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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_4
_database_code_depnum_ccdc_archive 'CCDC 1554035'
_audit_update_record             
;
2017-07-31 deposited with the CCDC.
2017-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H39 Cu2 Ho N8 O13'
_chemical_formula_weight         1107.78

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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   20.342(5)
_cell_length_b                   10.374(5)
_cell_length_c                   19.448(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.891(5)
_cell_angle_gamma                90
_cell_volume                     4030(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16606
_cell_measurement_theta_min      2.039
_cell_measurement_theta_max      24.000

_exptl_crystal_description       prismatic
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_F_000             2208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.042
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.028
_exptl_absorpt_coefficient_mu    3.067
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16606
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.039
_diffrn_reflns_theta_max         24.000
_diffrn_reflns_theta_full        24.000
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measured_fraction_theta_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_point_group_measured_fraction_full 0.954
_reflns_number_total             3010
_reflns_number_gt                2474
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0470P)²+39.7645P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3010
_refine_ls_number_parameters     327
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.1258
_refine_ls_wR_factor_gt          0.1132
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.99165(4) 0.43965(9) 0.35109(5) 0.0496(3) Uani 1 1 d . . . . .
Ho1 Ho 1.01176(5) 0.18861(6) 0.26536(5) 0.0384(3) Uani 0.5 1 d . . P . .
N1 N 0.9041(3) 0.5018(6) 0.3706(3) 0.0531(16) Uani 1 1 d . . . . .
N2 N 1.0371(3) 0.6019(6) 0.3678(4) 0.0639(18) Uani 1 1 d . . . . .
N4 N 0.9024(4) -0.0110(8) 0.2068(4) 0.068(2) Uani 1 1 d . . . . .
O1 O 0.9560(2) 0.2670(4) 0.3413(2) 0.0449(11) Uani 1 1 d . . . . .
O2 O 1.0590(2) 0.3729(6) 0.2983(3) 0.0570(14) Uani 1 1 d . . . . .
O3A O 0.9454(7) 0.0541(13) 0.1697(6) 0.067(3) Uani 0.5 1 d . . P A 1
O3B O 0.9568(5) -0.0327(13) 0.1937(8) 0.069(3) Uani 0.5 1 d . . P A 2
O4 O 0.8608(3) -0.0930(8) 0.1867(4) 0.096(2) Uani 1 1 d . . . . .
O5 O 0.9022(4) 0.0551(6) 0.2575(4) 0.090(2) Uani 1 1 d . . . . .
C1 C 0.9264(3) 0.2220(7) 0.3919(4) 0.0444(17) Uani 1 1 d . . . . .
C2 C 0.9398(4) 0.0961(8) 0.4158(4) 0.056(2) Uani 1 1 d . . . . .
H2 H 0.969537 0.045524 0.396556 0.067 Uiso 1 1 calc R U . . .
C3 C 0.9092(4) 0.0456(9) 0.4679(5) 0.071(2) Uani 1 1 d . . . . .
H3 H 0.919649 -0.037399 0.484506 0.085 Uiso 1 1 calc R U . . .
C4 C 0.8638(5) 0.1177(12) 0.4949(5) 0.082(3) Uani 1 1 d . . . . .
H4 H 0.842902 0.082992 0.529343 0.099 Uiso 1 1 calc R U . . .
C5 C 0.8489(4) 0.2412(12) 0.4714(5) 0.075(3) Uani 1 1 d . . . . .
H5 H 0.817893 0.289000 0.490227 0.090 Uiso 1 1 calc R U . . .
C6 C 0.8795(3) 0.2968(8) 0.4196(4) 0.0515(19) Uani 1 1 d . . . . .
C7 C 0.8625(4) 0.4297(8) 0.3968(4) 0.059(2) Uani 1 1 d . . . . .
C8 C 0.7937(4) 0.4783(10) 0.4025(6) 0.093(3) Uani 1 1 d . . . . .
H8A H 0.774906 0.525059 0.360780 0.140 Uiso 1 1 calc R U . . .
H8B H 0.797140 0.534214 0.442325 0.140 Uiso 1 1 calc R U . . .
H8C H 0.765350 0.406514 0.407909 0.140 Uiso 1 1 calc R U . . .
C9 C 0.8812(5) 0.6330(9) 0.3506(6) 0.082(3) Uani 1 1 d . . . . .
H9A H 0.860526 0.668657 0.387436 0.099 Uiso 1 1 calc R U . . .
H9B H 0.847062 0.628250 0.308495 0.099 Uiso 1 1 calc R U . . .
C10 C 0.9350(5) 0.7234(9) 0.3376(6) 0.091(3) Uani 1 1 d . . . . .
H10A H 0.944039 0.706855 0.291175 0.109 Uiso 1 1 calc R U . . .
H10B H 0.918406 0.811046 0.338017 0.109 Uiso 1 1 calc R U . . .
C11 C 0.9993(5) 0.7138(8) 0.3894(6) 0.077(3) Uani 1 1 d . . . . .
H11A H 1.025078 0.792463 0.389334 0.093 Uiso 1 1 calc R U . . .
H11B H 0.990485 0.700215 0.436109 0.093 Uiso 1 1 calc R U . . .
C12 C 1.0978(4) 0.6213(10) 0.3619(5) 0.070(2) Uani 1 1 d . . . . .
H12 H 1.114866 0.702822 0.374775 0.084 Uiso 1 1 calc R U . . .
C13 C 1.1430(4) 0.5332(10) 0.3379(5) 0.068(3) Uani 1 1 d . . . . .
C14 C 1.2107(5) 0.5715(12) 0.3448(6) 0.093(3) Uani 1 1 d . . . . .
H14 H 1.224187 0.649673 0.366415 0.111 Uiso 1 1 calc R U . . .
C15 C 1.2566(5) 0.4974(15) 0.3208(6) 0.107(4) Uani 1 1 d . . . . .
H15 H 1.300731 0.524623 0.325291 0.128 Uiso 1 1 calc R U . . .
C16 C 1.2367(4) 0.3825(13) 0.2899(6) 0.090(3) Uani 1 1 d . . . . .
H16 H 1.268172 0.331407 0.273722 0.108 Uiso 1 1 calc R U . . .
C17 C 1.1709(4) 0.3387(11) 0.2817(5) 0.074(3) Uani 1 1 d . . . . .
H17 H 1.158967 0.259977 0.260049 0.089 Uiso 1 1 calc R U . . .
C18 C 1.1222(4) 0.4146(9) 0.3066(4) 0.058(2) Uani 1 1 d . . . . .
N1B N 1.077(4) 0.364(6) 0.465(3) 0.13(2) Uani 0.5 1 d . . P B 1
C2B C 1.1229(17) 0.298(3) 0.4651(17) 0.074(9) Uani 0.5 1 d D . P B 1
C3B C 1.185(2) 0.225(6) 0.474(3) 0.14(3) Uani 0.5 1 d D . P B 1
H3B1 H 1.217642 0.264254 0.509493 0.217 Uiso 0.5 1 calc R U P B 1
H3B2 H 1.200580 0.223058 0.430571 0.217 Uiso 0.5 1 calc R U P B 1
H3B3 H 1.176549 0.138073 0.487737 0.217 Uiso 0.5 1 calc R U P B 1
O6 O 0.9084(6) 0.1735(12) 0.1191(8) 0.077(3) Uani 0.5 1 d . . P C 2
N7 N 0.8887(11) 0.253(2) 0.0641(14) 0.069(7) Uani 0.5 1 d . . P C 2
O8 O 0.8326(17) 0.227(3) 0.0343(18) 0.109(10) Uani 0.5 1 d . . P C 2
O9 O 0.9268(19) 0.339(4) 0.049(2) 0.072(8) Uani 0.5 1 d . . P C 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 1.919(6) . ?
Cu1 O1 1.929(5) . ?
Cu1 O2 1.986(5) . ?
Cu1 N1 1.997(6) . ?
Cu1 Ho1 3.1603(17) . ?
Cu1 Ho1 3.4434(16) 2_755 ?
Ho1 Ho1 0.6912(13) 2_755 ?
Ho1 O3A 1.971(11) 2_755 ?
Ho1 O2 2.180(6) . ?
Ho1 O1 2.182(5) . ?
Ho1 O5 2.340(6) 2_755 ?
Ho1 O1 2.430(5) 2_755 ?
Ho1 O3B 2.474(13) 2_755 ?
Ho1 O3A 2.506(12) . ?
Ho1 O6 2.517(14) 2_755 ?
Ho1 O2 2.565(5) 2_755 ?
Ho1 O5 2.604(6) . ?
Ho1 N4 2.697(9) 2_755 ?
N1 C7 1.302(10) . ?
N1 C9 1.467(11) . ?
N2 C12 1.277(10) . ?
N2 C11 1.495(11) . ?
N4 O5 1.202(9) . ?
N4 O3B 1.203(12) . ?
N4 O4 1.212(9) . ?
N4 O3A 1.408(13) . ?
O1 C1 1.331(8) . ?
O2 C18 1.337(8) . ?
C1 C2 1.396(11) . ?
C1 C6 1.414(10) . ?
C2 C3 1.389(11) . ?
C3 C4 1.369(13) . ?
C4 C5 1.375(15) . ?
C5 C6 1.404(12) . ?
C6 C7 1.470(12) . ?
C7 C8 1.511(10) . ?
C9 C10 1.499(14) . ?
C10 C11 1.496(13) . ?
C12 C13 1.436(13) . ?
C13 C18 1.402(13) . ?
C13 C14 1.415(11) . ?
C14 C15 1.359(16) . ?
C15 C16 1.361(18) . ?
C16 C17 1.394(12) . ?
C17 C18 1.421(12) . ?
N1B C2B 1.16(8) . ?
C2B C3B 1.45(2) . ?
O6 N7 1.35(3) . ?
N7 O8 1.21(3) . ?
N7 O9 1.26(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cu1 O1 172.8(3) . . ?
N2 Cu1 O2 92.1(3) . . ?
O1 Cu1 O2 84.7(2) . . ?
N2 Cu1 N1 95.9(3) . . ?
O1 Cu1 N1 89.2(2) . . ?
O2 Cu1 N1 159.8(2) . . ?
N2 Cu1 Ho1 134.9(2) . . ?
O1 Cu1 Ho1 42.79(13) . . ?
O2 Cu1 Ho1 43.01(16) . . ?
N1 Cu1 Ho1 125.13(17) . . ?
N2 Cu1 Ho1 136.4(2) . 2_755 ?
O1 Cu1 Ho1 43.27(13) . 2_755 ?
O2 Cu1 Ho1 47.62(15) . 2_755 ?
N1 Cu1 Ho1 117.49(17) . 2_755 ?
Ho1 Cu1 Ho1 10.97(2) . 2_755 ?
Ho1 Ho1 O3A 134.7(5) 2_755 2_755 ?
Ho1 Ho1 O2 116.63(15) 2_755 . ?
O3A Ho1 O2 108.4(5) 2_755 . ?
Ho1 Ho1 O1 102.8(3) 2_755 . ?
O3A Ho1 O1 93.1(3) 2_755 . ?
O2 Ho1 O1 74.42(17) . . ?
Ho1 Ho1 O5 104.8(3) 2_755 2_755 ?
O3A Ho1 O5 56.4(3) 2_755 2_755 ?
O2 Ho1 O5 105.7(2) . 2_755 ?
O1 Ho1 O5 148.5(2) . 2_755 ?
Ho1 Ho1 O1 61.1(2) 2_755 2_755 ?
O3A Ho1 O1 128.7(3) 2_755 2_755 ?
O2 Ho1 O1 77.41(17) . 2_755 ?
O1 Ho1 O1 135.4(2) . 2_755 ?
O5 Ho1 O1 72.74(19) 2_755 2_755 ?
Ho1 Ho1 O3B 111.9(3) 2_755 2_755 ?
O3A Ho1 O3B 23.2(5) 2_755 2_755 ?
O2 Ho1 O3B 130.3(3) . 2_755 ?
O1 Ho1 O3B 105.3(4) . 2_755 ?
O5 Ho1 O3B 49.8(3) 2_755 2_755 ?
O1 Ho1 O3B 119.4(4) 2_755 2_755 ?
Ho1 Ho1 O3A 34.0(4) 2_755 . ?
O3A Ho1 O3A 101.1(8) 2_755 . ?
O2 Ho1 O3A 148.4(4) . . ?
O1 Ho1 O3A 115.7(3) . . ?
O5 Ho1 O3A 81.2(4) 2_755 . ?
O1 Ho1 O3A 75.4(3) 2_755 . ?
Ho1 Ho1 O6 175.1(3) 2_755 2_755 ?
O3A Ho1 O6 41.5(5) 2_755 2_755 ?
O2 Ho1 O6 67.6(3) . 2_755 ?
O1 Ho1 O6 75.5(3) . 2_755 ?
O5 Ho1 O6 75.7(4) 2_755 2_755 ?
O1 Ho1 O6 123.3(3) 2_755 2_755 ?
O3B Ho1 O6 64.6(4) 2_755 2_755 ?
O3A Ho1 O6 142.6(5) . 2_755 ?
Ho1 Ho1 O2 49.43(13) 2_755 2_755 ?
O3A Ho1 O2 167.5(3) 2_755 2_755 ?
O2 Ho1 O2 70.4(3) . 2_755 ?
O1 Ho1 O2 74.49(16) . 2_755 ?
O5 Ho1 O2 136.1(2) 2_755 2_755 ?
O1 Ho1 O2 63.68(15) 2_755 2_755 ?
O3A Ho1 O2 83.2(4) . 2_755 ?
Ho1 Ho1 O5 60.3(2) 2_755 . ?
O3A Ho1 O5 86.0(5) 2_755 . ?
O2 Ho1 O5 143.92(19) . . ?
O1 Ho1 O5 71.87(18) . . ?
O5 Ho1 O5 109.7(3) 2_755 . ?
O1 Ho1 O5 119.6(2) 2_755 . ?
O3B Ho1 O5 72.0(3) 2_755 . ?
O3A Ho1 O5 47.6(3) . . ?
O6 Ho1 O5 114.8(3) 2_755 . ?
O2 Ho1 O5 88.4(2) 2_755 . ?
Ho1 Ho1 N4 119.3(2) 2_755 2_755 ?
O3A Ho1 N4 30.3(3) 2_755 2_755 ?
O2 Ho1 N4 112.4(2) . 2_755 ?
O1 Ho1 N4 123.4(2) . 2_755 ?
O5 Ho1 N4 26.41(19) 2_755 2_755 ?
O1 Ho1 N4 99.15(18) 2_755 2_755 ?
O3A Ho1 N4 87.7(4) . 2_755 ?
O2 Ho1 N4 162.13(19) 2_755 2_755 ?
O5 Ho1 N4 96.8(2) . 2_755 ?
C7 N1 C9 116.1(7) . . ?
C7 N1 Cu1 123.9(5) . . ?
C9 N1 Cu1 119.9(6) . . ?
C12 N2 C11 117.4(7) . . ?
C12 N2 Cu1 124.5(7) . . ?
C11 N2 Cu1 118.1(5) . . ?
O5 N4 O3B 115.2(10) . . ?
O5 N4 O4 123.7(7) . . ?
O3B N4 O4 114.5(9) . . ?
O5 N4 O3A 104.2(8) . . ?
O4 N4 O3A 129.5(8) . . ?
O5 N4 Ho1 60.0(4) . 2_755 ?
O4 N4 Ho1 172.0(7) . 2_755 ?
O3A N4 Ho1 45.0(5) . 2_755 ?
C1 O1 Cu1 117.8(4) . . ?
C1 O1 Ho1 137.3(4) . . ?
Cu1 O1 Ho1 100.31(18) . . ?
C1 O1 Ho1 138.3(4) . 2_755 ?
Cu1 O1 Ho1 103.77(18) . 2_755 ?
Ho1 O1 Ho1 16.10(5) . 2_755 ?
C18 O2 Cu1 124.4(5) . . ?
C18 O2 Ho1 132.8(5) . . ?
Cu1 O2 Ho1 98.58(19) . . ?
C18 O2 Ho1 137.6(5) . 2_755 ?
Cu1 O2 Ho1 97.51(17) . 2_755 ?
Ho1 O2 Ho1 13.94(4) . 2_755 ?
N4 O3A Ho1 104.7(7) . 2_755 ?
N4 O3A Ho1 100.7(7) . . ?
Ho1 O3A Ho1 11.30(12) 2_755 . ?
N4 O3B Ho1 87.2(8) . 2_755 ?
N4 O3B Ho1 92.2(8) . . ?
Ho1 O3B Ho1 13.21(7) 2_755 . ?
N4 O5 Ho1 93.6(5) . 2_755 ?
N4 O5 Ho1 102.5(5) . . ?
Ho1 O5 Ho1 14.87(6) 2_755 . ?
O1 C1 C2 119.2(6) . . ?
O1 C1 C6 121.4(6) . . ?
C2 C1 C6 119.3(7) . . ?
C3 C2 C1 120.6(8) . . ?
C4 C3 C2 120.2(9) . . ?
C3 C4 C5 120.2(8) . . ?
C4 C5 C6 121.5(9) . . ?
C5 C6 C1 118.1(8) . . ?
C5 C6 C7 119.4(8) . . ?
C1 C6 C7 122.5(7) . . ?
N1 C7 C6 121.5(7) . . ?
N1 C7 C8 121.1(8) . . ?
C6 C7 C8 117.3(8) . . ?
N1 C9 C10 114.9(8) . . ?
C11 C10 C9 114.7(9) . . ?
N2 C11 C10 107.1(8) . . ?
N2 C12 C13 128.2(9) . . ?
C18 C13 C14 119.8(10) . . ?
C18 C13 C12 122.7(7) . . ?
C14 C13 C12 117.5(9) . . ?
C15 C14 C13 121.8(11) . . ?
C14 C15 C16 118.8(9) . . ?
C15 C16 C17 122.3(11) . . ?
C16 C17 C18 119.8(10) . . ?
O2 C18 C13 122.8(8) . . ?
O2 C18 C17 119.7(8) . . ?
C13 C18 C17 117.4(7) . . ?
N1B C2B C3B 172(6) . . ?
O8 N7 O9 128(4) . . ?
O8 N7 O6 111(2) . . ?
O9 N7 O6 121(3) . . ?

