(17) 5_456 . ?
O3 Yb1 O6 85.02(18) . . ?
O2 Yb1 O6 79.44(19) 11_656 . ?
O6 Yb1 O6 72.2(2) 5_456 . ?
O4 Yb1 O6 147.66(17) 5_456 . ?
O7 Yb1 O6 70.91(16) . . ?
O3 Yb1 O8 79.1(3) . . ?
O2 Yb1 O8 73.4(2) 11_656 . ?
O6 Yb1 O8 131.0(2) 5_456 . ?
O4 Yb1 O8 71.1(2) 5_456 . ?
O7 Yb1 O8 139.5(2) . . ?
O6 Yb1 O8 141.1(2) . . ?
O3 Yb1 Yb2 122.87(14) . 3_557 ?
O2 Yb1 Yb2 69.38(16) 11_656 3_557 ?
O6 Yb1 Yb2 37.22(11) 5_456 3_557 ?
O4 Yb1 Yb2 123.57(16) 5_456 3_557 ?
O7 Yb1 Yb2 78.37(17) . 3_557 ?
O6 Yb1 Yb2 37.86(10) . 3_557 ?
O8 Yb1 Yb2 141.50(19) . 3_557 ?
O3 Yb1 Yb1 71.83(15) . 6_546 ?
O2 Yb1 Yb1 115.16(16) 11_656 6_546 ?
O6 Yb1 Yb1 78.15(11) 5_456 6_546 ?
O4 Yb1 Yb1 117.23(14) 5_456 6_546 ?
O7 Yb1 Yb1 37.55(10) . 6_546 ?
O6 Yb1 Yb1 35.77(10) . 6_546 ?
O8 Yb1 Yb1 150.9(2) . 6_546 ?
Yb2 Yb1 Yb1 59.921(6) 3_557 6_546 ?
O3 Yb1 Yb1 119.09(15) . 5_456 ?
O2 Yb1 Yb1 122.33(17) 11_656 5_456 ?
O6 Yb1 Yb1 37.50(11) 5_456 5_456 ?
O4 Yb1 Yb1 71.26(14) 5_456 5_456 ?
O7 Yb1 Yb1 37.55(10) . 5_456 ?
O6 Yb1 Yb1 77.17(10) . 5_456 ?
O8 Yb1 Yb1 141.28(19) . 5_456 ?
Yb2 Yb1 Yb1 59.921(6) 3_557 5_456 ?
Yb1 Yb1 Yb1 60.0 6_546 5_456 ?
O1 Yb2 O1 111.0(2) 7 8_545 ?
O1 Yb2 O1 111.0(2) 7 . ?
O1 Yb2 O1 111.0(2) 8_545 . ?
O1 Yb2 O6 150.0(3) 7 12_466 ?
O1 Yb2 O6 86.4(3) 8_545 12_466 ?
O1 Yb2 O6 83.1(3) . 12_466 ?
O1 Yb2 O6 86.4(3) 7 9_356 ?
O1 Yb2 O6 83.1(3) 8_545 9_356 ?
O1 Yb2 O6 150.0(3) . 9_356 ?
O6 Yb2 O6 71.14(16) 12_466 9_356 ?
O1 Yb2 O6 83.1(3) 7 3_457 ?
O1 Yb2 O6 150.0(3) 8_545 3_457 ?
O1 Yb2 O6 86.4(3) . 3_457 ?
O6 Yb2 O6 71.14(16) 12_466 3_457 ?
O6 Yb2 O6 71.14(16) 9_356 3_457 ?
O1 Yb2 O5 72.1(2) 7 . ?
O1 Yb2 O5 72.1(2) 8_545 . ?
O1 Yb2 O5 72.1(2) . . ?
O6 Yb2 O5 137.80(10) 12_466 . ?
O6 Yb2 O5 137.80(10) 9_356 . ?
O6 Yb2 O5 137.80(10) 3_457 . ?
O1 Yb2 Yb1 118.9(3) 7 12_466 ?
O1 Yb2 Yb1 124.6(2) 8_545 12_466 ?
O1 Yb2 Yb1 72.7(2) . 12_466 ?
O6 Yb2 Yb1 38.20(10) 12_466 12_466 ?
O6 Yb2 Yb1 77.54(10) 9_356 12_466 ?
O6 Yb2 Yb1 35.81(10) 3_457 12_466 ?
O5 Yb2 Yb1 144.639(7) . 12_466 ?
