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

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

data_eb3251x1
_database_code_depnum_ccdc_archive 'CCDC 991823'
_audit_update_record             
;
2015-03-27 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
_audit_creation_date             2015-03-27
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C56 H75 Cl4 Cu8 N8 O16 + solvent'
_chemical_formula_sum            'C56 H75 Cl4 Cu8 N8 O16'
_chemical_formula_weight         1766.36
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C50 H50 N8 O20 Cu Cl'
_chemical_oxdiff_usercomment     '@ 120 K RS31/PS'
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'
Cl Cl 0.1484 0.1585 '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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   25.5938(6)
_cell_length_b                   19.9423(4)
_cell_length_c                   32.2211(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16445.6(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    12270
_cell_measurement_temperature    170
_cell_measurement_theta_max      25.7310
_cell_measurement_theta_min      3.3470
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.214
_exptl_absorpt_correction_T_max  0.318
_exptl_absorpt_correction_T_min  0.142
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             7160
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Diffusion of ether, methanol and acetonitrile'
_exptl_crystal_size_max          0.4951
_exptl_crystal_size_mid          0.3405
_exptl_crystal_size_min          0.2465
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            97866
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        22.464
_diffrn_reflns_theta_max         22.464
_diffrn_reflns_theta_min         2.988
_diffrn_ambient_temperature      170
_diffrn_detector                 Eos
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -86.00   42.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7954   19.0000  -60.0000 256

#__ type_ start__ end____ width___ exp.time_
  2 omega   -5.00   20.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7954  -99.0000 -150.0000 50

#__ type_ start__ end____ width___ exp.time_
  3 omega   -8.00   25.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7954  -99.0000    0.0000 66

#__ type_ start__ end____ width___ exp.time_
  4 omega  -70.00  -24.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7954  109.0000  171.4014 92

#__ type_ start__ end____ width___ exp.time_
  5 omega   42.00  104.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2798  174.0000 -159.0000 124

#__ type_ start__ end____ width___ exp.time_
  6 omega  -94.00    9.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7954  -57.0000  -90.0000 206

#__ type_ start__ end____ width___ exp.time_
  7 omega  -98.00   20.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7954  -38.0000  120.0000 236
;
_diffrn_measurement_device       'Agilent Technologies XCalibur'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0262304000
_diffrn_orient_matrix_UB_12      0.0011572000
_diffrn_orient_matrix_UB_13      0.0070745000
_diffrn_orient_matrix_UB_21      0.0074861000
_diffrn_orient_matrix_UB_22      -0.0164999000
_diffrn_orient_matrix_UB_23      0.0185737000
_diffrn_orient_matrix_UB_31      0.0049025000
_diffrn_orient_matrix_UB_32      0.0314824000
_diffrn_orient_matrix_UB_33      0.0094693000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8178
_reflns_number_total             10680
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     22.42
_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, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         2.922
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.147
_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     847
_refine_ls_number_reflns         10680
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0765
_refine_ls_restrained_S_all      1.088
_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)+(0.0529P)²+306.6443P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1910
_refine_special_details          
;
The data set was cut at a resolution of 0.93 A since the values of R(int) began to rise rapidly after this point.

Residual peaks corresponding to disordered solvent were examined with PLATON SQUEEZE and Olex2 solvent masking.  The calculated densities reported by PLATON SQUEEZE and Olex2 are wildly different.  SQUEEZE reports 1350 electrons per unit cell, which corresponds to 169 electrons per asymmetric unit, or four molecules of diethyl ether.  The residual peak list (below) recorded before SQUEEZE is not consistent with four missing molecules of diethyl ether.   However, Olex2 records 24 electrons per unit cell.  Since neither calculation is consistent with each other, or with the residual peaks observed, then neither calculation can be considered as a realistic representation of the crystal contents.  2.	Since the identity of the solvent accounted for by SQUEEZE cannot be reliably established by diffraction methods it has not been included in the chemical formula.

REM Highest difference peak  4.247,  deepest hole -0.805,  1-sigma level  0.248
Q1    1   0.1003  0.8026  0.4771  11.00000  0.05    4.25
Q2    1   0.4174  0.3531  0.3807  11.00000  0.05    3.55
Q3    1   0.3555  0.4794  0.3420  11.00000  0.05    3.42
Q4    1   0.1649  0.1375  0.3773  11.00000  0.05    3.36
Q5    1   0.1643  0.8651  0.5575  11.00000  0.05    3.33
Q6    1   0.1430  0.4794  0.0837  11.00000  0.05    3.33
Q7    1   0.0792  0.1456  0.5470  11.00000  0.05    2.87
Q8    1   0.1012  0.1990  0.4545  11.00000  0.05    2.56
Q9    1   0.1680  0.6973  0.1351  11.00000  0.05    1.85
Q10   1   0.0428  0.3183  0.1041  11.00000  0.05    1.83
Q11   1   0.3234  0.8012  0.5599  11.00000  0.05    1.78
Q12   1  -0.0443  0.1740  0.5622  11.00000  0.05    1.74
Q13   1   0.0933  0.8505  0.4820  11.00000  0.05    1.63
Q14   1   0.1159  0.6971  0.4530  11.00000  0.05    1.37
Q15   1   0.5595  0.4790  0.4425  11.00000  0.05    1.26
Q16   1   0.1199  0.3048  0.4814  11.00000  0.05    1.24
Q17   1   0.0060  0.3359  0.1444  11.00000  0.05    1.12
Q18   1   0.3673  0.5220  0.2805  11.00000  0.05    1.08
Q19   1   0.5449  0.5378  0.4432  11.00000  0.05    0.94
Q20   1   0.2573  0.8634  0.5453  11.00000  0.05    0.93
Q21   1   0.2021  0.5438  0.0725  11.00000  0.05    0.93
Q22   1  -0.0104  0.2023  0.5961  11.00000  0.05    0.92
Q23   1   0.1365  0.5195  0.1568  11.00000  0.05    0.90
Q24   1   0.3418  0.5790  0.5521  11.00000  0.05    0.83
Q25   1   0.1567  0.1998  0.4179  11.00000  0.05    0.76
Q26   1   0.2402  0.9060  0.5206  11.00000  0.05    0.75
Q27   1   0.1199  0.7464  0.3641  11.00000  0.05    0.73
Q28   1   0.0984  0.4994  0.5219  11.00000  0.05    0.72
Q29   1  -0.0369  0.0949  0.4251  11.00000  0.05    0.71
Q30   1   0.3928  0.5951  0.4002  11.00000  0.05    0.68
Q31   1   0.1285  0.2440  0.5723  11.00000  0.05    0.65
Q32   1   0.3000  0.5486  0.3604  11.00000  0.05    0.65
Q33   1   0.4713  0.4170  0.5055  11.00000  0.05    0.65
Q34   1  -0.0993  0.0857  0.4625  11.00000  0.05    0.64
Q35   1   0.0414  0.4439  0.5018  11.00000  0.05    0.64
Q36   1   0.0783  0.1329  0.4242  11.00000  0.05    0.60
Q37   1   0.1415  0.5171  0.2974  11.00000  0.05    0.59
Q38   1  -0.2670  0.6369  0.3567  11.00000  0.05    0.59
Q39   1   0.1384  0.1181  0.5214  11.00000  0.05    0.59
Q40   1   0.0610  0.0779  0.5288  11.00000  0.05    0.57
Q41   1   0.1772  0.5175  0.5343  11.00000  0.05    0.57
Q42   1   0.2631  0.4393  0.2386  11.00000  0.05    0.57
Q43   1   0.1246  0.5407  0.4816  11.00000  0.05    0.56
Q44   1   0.1632  0.5171  0.5241  11.00000  0.05    0.55
Q45   1   0.2770  0.6811  0.3583  11.00000  0.05    0.55
Q46   1   0.1230  0.3609  0.1830  11.00000  0.05    0.55
Q47   1   0.4031  0.4257  0.3356  11.00000  0.05    0.54
Q48   1  -0.0788  0.6726  0.2720  11.00000  0.05    0.53
Q49   1   0.3012  0.7244  0.4206  11.00000  0.05    0.53
Q50   1   0.2025  0.2397  0.3014  11.00000  0.05    0.53
;

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.435 -0.002 0.000 2251 675 ' '
2 0.823 0.022 0.500 2252 675 ' '
3 0.625 0.010 0.647 7 0 ' '
4 0.125 0.010 0.853 7 0 ' '
5 0.625 0.489 0.147 7 0 ' '
6 0.125 0.489 0.353 7 0 ' '
7 0.875 0.510 0.647 7 0 ' '
8 0.375 0.510 0.853 7 0 ' '
9 0.875 0.989 0.147 7 0 ' '
10 0.375 0.989 0.353 7 0 ' '
# Missing Reflections Below sin(th)/lambda= 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
2 0 0 1.591
4 0 0 3.184
2 1 0 1.891
0 2 0 2.042
2 2 0 2.590
1 1 1 1.441
2 1 1 1.994
3 1 1 2.673
0 2 1 2.138
1 2 1 2.281
2 2 1 2.666
0 0 2 1.264
1 0 2 1.494
2 0 2 2.032
3 0 2 2.702
1 1 2 1.809
2 1 2 2.275
3 1 2 2.888
0 2 2 2.402
1 2 2 2.531
2 2 2 2.882
1 1 3 2.296
2 1 3 2.678
0 2 3 2.787
1 2 3 2.899
0 0 4 2.528
1 0 4 2.651
1 1 4 2.841
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          'see _refine_special_details'


# start Validation Reply Form
_vrf_THETM01_eb3251x1            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Please see the _refine_special_details section of the CIF.
;
# end Validation Reply Form

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O16-H16
 0.87 with sigma of 0.01
 O12-H12
 0.87 with sigma of 0.01
 O4-H4
 0.87 with sigma of 0.01
 C56-H16
 1.916969 with sigma of 0.02
 Cu8-H16
 3.10123 with sigma of 0.02
 C42-H12
 1.927814 with sigma of 0.02
 Cu6-H12
 3.125451 with sigma of 0.02
 C14-H4
 1.903518 with sigma of 0.02
 Cu2-H4
 3.097624 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 C27, C28, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B),
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
  C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C26(H26), C31(H31), C33(H33), C45(H45),
 C47(H47)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C)
5.d Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.14243(5) 0.51091(6) 0.22329(4) 0.0303(3) Uani 1 1 d . . . . .
Cu2 Cu 0.16333(5) 0.35596(6) 0.25543(4) 0.0236(3) Uani 1 1 d D . . . .
Cu3 Cu 0.09991(5) 0.29310(6) 0.33418(4) 0.0222(3) Uani 1 1 d . . . . .
Cu4 Cu 0.08284(5) 0.34400(6) 0.43097(4) 0.0251(3) Uani 1 1 d . . . . .
Cu5 Cu 0.14786(5) 0.47175(6) 0.46757(4) 0.0282(3) Uani 1 1 d . . . . .
Cu6 Cu 0.16960(5) 0.62727(6) 0.43434(4) 0.0279(3) Uani 1 1 d D . . . .
Cu7 Cu 0.10400(5) 0.69235(6) 0.35752(4) 0.0299(3) Uani 1 1 d . . . . .
Cu8 Cu 0.07975(5) 0.63776(6) 0.26267(4) 0.0287(3) Uani 1 1 d D . . . .
Cl1 Cl 0.12481(17) 0.46426(18) 0.16093(10) 0.0721(12) Uani 1 1 d . . . . .
Cl2 Cl 0.11300(11) 0.18842(12) 0.35978(8) 0.0355(7) Uani 1 1 d . . . . .
Cl3 Cl 0.13128(14) 0.52171(16) 0.52931(9) 0.0512(9) Uani 1 1 d . . . . .
Cl4 Cl 0.12258(13) 0.79279(14) 0.32775(10) 0.0528(9) Uani 1 1 d . . . . .
O1 O 0.1928(3) 0.4416(3) 0.2347(2) 0.0263(16) Uani 1 1 d . . . . .
O2 O 0.1368(3) 0.6040(3) 0.2927(2) 0.0318(17) Uani 1 1 d . . . . .
O3 O 0.1542(3) 0.2857(3) 0.29421(19) 0.0273(16) Uani 1 1 d . . . . .
O4 O 0.1245(3) 0.3200(4) 0.1944(2) 0.051(2) Uani 1 1 d D . . . .
H4 H 0.0949(8) 0.313(6) 0.1815(19) 0.076 Uiso 1 1 d DR . . . .
O5 O 0.0514(3) 0.3117(3) 0.37794(19) 0.0242(15) Uani 1 1 d . . . . .
O6 O 0.1067(3) 0.4053(3) 0.2769(2) 0.0301(17) Uani 1 1 d . . . . .
O7 O 0.0930(3) 0.4078(3) 0.4736(2) 0.0301(17) Uani 1 1 d . . . . .
O8 O 0.1169(3) 0.2349(4) 0.4507(2) 0.044(2) Uani 1 1 d . U . . .
H8 H 0.1238 0.2147 0.4285 0.065 Uiso 1 1 calc GR . . . .
O9 O 0.1980(3) 0.5401(3) 0.4542(2) 0.0271(16) Uani 1 1 d . . . . .
O10 O 0.1391(3) 0.3762(3) 0.4000(2) 0.0300(17) Uani 1 1 d . . . . .
O11 O 0.1612(3) 0.6968(3) 0.3950(2) 0.0309(17) Uani 1 1 d . . . . .
O12 O 0.1338(3) 0.6675(4) 0.4974(2) 0.043(2) Uani 1 1 d D . . . .
H12 H 0.1045(7) 0.678(5) 0.5097(18) 0.064 Uiso 1 1 d DR . . . .
O13 O 0.0525(3) 0.6741(3) 0.3165(2) 0.0289(16) Uani 1 1 d . . . . .
O14 O 0.1098(3) 0.5809(3) 0.4159(2) 0.0342(18) Uani 1 1 d . . . . .
O15 O 0.0869(3) 0.5735(4) 0.2196(2) 0.0347(18) Uani 1 1 d . . . . .
O16 O 0.1196(3) 0.7361(4) 0.2397(3) 0.044(2) Uani 1 1 d D . . . .
H16 H 0.1494(7) 0.755(3) 0.234(3) 0.066 Uiso 1 1 d DR . . . .
N1 N 0.1696(3) 0.5621(4) 0.2717(3) 0.027(2) Uani 1 1 d . . . . .
N2 N 0.2222(3) 0.3030(4) 0.2320(2) 0.028(2) Uani 1 1 d . . . . .
N3 N 0.0736(3) 0.3750(4) 0.3047(2) 0.0215(19) Uani 1 1 d . . . . .
N4 N 0.0231(3) 0.3084(4) 0.4650(3) 0.027(2) Uani 1 1 d . . . . .
N5 N 0.1734(3) 0.4195(4) 0.4184(2) 0.0233(19) Uani 1 1 d . . . . .
N6 N 0.2311(3) 0.6783(4) 0.4559(3) 0.030(2) Uani 1 1 d . . . . .
N7 N 0.0769(3) 0.6140(4) 0.3898(3) 0.028(2) Uani 1 1 d . . . . .
N8 N 0.0210(3) 0.6748(4) 0.2297(3) 0.032(2) Uani 1 1 d . . . . .
C1 C 0.2405(4) 0.4517(5) 0.2486(3) 0.026(2) Uani 1 1 d . . . . .
C2 C 0.2795(4) 0.4038(5) 0.2393(3) 0.028(2) Uani 1 1 d . . . . .
C3 C 0.3302(4) 0.4146(4) 0.2520(3) 0.026(2) Uani 1 1 d . . . . .
H3 H 0.3557 0.3813 0.2462 0.031 Uiso 1 1 calc R . . . .
C4 C 0.3457(4) 0.4721(5) 0.2730(3) 0.033(3) Uani 1 1 d . . . . .
C5 C 0.3073(4) 0.5161(5) 0.2845(3) 0.032(3) Uani 1 1 d . . . . .
H5 H 0.3168 0.5541 0.3005 0.038 Uiso 1 1 calc R . . . .
C6 C 0.2540(4) 0.5076(5) 0.2737(3) 0.027(2) Uani 1 1 d . . . . .
C7 C 0.2145(4) 0.5539(5) 0.2905(3) 0.025(2) Uani 1 1 d . . . . .
C8 C 0.2239(4) 0.5889(5) 0.3318(3) 0.034(3) Uani 1 1 d . . . . .
H8A H 0.1961 0.5768 0.3513 0.051 Uiso 1 1 calc GR . . . .
H8B H 0.2239 0.6376 0.3276 0.051 Uiso 1 1 calc GR . . . .
H8C H 0.2577 0.5749 0.3431 0.051 Uiso 1 1 calc GR . . . .
C9 C 0.4019(4) 0.4824(7) 0.2836(5) 0.057(4) Uani 1 1 d . . . . .
H9A H 0.4056 0.5230 0.3005 0.086 Uiso 1 1 calc GR . . . .
H9B H 0.4222 0.4874 0.2580 0.086 Uiso 1 1 calc GR . . . .
H9C H 0.4148 0.4436 0.2992 0.086 Uiso 1 1 calc GR . . . .
C10 C 0.2642(4) 0.3446(5) 0.2131(3) 0.032(3) Uani 1 1 d . . . . .
H10A H 0.2522 0.3609 0.1857 0.038 Uiso 1 1 calc R . . . .
H10B H 0.2954 0.3162 0.2085 0.038 Uiso 1 1 calc R . . . .
C11 C 0.2412(4) 0.2660(5) 0.2692(3) 0.030(3) Uani 1 1 d . . . . .
H11A H 0.2616 0.2966 0.2871 0.036 Uiso 1 1 calc R . . . .
H11B H 0.2645 0.2290 0.2604 0.036 Uiso 1 1 calc R . . . .
C12 C 0.1950(4) 0.2374(5) 0.2937(3) 0.034(3) Uani 1 1 d . . . . .
H12A H 0.1826 0.1955 0.2805 0.041 Uiso 1 1 calc R . . . .
H12B H 0.2060 0.2269 0.3224 0.041 Uiso 1 1 calc R . . . .
C13 C 0.2012(4) 0.2552(5) 0.2006(3) 0.035(3) Uani 1 1 d . . . . .
H13A H 0.1821 0.2188 0.2149 0.042 Uiso 1 1 calc R . . . .
H13B H 0.2306 0.2348 0.1851 0.042 Uiso 1 1 calc R . . . .
C14 C 0.1653(5) 0.2899(6) 0.1708(3) 0.048(3) Uani 1 1 d D . . . .
H14A H 0.1846 0.3246 0.1550 0.057 Uiso 1 1 calc R . . . .
H14B H 0.1506 0.2572 0.1509 0.057 Uiso 1 1 calc R . . . .
C15 C 0.0048(4) 0.3401(5) 0.3735(3) 0.023(2) Uani 1 1 d . . . . .
C16 C -0.0341(4) 0.3247(5) 0.4037(3) 0.024(2) Uani 1 1 d . . . . .
C17 C -0.0839(4) 0.3496(5) 0.3995(3) 0.030(3) Uani 1 1 d . . . . .
H17 H -0.1096 0.3379 0.4195 0.036 Uiso 1 1 calc R . . . .
C18 C -0.0976(4) 0.3916(5) 0.3667(3) 0.034(3) Uani 1 1 d . . . . .
C19 C -0.0597(4) 0.4082(5) 0.3395(3) 0.029(3) Uani 1 1 d . . . . .
H19 H -0.0688 0.4380 0.3177 0.035 Uiso 1 1 calc R . . . .
C20 C -0.0078(4) 0.3849(5) 0.3410(3) 0.027(2) Uani 1 1 d . . . . .
C21 C 0.0318(4) 0.4095(5) 0.3116(3) 0.023(2) Uani 1 1 d . . . . .
C22 C 0.0252(4) 0.4750(5) 0.2901(4) 0.040(3) Uani 1 1 d . . . . .
H22A H 0.0572 0.5017 0.2933 0.060 Uiso 1 1 calc GR . . . .
H22B H -0.0043 0.4993 0.3023 0.060 Uiso 1 1 calc GR . . . .
H22C H 0.0185 0.4673 0.2605 0.060 Uiso 1 1 calc GR . . . .
C23 C -0.1541(4) 0.4138(6) 0.3637(4) 0.042(3) Uani 1 1 d . . . . .
H23A H -0.1770 0.3755 0.3692 0.063 Uiso 1 1 calc GR . . . .
H23B H -0.1609 0.4311 0.3358 0.063 Uiso 1 1 calc GR . . . .
H23C H -0.1608 0.4491 0.3842 0.063 Uiso 1 1 calc GR . . . .
C24 C -0.0202(4) 0.2794(5) 0.4391(3) 0.027(2) Uani 1 1 d . . . . .
H24A H -0.0092 0.2353 0.4281 0.033 Uiso 1 1 calc R . . . .
H24B H -0.0514 0.2723 0.4567 0.033 Uiso 1 1 calc R . . . .
C25 C 0.0058(4) 0.3695(5) 0.4875(3) 0.032(3) Uani 1 1 d . . . . .
H25A H -0.0174 0.3568 0.5108 0.038 Uiso 1 1 calc R . . . .
H25B H -0.0141 0.3990 0.4685 0.038 Uiso 1 1 calc R . . . .
C26 C 0.0536(4) 0.4069(6) 0.5041(3) 0.037(3) Uani 1 1 d . . . . .
H26 H 0.0564 0.4265 0.5309 0.044 Uiso 1 1 calc R . . . .
C27 C 0.0441(5) 0.2566(6) 0.4937(3) 0.038(3) Uani 1 1 d . U . . .
H27A H 0.0147 0.2331 0.5074 0.046 Uiso 1 1 calc R . . . .
H27B H 0.0653 0.2786 0.5155 0.046 Uiso 1 1 calc R . . . .
C28 C 0.0790(5) 0.2038(5) 0.4700(3) 0.039(3) Uani 1 1 d . U . . .
H28A H 0.0937 0.1712 0.4900 0.047 Uiso 1 1 calc R . . . .
H28B H 0.0574 0.1790 0.4497 0.047 Uiso 1 1 calc R . . . .
C29 C 0.2461(4) 0.5284(5) 0.4390(3) 0.028(2) Uani 1 1 d . . . . .
C30 C 0.2854(4) 0.5749(5) 0.4488(3) 0.034(3) Uani 1 1 d . . . . .
C31 C 0.3361(4) 0.5642(5) 0.4351(3) 0.032(3) Uani 1 1 d . . . . .
H31 H 0.3624 0.5963 0.4413 0.038 Uiso 1 1 calc R . . . .
C32 C 0.3492(4) 0.5074(6) 0.4125(4) 0.044(3) Uani 1 1 d . . . . .
C33 C 0.3100(4) 0.4615(6) 0.4017(3) 0.039(3) Uani 1 1 d . . . . .
H33 H 0.3189 0.4224 0.3865 0.047 Uiso 1 1 calc R . . . .
C34 C 0.2574(4) 0.4723(5) 0.4132(3) 0.027(2) Uani 1 1 d . . . . .
C35 C 0.2167(4) 0.4273(5) 0.3985(3) 0.027(2) Uani 1 1 d . . . . .
C36 C 0.2236(4) 0.3926(5) 0.3573(3) 0.033(3) Uani 1 1 d . . . . .
H36A H 0.2217 0.3440 0.3613 0.050 Uiso 1 1 calc GR . . . .
H36B H 0.2577 0.4045 0.3456 0.050 Uiso 1 1 calc GR . . . .
H36C H 0.1959 0.4069 0.3383 0.050 Uiso 1 1 calc GR . . . .
C37 C 0.4055(4) 0.4950(7) 0.3990(5) 0.061(4) Uani 1 1 d . . . . .
H37A H 0.4266 0.4826 0.4232 0.091 Uiso 1 1 calc GR . . . .
H37B H 0.4197 0.5359 0.3865 0.091 Uiso 1 1 calc GR . . . .
H37C H 0.4064 0.4585 0.3786 0.091 Uiso 1 1 calc GR . . . .
C38 C 0.2734(4) 0.6345(5) 0.4742(3) 0.032(3) Uani 1 1 d . . . . .
H38A H 0.3056 0.6615 0.4774 0.038 Uiso 1 1 calc R . . . .
H38B H 0.2623 0.6196 0.5021 0.038 Uiso 1 1 calc R . . . .
C39 C 0.2499(4) 0.7136(5) 0.4177(3) 0.030(3) Uani 1 1 d . . . . .
H39A H 0.2689 0.6817 0.3996 0.036 Uiso 1 1 calc R . . . .
H39B H 0.2742 0.7501 0.4255 0.036 Uiso 1 1 calc R . . . .
C40 C 0.2031(4) 0.7424(6) 0.3946(3) 0.037(3) Uani 1 1 d . . . . .
H40A H 0.1922 0.7850 0.4078 0.045 Uiso 1 1 calc R . . . .
H40B H 0.2131 0.7522 0.3655 0.045 Uiso 1 1 calc R . . . .
C41 C 0.2126(5) 0.7296(5) 0.4868(3) 0.039(3) Uani 1 1 d . . . . .
H41A H 0.1933 0.7656 0.4722 0.046 Uiso 1 1 calc R . . . .
H41B H 0.2431 0.7501 0.5008 0.046 Uiso 1 1 calc R . . . .
C42 C 0.1772(5) 0.6969(6) 0.5188(4) 0.042(3) Uani 1 1 d D . . . .
H42A H 0.1966 0.6619 0.5343 0.051 Uiso 1 1 calc R . . . .
H42B H 0.1646 0.7308 0.5389 0.051 Uiso 1 1 calc R . . . .
C43 C 0.0042(4) 0.6511(5) 0.3234(3) 0.031(3) Uani 1 1 d . . . . .
C44 C -0.0347(4) 0.6651(5) 0.2930(4) 0.040(3) Uani 1 1 d . . . . .
C45 C -0.0849(5) 0.6425(6) 0.2994(4) 0.051(3) Uani 1 1 d . . . . .
H45 H -0.1101 0.6507 0.2784 0.061 Uiso 1 1 calc R . . . .
C46 C -0.1012(5) 0.6081(6) 0.3352(4) 0.049(3) Uani 1 1 d . . . . .
C47 C -0.0616(4) 0.5919(5) 0.3634(4) 0.039(3) Uani 1 1 d . . . . .
H47 H -0.0705 0.5671 0.3875 0.047 Uiso 1 1 calc R . . . .
C48 C -0.0094(4) 0.6108(5) 0.3573(4) 0.035(3) Uani 1 1 d . . . . .
C49 C 0.0322(4) 0.5839(5) 0.3859(3) 0.030(3) Uani 1 1 d . . . . .
C50 C 0.0229(4) 0.5205(5) 0.4087(3) 0.036(3) Uani 1 1 d . . . . .
H50A H 0.0488 0.4870 0.4002 0.054 Uiso 1 1 calc GR . . . .
H50B H -0.0123 0.5039 0.4024 0.054 Uiso 1 1 calc GR . . . .
H50C H 0.0260 0.5286 0.4386 0.054 Uiso 1 1 calc GR . . . .
C51 C -0.1579(5) 0.5896(7) 0.3428(5) 0.069(4) Uani 1 1 d . . . . .
H51A H -0.1723 0.5681 0.3179 0.103 Uiso 1 1 calc GR . . . .
H51B H -0.1780 0.6302 0.3491 0.103 Uiso 1 1 calc GR . . . .
H51C H -0.1602 0.5585 0.3663 0.103 Uiso 1 1 calc GR . . . .
C52 C -0.0207(4) 0.7067(5) 0.2561(4) 0.040(3) Uani 1 1 d . . . . .
H52A H -0.0083 0.7512 0.2657 0.048 Uiso 1 1 calc R . . . .
H52B H -0.0524 0.7139 0.2390 0.048 Uiso 1 1 calc R . . . .
C53 C -0.0004(4) 0.6157(5) 0.2085(4) 0.037(3) Uani 1 1 d . . . . .
H53A H -0.0245 0.6299 0.1861 0.045 Uiso 1 1 calc R . . . .
H53B H -0.0203 0.5878 0.2284 0.045 Uiso 1 1 calc R . . . .
C54 C 0.0452(5) 0.5747(6) 0.1901(4) 0.048(3) Uani 1 1 d . . . . .
H54A H 0.0335 0.5284 0.1840 0.058 Uiso 1 1 calc R . . . .
H54B H 0.0573 0.5955 0.1639 0.058 Uiso 1 1 calc R . . . .
C55 C 0.0409(4) 0.7236(6) 0.2001(4) 0.042(3) Uani 1 1 d . . . . .
H55A H 0.0112 0.7486 0.1879 0.050 Uiso 1 1 calc R . . . .
H55B H 0.0590 0.6998 0.1773 0.050 Uiso 1 1 calc R . . . .
C56 C 0.0783(5) 0.7727(6) 0.2201(4) 0.047(3) Uani 1 1 d D . . . .
H56A H 0.0929 0.8031 0.1987 0.056 Uiso 1 1 calc R . . . .
H56B H 0.0596 0.8003 0.2409 0.056 Uiso 1 1 calc R . . . .


