# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2021

####################################################################### 
# 
# 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_20180302c
_database_code_depnum_ccdc_archive 'CCDC 2109922'
loop_
_audit_author_name
_audit_author_address
'Hao-Ling Sun'
;Beijing Normal University
China
;
_audit_update_record             
;
2021-09-15 deposited with the CCDC.	2021-11-08 downloaded from the CCDC.
;
_audit_creation_date             2021-09-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.25(C248 H240 Dy16 Fe4 N72 O64), 5(H3.2 O1.6), Cl'
_chemical_formula_sum            'C62 H76 Cl Dy4 Fe N18 O24'
_chemical_formula_weight         2198.70
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 O1 N1 Dy1 Cl1 K1 Fe1 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -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'

_cell_length_a                   19.6086(4)
_cell_length_b                   19.6086(4)
_cell_length_c                   20.2453(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7784.3(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9705
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.7640
_cell_measurement_theta_min      4.4930
_shelx_estimated_absorpt_T_max   0.397
_shelx_estimated_absorpt_T_min   0.093
_exptl_absorpt_coefficient_mu    22.665
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4292
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26592
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.109
_diffrn_reflns_theta_min         4.510
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -123.00 -34.00   1.00    1.50    --  -39.74 178.00 -60.00   89
  2  ω   -110.00 -12.00   1.00    1.50    --  -39.74 -57.00  90.00   98
  3  ω   -113.00 -35.00   1.00    1.50    --  -39.74-178.00-150.00   78
  4  ω   -115.00  -7.00   1.00    1.50    --  -39.74 -77.00-150.00  108
  5  ω     94.00 178.00   1.00   14.00    --  107.19 125.00 150.00   84
  6  ω     55.00 113.00   1.00   14.00    --  107.19-125.00 -90.00   58
  7  ω     99.00 146.00   1.00   14.00    --  107.19 125.00-150.00   47
  8  ω     28.00  97.00   1.00   14.00    --  107.19 -94.00  90.00   69
  9  ω     82.00 178.00   1.00   14.00    --  107.19  30.00 -30.00   96
 10  ω     92.00 172.00   1.00   14.00    --  107.19  61.00  30.00   80
 11  ω    115.00 142.00   1.00   14.00    --  107.19 125.00 120.00   27
 12  ω     86.00 120.00   1.00   14.00    --  107.19-125.00  30.00   34
 13  ω     26.00  99.00   1.00   14.00    --  107.19 -94.00 150.00   73
 14  ω    109.00 178.00   1.00   14.00    --  107.19  30.00 -90.00   69
 15  ω     37.00 131.00   1.00   14.00    --  107.19 -61.00-120.00   94
 16  ω     62.00 133.00   1.00   14.00    --  107.19 -45.00  90.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0156516000
_diffrn_orient_matrix_UB_12      0.0746348000
_diffrn_orient_matrix_UB_13      -0.0182812000
_diffrn_orient_matrix_UB_21      -0.0759734000
_diffrn_orient_matrix_UB_22      0.0181856000
_diffrn_orient_matrix_UB_23      0.0085679000
_diffrn_orient_matrix_UB_31      0.0127178000
_diffrn_orient_matrix_UB_32      0.0163865000
_diffrn_orient_matrix_UB_33      0.0733311000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3515
_reflns_number_total             3872
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3872
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0318
_refine_ls_restrained_S_all      1.065
_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)+(0.0367P)²+28.9712P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0813
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 C16-H3
 1.891468 with sigma of 0.02
 Dy1-H3
 2.905263 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl6 \\sim O7 \\sim O8: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(Cl6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O8) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 0.0002
4. Others
 Sof(O7)=Sof(H7A)=Sof(H7B)=1-FVAR(1)
 Sof(O8)=Sof(H8A)=Sof(H8B)=FVAR(1)
 Fixed Sof: Cl6(0.25)
5.a Riding coordinates:
 O8(H8A,H8B)
5.b Free rotating group:
 O5(H5A,H5B), O7(H7A,H7B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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
Dy1 Dy 0.22538(2) 0.26968(2) 0.34289(2) 0.02286(9) Uani 1 1 d D . . . .
Fe1 Fe 0.500000 0.250000 0.375000 0.0203(2) Uani 1 4 d S T P . .
O1 O 0.19025(14) 0.31644(15) 0.43591(13) 0.0317(6) Uani 1 1 d . . . . .
O2 O 0.28061(12) 0.30689(13) 0.24420(12) 0.0243(5) Uani 1 1 d . . . . .
O3 O 0.13036(13) 0.32782(15) 0.29489(14) 0.0318(6) Uani 1 1 d D . . . .
H3 H 0.0930(10) 0.3062(14) 0.290(2) 0.048 Uiso 1 1 d DR . . . .
O4 O 0.24226(17) 0.16774(17) 0.41008(16) 0.0346(6) Uani 1 1 d . . . . .
O5 O 0.1758(2) 0.2033(2) 0.52243(19) 0.0587(10) Uani 1 1 d . . . . .
H5A H 0.181631 0.243973 0.509137 0.088 Uiso 1 1 d G . . . .
H5B H 0.139133 0.201323 0.545039 0.088 Uiso 1 1 d G . . . .
N1 N 0.37757(15) 0.30884(16) 0.15346(14) 0.0244(6) Uani 1 1 d . . . . .
N2 N 0.32416(16) 0.40261(17) 0.29593(15) 0.0271(6) Uani 1 1 d . . . . .
N3 N 0.27250(16) 0.38724(17) 0.34306(15) 0.0265(7) Uani 1 1 d . . . . .
N4 N 0.34409(16) 0.25487(18) 0.36573(17) 0.0301(7) Uani 1 1 d . . . . .
N5 N 0.500000 0.250000 0.5261(2) 0.0366(11) Uani 1 2 d S T P . .
C1 C 0.1794(2) 0.3776(2) 0.4607(2) 0.0341(9) Uani 1 1 d . . . . .
C2 C 0.1357(3) 0.3851(3) 0.5155(2) 0.0506(13) Uani 1 1 d . . . . .
H2 H 0.113360 0.346890 0.532026 0.061 Uiso 1 1 calc R . . . .
C3 C 0.1251(4) 0.4473(3) 0.5451(3) 0.075(2) Uani 1 1 d . . . . .
H3A H 0.096497 0.450357 0.581568 0.090 Uiso 1 1 calc R . . . .
C4 C 0.1565(4) 0.5054(3) 0.5213(3) 0.078(2) Uani 1 1 d . . . . .
H4 H 0.149110 0.547315 0.541544 0.093 Uiso 1 1 calc R . . . .
C5 C 0.1991(3) 0.5005(3) 0.4672(3) 0.0549(14) Uani 1 1 d . . . . .
H5 H 0.220416 0.539486 0.451046 0.066 Uiso 1 1 calc R . . . .
C6 C 0.2108(2) 0.4374(2) 0.4360(2) 0.0365(9) Uani 1 1 d . . . . .
C7 C 0.2590(2) 0.4382(2) 0.3812(2) 0.0324(8) Uani 1 1 d . . . . .
H7 H 0.281881 0.478858 0.373055 0.039 Uiso 1 1 calc R . . . .
C8 C 0.32395(17) 0.35795(19) 0.24847(17) 0.0232(7) Uani 1 1 d . . . . .
C9 C 0.37726(18) 0.3617(2) 0.19561(18) 0.0258(7) Uani 1 1 d . . . . .
C10 C 0.4228(2) 0.4151(2) 0.1905(2) 0.0318(8) Uani 1 1 d . . . . .
H10 H 0.420976 0.451266 0.220137 0.038 Uiso 1 1 calc R . . . .
C11 C 0.4714(2) 0.4141(2) 0.1404(2) 0.0360(9) Uani 1 1 d . . . . .
H11 H 0.502395 0.449651 0.135943 0.043 Uiso 1 1 calc R . . . .
C12 C 0.4728(2) 0.3593(2) 0.09751(19) 0.0332(9) Uani 1 1 d . . . . .
H12 H 0.505063 0.357003 0.063926 0.040 Uiso 1 1 calc R . . . .
C13 C 0.4248(2) 0.3077(2) 0.10568(19) 0.0301(8) Uani 1 1 d . . . . .
H13 H 0.425597 0.270883 0.076747 0.036 Uiso 1 1 calc R . . . .
C14 C 0.4025(2) 0.25232(18) 0.37150(18) 0.0270(7) Uani 1 1 d . . . . .
C15 C 0.500000 0.250000 0.4698(3) 0.0282(11) Uani 1 2 d S T P . .
C16 C 0.1276(2) 0.3879(2) 0.2551(2) 0.0417(10) Uani 1 1 d D . . . .
H16A H 0.149711 0.379356 0.213579 0.063 Uiso 1 1 calc GR . . . .
H16B H 0.150253 0.424560 0.277444 0.063 Uiso 1 1 calc GR . . . .
H16C H 0.080798 0.400018 0.247350 0.063 Uiso 1 1 calc GR . . . .
