# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_gac321_sq
_database_code_depnum_ccdc_archive 'CCDC 1966328'
loop_
_audit_author_name
_audit_author_address
'Gavin Craig'
;University of Strathclyde
United Kingdom
;
_audit_update_record             
;
2019-11-18 deposited with the CCDC.	2020-02-24 downloaded from the CCDC.
;
_audit_creation_date             2019-10-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3

# start Validation Reply Form
_vrf_PLAT420_gac321_sq           
;
PROBLEM: D-H without acceptor
RESPONSE: Due to the MeOH molecule coordinated to the external axial 
site of the Cu paddlewheel - disordered solvents have been removed using
SQUEEZE.
;

# end Validation Reply Form

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C116 H94 Cu4 N2 O24'
_chemical_formula_sum            'C134 H136 Cu4 N8 O30'
_chemical_formula_weight         2592.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cu4 C112 H80 O28 N2'
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'

_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           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   15.2966(4)
_cell_length_b                   17.7385(3)
_cell_length_c                   24.6648(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.051(2)
_cell_angle_gamma                90
_cell_volume                     6666.5(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    35516
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.3350
_cell_measurement_theta_min      1.9800
_shelx_estimated_absorpt_T_max   0.966
_shelx_estimated_absorpt_T_min   0.816
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0292
_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       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            84020
_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         25.681
_diffrn_reflns_theta_min         1.896
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -85.00  93.00   0.50   16.00    --    4.00  45.00 120.00  356
  2  ω    -28.00   2.00   0.50   16.00    --  -16.40  45.00 -18.65   60
  3  ω      6.00  72.00   0.50   16.00    --  -16.40  45.00 -18.65  132
  4  ω    -33.00  73.00   0.50   16.00    --  -16.40  45.00  60.00  212
  5  ω   -105.00  72.00   0.50   16.00    --  -16.40  45.00  30.00  354
  6  ω    -88.00 -59.00   0.50   16.00    --  -16.40  45.00 -18.65   58
  7  ω    -12.00  16.00   0.50   16.00    --  -16.40  45.00 153.56   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0099989000
_diffrn_orient_matrix_UB_12      -0.0078115000
_diffrn_orient_matrix_UB_13      -0.0269757000
_diffrn_orient_matrix_UB_21      0.0012450000
_diffrn_orient_matrix_UB_22      0.0391950000
_diffrn_orient_matrix_UB_23      -0.0055251000
_diffrn_orient_matrix_UB_31      0.0454734000
_diffrn_orient_matrix_UB_32      0.0005538000
_diffrn_orient_matrix_UB_33      0.0086524000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9661
_reflns_number_total             12664
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         12664
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0541
_refine_ls_restrained_S_all      1.039
_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)+(0.0986P)²+5.2946P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1694
_refine_special_details          SQUEEZE
_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
2. Restrained distances
 C1M-O1M
 1.38 with sigma of 0.02
 O1M-H1M
 0.82 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C52(H52A,H52B), C53(H53A,H53B)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C37(H37), C23(H23), C41(H41), C50(H50), C12(H12), C46(H46),
 C21(H21), C39(H39), C47(H47), C38(H38), C6(H6), C2(H2), C48(H48), C31(H31),
 C33(H33), C4(H4), C29(H29), C10(H10), C19(H19), C20(H20), C11(H11), C2D(H2D)
3.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C4D(H4DA,H4DB,H4DC), C5D(H5DA,H5DB,H5DC), C54(H54A,H54B,
 H54C), C1M(H1MA,H1MB,H1MC)
;
_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
Cu2 Cu -0.00932(2) 0.71215(2) 0.40020(2) 0.03736(12) Uani 1 1 d . . . . .
Cu1 Cu 0.01127(3) 0.82255(2) 0.33117(2) 0.03971(13) Uani 1 1 d . . . . .
O9 O -0.03247(15) 0.21567(11) 0.54403(8) 0.0423(5) Uani 1 1 d . . . . .
O8 O -0.05543(16) 0.12222(12) 0.60233(8) 0.0459(5) Uani 1 1 d . . . . .
O2 O 0.10831(15) 0.14481(11) 0.65794(9) 0.0428(5) Uani 1 1 d . . . . .
O3 O 0.12860(14) 0.24169(12) 0.60191(9) 0.0436(5) Uani 1 1 d . . . . .
O6 O -0.04283(15) 0.74966(13) 0.27834(9) 0.0479(5) Uani 1 1 d . . . . .
O7 O -0.05109(16) 0.65315(13) 0.33634(9) 0.0509(6) Uani 1 1 d . . . . .
O1M O 0.03832(18) 0.91573(15) 0.27961(10) 0.0546(6) Uani 1 1 d D . . . .
O5 O 0.11269(15) 0.68524(13) 0.38947(9) 0.0466(5) Uani 1 1 d . . . . .
O1D O -0.04193(17) 0.62567(13) 0.45711(11) 0.0570(6) Uani 1 1 d . . . . .
O1 O 0.72462(17) 0.38042(15) 0.44717(11) 0.0598(7) Uani 1 1 d . . . . .
O4 O 0.12615(15) 0.77661(14) 0.32757(9) 0.0499(6) Uani 1 1 d . . . . .
C13 C 0.2498(2) 0.16558(16) 0.63053(13) 0.0415(7) Uani 1 1 d . . . . .
O10 O -0.1539(2) 0.13793(17) 0.11316(11) 0.0751(8) Uani 1 1 d . . . . .
C14 C 0.3006(2) 0.19816(18) 0.59396(14) 0.0453(8) Uani 1 1 d . . . . .
H14 H 0.273652 0.228593 0.565530 0.054 Uiso 1 1 calc R . . . .
C51 C -0.0560(2) 0.14931(17) 0.55537(12) 0.0390(7) Uani 1 1 d . . . . .
C15 C 0.1548(2) 0.18484(16) 0.62975(12) 0.0390(7) Uani 1 1 d . . . . .
C40 C -0.1116(2) 0.63787(18) 0.24570(13) 0.0431(7) Uani 1 1 d . . . . .
C37 C -0.2022(2) 0.55529(19) 0.16429(13) 0.0488(8) Uani 1 1 d . . . . .
H37 H -0.233556 0.527124 0.136135 0.059 Uiso 1 1 calc R . . . .
C23 C 0.2819(2) 0.6336(2) 0.37597(13) 0.0476(8) Uani 1 1 d . . . . .
H23 H 0.246544 0.604040 0.397541 0.057 Uiso 1 1 calc R . . . .
C41 C -0.1131(2) 0.56030(18) 0.24884(13) 0.0441(7) Uani 1 1 d . . . . .
H41 H -0.084295 0.535580 0.279590 0.053 Uiso 1 1 calc R . . . .
C22 C 0.2472(2) 0.6983(2) 0.34970(13) 0.0478(8) Uani 1 1 d . . . . .
C50 C -0.0904(2) 0.12783(17) 0.45605(12) 0.0403(7) Uani 1 1 d . . . . .
H50 H -0.078099 0.179551 0.450232 0.048 Uiso 1 1 calc R . . . .
C45 C -0.1141(2) 0.08101(17) 0.41147(13) 0.0446(8) Uani 1 1 d . . . . .
C12 C 0.2889(2) 0.11944(18) 0.67133(15) 0.0500(8) Uani 1 1 d . . . . .
H12 H 0.253951 0.095777 0.696416 0.060 Uiso 1 1 calc R . . . .
C49 C -0.0849(2) 0.09943(16) 0.50860(12) 0.0391(7) Uani 1 1 d . . . . .
C42 C -0.0641(2) 0.68404(18) 0.29041(14) 0.0448(8) Uani 1 1 d . . . . .
C25 C 0.7865(2) 0.3278(2) 0.47205(14) 0.0521(9) Uani 1 1 d . . . . .
H25A H 0.770585 0.275782 0.460474 0.062 Uiso 1 1 calc R . . . .
H25B H 0.787611 0.330678 0.512189 0.062 Uiso 1 1 calc R . . . .
C36 C -0.1565(2) 0.51793(17) 0.20722(13) 0.0428(7) Uani 1 1 d . . . . .
C34 C -0.1508(3) 0.3703(2) 0.20798(13) 0.0523(9) Uani 1 1 d . . . . .