O1 Yb2 Yb1 124.6(2) 7 9_356 ?
O1 Yb2 Yb1 72.7(2) 8_545 9_356 ?
O1 Yb2 Yb1 118.9(3) . 9_356 ?
O6 Yb2 Yb1 35.81(10) 12_466 9_356 ?
O6 Yb2 Yb1 38.20(10) 9_356 9_356 ?
O6 Yb2 Yb1 77.54(10) 3_457 9_356 ?
O5 Yb2 Yb1 144.639(7) . 9_356 ?
Yb1 Yb2 Yb1 60.158(11) 12_466 9_356 ?
O1 Yb2 Yb1 72.7(2) 7 3_457 ?
O1 Yb2 Yb1 118.9(3) 8_545 3_457 ?
O1 Yb2 Yb1 124.6(2) . 3_457 ?
O6 Yb2 Yb1 77.54(10) 12_466 3_457 ?
O6 Yb2 Yb1 35.81(10) 9_356 3_457 ?
O6 Yb2 Yb1 38.20(11) 3_457 3_457 ?
O5 Yb2 Yb1 144.639(7) . 3_457 ?
Yb1 Yb2 Yb1 60.158(11) 12_466 3_457 ?
Yb1 Yb2 Yb1 60.158(11) 9_356 3_457 ?
C8 N1 C12 114.1(7) . . ?
C1 O1 Yb2 140.4(6) . . ?
C1 O2 Yb1 143.6(5) . 12_466 ?
C13 O3 Yb1 135.4(5) . . ?
C13 O4 Yb1 132.3(5) . 6_546 ?
Yb1 O6 Yb2 106.97(16) 6_546 3_557 ?
Yb1 O6 Yb1 106.74(16) 6_546 . ?
Yb2 O6 Yb1 103.94(16) 3_557 . ?
Yb1 O7 Yb1 104.90(19) . 5_456 ?
Yb1 O7 Yb1 104.89(19) . 6_546 ?
Yb1 O7 Yb1 104.90(19) 5_456 6_546 ?
O1 C1 C2 124.5(8) . . ?
O1 C1 O2 112.3(7) . . ?
C2 C1 O2 116.7(7) . . ?
C7 C2 C1 122.0(8) . . ?
C7 C2 C3 117.9(8) . . ?
C1 C2 C3 118.4(9) . . ?
C2 C3 C4 121.0(9) . . ?
C5 C4 C3 119.4(10) . . ?
C4 C5 C6 118.4(8) . . ?
C4 C5 C9 123.5(8) . . ?
C6 C5 C9 118.1(8) . . ?
C5 C6 C7 122.5(9) . . ?
C2 C7 C6 120.7(10) . . ?
N1 C8 C9 126.8(8) . . ?
C10 C9 C8 115.7(8) . . ?
C10 C9 C5 125.0(8) . . ?
C8 C9 C5 119.1(7) . . ?
C9 C10 C11 121.0(8) . . ?
C12 C11 C10 119.1(8) . . ?
C12 C11 C17 119.1(7) . . ?
C10 C11 C17 121.8(7) . . ?
C11 C12 N1 123.1(8) . . ?
O3 C13 O4 128.5(8) . . ?
O3 C13 C14 116.5(8) . . ?
O4 C13 C14 114.9(8) . . ?
C19 C14 C15 117.2(8) . . ?
C19 C14 C13 119.6(8) . . ?
C15 C14 C13 123.2(8) . . ?
C16 C15 C14 120.7(10) . . ?
C15 C16 C17 121.4(9) . . ?
C18 C17 C16 119.6(9) . . ?
C18 C17 C11 117.9(9) . . ?
C16 C17 C11 122.4(8) . . ?
C17 C18 C19 118.7(10) . . ?
C14 C19 C18 122.1(9) . . ?

_refine_diff_density_max         2.148
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.160

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1417631'
_audit_update_record             
;
2015-11-18 deposited with the CCDC.
2015-12-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C93 H157 Lu4 N17 O52'
_chemical_formula_weight         3045.23

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'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'

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

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

_cell_length_a                   29.394(5)
_cell_length_b                   29.394(5)
_cell_length_c                   29.394(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     25397(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9943
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      26.12

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_F_000             12272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    3.175
_shelx_estimated_absorpt_T_min   0.504
_shelx_estimated_absorpt_T_max   0.584
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_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            55591
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.200
_diffrn_reflns_theta_max         25.509
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7901
_reflns_number_gt                6604
_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.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.021 -0.109 -0.015 17161.0 5474
_platon_squeeze_details          
;
In order to subtract the contribution from the disordered solvent molecules,
the SQUEEZE command was applied.
