# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_Dy4Cu4
_audit_block_doi                 10.5517/cc1jhxjg
_database_code_depnum_ccdc_archive 'CCDC 1415476'
_audit_update_record             
;
2015-07-28 deposited with the CCDC.
2015-10-02 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            'C84 H132 Cl12 Cu4 Dy4 N28 O48'
_chemical_formula_weight         3631.73

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'

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

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

_cell_length_a                   19.3834(15)
_cell_length_b                   27.657(2)
_cell_length_c                   15.3958(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8253.6(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    9856
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      26.02

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_F_000             3600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.559
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50301
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.473
_diffrn_reflns_theta_max         26.043
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8543
_reflns_number_gt                5537
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8543
_refine_ls_number_parameters     405
_refine_ls_number_restraints     156
_refine_ls_R_factor_all          0.1814
_refine_ls_R_factor_gt           0.1311
_refine_ls_wR_factor_ref         0.4479
_refine_ls_wR_factor_gt          0.3842
_refine_ls_goodness_of_fit_ref   1.727
_refine_ls_restrained_S_all      1.756
_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 1.1489(8) 0.5152(7) 0.6543(11) 0.090(6) Uani 1 1 d D . . . .
H1A H 1.1778 0.5432 0.6647 0.108 Uiso 1 1 calc R U . . .
H1B H 1.1725 0.4939 0.6140 0.108 Uiso 1 1 calc R U . . .
N1 N 1.0268(4) 0.5081(3) 0.6500(6) 0.058(4) Uani 1 1 d DG . . . .
C2 C 1.0881(3) 0.5287(3) 0.6217(6) 0.058(4) Uani 1 1 d G U . . .
C3 C 1.0874(3) 0.5630(3) 0.5556(7) 0.072(5) Uani 1 1 d G . . . .
H3 H 1.1285 0.5768 0.5367 0.087 Uiso 1 1 calc R U . . .
C4 C 1.0252(5) 0.5766(3) 0.5179(6) 0.067(5) Uani 1 1 d G . . . .
H4 H 1.0247 0.5996 0.4737 0.080 Uiso 1 1 calc R U . . .
C5 C 0.9638(3) 0.5560(4) 0.5462(7) 0.068(5) Uani 1 1 d G . . . .
H5 H 0.9222 0.5651 0.5210 0.082 Uiso 1 1 calc R U . . .
C6 C 0.9646(3) 0.5217(4) 0.6122(7) 0.058(4) Uani 1 1 d G . . . .
C7 C 0.9041(7) 0.5011(6) 0.6479(10) 0.059(4) Uani 1 1 d . U . . .
H7 H 0.8608 0.5085 0.6256 0.070 Uiso 1 1 calc R U . . .
C8 C 0.8711(9) 0.4280(6) 0.8196(14) 0.071(4) Uani 1 1 d . U . . .
C9 C 0.8112(8) 0.4082(7) 0.8695(13) 0.077(5) Uani 1 1 d . U . . .
C10 C 0.8120(8) 0.3807(6) 0.9371(14) 0.080(5) Uani 1 1 d . U . . .
H10 H 0.8540 0.3691 0.9577 0.096 Uiso 1 1 calc R U . . .
C11 C 0.7500 0.3675(9) 0.9810(18) 0.081(7) Uani 1 2 d S TU P . .
H11 H 0.7500 0.3515 1.0341 0.097 Uiso 1 2 calc R U P . .
C12 C 0.8862(15) 0.2500 0.5688(17) 0.082(8) Uani 1 2 d S T P . .
H12 H 0.8513 0.2500 0.5275 0.098 Uiso 1 2 calc R U P . .
C13 C 0.9076(8) 0.2911(7) 0.5941(11) 0.077(5) Uani 1 1 d . . . . .
H13 H 0.8923 0.3196 0.5681 0.093 Uiso 1 1 calc R U . . .
C14 C 0.9551(7) 0.2918(5) 0.6627(10) 0.056(4) Uani 1 1 d . . . . .
C15 C 0.9838(7) 0.3342(6) 0.7093(10) 0.052(4) Uani 1 1 d . . . . .
C16 C 1.0863(7) 0.3525(7) 0.8885(11) 0.071(5) Uani 1 1 d . . . . .
H16 H 1.0983 0.3216 0.9065 0.086 Uiso 1 1 calc R U . . .
N8 N 1.0797(5) 0.4392(4) 0.9047(6) 0.068(4) Uani 1 1 d G U . . .
C17 C 1.1049(6) 0.3954(3) 0.9354(7) 0.080(5) Uani 1 1 d G U . . .
C18 C 1.1405(7) 0.3936(4) 1.0137(8) 0.093(6) Uani 1 1 d G U . . .
H18 H 1.1573 0.3643 1.0342 0.112 Uiso 1 1 calc R U . . .
