# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_Complex_1
_database_code_depnum_ccdc_archive 'CCDC 1514978'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 I6 La2 N6 O14'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       'Plate '
_exptl_crystal_colour            yellow
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2262.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   14.2221(6)
_cell_length_b                   25.5903(10)
_cell_length_c                   10.3810(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.5520(11)
_cell_angle_gamma                90
_cell_volume                     3770.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    39141
_cell_measurement_theta_min      4.983
_cell_measurement_theta_max      50.074
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_F_000             2136
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.106
_exptl_absorpt_coefficient_mu    3.639
_shelx_estimated_absorpt_T_min   0.330
_shelx_estimated_absorpt_T_max   0.699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5725
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38626
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.435
_diffrn_reflns_theta_max         28.213
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9276
_reflns_number_gt                6367
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0568P)²+8.2085P] 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         9276
_refine_ls_number_parameters     459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1332
_refine_ls_wR_factor_gt          0.1160
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8137(5) 0.1011(2) 0.7255(6) 0.0681(17) Uani 1 1 d . . . . .
H1 H 0.8300 0.0661 0.7352 0.082 Uiso 1 1 calc R U . . .
C2 C 0.7499(6) 0.1139(3) 0.6284(7) 0.079(2) Uani 1 1 d . . . . .
H2 H 0.7245 0.0888 0.5716 0.094 Uiso 1 1 calc R U . . .
C3 C 0.7243(7) 0.1650(4) 0.6173(8) 0.104(3) Uani 1 1 d . . . . .
H3 H 0.6805 0.1756 0.5524 0.124 Uiso 1 1 calc R U . . .
C4 C 0.7637(6) 0.2008(3) 0.7027(8) 0.093(2) Uani 1 1 d . . . . .
H4 H 0.7442 0.2355 0.6985 0.112 Uiso 1 1 calc R U . . .
C5 C 0.8323(4) 0.1854(2) 0.7948(5) 0.0511(13) Uani 1 1 d . . . . .
C6 C 0.8841(4) 0.2236(2) 0.8804(5) 0.0500(13) Uani 1 1 d . . . . .
C7 C 0.8725(5) 0.2775(2) 0.8603(6) 0.0693(18) Uani 1 1 d . . . . .
H7 H 0.8318 0.2895 0.7934 0.083 Uiso 1 1 calc R U . . .
C8 C 0.9210(6) 0.3122(2) 0.9390(7) 0.079(2) Uani 1 1 d . . . . .
H8 H 0.9144 0.3479 0.9254 0.094 Uiso 1 1 calc R U . . .
C9 C 0.9790(5) 0.2937(2) 1.0375(7) 0.0667(17) Uani 1 1 d . . . . .
H9 H 1.0110 0.3168 1.0938 0.080 Uiso 1 1 calc R U . . .
C10 C 0.9902(4) 0.23984(18) 1.0538(5) 0.0479(12) Uani 1 1 d . . . . .
C11 C 1.0558(4) 0.21873(18) 1.1578(5) 0.0462(12) Uani 1 1 d . . . . .
C12 C 1.1077(4) 0.2510(2) 1.2435(6) 0.0598(15) Uani 1 1 d . . . . .
H12 H 1.1036 0.2871 1.2348 0.072 Uiso 1 1 calc R U . . .
C13 C 1.1646(5) 0.2297(3) 1.3400(7) 0.0733(18) Uani 1 1 d . . . . .
H13 H 1.1978 0.2510 1.3993 0.088 Uiso 1 1 calc R U . . .
C14 C 1.1723(5) 0.1764(3) 1.3484(7) 0.0748(19) Uani 1 1 d . . . . .
H14 H 1.2119 0.1610 1.4122 0.090 Uiso 1 1 calc R U . . .
C15 C 1.1210(5) 0.1465(2) 1.2617(6) 0.0667(17) Uani 1 1 d . . . . .
H15 H 1.1266 0.1104 1.2679 0.080 Uiso 1 1 calc R U . . .
C16 C 1.0741(4) 0.08960(18) 0.7763(5) 0.0478(12) Uani 1 1 d . . . . .
C17 C 1.1416(4) 0.0812(2) 0.6727(5) 0.0492(12) Uani 1 1 d . . . . .
C18 C 1.2280(5) 0.1051(2) 0.6813(6) 0.0590(15) Uani 1 1 d . . . . .
H18 H 1.2422 0.1294 0.7462 0.071 Uiso 1 1 calc R U . . .
C19 C 1.2942(5) 0.0932(3) 0.5938(7) 0.0720(18) Uani 1 1 d . . . . .
H19 H 1.3539 0.1081 0.6014 0.086 Uiso 1 1 calc R U . . .
C20 C 1.2698(6) 0.0586(3) 0.4949(7) 0.076(2) Uani 1 1 d . . . . .
C21 C 1.1829(7) 0.0361(3) 0.4828(7) 0.085(2) Uani 1 1 d . . . . .
H21 H 1.1673 0.0137 0.4143 0.102 Uiso 1 1 calc R U . . .
C22 C 1.1192(6) 0.0466(2) 0.5717(6) 0.0707(18) Uani 1 1 d . . . . .
H22 H 1.0604 0.0306 0.5651 0.085 Uiso 1 1 calc R U . . .
C23 C 0.7639(4) 0.1236(2) 1.1937(6) 0.0503(13) Uani 1 1 d . . . . .
C24 C 0.6717(4) 0.1529(2) 1.1796(6) 0.0523(13) Uani 1 1 d . . . . .
C25 C 0.6524(5) 0.1862(2) 1.0772(6) 0.0636(15) Uani 1 1 d . . . . .
H25 H 0.6958 0.1899 1.0144 0.076 Uiso 1 1 calc R U . . .
C26 C 0.5688(5) 0.2145(3) 1.0664(8) 0.0759(19) Uani 1 1 d . . . . .
H26 H 0.5556 0.2363 0.9960 0.091 Uiso 1 1 calc R U . . .
C27 C 0.5061(5) 0.2098(3) 1.1606(8) 0.077(2) Uani 1 1 d . . . . .
C28 C 0.5218(5) 0.1760(4) 1.2592(9) 0.088(2) Uani 1 1 d . . . . .
H28 H 0.4772 0.1721 1.3203 0.105 Uiso 1 1 calc R U . . .
C29 C 0.6048(5) 0.1469(3) 1.2696(7) 0.0710(17) Uani 1 1 d . . . . .
H29 H 0.6152 0.1234 1.3372 0.085 Uiso 1 1 calc R U . . .
C30 C 0.8344(4) -0.01956(19) 0.9677(5) 0.0461(12) Uani 1 1 d . . . . .
C31 C 0.7400(4) -0.03687(19) 1.0090(5) 0.0471(12) Uani 1 1 d . . . . .
C32 C 0.6844(4) -0.0029(2) 1.0722(8) 0.076(2) Uani 1 1 d . . . . .
H32 H 0.7038 0.0316 1.0841 0.091 Uiso 1 1 calc R U . . .
C33 C 0.6010(5) -0.0187(3) 1.1181(9) 0.098(3) Uani 1 1 d . . . . .
H33 H 0.5643 0.0047 1.1618 0.117 Uiso 1 1 calc R U . . .
C34 C 0.5718(4) -0.0697(3) 1.0990(7) 0.0706(18) Uani 1 1 d . . . . .
C35 C 0.6251(5) -0.1041(2) 1.0352(7) 0.0684(17) Uani 1 1 d . . . . .
H35 H 0.6049 -0.1384 1.0220 0.082 Uiso 1 1 calc R U . . .
C36 C 0.7091(4) -0.0877(2) 0.9903(6) 0.0562(14) Uani 1 1 d . . . . .
H36 H 0.7457 -0.1111 0.9467 0.067 Uiso 1 1 calc R U . . .
N1 N 0.8553(3) 0.13546(17) 0.8089(5) 0.0549(11) Uani 1 1 d . . . . .
N2 N 0.9431(3) 0.20541(15) 0.9761(4) 0.0437(9) Uani 1 1 d . . . . .
N3 N 1.0628(3) 0.16629(16) 1.1678(4) 0.0519(11) Uani 1 1 d . . . . .
O3 O 1.0152(3) 0.05381(13) 0.7983(4) 0.0577(10) Uani 1 1 d . . . . .
O4 O 1.0797(3) 0.13102(13) 0.8418(4) 0.0582(10) Uani 1 1 d . . . . .
O1 O 0.8223(3) 0.13387(14) 1.1101(4) 0.0593(10) Uani 1 1 d . . . . .
O2 O 0.7786(3) 0.09356(16) 1.2860(4) 0.0642(11) Uani 1 1 d . . . . .
O5 O 0.8527(3) 0.02845(14) 0.9732(4) 0.0612(10) Uani 1 1 d . . . . .
O6 O 1.1102(3) 0.05312(14) 1.0698(4) 0.0575(10) Uani 1 1 d . . . . .
OW1 O 0.9522(3) 0.05582(17) 1.2345(4) 0.0578(10) Uani 1 1 d . . . . .
I1 I 1.36853(7) 0.03998(3) 0.36040(8) 0.1471(3) Uani 1 1 d . . . . .
I2 I 0.38222(5) 0.25451(3) 1.14704(9) 0.1362(3) Uani 1 1 d . . . . .
I3 I 0.44839(4) -0.09524(3) 1.18089(7) 0.1121(2) Uani 1 1 d . . . . .
La1 La 0.96316(2) 0.09965(2) 1.01086(3) 0.04073(10) Uani 1 1 d . . . . .
HW1A H 0.891(7) 0.058(4) 1.260(9) 0.13(4) Uiso 1 1 d . . . . .
HW1B H 0.957(5) 0.026(3) 1.204(7) 0.07(2) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.344(7) . ?
C1 C2 1.355(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.360(11) . ?
C2 H2 0.9300 . ?
C3 C4 1.369(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.380(9) . ?
C4 H4 0.9300 . ?
C5 N1 1.326(7) . ?
C5 C6 1.485(8) . ?
C6 N2 1.342(7) . ?
C6 C7 1.402(7) . ?
C7 C8 1.364(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.358(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.397(7) . ?
C9 H9 0.9300 . ?
C10 N2 1.345(7) . ?
C10 C11 1.485(8) . ?
C11 N3 1.349(6) . ?
C11 C12 1.391(8) . ?
C12 C13 1.362(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.370(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.358(9) . ?
C14 H14 0.9300 . ?
C15 N3 1.338(7) . ?
C15 H15 0.9300 . ?
C16 O4 1.259(6) . ?
C16 O3 1.272(6) . ?
C16 C17 1.500(7) . ?
C16 La1 2.994(5) . ?
C17 C18 1.371(8) . ?
C17 C22 1.393(8) . ?
C18 C19 1.381(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.383(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.362(11) . ?
C20 I1 2.096(6) . ?
C21 C22 1.359(9) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O2 1.235(7) . ?
C23 O1 1.267(7) . ?
C23 C24 1.510(8) . ?
C24 C25 1.377(9) . ?
C24 C29 1.383(8) . ?
C25 C26 1.389(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.369(10) . ?
C26 H26 0.9300 . ?
C27 C28 1.349(11) . ?
C27 I2 2.097(7) . ?
C28 C29 1.394(10) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 O6 1.244(6) 3_757 ?
C30 O5 1.257(6) . ?
C30 C31 1.501(7) . ?
C31 C32 1.370(8) . ?
C31 C36 1.382(7) . ?
C32 C33 1.368(9) . ?
C32 H32 0.9300 . ?
C33 C34 1.381(9) . ?
C33 H33 0.9300 . ?
C34 C35 1.360(9) . ?
C34 I3 2.101(6) . ?
C35 C36 1.376(9) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N1 La1 2.681(5) . ?
N2 La1 2.743(4) . ?
N3 La1 2.699(4) . ?
O3 La1 2.645(4) . ?
O4 La1 2.614(4) . ?
O1 La1 2.469(4) . ?
O5 La1 2.421(4) . ?
O6 C30 1.244(6) 3_757 ?
O6 La1 2.451(4) . ?
OW1 La1 2.592(4) . ?
OW1 HW1A 0.93(10) . ?
OW1 HW1B 0.82(7) . ?

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
N1 C1 C2 124.7(6) . . ?
N1 C1 H1 117.7 . . ?
C2 C1 H1 117.7 . . ?
C1 C2 C3 117.3(7) . . ?
C1 C2 H2 121.4 . . ?
C3 C2 H2 121.4 . . ?
C2 C3 C4 119.4(7) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C5 120.1(7) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
N1 C5 C4 120.6(6) . . ?
N1 C5 C6 117.2(5) . . ?
C4 C5 C6 122.1(5) . . ?
N2 C6 C7 120.9(5) . . ?
N2 C6 C5 118.6(4) . . ?
C7 C6 C5 120.5(5) . . ?
C8 C7 C6 120.0(6) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C9 C8 C7 119.1(5) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C10 119.5(6) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
N2 C10 C9 121.7(6) . . ?
N2 C10 C11 117.7(4) . . ?
C9 C10 C11 120.6(5) . . ?
N3 C11 C12 120.4(5) . . ?
N3 C11 C10 117.3(5) . . ?
C12 C11 C10 122.3(5) . . ?
C13 C12 C11 120.1(5) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 119.1(6) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
C15 C14 C13 118.7(6) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
N3 C15 C14 123.5(6) . . ?
N3 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
O4 C16 O3 122.0(5) . . ?
O4 C16 C17 119.1(5) . . ?
O3 C16 C17 118.9(4) . . ?
O4 C16 La1 60.5(3) . . ?
O3 C16 La1 61.9(3) . . ?
C17 C16 La1 171.1(4) . . ?
C18 C17 C22 119.6(6) . . ?
C18 C17 C16 120.0(5) . . ?
C22 C17 C16 120.3(5) . . ?
C17 C18 C19 120.3(6) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C20 118.7(7) . . ?
C18 C19 H19 120.7 . . ?
C20 C19 H19 120.7 . . ?
C21 C20 C19 121.5(6) . . ?
C21 C20 I1 118.9(5) . . ?
C19 C20 I1 119.5(6) . . ?
C22 C21 C20 119.5(7) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C21 C22 C17 120.4(7) . . ?
C21 C22 H22 119.8 . . ?
C17 C22 H22 119.8 . . ?
O2 C23 O1 125.0(5) . . ?
O2 C23 C24 119.3(5) . . ?
O1 C23 C24 115.6(5) . . ?
C25 C24 C29 118.5(6) . . ?
C25 C24 C23 120.9(5) . . ?
C29 C24 C23 120.6(6) . . ?
C24 C25 C26 120.8(6) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C27 C26 C25 119.3(7) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
C28 C27 C26 120.9(7) . . ?
C28 C27 I2 120.0(6) . . ?
C26 C27 I2 119.1(6) . . ?
C27 C28 C29 120.1(7) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C24 C29 C28 120.2(7) . . ?
C24 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
O6 C30 O5 123.8(5) 3_757 . ?
O6 C30 C31 118.7(4) 3_757 . ?
O5 C30 C31 117.5(5) . . ?
C32 C31 C36 118.5(5) . . ?
C32 C31 C30 120.1(5) . . ?
C36 C31 C30 121.3(5) . . ?
C33 C32 C31 121.2(6) . . ?
C33 C32 H32 119.4 . . ?
C31 C32 H32 119.4 . . ?
C32 C33 C34 119.3(6) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 H33 120.4 . . ?
C35 C34 C33 120.7(6) . . ?
C35 C34 I3 120.0(5) . . ?
C33 C34 I3 119.1(5) . . ?
C34 C35 C36 119.3(6) . . ?
C34 C35 H35 120.4 . . ?
C36 C35 H35 120.4 . . ?
C35 C36 C31 121.0(5) . . ?
C35 C36 H36 119.5 . . ?
C31 C36 H36 119.5 . . ?
C5 N1 C1 117.6(5) . . ?
C5 N1 La1 122.8(4) . . ?
C1 N1 La1 119.2(4) . . ?
C6 N2 C10 118.8(4) . . ?
C6 N2 La1 119.6(3) . . ?
C10 N2 La1 121.6(3) . . ?
C15 N3 C11 118.1(5) . . ?
C15 N3 La1 118.6(3) . . ?
C11 N3 La1 123.3(4) . . ?
C16 O3 La1 93.0(3) . . ?
C16 O4 La1 94.7(3) . . ?
C23 O1 La1 142.8(4) . . ?
C30 O5 La1 150.9(4) . . ?
C30 O6 La1 143.5(4) 3_757 . ?
La1 OW1 HW1A 110(6) . . ?
La1 OW1 HW1B 92(5) . . ?
HW1A OW1 HW1B 105(7) . . ?
O5 La1 O6 102.10(13) . . ?
O5 La1 O1 78.43(13) . . ?
O6 La1 O1 140.34(14) . . ?
O5 La1 OW1 75.21(14) . . ?
O6 La1 OW1 70.36(15) . . ?
O1 La1 OW1 71.60(15) . . ?
O5 La1 O4 123.68(13) . . ?
O6 La1 O4 75.52(13) . . ?
O1 La1 O4 137.38(12) . . ?
OW1 La1 O4 144.11(15) . . ?
O5 La1 O3 75.15(13) . . ?
O6 La1 O3 73.39(13) . . ?
O1 La1 O3 141.41(14) . . ?
OW1 La1 O3 126.21(14) . . ?
O4 La1 O3 49.78(11) . . ?
O5 La1 N1 78.29(14) . . ?
O6 La1 N1 143.04(14) . . ?
O1 La1 N1 76.44(14) . . ?
OW1 La1 N1 141.74(15) . . ?
O4 La1 N1 74.09(14) . . ?
O3 La1 N1 71.06(14) . . ?
O5 La1 N3 152.13(15) . . ?
O6 La1 N3 75.42(13) . . ?
O1 La1 N3 86.18(14) . . ?
OW1 La1 N3 77.94(14) . . ?
O4 La1 N3 83.12(14) . . ?
O3 La1 N3 128.33(13) . . ?
N1 La1 N3 120.64(13) . . ?
O5 La1 N2 131.30(13) . . ?
O6 La1 N2 126.33(13) . . ?
O1 La1 N2 67.95(12) . . ?
OW1 La1 N2 122.24(14) . . ?
O4 La1 N2 70.95(11) . . ?
O3 La1 N2 111.10(12) . . ?
N1 La1 N2 60.66(13) . . ?
N3 La1 N2 60.17(13) . . ?
O5 La1 C16 99.98(15) . . ?
O6 La1 C16 71.14(14) . . ?
O1 La1 C16 148.44(14) . . ?
OW1 La1 C16 139.06(15) . . ?
O4 La1 C16 24.78(12) . . ?
O3 La1 C16 25.10(12) . . ?
N1 La1 C16 72.43(15) . . ?
N3 La1 C16 105.18(15) . . ?
N2 La1 C16 91.91(12) . . ?

_refine_diff_density_max         1.926
_refine_diff_density_min         -1.793
_refine_diff_density_rms         0.109

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_14
_database_code_depnum_ccdc_archive 'CCDC 1514995'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 I6 Lu2 N6 O14'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293
_chemical_formula_weight         2334.52

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'
I I -0.4742 1.8119 '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      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                   11.1864(9)
_cell_length_b                   12.7860(7)
_cell_length_c                   14.4367(8)
_cell_angle_alpha                68.8850(10)
_cell_angle_beta                 88.375(3)
_cell_angle_gamma                72.644(2)
_cell_volume                     1831.3(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    27070
_cell_measurement_theta_min      4.366
_cell_measurement_theta_max      57.585

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_F_000             1096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.126
_exptl_absorpt_coefficient_mu    5.276
_shelx_estimated_absorpt_T_min   0.373
_shelx_estimated_absorpt_T_max   0.556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6230
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27068
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.518
_diffrn_reflns_theta_max         29.611
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10049
_reflns_number_gt                8557
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0540P)²+3.0182P] 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         10049
_refine_ls_number_parameters     469
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.1033
_refine_ls_wR_factor_gt          0.0973
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.002
_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
C15 C 1.0919(4) 0.7299(4) 0.6292(4) 0.0479(11) Uani 1 1 d . . . . .
H15 H 1.1273 0.6560 0.6254 0.057 Uiso 1 1 calc R U . . .
C14 C 1.1611(5) 0.7676(5) 0.6816(4) 0.0504(11) Uani 1 1 d . . . . .
H14 H 1.2409 0.7202 0.7119 0.060 Uiso 1 1 calc R U . . .
C13 C 1.1093(5) 0.8764(5) 0.6877(4) 0.0521(12) Uani 1 1 d . . . . .
H13 H 1.1531 0.9044 0.7223 0.062 Uiso 1 1 calc R U . . .
C12 C 0.9914(5) 0.9427(4) 0.6415(4) 0.0485(11) Uani 1 1 d . . . . .
H12 H 0.9547 1.0168 0.6445 0.058 Uiso 1 1 calc R U . . .
C11 C 0.9268(4) 0.9008(3) 0.5909(3) 0.0365(9) Uani 1 1 d . . . . .
C10 C 0.8031(4) 0.9721(4) 0.5366(3) 0.0401(9) Uani 1 1 d . . . . .
C9 C 0.7391(5) 1.0831(4) 0.5397(4) 0.0528(12) Uani 1 1 d . . . . .
H9 H 0.7733 1.1128 0.5788 0.063 Uiso 1 1 calc R U . . .
C8 C 0.6242(6) 1.1484(4) 0.4837(5) 0.0656(17) Uani 1 1 d . . . . .
H8 H 0.5793 1.2210 0.4868 0.079 Uiso 1 1 calc R U . . .
C7 C 0.5784(5) 1.1044(4) 0.4245(4) 0.0554(13) Uani 1 1 d . . . . .
H7 H 0.5032 1.1480 0.3847 0.066 Uiso 1 1 calc R U . . .
C6 C 0.6452(4) 0.9934(4) 0.4239(3) 0.0411(10) Uani 1 1 d . . . . .
C5 C 0.5965(4) 0.9401(4) 0.3646(4) 0.0465(11) Uani 1 1 d . . . . .
C4 C 0.4957(6) 1.0047(6) 0.2914(5) 0.0725(18) Uani 1 1 d . . . . .
H4 H 0.4592 1.0852 0.2760 0.087 Uiso 1 1 calc R U . . .
C3 C 0.4509(6) 0.9472(7) 0.2421(6) 0.086(2) Uani 1 1 d . . . . .
H3 H 0.3867 0.9891 0.1908 0.104 Uiso 1 1 calc R U . . .
C2 C 0.5024(6) 0.8277(7) 0.2698(6) 0.079(2) Uani 1 1 d . . . . .
H2 H 0.4695 0.7861 0.2416 0.094 Uiso 1 1 calc R U . . .
C1 C 0.6033(5) 0.7708(5) 0.3399(5) 0.0596(14) Uani 1 1 d . . . . .
H1 H 0.6406 0.6903 0.3559 0.072 Uiso 1 1 calc R U . . .
C16 C 0.6930(4) 0.6423(3) 0.6270(3) 0.0367(9) Uani 1 1 d . . . . .
C17 C 0.6036(4) 0.5993(4) 0.6977(3) 0.0377(9) Uani 1 1 d . . . . .
C18 C 0.5914(5) 0.6173(5) 0.7863(4) 0.0485(11) Uani 1 1 d . . . . .
H18 H 0.6417 0.6550 0.8034 0.058 Uiso 1 1 calc R U . . .
C19 C 0.5055(5) 0.5803(6) 0.8502(4) 0.0576(13) Uani 1 1 d . . . . .
H19 H 0.4985 0.5924 0.9101 0.069 Uiso 1 1 calc R U . . .
C20 C 0.4297(5) 0.5250(5) 0.8243(4) 0.0512(12) Uani 1 1 d . . . . .
C21 C 0.4393(5) 0.5070(5) 0.7359(4) 0.0560(13) Uani 1 1 d . . . . .
H21 H 0.3877 0.4704 0.7190 0.067 Uiso 1 1 calc R U . . .
C22 C 0.5263(5) 0.5435(4) 0.6719(4) 0.0476(11) Uani 1 1 d . . . . .
H22 H 0.5333 0.5310 0.6121 0.057 Uiso 1 1 calc R U . . .
C23 C 1.0132(4) 0.7898(4) 0.3401(3) 0.0384(9) Uani 1 1 d . . . . .
C24 C 1.0889(4) 0.8093(4) 0.2515(3) 0.0377(9) Uani 1 1 d . . . . .
C25 C 1.1918(5) 0.7180(5) 0.2467(4) 0.0492(11) Uani 1 1 d . . . . .
H25 H 1.2151 0.6455 0.2993 0.059 Uiso 1 1 calc R U . . .
C26 C 1.2591(5) 0.7352(5) 0.1637(4) 0.0560(13) Uani 1 1 d . . . . .
H26 H 1.3267 0.6738 0.1600 0.067 Uiso 1 1 calc R U . . .
C27 C 1.2264(5) 0.8431(5) 0.0866(4) 0.0541(12) Uani 1 1 d . . . . .
C28 C 1.1252(6) 0.9347(5) 0.0903(4) 0.0601(14) Uani 1 1 d . . . . .
H28 H 1.1038 1.0076 0.0382 0.072 Uiso 1 1 calc R U . . .
C29 C 1.0557(5) 0.9170(4) 0.1727(4) 0.0504(11) Uani 1 1 d . . . . .
H29 H 0.9864 0.9779 0.1749 0.060 Uiso 1 1 calc R U . . .
C30 C 0.9437(4) 0.5511(3) 0.3503(3) 0.0306(7) Uani 1 1 d . . . . .
C31 C 0.9373(4) 0.6035(3) 0.2386(3) 0.0322(8) Uani 1 1 d . . . . .
C32 C 0.8529(5) 0.7127(4) 0.1861(3) 0.0427(10) Uani 1 1 d . . . . .
H32 H 0.8026 0.7558 0.2206 0.051 Uiso 1 1 calc R U . . .
C33 C 0.8421(6) 0.7592(4) 0.0826(4) 0.0517(12) Uani 1 1 d . . . . .
H33 H 0.7848 0.8327 0.0477 0.062 Uiso 1 1 calc R U . . .
C34 C 0.9174(5) 0.6948(4) 0.0327(3) 0.0478(11) Uani 1 1 d . . . . .
C35 C 1.0050(5) 0.5876(4) 0.0830(4) 0.0483(11) Uani 1 1 d . . . . .
H35 H 1.0572 0.5462 0.0482 0.058 Uiso 1 1 calc R U . . .
C36 C 1.0146(4) 0.5423(4) 0.1858(3) 0.0403(9) Uani 1 1 d . . . . .
H36 H 1.0737 0.4698 0.2202 0.048 Uiso 1 1 calc R U . . .
N3 N 0.9772(3) 0.7939(3) 0.5842(3) 0.0381(8) Uani 1 1 d . . . . .
N2 N 0.7545(3) 0.9279(3) 0.4801(3) 0.0367(7) Uani 1 1 d . . . . .
N1 N 0.6513(4) 0.8245(3) 0.3867(3) 0.0445(9) Uani 1 1 d . . . . .
O1 O 0.7170(3) 0.6056(3) 0.5557(3) 0.0483(8) Uani 1 1 d . . . . .
O2 O 0.7406(3) 0.7156(3) 0.6361(2) 0.0407(7) Uani 1 1 d . . . . .
O3 O 1.0627(3) 0.7076(3) 0.4214(2) 0.0476(8) Uani 1 1 d . . . . .
O4 O 0.9015(3) 0.8531(3) 0.3324(2) 0.0430(7) Uani 1 1 d . . . . .
O5 O 0.8731(3) 0.6117(3) 0.3935(2) 0.0392(6) Uani 1 1 d . . . . .
O6 O 0.9821(3) 0.5508(3) 0.6072(2) 0.0419(7) Uani 1 1 d . . . . .
I1 I 0.29500(5) 0.47274(6) 0.91671(4) 0.0976(2) Uani 1 1 d . . . . .
I2 I 1.32945(6) 0.87085(6) -0.03902(4) 0.1058(2) Uani 1 1 d . . . . .
I3A I 0.8799(4) 0.7566(4) -0.1263(2) 0.0656(6) Uani 0.67(3) 1 d . . P A 1
I3B I 0.919(3) 0.7616(6) -0.1182(7) 0.081(3) Uani 0.33(3) 1 d . . P A 2
Lu1 Lu 0.86042(2) 0.71764(2) 0.49099(2) 0.03307(6) Uani 1 1 d . . . . .
OW1 O 0.3123(5) 0.5777(6) 0.5069(5) 0.0859(15) Uani 1 1 d D . . . .
HW1B H 0.238(2) 0.612(6) 0.487(6) 0.09(3) Uiso 1 1 d D . . . .
HW1A H 0.309(8) 0.517(4) 0.502(6) 0.09(3) Uiso 1 1 d 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
C15 N3 1.333(6) . ?
C15 C14 1.387(7) . ?
C15 H15 0.9300 . ?
C14 C13 1.372(7) . ?
C14 H14 0.9300 . ?
C13 C12 1.371(8) . ?
C13 H13 0.9300 . ?
C12 C11 1.373(6) . ?
C12 H12 0.9300 . ?
C11 N3 1.353(5) . ?
C11 C10 1.468(7) . ?
C10 N2 1.350(6) . ?
C10 C9 1.401(6) . ?
C9 C8 1.391(9) . ?
C9 H9 0.9300 . ?
C8 C7 1.362(9) . ?
C8 H8 0.9300 . ?
C7 C6 1.396(6) . ?
C7 H7 0.9300 . ?
C6 N2 1.346(6) . ?
C6 C5 1.470(7) . ?
C5 N1 1.338(6) . ?
C5 C4 1.399(7) . ?
C4 C3 1.384(10) . ?
C4 H4 0.9300 . ?
C3 C2 1.369(10) . ?
C3 H3 0.9300 . ?
C2 C1 1.368(8) . ?
C2 H2 0.9300 . ?
C1 N1 1.338(7) . ?
C1 H1 0.9300 . ?
C16 O2 1.253(5) . ?
C16 O1 1.268(5) . ?
C16 C17 1.487(6) . ?
C16 Lu1 2.792(4) . ?
C17 C18 1.375(7) . ?
C17 C22 1.406(7) . ?
C18 C19 1.379(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.388(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.370(8) . ?
C20 I1 2.084(5) . ?
C21 C22 1.388(7) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O4 1.252(5) . ?
C23 O3 1.260(5) . ?
C23 C24 1.501(6) . ?
C23 Lu1 2.793(4) . ?
C24 C29 1.385(7) . ?
C24 C25 1.394(6) . ?
C25 C26 1.381(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.376(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.381(8) . ?
C27 I2 2.099(5) . ?
C28 C29 1.388(7) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 O5 1.251(5) . ?
C30 O6 1.253(5) 2_766 ?
C30 C31 1.502(5) . ?
C31 C32 1.381(6) . ?
C31 C36 1.390(5) . ?
C32 C33 1.388(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.374(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.374(7) . ?
C34 I3B 2.034(8) . ?
C34 I3A 2.148(6) . ?
C35 C36 1.379(6) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N3 Lu1 2.504(4) . ?
N2 Lu1 2.542(3) . ?
N1 Lu1 2.534(4) . ?
O1 Lu1 2.413(3) . ?
O2 Lu1 2.451(3) . ?
O3 Lu1 2.437(3) . ?
O4 Lu1 2.452(3) . ?
O5 Lu1 2.255(3) . ?
O6 C30 1.253(5) 2_766 ?
O6 Lu1 2.245(3) . ?
OW1 HW1B 0.819(10) . ?
OW1 HW1A 0.821(10) . ?

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
N3 C15 C14 123.4(4) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
C13 C14 C15 118.6(5) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
C12 C13 C14 118.3(5) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C13 C12 C11 120.7(4) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
N3 C11 C12 121.5(4) . . ?
N3 C11 C10 116.5(4) . . ?
C12 C11 C10 121.9(4) . . ?
N2 C10 C9 120.8(5) . . ?
N2 C10 C11 116.9(3) . . ?
C9 C10 C11 122.2(5) . . ?
C8 C9 C10 119.6(5) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C7 C8 C9 118.9(4) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C8 C7 C6 119.5(5) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
N2 C6 C7 122.0(5) . . ?
N2 C6 C5 116.6(4) . . ?
C7 C6 C5 121.4(5) . . ?
N1 C5 C4 121.3(5) . . ?
N1 C5 C6 116.4(4) . . ?
C4 C5 C6 122.3(5) . . ?
C3 C4 C5 119.1(6) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C2 C3 C4 119.0(6) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C1 C2 C3 118.6(6) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
N1 C1 C2 123.6(6) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
O2 C16 O1 120.9(4) . . ?
O2 C16 C17 120.6(4) . . ?
O1 C16 C17 118.4(4) . . ?
O2 C16 Lu1 61.3(2) . . ?
O1 C16 Lu1 59.6(2) . . ?
C17 C16 Lu1 178.0(3) . . ?
C18 C17 C22 119.2(4) . . ?
C18 C17 C16 121.3(4) . . ?
C22 C17 C16 119.4(4) . . ?
C17 C18 C19 120.9(5) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.5 . . ?
C18 C19 C20 119.5(5) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C21 C20 C19 120.6(5) . . ?
C21 C20 I1 118.7(4) . . ?
C19 C20 I1 120.6(4) . . ?
C20 C21 C22 119.9(5) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C21 C22 C17 119.8(5) . . ?
C21 C22 H22 120.1 . . ?
C17 C22 H22 120.1 . . ?
O4 C23 O3 120.7(4) . . ?
O4 C23 C24 120.1(4) . . ?
O3 C23 C24 119.1(4) . . ?
O4 C23 Lu1 61.3(2) . . ?
O3 C23 Lu1 60.7(2) . . ?
C24 C23 Lu1 167.4(3) . . ?
C29 C24 C25 119.3(4) . . ?
C29 C24 C23 120.5(4) . . ?
C25 C24 C23 120.2(4) . . ?
C26 C25 C24 120.0(5) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C27 C26 C25 120.1(5) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C28 120.6(5) . . ?
C26 C27 I2 120.4(4) . . ?
C28 C27 I2 119.0(4) . . ?
C27 C28 C29 119.4(5) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C24 C29 C28 120.5(5) . . ?
C24 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
O5 C30 O6 125.2(4) . 2_766 ?
O5 C30 C31 117.6(3) . . ?
O6 C30 C31 117.2(3) 2_766 . ?
C32 C31 C36 118.6(4) . . ?
C32 C31 C30 120.7(4) . . ?
C36 C31 C30 120.7(4) . . ?
C31 C32 C33 121.0(4) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C34 C33 C32 118.8(4) . . ?
C34 C33 H33 120.6 . . ?
C32 C33 H33 120.6 . . ?
C33 C34 C35 121.4(4) . . ?
C33 C34 I3B 121.5(5) . . ?
C35 C34 I3B 116.7(6) . . ?
C33 C34 I3A 117.9(4) . . ?
C35 C34 I3A 120.3(4) . . ?
C34 C35 C36 119.1(4) . . ?
C34 C35 H35 120.4 . . ?
C36 C35 H35 120.4 . . ?
C35 C36 C31 121.0(4) . . ?
C35 C36 H36 119.5 . . ?
C31 C36 H36 119.5 . . ?
C15 N3 C11 117.5(4) . . ?
C15 N3 Lu1 120.9(3) . . ?
C11 N3 Lu1 121.6(3) . . ?
C6 N2 C10 119.1(4) . . ?
C6 N2 Lu1 120.8(3) . . ?
C10 N2 Lu1 119.9(3) . . ?
C1 N1 C5 118.2(4) . . ?
C1 N1 Lu1 120.1(3) . . ?
C5 N1 Lu1 120.8(3) . . ?
C16 O1 Lu1 93.4(3) . . ?
C16 O2 Lu1 92.0(3) . . ?
C23 O3 Lu1 92.5(3) . . ?
C23 O4 Lu1 92.1(3) . . ?
C30 O5 Lu1 146.4(3) . . ?
C30 O6 Lu1 162.7(3) 2_766 . ?
O6 Lu1 O5 86.62(11) . . ?
O6 Lu1 O1 76.60(12) . . ?
O5 Lu1 O1 75.93(12) . . ?
O6 Lu1 O3 80.11(12) . . ?
O5 Lu1 O3 74.70(12) . . ?
O1 Lu1 O3 143.27(12) . . ?
O6 Lu1 O2 79.74(11) . . ?
O5 Lu1 O2 129.43(11) . . ?
O1 Lu1 O2 53.58(11) . . ?
O3 Lu1 O2 147.10(11) . . ?
O6 Lu1 O4 133.09(11) . . ?
O5 Lu1 O4 79.14(11) . . ?
O1 Lu1 O4 139.56(12) . . ?
O3 Lu1 O4 53.07(10) . . ?
O2 Lu1 O4 141.63(10) . . ?
O6 Lu1 N3 77.79(12) . . ?
O5 Lu1 N3 146.58(12) . . ?
O1 Lu1 N3 127.19(12) . . ?
O3 Lu1 N3 73.60(12) . . ?
O2 Lu1 N3 76.90(11) . . ?
O4 Lu1 N3 90.15(12) . . ?
O6 Lu1 N1 146.99(13) . . ?
O5 Lu1 N1 79.22(12) . . ?
O1 Lu1 N1 71.11(13) . . ?
O3 Lu1 N1 123.42(12) . . ?
O2 Lu1 N1 86.49(12) . . ?
O4 Lu1 N1 73.32(12) . . ?
N3 Lu1 N1 128.04(12) . . ?
O6 Lu1 N2 135.72(12) . . ?
O5 Lu1 N2 137.65(11) . . ?
O1 Lu1 N2 108.20(11) . . ?
O3 Lu1 N2 108.33(12) . . ?
O2 Lu1 N2 70.43(10) . . ?
O4 Lu1 N2 71.40(10) . . ?
N3 Lu1 N2 64.29(12) . . ?
N1 Lu1 N2 63.75(13) . . ?
O6 Lu1 C16 76.20(12) . . ?
O5 Lu1 C16 102.80(12) . . ?
O1 Lu1 C16 26.95(12) . . ?
O3 Lu1 C16 156.29(11) . . ?
O2 Lu1 C16 26.64(11) . . ?
O4 Lu1 C16 150.48(11) . . ?
N3 Lu1 C16 101.89(13) . . ?
N1 Lu1 C16 78.11(13) . . ?
N2 Lu1 C16 89.54(11) . . ?
O6 Lu1 C23 106.50(13) . . ?
O5 Lu1 C23 72.19(12) . . ?
O1 Lu1 C23 147.66(12) . . ?
O3 Lu1 C23 26.80(12) . . ?
O2 Lu1 C23 158.29(11) . . ?
O4 Lu1 C23 26.63(11) . . ?
N3 Lu1 C23 84.05(12) . . ?
N1 Lu1 C23 97.36(13) . . ?
N2 Lu1 C23 92.04(12) . . ?
C16 Lu1 C23 173.94(13) . . ?
HW1B OW1 HW1A 93(7) . . ?

_refine_diff_density_max         2.266
_refine_diff_density_min         -2.370
_refine_diff_density_rms         0.127

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_2Prime
_database_code_depnum_ccdc_archive 'CCDC 1514980'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 Ce2 I6 N6 O14'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2264.82

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 '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                   11.198(5)
_cell_length_b                   13.030(5)
_cell_length_c                   14.604(5)
_cell_angle_alpha                69.314(4)
_cell_angle_beta                 89.085(3)
_cell_angle_gamma                72.956(5)
_cell_volume                     1896.8(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    28303
_cell_measurement_theta_min      4.716
_cell_measurement_theta_max      59.390

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_F_000             1070
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.182
_exptl_absorpt_coefficient_mu    3.691
_shelx_estimated_absorpt_T_min   0.288
_shelx_estimated_absorpt_T_max   0.553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6031
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focused sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28296
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.498
_diffrn_reflns_theta_max         30.517
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10668
_reflns_number_gt                9014
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0262P)²+0.8156P] 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         10668
_refine_ls_number_parameters     489
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_ref         0.0637
_refine_ls_wR_factor_gt          0.0597
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0905(3) 0.2968(3) 0.3315(3) 0.0752(10) Uani 1 1 d . . . . .
H1 H 0.1243 0.2183 0.3446 0.090 Uiso 1 1 calc R U . . .
C2 C -0.0085(4) 0.3592(4) 0.2600(3) 0.0971(14) Uani 1 1 d . . . . .
H2 H -0.0414 0.3235 0.2262 0.117 Uiso 1 1 calc R U . . .
C3 C -0.0567(4) 0.4736(4) 0.2399(3) 0.1060(15) Uani 1 1 d . . . . .
H3 H -0.1214 0.5183 0.1900 0.127 Uiso 1 1 calc R U . . .
C4 C -0.0099(3) 0.5240(3) 0.2937(3) 0.0867(11) Uani 1 1 d . . . . .
H4 H -0.0446 0.6021 0.2822 0.104 Uiso 1 1 calc R U . . .
C5 C 0.0906(2) 0.4556(2) 0.3659(2) 0.0549(7) Uani 1 1 d . . . . .
N2 N 0.25509(13) 0.43635(10) 0.48191(11) 0.0409(4) Uani 1 1 d G . . . .
C6 C 0.14059(13) 0.50248(13) 0.42664(12) 0.0495(6) Uani 1 1 d G . . . .
C7 C 0.07860(13) 0.60948(13) 0.43153(14) 0.0635(8) Uani 1 1 d G . . . .
H7 H 0.0020 0.6537 0.3946 0.076 Uiso 1 1 calc R U . . .
C8 C 0.13111(17) 0.65034(11) 0.49170(16) 0.0749(10) Uani 1 1 d G . . . .
H8 H 0.0896 0.7219 0.4950 0.090 Uiso 1 1 calc R U . . .
C9 C 0.24561(17) 0.58421(14) 0.54698(14) 0.0617(8) Uani 1 1 d G . . . .
H9 H 0.2807 0.6116 0.5872 0.074 Uiso 1 1 calc R U . . .
C10 C 0.30760(12) 0.47722(12) 0.54208(11) 0.0448(5) Uani 1 1 d G . . . .
C11 C 0.4311(2) 0.40605(19) 0.59292(17) 0.0410(5) Uani 1 1 d . . . . .
C12 C 0.4974(3) 0.4460(2) 0.6443(2) 0.0543(6) Uani 1 1 d . . . . .
H12 H 0.4618 0.5183 0.6482 0.065 Uiso 1 1 calc R U . . .
C13 C 0.6147(3) 0.3804(3) 0.6893(2) 0.0589(7) Uani 1 1 d . . . . .
H13 H 0.6594 0.4071 0.7242 0.071 Uiso 1 1 calc R U . . .
C14 C 0.6655(3) 0.2747(3) 0.6824(2) 0.0572(7) Uani 1 1 d . . . . .
H14 H 0.7453 0.2281 0.7122 0.069 Uiso 1 1 calc R U . . .
C15 C 0.5957(3) 0.2389(2) 0.6301(2) 0.0549(6) Uani 1 1 d . . . . .
H15 H 0.6304 0.1669 0.6255 0.066 Uiso 1 1 calc R U . . .
C16 C 0.1826(2) 0.1421(2) 0.62773(18) 0.0425(5) Uani 1 1 d . . . . .
C17 C 0.0951(2) 0.0972(2) 0.69853(18) 0.0425(5) Uani 1 1 d . . . . .
C18 C 0.0192(2) 0.0420(2) 0.6742(2) 0.0513(6) Uani 1 1 d . . . . .
H18 H 0.0249 0.0301 0.6150 0.062 Uiso 1 1 calc R U . . .
C19 C -0.0657(3) 0.0042(3) 0.7381(2) 0.0580(7) Uani 1 1 d . . . . .
H19 H -0.1165 -0.0331 0.7219 0.070 Uiso 1 1 calc R U . . .
C20 C -0.0737(3) 0.0226(3) 0.8254(2) 0.0557(7) Uani 1 1 d . . . . .
C21 C 0.0014(3) 0.0771(3) 0.8507(2) 0.0610(7) Uani 1 1 d . . . . .
H21 H -0.0044 0.0886 0.9101 0.073 Uiso 1 1 calc R U . . .
C22 C 0.0859(3) 0.1146(2) 0.7869(2) 0.0517(6) Uani 1 1 d . . . . .
H22 H 0.1367 0.1516 0.8036 0.062 Uiso 1 1 calc R U . . .
C23 C 0.5186(2) 0.2896(2) 0.33276(19) 0.0447(5) Uani 1 1 d . . . . .
C24 C 0.5929(2) 0.3080(2) 0.24620(19) 0.0438(5) Uani 1 1 d . . . . .
C25 C 0.5600(3) 0.4133(3) 0.1685(2) 0.0613(7) Uani 1 1 d . . . . .
H25 H 0.4905 0.4727 0.1702 0.074 Uiso 1 1 calc R U . . .
C26 C 0.6296(3) 0.4308(3) 0.0884(2) 0.0707(9) Uani 1 1 d . . . . .
H26 H 0.6086 0.5023 0.0375 0.085 Uiso 1 1 calc R U . . .
C27 C 0.7299(3) 0.3418(3) 0.0844(2) 0.0662(8) Uani 1 1 d . . . . .
C28 C 0.7624(3) 0.2358(3) 0.1601(2) 0.0693(9) Uani 1 1 d . . . . .
H28 H 0.8291 0.1754 0.1564 0.083 Uiso 1 1 calc R U . . .
C29 C 0.6954(3) 0.2198(3) 0.2413(2) 0.0581(7) Uani 1 1 d . . . . .
H29 H 0.7191 0.1491 0.2933 0.070 Uiso 1 1 calc R U . . .
C30 C 0.4356(2) 0.05301(18) 0.34324(17) 0.0382(5) Uani 1 1 d . . . . .
C31 C 0.4349(2) 0.10400(18) 0.23346(17) 0.0379(5) Uani 1 1 d . . . . .
C32 C 0.3534(3) 0.2120(2) 0.18029(19) 0.0507(6) Uani 1 1 d . . . . .
H32 H 0.3017 0.2547 0.2132 0.061 Uiso 1 1 calc R U . . .
C33 C 0.3479(3) 0.2574(2) 0.0786(2) 0.0588(7) Uani 1 1 d . . . . .
H33 H 0.2924 0.3298 0.0432 0.071 Uiso 1 1 calc R U . . .
C34 C 0.4251(3) 0.1943(2) 0.0308(2) 0.0602(7) Uani 1 1 d . . . . .
C35 C 0.5103(3) 0.0886(3) 0.0826(2) 0.0613(7) Uani 1 1 d . . . . .
H35 H 0.5644 0.0480 0.0495 0.074 Uiso 1 1 calc R U . . .
C36 C 0.5152(2) 0.0432(2) 0.1839(2) 0.0495(6) Uani 1 1 d . . . . .
H36 H 0.5724 -0.0284 0.2190 0.059 Uiso 1 1 calc R U . . .
N1 N 0.1406(2) 0.3433(2) 0.38306(18) 0.0550(6) Uani 1 1 d . . . . .
N3 N 0.48081(19) 0.30196(17) 0.58575(16) 0.0456(5) Uani 1 1 d . . . . .
O1 O 0.2015(2) 0.11055(18) 0.55493(15) 0.0582(5) Uani 1 1 d . . . . .
O2 O 0.23216(17) 0.21157(15) 0.64068(14) 0.0489(4) Uani 1 1 d . . . . .
O3 O 0.40749(17) 0.35399(14) 0.32523(14) 0.0504(4) Uani 1 1 d . . . . .
O4 O 0.56760(17) 0.20769(18) 0.41300(14) 0.0588(5) Uani 1 1 d . . . . .
O5 O 0.36174(18) 0.11226(14) 0.38413(13) 0.0488(4) Uani 1 1 d . . . . .
O6 O 0.49162(18) 0.04618(14) 0.61301(13) 0.0528(4) Uani 1 1 d . . . . .
OW1 O -0.1861(3) 0.0795(4) 0.5025(3) 0.1000(11) Uani 1 1 d . . . . .
I1A I -0.2012(3) -0.0383(4) 0.9173(2) 0.0986(5) Uani 0.603(19) 1 d . . P A 1
I1B I -0.2093(3) -0.0187(6) 0.9204(3) 0.0954(8) Uani 0.397(19) 1 d . . P A 2
I2A I 0.8364(3) 0.3762(3) -0.0345(3) 0.1131(7) Uani 0.652(18) 1 d . . P B 1
I2B I 0.8263(6) 0.3553(9) -0.0444(3) 0.1154(14) Uani 0.348(18) 1 d . . P B 2
I3A I 0.39057(19) 0.2508(2) -0.12789(13) 0.0768(5) Uani 0.511(12) 1 d . . P C .
I3B I 0.4299(9) 0.26251(19) -0.1172(3) 0.1144(12) Uani 0.489(12) 1 d . . P C 2
Ce1 Ce 0.35964(2) 0.21767(2) 0.49011(2) 0.03628(4) Uani 1 1 d . . . . .
HW1A H -0.246(5) 0.117(5) 0.478(4) 0.12(2) Uiso 1 1 d . . . . .
HW1B H -0.172(6) 0.011(6) 0.501(5) 0.16(3) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.335(4) . ?
C1 C2 1.375(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.350(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.379(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.400(4) . ?
C4 H4 0.9300 . ?
C5 N1 1.335(4) . ?
C5 C6 1.439(3) . ?
N2 C6 1.3900 . ?
N2 C10 1.3900 . ?
N2 Ce1 2.7041(14) . ?
C6 C7 1.3900 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 C9 1.3900 . ?
C8 H8 0.9300 . ?
C9 C10 1.3900 . ?
C9 H9 0.9300 . ?
C10 C11 1.455(3) . ?
C11 N3 1.348(3) . ?
C11 C12 1.381(4) . ?
C12 C13 1.365(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.366(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.377(4) . ?
C14 H14 0.9300 . ?
C15 N3 1.334(3) . ?
C15 H15 0.9300 . ?
C16 O2 1.258(3) . ?
C16 O1 1.263(3) . ?
C16 C17 1.499(3) . ?
C16 Ce1 2.926(3) . ?
C17 C22 1.384(4) . ?
C17 C18 1.384(4) . ?
C18 C19 1.392(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.374(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.376(4) . ?
C20 I1A 2.079(4) . ?
C20 I1B 2.099(4) . ?
C21 C22 1.386(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O3 1.262(3) . ?
C23 O4 1.267(3) . ?
C23 C24 1.489(3) . ?
C23 Ce1 2.941(3) . ?
C24 C29 1.388(4) . ?
C24 C25 1.387(4) . ?
C25 C26 1.383(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.375(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.379(5) . ?
C27 I2A 2.083(4) . ?
C27 I2B 2.133(5) . ?
C28 C29 1.378(4) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 O6 1.248(3) 2_656 ?
C30 O5 1.254(3) . ?
C30 C31 1.502(3) . ?
C31 C32 1.384(3) . ?
C31 C36 1.388(3) . ?
C32 C33 1.385(4) . ?
C32 H32 0.9300 . ?
C33 C34 1.372(4) . ?
C33 H33 0.9300 . ?
C34 C35 1.377(4) . ?
C34 I3B 2.033(4) . ?
C34 I3A 2.173(4) . ?
C35 C36 1.381(4) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N1 Ce1 2.665(2) . ?
N3 Ce1 2.649(2) . ?
O1 Ce1 2.538(2) . ?
O2 Ce1 2.5928(19) . ?
O3 Ce1 2.5952(19) . ?
O4 Ce1 2.559(2) . ?
O5 Ce1 2.4009(17) . ?
O6 C30 1.248(3) 2_656 ?
O6 Ce1 2.3904(18) . ?
OW1 HW1A 0.71(5) . ?
OW1 HW1B 0.86(6) . ?
I3A I3B 0.547(8) . ?

