# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1528628'
_audit_update_record             
;
2017-05-04 deposited with the CCDC.
2017-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H50 Cl6 Cu6 Gd2 N8 O13'
_chemical_formula_weight         1819.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   15.6116(5)
_cell_length_b                   15.6116(5)
_cell_length_c                   44.947(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9486.9(9)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3926
_cell_measurement_theta_min      3.1470
_cell_measurement_theta_max      25.3051

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_F_000             5304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    4.356
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5784
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'PHOTON100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13282
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         3.770
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             1845
_reflns_number_gt                1295
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0990P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1845
_refine_ls_number_parameters     122
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1529
_refine_ls_wR_factor_gt          0.1363
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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
C1 C 0.6075(7) 0.2276(7) 0.19947(19) 0.048(2) Uani 1 1 d . . . . .
H1A H 0.5945 0.2241 0.2211 0.057 Uiso 1 1 calc R U . . .
H1B H 0.6464 0.1945 0.1956 0.057 Uiso 1 1 calc R U . . .
C2 C 0.5103(7) 0.1735(7) 0.18306(18) 0.046(2) Uani 1 1 d . . . . .
H2A H 0.4824 0.1012 0.1850 0.055 Uiso 1 1 calc R U . . .
H2B H 0.4625 0.1908 0.1917 0.055 Uiso 1 1 calc R U . . .
C3 C 0.2638(9) 0.0923(11) 0.0786(3) 0.091(5) Uani 1 1 d . . . . .
H3 H 0.2308 0.0353 0.0908 0.109 Uiso 1 1 calc R U . . .
C4 C 0.2214(11) 0.0949(14) 0.0525(3) 0.122(7) Uani 1 1 d . . . . .
H4 H 0.1630 0.0380 0.0458 0.147 Uiso 1 1 calc R U . . .
C5 C 0.2662(12) 0.1858(15) 0.0350(4) 0.119(6) Uani 1 1 d . . . . .
H5 H 0.2349 0.1936 0.0179 0.143 Uiso 1 1 calc R U . . .
C6 C 0.3592(8) 0.2612(12) 0.0451(2) 0.085(4) Uani 1 1 d . . . . .
H6 H 0.3955 0.3195 0.0336 0.102 Uiso 1 1 calc R U . . .
C7 C 0.3978(7) 0.2512(9) 0.0713(2) 0.056(3) Uani 1 1 d . . . . .
C8 C 0.4971(8) 0.3333 0.0833 0.042(3) Uani 1 2 d S T P . .
Cl1 Cl 0.3145(2) 0.0265(2) 0.14203(7) 0.0719(9) Uani 1 1 d . . . . .
Cu1 Cu 0.42768(7) 0.17025(8) 0.12357(3) 0.0438(4) Uani 1 1 d . . . . .
Gd1 Gd 0.6667 0.3333 0.13438(2) 0.0289(3) Uani 1 3 d S T P . .
N1 N 0.6667 0.3333 0.1904(3) 0.039(3) Uani 1 3 d S T P . .
N2 N 0.3521(5) 0.1686(7) 0.08777(17) 0.055(2) Uani 1 1 d . . . . .
O1 O 0.5264(4) 0.2006(4) 0.15296(13) 0.0412(14) Uani 1 1 d . . . . .
O2 O 0.5261(4) 0.2948(4) 0.10630(12) 0.0384(13) Uani 1 1 d . . . . .
O3 O 0.0000 0.0000 0.0000 0.24(3) Uani 1 6 d S T P . .
H3A H 0.0449 0.0140 0.0130 0.294 Uiso 0.1667 1 d R U P . .
H3B H 0.0223 0.0459 -0.0130 0.294 Uiso 0.1667 1 d 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
C1 N1 1.489(10) . ?
C1 C2 1.510(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O1 1.402(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N2 1.359(14) . ?
C3 C4 1.356(18) . ?
C3 H3 0.9500 . ?
C4 C5 1.46(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.41(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.367(14) . ?
C6 H6 0.9500 . ?
C7 N2 1.341(13) . ?
C7 C8 1.534(13) . ?
C8 O2 1.380(8) . ?
C8 O2 1.380(9) 17_554 ?
C8 C7 1.534(13) 17_554 ?
Cl1 Cu1 2.209(3) . ?
Cu1 O1 1.901(6) . ?
Cu1 O2 1.939(6) . ?
Cu1 N2 1.988(8) . ?
Cu1 Gd1 3.3375(10) . ?
Gd1 O1 2.291(5) 2_655 ?
Gd1 O1 2.291(5) 3_665 ?
Gd1 O1 2.291(5) . ?
Gd1 O2 2.334(5) . ?
Gd1 O2 2.334(5) 2_655 ?
Gd1 O2 2.334(5) 3_665 ?
Gd1 N1 2.517(13) . ?
Gd1 Cu1 3.3375(10) 2_655 ?
Gd1 Cu1 3.3375(10) 3_665 ?
N1 C1 1.489(10) 2_655 ?
N1 C1 1.489(10) 3_665 ?
O3 H3A 0.8521 . ?
O3 H3B 0.8521 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 112.3(7) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
O1 C2 C1 108.9(7) . . ?
O1 C2 H2A 109.9 . . ?
C1 C2 H2A 109.9 . . ?
O1 C2 H2B 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
N2 C3 C4 122.2(14) . . ?
N2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C5 119.5(14) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 115.4(13) . . ?
C6 C5 H5 122.3 . . ?
C4 C5 H5 122.3 . . ?
C7 C6 C5 120.8(13) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
N2 C7 C6 122.1(11) . . ?
N2 C7 C8 116.0(7) . . ?
C6 C7 C8 121.8(9) . . ?
O2 C8 O2 113.8(10) . 17_554 ?
O2 C8 C7 109.5(4) . 17_554 ?
O2 C8 C7 108.3(5) 17_554 17_554 ?
O2 C8 C7 108.3(5) . . ?
O2 C8 C7 109.5(4) 17_554 . ?
C7 C8 C7 107.2(11) 17_554 . ?
O1 Cu1 O2 83.7(2) . . ?
O1 Cu1 N2 165.4(3) . . ?
O2 Cu1 N2 81.7(3) . . ?
O1 Cu1 Cl1 97.41(18) . . ?
O2 Cu1 Cl1 178.4(2) . . ?
N2 Cu1 Cl1 97.1(2) . . ?
O1 Cu1 Gd1 41.51(16) . . ?
O2 Cu1 Gd1 43.09(16) . . ?
N2 Cu1 Gd1 123.9(2) . . ?
Cl1 Cu1 Gd1 137.84(9) . . ?
O1 Gd1 O1 107.50(16) 2_655 3_665 ?
O1 Gd1 O1 107.50(16) 2_655 . ?
O1 Gd1 O1 107.50(16) 3_665 . ?
O1 Gd1 O2 160.3(2) 2_655 . ?
O1 Gd1 O2 92.0(2) 3_665 . ?
O1 Gd1 O2 67.3(2) . . ?
O1 Gd1 O2 67.3(2) 2_655 2_655 ?
O1 Gd1 O2 160.3(2) 3_665 2_655 ?
O1 Gd1 O2 92.0(2) . 2_655 ?
O2 Gd1 O2 93.53(19) . 2_655 ?
O1 Gd1 O2 92.0(2) 2_655 3_665 ?
O1 Gd1 O2 67.3(2) 3_665 3_665 ?
O1 Gd1 O2 160.3(2) . 3_665 ?
O2 Gd1 O2 93.53(19) . 3_665 ?
O2 Gd1 O2 93.53(19) 2_655 3_665 ?
O1 Gd1 N1 68.62(15) 2_655 . ?
O1 Gd1 N1 68.62(15) 3_665 . ?
O1 Gd1 N1 68.62(15) . . ?
O2 Gd1 N1 122.73(14) . . ?
O2 Gd1 N1 122.73(14) 2_655 . ?
O2 Gd1 N1 122.73(14) 3_665 . ?
O1 Gd1 Cu1 135.13(16) 2_655 . ?
O1 Gd1 Cu1 106.60(15) 3_665 . ?
O1 Gd1 Cu1 33.35(15) . . ?
O2 Gd1 Cu1 34.57(14) . . ?
O2 Gd1 Cu1 88.39(15) 2_655 . ?
O2 Gd1 Cu1 127.99(15) 3_665 . ?
N1 Gd1 Cu1 98.37(2) . . ?
O1 Gd1 Cu1 33.35(15) 2_655 2_655 ?
O1 Gd1 Cu1 135.13(15) 3_665 2_655 ?
O1 Gd1 Cu1 106.60(15) . 2_655 ?
O2 Gd1 Cu1 127.99(15) . 2_655 ?
O2 Gd1 Cu1 34.58(14) 2_655 2_655 ?
O2 Gd1 Cu1 88.39(15) 3_665 2_655 ?
N1 Gd1 Cu1 98.37(2) . 2_655 ?
Cu1 Gd1 Cu1 117.921(11) . 2_655 ?
O1 Gd1 Cu1 106.60(15) 2_655 3_665 ?
O1 Gd1 Cu1 33.35(15) 3_665 3_665 ?
O1 Gd1 Cu1 135.13(15) . 3_665 ?
O2 Gd1 Cu1 88.39(15) . 3_665 ?
O2 Gd1 Cu1 127.99(15) 2_655 3_665 ?
O2 Gd1 Cu1 34.58(14) 3_665 3_665 ?
N1 Gd1 Cu1 98.37(2) . 3_665 ?
Cu1 Gd1 Cu1 117.919(11) . 3_665 ?
Cu1 Gd1 Cu1 117.921(11) 2_655 3_665 ?
C1 N1 C1 112.8(5) . 2_655 ?
C1 N1 C1 112.8(5) . 3_665 ?
C1 N1 C1 112.8(5) 2_655 3_665 ?
C1 N1 Gd1 105.9(6) . . ?
C1 N1 Gd1 105.9(6) 2_655 . ?
C1 N1 Gd1 105.9(6) 3_665 . ?
C7 N2 C3 119.6(10) . . ?
C7 N2 Cu1 114.0(6) . . ?
C3 N2 Cu1 126.3(8) . . ?
C2 O1 Cu1 126.5(5) . . ?
C2 O1 Gd1 124.8(5) . . ?
Cu1 O1 Gd1 105.1(2) . . ?
C8 O2 Cu1 117.9(5) . . ?
C8 O2 Gd1 139.7(5) . . ?
Cu1 O2 Gd1 102.3(2) . . ?
H3A O3 H3B 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 O1 43.0(11) . . . . ?
N2 C3 C4 C5 -6(3) . . . . ?
C3 C4 C5 C6 8(3) . . . . ?
C4 C5 C6 C7 -6(3) . . . . ?
C5 C6 C7 N2 3(2) . . . . ?
C5 C6 C7 C8 -178.0(14) . . . . ?
N2 C7 C8 O2 11.3(12) . . . . ?
C6 C7 C8 O2 -167.6(11) . . . . ?
N2 C7 C8 O2 135.9(9) . . . 17_554 ?
C6 C7 C8 O2 -42.9(14) . . . 17_554 ?
N2 C7 C8 C7 -106.8(9) . . . 17_554 ?
C6 C7 C8 C7 74.4(11) . . . 17_554 ?
C2 C1 N1 C1 -163.7(8) . . . 2_655 ?
C2 C1 N1 C1 67.2(14) . . . 3_665 ?
C2 C1 N1 Gd1 -48.3(8) . . . . ?
C6 C7 N2 C3 -1.0(18) . . . . ?
C8 C7 N2 C3 -179.9(10) . . . . ?
C6 C7 N2 Cu1 176.5(10) . . . . ?
C8 C7 N2 Cu1 -2.3(12) . . . . ?
C4 C3 N2 C7 3(2) . . . . ?
C4 C3 N2 Cu1 -174.6(13) . . . . ?
C1 C2 O1 Cu1 -170.0(6) . . . . ?
C1 C2 O1 Gd1 -14.5(10) . . . . ?
O2 C8 O2 Cu1 -137.6(5) 17_554 . . . ?
C7 C8 O2 Cu1 101.0(6) 17_554 . . . ?
C7 C8 O2 Cu1 -15.6(9) . . . . ?
O2 C8 O2 Gd1 43.2(5) 17_554 . . . ?
C7 C8 O2 Gd1 -78.1(11) 17_554 . . . ?
C7 C8 O2 Gd1 165.2(6) . . . . ?

