# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_at_cu6gd4
_audit_block_doi                 10.5517/ccdc.csd.cc2kky69
_database_code_depnum_ccdc_archive 'CCDC 2370731'
loop_
_audit_author_name
_audit_author_address
'Antonis Anastassiades'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-07-15 deposited with the CCDC.	2024-09-09 downloaded from the CCDC.
;
_audit_creation_date             2024-07-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H80 Cu6 Gd4 N16 O44, 3(C2 H3 N)'
_chemical_formula_sum            'C74 H89 Cu6 Gd4 N19 O44'
_chemical_formula_weight         2958.88
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cu6 Gd4 N8 O40 C100 H100'
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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -8.8380 11.9157 '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           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   17.70470(10)
_cell_length_b                   17.70470(10)
_cell_length_c                   16.4257(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5148.74(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    21399
_cell_measurement_temperature    180
_cell_measurement_theta_max      76.0720
_cell_measurement_theta_min      3.5130
_shelx_estimated_absorpt_T_max   0.458
_shelx_estimated_absorpt_T_min   0.088
_exptl_absorpt_coefficient_mu    18.497
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2896
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -7 8 0.0536
4 10 -3 0.0785
-1 -3 -10 0.0785
2 5 9 0.0991
4 -9 6 0.0134
-3 9 -6 0.0335
-9 6 2 0.0808
-10 -6 -2 0.1345
-9 7 -2 0.0733
-9 -4 -5 0.1287
0 11 2 0.0852
9 5 5 0.1065
-6 2 -9 0.0816
8 0 -8 0.1405
8 8 -1 0.0909
10 -5 2 0.0914
-2 -9 6 0.0596
-8 -2 8 0.0746

_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.05
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-2.6134 -7.3639 7.8192 0.2146 0.9102 0.3542
3.9534 10.3434 -2.8692 -0.1377 -0.5954 -0.7915
-1.4403 -2.7631 -10.2623 -0.1858 -0.7694 0.6111
2.2974 5.0318 9.3469 0.1499 0.6148 -0.7744
3.7119 -8.6812 6.0809 0.7192 0.6144 0.3245
-3.4932 8.9736 -5.8220 -0.7089 -0.6053 -0.3620
-9.1447 6.4430 2.4296 -0.9023 0.3154 -0.2938
-9.6526 -5.7029 -2.3496 -0.5662 0.2040 0.7986
-8.5964 7.3810 -1.7738 -0.9693 -0.0798 -0.2325
-9.2163 -4.4993 -4.8136 -0.6213 -0.0460 0.7822
-0.4558 11.1836 2.4377 -0.4147 -0.0386 -0.9091
9.1930 4.5453 4.8149 0.6178 0.0457 -0.7850
-6.3138 2.0585 -8.7008 -0.7145 -0.6108 0.3413
7.9257 -0.1473 -7.7138 0.4785 -0.8769 0.0451
8.0310 8.1166 -1.2323 0.2879 -0.5193 -0.8046
10.2489 -4.8155 1.8015 0.9997 -0.0239 -0.0100
-2.3596 -9.4232 5.7022 0.2748 0.7705 0.5752
-7.5707 -1.5662 7.8841 -0.3835 0.9211 0.0665

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0487
_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       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35749
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.761
_diffrn_reflns_theta_min         3.530
_diffrn_ambient_temperature      180
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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    -78.00  10.00   0.40    0.50    --  -47.19  97.00  33.00  220
  2  ω    -18.00  64.00   0.40    0.50    --   47.19 -97.00 -73.00  205
  3  ω   -145.00-117.00   0.40    2.50    -- -106.00 -97.00 -73.00   70
  4  ω   -105.00 -37.00   0.40    2.50    -- -106.00  97.00  33.00  170
  5  ω     87.00 162.20   0.40    2.50    --  106.24  97.00  33.00  188
  6  ω     57.00  98.20   0.40    2.50    --  106.24 -97.00 -73.00  103
  7  ω    -28.00   3.20   0.40    0.50    --  -47.19  19.00 150.00   78
  8  ω     73.00 100.20   0.40    0.50    --   47.19 126.00-120.00   68
  9  ω    -26.00  29.20   0.40    0.50    --   47.19 -19.00-150.00  138
 10  ω     73.00 101.00   0.40    0.50    --   47.19 126.00 -90.00   70
 11  ω    -12.00  29.20   0.40    0.50    --   47.19 -19.00  90.00  103
 12  ω    -92.00 -38.00   0.40    2.50    -- -106.00 126.00 -60.00  135
 13  ω    -67.00 -35.00   0.40    2.50    -- -106.00  61.00-120.00   80
 14  ω   -100.00 -34.00   0.40    2.50    -- -106.00  77.00-120.00  165
 15  ω    -66.00 -36.00   0.40    2.50    -- -106.00  61.00  30.00   75
 16  ω    -68.00 -38.00   0.40    2.50    -- -106.00  61.00-150.00   75
 17  ω     39.00  68.20   0.40    2.50    --  106.24 -61.00   0.00   73
 18  ω     38.00  69.20   0.40    2.50    --  106.24 -61.00 -30.00   78
 19  ω     94.00 170.00   0.40    2.50    --  106.24  15.00-150.00  190
 20  ω     35.00  67.00   0.40    2.50    --  106.24 -61.00 -60.00   80
 21  ω     39.00  67.00   0.40    2.50    --  106.24 -61.00 -90.00   70
 22  ω     42.00  68.00   0.40    2.50    --  106.24 -61.00 120.00   65
 23  ω     41.00  68.20   0.40    2.50    --  106.24 -61.00  60.00   68
 24  ω     38.00  70.00   0.40    2.50    --  106.24 -61.00  90.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0767119000
_diffrn_orient_matrix_UB_12      -0.0377746000
_diffrn_orient_matrix_UB_13      0.0175120000
_diffrn_orient_matrix_UB_21      -0.0281827000
_diffrn_orient_matrix_UB_22      -0.0231668000
_diffrn_orient_matrix_UB_23      0.0851694000
_diffrn_orient_matrix_UB_31      -0.0299526000
_diffrn_orient_matrix_UB_32      -0.0748397000
_diffrn_orient_matrix_UB_33      -0.0351947000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                5158
_reflns_number_total             5354
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 
;
 Flack x determined using 2147 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5354
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0439
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0573P)²+24.1025P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1142
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 C10-H5
 1.880761 with sigma of 0.02
 Cu2-H5
 3.067003 with sigma of 0.02
3. Rigid bond restraints
 O10, N4, O11, O9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N5, C18, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O10 \\sim N4 \\sim O11 \\sim O9: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C19 \\sim C18 \\sim N5: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
5. Others
 Fixed Sof: C18(0.75) N5(0.75) C19(0.75) H19a(0.75) H19b(0.75) H19c(0.75)
6.a Ternary CH refined with riding coordinates:
 C12(H12)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C11(H11a,H11b), C10(H10a,H10b)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C17(H17), C7(H7), C8(H8), C14(H14), C9(H9), C16(H16), C15(H15)
6.d Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Gd1 Gd 0.53900(3) 0.68117(3) 0.66074(4) 0.03008(15) Uani 1 1 d . . . . .
Cu1 Cu 0.500000 0.500000 0.65567(12) 0.0308(4) Uani 1 2 d S T P . .
Cu2 Cu 0.74284(8) 0.35556(7) 0.49269(8) 0.0328(3) Uani 1 1 d D . . . .
O1 O 0.5856(3) 0.5627(4) 0.6703(4) 0.0352(14) Uani 1 1 d . . . . .
O3 O 0.7010(4) 0.4560(4) 0.4759(4) 0.0348(13) Uani 1 1 d . . . . .
O2 O 0.5549(3) 0.4082(3) 0.6370(4) 0.0330(14) Uani 1 1 d . . . . .
O4 O 0.7082(5) 0.3394(4) 0.3830(4) 0.0422(16) Uani 1 1 d . . . . .
O8 O 0.5572(5) 0.6947(6) 0.9120(5) 0.059(2) Uani 1 1 d . . . . .
N1 N 0.7919(4) 0.3921(4) 0.5952(5) 0.0320(15) Uani 1 1 d . . . . .
N2 N 0.7586(4) 0.2447(4) 0.5150(5) 0.0353(16) Uani 1 1 d . . . . .
O6 O 0.6066(4) 0.7013(5) 0.7912(4) 0.0474(18) Uani 1 1 d . . . . .
O7 O 0.4900(4) 0.6730(7) 0.8031(5) 0.062(2) Uani 1 1 d . . . . .
O5 O 0.8614(5) 0.3383(6) 0.4248(6) 0.067(2) Uani 1 1 d D . . . .
H5 H 0.906(2) 0.355(7) 0.430(8) 0.100 Uiso 1 1 d D U . . .
N3 N 0.5517(5) 0.6886(5) 0.8377(5) 0.0417(18) Uani 1 1 d . . . . .
C6 C 0.8106(6) 0.4862(6) 0.6961(6) 0.037(2) Uani 1 1 d . . . . .
H6 H 0.791474 0.527254 0.727198 0.045 Uiso 1 1 calc R U . . .
O9 O 0.5210(5) 0.8175(5) 0.6909(7) 0.0682(15) Uani 1 1 d . U . . .
C13 C 0.7823(6) 0.1982(5) 0.4552(6) 0.040(2) Uani 1 1 d . . . . .
C5 C 0.7641(5) 0.4497(5) 0.6406(5) 0.0293(18) Uani 1 1 d . . . . .
O10 O 0.4183(5) 0.7566(5) 0.6668(7) 0.0684(15) Uani 1 1 d . U . . .
C1 C 0.6572(5) 0.5343(6) 0.6855(6) 0.0353(19) Uani 1 1 d . . . . .
H1A H 0.658733 0.514135 0.741704 0.042 Uiso 1 1 calc R U . . .
H1B H 0.694190 0.576057 0.682017 0.042 Uiso 1 1 calc R U . . .
C2 C 0.6730(5) 0.5025(5) 0.5385(5) 0.0320(17) Uani 1 1 d . . . . .
H2A H 0.618783 0.512310 0.527934 0.038 Uiso 1 1 calc R U . . .
H2B H 0.699555 0.551664 0.535900 0.038 Uiso 1 1 calc R U . . .
C17 C 0.7437(5) 0.2156(5) 0.5893(6) 0.038(2) Uani 1 1 d . . . . .
H17 H 0.726751 0.248360 0.631311 0.046 Uiso 1 1 calc R U . . .
C4 C 0.6810(5) 0.4710(5) 0.6256(5) 0.0274(16) Uani 1 1 d . . . . .
C7 C 0.8852(5) 0.4631(6) 0.7065(6) 0.043(2) Uani 1 1 d . . . . .
H7 H 0.917227 0.488403 0.744020 0.051 Uiso 1 1 calc R U . . .
C8 C 0.9115(5) 0.4036(6) 0.6622(7) 0.042(2) Uani 1 1 d . . . . .
H8 H 0.961748 0.385847 0.669215 0.051 Uiso 1 1 calc R U . . .
C3 C 0.6339(5) 0.3985(5) 0.6402(5) 0.0326(19) Uani 1 1 d . . . . .
H3A H 0.648555 0.360530 0.598875 0.039 Uiso 1 1 calc R U . . .
H3B H 0.647389 0.377823 0.694265 0.039 Uiso 1 1 calc R U . . .
C14 C 0.7926(7) 0.1219(6) 0.4697(7) 0.050(3) Uani 1 1 d . . . . .
H14 H 0.810147 0.089323 0.427832 0.060 Uiso 1 1 calc R U . . .
C12 C 0.7936(7) 0.2302(6) 0.3723(7) 0.051(3) Uani 1 1 d . . . . .
H12 H 0.802309 0.186476 0.334952 0.061 Uiso 1 1 calc R U . . .
N4 N 0.4482(6) 0.8149(6) 0.6949(8) 0.0687(14) Uani 1 1 d . U . . .
C9 C 0.8636(6) 0.3697(5) 0.6067(6) 0.040(2) Uani 1 1 d . . . . .
H9 H 0.882246 0.328712 0.575182 0.047 Uiso 1 1 calc R U . . .
C11 C 0.7225(8) 0.2711(6) 0.3413(7) 0.058(3) Uani 1 1 d . . . . .
H11A H 0.728487 0.281861 0.282565 0.069 Uiso 1 1 calc R U . . .
H11B H 0.678369 0.237227 0.347776 0.069 Uiso 1 1 calc R U . . .
C16 C 0.7521(7) 0.1407(6) 0.6059(7) 0.051(3) Uani 1 1 d . . . . .
H16 H 0.740862 0.121457 0.658501 0.061 Uiso 1 1 calc R U . . .
O11 O 0.4107(5) 0.8657(6) 0.7238(7) 0.0746(17) Uani 1 1 d . U . . .
C15 C 0.7768(8) 0.0941(7) 0.5463(8) 0.056(3) Uani 1 1 d . . . . .
H15 H 0.783291 0.041797 0.557249 0.067 Uiso 1 1 calc R U . . .
C10 C 0.8608(9) 0.2798(9) 0.3655(9) 0.072(4) Uani 1 1 d D . . . .
H10A H 0.906962 0.248830 0.371649 0.086 Uiso 1 1 calc R U . . .
H10B H 0.861781 0.302744 0.310493 0.086 Uiso 1 1 calc R U . . .
C18 C 1.0559(11) 0.4187(12) 0.4661(16) 0.081(4) Uani 0.75 1 d . U P . .
N5 N 1.0028(10) 0.4030(10) 0.4382(12) 0.082(4) Uani 0.75 1 d . U P . .
C19 C 1.1257(10) 0.4403(12) 0.4982(16) 0.082(4) Uani 0.75 1 d . U P . .
H19A H 1.164406 0.403857 0.481472 0.123 Uiso 0.75 1 calc R U P . .
H19B H 1.122672 0.441615 0.557712 0.123 Uiso 0.75 1 calc R U P . .
H19C H 1.139081 0.490558 0.477733 0.123 Uiso 0.75 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 Cu1 3.2820(5) . ?
Gd1 Cu2 3.3210(14) 4_656 ?
Gd1 O1 2.260(6) . ?
Gd1 O3 2.273(6) 4_656 ?
Gd1 O2 2.328(6) 2_665 ?
Gd1 O4 2.319(6) 4_656 ?
Gd1 O6 2.481(7) . ?
Gd1 O7 2.498(8) . ?
Gd1 N3 2.918(8) . ?
Gd1 O9 2.484(9) . ?
Gd1 O10 2.522(9) . ?
Gd1 N4 2.916(11) . ?
Cu1 O1 1.893(6) 2_665 ?
Cu1 O1 1.894(6) . ?
Cu1 O2 1.918(6) 2_665 ?
Cu1 O2 1.918(6) . ?
Cu2 O3 1.946(7) . ?
Cu2 O4 1.925(7) . ?
Cu2 N1 2.002(8) . ?
Cu2 N2 2.017(8) . ?
Cu2 O5 2.397(9) . ?
O1 C1 1.386(11) . ?
O3 C2 1.409(10) . ?
O2 C3 1.411(11) . ?
O4 C11 1.413(11) . ?
O8 N3 1.229(11) . ?
N1 C5 1.356(12) . ?
N1 C9 1.343(12) . ?
N2 C13 1.349(12) . ?
N2 C17 1.351(12) . ?
O6 N3 1.256(11) . ?
O7 N3 1.262(11) . ?
O5 H5 0.850(13) . ?
O5 C10 1.422(17) . ?
C6 H6 0.9500 . ?
C6 C5 1.389(13) . ?
C6 C7 1.393(14) . ?
O9 N4 1.292(14) . ?
C13 C14 1.385(14) . ?
C13 C12 1.487(15) . ?
C5 C4 1.539(12) . ?
O10 N4 1.248(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C4 1.550(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C4 1.542(12) . ?
C17 H17 0.9500 . ?
C17 C16 1.362(14) . ?
C4 C3 1.547(11) . ?
C7 H7 0.9500 . ?
C7 C8 1.363(16) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(14) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C14 H14 0.9500 . ?
C14 C15 1.379(17) . ?
C12 H12 1.0000 . ?
C12 C11 1.538(16) . ?
C12 C10 1.48(2) . ?
N4 O11 1.215(14) . ?
C9 H9 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C16 H16 0.9500 . ?
C16 C15 1.353(18) . ?
C15 H15 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C18 N5 1.08(3) . ?
C18 C19 1.40(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

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
Cu1 Gd1 Cu2 114.85(4) . 4_656 ?
O1 Gd1 Cu1 34.03(15) . . ?
O1 Gd1 Cu2 98.79(17) . 4_656 ?
O1 Gd1 O3 101.4(2) . 4_656 ?
O1 Gd1 O2 69.0(2) . 2_665 ?