_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 Cl1 2.260(3) . ?
Cu1 O1 1.924(7) . ?
Cu1 O15 1.895(7) . ?
Cu1 N1 1.989(8) . ?
Cu2 O1 1.983(6) . ?
Cu2 O3 1.892(6) . ?
Cu2 O4 2.317(7) . ?
Cu2 O6 1.883(6) . ?
Cu2 N2 1.990(8) . ?
Cu3 Cl2 2.269(3) . ?
Cu3 O3 1.900(6) . ?
Cu3 O5 1.914(6) . ?
Cu3 N3 2.006(8) . ?
Cu4 O5 1.995(6) . ?
Cu4 O7 1.891(7) . ?
Cu4 O8 2.429(8) . ?
Cu4 O10 1.867(7) . ?
Cu4 N4 2.010(8) . ?
Cu5 Cl3 2.265(3) . ?
Cu5 O7 1.906(7) . ?
Cu5 O9 1.921(6) . ?
Cu5 N5 2.006(8) . ?
Cu6 O9 1.991(7) . ?
Cu6 O11 1.889(7) . ?
Cu6 O12 2.369(7) . ?
Cu6 O14 1.884(7) . ?
Cu6 N6 1.999(8) . ?
Cu7 Cl4 2.271(3) . ?
Cu7 O11 1.902(7) . ?
Cu7 O13 1.902(7) . ?
Cu7 N7 2.001(8) . ?
Cu8 O2 1.877(7) . ?
Cu8 O13 2.004(7) . ?
Cu8 O15 1.897(7) . ?
Cu8 O16 2.330(7) . ?
Cu8 N8 1.983(8) . ?
O1 C1 1.317(12) . ?
O2 N1 1.364(10) . ?
O3 C12 1.421(12) . ?
O4 H4 0.875(9) . ?
O4 C14 1.423(14) . ?
O5 C15 1.330(11) . ?
O6 N3 1.373(10) . ?
O7 C26 1.408(12) . ?
O8 H8 0.8400 . ?
O8 C28 1.308(13) . ?
O9 C29 1.347(12) . ?
O10 N5 1.367(10) . ?
O11 C40 1.407(12) . ?
O12 H12 0.872(10) . ?
O12 C42 1.433(13) . ?
O13 C43 1.339(12) . ?
O14 N7 1.361(10) . ?
O15 C54 1.430(13) . ?
O16 H16 0.874(10) . ?
O16 C56 1.434(13) . ?
N1 C7 1.309(12) . ?
N2 C10 1.489(13) . ?
N2 C11 1.488(13) . ?
N2 C13 1.490(13) . ?
N3 C21 1.291(12) . ?
N4 C24 1.503(12) . ?
N4 C25 1.486(13) . ?
N4 C27 1.488(13) . ?
N5 C35 1.290(12) . ?
N6 C38 1.510(13) . ?
N6 C39 1.496(13) . ?
N6 C41 1.504(13) . ?
N7 C49 1.297(13) . ?
N8 C52 1.507(14) . ?
N8 C53 1.468(13) . ?
N8 C55 1.455(14) . ?
C1 C2 1.414(14) . ?
C1 C6 1.420(14) . ?
C2 C3 1.379(14) . ?
C2 C10 1.503(14) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(14) . ?
C4 C5 1.367(15) . ?
C4 C9 1.493(15) . ?
C5 H5 0.9500 . ?
C5 C6 1.418(15) . ?
C6 C7 1.472(14) . ?
C7 C8 1.522(14) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.530(14) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.499(16) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.426(13) . ?
C15 C20 1.413(14) . ?
C16 C17 1.374(14) . ?
C16 C24 1.499(14) . ?
C17 H17 0.9500 . ?
C17 C18 1.393(15) . ?
C18 C19 1.347(15) . ?
C18 C23 1.516(15) . ?
C19 H19 0.9500 . ?
C19 C20 1.411(14) . ?
C20 C21 1.471(14) . ?
C21 C22 1.488(14) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.530(15) . ?
C26 H26 0.9500 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.577(15) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.404(14) . ?
C29 C34 1.422(14) . ?
C30 C31 1.388(15) . ?
C30 C38 1.474(15) . ?
C31 H31 0.9500 . ?
C31 C32 1.388(16) . ?
C32 C33 1.402(16) . ?
C32 C37 1.524(16) . ?
C33 H33 0.9500 . ?
C33 C34 1.413(15) . ?
C34 C35 1.454(14) . ?
C35 C36 1.507(14) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.523(15) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.522(15) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.424(16) . ?
C43 C48 1.398(15) . ?
C44 C45 1.380(16) . ?
C44 C52 1.492(16) . ?
C45 H45 0.9500 . ?
C45 C46 1.404(18) . ?
C46 C47 1.396(17) . ?
C46 C51 1.519(17) . ?
C47 H47 0.9500 . ?
C47 C48 1.404(15) . ?
C48 C49 1.507(15) . ?
C49 C50 1.484(14) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.544(16) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C56 1.513(16) . ?
C56 H56A 0.9900 . ?
C56 H56B 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
O1 Cu1 Cl1 90.4(2) . . ?
O1 Cu1 N1 89.1(3) . . ?
O15 Cu1 Cl1 93.8(2) . . ?
O15 Cu1 O1 170.6(3) . . ?
O15 Cu1 N1 88.5(3) . . ?
N1 Cu1 Cl1 168.0(3) . . ?
O1 Cu2 O4 98.2(3) . . ?
O1 Cu2 N2 92.4(3) . . ?
O3 Cu2 O1 155.2(3) . . ?
O3 Cu2 O4 106.2(3) . . ?
O3 Cu2 N2 87.2(3) . . ?
O6 Cu2 O1 88.1(3) . . ?
O6 Cu2 O3 92.8(3) . . ?
O6 Cu2 O4 98.3(3) . . ?
O6 Cu2 N2 178.9(3) . . ?
N2 Cu2 O4 80.7(3) . . ?
O3 Cu3 Cl2 93.8(2) . . ?
O3 Cu3 O5 171.2(3) . . ?
O3 Cu3 N3 89.3(3) . . ?
O5 Cu3 Cl2 90.4(2) . . ?
O5 Cu3 N3 88.5(3) . . ?
N3 Cu3 Cl2 166.1(2) . . ?
O5 Cu4 O8 94.6(3) . . ?
O5 Cu4 N4 92.7(3) . . ?
O7 Cu4 O5 153.6(3) . . ?
O7 Cu4 O8 111.2(3) . . ?
O7 Cu4 N4 86.9(3) . . ?
O10 Cu4 O5 87.9(3) . . ?
O10 Cu4 O7 92.9(3) . . ?
O10 Cu4 O8 99.8(3) . . ?
O10 Cu4 N4 179.0(3) . . ?
N4 Cu4 O8 79.3(3) . . ?
O7 Cu5 Cl3 93.8(2) . . ?
O7 Cu5 O9 171.7(3) . . ?
O7 Cu5 N5 88.4(3) . . ?
O9 Cu5 Cl3 90.6(2) . . ?
O9 Cu5 N5 88.5(3) . . ?
N5 Cu5 Cl3 169.5(3) . . ?
O9 Cu6 O12 99.3(3) . . ?
O9 Cu6 N6 92.6(3) . . ?
O11 Cu6 O9 153.9(3) . . ?
O11 Cu6 O12 106.4(3) . . ?
O11 Cu6 N6 87.1(3) . . ?
O14 Cu6 O9 88.2(3) . . ?
O14 Cu6 O11 93.3(3) . . ?
O14 Cu6 O12 97.0(3) . . ?
O14 Cu6 N6 177.4(3) . . ?
N6 Cu6 O12 80.5(3) . . ?
O11 Cu7 Cl4 93.8(2) . . ?
O11 Cu7 O13 170.0(3) . . ?
O11 Cu7 N7 88.4(3) . . ?
O13 Cu7 Cl4 91.1(2) . . ?
O13 Cu7 N7 88.4(3) . . ?
N7 Cu7 Cl4 168.8(3) . . ?
O2 Cu8 O13 87.4(3) . . ?
O2 Cu8 O15 93.4(3) . . ?
O2 Cu8 O16 97.1(3) . . ?
O2 Cu8 N8 178.2(4) . . ?
O13 Cu8 O16 97.0(3) . . ?
O15 Cu8 O13 155.5(3) . . ?
O15 Cu8 O16 107.1(3) . . ?
O15 Cu8 N8 86.1(3) . . ?
N8 Cu8 O13 93.7(3) . . ?
N8 Cu8 O16 81.3(3) . . ?
Cu1 O1 Cu2 115.4(3) . . ?
C1 O1 Cu1 125.1(6) . . ?
C1 O1 Cu2 111.7(6) . . ?
N1 O2 Cu8 116.3(5) . . ?
Cu2 O3 Cu3 118.7(3) . . ?
C12 O3 Cu2 113.7(6) . . ?
C12 O3 Cu3 126.8(6) . . ?
Cu2 O4 H4 145(2) . . ?
C14 O4 Cu2 105.6(6) . . ?
C14 O4 H4 109(2) . . ?
Cu3 O5 Cu4 115.6(3) . . ?
C15 O5 Cu3 125.8(6) . . ?
C15 O5 Cu4 108.5(5) . . ?
N3 O6 Cu2 119.0(5) . . ?
Cu4 O7 Cu5 118.5(3) . . ?
C26 O7 Cu4 113.5(6) . . ?
C26 O7 Cu5 127.4(6) . . ?
Cu4 O8 H8 106.4 . . ?
C28 O8 Cu4 106.4(6) . . ?
C28 O8 H8 109.5 . . ?
Cu5 O9 Cu6 116.6(3) . . ?
C29 O9 Cu5 124.8(6) . . ?
C29 O9 Cu6 111.6(6) . . ?
N5 O10 Cu4 118.6(5) . . ?
Cu6 O11 Cu7 118.7(3) . . ?
C40 O11 Cu6 113.3(6) . . ?
C40 O11 Cu7 127.6(6) . . ?
Cu6 O12 H12 143(2) . . ?
C42 O12 Cu6 104.6(6) . . ?
C42 O12 H12 111(2) . . ?
Cu7 O13 Cu8 115.5(3) . . ?
C43 O13 Cu7 126.1(7) . . ?
C43 O13 Cu8 110.0(6) . . ?
N7 O14 Cu6 117.4(5) . . ?
Cu1 O15 Cu8 118.1(3) . . ?
C54 O15 Cu1 127.8(7) . . ?
C54 O15 Cu8 113.8(6) . . ?
Cu8 O16 H16 145(2) . . ?
C56 O16 Cu8 104.3(6) . . ?
C56 O16 H16 109(2) . . ?
O2 N1 Cu1 119.2(6) . . ?
C7 N1 Cu1 127.3(7) . . ?
C7 N1 O2 112.8(8) . . ?
C10 N2 Cu2 113.9(6) . . ?
C10 N2 C13 109.8(8) . . ?
C11 N2 Cu2 101.9(6) . . ?
C11 N2 C10 111.8(8) . . ?
C11 N2 C13 110.4(8) . . ?
C13 N2 Cu2 108.9(6) . . ?
O6 N3 Cu3 117.4(5) . . ?
C21 N3 Cu3 129.1(7) . . ?
C21 N3 O6 112.9(8) . . ?
C24 N4 Cu4 113.2(6) . . ?
C25 N4 Cu4 101.8(6) . . ?
C25 N4 C24 111.5(8) . . ?
C25 N4 C27 112.0(8) . . ?
C27 N4 Cu4 108.1(6) . . ?
C27 N4 C24 110.1(8) . . ?
O10 N5 Cu5 117.6(6) . . ?
C35 N5 Cu5 127.6(7) . . ?
C35 N5 O10 114.3(8) . . ?
C38 N6 Cu6 113.9(6) . . ?
C39 N6 Cu6 101.9(6) . . ?
C39 N6 C38 111.2(8) . . ?
C39 N6 C41 108.9(8) . . ?
C41 N6 Cu6 109.2(7) . . ?
C41 N6 C38 111.2(8) . . ?
O14 N7 Cu7 119.1(6) . . ?
C49 N7 Cu7 128.0(7) . . ?
C49 N7 O14 112.4(8) . . ?
C52 N8 Cu8 113.1(6) . . ?
C53 N8 Cu8 103.5(6) . . ?
C53 N8 C52 109.7(8) . . ?
C55 N8 Cu8 109.6(7) . . ?
C55 N8 C52 109.6(8) . . ?
C55 N8 C53 111.3(9) . . ?
O1 C1 C2 118.7(9) . . ?
O1 C1 C6 122.7(9) . . ?
C2 C1 C6 118.6(9) . . ?
C1 C2 C10 117.8(9) . . ?
C3 C2 C1 119.8(10) . . ?
C3 C2 C10 122.3(9) . . ?
C2 C3 H3 118.6 . . ?
C2 C3 C4 122.8(10) . . ?
C4 C3 H3 118.6 . . ?
C3 C4 C9 119.9(10) . . ?
C5 C4 C3 117.2(10) . . ?
C5 C4 C9 122.8(11) . . ?
C4 C5 H5 118.4 . . ?
C4 C5 C6 123.2(10) . . ?
C6 C5 H5 118.4 . . ?
C1 C6 C7 122.3(9) . . ?
C5 C6 C1 117.9(9) . . ?
C5 C6 C7 119.7(9) . . ?
N1 C7 C6 120.7(9) . . ?
N1 C7 C8 119.1(9) . . ?
C6 C7 C8 120.1(9) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C2 113.3(8) . . ?
N2 C10 H10A 108.9 . . ?
N2 C10 H10B 108.9 . . ?
C2 C10 H10A 108.9 . . ?
C2 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
N2 C11 H11A 109.6 . . ?
N2 C11 H11B 109.6 . . ?
N2 C11 C12 110.3(8) . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 H11A 109.6 . . ?
C12 C11 H11B 109.6 . . ?
O3 C12 C11 108.8(8) . . ?
O3 C12 H12A 109.9 . . ?
O3 C12 H12B 109.9 . . ?
C11 C12 H12A 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
N2 C13 H13A 109.4 . . ?
N2 C13 H13B 109.4 . . ?
N2 C13 C14 111.2(9) . . ?
H13A C13 H13B 108.0 . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
O4 C14 C13 107.6(9) . . ?
O4 C14 H14A 110.2 . . ?
O4 C14 H14B 110.2 . . ?
C13 C14 H14A 110.2 . . ?
C13 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
O5 C15 C16 117.5(9) . . ?
O5 C15 C20 123.6(9) . . ?
C20 C15 C16 118.9(9) . . ?
C15 C16 C24 118.9(9) . . ?
C17 C16 C15 120.2(9) . . ?
C17 C16 C24 120.9(9) . . ?
C16 C17 H17 119.2 . . ?
C16 C17 C18 121.6(9) . . ?
C18 C17 H17 119.2 . . ?
C17 C18 C23 117.6(10) . . ?
C19 C18 C17 117.4(10) . . ?
C19 C18 C23 124.9(10) . . ?
C18 C19 H19 117.4 . . ?
C18 C19 C20 125.1(10) . . ?
C20 C19 H19 117.4 . . ?
C15 C20 C21 122.2(9) . . ?
C19 C20 C15 116.6(9) . . ?
C19 C20 C21 121.2(9) . . ?
N3 C21 C20 120.2(9) . . ?
N3 C21 C22 118.8(9) . . ?
C20 C21 C22 121.0(9) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 H24A 109.3 . . ?
N4 C24 H24B 109.3 . . ?
C16 C24 N4 111.5(8) . . ?
C16 C24 H24A 109.3 . . ?
C16 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?
N4 C25 H25A 109.8 . . ?
N4 C25 H25B 109.8 . . ?
N4 C25 C26 109.3(9) . . ?
H25A C25 H25B 108.3 . . ?
C26 C25 H25A 109.8 . . ?
C26 C25 H25B 109.8 . . ?
O7 C26 C25 109.6(8) . . ?
O7 C26 H26 125.2 . . ?
C25 C26 H26 125.2 . . ?
N4 C27 H27A 109.3 . . ?
N4 C27 H27B 109.3 . . ?
N4 C27 C28 111.5(8) . . ?
H27A C27 H27B 108.0 . . ?
C28 C27 H27A 109.3 . . ?
C28 C27 H27B 109.3 . . ?
O8 C28 C27 109.6(9) . . ?
O8 C28 H28A 109.8 . . ?
O8 C28 H28B 109.8 . . ?
C27 C28 H28A 109.8 . . ?
C27 C28 H28B 109.8 . . ?
H28A C28 H28B 108.2 . . ?
O9 C29 C30 117.3(9) . . ?
O9 C29 C34 122.2(9) . . ?
C30 C29 C34 120.5(9) . . ?
C29 C30 C38 120.5(10) . . ?
C31 C30 C29 119.7(10) . . ?
C31 C30 C38 119.8(10) . . ?
C30 C31 H31 119.4 . . ?
C30 C31 C32 121.3(10) . . ?
C32 C31 H31 119.4 . . ?
C31 C32 C33 119.3(11) . . ?
C31 C32 C37 120.7(11) . . ?
C33 C32 C37 120.1(12) . . ?
C32 C33 H33 119.4 . . ?
C32 C33 C34 121.3(11) . . ?
C34 C33 H33 119.4 . . ?
C29 C34 C35 122.1(9) . . ?
C33 C34 C29 117.7(9) . . ?
C33 C34 C35 120.1(9) . . ?
N5 C35 C34 121.8(9) . . ?
N5 C35 C36 118.9(9) . . ?
C34 C35 C36 119.2(9) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N6 C38 H38A 108.8 . . ?
N6 C38 H38B 108.8 . . ?
C30 C38 N6 113.6(8) . . ?
C30 C38 H38A 108.8 . . ?
C30 C38 H38B 108.8 . . ?
H38A C38 H38B 107.7 . . ?
N6 C39 H39A 109.9 . . ?
N6 C39 H39B 109.9 . . ?
N6 C39 C40 109.1(8) . . ?
H39A C39 H39B 108.3 . . ?
C40 C39 H39A 109.9 . . ?
C40 C39 H39B 109.9 . . ?
O11 C40 C39 110.5(9) . . ?
O11 C40 H40A 109.6 . . ?
O11 C40 H40B 109.6 . . ?
C39 C40 H40A 109.6 . . ?
C39 C40 H40B 109.6 . . ?
H40A C40 H40B 108.1 . . ?
N6 C41 H41A 109.6 . . ?
N6 C41 H41B 109.6 . . ?
N6 C41 C42 110.1(8) . . ?
H41A C41 H41B 108.2 . . ?
C42 C41 H41A 109.6 . . ?
C42 C41 H41B 109.6 . . ?
O12 C42 C41 108.1(9) . . ?
O12 C42 H42A 110.1 . . ?
O12 C42 H42B 110.1 . . ?
C41 C42 H42A 110.1 . . ?
C41 C42 H42B 110.1 . . ?
H42A C42 H42B 108.4 . . ?
O13 C43 C44 117.6(10) . . ?
O13 C43 C48 123.8(9) . . ?
C48 C43 C44 118.5(10) . . ?
C43 C44 C52 119.4(10) . . ?
C45 C44 C43 118.9(11) . . ?
C45 C44 C52 121.7(11) . . ?
C44 C45 H45 118.0 . . ?
C44 C45 C46 124.0(12) . . ?
C46 C45 H45 118.0 . . ?
C45 C46 C51 122.2(12) . . ?
C47 C46 C45 115.6(11) . . ?
C47 C46 C51 122.2(12) . . ?
C46 C47 H47 118.7 . . ?
C46 C47 C48 122.5(11) . . ?
C48 C47 H47 118.7 . . ?
C43 C48 C47 120.0(11) . . ?
C43 C48 C49 120.4(10) . . ?
C47 C48 C49 119.5(10) . . ?
N7 C49 C48 121.2(9) . . ?
N7 C49 C50 119.2(10) . . ?
C50 C49 C48 119.5(9) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C46 C51 H51A 109.5 . . ?
C46 C51 H51B 109.5 . . ?
C46 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N8 C52 H52A 109.1 . . ?
N8 C52 H52B 109.1 . . ?
C44 C52 N8 112.6(8) . . ?
C44 C52 H52A 109.1 . . ?
C44 C52 H52B 109.1 . . ?
H52A C52 H52B 107.8 . . ?
N8 C53 H53A 109.9 . . ?
N8 C53 H53B 109.9 . . ?
N8 C53 C54 108.7(9) . . ?
H53A C53 H53B 108.3 . . ?
C54 C53 H53A 109.9 . . ?
C54 C53 H53B 109.9 . . ?
O15 C54 C53 108.5(9) . . ?
O15 C54 H54A 110.0 . . ?
O15 C54 H54B 110.0 . . ?
C53 C54 H54A 110.0 . . ?
C53 C54 H54B 110.0 . . ?
H54A C54 H54B 108.4 . . ?
N8 C55 H55A 109.2 . . ?
N8 C55 H55B 109.2 . . ?
N8 C55 C56 112.1(9) . . ?
H55A C55 H55B 107.9 . . ?
C56 C55 H55A 109.2 . . ?
C56 C55 H55B 109.2 . . ?
O16 C56 C55 108.9(9) . . ?
O16 C56 H56A 109.9 . . ?
O16 C56 H56B 109.9 . . ?
C55 C56 H56A 109.9 . . ?
C55 C56 H56B 109.9 . . ?
H56A C56 H56B 108.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 C1 C2 -153.5(7) . . . . ?
Cu1 O1 C1 C6 28.8(12) . . . . ?
Cu1 O15 C54 C53 158.5(7) . . . . ?
Cu1 N1 C7 C6 6.9(13) . . . . ?
Cu1 N1 C7 C8 -168.6(7) . . . . ?
Cu2 O1 C1 C2 58.9(10) . . . . ?
Cu2 O1 C1 C6 -118.8(8) . . . . ?
Cu2 O3 C12 C11 13.9(10) . . . . ?
Cu2 O4 C14 C13 35.7(10) . . . . ?
Cu2 O6 N3 Cu3 19.4(8) . . . . ?
Cu2 O6 N3 C21 -168.8(6) . . . . ?
Cu2 N2 C10 C2 45.0(10) . . . . ?
Cu2 N2 C11 C12 44.5(9) . . . . ?
Cu2 N2 C13 C14 48.5(10) . . . . ?
Cu3 O3 C12 C11 -155.8(7) . . . . ?
Cu3 O5 C15 C16 153.5(7) . . . . ?
Cu3 O5 C15 C20 -27.4(12) . . . . ?
Cu3 N3 C21 C20 -8.6(13) . . . . ?
Cu3 N3 C21 C22 169.8(7) . . . . ?
Cu4 O5 C15 C16 -63.1(9) . . . . ?
Cu4 O5 C15 C20 116.0(8) . . . . ?
Cu4 O7 C26 C25 -16.9(11) . . . . ?
Cu4 O8 C28 C27 -31.9(9) . . . . ?
Cu4 O10 N5 Cu5 -22.8(8) . . . . ?
Cu4 O10 N5 C35 165.3(7) . . . . ?
Cu4 N4 C24 C16 -46.3(9) . . . . ?
Cu4 N4 C25 C26 -44.6(9) . . . . ?
Cu4 N4 C27 C28 -49.6(10) . . . . ?
Cu5 O7 C26 C25 154.5(7) . . . . ?
Cu5 O9 C29 C30 -150.4(7) . . . . ?
Cu5 O9 C29 C34 30.8(13) . . . . ?
Cu5 N5 C35 C34 8.0(14) . . . . ?
Cu5 N5 C35 C36 -167.5(7) . . . . ?
Cu6 O9 C29 C30 60.2(10) . . . . ?
Cu6 O9 C29 C34 -118.6(9) . . . . ?
Cu6 O11 C40 C39 14.7(11) . . . . ?
Cu6 O12 C42 C41 35.9(10) . . . . ?
Cu6 O14 N7 Cu7 21.1(9) . . . . ?
Cu6 O14 N7 C49 -166.4(7) . . . . ?
Cu6 N6 C38 C30 44.2(10) . . . . ?
Cu6 N6 C39 C40 44.0(9) . . . . ?
Cu6 N6 C41 C42 50.5(10) . . . . ?
Cu7 O11 C40 C39 -157.6(7) . . . . ?
Cu7 O13 C43 C44 155.5(7) . . . . ?
Cu7 O13 C43 C48 -28.6(13) . . . . ?
Cu7 N7 C49 C48 -6.3(14) . . . . ?
Cu7 N7 C49 C50 171.1(7) . . . . ?
Cu8 O2 N1 Cu1 -25.1(8) . . . . ?
Cu8 O2 N1 C7 164.1(6) . . . . ?
Cu8 O13 C43 C44 -58.1(10) . . . . ?
Cu8 O13 C43 C48 117.7(9) . . . . ?
Cu8 O15 C54 C53 -14.7(11) . . . . ?
Cu8 O16 C56 C55 -33.2(10) . . . . ?
Cu8 N8 C52 C44 -44.8(11) . . . . ?
Cu8 N8 C53 C54 -46.0(9) . . . . ?
Cu8 N8 C55 C56 -47.3(11) . . . . ?
Cl1 Cu1 O15 Cu8 -175.9(4) . . . . ?
Cl1 Cu1 O15 C54 11.0(9) . . . . ?
O1 Cu2 O3 Cu3 90.5(7) . . . . ?
O1 Cu2 O3 C12 -80.2(9) . . . . ?
O1 Cu2 O6 N3 -166.5(6) . . . . ?
O1 C1 C2 C3 177.3(9) . . . . ?
O1 C1 C2 C10 1.5(13) . . . . ?
O1 C1 C6 C5 -175.7(9) . . . . ?
O1 C1 C6 C7 8.0(14) . . . . ?
O2 Cu8 O15 Cu1 -1.3(5) . . . . ?
O2 Cu8 O15 C54 172.7(7) . . . . ?
O2 N1 C7 C6 176.9(8) . . . . ?
O2 N1 C7 C8 1.3(12) . . . . ?
O3 Cu2 O6 N3 -11.3(6) . . . . ?
O4 Cu2 O3 Cu3 -100.4(4) . . . . ?
O4 Cu2 O3 C12 88.9(7) . . . . ?
O4 Cu2 O6 N3 95.5(6) . . . . ?
O5 Cu4 O7 Cu5 -89.6(7) . . . . ?
O5 Cu4 O7 C26 82.5(9) . . . . ?
O5 Cu4 O10 N5 166.5(6) . . . . ?
O5 C15 C16 C17 -176.4(8) . . . . ?
O5 C15 C16 C24 1.6(13) . . . . ?
O5 C15 C20 C19 177.1(8) . . . . ?
O5 C15 C20 C21 -6.6(14) . . . . ?
O6 Cu2 O3 Cu3 -1.0(4) . . . . ?
O6 Cu2 O3 C12 -171.6(7) . . . . ?
O6 N3 C21 C20 -179.3(8) . . . . ?
O6 N3 C21 C22 -0.8(12) . . . . ?
O7 Cu4 O10 N5 12.9(7) . . . . ?
O8 Cu4 O7 Cu5 103.3(4) . . . . ?
O8 Cu4 O7 C26 -84.5(7) . . . . ?
O8 Cu4 O10 N5 -99.3(6) . . . . ?
O9 Cu6 O11 Cu7 92.2(7) . . . . ?
O9 Cu6 O11 C40 -80.8(9) . . . . ?
O9 Cu6 O14 N7 -166.2(6) . . . . ?
O9 C29 C30 C31 177.9(9) . . . . ?
O9 C29 C30 C38 -1.3(15) . . . . ?
O9 C29 C34 C33 -174.8(9) . . . . ?
O9 C29 C34 C35 5.8(15) . . . . ?
O10 Cu4 O7 Cu5 1.6(4) . . . . ?
O10 Cu4 O7 C26 173.8(7) . . . . ?
O10 N5 C35 C34 178.9(8) . . . . ?
O10 N5 C35 C36 3.4(13) . . . . ?
O11 Cu6 O14 N7 -12.3(7) . . . . ?
O12 Cu6 O11 Cu7 -98.7(4) . . . . ?
O12 Cu6 O11 C40 88.2(7) . . . . ?
O12 Cu6 O14 N7 94.7(6) . . . . ?
O13 Cu8 O2 N1 171.0(6) . . . . ?
O13 Cu8 O15 Cu1 -92.5(7) . . . . ?
O13 Cu8 O15 C54 81.4(10) . . . . ?
O13 C43 C44 C45 -179.5(10) . . . . ?
O13 C43 C44 C52 -2.6(15) . . . . ?
O13 C43 C48 C47 176.6(10) . . . . ?
O13 C43 C48 C49 -7.2(15) . . . . ?
O14 Cu6 O11 Cu7 -0.4(4) . . . . ?
O14 Cu6 O11 C40 -173.5(7) . . . . ?
O14 N7 C49 C48 -178.0(8) . . . . ?
O14 N7 C49 C50 -0.6(13) . . . . ?
O15 Cu8 O2 N1 15.5(6) . . . . ?
O16 Cu8 O2 N1 -92.2(6) . . . . ?
O16 Cu8 O15 Cu1 97.2(4) . . . . ?
O16 Cu8 O15 C54 -88.8(8) . . . . ?
N1 Cu1 O15 Cu8 -7.8(4) . . . . ?
N1 Cu1 O15 C54 179.2(9) . . . . ?
N2 Cu2 O3 Cu3 -179.9(4) . . . . ?
N2 Cu2 O3 C12 9.4(7) . . . . ?
N2 C11 C12 O3 -40.2(11) . . . . ?
N2 C13 C14 O4 -57.5(12) . . . . ?
N4 Cu4 O7 Cu5 -179.4(4) . . . . ?
N4 Cu4 O7 C26 -7.3(7) . . . . ?
N4 C25 C26 O7 42.5(11) . . . . ?
N4 C27 C28 O8 56.9(12) . . . . ?
N6 Cu6 O11 Cu7 -177.9(4) . . . . ?
N6 Cu6 O11 C40 9.1(7) . . . . ?
N6 C39 C40 O11 -40.6(11) . . . . ?
N6 C41 C42 O12 -59.0(12) . . . . ?
N8 Cu8 O15 Cu1 176.9(5) . . . . ?
N8 Cu8 O15 C54 -9.1(8) . . . . ?
N8 C53 C54 O15 41.1(12) . . . . ?
N8 C55 C56 O16 55.6(13) . . . . ?
C1 C2 C3 C4 -1.6(15) . . . . ?
C1 C2 C10 N2 -60.3(12) . . . . ?
C1 C6 C7 N1 -26.2(14) . . . . ?
C1 C6 C7 C8 149.3(9) . . . . ?
C2 C1 C6 C5 6.5(13) . . . . ?
C2 C1 C6 C7 -169.8(9) . . . . ?
C2 C3 C4 C5 6.1(15) . . . . ?
C2 C3 C4 C9 -176.3(11) . . . . ?
C3 C2 C10 N2 124.0(10) . . . . ?
C3 C4 C5 C6 -4.2(16) . . . . ?
C4 C5 C6 C1 -2.0(15) . . . . ?
C4 C5 C6 C7 174.4(9) . . . . ?
C5 C6 C7 N1 157.6(9) . . . . ?
C5 C6 C7 C8 -26.9(13) . . . . ?
C6 C1 C2 C3 -4.8(14) . . . . ?
C6 C1 C2 C10 179.3(8) . . . . ?
C9 C4 C5 C6 178.2(11) . . . . ?
C10 N2 C11 C12 166.5(8) . . . . ?
C10 N2 C13 C14 -76.9(11) . . . . ?
C10 C2 C3 C4 174.0(9) . . . . ?
C11 N2 C10 C2 -69.8(11) . . . . ?
C11 N2 C13 C14 159.5(9) . . . . ?
C13 N2 C10 C2 167.4(9) . . . . ?
C13 N2 C11 C12 -71.0(10) . . . . ?
C15 C16 C17 C18 -1.7(15) . . . . ?
C15 C16 C24 N4 60.9(11) . . . . ?
C15 C20 C21 N3 24.7(14) . . . . ?
C15 C20 C21 C22 -153.8(10) . . . . ?
C16 C15 C20 C19 -3.7(13) . . . . ?
C16 C15 C20 C21 172.5(9) . . . . ?
C16 C17 C18 C19 -1.4(15) . . . . ?
C16 C17 C18 C23 177.2(10) . . . . ?
C17 C16 C24 N4 -121.0(10) . . . . ?
C17 C18 C19 C20 2.0(16) . . . . ?
C18 C19 C20 C15 0.6(15) . . . . ?
C18 C19 C20 C21 -175.7(10) . . . . ?
C19 C20 C21 N3 -159.3(9) . . . . ?
C19 C20 C21 C22 22.3(14) . . . . ?
C20 C15 C16 C17 4.4(14) . . . . ?
C20 C15 C16 C24 -177.6(9) . . . . ?
C23 C18 C19 C20 -176.5(10) . . . . ?
C24 N4 C25 C26 -165.6(8) . . . . ?
C24 N4 C27 C28 74.5(11) . . . . ?
C24 C16 C17 C18 -179.8(9) . . . . ?
C25 N4 C24 C16 67.8(10) . . . . ?
C25 N4 C27 C28 -160.9(9) . . . . ?
C27 N4 C24 C16 -167.3(8) . . . . ?
C27 N4 C25 C26 70.5(11) . . . . ?
C29 C30 C31 C32 -1.5(16) . . . . ?
C29 C30 C38 N6 -57.6(13) . . . . ?
C29 C34 C35 N5 -25.6(15) . . . . ?
C29 C34 C35 C36 149.9(10) . . . . ?
C30 C29 C34 C33 6.5(15) . . . . ?
C30 C29 C34 C35 -173.0(10) . . . . ?
C30 C31 C32 C33 2.9(16) . . . . ?
C30 C31 C32 C37 -177.6(11) . . . . ?
C31 C30 C38 N6 123.2(10) . . . . ?
C31 C32 C33 C34 0.5(16) . . . . ?
C32 C33 C34 C29 -5.1(15) . . . . ?
C32 C33 C34 C35 174.4(10) . . . . ?
C33 C34 C35 N5 154.9(10) . . . . ?
C33 C34 C35 C36 -29.6(14) . . . . ?
C34 C29 C30 C31 -3.3(15) . . . . ?
C34 C29 C30 C38 177.5(9) . . . . ?
C37 C32 C33 C34 -178.9(11) . . . . ?
C38 N6 C39 C40 165.8(8) . . . . ?
C38 N6 C41 C42 -76.1(11) . . . . ?
C38 C30 C31 C32 177.7(10) . . . . ?
C39 N6 C38 C30 -70.3(10) . . . . ?
C39 N6 C41 C42 161.0(9) . . . . ?
C41 N6 C38 C30 168.1(9) . . . . ?
C41 N6 C39 C40 -71.3(10) . . . . ?
C43 C44 C45 C46 2.5(19) . . . . ?
C43 C44 C52 N8 62.0(13) . . . . ?
C43 C48 C49 N7 24.6(15) . . . . ?
C43 C48 C49 C50 -152.8(10) . . . . ?
C44 C43 C48 C47 -7.6(15) . . . . ?
C44 C43 C48 C49 168.6(9) . . . . ?
C44 C45 C46 C47 -5.8(19) . . . . ?
C44 C45 C46 C51 174.3(12) . . . . ?
C45 C44 C52 N8 -121.1(12) . . . . ?
C45 C46 C47 C48 2.3(18) . . . . ?
C46 C47 C48 C43 4.3(17) . . . . ?
C46 C47 C48 C49 -171.9(10) . . . . ?
C47 C48 C49 N7 -159.2(10) . . . . ?
C47 C48 C49 C50 23.4(15) . . . . ?
C48 C43 C44 C45 4.4(16) . . . . ?
C48 C43 C44 C52 -178.6(10) . . . . ?
C51 C46 C47 C48 -177.8(12) . . . . ?
C52 N8 C53 C54 -167.0(8) . . . . ?
C52 N8 C55 C56 77.3(11) . . . . ?
C52 C44 C45 C46 -174.5(11) . . . . ?
C53 N8 C52 C44 70.2(11) . . . . ?
C53 N8 C55 C56 -161.2(9) . . . . ?
C55 N8 C52 C44 -167.4(10) . . . . ?
C55 N8 C53 C54 71.6(11) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
29 -16 -5 0.1781 28.9997 -16.0000 -4.9999 -0.8146 0.3882 -0.4089
-22 21 11 0.1798 -21.9998 21.0000 10.9999 0.6792 -0.3069 0.6574
-35 -4 -11 0.1574 -34.9995 -4.0000 -11.0000 0.8356 -0.4003 -0.4017
-23 -19 -19 0.1946 -22.9996 -19.0000 -19.0000 0.4469 -0.2116 -0.8908
21 20 19 0.1752 20.9996 20.0000 19.0000 -0.3933 0.1801 0.9125
35 2 9 0.1845 34.9995 2.0000 9.0000 -0.8521 0.3962 0.3198
-11 -2 43 0.1068 -11.0000 -2.0000 42.9999 0.5904 0.7493 0.2903
-13 -26 8 0.2213 -12.9998 -26.0000 8.0000 0.3675 0.4803 -0.8065
-14 -13 37 0.1567 -13.9999 -13.0000 36.9999 0.6139 0.7969 -0.1275
6 -8 -43 0.1572 6.0001 -8.0000 -42.9999 -0.4708 -0.6217 -0.6296
-6 -25 -20 0.2426 -5.9998 -25.0000 -19.9999 -0.0130 -0.0039 -1.0059
12 5 -42 0.1305 12.0000 5.0000 -41.9999 -0.6061 -0.7728 -0.1815
0 -2 45 0.1096 -0.0002 -2.0000 44.9999 0.3160 0.8688 0.3632
-6 -25 21 0.2039 -5.9999 -25.0000 21.0000 0.2770 0.7576 -0.6176
1 8 -44 0.1283 1.0001 8.0000 -43.9999 -0.3283 -0.9418 -0.1599
-3 -10 -42 0.1590 -2.9998 -10.0000 -41.9999 -0.2300 -0.6376 -0.7272
16 9 38 0.1519 15.9996 9.0000 37.9999 -0.1404 0.6771 0.7216
17 -4 40 0.1291 16.9996 -4.0000 40.0000 -0.1676 0.9362 0.3362
10 -24 19 0.1906 9.9999 -24.0000 19.0000 -0.1557 0.8238 -0.5266
-15 -12 -37 0.1649 -14.9996 -12.0000 -36.9999 0.1178 -0.6015 -0.8017
-17 4 -40 0.1447 -16.9996 4.0000 -40.0000 0.1676 -0.9362 -0.3362
-16 12 -35 0.1673 -15.9997 12.0000 -35.0000 0.1860 -0.9679 -0.0321
26 5 30 0.1538 25.9995 5.0000 30.0000 -0.4640 0.6693 0.5690
28 -10 24 0.1560 27.9996 -10.0000 24.0000 -0.5762 0.8204 0.0497
-25 -5 31 0.1328 -24.9998 -5.0000 30.9999 0.8693 0.4711 0.0136
-20 5 36 0.1365 -19.9999 5.0000 35.9999 0.7851 0.4364 0.4003
23 20 -11 0.1847 22.9997 20.0000 -11.0000 -0.6580 -0.3621 0.6382
22 -4 -36 0.1358 21.9999 -4.0000 -35.9999 -0.8364 -0.4380 -0.3590
26 12 -25 0.1551 25.9997 12.0000 -24.9999 -0.8450 -0.4677 0.2685
-26 16 -19 0.1778 -25.9996 16.0000 -19.0000 0.5661 -0.8115 0.1963
-27 -1 -29 0.1393 -26.9995 -1.0000 -29.0000 0.5019 -0.7243 -0.4385

_olex2_date_sample_data_collection 5/11/13
_olex2_date_sample_submission    24/10/13
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Desktop Cooler'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_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_eb3252
_database_code_depnum_ccdc_archive 'CCDC 991824'
_audit_update_record             
;
2015-03-27 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
_audit_creation_date             2013-11-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2013-4
_publ_section_exptl              
;
Any special experimental details
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H76 Cl0.79 Cu8 N11.21 O25.62'
_chemical_formula_sum            'C56 H76 Cl0.79 Cu8 N11.21 O25.62'
_chemical_formula_weight         1852.53
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40 H80 N10 O20 Cu2'
_chemical_oxdiff_usercomment     '@ 170 K RS30/PS'
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'
Cl Cl 0.1484 0.1585 '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      hexagonal
_space_group_IT_number           171
_space_group_name_H-M_alt        'P 62'
_space_group_name_Hall           'P 62'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z'
'y, -x+y, z+2/3'
'x-y, x, z+1/3'

_cell_length_a                   20.2162(4)
_cell_length_b                   20.2162(4)
_cell_length_c                   16.8492(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5963.6(3)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    13218
_cell_measurement_temperature    170
_cell_measurement_theta_max      22.2360
_cell_measurement_theta_min      3.4920
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.199
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2823
_exptl_crystal_recrystallization_method 
'From diffusion of diethyl ether, methanol and acetonitrile.'
_exptl_crystal_size_length       0.000
_exptl_crystal_size_max          0.6545
_exptl_crystal_size_mid          0.1271
_exptl_crystal_size_min          0.084
_exptl_crystal_size_rad          0.000
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.720
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            74631
_diffrn_reflns_point_group_measured_fraction_full 0.718
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.460
_diffrn_reflns_theta_min         3.078
_diffrn_ambient_temperature      170
_diffrn_detector                 Eos
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9963
_diffrn_measured_fraction_theta_max 0.9967
_diffrn_measurement_device       'Agilent Technologies XCalibur'
_diffrn_measurement_device_type  'Agilent Technologies XCalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0113346000
_diffrn_orient_matrix_UB_12      0.0389124000
_diffrn_orient_matrix_UB_13      -0.0065287000
_diffrn_orient_matrix_UB_21      -0.0381831000
_diffrn_orient_matrix_UB_22      -0.0085014000
_diffrn_orient_matrix_UB_23      0.0060941000
_diffrn_orient_matrix_UB_31      0.0074484000
_diffrn_orient_matrix_UB_32      0.0074311000
_diffrn_orient_matrix_UB_33      0.0411292000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.715
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4751
_reflns_number_total             5175
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     22.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    
;
Olex2
;
_computing_publication_material  
;
Olex2
;
_computing_structure_refinement  
;
ShelXL
;
_computing_structure_solution    
;
Superflip
;
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 
;
 Flack x determined using 2144 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.010(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         5175
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0378
_refine_ls_restrained_S_all      1.089
_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)+(0.0797P)²+2.0020P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1126
_refine_special_details          
;
Ligand bonded to Cu2 is a disordered mix of nitrate (N6) and chloride (Cl1') 
in ratio 0.59:0.41.  The data set was cut at a resolution of 0.93 A during 
processing since R(int) began to rise rapidly after this point.  

#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..      22.46 Deg.

Data set cut as noted above.

090_ALERT_3_A Poor Data / Parameter Ratio (Zmax > 18) ........       5.58

This is an odd error.  There are 5175 unique reflections and 483 parameters as
reported by SHELXL.  That's a d/p ratio of 10.7.  

602_ALERT_2_A VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info

There are no missing solvent molecules and SQUEEZE was not used.

#===============================================================================
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............     0.0165 Ang.
#===============================================================================
041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ     Please Check
068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...     Please Check
077_ALERT_4_C Unitcell contains non-integer number of atoms ..     Please Check

Rounding errors resulting from substitutional disorder.

094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.49
220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...        3.8 Ratio
241_ALERT_2_C High      Ueq as Compared to Neighbors for .....        O10 Check
242_ALERT_2_C Low       Ueq as Compared to Neighbors for .....        Cu2 Check
242_ALERT_2_C Low       Ueq as Compared to Neighbors for .....         N5 Check

Insignificant. 
#===============================================================================

;


# start Validation Reply Form
_vrf_THETM01_eb3252              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Please see the _refine_special_details section of the CIF.
;
_vrf_PLAT602_eb3252              
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: There are no missing solvent molecules and SQUEEZE was not used.
;
# end Validation Reply Form


_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 Cu2, O15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Sof(Cl1')=1-FVAR(1)
 Sof(O13)=Sof(O14)=Sof(O15)=Sof(N6)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C00W(H00A,H00B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,
 H13B), C14(H14A,H14B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C17(H17), C19(H19)
4.c Tetrahedral OH refined with riding coordinates:
 O3(H3), O7(H7)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.26699(7) 0.34094(7) 0.29930(7) 0.0330(3) Uani 1 1 d . . . . .
Cu2 Cu 0.36262(7) 0.27443(7) 0.38869(7) 0.0333(3) Uani 1 1 d . U . . .
Cu3 Cu 0.54707(7) 0.33483(7) 0.41981(7) 0.0285(3) Uani 1 1 d . . . . .
Cu4 Cu 0.68227(7) 0.48354(7) 0.33398(7) 0.0305(3) Uani 1 1 d . . . . .
Cl1' Cl 0.3543(11) 0.1594(10) 0.3565(16) 0.057(6) Uani 0.40(3) 1 d . . P A 2
O1 O 0.2836(4) 0.4394(4) 0.2537(4) 0.0308(16) Uani 1 1 d . . . . .
O2 O 0.4786(4) 0.6241(4) 0.3332(4) 0.0367(17) Uani 1 1 d . . . . .
O3 O 0.1470(5) 0.2941(5) 0.3643(5) 0.053(2) Uani 1 1 d . . . . .
H3 H 0.1517 0.3362 0.3783 0.064 Uiso 1 1 calc R U . . .
O4 O 0.2942(4) 0.2643(4) 0.3077(4) 0.0413(19) Uani 1 1 d . . . . .
O5 O 0.3307(4) 0.3987(4) 0.3848(4) 0.0385(18) Uani 1 1 d . . . . .
O6 O 0.4423(4) 0.2940(4) 0.4618(4) 0.0318(16) Uani 1 1 d . . . . .
O7 O 0.5212(5) 0.2212(4) 0.3543(4) 0.046(2) Uani 1 1 d . . . . .
H7 H 0.4771 0.1956 0.3351 0.055 Uiso 1 1 calc R U . . .
O8 O 0.6518(4) 0.4084(4) 0.4138(4) 0.0350(17) Uani 1 1 d . . . . .
O9 O 0.7877(4) 0.5457(4) 0.3791(4) 0.0395(18) Uani 1 1 d . . . . .
O10 O 0.8020(5) 0.4731(6) 0.2968(6) 0.059(2) Uani 1 1 d . . . . .
O11 O 0.9003(5) 0.5735(6) 0.3435(6) 0.070(3) Uani 1 1 d . . . . .
O13 O 0.3318(14) 0.0738(10) 0.4139(16) 0.117(10) Uani 0.60(3) 1 d . . P A 1
O14 O 0.2839(11) 0.1430(11) 0.4517(14) 0.099(9) Uani 0.60(3) 1 d . . P A 1
O15 O 0.372(2) 0.1893(15) 0.357(3) 0.069(10) Uani 0.60(3) 1 d . U P A 1
N1 N 0.4202(5) 0.5725(5) 0.2862(5) 0.029(2) Uani 1 1 d . . . . .
N2 N 0.1966(5) 0.2784(5) 0.2111(5) 0.039(2) Uani 1 1 d . . . . .
N3 N 0.3565(5) 0.3622(5) 0.4326(5) 0.032(2) Uani 1 1 d . . . . .
N4 N 0.5756(5) 0.2869(5) 0.5073(5) 0.032(2) Uani 1 1 d . . . . .
N5 N 0.8290(5) 0.5279(6) 0.3372(5) 0.036(2) Uani 1 1 d . . . . .
N6 N 0.3269(14) 0.1323(14) 0.409(2) 0.062(6) Uani 0.60(3) 1 d . . P A 1
C00W C 0.5151(6) 0.2480(6) 0.5676(6) 0.034(2) Uani 1 1 d . . . . .
H00A H 0.5373 0.2367 0.6144 0.041 Uiso 1 1 calc R U . . .
H00B H 0.4751 0.1987 0.5455 0.041 Uiso 1 1 calc R U . . .
C1 C 0.3130(6) 0.4466(6) 0.1800(6) 0.029(2) Uani 1 1 d . . . . .
C2 C 0.2682(6) 0.3914(6) 0.1233(6) 0.032(2) Uani 1 1 d . . . . .
C3 C 0.2957(7) 0.3967(7) 0.0478(6) 0.037(3) Uani 1 1 d . . . . .
H3A H 0.2648 0.3587 0.0103 0.044 Uiso 1 1 calc R U . . .
C4 C 0.3666(7) 0.4551(7) 0.0240(6) 0.037(3) Uani 1 1 d . . . . .
C5 C 0.4102(6) 0.5085(6) 0.0796(6) 0.034(2) Uani 1 1 d . . . . .
H5 H 0.4586 0.5493 0.0635 0.040 Uiso 1 1 calc R U . . .
C6 C 0.3880(6) 0.5070(6) 0.1603(6) 0.031(2) Uani 1 1 d . . . . .
C7 C 0.4415(6) 0.5616(5) 0.2165(6) 0.028(2) Uani 1 1 d . . . . .
C8 C 0.5260(6) 0.6062(6) 0.1979(6) 0.036(3) Uani 1 1 d . . . . .
H8A H 0.5437 0.6610 0.1995 0.054 Uiso 1 1 calc R U . . .
H8B H 0.5350 0.5923 0.1449 0.054 Uiso 1 1 calc R U . . .
H8C H 0.5541 0.5941 0.2373 0.054 Uiso 1 1 calc R U . . .
C9 C 0.3962(7) 0.4569(7) -0.0570(6) 0.044(3) Uani 1 1 d . . . . .
H9A H 0.4242 0.5098 -0.0760 0.066 Uiso 1 1 calc R U . . .
H9B H 0.3534 0.4263 -0.0928 0.066 Uiso 1 1 calc R U . . .
H9C H 0.4306 0.4358 -0.0556 0.066 Uiso 1 1 calc R U . . .
C10 C 0.1920(6) 0.3266(7) 0.1480(6) 0.040(3) Uani 1 1 d . . . . .
H10A H 0.1599 0.3477 0.1670 0.048 Uiso 1 1 calc R U . . .
H10B H 0.1666 0.2943 0.1011 0.048 Uiso 1 1 calc R U . . .
C11 C 0.1191(7) 0.2253(7) 0.2434(7) 0.051(3) Uani 1 1 d . . . . .
H11A H 0.0821 0.2050 0.1990 0.061 Uiso 1 1 calc R U . . .
H11B H 0.1196 0.1817 0.2694 0.061 Uiso 1 1 calc R U . . .
C12 C 0.0936(7) 0.2631(8) 0.3015(8) 0.055(3) Uani 1 1 d . . . . .
H12A H 0.0890 0.3043 0.2750 0.066 Uiso 1 1 calc R U . . .
H12B H 0.0429 0.2255 0.3229 0.066 Uiso 1 1 calc R U . . .
C13 C 0.2340(7) 0.2363(7) 0.1799(7) 0.045(3) Uani 1 1 d . . . . .
H13A H 0.2788 0.2709 0.1472 0.053 Uiso 1 1 calc R U . . .
H13B H 0.1977 0.1934 0.1460 0.053 Uiso 1 1 calc R U . . .
C14 C 0.2593(7) 0.2058(7) 0.2493(7) 0.044(3) Uani 1 1 d . . . . .
H14A H 0.2147 0.1604 0.2724 0.053 Uiso 1 1 calc R U . . .
H14B H 0.2962 0.1905 0.2307 0.053 Uiso 1 1 calc R U . . .
C15 C 0.4442(6) 0.3167(6) 0.5373(6) 0.030(2) Uani 1 1 d . . . . .
C16 C 0.4777(5) 0.2934(6) 0.5948(6) 0.029(2) Uani 1 1 d . . . . .
C17 C 0.4730(6) 0.3093(6) 0.6741(6) 0.033(2) Uani 1 1 d . . . . .
H17 H 0.4947 0.2919 0.7130 0.039 Uiso 1 1 calc R U . . .
C18 C 0.4383(6) 0.3490(7) 0.6982(6) 0.038(3) Uani 1 1 d . . . . .
C19 C 0.4102(6) 0.3762(6) 0.6410(6) 0.037(3) Uani 1 1 d . . . . .
H19 H 0.3888 0.4065 0.6573 0.045 Uiso 1 1 calc R U . . .
C20 C 0.4109(6) 0.3618(6) 0.5598(6) 0.032(2) Uani 1 1 d . . . . .
C21 C 0.3821(6) 0.3945(6) 0.5019(6) 0.033(2) Uani 1 1 d . . . . .
C22 C 0.3825(8) 0.4680(7) 0.5191(7) 0.053(3) Uani 1 1 d . . . . .
H22A H 0.4008 0.5011 0.4723 0.079 Uiso 1 1 calc R U . . .
H22B H 0.4165 0.4939 0.5641 0.079 Uiso 1 1 calc R U . . .
H22C H 0.3306 0.4566 0.5321 0.079 Uiso 1 1 calc R U . . .
C23 C 0.4323(8) 0.3642(8) 0.7853(6) 0.050(3) Uani 1 1 d . . . . .
H23A H 0.4405 0.3287 0.8178 0.075 Uiso 1 1 calc R U . . .
H23B H 0.3814 0.3568 0.7960 0.075 Uiso 1 1 calc R U . . .
H23C H 0.4711 0.4168 0.7982 0.075 Uiso 1 1 calc R U . . .
C24 C 0.5920(6) 0.2307(6) 0.4693(6) 0.035(2) Uani 1 1 d . . . . .
H24A H 0.6404 0.2585 0.4391 0.042 Uiso 1 1 calc R U . . .
H24B H 0.5997 0.2008 0.5112 0.042 Uiso 1 1 calc R U . . .
C25 C 0.5316(7) 0.1776(6) 0.4154(6) 0.039(3) Uani 1 1 d . . . . .
H25A H 0.5462 0.1420 0.3915 0.047 Uiso 1 1 calc R U . . .
H25B H 0.4834 0.1473 0.4452 0.047 Uiso 1 1 calc R U . . .
C26 C 0.6460(6) 0.3534(6) 0.5404(6) 0.034(2) Uani 1 1 d . . . . .
H26A H 0.6736 0.3349 0.5739 0.040 Uiso 1 1 calc R U . . .
H26B H 0.6317 0.3844 0.5741 0.040 Uiso 1 1 calc R U . . .
C27 C 0.6969(6) 0.4018(7) 0.4744(7) 0.040(3) Uani 1 1 d . . . . .
H27A H 0.7341 0.4531 0.4949 0.048 Uiso 1 1 calc R U . . .
H27B H 0.7257 0.3782 0.4526 0.048 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.999(7) . ?
Cu1 O3 2.384(8) . ?
Cu1 O4 1.891(7) . ?
Cu1 O5 1.896(7) . ?
Cu1 N2 2.007(9) . ?
Cu2 Cl1' 2.311(15) . ?
Cu2 O4 1.881(7) . ?
Cu2 O6 1.906(7) . ?
Cu2 O15 1.90(3) . ?
Cu2 N3 1.982(9) . ?
Cu3 O2 1.876(7) 4_665 ?
Cu3 O6 1.980(7) . ?
Cu3 O7 2.361(7) . ?
Cu3 O8 1.886(7) . ?
Cu3 N4 2.002(8) . ?
Cu4 O1 1.912(6) 4_665 ?
Cu4 O8 1.887(6) . ?
Cu4 O9 2.006(7) . ?
Cu4 N1 1.968(8) 4_665 ?
O1 Cu4 1.912(6) 4_665 ?
O1 C1 1.353(12) . ?
O2 Cu3 1.876(7) 4_665 ?
O2 N1 1.371(11) . ?
O3 H3 0.8400 . ?
O3 C12 1.414(15) . ?
O4 C14 1.424(13) . ?
O5 N3 1.360(11) . ?
O6 C15 1.346(12) . ?
O7 H7 0.8400 . ?
O7 C25 1.438(13) . ?
O8 C27 1.419(12) . ?
O9 N5 1.275(12) . ?
O10 N5 1.177(13) . ?
O11 N5 1.269(13) . ?
O13 N6 1.24(3) . ?
O14 N6 1.22(3) . ?
O15 N6 1.38(6) . ?
N1 Cu4 1.968(8) 4_665 ?
N1 C7 1.306(12) . ?
N2 C10 1.477(14) . ?
N2 C11 1.491(15) . ?
N2 C13 1.488(14) . ?
N3 C21 1.312(13) . ?
N4 C00W 1.478(13) . ?
N4 C24 1.480(13) . ?
N4 C26 1.493(14) . ?
C00W H00A 0.9900 . ?
C00W H00B 0.9900 . ?
C00W C16 1.523(15) . ?
C1 C2 1.402(14) . ?
C1 C6 1.431(15) . ?
C2 C3 1.370(15) . ?
C2 C10 1.498(15) . ?
C3 H3A 0.9500 . ?
C3 C4 1.385(16) . ?
C4 C5 1.367(15) . ?
C4 C9 1.484(15) . ?
C5 H5 0.9500 . ?
C5 C6 1.428(14) . ?
C6 C7 1.446(15) . ?
C7 C8 1.513(15) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.483(17) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.526(16) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.391(14) . ?
C15 C20 1.428(15) . ?
C16 C17 1.388(15) . ?
C17 H17 0.9500 . ?
C17 C18 1.364(16) . ?
C18 C19 1.367(16) . ?
C18 C23 1.516(15) . ?
C19 H19 0.9500 . ?
C19 C20 1.401(15) . ?
C20 C21 1.454(15) . ?
C21 C22 1.509(16) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.468(16) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.499(15) . ?
C27 H27A 0.9900 . ?
C27 H27B 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
O1 Cu1 O3 101.7(3) . . ?
O1 Cu1 N2 93.2(3) . . ?
O4 Cu1 O1 150.6(3) . . ?
O4 Cu1 O3 107.2(3) . . ?
O4 Cu1 O5 93.5(3) . . ?
O4 Cu1 N2 86.8(3) . . ?
O5 Cu1 O1 87.4(3) . . ?
O5 Cu1 O3 97.9(3) . . ?
O5 Cu1 N2 178.1(4) . . ?
N2 Cu1 O3 80.2(3) . . ?
O4 Cu2 Cl1' 92.3(6) . . ?
O4 Cu2 O6 172.5(3) . . ?
O4 Cu2 O15 95.5(13) . . ?
O4 Cu2 N3 89.8(3) . . ?
O6 Cu2 Cl1' 89.4(6) . . ?
O6 Cu2 N3 89.8(3) . . ?
O15 Cu2 O6 85.1(12) . . ?
O15 Cu2 N3 174.3(14) . . ?
N3 Cu2 Cl1' 169.3(7) . . ?
O2 Cu3 O6 89.3(3) 4_665 . ?
O2 Cu3 O7 95.2(3) 4_665 . ?
O2 Cu3 O8 93.4(3) 4_665 . ?
O2 Cu3 N4 176.4(3) 4_665 . ?
O6 Cu3 O7 95.3(3) . . ?
O6 Cu3 N4 92.4(3) . . ?
O8 Cu3 O6 153.3(3) . . ?
O8 Cu3 O7 110.9(3) . . ?
O8 Cu3 N4 86.5(3) . . ?
N4 Cu3 O7 81.4(3) . . ?
O1 Cu4 O9 85.4(3) 4_665 . ?
O1 Cu4 N1 91.5(3) 4_665 4_665 ?
O8 Cu4 O1 178.2(3) . 4_665 ?
O8 Cu4 O9 92.9(3) . . ?
O8 Cu4 N1 90.1(3) . 4_665 ?
N1 Cu4 O9 176.8(3) 4_665 . ?
Cu4 O1 Cu1 110.6(3) 4_665 . ?
C1 O1 Cu1 107.8(6) . . ?
C1 O1 Cu4 127.0(6) . 4_665 ?
N1 O2 Cu3 117.6(5) . 4_665 ?
Cu1 O3 H3 98.6 . . ?
C12 O3 Cu1 103.4(7) . . ?
C12 O3 H3 109.5 . . ?
Cu2 O4 Cu1 117.7(4) . . ?
C14 O4 Cu1 113.8(6) . . ?
C14 O4 Cu2 128.6(7) . . ?
N3 O5 Cu1 116.3(5) . . ?
Cu2 O6 Cu3 118.2(3) . . ?
C15 O6 Cu2 124.0(6) . . ?
C15 O6 Cu3 110.7(6) . . ?
Cu3 O7 H7 115.4 . . ?
C25 O7 Cu3 103.4(6) . . ?
C25 O7 H7 109.5 . . ?
Cu3 O8 Cu4 117.3(3) . . ?
C27 O8 Cu3 114.1(6) . . ?
C27 O8 Cu4 128.5(6) . . ?
N5 O9 Cu4 104.7(6) . . ?
N6 O15 Cu2 104(2) . . ?
O2 N1 Cu4 117.3(6) . 4_665 ?
C7 N1 Cu4 127.7(7) . 4_665 ?
C7 N1 O2 114.6(8) . . ?
C10 N2 Cu1 112.0(6) . . ?
C10 N2 C11 110.3(9) . . ?
C10 N2 C13 109.9(9) . . ?
C11 N2 Cu1 110.0(7) . . ?
C13 N2 Cu1 102.7(6) . . ?
C13 N2 C11 111.7(9) . . ?
O5 N3 Cu2 118.5(6) . . ?
C21 N3 Cu2 126.3(7) . . ?
C21 N3 O5 114.8(8) . . ?
C00W N4 Cu3 113.6(6) . . ?
C00W N4 C24 109.5(8) . . ?
C00W N4 C26 112.7(8) . . ?
C24 N4 Cu3 106.4(6) . . ?
C24 N4 C26 112.0(8) . . ?
C26 N4 Cu3 102.4(6) . . ?
O10 N5 O9 121.7(10) . . ?
O10 N5 O11 123.7(10) . . ?
O11 N5 O9 114.6(10) . . ?
O13 N6 O15 120(3) . . ?
O14 N6 O13 122(3) . . ?
O14 N6 O15 117(2) . . ?
N4 C00W H00A 108.6 . . ?
N4 C00W H00B 108.6 . . ?
N4 C00W C16 114.5(8) . . ?
H00A C00W H00B 107.6 . . ?
C16 C00W H00A 108.6 . . ?
C16 C00W H00B 108.6 . . ?
O1 C1 C2 117.8(9) . . ?
O1 C1 C6 121.6(9) . . ?
C2 C1 C6 120.6(9) . . ?
C1 C2 C10 118.6(9) . . ?
C3 C2 C1 119.6(10) . . ?
C3 C2 C10 121.7(10) . . ?
C2 C3 H3A 118.6 . . ?
C2 C3 C4 122.8(10) . . ?
C4 C3 H3A 118.6 . . ?
C3 C4 C9 121.4(10) . . ?
C5 C4 C3 117.3(9) . . ?
C5 C4 C9 121.2(11) . . ?
C4 C5 H5 117.8 . . ?
C4 C5 C6 124.3(10) . . ?
C6 C5 H5 117.8 . . ?
C1 C6 C7 124.7(9) . . ?
C5 C6 C1 115.2(9) . . ?
C5 C6 C7 120.0(10) . . ?
N1 C7 C6 122.2(9) . . ?
N1 C7 C8 117.1(9) . . ?
C6 C7 C8 120.7(8) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C2 113.6(8) . . ?
N2 C10 H10A 108.8 . . ?
N2 C10 H10B 108.8 . . ?
C2 C10 H10A 108.8 . . ?
C2 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
N2 C11 H11A 109.1 . . ?
N2 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
C12 C11 N2 112.4(10) . . ?
C12 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
O3 C12 C11 109.8(10) . . ?
O3 C12 H12A 109.7 . . ?
O3 C12 H12B 109.7 . . ?
C11 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
N2 C13 H13A 109.8 . . ?
N2 C13 H13B 109.8 . . ?
N2 C13 C14 109.2(9) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
O4 C14 C13 108.7(9) . . ?
O4 C14 H14A 110.0 . . ?
O4 C14 H14B 110.0 . . ?
C13 C14 H14A 110.0 . . ?
C13 C14 H14B 110.0 . . ?
H14A C14 H14B 108.3 . . ?
O6 C15 C16 118.6(9) . . ?
O6 C15 C20 121.7(9) . . ?
C16 C15 C20 119.7(9) . . ?
C15 C16 C00W 117.8(9) . . ?
C17 C16 C00W 122.8(9) . . ?
C17 C16 C15 119.4(10) . . ?
C16 C17 H17 118.7 . . ?
C18 C17 C16 122.5(10) . . ?
C18 C17 H17 118.7 . . ?
C17 C18 C19 117.8(10) . . ?
C17 C18 C23 121.6(10) . . ?
C19 C18 C23 120.6(11) . . ?
C18 C19 H19 118.1 . . ?
C18 C19 C20 123.7(10) . . ?
C20 C19 H19 118.1 . . ?
C15 C20 C21 122.4(8) . . ?
C19 C20 C15 116.7(10) . . ?
C19 C20 C21 120.8(9) . . ?
N3 C21 C20 121.3(9) . . ?
N3 C21 C22 117.9(9) . . ?
C20 C21 C22 120.8(9) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 H24A 108.8 . . ?
N4 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
C25 C24 N4 113.9(9) . . ?
C25 C24 H24A 108.8 . . ?
C25 C24 H24B 108.8 . . ?
O7 C25 C24 108.6(9) . . ?
O7 C25 H25A 110.0 . . ?
O7 C25 H25B 110.0 . . ?
C24 C25 H25A 110.0 . . ?
C24 C25 H25B 110.0 . . ?
H25A C25 H25B 108.4 . . ?
N4 C26 H26A 109.6 . . ?
N4 C26 H26B 109.6 . . ?
N4 C26 C27 110.2(8) . . ?
H26A C26 H26B 108.1 . . ?
C27 C26 H26A 109.6 . . ?
C27 C26 H26B 109.6 . . ?
O8 C27 C26 109.4(8) . . ?
O8 C27 H27A 109.8 . . ?
O8 C27 H27B 109.8 . . ?
C26 C27 H27A 109.8 . . ?
C26 C27 H27B 109.8 . . ?
H27A C27 H27B 108.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O9 0.84 2.07 2.831(12) 150.7 4_665
O7 H7 O15 0.84 2.09 2.75(4) 134.7 .