C19 C 1.1509(7) 0.4357(5) 1.0613(7) 0.121(8) Uani 1 1 d G U . . .
H19 H 1.1747 0.4345 1.1137 0.145 Uiso 1 1 calc R U . . .
C20 C 1.1257(7) 0.4796(4) 1.0306(7) 0.091(5) Uani 1 1 d G U . . .
H20 H 1.1327 0.5077 1.0625 0.109 Uiso 1 1 calc R U . . .
C21 C 1.0901(6) 0.4813(3) 0.9523(7) 0.078(5) Uani 1 1 d G U . . .
C22 C 1.0624(10) 0.5243(7) 0.9185(13) 0.087(5) Uani 1 1 d . U . . .
H22A H 1.0996 0.5442 0.8962 0.104 Uiso 1 1 calc R U . . .
H22B H 1.0398 0.5420 0.9647 0.104 Uiso 1 1 calc R U . . .
Cl1 Cl 0.7500 0.5473(2) 0.7371(3) 0.0606(14) Uani 1 2 d S T P . .
Cl2 Cl 0.7500 0.4531(4) 0.5735(5) 0.119(3) Uani 1 2 d S TU P . .
Cl3 Cl 1.1568(3) 0.2500 0.8169(6) 0.092(2) Uani 1 2 d S T P . .
Cl4 Cl 0.9936(5) 0.2500 0.9386(6) 0.126(3) Uani 1 2 d S T P . .
Cl5 Cl 0.2500 0.5046(3) 0.8635(5) 0.107(3) Uani 1 2 d S TU P . .
Cu1 Cu 0.7500 0.46165(12) 0.7252(2) 0.0718(9) Uani 1 2 d S T P . .
Cu2 Cu 1.03950(12) 0.2500 0.79138(17) 0.0558(7) Uani 1 2 d S T P . .
Dy1 Dy 1.02538(3) 0.44271(3) 0.75944(6) 0.0632(4) Uani 1 1 d . . . . .
N2 N 0.9109(6) 0.4721(5) 0.7118(10) 0.065(3) Uani 1 1 d . U . . .
N3 N 0.8536(8) 0.4513(5) 0.7533(10) 0.066(4) Uani 1 1 d . . . . .
N4 N 0.7500 0.4196(5) 0.8239(12) 0.052(4) Uani 1 2 d S TU P . .
N5 N 0.9757(7) 0.2500 0.6960(10) 0.044(4) Uani 1 2 d S T P . .
N6 N 1.0261(5) 0.3203(5) 0.7745(8) 0.056(4) Uani 1 1 d . . . . .
N7 N 1.0501(6) 0.3614(6) 0.8160(9) 0.069(4) Uani 1 1 d . . . . .
O1 O 1.1335(6) 0.4874(5) 0.7442(8) 0.089(4) Uani 1 1 d D . . . .
H1D H 1.1524 0.5017 0.7843 0.133 Uiso 1 1 calc DR U . . .
O2 O 0.9308(4) 0.4208(4) 0.8464(8) 0.066(3) Uani 1 1 d . . . . .
O3 O 0.9688(5) 0.3762(4) 0.6886(8) 0.064(3) Uani 1 1 d . . . . .
O4 O 1.0124(6) 0.5150(5) 0.8484(9) 0.084(4) Uani 1 1 d D . . . .
H4D H 0.9732 0.5197 0.8665 0.126 Uiso 1 1 calc DR U . . .
O5 O 1.1001(5) 0.4075(4) 0.6540(7) 0.071(3) Uani 1 1 d . . . . .
O6 O 0.7500 0.3417(11) 0.597(2) 0.199(14) Uani 1 2 d S TU P . .
O7 O 0.7500 0.2999(12) 0.436(2) 0.190(13) Uani 1 2 d S TU P . .
O8 O 0.2500 0.4079(8) 0.6178(15) 0.119(7) Uani 1 2 d DS TU P . .
O9 O 0.1716(16) 0.2500 0.607(2) 0.165(10) Uani 1 2 d S TU P . .
O10 O 0.9846(13) 0.5998(8) 0.7898(18) 0.171(8) Uani 1 1 d . U . . .
O11 O 0.0116(18) 0.3002(11) 0.403(2) 0.223(11) Uani 1 1 d . U . . .
O12 O 0.0425(16) 0.6553(10) 0.945(2) 0.228(13) Uani 1 1 d . U . . .
O13 O 0.2500 0.6056(11) 0.801(2) 0.168(11) Uani 1 2 d S TU P . .
O14 O 0.0849(8) 0.3252(5) 0.5518(11) 0.108(5) Uani 1 1 d . U . . .
O15 O 0.2500 0.3565(19) 0.782(3) 0.28(2) Uani 1 2 d DS 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 1.334(17) . ?
C1 O1 1.611(17) . ?
N1 C2 1.3900 . ?
N1 C6 1.3900 . ?
N1 Dy1 2.472(9) . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.414(16) . ?
C7 N2 1.28(2) . ?
C8 O2 1.244(19) . ?
C8 N3 1.25(2) . ?
C8 C9 1.50(2) . ?
C9 C10 1.29(2) . ?
C9 N4 1.41(2) . ?
C10 C11 1.43(2) . ?
C11 C10 1.43(2) 8_755 ?
C12 C13 1.272(19) 7_565 ?
C12 C13 1.272(19) . ?
C13 C14 1.40(2) . ?
C14 N5 1.327(16) . ?
C14 C15 1.48(2) . ?
C15 O3 1.240(17) . ?
C15 N6 1.351(19) . ?
C16 N7 1.34(2) . ?
C16 C17 1.434(19) . ?
N8 C17 1.3900 . ?
N8 C21 1.3900 . ?
N8 Dy1 2.473(8) . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C19 C20 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.40(2) . ?
C22 O4 1.47(2) . ?
Cl1 Cu1 2.375(7) . ?
Cl2 Cu1 2.348(9) . ?
Cl3 Cu2 2.307(6) . ?
Cl4 Cu2 2.435(9) . ?
Cu1 N4 1.913(18) . ?
Cu1 N3 2.074(15) . ?
Cu1 N3 2.074(15) 8_755 ?
Cu2 N5 1.919(14) . ?
Cu2 N6 1.978(15) 7_565 ?
Cu2 N6 1.978(15) . ?
Dy1 O2 2.350(10) . ?
Dy1 O5 2.384(10) . ?
Dy1 O3 2.403(10) . ?
Dy1 O4 2.437(11) . ?
Dy1 O1 2.444(12) . ?
Dy1 N7 2.458(16) . ?
Dy1 N2 2.474(14) . ?
N2 N3 1.41(2) . ?
N4 C9 1.41(2) 8_755 ?
N5 C14 1.327(16) 7_565 ?
N6 N7 1.386(19) . ?

