# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_Tb6Zn6
_audit_block_doi                 10.5517/ccdc.csd.cc1nj4w6
_database_code_depnum_ccdc_archive 'CCDC 1534868'
_audit_update_record             
;
2017-02-26 deposited with the CCDC.
2018-01-03 downloaded from the CCDC.
;
_audit_creation_date             2017-02-26
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C126 H102 Cl12 N42 O30 Tb6 Zn6, 6(Cl1 O4), 31(O)'
_chemical_formula_sum            'C126 H163 Cl18 N42 O84 Tb6 Zn6'
_chemical_formula_weight         5593.81
_chemical_melting_point          ?
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'
Zn Zn 0.2839 1.4301 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'
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, -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'

_cell_length_a                   28.4167(7)
_cell_length_b                   28.4167(7)
_cell_length_c                   19.3922(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13561.4(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.24
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.313
_exptl_absorpt_correction_T_max  0.630
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi_scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       club
_exptl_crystal_F_000             5522
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1403
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            78703
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.097
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         0.83
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4486
_reflns_number_total             8023
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         2.572
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         8023
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.0838
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1709P)²+60.7791P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2403
_refine_ls_wR_factor_ref         0.2927
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H) groups, H17 of C17, H4 of C4, H10 of C10, All O(H) groups
 At 1.2 times of:
  H18 of C18, H12 of C12, H11 of C11, H19 of C19
2. Restrained distances
 Cl4-O8 = Cl4-O9
 1.44 with sigma of 0.02
 H1-H1A = H1-H1B
 2.19 with sigma of 0.01
3. Rigid bond restraints
 O8, Cl4, O9, Cl4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq,
Uanis(O15) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O16) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.12
5. Others
 Fixed Sof: Cl4(0.66667) O8(0.66667)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C14(H14),
 C17(H17), C18(H18), C19(H19)
6.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O4(H4A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.3019(7) 0.5362(6) 0.0941(6) 0.075(5) Uani 1 1 d . . . . .
H1A H 0.2671 0.5288 0.1125 0.113 Uiso 1 1 calc DR . . . .
H1B H 0.3259 0.5753 0.0936 0.113 Uiso 1 1 calc DR . . . .
C2 C 0.3256(5) 0.5105(5) 0.1401(8) 0.054(3) Uani 1 1 d . . . . .
C3 C 0.3422(6) 0.5290(5) 0.2047(8) 0.061(4) Uani 1 1 d . . . . .
H3 H 0.3398 0.5585 0.2210 0.04(3) Uiso 1 1 calc R . . . .
C4 C 0.3619(6) 0.5050(6) 0.2453(8) 0.066(4) Uani 1 1 d . . . . .
H4 H 0.3708 0.5159 0.2909 0.099 Uiso 1 1 calc R . . . .
C5 C 0.3692(6) 0.4636(6) 0.2187(9) 0.068(4) Uani 1 1 d . . . . .
H5 H 0.3842 0.4472 0.2454 0.07(4) Uiso 1 1 calc R . . . .
C6 C 0.3531(5) 0.4474(5) 0.1502(8) 0.056(4) Uani 1 1 d . . . . .
C7 C 0.3616(6) 0.4071(7) 0.1164(9) 0.078(5) Uani 1 1 d . . . . .
H7 H 0.3784 0.3903 0.1383 0.08(5) Uiso 1 1 calc R . . . .
C8 C 0.3971(6) 0.5057(8) -0.1053(10) 0.088(6) Uani 1 1 d . . . . .
H8A H 0.4104 0.4815 -0.1182 0.07(4) Uiso 1 1 calc R . . . .
H8B H 0.4262 0.5428 -0.1121 0.15(8) Uiso 1 1 calc R . . . .
C9 C 0.3506(5) 0.4950(5) -0.1484(9) 0.060(4) Uani 1 1 d . . . . .
C10 C 0.3582(6) 0.5096(7) -0.2196(11) 0.085(5) Uani 1 1 d . . . . .
H10 H 0.3927 0.5275 -0.2389 0.128 Uiso 1 1 calc R . . . .
C11 C 0.3132(7) 0.4966(8) -0.2586(9) 0.093(6) Uani 1 1 d . . . . .
H11 H 0.3166 0.5055 -0.3051 0.112 Uiso 1 1 calc R . . . .
C12 C 0.2629(6) 0.4702(7) -0.2278(9) 0.081(5) Uani 1 1 d . . . . .
H12 H 0.2319 0.4599 -0.2541 0.097 Uiso 1 1 calc R . . . .
C13 C 0.2585(5) 0.4592(6) -0.1601(8) 0.058(4) Uani 1 1 d . . . . .
C14 C 0.2064(5) 0.4326(6) -0.1233(8) 0.061(4) Uani 1 1 d . . . . .
H14 H 0.1740 0.4229 -0.1459 0.05(3) Uiso 1 1 calc R . . . .
C15 C 0.1690(5) 0.3971(6) 0.0433(8) 0.065(4) Uani 1 1 d . . . . .
C16 C 0.1222(6) 0.3805(8) 0.0892(10) 0.098(6) Uani 1 1 d . . . . .
C17 C 0.1224(8) 0.3697(9) 0.1595(10) 0.106(6) Uani 1 1 d . U . . .
H17 H 0.1522 0.3714 0.1815 0.159 Uiso 1 1 calc R . . . .
C18 C 0.0754(11) 0.3566(12) 0.1932(14) 0.155(10) Uani 1 1 d . U . . .
H18 H 0.0749 0.3544 0.2411 0.186 Uiso 1 1 calc R . . . .
C19 C 0.0286(9) 0.3464(10) 0.1594(11) 0.117(7) Uani 1 1 d . U . . .
H19 H -0.0036 0.3354 0.1833 0.141 Uiso 1 1 calc R . . . .
C20 C 0.0312(6) 0.3527(7) 0.0916(8) 0.081(5) Uani 1 1 d . U . . .
C21 C -0.0174(5) 0.3416(7) 0.0469(9) 0.083(5) Uani 1 1 d . . . . .
Cl1 Cl 0.0621(2) 0.3305(3) -0.1421(3) 0.127(2) Uani 1 1 d . . . . .
Cl2 Cl 0.10142(15) 0.47050(16) -0.0781(2) 0.0794(12) Uani 1 1 d . . . . .
Cl3 Cl 0.3333 0.6667 0.1981(4) 0.0588(15) Uani 1 3 d S T P . .
Cl4 Cl 0.5134(3) 0.5273(4) 0.2214(5) 0.118(3) Uani 0.6667 1 d D U . . .
Tb1 Tb 0.28987(2) 0.43094(2) -0.00333(4) 0.0483(3) Uani 1 1 d . . . . .
N1 N 0.3297(4) 0.4697(4) 0.1111(5) 0.046(2) Uani 1 1 d . . . . .
N2 N 0.3441(5) 0.3959(5) 0.0535(6) 0.058(3) Uani 1 1 d . . . . .
N3 N 0.3015(4) 0.4705(3) -0.1194(6) 0.047(3) Uani 1 1 d . . . . .
N4 N 0.2074(4) 0.4231(4) -0.0585(6) 0.046(2) Uani 1 1 d . . . . .
N5 N 0.1599(4) 0.4028(4) -0.0233(6) 0.053(3) Uani 1 1 d . . . . .