_refine_diff_density_max         2.882
_refine_diff_density_min         -1.774
_refine_diff_density_rms         0.177



####################################################################### 
# 
# 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 1528629'
_audit_update_record             
;
2017-05-05 deposited with the CCDC.
2017-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H48 Cl6 Cu6 N8 O12 Tb2'
_chemical_formula_weight         1804.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'

_cell_length_a                   15.8523(6)
_cell_length_b                   15.8523(6)
_cell_length_c                   44.490(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9682.3(17)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1640
_cell_measurement_theta_min      3.7631
_cell_measurement_theta_max      25.1980

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_F_000             5256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    4.402
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5156
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2012)'
_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  'PHOTON100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8945
_diffrn_reflns_av_unetI/netI     0.0979
_diffrn_reflns_av_R_equivalents  0.0958
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_theta_min         3.106
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             1861
_reflns_number_gt                981
_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    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00051(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1861
_refine_ls_number_parameters     121
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.1799
_refine_ls_R_factor_gt           0.1166
_refine_ls_wR_factor_ref         0.3585
_refine_ls_wR_factor_gt          0.3294
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_restrained_S_all      1.154
_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
C1 C 0.777(2) 0.383(2) 0.1992(6) 0.099(7) Uani 1 1 d . U . . .
H1A H 0.8071 0.4518 0.1939 0.119 Uiso 1 1 calc R U . . .
H1B H 0.7845 0.3794 0.2207 0.119 Uiso 1 1 calc R U . . .
C2 C 0.8247(17) 0.341(2) 0.1837(5) 0.086(6) Uani 1 1 d . U . . .
H2B H 0.8946 0.3829 0.1853 0.103 Uiso 1 1 calc R U . . .
H2A H 0.8076 0.2786 0.1928 0.103 Uiso 1 1 calc R U . . .
C3 C 0.900(4) 0.172(5) 0.0759(11) 0.23(3) Uani 1 1 d . U . . .
H3 H 0.9535 0.1891 0.0884 0.281 Uiso 1 1 calc R U . . .
C4 C 0.901(3) 0.136(3) 0.0522(9) 0.155(14) Uani 1 1 d . U . . .
H4 H 0.9572 0.1363 0.0455 0.186 Uiso 1 1 calc R U . . .
C5 C 0.818(4) 0.093(4) 0.0357(9) 0.183(17) Uani 1 1 d . U . . .
H5 H 0.8112 0.0565 0.0187 0.220 Uiso 1 1 calc R U . . .
C6 C 0.748(3) 0.107(3) 0.0444(6) 0.129(10) Uani 1 1 d . U . . .
H6 H 0.6951 0.0832 0.0315 0.155 Uiso 1 1 calc R U . . .
C7 C 0.7410(19) 0.1522(18) 0.0710(5) 0.083(5) Uani 1 1 d . U . . .
C8 C 0.6667 0.1673(18) 0.0833 0.070(5) Uani 1 2 d S TU P . .
Cl1 Cl 0.9655(5) 0.2830(7) 0.14232(18) 0.122(3) Uani 1 1 d . U . . .
Cu1 Cu 0.8262(2) 0.2573(2) 0.12393(6) 0.0800(12) Uani 1 1 d . U . . .
N1 N 0.6667 0.3333 0.1918(7) 0.071(6) Uani 1 3 d S TU P . .
N2 N 0.8309(17) 0.1901(16) 0.0863(5) 0.103(6) Uani 1 1 d . U . . .
O1 O 0.7974(9) 0.3263(10) 0.1527(3) 0.070(3) Uani 1 1 d . U . . .
O2 O 0.7057(11) 0.2339(11) 0.1072(3) 0.078(4) Uani 1 1 d . U . . .
Tb1 Tb 0.6667 0.3333 0.13461(4) 0.0589(8) Uani 1 3 d S TU 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
C1 C2 1.43(3) . ?
C1 N1 1.55(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 O1 1.43(2) . ?
C2 H2B 0.9700 . ?
C2 H2A 0.9700 . ?
C3 C4 1.20(4) . ?
C3 N2 1.35(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.37(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.28(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.42(3) . ?
C6 H6 0.9300 . ?
C7 N2 1.41(3) . ?
C7 C8 1.42(3) . ?
C8 O2 1.40(2) 17_654 ?
C8 O2 1.40(2) . ?
C8 C7 1.42(3) 17_654 ?
Cl1 Cu1 2.194(7) . ?
Cu1 O1 1.883(14) . ?
Cu1 O2 1.907(14) . ?
Cu1 N2 2.01(2) . ?
Cu1 Tb1 3.335(3) . ?
N1 C1 1.55(3) 3_665 ?
N1 C1 1.55(3) 2_655 ?
N1 Tb1 2.54(3) . ?
O1 Tb1 2.278(12) . ?
O2 Tb1 2.309(14) . ?
Tb1 O1 2.278(12) 3_665 ?
Tb1 O1 2.278(12) 2_655 ?
Tb1 O2 2.309(14) 2_655 ?
Tb1 O2 2.309(14) 3_665 ?
Tb1 Cu1 3.335(3) 3_665 ?
Tb1 Cu1 3.335(3) 2_655 ?