O7 O 0.0543(6) 0.1698(7) 0.5667(5) 0.112(4) Uani 0.600(11) 1 d . U . A 1
H7A H 0.093490 0.188286 0.566047 0.169 Uiso 0.600(11) 1 d G . . A 1
H7B H 0.034224 0.188138 0.599414 0.169 Uiso 0.600(11) 1 d G . . A 1
Cl6 Cl 0.0115(4) 0.2385(4) 0.5586(3) 0.0654(15) Uani 0.25 1 d . U . A -1
O8 O 0.0470(9) 0.0970(9) 0.5779(8) 0.106(4) Uani 0.400(11) 1 d . U . A 2
H8A H 0.033434 0.095788 0.617781 0.159 Uiso 0.400(11) 1 d R . . A 2
H8B H 0.086874 0.080288 0.575381 0.159 Uiso 0.400(11) 1 d R . . A 2
H4A H 0.279(3) 0.151(3) 0.419(3) 0.053(17) Uiso 1 1 d . . . . .
H4B H 0.223(4) 0.167(4) 0.444(4) 0.07(2) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Dy1 3.9591(4) 13 ?
Dy1 O1 2.205(3) . ?
Dy1 O2 2.319(2) 13 ?
Dy1 O2 2.387(2) . ?
Dy1 O3 2.391(3) . ?
Dy1 O4 2.440(3) . ?
Dy1 N1 2.540(3) 13 ?
Dy1 N3 2.483(3) . ?
Dy1 N4 2.391(3) . ?
Fe1 C14 1.914(4) 6_554 ?
Fe1 C14 1.914(4) 16_656 ?
Fe1 C14 1.914(4) . ?
Fe1 C14 1.914(4) 11_666 ?
Fe1 C15 1.919(6) . ?
Fe1 C15 1.919(6) 11_666 ?
O1 C1 1.318(5) . ?
O2 C8 1.316(4) . ?
O3 H3 0.852(9) . ?
O3 C16 1.428(5) . ?
O4 H4A 0.81(7) . ?
O4 H4B 0.78(8) . ?
O5 H5A 0.8503 . ?
O5 H5B 0.8529 . ?
N1 C9 1.342(5) . ?
N1 C13 1.340(5) . ?
N2 N3 1.424(4) . ?
N2 C8 1.300(5) . ?
N3 C7 1.291(5) . ?
N4 C14 1.153(5) . ?
N5 C15 1.139(8) . ?
C1 C2 1.409(6) . ?
C1 C6 1.415(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.376(7) . ?
C3 H3A 0.9300 . ?
C3 C4 1.381(9) . ?
C4 H4 0.9300 . ?
C4 C5 1.382(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.408(6) . ?
C6 C7 1.456(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.498(5) . ?
C9 C10 1.380(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.392(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.381(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.391(6) . ?
C13 H13 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
O7 H7A 0.8498 . ?
O7 H7B 0.8499 . ?
O7 Cl6 1.596(16) . ?
O8 H8A 0.8507 . ?
O8 H8B 0.8499 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 Dy1 165.62(8) . 13 ?
O1 Dy1 O2 154.54(10) . 13 ?
O1 Dy1 O2 136.85(10) . . ?
O1 Dy1 O3 84.57(10) . . ?
O1 Dy1 O4 84.66(11) . . ?
O1 Dy1 N1 88.79(10) . 13 ?
O1 Dy1 N3 74.28(10) . . ?
O1 Dy1 N4 100.92(11) . . ?
O2 Dy1 Dy1 33.25(6) 13 13 ?
O2 Dy1 Dy1 32.19(6) . 13 ?
O2 Dy1 O2 65.44(11) 13 . ?
O2 Dy1 O3 87.72(9) 13 . ?
O2 Dy1 O3 82.39(9) . . ?
O2 Dy1 O4 84.28(10) 13 . ?
O2 Dy1 O4 130.96(10) . . ?
O2 Dy1 N1 124.77(9) . 13 ?
O2 Dy1 N1 65.76(9) 13 13 ?
O2 Dy1 N3 128.38(9) 13 . ?
O2 Dy1 N3 63.17(9) . . ?
O2 Dy1 N4 75.96(10) . . ?
O2 Dy1 N4 96.76(10) 13 . ?
O3 Dy1 Dy1 84.08(7) . 13 ?
O3 Dy1 O4 136.29(10) . . ?
O3 Dy1 N1 71.42(10) . 13 ?
O3 Dy1 N3 81.25(10) . . ?
O4 Dy1 Dy1 109.68(8) . 13 ?
O4 Dy1 N1 66.11(10) . 13 ?
O4 Dy1 N3 135.16(10) . . ?
N1 Dy1 Dy1 95.93(7) 13 13 ?
N3 Dy1 Dy1 95.25(7) . 13 ?
N3 Dy1 N1 149.12(10) . 13 ?
N4 Dy1 Dy1 85.56(8) . 13 ?
N4 Dy1 O3 153.55(11) . . ?
N4 Dy1 O4 70.17(11) . . ?
N4 Dy1 N1 133.99(11) . 13 ?
N4 Dy1 N3 75.54(11) . . ?
C14 Fe1 C14 90.079(9) 16_656 . ?
C14 Fe1 C14 90.078(9) 11_666 . ?
C14 Fe1 C14 175.8(2) 11_666 16_656 ?
C14 Fe1 C14 90.079(8) 6_554 16_656 ?
C14 Fe1 C14 175.8(2) 6_554 . ?
C14 Fe1 C14 90.079(9) 11_666 6_554 ?
C14 Fe1 C15 87.88(11) 11_666 . ?
C14 Fe1 C15 92.12(11) . . ?
C14 Fe1 C15 87.88(11) 16_656 . ?
C14 Fe1 C15 87.88(11) 6_554 11_666 ?
C14 Fe1 C15 92.12(11) 11_666 11_666 ?
C14 Fe1 C15 92.12(11) 6_554 . ?
C14 Fe1 C15 92.12(11) 16_656 11_666 ?
C14 Fe1 C15 87.88(11) . 11_666 ?
C15 Fe1 C15 180.0 . 11_666 ?
C1 O1 Dy1 139.0(3) . . ?
Dy1 O2 Dy1 114.55(11) 13 . ?
C8 O2 Dy1 118.1(2) . . ?
C8 O2 Dy1 125.1(2) . 13 ?
Dy1 O3 H3 118.6(14) . . ?
C16 O3 Dy1 130.8(2) . . ?
C16 O3 H3 108.3(14) . . ?
Dy1 O4 H4A 125(4) . . ?
Dy1 O4 H4B 116(5) . . ?
H4A O4 H4B 104(6) . . ?
H5A O5 H5B 109.0 . . ?
C9 N1 Dy1 116.5(2) . 13 ?
C13 N1 Dy1 124.1(3) . 13 ?
C13 N1 C9 118.4(3) . . ?
C8 N2 N3 110.5(3) . . ?
N2 N3 Dy1 117.4(2) . . ?
C7 N3 Dy1 130.0(3) . . ?
C7 N3 N2 112.5(3) . . ?
C14 N4 Dy1 173.0(3) . . ?
O1 C1 C2 119.5(4) . . ?
O1 C1 C6 123.3(4) . . ?
C2 C1 C6 117.2(4) . . ?
C1 C2 H2 119.1 . . ?
C3 C2 C1 121.8(5) . . ?
C3 C2 H2 119.1 . . ?
C2 C3 H3A 119.6 . . ?
C2 C3 C4 120.8(5) . . ?
C4 C3 H3A 119.6 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.3(5) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.0(5) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C7 124.1(4) . . ?
C5 C6 C1 119.9(4) . . ?
C5 C6 C7 115.9(4) . . ?
N3 C7 C6 125.5(4) . . ?
N3 C7 H7 117.3 . . ?
C6 C7 H7 117.3 . . ?
O2 C8 C9 116.2(3) . . ?
N2 C8 O2 124.3(3) . . ?
N2 C8 C9 119.5(3) . . ?
N1 C9 C8 114.8(3) . . ?
N1 C9 C10 122.4(3) . . ?
C10 C9 C8 122.8(4) . . ?
C9 C10 H10 120.4 . . ?
C9 C10 C11 119.1(4) . . ?
C11 C10 H10 120.4 . . ?
C10 C11 H11 120.6 . . ?
C12 C11 C10 118.9(4) . . ?
C12 C11 H11 120.6 . . ?
C11 C12 H12 120.8 . . ?
C11 C12 C13 118.5(4) . . ?
C13 C12 H12 120.8 . . ?
N1 C13 C12 122.8(4) . . ?
N1 C13 H13 118.6 . . ?
C12 C13 H13 118.6 . . ?
N4 C14 Fe1 176.1(4) . . ?
N5 C15 Fe1 180.0 . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
H7A O7 H7B 104.5 . . ?
Cl6 O7 H7A 96.5 . . ?
Cl6 O7 H7B 58.6 . . ?
H8A O8 H8B 109.4 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.733
_oxdiff_exptl_absorpt_empirical_full_min 0.644
####################################################################### 
# 
# 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_20180320a
_database_code_depnum_ccdc_archive 'CCDC 2109925'
loop_
_audit_author_name
_audit_author_address
'Hao-Ling Sun'
;Beijing Normal University
China
;
_audit_update_record             
;
2021-09-15 deposited with the CCDC.	2021-11-08 downloaded from the CCDC.
