# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1935708'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh'
;University of Calcutta
India
;
_audit_update_record             
;
2019-08-10 deposited with the CCDC.	2019-09-05 downloaded from the CCDC.
;
_audit_creation_date             2019-08-05
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled 2019.07.31 svn.r3643 for OlexSys, GUI svn.r5859)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H22 Cu3 N2 O4, H2 O1, 2.5[H2O]'
_chemical_formula_sum            'C20 H29 Cu N2 O7.50'
_chemical_formula_weight         480.99
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.316(7)
_cell_length_b                   18.602(14)
_cell_length_c                   18.960(13)
_cell_angle_alpha                82.83(2)
_cell_angle_beta                 76.32(2)
_cell_angle_gamma                89.90(2)
_cell_volume                     3506(4)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    72801
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.137
_cell_measurement_theta_min      2.208
_shelx_estimated_absorpt_T_max   0.752
_shelx_estimated_absorpt_T_min   0.673
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.31
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1586
_diffrn_reflns_av_unetI/netI     0.1178
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            72729
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.208
_diffrn_ambient_temperature      296.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6194
_reflns_number_total             12271
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         12271
_refine_ls_number_restraints     715
_refine_ls_R_factor_all          0.1666
_refine_ls_R_factor_gt           0.0860
_refine_ls_restrained_S_all      1.031
_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)+(0.0937P)²+7.0636P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.2281
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C4A-C5A
 1.44 with sigma of 0.02
 C3A-C4A
 1.39 with sigma of 0.02
 C8AB-C9AB
 1.4 with sigma of 0.02
 C9AB-C10A
 1.42 with sigma of 0.02
 C20A-C19A \\sim C4-C3 \\sim C20C-C19C
 with sigma of 0.001
3. Rigid bond restraints
 C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C3 \\sim C4: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C9AB) \\sim Ueq, Uanis(C9AA) \\sim Ueq, Uanis(C8AB) \\sim Ueq,
Uanis(C8AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C16B, O4B, C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1A, C2A, C6A, O1A, C3A, O3A, C5A, C7A, Cu1A, C4A, C18A, N1A, N2A, O2A, C8AB,
 C10A, C11A, C17A, C9AB, C12A, C16A, C13A, C15A, O4A, C14A, C19A, C20A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1A, C8AA, C9AB, C10A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1A, C8AB, C9AA, C10A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N2B, C1B, C2B, C6B, O1B, C3B, O3B, C7B, C5B, Cu1B, C4B, C18B, N1B, O2B, C8B,
 C10B, C11B, C17B, C9B, C12B, C16B, C13B, C15B, O4B, C14B, C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1C, C2C, C6C, O1C, C3C, O3C, C5C, C7C, Cu1C, C4C, C18C, N1C, N2C, O2C, C8C,
 C10C, C11C, C17C, C9C, C12C, C16C, C13C, C15C, O4C, C14C, C19C, C20C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: C8AB(0.5) H8AA(0.5) H8AB(0.5) C9AB(0.5) H9AA(0.5) H9AB(0.5)
 H10A(0.5) H10B(0.5) H10C(0.5) H10D(0.5) C9AA(0.5) H9AC(0.5) H9AD(0.5)
 C8AA(0.5) H8AC(0.5) H8AD(0.5)
7.a Free rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB), O1(H1A,H1B)
7.b Secondary CH2 refined with riding coordinates:
 C8AB(H8AA,H8AB), C9AB(H9AA,H9AB), C10A(H10A,H10B), C10A(H10C,H10D), C19A(H19A,
 H19B), C8B(H8BA,H8BB), C9B(H9BA,H9BB), C10B(H10E,H10F), C8C(H8CA,H8CB),
 C9C(H9CA,H9CB), C10C(H10G,H10H), C19C(H19C,H19D), C3(H3C,H3D), C9AA(H9AC,H9AD),
  C8AA(H8AC,H8AD)
7.c Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C4A(H4A), C5A(H5A), C7A(H7A), C11A(H11A), C13A(H13A), C14A(H14A),
 C15A(H15A), C3B(H3B), C4B(H4B), C5B(H5B), C7B(H7B), C11B(H11B), C13B(H13B),
 C14B(H14B), C15B(H15B), C3C(H3CA), C4C(H4CA), C5C(H5C), C7C(H7C), C11C(H11C),
 C13C(H13C), C14C(H14C), C15C(H15C)
7.d Idealised Me refined as rotating group:
 C18A(H18A,H18B,H18C), C20A(H20A,H20B,H20C), C18B(H18D,H18E,H18F), C18C(H18G,
 H18H,H18I), C20C(H20D,H20E,H20F), C4(H4C,H4D,H4E)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1A C 0.5464(7) 0.7644(4) 0.8734(4) 0.0638(15) Uani 1 1 d . . . . .
C2A C 0.5885(9) 0.7861(4) 0.7959(5) 0.0735(18) Uani 1 1 d . . . . .
C3A C 0.5216(10) 0.8380(4) 0.7596(6) 0.095(2) Uani 1 1 d D . . . .
H3A H 0.550917 0.850975 0.708221 0.114 Uiso 1 1 calc R U . . .
C4A C 0.4112(10) 0.8706(5) 0.7995(7) 0.112(3) Uani 1 1 d D . . . .
H4A H 0.363945 0.905006 0.774559 0.134 Uiso 1 1 calc R U . . .
C5A C 0.3702(10) 0.8542(5) 0.8726(7) 0.109(3) Uani 1 1 d D . . . .
H5A H 0.295812 0.877787 0.898960 0.131 Uiso 1 1 calc R U . . .
O2W O 1.2670(10) 0.7126(5) 0.5237(4) 0.142(3) Uani 1 1 d G . . . .
H2WA H 1.272137 0.690577 0.485203 0.213 Uiso 1 1 d G U . . .
H2WB H 1.181939 0.718109 0.540353 0.213 Uiso 1 1 d G U . . .
C6A C 0.4381(8) 0.8019(4) 0.9103(5) 0.0789(18) Uani 1 1 d . . . . .
C7A C 0.3979(10) 0.7914(6) 0.9883(6) 0.103(2) Uani 1 1 d . . . . .
H7A H 0.334275 0.824176 1.009765 0.123 Uiso 1 1 calc R U . . .
C8AB C 0.3469(17) 0.7582(10) 1.1032(10) 0.086(3) Uani 0.5 1 d . U P A 2
H8AA H 0.252947 0.761434 1.099329 0.103 Uiso 0.5 1 calc R U P A 2
H8AB H 0.373935 0.803813 1.118304 0.103 Uiso 0.5 1 calc R U P A 2
C9AB C 0.2714(19) 0.6872(9) 1.1311(12) 0.111(4) Uani 0.5 1 d D U P A 1
H9AA H 0.200119 0.695876 1.174148 0.133 Uiso 0.5 1 calc R U P A 1
H9AB H 0.237837 0.694483 1.086037 0.133 Uiso 0.5 1 calc R U P A 1
C10A C 0.3356(8) 0.6167(5) 1.1412(4) 0.084(2) Uani 1 1 d D . . . .
H10A H 0.264663 0.578913 1.148265 0.101 Uiso 0.5 1 calc R U P A 1
H10B H 0.362273 0.614435 1.188281 0.101 Uiso 0.5 1 calc R U P A 1
H10C H 0.261454 0.627569 1.116983 0.101 Uiso 0.5 1 calc R U P A 2
H10D H 0.305164 0.576850 1.181608 0.101 Uiso 0.5 1 calc R U P A 2
C11A C 0.4854(8) 0.5275(5) 1.0997(4) 0.0708(17) Uani 1 1 d . . . . .
H11A H 0.426365 0.498408 1.138847 0.085 Uiso 1 1 calc R U . . .
C12A C 0.5993(7) 0.4920(5) 1.0623(4) 0.0651(15) Uani 1 1 d . . . . .
C13A C 0.6169(9) 0.4183(5) 1.0874(4) 0.0812(19) Uani 1 1 d . . . . .
H13A H 0.550698 0.393526 1.126394 0.097 Uiso 1 1 calc R U . . .
C14A C 0.7249(9) 0.3829(6) 1.0571(5) 0.0887(19) Uani 1 1 d . . . . .
H14A H 0.733443 0.333476 1.074639 0.106 Uiso 1 1 calc R U . . .
C15A C 0.8247(9) 0.4172(5) 1.0005(5) 0.0854(19) Uani 1 1 d . . . . .
H15A H 0.901606 0.391461 0.980746 0.102 Uiso 1 1 calc R U . . .
C16A C 0.8128(8) 0.4889(5) 0.9724(4) 0.0742(16) Uani 1 1 d . . . . .
C17A C 0.6960(7) 0.5291(5) 1.0023(4) 0.0650(15) Uani 1 1 d . . . . .
C18A C 0.7525(14) 0.7734(6) 0.6865(5) 0.146(5) Uani 1 1 d . . . . .
H18A H 0.684523 0.766854 0.659243 0.219 Uiso 1 1 calc R U . . .
H18B H 0.829879 0.744349 0.668633 0.219 Uiso 1 1 calc R U . . .
H18C H 0.780120 0.824654 0.679462 0.219 Uiso 1 1 calc R U . . .
C19A C 1.0147(8) 0.4940(6) 0.8795(5) 0.102(3) Uani 1 1 d D . . . .
H19A H 0.985463 0.451864 0.859536 0.123 Uiso 1 1 calc R U . . .
H19B H 1.068822 0.476321 0.914547 0.123 Uiso 1 1 calc R U . . .
C20A C 1.0946(9) 0.5453(6) 0.8200(5) 0.116(3) Uani 1 1 d D . . . .
H20A H 1.041504 0.561084 0.784588 0.174 Uiso 1 1 calc R U . . .
H20B H 1.174617 0.521583 0.795479 0.174 Uiso 1 1 calc R U . . .
H20C H 1.121003 0.587518 0.840099 0.174 Uiso 1 1 calc R U . . .
C1B C 1.1397(7) 0.5984(4) 0.4021(4) 0.0637(15) Uani 1 1 d . . . . .
C2B C 1.1385(9) 0.6692(5) 0.3634(4) 0.0801(18) Uani 1 1 d . . . . .
C3B C 1.0677(9) 0.6807(6) 0.3074(4) 0.095(2) Uani 1 1 d . . . . .
H3B H 1.065061 0.728072 0.282385 0.115 Uiso 1 1 calc R U . . .
C4B C 1.0033(9) 0.6239(7) 0.2892(5) 0.103(2) Uani 1 1 d . . . . .
H4B H 0.956293 0.632992 0.251707 0.123 Uiso 1 1 calc R U . . .
C5B C 1.0042(8) 0.5543(6) 0.3234(4) 0.090(2) Uani 1 1 d . . . . .
H5B H 0.959716 0.515742 0.309449 0.108 Uiso 1 1 calc R U . . .
C6B C 1.0745(7) 0.5413(5) 0.3812(4) 0.0694(15) Uani 1 1 d . . . . .
C7B C 1.0805(7) 0.4670(5) 0.4111(4) 0.0733(17) Uani 1 1 d . . . . .
H7B H 1.032951 0.432634 0.392936 0.088 Uiso 1 1 calc R U . . .
C8B C 1.1397(10) 0.3613(5) 0.4746(5) 0.099(2) Uani 1 1 d . . . . .
H8BA H 1.044935 0.345433 0.493695 0.119 Uiso 1 1 calc R U . . .
H8BB H 1.171123 0.342850 0.426896 0.119 Uiso 1 1 calc R U . . .
C9B C 1.2119(10) 0.3273(5) 0.5225(6) 0.108(3) Uani 1 1 d . . . . .
H9BA H 1.211792 0.274681 0.518663 0.129 Uiso 1 1 calc R U . . .
H9BB H 1.164347 0.333573 0.573092 0.129 Uiso 1 1 calc R U . . .
C10B C 1.3586(9) 0.3544(5) 0.5101(5) 0.098(2) Uani 1 1 d . . . . .
H10E H 1.408743 0.318209 0.535072 0.117 Uiso 1 1 calc R U . . .
H10F H 1.401841 0.360795 0.457102 0.117 Uiso 1 1 calc R U . . .
C11B C 1.4416(7) 0.4344(5) 0.5832(4) 0.0756(17) Uani 1 1 d . . . . .
H11B H 1.500406 0.395981 0.589010 0.091 Uiso 1 1 calc R U . . .
C12B C 1.4527(7) 0.4948(5) 0.6224(4) 0.0759(16) Uani 1 1 d . . . . .
C13B C 1.5549(8) 0.4932(6) 0.6643(4) 0.093(2) Uani 1 1 d . . . . .
H13B H 1.612345 0.453267 0.665127 0.111 Uiso 1 1 calc R U . . .
C14B C 1.5674(9) 0.5498(7) 0.7026(5) 0.108(2) Uani 1 1 d . . . . .
H14B H 1.637660 0.550616 0.727165 0.130 Uiso 1 1 calc R U . . .
C15B C 1.4796(8) 0.6048(6) 0.7056(4) 0.097(2) Uani 1 1 d . . . . .
H15B H 1.487223 0.642113 0.734500 0.116 Uiso 1 1 calc R U . . .
C16B C 1.3781(8) 0.6081(5) 0.6673(4) 0.0807(18) Uani 1 1 d . . . . .
C17B C 1.3676(7) 0.5524(5) 0.6219(4) 0.0647(15) Uani 1 1 d . . . . .
C18B C 1.2215(14) 0.7950(5) 0.3481(6) 0.147(5) Uani 1 1 d . . . . .
H18D H 1.266598 0.795774 0.296379 0.221 Uiso 1 1 calc R U . . .
H18E H 1.273914 0.824029 0.371722 0.221 Uiso 1 1 calc R U . . .
H18F H 1.132638 0.815245 0.352128 0.221 Uiso 1 1 calc R U . . .
C1C C 0.8696(8) 0.7588(5) 0.1409(4) 0.0721(17) Uani 1 1 d . . . . .
C2C C 0.7963(9) 0.7566(6) 0.2152(5) 0.089(2) Uani 1 1 d . . . . .
C3C C 0.7065(10) 0.6986(6) 0.2479(5) 0.108(3) Uani 1 1 d . . . . .
H3CA H 0.660219 0.696682 0.297842 0.129 Uiso 1 1 calc R U . . .
C4C C 0.6848(10) 0.6443(7) 0.2079(6) 0.113(3) Uani 1 1 d . . . . .
H4CA H 0.625144 0.604821 0.230881 0.136 Uiso 1 1 calc R U . . .
C5C C 0.7479(8) 0.6469(5) 0.1365(5) 0.097(3) Uani 1 1 d . . . . .
H5C H 0.732041 0.609396 0.109578 0.116 Uiso 1 1 calc R U . . .
C6C C 0.8383(7) 0.7059(4) 0.1010(5) 0.0704(16) Uani 1 1 d . . . . .
C7C C 0.8883(7) 0.7097(5) 0.0226(5) 0.078(2) Uani 1 1 d . . . . .
H7C H 0.865705 0.670115 0.000284 0.093 Uiso 1 1 calc R U . . .
C8C C 0.9896(11) 0.7578(5) -0.0985(5) 0.106(3) Uani 1 1 d . . . . .
H8CA H 0.955336 0.711125 -0.107913 0.127 Uiso 1 1 calc R U . . .
H8CB H 1.087393 0.760705 -0.118873 0.127 Uiso 1 1 calc R U . . .
C9C C 0.9242(16) 0.8206(7) -0.1359(7) 0.161(5) Uani 1 1 d . . . . .
H9CA H 0.935331 0.812289 -0.187563 0.193 Uiso 1 1 calc R U . . .
H9CB H 0.827321 0.816512 -0.113055 0.193 Uiso 1 1 calc R U . . .
