# Electronic Supplementary Material (ESI) for Green Chemistry.
# 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. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1430391'
_audit_update_record             
;
2015-10-09 deposited with the CCDC.
2017-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            9-Eu
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H72 Cu2 Eu2 I2 N14 O23'
_chemical_formula_weight         1898.00

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.1874(8)
_cell_length_b                   12.6000(9)
_cell_length_c                   15.1798(11)
_cell_angle_alpha                92.5280(10)
_cell_angle_beta                 96.8370(10)
_cell_angle_gamma                116.2890(10)
_cell_volume                     1893.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      0.608
_cell_measurement_theta_max      0.824

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.063
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             932
_exptl_absorpt_coefficient_mu    3.076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15346
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0205
_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       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         24.82
_reflns_number_total             6315
_reflns_number_gt                5629
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0646P)²+3.1834P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6315
_refine_ls_number_parameters     412
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0975
_refine_ls_wR_factor_gt          0.0894
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.29357(2) 0.889285(18) 0.963884(14) 0.02761(9) Uani 1 1 d . . .
I1 I 0.27501(3) 1.42813(3) 0.49164(2) 0.04524(12) Uani 1 1 d . . .
Cu1 Cu 0.51306(6) 1.49833(5) 0.58882(4) 0.03804(16) Uani 1 1 d . . .
O4 O 0.3828(3) 1.0493(3) 0.8739(2) 0.0426(8) Uani 1 1 d . . .
O3 O 0.6089(3) 1.1355(3) 0.8963(2) 0.0406(8) Uani 1 1 d . . .
O2 O 0.4892(4) 0.8842(3) 0.9304(2) 0.0435(8) Uani 1 1 d . . .
O1 O 0.7088(4) 0.9465(3) 0.9483(2) 0.0422(8) Uani 1 1 d . . .
O5 O 0.2289(4) 0.6783(3) 0.9558(3) 0.0558(10) Uani 1 1 d . . .
O6 O 0.1076(4) 0.8116(3) 1.0449(3) 0.0461(9) Uani 1 1 d . . .
N2 N 0.5043(4) 1.3605(4) 0.6622(3) 0.0397(10) Uani 1 1 d . . .
O8 O 0.0861(4) 0.8719(4) 0.8669(3) 0.0619(11) Uani 1 1 d . . .
N1 N 0.5430(4) 0.6278(4) 0.6908(3) 0.0406(10) Uani 1 1 d . . .
O7 O 0.1987(4) 0.7996(4) 0.8049(3) 0.0610(11) Uani 1 1 d . . .
C9 C 0.4989(5) 1.2029(4) 0.7875(3) 0.0356(10) Uani 1 1 d . . .
N4 N 0.0064(5) 0.8680(5) 1.1438(3) 0.0552(12) Uani 1 1 d . . .
C8 C 0.6187(5) 1.2817(5) 0.7623(4) 0.0424(12) Uani 1 1 d . . .
H8A H 0.7015 1.2833 0.7873 0.051 Uiso 1 1 calc R . .
C6 C 0.5920(5) 0.8791(4) 0.9100(3) 0.0340(10) Uani 1 1 d . . .
C12 C 0.4965(5) 1.1214(4) 0.8580(3) 0.0341(10) Uani 1 1 d . . .
N5 N 0.0997(5) 0.8232(5) 0.7988(4) 0.0609(14) Uani 1 1 d . . .
C3 C 0.5747(5) 0.7887(4) 0.8348(3) 0.0341(10) Uani 1 1 d . . .
C10 C 0.3817(6) 1.2013(6) 0.7459(4) 0.0554(16) Uani 1 1 d . . .
H10A H 0.2967 1.1458 0.7591 0.066 Uiso 1 1 calc R . .
C2 C 0.6857(5) 0.7866(5) 0.8044(4) 0.0429(12) Uani 1 1 d . . .
H2A H 0.7746 0.8396 0.8325 0.052 Uiso 1 1 calc R . .
C4 C 0.4478(5) 0.7072(5) 0.7925(4) 0.0474(13) Uani 1 1 d . . .
H4A H 0.3693 0.7054 0.8118 0.057 Uiso 1 1 calc R . .
C1 C 0.6644(5) 0.7056(5) 0.7319(4) 0.0454(12) Uani 1 1 d . . .
H1A H 0.7411 0.7060 0.7107 0.054 Uiso 1 1 calc R . .
C7 C 0.6168(5) 1.3583(5) 0.7002(4) 0.0455(13) Uani 1 1 d . . .
H7A H 0.7002 1.4123 0.6838 0.055 Uiso 1 1 calc R . .
C5 C 0.4365(5) 0.6293(5) 0.7226(4) 0.0508(14) Uani 1 1 d . . .
H5A H 0.3486 0.5731 0.6950 0.061 Uiso 1 1 calc R . .
N3 N 0.2194(6) 0.5208(4) 1.0269(4) 0.0698(15) Uani 1 1 d . . .
C18 C 0.1035(5) 0.8458(5) 1.1216(4) 0.0479(13) Uani 1 1 d . . .
H18A H 0.1750 0.8567 1.1673 0.057 Uiso 1 1 calc R . .
C11 C 0.3889(6) 1.2809(6) 0.6849(4) 0.0583(17) Uani 1 1 d . . .
H11A H 0.3070 1.2790 0.6575 0.070 Uiso 1 1 calc R . .
C15 C 0.1874(6) 0.6076(4) 1.0122(4) 0.0550(15) Uani 1 1 d . . .
H15A H 0.1277 0.6171 1.0478 0.066 Uiso 1 1 calc R . .
O9 O 0.0206(7) 0.7970(8) 0.7301(4) 0.132(3) Uani 1 1 d . . .
C17 C 0.0046(8) 0.9046(8) 1.2356(5) 0.085(2) Uani 1 1 d . . .
H17A H 0.0851 0.9109 1.2737 0.128 Uiso 1 1 calc R . .
H17B H -0.0764 0.8455 1.2560 0.128 Uiso 1 1 calc R . .
H17C H 0.0038 0.9822 1.2390 0.128 Uiso 1 1 calc R . .
C14 C 0.1610(9) 0.4359(6) 1.0917(5) 0.085(2) Uani 1 1 d . . .
H14A H 0.1009 0.4576 1.1218 0.127 Uiso 1 1 calc R . .
H14B H 0.2336 0.4381 1.1359 0.127 Uiso 1 1 calc R . .
H14C H 0.1095 0.3554 1.0604 0.127 Uiso 1 1 calc R . .
C16 C -0.1040(9) 0.8557(9) 1.0774(6) 0.099(3) Uani 1 1 d . . .
H16A H -0.0910 0.8309 1.0187 0.149 Uiso 1 1 calc R . .
H16B H -0.1068 0.9323 1.0761 0.149 Uiso 1 1 calc R . .
H16C H -0.1891 0.7957 1.0924 0.149 Uiso 1 1 calc R . .
C13 C 0.3152(14) 0.5053(11) 0.9760(10) 0.172(7) Uani 1 1 d . . .
H13A H 0.3471 0.5681 0.9364 0.257 Uiso 1 1 calc R . .
H13B H 0.2704 0.4274 0.9404 0.257 Uiso 1 1 calc R . .
H13C H 0.3921 0.5100 1.0174 0.257 Uiso 1 1 calc R . .
N6 N 0.9870(6) 0.5385(5) 0.3210(4) 0.0667(15) Uani 1 1 d . . .
N7 N 0.5100(8) 0.1065(6) 0.4071(5) 0.0859(19) Uani 1 1 d D . .
C20 C 0.9348(8) 0.4386(7) 0.3693(5) 0.078(2) Uani 1 1 d . . .
H20A H 0.8835 0.3663 0.3276 0.116 Uiso 1 1 calc R . .
H20B H 0.8754 0.4479 0.4082 0.116 Uiso 1 1 calc R . .
H20C H 1.0094 0.4323 0.4057 0.116 Uiso 1 1 calc R . .
O10 O 1.0107(8) 0.6029(6) 0.1854(5) 0.129(3) Uani 1 1 d . . .
C21 C 0.9654(9) 0.5246(8) 0.2343(6) 0.093(3) Uani 1 1 d . . .
H21A H 0.9092 0.4461 0.2063 0.111 Uiso 1 1 calc R . .
C19 C 1.0645(10) 0.6531(8) 0.3713(7) 0.107(3) Uani 1 1 d . . .
H19A H 1.0950 0.7144 0.3304 0.161 Uiso 1 1 calc R . .
H19B H 1.1430 0.6540 0.4084 0.161 Uiso 1 1 calc R . .
H19C H 1.0085 0.6691 0.4097 0.161 Uiso 1 1 calc R . .
O11 O 0.3460(13) -0.0358(11) 0.3163(9) 0.199(4) Uani 1 1 d DU . .
C24 C 0.3760(14) 0.0379(16) 0.3748(13) 0.252(11) Uani 1 1 d DU . .
H24A H 0.3088 0.0505 0.3998 0.303 Uiso 1 1 calc R . .
C22 C 0.5215(18) 0.1834(14) 0.4775(10) 0.194(6) Uani 1 1 d U . .
H22A H 0.6166 0.2281 0.5045 0.291 Uiso 1 1 calc R . .
H22B H 0.4686 0.1385 0.5220 0.291 Uiso 1 1 calc R . .
H22C H 0.4878 0.2390 0.4565 0.291 Uiso 1 1 calc R . .
C23 C 0.634(2) 0.128(2) 0.3972(15) 0.261(10) Uani 1 1 d U . .
H23A H 0.6311 0.0727 0.3484 0.391 Uiso 1 1 calc R . .
H23B H 0.6803 0.1172 0.4526 0.391 Uiso 1 1 calc R . .
H23C H 0.6837 0.2100 0.3831 0.391 Uiso 1 1 calc R . .
O1W O 0.0000 0.0000 0.5000 0.291(10) Uani 1 2 d SU . .


_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
Eu1 O2 2.332(3) . ?
Eu1 O3 2.366(3) 2_677 ?
Eu1 O4 2.390(3) . ?
Eu1 O6 2.390(4) . ?
Eu1 O5 2.420(4) . ?
Eu1 O1 2.423(3) 2_677 ?
Eu1 O8 2.512(4) . ?
Eu1 O7 2.513(4) . ?
Eu1 N5 2.933(5) . ?
Eu1 O2 3.025(4) 2_677 ?
Eu1 C6 3.071(5) 2_677 ?
Eu1 Eu1 4.1748(5) 2_677 ?
I1 Cu1 2.6106(7) 2_686 ?
I1 Cu1 2.6294(7) . ?
Cu1 N2 2.077(4) . ?
Cu1 N1 2.082(4) 1_565 ?
Cu1 I1 2.6106(7) 2_686 ?
Cu1 Cu1 2.6818(12) 2_686 ?
O4 C12 1.253(6) . ?
O3 C12 1.254(6) . ?
O3 Eu1 2.366(3) 2_677 ?
O2 C6 1.253(6) . ?
O2 Eu1 3.025(4) 2_677 ?
O1 C6 1.249(6) . ?
O1 Eu1 2.423(3) 2_677 ?
O5 C15 1.240(7) . ?
O6 C18 1.237(7) . ?
N2 C7 1.333(6) . ?
N2 C11 1.334(7) . ?
O8 N5 1.238(6) . ?
N1 C1 1.328(7) . ?
N1 C5 1.345(7) . ?
N1 Cu1 2.082(4) 1_545 ?
O7 N5 1.262(6) . ?
C9 C10 1.376(7) . ?
C9 C8 1.380(7) . ?
C9 C12 1.511(6) . ?
N4 C18 1.310(7) . ?
N4 C16 1.445(9) . ?
N4 C17 1.455(8) . ?
C8 C7 1.383(7) . ?
C6 C3 1.509(6) . ?
C6 Eu1 3.071(5) 2_677 ?
N5 O9 1.213(7) . ?
C3 C4 1.384(7) . ?
C3 C2 1.386(7) . ?
C10 C11 1.377(7) . ?
C2 C1 1.389(7) . ?
C4 C5 1.369(7) . ?
N3 C15 1.312(8) . ?
N3 C13 1.468(11) . ?
N3 C14 1.471(9) . ?
N6 C21 1.299(10) . ?
N6 C20 1.413(9) . ?
N6 C19 1.434(10) . ?
N7 C23 1.323(19) . ?
N7 C22 1.365(15) . ?
N7 C24 1.369(10) . ?
O10 C21 1.222(10) . ?
O11 C24 1.159(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
O2 Eu1 O3 77.71(12) . 2_677 ?
O2 Eu1 O4 76.68(12) . . ?
O3 Eu1 O4 128.97(12) 2_677 . ?
O2 Eu1 O6 147.32(13) . . ?
O3 Eu1 O6 76.64(13) 2_677 . ?
O4 Eu1 O6 135.80(13) . . ?
O2 Eu1 O5 78.41(14) . . ?
O3 Eu1 O5 75.74(13) 2_677 . ?
O4 Eu1 O5 138.72(13) . . ?
O6 Eu1 O5 75.90(14) . . ?
O2 Eu1 O1 124.15(13) . 2_677 ?
O3 Eu1 O1 81.89(12) 2_677 2_677 ?
O4 Eu1 O1 77.28(12) . 2_677 ?
O6 Eu1 O1 71.43(12) . 2_677 ?
O5 Eu1 O1 143.81(13) . 2_677 ?
O2 Eu1 O8 132.23(13) . . ?
O3 Eu1 O8 147.72(13) 2_677 . ?
O4 Eu1 O8 77.13(14) . . ?
O6 Eu1 O8 71.08(14) . . ?
O5 Eu1 O8 96.59(15) . . ?
O1 Eu1 O8 87.34(13) 2_677 . ?
O2 Eu1 O7 84.39(14) . . ?
O3 Eu1 O7 145.04(13) 2_677 . ?
O4 Eu1 O7 73.89(14) . . ?
O6 Eu1 O7 105.85(15) . . ?
O5 Eu1 O7 71.35(14) . . ?
O1 Eu1 O7 132.57(13) 2_677 . ?
O8 Eu1 O7 50.09(14) . . ?
O2 Eu1 N5 108.58(15) . . ?
O3 Eu1 N5 157.38(14) 2_677 . ?
O4 Eu1 N5 73.40(14) . . ?
O6 Eu1 N5 88.61(15) . . ?
O5 Eu1 N5 84.16(15) . . ?
O1 Eu1 N5 109.84(14) 2_677 . ?
O8 Eu1 N5 24.77(14) . . ?
O7 Eu1 N5 25.33(14) . . ?
O2 Eu1 O2 78.37(12) . 2_677 ?
O3 Eu1 O2 64.73(11) 2_677 2_677 ?
O4 Eu1 O2 67.30(11) . 2_677 ?
O6 Eu1 O2 108.02(11) . 2_677 ?
O5 Eu1 O2 137.42(12) . 2_677 ?
O1 Eu1 O2 46.02(10) 2_677 2_677 ?
O8 Eu1 O2 125.27(13) . 2_677 ?
O7 Eu1 O2 140.14(13) . 2_677 ?
N5 Eu1 O2 137.27(13) . 2_677 ?
O2 Eu1 C6 102.08(13) . 2_677 ?
O3 Eu1 C6 69.91(12) 2_677 2_677 ?
O4 Eu1 C6 73.38(12) . 2_677 ?
O6 Eu1 C6 87.74(13) . 2_677 ?
O5 Eu1 C6 144.55(13) . 2_677 ?
O1 Eu1 C6 22.57(12) 2_677 2_677 ?
O8 Eu1 C6 107.68(14) . 2_677 ?
O7 Eu1 C6 144.05(13) . 2_677 ?
N5 Eu1 C6 127.30(14) . 2_677 ?
O2 Eu1 C6 23.71(11) 2_677 2_677 ?
O2 Eu1 Eu1 45.20(9) . 2_677 ?
O3 Eu1 Eu1 64.65(8) 2_677 2_677 ?
O4 Eu1 Eu1 65.91(8) . 2_677 ?
O6 Eu1 Eu1 133.97(9) . 2_677 ?
O5 Eu1 Eu1 114.92(11) . 2_677 ?
O1 Eu1 Eu1 79.07(9) 2_677 2_677 ?
O8 Eu1 Eu1 142.54(11) . 2_677 ?
O7 Eu1 Eu1 120.10(11) . 2_677 ?
N5 Eu1 Eu1 135.25(12) . 2_677 ?
O2 Eu1 Eu1 33.17(6) 2_677 2_677 ?
C6 Eu1 Eu1 56.88(9) 2_677 2_677 ?
Cu1 I1 Cu1 61.57(2) 2_686 . ?
N2 Cu1 N1 100.68(17) . 1_565 ?
N2 Cu1 I1 109.46(12) . 2_686 ?
N1 Cu1 I1 109.32(12) 1_565 2_686 ?
N2 Cu1 I1 107.77(12) . . ?
N1 Cu1 I1 109.71(12) 1_565 . ?
I1 Cu1 I1 118.43(2) 2_686 . ?
N2 Cu1 Cu1 128.57(13) . 2_686 ?
N1 Cu1 Cu1 130.74(13) 1_565 2_686 ?
I1 Cu1 Cu1 59.56(2) 2_686 2_686 ?
I1 Cu1 Cu1 58.87(2) . 2_686 ?
C12 O4 Eu1 137.5(3) . . ?
C12 O3 Eu1 139.0(3) . 2_677 ?
C6 O2 Eu1 178.0(3) . . ?
C6 O2 Eu1 80.2(3) . 2_677 ?
Eu1 O2 Eu1 101.63(11) . 2_677 ?
C6 O1 Eu1 109.3(3) . 2_677 ?
C15 O5 Eu1 130.0(4) . . ?
C18 O6 Eu1 127.7(3) . . ?
C7 N2 C11 116.4(4) . . ?
C7 N2 Cu1 120.8(3) . . ?
C11 N2 Cu1 122.0(3) . . ?
N5 O8 Eu1 97.0(3) . . ?
C1 N1 C5 116.7(4) . . ?
C1 N1 Cu1 123.1(3) . 1_545 ?
C5 N1 Cu1 120.0(3) . 1_545 ?
N5 O7 Eu1 96.2(3) . . ?
C10 C9 C8 117.6(4) . . ?
C10 C9 C12 121.2(4) . . ?
C8 C9 C12 121.2(4) . . ?
C18 N4 C16 120.9(6) . . ?
C18 N4 C17 121.7(6) . . ?
C16 N4 C17 117.4(6) . . ?
C9 C8 C7 119.3(5) . . ?
O1 C6 O2 123.1(4) . . ?
O1 C6 C3 118.2(4) . . ?
O2 C6 C3 118.7(4) . . ?
O1 C6 Eu1 48.1(2) . 2_677 ?
O2 C6 Eu1 76.0(3) . 2_677 ?
C3 C6 Eu1 161.7(3) . 2_677 ?
O4 C12 O3 126.8(4) . . ?
O4 C12 C9 116.8(4) . . ?
O3 C12 C9 116.4(4) . . ?
O9 N5 O8 121.9(6) . . ?
O9 N5 O7 121.4(6) . . ?
O8 N5 O7 116.6(5) . . ?
O9 N5 Eu1 179.3(7) . . ?
O8 N5 Eu1 58.2(3) . . ?
O7 N5 Eu1 58.4(3) . . ?
C4 C3 C2 117.9(4) . . ?
C4 C3 C6 121.2(4) . . ?
C2 C3 C6 120.9(4) . . ?
C9 C10 C11 119.4(5) . . ?
C3 C2 C1 118.7(5) . . ?
C5 C4 C3 119.4(5) . . ?
N1 C1 C2 123.7(5) . . ?
N2 C7 C8 123.5(5) . . ?
N1 C5 C4 123.6(5) . . ?
C15 N3 C13 119.4(6) . . ?
C15 N3 C14 122.7(7) . . ?
C13 N3 C14 117.9(6) . . ?
O6 C18 N4 124.0(6) . . ?
N2 C11 C10 123.8(5) . . ?
O5 C15 N3 125.3(6) . . ?
C21 N6 C20 120.2(7) . . ?
C21 N6 C19 122.4(7) . . ?
C20 N6 C19 117.4(7) . . ?
C23 N7 C22 106.5(13) . . ?
C23 N7 C24 144.7(14) . . ?
C22 N7 C24 108.8(12) . . ?
O10 C21 N6 126.2(8) . . ?
O11 C24 N7 118.8(17) . . ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        24.82
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         1.301
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.125
####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1430398'
_audit_update_record             
;
2015-10-09 deposited with the CCDC.
2017-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            9-Y
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H72 Cu2 I2 N14 O23 Y2'
_chemical_formula_weight         1771.90

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.2135(7)
_cell_length_b                   12.5387(7)
_cell_length_c                   15.1202(9)
_cell_angle_alpha                92.0920(10)
_cell_angle_beta                 97.4150(10)
_cell_angle_gamma                116.3890(10)
_cell_volume                     1877.91(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.053
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             884
_exptl_absorpt_coefficient_mu    2.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15343
_diffrn_reflns_av_R_equivalents  0.0131
_diffrn_reflns_av_sigmaI/netI    0.0175
_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       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         24.84
_reflns_number_total             6287
_reflns_number_gt                5551
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0739P)²+2.8408P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6287
_refine_ls_number_parameters     407
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.1141
_refine_ls_wR_factor_gt          0.1095
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.27512(3) -0.07243(3) 0.49050(2) 0.04389(12) Uani 1 1 d . . .
Cu1 Cu 0.48627(6) 0.00199(5) 0.41057(3) 0.03700(15) Uani 1 1 d . . .
Y1 Y 0.70833(4) 0.61286(3) 0.03624(2) 0.02657(12) Uani 1 1 d . . .
O4 O 0.6182(3) 0.4550(3) 0.1239(2) 0.0398(7) Uani 1 1 d . . .
O3 O 0.3919(3) 0.3690(3) 0.1015(2) 0.0373(7) Uani 1 1 d . . .
O1 O 0.3018(3) 0.5521(3) 0.0510(2) 0.0372(7) Uani 1 1 d . . .
O2 O 0.5243(3) 0.6246(3) 0.0719(2) 0.0406(7) Uani 1 1 d . . .
O6 O 0.8898(3) 0.6849(3) -0.0429(2) 0.0435(8) Uani 1 1 d . . .
O5 O 0.7748(4) 0.8204(3) 0.0416(2) 0.0539(9) Uani 1 1 d . . .
N2 N 0.4965(4) 0.1419(3) 0.3373(2) 0.0390(8) Uani 1 1 d . . .
O7 O 0.8025(4) 0.7014(3) 0.1924(2) 0.0590(10) Uani 1 1 d . . .
N1 N 0.4580(4) 0.8733(3) 0.3083(2) 0.0396(9) Uani 1 1 d . . .
O8 O 0.9093(4) 0.6224(4) 0.1317(3) 0.0615(10) Uani 1 1 d . . .
N4 N 0.9922(4) 0.6304(4) -0.1409(3) 0.0529(11) Uani 1 1 d . . .
C9 C 0.5024(4) 0.3010(4) 0.2114(3) 0.0323(9) Uani 1 1 d . . .
C2 C 0.3177(4) 0.7115(4) 0.1945(3) 0.0400(10) Uani 1 1 d . . .
H2A H 0.2293 0.6562 0.1664 0.048 Uiso 1 1 calc R . .
C12 C 0.5043(4) 0.3826(4) 0.1397(3) 0.0322(9) Uani 1 1 d . . .
C6 C 0.4175(4) 0.6239(4) 0.0898(3) 0.0315(9) Uani 1 1 d . . .
C3 C 0.4304(4) 0.7130(4) 0.1642(3) 0.0316(9) Uani 1 1 d . . .
C8 C 0.3821(5) 0.2235(4) 0.2378(3) 0.0423(11) Uani 1 1 d . . .
H8A H 0.2996 0.2234 0.2136 0.051 Uiso 1 1 calc R . .
N5 N 0.8991(5) 0.6752(4) 0.1997(3) 0.0585(12) Uani 1 1 d . . .
N6 N 0.0140(5) 0.9601(5) 0.6793(4) 0.0665(13) Uani 1 1 d . . .
C7 C 0.3848(5) 0.1460(4) 0.3004(3) 0.0417(11) Uani 1 1 d . . .
H7A H 0.3019 0.0928 0.3178 0.050 Uiso 1 1 calc R . .
C4 C 0.5561(5) 0.7971(4) 0.2068(3) 0.0467(12) Uani 1 1 d . . .
H4A H 0.6354 0.8012 0.1879 0.056 Uiso 1 1 calc R . .
C5 C 0.5655(5) 0.8750(5) 0.2771(3) 0.0492(12) Uani 1 1 d . . .
H5A H 0.6527 0.9331 0.3049 0.059 Uiso 1 1 calc R . .
C15 C 0.8155(5) 0.8913(4) -0.0148(4) 0.0512(12) Uani 1 1 d . . .
H15A H 0.8763 0.8830 -0.0496 0.061 Uiso 1 1 calc R . .
C18 C 0.8940(5) 0.6494(4) -0.1195(3) 0.0450(11) Uani 1 1 d . . .
H18A H 0.8208 0.6352 -0.1656 0.054 Uiso 1 1 calc R . .
C10 C 0.6187(5) 0.3001(5) 0.2525(4) 0.0543(14) Uani 1 1 d . . .
H10A H 0.7036 0.3547 0.2386 0.065 Uiso 1 1 calc R . .
N3 N 0.7818(5) 0.9772(4) -0.0307(4) 0.0640(13) Uani 1 1 d . . .
C1 C 0.3365(5) 0.7919(4) 0.2663(3) 0.0434(11) Uani 1 1 d . . .
H1A H 0.2589 0.7893 0.2870 0.052 Uiso 1 1 calc R . .
O9 O 0.9792(6) 0.6990(7) 0.2684(4) 0.123(2) Uani 1 1 d . . .
O10 O -0.0084(8) 0.8947(5) 0.8149(4) 0.133(3) Uani 1 1 d . . .
C21 C 0.0366(8) 0.9744(7) 0.7666(5) 0.091(2) Uani 1 1 d . . .
H21A H 0.0926 1.0532 0.7950 0.109 Uiso 1 1 calc R . .
C14 C 0.8403(8) 1.0635(5) -0.0949(5) 0.082(2) Uani 1 1 d . . .
H14A H 0.9047 1.0453 -0.1221 0.122 Uiso 1 1 calc R . .
H14B H 0.8869 1.1446 -0.0636 0.122 Uiso 1 1 calc R . .
H14C H 0.7683 1.0581 -0.1418 0.122 Uiso 1 1 calc R . .
C11 C 0.6117(5) 0.2198(5) 0.3137(4) 0.0553(14) Uani 1 1 d . . .
H11A H 0.6932 0.2199 0.3406 0.066 Uiso 1 1 calc R . .
C17 C 0.9946(8) 0.5933(8) -0.2329(5) 0.081(2) Uani 1 1 d . . .
H17A H 0.9142 0.5865 -0.2719 0.122 Uiso 1 1 calc R . .
H17B H 0.9957 0.5155 -0.2356 0.122 Uiso 1 1 calc R . .
H17C H 1.0756 0.6529 -0.2530 0.122 Uiso 1 1 calc R . .
C20 C 0.0670(7) 1.0624(7) 0.6306(5) 0.0782(19) Uani 1 1 d . . .
H20A H 0.1209 1.1344 0.6727 0.117 Uiso 1 1 calc R . .
H20B H -0.0076 1.0706 0.5953 0.117 Uiso 1 1 calc R . .
H20C H 0.1239 1.0523 0.5903 0.117 Uiso 1 1 calc R . .
C19 C -0.0664(9) 0.8471(8) 0.6276(6) 0.111(3) Uani 1 1 d . . .
H19A H -0.0968 0.7840 0.6679 0.166 Uiso 1 1 calc R . .
H19B H -0.0127 0.8310 0.5877 0.166 Uiso 1 1 calc R . .
H19C H -0.1449 0.8485 0.5918 0.166 Uiso 1 1 calc R . .
C16 C 1.1038(7) 0.6454(7) -0.0731(5) 0.090(2) Uani 1 1 d . . .
H16A H 1.0900 0.6699 -0.0145 0.135 Uiso 1 1 calc R . .
H16B H 1.1881 0.7069 -0.0880 0.135 Uiso 1 1 calc R . .
H16C H 1.1087 0.5694 -0.0709 0.135 Uiso 1 1 calc R . .
C13 C 0.6839(12) 0.9899(10) 0.0185(9) 0.158(6) Uani 1 1 d . . .
H13A H 0.6532 0.9268 0.0587 0.237 Uiso 1 1 calc R . .
H13B H 0.6065 0.9831 -0.0240 0.237 Uiso 1 1 calc R . .
H13C H 0.7264 1.0684 0.0539 0.237 Uiso 1 1 calc R . .
N7 N 0.4898(7) 0.3920(5) 0.5917(4) 0.0804(16) Uani 1 1 d D . .
O11 O 0.6640(11) 0.5402(8) 0.6861(7) 0.178(4) Uani 1 1 d DU . .
C24 C 0.6153(13) 0.4644(11) 0.6324(9) 0.188(6) Uani 1 1 d DU . .
H24A H 0.6797 0.4462 0.6092 0.226 Uiso 1 1 calc R . .
C23 C 0.4754(17) 0.3163(13) 0.5181(10) 0.189(6) Uani 1 1 d U . .
H23A H 0.5644 0.3257 0.5090 0.284 Uiso 1 1 calc R . .
H23B H 0.4329 0.3362 0.4648 0.284 Uiso 1 1 calc R . .
H23C H 0.4188 0.2333 0.5284 0.284 Uiso 1 1 calc R . .
C22 C 0.3708(19) 0.3866(19) 0.6062(13) 0.241(8) Uani 1 1 d U . .
H22A H 0.3866 0.4442 0.6574 0.361 Uiso 1 1 calc R . .
H22B H 0.3112 0.3057 0.6192 0.361 Uiso 1 1 calc R . .
H22C H 0.3283 0.4061 0.5527 0.361 Uiso 1 1 calc R . .
O1W O 1.0000 0.5000 -0.5000 0.285(10) Uiso 1 2 d S . .