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
C2 C1 N1 113(2) . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
N1 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
O1 C2 C1 110.6(19) . . ?
O1 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
O1 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
H2B C2 H2A 108.1 . . ?
C4 C3 N2 127(4) . . ?
C4 C3 H3 116.3 . . ?
N2 C3 H3 116.3 . . ?
C3 C4 C5 118(4) . . ?
C3 C4 H4 121.2 . . ?
C5 C4 H4 121.2 . . ?
C6 C5 C4 117(4) . . ?
C6 C5 H5 121.3 . . ?
C4 C5 H5 121.3 . . ?
C5 C6 C7 129(4) . . ?
C5 C6 H6 115.4 . . ?
C7 C6 H6 115.4 . . ?
N2 C7 C8 119.1(18) . . ?
N2 C7 C6 107(2) . . ?
C8 C7 C6 134(2) . . ?
O2 C8 O2 116(2) 17_654 . ?
O2 C8 C7 107.0(11) 17_654 . ?
O2 C8 C7 109.1(12) . . ?
O2 C8 C7 109.1(12) 17_654 17_654 ?
O2 C8 C7 107.0(11) . 17_654 ?
C7 C8 C7 109(3) . 17_654 ?
O1 Cu1 O2 82.5(6) . . ?
O1 Cu1 N2 163.9(7) . . ?
O2 Cu1 N2 82.5(8) . . ?
O1 Cu1 Cl1 98.8(4) . . ?
O2 Cu1 Cl1 178.7(5) . . ?
N2 Cu1 Cl1 96.2(7) . . ?
O1 Cu1 Tb1 41.0(4) . . ?
O2 Cu1 Tb1 42.2(4) . . ?
N2 Cu1 Tb1 123.2(6) . . ?
Cl1 Cu1 Tb1 139.0(2) . . ?
C1 N1 C1 115.6(10) . 3_665 ?
C1 N1 C1 115.6(10) . 2_655 ?
C1 N1 C1 115.6(10) 3_665 2_655 ?
C1 N1 Tb1 102.3(15) . . ?
C1 N1 Tb1 102.3(15) 3_665 . ?
C1 N1 Tb1 102.3(15) 2_655 . ?
C3 N2 C7 120(3) . . ?
C3 N2 Cu1 131(2) . . ?
C7 N2 Cu1 109.3(15) . . ?
C2 O1 Cu1 127.4(13) . . ?
C2 O1 Tb1 123.0(12) . . ?
Cu1 O1 Tb1 106.1(6) . . ?
C8 O2 Cu1 117.6(11) . . ?
C8 O2 Tb1 138.2(11) . . ?
Cu1 O2 Tb1 104.2(6) . . ?
O1 Tb1 O1 108.2(3) . 3_665 ?
O1 Tb1 O1 108.2(3) . 2_655 ?
O1 Tb1 O1 108.2(3) 3_665 2_655 ?
O1 Tb1 O2 66.0(5) . . ?
O1 Tb1 O2 91.6(5) 3_665 . ?
O1 Tb1 O2 160.1(5) 2_655 . ?
O1 Tb1 O2 91.6(5) . 2_655 ?
O1 Tb1 O2 160.1(5) 3_665 2_655 ?
O1 Tb1 O2 66.0(5) 2_655 2_655 ?
O2 Tb1 O2 94.6(5) . 2_655 ?
O1 Tb1 O2 160.1(5) . 3_665 ?
O1 Tb1 O2 66.0(5) 3_665 3_665 ?
O1 Tb1 O2 91.6(5) 2_655 3_665 ?
O2 Tb1 O2 94.6(5) . 3_665 ?
O2 Tb1 O2 94.6(5) 2_655 3_665 ?
O1 Tb1 N1 69.3(3) . . ?
O1 Tb1 N1 69.3(3) 3_665 . ?
O1 Tb1 N1 69.3(3) 2_655 . ?
O2 Tb1 N1 121.9(4) . . ?
O2 Tb1 N1 121.9(4) 2_655 . ?
O2 Tb1 N1 121.9(4) 3_665 . ?
O1 Tb1 Cu1 32.9(3) . . ?
O1 Tb1 Cu1 106.1(4) 3_665 . ?
O1 Tb1 Cu1 135.6(4) 2_655 . ?
O2 Tb1 Cu1 33.7(3) . . ?
O2 Tb1 Cu1 89.3(4) 2_655 . ?
O2 Tb1 Cu1 128.2(4) 3_665 . ?
N1 Tb1 Cu1 98.19(5) . . ?
O1 Tb1 Cu1 135.6(4) . 3_665 ?
O1 Tb1 Cu1 32.9(3) 3_665 3_665 ?
O1 Tb1 Cu1 106.1(4) 2_655 3_665 ?
O2 Tb1 Cu1 89.3(4) . 3_665 ?
O2 Tb1 Cu1 128.2(4) 2_655 3_665 ?
O2 Tb1 Cu1 33.7(3) 3_665 3_665 ?
N1 Tb1 Cu1 98.19(5) . 3_665 ?
Cu1 Tb1 Cu1 118.01(3) . 3_665 ?
O1 Tb1 Cu1 106.1(4) . 2_655 ?
O1 Tb1 Cu1 135.6(4) 3_665 2_655 ?
O1 Tb1 Cu1 32.9(3) 2_655 2_655 ?
O2 Tb1 Cu1 128.2(4) . 2_655 ?
O2 Tb1 Cu1 33.7(3) 2_655 2_655 ?
O2 Tb1 Cu1 89.3(4) 3_665 2_655 ?
N1 Tb1 Cu1 98.19(5) . 2_655 ?
Cu1 Tb1 Cu1 118.01(3) . 2_655 ?
Cu1 Tb1 Cu1 118.01(3) 3_665 2_655 ?