O1 Gd1 O4 82.8(3) . 4_656 ?
O1 Gd1 O6 84.1(3) . . ?
O1 Gd1 O7 90.5(3) . . ?
O1 Gd1 N3 86.8(3) . . ?
O1 Gd1 O9 159.2(3) . . ?
O1 Gd1 O10 143.0(3) . . ?
O1 Gd1 N4 160.3(3) . . ?
O3 Gd1 Cu1 97.69(17) 4_656 . ?
O3 Gd1 Cu2 34.72(17) 4_656 4_656 ?
O3 Gd1 O2 88.1(2) 4_656 2_665 ?
O3 Gd1 O4 68.0(2) 4_656 4_656 ?
O3 Gd1 O6 144.3(2) 4_656 . ?
O3 Gd1 O7 161.2(3) 4_656 . ?
O3 Gd1 N3 166.7(2) 4_656 . ?
O3 Gd1 O9 93.0(3) 4_656 . ?
O3 Gd1 O10 89.4(3) 4_656 . ?
O3 Gd1 N4 94.9(3) 4_656 . ?
O2 Gd1 Cu1 35.04(15) 2_665 . ?
O2 Gd1 Cu2 119.86(16) 2_665 4_656 ?
O2 Gd1 O6 125.9(2) 2_665 . ?
O2 Gd1 O7 82.5(3) 2_665 . ?
O2 Gd1 N3 104.6(2) 2_665 . ?
O2 Gd1 O9 127.0(3) 2_665 . ?
O2 Gd1 O10 76.2(2) 2_665 . ?
O2 Gd1 N4 101.0(3) 2_665 . ?
O4 Gd1 Cu1 112.9(2) 4_656 . ?
O4 Gd1 Cu2 34.44(17) 4_656 4_656 ?
O4 Gd1 O2 138.7(2) 4_656 2_665 ?
O4 Gd1 O6 77.9(2) 4_656 . ?
O4 Gd1 O7 128.6(2) 4_656 . ?
O4 Gd1 N3 103.2(2) 4_656 . ?
O4 Gd1 O9 88.8(3) 4_656 . ?
O4 Gd1 O10 133.5(3) 4_656 . ?
O4 Gd1 N4 113.8(3) 4_656 . ?
O6 Gd1 Cu1 105.3(2) . . ?
O6 Gd1 Cu2 109.70(17) . 4_656 ?
O6 Gd1 O7 50.8(2) . . ?
O6 Gd1 N3 25.3(2) . . ?
O6 Gd1 O9 75.5(3) . . ?
O6 Gd1 O10 107.4(3) . . ?
O6 Gd1 N4 89.0(3) . . ?
O7 Gd1 Cu1 83.9(3) . . ?
O7 Gd1 Cu2 157.6(2) . 4_656 ?
O7 Gd1 N3 25.5(2) . . ?
O7 Gd1 O10 72.5(4) . . ?
O7 Gd1 N4 71.1(4) . . ?
N3 Gd1 Cu1 94.90(19) . . ?
N3 Gd1 Cu2 134.24(17) . 4_656 ?
O9 Gd1 Cu1 158.1(2) . . ?
O9 Gd1 Cu2 84.5(3) . 4_656 ?
O9 Gd1 O7 79.9(4) . . ?
O9 Gd1 N3 76.6(3) . . ?
O9 Gd1 O10 50.9(3) . . ?
O9 Gd1 N4 26.1(3) . . ?
O10 Gd1 Cu1 109.9(2) . . ?
O10 Gd1 Cu2 109.4(3) . 4_656 ?
O10 Gd1 N3 90.1(3) . . ?
O10 Gd1 N4 25.2(3) . . ?
N4 Gd1 Cu1 133.0(2) . . ?
N4 Gd1 Cu2 100.9(3) . 4_656 ?
N4 Gd1 N3 79.3(3) . . ?
Gd1 Cu1 Gd1 177.09(7) . 2_665 ?
O1 Cu1 Gd1 137.53(19) . 2_665 ?
O1 Cu1 Gd1 41.92(19) 2_665 2_665 ?
O1 Cu1 Gd1 137.53(19) 2_665 . ?
O1 Cu1 Gd1 41.92(19) . . ?
O1 Cu1 O1 165.4(4) 2_665 . ?
O1 Cu1 O2 96.4(3) . . ?
O1 Cu1 O2 96.4(3) 2_665 2_665 ?
O1 Cu1 O2 86.0(3) . 2_665 ?
O1 Cu1 O2 86.0(3) 2_665 . ?
O2 Cu1 Gd1 136.49(17) 2_665 2_665 ?
O2 Cu1 Gd1 136.50(17) . . ?
O2 Cu1 Gd1 44.18(17) . 2_665 ?
O2 Cu1 Gd1 44.18(17) 2_665 . ?
O2 Cu1 O2 161.6(4) . 2_665 ?
O3 Cu2 Gd1 41.70(18) . 3_566 ?
O3 Cu2 N1 89.4(3) . . ?
O3 Cu2 N2 165.5(3) . . ?
O3 Cu2 O5 112.6(3) . . ?
O4 Cu2 Gd1 42.96(19) . 3_566 ?
O4 Cu2 O3 83.2(3) . . ?
O4 Cu2 N1 166.8(3) . . ?
O4 Cu2 N2 94.0(3) . . ?
O4 Cu2 O5 79.9(3) . . ?
N1 Cu2 Gd1 126.8(2) . 3_566 ?
N1 Cu2 N2 95.8(3) . . ?
N1 Cu2 O5 93.0(3) . . ?
N2 Cu2 Gd1 136.9(2) . 3_566 ?
N2 Cu2 O5 80.7(3) . . ?
O5 Cu2 Gd1 90.4(2) . 3_566 ?
Cu1 O1 Gd1 104.1(3) . . ?
C1 O1 Gd1 133.1(6) . . ?
C1 O1 Cu1 122.8(6) . . ?
Cu2 O3 Gd1 103.6(3) . 3_566 ?
C2 O3 Gd1 130.1(5) . 3_566 ?
C2 O3 Cu2 124.4(5) . . ?
Cu1 O2 Gd1 100.8(2) . 2_665 ?
C3 O2 Gd1 128.3(5) . 2_665 ?
C3 O2 Cu1 126.9(5) . . ?
Cu2 O4 Gd1 102.6(3) . 3_566 ?
C11 O4 Gd1 133.0(6) . 3_566 ?
C11 O4 Cu2 121.6(6) . . ?
C5 N1 Cu2 123.2(6) . . ?
C9 N1 Cu2 115.6(7) . . ?
C9 N1 C5 119.2(8) . . ?
C13 N2 Cu2 120.3(6) . . ?
C13 N2 C17 119.1(8) . . ?
C17 N2 Cu2 120.6(6) . . ?
N3 O6 Gd1 97.2(5) . . ?
N3 O7 Gd1 96.2(6) . . ?
Cu2 O5 H5 136(3) . . ?
C10 O5 Cu2 113.9(8) . . ?
C10 O5 H5 109(3) . . ?
O8 N3 Gd1 177.5(8) . . ?
O8 N3 O6 121.8(8) . . ?
O8 N3 O7 122.3(9) . . ?
O6 N3 Gd1 57.5(4) . . ?
O6 N3 O7 115.8(8) . . ?
O7 N3 Gd1 58.3(5) . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.4(9) . . ?
C7 C6 H6 119.8 . . ?
N4 O9 Gd1 96.0(7) . . ?
N2 C13 C14 120.7(10) . . ?
N2 C13 C12 118.5(9) . . ?
C14 C13 C12 120.8(9) . . ?
N1 C5 C6 119.8(8) . . ?
N1 C5 C4 116.3(7) . . ?
C6 C5 C4 123.9(8) . . ?
N4 O10 Gd1 95.3(7) . . ?
O1 C1 H1A 108.9 . . ?
O1 C1 H1B 108.9 . . ?
O1 C1 C4 113.4(7) . . ?
H1A C1 H1B 107.7 . . ?
C4 C1 H1A 108.9 . . ?
C4 C1 H1B 108.9 . . ?
O3 C2 H2A 108.4 . . ?
O3 C2 H2B 108.4 . . ?
O3 C2 C4 115.7(7) . . ?
H2A C2 H2B 107.4 . . ?
C4 C2 H2A 108.4 . . ?
C4 C2 H2B 108.4 . . ?
N2 C17 H17 119.0 . . ?
N2 C17 C16 122.0(10) . . ?
C16 C17 H17 119.0 . . ?
C5 C4 C1 109.6(7) . . ?
C5 C4 C2 109.0(7) . . ?
C5 C4 C3 106.7(7) . . ?
C2 C4 C1 107.6(7) . . ?
C2 C4 C3 113.2(7) . . ?
C3 C4 C1 110.8(7) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.1(9) . . ?
C8 C7 H7 120.4 . . ?
C7 C8 H8 120.7 . . ?
C7 C8 C9 118.5(9) . . ?
C9 C8 H8 120.7 . . ?
O2 C3 C4 115.3(7) . . ?
O2 C3 H3A 108.5 . . ?
O2 C3 H3B 108.5 . . ?
C4 C3 H3A 108.5 . . ?
C4 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
C13 C14 H14 120.7 . . ?
C15 C14 C13 118.7(10) . . ?
C15 C14 H14 120.7 . . ?
C13 C12 H12 106.7 . . ?
C13 C12 C11 111.9(10) . . ?
C11 C12 H12 106.7 . . ?
C10 C12 C13 113.7(11) . . ?
C10 C12 H12 106.7 . . ?
C10 C12 C11 110.6(10) . . ?
O9 N4 Gd1 57.9(6) . . ?
O10 N4 Gd1 59.4(6) . . ?
O10 N4 O9 115.7(10) . . ?
O11 N4 Gd1 167.9(11) . . ?
O11 N4 O9 122.6(11) . . ?
O11 N4 O10 121.7(11) . . ?
N1 C9 C8 123.0(9) . . ?
N1 C9 H9 118.5 . . ?
C8 C9 H9 118.5 . . ?
O4 C11 C12 112.9(9) . . ?
O4 C11 H11A 109.0 . . ?
O4 C11 H11B 109.0 . . ?
C12 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C17 C16 H16 120.5 . . ?
C15 C16 C17 119.0(11) . . ?
C15 C16 H16 120.5 . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.5(11) . . ?
C16 C15 H15 119.7 . . ?
O5 C10 C12 112.7(10) . . ?
O5 C10 H10A 109.1 . . ?
O5 C10 H10B 109.1 . . ?
C12 C10 H10A 109.1 . . ?
C12 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N5 C18 C19 177(3) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 Cu1 O1 Gd1 -175.74(10) 2_665 . . . ?
Gd1 Cu1 O1 C1 2.6(9) 2_665 . . . ?
Gd1 Cu1 O1 C1 178.3(9) . . . . ?
Gd1 O1 C1 C4 -132.8(7) . . . . ?
Gd1 O3 C2 C4 164.7(5) 3_566 . . . ?
Gd1 O2 C3 C4 -176.9(5) 2_665 . . . ?
Gd1 O4 C11 C12 131.1(9) 3_566 . . . ?
Gd1 O6 N3 O8 -177.2(9) . . . . ?
Gd1 O6 N3 O7 -0.7(10) . . . . ?
Gd1 O7 N3 O8 177.1(9) . . . . ?
Gd1 O7 N3 O6 0.7(10) . . . . ?
Gd1 O9 N4 O10 -14.6(14) . . . . ?
Gd1 O9 N4 O11 165.6(13) . . . . ?
Gd1 O10 N4 O9 14.3(14) . . . . ?
Gd1 O10 N4 O11 -165.9(13) . . . . ?
Cu1 O1 C1 C4 49.4(10) . . . . ?
Cu1 O2 C3 C4 -24.0(11) . . . . ?
Cu2 O3 C2 C4 3.2(11) . . . . ?
Cu2 O4 C11 C12 -26.3(14) . . . . ?
Cu2 N1 C5 C6 -161.3(7) . . . . ?
Cu2 N1 C5 C4 18.0(10) . . . . ?
Cu2 N1 C9 C8 163.6(8) . . . . ?
Cu2 N2 C13 C14 -179.4(9) . . . . ?
Cu2 N2 C13 C12 -2.3(14) . . . . ?
Cu2 N2 C17 C16 178.5(8) . . . . ?
Cu2 O5 C10 C12 -14.0(14) . . . . ?
O1 Cu1 O1 Gd1 -96.0(2) 2_665 . . . ?
O1 Cu1 O1 C1 82.3(7) 2_665 . . . ?
O1 C1 C4 C5 173.3(7) . . . . ?
O1 C1 C4 C2 55.0(10) . . . . ?
O1 C1 C4 C3 -69.2(10) . . . . ?
O3 C2 C4 C5 53.8(10) . . . . ?
O3 C2 C4 C1 172.5(7) . . . . ?
O3 C2 C4 C3 -64.7(10) . . . . ?
O2 Cu1 O1 Gd1 165.5(3) . . . . ?
O2 Cu1 O1 Gd1 3.8(3) 2_665 . . . ?
O2 Cu1 O1 C1 -16.2(7) . . . . ?
O2 Cu1 O1 C1 -177.9(7) 2_665 . . . ?
N1 C5 C4 C1 176.8(7) . . . . ?
N1 C5 C4 C2 -65.8(9) . . . . ?
N1 C5 C4 C3 56.8(9) . . . . ?
N2 C13 C14 C15 1.1(18) . . . . ?
N2 C13 C12 C11 -54.1(14) . . . . ?
N2 C13 C12 C10 72.1(13) . . . . ?
N2 C17 C16 C15 0.5(18) . . . . ?
C6 C5 C4 C1 -3.9(12) . . . . ?
C6 C5 C4 C2 113.5(9) . . . . ?
C6 C5 C4 C3 -123.9(9) . . . . ?
C6 C7 C8 C9 1.7(15) . . . . ?
C13 N2 C17 C16 0.3(15) . . . . ?
C13 C14 C15 C16 0(2) . . . . ?
C13 C12 C11 O4 70.5(14) . . . . ?
C13 C12 C10 O5 -53.4(15) . . . . ?
C5 N1 C9 C8 -1.1(14) . . . . ?
C5 C6 C7 C8 -0.7(16) . . . . ?
C5 C4 C3 O2 174.1(7) . . . . ?
C1 C4 C3 O2 54.9(10) . . . . ?
C2 C4 C3 O2 -66.0(10) . . . . ?
C17 N2 C13 C14 -1.1(16) . . . . ?
C17 N2 C13 C12 176.0(10) . . . . ?
C17 C16 C15 C14 0(2) . . . . ?
C7 C6 C5 N1 -1.2(14) . . . . ?
C7 C6 C5 C4 179.5(9) . . . . ?
C7 C8 C9 N1 -0.9(15) . . . . ?
C14 C13 C12 C11 122.9(12) . . . . ?
C14 C13 C12 C10 -110.9(13) . . . . ?
C12 C13 C14 C15 -175.9(12) . . . . ?
C9 N1 C5 C6 2.1(13) . . . . ?
C9 N1 C5 C4 -178.6(8) . . . . ?
C11 C12 C10 O5 73.5(14) . . . . ?
C10 C12 C11 O4 -57.4(14) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 180.1 30.8 ?
2 0.500 0.500 0.000 180.1 26.4 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.851
_oxdiff_exptl_absorpt_empirical_full_min 0.619
####################################################################### 
# 
# 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_y4cu6_new
_audit_block_doi                 10.5517/ccdc.csd.cc2kky9d
_database_code_depnum_ccdc_archive 'CCDC 2370734'
loop_
_audit_author_name
_audit_author_address
'Antonis Anastassiades'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-07-15 deposited with the CCDC.	2024-09-09 downloaded from the CCDC.