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
Cu1 O1 C1 C2 62.1(9) . . . . ?
Cu1 O1 C1 C6 -116.1(8) . . . . ?
Cu1 O3 C12 C11 37.8(11) . . . . ?
Cu1 O4 C14 C13 20.5(11) . . . . ?
Cu1 O5 N3 Cu2 24.1(9) . . . . ?
Cu1 O5 N3 C21 -162.2(7) . . . . ?
Cu1 N2 C10 C2 45.9(11) . . . . ?
Cu1 N2 C11 C12 44.1(12) . . . . ?
Cu1 N2 C13 C14 44.2(10) . . . . ?
Cu2 O4 C14 C13 -158.7(7) . . . . ?
Cu2 O6 C15 C16 147.8(8) . . . . ?
Cu2 O6 C15 C20 -30.4(13) . . . . ?
Cu2 O15 N6 O13 -166(2) . . . . ?
Cu2 O15 N6 O14 12(3) . . . . ?
Cu2 N3 C21 C20 -7.5(14) . . . . ?
Cu2 N3 C21 C22 171.0(8) . . . . ?
Cu3 O2 N1 Cu4 -23.8(8) 4_665 . . 4_665 ?
Cu3 O2 N1 C7 162.4(6) 4_665 . . . ?
Cu3 O6 C15 C16 -62.5(10) . . . . ?
Cu3 O6 C15 C20 119.4(9) . . . . ?
Cu3 O7 C25 C24 -33.1(9) . . . . ?
Cu3 O8 C27 C26 -17.0(11) . . . . ?
Cu3 N4 C00W C16 -45.3(10) . . . . ?
Cu3 N4 C24 C25 -51.0(10) . . . . ?
Cu3 N4 C26 C27 -43.4(9) . . . . ?
Cu4 O1 C1 C2 -163.0(7) 4_665 . . . ?
Cu4 O1 C1 C6 18.8(12) 4_665 . . . ?
Cu4 O8 C27 C26 158.9(7) . . . . ?
Cu4 O9 N5 O10 -16.2(11) . . . . ?
Cu4 O9 N5 O11 164.2(7) . . . . ?
Cu4 N1 C7 C6 4.5(13) 4_665 . . . ?
Cu4 N1 C7 C8 -172.7(7) 4_665 . . . ?
Cl1' Cu2 O4 Cu1 177.1(8) . . . . ?
Cl1' Cu2 O4 C14 -3.7(11) . . . . ?
O1 Cu1 O4 Cu2 92.3(7) . . . . ?
O1 Cu1 O4 C14 -87.1(9) . . . . ?
O1 Cu1 O5 N3 -165.7(7) . . . . ?
O1 C1 C2 C3 179.8(9) . . . . ?
O1 C1 C2 C10 -1.9(14) . . . . ?
O1 C1 C6 C5 -178.2(8) . . . . ?
O1 C1 C6 C7 5.0(14) . . . . ?
O2 Cu3 O8 Cu4 0.8(5) 4_665 . . . ?
O2 Cu3 O8 C27 177.1(7) 4_665 . . . ?
O2 N1 C7 C6 177.5(8) . . . . ?
O2 N1 C7 C8 0.3(12) . . . . ?
O3 Cu1 O4 Cu2 -98.1(4) . . . . ?
O3 Cu1 O4 C14 82.5(8) . . . . ?
O3 Cu1 O5 N3 92.8(7) . . . . ?
O4 Cu1 O5 N3 -15.1(7) . . . . ?
O5 Cu1 O4 Cu2 1.3(5) . . . . ?
O5 Cu1 O4 C14 -178.1(7) . . . . ?
O5 N3 C21 C20 179.3(9) . . . . ?
O5 N3 C21 C22 -2.1(13) . . . . ?
O6 Cu3 O8 Cu4 -94.4(7) . . . . ?
O6 Cu3 O8 C27 82.0(9) . . . . ?
O6 C15 C16 C00W 4.1(14) . . . . ?
O6 C15 C16 C17 -173.2(9) . . . . ?
O6 C15 C20 C19 174.4(9) . . . . ?
O6 C15 C20 C21 -8.3(16) . . . . ?
O7 Cu3 O8 Cu4 97.7(4) . . . . ?
O7 Cu3 O8 C27 -86.0(7) . . . . ?
O9 Cu4 O8 Cu3 169.6(4) . . . . ?
O9 Cu4 O8 C27 -6.1(8) . . . . ?
O15 Cu2 O4 Cu1 -174.4(13) . . . . ?
O15 Cu2 O4 C14 4.9(15) . . . . ?
N1 Cu4 O8 Cu3 -9.6(4) 4_665 . . . ?
N1 Cu4 O8 C27 174.7(8) 4_665 . . . ?
N2 Cu1 O4 Cu2 -176.9(5) . . . . ?
N2 Cu1 O4 C14 3.8(8) . . . . ?
N2 C11 C12 O3 -57.3(14) . . . . ?
N2 C13 C14 O4 -44.1(12) . . . . ?
N3 Cu2 O4 Cu1 7.6(5) . . . . ?
N3 Cu2 O4 C14 -173.2(9) . . . . ?
N4 Cu3 O8 Cu4 177.1(4) . . . . ?
N4 Cu3 O8 C27 -6.5(7) . . . . ?
N4 C00W C16 C15 57.0(13) . . . . ?
N4 C00W C16 C17 -125.8(10) . . . . ?
N4 C24 C25 O7 59.0(12) . . . . ?
N4 C26 C27 O8 41.2(12) . . . . ?
C00W N4 C24 C25 72.1(11) . . . . ?
C00W N4 C26 C27 -165.8(8) . . . . ?
C00W C16 C17 C18 -178.9(10) . . . . ?
C1 C2 C3 C4 -0.4(16) . . . . ?
C1 C2 C10 N2 -61.4(13) . . . . ?
C1 C6 C7 N1 -17.0(15) . . . . ?
C1 C6 C7 C8 160.1(9) . . . . ?
C2 C1 C6 C5 3.7(14) . . . . ?
C2 C1 C6 C7 -173.1(9) . . . . ?
C2 C3 C4 C5 0.9(16) . . . . ?
C2 C3 C4 C9 176.8(10) . . . . ?
C3 C2 C10 N2 116.9(11) . . . . ?
C3 C4 C5 C6 1.1(16) . . . . ?
C4 C5 C6 C1 -3.3(15) . . . . ?
C4 C5 C6 C7 173.6(10) . . . . ?
C5 C6 C7 N1 166.5(9) . . . . ?
C5 C6 C7 C8 -16.5(14) . . . . ?
C6 C1 C2 C3 -2.0(15) . . . . ?
C6 C1 C2 C10 176.3(9) . . . . ?
C9 C4 C5 C6 -174.8(10) . . . . ?
C10 N2 C11 C12 -80.1(12) . . . . ?
C10 N2 C13 C14 163.6(9) . . . . ?
C10 C2 C3 C4 -178.6(10) . . . . ?
C11 N2 C10 C2 168.9(9) . . . . ?
C11 N2 C13 C14 -73.6(11) . . . . ?
C13 N2 C10 C2 -67.5(11) . . . . ?
C13 N2 C11 C12 157.4(10) . . . . ?
C15 C16 C17 C18 -1.8(16) . . . . ?
C15 C20 C21 N3 27.9(16) . . . . ?
C15 C20 C21 C22 -150.6(11) . . . . ?
C16 C15 C20 C19 -3.8(15) . . . . ?
C16 C15 C20 C21 173.5(10) . . . . ?
C16 C17 C18 C19 -2.6(16) . . . . ?
C16 C17 C18 C23 178.6(11) . . . . ?
C17 C18 C19 C20 3.9(17) . . . . ?
C18 C19 C20 C15 -0.7(16) . . . . ?
C18 C19 C20 C21 -178.1(11) . . . . ?
C19 C20 C21 N3 -154.9(10) . . . . ?
C19 C20 C21 C22 26.6(16) . . . . ?
C20 C15 C16 C00W -177.7(9) . . . . ?
C20 C15 C16 C17 5.0(15) . . . . ?
C23 C18 C19 C20 -177.3(11) . . . . ?
C24 N4 C00W C16 -164.0(9) . . . . ?
C24 N4 C26 C27 70.2(11) . . . . ?
C26 N4 C00W C16 70.6(11) . . . . ?
C26 N4 C24 C25 -162.1(9) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-26 23 0 0.0033 -26.0000 23.0000 0.0000 0.6003 0.7972 -0.0227
3 3 23 0.3212 3.0000 3.0000 23.0000 0.0006 0.0001 0.9906
-3 -3 -23 0.2935 -3.0000 -3.0000 -23.0000 -0.0006 -0.0001 -0.9906
-25 0 -2 0.0068 -25.0000 0.0000 -2.0000 -0.2703 0.9424 -0.2685
25 0 0 0.0884 25.0000 -0.0000 -0.0000 0.2834 -0.9546 0.1862
-25 0 1 0.0132 -25.0000 0.0000 1.0000 -0.2899 0.9607 -0.1451
8 -28 0 0.0132 8.0000 -28.0000 -0.0000 -0.9989 -0.0674 -0.1485

####################################################################### 
# 
# 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 991825'
_audit_update_record             
;
2014-10-16 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
# local name eb3263
_audit_creation_date             2013-11-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2013-4
_publ_section_exptl              
;
Any special experimental details
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C80 H98 Cu8 N12 O20, 2.78(C H4 O), 2(B F4), 2(C4 H10 O1)'
_chemical_formula_sum            'C90.78 H129.13 B2 Cu8 F8 N12 O24.78'
_chemical_formula_weight         2467.01
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N8 O20 Cu8 B F4'
_chemical_oxdiff_usercomment     '@ 120 K RS34'
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.3511(4)
_cell_length_b                   17.1783(2)
_cell_length_c                   26.2510(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.0240(17)
_cell_angle_gamma                90
_cell_volume                     10335.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    24681
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      30.9620
_cell_measurement_theta_min      3.5540
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5080
_exptl_crystal_size_max          0.4570
_exptl_crystal_size_mid          0.2853
_exptl_crystal_size_min          0.2033
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            72031
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.211
_diffrn_reflns_theta_min         2.850
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9105
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0273581000
_diffrn_orient_matrix_UB_12      0.0027017000
_diffrn_orient_matrix_UB_13      -0.0171667000
_diffrn_orient_matrix_UB_21      0.0029172000
_diffrn_orient_matrix_UB_22      0.0410660000
_diffrn_orient_matrix_UB_23      -0.0005555000
_diffrn_orient_matrix_UB_31      0.0141689000
_diffrn_orient_matrix_UB_32      -0.0032020000
_diffrn_orient_matrix_UB_33      -0.0215221000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          xp
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12230
_reflns_number_total             15269
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    
;
Olex2
;
_computing_publication_material  
;
Olex2
;
_computing_structure_refinement  
;
ShelXL
;
_computing_structure_solution    
;
XT
;
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         15269
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0410
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0407P)²+28.5670P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1035
_refine_special_details          
;
One methanol (containing O13) was modelled with partial occupancy (ca 40 %).  
The tetrafluoroborate anion and ether molecule were both 
modelled as entirely disorderd over two sites as evidenced by residual peaks 
in a difference Fourier map.  The geometry of the minor ether 
component was refined to be similar to that of the major component; 
coordinates and Uij values were fixed in place once the model had
converged.   No restraints were used on the tetrafluoroborate.


 
#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
411_ALERT_2_A Short Inter H...H Contact  H26B   ..  H42C    ..       1.76 Ang.

Pertains to minor component of ether disorder, the coordinates of which were 
not refined.

#===============================================================================
213_ALERT_2_B Atom C40             has ADP max/min Ratio .....        4.1 prolat

Refined with mild isotropic similarity restraint.

220_ALERT_2_B Large Non-Solvent    C     Ueq(max)/Ueq(min) ...        7.0 Ratio
222_ALERT_3_B Large Non-Solvent    H    Uiso(max)/Uiso(min) ..        7.1 Ratio

Pertain to minor component of ether disorder, the coordinates of which were 
not refined.


#===============================================================================
068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...     Please Check

Rounding error caused by partly occupied solvent.

161_ALERT_4_C Missing or Zero su (esd) on x-coordinate for ...       C41A
161_ALERT_4_C Missing or Zero su (esd) on x-coordinate for ...       C42A
161_ALERT_4_C Missing or Zero su (esd) on x-coordinate for ...       O11A
161_ALERT_4_C Missing or Zero su (esd) on x-coordinate for ...       C43A
161_ALERT_4_C Missing or Zero su (esd) on x-coordinate for ...       C44A
162_ALERT_4_C Missing or Zero su (esd) on y-coordinate for ...       C41A
162_ALERT_4_C Missing or Zero su (esd) on y-coordinate for ...       C42A
162_ALERT_4_C Missing or Zero su (esd) on y-coordinate for ...       O11A
162_ALERT_4_C Missing or Zero su (esd) on y-coordinate for ...       C43A
162_ALERT_4_C Missing or Zero su (esd) on y-coordinate for ...       C44A
163_ALERT_4_C Missing or Zero su (esd) on z-coordinate for ...       C41A
163_ALERT_4_C Missing or Zero su (esd) on z-coordinate for ...       C42A
163_ALERT_4_C Missing or Zero su (esd) on z-coordinate for ...       O11A
163_ALERT_4_C Missing or Zero su (esd) on z-coordinate for ...       C43A
163_ALERT_4_C Missing or Zero su (esd) on z-coordinate for ...       C44A
202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          5

Pertain to minor component of ether disorder, the coordinates of which were 
not refined.

241_ALERT_2_C High      Ueq as Compared to Neighbors for .....        O10 Check
242_ALERT_2_C Low       Ueq as Compared to Neighbors for .....        C39 Check

Insignificant.

411_ALERT_2_C Short Inter H...H Contact  H25B   ..  H42D    ..       2.04 Ang.
411_ALERT_2_C Short Inter H...H Contact  H27A   ..  H43C    ..       2.07 Ang.
413_ALERT_2_C Short Inter XH3 .. XHn     H40A   ..  H42B    ..       2.12 Ang.

Pertain to minor component of ether disorder, the coordinates of which were 
not refined.

#===============================================================================

;



# start Validation Reply Form
_vrf_PLAT411_eb3263              
;
PROBLEM: Short Inter H...H Contact  H26B   ..  H42C    ..       1.76 Ang.  
RESPONSE: Please see the _refine_special_details section of the CIF.
;


# end Validation Reply Form

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H12 of O12, H3 of O3, H8 of O8, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H13 of O13
2. Restrained distances
 C42A-C43A
 2.5 with sigma of 0.04
 C41-C42 \\sim C43-C44
 with sigma of 0.02
 O11-C42 \\sim O11-C43
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 C41, C42, O11, C43, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C41, C42, O11, C43, C44}
as
{C41A, C42A, O11A, C43A, C44A}
6. Others
 Sof(O13)=Sof(H13)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(1)
 Sof(B1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=1-FVAR(2)
 Sof(B1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(2)
 Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42A)=Sof(H42C)=Sof(H42D)=
 Sof(O11A)=Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=1-FVAR(3)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(O11)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(3)
7.a Everything fixed:
 C41A, C42A, O11A, C43A, C44A
7.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B), C42(H42A,H42B), C43(H43A,H43B), C42A(H42C,H42D), C43A(H43C,
 H43D)
7.c Me refined with riding coordinates:
 C41A(H41D,H41E,H41F), C44A(H44D,H44E,H44F)
7.d Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C17(H17), C19(H19), C29(H29), C30(H30), C31(H31), C32(H32),
 C35(H35), C36(H36), C37(H37), C38(H38)
7.e Tetrahedral OH refined with riding coordinates:
 O13(H13)
7.f Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C40(H40A,H40B,H40C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C41(H41A,H41B,
 H41C), C44(H44A,H44B,H44C)
7.g Idealised tetrahedral OH refined as rotating group:
 O3(H3), O8(H8), O12(H12)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 -0.01358(2) 0.74979(2) 0.90094(2) 0.01818(7) Uani 1 1 d . . . . .
Cu2 Cu -0.14271(2) 0.77689(2) 0.81397(2) 0.01670(6) Uani 1 1 d . . . . .
Cu3 Cu 0.17262(2) 0.68324(2) 0.79598(2) 0.01789(6) Uani 1 1 d . . . . .
Cu4 Cu 0.10179(2) 0.65008(2) 0.89019(2) 0.02083(7) Uani 1 1 d . . . . .
O1 O -0.07473(7) 0.81930(9) 0.86331(6) 0.0180(3) Uani 1 1 d . . . . .
O2 O 0.08022(8) 0.73298(10) 0.84325(7) 0.0240(4) Uani 1 1 d . . . . .
O3 O -0.20661(8) 0.71447(10) 0.85880(8) 0.0286(4) Uani 1 1 d . . . . .
H3 H -0.2327 0.6914 0.8378 0.034 Uiso 1 1 calc R U . . .
O4 O -0.18909(7) 0.76672(9) 0.74609(6) 0.0206(3) Uani 1 1 d . . . . .
O5 O 0.14934(7) 0.60698(9) 0.84115(6) 0.0207(3) Uani 1 1 d . . . . .
O6 O 0.09740(7) 0.68826(9) 0.69462(7) 0.0232(3) Uani 1 1 d . . . . .
O7 O 0.03302(8) 0.65683(10) 0.91812(7) 0.0244(4) Uani 1 1 d . . . . .
O8 O 0.18214(9) 0.71337(11) 0.94189(7) 0.0323(4) Uani 1 1 d . . . . .
H8 H 0.1989 0.7185 0.9165 0.039 Uiso 1 1 calc R U . . .
O9 O 0.23240(7) 0.71648(10) 0.85614(7) 0.0248(4) Uani 1 1 d . . . . .
O10 O 0.28852(11) 0.64452(15) 0.81589(9) 0.0533(7) Uani 1 1 d . . . . .
N1 N 0.03927(8) 0.78300(11) 0.85423(8) 0.0185(4) Uani 1 1 d . . . . .
N2 N -0.19431(8) 0.86877(11) 0.82210(8) 0.0204(4) Uani 1 1 d . . . . .
N3 N 0.11628(8) 0.64110(11) 0.73583(8) 0.0186(4) Uani 1 1 d . . . . .
N4 N 0.12749(10) 0.56478(12) 0.94171(8) 0.0271(5) Uani 1 1 d . . . . .
N5 N 0.01678(10) 0.82769(13) 0.96782(9) 0.0294(5) Uani 1 1 d . . . . .
N6 N -0.06905(9) 0.72412(12) 0.94852(8) 0.0236(4) Uani 1 1 d . . . . .
C1 C -0.06118(10) 0.89134(12) 0.84911(8) 0.0168(4) Uani 1 1 d . . . . .
C2 C -0.10414(10) 0.95017(13) 0.84507(9) 0.0189(4) Uani 1 1 d . . . . .
C3 C -0.09139(10) 1.02574(13) 0.83214(9) 0.0211(5) Uani 1 1 d . . . . .
H3A H -0.1211 1.0643 0.8283 0.025 Uiso 1 1 calc R U . . .
C4 C -0.03575(11) 1.04603(13) 0.82467(10) 0.0238(5) Uani 1 1 d . . . . .
C5 C 0.00532(11) 0.98757(14) 0.82628(10) 0.0233(5) Uani 1 1 d . . . . .
H5 H 0.0429 1.0007 0.8202 0.028 Uiso 1 1 calc R U . . .
C6 C -0.00649(10) 0.90915(13) 0.83667(9) 0.0184(4) Uani 1 1 d . . . . .
C7 C 0.03681(10) 0.84913(13) 0.83002(9) 0.0212(5) Uani 1 1 d . . . . .
C8 C 0.07724(15) 0.86246(18) 0.79266(13) 0.0446(9) Uani 1 1 d . . . . .
H8A H 0.1173 0.8677 0.8120 0.067 Uiso 1 1 calc R U . . .
H8B H 0.0659 0.9102 0.7728 0.067 Uiso 1 1 calc R U . . .
H8C H 0.0749 0.8182 0.7688 0.067 Uiso 1 1 calc R U . . .
C9 C -0.02056(13) 1.13026(15) 0.81644(13) 0.0352(6) Uani 1 1 d . . . . .
H9A H -0.0491 1.1522 0.7878 0.053 Uiso 1 1 calc R U . . .
H9B H 0.0185 1.1331 0.8080 0.053 Uiso 1 1 calc R U . . .
H9C H -0.0213 1.1600 0.8482 0.053 Uiso 1 1 calc R U . . .
C10 C -0.16284(10) 0.93032(13) 0.85679(10) 0.0226(5) Uani 1 1 d . . . . .
H10A H -0.1578 0.9124 0.8932 0.027 Uiso 1 1 calc R U . . .
H10B H -0.1871 0.9780 0.8534 0.027 Uiso 1 1 calc R U . . .
C11 C -0.24655(11) 0.84383(16) 0.84266(11) 0.0295(6) Uani 1 1 d . . . . .
H11A H -0.2773 0.8264 0.8136 0.035 Uiso 1 1 calc R U . . .
H11B H -0.2620 0.8886 0.8596 0.035 Uiso 1 1 calc R U . . .
C12 C -0.23168(13) 0.77813(16) 0.88153(11) 0.0325(6) Uani 1 1 d . . . . .
H12A H -0.2038 0.7970 0.9123 0.039 Uiso 1 1 calc R U . . .
H12B H -0.2675 0.7606 0.8931 0.039 Uiso 1 1 calc R U . . .
C13 C -0.21120(11) 0.89724(14) 0.76793(10) 0.0243(5) Uani 1 1 d . . . . .
H13A H -0.1779 0.9246 0.7577 0.029 Uiso 1 1 calc R U . . .
H13B H -0.2440 0.9345 0.7654 0.029 Uiso 1 1 calc R U . . .
C14 C -0.22947(11) 0.82836(14) 0.73150(10) 0.0253(5) Uani 1 1 d . . . . .
H14A H -0.2693 0.8111 0.7341 0.030 Uiso 1 1 calc R U . . .
H14B H -0.2297 0.8440 0.6952 0.030 Uiso 1 1 calc R U . . .
C15 C 0.12963(10) 0.53497(13) 0.82691(10) 0.0204(4) Uani 1 1 d . . . . .
C16 C 0.13365(11) 0.47831(13) 0.86630(10) 0.0232(5) Uani 1 1 d . . . . .
C17 C 0.11601(11) 0.40232(14) 0.85287(11) 0.0269(5) Uani 1 1 d . . . . .
H17 H 0.1182 0.3644 0.8795 0.032 Uiso 1 1 calc R U . . .
C18 C 0.09533(11) 0.38045(14) 0.80189(11) 0.0277(5) Uani 1 1 d . . . . .
C19 C 0.08818(11) 0.43797(13) 0.76410(11) 0.0249(5) Uani 1 1 d . . . . .
H19 H 0.0724 0.4240 0.7292 0.030 Uiso 1 1 calc R U . . .
C20 C 0.10349(10) 0.51641(13) 0.77540(10) 0.0203(4) Uani 1 1 d . . . . .
C21 C 0.08805(10) 0.57539(13) 0.73406(9) 0.0191(4) Uani 1 1 d . . . . .
C22 C 0.03770(11) 0.56096(15) 0.69021(10) 0.0276(5) Uani 1 1 d . . . . .
H22A H 0.0128 0.6073 0.6848 0.041 Uiso 1 1 calc R U . . .
H22B H 0.0150 0.5165 0.6987 0.041 Uiso 1 1 calc R U . . .
H22C H 0.0525 0.5496 0.6585 0.041 Uiso 1 1 calc R U . . .
C23 C 0.08072(14) 0.29654(15) 0.78722(14) 0.0396(7) Uani 1 1 d . . . . .
H23A H 0.1168 0.2660 0.7917 0.059 Uiso 1 1 calc R U . . .
H23B H 0.0606 0.2940 0.7509 0.059 Uiso 1 1 calc R U . . .
H23C H 0.0553 0.2754 0.8096 0.059 Uiso 1 1 calc R U . . .
C24 C 0.16009(12) 0.50071(14) 0.92096(10) 0.0276(5) Uani 1 1 d . . . . .
H24A H 0.1610 0.4544 0.9436 0.033 Uiso 1 1 calc R U . . .
H24B H 0.2009 0.5176 0.9223 0.033 Uiso 1 1 calc R U . . .
C25 C 0.07103(13) 0.53517(16) 0.95317(12) 0.0335(6) Uani 1 1 d . . . . .
H25A H 0.0785 0.5041 0.9855 0.040 Uiso 1 1 calc R U . . .
H25B H 0.0518 0.5011 0.9246 0.040 Uiso 1 1 calc R U . . .
C26 C 0.03124(14) 0.60351(16) 0.95917(11) 0.0343(6) Uani 1 1 d . . . . .
H26A H -0.0092 0.5849 0.9577 0.041 Uiso 1 1 calc R U . . .
H26B H 0.0447 0.6293 0.9931 0.041 Uiso 1 1 calc R U . . .
C27 C 0.16392(15) 0.59991(17) 0.98865(11) 0.0384(7) Uani 1 1 d . . . . .
H27A H 0.1829 0.5579 1.0117 0.046 Uiso 1 1 calc R U . . .
H27B H 0.1386 0.6299 1.0078 0.046 Uiso 1 1 calc R U . . .
C28 C 0.20998(14) 0.65286(18) 0.97501(12) 0.0404(7) Uani 1 1 d . . . . .
H28A H 0.2334 0.6756 1.0070 0.049 Uiso 1 1 calc R U . . .
H28B H 0.2365 0.6230 0.9571 0.049 Uiso 1 1 calc R U . . .
C29 C 0.06152(14) 0.87719(18) 0.97558(12) 0.0379(6) Uani 1 1 d . . . . .
H29 H 0.0895 0.8738 0.9538 0.046 Uiso 1 1 calc R U . . .
C30 C 0.06886(15) 0.93342(19) 1.01418(12) 0.0423(7) Uani 1 1 d . . . . .
H30 H 0.1017 0.9671 1.0193 0.051 Uiso 1 1 calc R U . . .
C31 C 0.02760(16) 0.93923(19) 1.04471(12) 0.0438(8) Uani 1 1 d . . . . .
H31 H 0.0309 0.9785 1.0706 0.053 Uiso 1 1 calc R U . . .
C32 C -0.01893(15) 0.88783(18) 1.03781(11) 0.0378(7) Uani 1 1 d . . . . .
H32 H -0.0475 0.8909 1.0591 0.045 Uiso 1 1 calc R U . . .
C33 C -0.02297(12) 0.83142(15) 0.99900(10) 0.0282(5) Uani 1 1 d . . . . .
C34 C -0.06930(12) 0.77195(15) 0.98943(10) 0.0271(5) Uani 1 1 d . . . . .
C35 C -0.11147(14) 0.76339(19) 1.02021(11) 0.0369(7) Uani 1 1 d . . . . .
H35 H -0.1119 0.7973 1.0487 0.044 Uiso 1 1 calc R U . . .
C36 C -0.15262(13) 0.70496(19) 1.00868(12) 0.0386(7) Uani 1 1 d . . . . .
H36 H -0.1820 0.6992 1.0289 0.046 Uiso 1 1 calc R U . . .
C37 C -0.15113(13) 0.65531(18) 0.96808(12) 0.0357(6) Uani 1 1 d . . . . .
H37 H -0.1783 0.6139 0.9604 0.043 Uiso 1 1 calc R U . . .
C38 C -0.10861(12) 0.66750(15) 0.93847(11) 0.0285(5) Uani 1 1 d . . . . .
H38 H -0.1077 0.6340 0.9098 0.034 Uiso 1 1 calc R U . . .
C39 C 0.28133(13) 0.6847(2) 0.85337(12) 0.0428(8) Uani 1 1 d . . . . .
C40 C 0.33034(18) 0.6981(5) 0.89903(18) 0.118(3) Uani 1 1 d . U . . .
H40A H 0.3673 0.7028 0.8868 0.177 Uiso 1 1 calc R U . . .
H40B H 0.3326 0.6540 0.9231 0.177 Uiso 1 1 calc R U . . .
H40C H 0.3230 0.7460 0.9169 0.177 Uiso 1 1 calc R U . . .
O12 O 0.29529(10) 0.65935(14) 0.71324(9) 0.0443(5) Uani 1 1 d . . . . .
H12 H 0.2912 0.6534 0.7441 0.053 Uiso 1 1 calc R U . . .
C45 C 0.33359(15) 0.60166(19) 0.70059(14) 0.0445(8) Uani 1 1 d . . . . .
H45A H 0.3353 0.6053 0.6636 0.067 Uiso 1 1 calc R U . . .
H45B H 0.3193 0.5500 0.7080 0.067 Uiso 1 1 calc R U . . .
H45C H 0.3727 0.6097 0.7214 0.067 Uiso 1 1 calc R U . . .
O13 O -0.3388(8) 0.4529(6) 0.8739(5) 0.163(7) Uani 0.391(7) 1 d . . P . .
H13 H -0.3454 0.4879 0.8944 0.245 Uiso 0.391(7) 1 calc R U P . .
C46 C -0.3147(5) 0.3895(5) 0.9018(3) 0.056(3) Uani 0.391(7) 1 d . . P . .
H46A H -0.3373 0.3428 0.8895 0.084 Uiso 0.391(7) 1 calc R U P . .
H46B H -0.3153 0.3976 0.9387 0.084 Uiso 0.391(7) 1 calc R U P . .
H46C H -0.2743 0.3829 0.8972 0.084 Uiso 0.391(7) 1 calc R U P . .
B1 B -0.2964(4) 0.5592(8) 0.9874(7) 0.061(3) Uani 0.579(6) 1 d . . P A 1
F1 F -0.30213(19) 0.5008(4) 1.0191(3) 0.098(2) Uani 0.579(6) 1 d . . P A 1
F2 F -0.3463(3) 0.5715(4) 0.9481(4) 0.101(3) Uani 0.579(6) 1 d . . P A 1
F3 F -0.2542(2) 0.5283(3) 0.9592(3) 0.0638(15) Uani 0.579(6) 1 d . . P A 1
F4 F -0.27406(19) 0.6245(3) 1.0107(3) 0.096(2) Uani 0.579(6) 1 d . . P A 1
C41 C -0.0084(3) 0.3363(5) 0.8967(3) 0.055(2) Uani 0.440(5) 1 d D U P B 1
H41A H 0.0054 0.2823 0.9003 0.083 Uiso 0.440(5) 1 calc R U P B 1
H41B H 0.0056 0.3644 0.9291 0.083 Uiso 0.440(5) 1 calc R U P B 1
H41C H 0.0066 0.3615 0.8684 0.083 Uiso 0.440(5) 1 calc R U P B 1
C42 C -0.0719(3) 0.3373(4) 0.8851(4) 0.054(2) Uani 0.440(5) 1 d D U P B 1
H42A H -0.0851 0.3112 0.8513 0.065 Uiso 0.440(5) 1 calc R U P B 1
H42B H -0.0862 0.3060 0.9118 0.065 Uiso 0.440(5) 1 calc R U P B 1
O11 O -0.09861(18) 0.4123(3) 0.8830(2) 0.0463(15) Uani 0.440(5) 1 d D U P B 1
C43 C -0.1590(2) 0.4157(4) 0.8627(3) 0.0504(19) Uani 0.440(5) 1 d D U P B 1
H43A H -0.1671 0.3891 0.8286 0.061 Uiso 0.440(5) 1 calc R U P B 1
H43B H -0.1802 0.3875 0.8863 0.061 Uiso 0.440(5) 1 calc R U P B 1
C44 C -0.1794(3) 0.4916(4) 0.8567(4) 0.059(2) Uani 0.440(5) 1 d D U P B 1
H44A H -0.1744 0.5115 0.8228 0.089 Uiso 0.440(5) 1 calc R U P B 1
H44B H -0.1573 0.5242 0.8843 0.089 Uiso 0.440(5) 1 calc R U P B 1
H44C H -0.2208 0.4927 0.8588 0.089 Uiso 0.440(5) 1 calc R U P B 1
B1A B -0.3065(6) 0.5558(13) 0.9591(8) 0.073(5) Uani 0.421(6) 1 d . . P A 2
F1A F -0.2928(4) 0.6348(6) 0.9458(6) 0.151(5) Uani 0.421(6) 1 d . . P A 2
F2A F -0.3157(7) 0.5643(8) 1.0119(4) 0.156(6) Uani 0.421(6) 1 d . . P A 2
F3A F -0.3605(4) 0.5489(7) 0.9316(4) 0.079(3) Uani 0.421(6) 1 d . . P A 2
F4A F -0.2698(5) 0.5171(12) 0.9364(8) 0.194(9) Uani 0.421(6) 1 d . . P A 2
C41A C -0.0324 0.3645 0.8921 0.184 Uiso 0.5601 1 d D . P B 2
H41D H -0.0257 0.3809 0.8579 0.276 Uiso 0.560(5) 1 calc R U P B 2
H41E H -0.0578 0.3185 0.8881 0.276 Uiso 0.560(5) 1 calc R U P B 2
H41F H 0.0050 0.3516 0.9144 0.276 Uiso 0.560(5) 1 calc R U P B 2
C42A C -0.0606 0.4282 0.9157 0.088 Uiso 0.5601 1 d D . P B 2
H42C H -0.0766 0.4062 0.9449 0.105 Uiso 0.560(5) 1 calc R U P B 2
H42D H -0.0299 0.4659 0.9307 0.105 Uiso 0.560(5) 1 calc R U P B 2
O11A O -0.1047 0.4688 0.8842 0.322 Uiso 0.5601 1 d D . P B 2
C43A C -0.1634 0.4621 0.8790 0.095 Uiso 0.5601 1 d D . P B 2
H43C H -0.1741 0.4695 0.9134 0.114 Uiso 0.560(5) 1 calc R U P B 2
H43D H -0.1751 0.4087 0.8671 0.114 Uiso 0.560(5) 1 calc R U P B 2
C44A C -0.1943 0.5149 0.8445 0.062 Uiso 0.5601 1 d D . P B 2
H44D H -0.1673 0.5435 0.8271 0.093 Uiso 0.560(5) 1 calc R U P B 2
H44E H -0.2147 0.5515 0.8634 0.093 Uiso 0.560(5) 1 calc R U P B 2
H44F H -0.2228 0.4870 0.8186 0.093 Uiso 0.560(5) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.9750(16) . ?
Cu1 O7 1.9364(16) . ?
Cu1 N1 1.9827(19) . ?
Cu1 N5 2.214(2) . ?
Cu1 N6 2.013(2) . ?
Cu2 O1 1.9855(16) . ?
Cu2 O3 2.3309(18) . ?
Cu2 O4 1.9080(17) . ?
Cu2 O6 1.8919(16) 2_556 ?
Cu2 N2 2.0215(19) . ?
Cu3 O4 1.8938(16) 2_556 ?
Cu3 O5 1.9141(16) . ?
Cu3 O9 1.9813(18) . ?
Cu3 N3 1.988(2) . ?
Cu4 O2 1.8876(16) . ?
Cu4 O5 1.9964(16) . ?
Cu4 O7 1.8921(17) . ?
Cu4 O8 2.360(2) . ?
Cu4 N4 2.006(2) . ?
O1 C1 1.347(3) . ?
O2 N1 1.357(2) . ?
O3 H3 0.8400 . ?
O3 C12 1.424(3) . ?
O4 Cu3 1.8937(16) 2_556 ?
O4 C14 1.421(3) . ?
O5 C15 1.348(3) . ?
O6 Cu2 1.8919(16) 2_556 ?
O6 N3 1.356(2) . ?
O7 C26 1.421(3) . ?
O8 H8 0.8400 . ?
O8 C28 1.429(3) . ?
O9 C39 1.281(3) . ?
O10 C39 1.240(4) . ?
N1 C7 1.298(3) . ?
N2 C10 1.494(3) . ?
N2 C11 1.488(3) . ?
N2 C13 1.484(3) . ?
N3 C21 1.303(3) . ?
N4 C24 1.499(3) . ?
N4 C25 1.496(4) . ?
N4 C27 1.485(4) . ?
N5 C29 1.332(4) . ?
N5 C33 1.351(3) . ?
N6 C34 1.353(3) . ?
N6 C38 1.333(3) . ?
C1 C2 1.414(3) . ?
C1 C6 1.411(3) . ?
C2 C3 1.388(3) . ?
C2 C10 1.500(3) . ?
C3 H3A 0.9500 . ?
C3 C4 1.395(3) . ?
C4 C5 1.384(3) . ?
C4 C9 1.515(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.412(3) . ?
C6 C7 1.478(3) . ?
C7 C8 1.503(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.516(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.530(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.410(3) . ?
C15 C20 1.409(3) . ?
C16 C17 1.394(3) . ?
C16 C24 1.500(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.385(4) . ?
C18 C19 1.387(4) . ?
C18 C23 1.514(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.411(3) . ?
C20 C21 1.478(3) . ?
C21 C22 1.500(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.524(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.503(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29 0.9500 . ?
C29 C30 1.387(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.370(5) . ?
C31 H31 0.9500 . ?
C31 C32 1.385(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.396(4) . ?
C33 C34 1.474(4) . ?
C34 C35 1.396(4) . ?
C35 H35 0.9500 . ?
C35 C36 1.382(5) . ?
C36 H36 0.9500 . ?
C36 C37 1.371(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.389(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.508(5) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
O12 H12 0.8400 . ?
O12 C45 1.416(4) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
O13 H13 0.8400 . ?
O13 C46 1.371(14) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
B1 F1 1.328(18) . ?
B1 F2 1.416(16) . ?
B1 F3 1.442(14) . ?
B1 F4 1.335(13) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C41 C42 1.455(7) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 O11 1.429(6) . ?
O11 C43 1.410(6) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.387(7) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
B1A F1A 1.45(2) . ?
B1A F2A 1.45(2) . ?
B1A F3A 1.332(18) . ?
B1A F4A 1.32(3) . ?
C41A H41D 0.9800 . ?
C41A H41E 0.9800 . ?
C41A H41F 0.9800 . ?
C41A C42A 1.4737 . ?
C42A H42C 0.9900 . ?
C42A H42D 0.9900 . ?
C42A O11A 1.3805 . ?
O11A C43A 1.3582 . ?
C43A H43C 0.9900 . ?
C43A H43D 0.9900 . ?
C43A C44A 1.3822 . ?
C44A H44D 0.9800 . ?
C44A H44E 0.9800 . ?
C44A H44F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N1 89.58(7) . . ?
O1 Cu1 N5 97.03(8) . . ?
O1 Cu1 N6 87.32(7) . . ?
O7 Cu1 O1 159.28(7) . . ?
O7 Cu1 N1 89.59(7) . . ?
O7 Cu1 N5 103.49(8) . . ?
O7 Cu1 N6 94.27(8) . . ?
N1 Cu1 N5 100.01(8) . . ?
N1 Cu1 N6 175.88(8) . . ?
N6 Cu1 N5 77.69(9) . . ?
O1 Cu2 O3 110.40(7) . . ?
O1 Cu2 N2 93.61(7) . . ?
O4 Cu2 O1 152.02(7) . . ?
O4 Cu2 O3 97.21(7) . . ?
O4 Cu2 N2 85.81(8) . . ?
O6 Cu2 O1 88.70(7) 2_556 . ?
O6 Cu2 O3 96.69(7) 2_556 . ?
O6 Cu2 O4 92.61(7) 2_556 . ?
O6 Cu2 N2 177.49(8) 2_556 . ?
N2 Cu2 O3 81.60(7) . . ?
O4 Cu3 O5 173.15(7) 2_556 . ?
O4 Cu3 O9 93.21(7) 2_556 . ?
O4 Cu3 N3 89.42(7) 2_556 . ?
O5 Cu3 O9 86.78(7) . . ?
O5 Cu3 N3 91.12(8) . . ?
O9 Cu3 N3 175.02(7) . . ?
O2 Cu4 O5 88.32(7) . . ?
O2 Cu4 O7 93.81(7) . . ?
O2 Cu4 O8 96.39(8) . . ?
O2 Cu4 N4 177.56(10) . . ?
O5 Cu4 O8 93.59(7) . . ?
O5 Cu4 N4 91.85(8) . . ?
O7 Cu4 O5 152.94(8) . . ?
O7 Cu4 O8 112.91(8) . . ?
O7 Cu4 N4 87.14(8) . . ?
N4 Cu4 O8 81.17(8) . . ?
Cu1 O1 Cu2 121.05(8) . . ?
C1 O1 Cu1 120.54(14) . . ?
C1 O1 Cu2 110.93(13) . . ?
N1 O2 Cu4 116.75(13) . . ?
Cu2 O3 H3 109.9 . . ?
C12 O3 Cu2 102.26(14) . . ?
C12 O3 H3 109.5 . . ?
Cu3 O4 Cu2 118.15(8) 2_556 . ?
C14 O4 Cu2 114.35(14) . . ?
C14 O4 Cu3 127.25(15) . 2_556 ?
Cu3 O5 Cu4 113.86(7) . . ?
C15 O5 Cu3 125.37(15) . . ?
C15 O5 Cu4 108.46(14) . . ?
N3 O6 Cu2 118.17(13) . 2_556 ?
Cu4 O7 Cu1 116.17(8) . . ?
C26 O7 Cu1 127.71(15) . . ?
C26 O7 Cu4 113.85(15) . . ?
Cu4 O8 H8 91.8 . . ?
C28 O8 Cu4 103.52(17) . . ?
C28 O8 H8 109.5 . . ?
C39 O9 Cu3 109.41(18) . . ?
O2 N1 Cu1 119.76(14) . . ?
C7 N1 Cu1 125.48(16) . . ?
C7 N1 O2 114.67(18) . . ?
C10 N2 Cu2 112.54(14) . . ?
C11 N2 Cu2 111.10(15) . . ?
C11 N2 C10 108.94(19) . . ?
C13 N2 Cu2 102.17(14) . . ?
C13 N2 C10 111.13(18) . . ?
C13 N2 C11 110.9(2) . . ?
O6 N3 Cu3 118.74(13) . . ?
C21 N3 Cu3 126.65(16) . . ?
C21 N3 O6 113.83(19) . . ?
C24 N4 Cu4 113.48(15) . . ?
C25 N4 Cu4 102.85(15) . . ?
C25 N4 C24 110.6(2) . . ?
C27 N4 Cu4 108.22(16) . . ?
C27 N4 C24 110.5(2) . . ?
C27 N4 C25 111.0(2) . . ?
C29 N5 Cu1 129.1(2) . . ?
C29 N5 C33 119.1(2) . . ?
C33 N5 Cu1 110.87(18) . . ?
C34 N6 Cu1 117.41(18) . . ?
C38 N6 Cu1 122.77(18) . . ?
C38 N6 C34 119.5(2) . . ?
O1 C1 C2 118.5(2) . . ?
O1 C1 C6 122.28(19) . . ?
C6 C1 C2 119.2(2) . . ?
C1 C2 C10 119.0(2) . . ?
C3 C2 C1 120.3(2) . . ?
C3 C2 C10 120.6(2) . . ?
C2 C3 H3A 119.4 . . ?
C2 C3 C4 121.1(2) . . ?
C4 C3 H3A 119.4 . . ?
C3 C4 C9 120.6(2) . . ?
C5 C4 C3 118.2(2) . . ?
C5 C4 C9 121.2(2) . . ?
C4 C5 H5 118.7 . . ?
C4 C5 C6 122.6(2) . . ?
C6 C5 H5 118.7 . . ?
C1 C6 C5 118.1(2) . . ?
C1 C6 C7 123.1(2) . . ?
C5 C6 C7 118.7(2) . . ?
N1 C7 C6 121.3(2) . . ?
N1 C7 C8 118.6(2) . . ?
C6 C7 C8 120.0(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C2 113.47(19) . . ?
N2 C10 H10A 108.9 . . ?
N2 C10 H10B 108.9 . . ?
C2 C10 H10A 108.9 . . ?
C2 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
N2 C11 H11A 109.4 . . ?
N2 C11 H11B 109.4 . . ?
N2 C11 C12 111.1(2) . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
O3 C12 C11 110.4(2) . . ?
O3 C12 H12A 109.6 . . ?
O3 C12 H12B 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
N2 C13 H13A 109.8 . . ?
N2 C13 H13B 109.8 . . ?
N2 C13 C14 109.59(19) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
O4 C14 C13 108.45(19) . . ?
O4 C14 H14A 110.0 . . ?
O4 C14 H14B 110.0 . . ?
C13 C14 H14A 110.0 . . ?
C13 C14 H14B 110.0 . . ?
H14A C14 H14B 108.4 . . ?
O5 C15 C16 117.3(2) . . ?
O5 C15 C20 122.4(2) . . ?
C20 C15 C16 120.2(2) . . ?
C15 C16 C24 118.8(2) . . ?
C17 C16 C15 119.1(2) . . ?
C17 C16 C24 122.0(2) . . ?
C16 C17 H17 119.0 . . ?
C18 C17 C16 122.0(2) . . ?
C18 C17 H17 119.0 . . ?
C17 C18 C19 118.0(2) . . ?
C17 C18 C23 121.6(2) . . ?
C19 C18 C23 120.4(3) . . ?
C18 C19 H19 118.7 . . ?
C18 C19 C20 122.6(2) . . ?
C20 C19 H19 118.7 . . ?
C15 C20 C19 117.6(2) . . ?
C15 C20 C21 123.3(2) . . ?
C19 C20 C21 118.9(2) . . ?
N3 C21 C20 121.1(2) . . ?
N3 C21 C22 119.2(2) . . ?
C20 C21 C22 119.7(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 C16 113.0(2) . . ?
N4 C24 H24A 109.0 . . ?
N4 C24 H24B 109.0 . . ?
C16 C24 H24A 109.0 . . ?
C16 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
N4 C25 H25A 109.7 . . ?
N4 C25 H25B 109.7 . . ?
N4 C25 C26 109.7(2) . . ?
H25A C25 H25B 108.2 . . ?
C26 C25 H25A 109.7 . . ?
C26 C25 H25B 109.7 . . ?
O7 C26 C25 108.1(2) . . ?
O7 C26 H26A 110.1 . . ?
O7 C26 H26B 110.1 . . ?
C25 C26 H26A 110.1 . . ?
C25 C26 H26B 110.1 . . ?
H26A C26 H26B 108.4 . . ?
N4 C27 H27A 109.3 . . ?
N4 C27 H27B 109.3 . . ?
N4 C27 C28 111.8(2) . . ?
H27A C27 H27B 107.9 . . ?
C28 C27 H27A 109.3 . . ?
C28 C27 H27B 109.3 . . ?
O8 C28 C27 108.8(2) . . ?
O8 C28 H28A 109.9 . . ?
O8 C28 H28B 109.9 . . ?
C27 C28 H28A 109.9 . . ?
C27 C28 H28B 109.9 . . ?
H28A C28 H28B 108.3 . . ?
N5 C29 H29 118.7 . . ?
N5 C29 C30 122.7(3) . . ?
C30 C29 H29 118.7 . . ?
C29 C30 H30 120.8 . . ?
C31 C30 C29 118.4(3) . . ?
C31 C30 H30 120.8 . . ?
C30 C31 H31 120.0 . . ?
C30 C31 C32 119.9(3) . . ?
C32 C31 H31 120.0 . . ?
C31 C32 H32 120.7 . . ?
C31 C32 C33 118.7(3) . . ?
C33 C32 H32 120.7 . . ?
N5 C33 C32 121.1(3) . . ?
N5 C33 C34 115.5(2) . . ?
C32 C33 C34 123.4(3) . . ?
N6 C34 C33 116.2(2) . . ?
N6 C34 C35 120.4(3) . . ?
C35 C34 C33 123.4(3) . . ?
C34 C35 H35 120.4 . . ?
C36 C35 C34 119.2(3) . . ?
C36 C35 H35 120.4 . . ?
C35 C36 H36 119.9 . . ?
C37 C36 C35 120.1(3) . . ?
C37 C36 H36 119.9 . . ?
C36 C37 H37 121.0 . . ?
C36 C37 C38 117.9(3) . . ?
C38 C37 H37 121.0 . . ?
N6 C38 C37 122.8(3) . . ?
N6 C38 H38 118.6 . . ?
C37 C38 H38 118.6 . . ?
O9 C39 C40 116.1(3) . . ?
O10 C39 O9 122.7(3) . . ?
O10 C39 C40 121.2(3) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C45 O12 H12 109.5 . . ?
O12 C45 H45A 109.5 . . ?
O12 C45 H45B 109.5 . . ?
O12 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C46 O13 H13 109.5 . . ?
O13 C46 H46A 109.5 . . ?
O13 C46 H46B 109.5 . . ?
O13 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
F1 B1 F2 113.7(9) . . ?
F1 B1 F3 101.7(8) . . ?
F1 B1 F4 115.1(14) . . ?
F2 B1 F3 103.4(12) . . ?
F4 B1 F2 113.8(11) . . ?
F4 B1 F3 107.4(8) . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
C41 C42 H42A 108.3 . . ?
C41 C42 H42B 108.3 . . ?
H42A C42 H42B 107.4 . . ?
O11 C42 C41 116.0(6) . . ?
O11 C42 H42A 108.3 . . ?
O11 C42 H42B 108.3 . . ?
C43 O11 C42 116.7(5) . . ?
O11 C43 H43A 109.2 . . ?
O11 C43 H43B 109.2 . . ?
H43A C43 H43B 107.9 . . ?
C44 C43 O11 112.2(5) . . ?
C44 C43 H43A 109.2 . . ?
C44 C43 H43B 109.2 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
F2A B1A F1A 102.5(17) . . ?
F3A B1A F1A 100.5(14) . . ?
F3A B1A F2A 103.3(12) . . ?
F4A B1A F1A 99.7(15) . . ?
F4A B1A F2A 135.5(18) . . ?
F4A B1A F3A 109.8(18) . . ?
H41D C41A H41E 109.5 . . ?
H41D C41A H41F 109.5 . . ?
H41E C41A H41F 109.5 . . ?
C42A C41A H41D 109.5 . . ?
C42A C41A H41E 109.5 . . ?
C42A C41A H41F 109.5 . . ?
C41A C42A H42C 107.9 . . ?
C41A C42A H42D 107.9 . . ?
H42C C42A H42D 107.2 . . ?
O11A C42A C41A 117.7 . . ?
O11A C42A H42C 107.9 . . ?
O11A C42A H42D 107.9 . . ?
C43A O11A C42A 129.9 . . ?
O11A C43A H43C 108.8 . . ?
O11A C43A H43D 108.8 . . ?
O11A C43A C44A 113.6 . . ?
H43C C43A H43D 107.7 . . ?
C44A C43A H43C 108.8 . . ?
C44A C43A H43D 108.8 . . ?
C43A C44A H44D 109.5 . . ?
C43A C44A H44E 109.5 . . ?
C43A C44A H44F 109.5 . . ?
H44D C44A H44E 109.5 . . ?
H44D C44A H44F 109.5 . . ?
H44E C44A H44F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O12 0.84 1.87 2.695(3) 168.9 2_556
O8 H8 O9 0.84 1.90 2.731(3) 172.1 .
O12 H12 O10 0.84 1.90 2.741(3) 174.9 .
O13 H13 F2 0.84 2.02 2.848(14) 170.2 .
O13 H13 F3A 0.84 1.52 2.357(17) 176.8 .