C44 C -0.1211(3) 0.11124(18) 0.35723(14) 0.0505(8) Uani 1 1 d . . . . .
C46 C -0.1311(3) 0.00503(18) 0.42085(14) 0.0523(9) Uani 1 1 d . . . . .
H46 H -0.146261 -0.027626 0.390966 0.063 Uiso 1 1 calc R . . . .
C24 C 0.1548(2) 0.72126(19) 0.35598(13) 0.0452(8) Uani 1 1 d . . . . .
C30 C -0.1468(3) 0.28946(19) 0.20885(14) 0.0503(8) Uani 1 1 d . . . . .
C35 C -0.1541(2) 0.43774(19) 0.20828(13) 0.0475(8) Uani 1 1 d . . . . .
C21 C 0.2986(2) 0.7402(2) 0.31775(15) 0.0575(9) Uani 1 1 d . . . . .
H21 H 0.274883 0.783706 0.299401 0.069 Uiso 1 1 calc R . . . .
C39 C -0.1559(2) 0.67462(19) 0.20192(15) 0.0522(9) Uani 1 1 d . . . . .
H39 H -0.154321 0.728021 0.199300 0.063 Uiso 1 1 calc R . . . .
C9 C 0.3914(3) 0.1874(2) 0.59774(17) 0.0555(9) Uani 1 1 d . . . . .
C47 C -0.1260(3) -0.02296(18) 0.47320(14) 0.0538(9) Uani 1 1 d . . . . .
H47 H -0.138123 -0.074671 0.479210 0.065 Uiso 1 1 calc R . . . .
C3 C 0.5166(3) 0.3233(2) 0.49859(16) 0.0570(9) Uani 1 1 d . . . . .
C38 C -0.2027(3) 0.6322(2) 0.16204(15) 0.0576(10) Uani 1 1 d . . . . .
H38 H -0.235530 0.657003 0.132767 0.069 Uiso 1 1 calc R . . . .
C32 C -0.1334(3) 0.17425(19) 0.26051(14) 0.0520(9) Uani 1 1 d . . . . .
C6 C 0.5855(3) 0.4325(2) 0.43478(14) 0.0541(9) Uani 1 1 d . . . . .
H6 H 0.609767 0.469891 0.412974 0.065 Uiso 1 1 calc R . . . .
C2 C 0.6055(3) 0.3217(2) 0.49041(14) 0.0536(9) Uani 1 1 d . . . . .
H2 H 0.642480 0.283486 0.506779 0.064 Uiso 1 1 calc R . . . .
C43 C -0.1259(3) 0.13765(18) 0.31269(14) 0.0524(9) Uani 1 1 d . . . . .
C48 C -0.1035(2) 0.02375(18) 0.51680(13) 0.0473(8) Uani 1 1 d . . . . .
H48 H -0.100696 0.004129 0.552749 0.057 Uiso 1 1 calc R . . . .
C18 C 0.3690(2) 0.6126(2) 0.37045(14) 0.0542(9) Uani 1 1 d . . . . .
C26 C 0.8739(2) 0.3483(2) 0.45415(14) 0.0536(9) Uani 1 1 d . . . . .
H26A H 0.919381 0.315614 0.473038 0.064 Uiso 1 1 calc R . . . .
H26B H 0.887663 0.401152 0.464742 0.064 Uiso 1 1 calc R . . . .
C1 C 0.6389(2) 0.3759(2) 0.45844(14) 0.0514(8) Uani 1 1 d . . . . .
C31 C -0.1356(3) 0.25176(19) 0.25886(14) 0.0541(9) Uani 1 1 d . . . . .
H31 H -0.129396 0.279822 0.291781 0.065 Uiso 1 1 calc R . . . .
C5 C 0.4976(2) 0.4346(2) 0.44277(15) 0.0566(9) Uani 1 1 d . . . . .
C17 C 0.4074(2) 0.5472(2) 0.39745(15) 0.0567(9) Uani 1 1 d . . . . .
C33 C -0.1399(3) 0.13295(19) 0.21190(14) 0.0547(9) Uani 1 1 d . . . . .
H33 H -0.138676 0.079411 0.212659 0.066 Uiso 1 1 calc R . . . .
C27 C 0.8771(3) 0.3401(2) 0.39299(15) 0.0588(9) Uani 1 1 d . . . . .
H27A H 0.863731 0.287852 0.382319 0.088 Uiso 1 1 calc GR . . . .
H27B H 0.935819 0.353318 0.383109 0.088 Uiso 1 1 calc GR . . . .
H27C H 0.833688 0.373818 0.374118 0.088 Uiso 1 1 calc GR . . . .
C4 C 0.4634(3) 0.3795(2) 0.47451(16) 0.0606(10) Uani 1 1 d . . . . .
H4 H 0.402649 0.380158 0.479879 0.073 Uiso 1 1 calc R . . . .
C28 C -0.1482(3) 0.1711(2) 0.16278(14) 0.0556(9) Uani 1 1 d . . . . .
C8 C 0.4422(3) 0.2283(2) 0.56134(18) 0.0599(10) Uani 1 1 d . . . . .
C29 C -0.1527(3) 0.24900(19) 0.16116(14) 0.0521(9) Uani 1 1 d . . . . .
H29 H -0.159970 0.274428 0.127160 0.062 Uiso 1 1 calc R . . . .
C10 C 0.4300(3) 0.1408(2) 0.63907(18) 0.0630(11) Uani 1 1 d . . . . .
H10 H 0.491471 0.131803 0.641991 0.076 Uiso 1 1 calc R . . . .
N3D N -0.1434(2) 0.5664(2) 0.50633(16) 0.0790(11) Uani 1 1 d . . . . .
C19 C 0.4198(3) 0.6566(3) 0.33794(16) 0.0628(10) Uani 1 1 d . . . . .
H19 H 0.478802 0.642684 0.333797 0.075 Uiso 1 1 calc R . . . .
C20 C 0.3851(3) 0.7193(3) 0.31222(16) 0.0649(11) Uani 1 1 d . . . . .
H20 H 0.420149 0.748875 0.290417 0.078 Uiso 1 1 calc R . . . .
C16 C 0.4450(3) 0.4950(2) 0.41805(16) 0.0597(10) Uani 1 1 d . . . . .
C7 C 0.4787(3) 0.2688(2) 0.53275(18) 0.0610(10) Uani 1 1 d . . . . .
C11 C 0.3781(3) 0.1081(2) 0.67529(18) 0.0627(11) Uani 1 1 d . . . . .
H11 H 0.404403 0.077116 0.703613 0.075 Uiso 1 1 calc R . . . .
C2D C -0.1169(3) 0.6071(3) 0.4649(2) 0.0779(13) Uani 1 1 d . . . . .
H2D H -0.161685 0.623505 0.438364 0.094 Uiso 1 1 calc R . . . .
C52 C -0.1408(4) 0.0634(3) 0.1106(2) 0.0869(14) Uani 1 1 d . . . . .
H52A H -0.188536 0.035783 0.126686 0.104 Uiso 1 1 calc R . . . .
H52B H -0.084139 0.049416 0.130541 0.104 Uiso 1 1 calc R . . . .
C4D C -0.2350(3) 0.5489(3) 0.5094(2) 0.0932(15) Uani 1 1 d . . . . .
H4DA H -0.270593 0.577585 0.481552 0.140 Uiso 1 1 calc GR . . . .
H4DB H -0.252141 0.562503 0.545506 0.140 Uiso 1 1 calc GR . . . .
H4DC H -0.244500 0.494865 0.503247 0.140 Uiso 1 1 calc GR . . . .
C5D C -0.0832(4) 0.5339(3) 0.5488(2) 0.0948(16) Uani 1 1 d . . . . .
H5DA H -0.024832 0.529200 0.535656 0.142 Uiso 1 1 calc GR . . . .
H5DB H -0.104352 0.483931 0.558455 0.142 Uiso 1 1 calc GR . . . .
H5DC H -0.079844 0.566582 0.580944 0.142 Uiso 1 1 calc GR . . . .
C53 C -0.1404(5) 0.0447(3) 0.0482(2) 0.1014(18) Uani 1 1 d . . . . .
H53A H -0.141221 -0.010592 0.042753 0.122 Uiso 1 1 calc R . . . .