;
_audit_creation_date             2024-07-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H80 Cu6 N16 O44 Y4, 4(C2 H3 N)'
_chemical_formula_sum            'C76 H92 Cu6 N20 O44 Y4'
_chemical_formula_weight         2726.57
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C72 H86 Cu6 Y4 N18 O44'
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'
Cu Cu -1.9646 0.5888 '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'
Y Y -0.2670 2.0244 '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           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   17.75090(10)
_cell_length_b                   17.75090(10)
_cell_length_c                   16.2759(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5128.45(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    28906
_cell_measurement_temperature    150.1(2)
_cell_measurement_theta_max      79.8550
_cell_measurement_theta_min      2.5140
_shelx_estimated_absorpt_T_max   0.616
_shelx_estimated_absorpt_T_min   0.215
_exptl_absorpt_coefficient_mu    5.060
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.414
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2740
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 0 8 0.1156
2 -7 8 0.1514
9 -6 -3 0.1117
-6 9 -4 0.1036
-9 7 3 0.1409
7 9 -1 0.0437
7 -8 -3 0.0966
-8 -8 1 0.0488
9 6 4 0.0846
3 9 5 0.0891
-9 -6 -4 0.0926
-3 -11 -2 0.0894
0 5 -9 0.2429
-10 4 -5 0.1006
11 4 -1 0.0768
1 11 -3 0.0894
7 -2 8 0.1546
0 8 8 0.1089
2 11 1 0.0734

_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.439
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.106
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-7.2685 0.4841 8.1852 0.1522 0.6555 0.7397
1.8322 -7.4422 7.8840 0.2241 0.9375 -0.2663
9.2505 -5.9376 -3.1859 -0.0029 -0.0326 -0.9995
-6.4122 8.5928 -3.8754 -0.1585 -0.6518 0.7416
-8.7095 6.9236 2.7731 -0.0813 -0.0304 0.9962
7.2135 8.9470 -0.6717 -0.9524 -0.2838 -0.1114
7.4795 -8.2922 -2.6411 0.2328 0.0755 -0.9696
-8.3476 -7.8461 1.0549 0.9280 0.2756 0.2508
9.0552 5.7832 3.8007 -0.9371 0.2211 -0.2701
3.4436 9.2538 5.4581 -0.9203 0.2206 0.3232
-9.0784 -5.7571 -3.7871 0.9362 -0.2209 0.2732
-3.0444 -10.9736 -1.6354 0.9275 0.1723 -0.3317
0.1688 5.0305 -9.4989 -0.1281 -0.9914 -0.0253
-9.5655 4.0777 -4.5435 0.3202 -0.5940 0.7380
11.0002 3.9998 -0.9999 -0.8075 -0.1335 -0.6107
1.0003 10.9998 -3.0000 -0.7188 -0.5963 0.3567
6.9999 -2.0000 8.0001 -0.4071 0.8166 -0.3750
-0.0000 8.0000 8.0000 -0.7183 0.4591 0.5715
2.0002 10.9998 1.0000 -0.8614 -0.2365 0.3895

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35166
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.521
_diffrn_ambient_temperature      150.1(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     48.00 106.00   0.50    1.50    --  111.50 -99.00 -90.00  116
  2  ω     50.00 107.00   0.50    1.50    --  111.50 -79.00 -37.00  114
  3  ω    -18.00  55.00   0.50    0.50    --   49.55 -79.00 -37.00  146
  4  ω    -18.00  21.00   0.50    0.50    --   49.55 -19.00 -30.00   78
  5  ω     65.00 103.00   0.50    1.50    --  111.50   0.00  90.00   76
  6  ω    109.00 176.00   0.50    1.50    --  111.50  38.00  60.00  134
  7  ω    100.00 175.00   0.50    1.50    --  111.50  57.00  30.00  150
  8  ω    115.00 177.00   0.50    1.50    --  111.50  79.00  86.00  124
  9  ω     75.00 119.00   0.50    0.50    --   49.55 126.00   0.00   88
 10  ω     77.00 119.00   0.50    0.50    --   49.55 126.00 -60.00   84
 11  ω     77.00 119.00   0.50    0.50    --   49.55 126.00-150.00   84
 12  ω    -68.00  19.00   0.50    0.50    --  -49.55  79.00  86.00  174
 13  ω    -85.00 -34.00   0.50    1.50    -- -106.00  79.00  86.00  102
 14  ω    -65.00 -34.00   0.50    1.50    -- -106.00  57.00  60.00   62
 15  ω    -62.00 -37.00   0.50    1.50    -- -106.00  57.00  30.00   50
 16  ω    -20.00  19.00   0.50    0.50    --  -49.55  19.00-180.00   78
 17  ω    -62.00 -36.00   0.50    1.50    -- -106.00  57.00-120.00   52
 18  ω    -64.00 -36.00   0.50    1.50    -- -106.00  57.00 -90.00   56
 19  ω   -154.00-107.00   0.50    1.50    -- -106.00   0.00-150.00   94
 20  ω   -141.00-101.00   0.50    1.50    -- -106.00 -38.00-180.00   80
 21  ω   -162.00-129.00   0.50    1.50    -- -106.00 -79.00 -37.00   66
 22  ω   -174.00 -94.00   0.50    1.50    -- -106.00 -57.00   0.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0511480000
_diffrn_orient_matrix_UB_12      -0.0669271000
_diffrn_orient_matrix_UB_13      -0.0228656000
_diffrn_orient_matrix_UB_21      0.0070777000
_diffrn_orient_matrix_UB_22      -0.0308041000
_diffrn_orient_matrix_UB_23      0.0881862000
_diffrn_orient_matrix_UB_31      -0.0698271000
_diffrn_orient_matrix_UB_32      0.0457723000
_diffrn_orient_matrix_UB_33      0.0256601000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4544
_reflns_number_total             4579
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 
;
 Flack x determined using 1999 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4579
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0215
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+2.1113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0595
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 C11-H5
 1.878048 with sigma of 0.02
 Cu2-H5
 3.065512 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C12(H12)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B), C11(H11A,H11B)
3.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C17(H17), C14(H14), C6(H6), C8(H8), C7(H7), C16(H16), C15(H15)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Y1 Y 0.45884(2) 0.67840(2) 0.66072(2) 0.02984(9) Uani 1 1 d . . . . .
Cu1 Cu 0.500000 0.500000 0.65564(5) 0.02982(16) Uani 1 2 d S T P . .
Cu2 Cu 0.25950(3) 0.35419(3) 0.49180(3) 0.03255(13) Uani 1 1 d D . . . .
O1 O 0.41476(13) 0.56202(14) 0.67049(17) 0.0342(6) Uani 1 1 d . . . . .
O2 O 0.44663(14) 0.40739(14) 0.63742(16) 0.0318(6) Uani 1 1 d . . . . .
O3 O 0.30095(14) 0.45448(15) 0.47493(16) 0.0337(5) Uani 1 1 d . . . . .
O4 O 0.29546(16) 0.33846(15) 0.38100(17) 0.0393(6) Uani 1 1 d . . . . .
O9 O 0.39081(15) 0.69562(17) 0.79042(16) 0.0418(7) Uani 1 1 d . . . . .
O6 O 0.47174(19) 0.81233(18) 0.6911(2) 0.0557(8) Uani 1 1 d . . . . .
O10 O 0.50890(17) 0.6724(2) 0.80109(19) 0.0529(8) Uani 1 1 d . . . . .
O11 O 0.44211(19) 0.6911(2) 0.91168(19) 0.0586(9) Uani 1 1 d . . . . .
N1 N 0.20943(17) 0.39005(17) 0.5948(2) 0.0333(6) Uani 1 1 d . . . . .
O7 O 0.57602(17) 0.75543(17) 0.6637(2) 0.0545(8) Uani 1 1 d . . . . .
N4 N 0.44680(18) 0.6862(2) 0.8374(2) 0.0419(8) Uani 1 1 d . . . . .
N2 N 0.24586(18) 0.24384(18) 0.51481(19) 0.0350(7) Uani 1 1 d . . . . .
O5 O 0.14112(18) 0.3344(2) 0.4245(2) 0.0579(8) Uani 1 1 d D . . . .
H5 H 0.0990(15) 0.357(3) 0.423(3) 0.087 Uiso 1 1 d D U . . .
C13 C 0.2227(2) 0.1968(2) 0.4547(3) 0.0384(9) Uani 1 1 d . . . . .
C9 C 0.1383(2) 0.3671(2) 0.6064(2) 0.0391(9) Uani 1 1 d . . . . .
H9 H 0.120176 0.325449 0.575550 0.047 Uiso 1 1 calc R U . . .
N3 N 0.5442(2) 0.8129(2) 0.6926(3) 0.0562(10) Uani 1 1 d . . . . .
C1 C 0.3432(2) 0.5314(2) 0.6869(2) 0.0331(8) Uani 1 1 d . . . . .
H1A H 0.305405 0.572357 0.685234 0.040 Uiso 1 1 calc R U . . .
H1B H 0.343201 0.510230 0.743208 0.040 Uiso 1 1 calc R U . . .
O8 O 0.5800(2) 0.8662(2) 0.7200(3) 0.0917(16) Uani 1 1 d . . . . .
C4 C 0.3197(2) 0.4692(2) 0.6259(2) 0.0314(7) Uani 1 1 d . . . . .
C5 C 0.2379(2) 0.4478(2) 0.6405(2) 0.0320(8) Uani 1 1 d . . . . .
C2 C 0.3277(2) 0.5012(2) 0.5373(2) 0.0312(7) Uani 1 1 d . . . . .
H2A H 0.300458 0.549806 0.534471 0.037 Uiso 1 1 calc R U . . .
H2B H 0.381675 0.511762 0.526885 0.037 Uiso 1 1 calc R U . . .
C17 C 0.2603(2) 0.2150(2) 0.5893(2) 0.0370(8) Uani 1 1 d . . . . .
H17 H 0.276497 0.248180 0.631562 0.044 Uiso 1 1 calc R U . . .
C12 C 0.2109(3) 0.2292(2) 0.3707(3) 0.0458(10) Uani 1 1 d . . . . .
H12 H 0.202996 0.185407 0.333098 0.055 Uiso 1 1 calc R U . . .
C14 C 0.2135(2) 0.1204(2) 0.4698(3) 0.0435(9) Uani 1 1 d . . . . .
H14 H 0.197233 0.087743 0.427088 0.052 Uiso 1 1 calc R U . . .
C6 C 0.1913(2) 0.4824(2) 0.6982(2) 0.0374(8) Uani 1 1 d . . . . .
H6 H 0.210884 0.521669 0.731572 0.045 Uiso 1 1 calc R U . . .
C8 C 0.0901(2) 0.4016(2) 0.6616(3) 0.0434(8) Uani 1 1 d . . . . .
H8 H 0.039527 0.385071 0.667472 0.052 Uiso 1 1 calc R U . . .
C7 C 0.1173(2) 0.4604(3) 0.7075(3) 0.0424(9) Uani 1 1 d . . . . .
H7 H 0.085490 0.485714 0.745462 0.051 Uiso 1 1 calc R U . . .
C3 C 0.3681(2) 0.3975(2) 0.6404(2) 0.0327(8) Uani 1 1 d . . . . .
H3A H 0.354892 0.376595 0.694956 0.039 Uiso 1 1 calc R U . . .
H3B H 0.353932 0.359480 0.598730 0.039 Uiso 1 1 calc R U . . .
C16 C 0.2526(3) 0.1396(2) 0.6074(3) 0.0462(10) Uani 1 1 d . . . . .
H16 H 0.264102 0.120990 0.660698 0.055 Uiso 1 1 calc R U . . .
C15 C 0.2281(3) 0.0921(3) 0.5467(3) 0.0510(11) Uani 1 1 d . . . . .
H15 H 0.221153 0.040024 0.557689 0.061 Uiso 1 1 calc R U . . .
C10 C 0.2822(3) 0.2698(2) 0.3400(3) 0.0486(10) Uani 1 1 d . . . . .
H10A H 0.326196 0.236327 0.347783 0.058 Uiso 1 1 calc R U . . .
H10B H 0.277017 0.279726 0.280369 0.058 Uiso 1 1 calc R U . . .
C11 C 0.1423(3) 0.2777(3) 0.3628(3) 0.0603(13) Uani 1 1 d D . . . .
H11A H 0.141766 0.301644 0.307876 0.072 Uiso 1 1 calc R U . . .
H11B H 0.096630 0.245971 0.367721 0.072 Uiso 1 1 calc R U . . .
C18 C 0.0545(3) 0.5802(3) 0.4672(5) 0.0782(18) Uani 1 1 d . . . . .
C19 C 0.1263(3) 0.5600(4) 0.5008(5) 0.088(2) Uani 1 1 d . . . . .
H19A H 0.144660 0.514146 0.473867 0.132 Uiso 1 1 calc R U . . .
H19B H 0.121272 0.550991 0.559904 0.132 Uiso 1 1 calc R U . . .
H19C H 0.162216 0.601095 0.491437 0.132 Uiso 1 1 calc R U . . .
N5 N -0.0025(3) 0.5987(4) 0.4422(5) 0.107(2) Uani 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
Y1 Cu1 3.2509(3) . ?
Y1 Cu2 3.2907(6) 3_566 ?
Y1 O1 2.215(3) . ?
Y1 O2 2.297(3) 2_665 ?
Y1 O3 2.239(3) 3_566 ?
Y1 O4 2.290(3) 3_566 ?
Y1 O9 2.451(3) . ?
Y1 O6 2.439(3) . ?
Y1 O10 2.454(3) . ?
Y1 O7 2.490(3) . ?
Y1 N4 2.887(4) . ?
Y1 N3 2.874(4) . ?
Cu1 O1 1.887(2) . ?
Cu1 O1 1.887(2) 2_665 ?
Cu1 O2 1.920(2) . ?
Cu1 O2 1.920(2) 2_665 ?
Cu2 O3 1.946(3) . ?
Cu2 O4 1.933(3) . ?
Cu2 N1 2.001(3) . ?
Cu2 N2 2.009(3) . ?
Cu2 O5 2.396(3) . ?
O1 C1 1.406(4) . ?
O2 C3 1.406(4) . ?
O3 C2 1.395(4) . ?
O4 C10 1.410(5) . ?
O9 N4 1.265(4) . ?
O6 N3 1.286(5) . ?
O10 N4 1.275(5) . ?
O11 N4 1.215(5) . ?
N1 C9 1.341(5) . ?
N1 C5 1.364(5) . ?
O7 N3 1.257(5) . ?
N2 C13 1.350(5) . ?
N2 C17 1.340(5) . ?
O5 H5 0.847(13) . ?
O5 C11 1.422(7) . ?
C13 C12 1.497(6) . ?
C13 C14 1.389(6) . ?
C9 H9 0.9500 . ?
C9 C8 1.382(6) . ?
N3 O8 1.224(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C4 1.544(5) . ?
C4 C5 1.518(5) . ?
C4 C2 1.556(5) . ?
C4 C3 1.553(5) . ?
C5 C6 1.394(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C17 H17 0.9500 . ?
C17 C16 1.378(6) . ?
C12 H12 1.0000 . ?
C12 C10 1.540(6) . ?
C12 C11 1.496(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.372(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.379(6) . ?
C8 H8 0.9500 . ?
C8 C7 1.372(6) . ?
C7 H7 0.9500 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C16 H16 0.9500 . ?
C16 C15 1.371(7) . ?
C15 H15 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C18 C19 1.433(9) . ?
C18 N5 1.138(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

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
Cu1 Y1 Cu2 115.721(17) . 3_566 ?
O1 Y1 Cu1 34.17(6) . . ?
O1 Y1 Cu2 99.62(7) . 3_566 ?
O1 Y1 O2 69.62(8) . 2_665 ?
O1 Y1 O3 102.20(10) . 3_566 ?
O1 Y1 O4 83.14(10) . 3_566 ?
O1 Y1 O9 83.13(10) . . ?
O1 Y1 O6 158.09(11) . . ?
O1 Y1 O10 91.16(12) . . ?
O1 Y1 O7 143.71(10) . . ?
O1 Y1 N4 86.98(10) . . ?
O1 Y1 N3 161.42(12) . . ?
O2 Y1 Cu1 35.52(6) 2_665 . ?
O2 Y1 Cu2 120.66(6) 2_665 3_566 ?
O2 Y1 O9 125.78(9) 2_665 . ?
O2 Y1 O6 127.65(10) 2_665 . ?
O2 Y1 O10 81.96(10) 2_665 . ?
O2 Y1 O7 75.94(9) 2_665 . ?
O2 Y1 N4 104.50(10) 2_665 . ?
O2 Y1 N3 101.25(10) 2_665 . ?
O3 Y1 Cu1 98.17(7) 3_566 . ?
O3 Y1 Cu2 35.11(7) 3_566 3_566 ?
O3 Y1 O2 88.34(9) 3_566 2_665 ?
O3 Y1 O4 69.04(10) 3_566 3_566 ?
O3 Y1 O9 144.26(9) 3_566 . ?
O3 Y1 O6 92.50(11) 3_566 . ?
O3 Y1 O10 159.66(11) 3_566 . ?
O3 Y1 O7 87.60(12) 3_566 . ?
O3 Y1 N4 166.31(10) 3_566 . ?
O3 Y1 N3 93.44(12) 3_566 . ?
O4 Y1 Cu1 113.56(8) 3_566 . ?
O4 Y1 Cu2 35.07(7) 3_566 3_566 ?
O4 Y1 O2 140.09(10) 3_566 2_665 ?
O4 Y1 O9 76.72(9) 3_566 . ?
O4 Y1 O6 87.15(11) 3_566 . ?