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 O1 107.1(12) . . ?
C2 N1 C6 120.0 . . ?
C2 N1 Dy1 121.6(4) . . ?
C6 N1 Dy1 118.3(4) . . ?
C1 C2 N1 121.5(10) . . ?
C1 C2 C3 118.5(10) . . ?
N1 C2 C3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C4 C5 C6 120.0 . . ?
C5 C6 N1 120.0 . . ?
C5 C6 C7 123.3(9) . . ?
N1 C6 C7 116.6(9) . . ?
N2 C7 C6 117.8(13) . . ?
O2 C8 N3 127.2(18) . . ?
O2 C8 C9 119.5(19) . . ?
N3 C8 C9 113.3(16) . . ?
C10 C9 N4 122.9(15) . . ?
C10 C9 C8 128.4(17) . . ?
N4 C9 C8 108.3(17) . . ?
C9 C10 C11 121.6(17) . . ?
C10 C11 C10 115(2) . 8_755 ?
C13 C12 C13 127(3) 7_565 . ?
C12 C13 C14 117.1(19) . . ?
N5 C14 C13 118.5(15) . . ?
N5 C14 C15 112.9(13) . . ?
C13 C14 C15 128.5(15) . . ?
O3 C15 N6 126.9(14) . . ?
O3 C15 C14 121.9(13) . . ?
N6 C15 C14 111.3(13) . . ?
N7 C16 C17 113.5(15) . . ?
C17 N8 C21 120.0 . . ?
C17 N8 Dy1 119.4(5) . . ?
C21 N8 Dy1 120.4(5) . . ?
C18 C17 N8 120.0 . . ?
C18 C17 C16 122.1(10) . . ?
N8 C17 C16 117.5(10) . . ?
C17 C18 C19 120.0 . . ?
C18 C19 C20 120.0 . . ?
C21 C20 C19 120.0 . . ?
C20 C21 N8 120.0 . . ?
C20 C21 C22 122.8(10) . . ?
N8 C21 C22 117.2(10) . . ?
C21 C22 O4 112.1(14) . . ?
N4 Cu1 N3 75.5(5) . . ?
N4 Cu1 N3 75.5(5) . 8_755 ?
N3 Cu1 N3 151.0(9) . 8_755 ?
N4 Cu1 Cl2 136.8(6) . . ?
N3 Cu1 Cl2 101.2(4) . . ?
N3 Cu1 Cl2 101.2(4) 8_755 . ?
N4 Cu1 Cl1 123.0(5) . . ?
N3 Cu1 Cl1 97.0(4) . . ?
N3 Cu1 Cl1 97.0(4) 8_755 . ?
Cl2 Cu1 Cl1 100.2(3) . . ?
N5 Cu2 N6 79.3(3) . 7_565 ?
N5 Cu2 N6 79.3(3) . . ?
N6 Cu2 N6 158.6(6) 7_565 . ?
N5 Cu2 Cl3 139.9(5) . . ?
N6 Cu2 Cl3 98.7(3) 7_565 . ?
N6 Cu2 Cl3 98.7(3) . . ?
N5 Cu2 Cl4 118.5(6) . . ?
N6 Cu2 Cl4 94.3(4) 7_565 . ?
N6 Cu2 Cl4 94.3(4) . . ?
Cl3 Cu2 Cl4 101.6(3) . . ?
O2 Dy1 O5 139.2(4) . . ?
O2 Dy1 O3 72.9(4) . . ?
O5 Dy1 O3 69.8(4) . . ?
O2 Dy1 O4 79.1(4) . . ?
O5 Dy1 O4 141.4(4) . . ?
O3 Dy1 O4 146.7(3) . . ?
O2 Dy1 O1 148.7(4) . . ?
O5 Dy1 O1 67.7(4) . . ?
O3 Dy1 O1 137.3(4) . . ?
O4 Dy1 O1 74.2(4) . . ?
O2 Dy1 N7 73.4(4) . . ?
O5 Dy1 N7 75.5(4) . . ?
O3 Dy1 N7 63.3(4) . . ?
O4 Dy1 N7 124.9(5) . . ?
O1 Dy1 N7 109.2(5) . . ?
O2 Dy1 N1 125.8(3) . . ?
O5 Dy1 N1 80.1(4) . . ?
O3 Dy1 N1 104.8(4) . . ?
O4 Dy1 N1 77.5(4) . . ?
O1 Dy1 N1 63.6(4) . . ?
N7 Dy1 N1 155.3(4) . . ?
O2 Dy1 N8 78.9(3) . . ?
O5 Dy1 N8 110.0(3) . . ?
O3 Dy1 N8 125.1(4) . . ?
O4 Dy1 N8 64.4(4) . . ?
O1 Dy1 N8 75.0(4) . . ?
N7 Dy1 N8 64.0(4) . . ?
N1 Dy1 N8 129.8(3) . . ?
O2 Dy1 N2 63.5(4) . . ?
O5 Dy1 N2 118.5(4) . . ?
O3 Dy1 N2 73.0(4) . . ?
O4 Dy1 N2 78.7(4) . . ?
O1 Dy1 N2 125.0(5) . . ?
N7 Dy1 N2 125.5(4) . . ?
N1 Dy1 N2 64.4(4) . . ?
N8 Dy1 N2 131.5(4) . . ?
C7 N2 N3 121.8(14) . . ?
C7 N2 Dy1 121.9(10) . . ?
N3 N2 Dy1 116.1(11) . . ?
C8 N3 N2 111.5(15) . . ?
C8 N3 Cu1 120.3(13) . . ?
N2 N3 Cu1 127.9(12) . . ?
C9 N4 C9 114(2) 8_755 . ?
C9 N4 Cu1 122.0(10) 8_755 . ?
C9 N4 Cu1 122.0(10) . . ?
C14 N5 C14 121.3(16) 7_565 . ?
C14 N5 Cu2 119.3(8) 7_565 . ?
C14 N5 Cu2 119.3(8) . . ?
C15 N6 N7 108.2(13) . . ?
C15 N6 Cu2 117.2(10) . . ?
N7 N6 Cu2 134.6(9) . . ?
C16 N7 N6 114.1(15) . . ?
C16 N7 Dy1 124.4(12) . . ?
N6 N7 Dy1 121.5(9) . . ?
C1 O1 Dy1 118.9(8) . . ?
C8 O2 Dy1 119.6(13) . . ?
C15 O3 Dy1 119.6(9) . . ?
C22 O4 Dy1 119.1(11) . . ?