H53B H -0.193363 0.066200 0.027874 0.122 Uiso 1 1 calc R . . . .
C54 C -0.0617(6) 0.0767(5) 0.0278(3) 0.158(3) Uani 1 1 d . . . . .
H54A H -0.054739 0.129076 0.040054 0.238 Uiso 1 1 calc GR . . . .
H54B H -0.067223 0.075118 -0.012052 0.238 Uiso 1 1 calc GR . . . .
H54C H -0.010307 0.047335 0.041793 0.238 Uiso 1 1 calc GR . . . .
C1M C 0.0250(6) 0.9877(3) 0.2975(2) 0.121(3) Uani 1 1 d D . . . .
H1MA H 0.050727 1.023788 0.273369 0.182 Uiso 1 1 calc GR . . . .
H1MB H 0.052992 0.993499 0.334594 0.182 Uiso 1 1 calc GR . . . .
H1MC H -0.038081 0.997225 0.297415 0.182 Uiso 1 1 calc GR . . . .
H1M H 0.085(2) 0.910(3) 0.264(2) 0.12(2) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu2 Cu1 2.6321(5) . ?
Cu2 O9 1.946(2) 3_566 ?
Cu2 O3 1.996(2) 3_566 ?
Cu2 O7 1.951(2) . ?
Cu2 O5 1.967(2) . ?
Cu2 O1D 2.167(2) . ?
Cu1 O8 1.978(2) 3_566 ?
Cu1 O2 1.959(2) 3_566 ?
Cu1 O6 1.966(2) . ?
Cu1 O1M 2.148(2) . ?
Cu1 O4 1.946(2) . ?
O9 C51 1.269(4) . ?
O8 C51 1.254(4) . ?
O2 C15 1.257(4) . ?
O3 C15 1.265(4) . ?
O6 C42 1.252(4) . ?
O7 C42 1.258(4) . ?
O1M C1M 1.372(5) . ?
O5 C24 1.264(4) . ?
O1D C2D 1.223(5) . ?
O1 C25 1.429(4) . ?
O1 C1 1.366(4) . ?
O4 C24 1.262(4) . ?
C13 C14 1.370(5) . ?
C13 C15 1.491(5) . ?
C13 C12 1.391(4) . ?
O10 C28 1.354(4) . ?
O10 C52 1.339(5) . ?
C14 C9 1.396(5) . ?
C51 C49 1.490(4) . ?
C40 C41 1.379(5) . ?
C40 C42 1.508(4) . ?
C40 C39 1.387(5) . ?
C37 C36 1.385(5) . ?
C37 C38 1.366(5) . ?
C23 C22 1.398(5) . ?
C23 C18 1.401(5) . ?
C41 C36 1.393(4) . ?
C22 C24 1.492(5) . ?
C22 C21 1.380(5) . ?
C50 C45 1.400(4) . ?
C50 C49 1.386(4) . ?
C45 C44 1.437(5) . ?
C45 C46 1.396(5) . ?
C12 C11 1.375(5) . ?
C49 C48 1.391(4) . ?
C25 C26 1.490(5) . ?
C36 C35 1.423(5) . ?
C34 C30 1.436(5) . ?
C34 C35 1.197(5) . ?
C44 C43 1.191(5) . ?
C46 C47 1.379(5) . ?
C30 C31 1.400(5) . ?
C30 C29 1.374(5) . ?
C21 C20 1.392(6) . ?
C39 C38 1.386(5) . ?
C9 C8 1.435(6) . ?
C9 C10 1.403(5) . ?
C47 C48 1.377(5) . ?
C3 C2 1.392(5) . ?
C3 C4 1.387(6) . ?
C3 C7 1.438(6) . ?
C32 C43 1.437(5) . ?
C32 C31 1.376(5) . ?
C32 C33 1.401(5) . ?
C6 C1 1.390(5) . ?
C6 C5 1.376(5) . ?
C2 C1 1.371(5) . ?
C18 C17 1.437(6) . ?
C18 C19 1.403(6) . ?
C26 C27 1.521(5) . ?
C5 C4 1.383(6) . ?
C5 C16 1.443(5) . ?
C17 C16 1.181(5) . ?
C33 C28 1.383(5) . ?
C28 C29 1.384(5) . ?
C8 C7 1.181(6) . ?
C10 C11 1.374(6) . ?
N3D C2D 1.343(6) . ?
N3D C4D 1.444(6) . ?
N3D C5D 1.452(6) . ?
C19 C20 1.365(6) . ?
C52 C53 1.577(7) . ?
C53 C54 1.459(10) . ?

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
O9 Cu2 Cu1 85.24(6) 3_566 . ?
O9 Cu2 O3 89.49(9) 3_566 3_566 ?
O9 Cu2 O7 170.95(9) 3_566 . ?
O9 Cu2 O5 89.90(10) 3_566 . ?
O9 Cu2 O1D 95.05(9) 3_566 . ?
O3 Cu2 Cu1 80.74(6) 3_566 . ?
O3 Cu2 O1D 92.59(10) 3_566 . ?
O7 Cu2 Cu1 85.76(7) . . ?
O7 Cu2 O3 88.02(10) . 3_566 ?
O7 Cu2 O5 90.48(10) . . ?
O7 Cu2 O1D 93.76(10) . . ?
O5 Cu2 Cu1 85.67(7) . . ?
O5 Cu2 O3 166.40(9) . 3_566 ?
O5 Cu2 O1D 100.99(10) . . ?
O1D Cu2 Cu1 173.33(7) . . ?
O8 Cu1 Cu2 83.32(6) 3_566 . ?
O8 Cu1 O1M 92.30(9) 3_566 . ?
O2 Cu1 Cu2 87.98(6) 3_566 . ?
O2 Cu1 O8 89.70(10) 3_566 3_566 ?
O2 Cu1 O6 86.66(9) 3_566 . ?
O2 Cu1 O1M 94.86(10) 3_566 . ?
O6 Cu1 Cu2 82.65(7) . . ?
O6 Cu1 O8 165.62(10) . 3_566 ?
O6 Cu1 O1M 101.86(10) . . ?
O1M Cu1 Cu2 174.78(7) . . ?
O4 Cu1 Cu2 82.99(7) . . ?
O4 Cu1 O8 90.08(10) . 3_566 ?
O4 Cu1 O2 170.93(9) . 3_566 ?
O4 Cu1 O6 91.34(10) . . ?
O4 Cu1 O1M 94.20(10) . . ?
C51 O9 Cu2 122.44(19) . 3_566 ?
C51 O8 Cu1 123.40(19) . 3_566 ?
C15 O2 Cu1 119.3(2) . 3_566 ?
C15 O3 Cu2 125.9(2) . 3_566 ?
C42 O6 Cu1 123.9(2) . . ?
C42 O7 Cu2 120.5(2) . . ?
C1M O1M Cu1 118.9(3) . . ?
C24 O5 Cu2 120.6(2) . . ?
C2D O1D Cu2 124.3(3) . . ?
C1 O1 C25 119.1(3) . . ?
C24 O4 Cu1 124.8(2) . . ?
C14 C13 C15 120.3(3) . . ?
C14 C13 C12 119.5(3) . . ?
C12 C13 C15 120.0(3) . . ?
C52 O10 C28 118.2(4) . . ?
C13 C14 C9 121.2(3) . . ?
O9 C51 C49 116.8(3) . . ?
O8 C51 O9 125.5(3) . . ?
O8 C51 C49 117.7(3) . . ?
O2 C15 O3 125.6(3) . . ?
O2 C15 C13 117.5(3) . . ?
O3 C15 C13 116.8(3) . . ?
C41 C40 C42 120.7(3) . . ?
C41 C40 C39 120.2(3) . . ?
C39 C40 C42 119.0(3) . . ?
C38 C37 C36 120.6(3) . . ?
C22 C23 C18 119.9(3) . . ?
C40 C41 C36 120.4(3) . . ?
C23 C22 C24 120.1(3) . . ?
C21 C22 C23 119.6(3) . . ?
C21 C22 C24 120.3(3) . . ?
C49 C50 C45 120.6(3) . . ?
C50 C45 C44 120.2(3) . . ?
C46 C45 C50 118.8(3) . . ?
C46 C45 C44 121.0(3) . . ?