O4 Y1 O10 128.53(10) 3_566 . ?
O4 Y1 O7 132.39(11) 3_566 . ?
O4 Y1 N4 102.51(10) 3_566 . ?
O4 Y1 N3 112.15(12) 3_566 . ?
O9 Y1 Cu1 104.72(7) . . ?
O9 Y1 Cu2 109.25(7) . 3_566 ?
O9 Y1 O10 51.83(10) . . ?
O9 Y1 O7 109.05(11) . . ?
O9 Y1 N4 25.80(9) . . ?
O9 Y1 N3 90.04(11) . . ?
O6 Y1 Cu1 158.99(9) . . ?
O6 Y1 Cu2 83.08(9) . 3_566 ?
O6 Y1 O9 75.52(11) . . ?
O6 Y1 O10 79.62(13) . . ?
O6 Y1 O7 51.85(10) . . ?
O6 Y1 N4 75.99(11) . . ?
O6 Y1 N3 26.43(11) . . ?
O10 Y1 Cu1 84.24(9) . . ?
O10 Y1 Cu2 157.14(8) . 3_566 ?
O10 Y1 O7 72.74(13) . . ?
O10 Y1 N4 26.03(10) . . ?
O10 Y1 N3 71.18(13) . . ?
O7 Y1 Cu1 110.35(7) . . ?
O7 Y1 Cu2 107.60(9) . 3_566 ?
O7 Y1 N4 90.92(11) . . ?
O7 Y1 N3 25.85(10) . . ?
N4 Y1 Cu1 95.10(8) . . ?
N4 Y1 Cu2 133.91(7) . 3_566 ?
N3 Y1 Cu1 134.03(9) . . ?
N3 Y1 Cu2 98.94(10) . 3_566 ?
N3 Y1 N4 79.59(11) . . ?
Y1 Cu1 Y1 177.08(3) . 2_665 ?
O1 Cu1 Y1 138.18(8) . 2_665 ?
O1 Cu1 Y1 41.25(8) 2_665 2_665 ?
O1 Cu1 Y1 138.19(8) 2_665 . ?
O1 Cu1 Y1 41.25(8) . . ?
O1 Cu1 O1 165.27(18) 2_665 . ?
O1 Cu1 O2 97.10(11) . . ?
O1 Cu1 O2 97.10(11) 2_665 2_665 ?
O1 Cu1 O2 85.18(11) . 2_665 ?
O1 Cu1 O2 85.18(11) 2_665 . ?
O2 Cu1 Y1 136.63(7) 2_665 2_665 ?
O2 Cu1 Y1 136.63(7) . . ?
O2 Cu1 Y1 44.02(7) . 2_665 ?
O2 Cu1 Y1 44.02(7) 2_665 . ?
O2 Cu1 O2 162.24(16) . 2_665 ?
O3 Cu2 Y1 41.44(8) . 4_656 ?
O3 Cu2 N1 89.72(12) . . ?
O3 Cu2 N2 164.58(12) . . ?
O3 Cu2 O5 113.66(11) . . ?
O4 Cu2 Y1 42.88(8) . 4_656 ?
O4 Cu2 O3 82.86(11) . . ?
O4 Cu2 N1 166.87(13) . . ?
O4 Cu2 N2 94.18(12) . . ?
O4 Cu2 O5 80.90(12) . . ?
N1 Cu2 Y1 126.94(9) . 4_656 ?
N1 Cu2 N2 95.77(13) . . ?
N1 Cu2 O5 92.30(13) . . ?
N2 Cu2 Y1 137.01(9) . 4_656 ?
N2 Cu2 O5 80.58(12) . . ?
O5 Cu2 Y1 91.82(9) . 4_656 ?
Cu1 O1 Y1 104.57(11) . . ?
C1 O1 Y1 133.9(2) . . ?
C1 O1 Cu1 121.5(2) . . ?
Cu1 O2 Y1 100.46(10) . 2_665 ?
C3 O2 Y1 129.5(2) . 2_665 ?
C3 O2 Cu1 126.2(2) . . ?
Cu2 O3 Y1 103.45(11) . 4_656 ?
C2 O3 Y1 129.9(2) . 4_656 ?
C2 O3 Cu2 124.8(2) . . ?
Cu2 O4 Y1 102.05(11) . 4_656 ?
C10 O4 Y1 134.4(3) . 4_656 ?
C10 O4 Cu2 120.8(2) . . ?
N4 O9 Y1 96.7(2) . . ?
N3 O6 Y1 96.0(2) . . ?
N4 O10 Y1 96.3(2) . . ?
C9 N1 Cu2 116.1(3) . . ?
C9 N1 C5 120.0(3) . . ?
C5 N1 Cu2 122.1(2) . . ?
N3 O7 Y1 94.4(2) . . ?
O9 N4 Y1 57.48(18) . . ?
O9 N4 O10 115.1(3) . . ?
O10 N4 Y1 57.6(2) . . ?
O11 N4 Y1 178.7(3) . . ?
O11 N4 O9 122.6(3) . . ?
O11 N4 O10 122.3(4) . . ?
C13 N2 Cu2 120.3(3) . . ?
C17 N2 Cu2 121.2(3) . . ?
C17 N2 C13 118.6(3) . . ?
Cu2 O5 H5 136(2) . . ?
C11 O5 Cu2 114.5(3) . . ?
C11 O5 H5 109(2) . . ?
N2 C13 C12 117.8(3) . . ?
N2 C13 C14 120.7(4) . . ?
C14 C13 C12 121.4(4) . . ?
N1 C9 H9 118.7 . . ?
N1 C9 C8 122.7(4) . . ?
C8 C9 H9 118.7 . . ?
O6 N3 Y1 57.5(2) . . ?
O7 N3 Y1 59.7(2) . . ?
O7 N3 O6 115.9(4) . . ?
O8 N3 Y1 168.9(4) . . ?
O8 N3 O6 122.1(4) . . ?
O8 N3 O7 122.0(4) . . ?
O1 C1 H1A 108.9 . . ?
O1 C1 H1B 108.9 . . ?
O1 C1 C4 113.5(3) . . ?
H1A C1 H1B 107.7 . . ?
C4 C1 H1A 108.9 . . ?
C4 C1 H1B 108.9 . . ?
C1 C4 C2 108.0(3) . . ?
C1 C4 C3 109.7(3) . . ?
C5 C4 C1 109.7(3) . . ?
C5 C4 C2 109.0(3) . . ?
C5 C4 C3 107.5(3) . . ?
C3 C4 C2 113.0(3) . . ?
N1 C5 C4 117.2(3) . . ?
N1 C5 C6 118.6(3) . . ?
C6 C5 C4 124.2(3) . . ?
O3 C2 C4 115.2(3) . . ?
O3 C2 H2A 108.5 . . ?
O3 C2 H2B 108.5 . . ?
C4 C2 H2A 108.5 . . ?
C4 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
N2 C17 H17 118.5 . . ?
N2 C17 C16 123.1(4) . . ?
C16 C17 H17 118.5 . . ?
C13 C12 H12 106.3 . . ?
C13 C12 C10 111.2(4) . . ?
C10 C12 H12 106.3 . . ?
C11 C12 C13 114.4(4) . . ?
C11 C12 H12 106.3 . . ?
C11 C12 C10 111.8(4) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 119.8(4) . . ?
C15 C14 H14 120.1 . . ?
C5 C6 H6 119.5 . . ?
C7 C6 C5 121.0(4) . . ?
C7 C6 H6 119.5 . . ?
C9 C8 H8 120.9 . . ?
C7 C8 C9 118.3(4) . . ?
C7 C8 H8 120.9 . . ?
C6 C7 H7 120.3 . . ?
C8 C7 C6 119.4(4) . . ?
C8 C7 H7 120.3 . . ?
O2 C3 C4 116.2(3) . . ?
O2 C3 H3A 108.2 . . ?
O2 C3 H3B 108.2 . . ?
C4 C3 H3A 108.2 . . ?
C4 C3 H3B 108.2 . . ?
H3A C3 H3B 107.4 . . ?
C17 C16 H16 120.8 . . ?
C15 C16 C17 118.3(4) . . ?
C15 C16 H16 120.8 . . ?
C14 C15 C16 119.5(4) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
O4 C10 C12 112.8(4) . . ?
O4 C10 H10A 109.0 . . ?
O4 C10 H10B 109.0 . . ?
C12 C10 H10A 109.0 . . ?
C12 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
O5 C11 C12 111.0(4) . . ?
O5 C11 H11A 109.4 . . ?
O5 C11 H11B 109.4 . . ?
C12 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
N5 C18 C19 177.4(9) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Y1 Cu1 O1 Y1 175.69(4) 2_665 . . . ?
Y1 Cu1 O1 C1 -2.2(3) 2_665 . . . ?
Y1 Cu1 O1 C1 -177.8(3) . . . . ?
Y1 O1 C1 C4 131.8(3) . . . . ?
Y1 O2 C3 C4 176.8(2) 2_665 . . . ?
Y1 O3 C2 C4 -164.2(2) 4_656 . . . ?
Y1 O4 C10 C12 -130.6(3) 4_656 . . . ?
Y1 O9 N4 O10 -0.6(4) . . . . ?
Y1 O9 N4 O11 178.4(4) . . . . ?
Y1 O6 N3 O7 13.5(5) . . . . ?
Y1 O6 N3 O8 -166.9(5) . . . . ?
Y1 O10 N4 O9 0.6(4) . . . . ?
Y1 O10 N4 O11 -178.5(4) . . . . ?
Y1 O7 N3 O6 -13.2(5) . . . . ?
Y1 O7 N3 O8 167.2(5) . . . . ?
Cu1 O1 C1 C4 -51.1(4) . . . . ?
Cu1 O2 C3 C4 23.3(4) . . . . ?
Cu2 O3 C2 C4 -2.4(4) . . . . ?
Cu2 O4 C10 C12 27.0(5) . . . . ?
Cu2 N1 C9 C8 -162.7(3) . . . . ?
Cu2 N1 C5 C4 -17.4(4) . . . . ?
Cu2 N1 C5 C6 163.6(3) . . . . ?
Cu2 N2 C13 C12 2.5(5) . . . . ?
Cu2 N2 C13 C14 179.6(3) . . . . ?
Cu2 N2 C17 C16 -179.1(3) . . . . ?
Cu2 O5 C11 C12 16.0(5) . . . . ?
O1 Cu1 O1 Y1 96.23(10) 2_665 . . . ?
O1 Cu1 O1 C1 -81.6(3) 2_665 . . . ?
O1 C1 C4 C5 -171.7(3) . . . . ?
O1 C1 C4 C2 -53.1(4) . . . . ?
O1 C1 C4 C3 70.5(4) . . . . ?
O2 Cu1 O1 Y1 -165.68(12) . . . . ?
O2 Cu1 O1 Y1 -3.39(12) 2_665 . . . ?
O2 Cu1 O1 C1 178.8(3) 2_665 . . . ?
O2 Cu1 O1 C1 16.5(3) . . . . ?
N1 C9 C8 C7 -1.8(6) . . . . ?
N1 C5 C6 C7 -1.8(6) . . . . ?
N2 C13 C12 C10 55.0(5) . . . . ?
N2 C13 C12 C11 -72.8(5) . . . . ?
N2 C13 C14 C15 0.1(7) . . . . ?
N2 C17 C16 C15 -1.0(7) . . . . ?
C13 N2 C17 C16 0.1(6) . . . . ?
C13 C12 C10 O4 -72.1(5) . . . . ?
C13 C12 C11 O5 52.4(5) . . . . ?
C13 C14 C15 C16 -1.0(7) . . . . ?
C9 N1 C5 C4 178.2(3) . . . . ?
C9 N1 C5 C6 -0.8(5) . . . . ?
C9 C8 C7 C6 -0.8(6) . . . . ?
C1 C4 C5 N1 -176.1(3) . . . . ?
C1 C4 C5 C6 2.7(5) . . . . ?
C1 C4 C2 O3 -173.5(3) . . . . ?
C1 C4 C3 O2 -55.0(4) . . . . ?
C4 C5 C6 C7 179.4(4) . . . . ?
C5 N1 C9 C8 2.6(6) . . . . ?
C5 C4 C2 O3 -54.4(4) . . . . ?
C5 C4 C3 O2 -174.2(3) . . . . ?
C5 C6 C7 C8 2.6(6) . . . . ?
C2 C4 C5 N1 65.8(4) . . . . ?
C2 C4 C5 C6 -115.3(4) . . . . ?
C2 C4 C3 O2 65.6(4) . . . . ?
C17 N2 C13 C12 -176.7(4) . . . . ?
C17 N2 C13 C14 0.4(6) . . . . ?
C17 C16 C15 C14 1.4(7) . . . . ?
C12 C13 C14 C15 177.1(4) . . . . ?
C14 C13 C12 C10 -122.1(4) . . . . ?
C14 C13 C12 C11 110.0(5) . . . . ?
C3 C4 C5 N1 -56.9(4) . . . . ?
C3 C4 C5 C6 122.0(4) . . . . ?
C3 C4 C2 O3 64.9(4) . . . . ?
C10 C12 C11 O5 -75.1(5) . . . . ?
C11 C12 C10 O4 57.2(5) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 170.6 38.5 ?
2 0.500 0.500 0.000 170.6 37.7 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.389
_oxdiff_exptl_absorpt_empirical_full_min 0.721
####################################################################### 
# 
# 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_at_dy4cu6_new
_audit_block_doi                 10.5517/ccdc.csd.cc2kky8c
_database_code_depnum_ccdc_archive 'CCDC 2370733'
loop_
_audit_author_name
_audit_author_address
'Antonis Anastassiades'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-07-15 deposited with the CCDC.	2024-09-09 downloaded from the CCDC.