SQUEEZE removed disordered solvent molecules per formula unit. This valueis calculated based upon volume/count_electrons analysis.
See ref. P. van der Sluis and A. L. Spek, Acta Crystallogr., 1990, A46, 194.

CHEMW03_ALERT_2_A ALERT: The ratio of given/expected molecular weight as
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for two disordered nitrate ions, twelve disordered DMF and fourteen disordered H2O omitted by SQUEEZE.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    diamond
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0602P)²+4.8948P] 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         7901
_refine_ls_number_parameters     254
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0998
_refine_ls_wR_factor_gt          0.0979
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.005
_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
Lu1 Lu 0.81877(2) 0.14138(2) 0.74316(2) 0.03653(8) Uani 1 1 d . . . . .
Lu2 Lu 0.75237(2) 0.24763(2) 0.74763(2) 0.03578(10) Uani 1 3 d S T P . .
O1 O 0.7529(2) 0.21812(19) 0.81799(14) 0.136(2) Uani 1 1 d . . . . .
O2 O 0.79815(16) 0.15652(13) 0.81557(12) 0.0892(13) Uani 1 1 d . . . . .
O3 O 0.75877(12) 0.10579(11) 0.64102(11) 0.0614(9) Uani 1 1 d . . . . .
O4 O 0.79884(13) 0.08036(10) 0.69858(11) 0.0635(9) Uani 1 1 d . . . . .
O5 O 0.70540(13) 0.29460(13) 0.79460(13) 0.142(4) Uani 1 3 d S T P . .
H5A H 0.7225 0.3043 0.8203 0.213 Uiso 0.3333 1 d R U P . .
H5B H 0.6794 0.2772 0.8043 0.213 Uiso 0.3333 1 d R U P . .
O6 O 0.75247(7) 0.17310(8) 0.72100(8) 0.0274(5) Uani 1 1 d . . . . .
H6A H 0.7302 0.1585 0.7323 0.033 Uiso 1 1 d R U . . .
O7 O 0.82927(9) 0.17073(9) 0.67073(9) 0.0369(10) Uani 1 3 d DS T P . .
H7A H 0.84598(17) 0.1540(3) 0.6540(3) 0.044 Uiso 1 3 d DR U P . .
O8 O 0.83520(19) 0.07406(12) 0.78615(13) 0.1136(18) Uani 1 1 d . . . . .
H8A H 0.8519 0.0532 0.7673 0.170 Uiso 1 1 d R U . . .
H8B H 0.8074 0.0600 0.7959 0.170 Uiso 1 1 d R U . . .
C1 C 0.7736(3) 0.1851(2) 0.83637(18) 0.0813(18) Uani 1 1 d . . . . .
C2 C 0.7699(2) 0.17890(17) 0.88586(17) 0.0711(15) Uani 1 1 d . . . . .
C3 C 0.7503(2) 0.2111(2) 0.91359(19) 0.093(2) Uani 1 1 d . . . . .
H3 H 0.7406 0.2382 0.9006 0.111 Uiso 1 1 calc R U . . .
C4 C 0.7444(2) 0.2052(2) 0.95905(18) 0.099(2) Uani 1 1 d . . . . .
H4 H 0.7299 0.2273 0.9764 0.119 Uiso 1 1 calc R U . . .
C5 C 0.7606(2) 0.16459(17) 0.97950(16) 0.0753(18) Uani 1 1 d . . . . .
C6 C 0.7813(2) 0.13313(17) 0.95200(16) 0.0815(19) Uani 1 1 d . . . . .
H6 H 0.7921 0.1063 0.9648 0.098 Uiso 1 1 calc R U . . .
C7 C 0.7867(2) 0.14008(17) 0.90623(17) 0.0819(19) Uani 1 1 d . . . . .
H7 H 0.8018 0.1185 0.8887 0.098 Uiso 1 1 calc R U . . .
C8 C 0.7586(2) 0.19114(17) 1.06098(17) 0.0778(19) Uani 1 1 d . . . . .
H8 H 0.7632 0.2206 1.0504 0.093 Uiso 1 1 calc R U . . .