N6 N 0.0765(4) 0.3675(6) 0.0552(6) 0.071(4) Uani 1 1 d . . . . .
N8 N -0.0049(4) 0.3553(5) -0.0171(6) 0.066(3) Uani 1 1 d . . . . .
O1 O 0.2946(4) 0.5160(4) 0.0255(5) 0.064(3) Uani 1 1 d . . . . .
H1 H 0.2818 0.5307 0.0017 0.096 Uiso 1 1 calc DGR . . . .
O2 O -0.0641(3) 0.3209(5) 0.0767(6) 0.092(4) Uani 1 1 d . . . . .
O3 O 0.2145(3) 0.4086(4) 0.0706(5) 0.071(3) Uani 1 1 d . . . . .
O4 O 0.3813(3) 0.4976(5) -0.0348(6) 0.079(3) Uani 1 1 d . . . . .
H4A H 0.4063 0.4999 -0.0113 0.119 Uiso 1 1 calc GR . . . .
O5 O 0.2278(5) 0.3347(4) -0.0058(8) 0.115(5) Uani 1 1 d . . . . .
O6 O 0.3333 0.6667 0.1269(13) 0.112(7) Uani 1 3 d S T P . .
O7 O 0.3319(4) 0.7136(4) 0.2161(7) 0.091(4) Uani 1 1 d . . . . .
O8 O 0.5069(14) 0.5605(11) 0.1676(13) 0.188(10) Uani 0.6667 1 d D U . . .
O9 O 0.4813(7) 0.5118(7) 0.2916(8) 0.156(5) Uani 1 1 d D U . . .
O10 O 0.5719(13) 0.5516(12) 0.2269(16) 0.270(14) Uani 1 1 d . U . . .
O11 O 0.1781(13) 0.5279(13) 0.0525(13) 0.295(14) Uani 1 1 d . U . . .
O12 O 0.1319(15) 0.2660(15) 0.0439(15) 0.320(15) Uani 1 1 d . U . . .
O13 O 0.886(2) 0.1782(19) 0.175(2) 0.44(3) Uani 1 1 d . U . . .
O14 O 0.4615(10) 0.5077(11) 0.0490(12) 0.236(10) Uani 1 1 d . U . . .
O15 O 0.2124(18) 0.3063(18) 0.190(2) 0.39(2) Uani 1 1 d . U . . .
Zn1 Zn 0.07831(5) 0.38434(7) -0.04883(9) 0.0565(5) Uani 1 1 d . . . . .
O16 O 0.0000 0.0000 0.0000 0.57(8) Uani 1 6 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 1.510(18) . ?
C1 O1 1.421(7) . ?
C2 C3 1.349(19) . ?
C2 N1 1.344(15) . ?
C3 C4 1.334(19) . ?
C4 C5 1.391(19) . ?
C5 C6 1.41(2) . ?
C6 C7 1.441(18) . ?
C6 N1 1.356(16) . ?
C7 N2 1.296(18) . ?
C8 C9 1.46(2) . ?
C8 O4 1.420(19) . ?
C9 C10 1.43(2) . ?
C9 N3 1.332(16) . ?
C10 C11 1.37(2) . ?
C11 C12 1.37(2) . ?
C12 C13 1.34(2) . ?
C13 C14 1.466(18) . ?
C13 N3 1.351(16) . ?
C14 N4 1.289(16) . ?
C15 C16 1.47(2) . ?
C15 N5 1.343(17) . ?
C15 O3 1.279(15) . ?
C16 C17 1.40(2) . ?
C16 N6 1.334(17) . ?
C17 C18 1.36(3) . ?
C18 C19 1.38(3) . ?
C19 C20 1.32(2) . ?
C20 C21 1.52(2) . ?
C20 N6 1.339(18) . ?
C21 N8 1.295(18) . ?
C21 O2 1.290(16) . ?
Cl1 Zn1 2.263(5) . ?
Cl2 Zn1 2.267(4) . ?
Cl3 O6 1.38(2) . ?
Cl3 O7 1.398(9) 2_665 ?
Cl3 O7 1.398(9) . ?
Cl3 O7 1.398(9) 3_565 ?
Cl4 Cl4 1.301(18) 4 ?
Cl4 O8 1.479(17) . ?
Cl4 O9 1.308(15) 4 ?
Cl4 O9 1.574(14) . ?
Cl4 O10 1.45(3) . ?
Cl4 O10 1.55(3) 4 ?
Tb1 N1 2.484(10) . ?
Tb1 N2 2.473(10) . ?
Tb1 N3 2.464(11) . ?
Tb1 N4 2.482(10) . ?
Tb1 O1 2.419(9) . ?
Tb1 O2 2.378(10) 8 ?
Tb1 O3 2.384(9) . ?
Tb1 O4 2.406(10) . ?
Tb1 O5 2.401(11) . ?
N2 N8 1.397(14) 8 ?
N4 N5 1.358(13) . ?
N5 Zn1 2.163(9) . ?
N6 Zn1 2.069(11) . ?
N8 N2 1.397(14) 9 ?
N8 Zn1 2.168(11) . ?
O2 Tb1 2.378(10) 9 ?
O9 Cl4 1.308(15) 4 ?
O10 Cl4 1.55(3) 4 ?
O10 O10 1.34(5) 4 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 111.6(10) . . ?
C3 C2 C1 120.9(12) . . ?
N1 C2 C1 114.9(12) . . ?
N1 C2 C3 124.2(13) . . ?
C4 C3 C2 120.2(13) . . ?
C3 C4 C5 119.5(15) . . ?
C4 C5 C6 117.7(14) . . ?
C5 C6 C7 122.2(13) . . ?
N1 C6 C5 122.1(12) . . ?
N1 C6 C7 115.7(13) . . ?
N2 C7 C6 115.3(13) . . ?
O4 C8 C9 109.7(12) . . ?
C10 C9 C8 120.3(14) . . ?
N3 C9 C8 117.9(15) . . ?
N3 C9 C10 121.8(13) . . ?
C11 C10 C9 118.2(15) . . ?
C10 C11 C12 118.9(16) . . ?
C13 C12 C11 120.1(15) . . ?
C12 C13 C14 123.3(13) . . ?
C12 C13 N3 123.2(13) . . ?
N3 C13 C14 113.5(13) . . ?
N4 C14 C13 117.4(12) . . ?
N5 C15 C16 115.0(11) . . ?
O3 C15 C16 117.9(14) . . ?
O3 C15 N5 126.8(12) . . ?
C17 C16 C15 124.0(15) . . ?
N6 C16 C15 112.9(15) . . ?
N6 C16 C17 122.1(15) . . ?
C18 C17 C16 115(2) . . ?
C17 C18 C19 123(2) . . ?
C20 C19 C18 118(2) . . ?
C19 C20 C21 123.8(16) . . ?
C19 C20 N6 123.0(15) . . ?
N6 C20 C21 113.2(13) . . ?
N8 C21 C20 113.6(12) . . ?
O2 C21 C20 117.3(14) . . ?
O2 C21 N8 129.1(13) . . ?
O6 Cl3 O7 104.4(6) . . ?
O6 Cl3 O7 104.4(6) . 2_665 ?
O6 Cl3 O7 104.4(6) . 3_565 ?
O7 Cl3 O7 114.0(5) . 3_565 ?
O7 Cl3 O7 114.0(5) 2_665 3_565 ?
O7 Cl3 O7 114.0(5) . 2_665 ?