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
N1 C1 C2 123.4(4) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C2 C1 118.4(4) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 119.9(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 118.9(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 120.9(3) . . ?
N1 C5 C6 117.7(2) . . ?
C4 C5 C6 121.4(3) . . ?
C6 N2 C10 120.0 . . ?
C6 N2 Ce1 119.58(7) . . ?
C10 N2 Ce1 119.95(7) . . ?
N2 C6 C7 120.0 . . ?
N2 C6 C5 117.54(14) . . ?
C7 C6 C5 122.46(14) . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 120.0 . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 120.0 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 N2 120.0 . . ?
C9 C10 C11 123.29(13) . . ?
N2 C10 C11 116.60(13) . . ?
N3 C11 C12 120.9(2) . . ?
N3 C11 C10 118.4(2) . . ?
C12 C11 C10 120.7(2) . . ?
C13 C12 C11 120.5(3) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 118.9(3) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
C13 C14 C15 118.4(3) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
N3 C15 C14 123.5(3) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
O2 C16 O1 122.0(2) . . ?
O2 C16 C17 119.7(2) . . ?
O1 C16 C17 118.2(2) . . ?
O2 C16 Ce1 62.31(13) . . ?
O1 C16 Ce1 59.84(13) . . ?
C17 C16 Ce1 177.10(16) . . ?
C22 C17 C18 119.4(2) . . ?
C22 C17 C16 120.4(2) . . ?
C18 C17 C16 120.1(2) . . ?
C17 C18 C19 120.3(3) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C20 C19 C18 119.4(3) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C21 121.0(3) . . ?
C19 C20 I1A 117.0(2) . . ?
C21 C20 I1A 122.1(2) . . ?
C19 C20 I1B 122.0(3) . . ?
C21 C20 I1B 116.9(3) . . ?
C20 C21 C22 119.5(3) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C17 C22 C21 120.4(3) . . ?
C17 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
O3 C23 O4 120.8(2) . . ?
O3 C23 C24 120.0(2) . . ?
O4 C23 C24 119.2(2) . . ?
O3 C23 Ce1 61.79(13) . . ?
O4 C23 Ce1 60.18(13) . . ?
C24 C23 Ce1 168.10(17) . . ?
C29 C24 C25 118.8(3) . . ?
C29 C24 C23 120.6(2) . . ?
C25 C24 C23 120.6(2) . . ?
C26 C25 C24 120.6(3) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C27 C26 C25 119.7(3) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C28 C27 C26 120.5(3) . . ?
C28 C27 I2A 121.6(3) . . ?
C26 C27 I2A 117.7(3) . . ?
C28 C27 I2B 117.4(3) . . ?
C26 C27 I2B 121.7(3) . . ?
C27 C28 C29 119.6(3) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C28 C29 C24 120.7(3) . . ?
C28 C29 H29 119.6 . . ?
C24 C29 H29 119.6 . . ?
O6 C30 O5 124.7(2) 2_656 . ?
O6 C30 C31 117.5(2) 2_656 . ?
O5 C30 C31 117.73(19) . . ?
C32 C31 C36 119.1(2) . . ?
C32 C31 C30 120.4(2) . . ?
C36 C31 C30 120.5(2) . . ?
C31 C32 C33 120.7(2) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C34 C33 C32 119.2(3) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C33 C34 C35 120.9(3) . . ?
C33 C34 I3B 120.5(2) . . ?
C35 C34 I3B 118.2(2) . . ?
C33 C34 I3A 118.5(2) . . ?
C35 C34 I3A 119.9(2) . . ?
I3B C34 I3A 14.5(2) . . ?
C36 C35 C34 119.8(3) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C35 C36 C31 120.2(2) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C5 N1 C1 118.5(3) . . ?
C5 N1 Ce1 122.47(19) . . ?
C1 N1 Ce1 118.00(19) . . ?
C15 N3 C11 117.9(2) . . ?
C15 N3 Ce1 119.20(17) . . ?
C11 N3 Ce1 122.91(16) . . ?
C16 O1 Ce1 94.69(16) . . ?
C16 O2 Ce1 92.24(14) . . ?
C23 O3 Ce1 92.84(15) . . ?
C23 O4 Ce1 94.37(15) . . ?
C30 O5 Ce1 141.51(16) . . ?
C30 O6 Ce1 163.43(16) 2_656 . ?
HW1A OW1 HW1B 112(6) . . ?
I3B I3A C34 68.1(4) . . ?
I3A I3B C34 97.4(5) . . ?
O6 Ce1 O5 89.69(7) . . ?
O6 Ce1 O1 79.60(8) . . ?
O5 Ce1 O1 76.12(7) . . ?
O6 Ce1 O4 80.82(7) . . ?
O5 Ce1 O4 74.93(7) . . ?
O1 Ce1 O4 144.90(7) . . ?
O6 Ce1 O2 79.40(7) . . ?
O5 Ce1 O2 126.94(6) . . ?
O1 Ce1 O2 50.89(6) . . ?
O4 Ce1 O2 150.09(6) . . ?
O6 Ce1 O3 131.31(7) . . ?
O5 Ce1 O3 78.15(7) . . ?
O1 Ce1 O3 139.26(7) . . ?
O4 Ce1 O3 50.50(6) . . ?
O2 Ce1 O3 143.88(5) . . ?
O6 Ce1 N3 78.05(7) . . ?
O5 Ce1 N3 149.66(7) . . ?
O1 Ce1 N3 127.35(7) . . ?
O4 Ce1 N3 75.75(7) . . ?
O2 Ce1 N3 78.36(7) . . ?
O3 Ce1 N3 89.20(7) . . ?
O6 Ce1 N1 151.70(8) . . ?
O5 Ce1 N1 80.68(7) . . ?
O1 Ce1 N1 72.28(8) . . ?
O4 Ce1 N1 121.34(7) . . ?
O2 Ce1 N1 85.26(7) . . ?
O3 Ce1 N1 72.80(7) . . ?
N3 Ce1 N1 122.00(7) . . ?
O6 Ce1 N2 133.47(6) . . ?
O5 Ce1 N2 136.84(5) . . ?
O1 Ce1 N2 107.11(6) . . ?
O4 Ce1 N2 107.53(6) . . ?
O2 Ce1 N2 71.76(5) . . ?
O3 Ce1 N2 72.54(5) . . ?
N3 Ce1 N2 61.11(6) . . ?
N1 Ce1 N2 60.90(6) . . ?
O6 Ce1 C16 77.37(7) . . ?
O5 Ce1 C16 101.49(7) . . ?
O1 Ce1 C16 25.47(6) . . ?
O4 Ce1 C16 157.93(6) . . ?
O2 Ce1 C16 25.45(6) . . ?
O3 Ce1 C16 151.08(6) . . ?
N3 Ce1 C16 102.69(7) . . ?
N1 Ce1 C16 78.58(8) . . ?
N2 Ce1 C16 90.09(6) . . ?
O6 Ce1 C23 106.04(7) . . ?
O5 Ce1 C23 72.19(7) . . ?
O1 Ce1 C23 147.70(7) . . ?
O4 Ce1 C23 25.45(6) . . ?
O2 Ce1 C23 160.64(6) . . ?
O3 Ce1 C23 25.36(6) . . ?
N3 Ce1 C23 84.55(7) . . ?
N1 Ce1 C23 96.30(8) . . ?
N2 Ce1 C23 92.07(6) . . ?
C16 Ce1 C23 172.58(7) . . ?

_refine_diff_density_max         0.764
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.069

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_2
_database_code_depnum_ccdc_archive 'CCDC 1514979'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 Ce2 I6 N6 O14'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          293(2)

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2264.82

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   14.2470(11)
_cell_length_b                   25.523(2)
_cell_length_c                   10.3649(8)
_cell_angle_alpha                90
_cell_angle_beta                 93.3000(9)
_cell_angle_gamma                90
_cell_volume                     3762.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    38495
_cell_measurement_theta_min      4.995
_cell_measurement_theta_max      50.210
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_F_000             2140
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.029
_exptl_absorpt_coefficient_mu    3.721
_shelx_estimated_absorpt_T_min   0.559
_shelx_estimated_absorpt_T_max   0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6176
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37972
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.432
_diffrn_reflns_theta_max         27.942
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8867
_reflns_number_gt                6145
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0419P)²+9.6207P] 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         8867
_refine_ls_number_parameters     459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.1151
_refine_ls_wR_factor_gt          0.0999
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3152(5) 0.6003(2) -0.2710(6) 0.0660(16) Uani 1 1 d . . . . .
H1 H 0.3311 0.5652 -0.2600 0.079 Uiso 1 1 calc R U . . .
C2 C 0.2513(5) 0.6128(3) -0.3698(7) 0.0755(19) Uani 1 1 d . . . . .
H2 H 0.2267 0.5876 -0.4269 0.091 Uiso 1 1 calc R U . . .
C3 C 0.2255(6) 0.6642(3) -0.3803(8) 0.096(3) Uani 1 1 d . . . . .
H3 H 0.1807 0.6746 -0.4441 0.115 Uiso 1 1 calc R U . . .
C4 C 0.2657(6) 0.7001(3) -0.2966(7) 0.087(2) Uani 1 1 d . . . . .
H4 H 0.2473 0.7351 -0.3024 0.104 Uiso 1 1 calc R U . . .
C5 C 0.3331(4) 0.6852(2) -0.2041(5) 0.0497(12) Uani 1 1 d . . . . .
C6 C 0.3846(4) 0.72358(19) -0.1181(5) 0.0472(12) Uani 1 1 d . . . . .
C7 C 0.3736(5) 0.7771(2) -0.1383(6) 0.0672(17) Uani 1 1 d . . . . .
H7 H 0.3329 0.7891 -0.2051 0.081 Uiso 1 1 calc R U . . .
C8 C 0.4222(6) 0.8122(2) -0.0605(7) 0.080(2) Uani 1 1 d . . . . .
H8 H 0.4158 0.8480 -0.0744 0.096 Uiso 1 1 calc R U . . .
C9 C 0.4799(5) 0.7936(2) 0.0372(6) 0.0654(17) Uani 1 1 d . . . . .
H9 H 0.5122 0.8167 0.0930 0.079 Uiso 1 1 calc R U . . .
C10 C 0.4909(4) 0.73971(18) 0.0542(5) 0.0464(12) Uani 1 1 d . . . . .
C11 C 0.5560(4) 0.71845(18) 0.1577(5) 0.0463(12) Uani 1 1 d . . . . .
C12 C 0.6076(4) 0.7505(2) 0.2438(6) 0.0587(15) Uani 1 1 d . . . . .
H12 H 0.6029 0.7868 0.2365 0.070 Uiso 1 1 calc R U . . .
C13 C 0.6648(5) 0.7289(3) 0.3385(7) 0.0726(18) Uani 1 1 d . . . . .
H13 H 0.6986 0.7503 0.3971 0.087 Uiso 1 1 calc R U . . .
C14 C 0.6725(5) 0.6758(3) 0.3475(6) 0.0721(18) Uani 1 1 d . . . . .
H14 H 0.7122 0.6603 0.4107 0.086 Uiso 1 1 calc R U . . .
C15 C 0.6201(5) 0.6460(2) 0.2608(6) 0.0651(16) Uani 1 1 d . . . . .
H15 H 0.6250 0.6097 0.2676 0.078 Uiso 1 1 calc R U . . .
C16 C 0.5734(4) 0.58970(19) -0.2220(5) 0.0496(13) Uani 1 1 d . . . . .
C17 C 0.6413(4) 0.58130(19) -0.3255(5) 0.0488(12) Uani 1 1 d . . . . .
C18 C 0.7280(4) 0.6054(2) -0.3174(6) 0.0589(14) Uani 1 1 d . . . . .
H18 H 0.7420 0.6297 -0.2523 0.071 Uiso 1 1 calc R U . . .
C19 C 0.7946(5) 0.5938(3) -0.4051(7) 0.0728(18) Uani 1 1 d . . . . .
H19 H 0.8539 0.6090 -0.3980 0.087 Uiso 1 1 calc R U . . .
C20 C 0.7705(6) 0.5588(3) -0.5040(6) 0.0735(19) Uani 1 1 d . . . . .
C21 C 0.6836(6) 0.5361(3) -0.5157(7) 0.084(2) Uani 1 1 d . . . . .
H21 H 0.6680 0.5136 -0.5841 0.101 Uiso 1 1 calc R U . . .
C22 C 0.6195(5) 0.5469(2) -0.4257(6) 0.0684(17) Uani 1 1 d . . . . .
H22 H 0.5608 0.5309 -0.4321 0.082 Uiso 1 1 calc R U . . .
C23 C 0.2655(4) 0.6238(2) 0.1944(6) 0.0501(13) Uani 1 1 d . . . . .
C24 C 0.1732(4) 0.6527(2) 0.1803(6) 0.0522(13) Uani 1 1 d . . . . .
C25 C 0.1543(4) 0.6865(2) 0.0779(6) 0.0628(15) Uani 1 1 d . . . . .
H25 H 0.1980 0.6903 0.0154 0.075 Uiso 1 1 calc R U . . .
C26 C 0.0720(5) 0.7148(3) 0.0667(7) 0.0749(18) Uani 1 1 d . . . . .
H26 H 0.0600 0.7371 -0.0033 0.090 Uiso 1 1 calc R U . . .
C27 C 0.0077(5) 0.7100(3) 0.1596(8) 0.078(2) Uani 1 1 d . . . . .
C28 C 0.0235(5) 0.6760(3) 0.2602(8) 0.088(2) Uani 1 1 d . . . . .
H28 H -0.0210 0.6722 0.3217 0.106 Uiso 1 1 calc R U . . .
C29 C 0.1062(4) 0.6471(3) 0.2704(7) 0.0695(17) Uani 1 1 d . . . . .
H29 H 0.1166 0.6238 0.3387 0.083 Uiso 1 1 calc R U . . .
C30 C 0.3364(4) 0.48080(19) -0.0311(5) 0.0452(11) Uani 1 1 d . . . . .
C31 C 0.2420(4) 0.46322(19) 0.0091(5) 0.0476(12) Uani 1 1 d . . . . .
C32 C 0.1855(4) 0.4972(2) 0.0726(7) 0.077(2) Uani 1 1 d . . . . .
H32 H 0.2047 0.5318 0.0855 0.092 Uiso 1 1 calc R U . . .
C33 C 0.1017(5) 0.4812(3) 0.1171(9) 0.094(3) Uani 1 1 d . . . . .
H33 H 0.0646 0.5047 0.1604 0.113 Uiso 1 1 calc R U . . .
C34 C 0.0724(4) 0.4307(3) 0.0979(7) 0.0694(18) Uani 1 1 d . . . . .
C35 C 0.1260(4) 0.3960(2) 0.0340(6) 0.0657(16) Uani 1 1 d . . . . .
H35 H 0.1055 0.3617 0.0200 0.079 Uiso 1 1 calc R U . . .
C36 C 0.2114(4) 0.4122(2) -0.0099(6) 0.0559(14) Uani 1 1 d . . . . .
H36 H 0.2484 0.3886 -0.0526 0.067 Uiso 1 1 calc R U . . .
N1 N 0.3564(3) 0.63489(17) -0.1892(4) 0.0533(11) Uani 1 1 d . . . . .
N2 N 0.4437(3) 0.70485(15) -0.0232(4) 0.0431(9) Uani 1 1 d . . . . .
N3 N 0.5623(3) 0.66572(15) 0.1667(4) 0.0507(11) Uani 1 1 d . . . . .
O4 O 0.5791(3) 0.63120(13) -0.1557(4) 0.0567(10) Uani 1 1 d . . . . .
O3 O 0.5151(3) 0.55384(13) -0.1997(4) 0.0559(9) Uani 1 1 d . . . . .
O1 O 0.3240(3) 0.63398(14) 0.1099(4) 0.0584(10) Uani 1 1 d . . . . .
O2 O 0.2793(3) 0.59352(16) 0.2865(4) 0.0644(11) Uani 1 1 d . . . . .
O5 O 0.3545(3) 0.52876(13) -0.0244(4) 0.0599(10) Uani 1 1 d . . . . .
O6 O 0.6079(3) 0.55291(14) 0.0685(4) 0.0560(9) Uani 1 1 d . . . . .
OW1 O 0.4528(3) 0.55649(17) 0.2334(4) 0.0583(11) Uani 1 1 d . . . . .
I1 I 0.86962(6) 0.54030(3) -0.63863(7) 0.1439(3) Uani 1 1 d . . . . .
I2 I -0.11644(4) 0.75433(3) 0.14736(9) 0.1332(3) Uani 1 1 d . . . . .
I3 I -0.05116(4) 0.40470(2) 0.17877(7) 0.1079(2) Uani 1 1 d . . . . .
Ce1 Ce 0.46334(2) 0.59993(2) 0.01135(3) 0.04043(9) Uani 1 1 d . . . . .
HW1A H 0.455(5) 0.530(3) 0.211(6) 0.06(2) Uiso 1 1 d . . . . .
HW1B H 0.385(8) 0.561(5) 0.258(11) 0.18(5) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.337(7) . ?
C1 C2 1.368(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.363(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.367(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.371(8) . ?
C4 H4 0.9300 . ?
C5 N1 1.333(6) . ?
C5 C6 1.489(8) . ?
C6 N2 1.345(6) . ?
C6 C7 1.389(7) . ?
C7 C8 1.366(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.353(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.393(7) . ?
C9 H9 0.9300 . ?
C10 N2 1.351(7) . ?
C10 C11 1.480(8) . ?
C11 N3 1.352(6) . ?
C11 C12 1.390(7) . ?
C12 C13 1.356(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.364(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.365(8) . ?
C14 H14 0.9300 . ?
C15 N3 1.339(7) . ?
C15 H15 0.9300 . ?
C16 O4 1.262(6) . ?
C16 O3 1.266(6) . ?
C16 C17 1.501(7) . ?
C16 Ce1 2.969(5) . ?
C17 C18 1.378(8) . ?
C17 C22 1.381(8) . ?
C18 C19 1.382(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.388(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.365(10) . ?
C20 I1 2.096(6) . ?
C21 C22 1.370(9) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O2 1.235(7) . ?
C23 O1 1.270(6) . ?
C23 C24 1.507(8) . ?
C24 C29 1.381(8) . ?
C24 C25 1.383(8) . ?
C25 C26 1.376(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.372(10) . ?
C26 H26 0.9300 . ?
C27 C28 1.365(11) . ?
C27 I2 2.098(7) . ?
C28 C29 1.389(10) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 O6 1.247(6) 3_665 ?
C30 O5 1.252(6) . ?
C30 C31 1.499(7) . ?
C31 C32 1.378(7) . ?
C31 C36 1.383(7) . ?
C32 C33 1.367(9) . ?
C32 H32 0.9300 . ?
C33 C34 1.368(9) . ?
C33 H33 0.9300 . ?
C34 C35 1.365(8) . ?
C34 I3 2.101(6) . ?
C35 C36 1.386(8) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N1 Ce1 2.659(5) . ?
N2 Ce1 2.714(4) . ?
N3 Ce1 2.671(4) . ?
O4 Ce1 2.585(4) . ?
O3 Ce1 2.627(4) . ?
O1 Ce1 2.444(4) . ?
O5 Ce1 2.403(4) . ?
O6 C30 1.247(6) 3_665 ?
O6 Ce1 2.427(4) . ?
OW1 Ce1 2.567(4) . ?
OW1 HW1A 0.73(6) . ?
OW1 HW1B 1.01(12) . ?

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
N1 C1 C2 124.7(6) . . ?
N1 C1 H1 117.6 . . ?
C2 C1 H1 117.6 . . ?
C3 C2 C1 116.7(7) . . ?
C3 C2 H2 121.6 . . ?
C1 C2 H2 121.6 . . ?
C2 C3 C4 119.5(7) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C3 C4 C5 120.5(7) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
N1 C5 C4 120.6(6) . . ?
N1 C5 C6 116.9(5) . . ?
C4 C5 C6 122.4(5) . . ?
N2 C6 C7 121.3(5) . . ?
N2 C6 C5 118.0(4) . . ?
C7 C6 C5 120.6(5) . . ?
C8 C7 C6 120.4(6) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C9 C8 C7 118.5(5) . . ?
C9 C8 H8 120.8 . . ?
C7 C8 H8 120.8 . . ?
C8 C9 C10 120.0(6) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
N2 C10 C9 121.7(5) . . ?
N2 C10 C11 117.3(4) . . ?
C9 C10 C11 121.0(5) . . ?
N3 C11 C12 120.8(5) . . ?
N3 C11 C10 116.8(5) . . ?
C12 C11 C10 122.4(5) . . ?
C13 C12 C11 119.9(5) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 119.7(6) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C13 C14 C15 118.1(6) . . ?
C13 C14 H14 121.0 . . ?
C15 C14 H14 121.0 . . ?
N3 C15 C14 124.0(6) . . ?
N3 C15 H15 118.0 . . ?
C14 C15 H15 118.0 . . ?
O4 C16 O3 122.0(5) . . ?
O4 C16 C17 119.0(5) . . ?
O3 C16 C17 118.9(5) . . ?
O4 C16 Ce1 60.2(3) . . ?
O3 C16 Ce1 62.1(3) . . ?
C17 C16 Ce1 170.9(4) . . ?
C18 C17 C22 119.4(5) . . ?
C18 C17 C16 120.3(5) . . ?
C22 C17 C16 120.2(5) . . ?
C17 C18 C19 120.7(6) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C18 C19 C20 118.3(7) . . ?
C18 C19 H19 120.9 . . ?
C20 C19 H19 120.9 . . ?
C21 C20 C19 121.5(6) . . ?
C21 C20 I1 119.2(5) . . ?
C19 C20 I1 119.3(6) . . ?
C20 C21 C22 119.4(6) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C21 C22 C17 120.7(6) . . ?
C21 C22 H22 119.7 . . ?
C17 C22 H22 119.7 . . ?
O2 C23 O1 125.4(5) . . ?
O2 C23 C24 118.7(5) . . ?
O1 C23 C24 115.9(5) . . ?
C29 C24 C25 118.1(6) . . ?
C29 C24 C23 121.1(6) . . ?
C25 C24 C23 120.7(5) . . ?
C26 C25 C24 121.3(6) . . ?
C26 C25 H25 119.3 . . ?
C24 C25 H25 119.3 . . ?
C27 C26 C25 119.6(7) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C28 C27 C26 120.4(7) . . ?
C28 C27 I2 119.4(6) . . ?
C26 C27 I2 120.2(6) . . ?
C27 C28 C29 119.8(7) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C24 C29 C28 120.7(7) . . ?
C24 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
O6 C30 O5 124.0(5) 3_665 . ?
O6 C30 C31 118.5(4) 3_665 . ?
O5 C30 C31 117.5(5) . . ?
C32 C31 C36 118.2(5) . . ?
C32 C31 C30 120.2(5) . . ?
C36 C31 C30 121.5(5) . . ?
C33 C32 C31 121.3(6) . . ?
C33 C32 H32 119.4 . . ?
C31 C32 H32 119.4 . . ?
C32 C33 C34 119.8(6) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C35 C34 C33 120.6(6) . . ?
C35 C34 I3 119.6(5) . . ?
C33 C34 I3 119.6(5) . . ?
C34 C35 C36 119.4(5) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.3 . . ?
C31 C36 C35 120.7(5) . . ?
C31 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
C5 N1 C1 117.7(5) . . ?
C5 N1 Ce1 122.8(4) . . ?
C1 N1 Ce1 119.0(4) . . ?
C6 N2 C10 118.0(4) . . ?
C6 N2 Ce1 120.2(3) . . ?
C10 N2 Ce1 121.8(3) . . ?
C15 N3 C11 117.4(5) . . ?
C15 N3 Ce1 118.9(3) . . ?
C11 N3 Ce1 123.6(4) . . ?
C16 O4 Ce1 94.7(3) . . ?
C16 O3 Ce1 92.7(3) . . ?
C23 O1 Ce1 142.8(4) . . ?
C30 O5 Ce1 151.2(4) . . ?
C30 O6 Ce1 144.2(4) 3_665 . ?
Ce1 OW1 HW1A 96(5) . . ?
Ce1 OW1 HW1B 106(6) . . ?
HW1A OW1 HW1B 104(8) . . ?
O5 Ce1 O6 101.24(12) . . ?
O5 Ce1 O1 78.51(13) . . ?
O6 Ce1 O1 140.52(14) . . ?
O5 Ce1 OW1 75.02(14) . . ?
O6 Ce1 OW1 70.12(14) . . ?
O1 Ce1 OW1 71.83(14) . . ?
O5 Ce1 O4 124.11(13) . . ?
O6 Ce1 O4 75.60(13) . . ?
O1 Ce1 O4 137.30(12) . . ?
OW1 Ce1 O4 143.73(14) . . ?
O5 Ce1 O3 75.10(13) . . ?
O6 Ce1 O3 72.96(13) . . ?
O1 Ce1 O3 141.37(13) . . ?
OW1 Ce1 O3 125.95(13) . . ?
O4 Ce1 O3 50.19(11) . . ?
O5 Ce1 N1 78.32(14) . . ?
O6 Ce1 N1 142.79(14) . . ?
O1 Ce1 N1 76.41(14) . . ?
OW1 Ce1 N1 141.77(15) . . ?
O4 Ce1 N1 74.43(14) . . ?
O3 Ce1 N1 71.03(13) . . ?
O5 Ce1 N3 151.82(14) . . ?
O6 Ce1 N3 75.69(13) . . ?
O1 Ce1 N3 86.43(13) . . ?
OW1 Ce1 N3 77.71(14) . . ?
O4 Ce1 N3 82.81(13) . . ?
O3 Ce1 N3 128.28(13) . . ?
N1 Ce1 N3 121.24(13) . . ?
O5 Ce1 N2 131.66(13) . . ?
O6 Ce1 N2 126.84(13) . . ?
O1 Ce1 N2 67.93(12) . . ?
OW1 Ce1 N2 122.25(13) . . ?
O4 Ce1 N2 70.84(11) . . ?
O3 Ce1 N2 111.32(11) . . ?
N1 Ce1 N2 61.04(13) . . ?
N3 Ce1 N2 60.40(13) . . ?
O5 Ce1 C16 100.04(14) . . ?
O6 Ce1 C16 71.03(14) . . ?
O1 Ce1 C16 148.39(14) . . ?
OW1 Ce1 C16 138.88(15) . . ?
O4 Ce1 C16 25.07(12) . . ?
O3 Ce1 C16 25.21(12) . . ?
N1 Ce1 C16 72.44(14) . . ?
N3 Ce1 C16 105.13(15) . . ?
N2 Ce1 C16 91.97(12) . . ?

_refine_diff_density_max         1.784
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.103

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_11Prime
_database_code_depnum_ccdc_archive 'CCDC 1514990'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H38 Er2 I4 N6 O12'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1877.08

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'
I I -0.4742 1.8119 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   10.0196(4)
_cell_length_b                   10.4670(4)
_cell_length_c                   15.3792(6)
_cell_angle_alpha                85.2250(10)
_cell_angle_beta                 75.107(2)
_cell_angle_gamma                75.1700(10)
_cell_volume                     1506.53(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    22508
_cell_measurement_theta_min      4.528
_cell_measurement_theta_max      48.189

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_F_000             884
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.166
_exptl_absorpt_coefficient_mu    4.882
_shelx_estimated_absorpt_T_min   0.232
_shelx_estimated_absorpt_T_max   0.498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5599
_exptl_absorpt_correction_T_max  0.7491
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focused sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22508
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.370
_diffrn_reflns_theta_max         30.427
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8438
_reflns_number_gt                6853
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  WinGX
_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)+(0.0378P)²+0.2412P] 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         8438
_refine_ls_number_parameters     399
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.0886
_refine_ls_wR_factor_gt          0.0829
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_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 0.24787(2) 0.17808(2) 0.11659(2) 0.03222(6) Uani 1 1 d . . . . .
I1 I 0.02159(6) 0.80025(4) 0.53701(3) 0.09179(16) Uani 1 1 d . . . . .
O5 O 0.4957(3) 0.1269(3) 0.06764(19) 0.0380(6) Uani 1 1 d . . . . .
O1 O 0.0792(3) 0.3502(3) 0.2052(2) 0.0441(7) Uani 1 1 d . . . . .
O2 O 0.3021(3) 0.3609(3) 0.1747(2) 0.0492(8) Uani 1 1 d . . . . .
N2 N 0.0575(3) 0.2385(3) 0.0299(2) 0.0329(7) Uani 1 1 d . . . . .
N1 N 0.0359(4) 0.0776(3) 0.1768(2) 0.0398(8) Uani 1 1 d . . . . .
N3 N 0.2922(4) 0.3339(3) -0.0157(2) 0.0394(8) Uani 1 1 d . . . . .
C17 C 0.1374(4) 0.4999(4) 0.2896(3) 0.0370(9) Uani 1 1 d . . . . .
C10 C 0.0739(4) 0.3138(4) -0.0452(3) 0.0371(9) Uani 1 1 d . . . . .
C20 C 0.0694(6) 0.6756(4) 0.4283(3) 0.0498(11) Uani 1 1 d . . . . .
C16 C 0.1757(5) 0.3990(4) 0.2191(3) 0.0387(9) Uani 1 1 d . . . . .
C11 C 0.1952(4) 0.3783(4) -0.0644(3) 0.0396(9) Uani 1 1 d . . . . .
C1 C 0.0189(5) 0.0086(5) 0.2546(3) 0.0549(12) Uani 1 1 d . . . . .
H1 H 0.0919 -0.0090 0.2843 0.066 Uiso 1 1 calc R U . . .
C5 C -0.0706(4) 0.1021(4) 0.1343(3) 0.0403(9) Uani 1 1 d . . . . .
C22 C 0.2351(5) 0.5644(5) 0.3016(3) 0.0491(11) Uani 1 1 d . . . . .
H22 H 0.3253 0.5479 0.2626 0.059 Uiso 1 1 calc R U . . .
C19 C -0.0312(6) 0.6158(5) 0.4164(4) 0.0644(15) Uani 1 1 d . . . . .
H19 H -0.1217 0.6340 0.4550 0.077 Uiso 1 1 calc R U . . .
C21 C 0.2020(6) 0.6528(5) 0.3701(3) 0.0543(12) Uani 1 1 d . . . . .
H21 H 0.2687 0.6963 0.3768 0.065 Uiso 1 1 calc R U . . .
C7 C -0.1429(5) 0.1908(5) -0.0064(3) 0.0499(11) Uani 1 1 d . . . . .
H7 H -0.2165 0.1479 0.0083 0.060 Uiso 1 1 calc R U . . .
C15 C 0.4073(5) 0.3842(5) -0.0358(3) 0.0493(11) Uani 1 1 d . . . . .
H15 H 0.4772 0.3517 -0.0044 0.059 Uiso 1 1 calc R U . . .
C14 C 0.4272(6) 0.4816(5) -0.1007(4) 0.0585(13) Uani 1 1 d . . . . .
H14 H 0.5088 0.5135 -0.1127 0.070 Uiso 1 1 calc R U . . .
C4 C -0.1922(6) 0.0560(6) 0.1695(4) 0.0674(16) Uani 1 1 d . . . . .
H4 H -0.2639 0.0716 0.1389 0.081 Uiso 1 1 calc R U . . .
C6 C -0.0513(4) 0.1792(4) 0.0491(3) 0.0360(9) Uani 1 1 d . . . . .
C9 C -0.0139(5) 0.3288(5) -0.1032(3) 0.0555(13) Uani 1 1 d . . . . .
H9 H 0.0009 0.3806 -0.1553 0.067 Uiso 1 1 calc R U . . .
C18 C 0.0013(5) 0.5293(5) 0.3475(3) 0.0506(12) Uani 1 1 d . . . . .
H18 H -0.0677 0.4899 0.3392 0.061 Uiso 1 1 calc R U . . .
C8 C -0.1231(6) 0.2663(6) -0.0831(4) 0.0635(14) Uani 1 1 d . . . . .
H8 H -0.1833 0.2753 -0.1215 0.076 Uiso 1 1 calc R U . . .
C24 C 0.4207(6) -0.0987(5) 0.3126(3) 0.0570(13) Uani 1 1 d D . . . .
C2 C -0.1003(6) -0.0377(6) 0.2932(4) 0.0697(16) Uani 1 1 d . . . . .
H2 H -0.1081 -0.0847 0.3475 0.084 Uiso 1 1 calc R U . . .
C12 C 0.2066(5) 0.4784(5) -0.1291(3) 0.0518(12) Uani 1 1 d . . . . .
H12 H 0.1358 0.5101 -0.1600 0.062 Uiso 1 1 calc R U . . .
C13 C 0.3247(6) 0.5301(5) -0.1469(3) 0.0583(13) Uani 1 1 d . . . . .
H13 H 0.3344 0.5972 -0.1899 0.070 Uiso 1 1 calc R U . . .
O6 O 0.3203(3) 0.0303(3) 0.0007(2) 0.0414(7) Uani 1 1 d . . . . .
C30 C 0.5501(4) 0.0287(4) 0.0196(3) 0.0325(8) Uani 1 1 d . . . . .
O3 O 0.2947(5) 0.0974(6) 0.2516(4) 0.1069(19) Uani 1 1 d . . . . .
C29 C 0.3748(6) -0.0436(6) 0.3964(4) 0.0725(16) Uani 1 1 d . . . . .
H29 H 0.3153 0.0410 0.4041 0.087 Uiso 1 1 calc R U . . .
C23 C 0.3580(8) -0.0204(9) 0.2378(4) 0.086(2) Uani 1 1 d D . . . .
C25 C 0.5128(7) -0.2207(7) 0.3025(5) 0.089(2) Uani 1 1 d . . . . .
H25 H 0.5463 -0.2586 0.2459 0.107 Uiso 1 1 calc R U . . .
C3 C -0.2051(7) -0.0128(7) 0.2496(4) 0.086(2) Uani 1 1 d . . . . .
H3 H -0.2870 -0.0425 0.2742 0.103 Uiso 1 1 calc R U . . .
C28 C 0.4165(8) -0.1133(10) 0.4695(5) 0.105(3) Uani 1 1 d . . . . .
H28 H 0.3833 -0.0765 0.5264 0.125 Uiso 1 1 calc R U . . .
C27 C 0.5048(8) -0.2337(10) 0.4578(7) 0.112(4) Uani 1 1 d . . . . .
C26 C 0.5568(7) -0.2879(7) 0.3743(8) 0.117(4) Uani 1 1 d . . . . .
H26 H 0.6216 -0.3700 0.3665 0.141 Uiso 1 1 calc R U . . .
I2A I 0.5804(3) -0.3785(6) 0.5465(4) 0.1289(18) Uani 0.503(8) 1 d . . P A 1
I2B I 0.5487(3) -0.2939(7) 0.5914(3) 0.1408(14) Uani 0.497(8) 1 d . . P A 2
O4A O 0.3510(8) -0.0568(10) 0.1717(4) 0.054(3) Uani 0.61(2) 1 d . . P B 1
O4B O 0.439(3) -0.1316(19) 0.1650(9) 0.112(8) Uani 0.39(2) 1 d . . P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O3 2.292(4) . ?
Er1 O6 2.305(3) . ?
Er1 O5 2.334(3) . ?
Er1 O1 2.372(3) . ?
Er1 O2 2.413(3) . ?
Er1 N3 2.520(3) . ?
Er1 N2 2.524(3) . ?
Er1 N1 2.539(3) . ?
Er1 O4A 2.576(10) . ?
Er1 C16 2.742(4) . ?
Er1 C23 2.872(7) . ?
I1 C20 2.088(4) . ?
O5 C30 1.237(4) . ?
O1 C16 1.272(5) . ?
O2 C16 1.253(5) . ?
N2 C10 1.341(5) . ?
N2 C6 1.345(5) . ?
N1 C1 1.340(6) . ?
N1 C5 1.349(5) . ?
N3 C15 1.343(5) . ?
N3 C11 1.344(5) . ?
C17 C22 1.378(6) . ?
C17 C18 1.397(6) . ?
C17 C16 1.486(6) . ?
C10 C9 1.380(6) . ?
C10 C11 1.490(6) . ?
C20 C19 1.371(7) . ?
C20 C21 1.373(7) . ?
C11 C12 1.390(6) . ?
C1 C2 1.378(7) . ?
C1 H1 0.9300 . ?
C5 C4 1.389(6) . ?
C5 C6 1.477(6) . ?
C22 C21 1.379(6) . ?
C22 H22 0.9300 . ?
C19 C18 1.371(7) . ?
C19 H19 0.9300 . ?
C21 H21 0.9300 . ?
C7 C8 1.363(7) . ?
C7 C6 1.384(6) . ?
C7 H7 0.9300 . ?
C15 C14 1.382(7) . ?
C15 H15 0.9300 . ?
C14 C13 1.366(7) . ?
C14 H14 0.9300 . ?
C4 C3 1.368(8) . ?
C4 H4 0.9300 . ?
C9 C8 1.371(7) . ?
C9 H9 0.9300 . ?
C18 H18 0.9300 . ?
C8 H8 0.9300 . ?
C24 C25 1.364(8) . ?
C24 C29 1.375(8) . ?
C24 C23 1.530(7) . ?
C2 C3 1.346(8) . ?
C2 H2 0.9300 . ?
C12 C13 1.380(7) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
O6 C30 1.257(4) 2_655 ?
C30 O6 1.257(4) 2_655 ?
C30 C30 1.554(7) 2_655 ?
O3 C23 1.242(9) . ?
C29 C28 1.386(8) . ?
C29 H29 0.9300 . ?
C23 O4A 1.140(8) . ?
C23 O4B 1.59(2) . ?
C25 C26 1.369(11) . ?
C25 H25 0.9300 . ?
C3 H3 0.9300 . ?
C28 C27 1.338(12) . ?
C28 H28 0.9300 . ?
C27 C26 1.366(12) . ?
C27 I2A 2.081(7) . ?
C27 I2B 2.218(8) . ?
C26 H26 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 Er1 O6 116.62(19) . . ?
O3 Er1 O5 83.04(14) . . ?
O6 Er1 O5 70.60(9) . . ?
O3 Er1 O1 83.91(18) . . ?
O6 Er1 O1 152.56(10) . . ?
O5 Er1 O1 133.17(10) . . ?
O3 Er1 O2 76.69(18) . . ?
O6 Er1 O2 143.98(10) . . ?
O5 Er1 O2 78.74(9) . . ?
O1 Er1 O2 54.50(10) . . ?
O3 Er1 N3 147.63(16) . . ?
O6 Er1 N3 80.19(11) . . ?
O5 Er1 N3 76.82(11) . . ?
O1 Er1 N3 91.60(11) . . ?
O2 Er1 N3 74.71(11) . . ?
O3 Er1 N2 144.13(14) . . ?
O6 Er1 N2 74.14(10) . . ?
O5 Er1 N2 131.10(10) . . ?
O1 Er1 N2 78.69(10) . . ?
O2 Er1 N2 115.85(10) . . ?
N3 Er1 N2 64.57(11) . . ?
O3 Er1 N1 81.32(14) . . ?
O6 Er1 N1 87.41(11) . . ?
O5 Er1 N1 143.44(11) . . ?
O1 Er1 N1 77.49(11) . . ?
O2 Er1 N1 128.53(11) . . ?
N3 Er1 N1 129.02(11) . . ?
N2 Er1 N1 64.47(11) . . ?
O3 Er1 O4A 47.7(2) . . ?
O6 Er1 O4A 69.09(17) . . ?
O5 Er1 O4A 70.59(16) . . ?
O1 Er1 O4A 126.57(17) . . ?
O2 Er1 O4A 117.98(16) . . ?
N3 Er1 O4A 140.87(17) . . ?
N2 Er1 O4A 125.12(16) . . ?
N1 Er1 O4A 74.43(16) . . ?
O3 Er1 C16 76.10(19) . . ?
O6 Er1 C16 165.34(12) . . ?
O5 Er1 C16 105.59(11) . . ?
O1 Er1 C16 27.60(11) . . ?
O2 Er1 C16 27.20(11) . . ?
N3 Er1 C16 85.16(12) . . ?
N2 Er1 C16 100.04(11) . . ?
N1 Er1 C16 102.38(12) . . ?
O4A Er1 C16 123.81(18) . . ?
O3 Er1 C23 24.7(2) . . ?
O6 Er1 C23 91.90(19) . . ?
O5 Er1 C23 72.62(16) . . ?
O1 Er1 C23 107.42(19) . . ?
O2 Er1 C23 96.65(17) . . ?
N3 Er1 C23 149.34(15) . . ?
N2 Er1 C23 141.55(14) . . ?
N1 Er1 C23 79.56(14) . . ?
O4A Er1 C23 23.4(2) . . ?
C16 Er1 C23 100.52(19) . . ?
C30 O5 Er1 115.7(2) . . ?
C16 O1 Er1 92.6(2) . . ?
C16 O2 Er1 91.2(3) . . ?
C10 N2 C6 117.8(3) . . ?
C10 N2 Er1 120.7(3) . . ?
C6 N2 Er1 120.7(3) . . ?
C1 N1 C5 117.5(4) . . ?
C1 N1 Er1 122.2(3) . . ?
C5 N1 Er1 120.1(3) . . ?
C15 N3 C11 117.4(4) . . ?
C15 N3 Er1 121.5(3) . . ?
C11 N3 Er1 120.9(3) . . ?
C22 C17 C18 118.1(4) . . ?
C22 C17 C16 121.4(4) . . ?
C18 C17 C16 120.5(4) . . ?
N2 C10 C9 122.2(4) . . ?
N2 C10 C11 116.5(4) . . ?
C9 C10 C11 121.3(4) . . ?
C19 C20 C21 120.6(4) . . ?
C19 C20 I1 119.7(4) . . ?
C21 C20 I1 119.7(4) . . ?
O2 C16 O1 120.4(4) . . ?
O2 C16 C17 120.4(4) . . ?
O1 C16 C17 119.2(4) . . ?
O2 C16 Er1 61.6(2) . . ?
O1 C16 Er1 59.8(2) . . ?
C17 C16 Er1 168.8(3) . . ?
N3 C11 C12 122.3(4) . . ?
N3 C11 C10 116.2(4) . . ?
C12 C11 C10 121.6(4) . . ?
N1 C1 C2 123.8(5) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
N1 C5 C4 121.1(4) . . ?
N1 C5 C6 117.0(4) . . ?
C4 C5 C6 121.9(4) . . ?
C17 C22 C21 121.5(4) . . ?
C17 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C20 C19 C18 120.1(5) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C21 C22 119.2(5) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
C8 C7 C6 118.8(4) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
N3 C15 C14 123.4(5) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
C13 C14 C15 118.6(5) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
C3 C4 C5 119.1(5) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N2 C6 C7 122.5(4) . . ?
N2 C6 C5 116.5(3) . . ?
C7 C6 C5 121.0(4) . . ?
C8 C9 C10 119.2(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C19 C18 C17 120.5(5) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C7 C8 C9 119.5(4) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C25 C24 C29 118.5(6) . . ?
C25 C24 C23 124.6(7) . . ?
C29 C24 C23 116.8(6) . . ?
C3 C2 C1 117.8(5) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C13 C12 C11 118.9(5) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C14 C13 C12 119.3(5) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C30 O6 Er1 116.8(2) 2_655 . ?
O5 C30 O6 126.3(3) . 2_655 ?
O5 C30 C30 117.6(4) . 2_655 ?
O6 C30 C30 116.1(4) 2_655 2_655 ?
C23 O3 Er1 104.8(5) . . ?
C24 C29 C28 120.5(6) . . ?
C24 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
O4A C23 O3 112.9(9) . . ?
O4A C23 C24 129.1(9) . . ?
O3 C23 C24 117.7(6) . . ?
O3 C23 O4B 146.7(8) . . ?
C24 C23 O4B 93.6(9) . . ?
O4A C23 Er1 63.6(6) . . ?
O3 C23 Er1 50.5(4) . . ?
C24 C23 Er1 166.7(5) . . ?
O4B C23 Er1 97.0(7) . . ?
C24 C25 C26 120.9(7) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C2 C3 C4 120.6(5) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C27 C28 C29 119.6(7) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C28 C27 C26 120.9(7) . . ?
C28 C27 I2A 133.1(8) . . ?
C26 C27 I2A 105.9(8) . . ?
C28 C27 I2B 105.0(8) . . ?
C26 C27 I2B 133.8(7) . . ?
C27 C26 C25 119.5(7) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C23 O4A Er1 93.1(7) . . ?

_refine_diff_density_max         1.180
_refine_diff_density_min         -1.513
_refine_diff_density_rms         0.120

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_13
_database_code_depnum_ccdc_archive 'CCDC 1514993'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 I6 N6 O14 Yb2'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293
_chemical_formula_weight         2330.66

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'
I I -0.4742 1.8119 '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      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                   11.1925(5)
_cell_length_b                   12.7725(5)
_cell_length_c                   14.4360(6)
_cell_angle_alpha                68.862(2)
_cell_angle_beta                 88.3120(10)
_cell_angle_gamma                72.6240(10)
_cell_volume                     1829.91(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    27131
_cell_measurement_theta_min      4.673
_cell_measurement_theta_max      46.410