_refine_diff_density_max         0.879
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.102

####################################################################### 
# 
# 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 1554034'
_audit_update_record             
;
2017-07-31 deposited with the CCDC.
2017-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H42 Cu2 Dy N9 O13'
_chemical_formula_weight         1146.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   17.317(5)
_cell_length_b                   17.317(5)
_cell_length_c                   30.722(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9213(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10506
_cell_measurement_theta_min      1.350
_cell_measurement_theta_max      25.052

_exptl_crystal_description       prismatic
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_F_000             4584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    2.592
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_process_details   SADABS
_diffrn_ambient_temperature      293(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_reflns_number            10506
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.350
_diffrn_reflns_theta_max         25.052
_diffrn_reflns_theta_full        25.052
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             4049
_reflns_number_gt                2793
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1006P)²+6.8432P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4049
_refine_ls_number_parameters     297
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0709
_refine_ls_wR_factor_ref         0.1996
_refine_ls_wR_factor_gt          0.1823
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_restrained_S_all      1.161
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.51549(6) 0.07150(6) 0.62904(3) 0.0517(3) Uani 1 1 d . . . . .
Dy1 Dy 0.500000 0.250000 0.59146(2) 0.0619(3) Uani 1 2 d S T P . .
N1 N 0.4699(4) 0.0375(4) 0.6858(3) 0.069(2) Uani 1 1 d . . . . .
N2 N 0.4980(4) -0.0259(4) 0.5969(3) 0.0582(19) Uani 1 1 d . . . . .
N4 N 0.500000 0.250000 0.4970(5) 0.087(4) Uani 1 2 d S TU P . .
N5 N 0.3345(8) 0.1736(7) 0.6023(4) 0.102(3) Uani 1 1 d . . . . .
O1 O 0.5297(3) 0.1758(3) 0.65276(18) 0.0538(14) Uani 1 1 d . . . . .
O2 O 0.5488(3) 0.1250(3) 0.57517(19) 0.0523(14) Uani 1 1 d . . . . .
O3 O 0.500000 0.250000 0.4558(5) 0.131(5) Uani 1 2 d S TU P . .
O4 O 0.4510(5) 0.2142(4) 0.5169(3) 0.091(2) Uani 1 1 d . U . . .
O6 O 0.3908(8) 0.1361(7) 0.6030(4) 0.144(4) Uani 1 1 d . U . . .
O7 O 0.3471(7) 0.2447(8) 0.5959(4) 0.145(4) Uani 1 1 d . U . . .
O5 O 0.2740(6) 0.1503(7) 0.6074(4) 0.147(4) Uani 1 1 d . . . . .
C1 C 0.5603(5) 0.1817(5) 0.6916(3) 0.058(2) Uani 1 1 d . . . . .
C2 C 0.6118(5) 0.2422(6) 0.6999(3) 0.067(2) Uani 1 1 d . . . . .
H2 H 0.621914 0.278218 0.678143 0.081 Uiso 1 1 calc R U . . .
C3 C 0.6489(7) 0.2497(8) 0.7408(5) 0.096(4) Uani 1 1 d . . . . .
H3 H 0.681425 0.291436 0.745771 0.115 Uiso 1 1 calc R U . . .
C4 C 0.6380(9) 0.1983(10) 0.7718(5) 0.121(5) Uani 1 1 d . . . . .
H4 H 0.666373 0.200133 0.797509 0.146 Uiso 1 1 calc R U . . .
C5 C 0.5816(9) 0.1401(8) 0.7649(4) 0.108(4) Uani 1 1 d . . . . .
H5 H 0.569753 0.107180 0.787826 0.129 Uiso 1 1 calc R U . . .
C6 C 0.5430(6) 0.1296(6) 0.7256(3) 0.070(3) Uani 1 1 d . . . . .
C7 C 0.4852(6) 0.0711(6) 0.7223(3) 0.071(3) Uani 1 1 d . . . . .
C8 C 0.4449(9) 0.0494(9) 0.7630(4) 0.123(5) Uani 1 1 d . . . . .
H8A H 0.448918 -0.005376 0.767353 0.185 Uiso 1 1 calc R U . . .
H8B H 0.391494 0.063704 0.761035 0.185 Uiso 1 1 calc R U . . .
H8C H 0.468309 0.075763 0.787167 0.185 Uiso 1 1 calc R U . . .
C9 C 0.4100(8) -0.0233(8) 0.6857(4) 0.105(4) Uani 1 1 d . . . . .
H9A H 0.363976 -0.003310 0.699705 0.126 Uiso 1 1 calc R U . . .
H9B H 0.428322 -0.066618 0.702869 0.126 Uiso 1 1 calc R U . . .
C10 C 0.3881(10) -0.0529(10) 0.6392(6) 0.137(5) Uani 1 1 d . U . . .
H10A H 0.347113 -0.090683 0.641931 0.165 Uiso 1 1 calc R U . . .
H10B H 0.368158 -0.009835 0.622443 0.165 Uiso 1 1 calc R U . . .
C11 C 0.4492(7) -0.0860(6) 0.6164(4) 0.089(3) Uani 1 1 d . . . . .
H11A H 0.429074 -0.119358 0.593736 0.107 Uiso 1 1 calc R U . . .
H11B H 0.479887 -0.117385 0.636065 0.107 Uiso 1 1 calc R U . . .
C12 C 0.5286(5) -0.0394(5) 0.5596(3) 0.060(2) Uani 1 1 d . . . . .
H12 H 0.516895 -0.086573 0.546719 0.072 Uiso 1 1 calc R U . . .
C13 C 0.5787(5) 0.0104(5) 0.5360(3) 0.0513(19) Uani 1 1 d . . . . .
C14 C 0.6199(5) -0.0231(5) 0.5005(3) 0.062(2) Uani 1 1 d . . . . .
H14 H 0.611374 -0.074773 0.493764 0.075 Uiso 1 1 calc R U . . .
C15 C 0.6709(6) 0.0176(6) 0.4764(3) 0.068(2) Uani 1 1 d . . . . .
H15 H 0.698045 -0.005540 0.453760 0.081 Uiso 1 1 calc R U . . .
C16 C 0.6814(6) 0.0935(6) 0.4862(3) 0.072(3) Uani 1 1 d . . . . .
H16 H 0.716857 0.121642 0.469916 0.086 Uiso 1 1 calc R U . . .
C17 C 0.6419(6) 0.1307(5) 0.5192(3) 0.059(2) Uani 1 1 d . . . . .
H17 H 0.651128 0.182729 0.524771 0.071 Uiso 1 1 calc R U . . .
C18 C 0.5879(4) 0.0898(4) 0.5444(3) 0.0443(18) Uani 1 1 d . . . . .
N3 N 0.6516(7) 0.0453(6) 0.6436(4) 0.098(3) Uani 1 1 d . . . . .
C19 C 0.7040(8) 0.0750(9) 0.6395(5) 0.104(4) Uani 1 1 d . . . . .
C20A C 0.7742(17) 0.1209(18) 0.6391(10) 0.120(13) Uiso 0.55(5) 1 d . . P . .
H20A H 0.803809 0.108695 0.613603 0.180 Uiso 0.55(5) 1 calc R U P . .
H20B H 0.761067 0.174785 0.638814 0.180 Uiso 0.55(5) 1 calc R U P . .
H20C H 0.804171 0.109668 0.664627 0.180 Uiso 0.55(5) 1 calc R U P . .
C20B C 0.760(5) 0.068(5) 0.610(3) 0.31(5) Uiso 0.45(5) 1 d . . P . .
H20D H 0.799940 0.104185 0.615619 0.458 Uiso 0.45(5) 1 calc R U P . .
H20E H 0.780167 0.016261 0.610777 0.458 Uiso 0.45(5) 1 calc R U P . .
H20F H 0.738478 0.077342 0.581345 0.458 Uiso 0.45(5) 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.963(5) . ?
Cu1 N2 1.978(7) . ?
Cu1 O2 1.982(6) . ?
Cu1 N1 2.002(8) . ?
Cu1 N3 2.441(12) . ?
Cu1 Dy1 3.3105(13) . ?
Dy1 O1 2.337(5) 2_655 ?
Dy1 O1 2.337(5) . ?
Dy1 O2 2.376(5) 2_655 ?
Dy1 O2 2.376(5) . ?
Dy1 O4 2.520(8) . ?
Dy1 O4 2.520(8) 2_655 ?
Dy1 O7 2.653(12) . ?
Dy1 O7 2.653(12) 2_655 ?
Dy1 O6 2.756(13) 2_655 ?
Dy1 O6 2.756(13) . ?
Dy1 N4 2.902(15) . ?
N1 C7 1.292(13) . ?
N1 C9 1.477(13) . ?
N2 C12 1.285(11) . ?
N2 C11 1.469(12) . ?
N4 O4 1.216(10) 2_655 ?
N4 O4 1.216(10) . ?
N4 O3 1.265(19) . ?
N5 O5 1.135(13) . ?
N5 O6 1.171(14) . ?
N5 O7 1.265(14) . ?
O1 C1 1.310(10) . ?
O2 C18 1.314(9) . ?
C1 C2 1.400(13) . ?
C1 C6 1.412(13) . ?
C2 C3 1.416(15) . ?
C2 H2 0.9300 . ?
C3 C4 1.318(18) . ?
C3 H3 0.9300 . ?
C4 C5 1.42(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.391(16) . ?
C5 H5 0.9300 . ?
C6 C7 1.428(15) . ?
C7 C8 1.481(15) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.56(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.392(19) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.423(12) . ?
C12 H12 0.9300 . ?
C13 C18 1.408(11) . ?
C13 C14 1.425(12) . ?
C14 C15 1.352(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.360(13) . ?
C15 H15 0.9300 . ?
C16 C17 1.384(12) . ?
C16 H16 0.9300 . ?
C17 C18 1.405(11) . ?
C17 H17 0.9300 . ?
N3 C19 1.051(15) . ?
C19 C20B 1.33(8) . ?
C19 C20A 1.45(3) . ?
C20A H20A 0.9600 . ?
C20A H20B 0.9600 . ?
C20A H20C 0.9600 . ?
C20B H20D 0.9600 . ?
C20B H20E 0.9600 . ?
C20B H20F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag

O1 Cu1 N2 171.6(3) . . ?
O1 Cu1 O2 81.0(2) . . ?
N2 Cu1 O2 91.5(3) . . ?
O1 Cu1 N1 89.8(3) . . ?
N2 Cu1 N1 97.1(3) . . ?
O2 Cu1 N1 168.2(3) . . ?
O1 Cu1 N3 89.0(3) . . ?
N2 Cu1 N3 94.6(4) . . ?
O2 Cu1 N3 87.6(3) . . ?
N1 Cu1 N3 99.6(4) . . ?
O1 Dy1 O1 72.6(3) 2_655 . ?
O1 Dy1 O2 65.85(19) 2_655 2_655 ?
O1 Dy1 O2 138.46(19) . 2_655 ?
O1 Dy1 O2 138.46(19) 2_655 . ?
O1 Dy1 O2 65.85(19) . . ?
O2 Dy1 O2 155.7(3) 2_655 . ?
O1 Dy1 O4 142.5(2) 2_655 . ?
O1 Dy1 O4 132.2(2) . . ?
O2 Dy1 O4 85.0(2) 2_655 . ?
O2 Dy1 O4 72.8(2) . . ?
O1 Dy1 O4 132.2(2) 2_655 2_655 ?
O1 Dy1 O4 142.5(2) . 2_655 ?
O2 Dy1 O4 72.8(2) 2_655 2_655 ?
O2 Dy1 O4 85.0(2) . 2_655 ?
O4 Dy1 O4 49.3(4) . 2_655 ?
O1 Dy1 O7 76.0(3) 2_655 . ?
O1 Dy1 O7 99.1(3) . . ?
O2 Dy1 O7 71.8(3) 2_655 . ?
O2 Dy1 O7 109.5(3) . . ?
O4 Dy1 O7 72.7(3) . . ?
O4 Dy1 O7 113.1(3) 2_655 . ?
O1 Dy1 O7 99.1(3) 2_655 2_655 ?
O1 Dy1 O7 76.0(3) . 2_655 ?
O2 Dy1 O7 109.5(3) 2_655 2_655 ?
O2 Dy1 O7 71.8(3) . 2_655 ?
O4 Dy1 O7 113.1(3) . 2_655 ?
O4 Dy1 O7 72.7(3) 2_655 2_655 ?
O7 Dy1 O7 174.1(5) . 2_655 ?
O1 Dy1 O6 69.7(3) 2_655 2_655 ?
O1 Dy1 O6 98.0(3) . 2_655 ?
O2 Dy1 O6 67.6(3) 2_655 2_655 ?
O2 Dy1 O6 115.8(3) . 2_655 ?
O4 Dy1 O6 121.6(3) . 2_655 ?
O4 Dy1 O6 73.1(3) 2_655 2_655 ?
O7 Dy1 O6 134.7(4) . 2_655 ?
O7 Dy1 O6 44.2(4) 2_655 2_655 ?
O1 Dy1 O6 98.0(3) 2_655 . ?
O1 Dy1 O6 69.7(3) . . ?
O2 Dy1 O6 115.8(3) 2_655 . ?
O2 Dy1 O6 67.6(3) . . ?
O4 Dy1 O6 73.1(3) . . ?
O4 Dy1 O6 121.6(3) 2_655 . ?
O7 Dy1 O6 44.2(4) . . ?
O7 Dy1 O6 134.7(4) 2_655 . ?
O6 Dy1 O6 165.2(5) 2_655 . ?
O1 Dy1 N4 143.69(14) 2_655 . ?
O1 Dy1 N4 143.69(14) . . ?
O2 Dy1 N4 77.84(14) 2_655 . ?
O2 Dy1 N4 77.84(14) . . ?
O4 Dy1 N4 24.7(2) . . ?
O4 Dy1 N4 24.7(2) 2_655 . ?
O7 Dy1 N4 93.0(3) . . ?
O7 Dy1 N4 93.0(3) 2_655 . ?
O6 Dy1 N4 97.4(3) 2_655 . ?
O6 Dy1 N4 97.4(3) . . ?
C7 N1 C9 117.7(9) . . ?
C7 N1 Cu1 122.9(7) . . ?
C9 N1 Cu1 119.1(7) . . ?
C12 N2 C11 118.2(8) . . ?
C12 N2 Cu1 122.5(6) . . ?
C11 N2 Cu1 119.3(7) . . ?
O4 N4 O4 119.6(15) 2_655 . ?
O4 N4 O3 120.2(8) 2_655 . ?
O4 N4 O3 120.2(8) . . ?
O4 N4 Dy1 59.8(8) 2_655 . ?
O4 N4 Dy1 59.8(8) . . ?
O3 N4 Dy1 180.0 . . ?
O5 N5 O6 124.6(15) . . ?
O5 N5 O7 121.8(15) . . ?
O6 N5 O7 113.6(13) . . ?
C1 O1 Cu1 117.4(5) . . ?
C1 O1 Dy1 141.3(5) . . ?
Cu1 O1 Dy1 100.3(2) . . ?
C18 O2 Cu1 122.3(5) . . ?
C18 O2 Dy1 139.2(5) . . ?
Cu1 O2 Dy1 98.4(2) . . ?
N4 O4 Dy1 95.6(8) . . ?
N5 O6 Dy1 99.8(10) . . ?
N5 O7 Dy1 102.3(10) . . ?
O1 C1 C2 118.8(8) . . ?
O1 C1 C6 122.5(9) . . ?
C2 C1 C6 118.6(9) . . ?
C1 C2 C3 121.2(11) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
C4 C3 C2 121.1(13) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 117.9(12) . . ?
C3 C4 H4 121.0 . . ?
C5 C4 H4 121.0 . . ?
C6 C5 C4 123.6(12) . . ?
C6 C5 H5 118.2 . . ?
C4 C5 H5 118.2 . . ?
C5 C6 C1 117.1(11) . . ?
C5 C6 C7 119.4(10) . . ?
C1 C6 C7 123.4(9) . . ?
N1 C7 C6 121.6(9) . . ?
N1 C7 C8 121.6(11) . . ?
C6 C7 C8 116.8(11) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C10 113.8(10) . . ?
N1 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N1 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C11 C10 C9 114.2(14) . . ?
C11 C10 H10A 108.7 . . ?
C9 C10 H10A 108.7 . . ?
C11 C10 H10B 108.7 . . ?
C9 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
C10 C11 N2 110.5(11) . . ?
C10 C11 H11A 109.6 . . ?
N2 C11 H11A 109.6 . . ?
C10 C11 H11B 109.6 . . ?
N2 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
N2 C12 C13 126.6(8) . . ?
N2 C12 H12 116.7 . . ?
C13 C12 H12 116.7 . . ?
C18 C13 C12 124.6(8) . . ?
C18 C13 C14 118.8(8) . . ?
C12 C13 C14 116.6(8) . . ?
C15 C14 C13 122.2(9) . . ?
C15 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?
C14 C15 C16 118.0(9) . . ?
C14 C15 H15 121.0 . . ?
C16 C15 H15 121.0 . . ?
C15 C16 C17 123.2(9) . . ?
C15 C16 H16 118.4 . . ?
C17 C16 H16 118.4 . . ?
C16 C17 C18 119.8(8) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
O2 C18 C17 120.4(7) . . ?
O2 C18 C13 121.8(7) . . ?
C17 C18 C13 117.8(7) . . ?
C19 N3 Cu1 136.2(11) . . ?
N3 C19 C20B 131(5) . . ?
N3 C19 C20A 173(2) . . ?
C20B C19 C20A 56(4) . . ?
C19 C20A H20A 109.5 . . ?
C19 C20A H20B 109.5 . . ?
H20A C20A H20B 109.5 . . ?
C19 C20A H20C 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
C19 C20B H20D 109.5 . . ?
C19 C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
C19 C20B H20F 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?