;
_audit_creation_date             2021-09-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.25(C248 H240 Co4 Dy16 N72 O64), 4(C H4 O), Br'
_chemical_formula_sum            'C66 H76 Br Co Dy4 N18 O20'
_chemical_formula_weight         2230.28
_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 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -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'

_cell_length_a                   19.83570(10)
_cell_length_b                   19.83570(10)
_cell_length_c                   19.0251(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7485.52(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13635
_cell_measurement_temperature    293.00(10)
_cell_measurement_theta_max      73.0410
_cell_measurement_theta_min      4.4550
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    24.002
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_density_diffrn    1.979
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4336
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24817
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.267
_diffrn_reflns_theta_min         4.458
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -46.00  -4.00   1.00    1.00    --  -41.49 125.00 120.00   42
  2  ω   -107.00 -81.00   1.00    1.00    --  -41.49 -37.00-120.00   26
  3  ω   -114.00 -27.00   1.00    1.00    --  -41.49 -37.00 -90.00   87
  4  ω    -48.00  33.00   1.00    1.00    --  -41.49  37.00  60.00   81
  5  ω     33.00  98.00   1.00    1.00    --   41.49-125.00 120.00   65
  6  ω     26.00  72.00   1.00    1.00    --   41.49-125.00 -60.00   46
  7  ω      1.00  27.00   1.00    1.00    --   41.49 -99.00 150.00   26
  8  ω     95.00 153.00   1.00    9.00    --  107.19 125.00-150.00   58
  9  ω    103.00 143.00   1.00    9.00    --  107.19  30.00  90.00   40
 10  ω     68.00 120.00   1.00    9.00    --  107.19-125.00 -90.00   52
 11  ω     29.00 105.00   1.00    9.00    --  107.19 -94.00 120.00   76
 12  ω     40.00 133.00   1.00    9.00    --  107.19 -45.00 120.00   93
 13  ω     26.00 104.00   1.00    9.00    --  107.19 -94.00  30.00   78
 14  ω     91.00 129.00   1.00    9.00    --  107.19 -45.00 -60.00   38
 15  ω     69.00 172.00   1.00    9.00    --  107.19  15.00-150.00  103
 16  ω     58.00 106.00   1.00    9.00    --  107.19 -94.00 -60.00   48
 17  ω     39.00 130.00   1.00    9.00    --  107.19 -45.00-150.00   91
 18  ω     43.00  72.00   1.00    9.00    --  107.19 -45.00 -60.00   29
 19  ω    101.00 172.00   1.00    9.00    --  107.19  77.00 -90.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3402
_reflns_number_total             3732
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         3732
_refine_ls_number_restraints     95
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0245
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0300P)²+12.5584P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0563
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 O6-C19
 1.4 with sigma of 0.02
 C16-H3
 1.882179 with sigma of 0.02
 Dy1-H3
 2.902246 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O6 \\sim C19 \\sim O7 \\sim C18 \\sim O5 \\sim C17: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 0.0002
4. Others
 1*[Sof(O6)+Sof(H6)+Sof(C19)+Sof(H19A)+Sof(H19B)+Sof(H19C)]+1*[Sof(O7)+
 Sof(H7A)+Sof(C18)+Sof(H18A)+Sof(H18B)+Sof(H18C)]+1*[Sof(O5)+Sof(H5A)+Sof(C17)+
 Sof(H17A)+Sof(H17B)+Sof(H17C)]=1 with esd of 0.0001
 Sof(O6)=Sof(H6)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Sof(O7)=Sof(H7A)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(2)
 Sof(O5)=Sof(H5A)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(3)
 Fixed Sof: Br1(0.25)
5.a Rotating group:
 O4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
5.d Idealised tetrahedral OH refined as rotating group:
 O6(H6), O5(H5A), O7(H7A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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
Dy1 Dy 0.23118(2) 0.72068(2) 0.65287(2) 0.01113(6) Uani 1 1 d D . . . .
Co1 Co 0.500000 0.750000 0.625000 0.00768(15) Uani 1 4 d S T P . .
O2 O 0.28192(9) 0.69435(9) 0.76433(9) 0.0125(4) Uani 1 1 d . . . . .
O1 O 0.20021(11) 0.66126(11) 0.56173(11) 0.0217(4) Uani 1 1 d . . . . .
O3 O 0.13356(10) 0.66936(11) 0.70455(11) 0.0188(4) Uani 1 1 d D . . . .
H3 H 0.0971(8) 0.6917(12) 0.7053(19) 0.028 Uiso 1 1 d DR . . . .
O4 O 0.24969(12) 0.80763(15) 0.56312(15) 0.0391(7) Uani 1 1 d . . . . .
H4A H 0.288484 0.825476 0.569038 0.059 Uiso 1 1 d GR . . . .
H4B H 0.222121 0.840176 0.569541 0.059 Uiso 1 1 d GR . . . .
N1 N 0.37072(11) 0.70522(12) 0.86639(12) 0.0137(4) Uani 1 1 d . . . . .
N2 N 0.33325(12) 0.59940(12) 0.71944(12) 0.0151(5) Uani 1 1 d . . . . .
N3 N 0.28220(12) 0.60630(12) 0.66782(12) 0.0139(5) Uani 1 1 d . . . . .
N4 N 0.34871(12) 0.74160(12) 0.63649(13) 0.0160(5) Uani 1 1 d . . . . .
N5 N 0.500000 0.750000 0.46566(19) 0.0228(8) Uani 1 2 d S T P . .
C1 C 0.18558(15) 0.59766(16) 0.54798(15) 0.0198(6) Uani 1 1 d . . . . .
C2 C 0.13585(18) 0.58229(18) 0.49725(17) 0.0282(7) Uani 1 1 d . . . . .
H2 H 0.113141 0.617173 0.474749 0.034 Uiso 1 1 calc R . . . .
C3 C 0.12041(19) 0.5162(2) 0.48053(19) 0.0337(8) Uani 1 1 d . . . . .
H3A H 0.086666 0.507450 0.447846 0.040 Uiso 1 1 calc R . . . .
C4 C 0.15452(19) 0.46238(19) 0.5118(2) 0.0343(8) Uani 1 1 d . . . . .
H4 H 0.144590 0.418158 0.499268 0.041 Uiso 1 1 calc R . . . .
C5 C 0.20309(18) 0.47601(17) 0.56144(18) 0.0270(7) Uani 1 1 d . . . . .
H5 H 0.225898 0.440439 0.582624 0.032 Uiso 1 1 calc R . . . .
C6 C 0.21901(15) 0.54258(16) 0.58088(15) 0.0194(6) Uani 1 1 d . . . . .
C7 C 0.26952(15) 0.55056(15) 0.63536(15) 0.0181(6) Uani 1 1 d . . . . .
H7 H 0.294592 0.512792 0.647827 0.022 Uiso 1 1 calc R . . . .
C8 C 0.32835(13) 0.64759(13) 0.76545(14) 0.0126(5) Uani 1 1 d . . . . .
C9 C 0.37838(14) 0.65135(14) 0.82427(14) 0.0140(5) Uani 1 1 d . . . . .
C10 C 0.42856(16) 0.60353(15) 0.83551(17) 0.0212(6) Uani 1 1 d . . . . .
H10 H 0.433067 0.566638 0.805712 0.025 Uiso 1 1 calc R . . . .
C11 C 0.47185(16) 0.61217(17) 0.89234(17) 0.0240(7) Uani 1 1 d . . . . .
H11 H 0.506104 0.581209 0.900805 0.029 Uiso 1 1 calc R . . . .
C12 C 0.46356(15) 0.66683(17) 0.93587(16) 0.0226(6) Uani 1 1 d . . . . .
H12 H 0.491618 0.673128 0.974475 0.027 Uiso 1 1 calc R . . . .
C13 C 0.41283(15) 0.71211(16) 0.92112(15) 0.0181(6) Uani 1 1 d . . . . .
H13 H 0.407513 0.749213 0.950491 0.022 Uiso 1 1 calc R . . . .
C14 C 0.40565(15) 0.74550(13) 0.62932(13) 0.0136(5) Uani 1 1 d . . . . .
C15 C 0.500000 0.750000 0.5261(2) 0.0141(7) Uani 1 2 d S T P . .
C16 C 0.12465(18) 0.60964(17) 0.7450(2) 0.0301(7) Uani 1 1 d D . . . .
H16A H 0.153546 0.574807 0.727108 0.045 Uiso 1 1 calc GR . . . .
H16B H 0.078539 0.595239 0.741951 0.045 Uiso 1 1 calc GR . . . .
H16C H 0.135866 0.618602 0.793176 0.045 Uiso 1 1 calc GR . . . .