_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
I1 Cu1 2.6067(6) . ?
I1 Cu1 2.6356(6) 2_656 ?
Cu1 N2 2.078(4) . ?
Cu1 N1 2.081(4) 1_545 ?
Cu1 I1 2.6356(6) 2_656 ?
Cu1 Cu1 2.6870(10) 2_656 ?
Y1 O2 2.263(3) . ?
Y1 O3 2.304(3) 2_665 ?
Y1 O4 2.336(3) . ?
Y1 O6 2.337(3) . ?
Y1 O5 2.362(3) . ?
Y1 O1 2.364(3) 2_665 ?
Y1 O7 2.459(3) . ?
Y1 O8 2.467(4) . ?
Y1 N5 2.882(4) . ?
O4 C12 1.255(5) . ?
O3 C12 1.251(5) . ?
O3 Y1 2.304(3) 2_665 ?
O1 C6 1.251(5) . ?
O1 Y1 2.364(3) 2_665 ?
O2 C6 1.258(5) . ?
O6 C18 1.240(6) . ?
O5 C15 1.234(6) . ?
N2 C7 1.326(6) . ?
N2 C11 1.331(6) . ?
O7 N5 1.258(6) . ?
N1 C1 1.339(6) . ?
N1 C5 1.342(6) . ?
N1 Cu1 2.081(4) 1_565 ?
O8 N5 1.247(6) . ?
N4 C18 1.301(6) . ?
N4 C16 1.448(8) . ?
N4 C17 1.458(8) . ?
C9 C10 1.375(7) . ?
C9 C8 1.389(6) . ?
C9 C12 1.513(6) . ?
C2 C1 1.382(6) . ?
C2 C3 1.391(6) . ?
C6 C3 1.503(6) . ?
C3 C4 1.382(6) . ?
C8 C7 1.388(6) . ?
N5 O9 1.213(6) . ?
N6 C21 1.302(9) . ?
N6 C19 1.426(9) . ?
N6 C20 1.431(9) . ?
C4 C5 1.377(7) . ?
C15 N3 1.311(7) . ?
C10 C11 1.377(7) . ?
N3 C13 1.464(10) . ?
N3 C14 1.467(8) . ?
O10 C21 1.219(9) . ?
N7 C24 1.335(9) . ?
N7 C22 1.354(18) . ?
N7 C23 1.380(15) . ?
O11 C24 1.108(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
Cu1 I1 Cu1 61.67(2) . 2_656 ?
N2 Cu1 N1 100.85(15) . 1_545 ?
N2 Cu1 I1 109.69(11) . . ?
N1 Cu1 I1 109.89(11) 1_545 . ?
N2 Cu1 I1 107.36(11) . 2_656 ?
N1 Cu1 I1 109.28(11) 1_545 2_656 ?
I1 Cu1 I1 118.33(2) . 2_656 ?
N2 Cu1 Cu1 128.28(11) . 2_656 ?
N1 Cu1 Cu1 130.83(11) 1_545 2_656 ?
I1 Cu1 Cu1 59.70(2) . 2_656 ?
I1 Cu1 Cu1 58.64(2) 2_656 2_656 ?
O2 Y1 O3 78.47(11) . 2_665 ?
O2 Y1 O4 76.72(11) . . ?
O3 Y1 O4 126.51(11) 2_665 . ?
O2 Y1 O6 148.05(11) . . ?
O3 Y1 O6 78.13(11) 2_665 . ?
O4 Y1 O6 135.11(11) . . ?
O2 Y1 O5 77.64(12) . . ?
O3 Y1 O5 77.05(12) 2_665 . ?
O4 Y1 O5 139.74(12) . . ?
O6 Y1 O5 76.15(12) . . ?
O2 Y1 O1 123.69(11) . 2_665 ?
O3 Y1 O1 79.28(11) 2_665 2_665 ?
O4 Y1 O1 76.53(11) . 2_665 ?
O6 Y1 O1 72.31(11) . 2_665 ?
O5 Y1 O1 143.70(12) . 2_665 ?
O2 Y1 O7 82.49(13) . . ?
O3 Y1 O7 146.28(12) 2_665 . ?
O4 Y1 O7 74.48(12) . . ?
O6 Y1 O7 106.06(13) . . ?
O5 Y1 O7 71.82(13) . . ?
O1 Y1 O7 134.28(12) 2_665 . ?
O2 Y1 O8 131.16(12) . . ?
O3 Y1 O8 148.92(12) 2_665 . ?
O4 Y1 O8 76.58(13) . . ?
O6 Y1 O8 70.97(13) . . ?
O5 Y1 O8 98.27(14) . . ?
O1 Y1 O8 88.13(12) 2_665 . ?
O7 Y1 O8 51.20(13) . . ?
O2 Y1 N5 107.03(13) . . ?
O3 Y1 N5 159.70(12) 2_665 . ?
O4 Y1 N5 73.62(12) . . ?
O6 Y1 N5 88.56(14) . . ?
O5 Y1 N5 84.97(14) . . ?
O1 Y1 N5 111.42(13) 2_665 . ?
O7 Y1 N5 25.72(13) . . ?
O8 Y1 N5 25.48(13) . . ?
C12 O4 Y1 138.1(3) . . ?
C12 O3 Y1 139.5(3) . 2_665 ?
C6 O1 Y1 114.5(3) . 2_665 ?
C6 O2 Y1 176.2(3) . . ?
C18 O6 Y1 128.2(3) . . ?
C15 O5 Y1 131.2(3) . . ?
C7 N2 C11 117.0(4) . . ?
C7 N2 Cu1 120.6(3) . . ?
C11 N2 Cu1 121.6(3) . . ?
N5 O7 Y1 96.3(3) . . ?
C1 N1 C5 116.6(4) . . ?
C1 N1 Cu1 123.7(3) . 1_565 ?
C5 N1 Cu1 119.5(3) . 1_565 ?
N5 O8 Y1 96.2(3) . . ?
C18 N4 C16 120.6(5) . . ?
C18 N4 C17 121.9(5) . . ?
C16 N4 C17 117.5(5) . . ?
C10 C9 C8 117.4(4) . . ?
C10 C9 C12 121.7(4) . . ?
C8 C9 C12 120.8(4) . . ?
C1 C2 C3 118.8(4) . . ?
O3 C12 O4 127.1(4) . . ?
O3 C12 C9 116.3(4) . . ?
O4 C12 C9 116.5(4) . . ?
O1 C6 O2 124.1(4) . . ?
O1 C6 C3 118.3(4) . . ?
O2 C6 C3 117.6(4) . . ?
C4 C3 C2 117.8(4) . . ?
C4 C3 C6 120.5(4) . . ?
C2 C3 C6 121.7(4) . . ?
C7 C8 C9 118.6(4) . . ?
O9 N5 O8 120.8(5) . . ?
O9 N5 O7 122.9(5) . . ?
O8 N5 O7 116.3(4) . . ?
O9 N5 Y1 178.7(5) . . ?
O8 N5 Y1 58.3(2) . . ?
O7 N5 Y1 58.0(2) . . ?
C21 N6 C19 123.7(7) . . ?
C21 N6 C20 119.5(6) . . ?
C19 N6 C20 116.7(6) . . ?
N2 C7 C8 123.7(4) . . ?
C5 C4 C3 119.5(4) . . ?
N1 C5 C4 123.5(4) . . ?
O5 C15 N3 125.3(5) . . ?
O6 C18 N4 124.1(5) . . ?
C9 C10 C11 119.9(4) . . ?
C15 N3 C13 119.2(6) . . ?
C15 N3 C14 122.7(6) . . ?
C13 N3 C14 118.1(6) . . ?
N1 C1 C2 123.7(4) . . ?
O10 C21 N6 125.2(7) . . ?
N2 C11 C10 123.2(4) . . ?
C24 N7 C22 130.1(13) . . ?
C24 N7 C23 117.2(11) . . ?
C22 N7 C23 112.5(12) . . ?
O11 C24 N7 136.7(17) . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        24.84
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         1.316
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.104
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1430396'
_audit_update_record             
;
2015-10-09 deposited with the CCDC.
2017-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            9-Er
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H72 Cu2 Er2 I2 N14 O23'
_chemical_formula_weight         1928.60

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.2006(9)
_cell_length_b                   12.5227(10)
_cell_length_c                   15.1130(13)
_cell_angle_alpha                92.0840(10)
_cell_angle_beta                 97.4140(10)
_cell_angle_gamma                116.4500(10)
_cell_volume                     1871.5(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.088
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             942
_exptl_absorpt_coefficient_mu    3.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.453
_exptl_absorpt_correction_T_max  0.723
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13597
_diffrn_reflns_av_R_equivalents  0.0101
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         24.79
_reflns_number_total             6257
_reflns_number_gt                5860
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0375P)²+5.7515P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6257
_refine_ls_number_parameters     412
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0228
_refine_ls_wR_factor_ref         0.0740
_refine_ls_wR_factor_gt          0.0722
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.208149(18) 0.112704(15) 0.536189(12) 0.02553(7) Uani 1 1 d . . .
Cu1 Cu 0.01376(6) 0.49799(5) 0.08948(4) 0.03552(14) Uani 1 1 d . . .
I1 I 0.22515(3) 0.57300(3) 0.00946(2) 0.04211(10) Uani 1 1 d . . .
O1 O 0.1982(3) -0.0518(3) 0.4498(2) 0.0357(7) Uani 1 1 d . . .
O2 O -0.0245(3) -0.1249(3) 0.4286(2) 0.0390(7) Uani 1 1 d . . .
O3 O 0.1085(3) 0.1310(3) 0.3988(2) 0.0359(7) Uani 1 1 d . . .
O4 O -0.1180(3) 0.0453(3) 0.3767(2) 0.0381(7) Uani 1 1 d . . .
O5 O 0.3894(3) 0.1848(3) 0.4578(2) 0.0430(8) Uani 1 1 d . . .
O6 O 0.2744(4) 0.3200(3) 0.5420(3) 0.0516(9) Uani 1 1 d . . .
O7 O 0.3021(4) 0.2014(4) 0.6919(3) 0.0591(11) Uani 1 1 d . . .
O8 O 0.4080(4) 0.1215(4) 0.6309(3) 0.0593(10) Uani 1 1 d . . .
O9 O 0.4780(7) 0.1995(7) 0.7683(4) 0.120(2) Uani 1 1 d . . .
O10 O 0.5063(8) 0.6063(6) 0.6843(4) 0.129(3) Uani 1 1 d . . .
N1 N 0.0424(4) -0.3731(4) 0.1921(3) 0.0382(9) Uani 1 1 d . . .
N2 N 0.0040(4) 0.3587(4) 0.1634(3) 0.0372(9) Uani 1 1 d . . .
N3 N 0.3980(5) 0.1745(5) 0.6991(3) 0.0577(13) Uani 1 1 d . . .
N4 N 0.4932(5) 0.1310(4) 0.3596(3) 0.0507(11) Uani 1 1 d . . .
N5 N 0.2823(6) 0.4768(4) 0.4689(4) 0.0631(14) Uani 1 1 d . . .
N6 N 0.4852(5) 0.5396(5) 0.8205(4) 0.0642(14) Uani 1 1 d . . .
C1 C 0.1633(5) -0.2922(5) 0.2338(3) 0.0410(11) Uani 1 1 d . . .
H1A H 0.2411 -0.2894 0.2131 0.049 Uiso 1 1 calc R . .
C2 C 0.1818(5) -0.2116(4) 0.3060(3) 0.0396(11) Uani 1 1 d . . .
H2A H 0.2701 -0.1562 0.3345 0.048 Uiso 1 1 calc R . .
C3 C 0.0689(4) -0.2135(4) 0.3356(3) 0.0307(9) Uani 1 1 d . . .
C4 C -0.0565(5) -0.2971(5) 0.2932(4) 0.0450(12) Uani 1 1 d . . .
H4A H -0.1360 -0.3016 0.3124 0.054 Uiso 1 1 calc R . .
C5 C -0.0653(5) -0.3745(5) 0.2224(4) 0.0484(13) Uani 1 1 d . . .
H5A H -0.1526 -0.4317 0.1935 0.058 Uiso 1 1 calc R . .
C6 C 0.0818(5) -0.1239(4) 0.4106(3) 0.0303(9) Uani 1 1 d . . .
C7 C 0.1161(5) 0.3541(5) 0.2005(3) 0.0419(11) Uani 1 1 d . . .
H7A H 0.1993 0.4069 0.1831 0.050 Uiso 1 1 calc R . .
C8 C 0.1176(5) 0.2772(4) 0.2627(3) 0.0388(11) Uani 1 1 d . . .
H8A H 0.2002 0.2774 0.2872 0.047 Uiso 1 1 calc R . .
C9 C -0.0015(5) 0.1997(4) 0.2893(3) 0.0319(9) Uani 1 1 d . . .
C10 C -0.1187(5) 0.2005(5) 0.2488(4) 0.0521(14) Uani 1 1 d . . .
H10A H -0.2034 0.1464 0.2635 0.063 Uiso 1 1 calc R . .
C11 C -0.1119(5) 0.2801(5) 0.1871(4) 0.0544(15) Uani 1 1 d . . .
H11A H -0.1937 0.2793 0.1599 0.065 Uiso 1 1 calc R . .
C12 C -0.0049(5) 0.1172(4) 0.3607(3) 0.0311(9) Uani 1 1 d . . .
C13 C 0.6067(8) 0.1486(8) 0.4274(6) 0.090(3) Uani 1 1 d . . .
H13A H 0.5926 0.1727 0.4860 0.134 Uiso 1 1 calc R . .
H13B H 0.6902 0.2115 0.4121 0.134 Uiso 1 1 calc R . .
H13C H 0.6139 0.0736 0.4298 0.134 Uiso 1 1 calc R . .
C14 C 0.4960(8) 0.0955(8) 0.2675(5) 0.079(2) Uani 1 1 d . . .
H14A H 0.4144 0.0871 0.2288 0.118 Uiso 1 1 calc R . .
H14B H 0.4995 0.0186 0.2644 0.118 Uiso 1 1 calc R . .
H14C H 0.5760 0.1567 0.2473 0.118 Uiso 1 1 calc R . .
C15 C 0.3941(5) 0.1493(5) 0.3811(4) 0.0437(12) Uani 1 1 d . . .
H15A H 0.3207 0.1345 0.3350 0.052 Uiso 1 1 calc R . .
C16 C 0.1862(13) 0.4906(10) 0.5186(9) 0.154(6) Uani 1 1 d . . .
H16A H 0.1544 0.4267 0.5582 0.231 Uiso 1 1 calc R . .
H16B H 0.1092 0.4855 0.4765 0.231 Uiso 1 1 calc R . .
H16C H 0.2304 0.5688 0.5547 0.231 Uiso 1 1 calc R . .
C17 C 0.3419(8) 0.5626(6) 0.4050(5) 0.079(2) Uani 1 1 d . . .
H17A H 0.4031 0.5415 0.3760 0.118 Uiso 1 1 calc R . .
H17B H 0.3925 0.6435 0.4367 0.118 Uiso 1 1 calc R . .
H17C H 0.2700 0.5603 0.3593 0.118 Uiso 1 1 calc R . .
C18 C 0.3163(6) 0.3913(4) 0.4854(4) 0.0495(13) Uani 1 1 d . . .
H18A H 0.3780 0.3833 0.4513 0.059 Uiso 1 1 calc R . .
C19 C 0.5653(9) 0.6541(8) 0.8722(6) 0.106(3) Uani 1 1 d . . .
H19A H 0.5951 0.7170 0.8317 0.159 Uiso 1 1 calc R . .
H19B H 0.6444 0.6538 0.9082 0.159 Uiso 1 1 calc R . .
H19C H 0.5110 0.6697 0.9120 0.159 Uiso 1 1 calc R . .
C20 C 0.4331(8) 0.4368(7) 0.8694(5) 0.0739(19) Uani 1 1 d . . .
H20A H 0.3804 0.3645 0.8272 0.111 Uiso 1 1 calc R . .
H20B H 0.3751 0.4459 0.9092 0.111 Uiso 1 1 calc R . .
H20C H 0.5083 0.4299 0.9051 0.111 Uiso 1 1 calc R . .
C21 C 0.4623(9) 0.5261(7) 0.7329(5) 0.088(2) Uani 1 1 d . . .
H21A H 0.4065 0.4472 0.7045 0.105 Uiso 1 1 calc R . .
N7 N -0.0105(7) 0.8912(5) 0.0923(4) 0.0800(17) Uani 1 1 d D . .
O11 O 0.1648(11) 1.0416(9) 0.1857(7) 0.175(4) Uani 1 1 d DU . .
C23 C -0.0279(17) 0.8137(13) 0.0229(9) 0.178(6) Uani 1 1 d U . .
H23A H 0.0605 0.8245 0.0108 0.268 Uiso 1 1 calc R . .
H23B H -0.0764 0.8283 -0.0302 0.268 Uiso 1 1 calc R . .
H23C H -0.0803 0.7316 0.0372 0.268 Uiso 1 1 calc R . .
C22 C -0.134(2) 0.8776(19) 0.1109(14) 0.247(9) Uani 1 1 d U . .
H22A H -0.2069 0.8138 0.0686 0.370 Uiso 1 1 calc R . .
H22B H -0.1395 0.9530 0.1048 0.370 Uiso 1 1 calc R . .
H22C H -0.1431 0.8563 0.1723 0.370 Uiso 1 1 calc R . .
O1W O 0.5000 0.0000 0.0000 0.297(11) Uani 1 2 d SU . .
C24 C 0.1162(13) 0.9621(11) 0.1300(9) 0.187(6) Uani 1 1 d DU . .
H24A H 0.1813 0.9445 0.1057 0.225 Uiso 1 1 d R . .


_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 O2 2.257(3) 2_556 ?
Er1 O3 2.296(3) . ?
Er1 O5 2.325(3) . ?
Er1 O4 2.328(3) 2_556 ?
Er1 O1 2.351(3) . ?
Er1 O6 2.356(3) . ?
Er1 O7 2.451(4) . ?
Er1 O8 2.452(4) . ?
Er1 N3 2.868(4) . ?
Cu1 N2 2.075(4) . ?
Cu1 N1 2.084(4) 1_565 ?
Cu1 I1 2.6060(7) . ?
Cu1 I1 2.6341(7) 2_565 ?
Cu1 Cu1 2.6873(11) 2_565 ?
I1 Cu1 2.6341(7) 2_565 ?
O1 C6 1.256(5) . ?
O2 C6 1.250(5) . ?
O2 Er1 2.257(3) 2_556 ?
O3 C12 1.259(5) . ?
O4 C12 1.246(5) . ?
O4 Er1 2.328(3) 2_556 ?
O5 C15 1.243(6) . ?
O6 C18 1.239(6) . ?
O7 N3 1.255(6) . ?
O8 N3 1.248(6) . ?
O9 N3 1.217(6) . ?
O10 C21 1.223(9) . ?
N1 C1 1.330(6) . ?
N1 C5 1.338(6) . ?
N1 Cu1 2.084(4) 1_545 ?
N2 C7 1.333(6) . ?
N2 C11 1.338(6) . ?
N4 C15 1.305(7) . ?
N4 C13 1.454(8) . ?
N4 C14 1.455(8) . ?
N5 C18 1.308(7) . ?
N5 C16 1.455(11) . ?
N5 C17 1.462(8) . ?
N6 C21 1.305(9) . ?
N6 C20 1.433(9) . ?
N6 C19 1.437(9) . ?
C1 C2 1.388(7) . ?
C2 C3 1.385(7) . ?
C3 C4 1.374(7) . ?
C3 C6 1.512(6) . ?
C4 C5 1.381(7) . ?
C7 C8 1.374(7) . ?
C8 C9 1.376(6) . ?
C9 C10 1.379(7) . ?
C9 C12 1.513(6) . ?
C10 C11 1.374(7) . ?
N7 C24 1.326(9) . ?
N7 C23 1.336(14) . ?
N7 C22 1.384(19) . ?
O11 C24 1.155(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
O2 Er1 O3 78.38(11) 2_556 . ?
O2 Er1 O5 147.88(12) 2_556 . ?
O3 Er1 O5 78.19(12) . . ?
O2 Er1 O4 76.99(12) 2_556 2_556 ?
O3 Er1 O4 126.52(11) . 2_556 ?
O5 Er1 O4 135.02(12) . 2_556 ?
O2 Er1 O1 123.81(12) 2_556 . ?
O3 Er1 O1 79.44(11) . . ?
O5 Er1 O1 72.45(12) . . ?
O4 Er1 O1 76.30(12) 2_556 . ?
O2 Er1 O6 77.32(13) 2_556 . ?
O3 Er1 O6 77.10(12) . . ?
O5 Er1 O6 76.27(13) . . ?
O4 Er1 O6 139.67(12) 2_556 . ?
O1 Er1 O6 144.00(12) . . ?
O2 Er1 O7 82.50(13) 2_556 . ?
O3 Er1 O7 146.18(12) . . ?
O5 Er1 O7 105.91(14) . . ?
O4 Er1 O7 74.65(13) 2_556 . ?
O1 Er1 O7 134.22(12) . . ?
O6 Er1 O7 71.61(13) . . ?
O2 Er1 O8 131.39(13) 2_556 . ?
O3 Er1 O8 148.80(13) . . ?
O5 Er1 O8 70.82(13) . . ?
O4 Er1 O8 76.51(13) 2_556 . ?
O1 Er1 O8 87.79(13) . . ?
O6 Er1 O8 98.47(15) . . ?
O7 Er1 O8 51.44(13) . . ?
O2 Er1 N3 107.10(14) 2_556 . ?
O3 Er1 N3 159.72(13) . . ?
O5 Er1 N3 88.47(14) . . ?
O4 Er1 N3 73.60(13) 2_556 . ?
O1 Er1 N3 111.23(13) . . ?
O6 Er1 N3 84.98(14) . . ?
O7 Er1 N3 25.80(14) . . ?
O8 Er1 N3 25.64(14) . . ?
N2 Cu1 N1 100.40(16) . 1_565 ?
N2 Cu1 I1 109.85(11) . . ?
N1 Cu1 I1 109.84(11) 1_565 . ?
N2 Cu1 I1 107.51(11) . 2_565 ?
N1 Cu1 I1 109.43(11) 1_565 2_565 ?
I1 Cu1 I1 118.30(2) . 2_565 ?
N2 Cu1 Cu1 128.62(12) . 2_565 ?
N1 Cu1 Cu1 130.93(12) 1_565 2_565 ?
I1 Cu1 Cu1 59.66(2) . 2_565 ?
I1 Cu1 Cu1 58.63(2) 2_565 2_565 ?
Cu1 I1 Cu1 61.70(2) . 2_565 ?
C6 O1 Er1 114.4(3) . . ?
C6 O2 Er1 176.0(3) . 2_556 ?
C12 O3 Er1 139.2(3) . . ?
C12 O4 Er1 138.3(3) . 2_556 ?
C15 O5 Er1 128.3(3) . . ?
C18 O6 Er1 130.8(3) . . ?
N3 O7 Er1 96.0(3) . . ?
N3 O8 Er1 96.2(3) . . ?
C1 N1 C5 117.0(4) . . ?
C1 N1 Cu1 123.7(3) . 1_545 ?
C5 N1 Cu1 119.2(3) . 1_545 ?
C7 N2 C11 116.6(4) . . ?
C7 N2 Cu1 121.0(3) . . ?
C11 N2 Cu1 121.6(3) . . ?
O9 N3 O8 121.6(6) . . ?
O9 N3 O7 122.0(6) . . ?
O8 N3 O7 116.4(4) . . ?
O9 N3 Er1 179.4(6) . . ?
O8 N3 Er1 58.2(2) . . ?
O7 N3 Er1 58.2(2) . . ?
C15 N4 C13 120.6(5) . . ?
C15 N4 C14 121.6(5) . . ?
C13 N4 C14 117.7(5) . . ?
C18 N5 C16 119.1(6) . . ?
C18 N5 C17 122.3(6) . . ?
C16 N5 C17 118.6(6) . . ?
C21 N6 C20 120.0(6) . . ?
C21 N6 C19 123.0(7) . . ?
C20 N6 C19 117.0(6) . . ?
N1 C1 C2 123.4(4) . . ?
C3 C2 C1 118.7(4) . . ?
C4 C3 C2 118.4(4) . . ?
C4 C3 C6 120.3(4) . . ?
C2 C3 C6 121.3(4) . . ?
C3 C4 C5 119.0(5) . . ?
N1 C5 C4 123.5(5) . . ?
O2 C6 O1 124.1(4) . . ?
O2 C6 C3 117.6(4) . . ?
O1 C6 C3 118.3(4) . . ?
N2 C7 C8 123.5(4) . . ?
C7 C8 C9 119.5(4) . . ?
C8 C9 C10 117.5(4) . . ?
C8 C9 C12 121.8(4) . . ?
C10 C9 C12 120.7(4) . . ?
C11 C10 C9 119.5(5) . . ?
N2 C11 C10 123.3(5) . . ?
O4 C12 O3 127.1(4) . . ?
O4 C12 C9 117.3(4) . . ?
O3 C12 C9 115.6(4) . . ?
O5 C15 N4 124.3(5) . . ?
O6 C18 N5 125.1(6) . . ?
O10 C21 N6 125.8(8) . . ?
C24 N7 C23 116.2(12) . . ?
C24 N7 C22 133.2(13) . . ?
C23 N7 C22 110.6(12) . . ?
O11 C24 N7 133.2(16) . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        24.79
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         1.264
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.108
####################################################################### 
# 
# 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_2
_audit_block_doi                 10.5517/ccdc.csd.cc1mf0vx
_database_code_depnum_ccdc_archive 'CCDC 1502069'
_audit_update_record             
;
2016-09-01 deposited with the CCDC.
2017-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            2-Nd
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H40 Cl0 Cu8 I8 N8 Na2 Nd2 O25'
_chemical_formula_weight         2986.86

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   C222(1)

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

_cell_length_a                   17.889(2)
_cell_length_b                   31.835(4)
_cell_length_c                   24.831(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     14141(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7822
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      23.56

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5528
_exptl_absorpt_coefficient_mu    3.690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36780
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0928
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         26.00
_reflns_number_total             13898
_reflns_number_gt                7752
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1245P)²+189.9995P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         13898
_refine_ls_number_parameters     386
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.1594
_refine_ls_R_factor_gt           0.0853
_refine_ls_wR_factor_ref         0.2635
_refine_ls_wR_factor_gt          0.2168
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.68555(6) -0.10695(3) -0.45493(6) 0.0739(4) Uani 1 1 d . . .
I1 I 0.20926(7) -0.01846(4) -0.33508(8) 0.0776(5) Uani 1 1 d . . .
I2 I 0.30618(8) 0.11143(5) -0.32733(8) 0.0825(5) Uani 1 1 d . . .
I3 I 0.18472(8) 0.07032(4) -0.47942(7) 0.0722(4) Uani 1 1 d . . .
I4 I 0.05507(7) 0.09470(4) -0.32693(7) 0.0700(5) Uani 1 1 d . . .
Cu1 Cu 0.26790(13) 0.05164(9) -0.39377(15) 0.0774(9) Uani 1 1 d . . .
Cu2 Cu 0.18508(17) 0.05902(9) -0.30492(13) 0.0785(9) Uani 1 1 d . . .
Cu3 Cu 0.12662(13) 0.03364(8) -0.39386(15) 0.0780(9) Uani 1 1 d . . .
Cu4 Cu 0.17187(15) 0.11162(7) -0.38624(14) 0.0767(9) Uani 1 1 d . . .
Na1 Na 0.6928(5) 0.0000 -0.5000 0.058(3) Uani 1 2 d S . .
O1 O 0.7664(8) -0.1142(5) -0.5366(8) 0.092(5) Uani 1 1 d . . .
O2 O 0.6792(7) -0.0652(4) -0.5427(6) 0.070(4) Uani 1 1 d . . .
O3 O 0.7726(7) -0.0450(4) -0.4535(7) 0.074(4) Uani 1 1 d . . .
O4 O 0.8221(8) -0.1021(5) -0.4238(8) 0.097(6) Uani 1 1 d . . .
O5 O 0.6177(6) -0.0370(4) -0.4422(7) 0.066(4) Uani 1 1 d . . .
O6 O 0.5472(8) -0.0930(4) -0.4487(8) 0.087(5) Uani 1 1 d . . .
O7 O 0.7379(9) -0.1786(5) -0.4510(9) 0.106(3) Uani 1 1 d . . .
O8 O 0.6307(9) -0.1699(5) -0.4063(9) 0.106(3) Uani 1 1 d . . .
O9 O 0.6894(14) -0.0943(8) -0.3597(9) 0.149(8) Uani 1 1 d U . .
H9A H 0.7303 -0.0822 -0.3516 0.179 Uiso 1 1 d R . .
H9B H 0.6529 -0.0786 -0.3510 0.179 Uiso 1 1 d R . .
O10 O 0.6183(12) -0.1515(7) -0.5243(12) 0.147(10) Uani 1 1 d . . .
H10A H 0.6435 -0.1521 -0.5533 0.177 Uiso 1 1 d R . .
H10D H 0.5755 -0.1410 -0.5305 0.177 Uiso 1 1 d R . .
N1 N 0.8046(7) -0.0599(4) -0.7252(5) 0.085(6) Uani 1 1 d G . .
C1 C 0.8354(7) -0.0932(4) -0.6967(6) 0.090(8) Uani 1 1 d G . .
H1B H 0.8716 -0.1108 -0.7133 0.108 Uiso 1 1 calc R . .
C2 C 0.8134(8) -0.1009(4) -0.6439(6) 0.072(6) Uani 1 1 d G . .
H2A H 0.8345 -0.1236 -0.6245 0.086 Uiso 1 1 calc R . .
C3 C 0.7604(7) -0.0751(5) -0.6196(5) 0.067(6) Uani 1 1 d G . .
C4 C 0.7295(7) -0.0418(4) -0.6481(6) 0.072(6) Uani 1 1 d GU . .
H4A H 0.6934 -0.0242 -0.6315 0.086 Uiso 1 1 calc R . .
C5 C 0.7516(7) -0.0341(4) -0.7009(6) 0.075(6) Uani 1 1 d GU . .
H5A H 0.7305 -0.0114 -0.7203 0.090 Uiso 1 1 calc R . .
N2 N 1.0357(5) 0.0013(3) -0.4158(6) 0.069(6) Uani 1 1 d G . .
C7 C 0.9717(6) 0.0233(3) -0.4305(7) 0.083(8) Uani 1 1 d G . .
H7A H 0.9741 0.0528 -0.4359 0.100 Uiso 1 1 calc R . .
C8 C 0.9044(5) 0.0022(3) -0.4372(7) 0.082(8) Uani 1 1 d G . .
H8A H 0.8607 0.0172 -0.4473 0.098 Uiso 1 1 calc R . .
C9 C 0.9010(5) -0.0410(3) -0.4293(7) 0.065(6) Uani 1 1 d G . .
C10 C 0.9649(6) -0.0630(3) -0.4147(7) 0.083(8) Uani 1 1 d G . .
H10B H 0.9626 -0.0926 -0.4092 0.099 Uiso 1 1 calc R . .
C11 C 1.0323(5) -0.0419(3) -0.4079(6) 0.073(7) Uani 1 1 d G . .
H11A H 1.0760 -0.0569 -0.3979 0.087 Uiso 1 1 calc R . .
N3 N 0.3601(4) 0.0212(4) -0.4168(5) 0.066(5) Uani 1 1 d G . .
C13 C 0.4305(5) 0.0387(3) -0.4093(5) 0.048(5) Uani 1 1 d G . .
H13A H 0.4351 0.0671 -0.3980 0.058 Uiso 1 1 calc R . .
C14 C 0.4942(4) 0.0147(3) -0.4183(5) 0.057(6) Uani 1 1 d G . .
H14A H 0.5423 0.0267 -0.4131 0.068 Uiso 1 1 calc R . .
C15 C 0.4875(5) -0.0268(3) -0.4349(6) 0.046(5) Uani 1 1 d G . .
C16 C 0.4171(6) -0.0444(3) -0.4424(6) 0.071(7) Uani 1 1 d G . .
H16A H 0.4125 -0.0728 -0.4537 0.086 Uiso 1 1 calc R . .
C17 C 0.3534(4) -0.0204(4) -0.4334(6) 0.078(8) Uani 1 1 d G . .
H17A H 0.3053 -0.0323 -0.4385 0.094 Uiso 1 1 calc R . .
N4 N 0.6670(7) -0.3270(3) -0.4052(7) 0.072(5) Uani 1 1 d G . .
C19 C 0.7236(8) -0.3102(4) -0.4369(7) 0.106(3) Uani 1 1 d G . .
H19A H 0.7588 -0.3282 -0.4537 0.127 Uiso 1 1 calc R . .
C20 C 0.7287(8) -0.2670(4) -0.4439(8) 0.106(3) Uani 1 1 d G . .
H20A H 0.7674 -0.2555 -0.4655 0.127 Uiso 1 1 calc R . .
C21 C 0.6772(9) -0.2405(3) -0.4192(9) 0.106(3) Uani 1 1 d G . .
C22 C 0.6205(9) -0.2574(4) -0.3875(8) 0.106(3) Uani 1 1 d G . .
H22A H 0.5853 -0.2393 -0.3707 0.127 Uiso 1 1 calc R . .
C23 C 0.6154(7) -0.3006(4) -0.3805(7) 0.106(3) Uani 1 1 d G . .
H23A H 0.5767 -0.3121 -0.3588 0.127 Uiso 1 1 calc R . .
C6 C 0.7354(11) -0.0858(6) -0.5666(14) 0.090(9) Uani 1 1 d . . .
C12 C 0.8266(10) -0.0661(7) -0.4350(9) 0.065(6) Uani 1 1 d . . .
C18 C 0.5552(10) -0.0560(7) -0.4412(9) 0.060(6) Uani 1 1 d . . .
C24 C 0.6844(16) -0.1924(7) -0.4240(14) 0.106(3) Uani 1 1 d U . .
Na2 Na 0.4913(16) -0.1504(7) -0.3855(12) 0.124(8) Uani 0.50 1 d PU . .
O1W O 0.557(4) 0.134(2) 0.622(3) 0.21(3) Uani 0.50 1 d PU . .
O2W O 0.5000 0.014(3) 0.7500 0.33(4) Uani 1 2 d SU . .
O3W O 0.0000 0.024(3) 0.2500 0.42(6) Uani 1 2 d SU . .
O4W O 0.409(4) 0.152(2) 0.524(3) 0.21(3) Uani 0.50 1 d PU . .
O1W' O 0.558(3) 0.1328(16) 0.668(2) 0.133(15) Uani 0.50 1 d PU . .