C11 C12 C13 119.9(4) . . ?
C50 C49 C51 119.9(3) . . ?
C50 C49 C48 119.4(3) . . ?
C48 C49 C51 120.8(3) . . ?
O6 C42 O7 126.5(3) . . ?
O6 C42 C40 116.7(3) . . ?
O7 C42 C40 116.7(3) . . ?
O1 C25 C26 106.9(3) . . ?
C37 C36 C41 118.8(3) . . ?
C37 C36 C35 120.2(3) . . ?
C41 C36 C35 121.0(3) . . ?
C35 C34 C30 178.8(4) . . ?
C43 C44 C45 178.5(4) . . ?
C47 C46 C45 120.4(3) . . ?
O5 C24 C22 118.1(3) . . ?
O4 C24 O5 125.8(3) . . ?
O4 C24 C22 116.1(3) . . ?
C31 C30 C34 119.5(3) . . ?
C29 C30 C34 120.6(3) . . ?
C29 C30 C31 119.9(3) . . ?
C34 C35 C36 178.3(4) . . ?
C22 C21 C20 120.5(4) . . ?
C38 C39 C40 119.0(3) . . ?
C14 C9 C8 118.7(3) . . ?
C14 C9 C10 118.8(4) . . ?
C10 C9 C8 122.4(4) . . ?
C48 C47 C46 120.3(3) . . ?
C2 C3 C7 121.4(4) . . ?
C4 C3 C2 119.8(4) . . ?
C4 C3 C7 118.8(4) . . ?
C37 C38 C39 120.8(3) . . ?
C31 C32 C43 118.5(3) . . ?
C31 C32 C33 119.8(3) . . ?
C33 C32 C43 121.6(3) . . ?
C5 C6 C1 120.3(4) . . ?
C1 C2 C3 119.2(4) . . ?
C44 C43 C32 176.1(4) . . ?
C47 C48 C49 120.5(3) . . ?
C23 C18 C17 121.6(4) . . ?
C23 C18 C19 119.1(4) . . ?
C19 C18 C17 119.3(3) . . ?
C25 C26 C27 112.2(3) . . ?
O1 C1 C6 114.3(3) . . ?
O1 C1 C2 124.9(3) . . ?
C2 C1 C6 120.8(3) . . ?
C32 C31 C30 120.3(3) . . ?
C6 C5 C4 119.0(4) . . ?
C6 C5 C16 118.3(4) . . ?
C4 C5 C16 122.6(4) . . ?
C16 C17 C18 174.8(4) . . ?
C28 C33 C32 119.2(3) . . ?
C5 C4 C3 120.8(4) . . ?
O10 C28 C33 125.0(3) . . ?
O10 C28 C29 114.1(3) . . ?
C33 C28 C29 120.9(3) . . ?
C7 C8 C9 172.6(4) . . ?
C30 C29 C28 119.8(3) . . ?
C11 C10 C9 119.4(4) . . ?
C2D N3D C4D 121.0(4) . . ?
C2D N3D C5D 123.3(4) . . ?
C4D N3D C5D 115.7(4) . . ?
C20 C19 C18 120.5(4) . . ?
C19 C20 C21 120.4(4) . . ?
C17 C16 C5 175.3(5) . . ?
C8 C7 C3 174.5(4) . . ?
C10 C11 C12 121.3(3) . . ?
O1D C2D N3D 127.8(4) . . ?
O10 C52 C53 105.5(4) . . ?
C54 C53 C52 109.2(5) . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.207 0.250 1021 240 ' '
2 -0.250 0.793 0.750 1022 240 ' '
3 0.079 0.499 0.624 7 0 ' '
4 0.420 0.499 0.876 7 0 ' '
5 0.579 0.501 0.124 7 0 ' '
6 0.920 0.501 0.376 7 0 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.448
_oxdiff_exptl_absorpt_empirical_full_min 0.608
_exptl_crystal_preparation       'Gas sorption'
####################################################################### 
# 
# 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_gac354_sq
_database_code_depnum_ccdc_archive 'CCDC 1966329'
loop_
_audit_author_name
_audit_author_address
'Gavin Craig'
;University of Strathclyde
United Kingdom
;
_audit_update_record             
;
2019-11-18 deposited with the CCDC.	2020-02-24 downloaded from the CCDC.
;
_audit_creation_date             2019-10-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3

# start Validation Reply Form
_vrf_PLAT420_gac354_sq           
;
PROBLEM: D-H without acceptor
RESPONSE: The water molecule bound to the Cu paddlewheel points into the 
void of the cage complex, and SQUEEZE has been used to account for the
disordered solvent therein.
;

# end Validation Reply Form

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C108.5 H79 Cu4 N2 O24, 1.4(C4 H9 N O)'
_chemical_formula_sum            'C128.50 H124 Cu4 N7 O29'
_chemical_formula_weight         2484.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cu4 C100 H65 O10 N2'
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'

_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                   14.2345(3)
_cell_length_b                   29.3603(5)
_cell_length_c                   16.5980(4)
_cell_angle_alpha                90
_cell_angle_beta                 111.254(3)
_cell_angle_gamma                90
_cell_volume                     6465.0(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    28687
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.5460
_cell_measurement_theta_min      2.0990
_shelx_estimated_absorpt_T_max   0.931
_shelx_estimated_absorpt_T_min   0.899
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            78471
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.075
_diffrn_reflns_theta_min         1.912
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  67.00   0.30   16.00    --  -20.60  45.00 -18.92  590
  2  ω   -110.00  67.00   0.30   16.00    --  -20.60  45.00 -18.92  590
  3  ω     18.00  67.20   0.30   16.00    --  -20.60  45.00  -6.80  164
  4  ω    -86.00 -60.20   0.30   16.00    --  -20.60  45.00  60.00   86
  5  ω    -19.00  63.20   0.30   16.00    --  -20.60  45.00  60.00  274
  6  ω   -109.00  67.10   0.30   16.00    --  -20.60  45.00 179.59  587
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0086064000
_diffrn_orient_matrix_UB_12      0.0147329000
_diffrn_orient_matrix_UB_13      0.0358596000
_diffrn_orient_matrix_UB_21      0.0072802000
_diffrn_orient_matrix_UB_22      0.0184840000
_diffrn_orient_matrix_UB_23      -0.0246376000
_diffrn_orient_matrix_UB_31      -0.0522509000
_diffrn_orient_matrix_UB_32      0.0049703000
_diffrn_orient_matrix_UB_33      -0.0145318000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12704
_reflns_number_total             15871
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         15871
_refine_ls_number_restraints     112
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0602
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0784P)²+9.0344P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1746
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O60-H60A = O60-H60B
 0.88 with sigma of 0.01
 H60A-H60B
 1.33 with sigma of 0.02
 C80-N82 = N2S-C5S
 1.35 with sigma of 0.01
 N82-C83 = N2S-C8S = N2S-C7S
 1.46 with sigma of 0.01
 N82-C84
 1.46 with sigma of 0.01
 C81-C84
 2.88 with sigma of 0.02
 C83-C84
 2.5 with sigma of 0.02
 C5S-C6S
 1.5 with sigma of 0.01
3. Rigid bond restraints
 O70, C71, N72, C74, C75, C73
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O1S, N1S, C3S, C2S, C4S, C1S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O70 \\sim C71 \\sim N72 \\sim C74 \\sim C75 \\sim C73: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.02
O1S \\sim N1S \\sim C3S \\sim C2S \\sim C4S \\sim C1S: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.02
Uanis(N72) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq: with sigma of
0.007 and sigma for terminal atoms of 0.014
Uanis(O70) = Uanis(O80)
Uanis(N82) = Uanis(N72)
Uanis(C80) = Uanis(C71)
Uanis(C81) = Uanis(C73)
Uanis(C83) = Uanis(C74)
Uanis(C84) = Uanis(C75)
5. Others
 Sof(O80)=Sof(C80)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C83)=Sof(H83A)=
 Sof(H83B)=Sof(H83C)=Sof(N82)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=1-FVAR(1)
 Sof(O70)=Sof(C71)=Sof(N72)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=Sof(C75)=
 Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=FVAR(1)
 Fixed Sof: H60A(0.75) O1S(0.5) N1S(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5)
 H3SC(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5) H2SC(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5)
 H4SC(0.5) C1S(0.5) C61(0.25) H61A(0.25) H61B(0.25) H61C(0.25) O4S(0.2)
 C5S(0.2) N2S(0.2) C7S(0.2) H7SA(0.2) H7SB(0.2) H7SC(0.2) C6S(0.2) H6SA(0.2)
 H6SB(0.2) H6SC(0.2) C8S(0.2) H8SA(0.2) H8SB(0.2) H8SC(0.2)
6.a Fixed occupancy and ADP/Uiso:
 H60A, H60B
6.b Riding coordinates:
 C81(H81A,H81B,H81C), C83(H83A,H83B,H83C)
6.c Me refined with riding coordinates:
 C74(H74A,H74B,H74C), C84(H84A,H84B,H84C), C7S(H7SA,H7SB,H7SC), C6S(H6SA,H6SB,
 H6SC), C8S(H8SA,H8SB,H8SC)
6.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C14(H14), C23(H23), C21(H21), C48(H48), C20(H20), C12(H12), C2(H2),
 C10(H10), C37(H37), C39(H39), C4(H4), C19(H19), C27(H27), C35(H35), C45(H45),
 C44(H44), C11(H11), C46(H46), C36(H36), C31(H31), C29(H29)
6.e Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C50(H50A,H50B,H50C), C75(H75A,H75B,H75C), C73(H73A,H73B,
 H73C), C3S(H3SA,H3SB,H3SC), C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC), C61(H61A,
 H61B,H61C)
;
_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
Cu1 Cu -0.16189(3) 0.64381(2) 0.11603(2) 0.03210(10) Uani 1 1 d . . . . .