Cl4 Cl4 O8 161.3(14) 4 . ?
Cl4 Cl4 O9 74.2(9) 4 4 ?
Cl4 Cl4 O9 53.1(8) 4 . ?
Cl4 Cl4 O10 68.5(14) 4 . ?
Cl4 Cl4 O10 60.2(13) 4 4 ?
O8 Cl4 O9 123.3(15) . . ?
O8 Cl4 O10 101.2(18) . 4 ?
O9 Cl4 O8 123.2(16) 4 . ?
O9 Cl4 O9 99.2(13) 4 . ?
O9 Cl4 O10 127.0(17) 4 4 ?
O9 Cl4 O10 87.2(14) 4 . ?
O10 Cl4 O8 103(2) . . ?
O10 Cl4 O9 115.9(16) . . ?
O10 Cl4 O9 75.0(12) 4 . ?
O10 Cl4 O10 53(2) . 4 ?
N2 Tb1 N1 62.8(3) . . ?
N2 Tb1 N4 155.0(4) . . ?
N3 Tb1 N1 133.3(3) . . ?
N3 Tb1 N2 128.5(3) . . ?
N3 Tb1 N4 63.4(3) . . ?
N4 Tb1 N1 128.7(3) . . ?
O1 Tb1 N1 64.2(3) . . ?
O1 Tb1 N2 124.4(3) . . ?
O1 Tb1 N3 80.1(3) . . ?
O1 Tb1 N4 76.6(3) . . ?
O2 Tb1 N1 124.4(3) 8 . ?
O2 Tb1 N2 64.4(3) 8 . ?
O2 Tb1 N3 72.7(3) 8 . ?
O2 Tb1 N4 106.6(3) 8 . ?
O2 Tb1 O1 146.7(4) 8 . ?
O2 Tb1 O3 138.0(4) 8 . ?
O2 Tb1 O4 74.3(4) 8 . ?
O2 Tb1 O5 68.1(5) 8 . ?
O3 Tb1 N1 74.4(3) . . ?
O3 Tb1 N2 106.4(4) . . ?
O3 Tb1 N3 124.7(3) . . ?
O3 Tb1 N4 63.5(3) . . ?
O3 Tb1 O1 73.8(3) . . ?
O3 Tb1 O4 146.6(4) . . ?
O3 Tb1 O5 70.0(5) . . ?
O4 Tb1 N1 78.7(3) . . ?
O4 Tb1 N2 77.5(4) . . ?
O4 Tb1 N3 64.1(3) . . ?
O4 Tb1 N4 124.1(4) . . ?
O4 Tb1 O1 76.9(4) . . ?
O5 Tb1 N1 115.8(4) . . ?
O5 Tb1 N2 78.6(4) . . ?
O5 Tb1 N3 110.9(4) . . ?
O5 Tb1 N4 76.5(3) . . ?
O5 Tb1 O1 141.7(4) . . ?
O5 Tb1 O4 141.3(5) . . ?
C2 N1 C6 116.2(12) . . ?
C2 N1 Tb1 122.7(9) . . ?
C6 N1 Tb1 120.9(8) . . ?
C7 N2 Tb1 124.1(9) . . ?
C7 N2 N8 117.1(10) . 8 ?
N8 N2 Tb1 118.8(8) 8 . ?
C9 N3 C13 117.7(12) . . ?
C9 N3 Tb1 119.4(9) . . ?
C13 N3 Tb1 121.7(8) . . ?
C14 N4 Tb1 121.4(8) . . ?
C14 N4 N5 117.2(10) . . ?
N5 N4 Tb1 121.0(8) . . ?
C15 N5 N4 108.9(9) . . ?
C15 N5 Zn1 116.0(8) . . ?
N4 N5 Zn1 134.9(8) . . ?
C16 N6 C20 118.5(13) . . ?
C16 N6 Zn1 120.7(10) . . ?
C20 N6 Zn1 119.7(9) . . ?
C21 N8 N2 109.2(11) . 9 ?
C21 N8 Zn1 117.9(9) . . ?
N2 N8 Zn1 132.7(9) 9 . ?
C1 O1 Tb1 123.0(7) . . ?
C21 O2 Tb1 116.6(10) . 9 ?
C15 O3 Tb1 118.5(9) . . ?
C8 O4 Tb1 120.1(8) . . ?
Cl4 O9 Cl4 52.7(9) 4 . ?
Cl4 O10 Cl4 51.2(12) . 4 ?
O10 O10 Cl4 59.5(14) 4 4 ?
O10 O10 Cl4 67.5(17) 4 . ?
Cl1 Zn1 Cl2 112.4(2) . . ?
N5 Zn1 Cl1 100.3(3) . . ?
N5 Zn1 Cl2 95.7(3) . . ?
N5 Zn1 N8 149.3(4) . . ?
N6 Zn1 Cl1 130.6(5) . . ?
N6 Zn1 Cl2 117.1(4) . . ?
N6 Zn1 N5 74.5(4) . . ?
N6 Zn1 N8 74.9(4) . . ?
N8 Zn1 Cl1 98.9(4) . . ?
N8 Zn1 Cl2 98.9(3) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.363 2993.7 1142.7 ?
2 0.000 0.356 0.750 7.3 0.0 ?
3 0.000 0.644 0.250 7.3 0.0 ?
4 0.333 0.667 0.906 214.5 0.0 ?
5 0.333 0.667 0.406 214.5 0.0 ?
6 0.356 0.356 0.250 7.3 0.0 ?
7 0.356 1.000 0.750 7.3 0.0 ?
8 0.667 0.333 0.594 214.5 0.0 ?
9 0.667 0.333 0.094 214.5 0.0 ?
10 0.644 0.644 0.750 7.3 0.0 ?
11 0.644 1.000 0.250 7.3 0.0 ?


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Tb6Cu6
_audit_block_doi                 10.5517/ccdc.csd.cc1nj4x7
_database_code_depnum_ccdc_archive 'CCDC 1534869'
_audit_update_record             
;
2017-02-26 deposited with the CCDC.
2018-01-03 downloaded from the CCDC.
;
_audit_creation_date             2016-12-23
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5273)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C126 H102 Cl12 Cu6 N42 O30 Tb6, 5(Cl1 O4), 1(O)'
_chemical_formula_sum            'C126 H115 Cl17 Cu6 N42 O51 Tb6'
_chemical_formula_weight         4971.00
_chemical_melting_point          ?
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'
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'
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, -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'

_cell_length_a                   28.1810(11)
_cell_length_b                   28.1810(11)
_cell_length_c                   20.0915(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13818.3(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.81
_cell_measurement_theta_min      2.19
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.186
_exptl_absorpt_correction_T_max  0.632
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   multi_scan
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       club
_exptl_crystal_F_000             4852
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1216
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            87453
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.11
_diffrn_reflns_theta_min         0.83
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5269
_reflns_number_total             9146
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         1.958
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         9146
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0714
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1531P)²+23.4291P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2162
_refine_ls_wR_factor_ref         0.2606
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 Cl3-O6 = Cl3-O7 = Cl4-O8 = Cl4-O9
 1.4 with sigma of 0.02
 H1-H1A = H1-H1B = H3A-H21A = H3A-H21B
 2.1 with sigma of 0.01
 O1-H1 = O3-H3A
 0.82 with sigma of 0.01
 O6-O7 = O8-O9
 2.32 with sigma of 0.01
3. Rigid bond restraints
 O7, Cl3, O8, Cl4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O9) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C15(H15),
 C17(H17), C18(H18), C19(H19)
5.c Fitted hexagon refined as free rotating group:
 N1(C2,C3,C4,C5,C6), N4(C9,C10,C11,C12,C13), N7(C16,C17,C18,C19,C20)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.1129(5) 0.5091(6) 0.6044(4) 0.079(3) Uani 1 1 d . . . . .