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.115
_exptl_crystal_F_000             1094
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.086
_exptl_absorpt_coefficient_mu    5.138
_shelx_estimated_absorpt_T_min   0.350
_shelx_estimated_absorpt_T_max   0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5711
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27129
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.518
_diffrn_reflns_theta_max         29.652
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10070
_reflns_number_gt                7559
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0451P)²+1.2386P] 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         10070
_refine_ls_number_parameters     469
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.1092
_refine_ls_wR_factor_gt          0.0996
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
Yb1 Yb 0.36056(2) 0.21760(2) 0.49098(2) 0.03037(7) Uani 1 1 d . . . . .
I1 I 0.82905(7) 0.37064(7) -0.03877(5) 0.1064(2) Uani 1 1 d . . . . .
O5 O 0.4815(3) 0.0510(3) 0.6069(3) 0.0396(9) Uani 1 1 d . . . . .
O6 O 0.3743(3) 0.1117(3) 0.3940(3) 0.0386(9) Uani 1 1 d . . . . .
O2 O 0.4013(3) 0.3529(3) 0.3334(3) 0.0416(9) Uani 1 1 d . . . . .
O1 O 0.5630(4) 0.2074(4) 0.4222(3) 0.0477(10) Uani 1 1 d . . . . .
O4 O 0.2406(3) 0.2161(3) 0.6351(3) 0.0404(9) Uani 1 1 d . . . . .
N2 N 0.2546(4) 0.4274(4) 0.4800(3) 0.0357(10) Uani 1 1 d . . . . .
O3 O 0.2173(4) 0.1059(4) 0.5548(3) 0.0485(10) Uani 1 1 d . . . . .
N1 N 0.4766(4) 0.2930(4) 0.5848(3) 0.0362(10) Uani 1 1 d . . . . .
N3 N 0.1532(4) 0.3237(4) 0.3865(4) 0.0435(11) Uani 1 1 d . . . . .
C18 C 0.6917(6) 0.2193(5) 0.2462(5) 0.0479(14) Uani 1 1 d . . . . .
H18 H 0.7155 0.1468 0.2991 0.058 Uiso 1 1 calc R U . . .
C6 C 0.3023(5) 0.4719(4) 0.5367(4) 0.0398(13) Uani 1 1 d . . . . .
C23 C 0.1922(5) 0.1428(5) 0.6258(4) 0.0374(12) Uani 1 1 d . . . . .
C16 C 0.5135(5) 0.2901(5) 0.3404(4) 0.0378(12) Uani 1 1 d . . . . .
C5 C 0.4265(5) 0.3998(4) 0.5908(4) 0.0340(11) Uani 1 1 d . . . . .
C11 C 0.0965(5) 0.4392(5) 0.3647(4) 0.0458(14) Uani 1 1 d . . . . .
C3 C 0.6088(6) 0.3762(6) 0.6874(5) 0.0524(16) Uani 1 1 d . . . . .
H3 H 0.6526 0.4039 0.7222 0.063 Uiso 1 1 calc R U . . .
C30 C 0.5547(5) -0.0513(4) 0.6499(4) 0.0311(11) Uani 1 1 d . . . . .
C31 C 0.5621(5) -0.1025(4) 0.7609(4) 0.0315(11) Uani 1 1 d . . . . .
C17 C 0.5887(5) 0.3092(5) 0.2519(4) 0.0381(12) Uani 1 1 d . . . . .
C36 C 0.6460(6) -0.2122(5) 0.8136(4) 0.0443(14) Uani 1 1 d . . . . .
H36 H 0.6958 -0.2555 0.7790 0.053 Uiso 1 1 calc R U . . .
C12 C -0.0044(6) 0.5032(7) 0.2915(6) 0.072(2) Uani 1 1 d . . . . .
H12 H -0.0419 0.5836 0.2763 0.086 Uiso 1 1 calc R U . . .
C34 C 0.5829(6) -0.1953(5) 0.9676(4) 0.0485(15) Uani 1 1 d . . . . .
C2 C 0.6606(6) 0.2674(5) 0.6813(5) 0.0495(15) Uani 1 1 d . . . . .
H2 H 0.7405 0.2201 0.7115 0.059 Uiso 1 1 calc R U . . .
C13 C -0.0473(7) 0.4451(8) 0.2423(7) 0.085(3) Uani 1 1 d . . . . .
H13 H -0.1112 0.4870 0.1909 0.102 Uiso 1 1 calc R U . . .
C32 C 0.4845(5) -0.0421(5) 0.8136(4) 0.0424(13) Uani 1 1 d . . . . .
H32 H 0.4249 0.0301 0.7791 0.051 Uiso 1 1 calc R U . . .
C20 C 0.7256(6) 0.3435(6) 0.0867(5) 0.0526(16) Uani 1 1 d . . . . .
C33 C 0.4937(6) -0.0868(5) 0.9164(5) 0.0485(15) Uani 1 1 d . . . . .
H33 H 0.4412 -0.0451 0.9509 0.058 Uiso 1 1 calc R U . . .
C24 C 0.1038(5) 0.0993(5) 0.6972(4) 0.0386(12) Uani 1 1 d . . . . .
C1 C 0.5918(5) 0.2291(5) 0.6295(5) 0.0461(14) Uani 1 1 d . . . . .
H1 H 0.6274 0.1552 0.6257 0.055 Uiso 1 1 calc R U . . .
C10 C 0.1462(5) 0.4934(5) 0.4238(4) 0.0408(13) Uani 1 1 d . . . . .
C29 C 0.0920(6) 0.1168(6) 0.7863(5) 0.0495(15) Uani 1 1 d . . . . .
H29 H 0.1428 0.1539 0.8036 0.059 Uiso 1 1 calc R U . . .
C21 C 0.6251(7) 0.4355(6) 0.0905(5) 0.0612(18) Uani 1 1 d . . . . .
H21 H 0.6037 0.5087 0.0385 0.073 Uiso 1 1 calc R U . . .
C4 C 0.4901(6) 0.4439(5) 0.6406(5) 0.0479(15) Uani 1 1 d . . . . .
H4 H 0.4536 0.5186 0.6427 0.057 Uiso 1 1 calc R U . . .
C22 C 0.5563(6) 0.4168(5) 0.1735(5) 0.0508(15) Uani 1 1 d . . . . .
H22 H 0.4874 0.4778 0.1763 0.061 Uiso 1 1 calc R U . . .
C15 C 0.1053(6) 0.2699(6) 0.3394(5) 0.0562(17) Uani 1 1 d . . . . .
H15 H 0.1426 0.1893 0.3553 0.067 Uiso 1 1 calc R U . . .
C28 C 0.0058(6) 0.0800(6) 0.8499(5) 0.0584(17) Uani 1 1 d . . . . .
H28 H -0.0014 0.0919 0.9100 0.070 Uiso 1 1 calc R U . . .
I3A I 0.6209(5) -0.2561(5) 1.1256(4) 0.0645(9) Uani 0.58(4) 1 d . . P A 1
I3B I 0.587(3) -0.2609(7) 1.1194(7) 0.088(3) Uani 0.42(4) 1 d . . P A 2
I2 I -0.20426(6) -0.02764(7) 0.91666(4) 0.0984(2) Uani 1 1 d . . . . .
OW1 O 0.1875(6) -0.0764(7) 0.4919(5) 0.0873(18) Uani 1 1 d D . . . .
C25 C 0.0269(5) 0.0438(5) 0.6712(5) 0.0466(14) Uani 1 1 d . . . . .
H25 H 0.0343 0.0311 0.6115 0.056 Uiso 1 1 calc R U . . .
C35 C 0.6578(6) -0.2589(5) 0.9166(4) 0.0504(15) Uani 1 1 d . . . . .
H35 H 0.7154 -0.3324 0.9510 0.060 Uiso 1 1 calc R U . . .
C9 C 0.0781(6) 0.6040(5) 0.4241(5) 0.0549(17) Uani 1 1 d . . . . .
H9 H 0.0027 0.6474 0.3846 0.066 Uiso 1 1 calc R U . . .
C26 C -0.0602(6) 0.0079(6) 0.7352(5) 0.0529(16) Uani 1 1 d . . . . .
H26 H -0.1122 -0.0281 0.7178 0.063 Uiso 1 1 calc R U . . .
C7 C 0.2388(6) 0.5822(5) 0.5403(5) 0.0525(16) Uani 1 1 d . . . . .
H7 H 0.2729 0.6114 0.5801 0.063 Uiso 1 1 calc R U . . .
C19 C 0.7591(6) 0.2354(6) 0.1636(5) 0.0581(17) Uani 1 1 d . . . . .
H19 H 0.8266 0.1738 0.1599 0.070 Uiso 1 1 calc R U . . .
C27 C -0.0702(5) 0.0249(6) 0.8233(5) 0.0501(15) Uani 1 1 d . . . . .
C14 C 0.0036(7) 0.3275(8) 0.2688(6) 0.080(3) Uani 1 1 d . . . . .
H14 H -0.0291 0.2861 0.2402 0.096 Uiso 1 1 calc R U . . .
C8 C 0.1258(7) 0.6476(5) 0.4848(6) 0.0629(19) Uani 1 1 d . . . . .
H8 H 0.0818 0.7204 0.4879 0.075 Uiso 1 1 calc R U . . .
HW1A H 0.261(3) -0.118(7) 0.509(7) 0.11(4) Uiso 1 1 d D . . . .
HW1B H 0.198(7) -0.022(5) 0.504(6) 0.08(3) Uiso 1 1 d 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
Yb1 O5 2.238(3) . ?
Yb1 O6 2.245(3) . ?
Yb1 O3 2.405(4) . ?
Yb1 O1 2.434(4) . ?
Yb1 O2 2.438(4) . ?
Yb1 O4 2.440(4) . ?
Yb1 N1 2.498(4) . ?
Yb1 N3 2.521(5) . ?
Yb1 N2 2.534(4) . ?
Yb1 C23 2.787(6) . ?
Yb1 C16 2.791(6) . ?
I1 C20 2.099(6) . ?
O5 C30 1.252(6) . ?
O6 C30 1.260(6) 2_656 ?
O2 C16 1.256(6) . ?
O1 C16 1.267(6) . ?
O4 C23 1.259(6) . ?
N2 C10 1.340(7) . ?
N2 C6 1.349(7) . ?
O3 C23 1.266(7) . ?
N1 C1 1.336(7) . ?
N1 C5 1.345(6) . ?
N3 C11 1.340(7) . ?
N3 C15 1.341(8) . ?
C18 C19 1.378(8) . ?
C18 C17 1.388(8) . ?
C18 H18 0.9300 . ?
C6 C7 1.395(7) . ?
C6 C5 1.473(8) . ?
C23 C24 1.486(8) . ?
C16 C17 1.495(8) . ?
C5 C4 1.380(8) . ?
C11 C12 1.398(8) . ?
C11 C10 1.484(9) . ?
C3 C2 1.371(9) . ?
C3 C4 1.384(9) . ?
C3 H3 0.9300 . ?
C30 O6 1.260(6) 2_656 ?
C30 C31 1.490(7) . ?
C31 C36 1.383(7) . ?
C31 C32 1.384(7) . ?
C17 C22 1.380(8) . ?
C36 C35 1.382(8) . ?
C36 H36 0.9300 . ?
C12 C13 1.378(11) . ?
C12 H12 0.9300 . ?
C34 C35 1.376(8) . ?
C34 C33 1.394(8) . ?
C34 I3B 2.041(10) . ?
C34 I3A 2.138(8) . ?
C2 C1 1.384(8) . ?
C2 H2 0.9300 . ?
C13 C14 1.347(11) . ?
C13 H13 0.9300 . ?
C32 C33 1.378(8) . ?
C32 H32 0.9300 . ?
C20 C19 1.375(9) . ?
C20 C21 1.379(9) . ?
C33 H33 0.9300 . ?
C24 C29 1.378(8) . ?
C24 C25 1.400(8) . ?
C1 H1 0.9300 . ?
C10 C9 1.392(8) . ?
C29 C28 1.380(9) . ?
C29 H29 0.9300 . ?
C21 C22 1.391(9) . ?
C21 H21 0.9300 . ?
C4 H4 0.9300 . ?
C22 H22 0.9300 . ?
C15 C14 1.379(9) . ?
C15 H15 0.9300 . ?
C28 C27 1.392(9) . ?
C28 H28 0.9300 . ?
I2 C27 2.085(6) . ?
OW1 HW1A 0.818(10) . ?
OW1 HW1B 0.819(10) . ?
C25 C26 1.387(9) . ?
C25 H25 0.9300 . ?
C35 H35 0.9300 . ?
C9 C8 1.386(10) . ?
C9 H9 0.9300 . ?
C26 C27 1.362(9) . ?
C26 H26 0.9300 . ?
C7 C8 1.373(9) . ?
C7 H7 0.9300 . ?
C19 H19 0.9300 . ?
C14 H14 0.9300 . ?
C8 H8 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
O5 Yb1 O6 86.49(13) . . ?
O5 Yb1 O3 76.69(14) . . ?
O6 Yb1 O3 75.89(14) . . ?
O5 Yb1 O1 80.00(14) . . ?
O6 Yb1 O1 74.67(14) . . ?
O3 Yb1 O1 143.24(14) . . ?
O5 Yb1 O2 133.25(13) . . ?
O6 Yb1 O2 79.23(13) . . ?
O3 Yb1 O2 139.35(14) . . ?
O1 Yb1 O2 53.34(13) . . ?
O5 Yb1 O4 79.88(13) . . ?
O6 Yb1 O4 129.59(13) . . ?
O3 Yb1 O4 53.79(13) . . ?
O1 Yb1 O4 146.99(13) . . ?
O2 Yb1 O4 141.34(12) . . ?
O5 Yb1 N1 77.60(14) . . ?
O6 Yb1 N1 146.43(14) . . ?
O3 Yb1 N1 127.15(14) . . ?
O1 Yb1 N1 73.58(14) . . ?
O2 Yb1 N1 90.38(14) . . ?
O4 Yb1 N1 76.71(14) . . ?
O5 Yb1 N3 146.95(15) . . ?
O6 Yb1 N3 79.17(14) . . ?
O3 Yb1 N3 71.01(15) . . ?
O1 Yb1 N3 123.41(15) . . ?
O2 Yb1 N3 73.11(14) . . ?
O4 Yb1 N3 86.59(14) . . ?
N1 Yb1 N3 128.36(14) . . ?
O5 Yb1 N2 135.76(14) . . ?
O6 Yb1 N2 137.74(14) . . ?
O3 Yb1 N2 108.15(14) . . ?
O1 Yb1 N2 108.40(14) . . ?
O2 Yb1 N2 71.28(13) . . ?
O4 Yb1 N2 70.26(13) . . ?
N1 Yb1 N2 64.50(14) . . ?
N3 Yb1 N2 63.86(15) . . ?
O5 Yb1 C23 76.42(14) . . ?
O6 Yb1 C23 102.79(15) . . ?
O3 Yb1 C23 26.96(14) . . ?
O1 Yb1 C23 156.40(14) . . ?
O2 Yb1 C23 150.10(13) . . ?
O4 Yb1 C23 26.84(14) . . ?
N1 Yb1 C23 101.90(16) . . ?
N3 Yb1 C23 77.97(15) . . ?
N2 Yb1 C23 89.41(14) . . ?
O5 Yb1 C16 106.56(15) . . ?
O6 Yb1 C16 72.18(14) . . ?
O3 Yb1 C16 147.56(14) . . ?
O1 Yb1 C16 26.98(14) . . ?
O2 Yb1 C16 26.72(13) . . ?
O4 Yb1 C16 158.12(14) . . ?
N1 Yb1 C16 84.20(15) . . ?
N3 Yb1 C16 97.20(16) . . ?
N2 Yb1 C16 92.01(14) . . ?
C23 Yb1 C16 173.74(16) . . ?
C30 O5 Yb1 162.9(4) . . ?
C30 O6 Yb1 146.6(3) 2_656 . ?
C16 O2 Yb1 92.5(3) . . ?
C16 O1 Yb1 92.4(3) . . ?
C23 O4 Yb1 92.1(3) . . ?
C10 N2 C6 118.5(5) . . ?
C10 N2 Yb1 121.2(4) . . ?
C6 N2 Yb1 120.1(3) . . ?
C23 O3 Yb1 93.6(3) . . ?
C1 N1 C5 117.7(5) . . ?
C1 N1 Yb1 121.0(3) . . ?
C5 N1 Yb1 121.4(3) . . ?
C11 N3 C15 117.5(5) . . ?
C11 N3 Yb1 121.4(4) . . ?
C15 N3 Yb1 120.4(4) . . ?
C19 C18 C17 121.2(6) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
N2 C6 C7 121.3(6) . . ?
N2 C6 C5 116.3(4) . . ?
C7 C6 C5 122.3(5) . . ?
O4 C23 O3 120.5(5) . . ?
O4 C23 C24 120.5(5) . . ?
O3 C23 C24 119.0(5) . . ?
O4 C23 Yb1 61.0(3) . . ?
O3 C23 Yb1 59.5(3) . . ?
C24 C23 Yb1 178.2(4) . . ?
O2 C16 O1 120.1(5) . . ?
O2 C16 C17 120.6(5) . . ?
O1 C16 C17 119.3(5) . . ?
O2 C16 Yb1 60.8(3) . . ?
O1 C16 Yb1 60.6(3) . . ?
C17 C16 Yb1 167.0(4) . . ?
N1 C5 C4 122.2(5) . . ?
N1 C5 C6 117.1(5) . . ?
C4 C5 C6 120.7(5) . . ?
N3 C11 C12 121.5(6) . . ?
N3 C11 C10 115.9(5) . . ?
C12 C11 C10 122.6(6) . . ?
C2 C3 C4 118.7(6) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
O5 C30 O6 124.4(5) . 2_656 ?
O5 C30 C31 117.6(4) . . ?
O6 C30 C31 117.9(4) 2_656 . ?
C36 C31 C32 118.3(5) . . ?
C36 C31 C30 120.8(5) . . ?
C32 C31 C30 120.9(5) . . ?
C22 C17 C18 118.6(5) . . ?
C22 C17 C16 120.5(5) . . ?
C18 C17 C16 120.9(5) . . ?
C35 C36 C31 121.5(5) . . ?
C35 C36 H36 119.2 . . ?
C31 C36 H36 119.2 . . ?
C13 C12 C11 118.9(7) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C35 C34 C33 120.6(6) . . ?
C35 C34 I3B 121.8(6) . . ?
C33 C34 I3B 117.4(6) . . ?
C35 C34 I3A 118.5(5) . . ?
C33 C34 I3A 120.5(5) . . ?
C3 C2 C1 118.8(6) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C14 C13 C12 119.8(7) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C33 C32 C31 121.4(5) . . ?
C33 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C19 C20 C21 121.2(6) . . ?
C19 C20 I1 119.8(5) . . ?
C21 C20 I1 119.0(5) . . ?
C32 C33 C34 119.0(5) . . ?
C32 C33 H33 120.5 . . ?
C34 C33 H33 120.5 . . ?
C29 C24 C25 119.5(5) . . ?
C29 C24 C23 121.6(5) . . ?
C25 C24 C23 118.9(5) . . ?
N1 C1 C2 123.2(5) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
N2 C10 C9 123.0(6) . . ?
N2 C10 C11 116.3(5) . . ?
C9 C10 C11 120.6(5) . . ?
C24 C29 C28 120.8(6) . . ?
C24 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C20 C21 C22 118.7(6) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
C5 C4 C3 119.5(5) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C17 C22 C21 121.1(6) . . ?
C17 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
N3 C15 C14 123.6(7) . . ?
N3 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
C29 C28 C27 119.3(6) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
HW1A OW1 HW1B 93(8) . . ?
C26 C25 C24 119.4(6) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C34 C35 C36 119.1(6) . . ?
C34 C35 H35 120.5 . . ?
C36 C35 H35 120.5 . . ?
C8 C9 C10 118.1(6) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 H9 120.9 . . ?
C27 C26 C25 120.6(6) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C8 C7 C6 119.7(6) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C20 C19 C18 119.2(6) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
C26 C27 C28 120.4(6) . . ?
C26 C27 I2 119.5(5) . . ?
C28 C27 I2 120.0(5) . . ?
C13 C14 C15 118.4(7) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C7 C8 C9 119.3(6) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?

_refine_diff_density_max         1.784
_refine_diff_density_min         -2.138
_refine_diff_density_rms         0.145

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_12
_database_code_depnum_ccdc_archive 'CCDC 1514991'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 I6 N6 O14 Tm2'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2322.44

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 '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                   11.194(3)
_cell_length_b                   12.797(4)
_cell_length_c                   14.456(4)
_cell_angle_alpha                68.894(3)
_cell_angle_beta                 88.362(4)
_cell_angle_gamma                72.638(4)
_cell_volume                     1836.6(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    26862
_cell_measurement_theta_min      4.668
_cell_measurement_theta_max      48.074

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_F_000             1092
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.124
_exptl_absorpt_coefficient_mu    4.988
_shelx_estimated_absorpt_T_min   0.526
_shelx_estimated_absorpt_T_max   0.577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6606
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focused sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26861
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.516
_diffrn_reflns_theta_max         29.256
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9842
_reflns_number_gt                7431
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SHELXS 2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0488P)²+1.8140P] 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         9842
_refine_ls_number_parameters     469
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1096
_refine_ls_wR_factor_gt          0.0984
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6036(6) 0.7716(6) 0.3394(5) 0.0628(17) Uani 1 1 d . . . . .
H1 H 0.6408 0.6911 0.3554 0.075 Uiso 1 1 calc R U . . .
C2 C 0.5027(7) 0.8282(8) 0.2698(6) 0.083(2) Uani 1 1 d . . . . .
H2 H 0.4694 0.7867 0.2418 0.100 Uiso 1 1 calc R U . . .
C3 C 0.4521(7) 0.9468(8) 0.2425(6) 0.088(3) Uani 1 1 d . . . . .
H3 H 0.3880 0.9888 0.1913 0.106 Uiso 1 1 calc R U . . .
C4 C 0.4964(6) 1.0045(7) 0.2913(6) 0.073(2) Uani 1 1 d . . . . .
H4 H 0.4602 1.0850 0.2756 0.088 Uiso 1 1 calc R U . . .
C5 C 0.5964(5) 0.9400(5) 0.3644(4) 0.0482(13) Uani 1 1 d . . . . .
C6 C 0.6453(5) 0.9936(5) 0.4241(4) 0.0465(13) Uani 1 1 d . . . . .
C7 C 0.5791(6) 1.1041(5) 0.4256(5) 0.0578(16) Uani 1 1 d . . . . .
H7 H 0.5035 1.1474 0.3865 0.069 Uiso 1 1 calc R U . . .
C8 C 0.6247(7) 1.1483(5) 0.4837(5) 0.0664(19) Uani 1 1 d . . . . .
H8 H 0.5803 1.2213 0.4859 0.080 Uiso 1 1 calc R U . . .
C9 C 0.7391(6) 1.0830(5) 0.5402(5) 0.0561(15) Uani 1 1 d . . . . .
H9 H 0.7730 1.1126 0.5796 0.067 Uiso 1 1 calc R U . . .
C10 C 0.8026(5) 0.9718(4) 0.5370(4) 0.0426(12) Uani 1 1 d . . . . .
C11 C 0.9268(5) 0.9004(4) 0.5910(4) 0.0379(11) Uani 1 1 d . . . . .
C12 C 0.9907(6) 0.9435(5) 0.6409(4) 0.0504(14) Uani 1 1 d . . . . .
H12 H 0.9542 1.0181 0.6430 0.060 Uiso 1 1 calc R U . . .
C13 C 1.1080(6) 0.8770(6) 0.6876(5) 0.0543(15) Uani 1 1 d . . . . .
H13 H 1.1513 0.9049 0.7225 0.065 Uiso 1 1 calc R U . . .
C14 C 1.1605(6) 0.7674(6) 0.6818(5) 0.0544(14) Uani 1 1 d . . . . .
H14 H 1.2401 0.7199 0.7124 0.065 Uiso 1 1 calc R U . . .
C15 C 1.0920(5) 0.7304(5) 0.6293(4) 0.0501(14) Uani 1 1 d . . . . .
H15 H 1.1280 0.6570 0.6249 0.060 Uiso 1 1 calc R U . . .
C23 C 1.0145(5) 0.7901(4) 0.3399(4) 0.0412(11) Uani 1 1 d . . . . .
C28 C 1.1245(7) 0.9355(6) 0.0901(5) 0.0633(17) Uani 1 1 d . . . . .
H19 H 1.1028 1.0083 0.0379 0.076 Uiso 1 1 calc R U . . .
C16 C 0.6929(5) 0.6426(4) 0.6264(4) 0.0405(11) Uani 1 1 d . . . . .
C17 C 0.6031(5) 0.5992(4) 0.6973(4) 0.0415(12) Uani 1 1 d . . . . .
C18 C 0.5266(5) 0.5438(5) 0.6717(5) 0.0497(13) Uani 1 1 d . . . . .
H25 H 0.5339 0.5316 0.6118 0.060 Uiso 1 1 calc R U . . .
C19 C 0.4396(6) 0.5067(5) 0.7353(5) 0.0573(15) Uani 1 1 d . . . . .
H26 H 0.3881 0.4701 0.7182 0.069 Uiso 1 1 calc R U . . .
C20 C 0.4302(5) 0.5246(6) 0.8239(5) 0.0549(15) Uani 1 1 d . . . . .
C21 C 0.5051(6) 0.5800(6) 0.8500(5) 0.0606(16) Uani 1 1 d . . . . .
H28 H 0.4974 0.5926 0.9097 0.073 Uiso 1 1 calc R U . . .
C22 C 0.5917(5) 0.6166(5) 0.7861(4) 0.0507(14) Uani 1 1 d . . . . .
H29 H 0.6427 0.6534 0.8034 0.061 Uiso 1 1 calc R U . . .
C33 C 1.1571(6) 0.2409(5) 0.9177(4) 0.0547(15) Uani 1 1 d . . . . .
H33 H 1.2146 0.1677 0.9527 0.066 Uiso 1 1 calc R U . . .
N1 N 0.6522(4) 0.8252(4) 0.3860(4) 0.0491(11) Uani 1 1 d . . . . .
N2 N 0.7546(4) 0.9280(4) 0.4800(3) 0.0395(9) Uani 1 1 d . . . . .
N3 N 0.9772(4) 0.7936(4) 0.5844(3) 0.0411(10) Uani 1 1 d . . . . .
O1 O 0.7404(3) 0.7155(3) 0.6357(3) 0.0441(8) Uani 1 1 d . . . . .
O2 O 0.7169(4) 0.6058(3) 0.5552(3) 0.0517(9) Uani 1 1 d . . . . .
O6 O 0.8736(3) 0.6119(3) 0.3933(3) 0.0425(8) Uani 1 1 d . . . . .
OW1 O 1.3119(6) 0.5771(6) 0.5078(5) 0.0901(18) Uani 1 1 d D . . . .
I2 I 1.32923(6) 0.87060(7) -0.03875(5) 0.1113(2) Uani 1 1 d . . . . .
I1 I 0.29578(5) 0.47186(7) 0.91687(4) 0.1019(2) Uani 1 1 d . . . . .
C24 C 1.0890(5) 0.8094(4) 0.2516(4) 0.0394(11) Uani 1 1 d . . . . .
C29 C 1.0562(6) 0.9169(5) 0.1728(4) 0.0534(14) Uani 1 1 d . . . . .
H18 H 0.9871 0.9777 0.1754 0.064 Uiso 1 1 calc R U . . .
C27 C 1.2261(6) 0.8431(6) 0.0868(5) 0.0571(15) Uani 1 1 d . . . . .
C26 C 1.2590(6) 0.7352(6) 0.1641(5) 0.0608(16) Uani 1 1 d . . . . .
H21 H 1.3267 0.6738 0.1607 0.073 Uiso 1 1 calc R U . . .
C25 C 1.1914(5) 0.7187(5) 0.2465(5) 0.0516(14) Uani 1 1 d . . . . .
H22 H 1.2145 0.6462 0.2991 0.062 Uiso 1 1 calc R U . . .
C30 C 1.0563(4) 0.4490(4) 0.6495(4) 0.0331(10) Uani 1 1 d . . . . .
C31 C 1.0623(5) 0.3969(4) 0.7616(4) 0.0355(10) Uani 1 1 d . . . . .
C32 C 1.1460(5) 0.2877(5) 0.8143(4) 0.0478(13) Uani 1 1 d . . . . .
H32 H 1.1961 0.2445 0.7798 0.057 Uiso 1 1 calc R U . . .
C34 C 1.0813(6) 0.3050(5) 0.9665(4) 0.0519(14) Uani 1 1 d . . . . .
C35 C 0.9944(6) 0.4130(5) 0.9172(4) 0.0520(14) Uani 1 1 d . . . . .
H35 H 0.9434 0.4550 0.9521 0.062 Uiso 1 1 calc R U . . .
C36 C 0.9847(5) 0.4578(5) 0.8136(4) 0.0449(12) Uani 1 1 d . . . . .
H36 H 0.9252 0.5299 0.7789 0.054 Uiso 1 1 calc R U . . .
O4 O 0.9018(3) 0.8529(3) 0.3328(3) 0.0453(9) Uani 1 1 d . . . . .
O3 O 1.0627(4) 0.7078(4) 0.4214(3) 0.0513(9) Uani 1 1 d . . . . .
O5 O 0.9820(3) 0.5505(3) 0.6074(3) 0.0446(9) Uani 1 1 d . . . . .
I3A I 1.1193(4) 0.2441(5) 1.1257(3) 0.0691(10) Uani 0.59(4) 1 d . . P A 1
I3B I 1.086(3) 0.2388(7) 1.1192(7) 0.098(3) Uani 0.41(4) 1 d . . P A 2
Tm1 Tm 0.86043(2) 0.71775(2) 0.49099(2) 0.03437(7) Uani 1 1 d . . . . .
HW1B H 1.306(7) 0.520(4) 0.496(6) 0.08(3) Uiso 1 1 d D . . . .
HW1A H 1.241(3) 0.619(5) 0.484(5) 0.08(2) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.341(8) . ?
C1 C2 1.366(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.360(11) . ?
C2 H2 0.9300 . ?
C3 C4 1.379(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.393(8) . ?
C4 H4 0.9300 . ?
C5 N1 1.333(7) . ?
C5 C6 1.481(9) . ?
C6 N2 1.345(7) . ?
C6 C7 1.394(8) . ?
C7 C8 1.351(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.391(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.405(7) . ?
C9 H9 0.9300 . ?
C10 N2 1.350(7) . ?
C10 C11 1.473(8) . ?
C11 N3 1.351(6) . ?
C11 C12 1.375(7) . ?
C12 C13 1.369(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.382(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.377(8) . ?
C14 H14 0.9300 . ?
C15 N3 1.333(7) . ?
C15 H15 0.9300 . ?
C23 O3 1.262(6) . ?
C23 O4 1.262(6) . ?
C23 C24 1.490(7) . ?
C23 Tm1 2.808(5) . ?
C28 C29 1.387(8) . ?
C28 C27 1.388(9) . ?
C28 H19 0.9300 . ?
C16 O1 1.250(6) . ?
C16 O2 1.269(6) . ?
C16 C17 1.495(7) . ?
C16 Tm1 2.790(5) . ?
C17 C22 1.375(8) . ?
C17 C18 1.393(8) . ?
C18 C19 1.390(8) . ?
C18 H25 0.9300 . ?
C19 C20 1.375(9) . ?
C19 H26 0.9300 . ?
C20 C21 1.385(9) . ?
C20 I1 2.089(6) . ?
C21 C22 1.385(8) . ?
C21 H28 0.9300 . ?
C22 H29 0.9300 . ?
C33 C34 1.362(8) . ?
C33 C32 1.390(8) . ?
C33 H33 0.9300 . ?
N1 Tm1 2.533(4) . ?
N2 Tm1 2.543(4) . ?
N3 Tm1 2.505(4) . ?
O1 Tm1 2.450(4) . ?
O2 Tm1 2.414(4) . ?
O6 C30 1.249(5) 2_766 ?
O6 Tm1 2.258(3) . ?
OW1 HW1B 0.822(10) . ?
OW1 HW1A 0.818(10) . ?
I2 C27 2.101(6) . ?
C24 C29 1.385(8) . ?
C24 C25 1.389(7) . ?
C29 H18 0.9300 . ?
C27 C26 1.379(9) . ?
C26 C25 1.378(8) . ?
C26 H21 0.9300 . ?
C25 H22 0.9300 . ?
C30 O6 1.249(5) 2_766 ?
C30 O5 1.250(6) . ?
C30 C31 1.509(7) . ?
C31 C32 1.380(7) . ?
C31 C36 1.381(7) . ?
C32 H32 0.9300 . ?
C34 C35 1.376(8) . ?
C34 I3B 2.056(10) . ?
C34 I3A 2.157(7) . ?
C35 C36 1.391(8) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
O4 Tm1 2.450(4) . ?
O3 Tm1 2.439(4) . ?
O5 Tm1 2.250(3) . ?

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
N1 C1 C2 123.8(6) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C3 C2 C1 118.2(7) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 119.5(7) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C3 C4 C5 118.8(7) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 121.6(6) . . ?
N1 C5 C6 116.1(5) . . ?
C4 C5 C6 122.3(6) . . ?
N2 C6 C7 121.8(6) . . ?
N2 C6 C5 116.4(5) . . ?
C7 C6 C5 121.8(5) . . ?
C8 C7 C6 120.1(6) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 119.1(5) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C8 C9 C10 119.1(6) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
N2 C10 C9 121.1(5) . . ?
N2 C10 C11 116.7(4) . . ?
C9 C10 C11 122.1(5) . . ?
N3 C11 C12 122.0(5) . . ?
N3 C11 C10 116.8(5) . . ?
C12 C11 C10 121.2(5) . . ?
C13 C12 C11 120.1(5) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 118.6(6) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
C15 C14 C13 118.3(6) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
N3 C15 C14 123.9(5) . . ?
N3 C15 H15 118.0 . . ?
C14 C15 H15 118.0 . . ?
O3 C23 O4 119.6(5) . . ?
O3 C23 C24 120.0(5) . . ?
O4 C23 C24 120.4(5) . . ?
O3 C23 Tm1 60.1(3) . . ?
O4 C23 Tm1 60.6(3) . . ?
C24 C23 Tm1 167.1(4) . . ?
C29 C28 C27 118.6(6) . . ?
C29 C28 H19 120.7 . . ?
C27 C28 H19 120.7 . . ?
O1 C16 O2 121.0(5) . . ?
O1 C16 C17 120.7(5) . . ?
O2 C16 C17 118.2(5) . . ?
O1 C16 Tm1 61.3(3) . . ?
O2 C16 Tm1 59.7(3) . . ?
C17 C16 Tm1 177.9(4) . . ?
C22 C17 C18 119.4(5) . . ?
C22 C17 C16 121.0(5) . . ?
C18 C17 C16 119.6(5) . . ?
C19 C18 C17 120.2(6) . . ?
C19 C18 H25 119.9 . . ?
C17 C18 H25 119.9 . . ?
C20 C19 C18 119.4(6) . . ?
C20 C19 H26 120.3 . . ?
C18 C19 H26 120.3 . . ?
C19 C20 C21 121.0(6) . . ?
C19 C20 I1 118.8(4) . . ?
C21 C20 I1 120.1(5) . . ?
C20 C21 C22 119.1(6) . . ?
C20 C21 H28 120.4 . . ?
C22 C21 H28 120.4 . . ?
C17 C22 C21 120.9(6) . . ?
C17 C22 H29 119.6 . . ?
C21 C22 H29 119.6 . . ?
C34 C33 C32 118.2(5) . . ?
C34 C33 H33 120.9 . . ?
C32 C33 H33 120.9 . . ?
C5 N1 C1 117.7(5) . . ?
C5 N1 Tm1 121.4(4) . . ?
C1 N1 Tm1 120.2(4) . . ?
C6 N2 C10 118.9(4) . . ?
C6 N2 Tm1 121.0(4) . . ?
C10 N2 Tm1 119.9(3) . . ?
C15 N3 C11 117.2(5) . . ?
C15 N3 Tm1 121.3(3) . . ?
C11 N3 Tm1 121.5(3) . . ?
C16 O1 Tm1 92.1(3) . . ?
C16 O2 Tm1 93.3(3) . . ?
C30 O6 Tm1 146.7(3) 2_766 . ?
HW1B OW1 HW1A 95(7) . . ?
C29 C24 C25 119.0(5) . . ?
C29 C24 C23 120.8(5) . . ?
C25 C24 C23 120.2(5) . . ?
C24 C29 C28 121.2(5) . . ?
C24 C29 H18 119.4 . . ?
C28 C29 H18 119.4 . . ?
C26 C27 C28 121.0(6) . . ?
C26 C27 I2 120.4(5) . . ?
C28 C27 I2 118.7(5) . . ?
C25 C26 C27 119.8(6) . . ?
C25 C26 H21 120.1 . . ?
C27 C26 H21 120.1 . . ?
C26 C25 C24 120.5(6) . . ?
C26 C25 H22 119.8 . . ?
C24 C25 H22 119.8 . . ?
O6 C30 O5 125.5(5) 2_766 . ?
O6 C30 C31 117.6(4) 2_766 . ?
O5 C30 C31 116.9(4) . . ?
C32 C31 C36 118.7(5) . . ?
C32 C31 C30 120.6(4) . . ?
C36 C31 C30 120.7(4) . . ?
C31 C32 C33 121.4(5) . . ?
C31 C32 H32 119.3 . . ?
C33 C32 H32 119.3 . . ?
C33 C34 C35 122.5(5) . . ?
C33 C34 I3B 120.6(6) . . ?
C35 C34 I3B 116.8(6) . . ?
C33 C34 I3A 117.5(5) . . ?
C35 C34 I3A 119.4(4) . . ?
C34 C35 C36 118.2(5) . . ?
C34 C35 H35 120.9 . . ?
C36 C35 H35 120.9 . . ?
C31 C36 C35 121.0(5) . . ?
C31 C36 H36 119.5 . . ?
C35 C36 H36 119.5 . . ?
C23 O4 Tm1 92.7(3) . . ?
C23 O3 Tm1 93.2(3) . . ?
C30 O5 Tm1 162.6(3) . . ?
O5 Tm1 O6 86.63(13) . . ?
O5 Tm1 O2 76.58(14) . . ?
O6 Tm1 O2 75.96(13) . . ?
O5 Tm1 O3 80.22(14) . . ?
O6 Tm1 O3 74.55(14) . . ?
O2 Tm1 O3 143.22(14) . . ?
O5 Tm1 O1 79.70(13) . . ?
O6 Tm1 O1 129.46(13) . . ?
O2 Tm1 O1 53.59(12) . . ?
O3 Tm1 O1 147.24(13) . . ?
O5 Tm1 O4 133.13(13) . . ?
O6 Tm1 O4 79.02(13) . . ?
O2 Tm1 O4 139.48(13) . . ?
O3 Tm1 O4 52.99(12) . . ?
O1 Tm1 O4 141.71(11) . . ?
O5 Tm1 N3 77.75(14) . . ?
O6 Tm1 N3 146.46(14) . . ?
O2 Tm1 N3 127.24(14) . . ?
O3 Tm1 N3 73.66(14) . . ?
O1 Tm1 N3 76.96(13) . . ?
O4 Tm1 N3 90.22(14) . . ?
O5 Tm1 N1 147.21(15) . . ?
O6 Tm1 N1 79.22(14) . . ?
O2 Tm1 N1 71.37(15) . . ?
O3 Tm1 N1 123.04(14) . . ?
O1 Tm1 N1 86.72(14) . . ?
O4 Tm1 N1 73.01(14) . . ?
N3 Tm1 N1 128.03(15) . . ?
O5 Tm1 N2 135.76(13) . . ?
O6 Tm1 N2 137.60(13) . . ?
O2 Tm1 N2 108.26(13) . . ?
O3 Tm1 N2 108.30(14) . . ?
O1 Tm1 N2 70.52(12) . . ?
O4 Tm1 N2 71.39(12) . . ?
N3 Tm1 N2 64.38(14) . . ?
N1 Tm1 N2 63.65(15) . . ?
O5 Tm1 C16 76.15(14) . . ?
O6 Tm1 C16 102.89(15) . . ?
O2 Tm1 C16 27.00(14) . . ?
O3 Tm1 C16 156.35(14) . . ?
O1 Tm1 C16 26.59(13) . . ?
O4 Tm1 C16 150.49(13) . . ?
N3 Tm1 C16 101.89(15) . . ?
N1 Tm1 C16 78.41(15) . . ?
N2 Tm1 C16 89.59(14) . . ?
O5 Tm1 C23 106.48(15) . . ?
O6 Tm1 C23 72.12(14) . . ?
O2 Tm1 C23 147.62(14) . . ?
O3 Tm1 C23 26.65(14) . . ?
O1 Tm1 C23 158.33(14) . . ?
O4 Tm1 C23 26.67(13) . . ?
N3 Tm1 C23 84.01(15) . . ?
N1 Tm1 C23 97.14(16) . . ?
N2 Tm1 C23 92.02(14) . . ?
C16 Tm1 C23 173.99(16) . . ?

_refine_diff_density_max         1.670
_refine_diff_density_min         -2.150
_refine_diff_density_rms         0.132

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_15
_database_code_depnum_ccdc_archive 'CCDC 1514997'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 I6 N6 O14 Y2'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2162.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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                   11.1808(5)
_cell_length_b                   12.8254(5)
_cell_length_c                   14.4618(6)
_cell_angle_alpha                68.8920(10)
_cell_angle_beta                 88.4450(11)
_cell_angle_gamma                72.6910(9)
_cell_volume                     1839.57(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    27290
_cell_measurement_theta_min      4.667
_cell_measurement_theta_max      57.460
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_F_000             1032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    4.154
_shelx_estimated_absorpt_T_min   0.414
_shelx_estimated_absorpt_T_max   0.476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6194
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27289
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.515
_diffrn_reflns_theta_max         29.651
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10131
_reflns_number_gt                7438
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0782P)²+2.2837P] 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         10131
_refine_ls_number_parameters     469
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1508
_refine_ls_wR_factor_gt          0.1372
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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
C15 C 0.1003(5) 0.7742(5) -0.6605(5) 0.0617(14) Uani 1 1 d . . . . .
H15 H 0.1351 0.6935 -0.6437 0.074 Uiso 1 1 calc R U . . .
C14 C 0.0006(6) 0.8340(7) -0.7319(6) 0.083(2) Uani 1 1 d . . . . .
H14 H -0.0320 0.7940 -0.7620 0.099 Uiso 1 1 calc R U . . .
C13 C -0.0500(6) 0.9516(7) -0.7583(6) 0.085(2) Uani 1 1 d . . . . .
H13 H -0.1142 0.9939 -0.8094 0.102 Uiso 1 1 calc R U . . .
C12 C -0.0052(5) 1.0076(5) -0.7086(5) 0.0753(18) Uani 1 1 d . . . . .
H12 H -0.0413 1.0878 -0.7235 0.090 Uiso 1 1 calc R U . . .
C11 C 0.0953(4) 0.9423(4) -0.6355(4) 0.0483(10) Uani 1 1 d . . . . .
C10 C 0.1446(4) 0.9954(4) -0.5756(3) 0.0432(10) Uani 1 1 d . . . . .
C9 C 0.0785(5) 1.1059(4) -0.5749(4) 0.0566(13) Uani 1 1 d . . . . .
H9 H 0.0032 1.1500 -0.6143 0.068 Uiso 1 1 calc R U . . .
C8 C 0.1269(5) 1.1482(4) -0.5148(5) 0.0632(15) Uani 1 1 d . . . . .
H8 H 0.0832 1.2208 -0.5117 0.076 Uiso 1 1 calc R U . . .
C7 C 0.2395(5) 1.0835(4) -0.4596(4) 0.0562(13) Uani 1 1 d . . . . .
H7 H 0.2739 1.1127 -0.4201 0.067 Uiso 1 1 calc R U . . .
C6 C 0.3026(4) 0.9732(3) -0.4627(3) 0.0408(9) Uani 1 1 d . . . . .
C5 C 0.4272(4) 0.9014(3) -0.4086(3) 0.0379(8) Uani 1 1 d . . . . .
C4 C 0.4925(5) 0.9440(4) -0.3579(4) 0.0498(11) Uani 1 1 d . . . . .
H4 H 0.4564 1.0180 -0.3551 0.060 Uiso 1 1 calc R U . . .
C3 C 0.6100(5) 0.8770(5) -0.3118(4) 0.0534(11) Uani 1 1 d . . . . .
H3 H 0.6538 0.9044 -0.2768 0.064 Uiso 1 1 calc R U . . .
C2 C 0.6619(5) 0.7693(5) -0.3180(4) 0.0531(11) Uani 1 1 d . . . . .
H2 H 0.7420 0.7224 -0.2880 0.064 Uiso 1 1 calc R U . . .
C1 C 0.5923(4) 0.7310(4) -0.3701(4) 0.0482(10) Uani 1 1 d . . . . .
H1 H 0.6277 0.6574 -0.3738 0.058 Uiso 1 1 calc R U . . .
C16 C 0.5141(4) 0.7897(4) -0.6605(3) 0.0394(9) Uani 1 1 d . . . . .
C17 C 0.5894(4) 0.8090(4) -0.7495(3) 0.0390(8) Uani 1 1 d . . . . .
C18 C 0.6920(4) 0.7191(4) -0.7542(4) 0.0503(11) Uani 1 1 d . . . . .
H18 H 0.7160 0.6473 -0.7010 0.060 Uiso 1 1 calc R U . . .
C19 C 0.7590(5) 0.7350(5) -0.8367(4) 0.0594(13) Uani 1 1 d . . . . .
H19 H 0.8258 0.6734 -0.8407 0.071 Uiso 1 1 calc R U . . .
C20 C 0.7261(5) 0.8432(5) -0.9135(4) 0.0571(12) Uani 1 1 d . . . . .
C21 C 0.6260(6) 0.9342(5) -0.9094(4) 0.0613(13) Uani 1 1 d . . . . .
H21 H 0.6057 1.0074 -0.9608 0.074 Uiso 1 1 calc R U . . .
C22 C 0.5555(5) 0.9162(4) -0.8284(4) 0.0523(11) Uani 1 1 d . . . . .
H22 H 0.4850 0.9763 -0.8268 0.063 Uiso 1 1 calc R U . . .
C23 C 0.1916(4) 0.6420(3) -0.3732(3) 0.0383(8) Uani 1 1 d . . . . .
C24 C 0.1027(4) 0.5990(3) -0.3027(3) 0.0404(9) Uani 1 1 d . . . . .
C25 C 0.0246(4) 0.5436(4) -0.3276(4) 0.0486(10) Uani 1 1 d . . . . .
H25 H 0.0307 0.5319 -0.3876 0.058 Uiso 1 1 calc R U . . .
C26 C -0.0608(5) 0.5063(5) -0.2642(4) 0.0554(12) Uani 1 1 d . . . . .
H26 H -0.1115 0.4688 -0.2809 0.067 Uiso 1 1 calc R U . . .
C27 C -0.0708(4) 0.5247(5) -0.1769(4) 0.0553(12) Uani 1 1 d . . . . .
C28 C 0.0043(5) 0.5801(5) -0.1493(4) 0.0593(13) Uani 1 1 d . . . . .
H28 H -0.0032 0.5922 -0.0895 0.071 Uiso 1 1 calc R U . . .
C29 C 0.0912(5) 0.6168(4) -0.2143(4) 0.0502(11) Uani 1 1 d . . . . .
H29 H 0.1421 0.6540 -0.1974 0.060 Uiso 1 1 calc R U . . .
C30 C 0.5572(4) 0.4486(3) -0.3491(3) 0.0321(7) Uani 1 1 d . . . . .
C31 C 0.5635(4) 0.3969(3) -0.2375(3) 0.0351(8) Uani 1 1 d . . . . .
C32 C 0.6470(5) 0.2875(4) -0.1854(3) 0.0464(10) Uani 1 1 d . . . . .
H32 H 0.6968 0.2443 -0.2198 0.056 Uiso 1 1 calc R U . . .
C33 C 0.6572(5) 0.2411(4) -0.0821(4) 0.0536(12) Uani 1 1 d . . . . .
H33 H 0.7142 0.1677 -0.0473 0.064 Uiso 1 1 calc R U . . .
C34 C 0.5821(5) 0.3051(4) -0.0318(3) 0.0491(11) Uani 1 1 d . . . . .
C35 C 0.4940(5) 0.4117(4) -0.0826(4) 0.0508(11) Uani 1 1 d . . . . .
H35 H 0.4406 0.4524 -0.0481 0.061 Uiso 1 1 calc R U . . .
C36 C 0.4855(4) 0.4579(4) -0.1856(3) 0.0427(9) Uani 1 1 d . . . . .
H36 H 0.4269 0.5304 -0.2202 0.051 Uiso 1 1 calc R U . . .
N3 N 0.1496(3) 0.8271(3) -0.6140(3) 0.0463(8) Uani 1 1 d . . . . .
N2 N 0.2546(3) 0.9296(3) -0.5198(3) 0.0369(7) Uani 1 1 d . . . . .
N1 N 0.4777(3) 0.7947(3) -0.4148(3) 0.0404(8) Uani 1 1 d . . . . .
O1 O 0.4020(3) 0.8534(2) -0.6688(2) 0.0436(7) Uani 1 1 d . . . . .
O2 O 0.5636(3) 0.7075(3) -0.5793(2) 0.0497(7) Uani 1 1 d . . . . .
O3 O 0.2395(3) 0.7147(2) -0.3631(2) 0.0420(6) Uani 1 1 d . . . . .
O4 O 0.2148(3) 0.6063(3) -0.4445(3) 0.0502(7) Uani 1 1 d . . . . .
O5 O 0.4841(3) 0.5498(2) -0.3917(2) 0.0427(7) Uani 1 1 d . . . . .
O6 O 0.6281(3) 0.3878(2) -0.3923(2) 0.0417(7) Uani 1 1 d . . . . .
OW1 O 0.8124(5) 0.5763(6) -0.4922(4) 0.0899(16) Uani 1 1 d D . . . .
Y1 Y 0.36059(3) 0.71734(3) -0.50893(3) 0.03153(10) Uani 1 1 d . . . . .
I1 I 0.83006(6) 0.87051(6) -1.03880(4) 0.1093(2) Uani 1 1 d . . . . .
I2 I -0.20490(5) 0.47209(6) -0.08301(4) 0.0992(2) Uani 1 1 d . . . . .
I3A I 0.6194(4) 0.2439(4) 0.1269(2) 0.0677(6) Uani 0.64(3) 1 d . . P A 1
I3B I 0.581(2) 0.2386(5) 0.1179(7) 0.084(3) Uani 0.36(3) 1 d . . P A 2
HW1A H 0.745(5) 0.608(8) -0.526(6) 0.12(3) Uiso 1 1 d D . . . .
HW1B H 0.802(11) 0.518(6) -0.498(9) 0.16(5) Uiso 1 1 d 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
C15 N3 1.337(7) . ?
C15 C14 1.372(8) . ?
C15 H15 0.9300 . ?
C14 C13 1.352(10) . ?
C14 H14 0.9300 . ?
C13 C12 1.375(10) . ?
C13 H13 0.9300 . ?
C12 C11 1.396(7) . ?
C12 H12 0.9300 . ?
C11 N3 1.339(6) . ?
C11 C10 1.481(7) . ?
C10 N2 1.349(5) . ?
C10 C9 1.394(6) . ?
C9 C8 1.371(8) . ?
C9 H9 0.9300 . ?
C8 C7 1.367(8) . ?
C8 H8 0.9300 . ?
C7 C6 1.397(6) . ?
C7 H7 0.9300 . ?
C6 N2 1.349(6) . ?
C6 C5 1.475(6) . ?
C5 N1 1.351(5) . ?
C5 C4 1.387(6) . ?
C4 C3 1.368(8) . ?
C4 H4 0.9300 . ?
C3 C2 1.365(7) . ?
C3 H3 0.9300 . ?
C2 C1 1.392(7) . ?
C2 H2 0.9300 . ?
C1 N1 1.330(6) . ?
C1 H1 0.9300 . ?
C16 O1 1.257(5) . ?
C16 O2 1.263(5) . ?
C16 C17 1.504(6) . ?
C16 Y1 2.809(4) . ?
C17 C18 1.383(6) . ?
C17 C22 1.386(6) . ?
C18 C19 1.377(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.380(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.374(8) . ?
C20 I1 2.104(5) . ?
C21 C22 1.382(7) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O3 1.256(5) . ?
C23 O4 1.264(5) . ?
C23 C24 1.482(6) . ?
C23 Y1 2.807(4) . ?
C24 C29 1.374(7) . ?
C24 C25 1.404(6) . ?
C25 C26 1.375(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.362(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.394(8) . ?
C27 I2 2.092(5) . ?
C28 C29 1.397(7) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 O5 1.246(4) . ?
C30 O6 1.258(4) . ?
C30 C31 1.502(5) . ?
C31 C32 1.381(6) . ?
C31 C36 1.385(5) . ?
C32 C33 1.388(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.377(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.376(7) . ?
C34 I3B 2.021(8) . ?
C34 I3A 2.149(6) . ?
C35 C36 1.384(6) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N3 Y1 2.556(4) . ?
N2 Y1 2.573(3) . ?
N1 Y1 2.528(4) . ?
O1 Y1 2.475(3) . ?
O2 Y1 2.450(3) . ?
O3 Y1 2.471(3) . ?
O4 Y1 2.428(3) . ?
O5 Y1 2.266(3) . ?
O6 Y1 2.269(3) 2_664 ?
OW1 HW1A 0.822(10) . ?
OW1 HW1B 0.822(10) . ?
Y1 O6 2.269(3) 2_664 ?

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
N3 C15 C14 122.6(6) . . ?
N3 C15 H15 118.7 . . ?
C14 C15 H15 118.7 . . ?
C13 C14 C15 119.5(6) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C14 C13 C12 119.1(6) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C12 C11 119.0(6) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
N3 C11 C12 121.4(5) . . ?
N3 C11 C10 116.6(4) . . ?
C12 C11 C10 122.0(5) . . ?
N2 C10 C9 122.1(5) . . ?
N2 C10 C11 116.4(4) . . ?
C9 C10 C11 121.5(4) . . ?
C8 C9 C10 118.6(5) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C7 C8 C9 119.8(4) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C8 C7 C6 119.6(5) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
N2 C6 C7 121.1(4) . . ?
N2 C6 C5 116.6(3) . . ?
C7 C6 C5 122.2(4) . . ?
N1 C5 C4 121.4(4) . . ?
N1 C5 C6 117.1(4) . . ?
C4 C5 C6 121.5(4) . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C2 C3 C4 119.0(5) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C3 C2 C1 118.6(5) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
N1 C1 C2 123.2(4) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
O1 C16 O2 121.1(4) . . ?
O1 C16 C17 119.6(4) . . ?
O2 C16 C17 119.2(4) . . ?
O1 C16 Y1 61.7(2) . . ?
O2 C16 Y1 60.6(2) . . ?
C17 C16 Y1 167.2(3) . . ?
C18 C17 C22 119.3(4) . . ?
C18 C17 C16 120.3(4) . . ?
C22 C17 C16 120.4(4) . . ?
C19 C18 C17 120.6(5) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C20 119.4(5) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C21 C20 C19 120.9(5) . . ?
C21 C20 I1 119.2(4) . . ?
C19 C20 I1 119.9(4) . . ?
C20 C21 C22 119.5(5) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C21 C22 C17 120.2(5) . . ?
C21 C22 H22 119.9 . . ?
C17 C22 H22 119.9 . . ?
O3 C23 O4 121.3(4) . . ?
O3 C23 C24 120.2(4) . . ?
O4 C23 C24 118.5(4) . . ?
O3 C23 Y1 61.6(2) . . ?
O4 C23 Y1 59.7(2) . . ?
C24 C23 Y1 178.1(3) . . ?
C29 C24 C25 118.8(4) . . ?
C29 C24 C23 121.1(4) . . ?
C25 C24 C23 120.1(4) . . ?
C26 C25 C24 120.7(5) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C27 C26 C25 119.7(5) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C26 C27 C28 121.7(5) . . ?
C26 C27 I2 119.3(4) . . ?
C28 C27 I2 119.1(4) . . ?
C27 C28 C29 118.0(5) . . ?
C27 C28 H28 121.0 . . ?
C29 C28 H28 121.0 . . ?
C24 C29 C28 121.2(5) . . ?
C24 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
O5 C30 O6 124.9(4) . . ?
O5 C30 C31 117.3(3) . . ?
O6 C30 C31 117.7(3) . . ?
C32 C31 C36 119.1(4) . . ?
C32 C31 C30 120.3(4) . . ?
C36 C31 C30 120.6(3) . . ?
C31 C32 C33 120.7(4) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
C34 C33 C32 119.2(4) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C35 C34 C33 120.8(4) . . ?
C35 C34 I3B 117.1(5) . . ?
C33 C34 I3B 121.6(5) . . ?
C35 C34 I3A 120.6(4) . . ?
C33 C34 I3A 118.3(4) . . ?
C34 C35 C36 119.5(4) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.3 . . ?
C35 C36 C31 120.5(4) . . ?
C35 C36 H36 119.7 . . ?
C31 C36 H36 119.7 . . ?
C15 N3 C11 118.2(4) . . ?
C15 N3 Y1 120.0(3) . . ?
C11 N3 Y1 121.2(3) . . ?
C6 N2 C10 118.7(3) . . ?
C6 N2 Y1 120.1(3) . . ?
C10 N2 Y1 120.9(3) . . ?
C1 N1 C5 117.8(4) . . ?
C1 N1 Y1 120.5(3) . . ?
C5 N1 Y1 121.6(3) . . ?
C16 O1 Y1 91.7(2) . . ?
C16 O2 Y1 92.7(3) . . ?
C23 O3 Y1 91.8(2) . . ?
C23 O4 Y1 93.6(3) . . ?
C30 O5 Y1 162.9(3) . . ?
C30 O6 Y1 146.0(3) . 2_664 ?
HW1A OW1 HW1B 81(9) . . ?
O5 Y1 O6 87.20(10) . 2_664 ?
O5 Y1 O4 77.23(12) . . ?
O6 Y1 O4 76.02(11) 2_664 . ?
O5 Y1 O2 80.09(11) . . ?
O6 Y1 O2 74.74(12) 2_664 . ?
O4 Y1 O2 143.57(11) . . ?
O5 Y1 O3 79.77(11) . . ?
O6 Y1 O3 129.19(11) 2_664 . ?
O4 Y1 O3 53.26(10) . . ?
O2 Y1 O3 147.48(11) . . ?
O5 Y1 O1 132.95(11) . . ?
O6 Y1 O1 78.83(10) 2_664 . ?
O4 Y1 O1 139.23(12) . . ?
O2 Y1 O1 52.93(10) . . ?
O3 Y1 O1 141.82(9) . . ?
O5 Y1 N1 77.74(11) . . ?
O6 Y1 N1 147.18(11) 2_664 . ?
O4 Y1 N1 127.14(12) . . ?
O2 Y1 N1 74.03(11) . . ?
O3 Y1 N1 76.91(11) . . ?
O1 Y1 N1 90.28(11) . . ?
O5 Y1 N3 147.81(13) . . ?
O6 Y1 N3 79.33(11) 2_664 . ?
O4 Y1 N3 71.21(13) . . ?
O2 Y1 N3 123.13(12) . . ?
O3 Y1 N3 86.32(12) . . ?
O1 Y1 N3 72.98(12) . . ?
N1 Y1 N3 127.13(12) . . ?
O5 Y1 N2 135.44(11) . . ?
O6 Y1 N2 137.35(11) 2_664 . ?
O4 Y1 N2 108.09(11) . . ?
O2 Y1 N2 108.09(11) . . ?
O3 Y1 N2 70.70(10) . . ?
O1 Y1 N2 71.37(10) . . ?
N1 Y1 N2 63.79(11) . . ?
N3 Y1 N2 63.35(12) . . ?
O5 Y1 C23 76.52(11) . . ?
O6 Y1 C23 102.66(12) 2_664 . ?
O4 Y1 C23 26.71(11) . . ?
O2 Y1 C23 156.58(11) . . ?
O3 Y1 C23 26.56(11) . . ?
O1 Y1 C23 150.30(11) . . ?
N1 Y1 C23 101.91(12) . . ?
N3 Y1 C23 78.13(12) . . ?
N2 Y1 C23 89.73(11) . . ?
O5 Y1 C16 106.40(12) . . ?
O6 Y1 C16 72.13(12) 2_664 . ?
O4 Y1 C16 147.65(11) . . ?
O2 Y1 C16 26.68(12) . . ?
O3 Y1 C16 158.56(11) . . ?
O1 Y1 C16 26.58(11) . . ?
N1 Y1 C16 84.28(12) . . ?
N3 Y1 C16 97.13(13) . . ?
N2 Y1 C16 91.87(11) . . ?
C23 Y1 C16 173.67(12) . . ?