Cu2 Cu 0.09217(3) 0.40648(2) 0.74324(2) 0.03262(10) Uani 1 1 d . . . . .
O9 O -0.01975(16) 0.65796(8) 0.13909(14) 0.0423(5) Uani 1 1 d . . . . .
O7 O 0.29259(16) 0.37679(7) 0.88336(14) 0.0410(5) Uani 1 1 d . . . . .
O2 O -0.16371(18) 0.69352(7) 0.19414(14) 0.0437(5) Uani 1 1 d . . . . .
O4 O 0.14883(17) 0.41316(7) 0.94129(14) 0.0410(5) Uani 1 1 d . . . . .
O10 O 0.03886(16) 0.61097(8) 0.25264(15) 0.0457(5) Uani 1 1 d . . . . .
O8 O 0.23347(16) 0.41630(8) 0.75928(14) 0.0414(5) Uani 1 1 d . . . . .
O5 O 0.10099(18) 0.45682(7) 0.82221(15) 0.0438(5) Uani 1 1 d . . . . .
O3 O -0.09502(19) 0.65119(7) 0.31374(14) 0.0445(5) Uani 1 1 d . . . . .
O1 O 0.19703(17) 0.81255(7) 0.92869(14) 0.0417(5) Uani 1 1 d . . . . .
O60 O 0.0297(3) 0.44451(11) 0.62568(19) 0.0692(8) Uani 1 1 d D . . . .
H60A H 0.064(5) 0.456(3) 0.595(3) 0.104 Uiso 0.75 1 d D . P A 1
H60B H -0.013(3) 0.4291(17) 0.581(2) 0.104 Uiso 1 1 d D . . B 1
C13 C -0.1256(2) 0.72839(10) 0.3306(2) 0.0369(6) Uani 1 1 d . . . . .
C22 C 0.1257(2) 0.49189(10) 0.9558(2) 0.0352(6) Uani 1 1 d . . . . .
C49 C 0.0493(2) 0.63992(10) 0.20058(19) 0.0360(6) Uani 1 1 d . . . . .
O6 O 0.7806(2) 0.64059(11) 0.6911(2) 0.0756(10) Uani 1 1 d . . . . .
C6 C 0.1498(2) 0.73658(10) 0.9105(2) 0.0395(6) Uani 1 1 d . . . . .
H6 H 0.177315 0.733580 0.970297 0.047 Uiso 1 1 calc R . . . .
C24 C 0.1254(2) 0.45050(10) 0.9020(2) 0.0354(6) Uani 1 1 d . . . . .
C5 C 0.1079(2) 0.69874(10) 0.8592(2) 0.0423(7) Uani 1 1 d . . . . .
C40 C 0.3031(2) 0.40028(9) 0.8237(2) 0.0347(6) Uani 1 1 d . . . . .
C14 C -0.0833(2) 0.72409(11) 0.4195(2) 0.0396(6) Uani 1 1 d . . . . .
H14 H -0.059262 0.695939 0.444006 0.047 Uiso 1 1 calc R . . . .
C38 C 0.4090(2) 0.41011(9) 0.8305(2) 0.0355(6) Uani 1 1 d . . . . .
C23 C 0.1191(2) 0.53475(10) 0.9190(2) 0.0374(6) Uani 1 1 d . . . . .
H23 H 0.116676 0.537659 0.862438 0.045 Uiso 1 1 calc R . . . .
C1 C 0.1508(2) 0.77874(10) 0.8726(2) 0.0375(6) Uani 1 1 d . . . . .
C8 C -0.0284(3) 0.75733(12) 0.5647(2) 0.0473(8) Uani 1 1 d . . . . .
C15 C -0.1283(2) 0.68786(10) 0.27500(19) 0.0358(6) Uani 1 1 d . . . . .
C18 C 0.1162(2) 0.57342(10) 0.9666(2) 0.0412(7) Uani 1 1 d . . . . .
C16 C 0.1110(2) 0.65464(11) 0.8985(2) 0.0453(7) Uani 1 1 d . . . . .
C21 C 0.1295(2) 0.48718(11) 1.0400(2) 0.0402(6) Uani 1 1 d . . . . .
H21 H 0.135529 0.458470 1.065026 0.048 Uiso 1 1 calc R . . . .
C9 C -0.0765(2) 0.76168(12) 0.4726(2) 0.0439(7) Uani 1 1 d . . . . .
C47 C 0.1561(2) 0.65323(11) 0.2134(2) 0.0398(6) Uani 1 1 d . . . . .
C48 C 0.2335(2) 0.63755(12) 0.2854(2) 0.0445(7) Uani 1 1 d . . . . .
H48 H 0.219266 0.618873 0.324698 0.053 Uiso 1 1 calc R . . . .
C20 C 0.1244(2) 0.52551(12) 1.0862(2) 0.0452(7) Uani 1 1 d . . . . .
H20 H 0.125387 0.522474 1.142290 0.054 Uiso 1 1 calc R . . . .
C7 C 0.0148(3) 0.75255(12) 0.6404(2) 0.0473(8) Uani 1 1 d . . . . .
C12 C -0.1653(2) 0.76995(11) 0.2931(2) 0.0417(7) Uani 1 1 d . . . . .
H12 H -0.194730 0.772658 0.233348 0.050 Uiso 1 1 calc R . . . .
C17 C 0.1128(2) 0.61791(11) 0.9291(2) 0.0453(7) Uani 1 1 d . . . . .
C2 C 0.1080(2) 0.78413(11) 0.7838(2) 0.0390(6) Uani 1 1 d . . . . .
H2 H 0.108405 0.812406 0.758669 0.047 Uiso 1 1 calc R . . . .
C10 C -0.1163(3) 0.80350(12) 0.4339(2) 0.0497(8) Uani 1 1 d . . . . .
H10 H -0.112618 0.828911 0.468368 0.060 Uiso 1 1 calc R . . . .
C37 C 0.4887(3) 0.38819(12) 0.8917(2) 0.0486(8) Uani 1 1 d . . . . .
H37 H 0.476887 0.366991 0.928545 0.058 Uiso 1 1 calc R . . . .
C34 C 0.5254(3) 0.45168(11) 0.7829(2) 0.0452(7) Uani 1 1 d . . . . .
C3 C 0.0639(2) 0.74629(11) 0.7323(2) 0.0425(7) Uani 1 1 d . . . . .
C39 C 0.4271(2) 0.44144(10) 0.7757(2) 0.0393(6) Uani 1 1 d . . . . .
H39 H 0.373219 0.455784 0.733580 0.047 Uiso 1 1 calc R . . . .