C10C C 0.9634(12) 0.8905(6) -0.1365(6) 0.120(3) Uani 1 1 d . . . . .
H10G H 0.882951 0.920186 -0.133271 0.144 Uiso 1 1 calc R U . . .
H10H H 1.023540 0.905976 -0.185101 0.144 Uiso 1 1 calc R U . . .
C11C C 1.0957(8) 0.9721(4) -0.0988(4) 0.0706(17) Uani 1 1 d . . . . .
H11C H 1.086006 0.999585 -0.142935 0.085 Uiso 1 1 calc R U . . .
C12C C 1.1795(8) 1.0041(4) -0.0603(4) 0.0673(16) Uani 1 1 d . . . . .
C13C C 1.2477(9) 1.0714(5) -0.0923(5) 0.091(2) Uani 1 1 d . . . . .
H13C H 1.233807 1.094405 -0.137384 0.110 Uiso 1 1 calc R U . . .
C14C C 1.3320(10) 1.1031(5) -0.0594(6) 0.103(3) Uani 1 1 d . . . . .
H14C H 1.375926 1.147795 -0.082279 0.123 Uiso 1 1 calc R U . . .
C15C C 1.3558(9) 1.0723(4) 0.0062(5) 0.092(2) Uani 1 1 d . . . . .
H15C H 1.414830 1.095730 0.028200 0.111 Uiso 1 1 calc R U . . .
C16C C 1.2923(8) 1.0060(4) 0.0402(4) 0.0700(17) Uani 1 1 d . . . . .
C17C C 1.2011(7) 0.9708(4) 0.0076(4) 0.0613(15) Uani 1 1 d . . . . .
C18C C 0.7407(16) 0.8276(8) 0.3211(5) 0.195(7) Uani 1 1 d . . . . .
H18G H 0.646970 0.827553 0.318546 0.293 Uiso 1 1 calc R U . . .
H18H H 0.766009 0.875046 0.331964 0.293 Uiso 1 1 calc R U . . .
H18I H 0.752926 0.789950 0.359798 0.293 Uiso 1 1 calc R U . . .
C19C C 1.3966(10) 1.0038(5) 0.1431(5) 0.096(3) Uani 1 1 d D . . . .
H19C H 1.487764 1.011170 0.111166 0.115 Uiso 1 1 calc R U . . .
H19D H 1.362558 1.051602 0.155531 0.115 Uiso 1 1 calc R U . . .
C20C C 1.3989(12) 0.9552(6) 0.2101(5) 0.130(4) Uani 1 1 d D . . . .
H20D H 1.424145 0.906739 0.197508 0.195 Uiso 1 1 calc R U . . .
H20E H 1.310112 0.952395 0.243480 0.195 Uiso 1 1 calc R U . . .
H20F H 1.463957 0.974002 0.233885 0.195 Uiso 1 1 calc R U . . .
Cu1A Cu 0.54352(9) 0.66127(5) 1.00084(5) 0.0660(3) Uani 1 1 d . . . . .
Cu1B Cu 1.24380(8) 0.50140(5) 0.51063(4) 0.0576(3) Uani 1 1 d . . . . .
Cu1C Cu 1.01837(8) 0.84926(5) 0.01341(5) 0.0593(3) Uani 1 1 d . . . . .
N1A N 0.4358(8) 0.7441(4) 1.0328(4) 0.0945(18) Uani 1 1 d . . . . .
N2A N 0.4527(6) 0.5931(4) 1.0874(3) 0.0692(14) Uani 1 1 d . . . . .
N1B N 1.1446(6) 0.4407(4) 0.4610(3) 0.0706(14) Uani 1 1 d . . . . .
N2B N 1.3602(6) 0.4253(4) 0.5401(3) 0.0703(13) Uani 1 1 d . . . . .
N1C N 0.9600(6) 0.7613(4) -0.0196(3) 0.0687(14) Uani 1 1 d . . . . .
N2C N 1.0311(6) 0.9102(4) -0.0809(3) 0.0693(14) Uani 1 1 d . . . . .
O1A O 0.6107(4) 0.7138(3) 0.9050(3) 0.0652(12) Uani 1 1 d . . . . .
O2A O 0.6866(4) 0.5964(3) 0.9735(2) 0.0674(12) Uani 1 1 d . . . . .
O3A O 0.6976(6) 0.7502(3) 0.7635(3) 0.0906(17) Uani 1 1 d . . . . .
O4A O 0.9016(5) 0.5306(3) 0.9157(3) 0.0850(15) Uani 1 1 d . . . . .
O1B O 1.2034(5) 0.5892(3) 0.4561(2) 0.0666(12) Uani 1 1 d . . . . .
O2B O 1.2755(4) 0.5604(3) 0.5817(2) 0.0657(12) Uani 1 1 d . . . . .
O3B O 1.2084(7) 0.7206(3) 0.3841(3) 0.108(2) Uani 1 1 d . . . . .
O4B O 1.2859(6) 0.6604(4) 0.6689(3) 0.0999(17) Uani 1 1 d . . . . .
O1C O 0.9590(5) 0.8122(3) 0.1147(3) 0.0708(13) Uani 1 1 d . . . . .
O2C O 1.1411(5) 0.9099(2) 0.0434(2) 0.0592(11) Uani 1 1 d . . . . .
O3C O 0.8263(7) 0.8129(4) 0.2496(3) 0.113(2) Uani 1 1 d . . . . .
O4C O 1.3085(5) 0.9698(3) 0.1054(3) 0.0768(14) Uani 1 1 d . . . . .
O1W O 0.7809(8) 0.6115(4) 0.8081(4) 0.119(2) Uani 1 1 d G . . . .
H1WA H 0.734301 0.650460 0.807822 0.179 Uiso 1 1 d G U . . .
H1WB H 0.754770 0.589554 0.852625 0.179 Uiso 1 1 d G U . . .
C3 C 1.3089(15) 0.7175(8) 0.7083(9) 0.205(5) Uani 1 1 d D U . . .
H3C H 1.395591 0.743015 0.685427 0.246 Uiso 1 1 calc R U . . .
H3D H 1.306195 0.699354 0.759980 0.246 Uiso 1 1 calc R U . . .
C4 C 1.1964(15) 0.7645(8) 0.7022(9) 0.208(5) Uani 1 1 d D U . . .
H4C H 1.211323 0.789270 0.652081 0.311 Uiso 1 1 calc R U . . .
H4D H 1.189283 0.800515 0.736374 0.311 Uiso 1 1 calc R U . . .
H4E H 1.113627 0.735033 0.714023 0.311 Uiso 1 1 calc R U . . .
O1 O 1.0848(8) 0.8919(4) 0.2072(3) 0.113(2) Uani 1 1 d G . . . .
H1A H 1.135999 0.899237 0.163265 0.170 Uiso 1 1 d G U . . .
H1B H 1.024442 0.860511 0.204579 0.170 Uiso 1 1 d G U . . .
C9AA C 0.3679(17) 0.6783(11) 1.1699(10) 0.096(3) Uani 0.5 1 d . U P A 2
H9AC H 0.461026 0.676636 1.175192 0.115 Uiso 0.5 1 calc R U P A 2
H9AD H 0.307662 0.681300 1.218464 0.115 Uiso 0.5 1 calc R U P A 2
C8AA C 0.422(2) 0.7376(12) 1.1235(11) 0.105(4) Uani 0.5 1 d . U P A 1
H8AC H 0.409005 0.784307 1.143839 0.126 Uiso 0.5 1 calc R U P A 1
H8AD H 0.492274 0.709286 1.140774 0.126 Uiso 0.5 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
C1A C2A 1.436(11) . ?
C1A C6A 1.405(10) . ?
C1A O1A 1.314(8) . ?
C2A C3A 1.391(11) . ?
C2A O3A 1.366(9) . ?
C3A H3A 0.9500 . ?
C3A C4A 1.393(11) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.346(12) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.418(12) . ?
O2W H2WA 0.8704 . ?
O2W H2WB 0.8699 . ?
C6A C7A 1.427(13) . ?
C7A H7A 0.9500 . ?
C7A N1A 1.267(12) . ?
C8AB H8AA 0.9900 . ?
C8AB H8AB 0.9900 . ?
C8AB N1A 1.483(17) . ?
C8AB C9AA 1.87(3) . ?
C9AB H9AA 0.9900 . ?
C9AB H9AB 0.9900 . ?
C9AB C10A 1.480(15) . ?
C9AB C8AA 1.78(3) . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
C10A H10C 0.9900 . ?
C10A H10D 0.9900 . ?
C10A N2A 1.490(10) . ?
C10A C9AA 1.400(19) . ?
C11A H11A 0.9500 . ?
C11A C12A 1.428(11) . ?
C11A N2A 1.273(10) . ?
C12A C13A 1.421(11) . ?
C12A C17A 1.426(10) . ?
C13A H13A 0.9500 . ?
C13A C14A 1.339(12) . ?
C14A H14A 0.9500 . ?
C14A C15A 1.388(12) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.389(11) . ?
C16A C17A 1.452(11) . ?
C16A O4A 1.387(9) . ?
C17A O2A 1.316(9) . ?
C18A H18A 0.9800 . ?
C18A H18B 0.9800 . ?
C18A H18C 0.9800 . ?
C18A O3A 1.446(10) . ?
C19A H19A 0.9900 . ?
C19A H19B 0.9900 . ?
C19A C20A 1.469(8) . ?
C19A O4A 1.424(10) . ?
C20A H20A 0.9800 . ?
C20A H20B 0.9800 . ?
C20A H20C 0.9800 . ?
C1B C2B 1.427(11) . ?
C1B C6B 1.404(11) . ?
C1B O1B 1.336(8) . ?
C2B C3B 1.420(12) . ?
C2B O3B 1.348(11) . ?
C3B H3B 0.9500 . ?
C3B C4B 1.371(13) . ?
C4B H4B 0.9500 . ?
C4B C5B 1.375(13) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.447(11) . ?
C6B C7B 1.434(11) . ?
C7B H7B 0.9500 . ?
C7B N1B 1.323(9) . ?
C8B H8BA 0.9900 . ?
C8B H8BB 0.9900 . ?
C8B C9B 1.397(12) . ?
C8B N1B 1.466(10) . ?
C9B H9BA 0.9900 . ?
C9B H9BB 0.9900 . ?
C9B C10B 1.551(12) . ?
C10B H10E 0.9900 . ?
C10B H10F 0.9900 . ?
C10B N2B 1.503(11) . ?
C11B H11B 0.9500 . ?
C11B C12B 1.440(12) . ?
C11B N2B 1.327(10) . ?
C12B C13B 1.461(11) . ?
C12B C17B 1.385(11) . ?
C13B H13B 0.9500 . ?
C13B C14B 1.375(14) . ?
C14B H14B 0.9500 . ?
C14B C15B 1.363(14) . ?
C15B H15B 0.9500 . ?
C15B C16B 1.406(11) . ?
C16B C17B 1.447(11) . ?
C16B O4B 1.357(10) . ?
C17B O2B 1.349(8) . ?
C18B H18D 0.9800 . ?
C18B H18E 0.9800 . ?
C18B H18F 0.9800 . ?
C18B O3B 1.456(10) . ?
C1C C2C 1.428(11) . ?
C1C C6C 1.396(11) . ?
C1C O1C 1.321(8) . ?
C2C C3C 1.404(12) . ?
C2C O3C 1.373(11) . ?
C3C H3CA 0.9500 . ?
C3C C4C 1.386(14) . ?
C4C H4CA 0.9500 . ?
C4C C5C 1.352(13) . ?
C5C H5C 0.9500 . ?
C5C C6C 1.431(10) . ?
C6C C7C 1.446(11) . ?
C7C H7C 0.9500 . ?
C7C N1C 1.280(9) . ?
C8C H8CA 0.9900 . ?
C8C H8CB 0.9900 . ?
C8C C9C 1.529(14) . ?
C8C N1C 1.464(10) . ?
C9C H9CA 0.9900 . ?
C9C H9CB 0.9900 . ?
C9C C10C 1.360(14) . ?
C10C H10G 0.9900 . ?
C10C H10H 0.9900 . ?
C10C N2C 1.477(11) . ?
C11C H11C 0.9500 . ?
C11C C12C 1.429(11) . ?
C11C N2C 1.298(9) . ?
C12C C13C 1.429(11) . ?
C12C C17C 1.425(10) . ?
C13C H13C 0.9500 . ?
C13C C14C 1.357(13) . ?
C14C H14C 0.9500 . ?
C14C C15C 1.379(12) . ?
C15C H15C 0.9500 . ?
C15C C16C 1.404(10) . ?
C16C C17C 1.439(11) . ?
C16C O4C 1.379(9) . ?
C17C O2C 1.320(8) . ?
C18C H18G 0.9800 . ?
C18C H18H 0.9800 . ?
C18C H18I 0.9800 . ?
C18C O3C 1.489(12) . ?
C19C H19C 0.9900 . ?
C19C H19D 0.9900 . ?
C19C C20C 1.469(8) . ?
C19C O4C 1.470(9) . ?
C20C H20D 0.9800 . ?
C20C H20E 0.9800 . ?
C20C H20F 0.9800 . ?
Cu1A N1A 1.972(8) . ?
Cu1A N2A 1.984(6) . ?
Cu1A O1A 1.924(5) . ?
Cu1A O2A 1.921(5) . ?
Cu1B N1B 1.984(7) . ?
Cu1B N2B 1.967(6) . ?
Cu1B O1B 1.921(5) . ?
Cu1B O2B 1.926(5) . ?
Cu1C N1C 1.968(7) . ?
Cu1C N2C 1.970(6) . ?
Cu1C O1C 1.911(5) . ?
Cu1C O2C 1.924(5) . ?
N1A C8AA 1.68(2) . ?
O4B C3 1.423(13) . ?
O1W H1WA 0.8696 . ?
O1W H1WB 0.8710 . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C3 C4 1.469(8) . ?
C4 H4C 0.9800 . ?
C4 H4D 0.9800 . ?
C4 H4E 0.9800 . ?
O1 H1A 0.8695 . ?
O1 H1B 0.8694 . ?
C9AA H9AC 0.9900 . ?
C9AA H9AD 0.9900 . ?
C8AA H8AC 0.9900 . ?
C8AA H8AD 0.9900 . ?

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
C6A C1A C2A 115.4(8) . . ?
O1A C1A C2A 119.8(7) . . ?
O1A C1A C6A 124.8(8) . . ?
C3A C2A C1A 122.0(8) . . ?
O3A C2A C1A 112.8(7) . . ?
O3A C2A C3A 125.2(8) . . ?
C2A C3A H3A 120.3 . . ?
C2A C3A C4A 119.4(10) . . ?
C4A C3A H3A 120.3 . . ?
C3A C4A H4A 119.4 . . ?
C5A C4A C3A 121.2(11) . . ?
C5A C4A H4A 119.4 . . ?
C4A C5A H5A 120.0 . . ?
C4A C5A C6A 120.0(10) . . ?
C6A C5A H5A 120.0 . . ?
H2WA O2W H2WB 104.5 . . ?
C1A C6A C5A 122.0(9) . . ?
C1A C6A C7A 120.4(9) . . ?
C5A C6A C7A 117.5(9) . . ?
C6A C7A H7A 115.7 . . ?
N1A C7A C6A 128.6(10) . . ?
N1A C7A H7A 115.7 . . ?
H8AA C8AB H8AB 108.9 . . ?
N1A C8AB H8AA 110.9 . . ?
N1A C8AB H8AB 110.9 . . ?
N1A C8AB C9AA 104.4(12) . . ?
C9AA C8AB H8AA 110.9 . . ?
C9AA C8AB H8AB 110.9 . . ?
H9AA C9AB H9AB 110.5 . . ?
C10A C9AB H9AA 113.1 . . ?