_refine_diff_density_max         2.819
_refine_diff_density_min         -1.479
_refine_diff_density_rms         0.265

####################################################################### 
# 
# 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 1528626'
_audit_update_record             
;
2017-05-04 deposited with the CCDC.
2017-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H50 Cl6 Cu6 Ho2 N8 O13'
_chemical_formula_weight         1834.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   15.6219(5)
_cell_length_b                   15.6219(5)
_cell_length_c                   44.866(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9482.3(8)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2106
_cell_measurement_theta_min      3.1456
_cell_measurement_theta_max      25.2813

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_F_000             5340
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    4.763
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6001
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'PHOTON100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7941
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         3.772
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             1840
_reflns_number_gt                1244
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0430P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1840
_refine_ls_number_parameters     122
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.0867
_refine_ls_wR_factor_gt          0.0787
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6082(6) 0.2282(5) 0.19971(14) 0.0455(19) Uani 1 1 d . . . . .
H1A H 0.5933 0.2256 0.2213 0.055 Uiso 1 1 calc R U . . .
H1B H 0.6484 0.1961 0.1967 0.055 Uiso 1 1 calc R U . . .
C2 C 0.5137(5) 0.1721(5) 0.18293(14) 0.0418(19) Uani 1 1 d . . . . .
H2A H 0.4888 0.1003 0.1847 0.050 Uiso 1 1 calc R U . . .
H2B H 0.4634 0.1860 0.1914 0.050 Uiso 1 1 calc R U . . .
C3 C 0.2659(6) 0.0930(8) 0.07878(17) 0.085(4) Uani 1 1 d . . . . .
H3 H 0.2341 0.0345 0.0904 0.102 Uiso 1 1 calc R U . . .
C4 C 0.2214(7) 0.1000(10) 0.0532(2) 0.130(6) Uani 1 1 d . . . . .
H4 H 0.1589 0.0468 0.0473 0.156 Uiso 1 1 calc R U . . .
C5 C 0.2680(8) 0.1848(11) 0.0361(2) 0.126(6) Uani 1 1 d . . . . .
H5 H 0.2379 0.1904 0.0184 0.151 Uiso 1 1 calc R U . . .
C6 C 0.3607(7) 0.2627(9) 0.04524(17) 0.079(3) Uani 1 1 d . . . . .
H6 H 0.3941 0.3215 0.0337 0.095 Uiso 1 1 calc R U . . .
C7 C 0.4019(6) 0.2522(7) 0.07114(15) 0.050(2) Uani 1 1 d . . . . .
C8 C 0.5002(6) 0.3333 0.0833 0.034(2) Uani 1 2 d S T P . .
Cl1 Cl 0.31630(15) 0.02718(17) 0.14228(5) 0.0688(7) Uani 1 1 d . . . . .
Cu1 Cu 0.43030(6) 0.16973(7) 0.12341(2) 0.0398(3) Uani 1 1 d . . . . .
Ho1 Ho 0.6667 0.3333 0.13474(2) 0.02254(16) Uani 1 3 d S T P . .
N1 N 0.6667 0.3333 0.19028(18) 0.032(2) Uani 1 3 d S T P . .
N2 N 0.3547(4) 0.1687(6) 0.08763(12) 0.0558(19) Uani 1 1 d . . . . .
O1 O 0.5298(3) 0.2005(3) 0.15246(8) 0.0346(11) Uani 1 1 d . . . . .
O2 O 0.5298(3) 0.2946(3) 0.10625(9) 0.0311(11) Uani 1 1 d . . . . .
O3 O 0.0000 0.0000 0.0000 0.28(2) Uani 1 6 d S T P . .
H3A H 0.0449 0.0140 0.0130 0.332 Uiso 0.1667 1 d R U P . .
H3B H 0.0223 0.0459 -0.0130 0.332 Uiso 0.1667 1 d 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
C1 N1 1.486(7) . ?
C1 C2 1.490(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O1 1.421(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N2 1.356(10) . ?
C3 C4 1.373(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(16) . ?
C4 H4 0.9500 . ?
C5 C6 1.408(14) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(10) . ?
C6 H6 0.9500 . ?
C7 N2 1.354(10) . ?
C7 C8 1.523(9) . ?
C8 O2 1.385(6) . ?
C8 O2 1.385(6) 17_554 ?
C8 C7 1.522(9) 17_554 ?
Cl1 Cu1 2.209(2) . ?
Cu1 O1 1.897(4) . ?
Cu1 O2 1.945(4) . ?
Cu1 N2 1.988(6) . ?
Cu1 Ho1 3.3147(8) . ?
Ho1 O1 2.252(4) . ?
Ho1 O1 2.252(4) 2_655 ?
Ho1 O1 2.252(4) 3_665 ?
Ho1 O2 2.297(4) . ?
Ho1 O2 2.297(4) 2_655 ?
Ho1 O2 2.297(4) 3_665 ?
Ho1 N1 2.492(8) . ?
Ho1 Cu1 3.3147(8) 2_655 ?
Ho1 Cu1 3.3147(8) 3_665 ?
N1 C1 1.486(7) 2_655 ?
N1 C1 1.486(7) 3_665 ?
O3 H3A 0.8517 . ?
O3 H3B 0.8517 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 112.8(5) . . ?
N1 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
O1 C2 C1 109.5(5) . . ?
O1 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
O1 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
N2 C3 C4 120.9(10) . . ?
N2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 119.7(10) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 119.2(9) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C7 C6 C5 118.8(10) . . ?
C7 C6 H6 120.6 . . ?
C5 C6 H6 120.6 . . ?
N2 C7 C6 121.0(8) . . ?
N2 C7 C8 116.2(5) . . ?
C6 C7 C8 122.8(8) . . ?
O2 C8 O2 112.9(7) . 17_554 ?
O2 C8 C7 109.5(3) . 17_554 ?
O2 C8 C7 108.8(4) 17_554 17_554 ?
O2 C8 C7 108.8(4) . . ?
O2 C8 C7 109.5(3) 17_554 . ?
C7 C8 C7 107.3(8) 17_554 . ?
O1 Cu1 O2 82.80(18) . . ?
O1 Cu1 N2 164.8(2) . . ?
O2 Cu1 N2 82.1(2) . . ?
O1 Cu1 Cl1 97.92(14) . . ?
O2 Cu1 Cl1 179.20(14) . . ?
N2 Cu1 Cl1 97.2(2) . . ?
O1 Cu1 Ho1 40.84(13) . . ?
O2 Cu1 Ho1 42.58(12) . . ?
N2 Cu1 Ho1 123.94(19) . . ?
Cl1 Cu1 Ho1 138.09(7) . . ?
O1 Ho1 O1 108.24(10) . 2_655 ?
O1 Ho1 O1 108.24(10) . 3_665 ?
O1 Ho1 O1 108.24(10) 2_655 3_665 ?
O1 Ho1 O2 67.92(15) . . ?
O1 Ho1 O2 159.76(15) 2_655 . ?
O1 Ho1 O2 91.55(16) 3_665 . ?
O1 Ho1 O2 91.55(16) . 2_655 ?
O1 Ho1 O2 67.92(15) 2_655 2_655 ?
O1 Ho1 O2 159.76(15) 3_665 2_655 ?
O2 Ho1 O2 92.04(14) . 2_655 ?
O1 Ho1 O2 159.75(15) . 3_665 ?
O1 Ho1 O2 91.55(16) 2_655 3_665 ?
O1 Ho1 O2 67.92(15) 3_665 3_665 ?
O2 Ho1 O2 92.04(14) . 3_665 ?
O2 Ho1 O2 92.04(14) 2_655 3_665 ?
O1 Ho1 N1 69.32(10) . . ?
O1 Ho1 N1 69.32(10) 2_655 . ?
O1 Ho1 N1 69.32(10) 3_665 . ?
O2 Ho1 N1 123.81(10) . . ?
O2 Ho1 N1 123.80(10) 2_655 . ?
O2 Ho1 N1 123.80(10) 3_665 . ?
O1 Ho1 Cu1 106.12(12) . 2_655 ?
O1 Ho1 Cu1 33.43(10) 2_655 2_655 ?
O1 Ho1 Cu1 135.99(12) 3_665 2_655 ?
O2 Ho1 Cu1 126.88(11) . 2_655 ?
O2 Ho1 Cu1 34.95(11) 2_655 2_655 ?
O2 Ho1 Cu1 87.92(11) 3_665 2_655 ?
N1 Ho1 Cu1 98.816(16) . 2_655 ?
O1 Ho1 Cu1 135.99(12) . 3_665 ?
O1 Ho1 Cu1 106.13(12) 2_655 3_665 ?
O1 Ho1 Cu1 33.43(10) 3_665 3_665 ?
O2 Ho1 Cu1 87.92(11) . 3_665 ?
O2 Ho1 Cu1 126.88(11) 2_655 3_665 ?
O2 Ho1 Cu1 34.95(11) 3_665 3_665 ?
N1 Ho1 Cu1 98.816(16) . 3_665 ?
Cu1 Ho1 Cu1 117.695(8) 2_655 3_665 ?
O1 Ho1 Cu1 33.43(10) . . ?
O1 Ho1 Cu1 135.99(12) 2_655 . ?
O1 Ho1 Cu1 106.13(12) 3_665 . ?
O2 Ho1 Cu1 34.95(11) . . ?
O2 Ho1 Cu1 87.92(11) 2_655 . ?
O2 Ho1 Cu1 126.87(11) 3_665 . ?
N1 Ho1 Cu1 98.818(16) . . ?
Cu1 Ho1 Cu1 117.694(8) 2_655 . ?
Cu1 Ho1 Cu1 117.695(8) 3_665 . ?
C1 N1 C1 112.2(4) 2_655 . ?
C1 N1 C1 112.2(4) 2_655 3_665 ?
C1 N1 C1 112.2(4) . 3_665 ?
C1 N1 Ho1 106.5(4) 2_655 . ?
C1 N1 Ho1 106.5(4) . . ?
C1 N1 Ho1 106.5(4) 3_665 . ?
C3 N2 C7 120.4(7) . . ?
C3 N2 Cu1 126.0(6) . . ?
C7 N2 Cu1 113.5(5) . . ?
C2 O1 Cu1 126.0(4) . . ?
C2 O1 Ho1 124.5(4) . . ?
Cu1 O1 Ho1 105.74(18) . . ?
C8 O2 Cu1 117.3(3) . . ?
C8 O2 Ho1 140.2(4) . . ?
Cu1 O2 Ho1 102.47(17) . . ?
H3A O3 H3B 108.3 . . ?