_refine_diff_density_max         7.729
_refine_diff_density_min         -1.813
_refine_diff_density_rms         0.338



####################################################################### 
# 
# 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_Dy4L4CF3SO3
_audit_block_doi                 10.5517/cc1jhxkh
_database_code_depnum_ccdc_archive 'CCDC 1415477'
_audit_update_record             
;
2015-07-28 deposited with the CCDC.
2015-10-02 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            'C80 H76 Dy4 F12 N28 O44 S4'
_chemical_formula_weight         3139.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_H-M_alt        'I 41/a m d'
_space_group_name_Hall           '-I 4bd 2'

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

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

_cell_length_a                   21.384(3)
_cell_length_b                   21.384(3)
_cell_length_c                   38.507(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17609(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9107
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      24.63

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_F_000             6160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    1.801
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49084
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_av_R_equivalents  0.1199
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.712
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_full        24.995
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4117
_reflns_number_gt                2309
_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.

The command 'isor' was also used to restrain the o5 o6 o7 f2 atoms with NPD and ADP
problems. The restraint command lead to restraint number 24, but cannot be
completely avoided. Refinement of F² against ALL reflections.

;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4117
_refine_ls_number_parameters     206
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1603
_refine_ls_R_factor_gt           0.0985
_refine_ls_wR_factor_ref         0.3384
_refine_ls_wR_factor_gt          0.2971
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_restrained_S_all      1.186
_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 0.1914(7) 0.4341(6) 0.7952(3) 0.081(4) Uani 1 1 d . . . . .
H1 H 0.1987 0.3968 0.8069 0.097 Uiso 1 1 calc R U . . .
C2 C 0.1696(7) 0.4299(7) 0.7616(4) 0.089(4) Uani 1 1 d . . . . .
H2 H 0.1617 0.3908 0.7519 0.107 Uiso 1 1 calc R U . . .
C3 C 0.1596(8) 0.4816(8) 0.7427(4) 0.103(5) Uani 1 1 d . . . . .
H3 H 0.1463 0.4797 0.7198 0.124 Uiso 1 1 calc R U . . .
C4 C 0.1709(7) 0.5417(7) 0.7606(3) 0.082(4) Uani 1 1 d . . . . .
H4 H 0.1635 0.5795 0.7493 0.098 Uiso 1 1 calc R U . . .
C5 C 0.1925(5) 0.5403(6) 0.7941(3) 0.061(3) Uani 1 1 d . . . . .
C6 C 0.2079(5) 0.5972(5) 0.8114(3) 0.063(3) Uani 1 1 d . . . . .
H6 H 0.2032 0.6358 0.8005 0.076 Uiso 1 1 calc R U . . .
C7 C 0.3890(6) 0.5170(6) 0.8581(3) 0.065(3) Uani 1 1 d . . . . .
C8 C 0.4446(5) 0.5397(6) 0.8414(2) 0.063(3) Uani 1 1 d . . . . .
C9 C 0.4443(6) 0.5742(6) 0.8110(3) 0.071(3) Uani 1 1 d . . . . .
H9 H 0.4069 0.5872 0.8011 0.086 Uiso 1 1 calc R U . . .
C10 C 0.5000 0.5889(9) 0.7960(4) 0.077(5) Uani 1 2 d S T P . .
H10 H 0.5000 0.6097 0.7748 0.092 Uiso 1 2 calc R U P . .
C11 C 0.3841(15) 0.7500 0.8223(9) 0.141(10) Uani 1 2 d S T P . .
Dy1 Dy 0.24187(3) 0.49187(3) 0.8750 0.0584(4) Uani 1 2 d S T P . .
F1 F 0.3800(6) 0.6985(6) 0.8404(4) 0.173(5) Uani 1 1 d . . . . .
F2 F 0.4387(10) 0.7500 0.8075(5) 0.203(8) Uani 1 2 d S TU P . .
N1 N 0.2026(5) 0.4858(4) 0.8120(2) 0.064(2) Uani 1 1 d . . . . .
N2 N 0.2285(4) 0.5928(4) 0.8426(2) 0.061(2) Uani 1 1 d . . . . .
N3 N 0.2457(4) 0.6457(5) 0.8591(2) 0.060(2) Uani 1 1 d . . . . .
N4 N 0.5000 0.5209(7) 0.8562(3) 0.071(4) Uani 1 2 d S T P . .
O1 O 0.1615(4) 0.4115(4) 0.8750 0.112(5) Uani 1 2 d S T P . .
O2 O 0.2885(5) 0.3973(4) 0.8569(2) 0.101(3) Uani 1 1 d . . . . .
O3 O 0.3367(4) 0.5223(4) 0.84506(18) 0.071(2) Uani 1 1 d . . . . .
O4 O 0.2655(7) 0.7500 0.8124(3) 0.099(4) Uani 1 2 d S T P . .
O5 O 0.3266(7) 0.8059(6) 0.7702(3) 0.160(5) Uani 1 1 d . U . . .
O6 O 0.4019(12) 0.3856(12) 0.8242(6) 0.289(11) Uani 1 1 d . U . . .
O7 O 0.231(2) 0.2500 0.9086(11) 0.34(2) Uani 1 2 d S TU P . .
S1 S 0.3189(4) 0.7500 0.78877(17) 0.116(2) Uani 1 2 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 N1 1.303(14) . ?
C1 C2 1.377(17) . ?
C2 C3 1.34(2) . ?
C3 C4 1.48(2) . ?
C4 C5 1.374(14) . ?
C5 N1 1.370(14) . ?
C5 C6 1.425(15) . ?
C6 N2 1.286(12) . ?
C7 O3 1.230(13) . ?
C7 N3 1.349(14) 15_446 ?
C7 C8 1.437(16) . ?
C8 N4 1.374(12) . ?
C8 C9 1.383(14) . ?
C9 C10 1.360(13) . ?
C10 C9 1.360(13) 22_655 ?
C11 F2 1.30(3) . ?
C11 F1 1.307(18) . ?
C11 F1 1.307(18) 29_565 ?
C11 S1 1.90(3) . ?
Dy1 O2 2.362(9) 15_446 ?
Dy1 O2 2.362(9) . ?
Dy1 O3 2.422(8) . ?
Dy1 O3 2.422(8) 15_446 ?
Dy1 O1 2.432(13) . ?
Dy1 N2 2.508(9) 15_446 ?
Dy1 N2 2.508(9) . ?
Dy1 N1 2.571(9) . ?
Dy1 N1 2.571(9) 15_446 ?
N2 N3 1.347(13) . ?
N3 C7 1.349(14) 15_446 ?
N4 C8 1.374(12) 22_655 ?
O4 S1 1.459(15) . ?
O5 S1 1.403(11) . ?
S1 O5 1.403(11) 29_565 ?