H1A H 0.0752 0.4875 0.6190 0.095 Uiso 1 1 calc DR . . . .
H1B H 0.1237 0.5474 0.6090 0.095 Uiso 1 1 calc DR . . . .
N1 N 0.1708(2) 0.4688(3) 0.6168(2) 0.0535(19) Uani 1 1 d . . . . .
C2 C 0.1483(3) 0.4969(3) 0.6483(3) 0.071(3) Uani 1 1 d G . . . .
C3 C 0.1597(3) 0.5113(3) 0.7150(4) 0.089(4) Uani 1 1 d G . . . .
H3 H 0.1447 0.5301 0.7360 0.107 Uiso 1 1 calc R . . . .
C4 C 0.1936(4) 0.4975(4) 0.7502(3) 0.104(5) Uani 1 1 d G . . . .
H4 H 0.2012 0.5072 0.7948 0.124 Uiso 1 1 calc R . . . .
C5 C 0.2160(3) 0.4694(4) 0.7187(3) 0.097(5) Uani 1 1 d G . . . .
H5 H 0.2387 0.4602 0.7423 0.117 Uiso 1 1 calc R . . . .
C6 C 0.2046(3) 0.4550(3) 0.6520(3) 0.062(3) Uani 1 1 d G . . . .
C7 C 0.2278(4) 0.4298(4) 0.6154(5) 0.061(3) Uani 1 1 d . . . . .
H7 H 0.2518 0.4204 0.6351 0.073 Uiso 1 1 calc R . . . .
C8 C 0.2239(4) 0.3949(4) 0.4502(5) 0.056(2) Uani 1 1 d . . . . .
N4 N 0.2893(3) 0.3681(3) 0.4381(2) 0.064(2) Uani 1 1 d . . . . .
C9 C 0.2513(3) 0.3778(3) 0.4057(3) 0.066(3) Uani 1 1 d G . . . .
C10 C 0.2447(3) 0.3709(4) 0.3372(3) 0.095(4) Uani 1 1 d G . . . .
H10 H 0.2193 0.3774 0.3155 0.114 Uiso 1 1 calc R . . . .
C11 C 0.2760(4) 0.3544(5) 0.3011(2) 0.131(7) Uani 1 1 d G . . . .
H11 H 0.2716 0.3498 0.2552 0.157 Uiso 1 1 calc R . . . .
C12 C 0.3139(4) 0.3447(5) 0.3335(3) 0.102(5) Uani 1 1 d G . . . .
H12 H 0.3349 0.3337 0.3094 0.122 Uiso 1 1 calc R . . . .
C13 C 0.3206(3) 0.3516(4) 0.4020(3) 0.073(3) Uani 1 1 d G . . . .
C14 C 0.0143(4) 0.3570(5) 0.5549(6) 0.066(3) Uani 1 1 d . . . . .
C15 C 0.0380(4) 0.4012(5) 0.3927(6) 0.073(3) Uani 1 1 d . . . . .
H15 H 0.0037 0.3827 0.3725 0.088 Uiso 1 1 calc R . . . .
N7 N 0.1323(2) 0.4668(3) 0.3953(3) 0.059(2) Uani 1 1 d . . . . .
C16 C 0.0841(2) 0.4405(3) 0.3585(3) 0.067(3) Uani 1 1 d G . . . .
C17 C 0.0832(3) 0.4563(3) 0.2932(3) 0.090(4) Uani 1 1 d G . . . .
H17 H 0.0510 0.4387 0.2686 0.108 Uiso 1 1 calc R . . . .
C18 C 0.1305(3) 0.4985(3) 0.2647(3) 0.093(4) Uani 1 1 d G . . . .
H18 H 0.1299 0.5090 0.2210 0.112 Uiso 1 1 calc R . . . .
C19 C 0.1787(3) 0.5248(3) 0.3014(4) 0.087(4) Uani 1 1 d G . . . .
H19 H 0.2103 0.5530 0.2823 0.104 Uiso 1 1 calc R . . . .
C20 C 0.1796(2) 0.5090(3) 0.3667(3) 0.066(3) Uani 1 1 d G . . . .
C21 C 0.2293(5) 0.5337(6) 0.4095(5) 0.092(4) Uani 1 1 d . . . . .
H21A H 0.2559 0.5252 0.3909 0.110 Uiso 1 1 calc DR . . . .
H21B H 0.2454 0.5732 0.4092 0.110 Uiso 1 1 calc DR . . . .
Cl1 Cl 0.36243(13) 0.46704(14) 0.5794(2) 0.0930(11) Uani 1 1 d . . . . .
Cl2 Cl 0.2626(2) 0.3253(2) 0.6243(2) 0.145(2) Uani 1 1 d . . . . .
Cu2 Cu 0.30031(5) 0.38024(6) 0.53155(6) 0.0605(4) Uani 1 1 d . . . . .
N2 N 0.2149(3) 0.4198(3) 0.5535(4) 0.058(2) Uani 1 1 d . . . . .
N3 N 0.2398(4) 0.3987(4) 0.5132(4) 0.063(2) Uani 1 1 d . . . . .
N5 N -0.0005(3) 0.3554(3) 0.4920(4) 0.058(2) Uani 1 1 d . . . . .
N6 N 0.0451(3) 0.3916(4) 0.4536(5) 0.063(2) Uani 1 1 d . . . . .
O1 O 0.1161(3) 0.4981(3) 0.5397(4) 0.071(2) Uani 1 1 d D . . . .
H1 H 0.0961 0.5054 0.5176 0.107 Uiso 1 1 calc DGR . . . .
O2 O 0.1886(3) 0.4057(3) 0.4297(3) 0.067(2) Uani 1 1 d . . . . .
O3 O 0.2187(3) 0.5157(3) 0.4732(4) 0.073(2) Uani 1 1 d D . . . .
H3A H 0.2472 0.5304 0.4947 0.110 Uiso 1 1 calc DGR . . . .
O4 O 0.0613(3) 0.3844(3) 0.5795(3) 0.069(2) Uani 1 1 d . . . . .
O5 O 0.1027(4) 0.3297(4) 0.5037(6) 0.111(3) Uani 1 1 d . . . . .
Tb1 Tb 0.13795(2) 0.42937(2) 0.50482(2) 0.0526(2) Uani 1 1 d . . . . .
Cl3 Cl 0.3333 0.6667 0.2967(5) 0.121(2) Uani 1 3 d DS TU P . .
Cl4 Cl 1.0000 0.5289(3) 0.2500 0.178(4) Uani 1 2 d DS TU P . .
O9 O 0.9701(6) 0.4853(5) 0.2911(7) 0.194(7) Uani 1 1 d D U . . .
O6 O 0.3816(6) 0.7169(6) 0.2872(8) 0.228(8) Uani 1 1 d D U . . .
O7 O 0.3333 0.6667 0.3752(8) 0.303(12) Uani 1 3 d DS TU P . .