C10A C9AB H9AB 113.1 . . ?
C10A C9AB C8AA 93.0(13) . . ?
C8AA C9AB H9AA 113.1 . . ?
C8AA C9AB H9AB 113.1 . . ?
C9AB C10A H10A 106.4 . . ?
C9AB C10A H10B 106.4 . . ?
C9AB C10A N2A 123.9(10) . . ?
H10A C10A H10B 106.4 . . ?
H10C C10A H10D 108.0 . . ?
N2A C10A H10A 106.4 . . ?
N2A C10A H10B 106.4 . . ?
N2A C10A H10C 109.4 . . ?
N2A C10A H10D 109.4 . . ?
C9AA C10A H10C 109.4 . . ?
C9AA C10A H10D 109.4 . . ?
C9AA C10A N2A 111.2(9) . . ?
C12A C11A H11A 115.8 . . ?
N2A C11A H11A 115.8 . . ?
N2A C11A C12A 128.5(8) . . ?
C13A C12A C11A 118.3(7) . . ?
C13A C12A C17A 119.9(8) . . ?
C17A C12A C11A 121.8(8) . . ?
C12A C13A H13A 119.4 . . ?
C14A C13A C12A 121.3(9) . . ?
C14A C13A H13A 119.4 . . ?
C13A C14A H14A 119.4 . . ?
C13A C14A C15A 121.3(10) . . ?
C15A C14A H14A 119.4 . . ?
C14A C15A H15A 119.8 . . ?
C14A C15A C16A 120.5(9) . . ?
C16A C15A H15A 119.8 . . ?
C15A C16A C17A 120.4(8) . . ?
O4A C16A C15A 127.7(8) . . ?
O4A C16A C17A 111.9(8) . . ?
C12A C17A C16A 116.7(8) . . ?
O2A C17A C12A 124.5(7) . . ?
O2A C17A C16A 118.8(7) . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
O3A C18A H18A 109.5 . . ?
O3A C18A H18B 109.5 . . ?
O3A C18A H18C 109.5 . . ?
H19A C19A H19B 108.4 . . ?
C20A C19A H19A 110.0 . . ?
C20A C19A H19B 110.0 . . ?
O4A C19A H19A 110.0 . . ?
O4A C19A H19B 110.0 . . ?
O4A C19A C20A 108.3(8) . . ?
C19A C20A H20A 109.5 . . ?
C19A C20A H20B 109.5 . . ?
C19A C20A H20C 109.5 . . ?
H20A C20A H20B 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
C6B C1B C2B 118.4(8) . . ?
O1B C1B C2B 118.7(8) . . ?
O1B C1B C6B 122.9(7) . . ?
C3B C2B C1B 119.7(10) . . ?
O3B C2B C1B 115.1(8) . . ?
O3B C2B C3B 125.2(9) . . ?
C2B C3B H3B 119.8 . . ?
C4B C3B C2B 120.3(10) . . ?
C4B C3B H3B 119.8 . . ?
C3B C4B H4B 118.8 . . ?
C3B C4B C5B 122.3(10) . . ?
C5B C4B H4B 118.8 . . ?
C4B C5B H5B 120.8 . . ?
C4B C5B C6B 118.4(10) . . ?
C6B C5B H5B 120.8 . . ?
C1B C6B C5B 120.8(8) . . ?
C1B C6B C7B 123.2(7) . . ?
C7B C6B C5B 115.9(8) . . ?
C6B C7B H7B 116.2 . . ?
N1B C7B C6B 127.5(8) . . ?
N1B C7B H7B 116.2 . . ?
H8BA C8B H8BB 107.1 . . ?
C9B C8B H8BA 107.7 . . ?
C9B C8B H8BB 107.7 . . ?
C9B C8B N1B 118.5(9) . . ?
N1B C8B H8BA 107.7 . . ?
N1B C8B H8BB 107.7 . . ?
C8B C9B H9BA 108.3 . . ?
C8B C9B H9BB 108.3 . . ?
C8B C9B C10B 116.1(8) . . ?
H9BA C9B H9BB 107.4 . . ?
C10B C9B H9BA 108.3 . . ?
C10B C9B H9BB 108.3 . . ?
C9B C10B H10E 109.9 . . ?
C9B C10B H10F 109.9 . . ?
H10E C10B H10F 108.3 . . ?
N2B C10B C9B 109.0(7) . . ?
N2B C10B H10E 109.9 . . ?
N2B C10B H10F 109.9 . . ?
C12B C11B H11B 115.6 . . ?
N2B C11B H11B 115.6 . . ?
N2B C11B C12B 128.7(8) . . ?
C11B C12B C13B 118.3(9) . . ?
C17B C12B C11B 121.4(8) . . ?
C17B C12B C13B 120.4(9) . . ?
C12B C13B H13B 120.2 . . ?
C14B C13B C12B 119.6(10) . . ?
C14B C13B H13B 120.2 . . ?
C13B C14B H14B 119.8 . . ?
C15B C14B C13B 120.3(10) . . ?
C15B C14B H14B 119.8 . . ?
C14B C15B H15B 119.0 . . ?
C14B C15B C16B 122.1(11) . . ?
C16B C15B H15B 119.0 . . ?
C15B C16B C17B 119.3(9) . . ?
O4B C16B C15B 125.2(9) . . ?
O4B C16B C17B 115.5(7) . . ?
C12B C17B C16B 118.0(8) . . ?
O2B C17B C12B 124.5(8) . . ?
O2B C17B C16B 117.5(8) . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
O3B C18B H18D 109.5 . . ?
O3B C18B H18E 109.5 . . ?
O3B C18B H18F 109.5 . . ?
C6C C1C C2C 117.5(8) . . ?
O1C C1C C2C 117.4(8) . . ?
O1C C1C C6C 125.1(7) . . ?
C3C C2C C1C 120.2(10) . . ?
O3C C2C C1C 114.3(8) . . ?
O3C C2C C3C 125.4(9) . . ?
C2C C3C H3CA 119.8 . . ?
C4C C3C C2C 120.4(10) . . ?
C4C C3C H3CA 119.8 . . ?
C3C C4C H4CA 119.7 . . ?
C5C C4C C3C 120.6(10) . . ?
C5C C4C H4CA 119.7 . . ?
C4C C5C H5C 119.8 . . ?
C4C C5C C6C 120.5(10) . . ?
C6C C5C H5C 119.8 . . ?
C1C C6C C5C 120.4(8) . . ?
C1C C6C C7C 122.5(7) . . ?
C5C C6C C7C 117.0(8) . . ?
C6C C7C H7C 116.8 . . ?
N1C C7C C6C 126.4(8) . . ?
N1C C7C H7C 116.8 . . ?
H8CA C8C H8CB 108.2 . . ?
C9C C8C H8CA 109.7 . . ?
C9C C8C H8CB 109.7 . . ?
N1C C8C H8CA 109.7 . . ?
N1C C8C H8CB 109.7 . . ?
N1C C8C C9C 109.7(9) . . ?
C8C C9C H9CA 107.1 . . ?
C8C C9C H9CB 107.1 . . ?
H9CA C9C H9CB 106.8 . . ?
C10C C9C C8C 121.0(10) . . ?
C10C C9C H9CA 107.1 . . ?
C10C C9C H9CB 107.1 . . ?
C9C C10C H10G 107.2 . . ?
C9C C10C H10H 107.2 . . ?
C9C C10C N2C 120.4(10) . . ?
H10G C10C H10H 106.9 . . ?
N2C C10C H10G 107.2 . . ?
N2C C10C H10H 107.2 . . ?
C12C C11C H11C 116.0 . . ?
N2C C11C H11C 116.0 . . ?
N2C C11C C12C 127.9(7) . . ?
C11C C12C C13C 118.7(8) . . ?
C17C C12C C11C 123.0(7) . . ?
C17C C12C C13C 118.3(8) . . ?
C12C C13C H13C 119.3 . . ?
C14C C13C C12C 121.3(9) . . ?
C14C C13C H13C 119.3 . . ?
C13C C14C H14C 119.1 . . ?
C13C C14C C15C 121.8(9) . . ?
C15C C14C H14C 119.1 . . ?
C14C C15C H15C 120.2 . . ?
C14C C15C C16C 119.6(9) . . ?
C16C C15C H15C 120.2 . . ?
C15C C16C C17C 120.4(8) . . ?
O4C C16C C15C 124.9(8) . . ?
O4C C16C C17C 114.7(6) . . ?
C12C C17C C16C 118.5(7) . . ?
O2C C17C C12C 123.9(7) . . ?
O2C C17C C16C 117.6(7) . . ?
H18G C18C H18H 109.5 . . ?
H18G C18C H18I 109.5 . . ?
H18H C18C H18I 109.5 . . ?
O3C C18C H18G 109.5 . . ?
O3C C18C H18H 109.5 . . ?
O3C C18C H18I 109.5 . . ?
H19C C19C H19D 108.5 . . ?
C20C C19C H19C 110.2 . . ?
C20C C19C H19D 110.2 . . ?
C20C C19C O4C 107.5(7) . . ?
O4C C19C H19C 110.2 . . ?
O4C C19C H19D 110.2 . . ?
C19C C20C H20D 109.5 . . ?
C19C C20C H20E 109.5 . . ?
C19C C20C H20F 109.5 . . ?
H20D C20C H20E 109.5 . . ?
H20D C20C H20F 109.5 . . ?
H20E C20C H20F 109.5 . . ?
N1A Cu1A N2A 93.9(3) . . ?
O1A Cu1A N1A 90.9(3) . . ?
O1A Cu1A N2A 166.7(2) . . ?
O2A Cu1A N1A 164.6(3) . . ?
O2A Cu1A N2A 92.8(3) . . ?
O2A Cu1A O1A 85.7(2) . . ?
N2B Cu1B N1B 97.0(3) . . ?
O1B Cu1B N1B 92.3(3) . . ?
O1B Cu1B N2B 155.4(2) . . ?
O1B Cu1B O2B 87.1(2) . . ?
O2B Cu1B N1B 158.9(2) . . ?
O2B Cu1B N2B 92.1(3) . . ?
N1C Cu1C N2C 94.5(3) . . ?
O1C Cu1C N1C 93.4(2) . . ?
O1C Cu1C N2C 160.6(2) . . ?
O1C Cu1C O2C 86.1(2) . . ?
O2C Cu1C N1C 155.3(2) . . ?
O2C Cu1C N2C 93.9(2) . . ?
C7A N1A C8AB 101.1(11) . . ?
C7A N1A Cu1A 122.6(7) . . ?
C7A N1A C8AA 132.2(11) . . ?
C8AB N1A Cu1A 133.7(10) . . ?
C8AA N1A Cu1A 105.1(9) . . ?
C10A N2A Cu1A 120.2(6) . . ?
C11A N2A C10A 116.0(7) . . ?
C11A N2A Cu1A 123.8(6) . . ?
C7B N1B C8B 113.4(8) . . ?
C7B N1B Cu1B 124.0(6) . . ?
C8B N1B Cu1B 122.5(6) . . ?
C10B N2B Cu1B 117.6(6) . . ?
C11B N2B C10B 119.0(7) . . ?
C11B N2B Cu1B 123.3(6) . . ?
C7C N1C C8C 117.7(7) . . ?
C7C N1C Cu1C 124.4(6) . . ?
C8C N1C Cu1C 117.6(5) . . ?
C10C N2C Cu1C 122.7(6) . . ?
C11C N2C C10C 113.9(7) . . ?
C11C N2C Cu1C 123.3(6) . . ?
C1A O1A Cu1A 124.9(5) . . ?
C17A O2A Cu1A 127.7(5) . . ?
C2A O3A C18A 115.9(7) . . ?
C16A O4A C19A 115.8(7) . . ?
C1B O1B Cu1B 129.7(5) . . ?
C17B O2B Cu1B 128.5(5) . . ?
C2B O3B C18B 121.9(8) . . ?
C16B O4B C3 113.1(8) . . ?
C1C O1C Cu1C 124.7(5) . . ?
C17C O2C Cu1C 127.5(5) . . ?
C2C O3C C18C 121.2(9) . . ?
C16C O4C C19C 117.6(6) . . ?
H1WA O1W H1WB 104.5 . . ?
O4B C3 H3C 111.4 . . ?
O4B C3 H3D 111.4 . . ?
O4B C3 C4 101.6(11) . . ?
H3C C3 H3D 109.3 . . ?
C4 C3 H3C 111.4 . . ?
C4 C3 H3D 111.4 . . ?
C3 C4 H4C 109.5 . . ?
C3 C4 H4D 109.5 . . ?
C3 C4 H4E 109.5 . . ?
H4C C4 H4D 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
H1A O1 H1B 104.6 . . ?
C8AB C9AA H9AC 110.5 . . ?
C8AB C9AA H9AD 110.5 . . ?
C10A C9AA C8AB 106.3(13) . . ?
C10A C9AA H9AC 110.5 . . ?
C10A C9AA H9AD 110.5 . . ?
H9AC C9AA H9AD 108.7 . . ?
C9AB C8AA H8AC 114.5 . . ?
C9AB C8AA H8AD 114.5 . . ?
N1A C8AA C9AB 85.1(12) . . ?
N1A C8AA H8AC 114.5 . . ?
N1A C8AA H8AD 114.5 . . ?
H8AC C8AA H8AD 111.6 . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 161 electrons were
found in a volume of 835Å^3 in 1 void per unit cell.
This is consistent with the presence of 2.5[H2O] per
Formula Unit which account for 150 electrons per unit cell.
;
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 -0.182 0.000 0.500 835.0 161.1 '15 water'

_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1935711'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh'
;University of Calcutta
India
;
_audit_update_record             
;
2019-08-10 deposited with the CCDC.	2019-09-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-22
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5830)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H44 Cu2 Gd2 N6 O20, C2 H8 O2'
_chemical_formula_sum            'C44 H52 Cu2 Gd2 N6 O22'
_chemical_formula_weight         1458.52
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.1519(7)
_cell_length_b                   12.4217(6)
_cell_length_c                   14.2822(7)
_cell_angle_alpha                90
_cell_angle_beta                 92.9310(10)
_cell_angle_gamma                90
_cell_volume                     2507.4(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    70765
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.995
_cell_measurement_theta_min      2.568
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.536
_exptl_absorpt_correction_T_max  0.372
_exptl_absorpt_correction_T_min  0.262
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.28
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            70765
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.995
_diffrn_reflns_theta_min         2.568
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4423
_reflns_number_total             5462
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         1.531
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5462
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0449
_refine_ls_restrained_S_all      1.150
_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)+(0.0262P)²+18.8393P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1182
_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 Gd(H) groups
2. Restrained distances
 C19B-C20
 1.59 with sigma of 0.02
 O8-H8
 0.85 with sigma of 0.01
 Cu1-H8
 2.945074 with sigma of 0.02
 C22-H8
 1.850517 with sigma of 0.02
3. Rigid bond restraints
 C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C20: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C18A \\sim C18B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C19B \\sim C18: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C20) \\sim Ueq: with sigma of 0.06 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O3, C18B, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C19B, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C18A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C18)=
 Sof(H18F)=Sof(H18G)=Sof(H18H)=1-FVAR(1)
 Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(H18E)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C18B(H18A,H18B), C19B(H19A,H19B)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C13(H13), C14(H14), C15(H15)
7.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C18A(H18C,H18D,
 H18E), C18(H18F,H18G,H18H)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7236(5) 0.3263(6) 0.5508(5) 0.0447(15) Uani 1 1 d . . . . .
C2 C 0.6947(6) 0.2833(7) 0.4638(5) 0.0579(19) Uani 1 1 d . . . . .
C3 C 0.7586(7) 0.2547(8) 0.3980(6) 0.076(3) Uani 1 1 d . . . . .