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 125.7(12) . . ?
C3 C2 C1 120.6(14) . . ?
C2 C3 C4 116.1(14) . . ?
C5 C4 C3 118.3(14) . . ?
N1 C5 C4 122.9(11) . . ?
N1 C5 C6 117.1(9) . . ?
C4 C5 C6 119.9(11) . . ?
N2 C6 C5 116.9(10) . . ?
O3 C7 N3 120.7(11) . 15_446 ?
O3 C7 C8 122.5(10) . . ?
N3 C7 C8 116.4(9) 15_446 . ?
N4 C8 C9 120.6(11) . . ?
N4 C8 C7 115.4(9) . . ?
C9 C8 C7 123.8(11) . . ?
C10 C9 C8 118.6(12) . . ?
C9 C10 C9 122.2(15) . 22_655 ?
F2 C11 F1 107.1(19) . . ?
F2 C11 F1 107.1(19) . 29_565 ?
F1 C11 F1 115(3) . 29_565 ?
F2 C11 S1 111(2) . . ?
F1 C11 S1 108.3(17) . . ?
F1 C11 S1 108.3(17) 29_565 . ?
O2 Dy1 O2 144.3(5) 15_446 . ?
O2 Dy1 O3 138.1(3) 15_446 . ?
O2 Dy1 O3 74.6(3) . . ?
O2 Dy1 O3 74.6(3) 15_446 15_446 ?
O2 Dy1 O3 138.1(3) . 15_446 ?
O3 Dy1 O3 77.1(4) . 15_446 ?
O2 Dy1 O1 72.1(3) 15_446 . ?
O2 Dy1 O1 72.1(3) . . ?
O3 Dy1 O1 141.4(2) . . ?
O3 Dy1 O1 141.4(2) 15_446 . ?
O2 Dy1 N2 129.7(3) 15_446 15_446 ?
O2 Dy1 N2 71.7(3) . 15_446 ?
O3 Dy1 N2 63.0(3) . 15_446 ?
O3 Dy1 N2 68.2(3) 15_446 15_446 ?
O1 Dy1 N2 121.9(2) . 15_446 ?
O2 Dy1 N2 71.7(3) 15_446 . ?
O2 Dy1 N2 129.7(3) . . ?
O3 Dy1 N2 68.2(3) . . ?
O3 Dy1 N2 63.0(3) 15_446 . ?
O1 Dy1 N2 121.9(2) . . ?
N2 Dy1 N2 116.2(4) 15_446 . ?
O2 Dy1 N1 91.2(3) 15_446 . ?
O2 Dy1 N1 79.4(3) . . ?
O3 Dy1 N1 80.7(3) . . ?
O3 Dy1 N1 125.4(3) 15_446 . ?
O1 Dy1 N1 74.5(2) . . ?
N2 Dy1 N1 138.1(3) 15_446 . ?
N2 Dy1 N1 62.4(3) . . ?
O2 Dy1 N1 79.4(3) 15_446 15_446 ?
O2 Dy1 N1 91.2(3) . 15_446 ?
O3 Dy1 N1 125.4(3) . 15_446 ?
O3 Dy1 N1 80.7(3) 15_446 15_446 ?
O1 Dy1 N1 74.5(2) . 15_446 ?
N2 Dy1 N1 62.4(3) 15_446 15_446 ?
N2 Dy1 N1 138.1(3) . 15_446 ?
N1 Dy1 N1 149.1(4) . 15_446 ?
C1 N1 C5 116.3(10) . . ?
C1 N1 Dy1 124.9(8) . . ?
C5 N1 Dy1 118.8(7) . . ?
C6 N2 N3 118.2(10) . . ?
C6 N2 Dy1 124.6(8) . . ?
N3 N2 Dy1 117.2(6) . . ?
N2 N3 C7 116.3(9) . 15_446 ?
C8 N4 C8 119.1(13) 22_655 . ?
C7 O3 Dy1 122.8(7) . . ?
O5 S1 O5 116.9(12) . 29_565 ?
O5 S1 O4 114.2(7) . . ?
O5 S1 O4 114.2(7) 29_565 . ?
O5 S1 C11 105.1(9) . . ?
O5 S1 C11 105.1(9) 29_565 . ?
O4 S1 C11 98.6(12) . . ?

_refine_diff_density_max         3.154
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.282



####################################################################### 
# 
# 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_Dy4L4Cl
_audit_block_doi                 10.5517/cc1jhxlj
_database_code_depnum_ccdc_archive 'CCDC 1415478'
_audit_update_record             
;
2015-07-28 deposited with the CCDC.
2015-10-02 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            'C76 H76 Cl12 Dy4 N28 O16'
_chemical_formula_weight         2713.04

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'
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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

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

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

_cell_length_a                   21.9388(14)
_cell_length_b                   21.9388(14)
_cell_length_c                   16.3350(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7862.2(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9792
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      24.34

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_F_000             2648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.130
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_T_max  0.639
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49144
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.554
_diffrn_reflns_theta_max         26.148
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7803
_reflns_number_gt                3872
_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.

The command 'isor' was also used to restrain the C O and Cl atom with NPD and ADP
problems. The restraint command lead to restraint number 114, but cannot be
completely avoided. Refinement of F² against ALL reflections.