O6 O 0.1905(19) 0.7701(15) 0.432(2) 0.041(4) Uani 0.175(3) 1 d D U . A 1
H6 H 0.153779 0.762193 0.450107 0.061 Uiso 0.175(3) 1 calc GR . . A 1
C19 C 0.2145(16) 0.7120(14) 0.3990(16) 0.043(5) Uani 0.175(3) 1 d D U . A 1
H19A H 0.218545 0.720012 0.349409 0.064 Uiso 0.175(3) 1 calc GR . . A 1
H19B H 0.183679 0.675464 0.406951 0.064 Uiso 0.175(3) 1 calc GR . . A 1
H19C H 0.257922 0.700450 0.417881 0.064 Uiso 0.175(3) 1 calc GR . . A 1
O5 O 0.2043(4) 0.7569(4) 0.4512(4) 0.037(2) Uani 0.438(3) 1 d . U . B 3
H5A H 0.199514 0.726048 0.479432 0.056 Uiso 0.438(3) 1 calc GR . . B 3
C17 C 0.1495(6) 0.7566(7) 0.4027(6) 0.052(2) Uani 0.438(3) 1 d . U . B 3
H17A H 0.156362 0.721692 0.368452 0.078 Uiso 0.438(3) 1 calc GR . . B 3
H17B H 0.146965 0.799453 0.379442 0.078 Uiso 0.438(3) 1 calc GR . . B 3
H17C H 0.108141 0.748347 0.427526 0.078 Uiso 0.438(3) 1 calc GR . . B 3
O7 O 0.1794(5) 0.7934(5) 0.4298(5) 0.039(2) Uani 0.387(3) 1 d . U . C 2
H7A H 0.141441 0.808081 0.422152 0.058 Uiso 0.387(3) 1 calc GR . . C 2
C18 C 0.1868(8) 0.7289(8) 0.3967(7) 0.046(3) Uani 0.387(3) 1 d . U . C 2
H18A H 0.208537 0.698279 0.428503 0.069 Uiso 0.387(3) 1 calc GR . . C 2
H18B H 0.213766 0.733635 0.355010 0.069 Uiso 0.387(3) 1 calc GR . . C 2
H18C H 0.143223 0.711650 0.384251 0.069 Uiso 0.387(3) 1 calc GR . . C 2
Br1 Br -0.02237(8) 0.70969(9) 0.37125(8) 0.0380(3) Uani 0.25 1 d . . . D -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Dy1 3.9458(3) 13_566 ?
Dy1 O2 2.3216(18) 13_566 ?
Dy1 O2 2.4046(18) . ?
Dy1 O1 2.1847(19) . ?
Dy1 O3 2.3985(19) . ?
Dy1 O4 2.455(2) . ?
Dy1 N1 2.526(2) 13_566 ?
Dy1 N3 2.501(2) . ?
Dy1 N4 2.388(2) . ?
Co1 C14 1.876(3) . ?
Co1 C14 1.876(3) 6_564 ?
Co1 C14 1.876(3) 12_767 ?
Co1 C14 1.876(3) 15_566 ?
Co1 C15 1.882(4) . ?
Co1 C15 1.882(4) 15_566 ?
O2 C8 1.307(3) . ?
O1 C1 1.321(4) . ?
O3 H3 0.848(9) . ?
O3 C16 1.423(4) . ?
O4 H4A 0.8544 . ?
O4 H4B 0.8548 . ?
N1 C9 1.344(4) . ?
N1 C13 1.342(4) . ?
N2 N3 1.417(3) . ?
N2 C8 1.300(4) . ?
N3 C7 1.291(4) . ?
N4 C14 1.140(4) . ?
N5 C15 1.150(6) . ?
C1 C2 1.413(4) . ?
C1 C6 1.423(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.383(5) . ?
C3 H3A 0.9300 . ?
C3 C4 1.397(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.376(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.407(4) . ?
C6 C7 1.450(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.497(4) . ?
C9 C10 1.392(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.391(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.374(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.378(4) . ?
C13 H13 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
O6 H6 0.8200 . ?
O6 C19 1.398(19) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
O5 H5A 0.8200 . ?
O5 C17 1.426(13) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
O7 H7A 0.8200 . ?
O7 C18 1.434(19) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 Dy1 32.74(4) . 13_566 ?
O2 Dy1 Dy1 34.07(5) 13_566 13_566 ?
O2 Dy1 O2 66.81(8) 13_566 . ?
O2 Dy1 O3 86.54(7) 13_566 . ?
O2 Dy1 O4 88.77(9) 13_566 . ?
O2 Dy1 O4 134.70(8) . . ?
O2 Dy1 N1 126.11(7) . 13_566 ?
O2 Dy1 N1 65.57(7) 13_566 13_566 ?
O2 Dy1 N3 62.17(7) . . ?
O2 Dy1 N3 128.81(7) 13_566 . ?
O2 Dy1 N4 94.11(8) 13_566 . ?
O1 Dy1 Dy1 162.87(6) . 13_566 ?
O1 Dy1 O2 153.99(7) . 13_566 ?
O1 Dy1 O2 134.46(7) . . ?
O1 Dy1 O3 82.49(8) . . ?
O1 Dy1 O4 82.48(10) . . ?
O1 Dy1 N1 88.50(8) . 13_566 ?
O1 Dy1 N3 73.42(8) . . ?
O1 Dy1 N4 105.35(8) . . ?
O3 Dy1 Dy1 83.91(5) . 13_566 ?
O3 Dy1 O2 83.35(7) . . ?
O3 Dy1 O4 134.77(7) . . ?
O3 Dy1 N1 70.15(7) . 13_566 ?
O3 Dy1 N3 83.97(7) . . ?
O4 Dy1 Dy1 114.59(8) . 13_566 ?
O4 Dy1 N1 67.04(8) . 13_566 ?
O4 Dy1 N3 131.01(9) . . ?
N1 Dy1 Dy1 96.65(5) 13_566 13_566 ?
N3 Dy1 Dy1 94.84(5) . 13_566 ?
N3 Dy1 N1 150.27(8) . 13_566 ?
N4 Dy1 Dy1 83.47(6) . 13_566 ?
N4 Dy1 O2 75.18(7) . . ?
N4 Dy1 O3 156.25(8) . . ?
N4 Dy1 O4 68.97(8) . . ?
N4 Dy1 N1 131.38(8) . 13_566 ?
N4 Dy1 N3 77.14(8) . . ?
C14 Co1 C14 174.98(16) 12_767 15_566 ?
C14 Co1 C14 90.109(7) . 15_566 ?
C14 Co1 C14 90.110(7) 6_564 12_767 ?
C14 Co1 C14 174.98(16) . 6_564 ?
C14 Co1 C14 90.110(7) 6_564 15_566 ?
C14 Co1 C14 90.111(8) . 12_767 ?
C14 Co1 C15 92.51(8) 6_564 . ?
C14 Co1 C15 92.51(8) 12_767 15_566 ?
C14 Co1 C15 92.51(8) 15_566 15_566 ?
C14 Co1 C15 87.49(8) 6_564 15_566 ?
C14 Co1 C15 87.49(8) 15_566 . ?
C14 Co1 C15 92.51(8) . . ?
C14 Co1 C15 87.49(8) . 15_566 ?
C14 Co1 C15 87.49(8) 12_767 . ?
C15 Co1 C15 180.0 . 15_566 ?
Dy1 O2 Dy1 113.19(8) 13_566 . ?
C8 O2 Dy1 125.65(16) . 13_566 ?
C8 O2 Dy1 117.61(16) . . ?
C1 O1 Dy1 137.2(2) . . ?
Dy1 O3 H3 118.2(13) . . ?
C16 O3 Dy1 132.45(19) . . ?
C16 O3 H3 108.7(13) . . ?
Dy1 O4 H4A 109.5 . . ?
Dy1 O4 H4B 109.6 . . ?
H4A O4 H4B 104.2 . . ?
C9 N1 Dy1 117.81(17) . 13_566 ?
C13 N1 Dy1 123.5(2) . 13_566 ?
C13 N1 C9 118.2(2) . . ?
C8 N2 N3 110.0(2) . . ?
N2 N3 Dy1 117.11(16) . . ?
C7 N3 Dy1 130.1(2) . . ?
C7 N3 N2 112.8(2) . . ?
C14 N4 Dy1 173.8(2) . . ?
O1 C1 C2 119.6(3) . . ?
O1 C1 C6 122.9(3) . . ?
C2 C1 C6 117.4(3) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 C1 121.1(3) . . ?
C3 C2 H2 119.5 . . ?
C2 C3 H3A 119.4 . . ?
C2 C3 C4 121.3(3) . . ?
C4 C3 H3A 119.4 . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.8(3) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 119.3 . . ?
C4 C5 C6 121.5(3) . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C7 123.5(3) . . ?
C5 C6 C1 120.0(3) . . ?
C5 C6 C7 116.4(3) . . ?
N3 C7 C6 124.7(3) . . ?
N3 C7 H7 117.6 . . ?
C6 C7 H7 117.6 . . ?
O2 C8 C9 116.3(2) . . ?
N2 C8 O2 124.3(3) . . ?
N2 C8 C9 119.4(2) . . ?
N1 C9 C8 114.2(2) . . ?
N1 C9 C10 122.1(3) . . ?
C10 C9 C8 123.7(3) . . ?
C9 C10 H10 120.8 . . ?
C11 C10 C9 118.5(3) . . ?
C11 C10 H10 120.8 . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.5(3) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 120.7 . . ?
C11 C12 C13 118.6(3) . . ?
C13 C12 H12 120.7 . . ?
N1 C13 C12 123.1(3) . . ?
N1 C13 H13 118.4 . . ?
C12 C13 H13 118.4 . . ?
N4 C14 Co1 175.5(2) . . ?
N5 C15 Co1 180.0 . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C19 O6 H6 109.5 . . ?
O6 C19 H19A 109.5 . . ?
O6 C19 H19B 109.5 . . ?
O6 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 O5 H5A 109.5 . . ?
O5 C17 H17A 109.5 . . ?
O5 C17 H17B 109.5 . . ?
O5 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C18 O7 H7A 109.5 . . ?
O7 C18 H18A 109.5 . . ?
O7 C18 H18B 109.5 . . ?