O8 O 0.9711(11) 0.5495(10) 0.2195(14) 0.395(16) Uani 1 1 d D U . . .
O10 O 0.0000 0.0000 0.5000 0.47(6) Uani 1 6 d S T 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 1.493(12) . ?
C1 O1 1.350(7) . ?
N1 C2 1.3900 . ?
N1 C6 1.3900 . ?
N1 Tb1 2.475(5) . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.390(11) . ?
C7 N2 1.288(12) . ?
C8 C9 1.415(10) . ?
C8 N3 1.330(12) . ?
C8 O2 1.246(10) . ?
N4 C9 1.3900 . ?
N4 C13 1.3900 . ?
N4 Cu2 1.905(5) . ?
C9 C10 1.3900 . ?
C10 C11 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.456(11) 8_556 ?
C14 C13 1.46(4) 9_556 ?
C14 N5 1.325(13) . ?
C14 O4 1.253(11) . ?
C15 C16 1.396(12) . ?
C15 N6 1.289(13) . ?
N7 C16 1.3900 . ?
N7 C20 1.3900 . ?
N7 Tb1 2.480(5) . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C19 C20 1.3900 . ?
C20 C21 1.487(12) . ?
C21 O3 1.353(7) . ?
Cl1 Cu2 2.385(3) . ?
Cl2 Cu2 2.313(4) . ?
Cu2 N3 2.050(7) . ?
Cu2 N5 2.042(8) 8_556 ?
N2 N3 1.386(10) . ?
N2 Tb1 2.513(8) . ?
N5 Cu2 2.042(8) 9_556 ?
N5 N6 1.405(11) . ?
N6 Tb1 2.501(8) . ?
O1 Tb1 2.412(7) . ?
O2 Tb1 2.390(6) . ?
O3 Tb1 2.443(7) . ?
O4 Tb1 2.405(7) . ?
O5 Tb1 2.467(9) . ?
Cl3 O6 1.402(12) . ?
Cl3 O6 1.402(12) 2_665 ?
Cl3 O6 1.402(12) 3_565 ?
Cl3 O7 1.577(16) . ?
Cl4 O9 1.367(11) 6_765 ?
Cl4 O9 1.367(11) . ?
Cl4 O8 1.360(14) 6_765 ?
Cl4 O8 1.360(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 112.9(8) . . ?
C2 N1 C6 120.0 . . ?
C2 N1 Tb1 119.7(3) . . ?
C6 N1 Tb1 119.5(3) . . ?
N1 C2 C1 114.2(6) . . ?
N1 C2 C3 120.0 . . ?
C3 C2 C1 125.8(6) . . ?
C4 C3 C2 120.0 . . ?
C3 C4 C5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C5 C6 N1 120.0 . . ?
C7 C6 N1 115.9(6) . . ?
C7 C6 C5 124.0(6) . . ?
N2 C7 C6 118.0(9) . . ?
N3 C8 C9 114.2(7) . . ?
O2 C8 C9 120.9(9) . . ?
O2 C8 N3 124.9(9) . . ?
C9 N4 C13 120.0 . . ?
C9 N4 Cu2 120.0(3) . . ?
C13 N4 Cu2 120.0(3) . . ?
N4 C9 C8 112.0(6) . . ?
N4 C9 C10 120.0 . . ?
C10 C9 C8 128.0(6) . . ?
C9 C10 C11 120.0 . . ?
C10 C11 C12 120.0 . . ?
C13 C12 C11 120.0 . . ?
N4 C13 C14 111.6(6) . 8_556 ?
C12 C13 N4 120.0 . . ?
C12 C13 C14 128.4(6) . 8_556 ?
N5 C14 C13 113.1(14) . 9_556 ?
O4 C14 C13 119.0(15) . 9_556 ?
O4 C14 N5 127.8(10) . . ?
N6 C15 C16 116.9(9) . . ?
C16 N7 C20 120.0 . . ?
C16 N7 Tb1 119.9(3) . . ?
C20 N7 Tb1 119.4(3) . . ?
N7 C16 C15 115.8(6) . . ?
C17 C16 C15 124.1(6) . . ?
C17 C16 N7 120.0 . . ?
C16 C17 C18 120.0 . . ?
C19 C18 C17 120.0 . . ?
C20 C19 C18 120.0 . . ?
N7 C20 C21 116.0(6) . . ?
C19 C20 N7 120.0 . . ?
C19 C20 C21 124.0(6) . . ?
O3 C21 C20 113.0(9) . . ?
N4 Cu2 Cl1 123.4(3) . . ?
N4 Cu2 Cl2 134.0(3) . . ?
N4 Cu2 N3 77.6(3) . . ?
N4 Cu2 N5 78.2(3) . 8_556 ?
Cl2 Cu2 Cl1 102.58(19) . . ?
N3 Cu2 Cl1 95.1(3) . . ?
N3 Cu2 Cl2 98.8(3) . . ?
N5 Cu2 Cl1 98.4(3) 8_556 . ?
N5 Cu2 Cl2 97.7(3) 8_556 . ?
N5 Cu2 N3 155.8(3) 8_556 . ?
C7 N2 N3 120.7(8) . . ?
C7 N2 Tb1 121.1(6) . . ?
N3 N2 Tb1 117.9(6) . . ?
C8 N3 Cu2 116.1(6) . . ?
C8 N3 N2 111.6(7) . . ?
N2 N3 Cu2 131.9(6) . . ?
C14 N5 Cu2 116.9(7) . 9_556 ?
C14 N5 N6 110.0(8) . . ?
N6 N5 Cu2 133.0(6) . 9_556 ?
C15 N6 N5 119.5(8) . . ?
C15 N6 Tb1 122.7(7) . . ?
N5 N6 Tb1 117.7(6) . . ?
C1 O1 Tb1 122.4(6) . . ?
C8 O2 Tb1 121.4(6) . . ?
C21 O3 Tb1 122.7(7) . . ?
C14 O4 Tb1 118.3(7) . . ?
N1 Tb1 N7 134.8(2) . . ?
N1 Tb1 N2 62.9(2) . . ?
N1 Tb1 N6 129.9(3) . . ?
N7 Tb1 N2 129.3(2) . . ?
N7 Tb1 N6 62.6(2) . . ?
N6 Tb1 N2 152.9(3) . . ?
O1 Tb1 N1 64.1(2) . . ?
O1 Tb1 N7 79.6(2) . . ?
O1 Tb1 N2 123.6(3) . . ?
O1 Tb1 N6 80.1(3) . . ?
O1 Tb1 O3 76.1(3) . . ?
O1 Tb1 O5 142.9(3) . . ?
O2 Tb1 N1 123.9(2) . . ?
O2 Tb1 N7 74.5(2) . . ?
O2 Tb1 N2 63.1(3) . . ?
O2 Tb1 N6 105.4(3) . . ?
O2 Tb1 O1 146.7(3) . . ?
O2 Tb1 O3 74.1(3) . . ?
O2 Tb1 O4 138.7(3) . . ?
O2 Tb1 O5 68.5(3) . . ?
O3 Tb1 N1 80.6(2) . . ?
O3 Tb1 N7 64.6(2) . . ?
O3 Tb1 N2 77.5(3) . . ?
O3 Tb1 N6 124.9(3) . . ?
O3 Tb1 O5 140.9(3) . . ?
O4 Tb1 N1 72.8(2) . . ?