_refine_diff_density_max         1.532
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.151

####################################################################### 
# 
# 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 1554033'
_audit_update_record             
;
2017-07-31 deposited with the CCDC.
2017-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H42 Cu2 N9 O13 Tb'
_chemical_formula_weight         1142.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   17.351(17)
_cell_length_b                   17.351(17)
_cell_length_c                   30.46(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9170(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    21103
_cell_measurement_theta_min      1.351
_cell_measurement_theta_max      25.107

_exptl_crystal_description       prismatic
_exptl_crystal_colour            green
_exptl_crystal_density_measured  ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_F_000             4576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.516
_shelx_estimated_absorpt_T_min   0.704
_shelx_estimated_absorpt_T_max   0.787
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(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_reflns_number            21103
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.351
_diffrn_reflns_theta_max         25.107
_diffrn_reflns_theta_full        25.107
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4091
_reflns_number_gt                2843
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL-2016/6, PLATON, WINGX (Ferrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0697P)²+9.0413P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4091
_refine_ls_number_parameters     297
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1335
_refine_ls_wR_factor_gt          0.1175
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.51709(4) 0.07148(4) 0.63008(2) 0.0516(2) Uani 1 1 d . . . . .
Tb1 Tb 0.500000 0.250000 0.59202(2) 0.05520(18) Uani 1 2 d S T P . .
N1 N 0.4691(3) 0.0381(3) 0.68664(19) 0.0669(15) Uani 1 1 d . . . . .
N2 N 0.5015(3) -0.0257(3) 0.59801(18) 0.0584(13) Uani 1 1 d . . . . .
N3 N 0.6534(6) 0.0466(5) 0.6440(3) 0.112(3) Uani 1 1 d . . . . .
N4 N 0.500000 0.250000 0.4954(3) 0.093(3) Uani 1 2 d S T P . .
N5 N 0.3380(5) 0.1729(4) 0.6033(2) 0.0847(19) Uani 1 1 d . . . . .
O1 O 0.5305(2) 0.1752(2) 0.65405(12) 0.0521(10) Uani 1 1 d . . . . .
O2 O 0.5510(2) 0.1249(2) 0.57637(13) 0.0524(10) Uani 1 1 d . . . . .
O3 O 0.500000 0.250000 0.4560(3) 0.136(4) Uani 1 2 d S T P . .
O4 O 0.4515(4) 0.2135(3) 0.51755(17) 0.0896(17) Uani 1 1 d . . . . .
O5 O 0.2765(4) 0.1473(4) 0.6093(3) 0.134(3) Uani 1 1 d . . . . .
O6 O 0.3946(4) 0.1382(5) 0.6026(2) 0.143(3) Uani 1 1 d . . . . .
O7 O 0.3475(4) 0.2461(4) 0.5963(2) 0.126(2) Uani 1 1 d . . . . .
C1 C 0.5617(3) 0.1823(4) 0.6934(2) 0.0555(15) Uani 1 1 d . . . . .
C2 C 0.6120(4) 0.2421(4) 0.7021(2) 0.0714(19) Uani 1 1 d . . . . .
H2 H 0.621186 0.278476 0.680270 0.086 Uiso 1 1 calc R U . . .
C3 C 0.6489(5) 0.2500(6) 0.7415(3) 0.099(3) Uani 1 1 d . . . . .
H3 H 0.683756 0.290003 0.745917 0.119 Uiso 1 1 calc R U . . .
C4 C 0.6343(7) 0.1985(7) 0.7745(3) 0.124(4) Uani 1 1 d . . . . .
H4 H 0.659627 0.202857 0.801246 0.149 Uiso 1 1 calc R U . . .
C5 C 0.5821(6) 0.1406(6) 0.7678(3) 0.108(3) Uani 1 1 d . . . . .
H5 H 0.572022 0.106699 0.790712 0.129 Uiso 1 1 calc R U . . .
C6 C 0.5429(4) 0.1300(5) 0.7277(2) 0.077(2) Uani 1 1 d . . . . .
C7 C 0.4847(4) 0.0704(4) 0.7232(3) 0.074(2) Uani 1 1 d . . . . .
C8 C 0.4423(6) 0.0494(6) 0.7652(3) 0.128(4) Uani 1 1 d . . . . .
H8A H 0.388943 0.063157 0.762499 0.193 Uiso 1 1 calc R U . . .
H8B H 0.464676 0.076837 0.789463 0.193 Uiso 1 1 calc R U . . .
H8C H 0.446587 -0.005051 0.770310 0.193 Uiso 1 1 calc R U . . .
C9 C 0.4079(5) -0.0219(5) 0.6862(3) 0.102(3) Uani 1 1 d . . . . .
H9A H 0.361377 -0.000685 0.699074 0.122 Uiso 1 1 calc R U . . .
H9B H 0.424220 -0.064917 0.704288 0.122 Uiso 1 1 calc R U . . .
C10 C 0.3900(6) -0.0508(7) 0.6411(4) 0.135(4) Uani 1 1 d . . . . .
H10A H 0.348598 -0.088166 0.643295 0.162 Uiso 1 1 calc R U . . .
H10B H 0.370849 -0.007867 0.623767 0.162 Uiso 1 1 calc R U . . .
C11 C 0.4526(5) -0.0856(4) 0.6177(3) 0.088(2) Uani 1 1 d . . . . .
H11A H 0.432566 -0.119005 0.594849 0.106 Uiso 1 1 calc R U . . .
H11B H 0.482996 -0.116799 0.637672 0.106 Uiso 1 1 calc R U . . .
C12 C 0.5298(4) -0.0389(3) 0.5609(2) 0.0582(16) Uani 1 1 d . . . . .
H12 H 0.516828 -0.085822 0.548141 0.070 Uiso 1 1 calc R U . . .
C13 C 0.5798(3) 0.0099(3) 0.53578(19) 0.0498(14) Uani 1 1 d . . . . .
C14 C 0.6194(4) -0.0231(3) 0.5002(2) 0.0572(16) Uani 1 1 d . . . . .
H14 H 0.610641 -0.074604 0.493464 0.069 Uiso 1 1 calc R U . . .
C15 C 0.6695(4) 0.0172(4) 0.4757(2) 0.0702(18) Uani 1 1 d . . . . .
H15 H 0.695426 -0.006139 0.452528 0.084 Uiso 1 1 calc R U . . .
C16 C 0.6818(4) 0.0945(4) 0.4855(2) 0.0717(19) Uani 1 1 d . . . . .
H16 H 0.717570 0.122621 0.469406 0.086 Uiso 1 1 calc R U . . .
C17 C 0.6418(4) 0.1295(4) 0.5187(2) 0.0613(17) Uani 1 1 d . . . . .
H17 H 0.649605 0.181712 0.523905 0.074 Uiso 1 1 calc R U . . .
C18 C 0.5895(3) 0.0891(3) 0.54484(18) 0.0450(13) Uani 1 1 d . . . . .
C19 C 0.7075(7) 0.0780(6) 0.6402(4) 0.109(3) Uani 1 1 d . . . . .
C20A C 0.7796(10) 0.1258(11) 0.6409(8) 0.129(5) Uiso 0.67(2) 1 d . U P . .
H20A H 0.771957 0.171311 0.623529 0.194 Uiso 0.67(2) 1 calc R U P . .
H20B H 0.821502 0.096362 0.628966 0.194 Uiso 0.67(2) 1 calc R U P . .
H20C H 0.791302 0.140157 0.670565 0.194 Uiso 0.67(2) 1 calc R U P . .
C20B C 0.773(2) 0.105(2) 0.6114(15) 0.129(5) Uiso 0.33(2) 1 d . U P . .
H20D H 0.796050 0.061420 0.596849 0.194 Uiso 0.33(2) 1 calc R U P . .
H20E H 0.811663 0.129857 0.629253 0.194 Uiso 0.33(2) 1 calc R U P . .
H20F H 0.754347 0.140649 0.589946 0.194 Uiso 0.33(2) 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.956(4) . ?
Cu1 N2 1.967(5) . ?
Cu1 O2 1.970(4) . ?
Cu1 N1 2.000(5) . ?
Cu1 N3 2.442(10) . ?
Cu1 Tb1 3.321(3) . ?
Tb1 O1 2.353(4) . ?
Tb1 O1 2.353(4) 7_554 ?
Tb1 O2 2.392(4) 7_554 ?
Tb1 O2 2.392(4) . ?
Tb1 O4 2.501(5) 7_554 ?
Tb1 O4 2.501(5) . ?
Tb1 O7 2.650(8) 7_554 ?
Tb1 O7 2.650(8) . ?
Tb1 O6 2.685(9) . ?
Tb1 O6 2.685(9) 7_554 ?
N1 C7 1.275(9) . ?
N1 C9 1.486(9) . ?
N2 C12 1.254(8) . ?
N2 C11 1.470(8) . ?
N3 C19 1.091(12) . ?
N4 O3 1.199(11) . ?
N4 O4 1.250(7) . ?
N4 O4 1.250(7) 7_554 ?
N5 O6 1.152(9) . ?
N5 O5 1.170(8) . ?
N5 O7 1.300(8) . ?
O1 C1 1.321(7) . ?
O2 C18 1.325(6) . ?
C1 C2 1.382(10) . ?
C1 C6 1.421(9) . ?
C2 C3 1.368(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.366(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.368(14) . ?
C4 H4 0.9300 . ?
C5 C6 1.410(11) . ?
C5 H5 0.9300 . ?
C6 C7 1.452(11) . ?
C7 C8 1.521(10) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.496(14) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.433(13) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.433(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.405(8) . ?
C13 C18 1.412(8) . ?
C14 C15 1.342(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.390(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.367(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.396(8) . ?
C17 H17 0.9300 . ?
C19 C20A 1.50(2) . ?
C19 C20B 1.52(4) . ?
C20A H20A 0.9600 . ?
C20A H20B 0.9600 . ?
C20A H20C 0.9600 . ?
C20B H20D 0.9600 . ?
C20B H20E 0.9600 . ?
C20B H20F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag

O1 Cu1 N2 172.01(19) . . ?
O1 Cu1 O2 80.89(16) . . ?
N2 Cu1 O2 91.83(19) . . ?
O1 Cu1 N1 89.7(2) . . ?
N2 Cu1 N1 97.0(2) . . ?
O2 Cu1 N1 167.48(19) . . ?
O1 Cu1 N3 89.0(2) . . ?
N2 Cu1 N3 93.9(3) . . ?
O2 Cu1 N3 86.5(2) . . ?
N1 Cu1 N3 101.7(3) . . ?
O1 Tb1 O1 73.2(2) . 7_554 ?
O1 Tb1 O2 138.08(13) . 7_554 ?
O1 Tb1 O2 64.91(14) 7_554 7_554 ?
O1 Tb1 O2 64.91(14) . . ?
O1 Tb1 O2 138.09(13) 7_554 . ?
O2 Tb1 O2 157.01(19) 7_554 . ?
O1 Tb1 O4 142.40(16) . 7_554 ?
O1 Tb1 O4 131.64(15) 7_554 7_554 ?
O2 Tb1 O4 73.38(15) 7_554 7_554 ?
O2 Tb1 O4 85.67(14) . 7_554 ?
O1 Tb1 O4 131.64(15) . . ?
O1 Tb1 O4 142.39(16) 7_554 . ?
O2 Tb1 O4 85.67(14) 7_554 . ?
O2 Tb1 O4 73.37(15) . . ?
O4 Tb1 O4 49.8(3) 7_554 . ?
O1 Tb1 O7 75.51(17) . 7_554 ?
O1 Tb1 O7 99.88(18) 7_554 7_554 ?
O2 Tb1 O7 110.84(18) 7_554 7_554 ?
O2 Tb1 O7 70.35(18) . 7_554 ?
O4 Tb1 O7 72.7(2) 7_554 7_554 ?
O4 Tb1 O7 112.7(2) . 7_554 ?
O1 Tb1 O7 99.88(18) . . ?
O1 Tb1 O7 75.51(17) 7_554 . ?
O2 Tb1 O7 70.35(18) 7_554 . ?
O2 Tb1 O7 110.85(18) . . ?
O4 Tb1 O7 112.7(2) 7_554 . ?
O4 Tb1 O7 72.7(2) . . ?
O7 Tb1 O7 174.4(3) 7_554 . ?
O1 Tb1 O6 70.04(19) . . ?
O1 Tb1 O6 98.59(19) 7_554 . ?
O2 Tb1 O6 115.3(2) 7_554 . ?
O2 Tb1 O6 67.66(19) . . ?
O4 Tb1 O6 121.4(2) 7_554 . ?
O4 Tb1 O6 72.3(2) . . ?
O7 Tb1 O6 133.8(2) 7_554 . ?
O7 Tb1 O6 45.2(2) . . ?
O1 Tb1 O6 98.59(19) . 7_554 ?
O1 Tb1 O6 70.04(19) 7_554 7_554 ?
O2 Tb1 O6 67.66(19) 7_554 7_554 ?
O2 Tb1 O6 115.3(2) . 7_554 ?
O4 Tb1 O6 72.3(2) 7_554 7_554 ?
O4 Tb1 O6 121.4(2) . 7_554 ?
O7 Tb1 O6 45.2(2) 7_554 7_554 ?
O7 Tb1 O6 133.8(2) . 7_554 ?
O6 Tb1 O6 166.3(3) . 7_554 ?
C7 N1 C9 117.8(6) . . ?
C7 N1 Cu1 122.4(5) . . ?
C9 N1 Cu1 119.5(5) . . ?
C12 N2 C11 117.7(6) . . ?
C12 N2 Cu1 123.4(4) . . ?
C11 N2 Cu1 118.9(5) . . ?
C19 N3 Cu1 136.6(9) . . ?
O3 N4 O4 122.6(4) . . ?
O3 N4 O4 122.7(4) . 7_554 ?
O4 N4 O4 114.7(9) . 7_554 ?
O3 N4 Tb1 180.0 . . ?
O4 N4 Tb1 57.4(4) . . ?
O4 N4 Tb1 57.3(4) 7_554 . ?
O6 N5 O5 125.7(9) . . ?
O6 N5 O7 113.5(8) . . ?
O5 N5 O7 120.8(9) . . ?
C1 O1 Cu1 118.3(4) . . ?
C1 O1 Tb1 140.3(4) . . ?
Cu1 O1 Tb1 100.42(17) . . ?
C18 O2 Cu1 122.2(3) . . ?
C18 O2 Tb1 139.1(3) . . ?
Cu1 O2 Tb1 98.69(16) . . ?
N4 O4 Tb1 97.8(5) . . ?
N5 O6 Tb1 101.9(7) . . ?
N5 O7 Tb1 99.2(6) . . ?
O1 C1 C2 120.2(6) . . ?
O1 C1 C6 120.8(6) . . ?
C2 C1 C6 119.0(6) . . ?
C3 C2 C1 122.6(8) . . ?
C3 C2 H2 118.7 . . ?
C1 C2 H2 118.7 . . ?
C4 C3 C2 119.5(9) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 119.6(9) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 123.0(9) . . ?
C4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
C5 C6 C1 116.2(8) . . ?
C5 C6 C7 120.7(8) . . ?
C1 C6 C7 123.1(7) . . ?
N1 C7 C6 122.9(6) . . ?
N1 C7 C8 121.8(8) . . ?
C6 C7 C8 115.3(8) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C10 113.0(7) . . ?
N1 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
N1 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C11 C10 C9 116.1(10) . . ?
C11 C10 H10A 108.3 . . ?
C9 C10 H10A 108.3 . . ?
C11 C10 H10B 108.3 . . ?
C9 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C10 C11 N2 110.0(7) . . ?
C10 C11 H11A 109.7 . . ?
N2 C11 H11A 109.7 . . ?
C10 C11 H11B 109.7 . . ?
N2 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
N2 C12 C13 127.6(6) . . ?
N2 C12 H12 116.2 . . ?
C13 C12 H12 116.2 . . ?
C14 C13 C18 119.3(5) . . ?
C14 C13 C12 117.8(6) . . ?
C18 C13 C12 122.9(6) . . ?
C15 C14 C13 122.3(6) . . ?
C15 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?
C14 C15 C16 118.8(6) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C17 C16 C15 120.6(6) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 121.9(6) . . ?
C16 C17 H17 119.0 . . ?
C18 C17 H17 119.0 . . ?
O2 C18 C17 120.5(5) . . ?
O2 C18 C13 122.5(5) . . ?
C17 C18 C13 117.0(5) . . ?
N3 C19 C20A 172.4(16) . . ?
N3 C19 C20B 150(2) . . ?
C19 C20A H20A 109.5 . . ?
C19 C20A H20B 109.5 . . ?
H20A C20A H20B 109.5 . . ?
C19 C20A H20C 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
C19 C20B H20D 109.5 . . ?
C19 C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
C19 C20B H20F 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?