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
Cu1 O1 C1 C2 -151.02(16) . . . . ?
Cu1 O1 C1 C6 31.0(3) . . . . ?
Cu1 O7 C26 C25 173.73(19) . . . . ?
Cu1 N1 C7 C6 1.9(3) . . . . ?
Cu1 N1 C7 C8 -175.1(2) . . . . ?
Cu1 N5 C29 C30 166.9(2) . . . . ?
Cu1 N5 C33 C32 -167.5(2) . . . . ?
Cu1 N5 C33 C34 13.3(3) . . . . ?
Cu1 N6 C34 C33 -8.4(3) . . . . ?
Cu1 N6 C34 C35 172.0(2) . . . . ?
Cu1 N6 C38 C37 -172.6(2) . . . . ?
Cu2 O1 C1 C2 58.9(2) . . . . ?
Cu2 O1 C1 C6 -119.1(2) . . . . ?
Cu2 O3 C12 C11 43.0(2) . . . . ?
Cu2 O4 C14 C13 17.2(2) . . . . ?
Cu2 O6 N3 Cu3 20.2(2) 2_556 . . . ?
Cu2 O6 N3 C21 -169.31(15) 2_556 . . . ?
Cu2 N2 C10 C2 46.5(2) . . . . ?
Cu2 N2 C11 C12 36.0(3) . . . . ?
Cu2 N2 C13 C14 46.0(2) . . . . ?
Cu3 O4 C14 C13 -157.03(16) 2_556 . . . ?
Cu3 O5 C15 C16 158.50(16) . . . . ?
Cu3 O5 C15 C20 -24.3(3) . . . . ?
Cu3 O9 C39 O10 4.8(4) . . . . ?
Cu3 O9 C39 C40 -174.4(4) . . . . ?
Cu3 N3 C21 C20 -11.4(3) . . . . ?
Cu3 N3 C21 C22 166.41(17) . . . . ?
Cu4 O2 N1 Cu1 -20.9(2) . . . . ?
Cu4 O2 N1 C7 162.45(17) . . . . ?
Cu4 O5 C15 C16 -62.0(2) . . . . ?
Cu4 O5 C15 C20 115.2(2) . . . . ?
Cu4 O7 C26 C25 -24.2(3) . . . . ?
Cu4 O8 C28 C27 -36.1(2) . . . . ?
Cu4 N4 C24 C16 -41.8(3) . . . . ?
Cu4 N4 C25 C26 -42.4(2) . . . . ?
Cu4 N4 C27 C28 -48.6(3) . . . . ?
O1 C1 C2 C3 178.0(2) . . . . ?
O1 C1 C2 C10 0.1(3) . . . . ?
O1 C1 C6 C5 -175.0(2) . . . . ?
O1 C1 C6 C7 9.9(3) . . . . ?
O2 Cu4 O7 Cu1 -13.31(11) . . . . ?
O2 Cu4 O7 C26 -177.55(19) . . . . ?
O2 N1 C7 C6 178.4(2) . . . . ?
O2 N1 C7 C8 1.3(4) . . . . ?
O5 Cu4 O2 N1 173.28(16) . . . . ?
O5 Cu4 O7 Cu1 -107.08(15) . . . . ?
O5 Cu4 O7 C26 88.7(2) . . . . ?
O5 C15 C16 C17 -177.3(2) . . . . ?
O5 C15 C16 C24 -0.9(3) . . . . ?
O5 C15 C20 C19 175.6(2) . . . . ?
O5 C15 C20 C21 -8.5(3) . . . . ?
O6 N3 C21 C20 179.00(19) . . . . ?
O6 N3 C21 C22 -3.2(3) . . . . ?
O7 Cu4 O2 N1 20.28(17) . . . . ?
O8 Cu4 O2 N1 -93.30(16) . . . . ?
O8 Cu4 O7 Cu1 85.27(11) . . . . ?
O8 Cu4 O7 C26 -79.0(2) . . . . ?
N2 C11 C12 O3 -56.1(3) . . . . ?
N2 C13 C14 O4 -43.2(3) . . . . ?
N4 Cu4 O7 Cu1 164.43(12) . . . . ?
N4 Cu4 O7 C26 0.2(2) . . . . ?
N4 C25 C26 O7 45.1(3) . . . . ?
N4 C27 C28 O8 59.2(3) . . . . ?
N5 C29 C30 C31 -1.5(5) . . . . ?
N5 C33 C34 N6 -4.4(3) . . . . ?
N5 C33 C34 C35 175.2(3) . . . . ?
N6 C34 C35 C36 0.6(4) . . . . ?
C1 C2 C3 C4 -2.3(4) . . . . ?
C1 C2 C10 N2 -60.6(3) . . . . ?
C1 C6 C7 N1 -28.3(4) . . . . ?
C1 C6 C7 C8 148.7(3) . . . . ?
C2 C1 C6 C5 7.0(3) . . . . ?
C2 C1 C6 C7 -168.0(2) . . . . ?
C2 C3 C4 C5 5.2(4) . . . . ?
C2 C3 C4 C9 -173.2(2) . . . . ?
C3 C2 C10 N2 121.6(2) . . . . ?
C3 C4 C5 C6 -1.9(4) . . . . ?
C4 C5 C6 C1 -4.2(4) . . . . ?
C4 C5 C6 C7 171.1(2) . . . . ?
C5 C6 C7 N1 156.7(2) . . . . ?
C5 C6 C7 C8 -26.3(4) . . . . ?
C6 C1 C2 C3 -4.0(3) . . . . ?
C6 C1 C2 C10 178.2(2) . . . . ?
C9 C4 C5 C6 176.5(3) . . . . ?
C10 N2 C11 C12 -88.5(2) . . . . ?
C10 N2 C13 C14 166.23(19) . . . . ?
C10 C2 C3 C4 175.5(2) . . . . ?
C11 N2 C10 C2 170.2(2) . . . . ?
C11 N2 C13 C14 -72.5(2) . . . . ?
C13 N2 C10 C2 -67.4(2) . . . . ?
C13 N2 C11 C12 148.9(2) . . . . ?
C15 C16 C17 C18 0.8(4) . . . . ?
C15 C16 C24 N4 60.6(3) . . . . ?
C15 C20 C21 N3 27.0(3) . . . . ?
C15 C20 C21 C22 -150.7(2) . . . . ?
C16 C15 C20 C19 -7.3(3) . . . . ?
C16 C15 C20 C21 168.6(2) . . . . ?
C16 C17 C18 C19 -4.9(4) . . . . ?
C16 C17 C18 C23 175.2(2) . . . . ?
C17 C16 C24 N4 -123.1(2) . . . . ?
C17 C18 C19 C20 2.8(4) . . . . ?
C18 C19 C20 C15 3.2(4) . . . . ?
C18 C19 C20 C21 -172.9(2) . . . . ?
C19 C20 C21 N3 -157.2(2) . . . . ?
C19 C20 C21 C22 25.1(3) . . . . ?
C20 C15 C16 C17 5.4(3) . . . . ?
C20 C15 C16 C24 -178.2(2) . . . . ?
C23 C18 C19 C20 -177.2(2) . . . . ?
C24 N4 C25 C26 -163.9(2) . . . . ?
C24 N4 C27 C28 76.2(3) . . . . ?
C24 C16 C17 C18 -175.5(2) . . . . ?
C25 N4 C24 C16 73.1(3) . . . . ?
C25 N4 C27 C28 -160.8(2) . . . . ?
C27 N4 C24 C16 -163.6(2) . . . . ?
C27 N4 C25 C26 73.1(3) . . . . ?
C29 N5 C33 C32 2.3(4) . . . . ?
C29 N5 C33 C34 -177.0(2) . . . . ?
C29 C30 C31 C32 2.3(5) . . . . ?
C30 C31 C32 C33 -0.8(5) . . . . ?
C31 C32 C33 N5 -1.5(4) . . . . ?
C31 C32 C33 C34 177.7(3) . . . . ?
C32 C33 C34 N6 176.4(2) . . . . ?
C32 C33 C34 C35 -4.0(4) . . . . ?
C33 N5 C29 C30 -0.7(4) . . . . ?
C33 C34 C35 C36 -178.9(3) . . . . ?
C34 N6 C38 C37 0.6(4) . . . . ?
C34 C35 C36 C37 1.2(4) . . . . ?
C35 C36 C37 C38 -2.1(4) . . . . ?
C36 C37 C38 N6 1.2(4) . . . . ?
C38 N6 C34 C33 178.0(2) . . . . ?
C38 N6 C34 C35 -1.5(4) . . . . ?
C41 C42 O11 C43 168.8(7) . . . . ?
C42 O11 C43 C44 -173.0(8) . . . . ?
C41A C42A O11A C43A 100.2 . . . . ?
C42A O11A C43A C44A 178.0 . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-11 20 -14 0.0889 -11.0000 20.0000 -14.0002 0.5953 0.7970 0.0814
-20 1 33 0.2019 -20.0000 0.9999 33.0004 -0.0166 -0.0356 -0.9968
-5 -13 31 0.2283 -5.0000 -13.0000 31.0004 -0.4305 -0.5657 -0.6964
21 -18 -6 0.1094 21.0000 -18.0000 -6.0001 -0.5202 -0.6746 0.4843
23 -17 -11 0.1249 23.0000 -17.0000 -11.0001 -0.4863 -0.6249 0.6171
6 -7 -35 0.1549 6.0001 -6.9999 -35.0003 0.4178 -0.2505 0.8607
-23 -11 -16 0.1084 -22.9999 -11.0000 -16.0000 0.8742 -0.5099 0.0537
23 11 15 0.1050 22.9999 11.0000 15.0000 -0.8570 0.5105 -0.0322
20 11 19 0.0830 19.9999 11.0000 19.0000 -0.8436 0.4995 -0.1608
4 24 2 0.1085 3.9999 24.0000 1.9999 -0.0789 0.9961 -0.0632
14 -14 -28 0.1420 14.0001 -13.9999 -28.0002 0.0598 -0.5185 0.8458
19 14 -25 0.2313 19.0000 14.0000 -25.0004 -0.0528 0.6442 0.7624
4 -22 -14 0.1063 4.0001 -21.9999 -14.0000 0.0715 -0.8840 0.4284
-19 -14 25 0.1966 -19.0000 -14.0000 25.0004 0.0528 -0.6442 -0.7624
-4 -24 -2 0.1315 -3.9999 -24.0000 -1.9999 0.0789 -0.9961 0.0632
-24 6 -18 0.0984 -23.9999 6.0000 -18.0001 0.9818 0.1864 0.0281
-2 3 -36 0.1473 -1.9999 3.0001 -36.0003 0.6808 0.1374 0.7369
-15 1 35 0.2016 -15.0001 0.9999 35.0004 -0.1878 -0.0221 -0.9690
24 -6 18 0.1346 23.9999 -6.0000 18.0001 -0.9818 -0.1864 -0.0281
-24 -16 -1 0.1308 -23.9999 -16.0000 -0.9998 0.6305 -0.7265 -0.2673
26 -14 -1 0.1187 26.0000 -14.0000 -1.0001 -0.7320 -0.4985 0.4347
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 991826'
_audit_update_record             
;
2014-10-16 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
# local name eb3284b
_audit_creation_date             2013-11-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715)
;
_shelxl_version_number           2013-4
_publ_section_exptl              
;
Any special experimental details
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H76 Cu8 N20 O16'
_chemical_formula_sum            'C67 H120 Cu8 N20 O27'
_chemical_formula_weight         2146.17
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H40 N5 O10 Cu4'
_chemical_oxdiff_usercomment     '@ 120 K RS100(Et)'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   25.2990(5)
_cell_length_b                   20.7375(4)
_cell_length_c                   32.5445(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17074.1(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    16475
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.8530
_cell_measurement_theta_min      3.8660
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.883
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             8880
_exptl_crystal_size_max          0.4772
_exptl_crystal_size_mid          0.1391
_exptl_crystal_size_min          0.0295
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            87780
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.987
_diffrn_reflns_theta_min         3.072
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0085270000
_diffrn_orient_matrix_UB_12      0.0006366000
_diffrn_orient_matrix_UB_13      -0.0469074000
_diffrn_orient_matrix_UB_21      -0.0550907000
_diffrn_orient_matrix_UB_22      0.0301132000
_diffrn_orient_matrix_UB_23      0.0062288000
_diffrn_orient_matrix_UB_31      0.0244947000
_diffrn_orient_matrix_UB_32      0.0678523000
_diffrn_orient_matrix_UB_33      -0.0022842000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12269
_reflns_number_total             17342
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    
;
%$getVar(olex2_reference_short)%
;
_computing_publication_material  
;
%$getVar(olex2_reference_short)%
;
_computing_structure_refinement  
;
%$getVar(refinement_reference_short)%
;
_computing_structure_solution    
;
%$getVar(solution_reference_short)%
;
_refine_diff_density_max         2.987
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         17342
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0956
_refine_ls_restrained_S_all      1.073
_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)+(0.1031P)²+162.7584P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2426
_refine_ls_wR_factor_ref         0.2636
_refine_special_details          
;
The SQUEEZE routine of PLATON removed electron density corresponding to eleven 
molecules of methanol per asymmetric unit which could not be modelled.  The 
chemical formula includes this solvent which is missing from the model and 
this causes alerts in checkCIF which shoudl be ignored.

The crystals were few in number and of poor quality, suffering badly from 
stacking faults as evidenced by broad reflections and diffuse scattering.  
This is reflected in the high refinement residuals.

Three of the azide ligands are well behaved.  The fourth, defined by N12 to 
N14, manifestly is not.  It was refined over three positions with site 
occupancies refined as free variables which sum to 1.  The major component 
was refined anisotropcally.  The two minor components were refined with 
Uiso = 0.05.  Bond distances were restrained to be similar to those in a 
well-behaved ligand.


The largest peak is 3 e.A-3 high located 1.74 A from N14A.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
051_ALERT_1_B Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .       7.09 %

SQUEEZE used.  See above.

097_ALERT_2_B Large Reported Max.  (Positive) Residual Density       2.99 eA-3

The largest peak is 3 e.A-3 high located 1.74 A from N14A.  See above.


220_ALERT_2_B Large Non-Solvent    N     Ueq(max)/Ueq(min) ...        5.6 Ratio

See above.

415_ALERT_2_B Short Inter D-H..H-X       H12    ..  H38B    ..       2.03 Ang.
415_ALERT_2_B Short Inter D-H..H-X       H16    ..  H52A    ..       2.06 Ang.

H atoms positioned without recourse to residual density.

420_ALERT_2_B D-H Without Acceptor       O4     -   H4     ...     Please Check
420_ALERT_2_B D-H Without Acceptor       O8     -   H8     ...     Please Check
420_ALERT_2_B D-H Without Acceptor       O12    -   H12    ...     Please Check
420_ALERT_2_B D-H Without Acceptor       O16    -   H16    ...     Please Check

SQUEEZE used.  

#===============================================================================
041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ     Please Check
068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...     Please Check

SQUEEZE used.

084_ALERT_3_C High wR2 Value (i.e. > 0.25) ...................       0.26
094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       3.65
213_ALERT_2_C Atom N14             has ADP max/min Ratio .....        3.6 prolat
241_ALERT_2_C High      Ueq as Compared to Neighbors for .....         O8 Check
242_ALERT_2_C Low       Ueq as Compared to Neighbors for .....        N19 Check
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0116 Ang.

Problematic refinement, see above

#===============================================================================


;


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.001 -0.004 0.000 2194 701 ' '
2 0.523 -0.005 0.500 2194 703 ' '
3 0.879 0.009 0.655 7 1 ' '
4 0.379 0.009 0.845 7 1 ' '
5 0.879 0.491 0.155 7 1 ' '
6 0.379 0.491 0.345 7 1 ' '
7 0.621 0.509 0.655 7 1 ' '
8 0.121 0.509 0.845 7 1 ' '
9 0.621 0.991 0.155 7 1 ' '
10 0.121 0.991 0.345 7 1 ' '
_platon_squeeze_details          
'11 MeOH per asymmetric unit removed with SQUEEZE'

_vrf_CHEMW03_eb3284b             
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Please see the _refine_special_details section of the CIF.
;


_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O12-H12
 0.85 with sigma of 0.01
 O16-H16
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 O8-H8
 0.85 with sigma of 0.01
 C56-H12
 1.891964 with sigma of 0.02
 Cu6-H12
 3.078947 with sigma of 0.02
 C40-H16
 1.921845 with sigma of 0.02
 Cu8-H16
 3.121661 with sigma of 0.02
 C14-H4
 1.895716 with sigma of 0.02
 Cu2-H4
 3.135147 with sigma of 0.02
 C28-H8
 1.907963 with sigma of 0.02
 Cu4-H8
 3.07293 with sigma of 0.02
 Cu3-N12A \\sim Cu3-N12B \\sim Cu3-N12 \\sim Cu5-N15
 with sigma of 0.02
 N13A-N12A \\sim N13B-N12B \\sim N13-N12 \\sim N16-N15
 with sigma of 0.02
 N14A-N13A \\sim N14B-N13B \\sim N14-N13 \\sim N17-N16
 with sigma of 0.02
 N12A-N14A \\sim N15-N17
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N12, N13, N14, Cu3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C56, C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 1*[Sof(N12)+Sof(N13)+Sof(N14)]+1*[Sof(N12B)+Sof(N13B)+Sof(N14B)]+1*[Sof(N12A)+
 Sof(N13A)+Sof(N14A)]=1 with esd of 0.001
 Sof(N12)=Sof(N13)=Sof(N14)=FVAR(1)
 Sof(N12B)=Sof(N13B)=Sof(N14B)=FVAR(2)
 Sof(N12A)=Sof(N13A)=Sof(N14A)=FVAR(3)
 Fixed Uiso: N12A(0.05) N12B(0.05) N13A(0.05) N13B(0.05) N14A(0.05) N14B(0.05)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
  C42(H42A,H42B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C56(H56A,H56B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C31(H31), C33(H33), C45(H45), C47(H47)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.39752(4) 0.81597(5) 0.84486(4) 0.0298(3) Uani 1 1 d . . . . .
Cu2 Cu 0.42187(4) 0.87140(5) 0.75235(4) 0.0289(3) Uani 1 1 d D . . . .
Cu3 Cu 0.35970(5) 0.99769(6) 0.71688(4) 0.0367(3) Uani 1 1 d . . . . .
Cu4 Cu 0.33933(4) 1.14569(5) 0.75375(3) 0.0270(2) Uani 1 1 d D . . . .
Cu5 Cu 0.39918(4) 1.19805(5) 0.83576(3) 0.0270(2) Uani 1 1 d . . . . .
Cu6 Cu 0.41775(4) 1.14438(5) 0.92894(3) 0.0271(2) Uani 1 1 d D . . . .
Cu7 Cu 0.35579(4) 1.01618(5) 0.96020(4) 0.0308(3) Uani 1 1 d . . . . .
Cu8 Cu 0.33435(4) 0.86944(5) 0.92557(3) 0.0281(3) Uani 1 1 d D . . . .
O1 O 0.45018(19) 0.8328(2) 0.80361(17) 0.0305(11) Uani 1 1 d . . . . .
O2 O 0.3932(2) 0.9168(3) 0.90627(18) 0.0361(13) Uani 1 1 d . . . . .
O3 O 0.4146(2) 0.9356(3) 0.71113(18) 0.0361(13) Uani 1 1 d . . . . .
O4 O 0.3787(2) 0.7762(3) 0.72892(19) 0.0378(13) Uani 1 1 d D . . . .
H4 H 0.3526(14) 0.7510(17) 0.733(2) 0.057 Uiso 1 1 d DR . . . .
O5 O 0.3103(2) 1.0654(3) 0.72941(18) 0.0341(12) Uani 1 1 d . . . . .
O6 O 0.3657(2) 0.9047(3) 0.78368(17) 0.0356(12) Uani 1 1 d . . . . .
O7 O 0.3463(2) 1.2101(2) 0.79475(17) 0.0301(11) Uani 1 1 d . . . . .
O8 O 0.3818(3) 1.1883(4) 0.6966(2) 0.070(2) Uani 1 1 d D . . . .
H8 H 0.4087(15) 1.184(4) 0.6809(14) 0.106 Uiso 1 1 d DR . . . .
O9 O 0.44970(19) 1.1808(2) 0.87806(17) 0.0307(11) Uani 1 1 d . . . . .
O10 O 0.3954(2) 1.0966(3) 0.77526(17) 0.0341(12) Uani 1 1 d . . . . .
O11 O 0.4083(2) 1.0804(3) 0.96980(16) 0.0311(11) Uani 1 1 d . . . . .
O12 O 0.3780(2) 1.2422(3) 0.94982(19) 0.0386(13) Uani 1 1 d D . . . .
H12 H 0.3524(16) 1.2671(16) 0.943(2) 0.058 Uiso 1 1 d DR . . . .
O13 O 0.3046(2) 0.9505(2) 0.94738(16) 0.0305(11) Uani 1 1 d . . . . .
O14 O 0.3619(2) 1.1129(3) 0.89621(16) 0.0314(11) Uani 1 1 d . . . . .
O15 O 0.3430(2) 0.8040(2) 0.88526(17) 0.0315(12) Uani 1 1 d . . . . .
O16 O 0.3727(2) 0.8308(3) 0.98735(19) 0.0482(16) Uani 1 1 d D . . . .
H16 H 0.3984(16) 0.836(4) 1.0039(12) 0.072 Uiso 1 1 d DR . . . .
N1 N 0.4258(2) 0.8883(3) 0.8788(2) 0.0294(13) Uani 1 1 d . . . . .
N2 N 0.4803(3) 0.8344(3) 0.7183(2) 0.0341(15) Uani 1 1 d . . . . .
N3 N 0.3328(3) 0.9471(3) 0.7645(2) 0.0300(14) Uani 1 1 d . . . . .
N4 N 0.2795(3) 1.1992(3) 0.7312(2) 0.0310(14) Uani 1 1 d . . . . .
N5 N 0.4272(2) 1.1234(3) 0.8035(2) 0.0283(13) Uani 1 1 d . . . . .
N6 N 0.4764(2) 1.1796(3) 0.9641(2) 0.0311(14) Uani 1 1 d . . . . .
N7 N 0.3285(2) 1.0693(3) 0.91358(19) 0.0282(13) Uani 1 1 d . . . . .
N8 N 0.2728(2) 0.8172(3) 0.9468(2) 0.0314(14) Uani 1 1 d . . . . .
N9 N 0.3721(3) 0.7445(3) 0.8092(2) 0.0406(17) Uani 1 1 d . . . . .
N10 N 0.3717(3) 0.6911(3) 0.8250(3) 0.0402(17) Uani 1 1 d . . . . .
N11 N 0.3707(3) 0.6399(3) 0.8395(3) 0.055(2) Uani 1 1 d . . . . .
N12 N 0.3881(7) 1.0561(7) 0.6718(4) 0.059(4) Uani 0.563(11) 1 d . . P A 1
N12A N 0.3128(13) 0.9605(17) 0.6690(8) 0.050 Uiso 0.203(8) 1 d . . P A 3
N12B N 0.3674(12) 1.0268(18) 0.6578(6) 0.050 Uiso 0.234(9) 1 d . . P A 2
N13 N 0.3983(9) 1.0408(9) 0.6371(4) 0.099(7) Uani 0.563(11) 1 d . . P A 1
N13A N 0.2884(14) 0.9778(19) 0.6382(8) 0.050 Uiso 0.203(8) 1 d . . P A 3
N13B N 0.3291(12) 1.0529(16) 0.6434(10) 0.050 Uiso 0.234(9) 1 d . . P A 2
N14 N 0.3850(14) 1.0201(9) 0.6049(6) 0.156(12) Uani 0.563(11) 1 d . . P A 1
N14A N 0.2803(15) 0.980(2) 0.6031(8) 0.050 Uiso 0.203(8) 1 d . . P A 3
N14B N 0.2965(12) 1.0795(16) 0.6247(10) 0.050 Uiso 0.234(9) 1 d . . P A 2
N15 N 0.3793(3) 1.2763(3) 0.8681(2) 0.0427(17) Uani 1 1 d . . . . .
N16 N 0.3743(3) 1.3271(3) 0.8516(2) 0.0390(16) Uani 1 1 d . . . . .
N17 N 0.3691(3) 1.3767(3) 0.8365(2) 0.0440(18) Uani 1 1 d . . . . .
N18 N 0.3769(4) 0.9634(4) 1.0073(3) 0.057(2) Uani 1 1 d . . . . .
N19 N 0.3723(4) 0.9898(4) 1.0377(3) 0.058(2) Uani 1 1 d . . . . .
N20 N 0.3705(5) 1.0172(6) 1.0702(3) 0.090(4) Uani 1 1 d . . . . .
C1 C 0.4988(3) 0.8556(4) 0.8102(3) 0.0314(17) Uani 1 1 d . . . . .
C2 C 0.5375(3) 0.8439(4) 0.7807(3) 0.0317(17) Uani 1 1 d . . . . .
C3 C 0.5888(3) 0.8657(4) 0.7860(3) 0.0376(19) Uani 1 1 d . . . . .
H3 H 0.6140 0.8589 0.7648 0.045 Uiso 1 1 calc R . . . .
C4 C 0.6044(3) 0.8979(4) 0.8222(3) 0.042(2) Uani 1 1 d . . . . .
C5 C 0.5655(3) 0.9115(4) 0.8508(3) 0.0345(17) Uani 1 1 d . . . . .
H5 H 0.5749 0.9347 0.8749 0.041 Uiso 1 1 calc R . . . .
C6 C 0.5118(3) 0.8924(4) 0.8456(2) 0.0293(16) Uani 1 1 d . . . . .
C7 C 0.4721(3) 0.9157(3) 0.8753(2) 0.0281(15) Uani 1 1 d . . . . .
C8 C 0.4825(3) 0.9747(4) 0.9011(3) 0.0354(18) Uani 1 1 d . . . . .
H8A H 0.4568 1.0083 0.8942 0.053 Uiso 1 1 calc GR . . . .
H8B H 0.5183 0.9906 0.8955 0.053 Uiso 1 1 calc GR . . . .
H8C H 0.4794 0.9636 0.9302 0.053 Uiso 1 1 calc GR . . . .
C9 C 0.6618(4) 0.9174(6) 0.8284(4) 0.062(3) Uani 1 1 d . . . . .
H9A H 0.6846 0.8795 0.8252 0.093 Uiso 1 1 calc GR . . . .
H9B H 0.6663 0.9353 0.8560 0.093 Uiso 1 1 calc GR . . . .
H9C H 0.6716 0.9500 0.8079 0.093 Uiso 1 1 calc GR . . . .
C10 C 0.5243(3) 0.8053(4) 0.7427(3) 0.0356(18) Uani 1 1 d . . . . .
H10A H 0.5562 0.8022 0.7251 0.043 Uiso 1 1 calc R . . . .
H10B H 0.5143 0.7610 0.7509 0.043 Uiso 1 1 calc R . . . .
C11 C 0.4996(3) 0.8928(4) 0.6955(3) 0.0378(19) Uani 1 1 d . . . . .
H11A H 0.5223 0.8792 0.6723 0.045 Uiso 1 1 calc R . . . .
H11B H 0.5211 0.9200 0.7141 0.045 Uiso 1 1 calc R . . . .
C12 C 0.4530(3) 0.9316(4) 0.6793(3) 0.042(2) Uani 1 1 d . . . . .
H12A H 0.4648 0.9754 0.6712 0.051 Uiso 1 1 calc R . . . .
H12B H 0.4377 0.9102 0.6548 0.051 Uiso 1 1 calc R . . . .
C13 C 0.4578(3) 0.7849(4) 0.6896(3) 0.043(2) Uani 1 1 d . . . . .
H13A H 0.4389 0.8071 0.6670 0.051 Uiso 1 1 calc R . . . .
H13B H 0.4871 0.7599 0.6772 0.051 Uiso 1 1 calc R . . . .
C14 C 0.4205(3) 0.7394(4) 0.7106(3) 0.041(2) Uani 1 1 d D . . . .
H14A H 0.4057 0.7086 0.6904 0.049 Uiso 1 1 calc R . . . .
H14B H 0.4395 0.7146 0.7319 0.049 Uiso 1 1 calc R . . . .
C15 C 0.2615(3) 1.0548(4) 0.7439(3) 0.0312(17) Uani 1 1 d . . . . .
C16 C 0.2222(3) 1.1011(4) 0.7345(3) 0.0325(17) Uani 1 1 d . . . . .
C17 C 0.1701(3) 1.0910(4) 0.7477(2) 0.0317(16) Uani 1 1 d . . . . .
H17 H 0.1444 1.1236 0.7430 0.038 Uiso 1 1 calc R . . . .
C18 C 0.1550(3) 1.0344(4) 0.7673(3) 0.0349(18) Uani 1 1 d . . . . .
C19 C 0.1943(3) 0.9910(4) 0.7777(3) 0.0338(17) Uani 1 1 d . . . . .
H19 H 0.1848 0.9534 0.7926 0.041 Uiso 1 1 calc R . . . .
C20 C 0.2474(3) 1.0004(4) 0.7672(3) 0.0310(16) Uani 1 1 d . . . . .
C21 C 0.2877(3) 0.9540(4) 0.7834(3) 0.0329(17) Uani 1 1 d . . . . .
C22 C 0.2773(3) 0.9170(4) 0.8223(3) 0.040(2) Uani 1 1 d . . . . .
H22A H 0.2799 0.8706 0.8168 0.060 Uiso 1 1 calc GR . . . .
H22B H 0.2417 0.9270 0.8324 0.060 Uiso 1 1 calc GR . . . .
H22C H 0.3034 0.9291 0.8432 0.060 Uiso 1 1 calc GR . . . .
C23 C 0.0991(3) 1.0221(4) 0.7777(3) 0.046(2) Uani 1 1 d . . . . .
H23A H 0.0821 0.9986 0.7551 0.068 Uiso 1 1 calc GR . . . .
H23B H 0.0808 1.0632 0.7820 0.068 Uiso 1 1 calc GR . . . .
H23C H 0.0971 0.9963 0.8029 0.068 Uiso 1 1 calc GR . . . .
C24 C 0.2380(3) 1.1599(4) 0.7109(3) 0.0351(18) Uani 1 1 d . . . . .
H24A H 0.2510 1.1465 0.6835 0.042 Uiso 1 1 calc R . . . .
H24B H 0.2064 1.1872 0.7066 0.042 Uiso 1 1 calc R . . . .
C25 C 0.2593(3) 1.2311(4) 0.7691(3) 0.0338(17) Uani 1 1 d . . . . .
H25A H 0.2391 1.1995 0.7857 0.041 Uiso 1 1 calc R . . . .
H25B H 0.2351 1.2667 0.7615 0.041 Uiso 1 1 calc R . . . .
C26 C 0.3051(3) 1.2578(4) 0.7946(3) 0.0319(17) Uani 1 1 d . . . . .
H26A H 0.3183 1.2985 0.7824 0.038 Uiso 1 1 calc R . . . .
H26B H 0.2933 1.2667 0.8231 0.038 Uiso 1 1 calc R . . . .
C27 C 0.3011(4) 1.2474(4) 0.7015(3) 0.042(2) Uani 1 1 d . . . . .
H27A H 0.3185 1.2827 0.7169 0.051 Uiso 1 1 calc R . . . .
H27B H 0.2716 1.2664 0.6856 0.051 Uiso 1 1 calc R . . . .
C28 C 0.3400(4) 1.2178(6) 0.6726(3) 0.060(3) Uani 1 1 d D . . . .
H28A H 0.3223 1.1848 0.6555 0.072 Uiso 1 1 calc R . . . .
H28B H 0.3548 1.2512 0.6543 0.072 Uiso 1 1 calc R . . . .
C29 C 0.2556(3) 0.9624(4) 0.9332(2) 0.0292(16) Uani 1 1 d . . . . .
C30 C 0.2158(3) 0.9176(4) 0.9424(2) 0.0312(16) Uani 1 1 d . . . . .
C31 C 0.1641(3) 0.9278(4) 0.9306(2) 0.0336(17) Uani 1 1 d . . . . .
H31 H 0.1381 0.8959 0.9359 0.040 Uiso 1 1 calc R . . . .
C32 C 0.1500(3) 0.9854(4) 0.9108(3) 0.0382(19) Uani 1 1 d . . . . .
C33 C 0.1891(3) 1.0281(4) 0.9000(2) 0.0330(17) Uani 1 1 d . . . . .
H33 H 0.1798 1.0661 0.8855 0.040 Uiso 1 1 calc R . . . .
C34 C 0.2433(3) 1.0170(3) 0.9101(2) 0.0274(15) Uani 1 1 d . . . . .
C35 C 0.2834(3) 1.0622(4) 0.8955(2) 0.0288(16) Uani 1 1 d . . . . .
C36 C 0.2741(3) 1.1003(4) 0.8562(3) 0.0343(17) Uani 1 1 d . . . . .
H36A H 0.2755 1.1465 0.8622 0.052 Uiso 1 1 calc GR . . . .
H36B H 0.2392 1.0894 0.8449 0.052 Uiso 1 1 calc GR . . . .
H36C H 0.3014 1.0894 0.8360 0.052 Uiso 1 1 calc GR . . . .
C37 C 0.0930(3) 0.9987(4) 0.9000(3) 0.046(2) Uani 1 1 d . . . . .
H37A H 0.0801 0.9653 0.8813 0.069 Uiso 1 1 calc GR . . . .
H37B H 0.0904 1.0410 0.8867 0.069 Uiso 1 1 calc GR . . . .
H37C H 0.0716 0.9987 0.9251 0.069 Uiso 1 1 calc GR . . . .
C38 C 0.2302(3) 0.8576(4) 0.9663(3) 0.0356(18) Uani 1 1 d . . . . .
H38A H 0.2421 0.8706 0.9941 0.043 Uiso 1 1 calc R . . . .
H38B H 0.1981 0.8308 0.9697 0.043 Uiso 1 1 calc R . . . .
C39 C 0.2929(3) 0.7696(4) 0.9773(3) 0.0391(19) Uani 1 1 d . . . . .
H39A H 0.3127 0.7354 0.9627 0.047 Uiso 1 1 calc R . . . .
H39B H 0.2625 0.7491 0.9914 0.047 Uiso 1 1 calc R . . . .
C40 C 0.3289(4) 0.8003(5) 1.0094(3) 0.049(2) Uani 1 1 d D . . . .
H40A H 0.3091 0.8329 1.0255 0.059 Uiso 1 1 calc R . . . .
H40B H 0.3424 0.7671 1.0285 0.059 Uiso 1 1 calc R . . . .
C41 C 0.2534(3) 0.7856(4) 0.9085(2) 0.0288(15) Uani 1 1 d . . . . .
H41A H 0.2342 0.8174 0.8914 0.035 Uiso 1 1 calc R . . . .
H41B H 0.2288 0.7502 0.9155 0.035 Uiso 1 1 calc R . . . .
C42 C 0.3008(3) 0.7589(4) 0.8848(3) 0.0336(17) Uani 1 1 d . . . . .
H42A H 0.3125 0.7179 0.8974 0.040 Uiso 1 1 calc R . . . .
H42B H 0.2903 0.7499 0.8561 0.040 Uiso 1 1 calc R . . . .
C43 C 0.4982(3) 1.1540(4) 0.8730(2) 0.0290(16) Uani 1 1 d . . . . .
C44 C 0.5363(3) 1.1676(4) 0.9039(3) 0.0315(17) Uani 1 1 d . . . . .
C45 C 0.5872(3) 1.1441(4) 0.8997(3) 0.0362(18) Uani 1 1 d . . . . .
H45 H 0.6127 1.1530 0.9204 0.043 Uiso 1 1 calc R . . . .
C46 C 0.6017(3) 1.1076(5) 0.8656(3) 0.040(2) Uani 1 1 d . . . . .
C47 C 0.5631(3) 1.0916(4) 0.8373(2) 0.0337(17) Uani 1 1 d . . . . .
H47 H 0.5721 1.0640 0.8151 0.040 Uiso 1 1 calc R . . . .
C48 C 0.5108(3) 1.1148(4) 0.8403(2) 0.0273(15) Uani 1 1 d . . . . .
C49 C 0.4707(3) 1.0917(3) 0.8102(2) 0.0293(16) Uani 1 1 d . . . . .
C50 C 0.4779(3) 1.0292(4) 0.7876(3) 0.0366(18) Uani 1 1 d . . . . .
H50A H 0.4465 1.0021 0.7915 0.055 Uiso 1 1 calc GR . . . .
H50B H 0.5091 1.0067 0.7983 0.055 Uiso 1 1 calc GR . . . .
H50C H 0.4827 1.0379 0.7582 0.055 Uiso 1 1 calc GR . . . .
C51 C 0.6587(4) 1.0870(6) 0.8619(3) 0.060(3) Uani 1 1 d . . . . .
H51A H 0.6817 1.1249 0.8645 0.090 Uiso 1 1 calc GR . . . .
H51B H 0.6644 1.0667 0.8351 0.090 Uiso 1 1 calc GR . . . .
H51C H 0.6671 1.0561 0.8838 0.090 Uiso 1 1 calc GR . . . .
C52 C 0.5204(3) 1.2081(4) 0.9399(3) 0.0360(18) Uani 1 1 d . . . . .
H52A H 0.5514 1.2140 0.9580 0.043 Uiso 1 1 calc R . . . .
H52B H 0.5095 1.2511 0.9299 0.043 Uiso 1 1 calc R . . . .
C53 C 0.4952(3) 1.1206(4) 0.9862(3) 0.0390(19) Uani 1 1 d . . . . .
H53A H 0.5175 1.1332 1.0099 0.047 Uiso 1 1 calc R . . . .
H53B H 0.5169 1.0938 0.9675 0.047 Uiso 1 1 calc R . . . .
C54 C 0.4474(3) 1.0819(4) 1.0012(3) 0.0343(17) Uani 1 1 d . . . . .
H54A H 0.4584 1.0374 1.0081 0.041 Uiso 1 1 calc R . . . .
H54B H 0.4327 1.1021 1.0263 0.041 Uiso 1 1 calc R . . . .
C55 C 0.4538(3) 1.2278(4) 0.9930(3) 0.0403(19) Uani 1 1 d . . . . .
H55A H 0.4831 1.2505 1.0071 0.048 Uiso 1 1 calc R . . . .
H55B H 0.4328 1.2050 1.0142 0.048 Uiso 1 1 calc R . . . .
C56 C 0.4166(3) 1.2804(5) 0.9707(3) 0.043(2) Uani 1 1 d D . . . .
H56A H 0.3997 1.3093 0.9911 0.052 Uiso 1 1 calc R . . . .
H56B H 0.4372 1.3068 0.9510 0.052 Uiso 1 1 calc R . . . .