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
N1 C1 C2 O1 40.3(8) . . . . ?
N2 C3 C4 C5 0.6(19) . . . . ?
C3 C4 C5 C6 0(2) . . . . ?
C4 C5 C6 C7 -0.4(19) . . . . ?
C5 C6 C7 N2 0.1(14) . . . . ?
C5 C6 C7 C8 -178.2(9) . . . . ?
N2 C7 C8 O2 12.3(9) . . . . ?
C6 C7 C8 O2 -169.4(7) . . . . ?
N2 C7 C8 O2 136.1(6) . . . 17_554 ?
C6 C7 C8 O2 -45.6(10) . . . 17_554 ?
N2 C7 C8 C7 -106.0(7) . . . 17_554 ?
C6 C7 C8 C7 72.3(8) . . . 17_554 ?
C2 C1 N1 C1 -162.1(6) . . . 2_655 ?
C2 C1 N1 C1 70.4(10) . . . 3_665 ?
C2 C1 N1 Ho1 -45.9(6) . . . . ?
C4 C3 N2 C7 -0.9(15) . . . . ?
C4 C3 N2 Cu1 -178.7(8) . . . . ?
C6 C7 N2 C3 0.6(12) . . . . ?
C8 C7 N2 C3 178.9(7) . . . . ?
C6 C7 N2 Cu1 178.6(7) . . . . ?
C8 C7 N2 Cu1 -3.1(9) . . . . ?
C1 C2 O1 Cu1 -167.7(4) . . . . ?
C1 C2 O1 Ho1 -13.0(8) . . . . ?
O2 Cu1 O1 C2 150.0(5) . . . . ?
N2 Cu1 O1 C2 157.3(9) . . . . ?
Cl1 Cu1 O1 C2 -30.3(5) . . . . ?
Ho1 Cu1 O1 C2 158.5(6) . . . . ?
O2 Cu1 O1 Ho1 -8.52(19) . . . . ?
N2 Cu1 O1 Ho1 -1.2(10) . . . . ?
Cl1 Cu1 O1 Ho1 171.14(16) . . . . ?
O2 C8 O2 Cu1 -138.0(3) 17_554 . . . ?
C7 C8 O2 Cu1 100.6(5) 17_554 . . . ?
C7 C8 O2 Cu1 -16.3(6) . . . . ?
O2 C8 O2 Ho1 45.4(4) 17_554 . . . ?
C7 C8 O2 Ho1 -75.9(8) 17_554 . . . ?
C7 C8 O2 Ho1 167.1(4) . . . . ?

_refine_diff_density_max         1.470
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.140



####################################################################### 
# 
# 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 1528627'
_audit_update_record             
;
2017-05-04 deposited with the CCDC.
2017-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H62 Cl6 Cu6 Er2 N8 O19'
_chemical_formula_weight         1947.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   15.7612(5)
_cell_length_b                   15.7612(5)
_cell_length_c                   44.844(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9647.5(8)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2903
_cell_measurement_theta_min      3.7574
_cell_measurement_theta_max      25.1669