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
O3 N4 O4 Tb1 180.0 . . . . ?
O4 N4 O4 Tb1 0.001(0) 7_554 . . . ?
O5 N5 O6 Tb1 -176.6(8) . . . . ?
O7 N5 O6 Tb1 4.1(8) . . . . ?
O6 N5 O7 Tb1 -4.2(8) . . . . ?
O5 N5 O7 Tb1 176.5(7) . . . . ?
Cu1 O1 C1 C2 141.9(5) . . . . ?
Tb1 O1 C1 C2 -24.0(9) . . . . ?
Cu1 O1 C1 C6 -39.3(7) . . . . ?
Tb1 O1 C1 C6 154.7(5) . . . . ?
O1 C1 C2 C3 -176.5(6) . . . . ?
C6 C1 C2 C3 4.7(10) . . . . ?
C1 C2 C3 C4 -2.1(13) . . . . ?
C2 C3 C4 C5 -1.0(15) . . . . ?
C3 C4 C5 C6 1.3(17) . . . . ?
C4 C5 C6 C1 1.3(14) . . . . ?
C4 C5 C6 C7 -176.3(9) . . . . ?
O1 C1 C6 C5 177.0(6) . . . . ?
C2 C1 C6 C5 -4.2(10) . . . . ?
O1 C1 C6 C7 -5.4(10) . . . . ?
C2 C1 C6 C7 173.4(6) . . . . ?
C9 N1 C7 C6 -179.6(7) . . . . ?
Cu1 N1 C7 C6 -4.9(10) . . . . ?
C9 N1 C7 C8 -0.4(11) . . . . ?
Cu1 N1 C7 C8 174.2(6) . . . . ?
C5 C6 C7 N1 -152.2(8) . . . . ?
C1 C6 C7 N1 30.3(11) . . . . ?
C5 C6 C7 C8 28.6(11) . . . . ?
C1 C6 C7 C8 -148.9(7) . . . . ?
C7 N1 C9 C10 175.1(8) . . . . ?
Cu1 N1 C9 C10 0.2(11) . . . . ?
N1 C9 C10 C11 60.0(12) . . . . ?
C9 C10 C11 N2 -81.0(11) . . . . ?
C12 N2 C11 C10 -142.8(8) . . . . ?
Cu1 N2 C11 C10 35.6(10) . . . . ?
C11 N2 C12 C13 -178.9(7) . . . . ?
Cu1 N2 C12 C13 2.8(9) . . . . ?
N2 C12 C13 C14 164.9(6) . . . . ?
N2 C12 C13 C18 -16.2(10) . . . . ?
C18 C13 C14 C15 3.4(9) . . . . ?
C12 C13 C14 C15 -177.7(6) . . . . ?
C13 C14 C15 C16 -0.8(10) . . . . ?
C14 C15 C16 C17 -2.1(11) . . . . ?
C15 C16 C17 C18 2.4(11) . . . . ?
Cu1 O2 C18 C17 -150.4(5) . . . . ?
Tb1 O2 C18 C17 30.7(9) . . . . ?
Cu1 O2 C18 C13 30.2(7) . . . . ?
Tb1 O2 C18 C13 -148.7(4) . . . . ?
C16 C17 C18 O2 -179.2(6) . . . . ?
C16 C17 C18 C13 0.3(10) . . . . ?
C14 C13 C18 O2 176.4(5) . . . . ?
C12 C13 C18 O2 -2.4(9) . . . . ?
C14 C13 C18 C17 -3.0(8) . . . . ?
C12 C13 C18 C17 178.1(6) . . . . ?
Cu1 N3 C19 C20B -81(4) . . . . ?

_refine_diff_density_max         1.010
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.096

####################################################################### 
# 
# 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 1554032'
_audit_update_record             
;
2017-07-31 deposited with the CCDC.
2017-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H42 Cu2 Gd N9 O13'
_chemical_formula_weight         1141.15

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   17.341(3)
_cell_length_b                   17.341(3)
_cell_length_c                   30.703(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9233(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    21426
_cell_measurement_theta_min      1.349
_cell_measurement_theta_max      25.510

_exptl_crystal_description       prismatic
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_F_000             4568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    2.404
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(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_reflns_number            21426
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_av_R_equivalents  0.0915
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.349
_diffrn_reflns_theta_max         25.510
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4241
_reflns_number_gt                2651
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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



_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1532P)²+22.4622P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4241
_refine_ls_number_parameters     297
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.2331
_refine_ls_wR_factor_gt          0.1931
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_restrained_S_all      0.975
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.51685(6) 0.07054(6) 0.62909(3) 0.0530(4) Uani 1 1 d . . . . .
Gd1 Gd 0.500000 0.250000 0.59122(2) 0.0613(3) Uani 1 2 d S T P . .
N1 N 0.4692(5) 0.0368(4) 0.6857(3) 0.069(2) Uani 1 1 d . . . . .
N2 N 0.4995(5) -0.0261(4) 0.5966(3) 0.061(2) Uani 1 1 d . . . . .
N3 N 0.6484(8) 0.0467(7) 0.6425(4) 0.100(3) Uani 1 1 d . . . . .
N4 N 0.500000 0.250000 0.4949(5) 0.112(7) Uani 1 2 d S T P . .
N5 N 0.3365(8) 0.1740(8) 0.6028(4) 0.104(3) Uani 1 1 d . U . . .
O1 O 0.5294(3) 0.1742(3) 0.65321(17) 0.0525(14) Uani 1 1 d . . . . .
O2 O 0.5500(3) 0.1235(3) 0.5753(2) 0.0553(15) Uani 1 1 d . . . . .
O3 O 0.500000 0.250000 0.4551(5) 0.118(4) Uani 1 2 d S TU P . .
O4 O 0.4516(6) 0.2144(4) 0.5164(3) 0.103(3) Uani 1 1 d . . . . .
O5 O 0.2753(6) 0.1480(6) 0.6083(4) 0.133(4) Uani 1 1 d . . . . .
O6 O 0.3913(8) 0.1379(7) 0.6026(4) 0.139(4) Uani 1 1 d . U . . .
O7 O 0.3465(6) 0.2480(6) 0.5961(3) 0.124(3) Uani 1 1 d . U . . .
C1 C 0.5615(5) 0.1819(5) 0.6926(3) 0.060(2) Uani 1 1 d . . . . .
C2 C 0.6136(6) 0.2406(6) 0.7014(4) 0.072(3) Uani 1 1 d . . . . .
H2 H 0.623954 0.276160 0.679496 0.086 Uiso 1 1 calc R U . . .
C3 C 0.6496(6) 0.2490(8) 0.7392(5) 0.093(4) Uani 1 1 d . . . . .
H3 H 0.683447 0.289738 0.743970 0.112 Uiso 1 1 calc R U . . .
C4 C 0.6350(9) 0.1944(10) 0.7716(5) 0.123(5) Uani 1 1 d . . . . .
H4 H 0.662235 0.196711 0.797691 0.147 Uiso 1 1 calc R U . . .
C5 C 0.5829(9) 0.1395(9) 0.7658(4) 0.106(4) Uani 1 1 d . . . . .
H5 H 0.572053 0.106678 0.789027 0.127 Uiso 1 1 calc R U . . .
C6 C 0.5427(7) 0.1280(7) 0.7261(3) 0.078(3) Uani 1 1 d . . . . .
C7 C 0.4860(6) 0.0693(6) 0.7218(4) 0.072(3) Uani 1 1 d . . . . .
C8 C 0.4415(9) 0.0468(9) 0.7633(4) 0.124(5) Uani 1 1 d . . . . .
H8A H 0.387264 0.053602 0.758455 0.186 Uiso 1 1 calc R U . . .
H8B H 0.457808 0.078888 0.787013 0.186 Uiso 1 1 calc R U . . .
H8C H 0.451764 -0.006242 0.770177 0.186 Uiso 1 1 calc R U . . .
C9 C 0.4098(7) -0.0240(8) 0.6856(4) 0.098(4) Uani 1 1 d . . . . .
H9A H 0.364113 -0.004769 0.700293 0.118 Uiso 1 1 calc R U . . .
H9B H 0.428677 -0.067883 0.702059 0.118 Uiso 1 1 calc R U . . .
C10 C 0.3866(10) -0.0518(10) 0.6384(6) 0.128(5) Uani 1 1 d . U . . .
H10A H 0.345206 -0.089206 0.640503 0.153 Uiso 1 1 calc R U . . .
H10B H 0.368005 -0.008174 0.621707 0.153 Uiso 1 1 calc R U . . .
C11 C 0.4503(7) -0.0855(6) 0.6167(4) 0.081(3) Uani 1 1 d . . . . .
H11A H 0.431733 -0.120478 0.594422 0.097 Uiso 1 1 calc R U . . .
H11B H 0.480497 -0.115130 0.637387 0.097 Uiso 1 1 calc R U . . .
C12 C 0.5304(5) -0.0380(5) 0.5588(3) 0.059(2) Uani 1 1 d . . . . .
H12 H 0.518402 -0.084792 0.545666 0.071 Uiso 1 1 calc R U . . .
C13 C 0.5799(5) 0.0105(4) 0.5353(3) 0.0493(19) Uani 1 1 d . . . . .
C14 C 0.6190(5) -0.0241(5) 0.5001(3) 0.059(2) Uani 1 1 d . . . . .
H14 H 0.609678 -0.075558 0.493330 0.071 Uiso 1 1 calc R U . . .
C15 C 0.6705(6) 0.0176(6) 0.4758(3) 0.071(3) Uani 1 1 d . . . . .
H15 H 0.698025 -0.005641 0.453290 0.086 Uiso 1 1 calc R U . . .
C16 C 0.6809(6) 0.0955(6) 0.4854(3) 0.074(3) Uani 1 1 d . . . . .
H16 H 0.715426 0.124496 0.469002 0.088 Uiso 1 1 calc R U . . .
C17 C 0.6412(6) 0.1298(5) 0.5186(3) 0.061(2) Uani 1 1 d . . . . .
H17 H 0.649440 0.181747 0.524442 0.074 Uiso 1 1 calc R U . . .
C18 C 0.5882(5) 0.0882(4) 0.5442(3) 0.0470(19) Uani 1 1 d . . . . .
C19 C 0.7026(10) 0.0758(10) 0.6403(5) 0.107(5) Uani 1 1 d . . . . .
C20 C 0.7807(12) 0.1167(13) 0.6331(7) 0.183(9) Uani 1 1 d . U . . .
H20A H 0.772110 0.165667 0.619374 0.274 Uiso 1 1 calc R U . . .
H20B H 0.812834 0.085364 0.614811 0.274 Uiso 1 1 calc R U . . .
H20C H 0.805629 0.124424 0.660677 0.274 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.956(6) . ?
Cu1 N2 1.973(8) . ?
Cu1 O2 1.975(6) . ?
Cu1 N1 2.013(8) . ?
Cu1 N3 2.354(14) . ?
Cu1 Gd1 3.3351(12) . ?
Gd1 O1 2.369(5) 2_655 ?
Gd1 O1 2.369(5) . ?
Gd1 O2 2.408(5) 2_655 ?
Gd1 O2 2.408(5) . ?
Gd1 O4 2.521(7) . ?
Gd1 O4 2.521(7) 2_655 ?
Gd1 O7 2.666(11) 2_655 ?
Gd1 O7 2.666(11) . ?
Gd1 O6 2.730(12) 2_655 ?
Gd1 O6 2.730(12) . ?
N1 C7 1.277(13) . ?
N1 C9 1.474(14) . ?
N2 C12 1.293(12) . ?
N2 C11 1.474(12) . ?
N3 C19 1.070(17) . ?
N4 O4 1.234(11) 2_655 ?
N4 O4 1.234(11) . ?
N4 O3 1.221(18) . ?
N5 O6 1.137(14) . ?
N5 O5 1.166(14) . ?
N5 O7 1.311(14) . ?
O1 C1 1.339(10) . ?
O2 C18 1.315(9) . ?
C1 C2 1.388(14) . ?
C1 C6 1.427(14) . ?
C2 C3 1.326(15) . ?
C3 C4 1.396(19) . ?
C4 C5 1.33(2) . ?
C5 C6 1.420(17) . ?
C6 C7 1.421(16) . ?
C7 C8 1.538(14) . ?
C9 C10 1.58(2) . ?
C10 C11 1.415(19) . ?
C12 C13 1.403(12) . ?
C13 C18 1.381(11) . ?
C13 C14 1.409(12) . ?
C14 C15 1.371(13) . ?
C15 C16 1.395(13) . ?
C16 C17 1.366(13) . ?
C17 C18 1.409(12) . ?
C19 C20 1.54(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag


O1 Cu1 N2 171.3(3) . . ?
O1 Cu1 O2 81.7(2) . . ?
N2 Cu1 O2 90.9(3) . . ?
O1 Cu1 N1 89.2(3) . . ?
N2 Cu1 N1 97.3(3) . . ?
O2 Cu1 N1 167.7(3) . . ?
O1 Cu1 N3 89.3(3) . . ?
N2 Cu1 N3 95.0(4) . . ?
O2 Cu1 N3 86.9(3) . . ?
N1 Cu1 N3 101.3(4) . . ?
O1 Cu1 Gd1 44.30(16) . . ?
N2 Cu1 Gd1 127.0(2) . . ?
O2 Cu1 Gd1 45.55(15) . . ?
N1 Cu1 Gd1 122.5(2) . . ?
N3 Cu1 Gd1 108.0(3) . . ?
O1 Gd1 O1 73.1(3) 2_655 . ?
O1 Gd1 O2 65.2(2) 2_655 2_655 ?
O1 Gd1 O2 138.2(2) . 2_655 ?
O1 Gd1 O2 138.2(2) 2_655 . ?
O1 Gd1 O2 65.2(2) . . ?
O2 Gd1 O2 156.6(3) 2_655 . ?
O1 Gd1 O4 142.8(2) 2_655 . ?
O1 Gd1 O4 131.9(2) . . ?
O2 Gd1 O4 85.4(2) 2_655 . ?
O2 Gd1 O4 73.3(2) . . ?
O1 Gd1 O4 131.9(2) 2_655 2_655 ?
O1 Gd1 O4 142.8(2) . 2_655 ?
O2 Gd1 O4 73.3(2) 2_655 2_655 ?
O2 Gd1 O4 85.4(2) . 2_655 ?
O4 Gd1 O4 48.8(5) . 2_655 ?
O1 Gd1 O7 99.3(3) 2_655 2_655 ?
O1 Gd1 O7 75.3(3) . 2_655 ?
O2 Gd1 O7 111.0(3) 2_655 2_655 ?
O2 Gd1 O7 70.4(3) . 2_655 ?
O4 Gd1 O7 112.8(3) . 2_655 ?
O4 Gd1 O7 73.5(3) 2_655 2_655 ?
O1 Gd1 O7 75.3(3) 2_655 . ?
O1 Gd1 O7 99.3(3) . . ?
O2 Gd1 O7 70.4(3) 2_655 . ?
O2 Gd1 O7 111.0(3) . . ?
O4 Gd1 O7 73.5(3) . . ?
O4 Gd1 O7 112.8(3) 2_655 . ?
O7 Gd1 O7 173.5(5) 2_655 . ?
O1 Gd1 O6 69.5(3) 2_655 2_655 ?
O1 Gd1 O6 98.3(3) . 2_655 ?
O2 Gd1 O6 68.1(3) 2_655 2_655 ?
O2 Gd1 O6 115.2(3) . 2_655 ?
O4 Gd1 O6 121.4(3) . 2_655 ?
O4 Gd1 O6 73.3(3) 2_655 2_655 ?
O7 Gd1 O6 45.1(4) 2_655 2_655 ?
O7 Gd1 O6 133.7(4) . 2_655 ?
O1 Gd1 O6 98.3(3) 2_655 . ?
O1 Gd1 O6 69.5(3) . . ?
O2 Gd1 O6 115.2(3) 2_655 . ?
O2 Gd1 O6 68.1(3) . . ?
O4 Gd1 O6 73.3(3) . . ?
O4 Gd1 O6 121.4(3) 2_655 . ?
O7 Gd1 O6 133.7(4) 2_655 . ?
O7 Gd1 O6 45.1(4) . . ?
O6 Gd1 O6 165.3(5) 2_655 . ?
C7 N1 C9 118.6(9) . . ?
C7 N1 Cu1 121.8(7) . . ?
C9 N1 Cu1 119.5(7) . . ?
C12 N2 C11 120.3(8) . . ?
C12 N2 Cu1 121.7(6) . . ?
C11 N2 Cu1 118.0(7) . . ?
C19 N3 Cu1 139.3(12) . . ?
O4 N4 O4 115.2(14) 2_655 . ?
O4 N4 O3 122.4(7) 2_655 . ?
O4 N4 O3 122.4(7) . . ?
O4 N4 Gd1 57.6(7) 2_655 . ?
O4 N4 Gd1 57.6(7) . . ?
O3 N4 Gd1 180.0 . . ?
O6 N5 O5 123.3(15) . . ?
O6 N5 O7 115.3(14) . . ?
O5 N5 O7 121.4(14) . . ?
C1 O1 Cu1 118.7(5) . . ?
C1 O1 Gd1 139.5(5) . . ?
Cu1 O1 Gd1 100.5(2) . . ?
C18 O2 Cu1 122.5(5) . . ?
C18 O2 Gd1 138.9(5) . . ?
Cu1 O2 Gd1 98.6(2) . . ?
N4 O4 Gd1 98.0(8) . . ?
N5 O6 Gd1 100.7(10) . . ?
N5 O7 Gd1 98.8(9) . . ?
O1 C1 C2 121.4(9) . . ?
O1 C1 C6 119.3(9) . . ?
C2 C1 C6 119.3(9) . . ?
C3 C2 C1 123.9(11) . . ?
C2 C3 C4 117.7(13) . . ?
C5 C4 C3 121.0(13) . . ?
C4 C5 C6 123.4(13) . . ?
C7 C6 C5 121.2(11) . . ?
C7 C6 C1 124.2(10) . . ?
C5 C6 C1 114.5(12) . . ?
N1 C7 C6 123.7(9) . . ?
N1 C7 C8 119.4(11) . . ?
C6 C7 C8 116.9(11) . . ?
N1 C9 C10 113.5(9) . . ?
C11 C10 C9 111.1(14) . . ?
C10 C11 N2 111.1(11) . . ?
N2 C12 C13 128.3(8) . . ?
C18 C13 C12 123.1(8) . . ?
C18 C13 C14 121.2(8) . . ?
C12 C13 C14 115.7(8) . . ?
C15 C14 C13 120.4(8) . . ?
C14 C15 C16 118.6(9) . . ?
C17 C16 C15 121.0(9) . . ?
C16 C17 C18 121.5(8) . . ?
O2 C18 C13 123.2(7) . . ?
O2 C18 C17 119.7(7) . . ?
C13 C18 C17 117.1(7) . . ?
N3 C19 C20 175(2) . . ?

_refine_diff_density_max         1.643
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.167

####################################################################### 
# 
# 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 1554036'
_audit_update_record             
;
2017-07-31 deposited with the CCDC.
2017-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H40.50 Cu2 Er N8.50 O13'
_chemical_formula_weight         1130.64

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'
Cu Cu 0.3201 1.2651 '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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

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

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

_cell_length_a                   10.212(5)
_cell_length_b                   20.369(5)
_cell_length_c                   23.068(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.324(5)
_cell_angle_gamma                90
_cell_volume                     4721(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    15287
_cell_measurement_theta_min      1.795
_cell_measurement_theta_max      25.337

_exptl_crystal_description       prismatic
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_F_000             2256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    2.722
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(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_reflns_number            15287
_diffrn_reflns_av_unetI/netI     0.1218
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.795
_diffrn_reflns_theta_max         25.337
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             7816
_reflns_number_gt                5486
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_max     0.979
_reflns_Friedel_fraction_full    0.984

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

  many of the light atoms could not be refined anisotropically to
  reasonable thermal parameters probably because of disorder. 
  Accordingly all light atoms were refined isotropically.