C9 C 0.7551(2) 0.15666(15) 1.02886(15) 0.0677(16) Uani 1 1 d . . . . .
C10 C 0.74760(19) 0.11377(16) 1.04513(16) 0.0720(17) Uani 1 1 d . . . . .
H10 H 0.7449 0.0896 1.0249 0.086 Uiso 1 1 calc R U . . .
C11 C 0.7440(2) 0.10590(16) 1.09192(15) 0.0696(16) Uani 1 1 d . . . . .
C12 C 0.7496(2) 0.14272(17) 1.11964(16) 0.0796(19) Uani 1 1 d . . . . .
H12 H 0.7489 0.1379 1.1509 0.096 Uiso 1 1 calc R U . . .
C13 C 0.77718(19) 0.07527(15) 0.66289(16) 0.0569(12) Uani 1 1 d . . . . .
C14 C 0.7274(2) -0.02740(15) 1.14511(16) 0.0674(15) Uani 1 1 d . . . . .
C15 C 0.7109(2) 0.00922(16) 1.16758(17) 0.086(2) Uani 1 1 d . . . . .
H15 H 0.6955 0.0052 1.1949 0.103 Uiso 1 1 calc R U . . .
C16 C 0.7169(3) 0.05192(17) 1.15049(18) 0.096(2) Uani 1 1 d . . . . .
H16 H 0.7054 0.0766 1.1666 0.115 Uiso 1 1 calc R U . . .
C17 C 0.7393(2) 0.05974(15) 1.11012(16) 0.0709(16) Uani 1 1 d . . . . .
C18 C 0.7566(2) 0.02242(19) 1.0881(2) 0.093(2) Uani 1 1 d . . . . .
H18 H 0.7731 0.0265 1.0615 0.112 Uiso 1 1 calc R U . . .
C19 C 0.7502(2) -0.02024(17) 1.1045(2) 0.089(2) Uani 1 1 d . . . . .
H19 H 0.7613 -0.0450 1.0882 0.107 Uiso 1 1 calc R U . . .
N1 N 0.75611(18) 0.18531(13) 1.10497(15) 0.0768(15) 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
Lu1 O3 2.218(3) 8_646 ?
Lu1 O6 2.256(2) . ?
Lu1 O2 2.257(4) . ?
Lu1 O4 2.297(3) . ?
Lu1 O7 2.3176(18) . ?
Lu1 O6 2.356(2) 8_646 ?
Lu1 O8 2.397(3) . ?
Lu1 Lu2 3.6852(7) . ?
Lu1 Lu1 3.6925(7) 8_646 ?
Lu1 Lu1 3.6926(7) 7_665 ?
Lu2 O1 2.243(4) . ?
Lu2 O1 2.243(4) 7_665 ?
Lu2 O1 2.243(4) 8_646 ?
Lu2 O6 2.327(2) . ?
Lu2 O6 2.327(2) 8_646 ?
Lu2 O6 2.327(2) 7_665 ?
Lu2 O5 2.391(7) . ?
Lu2 Lu1 3.6852(7) 7_665 ?
Lu2 Lu1 3.6852(7) 8_646 ?
O1 C1 1.267(7) . ?
O2 C1 1.265(6) . ?
O3 C13 1.229(5) . ?
O3 Lu1 2.218(3) 7_665 ?
O4 C13 1.236(5) . ?
O5 H5A 0.9503 . ?
O5 H5B 0.9620 . ?
O6 Lu1 2.356(2) 7_665 ?
O6 H6A 0.8500 . ?
O7 Lu1 2.3176(17) 7_665 ?
O7 Lu1 2.3176(18) 8_646 ?
O7 H7A 0.850(10) . ?
O8 H8A 0.9600 . ?
O8 H8B 0.9600 . ?
C1 C2 1.470(7) . ?
C2 C3 1.375(7) . ?
C2 C7 1.380(7) . ?
C3 C4 1.359(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.418(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.371(7) . ?
C5 C9 1.479(6) . ?
C6 C7 1.370(7) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 N1 1.307(6) . ?
C8 C9 1.389(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.366(6) . ?
C10 C11 1.399(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.365(7) . ?
C11 C17 1.465(6) . ?
C12 N1 1.337(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.507(6) 2_654 ?
C14 C15 1.352(7) . ?
C14 C19 1.387(7) . ?
C14 C13 1.507(6) 2_655 ?