;
_audit_creation_date             2024-07-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H80 Cu6 Dy4 N16 O44, 4(C2 H3 N)'
_chemical_formula_sum            'C76 H92 Cu6 Dy4 N20 O44'
_chemical_formula_weight         3020.93
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C72 H86 Cu6 Dy4 N18 O44'
_chemical_oxdiff_usercomment     OVEN@120for2hrs_RTdatacol
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'
Cu Cu -1.9646 0.5888 '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           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   17.45300(10)
_cell_length_b                   17.45300(10)
_cell_length_c                   16.65680(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5073.78(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    27408
_cell_measurement_temperature    149.94(10)
_cell_measurement_theta_max      78.0810
_cell_measurement_theta_min      3.5720
_shelx_estimated_absorpt_T_max   0.247
_shelx_estimated_absorpt_T_min   0.143
_exptl_absorpt_coefficient_mu    17.634
_exptl_absorpt_correction_T_max  0.650
_exptl_absorpt_correction_T_min  0.363
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2956
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -8 -8 0.0571
0 8 8 0.0496
-8 -8 0 0.0648
-8 0 8 0.0575
10 4 -4 0.0828
5 9 5 0.0581
-9 4 -6 0.0694
8 -4 6 0.0635
-7 -4 7 0.0657
1 6 -9 0.1198
11 0 -1 0.0907
-1 11 -4 0.0897
-9 7 1 0.0659
-3 9 5 0.0610
8 7 -3 0.0852
5 10 0 0.0826
-2 10 4 0.0633
-6 7 6 0.0607
1 -10 -4 0.0739
7 2 8 0.0611
0 0 11 0.0608
8 -8 0 0.0852
1 -8 -7 0.0587
-9 -2 6 0.0587
-4 -5 -9 0.0651
6 9 -4 0.0890
-4 11 2 0.0709
6 7 6 0.0573
3 6 9 0.0519

_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0000 -8.0000 -8.0000 -0.9956 -0.0750 0.2235
0.0000 8.0000 8.0000 0.9956 0.0750 -0.2235
-8.0000 -8.0000 -0.0000 -0.6679 -0.0112 -0.7428
-8.0000 -0.0000 8.0000 0.3277 0.0638 -0.9663
10.0000 4.0000 -4.0000 0.1951 0.0729 0.9985
5.0000 9.0000 5.0000 0.9687 0.1020 0.3037
-9.0000 4.0000 -6.0000 -0.1494 -0.9839 -0.2714
8.0000 -4.0000 6.0000 0.1369 0.9343 0.1995
-7.0000 -4.0000 7.0000 0.0028 0.2484 -0.9290
1.0000 6.0000 -9.0000 -0.0428 -0.7572 0.6365
11.0000 0.0000 -1.0000 0.0841 0.4876 0.8405
-1.0000 11.0000 -4.0000 0.5544 -0.8094 0.3529
-9.0000 7.0000 1.0000 0.4378 -0.7256 -0.5505
-3.0000 9.0000 5.0000 0.8686 -0.2944 -0.2721
8.0000 7.0000 -3.0000 0.4365 -0.1132 0.8683
5.0000 10.0000 0.0000 0.7723 -0.2338 0.5686
-2.0000 10.0000 4.0000 0.8986 -0.3506 -0.1305
-6.0000 7.0000 6.0000 0.7426 -0.2893 -0.5786
1.0000 -10.0000 -4.0000 -0.9112 0.3010 0.0585
7.0000 2.0000 8.0000 0.6572 0.7109 0.1551
-0.0000 0.0000 11.0000 0.5881 0.6328 -0.5369
8.0000 -8.0000 -0.0000 -0.4678 0.7817 0.4088
1.0000 -8.0000 -7.0000 -0.9296 0.0321 0.2467
-9.0000 -2.0000 6.0000 0.0663 -0.0046 -0.9824
-4.0000 -5.0000 -9.0000 -0.8861 -0.4752 0.0470
6.0000 9.0000 -4.0000 0.5000 -0.3662 0.8149
-4.0000 11.0000 2.0000 0.8377 -0.6129 -0.1559
6.0000 7.0000 6.0000 0.8927 0.3055 0.2851
3.0000 6.0000 9.0000 0.9446 0.3775 -0.0981

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36897
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.581
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.94(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00  17.00   0.50    0.50    --  -49.93  47.00 -29.00   78
  2  ω   -114.00 -43.00   0.50    0.50    --  -49.93 -47.00-178.00  142
  3  ω     43.00  68.00   0.50    0.50    --   49.93  47.00 -29.00   50
  4  ω    -19.00  30.00   0.50    0.50    --   49.93 -47.00-178.00   98
  5  ω   -176.00 -99.00   0.50    1.50    -- -106.00 -47.00-178.00  154
  6  ω    116.00 141.00   0.50    1.50    --  111.50  47.00 -29.00   50
  7  ω   -116.00 -75.00   0.50    0.50    --  -49.93-126.00-120.00   82
  8  ω   -119.00 -73.00   0.50    0.50    --  -49.93-126.00   0.00   92
  9  ω     87.00 112.00   0.50    0.50    --   49.93  47.00 -29.00   50
 10  ω    -22.00  25.00   0.50    0.50    --   49.93 -19.00  30.00   94
 11  ω    -64.00 -34.00   0.50    1.50    -- -106.00  57.00-180.00   60
 12  ω    -63.00 -36.00   0.50    1.50    -- -106.00  57.00 -30.00   54
 13  ω    -63.00 -37.00   0.50    1.50    -- -106.00  57.00-120.00   52
 14  ω    -65.00 -40.00   0.50    1.50    -- -106.00  57.00   0.00   50
 15  ω    -62.00 -36.00   0.50    1.50    -- -106.00  57.00  90.00   52
 16  ω    -65.00 -40.00   0.50    1.50    -- -106.00  57.00 -60.00   50
 17  ω    -64.00 -39.00   0.50    1.50    -- -106.00  57.00  60.00   50
 18  ω   -146.00-103.00   0.50    1.50    -- -106.00   0.00-120.00   86
 19  ω    -65.00 -40.00   0.50    1.50    -- -106.00  57.00 120.00   50
 20  ω    -65.00 -40.00   0.50    1.50    -- -106.00  57.00 150.00   50
 21  ω     46.00 101.00   0.50    1.50    --  111.50 -77.00  30.00  110
 22  ω     59.00 102.00   0.50    1.50    --  111.50-126.00  30.00   86
 23  ω     41.00  95.00   0.50    1.50    --  111.50 -77.00 150.00  108
 24  ω     50.00  88.00   0.50    1.50    --  111.50 -77.00-180.00   76
 25  ω    115.00 141.00   0.50    1.50    --  111.50  57.00  60.00   52
 26  ω     43.00  98.00   0.50    1.50    --  111.50 -77.00 -30.00  110
 27  ω     64.00  96.00   0.50    1.50    --  111.50   0.00 150.00   64
 28  ω    147.00 178.00   0.50    1.50    --  111.50  57.00  60.00   62
 29  ω     54.00  87.00   0.50    1.50    --  111.50 -77.00-150.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0125061000
_diffrn_orient_matrix_UB_12      0.0709785000
_diffrn_orient_matrix_UB_13      0.0534677000
_diffrn_orient_matrix_UB_21      0.0495614000
_diffrn_orient_matrix_UB_22      -0.0481568000
_diffrn_orient_matrix_UB_23      0.0575302000
_diffrn_orient_matrix_UB_31      0.0719756000
_diffrn_orient_matrix_UB_32      0.0208718000
_diffrn_orient_matrix_UB_33      -0.0488093000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4465
_reflns_number_total             4526
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 
;
 Flack x determined using 1915 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0006(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4526
_refine_ls_number_restraints     82
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0239
_refine_ls_restrained_S_all      1.100
_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)+(0.0405P)²+4.8529P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0658
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N5-C18
 1.14 with sigma of 0.02
 C18-N5
 1.137 with sigma of 0.01
 C18-C19
 1.456 with sigma of 0.01
 C19-N5
 2.593 with sigma of 0.02
 N6-C20
 1.14 with sigma of 0.02
 C20-N6
 1.137 with sigma of 0.01
 C20-C21
 1.456 with sigma of 0.01
 C21-N6
 2.593 with sigma of 0.02
 N5-C19
 2.59 with sigma of 0.04
 N6-C21
 2.59 with sigma of 0.04
3. Rigid bond restraints
 O8, N3, O7, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O7, N3, O6, O8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
N5 \\sim C18 \\sim C19: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N6 \\sim C20 \\sim C21: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O8 \\sim O6 \\sim O7 \\sim N3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N5, C18, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N6, C20, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: N5(0.75) C18(0.75) C19(0.75) H19a(0.75) H19b(0.75) H19c(0.75)
 N6(0.25) C20(0.25) C21(0.25) H21a(0.25) H21b(0.25) H21c(0.25)
7.a Ternary CH refined with riding coordinates:
 C12(H12)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C3(H3a,H3b), C2(H2a,H2b), C10(H10a,H10b), C11(H11a,H11b)
7.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C17(H17), C7(H7), C8(H8), C9(H9), C16(H16), C14(H14), C15(H15)
7.d Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C21(H21a,H21b,H21c)
7.e Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.31797(2) 0.46040(2) 0.65765(2) 0.03248(10) Uani 1 1 d . . . . .
Cu1 Cu 0.500000 0.500000 0.65284(7) 0.0314(2) Uani 1 2 d S T P . .
Cu2 Cu 0.64585(5) 0.25379(5) 0.49168(5) 0.03650(19) Uani 1 1 d . . . . .
O1 O 0.4364(2) 0.4135(2) 0.6658(3) 0.0377(9) Uani 1 1 d . . . . .
O3 O 0.5450(2) 0.2974(2) 0.4755(2) 0.0376(9) Uani 1 1 d . . . . .
O2 O 0.5932(2) 0.4446(2) 0.6347(2) 0.0325(8) Uani 1 1 d . . . . .
O11 O 0.3100(3) 0.4437(3) 0.9045(3) 0.0546(12) Uani 1 1 d . . . . .
O9 O 0.3013(3) 0.3920(2) 0.7860(2) 0.0433(10) Uani 1 1 d . . . . .
O4 O 0.6615(2) 0.2878(3) 0.3824(2) 0.0478(11) Uani 1 1 d . . . . .
N1 N 0.6096(3) 0.2039(3) 0.5929(3) 0.0357(10) Uani 1 1 d . . . . .
O10 O 0.3248(4) 0.5116(3) 0.7956(3) 0.0575(13) Uani 1 1 d . . . . .
N4 N 0.3120(3) 0.4483(3) 0.8311(3) 0.0414(11) Uani 1 1 d . . . . .
N2 N 0.7573(3) 0.2381(3) 0.5129(3) 0.0397(11) Uani 1 1 d . . . . .
O7 O 0.2393(3) 0.5799(3) 0.6607(4) 0.0702(10) Uani 1 1 d . U . . .
C5 C 0.5513(3) 0.2323(3) 0.6380(3) 0.0326(12) Uani 1 1 d . . . . .
O5 O 0.6650(4) 0.1297(4) 0.4256(4) 0.0805(18) Uani 1 1 d . . . . .
H5 H 0.626633 0.106100 0.407811 0.121 Uiso 1 1 calc R U . . .
O6 O 0.1805(3) 0.4753(3) 0.6859(4) 0.0708(10) Uani 1 1 d . U . . .
C13 C 0.8041(4) 0.2141(4) 0.4541(4) 0.0490(16) Uani 1 1 d . . . . .
C1 C 0.4661(4) 0.3406(3) 0.6826(3) 0.0372(12) Uani 1 1 d . . . . .
H1A H 0.424036 0.302641 0.680809 0.045 Uiso 1 1 calc R U . . .
H1B H 0.487431 0.340519 0.737701 0.045 Uiso 1 1 calc R U . . .
C3 C 0.4972(3) 0.3250(3) 0.5370(3) 0.0325(11) Uani 1 1 d . . . . .
H3A H 0.447572 0.297729 0.533843 0.039 Uiso 1 1 calc R U . . .
H3B H 0.487105 0.379963 0.527008 0.039 Uiso 1 1 calc R U . . .
C6 C 0.5156(4) 0.1859(3) 0.6936(4) 0.0390(12) Uani 1 1 d . . . . .
H6 H 0.474539 0.205566 0.724819 0.047 Uiso 1 1 calc R U . . .
C4 C 0.5292(3) 0.3161(3) 0.6233(3) 0.0323(11) Uani 1 1 d . . . . .
C17 C 0.7877(4) 0.2532(4) 0.5852(4) 0.0412(13) Uani 1 1 d . . . . .
H17 H 0.754638 0.270567 0.626693 0.049 Uiso 1 1 calc R U . . .
C7 C 0.5392(4) 0.1110(3) 0.7044(4) 0.0449(14) Uani 1 1 d . . . . .
H7 H 0.514059 0.078903 0.742191 0.054 Uiso 1 1 calc R U . . .
C8 C 0.5991(4) 0.0835(3) 0.6599(4) 0.0449(13) Uani 1 1 d . . . . .
H8 H 0.616789 0.032447 0.666911 0.054 Uiso 1 1 calc R U . . .
C2 C 0.6026(3) 0.3647(3) 0.6375(3) 0.0326(11) Uani 1 1 d . . . . .
H2A H 0.623889 0.350950 0.690704 0.039 Uiso 1 1 calc R U . . .
H2B H 0.641102 0.349986 0.596631 0.039 Uiso 1 1 calc R U . . .
N3 N 0.1805(4) 0.5477(4) 0.6864(5) 0.0722(9) Uani 1 1 d . U . . .
C12 C 0.7713(4) 0.2018(5) 0.3719(4) 0.065(2) Uani 1 1 d . . . . .
H12 H 0.815882 0.193135 0.335213 0.077 Uiso 1 1 calc R U . . .
C9 C 0.6329(4) 0.1312(3) 0.6052(4) 0.0429(14) Uani 1 1 d . . . . .
H9 H 0.674564 0.112194 0.574398 0.051 Uiso 1 1 calc R U . . .
C16 C 0.8636(4) 0.2449(5) 0.6018(5) 0.0579(18) Uani 1 1 d . . . . .
H16 H 0.883039 0.255896 0.653822 0.070 Uiso 1 1 calc R U . . .
C14 C 0.8811(4) 0.2038(5) 0.4673(4) 0.062(2) Uani 1 1 d . . . . .
H14 H 0.913062 0.185394 0.425449 0.074 Uiso 1 1 calc R U . . .
C15 C 0.9117(4) 0.2203(6) 0.5413(5) 0.072(2) Uani 1 1 d . . . . .
H15 H 0.965092 0.214730 0.550732 0.087 Uiso 1 1 calc R U . . .
C10 C 0.7307(4) 0.2729(6) 0.3414(5) 0.074(3) Uani 1 1 d . . . . .
H10A H 0.765182 0.317590 0.347454 0.089 Uiso 1 1 calc R U . . .
H10B H 0.719628 0.266622 0.283469 0.089 Uiso 1 1 calc R U . . .
O8 O 0.1264(4) 0.5852(4) 0.7118(5) 0.0869(13) Uani 1 1 d . U . . .
C11 C 0.7224(6) 0.1322(7) 0.3659(6) 0.093(4) Uani 1 1 d . . . . .
H11A H 0.697899 0.130993 0.312341 0.111 Uiso 1 1 calc R U . . .
H11B H 0.755177 0.086160 0.370804 0.111 Uiso 1 1 calc R U . . .
N5 N 0.5905(11) -0.0001(8) 0.4313(10) 0.149(7) Uani 0.75 1 d D U P . .
C18 C 0.5790(9) -0.0536(7) 0.4663(11) 0.105(5) Uani 0.75 1 d D U P . .
C19 C 0.5628(13) -0.1233(9) 0.5060(12) 0.148(9) Uani 0.75 1 d D U P . .
H19A H 0.510200 -0.139182 0.493643 0.222 Uiso 0.75 1 calc R U P . .
H19B H 0.568188 -0.116150 0.564047 0.222 Uiso 0.75 1 calc R U P . .
H19C H 0.598608 -0.162854 0.487756 0.222 Uiso 0.75 1 calc R U P . .
N6 N 0.489(2) 0.5476(11) 0.878(2) 0.060(8) Uani 0.25 1 d D U P A -1
C20 C 0.502(3) 0.4841(12) 0.878(3) 0.063(10) Uani 0.25 1 d D U P A -1
C21 C 0.528(2) 0.4064(12) 0.868(2) 0.061(8) Uani 0.25 1 d D U P A -1
H21A H 0.488078 0.376885 0.839371 0.092 Uiso 0.25 1 calc R U P A -1
H21B H 0.537122 0.383251 0.920275 0.092 Uiso 0.25 1 calc R U P A -1
H21C H 0.574928 0.406127 0.836091 0.092 Uiso 0.25 1 calc R U P A -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 Cu1 3.2523(3) . ?
Dy1 Cu2 3.2987(9) 3_566 ?
Dy1 O1 2.227(4) . ?
Dy1 O3 2.249(4) 3_566 ?
Dy1 O2 2.302(4) 2_665 ?
Dy1 O9 2.465(4) . ?
Dy1 O4 2.291(4) 3_566 ?
Dy1 O10 2.469(4) . ?
Dy1 N4 2.898(5) . ?
Dy1 O7 2.496(5) . ?
Dy1 O6 2.459(5) . ?
Dy1 N3 2.883(6) . ?
Cu1 O1 1.887(4) . ?
Cu1 O1 1.887(4) 2_665 ?
Cu1 O2 1.916(4) 2_665 ?
Cu1 O2 1.916(4) . ?
Cu2 O3 1.937(4) . ?
Cu2 O4 1.933(4) . ?
Cu2 N1 1.999(5) . ?
Cu2 N2 1.997(5) . ?
Cu2 O5 2.452(6) . ?
O1 C1 1.403(7) . ?
O3 C3 1.405(6) . ?
O2 C2 1.405(6) . ?
O11 N4 1.227(7) . ?
O9 N4 1.251(6) . ?
O4 C10 1.412(8) . ?
N1 C5 1.360(7) . ?
N1 C9 1.348(8) . ?
O10 N4 1.272(7) . ?
N2 C13 1.342(8) . ?
N2 C17 1.341(8) . ?
O7 N3 1.246(8) . ?
C5 C6 1.379(8) . ?
C5 C4 1.532(7) . ?
O5 H5 0.8400 . ?
O5 C11 1.412(13) . ?
O6 N3 1.264(9) . ?
C13 C12 1.500(9) . ?
C13 C14 1.373(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C4 1.540(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.551(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.383(8) . ?
C4 C2 1.554(8) . ?
C17 H17 0.9500 . ?
C17 C16 1.362(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.367(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.369(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
N3 O8 1.223(8) . ?
C12 H12 1.0000 . ?
C12 C10 1.518(11) . ?
C12 C11 1.487(15) . ?
C9 H9 0.9500 . ?
C16 H16 0.9500 . ?
C16 C15 1.380(12) . ?
C14 H14 0.9500 . ?
C14 C15 1.374(12) . ?
C15 H15 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N5 C18 1.119(11) . ?
C18 C19 1.413(11) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
N6 C20 1.130(12) . ?
C20 C21 1.439(13) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?

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
Cu1 Dy1 Cu2 115.63(2) . 3_566 ?
O1 Dy1 Cu1 34.22(9) . . ?
O1 Dy1 Cu2 98.87(11) . 3_566 ?
O1 Dy1 O3 101.12(16) . 3_566 ?
O1 Dy1 O2 69.51(13) . 2_665 ?
O1 Dy1 O9 83.07(15) . . ?
O1 Dy1 O4 83.65(16) . 3_566 ?
O1 Dy1 O10 91.82(19) . . ?