;

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

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0989P)²+135.1464P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7816
_refine_ls_number_parameters     277
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1385
_refine_ls_R_factor_gt           0.1022
_refine_ls_wR_factor_ref         0.2576
_refine_ls_wR_factor_gt          0.2387
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.6315(3) 0.18676(19) 0.74173(17) 0.0497(10) Uani 1 1 d . . . . .
Cu2 Cu 0.7196(4) 0.1573(2) 0.9344(2) 0.0694(14) Uani 1 1 d . . . . .
Er1 Er 0.90951(7) 0.16886(6) 0.83395(6) 0.0477(4) Uani 1 1 d . . . . .
N1 N 0.552(3) 0.2762(14) 0.7334(12) 0.057(7) Uiso 1 1 d . . . . .
N2 N 0.457(3) 0.1369(14) 0.7279(12) 0.054(7) Uiso 1 1 d . . . . .
N3 N 0.652(4) 0.1583(17) 0.6392(16) 0.086(10) Uiso 1 1 d . . . . .
N4 N 0.629(3) 0.0728(18) 0.9270(15) 0.084(10) Uiso 1 1 d . . . . .
N5 N 0.548(3) 0.2046(15) 0.9425(13) 0.063(7) Uiso 1 1 d . . . . .
N6 N 1.091(3) 0.0841(14) 0.7929(13) 0.059(7) Uiso 1 1 d . . . . .
N7 N 1.119(3) 0.2563(14) 0.8737(12) 0.053(7) Uiso 1 1 d . . . . .
N8 N 0.836(4) 0.1870(19) 1.0495(17) 0.087(10) Uiso 1 1 d . . . . .
O1 O 0.8031(19) 0.2252(9) 0.7528(8) 0.041(5) Uiso 1 1 d . . . . .
O2 O 0.7245(18) 0.1127(10) 0.7875(9) 0.045(5) Uiso 1 1 d . . . . .
O3 O 0.879(2) 0.1146(11) 0.9109(10) 0.059(6) Uiso 1 1 d . . . . .
O4 O 0.7567(18) 0.2255(9) 0.8786(8) 0.040(4) Uiso 1 1 d . . . . .
O5 O 1.164(4) 0.0451(19) 0.7660(17) 0.121(12) Uiso 1 1 d . . . . .
O6 O 1.088(3) 0.0873(14) 0.8425(13) 0.079(7) Uiso 1 1 d . . . . .
O7 O 1.008(3) 0.1148(13) 0.7540(12) 0.076(7) Uiso 1 1 d . . . . .
O8 O 1.210(3) 0.2958(13) 0.8916(12) 0.076(7) Uiso 1 1 d . . . . .
O9 O 1.074(3) 0.2245(13) 0.9067(12) 0.074(7) Uiso 1 1 d . . . . .
O10 O 1.073(3) 0.2487(13) 0.8205(12) 0.072(7) Uiso 1 1 d . . . . .
O11 O 0.892(3) 0.2017(17) 1.0998(16) 0.111(10) Uiso 1 1 d . . . . .
O12 O 0.752(5) 0.140(2) 1.0478(19) 0.145(14) Uiso 1 1 d . . . . .
O13 O 0.852(3) 0.2172(18) 1.0034(16) 0.110(11) Uiso 1 1 d . . . . .
C1 C 0.830(3) 0.2677(14) 0.7136(13) 0.043(7) Uiso 1 1 d . . . . .
C2 C 0.939(4) 0.263(2) 0.6916(17) 0.072(10) Uiso 1 1 d . . . . .
H2 H 0.998040 0.228293 0.703713 0.087 Uiso 1 1 calc R U . . .
C3 C 0.971(4) 0.309(2) 0.6489(18) 0.077(11) Uiso 1 1 d . . . . .
H3 H 1.051706 0.306992 0.635884 0.092 Uiso 1 1 calc R U . . .
C4 C 0.881(6) 0.354(3) 0.629(2) 0.113(17) Uiso 1 1 d . . . . .
H4 H 0.899909 0.382430 0.599515 0.135 Uiso 1 1 calc R U . . .
C5 C 0.766(5) 0.362(2) 0.647(2) 0.094(13) Uiso 1 1 d . . . . .
H5 H 0.707403 0.395273 0.631716 0.113 Uiso 1 1 calc R U . . .
C6 C 0.730(3) 0.3175(18) 0.6928(16) 0.069(10) Uiso 1 1 d D . . . .
C7 C 0.607(3) 0.3216(18) 0.7144(15) 0.062(9) Uiso 1 1 d D . . . .
C8 C 0.547(5) 0.396(2) 0.708(2) 0.097(14) Uiso 1 1 d . . . . .
H8A H 0.473020 0.397333 0.675581 0.145 Uiso 1 1 calc R U . . .
H8B H 0.614337 0.425869 0.700774 0.145 Uiso 1 1 calc R U . . .
H8C H 0.516730 0.407884 0.743618 0.145 Uiso 1 1 calc R U . . .
C9 C 0.431(5) 0.290(3) 0.751(3) 0.115(17) Uiso 1 1 d . . . . .
H9A H 0.448774 0.312340 0.789037 0.139 Uiso 1 1 calc R U . . .
H9B H 0.379600 0.319477 0.722909 0.139 Uiso 1 1 calc R U . . .
C10 C 0.360(8) 0.235(4) 0.756(3) 0.18(3) Uiso 1 1 d . . . . .
H10A H 0.272185 0.248615 0.761478 0.215 Uiso 1 1 calc R U . . .
H10B H 0.401408 0.212752 0.791717 0.215 Uiso 1 1 calc R U . . .
C11 C 0.343(6) 0.186(3) 0.707(2) 0.106(16) Uiso 1 1 d . . . . .
H11A H 0.351766 0.205723 0.669588 0.127 Uiso 1 1 calc R U . . .
H11B H 0.256653 0.164029 0.702402 0.127 Uiso 1 1 calc R U . . .
C12 C 0.459(4) 0.0769(18) 0.7327(16) 0.068(10) Uiso 1 1 d D . . . .
H12 H 0.379916 0.056751 0.715946 0.081 Uiso 1 1 calc R U . . .
C13 C 0.561(3) 0.0318(16) 0.7590(15) 0.058(8) Uiso 1 1 d D . . . .
C14 C 0.525(4) -0.0372(19) 0.7526(17) 0.071(10) Uiso 1 1 d . . . . .
H14 H 0.442878 -0.049367 0.730668 0.086 Uiso 1 1 calc R U . . .
C15 C 0.609(4) -0.083(2) 0.7780(19) 0.081(12) Uiso 1 1 d . . . . .
H15 H 0.581249 -0.126631 0.777104 0.097 Uiso 1 1 calc R U . . .
C16 C 0.741(3) -0.0669(18) 0.8064(15) 0.059(9) Uiso 1 1 d . . . . .
H16 H 0.801239 -0.099641 0.820795 0.071 Uiso 1 1 calc R U . . .
C17 C 0.777(4) 0.0008(19) 0.8123(16) 0.070(10) Uiso 1 1 d . . . . .
H17 H 0.859221 0.012807 0.834395 0.084 Uiso 1 1 calc R U . . .
C18 C 0.689(3) 0.0496(14) 0.7842(13) 0.042(7) Uiso 1 1 d . . . . .
C19 C 0.657(4) 0.187(2) 0.596(2) 0.080(11) Uiso 1 1 d . . . . .
C20 C 0.682(6) 0.222(3) 0.542(3) 0.14(2) Uiso 1 1 d . . . . .
H20A H 0.600356 0.226418 0.514796 0.204 Uiso 1 1 calc R U . . .
H20B H 0.744778 0.197351 0.524433 0.204 Uiso 1 1 calc R U . . .
H20C H 0.718276 0.264739 0.553064 0.204 Uiso 1 1 calc R U . . .
C21 C 0.920(3) 0.0668(12) 0.9527(11) 0.065(9) Uiso 1 1 d G . . . .
C22 C 1.053(2) 0.0657(14) 0.9798(13) 0.090(13) Uiso 1 1 d G . . . .
H22 H 1.112533 0.096469 0.969474 0.108 Uiso 1 1 calc R U . . .
C23 C 1.098(2) 0.0186(17) 1.0224(14) 0.120(19) Uiso 1 1 d G . . . .
H23 H 1.187239 0.017885 1.040524 0.144 Uiso 1 1 calc R U . . .
C24 C 1.010(3) -0.0274(15) 1.0379(13) 0.095(14) Uiso 1 1 d G . . . .
H24 H 1.039935 -0.058860 1.066343 0.114 Uiso 1 1 calc R U . . .
C25 C 0.877(3) -0.0263(14) 1.0108(14) 0.16(3) Uiso 1 1 d G . . . .
H25 H 0.817922 -0.057022 1.021110 0.188 Uiso 1 1 calc R U . . .
C26 C 0.832(2) 0.0208(14) 0.9682(13) 0.073(11) Uiso 1 1 d G . . . .
C27 C 0.694(4) 0.0184(19) 0.9391(16) 0.068(10) Uiso 1 1 d . . . . .
C28 C 0.580(7) -0.038(4) 0.935(3) 0.18(3) Uiso 1 1 d . . . . .
H28A H 0.621953 -0.080408 0.943389 0.211 Uiso 1 1 calc R U . . .
H28B H 0.523589 -0.029340 0.962967 0.211 Uiso 1 1 calc R U . . .
H28C H 0.527967 -0.038932 0.895912 0.211 Uiso 1 1 calc R U . . .
C29 C 0.487(6) 0.088(4) 0.897(3) 0.15(2) Uiso 1 1 d . . . . .
H29A H 0.490200 0.121174 0.867236 0.179 Uiso 1 1 calc R U . . .
H29B H 0.449246 0.048576 0.877073 0.179 Uiso 1 1 calc R U . . .
C30 C 0.404(8) 0.109(3) 0.934(3) 0.17(3) Uiso 1 1 d D . . . .
H30A H 0.321552 0.124495 0.909846 0.209 Uiso 1 1 calc R U . . .
H30B H 0.382072 0.072311 0.956810 0.209 Uiso 1 1 calc R U . . .
C31 C 0.458(5) 0.164(2) 0.976(2) 0.088(14) Uiso 1 1 d D . . . .
H31A H 0.509387 0.146627 1.012547 0.106 Uiso 1 1 calc R U . . .
H31B H 0.386811 0.191237 0.986008 0.106 Uiso 1 1 calc R U . . .
C32 C 0.526(4) 0.264(2) 0.9315(16) 0.069(10) Uiso 1 1 d . . . . .
H32 H 0.451695 0.282523 0.942997 0.082 Uiso 1 1 calc R U . . .
C33 C 0.611(3) 0.3060(17) 0.9009(15) 0.058(9) Uiso 1 1 d . . . . .
C34 C 0.572(3) 0.3770(17) 0.9052(15) 0.060(9) Uiso 1 1 d . . . . .
H34 H 0.503009 0.390041 0.923824 0.072 Uiso 1 1 calc R U . . .
C35 C 0.647(4) 0.4216(19) 0.8795(16) 0.065(10) Uiso 1 1 d . . . . .
H35 H 0.624302 0.465706 0.879655 0.078 Uiso 1 1 calc R U . . .
C36 C 0.760(4) 0.4034(19) 0.8525(17) 0.069(10) Uiso 1 1 d . . . . .
H36 H 0.807590 0.433437 0.834245 0.083 Uiso 1 1 calc R U . . .
C37 C 0.789(4) 0.3381(18) 0.8564(16) 0.067(9) Uiso 1 1 d . . . . .
H37 H 0.863122 0.325534 0.841067 0.080 Uiso 1 1 calc R U . . .
C38 C 0.723(3) 0.2868(15) 0.8802(13) 0.043(7) Uiso 1 1 d . . . . .
N1B N 0.501(4) -0.001(3) 0.570(2) 0.054(13) Uiso 0.5 1 d D . P . .
C2B C 0.602(4) -0.006(3) 0.605(2) 0.044(14) Uiso 0.5 1 d D . P . .
C3B C 0.743(4) -0.009(3) 0.637(2) 0.046(14) Uiso 0.5 1 d D . P . .
H3B1 H 0.789592 -0.043687 0.620888 0.069 Uiso 0.5 1 calc R U P . .
H3B2 H 0.743446 -0.018140 0.678101 0.069 Uiso 0.5 1 calc R U P . .
H3B3 H 0.785975 0.031904 0.633281 0.069 Uiso 0.5 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.89(2) . ?
Cu1 O2 1.98(2) . ?
Cu1 N1 1.99(3) . ?
Cu1 N2 2.02(3) . ?
Cu1 Er1 3.248(4) . ?
Cu2 N4 1.95(4) . ?
Cu2 O4 1.98(2) . ?
Cu2 O3 2.00(2) . ?
Cu2 N5 2.04(3) . ?
Cu2 O13 2.25(4) . ?
Cu2 Er1 3.285(5) . ?
Er1 O3 2.16(2) . ?
Er1 O1 2.296(19) . ?
Er1 O2 2.303(19) . ?
Er1 O4 2.326(19) . ?
Er1 O10 2.39(3) . ?
Er1 O9 2.43(3) . ?
Er1 O6 2.45(3) . ?
Er1 O7 2.51(3) . ?
Er1 N7 2.81(3) . ?
Er1 N6 2.82(3) . ?
N1 C7 1.20(4) . ?
N1 C9 1.40(6) . ?
N2 C12 1.23(4) . ?
N2 C11 1.55(6) . ?
N3 C19 1.16(5) . ?
N4 C27 1.30(5) . ?
N4 C29 1.52(7) . ?
N5 C32 1.24(5) . ?
N5 C31 1.54(5) . ?
N6 O6 1.15(4) . ?
N6 O7 1.28(4) . ?
N6 O5 1.32(4) . ?
N7 O9 1.16(3) . ?
N7 O8 1.24(3) . ?
N7 O10 1.24(3) . ?
N8 O11 1.24(4) . ?