_refine_diff_density_max         1.998
_refine_diff_density_min         -2.166
_refine_diff_density_rms         0.111

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
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data_Complex_10
_database_code_depnum_ccdc_archive 'CCDC 1514988'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 Ho2 I6 N6 O14'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2314.44

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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                   11.2147(5)
_cell_length_b                   12.8161(6)
_cell_length_c                   14.4733(7)
_cell_angle_alpha                68.947(2)
_cell_angle_beta                 88.4170(10)
_cell_angle_gamma                72.6810(10)
_cell_volume                     1845.99(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    27606
_cell_measurement_theta_min      4.355
_cell_measurement_theta_max      54.654

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_F_000             1088
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.115
_exptl_absorpt_coefficient_mu    4.703
_shelx_estimated_absorpt_T_min   0.374
_shelx_estimated_absorpt_T_max   0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6812
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27603
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.514
_diffrn_reflns_theta_max         30.631
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10361
_reflns_number_gt                8078
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0305P)²+2.4055P] 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         10361
_refine_ls_number_parameters     469
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0842
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.150
_refine_ls_shift/su_max          0.002
_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
Ho1 Ho 0.36012(2) 0.71795(2) 0.49089(2) 0.03274(6) Uani 1 1 d . . . . .
I3A I 0.6175(3) 0.2439(4) 1.1268(3) 0.0668(8) Uani 0.58(3) 1 d . . P A 1
I3B I 0.584(2) 0.2391(5) 1.1182(6) 0.097(2) Uani 0.42(3) 1 d . . P A 2
I1 I 0.82961(5) 0.86958(5) -0.03812(4) 0.10988(19) Uani 1 1 d . U . . .
I2 I -0.20423(4) 0.47126(5) 0.91688(3) 0.09344(16) Uani 1 1 d . U . . .
O5 O 0.4838(3) 0.5503(2) 0.6082(2) 0.0441(7) Uani 1 1 d . . . . .
O6 O 0.3722(3) 0.6119(2) 0.3921(2) 0.0408(6) Uani 1 1 d . . . . .
O1 O 0.4019(3) 0.8536(2) 0.3311(2) 0.0430(7) Uani 1 1 d . . . . .
O2 O 0.5632(3) 0.7081(3) 0.4210(2) 0.0498(7) Uani 1 1 d . . . . .
O3 O 0.2388(3) 0.7151(2) 0.6368(2) 0.0425(7) Uani 1 1 d . . . . .
N2 N 0.2539(3) 0.9297(3) 0.4803(2) 0.0365(7) Uani 1 1 d . . . . .
N1 N 0.4775(3) 0.7948(3) 0.5851(3) 0.0400(8) Uani 1 1 d . . . . .
O4 O 0.2147(3) 0.6068(3) 0.5548(2) 0.0494(7) Uani 1 1 d . . . . .
C30 C 0.5563(3) 0.4492(3) 0.6507(3) 0.0327(8) Uani 1 1 d . . . . .
N3 N 0.1499(3) 0.8275(3) 0.3858(3) 0.0459(8) Uani 1 1 d . . . . .
C6 C 0.3029(4) 0.9730(3) 0.5377(3) 0.0387(9) Uani 1 1 d . . . . .
C17 C 0.5891(4) 0.8093(4) 0.2508(3) 0.0388(9) Uani 1 1 d . . . . .
C16 C 0.5144(4) 0.7905(4) 0.3397(3) 0.0397(9) Uani 1 1 d . . . . .
C23 C 0.1912(4) 0.6423(3) 0.6263(3) 0.0381(9) Uani 1 1 d . . . . .
C22 C 0.6923(4) 0.7188(4) 0.2466(3) 0.0510(11) Uani 1 1 d . . . . .
H22 H 0.7162 0.6472 0.2999 0.061 Uiso 1 1 calc R U . . .
C3 C 0.6093(5) 0.8782(4) 0.6871(3) 0.0530(11) Uani 1 1 d . . . . .
H3 H 0.6531 0.9066 0.7212 0.064 Uiso 1 1 calc R U . . .
C5 C 0.4271(4) 0.9014(3) 0.5914(3) 0.0373(9) Uani 1 1 d . . . . .
C2 C 0.6612(4) 0.7688(4) 0.6814(3) 0.0503(11) Uani 1 1 d . . . . .
H2 H 0.7410 0.7217 0.7114 0.060 Uiso 1 1 calc R U . . .
C12 C -0.0049(5) 1.0071(5) 0.2921(4) 0.0735(16) Uani 1 1 d . . . . .
H12 H -0.0412 1.0873 0.2774 0.088 Uiso 1 1 calc R U . . .
C1 C 0.5922(4) 0.7313(4) 0.6301(3) 0.0482(10) Uani 1 1 d . . . . .
H1 H 0.6274 0.6574 0.6267 0.058 Uiso 1 1 calc R U . . .
C24 C 0.1024(4) 0.5984(3) 0.6971(3) 0.0384(9) Uani 1 1 d . . . . .
C32 C 0.4854(4) 0.4577(4) 0.8144(3) 0.0432(10) Uani 1 1 d . . . . .
H32 H 0.4276 0.5307 0.7799 0.052 Uiso 1 1 calc R U . . .
C29 C 0.0898(4) 0.6169(4) 0.7858(3) 0.0490(10) Uani 1 1 d . . . . .
H29 H 0.1396 0.6550 0.8027 0.059 Uiso 1 1 calc R U . . .
C31 C 0.5624(4) 0.3968(3) 0.7622(3) 0.0339(8) Uani 1 1 d . . . . .
C11 C 0.0955(4) 0.9425(4) 0.3647(3) 0.0466(10) Uani 1 1 d . . . . .
C34 C 0.5804(5) 0.3048(4) 0.9675(3) 0.0474(10) Uani 1 1 d . . . . .
C26 C -0.0610(4) 0.5061(4) 0.7356(4) 0.0518(11) Uani 1 1 d . . . . .
H26 H -0.1123 0.4693 0.7187 0.062 Uiso 1 1 calc R U . . .
C36 C 0.6462(4) 0.2870(4) 0.8150(3) 0.0436(10) Uani 1 1 d . . . . .
H36 H 0.6963 0.2437 0.7808 0.052 Uiso 1 1 calc R U . . .
C10 C 0.1448(4) 0.9954(3) 0.4246(3) 0.0423(10) Uani 1 1 d . . . . .
C8 C 0.1254(5) 1.1484(4) 0.4858(4) 0.0643(15) Uani 1 1 d . . . . .
H8 H 0.0810 1.2208 0.4891 0.077 Uiso 1 1 calc R U . . .
C27 C -0.0701(4) 0.5246(4) 0.8238(3) 0.0511(11) Uani 1 1 d . . . . .
C28 C 0.0044(5) 0.5795(4) 0.8497(3) 0.0553(12) Uani 1 1 d . . . . .
H28 H -0.0026 0.5913 0.9096 0.066 Uiso 1 1 calc R U . . .
C33 C 0.4930(4) 0.4118(4) 0.9171(3) 0.0509(11) Uani 1 1 d . . . . .
H33 H 0.4398 0.4526 0.9517 0.061 Uiso 1 1 calc R U . . .
C4 C 0.4921(4) 0.9437(4) 0.6417(3) 0.0470(10) Uani 1 1 d . . . . .
H4 H 0.4556 1.0176 0.6447 0.056 Uiso 1 1 calc R U . . .
C9 C 0.0792(5) 1.1054(4) 0.4260(4) 0.0566(12) Uani 1 1 d . . . . .
H9 H 0.0043 1.1494 0.3864 0.068 Uiso 1 1 calc R U . . .
OW1 O 0.8119(5) 0.5769(6) 0.5083(4) 0.0875(16) Uani 1 1 d . . . . .
C25 C 0.0254(4) 0.5432(4) 0.6726(3) 0.0470(10) Uani 1 1 d . . . . .
H25 H 0.0321 0.5309 0.6129 0.056 Uiso 1 1 calc R U . . .
C35 C 0.6561(5) 0.2410(4) 0.9179(3) 0.0515(11) Uani 1 1 d . . . . .
H35 H 0.7134 0.1680 0.9529 0.062 Uiso 1 1 calc R U . . .
C18 C 0.5564(5) 0.9158(4) 0.1724(3) 0.0530(11) Uani 1 1 d . . . . .
H18 H 0.4871 0.9764 0.1746 0.064 Uiso 1 1 calc R U . . .
C21 C 0.7592(5) 0.7343(5) 0.1645(4) 0.0597(13) Uani 1 1 d . . . . .
H21 H 0.8261 0.6725 0.1610 0.072 Uiso 1 1 calc R U . . .
C19 C 0.6255(5) 0.9341(5) 0.0902(4) 0.0625(14) Uani 1 1 d . . . . .
H19 H 0.6043 1.0068 0.0382 0.075 Uiso 1 1 calc R U . . .
C15 C 0.1024(5) 0.7751(5) 0.3385(4) 0.0613(13) Uani 1 1 d . . . . .
H15 H 0.1383 0.6946 0.3548 0.074 Uiso 1 1 calc R U . . .
C20 C 0.7265(5) 0.8422(5) 0.0869(4) 0.0564(12) Uani 1 1 d . . . . .
C14 C 0.0037(6) 0.8330(6) 0.2673(5) 0.0813(18) Uani 1 1 d . . . . .
H14 H -0.0267 0.7926 0.2364 0.098 Uiso 1 1 calc R U . . .
C13 C -0.0497(6) 0.9509(6) 0.2423(5) 0.087(2) Uani 1 1 d . . . . .
H13 H -0.1153 0.9928 0.1925 0.105 Uiso 1 1 calc R U . . .
C7 C 0.2393(5) 1.0832(4) 0.5416(4) 0.0535(12) Uani 1 1 d . . . . .
H7 H 0.2732 1.1123 0.5813 0.064 Uiso 1 1 calc R U . . .
HW1B H 0.749(7) 0.616(7) 0.482(6) 0.10(3) Uiso 1 1 d . . . . .
HW1A H 0.810(6) 0.527(6) 0.497(5) 0.07(2) Uiso 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
Ho1 O5 2.271(3) . ?
Ho1 O6 2.277(3) . ?
Ho1 O4 2.428(3) . ?
Ho1 O2 2.453(3) . ?
Ho1 O1 2.475(3) . ?
Ho1 O3 2.476(3) . ?
Ho1 N1 2.529(3) . ?
Ho1 N3 2.556(3) . ?
Ho1 N2 2.567(3) . ?
Ho1 C23 2.810(4) . ?
Ho1 C16 2.817(4) . ?
I3A C34 2.159(6) . ?
I3B C34 2.032(8) . ?
I1 C20 2.099(4) . ?
I2 C27 2.094(4) . ?
O5 C30 1.244(4) . ?
O6 C30 1.260(4) 2_666 ?
O1 C16 1.261(5) . ?
O2 C16 1.265(5) . ?
O3 C23 1.258(5) . ?
N2 C10 1.345(5) . ?
N2 C6 1.356(5) . ?
N1 C1 1.336(5) . ?
N1 C5 1.350(5) . ?
O4 C23 1.265(5) . ?
C30 O6 1.260(4) 2_666 ?
C30 C31 1.504(5) . ?
N3 C15 1.330(6) . ?
N3 C11 1.338(5) . ?
C6 C7 1.401(5) . ?
C6 C5 1.475(6) . ?
C17 C18 1.378(6) . ?
C17 C22 1.392(6) . ?
C17 C16 1.501(6) . ?
C23 C24 1.491(6) . ?
C22 C21 1.372(6) . ?
C22 H22 0.9300 . ?
C3 C4 1.362(7) . ?
C3 C2 1.381(7) . ?
C3 H3 0.9300 . ?
C5 C4 1.380(6) . ?
C2 C1 1.375(6) . ?
C2 H2 0.9300 . ?
C12 C13 1.378(8) . ?
C12 C11 1.393(6) . ?
C12 H12 0.9300 . ?
C1 H1 0.9300 . ?
C24 C29 1.383(6) . ?
C24 C25 1.390(6) . ?
C32 C31 1.383(5) . ?
C32 C33 1.383(6) . ?
C32 H32 0.9300 . ?
C29 C28 1.381(6) . ?
C29 H29 0.9300 . ?
C31 C36 1.388(5) . ?
C11 C10 1.479(7) . ?
C34 C35 1.371(6) . ?
C34 C33 1.376(6) . ?
C26 C27 1.375(7) . ?
C26 C25 1.382(6) . ?
C26 H26 0.9300 . ?
C36 C35 1.385(6) . ?
C36 H36 0.9300 . ?
C10 C9 1.390(6) . ?
C8 C9 1.363(7) . ?
C8 C7 1.385(7) . ?
C8 H8 0.9300 . ?
C27 C28 1.374(7) . ?
C28 H28 0.9300 . ?
C33 H33 0.9300 . ?
C4 H4 0.9300 . ?
C9 H9 0.9300 . ?
OW1 HW1B 0.75(7) . ?
OW1 HW1A 0.72(6) . ?
C25 H25 0.9300 . ?
C35 H35 0.9300 . ?
C18 C19 1.389(7) . ?
C18 H18 0.9300 . ?
C21 C20 1.383(7) . ?
C21 H21 0.9300 . ?
C19 C20 1.383(7) . ?
C19 H19 0.9300 . ?
C15 C14 1.364(7) . ?
C15 H15 0.9300 . ?
C14 C13 1.361(9) . ?
C14 H14 0.9300 . ?
C13 H13 0.9300 . ?
C7 H7 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
O5 Ho1 O6 87.14(10) . . ?
O5 Ho1 O4 77.44(11) . . ?
O6 Ho1 O4 75.94(10) . . ?
O5 Ho1 O2 79.92(11) . . ?
O6 Ho1 O2 74.78(11) . . ?
O4 Ho1 O2 143.57(11) . . ?
O5 Ho1 O1 132.75(10) . . ?
O6 Ho1 O1 78.78(10) . . ?
O4 Ho1 O1 139.12(10) . . ?
O2 Ho1 O1 52.91(9) . . ?
O5 Ho1 O3 79.78(10) . . ?
O6 Ho1 O3 129.12(10) . . ?
O4 Ho1 O3 53.28(10) . . ?
O2 Ho1 O3 147.38(10) . . ?
O1 Ho1 O3 142.03(9) . . ?
O5 Ho1 N1 77.40(10) . . ?
O6 Ho1 N1 146.81(11) . . ?
O4 Ho1 N1 127.32(11) . . ?
O2 Ho1 N1 73.70(11) . . ?
O1 Ho1 N1 90.35(10) . . ?
O3 Ho1 N1 77.13(10) . . ?
O5 Ho1 N3 147.93(12) . . ?
O6 Ho1 N3 79.46(11) . . ?
O4 Ho1 N3 71.11(11) . . ?
O2 Ho1 N3 123.25(11) . . ?
O1 Ho1 N3 73.06(11) . . ?
O3 Ho1 N3 86.32(11) . . ?
N1 Ho1 N3 127.43(11) . . ?
O5 Ho1 N2 135.36(10) . . ?
O6 Ho1 N2 137.50(10) . . ?
O4 Ho1 N2 107.93(10) . . ?
O2 Ho1 N2 108.25(11) . . ?
O1 Ho1 N2 71.66(9) . . ?
O3 Ho1 N2 70.62(9) . . ?
N1 Ho1 N2 64.15(11) . . ?
N3 Ho1 N2 63.28(11) . . ?
O5 Ho1 C23 76.62(11) . . ?
O6 Ho1 C23 102.56(12) . . ?
O4 Ho1 C23 26.70(11) . . ?
O2 Ho1 C23 156.50(10) . . ?
O1 Ho1 C23 150.38(10) . . ?
O3 Ho1 C23 26.59(10) . . ?
N1 Ho1 C23 102.14(12) . . ?
N3 Ho1 C23 78.08(12) . . ?
N2 Ho1 C23 89.63(11) . . ?
O5 Ho1 C16 106.20(12) . . ?
O6 Ho1 C16 72.28(11) . . ?
O4 Ho1 C16 147.72(11) . . ?
O2 Ho1 C16 26.65(11) . . ?
O1 Ho1 C16 26.57(10) . . ?
O3 Ho1 C16 158.49(11) . . ?
N1 Ho1 C16 83.97(11) . . ?
N3 Ho1 C16 97.30(12) . . ?
N2 Ho1 C16 92.01(11) . . ?
C23 Ho1 C16 173.77(12) . . ?
C30 O5 Ho1 162.7(3) . . ?
C30 O6 Ho1 145.8(3) 2_666 . ?
C16 O1 Ho1 92.0(2) . . ?
C16 O2 Ho1 92.9(2) . . ?
C23 O3 Ho1 91.7(2) . . ?
C10 N2 C6 119.1(3) . . ?
C10 N2 Ho1 121.0(3) . . ?
C6 N2 Ho1 119.6(2) . . ?
C1 N1 C5 117.5(4) . . ?
C1 N1 Ho1 121.1(3) . . ?
C5 N1 Ho1 121.4(3) . . ?
C23 O4 Ho1 93.7(3) . . ?
O5 C30 O6 125.2(4) . 2_666 ?
O5 C30 C31 117.6(3) . . ?
O6 C30 C31 117.2(3) 2_666 . ?
C15 N3 C11 118.1(4) . . ?
C15 N3 Ho1 119.9(3) . . ?
C11 N3 Ho1 121.2(3) . . ?
N2 C6 C7 120.7(4) . . ?
N2 C6 C5 117.0(3) . . ?
C7 C6 C5 122.3(4) . . ?
C18 C17 C22 119.2(4) . . ?
C18 C17 C16 120.6(4) . . ?
C22 C17 C16 120.2(4) . . ?
O1 C16 O2 120.8(4) . . ?
O1 C16 C17 119.6(4) . . ?
O2 C16 C17 119.5(4) . . ?
O1 C16 Ho1 61.4(2) . . ?
O2 C16 Ho1 60.4(2) . . ?
C17 C16 Ho1 166.6(3) . . ?
O3 C23 O4 121.3(4) . . ?
O3 C23 C24 120.2(4) . . ?
O4 C23 C24 118.5(4) . . ?
O3 C23 Ho1 61.7(2) . . ?
O4 C23 Ho1 59.6(2) . . ?
C24 C23 Ho1 177.9(3) . . ?
C21 C22 C17 120.5(4) . . ?
C21 C22 H22 119.7 . . ?
C17 C22 H22 119.7 . . ?
C4 C3 C2 118.4(4) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
N1 C5 C4 121.3(4) . . ?
N1 C5 C6 117.1(4) . . ?
C4 C5 C6 121.6(4) . . ?
C1 C2 C3 118.4(4) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C13 C12 C11 119.2(5) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
N1 C1 C2 123.8(4) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C29 C24 C25 118.5(4) . . ?
C29 C24 C23 121.1(4) . . ?
C25 C24 C23 120.3(4) . . ?
C31 C32 C33 121.0(4) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C28 C29 C24 120.9(4) . . ?
C28 C29 H29 119.6 . . ?
C24 C29 H29 119.6 . . ?
C32 C31 C36 118.6(4) . . ?
C32 C31 C30 120.6(3) . . ?
C36 C31 C30 120.8(3) . . ?
N3 C11 C12 121.2(5) . . ?
N3 C11 C10 116.4(4) . . ?
C12 C11 C10 122.4(4) . . ?
C35 C34 C33 121.3(4) . . ?
C35 C34 I3B 121.1(4) . . ?
C33 C34 I3B 117.4(5) . . ?
C35 C34 I3A 118.0(4) . . ?
C33 C34 I3A 120.2(3) . . ?
C27 C26 C25 118.9(4) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
C35 C36 C31 120.9(4) . . ?
C35 C36 H36 119.6 . . ?
C31 C36 H36 119.6 . . ?
N2 C10 C9 121.8(4) . . ?
N2 C10 C11 116.5(4) . . ?
C9 C10 C11 121.6(4) . . ?
C9 C8 C7 119.2(4) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C28 C27 C26 121.3(4) . . ?
C28 C27 I2 120.4(4) . . ?
C26 C27 I2 118.4(3) . . ?
C27 C28 C29 119.3(4) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C34 C33 C32 119.0(4) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C3 C4 C5 120.7(4) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C8 C9 C10 119.6(5) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
HW1B OW1 HW1A 96(7) . . ?
C26 C25 C24 121.1(4) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C34 C35 C36 119.1(4) . . ?
C34 C35 H35 120.5 . . ?
C36 C35 H35 120.5 . . ?
C17 C18 C19 120.9(4) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C22 C21 C20 119.7(5) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C20 C19 C18 118.8(5) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
N3 C15 C14 123.5(5) . . ?
N3 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
C21 C20 C19 120.8(4) . . ?
C21 C20 I1 120.5(4) . . ?
C19 C20 I1 118.7(4) . . ?
C13 C14 C15 119.0(6) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C14 C13 C12 118.8(5) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C8 C7 C6 119.4(5) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?

_refine_diff_density_max         1.856
_refine_diff_density_min         -1.781
_refine_diff_density_rms         0.112

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_12Prime
_database_code_depnum_ccdc_archive 'CCDC 1514992'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H38 I4 N6 O12 Tm2'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293
_chemical_formula_weight         1880.42

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 '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                   9.9471(3)
_cell_length_b                   10.5094(4)
_cell_length_c                   15.3693(5)
_cell_angle_alpha                85.3250(10)
_cell_angle_beta                 75.351(2)
_cell_angle_gamma                74.9130(10)
_cell_volume                     1500.66(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    22212
_cell_measurement_theta_min      4.370
_cell_measurement_theta_max      52.651

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_F_000             886
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.544
_exptl_crystal_size_mid          0.299
_exptl_crystal_size_min          0.132
_exptl_absorpt_coefficient_mu    5.061
_shelx_estimated_absorpt_T_min   0.169
_shelx_estimated_absorpt_T_max   0.555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5191
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focused sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22208
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.370
_diffrn_reflns_theta_max         29.731
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8247
_reflns_number_gt                7270
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0331P)²+1.4814P] 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         8247
_refine_ls_number_parameters     409
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0758
_refine_ls_wR_factor_gt          0.0728
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Tm1 Tm 0.25095(2) 0.32017(2) 0.38413(2) 0.02943(5) Uani 1 1 d . . . . .
I1 I 0.48216(5) -0.30109(4) -0.03770(3) 0.08342(13) Uani 1 1 d . . . . .
I2A I -0.0349(2) 0.7890(3) -0.09896(14) 0.1344(7) Uani 0.620(6) 1 d . . P A 1
I2B I -0.0742(3) 0.8735(6) -0.0521(4) 0.141(2) Uani 0.380(6) 1 d . . P A 2
O5 O 0.1825(2) 0.4714(3) 0.49536(19) 0.0415(6) Uani 1 1 d . . . . .
O6 O 0.0024(2) 0.3719(2) 0.43354(17) 0.0362(5) Uani 1 1 d . . . . .
O1 O 0.4195(3) 0.1527(3) 0.29339(18) 0.0421(6) Uani 1 1 d . . . . .
O2 O 0.1954(3) 0.1423(3) 0.3221(2) 0.0489(7) Uani 1 1 d . . . . .
N1 N 0.4617(3) 0.4216(3) 0.3242(2) 0.0371(6) Uani 1 1 d . . . . .
N3 N 0.2072(3) 0.1649(3) 0.5150(2) 0.0371(6) Uani 1 1 d . . . . .
N2 N 0.4426(3) 0.2600(3) 0.47015(19) 0.0303(6) Uani 1 1 d . . . . .
C16 C 0.3236(4) 0.1044(3) 0.2787(2) 0.0359(7) Uani 1 1 d . . . . .
O3A O 0.1767(12) 0.455(2) 0.2773(9) 0.043(3) Uani 0.49(5) 1 d . . P B 1
O3B O 0.2062(18) 0.399(3) 0.2479(17) 0.063(6) Uani 0.51(5) 1 d . . P B 2
C10 C 0.4269(4) 0.1838(3) 0.5449(2) 0.0351(7) Uani 1 1 d . . . . .
C4 C 0.6914(5) 0.4439(6) 0.3323(3) 0.0655(14) Uani 1 1 d . . . . .
H4 H 0.7638 0.4272 0.3630 0.079 Uiso 1 1 calc R U . . .
C17 C 0.3641(4) 0.0020(3) 0.2087(2) 0.0350(7) Uani 1 1 d . . . . .
C5 C 0.5691(4) 0.3984(4) 0.3662(2) 0.0377(8) Uani 1 1 d . . . . .
C11 C 0.3054(4) 0.1198(3) 0.5640(2) 0.0365(7) Uani 1 1 d . . . . .
C14 C 0.0701(5) 0.0205(4) 0.6002(3) 0.0540(11) Uani 1 1 d . . . . .
H14 H -0.0129 -0.0097 0.6124 0.065 Uiso 1 1 calc R U . . .
C21 C 0.2995(5) -0.1513(4) 0.1279(3) 0.0513(10) Uani 1 1 d . . . . .
H21 H 0.2325 -0.1945 0.1207 0.062 Uiso 1 1 calc R U . . .
C22 C 0.2653(5) -0.0627(4) 0.1966(3) 0.0474(9) Uani 1 1 d . . . . .
H22 H 0.1745 -0.0462 0.2354 0.057 Uiso 1 1 calc R U . . .
C20 C 0.4330(5) -0.1748(4) 0.0706(3) 0.0451(9) Uani 1 1 d . . . . .
C1 C 0.4764(5) 0.4924(5) 0.2470(3) 0.0532(10) Uani 1 1 d . . . . .
H1 H 0.4026 0.5102 0.2173 0.064 Uiso 1 1 calc R U . . .
C19 C 0.5347(5) -0.1151(4) 0.0827(3) 0.0554(11) Uani 1 1 d . . . . .
H19 H 0.6263 -0.1341 0.0449 0.066 Uiso 1 1 calc R U . . .
C12 C 0.2935(5) 0.0200(4) 0.6288(3) 0.0487(10) Uani 1 1 d . . . . .
H12 H 0.3652 -0.0128 0.6595 0.058 Uiso 1 1 calc R U . . .
C7 C 0.6446(5) 0.3067(4) 0.5069(3) 0.0509(10) Uani 1 1 d . . . . .
H7 H 0.7187 0.3492 0.4922 0.061 Uiso 1 1 calc R U . . .
C9 C 0.5167(5) 0.1677(4) 0.6034(3) 0.0519(10) Uani 1 1 d . . . . .
H9 H 0.5033 0.1149 0.6549 0.062 Uiso 1 1 calc R U . . .
C6 C 0.5516(4) 0.3187(3) 0.4513(2) 0.0343(7) Uani 1 1 d . . . . .
C15 C 0.0913(4) 0.1169(4) 0.5345(3) 0.0468(9) Uani 1 1 d . . . . .
H15 H 0.0212 0.1496 0.5025 0.056 Uiso 1 1 calc R U . . .
C18 C 0.4994(4) -0.0267(4) 0.1518(3) 0.0469(9) Uani 1 1 d . . . . .
H18 H 0.5678 0.0139 0.1600 0.056 Uiso 1 1 calc R U . . .
C13 C 0.1734(5) -0.0294(4) 0.6467(3) 0.0551(11) Uani 1 1 d . . . . .
H13 H 0.1628 -0.0957 0.6899 0.066 Uiso 1 1 calc R U . . .
C24 C 0.0709(5) 0.6068(5) 0.1878(3) 0.0525(10) Uani 1 1 d . . . . .
C8 C 0.6253(5) 0.2312(5) 0.5837(3) 0.0606(12) Uani 1 1 d . . . . .
H8 H 0.6856 0.2229 0.6224 0.073 Uiso 1 1 calc R U . . .
C25 C 0.1250(5) 0.5445(5) 0.1071(3) 0.0662(13) Uani 1 1 d . . . . .
H25 H 0.1851 0.4600 0.1045 0.079 Uiso 1 1 calc R U . . .
C2 C 0.5945(6) 0.5393(6) 0.2100(3) 0.0693(14) Uani 1 1 d . . . . .
H2 H 0.6002 0.5878 0.1564 0.083 Uiso 1 1 calc R U . . .
C3 C 0.7036(6) 0.5144(6) 0.2521(4) 0.0812(18) Uani 1 1 d . . . . .
H3 H 0.7853 0.5445 0.2273 0.097 Uiso 1 1 calc R U . . .
C30 C 0.0516(3) 0.5292(3) 0.5179(2) 0.0308(7) Uani 1 1 d . . . . .
C29 C -0.0231(6) 0.7309(6) 0.1889(5) 0.0834(18) Uani 1 1 d . . . . .
H29 H -0.0644 0.7754 0.2429 0.100 Uiso 1 1 calc R U . . .
C28 C -0.0553(7) 0.7884(6) 0.1095(7) 0.108(3) Uani 1 1 d . . . . .
H28 H -0.1178 0.8715 0.1101 0.130 Uiso 1 1 calc R U . . .
C26 C 0.0922(7) 0.6044(8) 0.0296(4) 0.095(2) Uani 1 1 d . . . . .
H26 H 0.1320 0.5612 -0.0249 0.115 Uiso 1 1 calc R U . . .
C27 C 0.0040(8) 0.7236(9) 0.0323(6) 0.102(3) Uani 1 1 d . . . . .
O4A O 0.0424(15) 0.6346(8) 0.3412(4) 0.111(4) Uani 0.593(16) 1 d . . P B 1
O4B O 0.1444(12) 0.5610(12) 0.3306(5) 0.058(4) Uani 0.407(16) 1 d . . P B 2
C23 C 0.1141(10) 0.5456(10) 0.2702(5) 0.100(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tm1 O3A 2.220(10) . ?
Tm1 O5 2.281(2) . ?
Tm1 O3B 2.293(14) . ?
Tm1 O6 2.325(2) . ?
Tm1 O1 2.352(3) . ?
Tm1 O2 2.409(3) . ?
Tm1 N3 2.508(3) . ?
Tm1 N2 2.509(3) . ?
Tm1 N1 2.531(3) . ?
Tm1 O4B 2.629(12) . ?
Tm1 C16 2.728(4) . ?
I1 C20 2.094(4) . ?
I2A C27 2.173(7) . ?
I2B C27 2.076(6) . ?
O5 C30 1.257(4) . ?
O6 C30 1.248(4) 2_566 ?
O1 C16 1.264(4) . ?
O2 C16 1.257(4) . ?
N1 C5 1.342(5) . ?
N1 C1 1.344(5) . ?
N3 C15 1.334(5) . ?
N3 C11 1.349(5) . ?
N2 C6 1.343(4) . ?
N2 C10 1.344(4) . ?
C16 C17 1.490(5) . ?
O3A C23 1.010(19) . ?
O3B C23 1.59(3) . ?
C10 C9 1.393(5) . ?
C10 C11 1.487(5) . ?
C4 C3 1.380(7) . ?
C4 C5 1.386(5) . ?
C4 H4 0.9300 . ?
C17 C18 1.379(5) . ?
C17 C22 1.387(5) . ?
C5 C6 1.492(5) . ?
C11 C12 1.393(5) . ?
C14 C13 1.368(7) . ?
C14 C15 1.389(6) . ?
C14 H14 0.9300 . ?
C21 C20 1.368(6) . ?
C21 C22 1.383(6) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C20 C19 1.377(6) . ?
C1 C2 1.365(6) . ?
C1 H1 0.9300 . ?
C19 C18 1.384(6) . ?
C19 H19 0.9300 . ?
C12 C13 1.381(6) . ?
C12 H12 0.9300 . ?
C7 C8 1.369(6) . ?
C7 C6 1.386(5) . ?
C7 H7 0.9300 . ?
C9 C8 1.371(6) . ?
C9 H9 0.9300 . ?
C15 H15 0.9300 . ?
C18 H18 0.9300 . ?
C13 H13 0.9300 . ?
C24 C25 1.368(7) . ?
C24 C29 1.391(8) . ?
C24 C23 1.484(8) . ?
C8 H8 0.9300 . ?
C25 C26 1.374(7) . ?
C25 H25 0.9300 . ?
C2 C3 1.358(7) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C30 O6 1.248(4) 2_566 ?
C30 C30 1.550(6) 2_566 ?
C29 C28 1.391(10) . ?
C29 H29 0.9300 . ?
C28 C27 1.338(11) . ?
C28 H28 0.9300 . ?
C26 C27 1.326(10) . ?
C26 H26 0.9300 . ?
O4A C23 1.414(12) . ?
O4B C23 1.081(9) . ?

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
O3A Tm1 O5 97.5(6) . . ?
O5 Tm1 O3B 115.9(9) . . ?
O3A Tm1 O6 76.2(3) . . ?
O5 Tm1 O6 71.28(8) . . ?
O3B Tm1 O6 84.1(5) . . ?
O3A Tm1 O1 99.3(5) . . ?
O5 Tm1 O1 152.94(9) . . ?
O3B Tm1 O1 81.9(9) . . ?
O6 Tm1 O1 133.55(8) . . ?
O3A Tm1 O2 89.7(5) . . ?
O5 Tm1 O2 146.44(9) . . ?
O3B Tm1 O2 74.8(8) . . ?
O6 Tm1 O2 78.84(9) . . ?
O1 Tm1 O2 54.77(9) . . ?
O3A Tm1 N3 151.2(2) . . ?
O5 Tm1 N3 82.46(10) . . ?
O3B Tm1 N3 147.5(5) . . ?
O6 Tm1 N3 76.60(9) . . ?
O1 Tm1 N3 92.65(10) . . ?
O2 Tm1 N3 75.98(10) . . ?
O3A Tm1 N2 143.0(3) . . ?
O5 Tm1 N2 74.43(9) . . ?
O3B Tm1 N2 143.4(3) . . ?
O6 Tm1 N2 130.89(9) . . ?
O1 Tm1 N2 79.39(9) . . ?
O2 Tm1 N2 117.23(10) . . ?
N3 Tm1 N2 64.89(9) . . ?
O3A Tm1 N1 78.8(2) . . ?
O5 Tm1 N1 85.40(10) . . ?
O3B Tm1 N1 80.6(3) . . ?
O6 Tm1 N1 142.84(9) . . ?
O1 Tm1 N1 77.30(10) . . ?
O2 Tm1 N1 128.15(9) . . ?
N3 Tm1 N1 129.65(10) . . ?
N2 Tm1 N1 64.77(9) . . ?
O5 Tm1 O4B 66.6(2) . . ?
O3B Tm1 O4B 49.3(10) . . ?
O6 Tm1 O4B 70.7(2) . . ?
O1 Tm1 O4B 126.0(2) . . ?
O2 Tm1 O4B 117.34(19) . . ?
N3 Tm1 O4B 140.5(2) . . ?
N2 Tm1 O4B 124.30(19) . . ?
N1 Tm1 O4B 73.7(2) . . ?
O3A Tm1 C16 92.5(6) . . ?
O5 Tm1 C16 168.55(10) . . ?
O3B Tm1 C16 74.3(9) . . ?
O6 Tm1 C16 106.01(10) . . ?
O1 Tm1 C16 27.56(10) . . ?
O2 Tm1 C16 27.44(10) . . ?
N3 Tm1 C16 86.09(10) . . ?
N2 Tm1 C16 100.72(10) . . ?
N1 Tm1 C16 102.07(10) . . ?
O4B Tm1 C16 123.6(2) . . ?
C30 O5 Tm1 117.1(2) . . ?
C30 O6 Tm1 115.3(2) 2_566 . ?
C16 O1 Tm1 93.0(2) . . ?
C16 O2 Tm1 90.6(2) . . ?
C5 N1 C1 117.3(3) . . ?
C5 N1 Tm1 120.3(2) . . ?
C1 N1 Tm1 122.3(3) . . ?
C15 N3 C11 117.7(3) . . ?
C15 N3 Tm1 121.2(3) . . ?
C11 N3 Tm1 120.9(2) . . ?
C6 N2 C10 117.9(3) . . ?
C6 N2 Tm1 120.8(2) . . ?
C10 N2 Tm1 120.5(2) . . ?
O2 C16 O1 120.7(3) . . ?
O2 C16 C17 120.1(3) . . ?
O1 C16 C17 119.2(3) . . ?
O2 C16 Tm1 61.99(19) . . ?
O1 C16 Tm1 59.43(18) . . ?
C17 C16 Tm1 170.8(2) . . ?
C23 O3A Tm1 139.9(14) . . ?
C23 O3B Tm1 102.6(16) . . ?
N2 C10 C9 122.3(3) . . ?
N2 C10 C11 116.8(3) . . ?
C9 C10 C11 121.0(3) . . ?
C3 C4 C5 118.7(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C18 C17 C22 118.3(4) . . ?
C18 C17 C16 120.6(3) . . ?
C22 C17 C16 121.0(3) . . ?
N1 C5 C4 122.3(4) . . ?
N1 C5 C6 116.6(3) . . ?
C4 C5 C6 121.1(3) . . ?
N3 C11 C12 122.2(4) . . ?
N3 C11 C10 115.7(3) . . ?
C12 C11 C10 122.1(3) . . ?
C13 C14 C15 118.8(4) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C20 C21 C22 119.3(4) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
C21 C22 C17 121.2(4) . . ?
C21 C22 H22 119.4 . . ?
C17 C22 H22 119.4 . . ?
C21 C20 C19 120.8(4) . . ?
C21 C20 I1 119.5(3) . . ?
C19 C20 I1 119.6(3) . . ?
N1 C1 C2 123.1(4) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C20 C19 C18 119.4(4) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C13 C12 C11 118.8(4) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C8 C7 C6 118.8(4) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C8 C9 C10 118.7(4) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
N2 C6 C7 122.6(3) . . ?
N2 C6 C5 116.4(3) . . ?
C7 C6 C5 121.0(3) . . ?
N3 C15 C14 123.1(4) . . ?
N3 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C17 C18 C19 121.0(4) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C14 C13 C12 119.2(4) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C25 C24 C29 117.3(5) . . ?
C25 C24 C23 121.1(6) . . ?
C29 C24 C23 121.5(6) . . ?
C7 C8 C9 119.7(4) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C24 C25 C26 121.2(5) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C3 C2 C1 119.5(4) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 119.1(4) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
O6 C30 O5 126.2(3) 2_566 . ?
O6 C30 C30 117.5(4) 2_566 2_566 ?
O5 C30 C30 116.3(4) . 2_566 ?
C24 C29 C28 120.1(6) . . ?
C24 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C27 C28 C29 119.6(6) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C27 C26 C25 120.2(7) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C28 121.5(6) . . ?
C26 C27 I2B 141.1(7) . . ?
C28 C27 I2B 97.2(6) . . ?
C26 C27 I2A 111.9(7) . . ?
C28 C27 I2A 126.6(6) . . ?
C23 O4B Tm1 103.3(9) . . ?
O3A C23 O4A 124.7(11) . . ?
O3A C23 C24 127.7(12) . . ?
O4B C23 C24 146.2(10) . . ?
O4A C23 C24 107.4(8) . . ?
O4B C23 O3B 100.2(12) . . ?
C24 C23 O3B 108.3(9) . . ?

_refine_diff_density_max         1.776
_refine_diff_density_min         -1.472
_refine_diff_density_rms         0.107

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_14Prime
_database_code_depnum_ccdc_archive 'CCDC 1514996'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H25 I3 Lu N3 O7'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Rod
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293
_chemical_formula_weight         1167.26

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'
I I -0.4742 1.8119 '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      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                   8.7900(13)
_cell_length_b                   13.516(2)
_cell_length_c                   15.488(2)
_cell_angle_alpha                103.430(3)
_cell_angle_beta                 91.225(2)
_cell_angle_gamma                93.761(2)
_cell_volume                     1784.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25017
_cell_measurement_theta_min      4.573
_cell_measurement_theta_max      57.588
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.172
_exptl_crystal_F_000             1096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.153
_exptl_absorpt_coefficient_mu    5.413
_shelx_estimated_absorpt_T_min   0.312
_shelx_estimated_absorpt_T_max   0.491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4426
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25003
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.353
_diffrn_reflns_theta_max         28.794
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             9170
_reflns_number_gt                8240
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0171P)²+4.1602P] 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         9170
_refine_ls_number_parameters     459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0631
_refine_ls_wR_factor_gt          0.0611
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.002
_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
C15 C 0.8613(4) 0.4219(3) 0.1608(2) 0.0315(7) Uani 1 1 d . . . . .
H15 H 0.8537 0.4513 0.1123 0.038 Uiso 1 1 calc R U . . .
C14 C 0.9913(4) 0.3732(3) 0.1717(3) 0.0364(8) Uani 1 1 d . . . . .
H14 H 1.0696 0.3706 0.1320 0.044 Uiso 1 1 calc R U . . .
C13 C 1.0021(4) 0.3284(3) 0.2427(3) 0.0383(9) Uani 1 1 d . . . . .
H13 H 1.0889 0.2962 0.2525 0.046 Uiso 1 1 calc R U . . .
C12 C 0.8815(4) 0.3321(3) 0.2994(3) 0.0349(8) Uani 1 1 d . . . . .
H12 H 0.8856 0.3009 0.3470 0.042 Uiso 1 1 calc R U . . .
C11 C 0.7543(4) 0.3827(3) 0.2846(2) 0.0267(7) Uani 1 1 d . . . . .
C10 C 0.6197(4) 0.3874(3) 0.3412(2) 0.0296(7) Uani 1 1 d . . . . .
C9 C 0.6070(5) 0.3323(4) 0.4062(3) 0.0509(12) Uani 1 1 d . . . . .
H9 H 0.6840 0.2915 0.4155 0.061 Uiso 1 1 calc R U . . .
C8 C 0.4804(6) 0.3384(5) 0.4567(4) 0.0655(16) Uani 1 1 d . . . . .
H8 H 0.4715 0.3025 0.5011 0.079 Uiso 1 1 calc R U . . .
C7 C 0.3663(6) 0.3979(4) 0.4412(3) 0.0562(13) Uani 1 1 d . . . . .
H7 H 0.2794 0.4029 0.4747 0.067 Uiso 1 1 calc R U . . .
C6 C 0.3836(4) 0.4504(3) 0.3744(2) 0.0330(8) Uani 1 1 d . . . . .
C5 C 0.2653(4) 0.5151(3) 0.3530(2) 0.0286(7) Uani 1 1 d . . . . .
C4 C 0.1348(4) 0.5329(3) 0.4026(3) 0.0392(9) Uani 1 1 d . . . . .
H4 H 0.1231 0.5078 0.4533 0.047 Uiso 1 1 calc R U . . .
C3 C 0.0236(4) 0.5880(3) 0.3761(3) 0.0400(9) Uani 1 1 d . . . . .
H3 H -0.0650 0.5986 0.4076 0.048 Uiso 1 1 calc R U . . .
C2 C 0.0450(4) 0.6273(3) 0.3025(3) 0.0380(9) Uani 1 1 d . . . . .
H2 H -0.0289 0.6641 0.2828 0.046 Uiso 1 1 calc R U . . .
C1 C 0.1802(4) 0.6102(3) 0.2585(2) 0.0329(8) Uani 1 1 d . . . . .
H1 H 0.1969 0.6388 0.2101 0.040 Uiso 1 1 calc R U . . .
C16 C 0.4435(4) 0.3362(3) 0.0864(2) 0.0270(7) Uani 1 1 d . . . . .
C17 C 0.3981(4) 0.2311(3) 0.0320(2) 0.0284(7) Uani 1 1 d . . . . .
C18 C 0.2787(5) 0.1733(3) 0.0579(3) 0.0470(10) Uani 1 1 d . . . . .
H18 H 0.2257 0.2004 0.1082 0.056 Uiso 1 1 calc R U . . .
C19 C 0.2385(6) 0.0750(3) 0.0084(3) 0.0527(12) Uani 1 1 d . . . . .
H19 H 0.1587 0.0361 0.0256 0.063 Uiso 1 1 calc R U . . .
C20 C 0.3172(5) 0.0353(3) -0.0663(3) 0.0458(10) Uani 1 1 d . . . . .
C21 C 0.4357(6) 0.0921(3) -0.0926(3) 0.0535(12) Uani 1 1 d . . . . .
H21 H 0.4893 0.0643 -0.1425 0.064 Uiso 1 1 calc R U . . .
C22 C 0.4751(5) 0.1916(3) -0.0439(3) 0.0441(10) Uani 1 1 d . . . . .
H22 H 0.5527 0.2311 -0.0625 0.053 Uiso 1 1 calc R U . . .
C23 C 0.5869(4) 0.7179(3) 0.3110(2) 0.0292(7) Uani 1 1 d . . . . .
C24 C 0.6328(4) 0.8216(3) 0.3676(2) 0.0299(7) Uani 1 1 d . . . . .
C25 C 0.7484(4) 0.8359(3) 0.4329(3) 0.0353(8) Uani 1 1 d . . . . .
H25 H 0.7949 0.7798 0.4433 0.042 Uiso 1 1 calc R U . . .
C26 C 0.7953(5) 0.9325(3) 0.4826(3) 0.0372(8) Uani 1 1 d . . . . .
H26 H 0.8737 0.9413 0.5256 0.045 Uiso 1 1 calc R U . . .
C27 C 0.7248(5) 1.0152(3) 0.4677(3) 0.0366(8) Uani 1 1 d . . . . .
C28 C 0.6095(5) 1.0037(3) 0.4031(3) 0.0416(9) Uani 1 1 d . . . . .
H28 H 0.5636 1.0603 0.3930 0.050 Uiso 1 1 calc R U . . .
C29 C 0.5635(5) 0.9067(3) 0.3538(3) 0.0376(8) Uani 1 1 d . . . . .
H29 H 0.4852 0.8982 0.3108 0.045 Uiso 1 1 calc R U . . .
C30 C 0.8065(4) 0.6311(3) 0.0785(2) 0.0271(7) Uani 1 1 d . . . . .
C31 C 0.9002(4) 0.7300(3) 0.1187(2) 0.0285(7) Uani 1 1 d . . . . .
C32 C 1.0429(5) 0.7503(3) 0.0882(3) 0.0450(10) Uani 1 1 d . . . . .
H32 H 1.0812 0.7037 0.0413 0.054 Uiso 1 1 calc R U . . .
C33 C 1.1298(5) 0.8405(4) 0.1273(3) 0.0521(12) Uani 1 1 d . . . . .
H33 H 1.2257 0.8542 0.1067 0.063 Uiso 1 1 calc R U . . .
C34 C 1.0720(5) 0.9087(3) 0.1966(3) 0.0376(8) Uani 1 1 d . . . . .
C35 C 0.9281(5) 0.8911(3) 0.2264(3) 0.0430(9) Uani 1 1 d . . . . .
H35 H 0.8888 0.9385 0.2725 0.052 Uiso 1 1 calc R U . . .
C36 C 0.8437(5) 0.8017(3) 0.1864(3) 0.0381(9) Uani 1 1 d . . . . .
H36 H 0.7463 0.7895 0.2056 0.046 Uiso 1 1 calc R U . . .
N3 N 0.7451(3) 0.4293(2) 0.21672(18) 0.0255(6) Uani 1 1 d . . . . .
N2 N 0.5095(3) 0.4460(2) 0.32562(17) 0.0244(5) Uani 1 1 d . . . . .
N1 N 0.2878(3) 0.5551(2) 0.28199(19) 0.0277(6) Uani 1 1 d . . . . .
O1 O 0.3775(3) 0.37015(19) 0.15785(16) 0.0330(5) Uani 1 1 d . . . . .
O2 O 0.5488(3) 0.38998(19) 0.06164(16) 0.0322(5) Uani 1 1 d . . . . .
O3 O 0.6502(3) 0.64073(19) 0.32537(17) 0.0350(6) Uani 1 1 d . . . . .
O4 O 0.4912(3) 0.7089(2) 0.24777(17) 0.0340(6) Uani 1 1 d . . . . .
O5 O 0.7006(3) 0.6049(2) 0.12519(17) 0.0351(6) Uani 1 1 d . . . . .
O6 O 0.8383(3) 0.5825(2) 0.00388(17) 0.0406(6) Uani 1 1 d . . . . .
OW1 O 0.3599(3) 0.5619(2) 0.09014(17) 0.0299(5) Uani 1 1 d . . . . .
I1 I 0.25286(5) -0.11146(2) -0.14189(3) 0.07994(13) Uani 1 1 d . . . . .
I2 I 0.79679(3) 1.16094(2) 0.54442(2) 0.04808(8) Uani 1 1 d . . . . .
I3 I 1.20467(4) 1.04333(2) 0.25744(2) 0.05563(9) Uani 1 1 d . . . . .
Lu1 Lu 0.52553(2) 0.52895(2) 0.19504(2) 0.02204(4) Uani 1 1 d . . . . .
HW1B H 0.400(6) 0.586(4) 0.055(3) 0.047(14) Uiso 1 1 d . . . . .
HW1A H 0.296(6) 0.519(4) 0.062(3) 0.057(15) Uiso 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
C15 N3 1.347(4) . ?
C15 C14 1.382(5) . ?
C15 H15 0.9300 . ?
C14 C13 1.377(6) . ?
C14 H14 0.9300 . ?
C13 C12 1.387(5) . ?
C13 H13 0.9300 . ?
C12 C11 1.391(5) . ?
C12 H12 0.9300 . ?
C11 N3 1.348(4) . ?
C11 C10 1.485(5) . ?
C10 N2 1.343(5) . ?
C10 C9 1.386(5) . ?
C9 C8 1.370(6) . ?
C9 H9 0.9300 . ?
C8 C7 1.377(7) . ?
C8 H8 0.9300 . ?
C7 C6 1.390(6) . ?
C7 H7 0.9300 . ?
C6 N2 1.349(4) . ?
C6 C5 1.482(5) . ?
C5 N1 1.346(4) . ?
C5 C4 1.397(5) . ?
C4 C3 1.379(6) . ?
C4 H4 0.9300 . ?
C3 C2 1.375(6) . ?
C3 H3 0.9300 . ?
C2 C1 1.389(5) . ?
C2 H2 0.9300 . ?
C1 N1 1.336(5) . ?
C1 H1 0.9300 . ?
C16 O2 1.261(4) . ?
C16 O1 1.264(4) . ?
C16 C17 1.498(5) . ?
C16 Lu1 2.794(3) . ?
C17 C22 1.383(5) . ?
C17 C18 1.388(5) . ?
C18 C19 1.390(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.377(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.379(7) . ?
C20 I1 2.090(4) . ?
C21 C22 1.398(6) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O4 1.255(4) . ?
C23 O3 1.275(4) . ?
C23 C24 1.496(5) . ?
C23 Lu1 2.772(3) . ?
C24 C25 1.389(5) . ?
C24 C29 1.393(5) . ?
C25 C26 1.384(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.376(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.384(6) . ?
C27 I2 2.101(4) . ?
C28 C29 1.385(5) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 O6 1.237(4) . ?
C30 O5 1.273(4) . ?
C30 C31 1.517(5) . ?
C31 C36 1.378(5) . ?
C31 C32 1.382(5) . ?
C32 C33 1.398(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.372(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.381(6) . ?
C34 I3 2.106(4) . ?
C35 C36 1.383(6) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N3 Lu1 2.486(3) . ?
N2 Lu1 2.532(3) . ?
N1 Lu1 2.510(3) . ?
O1 Lu1 2.379(2) . ?
O2 Lu1 2.471(2) . ?
O3 Lu1 2.415(3) . ?
O4 Lu1 2.421(3) . ?
O5 Lu1 2.230(2) . ?
OW1 Lu1 2.297(3) . ?
OW1 HW1B 0.78(5) . ?
OW1 HW1A 0.82(5) . ?