_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 O1 1.923(5) . ?
Cu1 O15 1.921(5) . ?
Cu1 N1 1.997(6) . ?
Cu1 N9 1.988(7) . ?
Cu2 O1 1.984(6) . ?
Cu2 O3 1.899(6) . ?
Cu2 O4 2.380(5) . ?
Cu2 O6 1.880(6) . ?
Cu2 N2 2.001(7) . ?
Cu3 O3 1.904(5) . ?
Cu3 O5 1.923(5) . ?
Cu3 N3 1.991(7) . ?
Cu3 N12 2.034(11) . ?
Cu3 N12A 2.104(16) . ?
Cu3 N12B 2.025(16) . ?
Cu4 O5 1.985(6) . ?
Cu4 O7 1.896(5) . ?
Cu4 O8 2.323(7) . ?
Cu4 O10 1.881(5) . ?
Cu4 N4 2.015(6) . ?
Cu5 O7 1.906(5) . ?
Cu5 O9 1.912(5) . ?
Cu5 N5 2.000(6) . ?
Cu5 N15 1.998(7) . ?
Cu6 O9 1.992(6) . ?
Cu6 O11 1.894(5) . ?
Cu6 O12 2.364(5) . ?
Cu6 O14 1.887(5) . ?
Cu6 N6 2.011(6) . ?
Cu7 O11 1.906(5) . ?
Cu7 O13 1.925(5) . ?
Cu7 N7 1.998(6) . ?
Cu7 N18 1.958(8) . ?
Cu8 O2 1.891(5) . ?
Cu8 O13 1.974(5) . ?
Cu8 O15 1.900(5) . ?
Cu8 O16 2.372(6) . ?
Cu8 N8 2.019(6) . ?
O1 C1 1.335(9) . ?
O2 N1 1.351(8) . ?
O3 C12 1.423(10) . ?
O4 H4 0.855(10) . ?
O4 C14 1.434(10) . ?
O5 C15 1.340(9) . ?
O6 N3 1.362(8) . ?
O7 C26 1.437(8) . ?
O8 H8 0.856(10) . ?
O8 C28 1.450(12) . ?
O9 C43 1.358(8) . ?
O10 N5 1.341(8) . ?
O11 C54 1.423(9) . ?
O12 H12 0.856(10) . ?
O12 C56 1.429(9) . ?
O13 C29 1.345(9) . ?
O14 N7 1.359(8) . ?
O15 C42 1.420(8) . ?
O16 H16 0.852(10) . ?
O16 C40 1.464(11) . ?
N1 C7 1.306(9) . ?
N2 C10 1.494(10) . ?
N2 C11 1.502(10) . ?
N2 C13 1.501(10) . ?
N3 C21 1.306(10) . ?
N4 C24 1.483(10) . ?
N4 C25 1.491(10) . ?
N4 C27 1.493(10) . ?
N5 C49 1.303(9) . ?
N6 C52 1.486(10) . ?
N6 C53 1.497(10) . ?
N6 C55 1.488(10) . ?
N7 C35 1.293(9) . ?
N8 C38 1.506(10) . ?
N8 C39 1.489(10) . ?
N8 C41 1.490(10) . ?
N9 N10 1.221(10) . ?
N10 N11 1.163(10) . ?
N12 N13 1.201(15) . ?
N12A N13A 1.230(18) . ?
N12B N13B 1.204(19) . ?
N13 N14 1.180(17) . ?
N13A N14A 1.163(18) . ?
N13B N14B 1.164(19) . ?
N15 N16 1.188(9) . ?
N16 N17 1.149(9) . ?
N18 N19 1.137(12) . ?
N19 N20 1.200(13) . ?
C1 C2 1.392(11) . ?
C1 C6 1.421(11) . ?
C2 C3 1.387(11) . ?
C2 C10 1.511(11) . ?
C3 H3 0.9500 . ?
C3 C4 1.410(12) . ?
C4 C5 1.384(12) . ?
C4 C9 1.522(12) . ?
C5 H5 0.9500 . ?
C5 C6 1.424(10) . ?
C6 C7 1.476(11) . ?
C7 C8 1.507(10) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.522(12) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.498(12) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.417(10) . ?
C15 C20 1.404(11) . ?
C16 C17 1.402(11) . ?
C16 C24 1.496(11) . ?
C17 H17 0.9500 . ?
C17 C18 1.389(11) . ?
C18 C19 1.383(11) . ?
C18 C23 1.478(11) . ?
C19 H19 0.9500 . ?
C19 C20 1.401(11) . ?
C20 C21 1.497(11) . ?
C21 C22 1.504(11) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.531(11) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.493(14) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.404(10) . ?
C29 C34 1.394(11) . ?
C30 C31 1.379(11) . ?
C30 C38 1.511(11) . ?
C31 H31 0.9500 . ?
C31 C32 1.402(12) . ?
C32 C33 1.372(12) . ?
C32 C37 1.509(11) . ?
C33 H33 0.9500 . ?
C33 C34 1.430(11) . ?
C34 C35 1.460(10) . ?
C35 C36 1.523(11) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.524(12) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.531(11) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.420(11) . ?
C43 C48 1.377(11) . ?
C44 C45 1.384(11) . ?
C44 C52 1.494(11) . ?
C45 H45 0.9500 . ?
C45 C46 1.392(13) . ?
C46 C47 1.383(12) . ?
C46 C51 1.510(11) . ?
C47 H47 0.9500 . ?
C47 C48 1.412(10) . ?
C48 C49 1.489(11) . ?
C49 C50 1.501(11) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.531(11) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C56 1.613(13) . ?
C56 H56A 0.9900 . ?
C56 H56B 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
O1 Cu1 N1 90.1(2) . . ?
O1 Cu1 N9 87.2(3) . . ?
O15 Cu1 O1 176.6(2) . . ?
O15 Cu1 N1 88.6(2) . . ?
O15 Cu1 N9 94.1(3) . . ?
N9 Cu1 N1 177.3(3) . . ?
O1 Cu2 O4 95.8(2) . . ?
O1 Cu2 N2 92.5(3) . . ?
O3 Cu2 O1 155.7(2) . . ?
O3 Cu2 O4 108.1(2) . . ?
O3 Cu2 N2 87.1(3) . . ?
O6 Cu2 O1 88.0(2) . . ?
O6 Cu2 O3 93.0(2) . . ?
O6 Cu2 O4 97.6(2) . . ?
O6 Cu2 N2 178.5(3) . . ?
N2 Cu2 O4 81.0(2) . . ?
O3 Cu3 O5 171.4(3) . . ?
O3 Cu3 N3 88.2(2) . . ?
O3 Cu3 N12 94.2(4) . . ?
O3 Cu3 N12A 95.2(11) . . ?
O3 Cu3 N12B 92.2(9) . . ?
O5 Cu3 N3 89.9(2) . . ?
O5 Cu3 N12 87.0(4) . . ?
O5 Cu3 N12A 93.3(11) . . ?
O5 Cu3 N12B 92.6(9) . . ?
N3 Cu3 N12 174.9(5) . . ?
N3 Cu3 N12A 100.9(10) . . ?
N3 Cu3 N12B 158.3(12) . . ?
O5 Cu4 O8 99.8(3) . . ?
O5 Cu4 N4 92.2(2) . . ?
O7 Cu4 O5 155.0(2) . . ?
O7 Cu4 O8 104.6(3) . . ?
O7 Cu4 N4 86.5(2) . . ?
O10 Cu4 O5 88.5(2) . . ?
O10 Cu4 O7 92.8(2) . . ?
O10 Cu4 O8 98.9(3) . . ?
O10 Cu4 N4 179.3(3) . . ?
N4 Cu4 O8 81.1(3) . . ?
O7 Cu5 O9 176.1(2) . . ?
O7 Cu5 N5 89.0(2) . . ?
O7 Cu5 N15 94.9(3) . . ?
O9 Cu5 N5 89.8(2) . . ?
O9 Cu5 N15 86.6(3) . . ?
N15 Cu5 N5 173.8(3) . . ?
O9 Cu6 O12 94.9(2) . . ?
O9 Cu6 N6 92.1(2) . . ?
O11 Cu6 O9 154.3(2) . . ?
O11 Cu6 O12 110.2(2) . . ?
O11 Cu6 N6 87.0(2) . . ?
O14 Cu6 O9 88.1(2) . . ?
O14 Cu6 O11 93.4(2) . . ?
O14 Cu6 O12 98.1(2) . . ?
O14 Cu6 N6 178.8(3) . . ?
N6 Cu6 O12 80.7(2) . . ?
O11 Cu7 O13 176.7(2) . . ?
O11 Cu7 N7 88.8(2) . . ?
O11 Cu7 N18 94.2(3) . . ?
O13 Cu7 N7 89.6(2) . . ?
O13 Cu7 N18 87.6(3) . . ?
N18 Cu7 N7 175.6(4) . . ?
O2 Cu8 O13 88.7(2) . . ?
O2 Cu8 O15 92.9(2) . . ?
O2 Cu8 O16 97.8(2) . . ?
O2 Cu8 N8 178.5(3) . . ?
O13 Cu8 O16 98.0(2) . . ?
O13 Cu8 N8 92.3(2) . . ?
O15 Cu8 O13 154.2(2) . . ?
O15 Cu8 O16 107.3(3) . . ?
O15 Cu8 N8 86.7(2) . . ?
N8 Cu8 O16 81.0(2) . . ?
Cu1 O1 Cu2 114.2(2) . . ?
C1 O1 Cu1 126.2(5) . . ?
C1 O1 Cu2 109.0(5) . . ?
N1 O2 Cu8 118.3(4) . . ?
Cu2 O3 Cu3 118.4(3) . . ?
C12 O3 Cu2 114.1(5) . . ?
C12 O3 Cu3 127.5(5) . . ?
Cu2 O4 H4 144(3) . . ?
C14 O4 Cu2 103.7(4) . . ?
C14 O4 H4 108.3(19) . . ?
Cu3 O5 Cu4 117.2(3) . . ?
C15 O5 Cu3 123.6(5) . . ?
C15 O5 Cu4 109.7(5) . . ?
N3 O6 Cu2 116.8(5) . . ?
Cu4 O7 Cu5 117.8(2) . . ?
C26 O7 Cu4 114.5(5) . . ?
C26 O7 Cu5 126.9(5) . . ?
Cu4 O8 H8 144(3) . . ?
C28 O8 Cu4 104.7(5) . . ?
C28 O8 H8 108(2) . . ?
Cu5 O9 Cu6 113.5(2) . . ?
C43 O9 Cu5 126.5(5) . . ?
C43 O9 Cu6 108.1(4) . . ?
N5 O10 Cu4 118.8(4) . . ?
Cu6 O11 Cu7 117.5(3) . . ?
C54 O11 Cu6 113.6(4) . . ?
C54 O11 Cu7 128.1(5) . . ?
Cu6 O12 H12 140(2) . . ?
C56 O12 Cu6 108.8(5) . . ?
C56 O12 H12 107.8(19) . . ?
Cu7 O13 Cu8 115.1(3) . . ?
C29 O13 Cu7 124.3(5) . . ?
C29 O13 Cu8 112.6(4) . . ?
N7 O14 Cu6 117.4(4) . . ?
Cu8 O15 Cu1 117.6(2) . . ?
C42 O15 Cu1 128.2(5) . . ?
C42 O15 Cu8 113.0(5) . . ?
Cu8 O16 H16 143(3) . . ?
C40 O16 Cu8 104.6(5) . . ?
C40 O16 H16 109(2) . . ?
O2 N1 Cu1 118.4(4) . . ?
C7 N1 Cu1 126.8(5) . . ?
C7 N1 O2 114.5(6) . . ?
C10 N2 Cu2 114.3(5) . . ?
C10 N2 C11 110.2(6) . . ?
C10 N2 C13 109.7(6) . . ?
C11 N2 Cu2 101.8(5) . . ?
C13 N2 Cu2 109.1(5) . . ?
C13 N2 C11 111.5(7) . . ?
O6 N3 Cu3 119.2(5) . . ?
C21 N3 Cu3 127.5(5) . . ?
C21 N3 O6 112.9(7) . . ?
C24 N4 Cu4 113.0(5) . . ?
C24 N4 C25 111.6(6) . . ?
C24 N4 C27 109.8(6) . . ?
C25 N4 Cu4 101.6(4) . . ?
C25 N4 C27 111.3(6) . . ?
C27 N4 Cu4 109.3(5) . . ?
O10 N5 Cu5 118.0(4) . . ?
C49 N5 Cu5 127.1(5) . . ?
C49 N5 O10 114.3(6) . . ?
C52 N6 Cu6 113.2(5) . . ?
C52 N6 C53 110.0(6) . . ?
C52 N6 C55 110.8(6) . . ?
C53 N6 Cu6 102.2(5) . . ?
C55 N6 Cu6 108.7(5) . . ?
C55 N6 C53 111.6(7) . . ?
O14 N7 Cu7 117.9(4) . . ?
C35 N7 Cu7 126.0(5) . . ?
C35 N7 O14 115.8(6) . . ?
C38 N8 Cu8 113.4(5) . . ?
C39 N8 Cu8 108.7(5) . . ?
C39 N8 C38 109.4(6) . . ?
C39 N8 C41 112.3(6) . . ?
C41 N8 Cu8 101.7(5) . . ?
C41 N8 C38 111.2(6) . . ?
N10 N9 Cu1 115.7(6) . . ?
N11 N10 N9 178.8(11) . . ?
N13 N12 Cu3 126.6(15) . . ?
N13A N12A Cu3 141(3) . . ?
N13B N12B Cu3 115(2) . . ?
N14 N13 N12 150(3) . . ?
N14A N13A N12A 154(4) . . ?
N14B N13B N12B 171(4) . . ?
N16 N15 Cu5 120.6(6) . . ?
N17 N16 N15 178.6(10) . . ?
N19 N18 Cu7 112.6(8) . . ?
N18 N19 N20 176.3(14) . . ?
O1 C1 C2 118.4(7) . . ?
O1 C1 C6 122.3(7) . . ?
C2 C1 C6 119.4(7) . . ?
C1 C2 C10 120.2(7) . . ?
C3 C2 C1 121.1(8) . . ?
C3 C2 C10 118.8(7) . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.3(8) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C9 120.2(8) . . ?
C5 C4 C3 117.4(8) . . ?
C5 C4 C9 122.4(9) . . ?
C4 C5 H5 118.6 . . ?
C4 C5 C6 122.8(8) . . ?
C6 C5 H5 118.6 . . ?
C1 C6 C5 117.8(7) . . ?
C1 C6 C7 123.3(7) . . ?
C5 C6 C7 118.7(7) . . ?
N1 C7 C6 121.7(7) . . ?
N1 C7 C8 117.5(7) . . ?
C6 C7 C8 120.7(6) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C2 112.7(6) . . ?
N2 C10 H10A 109.1 . . ?
N2 C10 H10B 109.1 . . ?
C2 C10 H10A 109.1 . . ?
C2 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N2 C11 H11A 109.6 . . ?
N2 C11 H11B 109.6 . . ?
N2 C11 C12 110.3(7) . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 H11A 109.6 . . ?
C12 C11 H11B 109.6 . . ?
O3 C12 C11 107.8(7) . . ?
O3 C12 H12A 110.1 . . ?
O3 C12 H12B 110.1 . . ?
C11 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.5 . . ?
N2 C13 H13A 109.1 . . ?
N2 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C14 C13 N2 112.7(7) . . ?
C14 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
O4 C14 C13 108.6(7) . . ?
O4 C14 H14A 110.0 . . ?
O4 C14 H14B 110.0 . . ?
C13 C14 H14A 110.0 . . ?
C13 C14 H14B 110.0 . . ?
H14A C14 H14B 108.3 . . ?
O5 C15 C16 117.3(7) . . ?
O5 C15 C20 123.8(7) . . ?
C20 C15 C16 118.9(7) . . ?
C15 C16 C24 118.5(7) . . ?
C17 C16 C15 119.5(7) . . ?
C17 C16 C24 122.1(7) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 C16 121.7(7) . . ?
C18 C17 H17 119.1 . . ?
C17 C18 C23 121.0(7) . . ?
C19 C18 C17 117.7(7) . . ?
C19 C18 C23 121.3(8) . . ?
C18 C19 H19 118.7 . . ?
C18 C19 C20 122.6(8) . . ?
C20 C19 H19 118.7 . . ?
C15 C20 C21 122.2(7) . . ?
C19 C20 C15 119.2(7) . . ?
C19 C20 C21 118.5(7) . . ?
N3 C21 C20 119.9(7) . . ?
N3 C21 C22 119.6(7) . . ?
C20 C21 C22 120.4(7) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 C16 114.1(6) . . ?
N4 C24 H24A 108.7 . . ?
N4 C24 H24B 108.7 . . ?
C16 C24 H24A 108.7 . . ?
C16 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
N4 C25 H25A 109.6 . . ?
N4 C25 H25B 109.6 . . ?
N4 C25 C26 110.4(6) . . ?
H25A C25 H25B 108.1 . . ?
C26 C25 H25A 109.6 . . ?
C26 C25 H25B 109.6 . . ?
O7 C26 C25 107.6(6) . . ?
O7 C26 H26A 110.2 . . ?
O7 C26 H26B 110.2 . . ?
C25 C26 H26A 110.2 . . ?
C25 C26 H26B 110.2 . . ?
H26A C26 H26B 108.5 . . ?
N4 C27 H27A 109.2 . . ?
N4 C27 H27B 109.2 . . ?
N4 C27 C28 111.8(7) . . ?
H27A C27 H27B 107.9 . . ?
C28 C27 H27A 109.2 . . ?
C28 C27 H27B 109.2 . . ?
O8 C28 C27 108.4(8) . . ?
O8 C28 H28A 110.0 . . ?
O8 C28 H28B 110.0 . . ?
C27 C28 H28A 110.0 . . ?
C27 C28 H28B 110.0 . . ?
H28A C28 H28B 108.4 . . ?
O13 C29 C30 117.8(7) . . ?
O13 C29 C34 122.7(6) . . ?
C34 C29 C30 119.5(7) . . ?
C29 C30 C38 118.8(7) . . ?
C31 C30 C29 121.2(8) . . ?
C31 C30 C38 120.0(7) . . ?
C30 C31 H31 120.0 . . ?
C30 C31 C32 120.1(7) . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C37 120.5(8) . . ?
C33 C32 C31 118.9(7) . . ?
C33 C32 C37 120.6(8) . . ?
C32 C33 H33 119.0 . . ?
C32 C33 C34 121.9(8) . . ?
C34 C33 H33 119.0 . . ?
C29 C34 C33 117.9(7) . . ?
C29 C34 C35 122.8(7) . . ?
C33 C34 C35 119.3(7) . . ?
N7 C35 C34 122.6(7) . . ?
N7 C35 C36 117.4(7) . . ?
C34 C35 C36 119.9(7) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N8 C38 C30 114.4(6) . . ?
N8 C38 H38A 108.7 . . ?
N8 C38 H38B 108.7 . . ?
C30 C38 H38A 108.7 . . ?
C30 C38 H38B 108.7 . . ?
H38A C38 H38B 107.6 . . ?
N8 C39 H39A 109.1 . . ?
N8 C39 H39B 109.1 . . ?
N8 C39 C40 112.6(7) . . ?
H39A C39 H39B 107.8 . . ?
C40 C39 H39A 109.1 . . ?
C40 C39 H39B 109.1 . . ?
O16 C40 C39 107.2(7) . . ?
O16 C40 H40A 110.3 . . ?
O16 C40 H40B 110.3 . . ?
C39 C40 H40A 110.3 . . ?
C39 C40 H40B 110.3 . . ?
H40A C40 H40B 108.5 . . ?
N8 C41 H41A 109.9 . . ?
N8 C41 H41B 109.9 . . ?
N8 C41 C42 108.8(6) . . ?
H41A C41 H41B 108.3 . . ?
C42 C41 H41A 109.9 . . ?
C42 C41 H41B 109.9 . . ?
O15 C42 C41 110.2(6) . . ?
O15 C42 H42A 109.6 . . ?
O15 C42 H42B 109.6 . . ?
C41 C42 H42A 109.6 . . ?
C41 C42 H42B 109.6 . . ?
H42A C42 H42B 108.1 . . ?
O9 C43 C44 116.5(7) . . ?
O9 C43 C48 122.9(7) . . ?
C48 C43 C44 120.6(7) . . ?
C43 C44 C52 118.9(7) . . ?
C45 C44 C43 119.4(8) . . ?
C45 C44 C52 121.8(7) . . ?
C44 C45 H45 119.5 . . ?
C44 C45 C46 121.1(8) . . ?
C46 C45 H45 119.5 . . ?
C45 C46 C51 118.0(8) . . ?
C47 C46 C45 118.4(7) . . ?
C47 C46 C51 123.6(9) . . ?
C46 C47 H47 118.9 . . ?
C46 C47 C48 122.3(8) . . ?
C48 C47 H47 118.9 . . ?
C43 C48 C47 118.1(7) . . ?
C43 C48 C49 122.8(6) . . ?
C47 C48 C49 118.8(7) . . ?
N5 C49 C48 121.5(7) . . ?
N5 C49 C50 117.2(7) . . ?
C48 C49 C50 121.3(6) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C46 C51 H51A 109.5 . . ?
C46 C51 H51B 109.5 . . ?
C46 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N6 C52 C44 113.2(6) . . ?
N6 C52 H52A 108.9 . . ?
N6 C52 H52B 108.9 . . ?
C44 C52 H52A 108.9 . . ?
C44 C52 H52B 108.9 . . ?
H52A C52 H52B 107.8 . . ?
N6 C53 H53A 109.8 . . ?
N6 C53 H53B 109.8 . . ?
N6 C53 C54 109.2(7) . . ?
H53A C53 H53B 108.3 . . ?
C54 C53 H53A 109.8 . . ?
C54 C53 H53B 109.8 . . ?
O11 C54 C53 109.4(6) . . ?
O11 C54 H54A 109.8 . . ?
O11 C54 H54B 109.8 . . ?
C53 C54 H54A 109.8 . . ?
C53 C54 H54B 109.8 . . ?
H54A C54 H54B 108.2 . . ?
N6 C55 H55A 108.9 . . ?
N6 C55 H55B 108.9 . . ?
N6 C55 C56 113.2(7) . . ?
H55A C55 H55B 107.7 . . ?
C56 C55 H55A 108.9 . . ?
C56 C55 H55B 108.9 . . ?
O12 C56 C55 103.7(7) . . ?
O12 C56 H56A 111.0 . . ?
O12 C56 H56B 111.0 . . ?
C55 C56 H56A 111.0 . . ?
C55 C56 H56B 111.0 . . ?
H56A C56 H56B 109.0 . . ?

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
Cu1 O1 C1 C2 157.5(5) . . . . ?
Cu1 O1 C1 C6 -24.0(10) . . . . ?
Cu1 O15 C42 C41 -151.3(5) . . . . ?
Cu1 N1 C7 C6 -3.6(11) . . . . ?
Cu1 N1 C7 C8 173.0(5) . . . . ?
Cu2 O1 C1 C2 -60.5(8) . . . . ?
Cu2 O1 C1 C6 118.0(7) . . . . ?
Cu2 O3 C12 C11 -20.1(8) . . . . ?
Cu2 O4 C14 C13 -36.5(8) . . . . ?
Cu2 O6 N3 Cu3 -25.1(7) . . . . ?
Cu2 O6 N3 C21 161.9(5) . . . . ?
Cu2 N2 C10 C2 -39.1(8) . . . . ?
Cu2 N2 C11 C12 -44.6(7) . . . . ?
Cu2 N2 C13 C14 -46.3(9) . . . . ?
Cu3 O3 C12 C11 158.5(5) . . . . ?
Cu3 O5 C15 C16 -151.6(6) . . . . ?
Cu3 O5 C15 C20 27.3(10) . . . . ?
Cu3 N3 C21 C20 5.9(11) . . . . ?
Cu3 N3 C21 C22 -172.0(6) . . . . ?
Cu3 N12 N13 N14 60(5) . . . . ?
Cu3 N12A N13A N14A 114(10) . . . . ?
Cu4 O5 C15 C16 63.2(8) . . . . ?
Cu4 O5 C15 C20 -117.9(7) . . . . ?
Cu4 O7 C26 C25 16.2(8) . . . . ?
Cu4 O8 C28 C27 37.0(10) . . . . ?
Cu4 O10 N5 Cu5 22.2(7) . . . . ?
Cu4 O10 N5 C49 -166.3(5) . . . . ?
Cu4 N4 C24 C16 44.9(8) . . . . ?
Cu4 N4 C25 C26 46.0(6) . . . . ?
Cu4 N4 C27 C28 45.4(8) . . . . ?
Cu5 O7 C26 C25 -153.7(5) . . . . ?
Cu5 O9 C43 C44 156.5(5) . . . . ?
Cu5 O9 C43 C48 -24.1(10) . . . . ?
Cu5 N5 C49 C48 -10.1(10) . . . . ?
Cu5 N5 C49 C50 167.5(5) . . . . ?
Cu6 O9 C43 C44 -63.8(7) . . . . ?
Cu6 O9 C43 C48 115.6(7) . . . . ?
Cu6 O11 C54 C53 -17.6(8) . . . . ?
Cu6 O12 C56 C55 -32.5(7) . . . . ?
Cu6 O14 N7 Cu7 -24.9(6) . . . . ?
Cu6 O14 N7 C35 161.4(5) . . . . ?
Cu6 N6 C52 C44 -44.2(8) . . . . ?
Cu6 N6 C53 C54 -44.2(7) . . . . ?
Cu6 N6 C55 C56 -49.3(8) . . . . ?
Cu7 O11 C54 C53 152.6(5) . . . . ?
Cu7 O13 C29 C30 -151.6(6) . . . . ?
Cu7 O13 C29 C34 28.3(10) . . . . ?
Cu7 N7 C35 C34 6.4(10) . . . . ?
Cu7 N7 C35 C36 -170.0(5) . . . . ?
Cu8 O2 N1 Cu1 22.9(7) . . . . ?
Cu8 O2 N1 C7 -162.5(5) . . . . ?
Cu8 O13 C29 C30 61.2(8) . . . . ?
Cu8 O13 C29 C34 -118.9(7) . . . . ?
Cu8 O15 C42 C41 15.4(8) . . . . ?
Cu8 O16 C40 C39 34.9(8) . . . . ?
Cu8 N8 C38 C30 44.5(8) . . . . ?
Cu8 N8 C39 C40 49.1(8) . . . . ?
Cu8 N8 C41 C42 45.6(6) . . . . ?
O1 Cu2 O3 Cu3 -93.3(6) . . . . ?
O1 Cu2 O3 C12 85.5(8) . . . . ?
O1 Cu2 O6 N3 171.4(5) . . . . ?
O1 C1 C2 C3 -179.3(7) . . . . ?
O1 C1 C2 C10 -1.0(11) . . . . ?
O1 C1 C6 C5 176.8(7) . . . . ?
O1 C1 C6 C7 -8.0(12) . . . . ?
O2 N1 C7 C6 -177.7(6) . . . . ?
O2 N1 C7 C8 -1.1(10) . . . . ?
O3 Cu2 O6 N3 15.6(5) . . . . ?
O4 Cu2 O3 Cu3 97.6(3) . . . . ?
O4 Cu2 O3 C12 -83.7(6) . . . . ?
O4 Cu2 O6 N3 -93.1(5) . . . . ?
O5 Cu4 O7 Cu5 91.0(6) . . . . ?
O5 Cu4 O7 C26 -79.8(7) . . . . ?
O5 Cu4 O10 N5 -167.7(5) . . . . ?
O5 C15 C16 C17 177.6(7) . . . . ?
O5 C15 C16 C24 -3.0(11) . . . . ?
O5 C15 C20 C19 -174.3(7) . . . . ?
O5 C15 C20 C21 9.7(12) . . . . ?
O6 Cu2 O3 Cu3 -1.5(4) . . . . ?
O6 Cu2 O3 C12 177.3(6) . . . . ?
O6 N3 C21 C20 178.1(6) . . . . ?
O6 N3 C21 C22 0.2(10) . . . . ?
O7 Cu4 O10 N5 -12.7(5) . . . . ?
O8 Cu4 O7 Cu5 -101.3(3) . . . . ?
O8 Cu4 O7 C26 87.8(5) . . . . ?
O8 Cu4 O10 N5 92.6(6) . . . . ?
O9 Cu6 O11 Cu7 -89.2(5) . . . . ?
O9 Cu6 O11 C54 82.1(7) . . . . ?
O9 Cu6 O14 N7 167.3(5) . . . . ?
O9 C43 C44 C45 -177.1(7) . . . . ?
O9 C43 C44 C52 1.9(10) . . . . ?
O9 C43 C48 C47 177.5(7) . . . . ?
O9 C43 C48 C49 -7.9(11) . . . . ?
O10 Cu4 O7 Cu5 -1.4(3) . . . . ?
O10 Cu4 O7 C26 -172.2(5) . . . . ?
O10 N5 C49 C48 179.4(6) . . . . ?
O10 N5 C49 C50 -3.1(10) . . . . ?
O11 Cu6 O14 N7 13.0(5) . . . . ?
O12 Cu6 O11 Cu7 103.2(3) . . . . ?
O12 Cu6 O11 C54 -85.5(5) . . . . ?
O12 Cu6 O14 N7 -98.0(5) . . . . ?
O13 Cu8 O2 N1 -165.6(5) . . . . ?
O13 C29 C30 C31 177.0(7) . . . . ?
O13 C29 C30 C38 -2.0(11) . . . . ?
O13 C29 C34 C33 -174.0(7) . . . . ?
O13 C29 C34 C35 6.9(11) . . . . ?
O14 Cu6 O11 Cu7 3.3(3) . . . . ?
O14 Cu6 O11 C54 174.6(5) . . . . ?
O14 N7 C35 C34 179.5(6) . . . . ?
O14 N7 C35 C36 3.1(10) . . . . ?
O15 Cu8 O2 N1 -11.3(5) . . . . ?
O16 Cu8 O2 N1 96.6(5) . . . . ?
N2 Cu2 O3 Cu3 177.1(4) . . . . ?
N2 Cu2 O3 C12 -4.2(6) . . . . ?
N2 C11 C12 O3 44.1(9) . . . . ?
N2 C13 C14 O4 57.8(10) . . . . ?
N4 Cu4 O7 Cu5 178.8(3) . . . . ?
N4 Cu4 O7 C26 7.9(5) . . . . ?
N4 C25 C26 O7 -42.6(8) . . . . ?
N4 C27 C28 O8 -56.9(11) . . . . ?
N6 Cu6 O11 Cu7 -177.8(3) . . . . ?
N6 Cu6 O11 C54 -6.5(5) . . . . ?
N6 C53 C54 O11 42.3(9) . . . . ?
N6 C55 C56 O12 55.6(9) . . . . ?
N8 C39 C40 O16 -57.9(10) . . . . ?
N8 C41 C42 O15 -42.2(8) . . . . ?
C1 C2 C3 C4 3.0(13) . . . . ?
C1 C2 C10 N2 58.1(10) . . . . ?
C1 C6 C7 N1 22.1(11) . . . . ?
C1 C6 C7 C8 -154.4(7) . . . . ?
C2 C1 C6 C5 -4.8(11) . . . . ?
C2 C1 C6 C7 170.4(7) . . . . ?
C2 C3 C4 C5 -5.1(13) . . . . ?
C2 C3 C4 C9 175.9(9) . . . . ?
C3 C2 C10 N2 -123.5(8) . . . . ?
C3 C4 C5 C6 2.3(13) . . . . ?
C4 C5 C6 C1 2.6(12) . . . . ?
C4 C5 C6 C7 -172.9(8) . . . . ?
C5 C6 C7 N1 -162.8(7) . . . . ?
C5 C6 C7 C8 20.8(11) . . . . ?
C6 C1 C2 C3 2.1(12) . . . . ?
C6 C1 C2 C10 -179.5(7) . . . . ?
C9 C4 C5 C6 -178.7(9) . . . . ?
C10 N2 C11 C12 -166.3(7) . . . . ?
C10 N2 C13 C14 79.6(9) . . . . ?
C10 C2 C3 C4 -175.4(8) . . . . ?
C11 N2 C10 C2 74.8(8) . . . . ?
C11 N2 C13 C14 -158.0(7) . . . . ?
C13 N2 C10 C2 -162.0(7) . . . . ?
C13 N2 C11 C12 71.6(8) . . . . ?
C15 C16 C17 C18 -4.6(12) . . . . ?
C15 C16 C24 N4 -58.8(10) . . . . ?
C15 C20 C21 N3 -26.9(12) . . . . ?
C15 C20 C21 C22 151.0(8) . . . . ?
C16 C15 C20 C19 4.6(11) . . . . ?
C16 C15 C20 C21 -171.3(7) . . . . ?
C16 C17 C18 C19 7.1(12) . . . . ?
C16 C17 C18 C23 -174.6(8) . . . . ?
C17 C16 C24 N4 120.7(8) . . . . ?
C17 C18 C19 C20 -3.8(13) . . . . ?
C18 C19 C20 C15 -2.1(12) . . . . ?
C18 C19 C20 C21 174.0(8) . . . . ?
C19 C20 C21 N3 157.1(7) . . . . ?
C19 C20 C21 C22 -25.0(11) . . . . ?
C20 C15 C16 C17 -1.4(12) . . . . ?
C20 C15 C16 C24 178.1(7) . . . . ?
C23 C18 C19 C20 177.9(8) . . . . ?
C24 N4 C25 C26 166.7(6) . . . . ?
C24 N4 C27 C28 -79.0(9) . . . . ?
C24 C16 C17 C18 175.9(8) . . . . ?
C25 N4 C24 C16 -68.9(8) . . . . ?
C25 N4 C27 C28 156.8(7) . . . . ?
C27 N4 C24 C16 167.2(7) . . . . ?
C27 N4 C25 C26 -70.2(8) . . . . ?
C29 C30 C31 C32 -3.3(12) . . . . ?
C29 C30 C38 N8 -57.1(10) . . . . ?
C29 C34 C35 N7 -25.1(11) . . . . ?
C29 C34 C35 C36 151.3(7) . . . . ?
C30 C29 C34 C33 5.9(11) . . . . ?
C30 C29 C34 C35 -173.2(7) . . . . ?
C30 C31 C32 C33 6.2(12) . . . . ?
C30 C31 C32 C37 -176.4(8) . . . . ?
C31 C30 C38 N8 123.8(8) . . . . ?
C31 C32 C33 C34 -3.0(12) . . . . ?
C32 C33 C34 C29 -3.0(11) . . . . ?
C32 C33 C34 C35 176.1(7) . . . . ?
C33 C34 C35 N7 155.8(7) . . . . ?
C33 C34 C35 C36 -27.8(10) . . . . ?
C34 C29 C30 C31 -2.9(12) . . . . ?
C34 C29 C30 C38 178.1(7) . . . . ?
C37 C32 C33 C34 179.5(8) . . . . ?
C38 N8 C39 C40 -75.2(9) . . . . ?
C38 N8 C41 C42 166.6(6) . . . . ?
C38 C30 C31 C32 175.7(7) . . . . ?
C39 N8 C38 C30 166.0(6) . . . . ?
C39 N8 C41 C42 -70.4(8) . . . . ?
C41 N8 C38 C30 -69.4(8) . . . . ?
C41 N8 C39 C40 160.9(7) . . . . ?
C43 C44 C45 C46 0.3(12) . . . . ?
C43 C44 C52 N6 60.1(10) . . . . ?
C43 C48 C49 N5 25.3(11) . . . . ?
C43 C48 C49 C50 -152.1(8) . . . . ?
C44 C43 C48 C47 -3.1(11) . . . . ?
C44 C43 C48 C49 171.4(7) . . . . ?
C44 C45 C46 C47 -4.2(13) . . . . ?
C44 C45 C46 C51 176.4(8) . . . . ?
C45 C44 C52 N6 -120.9(8) . . . . ?
C45 C46 C47 C48 4.6(13) . . . . ?
C46 C47 C48 C43 -0.9(12) . . . . ?
C46 C47 C48 C49 -175.7(7) . . . . ?
C47 C48 C49 N5 -160.1(7) . . . . ?
C47 C48 C49 C50 22.5(11) . . . . ?
C48 C43 C44 C45 3.5(11) . . . . ?
C48 C43 C44 C52 -177.5(7) . . . . ?
C51 C46 C47 C48 -176.0(9) . . . . ?
C52 N6 C53 C54 -164.8(6) . . . . ?
C52 N6 C55 C56 75.7(8) . . . . ?
C52 C44 C45 C46 -178.7(8) . . . . ?
C53 N6 C52 C44 69.5(8) . . . . ?
C53 N6 C55 C56 -161.3(6) . . . . ?
C55 N6 C52 C44 -166.6(7) . . . . ?
C55 N6 C53 C54 71.8(8) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-16 0 -2 0.0758 -16.0001 0.0000 -2.0005 0.2303 0.8690 -0.3873
16 0 2 0.0536 16.0001 -0.0000 2.0005 -0.2303 -0.8690 0.3873
8 12 -1 0.1714 8.0005 12.0000 -1.0004 -0.0137 -0.0856 1.0125
2 0 21 0.0148 2.0001 0.0000 20.9992 -1.0021 0.0206 0.0010
-2 0 -21 0.0148 -2.0001 -0.0000 -20.9992 1.0021 -0.0206 -0.0010
4 -13 1 0.2112 3.9996 -13.0000 1.0009 -0.0893 -0.6056 -0.7864
11 -6 12 0.0825 10.9999 -6.0000 12.0003 -0.6605 -0.7119 -0.1651
####################################################################### 
# 
# 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_eb4022
_database_code_depnum_ccdc_archive 'CCDC 991827'
_audit_update_record             
;
2015-03-27 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
_audit_creation_date             2014-02-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H76 Cu6 N8 O16'
_chemical_formula_sum            'C56 H76 Cu6 N8 O16'
_chemical_formula_weight         1498.48
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N8 O20 Cu'
_chemical_oxdiff_usercomment     '@ 120 K JF2966.2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.5984(3)
_cell_length_b                   26.6204(7)
_cell_length_c                   18.8428(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.153(2)
_cell_angle_gamma                90
_cell_volume                     7100.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11838
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      74.6490
_cell_measurement_theta_min      3.7910
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.487
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3080
_exptl_crystal_recrystallization_method 
'Diffusion of hexane into a methanol solution'
_exptl_crystal_size_max          0.2685
_exptl_crystal_size_mid          0.0398
_exptl_crystal_size_min          0.0303
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44755
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.802
_diffrn_reflns_theta_min         3.320
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0927246000
_diffrn_orient_matrix_UB_12      0.0239937000
_diffrn_orient_matrix_UB_13      -0.0085632000
_diffrn_orient_matrix_UB_21      -0.0480045000
_diffrn_orient_matrix_UB_22      0.0519058000
_diffrn_orient_matrix_UB_23      -0.0101383000
_diffrn_orient_matrix_UB_31      0.0306523000
_diffrn_orient_matrix_UB_32      0.0088225000
_diffrn_orient_matrix_UB_33      0.0833000000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5830
_reflns_number_total             7393
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7393
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0486
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0763P)²+11.4089P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1410
_refine_special_details          
;
The SQUEEZE routine of PLATON was used to remove electron density 
corresponding to 2.6 molecules of hexane per asymmetric unit.  This was 
observed as ridge of several residual peaks in a difference Fourier map 
connected into a long chain.  However, an adequate model which converged 
satisfactorily could not be constructed, so the density was masked using 
SQUEEZE.  The chemical formula includes this missing hexane and so several 
checkCIF alerts are triggered, all of which can be ignored. 

When the structure was solved it was quite clear that the fragment defined by 
C27, C28 and O8 needed to be modelled as disordered.  The chain has been 
modelled over two sites, as evidenced by difference Fourier maps. However, 
displacment ellipsoids are still very large and suggestive of a further one 
or two extra sites.  This has not been modelled since refinement has 
converged reasonably well.  The very large displacement ellipsoids are 
controlled by means of rigid bond and isotropic similarity restraints, along 
with bond distance restraints.  H-atoms were placed in calculated positions.  
The H atom bonded to O4 was observed in a difference Fourier map and, although 
free refinement is stable, it was felt prefereable to refine using the AFIX 
147 restraint in SHELXL.  This is adjacent to the O8/O8' disordered site.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
420_ALERT_2_B D-H Without Acceptor       O4     -   H4     ...     Please Check
420_ALERT_2_B D-H Without Acceptor      >O8     -  >H8     ...     Please Check

See description above.

#===============================================================================
220_ALERT_2_C Large Non-Solvent  C     Ueq(max)/Ueq(min) Range        3.2 Ratio
220_ALERT_2_C Large Non-Solvent  O     Ueq(max)/Ueq(min) Range        4.3 Ratio
220_ALERT_2_C Large Non-Solvent  C     Ueq(max)/Ueq(min) Range        3.2 Ratio
220_ALERT_2_C Large Non-Solvent  O     Ueq(max)/Ueq(min) Range        4.3 Ratio
222_ALERT_3_C Large Non-Solvent    H    Uiso(max)/Uiso(min) ..        4.1 Ratio
222_ALERT_3_C Large Non-Solvent    H    Uiso(max)/Uiso(min) ..        4.1 Ratio
234_ALERT_4_C Large Hirshfeld Difference O8     --  C28     ..       0.20 Ang.
241_ALERT_2_C High      Ueq as Compared to Neighbors for .....         O7 Check
241_ALERT_2_C High      Ueq as Compared to Neighbors for .....         O7 Check

See description above.