C4 C 0.0656(2) 0.70377(11) 0.7700(2) 0.0452(7) Uani 1 1 d . . . . .
H4 H 0.038283 0.678634 0.735292 0.054 Uiso 1 1 calc R . . . .
C43 C 0.3331(3) 0.64947(14) 0.2996(2) 0.0526(9) Uani 1 1 d . . . . .
C19 C 0.1180(3) 0.56804(12) 1.0506(2) 0.0478(8) Uani 1 1 d . . . . .
H19 H 0.114746 0.593544 1.082680 0.057 Uiso 1 1 calc R . . . .
C28 C 0.5406(3) 0.60572(13) 0.5251(2) 0.0497(8) Uani 1 1 d . . . . .
C27 C 0.6290(2) 0.63088(13) 0.5653(2) 0.0489(8) Uani 1 1 d . . . . .
H27 H 0.643517 0.656079 0.537882 0.059 Uiso 1 1 calc R . . . .
C33 C 0.5452(3) 0.48636(13) 0.7300(3) 0.0534(9) Uani 1 1 d . . . . .
C35 C 0.6047(3) 0.42944(14) 0.8438(3) 0.0589(10) Uani 1 1 d . . . . .
H35 H 0.670461 0.435686 0.848367 0.071 Uiso 1 1 calc R . . . .
C30 C 0.5856(3) 0.55521(13) 0.6468(3) 0.0545(9) Uani 1 1 d . . . . .
C45 C 0.2751(3) 0.69139(15) 0.1653(3) 0.0584(10) Uani 1 1 d . . . . .
H45 H 0.289230 0.708935 0.124419 0.070 Uiso 1 1 calc R . . . .
C44 C 0.3530(3) 0.67651(15) 0.2386(3) 0.0630(11) Uani 1 1 d . . . . .
H44 H 0.419049 0.684618 0.247146 0.076 Uiso 1 1 calc R . . . .
C32 C 0.5625(3) 0.51657(14) 0.6907(3) 0.0595(10) Uani 1 1 d . . . . .
C25 C 0.2048(3) 0.85621(11) 0.8927(2) 0.0487(8) Uani 1 1 d . . . . .
H25A H 0.138515 0.868238 0.862878 0.073 Uiso 1 1 calc GR . . . .
H25B H 0.239251 0.852957 0.852875 0.073 Uiso 1 1 calc GR . . . .
H25C H 0.241874 0.876648 0.938309 0.073 Uiso 1 1 calc GR . . . .
C11 C -0.1605(3) 0.80714(11) 0.3456(2) 0.0485(8) Uani 1 1 d . . . . .
H11 H -0.187527 0.834875 0.320834 0.058 Uiso 1 1 calc R . . . .
C46 C 0.1771(3) 0.68026(12) 0.1530(2) 0.0464(7) Uani 1 1 d . . . . .
H46 H 0.124861 0.690760 0.104335 0.056 Uiso 1 1 calc R . . . .
C36 C 0.5865(3) 0.39771(15) 0.8983(3) 0.0666(12) Uani 1 1 d . . . . .
H36 H 0.640174 0.382763 0.939408 0.080 Uiso 1 1 calc R . . . .
C41 C 0.4706(3) 0.62054(14) 0.4424(3) 0.0567(9) Uani 1 1 d . . . . .
C26 C 0.6940(3) 0.61784(14) 0.6457(3) 0.0555(9) Uani 1 1 d . . . . .
C31 C 0.6724(3) 0.58055(14) 0.6879(3) 0.0567(9) Uani 1 1 d . . . . .
H31 H 0.715748 0.572635 0.743092 0.068 Uiso 1 1 calc R . . . .
C42 C 0.4110(3) 0.63416(15) 0.3762(2) 0.0572(10) Uani 1 1 d . . . . .
C29 C 0.5202(3) 0.56755(14) 0.5655(3) 0.0541(9) Uani 1 1 d . . . . .
H29 H 0.462592 0.550349 0.537843 0.065 Uiso 1 1 calc R . . . .
C50 C 0.8069(4) 0.67741(18) 0.6456(3) 0.0836(16) Uani 1 1 d . . . . .
H50A H 0.815357 0.665754 0.594646 0.125 Uiso 1 1 calc GR . . . .
H50B H 0.868703 0.691173 0.682513 0.125 Uiso 1 1 calc GR . . . .
H50C H 0.754136 0.699791 0.629480 0.125 Uiso 1 1 calc GR . . . .
O70 O -0.2294(3) 0.68353(15) 0.0029(3) 0.0493(9) Uani 0.733(4) 1 d . U P C 1
C71 C -0.2176(5) 0.6897(2) -0.0606(4) 0.0657(13) Uani 0.733(4) 1 d . U P C 1
N72 N -0.2870(6) 0.7149(3) -0.1241(4) 0.096(2) Uani 0.733(4) 1 d . U P C 1
C74 C -0.2784(10) 0.7256(4) -0.2049(7) 0.160(4) Uani 0.733(4) 1 d . U P C 1
H74A H -0.335314 0.743478 -0.238999 0.240 Uiso 0.733(4) 1 calc R . P C 1
H74B H -0.217527 0.742526 -0.194979 0.240 Uiso 0.733(4) 1 calc R . P C 1
H74C H -0.276433 0.697896 -0.235006 0.240 Uiso 0.733(4) 1 calc R . P C 1
C75 C -0.3716(9) 0.7355(5) -0.1110(9) 0.167(4) Uani 0.733(4) 1 d . U P C 1
H75A H -0.401359 0.757777 -0.155228 0.251 Uiso 0.733(4) 1 calc GR . P C 1
H75B H -0.349516 0.749996 -0.055360 0.251 Uiso 0.733(4) 1 calc GR . P C 1
H75C H -0.420510 0.712501 -0.113512 0.251 Uiso 0.733(4) 1 calc GR . P C 1
C73 C -0.1332(5) 0.6684(3) -0.0790(5) 0.0819(18) Uani 0.733(4) 1 d . U P C 1
H73A H -0.101157 0.646021 -0.035442 0.123 Uiso 0.733(4) 1 calc GR . P C 1
H73B H -0.085039 0.691335 -0.078697 0.123 Uiso 0.733(4) 1 calc GR . P C 1
H73C H -0.158619 0.653968 -0.134631 0.123 Uiso 0.733(4) 1 calc GR . P C 1
O1S O 0.8618(5) 0.58053(19) 0.5673(4) 0.0672(15) Uani 0.5 1 d . U P D 1
N1S N 0.7964(6) 0.5135(2) 0.5744(6) 0.0688(18) Uani 0.5 1 d . U P D 1
C3S C 0.7216(7) 0.5178(3) 0.4914(8) 0.067(2) Uani 0.5 1 d . U P D 1
H3SA H 0.659983 0.528141 0.496495 0.100 Uiso 0.5 1 calc GR . P D 1
H3SB H 0.710533 0.488715 0.462971 0.100 Uiso 0.5 1 calc GR . P D 1
H3SC H 0.743165 0.539342 0.458261 0.100 Uiso 0.5 1 calc GR . P D 1
C2S C 0.9225(8) 0.5415(4) 0.7037(8) 0.087(3) Uani 0.5 1 d . U P D 1
H2SA H 0.884922 0.553543 0.736637 0.130 Uiso 0.5 1 calc GR . P D 1
H2SB H 0.984607 0.558030 0.717532 0.130 Uiso 0.5 1 calc GR . P D 1
H2SC H 0.936821 0.509919 0.717481 0.130 Uiso 0.5 1 calc GR . P D 1
C4S C 0.7815(9) 0.4732(3) 0.6182(9) 0.081(3) Uani 0.5 1 d . U P D 1
H4SA H 0.831408 0.472182 0.675584 0.122 Uiso 0.5 1 calc GR . P D 1
H4SB H 0.787581 0.446617 0.586801 0.122 Uiso 0.5 1 calc GR . P D 1
H4SC H 0.715494 0.473987 0.621462 0.122 Uiso 0.5 1 calc GR . P D 1
C1S C 0.8597(8) 0.5466(3) 0.6057(7) 0.071(2) Uani 0.5 1 d . U P D 1