C15 C16 1.363(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.376(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.371(7) . ?
C18 C19 1.356(7) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?

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
O3 Lu1 O6 149.09(10) 8_646 . ?
O3 Lu1 O2 107.06(15) 8_646 . ?
O6 Lu1 O2 87.64(13) . . ?
O3 Lu1 O4 103.69(13) 8_646 . ?
O6 Lu1 O4 86.42(11) . . ?
O2 Lu1 O4 128.55(14) . . ?
O3 Lu1 O7 81.10(10) 8_646 . ?
O6 Lu1 O7 72.30(10) . . ?
O2 Lu1 O7 145.94(14) . . ?
O4 Lu1 O7 78.50(10) . . ?
O3 Lu1 O6 84.53(10) 8_646 8_646 ?
O6 Lu1 O6 72.12(11) . 8_646 ?
O2 Lu1 O6 77.30(11) . 8_646 ?
O4 Lu1 O6 146.36(9) . 8_646 ?
O7 Lu1 O6 70.54(9) . 8_646 ?
O3 Lu1 O8 78.94(16) 8_646 . ?
O6 Lu1 O8 131.85(15) . . ?
O2 Lu1 O8 73.72(14) . . ?
O4 Lu1 O8 72.99(13) . . ?
O7 Lu1 O8 139.88(14) . . ?
O6 Lu1 O8 140.43(11) 8_646 . ?
O3 Lu1 Lu2 122.31(8) 8_646 . ?
O6 Lu1 Lu2 37.13(6) . . ?
O2 Lu1 Lu2 69.95(10) . . ?
O4 Lu1 Lu2 123.16(9) . . ?
O7 Lu1 Lu2 77.75(10) . . ?
O6 Lu1 Lu2 37.81(6) 8_646 . ?
O8 Lu1 Lu2 141.95(12) . . ?
O3 Lu1 Lu1 70.99(8) 8_646 8_646 ?
O6 Lu1 Lu1 78.28(6) . 8_646 ?
O2 Lu1 Lu1 112.98(10) . 8_646 ?
O4 Lu1 Lu1 115.61(8) . 8_646 ?
O7 Lu1 Lu1 37.19(6) . 8_646 ?
O6 Lu1 Lu1 35.90(5) 8_646 8_646 ?
O8 Lu1 Lu1 149.86(14) . 8_646 ?
Lu2 Lu1 Lu1 59.934(3) . 8_646 ?
O3 Lu1 Lu1 118.27(8) 8_646 7_665 ?
O6 Lu1 Lu1 37.75(6) . 7_665 ?
O2 Lu1 Lu1 124.68(11) . 7_665 ?
O4 Lu1 Lu1 70.11(8) . 7_665 ?
O7 Lu1 Lu1 37.19(6) . 7_665 ?
O6 Lu1 Lu1 77.24(5) 8_646 7_665 ?
O8 Lu1 Lu1 142.02(10) . 7_665 ?
Lu2 Lu1 Lu1 59.933(3) . 7_665 ?
Lu1 Lu1 Lu1 60.0 8_646 7_665 ?
O1 Lu2 O1 111.11(10) . 7_665 ?
O1 Lu2 O1 111.11(10) . 8_646 ?
O1 Lu2 O1 111.11(10) 7_665 8_646 ?
O1 Lu2 O6 86.91(16) . . ?
O1 Lu2 O6 82.23(13) 7_665 . ?
O1 Lu2 O6 149.95(12) 8_646 . ?
O1 Lu2 O6 82.23(13) . 8_646 ?
O1 Lu2 O6 149.96(12) 7_665 8_646 ?
O1 Lu2 O6 86.91(16) 8_646 8_646 ?
O6 Lu2 O6 71.43(8) . 8_646 ?
O1 Lu2 O6 149.95(12) . 7_665 ?
O1 Lu2 O6 86.91(16) 7_665 7_665 ?
O1 Lu2 O6 82.23(13) 8_646 7_665 ?
O6 Lu2 O6 71.42(8) . 7_665 ?
O6 Lu2 O6 71.43(8) 8_646 7_665 ?
O1 Lu2 O5 72.23(11) . . ?
O1 Lu2 O5 72.23(11) 7_665 . ?
O1 Lu2 O5 72.23(11) 8_646 . ?
O6 Lu2 O5 137.62(5) . . ?
O6 Lu2 O5 137.62(5) 8_646 . ?