O4 Tb1 N7 123.1(2) . . ?
O4 Tb1 N2 107.3(3) . . ?
O4 Tb1 N6 63.8(3) . . ?
O4 Tb1 O1 73.7(3) . . ?
O4 Tb1 O3 146.2(3) . . ?
O4 Tb1 O5 70.2(3) . . ?
O5 Tb1 N1 111.5(3) . . ?
O5 Tb1 N7 113.7(3) . . ?
O5 Tb1 N2 76.1(3) . . ?
O5 Tb1 N6 76.8(3) . . ?
O6 Cl3 O6 118.2(3) 2_665 . ?
O6 Cl3 O6 118.2(3) 2_665 3_565 ?
O6 Cl3 O6 118.2(4) . 3_565 ?
O6 Cl3 O7 97.8(8) 2_665 . ?
O6 Cl3 O7 97.8(8) . . ?
O6 Cl3 O7 97.8(8) 3_565 . ?
O9 Cl4 O9 107.4(13) . 6_765 ?
O8 Cl4 O9 115.2(11) 6_765 6_765 ?
O8 Cl4 O9 115.2(11) . . ?
O8 Cl4 O9 115.8(15) . 6_765 ?
O8 Cl4 O9 115.8(15) 6_765 . ?
O8 Cl4 O8 87(3) 6_765 . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.372 4466.1 1443.8 ?
2 -0.904 -0.082 0.500 1087.9 0.0 ?
3 -0.459 -0.927 0.000 1087.9 0.0 ?


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Dy6Zn6
_audit_block_doi                 10.5517/ccdc.csd.cc1nj4y8
_database_code_depnum_ccdc_archive 'CCDC 1534870'
_audit_update_record             
;
2017-02-26 deposited with the CCDC.
2018-01-03 downloaded from the CCDC.
;
_audit_creation_date             2017-02-26
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C126 H102 Cl12 Dy6 N42 O30 Zn6, 6(Cl1 O4), 31(O)'
_chemical_formula_sum            'C126 H163 Cl18 Dy6 N42 O84 Zn6'
_chemical_formula_weight         5615.29
_chemical_melting_point          ?
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'
Zn Zn 0.2839 1.4301 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'
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, -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'

_cell_length_a                   28.4167(7)
_cell_length_b                   28.4167(7)
_cell_length_c                   19.3922(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13561.4(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9364
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.47
_cell_measurement_theta_min      2.19
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.402
_exptl_absorpt_correction_T_max  0.619
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   multi_scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       club
_exptl_crystal_F_000             5534
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            85888
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         0.83
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5973
_reflns_number_total             8951
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         2.208
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         8951
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0710
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1329P)²+104.9525P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2055
_refine_ls_wR_factor_ref         0.2406
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H) groups, H4 of C4, H17 of C17, H10 of C10, All O(H) groups
 At 1.2 times of:
  H12 of C12, H18 of C18, H19 of C19, H11 of C11
2. Restrained distances
 Cl4-O8 = Cl4-O9
 1.44 with sigma of 0.02
 H1-H1A = H1-H1B
 2.19 with sigma of 0.01
3. Rigid bond restraints
 O8, Cl4, O9, Cl4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O15) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O16) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.12
5. Others
 Fixed Sof: Cl4(0.66667) O8(0.66667)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C14(H14),
 C17(H17), C18(H18), C19(H19)
6.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O4(H4A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.3007(5) 0.5349(5) 0.0917(4) 0.064(3) Uani 1 1 d . . . . .
H1A H 0.2654 0.5265 0.1096 0.096 Uiso 1 1 calc DR . . . .
H1B H 0.3238 0.5742 0.0916 0.096 Uiso 1 1 calc DR . . . .
C2 C 0.3249(4) 0.5107(4) 0.1378(6) 0.046(2) Uani 1 1 d . . . . .
C3 C 0.3408(4) 0.5288(4) 0.2043(6) 0.051(3) Uani 1 1 d . . . . .
H3 H 0.3373 0.5575 0.2216 0.05(3) Uiso 1 1 calc R . . . .
C4 C 0.3613(4) 0.5045(4) 0.2437(6) 0.051(3) Uani 1 1 d . . . . .
H4 H 0.3709 0.5155 0.2892 0.077 Uiso 1 1 calc R . . . .
C5 C 0.3683(4) 0.4628(5) 0.2168(6) 0.056(3) Uani 1 1 d . . . . .
H5 H 0.3830 0.4461 0.2434 0.10(5) Uiso 1 1 calc R . . . .
C6 C 0.3528(4) 0.4474(4) 0.1497(5) 0.046(2) Uani 1 1 d . . . . .
C7 C 0.3617(5) 0.4071(5) 0.1143(6) 0.059(3) Uani 1 1 d . . . . .
H7 H 0.3796 0.3911 0.1356 0.05(3) Uiso 1 1 calc R . . . .
C8 C 0.3981(4) 0.5062(6) -0.1055(6) 0.065(3) Uani 1 1 d . . . . .
H8A H 0.4116 0.4822 -0.1185 0.07(4) Uiso 1 1 calc R . . . .
H8B H 0.4270 0.5434 -0.1120 0.06(3) Uiso 1 1 calc R . . . .
C9 C 0.3512(4) 0.4953(4) -0.1492(6) 0.048(2) Uani 1 1 d . . . . .
C10 C 0.3582(5) 0.5095(5) -0.2195(7) 0.066(3) Uani 1 1 d . . . . .
H10 H 0.3928 0.5276 -0.2386 0.098 Uiso 1 1 calc R . . . .
C11 C 0.3136(6) 0.4963(6) -0.2592(7) 0.082(4) Uani 1 1 d . . . . .
H11 H 0.3175 0.5050 -0.3058 0.098 Uiso 1 1 calc R . . . .
C12 C 0.2621(5) 0.4697(6) -0.2289(6) 0.068(3) Uani 1 1 d . . . . .
H12 H 0.2310 0.4597 -0.2550 0.082 Uiso 1 1 calc R . . . .
C13 C 0.2587(4) 0.4588(4) -0.1600(5) 0.045(2) Uani 1 1 d . . . . .
C14 C 0.2062(4) 0.4324(4) -0.1227(6) 0.047(2) Uani 1 1 d . . . . .
H14 H 0.1737 0.4239 -0.1445 0.07(3) Uiso 1 1 calc R . . . .
C15 C 0.1699(4) 0.3972(4) 0.0439(6) 0.049(3) Uani 1 1 d . . . . .
C16 C 0.1226(4) 0.3788(6) 0.0895(6) 0.064(3) Uani 1 1 d . . . . .
C17 C 0.1223(5) 0.3697(6) 0.1589(7) 0.079(4) Uani 1 1 d . U . . .
H17 H 0.1528 0.3726 0.1807 0.118 Uiso 1 1 calc R . . . .
C18 C 0.0766(7) 0.3565(8) 0.1950(9) 0.114(6) Uani 1 1 d . U . . .
H18 H 0.0772 0.3544 0.2428 0.137 Uiso 1 1 calc R . . . .
C19 C 0.0289(6) 0.3461(7) 0.1623(7) 0.094(4) Uani 1 1 d . U . . .
H19 H -0.0032 0.3350 0.1866 0.112 Uiso 1 1 calc R . . . .
C20 C 0.0317(4) 0.3531(6) 0.0923(6) 0.069(3) Uani 1 1 d . U . . .