O7 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
####################################################################### 
# 
# 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_20181020a
_database_code_depnum_ccdc_archive 'CCDC 2109924'
loop_
_audit_author_name
_audit_author_address
'Hao-Ling Sun'
;Beijing Normal University
China
;
_audit_update_record             
;
2021-09-15 deposited with the CCDC.	2021-11-08 downloaded from the CCDC.
;
_audit_creation_date             2021-09-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.25(C248 H240 Dy16 Fe4 N72 O64), C4 H16 Br O4'
_chemical_formula_sum            'C66 H76 Br Dy4 Fe N18 O20'
_chemical_formula_weight         2227.20
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Dy1 C1 H1 O1 Br1 N1 Fe1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -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'

_cell_length_a                   19.90460(10)
_cell_length_b                   19.90460(10)
_cell_length_c                   19.0126(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7532.66(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14598
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.8580
_cell_measurement_theta_min      4.4290
_shelx_estimated_absorpt_T_max   0.201
_shelx_estimated_absorpt_T_min   0.067
_exptl_absorpt_coefficient_mu    23.672
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4332
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26178
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.983
_diffrn_reflns_theta_min         4.443
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -85.00 -52.00   1.00    1.00    --  -41.49 125.00  60.00   33
  2  ω    -66.00  31.00   1.00    1.00    --  -41.49  57.00   0.00   97
  3  ω    -63.00  33.00   1.00    1.00    --  -41.49  37.00 150.00   96
  4  ω   -110.00 -18.00   1.00    1.00    --  -41.49 -57.00-150.00   92
  5  ω      2.00  29.00   1.00    1.00    --   41.49 -99.00-180.00   27
  6  ω     68.00 108.00   1.00   10.00    --  104.69 -94.00-180.00   40
  7  ω     24.00 152.00   1.00   10.00    --  104.69 -15.00 -30.00  128
  8  ω     36.00 132.00   1.00   10.00    --  104.69 -30.00 120.00   96
  9  ω     76.00 118.00   1.00   10.00    --  104.69-125.00 150.00   42
 10  ω     58.00  84.00   1.00   10.00    --  104.69 -61.00-120.00   26
 11  ω     91.00 170.00   1.00   10.00    --  104.69  45.00 150.00   79
 12  ω     91.00 137.00   1.00   10.00    --  104.69 -77.00 150.00   46
 13  ω     23.00 105.00   1.00   10.00    --  104.69 -94.00   0.00   82
 14  ω     29.00  76.00   1.00   10.00    --  104.69 -77.00 150.00   47
 15  ω    142.00 175.00   1.00   10.00    --  104.69  61.00  60.00   33
 16  ω     31.00 116.00   1.00   10.00    --  104.69-125.00   0.00   85
 17  ω     32.00 131.00   1.00   10.00    --  104.69 -61.00   0.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0506518000
_diffrn_orient_matrix_UB_12      -0.0584832000
_diffrn_orient_matrix_UB_13      -0.0015132000
_diffrn_orient_matrix_UB_21      -0.0009581000
_diffrn_orient_matrix_UB_22      0.0010394000
_diffrn_orient_matrix_UB_23      -0.0810477000
_diffrn_orient_matrix_UB_31      0.0584772000
_diffrn_orient_matrix_UB_32      0.0506778000
_diffrn_orient_matrix_UB_33      -0.0000409000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3584
_reflns_number_total             3691
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3691
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0284
_refine_ls_restrained_S_all      1.091
_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)+(0.0295P)²+37.5044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0687
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 O5-C17
 1.35 with sigma of 0.01
 C16-H3
 1.88629 with sigma of 0.02
 Dy1-H3
 2.916851 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: Br1(0.25)
5.a Rotating group:
 O4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C7(H7), C10(H10), C12(H12), C2(H2), C11(H11), C3(H3A), C5(H5), C4(H4)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H1)
5.d Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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
Dy1 Dy 0.23064(2) 0.27929(2) 0.34699(2) 0.01209(8) Uani 1 1 d D . . . .
Fe1 Fe 0.500000 0.250000 0.375000 0.00820(17) Uani 1 4 d S T P . .
O2 O 0.28171(11) 0.30549(11) 0.23576(12) 0.0135(4) Uani 1 1 d . . . . .
O3 O 0.13364(11) 0.33099(12) 0.29547(13) 0.0201(5) Uani 1 1 d D . . . .
H3 H 0.0973(9) 0.3085(12) 0.293(2) 0.030 Uiso 1 1 d DR . . . .
O1 O 0.20014(13) 0.33815(13) 0.43855(13) 0.0240(5) Uani 1 1 d . . . . .
O4 O 0.24894(13) 0.19132(17) 0.43581(18) 0.0407(8) Uani 1 1 d . . . . .
H4A H 0.231353 0.201833 0.484848 0.061 Uiso 1 1 d GR . . . .
H4B H 0.297654 0.179434 0.445589 0.061 Uiso 1 1 d GR . . . .
N3 N 0.37077(13) 0.29467(14) 0.13396(15) 0.0148(5) Uani 1 1 d . . . . .
N4 N 0.34745(14) 0.25754(14) 0.36296(16) 0.0183(6) Uani 1 1 d . . . . .
N5 N 0.500000 0.250000 0.5365(2) 0.0259(9) Uani 1 2 d S T P . .
N2 N 0.33300(13) 0.40014(14) 0.28066(15) 0.0159(5) Uani 1 1 d . . . . .
N1 N 0.28202(14) 0.39346(14) 0.33250(15) 0.0157(5) Uani 1 1 d . . . . .
C14 C 0.40430(16) 0.25384(15) 0.36996(17) 0.0137(6) Uani 1 1 d . . . . .
C15 C 0.500000 0.250000 0.4757(2) 0.0151(9) Uani 1 2 d S T P . .
C9 C 0.37777(16) 0.34854(16) 0.17567(17) 0.0147(6) Uani 1 1 d . . . . .
C13 C 0.41276(17) 0.28773(18) 0.07895(18) 0.0197(7) Uani 1 1 d . . . . .
H13 H 0.407751 0.250585 0.049750 0.024 Uiso 1 1 calc R . . . .
C7 C 0.26945(17) 0.44847(17) 0.36495(19) 0.0187(7) Uani 1 1 d . . . . .
H7 H 0.294482 0.486139 0.352677 0.022 Uiso 1 1 calc R . . . .
C8 C 0.32813(15) 0.35247(15) 0.23470(17) 0.0131(6) Uani 1 1 d . . . . .
C6 C 0.21889(18) 0.45627(18) 0.41958(19) 0.0213(7) Uani 1 1 d . . . . .
C16 C 0.1249(2) 0.39070(19) 0.2550(2) 0.0324(9) Uani 1 1 d D . . . .
H16A H 0.133895 0.381282 0.206425 0.049 Uiso 1 1 calc GR . . . .
H16B H 0.155311 0.424638 0.271509 0.049 Uiso 1 1 calc GR . . . .
H16C H 0.079498 0.406369 0.259958 0.049 Uiso 1 1 calc GR . . . .
C10 C 0.42754(18) 0.39644(18) 0.1644(2) 0.0221(7) Uani 1 1 d . . . . .
H10 H 0.431804 0.433281 0.194132 0.027 Uiso 1 1 calc R . . . .
C12 C 0.46302(17) 0.33347(19) 0.06402(19) 0.0225(7) Uani 1 1 d . . . . .
H12 H 0.490974 0.327481 0.025332 0.027 Uiso 1 1 calc R . . . .
C1 C 0.18554(18) 0.40209(18) 0.45228(19) 0.0218(7) Uani 1 1 d . . . . .
C2 C 0.1362(2) 0.4172(2) 0.5032(2) 0.0316(9) Uani 1 1 d . . . . .
H2 H 0.113568 0.382378 0.525606 0.038 Uiso 1 1 calc R . . . .
C11 C 0.47078(18) 0.38798(19) 0.1076(2) 0.0246(8) Uani 1 1 d . . . . .
H11 H 0.504748 0.419035 0.099163 0.030 Uiso 1 1 calc R . . . .
C3 C 0.1210(2) 0.4831(2) 0.5201(2) 0.0363(10) Uani 1 1 d . . . . .
H3A H 0.087728 0.491825 0.553218 0.044 Uiso 1 1 calc R . . . .
C5 C 0.2032(2) 0.5228(2) 0.4391(2) 0.0289(8) Uani 1 1 d . . . . .
H5 H 0.226222 0.558217 0.418147 0.035 Uiso 1 1 calc R . . . .
C4 C 0.1546(2) 0.5364(2) 0.4886(2) 0.0369(10) Uani 1 1 d . . . . .
H4 H 0.144446 0.580464 0.500732 0.044 Uiso 1 1 calc R . . . .
Br1 Br 0.04137(10) 0.27252(9) 0.62116(10) 0.0376(4) Uani 0.25 1 d . . . . .
O5 O 0.1950(3) 0.2305(5) 0.5578(3) 0.145(4) Uani 1 1 d D U . . .
H5A H 0.170268 0.197882 0.553104 0.218 Uiso 1 1 calc GR . . . .
C17 C 0.1740(10) 0.2662(7) 0.6067(4) 0.238(12) Uani 1 1 d D . . . .
H17A H 0.172100 0.312164 0.591547 0.357 Uiso 1 1 calc GR . . . .
H17B H 0.203858 0.262473 0.646199 0.357 Uiso 1 1 calc GR . . . .