O6 Lu2 O5 137.62(5) 7_665 . ?
O1 Lu2 Lu1 125.20(15) . 7_665 ?
O1 Lu2 Lu1 72.64(11) 7_665 7_665 ?
O1 Lu2 Lu1 117.97(13) 8_646 7_665 ?
O6 Lu2 Lu1 38.37(6) . 7_665 ?
O6 Lu2 Lu1 77.71(5) 8_646 7_665 ?
O6 Lu2 Lu1 35.83(5) 7_665 7_665 ?
O5 Lu2 Lu1 144.655(4) . 7_665 ?
O1 Lu2 Lu1 117.97(13) . 8_646 ?
O1 Lu2 Lu1 125.20(14) 7_665 8_646 ?
O1 Lu2 Lu1 72.64(11) 8_646 8_646 ?
O6 Lu2 Lu1 77.70(5) . 8_646 ?
O6 Lu2 Lu1 35.83(5) 8_646 8_646 ?
O6 Lu2 Lu1 38.38(6) 7_665 8_646 ?
O5 Lu2 Lu1 144.655(4) . 8_646 ?
Lu1 Lu2 Lu1 60.132(6) 7_665 8_646 ?
O1 Lu2 Lu1 72.64(11) . . ?
O1 Lu2 Lu1 117.97(13) 7_665 . ?
O1 Lu2 Lu1 125.20(15) 8_646 . ?
O6 Lu2 Lu1 35.83(5) . . ?
O6 Lu2 Lu1 38.38(6) 8_646 . ?
O6 Lu2 Lu1 77.71(5) 7_665 . ?
O5 Lu2 Lu1 144.655(4) . . ?
Lu1 Lu2 Lu1 60.134(6) 7_665 . ?
Lu1 Lu2 Lu1 60.131(6) 8_646 . ?
C1 O1 Lu2 133.8(4) . . ?
C1 O2 Lu1 137.7(4) . . ?
C13 O3 Lu1 137.6(3) . 7_665 ?
C13 O4 Lu1 135.2(3) . . ?
Lu2 O5 H5A 109.0 . . ?
Lu2 O5 H5B 108.8 . . ?
H5A O5 H5B 110.1 . . ?
Lu1 O6 Lu2 107.04(9) . . ?
Lu1 O6 Lu1 106.36(9) . 7_665 ?
Lu2 O6 Lu1 103.82(9) . 7_665 ?
Lu1 O6 H6A 110.1 . . ?
Lu2 O6 H6A 110.1 . . ?
Lu1 O6 H6A 118.7 7_665 . ?
Lu1 O7 Lu1 105.62(11) . 7_665 ?
Lu1 O7 Lu1 105.62(11) . 8_646 ?
Lu1 O7 Lu1 105.62(11) 7_665 8_646 ?
Lu1 O7 H7A 113.1 . . ?
Lu1 O7 H7A 113.1 7_665 . ?
Lu1 O7 H7A 113.1 8_646 . ?
Lu1 O8 H8A 109.0 . . ?
Lu1 O8 H8B 110.0 . . ?
H8A O8 H8B 109.5 . . ?
O2 C1 O1 125.3(5) . . ?
O2 C1 C2 116.0(5) . . ?
O1 C1 C2 118.8(5) . . ?
C3 C2 C7 117.5(5) . . ?
C3 C2 C1 122.2(5) . . ?
C7 C2 C1 120.4(5) . . ?
C4 C3 C2 123.3(5) . . ?
C4 C3 H3 118.4 . . ?
C2 C3 H3 118.4 . . ?
C3 C4 C5 118.8(5) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 117.8(5) . . ?
C6 C5 C9 121.4(5) . . ?
C4 C5 C9 120.8(5) . . ?
C7 C6 C5 122.0(5) . . ?
C7 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C6 C7 C2 120.5(5) . . ?
C6 C7 H7 119.7 . . ?
C2 C7 H7 119.7 . . ?
N1 C8 C9 124.9(4) . . ?
N1 C8 H8 117.5 . . ?
C9 C8 H8 117.5 . . ?
C10 C9 C8 116.6(4) . . ?
C10 C9 C5 120.5(4) . . ?
C8 C9 C5 122.9(4) . . ?
C9 C10 C11 120.6(5) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C12 C11 C10 116.5(4) . . ?
C12 C11 C17 121.9(4) . . ?
C10 C11 C17 121.3(4) . . ?