_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
Nd1 O9 2.40(2) . ?
Nd1 O7 2.469(15) . ?
Nd1 O1 2.501(17) . ?
Nd1 O3 2.513(13) . ?
Nd1 O6 2.518(14) . ?
Nd1 O10 2.53(2) . ?
Nd1 O8 2.538(16) . ?
Nd1 O2 2.555(15) . ?
Nd1 O5 2.555(12) . ?
Nd1 O4 2.567(15) . ?
Nd1 C24 2.83(2) . ?
Nd1 C18 2.860(17) . ?
I1 Cu2 2.614(3) . ?
I1 Cu3 2.658(3) . ?
I1 Cu1 2.864(4) . ?
I2 Cu1 2.610(3) . ?
I2 Cu2 2.790(3) . ?
I2 Cu4 2.813(4) . ?
I3 Cu3 2.638(4) . ?
I3 Cu1 2.663(4) . ?
I3 Cu4 2.671(4) . ?
I4 Cu4 2.612(3) . ?
I4 Cu2 2.646(3) . ?
I4 Cu3 2.860(4) . ?
Cu1 N3 1.997(8) . ?
Cu1 Cu4 2.575(3) . ?
Cu1 Cu3 2.591(3) . ?
Cu1 Cu2 2.668(4) . ?
Cu2 N1 1.989(13) 2_655 ?
Cu2 Cu3 2.574(5) . ?
Cu2 Cu4 2.634(4) . ?
Cu3 N2 2.002(8) 1_455 ?
Cu3 Cu4 2.618(4) . ?
Cu4 N4 2.012(10) 5_455 ?
Na1 O5 2.293(15) . ?
Na1 O5 2.293(15) 3_554 ?
Na1 O3 2.328(15) . ?
Na1 O3 2.328(15) 3_554 ?
Na1 O2 2.342(14) . ?
Na1 O2 2.342(14) 3_554 ?
Na1 Nd1 3.5862(11) 3_554 ?
O1 C6 1.30(3) . ?
O2 C6 1.34(3) . ?
O3 C12 1.26(2) . ?
O4 C12 1.18(2) . ?
O5 C18 1.27(2) . ?
O6 C18 1.20(2) . ?
O6 Na2 2.61(3) . ?
O7 C24 1.25(3) . ?
O8 C24 1.28(3) . ?
O8 Na2 2.62(3) . ?
O9 H9A 0.8501 . ?
O9 H9B 0.8502 . ?
O10 H10A 0.8502 . ?
O10 H10D 0.8500 . ?
N1 C1 1.3900 . ?
N1 C5 1.3900 . ?
N1 Cu2 1.989(13) 2_654 ?
C1 C2 1.3900 . ?
C1 H1B 0.9500 . ?
C2 C3 1.3900 . ?
C2 H2A 0.9500 . ?
C3 C4 1.3900 . ?
C3 C6 1.43(3) . ?
C4 C5 1.3900 . ?
C4 H4A 0.9500 . ?
C5 H5A 0.9500 . ?
N2 C7 1.3900 . ?
N2 C11 1.3900 . ?
N2 Cu3 2.002(8) 1_655 ?
C7 C8 1.3900 . ?
C7 H7A 0.9500 . ?
C8 C9 1.3900 . ?
C8 H8A 0.9500 . ?
C9 C10 1.3900 . ?
C9 C12 1.56(2) . ?
C10 C11 1.3900 . ?
C10 H10B 0.9500 . ?
C11 H11A 0.9500 . ?
N3 C13 1.3900 . ?
N3 C17 1.3900 . ?
C13 C14 1.3900 . ?
C13 H13A 0.9500 . ?
C14 C15 1.3900 . ?
C14 H14A 0.9500 . ?
C15 C16 1.3900 . ?
C15 C18 1.535(18) . ?
C16 C17 1.3900 . ?
C16 H16A 0.9500 . ?
C17 H17A 0.9500 . ?
N4 C19 1.3900 . ?
N4 C23 1.3900 . ?
N4 Cu4 2.012(10) 5_545 ?
C19 C20 1.3900 . ?
C19 H19A 0.9500 . ?
C20 C21 1.3900 . ?
C20 H20A 0.9500 . ?
C21 C22 1.3900 . ?
C21 C24 1.54(3) . ?
C22 C23 1.3900 . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
O1W O1W' 1.15(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
O9 Nd1 O7 96.0(8) . . ?
O9 Nd1 O1 142.9(7) . . ?
O7 Nd1 O1 74.1(6) . . ?
O9 Nd1 O3 80.6(7) . . ?
O7 Nd1 O3 119.3(5) . . ?
O1 Nd1 O3 74.1(6) . . ?
O9 Nd1 O6 86.5(8) . . ?
O7 Nd1 O6 122.2(5) . . ?
O1 Nd1 O6 129.4(6) . . ?
O3 Nd1 O6 118.0(4) . . ?
O9 Nd1 O10 141.0(9) . . ?
O7 Nd1 O10 71.9(7) . . ?
O1 Nd1 O10 70.8(8) . . ?
O3 Nd1 O10 138.0(7) . . ?
O6 Nd1 O10 71.0(7) . . ?
O9 Nd1 O8 71.0(8) . . ?
O7 Nd1 O8 53.0(5) . . ?
O1 Nd1 O8 122.4(6) . . ?
O3 Nd1 O8 148.5(7) . . ?
O6 Nd1 O8 74.3(5) . . ?
O10 Nd1 O8 72.4(8) . . ?
O9 Nd1 O2 139.0(7) . . ?
O7 Nd1 O2 122.1(6) . . ?
O1 Nd1 O2 51.9(5) . . ?
O3 Nd1 O2 68.3(5) . . ?
O6 Nd1 O2 85.3(5) . . ?
O10 Nd1 O2 72.0(7) . . ?
O8 Nd1 O2 143.1(6) . . ?
O9 Nd1 O5 75.3(7) . . ?
O7 Nd1 O5 168.7(6) . . ?
O1 Nd1 O5 117.1(5) . . ?
O3 Nd1 O5 67.0(4) . . ?
O6 Nd1 O5 51.1(4) . . ?
O10 Nd1 O5 110.2(6) . . ?
O8 Nd1 O5 116.4(5) . . ?
O2 Nd1 O5 68.4(5) . . ?
O9 Nd1 O4 70.5(8) . . ?
O7 Nd1 O4 71.5(6) . . ?
O1 Nd1 O4 72.5(6) . . ?
O3 Nd1 O4 50.1(4) . . ?
O6 Nd1 O4 155.0(6) . . ?
O10 Nd1 O4 133.6(7) . . ?
O8 Nd1 O4 105.8(6) . . ?
O2 Nd1 O4 105.5(5) . . ?
O5 Nd1 O4 111.3(5) . . ?
O9 Nd1 C24 83.9(9) . . ?
O7 Nd1 C24 26.1(6) . . ?
O1 Nd1 C24 97.7(7) . . ?
O3 Nd1 C24 139.1(7) . . ?
O6 Nd1 C24 98.4(6) . . ?
O10 Nd1 C24 69.1(9) . . ?
O8 Nd1 C24 26.9(6) . . ?
O2 Nd1 C24 137.1(8) . . ?
O5 Nd1 C24 143.3(6) . . ?
O4 Nd1 C24 89.0(7) . . ?
O9 Nd1 C18 79.1(8) . . ?
O7 Nd1 C18 145.9(6) . . ?
O1 Nd1 C18 128.4(6) . . ?
O3 Nd1 C18 93.3(5) . . ?
O6 Nd1 C18 24.8(5) . . ?
O10 Nd1 C18 90.6(7) . . ?
O8 Nd1 C18 94.3(6) . . ?
O2 Nd1 C18 76.7(5) . . ?
O5 Nd1 C18 26.4(5) . . ?
O4 Nd1 C18 134.9(6) . . ?
C24 Nd1 C18 120.5(7) . . ?
Cu2 I1 Cu3 58.43(10) . . ?
Cu2 I1 Cu1 58.07(9) . . ?
Cu3 I1 Cu1 55.82(8) . . ?
Cu1 I2 Cu2 59.09(10) . . ?
Cu1 I2 Cu4 56.55(8) . . ?
Cu2 I2 Cu4 56.08(9) . . ?
Cu3 I3 Cu1 58.54(9) . . ?
Cu3 I3 Cu4 59.09(9) . . ?
Cu1 I3 Cu4 57.74(9) . . ?
Cu4 I4 Cu2 60.12(10) . . ?
Cu4 I4 Cu3 56.95(8) . . ?
Cu2 I4 Cu3 55.58(9) . . ?
N3 Cu1 Cu4 158.7(4) . . ?
N3 Cu1 Cu3 134.3(3) . . ?
Cu4 Cu1 Cu3 60.89(10) . . ?
N3 Cu1 I2 108.6(3) . . ?
Cu4 Cu1 I2 65.70(11) . . ?
Cu3 Cu1 I2 114.68(13) . . ?
N3 Cu1 I3 109.9(4) . . ?
Cu4 Cu1 I3 61.29(11) . . ?
Cu3 Cu1 I3 60.25(11) . . ?
I2 Cu1 I3 119.24(12) . . ?
N3 Cu1 Cu2 137.6(5) . . ?
Cu4 Cu1 Cu2 60.28(11) . . ?
Cu3 Cu1 Cu2 58.57(12) . . ?
I2 Cu1 Cu2 63.82(11) . . ?
I3 Cu1 Cu2 109.30(11) . . ?
N3 Cu1 I1 94.0(4) . . ?
Cu4 Cu1 I1 107.25(11) . . ?
Cu3 Cu1 I1 58.06(9) . . ?
I2 Cu1 I1 110.04(14) . . ?
I3 Cu1 I1 112.07(10) . . ?
Cu2 Cu1 I1 56.25(10) . . ?
N1 Cu2 Cu3 153.7(4) 2_655 . ?
N1 Cu2 I1 106.4(4) 2_655 . ?
Cu3 Cu2 I1 61.65(10) . . ?
N1 Cu2 Cu4 139.7(4) 2_655 . ?
Cu3 Cu2 Cu4 60.35(11) . . ?
I1 Cu2 Cu4 113.28(14) . . ?
N1 Cu2 I4 106.4(4) 2_655 . ?
Cu3 Cu2 I4 66.43(10) . . ?
I1 Cu2 I4 119.44(14) . . ?
Cu4 Cu2 I4 59.32(9) . . ?
N1 Cu2 Cu1 140.6(4) 2_655 . ?
Cu3 Cu2 Cu1 59.23(11) . . ?
I1 Cu2 Cu1 65.67(10) . . ?
Cu4 Cu2 Cu1 58.12(11) . . ?
I4 Cu2 Cu1 110.80(13) . . ?
N1 Cu2 I2 96.8(4) 2_655 . ?
Cu3 Cu2 I2 109.39(13) . . ?
I1 Cu2 I2 112.25(11) . . ?
Cu4 Cu2 I2 62.39(10) . . ?
I4 Cu2 I2 112.61(11) . . ?
Cu1 Cu2 I2 57.08(9) . . ?
N2 Cu3 Cu2 136.5(5) 1_455 . ?
N2 Cu3 Cu1 155.1(4) 1_455 . ?
Cu2 Cu3 Cu1 62.19(12) . . ?
N2 Cu3 Cu4 139.4(3) 1_455 . ?
Cu2 Cu3 Cu4 60.97(12) . . ?
Cu1 Cu3 Cu4 59.25(10) . . ?
N2 Cu3 I3 109.2(5) 1_455 . ?
Cu2 Cu3 I3 113.08(12) . . ?
Cu1 Cu3 I3 61.22(11) . . ?
Cu4 Cu3 I3 61.09(10) . . ?
N2 Cu3 I1 106.3(4) 1_455 . ?
Cu2 Cu3 I1 59.92(10) . . ?
Cu1 Cu3 I1 66.11(10) . . ?
Cu4 Cu3 I1 112.33(13) . . ?
I3 Cu3 I1 119.95(11) . . ?
N2 Cu3 I4 98.3(4) 1_455 . ?
Cu2 Cu3 I4 57.99(10) . . ?
Cu1 Cu3 I4 106.60(12) . . ?
Cu4 Cu3 I4 56.76(9) . . ?
I3 Cu3 I4 110.09(10) . . ?
I1 Cu3 I4 110.73(14) . . ?
N4 Cu4 Cu1 137.1(4) 5_455 . ?
N4 Cu4 I4 107.3(4) 5_455 . ?
Cu1 Cu4 I4 114.93(12) . . ?
N4 Cu4 Cu3 153.0(5) 5_455 . ?
Cu1 Cu4 Cu3 59.86(10) . . ?
I4 Cu4 Cu3 66.29(10) . . ?
N4 Cu4 Cu2 143.2(5) 5_455 . ?
Cu1 Cu4 Cu2 61.60(12) . . ?
I4 Cu4 Cu2 60.56(9) . . ?
Cu3 Cu4 Cu2 58.68(12) . . ?
N4 Cu4 I3 106.2(5) 5_455 . ?
Cu1 Cu4 I3 60.97(10) . . ?
I4 Cu4 I3 117.11(12) . . ?
Cu3 Cu4 I3 59.82(11) . . ?
Cu2 Cu4 I3 110.08(11) . . ?
N4 Cu4 I2 99.3(5) 5_455 . ?
Cu1 Cu4 I2 57.75(9) . . ?
I4 Cu4 I2 112.93(13) . . ?
Cu3 Cu4 I2 107.44(11) . . ?
Cu2 Cu4 I2 61.53(10) . . ?
I3 Cu4 I2 112.08(9) . . ?
O5 Na1 O5 108.2(8) . 3_554 ?
O5 Na1 O3 74.5(5) . . ?
O5 Na1 O3 170.4(6) 3_554 . ?
O5 Na1 O3 170.4(6) . 3_554 ?
O5 Na1 O3 74.5(5) 3_554 3_554 ?
O3 Na1 O3 104.4(8) . 3_554 ?
O5 Na1 O2 76.5(5) . . ?
O5 Na1 O2 96.4(5) 3_554 . ?
O3 Na1 O2 75.1(5) . . ?
O3 Na1 O2 112.6(6) 3_554 . ?
O5 Na1 O2 96.4(5) . 3_554 ?
O5 Na1 O2 76.5(5) 3_554 3_554 ?
O3 Na1 O2 112.6(6) . 3_554 ?
O3 Na1 O2 75.1(5) 3_554 3_554 ?
O2 Na1 O2 168.1(7) . 3_554 ?
O5 Na1 Nd1 45.2(3) . . ?
O5 Na1 Nd1 131.5(4) 3_554 . ?
O3 Na1 Nd1 44.2(3) . . ?
O3 Na1 Nd1 139.6(4) 3_554 . ?
O2 Na1 Nd1 45.3(4) . . ?
O2 Na1 Nd1 134.1(4) 3_554 . ?
O5 Na1 Nd1 131.5(4) . 3_554 ?
O5 Na1 Nd1 45.2(3) 3_554 3_554 ?
O3 Na1 Nd1 139.6(4) . 3_554 ?
O3 Na1 Nd1 44.2(3) 3_554 3_554 ?
O2 Na1 Nd1 134.1(4) . 3_554 ?
O2 Na1 Nd1 45.3(4) 3_554 3_554 ?
Nd1 Na1 Nd1 175.8(3) . 3_554 ?
C6 O1 Nd1 98.8(15) . . ?
C6 O2 Na1 123.8(13) . . ?
C6 O2 Nd1 95.2(14) . . ?
Na1 O2 Nd1 94.1(5) . . ?
C12 O3 Na1 167.5(13) . . ?
C12 O3 Nd1 93.6(12) . . ?
Na1 O3 Nd1 95.5(5) . . ?
C12 O4 Nd1 93.0(12) . . ?
C18 O5 Na1 140.5(15) . . ?
C18 O5 Nd1 90.3(11) . . ?
Na1 O5 Nd1 95.3(5) . . ?
C18 O6 Nd1 93.7(11) . . ?
C18 O6 Na2 129.8(17) . . ?
Nd1 O6 Na2 106.9(8) . . ?
C24 O7 Nd1 93.2(14) . . ?
C24 O8 Nd1 89.3(13) . . ?
C24 O8 Na2 156(2) . . ?
Nd1 O8 Na2 106.0(7) . . ?
Nd1 O9 H9A 109.5 . . ?
Nd1 O9 H9B 109.1 . . ?
H9A O9 H9B 109.5 . . ?
Nd1 O10 H10A 109.8 . . ?
Nd1 O10 H10D 109.3 . . ?
H10A O10 H10D 109.5 . . ?
C1 N1 C5 120.0 . . ?
C1 N1 Cu2 118.7(7) . 2_654 ?
C5 N1 Cu2 119.2(7) . 2_654 ?
C2 C1 N1 120.0 . . ?
C2 C1 H1B 120.0 . . ?
N1 C1 H1B 120.0 . . ?
C1 C2 C3 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C3 C2 H2A 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 C6 121.6(11) . . ?
C2 C3 C6 118.2(12) . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C5 C4 H4A 120.0 . . ?
C4 C5 N1 120.0 . . ?
C4 C5 H5A 120.0 . . ?
N1 C5 H5A 120.0 . . ?
C7 N2 C11 120.0 . . ?
C7 N2 Cu3 118.7(6) . 1_655 ?
C11 N2 Cu3 120.4(6) . 1_655 ?
C8 C7 N2 120.0 . . ?
C8 C7 H7A 120.0 . . ?
N2 C7 H7A 120.0 . . ?
C7 C8 C9 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C9 C8 H8A 120.0 . . ?
C8 C9 C10 120.0 . . ?
C8 C9 C12 122.1(10) . . ?
C10 C9 C12 117.9(10) . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10B 120.0 . . ?
C9 C10 H10B 120.0 . . ?
C10 C11 N2 120.0 . . ?
C10 C11 H11A 120.0 . . ?
N2 C11 H11A 120.0 . . ?
C13 N3 C17 120.0 . . ?
C13 N3 Cu1 121.0(6) . . ?
C17 N3 Cu1 118.4(6) . . ?
C14 C13 N3 120.0 . . ?
C14 C13 H13A 120.0 . . ?
N3 C13 H13A 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 H14A 120.0 . . ?
C15 C14 H14A 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 C18 117.3(11) . . ?
C14 C15 C18 122.5(11) . . ?
C15 C16 C17 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C17 C16 H16A 120.0 . . ?
C16 C17 N3 120.0 . . ?
C16 C17 H17A 120.0 . . ?
N3 C17 H17A 120.0 . . ?
C19 N4 C23 120.0 . . ?
C19 N4 Cu4 118.3(6) . 5_545 ?
C23 N4 Cu4 120.9(7) . 5_545 ?
N4 C19 C20 120.0 . . ?
N4 C19 H19A 120.0 . . ?
C20 C19 H19A 120.0 . . ?
C19 C20 C21 120.0 . . ?
C19 C20 H20A 120.0 . . ?
C21 C20 H20A 120.0 . . ?
C20 C21 C22 120.0 . . ?
C20 C21 C24 120.7(13) . . ?
C22 C21 C24 119.2(13) . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22A 120.0 . . ?
C21 C22 H22A 120.0 . . ?
C22 C23 N4 120.0 . . ?
C22 C23 H23A 120.0 . . ?
N4 C23 H23A 120.0 . . ?
O1 C6 O2 114(3) . . ?
O1 C6 C3 124.0(19) . . ?
O2 C6 C3 121.8(19) . . ?
O1 C6 Nd1 55.8(14) . . ?
O2 C6 Nd1 58.3(14) . . ?
C3 C6 Nd1 178.8(17) . . ?
O4 C12 O3 123.2(19) . . ?
O4 C12 C9 122.3(16) . . ?
O3 C12 C9 114.5(16) . . ?
O4 C12 Nd1 62.8(12) . . ?
O3 C12 Nd1 60.5(10) . . ?
C9 C12 Nd1 174.0(13) . . ?
O6 C18 O5 124.7(16) . . ?
O6 C18 C15 121.0(17) . . ?
O5 C18 C15 114.1(17) . . ?
O6 C18 Nd1 61.5(10) . . ?
O5 C18 Nd1 63.3(9) . . ?
C15 C18 Nd1 177.2(13) . . ?
O7 C24 O8 124(2) . . ?
O7 C24 C21 117(2) . . ?
O8 C24 C21 118(2) . . ?
O7 C24 Nd1 60.7(11) . . ?
O8 C24 Nd1 63.8(11) . . ?
C21 C24 Nd1 168(2) . . ?
O6 Na2 O8 71.5(8) . . ?
O6 Na2 Nd1 35.8(5) . . ?
O8 Na2 Nd1 36.3(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu2 I2 Cu1 N3 -134.7(5) . . . . ?
Cu4 I2 Cu1 N3 157.9(5) . . . . ?
Cu2 I2 Cu1 Cu4 67.41(10) . . . . ?
Cu2 I2 Cu1 Cu3 30.08(14) . . . . ?
Cu4 I2 Cu1 Cu3 -37.33(14) . . . . ?
Cu2 I2 Cu1 I3 98.45(13) . . . . ?
Cu4 I2 Cu1 I3 31.03(10) . . . . ?
Cu4 I2 Cu1 Cu2 -67.41(10) . . . . ?
Cu2 I2 Cu1 I1 -33.05(9) . . . . ?
Cu4 I2 Cu1 I1 -100.46(11) . . . . ?
Cu3 I3 Cu1 N3 130.4(4) . . . . ?
Cu4 I3 Cu1 N3 -158.6(4) . . . . ?
Cu3 I3 Cu1 Cu4 -70.98(11) . . . . ?
Cu4 I3 Cu1 Cu3 70.98(11) . . . . ?
Cu3 I3 Cu1 I2 -103.37(15) . . . . ?
Cu4 I3 Cu1 I2 -32.39(11) . . . . ?
Cu3 I3 Cu1 Cu2 -33.22(12) . . . . ?
Cu4 I3 Cu1 Cu2 37.76(11) . . . . ?
Cu3 I3 Cu1 I1 27.23(10) . . . . ?
Cu4 I3 Cu1 I1 98.21(12) . . . . ?
Cu2 I1 Cu1 N3 147.5(4) . . . . ?
Cu3 I1 Cu1 N3 -141.3(4) . . . . ?
Cu2 I1 Cu1 Cu4 -33.73(14) . . . . ?
Cu3 I1 Cu1 Cu4 37.45(14) . . . . ?
Cu2 I1 Cu1 Cu3 -71.19(13) . . . . ?
Cu2 I1 Cu1 I2 36.06(11) . . . . ?
Cu3 I1 Cu1 I2 107.24(13) . . . . ?
Cu2 I1 Cu1 I3 -99.10(13) . . . . ?
Cu3 I1 Cu1 I3 -27.91(12) . . . . ?
Cu3 I1 Cu1 Cu2 71.19(13) . . . . ?
Cu3 I1 Cu2 N1 154.5(4) . . . 2_655 ?
Cu1 I1 Cu2 N1 -138.7(4) . . . 2_655 ?
Cu1 I1 Cu2 Cu3 66.80(11) . . . . ?
Cu3 I1 Cu2 Cu4 -32.43(12) . . . . ?
Cu1 I1 Cu2 Cu4 34.37(12) . . . . ?
Cu3 I1 Cu2 I4 34.30(13) . . . . ?
Cu1 I1 Cu2 I4 101.09(15) . . . . ?
Cu3 I1 Cu2 Cu1 -66.80(11) . . . . ?
Cu3 I1 Cu2 I2 -100.77(14) . . . . ?
Cu1 I1 Cu2 I2 -33.98(11) . . . . ?
Cu4 I4 Cu2 N1 138.6(5) . . . 2_655 ?
Cu3 I4 Cu2 N1 -153.0(5) . . . 2_655 ?
Cu4 I4 Cu2 Cu3 -68.36(11) . . . . ?
Cu4 I4 Cu2 I1 -101.11(16) . . . . ?
Cu3 I4 Cu2 I1 -32.75(12) . . . . ?
Cu3 I4 Cu2 Cu4 68.36(11) . . . . ?
Cu4 I4 Cu2 Cu1 -28.06(12) . . . . ?
Cu3 I4 Cu2 Cu1 40.29(12) . . . . ?
Cu4 I4 Cu2 I2 33.81(12) . . . . ?
Cu3 I4 Cu2 I2 102.17(14) . . . . ?
N3 Cu1 Cu2 N1 33.8(9) . . . 2_655 ?
Cu4 Cu1 Cu2 N1 -131.2(7) . . . 2_655 ?
Cu3 Cu1 Cu2 N1 156.8(7) . . . 2_655 ?
I2 Cu1 Cu2 N1 -55.5(7) . . . 2_655 ?
I3 Cu1 Cu2 N1 -169.4(6) . . . 2_655 ?
I1 Cu1 Cu2 N1 86.5(7) . . . 2_655 ?
N3 Cu1 Cu2 Cu3 -122.9(5) . . . . ?
Cu4 Cu1 Cu2 Cu3 72.07(12) . . . . ?
I2 Cu1 Cu2 Cu3 147.75(13) . . . . ?
I3 Cu1 Cu2 Cu3 33.88(11) . . . . ?
I1 Cu1 Cu2 Cu3 -70.29(10) . . . . ?
N3 Cu1 Cu2 I1 -52.7(5) . . . . ?
Cu4 Cu1 Cu2 I1 142.36(14) . . . . ?
Cu3 Cu1 Cu2 I1 70.29(10) . . . . ?
I2 Cu1 Cu2 I1 -141.97(11) . . . . ?
I3 Cu1 Cu2 I1 104.17(12) . . . . ?
N3 Cu1 Cu2 Cu4 165.0(5) . . . . ?
Cu3 Cu1 Cu2 Cu4 -72.07(12) . . . . ?
I2 Cu1 Cu2 Cu4 75.67(11) . . . . ?
I3 Cu1 Cu2 Cu4 -38.19(12) . . . . ?
I1 Cu1 Cu2 Cu4 -142.36(14) . . . . ?
N3 Cu1 Cu2 I4 -166.6(5) . . . . ?
Cu4 Cu1 Cu2 I4 28.45(12) . . . . ?
Cu3 Cu1 Cu2 I4 -43.62(12) . . . . ?
I2 Cu1 Cu2 I4 104.12(12) . . . . ?
I3 Cu1 Cu2 I4 -9.74(17) . . . . ?
I1 Cu1 Cu2 I4 -113.91(14) . . . . ?
N3 Cu1 Cu2 I2 89.3(5) . . . . ?
Cu4 Cu1 Cu2 I2 -75.67(11) . . . . ?
Cu3 Cu1 Cu2 I2 -147.75(13) . . . . ?
I3 Cu1 Cu2 I2 -113.87(13) . . . . ?
I1 Cu1 Cu2 I2 141.97(11) . . . . ?
Cu1 I2 Cu2 N1 148.2(4) . . . 2_655 ?
Cu4 I2 Cu2 N1 -143.6(4) . . . 2_655 ?
Cu1 I2 Cu2 Cu3 -29.09(12) . . . . ?
Cu4 I2 Cu2 Cu3 39.10(11) . . . . ?
Cu1 I2 Cu2 I1 37.34(12) . . . . ?
Cu4 I2 Cu2 I1 105.54(15) . . . . ?
Cu1 I2 Cu2 Cu4 -68.19(12) . . . . ?
Cu1 I2 Cu2 I4 -100.88(15) . . . . ?
Cu4 I2 Cu2 I4 -32.68(11) . . . . ?
Cu4 I2 Cu2 Cu1 68.19(12) . . . . ?
N1 Cu2 Cu3 N2 13.5(10) 2_655 . . 1_455 ?
I1 Cu2 Cu3 N2 82.0(5) . . . 1_455 ?
Cu4 Cu2 Cu3 N2 -132.6(5) . . . 1_455 ?
I4 Cu2 Cu3 N2 -65.7(5) . . . 1_455 ?
Cu1 Cu2 Cu3 N2 159.1(5) . . . 1_455 ?
I2 Cu2 Cu3 N2 -172.6(5) . . . 1_455 ?
N1 Cu2 Cu3 Cu1 -145.6(9) 2_655 . . . ?
I1 Cu2 Cu3 Cu1 -77.08(10) . . . . ?
Cu4 Cu2 Cu3 Cu1 68.38(11) . . . . ?
I4 Cu2 Cu3 Cu1 135.29(12) . . . . ?
I2 Cu2 Cu3 Cu1 28.36(11) . . . . ?
N1 Cu2 Cu3 Cu4 146.0(9) 2_655 . . . ?
I1 Cu2 Cu3 Cu4 -145.47(12) . . . . ?
I4 Cu2 Cu3 Cu4 66.90(8) . . . . ?
Cu1 Cu2 Cu3 Cu4 -68.38(11) . . . . ?
I2 Cu2 Cu3 Cu4 -40.03(10) . . . . ?
N1 Cu2 Cu3 I3 179.1(8) 2_655 . . . ?
I1 Cu2 Cu3 I3 -112.35(12) . . . . ?
Cu4 Cu2 Cu3 I3 33.12(11) . . . . ?
I4 Cu2 Cu3 I3 100.02(11) . . . . ?
Cu1 Cu2 Cu3 I3 -35.27(12) . . . . ?
I2 Cu2 Cu3 I3 -6.91(16) . . . . ?
N1 Cu2 Cu3 I1 -68.5(8) 2_655 . . . ?
Cu4 Cu2 Cu3 I1 145.47(12) . . . . ?
I4 Cu2 Cu3 I1 -147.63(11) . . . . ?
Cu1 Cu2 Cu3 I1 77.08(10) . . . . ?
I2 Cu2 Cu3 I1 105.44(11) . . . . ?
N1 Cu2 Cu3 I4 79.1(8) 2_655 . . . ?
I1 Cu2 Cu3 I4 147.63(11) . . . . ?
Cu4 Cu2 Cu3 I4 -66.90(8) . . . . ?
Cu1 Cu2 Cu3 I4 -135.29(12) . . . . ?
I2 Cu2 Cu3 I4 -106.93(11) . . . . ?
N3 Cu1 Cu3 N2 -16.5(13) . . . 1_455 ?
Cu4 Cu1 Cu3 N2 144.6(10) . . . 1_455 ?
I2 Cu1 Cu3 N2 -176.1(10) . . . 1_455 ?
I3 Cu1 Cu3 N2 73.0(10) . . . 1_455 ?
Cu2 Cu1 Cu3 N2 -144.3(10) . . . 1_455 ?
I1 Cu1 Cu3 N2 -77.0(10) . . . 1_455 ?
N3 Cu1 Cu3 Cu2 127.8(6) . . . . ?
Cu4 Cu1 Cu3 Cu2 -71.06(13) . . . . ?
I2 Cu1 Cu3 Cu2 -31.81(14) . . . . ?
I3 Cu1 Cu3 Cu2 -142.70(12) . . . . ?
I1 Cu1 Cu3 Cu2 67.28(11) . . . . ?
N3 Cu1 Cu3 Cu4 -161.1(6) . . . . ?
I2 Cu1 Cu3 Cu4 39.25(15) . . . . ?
I3 Cu1 Cu3 Cu4 -71.64(11) . . . . ?
Cu2 Cu1 Cu3 Cu4 71.06(13) . . . . ?
I1 Cu1 Cu3 Cu4 138.34(15) . . . . ?
N3 Cu1 Cu3 I3 -89.5(6) . . . . ?
Cu4 Cu1 Cu3 I3 71.64(11) . . . . ?
I2 Cu1 Cu3 I3 110.89(15) . . . . ?
Cu2 Cu1 Cu3 I3 142.70(12) . . . . ?
I1 Cu1 Cu3 I3 -150.02(12) . . . . ?
N3 Cu1 Cu3 I1 60.5(6) . . . . ?
Cu4 Cu1 Cu3 I1 -138.34(15) . . . . ?
I2 Cu1 Cu3 I1 -99.09(16) . . . . ?
I3 Cu1 Cu3 I1 150.02(12) . . . . ?
Cu2 Cu1 Cu3 I1 -67.28(11) . . . . ?
N3 Cu1 Cu3 I4 166.3(6) . . . . ?
Cu4 Cu1 Cu3 I4 -32.55(13) . . . . ?
I2 Cu1 Cu3 I4 6.7(2) . . . . ?
I3 Cu1 Cu3 I4 -104.20(11) . . . . ?
Cu2 Cu1 Cu3 I4 38.50(12) . . . . ?
I1 Cu1 Cu3 I4 105.78(14) . . . . ?
Cu1 I3 Cu3 N2 -154.7(4) . . . 1_455 ?
Cu4 I3 Cu3 N2 136.6(4) . . . 1_455 ?
Cu1 I3 Cu3 Cu2 35.64(12) . . . . ?
Cu4 I3 Cu3 Cu2 -33.07(12) . . . . ?
Cu4 I3 Cu3 Cu1 -68.71(11) . . . . ?
Cu1 I3 Cu3 Cu4 68.71(11) . . . . ?
Cu1 I3 Cu3 I1 -31.82(12) . . . . ?
Cu4 I3 Cu3 I1 -100.54(15) . . . . ?
Cu1 I3 Cu3 I4 98.40(13) . . . . ?
Cu4 I3 Cu3 I4 29.69(10) . . . . ?
Cu2 I1 Cu3 N2 -134.8(4) . . . 1_455 ?
Cu1 I1 Cu3 N2 154.7(5) . . . 1_455 ?
Cu1 I1 Cu3 Cu2 -70.54(12) . . . . ?
Cu2 I1 Cu3 Cu1 70.54(12) . . . . ?
Cu2 I1 Cu3 Cu4 32.40(14) . . . . ?
Cu1 I1 Cu3 Cu4 -38.14(13) . . . . ?
Cu2 I1 Cu3 I3 100.90(15) . . . . ?
Cu1 I1 Cu3 I3 30.36(12) . . . . ?
Cu2 I1 Cu3 I4 -29.04(10) . . . . ?
Cu1 I1 Cu3 I4 -99.58(12) . . . . ?
Cu4 I4 Cu3 N2 -145.2(4) . . . 1_455 ?
Cu2 I4 Cu3 N2 140.7(4) . . . 1_455 ?
Cu4 I4 Cu3 Cu2 74.06(13) . . . . ?
Cu4 I4 Cu3 Cu1 33.57(14) . . . . ?
Cu2 I4 Cu3 Cu1 -40.50(14) . . . . ?
Cu2 I4 Cu3 Cu4 -74.06(13) . . . . ?
Cu4 I4 Cu3 I3 -31.23(11) . . . . ?
Cu2 I4 Cu3 I3 -105.29(12) . . . . ?
Cu4 I4 Cu3 I1 103.75(13) . . . . ?
Cu2 I4 Cu3 I1 29.69(10) . . . . ?
N3 Cu1 Cu4 N4 -12.2(14) . . . 5_455 ?
Cu3 Cu1 Cu4 N4 -152.6(8) . . . 5_455 ?
I2 Cu1 Cu4 N4 66.5(8) . . . 5_455 ?
I3 Cu1 Cu4 N4 -82.7(8) . . . 5_455 ?
Cu2 Cu1 Cu4 N4 139.0(8) . . . 5_455 ?
I1 Cu1 Cu4 N4 171.2(8) . . . 5_455 ?
N3 Cu1 Cu4 I4 178.9(10) . . . . ?
Cu3 Cu1 Cu4 I4 38.50(16) . . . . ?
I2 Cu1 Cu4 I4 -102.40(15) . . . . ?
I3 Cu1 Cu4 I4 108.46(15) . . . . ?
Cu2 Cu1 Cu4 I4 -29.83(14) . . . . ?
I1 Cu1 Cu4 I4 2.3(2) . . . . ?
N3 Cu1 Cu4 Cu3 140.4(11) . . . . ?
I2 Cu1 Cu4 Cu3 -140.90(16) . . . . ?
I3 Cu1 Cu4 Cu3 69.96(12) . . . . ?
Cu2 Cu1 Cu4 Cu3 -68.33(14) . . . . ?
I1 Cu1 Cu4 Cu3 -36.21(13) . . . . ?
N3 Cu1 Cu4 Cu2 -151.2(10) . . . . ?
Cu3 Cu1 Cu4 Cu2 68.33(14) . . . . ?
I2 Cu1 Cu4 Cu2 -72.57(12) . . . . ?
I3 Cu1 Cu4 Cu2 138.29(12) . . . . ?
I1 Cu1 Cu4 Cu2 32.12(13) . . . . ?
N3 Cu1 Cu4 I3 70.5(10) . . . . ?
Cu3 Cu1 Cu4 I3 -69.96(12) . . . . ?
I2 Cu1 Cu4 I3 149.14(11) . . . . ?
Cu2 Cu1 Cu4 I3 -138.29(12) . . . . ?
I1 Cu1 Cu4 I3 -106.17(12) . . . . ?
N3 Cu1 Cu4 I2 -78.7(10) . . . . ?
Cu3 Cu1 Cu4 I2 140.90(16) . . . . ?
I3 Cu1 Cu4 I2 -149.14(11) . . . . ?
Cu2 Cu1 Cu4 I2 72.57(12) . . . . ?
I1 Cu1 Cu4 I2 104.69(14) . . . . ?
Cu2 I4 Cu4 N4 -141.9(6) . . . 5_455 ?
Cu3 I4 Cu4 N4 151.9(6) . . . 5_455 ?
Cu2 I4 Cu4 Cu1 30.16(15) . . . . ?
Cu3 I4 Cu4 Cu1 -36.02(14) . . . . ?
Cu2 I4 Cu4 Cu3 66.17(12) . . . . ?
Cu3 I4 Cu4 Cu2 -66.17(12) . . . . ?
Cu2 I4 Cu4 I3 98.86(13) . . . . ?
Cu3 I4 Cu4 I3 32.69(11) . . . . ?
Cu2 I4 Cu4 I2 -33.59(10) . . . . ?
Cu3 I4 Cu4 I2 -99.76(12) . . . . ?
N2 Cu3 Cu4 N4 -21.5(12) 1_455 . . 5_455 ?
Cu2 Cu3 Cu4 N4 -150.4(9) . . . 5_455 ?
Cu1 Cu3 Cu4 N4 136.5(9) . . . 5_455 ?
I3 Cu3 Cu4 N4 64.6(9) . . . 5_455 ?
I1 Cu3 Cu4 N4 177.6(9) . . . 5_455 ?
I4 Cu3 Cu4 N4 -81.6(9) . . . 5_455 ?
N2 Cu3 Cu4 Cu1 -158.0(7) 1_455 . . . ?
Cu2 Cu3 Cu4 Cu1 73.11(14) . . . . ?
I3 Cu3 Cu4 Cu1 -71.85(12) . . . . ?
I1 Cu3 Cu4 Cu1 41.08(14) . . . . ?
I4 Cu3 Cu4 Cu1 141.94(16) . . . . ?
N2 Cu3 Cu4 I4 60.1(7) 1_455 . . . ?
Cu2 Cu3 Cu4 I4 -68.83(11) . . . . ?
Cu1 Cu3 Cu4 I4 -141.94(16) . . . . ?
I3 Cu3 Cu4 I4 146.21(11) . . . . ?
I1 Cu3 Cu4 I4 -100.86(15) . . . . ?
N2 Cu3 Cu4 Cu2 128.9(7) 1_455 . . . ?
Cu1 Cu3 Cu4 Cu2 -73.11(14) . . . . ?
I3 Cu3 Cu4 Cu2 -144.96(11) . . . . ?
I1 Cu3 Cu4 Cu2 -32.02(13) . . . . ?
I4 Cu3 Cu4 Cu2 68.83(11) . . . . ?
N2 Cu3 Cu4 I3 -86.1(7) 1_455 . . . ?
Cu2 Cu3 Cu4 I3 144.96(11) . . . . ?
Cu1 Cu3 Cu4 I3 71.85(12) . . . . ?
I1 Cu3 Cu4 I3 112.94(14) . . . . ?
I4 Cu3 Cu4 I3 -146.21(11) . . . . ?
N2 Cu3 Cu4 I2 168.0(7) 1_455 . . . ?
Cu2 Cu3 Cu4 I2 39.11(12) . . . . ?
Cu1 Cu3 Cu4 I2 -33.99(14) . . . . ?
I3 Cu3 Cu4 I2 -105.85(11) . . . . ?
I1 Cu3 Cu4 I2 7.09(18) . . . . ?
I4 Cu3 Cu4 I2 107.94(13) . . . . ?
N1 Cu2 Cu4 N4 0.5(9) 2_655 . . 5_455 ?
Cu3 Cu2 Cu4 N4 158.0(6) . . . 5_455 ?
I1 Cu2 Cu4 N4 -169.1(6) . . . 5_455 ?
I4 Cu2 Cu4 N4 79.4(6) . . . 5_455 ?
Cu1 Cu2 Cu4 N4 -131.8(6) . . . 5_455 ?
I2 Cu2 Cu4 N4 -65.2(6) . . . 5_455 ?
N1 Cu2 Cu4 Cu1 132.4(6) 2_655 . . . ?
Cu3 Cu2 Cu4 Cu1 -70.18(12) . . . . ?
I1 Cu2 Cu4 Cu1 -37.28(12) . . . . ?
I4 Cu2 Cu4 Cu1 -148.81(14) . . . . ?
I2 Cu2 Cu4 Cu1 66.62(9) . . . . ?
N1 Cu2 Cu4 I4 -78.8(6) 2_655 . . . ?
Cu3 Cu2 Cu4 I4 78.63(11) . . . . ?
I1 Cu2 Cu4 I4 111.53(14) . . . . ?
Cu1 Cu2 Cu4 I4 148.81(14) . . . . ?
I2 Cu2 Cu4 I4 -144.57(11) . . . . ?
N1 Cu2 Cu4 Cu3 -157.5(6) 2_655 . . . ?
I1 Cu2 Cu4 Cu3 32.89(12) . . . . ?
I4 Cu2 Cu4 Cu3 -78.63(11) . . . . ?
Cu1 Cu2 Cu4 Cu3 70.18(12) . . . . ?
I2 Cu2 Cu4 Cu3 136.79(11) . . . . ?
N1 Cu2 Cu4 I3 170.6(6) 2_655 . . . ?
Cu3 Cu2 Cu4 I3 -31.90(11) . . . . ?
I1 Cu2 Cu4 I3 0.99(17) . . . . ?
I4 Cu2 Cu4 I3 -110.53(12) . . . . ?
Cu1 Cu2 Cu4 I3 38.28(11) . . . . ?
I2 Cu2 Cu4 I3 104.89(11) . . . . ?
N1 Cu2 Cu4 I2 65.7(6) 2_655 . . . ?
Cu3 Cu2 Cu4 I2 -136.79(11) . . . . ?
I1 Cu2 Cu4 I2 -103.90(13) . . . . ?
I4 Cu2 Cu4 I2 144.57(11) . . . . ?
Cu1 Cu2 Cu4 I2 -66.62(9) . . . . ?
Cu3 I3 Cu4 N4 -154.7(4) . . . 5_455 ?
Cu1 I3 Cu4 N4 135.3(4) . . . 5_455 ?
Cu3 I3 Cu4 Cu1 70.03(11) . . . . ?
Cu3 I3 Cu4 I4 -34.89(10) . . . . ?
Cu1 I3 Cu4 I4 -104.93(14) . . . . ?
Cu1 I3 Cu4 Cu3 -70.03(11) . . . . ?
Cu3 I3 Cu4 Cu2 31.48(11) . . . . ?
Cu1 I3 Cu4 Cu2 -38.55(12) . . . . ?
Cu3 I3 Cu4 I2 97.94(12) . . . . ?
Cu1 I3 Cu4 I2 27.91(10) . . . . ?
Cu1 I2 Cu4 N4 -140.8(4) . . . 5_455 ?
Cu2 I2 Cu4 N4 146.6(4) . . . 5_455 ?
Cu2 I2 Cu4 Cu1 -72.68(12) . . . . ?
Cu1 I2 Cu4 I4 105.92(14) . . . . ?
Cu2 I2 Cu4 I4 33.24(10) . . . . ?
Cu1 I2 Cu4 Cu3 34.87(14) . . . . ?
Cu2 I2 Cu4 Cu3 -37.81(13) . . . . ?
Cu1 I2 Cu4 Cu2 72.68(12) . . . . ?
Cu1 I2 Cu4 I3 -28.94(11) . . . . ?
Cu2 I2 Cu4 I3 -101.63(12) . . . . ?
O9 Nd1 Na1 O5 -54.2(8) . . . . ?
O7 Nd1 Na1 O5 -173.6(13) . . . . ?
O1 Nd1 Na1 O5 163.3(7) . . . . ?
O3 Nd1 Na1 O5 -118.6(8) . . . . ?
O6 Nd1 Na1 O5 31.2(7) . . . . ?
O10 Nd1 Na1 O5 98.3(8) . . . . ?
O8 Nd1 Na1 O5 7.7(14) . . . . ?
O2 Nd1 Na1 O5 121.4(7) . . . . ?
O4 Nd1 Na1 O5 -124.5(7) . . . . ?
C24 Nd1 Na1 O5 162(14) . . . . ?
C18 Nd1 Na1 O5 18.5(8) . . . . ?
O9 Nd1 Na1 O5 -127.4(8) . . . 3_554 ?
O7 Nd1 Na1 O5 113.2(13) . . . 3_554 ?
O1 Nd1 Na1 O5 90.1(7) . . . 3_554 ?
O3 Nd1 Na1 O5 168.2(9) . . . 3_554 ?
O6 Nd1 Na1 O5 -42.0(7) . . . 3_554 ?
O10 Nd1 Na1 O5 25.1(9) . . . 3_554 ?
O8 Nd1 Na1 O5 -65.5(14) . . . 3_554 ?
O2 Nd1 Na1 O5 48.2(7) . . . 3_554 ?
O5 Nd1 Na1 O5 -73.2(11) . . . 3_554 ?
O4 Nd1 Na1 O5 162.3(7) . . . 3_554 ?
C24 Nd1 Na1 O5 89(14) . . . 3_554 ?
C18 Nd1 Na1 O5 -54.6(8) . . . 3_554 ?
O9 Nd1 Na1 O3 64.4(9) . . . . ?
O7 Nd1 Na1 O3 -55.0(14) . . . . ?
O1 Nd1 Na1 O3 -78.0(8) . . . . ?
O6 Nd1 Na1 O3 149.9(8) . . . . ?
O10 Nd1 Na1 O3 -143.0(9) . . . . ?
O8 Nd1 Na1 O3 126.3(15) . . . . ?
O2 Nd1 Na1 O3 -119.9(8) . . . . ?
O5 Nd1 Na1 O3 118.6(8) . . . . ?
O4 Nd1 Na1 O3 -5.9(8) . . . . ?
C24 Nd1 Na1 O3 -79(14) . . . . ?
C18 Nd1 Na1 O3 137.2(8) . . . . ?
O9 Nd1 Na1 O3 113.5(9) . . . 3_554 ?
O7 Nd1 Na1 O3 -5.9(13) . . . 3_554 ?
O1 Nd1 Na1 O3 -28.9(8) . . . 3_554 ?
O3 Nd1 Na1 O3 49.1(13) . . . 3_554 ?
O6 Nd1 Na1 O3 -161.1(8) . . . 3_554 ?
O10 Nd1 Na1 O3 -93.9(10) . . . 3_554 ?
O8 Nd1 Na1 O3 175.4(15) . . . 3_554 ?
O2 Nd1 Na1 O3 -70.8(8) . . . 3_554 ?
O5 Nd1 Na1 O3 167.7(10) . . . 3_554 ?
O4 Nd1 Na1 O3 43.2(8) . . . 3_554 ?
C24 Nd1 Na1 O3 -30(14) . . . 3_554 ?
C18 Nd1 Na1 O3 -173.7(9) . . . 3_554 ?
O9 Nd1 Na1 O2 -175.7(8) . . . . ?
O7 Nd1 Na1 O2 64.9(13) . . . . ?
O1 Nd1 Na1 O2 41.9(6) . . . . ?
O3 Nd1 Na1 O2 119.9(8) . . . . ?
O6 Nd1 Na1 O2 -90.2(6) . . . . ?
O10 Nd1 Na1 O2 -23.1(8) . . . . ?
O8 Nd1 Na1 O2 -113.8(14) . . . . ?
O5 Nd1 Na1 O2 -121.4(7) . . . . ?
O4 Nd1 Na1 O2 114.1(7) . . . . ?
C24 Nd1 Na1 O2 41(14) . . . . ?
C18 Nd1 Na1 O2 -102.9(7) . . . . ?
O9 Nd1 Na1 O2 -12.3(9) . . . 3_554 ?
O7 Nd1 Na1 O2 -131.8(13) . . . 3_554 ?
O1 Nd1 Na1 O2 -154.8(8) . . . 3_554 ?
O3 Nd1 Na1 O2 -76.8(8) . . . 3_554 ?
O6 Nd1 Na1 O2 73.1(7) . . . 3_554 ?
O10 Nd1 Na1 O2 140.2(8) . . . 3_554 ?
O8 Nd1 Na1 O2 49.6(15) . . . 3_554 ?
O2 Nd1 Na1 O2 163.3(10) . . . 3_554 ?
O5 Nd1 Na1 O2 41.9(8) . . . 3_554 ?
O4 Nd1 Na1 O2 -82.6(8) . . . 3_554 ?
C24 Nd1 Na1 O2 -156(14) . . . 3_554 ?
C18 Nd1 Na1 O2 60.4(8) . . . 3_554 ?
O9 Nd1 Na1 Nd1 -92.0(6) . . . 3_554 ?
O7 Nd1 Na1 Nd1 148.6(12) . . . 3_554 ?
O1 Nd1 Na1 Nd1 125.6(4) . . . 3_554 ?
O3 Nd1 Na1 Nd1 -156.4(6) . . . 3_554 ?
O6 Nd1 Na1 Nd1 -6.5(4) . . . 3_554 ?
O10 Nd1 Na1 Nd1 60.6(6) . . . 3_554 ?
O8 Nd1 Na1 Nd1 -30.1(13) . . . 3_554 ?
O2 Nd1 Na1 Nd1 83.7(5) . . . 3_554 ?
O5 Nd1 Na1 Nd1 -37.8(5) . . . 3_554 ?
O4 Nd1 Na1 Nd1 -162.3(5) . . . 3_554 ?
C24 Nd1 Na1 Nd1 124(14) . . . 3_554 ?
C18 Nd1 Na1 Nd1 -19.2(5) . . . 3_554 ?
O9 Nd1 O1 C6 -124.6(16) . . . . ?
O7 Nd1 O1 C6 156.6(16) . . . . ?
O3 Nd1 O1 C6 -75.8(14) . . . . ?
O6 Nd1 O1 C6 37.7(17) . . . . ?
O10 Nd1 O1 C6 80.6(15) . . . . ?
O8 Nd1 O1 C6 133.8(14) . . . . ?
O2 Nd1 O1 C6 -1.1(13) . . . . ?
O5 Nd1 O1 C6 -22.9(16) . . . . ?
O4 Nd1 O1 C6 -128.3(15) . . . . ?
C24 Nd1 O1 C6 145.2(16) . . . . ?
C18 Nd1 O1 C6 5.7(18) . . . . ?
O5 Na1 O2 C6 -138(2) . . . . ?
O5 Na1 O2 C6 115.2(19) 3_554 . . . ?
O3 Na1 O2 C6 -60.3(19) . . . . ?
O3 Na1 O2 C6 39(2) 3_554 . . . ?
O2 Na1 O2 C6 168.0(19) 3_554 . . . ?
Nd1 Na1 O2 C6 -99.0(19) . . . . ?
Nd1 Na1 O2 C6 87(2) 3_554 . . . ?
O5 Na1 O2 Nd1 -38.5(5) . . . . ?
O5 Na1 O2 Nd1 -145.8(5) 3_554 . . . ?
O3 Na1 O2 Nd1 38.7(5) . . . . ?
O3 Na1 O2 Nd1 138.4(5) 3_554 . . . ?
O2 Na1 O2 Nd1 -93.0(3) 3_554 . . . ?
Nd1 Na1 O2 Nd1 -174.2(4) 3_554 . . . ?
O9 Nd1 O2 C6 131.1(15) . . . . ?
O7 Nd1 O2 C6 -24.4(14) . . . . ?
O1 Nd1 O2 C6 1.1(12) . . . . ?
O3 Nd1 O2 C6 87.5(13) . . . . ?
O6 Nd1 O2 C6 -149.8(13) . . . . ?
O10 Nd1 O2 C6 -78.3(14) . . . . ?
O8 Nd1 O2 C6 -94.1(14) . . . . ?
O5 Nd1 O2 C6 160.3(13) . . . . ?
O4 Nd1 O2 C6 53.2(13) . . . . ?
C24 Nd1 O2 C6 -52.6(16) . . . . ?
C18 Nd1 O2 C6 -173.4(14) . . . . ?
O9 Nd1 O2 Na1 6.6(12) . . . . ?
O7 Nd1 O2 Na1 -149.0(6) . . . . ?
O1 Nd1 O2 Na1 -123.5(8) . . . . ?
O3 Nd1 O2 Na1 -37.0(5) . . . . ?
O6 Nd1 O2 Na1 85.6(5) . . . . ?
O10 Nd1 O2 Na1 157.1(7) . . . . ?
O8 Nd1 O2 Na1 141.4(7) . . . . ?
O5 Nd1 O2 Na1 35.8(4) . . . . ?
O4 Nd1 O2 Na1 -71.4(6) . . . . ?
C24 Nd1 O2 Na1 -177.2(9) . . . . ?
C18 Nd1 O2 Na1 62.0(6) . . . . ?
O5 Na1 O3 C12 177(8) . . . . ?
O5 Na1 O3 C12 69(9) 3_554 . . . ?
O3 Na1 O3 C12 -13(7) 3_554 . . . ?
O2 Na1 O3 C12 97(8) . . . . ?
O2 Na1 O3 C12 -93(8) 3_554 . . . ?
Nd1 Na1 O3 C12 136(8) . . . . ?
Nd1 Na1 O3 C12 -46(8) 3_554 . . . ?
O5 Na1 O3 Nd1 40.3(5) . . . . ?
O5 Na1 O3 Nd1 -67(4) 3_554 . . . ?
O3 Na1 O3 Nd1 -149.6(8) 3_554 . . . ?
O2 Na1 O3 Nd1 -39.6(5) . . . . ?
O2 Na1 O3 Nd1 130.8(6) 3_554 . . . ?
Nd1 Na1 O3 Nd1 177.4(2) 3_554 . . . ?
O9 Nd1 O3 C12 73.4(14) . . . . ?
O7 Nd1 O3 C12 -18.3(16) . . . . ?
O1 Nd1 O3 C12 -79.2(14) . . . . ?
O6 Nd1 O3 C12 154.2(13) . . . . ?
O10 Nd1 O3 C12 -113.6(15) . . . . ?
O8 Nd1 O3 C12 47.8(18) . . . . ?
O2 Nd1 O3 C12 -133.9(14) . . . . ?
O5 Nd1 O3 C12 151.3(15) . . . . ?
O4 Nd1 O3 C12 1.0(13) . . . . ?
C24 Nd1 O3 C12 4(2) . . . . ?
C18 Nd1 O3 C12 151.8(14) . . . . ?
O9 Nd1 O3 Na1 -115.3(8) . . . . ?
O7 Nd1 O3 Na1 153.1(7) . . . . ?
O1 Nd1 O3 Na1 92.1(6) . . . . ?
O6 Nd1 O3 Na1 -34.4(9) . . . . ?
O10 Nd1 O3 Na1 57.8(11) . . . . ?
O8 Nd1 O3 Na1 -140.8(8) . . . . ?
O2 Nd1 O3 Na1 37.4(5) . . . . ?
O5 Nd1 O3 Na1 -37.4(5) . . . . ?
O4 Nd1 O3 Na1 172.3(10) . . . . ?
C24 Nd1 O3 Na1 175.6(10) . . . . ?
C18 Nd1 O3 Na1 -36.9(7) . . . . ?
O9 Nd1 O4 C12 -95.1(17) . . . . ?
O7 Nd1 O4 C12 161.3(17) . . . . ?
O1 Nd1 O4 C12 82.6(16) . . . . ?
O3 Nd1 O4 C12 -1.1(14) . . . . ?
O6 Nd1 O4 C12 -71(2) . . . . ?
O10 Nd1 O4 C12 121.7(16) . . . . ?
O8 Nd1 O4 C12 -157.8(15) . . . . ?
O2 Nd1 O4 C12 42.0(17) . . . . ?
O5 Nd1 O4 C12 -30.4(17) . . . . ?
C24 Nd1 O4 C12 -179.0(17) . . . . ?
C18 Nd1 O4 C12 -44.6(19) . . . . ?
O5 Na1 O5 C18 34.1(17) 3_554 . . . ?
O3 Na1 O5 C18 -136(2) . . . . ?
O3 Na1 O5 C18 139(3) 3_554 . . . ?
O2 Na1 O5 C18 -58.3(19) . . . . ?
O2 Na1 O5 C18 112.0(19) 3_554 . . . ?
Nd1 Na1 O5 C18 -97(2) . . . . ?
Nd1 Na1 O5 C18 80(2) 3_554 . . . ?
O5 Na1 O5 Nd1 131.0(6) 3_554 . . . ?
O3 Na1 O5 Nd1 -39.4(5) . . . . ?
O3 Na1 O5 Nd1 -124(3) 3_554 . . . ?
O2 Na1 O5 Nd1 38.6(5) . . . . ?
O2 Na1 O5 Nd1 -151.2(5) 3_554 . . . ?
Nd1 Na1 O5 Nd1 176.6(2) 3_554 . . . ?
O9 Nd1 O5 C18 -95.2(15) . . . . ?
O7 Nd1 O5 C18 -55(4) . . . . ?
O1 Nd1 O5 C18 122.4(13) . . . . ?
O3 Nd1 O5 C18 178.9(15) . . . . ?
O6 Nd1 O5 C18 2.3(13) . . . . ?
O10 Nd1 O5 C18 44.2(15) . . . . ?
O8 Nd1 O5 C18 -35.6(16) . . . . ?
O2 Nd1 O5 C18 104.1(14) . . . . ?
O4 Nd1 O5 C18 -157.0(13) . . . . ?
C24 Nd1 O5 C18 -38(2) . . . . ?
O9 Nd1 O5 Na1 123.9(8) . . . . ?
O7 Nd1 O5 Na1 164(3) . . . . ?
O1 Nd1 O5 Na1 -18.5(8) . . . . ?
O3 Nd1 O5 Na1 38.0(5) . . . . ?
O6 Nd1 O5 Na1 -138.6(9) . . . . ?
O10 Nd1 O5 Na1 -96.7(8) . . . . ?
O8 Nd1 O5 Na1 -176.5(6) . . . . ?
O2 Nd1 O5 Na1 -36.7(5) . . . . ?
O4 Nd1 O5 Na1 62.1(7) . . . . ?
C24 Nd1 O5 Na1 -178.5(12) . . . . ?
C18 Nd1 O5 Na1 -140.9(16) . . . . ?
O9 Nd1 O6 C18 71.5(16) . . . . ?
O7 Nd1 O6 C18 166.4(15) . . . . ?
O1 Nd1 O6 C18 -97.9(16) . . . . ?
O3 Nd1 O6 C18 -5.9(18) . . . . ?
O10 Nd1 O6 C18 -140.9(17) . . . . ?
O8 Nd1 O6 C18 142.7(17) . . . . ?
O2 Nd1 O6 C18 -68.3(16) . . . . ?
O5 Nd1 O6 C18 -2.4(14) . . . . ?
O4 Nd1 O6 C18 49(2) . . . . ?
C24 Nd1 O6 C18 154.8(17) . . . . ?
O9 Nd1 O6 Na2 -62.2(10) . . . . ?
O7 Nd1 O6 Na2 32.7(12) . . . . ?
O1 Nd1 O6 Na2 128.4(9) . . . . ?
O3 Nd1 O6 Na2 -139.6(9) . . . . ?
O10 Nd1 O6 Na2 85.5(10) . . . . ?
O8 Nd1 O6 Na2 9.1(9) . . . . ?
O2 Nd1 O6 Na2 158.1(9) . . . . ?
O5 Nd1 O6 Na2 -136.0(12) . . . . ?
O4 Nd1 O6 Na2 -84.8(14) . . . . ?
C24 Nd1 O6 Na2 21.1(11) . . . . ?
C18 Nd1 O6 Na2 -134(2) . . . . ?
O9 Nd1 O7 C24 63(2) . . . . ?
O1 Nd1 O7 C24 -154(2) . . . . ?
O3 Nd1 O7 C24 145(2) . . . . ?
O6 Nd1 O7 C24 -27(2) . . . . ?
O10 Nd1 O7 C24 -79(2) . . . . ?
O8 Nd1 O7 C24 2(2) . . . . ?
O2 Nd1 O7 C24 -133(2) . . . . ?
O5 Nd1 O7 C24 24(4) . . . . ?
O4 Nd1 O7 C24 130(2) . . . . ?
C18 Nd1 O7 C24 -17(3) . . . . ?
O9 Nd1 O8 C24 -116(2) . . . . ?
O7 Nd1 O8 C24 -2.0(19) . . . . ?
O1 Nd1 O8 C24 26(2) . . . . ?
O3 Nd1 O8 C24 -89(2) . . . . ?
O6 Nd1 O8 C24 153(2) . . . . ?
O10 Nd1 O8 C24 78(2) . . . . ?
O2 Nd1 O8 C24 94(2) . . . . ?
O5 Nd1 O8 C24 -177.4(19) . . . . ?
O4 Nd1 O8 C24 -53(2) . . . . ?
C18 Nd1 O8 C24 168(2) . . . . ?
O9 Nd1 O8 Na2 82.6(11) . . . . ?
O7 Nd1 O8 Na2 -163.9(14) . . . . ?
O1 Nd1 O8 Na2 -136.0(9) . . . . ?
O3 Nd1 O8 Na2 109.4(12) . . . . ?
O6 Nd1 O8 Na2 -9.0(10) . . . . ?
O10 Nd1 O8 Na2 -83.6(11) . . . . ?
O2 Nd1 O8 Na2 -67.9(13) . . . . ?
O5 Nd1 O8 Na2 20.8(12) . . . . ?
O4 Nd1 O8 Na2 144.9(10) . . . . ?
C24 Nd1 O8 Na2 -162(3) . . . . ?
C18 Nd1 O8 Na2 5.7(11) . . . . ?
C5 N1 C1 C2 0.0 . . . . ?
Cu2 N1 C1 C2 -163.2(9) 2_654 . . . ?
N1 C1 C2 C3 0.0 . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C1 C2 C3 C6 175.7(16) . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C6 C3 C4 C5 -175.6(17) . . . . ?
C3 C4 C5 N1 0.0 . . . . ?
C1 N1 C5 C4 0.0 . . . . ?
Cu2 N1 C5 C4 163.1(10) 2_654 . . . ?
C11 N2 C7 C8 0.0 . . . . ?
Cu3 N2 C7 C8 -169.3(11) 1_655 . . . ?
N2 C7 C8 C9 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C7 C8 C9 C12 178.5(17) . . . . ?
C8 C9 C10 C11 0.0 . . . . ?
C12 C9 C10 C11 -178.5(16) . . . . ?
C9 C10 C11 N2 0.0 . . . . ?
C7 N2 C11 C10 0.0 . . . . ?
Cu3 N2 C11 C10 169.1(10) 1_655 . . . ?
Cu4 Cu1 N3 C13 54.1(15) . . . . ?
Cu3 Cu1 N3 C13 -176.9(6) . . . . ?
I2 Cu1 N3 C13 -16.4(9) . . . . ?
I3 Cu1 N3 C13 115.6(7) . . . . ?
Cu2 Cu1 N3 C13 -87.6(9) . . . . ?
I1 Cu1 N3 C13 -129.1(8) . . . . ?
Cu4 Cu1 N3 C17 -135.1(9) . . . . ?
Cu3 Cu1 N3 C17 -6.1(10) . . . . ?
I2 Cu1 N3 C17 154.4(6) . . . . ?
I3 Cu1 N3 C17 -73.5(7) . . . . ?
Cu2 Cu1 N3 C17 83.2(8) . . . . ?
I1 Cu1 N3 C17 41.7(7) . . . . ?
C17 N3 C13 C14 0.0 . . . . ?
Cu1 N3 C13 C14 170.7(10) . . . . ?
N3 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
C13 C14 C15 C18 -175.1(15) . . . . ?
C14 C15 C16 C17 0.0 . . . . ?
C18 C15 C16 C17 175.3(14) . . . . ?
C15 C16 C17 N3 0.0 . . . . ?
C13 N3 C17 C16 0.0 . . . . ?
Cu1 N3 C17 C16 -170.9(10) . . . . ?
C23 N4 C19 C20 0.0 . . . . ?
Cu4 N4 C19 C20 -170.0(13) 5_545 . . . ?
N4 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C19 C20 C21 C24 177(2) . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C24 C21 C22 C23 -177(2) . . . . ?
C21 C22 C23 N4 0.0 . . . . ?
C19 N4 C23 C22 0.0 . . . . ?
Cu4 N4 C23 C22 169.7(13) 5_545 . . . ?
Nd1 O1 C6 O2 2(2) . . . . ?
Nd1 O1 C6 C3 178.6(19) . . . . ?
Na1 O2 C6 O1 97(2) . . . . ?
Nd1 O2 C6 O1 -2(2) . . . . ?
Na1 O2 C6 C3 -80(3) . . . . ?
Nd1 O2 C6 C3 -178.7(19) . . . . ?
Na1 O2 C6 Nd1 98.4(14) . . . . ?
C4 C3 C6 O1 -174.0(18) . . . . ?
C2 C3 C6 O1 10(3) . . . . ?
C4 C3 C6 O2 3(3) . . . . ?
C2 C3 C6 O2 -173.1(16) . . . . ?
C4 C3 C6 Nd1 -95(71) . . . . ?
C2 C3 C6 Nd1 90(72) . . . . ?
O9 Nd1 C6 O1 93.8(19) . . . . ?
O7 Nd1 C6 O1 -22.7(15) . . . . ?
O3 Nd1 C6 O1 95.9(15) . . . . ?
O6 Nd1 C6 O1 -150.2(14) . . . . ?
O10 Nd1 C6 O1 -89.9(15) . . . . ?
O8 Nd1 C6 O1 -64.0(17) . . . . ?
O2 Nd1 C6 O1 178(2) . . . . ?
O5 Nd1 C6 O1 159.7(14) . . . . ?
O4 Nd1 C6 O1 48.5(14) . . . . ?
C24 Nd1 C6 O1 -39.8(17) . . . . ?
C18 Nd1 C6 O1 -175.4(14) . . . . ?
O9 Nd1 C6 O2 -84.2(19) . . . . ?
O7 Nd1 C6 O2 159.3(12) . . . . ?
O1 Nd1 C6 O2 -178(2) . . . . ?
O3 Nd1 C6 O2 -82.1(12) . . . . ?
O6 Nd1 C6 O2 31.8(13) . . . . ?
O10 Nd1 C6 O2 92.1(13) . . . . ?
O8 Nd1 C6 O2 118.0(12) . . . . ?
O5 Nd1 C6 O2 -18.3(12) . . . . ?
O4 Nd1 C6 O2 -129.5(12) . . . . ?
C24 Nd1 C6 O2 142.2(13) . . . . ?
C18 Nd1 C6 O2 6.6(14) . . . . ?
O9 Nd1 C6 C3 14(72) . . . . ?
O7 Nd1 C6 C3 -103(72) . . . . ?
O1 Nd1 C6 C3 -80(71) . . . . ?
O3 Nd1 C6 C3 16(72) . . . . ?
O6 Nd1 C6 C3 130(72) . . . . ?
O10 Nd1 C6 C3 -170(100) . . . . ?
O8 Nd1 C6 C3 -144(71) . . . . ?
O2 Nd1 C6 C3 98(72) . . . . ?
O5 Nd1 C6 C3 80(72) . . . . ?
O4 Nd1 C6 C3 -32(72) . . . . ?
C24 Nd1 C6 C3 -120(72) . . . . ?
C18 Nd1 C6 C3 104(72) . . . . ?
Nd1 O4 C12 O3 2(3) . . . . ?
Nd1 O4 C12 C9 -176.3(18) . . . . ?
Na1 O3 C12 O4 -138(6) . . . . ?
Nd1 O3 C12 O4 -2(3) . . . . ?
Na1 O3 C12 C9 40(9) . . . . ?
Nd1 O3 C12 C9 176.4(15) . . . . ?
Na1 O3 C12 Nd1 -136(8) . . . . ?
C8 C9 C12 O4 -173(2) . . . . ?
C10 C9 C12 O4 5(3) . . . . ?
C8 C9 C12 O3 8(3) . . . . ?
C10 C9 C12 O3 -173.3(16) . . . . ?
C8 C9 C12 Nd1 40(14) . . . . ?
C10 C9 C12 Nd1 -142(13) . . . . ?
O9 Nd1 C12 O4 77.2(17) . . . . ?
O7 Nd1 C12 O4 -17.8(17) . . . . ?
O1 Nd1 C12 O4 -89.3(16) . . . . ?
O3 Nd1 C12 O4 178(2) . . . . ?
O6 Nd1 C12 O4 141.1(15) . . . . ?
O10 Nd1 C12 O4 -84.1(19) . . . . ?
O8 Nd1 C12 O4 27.5(19) . . . . ?
O2 Nd1 C12 O4 -139.8(16) . . . . ?
O5 Nd1 C12 O4 151.9(16) . . . . ?
C24 Nd1 C12 O4 1.1(18) . . . . ?
C18 Nd1 C12 O4 146.4(15) . . . . ?
O9 Nd1 C12 O3 -100.9(15) . . . . ?
O7 Nd1 C12 O3 164.1(14) . . . . ?
O1 Nd1 C12 O3 92.5(14) . . . . ?
O6 Nd1 C12 O3 -37.0(18) . . . . ?
O10 Nd1 C12 O3 97.8(16) . . . . ?
O8 Nd1 C12 O3 -150.7(13) . . . . ?
O2 Nd1 C12 O3 42.1(13) . . . . ?
O5 Nd1 C12 O3 -26.3(14) . . . . ?
O4 Nd1 C12 O3 -178(2) . . . . ?
C24 Nd1 C12 O3 -177.0(14) . . . . ?
C18 Nd1 C12 O3 -31.7(15) . . . . ?
O9 Nd1 C12 C9 -134(14) . . . . ?
O7 Nd1 C12 C9 131(14) . . . . ?
O1 Nd1 C12 C9 59(14) . . . . ?
O3 Nd1 C12 C9 -33(13) . . . . ?
O6 Nd1 C12 C9 -70(14) . . . . ?
O10 Nd1 C12 C9 64(14) . . . . ?
O8 Nd1 C12 C9 176(13) . . . . ?
O2 Nd1 C12 C9 9(14) . . . . ?
O5 Nd1 C12 C9 -60(14) . . . . ?
O4 Nd1 C12 C9 149(14) . . . . ?
C24 Nd1 C12 C9 150(13) . . . . ?
C18 Nd1 C12 C9 -65(14) . . . . ?
Nd1 O6 C18 O5 5(3) . . . . ?
Na2 O6 C18 O5 120(2) . . . . ?
Nd1 O6 C18 C15 178.6(17) . . . . ?
Na2 O6 C18 C15 -66(3) . . . . ?
Na2 O6 C18 Nd1 115.7(19) . . . . ?
Na1 O5 C18 O6 94(3) . . . . ?
Nd1 O5 C18 O6 -5(3) . . . . ?
Na1 O5 C18 C15 -80(3) . . . . ?
Nd1 O5 C18 C15 -178.9(15) . . . . ?
Na1 O5 C18 Nd1 98.6(17) . . . . ?
C16 C15 C18 O6 -5(3) . . . . ?
C14 C15 C18 O6 170.2(18) . . . . ?
C16 C15 C18 O5 169.6(15) . . . . ?
C14 C15 C18 O5 -15(2) . . . . ?
C16 C15 C18 Nd1 148(31) . . . . ?
C14 C15 C18 Nd1 -37(32) . . . . ?
O9 Nd1 C18 O6 -105.5(16) . . . . ?
O7 Nd1 C18 O6 -21(2) . . . . ?
O1 Nd1 C18 O6 102.4(16) . . . . ?
O3 Nd1 C18 O6 174.8(16) . . . . ?
O10 Nd1 C18 O6 36.6(16) . . . . ?
O8 Nd1 C18 O6 -35.8(17) . . . . ?
O2 Nd1 C18 O6 107.9(16) . . . . ?
O5 Nd1 C18 O6 176(2) . . . . ?
O4 Nd1 C18 O6 -153.3(15) . . . . ?
C24 Nd1 C18 O6 -29.3(19) . . . . ?
O9 Nd1 C18 O5 78.7(14) . . . . ?
O7 Nd1 C18 O5 163.4(14) . . . . ?
O1 Nd1 C18 O5 -73.4(15) . . . . ?
O3 Nd1 C18 O5 -1.0(14) . . . . ?
O6 Nd1 C18 O5 -176(2) . . . . ?
O10 Nd1 C18 O5 -139.2(14) . . . . ?
O8 Nd1 C18 O5 148.4(14) . . . . ?
O2 Nd1 C18 O5 -67.8(13) . . . . ?
O4 Nd1 C18 O5 30.9(17) . . . . ?
C24 Nd1 C18 O5 154.9(14) . . . . ?
O9 Nd1 C18 C15 101(32) . . . . ?
O7 Nd1 C18 C15 -175(100) . . . . ?
O1 Nd1 C18 C15 -51(32) . . . . ?
O3 Nd1 C18 C15 21(32) . . . . ?
O6 Nd1 C18 C15 -154(33) . . . . ?
O10 Nd1 C18 C15 -117(32) . . . . ?
O8 Nd1 C18 C15 170(32) . . . . ?
O2 Nd1 C18 C15 -46(32) . . . . ?
O5 Nd1 C18 C15 22(31) . . . . ?
O4 Nd1 C18 C15 53(32) . . . . ?
C24 Nd1 C18 C15 177(100) . . . . ?
Nd1 O7 C24 O8 -4(4) . . . . ?
Nd1 O7 C24 C21 166(2) . . . . ?
Nd1 O8 C24 O7 4(4) . . . . ?
Na2 O8 C24 O7 135(4) . . . . ?
Nd1 O8 C24 C21 -167(3) . . . . ?
Na2 O8 C24 C21 -35(7) . . . . ?
Na2 O8 C24 Nd1 131(5) . . . . ?
C20 C21 C24 O7 0(4) . . . . ?
C22 C21 C24 O7 177(2) . . . . ?
C20 C21 C24 O8 171(2) . . . . ?
C22 C21 C24 O8 -12(4) . . . . ?
C20 C21 C24 Nd1 77(8) . . . . ?
C22 C21 C24 Nd1 -107(7) . . . . ?
O9 Nd1 C24 O7 -117(2) . . . . ?
O1 Nd1 C24 O7 25(2) . . . . ?
O3 Nd1 C24 O7 -49(3) . . . . ?
O6 Nd1 C24 O7 157(2) . . . . ?
O10 Nd1 C24 O7 91(2) . . . . ?
O8 Nd1 C24 O7 -176(4) . . . . ?
O2 Nd1 C24 O7 65(2) . . . . ?
O5 Nd1 C24 O7 -172.4(15) . . . . ?
O4 Nd1 C24 O7 -47(2) . . . . ?
C18 Nd1 C24 O7 169.3(18) . . . . ?
O9 Nd1 C24 O8 59(2) . . . . ?
O7 Nd1 C24 O8 176(4) . . . . ?
O1 Nd1 C24 O8 -158.2(19) . . . . ?
O3 Nd1 C24 O8 127.1(17) . . . . ?
O6 Nd1 C24 O8 -26(2) . . . . ?
O10 Nd1 C24 O8 -92(2) . . . . ?
O2 Nd1 C24 O8 -118.4(18) . . . . ?
O5 Nd1 C24 O8 4(3) . . . . ?
O4 Nd1 C24 O8 130(2) . . . . ?
C18 Nd1 C24 O8 -14(2) . . . . ?
O9 Nd1 C24 C21 160(8) . . . . ?
O7 Nd1 C24 C21 -83(8) . . . . ?
O1 Nd1 C24 C21 -57(8) . . . . ?
O3 Nd1 C24 C21 -132(7) . . . . ?
O6 Nd1 C24 C21 75(8) . . . . ?
O10 Nd1 C24 C21 9(7) . . . . ?
O8 Nd1 C24 C21 101(8) . . . . ?
O2 Nd1 C24 C21 -17(8) . . . . ?
O5 Nd1 C24 C21 105(7) . . . . ?
O4 Nd1 C24 C21 -129(8) . . . . ?
C18 Nd1 C24 C21 87(8) . . . . ?
C18 O6 Na2 O8 -119(2) . . . . ?
Nd1 O6 Na2 O8 -9.0(9) . . . . ?
C18 O6 Na2 Nd1 -110(2) . . . . ?
C24 O8 Na2 O6 -120(5) . . . . ?
Nd1 O8 Na2 O6 8.9(9) . . . . ?
C24 O8 Na2 Nd1 -129(6) . . . . ?
O9 Nd1 Na2 O6 110.7(11) . . . . ?
O7 Nd1 Na2 O6 -152.8(10) . . . . ?
O1 Nd1 Na2 O6 -90.2(11) . . . . ?
O3 Nd1 Na2 O6 66.4(12) . . . . ?
O10 Nd1 Na2 O6 -81.6(10) . . . . ?
O8 Nd1 Na2 O6 -165.6(15) . . . . ?
O2 Nd1 Na2 O6 -25.4(10) . . . . ?
O5 Nd1 Na2 O6 33.2(9) . . . . ?
O4 Nd1 Na2 O6 144.0(9) . . . . ?
C24 Nd1 Na2 O6 -156.5(13) . . . . ?
C18 Nd1 Na2 O6 21.2(9) . . . . ?
O9 Nd1 Na2 O8 -83.7(12) . . . . ?
O7 Nd1 Na2 O8 12.8(11) . . . . ?
O1 Nd1 Na2 O8 75.4(14) . . . . ?
O3 Nd1 Na2 O8 -128.0(11) . . . . ?
O6 Nd1 Na2 O8 165.6(15) . . . . ?
O10 Nd1 Na2 O8 83.9(12) . . . . ?
O2 Nd1 Na2 O8 140.2(10) . . . . ?
O5 Nd1 Na2 O8 -161.3(11) . . . . ?
O4 Nd1 Na2 O8 -50.5(13) . . . . ?
C24 Nd1 Na2 O8 9.0(13) . . . . ?
C18 Nd1 Na2 O8 -173.2(13) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.588
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.230
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1430393'
_audit_update_record             
;
2015-10-09 deposited with the CCDC.
2017-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            9-Tb
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H72 Cu2 I2 N14 O23 Tb2'
_chemical_formula_weight         1911.92