;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1854P)²+24.3332P] 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         7803
_refine_ls_number_parameters     307
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.0817
_refine_ls_wR_factor_ref         0.3436
_refine_ls_wR_factor_gt          0.2662
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.068
_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 0.6545(7) 0.3671(7) 0.0478(11) 0.114(5) Uani 1 1 d . U . . .
H1 H 0.6785 0.3928 0.0798 0.137 Uiso 1 1 calc R U . . .
C2 C 0.6579(8) 0.3714(8) -0.0363(11) 0.116(5) Uani 1 1 d . U . . .
H2 H 0.6854 0.3978 -0.0610 0.139 Uiso 1 1 calc R U . . .
C3 C 0.6237(10) 0.3394(10) -0.0779(15) 0.143(7) Uani 1 1 d . U . . .
H3 H 0.6245 0.3455 -0.1342 0.172 Uiso 1 1 calc R U . . .
C4 C 0.5827(7) 0.2935(8) -0.0475(10) 0.113(5) Uani 1 1 d . U . . .
H4 H 0.5589 0.2683 -0.0804 0.136 Uiso 1 1 calc R U . . .
C5 C 0.5832(7) 0.2916(7) 0.0389(9) 0.090(4) Uani 1 1 d . U . . .
C6 C 0.5461(6) 0.2461(6) 0.0788(8) 0.089(4) Uani 1 1 d . . . . .
H6 H 0.5236 0.2176 0.0495 0.107 Uiso 1 1 calc R U . . .
C7 C 0.5086(5) 0.2155(5) 0.2790(7) 0.062(3) Uani 1 1 d . . . . .
C8 C 0.4717(5) 0.1714(6) 0.3270(7) 0.072(3) Uani 1 1 d . . . . .
C9 C 0.4604(7) 0.1829(7) 0.4063(9) 0.102(4) Uani 1 1 d . U . . .
H9 H 0.4771 0.2170 0.4314 0.123 Uiso 1 1 calc R U . . .
C10 C 0.4244(8) 0.1444(8) 0.4494(11) 0.125(5) Uani 1 1 d . U . . .
H10 H 0.4145 0.1526 0.5037 0.151 Uiso 1 1 calc R U . . .
C11 C 0.4026(8) 0.0924(8) 0.4110(10) 0.122(5) Uani 1 1 d . U . . .
H11 H 0.3788 0.0641 0.4386 0.146 Uiso 1 1 calc R U . . .
C12 C 0.4179(6) 0.0848(6) 0.3300(7) 0.082(3) Uani 1 1 d . . . . .
C13 C 0.6752(7) 0.3123(6) 0.4272(9) 0.092(4) Uani 1 1 d . U . . .
H13 H 0.7051 0.2965 0.3929 0.111 Uiso 1 1 calc R U . . .
C14 C 0.6843(8) 0.3105(8) 0.5098(12) 0.118(5) Uani 1 1 d . U . . .
H14 H 0.7187 0.2912 0.5308 0.141 Uiso 1 1 calc R U . . .
C15 C 0.6447(8) 0.3361(7) 0.5602(10) 0.106(5) Uani 1 1 d . U . . .
H15 H 0.6515 0.3368 0.6164 0.127 Uiso 1 1 calc R U . . .
C16 C 0.5905(7) 0.3630(7) 0.5256(11) 0.109(5) Uani 1 1 d . U . . .
H16 H 0.5613 0.3804 0.5594 0.130 Uiso 1 1 calc R U . . .
C17 C 0.5829(6) 0.3625(6) 0.4455(9) 0.085(3) Uani 1 1 d . U . . .
C18 C 0.5305(6) 0.3876(6) 0.4054(9) 0.092(4) Uani 1 1 d . . . . .