H1 H 0.129919 0.251545 0.620200 0.357 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Dy1 3.9442(4) 13 ?
Dy1 O2 2.404(2) . ?
Dy1 O2 2.320(2) 13 ?
Dy1 O3 2.397(2) . ?
Dy1 O1 2.184(2) . ?
Dy1 O4 2.460(3) . ?
Dy1 N3 2.525(3) 13 ?
Dy1 N4 2.384(3) . ?
Dy1 N1 2.507(3) . ?
Fe1 C14 1.909(3) 16_656 ?
Fe1 C14 1.909(3) 11_666 ?
Fe1 C14 1.909(3) . ?
Fe1 C14 1.909(3) 6_554 ?
Fe1 C15 1.914(5) . ?
Fe1 C15 1.914(5) 11_666 ?
O2 C8 1.315(4) . ?
O3 H3 0.853(9) . ?
O3 C16 1.426(4) . ?
O1 C1 1.331(4) . ?
O4 H4A 1.0177 . ?
O4 H4B 1.0152 . ?
N3 C9 1.341(4) . ?
N3 C13 1.346(4) . ?
N4 C14 1.142(4) . ?
N5 C15 1.157(7) . ?
N2 N1 1.421(4) . ?
N2 C8 1.294(4) . ?
N1 C7 1.281(4) . ?
C9 C8 1.497(4) . ?
C9 C10 1.392(5) . ?
C13 H13 0.9300 . ?
C13 C12 1.382(5) . ?
C7 H7 0.9300 . ?
C7 C6 1.455(5) . ?
C6 C1 1.411(6) . ?
C6 C5 1.410(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C10 H10 0.9300 . ?
C10 C11 1.391(5) . ?
C12 H12 0.9300 . ?
C12 C11 1.374(6) . ?
C1 C2 1.411(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.384(6) . ?
C11 H11 0.9300 . ?
C3 H3A 0.9300 . ?
C3 C4 1.391(7) . ?
C5 H5 0.9300 . ?
C5 C4 1.376(6) . ?
C4 H4 0.9300 . ?
Br1 Br1 1.334(3) 12_667 ?
Br1 Br1 1.334(3) 15_556 ?
Br1 Br1 1.875(4) 6_454 ?
O5 H5A 0.8200 . ?
O5 C17 1.242(8) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H1 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 Dy1 32.73(5) . 13 ?
O2 Dy1 Dy1 34.06(5) 13 13 ?
O2 Dy1 O2 66.79(9) 13 . ?
O2 Dy1 O3 87.12(8) 13 . ?
O2 Dy1 O4 87.91(11) 13 . ?
O2 Dy1 O4 134.09(9) . . ?
O2 Dy1 N3 126.22(8) . 13 ?
O2 Dy1 N3 65.70(8) 13 13 ?
O2 Dy1 N4 93.30(9) 13 . ?
O2 Dy1 N1 62.24(8) . . ?
O2 Dy1 N1 128.89(8) 13 . ?
O3 Dy1 Dy1 84.39(6) . 13 ?
O3 Dy1 O2 83.57(8) . . ?
O3 Dy1 O4 134.86(9) . . ?
O3 Dy1 N3 70.42(8) . 13 ?
O3 Dy1 N1 83.95(8) . . ?
O1 Dy1 Dy1 163.35(7) . 13 ?
O1 Dy1 O2 154.30(9) . 13 ?
O1 Dy1 O2 134.62(9) . . ?
O1 Dy1 O3 82.62(10) . . ?
O1 Dy1 O4 82.87(12) . . ?
O1 Dy1 N3 88.64(9) . 13 ?
O1 Dy1 N4 105.48(10) . . ?
O1 Dy1 N1 73.43(9) . . ?
O4 Dy1 Dy1 113.74(9) . 13 ?
O4 Dy1 N3 66.72(9) . 13 ?
O4 Dy1 N1 131.32(10) . . ?
N3 Dy1 Dy1 96.78(6) 13 13 ?
N4 Dy1 Dy1 82.81(7) . 13 ?
N4 Dy1 O2 74.87(9) . . ?
N4 Dy1 O3 156.26(9) . . ?
N4 Dy1 O4 68.83(9) . . ?
N4 Dy1 N3 130.96(9) . 13 ?
N4 Dy1 N1 77.34(9) . . ?
N1 Dy1 Dy1 94.90(6) . 13 ?
N1 Dy1 N3 150.51(9) . 13 ?
C14 Fe1 C14 90.146(10) . 16_656 ?
C14 Fe1 C14 174.24(19) . 6_554 ?
C14 Fe1 C14 90.145(10) 11_666 6_554 ?
C14 Fe1 C14 90.143(10) . 11_666 ?
C14 Fe1 C14 90.145(10) 16_656 6_554 ?
C14 Fe1 C14 174.24(19) 11_666 16_656 ?
C14 Fe1 C15 92.88(10) 11_666 11_666 ?
C14 Fe1 C15 87.12(10) 6_554 11_666 ?
C14 Fe1 C15 92.88(10) 16_656 11_666 ?
C14 Fe1 C15 87.12(10) 11_666 . ?
C14 Fe1 C15 92.88(10) . . ?
C14 Fe1 C15 87.12(10) . 11_666 ?
C14 Fe1 C15 92.88(10) 6_554 . ?
C14 Fe1 C15 87.12(10) 16_656 . ?
C15 Fe1 C15 180.0 11_666 . ?
Dy1 O2 Dy1 113.21(9) 13 . ?
C8 O2 Dy1 117.71(19) . . ?
C8 O2 Dy1 125.54(19) . 13 ?
Dy1 O3 H3 118.9(13) . . ?
C16 O3 Dy1 132.6(2) . . ?
C16 O3 H3 107.6(13) . . ?
C1 O1 Dy1 136.9(2) . . ?
Dy1 O4 H4A 115.6 . . ?
Dy1 O4 H4B 115.7 . . ?
H4A O4 H4B 102.0 . . ?
C9 N3 Dy1 117.7(2) . 13 ?
C9 N3 C13 118.5(3) . . ?
C13 N3 Dy1 123.2(2) . 13 ?
C14 N4 Dy1 173.2(3) . . ?
C8 N2 N1 110.3(3) . . ?
N2 N1 Dy1 116.89(19) . . ?
C7 N1 Dy1 129.9(2) . . ?
C7 N1 N2 113.2(3) . . ?
N4 C14 Fe1 175.9(3) . . ?
N5 C15 Fe1 180.0 . . ?
N3 C9 C8 114.6(3) . . ?
N3 C9 C10 122.0(3) . . ?
C10 C9 C8 123.3(3) . . ?
N3 C13 H13 118.6 . . ?
N3 C13 C12 122.8(3) . . ?
C12 C13 H13 118.6 . . ?
N1 C7 H7 117.6 . . ?
N1 C7 C6 124.8(3) . . ?
C6 C7 H7 117.6 . . ?
O2 C8 C9 116.0(3) . . ?
N2 C8 O2 124.3(3) . . ?
N2 C8 C9 119.7(3) . . ?
C1 C6 C7 124.0(3) . . ?
C5 C6 C7 116.2(3) . . ?
C5 C6 C1 119.9(3) . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C9 C10 H10 120.7 . . ?
C11 C10 C9 118.5(3) . . ?
C11 C10 H10 120.7 . . ?
C13 C12 H12 120.7 . . ?
C11 C12 C13 118.5(3) . . ?
C11 C12 H12 120.7 . . ?
O1 C1 C6 122.8(3) . . ?
O1 C1 C2 119.3(4) . . ?
C6 C1 C2 117.8(3) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 C1 120.9(4) . . ?
C3 C2 H2 119.5 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.6(3) . . ?
C12 C11 H11 120.2 . . ?
C2 C3 H3A 119.4 . . ?
C2 C3 C4 121.2(4) . . ?
C4 C3 H3A 119.4 . . ?
C6 C5 H5 119.4 . . ?
C4 C5 C6 121.3(4) . . ?
C4 C5 H5 119.4 . . ?
C3 C4 H4 120.5 . . ?
C5 C4 C3 118.9(4) . . ?
C5 C4 H4 120.5 . . ?
Br1 Br1 Br1 89.31(3) 15_556 12_667 ?
Br1 Br1 Br1 45.341(17) 15_556 6_454 ?
Br1 Br1 Br1 45.341(17) 12_667 6_454 ?
C17 O5 H5A 109.5 . . ?
O5 C17 H17A 109.5 . . ?
O5 C17 H17B 109.5 . . ?
O5 C17 H1 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H1 109.5 . . ?
H17B C17 H1 109.5 . . ?

_olex2_date_sample_data_collection 2018-10-20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.972
_oxdiff_exptl_absorpt_empirical_full_min 0.428
####################################################################### 
# 
# 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_20181012b
_database_code_depnum_ccdc_archive 'CCDC 2109923'
loop_
_audit_author_name
_audit_author_address
'Hao-Ling Sun'
;Beijing Normal University
China
;
_audit_update_record             
;
2021-09-15 deposited with the CCDC.	2021-11-08 downloaded from the CCDC.