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.2008(10)
_cell_length_b                   12.5798(11)
_cell_length_c                   15.1576(14)
_cell_angle_alpha                92.2910(10)
_cell_angle_beta                 97.1310(10)
_cell_angle_gamma                116.3470(10)
_cell_volume                     1888.2(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.066
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    3.296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15120
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         24.82
_reflns_number_total             6304
_reflns_number_gt                5907
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0431P)²+5.5142P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6304
_refine_ls_number_parameters     412
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0799
_refine_ls_wR_factor_gt          0.0779
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.051
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.707222(18) 0.111576(16) 0.036176(12) 0.02627(8) Uani 1 1 d . . .
I1 I 0.27494(3) 0.42770(3) 0.49105(2) 0.04336(10) Uani 1 1 d . . .
Cu1 Cu 0.48669(6) 0.50192(5) 0.41092(3) 0.03671(14) Uani 1 1 d . . .
O4 O 0.6174(3) -0.0477(3) 0.1248(2) 0.0397(7) Uani 1 1 d . . .
O3 O 0.3912(3) -0.1334(3) 0.1027(2) 0.0382(7) Uani 1 1 d . . .
O2 O 0.5171(3) 0.1202(3) 0.0706(2) 0.0421(8) Uani 1 1 d . . .
O1 O 0.2963(3) 0.0531(3) 0.0513(2) 0.0388(7) Uani 1 1 d . . .
O5 O 0.7724(4) 0.3212(3) 0.0431(3) 0.0548(9) Uani 1 1 d . . .
O6 O 0.8911(3) 0.1866(3) -0.0435(2) 0.0452(8) Uani 1 1 d . . .
N2 N 0.4955(4) -0.3598(4) 0.3371(3) 0.0387(9) Uani 1 1 d . . .
N1 N 0.4577(4) 0.3730(3) 0.3084(3) 0.0395(9) Uani 1 1 d . . .
O7 O 0.8020(4) 0.2009(4) 0.1939(3) 0.0603(10) Uani 1 1 d . . .
O8 O 0.9114(4) 0.1244(4) 0.1323(3) 0.0609(10) Uani 1 1 d . . .
C9 C 0.5014(4) -0.2016(4) 0.2118(3) 0.0323(9) Uani 1 1 d . . .
C8 C 0.3818(5) -0.2797(4) 0.2377(3) 0.0414(11) Uani 1 1 d . . .
H8A H 0.2991 -0.2805 0.2129 0.050 Uiso 1 1 calc R . .
N4 N 0.9935(4) 0.1315(4) -0.1420(3) 0.0525(11) Uani 1 1 d . . .
C4 C 0.4126(5) 0.1227(4) 0.0897(3) 0.0324(9) Uani 1 1 d . . .
C12 C 0.5043(4) -0.1196(4) 0.1409(3) 0.0321(9) Uani 1 1 d . . .
C3 C 0.4281(4) 0.2125(4) 0.1648(3) 0.0324(9) Uani 1 1 d . . .
N5 N 0.8993(5) 0.1758(5) 0.2006(3) 0.0594(12) Uani 1 1 d . . .
C2 C 0.3163(5) 0.2127(4) 0.1952(3) 0.0409(11) Uani 1 1 d . . .
H2A H 0.2277 0.1583 0.1672 0.049 Uiso 1 1 calc R . .
C10 C 0.6179(5) -0.2013(5) 0.2529(4) 0.0542(14) Uani 1 1 d . . .
H10A H 0.7027 -0.1464 0.2390 0.065 Uiso 1 1 calc R . .
C5 C 0.5541(5) 0.2949(5) 0.2069(3) 0.0467(12) Uani 1 1 d . . .
H5A H 0.6330 0.2981 0.1874 0.056 Uiso 1 1 calc R . .
C1 C 0.3359(5) 0.2932(5) 0.2670(3) 0.0431(11) Uani 1 1 d . . .
H1A H 0.2587 0.2917 0.2879 0.052 Uiso 1 1 calc R . .
N6 N 0.0142(5) 0.4612(5) 0.6795(4) 0.0656(13) Uani 1 1 d . . .
C7 C 0.3833(5) -0.3562(4) 0.2997(3) 0.0433(11) Uani 1 1 d . . .
H7A H 0.3001 -0.4093 0.3168 0.052 Uiso 1 1 calc R . .
C6 C 0.5646(5) 0.3729(5) 0.2778(4) 0.0490(13) Uani 1 1 d . . .
H6A H 0.6521 0.4293 0.3061 0.059 Uiso 1 1 calc R . .
N3 N 0.7813(6) 0.4782(4) -0.0291(4) 0.0664(14) Uani 1 1 d . . .
C18 C 0.8955(5) 0.1516(5) -0.1206(3) 0.0447(11) Uani 1 1 d . . .
H18A H 0.8231 0.1388 -0.1666 0.054 Uiso 1 1 calc R . .
C15 C 0.8143(6) 0.3921(4) -0.0133(4) 0.0513(13) Uani 1 1 d . . .
H15A H 0.8751 0.3833 -0.0480 0.062 Uiso 1 1 calc R . .
C11 C 0.6117(5) -0.2807(5) 0.3143(4) 0.0566(15) Uani 1 1 d . . .
H11A H 0.6935 -0.2792 0.3417 0.068 Uiso 1 1 calc R . .
O9 O 0.9788(7) 0.2011(7) 0.2697(4) 0.125(3) Uani 1 1 d . . .
N7 N 0.4896(7) 0.8921(6) 0.5925(4) 0.0825(17) Uani 1 1 d D . .
O10 O -0.0092(8) 0.3955(6) 0.8154(4) 0.132(3) Uani 1 1 d . . .
C17 C 0.9957(8) 0.0954(8) -0.2339(5) 0.083(2) Uani 1 1 d . . .
H17A H 0.9150 0.0887 -0.2723 0.124 Uiso 1 1 calc R . .
H17B H 0.9971 0.0180 -0.2372 0.124 Uiso 1 1 calc R . .
H17C H 1.0765 0.1551 -0.2541 0.124 Uiso 1 1 calc R . .
C21 C 0.0368(9) 0.4752(7) 0.7668(5) 0.091(2) Uani 1 1 d . . .
H21A H 0.0936 0.5536 0.7951 0.109 Uiso 1 1 calc R . .
C20 C 0.0662(8) 0.5624(7) 0.6303(5) 0.0756(19) Uani 1 1 d . . .
H20A H 0.1182 0.6348 0.6720 0.113 Uiso 1 1 calc R . .
H20B H -0.0087 0.5687 0.5942 0.113 Uiso 1 1 calc R . .
H20C H 0.1249 0.5530 0.5910 0.113 Uiso 1 1 calc R . .
C14 C 0.8396(8) 0.5628(6) -0.0937(5) 0.085(2) Uani 1 1 d . . .
H14A H 0.8998 0.5412 -0.1234 0.127 Uiso 1 1 calc R . .
H14B H 0.8909 0.6435 -0.0626 0.127 Uiso 1 1 calc R . .
H14C H 0.7670 0.5604 -0.1385 0.127 Uiso 1 1 calc R . .
C16 C 1.1051(8) 0.1462(8) -0.0750(6) 0.094(3) Uani 1 1 d . . .
H16A H 1.0915 0.1708 -0.0164 0.141 Uiso 1 1 calc R . .
H16B H 1.1895 0.2074 -0.0901 0.141 Uiso 1 1 calc R . .
H16C H 1.1099 0.0704 -0.0730 0.141 Uiso 1 1 calc R . .
C19 C -0.0655(9) 0.3462(8) 0.6282(6) 0.107(3) Uani 1 1 d . . .
H19A H -0.0955 0.2842 0.6690 0.160 Uiso 1 1 calc R . .
H19B H -0.0107 0.3302 0.5890 0.160 Uiso 1 1 calc R . .
H19C H -0.1443 0.3461 0.5919 0.160 Uiso 1 1 calc R . .
O11 O 0.6619(12) 1.0406(10) 0.6859(7) 0.186(4) Uani 1 1 d DU . .
C24 C 0.6173(13) 0.9645(12) 0.6308(10) 0.200(7) Uani 1 1 d DU . .
H24A H 0.6827 0.9484 0.6068 0.240 Uiso 1 1 calc R . .
C13 C 0.6863(13) 0.4926(11) 0.0218(10) 0.167(6) Uani 1 1 d . . .
H13A H 0.6551 0.4293 0.0614 0.251 Uiso 1 1 calc R . .
H13B H 0.6090 0.4877 -0.0195 0.251 Uiso 1 1 calc R . .
H13C H 0.7310 0.5705 0.0576 0.251 Uiso 1 1 calc R . .
C23 C 0.4744(17) 0.8167(13) 0.5229(9) 0.185(6) Uani 1 1 d U . .
H23A H 0.5632 0.8276 0.5116 0.277 Uiso 1 1 calc R . .
H23B H 0.4275 0.8326 0.4699 0.277 Uiso 1 1 calc R . .
H23C H 0.4212 0.7346 0.5358 0.277 Uiso 1 1 calc R . .
C22 C 0.367(2) 0.8781(19) 0.6109(14) 0.248(9) Uani 1 1 d U . .
H22A H 0.2950 0.8164 0.5674 0.371 Uiso 1 1 calc R . .
H22B H 0.3624 0.9537 0.6071 0.371 Uiso 1 1 calc R . .
H22C H 0.3567 0.8542 0.6713 0.371 Uiso 1 1 calc R . .
O1W O 1.0000 0.0000 -0.5000 0.287(10) Uani 1 2 d SU . .