O1 Dy1 N4 86.90(15) . . ?
O1 Dy1 O7 144.68(16) . . ?
O1 Dy1 O6 158.87(16) . . ?
O1 Dy1 N3 163.1(2) . . ?
O3 Dy1 Cu1 98.09(10) 3_566 . ?
O3 Dy1 Cu2 34.77(11) 3_566 3_566 ?
O3 Dy1 O2 88.51(14) 3_566 2_665 ?
O3 Dy1 O9 144.68(14) 3_566 . ?
O3 Dy1 O4 68.72(15) 3_566 3_566 ?
O3 Dy1 O10 160.20(16) 3_566 . ?
O3 Dy1 N4 166.98(15) 3_566 . ?
O3 Dy1 O7 88.1(2) 3_566 . ?
O3 Dy1 O6 92.13(19) 3_566 . ?
O3 Dy1 N3 93.0(2) 3_566 . ?
O2 Dy1 Cu1 35.41(9) 2_665 . ?
O2 Dy1 Cu2 120.56(10) 2_665 3_566 ?
O2 Dy1 O9 124.91(14) 2_665 . ?
O2 Dy1 O10 82.02(15) 2_665 . ?
O2 Dy1 N4 103.99(14) 2_665 . ?
O2 Dy1 O7 76.82(15) 2_665 . ?
O2 Dy1 O6 127.79(16) 2_665 . ?
O2 Dy1 N3 101.97(16) 2_665 . ?
O9 Dy1 Cu1 103.88(11) . . ?
O9 Dy1 Cu2 109.97(9) . 3_566 ?
O9 Dy1 O10 51.24(14) . . ?
O9 Dy1 N4 25.37(13) . . ?
O9 Dy1 O7 108.76(18) . . ?
O9 Dy1 N3 90.76(18) . . ?
O4 Dy1 Cu1 114.48(13) 3_566 . ?
O4 Dy1 Cu2 34.93(11) 3_566 3_566 ?
O4 Dy1 O2 140.82(15) 3_566 2_665 ?
O4 Dy1 O9 77.06(14) 3_566 . ?
O4 Dy1 O10 128.22(14) 3_566 . ?
O4 Dy1 N4 102.41(14) 3_566 . ?
O4 Dy1 O7 130.9(2) 3_566 . ?
O4 Dy1 O6 86.0(2) 3_566 . ?
O4 Dy1 N3 110.4(2) 3_566 . ?
O10 Dy1 Cu1 84.19(15) . . ?
O10 Dy1 Cu2 157.21(12) . 3_566 ?
O10 Dy1 N4 25.87(14) . . ?
O10 Dy1 O7 72.9(2) . . ?
O10 Dy1 N3 72.2(2) . . ?
N4 Dy1 Cu1 94.29(11) . . ?
N4 Dy1 Cu2 134.32(10) . 3_566 ?
O7 Dy1 Cu1 111.11(13) . . ?
O7 Dy1 Cu2 107.34(17) . 3_566 ?
O7 Dy1 N4 91.20(18) . . ?
O7 Dy1 N3 25.52(18) . . ?
O6 Dy1 Cu1 159.31(15) . . ?
O6 Dy1 Cu2 82.67(16) . 3_566 ?
O6 Dy1 O9 76.69(18) . . ?
O6 Dy1 O10 80.3(2) . . ?
O6 Dy1 N4 77.42(18) . . ?
O6 Dy1 O7 51.05(17) . . ?
O6 Dy1 N3 25.85(19) . . ?
N3 Dy1 Cu1 134.82(15) . . ?
N3 Dy1 Cu2 98.04(18) . 3_566 ?
N3 Dy1 N4 80.97(19) . . ?
Dy1 Cu1 Dy1 177.17(4) 2_665 . ?
O1 Cu1 Dy1 137.93(12) 2_665 . ?
O1 Cu1 Dy1 137.93(12) . 2_665 ?
O1 Cu1 Dy1 41.59(12) 2_665 2_665 ?
O1 Cu1 Dy1 41.59(12) . . ?
O1 Cu1 O1 166.9(3) . 2_665 ?
O1 Cu1 O2 96.53(16) 2_665 2_665 ?
O1 Cu1 O2 85.54(16) 2_665 . ?
O1 Cu1 O2 96.53(16) . . ?
O1 Cu1 O2 85.54(16) . 2_665 ?
O2 Cu1 Dy1 44.11(10) 2_665 . ?
O2 Cu1 Dy1 44.11(10) . 2_665 ?
O2 Cu1 Dy1 136.53(11) 2_665 2_665 ?
O2 Cu1 Dy1 136.53(11) . . ?
O2 Cu1 O2 161.9(2) 2_665 . ?
O3 Cu2 Dy1 41.47(11) . 4_656 ?
O3 Cu2 N1 90.04(18) . . ?
O3 Cu2 N2 164.7(2) . . ?
O3 Cu2 O5 114.1(2) . . ?
O4 Cu2 Dy1 42.72(12) . 4_656 ?
O4 Cu2 O3 82.92(16) . . ?
O4 Cu2 N1 166.3(2) . . ?
O4 Cu2 N2 94.08(18) . . ?
O4 Cu2 O5 80.2(2) . . ?
N1 Cu2 Dy1 127.28(14) . 4_656 ?
N1 Cu2 O5 92.1(2) . . ?
N2 Cu2 Dy1 136.72(14) . 4_656 ?
N2 Cu2 N1 95.7(2) . . ?
N2 Cu2 O5 80.0(2) . . ?
O5 Cu2 Dy1 92.17(15) . 4_656 ?
Cu1 O1 Dy1 104.20(16) . . ?
C1 O1 Dy1 133.6(3) . . ?
C1 O1 Cu1 122.0(4) . . ?
Cu2 O3 Dy1 103.76(17) . 4_656 ?
C3 O3 Dy1 129.7(3) . 4_656 ?
C3 O3 Cu2 124.9(3) . . ?
Cu1 O2 Dy1 100.47(14) . 2_665 ?
C2 O2 Dy1 129.1(3) . 2_665 ?
C2 O2 Cu1 126.5(3) . . ?
N4 O9 Dy1 97.0(3) . . ?
Cu2 O4 Dy1 102.35(18) . 4_656 ?
C10 O4 Dy1 134.0(4) . 4_656 ?
C10 O4 Cu2 121.3(4) . . ?
C5 N1 Cu2 123.0(4) . . ?
C9 N1 Cu2 116.3(4) . . ?
C9 N1 C5 119.0(5) . . ?
N4 O10 Dy1 96.2(3) . . ?
O11 N4 Dy1 179.4(5) . . ?
O11 N4 O9 122.9(5) . . ?
O11 N4 O10 121.6(5) . . ?
O9 N4 Dy1 57.6(3) . . ?
O9 N4 O10 115.5(5) . . ?
O10 N4 Dy1 57.9(3) . . ?
C13 N2 Cu2 120.4(4) . . ?
C17 N2 Cu2 121.1(4) . . ?
C17 N2 C13 118.5(5) . . ?
N3 O7 Dy1 94.9(4) . . ?
N1 C5 C6 119.7(5) . . ?
N1 C5 C4 116.6(5) . . ?
C6 C5 C4 123.7(5) . . ?
Cu2 O5 H5 118.9 . . ?
C11 O5 Cu2 112.6(6) . . ?
C11 O5 H5 109.5 . . ?
N3 O6 Dy1 96.1(4) . . ?
N2 C13 C12 118.7(6) . . ?
N2 C13 C14 121.2(6) . . ?
C14 C13 C12 120.1(6) . . ?
O1 C1 H1A 109.0 . . ?
O1 C1 H1B 109.0 . . ?
O1 C1 C4 112.9(4) . . ?
H1A C1 H1B 107.8 . . ?
C4 C1 H1A 109.0 . . ?
C4 C1 H1B 109.0 . . ?
O3 C3 H3A 108.4 . . ?
O3 C3 H3B 108.4 . . ?
O3 C3 C4 115.3(4) . . ?
H3A C3 H3B 107.5 . . ?
C4 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.6(6) . . ?
C7 C6 H6 119.7 . . ?
C5 C4 C1 110.0(4) . . ?
C5 C4 C3 109.5(4) . . ?
C5 C4 C2 106.8(4) . . ?
C1 C4 C3 108.0(5) . . ?
C1 C4 C2 109.9(4) . . ?
C3 C4 C2 112.6(4) . . ?
N2 C17 H17 118.5 . . ?
N2 C17 C16 123.1(6) . . ?
C16 C17 H17 118.5 . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.3(6) . . ?
C8 C7 H7 120.4 . . ?
C7 C8 H8 120.8 . . ?
C7 C8 C9 118.5(6) . . ?
C9 C8 H8 120.8 . . ?
O2 C2 C4 116.1(4) . . ?
O2 C2 H2A 108.3 . . ?
O2 C2 H2B 108.3 . . ?
C4 C2 H2A 108.3 . . ?
C4 C2 H2B 108.3 . . ?
H2A C2 H2B 107.4 . . ?
O7 N3 Dy1 59.6(3) . . ?
O7 N3 O6 116.6(6) . . ?
O6 N3 Dy1 58.0(3) . . ?
O8 N3 Dy1 169.1(7) . . ?
O8 N3 O7 121.0(7) . . ?
O8 N3 O6 122.4(7) . . ?
C13 C12 H12 106.4 . . ?
C13 C12 C10 111.5(7) . . ?
C10 C12 H12 106.4 . . ?
C11 C12 C13 113.4(8) . . ?
C11 C12 H12 106.4 . . ?
C11 C12 C10 112.2(7) . . ?
N1 C9 C8 123.0(6) . . ?
N1 C9 H9 118.5 . . ?
C8 C9 H9 118.5 . . ?
C17 C16 H16 120.8 . . ?
C17 C16 C15 118.5(7) . . ?
C15 C16 H16 120.8 . . ?
C13 C14 H14 120.1 . . ?
C13 C14 C15 119.8(7) . . ?
C15 C14 H14 120.1 . . ?
C16 C15 H15 120.5 . . ?
C14 C15 C16 118.9(7) . . ?
C14 C15 H15 120.5 . . ?
O4 C10 C12 112.9(7) . . ?
O4 C10 H10A 109.0 . . ?
O4 C10 H10B 109.0 . . ?
C12 C10 H10A 109.0 . . ?
C12 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
O5 C11 C12 112.7(7) . . ?
O5 C11 H11A 109.0 . . ?
O5 C11 H11B 109.0 . . ?
C12 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N5 C18 C19 176(2) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N6 C20 C21 170(5) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 Cu1 O1 Dy1 175.82(6) 2_665 . . . ?
Dy1 Cu1 O1 C1 -175.7(5) . . . . ?
Dy1 Cu1 O1 C1 0.1(5) 2_665 . . . ?
Dy1 O1 C1 C4 133.5(4) . . . . ?
Dy1 O3 C3 C4 -165.2(3) 4_656 . . . ?
Dy1 O2 C2 C4 176.8(3) 2_665 . . . ?
Dy1 O9 N4 O11 -179.6(5) . . . . ?
Dy1 O9 N4 O10 0.9(6) . . . . ?
Dy1 O4 C10 C12 -132.7(6) 4_656 . . . ?
Dy1 O10 N4 O11 179.6(5) . . . . ?
Dy1 O10 N4 O9 -0.9(6) . . . . ?
Dy1 O7 N3 O6 -11.6(9) . . . . ?
Dy1 O7 N3 O8 167.4(8) . . . . ?
Dy1 O6 N3 O7 11.8(9) . . . . ?
Dy1 O6 N3 O8 -167.2(8) . . . . ?
Cu1 O1 C1 C4 -52.3(6) . . . . ?
Cu1 O2 C2 C4 23.5(6) . . . . ?
Cu2 O3 C3 C4 -2.1(7) . . . . ?
Cu2 O4 C10 C12 26.9(10) . . . . ?
Cu2 N1 C5 C6 162.5(4) . . . . ?
Cu2 N1 C5 C4 -17.7(6) . . . . ?
Cu2 N1 C9 C8 -163.7(5) . . . . ?
Cu2 N2 C13 C12 1.8(10) . . . . ?
Cu2 N2 C13 C14 179.3(6) . . . . ?
Cu2 N2 C17 C16 -178.6(5) . . . . ?
Cu2 O5 C11 C12 15.3(10) . . . . ?
O1 Cu1 O1 Dy1 95.27(15) 2_665 . . . ?
O1 Cu1 O1 C1 -80.5(4) 2_665 . . . ?
O1 C1 C4 C5 -172.3(5) . . . . ?
O1 C1 C4 C3 -52.8(6) . . . . ?
O1 C1 C4 C2 70.4(6) . . . . ?
O3 C3 C4 C5 -53.9(6) . . . . ?
O3 C3 C4 C1 -173.6(4) . . . . ?
O3 C3 C4 C2 64.8(6) . . . . ?
O2 Cu1 O1 Dy1 -166.30(18) . . . . ?
O2 Cu1 O1 Dy1 -4.39(18) 2_665 . . . ?
O2 Cu1 O1 C1 18.0(4) . . . . ?
O2 Cu1 O1 C1 179.9(4) 2_665 . . . ?
N1 C5 C6 C7 0.5(9) . . . . ?
N1 C5 C4 C1 -176.4(5) . . . . ?
N1 C5 C4 C3 65.0(6) . . . . ?
N1 C5 C4 C2 -57.1(6) . . . . ?
N2 C13 C12 C10 54.8(10) . . . . ?
N2 C13 C12 C11 -72.9(9) . . . . ?
N2 C13 C14 C15 -1.9(14) . . . . ?
N2 C17 C16 C15 0.4(12) . . . . ?
C5 N1 C9 C8 1.6(9) . . . . ?
C5 C6 C7 C8 0.9(9) . . . . ?
C5 C4 C2 O2 -174.0(4) . . . . ?
C13 N2 C17 C16 -0.4(10) . . . . ?
C13 C12 C10 O4 -70.6(10) . . . . ?
C13 C12 C11 O5 52.0(10) . . . . ?
C13 C14 C15 C16 1.8(15) . . . . ?
C1 C4 C2 O2 -54.7(6) . . . . ?
C3 C4 C2 O2 65.8(6) . . . . ?
C6 C5 C4 C1 3.3(7) . . . . ?
C6 C5 C4 C3 -115.2(6) . . . . ?
C6 C5 C4 C2 122.6(6) . . . . ?
C6 C7 C8 C9 -1.0(9) . . . . ?
C4 C5 C6 C7 -179.2(5) . . . . ?
C17 N2 C13 C12 -176.3(7) . . . . ?
C17 N2 C13 C14 1.2(11) . . . . ?
C17 C16 C15 C14 -1.1(14) . . . . ?
C7 C8 C9 N1 -0.2(9) . . . . ?
C12 C13 C14 C15 175.6(9) . . . . ?
C9 N1 C5 C6 -1.8(8) . . . . ?
C9 N1 C5 C4 178.0(5) . . . . ?
C14 C13 C12 C10 -122.7(8) . . . . ?
C14 C13 C12 C11 109.6(9) . . . . ?
C10 C12 C11 O5 -75.3(10) . . . . ?
C11 C12 C10 O4 57.8(9) . . . . ?


_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.202
_oxdiff_exptl_absorpt_empirical_full_min 0.812
####################################################################### 
# 
# 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_tb4cu6_new
_audit_block_doi                 10.5517/ccdc.csd.cc2kky7b
_database_code_depnum_ccdc_archive 'CCDC 2370732'
loop_
_audit_author_name
_audit_author_address
'Antonis Anastassiades'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-07-15 deposited with the CCDC.	2024-09-09 downloaded from the CCDC.