H3 H 0.737433 0.226185 0.340530 0.091 Uiso 1 1 calc R U . . .
C4 C 0.8538(7) 0.2689(10) 0.4185(7) 0.092(3) Uani 1 1 d . . . . .
H4 H 0.897360 0.248545 0.375225 0.110 Uiso 1 1 calc R U . . .
C5 C 0.8837(6) 0.3120(10) 0.5009(7) 0.085(3) Uani 1 1 d . . . . .
H5 H 0.948241 0.322515 0.513070 0.103 Uiso 1 1 calc R U . . .
C6 C 0.8207(5) 0.3419(7) 0.5695(6) 0.0578(19) Uani 1 1 d . . . . .
C7 C 0.8604(5) 0.3895(8) 0.6545(6) 0.066(2) Uani 1 1 d . . . . .
H7 H 0.926064 0.393263 0.659918 0.080 Uiso 1 1 calc R U . . .
C8 C 0.8761(6) 0.4791(10) 0.7985(7) 0.086(3) Uani 1 1 d . . . . .
H8A H 0.939579 0.449585 0.797983 0.103 Uiso 1 1 calc R U . . .
H8B H 0.880360 0.555308 0.784628 0.103 Uiso 1 1 calc R U . . .
C9 C 0.8437(7) 0.4674(10) 0.8889(7) 0.087(3) Uani 1 1 d . . . . .
H9A H 0.895579 0.486438 0.932815 0.104 Uiso 1 1 calc R U . . .
H9B H 0.830809 0.391571 0.898081 0.104 Uiso 1 1 calc R U . . .
C10 C 0.7626(8) 0.5256(10) 0.9157(7) 0.097(4) Uani 1 1 d . . . . .
H10A H 0.776008 0.601938 0.911104 0.116 Uiso 1 1 calc R U . . .
H10B H 0.752726 0.509986 0.981039 0.116 Uiso 1 1 calc R U . . .
C11 C 0.5961(7) 0.5375(7) 0.8933(6) 0.068(2) Uani 1 1 d . . . . .
H11 H 0.603715 0.570088 0.951866 0.081 Uiso 1 1 calc R U . . .
C12 C 0.4999(6) 0.5336(7) 0.8536(5) 0.063(2) Uani 1 1 d . . . . .
C13 C 0.4321(8) 0.5914(9) 0.9011(6) 0.080(3) Uani 1 1 d . . . . .
H13 H 0.450470 0.626707 0.956528 0.096 Uiso 1 1 calc R U . . .
C14 C 0.3412(8) 0.5972(9) 0.8689(7) 0.087(3) Uani 1 1 d . . . . .
H14 H 0.297009 0.632923 0.903585 0.104 Uiso 1 1 calc R U . . .
C15 C 0.3135(6) 0.5500(8) 0.7843(7) 0.073(3) Uani 1 1 d . . . . .
H15 H 0.251221 0.556210 0.760739 0.088 Uiso 1 1 calc R U . . .
C16 C 0.3786(5) 0.4937(7) 0.7348(5) 0.0541(18) Uani 1 1 d . . . . .
C17 C 0.4732(5) 0.4805(6) 0.7701(5) 0.0495(17) Uani 1 1 d . . . . .
C18B C 0.569(3) 0.187(3) 0.3893(19) 0.067(7) Uani 0.428(18) 1 d . U P A 2
H18A H 0.619509 0.134723 0.385944 0.081 Uiso 0.428(18) 1 calc R U P A 2
H18B H 0.513384 0.151111 0.412518 0.081 Uiso 0.428(18) 1 calc R U P A 2
C19B C 0.2661(19) 0.4634(19) 0.606(2) 0.066(5) Uani 0.572(18) 1 d D U P A 1
H19A H 0.266644 0.451418 0.538699 0.080 Uiso 0.572(18) 1 calc R U P A 1
H19B H 0.245413 0.536710 0.616149 0.080 Uiso 0.572(18) 1 calc R U P A 1
C20 C 0.1974(14) 0.3841(16) 0.6493(16) 0.099(7) Uani 0.572(18) 1 d D U P A 1
H20A H 0.137461 0.386484 0.614786 0.149 Uiso 0.572(18) 1 calc R U P A 1
H20B H 0.189145 0.403731 0.713360 0.149 Uiso 0.572(18) 1 calc R U P A 1
H20C H 0.222864 0.312559 0.646899 0.149 Uiso 0.572(18) 1 calc R U P A 1
C21 C 0.6221(5) 0.6047(6) 0.5923(5) 0.0483(16) Uani 1 1 d . . . . .
C22 C 0.6270(7) 0.2314(10) 0.8687(7) 0.091(3) Uani 1 1 d D . . . .
H22A H 0.563931 0.256336 0.853389 0.136 Uiso 1 1 calc R U . . .
H22B H 0.648281 0.259131 0.928901 0.136 Uiso 1 1 calc R U . . .
H22C H 0.627488 0.154146 0.870511 0.136 Uiso 1 1 calc R U . . .
Cu1 Cu 0.67503(6) 0.43194(8) 0.73146(6) 0.0516(2) Uani 1 1 d D . . . .
Gd1 Gd 0.49570(2) 0.36020(3) 0.57084(2) 0.04152(11) Uani 1 1 d . . . . .
H8 H 0.733(3) 0.222(3) 0.803(4) 0.062 Uiso 1 1 d D U . . .
N1 N 0.8172(4) 0.4270(6) 0.7231(5) 0.0587(16) Uani 1 1 d . . . . .
N2 N 0.6717(5) 0.5026(6) 0.8595(4) 0.0658(19) Uani 1 1 d . . . . .
N3 N 0.4347(5) 0.1491(6) 0.6364(6) 0.074(2) Uani 1 1 d . . . . .
O1 O 0.6580(3) 0.3490(4) 0.6097(3) 0.0456(11) Uani 1 1 d . . . . .
O2 O 0.5311(3) 0.4197(4) 0.7242(3) 0.0483(11) Uani 1 1 d . . . . .
O3 O 0.5974(4) 0.2791(5) 0.4485(4) 0.0590(13) Uani 1 1 d . . . . .
O4 O 0.3602(3) 0.4481(4) 0.6480(4) 0.0562(13) Uani 1 1 d . . . . .
O5 O 0.6734(3) 0.5832(4) 0.6650(3) 0.0536(12) Uani 1 1 d . . . . .
O6 O 0.5581(3) 0.5367(4) 0.5585(3) 0.0523(12) Uani 1 1 d . . . . .
O7 O 0.6285(3) 0.6912(4) 0.5451(4) 0.0561(13) Uani 1 1 d . . . . .
O8 O 0.6866(4) 0.2667(5) 0.8017(4) 0.0664(15) Uani 1 1 d D . . . .
O9 O 0.5015(4) 0.1613(5) 0.5842(5) 0.0797(19) Uani 1 1 d . . . . .
O10 O 0.3974(5) 0.2319(5) 0.6642(5) 0.0819(19) Uani 1 1 d . . . . .
O11 O 0.4059(5) 0.0602(6) 0.6566(8) 0.128(4) Uani 1 1 d . . . . .
C23 C 0.547(2) 0.236(2) 0.2989(18) 0.092(9) Uani 0.428(18) 1 d . . P A 2
H23A H 0.539223 0.181585 0.251805 0.137 Uiso 0.428(18) 1 calc R U P A 2
H23B H 0.598028 0.283256 0.283812 0.137 Uiso 0.428(18) 1 calc R U P A 2
H23C H 0.489707 0.277333 0.301378 0.137 Uiso 0.428(18) 1 calc R U P A 2
C18A C 0.5580(17) 0.2287(17) 0.3610(14) 0.064(5) Uani 0.572(18) 1 d . U P A 1
H18C H 0.575582 0.270563 0.308172 0.096 Uiso 0.572(18) 1 calc R U P A 1
H18D H 0.490301 0.225815 0.362257 0.096 Uiso 0.572(18) 1 calc R U P A 1
H18E H 0.582646 0.157047 0.355984 0.096 Uiso 0.572(18) 1 calc R U P A 1
C18 C 0.260(2) 0.420(3) 0.619(3) 0.075(8) Uani 0.428(18) 1 d . U P A 2
H18F H 0.234679 0.372061 0.664205 0.112 Uiso 0.428(18) 1 calc R U P A 2
H18G H 0.258348 0.384388 0.558705 0.112 Uiso 0.428(18) 1 calc R U P A 2
H18H H 0.222275 0.483885 0.614195 0.112 Uiso 0.428(18) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.394(10) . ?
C1 C6 1.400(10) . ?
C1 O1 1.315(8) . ?
C2 C3 1.384(11) . ?
C2 O3 1.384(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.374(13) . ?
C4 H4 0.9300 . ?
C4 C5 1.342(14) . ?
C5 H5 0.9300 . ?
C5 C6 1.409(11) . ?
C6 C7 1.439(12) . ?
C7 H7 0.9300 . ?
C7 N1 1.269(10) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.400(13) . ?
C8 N1 1.478(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.425(14) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 N2 1.508(11) . ?
C11 H11 0.9300 . ?
C11 C12 1.449(12) . ?
C11 N2 1.272(11) . ?
C12 C13 1.401(11) . ?
C12 C17 1.398(11) . ?
C13 H13 0.9300 . ?
C13 C14 1.347(14) . ?
C14 H14 0.9300 . ?
C14 C15 1.382(14) . ?
C15 H15 0.9300 . ?
C15 C16 1.380(10) . ?
C16 C17 1.416(10) . ?
C16 O4 1.376(9) . ?
C17 O2 1.313(8) . ?
C18B H18A 0.9700 . ?
C18B H18B 0.9700 . ?
C18B O3 1.47(3) . ?
C18B C23 1.45(3) . ?
C19B H19A 0.9700 . ?
C19B H19B 0.9700 . ?
C19B C20 1.537(16) . ?
C19B O4 1.45(3) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O5 1.264(8) . ?
C21 O6 1.311(8) . ?
C21 O7 1.274(9) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C22 O8 1.379(11) . ?
Cu1 N1 2.023(6) . ?
Cu1 N2 2.032(6) . ?
Cu1 O1 2.025(5) . ?
Cu1 O2 2.040(5) . ?
Cu1 O5 2.105(5) . ?
Gd1 O1 2.339(4) . ?
Gd1 O2 2.341(5) . ?
Gd1 O3 2.529(5) . ?
Gd1 O4 2.511(5) . ?
Gd1 O6 2.343(5) 3_666 ?
Gd1 O6 2.374(5) . ?
Gd1 O7 2.437(5) 3_666 ?
Gd1 O9 2.479(6) . ?
Gd1 O10 2.538(6) . ?
N3 O9 1.243(9) . ?
N3 O10 1.231(9) . ?
N3 O11 1.217(9) . ?
O3 C18A 1.48(2) . ?
O4 C18 1.50(4) . ?
O8 H8 0.865(9) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C18A H18C 0.9600 . ?
C18A H18D 0.9600 . ?
C18A H18E 0.9600 . ?
C18 H18F 0.9600 . ?
C18 H18G 0.9600 . ?
C18 H18H 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 117.6(7) . . ?
O1 C1 C2 117.9(6) . . ?
O1 C1 C6 124.5(7) . . ?
C3 C2 C1 122.1(8) . . ?
C3 C2 O3 124.3(7) . . ?
O3 C2 C1 113.5(6) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.4(9) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0(8) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 118.9 . . ?
C4 C5 C6 122.2(8) . . ?
C6 C5 H5 118.9 . . ?
C1 C6 C5 118.7(8) . . ?
C1 C6 C7 123.7(7) . . ?
C5 C6 C7 117.5(7) . . ?
C6 C7 H7 115.9 . . ?
N1 C7 C6 128.3(7) . . ?
N1 C7 H7 115.9 . . ?
H8A C8 H8B 107.5 . . ?
C9 C8 H8A 108.4 . . ?
C9 C8 H8B 108.4 . . ?
C9 C8 N1 115.3(9) . . ?
N1 C8 H8A 108.4 . . ?
N1 C8 H8B 108.4 . . ?
C8 C9 H9A 107.3 . . ?
C8 C9 H9B 107.3 . . ?
C8 C9 C10 120.1(10) . . ?
H9A C9 H9B 106.9 . . ?
C10 C9 H9A 107.3 . . ?
C10 C9 H9B 107.3 . . ?
C9 C10 H10A 108.3 . . ?
C9 C10 H10B 108.3 . . ?
C9 C10 N2 116.0(8) . . ?
H10A C10 H10B 107.4 . . ?
N2 C10 H10A 108.3 . . ?
N2 C10 H10B 108.3 . . ?
C12 C11 H11 115.4 . . ?
N2 C11 H11 115.4 . . ?
N2 C11 C12 129.2(8) . . ?
C13 C12 C11 116.5(8) . . ?
C17 C12 C11 123.9(7) . . ?
C17 C12 C13 119.6(8) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 C12 121.9(9) . . ?
C14 C13 H13 119.1 . . ?
C13 C14 H14 120.0 . . ?
C13 C14 C15 120.0(8) . . ?
C15 C14 H14 120.0 . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.7(9) . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C17 121.4(8) . . ?
O4 C16 C15 124.7(7) . . ?
O4 C16 C17 113.9(6) . . ?
C12 C17 C16 117.3(7) . . ?
O2 C17 C12 123.3(7) . . ?
O2 C17 C16 119.4(7) . . ?
H18A C18B H18B 109.2 . . ?
O3 C18B H18A 111.2 . . ?
O3 C18B H18B 111.2 . . ?
C23 C18B H18A 111.2 . . ?
C23 C18B H18B 111.2 . . ?
C23 C18B O3 103(2) . . ?
H19A C19B H19B 108.2 . . ?
C20 C19B H19A 109.8 . . ?
C20 C19B H19B 109.8 . . ?
O4 C19B H19A 109.8 . . ?
O4 C19B H19B 109.8 . . ?
O4 C19B C20 109.6(18) . . ?
C19B C20 H20A 109.5 . . ?
C19B C20 H20B 109.5 . . ?
C19B C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O5 C21 O6 121.5(7) . . ?
O5 C21 O7 124.0(7) . . ?
O7 C21 O6 114.5(6) . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O8 C22 H22A 109.5 . . ?
O8 C22 H22B 109.5 . . ?
O8 C22 H22C 109.5 . . ?
N1 Cu1 N2 97.8(3) . . ?
N1 Cu1 O1 90.5(2) . . ?
N1 Cu1 O2 171.3(2) . . ?
N1 Cu1 O5 89.4(2) . . ?
N2 Cu1 O2 90.5(3) . . ?
N2 Cu1 O5 91.2(3) . . ?
O1 Cu1 N2 170.3(3) . . ?
O1 Cu1 O2 81.00(18) . . ?
O1 Cu1 O5 93.93(19) . . ?
O2 Cu1 O5 93.2(2) . . ?
O1 Gd1 O2 68.68(15) . . ?
O1 Gd1 O3 63.51(16) . . ?
O1 Gd1 O4 133.20(16) . . ?
O1 Gd1 O6 119.70(17) . 3_666 ?
O1 Gd1 O6 73.01(17) . . ?
O1 Gd1 O7 144.20(17) . 3_666 ?
O1 Gd1 O9 83.93(19) . . ?
O1 Gd1 O10 113.3(2) . . ?
O2 Gd1 O3 132.08(16) . . ?
O2 Gd1 O4 65.39(16) . . ?
O2 Gd1 O6 127.62(18) . 3_666 ?
O2 Gd1 O6 73.44(17) . . ?
O2 Gd1 O7 146.12(17) . 3_666 ?
O2 Gd1 O9 103.8(2) . . ?
O2 Gd1 O10 78.7(2) . . ?
O3 Gd1 O10 117.3(2) . . ?