O80 O -0.2007(11) 0.6750(5) -0.0019(10) 0.0493(9) Uani 0.267(4) 1 d . . P C 2
C80 C -0.2630(14) 0.7063(6) -0.0312(11) 0.0657(13) Uani 0.267(4) 1 d D . P C 2
C81 C -0.3379(14) 0.7199(7) 0.0111(13) 0.0819(18) Uani 0.267(4) 1 d D . P C 2
H81A H -0.324837 0.703273 0.063908 0.123 Uiso 0.267(4) 1 d R . P C 2
H81B H -0.406307 0.714693 -0.026792 0.123 Uiso 0.267(4) 1 d R . P C 2
H81C H -0.327807 0.751803 0.023648 0.123 Uiso 0.267(4) 1 d R . P C 2
C83 C -0.173(2) 0.7183(10) -0.1354(18) 0.160(4) Uani 0.267(4) 1 d D . P C 2
H83A H -0.119859 0.698665 -0.100580 0.240 Uiso 0.267(4) 1 d R . P C 2
H83B H -0.145929 0.747775 -0.139320 0.240 Uiso 0.267(4) 1 d R . P C 2
H83C H -0.203219 0.705514 -0.192320 0.240 Uiso 0.267(4) 1 d R . P C 2
N82 N -0.2466(16) 0.7295(6) -0.0956(12) 0.096(2) Uani 0.267(4) 1 d D . P C 2
C84 C -0.264(2) 0.7783(7) -0.085(2) 0.167(4) Uani 0.267(4) 1 d D . P C 2
H84A H -0.252346 0.795545 -0.129395 0.251 Uiso 0.267(4) 1 calc R . P C 2
H84B H -0.331654 0.782787 -0.087769 0.251 Uiso 0.267(4) 1 calc R . P C 2
H84C H -0.217766 0.788409 -0.029216 0.251 Uiso 0.267(4) 1 calc R . P C 2
C61 C 0.0808(14) 0.4770(6) 0.6042(11) 0.062(4) Uiso 0.25 1 d . . P E 2
H61A H 0.111759 0.496613 0.653041 0.092 Uiso 0.25 1 calc GR . P E 2
H61B H 0.035731 0.494517 0.557195 0.092 Uiso 0.25 1 calc GR . P E 2
H61C H 0.132017 0.463564 0.586945 0.092 Uiso 0.25 1 calc GR . P E 2
O4S O 0.8722(10) 0.5648(5) 0.5080(9) 0.056(3) Uiso 0.2 1 d . . P F 2
C5S C 0.8291(17) 0.5352(8) 0.5342(12) 0.069(5) Uiso 0.2 1 d D . P F 2
N2S N 0.8482(19) 0.5237(9) 0.6170(13) 0.081(7) Uiso 0.2 1 d D . P F 2
C7S C 0.942(2) 0.5471(14) 0.669(2) 0.115(14) Uiso 0.2 1 d D . P F 2
H7SA H 0.958208 0.539748 0.728847 0.173 Uiso 0.2 1 calc R . P F 2
H7SB H 0.995409 0.537306 0.650869 0.173 Uiso 0.2 1 calc R . P F 2
H7SC H 0.932739 0.579369 0.660976 0.173 Uiso 0.2 1 calc R . P F 2
C6S C 0.745(2) 0.5111(14) 0.466(2) 0.105(13) Uiso 0.2 1 d D . P F 2
H6SA H 0.715699 0.488811 0.491952 0.158 Uiso 0.2 1 calc R . P F 2
H6SB H 0.693937 0.532838 0.434659 0.158 Uiso 0.2 1 calc R . P F 2
H6SC H 0.770195 0.496340 0.426153 0.158 Uiso 0.2 1 calc R . P F 2
C8S C 0.818(3) 0.4850(11) 0.657(2) 0.098(12) Uiso 0.2 1 d D . P F 2
H8SA H 0.845894 0.488054 0.718633 0.148 Uiso 0.2 1 calc R . P F 2
H8SB H 0.745568 0.484062 0.638039 0.148 Uiso 0.2 1 calc R . P F 2
H8SC H 0.841779 0.457329 0.640178 0.148 Uiso 0.2 1 calc R . P F 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
Cu1 Cu2 2.6345(5) 3_566 ?
Cu1 O9 1.962(2) . ?
Cu1 O7 1.960(2) 3_566 ?
Cu1 O2 1.959(2) . ?
Cu1 O4 1.966(2) 3_566 ?
Cu1 O70 2.121(4) . ?
Cu1 O80 2.048(15) . ?
Cu2 O10 1.959(2) 3_566 ?
Cu2 O8 1.952(2) . ?
Cu2 O5 1.949(2) . ?
Cu2 O3 1.947(2) 3_566 ?
Cu2 O60 2.142(3) . ?
O9 C49 1.250(4) . ?
O7 C40 1.260(4) . ?
O2 C15 1.262(4) . ?
O4 C24 1.258(4) . ?
O10 C49 1.259(4) . ?
O8 C40 1.257(4) . ?
O5 C24 1.255(4) . ?
O3 C15 1.255(4) . ?
O1 C1 1.357(3) . ?
O1 C25 1.435(4) . ?
O60 C61 1.325(17) . ?
C13 C14 1.383(4) . ?
C13 C15 1.498(4) . ?
C13 C12 1.393(4) . ?
C22 C24 1.508(4) . ?
C22 C23 1.388(4) . ?
C22 C21 1.384(4) . ?
C49 C47 1.508(4) . ?
O6 C26 1.364(4) . ?
O6 C50 1.444(5) . ?
C6 C5 1.395(4) . ?
C6 C1 1.390(4) . ?
C5 C16 1.444(5) . ?
C5 C4 1.390(5) . ?
C40 C38 1.498(4) . ?
C14 C9 1.394(4) . ?
C38 C37 1.378(4) . ?
C38 C39 1.383(4) . ?
C23 C18 1.393(4) . ?
C1 C2 1.385(5) . ?
C8 C9 1.437(5) . ?
C8 C7 1.189(5) . ?
C18 C17 1.440(5) . ?
C18 C19 1.393(5) . ?
C16 C17 1.188(5) . ?
C21 C20 1.379(4) . ?
C9 C10 1.406(5) . ?
C47 C48 1.378(5) . ?
C47 C46 1.394(5) . ?
C48 C43 1.393(5) . ?
C20 C19 1.371(5) . ?
C7 C3 1.441(5) . ?
C12 C11 1.383(4) . ?
C2 C3 1.404(4) . ?
C10 C11 1.374(5) . ?
C37 C36 1.384(5) . ?
C34 C39 1.393(4) . ?
C34 C33 1.438(5) . ?
C34 C35 1.376(5) . ?
C3 C4 1.393(5) . ?
C43 C44 1.395(5) . ?
C43 C42 1.423(5) . ?
C28 C27 1.403(5) . ?
C28 C41 1.440(5) . ?
C28 C29 1.389(5) . ?
C27 C26 1.374(5) . ?
C33 C32 1.179(5) . ?
C35 C36 1.386(5) . ?
C30 C32 1.449(5) . ?
C30 C31 1.391(5) . ?
C30 C29 1.382(5) . ?
C45 C44 1.386(5) . ?
C45 C46 1.373(5) . ?
C41 C42 1.188(5) . ?
C26 C31 1.392(5) . ?
O70 C71 1.140(7) . ?
C71 N72 1.371(9) . ?
C71 C73 1.482(9) . ?
N72 C74 1.424(11) . ?
N72 C75 1.432(11) . ?
O1S C1S 1.190(11) . ?
N1S C3S 1.408(13) . ?
N1S C4S 1.445(10) . ?
N1S C1S 1.297(13) . ?
C2S C1S 1.553(15) . ?
O80 C80 1.247(19) . ?
C80 C81 1.53(2) . ?
C80 N82 1.358(10) . ?
C83 N82 1.464(10) . ?
N82 C84 1.476(10) . ?
O4S C5S 1.23(2) . ?
C5S N2S 1.343(10) . ?
C5S C6S 1.500(10) . ?
N2S C7S 1.466(10) . ?
N2S C8S 1.459(10) . ?

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
O9 Cu1 Cu2 85.15(7) . 3_566 ?
O9 Cu1 O4 90.17(10) . 3_566 ?
O9 Cu1 O70 99.25(14) . . ?
O9 Cu1 O80 89.6(4) . . ?