;
_audit_creation_date             2024-07-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H80 Cu6 N16 O44 Tb4, 3(C2 H3 N)'
_chemical_formula_sum            'C74 H89 Cu6 N19 O44 Tb4'
_chemical_formula_weight         2965.56
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C72 H86 Cu6 Tb4 N18 O44'
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'
Cu Cu -1.9646 0.5888 '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'
Tb Tb -9.1472 9.1891 '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           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   17.58050(10)
_cell_length_b                   17.58050(10)
_cell_length_c                   16.51130(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5103.21(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    30284
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      79.1560
_cell_measurement_theta_min      3.5260
_shelx_estimated_absorpt_T_max   0.191
_shelx_estimated_absorpt_T_min   0.178
_exptl_absorpt_coefficient_mu    15.480
_exptl_absorpt_correction_T_max  0.618
_exptl_absorpt_correction_T_min  0.341
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2904
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 -8 -5 0.0780
7 -3 8 0.0860
-8 3 -8 0.0782
-10 0 5 0.0954
-7 -1 9 0.0948
10 -1 -6 0.0671
-10 1 5 0.0937
3 -3 10 0.0966
-9 5 5 0.0868
-7 2 8 0.0927
-1 11 0 0.0861
-2 9 6 0.0836
-3 3 10 0.0961
2 7 -8 0.0689
3 -5 -9 0.1082
-2 -7 8 0.0855
5 10 0 0.0774
5 9 -5 0.0755
3 8 8 0.0849
8 8 0 0.0717
4 5 -9 0.0717
7 8 -4 0.0719
6 7 7 0.0844
4 5 9 0.0925
9 5 -5 0.0665
10 4 4 0.0823
6 2 9 0.0901
9 2 -7 0.0609
9 -5 -5 0.0685
4 -6 8 0.0867
9 -7 1 0.0737
-9 -6 4 0.0908
-4 -9 -5 0.0805
-2 9 -7 0.0724
-6 9 3 0.0770
-6 10 -2 0.0742
8 -6 5 0.0784
10 -5 0 0.0781

_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.0460 -8.1976 -4.8249 0.9850 -0.0245 0.1710
7.4701 -2.7180 7.6891 -0.4206 -0.6825 -0.5977
-7.5353 2.7116 -7.6347 0.4229 0.6864 0.5915
-10.0395 -0.1785 5.0813 0.3964 0.6580 -0.6403
-6.6241 -1.4279 8.6234 0.2038 0.3455 -0.9160
9.7457 -0.6003 -5.5379 -0.3175 -0.6794 0.6615
-9.9350 0.7290 5.2177 0.3276 0.7004 -0.6341
3.2927 -3.3867 9.7610 -0.2155 -0.4413 -0.8711
-9.0108 4.9571 4.6378 0.0177 0.8721 -0.4890
-6.8184 1.8008 8.4246 0.0074 0.5371 -0.8435
-0.6822 11.3979 -0.0329 -0.7119 0.6742 0.1966
-2.0351 9.0840 6.2019 -0.6595 0.6194 -0.4259
-2.5889 2.9003 10.0775 -0.3304 0.3044 -0.8934
1.5268 7.2037 -8.1970 -0.3290 0.3184 0.8890
2.5199 -5.3366 -9.1737 0.4693 -0.4367 0.7675
-1.5995 -6.8880 8.4208 0.3059 -0.2968 -0.9046
5.0132 10.2530 -0.0656 -0.9327 0.2234 0.2832
4.9307 9.0246 -4.6548 -0.7226 0.1757 0.6686
2.8228 7.5358 7.5977 -0.8491 0.1989 -0.4893
7.8231 8.3027 -0.1257 -0.9494 -0.0752 0.3048
4.3687 4.5730 -8.9256 -0.2845 -0.0177 0.9585
7.3479 7.7724 -3.7349 -0.7914 -0.0607 0.6082
6.1685 6.5944 6.5470 -0.9330 -0.0775 -0.3513
4.3066 4.6350 8.9172 -0.7720 -0.0660 -0.6322
9.1533 4.6407 -4.6788 -0.6542 -0.3532 0.6688
9.9929 3.8822 3.6498 -0.8753 -0.4782 -0.0720
6.4216 1.6324 8.7230 -0.6798 -0.3748 -0.6304
8.6265 1.6180 -6.8452 -0.3691 -0.4770 0.7976
9.0448 -4.9048 -4.6284 -0.0231 -0.8716 0.4897
3.8290 -6.2736 8.2068 -0.0115 -0.6320 -0.7749
8.8918 -7.0838 0.9288 -0.0237 -0.9986 -0.0479
-8.5484 -6.2322 4.0119 0.7453 0.2264 -0.6271
-4.0729 -9.4572 -4.6184 0.9592 -0.2289 0.1660
-2.2890 8.6562 -6.6581 -0.2675 0.6534 0.7082
-5.9212 9.2585 2.8952 -0.3783 0.9040 -0.1992
-5.9397 9.6088 -1.5537 -0.2790 0.9385 0.2034
8.4385 -5.5541 4.9858 -0.2111 -0.8962 -0.3902
10.3687 -4.7550 0.0878 -0.2306 -0.9683 0.0962

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35230
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.027
_diffrn_reflns_theta_max         67.027
_diffrn_reflns_theta_min         3.555
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00 -40.00   0.50    2.00    -- -106.00  57.00-120.00   50
  2  ω    -64.00 -37.00   0.50    2.00    -- -106.00  57.00 -30.00   54
  3  ω    -65.00 -34.00   0.50    2.00    -- -106.00  57.00   0.00   62
  4  ω    -64.00 -39.00   0.50    2.00    -- -106.00  57.00  30.00   50
  5  ω   -134.00 -99.00   0.50    2.00    -- -106.00   0.00 -30.00   70
  6  ω   -139.00-100.00   0.50    2.00    -- -106.00   0.00 -90.00   78
  7  ω   -160.00-108.00   0.50    2.00    -- -106.00 -19.00-180.00  104
  8  ω   -171.00-130.00   0.50    2.00    -- -106.00 -38.00   0.00   82
  9  ω   -125.00-100.00   0.50    2.00    -- -106.00 -38.00   0.00   50
 10  ω    -54.00  -7.00   0.50    0.50    --  -49.80 111.00   7.00   94
 11  ω    -98.00 -70.00   0.50    2.00    -- -106.00 111.00   7.00   56
 12  ω   -119.00 -35.00   0.50    0.50    --  -49.80 -77.00  30.00  168
 13  ω   -113.00 -73.00   0.50    0.50    --  -49.80-126.00 -30.00   80
 14  ω   -164.00 -95.00   0.50    2.00    -- -106.00-111.00 -86.00  138
 15  ω   -113.00 -87.00   0.50    0.50    --  -49.80-126.00 120.00   52
 16  ω    -22.00  24.00   0.50    0.50    --   49.80 -19.00-180.00   92
 17  ω     41.00  92.00   0.50    2.00    --  111.50 -77.00 -90.00  102
 18  ω     51.00  87.00   0.50    2.00    --  111.50 -77.00 -60.00   72
 19  ω     54.00  90.00   0.50    2.00    --  111.50 -77.00 -30.00   72
 20  ω     64.00 100.00   0.50    2.00    --  111.50-111.00 -86.00   72
 21  ω     82.00 113.00   0.50    2.00    --  111.50-126.00 -30.00   62
 22  ω     42.00  68.00   0.50    2.00    --  111.50-126.00 -30.00   52
 23  ω     29.00  84.00   0.50    0.50    --   49.80-111.00 -86.00  110
 24  ω     76.00 116.00   0.50    2.00    --  111.50   0.00 -30.00   80
 25  ω    103.00 158.00   0.50    2.00    --  111.50 111.00   7.00  110
 26  ω     76.00 109.00   0.50    0.50    --   49.80 126.00 -90.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0521191000
_diffrn_orient_matrix_UB_12      -0.0656587000
_diffrn_orient_matrix_UB_13      -0.0272746000
_diffrn_orient_matrix_UB_21      -0.0681059000
_diffrn_orient_matrix_UB_22      0.0550651000
_diffrn_orient_matrix_UB_23      -0.0031350000
_diffrn_orient_matrix_UB_31      0.0183314000
_diffrn_orient_matrix_UB_32      0.0180869000
_diffrn_orient_matrix_UB_33      -0.0891498000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4520
_reflns_number_total             4546
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 
;
 Flack x determined using 1960 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4546
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0320
_refine_ls_restrained_S_all      1.037
_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)+(0.0436P)²+20.8085P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0830
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-H5
 0.87 with sigma of 0.01
 C11-H5
 1.884088 with sigma of 0.02
 Cu2-H5
 3.113764 with sigma of 0.02
3. Rigid bond restraints
 O10, O9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N5, C18, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C19 \\sim C18 \\sim N5: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
N5 \\sim C18 \\sim C19: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Uanis(O11) = Uanis(O10) = Uanis(O9)
5. Rigid body (RIGU) restrains
 O10, O9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: N5(0.75) C19(0.75) H19a(0.75) H19b(0.75) H19c(0.75) C18(0.75)
7.a Ternary CH refined with riding coordinates:
 C12(H12)
7.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C1(H1a,H1b), C2(H2a,H2b), C10(H10a,H10b), C11(H11a,H11b)
7.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C17(H17), C7(H7), C8(H8), C14(H14), C9(H9), C15(H15), C16(H16)
7.d Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Tb1 Tb 0.54002(2) 0.68136(2) 0.65923(3) 0.02067(13) Uani 1 1 d . . . . .
Cu1 Cu 0.500000 0.500000 0.65483(9) 0.0209(3) Uani 1 2 d S T P . .
Cu2 Cu 0.74393(6) 0.35399(6) 0.49220(6) 0.0236(2) Uani 1 1 d D . . . .
O1 O 0.5863(3) 0.5627(3) 0.6683(3) 0.0254(11) Uani 1 1 d . . . . .
O3 O 0.7022(3) 0.4546(3) 0.4757(3) 0.0259(11) Uani 1 1 d . . . . .
O4 O 0.7091(4) 0.3383(3) 0.3830(3) 0.0337(13) Uani 1 1 d . . . . .
O2 O 0.5551(3) 0.4079(3) 0.6362(3) 0.0224(11) Uani 1 1 d . . . . .
O6 O 0.6084(3) 0.6998(4) 0.7888(3) 0.0339(13) Uani 1 1 d . . . . .
O8 O 0.5578(4) 0.6912(4) 0.9089(3) 0.0428(16) Uani 1 1 d . . . . .
N1 N 0.7937(3) 0.3906(3) 0.5942(4) 0.0224(12) Uani 1 1 d . . . . .
N3 N 0.5525(3) 0.6877(4) 0.8348(4) 0.0298(14) Uani 1 1 d . . . . .
N2 N 0.7593(4) 0.2428(3) 0.5142(4) 0.0242(13) Uani 1 1 d . . . . .
O7 O 0.4896(3) 0.6740(5) 0.7999(4) 0.0474(18) Uani 1 1 d . . . . .
C6 C 0.8124(4) 0.4848(4) 0.6949(5) 0.0269(16) Uani 1 1 d . . . . .
H6 H 0.792924 0.525673 0.726241 0.032 Uiso 1 1 calc R U . . .
O9 O 0.5240(4) 0.8190(4) 0.6878(5) 0.0605(12) Uani 1 1 d . . . . .
O5 O 0.8648(4) 0.3354(5) 0.4253(5) 0.058(2) Uani 1 1 d D . . . .
H5 H 0.908(3) 0.359(5) 0.423(6) 0.086 Uiso 1 1 d D U . . .
C13 C 0.7833(5) 0.1964(5) 0.4545(5) 0.0321(18) Uani 1 1 d . . . . .
O10 O 0.4200(4) 0.7587(4) 0.6639(6) 0.0605(12) Uani 1 1 d . . . . .
C5 C 0.7661(4) 0.4487(4) 0.6389(4) 0.0210(15) Uani 1 1 d . . . . .
C3 C 0.6738(4) 0.5022(4) 0.5377(4) 0.0216(14) Uani 1 1 d . . . . .
H3A H 0.619202 0.511833 0.527366 0.026 Uiso 1 1 calc R U . . .
H3B H 0.700517 0.551714 0.534817 0.026 Uiso 1 1 calc R U . . .
C1 C 0.6584(4) 0.5334(5) 0.6847(4) 0.0267(16) Uani 1 1 d . . . . .
H1A H 0.658957 0.512415 0.740305 0.032 Uiso 1 1 calc R U . . .
H1B H 0.696072 0.575196 0.682368 0.032 Uiso 1 1 calc R U . . .
C4 C 0.6825(4) 0.4703(4) 0.6246(4) 0.0200(14) Uani 1 1 d . . . . .
C17 C 0.7443(4) 0.2133(4) 0.5877(5) 0.0284(16) Uani 1 1 d . . . . .
H17 H 0.727574 0.246264 0.629687 0.034 Uiso 1 1 calc R U . . .
C7 C 0.8875(4) 0.4612(5) 0.7054(5) 0.0321(18) Uani 1 1 d . . . . .
H7 H 0.919631 0.486423 0.743125 0.039 Uiso 1 1 calc R U . . .
N4 N 0.4509(5) 0.8175(5) 0.6898(6) 0.052(2) Uani 1 1 d . . . . .
C8 C 0.9143(4) 0.4013(5) 0.6607(6) 0.0325(16) Uani 1 1 d . . . . .
H8 H 0.965067 0.383661 0.667075 0.039 Uiso 1 1 calc R U . . .
C14 C 0.7930(6) 0.1195(5) 0.4685(5) 0.041(2) Uani 1 1 d . . . . .
H14 H 0.810380 0.087057 0.426396 0.049 Uiso 1 1 calc R U . . .
C2 C 0.6343(4) 0.3974(4) 0.6393(4) 0.0223(15) Uani 1 1 d . . . . .
H2A H 0.648668 0.358931 0.598318 0.027 Uiso 1 1 calc R U . . .
H2B H 0.647645 0.376530 0.693185 0.027 Uiso 1 1 calc R U . . .
C9 C 0.8657(4) 0.3674(5) 0.6062(5) 0.0299(17) Uani 1 1 d . . . . .
H9 H 0.883936 0.325516 0.575468 0.036 Uiso 1 1 calc R U . . .
C12 C 0.7950(6) 0.2284(5) 0.3715(5) 0.041(2) Uani 1 1 d . . . . .
H12 H 0.803898 0.184283 0.334428 0.049 Uiso 1 1 calc R U . . .
C15 C 0.7773(7) 0.0902(5) 0.5444(6) 0.049(3) Uani 1 1 d . . . . .
H15 H 0.783659 0.037468 0.554881 0.058 Uiso 1 1 calc R U . . .
C10 C 0.7230(7) 0.2694(5) 0.3411(6) 0.050(3) Uani 1 1 d . . . . .
H10A H 0.728585 0.280358 0.282602 0.060 Uiso 1 1 calc R U . . .
H10B H 0.678626 0.235330 0.347905 0.060 Uiso 1 1 calc R U . . .
C16 C 0.7525(6) 0.1377(5) 0.6039(6) 0.043(2) Uani 1 1 d . . . . .
H16 H 0.740933 0.118351 0.656197 0.051 Uiso 1 1 calc R U . . .
C11 C 0.8632(7) 0.2786(7) 0.3653(7) 0.062(3) Uani 1 1 d D . . . .
H11A H 0.909688 0.247035 0.370034 0.075 Uiso 1 1 calc R U . . .
H11B H 0.863788 0.302964 0.311262 0.075 Uiso 1 1 calc R U . . .
N5 N 1.0030(9) 0.4046(9) 0.4360(11) 0.081(3) Uani 0.75 1 d . U P . .
C19 C 1.1246(10) 0.4419(11) 0.4984(14) 0.081(3) Uani 0.75 1 d . U P . .
H19A H 1.148793 0.478157 0.461368 0.122 Uiso 0.75 1 calc R U P . .
H19B H 1.157415 0.397232 0.504788 0.122 Uiso 0.75 1 calc R U P . .
H19C H 1.116929 0.466103 0.551248 0.122 Uiso 0.75 1 calc R U P . .
C18 C 1.0566(10) 0.4202(11) 0.4678(14) 0.081(3) Uani 0.75 1 d . U P . .
O11 O 0.4133(4) 0.8696(4) 0.7189(5) 0.0605(12) Uani 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
Tb1 Cu1 3.2659(4) . ?
Tb1 Cu2 3.3066(11) 4_656 ?
Tb1 O1 2.244(5) . ?
Tb1 O3 2.259(5) 4_656 ?
Tb1 O4 2.302(5) 4_656 ?
Tb1 O2 2.325(5) 2_665 ?
Tb1 O6 2.475(5) . ?
Tb1 N3 2.909(7) . ?
Tb1 O7 2.489(6) . ?
Tb1 O9 2.481(7) . ?
Tb1 O10 2.511(7) . ?
Tb1 N4 2.905(8) . ?
Cu1 O1 1.888(5) 2_665 ?
Cu1 O1 1.888(5) . ?
Cu1 O2 1.912(5) . ?
Cu1 O2 1.912(5) 2_665 ?
Cu2 O3 1.935(6) . ?
Cu2 O4 1.925(6) . ?
Cu2 N1 2.004(6) . ?
Cu2 N2 2.007(6) . ?
Cu2 O5 2.417(7) . ?
O1 C1 1.396(9) . ?
O3 C3 1.414(8) . ?
O4 C10 1.415(9) . ?
O2 C2 1.405(8) . ?
O6 N3 1.260(8) . ?
O8 N3 1.229(9) . ?
N1 C5 1.350(9) . ?
N1 C9 1.344(10) . ?
N3 O7 1.270(9) . ?
N2 C13 1.347(10) . ?
N2 C17 1.346(10) . ?