_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
Tb1 O2 2.301(3) . ?
Tb1 O3 2.337(3) 2_655 ?
Tb1 O6 2.361(3) . ?
Tb1 O4 2.365(3) . ?
Tb1 O1 2.398(3) 2_655 ?
Tb1 O5 2.398(3) . ?
Tb1 O7 2.491(4) . ?
Tb1 O8 2.491(4) . ?
Tb1 N5 2.908(4) . ?
I1 Cu1 2.6101(7) . ?
I1 Cu1 2.6329(7) 2_666 ?
Cu1 N2 2.078(4) 1_565 ?
Cu1 N1 2.087(4) . ?
Cu1 I1 2.6329(7) 2_666 ?
Cu1 Cu1 2.6846(11) 2_666 ?
O4 C12 1.249(5) . ?
O3 C12 1.259(5) . ?
O3 Tb1 2.337(3) 2_655 ?
O2 C4 1.255(5) . ?
O1 C4 1.250(5) . ?
O1 Tb1 2.398(3) 2_655 ?
O5 C15 1.239(6) . ?
O6 C18 1.247(6) . ?
N2 C7 1.334(6) . ?
N2 C11 1.339(6) . ?
N2 Cu1 2.078(4) 1_545 ?
N1 C1 1.337(6) . ?
N1 C6 1.337(6) . ?
O7 N5 1.257(6) . ?
O8 N5 1.252(6) . ?
C9 C10 1.372(7) . ?
C9 C8 1.382(6) . ?
C9 C12 1.512(6) . ?
C8 C7 1.376(6) . ?
N4 C18 1.305(6) . ?
N4 C16 1.447(8) . ?
N4 C17 1.454(8) . ?
C4 C3 1.507(6) . ?
C3 C5 1.378(7) . ?
C3 C2 1.389(6) . ?
N5 O9 1.217(6) . ?
C2 C1 1.383(7) . ?
C10 C11 1.378(7) . ?
C5 C6 1.383(7) . ?
N6 C21 1.306(9) . ?
N6 C20 1.429(9) . ?
N6 C19 1.444(9) . ?
N3 C15 1.313(7) . ?
N3 C13 1.457(11) . ?
N3 C14 1.464(8) . ?
N7 C23 1.332(14) . ?
N7 C24 1.344(9) . ?
N7 C22 1.369(18) . ?
O10 C21 1.228(9) . ?
O11 C24 1.127(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
O2 Tb1 O3 78.09(11) . 2_655 ?
O2 Tb1 O6 147.60(12) . . ?
O3 Tb1 O6 77.34(11) 2_655 . ?
O2 Tb1 O4 76.86(11) . . ?
O3 Tb1 O4 127.82(11) 2_655 . ?
O6 Tb1 O4 135.39(12) . . ?
O2 Tb1 O1 124.05(11) . 2_655 ?
O3 Tb1 O1 80.70(11) 2_655 2_655 ?
O6 Tb1 O1 71.89(11) . 2_655 ?
O4 Tb1 O1 76.79(11) . 2_655 ?
O2 Tb1 O5 77.78(13) . . ?
O3 Tb1 O5 76.32(12) 2_655 . ?
O6 Tb1 O5 76.14(13) . . ?
O4 Tb1 O5 139.21(12) . . ?
O1 Tb1 O5 143.91(12) 2_655 . ?
O2 Tb1 O7 83.49(13) . . ?
O3 Tb1 O7 145.58(12) 2_655 . ?
O6 Tb1 O7 105.81(13) . . ?
O4 Tb1 O7 74.34(13) . . ?
O1 Tb1 O7 133.38(12) 2_655 . ?
O5 Tb1 O7 71.48(13) . . ?
O2 Tb1 O8 131.84(12) . . ?
O3 Tb1 O8 148.21(12) 2_655 . ?
O6 Tb1 O8 70.94(13) . . ?
O4 Tb1 O8 76.80(13) . . ?
O1 Tb1 O8 87.47(12) 2_655 . ?
O5 Tb1 O8 97.65(15) . . ?
O7 Tb1 O8 50.78(13) . . ?
O2 Tb1 N5 107.77(14) . . ?
O3 Tb1 N5 158.40(13) 2_655 . ?
O6 Tb1 N5 88.55(14) . . ?
O4 Tb1 N5 73.57(13) . . ?
O1 Tb1 N5 110.61(13) 2_655 . ?
O5 Tb1 N5 84.53(14) . . ?
O7 Tb1 N5 25.45(13) . . ?
O8 Tb1 N5 25.34(13) . . ?
Cu1 I1 Cu1 61.60(2) . 2_666 ?
N2 Cu1 N1 100.42(16) 1_565 . ?
N2 Cu1 I1 109.57(11) 1_565 . ?
N1 Cu1 I1 109.66(11) . . ?
N2 Cu1 I1 107.77(11) 1_565 2_666 ?
N1 Cu1 I1 109.51(11) . 2_666 ?
I1 Cu1 I1 118.40(2) . 2_666 ?
N2 Cu1 Cu1 128.67(12) 1_565 2_666 ?
N1 Cu1 Cu1 130.89(12) . 2_666 ?
I1 Cu1 Cu1 59.62(2) . 2_666 ?
I1 Cu1 Cu1 58.78(2) 2_666 2_666 ?
C12 O4 Tb1 138.0(3) . . ?
C12 O3 Tb1 139.0(3) . 2_655 ?
C4 O2 Tb1 178.8(3) . . ?
C4 O1 Tb1 111.8(3) . 2_655 ?
C15 O5 Tb1 130.3(3) . . ?
C18 O6 Tb1 127.9(3) . . ?
C7 N2 C11 116.8(4) . . ?
C7 N2 Cu1 121.1(3) . 1_545 ?
C11 N2 Cu1 121.4(3) . 1_545 ?
C1 N1 C6 117.0(4) . . ?
C1 N1 Cu1 123.2(3) . . ?
C6 N1 Cu1 119.6(3) . . ?
N5 O7 Tb1 96.2(3) . . ?
N5 O8 Tb1 96.3(3) . . ?
C10 C9 C8 117.4(4) . . ?
C10 C9 C12 121.2(4) . . ?
C8 C9 C12 121.4(4) . . ?
C7 C8 C9 119.4(4) . . ?
C18 N4 C16 120.9(5) . . ?
C18 N4 C17 121.4(5) . . ?
C16 N4 C17 117.6(5) . . ?
O1 C4 O2 123.5(4) . . ?
O1 C4 C3 118.4(4) . . ?
O2 C4 C3 118.1(4) . . ?
O4 C12 O3 126.8(4) . . ?
O4 C12 C9 117.2(4) . . ?
O3 C12 C9 116.0(4) . . ?
C5 C3 C2 117.9(4) . . ?
C5 C3 C4 120.9(4) . . ?
C2 C3 C4 121.2(4) . . ?
O9 N5 O8 121.5(5) . . ?
O9 N5 O7 121.8(6) . . ?
O8 N5 O7 116.7(4) . . ?
O9 N5 Tb1 179.1(6) . . ?
O8 N5 Tb1 58.4(2) . . ?
O7 N5 Tb1 58.4(2) . . ?
C1 C2 C3 119.0(4) . . ?
C9 C10 C11 120.0(5) . . ?
C3 C5 C6 119.3(4) . . ?
N1 C1 C2 123.4(4) . . ?
C21 N6 C20 120.1(6) . . ?
C21 N6 C19 122.9(7) . . ?
C20 N6 C19 116.9(6) . . ?
N2 C7 C8 123.4(4) . . ?
N1 C6 C5 123.3(4) . . ?
C15 N3 C13 118.7(6) . . ?
C15 N3 C14 122.5(6) . . ?
C13 N3 C14 118.7(6) . . ?
O6 C18 N4 123.9(5) . . ?
O5 C15 N3 125.2(6) . . ?
N2 C11 C10 122.9(5) . . ?
C23 N7 C24 116.2(12) . . ?
C23 N7 C22 111.0(12) . . ?
C24 N7 C22 132.8(13) . . ?
O10 C21 N6 125.4(8) . . ?
O11 C24 N7 132.6(17) . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        24.82
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         1.246
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.120
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1430394'
_audit_update_record             
;
2015-10-09 deposited with the CCDC.
2017-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            9-Dy
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H72 Cu2 Dy2 I2 N14 O23'
_chemical_formula_weight         1919.08

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.1272(5)
_cell_length_b                   12.4509(6)
_cell_length_c                   15.1320(7)
_cell_angle_alpha                81.3650(10)
_cell_angle_beta                 82.8470(10)
_cell_angle_gamma                63.9260(10)
_cell_volume                     1857.69(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.100
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             938
_exptl_absorpt_coefficient_mu    3.458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13830
_diffrn_reflns_av_R_equivalents  0.0142
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         24.80
_reflns_number_total             6221
_reflns_number_gt                5859
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0365P)²+5.8943P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6221
_refine_ls_number_parameters     412
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0222
_refine_ls_wR_factor_ref         0.0713
_refine_ls_wR_factor_gt          0.0698
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.903431(17) -0.113025(15) 0.036986(11) 0.01971(7) Uani 1 1 d . . .
Cu1 Cu 0.51511(5) 0.49889(5) 0.41119(3) 0.02763(12) Uani 1 1 d . . .
I1 I 0.65238(3) 0.57534(3) 0.491388(18) 0.03353(9) Uani 1 1 d . . .
O1 O 1.2560(3) -0.0511(2) 0.05080(19) 0.0290(6) Uani 1 1 d . . .
O2 O 1.1016(3) -0.1211(3) 0.07106(19) 0.0308(7) Uani 1 1 d . . .
O3 O 0.9763(3) 0.1351(3) 0.10137(18) 0.0280(6) Uani 1 1 d . . .
O4 O 0.8354(3) 0.0472(3) 0.12410(19) 0.0301(7) Uani 1 1 d . . .
O5 O 1.0449(3) -0.3228(3) 0.0454(2) 0.0402(8) Uani 1 1 d . . .
O6 O 0.7938(3) -0.1887(3) -0.0420(2) 0.0333(7) Uani 1 1 d . . .
O7 O 0.8990(3) -0.2001(3) 0.1954(2) 0.0436(8) Uani 1 1 d . . .
O8 O 0.7122(3) -0.1260(3) 0.1330(2) 0.0447(8) Uani 1 1 d . . .
O9 O 0.7210(5) -0.1993(6) 0.2723(3) 0.0924(18) Uani 1 1 d . . .
O10 O 0.9040(6) 0.6062(4) 0.8144(3) 0.0879(17) Uani 1 1 d . . .
O11 O 0.8799(8) -0.0446(7) 0.6884(6) 0.164(4) Uani 1 1 d D . .
N1 N 1.4143(4) -0.3714(3) 0.3098(2) 0.0296(8) Uani 1 1 d . . .
N2 N 0.6455(4) 0.3603(3) 0.3380(2) 0.0298(8) Uani 1 1 d . . .
N3 N 1.1954(5) -0.4796(4) -0.0267(3) 0.0479(11) Uani 1 1 d . . .
N4 N 0.6373(4) -0.1333(4) -0.1423(3) 0.0397(9) Uani 1 1 d . . .
N5 N 0.7755(4) -0.1761(4) 0.2025(3) 0.0433(10) Uani 1 1 d . . .
N6 N 0.9485(5) 0.5384(4) 0.6777(3) 0.0470(11) Uani 1 1 d . . .
N7 N 0.9029(6) 0.1071(4) 0.5915(3) 0.0623(14) Uani 1 1 d D . .
C1 C 1.4572(4) -0.2911(4) 0.2675(3) 0.0329(10) Uani 1 1 d . . .
H1A H 1.5336 -0.2892 0.2878 0.039 Uiso 1 1 calc R . .
C2 C 1.3957(4) -0.2106(4) 0.1954(3) 0.0313(9) Uani 1 1 d . . .
H2A H 1.4303 -0.1558 0.1667 0.038 Uiso 1 1 calc R . .
C3 C 1.2831(4) -0.2110(3) 0.1656(3) 0.0247(8) Uani 1 1 d . . .
C4 C 1.2381(5) -0.2938(4) 0.2088(3) 0.0347(10) Uani 1 1 d . . .
H4A H 1.1615 -0.2971 0.1902 0.042 Uiso 1 1 calc R . .
C5 C 1.3065(5) -0.3715(4) 0.2795(3) 0.0382(11) Uani 1 1 d . . .
H5A H 1.2751 -0.4284 0.3083 0.046 Uiso 1 1 calc R . .
C6 C 1.2087(4) -0.1217(3) 0.0900(3) 0.0251(9) Uani 1 1 d . . .
C7 C 0.7608(4) 0.3589(4) 0.2995(3) 0.0317(10) Uani 1 1 d . . .
H7A H 0.7902 0.4137 0.3162 0.038 Uiso 1 1 calc R . .
C8 C 0.8400(4) 0.2822(4) 0.2367(3) 0.0314(10) Uani 1 1 d . . .
H8A H 0.9215 0.2845 0.2114 0.038 Uiso 1 1 calc R . .
C9 C 0.7987(4) 0.2021(4) 0.2114(3) 0.0250(8) Uani 1 1 d . . .
C10 C 0.6822(5) 0.1995(5) 0.2533(3) 0.0403(12) Uani 1 1 d . . .
H10A H 0.6526 0.1435 0.2394 0.048 Uiso 1 1 calc R . .
C11 C 0.6091(5) 0.2790(5) 0.3155(4) 0.0428(12) Uani 1 1 d . . .
H11A H 0.5293 0.2760 0.3437 0.051 Uiso 1 1 calc R . .
C12 C 0.8770(4) 0.1207(3) 0.1397(3) 0.0245(8) Uani 1 1 d . . .
C13 C 1.3031(8) -0.4976(8) 0.0284(7) 0.117(4) Uani 1 1 d . . .
H13A H 1.2702 -0.4349 0.0691 0.176 Uiso 1 1 calc R . .
H13B H 1.3787 -0.4934 -0.0103 0.176 Uiso 1 1 calc R . .
H13C H 1.3327 -0.5767 0.0635 0.176 Uiso 1 1 calc R . .
C14 C 1.2237(7) -0.5638(5) -0.0928(4) 0.0584(16) Uani 1 1 d . . .
H14A H 1.1432 -0.5405 -0.1250 0.088 Uiso 1 1 calc R . .
H14B H 1.2500 -0.6453 -0.0623 0.088 Uiso 1 1 calc R . .
H14C H 1.2968 -0.5620 -0.1355 0.088 Uiso 1 1 calc R . .
C15 C 1.0756(5) -0.3930(4) -0.0130(3) 0.0375(11) Uani 1 1 d . . .
H15A H 1.0076 -0.3831 -0.0500 0.045 Uiso 1 1 calc R . .
C16 C 0.5381(6) -0.1470(6) -0.0757(5) 0.0679(19) Uani 1 1 d . . .
H16A H 0.5749 -0.1704 -0.0166 0.102 Uiso 1 1 calc R . .
H16B H 0.5149 -0.2093 -0.0904 0.102 Uiso 1 1 calc R . .
H16C H 0.4576 -0.0706 -0.0750 0.102 Uiso 1 1 calc R . .
C17 C 0.6021(6) -0.0989(6) -0.2352(4) 0.0609(16) Uani 1 1 d . . .
H17A H 0.6777 -0.0929 -0.2727 0.091 Uiso 1 1 calc R . .
H17B H 0.5236 -0.0209 -0.2400 0.091 Uiso 1 1 calc R . .
H17C H 0.5813 -0.1597 -0.2553 0.091 Uiso 1 1 calc R . .
C18 C 0.7567(5) -0.1543(4) -0.1197(3) 0.0344(10) Uani 1 1 d . . .
H18A H 0.8180 -0.1426 -0.1653 0.041 Uiso 1 1 calc R . .
C19 C 0.9153(8) 0.6548(6) 0.6264(5) 0.074(2) Uani 1 1 d . . .
H19A H 0.8843 0.7171 0.6674 0.112 Uiso 1 1 calc R . .
H19B H 0.8442 0.6718 0.5869 0.112 Uiso 1 1 calc R . .
H19C H 0.9950 0.6542 0.5903 0.112 Uiso 1 1 calc R . .
C20 C 0.9965(6) 0.4349(5) 0.6280(4) 0.0519(13) Uani 1 1 d . . .
H20A H 1.0151 0.3622 0.6699 0.078 Uiso 1 1 calc R . .
H20B H 1.0788 0.4273 0.5920 0.078 Uiso 1 1 calc R . .
H20C H 0.9280 0.4452 0.5884 0.078 Uiso 1 1 calc R . .
C21 C 0.9389(7) 0.5253(5) 0.7660(4) 0.0586(16) Uani 1 1 d . . .
H21A H 0.9611 0.4463 0.7947 0.070 Uiso 1 1 calc R . .
C22 C 1.0190(14) 0.1129(18) 0.6100(11) 0.225(10) Uani 1 1 d . . .
H22A H 1.0590 0.0539 0.6610 0.338 Uiso 1 1 calc R . .
H22B H 0.9969 0.1938 0.6247 0.338 Uiso 1 1 calc R . .
H22C H 1.0828 0.0950 0.5575 0.338 Uiso 1 1 calc R . .
C23 C 0.8414(12) 0.1853(10) 0.5211(7) 0.142(4) Uani 1 1 d U . .
H23A H 0.7597 0.1780 0.5122 0.214 Uiso 1 1 calc R . .
H23B H 0.9020 0.1670 0.4670 0.214 Uiso 1 1 calc R . .
H23C H 0.8180 0.2676 0.5333 0.214 Uiso 1 1 calc R . .
C24 C 0.8551(12) 0.0320(8) 0.6367(7) 0.136(4) Uani 1 1 d DU . .
H24A H 0.7691 0.0523 0.6172 0.163 Uiso 1 1 calc R . .
O1W O 0.5000 0.0000 -0.5000 0.274(9) Uani 1 2 d SU . .