#==============================================================================
;


# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.023 0.250 0.720 916 252 ' '
2 0.068 0.750 0.597 916 252 ' '
_platon_squeeze_details          '2.6 molecules of hexane per asymmetric unit'



_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H8' of O8', H4 of O4, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H8 of O8
2. Restrained distances
 C28'-C27' \\sim C28-C27
 with sigma of 0.02
 O8-C28 \\sim O8'-C28' \\sim O4-C14
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C28') \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.1
Uanis(O8') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C28, O8, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27', C28', O8'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O8')=Sof(H8')=Sof(C27')=Sof(H27C)=Sof(H27D)=Sof(C28')=Sof(H28C)=Sof(H28D)=
 1-FVAR(1)
 Sof(O8)=Sof(H8)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
 C27'(H27C,H27D), C28(H28A,H28B), C28'(H28C,H28D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19)
6.c Tetrahedral OH refined with riding coordinates:
 O8'(H8')
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
6.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O8(H8)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.74940(3) 0.57681(2) 0.32031(3) 0.04394(15) Uani 1 1 d . . . . .
Cu2 Cu 0.54444(3) 0.57034(2) 0.35431(3) 0.03710(13) Uani 1 1 d . . . . .
Cu3 Cu 0.31878(3) 0.55830(2) 0.34498(3) 0.04396(15) Uani 1 1 d . . . . .
O1 O 0.65765(16) 0.61125(10) 0.36996(13) 0.0448(5) Uani 1 1 d . . . . .
O2 O 0.36908(16) 0.61611(10) 0.30968(15) 0.0495(6) Uani 1 1 d . . . . .
O3 O 0.79690(15) 0.57426(11) 0.23124(13) 0.0483(6) Uani 1 1 d . . . . .
O4 O 0.8401(2) 0.52667(15) 0.41443(19) 0.0717(9) Uani 1 1 d . . . . .
H4 H 0.8500 0.4966 0.4049 0.086 Uiso 1 1 calc GR . . . .
O5 O 0.44688(14) 0.52858(9) 0.37819(13) 0.0401(5) Uani 1 1 d . . . . .
O6 O 0.66832(16) 0.52305(9) 0.28422(13) 0.0427(5) Uani 1 1 d . . . . .
O7 O 0.2845(2) 0.60947(15) 0.44051(18) 0.0730(9) Uani 1 1 d . . . . .
O8 O 0.1184(8) 0.4874(6) 0.2482(6) 0.131(5) Uani 0.506(14) 1 d . . P A 1
H8 H 0.0895 0.4692 0.2135 0.197 Uiso 0.506(14) 1 calc GR . P A 1
O8' O 0.0491(8) 0.4784(6) 0.3217(9) 0.174(6) Uani 0.494(14) 1 d . U P A 2
H8' H 0.0533 0.4641 0.3621 0.208 Uiso 0.494(14) 1 calc R . P A 2
N1 N 0.46184(19) 0.62781(12) 0.33606(16) 0.0426(6) Uani 1 1 d . . . . .
N2 N 0.8565(2) 0.62202(14) 0.35846(17) 0.0526(8) Uani 1 1 d . . . . .
N3 N 0.60791(17) 0.51179(11) 0.32739(14) 0.0374(6) Uani 1 1 d . . . . .
N4 N 0.25570(18) 0.50934(13) 0.40085(16) 0.0464(7) Uani 1 1 d . . . . .
C1 C 0.6614(3) 0.66210(15) 0.3763(2) 0.0505(9) Uani 1 1 d . . . . .
C2 C 0.7523(3) 0.68423(19) 0.3984(3) 0.0654(12) Uani 1 1 d . . . . .
C3 C 0.7605(4) 0.7361(2) 0.4044(4) 0.0868(18) Uani 1 1 d . . . . .
H3 H 0.8218 0.7506 0.4182 0.104 Uiso 1 1 calc R . . . .
C4 C 0.6825(4) 0.7673(2) 0.3907(4) 0.0858(17) Uani 1 1 d . . . . .
C5 C 0.5941(4) 0.74519(18) 0.3709(3) 0.0672(12) Uani 1 1 d . . . . .
H5 H 0.5400 0.7663 0.3624 0.081 Uiso 1 1 calc R . . . .
C6 C 0.5805(3) 0.69296(15) 0.3628(2) 0.0521(9) Uani 1 1 d . . . . .
C7 C 0.4819(3) 0.67552(14) 0.3398(2) 0.0477(8) Uani 1 1 d . . . . .
C8 C 0.4026(3) 0.71209(17) 0.3218(3) 0.0672(11) Uani 1 1 d . . . . .
H8A H 0.3424 0.6939 0.3104 0.101 Uiso 1 1 calc GR . . . .
H8B H 0.4077 0.7322 0.2794 0.101 Uiso 1 1 calc GR . . . .
H8C H 0.4054 0.7343 0.3638 0.101 Uiso 1 1 calc GR . . . .
C9 C 0.6923(6) 0.8242(2) 0.3956(5) 0.117(3) Uani 1 1 d . . . . .
H9A H 0.7132 0.8367 0.3533 0.176 Uiso 1 1 calc GR . . . .
H9B H 0.7388 0.8333 0.4407 0.176 Uiso 1 1 calc GR . . . .
H9C H 0.6311 0.8391 0.3960 0.176 Uiso 1 1 calc GR . . . .
C10 C 0.8389(3) 0.6534(2) 0.4187(3) 0.0680(13) Uani 1 1 d . . . . .
H10A H 0.8346 0.6312 0.4599 0.082 Uiso 1 1 calc R . . . .
H10B H 0.8937 0.6760 0.4362 0.082 Uiso 1 1 calc R . . . .
C11 C 0.8634(3) 0.65159(18) 0.2932(2) 0.0598(10) Uani 1 1 d . . . . .
H11A H 0.9240 0.6701 0.3037 0.072 Uiso 1 1 calc R . . . .
H11B H 0.8113 0.6763 0.2812 0.072 Uiso 1 1 calc R . . . .
C12 C 0.8576(3) 0.6162(2) 0.2283(2) 0.0625(11) Uani 1 1 d . . . . .
H12A H 0.8333 0.6349 0.1821 0.075 Uiso 1 1 calc R . . . .
H12B H 0.9217 0.6038 0.2287 0.075 Uiso 1 1 calc R . . . .
C13 C 0.9423(3) 0.5906(2) 0.3852(2) 0.0615(11) Uani 1 1 d . . . . .
H13A H 0.9963 0.6126 0.4077 0.074 Uiso 1 1 calc R . . . .
H13B H 0.9577 0.5732 0.3431 0.074 Uiso 1 1 calc R . . . .
C14 C 0.9288(3) 0.5520(2) 0.4407(3) 0.0752(15) Uani 1 1 d . . . . .
H14A H 0.9810 0.5273 0.4491 0.090 Uiso 1 1 calc R . . . .
H14B H 0.9300 0.5688 0.4878 0.090 Uiso 1 1 calc R . . . .
C15 C 0.4601(2) 0.48004(13) 0.39916(17) 0.0375(6) Uani 1 1 d . . . . .
C16 C 0.4033(2) 0.45968(15) 0.44257(17) 0.0423(7) Uani 1 1 d . . . . .
C17 C 0.4138(2) 0.40959(15) 0.46455(19) 0.0476(8) Uani 1 1 d . . . . .
H17 H 0.3742 0.3965 0.4934 0.057 Uiso 1 1 calc R . . . .
C18 C 0.4797(3) 0.37827(14) 0.44594(19) 0.0470(8) Uani 1 1 d . . . . .
C19 C 0.5348(2) 0.39826(14) 0.40246(18) 0.0422(7) Uani 1 1 d . . . . .
H19 H 0.5799 0.3772 0.3885 0.051 Uiso 1 1 calc R . . . .
C20 C 0.5267(2) 0.44866(13) 0.37813(17) 0.0375(6) Uani 1 1 d . . . . .
C21 C 0.5897(2) 0.46484(13) 0.33181(17) 0.0367(6) Uani 1 1 d . . . . .
C22 C 0.6355(3) 0.42716(14) 0.2926(2) 0.0462(8) Uani 1 1 d . . . . .
H22A H 0.6376 0.4404 0.2445 0.069 Uiso 1 1 calc GR . . . .
H22B H 0.5989 0.3959 0.2863 0.069 Uiso 1 1 calc GR . . . .
H22C H 0.6999 0.4205 0.3213 0.069 Uiso 1 1 calc GR . . . .
C23 C 0.4937(4) 0.32408(17) 0.4715(3) 0.0631(11) Uani 1 1 d . . . . .
H23A H 0.4978 0.3026 0.4302 0.095 Uiso 1 1 calc GR . . . .
H23B H 0.4402 0.3134 0.4907 0.095 Uiso 1 1 calc GR . . . .
H23C H 0.5522 0.3213 0.5101 0.095 Uiso 1 1 calc GR . . . .
C24 C 0.3315(2) 0.49217(16) 0.46476(18) 0.0467(8) Uani 1 1 d . . . . .
H24A H 0.3024 0.4732 0.4988 0.056 Uiso 1 1 calc R . . . .
H24B H 0.3635 0.5219 0.4912 0.056 Uiso 1 1 calc R . . . .
C25 C 0.1842(2) 0.5385(2) 0.4286(2) 0.0592(11) Uani 1 1 d . . . . .
H25A H 0.1537 0.5159 0.4577 0.071 Uiso 1 1 calc R . . . .
H25B H 0.1347 0.5507 0.3865 0.071 Uiso 1 1 calc R . . . .
C26 C 0.2265(3) 0.5828(2) 0.4755(2) 0.0664(12) Uani 1 1 d . . . . .
H26A H 0.1755 0.6048 0.4837 0.080 Uiso 1 1 calc R . . . .
H26B H 0.2638 0.5708 0.5237 0.080 Uiso 1 1 calc R . . . .
C27 C 0.2119(10) 0.4590(6) 0.3676(8) 0.045(3) Uani 0.506(14) 1 d . . P A 1
H27A H 0.2547 0.4440 0.3400 0.054 Uiso 0.506(14) 1 calc R . P A 1
H27B H 0.2102 0.4359 0.4084 0.054 Uiso 0.506(14) 1 calc R . P A 1
C27' C 0.2085(10) 0.4719(8) 0.3517(9) 0.072(5) Uani 0.494(14) 1 d . . P A 2
H27C H 0.2604 0.4586 0.3317 0.087 Uiso 0.494(14) 1 calc R . P A 2
H27D H 0.1975 0.4455 0.3857 0.087 Uiso 0.494(14) 1 calc R . P A 2
C28 C 0.1215(11) 0.4610(9) 0.3214(9) 0.115(6) Uani 0.506(14) 1 d . U P A 1
H28A H 0.0792 0.4790 0.3466 0.138 Uiso 0.506(14) 1 calc R . P A 1
H28B H 0.0972 0.4264 0.3113 0.138 Uiso 0.506(14) 1 calc R . P A 1
C28' C 0.1327(8) 0.4659(5) 0.2942(7) 0.079(4) Uani 0.494(14) 1 d . U P A 2
H28C H 0.1289 0.4309 0.2762 0.095 Uiso 0.494(14) 1 calc R . P A 2
H28D H 0.1372 0.4887 0.2536 0.095 Uiso 0.494(14) 1 calc R . 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
Cu1 O1 2.030(2) . ?
Cu1 O3 1.968(2) . ?
Cu1 O4 2.352(3) . ?
Cu1 O6 1.876(2) . ?
Cu1 N2 1.964(3) . ?
Cu2 O1 1.941(2) . ?
Cu2 O5 1.944(2) . ?
Cu2 N1 1.926(3) . ?
Cu2 N3 1.943(3) . ?
Cu3 O2 1.894(3) . ?
Cu3 O3 1.977(2) 2_655 ?
Cu3 O5 1.985(2) . ?
Cu3 O7 2.406(3) . ?
Cu3 N4 2.032(3) . ?
O1 C1 1.359(5) . ?
O2 N1 1.360(4) . ?
O3 Cu3 1.977(2) 2_655 ?
O3 C12 1.435(5) . ?
O4 H4 0.8400 . ?
O4 C14 1.437(5) . ?
O5 C15 1.351(4) . ?
O6 N3 1.371(3) . ?
O7 C26 1.389(6) . ?
O8 H8 0.8400 . ?
O8 C28 1.537(14) . ?
O8' H8' 0.8400 . ?
O8' C28' 1.475(14) . ?
N1 C7 1.302(5) . ?
N2 C10 1.482(5) . ?
N2 C11 1.484(5) . ?
N2 C13 1.488(6) . ?
N3 C21 1.285(4) . ?
N4 C24 1.494(5) . ?
N4 C25 1.494(5) . ?
N4 C27 1.549(16) . ?
N4 C27' 1.419(15) . ?
C1 C2 1.418(5) . ?
C1 C6 1.409(6) . ?
C2 C3 1.387(7) . ?
C2 C10 1.478(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.382(9) . ?
C4 C5 1.384(7) . ?
C4 C9 1.522(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.408(6) . ?
C6 C7 1.473(5) . ?
C7 C8 1.488(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.530(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.512(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.408(4) . ?
C15 C20 1.410(5) . ?
C16 C17 1.394(6) . ?
C16 C24 1.494(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.381(6) . ?
C18 C19 1.387(5) . ?
C18 C23 1.519(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.413(5) . ?
C20 C21 1.478(4) . ?
C21 C22 1.497(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.512(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.393(14) . ?
C27' H27C 0.9900 . ?
C27' H27D 0.9900 . ?
C27' C28' 1.355(12) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28' H28C 0.9900 . ?
C28' H28D 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
O1 Cu1 O4 102.83(12) . . ?
O3 Cu1 O1 144.92(11) . . ?
O3 Cu1 O4 111.88(12) . . ?
O6 Cu1 O1 94.74(10) . . ?
O6 Cu1 O3 89.27(10) . . ?
O6 Cu1 O4 91.69(12) . . ?
O6 Cu1 N2 167.23(13) . . ?
N2 Cu1 O1 96.34(12) . . ?
N2 Cu1 O3 85.32(12) . . ?
N2 Cu1 O4 79.67(14) . . ?
O1 Cu2 O5 158.52(10) . . ?
O1 Cu2 N3 92.70(11) . . ?
N1 Cu2 O1 93.10(12) . . ?
N1 Cu2 O5 91.91(11) . . ?
N1 Cu2 N3 155.27(12) . . ?
N3 Cu2 O5 91.42(11) . . ?
O2 Cu3 O3 84.60(11) . 2_655 ?
O2 Cu3 O5 91.05(10) . . ?
O2 Cu3 O7 88.41(13) . . ?
O2 Cu3 N4 165.16(13) . . ?
O3 Cu3 O5 152.36(10) 2_655 . ?
O3 Cu3 O7 97.16(11) 2_655 . ?
O3 Cu3 N4 95.71(11) 2_655 . ?
O5 Cu3 O7 110.01(11) . . ?
O5 Cu3 N4 95.30(11) . . ?
N4 Cu3 O7 76.81(13) . . ?
Cu2 O1 Cu1 108.05(12) . . ?
C1 O1 Cu1 118.28(19) . . ?
C1 O1 Cu2 125.9(2) . . ?
N1 O2 Cu3 119.6(2) . . ?
Cu1 O3 Cu3 102.15(9) . 2_655 ?
C12 O3 Cu1 110.9(2) . . ?
C12 O3 Cu3 124.4(2) . 2_655 ?
Cu1 O4 H4 118.3 . . ?
C14 O4 Cu1 106.7(3) . . ?
C14 O4 H4 109.5 . . ?
Cu2 O5 Cu3 112.71(12) . . ?
C15 O5 Cu2 123.66(18) . . ?
C15 O5 Cu3 121.95(18) . . ?
N3 O6 Cu1 113.08(19) . . ?
C26 O7 Cu3 109.2(3) . . ?
C28 O8 H8 109.5 . . ?
C28' O8' H8' 109.5 . . ?
O2 N1 Cu2 114.0(2) . . ?
C7 N1 Cu2 130.0(3) . . ?
C7 N1 O2 115.8(3) . . ?
C10 N2 Cu1 110.8(2) . . ?
C10 N2 C11 113.3(4) . . ?
C10 N2 C13 110.3(3) . . ?
C11 N2 Cu1 103.4(2) . . ?
C11 N2 C13 110.8(3) . . ?
C13 N2 Cu1 108.0(3) . . ?
O6 N3 Cu2 113.4(2) . . ?
C21 N3 Cu2 130.1(2) . . ?
C21 N3 O6 115.1(3) . . ?
C24 N4 Cu3 105.87(19) . . ?
C24 N4 C27 102.3(5) . . ?
C25 N4 Cu3 107.0(3) . . ?
C25 N4 C24 108.6(3) . . ?
C25 N4 C27 109.6(7) . . ?
C27 N4 Cu3 122.7(6) . . ?
C27' N4 Cu3 108.8(8) . . ?
C27' N4 C24 117.2(8) . . ?
C27' N4 C25 108.9(7) . . ?
O1 C1 C2 117.0(4) . . ?
O1 C1 C6 123.4(3) . . ?
C6 C1 C2 119.6(4) . . ?
C1 C2 C10 121.7(4) . . ?
C3 C2 C1 119.5(5) . . ?
C3 C2 C10 118.7(4) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 C2 122.1(5) . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C5 117.8(5) . . ?
C3 C4 C9 121.7(5) . . ?
C5 C4 C9 120.4(6) . . ?
C4 C5 H5 118.4 . . ?
C4 C5 C6 123.1(5) . . ?
C6 C5 H5 118.4 . . ?
C1 C6 C7 125.8(3) . . ?
C5 C6 C1 117.8(4) . . ?
C5 C6 C7 116.4(4) . . ?
N1 C7 C6 121.0(4) . . ?
N1 C7 C8 118.3(4) . . ?
C6 C7 C8 120.8(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10A 108.7 . . ?
N2 C10 H10B 108.7 . . ?
C2 C10 N2 114.4(4) . . ?
C2 C10 H10A 108.7 . . ?
C2 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
N2 C11 H11A 109.8 . . ?
N2 C11 H11B 109.8 . . ?
N2 C11 C12 109.5(4) . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
O3 C12 C11 111.2(3) . . ?
O3 C12 H12A 109.4 . . ?
O3 C12 H12B 109.4 . . ?
C11 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
N2 C13 H13A 109.2 . . ?
N2 C13 H13B 109.2 . . ?
N2 C13 C14 112.0(3) . . ?
H13A C13 H13B 107.9 . . ?
C14 C13 H13A 109.2 . . ?
C14 C13 H13B 109.2 . . ?
O4 C14 C13 109.9(3) . . ?
O4 C14 H14A 109.7 . . ?
O4 C14 H14B 109.7 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
O5 C15 C16 118.4(3) . . ?
O5 C15 C20 122.9(3) . . ?
C16 C15 C20 118.7(3) . . ?
C15 C16 C24 119.5(3) . . ?
C17 C16 C15 120.2(3) . . ?
C17 C16 C24 120.3(3) . . ?
C16 C17 H17 118.8 . . ?
C18 C17 C16 122.3(3) . . ?
C18 C17 H17 118.8 . . ?
C17 C18 C19 117.3(4) . . ?
C17 C18 C23 122.8(3) . . ?
C19 C18 C23 119.9(4) . . ?
C18 C19 H19 118.6 . . ?
C18 C19 C20 122.8(3) . . ?
C20 C19 H19 118.6 . . ?
C15 C20 C19 118.7(3) . . ?
C15 C20 C21 124.4(3) . . ?
C19 C20 C21 117.0(3) . . ?
N3 C21 C20 119.4(3) . . ?
N3 C21 C22 119.7(3) . . ?
C20 C21 C22 120.9(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 C16 112.5(3) . . ?
N4 C24 H24A 109.1 . . ?
N4 C24 H24B 109.1 . . ?
C16 C24 H24A 109.1 . . ?
C16 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
N4 C25 H25A 109.0 . . ?
N4 C25 H25B 109.0 . . ?
N4 C25 C26 112.9(3) . . ?
H25A C25 H25B 107.8 . . ?
C26 C25 H25A 109.0 . . ?
C26 C25 H25B 109.0 . . ?
O7 C26 C25 109.3(3) . . ?
O7 C26 H26A 109.8 . . ?
O7 C26 H26B 109.8 . . ?
C25 C26 H26A 109.8 . . ?
C25 C26 H26B 109.8 . . ?
H26A C26 H26B 108.3 . . ?
N4 C27 H27A 108.0 . . ?
N4 C27 H27B 108.0 . . ?
H27A C27 H27B 107.3 . . ?
C28 C27 N4 117.0(15) . . ?
C28 C27 H27A 108.0 . . ?
C28 C27 H27B 108.0 . . ?
N4 C27' H27C 101.8 . . ?
N4 C27' H27D 101.8 . . ?
H27C C27' H27D 104.7 . . ?
C28' C27' N4 140.8(17) . . ?
C28' C27' H27C 101.8 . . ?
C28' C27' H27D 101.8 . . ?
O8 C28 H28A 108.9 . . ?
O8 C28 H28B 108.9 . . ?
C27 C28 O8 113.2(13) . . ?
C27 C28 H28A 108.9 . . ?
C27 C28 H28B 108.9 . . ?
H28A C28 H28B 107.7 . . ?
O8' C28' H28C 110.5 . . ?
O8' C28' H28D 110.5 . . ?
C27' C28' O8' 106.1(14) . . ?
C27' C28' H28C 110.5 . . ?
C27' C28' H28D 110.5 . . ?
H28C C28' H28D 108.7 . . ?

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
Cu1 O1 C1 C2 -43.7(4) . . . . ?
Cu1 O1 C1 C6 136.9(3) . . . . ?
Cu1 O3 C12 C11 -2.8(4) . . . . ?
Cu1 O4 C14 C13 -17.4(5) . . . . ?
Cu1 O6 N3 Cu2 48.2(2) . . . . ?
Cu1 O6 N3 C21 -144.1(2) . . . . ?
Cu1 N2 C10 C2 -57.7(5) . . . . ?
Cu1 N2 C11 C12 -46.6(4) . . . . ?
Cu1 N2 C13 C14 -55.1(4) . . . . ?
Cu2 O1 C1 C2 170.8(3) . . . . ?
Cu2 O1 C1 C6 -8.6(5) . . . . ?
Cu2 O5 C15 C16 154.3(2) . . . . ?
Cu2 O5 C15 C20 -27.1(4) . . . . ?
Cu2 N1 C7 C6 -1.8(5) . . . . ?
Cu2 N1 C7 C8 179.4(3) . . . . ?
Cu2 N3 C21 C20 -15.9(4) . . . . ?
Cu2 N3 C21 C22 166.6(2) . . . . ?
Cu3 O2 N1 Cu2 37.5(3) . . . . ?
Cu3 O2 N1 C7 -147.5(3) . . . . ?
Cu3 O3 C12 C11 119.5(3) 2_655 . . . ?
Cu3 O5 C15 C16 -41.5(4) . . . . ?
Cu3 O5 C15 C20 137.0(2) . . . . ?
Cu3 O7 C26 C25 -15.9(4) . . . . ?
Cu3 N4 C24 C16 -69.2(3) . . . . ?
Cu3 N4 C25 C26 -56.7(4) . . . . ?
Cu3 N4 C27 C28 -81.3(15) . . . . ?
Cu3 N4 C27' C28' -70(3) . . . . ?
O1 Cu1 O6 N3 -29.3(2) . . . . ?
O1 C1 C2 C3 178.6(4) . . . . ?
O1 C1 C2 C10 -4.2(6) . . . . ?
O1 C1 C6 C5 -179.6(4) . . . . ?
O1 C1 C6 C7 -0.3(6) . . . . ?
O2 N1 C7 C6 -175.9(3) . . . . ?
O2 N1 C7 C8 5.4(5) . . . . ?
O3 Cu1 O6 N3 -174.4(2) . . . . ?
O3 Cu3 O2 N1 -173.9(2) 2_655 . . . ?
O4 Cu1 O6 N3 73.7(2) . . . . ?
O5 Cu3 O2 N1 -21.2(2) . . . . ?
O5 C15 C16 C17 179.2(3) . . . . ?
O5 C15 C16 C24 -0.7(4) . . . . ?
O5 C15 C20 C19 -179.6(3) . . . . ?
O5 C15 C20 C21 0.4(5) . . . . ?
O6 N3 C21 C20 178.8(2) . . . . ?
O6 N3 C21 C22 1.4(4) . . . . ?
O7 Cu3 O2 N1 88.8(2) . . . . ?
N2 Cu1 O6 N3 120.8(5) . . . . ?
N2 C11 C12 O3 33.4(5) . . . . ?
N2 C13 C14 O4 47.1(6) . . . . ?
N4 Cu3 O2 N1 94.2(5) . . . . ?
N4 C25 C26 O7 47.4(5) . . . . ?
N4 C27 C28 O8 69(2) . . . . ?
N4 C27' C28' O8' -61(3) . . . . ?
C1 C2 C3 C4 1.3(9) . . . . ?
C1 C2 C10 N2 63.0(6) . . . . ?
C1 C6 C7 N1 5.9(6) . . . . ?
C1 C6 C7 C8 -175.4(4) . . . . ?
C2 C1 C6 C5 0.9(6) . . . . ?
C2 C1 C6 C7 -179.8(4) . . . . ?
C2 C3 C4 C5 0.2(9) . . . . ?
C2 C3 C4 C9 -178.5(6) . . . . ?
C3 C2 C10 N2 -119.8(5) . . . . ?
C3 C4 C5 C6 -1.3(9) . . . . ?
C4 C5 C6 C1 0.6(7) . . . . ?
C4 C5 C6 C7 -178.7(5) . . . . ?
C5 C6 C7 N1 -174.9(4) . . . . ?
C5 C6 C7 C8 3.9(6) . . . . ?
C6 C1 C2 C3 -1.9(7) . . . . ?
C6 C1 C2 C10 175.3(4) . . . . ?
C9 C4 C5 C6 177.6(6) . . . . ?
C10 N2 C11 C12 -166.5(3) . . . . ?
C10 N2 C13 C14 66.1(5) . . . . ?
C10 C2 C3 C4 -176.0(5) . . . . ?
C11 N2 C10 C2 57.9(4) . . . . ?
C11 N2 C13 C14 -167.6(4) . . . . ?
C13 N2 C10 C2 -177.2(4) . . . . ?
C13 N2 C11 C12 68.9(4) . . . . ?
C15 C16 C17 C18 0.7(5) . . . . ?
C15 C16 C24 N4 64.3(4) . . . . ?
C15 C20 C21 N3 22.1(4) . . . . ?
C15 C20 C21 C22 -160.5(3) . . . . ?
C16 C15 C20 C19 -1.0(4) . . . . ?
C16 C15 C20 C21 179.0(3) . . . . ?
C16 C17 C18 C19 -1.4(5) . . . . ?
C16 C17 C18 C23 178.1(3) . . . . ?
C17 C16 C24 N4 -115.6(4) . . . . ?
C17 C18 C19 C20 0.9(5) . . . . ?
C18 C19 C20 C15 0.3(5) . . . . ?
C18 C19 C20 C21 -179.7(3) . . . . ?
C19 C20 C21 N3 -157.9(3) . . . . ?
C19 C20 C21 C22 19.5(4) . . . . ?
C20 C15 C16 C17 0.5(4) . . . . ?
C20 C15 C16 C24 -179.3(3) . . . . ?
C23 C18 C19 C20 -178.6(3) . . . . ?
C24 N4 C25 C26 57.2(5) . . . . ?
C24 N4 C27 C28 160.6(12) . . . . ?
C24 N4 C27' C28' 170(2) . . . . ?
C24 C16 C17 C18 -179.4(3) . . . . ?
C25 N4 C24 C16 176.2(3) . . . . ?
C25 N4 C27 C28 45.4(14) . . . . ?
C25 N4 C27' C28' 46(3) . . . . ?
C27 N4 C24 C16 60.3(8) . . . . ?
C27 N4 C25 C26 168.2(6) . . . . ?
C27 N4 C27' C28' 142(6) . . . . ?
C27' N4 C24 C16 52.3(9) . . . . ?
C27' N4 C25 C26 -174.1(9) . . . . ?
C27' N4 C27 C28 -45(4) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6 13 1 0.0131 -5.9999 12.9989 0.9996 -0.2530 0.9526 0.0140
0 3 12 0.1279 -0.0001 3.0002 12.0002 -0.0308 0.0341 1.0261
0 -3 -12 0.1279 0.0001 -3.0002 -12.0002 0.0308 -0.0341 -1.0261
9 6 -1 0.0187 8.9999 6.0010 -0.9996 0.9871 -0.1104 0.2455
-9 -6 0 0.0104 -8.9999 -6.0010 -0.0004 -0.9785 0.1206 -0.3288
3 16 -1 0.0167 3.0000 15.9999 -1.0000 0.6706 0.6966 0.1498
-3 -16 1 0.0167 -3.0000 -15.9999 1.0000 -0.6706 -0.6966 -0.1498
7 -12 -1 0.0164 6.9999 -11.9988 -0.9995 0.3697 -0.9487 0.0254

####################################################################### 
# 
# 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_eb3275b
_database_code_depnum_ccdc_archive 'CCDC 991828'
_audit_update_record             
;
2015-03-27 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
_audit_creation_date             2015-03-27
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C56 H78 Cu4 N8 Na2 O16, 2.5 C H4 O'
_chemical_formula_sum            'C58.50 H84 Cu4 N8 Na2 O18.50'
_chemical_formula_weight         1495.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H50 N10 O20 Cu8 B F4'
_chemical_oxdiff_usercomment     '@ 120 K RS60'
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'
Na Na 0.0362 0.0249 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   15.2213(3)
_cell_length_b                   26.3669(6)
_cell_length_c                   17.2409(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.295(2)
_cell_angle_gamma                90
_cell_volume                     6908.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11836
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.1480
_cell_measurement_theta_min      3.0920
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.948
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3108
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of methanol and diethyl ether by solvent layering'
_exptl_crystal_size_max          0.2457
_exptl_crystal_size_mid          0.1298
_exptl_crystal_size_min          0.0164
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57914
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.887
_diffrn_reflns_theta_min         2.826
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -76.00    9.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -57.0000  150.0000 85

#__ type_ start__ end____ width___ exp.time_
  2 omega  -70.00  -43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -19.0000  -90.0000 27

#__ type_ start__ end____ width___ exp.time_
  3 omega  -15.00   16.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -19.0000  -90.0000 31

#__ type_ start__ end____ width___ exp.time_
  4 omega  -81.00    0.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -77.0000   60.0000 81

#__ type_ start__ end____ width___ exp.time_
  5 omega  -67.00  -35.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  132.0000 -116.5641 32

#__ type_ start__ end____ width___ exp.time_
  6 omega  -28.00   27.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352   38.0000  150.0000 55

#__ type_ start__ end____ width___ exp.time_
  7 omega  -42.00    1.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352   19.0000   30.0000 43

#__ type_ start__ end____ width___ exp.time_
  8 omega   36.00   63.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352   19.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
  9 omega  -38.00    0.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -77.0000  -90.0000 38

#__ type_ start__ end____ width___ exp.time_
 10 omega   24.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633 -125.0000  -52.0766 27

#__ type_ start__ end____ width___ exp.time_
 11 omega  -19.00   36.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -99.0000  -30.0000 55

#__ type_ start__ end____ width___ exp.time_
 12 omega  -42.00  -15.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -38.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
 13 omega  -30.00   46.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352   38.0000   90.0000 76
;
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0088758000
_diffrn_orient_matrix_UB_12      0.0263376000
_diffrn_orient_matrix_UB_13      0.0025292000
_diffrn_orient_matrix_UB_21      -0.0347079000
_diffrn_orient_matrix_UB_22      -0.0051507000
_diffrn_orient_matrix_UB_23      0.0246082000
_diffrn_orient_matrix_UB_31      0.0299335000
_diffrn_orient_matrix_UB_32      0.0018291000
_diffrn_orient_matrix_UB_33      0.0329514000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5909
_reflns_number_total             8317
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         8317
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0472
_refine_ls_restrained_S_all      1.033
_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)+(0.0384P)²+14.6993P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1062
_refine_special_details          
'The squeeze routine of PLATON was used to removed 2.5 methanol per asymmetric unit, which could be identifed in a difference Fourier map but not modelled with discrete atoms to a satisfactory convergence. The missing solvent has been included in the total chemical formula and this triggers several alerts in checkCIF which should be ignored.'



# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.003 0.250 294 82 ' '
2 0.000 -0.004 0.750 289 82 ' '
3 0.000 0.337 0.750 8 0 ' '
4 0.000 0.409 0.250 6 0 ' '
5 0.000 0.417 0.750 8 0 ' '
6 0.000 0.585 0.250 9 0 ' '
7 0.000 0.591 0.750 6 0 ' '
8 0.000 0.666 0.250 7 0 ' '
9 0.500 0.504 0.250 294 82 ' '
10 0.500 0.496 0.750 289 82 ' '
11 0.500 0.085 0.250 9 0 ' '
12 0.500 0.091 0.750 6 0 ' '
13 0.500 0.166 0.250 7 0 ' '
14 0.500 0.837 0.750 8 0 ' '
15 0.500 0.909 0.250 6 0 ' '
16 0.500 0.917 0.750 8 0 ' '
# Missing Reflections Below sin(th)/lambda= 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
2 0 0 2.681
1 1 0 1.547
0 2 0 1.545
1 3 0 2.677
3 9 0 8.055
-1 1 1 1.900
1 1 1 1.994
0 2 1 1.946
0 0 2 2.367
-1 1 2 2.762
1 1 2 2.891
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          '2.5 methanol per asymmetric unit'


_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H3 of O3, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H7 of O7, H8 of O8
2. Restrained distances
 O3-H3
 0.84 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C17(H17), C19(H19)
3.c Tetrahedral OH refined with riding coordinates:
 O7(H7), O8(H8)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.65622(2) 0.18669(2) 0.10996(2) 0.01884(10) Uani 1 1 d . . . . .
Cu2 Cu 0.44471(2) 0.20592(2) 0.11425(2) 0.01745(10) Uani 1 1 d . . . . .
Na1 Na 0.27190(7) 0.23358(4) 0.22714(7) 0.0230(3) Uani 1 1 d . . . . .
O1 O 0.53721(12) 0.16567(7) 0.07134(11) 0.0189(4) Uani 1 1 d . . . . .
O2 O 0.31306(13) 0.15099(8) 0.18265(11) 0.0228(5) Uani 1 1 d . . . . .
O3 O 0.66329(14) 0.11047(8) 0.17929(12) 0.0251(5) Uani 1 1 d D . . . .
H3 H 0.664(2) 0.1229(12) 0.2240(10) 0.030 Uiso 1 1 d DR . . . .
O4 O 0.77032(13) 0.21559(8) 0.13861(12) 0.0264(5) Uani 1 1 d . . . . .
O5 O 0.34935(12) 0.25161(7) 0.11965(11) 0.0194(4) Uani 1 1 d . . . . .
O6 O 0.60829(12) 0.23895(8) 0.17241(12) 0.0242(5) Uani 1 1 d . . . . .
O7 O 0.20826(13) 0.30511(8) 0.30160(12) 0.0264(5) Uani 1 1 d . . . . .
H7 H 0.2269 0.3327 0.3206 0.040 Uiso 1 1 calc R . . . .
O8 O 0.14336(15) 0.16917(9) 0.17349(13) 0.0362(6) Uani 1 1 d . . . . .
H8 H 0.1290 0.1384 0.1733 0.054 Uiso 1 1 calc R . . . .
N1 N 0.37285(15) 0.14612(9) 0.12727(13) 0.0186(5) Uani 1 1 d . . . . .
N2 N 0.71909(15) 0.14345(9) 0.03439(14) 0.0204(5) Uani 1 1 d . . . . .
N3 N 0.52982(15) 0.25765(9) 0.14228(14) 0.0195(5) Uani 1 1 d . . . . .
N4 N 0.15456(15) 0.28079(10) 0.13930(14) 0.0236(6) Uani 1 1 d . . . . .
C1 C 0.51929(18) 0.12503(10) 0.02570(16) 0.0181(6) Uani 1 1 d . . . . .
C2 C 0.57802(19) 0.11198(11) -0.03121(17) 0.0202(6) Uani 1 1 d . . . . .
C3 C 0.5561(2) 0.07318(11) -0.08397(17) 0.0220(6) Uani 1 1 d . . . . .
H3A H 0.5958 0.0653 -0.1228 0.026 Uiso 1 1 calc R . . . .
C4 C 0.4786(2) 0.04587(11) -0.08155(17) 0.0220(6) Uani 1 1 d . . . . .
C5 C 0.42505(19) 0.05621(11) -0.02108(17) 0.0211(6) Uani 1 1 d . . . . .
H5 H 0.3736 0.0363 -0.0166 0.025 Uiso 1 1 calc R . . . .
C6 C 0.44340(18) 0.09479(11) 0.03389(17) 0.0194(6) Uani 1 1 d . . . . .
C7 C 0.38150(18) 0.10183(11) 0.09559(16) 0.0190(6) Uani 1 1 d . . . . .
C8 C 0.3262(2) 0.05874(12) 0.12276(19) 0.0271(7) Uani 1 1 d . . . . .
H8A H 0.3344 0.0556 0.1794 0.041 Uiso 1 1 calc GR . . . .
H8B H 0.3442 0.0271 0.0983 0.041 Uiso 1 1 calc GR . . . .
H8C H 0.2641 0.0654 0.1083 0.041 Uiso 1 1 calc GR . . . .
C9 C 0.4526(2) 0.00676(12) -0.14215(19) 0.0292(7) Uani 1 1 d . . . . .
H9A H 0.4087 0.0213 -0.1797 0.044 Uiso 1 1 calc GR . . . .
H9B H 0.4275 -0.0228 -0.1171 0.044 Uiso 1 1 calc GR . . . .
H9C H 0.5046 -0.0036 -0.1692 0.044 Uiso 1 1 calc GR . . . .
C10 C 0.66233(19) 0.14051(12) -0.03934(16) 0.0227(7) Uani 1 1 d . . . . .
H10A H 0.6960 0.1238 -0.0797 0.027 Uiso 1 1 calc R . . . .
H10B H 0.6482 0.1754 -0.0574 0.027 Uiso 1 1 calc R . . . .
C11 C 0.7401(2) 0.09214(12) 0.06683(17) 0.0250(7) Uani 1 1 d . . . . .
H11A H 0.7974 0.0809 0.0485 0.030 Uiso 1 1 calc R . . . .
H11B H 0.6947 0.0678 0.0469 0.030 Uiso 1 1 calc R . . . .
C12 C 0.7445(2) 0.09113(12) 0.15536(18) 0.0270(7) Uani 1 1 d . . . . .
H12A H 0.7535 0.0560 0.1745 0.032 Uiso 1 1 calc R . . . .
H12B H 0.7939 0.1123 0.1765 0.032 Uiso 1 1 calc R . . . .
C13 C 0.7999(2) 0.17346(13) 0.01986(19) 0.0276(7) Uani 1 1 d . . . . .
H13A H 0.7848 0.2013 -0.0171 0.033 Uiso 1 1 calc R . . . .
H13B H 0.8438 0.1513 -0.0035 0.033 Uiso 1 1 calc R . . . .
C14 C 0.8385(2) 0.19537(13) 0.09600(19) 0.0282(7) Uani 1 1 d . . . . .
H14A H 0.8697 0.1685 0.1266 0.034 Uiso 1 1 calc R . . . .
H14B H 0.8814 0.2223 0.0853 0.034 Uiso 1 1 calc R . . . .
C15 C 0.35615(19) 0.30103(11) 0.10509(16) 0.0198(6) Uani 1 1 d . . . . .
C16 C 0.27789(19) 0.32711(12) 0.07954(17) 0.0233(7) Uani 1 1 d . . . . .
C17 C 0.2818(2) 0.37823(13) 0.06265(19) 0.0317(8) Uani 1 1 d . . . . .
H17 H 0.2289 0.3951 0.0459 0.038 Uiso 1 1 calc R . . . .
C18 C 0.3592(2) 0.40616(13) 0.0690(2) 0.0363(8) Uani 1 1 d . . . . .
C19 C 0.4350(2) 0.38090(13) 0.0956(2) 0.0311(8) Uani 1 1 d . . . . .
H19 H 0.4886 0.3994 0.1013 0.037 Uiso 1 1 calc R . . . .
C20 C 0.43549(19) 0.32882(11) 0.11449(16) 0.0199(6) Uani 1 1 d . . . . .
C21 C 0.51853(19) 0.30625(11) 0.14604(17) 0.0197(6) Uani 1 1 d . . . . .
C22 C 0.5891(2) 0.33906(12) 0.18337(18) 0.0255(7) Uani 1 1 d . . . . .
H22A H 0.6149 0.3222 0.2300 0.038 Uiso 1 1 calc GR . . . .
H22B H 0.5638 0.3716 0.1979 0.038 Uiso 1 1 calc GR . . . .
H22C H 0.6350 0.3448 0.1467 0.038 Uiso 1 1 calc GR . . . .
C23 C 0.3606(3) 0.46223(15) 0.0499(3) 0.0649(14) Uani 1 1 d . . . . .
H23A H 0.4211 0.4749 0.0566 0.097 Uiso 1 1 calc GR . . . .
H23B H 0.3232 0.4806 0.0848 0.097 Uiso 1 1 calc GR . . . .
H23C H 0.3385 0.4674 -0.0040 0.097 Uiso 1 1 calc GR . . . .
C24 C 0.19238(19) 0.29828(12) 0.06754(17) 0.0243(7) Uani 1 1 d . . . . .
H24A H 0.1489 0.3203 0.0391 0.029 Uiso 1 1 calc R . . . .
H24B H 0.2024 0.2684 0.0343 0.029 Uiso 1 1 calc R . . . .
C25 C 0.1239(2) 0.32435(13) 0.18413(18) 0.0274(7) Uani 1 1 d . . . . .
H25A H 0.0644 0.3344 0.1635 0.033 Uiso 1 1 calc R . . . .
H25B H 0.1640 0.3535 0.1778 0.033 Uiso 1 1 calc R . . . .
C26 C 0.12098(19) 0.31175(13) 0.26933(18) 0.0262(7) Uani 1 1 d . . . . .
H26A H 0.0918 0.3395 0.2967 0.031 Uiso 1 1 calc R . . . .
H26B H 0.0867 0.2803 0.2758 0.031 Uiso 1 1 calc R . . . .
C27 C 0.0814(2) 0.24596(13) 0.11916(19) 0.0296(8) Uani 1 1 d . . . . .
H27A H 0.0477 0.2592 0.0727 0.036 Uiso 1 1 calc R . . . .
H27B H 0.0415 0.2453 0.1625 0.036 Uiso 1 1 calc R . . . .
C28 C 0.1105(2) 0.19238(13) 0.1029(2) 0.0334(8) Uani 1 1 d . . . . .
H28A H 0.0602 0.1726 0.0801 0.040 Uiso 1 1 calc R . . . .
H28B H 0.1571 0.1929 0.0652 0.040 Uiso 1 1 calc R . . . .