;
_audit_creation_date             2021-09-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.25(C248 H240 Co4 Dy16 N72 O64), Cl, 8(H2 O1)'
_chemical_formula_sum            'C62 H76 Cl Co Dy4 N18 O24'
_chemical_formula_weight         2201.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Dy1  Cl1 Co1 C1 H1 N1 O1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -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'

_cell_length_a                   19.5160(2)
_cell_length_b                   19.5160(2)
_cell_length_c                   20.1999(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7693.6(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11717
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.5540
_cell_measurement_theta_min      4.5190
_shelx_estimated_absorpt_T_max   0.655
_shelx_estimated_absorpt_T_min   0.091
_exptl_absorpt_coefficient_mu    23.109
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4296
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26268
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.903
_diffrn_reflns_theta_min         5.522
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  24.00   1.00    2.00    --  -39.74  77.00-180.00   94
  2  ω   -108.00 -15.00   1.00    2.00    --  -39.74 -37.00 -90.00   93
  3  ω    -62.00  34.00   1.00    2.00    --  -39.74  37.00  90.00   96
  4  ω     99.00 126.00   1.00    2.00    --   39.74 178.00 120.00   27
  5  ω     63.00 113.00   1.00    2.00    --   39.74 178.00   0.00   50
  6  ω     40.00 130.00   1.00   18.00    --  104.69 -30.00-180.00   90
  7  ω     32.00 113.00   1.00   18.00    --  104.69 -45.00   0.00   81
  8  ω     58.00 110.00   1.00   18.00    --  104.69 -77.00-150.00   52
  9  ω     23.00 143.00   1.00   18.00    --  104.69 -15.00   0.00  120
 10  ω     44.00 115.00   1.00   18.00    --  104.69-125.00-180.00   71
 11  ω     66.00 100.00   1.00   18.00    --  104.69 -94.00  30.00   34
 12  ω    103.00 161.00   1.00   18.00    --  104.69 125.00 -60.00   58
 13  ω     46.00 134.00   1.00   18.00    --  104.69 -61.00 -90.00   88
 14  ω     93.00 118.00   1.00   18.00    --  104.69-125.00 -30.00   25
 15  ω    143.00 168.00   1.00   18.00    --  104.69 125.00-150.00   25
 16  ω    125.00 176.00   1.00   18.00    --  104.69 125.00 -30.00   51
 17  ω     79.00 178.00   1.00   18.00    --  104.69  45.00   0.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0246913000
_diffrn_orient_matrix_UB_12      -0.0520891000
_diffrn_orient_matrix_UB_13      0.0521688000
_diffrn_orient_matrix_UB_21      -0.0477532000
_diffrn_orient_matrix_UB_22      -0.0546436000
_diffrn_orient_matrix_UB_23      -0.0299188000
_diffrn_orient_matrix_UB_31      0.0577552000
_diffrn_orient_matrix_UB_32      -0.0230789000
_diffrn_orient_matrix_UB_33      -0.0469511000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3535
_reflns_number_total             3750
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3750
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0272
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0284P)²+31.5063P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0665
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O4-H4
 0.85 with sigma of 0.01
 Dy1-H4
 2.910048 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O7 \\sim O5 \\sim O6: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(O7)=Sof(H7A)=Sof(H7B)=Sof(O8)=Sof(H8A)=Sof(H8B)=1-FVAR(1)
 Sof(O5)=Sof(H5A)=Sof(H5B)=Sof(O6)=Sof(H6A)=Sof(H6B)=FVAR(1)
 Fixed Sof: Cl1(0.25)
5.a Riding coordinates:
 O5(H5A,H5B), O6(H6A,H6B), O8(H8A,H8B)
5.b Free rotating group:
 O7(H7A,H7B)
5.c Rotating group:
 O3(H3A,H3B)
5.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C11(H11), C13(H13), C10(H10), C12(H12), C3(H3), C4(H4A), C2(H2), C1(H1)
5.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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
Dy1 Dy 0.98061(2) 0.52421(2) 0.59329(2) 0.01802(7) Uani 1 1 d D . . . .
Co1 Co 1.000000 0.250000 0.625000 0.01644(19) Uani 1 4 d S T P . .
O2 O 0.94294(11) 0.46940(11) 0.49428(10) 0.0192(4) Uani 1 1 d . . . . .
O1 O 0.93431(12) 0.55975(12) 0.68656(11) 0.0249(5) Uani 1 1 d . . . . .
O4 O 0.92227(12) 0.61985(11) 0.54531(12) 0.0243(5) Uani 1 1 d D . . . .
H4 H 0.9422(14) 0.6578(9) 0.540(2) 0.036 Uiso 1 1 d DR . . . .
O3 O 1.08328(13) 0.50726(12) 0.65952(12) 0.0276(5) Uani 1 1 d . . . . .
H3A H 1.091555 0.463379 0.665339 0.041 Uiso 1 1 d GR . . . .
H3B H 1.077048 0.522393 0.700045 0.041 Uiso 1 1 d GR . . . .
N3 N 0.94109(14) 0.37206(13) 0.40323(13) 0.0204(5) Uani 1 1 d . . . . .
N4 N 0.99478(15) 0.40453(14) 0.61638(14) 0.0235(6) Uani 1 1 d . . . . .
N1 N 0.86237(14) 0.47754(13) 0.59353(13) 0.0201(5) Uani 1 1 d . . . . .
N5 N 1.000000 0.250000 0.7742(2) 0.0290(9) Uani 1 2 d S T P . .
N2 N 0.84711(14) 0.42562(13) 0.54625(13) 0.0214(5) Uani 1 1 d . . . . .
C15 C 0.99727(16) 0.34618(17) 0.62187(15) 0.0208(6) Uani 1 1 d . . . . .
C16 C 1.000000 0.250000 0.7180(3) 0.0239(10) Uani 1 2 d S T P . .
C9 C 0.88812(17) 0.37196(16) 0.44600(16) 0.0209(6) Uani 1 1 d . . . . .
C7 C 0.81155(18) 0.49104(18) 0.63191(17) 0.0258(7) Uani 1 1 d . . . . .
H7 H 0.770538 0.468390 0.623498 0.031 Uiso 1 1 calc R . . . .
C6 C 0.87276(18) 0.57023(18) 0.71197(17) 0.0267(7) Uani 1 1 d . . . . .
C11 C 0.83620(19) 0.27663(18) 0.39135(18) 0.0286(7) Uani 1 1 d . . . . .
H11 H 0.800808 0.245012 0.387194 0.034 Uiso 1 1 calc R . . . .
C13 C 0.94207(18) 0.32413(17) 0.35555(16) 0.0250(7) Uani 1 1 d . . . . .
H13 H 0.978859 0.323508 0.326287 0.030 Uiso 1 1 calc R . . . .
C8 C 0.89185(16) 0.42542(15) 0.49884(15) 0.0189(6) Uani 1 1 d . . . . .
C10 C 0.83485(18) 0.32539(18) 0.44115(17) 0.0266(7) Uani 1 1 d . . . . .
H10 H 0.798583 0.326829 0.470981 0.032 Uiso 1 1 calc R . . . .
C5 C 0.8126(2) 0.53852(19) 0.68717(18) 0.0299(8) Uani 1 1 d . . . . .
C12 C 0.8910(2) 0.27562(17) 0.34785(16) 0.0268(7) Uani 1 1 d . . . . .
H12 H 0.893393 0.243127 0.314257 0.032 Uiso 1 1 calc R . . . .
C14 C 0.86270(19) 0.62248(19) 0.50469(19) 0.0314(8) Uani 1 1 d . . . . .
H14A H 0.873287 0.604542 0.461632 0.047 Uiso 1 1 calc GR . . . .
H14B H 0.847672 0.669120 0.500591 0.047 Uiso 1 1 calc GR . . . .
H14C H 0.826992 0.595535 0.524455 0.047 Uiso 1 1 calc GR . . . .
C3 C 0.8659(2) 0.6133(2) 0.7675(2) 0.0393(9) Uani 1 1 d . . . . .
H3 H 0.904414 0.635452 0.784106 0.047 Uiso 1 1 calc R . . . .
C4 C 0.7498(2) 0.5501(2) 0.7190(2) 0.0422(10) Uani 1 1 d . . . . .
H4A H 0.710541 0.528955 0.702743 0.051 Uiso 1 1 calc R . . . .
C2 C 0.8035(2) 0.6236(3) 0.7980(2) 0.0545(13) Uani 1 1 d . . . . .
H2 H 0.800636 0.651862 0.834965 0.065 Uiso 1 1 calc R . . . .
C1 C 0.7446(2) 0.5917(3) 0.7737(3) 0.0571(14) Uani 1 1 d . . . . .
H1 H 0.702478 0.598627 0.794138 0.069 Uiso 1 1 calc R . . . .