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
N3 C15 C14 123.5(3) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
C13 C14 C15 118.4(3) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C14 C13 C12 119.1(4) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C12 C11 119.3(4) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
N3 C11 C12 121.8(3) . . ?
N3 C11 C10 115.9(3) . . ?
C12 C11 C10 122.2(3) . . ?
N2 C10 C9 121.5(3) . . ?
N2 C10 C11 117.0(3) . . ?
C9 C10 C11 121.5(3) . . ?
C8 C9 C10 119.6(4) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C9 C8 C7 119.5(4) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C7 C6 118.6(4) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
N2 C6 C7 122.0(4) . . ?
N2 C6 C5 116.1(3) . . ?
C7 C6 C5 121.9(3) . . ?
N1 C5 C4 121.0(3) . . ?
N1 C5 C6 116.8(3) . . ?
C4 C5 C6 122.2(3) . . ?
C3 C4 C5 119.6(4) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C2 C3 C4 119.4(3) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C3 C2 C1 117.9(4) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
N1 C1 C2 123.6(4) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
O2 C16 O1 120.1(3) . . ?
O2 C16 C17 120.0(3) . . ?
O1 C16 C17 119.8(3) . . ?
O2 C16 Lu1 62.15(18) . . ?
O1 C16 Lu1 57.98(17) . . ?
C17 C16 Lu1 177.3(2) . . ?
C22 C17 C18 120.1(4) . . ?
C22 C17 C16 120.0(3) . . ?
C18 C17 C16 119.9(3) . . ?
C17 C18 C19 119.9(4) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 119.9(4) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 120.7(4) . . ?
C19 C20 I1 119.6(3) . . ?
C21 C20 I1 119.7(3) . . ?
C20 C21 C22 119.7(4) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C17 C22 C21 119.7(4) . . ?
C17 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
O4 C23 O3 121.2(3) . . ?
O4 C23 C24 119.3(3) . . ?
O3 C23 C24 119.4(3) . . ?
O4 C23 Lu1 60.76(18) . . ?
O3 C23 Lu1 60.51(18) . . ?
C24 C23 Lu1 174.2(2) . . ?
C25 C24 C29 118.5(3) . . ?
C25 C24 C23 121.1(3) . . ?
C29 C24 C23 120.3(3) . . ?
C26 C25 C24 121.0(4) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C27 C26 C25 119.2(4) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C26 C27 C28 121.3(4) . . ?
C26 C27 I2 118.6(3) . . ?
C28 C27 I2 120.1(3) . . ?
C27 C28 C29 118.9(4) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C28 C29 C24 121.0(4) . . ?
C28 C29 H29 119.5 . . ?
C24 C29 H29 119.5 . . ?
O6 C30 O5 125.3(3) . . ?
O6 C30 C31 118.2(3) . . ?
O5 C30 C31 116.6(3) . . ?
C36 C31 C32 118.8(3) . . ?
C36 C31 C30 120.2(3) . . ?
C32 C31 C30 121.0(3) . . ?
C31 C32 C33 120.5(4) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C34 C33 C32 119.2(4) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C33 C34 C35 121.2(4) . . ?
C33 C34 I3 119.3(3) . . ?
C35 C34 I3 119.5(3) . . ?
C34 C35 C36 118.6(4) . . ?
C34 C35 H35 120.7 . . ?
C36 C35 H35 120.7 . . ?
C31 C36 C35 121.7(4) . . ?
C31 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
C15 N3 C11 117.8(3) . . ?
C15 N3 Lu1 120.2(2) . . ?
C11 N3 Lu1 122.0(2) . . ?
C10 N2 C6 118.8(3) . . ?
C10 N2 Lu1 120.0(2) . . ?
C6 N2 Lu1 120.9(2) . . ?
C1 N1 C5 118.4(3) . . ?
C1 N1 Lu1 120.1(2) . . ?
C5 N1 Lu1 121.6(2) . . ?
C16 O1 Lu1 95.2(2) . . ?
C16 O2 Lu1 91.0(2) . . ?
C23 O3 Lu1 92.1(2) . . ?
C23 O4 Lu1 92.3(2) . . ?
C30 O5 Lu1 169.1(2) . . ?
Lu1 OW1 HW1B 114(4) . . ?
Lu1 OW1 HW1A 123(4) . . ?
HW1B OW1 HW1A 105(5) . . ?
O5 Lu1 OW1 83.88(10) . . ?
O5 Lu1 O1 134.10(9) . . ?
OW1 Lu1 O1 80.57(10) . . ?
O5 Lu1 O3 82.69(9) . . ?
OW1 Lu1 O3 130.86(9) . . ?
O1 Lu1 O3 138.03(9) . . ?
O5 Lu1 O4 75.97(9) . . ?
OW1 Lu1 O4 76.65(9) . . ?
O1 Lu1 O4 139.57(9) . . ?
O3 Lu1 O4 54.25(9) . . ?
O5 Lu1 O2 80.70(9) . . ?
OW1 Lu1 O2 74.83(9) . . ?
O1 Lu1 O2 53.60(8) . . ?
O3 Lu1 O2 147.36(9) . . ?
O4 Lu1 O2 144.70(8) . . ?
O5 Lu1 N3 81.24(10) . . ?
OW1 Lu1 N3 143.78(9) . . ?
O1 Lu1 N3 86.47(9) . . ?
O3 Lu1 N3 79.57(9) . . ?
O4 Lu1 N3 130.22(9) . . ?
O2 Lu1 N3 70.28(9) . . ?
O5 Lu1 N1 144.03(10) . . ?
OW1 Lu1 N1 79.31(10) . . ?
O1 Lu1 N1 73.94(9) . . ?
O3 Lu1 N1 84.68(9) . . ?
O4 Lu1 N1 69.33(9) . . ?
O2 Lu1 N1 124.09(9) . . ?
N3 Lu1 N1 129.08(9) . . ?
O5 Lu1 N2 139.10(10) . . ?
OW1 Lu1 N2 137.03(10) . . ?
O1 Lu1 N2 68.34(9) . . ?
O3 Lu1 N2 69.89(9) . . ?
O4 Lu1 N2 108.54(9) . . ?
O2 Lu1 N2 106.47(9) . . ?
N3 Lu1 N2 64.75(9) . . ?
N1 Lu1 N2 64.35(9) . . ?
O5 Lu1 C23 77.08(10) . . ?
OW1 Lu1 C23 103.49(11) . . ?
O1 Lu1 C23 148.62(9) . . ?
O3 Lu1 C23 27.37(10) . . ?
O4 Lu1 C23 26.90(10) . . ?
O2 Lu1 C23 157.75(9) . . ?
N3 Lu1 C23 105.04(10) . . ?
N1 Lu1 C23 76.30(9) . . ?
N2 Lu1 C23 89.96(10) . . ?
O5 Lu1 C16 107.45(10) . . ?
OW1 Lu1 C16 76.39(10) . . ?
O1 Lu1 C16 26.78(9) . . ?
O3 Lu1 C16 152.48(9) . . ?
O4 Lu1 C16 152.24(9) . . ?
O2 Lu1 C16 26.82(9) . . ?
N3 Lu1 C16 76.93(9) . . ?
N1 Lu1 C16 99.19(10) . . ?
N2 Lu1 C16 87.12(9) . . ?
C23 Lu1 C16 175.38(10) . . ?

_refine_diff_density_max         1.201
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.107

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_13Prime
_database_code_depnum_ccdc_archive 'CCDC 1514994'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H25 I3 N3 O7 Yb'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293
_chemical_formula_weight         1165.33

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'
I I -0.4742 1.8119 '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      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                   8.7843(5)
_cell_length_b                   13.5206(7)
_cell_length_c                   15.4808(8)
_cell_angle_alpha                103.4710(10)
_cell_angle_beta                 91.1970(11)
_cell_angle_gamma                93.7450(12)
_cell_volume                     1783.00(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25201
_cell_measurement_theta_min      4.575
_cell_measurement_theta_max      57.599
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.171
_exptl_crystal_F_000             1094
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.105
_exptl_absorpt_coefficient_mu    5.273
_shelx_estimated_absorpt_T_min   0.358
_shelx_estimated_absorpt_T_max   0.607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5690
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25200
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.354
_diffrn_reflns_theta_max         28.810
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9219
_reflns_number_gt                7792
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0403P)²+1.3671P] 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         9219
_refine_ls_number_parameters     459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0785
_refine_ls_wR_factor_gt          0.0731
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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
Yb1 Yb 0.97418(2) 0.47128(2) 0.30490(2) 0.02465(5) Uani 1 1 d . . . . .
I2 I 1.24742(6) 1.11128(3) 0.64243(3) 0.08399(14) Uani 1 1 d . . . . .
I1 I 0.70320(4) -0.16092(2) -0.04469(2) 0.05385(9) Uani 1 1 d . . . . .
O5 O 0.7982(3) 0.3952(2) 0.37511(18) 0.0385(6) Uani 1 1 d . . . . .
O3 O 1.1227(3) 0.6306(2) 0.34207(17) 0.0358(6) Uani 1 1 d . . . . .
OW1 O 1.1407(3) 0.4380(2) 0.40996(18) 0.0327(6) Uani 1 1 d . . . . .
O2 O 0.8499(3) 0.3589(2) 0.17479(17) 0.0376(6) Uani 1 1 d . . . . .
O4 O 0.9509(3) 0.6104(2) 0.43833(16) 0.0343(6) Uani 1 1 d . . . . .
O6 O 0.6601(3) 0.4173(2) 0.49652(18) 0.0450(7) Uani 1 1 d . . . . .
N2 N 0.9902(3) 0.5547(2) 0.17384(18) 0.0278(6) Uani 1 1 d . . . . .
O1 O 1.0084(3) 0.2906(2) 0.25208(17) 0.0371(6) Uani 1 1 d . . . . .
N1 N 1.2123(3) 0.4455(2) 0.2175(2) 0.0303(6) Uani 1 1 d . . . . .
N3 N 0.7539(3) 0.5715(2) 0.28309(19) 0.0289(6) Uani 1 1 d . . . . .
C23 C 1.0567(4) 0.6648(3) 0.4135(2) 0.0295(7) Uani 1 1 d . . . . .
C19 C 0.7042(5) 0.0675(3) 0.0173(3) 0.0411(9) Uani 1 1 d . . . . .
H19 H 0.6257 0.0588 -0.0256 0.049 Uiso 1 1 calc R U . . .
C20 C 0.7754(5) -0.0157(3) 0.0323(3) 0.0396(9) Uani 1 1 d . . . . .
C29 C 1.2219(6) 0.8271(3) 0.4420(3) 0.0509(11) Uani 1 1 d . . . . .
H29 H 1.2754 0.8000 0.3918 0.061 Uiso 1 1 calc R U . . .
C27 C 1.1824(6) 0.9645(3) 0.5665(3) 0.0484(11) Uani 1 1 d . . . . .
C24 C 1.1012(4) 0.7693(3) 0.4681(2) 0.0321(8) Uani 1 1 d . . . . .
C10 C 0.8797(4) 0.6130(3) 0.1581(2) 0.0322(8) Uani 1 1 d . . . . .
C18 C 0.7520(5) 0.1641(3) 0.0675(3) 0.0376(8) Uani 1 1 d . . . . .
H18 H 0.7057 0.2204 0.0573 0.045 Uiso 1 1 calc R U . . .
C32 C 0.4566(5) 0.2499(4) 0.4126(3) 0.0495(11) Uani 1 1 d . . . . .
H32 H 0.4191 0.2960 0.4604 0.059 Uiso 1 1 calc R U . . .
C11 C 0.7447(4) 0.6176(3) 0.2149(2) 0.0295(7) Uani 1 1 d . . . . .
C5 C 1.2346(4) 0.4850(3) 0.1468(2) 0.0323(8) Uani 1 1 d . . . . .
C31 C 0.5994(4) 0.2702(3) 0.3812(2) 0.0323(8) Uani 1 1 d . . . . .
C12 C 0.6180(5) 0.6686(3) 0.1998(3) 0.0388(9) Uani 1 1 d . . . . .
H12 H 0.6138 0.6998 0.1524 0.047 Uiso 1 1 calc R U . . .
C6 C 1.1168(4) 0.5498(3) 0.1257(2) 0.0358(8) Uani 1 1 d . . . . .
C22 C 0.9362(5) 0.0934(3) 0.1467(3) 0.0415(9) Uani 1 1 d . . . . .
H22 H 1.0133 0.1018 0.1904 0.050 Uiso 1 1 calc R U . . .
C3 C 1.4756(5) 0.4123(3) 0.1232(3) 0.0465(11) Uani 1 1 d . . . . .
H3 H 1.5641 0.4017 0.0914 0.056 Uiso 1 1 calc R U . . .
C15 C 0.6383(4) 0.5785(3) 0.3383(3) 0.0359(8) Uani 1 1 d . . . . .
H15 H 0.6458 0.5489 0.3866 0.043 Uiso 1 1 calc R U . . .
C30 C 0.6925(4) 0.3682(3) 0.4216(2) 0.0304(7) Uani 1 1 d . . . . .
C1 C 1.3194(4) 0.3892(3) 0.2407(3) 0.0372(8) Uani 1 1 d . . . . .
H1 H 1.3023 0.3599 0.2887 0.045 Uiso 1 1 calc R U . . .
C16 C 0.9124(4) 0.2818(3) 0.1896(2) 0.0310(8) Uani 1 1 d . . . . .
C36 C 0.6550(5) 0.1992(3) 0.3136(3) 0.0435(10) Uani 1 1 d . . . . .
H36 H 0.7522 0.2115 0.2940 0.052 Uiso 1 1 calc R U . . .
C14 C 0.5075(5) 0.6275(3) 0.3276(3) 0.0397(9) Uani 1 1 d . . . . .
H14 H 0.4288 0.6300 0.3672 0.048 Uiso 1 1 calc R U . . .
C17 C 0.8672(4) 0.1780(3) 0.1323(2) 0.0322(8) Uani 1 1 d . . . . .
C2 C 1.4543(5) 0.3726(3) 0.1966(3) 0.0414(9) Uani 1 1 d . . . . .
H2 H 1.5284 0.3358 0.2161 0.050 Uiso 1 1 calc R U . . .
I3 I 0.29497(4) -0.04329(3) 0.24241(2) 0.06044(10) Uani 1 1 d . . . . .
C34 C 0.4271(5) 0.0913(3) 0.3031(3) 0.0414(9) Uani 1 1 d . . . . .
C35 C 0.5705(5) 0.1091(3) 0.2736(3) 0.0468(10) Uani 1 1 d . . . . .
H35 H 0.6102 0.0617 0.2277 0.056 Uiso 1 1 calc R U . . .
C25 C 1.0259(5) 0.8086(3) 0.5438(3) 0.0462(10) Uani 1 1 d . . . . .
H25 H 0.9487 0.7689 0.5624 0.055 Uiso 1 1 calc R U . . .
C13 C 0.4980(5) 0.6718(3) 0.2569(3) 0.0433(10) Uani 1 1 d . . . . .
H13 H 0.4112 0.7042 0.2472 0.052 Uiso 1 1 calc R U . . .
C4 C 1.3648(5) 0.4676(3) 0.0972(3) 0.0448(10) Uani 1 1 d . . . . .
H4 H 1.3767 0.4934 0.0469 0.054 Uiso 1 1 calc R U . . .
C33 C 0.3696(5) 0.1606(4) 0.3728(4) 0.0584(13) Uani 1 1 d . . . . .
H33 H 0.2731 0.1475 0.3930 0.070 Uiso 1 1 calc R U . . .
C26 C 1.0645(6) 0.9079(4) 0.5929(3) 0.0560(12) Uani 1 1 d . . . . .
H26 H 1.0109 0.9355 0.6429 0.067 Uiso 1 1 calc R U . . .
C21 C 0.8908(5) -0.0038(3) 0.0962(3) 0.0460(10) Uani 1 1 d . . . . .
H21 H 0.9381 -0.0602 0.1055 0.055 Uiso 1 1 calc R U . . .
C9 C 0.8936(6) 0.6681(4) 0.0935(3) 0.0534(12) Uani 1 1 d . . . . .
H9 H 0.8167 0.7091 0.0843 0.064 Uiso 1 1 calc R U . . .
C8 C 1.0190(6) 0.6626(5) 0.0435(4) 0.0686(16) Uani 1 1 d . . . . .
H8 H 1.0276 0.6986 -0.0007 0.082 Uiso 1 1 calc R U . . .
C28 C 1.2608(6) 0.9248(3) 0.4917(3) 0.0569(13) Uani 1 1 d . . . . .
H28 H 1.3404 0.9640 0.4744 0.068 Uiso 1 1 calc R U . . .
C7 C 1.1337(6) 0.6031(4) 0.0590(4) 0.0612(14) Uani 1 1 d . . . . .
H7 H 1.2207 0.5986 0.0255 0.073 Uiso 1 1 calc R U . . .
HW1A H 1.108(6) 0.418(4) 0.445(4) 0.061(18) Uiso 1 1 d . . . . .
HW1B H 1.201(6) 0.479(4) 0.435(3) 0.051(15) Uiso 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
Yb1 O5 2.239(2) . ?
Yb1 OW1 2.305(3) . ?
Yb1 O3 2.387(3) . ?
Yb1 O2 2.413(3) . ?
Yb1 O1 2.429(3) . ?
Yb1 O4 2.471(2) . ?
Yb1 N3 2.495(3) . ?
Yb1 N1 2.514(3) . ?
Yb1 N2 2.543(3) . ?
Yb1 C16 2.773(3) . ?
Yb1 C23 2.802(3) . ?
Yb1 HW1A 2.71(6) . ?
I2 C27 2.094(4) . ?
I1 C20 2.096(4) . ?
O5 C30 1.273(4) . ?
O3 C23 1.263(4) . ?
OW1 HW1A 0.72(6) . ?
OW1 HW1B 0.77(5) . ?
O2 C16 1.274(5) . ?
O4 C23 1.269(4) . ?
O6 C30 1.243(4) . ?
N2 C10 1.341(5) . ?
N2 C6 1.349(4) . ?
O1 C16 1.248(4) . ?
N1 C5 1.338(5) . ?
N1 C1 1.342(5) . ?
N3 C15 1.335(5) . ?
N3 C11 1.349(5) . ?
C23 C24 1.491(5) . ?
C19 C20 1.385(6) . ?
C19 C18 1.388(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.376(6) . ?
C29 C28 1.383(6) . ?
C29 C24 1.397(6) . ?
C29 H29 0.9300 . ?
C27 C26 1.373(7) . ?
C27 C28 1.377(7) . ?
C24 C25 1.370(5) . ?
C10 C9 1.382(5) . ?
C10 C11 1.487(5) . ?
C18 C17 1.382(5) . ?
C18 H18 0.9300 . ?
C32 C31 1.389(5) . ?
C32 C33 1.391(6) . ?
C32 H32 0.9300 . ?
C11 C12 1.390(5) . ?
C5 C4 1.393(5) . ?
C5 C6 1.477(6) . ?
C31 C36 1.367(5) . ?
C31 C30 1.506(5) . ?
C12 C13 1.385(6) . ?
C12 H12 0.9300 . ?
C6 C7 1.396(6) . ?
C22 C17 1.388(6) . ?
C22 C21 1.393(6) . ?
C22 H22 0.9300 . ?
C3 C4 1.373(6) . ?
C3 C2 1.377(6) . ?
C3 H3 0.9300 . ?
C15 C14 1.389(6) . ?
C15 H15 0.9300 . ?
C1 C2 1.384(6) . ?
C1 H1 0.9300 . ?
C16 C17 1.500(5) . ?
C36 C35 1.390(6) . ?
C36 H36 0.9300 . ?
C14 C13 1.369(6) . ?
C14 H14 0.9300 . ?
C2 H2 0.9300 . ?
I3 C34 2.104(4) . ?
C34 C35 1.374(6) . ?
C34 C33 1.382(6) . ?
C35 H35 0.9300 . ?
C25 C26 1.397(6) . ?
C25 H25 0.9300 . ?
C13 H13 0.9300 . ?
C4 H4 0.9300 . ?
C33 H33 0.9300 . ?
C26 H26 0.9300 . ?
C21 H21 0.9300 . ?
C9 C8 1.355(7) . ?
C9 H9 0.9300 . ?
C8 C7 1.381(7) . ?
C8 H8 0.9300 . ?
C28 H28 0.9300 . ?
C7 H7 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
O5 Yb1 OW1 83.94(11) . . ?
O5 Yb1 O3 134.12(9) . . ?
OW1 Yb1 O3 80.69(10) . . ?
O5 Yb1 O2 82.59(10) . . ?
OW1 Yb1 O2 130.50(10) . . ?
O3 Yb1 O2 138.15(9) . . ?
O5 Yb1 O1 75.93(9) . . ?
OW1 Yb1 O1 76.52(9) . . ?
O3 Yb1 O1 139.63(9) . . ?
O2 Yb1 O1 54.01(9) . . ?
O5 Yb1 O4 80.72(9) . . ?
OW1 Yb1 O4 74.97(9) . . ?
O3 Yb1 O4 53.60(8) . . ?
O2 Yb1 O4 147.53(9) . . ?
O1 Yb1 O4 144.68(9) . . ?
O5 Yb1 N3 81.28(10) . . ?
OW1 Yb1 N3 143.92(10) . . ?
O3 Yb1 N3 86.36(10) . . ?
O2 Yb1 N3 79.82(9) . . ?
O1 Yb1 N3 130.26(9) . . ?
O4 Yb1 N3 70.27(9) . . ?
O5 Yb1 N1 144.23(10) . . ?
OW1 Yb1 N1 79.34(10) . . ?
O3 Yb1 N1 73.83(9) . . ?
O2 Yb1 N1 84.62(9) . . ?
O1 Yb1 N1 69.53(9) . . ?
O4 Yb1 N1 124.02(9) . . ?
N3 Yb1 N1 128.84(10) . . ?
O5 Yb1 N2 139.04(10) . . ?
OW1 Yb1 N2 137.02(10) . . ?
O3 Yb1 N2 68.23(9) . . ?
O2 Yb1 N2 70.14(9) . . ?
O1 Yb1 N2 108.69(9) . . ?
O4 Yb1 N2 106.34(9) . . ?
N3 Yb1 N2 64.60(9) . . ?
N1 Yb1 N2 64.26(10) . . ?
O5 Yb1 C16 76.83(10) . . ?
OW1 Yb1 C16 103.18(11) . . ?
O3 Yb1 C16 148.84(9) . . ?
O2 Yb1 C16 27.32(10) . . ?
O1 Yb1 C16 26.74(10) . . ?
O4 Yb1 C16 157.53(9) . . ?
N3 Yb1 C16 105.17(11) . . ?
N1 Yb1 C16 76.55(10) . . ?
N2 Yb1 C16 90.35(10) . . ?
O5 Yb1 C23 107.58(10) . . ?
OW1 Yb1 C23 76.60(10) . . ?
O3 Yb1 C23 26.67(9) . . ?
O2 Yb1 C23 152.60(10) . . ?
O1 Yb1 C23 152.32(10) . . ?
O4 Yb1 C23 26.93(9) . . ?
N3 Yb1 C23 76.84(10) . . ?
N1 Yb1 C23 99.01(10) . . ?
N2 Yb1 C23 86.88(10) . . ?
C16 Yb1 C23 175.47(10) . . ?
O5 Yb1 HW1A 70.5(12) . . ?
OW1 Yb1 HW1A 13.6(12) . . ?
O3 Yb1 HW1A 89.3(12) . . ?
O2 Yb1 HW1A 127.4(12) . . ?
O1 Yb1 HW1A 75.6(12) . . ?
O4 Yb1 HW1A 71.7(12) . . ?
N3 Yb1 HW1A 135.5(12) . . ?
N1 Yb1 HW1A 91.8(12) . . ?
N2 Yb1 HW1A 150.4(12) . . ?
C16 Yb1 HW1A 101.1(12) . . ?
C23 Yb1 HW1A 79.8(12) . . ?
C30 O5 Yb1 169.7(3) . . ?
C23 O3 Yb1 95.3(2) . . ?
Yb1 OW1 HW1A 118(5) . . ?
Yb1 OW1 HW1B 121(4) . . ?
HW1A OW1 HW1B 102(5) . . ?
C16 O2 Yb1 92.3(2) . . ?
C23 O4 Yb1 91.2(2) . . ?
C10 N2 C6 119.4(3) . . ?
C10 N2 Yb1 120.0(2) . . ?
C6 N2 Yb1 120.2(2) . . ?
C16 O1 Yb1 92.2(2) . . ?
C5 N1 C1 118.5(3) . . ?
C5 N1 Yb1 121.7(2) . . ?
C1 N1 Yb1 119.8(2) . . ?
C15 N3 C11 117.9(3) . . ?
C15 N3 Yb1 120.1(2) . . ?
C11 N3 Yb1 122.0(2) . . ?
O3 C23 O4 119.8(3) . . ?
O3 C23 C24 120.3(3) . . ?
O4 C23 C24 119.8(3) . . ?
O3 C23 Yb1 58.01(18) . . ?
O4 C23 Yb1 61.83(18) . . ?
C24 C23 Yb1 177.8(3) . . ?
C20 C19 C18 118.9(4) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
C21 C20 C19 121.1(4) . . ?
C21 C20 I1 120.5(3) . . ?
C19 C20 I1 118.4(3) . . ?
C28 C29 C24 119.3(4) . . ?
C28 C29 H29 120.4 . . ?
C24 C29 H29 120.4 . . ?
C26 C27 C28 120.7(4) . . ?
C26 C27 I2 119.7(3) . . ?
C28 C27 I2 119.6(4) . . ?
C25 C24 C29 120.0(4) . . ?
C25 C24 C23 120.6(4) . . ?
C29 C24 C23 119.3(3) . . ?
N2 C10 C9 121.1(4) . . ?
N2 C10 C11 117.0(3) . . ?
C9 C10 C11 121.8(4) . . ?
C17 C18 C19 121.2(4) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C31 C32 C33 120.0(4) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
N3 C11 C12 122.0(3) . . ?
N3 C11 C10 116.0(3) . . ?
C12 C11 C10 122.0(3) . . ?
N1 C5 C4 121.2(4) . . ?
N1 C5 C6 116.7(3) . . ?
C4 C5 C6 122.0(4) . . ?
C36 C31 C32 118.9(4) . . ?
C36 C31 C30 120.5(3) . . ?
C32 C31 C30 120.6(3) . . ?
C13 C12 C11 118.7(4) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
N2 C6 C7 121.0(4) . . ?
N2 C6 C5 116.8(3) . . ?
C7 C6 C5 122.2(4) . . ?
C17 C22 C21 120.5(4) . . ?
C17 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C4 C3 C2 119.4(4) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
N3 C15 C14 123.7(4) . . ?
N3 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
O6 C30 O5 124.9(3) . . ?
O6 C30 C31 118.4(3) . . ?
O5 C30 C31 116.7(3) . . ?
N1 C1 C2 123.2(4) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
O1 C16 O2 121.4(3) . . ?
O1 C16 C17 119.3(3) . . ?
O2 C16 C17 119.3(3) . . ?
O1 C16 Yb1 61.11(19) . . ?
O2 C16 Yb1 60.41(18) . . ?
C17 C16 Yb1 174.9(2) . . ?
C31 C36 C35 121.8(4) . . ?
C31 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
C13 C14 C15 117.8(4) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 H14 121.1 . . ?
C18 C17 C22 119.0(4) . . ?
C18 C17 C16 120.9(4) . . ?
C22 C17 C16 120.0(3) . . ?
C3 C2 C1 118.0(4) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C35 C34 C33 120.6(4) . . ?
C35 C34 I3 119.6(3) . . ?
C33 C34 I3 119.7(3) . . ?
C34 C35 C36 118.7(4) . . ?
C34 C35 H35 120.6 . . ?
C36 C35 H35 120.6 . . ?
C24 C25 C26 120.3(4) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C14 C13 C12 119.9(4) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C34 C33 C32 119.8(4) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C27 C26 C25 119.3(4) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C20 C21 C22 119.4(4) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C8 C9 C10 120.2(4) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C8 C7 119.4(4) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C27 C28 C29 120.3(4) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C8 C7 C6 118.8(4) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?

_refine_diff_density_max         1.637
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.128

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_7
_database_code_depnum_ccdc_archive 'CCDC 1514985'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 Gd2 I6 N6 O14'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2299.08

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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                   11.2083(4)
_cell_length_b                   12.8703(5)
_cell_length_c                   14.5009(6)
_cell_angle_alpha                69.063(2)
_cell_angle_beta                 88.6150(10)
_cell_angle_gamma                72.7400(10)
_cell_volume                     1857.85(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    27866
_cell_measurement_theta_min      4.347
_cell_measurement_theta_max      46.964

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_F_000             1082
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.139
_exptl_absorpt_coefficient_mu    4.328
_shelx_estimated_absorpt_T_min   0.346
_shelx_estimated_absorpt_T_max   0.584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6155
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27861
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.510
_diffrn_reflns_theta_max         30.569
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10456
_reflns_number_gt                7929
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0314P)²+1.0735P] 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         10456
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0867
_refine_ls_wR_factor_gt          0.0786
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9012(4) 0.2193(5) 0.1633(4) 0.0602(13) Uani 1 1 d . . . . .
H1 H 0.8657 0.2992 0.1484 0.072 Uiso 1 1 calc R U . . .
C2 C 1.0013(5) 0.1589(6) 0.2347(5) 0.0849(19) Uani 1 1 d . . . . .
H2 H 1.0336 0.1979 0.2659 0.102 Uiso 1 1 calc R U . . .
C3 C 1.0523(6) 0.0417(6) 0.2589(5) 0.093(2) Uani 1 1 d . . . . .
H3 H 1.1170 -0.0013 0.3093 0.111 Uiso 1 1 calc R U . . .
C4 C 1.0066(5) -0.0127(5) 0.2077(4) 0.0701(16) Uani 1 1 d . . . . .
H4 H 1.0425 -0.0922 0.2212 0.084 Uiso 1 1 calc R U . . .
C5 C 0.9055(4) 0.0535(4) 0.1351(3) 0.0463(11) Uani 1 1 d . . . . .
C6 C 0.8556(4) 0.0027(3) 0.0746(3) 0.0415(10) Uani 1 1 d . . . . .
C7 C 0.9203(4) -0.1068(4) 0.0723(4) 0.0564(13) Uani 1 1 d . . . . .
H7 H 0.9957 -0.1511 0.1113 0.068 Uiso 1 1 calc R U . . .
C8 C 0.8718(5) -0.1489(4) 0.0120(4) 0.0643(15) Uani 1 1 d . . . . .
H8 H 0.9151 -0.2211 0.0087 0.077 Uiso 1 1 calc R U . . .
C9 C 0.7597(5) -0.0840(4) -0.0429(4) 0.0532(12) Uani 1 1 d . . . . .
H9 H 0.7253 -0.1121 -0.0831 0.064 Uiso 1 1 calc R U . . .
C10 C 0.6971(4) 0.0250(3) -0.0382(3) 0.0397(9) Uani 1 1 d . . . . .
C11 C 0.5712(4) 0.0968(3) -0.0915(3) 0.0356(9) Uani 1 1 d . . . . .
C12 C 0.5071(4) 0.0553(4) -0.1427(3) 0.0458(10) Uani 1 1 d . . . . .
H12 H 0.5439 -0.0178 -0.1465 0.055 Uiso 1 1 calc R U . . .
C13 C 0.3893(5) 0.1211(4) -0.1881(3) 0.0515(11) Uani 1 1 d . . . . .
H13 H 0.3449 0.0931 -0.2221 0.062 Uiso 1 1 calc R U . . .
C14 C 0.3383(4) 0.2290(4) -0.1821(3) 0.0495(11) Uani 1 1 d . . . . .
H14 H 0.2589 0.2764 -0.2126 0.059 Uiso 1 1 calc R U . . .
C15 C 0.4071(4) 0.2661(4) -0.1301(3) 0.0487(11) Uani 1 1 d . . . . .
H15 H 0.3715 0.3391 -0.1258 0.058 Uiso 1 1 calc R U . . .
C16 C 0.8116(4) 0.3579(3) -0.1268(3) 0.0382(9) Uani 1 1 d . . . . .
C17 C 0.8998(4) 0.4015(3) -0.1972(3) 0.0374(9) Uani 1 1 d . . . . .
C18 C 0.9762(4) 0.4574(4) -0.1736(3) 0.0456(10) Uani 1 1 d . . . . .
H18 H 0.9690 0.4707 -0.1144 0.055 Uiso 1 1 calc R U . . .
C19 C 1.0629(4) 0.4938(4) -0.2365(4) 0.0518(12) Uani 1 1 d . . . . .
H19 H 1.1149 0.5296 -0.2192 0.062 Uiso 1 1 calc R U . . .
C20 C 1.0711(4) 0.4765(4) -0.3238(4) 0.0515(12) Uani 1 1 d . . . . .
C21 C 0.9968(4) 0.4204(4) -0.3496(3) 0.0548(12) Uani 1 1 d . . . . .
H21 H 1.0047 0.4074 -0.4089 0.066 Uiso 1 1 calc R U . . .
C22 C 0.9107(4) 0.3841(4) -0.2863(3) 0.0469(10) Uani 1 1 d . . . . .
H22 H 0.8595 0.3477 -0.3037 0.056 Uiso 1 1 calc R U . . .
C23 C 0.4850(4) 0.2104(4) 0.1623(3) 0.0401(9) Uani 1 1 d . . . . .
C24 C 0.4095(4) 0.1913(3) 0.2503(3) 0.0380(9) Uani 1 1 d . . . . .
C25 C 0.3075(4) 0.2813(4) 0.2552(4) 0.0509(11) Uani 1 1 d . . . . .
H25 H 0.2843 0.3531 0.2028 0.061 Uiso 1 1 calc R U . . .
C26 C 0.2398(4) 0.2649(5) 0.3379(4) 0.0596(13) Uani 1 1 d . . . . .
H26 H 0.1727 0.3259 0.3418 0.072 Uiso 1 1 calc R U . . .
C27 C 0.2728(5) 0.1583(5) 0.4133(4) 0.0564(12) Uani 1 1 d . . . . .
C28 C 0.3732(5) 0.0669(4) 0.4099(4) 0.0615(14) Uani 1 1 d . . . . .
H28 H 0.3939 -0.0058 0.4612 0.074 Uiso 1 1 calc R U . . .
C29 C 0.4420(4) 0.0856(4) 0.3287(3) 0.0513(11) Uani 1 1 d . . . . .
H29 H 0.5120 0.0256 0.3270 0.062 Uiso 1 1 calc R U . . .
C30 C 0.5588(3) 0.4483(3) 0.1530(3) 0.0315(8) Uani 1 1 d . . . . .
C31 C 0.5634(3) 0.3965(3) 0.2635(3) 0.0325(8) Uani 1 1 d . . . . .
C32 C 0.4846(4) 0.4570(4) 0.3155(3) 0.0421(10) Uani 1 1 d . . . . .
H32 H 0.4259 0.5290 0.2809 0.050 Uiso 1 1 calc R U . . .
C33 C 0.4925(4) 0.4115(4) 0.4178(3) 0.0520(12) Uani 1 1 d . . . . .
H33 H 0.4396 0.4524 0.4522 0.062 Uiso 1 1 calc R U . . .
C34 C 0.5800(5) 0.3043(4) 0.4685(3) 0.0491(11) Uani 1 1 d . . . . .
C35 C 0.6563(5) 0.2418(4) 0.4185(3) 0.0514(12) Uani 1 1 d . . . . .
H35 H 0.7141 0.1693 0.4533 0.062 Uiso 1 1 calc R U . . .
C36 C 0.6466(4) 0.2871(3) 0.3163(3) 0.0443(10) Uani 1 1 d . . . . .
H36 H 0.6964 0.2437 0.2823 0.053 Uiso 1 1 calc R U . . .
N1 N 0.8527(3) 0.1682(3) 0.1145(3) 0.0455(9) Uani 1 1 d . . . . .
N2 N 0.7458(3) 0.0684(3) 0.0189(2) 0.0355(7) Uani 1 1 d . . . . .
N3 N 0.5219(3) 0.2029(3) -0.0855(3) 0.0385(8) Uani 1 1 d . . . . .
O1 O 0.7633(3) 0.2857(2) -0.1378(2) 0.0421(7) Uani 1 1 d . . . . .
O2 O 0.7889(3) 0.3931(3) -0.0555(2) 0.0494(8) Uani 1 1 d . . . . .
O3 O 0.4352(3) 0.2921(3) 0.0810(2) 0.0497(8) Uani 1 1 d . . . . .
O4 O 0.5967(3) 0.1459(2) 0.1706(2) 0.0435(7) Uani 1 1 d . . . . .
O5 O 0.6310(3) 0.3882(2) 0.1101(2) 0.0407(7) Uani 1 1 d . . . . .
O6 O 0.5146(3) 0.4511(2) -0.1097(2) 0.0441(7) Uani 1 1 d . . . . .
OW1 O 0.1875(5) 0.4229(6) -0.0067(4) 0.0877(16) Uani 1 1 d . . . . .
I1 I 1.20498(4) 0.52860(5) -0.41737(3) 0.09389(17) Uani 1 1 d . . . . .
I2 I 0.16923(5) 0.13076(5) 0.53812(4) 0.11152(19) Uani 1 1 d . . . . .
I3A I 0.6155(3) 0.2453(4) 0.6266(2) 0.0686(7) Uani 0.61(3) 1 d . . P A 1
I3B I 0.579(2) 0.2373(5) 0.6188(6) 0.097(2) Uani 0.39(3) 1 d . . P A 2
Gd1 Gd 0.64020(2) 0.28207(2) 0.00921(2) 0.03111(6) Uani 1 1 d . . . . .
HW1A H 0.252(6) 0.382(5) 0.017(5) 0.08(2) Uiso 1 1 d . . . . .
HW1B H 0.172(7) 0.485(7) 0.001(6) 0.13(3) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.338(6) . ?
C1 C2 1.377(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.359(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.381(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.400(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.340(5) . ?
C5 C6 1.470(6) . ?
C6 N2 1.350(5) . ?
C6 C7 1.392(6) . ?
C7 C8 1.375(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.364(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.395(5) . ?
C9 H9 0.9300 . ?
C10 N2 1.351(5) . ?
C10 C11 1.488(6) . ?
C11 N3 1.346(5) . ?
C11 C12 1.374(6) . ?
C12 C13 1.369(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.370(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.376(6) . ?
C14 H14 0.9300 . ?
C15 N3 1.334(5) . ?
C15 H15 0.9300 . ?
C16 O1 1.261(5) . ?
C16 O2 1.262(5) . ?
C16 C17 1.485(6) . ?
C16 Gd1 2.843(4) . ?
C17 C22 1.384(6) . ?
C17 C18 1.387(6) . ?
C18 C19 1.385(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.358(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.385(6) . ?
C20 I1 2.095(4) . ?
C21 C22 1.383(6) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O4 1.261(5) . ?
C23 O3 1.267(5) . ?
C23 C24 1.500(6) . ?
C23 Gd1 2.847(4) . ?
C24 C29 1.377(6) . ?
C24 C25 1.387(6) . ?
C25 C26 1.388(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.365(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.380(7) . ?
C27 I2 2.105(5) . ?
C28 C29 1.379(6) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 O6 1.249(4) 2_665 ?
C30 O5 1.260(4) . ?
C30 C31 1.496(5) . ?
C31 C36 1.387(5) . ?
C31 C32 1.390(5) . ?
C32 C33 1.381(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.383(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.373(6) . ?
C34 I3B 2.039(7) . ?
C34 I3A 2.148(5) . ?
C35 C36 1.378(6) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N1 Gd1 2.580(3) . ?
N2 Gd1 2.605(3) . ?
N3 Gd1 2.563(3) . ?
O1 Gd1 2.505(3) . ?
O2 Gd1 2.466(3) . ?
O3 Gd1 2.487(3) . ?
O4 Gd1 2.511(3) . ?
O5 Gd1 2.313(3) . ?
O6 C30 1.249(4) 2_665 ?
O6 Gd1 2.304(3) . ?
OW1 HW1A 0.76(6) . ?
OW1 HW1B 0.82(8) . ?

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
N1 C1 C2 123.0(5) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 119.1(6) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 119.0(5) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C5 119.2(5) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 121.2(5) . . ?
N1 C5 C6 116.5(4) . . ?
C4 C5 C6 122.2(4) . . ?
N2 C6 C7 121.3(4) . . ?
N2 C6 C5 117.1(4) . . ?
C7 C6 C5 121.6(4) . . ?
C8 C7 C6 119.4(5) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C9 C8 C7 119.5(4) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 119.4(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 121.4(4) . . ?
N2 C10 C11 116.6(3) . . ?
C9 C10 C11 122.0(4) . . ?
N3 C11 C12 121.7(4) . . ?
N3 C11 C10 117.0(4) . . ?
C12 C11 C10 121.3(4) . . ?
C13 C12 C11 120.4(4) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 118.4(4) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C13 C14 C15 118.7(4) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
N3 C15 C14 123.6(4) . . ?
N3 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
O1 C16 O2 121.6(4) . . ?
O1 C16 C17 120.1(4) . . ?
O2 C16 C17 118.3(4) . . ?
O1 C16 Gd1 61.7(2) . . ?
O2 C16 Gd1 59.9(2) . . ?
C17 C16 Gd1 177.9(3) . . ?
C22 C17 C18 118.4(4) . . ?
C22 C17 C16 121.0(4) . . ?
C18 C17 C16 120.6(4) . . ?
C19 C18 C17 121.2(4) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C20 C19 C18 119.2(4) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
C19 C20 C21 121.1(4) . . ?
C19 C20 I1 119.1(3) . . ?
C21 C20 I1 119.7(4) . . ?
C22 C21 C20 119.3(4) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C21 C22 C17 120.7(4) . . ?
C21 C22 H22 119.6 . . ?
C17 C22 H22 119.6 . . ?
O4 C23 O3 121.2(4) . . ?
O4 C23 C24 119.7(4) . . ?
O3 C23 C24 119.1(4) . . ?
O4 C23 Gd1 61.8(2) . . ?
O3 C23 Gd1 60.7(2) . . ?
C24 C23 Gd1 167.8(3) . . ?
C29 C24 C25 118.8(4) . . ?
C29 C24 C23 120.9(4) . . ?
C25 C24 C23 120.4(4) . . ?
C24 C25 C26 120.5(4) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C27 C26 C25 119.3(4) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C26 C27 C28 121.4(4) . . ?
C26 C27 I2 119.8(4) . . ?
C28 C27 I2 118.7(4) . . ?
C29 C28 C27 118.6(5) . . ?
C29 C28 H28 120.7 . . ?
C27 C28 H28 120.7 . . ?
C24 C29 C28 121.4(4) . . ?
C24 C29 H29 119.3 . . ?
C28 C29 H29 119.3 . . ?
O6 C30 O5 124.5(4) 2_665 . ?
O6 C30 C31 117.7(3) 2_665 . ?
O5 C30 C31 117.7(3) . . ?
C36 C31 C32 118.6(4) . . ?
C36 C31 C30 120.6(3) . . ?
C32 C31 C30 120.8(3) . . ?
C33 C32 C31 120.8(4) . . ?
C33 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C32 C33 C34 119.2(4) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 H33 120.4 . . ?
C35 C34 C33 120.9(4) . . ?
C35 C34 I3B 121.8(4) . . ?
C33 C34 I3B 117.1(5) . . ?
C35 C34 I3A 118.8(4) . . ?
C33 C34 I3A 119.7(3) . . ?
C34 C35 C36 119.5(4) . . ?
C34 C35 H35 120.2 . . ?
C36 C35 H35 120.2 . . ?
C35 C36 C31 120.9(4) . . ?
C35 C36 H36 119.6 . . ?
C31 C36 H36 119.6 . . ?
C1 N1 C5 118.3(4) . . ?
C1 N1 Gd1 119.3(3) . . ?
C5 N1 Gd1 121.5(3) . . ?
C6 N2 C10 118.9(3) . . ?
C6 N2 Gd1 120.5(3) . . ?
C10 N2 Gd1 120.4(2) . . ?
C15 N3 C11 117.3(4) . . ?
C15 N3 Gd1 120.5(3) . . ?
C11 N3 Gd1 122.1(3) . . ?
C16 O1 Gd1 92.0(2) . . ?
C16 O2 Gd1 93.8(2) . . ?
C23 O3 Gd1 92.9(2) . . ?
C23 O4 Gd1 91.9(2) . . ?
C30 O5 Gd1 144.6(3) . . ?
C30 O6 Gd1 163.3(3) 2_665 . ?
HW1A OW1 HW1B 111(7) . . ?
O6 Gd1 O5 87.77(9) . . ?
O6 Gd1 O2 77.68(11) . . ?
O5 Gd1 O2 75.91(10) . . ?
O6 Gd1 O3 80.22(10) . . ?
O5 Gd1 O3 74.94(10) . . ?
O2 Gd1 O3 143.82(10) . . ?
O6 Gd1 O1 79.64(10) . . ?
O5 Gd1 O1 128.42(10) . . ?
O2 Gd1 O1 52.59(9) . . ?
O3 Gd1 O1 148.12(10) . . ?
O6 Gd1 O4 132.45(10) . . ?
O5 Gd1 O4 78.69(9) . . ?
O2 Gd1 O4 139.34(10) . . ?
O3 Gd1 O4 52.29(9) . . ?
O1 Gd1 O4 142.51(9) . . ?
O6 Gd1 N3 77.77(10) . . ?
O5 Gd1 N3 147.75(10) . . ?
O2 Gd1 N3 127.26(10) . . ?
O3 Gd1 N3 74.28(10) . . ?
O1 Gd1 N3 77.47(10) . . ?
O4 Gd1 N3 89.98(10) . . ?
O6 Gd1 N1 148.82(12) . . ?
O5 Gd1 N1 79.80(10) . . ?
O2 Gd1 N1 71.60(11) . . ?
O3 Gd1 N1 122.85(11) . . ?
O1 Gd1 N1 85.89(11) . . ?
O4 Gd1 N1 73.05(11) . . ?
N3 Gd1 N1 125.83(11) . . ?
O6 Gd1 N2 134.82(10) . . ?
O5 Gd1 N2 137.41(10) . . ?
O2 Gd1 N2 107.90(10) . . ?
O3 Gd1 N2 108.02(10) . . ?
O1 Gd1 N2 70.90(9) . . ?
O4 Gd1 N2 71.91(9) . . ?
N3 Gd1 N2 63.13(10) . . ?
N1 Gd1 N2 62.70(11) . . ?
O6 Gd1 C16 76.73(11) . . ?
O5 Gd1 C16 102.12(11) . . ?
O2 Gd1 C16 26.28(10) . . ?
O3 Gd1 C16 156.87(10) . . ?
O1 Gd1 C16 26.32(10) . . ?
O4 Gd1 C16 150.55(10) . . ?
N3 Gd1 C16 102.34(12) . . ?
N1 Gd1 C16 78.11(11) . . ?
N2 Gd1 C16 89.80(10) . . ?
O6 Gd1 C23 106.23(12) . . ?
O5 Gd1 C23 72.09(11) . . ?
O2 Gd1 C23 147.51(11) . . ?
O3 Gd1 C23 26.38(10) . . ?
O1 Gd1 C23 159.35(10) . . ?
O4 Gd1 C23 26.27(10) . . ?
N3 Gd1 C23 84.38(11) . . ?
N1 Gd1 C23 97.03(12) . . ?
N2 Gd1 C23 92.21(11) . . ?
C16 Gd1 C23 173.17(12) . . ?