_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 O2 2.283(3) . ?
Dy1 O3 2.324(3) 2_755 ?
Dy1 O4 2.346(3) . ?
Dy1 O6 2.349(3) . ?
Dy1 O5 2.377(3) . ?
Dy1 O1 2.381(3) 2_755 ?
Dy1 O8 2.476(3) . ?
Dy1 O7 2.482(3) . ?
Dy1 N5 2.902(4) . ?
Cu1 N2 2.070(3) . ?
Cu1 N1 2.076(3) 1_465 ?
Cu1 I1 2.6073(6) . ?
Cu1 I1 2.6309(6) 2_666 ?
Cu1 Cu1 2.6695(10) 2_666 ?
I1 Cu1 2.6309(6) 2_666 ?
O1 C6 1.255(5) . ?
O1 Dy1 2.381(3) 2_755 ?
O2 C6 1.256(5) . ?
O3 C12 1.254(5) . ?
O3 Dy1 2.324(3) 2_755 ?
O4 C12 1.254(5) . ?
O5 C15 1.248(6) . ?
O6 C18 1.246(6) . ?
O7 N5 1.265(5) . ?
O8 N5 1.261(5) . ?
O9 N5 1.213(6) . ?
O10 C21 1.228(7) . ?
O11 C24 1.093(8) . ?
N1 C1 1.338(6) . ?
N1 C5 1.338(6) . ?
N1 Cu1 2.076(3) 1_645 ?
N2 C7 1.336(6) . ?
N2 C11 1.342(6) . ?
N3 C15 1.310(6) . ?
N3 C13 1.463(9) . ?
N3 C14 1.465(7) . ?
N4 C18 1.316(6) . ?
N4 C16 1.449(7) . ?
N4 C17 1.456(7) . ?
N6 C21 1.317(7) . ?
N6 C20 1.449(7) . ?
N6 C19 1.451(7) . ?
N7 C24 1.334(8) . ?
N7 C23 1.354(11) . ?
N7 C22 1.389(13) . ?
C1 C2 1.384(6) . ?
C2 C3 1.386(6) . ?
C3 C4 1.383(6) . ?
C3 C6 1.509(5) . ?
C4 C5 1.379(6) . ?
C7 C8 1.384(6) . ?
C8 C9 1.382(6) . ?
C9 C10 1.381(6) . ?
C9 C12 1.510(5) . ?
C10 C11 1.381(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O3 78.09(10) . 2_755 ?
O2 Dy1 O4 76.78(10) . . ?
O3 Dy1 O4 127.51(10) 2_755 . ?
O2 Dy1 O6 147.71(11) . . ?
O3 Dy1 O6 77.45(11) 2_755 . ?
O4 Dy1 O6 135.36(11) . . ?
O2 Dy1 O5 77.99(11) . . ?
O3 Dy1 O5 76.83(11) 2_755 . ?
O4 Dy1 O5 139.14(11) . . ?
O6 Dy1 O5 76.16(11) . . ?
O2 Dy1 O1 124.04(10) . 2_755 ?
O3 Dy1 O1 80.47(10) 2_755 2_755 ?
O4 Dy1 O1 76.83(10) . 2_755 ?
O6 Dy1 O1 71.74(10) . 2_755 ?
O5 Dy1 O1 143.91(11) . 2_755 ?
O2 Dy1 O8 131.73(11) . . ?
O3 Dy1 O8 148.34(11) 2_755 . ?
O4 Dy1 O8 76.96(11) . . ?
O6 Dy1 O8 70.96(11) . . ?
O5 Dy1 O8 97.18(12) . . ?
O1 Dy1 O8 87.68(11) 2_755 . ?
O2 Dy1 O7 82.70(11) . . ?
O3 Dy1 O7 145.68(10) 2_755 . ?
O4 Dy1 O7 73.85(11) . . ?
O6 Dy1 O7 106.76(12) . . ?
O5 Dy1 O7 71.49(11) . . ?
O1 Dy1 O7 133.65(10) 2_755 . ?
O8 Dy1 O7 51.28(11) . . ?
O2 Dy1 N5 107.31(12) . . ?
O3 Dy1 N5 158.87(11) 2_755 . ?
O4 Dy1 N5 73.36(11) . . ?
O6 Dy1 N5 89.05(12) . . ?
O5 Dy1 N5 84.25(12) . . ?
O1 Dy1 N5 110.90(11) 2_755 . ?
O8 Dy1 N5 25.59(11) . . ?
O7 Dy1 N5 25.70(11) . . ?
N2 Cu1 N1 101.11(14) . 1_465 ?
N2 Cu1 I1 109.35(10) . . ?
N1 Cu1 I1 109.51(10) 1_465 . ?
N2 Cu1 I1 107.33(10) . 2_666 ?
N1 Cu1 I1 109.35(10) 1_465 2_666 ?
I1 Cu1 I1 118.725(19) . 2_666 ?
N2 Cu1 Cu1 128.11(11) . 2_666 ?
N1 Cu1 Cu1 130.75(11) 1_465 2_666 ?
I1 Cu1 Cu1 59.80(2) . 2_666 ?
I1 Cu1 Cu1 58.93(2) 2_666 2_666 ?
Cu1 I1 Cu1 61.28(2) . 2_666 ?
C6 O1 Dy1 112.1(2) . 2_755 ?
C6 O2 Dy1 178.1(3) . . ?
C12 O3 Dy1 139.0(3) . 2_755 ?
C12 O4 Dy1 138.2(3) . . ?
C15 O5 Dy1 129.2(3) . . ?
C18 O6 Dy1 127.4(3) . . ?
N5 O7 Dy1 96.0(3) . . ?
N5 O8 Dy1 96.4(3) . . ?
C1 N1 C5 116.8(4) . . ?
C1 N1 Cu1 123.2(3) . 1_645 ?
C5 N1 Cu1 119.8(3) . 1_645 ?
C7 N2 C11 116.8(4) . . ?
C7 N2 Cu1 121.0(3) . . ?
C11 N2 Cu1 121.4(3) . . ?
C15 N3 C13 119.6(5) . . ?
C15 N3 C14 121.9(5) . . ?
C13 N3 C14 118.4(5) . . ?
C18 N4 C16 120.8(5) . . ?
C18 N4 C17 121.1(4) . . ?
C16 N4 C17 118.1(5) . . ?
O9 N5 O8 121.9(5) . . ?
O9 N5 O7 121.8(5) . . ?
O8 N5 O7 116.3(4) . . ?
O9 N5 Dy1 178.1(4) . . ?
O8 N5 Dy1 58.0(2) . . ?
O7 N5 Dy1 58.3(2) . . ?
C21 N6 C20 120.6(5) . . ?
C21 N6 C19 122.1(5) . . ?
C20 N6 C19 117.2(5) . . ?
C24 N7 C23 122.1(9) . . ?
C24 N7 C22 124.5(11) . . ?
C23 N7 C22 113.4(11) . . ?
N1 C1 C2 123.2(4) . . ?
C1 C2 C3 119.2(4) . . ?
C4 C3 C2 118.1(4) . . ?
C4 C3 C6 120.5(4) . . ?
C2 C3 C6 121.4(4) . . ?
C5 C4 C3 118.8(4) . . ?
N1 C5 C4 123.9(4) . . ?
O1 C6 O2 123.9(4) . . ?
O1 C6 C3 118.1(4) . . ?
O2 C6 C3 118.0(4) . . ?
N2 C7 C8 123.6(4) . . ?
C9 C8 C7 119.0(4) . . ?
C10 C9 C8 117.8(4) . . ?
C10 C9 C12 120.7(4) . . ?
C8 C9 C12 121.5(4) . . ?
C11 C10 C9 119.5(4) . . ?
N2 C11 C10 123.1(4) . . ?
O4 C12 O3 126.9(4) . . ?
O4 C12 C9 117.0(4) . . ?
O3 C12 C9 116.1(4) . . ?
O5 C15 N3 124.3(5) . . ?
O6 C18 N4 123.7(5) . . ?
O10 C21 N6 125.8(6) . . ?
O11 C24 N7 142.2(14) . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        24.80
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         1.671
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.112
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1430395'
_audit_update_record             
;
2015-10-09 deposited with the CCDC.
2017-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            9-Ho
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H72 Cu2 Ho2 I2 N14 O23'
_chemical_formula_weight         1923.94

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.1399(9)
_cell_length_b                   12.4564(10)
_cell_length_c                   15.1237(12)
_cell_angle_alpha                81.3200(10)
_cell_angle_beta                 82.7230(10)
_cell_angle_gamma                63.8830(10)
_cell_volume                     1858.5(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.056
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             940
_exptl_absorpt_coefficient_mu    3.575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13536
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         24.76
_reflns_number_total             6191
_reflns_number_gt                5867
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0388P)²+5.5671P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6191
_refine_ls_number_parameters     412
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0218
_refine_ls_wR_factor_ref         0.0719
_refine_ls_wR_factor_gt          0.0705
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.055
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.403528(16) 0.886586(15) 0.036968(11) 0.01982(7) Uani 1 1 d . . .
I1 I 0.15240(3) 1.57529(3) 0.491036(18) 0.03317(9) Uani 1 1 d . . .
Cu1 Cu 0.01528(5) 1.49876(5) 0.41106(3) 0.02778(12) Uani 1 1 d . . .
O3 O 0.4772(3) 1.1340(3) 0.10089(19) 0.0287(6) Uani 1 1 d . . .
O4 O 0.3360(3) 1.0464(3) 0.12359(19) 0.0301(6) Uani 1 1 d . . .
O2 O 0.6007(3) 0.8775(3) 0.0714(2) 0.0314(7) Uani 1 1 d . . .
O1 O 0.7533(3) 0.9496(2) 0.05055(19) 0.0284(6) Uani 1 1 d . . .
O5 O 0.5438(3) 0.6776(3) 0.0450(2) 0.0405(8) Uani 1 1 d . . .
O6 O 0.2940(3) 0.8115(3) -0.0416(2) 0.0336(7) Uani 1 1 d . . .
O7 O 0.3991(3) 0.7997(3) 0.1947(2) 0.0444(8) Uani 1 1 d . . .
O8 O 0.2124(3) 0.8753(3) 0.1326(2) 0.0449(8) Uani 1 1 d . . .
N2 N 0.1456(4) 1.3599(3) 0.3377(2) 0.0300(8) Uani 1 1 d . . .
N1 N 0.9143(3) 0.6284(3) 0.3096(2) 0.0294(8) Uani 1 1 d . . .
C9 C 0.2990(4) 1.2012(4) 0.2112(3) 0.0249(8) Uani 1 1 d . . .
N4 N 0.1373(4) 0.8666(4) -0.1414(3) 0.0405(9) Uani 1 1 d . . .
C8 C 0.3405(4) 1.2811(4) 0.2367(3) 0.0315(10) Uani 1 1 d . . .
H8A H 0.4222 1.2830 0.2116 0.038 Uiso 1 1 calc R . .
C12 C 0.3777(4) 1.1198(4) 0.1394(3) 0.0244(8) Uani 1 1 d . . .
C6 C 0.7072(4) 0.8781(4) 0.0898(3) 0.0243(8) Uani 1 1 d . . .
N5 N 0.2749(4) 0.8249(4) 0.2020(3) 0.0438(10) Uani 1 1 d . . .
C3 C 0.7822(4) 0.7891(4) 0.1655(3) 0.0247(8) Uani 1 1 d . . .
N6 N 0.4478(5) 0.5389(4) 0.6776(3) 0.0473(11) Uani 1 1 d . . .
C4 C 0.7384(5) 0.7054(4) 0.2088(3) 0.0356(10) Uani 1 1 d . . .
H4A H 0.6622 0.7016 0.1901 0.043 Uiso 1 1 calc R . .
C7 C 0.2611(4) 1.3581(4) 0.2995(3) 0.0314(9) Uani 1 1 d . . .
H7A H 0.2905 1.4127 0.3162 0.038 Uiso 1 1 calc R . .
C2 C 0.8950(4) 0.7899(4) 0.1952(3) 0.0316(9) Uani 1 1 d . . .
H2A H 0.9293 0.8449 0.1665 0.038 Uiso 1 1 calc R . .
N3 N 0.6947(4) 0.5210(4) -0.0275(3) 0.0478(11) Uani 1 1 d . . .
C10 C 0.1818(5) 1.1993(5) 0.2529(3) 0.0412(12) Uani 1 1 d . . .
H10A H 0.1519 1.1437 0.2388 0.049 Uiso 1 1 calc R . .
C15 C 0.5748(5) 0.6074(4) -0.0133(3) 0.0376(11) Uani 1 1 d . . .
H15A H 0.5068 0.6171 -0.0500 0.045 Uiso 1 1 calc R . .
C1 C 0.9564(4) 0.7094(4) 0.2671(3) 0.0324(10) Uani 1 1 d . . .
H1A H 1.0324 0.7117 0.2875 0.039 Uiso 1 1 calc R . .
C5 C 0.8066(5) 0.6276(4) 0.2793(3) 0.0386(11) Uani 1 1 d . . .
H5A H 0.7756 0.5703 0.3080 0.046 Uiso 1 1 calc R . .
C18 C 0.2564(5) 0.8462(4) -0.1192(3) 0.0348(10) Uani 1 1 d . . .
H18A H 0.3172 0.8586 -0.1649 0.042 Uiso 1 1 calc R . .
O9 O 0.2206(5) 0.8014(6) 0.2720(3) 0.0927(18) Uani 1 1 d . . .
N7 N 0.4032(6) 0.1072(4) 0.5914(3) 0.0628(14) Uani 1 1 d D . .
C11 C 0.1088(5) 1.2789(5) 0.3151(4) 0.0437(12) Uani 1 1 d . . .
H11A H 0.0287 1.2763 0.3432 0.052 Uiso 1 1 calc R . .
O10 O 0.4029(6) 0.6068(4) 0.8142(3) 0.0894(17) Uani 1 1 d . . .
C21 C 0.4389(7) 0.5257(6) 0.7660(4) 0.0596(16) Uani 1 1 d . . .
H21A H 0.4625 0.4466 0.7949 0.072 Uiso 1 1 calc R . .
C17 C 0.1023(6) 0.9010(6) -0.2346(4) 0.0608(16) Uani 1 1 d . . .
H17A H 0.1778 0.9074 -0.2722 0.091 Uiso 1 1 calc R . .
H17B H 0.0236 0.9788 -0.2393 0.091 Uiso 1 1 calc R . .
H17C H 0.0821 0.8400 -0.2548 0.091 Uiso 1 1 calc R . .
C14 C 0.7231(6) 0.4361(5) -0.0932(4) 0.0580(15) Uani 1 1 d . . .
H14A H 0.6426 0.4589 -0.1251 0.087 Uiso 1 1 calc R . .
H14B H 0.7496 0.3548 -0.0622 0.087 Uiso 1 1 calc R . .
H14C H 0.7960 0.4377 -0.1362 0.087 Uiso 1 1 calc R . .
C20 C 0.4961(6) 0.4351(5) 0.6283(4) 0.0530(14) Uani 1 1 d . . .
H20A H 0.5138 0.3627 0.6705 0.079 Uiso 1 1 calc R . .
H20B H 0.5790 0.4269 0.5928 0.079 Uiso 1 1 calc R . .
H20C H 0.4282 0.4454 0.5884 0.079 Uiso 1 1 calc R . .
C19 C 0.4155(8) 0.6549(6) 0.6262(5) 0.075(2) Uani 1 1 d . . .
H19A H 0.3842 0.7174 0.6671 0.113 Uiso 1 1 calc R . .
H19B H 0.3449 0.6720 0.5864 0.113 Uiso 1 1 calc R . .
H19C H 0.4956 0.6540 0.5903 0.113 Uiso 1 1 calc R . .
C16 C 0.0378(6) 0.8524(7) -0.0745(5) 0.0681(19) Uani 1 1 d . . .
H16A H 0.0743 0.8292 -0.0153 0.102 Uiso 1 1 calc R . .
H16B H 0.0152 0.7899 -0.0893 0.102 Uiso 1 1 calc R . .
H16C H -0.0430 0.9287 -0.0738 0.102 Uiso 1 1 calc R . .
O11 O 0.3792(9) -0.0444(7) 0.6881(6) 0.165(4) Uani 1 1 d D . .
C13 C 0.8023(7) 0.5035(8) 0.0268(8) 0.119(4) Uani 1 1 d . . .
H13A H 0.7696 0.5665 0.0672 0.179 Uiso 1 1 calc R . .
H13B H 0.8776 0.5075 -0.0124 0.179 Uiso 1 1 calc R . .
H13C H 0.8320 0.4246 0.0622 0.179 Uiso 1 1 calc R . .
C24 C 0.3569(12) 0.0318(8) 0.6365(7) 0.135(4) Uani 1 1 d DU . .
H24A H 0.2716 0.0520 0.6162 0.162 Uiso 1 1 calc R . .
C23 C 0.3414(13) 0.1858(11) 0.5211(7) 0.144(4) Uani 1 1 d U . .
H23A H 0.2602 0.1781 0.5119 0.216 Uiso 1 1 calc R . .
H23B H 0.4021 0.1683 0.4669 0.216 Uiso 1 1 calc R . .
H23C H 0.3173 0.2680 0.5337 0.216 Uiso 1 1 calc R . .
C22 C 0.5190(14) 0.1137(18) 0.6097(12) 0.227(10) Uani 1 1 d . . .
H22A H 0.5596 0.0545 0.6604 0.340 Uiso 1 1 calc R . .
H22B H 0.4963 0.1945 0.6247 0.340 Uiso 1 1 calc R . .
H22C H 0.5825 0.0966 0.5568 0.340 Uiso 1 1 calc R . .
O1W O 0.0000 1.0000 -0.5000 0.379(19) Uani 1 2 d S . .


_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 O2 2.272(3) . ?
Ho1 O3 2.311(3) 2_675 ?
Ho1 O4 2.338(3) . ?
Ho1 O6 2.341(3) . ?
Ho1 O1 2.367(3) 2_675 ?
Ho1 O5 2.367(3) . ?
Ho1 O8 2.463(3) . ?
Ho1 O7 2.470(3) . ?
Ho1 N5 2.892(4) . ?
I1 Cu1 2.6082(6) . ?
I1 Cu1 2.6338(6) 2_586 ?
Cu1 N2 2.071(3) . ?
Cu1 N1 2.078(3) 1_465 ?
Cu1 I1 2.6338(6) 2_586 ?
Cu1 Cu1 2.6716(10) 2_586 ?
O3 C12 1.256(5) . ?
O3 Ho1 2.311(3) 2_675 ?
O4 C12 1.255(5) . ?
O2 C6 1.255(5) . ?
O1 C6 1.255(5) . ?
O1 Ho1 2.367(3) 2_675 ?
O5 C15 1.245(6) . ?
O6 C18 1.246(6) . ?
O7 N5 1.271(5) . ?
O8 N5 1.258(5) . ?
N2 C7 1.335(6) . ?
N2 C11 1.344(6) . ?
N1 C1 1.340(6) . ?
N1 C5 1.343(6) . ?
N1 Cu1 2.078(3) 1_645 ?
C9 C10 1.384(6) . ?
C9 C8 1.385(6) . ?
C9 C12 1.511(5) . ?
N4 C18 1.315(6) . ?
N4 C16 1.456(7) . ?
N4 C17 1.459(7) . ?
C8 C7 1.385(6) . ?
C6 C3 1.510(5) . ?
N5 O9 1.214(6) . ?
C3 C4 1.384(6) . ?
C3 C2 1.392(6) . ?
N6 C21 1.319(7) . ?
N6 C20 1.447(7) . ?
N6 C19 1.448(7) . ?
C4 C5 1.378(6) . ?
C2 C1 1.383(6) . ?
N3 C15 1.311(6) . ?
N3 C13 1.457(9) . ?
N3 C14 1.466(7) . ?
C10 C11 1.381(7) . ?
N7 C24 1.325(8) . ?
N7 C23 1.356(11) . ?
N7 C22 1.391(13) . ?
O10 C21 1.226(7) . ?
O11 C24 1.091(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
O2 Ho1 O3 78.22(10) . 2_675 ?
O2 Ho1 O4 76.76(10) . . ?
O3 Ho1 O4 126.98(10) 2_675 . ?
O2 Ho1 O6 147.79(11) . . ?
O3 Ho1 O6 77.75(11) 2_675 . ?
O4 Ho1 O6 135.31(11) . . ?
O2 Ho1 O1 123.89(11) . 2_675 ?
O3 Ho1 O1 79.96(10) 2_675 2_675 ?
O4 Ho1 O1 76.64(10) . 2_675 ?
O6 Ho1 O1 72.05(10) . 2_675 ?
O2 Ho1 O5 77.92(11) . . ?
O3 Ho1 O5 77.17(11) 2_675 . ?
O4 Ho1 O5 139.34(11) . . ?
O6 Ho1 O5 76.08(11) . . ?
O1 Ho1 O5 143.94(11) 2_675 . ?
O2 Ho1 O8 131.54(11) . . ?
O3 Ho1 O8 148.60(11) 2_675 . ?
O4 Ho1 O8 76.82(11) . . ?
O6 Ho1 O8 70.97(11) . . ?
O1 Ho1 O8 87.79(11) 2_675 . ?
O5 Ho1 O8 97.50(13) . . ?
O2 Ho1 O7 82.34(11) . . ?
O3 Ho1 O7 145.90(11) 2_675 . ?
O4 Ho1 O7 74.03(11) . . ?
O6 Ho1 O7 106.73(12) . . ?
O1 Ho1 O7 134.00(10) 2_675 . ?
O5 Ho1 O7 71.49(12) . . ?
O8 Ho1 O7 51.53(11) . . ?
O2 Ho1 N5 107.13(12) . . ?
O3 Ho1 N5 159.46(11) 2_675 . ?
O4 Ho1 N5 73.34(11) . . ?
O6 Ho1 N5 88.99(12) . . ?
O1 Ho1 N5 111.03(11) 2_675 . ?
O5 Ho1 N5 84.51(12) . . ?
O8 Ho1 N5 25.61(12) . . ?
O7 Ho1 N5 25.93(11) . . ?
Cu1 I1 Cu1 61.28(2) . 2_586 ?
N2 Cu1 N1 101.11(14) . 1_465 ?
N2 Cu1 I1 109.41(10) . . ?
N1 Cu1 I1 109.57(10) 1_465 . ?
N2 Cu1 I1 107.31(10) . 2_586 ?
N1 Cu1 I1 109.26(10) 1_465 2_586 ?
I1 Cu1 I1 118.72(2) . 2_586 ?
N2 Cu1 Cu1 128.16(11) . 2_586 ?
N1 Cu1 Cu1 130.71(11) 1_465 2_586 ?
I1 Cu1 Cu1 59.83(2) . 2_586 ?
I1 Cu1 Cu1 58.89(2) 2_586 2_586 ?
C12 O3 Ho1 139.2(3) . 2_675 ?
C12 O4 Ho1 138.4(3) . . ?
C6 O2 Ho1 177.2(3) . . ?
C6 O1 Ho1 113.1(2) . 2_675 ?
C15 O5 Ho1 129.5(3) . . ?
C18 O6 Ho1 127.5(3) . . ?
N5 O7 Ho1 95.9(3) . . ?
N5 O8 Ho1 96.6(3) . . ?
C7 N2 C11 116.9(4) . . ?
C7 N2 Cu1 120.9(3) . . ?
C11 N2 Cu1 121.4(3) . . ?
C1 N1 C5 116.8(4) . . ?
C1 N1 Cu1 123.4(3) . 1_645 ?
C5 N1 Cu1 119.6(3) . 1_645 ?
C10 C9 C8 117.8(4) . . ?
C10 C9 C12 120.9(4) . . ?
C8 C9 C12 121.3(4) . . ?
C18 N4 C16 121.1(5) . . ?
C18 N4 C17 120.8(4) . . ?
C16 N4 C17 118.0(4) . . ?
C7 C8 C9 119.0(4) . . ?
O4 C12 O3 126.8(4) . . ?
O4 C12 C9 116.9(4) . . ?
O3 C12 C9 116.3(4) . . ?
O2 C6 O1 124.1(4) . . ?
O2 C6 C3 117.7(4) . . ?
O1 C6 C3 118.2(3) . . ?
O9 N5 O8 122.4(5) . . ?
O9 N5 O7 121.6(5) . . ?
O8 N5 O7 116.0(4) . . ?
O9 N5 Ho1 178.5(4) . . ?
O8 N5 Ho1 57.8(2) . . ?
O7 N5 Ho1 58.2(2) . . ?
C4 C3 C2 117.9(4) . . ?
C4 C3 C6 120.5(4) . . ?
C2 C3 C6 121.5(4) . . ?
C21 N6 C20 120.3(5) . . ?
C21 N6 C19 122.2(5) . . ?
C20 N6 C19 117.4(5) . . ?
C5 C4 C3 119.3(4) . . ?
N2 C7 C8 123.6(4) . . ?
C1 C2 C3 119.0(4) . . ?
C15 N3 C13 119.5(5) . . ?
C15 N3 C14 122.1(5) . . ?
C13 N3 C14 118.2(5) . . ?
C11 C10 C9 119.5(4) . . ?
O5 C15 N3 124.6(5) . . ?
N1 C1 C2 123.5(4) . . ?
N1 C5 C4 123.6(4) . . ?
O6 C18 N4 123.8(4) . . ?
C24 N7 C23 122.6(10) . . ?
C24 N7 C22 124.3(11) . . ?
C23 N7 C22 113.1(11) . . ?
N2 C11 C10 123.1(4) . . ?
O10 C21 N6 125.6(6) . . ?
O11 C24 N7 144.1(14) . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        24.76
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         1.464
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.115
####################################################################### 
# 
# 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_1
_audit_block_doi                 10.5517/ccdc.csd.cc1jnfp9
_database_code_depnum_ccdc_archive 'CCDC 1419821'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C6CE00540C 2016
_audit_update_record             
;
2016-09-01 deposited with the CCDC.
2017-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            2-Pr
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H40 Cu8 I8 N8 Na2 O25 Pr2'
_chemical_formula_weight         2980.20

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   C222(1)

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

_cell_length_a                   17.8961(19)
_cell_length_b                   31.932(3)
_cell_length_c                   25.078(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     14331(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9666
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      24.76

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.042
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5520
_exptl_absorpt_coefficient_mu    3.597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41369
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.28
_diffrn_reflns_theta_max         24.76
_reflns_number_total             11762
_reflns_number_gt                9807
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0730P)²+836.3642P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         11762
_refine_ls_number_parameters     440
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0862
_refine_ls_wR_factor_ref         0.2290
_refine_ls_wR_factor_gt          0.2128
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.31542(6) 0.89231(3) 0.04219(6) 0.0554(3) Uani 1 1 d . . .
Cu4 Cu 0.82951(15) 1.11097(7) 0.11373(13) 0.0621(8) Uani 1 1 d . . .
Cu3 Cu 0.81403(17) 1.05872(9) 0.19474(11) 0.0612(7) Uani 1 1 d . . .
Cu2 Cu 0.87351(13) 1.03256(8) 0.10675(14) 0.0608(7) Uani 1 1 d . . .
Cu1 Cu 0.73259(13) 1.05158(9) 0.10636(14) 0.0621(8) Uani 1 1 d . . .
I2 I 0.81692(8) 1.06941(4) 0.02141(6) 0.0582(4) Uani 1 1 d . . .
I4 I 0.94519(7) 1.09365(4) 0.17325(7) 0.0550(4) Uani 1 1 d . . .
I3 I 0.69434(8) 1.11157(5) 0.17179(7) 0.0672(4) Uani 1 1 d . . .
I1 I 0.78992(7) 0.98112(4) 0.16465(7) 0.0615(4) Uani 1 1 d . . .
O1 O 0.1758(9) 0.8960(4) 0.0732(8) 0.074(5) Uani 1 1 d . . .
O1W O 0.438(4) 0.871(2) 0.872(3) 0.17(3) Uani 0.50 1 d PU . .
O1W' O 0.362(4) 0.839(2) 0.885(3) 0.19(3) Uani 0.50 1 d PU . .
O2 O 0.2256(7) 0.9546(3) 0.0453(7) 0.057(4) Uani 1 1 d . . .
O2W O 0.511(4) 0.848(2) 0.118(3) 0.17(2) Uani 0.50 1 d PU . .
O3 O 0.3213(7) 0.9352(4) -0.0456(6) 0.050(3) Uani 1 1 d . . .
O3W O 0.184(7) 0.784(3) 0.922(4) 0.28(5) Uani 0.50 1 d PU . .
O4 O 0.2321(8) 0.8869(5) -0.0392(7) 0.070(4) Uani 1 1 d . . .
O5 O 0.3835(7) 0.9624(4) 0.0553(7) 0.052(4) Uani 1 1 d . . .
O6 O 0.4542(8) 0.9077(5) 0.0487(8) 0.076(5) Uani 1 1 d . . .
O6W O 0.0000 0.973(3) 0.2500 0.37(5) Uani 1 2 d SU . .
O7 O 0.2637(9) 0.8195(5) 0.0452(10) 0.098(7) Uani 1 1 d . . .
O8 O 0.3690(12) 0.8288(5) 0.0892(11) 0.113(9) Uani 1 1 d . . .
O9 O 0.3823(12) 0.8496(6) -0.0280(12) 0.125(9) Uani 1 1 d . . .
H9A H 0.3843 0.8242 -0.0181 0.150 Uiso 1 1 d R . .
H9B H 0.3586 0.8512 -0.0573 0.150 Uiso 1 1 d R . .
O10 O 0.3129(14) 0.9068(7) 0.1394(9) 0.120(8) Uani 1 1 d . . .
H10A H 0.3147 0.8838 0.1564 0.145 Uiso 1 1 d R . .
H10C H 0.3505 0.9218 0.1475 0.145 Uiso 1 1 d R . .
N1 N -0.0345(5) 1.0001(3) 0.0866(6) 0.054(5) Uani 1 1 d G . .
C1 C -0.0308(6) 0.9571(3) 0.0943(7) 0.069(7) Uani 1 1 d G . .
H1B H -0.0742 0.9420 0.1048 0.082 Uiso 1 1 calc R . .
C2 C 0.0364(7) 0.9360(3) 0.0869(8) 0.078(8) Uani 1 1 d G . .
H2A H 0.0389 0.9066 0.0922 0.094 Uiso 1 1 calc R . .
C3 C 0.0999(6) 0.9581(4) 0.0716(7) 0.057(6) Uani 1 1 d G . .
C4 C 0.0962(5) 1.0011(4) 0.0638(7) 0.066(7) Uani 1 1 d G . .
H4A H 0.1395 1.0162 0.0534 0.080 Uiso 1 1 calc R . .
C5 C 0.0289(6) 1.0221(3) 0.0713(7) 0.074(8) Uani 1 1 d G . .
H5A H 0.0264 1.0516 0.0660 0.088 Uiso 1 1 calc R . .
C6 C 0.1733(10) 0.9328(7) 0.0629(9) 0.058(6) Uani 1 1 d . . .
N2 N 0.1973(7) 0.9402(4) -0.2252(4) 0.056(4) Uani 1 1 d G . .
C7 C 0.2503(7) 0.9659(4) -0.2013(6) 0.065(7) Uani 1 1 d G . .
H7A H 0.2720 0.9883 -0.2209 0.078 Uiso 1 1 calc R . .
C8 C 0.2717(7) 0.9588(4) -0.1488(5) 0.063(6) Uani 1 1 d G . .
H8A H 0.3080 0.9763 -0.1325 0.076 Uiso 1 1 calc R . .
C9 C 0.2400(8) 0.9260(5) -0.1202(4) 0.059(6) Uani 1 1 d G . .
C10 C 0.1869(8) 0.9004(4) -0.1440(5) 0.059(5) Uani 1 1 d G . .
H10B H 0.1652 0.8780 -0.1245 0.071 Uiso 1 1 calc R . .
C11 C 0.1655(7) 0.9075(4) -0.1966(5) 0.071(7) Uani 1 1 d G . .
H11A H 0.1293 0.8899 -0.2129 0.085 Uiso 1 1 calc R . .
C12 C 0.2624(12) 0.9157(6) -0.0645(11) 0.067(7) Uani 1 1 d . . .
N3 N 0.6395(5) 1.0216(3) 0.0821(6) 0.063(5) Uani 1 1 d G . .
C13 C 0.5687(6) 1.0381(3) 0.0905(6) 0.045(5) Uani 1 1 d G . .
H13A H 0.5633 1.0661 0.1029 0.054 Uiso 1 1 calc R . .
C14 C 0.5057(4) 1.0138(3) 0.0808(6) 0.047(5) Uani 1 1 d G . .
H14A H 0.4573 1.0251 0.0866 0.056 Uiso 1 1 calc R . .
C15 C 0.5136(5) 0.9729(3) 0.0627(6) 0.045(5) Uani 1 1 d G . .
C16 C 0.5845(6) 0.9563(3) 0.0543(6) 0.064(6) Uani 1 1 d G . .
H16A H 0.5899 0.9284 0.0419 0.077 Uiso 1 1 calc R . .
C17 C 0.6474(5) 0.9807(4) 0.0640(6) 0.056(6) Uani 1 1 d G . .
H17A H 0.6959 0.9694 0.0582 0.067 Uiso 1 1 calc R . .
C18 C 0.4458(11) 0.9444(6) 0.0588(8) 0.043(4) Uani 1 1 d . . .
N4 N 0.3353(8) 0.6722(3) 0.0939(7) 0.066(6) Uani 1 1 d G . .
C19 C 0.2802(7) 0.6882(3) 0.0605(6) 0.062(6) Uani 1 1 d GU . .
H19A H 0.2468 0.6697 0.0429 0.074 Uiso 1 1 calc R . .
C20 C 0.2742(8) 0.7312(4) 0.0529(6) 0.080(7) Uani 1 1 d GU . .
H20A H 0.2365 0.7421 0.0301 0.096 Uiso 1 1 calc R . .
C21 C 0.3231(9) 0.7582(3) 0.0788(7) 0.052(5) Uani 1 1 d GU . .
C22 C 0.3782(10) 0.7422(4) 0.1122(8) 0.130(16) Uani 1 1 d G . .
H22A H 0.4117 0.7607 0.1298 0.156 Uiso 1 1 calc R . .
C23 C 0.3843(9) 0.6992(4) 0.1197(8) 0.111(14) Uani 1 1 d G . .
H23A H 0.4219 0.6883 0.1425 0.133 Uiso 1 1 calc R . .
C24 C 0.3157(14) 0.8050(8) 0.0707(12) 0.075(7) Uani 1 1 d . . .
Na1 Na 0.3070(5) 1.0000 0.0000 0.047(3) Uani 1 2 d S . .
Na2 Na 0.030(5) 0.826(3) 0.020(4) 0.06(2) Uani 0.10 1 d PU . .
Na2' Na 0.057(4) 0.845(2) -0.026(3) 0.22(3) Uani 0.40 1 d PU . .