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_F_000             5712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    4.843
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6550
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2012)'
_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  'PHOTON100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11237
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         3.120
_diffrn_reflns_theta_max         25.359
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             1958
_reflns_number_gt                1378
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0486P)²+40.7458P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1958
_refine_ls_number_parameters     161
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.0918
_refine_ls_wR_factor_gt          0.0784
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.045
_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
C1 C 0.6100(6) 0.2295(5) 0.19937(15) 0.052(2) Uani 1 1 d . . . . .
H1A H 0.5959 0.2265 0.2205 0.10(3) Uiso 1 1 calc R . . . .
H1B H 0.6497 0.1991 0.1963 0.08(3) Uiso 1 1 calc R . . . .
C2 C 0.5158(5) 0.1725(6) 0.18280(14) 0.0439(18) Uani 1 1 d . . . . .
H2A H 0.4929 0.1030 0.1843 0.07(3) Uiso 1 1 calc R . . . .
H2B H 0.4664 0.1847 0.1913 0.14(5) Uiso 1 1 calc R . . . .
C3 C 0.2701(6) 0.0976(9) 0.07860(19) 0.094(4) Uani 1 1 d . . . . .
H3 H 0.2374 0.0417 0.0903 0.06(2) Uiso 1 1 calc R . . . .
C4 C 0.2282(8) 0.1032(10) 0.0529(2) 0.129(6) Uani 1 1 d . . . . .
H4 H 0.1673 0.0521 0.0471 0.09(3) Uiso 1 1 calc R . . . .
C5 C 0.2776(7) 0.1864(12) 0.0354(2) 0.130(6) Uani 1 1 d . . . . .
H5 H 0.2500 0.1912 0.0176 0.12(4) Uiso 1 1 calc R . . . .
C6 C 0.3662(6) 0.2607(9) 0.04426(17) 0.085(4) Uani 1 1 d . . . . .
H6 H 0.3997 0.3167 0.0326 0.039(19) Uiso 1 1 calc R . . . .
C7 C 0.4061(5) 0.2521(7) 0.07090(15) 0.052(2) Uani 1 1 d . . . . .
C8 C 0.5035(6) 0.3333 0.0833 0.035(2) Uani 1 2 d S T P . .
Cl1 Cl 0.31740(14) 0.03148(16) 0.14236(5) 0.0656(6) Uani 1 1 d . . . . .
Cu1 Cu 0.43258(6) 0.17163(6) 0.12343(2) 0.0385(2) Uani 1 1 d . . . . .
Er1 Er 0.6667 0.3333 0.13477(2) 0.02272(16) Uani 1 3 d S T P . .
N1 N 0.6667 0.3333 0.19015(19) 0.033(2) Uani 1 3 d S T P . .
N2 N 0.3575(4) 0.1702(5) 0.08766(11) 0.0546(18) Uani 1 1 d . . . . .
O1 O 0.5314(3) 0.2018(3) 0.15215(9) 0.0337(10) Uani 1 1 d . . . . .
O2 O 0.5322(3) 0.2940(3) 0.10630(9) 0.0346(11) Uani 1 1 d . . . . .
O3 O 0.0000 0.0000 0.0000 0.29(2) Uani 1 6 d S T P . .
H3A H 0.0449 0.0140 0.0130 0.347 Uiso 0.1667 1 d R U P . .
H3B H 0.0223 0.0459 -0.0130 0.347 Uiso 0.1667 1 d R U P . .
O4A O 0.173(3) 0.797(2) 0.0963(10) 0.25(2) Uani 0.48(3) 1 d D U P A 1
H4AB H 0.145(16) 0.830(15) 0.101(7) 0.296 Uiso 0.48(3) 1 d D U P A 1
H4AA H 0.15(2) 0.77(2) 0.080(4) 0.296 Uiso 0.48(3) 1 d D U P A 1
O4B O 0.239(6) 0.775(5) 0.123(2) 0.52(4) Uani 0.52(3) 1 d D U P A 2
H4BA H 0.25(3) 0.729(17) 0.118(9) 0.627 Uiso 0.52(3) 1 d D U P A 2
H4BB H 0.25(4) 0.78(3) 0.141(3) 0.627 Uiso 0.52(3) 1 d D U P A 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
C1 N1 1.478(7) . ?
C1 C2 1.493(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 O1 1.431(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.339(10) . ?
C3 C4 1.352(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(17) . ?
C4 H4 0.9300 . ?
C5 C6 1.359(14) . ?
C5 H5 0.9300 . ?
C6 C7 1.388(10) . ?
C6 H6 0.9300 . ?
C7 N2 1.352(10) . ?
C7 C8 1.531(9) . ?
C8 O2 1.389(6) 17_554 ?
C8 O2 1.389(6) . ?
C8 C7 1.531(9) 17_554 ?
Cl1 Cu1 2.210(2) . ?
Cu1 O1 1.889(4) . ?
Cu1 O2 1.936(4) . ?
Cu1 N2 1.987(6) . ?
Cu1 Er1 3.3112(8) . ?
Er1 O1 2.243(4) . ?
Er1 O1 2.243(4) 3_665 ?
Er1 O1 2.243(4) 2_655 ?
Er1 O2 2.278(4) 2_655 ?
Er1 O2 2.278(4) 3_665 ?
Er1 O2 2.278(4) . ?
Er1 N1 2.483(8) . ?
Er1 Cu1 3.3112(8) 2_655 ?
Er1 Cu1 3.3112(8) 3_665 ?
N1 C1 1.478(7) 3_665 ?
N1 C1 1.478(7) 2_655 ?
O3 H3A 0.8556 . ?
O3 H3B 0.8556 . ?
O4A O4A 1.64(10) 16_454 ?
O4A H4AA 0.851(10) . ?
O4B H4BA 0.850(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 113.3(6) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
O1 C2 C1 109.0(6) . . ?
O1 C2 H2A 109.9 . . ?
C1 C2 H2A 109.9 . . ?
O1 C2 H2B 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
N2 C3 C4 122.0(10) . . ?
N2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C3 C4 C5 118.9(10) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 119.9(9) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 119.2(10) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
N2 C7 C6 120.3(8) . . ?
N2 C7 C8 116.7(5) . . ?
C6 C7 C8 123.1(7) . . ?
O2 C8 O2 113.5(7) 17_554 . ?
O2 C8 C7 108.1(3) 17_554 17_554 ?
O2 C8 C7 109.3(3) . 17_554 ?
O2 C8 C7 109.3(3) 17_554 . ?
O2 C8 C7 108.1(3) . . ?
C7 C8 C7 108.3(8) 17_554 . ?
O1 Cu1 O2 82.17(17) . . ?
O1 Cu1 N2 164.7(2) . . ?
O2 Cu1 N2 82.7(2) . . ?
O1 Cu1 Cl1 98.71(13) . . ?
O2 Cu1 Cl1 179.11(14) . . ?
N2 Cu1 Cl1 96.42(19) . . ?
O1 Cu1 Er1 40.58(12) . . ?
O2 Cu1 Er1 42.05(12) . . ?
N2 Cu1 Er1 124.13(17) . . ?
Cl1 Cu1 Er1 138.81(6) . . ?
O1 Er1 O1 108.60(10) . 3_665 ?
O1 Er1 O1 108.60(10) . 2_655 ?
O1 Er1 O1 108.60(10) 3_665 2_655 ?
O1 Er1 O2 91.84(16) . 2_655 ?
O1 Er1 O2 159.01(16) 3_665 2_655 ?
O1 Er1 O2 67.56(14) 2_655 2_655 ?
O1 Er1 O2 159.01(16) . 3_665 ?
O1 Er1 O2 67.56(14) 3_665 3_665 ?
O1 Er1 O2 91.84(16) 2_655 3_665 ?
O2 Er1 O2 91.66(14) 2_655 3_665 ?
O1 Er1 O2 67.56(14) . . ?
O1 Er1 O2 91.85(16) 3_665 . ?
O1 Er1 O2 159.01(16) 2_655 . ?
O2 Er1 O2 91.66(14) 2_655 . ?
O2 Er1 O2 91.66(14) 3_665 . ?
O1 Er1 N1 69.67(10) . . ?
O1 Er1 N1 69.67(10) 3_665 . ?
O1 Er1 N1 69.67(10) 2_655 . ?
O2 Er1 N1 124.08(10) 2_655 . ?
O2 Er1 N1 124.08(10) 3_665 . ?
O2 Er1 N1 124.09(10) . . ?
O1 Er1 Cu1 105.96(11) . 2_655 ?
O1 Er1 Cu1 136.20(11) 3_665 2_655 ?
O1 Er1 Cu1 33.23(10) 2_655 2_655 ?
O2 Er1 Cu1 34.69(10) 2_655 2_655 ?
O2 Er1 Cu1 88.41(11) 3_665 2_655 ?
O2 Er1 Cu1 126.27(12) . 2_655 ?
N1 Er1 Cu1 98.842(15) . 2_655 ?
O1 Er1 Cu1 33.23(10) . . ?
O1 Er1 Cu1 105.96(11) 3_665 . ?
O1 Er1 Cu1 136.20(11) 2_655 . ?
O2 Er1 Cu1 88.41(11) 2_655 . ?
O2 Er1 Cu1 126.27(12) 3_665 . ?
O2 Er1 Cu1 34.69(10) . . ?
N1 Er1 Cu1 98.841(15) . . ?
Cu1 Er1 Cu1 117.681(8) 2_655 . ?
O1 Er1 Cu1 136.20(11) . 3_665 ?
O1 Er1 Cu1 33.23(10) 3_665 3_665 ?
O1 Er1 Cu1 105.96(11) 2_655 3_665 ?
O2 Er1 Cu1 126.27(12) 2_655 3_665 ?
O2 Er1 Cu1 34.69(10) 3_665 3_665 ?
O2 Er1 Cu1 88.41(11) . 3_665 ?
N1 Er1 Cu1 98.842(15) . 3_665 ?
Cu1 Er1 Cu1 117.681(8) 2_655 3_665 ?
Cu1 Er1 Cu1 117.683(8) . 3_665 ?
C1 N1 C1 112.5(4) 3_665 2_655 ?
C1 N1 C1 112.5(4) 3_665 . ?
C1 N1 C1 112.5(4) 2_655 . ?
C1 N1 Er1 106.2(4) 3_665 . ?
C1 N1 Er1 106.2(4) 2_655 . ?
C1 N1 Er1 106.2(4) . . ?
C3 N2 C7 119.8(7) . . ?
C3 N2 Cu1 127.3(6) . . ?
C7 N2 Cu1 112.8(5) . . ?
C2 O1 Cu1 125.9(4) . . ?
C2 O1 Er1 124.2(4) . . ?
Cu1 O1 Er1 106.19(17) . . ?
C8 O2 Cu1 117.1(3) . . ?
C8 O2 Er1 139.5(3) . . ?
Cu1 O2 Er1 103.26(17) . . ?
H3A O3 H3B 108.0 . . ?
O4A O4A H4AA 53(10) 16_454 . ?