_refine_diff_density_max         1.657
_refine_diff_density_min         -1.947
_refine_diff_density_rms         0.113

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_8
_database_code_depnum_ccdc_archive 'CCDC 1514986'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 I6 N6 O14 Tb2'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2302.42

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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                   11.1954(7)
_cell_length_b                   12.8463(8)
_cell_length_c                   14.4794(8)
_cell_angle_alpha                69.0230(10)
_cell_angle_beta                 88.579(2)
_cell_angle_gamma                72.7520(10)
_cell_volume                     1849.22(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    27465
_cell_measurement_theta_min      4.354
_cell_measurement_theta_max      47.058

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_F_000             1084
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.179
_exptl_absorpt_coefficient_mu    4.467
_shelx_estimated_absorpt_T_min   0.434
_shelx_estimated_absorpt_T_max   0.502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6769
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27462
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.512
_diffrn_reflns_theta_max         29.723
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10189
_reflns_number_gt                7886
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0348P)²+1.8577P] 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         10189
_refine_ls_number_parameters     469
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0849
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5996(5) 0.7780(5) 0.3383(4) 0.0614(15) Uani 1 1 d . . . . .
H1 H 0.6353 0.6977 0.3542 0.074 Uiso 1 1 calc R U . . .
C2 C 0.4991(6) 0.8373(7) 0.2666(5) 0.084(2) Uani 1 1 d . . . . .
H2 H 0.4667 0.7976 0.2361 0.100 Uiso 1 1 calc R U . . .
C3 C 0.4490(6) 0.9547(7) 0.2416(5) 0.088(2) Uani 1 1 d . . . . .
H3 H 0.3841 0.9972 0.1912 0.105 Uiso 1 1 calc R U . . .
C4 C 0.4945(5) 1.0109(5) 0.2912(5) 0.0734(18) Uani 1 1 d . . . . .
H4 H 0.4593 1.0911 0.2758 0.088 Uiso 1 1 calc R U . . .
C5 C 0.5944(4) 0.9454(4) 0.3649(4) 0.0443(11) Uani 1 1 d . . . . .
C6 C 0.6451(4) 0.9960(4) 0.4250(3) 0.0416(10) Uani 1 1 d . . . . .
C7 C 0.5787(5) 1.1064(4) 0.4271(4) 0.0540(13) Uani 1 1 d . . . . .
H7 H 0.5029 1.1502 0.3885 0.065 Uiso 1 1 calc R U . . .
C8 C 0.6276(5) 1.1486(4) 0.4870(5) 0.0639(16) Uani 1 1 d . . . . .
H8 H 0.5843 1.2210 0.4902 0.077 Uiso 1 1 calc R U . . .
C9 C 0.7408(5) 1.0836(4) 0.5423(4) 0.0520(13) Uani 1 1 d . . . . .
H9 H 0.7752 1.1119 0.5825 0.062 Uiso 1 1 calc R U . . .
C10 C 0.8036(4) 0.9744(3) 0.5374(3) 0.0378(10) Uani 1 1 d . . . . .
C11 C 0.9278(4) 0.9031(3) 0.5910(3) 0.0348(9) Uani 1 1 d . . . . .
C12 C 0.9926(5) 0.9449(4) 0.6422(4) 0.0460(11) Uani 1 1 d . . . . .
H12 H 0.9564 1.0184 0.6457 0.055 Uiso 1 1 calc R U . . .
C13 C 1.1099(5) 0.8780(5) 0.6876(4) 0.0521(13) Uani 1 1 d . . . . .
H13 H 1.1539 0.9057 0.7222 0.063 Uiso 1 1 calc R U . . .
C14 C 1.1620(5) 0.7704(5) 0.6821(4) 0.0501(12) Uani 1 1 d . . . . .
H14 H 1.2418 0.7235 0.7126 0.060 Uiso 1 1 calc R U . . .
C15 C 1.0931(4) 0.7329(4) 0.6299(4) 0.0487(12) Uani 1 1 d . . . . .
H15 H 1.1287 0.6597 0.6255 0.058 Uiso 1 1 calc R U . . .
C16 C 0.6895(4) 0.6422(4) 0.6266(3) 0.0384(10) Uani 1 1 d . . . . .
C17 C 0.6005(4) 0.5983(4) 0.6977(3) 0.0371(10) Uani 1 1 d . . . . .
C18 C 0.5243(4) 0.5424(4) 0.6731(4) 0.0466(11) Uani 1 1 d . . . . .
H18 H 0.5318 0.5294 0.6138 0.056 Uiso 1 1 calc R U . . .
C19 C 0.4378(5) 0.5062(5) 0.7356(4) 0.0522(12) Uani 1 1 d . . . . .
H19 H 0.3861 0.4698 0.7184 0.063 Uiso 1 1 calc R U . . .
C20 C 0.4289(4) 0.5243(5) 0.8233(4) 0.0524(13) Uani 1 1 d . . . . .
C21 C 0.5039(5) 0.5792(5) 0.8503(4) 0.0545(13) Uani 1 1 d . . . . .
H21 H 0.4970 0.5909 0.9102 0.065 Uiso 1 1 calc R U . . .
C22 C 0.5895(5) 0.6164(4) 0.7860(4) 0.0477(11) Uani 1 1 d . . . . .
H22 H 0.6400 0.6539 0.8028 0.057 Uiso 1 1 calc R U . . .
C23 C 1.0146(4) 0.7901(4) 0.3385(3) 0.0377(10) Uani 1 1 d . . . . .
C24 C 1.0900(4) 0.8088(4) 0.2503(3) 0.0372(9) Uani 1 1 d . . . . .
C25 C 1.1923(5) 0.7191(4) 0.2450(4) 0.0495(12) Uani 1 1 d . . . . .
H25 H 1.2158 0.6471 0.2976 0.059 Uiso 1 1 calc R U . . .
C26 C 1.2593(5) 0.7349(5) 0.1632(4) 0.0590(14) Uani 1 1 d . . . . .
H26 H 1.3259 0.6733 0.1594 0.071 Uiso 1 1 calc R U . . .
C27 C 1.2275(5) 0.8423(5) 0.0868(4) 0.0568(14) Uani 1 1 d . . . . .
C28 C 1.1265(6) 0.9337(5) 0.0897(4) 0.0634(15) Uani 1 1 d . . . . .
H28 H 1.1054 1.0063 0.0380 0.076 Uiso 1 1 calc R U . . .
C29 C 1.0571(5) 0.9148(4) 0.1719(4) 0.0514(12) Uani 1 1 d . . . . .
H29 H 0.9873 0.9749 0.1738 0.062 Uiso 1 1 calc R U . . .
C30 C 1.0580(4) 0.4480(3) 0.6522(3) 0.0314(8) Uani 1 1 d . . . . .
C31 C 1.0634(4) 0.3965(3) 0.7634(3) 0.0315(8) Uani 1 1 d . . . . .
C32 C 0.9847(4) 0.4571(4) 0.8145(3) 0.0431(11) Uani 1 1 d . . . . .
H32 H 0.9262 0.5292 0.7795 0.052 Uiso 1 1 calc R U . . .
C33 C 0.9919(5) 0.4120(4) 0.9168(4) 0.0498(12) Uani 1 1 d . . . . .
H33 H 0.9380 0.4529 0.9508 0.060 Uiso 1 1 calc R U . . .
C34 C 1.0811(5) 0.3044(4) 0.9686(3) 0.0488(12) Uani 1 1 d . . . . .
C35 C 1.1560(5) 0.2418(4) 0.9184(4) 0.0515(13) Uani 1 1 d . . . . .
H35 H 1.2131 0.1687 0.9531 0.062 Uiso 1 1 calc R U . . .
C36 C 1.1466(5) 0.2877(4) 0.8158(3) 0.0457(11) Uani 1 1 d . . . . .
H36 H 1.1970 0.2447 0.7817 0.055 Uiso 1 1 calc R U . . .
N1 N 0.6479(3) 0.8300(3) 0.3858(3) 0.0441(9) Uani 1 1 d . . . . .
N2 N 0.7542(3) 0.9310(3) 0.4804(3) 0.0357(8) Uani 1 1 d . . . . .
N3 N 0.9780(3) 0.7962(3) 0.5853(3) 0.0377(8) Uani 1 1 d . . . . .
O1 O 0.7124(3) 0.6070(3) 0.5552(2) 0.0485(8) Uani 1 1 d . . . . .
O2 O 0.7375(3) 0.7149(3) 0.6371(2) 0.0420(7) Uani 1 1 d . . . . .
O3 O 1.0634(3) 0.7085(3) 0.4196(2) 0.0496(8) Uani 1 1 d . . . . .
O4 O 0.9030(3) 0.8536(3) 0.3304(2) 0.0428(7) Uani 1 1 d . . . . .
O5 O 0.8699(3) 0.6117(3) 0.3905(2) 0.0402(7) Uani 1 1 d . . . . .
O6 O 0.9847(3) 0.5492(2) 0.6092(2) 0.0432(7) Uani 1 1 d . . . . .
OW1 O 0.6877(5) 0.4222(6) 0.4934(4) 0.0870(15) Uani 1 1 d D . . . .
I1 I 0.29508(4) 0.47158(6) 0.91720(3) 0.09558(19) Uani 1 1 d . . . . .
I2 I 1.33042(6) 0.86946(6) -0.03827(4) 0.1101(2) Uani 1 1 d . . . . .
I3A I 1.1173(4) 0.2448(4) 1.1269(3) 0.0671(8) Uani 0.60(3) 1 d . . P A 1
I3B I 1.081(2) 0.2379(5) 1.1186(6) 0.092(3) Uani 0.40(3) 1 d . . P A 2
Tb1 Tb 0.85992(2) 0.71787(2) 0.49084(2) 0.03110(6) Uani 1 1 d . . . . .
HW1A H 0.689(7) 0.486(3) 0.492(6) 0.10(3) Uiso 1 1 d D . . . .
HW1B H 0.756(5) 0.374(7) 0.518(7) 0.16(4) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.332(6) . ?
C1 C2 1.382(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.356(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.380(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.399(7) . ?
C4 H4 0.9300 . ?
C5 N1 1.346(6) . ?
C5 C6 1.466(7) . ?
C6 N2 1.341(5) . ?
C6 C7 1.402(6) . ?
C7 C8 1.373(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.374(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.397(6) . ?
C9 H9 0.9300 . ?
C10 N2 1.353(6) . ?
C10 C11 1.471(6) . ?
C11 N3 1.353(5) . ?
C11 C12 1.380(6) . ?
C12 C13 1.366(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.362(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.383(7) . ?
C14 H14 0.9300 . ?
C15 N3 1.335(6) . ?
C15 H15 0.9300 . ?
C16 O2 1.260(5) . ?
C16 O1 1.263(5) . ?
C16 C17 1.496(6) . ?
C16 Tb1 2.828(5) . ?
C17 C22 1.376(6) . ?
C17 C18 1.389(6) . ?
C18 C19 1.377(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.366(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.386(7) . ?
C20 I1 2.096(5) . ?
C21 C22 1.386(7) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O4 1.254(5) . ?
C23 O3 1.260(5) . ?
C23 C24 1.500(6) . ?
C23 Tb1 2.832(4) . ?
C24 C29 1.377(6) . ?
C24 C25 1.387(6) . ?
C25 C26 1.372(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.374(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.380(8) . ?
C27 I2 2.101(5) . ?
C28 C29 1.391(7) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 O6 1.251(5) . ?
C30 O5 1.254(5) 2_766 ?
C30 C31 1.501(6) . ?
C31 C36 1.378(6) . ?
C31 C32 1.379(6) . ?
C32 C33 1.378(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.396(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.366(7) . ?
C34 I3B 2.029(8) . ?
C34 I3A 2.147(6) . ?
C35 C36 1.382(6) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N1 Tb1 2.570(4) . ?
N2 Tb1 2.590(3) . ?
N3 Tb1 2.548(4) . ?
O1 Tb1 2.448(3) . ?
O2 Tb1 2.489(3) . ?
O3 Tb1 2.466(3) . ?
O4 Tb1 2.493(3) . ?
O5 C30 1.254(5) 2_766 ?
O5 Tb1 2.302(3) . ?
O6 Tb1 2.291(3) . ?
OW1 HW1A 0.820(10) . ?
OW1 HW1B 0.819(10) . ?

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
N1 C1 C2 123.2(6) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C3 C2 C1 118.4(6) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 119.9(6) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 118.9(6) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 120.8(5) . . ?
N1 C5 C6 116.2(4) . . ?
C4 C5 C6 123.0(5) . . ?
N2 C6 C7 121.6(5) . . ?
N2 C6 C5 117.5(4) . . ?
C7 C6 C5 120.8(4) . . ?
C8 C7 C6 118.9(5) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C7 C8 C9 119.8(5) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C8 C9 C10 119.2(5) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N2 C10 C9 121.3(4) . . ?
N2 C10 C11 116.9(4) . . ?
C9 C10 C11 121.8(4) . . ?
N3 C11 C12 121.2(4) . . ?
N3 C11 C10 117.2(4) . . ?
C12 C11 C10 121.6(4) . . ?
C13 C12 C11 119.8(4) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 C12 119.7(5) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 118.1(5) . . ?
C13 C14 H14 120.9 . . ?
C15 C14 H14 120.9 . . ?
N3 C15 C14 123.4(5) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
O2 C16 O1 121.3(4) . . ?
O2 C16 C17 120.3(4) . . ?
O1 C16 C17 118.5(4) . . ?
O2 C16 Tb1 61.6(2) . . ?
O1 C16 Tb1 59.7(2) . . ?
C17 C16 Tb1 178.0(3) . . ?
C22 C17 C18 119.2(4) . . ?
C22 C17 C16 120.7(4) . . ?
C18 C17 C16 120.0(4) . . ?
C19 C18 C17 120.8(5) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C20 C19 C18 119.1(5) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
C19 C20 C21 121.6(5) . . ?
C19 C20 I1 119.0(4) . . ?
C21 C20 I1 119.4(4) . . ?
C22 C21 C20 118.6(5) . . ?
C22 C21 H21 120.7 . . ?
C20 C21 H21 120.7 . . ?
C17 C22 C21 120.7(5) . . ?
C17 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
O4 C23 O3 120.7(4) . . ?
O4 C23 C24 119.9(4) . . ?
O3 C23 C24 119.3(4) . . ?
O4 C23 Tb1 61.6(2) . . ?
O3 C23 Tb1 60.4(2) . . ?
C24 C23 Tb1 167.2(3) . . ?
C29 C24 C25 118.7(4) . . ?
C29 C24 C23 120.6(4) . . ?
C25 C24 C23 120.8(4) . . ?
C26 C25 C24 120.9(5) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C25 C26 C27 119.7(5) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 H26 120.2 . . ?
C26 C27 C28 121.0(5) . . ?
C26 C27 I2 120.4(4) . . ?
C28 C27 I2 118.6(4) . . ?
C27 C28 C29 118.5(5) . . ?
C27 C28 H28 120.7 . . ?
C29 C28 H28 120.7 . . ?
C24 C29 C28 121.2(5) . . ?
C24 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
O6 C30 O5 124.7(4) . 2_766 ?
O6 C30 C31 117.5(4) . . ?
O5 C30 C31 117.8(3) 2_766 . ?
C36 C31 C32 119.2(4) . . ?
C36 C31 C30 120.4(4) . . ?
C32 C31 C30 120.4(4) . . ?
C33 C32 C31 120.8(4) . . ?
C33 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C32 C33 C34 119.2(4) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 H33 120.4 . . ?
C35 C34 C33 120.3(4) . . ?
C35 C34 I3B 121.9(5) . . ?
C33 C34 I3B 117.4(5) . . ?
C35 C34 I3A 118.9(4) . . ?
C33 C34 I3A 120.3(4) . . ?
C34 C35 C36 119.7(4) . . ?
C34 C35 H35 120.2 . . ?
C36 C35 H35 120.2 . . ?
C31 C36 C35 120.8(4) . . ?
C31 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
C1 N1 C5 118.6(4) . . ?
C1 N1 Tb1 119.3(3) . . ?
C5 N1 Tb1 121.3(3) . . ?
C6 N2 C10 119.2(4) . . ?
C6 N2 Tb1 120.6(3) . . ?
C10 N2 Tb1 120.0(3) . . ?
C15 N3 C11 117.7(4) . . ?
C15 N3 Tb1 120.6(3) . . ?
C11 N3 Tb1 121.6(3) . . ?
C16 O1 Tb1 93.8(3) . . ?
C16 O2 Tb1 92.0(3) . . ?
C23 O3 Tb1 93.3(3) . . ?
C23 O4 Tb1 92.1(3) . . ?
C30 O5 Tb1 144.6(3) 2_766 . ?
C30 O6 Tb1 163.0(3) . . ?
HW1A OW1 HW1B 108(9) . . ?
O6 Tb1 O5 87.52(10) . . ?
O6 Tb1 O1 77.53(12) . . ?
O5 Tb1 O1 75.88(11) . . ?
O6 Tb1 O3 80.30(11) . . ?
O5 Tb1 O3 74.97(11) . . ?
O1 Tb1 O3 143.85(11) . . ?
O6 Tb1 O2 79.79(11) . . ?
O5 Tb1 O2 128.69(11) . . ?
O1 Tb1 O2 52.88(10) . . ?
O3 Tb1 O2 147.96(11) . . ?
O6 Tb1 O4 132.54(11) . . ?
O5 Tb1 O4 78.77(10) . . ?
O1 Tb1 O4 139.34(11) . . ?
O3 Tb1 O4 52.31(10) . . ?
O2 Tb1 O4 142.24(10) . . ?
O6 Tb1 N3 77.75(11) . . ?
O5 Tb1 N3 147.48(11) . . ?
O1 Tb1 N3 127.31(11) . . ?
O3 Tb1 N3 74.06(11) . . ?
O2 Tb1 N3 77.35(11) . . ?
O4 Tb1 N3 90.01(11) . . ?
O6 Tb1 N1 148.36(13) . . ?
O5 Tb1 N1 79.65(11) . . ?
O1 Tb1 N1 71.35(12) . . ?
O3 Tb1 N1 122.96(12) . . ?
O2 Tb1 N1 85.89(12) . . ?
O4 Tb1 N1 73.21(11) . . ?
N3 Tb1 N1 126.39(12) . . ?
O6 Tb1 N2 135.16(11) . . ?
O5 Tb1 N2 137.31(11) . . ?
O1 Tb1 N2 108.00(11) . . ?
O3 Tb1 N2 107.89(11) . . ?
O2 Tb1 N2 70.82(10) . . ?
O4 Tb1 N2 71.69(10) . . ?
N3 Tb1 N2 63.50(11) . . ?
N1 Tb1 N2 62.89(12) . . ?
O6 Tb1 C16 76.63(12) . . ?
O5 Tb1 C16 102.26(12) . . ?
O1 Tb1 C16 26.46(12) . . ?
O3 Tb1 C16 156.88(11) . . ?
O2 Tb1 C16 26.44(11) . . ?
O4 Tb1 C16 150.57(11) . . ?
N3 Tb1 C16 102.26(13) . . ?
N1 Tb1 C16 78.03(12) . . ?
N2 Tb1 C16 89.84(11) . . ?
O6 Tb1 C23 106.30(12) . . ?
O5 Tb1 C23 72.27(12) . . ?
O1 Tb1 C23 147.65(11) . . ?
O3 Tb1 C23 26.37(11) . . ?
O2 Tb1 C23 158.90(11) . . ?
O4 Tb1 C23 26.27(11) . . ?
N3 Tb1 C23 84.16(12) . . ?
N1 Tb1 C23 97.19(13) . . ?
N2 Tb1 C23 91.93(12) . . ?
C16 Tb1 C23 173.45(13) . . ?

_refine_diff_density_max         1.761
_refine_diff_density_min         -1.997
_refine_diff_density_rms         0.119

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_4
_database_code_depnum_ccdc_archive 'CCDC 1514982'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 I6 N6 Nd2 O14'
_exptl_crystal_recrystallization_method HYdrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2273.06

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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                   11.2063(3)
_cell_length_b                   12.9586(4)
_cell_length_c                   14.5704(4)
_cell_angle_alpha                69.2310(11)
_cell_angle_beta                 88.870(2)
_cell_angle_gamma                72.8990(10)
_cell_volume                     1882.44(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    27696
_cell_measurement_theta_min      5.078
_cell_measurement_theta_max      59.355
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_F_000             1074
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.525
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.227
_exptl_absorpt_coefficient_mu    3.889
_shelx_estimated_absorpt_T_min   0.235
_shelx_estimated_absorpt_T_max   0.472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5681
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27666
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.501
_diffrn_reflns_theta_max         29.681
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10349
_reflns_number_gt                9204
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0320P)²+2.9125P] 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         10349
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0788
_refine_ls_wR_factor_gt          0.0751
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.002
_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
C10 C 0.6954(3) 0.5238(2) -0.0390(2) 0.0407(6) Uani 1 1 d . . . . .
C11 C 0.5704(3) 0.5948(2) -0.0921(2) 0.0372(6) Uani 1 1 d . . . . .
C12 C 0.5045(4) 0.5540(3) -0.1436(3) 0.0500(7) Uani 1 1 d . . . . .
H12 H 0.5403 0.4813 -0.1474 0.060 Uiso 1 1 calc R U . . .
C13 C 0.3871(4) 0.6200(3) -0.1890(3) 0.0544(8) Uani 1 1 d . . . . .
H13 H 0.3426 0.5928 -0.2235 0.065 Uiso 1 1 calc R U . . .
C14 C 0.3362(3) 0.7269(3) -0.1827(3) 0.0533(8) Uani 1 1 d . . . . .
H14 H 0.2568 0.7740 -0.2132 0.064 Uiso 1 1 calc R U . . .
C15 C 0.4057(3) 0.7631(3) -0.1300(3) 0.0510(8) Uani 1 1 d . . . . .
H15 H 0.3705 0.8353 -0.1251 0.061 Uiso 1 1 calc R U . . .
C16 C 0.8156(3) 0.8579(2) -0.1273(2) 0.0395(6) Uani 1 1 d . . . . .
C17 C 0.9032(3) 0.9027(2) -0.1980(2) 0.0391(6) Uani 1 1 d . . . . .
C18 C 0.9796(3) 0.9577(3) -0.1738(3) 0.0479(7) Uani 1 1 d . . . . .
H18 H 0.9738 0.9695 -0.1143 0.057 Uiso 1 1 calc R U . . .
C19 C 1.0645(3) 0.9955(3) -0.2374(3) 0.0533(8) Uani 1 1 d . . . . .
H19 H 1.1154 1.0327 -0.2209 0.064 Uiso 1 1 calc R U . . .
C20 C 1.0728(3) 0.9773(3) -0.3252(3) 0.0523(8) Uani 1 1 d . . . . .
C21 C 0.9979(4) 0.9219(4) -0.3506(3) 0.0566(9) Uani 1 1 d . . . . .
H21 H 1.0044 0.9098 -0.4099 0.068 Uiso 1 1 calc R U . . .
C22 C 0.9131(3) 0.8847(3) -0.2868(2) 0.0480(7) Uani 1 1 d . . . . .
H22 H 0.8624 0.8475 -0.3035 0.058 Uiso 1 1 calc R U . . .
C23 C 0.4832(3) 0.7101(3) 0.1650(2) 0.0403(6) Uani 1 1 d . . . . .
C24 C 0.4084(3) 0.6919(3) 0.2525(2) 0.0406(6) Uani 1 1 d . . . . .
C25 C 0.3058(3) 0.7808(3) 0.2571(3) 0.0538(8) Uani 1 1 d . . . . .
H25 H 0.2820 0.8516 0.2045 0.065 Uiso 1 1 calc R U . . .
C26 C 0.2385(4) 0.7653(4) 0.3389(3) 0.0653(10) Uani 1 1 d . . . . .
H26 H 0.1719 0.8262 0.3426 0.078 Uiso 1 1 calc R U . . .
C27 C 0.2714(4) 0.6586(4) 0.4148(3) 0.0615(9) Uani 1 1 d . . . . .
C28 C 0.3717(4) 0.5686(4) 0.4110(3) 0.0665(10) Uani 1 1 d . . . . .
H28 H 0.3927 0.4967 0.4621 0.080 Uiso 1 1 calc R U . . .
C29 C 0.4408(4) 0.5863(3) 0.3304(3) 0.0570(9) Uani 1 1 d . . . . .
H29 H 0.5102 0.5265 0.3286 0.068 Uiso 1 1 calc R U . . .
C30 C 0.5621(3) 0.9475(2) 0.1552(2) 0.0345(5) Uani 1 1 d . . . . .
C31 C 0.5644(3) 0.8961(2) 0.2655(2) 0.0349(5) Uani 1 1 d . . . . .
C32 C 0.4850(3) 0.9569(3) 0.3159(2) 0.0448(7) Uani 1 1 d . . . . .
H32 H 0.4275 1.0288 0.2810 0.054 Uiso 1 1 calc R U . . .
C33 C 0.4911(4) 0.9113(3) 0.4177(3) 0.0561(9) Uani 1 1 d . . . . .
H33 H 0.4375 0.9521 0.4513 0.067 Uiso 1 1 calc R U . . .
C34 C 0.5767(4) 0.8055(3) 0.4688(3) 0.0542(8) Uani 1 1 d . . . . .
C35 C 0.6536(4) 0.7416(3) 0.4208(3) 0.0559(9) Uani 1 1 d . . . . .
H35 H 0.7092 0.6689 0.4560 0.067 Uiso 1 1 calc R U . . .
C36 C 0.6468(3) 0.7876(3) 0.3186(2) 0.0465(7) Uani 1 1 d . . . . .
H36 H 0.6982 0.7450 0.2853 0.056 Uiso 1 1 calc R U . . .
N1 N 0.8569(3) 0.6615(2) 0.1157(2) 0.0489(6) Uani 1 1 d . . . . .
N2 N 0.7455(2) 0.56511(19) 0.01809(18) 0.0374(5) Uani 1 1 d . . . . .
N3 N 0.5204(2) 0.6999(2) -0.0856(2) 0.0419(5) Uani 1 1 d . . . . .
O1 O 0.7949(2) 0.8908(2) -0.05469(18) 0.0537(6) Uani 1 1 d . . . . .
O2 O 0.7664(2) 0.78720(19) -0.13938(17) 0.0448(5) Uani 1 1 d . . . . .
O3 O 0.4338(2) 0.7917(2) 0.08452(17) 0.0539(6) Uani 1 1 d . . . . .
O4 O 0.5945(2) 0.64593(18) 0.17329(17) 0.0466(5) Uani 1 1 d . . . . .
O5 O 0.6356(2) 0.88811(18) 0.11366(16) 0.0450(5) Uani 1 1 d . . . . .
O6 O 0.5110(2) 0.95277(18) -0.11203(16) 0.0486(5) Uani 1 1 d . . . . .
OW1 O 0.1874(4) 0.9202(5) -0.0039(3) 0.0917(13) Uani 1 1 d . . . . .
I1 I 1.20505(3) 1.03007(4) -0.41811(2) 0.09610(13) Uani 1 1 d . . . . .
I2 I 0.16792(4) 0.63094(5) 0.53819(3) 0.11864(17) Uani 1 1 d . . . . .
Nd1 Nd 0.64058(2) 0.78215(2) 0.00958(2) 0.03315(5) Uani 1 1 d . . . . .
I3A I 0.6123(2) 0.7476(3) 0.62764(16) 0.0719(6) Uani 0.522(17) 1 d . . P A 1
I3B I 0.5752(12) 0.7377(3) 0.6177(3) 0.1094(16) Uani 0.478(17) 1 d . . P A 2
C6 C 0.8560(3) 0.4991(3) 0.0728(2) 0.0446(7) Uani 1 1 d . . . . .
C7 C 0.9203(3) 0.3911(3) 0.0694(3) 0.0571(9) Uani 1 1 d . . . . .
H7 H 0.9964 0.3474 0.1073 0.068 Uiso 1 1 calc R U . . .
C5 C 0.9081(3) 0.5482(3) 0.1342(3) 0.0502(8) Uani 1 1 d . . . . .
C9 C 0.7571(4) 0.4152(3) -0.0444(3) 0.0566(9) Uani 1 1 d . . . . .
H9 H 0.7217 0.3877 -0.0844 0.068 Uiso 1 1 calc R U . . .
C8 C 0.8708(4) 0.3498(3) 0.0102(4) 0.0698(12) Uani 1 1 d . . . . .
H8 H 0.9134 0.2781 0.0066 0.084 Uiso 1 1 calc R U . . .
C1 C 0.9065(4) 0.7100(4) 0.1658(3) 0.0682(11) Uani 1 1 d . . . . .
H1 H 0.8723 0.7892 0.1515 0.082 Uiso 1 1 calc R U . . .
C4 C 1.0084(4) 0.4808(4) 0.2066(4) 0.0794(13) Uani 1 1 d . . . . .
H4 H 1.0431 0.4019 0.2194 0.095 Uiso 1 1 calc R U . . .
C2 C 1.0060(5) 0.6486(5) 0.2377(4) 0.0894(16) Uani 1 1 d . . . . .
H2 H 1.0383 0.6855 0.2708 0.107 Uiso 1 1 calc R U . . .
C3 C 1.0550(5) 0.5331(5) 0.2587(4) 0.0989(19) Uani 1 1 d . . . . .
H3 H 1.1202 0.4891 0.3083 0.119 Uiso 1 1 calc R U . . .
HW1A H 0.259(7) 0.882(6) 0.022(5) 0.11(2) Uiso 1 1 d . . . . .
HW1B H 0.180(6) 0.980(6) -0.001(5) 0.10(2) Uiso 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
C10 N2 1.343(4) . ?
C10 C9 1.403(4) . ?
C10 C11 1.478(4) . ?
C11 N3 1.348(4) . ?
C11 C12 1.386(4) . ?
C12 C13 1.368(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.369(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.382(5) . ?
C14 H14 0.9300 . ?
C15 N3 1.334(4) . ?
C15 H15 0.9300 . ?
C16 O2 1.261(4) . ?
C16 O1 1.267(4) . ?
C16 C17 1.495(4) . ?
C16 Nd1 2.894(3) . ?
C17 C18 1.384(4) . ?
C17 C22 1.390(4) . ?
C18 C19 1.386(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.378(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.381(5) . ?
C20 I1 2.087(3) . ?
C21 C22 1.384(5) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O4 1.260(4) . ?
C23 O3 1.265(4) . ?
C23 C24 1.498(4) . ?
C23 Nd1 2.902(3) . ?
C24 C29 1.384(5) . ?
C24 C25 1.388(4) . ?
C25 C26 1.383(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.380(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.378(6) . ?
C27 I2 2.100(4) . ?
C28 C29 1.381(5) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 O6 1.248(3) 2_675 ?
C30 O5 1.255(3) . ?
C30 C31 1.503(4) . ?
C31 C32 1.387(4) . ?
C31 C36 1.386(4) . ?
C32 C33 1.383(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.374(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.373(5) . ?
C34 I3B 2.033(5) . ?
C34 I3A 2.169(4) . ?
C35 C36 1.387(5) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N1 C1 1.335(5) . ?
N1 C5 1.337(4) . ?
N1 Nd1 2.630(3) . ?
N2 C6 1.353(4) . ?
N2 Nd1 2.669(2) . ?
N3 Nd1 2.615(3) . ?
O1 Nd1 2.506(2) . ?
O2 Nd1 2.556(2) . ?
O3 Nd1 2.530(2) . ?
O4 Nd1 2.564(2) . ?
O5 Nd1 2.370(2) . ?
O6 C30 1.248(3) 2_675 ?
O6 Nd1 2.361(2) . ?
OW1 HW1A 0.82(7) . ?
OW1 HW1B 0.77(6) . ?
C6 C7 1.391(4) . ?
C6 C5 1.479(5) . ?
C7 C8 1.365(6) . ?
C7 H7 0.9300 . ?
C5 C4 1.399(5) . ?
C9 C8 1.379(6) . ?
C9 H9 0.9300 . ?
C8 H8 0.9300 . ?
C1 C2 1.381(6) . ?
C1 H1 0.9300 . ?
C4 C3 1.377(8) . ?
C4 H4 0.9300 . ?
C2 C3 1.354(8) . ?
C2 H2 0.9300 . ?
C3 H3 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
N2 C10 C9 121.0(3) . . ?
N2 C10 C11 117.4(2) . . ?
C9 C10 C11 121.5(3) . . ?
N3 C11 C12 120.9(3) . . ?
N3 C11 C10 117.3(3) . . ?
C12 C11 C10 121.8(3) . . ?
C13 C12 C11 120.4(3) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C12 118.8(3) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 118.4(3) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
N3 C15 C14 123.5(3) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
O2 C16 O1 121.6(3) . . ?
O2 C16 C17 120.0(3) . . ?
O1 C16 C17 118.4(3) . . ?
O2 C16 Nd1 61.97(16) . . ?
O1 C16 Nd1 59.72(16) . . ?
C17 C16 Nd1 177.3(2) . . ?
C18 C17 C22 119.2(3) . . ?
C18 C17 C16 120.3(3) . . ?
C22 C17 C16 120.4(3) . . ?
C17 C18 C19 120.7(3) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C20 C19 C18 119.3(3) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
C19 C20 C21 121.0(3) . . ?
C19 C20 I1 118.8(3) . . ?
C21 C20 I1 120.2(3) . . ?
C20 C21 C22 119.4(3) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C21 C22 C17 120.5(3) . . ?
C21 C22 H22 119.8 . . ?
C17 C22 H22 119.8 . . ?
O4 C23 O3 121.3(3) . . ?
O4 C23 C24 119.6(3) . . ?
O3 C23 C24 119.1(3) . . ?
O4 C23 Nd1 61.98(16) . . ?
O3 C23 Nd1 60.48(16) . . ?
C24 C23 Nd1 167.5(2) . . ?
C29 C24 C25 118.8(3) . . ?
C29 C24 C23 120.6(3) . . ?
C25 C24 C23 120.6(3) . . ?
C26 C25 C24 120.8(3) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C27 C26 C25 119.2(4) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C28 C27 C26 120.9(3) . . ?
C28 C27 I2 119.0(3) . . ?
C26 C27 I2 120.2(3) . . ?
C27 C28 C29 119.4(4) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C28 C29 C24 120.9(3) . . ?
C28 C29 H29 119.6 . . ?
C24 C29 H29 119.6 . . ?
O6 C30 O5 124.9(3) 2_675 . ?
O6 C30 C31 117.4(2) 2_675 . ?
O5 C30 C31 117.7(2) . . ?
C32 C31 C36 118.9(3) . . ?
C32 C31 C30 120.6(3) . . ?
C36 C31 C30 120.5(3) . . ?
C33 C32 C31 120.4(3) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C34 C33 C32 119.6(3) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C34 C35 121.3(3) . . ?
C33 C34 I3B 118.1(3) . . ?
C35 C34 I3B 120.3(3) . . ?
C33 C34 I3A 120.0(3) . . ?
C35 C34 I3A 118.1(3) . . ?
C34 C35 C36 118.8(3) . . ?
C34 C35 H35 120.6 . . ?
C36 C35 H35 120.6 . . ?
C31 C36 C35 121.0(3) . . ?
C31 C36 H36 119.5 . . ?
C35 C36 H36 119.5 . . ?
C1 N1 C5 118.4(3) . . ?
C1 N1 Nd1 118.6(2) . . ?
C5 N1 Nd1 122.1(2) . . ?
C10 N2 C6 119.1(3) . . ?
C10 N2 Nd1 120.23(18) . . ?
C6 N2 Nd1 120.4(2) . . ?
C15 N3 C11 118.0(3) . . ?
C15 N3 Nd1 119.7(2) . . ?
C11 N3 Nd1 122.3(2) . . ?
C16 O1 Nd1 94.39(19) . . ?
C16 O2 Nd1 92.21(17) . . ?
C23 O3 Nd1 93.73(18) . . ?
C23 O4 Nd1 92.31(18) . . ?
C30 O5 Nd1 142.5(2) . . ?
C30 O6 Nd1 163.1(2) 2_675 . ?
HW1A OW1 HW1B 103(6) . . ?
O6 Nd1 O5 89.06(7) . . ?
O6 Nd1 O1 78.98(9) . . ?
O5 Nd1 O1 75.92(8) . . ?
O6 Nd1 O3 80.63(8) . . ?
O5 Nd1 O3 75.05(9) . . ?
O1 Nd1 O3 144.55(8) . . ?
O6 Nd1 O2 79.48(8) . . ?
O5 Nd1 O2 127.52(8) . . ?
O1 Nd1 O2 51.67(7) . . ?
O3 Nd1 O2 149.29(8) . . ?
O6 Nd1 O4 131.78(8) . . ?
O5 Nd1 O4 78.25(8) . . ?
O1 Nd1 O4 139.07(8) . . ?
O3 Nd1 O4 51.18(7) . . ?
O2 Nd1 O4 143.37(7) . . ?
O6 Nd1 N3 77.79(8) . . ?
O5 Nd1 N3 148.87(8) . . ?
O1 Nd1 N3 127.50(8) . . ?
O3 Nd1 N3 75.03(8) . . ?
O2 Nd1 N3 78.06(8) . . ?
O4 Nd1 N3 89.61(8) . . ?
O6 Nd1 N1 150.59(9) . . ?
O5 Nd1 N1 80.30(8) . . ?
O1 Nd1 N1 71.87(9) . . ?
O3 Nd1 N1 121.98(8) . . ?
O2 Nd1 N1 85.43(8) . . ?
O4 Nd1 N1 72.89(9) . . ?
N3 Nd1 N1 123.60(8) . . ?
O6 Nd1 N2 133.81(8) . . ?
O5 Nd1 N2 137.13(8) . . ?
O1 Nd1 N2 107.46(8) . . ?
O3 Nd1 N2 107.61(8) . . ?
O2 Nd1 N2 71.34(7) . . ?
O4 Nd1 N2 72.42(7) . . ?
N3 Nd1 N2 61.89(8) . . ?
N1 Nd1 N2 61.72(8) . . ?
O6 Nd1 C16 77.14(8) . . ?
O5 Nd1 C16 101.71(9) . . ?
O1 Nd1 C16 25.88(8) . . ?
O3 Nd1 C16 157.60(8) . . ?
O2 Nd1 C16 25.82(8) . . ?
O4 Nd1 C16 150.81(8) . . ?
N3 Nd1 C16 102.62(9) . . ?
N1 Nd1 C16 78.31(9) . . ?
N2 Nd1 C16 89.96(8) . . ?
O6 Nd1 C23 106.14(9) . . ?
O5 Nd1 C23 72.23(8) . . ?
O1 Nd1 C23 147.58(8) . . ?
O3 Nd1 C23 25.79(8) . . ?
O2 Nd1 C23 160.04(8) . . ?
O4 Nd1 C23 25.71(8) . . ?
N3 Nd1 C23 84.38(8) . . ?
N1 Nd1 C23 96.64(9) . . ?
N2 Nd1 C23 92.09(8) . . ?
C16 Nd1 C23 172.84(9) . . ?
N2 C6 C7 121.7(3) . . ?
N2 C6 C5 117.2(3) . . ?
C7 C6 C5 121.0(3) . . ?
C8 C7 C6 119.4(3) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
N1 C5 C4 121.0(4) . . ?
N1 C5 C6 116.9(3) . . ?
C4 C5 C6 122.1(3) . . ?
C8 C9 C10 119.4(4) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C7 C8 C9 119.4(3) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
N1 C1 C2 123.4(4) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C4 C5 118.9(4) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C3 C2 C1 118.1(5) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C2 C3 C4 120.1(4) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?

_refine_diff_density_max         1.930
_refine_diff_density_min         -1.961
_refine_diff_density_rms         0.091

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_5
_database_code_depnum_ccdc_archive 'CCDC 1514983'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 I6 N6 O14 Sm2'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2285.30

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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                   11.2048(4)
_cell_length_b                   12.9132(5)
_cell_length_c                   14.5273(6)
_cell_angle_alpha                69.1340(10)
_cell_angle_beta                 88.7220(10)
_cell_angle_gamma                72.806(2)
_cell_volume                     1868.20(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    24486
_cell_measurement_theta_min      4.642
_cell_measurement_theta_max      47.569

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.031
_exptl_crystal_F_000             1078
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.183
_exptl_absorpt_coefficient_mu    4.101
_shelx_estimated_absorpt_T_min   0.342
_shelx_estimated_absorpt_T_max   0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6513
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24485
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.507
_diffrn_reflns_theta_max         27.460
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8517
_reflns_number_gt                6872
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0320P)²+2.8215P] 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         8517
_refine_ls_number_parameters     469
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0822
_refine_ls_wR_factor_gt          0.0758
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.976
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9043(5) 0.7151(5) 0.1639(4) 0.0655(15) Uani 1 1 d . . . . .
H1 H 0.8701 0.7949 0.1484 0.079 Uiso 1 1 calc R U . . .
C2 C 1.0032(6) 0.6549(7) 0.2360(5) 0.088(2) Uani 1 1 d . . . . .
H2 H 1.0353 0.6930 0.2681 0.105 Uiso 1 1 calc R U . . .
C3 C 1.0528(6) 0.5383(7) 0.2589(6) 0.092(2) Uani 1 1 d . . . . .
H3 H 1.1176 0.4949 0.3091 0.110 Uiso 1 1 calc R U . . .
C4 C 1.0071(5) 0.4844(5) 0.2075(5) 0.0777(18) Uani 1 1 d . . . . .
H4 H 1.0420 0.4050 0.2213 0.093 Uiso 1 1 calc R U . . .
C5 C 0.9070(4) 0.5515(4) 0.1343(3) 0.0477(11) Uani 1 1 d . . . . .
C6 C 0.8560(4) 0.5012(4) 0.0737(3) 0.0435(11) Uani 1 1 d . . . . .
C7 C 0.9206(5) 0.3921(4) 0.0705(4) 0.0558(13) Uani 1 1 d . . . . .
H7 H 0.9966 0.3482 0.1086 0.067 Uiso 1 1 calc R U . . .
C8 C 0.8718(5) 0.3507(4) 0.0117(5) 0.0682(16) Uani 1 1 d . . . . .
H8 H 0.9146 0.2785 0.0087 0.082 Uiso 1 1 calc R U . . .
C9 C 0.7584(5) 0.4159(4) -0.0437(4) 0.0551(13) Uani 1 1 d . . . . .
H9 H 0.7237 0.3880 -0.0839 0.066 Uiso 1 1 calc R U . . .
C10 C 0.6964(4) 0.5249(3) -0.0384(3) 0.0398(10) Uani 1 1 d . . . . .
C11 C 0.5715(4) 0.5958(3) -0.0921(3) 0.0368(9) Uani 1 1 d . . . . .
C12 C 0.5059(5) 0.5550(4) -0.1432(4) 0.0491(12) Uani 1 1 d . . . . .
H12 H 0.5421 0.4820 -0.1469 0.059 Uiso 1 1 calc R U . . .
C13 C 0.3884(5) 0.6205(4) -0.1885(4) 0.0524(12) Uani 1 1 d . . . . .
H13 H 0.3441 0.5929 -0.2228 0.063 Uiso 1 1 calc R U . . .
C14 C 0.3372(5) 0.7282(4) -0.1822(4) 0.0519(12) Uani 1 1 d . . . . .
H14 H 0.2575 0.7753 -0.2122 0.062 Uiso 1 1 calc R U . . .
C15 C 0.4066(4) 0.7646(4) -0.1304(4) 0.0498(12) Uani 1 1 d . . . . .
H15 H 0.3715 0.8374 -0.1261 0.060 Uiso 1 1 calc R U . . .
C16 C 0.4839(4) 0.7098(4) 0.1634(3) 0.0407(10) Uani 1 1 d . . . . .
C17 C 0.4092(4) 0.6915(4) 0.2514(3) 0.0381(9) Uani 1 1 d . . . . .
C18 C 0.4419(5) 0.5859(4) 0.3297(4) 0.0551(13) Uani 1 1 d . . . . .
H18 H 0.5116 0.5260 0.3280 0.066 Uiso 1 1 calc R U . . .
C19 C 0.3730(5) 0.5678(5) 0.4104(4) 0.0641(15) Uani 1 1 d . . . . .
H19 H 0.3940 0.4955 0.4616 0.077 Uiso 1 1 calc R U . . .
C20 C 0.2722(5) 0.6582(5) 0.4144(4) 0.0591(14) Uani 1 1 d . . . . .
C21 C 0.2395(5) 0.7656(5) 0.3379(4) 0.0608(14) Uani 1 1 d . . . . .
H21 H 0.1729 0.8268 0.3416 0.073 Uiso 1 1 calc R U . . .
C22 C 0.3065(4) 0.7808(4) 0.2563(4) 0.0536(12) Uani 1 1 d . . . . .
H22 H 0.2828 0.8520 0.2036 0.064 Uiso 1 1 calc R U . . .
C23 C 0.8134(4) 0.8581(4) -0.1268(3) 0.0389(10) Uani 1 1 d . . . . .
C24 C 0.9020(4) 0.9023(3) -0.1978(3) 0.0376(10) Uani 1 1 d . . . . .
C25 C 0.9120(4) 0.8845(4) -0.2864(4) 0.0492(11) Uani 1 1 d . . . . .
H25 H 0.8613 0.8473 -0.3031 0.059 Uiso 1 1 calc R U . . .
C26 C 0.9968(5) 0.9217(5) -0.3502(4) 0.0575(13) Uani 1 1 d . . . . .
H26 H 1.0033 0.9098 -0.4098 0.069 Uiso 1 1 calc R U . . .
C27 C 1.0717(4) 0.9768(5) -0.3245(4) 0.0530(12) Uani 1 1 d . . . . .
C28 C 1.0634(5) 0.9946(4) -0.2365(4) 0.0536(12) Uani 1 1 d . . . . .
H28 H 1.1148 1.0312 -0.2195 0.064 Uiso 1 1 calc R U . . .
C29 C 0.9781(4) 0.9576(4) -0.1738(4) 0.0474(11) Uani 1 1 d . . . . .
H29 H 0.9716 0.9700 -0.1143 0.057 Uiso 1 1 calc R U . . .
C30 C 0.4397(4) 1.0517(3) -0.1536(3) 0.0334(9) Uani 1 1 d . . . . .
C31 C 0.4363(4) 1.1040(3) -0.2645(3) 0.0347(9) Uani 1 1 d . . . . .
C32 C 0.5147(4) 1.0438(4) -0.3158(3) 0.0434(10) Uani 1 1 d . . . . .
H32 H 0.5726 0.9717 -0.2810 0.052 Uiso 1 1 calc R U . . .
C33 C 0.5084(5) 1.0888(4) -0.4179(4) 0.0533(12) Uani 1 1 d . . . . .
H33 H 0.5622 1.0481 -0.4517 0.064 Uiso 1 1 calc R U . . .
C34 C 0.4215(5) 1.1947(4) -0.4687(3) 0.0517(12) Uani 1 1 d . . . . .
C35 C 0.3449(5) 1.2584(4) -0.4194(3) 0.0529(13) Uani 1 1 d . . . . .
H35 H 0.2884 1.3312 -0.4543 0.064 Uiso 1 1 calc R U . . .
C36 C 0.3537(5) 1.2123(4) -0.3176(3) 0.0472(11) Uani 1 1 d . . . . .
H36 H 0.3029 1.2551 -0.2838 0.057 Uiso 1 1 calc R U . . .
N1 N 0.5218(3) 0.7014(3) -0.0857(3) 0.0400(8) Uani 1 1 d . . . . .
N2 N 0.7458(3) 0.5667(3) 0.0186(3) 0.0368(8) Uani 1 1 d . . . . .
N3 N 0.8546(3) 0.6654(3) 0.1151(3) 0.0475(9) Uani 1 1 d . . . . .
O1 O 0.5958(3) 0.6459(2) 0.1716(2) 0.0449(7) Uani 1 1 d . . . . .
O2 O 0.4350(3) 0.7913(3) 0.0828(2) 0.0527(8) Uani 1 1 d . . . . .
O3 O 0.7915(3) 0.8915(3) -0.0551(2) 0.0516(8) Uani 1 1 d . . . . .
O4 O 0.7647(3) 0.7866(3) -0.1386(2) 0.0439(7) Uani 1 1 d . . . . .
O5 O 0.5131(3) 0.9516(2) -0.1105(2) 0.0470(8) Uani 1 1 d . . . . .
O6 O 0.6332(3) 0.8881(2) 0.1116(2) 0.0429(7) Uani 1 1 d . . . . .
OW1 O 0.1875(5) 0.9215(5) -0.0058(4) 0.0911(15) Uani 1 1 d D . . . .
I1 I 0.16872(5) 0.63082(6) 0.53818(4) 0.1157(2) Uani 1 1 d . . . . .
I2 I 1.20487(4) 1.02945(5) -0.41775(3) 0.09604(18) Uani 1 1 d . . . . .
I3A I 0.3854(3) 1.2538(4) -0.6277(3) 0.0695(9) Uani 0.55(3) 1 d . . P A 1
I3B I 0.4210(19) 1.2618(5) -0.6181(6) 0.104(2) Uani 0.45(3) 1 d . . P A 2
Sm1 Sm 0.64035(2) 0.78201(2) 0.00937(2) 0.03246(7) Uani 1 1 d . . . . .
HW1B H 0.179(7) 0.979(4) 0.008(5) 0.10(3) Uiso 1 1 d D . . . .
HW1A H 0.257(3) 0.883(6) 0.023(5) 0.12(3) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.333(6) . ?
C1 C2 1.376(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.357(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.380(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.401(7) . ?
C4 H4 0.9300 . ?
C5 N3 1.338(6) . ?
C5 C6 1.475(7) . ?
C6 N2 1.351(5) . ?
C6 C7 1.397(6) . ?
C7 C8 1.355(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.378(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.403(6) . ?
C9 H9 0.9300 . ?
C10 N2 1.342(6) . ?
C10 C11 1.479(6) . ?
C11 N1 1.349(5) . ?
C11 C12 1.377(6) . ?
C12 C13 1.366(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.374(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.373(6) . ?
C14 H14 0.9300 . ?
C15 N1 1.338(6) . ?
C15 H15 0.9300 . ?
C16 O2 1.260(5) . ?
C16 O1 1.262(5) . ?
C16 C17 1.499(6) . ?
C16 Sm1 2.873(5) . ?
C17 C18 1.381(6) . ?
C17 C22 1.389(6) . ?
C18 C19 1.377(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.381(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.382(7) . ?
C20 I1 2.097(5) . ?
C21 C22 1.375(7) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O3 1.256(5) . ?
C23 O4 1.263(5) . ?
C23 C24 1.498(6) . ?
C23 Sm1 2.865(4) . ?
C24 C25 1.382(6) . ?
C24 C29 1.382(6) . ?
C25 C26 1.380(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.380(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.374(7) . ?
C27 I2 2.092(5) . ?
C28 C29 1.376(7) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 O5 1.248(5) . ?
C30 O6 1.258(5) 2_675 ?
C30 C31 1.505(6) . ?
C31 C36 1.380(6) . ?
C31 C32 1.383(6) . ?
C32 C33 1.381(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.374(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.378(7) . ?
C34 I3B 2.030(7) . ?
C34 I3A 2.165(6) . ?
C35 C36 1.377(6) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N1 Sm1 2.585(4) . ?
N2 Sm1 2.635(3) . ?
N3 Sm1 2.602(4) . ?
O1 Sm1 2.532(3) . ?
O2 Sm1 2.503(3) . ?
O3 Sm1 2.479(3) . ?
O4 Sm1 2.528(3) . ?
O5 Sm1 2.326(3) . ?
O6 C30 1.258(5) 2_675 ?
O6 Sm1 2.338(3) . ?
OW1 HW1B 0.817(10) . ?
OW1 HW1A 0.819(10) . ?

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
N3 C1 C2 123.6(6) . . ?
N3 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 118.2(6) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 119.8(6) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 118.8(6) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N3 C5 C4 121.1(5) . . ?
N3 C5 C6 116.9(4) . . ?
C4 C5 C6 122.0(5) . . ?
N2 C6 C7 121.2(5) . . ?
N2 C6 C5 117.1(4) . . ?
C7 C6 C5 121.6(4) . . ?
C8 C7 C6 119.6(5) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C9 119.8(4) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C8 C9 C10 118.9(5) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
N2 C10 C9 121.3(4) . . ?
N2 C10 C11 117.5(3) . . ?
C9 C10 C11 121.2(4) . . ?
N1 C11 C12 121.0(4) . . ?
N1 C11 C10 116.8(4) . . ?
C12 C11 C10 122.2(4) . . ?
C13 C12 C11 120.8(4) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 118.4(5) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C15 C14 C13 118.3(5) . . ?
C15 C14 H14 120.8 . . ?
C13 C14 H14 120.8 . . ?
N1 C15 C14 123.9(4) . . ?
N1 C15 H15 118.1 . . ?
C14 C15 H15 118.1 . . ?
O2 C16 O1 120.9(4) . . ?
O2 C16 C17 119.4(4) . . ?
O1 C16 C17 119.7(4) . . ?
O2 C16 Sm1 60.4(2) . . ?
O1 C16 Sm1 61.7(2) . . ?
C17 C16 Sm1 167.2(3) . . ?
C18 C17 C22 118.7(4) . . ?
C18 C17 C16 120.7(4) . . ?
C22 C17 C16 120.6(4) . . ?
C19 C18 C17 121.0(5) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 C20 119.3(5) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C19 C20 C21 120.6(5) . . ?
C19 C20 I1 119.2(4) . . ?
C21 C20 I1 120.2(4) . . ?
C22 C21 C20 119.3(5) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C21 C22 C17 120.9(5) . . ?
C21 C22 H22 119.5 . . ?
C17 C22 H22 119.5 . . ?
O3 C23 O4 121.4(4) . . ?
O3 C23 C24 118.7(4) . . ?
O4 C23 C24 119.8(4) . . ?
O3 C23 Sm1 59.6(2) . . ?
O4 C23 Sm1 61.9(2) . . ?
C24 C23 Sm1 177.9(3) . . ?
C25 C24 C29 119.1(4) . . ?
C25 C24 C23 120.5(4) . . ?
C29 C24 C23 120.3(4) . . ?
C26 C25 C24 120.5(5) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C27 C26 C25 119.3(5) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C28 C27 C26 121.0(5) . . ?
C28 C27 I2 118.8(4) . . ?
C26 C27 I2 120.1(4) . . ?
C27 C28 C29 119.1(5) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C28 C29 C24 121.0(5) . . ?
C28 C29 H29 119.5 . . ?
C24 C29 H29 119.5 . . ?
O5 C30 O6 125.0(4) . 2_675 ?
O5 C30 C31 117.6(4) . . ?
O6 C30 C31 117.3(3) 2_675 . ?
C36 C31 C32 118.4(4) . . ?
C36 C31 C30 120.9(4) . . ?
C32 C31 C30 120.7(4) . . ?
C33 C32 C31 121.1(4) . . ?
C33 C32 H32 119.5 . . ?
C31 C32 H32 119.5 . . ?
C34 C33 C32 119.0(4) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C33 C34 C35 121.1(4) . . ?
C33 C34 I3B 117.8(4) . . ?
C35 C34 I3B 120.8(4) . . ?
C33 C34 I3A 120.1(4) . . ?
C35 C34 I3A 118.3(4) . . ?
C36 C35 C34 118.8(4) . . ?
C36 C35 H35 120.6 . . ?
C34 C35 H35 120.6 . . ?
C35 C36 C31 121.5(4) . . ?
C35 C36 H36 119.3 . . ?
C31 C36 H36 119.3 . . ?
C15 N1 C11 117.5(4) . . ?
C15 N1 Sm1 120.1(3) . . ?
C11 N1 Sm1 122.3(3) . . ?
C10 N2 C6 119.2(4) . . ?
C10 N2 Sm1 120.1(3) . . ?
C6 N2 Sm1 120.4(3) . . ?
C1 N3 C5 118.3(4) . . ?
C1 N3 Sm1 119.2(3) . . ?
C5 N3 Sm1 121.7(3) . . ?
C16 O1 Sm1 92.2(3) . . ?
C16 O2 Sm1 93.7(3) . . ?
C23 O3 Sm1 94.5(3) . . ?
C23 O4 Sm1 92.0(3) . . ?
C30 O5 Sm1 163.1(3) . . ?
C30 O6 Sm1 143.6(3) 2_675 . ?
HW1B OW1 HW1A 99(7) . . ?
O5 Sm1 O6 88.28(10) . . ?
O5 Sm1 O3 78.31(11) . . ?
O6 Sm1 O3 75.91(11) . . ?
O5 Sm1 O2 80.53(11) . . ?
O6 Sm1 O2 75.10(11) . . ?
O3 Sm1 O2 144.36(11) . . ?
O5 Sm1 O4 79.56(10) . . ?
O6 Sm1 O4 127.87(10) . . ?
O3 Sm1 O4 52.04(10) . . ?
O2 Sm1 O4 148.73(11) . . ?
O5 Sm1 O1 132.15(10) . . ?
O6 Sm1 O1 78.59(10) . . ?
O3 Sm1 O1 139.23(11) . . ?
O2 Sm1 O1 51.66(10) . . ?
O4 Sm1 O1 142.93(9) . . ?
O5 Sm1 N1 77.86(11) . . ?
O6 Sm1 N1 148.44(11) . . ?
O3 Sm1 N1 127.24(11) . . ?
O2 Sm1 N1 74.73(11) . . ?
O4 Sm1 N1 77.67(11) . . ?
O1 Sm1 N1 89.85(11) . . ?
O5 Sm1 N3 149.55(12) . . ?
O6 Sm1 N3 79.95(11) . . ?
O3 Sm1 N3 71.63(12) . . ?
O2 Sm1 N3 122.36(11) . . ?
O4 Sm1 N3 85.69(11) . . ?
O1 Sm1 N3 73.00(11) . . ?
N1 Sm1 N3 124.81(11) . . ?
O5 Sm1 N2 134.43(11) . . ?
O6 Sm1 N2 137.28(11) . . ?
O3 Sm1 N2 107.63(10) . . ?
O2 Sm1 N2 107.69(11) . . ?
O4 Sm1 N2 71.19(10) . . ?
O1 Sm1 N2 72.07(10) . . ?
N1 Sm1 N2 62.50(11) . . ?
N3 Sm1 N2 62.32(12) . . ?
O5 Sm1 C23 76.92(11) . . ?
O6 Sm1 C23 101.74(12) . . ?
O3 Sm1 C23 25.91(11) . . ?
O2 Sm1 C23 157.33(11) . . ?
O4 Sm1 C23 26.15(11) . . ?
O1 Sm1 C23 150.65(11) . . ?
N1 Sm1 C23 102.48(12) . . ?
N3 Sm1 C23 78.14(12) . . ?
N2 Sm1 C23 89.98(11) . . ?
O5 Sm1 C16 106.16(12) . . ?
O6 Sm1 C16 72.37(11) . . ?
O3 Sm1 C16 147.74(11) . . ?
O2 Sm1 C16 25.95(11) . . ?
O4 Sm1 C16 159.60(11) . . ?
O1 Sm1 C16 26.04(11) . . ?
N1 Sm1 C16 84.35(12) . . ?
N3 Sm1 C16 96.93(13) . . ?
N2 Sm1 C16 92.05(11) . . ?
C23 Sm1 C16 173.04(13) . . ?