C21 C -0.0173(4) 0.3415(5) 0.0495(6) 0.063(3) Uani 1 1 d . . . . .
Cl1 Cl 0.06137(15) 0.3287(2) -0.1404(2) 0.1112(16) Uani 1 1 d . . . . .
Cl2 Cl 0.10240(12) 0.46984(12) -0.07951(17) 0.0636(8) Uani 1 1 d . . . . .
Cl3 Cl 0.3333 0.6667 0.1968(2) 0.0479(10) Uani 1 3 d S T P . .
Cl4 Cl 0.5140(3) 0.5269(3) 0.2226(3) 0.0938(18) Uani 0.6667 1 d D U . . .
Dy1 Dy 0.29026(2) 0.43072(2) -0.00392(2) 0.03750(19) Uani 1 1 d . . . . .
N1 N 0.3301(3) 0.4701(3) 0.1097(4) 0.0374(17) Uani 1 1 d . . . . .
N2 N 0.3439(3) 0.3949(4) 0.0537(4) 0.047(2) Uani 1 1 d . . . . .
N3 N 0.3021(3) 0.4700(3) -0.1202(4) 0.0374(17) Uani 1 1 d . . . . .
N4 N 0.2078(3) 0.4221(3) -0.0596(4) 0.0390(17) Uani 1 1 d . . . . .
N5 N 0.1601(3) 0.4013(3) -0.0225(4) 0.0436(19) Uani 1 1 d . . . . .
N6 N 0.0769(3) 0.3680(4) 0.0557(4) 0.056(2) Uani 1 1 d . . . . .
N8 N -0.0045(3) 0.3549(4) -0.0168(4) 0.055(2) Uani 1 1 d . . . . .
O1 O 0.2945(3) 0.5153(3) 0.0228(3) 0.0474(17) Uani 1 1 d . . . . .
H1 H 0.2813 0.5296 -0.0011 0.071 Uiso 1 1 calc DGR . . . .
O2 O -0.0631(3) 0.3220(4) 0.0768(4) 0.069(3) Uani 1 1 d . . . . .
O3 O 0.2153(3) 0.4084(3) 0.0708(4) 0.0541(19) Uani 1 1 d . . . . .
O4 O 0.3815(3) 0.4975(4) -0.0352(4) 0.063(2) Uani 1 1 d . . . . .
H4A H 0.4079 0.5055 -0.0105 0.094 Uiso 1 1 calc GR . . . .
O5 O 0.2286(4) 0.3349(3) -0.0057(6) 0.095(3) Uani 1 1 d . . . . .
O6 O 0.3333 0.6667 0.1221(8) 0.084(5) Uani 1 3 d S T P . .
O7 O 0.3315(3) 0.7134(3) 0.2167(5) 0.073(2) Uani 1 1 d . . . . .
O8 O 0.5074(11) 0.5616(9) 0.1700(11) 0.158(7) Uani 0.6667 1 d D U . . .
O9 O 0.4810(5) 0.5123(6) 0.2908(6) 0.133(4) Uani 1 1 d D U . . .
O10 O 0.5722(10) 0.5499(10) 0.2327(14) 0.244(11) Uani 1 1 d . U . . .
O11 O 0.1771(10) 0.5203(10) 0.0495(11) 0.240(10) Uani 1 1 d . U . . .
O12 O 0.1334(12) 0.2687(11) 0.0441(12) 0.277(12) Uani 1 1 d . U . . .
O13 O 0.907(2) 0.1865(17) 0.160(2) 0.43(2) Uani 1 1 d . U . . .
O14 O 0.4639(8) 0.5083(10) 0.0445(10) 0.230(9) Uani 1 1 d . U . . .
O15 O 0.2172(13) 0.3115(13) 0.1857(15) 0.307(13) Uani 1 1 d . U . . .
Zn1 Zn 0.07846(4) 0.38374(5) -0.04856(6) 0.0428(3) Uani 1 1 d . . . . .
O16 O 0.0000 0.0000 0.0000 0.46(6) Uani 1 6 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 1.491(14) . ?
C1 O1 1.425(7) . ?
C2 C3 1.378(15) . ?
C2 N1 1.347(12) . ?
C3 C4 1.344(15) . ?
C4 C5 1.397(15) . ?
C5 C6 1.374(15) . ?
C6 C7 1.462(13) . ?
C6 N1 1.361(12) . ?
C7 N2 1.257(13) . ?
C8 C9 1.475(15) . ?
C8 O4 1.423(14) . ?
C9 C10 1.407(16) . ?
C9 N3 1.333(12) . ?
C10 C11 1.365(18) . ?
C11 C12 1.397(17) . ?
C12 C13 1.364(15) . ?
C13 C14 1.482(13) . ?
C13 N3 1.350(12) . ?
C14 N4 1.264(12) . ?
C15 C16 1.468(14) . ?
C15 N5 1.334(13) . ?
C15 O3 1.277(11) . ?
C16 C17 1.370(16) . ?
C16 N6 1.347(13) . ?
C17 C18 1.35(2) . ?
C18 C19 1.39(2) . ?
C19 C20 1.369(18) . ?
C20 C21 1.511(14) . ?
C20 N6 1.337(14) . ?
C21 N8 1.338(14) . ?
C21 O2 1.248(12) . ?
Cl1 Zn1 2.257(4) . ?
Cl2 Zn1 2.268(3) . ?
Cl3 O6 1.449(16) . ?
Cl3 O7 1.408(8) 3_565 ?
Cl3 O7 1.408(8) . ?
Cl3 O7 1.408(8) 2_665 ?
Cl4 Cl4 1.239(12) 4 ?
Cl4 O8 1.494(15) . ?
Cl4 O9 1.555(11) . ?
Cl4 O9 1.308(12) 4 ?
Cl4 O10 1.46(2) 4 ?
Cl4 O10 1.46(2) . ?
Dy1 N1 2.474(8) . ?
Dy1 N2 2.482(7) . ?
Dy1 N3 2.464(8) . ?
Dy1 N4 2.478(7) . ?
Dy1 O1 2.401(6) . ?
Dy1 O2 2.379(7) 8 ?
Dy1 O3 2.384(7) . ?
Dy1 O4 2.403(7) . ?
Dy1 O5 2.390(8) . ?
N2 N8 1.392(11) 8 ?
N4 N5 1.380(10) . ?
N5 Zn1 2.175(7) . ?
N6 Zn1 2.066(8) . ?
N8 N2 1.392(11) 9 ?
N8 Zn1 2.163(8) . ?
O2 Dy1 2.379(7) 9 ?
O9 Cl4 1.308(12) 4 ?
O10 Cl4 1.46(2) 4 ?
O10 O10 1.29(4) 4 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 112.1(8) . . ?
C3 C2 C1 121.8(9) . . ?
N1 C2 C1 115.2(9) . . ?
N1 C2 C3 123.0(9) . . ?
C4 C3 C2 118.9(10) . . ?
C3 C4 C5 120.5(11) . . ?
C6 C5 C4 117.7(10) . . ?
C5 C6 C7 122.7(9) . . ?
N1 C6 C5 122.8(9) . . ?
N1 C6 C7 114.4(9) . . ?
N2 C7 C6 116.8(9) . . ?
O4 C8 C9 109.2(9) . . ?
C10 C9 C8 120.8(9) . . ?
N3 C9 C8 117.6(10) . . ?