O4 Gd1 O3 162.00(17) . . ?
O4 Gd1 O10 65.9(2) . . ?
O6 Gd1 O3 95.14(18) . . ?
O6 Gd1 O3 81.17(19) 3_666 . ?
O6 Gd1 O4 85.78(18) . . ?
O6 Gd1 O4 83.31(18) 3_666 . ?
O6 Gd1 O6 62.88(18) 3_666 . ?
O6 Gd1 O7 116.73(16) . 3_666 ?
O6 Gd1 O7 54.08(16) 3_666 3_666 ?
O6 Gd1 O9 127.8(2) 3_666 . ?
O6 Gd1 O9 156.23(18) . . ?
O6 Gd1 O10 126.3(2) 3_666 . ?
O6 Gd1 O10 146.6(2) . . ?
O7 Gd1 O3 80.95(18) 3_666 . ?
O7 Gd1 O4 82.60(18) 3_666 . ?
O7 Gd1 O9 79.1(2) 3_666 . ?
O7 Gd1 O10 78.3(2) 3_666 . ?
O9 Gd1 O3 68.8(2) . . ?
O9 Gd1 O4 115.02(19) . . ?
O9 Gd1 O10 49.5(2) . . ?
C7 N1 C8 116.6(7) . . ?
C7 N1 Cu1 125.2(5) . . ?
C8 N1 Cu1 118.0(6) . . ?
C10 N2 Cu1 120.2(6) . . ?
C11 N2 C10 116.4(7) . . ?
C11 N2 Cu1 123.2(6) . . ?
O10 N3 O9 116.4(7) . . ?
O11 N3 O9 121.8(9) . . ?
O11 N3 O10 121.8(8) . . ?
C1 O1 Cu1 127.0(4) . . ?
C1 O1 Gd1 125.3(4) . . ?
Cu1 O1 Gd1 104.25(18) . . ?
C17 O2 Cu1 125.3(5) . . ?
C17 O2 Gd1 122.7(4) . . ?
Cu1 O2 Gd1 103.67(18) . . ?
C2 O3 C18B 111.4(15) . . ?
C2 O3 Gd1 118.2(4) . . ?
C2 O3 C18A 118.5(11) . . ?
C18B O3 Gd1 123.9(15) . . ?
C18A O3 Gd1 123.3(10) . . ?
C16 O4 C19B 116.8(14) . . ?
C16 O4 Gd1 117.4(4) . . ?
C16 O4 C18 118.8(19) . . ?
C19B O4 Gd1 125.6(14) . . ?
C18 O4 Gd1 120.5(18) . . ?
C21 O5 Cu1 123.5(5) . . ?
C21 O6 Gd1 145.1(4) . . ?
C21 O6 Gd1 97.4(4) . 3_666 ?
Gd1 O6 Gd1 117.12(18) 3_666 . ?
C21 O7 Gd1 94.0(4) . 3_666 ?
C22 O8 Cu1 123.9(6) . . ?
C22 O8 H8 105.9(17) . . ?
Cu1 O8 H8 128.7(17) . . ?
N3 O9 Gd1 98.3(5) . . ?
N3 O10 Gd1 95.7(5) . . ?
C18B C23 H23A 109.5 . . ?
C18B C23 H23B 109.5 . . ?
C18B C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O3 C18A H18C 109.5 . . ?
O3 C18A H18D 109.5 . . ?
O3 C18A H18E 109.5 . . ?
H18C C18A H18D 109.5 . . ?
H18C C18A H18E 109.5 . . ?
H18D C18A H18E 109.5 . . ?
O4 C18 H18F 109.5 . . ?
O4 C18 H18G 109.5 . . ?
O4 C18 H18H 109.5 . . ?
H18F C18 H18G 109.5 . . ?
H18F C18 H18H 109.5 . . ?
H18G C18 H18H 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
C1 C2 C3 C4 0.0(15) . . . . ?
C1 C2 O3 C18B -148.2(13) . . . . ?
C1 C2 O3 Gd1 4.5(9) . . . . ?
C1 C2 O3 C18A -176.2(11) . . . . ?
C1 C6 C7 N1 -2.2(15) . . . . ?
C2 C1 C6 C5 -1.0(12) . . . . ?
C2 C1 C6 C7 177.4(8) . . . . ?
C2 C1 O1 Cu1 -170.0(5) . . . . ?
C2 C1 O1 Gd1 -14.5(9) . . . . ?
C2 C3 C4 C5 -1.3(18) . . . . ?
C3 C2 O3 C18B 35.8(16) . . . . ?
C3 C2 O3 Gd1 -171.5(7) . . . . ?
C3 C2 O3 C18A 7.8(15) . . . . ?
C3 C4 C5 C6 1.4(19) . . . . ?
C4 C5 C6 C1 -0.2(16) . . . . ?
C4 C5 C6 C7 -178.7(11) . . . . ?
C5 C6 C7 N1 176.2(10) . . . . ?
C6 C1 C2 C3 1.1(12) . . . . ?
C6 C1 C2 O3 -175.0(7) . . . . ?
C6 C1 O1 Cu1 10.4(10) . . . . ?
C6 C1 O1 Gd1 165.8(6) . . . . ?
C6 C7 N1 C8 -175.4(9) . . . . ?
C6 C7 N1 Cu1 -0.8(14) . . . . ?
C8 C9 C10 N2 60.7(15) . . . . ?
C9 C8 N1 C7 -146.8(10) . . . . ?
C9 C8 N1 Cu1 38.3(12) . . . . ?
C9 C10 N2 C11 166.9(10) . . . . ?
C9 C10 N2 Cu1 -18.5(14) . . . . ?
C11 C12 C13 C14 177.4(10) . . . . ?
C11 C12 C17 C16 -173.2(8) . . . . ?
C11 C12 C17 O2 7.1(13) . . . . ?
C12 C11 N2 C10 176.1(10) . . . . ?
C12 C11 N2 Cu1 1.7(14) . . . . ?
C12 C13 C14 C15 -3.4(17) . . . . ?
C12 C17 O2 Cu1 -24.3(10) . . . . ?
C12 C17 O2 Gd1 -167.3(6) . . . . ?
C13 C12 C17 C16 3.7(12) . . . . ?
C13 C12 C17 O2 -176.0(8) . . . . ?
C13 C14 C15 C16 2.4(16) . . . . ?
C14 C15 C16 C17 1.7(14) . . . . ?
C14 C15 C16 O4 -176.7(9) . . . . ?
C15 C16 C17 C12 -4.7(12) . . . . ?
C15 C16 C17 O2 175.0(7) . . . . ?
C15 C16 O4 C19B 1.5(13) . . . . ?
C15 C16 O4 Gd1 176.3(7) . . . . ?
C15 C16 O4 C18 -24.1(18) . . . . ?
C16 C17 O2 Cu1 156.0(5) . . . . ?
C16 C17 O2 Gd1 13.0(9) . . . . ?
C17 C12 C13 C14 0.3(15) . . . . ?
C17 C16 O4 C19B -176.9(10) . . . . ?
C17 C16 O4 Gd1 -2.2(8) . . . . ?
C17 C16 O4 C18 157.4(16) . . . . ?
C20 C19B O4 C16 -79(2) . . . . ?
C20 C19B O4 Gd1 106.4(19) . . . . ?
N1 C8 C9 C10 -72.9(14) . . . . ?
N2 C11 C12 C13 -171.7(10) . . . . ?
N2 C11 C12 C17 5.3(16) . . . . ?
O1 C1 C2 C3 -178.5(8) . . . . ?
O1 C1 C2 O3 5.4(10) . . . . ?
O1 C1 C6 C5 178.6(8) . . . . ?
O1 C1 C6 C7 -3.0(13) . . . . ?
O3 C2 C3 C4 175.7(9) . . . . ?
O4 C16 C17 C12 173.9(7) . . . . ?
O4 C16 C17 O2 -6.4(10) . . . . ?
O5 C21 O6 Gd1 -7.5(13) . . . . ?
O5 C21 O6 Gd1 -178.9(6) . . . 3_666 ?
O5 C21 O7 Gd1 178.9(6) . . . 3_666 ?
O6 C21 O5 Cu1 7.3(9) . . . . ?
O6 C21 O7 Gd1 0.2(6) . . . 3_666 ?
O7 C21 O5 Cu1 -171.3(5) . . . . ?
O7 C21 O6 Gd1 171.2(5) . . . . ?
O7 C21 O6 Gd1 -0.2(7) . . . 3_666 ?
O9 N3 O10 Gd1 3.7(9) . . . . ?
O10 N3 O9 Gd1 -3.8(9) . . . . ?
O11 N3 O9 Gd1 174.0(9) . . . . ?
O11 N3 O10 Gd1 -174.1(9) . . . . ?
C23 C18B O3 C2 -103(2) . . . . ?
C23 C18B O3 Gd1 106(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1935710'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh'
;University of Calcutta
India
;
_audit_update_record             
;
2019-08-10 deposited with the CCDC.	2019-09-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-22
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5830)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H52 Cu2 N6 O22 Tb2'
_chemical_formula_sum            'C44 H52 Cu2 N6 O22 Tb2'
_chemical_formula_weight         1461.88
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.1685(14)
_cell_length_b                   12.4034(13)
_cell_length_c                   14.3048(15)
_cell_angle_alpha                90
_cell_angle_beta                 92.458(2)
_cell_angle_gamma                90
_cell_volume                     2511.6(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    23158
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.481
_cell_measurement_theta_min      2.174
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.705
_exptl_absorpt_correction_T_max  0.382
_exptl_absorpt_correction_T_min  0.342
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23158
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.481
_diffrn_reflns_theta_min         2.174
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4534
_reflns_number_total             6295
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.795
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         6295
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0524
_refine_ls_restrained_S_all      1.084
_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)+(0.0805P)²+6.7693P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1647
_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 Tb(H) groups
2. Restrained distances
 C19B-C20
 1.59 with sigma of 0.02
 O8-H8
 0.85 with sigma of 0.01
 Cu1-H8
 2.945074 with sigma of 0.02
 C22-H8
 1.850517 with sigma of 0.02
3. Rigid bond restraints
 C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C20: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C18A \\sim C18B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C19B \\sim C18: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C20) \\sim Ueq: with sigma of 0.06 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O3, C18B, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C19B, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C18A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C18)=
 Sof(H18F)=Sof(H18G)=Sof(H18H)=1-FVAR(1)
 Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(H18E)=FVAR(1)
7.a Riding coordinates:
 C22(H22A,H22B,H22C)
7.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C18B(H18A,H18B), C19B(H19A,H19B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C13(H13), C14(H14), C15(H15)
7.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C18A(H18C,H18D,H18E), C18(H18F,H18G,
 H18H)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7237(5) 0.3264(6) 0.5505(5) 0.0527(15) Uani 1 1 d . . . . .
C2 C 0.6951(6) 0.2843(7) 0.4634(5) 0.0639(19) Uani 1 1 d . . . . .
C3 C 0.7584(7) 0.2541(8) 0.3978(6) 0.083(3) Uani 1 1 d . . . . .
H3 H 0.737339 0.224878 0.340846 0.100 Uiso 1 1 calc R U . . .
C4 C 0.8544(7) 0.2681(11) 0.4183(7) 0.100(3) Uani 1 1 d . . . . .
H4 H 0.898125 0.247316 0.375105 0.119 Uiso 1 1 calc R U . . .
C5 C 0.8839(7) 0.3116(11) 0.5003(7) 0.093(3) Uani 1 1 d . . . . .
H5 H 0.948235 0.321961 0.512571 0.111 Uiso 1 1 calc R U . . .
C6 C 0.8198(6) 0.3422(7) 0.5687(6) 0.068(2) Uani 1 1 d . . . . .
C7 C 0.8602(6) 0.3907(8) 0.6526(6) 0.074(2) Uani 1 1 d . . . . .
H7 H 0.925738 0.395985 0.656494 0.089 Uiso 1 1 calc R U . . .
C8 C 0.8766(7) 0.4796(10) 0.7961(7) 0.095(3) Uani 1 1 d . . . . .
H8A H 0.939898 0.450041 0.794310 0.115 Uiso 1 1 calc R U . . .
H8B H 0.880500 0.555998 0.782364 0.115 Uiso 1 1 calc R U . . .
C9 C 0.8435(8) 0.4665(11) 0.8883(7) 0.097(3) Uani 1 1 d . . . . .
H9A H 0.894630 0.485805 0.932387 0.116 Uiso 1 1 calc R U . . .
H9B H 0.830437 0.390484 0.897396 0.116 Uiso 1 1 calc R U . . .
C10 C 0.7613(9) 0.5259(11) 0.9129(8) 0.111(4) Uani 1 1 d . . . . .
H10A H 0.775390 0.602118 0.907286 0.133 Uiso 1 1 calc R U . . .
H10B H 0.750292 0.511857 0.978196 0.133 Uiso 1 1 calc R U . . .
C11 C 0.5950(7) 0.5383(8) 0.8922(6) 0.079(2) Uani 1 1 d . . . . .
H11 H 0.602150 0.570964 0.950613 0.095 Uiso 1 1 calc R U . . .
C12 C 0.4988(6) 0.5334(8) 0.8531(5) 0.071(2) Uani 1 1 d . . . . .
C13 C 0.4313(8) 0.5915(9) 0.9016(6) 0.089(3) Uani 1 1 d . . . . .
H13 H 0.449045 0.626723 0.956987 0.107 Uiso 1 1 calc R U . . .
C14 C 0.3406(8) 0.5964(10) 0.8683(8) 0.099(3) Uani 1 1 d . . . . .
H14 H 0.295901 0.632294 0.902480 0.119 Uiso 1 1 calc R U . . .
C15 C 0.3134(6) 0.5488(8) 0.7841(7) 0.081(3) Uani 1 1 d . . . . .
H15 H 0.251227 0.554169 0.761060 0.097 Uiso 1 1 calc R U . . .
C16 C 0.3786(5) 0.4935(7) 0.7348(5) 0.0631(18) Uani 1 1 d . . . . .
C17 C 0.4730(6) 0.4821(6) 0.7692(5) 0.0601(18) Uani 1 1 d . . . . .
C18B C 0.567(3) 0.190(3) 0.388(2) 0.077(7) Uani 0.45(2) 1 d . U P A 2
H18A H 0.617616 0.137266 0.383784 0.093 Uiso 0.45(2) 1 calc R U P A 2
H18B H 0.512169 0.154602 0.411574 0.093 Uiso 0.45(2) 1 calc R U P A 2
C19B C 0.267(2) 0.463(2) 0.606(3) 0.076(6) Uani 0.55(2) 1 d D U P A 1
H19A H 0.267815 0.448509 0.539309 0.092 Uiso 0.55(2) 1 calc R U P A 1
H19B H 0.246826 0.536885 0.614408 0.092 Uiso 0.55(2) 1 calc R U P A 1
C20 C 0.1984(17) 0.3855(17) 0.6522(19) 0.111(8) Uani 0.55(2) 1 d D U P A 1
H20A H 0.141075 0.380429 0.614116 0.167 Uiso 0.55(2) 1 calc R U P A 1
H20B H 0.184361 0.412243 0.712983 0.167 Uiso 0.55(2) 1 calc R U P A 1
H20C H 0.226810 0.315439 0.658215 0.167 Uiso 0.55(2) 1 calc R U P A 1
C21 C 0.6212(5) 0.6054(7) 0.5912(5) 0.0614(18) Uani 1 1 d . . . . .
C22 C 0.6270(8) 0.2346(11) 0.8687(8) 0.106(4) Uani 1 1 d D . . . .
H22A H 0.611413 0.159805 0.860461 0.159 Uiso 1 1 d R U . . .
H22B H 0.570283 0.276985 0.863801 0.159 Uiso 1 1 d R U . . .