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
N1 C1 C2 O1 40.0(9) . . . . ?
N2 C3 C4 C5 0(2) . . . . ?
C3 C4 C5 C6 0(2) . . . . ?
C4 C5 C6 C7 0(2) . . . . ?
C5 C6 C7 N2 0.5(16) . . . . ?
C5 C6 C7 C8 -177.7(10) . . . . ?
N2 C7 C8 O2 138.5(6) . . . 17_554 ?
C6 C7 C8 O2 -43.2(10) . . . 17_554 ?
N2 C7 C8 O2 14.5(9) . . . . ?
C6 C7 C8 O2 -167.2(8) . . . . ?
N2 C7 C8 C7 -103.8(7) . . . 17_554 ?
C6 C7 C8 C7 74.4(8) . . . 17_554 ?
C2 C1 N1 C1 69.5(11) . . . 3_665 ?
C2 C1 N1 C1 -162.2(7) . . . 2_655 ?
C2 C1 N1 Er1 -46.4(7) . . . . ?
C4 C3 N2 C7 0.1(16) . . . . ?
C4 C3 N2 Cu1 -176.6(9) . . . . ?
C6 C7 N2 C3 -0.6(13) . . . . ?
C8 C7 N2 C3 177.8(8) . . . . ?
C6 C7 N2 Cu1 176.6(7) . . . . ?
C8 C7 N2 Cu1 -5.1(9) . . . . ?
C1 C2 O1 Cu1 -167.1(5) . . . . ?
C1 C2 O1 Er1 -11.7(8) . . . . ?
O2 Cu1 O1 C2 151.5(5) . . . . ?
N2 Cu1 O1 C2 159.8(9) . . . . ?
Cl1 Cu1 O1 C2 -28.6(5) . . . . ?
Er1 Cu1 O1 C2 158.9(6) . . . . ?
O2 Cu1 O1 Er1 -7.43(19) . . . . ?
N2 Cu1 O1 Er1 0.8(10) . . . . ?
Cl1 Cu1 O1 Er1 172.45(15) . . . . ?
O2 C8 O2 Cu1 -139.2(4) 17_554 . . . ?
C7 C8 O2 Cu1 100.1(5) 17_554 . . . ?
C7 C8 O2 Cu1 -17.7(6) . . . . ?
O2 C8 O2 Er1 46.0(4) 17_554 . . . ?
C7 C8 O2 Er1 -74.7(8) 17_554 . . . ?
C7 C8 O2 Er1 167.5(4) . . . . ?

_refine_diff_density_max         1.580
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.133



####################################################################### 
# 
# 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 1528630'
_audit_update_record             
;
2017-05-04 deposited with the CCDC.
2017-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H50 Cl6 Cu6 Dy2 N8 O13'
_chemical_formula_weight         1829.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'

_cell_length_a                   15.6308(12)
_cell_length_b                   15.6308(12)
_cell_length_c                   44.638(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9445(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1501
_cell_measurement_theta_min      3.7814
_cell_measurement_theta_max      25.2571

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_F_000             5327
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    4.642
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4824
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2012)'
_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  'PHOTON100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7435
_diffrn_reflns_av_unetI/netI     0.0939
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_theta_min         3.521
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             1829
_reflns_number_gt                1058
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1029P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00024(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1829
_refine_ls_number_parameters     123
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.0732
_refine_ls_wR_factor_ref         0.1934
_refine_ls_wR_factor_gt          0.1781
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
C1 C 0.6053(11) 0.2243(11) 0.1989(3) 0.056(4) Uani 1 1 d . . . . .
H1A H 0.6433 0.1922 0.1948 0.067 Uiso 1 1 calc R U . . .
H1B H 0.5923 0.2193 0.2203 0.067 Uiso 1 1 calc R U . . .
C2 C 0.5127(11) 0.1731(11) 0.1832(3) 0.055(4) Uani 1 1 d . . . . .
H2A H 0.4853 0.1023 0.1851 0.066 Uiso 1 1 calc R U . . .
H2B H 0.4661 0.1901 0.1917 0.066 Uiso 1 1 calc R U . . .
C3 C 0.2664(15) 0.094(2) 0.0789(4) 0.127(10) Uani 1 1 d . . . . .
H3 H 0.2334 0.0412 0.0918 0.153 Uiso 1 1 calc R U . . .
C4 C 0.2225(15) 0.092(2) 0.0528(4) 0.156(15) Uani 1 1 d . . . . .
H4 H 0.1659 0.0363 0.0459 0.187 Uiso 1 1 calc R U . . .
C5 C 0.2722(15) 0.186(2) 0.0360(5) 0.149(9) Uani 1 1 d . U . . .
H5 H 0.2407 0.1936 0.0195 0.179 Uiso 1 1 calc R U . . .
C6 C 0.3616(14) 0.2595(18) 0.0439(3) 0.104(6) Uani 1 1 d . U . . .
H6 H 0.3950 0.3138 0.0314 0.125 Uiso 1 1 calc R U . . .
C7 C 0.4060(12) 0.2555(15) 0.0715(3) 0.071(5) Uani 1 1 d . . . . .
C8 C 0.5009(11) 0.3333 0.0833 0.041(5) Uani 1 2 d S T P . .
Cl1 Cl 0.3154(3) 0.0292(3) 0.14236(10) 0.0850(15) Uani 1 1 d . . . . .
Cu1 Cu 0.43026(13) 0.17111(14) 0.12352(4) 0.0534(6) Uani 1 1 d . . . . .
Dy1 Dy 0.6667 0.3333 0.13455(2) 0.0359(4) Uani 1 3 d S T P . .
N1 N 0.6667 0.3333 0.1904(4) 0.042(4) Uani 1 3 d S T P . .
N2 N 0.3550(9) 0.1688(11) 0.0875(2) 0.064(4) Uani 1 1 d . . . . .
O1 O 0.5294(7) 0.2010(6) 0.15233(16) 0.047(2) Uani 1 1 d . . . . .
O2 O 0.5296(6) 0.2963(7) 0.10647(18) 0.049(2) Uani 1 1 d . . . . .
O3 O 0.0000 0.0000 0.0000 0.31(5) Uani 1 6 d S T P . .
H3A H 0.0449 0.0140 0.0130 0.371 Uiso 0.1667 1 d R U P . .
H3B H 0.0223 0.0459 -0.0130 0.371 Uiso 0.1667 1 d 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
C1 C2 1.438(19) . ?
C1 N1 1.528(15) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 O1 1.428(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.34(2) . ?
C3 C4 1.34(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.47(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.34(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.431(18) . ?
C6 H6 0.9300 . ?
C7 N2 1.38(2) . ?
C7 C8 1.467(19) . ?
C8 O2 1.365(13) 18_554 ?
C8 O2 1.365(13) . ?
C8 C7 1.467(19) 18_554 ?
Cl1 Cu1 2.206(4) . ?
Cu1 O1 1.884(9) . ?
Cu1 O2 1.945(9) . ?
Cu1 N2 1.982(11) . ?
Cu1 Dy1 3.3101(18) . ?
Dy1 O1 2.253(9) . ?
Dy1 O1 2.253(9) 2_655 ?
Dy1 O1 2.253(9) 3_665 ?
Dy1 O2 2.293(8) 2_655 ?
Dy1 O2 2.293(8) 3_665 ?
Dy1 O2 2.293(8) . ?
Dy1 N1 2.493(17) . ?
Dy1 Cu1 3.3101(18) 2_655 ?
Dy1 Cu1 3.3101(18) 3_665 ?
N1 C1 1.528(15) 2_655 ?
N1 C1 1.528(15) 3_665 ?
O3 H3A 0.8500 . ?
O3 H3B 0.8499 . ?