H18 H 0.5010 0.4077 0.4361 0.111 Uiso 1 1 calc R U . . .
C19 C 0.4717(6) 0.3951(6) 0.2118(9) 0.081(3) Uani 1 1 d . . . . .
Cl1 Cl 0.66646(15) 0.22209(15) 0.25160(18) 0.0791(9) Uani 1 1 d . . . . .
Cl2 Cl 0.4767(3) 0.1027(2) 0.0763(3) 0.145(2) Uani 1 1 d . U . . .
Dy1 Dy 0.60167(3) 0.32697(3) 0.24120(4) 0.0723(3) Uani 1 1 d . . . . .
N1 N 0.6174(5) 0.3268(5) 0.0846(8) 0.088(3) Uani 1 1 d . U . . .
N2 N 0.5461(4) 0.2475(4) 0.1574(6) 0.071(2) Uani 1 1 d . . . . .
N3 N 0.5123(4) 0.2059(4) 0.1983(6) 0.070(2) Uani 1 1 d . . . . .
H3A H 0.4947 0.1758 0.1744 0.084 Uiso 1 1 calc R U . . .
N4 N 0.4509(4) 0.1233(5) 0.2880(6) 0.073(2) Uani 1 1 d . . . . .
N5 N 0.6251(5) 0.3358(4) 0.3941(7) 0.082(3) Uani 1 1 d . . . . .
N6 N 0.5240(5) 0.3830(4) 0.3307(7) 0.078(3) Uani 1 1 d . . . . .
N7 N 0.4751(5) 0.4062(5) 0.2925(7) 0.078(3) Uani 1 1 d . . . . .
H7 H 0.4477 0.4268 0.3181 0.094 Uiso 1 1 calc R U . . .
O1 O 0.5338(4) 0.2591(4) 0.3138(5) 0.078(2) Uani 1 1 d . . . . .
O2 O 0.5112(4) 0.3663(4) 0.1754(5) 0.089(2) Uani 1 1 d . U . . .
O3 O 0.6174(5) 0.4344(5) 0.2283(7) 0.128(4) Uani 1 1 d . U . . .
H3B H 0.6015 0.4365 0.1816 0.193 Uiso 1 1 d R U . . .
H3C H 0.6141 0.4706 0.2465 0.193 Uiso 1 1 d R U . . .
O4 O 0.7080(4) 0.3497(5) 0.2366(6) 0.105(3) Uani 1 1 d . U . . .
H4A H 0.7047 0.3464 0.1848 0.157 Uiso 1 1 d R U . . .
H4B H 0.7102 0.3882 0.2414 0.157 Uiso 1 1 d R U . . .
Cl3 Cl 0.7564(6) 0.4728(5) 0.2288(7) 0.300(6) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.346(18) . ?
C1 C2 1.38(2) . ?
C2 C3 1.23(2) . ?
C3 C4 1.44(3) . ?
C4 C5 1.41(2) . ?
C5 N1 1.310(19) . ?
C5 C6 1.445(18) . ?
C6 N2 1.285(15) . ?
C7 O1 1.243(13) . ?
C7 N3 1.337(14) . ?
C7 C8 1.484(16) . ?
C8 N4 1.315(14) . ?
C8 C9 1.343(17) . ?
C9 C10 1.35(2) . ?
C10 C11 1.39(2) . ?
C11 C12 1.375(19) . ?
C12 N4 1.307(14) . ?
C12 C19 1.501(18) 7_566 ?
C13 N5 1.328(16) . ?
C13 C14 1.36(2) . ?
C14 C15 1.32(2) . ?
C15 C16 1.44(2) . ?
C16 C17 1.32(2) . ?
C17 N5 1.380(18) . ?
C17 C18 1.433(17) . ?
C18 N6 1.232(16) . ?
C19 O2 1.226(14) . ?
C19 N7 1.343(17) . ?
C19 C12 1.501(18) 8_656 ?
Cl1 Dy1 2.710(3) . ?
Dy1 O4 2.387(9) . ?
Dy1 O3 2.392(11) . ?
Dy1 O1 2.416(8) . ?
Dy1 O2 2.416(9) . ?
Dy1 N2 2.530(10) . ?
Dy1 N5 2.558(12) . ?
Dy1 N6 2.559(11) . ?
Dy1 N1 2.581(12) . ?
N2 N3 1.352(12) . ?
N6 N7 1.341(13) . ?