N1 C12 C11 124.5(4) . . ?
N1 C12 H12 117.7 . . ?
C11 C12 H12 117.7 . . ?
O3 C13 O4 125.6(4) . . ?
O3 C13 C14 117.5(4) . 2_654 ?
O4 C13 C14 116.9(4) . 2_654 ?
C15 C14 C19 118.2(4) . . ?
C15 C14 C13 122.8(4) . 2_655 ?
C19 C14 C13 118.9(5) . 2_655 ?
C14 C15 C16 120.5(5) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C17 122.2(5) . . ?
C15 C16 H16 118.9 . . ?
C17 C16 H16 118.9 . . ?
C18 C17 C16 116.8(4) . . ?
C18 C17 C11 122.2(4) . . ?
C16 C17 C11 121.0(5) . . ?
C19 C18 C17 121.5(5) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C18 C19 C14 120.8(5) . . ?
C18 C19 H19 119.6 . . ?
C14 C19 H19 119.6 . . ?
C8 N1 C12 116.7(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Lu1 O2 C1 O1 -2.9(13) . . . . ?
Lu1 O2 C1 C2 177.7(4) . . . . ?
Lu2 O1 C1 O2 -7.1(13) . . . . ?
Lu2 O1 C1 C2 172.3(5) . . . . ?
O2 C1 C2 C3 169.9(7) . . . . ?
O1 C1 C2 C3 -9.6(11) . . . . ?
O2 C1 C2 C7 -9.5(10) . . . . ?
O1 C1 C2 C7 171.0(7) . . . . ?
C7 C2 C3 C4 -4.1(11) . . . . ?
C1 C2 C3 C4 176.5(7) . . . . ?
C2 C3 C4 C5 2.4(12) . . . . ?
C3 C4 C5 C6 -0.4(10) . . . . ?
C3 C4 C5 C9 179.8(6) . . . . ?
C4 C5 C6 C7 0.3(11) . . . . ?
C9 C5 C6 C7 -179.9(6) . . . . ?
C5 C6 C7 C2 -2.0(11) . . . . ?
C3 C2 C7 C6 3.8(10) . . . . ?
C1 C2 C7 C6 -176.8(7) . . . . ?
N1 C8 C9 C10 1.1(10) . . . . ?
N1 C8 C9 C5 -176.7(6) . . . . ?
C6 C5 C9 C10 -34.2(9) . . . . ?
C4 C5 C9 C10 145.6(6) . . . . ?
C6 C5 C9 C8 143.5(7) . . . . ?
C4 C5 C9 C8 -36.7(10) . . . . ?
C8 C9 C10 C11 -0.2(9) . . . . ?
C5 C9 C10 C11 177.6(6) . . . . ?
C9 C10 C11 C12 -1.8(9) . . . . ?
C9 C10 C11 C17 -175.6(6) . . . . ?
C10 C11 C12 N1 3.2(10) . . . . ?
C17 C11 C12 N1 176.9(6) . . . . ?
Lu1 O3 C13 O4 8.9(9) 7_665 . . . ?
Lu1 O3 C13 C14 -171.8(4) 7_665 . . 2_654 ?
Lu1 O4 C13 O3 -1.0(9) . . . . ?
Lu1 O4 C13 C14 179.7(3) . . . 2_654 ?
C19 C14 C15 C16 0.0(11) . . . . ?
C13 C14 C15 C16 178.5(6) 2_655 . . . ?
C14 C15 C16 C17 0.4(12) . . . . ?
C15 C16 C17 C18 -1.7(11) . . . . ?
C15 C16 C17 C11 178.2(7) . . . . ?
C12 C11 C17 C18 -145.1(7) . . . . ?
C10 C11 C17 C18 28.4(10) . . . . ?
C12 C11 C17 C16 35.0(10) . . . . ?
C10 C11 C17 C16 -151.5(6) . . . . ?
C16 C17 C18 C19 2.8(11) . . . . ?
C11 C17 C18 C19 -177.1(7) . . . . ?
C17 C18 C19 C14 -2.6(11) . . . . ?
C15 C14 C19 C18 1.1(10) . . . . ?
C13 C14 C19 C18 -177.5(6) 2_655 . . . ?
C9 C8 N1 C12 0.1(10) . . . . ?
C11 C12 N1 C8 -2.3(10) . . . . ?

_refine_diff_density_max         1.810
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.088

_shelxl_version_number           2014/6