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
C2 C1 N1 113.3(11) . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
N1 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
O1 C2 C1 108.8(11) . . ?
O1 C2 H2A 109.9 . . ?
C1 C2 H2A 109.9 . . ?
O1 C2 H2B 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
N2 C3 C4 124(2) . . ?
N2 C3 H3 117.8 . . ?
C4 C3 H3 117.8 . . ?
C3 C4 C5 114(2) . . ?
C3 C4 H4 123.1 . . ?
C5 C4 H4 123.1 . . ?
C6 C5 C4 121.8(19) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C5 C6 C7 121(2) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
N2 C7 C6 115.7(16) . . ?
N2 C7 C8 118.5(10) . . ?
C6 C7 C8 125.8(16) . . ?
O2 C8 O2 114.5(15) 18_554 . ?
O2 C8 C7 108.3(7) 18_554 . ?
O2 C8 C7 109.3(7) . . ?
O2 C8 C7 109.3(7) 18_554 18_554 ?
O2 C8 C7 108.3(7) . 18_554 ?
C7 C8 C7 106.7(19) . 18_554 ?
O1 Cu1 O2 82.8(4) . . ?
O1 Cu1 N2 164.9(5) . . ?
O2 Cu1 N2 82.5(5) . . ?
O1 Cu1 Cl1 98.3(3) . . ?
O2 Cu1 Cl1 178.9(3) . . ?
N2 Cu1 Cl1 96.5(4) . . ?
O1 Cu1 Dy1 40.9(2) . . ?
O2 Cu1 Dy1 42.6(2) . . ?
N2 Cu1 Dy1 124.0(4) . . ?
Cl1 Cu1 Dy1 138.53(14) . . ?
O1 Dy1 O1 108.3(2) . 2_655 ?
O1 Dy1 O1 108.3(2) . 3_665 ?
O1 Dy1 O1 108.3(2) 2_655 3_665 ?
O1 Dy1 O2 90.9(3) . 2_655 ?
O1 Dy1 O2 67.7(3) 2_655 2_655 ?
O1 Dy1 O2 160.4(3) 3_665 2_655 ?
O1 Dy1 O2 160.4(3) . 3_665 ?
O1 Dy1 O2 90.9(3) 2_655 3_665 ?
O1 Dy1 O2 67.7(3) 3_665 3_665 ?
O2 Dy1 O2 93.0(3) 2_655 3_665 ?
O1 Dy1 O2 67.7(3) . . ?
O1 Dy1 O2 160.4(3) 2_655 . ?
O1 Dy1 O2 90.9(3) 3_665 . ?
O2 Dy1 O2 93.0(3) 2_655 . ?
O2 Dy1 O2 93.0(3) 3_665 . ?
O1 Dy1 N1 69.37(19) . . ?
O1 Dy1 N1 69.36(19) 2_655 . ?
O1 Dy1 N1 69.36(19) 3_665 . ?
O2 Dy1 N1 123.1(2) 2_655 . ?
O2 Dy1 N1 123.1(2) 3_665 . ?
O2 Dy1 N1 123.1(2) . . ?
O1 Dy1 Cu1 106.0(2) . 2_655 ?
O1 Dy1 Cu1 33.2(2) 2_655 2_655 ?
O1 Dy1 Cu1 136.0(2) 3_665 2_655 ?
O2 Dy1 Cu1 35.0(2) 2_655 2_655 ?
O2 Dy1 Cu1 87.8(2) 3_665 2_655 ?
O2 Dy1 Cu1 127.8(2) . 2_655 ?
N1 Dy1 Cu1 98.55(3) . 2_655 ?
O1 Dy1 Cu1 33.2(2) . . ?
O1 Dy1 Cu1 136.0(2) 2_655 . ?
O1 Dy1 Cu1 106.0(2) 3_665 . ?
O2 Dy1 Cu1 87.8(3) 2_655 . ?
O2 Dy1 Cu1 127.8(2) 3_665 . ?
O2 Dy1 Cu1 35.0(2) . . ?
N1 Dy1 Cu1 98.55(3) . . ?
Cu1 Dy1 Cu1 117.830(16) 2_655 . ?
O1 Dy1 Cu1 136.0(2) . 3_665 ?
O1 Dy1 Cu1 106.0(2) 2_655 3_665 ?
O1 Dy1 Cu1 33.2(2) 3_665 3_665 ?
O2 Dy1 Cu1 127.8(2) 2_655 3_665 ?
O2 Dy1 Cu1 35.0(2) 3_665 3_665 ?
O2 Dy1 Cu1 87.8(2) . 3_665 ?
N1 Dy1 Cu1 98.55(3) . 3_665 ?
Cu1 Dy1 Cu1 117.830(16) 2_655 3_665 ?
Cu1 Dy1 Cu1 117.829(16) . 3_665 ?
C1 N1 C1 114.0(6) . 2_655 ?
C1 N1 C1 114.0(6) . 3_665 ?
C1 N1 C1 114.0(6) 2_655 3_665 ?
C1 N1 Dy1 104.4(8) . . ?
C1 N1 Dy1 104.4(8) 2_655 . ?
C1 N1 Dy1 104.4(8) 3_665 . ?
C3 N2 C7 122.8(15) . . ?
C3 N2 Cu1 126.4(14) . . ?
C7 N2 Cu1 110.8(9) . . ?
C2 O1 Cu1 125.5(8) . . ?
C2 O1 Dy1 124.4(8) . . ?
Cu1 O1 Dy1 105.9(3) . . ?
C8 O2 Cu1 117.2(7) . . ?
C8 O2 Dy1 140.4(7) . . ?
Cu1 O2 Dy1 102.4(4) . . ?
H3A O3 H3B 108.1 . . ?

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
N1 C1 C2 O1 44.0(16) . . . . ?
N2 C3 C4 C5 -9(4) . . . . ?
C3 C4 C5 C6 11(4) . . . . ?
C4 C5 C6 C7 -9(4) . . . . ?
C5 C6 C7 N2 5(3) . . . . ?
C5 C6 C7 C8 -177(2) . . . . ?
N2 C7 C8 O2 136.1(13) . . . 18_554 ?
C6 C7 C8 O2 -42(2) . . . 18_554 ?
N2 C7 C8 O2 10.7(19) . . . . ?
C6 C7 C8 O2 -167.0(17) . . . . ?
N2 C7 C8 C7 -106.3(14) . . . 18_554 ?
C6 C7 C8 C7 76.0(18) . . . 18_554 ?
C2 C1 N1 C1 -162.1(12) . . . 2_655 ?
C2 C1 N1 C1 64.7(19) . . . 3_665 ?
C2 C1 N1 Dy1 -48.7(11) . . . . ?
C4 C3 N2 C7 7(4) . . . . ?
C4 C3 N2 Cu1 -173(2) . . . . ?
C6 C7 N2 C3 -4(2) . . . . ?
C8 C7 N2 C3 178.3(17) . . . . ?
C6 C7 N2 Cu1 175.9(13) . . . . ?
C8 C7 N2 Cu1 -2.0(18) . . . . ?
C1 C2 O1 Cu1 -169.5(9) . . . . ?
C1 C2 O1 Dy1 -15.8(15) . . . . ?
O2 Cu1 O1 C2 148.6(10) . . . . ?
N2 Cu1 O1 C2 160.4(17) . . . . ?
Cl1 Cu1 O1 C2 -31.0(10) . . . . ?
Dy1 Cu1 O1 C2 157.6(12) . . . . ?
O2 Cu1 O1 Dy1 -9.0(4) . . . . ?
N2 Cu1 O1 Dy1 3(2) . . . . ?
Cl1 Cu1 O1 Dy1 171.3(3) . . . . ?
O2 C8 O2 Cu1 -136.4(8) 18_554 . . . ?
C7 C8 O2 Cu1 -14.7(14) . . . . ?
C7 C8 O2 Cu1 101.3(11) 18_554 . . . ?
O2 C8 O2 Dy1 43.1(9) 18_554 . . . ?
C7 C8 O2 Dy1 164.8(10) . . . . ?
C7 C8 O2 Dy1 -79.2(18) 18_554 . . . ?

_refine_diff_density_max         1.918
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.229