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 121.5(18) . . ?
C3 C2 C1 118.6(19) . . ?
C2 C3 C4 126(2) . . ?
C5 C4 C3 111.1(18) . . ?
N1 C5 C4 123.9(15) . . ?
N1 C5 C6 118.2(13) . . ?
C4 C5 C6 117.8(16) . . ?
N2 C6 C5 115.7(14) . . ?
O1 C7 N3 122.9(10) . . ?
O1 C7 C8 120.3(10) . . ?
N3 C7 C8 116.8(10) . . ?
N4 C8 C9 123.6(12) . . ?
N4 C8 C7 117.2(10) . . ?
C9 C8 C7 119.2(11) . . ?
C8 C9 C10 119.5(15) . . ?
C9 C10 C11 118.6(16) . . ?
C12 C11 C10 116.8(15) . . ?
N4 C12 C11 124.2(13) . . ?
N4 C12 C19 118.7(11) . 7_566 ?
C11 C12 C19 117.1(12) . 7_566 ?
N5 C13 C14 122.3(16) . . ?
C15 C14 C13 120.5(17) . . ?
C14 C15 C16 118.1(16) . . ?
C17 C16 C15 119.4(16) . . ?
C16 C17 N5 121.4(14) . . ?
C16 C17 C18 123.5(15) . . ?
N5 C17 C18 115.0(13) . . ?
N6 C18 C17 120.9(13) . . ?
O2 C19 N7 121.9(12) . . ?
O2 C19 C12 122.4(13) . 8_656 ?
N7 C19 C12 115.6(10) . 8_656 ?
O4 Dy1 O3 69.5(4) . . ?
O4 Dy1 O1 138.3(3) . . ?
O3 Dy1 O1 137.7(3) . . ?
O4 Dy1 O2 135.6(3) . . ?
O3 Dy1 O2 74.2(4) . . ?
O1 Dy1 O2 86.1(3) . . ?
O4 Dy1 N2 126.7(3) . . ?
O3 Dy1 N2 134.5(4) . . ?
O1 Dy1 N2 62.8(3) . . ?
O2 Dy1 N2 67.0(3) . . ?
O4 Dy1 N5 79.5(4) . . ?
O3 Dy1 N5 89.0(4) . . ?
O1 Dy1 N5 72.0(3) . . ?
O2 Dy1 N5 124.9(3) . . ?
N2 Dy1 N5 132.6(3) . . ?
O4 Dy1 N6 124.6(3) . . ?
O3 Dy1 N6 70.9(4) . . ?
O1 Dy1 N6 66.8(3) . . ?
O2 Dy1 N6 62.3(3) . . ?
N2 Dy1 N6 108.6(3) . . ?
N5 Dy1 N6 62.6(3) . . ?
O4 Dy1 N1 80.7(4) . . ?
O3 Dy1 N1 84.0(4) . . ?
O1 Dy1 N1 124.6(3) . . ?
O2 Dy1 N1 70.7(3) . . ?
N2 Dy1 N1 61.8(4) . . ?
N5 Dy1 N1 160.3(4) . . ?
N6 Dy1 N1 131.0(3) . . ?
O4 Dy1 Cl1 70.5(3) . . ?
O3 Dy1 Cl1 140.0(3) . . ?
O1 Dy1 Cl1 76.6(2) . . ?
O2 Dy1 Cl1 139.6(2) . . ?
N2 Dy1 Cl1 72.6(2) . . ?
N5 Dy1 Cl1 84.1(2) . . ?
N6 Dy1 Cl1 136.2(3) . . ?
N1 Dy1 Cl1 89.5(2) . . ?
C5 N1 C1 118.7(14) . . ?
C5 N1 Dy1 119.3(9) . . ?
C1 N1 Dy1 121.5(12) . . ?
C6 N2 N3 118.5(11) . . ?
C6 N2 Dy1 123.9(9) . . ?
N3 N2 Dy1 117.5(7) . . ?
C7 N3 N2 114.5(9) . . ?
C12 N4 C8 117.2(11) . . ?
C13 N5 C17 118.2(13) . . ?
C13 N5 Dy1 122.3(10) . . ?
C17 N5 Dy1 119.4(8) . . ?
C18 N6 N7 121.4(12) . . ?
C18 N6 Dy1 121.9(9) . . ?
N7 N6 Dy1 116.7(8) . . ?
N6 N7 C19 115.6(10) . . ?
C7 O1 Dy1 121.7(7) . . ?
C19 O2 Dy1 123.3(9) . . ?

_refine_diff_density_max         2.229
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.187