_refine_diff_density_max         1.510
_refine_diff_density_min         -1.586
_refine_diff_density_rms         0.098

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_11
_database_code_depnum_ccdc_archive 'CCDC 1514989'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 Er2 I6 N6 O14'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2319.10

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'
I I -0.4742 1.8119 '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      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                   11.2063(3)
_cell_length_b                   12.7987(4)
_cell_length_c                   14.4542(4)
_cell_angle_alpha                68.9140(10)
_cell_angle_beta                 88.394(2)
_cell_angle_gamma                72.6400(10)
_cell_volume                     1838.85(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    27443
_cell_measurement_theta_min      4.359
_cell_measurement_theta_max      51.748

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.094
_exptl_crystal_F_000             1090
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.186
_exptl_absorpt_coefficient_mu    4.851
_shelx_estimated_absorpt_T_min   0.341
_shelx_estimated_absorpt_T_max   0.466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6522
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27437
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.516
_diffrn_reflns_theta_max         30.612
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10316
_reflns_number_gt                8428
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0333P)²+1.9187P] 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         10316
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.0837
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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 0.63972(2) 0.78216(2) 0.00907(2) 0.02917(5) Uani 1 1 d . . . . .
I3A I 0.3816(3) 1.2562(4) -0.6263(2) 0.0640(6) Uani 0.65(3) 1 d . . P A 1
I3B I 0.419(2) 1.2619(5) -0.6180(6) 0.085(3) Uani 0.35(3) 1 d . . P A 2
I1 I 0.17046(5) 0.62996(5) 0.53839(4) 0.10566(19) Uani 1 1 d . . . . .
I2 I 1.20440(4) 1.02808(5) -0.41671(3) 0.09215(17) Uani 1 1 d . . . . .
O5 O 0.5172(3) 0.9493(2) -0.1078(2) 0.0396(6) Uani 1 1 d . . . . .
O6 O 0.6271(3) 0.8881(2) 0.1071(2) 0.0379(6) Uani 1 1 d . . . . .
O1 O 0.5985(3) 0.6466(2) 0.1681(2) 0.0408(7) Uani 1 1 d . . . . .
O2 O 0.4367(3) 0.7921(3) 0.0789(2) 0.0472(7) Uani 1 1 d . . . . .
OW1 O 0.8119(5) 0.0761(6) 0.0084(4) 0.0840(16) Uani 1 1 d . . . . .
O3 O 0.7601(3) 0.7847(2) -0.1365(2) 0.0397(6) Uani 1 1 d . . . . .
O4 O 0.7839(3) 0.8938(3) -0.0553(2) 0.0465(7) Uani 1 1 d . . . . .
N2 N 0.7452(3) 0.5713(3) 0.0198(2) 0.0344(7) Uani 1 1 d . . . . .
N1 N 0.5229(3) 0.7054(3) -0.0846(2) 0.0360(7) Uani 1 1 d . . . . .
N3 N 0.8490(3) 0.6739(3) 0.1138(3) 0.0430(8) Uani 1 1 d . . . . .
C30 C 0.4440(3) 1.0509(3) -0.1503(3) 0.0292(7) Uani 1 1 d . . . . .
C11 C 0.9036(4) 0.5585(4) 0.1355(3) 0.0436(10) Uani 1 1 d . . . . .
C5 C 0.5734(4) 0.5987(3) -0.0911(3) 0.0340(8) Uani 1 1 d . . . . .
C16 C 0.4859(4) 0.7099(3) 0.1602(3) 0.0372(9) Uani 1 1 d . . . . .
C34 C 0.4187(5) 1.1948(4) -0.4680(3) 0.0466(10) Uani 1 1 d . . . . .
C23 C 0.8079(4) 0.8581(3) -0.1261(3) 0.0359(8) Uani 1 1 d . . . . .
C12 C 1.0047(5) 0.4943(5) 0.2085(4) 0.0689(16) Uani 1 1 d . . . . .
H12 H 1.0415 0.4140 0.2235 0.083 Uiso 1 1 calc R U . . .
C3 C 0.3912(5) 0.6227(4) -0.1875(4) 0.0502(11) Uani 1 1 d . . . . .
H3 H 0.3475 0.5947 -0.2221 0.060 Uiso 1 1 calc R U . . .
C18 C 0.3082(4) 0.7809(4) 0.2536(3) 0.0467(10) Uani 1 1 d . . . . .
H18 H 0.2844 0.8529 0.2006 0.056 Uiso 1 1 calc R U . . .
C17 C 0.4109(4) 0.6907(3) 0.2484(3) 0.0351(8) Uani 1 1 d . . . . .
C6 C 0.6978(4) 0.5274(3) -0.0371(3) 0.0378(9) Uani 1 1 d . . . . .
C2 C 0.3393(4) 0.7316(4) -0.1815(3) 0.0480(10) Uani 1 1 d . . . . .
H2 H 0.2595 0.7788 -0.2118 0.058 Uiso 1 1 calc R U . . .
C31 C 0.4381(3) 1.1031(3) -0.2619(3) 0.0307(7) Uani 1 1 d . . . . .
C36 C 0.5151(4) 1.0419(4) -0.3139(3) 0.0385(9) Uani 1 1 d . . . . .
H36 H 0.5734 0.9691 -0.2793 0.046 Uiso 1 1 calc R U . . .
C10 C 0.8546(4) 0.5059(3) 0.0757(3) 0.0404(9) Uani 1 1 d . . . . .
C32 C 0.3532(4) 1.2122(3) -0.3145(3) 0.0418(10) Uani 1 1 d . . . . .
H32 H 0.3024 1.2550 -0.2801 0.050 Uiso 1 1 calc R U . . .
C14 C 0.9975(5) 0.6687(6) 0.2322(5) 0.0792(18) Uani 1 1 d . . . . .
H14 H 1.0295 0.7091 0.2621 0.095 Uiso 1 1 calc R U . . .
C20 C 0.2739(5) 0.6571(4) 0.4130(4) 0.0515(11) Uani 1 1 d . . . . .
C1 C 0.4076(4) 0.7693(4) -0.1298(3) 0.0445(10) Uani 1 1 d . . . . .
H1 H 0.3720 0.8430 -0.1260 0.053 Uiso 1 1 calc R U . . .
C35 C 0.5066(4) 1.0875(4) -0.4169(3) 0.0474(10) Uani 1 1 d . . . . .
H35 H 0.5596 1.0462 -0.4514 0.057 Uiso 1 1 calc R U . . .
C27 C 1.0703(4) 0.9757(4) -0.3235(4) 0.0495(11) Uani 1 1 d . . . . .
C24 C 0.8974(4) 0.9007(3) -0.1971(3) 0.0354(8) Uani 1 1 d . . . . .
C7 C 0.7615(4) 0.4170(4) -0.0412(4) 0.0493(11) Uani 1 1 d . . . . .
H7 H 0.7280 0.3882 -0.0815 0.059 Uiso 1 1 calc R U . . .
C33 C 0.3428(5) 1.2584(4) -0.4174(3) 0.0486(11) Uani 1 1 d . . . . .
H33 H 0.2853 1.3317 -0.4521 0.058 Uiso 1 1 calc R U . . .
C22 C 0.4441(5) 0.5839(4) 0.3276(3) 0.0498(11) Uani 1 1 d . . . . .
H22 H 0.5143 0.5235 0.3260 0.060 Uiso 1 1 calc R U . . .
C8 C 0.8729(5) 0.3524(4) 0.0147(4) 0.0615(14) Uani 1 1 d . . . . .
H8 H 0.9163 0.2792 0.0124 0.074 Uiso 1 1 calc R U . . .
C26 C 0.9956(5) 0.9203(5) -0.3503(4) 0.0543(12) Uani 1 1 d . . . . .
H26 H 1.0031 0.9082 -0.4102 0.065 Uiso 1 1 calc R U . . .
C9 C 0.9211(4) 0.3953(4) 0.0745(4) 0.0531(12) Uani 1 1 d . . . . .
H9 H 0.9967 0.3515 0.1134 0.064 Uiso 1 1 calc R U . . .
C28 C 1.0605(4) 0.9931(4) -0.2357(4) 0.0507(11) Uani 1 1 d . . . . .
H28 H 1.1121 1.0295 -0.2183 0.061 Uiso 1 1 calc R U . . .
C25 C 0.9095(4) 0.8833(4) -0.2860(3) 0.0460(10) Uani 1 1 d . . . . .
H25 H 0.8590 0.8460 -0.3032 0.055 Uiso 1 1 calc R U . . .
C19 C 0.2411(4) 0.7650(5) 0.3361(4) 0.0562(12) Uani 1 1 d . . . . .
H19 H 0.1742 0.8267 0.3399 0.067 Uiso 1 1 calc R U . . .
C4 C 0.5088(4) 0.5562(4) -0.1415(3) 0.0446(10) Uani 1 1 d . . . . .
H4 H 0.5453 0.4820 -0.1442 0.054 Uiso 1 1 calc R U . . .
C29 C 0.9740(4) 0.9568(4) -0.1724(3) 0.0449(10) Uani 1 1 d . . . . .
H29 H 0.9667 0.9697 -0.1128 0.054 Uiso 1 1 calc R U . . .
C15 C 0.8963(4) 0.7276(5) 0.1607(4) 0.0562(12) Uani 1 1 d . . . . .
H15 H 0.8596 0.8081 0.1446 0.067 Uiso 1 1 calc R U . . .
C21 C 0.3744(5) 0.5653(4) 0.4097(4) 0.0580(13) Uani 1 1 d . . . . .
H21 H 0.3952 0.4922 0.4614 0.070 Uiso 1 1 calc R U . . .
C13 C 1.0489(6) 0.5506(6) 0.2575(5) 0.086(2) Uani 1 1 d . . . . .
H13 H 1.1138 0.5083 0.3080 0.103 Uiso 1 1 calc R U . . .
HW1A H 0.809(7) 0.012(7) -0.002(5) 0.10(3) Uiso 1 1 d . . . . .
HW1B H 0.754(6) 0.110(6) -0.008(5) 0.07(2) Uiso 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 O5 2.257(3) . ?
Er1 O6 2.265(2) . ?
Er1 O4 2.420(3) . ?
Er1 O2 2.450(3) . ?
Er1 O1 2.461(3) . ?
Er1 O3 2.463(3) . ?
Er1 N1 2.517(3) . ?
Er1 N3 2.542(3) . ?
Er1 N2 2.552(3) . ?
Er1 C23 2.799(4) . ?
Er1 C16 2.809(4) . ?
I3A C34 2.143(5) . ?
I3B C34 2.026(8) . ?
I1 C20 2.102(4) . ?
I2 C27 2.088(4) . ?
O5 C30 1.248(4) . ?
O6 C30 1.259(4) 2_675 ?
O1 C16 1.263(5) . ?
O2 C16 1.263(5) . ?
OW1 HW1A 0.89(8) . ?
OW1 HW1B 0.66(6) . ?
O3 C23 1.264(5) . ?
O4 C23 1.257(5) . ?
N2 C6 1.345(5) . ?
N2 C10 1.347(5) . ?
N1 C1 1.340(5) . ?
N1 C5 1.350(5) . ?
N3 C15 1.337(6) . ?
N3 C11 1.338(5) . ?
C30 O6 1.259(4) 2_675 ?
C30 C31 1.502(5) . ?
C11 C12 1.400(6) . ?
C11 C10 1.472(6) . ?
C5 C4 1.378(6) . ?
C5 C6 1.474(6) . ?
C16 C17 1.493(5) . ?
C34 C33 1.378(6) . ?
C34 C35 1.381(6) . ?
C23 C24 1.491(5) . ?
C12 C13 1.366(8) . ?
C12 H12 0.9300 . ?
C3 C4 1.370(7) . ?
C3 C2 1.374(6) . ?
C3 H3 0.9300 . ?
C18 C19 1.377(6) . ?
C18 C17 1.388(6) . ?
C18 H18 0.9300 . ?
C17 C22 1.383(6) . ?
C6 C7 1.402(5) . ?
C2 C1 1.375(6) . ?
C2 H2 0.9300 . ?
C31 C36 1.381(5) . ?
C31 C32 1.385(5) . ?
C36 C35 1.384(6) . ?
C36 H36 0.9300 . ?
C10 C9 1.395(6) . ?
C32 C33 1.383(6) . ?
C32 H32 0.9300 . ?
C14 C13 1.358(9) . ?
C14 C15 1.385(7) . ?
C14 H14 0.9300 . ?
C20 C19 1.376(7) . ?
C20 C21 1.378(7) . ?
C1 H1 0.9300 . ?
C35 H35 0.9300 . ?
C27 C28 1.363(7) . ?
C27 C26 1.386(7) . ?
C24 C25 1.377(6) . ?
C24 C29 1.397(6) . ?
C7 C8 1.362(7) . ?
C7 H7 0.9300 . ?
C33 H33 0.9300 . ?
C22 C21 1.389(6) . ?
C22 H22 0.9300 . ?
C8 C9 1.374(7) . ?
C8 H8 0.9300 . ?
C26 C25 1.388(6) . ?
C26 H26 0.9300 . ?
C9 H9 0.9300 . ?
C28 C29 1.381(6) . ?
C28 H28 0.9300 . ?
C25 H25 0.9300 . ?
C19 H19 0.9300 . ?
C4 H4 0.9300 . ?
C29 H29 0.9300 . ?
C15 H15 0.9300 . ?
C21 H21 0.9300 . ?
C13 H13 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
O5 Er1 O6 86.92(10) . . ?
O5 Er1 O4 76.96(11) . . ?
O6 Er1 O4 75.96(10) . . ?
O5 Er1 O2 80.05(10) . . ?
O6 Er1 O2 74.73(11) . . ?
O4 Er1 O2 143.40(10) . . ?
O5 Er1 O1 133.01(10) . . ?
O6 Er1 O1 78.99(10) . . ?
O4 Er1 O1 139.37(10) . . ?
O2 Er1 O1 53.04(9) . . ?
O5 Er1 O3 79.66(10) . . ?
O6 Er1 O3 129.31(10) . . ?
O4 Er1 O3 53.44(9) . . ?
O2 Er1 O3 147.19(10) . . ?
O1 Er1 O3 141.81(9) . . ?
O5 Er1 N1 77.62(10) . . ?
O6 Er1 N1 146.71(10) . . ?
O4 Er1 N1 127.25(10) . . ?
O2 Er1 N1 73.67(11) . . ?
O1 Er1 N1 90.21(10) . . ?
O3 Er1 N1 76.97(10) . . ?
O5 Er1 N3 147.51(11) . . ?
O6 Er1 N3 79.38(11) . . ?
O4 Er1 N3 71.20(11) . . ?
O2 Er1 N3 123.31(11) . . ?
O1 Er1 N3 73.12(11) . . ?
O3 Er1 N3 86.47(11) . . ?
N1 Er1 N3 127.64(11) . . ?
O5 Er1 N2 135.41(10) . . ?
O6 Er1 N2 137.66(10) . . ?
O4 Er1 N2 108.21(10) . . ?
O2 Er1 N2 108.18(10) . . ?
O1 Er1 N2 71.44(9) . . ?
O3 Er1 N2 70.59(9) . . ?
N1 Er1 N2 64.04(10) . . ?
N3 Er1 N2 63.60(11) . . ?
O5 Er1 C23 76.37(11) . . ?
O6 Er1 C23 102.50(11) . . ?
O4 Er1 C23 26.62(10) . . ?
O2 Er1 C23 156.38(10) . . ?
O1 Er1 C23 150.37(10) . . ?
O3 Er1 C23 26.83(10) . . ?
N1 Er1 C23 102.21(11) . . ?
N3 Er1 C23 78.06(11) . . ?
N2 Er1 C23 89.80(10) . . ?
O5 Er1 C16 106.34(11) . . ?
O6 Er1 C16 72.19(11) . . ?
O4 Er1 C16 147.67(11) . . ?
O2 Er1 C16 26.69(10) . . ?
O1 Er1 C16 26.69(10) . . ?
O3 Er1 C16 158.42(10) . . ?
N1 Er1 C16 84.02(11) . . ?
N3 Er1 C16 97.34(12) . . ?
N2 Er1 C16 92.01(10) . . ?
C23 Er1 C16 173.67(12) . . ?
C30 O5 Er1 162.7(3) . . ?
C30 O6 Er1 146.2(3) 2_675 . ?
C16 O1 Er1 92.2(2) . . ?
C16 O2 Er1 92.7(2) . . ?
HW1A OW1 HW1B 99(7) . . ?
C23 O3 Er1 91.6(2) . . ?
C23 O4 Er1 93.8(2) . . ?
C6 N2 C10 118.9(3) . . ?
C6 N2 Er1 120.2(2) . . ?
C10 N2 Er1 120.6(3) . . ?
C1 N1 C5 117.5(4) . . ?
C1 N1 Er1 121.0(3) . . ?
C5 N1 Er1 121.5(3) . . ?
C15 N3 C11 118.5(4) . . ?
C15 N3 Er1 119.6(3) . . ?
C11 N3 Er1 121.1(3) . . ?
O5 C30 O6 125.1(3) . 2_675 ?
O5 C30 C31 117.3(3) . . ?
O6 C30 C31 117.6(3) 2_675 . ?
N3 C11 C12 120.9(5) . . ?
N3 C11 C10 116.2(4) . . ?
C12 C11 C10 122.8(4) . . ?
N1 C5 C4 121.5(4) . . ?
N1 C5 C6 116.7(3) . . ?
C4 C5 C6 121.7(4) . . ?
O1 C16 O2 120.5(4) . . ?
O1 C16 C17 120.1(4) . . ?
O2 C16 C17 119.4(4) . . ?
O1 C16 Er1 61.1(2) . . ?
O2 C16 Er1 60.6(2) . . ?
C17 C16 Er1 167.2(3) . . ?
C33 C34 C35 120.7(4) . . ?
C33 C34 I3B 121.7(5) . . ?
C35 C34 I3B 117.3(5) . . ?
C33 C34 I3A 118.3(3) . . ?
C35 C34 I3A 120.6(3) . . ?
O4 C23 O3 121.1(4) . . ?
O4 C23 C24 119.1(4) . . ?
O3 C23 C24 119.8(4) . . ?
O4 C23 Er1 59.6(2) . . ?
O3 C23 Er1 61.6(2) . . ?
C24 C23 Er1 178.6(3) . . ?
C13 C12 C11 119.4(5) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C4 C3 C2 118.6(4) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C19 C18 C17 120.9(4) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C22 C17 C18 118.7(4) . . ?
C22 C17 C16 120.8(4) . . ?
C18 C17 C16 120.5(4) . . ?
N2 C6 C7 121.4(4) . . ?
N2 C6 C5 116.7(3) . . ?
C7 C6 C5 121.9(4) . . ?
C3 C2 C1 118.6(4) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C36 C31 C32 118.8(4) . . ?
C36 C31 C30 120.6(3) . . ?
C32 C31 C30 120.5(3) . . ?
C31 C36 C35 120.9(4) . . ?
C31 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
N2 C10 C9 121.8(4) . . ?
N2 C10 C11 116.8(3) . . ?
C9 C10 C11 121.3(4) . . ?
C33 C32 C31 121.0(4) . . ?
C33 C32 H32 119.5 . . ?
C31 C32 H32 119.5 . . ?
C13 C14 C15 118.5(6) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
C19 C20 C21 121.1(4) . . ?
C19 C20 I1 120.1(3) . . ?
C21 C20 I1 118.8(4) . . ?
N1 C1 C2 123.5(4) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C34 C35 C36 119.3(4) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.3 . . ?
C28 C27 C26 121.1(4) . . ?
C28 C27 I2 119.3(3) . . ?
C26 C27 I2 119.6(4) . . ?
C25 C24 C29 118.6(4) . . ?
C25 C24 C23 121.7(4) . . ?
C29 C24 C23 119.7(4) . . ?
C8 C7 C6 119.2(5) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C34 C33 C32 119.3(4) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C17 C22 C21 121.0(4) . . ?
C17 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C7 C8 C9 120.0(4) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C27 C26 C25 118.7(4) . . ?
C27 C26 H26 120.7 . . ?
C25 C26 H26 120.7 . . ?
C8 C9 C10 118.8(4) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
C27 C28 C29 119.9(4) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C24 C25 C26 121.3(4) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C20 C19 C18 119.5(4) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C3 C4 C5 120.3(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C28 C29 C24 120.4(4) . . ?
C28 C29 H29 119.8 . . ?
C24 C29 H29 119.8 . . ?
N3 C15 C14 122.9(5) . . ?
N3 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
C20 C21 C22 118.8(4) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
C14 C13 C12 119.6(5) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?

_refine_diff_density_max         1.812
_refine_diff_density_min         -2.088
_refine_diff_density_rms         0.115

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_3
_database_code_depnum_ccdc_archive 'CCDC 1514981'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 I6 N6 O14 Pr2'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2266.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 '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                   11.1520(3)
_cell_length_b                   12.9748(4)
_cell_length_c                   14.5744(4)
_cell_angle_alpha                69.2460(10)
_cell_angle_beta                 88.950(2)
_cell_angle_gamma                73.0660(10)
_cell_volume                     1877.98(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25185
_cell_measurement_theta_min      4.347
_cell_measurement_theta_max      52.043

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_F_000             1072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.221
_exptl_absorpt_coefficient_mu    3.813
_shelx_estimated_absorpt_T_min   0.465
_shelx_estimated_absorpt_T_max   0.486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6513
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25183
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.501
_diffrn_reflns_theta_max         27.792
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8854
_reflns_number_gt                7262
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0428P)²+2.8668P] 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         8854
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0986
_refine_ls_wR_factor_gt          0.0917
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4046(4) 0.2618(4) 0.8698(4) 0.0526(12) Uani 1 1 d . . . . .
H1 H 0.3693 0.3337 0.8749 0.063 Uiso 1 1 calc R U . . .
C2 C 0.3350(5) 0.2263(4) 0.8167(4) 0.0549(12) Uani 1 1 d . . . . .
H2 H 0.2553 0.2729 0.7862 0.066 Uiso 1 1 calc R U . . .
C3 C 0.3875(5) 0.1194(5) 0.8103(4) 0.0568(12) Uani 1 1 d . . . . .
H3 H 0.3435 0.0921 0.7753 0.068 Uiso 1 1 calc R U . . .
C4 C 0.5038(5) 0.0545(4) 0.8554(4) 0.0524(11) Uani 1 1 d . . . . .
H4 H 0.5400 -0.0178 0.8513 0.063 Uiso 1 1 calc R U . . .
C5 C 0.5694(4) 0.0945(3) 0.9075(3) 0.0389(9) Uani 1 1 d . . . . .
C6 C 0.6948(4) 0.0232(3) 0.9608(3) 0.0418(10) Uani 1 1 d . . . . .
C7 C 0.7567(5) -0.0852(4) 0.9560(4) 0.0587(13) Uani 1 1 d . . . . .
H7 H 0.7216 -0.1127 0.9156 0.070 Uiso 1 1 calc R U . . .
C8 C 0.8693(5) -0.1503(4) 1.0112(5) 0.0694(16) Uani 1 1 d . . . . .
H8 H 0.9108 -0.2226 1.0087 0.083 Uiso 1 1 calc R U . . .
C9 C 0.9202(5) -0.1092(4) 1.0693(4) 0.0603(14) Uani 1 1 d . . . . .
H9 H 0.9971 -0.1527 1.1064 0.072 Uiso 1 1 calc R U . . .
C10 C 0.8562(4) -0.0012(4) 1.0730(3) 0.0466(11) Uani 1 1 d . . . . .
C23 C 0.4825(4) 0.2105(4) 1.1665(3) 0.0420(9) Uani 1 1 d . . . . .
C24 C 0.4077(4) 0.1920(4) 1.2536(3) 0.0422(9) Uani 1 1 d . . . . .
C29 C 0.4397(5) 0.0870(4) 1.3309(4) 0.0579(13) Uani 1 1 d . . . . .
H18 H 0.5087 0.0272 1.3286 0.069 Uiso 1 1 calc R U . . .
C28 C 0.3709(6) 0.0688(5) 1.4121(4) 0.0699(15) Uani 1 1 d . . . . .
H19 H 0.3924 -0.0030 1.4633 0.084 Uiso 1 1 calc R U . . .
C27 C 0.2699(5) 0.1586(5) 1.4161(4) 0.0627(14) Uani 1 1 d . . . . .
C26 C 0.2389(5) 0.2648(5) 1.3404(4) 0.0651(14) Uani 1 1 d . . . . .
H21 H 0.1729 0.3258 1.3445 0.078 Uiso 1 1 calc R U . . .
C25 C 0.3053(4) 0.2810(4) 1.2588(4) 0.0537(12) Uani 1 1 d . . . . .
H22 H 0.2816 0.3521 1.2067 0.064 Uiso 1 1 calc R U . . .
C16 C 0.8168(4) 0.3582(4) 0.8719(3) 0.0413(9) Uani 1 1 d . . . . .
C17 C 0.9048(4) 0.4027(3) 0.8004(3) 0.0420(9) Uani 1 1 d . . . . .
C22 C 0.9140(5) 0.3846(4) 0.7127(4) 0.0521(11) Uani 1 1 d . . . . .
H25 H 0.8631 0.3472 0.6961 0.063 Uiso 1 1 calc R U . . .
C21 C 0.9997(5) 0.4224(5) 0.6489(4) 0.0603(13) Uani 1 1 d . . . . .
H26 H 1.0064 0.4103 0.5896 0.072 Uiso 1 1 calc R U . . .
C20 C 1.0738(5) 0.4772(5) 0.6737(4) 0.0557(12) Uani 1 1 d . . . . .
C19 C 1.0666(5) 0.4961(4) 0.7604(4) 0.0573(12) Uani 1 1 d . . . . .
H28 H 1.1184 0.5331 0.7763 0.069 Uiso 1 1 calc R U . . .
C18 C 0.9808(4) 0.4593(4) 0.8244(4) 0.0519(11) Uani 1 1 d . . . . .
H29 H 0.9742 0.4725 0.8832 0.062 Uiso 1 1 calc R U . . .
C30 C 0.5639(4) 0.4477(3) 1.1560(3) 0.0356(8) Uani 1 1 d . . . . .
C31 C 0.5661(4) 0.3962(3) 1.2659(3) 0.0366(8) Uani 1 1 d . . . . .
C32 C 0.4856(4) 0.4563(4) 1.3162(3) 0.0476(10) Uani 1 1 d . . . . .
H32 H 0.4277 0.5278 1.2813 0.057 Uiso 1 1 calc R U . . .
C33 C 0.4909(5) 0.4108(5) 1.4175(4) 0.0600(13) Uani 1 1 d . . . . .
H33 H 0.4359 0.4508 1.4509 0.072 Uiso 1 1 calc R U . . .
C34 C 0.5781(6) 0.3056(4) 1.4691(4) 0.0591(13) Uani 1 1 d . . . . .
C35 C 0.6548(5) 0.2429(4) 1.4208(4) 0.0581(13) Uani 1 1 d . . . . .
H35 H 0.7108 0.1704 1.4559 0.070 Uiso 1 1 calc R U . . .
C36 C 0.6480(5) 0.2886(4) 1.3192(3) 0.0512(11) Uani 1 1 d . . . . .
H36 H 0.6997 0.2459 1.2861 0.061 Uiso 1 1 calc R U . . .
N1 N 0.5198(3) 0.1988(3) 0.9143(3) 0.0428(8) Uani 1 1 d . . . . .
N2 N 0.7461(3) 0.0643(3) 1.0183(3) 0.0393(8) Uani 1 1 d . . . . .
N3 N 0.8596(4) 0.1605(3) 1.1154(3) 0.0516(9) Uani 1 1 d . . . . .
O4 O 0.5934(3) 0.1464(2) 1.1741(2) 0.0476(7) Uani 1 1 d . . . . .
O3 O 0.4331(3) 0.2919(3) 1.0866(2) 0.0567(9) Uani 1 1 d . . . . .
O2 O 0.7670(3) 0.2880(3) 0.8596(2) 0.0464(7) Uani 1 1 d . . . . .
O1 O 0.7976(3) 0.3907(3) 0.9440(3) 0.0559(8) Uani 1 1 d . . . . .
O6 O 0.5097(3) 0.4535(2) 0.8875(2) 0.0505(8) Uani 1 1 d . . . . .
O5 O 0.6385(3) 0.3885(2) 1.1146(2) 0.0467(7) Uani 1 1 d . . . . .
I2 I 0.16679(6) 0.13027(6) 1.53916(4) 0.1207(2) Uani 1 1 d . . . . .
I1 I 1.20603(5) 0.52898(6) 0.58081(4) 0.1060(2) Uani 1 1 d . . . . .
Pr1 Pr 0.64077(2) 0.28260(2) 1.00964(2) 0.03429(7) Uani 1 1 d . . . . .
OW1 O 0.1848(6) 0.4188(7) 0.9978(5) 0.100(2) Uani 1 1 d . . . . .
I3A I 0.6125(3) 0.2484(4) 1.6277(2) 0.0763(9) Uani 0.52(2) 1 d . . P A 1
I3B I 0.5737(16) 0.2377(4) 1.6167(5) 0.116(2) Uani 0.48(2) 1 d . . P A 2
C11 C 0.9099(4) 0.0469(4) 1.1343(4) 0.0506(11) Uani 1 1 d . . . . .
C15 C 0.9099(5) 0.2087(5) 1.1659(4) 0.0697(16) Uani 1 1 d . . . . .
H15 H 0.8771 0.2879 1.1516 0.084 Uiso 1 1 calc R U . . .
C12 C 1.0092(6) -0.0197(5) 1.2067(5) 0.0809(19) Uani 1 1 d . . . . .
H12 H 1.0431 -0.0986 1.2197 0.097 Uiso 1 1 calc R U . . .
C14 C 1.0088(6) 0.1452(7) 1.2383(5) 0.092(2) Uani 1 1 d . . . . .
H14 H 1.0412 0.1813 1.2724 0.111 Uiso 1 1 calc R U . . .
C13 C 1.0575(6) 0.0316(7) 1.2591(6) 0.100(2) Uani 1 1 d . . . . .
H13 H 1.1232 -0.0124 1.3084 0.120 Uiso 1 1 calc R U . . .
HW1A H 0.241(7) 0.390(7) 1.013(6) 0.09(3) Uiso 1 1 d . . . . .
HW1B H 0.166(7) 0.482(7) 0.994(6) 0.09(3) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.336(6) . ?
C1 C2 1.377(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.374(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.352(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.379(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.344(5) . ?
C5 C6 1.481(6) . ?
C6 N2 1.351(6) . ?
C6 C7 1.401(6) . ?
C7 C8 1.369(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.356(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.395(6) . ?
C9 H9 0.9300 . ?
C10 N2 1.346(5) . ?
C10 C11 1.476(7) . ?
C23 O4 1.254(5) . ?
C23 O3 1.260(5) . ?
C23 C24 1.492(6) . ?
C23 Pr1 2.918(4) . ?
C24 C29 1.377(6) . ?
C24 C25 1.391(6) . ?
C29 C28 1.385(7) . ?
C29 H18 0.9300 . ?
C28 C27 1.382(8) . ?
C28 H19 0.9300 . ?
C27 C26 1.377(8) . ?
C27 I2 2.093(5) . ?
C26 C25 1.373(7) . ?
C26 H21 0.9300 . ?
C25 H22 0.9300 . ?
C16 O1 1.257(5) . ?
C16 O2 1.259(5) . ?
C16 C17 1.500(6) . ?
C16 Pr1 2.903(4) . ?
C17 C22 1.375(6) . ?
C17 C18 1.391(6) . ?
C22 C21 1.391(7) . ?
C22 H25 0.9300 . ?
C21 C20 1.362(7) . ?
C21 H26 0.9300 . ?
C20 C19 1.366(7) . ?
C20 I1 2.078(5) . ?
C19 C18 1.389(7) . ?
C19 H28 0.9300 . ?
C18 H29 0.9300 . ?
C30 O6 1.244(5) 2_667 ?
C30 O5 1.258(5) . ?
C30 C31 1.499(6) . ?
C31 C36 1.379(6) . ?
C31 C32 1.388(6) . ?
C32 C33 1.377(7) . ?
C32 H32 0.9300 . ?
C33 C34 1.379(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.366(7) . ?
C34 I3B 2.021(7) . ?
C34 I3A 2.167(6) . ?
C35 C36 1.381(6) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N1 Pr1 2.631(4) . ?
N2 Pr1 2.689(3) . ?
N3 C15 1.339(7) . ?
N3 C11 1.342(6) . ?
N3 Pr1 2.645(4) . ?
O4 Pr1 2.577(3) . ?
O3 Pr1 2.545(3) . ?
O2 Pr1 2.569(3) . ?
O1 Pr1 2.522(3) . ?
O6 C30 1.244(5) 2_667 ?
O6 Pr1 2.374(3) . ?
O5 Pr1 2.386(3) . ?
OW1 HW1A 0.62(7) . ?
OW1 HW1B 0.77(7) . ?
C11 C12 1.388(7) . ?
C15 C14 1.381(8) . ?
C15 H15 0.9300 . ?
C12 C13 1.380(10) . ?
C12 H12 0.9300 . ?
C14 C13 1.335(10) . ?
C14 H14 0.9300 . ?
C13 H13 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
N1 C1 C2 123.6(4) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 117.7(5) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C4 C3 C2 119.3(5) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 120.5(4) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
N1 C5 C4 121.0(4) . . ?
N1 C5 C6 117.3(4) . . ?
C4 C5 C6 121.6(4) . . ?
N2 C6 C7 120.6(4) . . ?
N2 C6 C5 117.5(3) . . ?
C7 C6 C5 121.9(4) . . ?
C8 C7 C6 119.4(5) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C9 C8 C7 119.9(5) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 119.4(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 121.3(5) . . ?
N2 C10 C11 117.9(4) . . ?
C9 C10 C11 120.8(4) . . ?
O4 C23 O3 121.1(4) . . ?
O4 C23 C24 119.9(4) . . ?
O3 C23 C24 119.0(4) . . ?
O4 C23 Pr1 61.9(2) . . ?
O3 C23 Pr1 60.4(2) . . ?
C24 C23 Pr1 168.0(3) . . ?
C29 C24 C25 118.7(4) . . ?
C29 C24 C23 120.7(4) . . ?
C25 C24 C23 120.6(4) . . ?
C24 C29 C28 121.2(5) . . ?
C24 C29 H18 119.4 . . ?
C28 C29 H18 119.4 . . ?
C27 C28 C29 119.1(5) . . ?
C27 C28 H19 120.4 . . ?
C29 C28 H19 120.4 . . ?
C26 C27 C28 120.2(5) . . ?
C26 C27 I2 120.9(4) . . ?
C28 C27 I2 118.9(4) . . ?
C25 C26 C27 120.2(5) . . ?
C25 C26 H21 119.9 . . ?
C27 C26 H21 119.9 . . ?
C26 C25 C24 120.5(5) . . ?
C26 C25 H22 119.8 . . ?
C24 C25 H22 119.8 . . ?
O1 C16 O2 122.1(4) . . ?
O1 C16 C17 118.4(4) . . ?
O2 C16 C17 119.5(4) . . ?
O1 C16 Pr1 60.0(2) . . ?
O2 C16 Pr1 62.2(2) . . ?
C17 C16 Pr1 177.5(3) . . ?
C22 C17 C18 119.7(4) . . ?
C22 C17 C16 120.6(4) . . ?
C18 C17 C16 119.7(4) . . ?
C17 C22 C21 119.8(5) . . ?
C17 C22 H25 120.1 . . ?
C21 C22 H25 120.1 . . ?
C20 C21 C22 119.7(5) . . ?
C20 C21 H26 120.2 . . ?
C22 C21 H26 120.2 . . ?
C21 C20 C19 121.6(5) . . ?
C21 C20 I1 119.8(4) . . ?
C19 C20 I1 118.5(4) . . ?
C20 C19 C18 119.2(5) . . ?
C20 C19 H28 120.4 . . ?
C18 C19 H28 120.4 . . ?
C19 C18 C17 120.0(5) . . ?
C19 C18 H29 120.0 . . ?
C17 C18 H29 120.0 . . ?
O6 C30 O5 124.8(4) 2_667 . ?
O6 C30 C31 117.7(4) 2_667 . ?
O5 C30 C31 117.5(3) . . ?
C36 C31 C32 118.6(4) . . ?
C36 C31 C30 120.9(4) . . ?
C32 C31 C30 120.5(4) . . ?
C33 C32 C31 120.5(4) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C32 C33 C34 119.6(4) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
C35 C34 C33 120.9(5) . . ?
C35 C34 I3B 120.8(4) . . ?
C33 C34 I3B 117.9(4) . . ?
C35 C34 I3A 118.7(4) . . ?
C33 C34 I3A 120.0(4) . . ?
C34 C35 C36 119.1(4) . . ?
C34 C35 H35 120.4 . . ?
C36 C35 H35 120.4 . . ?
C31 C36 C35 121.3(4) . . ?
C31 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
C1 N1 C5 117.8(4) . . ?
C1 N1 Pr1 119.5(3) . . ?
C5 N1 Pr1 122.7(3) . . ?
C10 N2 C6 119.3(4) . . ?
C10 N2 Pr1 120.3(3) . . ?
C6 N2 Pr1 120.1(3) . . ?
C15 N3 C11 118.5(4) . . ?
C15 N3 Pr1 118.3(3) . . ?
C11 N3 Pr1 122.2(3) . . ?
C23 O4 Pr1 92.7(3) . . ?
C23 O3 Pr1 94.1(3) . . ?
C16 O2 Pr1 92.1(3) . . ?
C16 O1 Pr1 94.4(3) . . ?
C30 O6 Pr1 163.4(3) 2_667 . ?
C30 O5 Pr1 141.4(3) . . ?
O6 Pr1 O5 89.45(10) . . ?
O6 Pr1 O1 79.21(12) . . ?
O5 Pr1 O1 76.02(11) . . ?
O6 Pr1 O3 80.86(11) . . ?
O5 Pr1 O3 75.12(12) . . ?
O1 Pr1 O3 144.84(11) . . ?
O6 Pr1 O2 79.42(11) . . ?
O5 Pr1 O2 127.20(11) . . ?
O1 Pr1 O2 51.24(10) . . ?
O3 Pr1 O2 149.72(11) . . ?
O6 Pr1 O4 131.46(11) . . ?
O5 Pr1 O4 78.31(10) . . ?
O1 Pr1 O4 139.41(11) . . ?
O3 Pr1 O4 50.61(10) . . ?
O2 Pr1 O4 143.62(9) . . ?
O6 Pr1 N1 77.96(11) . . ?
O5 Pr1 N1 149.62(11) . . ?
O1 Pr1 N1 127.13(11) . . ?
O3 Pr1 N1 75.63(12) . . ?
O2 Pr1 N1 77.93(11) . . ?
O4 Pr1 N1 89.43(11) . . ?
O6 Pr1 N3 150.88(13) . . ?
O5 Pr1 N3 80.27(11) . . ?
O1 Pr1 N3 71.90(12) . . ?
O3 Pr1 N3 121.71(12) . . ?
O2 Pr1 N3 85.26(12) . . ?
O4 Pr1 N3 73.18(12) . . ?
N1 Pr1 N3 122.87(11) . . ?
O6 Pr1 N2 133.75(11) . . ?
O5 Pr1 N2 136.80(10) . . ?
O1 Pr1 N2 107.13(11) . . ?
O3 Pr1 N2 107.60(11) . . ?
O2 Pr1 N2 71.48(10) . . ?
O4 Pr1 N2 72.50(10) . . ?
N1 Pr1 N2 61.54(11) . . ?
N3 Pr1 N2 61.33(12) . . ?
O6 Pr1 C16 77.23(11) . . ?
O5 Pr1 C16 101.51(12) . . ?
O1 Pr1 C16 25.59(11) . . ?
O3 Pr1 C16 157.89(11) . . ?
O2 Pr1 C16 25.69(11) . . ?
O4 Pr1 C16 151.06(10) . . ?
N1 Pr1 C16 102.44(12) . . ?
N3 Pr1 C16 78.25(12) . . ?
N2 Pr1 C16 89.94(11) . . ?
O6 Pr1 C23 106.12(12) . . ?
O5 Pr1 C23 72.33(12) . . ?
O1 Pr1 C23 147.77(11) . . ?
O3 Pr1 C23 25.51(11) . . ?
O2 Pr1 C23 160.25(11) . . ?
O4 Pr1 C23 25.42(10) . . ?
N1 Pr1 C23 84.65(12) . . ?
N3 Pr1 C23 96.64(13) . . ?
N2 Pr1 C23 92.12(11) . . ?
C16 Pr1 C23 172.73(12) . . ?
HW1A OW1 HW1B 116(10) . . ?
N3 C11 C12 120.7(5) . . ?
N3 C11 C10 116.6(4) . . ?
C12 C11 C10 122.7(5) . . ?
N3 C15 C14 122.5(6) . . ?
N3 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
C13 C12 C11 119.6(6) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C13 C14 C15 119.4(7) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C14 C13 C12 119.3(6) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?

_refine_diff_density_max         1.598
_refine_diff_density_min         -2.004
_refine_diff_density_rms         0.098

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_15Prime
_database_code_depnum_ccdc_archive 'CCDC 1514998'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H25 I3 N3 O7 Y'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Rod
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1081.20

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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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                   8.7799(4)
_cell_length_b                   13.5630(6)
_cell_length_c                   15.5082(7)
_cell_angle_alpha                103.533(2)
_cell_angle_beta                 91.2620(10)
_cell_angle_gamma                93.5510(10)
_cell_volume                     1790.75(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    19727
_cell_measurement_theta_min      5.292
_cell_measurement_theta_max      52.606
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_F_000             1032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.433
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    4.267
_shelx_estimated_absorpt_T_min   0.259
_shelx_estimated_absorpt_T_max   0.427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6099
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19727
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.351
_diffrn_reflns_theta_max         26.474
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7369
_reflns_number_gt                5970
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0242P)²+1.0786P] 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         7369
_refine_ls_number_parameters     459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0283
_refine_ls_wR_factor_ref         0.0597
_refine_ls_wR_factor_gt          0.0557
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C34 C -0.0735(4) 0.5908(2) 0.8041(2) 0.0374(8) Uani 1 1 d . . . . .
C20 C 0.6816(4) 1.4641(2) 1.0670(2) 0.0463(9) Uani 1 1 d . . . . .
C27 C 0.2751(4) 0.4838(2) 0.5321(2) 0.0338(7) Uani 1 1 d . . . . .
C35 C -0.1301(4) 0.6586(3) 0.8746(3) 0.0536(10) Uani 1 1 d . . . . .
H35 H -0.2251 0.6444 0.8961 0.064 Uiso 1 1 calc R U . . .
C26 C 0.2052(4) 0.5661(2) 0.5167(2) 0.0352(7) Uani 1 1 d . . . . .
H26 H 0.1278 0.5574 0.4731 0.042 Uiso 1 1 calc R U . . .
C1 C 0.1350(3) 1.0794(2) 0.8366(2) 0.0316(7) Uani 1 1 d . . . . .
H1 H 0.1412 1.0498 0.8848 0.038 Uiso 1 1 calc R U . . .
C18 C 0.7186(4) 1.3281(3) 0.9432(2) 0.0452(9) Uani 1 1 d . . . . .
H18 H 0.7710 1.3017 0.8924 0.054 Uiso 1 1 calc R U . . .
C24 C 0.3673(3) 0.6765(2) 0.63190(19) 0.0272(7) Uani 1 1 d . . . . .
C28 C 0.3907(4) 0.4951(2) 0.5966(2) 0.0404(8) Uani 1 1 d . . . . .
H28 H 0.4369 0.4387 0.6066 0.048 Uiso 1 1 calc R U . . .
C21 C 0.5652(4) 1.4068(3) 1.0936(2) 0.0514(10) Uani 1 1 d . . . . .
H21 H 0.5126 1.4336 1.1442 0.062 Uiso 1 1 calc R U . . .
C2 C 0.0060(4) 1.1290(2) 0.8251(2) 0.0360(8) Uani 1 1 d . . . . .
H2 H -0.0730 1.1318 0.8644 0.043 Uiso 1 1 calc R U . . .
C5 C 0.2447(3) 1.1184(2) 0.71391(19) 0.0264(6) Uani 1 1 d . . . . .
C14 C 0.9564(4) 0.8733(2) 0.6952(2) 0.0367(8) Uani 1 1 d . . . . .
H14 H 1.0308 0.8367 0.7146 0.044 Uiso 1 1 calc R U . . .
C17 C 0.6013(3) 1.2694(2) 0.96865(19) 0.0283(7) Uani 1 1 d . . . . .
C15 C 0.8214(3) 0.8897(2) 0.7395(2) 0.0318(7) Uani 1 1 d . . . . .
H15 H 0.8050 0.8609 0.7876 0.038 Uiso 1 1 calc R U . . .
C31 C 0.0963(3) 0.7699(2) 0.88234(19) 0.0273(7) Uani 1 1 d . . . . .
C25 C 0.2514(4) 0.6625(2) 0.5669(2) 0.0331(7) Uani 1 1 d . . . . .
H25 H 0.2040 0.7185 0.5570 0.040 Uiso 1 1 calc R U . . .
C11 C 0.7359(3) 0.9849(2) 0.64576(19) 0.0279(7) Uani 1 1 d . . . . .
C19 C 0.7590(5) 1.4257(3) 0.9926(3) 0.0539(10) Uani 1 1 d . . . . .
H19 H 0.8381 1.4647 0.9751 0.065 Uiso 1 1 calc R U . . .
C30 C 0.1885(3) 0.8679(2) 0.9227(2) 0.0270(7) Uani 1 1 d . . . . .
C33 C 0.0681(4) 0.6104(3) 0.7734(2) 0.0438(9) Uani 1 1 d . . . . .
H33 H 0.1070 0.5643 0.7263 0.053 Uiso 1 1 calc R U . . .
C16 C 0.5566(3) 1.1655(2) 0.91375(19) 0.0267(7) Uani 1 1 d . . . . .
C3 C -0.0037(4) 1.1739(2) 0.7548(2) 0.0384(8) Uani 1 1 d . . . . .
H3 H -0.0904 1.2064 0.7448 0.046 Uiso 1 1 calc R U . . .
C23 C 0.4131(3) 0.7802(2) 0.68840(19) 0.0277(7) Uani 1 1 d . . . . .
C36 C -0.0449(4) 0.7478(3) 0.9134(2) 0.0452(9) Uani 1 1 d . . . . .
H36 H -0.0832 0.7936 0.9610 0.054 Uiso 1 1 calc R U . . .
C29 C 0.4363(4) 0.5919(2) 0.6460(2) 0.0360(8) Uani 1 1 d . . . . .
H29 H 0.5142 0.6003 0.6892 0.043 Uiso 1 1 calc R U . . .
C6 C 0.3799(3) 1.1137(2) 0.65753(19) 0.0295(7) Uani 1 1 d . . . . .
C32 C 0.1518(4) 0.6997(2) 0.8135(2) 0.0379(8) Uani 1 1 d . . . . .
H32 H 0.2483 0.7127 0.7933 0.045 Uiso 1 1 calc R U . . .
C13 C 0.9771(4) 0.9124(3) 0.6224(2) 0.0412(8) Uani 1 1 d . . . . .
H13 H 1.0658 0.9019 0.5908 0.049 Uiso 1 1 calc R U . . .
C10 C 0.6156(3) 1.0494(2) 0.6245(2) 0.0306(7) Uani 1 1 d . . . . .
C4 C 0.1179(4) 1.1700(2) 0.6990(2) 0.0337(7) Uani 1 1 d . . . . .
H4 H 0.1150 1.2016 0.6519 0.040 Uiso 1 1 calc R U . . .
C7 C 0.3940(4) 1.1687(3) 0.5929(2) 0.0488(10) Uani 1 1 d . . . . .
H7 H 0.3175 1.2099 0.5835 0.059 Uiso 1 1 calc R U . . .
C9 C 0.6329(4) 1.1022(3) 0.5585(2) 0.0524(10) Uani 1 1 d . . . . .
H9 H 0.7199 1.0969 0.5250 0.063 Uiso 1 1 calc R U . . .
C12 C 0.8656(4) 0.9674(3) 0.5964(2) 0.0396(8) Uani 1 1 d . . . . .
H12 H 0.8771 0.9928 0.5460 0.048 Uiso 1 1 calc R U . . .
C8 C 0.5205(5) 1.1621(3) 0.5432(3) 0.0639(12) Uani 1 1 d . . . . .
H8 H 0.5304 1.1981 0.4991 0.077 Uiso 1 1 calc R U . . .
C22 C 0.5271(4) 1.3094(3) 1.0447(2) 0.0427(8) Uani 1 1 d . . . . .
H22 H 0.4498 1.2701 1.0634 0.051 Uiso 1 1 calc R U . . .
N1 N 0.2520(3) 1.07179(17) 0.78140(15) 0.0252(5) Uani 1 1 d . . . . .
N2 N 0.4907(3) 1.05475(17) 0.67316(15) 0.0239(5) Uani 1 1 d . . . . .
N3 N 0.7135(3) 0.94500(18) 0.71623(15) 0.0261(5) Uani 1 1 d . . . . .
O2 O 0.6233(2) 1.13157(15) 0.84290(13) 0.0325(5) Uani 1 1 d . . . . .
O1 O 0.4503(2) 1.11170(15) 0.93872(13) 0.0313(5) Uani 1 1 d . . . . .
O3 O 0.3497(2) 0.85634(15) 0.67325(13) 0.0342(5) Uani 1 1 d . . . . .
O4 O 0.5088(2) 0.78877(15) 0.75135(13) 0.0324(5) Uani 1 1 d . . . . .
O5 O 0.2941(2) 0.89530(16) 0.87650(14) 0.0345(5) Uani 1 1 d . . . . .
O6 O 0.1566(2) 0.91674(17) 0.99730(14) 0.0407(6) Uani 1 1 d . . . . .
OW1 O 0.6448(3) 0.93806(18) 0.91170(14) 0.0299(5) Uani 1 1 d . . . . .
Y1 Y 0.47343(3) 0.97025(2) 0.80578(2) 0.02117(7) Uani 1 1 d . . . . .
I2 I 0.20330(3) 0.33876(2) 0.45505(2) 0.04721(8) Uani 1 1 d . . . . .
I3 I -0.20459(3) 0.45669(2) 0.74292(2) 0.05497(8) Uani 1 1 d . . . . .
I1 I 0.74624(4) 1.61059(2) 1.14305(2) 0.07934(11) Uani 1 1 d . . . . .
HW1A H 0.605(4) 0.913(3) 0.948(2) 0.041(11) Uiso 1 1 d . . . . .
HW1B H 0.712(4) 0.980(3) 0.941(2) 0.052(12) Uiso 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
C34 C33 1.373(5) . ?
C34 C35 1.378(5) . ?
C34 I3 2.102(3) . ?
C20 C19 1.365(5) . ?
C20 C21 1.374(5) . ?
C20 I1 2.096(3) . ?
C27 C26 1.373(4) . ?
C27 C28 1.385(4) . ?
C27 I2 2.100(3) . ?
C35 C36 1.383(5) . ?
C35 H35 0.9300 . ?
C26 C25 1.387(4) . ?
C26 H26 0.9300 . ?
C1 N1 1.345(4) . ?
C1 C2 1.381(4) . ?
C1 H1 0.9300 . ?
C18 C17 1.383(4) . ?
C18 C19 1.385(5) . ?
C18 H18 0.9300 . ?
C24 C29 1.389(4) . ?
C24 C25 1.389(4) . ?
C24 C23 1.498(4) . ?
C28 C29 1.386(4) . ?
C28 H28 0.9300 . ?
C21 C22 1.378(4) . ?
C21 H21 0.9300 . ?
C2 C3 1.370(5) . ?
C2 H2 0.9300 . ?
C5 N1 1.345(4) . ?
C5 C4 1.395(4) . ?
C5 C6 1.485(4) . ?
C14 C13 1.366(5) . ?
C14 C15 1.386(4) . ?
C14 H14 0.9300 . ?
C17 C22 1.374(4) . ?
C17 C16 1.491(4) . ?
C15 N3 1.337(4) . ?
C15 H15 0.9300 . ?
C31 C32 1.374(4) . ?
C31 C36 1.380(4) . ?
C31 C30 1.506(4) . ?
C25 H25 0.9300 . ?
C11 N3 1.341(4) . ?
C11 C12 1.388(4) . ?
C11 C10 1.491(4) . ?
C19 H19 0.9300 . ?
C30 O6 1.239(4) . ?
C30 O5 1.273(3) . ?
C33 C32 1.383(4) . ?
C33 H33 0.9300 . ?
C16 O2 1.260(3) . ?
C16 O1 1.271(3) . ?
C16 Y1 2.825(3) . ?
C3 C4 1.385(5) . ?
C3 H3 0.9300 . ?
C23 O4 1.254(3) . ?
C23 O3 1.269(4) . ?
C23 Y1 2.798(3) . ?
C36 H36 0.9300 . ?
C29 H29 0.9300 . ?
C6 N2 1.349(4) . ?
C6 C7 1.386(4) . ?
C32 H32 0.9300 . ?
C13 C12 1.375(5) . ?
C13 H13 0.9300 . ?
C10 N2 1.341(4) . ?
C10 C9 1.385(4) . ?
C4 H4 0.9300 . ?
C7 C8 1.361(5) . ?
C7 H7 0.9300 . ?
C9 C8 1.368(5) . ?
C9 H9 0.9300 . ?
C12 H12 0.9300 . ?
C8 H8 0.9300 . ?
C22 H22 0.9300 . ?
N1 Y1 2.523(2) . ?
N2 Y1 2.581(2) . ?
N3 Y1 2.547(2) . ?
O2 Y1 2.4228(19) . ?
O1 Y1 2.488(2) . ?
O3 Y1 2.449(2) . ?
O4 Y1 2.450(2) . ?
O5 Y1 2.2618(19) . ?
OW1 Y1 2.337(2) . ?
OW1 HW1A 0.80(4) . ?
OW1 HW1B 0.84(4) . ?