H22C H 0.657443 0.245145 0.929201 0.159 Uiso 1 1 d R U . . .
Cu1 Cu 0.67442(7) 0.43292(8) 0.73048(6) 0.0606(2) Uani 1 1 d D . . . .
Tb1 Tb 0.49620(2) 0.36163(3) 0.57091(2) 0.05148(14) Uani 1 1 d . . . . .
H8 H 0.734(3) 0.222(4) 0.801(5) 0.077 Uiso 1 1 d D U . . .
N1 N 0.8167(5) 0.4274(6) 0.7226(5) 0.0662(16) Uani 1 1 d . . . . .
N2 N 0.6718(5) 0.5038(6) 0.8576(4) 0.0734(19) Uani 1 1 d . . . . .
N3 N 0.4352(5) 0.1502(6) 0.6363(7) 0.084(2) Uani 1 1 d . . . . .
O1 O 0.6575(3) 0.3503(4) 0.6093(3) 0.0551(11) Uani 1 1 d . . . . .
O2 O 0.5313(3) 0.4215(4) 0.7233(3) 0.0586(12) Uani 1 1 d . . . . .
O3 O 0.5974(4) 0.2798(5) 0.4490(4) 0.0695(14) Uani 1 1 d . . . . .
O4 O 0.3601(4) 0.4485(5) 0.6477(4) 0.0672(14) Uani 1 1 d . . . . .
O5 O 0.6734(4) 0.5858(5) 0.6629(4) 0.0670(13) Uani 1 1 d . . . . .
O6 O 0.5571(4) 0.5379(4) 0.5574(3) 0.0618(13) Uani 1 1 d . . . . .
O7 O 0.6272(4) 0.6917(5) 0.5426(4) 0.0670(14) Uani 1 1 d . . . . .
O8 O 0.6869(4) 0.2661(5) 0.8006(4) 0.0761(16) Uani 1 1 d D . . . .
O9 O 0.5025(5) 0.1629(6) 0.5847(6) 0.099(2) Uani 1 1 d . . . . .
O10 O 0.3981(5) 0.2322(6) 0.6637(5) 0.095(2) Uani 1 1 d . . . . .
O11 O 0.4077(6) 0.0617(6) 0.6577(9) 0.142(4) Uani 1 1 d . . . . .
C23 C 0.546(2) 0.238(2) 0.2979(18) 0.106(10) Uani 0.45(2) 1 d . . P A 2
H23A H 0.539696 0.181878 0.251367 0.160 Uiso 0.45(2) 1 calc R U P A 2
H23B H 0.595222 0.286145 0.282317 0.160 Uiso 0.45(2) 1 calc R U P A 2
H23C H 0.487074 0.276502 0.299795 0.160 Uiso 0.45(2) 1 calc R U P A 2
C18A C 0.556(2) 0.2307(19) 0.3629(16) 0.077(6) Uani 0.55(2) 1 d . U P A 1
H18C H 0.572390 0.273016 0.309832 0.115 Uiso 0.55(2) 1 calc R U P A 1
H18D H 0.488468 0.228217 0.366305 0.115 Uiso 0.55(2) 1 calc R U P A 1
H18E H 0.580003 0.158836 0.356543 0.115 Uiso 0.55(2) 1 calc R U P A 1
C18 C 0.259(3) 0.418(3) 0.616(3) 0.087(8) Uani 0.45(2) 1 d . U P A 2
H18F H 0.239717 0.355604 0.650355 0.130 Uiso 0.45(2) 1 calc R U P A 2
H18G H 0.256120 0.402681 0.550651 0.130 Uiso 0.45(2) 1 calc R U P A 2
H18H H 0.217324 0.477090 0.628838 0.130 Uiso 0.45(2) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.395(10) . ?
C1 C6 1.389(11) . ?
C1 O1 1.320(8) . ?
C2 C3 1.378(11) . ?
C2 O3 1.392(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.388(14) . ?
C4 H4 0.9300 . ?
C4 C5 1.343(15) . ?
C5 H5 0.9300 . ?
C5 C6 1.415(12) . ?
C6 C7 1.439(13) . ?
C7 H7 0.9300 . ?
C7 N1 1.283(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.429(14) . ?
C8 N1 1.472(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.434(15) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 N2 1.491(12) . ?
C11 H11 0.9300 . ?
C11 C12 1.453(13) . ?
C11 N2 1.287(11) . ?
C12 C13 1.404(12) . ?
C12 C17 1.393(11) . ?
C13 H13 0.9300 . ?
C13 C14 1.353(15) . ?
C14 H14 0.9300 . ?
C14 C15 1.380(15) . ?
C15 H15 0.9300 . ?
C15 C16 1.369(11) . ?
C16 C17 1.412(11) . ?
C16 O4 1.380(10) . ?
C17 O2 1.314(9) . ?
C18B H18A 0.9700 . ?
C18B H18B 0.9700 . ?
C18B O3 1.47(3) . ?
C18B C23 1.44(4) . ?
C19B H19A 0.9700 . ?
C19B H19B 0.9700 . ?
C19B C20 1.539(17) . ?
C19B O4 1.43(3) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 Tb1 2.825(8) 3_666 ?
C21 O5 1.262(9) . ?
C21 O6 1.313(9) . ?
C21 O7 1.281(10) . ?
C22 H22A 0.9599 . ?
C22 H22B 0.9599 . ?
C22 H22C 0.9599 . ?
C22 O8 1.376(11) . ?
Cu1 N1 2.025(7) . ?
Cu1 N2 2.022(6) . ?
Cu1 O1 2.019(5) . ?
Cu1 O2 2.031(5) . ?
Cu1 O5 2.128(6) . ?
Cu1 O8 2.303(6) . ?
Tb1 O1 2.332(5) . ?
Tb1 O2 2.335(5) . ?
Tb1 O3 2.518(5) . ?
Tb1 O4 2.503(5) . ?
Tb1 O6 2.361(5) . ?
Tb1 O6 2.318(5) 3_666 ?
Tb1 O7 2.427(5) 3_666 ?
Tb1 O9 2.474(7) . ?
Tb1 O10 2.535(7) . ?
N3 O9 1.240(10) . ?
N3 O10 1.218(10) . ?
N3 O11 1.208(10) . ?
O3 C18A 1.47(2) . ?
O4 C18 1.53(4) . ?
O8 H8 0.860(9) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C18A H18C 0.9600 . ?
C18A H18D 0.9600 . ?
C18A H18E 0.9600 . ?
C18 H18F 0.9600 . ?
C18 H18G 0.9600 . ?
C18 H18H 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 117.7(7) . . ?
O1 C1 C2 117.8(7) . . ?
O1 C1 C6 124.4(7) . . ?
C3 C2 C1 122.5(8) . . ?
C3 C2 O3 124.2(7) . . ?
O3 C2 C1 113.3(6) . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 118.9(9) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0(9) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.8(9) . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C5 119.0(8) . . ?
C1 C6 C7 124.6(8) . . ?
C5 C6 C7 116.4(8) . . ?
C6 C7 H7 116.1 . . ?
N1 C7 C6 127.8(8) . . ?
N1 C7 H7 116.1 . . ?
H8A C8 H8B 107.6 . . ?
C9 C8 H8A 108.8 . . ?
C9 C8 H8B 108.8 . . ?
C9 C8 N1 114.0(9) . . ?
N1 C8 H8A 108.8 . . ?
N1 C8 H8B 108.8 . . ?
C8 C9 H9A 107.8 . . ?
C8 C9 H9B 107.8 . . ?
C8 C9 C10 118.0(11) . . ?
H9A C9 H9B 107.1 . . ?
C10 C9 H9A 107.8 . . ?
C10 C9 H9B 107.8 . . ?
C9 C10 H10A 108.0 . . ?
C9 C10 H10B 108.0 . . ?
C9 C10 N2 117.2(8) . . ?
H10A C10 H10B 107.2 . . ?
N2 C10 H10A 108.0 . . ?
N2 C10 H10B 108.0 . . ?
C12 C11 H11 115.4 . . ?
N2 C11 H11 115.4 . . ?
N2 C11 C12 129.2(7) . . ?
C13 C12 C11 115.9(8) . . ?
C17 C12 C11 123.9(7) . . ?
C17 C12 C13 120.1(9) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.4(9) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 119.6 . . ?
C13 C14 C15 120.9(9) . . ?
C15 C14 H14 119.6 . . ?
C14 C15 H15 120.2 . . ?
C16 C15 C14 119.6(9) . . ?
C16 C15 H15 120.2 . . ?
C15 C16 C17 121.3(8) . . ?
C15 C16 O4 124.2(8) . . ?
O4 C16 C17 114.4(6) . . ?
C12 C17 C16 117.6(7) . . ?
O2 C17 C12 123.0(7) . . ?
O2 C17 C16 119.3(7) . . ?
H18A C18B H18B 108.8 . . ?
O3 C18B H18A 110.7 . . ?
O3 C18B H18B 110.7 . . ?
C23 C18B H18A 110.7 . . ?
C23 C18B H18B 110.7 . . ?
C23 C18B O3 105(2) . . ?
H19A C19B H19B 108.3 . . ?
C20 C19B H19A 109.8 . . ?
C20 C19B H19B 109.8 . . ?
O4 C19B H19A 109.8 . . ?
O4 C19B H19B 109.8 . . ?
O4 C19B C20 109(2) . . ?
C19B C20 H20A 109.5 . . ?
C19B C20 H20B 109.5 . . ?
C19B C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O5 C21 Tb1 177.2(6) . 3_666 ?
O5 C21 O6 123.2(8) . . ?
O5 C21 O7 123.5(7) . . ?
O6 C21 Tb1 54.3(4) . 3_666 ?
O7 C21 Tb1 59.0(4) . 3_666 ?
O7 C21 O6 113.2(7) . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O8 C22 H22A 109.5 . . ?
O8 C22 H22B 109.5 . . ?
O8 C22 H22C 109.5 . . ?
N1 Cu1 O2 171.5(2) . . ?
N1 Cu1 O5 89.6(2) . . ?
N1 Cu1 O8 86.3(2) . . ?
N2 Cu1 N1 97.0(3) . . ?
N2 Cu1 O2 91.1(3) . . ?
N2 Cu1 O5 91.2(3) . . ?
N2 Cu1 O8 90.2(3) . . ?
O1 Cu1 N1 91.0(2) . . ?
O1 Cu1 N2 170.7(3) . . ?
O1 Cu1 O2 80.8(2) . . ?
O1 Cu1 O5 93.7(2) . . ?
O1 Cu1 O8 85.5(2) . . ?
O2 Cu1 O5 93.0(2) . . ?
O2 Cu1 O8 91.0(2) . . ?
O5 Cu1 O8 175.8(2) . . ?
O1 Tb1 O2 68.42(16) . . ?
O1 Tb1 O3 63.73(16) . . ?
O1 Tb1 O4 133.49(17) . . ?
O1 Tb1 O6 73.58(18) . . ?
O1 Tb1 O7 144.28(19) . 3_666 ?
O1 Tb1 O9 83.6(2) . . ?
O1 Tb1 O10 113.1(2) . . ?
O2 Tb1 O3 132.04(17) . . ?
O2 Tb1 O4 65.85(18) . . ?
O2 Tb1 O6 73.64(18) . . ?
O2 Tb1 O7 146.06(19) . 3_666 ?
O2 Tb1 O9 103.7(2) . . ?
O2 Tb1 O10 79.2(2) . . ?
O3 Tb1 O10 116.7(2) . . ?
O4 Tb1 O3 161.69(19) . . ?
O4 Tb1 O10 66.0(2) . . ?
O6 Tb1 O1 120.12(18) 3_666 . ?
O6 Tb1 O2 128.09(19) 3_666 . ?
O6 Tb1 O3 81.0(2) 3_666 . ?
O6 Tb1 O3 95.5(2) . . ?
O6 Tb1 O4 85.90(19) . . ?
O6 Tb1 O4 83.39(19) 3_666 . ?
O6 Tb1 O6 62.9(2) 3_666 . ?
O6 Tb1 O7 116.93(18) . 3_666 ?
O6 Tb1 O7 54.26(18) 3_666 3_666 ?
O6 Tb1 O9 156.5(2) . . ?
O6 Tb1 O9 127.5(2) 3_666 . ?
O6 Tb1 O10 126.0(2) 3_666 . ?
O6 Tb1 O10 147.1(2) . . ?
O7 Tb1 O3 80.89(19) 3_666 . ?
O7 Tb1 O4 82.2(2) 3_666 . ?
O7 Tb1 O9 78.7(2) 3_666 . ?
O7 Tb1 O10 77.4(2) 3_666 . ?
O9 Tb1 O3 68.6(2) . . ?
O9 Tb1 O4 114.8(2) . . ?
O9 Tb1 O10 49.2(2) . . ?
C7 N1 C8 115.6(8) . . ?
C7 N1 Cu1 124.6(6) . . ?
C8 N1 Cu1 119.4(6) . . ?
C10 N2 Cu1 120.5(6) . . ?
C11 N2 C10 116.7(8) . . ?
C11 N2 Cu1 122.6(6) . . ?
O10 N3 O9 116.1(8) . . ?
O11 N3 O9 122.0(9) . . ?
O11 N3 O10 121.9(9) . . ?
C1 O1 Cu1 126.9(5) . . ?
C1 O1 Tb1 125.4(4) . . ?
Cu1 O1 Tb1 104.5(2) . . ?
C17 O2 Cu1 125.6(5) . . ?
C17 O2 Tb1 122.4(5) . . ?
Cu1 O2 Tb1 103.99(19) . . ?
C2 O3 C18B 112.3(16) . . ?
C2 O3 Tb1 118.3(4) . . ?
C2 O3 C18A 119.9(13) . . ?
C18B O3 Tb1 124.0(16) . . ?
C18A O3 Tb1 121.8(12) . . ?
C16 O4 C19B 117.4(16) . . ?
C16 O4 Tb1 116.8(4) . . ?
C16 O4 C18 120.1(19) . . ?
C19B O4 Tb1 125.6(15) . . ?
C18 O4 Tb1 119.7(18) . . ?
C21 O5 Cu1 122.3(5) . . ?
C21 O6 Tb1 98.4(5) . 3_666 ?
C21 O6 Tb1 144.1(5) . . ?
Tb1 O6 Tb1 117.1(2) 3_666 . ?
C21 O7 Tb1 94.2(4) . 3_666 ?
C22 O8 Cu1 121.7(6) . . ?
C22 O8 H8 107.9(18) . . ?
Cu1 O8 H8 128.7(18) . . ?
N3 O9 Tb1 98.5(6) . . ?
N3 O10 Tb1 96.1(5) . . ?
C18B C23 H23A 109.5 . . ?
C18B C23 H23B 109.5 . . ?
C18B C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O3 C18A H18C 109.5 . . ?
O3 C18A H18D 109.5 . . ?
O3 C18A H18E 109.5 . . ?
H18C C18A H18D 109.5 . . ?
H18C C18A H18E 109.5 . . ?
H18D C18A H18E 109.5 . . ?
O4 C18 H18F 109.5 . . ?
O4 C18 H18G 109.5 . . ?
O4 C18 H18H 109.5 . . ?
H18F C18 H18G 109.5 . . ?
H18F C18 H18H 109.5 . . ?
H18G C18 H18H 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
C1 C2 C3 C4 -1.3(15) . . . . ?
C1 C2 O3 C18B -149.4(14) . . . . ?
C1 C2 O3 Tb1 5.6(9) . . . . ?
C1 C2 O3 C18A -176.0(12) . . . . ?
C1 C6 C7 N1 -0.6(16) . . . . ?
C2 C1 C6 C5 -2.2(12) . . . . ?
C2 C1 C6 C7 176.2(8) . . . . ?