N8 O13 1.26(5) . ?
N8 O12 1.27(5) . ?
O1 C1 1.32(3) . ?
O2 C18 1.33(3) . ?
O3 C21 1.38(3) . ?
O4 C38 1.30(3) . ?
C1 C2 1.31(5) . ?
C1 C6 1.46(4) . ?
C2 C3 1.44(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.32(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.34(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.48(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.43(2) . ?
C7 C8 1.63(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.35(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.51(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.44(2) . ?
C12 H12 0.9300 . ?
C13 C18 1.38(4) . ?
C13 C14 1.45(5) . ?
C14 C15 1.33(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.42(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.43(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.42(4) . ?
C17 H17 0.9300 . ?
C19 C20 1.49(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 C24 1.3900 . ?
C23 H23 0.9300 . ?
C24 C25 1.3900 . ?
C24 H24 0.9300 . ?
C25 C26 1.3900 . ?
C25 H25 0.9300 . ?
C26 C27 1.45(4) . ?
C27 C28 1.63(8) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.38(9) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.53(3) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.49(5) . ?
C32 H32 0.9300 . ?
C33 C38 1.37(4) . ?
C33 C34 1.51(5) . ?
C34 C35 1.39(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.45(5) . ?
C35 H35 0.9300 . ?
C36 C37 1.36(5) . ?
C36 H36 0.9300 . ?
C37 C38 1.41(5) . ?
C37 H37 0.9300 . ?
N1B C2B 1.19(2) . ?
C2B C3B 1.50(2) . ?
C3B H3B1 0.9600 . ?
C3B H3B2 0.9600 . ?
C3B H3B3 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O2 84.3(8) . . ?
O1 Cu1 N1 89.1(10) . . ?
O2 Cu1 N1 153.7(10) . . ?
O1 Cu1 N2 174.0(10) . . ?
O2 Cu1 N2 91.4(10) . . ?
N1 Cu1 N2 96.6(11) . . ?
O1 Cu1 Er1 43.9(6) . . ?
O2 Cu1 Er1 44.6(6) . . ?
N1 Cu1 Er1 117.3(8) . . ?
N2 Cu1 Er1 133.4(8) . . ?
N4 Cu2 O4 135.2(12) . . ?
N4 Cu2 O3 89.4(13) . . ?
O4 Cu2 O3 82.5(9) . . ?
N4 Cu2 N5 91.3(14) . . ?
O4 Cu2 N5 89.7(10) . . ?
O3 Cu2 N5 169.7(11) . . ?
N4 Cu2 O13 139.0(14) . . ?
O4 Cu2 O13 85.3(11) . . ?
O3 Cu2 O13 90.8(11) . . ?
N5 Cu2 O13 95.4(12) . . ?
N4 Cu2 Er1 109.5(11) . . ?
O4 Cu2 Er1 44.3(5) . . ?
O3 Cu2 Er1 39.6(6) . . ?
N5 Cu2 Er1 131.1(9) . . ?
O13 Cu2 Er1 96.1(9) . . ?
O3 Er1 O1 144.0(8) . . ?
O3 Er1 O2 84.4(8) . . ?
O1 Er1 O2 68.9(7) . . ?
O3 Er1 O4 71.5(8) . . ?
O1 Er1 O4 81.8(7) . . ?
O2 Er1 O4 83.9(7) . . ?
O3 Er1 O10 131.4(9) . . ?
O1 Er1 O10 78.1(8) . . ?
O2 Er1 O10 144.2(8) . . ?
O4 Er1 O10 105.0(8) . . ?
O3 Er1 O9 81.6(9) . . ?
O1 Er1 O9 119.8(7) . . ?
O2 Er1 O9 163.9(8) . . ?
O4 Er1 O9 84.2(8) . . ?
O10 Er1 O9 50.2(9) . . ?
O3 Er1 O6 78.6(9) . . ?
O1 Er1 O6 129.9(9) . . ?
O2 Er1 O6 103.8(8) . . ?
O4 Er1 O6 148.3(9) . . ?
O10 Er1 O6 86.8(9) . . ?
O9 Er1 O6 81.2(9) . . ?
O3 Er1 O7 121.0(8) . . ?
O1 Er1 O7 79.2(8) . . ?
O2 Er1 O7 80.9(8) . . ?
O4 Er1 O7 159.0(7) . . ?
O10 Er1 O7 79.8(9) . . ?
O9 Er1 O7 113.2(9) . . ?
O6 Er1 O7 51.0(9) . . ?
O3 Er1 N7 105.6(8) . . ?
O1 Er1 N7 99.9(7) . . ?
O2 Er1 N7 168.7(7) . . ?
O4 Er1 N7 94.3(7) . . ?
O10 Er1 N7 26.1(8) . . ?
O9 Er1 N7 24.1(7) . . ?
O6 Er1 N7 83.6(9) . . ?
O7 Er1 N7 97.8(8) . . ?
O3 Er1 N6 99.4(9) . . ?
O1 Er1 N6 106.0(8) . . ?
O2 Er1 N6 94.2(8) . . ?
O4 Er1 N6 170.8(8) . . ?
O10 Er1 N6 81.8(9) . . ?
O9 Er1 N6 95.9(9) . . ?
O6 Er1 N6 24.0(8) . . ?
O7 Er1 N6 27.0(8) . . ?
N7 Er1 N6 89.4(8) . . ?
O3 Er1 Cu1 111.0(6) . . ?
O1 Er1 Cu1 34.9(5) . . ?
O2 Er1 Cu1 37.2(5) . . ?
O4 Er1 Cu1 70.0(5) . . ?
O10 Er1 Cu1 112.8(6) . . ?
O9 Er1 Cu1 144.6(6) . . ?
O6 Er1 Cu1 132.8(7) . . ?
O7 Er1 Cu1 89.2(6) . . ?
N7 Er1 Cu1 131.9(6) . . ?
N6 Er1 Cu1 113.5(6) . . ?
O3 Er1 Cu2 36.3(6) . . ?
O1 Er1 Cu2 111.0(5) . . ?
O2 Er1 Cu2 75.8(5) . . ?
O4 Er1 Cu2 36.4(5) . . ?
O10 Er1 Cu2 130.9(7) . . ?
O9 Er1 Cu2 88.3(7) . . ?
O6 Er1 Cu2 114.9(7) . . ?
O7 Er1 Cu2 148.4(6) . . ?
N7 Er1 Cu2 109.1(6) . . ?
N6 Er1 Cu2 134.4(6) . . ?
Cu1 Er1 Cu2 85.00(11) . . ?
C7 N1 C9 117(4) . . ?
C7 N1 Cu1 122(2) . . ?
C9 N1 Cu1 121(3) . . ?
C12 N2 C11 132(3) . . ?
C12 N2 Cu1 119(2) . . ?
C11 N2 Cu1 109(3) . . ?
C27 N4 C29 133(4) . . ?
C27 N4 Cu2 121(3) . . ?
C29 N4 Cu2 105(3) . . ?
C32 N5 C31 121(3) . . ?
C32 N5 Cu2 125(3) . . ?
C31 N5 Cu2 113(2) . . ?
O6 N6 O7 123(3) . . ?
O6 N6 O5 128(3) . . ?
O7 N6 O5 109(3) . . ?
O6 N6 Er1 60(2) . . ?
O7 N6 Er1 62.8(17) . . ?
O5 N6 Er1 172(3) . . ?
O9 N7 O8 120(3) . . ?
O9 N7 O10 117(3) . . ?
O8 N7 O10 123(3) . . ?
O9 N7 Er1 59.3(18) . . ?
O8 N7 Er1 179(2) . . ?
O10 N7 Er1 57.6(16) . . ?
O11 N8 O13 124(4) . . ?
O11 N8 O12 114(4) . . ?
O13 N8 O12 122(4) . . ?
C1 O1 Cu1 119.0(17) . . ?
C1 O1 Er1 139.5(18) . . ?
Cu1 O1 Er1 101.2(8) . . ?
C18 O2 Cu1 127.0(17) . . ?
C18 O2 Er1 134.3(17) . . ?
Cu1 O2 Er1 98.3(8) . . ?
C21 O3 Cu2 106.2(17) . . ?
C21 O3 Er1 149.6(19) . . ?
Cu2 O3 Er1 104.1(10) . . ?
C38 O4 Cu2 125.2(18) . . ?
C38 O4 Er1 133.9(18) . . ?
Cu2 O4 Er1 99.3(8) . . ?
N6 O6 Er1 96(2) . . ?
N6 O7 Er1 90.2(19) . . ?
N7 O9 Er1 97(2) . . ?
N7 O10 Er1 96.3(19) . . ?
N8 O13 Cu2 100(3) . . ?
C2 C1 O1 121(3) . . ?
C2 C1 C6 122(3) . . ?
O1 C1 C6 117(3) . . ?
C1 C2 C3 122(4) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 H2 119.2 . . ?
C4 C3 C2 118(5) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
C3 C4 C5 124(5) . . ?
C3 C4 H4 117.9 . . ?
C5 C4 H4 117.9 . . ?
C4 C5 C6 120(5) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C1 C6 C5 114(3) . . ?
C1 C6 C7 122(3) . . ?
C5 C6 C7 123(4) . . ?
N1 C7 C6 125(3) . . ?
N1 C7 C8 123(3) . . ?
C6 C7 C8 111(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N1 112(6) . . ?
C10 C9 H9A 109.2 . . ?
N1 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
N1 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 C11 119(7) . . ?
C9 C10 H10A 107.5 . . ?
C11 C10 H10A 107.5 . . ?
C9 C10 H10B 107.5 . . ?
C11 C10 H10B 107.5 . . ?
H10A C10 H10B 107.0 . . ?
C10 C11 N2 102(5) . . ?
C10 C11 H11A 111.3 . . ?
N2 C11 H11A 111.3 . . ?
C10 C11 H11B 111.3 . . ?
N2 C11 H11B 111.3 . . ?
H11A C11 H11B 109.2 . . ?
N2 C12 C13 132(4) . . ?
N2 C12 H12 113.8 . . ?
C13 C12 H12 113.8 . . ?
C18 C13 C14 120(3) . . ?
C18 C13 C12 125(3) . . ?
C14 C13 C12 115(3) . . ?
C15 C14 C13 120(4) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 121(4) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C15 C16 C17 119(3) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
C16 C17 C18 120(3) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
O2 C18 C13 120(3) . . ?
O2 C18 C17 120(3) . . ?
C13 C18 C17 119(3) . . ?
N3 C19 C20 172(5) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 C22 119(2) . . ?
O3 C21 C26 121(2) . . ?
C22 C21 C26 120.0 . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 120.0 . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 120.0 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C21 120.0 . . ?
C25 C26 C27 118(2) . . ?
C21 C26 C27 122(2) . . ?
N4 C27 C26 119(3) . . ?
N4 C27 C28 105(4) . . ?
C26 C27 C28 132(4) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N4 115(6) . . ?
C30 C29 H29A 108.4 . . ?
N4 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
N4 C29 H29B 108.4 . . ?
H29A C29 H29B 107.5 . . ?
C31 C30 C29 116(6) . . ?
C31 C30 H30A 108.3 . . ?
C29 C30 H30A 108.3 . . ?
C31 C30 H30B 108.4 . . ?
C29 C30 H30B 108.4 . . ?
H30A C30 H30B 107.4 . . ?
C30 C31 N5 104(4) . . ?
C30 C31 H31A 110.9 . . ?
N5 C31 H31A 110.9 . . ?
C30 C31 H31B 110.9 . . ?
N5 C31 H31B 110.9 . . ?
H31A C31 H31B 108.9 . . ?
N5 C32 C33 124(4) . . ?
N5 C32 H32 118.1 . . ?
C33 C32 H32 118.1 . . ?
C38 C33 C32 126(3) . . ?
C38 C33 C34 123(3) . . ?
C32 C33 C34 110(3) . . ?
C35 C34 C33 115(3) . . ?
C35 C34 H34 122.4 . . ?
C33 C34 H34 122.4 . . ?
C34 C35 C36 124(4) . . ?
C34 C35 H35 118.0 . . ?
C36 C35 H35 118.0 . . ?
C37 C36 C35 114(4) . . ?
C37 C36 H36 123.2 . . ?
C35 C36 H36 123.2 . . ?
C36 C37 C38 130(4) . . ?
C36 C37 H37 115.2 . . ?
C38 C37 H37 115.2 . . ?
O4 C38 C33 122(3) . . ?
O4 C38 C37 124(3) . . ?
C33 C38 C37 114(3) . . ?
N1B C2B C3B 168(6) . . ?
C2B C3B H3B1 109.5 . . ?
C2B C3B H3B2 109.5 . . ?
H3B1 C3B H3B2 109.5 . . ?
C2B C3B H3B3 109.5 . . ?
H3B1 C3B H3B3 109.5 . . ?
H3B2 C3B H3B3 109.5 . . ?

_refine_diff_density_max         1.588
_refine_diff_density_min         -3.229
_refine_diff_density_rms         0.206