_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
Pr1 O10 2.48(2) . ?
Pr1 O7 2.503(16) . ?
Pr1 O9 2.53(2) . ?
Pr1 O4 2.532(15) . ?
Pr1 O8 2.534(17) . ?
Pr1 O6 2.537(15) . ?
Pr1 O2 2.558(11) . ?
Pr1 O5 2.569(12) . ?
Pr1 O3 2.594(13) . ?
Pr1 O1 2.620(15) . ?
Pr1 C24 2.88(2) . ?
Pr1 C18 2.895(19) . ?
Cu4 N4 2.020(9) 5 ?
Cu4 Cu1 2.577(3) . ?
Cu4 I4 2.611(3) . ?
Cu4 Cu2 2.631(3) . ?
Cu4 Cu3 2.643(4) . ?
Cu4 I2 2.678(3) . ?
Cu4 I3 2.823(3) . ?
Cu3 N2 2.018(11) 2_675 ?
Cu3 Cu2 2.588(4) . ?
Cu3 I1 2.626(3) . ?
Cu3 I4 2.654(3) . ?
Cu3 Cu1 2.662(4) . ?
Cu3 I3 2.787(3) . ?
Cu2 N1 2.009(9) 1_655 ?
Cu2 Cu1 2.594(3) . ?
Cu2 I2 2.644(4) . ?
Cu2 I1 2.654(3) . ?
Cu2 I4 2.869(3) . ?
Cu1 N3 2.015(8) . ?
Cu1 I3 2.613(3) . ?
Cu1 I2 2.672(4) . ?
Cu1 I1 2.872(3) . ?
O1 C6 1.20(3) . ?
O1W O1W' 1.73(10) . ?
O2 C6 1.25(2) . ?
O2 Na1 2.349(14) . ?
O3 C12 1.31(2) . ?
O3 Na1 2.377(13) . ?
O4 C12 1.24(2) . ?
O5 C18 1.26(2) . ?
O5 Na1 2.290(14) . ?
O6 C18 1.21(2) . ?
O7 C24 1.22(3) . ?
O8 C24 1.30(3) . ?
N1 C1 1.3900 . ?
N1 C5 1.3900 . ?
N1 Cu2 2.009(9) 1_455 ?
C1 C2 1.3900 . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C3 C6 1.56(2) . ?
C4 C5 1.3900 . ?
N2 C7 1.3900 . ?
N2 C11 1.3900 . ?
N2 Cu3 2.018(11) 2_674 ?
C7 C8 1.3900 . ?
C8 C9 1.3900 . ?
C9 C10 1.3900 . ?
C9 C12 1.49(3) . ?
C10 C11 1.3900 . ?
N3 C13 1.3900 . ?
N3 C17 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C15 C18 1.52(2) . ?
C16 C17 1.3900 . ?
N4 C19 1.3900 . ?
N4 C23 1.3900 . ?
N4 Cu4 2.020(9) 5_445 ?
C19 C20 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.3900 . ?
C21 C24 1.52(3) . ?
C22 C23 1.3900 . ?
Na1 O5 2.290(14) 4_575 ?
Na1 O2 2.349(14) 4_575 ?
Na1 O3 2.377(13) 4_575 ?
Na1 Pr1 3.6011(11) 4_575 ?
Na2 Na2' 1.37(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
O10 Pr1 O7 97.9(8) . . ?
O10 Pr1 O9 142.5(9) . . ?
O7 Pr1 O9 72.2(8) . . ?
O10 Pr1 O4 142.5(7) . . ?
O7 Pr1 O4 75.2(6) . . ?
O9 Pr1 O4 71.4(8) . . ?
O10 Pr1 O8 72.5(8) . . ?
O7 Pr1 O8 51.9(6) . . ?
O9 Pr1 O8 73.3(9) . . ?
O4 Pr1 O8 122.9(6) . . ?
O10 Pr1 O6 85.3(7) . . ?
O7 Pr1 O6 122.7(5) . . ?
O9 Pr1 O6 71.7(7) . . ?
O4 Pr1 O6 129.9(6) . . ?
O8 Pr1 O6 75.8(6) . . ?
O10 Pr1 O2 79.2(7) . . ?
O7 Pr1 O2 119.3(5) . . ?
O9 Pr1 O2 137.6(8) . . ?
O4 Pr1 O2 73.0(6) . . ?
O8 Pr1 O2 147.7(7) . . ?
O6 Pr1 O2 117.5(4) . . ?
O10 Pr1 O5 73.7(6) . . ?
O7 Pr1 O5 168.6(6) . . ?
O9 Pr1 O5 109.5(6) . . ?
O4 Pr1 O5 116.2(5) . . ?
O8 Pr1 O5 117.2(5) . . ?
O6 Pr1 O5 50.1(4) . . ?
O2 Pr1 O5 67.5(4) . . ?
O10 Pr1 O3 137.3(6) . . ?
O7 Pr1 O3 122.1(6) . . ?
O9 Pr1 O3 71.1(7) . . ?
O4 Pr1 O3 51.4(4) . . ?
O8 Pr1 O3 143.3(7) . . ?
O6 Pr1 O3 85.0(5) . . ?
O2 Pr1 O3 69.0(5) . . ?
O5 Pr1 O3 68.2(5) . . ?
O10 Pr1 O1 71.5(7) . . ?
O7 Pr1 O1 71.3(5) . . ?
O9 Pr1 O1 133.0(7) . . ?
O4 Pr1 O1 71.4(6) . . ?
O8 Pr1 O1 105.0(7) . . ?
O6 Pr1 O1 154.9(6) . . ?
O2 Pr1 O1 50.0(4) . . ?
O5 Pr1 O1 112.1(4) . . ?
O3 Pr1 O1 105.5(5) . . ?
O10 Pr1 C24 86.4(8) . . ?
O7 Pr1 C24 25.0(6) . . ?
O9 Pr1 C24 69.5(8) . . ?
O4 Pr1 C24 97.8(7) . . ?
O8 Pr1 C24 27.0(6) . . ?
O6 Pr1 C24 99.8(6) . . ?
O2 Pr1 C24 138.3(6) . . ?
O5 Pr1 C24 144.2(6) . . ?
O3 Pr1 C24 136.2(7) . . ?
O1 Pr1 C24 88.4(6) . . ?
O10 Pr1 C18 76.5(7) . . ?
O7 Pr1 C18 145.8(5) . . ?
O9 Pr1 C18 91.6(7) . . ?
O4 Pr1 C18 129.0(5) . . ?
O8 Pr1 C18 95.0(6) . . ?
O6 Pr1 C18 24.5(5) . . ?
O2 Pr1 C18 93.2(5) . . ?
O5 Pr1 C18 25.7(5) . . ?
O3 Pr1 C18 77.6(5) . . ?
O1 Pr1 C18 134.5(5) . . ?
C24 Pr1 C18 121.3(6) . . ?
N4 Cu4 Cu1 136.8(4) 5 . ?
N4 Cu4 I4 107.8(3) 5 . ?
Cu1 Cu4 I4 114.76(12) . . ?
N4 Cu4 Cu2 152.8(5) 5 . ?
Cu1 Cu4 Cu2 59.74(10) . . ?
I4 Cu4 Cu2 66.37(9) . . ?
N4 Cu4 Cu3 143.7(5) 5 . ?
Cu1 Cu4 Cu3 61.31(11) . . ?
I4 Cu4 Cu3 60.67(9) . . ?
Cu2 Cu4 Cu3 58.78(11) . . ?
N4 Cu4 I2 105.7(5) 5 . ?
Cu1 Cu4 I2 61.09(10) . . ?
I4 Cu4 I2 117.12(11) . . ?
Cu2 Cu4 I2 59.73(10) . . ?
Cu3 Cu4 I2 110.04(11) . . ?
N4 Cu4 I3 99.5(5) 5 . ?
Cu1 Cu4 I3 57.67(9) . . ?
I4 Cu4 I3 112.70(12) . . ?
Cu2 Cu4 I3 107.29(11) . . ?
Cu3 Cu4 I3 61.20(10) . . ?
I2 Cu4 I3 112.15(10) . . ?
N2 Cu3 Cu2 153.5(4) 2_675 . ?
N2 Cu3 I1 106.6(4) 2_675 . ?
Cu2 Cu3 I1 61.19(9) . . ?
N2 Cu3 Cu4 139.9(4) 2_675 . ?
Cu2 Cu3 Cu4 60.36(11) . . ?
I1 Cu3 Cu4 113.08(12) . . ?
N2 Cu3 I4 106.5(3) 2_675 . ?
Cu2 Cu3 I4 66.35(10) . . ?
I1 Cu3 I4 118.92(12) . . ?
Cu4 Cu3 I4 59.07(9) . . ?
N2 Cu3 Cu1 140.8(4) 2_675 . ?
Cu2 Cu3 Cu1 59.19(10) . . ?
I1 Cu3 Cu1 65.79(9) . . ?
Cu4 Cu3 Cu1 58.11(10) . . ?
I4 Cu3 Cu1 110.55(12) . . ?
N2 Cu3 I3 96.8(4) 2_675 . ?
Cu2 Cu3 I3 109.60(12) . . ?
I1 Cu3 I3 112.69(11) . . ?
Cu4 Cu3 I3 62.59(10) . . ?
I4 Cu3 I3 112.54(11) . . ?
Cu1 Cu3 I3 57.26(9) . . ?
N1 Cu2 Cu3 135.9(5) 1_655 . ?
N1 Cu2 Cu1 156.3(4) 1_655 . ?
Cu3 Cu2 Cu1 61.83(12) . . ?
N1 Cu2 Cu4 138.8(3) 1_655 . ?
Cu3 Cu2 Cu4 60.85(11) . . ?
Cu1 Cu2 Cu4 59.10(9) . . ?
N1 Cu2 I2 109.8(4) 1_655 . ?
Cu3 Cu2 I2 112.89(11) . . ?
Cu1 Cu2 I2 61.34(10) . . ?
Cu4 Cu2 I2 61.03(9) . . ?
N1 Cu2 I1 106.3(4) 1_655 . ?
Cu3 Cu2 I1 60.10(10) . . ?
Cu1 Cu2 I1 66.36(10) . . ?
Cu4 Cu2 I1 112.58(12) . . ?
I2 Cu2 I1 120.16(11) . . ?
N1 Cu2 I4 97.5(4) 1_655 . ?
Cu3 Cu2 I4 57.92(9) . . ?
Cu1 Cu2 I4 106.12(11) . . ?
Cu4 Cu2 I4 56.49(8) . . ?
I2 Cu2 I4 109.82(10) . . ?
I1 Cu2 I4 110.78(13) . . ?
N3 Cu1 Cu4 158.1(4) . . ?
N3 Cu1 Cu2 133.9(3) . . ?
Cu4 Cu1 Cu2 61.16(10) . . ?
N3 Cu1 I3 108.7(3) . . ?
Cu4 Cu1 I3 65.90(10) . . ?
Cu2 Cu1 I3 115.08(12) . . ?
N3 Cu1 Cu3 138.1(5) . . ?
Cu4 Cu1 Cu3 60.58(10) . . ?
Cu2 Cu1 Cu3 58.99(12) . . ?
I3 Cu1 Cu3 63.77(10) . . ?
N3 Cu1 I2 109.1(4) . . ?
Cu4 Cu1 I2 61.33(10) . . ?
Cu2 Cu1 I2 60.25(10) . . ?
I3 Cu1 I2 119.49(12) . . ?
Cu3 Cu1 I2 109.65(11) . . ?
N3 Cu1 I1 94.4(4) . . ?
Cu4 Cu1 I1 107.43(11) . . ?
Cu2 Cu1 I1 57.82(9) . . ?
I3 Cu1 I1 110.38(13) . . ?
Cu3 Cu1 I1 56.49(9) . . ?
I2 Cu1 I1 111.77(10) . . ?
Cu2 I2 Cu1 58.41(9) . . ?
Cu2 I2 Cu4 59.24(9) . . ?
Cu1 I2 Cu4 57.58(9) . . ?
Cu4 I4 Cu3 60.26(9) . . ?
Cu4 I4 Cu2 57.14(8) . . ?
Cu3 I4 Cu2 55.72(9) . . ?
Cu1 I3 Cu3 58.97(9) . . ?
Cu1 I3 Cu4 56.42(8) . . ?
Cu3 I3 Cu4 56.22(8) . . ?
Cu3 I1 Cu2 58.71(9) . . ?
Cu3 I1 Cu1 57.71(9) . . ?
Cu2 I1 Cu1 55.82(8) . . ?
C6 O1 Pr1 90.9(12) . . ?
C6 O2 Na1 168.8(14) . . ?
C6 O2 Pr1 92.8(12) . . ?
Na1 O2 Pr1 94.3(5) . . ?
C12 O3 Na1 120.0(14) . . ?
C12 O3 Pr1 91.3(13) . . ?
Na1 O3 Pr1 92.7(5) . . ?
C12 O4 Pr1 96.0(14) . . ?
C18 O5 Na1 144.3(14) . . ?
C18 O5 Pr1 91.8(10) . . ?
Na1 O5 Pr1 95.5(5) . . ?
C18 O6 Pr1 94.6(12) . . ?
C24 O7 Pr1 94.9(15) . . ?
C24 O8 Pr1 91.3(15) . . ?
C1 N1 C5 120.0 . . ?
C1 N1 Cu2 120.9(6) . 1_455 ?
C5 N1 Cu2 118.5(6) . 1_455 ?
C2 C1 N1 120.0 . . ?
C1 C2 C3 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 C6 122.2(11) . . ?
C2 C3 C6 117.8(11) . . ?
C3 C4 C5 120.0 . . ?
C4 C5 N1 120.0 . . ?
O1 C6 O2 126(2) . . ?
O1 C6 C3 120.5(16) . . ?
O2 C6 C3 113.3(18) . . ?
O1 C6 Pr1 64.6(12) . . ?
O2 C6 Pr1 61.7(10) . . ?
C3 C6 Pr1 174.9(13) . . ?
C7 N2 C11 120.0 . . ?
C7 N2 Cu3 119.2(6) . 2_674 ?
C11 N2 Cu3 119.0(7) . 2_674 ?
N2 C7 C8 120.0 . . ?
C7 C8 C9 120.0 . . ?
C10 C9 C8 120.0 . . ?
C10 C9 C12 117.3(10) . . ?
C8 C9 C12 122.7(10) . . ?
C9 C10 C11 120.0 . . ?
C10 C11 N2 120.0 . . ?
O4 C12 O3 121(2) . . ?
O4 C12 C9 121.7(17) . . ?
O3 C12 C9 116.8(16) . . ?
O4 C12 Pr1 59.1(12) . . ?
O3 C12 Pr1 62.1(12) . . ?
C9 C12 Pr1 176.1(17) . . ?
C13 N3 C17 120.0 . . ?
C13 N3 Cu1 121.8(6) . . ?
C17 N3 Cu1 117.5(6) . . ?
N3 C13 C14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 C18 119.3(10) . . ?
C14 C15 C18 120.2(10) . . ?
C15 C16 C17 120.0 . . ?
C16 C17 N3 120.0 . . ?
O6 C18 O5 122.6(18) . . ?
O6 C18 C15 119.7(17) . . ?
O5 C18 C15 115.9(14) . . ?
O6 C18 Pr1 60.8(11) . . ?
O5 C18 Pr1 62.5(9) . . ?
C15 C18 Pr1 175.2(13) . . ?
C19 N4 C23 120.0 . . ?
C19 N4 Cu4 117.8(6) . 5_445 ?
C23 N4 Cu4 121.2(6) . 5_445 ?
N4 C19 C20 120.0 . . ?
C19 C20 C21 120.0 . . ?
C22 C21 C20 120.0 . . ?
C22 C21 C24 120.3(13) . . ?
C20 C21 C24 119.7(13) . . ?
C21 C22 C23 120.0 . . ?
C22 C23 N4 120.0 . . ?
O7 C24 O8 122(2) . . ?
O7 C24 C21 121(2) . . ?
O8 C24 C21 117.5(19) . . ?
O7 C24 Pr1 60.1(12) . . ?
O8 C24 Pr1 61.7(12) . . ?
C21 C24 Pr1 171.7(18) . . ?
O5 Na1 O5 106.5(8) . 4_575 ?
O5 Na1 O2 171.1(6) . 4_575 ?
O5 Na1 O2 75.7(5) 4_575 4_575 ?
O5 Na1 O2 75.7(5) . . ?
O5 Na1 O2 171.1(6) 4_575 . ?
O2 Na1 O2 103.4(7) 4_575 . ?
O5 Na1 O3 76.7(5) . . ?
O5 Na1 O3 95.8(5) 4_575 . ?
O2 Na1 O3 111.8(5) 4_575 . ?
O2 Na1 O3 76.2(5) . . ?
O5 Na1 O3 95.8(5) . 4_575 ?
O5 Na1 O3 76.7(5) 4_575 4_575 ?
O2 Na1 O3 76.2(5) 4_575 4_575 ?
O2 Na1 O3 111.8(5) . 4_575 ?
O3 Na1 O3 167.6(8) . 4_575 ?
O5 Na1 Pr1 45.3(3) . . ?
O5 Na1 Pr1 130.8(4) 4_575 . ?
O2 Na1 Pr1 139.3(4) 4_575 . ?
O2 Na1 Pr1 45.1(3) . . ?
O3 Na1 Pr1 46.0(3) . . ?
O3 Na1 Pr1 133.3(3) 4_575 . ?
O5 Na1 Pr1 130.8(4) . 4_575 ?
O5 Na1 Pr1 45.3(3) 4_575 4_575 ?
O2 Na1 Pr1 45.1(3) 4_575 4_575 ?
O2 Na1 Pr1 139.3(4) . 4_575 ?
O3 Na1 Pr1 133.3(3) . 4_575 ?
O3 Na1 Pr1 46.0(3) 4_575 4_575 ?
Pr1 Na1 Pr1 175.2(3) . 4_575 ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        24.76
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         1.463
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.345
####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 1430397'
_audit_update_record             
;
2015-10-09 deposited with the CCDC.
2017-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            9-Yb
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H72 Cu2 I2 N14 O23 Yb2'
_chemical_formula_weight         1940.16

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.1943(4)
_cell_length_b                   12.4986(4)
_cell_length_c                   15.0770(5)
_cell_angle_alpha                91.996(2)
_cell_angle_beta                 97.522(2)
_cell_angle_gamma                116.512(2)
_cell_volume                     1861.02(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.053
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             946
_exptl_absorpt_coefficient_mu    3.957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13229
_diffrn_reflns_av_R_equivalents  0.0123
_diffrn_reflns_av_sigmaI/netI    0.0188
_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       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         24.85
_reflns_number_total             6201
_reflns_number_gt                5703
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0424P)²+6.0103P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6201
_refine_ls_number_parameters     412
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0810
_refine_ls_wR_factor_gt          0.0780
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.291753(19) 0.387032(17) 0.463921(13) 0.02635(8) Uani 1 1 d . . .
I1 I 0.72505(3) 0.07297(4) 0.00956(2) 0.04381(11) Uani 1 1 d . . .
Cu1 Cu 0.51411(7) -0.00194(6) 0.08977(4) 0.03681(15) Uani 1 1 d . . .
O4 O 0.3811(4) 0.5431(3) 0.3773(2) 0.0379(8) Uani 1 1 d . . .
O2 O 0.4717(4) 0.3731(3) 0.4278(2) 0.0379(8) Uani 1 1 d . . .
O1 O 0.6949(3) 0.4487(3) 0.4504(2) 0.0354(8) Uani 1 1 d . . .
O3 O 0.6083(4) 0.6297(3) 0.3997(2) 0.0366(8) Uani 1 1 d . . .
O5 O 0.2253(4) 0.1812(3) 0.4587(3) 0.0505(10) Uani 1 1 d . . .
O6 O 0.1119(4) 0.3160(3) 0.5415(3) 0.0431(9) Uani 1 1 d . . .
N2 N 0.5036(4) 0.8578(4) 0.1641(3) 0.0379(10) Uani 1 1 d . . .
O8 O 0.0944(4) 0.3812(5) 0.3703(3) 0.0593(12) Uani 1 1 d . . .
O7 O 0.1985(5) 0.2987(4) 0.3094(3) 0.0602(12) Uani 1 1 d . . .
N1 N 0.5427(5) 0.1268(4) 0.1927(3) 0.0390(10) Uani 1 1 d . . .
C9 C 0.4974(5) 0.6984(4) 0.2898(3) 0.0323(11) Uani 1 1 d . . .
C6 C 0.5792(5) 0.3758(4) 0.4108(3) 0.0308(10) Uani 1 1 d . . .
N4 N 0.0075(5) 0.3695(5) 0.6390(4) 0.0515(12) Uani 1 1 d . . .
C8 C 0.6172(5) 0.7758(5) 0.2629(4) 0.0402(12) Uani 1 1 d . . .
H8A H 0.6998 0.7759 0.2874 0.048 Uiso 1 1 calc R . .
C3 C 0.5681(5) 0.2862(4) 0.3361(3) 0.0313(10) Uani 1 1 d . . .
C12 C 0.4955(5) 0.6160(4) 0.3616(3) 0.0314(11) Uani 1 1 d . . .
N5 N 0.1014(5) 0.3266(5) 0.3024(4) 0.0587(14) Uani 1 1 d . . .
C10 C 0.3820(6) 0.6999(6) 0.2501(4) 0.0518(16) Uani 1 1 d . . .
H10A H 0.2973 0.6460 0.2652 0.062 Uiso 1 1 calc R . .
C4 C 0.4422(6) 0.2020(5) 0.2932(4) 0.0461(14) Uani 1 1 d . . .
H4A H 0.3623 0.1977 0.3116 0.055 Uiso 1 1 calc R . .
C2 C 0.6807(5) 0.2891(5) 0.3066(4) 0.0395(12) Uani 1 1 d . . .
H2A H 0.7690 0.3454 0.3351 0.047 Uiso 1 1 calc R . .
C1 C 0.6628(5) 0.2084(5) 0.2346(4) 0.0412(12) Uani 1 1 d . . .
H1A H 0.7410 0.2118 0.2142 0.049 Uiso 1 1 calc R . .
N3 N 0.2173(6) 0.0233(5) 0.5318(4) 0.0651(15) Uani 1 1 d . . .
N6 N -0.0141(6) 0.0398(6) 0.8206(4) 0.0655(15) Uani 1 1 d . . .
C7 C 0.6156(6) 0.8528(5) 0.2005(4) 0.0432(13) Uani 1 1 d . . .
H7A H 0.6986 0.9051 0.1824 0.052 Uiso 1 1 calc R . .
C5 C 0.4343(6) 0.1241(6) 0.2231(4) 0.0496(15) Uani 1 1 d . . .
H5A H 0.3472 0.0654 0.1947 0.060 Uiso 1 1 calc R . .
C15 C 0.1838(6) 0.1105(5) 0.5154(4) 0.0499(14) Uani 1 1 d . . .
H15A H 0.1231 0.1193 0.5501 0.060 Uiso 1 1 calc R . .
C18 C 0.1073(6) 0.3517(5) 0.6182(4) 0.0440(13) Uani 1 1 d . . .
H18A H 0.1808 0.3670 0.6646 0.053 Uiso 1 1 calc R . .
C11 C 0.3876(6) 0.7793(6) 0.1882(4) 0.0559(17) Uani 1 1 d . . .
H11A H 0.3056 0.7785 0.1612 0.067 Uiso 1 1 calc R . .
O9 O 0.0234(7) 0.3019(7) 0.2323(4) 0.119(3) Uani 1 1 d . . .
O10 O 0.0022(10) 0.1081(6) 0.6845(5) 0.140(3) Uani 1 1 d . . .
C17 C 0.0048(8) 0.4046(8) 0.7317(5) 0.077(2) Uani 1 1 d . . .
H17A H 0.0877 0.4150 0.7701 0.115 Uiso 1 1 calc R . .
H17B H -0.0739 0.3419 0.7523 0.115 Uiso 1 1 calc R . .
H17C H -0.0012 0.4804 0.7349 0.115 Uiso 1 1 calc R . .
C21 C -0.0380(10) 0.0276(8) 0.7327(6) 0.090(3) Uani 1 1 d . . .
H21A H -0.0918 -0.0516 0.7038 0.108 Uiso 1 1 calc R . .
C20 C -0.0667(9) -0.0637(8) 0.8691(5) 0.076(2) Uani 1 1 d . . .
H20A H -0.1198 -0.1359 0.8265 0.115 Uiso 1 1 calc R . .
H20B H -0.1246 -0.0548 0.9092 0.115 Uiso 1 1 calc R . .
H20C H 0.0084 -0.0712 0.9048 0.115 Uiso 1 1 calc R . .
C14 C 0.1582(9) -0.0621(6) 0.5964(6) 0.082(3) Uani 1 1 d . . .
H14A H 0.0966 -0.0412 0.6250 0.124 Uiso 1 1 calc R . .
H14B H 0.2305 -0.0589 0.6425 0.124 Uiso 1 1 calc R . .
H14C H 0.1079 -0.1435 0.5651 0.124 Uiso 1 1 calc R . .
C19 C 0.0670(10) 0.1547(8) 0.8727(7) 0.104(3) Uani 1 1 d . . .
H19A H 0.0973 0.2179 0.8322 0.157 Uiso 1 1 calc R . .
H19B H 0.1460 0.1539 0.9088 0.157 Uiso 1 1 calc R . .
H19C H 0.0130 0.1705 0.9126 0.157 Uiso 1 1 calc R . .
C16 C -0.1078(8) 0.3494(8) 0.5714(6) 0.086(3) Uani 1 1 d . . .
H16A H -0.0935 0.3259 0.5125 0.128 Uiso 1 1 calc R . .
H16B H -0.1173 0.4235 0.5690 0.128 Uiso 1 1 calc R . .
H16C H -0.1902 0.2852 0.5871 0.128 Uiso 1 1 calc R . .
C13 C 0.3121(13) 0.0083(11) 0.4821(10) 0.151(6) Uani 1 1 d . . .
H13A H 0.3438 0.0717 0.4418 0.226 Uiso 1 1 calc R . .
H13B H 0.2672 -0.0705 0.4465 0.226 Uiso 1 1 calc R . .
H13C H 0.3894 0.0136 0.5243 0.226 Uiso 1 1 calc R . .
N7 N 0.4935(9) 0.3917(6) 0.0918(5) 0.085(2) Uani 1 1 d D . .
O11 O 0.6774(12) 0.5337(11) 0.1705(9) 0.190(5) Uani 1 1 d DU . .
C24 C 0.5626(15) 0.4759(14) 0.1650(10) 0.213(9) Uani 1 1 d DU . .
H24A H 0.5160 0.4861 0.2103 0.255 Uiso 1 1 calc R . .
C23 C 0.4798(18) 0.3176(14) 0.0245(10) 0.178(6) Uani 1 1 d U . .
H23A H 0.5693 0.3293 0.0142 0.266 Uiso 1 1 calc R . .
H23B H 0.4329 0.3326 -0.0295 0.266 Uiso 1 1 calc R . .
H23C H 0.4269 0.2348 0.0379 0.266 Uiso 1 1 calc R . .
C22 C 0.356(2) 0.367(2) 0.1044(15) 0.251(10) Uani 1 1 d U . .
H22A H 0.2901 0.3071 0.0562 0.377 Uiso 1 1 calc R . .
H22B H 0.3469 0.4414 0.1026 0.377 Uiso 1 1 calc R . .
H22C H 0.3390 0.3362 0.1627 0.377 Uiso 1 1 calc R . .
O1W O 0.0000 0.5000 1.0000 0.284(11) Uani 1 2 d SU . .


_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 O2 2.232(3) . ?
Yb1 O3 2.271(3) 2_666 ?
Yb1 O4 2.300(3) . ?
Yb1 O6 2.303(4) . ?
Yb1 O1 2.323(3) 2_666 ?
Yb1 O5 2.333(4) . ?
Yb1 O7 2.428(4) . ?
Yb1 O8 2.431(4) . ?
Yb1 N5 2.849(5) . ?
Yb1 C6 3.085(5) 2_666 ?
Yb1 Yb1 4.1952(4) 2_666 ?
I1 Cu1 2.6015(7) . ?
I1 Cu1 2.6333(7) 2_655 ?
Cu1 N2 2.081(4) 1_545 ?
Cu1 N1 2.083(4) . ?
Cu1 I1 2.6333(7) 2_655 ?
Cu1 Cu1 2.6887(12) 2_655 ?
O4 C12 1.256(6) . ?
O2 C6 1.248(6) . ?
O1 C6 1.254(6) . ?
O1 Yb1 2.323(3) 2_666 ?
O3 C12 1.251(6) . ?
O3 Yb1 2.271(3) 2_666 ?
O5 C15 1.232(7) . ?
O6 C18 1.240(7) . ?
N2 C7 1.330(7) . ?
N2 C11 1.339(7) . ?
N2 Cu1 2.081(4) 1_565 ?
O8 N5 1.242(7) . ?
O7 N5 1.275(7) . ?
N1 C1 1.324(7) . ?
N1 C5 1.340(7) . ?
C9 C10 1.360(8) . ?
C9 C8 1.382(7) . ?
C9 C12 1.515(6) . ?
C6 C3 1.512(6) . ?
C6 Yb1 3.085(5) 2_666 ?
N4 C18 1.306(7) . ?
N4 C16 1.455(9) . ?
N4 C17 1.457(9) . ?
C8 C7 1.373(7) . ?
C3 C2 1.376(7) . ?
C3 C4 1.380(7) . ?
N5 O9 1.213(7) . ?
C10 C11 1.372(8) . ?
C4 C5 1.378(8) . ?
C2 C1 1.387(7) . ?
N3 C15 1.321(8) . ?
N3 C13 1.449(12) . ?
N3 C14 1.463(9) . ?
N6 C21 1.307(10) . ?
N6 C20 1.433(10) . ?
N6 C19 1.441(10) . ?
O10 C21 1.215(10) . ?
N7 C23 1.296(15) . ?
N7 C24 1.375(10) . ?
N7 C22 1.47(2) . ?
O11 C24 1.149(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
O2 Yb1 O3 78.72(13) . 2_666 ?
O2 Yb1 O4 76.99(13) . . ?
O3 Yb1 O4 126.15(13) 2_666 . ?
O2 Yb1 O6 148.02(13) . . ?
O3 Yb1 O6 78.58(13) 2_666 . ?
O4 Yb1 O6 134.94(13) . . ?
O2 Yb1 O1 123.74(13) . 2_666 ?
O3 Yb1 O1 78.90(13) 2_666 2_666 ?
O4 Yb1 O1 76.12(13) . 2_666 ?
O6 Yb1 O1 72.97(13) . 2_666 ?
O2 Yb1 O5 77.05(14) . . ?
O3 Yb1 O5 77.41(14) 2_666 . ?
O4 Yb1 O5 139.72(14) . . ?
O6 Yb1 O5 76.23(14) . . ?
O1 Yb1 O5 144.15(13) 2_666 . ?
O2 Yb1 O7 81.75(15) . . ?
O3 Yb1 O7 146.33(14) 2_666 . ?
O4 Yb1 O7 74.61(15) . . ?
O6 Yb1 O7 105.90(16) . . ?
O1 Yb1 O7 134.67(13) 2_666 . ?
O5 Yb1 O7 71.61(15) . . ?
O2 Yb1 O8 131.17(14) . . ?
O3 Yb1 O8 148.96(14) 2_666 . ?
O4 Yb1 O8 76.07(14) . . ?
O6 Yb1 O8 70.73(15) . . ?
O1 Yb1 O8 87.63(14) 2_666 . ?
O5 Yb1 O8 99.20(17) . . ?
O7 Yb1 O8 52.13(15) . . ?
O2 Yb1 N5 106.99(16) . . ?
O3 Yb1 N5 160.17(15) 2_666 . ?
O4 Yb1 N5 73.57(15) . . ?
O6 Yb1 N5 88.01(16) . . ?
O1 Yb1 N5 111.23(15) 2_666 . ?
O5 Yb1 N5 85.30(16) . . ?
O7 Yb1 N5 26.45(16) . . ?
O8 Yb1 N5 25.68(15) . . ?
O2 Yb1 C6 102.73(13) . 2_666 ?
O3 Yb1 C6 67.59(13) 2_666 2_666 ?
O4 Yb1 C6 72.06(13) . 2_666 ?
O6 Yb1 C6 89.03(13) . 2_666 ?
O1 Yb1 C6 21.44(12) 2_666 2_666 ?
O5 Yb1 C6 144.13(13) . 2_666 ?
O7 Yb1 C6 144.26(14) . 2_666 ?
O8 Yb1 C6 106.57(15) . 2_666 ?
N5 Yb1 C6 127.29(15) . 2_666 ?
O2 Yb1 Yb1 48.23(9) . 2_666 ?
O3 Yb1 Yb1 63.31(9) 2_666 2_666 ?
O4 Yb1 Yb1 64.59(9) . 2_666 ?
O6 Yb1 Yb1 134.27(10) . 2_666 ?
O1 Yb1 Yb1 75.61(9) 2_666 2_666 ?
O5 Yb1 Yb1 115.86(11) . 2_666 ?
O7 Yb1 Yb1 119.82(12) . 2_666 ?
O8 Yb1 Yb1 139.78(12) . 2_666 ?
N5 Yb1 Yb1 134.66(12) . 2_666 ?
C6 Yb1 Yb1 54.50(9) 2_666 2_666 ?
Cu1 I1 Cu1 61.81(2) . 2_655 ?
N2 Cu1 N1 100.31(18) 1_545 . ?
N2 Cu1 I1 110.00(12) 1_545 . ?
N1 Cu1 I1 110.03(13) . . ?
N2 Cu1 I1 107.38(12) 1_545 2_655 ?
N1 Cu1 I1 109.41(13) . 2_655 ?
I1 Cu1 I1 118.19(2) . 2_655 ?
N2 Cu1 Cu1 128.56(13) 1_545 2_655 ?
N1 Cu1 Cu1 131.07(13) . 2_655 ?
I1 Cu1 Cu1 59.68(2) . 2_655 ?
I1 Cu1 Cu1 58.52(2) 2_655 2_655 ?
C12 O4 Yb1 138.2(3) . . ?
C6 O2 Yb1 174.4(3) . . ?
C6 O1 Yb1 115.9(3) . 2_666 ?
C12 O3 Yb1 139.5(3) . 2_666 ?
C15 O5 Yb1 130.8(4) . . ?
C18 O6 Yb1 128.3(4) . . ?
C7 N2 C11 116.7(5) . . ?
C7 N2 Cu1 120.8(4) . 1_565 ?
C11 N2 Cu1 121.8(4) . 1_565 ?
N5 O8 Yb1 96.3(3) . . ?
N5 O7 Yb1 95.5(3) . . ?
C1 N1 C5 116.8(4) . . ?
C1 N1 Cu1 124.2(4) . . ?
C5 N1 Cu1 118.9(4) . . ?
C10 C9 C8 117.5(5) . . ?
C10 C9 C12 121.4(5) . . ?
C8 C9 C12 121.1(5) . . ?
O2 C6 O1 124.4(4) . . ?
O2 C6 C3 117.4(4) . . ?
O1 C6 C3 118.2(4) . . ?
O2 C6 Yb1 82.8(3) . 2_666 ?
O1 C6 Yb1 42.6(2) . 2_666 ?
C3 C6 Yb1 157.3(3) . 2_666 ?
C18 N4 C16 121.1(6) . . ?
C18 N4 C17 121.1(6) . . ?
C16 N4 C17 117.7(6) . . ?
C7 C8 C9 119.3(5) . . ?
C2 C3 C4 118.4(5) . . ?
C2 C3 C6 121.9(5) . . ?
C4 C3 C6 119.7(5) . . ?
O3 C12 O4 127.3(4) . . ?
O3 C12 C9 116.2(4) . . ?
O4 C12 C9 116.5(4) . . ?
O9 N5 O8 123.2(6) . . ?
O9 N5 O7 120.7(6) . . ?
O8 N5 O7 116.1(5) . . ?
O9 N5 Yb1 178.2(6) . . ?
O8 N5 Yb1 58.0(3) . . ?
O7 N5 Yb1 58.0(3) . . ?
C9 C10 C11 120.1(5) . . ?
C5 C4 C3 118.8(5) . . ?
C3 C2 C1 118.7(5) . . ?
N1 C1 C2 123.7(5) . . ?
C15 N3 C13 119.4(6) . . ?
C15 N3 C14 122.3(7) . . ?
C13 N3 C14 118.2(7) . . ?
C21 N6 C20 120.2(7) . . ?
C21 N6 C19 122.6(8) . . ?
C20 N6 C19 117.2(7) . . ?
N2 C7 C8 123.3(5) . . ?
N1 C5 C4 123.6(5) . . ?
O5 C15 N3 125.0(6) . . ?
O6 C18 N4 124.0(6) . . ?
N2 C11 C10 122.9(5) . . ?
O10 C21 N6 126.1(9) . . ?
C23 N7 C24 155.7(14) . . ?
C23 N7 C22 106.3(13) . . ?
C24 N7 C22 97.6(13) . . ?
O11 C24 N7 119.1(17) . . ?