Cl1 Cl 1.0491(3) 0.5717(4) 0.7721(3) 0.0404(14) Uani 0.25 1 d . . . A 1
O5 O 0.8443(6) 0.7969(5) 0.8274(5) 0.085(3) Uani 0.475(6) 1 d . U . B 1
H5A H 0.838915 0.768975 0.859254 0.128 Uiso 0.475(6) 1 d R . . B 1
H5B H 0.822035 0.782835 0.793854 0.128 Uiso 0.475(6) 1 d R . . B 1
O6 O 0.9154(5) 0.8025(5) 0.8139(4) 0.066(2) Uani 0.475(6) 1 d . U . B 2
H6A H 0.909081 0.842388 0.829686 0.099 Uiso 0.475(6) 1 d R . . B 2
H6B H 0.935481 0.780718 0.844786 0.099 Uiso 0.475(6) 1 d R . . B 2
O7 O 0.9804(3) 0.7687(3) 0.8136(3) 0.0380(13) Uani 0.525(6) 1 d . U . B -1
H7A H 0.947849 0.787671 0.834620 0.057 Uiso 0.525(6) 1 d G . . B -1
H7B H 0.977584 0.784917 0.774622 0.057 Uiso 0.525(6) 1 d G . . B -1
O8 O 0.9526(10) 0.9196(10) 0.7724(8) 0.124(8) Uani 0.525(6) 1 d . . . B 2
H8A H 0.987879 0.940553 0.786608 0.186 Uiso 0.525(6) 1 d R . . B 2
H8B H 0.962479 0.877373 0.776488 0.186 Uiso 0.525(6) 1 d R . . B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Dy1 3.9588(3) 9_766 ?
Dy1 O2 2.384(2) . ?
Dy1 O2 2.318(2) 9_766 ?
Dy1 O1 2.201(2) . ?
Dy1 O4 2.392(2) . ?
Dy1 O3 2.432(2) . ?
Dy1 N3 2.537(3) 9_766 ?
Dy1 N4 2.398(3) . ?
Dy1 N1 2.481(3) . ?
Co1 C15 1.879(3) 6_654 ?
Co1 C15 1.879(3) 15_666 ?
Co1 C15 1.879(3) 12_757 ?
Co1 C15 1.879(3) . ?
Co1 C16 1.880(5) . ?
Co1 C16 1.879(5) 15_666 ?
O2 C8 1.319(4) . ?
O1 C6 1.322(4) . ?
O4 H4 0.843(10) . ?
O4 C14 1.424(4) . ?
O3 H3A 0.8794 . ?
O3 H3B 0.8788 . ?
N3 C9 1.347(4) . ?
N3 C13 1.343(4) . ?
N4 C15 1.145(4) . ?
N1 N2 1.424(4) . ?
N1 C7 1.286(4) . ?
N5 C16 1.135(7) . ?
N2 C8 1.296(4) . ?
C9 C8 1.494(4) . ?
C9 C10 1.384(5) . ?
C7 H7 0.9300 . ?
C7 C5 1.451(5) . ?
C6 C5 1.419(5) . ?
C6 C3 1.409(5) . ?
C11 H11 0.9300 . ?
C11 C10 1.385(5) . ?
C11 C12 1.384(5) . ?
C13 H13 0.9300 . ?
C13 C12 1.384(5) . ?
C10 H10 0.9300 . ?
C5 C4 1.402(5) . ?
C12 H12 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C3 H3 0.9300 . ?
C3 C2 1.378(6) . ?
C4 H4A 0.9300 . ?
C4 C1 1.375(6) . ?
C2 H2 0.9300 . ?
C2 C1 1.396(7) . ?
C1 H1 0.9300 . ?
O5 H5A 0.8497 . ?
O5 H5B 0.8497 . ?
O6 H6A 0.8496 . ?
O6 H6B 0.8504 . ?
O7 H7A 0.8494 . ?
O7 H7B 0.8493 . ?
O8 H8A 0.8504 . ?
O8 H8B 0.8504 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 Dy1 32.14(5) . 9_766 ?
O2 Dy1 Dy1 33.18(5) 9_766 9_766 ?
O2 Dy1 O2 65.32(9) 9_766 . ?
O2 Dy1 O4 87.43(8) 9_766 . ?
O2 Dy1 O4 82.15(8) . . ?
O2 Dy1 O3 84.07(8) 9_766 . ?
O2 Dy1 O3 130.88(8) . . ?
O2 Dy1 N3 124.53(8) . 9_766 ?
O2 Dy1 N3 65.82(8) 9_766 9_766 ?
O2 Dy1 N4 97.28(9) 9_766 . ?
O2 Dy1 N4 76.21(8) . . ?
O2 Dy1 N1 63.26(8) . . ?
O2 Dy1 N1 128.33(8) 9_766 . ?
O1 Dy1 Dy1 165.56(6) . 9_766 ?
O1 Dy1 O2 154.22(8) . 9_766 ?
O1 Dy1 O2 137.11(8) . . ?
O1 Dy1 O4 84.58(9) . . ?
O1 Dy1 O3 84.86(9) . . ?
O1 Dy1 N3 88.40(9) . 9_766 ?
O1 Dy1 N4 100.83(9) . . ?
O1 Dy1 N1 74.47(9) . . ?
O4 Dy1 Dy1 83.77(6) . 9_766 ?
O4 Dy1 O3 136.16(8) . . ?
O4 Dy1 N3 71.05(8) . 9_766 ?
O4 Dy1 N4 153.38(9) . . ?
O4 Dy1 N1 81.06(8) . . ?
O3 Dy1 Dy1 109.49(6) . 9_766 ?
O3 Dy1 N3 66.24(8) . 9_766 ?
O3 Dy1 N1 135.68(8) . . ?
N3 Dy1 Dy1 95.83(6) 9_766 9_766 ?
N4 Dy1 Dy1 86.02(7) . 9_766 ?
N4 Dy1 O3 70.46(9) . . ?
N4 Dy1 N3 134.61(9) . 9_766 ?
N4 Dy1 N1 75.48(9) . . ?
N1 Dy1 Dy1 95.28(6) . 9_766 ?
N1 Dy1 N3 148.54(9) . 9_766 ?
C15 Co1 C15 176.14(19) 6_654 . ?
C15 Co1 C15 90.065(7) 12_757 6_654 ?
C15 Co1 C15 176.14(19) 12_757 15_666 ?
C15 Co1 C15 90.064(7) 15_666 . ?
C15 Co1 C15 90.066(7) 12_757 . ?
C15 Co1 C15 90.065(7) 15_666 6_654 ?
C15 Co1 C16 91.93(9) 12_757 15_666 ?
C15 Co1 C16 88.07(9) 6_654 15_666 ?
C15 Co1 C16 88.07(9) . 15_666 ?
C15 Co1 C16 88.07(9) 12_757 . ?
C15 Co1 C16 91.93(9) . . ?
C15 Co1 C16 91.93(9) 15_666 15_666 ?
C15 Co1 C16 88.07(9) 15_666 . ?
C15 Co1 C16 91.93(9) 6_654 . ?
C16 Co1 C16 180.0 15_666 . ?
Dy1 O2 Dy1 114.68(9) 9_766 . ?
C8 O2 Dy1 125.11(18) . 9_766 ?
C8 O2 Dy1 117.81(18) . . ?
C6 O1 Dy1 138.9(2) . . ?
Dy1 O4 H4 121.1(18) . . ?
C14 O4 Dy1 130.6(2) . . ?
C14 O4 H4 105.9(19) . . ?
Dy1 O3 H3A 110.9 . . ?
Dy1 O3 H3B 110.7 . . ?
H3A O3 H3B 103.2 . . ?
C9 N3 Dy1 116.5(2) . 9_766 ?
C13 N3 Dy1 124.5(2) . 9_766 ?
C13 N3 C9 118.0(3) . . ?
C15 N4 Dy1 172.9(3) . . ?
N2 N1 Dy1 117.03(19) . . ?
C7 N1 Dy1 130.0(2) . . ?
C7 N1 N2 112.9(3) . . ?
C8 N2 N1 110.9(3) . . ?
N4 C15 Co1 176.3(3) . . ?
N5 C16 Co1 180.0 . . ?
N3 C9 C8 114.8(3) . . ?
N3 C9 C10 122.1(3) . . ?
C10 C9 C8 123.1(3) . . ?
N1 C7 H7 117.1 . . ?
N1 C7 C5 125.7(3) . . ?
C5 C7 H7 117.1 . . ?
O1 C6 C5 123.2(3) . . ?
O1 C6 C3 119.2(3) . . ?
C3 C6 C5 117.5(3) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
C12 C11 C10 119.1(3) . . ?
N3 C13 H13 118.4 . . ?
N3 C13 C12 123.2(3) . . ?
C12 C13 H13 118.4 . . ?
O2 C8 C9 116.2(3) . . ?
N2 C8 O2 124.0(3) . . ?
N2 C8 C9 119.8(3) . . ?
C9 C10 C11 119.2(3) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C6 C5 C7 124.2(3) . . ?
C4 C5 C7 116.3(4) . . ?
C4 C5 C6 119.4(3) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 C11 118.4(3) . . ?
C13 C12 H12 120.8 . . ?
O4 C14 H14A 109.5 . . ?
O4 C14 H14B 109.5 . . ?
O4 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C3 H3 119.1 . . ?
C2 C3 C6 121.8(4) . . ?
C2 C3 H3 119.1 . . ?
C5 C4 H4A 119.1 . . ?
C1 C4 C5 121.9(4) . . ?
C1 C4 H4A 119.1 . . ?
C3 C2 H2 119.8 . . ?
C3 C2 C1 120.3(4) . . ?
C1 C2 H2 119.8 . . ?
C4 C1 C2 119.1(4) . . ?
C4 C1 H1 120.5 . . ?
C2 C1 H1 120.5 . . ?
H5A O5 H5B 109.5 . . ?
H6A O6 H6B 104.5 . . ?
H7A O7 H7B 104.7 . . ?
H8A O8 H8B 104.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.576
_oxdiff_exptl_absorpt_empirical_full_min 0.528