C2 C1 O1 Cu1 -169.7(5) . . . . ?
C2 C1 O1 Tb1 -13.3(9) . . . . ?
C2 C3 C4 C5 -0.8(18) . . . . ?
C3 C2 O3 C18B 32.8(17) . . . . ?
C3 C2 O3 Tb1 -172.2(7) . . . . ?
C3 C2 O3 C18A 6.3(16) . . . . ?
C3 C4 C5 C6 1.4(19) . . . . ?
C4 C5 C6 C1 0.2(17) . . . . ?
C4 C5 C6 C7 -178.3(11) . . . . ?
C5 C6 C7 N1 177.9(10) . . . . ?
C6 C1 C2 C3 2.8(12) . . . . ?
C6 C1 C2 O3 -175.0(7) . . . . ?
C6 C1 O1 Cu1 9.2(10) . . . . ?
C6 C1 O1 Tb1 165.5(6) . . . . ?
C6 C7 N1 C8 -175.9(9) . . . . ?
C6 C7 N1 Cu1 -3.1(14) . . . . ?
C8 C9 C10 N2 61.3(17) . . . . ?
C9 C8 N1 C7 -147.3(10) . . . . ?
C9 C8 N1 Cu1 39.5(13) . . . . ?
C9 C10 N2 C11 165.0(11) . . . . ?
C9 C10 N2 Cu1 -19.4(15) . . . . ?
C11 C12 C13 C14 176.8(10) . . . . ?
C11 C12 C17 C16 -173.4(8) . . . . ?
C11 C12 C17 O2 8.8(14) . . . . ?
C12 C11 N2 C10 176.9(10) . . . . ?
C12 C11 N2 Cu1 1.4(15) . . . . ?
C12 C13 C14 C15 -2.9(18) . . . . ?
C12 C17 O2 Cu1 -25.0(10) . . . . ?
C12 C17 O2 Tb1 -168.7(6) . . . . ?
C13 C12 C17 C16 1.8(13) . . . . ?
C13 C12 C17 O2 -176.0(8) . . . . ?
C13 C14 C15 C16 1.6(17) . . . . ?
C14 C15 C16 C17 1.4(14) . . . . ?
C14 C15 C16 O4 -176.1(9) . . . . ?
C15 C16 C17 C12 -3.1(12) . . . . ?
C15 C16 C17 O2 174.8(8) . . . . ?
C15 C16 O4 C19B 1.4(14) . . . . ?
C15 C16 O4 Tb1 176.6(7) . . . . ?
C15 C16 O4 C18 -24(2) . . . . ?
C16 C17 O2 Cu1 157.3(5) . . . . ?
C16 C17 O2 Tb1 13.5(9) . . . . ?
C17 C12 C13 C14 1.2(16) . . . . ?
C17 C16 O4 C19B -176.2(11) . . . . ?
C17 C16 O4 Tb1 -1.1(8) . . . . ?
C17 C16 O4 C18 158.1(18) . . . . ?
C20 C19B O4 C16 -77(2) . . . . ?
C20 C19B O4 Tb1 108(2) . . . . ?
Tb1 C21 O6 Tb1 170.9(9) 3_666 . . . ?
N1 C8 C9 C10 -72.7(14) . . . . ?
N2 C11 C12 C13 -171.4(10) . . . . ?
N2 C11 C12 C17 4.0(16) . . . . ?
O1 C1 C2 C3 -178.3(8) . . . . ?
O1 C1 C2 O3 3.9(10) . . . . ?
O1 C1 C6 C5 178.9(8) . . . . ?
O1 C1 C6 C7 -2.6(13) . . . . ?
O3 C2 C3 C4 176.2(10) . . . . ?
O4 C16 C17 C12 174.7(7) . . . . ?
O4 C16 C17 O2 -7.5(10) . . . . ?
O5 C21 O6 Tb1 -7.5(14) . . . . ?
O5 C21 O6 Tb1 -178.4(7) . . . 3_666 ?
O5 C21 O7 Tb1 178.4(7) . . . 3_666 ?
O6 C21 O5 Cu1 6.7(10) . . . . ?
O6 C21 O7 Tb1 0.2(7) . . . 3_666 ?
O7 C21 O5 Cu1 -171.3(6) . . . . ?
O7 C21 O6 Tb1 170.7(6) . . . . ?
O7 C21 O6 Tb1 -0.2(7) . . . 3_666 ?
O9 N3 O10 Tb1 4.1(10) . . . . ?
O10 N3 O9 Tb1 -4.2(10) . . . . ?
O11 N3 O9 Tb1 175.3(10) . . . . ?
O11 N3 O10 Tb1 -175.4(10) . . . . ?
C23 C18B O3 C2 -102(2) . . . . ?
C23 C18B O3 Tb1 104(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1935709'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh'
;University of Calcutta
India
;
_audit_update_record             
;
2019-08-10 deposited with the CCDC.	2019-09-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-22
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5830)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H52 Cu2 Dy2 N6 O22'
_chemical_formula_sum            'C44 H52 Cu2 Dy2 N6 O22'
_chemical_formula_weight         1469.02
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.1416(8)
_cell_length_b                   12.3829(7)
_cell_length_c                   14.3320(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.0800(10)
_cell_angle_gamma                90
_cell_volume                     2508.1(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    39641
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.963
_cell_measurement_theta_min      2.580
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.870
_exptl_absorpt_correction_T_max  0.230
_exptl_absorpt_correction_T_min  0.184
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.38
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39641
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.963
_diffrn_reflns_theta_min         2.580
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3800
_reflns_number_total             5392
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         1.714
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5392
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0663
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0592P)²+19.4051P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1693
_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 Dy(H) groups
2. Restrained distances
 C19B-C20
 1.59 with sigma of 0.02
 O8-H8
 0.85 with sigma of 0.01
 Cu1-H8
 2.945074 with sigma of 0.02
 C22-H8
 1.850517 with sigma of 0.02
3. Rigid bond restraints
 C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C20: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C18A \\sim C18B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C19B \\sim C18: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C20) \\sim Ueq: with sigma of 0.06 and sigma for terminal atoms of 0.12
5. Rigid body (RIGU) restrains
 O3, C18B, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C19B, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C18A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C18)=
 Sof(H18F)=Sof(H18G)=Sof(H18H)=1-FVAR(1)
 Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(H18E)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C18B(H18A,H18B), C19B(H19A,H19B)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C13(H13), C14(H14), C15(H15)
7.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C18A(H18C,H18D,
 H18E), C18(H18F,H18G,H18H)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7233(7) 0.3260(8) 0.5509(7) 0.054(2) Uani 1 1 d . . . . .
C2 C 0.6946(8) 0.2830(10) 0.4641(7) 0.066(3) Uani 1 1 d . . . . .
C3 C 0.7588(9) 0.2529(11) 0.3979(9) 0.084(4) Uani 1 1 d . . . . .
H3 H 0.738026 0.223759 0.341003 0.100 Uiso 1 1 calc R U . . .
C4 C 0.8535(10) 0.2670(14) 0.4182(11) 0.104(5) Uani 1 1 d . . . . .
H4 H 0.897392 0.247419 0.374565 0.124 Uiso 1 1 calc R U . . .
C5 C 0.8836(9) 0.3092(14) 0.5011(10) 0.096(4) Uani 1 1 d . . . . .
H5 H 0.948189 0.317482 0.513761 0.115 Uiso 1 1 calc R U . . .
C6 C 0.8194(8) 0.3406(10) 0.5682(8) 0.068(3) Uani 1 1 d . . . . .
C7 C 0.8589(8) 0.3878(11) 0.6524(9) 0.076(3) Uani 1 1 d . . . . .
H7 H 0.924660 0.390635 0.657016 0.092 Uiso 1 1 calc R U . . .
C8 C 0.8751(10) 0.4772(15) 0.7973(10) 0.104(5) Uani 1 1 d . . . . .
H8A H 0.937587 0.445025 0.796970 0.125 Uiso 1 1 calc R U . . .
H8B H 0.881944 0.553306 0.782997 0.125 Uiso 1 1 calc R U . . .
C9 C 0.8412(11) 0.4680(16) 0.8872(10) 0.107(5) Uani 1 1 d . . . . .
H9A H 0.892233 0.489204 0.930351 0.129 Uiso 1 1 calc R U . . .
H9B H 0.829329 0.391977 0.898009 0.129 Uiso 1 1 calc R U . . .
C10 C 0.7591(11) 0.5252(15) 0.9131(10) 0.111(5) Uani 1 1 d . . . . .
H10A H 0.772751 0.601838 0.909799 0.133 Uiso 1 1 calc R U . . .
H10B H 0.747774 0.508426 0.977877 0.133 Uiso 1 1 calc R U . . .
C11 C 0.5932(10) 0.5381(11) 0.8916(8) 0.079(3) Uani 1 1 d . . . . .
H11 H 0.599838 0.569427 0.950429 0.095 Uiso 1 1 calc R U . . .
C12 C 0.4972(9) 0.5347(10) 0.8523(7) 0.072(3) Uani 1 1 d . . . . .
C13 C 0.4290(11) 0.5931(13) 0.9001(9) 0.092(4) Uani 1 1 d . . . . .
H13 H 0.446891 0.629088 0.954897 0.110 Uiso 1 1 calc R U . . .
C14 C 0.3374(11) 0.5984(13) 0.8681(10) 0.098(5) Uani 1 1 d . . . . .
H14 H 0.292454 0.633886 0.902612 0.117 Uiso 1 1 calc R U . . .
C15 C 0.3119(9) 0.5506(11) 0.7841(9) 0.084(4) Uani 1 1 d . . . . .
H15 H 0.249766 0.556060 0.761089 0.101 Uiso 1 1 calc R U . . .
C16 C 0.3771(7) 0.4948(9) 0.7337(8) 0.064(3) Uani 1 1 d . . . . .
C17 C 0.4713(7) 0.4827(9) 0.7688(7) 0.058(3) Uani 1 1 d . . . . .
C18B C 0.569(4) 0.181(4) 0.386(3) 0.081(9) Uani 0.44(2) 1 d . U P A 2
H18A H 0.621033 0.130038 0.382784 0.097 Uiso 0.44(2) 1 calc R U P A 2
H18B H 0.513808 0.144648 0.408340 0.097 Uiso 0.44(2) 1 calc R U P A 2
C19B C 0.263(2) 0.467(3) 0.606(3) 0.076(8) Uani 0.56(2) 1 d D U P A 1
H19A H 0.262856 0.455877 0.538648 0.091 Uiso 0.56(2) 1 calc R U P A 1
H19B H 0.241975 0.540047 0.617701 0.091 Uiso 0.56(2) 1 calc R U P A 1
C20 C 0.197(2) 0.384(2) 0.652(3) 0.132(14) Uani 0.56(2) 1 d D U P A 1
H20A H 0.139747 0.376401 0.614034 0.199 Uiso 0.56(2) 1 calc R U P A 1
H20B H 0.181651 0.409009 0.712815 0.199 Uiso 0.56(2) 1 calc R U P A 1
H20C H 0.228269 0.315465 0.656872 0.199 Uiso 0.56(2) 1 calc R U P A 1
C21 C 0.6208(7) 0.6070(10) 0.5896(7) 0.062(3) Uani 1 1 d . . . . .
C22 C 0.6263(11) 0.2288(17) 0.8701(11) 0.124(6) Uani 1 1 d D . . . .
H22A H 0.565777 0.210681 0.841882 0.186 Uiso 1 1 calc R U . . .
H22B H 0.618775 0.285495 0.914881 0.186 Uiso 1 1 calc R U . . .
H22C H 0.652872 0.166323 0.900860 0.186 Uiso 1 1 calc R U . . .
Cu1 Cu 0.67354(9) 0.43325(11) 0.73007(8) 0.0601(3) Uani 1 1 d D . . . .
Dy1 Dy 0.49594(3) 0.36230(4) 0.57127(3) 0.05279(18) Uani 1 1 d . . . . .
H8 H 0.735(3) 0.222(4) 0.803(6) 0.079 Uiso 1 1 d D U . . .
N1 N 0.8158(6) 0.4267(8) 0.7221(7) 0.067(2) Uani 1 1 d . . . . .
N2 N 0.6697(7) 0.5043(8) 0.8573(6) 0.073(3) Uani 1 1 d . . . . .
N3 N 0.4370(7) 0.1514(10) 0.6390(9) 0.084(3) Uani 1 1 d . . . . .
O1 O 0.6570(4) 0.3497(5) 0.6097(4) 0.0536(16) Uani 1 1 d . . . . .
O2 O 0.5300(5) 0.4223(6) 0.7224(5) 0.0606(17) Uani 1 1 d . . . . .
O3 O 0.5971(5) 0.2803(7) 0.4490(5) 0.072(2) Uani 1 1 d . . . . .
O4 O 0.3592(5) 0.4495(7) 0.6474(5) 0.0677(19) Uani 1 1 d . . . . .
O5 O 0.6726(5) 0.5870(7) 0.6616(5) 0.069(2) Uani 1 1 d . . . . .
O6 O 0.5572(5) 0.5385(6) 0.5565(5) 0.0615(18) Uani 1 1 d . . . . .
O7 O 0.6259(5) 0.6922(6) 0.5397(5) 0.0676(19) Uani 1 1 d . . . . .
O8 O 0.6863(6) 0.2632(8) 0.8017(6) 0.086(2) Uani 1 1 d D . . . .
O9 O 0.5047(6) 0.1646(8) 0.5870(8) 0.102(3) Uani 1 1 d . . . . .
O10 O 0.3990(7) 0.2336(8) 0.6653(7) 0.093(3) Uani 1 1 d . . . . .
O11 O 0.4096(7) 0.0611(9) 0.6595(11) 0.148(6) Uani 1 1 d . . . . .
C23 C 0.550(3) 0.233(3) 0.299(3) 0.107(13) Uani 0.44(2) 1 d . . P A 2
H23A H 0.544238 0.179116 0.250988 0.161 Uiso 0.44(2) 1 calc R U P A 2
H23B H 0.601522 0.280610 0.285967 0.161 Uiso 0.44(2) 1 calc R U P A 2
H23C H 0.492643 0.273051 0.301954 0.161 Uiso 0.44(2) 1 calc R U P A 2
C18A C 0.556(3) 0.231(2) 0.366(2) 0.075(8) Uani 0.56(2) 1 d . U P A 1
H18C H 0.569894 0.273730 0.312963 0.112 Uiso 0.56(2) 1 calc R U P A 1
H18D H 0.489092 0.224872 0.371991 0.112 Uiso 0.56(2) 1 calc R U P A 1
H18E H 0.582833 0.159770 0.359329 0.112 Uiso 0.56(2) 1 calc R U P A 1
C18 C 0.260(3) 0.418(4) 0.619(4) 0.083(10) Uani 0.44(2) 1 d . U P A 2
H18F H 0.239581 0.359898 0.658254 0.125 Uiso 0.44(2) 1 calc R U P A 2
H18G H 0.257871 0.394014 0.555128 0.125 Uiso 0.44(2) 1 calc R U P A 2
H18H H 0.218647 0.478536 0.625387 0.125 Uiso 0.44(2) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.400(15) . ?
C1 C6 1.385(14) . ?
C1 O1 1.316(11) . ?
C2 C3 1.387(15) . ?
C2 O3 1.387(13) . ?
C3 H3 0.9300 . ?
C3 C4 1.371(19) . ?
C4 H4 0.9300 . ?
C4 C5 1.35(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.402(16) . ?
C6 C7 1.436(17) . ?
C7 H7 0.9300 . ?
C7 N1 1.284(15) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.395(19) . ?
C8 N1 1.479(14) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.42(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 N2 1.493(16) . ?
C11 H11 0.9300 . ?
C11 C12 1.451(17) . ?