C6 H6 0.9500 . ?
C6 C5 1.385(11) . ?
C6 C7 1.394(11) . ?
O9 N4 1.286(11) . ?
O5 H5 0.869(13) . ?
O5 C11 1.408(14) . ?
C13 C14 1.382(12) . ?
C13 C12 1.495(12) . ?
O10 N4 1.245(11) . ?
C5 C4 1.537(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.548(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C4 1.547(10) . ?
C4 C2 1.555(9) . ?
C17 H17 0.9500 . ?
C17 C16 1.363(12) . ?
C7 H7 0.9500 . ?
C7 C8 1.371(13) . ?
N4 O11 1.228(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.377(12) . ?
C14 H14 0.9500 . ?
C14 C15 1.382(13) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C9 H9 0.9500 . ?
C12 H12 1.0000 . ?
C12 C10 1.542(13) . ?
C12 C11 1.492(16) . ?
C15 H15 0.9500 . ?
C15 C16 1.361(14) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C16 H16 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N5 C18 1.11(2) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19 C18 1.35(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cu1 Tb1 Cu2 115.43(3) . 4_656 ?
O1 Tb1 Cu1 34.10(12) . . ?
O1 Tb1 Cu2 98.94(14) . 4_656 ?
O1 Tb1 O3 101.61(19) . 4_656 ?
O1 Tb1 O4 83.1(2) . 4_656 ?
O1 Tb1 O2 69.16(17) . 2_665 ?
O1 Tb1 O6 83.6(2) . . ?
O1 Tb1 N3 86.7(2) . . ?
O1 Tb1 O7 91.0(2) . . ?
O1 Tb1 O9 159.2(2) . . ?
O1 Tb1 O10 143.7(2) . . ?
O1 Tb1 N4 161.8(2) . . ?
O3 Tb1 Cu1 98.35(13) 4_656 . ?
O3 Tb1 Cu2 34.63(14) 4_656 4_656 ?
O3 Tb1 O4 68.20(19) 4_656 4_656 ?
O3 Tb1 O2 88.73(18) 4_656 2_665 ?
O3 Tb1 O6 144.15(19) 4_656 . ?
O3 Tb1 N3 166.65(19) 4_656 . ?
O3 Tb1 O7 160.6(2) 4_656 . ?
O3 Tb1 O9 92.0(2) 4_656 . ?
O3 Tb1 O10 88.7(3) 4_656 . ?
O3 Tb1 N4 93.5(2) 4_656 . ?
O4 Tb1 Cu1 113.61(17) 4_656 . ?
O4 Tb1 Cu2 34.62(14) 4_656 4_656 ?
O4 Tb1 O2 139.7(2) 4_656 2_665 ?
O4 Tb1 O6 77.41(18) 4_656 . ?
O4 Tb1 N3 102.88(18) 4_656 . ?
O4 Tb1 O7 128.61(19) 4_656 . ?
O4 Tb1 O9 87.5(2) 4_656 . ?
O4 Tb1 O10 132.5(3) 4_656 . ?
O4 Tb1 N4 112.3(3) 4_656 . ?
O2 Tb1 Cu1 35.17(12) 2_665 . ?
O2 Tb1 Cu2 120.41(12) 2_665 4_656 ?
O2 Tb1 O6 125.41(18) 2_665 . ?
O2 Tb1 N3 104.09(18) 2_665 . ?
O2 Tb1 O7 82.0(2) 2_665 . ?
O2 Tb1 O9 127.4(2) 2_665 . ?
O2 Tb1 O10 76.4(2) 2_665 . ?
O2 Tb1 N4 101.3(2) 2_665 . ?
O6 Tb1 Cu1 104.57(15) . . ?
O6 Tb1 Cu2 109.63(13) . 4_656 ?
O6 Tb1 N3 25.47(18) . . ?
O6 Tb1 O7 51.21(18) . . ?
O6 Tb1 O9 76.3(2) . . ?
O6 Tb1 O10 108.1(2) . . ?
O6 Tb1 N4 90.2(2) . . ?
N3 Tb1 Cu1 94.35(14) . . ?
N3 Tb1 Cu2 134.27(13) . 4_656 ?
O7 Tb1 Cu1 83.9(2) . . ?
O7 Tb1 Cu2 157.44(16) . 4_656 ?
O7 Tb1 N3 25.74(18) . . ?
O7 Tb1 O10 72.6(3) . . ?
O7 Tb1 N4 71.9(3) . . ?
O9 Tb1 Cu1 158.74(19) . . ?
O9 Tb1 Cu2 83.3(2) . 4_656 ?
O9 Tb1 N3 77.4(2) . . ?
O9 Tb1 O7 80.4(3) . . ?
O9 Tb1 O10 51.1(2) . . ?
O9 Tb1 N4 26.1(2) . . ?
O10 Tb1 Cu1 110.36(17) . . ?
O10 Tb1 Cu2 108.5(2) . 4_656 ?
O10 Tb1 N3 90.7(2) . . ?
O10 Tb1 N4 25.3(2) . . ?
N4 Tb1 Cu1 133.80(19) . . ?
N4 Tb1 Cu2 99.3(2) . 4_656 ?
N4 Tb1 N3 80.5(2) . . ?
Tb1 Cu1 Tb1 177.46(6) 2_665 . ?
O1 Cu1 Tb1 41.78(15) . . ?
O1 Cu1 Tb1 137.77(16) 2_665 . ?
O1 Cu1 Tb1 41.78(15) 2_665 2_665 ?
O1 Cu1 Tb1 137.77(16) . 2_665 ?
O1 Cu1 O1 166.5(3) 2_665 . ?
O1 Cu1 O2 96.1(2) . . ?
O1 Cu1 O2 96.1(2) 2_665 2_665 ?
O1 Cu1 O2 86.1(2) . 2_665 ?
O1 Cu1 O2 86.1(2) 2_665 . ?
O2 Cu1 Tb1 44.45(14) 2_665 . ?
O2 Cu1 Tb1 44.45(14) . 2_665 ?
O2 Cu1 Tb1 136.14(14) . . ?
O2 Cu1 Tb1 136.14(14) 2_665 2_665 ?
O2 Cu1 O2 161.5(3) . 2_665 ?
O3 Cu2 Tb1 41.57(15) . 3_566 ?
O3 Cu2 N1 89.5(2) . . ?
O3 Cu2 N2 165.4(2) . . ?
O3 Cu2 O5 113.1(2) . . ?
O4 Cu2 Tb1 42.80(15) . 3_566 ?
O4 Cu2 O3 83.0(2) . . ?
O4 Cu2 N1 166.5(3) . . ?
O4 Cu2 N2 94.2(2) . . ?
O4 Cu2 O5 80.3(3) . . ?
N1 Cu2 Tb1 126.86(17) . 3_566 ?
N1 Cu2 N2 95.8(2) . . ?
N1 Cu2 O5 92.5(3) . . ?
N2 Cu2 Tb1 136.94(18) . 3_566 ?
N2 Cu2 O5 80.4(3) . . ?
O5 Cu2 Tb1 91.31(19) . 3_566 ?
Cu1 O1 Tb1 104.1(2) . . ?
C1 O1 Tb1 133.3(5) . . ?
C1 O1 Cu1 122.5(5) . . ?
Cu2 O3 Tb1 103.8(2) . 3_566 ?
C3 O3 Tb1 129.3(4) . 3_566 ?
C3 O3 Cu2 124.9(4) . . ?
Cu2 O4 Tb1 102.6(2) . 3_566 ?
C10 O4 Tb1 133.2(5) . 3_566 ?
C10 O4 Cu2 121.7(5) . . ?
Cu1 O2 Tb1 100.4(2) . 2_665 ?
C2 O2 Tb1 128.2(4) . 2_665 ?
C2 O2 Cu1 127.4(4) . . ?
N3 O6 Tb1 96.9(4) . . ?
C5 N1 Cu2 123.1(5) . . ?
C9 N1 Cu2 115.9(5) . . ?
C9 N1 C5 119.1(7) . . ?
O6 N3 Tb1 57.6(3) . . ?
O6 N3 O7 115.9(6) . . ?
O8 N3 Tb1 179.4(6) . . ?
O8 N3 O6 122.2(6) . . ?
O8 N3 O7 121.8(6) . . ?
O7 N3 Tb1 58.3(4) . . ?
C13 N2 Cu2 120.0(5) . . ?
C17 N2 Cu2 120.7(5) . . ?
C17 N2 C13 119.3(7) . . ?
N3 O7 Tb1 95.9(4) . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C7 120.2(7) . . ?
C7 C6 H6 119.9 . . ?
N4 O9 Tb1 95.6(5) . . ?
Cu2 O5 H5 136(3) . . ?
C11 O5 Cu2 113.6(7) . . ?
C11 O5 H5 109(2) . . ?
N2 C13 C14 120.5(8) . . ?
N2 C13 C12 119.1(7) . . ?
C14 C13 C12 120.3(8) . . ?
N4 O10 Tb1 95.3(5) . . ?
N1 C5 C6 120.0(6) . . ?
N1 C5 C4 116.5(6) . . ?
C6 C5 C4 123.5(6) . . ?
O3 C3 H3A 108.5 . . ?
O3 C3 H3B 108.5 . . ?
O3 C3 C4 115.0(6) . . ?
H3A C3 H3B 107.5 . . ?
C4 C3 H3A 108.5 . . ?
C4 C3 H3B 108.5 . . ?
O1 C1 H1A 109.0 . . ?
O1 C1 H1B 109.0 . . ?
O1 C1 C4 112.9(6) . . ?
H1A C1 H1B 107.8 . . ?
C4 C1 H1A 109.0 . . ?
C4 C1 H1B 109.0 . . ?
C5 C4 C3 109.0(5) . . ?
C5 C4 C1 109.9(6) . . ?
C5 C4 C2 107.1(6) . . ?
C3 C4 C2 113.0(6) . . ?
C1 C4 C3 107.9(6) . . ?
C1 C4 C2 110.0(6) . . ?
N2 C17 H17 119.0 . . ?
N2 C17 C16 122.1(8) . . ?
C16 C17 H17 119.0 . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.1(7) . . ?
C8 C7 H7 120.4 . . ?
O9 N4 Tb1 58.2(4) . . ?
O10 N4 Tb1 59.4(4) . . ?
O10 N4 O9 116.4(8) . . ?
O11 N4 Tb1 166.8(8) . . ?
O11 N4 O9 122.3(8) . . ?
O11 N4 O10 121.3(9) . . ?
C7 C8 H8 121.0 . . ?
C7 C8 C9 118.1(7) . . ?
C9 C8 H8 121.0 . . ?
C13 C14 H14 120.3 . . ?
C13 C14 C15 119.5(8) . . ?
C15 C14 H14 120.3 . . ?
O2 C2 C4 115.2(6) . . ?
O2 C2 H2A 108.5 . . ?
O2 C2 H2B 108.5 . . ?
C4 C2 H2A 108.5 . . ?
C4 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
N1 C9 C8 123.4(8) . . ?
N1 C9 H9 118.3 . . ?
C8 C9 H9 118.3 . . ?
C13 C12 H12 106.9 . . ?
C13 C12 C10 111.2(8) . . ?
C10 C12 H12 106.9 . . ?
C11 C12 C13 113.4(9) . . ?
C11 C12 H12 106.9 . . ?
C11 C12 C10 111.2(8) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 C14 119.3(9) . . ?
C16 C15 H15 120.3 . . ?
O4 C10 C12 112.5(8) . . ?
O4 C10 H10A 109.1 . . ?
O4 C10 H10B 109.1 . . ?
C12 C10 H10A 109.1 . . ?
C12 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C17 C16 H16 120.3 . . ?
C15 C16 C17 119.4(9) . . ?
C15 C16 H16 120.3 . . ?
O5 C11 C12 112.8(8) . . ?
O5 C11 H11A 109.0 . . ?
O5 C11 H11B 109.0 . . ?
C12 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
N5 C18 C19 174(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 Cu1 O1 Tb1 -176.26(8) 2_665 . . . ?
Tb1 Cu1 O1 C1 176.7(7) . . . . ?
Tb1 Cu1 O1 C1 0.5(7) 2_665 . . . ?
Tb1 O1 C1 C4 -132.9(6) . . . . ?
Tb1 O3 C3 C4 164.8(4) 3_566 . . . ?
Tb1 O4 C10 C12 131.4(7) 3_566 . . . ?
Tb1 O2 C2 C4 -177.2(4) 2_665 . . . ?
Tb1 O6 N3 O8 -179.3(7) . . . . ?
Tb1 O6 N3 O7 -1.3(8) . . . . ?
Tb1 O9 N4 O10 -12.6(11) . . . . ?
Tb1 O9 N4 O11 164.4(10) . . . . ?
Tb1 O10 N4 O9 12.4(11) . . . . ?
Tb1 O10 N4 O11 -164.6(9) . . . . ?
Cu1 O1 C1 C4 51.5(8) . . . . ?
Cu1 O2 C2 C4 -24.4(8) . . . . ?
Cu2 O3 C3 C4 3.6(9) . . . . ?
Cu2 O4 C10 C12 -27.0(11) . . . . ?
Cu2 N1 C5 C6 -162.3(5) . . . . ?
Cu2 N1 C5 C4 18.5(8) . . . . ?
Cu2 N1 C9 C8 163.1(6) . . . . ?
Cu2 N2 C13 C14 -179.0(7) . . . . ?
Cu2 N2 C13 C12 -2.4(11) . . . . ?
Cu2 N2 C17 C16 178.3(7) . . . . ?
Cu2 O5 C11 C12 -15.8(11) . . . . ?
O1 Cu1 O1 Tb1 -95.68(19) 2_665 . . . ?
O1 Cu1 O1 C1 81.0(5) 2_665 . . . ?
O1 C1 C4 C5 172.2(6) . . . . ?
O1 C1 C4 C3 53.4(8) . . . . ?
O1 C1 C4 C2 -70.2(8) . . . . ?
O3 C3 C4 C5 53.5(8) . . . . ?
O3 C3 C4 C1 172.8(6) . . . . ?
O3 C3 C4 C2 -65.4(8) . . . . ?
O2 Cu1 O1 Tb1 165.7(2) . . . . ?
O2 Cu1 O1 Tb1 4.2(2) 2_665 . . . ?
O2 Cu1 O1 C1 -17.6(6) . . . . ?
O2 Cu1 O1 C1 -179.1(5) 2_665 . . . ?
O6 N3 O7 Tb1 1.3(8) . . . . ?
O8 N3 O7 Tb1 179.3(7) . . . . ?
N1 C5 C4 C3 -66.1(8) . . . . ?
N1 C5 C4 C1 175.9(6) . . . . ?
N1 C5 C4 C2 56.5(8) . . . . ?
N2 C13 C14 C15 0.6(15) . . . . ?
N2 C13 C12 C10 -54.2(11) . . . . ?
N2 C13 C12 C11 71.9(11) . . . . ?
N2 C17 C16 C15 0.7(15) . . . . ?
C6 C5 C4 C3 114.7(7) . . . . ?
C6 C5 C4 C1 -3.3(9) . . . . ?
C6 C5 C4 C2 -122.7(7) . . . . ?
C6 C7 C8 C9 0.8(12) . . . . ?
C13 N2 C17 C16 -0.1(12) . . . . ?
C13 C14 C15 C16 0.0(17) . . . . ?
C13 C12 C10 O4 70.5(11) . . . . ?
C13 C12 C11 O5 -51.4(12) . . . . ?
C5 N1 C9 C8 -1.9(11) . . . . ?
C5 C6 C7 C8 -1.1(12) . . . . ?
C5 C4 C2 O2 174.5(6) . . . . ?
C3 C4 C2 O2 -65.5(8) . . . . ?
C1 C4 C2 O2 55.1(8) . . . . ?
C17 N2 C13 C14 -0.5(13) . . . . ?
C17 N2 C13 C12 176.1(8) . . . . ?
C7 C6 C5 N1 -0.1(11) . . . . ?
C7 C6 C5 C4 179.0(7) . . . . ?
C7 C8 C9 N1 0.7(12) . . . . ?
C14 C13 C12 C10 122.4(10) . . . . ?
C14 C13 C12 C11 -111.5(10) . . . . ?
C14 C15 C16 C17 -0.6(17) . . . . ?
C9 N1 C5 C6 1.5(10) . . . . ?
C9 N1 C5 C4 -177.7(6) . . . . ?
C12 C13 C14 C15 -175.9(10) . . . . ?
C10 C12 C11 O5 74.7(11) . . . . ?
C11 C12 C10 O4 -56.8(11) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 178.8 33.9 ?
2 0.500 0.500 1.000 178.8 30.7 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.175
_oxdiff_exptl_absorpt_empirical_full_min 0.842