_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 O1 1.9733(18) . ?
Cu1 O3 2.338(2) . ?
Cu1 O4 1.934(2) . ?
Cu1 O6 1.919(2) . ?
Cu1 N2 2.014(2) . ?
Cu2 O1 1.9431(19) . ?
Cu2 O5 1.8928(19) . ?
Cu2 N1 1.939(2) . ?
Cu2 N3 1.924(2) . ?
Na1 Cu1 3.2032(12) 2_655 ?
Na1 O2 2.404(2) . ?
Na1 O4 2.483(2) 2_655 ?
Na1 O5 2.302(2) . ?
Na1 O6 2.446(2) 2_655 ?
Na1 O7 2.507(2) . ?
Na1 O8 2.713(3) . ?
Na1 N4 2.593(3) . ?
O1 C1 1.348(3) . ?
O2 N1 1.363(3) . ?
O3 H3 0.837(10) . ?
O3 C12 1.420(4) . ?
O4 Na1 2.483(2) 2_655 ?
O4 C14 1.410(4) . ?
O5 C15 1.332(3) . ?
O6 Na1 2.446(2) 2_655 ?
O6 N3 1.367(3) . ?
O7 H7 0.8400 . ?
O7 C26 1.421(3) . ?
O8 H8 0.8400 . ?
O8 C28 1.426(4) . ?
N1 C7 1.299(4) . ?
N2 C10 1.498(4) . ?
N2 C11 1.492(4) . ?
N2 C13 1.495(4) . ?
N3 C21 1.295(4) . ?
N4 C24 1.469(4) . ?
N4 C25 1.475(4) . ?
N4 C27 1.469(4) . ?
C1 C2 1.408(4) . ?
C1 C6 1.417(4) . ?
C2 C3 1.396(4) . ?
C2 C10 1.501(4) . ?
C3 H3A 0.9500 . ?
C3 C4 1.385(4) . ?
C4 C5 1.387(4) . ?
C4 C9 1.505(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.407(4) . ?
C6 C7 1.473(4) . ?
C7 C8 1.504(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.524(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.521(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.423(4) . ?
C15 C20 1.414(4) . ?
C16 C17 1.381(5) . ?
C16 C24 1.511(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.389(5) . ?
C18 C19 1.387(5) . ?
C18 C23 1.515(5) . ?
C19 H19 0.9500 . ?
C19 C20 1.411(4) . ?
C20 C21 1.473(4) . ?
C21 C22 1.496(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.509(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.512(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 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
O1 Cu1 O3 86.87(8) . . ?
O1 Cu1 N2 94.81(9) . . ?
O4 Cu1 O1 171.95(9) . . ?
O4 Cu1 O3 101.17(8) . . ?
O4 Cu1 N2 86.28(9) . . ?
O6 Cu1 O1 91.14(8) . . ?
O6 Cu1 O3 109.77(8) . . ?
O6 Cu1 O4 86.48(9) . . ?
O6 Cu1 N2 168.46(10) . . ?
N2 Cu1 O3 80.47(9) . . ?
O5 Cu2 O1 160.20(8) . . ?
O5 Cu2 N1 94.16(9) . . ?
O5 Cu2 N3 92.49(9) . . ?
N1 Cu2 O1 91.48(9) . . ?
N3 Cu2 O1 89.47(9) . . ?
N3 Cu2 N1 157.45(10) . . ?
O2 Na1 Cu1 81.26(6) . 2_655 ?
O2 Na1 O4 102.15(8) . 2_655 ?
O2 Na1 O6 94.65(8) . 2_655 ?
O2 Na1 O7 163.80(9) . . ?
O2 Na1 O8 61.33(7) . . ?
O2 Na1 N4 115.60(8) . . ?
O4 Na1 Cu1 37.12(5) 2_655 2_655 ?
O4 Na1 O7 62.50(8) 2_655 . ?
O4 Na1 O8 88.74(8) 2_655 . ?
O4 Na1 N4 115.45(8) 2_655 . ?
O5 Na1 Cu1 128.36(6) . 2_655 ?
O5 Na1 O2 77.02(8) . . ?
O5 Na1 O4 164.06(8) . 2_655 ?
O5 Na1 O6 99.35(8) . 2_655 ?
O5 Na1 O7 119.17(9) . . ?
O5 Na1 O8 104.33(8) . . ?
O5 Na1 N4 78.35(8) . . ?
O6 Na1 Cu1 36.71(5) 2_655 2_655 ?
O6 Na1 O4 64.75(7) 2_655 2_655 ?
O6 Na1 O7 83.58(8) 2_655 . ?
O6 Na1 O8 140.49(8) 2_655 . ?
O6 Na1 N4 147.81(9) 2_655 . ?
O7 Na1 Cu1 87.93(6) . 2_655 ?
O7 Na1 O8 110.68(8) . . ?
O7 Na1 N4 70.39(8) . . ?
O8 Na1 Cu1 105.11(6) . 2_655 ?
N4 Na1 Cu1 152.44(7) . 2_655 ?
N4 Na1 O8 69.04(8) . . ?
Cu2 O1 Cu1 112.91(9) . . ?
C1 O1 Cu1 124.84(17) . . ?
C1 O1 Cu2 121.98(17) . . ?
N1 O2 Na1 120.38(16) . . ?
Cu1 O3 H3 98(2) . . ?
C12 O3 Cu1 100.10(17) . . ?
C12 O3 H3 116(2) . . ?
Cu1 O4 Na1 92.10(8) . 2_655 ?
C14 O4 Cu1 113.25(18) . . ?
C14 O4 Na1 142.70(18) . 2_655 ?
Cu2 O5 Na1 109.74(9) . . ?
C15 O5 Cu2 123.05(18) . . ?
C15 O5 Na1 113.74(17) . . ?
Cu1 O6 Na1 93.65(8) . 2_655 ?
N3 O6 Cu1 113.45(15) . . ?
N3 O6 Na1 152.84(17) . 2_655 ?
Na1 O7 H7 136.0 . . ?
C26 O7 Na1 105.79(16) . . ?
C26 O7 H7 109.5 . . ?
Na1 O8 H8 142.0 . . ?
C28 O8 Na1 103.45(19) . . ?
C28 O8 H8 109.5 . . ?
O2 N1 Cu2 114.11(17) . . ?
C7 N1 Cu2 127.6(2) . . ?
C7 N1 O2 117.8(2) . . ?
C10 N2 Cu1 107.82(17) . . ?
C11 N2 Cu1 111.76(18) . . ?
C11 N2 C10 111.9(2) . . ?
C11 N2 C13 112.4(2) . . ?
C13 N2 Cu1 103.58(18) . . ?
C13 N2 C10 109.0(2) . . ?
O6 N3 Cu2 113.64(17) . . ?
C21 N3 Cu2 128.67(19) . . ?
C21 N3 O6 117.0(2) . . ?
C24 N4 Na1 110.64(16) . . ?
C24 N4 C25 110.4(2) . . ?
C24 N4 C27 109.0(2) . . ?
C25 N4 Na1 107.21(17) . . ?
C27 N4 Na1 108.97(19) . . ?
C27 N4 C25 110.6(2) . . ?
O1 C1 C2 119.1(3) . . ?
O1 C1 C6 121.9(3) . . ?
C2 C1 C6 119.1(3) . . ?
C1 C2 C10 121.6(3) . . ?
C3 C2 C1 119.7(3) . . ?
C3 C2 C10 118.7(3) . . ?
C2 C3 H3A 118.9 . . ?
C4 C3 C2 122.2(3) . . ?
C4 C3 H3A 118.9 . . ?
C3 C4 C5 117.3(3) . . ?
C3 C4 C9 121.8(3) . . ?
C5 C4 C9 120.9(3) . . ?
C4 C5 H5 118.5 . . ?
C4 C5 C6 123.1(3) . . ?
C6 C5 H5 118.5 . . ?
C1 C6 C7 124.1(3) . . ?
C5 C6 C1 118.1(3) . . ?
C5 C6 C7 117.8(3) . . ?
N1 C7 C6 120.1(3) . . ?
N1 C7 C8 118.4(3) . . ?
C6 C7 C8 121.5(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C2 113.7(2) . . ?
N2 C10 H10A 108.8 . . ?
N2 C10 H10B 108.8 . . ?
C2 C10 H10A 108.8 . . ?
C2 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
N2 C11 H11A 109.0 . . ?
N2 C11 H11B 109.0 . . ?
N2 C11 C12 112.8(2) . . ?
H11A C11 H11B 107.8 . . ?
C12 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
O3 C12 C11 107.2(2) . . ?
O3 C12 H12A 110.3 . . ?
O3 C12 H12B 110.3 . . ?
C11 C12 H12A 110.3 . . ?
C11 C12 H12B 110.3 . . ?
H12A C12 H12B 108.5 . . ?
N2 C13 H13A 109.7 . . ?
N2 C13 H13B 109.7 . . ?
N2 C13 C14 109.7(3) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.7 . . ?
C14 C13 H13B 109.7 . . ?
O4 C14 C13 109.5(2) . . ?
O4 C14 H14A 109.8 . . ?
O4 C14 H14B 109.8 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
H14A C14 H14B 108.2 . . ?
O5 C15 C16 117.3(3) . . ?
O5 C15 C20 124.1(3) . . ?
C20 C15 C16 118.6(3) . . ?
C15 C16 C24 119.9(3) . . ?
C17 C16 C15 119.5(3) . . ?
C17 C16 C24 120.6(3) . . ?
C16 C17 H17 118.4 . . ?
C16 C17 C18 123.2(3) . . ?
C18 C17 H17 118.4 . . ?
C17 C18 C23 121.5(3) . . ?
C19 C18 C17 117.2(3) . . ?
C19 C18 C23 121.2(3) . . ?
C18 C19 H19 118.8 . . ?
C18 C19 C20 122.5(3) . . ?
C20 C19 H19 118.8 . . ?
C15 C20 C21 122.8(3) . . ?
C19 C20 C15 119.0(3) . . ?
C19 C20 C21 118.1(3) . . ?
N3 C21 C20 119.7(3) . . ?
N3 C21 C22 120.0(3) . . ?
C20 C21 C22 120.4(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 C16 114.8(2) . . ?
N4 C24 H24A 108.6 . . ?
N4 C24 H24B 108.6 . . ?
C16 C24 H24A 108.6 . . ?
C16 C24 H24B 108.6 . . ?
H24A C24 H24B 107.6 . . ?
N4 C25 H25A 109.3 . . ?
N4 C25 H25B 109.3 . . ?
N4 C25 C26 111.5(3) . . ?
H25A C25 H25B 108.0 . . ?
C26 C25 H25A 109.3 . . ?
C26 C25 H25B 109.3 . . ?
O7 C26 C25 109.2(2) . . ?
O7 C26 H26A 109.8 . . ?
O7 C26 H26B 109.8 . . ?
C25 C26 H26A 109.8 . . ?
C25 C26 H26B 109.8 . . ?
H26A C26 H26B 108.3 . . ?
N4 C27 H27A 108.8 . . ?
N4 C27 H27B 108.8 . . ?
N4 C27 C28 113.7(3) . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 H27A 108.8 . . ?
C28 C27 H27B 108.8 . . ?
O8 C28 C27 109.6(3) . . ?
O8 C28 H28A 109.8 . . ?
O8 C28 H28B 109.8 . . ?
C27 C28 H28A 109.8 . . ?
C27 C28 H28B 109.8 . . ?
H28A C28 H28B 108.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O2 0.837(10) 1.788(12) 2.615(3) 169(3) 2_655

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
Cu1 O1 C1 C2 -35.9(3) . . . . ?
Cu1 O1 C1 C6 143.5(2) . . . . ?
Cu1 O3 C12 C11 -52.1(2) . . . . ?
Cu1 O4 C14 C13 22.8(3) . . . . ?
Cu1 O6 N3 Cu2 50.2(2) . . . . ?
Cu1 O6 N3 C21 -138.7(2) . . . . ?
Cu1 N2 C10 C2 -67.0(3) . . . . ?
Cu1 N2 C11 C12 -23.3(3) . . . . ?
Cu1 N2 C13 C14 42.2(3) . . . . ?
Cu2 O1 C1 C2 150.4(2) . . . . ?
Cu2 O1 C1 C6 -30.2(3) . . . . ?
Cu2 O5 C15 C16 154.6(2) . . . . ?
Cu2 O5 C15 C20 -26.3(4) . . . . ?
Cu2 N1 C7 C6 -9.4(4) . . . . ?
Cu2 N1 C7 C8 171.4(2) . . . . ?
Cu2 N3 C21 C20 -10.6(4) . . . . ?
Cu2 N3 C21 C22 168.5(2) . . . . ?
Na1 O2 N1 Cu2 18.4(2) . . . . ?
Na1 O2 N1 C7 -168.26(18) . . . . ?
Na1 O4 C14 C13 151.8(2) 2_655 . . . ?
Na1 O5 C15 C16 -68.8(3) . . . . ?
Na1 O5 C15 C20 110.3(3) . . . . ?
Na1 O6 N3 Cu2 -125.7(3) 2_655 . . . ?
Na1 O6 N3 C21 45.4(5) 2_655 . . . ?
Na1 O7 C26 C25 -59.9(3) . . . . ?
Na1 O8 C28 C27 -56.0(3) . . . . ?
Na1 N4 C24 C16 -50.1(3) . . . . ?
Na1 N4 C25 C26 -35.4(3) . . . . ?
Na1 N4 C27 C28 -39.2(3) . . . . ?
O1 Cu2 O5 Na1 156.2(2) . . . . ?
O1 Cu2 O5 C15 -65.8(3) . . . . ?
O1 C1 C2 C3 -173.6(2) . . . . ?
O1 C1 C2 C10 3.3(4) . . . . ?
O1 C1 C6 C5 173.7(2) . . . . ?
O1 C1 C6 C7 -5.1(4) . . . . ?
O2 N1 C7 C6 178.3(2) . . . . ?
O2 N1 C7 C8 -0.9(4) . . . . ?
O5 C15 C16 C17 -179.1(3) . . . . ?
O5 C15 C16 C24 -2.0(4) . . . . ?
O5 C15 C20 C19 178.7(3) . . . . ?
O5 C15 C20 C21 -3.7(4) . . . . ?
O6 N3 C21 C20 179.9(2) . . . . ?
O6 N3 C21 C22 -1.0(4) . . . . ?
N1 Cu2 O5 Na1 49.96(10) . . . . ?
N1 Cu2 O5 C15 -172.0(2) . . . . ?
N2 C11 C12 O3 55.2(3) . . . . ?
N2 C13 C14 O4 -44.2(3) . . . . ?
N3 Cu2 O5 Na1 -108.48(11) . . . . ?
N3 Cu2 O5 C15 29.6(2) . . . . ?
N4 C25 C26 O7 68.1(3) . . . . ?
N4 C27 C28 O8 70.2(4) . . . . ?
C1 C2 C3 C4 -1.4(4) . . . . ?
C1 C2 C10 N2 54.3(4) . . . . ?
C1 C6 C7 N1 26.4(4) . . . . ?
C1 C6 C7 C8 -154.4(3) . . . . ?
C2 C1 C6 C5 -6.9(4) . . . . ?
C2 C1 C6 C7 174.3(3) . . . . ?
C2 C3 C4 C5 -4.1(4) . . . . ?
C2 C3 C4 C9 175.4(3) . . . . ?
C3 C2 C10 N2 -128.7(3) . . . . ?
C3 C4 C5 C6 4.0(4) . . . . ?
C4 C5 C6 C1 1.4(4) . . . . ?
C4 C5 C6 C7 -179.7(3) . . . . ?
C5 C6 C7 N1 -152.4(3) . . . . ?
C5 C6 C7 C8 26.8(4) . . . . ?
C6 C1 C2 C3 7.0(4) . . . . ?
C6 C1 C2 C10 -176.1(3) . . . . ?
C9 C4 C5 C6 -175.5(3) . . . . ?
C10 N2 C11 C12 -144.3(3) . . . . ?
C10 N2 C13 C14 156.8(3) . . . . ?
C10 C2 C3 C4 -178.5(3) . . . . ?
C11 N2 C10 C2 56.2(3) . . . . ?
C11 N2 C13 C14 -78.6(3) . . . . ?
C13 N2 C10 C2 -178.8(2) . . . . ?
C13 N2 C11 C12 92.7(3) . . . . ?
C15 C16 C17 C18 0.2(5) . . . . ?
C15 C16 C24 N4 70.8(4) . . . . ?
C15 C20 C21 N3 23.0(4) . . . . ?
C15 C20 C21 C22 -156.1(3) . . . . ?
C16 C15 C20 C19 -2.2(4) . . . . ?
C16 C15 C20 C21 175.4(3) . . . . ?
C16 C17 C18 C19 -1.6(5) . . . . ?
C16 C17 C18 C23 180.0(4) . . . . ?
C17 C16 C24 N4 -112.1(3) . . . . ?
C17 C18 C19 C20 1.1(5) . . . . ?
C18 C19 C20 C15 0.8(5) . . . . ?
C18 C19 C20 C21 -176.9(3) . . . . ?
C19 C20 C21 N3 -159.3(3) . . . . ?
C19 C20 C21 C22 21.6(4) . . . . ?
C20 C15 C16 C17 1.7(4) . . . . ?
C20 C15 C16 C24 178.9(3) . . . . ?
C23 C18 C19 C20 179.5(4) . . . . ?
C24 N4 C25 C26 -156.0(2) . . . . ?
C24 N4 C27 C28 81.6(3) . . . . ?
C24 C16 C17 C18 -176.9(3) . . . . ?
C25 N4 C24 C16 68.4(3) . . . . ?
C25 N4 C27 C28 -156.9(3) . . . . ?
C27 N4 C24 C16 -169.9(3) . . . . ?
C27 N4 C25 C26 83.3(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1 3 24 0.0946 0.9049 2.9089 24.1148 0.1296 0.5470 0.8270
-17 2 16 0.0640 -16.6636 1.6449 16.3275 0.2325 0.9717 0.0422
-13 -2 -18 0.1131 -13.1404 -2.4378 -18.2695 0.0062 0.0191 -0.9998
17 -2 -16 0.0656 16.6809 -1.6418 -16.3046 -0.2325 -0.9717 -0.0409
0 -37 2 0.0049 0.0351 -37.0799 1.7486 -0.9725 0.2328 -0.0092
0 37 -2 0.0115 -0.0351 37.0799 -1.7486 0.9725 -0.2328 0.0092
14 2 17 0.1316 14.0001 2.0000 17.0001 -0.0286 -0.0779 0.9829

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_date_sample_data_collection 18/11/13
_olex2_date_sample_submission    13/11/13
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_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_eb4124
_database_code_depnum_ccdc_archive 'CCDC 1029554'
_audit_update_record             
;
2015-03-27 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
_audit_creation_date             2014-07-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C64 H88 Cu8 N8 O24, 5 C H4 O'
_chemical_formula_sum            'C69 H108 Cu8 N8 O29'
_chemical_formula_weight         2021.95
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C100 H200 Cu8 N20 O30 I'
_chemical_oxdiff_usercomment     '@ 120 K JF3144.2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      cubic
_space_group_IT_number           222
_space_group_name_H-M_alt        'P n -3 n'
_space_group_name_Hall           '-P 4a 2bc 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -z+1/2, y'
'z, x, y'
'-y+1/2, -x+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x+1/2, y, -z+1/2'
'-z+1/2, -x+1/2, y'
'-z+1/2, y, x'
'y, z, x'
'-x+1/2, z, y'
'x, z, -y+1/2'
'y, x, -z+1/2'
'-x+1/2, -y+1/2, z'
'-z+1/2, -y+1/2, -x+1/2'
'y, -x+1/2, z'
'-y+1/2, x, z'
'z, -y+1/2, x'
'-x+1/2, -z+1/2, -y+1/2'
'-y+1/2, -z+1/2, x'
'-z+1/2, x, -y+1/2'
'z, y, -x+1/2'
'z, -x+1/2, -y+1/2'
'y, -z+1/2, -x+1/2'
'-y+1/2, z, -x+1/2'
'-x, -y, -z'
'-x, z-1/2, -y'
'-z, -x, -y'
'y-1/2, x-1/2, z-1/2'
'-x, y-1/2, z-1/2'
'x-1/2, -y, z-1/2'
'z-1/2, x-1/2, -y'
'z-1/2, -y, -x'
'-y, -z, -x'
'x-1/2, -z, -y'
'-x, -z, y-1/2'
'-y, -x, z-1/2'
'x-1/2, y-1/2, -z'
'z-1/2, y-1/2, x-1/2'
'-y, x-1/2, -z'
'y-1/2, -x, -z'
'-z, y-1/2, -x'
'x-1/2, z-1/2, y-1/2'
'y-1/2, z-1/2, -x'
'z-1/2, -x, y-1/2'
'-z, -y, x-1/2'
'-z, x-1/2, y-1/2'
'-y, z-1/2, x-1/2'
'y-1/2, -z, x-1/2'

_cell_length_a                   37.57080(16)
_cell_length_b                   37.57080(16)
_cell_length_c                   37.57080(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     53033.6(7)
_cell_formula_units_Z            24
_cell_measurement_reflns_used    34890
_cell_measurement_temperature    120
_cell_measurement_theta_max      75.3000
_cell_measurement_theta_min      4.0510
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             25008
_exptl_crystal_recrystallization_method 
'Diffusion of MeOH and MeCN solution into THF.'
_exptl_crystal_size_max          0.2369
_exptl_crystal_size_mid          0.1238
_exptl_crystal_size_min          0.0664
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            232108
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.254
_diffrn_reflns_theta_min         3.327
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -50.00   28.00   0.7500    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186   38.0000 -150.0000 104

#__ type_ start__ end____ width___ exp.time_
  2 omega -116.00  -22.25   0.7500    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186  -38.0000   60.0000 125

#__ type_ start__ end____ width___ exp.time_
  3 omega   23.00   98.00   0.7500    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4186 -125.0000    0.0000 100

#__ type_ start__ end____ width___ exp.time_
  4 omega   30.00  108.00   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 104

#__ type_ start__ end____ width___ exp.time_
  5 omega   40.00   97.00   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -30.0000 76

#__ type_ start__ end____ width___ exp.time_
  6 omega   36.00   90.00   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -180.0000 72

#__ type_ start__ end____ width___ exp.time_
  7 omega   83.00  154.25   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 95

#__ type_ start__ end____ width___ exp.time_
  8 omega   99.00  176.25   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000 -120.0000 103

#__ type_ start__ end____ width___ exp.time_
  9 omega   56.00  134.00   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  120.0000 104

#__ type_ start__ end____ width___ exp.time_
 10 omega   53.00   79.25   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000    0.0000 35

#__ type_ start__ end____ width___ exp.time_
 11 omega   89.00  119.00   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0344990000
_diffrn_orient_matrix_UB_12      0.0057930000
_diffrn_orient_matrix_UB_13      -0.0214313000
_diffrn_orient_matrix_UB_21      -0.0022596000
_diffrn_orient_matrix_UB_22      -0.0384530000
_diffrn_orient_matrix_UB_23      -0.0139981000
_diffrn_orient_matrix_UB_31      -0.0221074000
_diffrn_orient_matrix_UB_32      0.0129503000
_diffrn_orient_matrix_UB_33      -0.0320103000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7731
_reflns_number_total             9253
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.266
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         9253
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0467
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0707P)²+79.8921P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1404
_refine_special_details          
;
The SQUEEZE routine of PLATON was used to remove electron density pertaining 
to approximately 5 molecules of solvent methanol per asymmetric unit, which 
could not be modelled with discrete atoms. Both of the acetate ligands show 
large displacement ellipsoids consistent with wagging or twisting of the 
ligand, C32 in particular since in the crystal packing four symmetry-related 
atoms are in close proximity with one another, and this triggers level A 
alerts in checkcif concerning close contacts between H atoms. Displacement 
ellipsoid similarity restraints were used on both 
ligands. O-bound H atoms were located in a difference Fourier map and refined 
as riding with bond distance restraints. C-bound H atoms were placed 
geometrically.





#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
413_ALERT_2_A Short Inter XH3 .. XHn     H32A   ..  H32C    ..       1.61 Ang.
413_ALERT_2_A Short Inter XH3 .. XHn     H32A   ..  H32A    ..       1.81 Ang.
413_ALERT_2_A Short Inter XH3 .. XHn     H32A   ..  H32A    ..       1.81 Ang.
413_ALERT_2_A Short Inter XH3 .. XHn     H32A   ..  H32C    ..       1.31 Ang.
413_ALERT_2_A Short Inter XH3 .. XHn     H32B   ..  H32B    ..       1.27 Ang.
413_ALERT_2_A Short Inter XH3 .. XHn     H32B   ..  H32C    ..       1.64 Ang.
413_ALERT_2_A Short Inter XH3 .. XHn     H32B   ..  H32B    ..       1.27 Ang.

See above. These are all on the methyl C atom of an acetate ligand which is in 
close proximity with symmetry-related ligands.

#===============================================================================
220_ALERT_2_B Large Non-Solvent  C     Ueq(max)/Ueq(min) Range        6.2 Ratio
230_ALERT_2_B Hirshfeld Test Diff for    O11    --  C31     ..       28.0 su
230_ALERT_2_B Hirshfeld Test Diff for    O12    --  C31     ..       32.0 su
241_ALERT_2_B High      Ueq as Compared to Neighbors for .....        O10 Check
242_ALERT_2_B Low       Ueq as Compared to Neighbors for .....        C31 Check

These all pertain to the acetate ligand mentioned above.  Distance and 
displacement ellipsoid restraints were used on this ligand.

#===============================================================================
041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ     Please Check
051_ALERT_1_C Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .       3.30 %
068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...     Please Check

Consequence of SQUEEZE as noted above.

213_ALERT_2_C Atom C31             has ADP max/min Ratio .....        3.2 prolat
220_ALERT_2_C Large Non-Solvent  O     Ueq(max)/Ueq(min) Range        3.5 Ratio
222_ALERT_3_C Large Non-Solvent    H    Uiso(max)/Uiso(min) ..        6.5 Ratio

These pertain to the acetate ligand mentioned above.

230_ALERT_2_C Hirshfeld Test Diff for    C31    --  C32     ..        6.0 su
241_ALERT_2_C High      Ueq as Compared to Neighbors for .....        O11 Check
241_ALERT_2_C High      Ueq as Compared to Neighbors for .....        O12 Check
242_ALERT_2_C Low       Ueq as Compared to Neighbors for .....        Cu2 Check
242_ALERT_2_C Low       Ueq as Compared to Neighbors for .....        Cu4 Check
242_ALERT_2_C Low       Ueq as Compared to Neighbors for .....        C29 Check
414_ALERT_2_C Short Intra D-H..H-X       H4     ..  H14B    ..       1.98 Ang.
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          5 Why ?
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          1 Note
976_ALERT_2_C Check Calcd Residual Density  0.71A From     O11      -0.79 eA-3
976_ALERT_2_C Check Calcd Residual Density  0.68A From     O12      -0.63 eA-3
976_ALERT_2_C Check Calcd Residual Density  0.51A From     O11      -0.49 eA-3

Not actioned.

#===============================================================================



;


# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.003 0.003 8 0 ' '
2 0.750 -0.003 -0.003 8 0 ' '
3 0.659 -0.002 0.128 10171 1340 ' '
4 0.003 0.003 0.250 8 0 ' '
5 0.497 0.003 0.250 8 0 ' '
6 0.250 0.003 0.497 8 0 ' '
7 0.750 -0.003 0.503 8 0 ' '
8 -0.003 -0.003 0.750 8 0 ' '
9 0.503 -0.003 0.750 8 0 ' '
10 0.250 0.250 0.250 1691 324 ' '
11 0.003 0.250 0.003 8 0 ' '
12 0.497 0.250 0.003 8 0 ' '
13 0.003 0.250 0.497 8 0 ' '
14 0.497 0.250 0.497 8 0 ' '
15 0.250 0.497 0.003 8 0 ' '
16 0.003 0.497 0.250 8 0 ' '
17 0.497 0.497 0.250 8 0 ' '
18 0.250 0.497 0.497 8 0 ' '
19 0.750 0.503 -0.003 8 0 ' '
20 0.750 0.503 0.503 8 0 ' '
21 -0.003 0.503 0.750 8 0 ' '
22 0.503 0.503 0.750 8 0 ' '
23 0.750 0.750 0.750 1691 324 ' '
24 -0.003 0.750 -0.003 8 0 ' '
25 0.503 0.750 -0.003 8 0 ' '
26 -0.003 0.750 0.503 8 0 ' '
27 0.503 0.750 0.503 8 0 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
' 5 molecules of solvent methanol per asymmetric unit'



# start Validation Reply Form
_vrf_PLAT413_eb4124              
;
PROBLEM: Short Inter XH3 .. XHn     H32A   ..  H32C    ..       1.61 Ang.  
RESPONSE: Please see the _refine_special_details section of the CIF, which 
discusses this and various other checkCIF alerts.
;
# end Validation Reply Form


_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-H4 = O8-H8
 0.84 with sigma of 0.01
 C32-C31 \\sim C23-C18
 with sigma of 0.02
 O11-C31 \\sim O12-C31 \\sim O9-C29 \\sim O10-C29
 with sigma of 0.02
3. Rigid bond restraints
 C32, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C31 \\sim C32: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C31) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 O11, C31, O12, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O9, C29, O10, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B)
6.b Me refined with riding coordinates:
 C32(H32A,H32B,H32C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.16572(2) 0.47101(2) 0.55983(2) 0.03623(13) Uani 1 1 d . . . . .
Cu2 Cu 0.22825(2) 0.41147(2) 0.56175(2) 0.04081(14) Uani 1 1 d . . . . .
Cu3 Cu 0.30996(2) 0.41290(2) 0.53658(2) 0.04221(14) Uani 1 1 d . . . . .
Cu4 Cu 0.34717(2) 0.48786(2) 0.51748(2) 0.03784(13) Uani 1 1 d . . . . .
O1 O 0.15492(6) 0.51843(6) 0.53893(6) 0.0349(5) Uani 1 1 d . . . . .
O2 O 0.21539(6) 0.54707(7) 0.45518(6) 0.0434(5) Uani 1 1 d . . . . .
O3 O 0.19321(6) 0.43832(7) 0.58665(7) 0.0436(5) Uani 1 1 d . . . . .
O4 O 0.11359(7) 0.44407(7) 0.54650(7) 0.0451(6) Uani 1 1 d D . . . .
H4 H 0.1056(12) 0.4544(11) 0.5283(8) 0.054 Uiso 1 1 d DR . . . .
O5 O 0.26404(6) 0.38607(6) 0.53562(7) 0.0445(6) Uani 1 1 d . . . . .
O6 O 0.18837(6) 0.45910(7) 0.51662(7) 0.0430(5) Uani 1 1 d . . . . .
O7 O 0.34613(6) 0.43764(7) 0.51226(8) 0.0482(6) Uani 1 1 d . . . . .
O8 O 0.32452(8) 0.40071(9) 0.59508(9) 0.0599(7) Uani 1 1 d D . . . .
H8 H 0.3033(5) 0.3998(14) 0.6020(14) 0.072 Uiso 1 1 d DR . . . .
N1 N 0.19620(7) 0.54782(8) 0.48567(7) 0.0369(6) Uani 1 1 d . . . . .
N2 N 0.14072(7) 0.48295(8) 0.60523(8) 0.0403(6) Uani 1 1 d . . . . .
N3 N 0.20762(7) 0.42843(8) 0.51570(8) 0.0387(6) Uani 1 1 d . . . . .
N4 N 0.33754(8) 0.36808(8) 0.52728(10) 0.0509(8) Uani 1 1 d . . . . .
C1 C 0.16806(8) 0.54480(8) 0.55919(9) 0.0348(6) Uani 1 1 d . . . . .
C2 C 0.15557(8) 0.54744(9) 0.59436(9) 0.0376(7) Uani 1 1 d . . . . .
C3 C 0.16596(9) 0.57558(10) 0.61569(10) 0.0432(7) Uani 1 1 d . . . . .
H3 H 0.1571 0.5772 0.6393 0.052 Uiso 1 1 calc R . . . .
C4 C 0.18936(9) 0.60170(10) 0.60288(10) 0.0436(7) Uani 1 1 d . . . . .
C5 C 0.20296(8) 0.59763(9) 0.56910(10) 0.0403(7) Uani 1 1 d . . . . .
H5 H 0.2194 0.6148 0.5606 0.048 Uiso 1 1 calc R . . . .
C6 C 0.19363(8) 0.56915(9) 0.54657(9) 0.0361(6) Uani 1 1 d . . . . .
C7 C 0.21070(8) 0.56579(9) 0.51150(9) 0.0365(7) Uani 1 1 d . . . . .
C8 C 0.24636(9) 0.58276(10) 0.50492(9) 0.0441(8) Uani 1 1 d . . . . .
H8A H 0.2628 0.5650 0.4951 0.066 Uiso 1 1 calc GR . . . .
H8B H 0.2559 0.5920 0.5274 0.066 Uiso 1 1 calc GR . . . .
H8C H 0.2437 0.6024 0.4879 0.066 Uiso 1 1 calc GR . . . .
C9 C 0.19873(12) 0.63359(12) 0.62560(12) 0.0583(10) Uani 1 1 d . . . . .
H9A H 0.1774 0.6481 0.6294 0.087 Uiso 1 1 calc GR . . . .
H9B H 0.2169 0.6479 0.6135 0.087 Uiso 1 1 calc GR . . . .
H9C H 0.2079 0.6255 0.6486 0.087 Uiso 1 1 calc GR . . . .
C10 C 0.12843(9) 0.52071(10) 0.60766(10) 0.0418(7) Uani 1 1 d . . . . .
H10A H 0.1227 0.5262 0.6328 0.050 Uiso 1 1 calc R . . . .
H10B H 0.1063 0.5234 0.5936 0.050 Uiso 1 1 calc R . . . .
C11 C 0.16792(10) 0.47451(11) 0.63269(10) 0.0469(8) Uani 1 1 d . . . . .
H11A H 0.1564 0.4726 0.6563 0.056 Uiso 1 1 calc R . . . .
H11B H 0.1857 0.4939 0.6338 0.056 Uiso 1 1 calc R . . . .
C12 C 0.18651(11) 0.43933(10) 0.62367(10) 0.0502(9) Uani 1 1 d . . . . .
H12A H 0.2092 0.4375 0.6370 0.060 Uiso 1 1 calc R . . . .
H12B H 0.1712 0.4190 0.6306 0.060 Uiso 1 1 calc R . . . .
C13 C 0.10906(11) 0.45907(11) 0.60781(11) 0.0521(9) Uani 1 1 d . . . . .
H13A H 0.0928 0.4682 0.6264 0.062 Uiso 1 1 calc R . . . .
H13B H 0.1169 0.4350 0.6151 0.062 Uiso 1 1 calc R . . . .
C14 C 0.08929(10) 0.45650(11) 0.57305(11) 0.0504(9) Uani 1 1 d . . . . .
H14A H 0.0691 0.4398 0.5754 0.061 Uiso 1 1 calc R . . . .
H14B H 0.0798 0.4801 0.5663 0.061 Uiso 1 1 calc R . . . .
C15 C 0.26099(9) 0.37248(9) 0.50276(11) 0.0446(8) Uani 1 1 d . . . . .
C16 C 0.28589(10) 0.34604(10) 0.49278(13) 0.0518(9) Uani 1 1 d . . . . .
C17 C 0.28320(11) 0.33018(11) 0.45974(14) 0.0610(12) Uani 1 1 d . . . . .
H17 H 0.2995 0.3118 0.4536 0.073 Uiso 1 1 calc R . . . .
C18 C 0.25728(11) 0.34030(12) 0.43517(13) 0.0603(11) Uani 1 1 d . . . . .
C19 C 0.23446(10) 0.36775(11) 0.44466(12) 0.0535(9) Uani 1 1 d . . . . .
H19 H 0.2170 0.3752 0.4280 0.064 Uiso 1 1 calc R . . . .
C20 C 0.23609(9) 0.38503(10) 0.47794(11) 0.0445(8) Uani 1 1 d . . . . .
C21 C 0.21426(9) 0.41699(9) 0.48388(10) 0.0408(7) Uani 1 1 d . . . . .
C22 C 0.20096(11) 0.43898(12) 0.45309(11) 0.0523(9) Uani 1 1 d . . . . .
H22A H 0.1750 0.4372 0.4517 0.078 Uiso 1 1 calc GR . . . .
H22B H 0.2115 0.4301 0.4309 0.078 Uiso 1 1 calc GR . . . .
H22C H 0.2078 0.4639 0.4566 0.078 Uiso 1 1 calc GR . . . .
C23 C 0.25493(15) 0.32278(17) 0.39941(16) 0.0856(17) Uani 1 1 d . . . . .
H23A H 0.2766 0.3279 0.3858 0.128 Uiso 1 1 calc GR . . . .
H23B H 0.2342 0.3320 0.3865 0.128 Uiso 1 1 calc GR . . . .
H23C H 0.2524 0.2970 0.4025 0.128 Uiso 1 1 calc GR . . . .
C24 C 0.31475(11) 0.33681(10) 0.51902(13) 0.0559(10) Uani 1 1 d . . . . .
H24A H 0.3038 0.3279 0.5413 0.067 Uiso 1 1 calc R . . . .
H24B H 0.3297 0.3175 0.5091 0.067 Uiso 1 1 calc R . . . .
C25 C 0.36015(10) 0.37784(11) 0.49639(13) 0.0545(10) Uani 1 1 d . . . . .
H25A H 0.3460 0.3760 0.4742 0.065 Uiso 1 1 calc R . . . .
H25B H 0.3803 0.3609 0.4946 0.065 Uiso 1 1 calc R . . . .
C26 C 0.37452(10) 0.41558(10) 0.50019(12) 0.0505(9) Uani 1 1 d . . . . .
H26A H 0.3944 0.4160 0.5175 0.061 Uiso 1 1 calc R . . . .
H26B H 0.3835 0.4242 0.4770 0.061 Uiso 1 1 calc R . . . .
C27 C 0.35965(11) 0.36151(12) 0.55975(13) 0.0624(11) Uani 1 1 d . . . . .
H27A H 0.3797 0.3786 0.5602 0.075 Uiso 1 1 calc R . . . .
H27B H 0.3698 0.3372 0.5586 0.075 Uiso 1 1 calc R . . . .
C28 C 0.33828(12) 0.36530(13) 0.59328(14) 0.0641(12) Uani 1 1 d . . . . .
H28A H 0.3184 0.3479 0.5933 0.077 Uiso 1 1 calc R . . . .
H28B H 0.3535 0.3605 0.6142 0.077 Uiso 1 1 calc R . . . .
C31 C 0.41206(8) 0.49080(8) 0.50794(8) 0.0331(6) Uani 1 1 d . U . . .
O9 O 0.25267(8) 0.39555(9) 0.60601(8) 0.0619(7) Uani 1 1 d . . . . .
O11 O 0.39102(9) 0.49125(8) 0.48721(9) 0.0630(7) Uani 1 1 d . . . . .
O12 O 0.40988(11) 0.48171(10) 0.53928(11) 0.0815(10) Uani 1 1 d . . . . .
O10 O 0.21340(12) 0.35408(13) 0.60112(17) 0.1226(19) Uani 1 1 d . . . . .
C29 C 0.23882(13) 0.36778(16) 0.61610(18) 0.0884(17) Uani 1 1 d . . . . .
C30 C 0.2540(3) 0.3479(3) 0.6481(3) 0.163(4) Uani 1 1 d . . . . .
H30A H 0.2712 0.3301 0.6399 0.245 Uiso 1 1 calc GR . . . .
H30B H 0.2347 0.3361 0.6610 0.245 Uiso 1 1 calc GR . . . .
H30C H 0.2660 0.3648 0.6640 0.245 Uiso 1 1 calc GR . . . .
C32 C 0.4515(2) 0.4923(4) 0.5010(4) 0.208(6) Uani 1 1 d . U . . .
H32A H 0.4644 0.4915 0.5236 0.311 Uiso 1 1 calc R . . . .
H32B H 0.4586 0.4720 0.4863 0.311 Uiso 1 1 calc R . . . .
H32C H 0.4573 0.5145 0.4885 0.311 Uiso 1 1 calc R . . . .


_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 O1 1.989(2) . ?
Cu1 O3 1.895(2) . ?
Cu1 O4 2.261(3) . ?
Cu1 O6 1.887(2) . ?
Cu1 N2 1.998(3) . ?
Cu2 O3 1.904(2) . ?
Cu2 O5 1.919(3) . ?
Cu2 N3 2.000(3) . ?
Cu2 O9 1.991(3) . ?
Cu3 O2 1.894(2) 10 ?
Cu3 O5 1.998(2) . ?
Cu3 O7 1.883(3) . ?
Cu3 O8 2.311(3) . ?
Cu3 N4 2.008(3) . ?
Cu4 O1 1.921(2) 10 ?
Cu4 O7 1.897(3) . ?
Cu4 N1 1.990(3) 10 ?
Cu4 O11 2.006(3) . ?
O1 Cu4 1.921(2) 10 ?
O1 C1 1.343(4) . ?
O2 Cu3 1.893(2) 10 ?
O2 N1 1.354(4) . ?
O3 C12 1.414(5) . ?
O4 H4 0.841(10) . ?
O4 C14 1.431(4) . ?
O5 C15 1.341(5) . ?
O6 N3 1.361(4) . ?
O7 C26 1.425(4) . ?
O8 H8 0.840(10) . ?
O8 C28 1.429(5) . ?
N1 Cu4 1.990(3) 10 ?
N1 C7 1.302(4) . ?
N2 C10 1.495(5) . ?
N2 C11 1.486(5) . ?
N2 C13 1.493(4) . ?
N3 C21 1.295(5) . ?
N4 C24 1.487(5) . ?
N4 C25 1.484(5) . ?
N4 C27 1.496(6) . ?
C1 C2 1.406(5) . ?
C1 C6 1.409(4) . ?
C2 C3 1.383(5) . ?
C2 C10 1.516(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.403(5) . ?
C4 C5 1.377(5) . ?
C4 C9 1.513(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.409(5) . ?
C6 C7 1.471(5) . ?
C7 C8 1.504(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.533(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.505(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.415(5) . ?
C15 C20 1.403(6) . ?
C16 C17 1.381(7) . ?
C16 C24 1.506(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.395(7) . ?
C18 C19 1.388(6) . ?
C18 C23 1.499(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.410(6) . ?
C20 C21 1.471(5) . ?
C21 C22 1.507(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.524(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.501(7) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C31 O11 1.110(4) . ?
C31 O12 1.229(5) . ?
C31 C32 1.507(8) . ?
O9 C29 1.226(6) . ?
O10 C29 1.223(7) . ?
C29 C30 1.525(8) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O4 97.87(9) . . ?
O1 Cu1 N2 92.29(11) . . ?
O3 Cu1 O1 154.39(11) . . ?
O3 Cu1 O4 107.45(11) . . ?
O3 Cu1 N2 87.02(11) . . ?
O6 Cu1 O1 87.98(10) . . ?
O6 Cu1 O3 93.32(10) . . ?
O6 Cu1 O4 95.40(11) . . ?
O6 Cu1 N2 178.65(12) . . ?
N2 Cu1 O4 83.25(11) . . ?
O3 Cu2 O5 177.74(11) . . ?
O3 Cu2 N3 89.34(11) . . ?
O3 Cu2 O9 93.87(12) . . ?
O5 Cu2 N3 89.27(11) . . ?
O5 Cu2 O9 87.41(12) . . ?
O9 Cu2 N3 175.34(12) . . ?
O2 Cu3 O5 89.59(10) 10 . ?
O2 Cu3 O8 95.01(12) 10 . ?
O2 Cu3 N4 177.90(14) 10 . ?
O5 Cu3 O8 96.98(11) . . ?
O5 Cu3 N4 91.12(12) . . ?
O7 Cu3 O2 92.85(10) . 10 ?
O7 Cu3 O5 149.70(13) . . ?
O7 Cu3 O8 112.85(12) . . ?
O7 Cu3 N4 87.53(12) . . ?
N4 Cu3 O8 82.94(14) . . ?
O1 Cu4 N1 89.84(10) 10 10 ?
O1 Cu4 O11 88.90(11) 10 . ?
O7 Cu4 O1 173.98(11) . 10 ?
O7 Cu4 N1 90.07(11) . 10 ?
O7 Cu4 O11 91.23(12) . . ?
N1 Cu4 O11 178.69(13) 10 . ?
Cu4 O1 Cu1 112.72(11) 10 . ?
C1 O1 Cu1 111.21(19) . . ?
C1 O1 Cu4 126.5(2) . 10 ?
N1 O2 Cu3 116.51(18) . 10 ?
Cu1 O3 Cu2 117.33(13) . . ?
C12 O3 Cu1 114.1(2) . . ?
C12 O3 Cu2 128.4(2) . . ?
Cu1 O4 H4 106(3) . . ?
C14 O4 Cu1 104.6(2) . . ?
C14 O4 H4 101(3) . . ?
Cu2 O5 Cu3 110.18(12) . . ?
C15 O5 Cu2 126.9(2) . . ?
C15 O5 Cu3 106.4(2) . . ?
N3 O6 Cu1 117.5(2) . . ?
Cu3 O7 Cu4 117.10(13) . . ?
C26 O7 Cu3 114.1(2) . . ?
C26 O7 Cu4 126.6(2) . . ?
Cu3 O8 H8 94(4) . . ?
C28 O8 Cu3 103.0(3) . . ?
C28 O8 H8 109(4) . . ?
O2 N1 Cu4 117.3(2) . 10 ?
C7 N1 Cu4 127.5(2) . 10 ?
C7 N1 O2 114.8(3) . . ?
C10 N2 Cu1 114.2(2) . . ?
C11 N2 Cu1 102.8(2) . . ?
C11 N2 C10 111.9(3) . . ?
C11 N2 C13 112.0(3) . . ?
C13 N2 Cu1 107.1(2) . . ?
C13 N2 C10 108.7(3) . . ?
O6 N3 Cu2 117.0(2) . . ?
C21 N3 Cu2 128.2(2) . . ?
C21 N3 O6 114.0(3) . . ?
C24 N4 Cu3 113.7(2) . . ?
C24 N4 C27 111.1(3) . . ?
C25 N4 Cu3 103.0(2) . . ?
C25 N4 C24 111.2(4) . . ?
C25 N4 C27 111.1(3) . . ?
C27 N4 Cu3 106.4(3) . . ?
O1 C1 C2 117.5(3) . . ?
O1 C1 C6 122.6(3) . . ?
C2 C1 C6 119.9(3) . . ?
C1 C2 C10 119.2(3) . . ?
C3 C2 C1 120.3(3) . . ?
C3 C2 C10 120.4(3) . . ?
C2 C3 H3 119.6 . . ?
C2 C3 C4 120.8(3) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C9 120.4(3) . . ?
C5 C4 C3 118.1(3) . . ?
C5 C4 C9 121.5(4) . . ?
C4 C5 H5 118.5 . . ?
C4 C5 C6 123.1(3) . . ?
C6 C5 H5 118.5 . . ?
C1 C6 C7 122.9(3) . . ?
C5 C6 C1 117.4(3) . . ?
C5 C6 C7 119.7(3) . . ?
N1 C7 C6 122.0(3) . . ?
N1 C7 C8 118.0(3) . . ?
C6 C7 C8 120.0(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C2 113.6(3) . . ?
N2 C10 H10A 108.8 . . ?
N2 C10 H10B 108.8 . . ?
C2 C10 H10A 108.8 . . ?
C2 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
N2 C11 H11A 109.6 . . ?
N2 C11 H11B 109.6 . . ?
N2 C11 C12 110.1(3) . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11A 109.6 . . ?
C12 C11 H11B 109.6 . . ?
O3 C12 C11 108.8(3) . . ?
O3 C12 H12A 109.9 . . ?
O3 C12 H12B 109.9 . . ?
C11 C12 H12A 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
N2 C13 H13A 109.2 . . ?
N2 C13 H13B 109.2 . . ?
N2 C13 C14 112.0(3) . . ?
H13A C13 H13B 107.9 . . ?
C14 C13 H13A 109.2 . . ?
C14 C13 H13B 109.2 . . ?
O4 C14 C13 108.1(3) . . ?
O4 C14 H14A 110.1 . . ?
O4 C14 H14B 110.1 . . ?
C13 C14 H14A 110.1 . . ?
C13 C14 H14B 110.1 . . ?
H14A C14 H14B 108.4 . . ?
O5 C15 C16 117.1(4) . . ?
O5 C15 C20 122.7(3) . . ?
C20 C15 C16 120.1(4) . . ?
C15 C16 C24 117.7(4) . . ?
C17 C16 C15 119.5(4) . . ?
C17 C16 C24 122.8(4) . . ?
C16 C17 H17 119.0 . . ?
C16 C17 C18 121.9(4) . . ?
C18 C17 H17 119.0 . . ?
C17 C18 C23 121.0(4) . . ?
C19 C18 C17 117.6(4) . . ?
C19 C18 C23 121.4(5) . . ?
C18 C19 H19 118.5 . . ?
C18 C19 C20 122.9(4) . . ?
C20 C19 H19 118.5 . . ?
C15 C20 C19 117.6(3) . . ?
C15 C20 C21 123.1(3) . . ?
C19 C20 C21 119.1(4) . . ?
N3 C21 C20 121.2(3) . . ?
N3 C21 C22 117.6(3) . . ?
C20 C21 C22 121.1(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 C16 111.7(3) . . ?
N4 C24 H24A 109.3 . . ?
N4 C24 H24B 109.3 . . ?
C16 C24 H24A 109.3 . . ?
C16 C24 H24B 109.3 . . ?
H24A C24 H24B 107.9 . . ?
N4 C25 H25A 109.4 . . ?
N4 C25 H25B 109.4 . . ?
N4 C25 C26 111.1(4) . . ?
H25A C25 H25B 108.0 . . ?
C26 C25 H25A 109.4 . . ?
C26 C25 H25B 109.4 . . ?
O7 C26 C25 107.8(3) . . ?
O7 C26 H26A 110.1 . . ?
O7 C26 H26B 110.1 . . ?
C25 C26 H26A 110.1 . . ?
C25 C26 H26B 110.1 . . ?
H26A C26 H26B 108.5 . . ?
N4 C27 H27A 109.3 . . ?
N4 C27 H27B 109.3 . . ?
N4 C27 C28 111.8(3) . . ?
H27A C27 H27B 107.9 . . ?
C28 C27 H27A 109.3 . . ?
C28 C27 H27B 109.3 . . ?
O8 C28 C27 108.8(4) . . ?
O8 C28 H28A 109.9 . . ?
O8 C28 H28B 109.9 . . ?
C27 C28 H28A 109.9 . . ?
C27 C28 H28B 109.9 . . ?
H28A C28 H28B 108.3 . . ?
O11 C31 O12 129.0(3) . . ?
O11 C31 C32 125.3(6) . . ?
O12 C31 C32 104.1(6) . . ?
C29 O9 Cu2 108.6(4) . . ?
C31 O11 Cu4 100.7(2) . . ?
O9 C29 C30 120.1(6) . . ?
O10 C29 O9 123.2(5) . . ?
O10 C29 C30 116.7(6) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O11 0.841(10) 1.86(2) 2.640(4) 153(5) 10
O8 H8 O9 0.840(10) 1.914(17) 2.738(4) 166(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
Cu1 O1 C1 C2 -60.5(3) . . . . ?
Cu1 O1 C1 C6 119.0(3) . . . . ?
Cu1 O3 C12 C11 -18.1(4) . . . . ?
Cu1 O4 C14 C13 -37.8(3) . . . . ?
Cu1 O6 N3 Cu2 -27.1(3) . . . . ?
Cu1 O6 N3 C21 162.4(2) . . . . ?
Cu1 N2 C10 C2 -42.8(4) . . . . ?
Cu1 N2 C11 C12 -42.7(3) . . . . ?
Cu1 N2 C13 C14 -44.3(4) . . . . ?
Cu2 O3 C12 C11 156.5(2) . . . . ?
Cu2 O5 C15 C16 -161.3(2) . . . . ?
Cu2 O5 C15 C20 22.9(5) . . . . ?
Cu2 N3 C21 C20 8.0(5) . . . . ?
Cu2 N3 C21 C22 -167.9(3) . . . . ?
Cu2 O9 C29 O10 -2.5(8) . . . . ?
Cu2 O9 C29 C30 175.5(6) . . . . ?
Cu3 O2 N1 Cu4 28.1(3) 10 . . 10 ?
Cu3 O2 N1 C7 -158.7(2) 10 . . . ?
Cu3 O5 C15 C16 66.5(3) . . . . ?
Cu3 O5 C15 C20 -109.2(3) . . . . ?
Cu3 O7 C26 C25 24.0(4) . . . . ?
Cu3 O8 C28 C27 38.2(4) . . . . ?
Cu3 N4 C24 C16 45.2(4) . . . . ?
Cu3 N4 C25 C26 40.2(4) . . . . ?
Cu3 N4 C27 C28 47.0(4) . . . . ?
Cu4 O1 C1 C2 156.1(2) 10 . . . ?
Cu4 O1 C1 C6 -24.4(4) 10 . . . ?
Cu4 O7 C26 C25 -173.7(3) . . . . ?
Cu4 N1 C7 C6 -7.1(5) 10 . . . ?
Cu4 N1 C7 C8 171.6(2) 10 . . . ?
O1 Cu1 O3 Cu2 -91.1(3) . . . . ?
O1 Cu1 O3 C12 84.1(3) . . . . ?
O1 Cu1 O6 N3 170.2(2) . . . . ?
O1 C1 C2 C3 -175.0(3) . . . . ?
O1 C1 C2 C10 0.3(4) . . . . ?
O1 C1 C6 C5 174.2(3) . . . . ?
O1 C1 C6 C7 -6.2(5) . . . . ?
O2 Cu3 O7 Cu4 12.47(17) 10 . . . ?
O2 Cu3 O7 C26 176.5(3) 10 . . . ?
O2 N1 C7 C6 -179.5(3) . . . . ?
O2 N1 C7 C8 -0.8(4) . . . . ?
O3 Cu1 O6 N3 15.8(2) . . . . ?
O4 Cu1 O3 Cu2 97.82(15) . . . . ?
O4 Cu1 O3 C12 -86.9(3) . . . . ?
O4 Cu1 O6 N3 -92.1(2) . . . . ?
O5 Cu3 O7 Cu4 106.5(2) . . . . ?
O5 Cu3 O7 C26 -89.4(3) . . . . ?
O5 C15 C16 C17 177.6(3) . . . . ?
O5 C15 C16 C24 -3.2(5) . . . . ?
O5 C15 C20 C19 -177.7(3) . . . . ?
O5 C15 C20 C21 8.0(5) . . . . ?
O6 Cu1 O3 Cu2 1.10(16) . . . . ?
O6 Cu1 O3 C12 176.4(3) . . . . ?
O6 N3 C21 C20 177.3(3) . . . . ?
O6 N3 C21 C22 1.4(4) . . . . ?
O8 Cu3 O7 Cu4 -84.18(17) . . . . ?
O8 Cu3 O7 C26 79.9(3) . . . . ?
N1 Cu4 O7 Cu3 -1.81(17) 10 . . . ?
N1 Cu4 O7 C26 -163.6(3) 10 . . . ?
N2 Cu1 O3 Cu2 179.79(16) . . . . ?
N2 Cu1 O3 C12 -5.0(3) . . . . ?
N2 C11 C12 O3 41.6(4) . . . . ?
N2 C13 C14 O4 57.5(4) . . . . ?
N4 Cu3 O7 Cu4 -165.46(18) . . . . ?
N4 Cu3 O7 C26 -1.4(3) . . . . ?
N4 C25 C26 O7 -43.6(5) . . . . ?
N4 C27 C28 O8 -60.3(5) . . . . ?
C1 C2 C3 C4 -0.7(5) . . . . ?
C1 C2 C10 N2 58.1(4) . . . . ?
C1 C6 C7 N1 22.3(5) . . . . ?
C1 C6 C7 C8 -156.4(3) . . . . ?
C2 C1 C6 C5 -6.3(4) . . . . ?
C2 C1 C6 C7 173.3(3) . . . . ?
C2 C3 C4 C5 -3.0(5) . . . . ?
C2 C3 C4 C9 176.1(4) . . . . ?
C3 C2 C10 N2 -126.6(3) . . . . ?
C3 C4 C5 C6 2.0(5) . . . . ?
C4 C5 C6 C1 2.6(5) . . . . ?
C4 C5 C6 C7 -177.0(3) . . . . ?
C5 C6 C7 N1 -158.1(3) . . . . ?
C5 C6 C7 C8 23.2(5) . . . . ?
C6 C1 C2 C3 5.5(5) . . . . ?
C6 C1 C2 C10 -179.2(3) . . . . ?
C9 C4 C5 C6 -177.1(3) . . . . ?
C10 N2 C11 C12 -165.7(3) . . . . ?
C10 N2 C13 C14 79.6(4) . . . . ?
C10 C2 C3 C4 -176.0(3) . . . . ?
C11 N2 C10 C2 73.5(4) . . . . ?
C11 N2 C13 C14 -156.3(3) . . . . ?
C13 N2 C10 C2 -162.4(3) . . . . ?
C13 N2 C11 C12 72.0(4) . . . . ?
C15 C16 C17 C18 2.3(6) . . . . ?
C15 C16 C24 N4 -60.9(5) . . . . ?
C15 C20 C21 N3 -23.7(5) . . . . ?
C15 C20 C21 C22 152.1(4) . . . . ?
C16 C15 C20 C19 6.7(5) . . . . ?
C16 C15 C20 C21 -167.6(3) . . . . ?
C16 C17 C18 C19 1.5(6) . . . . ?
C16 C17 C18 C23 179.8(4) . . . . ?
C17 C16 C24 N4 118.3(4) . . . . ?
C17 C18 C19 C20 -1.2(6) . . . . ?
C18 C19 C20 C15 -2.9(6) . . . . ?
C18 C19 C20 C21 171.6(4) . . . . ?
C19 C20 C21 N3 162.1(3) . . . . ?
C19 C20 C21 C22 -22.1(5) . . . . ?
C20 C15 C16 C17 -6.5(6) . . . . ?
C20 C15 C16 C24 172.7(3) . . . . ?
C23 C18 C19 C20 -179.5(4) . . . . ?
C24 N4 C25 C26 162.3(3) . . . . ?
C24 N4 C27 C28 -77.2(4) . . . . ?
C24 C16 C17 C18 -176.9(4) . . . . ?
C25 N4 C24 C16 -70.4(4) . . . . ?
C25 N4 C27 C28 158.4(4) . . . . ?
C27 N4 C24 C16 165.3(3) . . . . ?
C27 N4 C25 C26 -73.4(4) . . . . ?
O11 Cu4 O7 Cu3 177.97(18) . . . . ?
O11 Cu4 O7 C26 16.2(3) . . . . ?
O12 C31 O11 Cu4 16.3(5) . . . . ?
C32 C31 O11 Cu4 179.4(8) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-21 -6 -10 0.0417 -21.3925 -6.4667 -9.7297 -0.5670 0.4332 0.7006
1 -16 18 0.0751 0.7524 -15.9802 18.4173 -0.4613 0.3550 -0.8131
20 14 0 0.0410 19.9983 13.9329 0.2990 0.7642 -0.5851 -0.2712
13 -5 -20 0.0223 12.5716 -5.2001 -20.2451 0.8375 0.4549 0.3028
-20 10 10 0.0374 -20.1225 9.6215 9.8451 -0.8495 -0.4623 0.2543
-16 7 17 0.0395 -16.0756 7.1678 16.8801 -0.8748 -0.4756 -0.0921
13 -8 19 0.0885 12.9520 -7.6620 19.1937 -0.0089 -0.0033 -1.0000
15 -7 -18 0.0216 15.0187 -6.5648 -18.0597 0.8671 0.4713 0.1611
5 19 15 0.0420 5.0031 18.9981 15.0013 -0.0388 -0.9518 -0.3448