C11 N2 1.276(15) . ?
C12 C13 1.403(16) . ?
C12 C17 1.397(16) . ?
C13 H13 0.9300 . ?
C13 C14 1.36(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.38(2) . ?
C15 H15 0.9300 . ?
C15 C16 1.377(15) . ?
C16 C17 1.415(14) . ?
C16 O4 1.374(13) . ?
C17 O2 1.315(12) . ?
C18B H18A 0.9700 . ?
C18B H18B 0.9700 . ?
C18B O3 1.56(4) . ?
C18B C23 1.42(6) . ?
C19B H19A 0.9700 . ?
C19B H19B 0.9700 . ?
C19B C20 1.553(18) . ?
C19B O4 1.48(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 Dy1 2.813(10) 3_666 ?
C21 O5 1.268(12) . ?
C21 O6 1.312(12) . ?
C21 O7 1.279(13) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C22 O8 1.387(16) . ?
Cu1 N1 2.021(9) . ?
Cu1 N2 2.028(9) . ?
Cu1 O1 2.018(6) . ?
Cu1 O2 2.034(7) . ?
Cu1 O5 2.141(8) . ?
Cu1 O8 2.346(9) . ?
Dy1 O1 2.330(6) . ?
Dy1 O2 2.324(7) . ?
Dy1 O3 2.516(7) . ?
Dy1 O4 2.499(7) . ?
Dy1 O6 2.308(7) 3_666 ?
Dy1 O6 2.360(7) . ?
Dy1 O7 2.399(7) 3_666 ?
Dy1 O9 2.461(10) . ?
Dy1 O10 2.524(8) . ?
N3 O9 1.245(13) . ?
N3 O10 1.218(13) . ?
N3 O11 1.223(13) . ?
O3 C18A 1.44(3) . ?
O4 C18 1.50(5) . ?
O8 H8 0.855(10) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C18A H18C 0.9600 . ?
C18A H18D 0.9600 . ?
C18A H18E 0.9600 . ?
C18 H18F 0.9600 . ?
C18 H18G 0.9600 . ?
C18 H18H 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 117.4(9) . . ?
O1 C1 C2 117.6(9) . . ?
O1 C1 C6 125.0(10) . . ?
C3 C2 C1 122.2(11) . . ?
C3 C2 O3 124.0(10) . . ?
O3 C2 C1 113.7(9) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 C2 118.6(12) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.7(12) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.2(12) . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 119.8(11) . . ?
C1 C6 C7 123.6(10) . . ?
C5 C6 C7 116.6(11) . . ?
C6 C7 H7 115.6 . . ?
N1 C7 C6 128.7(10) . . ?
N1 C7 H7 115.6 . . ?
H8A C8 H8B 107.4 . . ?
C9 C8 H8A 108.4 . . ?
C9 C8 H8B 108.4 . . ?
C9 C8 N1 115.7(13) . . ?
N1 C8 H8A 108.4 . . ?
N1 C8 H8B 108.4 . . ?
C8 C9 H9A 107.1 . . ?
C8 C9 H9B 107.1 . . ?
C8 C9 C10 120.8(15) . . ?
H9A C9 H9B 106.8 . . ?
C10 C9 H9A 107.1 . . ?
C10 C9 H9B 107.1 . . ?
C9 C10 H10A 108.0 . . ?
C9 C10 H10B 108.0 . . ?
C9 C10 N2 117.2(12) . . ?
H10A C10 H10B 107.2 . . ?
N2 C10 H10A 108.0 . . ?
N2 C10 H10B 108.0 . . ?
C12 C11 H11 115.2 . . ?
N2 C11 H11 115.2 . . ?
N2 C11 C12 129.6(10) . . ?
C13 C12 C11 116.5(12) . . ?
C17 C12 C11 123.9(10) . . ?
C17 C12 C13 119.5(12) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 C12 121.6(13) . . ?
C14 C13 H13 119.2 . . ?
C13 C14 H14 120.3 . . ?
C13 C14 C15 119.3(12) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.0(12) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C17 120.4(12) . . ?
O4 C16 C15 124.9(11) . . ?
O4 C16 C17 114.6(9) . . ?
C12 C17 C16 118.0(10) . . ?
O2 C17 C12 123.0(10) . . ?
O2 C17 C16 119.0(10) . . ?
H18A C18B H18B 109.4 . . ?
O3 C18B H18A 111.6 . . ?
O3 C18B H18B 111.6 . . ?
C23 C18B H18A 111.6 . . ?
C23 C18B H18B 111.6 . . ?
C23 C18B O3 101(3) . . ?
H19A C19B H19B 108.6 . . ?
C20 C19B H19A 110.3 . . ?
C20 C19B H19B 110.4 . . ?
O4 C19B H19A 110.3 . . ?
O4 C19B H19B 110.4 . . ?
O4 C19B C20 107(2) . . ?
C19B C20 H20A 109.5 . . ?
C19B C20 H20B 109.5 . . ?
C19B C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O5 C21 Dy1 176.5(9) . 3_666 ?
O5 C21 O6 122.4(11) . . ?
O5 C21 O7 125.0(10) . . ?
O6 C21 Dy1 54.3(5) . 3_666 ?
O7 C21 Dy1 58.2(5) . 3_666 ?
O7 C21 O6 112.5(9) . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O8 C22 H22A 109.5 . . ?
O8 C22 H22B 109.5 . . ?
O8 C22 H22C 109.5 . . ?
N1 Cu1 N2 97.3(4) . . ?
N1 Cu1 O2 171.2(3) . . ?
N1 Cu1 O5 90.0(3) . . ?
N1 Cu1 O8 85.8(3) . . ?
N2 Cu1 O2 91.1(4) . . ?
N2 Cu1 O5 91.5(4) . . ?
N2 Cu1 O8 90.0(4) . . ?
O1 Cu1 N1 90.9(3) . . ?
O1 Cu1 N2 170.3(4) . . ?
O1 Cu1 O2 80.5(3) . . ?
O1 Cu1 O5 93.7(3) . . ?
O1 Cu1 O8 85.4(3) . . ?
O2 Cu1 O5 92.6(3) . . ?
O2 Cu1 O8 91.4(3) . . ?
O5 Cu1 O8 175.7(3) . . ?
O1 Dy1 O3 64.0(2) . . ?
O1 Dy1 O4 133.7(2) . . ?
O1 Dy1 O6 74.0(2) . . ?
O1 Dy1 O7 144.2(2) . 3_666 ?
O1 Dy1 O9 82.3(3) . . ?
O1 Dy1 O10 112.2(3) . . ?
O2 Dy1 O1 68.5(2) . . ?
O2 Dy1 O3 132.4(2) . . ?
O2 Dy1 O4 65.9(2) . . ?
O2 Dy1 O6 74.0(2) . . ?
O2 Dy1 O7 145.8(3) . 3_666 ?
O2 Dy1 O9 103.0(3) . . ?
O2 Dy1 O10 78.6(3) . . ?
O3 Dy1 O10 116.8(3) . . ?
O4 Dy1 O3 161.2(2) . . ?
O4 Dy1 O10 66.2(3) . . ?
O6 Dy1 O1 120.7(2) 3_666 . ?
O6 Dy1 O2 128.3(3) 3_666 . ?
O6 Dy1 O3 95.2(3) . . ?
O6 Dy1 O3 80.8(3) 3_666 . ?
O6 Dy1 O4 86.1(3) . . ?
O6 Dy1 O4 83.2(3) 3_666 . ?
O6 Dy1 O6 63.1(3) 3_666 . ?
O6 Dy1 O7 117.3(2) . 3_666 ?
O6 Dy1 O7 54.4(2) 3_666 3_666 ?
O6 Dy1 O9 155.6(3) . . ?
O6 Dy1 O9 128.0(3) 3_666 . ?
O6 Dy1 O10 147.1(3) . . ?
O6 Dy1 O10 126.3(3) 3_666 . ?
O7 Dy1 O3 80.7(3) 3_666 . ?
O7 Dy1 O4 82.1(3) 3_666 . ?
O7 Dy1 O9 79.2(3) 3_666 . ?
O7 Dy1 O10 77.6(3) 3_666 . ?
O9 Dy1 O3 68.6(3) . . ?
O9 Dy1 O4 115.3(3) . . ?
O9 Dy1 O10 49.4(3) . . ?
C7 N1 C8 116.9(10) . . ?
C7 N1 Cu1 124.1(7) . . ?
C8 N1 Cu1 118.8(9) . . ?
C10 N2 Cu1 120.5(9) . . ?
C11 N2 C10 116.8(10) . . ?
C11 N2 Cu1 122.6(8) . . ?
O10 N3 O9 115.7(11) . . ?
O10 N3 O11 122.8(12) . . ?
O11 N3 O9 121.5(13) . . ?
C1 O1 Cu1 126.8(6) . . ?
C1 O1 Dy1 125.2(6) . . ?
Cu1 O1 Dy1 104.4(3) . . ?
C17 O2 Cu1 125.6(7) . . ?
C17 O2 Dy1 122.7(6) . . ?
Cu1 O2 Dy1 104.1(3) . . ?
C2 O3 C18B 110(2) . . ?
C2 O3 Dy1 118.0(6) . . ?
C2 O3 C18A 120.3(17) . . ?
C18B O3 Dy1 125(2) . . ?
C18A O3 Dy1 121.7(16) . . ?
C16 O4 C19B 116.1(19) . . ?
C16 O4 Dy1 116.7(6) . . ?
C16 O4 C18 119(2) . . ?
C19B O4 Dy1 126.9(18) . . ?
C18 O4 Dy1 120(2) . . ?
C21 O5 Cu1 122.7(7) . . ?
C21 O6 Dy1 98.2(6) . 3_666 ?
C21 O6 Dy1 144.5(7) . . ?
Dy1 O6 Dy1 116.9(3) 3_666 . ?
C21 O7 Dy1 94.9(6) . 3_666 ?
C22 O8 Cu1 123.1(9) . . ?
C22 O8 H8 108(2) . . ?
Cu1 O8 H8 126(2) . . ?
N3 O9 Dy1 98.6(8) . . ?
N3 O10 Dy1 96.2(7) . . ?
C18B C23 H23A 109.5 . . ?
C18B C23 H23B 109.5 . . ?
C18B C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O3 C18A H18C 109.5 . . ?
O3 C18A H18D 109.5 . . ?
O3 C18A H18E 109.5 . . ?
H18C C18A H18D 109.5 . . ?
H18C C18A H18E 109.5 . . ?
H18D C18A H18E 109.5 . . ?
O4 C18 H18F 109.5 . . ?
O4 C18 H18G 109.5 . . ?
O4 C18 H18H 109.5 . . ?
H18F C18 H18G 109.5 . . ?
H18F C18 H18H 109.5 . . ?
H18G C18 H18H 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
C1 C2 C3 C4 -1(2) . . . . ?
C1 C2 O3 C18B -148(2) . . . . ?
C1 C2 O3 Dy1 4.1(12) . . . . ?
C1 C2 O3 C18A -175.0(17) . . . . ?
C1 C6 C7 N1 -3(2) . . . . ?
C2 C1 C6 C5 -2.2(17) . . . . ?
C2 C1 C6 C7 177.4(11) . . . . ?
C2 C1 O1 Cu1 -169.7(7) . . . . ?
C2 C1 O1 Dy1 -14.2(12) . . . . ?
C2 C3 C4 C5 0(2) . . . . ?
C3 C2 O3 C18B 36(2) . . . . ?
C3 C2 O3 Dy1 -171.9(10) . . . . ?
C3 C2 O3 C18A 9(2) . . . . ?
C3 C4 C5 C6 -1(3) . . . . ?
C4 C5 C6 C1 2(2) . . . . ?
C4 C5 C6 C7 -177.9(15) . . . . ?
C5 C6 C7 N1 177.0(14) . . . . ?
C6 C1 C2 C3 1.7(17) . . . . ?
C6 C1 C2 O3 -174.3(10) . . . . ?
C6 C1 O1 Cu1 10.1(14) . . . . ?
C6 C1 O1 Dy1 165.5(8) . . . . ?
C6 C7 N1 C8 -176.0(13) . . . . ?
C6 C7 N1 Cu1 -1.0(19) . . . . ?
C8 C9 C10 N2 58(2) . . . . ?
C9 C8 N1 C7 -148.0(15) . . . . ?
C9 C8 N1 Cu1 36.7(19) . . . . ?
C9 C10 N2 C11 166.2(15) . . . . ?
C9 C10 N2 Cu1 -17(2) . . . . ?
C11 C12 C13 C14 178.0(14) . . . . ?
C11 C12 C17 C16 -173.8(11) . . . . ?
C11 C12 C17 O2 7.1(18) . . . . ?
C12 C11 N2 C10 176.6(14) . . . . ?
C12 C11 N2 Cu1 0(2) . . . . ?
C12 C13 C14 C15 -4(2) . . . . ?
C12 C17 O2 Cu1 -23.8(14) . . . . ?
C12 C17 O2 Dy1 -168.4(8) . . . . ?
C13 C12 C17 C16 2.5(17) . . . . ?
C13 C12 C17 O2 -176.7(11) . . . . ?
C13 C14 C15 C16 2(2) . . . . ?
C14 C15 C16 C17 2.0(19) . . . . ?
C14 C15 C16 O4 -176.5(12) . . . . ?
C15 C16 C17 C12 -4.2(16) . . . . ?
C15 C16 C17 O2 175.0(10) . . . . ?
C15 C16 O4 C19B 2.5(18) . . . . ?
C15 C16 O4 Dy1 176.8(9) . . . . ?
C15 C16 O4 C18 -25(2) . . . . ?
C16 C17 O2 Cu1 157.1(7) . . . . ?
C16 C17 O2 Dy1 12.5(12) . . . . ?
C17 C12 C13 C14 2(2) . . . . ?
C17 C16 O4 C19B -176.0(13) . . . . ?
C17 C16 O4 Dy1 -1.8(11) . . . . ?
C17 C16 O4 C18 156(2) . . . . ?
C20 C19B O4 C16 -80(3) . . . . ?
C20 C19B O4 Dy1 106(2) . . . . ?
Dy1 C21 O6 Dy1 171.7(12) 3_666 . . . ?
N1 C8 C9 C10 -70(2) . . . . ?
N2 C11 C12 C13 -170.5(14) . . . . ?
N2 C11 C12 C17 6(2) . . . . ?
O1 C1 C2 C3 -178.5(11) . . . . ?
O1 C1 C2 O3 5.5(14) . . . . ?
O1 C1 C6 C5 178.1(11) . . . . ?
O1 C1 C6 C7 -2.3(18) . . . . ?
O3 C2 C3 C4 174.9(13) . . . . ?
O4 C16 C17 C12 174.5(9) . . . . ?
O4 C16 C17 O2 -6.4(14) . . . . ?
O5 C21 O6 Dy1 -178.5(9) . . . 3_666 ?
O5 C21 O6 Dy1 -6.8(18) . . . . ?
O5 C21 O7 Dy1 178.4(10) . . . 3_666 ?
O6 C21 O5 Cu1 6.6(14) . . . . ?
O6 C21 O7 Dy1 0.6(9) . . . 3_666 ?
O7 C21 O5 Cu1 -171.0(8) . . . . ?
O7 C21 O6 Dy1 -0.6(9) . . . 3_666 ?
O7 C21 O6 Dy1 171.1(8) . . . . ?
O9 N3 O10 Dy1 4.0(13) . . . . ?
O10 N3 O9 Dy1 -4.1(13) . . . . ?
O11 N3 O9 Dy1 173.8(12) . . . . ?
O11 N3 O10 Dy1 -173.9(13) . . . . ?
C23 C18B O3 C2 -104(3) . . . . ?
C23 C18B O3 Dy1 107(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