O7 Cu1 Cu2 82.85(6) 3_566 3_566 ?
O7 Cu1 O9 167.92(9) 3_566 . ?
O7 Cu1 O4 89.79(10) 3_566 3_566 ?
O7 Cu1 O70 92.73(14) 3_566 . ?
O7 Cu1 O80 102.4(4) 3_566 . ?
O2 Cu1 Cu2 85.52(7) . 3_566 ?
O2 Cu1 O9 88.46(10) . . ?
O2 Cu1 O7 89.21(10) . 3_566 ?
O2 Cu1 O4 168.67(9) . 3_566 ?
O2 Cu1 O70 93.76(14) . . ?
O2 Cu1 O80 103.7(4) . . ?
O4 Cu1 Cu2 83.16(7) 3_566 3_566 ?
O4 Cu1 O70 97.56(14) 3_566 . ?
O4 Cu1 O80 87.6(4) 3_566 . ?
O70 Cu1 Cu2 175.53(12) . 3_566 ?
O10 Cu2 Cu1 83.10(7) 3_566 3_566 ?
O10 Cu2 O60 94.71(12) 3_566 . ?
O8 Cu2 Cu1 85.62(6) . 3_566 ?
O8 Cu2 O10 168.72(9) . 3_566 ?
O8 Cu2 O60 96.55(11) . . ?
O5 Cu2 Cu1 85.24(7) . 3_566 ?
O5 Cu2 O10 90.28(10) . 3_566 ?
O5 Cu2 O8 89.10(10) . . ?
O5 Cu2 O60 96.98(11) . . ?
O3 Cu2 Cu1 82.86(7) 3_566 3_566 ?
O3 Cu2 O10 88.70(10) 3_566 3_566 ?
O3 Cu2 O8 89.59(10) 3_566 . ?
O3 Cu2 O5 168.10(10) 3_566 . ?
O3 Cu2 O60 94.92(11) 3_566 . ?
O60 Cu2 Cu1 176.90(9) . 3_566 ?
C49 O9 Cu1 121.3(2) . . ?
C40 O7 Cu1 123.8(2) . 3_566 ?
C15 O2 Cu1 120.6(2) . . ?
C24 O4 Cu1 123.0(2) . 3_566 ?
C49 O10 Cu2 123.5(2) . 3_566 ?
C40 O8 Cu2 121.13(19) . . ?
C24 O5 Cu2 121.54(19) . . ?
C15 O3 Cu2 124.6(2) . 3_566 ?
C1 O1 C25 117.4(3) . . ?
C61 O60 Cu2 122.2(8) . . ?
C14 C13 C15 119.3(3) . . ?
C14 C13 C12 120.4(3) . . ?
C12 C13 C15 120.4(3) . . ?
C23 C22 C24 119.0(3) . . ?
C21 C22 C24 120.5(3) . . ?
C21 C22 C23 120.5(3) . . ?
O9 C49 O10 126.4(3) . . ?
O9 C49 C47 117.4(3) . . ?
O10 C49 C47 116.2(3) . . ?
C26 O6 C50 115.6(3) . . ?
C1 C6 C5 120.4(3) . . ?
O4 C24 C22 116.9(3) . . ?
O5 C24 O4 126.6(3) . . ?
O5 C24 C22 116.5(3) . . ?
C6 C5 C16 120.1(3) . . ?
C4 C5 C6 119.3(3) . . ?
C4 C5 C16 120.5(3) . . ?
O7 C40 C38 116.7(3) . . ?
O8 C40 O7 126.3(3) . . ?
O8 C40 C38 117.0(3) . . ?
C13 C14 C9 120.4(3) . . ?
C37 C38 C40 120.2(3) . . ?
C37 C38 C39 119.7(3) . . ?
C39 C38 C40 120.1(3) . . ?
C22 C23 C18 120.0(3) . . ?
O1 C1 C6 115.1(3) . . ?
O1 C1 C2 124.3(3) . . ?
C2 C1 C6 120.7(3) . . ?
C7 C8 C9 177.0(4) . . ?
O2 C15 C13 117.5(3) . . ?
O3 C15 O2 126.1(3) . . ?
O3 C15 C13 116.4(3) . . ?
C23 C18 C17 119.8(3) . . ?
C23 C18 C19 118.8(3) . . ?
C19 C18 C17 121.4(3) . . ?
C17 C16 C5 178.6(4) . . ?
C20 C21 C22 119.3(3) . . ?
C14 C9 C8 120.0(3) . . ?
C14 C9 C10 118.6(3) . . ?
C10 C9 C8 121.5(3) . . ?
C48 C47 C49 119.0(3) . . ?
C48 C47 C46 120.1(3) . . ?
C46 C47 C49 121.0(3) . . ?
C47 C48 C43 120.5(3) . . ?
C19 C20 C21 120.8(3) . . ?
C8 C7 C3 178.0(4) . . ?
C11 C12 C13 119.4(3) . . ?
C16 C17 C18 179.3(3) . . ?
C1 C2 C3 119.0(3) . . ?
C11 C10 C9 120.6(3) . . ?
C38 C37 C36 120.0(3) . . ?
C39 C34 C33 120.9(3) . . ?
C35 C34 C39 119.5(3) . . ?
C35 C34 C33 119.6(3) . . ?
C2 C3 C7 118.8(3) . . ?
C4 C3 C7 120.9(3) . . ?
C4 C3 C2 120.3(3) . . ?
C38 C39 C34 120.5(3) . . ?
C5 C4 C3 120.3(3) . . ?
C48 C43 C44 118.7(3) . . ?
C48 C43 C42 119.2(3) . . ?
C44 C43 C42 122.0(3) . . ?
C20 C19 C18 120.6(3) . . ?
C27 C28 C41 119.1(3) . . ?
C29 C28 C27 120.3(3) . . ?
C29 C28 C41 120.7(3) . . ?
C26 C27 C28 119.1(3) . . ?
C32 C33 C34 176.0(5) . . ?
C34 C35 C36 120.0(3) . . ?
C31 C30 C32 119.7(4) . . ?
C29 C30 C32 120.1(3) . . ?
C29 C30 C31 120.2(3) . . ?
C46 C45 C44 120.1(3) . . ?
C45 C44 C43 120.6(3) . . ?
C33 C32 C30 176.8(5) . . ?
C10 C11 C12 120.6(3) . . ?
C45 C46 C47 120.0(3) . . ?
C37 C36 C35 120.3(3) . . ?
C42 C41 C28 176.9(5) . . ?
O6 C26 C27 123.7(3) . . ?
O6 C26 C31 115.3(3) . . ?
C27 C26 C31 120.9(3) . . ?
C30 C31 C26 119.5(3) . . ?
C41 C42 C43 175.1(4) . . ?
C30 C29 C28 119.9(3) . . ?
C71 O70 Cu1 137.2(4) . . ?
O70 C71 N72 119.3(6) . . ?
O70 C71 C73 121.7(6) . . ?
N72 C71 C73 118.8(6) . . ?
C71 N72 C74 123.9(8) . . ?
C71 N72 C75 121.4(8) . . ?
C74 N72 C75 114.5(8) . . ?
C3S N1S C4S 111.6(9) . . ?
C1S N1S C3S 119.7(7) . . ?
C1S N1S C4S 128.2(10) . . ?
O1S C1S N1S 124.1(10) . . ?
O1S C1S C2S 121.6(10) . . ?
N1S C1S C2S 113.6(10) . . ?
C80 O80 Cu1 127.6(11) . . ?
O80 C80 C81 122.0(13) . . ?
O80 C80 N82 112.1(17) . . ?
N82 C80 C81 125.4(17) . . ?
C80 N82 C83 126.7(18) . . ?
C80 N82 C84 107.9(17) . . ?
C83 N82 C84 116.9(14) . . ?
O4S C5S N2S 127(2) . . ?
O4S C5S C6S 115(2) . . ?
N2S C5S C6S 118(2) . . ?
C5S N2S C7S 107(2) . . ?
C5S N2S C8S 133(3) . . ?
C8S N2S C7S 117(3) . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 743 189 ' '
2 -0.500 0.500 0.000 742 189 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.084
_oxdiff_exptl_absorpt_empirical_full_min 0.923
_exptl_crystal_preparation       'Gas sorption measurements'