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
C33 C34 C35 120.4(3) . . ?
C33 C34 I3 119.8(3) . . ?
C35 C34 I3 119.8(2) . . ?
C19 C20 C21 120.7(3) . . ?
C19 C20 I1 119.3(3) . . ?
C21 C20 I1 120.0(3) . . ?
C26 C27 C28 121.4(3) . . ?
C26 C27 I2 118.5(2) . . ?
C28 C27 I2 120.2(2) . . ?
C34 C35 C36 119.6(3) . . ?
C34 C35 H35 120.2 . . ?
C36 C35 H35 120.2 . . ?
C27 C26 C25 119.2(3) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
N1 C1 C2 123.2(3) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C17 C18 C19 120.8(3) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C29 C24 C25 118.7(3) . . ?
C29 C24 C23 120.4(3) . . ?
C25 C24 C23 120.8(3) . . ?
C27 C28 C29 118.8(3) . . ?
C27 C28 H28 120.6 . . ?
C29 C28 H28 120.6 . . ?
C20 C21 C22 119.5(3) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C3 C2 C1 119.0(3) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
N1 C5 C4 121.5(3) . . ?
N1 C5 C6 116.5(3) . . ?
C4 C5 C6 121.9(3) . . ?
C13 C14 C15 118.2(3) . . ?
C13 C14 H14 120.9 . . ?
C15 C14 H14 120.9 . . ?
C22 C17 C18 118.6(3) . . ?
C22 C17 C16 121.2(3) . . ?
C18 C17 C16 120.2(3) . . ?
N3 C15 C14 123.1(3) . . ?
N3 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C32 C31 C36 118.3(3) . . ?
C32 C31 C30 120.4(3) . . ?
C36 C31 C30 121.3(3) . . ?
C26 C25 C24 120.9(3) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
N3 C11 C12 121.2(3) . . ?
N3 C11 C10 116.5(3) . . ?
C12 C11 C10 122.3(3) . . ?
C20 C19 C18 119.4(3) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
O6 C30 O5 124.4(3) . . ?
O6 C30 C31 118.6(3) . . ?
O5 C30 C31 117.0(3) . . ?
C34 C33 C32 119.0(3) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
O2 C16 O1 120.4(3) . . ?
O2 C16 C17 120.1(3) . . ?
O1 C16 C17 119.5(3) . . ?
O2 C16 Y1 58.71(14) . . ?
O1 C16 Y1 61.68(15) . . ?
C17 C16 Y1 178.5(2) . . ?
C2 C3 C4 118.7(3) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
O4 C23 O3 121.9(3) . . ?
O4 C23 C24 119.0(3) . . ?
O3 C23 C24 119.1(3) . . ?
O4 C23 Y1 61.01(15) . . ?
O3 C23 Y1 61.00(15) . . ?
C24 C23 Y1 173.9(2) . . ?
C31 C36 C35 120.8(3) . . ?
C31 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
C28 C29 C24 121.0(3) . . ?
C28 C29 H29 119.5 . . ?
C24 C29 H29 119.5 . . ?
N2 C6 C7 121.1(3) . . ?
N2 C6 C5 117.0(3) . . ?
C7 C6 C5 121.9(3) . . ?
C31 C32 C33 121.7(3) . . ?
C31 C32 H32 119.1 . . ?
C33 C32 H32 119.1 . . ?
C14 C13 C12 119.3(3) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
N2 C10 C9 121.7(3) . . ?
N2 C10 C11 116.6(3) . . ?
C9 C10 C11 121.7(3) . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C8 C7 C6 119.7(3) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C8 C9 C10 119.2(3) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C13 C12 C11 119.7(3) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C7 C8 C9 119.4(3) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C17 C22 C21 121.1(3) . . ?
C17 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C1 N1 C5 118.0(3) . . ?
C1 N1 Y1 119.63(19) . . ?
C5 N1 Y1 122.39(19) . . ?
C10 N2 C6 118.9(2) . . ?
C10 N2 Y1 120.91(19) . . ?
C6 N2 Y1 119.89(18) . . ?
C15 N3 C11 118.4(3) . . ?
C15 N3 Y1 119.32(19) . . ?
C11 N3 Y1 122.29(19) . . ?
C16 O2 Y1 94.91(17) . . ?
C16 O1 Y1 91.59(17) . . ?
C23 O3 Y1 92.05(17) . . ?
C23 O4 Y1 92.40(18) . . ?
C30 O5 Y1 170.6(2) . . ?
Y1 OW1 HW1A 114(3) . . ?
Y1 OW1 HW1B 125(3) . . ?
HW1A OW1 HW1B 104(3) . . ?
O5 Y1 OW1 85.10(8) . . ?
O5 Y1 O2 133.97(7) . . ?
OW1 Y1 O2 80.32(8) . . ?
O5 Y1 O3 83.05(7) . . ?
OW1 Y1 O3 130.67(8) . . ?
O2 Y1 O3 137.65(7) . . ?
O5 Y1 O4 76.85(7) . . ?
OW1 Y1 O4 77.19(7) . . ?
O2 Y1 O4 139.60(7) . . ?
O3 Y1 O4 53.49(7) . . ?
O5 Y1 O1 81.01(7) . . ?
OW1 Y1 O1 75.34(7) . . ?
O2 Y1 O1 53.11(7) . . ?
O3 Y1 O1 147.93(7) . . ?
O4 Y1 O1 145.88(7) . . ?
O5 Y1 N1 81.43(8) . . ?
OW1 Y1 N1 144.75(8) . . ?
O2 Y1 N1 85.94(7) . . ?
O3 Y1 N1 79.78(7) . . ?
O4 Y1 N1 130.05(7) . . ?
O1 Y1 N1 70.47(7) . . ?
O5 Y1 N3 145.32(8) . . ?
OW1 Y1 N3 79.46(8) . . ?
O2 Y1 N3 73.65(7) . . ?
O3 Y1 N3 83.85(7) . . ?
O4 Y1 N3 69.56(7) . . ?
O1 Y1 N3 123.71(7) . . ?
N1 Y1 N3 127.28(8) . . ?
O5 Y1 N2 138.85(7) . . ?
OW1 Y1 N2 136.04(8) . . ?
O2 Y1 N2 67.77(7) . . ?
O3 Y1 N2 70.12(7) . . ?
O4 Y1 N2 108.23(7) . . ?
O1 Y1 N2 105.55(7) . . ?
N1 Y1 N2 63.90(7) . . ?
N3 Y1 N2 63.39(7) . . ?
O5 Y1 C23 77.67(8) . . ?
OW1 Y1 C23 103.73(9) . . ?
O2 Y1 C23 148.24(8) . . ?
O3 Y1 C23 26.94(8) . . ?
O4 Y1 C23 26.59(8) . . ?
O1 Y1 C23 158.65(7) . . ?
N1 Y1 C23 104.94(8) . . ?
N3 Y1 C23 76.17(8) . . ?
N2 Y1 C23 89.99(8) . . ?
O5 Y1 C16 107.69(8) . . ?
OW1 Y1 C16 76.53(8) . . ?
O2 Y1 C16 26.38(7) . . ?
O3 Y1 C16 152.30(8) . . ?
O4 Y1 C16 152.79(8) . . ?
O1 Y1 C16 26.73(7) . . ?
N1 Y1 C16 76.84(8) . . ?
N3 Y1 C16 98.67(8) . . ?
N2 Y1 C16 86.25(8) . . ?
C23 Y1 C16 174.61(8) . . ?

_refine_diff_density_max         0.684
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.076

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?


#===END






####################################################################### 
# 
# 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_Complex_6
_database_code_depnum_ccdc_archive 'CCDC 1514984'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 Eu2 I6 N6 O14'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2288.50

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 '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                   11.1901(6)
_cell_length_b                   12.8834(6)
_cell_length_c                   14.5070(7)
_cell_angle_alpha                69.119(2)
_cell_angle_beta                 88.6990(10)
_cell_angle_gamma                72.8400(10)
_cell_volume                     1859.10(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25187
_cell_measurement_theta_min      4.350
_cell_measurement_theta_max      56.140

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.044
_exptl_crystal_F_000             1080
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.496
_exptl_crystal_size_mid          0.362
_exptl_crystal_size_min          0.272
_exptl_absorpt_coefficient_mu    4.228
_shelx_estimated_absorpt_T_min   0.228
_shelx_estimated_absorpt_T_max   0.393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6337
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25156
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.509
_diffrn_reflns_theta_max         28.115
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9002
_reflns_number_gt                8072
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0520P)²+3.4621P] 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         9002
_refine_ls_number_parameters     469
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0984
_refine_ls_wR_factor_gt          0.0939
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
C15 C -0.0934(4) 0.7655(4) -0.1300(4) 0.0503(10) Uani 1 1 d . . . . .
H15 H -0.1284 0.8386 -0.1258 0.060 Uiso 1 1 calc R U . . .
C14 C -0.1627(4) 0.7289(4) -0.1824(4) 0.0527(10) Uani 1 1 d . . . . .
H14 H -0.2424 0.7760 -0.2126 0.063 Uiso 1 1 calc R U . . .
C13 C -0.1111(5) 0.6207(4) -0.1889(3) 0.0548(11) Uani 1 1 d . . . . .
H13 H -0.1550 0.5933 -0.2239 0.066 Uiso 1 1 calc R U . . .
C12 C 0.0062(5) 0.5547(4) -0.1429(3) 0.0512(10) Uani 1 1 d . . . . .
H12 H 0.0422 0.4813 -0.1461 0.061 Uiso 1 1 calc R U . . .
C11 C 0.0722(4) 0.5960(3) -0.0917(3) 0.0391(8) Uani 1 1 d . . . . .
C10 C 0.1963(4) 0.5250(3) -0.0382(3) 0.0416(8) Uani 1 1 d . . . . .
C9 C 0.2583(5) 0.4155(4) -0.0425(4) 0.0557(11) Uani 1 1 d . . . . .
H9 H 0.2233 0.3869 -0.0821 0.067 Uiso 1 1 calc R U . . .
C8 C 0.3731(6) 0.3499(4) 0.0131(4) 0.0703(15) Uani 1 1 d . . . . .
H8 H 0.4165 0.2777 0.0100 0.084 Uiso 1 1 calc R U . . .
C7 C 0.4214(5) 0.3925(4) 0.0721(4) 0.0569(11) Uani 1 1 d . . . . .
H7 H 0.4974 0.3491 0.1105 0.068 Uiso 1 1 calc R U . . .
C6 C 0.3557(4) 0.5019(3) 0.0744(3) 0.0447(9) Uani 1 1 d . . . . .
C5 C 0.4068(4) 0.5528(4) 0.1345(3) 0.0500(10) Uani 1 1 d . . . . .
C4 C 0.5069(5) 0.4859(5) 0.2080(5) 0.0765(16) Uani 1 1 d . . . . .
H4 H 0.5416 0.4062 0.2223 0.092 Uiso 1 1 calc R U . . .
C3 C 0.5535(6) 0.5407(7) 0.2594(5) 0.092(2) Uani 1 1 d . . . . .
H3 H 0.6181 0.4976 0.3099 0.111 Uiso 1 1 calc R U . . .
C2 C 0.5038(6) 0.6574(7) 0.2351(5) 0.087(2) Uani 1 1 d . . . . .
H2 H 0.5367 0.6963 0.2661 0.105 Uiso 1 1 calc R U . . .
C1 C 0.4034(5) 0.7177(5) 0.1633(4) 0.0647(13) Uani 1 1 d . . . . .
H1 H 0.3682 0.7975 0.1483 0.078 Uiso 1 1 calc R U . . .
C16 C 0.3121(4) 0.8580(3) -0.1273(3) 0.0408(8) Uani 1 1 d . . . . .
C17 C 0.4006(4) 0.9017(3) -0.1980(3) 0.0413(8) Uani 1 1 d . . . . .
C18 C 0.4777(4) 0.9575(4) -0.1734(3) 0.0494(9) Uani 1 1 d . . . . .
H18 H 0.4712 0.9700 -0.1140 0.059 Uiso 1 1 calc R U . . .
C19 C 0.5638(4) 0.9945(4) -0.2369(4) 0.0554(11) Uani 1 1 d . . . . .
H19 H 0.6153 1.0312 -0.2201 0.067 Uiso 1 1 calc R U . . .
C20 C 0.5722(4) 0.9762(4) -0.3246(4) 0.0540(10) Uani 1 1 d . . . . .
C21 C 0.4974(5) 0.9205(5) -0.3506(4) 0.0584(11) Uani 1 1 d . . . . .
H21 H 0.5047 0.9080 -0.4100 0.070 Uiso 1 1 calc R U . . .
C22 C 0.4116(4) 0.8837(4) -0.2867(3) 0.0502(9) Uani 1 1 d . . . . .
H22 H 0.3609 0.8464 -0.3036 0.060 Uiso 1 1 calc R U . . .
C23 C -0.0157(4) 0.7102(3) 0.1631(3) 0.0408(8) Uani 1 1 d . . . . .
C24 C -0.0906(4) 0.6919(3) 0.2508(3) 0.0412(8) Uani 1 1 d . . . . .
C25 C -0.1932(4) 0.7814(4) 0.2561(4) 0.0523(10) Uani 1 1 d . . . . .
H25 H -0.2165 0.8531 0.2038 0.063 Uiso 1 1 calc R U . . .
C26 C -0.2608(5) 0.7656(5) 0.3378(4) 0.0624(12) Uani 1 1 d . . . . .
H26 H -0.3280 0.8267 0.3412 0.075 Uiso 1 1 calc R U . . .
C27 C -0.2280(5) 0.6584(5) 0.4144(4) 0.0611(12) Uani 1 1 d . . . . .
C28 C -0.1266(6) 0.5670(5) 0.4108(4) 0.0652(13) Uani 1 1 d . . . . .
H28 H -0.1052 0.4948 0.4625 0.078 Uiso 1 1 calc R U . . .
C29 C -0.0578(5) 0.5850(4) 0.3292(4) 0.0555(11) Uani 1 1 d . . . . .
H29 H 0.0112 0.5247 0.3268 0.067 Uiso 1 1 calc R U . . .
C30 C -0.0596(3) 1.0517(3) -0.1533(3) 0.0340(7) Uani 1 1 d . . . . .
C31 C -0.0642(3) 1.1037(3) -0.2645(3) 0.0360(7) Uani 1 1 d . . . . .
C32 C 0.0144(4) 1.0431(4) -0.3155(3) 0.0451(9) Uani 1 1 d . . . . .
H32 H 0.0726 0.9710 -0.2807 0.054 Uiso 1 1 calc R U . . .
C33 C 0.0072(5) 1.0890(4) -0.4183(3) 0.0538(10) Uani 1 1 d . . . . .
H33 H 0.0609 1.0486 -0.4525 0.065 Uiso 1 1 calc R U . . .
C34 C -0.0805(5) 1.1954(4) -0.4689(3) 0.0532(10) Uani 1 1 d . . . . .
C35 C -0.1563(5) 1.2589(4) -0.4194(3) 0.0553(11) Uani 1 1 d . . . . .
H35 H -0.2123 1.3322 -0.4542 0.066 Uiso 1 1 calc R U . . .
C36 C -0.1482(4) 1.2126(3) -0.3174(3) 0.0476(9) Uani 1 1 d . . . . .
H36 H -0.1998 1.2549 -0.2835 0.057 Uiso 1 1 calc R U . . .
N3 N 0.0212(3) 0.7019(3) -0.0851(3) 0.0412(7) Uani 1 1 d . . . . .
N2 N 0.2458(3) 0.5679(3) 0.0190(2) 0.0380(6) Uani 1 1 d . . . . .
N1 N 0.3547(3) 0.6671(3) 0.1146(3) 0.0479(8) Uani 1 1 d . . . . .
O1 O 0.2905(3) 0.8926(3) -0.0555(2) 0.0524(7) Uani 1 1 d . . . . .
O2 O 0.2639(3) 0.7862(2) -0.1382(2) 0.0438(6) Uani 1 1 d . . . . .
O3 O -0.0645(3) 0.7918(3) 0.0821(2) 0.0527(7) Uani 1 1 d . . . . .
O4 O 0.0964(3) 0.6462(2) 0.1711(2) 0.0459(6) Uani 1 1 d . . . . .
O6 O 0.0138(3) 0.9517(2) -0.1107(2) 0.0473(7) Uani 1 1 d . . . . .
O5 O 0.1328(3) 0.8883(2) 0.1110(2) 0.0436(6) Uani 1 1 d . . . . .
OW1 O -0.3127(5) 0.9211(5) -0.0054(4) 0.0915(15) Uani 1 1 d D . . . .
I1 I 0.70566(4) 1.02825(6) -0.41768(3) 0.09812(18) Uani 1 1 d . . . . .
I2 I -0.33138(6) 0.63063(6) 0.53846(4) 0.1142(2) Uani 1 1 d . . . . .
I3A I -0.1168(3) 1.2545(4) -0.6277(2) 0.0698(8) Uani 0.56(3) 1 d . . P A 1
I3B I -0.081(2) 1.2620(4) -0.6187(5) 0.101(2) Uani 0.44(3) 1 d . . P A 2
Eu1 Eu 0.14043(2) 0.78226(2) 0.00925(2) 0.03343(6) Uani 1 1 d . . . . .
HW1B H -0.243(3) 0.879(6) 0.021(5) 0.10(3) Uiso 1 1 d D . . . .
HW1A H -0.320(7) 0.984(3) -0.001(6) 0.10(3) Uiso 1 1 d 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
C15 N3 1.334(5) . ?
C15 C14 1.378(6) . ?
C15 H15 0.9300 . ?
C14 C13 1.379(7) . ?
C14 H14 0.9300 . ?
C13 C12 1.367(7) . ?
C13 H13 0.9300 . ?
C12 C11 1.384(6) . ?
C12 H12 0.9300 . ?
C11 N3 1.353(5) . ?
C11 C10 1.470(6) . ?
C10 N2 1.353(5) . ?
C10 C9 1.400(5) . ?
C9 C8 1.391(8) . ?
C9 H9 0.9300 . ?
C8 C7 1.363(8) . ?
C8 H8 0.9300 . ?
C7 C6 1.396(6) . ?
C7 H7 0.9300 . ?
C6 N2 1.350(5) . ?
C6 C5 1.472(7) . ?
C5 N1 1.339(6) . ?
C5 C4 1.402(7) . ?
C4 C3 1.391(9) . ?
C4 H4 0.9300 . ?
C3 C2 1.353(10) . ?
C3 H3 0.9300 . ?
C2 C1 1.382(8) . ?
C2 H2 0.9300 . ?
C1 N1 1.333(6) . ?
C1 H1 0.9300 . ?
C16 O2 1.254(5) . ?
C16 O1 1.264(5) . ?
C16 C17 1.491(6) . ?
C16 Eu1 2.849(4) . ?
C17 C22 1.383(6) . ?
C17 C18 1.397(6) . ?
C18 C19 1.385(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.370(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.385(7) . ?
C20 I1 2.088(5) . ?
C21 C22 1.386(6) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O3 1.262(5) . ?
C23 O4 1.263(5) . ?
C23 C24 1.493(5) . ?
C23 Eu1 2.864(4) . ?
C24 C29 1.389(6) . ?
C24 C25 1.390(6) . ?
C25 C26 1.376(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.380(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.388(8) . ?
C27 I2 2.096(5) . ?
C28 C29 1.385(7) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 O6 1.243(4) . ?
C30 O5 1.260(4) 2_575 ?
C30 C31 1.506(5) . ?
C31 C32 1.381(5) . ?
C31 C36 1.388(5) . ?
C32 C33 1.389(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.380(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.374(6) . ?
C34 I3B 2.031(7) . ?
C34 I3A 2.159(5) . ?
C35 C36 1.377(6) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N3 Eu1 2.575(3) . ?
N2 Eu1 2.616(3) . ?
N1 Eu1 2.595(3) . ?
O1 Eu1 2.471(3) . ?
O2 Eu1 2.514(3) . ?
O3 Eu1 2.491(3) . ?
O4 Eu1 2.520(3) . ?
O6 Eu1 2.320(3) . ?
O5 C30 1.260(4) 2_575 ?
O5 Eu1 2.327(3) . ?
OW1 HW1B 0.819(10) . ?
OW1 HW1A 0.819(10) . ?

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
N3 C15 C14 123.5(4) . . ?
N3 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
C15 C14 C13 118.4(4) . . ?
C15 C14 H14 120.8 . . ?
C13 C14 H14 120.8 . . ?
C12 C13 C14 118.5(4) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C13 C12 C11 120.8(4) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
N3 C11 C12 120.7(4) . . ?
N3 C11 C10 117.4(3) . . ?
C12 C11 C10 121.9(4) . . ?
N2 C10 C9 121.3(4) . . ?
N2 C10 C11 117.0(3) . . ?
C9 C10 C11 121.7(4) . . ?
C8 C9 C10 119.1(5) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C7 C8 C9 119.4(4) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C8 C7 C6 119.3(4) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
N2 C6 C7 122.0(4) . . ?
N2 C6 C5 116.9(3) . . ?
C7 C6 C5 121.0(4) . . ?
N1 C5 C4 121.0(5) . . ?
N1 C5 C6 116.9(4) . . ?
C4 C5 C6 122.0(4) . . ?
C3 C4 C5 118.9(6) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C2 C3 C4 119.3(5) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C3 C2 C1 118.7(6) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
N1 C1 C2 123.3(5) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
O2 C16 O1 121.7(4) . . ?
O2 C16 C17 120.1(4) . . ?
O1 C16 C17 118.2(4) . . ?
O2 C16 Eu1 61.8(2) . . ?
O1 C16 Eu1 59.9(2) . . ?
C17 C16 Eu1 177.9(3) . . ?
C22 C17 C18 119.0(4) . . ?
C22 C17 C16 120.9(4) . . ?
C18 C17 C16 120.1(4) . . ?
C19 C18 C17 120.6(4) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C20 C19 C18 119.3(4) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
C19 C20 C21 121.4(4) . . ?
C19 C20 I1 118.8(3) . . ?
C21 C20 I1 119.7(4) . . ?
C20 C21 C22 119.0(4) . . ?
C20 C21 H21 120.5 . . ?
C22 C21 H21 120.5 . . ?
C17 C22 C21 120.8(4) . . ?
C17 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
O3 C23 O4 120.6(4) . . ?
O3 C23 C24 119.4(4) . . ?
O4 C23 C24 120.0(4) . . ?
O3 C23 Eu1 60.3(2) . . ?
O4 C23 Eu1 61.6(2) . . ?
C24 C23 Eu1 167.4(3) . . ?
C29 C24 C25 118.8(4) . . ?
C29 C24 C23 120.3(4) . . ?
C25 C24 C23 120.9(4) . . ?
C26 C25 C24 121.0(4) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C25 C26 C27 119.5(4) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
C26 C27 C28 120.8(4) . . ?
C26 C27 I2 120.4(4) . . ?
C28 C27 I2 118.9(4) . . ?
C29 C28 C27 119.1(5) . . ?
C29 C28 H28 120.5 . . ?
C27 C28 H28 120.5 . . ?
C28 C29 C24 120.8(4) . . ?
C28 C29 H29 119.6 . . ?
C24 C29 H29 119.6 . . ?
O6 C30 O5 125.2(3) . 2_575 ?
O6 C30 C31 117.4(3) . . ?
O5 C30 C31 117.3(3) 2_575 . ?
C32 C31 C36 118.9(4) . . ?
C32 C31 C30 120.4(3) . . ?
C36 C31 C30 120.7(3) . . ?
C31 C32 C33 120.5(4) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
C34 C33 C32 119.1(4) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C35 C34 C33 121.1(4) . . ?
C35 C34 I3B 121.1(4) . . ?
C33 C34 I3B 117.4(4) . . ?
C35 C34 I3A 118.5(4) . . ?
C33 C34 I3A 119.9(3) . . ?
C34 C35 C36 119.1(4) . . ?
C34 C35 H35 120.4 . . ?
C36 C35 H35 120.4 . . ?
C35 C36 C31 121.1(4) . . ?
C35 C36 H36 119.5 . . ?
C31 C36 H36 119.5 . . ?
C15 N3 C11 118.1(4) . . ?
C15 N3 Eu1 120.1(3) . . ?
C11 N3 Eu1 121.8(3) . . ?
C6 N2 C10 118.8(3) . . ?
C6 N2 Eu1 120.8(3) . . ?
C10 N2 Eu1 120.2(2) . . ?
C1 N1 C5 118.6(4) . . ?
C1 N1 Eu1 119.1(3) . . ?
C5 N1 Eu1 121.4(3) . . ?
C16 O1 Eu1 93.8(2) . . ?
C16 O2 Eu1 92.1(2) . . ?
C23 O3 Eu1 93.6(2) . . ?
C23 O4 Eu1 92.3(2) . . ?
C30 O6 Eu1 162.8(3) . . ?
C30 O5 Eu1 143.6(3) 2_575 . ?
HW1B OW1 HW1A 106(8) . . ?
O6 Eu1 O5 88.25(10) . . ?
O6 Eu1 O1 77.95(11) . . ?
O5 Eu1 O1 75.90(10) . . ?
O6 Eu1 O3 80.52(11) . . ?
O5 Eu1 O3 75.03(11) . . ?
O1 Eu1 O3 144.09(11) . . ?
O6 Eu1 O2 79.50(10) . . ?
O5 Eu1 O2 128.18(10) . . ?
O1 Eu1 O2 52.34(9) . . ?
O3 Eu1 O2 148.48(10) . . ?
O6 Eu1 O4 132.39(10) . . ?
O5 Eu1 O4 78.60(10) . . ?
O1 Eu1 O4 139.31(10) . . ?
O3 Eu1 O4 51.91(10) . . ?
O2 Eu1 O4 142.68(9) . . ?
O6 Eu1 N3 77.83(10) . . ?
O5 Eu1 N3 148.07(10) . . ?
O1 Eu1 N3 127.42(10) . . ?
O3 Eu1 N3 74.41(11) . . ?
O2 Eu1 N3 77.71(10) . . ?
O4 Eu1 N3 89.73(10) . . ?
O6 Eu1 N1 149.09(12) . . ?
O5 Eu1 N1 79.79(10) . . ?
O1 Eu1 N1 71.54(12) . . ?
O3 Eu1 N1 122.63(11) . . ?
O2 Eu1 N1 85.70(11) . . ?
O4 Eu1 N1 73.13(11) . . ?
N3 Eu1 N1 125.32(11) . . ?
O6 Eu1 N2 134.58(10) . . ?
O5 Eu1 N2 137.16(10) . . ?
O1 Eu1 N2 107.78(10) . . ?
O3 Eu1 N2 107.83(10) . . ?
O2 Eu1 N2 71.06(9) . . ?
O4 Eu1 N2 71.93(9) . . ?
N3 Eu1 N2 62.86(10) . . ?
N1 Eu1 N2 62.46(11) . . ?
O6 Eu1 C16 76.65(11) . . ?
O5 Eu1 C16 102.08(11) . . ?
O1 Eu1 C16 26.26(11) . . ?
O3 Eu1 C16 157.08(10) . . ?
O2 Eu1 C16 26.10(10) . . ?
O4 Eu1 C16 150.72(10) . . ?
N3 Eu1 C16 102.40(11) . . ?
N1 Eu1 C16 78.16(12) . . ?
N2 Eu1 C16 89.87(10) . . ?
O6 Eu1 C23 106.29(11) . . ?
O5 Eu1 C23 72.26(11) . . ?
O1 Eu1 C23 147.66(10) . . ?
O3 Eu1 C23 26.10(10) . . ?
O2 Eu1 C23 159.41(10) . . ?
O4 Eu1 C23 26.15(10) . . ?
N3 Eu1 C23 84.16(11) . . ?
N1 Eu1 C23 97.08(12) . . ?
N2 Eu1 C23 92.06(10) . . ?
C16 Eu1 C23 173.32(11) . . ?

_refine_diff_density_max         1.750
_refine_diff_density_min         -2.329
_refine_diff_density_rms         0.111

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_9
_database_code_depnum_ccdc_archive 'CCDC 1514987'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_Complex_9           
;
PROBLEM: Check Calcd Residual Density  0.67A From      I2      -2.83 eA-3
RESPONSE: I2 was slightly disordered and attempts to model via PART command did not improve refinement.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H50 Dy2 I6 N6 O14'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         2309.58

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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                   11.1784(4)
_cell_length_b                   12.8338(5)
_cell_length_c                   14.4641(6)
_cell_angle_alpha                68.995(2)
_cell_angle_beta                 88.5430(10)
_cell_angle_gamma                72.7220(10)
_cell_volume                     1842.08(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    27271
_cell_measurement_theta_min      4.664
_cell_measurement_theta_max      57.375

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_F_000             1086
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.338
_exptl_crystal_size_min          0.138
_exptl_absorpt_coefficient_mu    4.593
_shelx_estimated_absorpt_T_min   0.244
_shelx_estimated_absorpt_T_max   0.570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4904
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focused sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27266
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.514
_diffrn_reflns_theta_max         29.733
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10158
_reflns_number_gt                8510
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'Superflip (Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0599P)²+4.2340P] 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         10158
_refine_ls_number_parameters     469
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_ref         0.1182
_refine_ls_wR_factor_gt          0.1105
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
Dy1 Dy 0.63988(2) 0.28232(2) 0.00907(2) 0.03094(7) Uani 1 1 d . . . . .
I3A I 0.3811(4) 0.7560(5) -0.6272(2) 0.0695(7) Uani 0.65(3) 1 d . . P A 1
I3B I 0.420(3) 0.7616(6) -0.6180(8) 0.090(3) Uani 0.35(3) 1 d . . P A 2
I1 I 0.16952(7) 0.12960(7) 0.53896(5) 0.1100(2) Uani 1 1 d . . . . .
I2 I 1.20560(6) 0.52742(7) -0.41720(4) 0.1010(2) Uani 1 1 d . . . . .
O5 O 0.5158(3) 0.4505(3) -0.1089(3) 0.0436(8) Uani 1 1 d . . . . .
O6 O 0.6297(3) 0.3883(3) 0.1087(2) 0.0415(7) Uani 1 1 d . . . . .
O2 O 0.5973(3) 0.1466(3) 0.1695(3) 0.0423(8) Uani 1 1 d . . . . .
O1 O 0.4363(3) 0.2923(4) 0.0804(3) 0.0509(9) Uani 1 1 d . . . . .
O4 O 0.7614(3) 0.2849(3) -0.1371(3) 0.0416(7) Uani 1 1 d . . . . .
N2 N 0.7459(4) 0.0701(3) 0.0197(3) 0.0367(8) Uani 1 1 d . . . . .
O3 O 0.7866(4) 0.3937(3) -0.0561(3) 0.0499(9) Uani 1 1 d . . . . .
N3 N 0.8511(4) 0.1718(4) 0.1138(4) 0.0468(10) Uani 1 1 d . . . . .
N1 N 0.5221(4) 0.2044(3) -0.0847(3) 0.0388(8) Uani 1 1 d . . . . .
C30 C 0.4420(4) 0.5514(3) -0.1516(3) 0.0316(8) Uani 1 1 d . . . . .
C18 C 0.3079(5) 0.2818(5) 0.2550(4) 0.0495(12) Uani 1 1 d . . . . .
H18 H 0.2850 0.3542 0.2027 0.059 Uiso 1 1 calc R U . . .
C16 C 0.4853(5) 0.2104(4) 0.1615(4) 0.0393(10) Uani 1 1 d . . . . .
C17 C 0.4106(4) 0.1913(4) 0.2499(4) 0.0386(10) Uani 1 1 d . . . . .
C3 C 0.3906(6) 0.1224(6) -0.1889(4) 0.0540(13) Uani 1 1 d . . . . .
H3 H 0.3473 0.0952 -0.2247 0.065 Uiso 1 1 calc R U . . .
C10 C 0.8551(5) 0.0048(4) 0.0755(4) 0.0423(11) Uani 1 1 d . . . . .
C23 C 0.8096(4) 0.3577(4) -0.1272(4) 0.0383(10) Uani 1 1 d . . . . .
C7 C 0.7604(6) -0.0840(5) -0.0405(5) 0.0570(15) Uani 1 1 d . . . . .
H7 H 0.7261 -0.1127 -0.0805 0.068 Uiso 1 1 calc R U . . .
C31 C 0.4356(4) 0.6038(4) -0.2632(3) 0.0333(9) Uani 1 1 d . . . . .
C34 C 0.4168(6) 0.6955(5) -0.4687(4) 0.0510(13) Uani 1 1 d . . . . .
C5 C 0.5726(5) 0.0980(4) -0.0912(3) 0.0375(10) Uani 1 1 d . . . . .
C32 C 0.5141(5) 0.5428(4) -0.3146(4) 0.0435(11) Uani 1 1 d . . . . .
H32 H 0.5730 0.4706 -0.2797 0.052 Uiso 1 1 calc R U . . .
C6 C 0.6969(5) 0.0265(4) -0.0374(4) 0.0401(10) Uani 1 1 d . . . . .
C27 C 1.0709(5) 0.4750(5) -0.3240(5) 0.0537(13) Uani 1 1 d . . . . .
C20 C 0.2731(6) 0.1574(6) 0.4141(5) 0.0582(14) Uani 1 1 d . . . . .
C36 C 0.3522(5) 0.7125(4) -0.3155(4) 0.0450(11) Uani 1 1 d . . . . .
H36 H 0.3022 0.7556 -0.2811 0.054 Uiso 1 1 calc R U . . .
C11 C 0.9053(5) 0.0568(5) 0.1351(4) 0.0476(12) Uani 1 1 d . . . . .
C29 C 0.9099(5) 0.3827(5) -0.2865(4) 0.0519(13) Uani 1 1 d . . . . .
H29 H 0.8598 0.3448 -0.3034 0.062 Uiso 1 1 calc R U . . .
C19 C 0.2397(6) 0.2651(6) 0.3371(5) 0.0609(15) Uani 1 1 d . . . . .
H19 H 0.1717 0.3260 0.3405 0.073 Uiso 1 1 calc R U . . .
C22 C 0.4431(6) 0.0839(5) 0.3279(4) 0.0531(13) Uani 1 1 d . . . . .
H22 H 0.5117 0.0230 0.3251 0.064 Uiso 1 1 calc R U . . .
C2 C 0.3379(5) 0.2305(5) -0.1819(4) 0.0525(13) Uani 1 1 d . . . . .
H2 H 0.2574 0.2769 -0.2114 0.063 Uiso 1 1 calc R U . . .
C21 C 0.3742(7) 0.0662(6) 0.4103(5) 0.0640(16) Uani 1 1 d . . . . .
H21 H 0.3959 -0.0063 0.4624 0.077 Uiso 1 1 calc R U . . .
C14 C 1.0020(7) 0.1655(8) 0.2321(7) 0.086(2) Uani 1 1 d . . . . .
H14 H 1.0365 0.2060 0.2603 0.103 Uiso 1 1 calc R U . . .
C1 C 0.4065(5) 0.2688(5) -0.1304(5) 0.0495(12) Uani 1 1 d . . . . .
H1 H 0.3712 0.3426 -0.1270 0.059 Uiso 1 1 calc R U . . .
C15 C 0.8996(6) 0.2244(6) 0.1611(5) 0.0628(16) Uani 1 1 d . . . . .
H15 H 0.8630 0.3045 0.1456 0.075 Uiso 1 1 calc R U . . .
C12 C 1.0055(6) -0.0087(6) 0.2098(6) 0.076(2) Uani 1 1 d . . . . .
H12 H 1.0407 -0.0890 0.2255 0.091 Uiso 1 1 calc R U . . .
C24 C 0.8986(4) 0.4008(4) -0.1984(4) 0.0396(10) Uani 1 1 d . . . . .
C33 C 0.5057(5) 0.5881(5) -0.4176(4) 0.0511(13) Uani 1 1 d . . . . .
H33 H 0.5589 0.5472 -0.4520 0.061 Uiso 1 1 calc R U . . .
C8 C 0.8725(7) -0.1495(5) 0.0148(5) 0.0668(18) Uani 1 1 d . . . . .
H8 H 0.9154 -0.2226 0.0125 0.080 Uiso 1 1 calc R U . . .
C28 C 0.9955(6) 0.4206(6) -0.3505(5) 0.0623(15) Uani 1 1 d . . . . .
H28 H 1.0021 0.4094 -0.4107 0.075 Uiso 1 1 calc R U . . .
OW1 O 0.1876(6) 0.4220(6) -0.0059(5) 0.0899(18) Uani 1 1 d D . . . .
C25 C 0.9758(5) 0.4567(5) -0.1728(5) 0.0502(12) Uani 1 1 d . . . . .
H25 H 0.9692 0.4687 -0.1129 0.060 Uiso 1 1 calc R U . . .
C26 C 1.0619(6) 0.4940(6) -0.2365(5) 0.0563(14) Uani 1 1 d . . . . .
H26 H 1.1130 0.5314 -0.2200 0.068 Uiso 1 1 calc R U . . .
C35 C 0.3415(6) 0.7588(5) -0.4185(4) 0.0544(14) Uani 1 1 d . . . . .
H35 H 0.2841 0.8319 -0.4531 0.065 Uiso 1 1 calc R U . . .
C4 C 0.5074(6) 0.0559(5) -0.1424(4) 0.0502(13) Uani 1 1 d . . . . .
H4 H 0.5436 -0.0181 -0.1451 0.060 Uiso 1 1 calc R U . . .
C9 C 0.9212(6) -0.1059(5) 0.0741(5) 0.0575(15) Uani 1 1 d . . . . .
H9 H 0.9972 -0.1494 0.1128 0.069 Uiso 1 1 calc R U . . .
C13 C 1.0507(7) 0.0472(8) 0.2594(7) 0.091(3) Uani 1 1 d . . . . .
H13 H 1.1140 0.0044 0.3112 0.109 Uiso 1 1 calc R U . . .
HW1A H 0.235(16) 0.371(12) -0.023(14) 0.30(11) Uiso 1 1 d D . . . .
HW1B H 0.191(9) 0.483(4) -0.002(7) 0.10(3) Uiso 1 1 d 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
Dy1 O5 2.279(3) . ?
Dy1 O6 2.291(3) . ?
Dy1 O3 2.443(4) . ?
Dy1 O1 2.462(4) . ?
Dy1 O4 2.479(3) . ?
Dy1 O2 2.486(3) . ?
Dy1 N1 2.533(4) . ?
Dy1 N3 2.556(4) . ?
Dy1 N2 2.576(3) . ?
Dy1 C23 2.820(5) . ?
Dy1 C16 2.827(5) . ?
I3A C34 2.145(7) . ?
I3B C34 2.022(9) . ?
I1 C20 2.099(6) . ?
I2 C27 2.094(6) . ?
O5 C30 1.248(5) . ?
O6 C30 1.255(5) 2_665 ?
O2 C16 1.258(6) . ?
O1 C16 1.260(6) . ?
O4 C23 1.258(6) . ?
N2 C10 1.343(6) . ?
N2 C6 1.355(6) . ?
O3 C23 1.262(6) . ?
N3 C15 1.336(8) . ?
N3 C11 1.339(7) . ?
N1 C1 1.344(7) . ?
N1 C5 1.350(6) . ?
C30 O6 1.255(5) 2_665 ?
C30 C31 1.504(6) . ?
C18 C19 1.380(8) . ?
C18 C17 1.393(7) . ?
C18 H18 0.9300 . ?
C16 C17 1.494(7) . ?
C17 C22 1.384(7) . ?
C3 C4 1.363(9) . ?
C3 C2 1.377(8) . ?
C3 H3 0.9300 . ?
C10 C9 1.400(7) . ?
C10 C11 1.470(8) . ?
C23 C24 1.491(7) . ?
C7 C8 1.364(10) . ?
C7 C6 1.400(6) . ?
C7 H7 0.9300 . ?
C31 C36 1.376(6) . ?
C31 C32 1.383(6) . ?
C34 C35 1.372(8) . ?
C34 C33 1.388(8) . ?
C5 C4 1.386(7) . ?
C5 C6 1.471(7) . ?
C32 C33 1.386(7) . ?
C32 H32 0.9300 . ?
C27 C26 1.367(9) . ?
C27 C28 1.380(9) . ?
C20 C19 1.379(9) . ?
C20 C21 1.381(9) . ?
C36 C35 1.385(7) . ?
C36 H36 0.9300 . ?
C11 C12 1.407(8) . ?
C29 C24 1.372(8) . ?
C29 C28 1.384(8) . ?
C29 H29 0.9300 . ?
C19 H19 0.9300 . ?
C22 C21 1.389(8) . ?
C22 H22 0.9300 . ?
C2 C1 1.379(8) . ?
C2 H2 0.9300 . ?
C21 H21 0.9300 . ?
C14 C13 1.360(12) . ?
C14 C15 1.388(9) . ?
C14 H14 0.9300 . ?
C1 H1 0.9300 . ?
C15 H15 0.9300 . ?
C12 C13 1.374(12) . ?
C12 H12 0.9300 . ?
C24 C25 1.403(7) . ?
C33 H33 0.9300 . ?
C8 C9 1.378(10) . ?
C8 H8 0.9300 . ?
C28 H28 0.9300 . ?
OW1 HW1A 0.820(10) . ?
OW1 HW1B 0.821(10) . ?
C25 C26 1.384(8) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C35 H35 0.9300 . ?
C4 H4 0.9300 . ?
C9 H9 0.9300 . ?
C13 H13 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
O5 Dy1 O6 87.38(12) . . ?
O5 Dy1 O3 77.15(14) . . ?
O6 Dy1 O3 76.00(13) . . ?
O5 Dy1 O1 80.30(13) . . ?
O6 Dy1 O1 74.81(14) . . ?
O3 Dy1 O1 143.63(13) . . ?
O5 Dy1 O4 79.71(12) . . ?
O6 Dy1 O4 128.91(12) . . ?
O3 Dy1 O4 52.98(12) . . ?
O1 Dy1 O4 147.80(13) . . ?
O5 Dy1 O2 132.73(12) . . ?
O6 Dy1 O2 78.85(12) . . ?
O3 Dy1 O2 139.55(13) . . ?
O1 Dy1 O2 52.49(12) . . ?
O4 Dy1 O2 142.07(10) . . ?
O5 Dy1 N1 77.82(13) . . ?
O6 Dy1 N1 147.37(13) . . ?
O3 Dy1 N1 127.12(13) . . ?
O1 Dy1 N1 74.13(13) . . ?
O4 Dy1 N1 77.15(12) . . ?
O2 Dy1 N1 90.03(13) . . ?
O5 Dy1 N3 147.99(15) . . ?
O6 Dy1 N3 79.42(13) . . ?
O3 Dy1 N3 71.42(14) . . ?
O1 Dy1 N3 122.97(14) . . ?
O4 Dy1 N3 86.13(14) . . ?
O2 Dy1 N3 73.20(14) . . ?
N1 Dy1 N3 126.76(13) . . ?
O5 Dy1 N2 135.32(13) . . ?
O6 Dy1 N2 137.29(12) . . ?
O3 Dy1 N2 107.95(12) . . ?
O1 Dy1 N2 108.17(13) . . ?
O4 Dy1 N2 70.66(11) . . ?
O2 Dy1 N2 71.64(11) . . ?
N1 Dy1 N2 63.71(13) . . ?
N3 Dy1 N2 63.05(14) . . ?
O5 Dy1 C23 76.45(13) . . ?
O6 Dy1 C23 102.45(14) . . ?
O3 Dy1 C23 26.52(13) . . ?
O1 Dy1 C23 156.70(13) . . ?
O4 Dy1 C23 26.48(13) . . ?
O2 Dy1 C23 150.58(12) . . ?
N1 Dy1 C23 102.08(14) . . ?
N3 Dy1 C23 78.13(14) . . ?
N2 Dy1 C23 89.68(12) . . ?
O5 Dy1 C16 106.36(14) . . ?
O6 Dy1 C16 72.21(13) . . ?
O3 Dy1 C16 147.75(13) . . ?
O1 Dy1 C16 26.42(13) . . ?
O4 Dy1 C16 158.75(12) . . ?
O2 Dy1 C16 26.41(12) . . ?
N1 Dy1 C16 84.18(14) . . ?
N3 Dy1 C16 97.22(15) . . ?
N2 Dy1 C16 92.08(12) . . ?
C23 Dy1 C16 173.63(14) . . ?
C30 O5 Dy1 162.9(3) . . ?
C30 O6 Dy1 145.1(3) 2_665 . ?
C16 O2 Dy1 92.1(3) . . ?
C16 O1 Dy1 93.2(3) . . ?
C23 O4 Dy1 92.1(3) . . ?
C10 N2 C6 119.1(4) . . ?
C10 N2 Dy1 120.7(3) . . ?
C6 N2 Dy1 120.0(3) . . ?
C23 O3 Dy1 93.6(3) . . ?
C15 N3 C11 118.3(5) . . ?
C15 N3 Dy1 119.5(4) . . ?
C11 N3 Dy1 121.4(4) . . ?
C1 N1 C5 117.7(4) . . ?
C1 N1 Dy1 120.6(3) . . ?
C5 N1 Dy1 121.7(3) . . ?
O5 C30 O6 125.0(4) . 2_665 ?
O5 C30 C31 117.7(4) . . ?
O6 C30 C31 117.3(4) 2_665 . ?
C19 C18 C17 120.6(5) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
O2 C16 O1 120.7(5) . . ?
O2 C16 C17 119.7(4) . . ?
O1 C16 C17 119.5(4) . . ?
O2 C16 Dy1 61.5(3) . . ?
O1 C16 Dy1 60.4(3) . . ?
C17 C16 Dy1 167.3(3) . . ?
C22 C17 C18 119.1(5) . . ?
C22 C17 C16 120.5(4) . . ?
C18 C17 C16 120.4(5) . . ?
C4 C3 C2 118.7(5) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
N2 C10 C9 121.7(5) . . ?
N2 C10 C11 117.0(4) . . ?
C9 C10 C11 121.3(5) . . ?
O4 C23 O3 121.2(5) . . ?
O4 C23 C24 120.3(4) . . ?
O3 C23 C24 118.5(4) . . ?
O4 C23 Dy1 61.4(2) . . ?
O3 C23 Dy1 59.8(3) . . ?
C24 C23 Dy1 178.2(3) . . ?
C8 C7 C6 120.3(6) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C36 C31 C32 119.1(4) . . ?
C36 C31 C30 120.8(4) . . ?
C32 C31 C30 120.1(4) . . ?
C35 C34 C33 120.8(5) . . ?
C35 C34 I3B 122.1(6) . . ?
C33 C34 I3B 116.7(7) . . ?
C35 C34 I3A 118.7(4) . . ?
C33 C34 I3A 120.2(4) . . ?
N1 C5 C4 121.3(5) . . ?
N1 C5 C6 117.1(4) . . ?
C4 C5 C6 121.5(4) . . ?
C31 C32 C33 120.6(5) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
N2 C6 C7 120.7(5) . . ?
N2 C6 C5 116.7(4) . . ?
C7 C6 C5 122.5(5) . . ?
C26 C27 C28 121.6(5) . . ?
C26 C27 I2 118.5(4) . . ?
C28 C27 I2 120.0(5) . . ?
C19 C20 C21 120.8(6) . . ?
C19 C20 I1 120.2(4) . . ?
C21 C20 I1 119.0(5) . . ?
C31 C36 C35 121.1(5) . . ?
C31 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
N3 C11 C12 121.0(6) . . ?
N3 C11 C10 116.3(4) . . ?
C12 C11 C10 122.8(5) . . ?
C24 C29 C28 120.4(5) . . ?
C24 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C20 C19 C18 119.6(5) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C17 C22 C21 120.5(5) . . ?
C17 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C3 C2 C1 118.8(5) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C20 C21 C22 119.3(6) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C13 C14 C15 118.4(7) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
N1 C1 C2 123.1(5) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
N3 C15 C14 123.3(7) . . ?
N3 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C13 C12 C11 119.3(7) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C29 C24 C25 119.4(5) . . ?
C29 C24 C23 121.2(5) . . ?
C25 C24 C23 119.4(5) . . ?
C32 C33 C34 119.1(5) . . ?
C32 C33 H33 120.5 . . ?
C34 C33 H33 120.5 . . ?
C7 C8 C9 119.0(5) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C27 C28 C29 119.3(6) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
HW1A OW1 HW1B 135(10) . . ?
C26 C25 C24 120.2(5) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C27 C26 C25 119.1(5) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
C34 C35 C36 119.1(5) . . ?
C34 C35 H35 120.4 . . ?
C36 C35 H35 120.4 . . ?
C3 C4 C5 120.4(5) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C8 C9 C10 119.3(6) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C14 C13 C12 119.4(6) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?

_refine_diff_density_max         2.415
_refine_diff_density_min         -2.721
_refine_diff_density_rms         0.134

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