N3 C9 C10 121.5(10) . . ?
C11 C10 C9 119.3(11) . . ?
C10 C11 C12 119.3(12) . . ?
C13 C12 C11 118.0(11) . . ?
C12 C13 C14 122.2(9) . . ?
N3 C13 C12 123.7(9) . . ?
N3 C13 C14 114.2(9) . . ?
N4 C14 C13 116.5(8) . . ?
N5 C15 C16 114.7(8) . . ?
O3 C15 C16 118.3(10) . . ?
O3 C15 N5 126.9(9) . . ?
C17 C16 C15 125.2(10) . . ?
N6 C16 C15 113.2(9) . . ?
N6 C16 C17 121.4(10) . . ?
C18 C17 C16 118.4(13) . . ?
C17 C18 C19 121.5(16) . . ?
C20 C19 C18 116.3(14) . . ?
C19 C20 C21 122.2(11) . . ?
N6 C20 C19 123.3(11) . . ?
N6 C20 C21 114.4(10) . . ?
N8 C21 C20 112.1(9) . . ?
O2 C21 C20 120.4(10) . . ?
O2 C21 N8 127.5(9) . . ?
O7 Cl3 O6 105.9(4) 3_565 . ?
O7 Cl3 O6 105.9(4) . . ?
O7 Cl3 O6 105.9(4) 2_665 . ?
O7 Cl3 O7 112.8(4) . 2_665 ?
O7 Cl3 O7 112.8(4) 2_665 3_565 ?
O7 Cl3 O7 112.8(4) . 3_565 ?
Cl4 Cl4 O8 159.2(10) 4 . ?
Cl4 Cl4 O9 54.4(6) 4 . ?
Cl4 Cl4 O9 75.2(8) 4 4 ?
Cl4 Cl4 O10 65.1(12) 4 . ?
Cl4 Cl4 O10 64.7(12) 4 4 ?
O8 Cl4 O9 119.9(12) . . ?
O9 Cl4 O8 124.7(12) 4 . ?
O9 Cl4 O9 100.8(10) 4 . ?
O9 Cl4 O10 86.7(11) 4 . ?
O9 Cl4 O10 131.2(15) 4 4 ?
O10 Cl4 O8 106.6(16) . . ?
O10 Cl4 O8 94.9(15) 4 . ?
O10 Cl4 O9 113.8(13) . . ?
O10 Cl4 O9 78.0(10) 4 . ?
O10 Cl4 O10 52.3(18) . 4 ?
N1 Dy1 N2 63.2(2) . . ?
N1 Dy1 N4 129.0(2) . . ?
N3 Dy1 N1 133.0(2) . . ?
N3 Dy1 N2 128.7(3) . . ?
N3 Dy1 N4 63.5(2) . . ?
N4 Dy1 N2 154.1(3) . . ?
O1 Dy1 N1 64.7(2) . . ?
O1 Dy1 N2 125.4(2) . . ?
O1 Dy1 N3 79.4(2) . . ?
O1 Dy1 N4 76.4(2) . . ?
O1 Dy1 O4 76.6(3) . . ?
O2 Dy1 N1 124.3(2) 8 . ?
O2 Dy1 N2 64.3(2) 8 . ?
O2 Dy1 N3 72.6(2) 8 . ?
O2 Dy1 N4 106.5(2) 8 . ?
O2 Dy1 O1 146.1(3) 8 . ?
O2 Dy1 O3 138.4(3) 8 . ?
O2 Dy1 O4 74.2(3) 8 . ?
O2 Dy1 O5 68.4(4) 8 . ?
O3 Dy1 N1 74.0(2) . . ?
O3 Dy1 N2 105.5(3) . . ?
O3 Dy1 N3 125.3(2) . . ?
O3 Dy1 N4 64.2(2) . . ?
O3 Dy1 O1 74.1(3) . . ?
O3 Dy1 O4 146.2(3) . . ?
O3 Dy1 O5 70.0(3) . . ?
O4 Dy1 N1 78.4(3) . . ?
O4 Dy1 N2 78.2(3) . . ?
O4 Dy1 N3 64.1(3) . . ?
O4 Dy1 N4 124.2(3) . . ?
O5 Dy1 N1 115.9(3) . . ?
O5 Dy1 N2 77.9(3) . . ?
O5 Dy1 N3 111.0(3) . . ?
O5 Dy1 N4 76.3(3) . . ?
O5 Dy1 O1 141.7(3) . . ?
O5 Dy1 O4 141.6(4) . . ?
C2 N1 C6 117.1(8) . . ?
C2 N1 Dy1 121.8(6) . . ?
C6 N1 Dy1 120.7(6) . . ?
C7 N2 Dy1 123.5(7) . . ?
C7 N2 N8 118.3(8) . 8 ?
N8 N2 Dy1 118.2(5) 8 . ?
C9 N3 C13 118.1(9) . . ?
C9 N3 Dy1 119.9(7) . . ?
C13 N3 Dy1 121.0(6) . . ?
C14 N4 Dy1 122.7(6) . . ?
C14 N4 N5 117.6(7) . . ?
N5 N4 Dy1 119.5(5) . . ?
C15 N5 N4 109.8(7) . . ?
C15 N5 Zn1 116.7(6) . . ?
N4 N5 Zn1 133.1(6) . . ?
C16 N6 Zn1 120.9(7) . . ?
C20 N6 C16 118.6(9) . . ?
C20 N6 Zn1 120.1(7) . . ?
C21 N8 N2 109.6(8) . 9 ?
C21 N8 Zn1 118.1(6) . . ?
N2 N8 Zn1 132.1(6) 9 . ?
C1 O1 Dy1 122.0(5) . . ?
C21 O2 Dy1 118.5(7) . 9 ?
C15 O3 Dy1 118.4(7) . . ?
C8 O4 Dy1 120.7(6) . . ?
Cl4 O9 Cl4 50.4(6) 4 . ?
Cl4 O10 Cl4 50.2(10) . 4 ?
O10 O10 Cl4 64.1(14) 4 . ?
O10 O10 Cl4 63.6(13) 4 4 ?
Cl1 Zn1 Cl2 112.52(18) . . ?
N5 Zn1 Cl1 100.2(3) . . ?
N5 Zn1 Cl2 96.0(2) . . ?
N6 Zn1 Cl1 130.4(3) . . ?
N6 Zn1 Cl2 117.1(3) . . ?
N6 Zn1 N5 74.2(3) . . ?
N6 Zn1 N8 74.8(3) . . ?
N8 Zn1 Cl1 98.4(3) . . ?
N8 Zn1 Cl2 99.5(3) . . ?
N8 Zn1 N5 148.9(3) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.265 2949.0 1134.3 ?
2 0.000 0.351 0.750 7.8 0.0 ?
3 0.000 0.649 0.250 7.8 0.0 ?
4 0.333 0.667 0.907 215.0 0.0 ?
5 0.333 0.667 0.407 215.0 0.0 ?
6 0.351 0.000 0.750 7.8 0.0 ?
7 0.351 0.351 0.250 7.8 0.0 ?
8 0.667 0.333 0.593 215.0 0.0 ?
9 0.667 0.333 0.093 215.0 0.0 ?
10 0.649 0.000 0.250 7.8 0.0 ?
11 0.649 0.649 0.750 7.8 0.0 ?


_olex2_submission_special_instructions 'No special instructions were received'