_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full        24.85
_diffrn_measured_fraction_theta_full 0.962
_refine_diff_density_max         1.312
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.117
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1430390'
_audit_update_record             
;
2015-10-09 deposited with the CCDC.
2017-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            9-Sm
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H72 Cu2 I2 N14 O23 Sm2'
_chemical_formula_weight         1894.78

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'
Cu Cu 0.3201 1.2651 '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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.0928(2)
_cell_length_b                   12.4805(2)
_cell_length_c                   15.1388(2)
_cell_angle_alpha                81.4630(10)
_cell_angle_beta                 83.4160(10)
_cell_angle_gamma                64.1330(10)
_cell_volume                     1862.06(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.055
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             930
_exptl_absorpt_coefficient_mu    3.020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15226
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         24.86
_reflns_number_total             6260
_reflns_number_gt                5706
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0439P)²+4.8574P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6260
_refine_ls_number_parameters     412
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0791
_refine_ls_wR_factor_gt          0.0764
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.903640(19) 0.388980(17) 0.036587(13) 0.02106(8) Uani 1 1 d . . .
Cu1 Cu 0.51409(5) 0.99920(5) 0.41169(3) 0.02900(13) Uani 1 1 d . . .
I1 I 0.65315(3) 1.07438(3) 0.492515(19) 0.03520(9) Uani 1 1 d . . .
O1 O 1.2675(3) 0.4478(3) 0.0516(2) 0.0325(7) Uani 1 1 d . . .
O1W O 0.5000 0.5000 -0.5000 0.270(9) Uani 1 2 d SU . .
O2 O 1.1058(3) 0.3877(3) 0.0691(2) 0.0336(7) Uani 1 1 d . . .
O3 O 0.9725(3) 0.6398(3) 0.10321(19) 0.0317(7) Uani 1 1 d . . .
O4 O 0.8334(3) 0.5500(3) 0.1268(2) 0.0336(7) Uani 1 1 d . . .
O5 O 1.0497(4) 0.1761(3) 0.0472(2) 0.0436(8) Uani 1 1 d . . .
O6 O 0.7954(3) 0.3083(3) -0.0446(2) 0.0355(7) Uani 1 1 d . . .
O7 O 0.8988(3) 0.3006(3) 0.1976(2) 0.0454(9) Uani 1 1 d . . .
O8 O 0.7125(3) 0.3698(4) 0.1341(2) 0.0475(9) Uani 1 1 d . . .
O9 O 0.7223(5) 0.2991(6) 0.2734(3) 0.101(2) Uani 1 1 d . . .
O10 O 0.0900(7) 0.8968(4) 0.1870(3) 0.0926(18) Uani 1 1 d . . .
O11 O 0.8804(9) 0.4566(7) 0.6883(7) 0.173(4) Uani 1 1 d D . .
N1 N 1.4140(4) 0.1294(3) 0.3107(2) 0.0311(8) Uani 1 1 d . . .
N2 N 0.6438(4) 0.8625(3) 0.3387(2) 0.0308(8) Uani 1 1 d . . .
N3 N 1.1986(5) 0.0187(4) -0.0234(3) 0.0525(12) Uani 1 1 d . . .
N4 N 0.6385(4) 0.3654(4) -0.1457(3) 0.0421(10) Uani 1 1 d . . .
N5 N 0.7760(5) 0.3229(4) 0.2038(3) 0.0466(11) Uani 1 1 d . . .
N6 N 0.0486(5) 0.9630(4) 0.3227(3) 0.0499(11) Uani 1 1 d . . .
N7 N 0.9019(6) 0.6073(5) 0.5911(4) 0.0645(14) Uani 1 1 d D . .
C1 C 1.4603(5) 0.2070(4) 0.2689(3) 0.0356(10) Uani 1 1 d . . .
H1A H 1.5379 0.2066 0.2900 0.043 Uiso 1 1 calc R . .
C2 C 1.4013(5) 0.2878(4) 0.1965(3) 0.0343(10) Uani 1 1 d . . .
H2A H 1.4388 0.3404 0.1680 0.041 Uiso 1 1 calc R . .
C3 C 1.2865(4) 0.2911(4) 0.1660(3) 0.0261(9) Uani 1 1 d . . .
C4 C 1.2381(5) 0.2110(4) 0.2090(3) 0.0367(11) Uani 1 1 d . . .
H4A H 1.1597 0.2104 0.1900 0.044 Uiso 1 1 calc R . .
C5 C 1.3047(5) 0.1321(4) 0.2796(3) 0.0390(11) Uani 1 1 d . . .
H5A H 1.2712 0.0765 0.3077 0.047 Uiso 1 1 calc R . .
C6 C 1.2159(4) 0.3813(4) 0.0898(3) 0.0271(9) Uani 1 1 d . . .
C7 C 0.7576(5) 0.8629(4) 0.2994(3) 0.0346(10) Uani 1 1 d . . .
H7A H 0.7860 0.9191 0.3149 0.042 Uiso 1 1 calc R . .
C8 C 0.8362(5) 0.7865(4) 0.2377(3) 0.0344(10) Uani 1 1 d . . .
H8A H 0.9170 0.7896 0.2122 0.041 Uiso 1 1 calc R . .
C9 C 0.7962(4) 0.7052(4) 0.2134(3) 0.0263(9) Uani 1 1 d . . .
C10 C 0.6816(5) 0.7003(5) 0.2563(4) 0.0438(13) Uani 1 1 d . . .
H10A H 0.6532 0.6428 0.2437 0.053 Uiso 1 1 calc R . .
C11 C 0.6095(5) 0.7796(5) 0.3173(4) 0.0446(13) Uani 1 1 d . . .
H11A H 0.5307 0.7753 0.3461 0.054 Uiso 1 1 calc R . .
C12 C 0.8744(4) 0.6239(4) 0.1423(3) 0.0267(9) Uani 1 1 d . . .
C13 C 1.3073(8) -0.0019(9) 0.0338(8) 0.121(4) Uani 1 1 d . . .
H13A H 1.2755 0.0607 0.0743 0.182 Uiso 1 1 calc R . .
H13B H 1.3843 0.0005 -0.0038 0.182 Uiso 1 1 calc R . .
H13C H 1.3343 -0.0804 0.0690 0.182 Uiso 1 1 calc R . .
C14 C 1.2265(7) -0.0651(5) -0.0889(4) 0.0622(17) Uani 1 1 d . . .
H14A H 1.1465 -0.0410 -0.1224 0.093 Uiso 1 1 calc R . .
H14B H 1.2508 -0.1459 -0.0580 0.093 Uiso 1 1 calc R . .
H14C H 1.3011 -0.0647 -0.1303 0.093 Uiso 1 1 calc R . .
C15 C 1.0795(5) 0.1063(4) -0.0100(3) 0.0405(11) Uani 1 1 d . . .
H15A H 1.0109 0.1167 -0.0472 0.049 Uiso 1 1 calc R . .
C16 C 0.5373(6) 0.3567(7) -0.0792(5) 0.074(2) Uani 1 1 d . . .
H16A H 0.5744 0.3324 -0.0200 0.111 Uiso 1 1 calc R . .
H16B H 0.5094 0.2970 -0.0936 0.111 Uiso 1 1 calc R . .
H16C H 0.4595 0.4348 -0.0792 0.111 Uiso 1 1 calc R . .
C17 C 0.6027(7) 0.4002(7) -0.2383(4) 0.0665(18) Uani 1 1 d . . .
H17A H 0.6795 0.4029 -0.2759 0.100 Uiso 1 1 calc R . .
H17B H 0.5267 0.4795 -0.2437 0.100 Uiso 1 1 calc R . .
H17C H 0.5776 0.3416 -0.2579 0.100 Uiso 1 1 calc R . .
C18 C 0.7583(5) 0.3423(4) -0.1224(3) 0.0360(11) Uani 1 1 d . . .
H18A H 0.8207 0.3520 -0.1676 0.043 Uiso 1 1 calc R . .
C19 C 0.0828(8) 0.8469(6) 0.3725(5) 0.079(2) Uani 1 1 d . . .
H19A H 0.1120 0.7859 0.3309 0.119 Uiso 1 1 calc R . .
H19B H 0.0041 0.8467 0.4091 0.119 Uiso 1 1 calc R . .
H19C H 0.1556 0.8290 0.4114 0.119 Uiso 1 1 calc R . .
C20 C 0.0031(6) 1.0645(5) 0.3723(4) 0.0549(14) Uani 1 1 d . . .
H20A H -0.0168 1.1374 0.3307 0.082 Uiso 1 1 calc R . .
H20B H 0.0733 1.0539 0.4111 0.082 Uiso 1 1 calc R . .
H20C H -0.0782 1.0714 0.4090 0.082 Uiso 1 1 calc R . .
C21 C 0.0571(7) 0.9768(6) 0.2349(4) 0.0630(17) Uani 1 1 d . . .
H21A H 0.0361 1.0554 0.2063 0.076 Uiso 1 1 calc R . .
C22 C 1.0176(16) 0.6151(16) 0.6083(11) 0.202(7) Uani 1 1 d U . .
H22A H 1.0602 0.5562 0.6588 0.302 Uiso 1 1 calc R . .
H22B H 0.9948 0.6958 0.6231 0.302 Uiso 1 1 calc R . .
H22C H 1.0797 0.5987 0.5553 0.302 Uiso 1 1 calc R . .
C23 C 0.8379(13) 0.6860(11) 0.5214(7) 0.149(4) Uani 1 1 d U . .
H23A H 0.7563 0.6777 0.5127 0.224 Uiso 1 1 calc R . .
H23B H 0.8972 0.6693 0.4671 0.224 Uiso 1 1 calc R . .
H23C H 0.8138 0.7678 0.5342 0.224 Uiso 1 1 calc R . .
C24 C 0.8551(15) 0.5329(9) 0.6365(7) 0.176(7) Uani 1 1 d D . .
H24A H 0.7685 0.5531 0.6171 0.211 Uiso 1 1 calc R . .


_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
Sm1 O2 2.344(3) . ?
Sm1 O3 2.371(3) 2_765 ?
Sm1 O4 2.391(3) . ?
Sm1 O6 2.393(3) . ?
Sm1 O5 2.426(3) . ?
Sm1 O1 2.437(3) 2_765 ?
Sm1 O8 2.520(3) . ?
Sm1 O7 2.527(3) . ?
Sm1 N5 2.945(4) . ?
Sm1 C6 3.046(4) 2_765 ?
Cu1 N2 2.063(4) . ?
Cu1 N1 2.071(3) 1_465 ?
Cu1 I1 2.6064(6) . ?
Cu1 I1 2.6196(6) 2_676 ?
Cu1 Cu1 2.6581(10) 2_676 ?
I1 Cu1 2.6196(6) 2_676 ?
O1 C6 1.244(5) . ?
O1 Sm1 2.437(3) 2_765 ?
O2 C6 1.261(5) . ?
O3 C12 1.257(5) . ?
O3 Sm1 2.371(3) 2_765 ?
O4 C12 1.252(5) . ?
O5 C15 1.235(6) . ?
O6 C18 1.244(6) . ?
O7 N5 1.261(5) . ?
O8 N5 1.256(5) . ?
O9 N5 1.213(6) . ?
O10 C21 1.222(8) . ?
O11 C24 1.095(8) . ?
N1 C1 1.334(6) . ?
N1 C5 1.336(6) . ?
N1 Cu1 2.071(3) 1_645 ?
N2 C7 1.335(6) . ?
N2 C11 1.338(6) . ?
N3 C15 1.314(6) . ?
N3 C14 1.458(7) . ?
N3 C13 1.474(9) . ?
N4 C18 1.310(6) . ?
N4 C16 1.449(7) . ?
N4 C17 1.453(7) . ?
N6 C21 1.312(7) . ?
N6 C20 1.436(7) . ?
N6 C19 1.440(8) . ?
N7 C24 1.324(8) . ?
N7 C23 1.356(11) . ?
N7 C22 1.385(15) . ?
C1 C2 1.381(6) . ?
C2 C3 1.385(6) . ?
C3 C4 1.381(6) . ?
C3 C6 1.505(6) . ?
C4 C5 1.375(6) . ?
C6 Sm1 3.046(4) 2_765 ?
C7 C8 1.376(6) . ?
C8 C9 1.379(6) . ?
C9 C10 1.381(6) . ?
C9 C12 1.511(6) . ?
C10 C11 1.373(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
O2 Sm1 O3 77.59(10) . 2_765 ?
O2 Sm1 O4 76.41(11) . . ?
O3 Sm1 O4 130.16(10) 2_765 . ?
O2 Sm1 O6 147.20(11) . . ?
O3 Sm1 O6 75.97(11) 2_765 . ?
O4 Sm1 O6 136.14(11) . . ?
O2 Sm1 O5 79.03(12) . . ?
O3 Sm1 O5 75.39(11) 2_765 . ?
O4 Sm1 O5 137.98(11) . . ?
O6 Sm1 O5 75.81(11) . . ?
O2 Sm1 O1 124.56(11) . 2_765 ?
O3 Sm1 O1 83.19(11) 2_765 2_765 ?
O4 Sm1 O1 77.81(11) . 2_765 ?
O6 Sm1 O1 70.84(10) . 2_765 ?
O5 Sm1 O1 143.81(11) . 2_765 ?
O2 Sm1 O8 132.67(11) . . ?
O3 Sm1 O8 147.12(11) 2_765 . ?
O4 Sm1 O8 77.16(12) . . ?
O6 Sm1 O8 71.15(12) . . ?
O5 Sm1 O8 95.88(13) . . ?
O1 Sm1 O8 86.48(11) 2_765 . ?
O2 Sm1 O7 84.61(11) . . ?
O3 Sm1 O7 144.46(11) 2_765 . ?
O4 Sm1 O7 73.06(12) . . ?
O6 Sm1 O7 106.41(12) . . ?
O5 Sm1 O7 71.14(12) . . ?
O1 Sm1 O7 131.75(11) 2_765 . ?
O8 Sm1 O7 50.24(11) . . ?
O2 Sm1 N5 108.66(12) . . ?
O3 Sm1 N5 156.69(12) 2_765 . ?
O4 Sm1 N5 72.78(12) . . ?
O6 Sm1 N5 89.20(12) . . ?
O5 Sm1 N5 83.67(12) . . ?
O1 Sm1 N5 109.13(12) 2_765 . ?
O8 Sm1 N5 25.07(12) . . ?
O7 Sm1 N5 25.19(11) . . ?
O2 Sm1 C6 102.12(11) . 2_765 ?
O3 Sm1 C6 71.04(11) 2_765 2_765 ?
O4 Sm1 C6 73.91(11) . 2_765 ?
O6 Sm1 C6 87.27(11) . 2_765 ?
O5 Sm1 C6 145.19(11) . 2_765 ?
O1 Sm1 C6 22.97(11) 2_765 2_765 ?
O8 Sm1 C6 107.26(12) . 2_765 ?
O7 Sm1 C6 143.57(11) . 2_765 ?
N5 Sm1 C6 126.91(12) . 2_765 ?
N2 Cu1 N1 101.12(15) . 1_465 ?
N2 Cu1 I1 109.01(10) . . ?
N1 Cu1 I1 109.07(10) 1_465 . ?
N2 Cu1 I1 107.70(11) . 2_676 ?
N1 Cu1 I1 109.62(10) 1_465 2_676 ?
I1 Cu1 I1 118.86(2) . 2_676 ?
N2 Cu1 Cu1 128.24(11) . 2_676 ?
N1 Cu1 Cu1 130.64(11) 1_465 2_676 ?
I1 Cu1 Cu1 59.67(2) . 2_676 ?
I1 Cu1 Cu1 59.18(2) 2_676 2_676 ?
Cu1 I1 Cu1 61.14(2) . 2_676 ?
C6 O1 Sm1 107.2(3) . 2_765 ?
C6 O2 Sm1 176.5(3) . . ?
C12 O3 Sm1 138.6(3) . 2_765 ?
C12 O4 Sm1 137.6(3) . . ?
C15 O5 Sm1 128.8(3) . . ?
C18 O6 Sm1 127.0(3) . . ?
N5 O7 Sm1 96.3(3) . . ?
N5 O8 Sm1 96.7(3) . . ?
C1 N1 C5 116.9(4) . . ?
C1 N1 Cu1 122.5(3) . 1_645 ?
C5 N1 Cu1 120.3(3) . 1_645 ?
C7 N2 C11 116.4(4) . . ?
C7 N2 Cu1 121.0(3) . . ?
C11 N2 Cu1 121.8(3) . . ?
C15 N3 C14 122.8(5) . . ?
C15 N3 C13 119.2(5) . . ?
C14 N3 C13 117.9(5) . . ?
C18 N4 C16 120.7(5) . . ?
C18 N4 C17 121.5(5) . . ?
C16 N4 C17 117.8(5) . . ?
O9 N5 O8 121.8(5) . . ?
O9 N5 O7 121.6(5) . . ?
O8 N5 O7 116.6(4) . . ?
O9 N5 Sm1 178.0(5) . . ?
O8 N5 Sm1 58.2(2) . . ?
O7 N5 Sm1 58.5(2) . . ?
C21 N6 C20 120.6(5) . . ?
C21 N6 C19 121.7(6) . . ?
C20 N6 C19 117.7(5) . . ?
C24 N7 C23 121.9(10) . . ?
C24 N7 C22 125.4(11) . . ?
C23 N7 C22 112.7(10) . . ?
N1 C1 C2 123.5(4) . . ?
C1 C2 C3 119.0(4) . . ?
C4 C3 C2 117.9(4) . . ?
C4 C3 C6 121.4(4) . . ?
C2 C3 C6 120.7(4) . . ?
C5 C4 C3 119.2(4) . . ?
N1 C5 C4 123.5(4) . . ?
O1 C6 O2 123.2(4) . . ?
O1 C6 C3 118.3(4) . . ?
O2 C6 C3 118.5(4) . . ?
O1 C6 Sm1 49.8(2) . 2_765 ?
O2 C6 Sm1 74.4(2) . 2_765 ?
C3 C6 Sm1 162.8(3) . 2_765 ?
N2 C7 C8 123.6(4) . . ?
C7 C8 C9 119.3(4) . . ?
C8 C9 C10 117.7(4) . . ?
C8 C9 C12 121.5(4) . . ?
C10 C9 C12 120.7(4) . . ?
C11 C10 C9 119.1(4) . . ?
N2 C11 C10 123.8(4) . . ?
O4 C12 O3 126.8(4) . . ?
O4 C12 C9 117.1(4) . . ?
O3 C12 C9 116.2(4) . . ?
O5 C15 N3 125.1(5) . . ?
O6 C18 N4 123.9(5) . . ?
O10 C21 N6 125.4(6) . . ?
O11 C24 N7 142.5(16) . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        24.86
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         1.620
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.107
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1430392'
_audit_update_record             
;
2015-10-09 deposited with the CCDC.
2017-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            9-Gd
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H72 Cu2 Gd2 I2 N14 O23'
_chemical_formula_weight         1908.58

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.1994(12)
_cell_length_b                   12.5884(14)
_cell_length_c                   15.1740(17)
_cell_angle_alpha                92.438(2)
_cell_angle_beta                 96.979(2)
_cell_angle_gamma                116.3080(10)
_cell_volume                     1892.3(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.093
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             934
_exptl_absorpt_coefficient_mu    3.173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.499
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15372
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         24.80
_reflns_number_total             6323
_reflns_number_gt                5806
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0454P)²+4.6446P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6323
_refine_ls_number_parameters     407
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_ref         0.0821
_refine_ls_wR_factor_gt          0.0796
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.042
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.793235(19) 0.388903(16) 0.963898(12) 0.02715(8) Uani 1 1 d . . .
I1 I 1.22489(3) 0.07185(3) 0.50866(2) 0.04439(10) Uani 1 1 d . . .
Cu1 Cu 1.01313(6) -0.00180(5) 0.58895(4) 0.03779(14) Uani 1 1 d . . .
O4 O 0.8826(3) 0.5485(3) 0.8743(2) 0.0418(7) Uani 1 1 d . . .
O2 O 0.9864(3) 0.3823(3) 0.9301(2) 0.0428(8) Uani 1 1 d . . .
O3 O 1.1088(3) 0.6346(3) 0.8969(2) 0.0403(7) Uani 1 1 d . . .
O1 O 1.2068(3) 0.4469(3) 0.9484(2) 0.0403(7) Uani 1 1 d . . .
O5 O 0.7286(4) 0.1787(3) 0.9563(3) 0.0563(9) Uani 1 1 d . . .
O6 O 0.6079(3) 0.3122(3) 1.0443(2) 0.0461(8) Uani 1 1 d . . .
N2 N 1.0044(4) 0.8604(3) 0.6627(2) 0.0389(9) Uani 1 1 d . . .
N1 N 1.0424(4) 0.1273(3) 0.6911(3) 0.0398(9) Uani 1 1 d . . .
O7 O 0.6986(4) 0.2993(4) 0.8052(3) 0.0614(10) Uani 1 1 d . . .
O8 O 0.5872(4) 0.3737(4) 0.8675(3) 0.0621(10) Uani 1 1 d . . .
C9 C 0.9990(4) 0.7025(4) 0.7876(3) 0.0334(9) Uani 1 1 d . . .
N4 N 0.5062(5) 0.3684(4) 1.1430(3) 0.0553(11) Uani 1 1 d . . .
C8 C 1.1185(5) 0.7808(4) 0.7622(3) 0.0431(11) Uani 1 1 d . . .
H8A H 1.2012 0.7821 0.7872 0.052 Uiso 1 1 calc R . .
C6 C 1.0901(5) 0.3779(4) 0.9103(3) 0.0335(9) Uani 1 1 d . . .
C12 C 0.9964(5) 0.6211(4) 0.8588(3) 0.0341(9) Uani 1 1 d . . .
N5 N 0.5998(5) 0.3237(4) 0.7993(3) 0.0613(13) Uani 1 1 d . . .
C3 C 1.0737(4) 0.2883(4) 0.8351(3) 0.0329(9) Uani 1 1 d . . .
C2 C 1.1849(5) 0.2872(4) 0.8047(3) 0.0421(11) Uani 1 1 d . . .
H2A H 1.2736 0.3410 0.8326 0.051 Uiso 1 1 calc R . .
C10 C 0.8824(5) 0.7017(5) 0.7464(4) 0.0565(15) Uani 1 1 d . . .
H10A H 0.7976 0.6467 0.7603 0.068 Uiso 1 1 calc R . .
C4 C 0.9472(5) 0.2065(5) 0.7931(3) 0.0473(12) Uani 1 1 d . . .
H4A H 0.8687 0.2041 0.8127 0.057 Uiso 1 1 calc R . .
C1 C 1.1647(5) 0.2061(4) 0.7326(3) 0.0441(11) Uani 1 1 d . . .
H1A H 1.2416 0.2066 0.7117 0.053 Uiso 1 1 calc R . .
C7 C 1.1168(5) 0.8573(4) 0.7001(3) 0.0443(11) Uani 1 1 d . . .
H7A H 1.2000 0.9104 0.6831 0.053 Uiso 1 1 calc R . .
N6 N 0.5140(5) 0.9615(5) 0.6793(4) 0.0688(14) Uani 1 1 d . . .
C5 C 0.9355(5) 0.1279(5) 0.7223(4) 0.0505(13) Uani 1 1 d . . .
H5A H 0.8478 0.0717 0.6944 0.061 Uiso 1 1 calc R . .
N3 N 0.7195(6) 0.0220(4) 1.0278(4) 0.0695(14) Uani 1 1 d . . .
C18 C 0.6044(5) 0.3472(5) 1.1213(4) 0.0472(12) Uani 1 1 d . . .
H18A H 0.6766 0.3593 1.1670 0.057 Uiso 1 1 calc R . .
C11 C 0.8887(5) 0.7804(5) 0.6854(4) 0.0570(15) Uani 1 1 d . . .
H11A H 0.8067 0.7782 0.6577 0.068 Uiso 1 1 calc R . .
C15 C 0.6869(6) 0.1080(4) 1.0124(4) 0.0523(13) Uani 1 1 d . . .
H15A H 0.6263 0.1168 1.0472 0.063 Uiso 1 1 calc R . .
O9 O 0.5213(7) 0.2982(7) 0.7300(4) 0.127(2) Uani 1 1 d . . .
N7 N -0.0071(7) 0.3924(5) 0.5914(4) 0.0855(18) Uani 1 1 d D . .
O10 O 0.4920(8) 0.8964(6) 0.8148(4) 0.138(3) Uani 1 1 d . . .
C17 C 0.5043(8) 0.4045(8) 1.2346(5) 0.086(2) Uani 1 1 d . . .
H17A H 0.5849 0.4109 1.2727 0.128 Uiso 1 1 calc R . .
H17B H 0.4236 0.3450 1.2549 0.128 Uiso 1 1 calc R . .
H17C H 0.5032 0.4819 1.2382 0.128 Uiso 1 1 calc R . .
C20 C 0.5659(7) 1.0623(7) 0.6304(5) 0.0773(19) Uani 1 1 d . . .
H20A H 0.6186 1.1346 0.6721 0.116 Uiso 1 1 calc R . .
H20B H 0.4910 1.0691 0.5949 0.116 Uiso 1 1 calc R . .
H20C H 0.6239 1.0525 0.5906 0.116 Uiso 1 1 calc R . .
C21 C 0.5358(9) 0.9756(7) 0.7667(5) 0.093(2) Uani 1 1 d . . .
H21A H 0.5903 1.0543 0.7950 0.111 Uiso 1 1 calc R . .
C14 C 0.6606(8) -0.0635(6) 1.0922(5) 0.083(2) Uani 1 1 d . . .
H14A H 0.5996 -0.0425 1.1216 0.125 Uiso 1 1 calc R . .
H14B H 0.7329 -0.0608 1.1371 0.125 Uiso 1 1 calc R . .
H14C H 0.6102 -0.1440 1.0608 0.125 Uiso 1 1 calc R . .
C19 C 0.4348(9) 0.8466(7) 0.6286(6) 0.110(3) Uani 1 1 d . . .
H19A H 0.4052 0.7849 0.6694 0.165 Uiso 1 1 calc R . .
H19B H 0.4895 0.8306 0.5892 0.165 Uiso 1 1 calc R . .
H19C H 0.3557 0.8462 0.5925 0.165 Uiso 1 1 calc R . .
C16 C 0.3953(8) 0.3548(8) 1.0757(6) 0.097(3) Uani 1 1 d . . .
H16A H 0.4090 0.3300 1.0172 0.145 Uiso 1 1 calc R . .
H16B H 0.3916 0.4310 1.0738 0.145 Uiso 1 1 calc R . .
H16C H 0.3104 0.2942 1.0906 0.145 Uiso 1 1 calc R . .
O11 O 0.1761(11) 0.5323(11) 0.6691(8) 0.200(4) Uani 1 1 d DU . .
C24 C 0.0617(14) 0.4758(13) 0.6634(10) 0.230(8) Uani 1 1 d DU . .
H24A H 0.0151 0.4868 0.7084 0.276 Uiso 1 1 calc R . .
C13 C 0.8152(12) 0.0062(10) 0.9778(10) 0.165(6) Uani 1 1 d . . .
H13A H 0.8472 0.0688 0.9378 0.248 Uiso 1 1 calc R . .
H13B H 0.7706 -0.0720 0.9425 0.248 Uiso 1 1 calc R . .
H13C H 0.8920 0.0113 1.0196 0.248 Uiso 1 1 calc R . .
C23 C -0.0155(17) 0.3207(13) 0.5239(10) 0.190(6) Uani 1 1 d U . .
H23A H 0.0754 0.3353 0.5146 0.284 Uiso 1 1 calc R . .
H23B H -0.0619 0.3349 0.4701 0.284 Uiso 1 1 calc R . .
H23C H -0.0662 0.2379 0.5362 0.284 Uiso 1 1 calc R . .
C22 C -0.1417(19) 0.3683(18) 0.6021(13) 0.248(9) Uani 1 1 d U . .
H22A H -0.2056 0.3097 0.5533 0.372 Uiso 1 1 calc R . .
H22B H -0.1508 0.4422 0.6008 0.372 Uiso 1 1 calc R . .
H22C H -0.1610 0.3365 0.6593 0.372 Uiso 1 1 calc R . .
O1W O 0.5000 0.5000 1.5000 0.289(10) Uiso 1 2 d S . .


_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
Gd1 O2 2.319(3) . ?
Gd1 O3 2.351(3) 2_767 ?
Gd1 O6 2.381(3) . ?
Gd1 O4 2.381(3) . ?
Gd1 O5 2.407(3) . ?
Gd1 O1 2.411(3) 2_767 ?
Gd1 O8 2.503(4) . ?
Gd1 O7 2.506(4) . ?
Gd1 N5 2.922(4) . ?
I1 Cu1 2.6110(7) . ?
I1 Cu1 2.6312(7) 2_756 ?
Cu1 N2 2.077(4) 1_545 ?
Cu1 N1 2.084(4) . ?
Cu1 I1 2.6312(7) 2_756 ?
Cu1 Cu1 2.6841(11) 2_756 ?
O4 C12 1.254(5) . ?
O2 C6 1.258(5) . ?
O3 C12 1.254(5) . ?
O3 Gd1 2.351(3) 2_767 ?
O1 C6 1.250(5) . ?
O1 Gd1 2.411(3) 2_767 ?
O5 C15 1.237(6) . ?
O6 C18 1.243(6) . ?
N2 C7 1.334(6) . ?
N2 C11 1.339(6) . ?
N2 Cu1 2.077(4) 1_565 ?
N1 C1 1.337(6) . ?
N1 C5 1.343(6) . ?
O7 N5 1.267(6) . ?
O8 N5 1.244(6) . ?
C9 C10 1.373(7) . ?
C9 C8 1.378(6) . ?
C9 C12 1.515(6) . ?
N4 C18 1.315(7) . ?
N4 C17 1.449(8) . ?
N4 C16 1.451(8) . ?
C8 C7 1.379(7) . ?
C6 C3 1.504(6) . ?
N5 O9 1.216(6) . ?
C3 C4 1.381(6) . ?
C3 C2 1.386(6) . ?
C2 C1 1.390(6) . ?
C10 C11 1.371(7) . ?
C4 C5 1.382(7) . ?
N6 C21 1.309(9) . ?
N6 C20 1.425(9) . ?
N6 C19 1.439(9) . ?
N3 C15 1.308(7) . ?
N3 C13 1.462(11) . ?
N3 C14 1.471(8) . ?
N7 C23 1.302(14) . ?
N7 C24 1.367(10) . ?
N7 C22 1.432(18) . ?
O10 C21 1.218(9) . ?
O11 C24 1.146(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
O2 Gd1 O3 77.79(11) . 2_767 ?
O2 Gd1 O6 147.45(12) . . ?
O3 Gd1 O6 77.05(12) 2_767 . ?
O2 Gd1 O4 76.76(11) . . ?
O3 Gd1 O4 128.54(11) 2_767 . ?
O6 Gd1 O4 135.62(12) . . ?
O2 Gd1 O5 78.09(13) . . ?
O3 Gd1 O5 75.97(12) 2_767 . ?
O6 Gd1 O5 76.03(13) . . ?
O4 Gd1 O5 138.81(12) . . ?
O2 Gd1 O1 124.14(11) . 2_767 ?
O3 Gd1 O1 81.39(11) 2_767 2_767 ?
O6 Gd1 O1 71.60(11) . 2_767 ?
O4 Gd1 O1 77.22(11) . 2_767 ?
O5 Gd1 O1 143.82(12) . 2_767 ?
O2 Gd1 O8 132.18(12) . . ?
O3 Gd1 O8 147.92(12) 2_767 . ?
O6 Gd1 O8 70.90(13) . . ?
O4 Gd1 O8 76.95(13) . . ?
O5 Gd1 O8 97.12(14) . . ?
O1 Gd1 O8 87.30(12) 2_767 . ?
O2 Gd1 O7 83.96(13) . . ?
O3 Gd1 O7 145.23(12) 2_767 . ?
O6 Gd1 O7 105.85(14) . . ?
O4 Gd1 O7 73.94(13) . . ?
O5 Gd1 O7 71.42(13) . . ?
O1 Gd1 O7 132.97(12) 2_767 . ?
O8 Gd1 O7 50.54(13) . . ?
O2 Gd1 N5 108.37(14) . . ?
O3 Gd1 N5 157.81(13) 2_767 . ?
O6 Gd1 N5 88.43(14) . . ?
O4 Gd1 N5 73.42(13) . . ?
O5 Gd1 N5 84.36(14) . . ?
O1 Gd1 N5 110.11(13) 2_767 . ?
O8 Gd1 N5 25.01(13) . . ?
O7 Gd1 N5 25.54(13) . . ?
Cu1 I1 Cu1 61.60(2) . 2_756 ?
N2 Cu1 N1 100.45(16) 1_545 . ?
N2 Cu1 I1 109.48(11) 1_545 . ?
N1 Cu1 I1 109.57(11) . . ?
N2 Cu1 I1 107.88(11) 1_545 2_756 ?
N1 Cu1 I1 109.54(11) . 2_756 ?
I1 Cu1 I1 118.40(2) . 2_756 ?
N2 Cu1 Cu1 128.71(11) 1_545 2_756 ?
N1 Cu1 Cu1 130.82(12) . 2_756 ?
I1 Cu1 Cu1 59.57(2) . 2_756 ?
I1 Cu1 Cu1 58.83(2) 2_756 2_756 ?
C12 O4 Gd1 137.5(3) . . ?
C6 O2 Gd1 178.9(3) . . ?
C12 O3 Gd1 139.0(3) . 2_767 ?
C6 O1 Gd1 110.5(3) . 2_767 ?
C15 O5 Gd1 130.2(3) . . ?
C18 O6 Gd1 127.3(3) . . ?
C7 N2 C11 116.5(4) . . ?
C7 N2 Cu1 121.0(3) . 1_565 ?
C11 N2 Cu1 121.9(3) . 1_565 ?
C1 N1 C5 117.2(4) . . ?
C1 N1 Cu1 122.9(3) . . ?
C5 N1 Cu1 119.7(3) . . ?
N5 O7 Gd1 95.9(3) . . ?
N5 O8 Gd1 96.7(3) . . ?
C10 C9 C8 117.5(4) . . ?
C10 C9 C12 121.2(4) . . ?
C8 C9 C12 121.3(4) . . ?
C18 N4 C17 121.3(5) . . ?
C18 N4 C16 120.7(5) . . ?
C17 N4 C16 117.9(5) . . ?
C9 C8 C7 119.4(4) . . ?
O1 C6 O2 123.2(4) . . ?
O1 C6 C3 118.3(4) . . ?
O2 C6 C3 118.5(4) . . ?
O4 C12 O3 126.9(4) . . ?
O4 C12 C9 116.8(4) . . ?
O3 C12 C9 116.3(4) . . ?
O9 N5 O8 122.2(6) . . ?
O9 N5 O7 121.0(6) . . ?
O8 N5 O7 116.8(4) . . ?
O9 N5 Gd1 178.7(6) . . ?
O8 N5 Gd1 58.3(2) . . ?
O7 N5 Gd1 58.5(2) . . ?
C4 C3 C2 118.0(4) . . ?
C4 C3 C6 120.9(4) . . ?
C2 C3 C6 121.1(4) . . ?
C3 C2 C1 119.0(4) . . ?
C11 C10 C9 119.8(5) . . ?
C3 C4 C5 119.5(4) . . ?
N1 C1 C2 123.2(4) . . ?
N2 C7 C8 123.4(4) . . ?
C21 N6 C20 120.1(6) . . ?
C21 N6 C19 122.6(7) . . ?
C20 N6 C19 117.2(6) . . ?
N1 C5 C4 123.0(5) . . ?
C15 N3 C13 119.6(6) . . ?
C15 N3 C14 122.8(6) . . ?
C13 N3 C14 117.6(6) . . ?
O6 C18 N4 123.5(5) . . ?
N2 C11 C10 123.4(5) . . ?
O5 C15 N3 125.4(6) . . ?
C23 N7 C24 153.3(13) . . ?
C23 N7 C22 107.4(12) . . ?
C24 N7 C22 99.0(12) . . ?
O10 C21 N6 125.5(8) . . ?
O11 C24 N7 119.6(16) . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        24.80
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         1.280
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.107