_olex2_exptl_crystal_mounting_method 'Mitegen tip, Paratone oil.'
_olex2_submission_original_sample_id JF3144.2
_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_6
_database_code_depnum_ccdc_archive 'CCDC 1029555'
_audit_update_record             
;
2014-10-16 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
# local name eb4168
_audit_creation_date             2014-08-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4862)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H84 Cl4 Cu8 N8 O16, 4(C2 H5 O0.5)'
_chemical_formula_sum            'C68 H104 Cl4 Cu8 N8 O18'
_chemical_formula_weight         1971.71
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N8 O20 Cu I'
_chemical_oxdiff_usercomment     '@ 200 K JF3243.1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   15.74110(10)
_cell_length_b                   20.12890(10)
_cell_length_c                   51.7316(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.2820(10)
_cell_angle_gamma                90
_cell_volume                     16364.3(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    77684
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      75.9440
_cell_measurement_theta_min      3.8530
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.997
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             8096
_exptl_crystal_size_max          0.1101
_exptl_crystal_size_mid          0.0934
_exptl_crystal_size_min          0.0377
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            200377
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.197
_diffrn_reflns_theta_min         3.378
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -70.00   27.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   57.0000    0.0000 97

#__ type_ start__ end____ width___ exp.time_
  2 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000 -180.0000 79

#__ type_ start__ end____ width___ exp.time_
  3 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000 -150.0000 79

#__ type_ start__ end____ width___ exp.time_
  4 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  -90.0000 79

#__ type_ start__ end____ width___ exp.time_
  5 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000   90.0000 79

#__ type_ start__ end____ width___ exp.time_
  6 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  120.0000 79

#__ type_ start__ end____ width___ exp.time_
  7 omega -111.00  -16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  152.0000   63.9967 95

#__ type_ start__ end____ width___ exp.time_
  8 omega   23.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -125.0000    0.0000 75

#__ type_ start__ end____ width___ exp.time_
  9 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  150.0000 55

#__ type_ start__ end____ width___ exp.time_
 10 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   30.0000 82

#__ type_ start__ end____ width___ exp.time_
 11 omega   99.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  115.0000  161.0000 79

#__ type_ start__ end____ width___ exp.time_
 12 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 79

#__ type_ start__ end____ width___ exp.time_
 13 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   30.0000 55

#__ type_ start__ end____ width___ exp.time_
 14 omega   24.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000    0.0000 -180.0000 154

#__ type_ start__ end____ width___ exp.time_
 15 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 82

#__ type_ start__ end____ width___ exp.time_
 16 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -30.0000 55

#__ type_ start__ end____ width___ exp.time_
 17 omega   40.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 58

#__ type_ start__ end____ width___ exp.time_
 18 omega   37.00  142.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000   90.0000 105

#__ type_ start__ end____ width___ exp.time_
 19 omega   40.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  150.0000 58

#__ type_ start__ end____ width___ exp.time_
 20 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -150.0000 55

#__ type_ start__ end____ width___ exp.time_
 21 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   90.0000 55

#__ type_ start__ end____ width___ exp.time_
 22 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 82

#__ type_ start__ end____ width___ exp.time_
 23 omega   94.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
 24 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  120.0000 82

#__ type_ start__ end____ width___ exp.time_
 25 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   90.0000 91

#__ type_ start__ end____ width___ exp.time_
 26 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 79

#__ type_ start__ end____ width___ exp.time_
 27 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 79

#__ type_ start__ end____ width___ exp.time_
 28 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 82

#__ type_ start__ end____ width___ exp.time_
 29 omega   80.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   76.0000  142.7898 98

#__ type_ start__ end____ width___ exp.time_
 30 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -150.0000 82

#__ type_ start__ end____ width___ exp.time_
 31 omega   41.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  -60.0000 98

#__ type_ start__ end____ width___ exp.time_
 32 omega   31.00  156.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000 -180.0000 125

#__ type_ start__ end____ width___ exp.time_
 33 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -120.0000 55

#__ type_ start__ end____ width___ exp.time_
 34 omega   40.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -30.0000 58

#__ type_ start__ end____ width___ exp.time_
 35 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 79

#__ type_ start__ end____ width___ exp.time_
 36 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -123.0000  -27.4213 82

#__ type_ start__ end____ width___ exp.time_
 37 omega -113.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000   60.0000 96

#__ type_ start__ end____ width___ exp.time_
 38 omega -113.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000  -30.0000 96

#__ type_ start__ end____ width___ exp.time_
 39 omega -117.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000  150.0000 105

#__ type_ start__ end____ width___ exp.time_
 40 omega -113.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000 -120.0000 96

#__ type_ start__ end____ width___ exp.time_
 41 omega -117.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000 -120.0000 105

#__ type_ start__ end____ width___ exp.time_
 42 omega -117.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000   60.0000 105

#__ type_ start__ end____ width___ exp.time_
 43 omega   11.00   46.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686   81.0000  -86.8446 35

#__ type_ start__ end____ width___ exp.time_
 44 omega   83.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -158.7046 95

#__ type_ start__ end____ width___ exp.time_
 45 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000    0.0000 91

#__ type_ start__ end____ width___ exp.time_
 46 omega   83.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 48

#__ type_ start__ end____ width___ exp.time_
 47 omega   66.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  -60.0000 112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0092388000
_diffrn_orient_matrix_UB_12      0.0060544000
_diffrn_orient_matrix_UB_13      0.0297170000
_diffrn_orient_matrix_UB_21      -0.0848032000
_diffrn_orient_matrix_UB_22      0.0382413000
_diffrn_orient_matrix_UB_23      -0.0002214000
_diffrn_orient_matrix_UB_31      -0.0482758000
_diffrn_orient_matrix_UB_32      -0.0660251000
_diffrn_orient_matrix_UB_33      0.0025985000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15363
_reflns_number_total             17064
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_refine_diff_density_max         1.913
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         17064
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0588
_refine_ls_restrained_S_all      1.138
_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)+(0.0564P)²+128.6241P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1580
_refine_special_details          
;
Three molecules of ether of crystallization were identified. One (containing 
O18) lies entirely in general positions, the other two lie on crystallographic 
twofold rotation axes.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.33 Why ?
216_ALERT_3_C Disordered C64     (An/Solv) ADP max/min Ratio          6.3

Disordered over twofold axis.

241_ALERT_2_C High      Ueq as Compared to Neighbors for .....        O16 Check
243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors of         C69 Check

Ether of crystallization showing high thermal motion.

341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0080 Ang.
413_ALERT_2_C Short Inter XH3 .. XHn     H11A   ..  H64B    ..       2.09 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......      6.706 Check
971_ALERT_2_C Check Calcd Residual Density  1.17A From     Cl4       2.09 eA-3

Cannot be modelled as anything chemically sensible.

#===============================================================================


;


_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O8-H8 = O4-H4
 0.84 with sigma of 0.02
 O12-H12
 0.84 with sigma of 0.02
 O16-H16
 0.84 with sigma of 0.02
 C68-C67 \\sim C66-C65 \\sim C64-C63 \\sim C62-C61 \\sim C69-C70
 with sigma of 0.02
 O18-C67 \\sim O18-C66 \\sim O17-C63 \\sim O17-C62 \\sim O19-C69
 with sigma of 0.02
3. Rigid bond restraints
 C69, O19, C69, C70
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Rigid body (RIGU) restrains
 C68, C67, O18, C66, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C70, C69, O19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C64, C63, O17, C62, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O17(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) C62(0.5) H62A(0.5)
 H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
  C29(H29A,H29B), C30(H30A,H30B), C38(H38A,H38B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C53(H53A,H53B),
 C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B),
  C69(H69A,H69B), C62(H62A,H62B), C63(H63A,H63B), C66(H66A,H66B), C67(H67A,H67B)
6.b Me refined with riding coordinates:
 C25(H25A,H25B,H25C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C18(H18), C20(H20), C33(H33), C35(H35), C48(H48), C50(H50)
6.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C24(H24A,H24B,H24C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C70(H70A,
 H70B,H70C), C61(H61A,H61B,H61C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C),
 C68(H68A,H68B,H68C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.64511(4) 0.63966(3) 0.43139(2) 0.03630(16) Uani 1 1 d . . . . .
Cu2 Cu 0.85608(4) 0.62460(4) 0.43294(2) 0.03677(16) Uani 1 1 d . . . . .
Cu3 Cu 0.96278(4) 0.64054(3) 0.38090(2) 0.03371(15) Uani 1 1 d . . . . .
Cu4 Cu 0.96675(4) 0.75241(3) 0.33261(2) 0.03092(15) Uani 1 1 d . . . . .
Cu5 Cu 0.85878(4) 0.89073(3) 0.33198(2) 0.02923(14) Uani 1 1 d . . . . .
Cu6 Cu 0.65630(4) 0.92687(3) 0.34299(2) 0.02960(14) Uani 1 1 d . . . . .
Cu7 Cu 0.51025(4) 0.81493(3) 0.34959(2) 0.03537(16) Uani 1 1 d . . . . .
Cu8 Cu 0.50028(4) 0.67866(3) 0.38637(2) 0.03350(15) Uani 1 1 d . . . . .
Cl1 Cl 0.64346(9) 0.54293(7) 0.45542(3) 0.0496(3) Uani 1 1 d . . . . .
Cl2 Cl 1.10575(8) 0.64673(8) 0.38079(3) 0.0530(3) Uani 1 1 d . . . . .
Cl3 Cl 0.84912(8) 0.96262(7) 0.29846(2) 0.0462(3) Uani 1 1 d . . . . .
Cl4 Cl 0.37100(10) 0.83564(8) 0.35522(5) 0.0773(6) Uani 1 1 d . . . . .
O1 O 0.7521(2) 0.66312(16) 0.44832(6) 0.0358(7) Uani 1 1 d . . . . .
O2 O 0.5797(2) 0.74415(17) 0.39688(7) 0.0417(8) Uani 1 1 d . . . . .
O3 O 0.9618(2) 0.6337(2) 0.41752(7) 0.0443(8) Uani 1 1 d . . . . .
O4 O 0.8341(3) 0.5128(2) 0.44579(8) 0.0539(10) Uani 1 1 d D . . . .
H4 H 0.7811(15) 0.520(4) 0.4449(14) 0.065 Uiso 1 1 d DR . . . .
O5 O 0.9557(2) 0.65846(15) 0.34449(6) 0.0339(7) Uani 1 1 d . . . . .
O6 O 0.7950(2) 0.6206(2) 0.40061(7) 0.0436(8) Uani 1 1 d . . . . .
O7 O 0.9232(2) 0.82780(16) 0.31396(6) 0.0357(7) Uani 1 1 d . . . . .
O8 O 1.1118(2) 0.7689(2) 0.34571(8) 0.0455(8) Uani 1 1 d D . . . .
H8 H 1.111(4) 0.741(3) 0.3579(9) 0.055 Uiso 1 1 d DR . . . .
O9 O 0.78008(19) 0.94161(15) 0.35048(6) 0.0322(6) Uani 1 1 d . . . . .
O10 O 0.9246(2) 0.78120(16) 0.36387(6) 0.0370(7) Uani 1 1 d . . . . .
O11 O 0.5454(2) 0.90439(15) 0.35286(7) 0.0365(7) Uani 1 1 d . . . . .
O12 O 0.6542(2) 0.9711(2) 0.29976(8) 0.0473(9) Uani 1 1 d D . . . .
H12 H 0.7053(18) 0.963(3) 0.2969(13) 0.057 Uiso 1 1 d DR . . . .
O13 O 0.4894(2) 0.72155(15) 0.35164(6) 0.0341(7) Uani 1 1 d . . . . .
O14 O 0.68112(19) 0.83916(16) 0.33365(7) 0.0366(7) Uani 1 1 d . . . . .
O15 O 0.5474(2) 0.61543(17) 0.41013(7) 0.0432(8) Uani 1 1 d . . . . .
O16 O 0.3830(3) 0.7366(2) 0.40209(11) 0.0642(12) Uani 1 1 d D . . . .
H16 H 0.395(5) 0.772(2) 0.3939(14) 0.077 Uiso 1 1 d DR . . . .
N1 N 0.6343(2) 0.7329(2) 0.41773(8) 0.0344(8) Uani 1 1 d . . . . .
N2 N 0.9217(3) 0.6255(2) 0.46732(8) 0.0420(9) Uani 1 1 d . . . . .
N3 N 0.8387(3) 0.6173(2) 0.37872(8) 0.0354(8) Uani 1 1 d . . . . .
N4 N 1.0196(2) 0.7256(2) 0.29994(8) 0.0348(8) Uani 1 1 d . . . . .
N5 N 0.8935(2) 0.84403(18) 0.36497(7) 0.0309(8) Uani 1 1 d . . . . .
N6 N 0.6272(2) 1.02123(18) 0.35014(8) 0.0349(8) Uani 1 1 d . . . . .
N7 N 0.6162(2) 0.79482(18) 0.33185(8) 0.0319(8) Uani 1 1 d . . . . .
N8 N 0.4091(2) 0.6125(2) 0.37686(8) 0.0372(9) Uani 1 1 d . . . . .
C1 C 0.7736(3) 0.7230(2) 0.45797(9) 0.0349(10) Uani 1 1 d . . . . .
C2 C 0.8377(3) 0.7249(3) 0.47818(9) 0.0386(10) Uani 1 1 d . . . . .
C3 C 0.8643(3) 0.7853(3) 0.48859(9) 0.0413(11) Uani 1 1 d . . . . .
H3 H 0.9076 0.7860 0.5022 0.050 Uiso 1 1 calc R . . . .
C4 C 0.8294(3) 0.8449(3) 0.47973(9) 0.0394(11) Uani 1 1 d . . . . .
C5 C 0.7667(3) 0.8425(2) 0.45990(9) 0.0365(10) Uani 1 1 d . . . . .
H5 H 0.7420 0.8831 0.4538 0.044 Uiso 1 1 calc R . . . .
C6 C 0.7377(3) 0.7829(2) 0.44837(9) 0.0330(9) Uani 1 1 d . . . . .
C7 C 0.6746(3) 0.7858(2) 0.42610(9) 0.0330(9) Uani 1 1 d . . . . .
C8 C 0.6531(3) 0.8513(2) 0.41350(10) 0.0399(11) Uani 1 1 d . . . . .
H8A H 0.6432 0.8449 0.3946 0.048 Uiso 1 1 calc R . . . .
H8B H 0.7016 0.8822 0.4164 0.048 Uiso 1 1 calc R . . . .
C9 C 0.5746(4) 0.8813(3) 0.42430(13) 0.0562(15) Uani 1 1 d . . . . .
H9A H 0.5251 0.8535 0.4195 0.084 Uiso 1 1 calc GR . . . .
H9B H 0.5655 0.9260 0.4172 0.084 Uiso 1 1 calc GR . . . .
H9C H 0.5823 0.8838 0.4432 0.084 Uiso 1 1 calc GR . . . .
C10 C 0.8601(4) 0.9105(3) 0.49098(11) 0.0516(13) Uani 1 1 d . . . . .
H10A H 0.8543 0.9105 0.5097 0.077 Uiso 1 1 calc GR . . . .
H10B H 0.8260 0.9467 0.4831 0.077 Uiso 1 1 calc GR . . . .
H10C H 0.9200 0.9170 0.4874 0.077 Uiso 1 1 calc GR . . . .
C11 C 0.8749(3) 0.6603(3) 0.48779(10) 0.0437(11) Uani 1 1 d . . . . .
H11A H 0.9145 0.6688 0.5030 0.052 Uiso 1 1 calc R . . . .
H11B H 0.8287 0.6312 0.4934 0.052 Uiso 1 1 calc R . . . .
C12 C 1.0001(3) 0.6611(3) 0.46144(10) 0.0465(12) Uani 1 1 d . . . . .
H12A H 1.0442 0.6537 0.4756 0.056 Uiso 1 1 calc R . . . .
H12B H 0.9883 0.7094 0.4603 0.056 Uiso 1 1 calc R . . . .
C13 C 1.0328(3) 0.6370(3) 0.43590(10) 0.0467(12) Uani 1 1 d . . . . .
H13A H 1.0761 0.6681 0.4298 0.056 Uiso 1 1 calc R . . . .
H13B H 1.0592 0.5926 0.4382 0.056 Uiso 1 1 calc R . . . .
C14 C 0.9420(4) 0.5559(3) 0.47558(12) 0.0520(14) Uani 1 1 d . . . . .
H14A H 0.9633 0.5559 0.4940 0.062 Uiso 1 1 calc R . . . .
H14B H 0.9875 0.5382 0.4651 0.062 Uiso 1 1 calc R . . . .
C15 C 0.8650(4) 0.5118(3) 0.47241(12) 0.0562(15) Uani 1 1 d . . . . .
H15A H 0.8802 0.4659 0.4777 0.067 Uiso 1 1 calc R . . . .
H15B H 0.8201 0.5279 0.4835 0.067 Uiso 1 1 calc R . . . .
C16 C 0.9068(3) 0.6241(2) 0.32686(9) 0.0328(9) Uani 1 1 d . . . . .
C17 C 0.9349(3) 0.6213(2) 0.30149(9) 0.0357(10) Uani 1 1 d . . . . .
C18 C 0.8858(3) 0.5884(3) 0.28229(10) 0.0405(11) Uani 1 1 d . . . . .
H18 H 0.9040 0.5877 0.2651 0.049 Uiso 1 1 calc R . . . .
C19 C 0.8103(3) 0.5563(3) 0.28777(10) 0.0422(11) Uani 1 1 d . . . . .
C20 C 0.7838(3) 0.5602(3) 0.31279(10) 0.0398(10) Uani 1 1 d . . . . .
H20 H 0.7328 0.5382 0.3168 0.048 Uiso 1 1 calc R . . . .
C21 C 0.8293(3) 0.5955(2) 0.33259(9) 0.0340(9) Uani 1 1 d . . . . .
C22 C 0.7921(3) 0.6019(2) 0.35805(9) 0.0330(9) Uani 1 1 d . . . . .
C23 C 0.6986(3) 0.5890(3) 0.36015(10) 0.0406(11) Uani 1 1 d . . . . .
H23A H 0.6685 0.5954 0.3430 0.049 Uiso 1 1 calc R . . . .
H23B H 0.6753 0.6212 0.3723 0.049 Uiso 1 1 calc R . . . .
C24 C 0.6830(4) 0.5183(3) 0.36965(13) 0.0537(14) Uani 1 1 d . . . . .
H24A H 0.7066 0.4863 0.3577 0.080 Uiso 1 1 calc GR . . . .
H24B H 0.6216 0.5107 0.3704 0.080 Uiso 1 1 calc GR . . . .
H24C H 0.7107 0.5125 0.3870 0.080 Uiso 1 1 calc GR . . . .
C25 C 0.7615(4) 0.5178(4) 0.26678(13) 0.0661(18) Uani 1 1 d . . . . .
H25A H 0.7907 0.5213 0.2506 0.099 Uiso 1 1 calc R . . . .
H25B H 0.7581 0.4710 0.2719 0.099 Uiso 1 1 calc R . . . .
H25C H 0.7039 0.5361 0.2642 0.099 Uiso 1 1 calc R . . . .
C26 C 1.0187(3) 0.6519(2) 0.29616(10) 0.0394(11) Uani 1 1 d . . . . .
H26A H 1.0321 0.6418 0.2781 0.047 Uiso 1 1 calc R . . . .
H26B H 1.0637 0.6317 0.3078 0.047 Uiso 1 1 calc R . . . .
C27 C 0.9642(3) 0.7583(2) 0.27949(9) 0.0369(10) Uani 1 1 d . . . . .
H27A H 0.9109 0.7326 0.2765 0.044 Uiso 1 1 calc R . . . .
H27B H 0.9936 0.7593 0.2631 0.044 Uiso 1 1 calc R . . . .
C28 C 0.9435(3) 0.8288(2) 0.28760(9) 0.0359(10) Uani 1 1 d . . . . .
H28A H 0.9929 0.8582 0.2854 0.043 Uiso 1 1 calc R . . . .
H28B H 0.8946 0.8460 0.2767 0.043 Uiso 1 1 calc R . . . .
C29 C 1.1086(3) 0.7513(3) 0.29999(10) 0.0433(11) Uani 1 1 d . . . . .
H29A H 1.1072 0.7995 0.2962 0.052 Uiso 1 1 calc R . . . .
H29B H 1.1387 0.7289 0.2861 0.052 Uiso 1 1 calc R . . . .
C30 C 1.1575(3) 0.7399(3) 0.32586(11) 0.0467(12) Uani 1 1 d . . . . .
H30A H 1.1644 0.6916 0.3291 0.056 Uiso 1 1 calc R . . . .
H30B H 1.2147 0.7601 0.3256 0.056 Uiso 1 1 calc R . . . .
C31 C 0.7976(3) 0.9662(2) 0.37421(9) 0.0316(9) Uani 1 1 d . . . . .
C32 C 0.7577(3) 1.0263(2) 0.38084(10) 0.0350(10) Uani 1 1 d . . . . .
C33 C 0.7783(3) 1.0555(2) 0.40455(10) 0.0407(11) Uani 1 1 d . . . . .
H33 H 0.7508 1.0956 0.4089 0.049 Uiso 1 1 calc R . . . .
C34 C 0.8383(3) 1.0278(3) 0.42229(10) 0.0425(11) Uani 1 1 d . . . . .
C35 C 0.8738(3) 0.9673(3) 0.41607(9) 0.0377(10) Uani 1 1 d . . . . .
H35 H 0.9135 0.9473 0.4282 0.045 Uiso 1 1 calc R . . . .
C36 C 0.8535(3) 0.9339(2) 0.39245(9) 0.0328(9) Uani 1 1 d . . . . .
C37 C 0.8888(3) 0.8677(2) 0.38832(8) 0.0307(9) Uani 1 1 d . . . . .
C38 C 0.9212(3) 0.8255(3) 0.41095(9) 0.0391(11) Uani 1 1 d . . . . .
H38A H 0.9015 0.7791 0.4082 0.047 Uiso 1 1 calc R . . . .
H38B H 0.8971 0.8421 0.4270 0.047 Uiso 1 1 calc R . . . .
C39 C 1.0195(4) 0.8265(3) 0.41429(11) 0.0537(14) Uani 1 1 d . . . . .
H39A H 1.0435 0.8102 0.3984 0.081 Uiso 1 1 calc GR . . . .
H39B H 1.0383 0.7978 0.4288 0.081 Uiso 1 1 calc GR . . . .
H39C H 1.0390 0.8720 0.4177 0.081 Uiso 1 1 calc GR . . . .
C40 C 0.8659(4) 1.0633(3) 0.44722(12) 0.0579(15) Uani 1 1 d . . . . .
H40A H 0.8693 1.1111 0.4440 0.087 Uiso 1 1 calc GR . . . .
H40B H 0.9219 1.0468 0.4535 0.087 Uiso 1 1 calc GR . . . .
H40C H 0.8244 1.0548 0.4602 0.087 Uiso 1 1 calc GR . . . .
C41 C 0.7018(3) 1.0613(2) 0.36073(11) 0.0393(11) Uani 1 1 d . . . . .
H41A H 0.7368 1.0740 0.3462 0.047 Uiso 1 1 calc R . . . .
H41B H 0.6803 1.1027 0.3684 0.047 Uiso 1 1 calc R . . . .
C42 C 0.5609(3) 1.0147(2) 0.36948(11) 0.0386(11) Uani 1 1 d . . . . .
H42A H 0.5298 1.0572 0.3708 0.046 Uiso 1 1 calc R . . . .
H42B H 0.5883 1.0044 0.3867 0.046 Uiso 1 1 calc R . . . .
C43 C 0.4985(3) 0.9596(2) 0.36145(10) 0.0376(10) Uani 1 1 d . . . . .
H43A H 0.4653 0.9466 0.3763 0.045 Uiso 1 1 calc R . . . .
H43B H 0.4584 0.9754 0.3473 0.045 Uiso 1 1 calc R . . . .
C44 C 0.5898(3) 1.0523(3) 0.32597(11) 0.0421(11) Uani 1 1 d . . . . .
H44A H 0.5837 1.1007 0.3287 0.051 Uiso 1 1 calc R . . . .
H44B H 0.5324 1.0337 0.3219 0.051 Uiso 1 1 calc R . . . .
C45 C 0.6443(4) 1.0407(3) 0.30327(11) 0.0462(12) Uani 1 1 d . . . . .
H45A H 0.6168 1.0607 0.2874 0.055 Uiso 1 1 calc R . . . .
H45B H 0.7006 1.0618 0.3066 0.055 Uiso 1 1 calc R . . . .
C46 C 0.5034(3) 0.6788(2) 0.33256(9) 0.0321(9) Uani 1 1 d . . . . .
C47 C 0.4517(3) 0.6212(2) 0.33089(9) 0.0339(9) Uani 1 1 d . . . . .
C48 C 0.4617(3) 0.5766(2) 0.31097(10) 0.0382(10) Uani 1 1 d . . . . .
H48 H 0.4276 0.5376 0.3101 0.046 Uiso 1 1 calc R . . . .
C49 C 0.5208(3) 0.5870(2) 0.29207(10) 0.0392(10) Uani 1 1 d . . . . .
C50 C 0.5724(3) 0.6424(2) 0.29467(10) 0.0351(10) Uani 1 1 d . . . . .
H50 H 0.6133 0.6499 0.2822 0.042 Uiso 1 1 calc R . . . .
C51 C 0.5671(3) 0.6885(2) 0.31514(9) 0.0305(9) Uani 1 1 d . . . . .
C52 C 0.6299(3) 0.7426(2) 0.31781(9) 0.0312(9) Uani 1 1 d . . . . .
C53 C 0.7120(3) 0.7388(2) 0.30424(10) 0.0394(11) Uani 1 1 d . . . . .
H53A H 0.7225 0.6923 0.2991 0.047 Uiso 1 1 calc R . . . .
H53B H 0.7598 0.7530 0.3162 0.047 Uiso 1 1 calc R . . . .
C54 C 0.7078(4) 0.7834(3) 0.28019(11) 0.0528(14) Uani 1 1 d . . . . .
H54A H 0.6609 0.7689 0.2682 0.079 Uiso 1 1 calc GR . . . .
H54B H 0.7616 0.7803 0.2716 0.079 Uiso 1 1 calc GR . . . .
H54C H 0.6984 0.8295 0.2854 0.079 Uiso 1 1 calc GR . . . .
C55 C 0.5264(4) 0.5401(3) 0.26959(11) 0.0504(13) Uani 1 1 d . . . . .
H55A H 0.5465 0.4966 0.2759 0.076 Uiso 1 1 calc GR . . . .
H55B H 0.5662 0.5578 0.2575 0.076 Uiso 1 1 calc GR . . . .
H55C H 0.4700 0.5351 0.2607 0.076 Uiso 1 1 calc GR . . . .
C56 C 0.3806(3) 0.6139(3) 0.34904(10) 0.0396(11) Uani 1 1 d . . . . .
H56A H 0.3404 0.6513 0.3461 0.048 Uiso 1 1 calc R . . . .
H56B H 0.3493 0.5723 0.3448 0.048 Uiso 1 1 calc R . . . .
C57 C 0.4507(3) 0.5480(3) 0.38400(11) 0.0441(12) Uani 1 1 d . . . . .
H57A H 0.4887 0.5347 0.3703 0.053 Uiso 1 1 calc R . . . .
H57B H 0.4067 0.5132 0.3853 0.053 Uiso 1 1 calc R . . . .
C58 C 0.5020(3) 0.5536(3) 0.40971(11) 0.0460(12) Uani 1 1 d . . . . .
H58A H 0.4635 0.5520 0.4242 0.055 Uiso 1 1 calc R . . . .
H58B H 0.5426 0.5161 0.4117 0.055 Uiso 1 1 calc R . . . .
C59 C 0.3361(3) 0.6254(3) 0.39351(12) 0.0470(12) Uani 1 1 d . . . . .
H59A H 0.2868 0.5980 0.3872 0.056 Uiso 1 1 calc R . . . .
H59B H 0.3522 0.6115 0.4115 0.056 Uiso 1 1 calc R . . . .
C60 C 0.3104(3) 0.6967(3) 0.39346(14) 0.0555(15) Uani 1 1 d . . . . .
H60A H 0.2901 0.7103 0.3758 0.067 Uiso 1 1 calc R . . . .
H60B H 0.2635 0.7034 0.4052 0.067 Uiso 1 1 calc R . . . .
O19 O 0.7500 1.1029(9) 0.5000 0.178(6) Uani 1 2 d S TU P . .
C69 C 0.6732(11) 1.1370(12) 0.4865(4) 0.248(10) Uani 1 1 d . U . . .
H69A H 0.6430 1.1637 0.4992 0.298 Uiso 1 1 calc R . . . .
H69B H 0.6920 1.1672 0.4729 0.298 Uiso 1 1 calc R . . . .
C70 C 0.6149(14) 1.0851(11) 0.4748(4) 0.255(10) Uani 1 1 d . U . . .
H70A H 0.5606 1.1056 0.4691 0.382 Uiso 1 1 calc GR . . . .
H70B H 0.6051 1.0508 0.4877 0.382 Uiso 1 1 calc GR . . . .
H70C H 0.6409 1.0650 0.4599 0.382 Uiso 1 1 calc GR . . . .
O17 O 0.3340(7) 0.6708(7) 0.4913(2) 0.092(3) Uani 0.5 1 d . . . A -1
C61 C 0.2475(16) 0.6425(12) 0.5281(4) 0.118(7) Uani 0.5 1 d . . . A -1
H61A H 0.2818 0.6033 0.5328 0.177 Uiso 0.5 1 calc GR . . A -1
H61B H 0.1891 0.6358 0.5332 0.177 Uiso 0.5 1 calc GR . . A -1
H61C H 0.2719 0.6816 0.5370 0.177 Uiso 0.5 1 calc GR . . A -1
C62 C 0.2470(15) 0.6531(9) 0.4994(6) 0.110(5) Uani 0.5 1 d . . . A -1
H62A H 0.2273 0.6120 0.4904 0.132 Uiso 0.5 1 calc R . . A -1
H62B H 0.2067 0.6892 0.4943 0.132 Uiso 0.5 1 calc R . . A -1
C63 C 0.3517(11) 0.6912(12) 0.4644(3) 0.102(5) Uani 0.5 1 d . . . A -1
H63A H 0.3212 0.7331 0.4601 0.122 Uiso 0.5 1 calc R . . A -1
H63B H 0.3304 0.6566 0.4521 0.122 Uiso 0.5 1 calc R . . A -1
C64 C 0.4457(10) 0.7011(14) 0.4618(2) 0.118(9) Uani 0.5 1 d . . . A -1
H64A H 0.4583 0.6984 0.4435 0.177 Uiso 0.5 1 calc GR . . A -1
H64B H 0.4775 0.6665 0.4715 0.177 Uiso 0.5 1 calc GR . . A -1
H64C H 0.4626 0.7449 0.4686 0.177 Uiso 0.5 1 calc GR . . A -1
O18 O 0.3689(7) 0.8012(5) 0.26267(16) 0.145(3) Uani 1 1 d . . . . .
C65 C 0.3299(9) 0.6783(7) 0.2675(3) 0.158(6) Uani 1 1 d . . . . .
H65A H 0.2913 0.6864 0.2523 0.237 Uiso 1 1 calc GR . . . .
H65B H 0.3013 0.6503 0.2799 0.237 Uiso 1 1 calc GR . . . .
H65C H 0.3811 0.6557 0.2622 0.237 Uiso 1 1 calc GR . . . .
C66 C 0.3543(10) 0.7433(8) 0.2801(3) 0.158(5) Uani 1 1 d . . . . .
H66A H 0.3090 0.7557 0.2917 0.190 Uiso 1 1 calc R . . . .
H66B H 0.4070 0.7361 0.2911 0.190 Uiso 1 1 calc R . . . .
C67 C 0.3807(8) 0.8685(7) 0.2739(3) 0.142(4) Uani 1 1 d . . . . .
H67A H 0.3639 0.9016 0.2604 0.170 Uiso 1 1 calc R . . . .
H67B H 0.3420 0.8737 0.2881 0.170 Uiso 1 1 calc R . . . .
C68 C 0.4685(7) 0.8831(6) 0.2839(2) 0.108(3) Uani 1 1 d . . . . .
H68A H 0.5088 0.8682 0.2713 0.162 Uiso 1 1 calc GR . . . .
H68B H 0.4801 0.8597 0.3003 0.162 Uiso 1 1 calc GR . . . .
H68C H 0.4749 0.9310 0.2867 0.162 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cl1 2.3111(15) . ?
Cu1 O1 1.912(3) . ?
Cu1 O15 1.903(3) . ?
Cu1 N1 2.009(4) . ?
Cu2 O1 2.016(3) . ?
Cu2 O3 1.895(4) . ?
Cu2 O4 2.378(4) . ?
Cu2 O6 1.883(3) . ?
Cu2 N2 2.005(4) . ?
Cu3 Cl2 2.2542(14) . ?
Cu3 O3 1.901(4) . ?
Cu3 O5 1.915(3) . ?
Cu3 N3 2.006(4) . ?
Cu4 O5 1.999(3) . ?
Cu4 O7 1.905(3) . ?
Cu4 O8 2.368(4) . ?
Cu4 O10 1.875(3) . ?
Cu4 N4 2.000(4) . ?
Cu5 Cl3 2.2569(14) . ?
Cu5 O7 1.901(3) . ?
Cu5 O9 1.907(3) . ?
Cu5 N5 1.997(4) . ?
Cu6 O9 1.987(3) . ?
Cu6 O11 1.901(3) . ?
Cu6 O12 2.405(4) . ?
Cu6 O14 1.878(3) . ?
Cu6 N6 1.993(4) . ?
Cu7 Cl4 2.2664(16) . ?
Cu7 O11 1.888(3) . ?
Cu7 O13 1.912(3) . ?
Cu7 N7 1.990(4) . ?
Cu8 O2 1.876(3) . ?
Cu8 O13 1.992(3) . ?
Cu8 O15 1.891(3) . ?
Cu8 O16 2.367(4) . ?
Cu8 N8 1.999(4) . ?
O1 C1 1.341(6) . ?
O2 N1 1.359(5) . ?
O3 C13 1.426(6) . ?
O4 H4 0.84(2) . ?
O4 C15 1.434(7) . ?
O5 C16 1.350(5) . ?
O6 N3 1.360(5) . ?
O7 C28 1.418(5) . ?
O8 H8 0.84(2) . ?
O8 C30 1.413(6) . ?
O9 C31 1.337(5) . ?
O10 N5 1.359(5) . ?
O11 C43 1.420(5) . ?
O12 H12 0.84(2) . ?
O12 C45 1.423(7) . ?
O13 C46 1.337(6) . ?
O14 N7 1.356(5) . ?
O15 C58 1.435(6) . ?
O16 H16 0.85(2) . ?
O16 C60 1.446(7) . ?
N1 C7 1.301(6) . ?
N2 C11 1.498(7) . ?
N2 C12 1.474(7) . ?
N2 C14 1.493(7) . ?
N3 C22 1.299(6) . ?
N4 C26 1.497(6) . ?
N4 C27 1.485(6) . ?
N4 C29 1.494(6) . ?
N5 C37 1.305(6) . ?
N6 C41 1.501(6) . ?
N6 C42 1.493(6) . ?
N6 C44 1.490(6) . ?
N7 C52 1.303(6) . ?
N8 C56 1.483(6) . ?
N8 C57 1.492(7) . ?
N8 C59 1.497(6) . ?
C1 C2 1.411(7) . ?
C1 C6 1.410(7) . ?
C2 C3 1.386(7) . ?
C2 C11 1.499(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.386(8) . ?
C4 C5 1.383(7) . ?
C4 C10 1.512(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.405(7) . ?
C6 C7 1.479(6) . ?
C7 C8 1.502(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.510(8) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.525(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.504(9) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.410(7) . ?
C16 C21 1.396(7) . ?
C17 C18 1.392(7) . ?
C17 C26 1.496(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.395(8) . ?
C19 C20 1.385(7) . ?
C19 C25 1.508(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.408(7) . ?
C21 C22 1.478(7) . ?
C22 C23 1.505(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.530(8) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.521(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.522(8) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.415(6) . ?
C31 C36 1.411(7) . ?
C32 C33 1.382(7) . ?
C32 C41 1.499(7) . ?
C33 H33 0.9500 . ?
C33 C34 1.394(8) . ?
C34 C35 1.387(7) . ?
C34 C40 1.515(7) . ?
C35 H35 0.9500 . ?
C35 C36 1.415(6) . ?
C36 C37 1.463(6) . ?
C37 C38 1.512(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.548(8) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.522(7) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.511(8) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.417(6) . ?
C46 C51 1.399(7) . ?
C47 C48 1.383(7) . ?
C47 C56 1.509(7) . ?
C48 H48 0.9500 . ?
C48 C49 1.403(7) . ?
C49 C50 1.383(7) . ?
C49 C55 1.505(7) . ?
C50 H50 0.9500 . ?
C50 C51 1.414(6) . ?
C51 C52 1.472(6) . ?
C52 C53 1.507(6) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.533(8) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.520(7) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.492(8) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
O19 C69 1.524(15) 2_656 ?
O19 C69 1.524(15) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C69 C70 1.496(17) . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
O17 C62 1.498(18) . ?
O17 C63 1.491(14) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C61 C62 1.500(19) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.507(16) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
O18 C66 1.500(12) . ?
O18 C67 1.480(11) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C65 C66 1.501(14) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C67 C68 1.477(13) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 Cl1 89.91(11) . . ?
O1 Cu1 N1 89.16(15) . . ?
O15 Cu1 Cl1 93.52(11) . . ?
O15 Cu1 O1 171.76(16) . . ?
O15 Cu1 N1 89.22(15) . . ?
N1 Cu1 Cl1 166.61(13) . . ?
O1 Cu2 O4 96.87(15) . . ?
O3 Cu2 O1 151.80(16) . . ?
O3 Cu2 O4 110.77(16) . . ?
O3 Cu2 N2 87.27(17) . . ?
O6 Cu2 O1 88.96(14) . . ?
O6 Cu2 O3 92.67(15) . . ?
O6 Cu2 O4 97.63(16) . . ?
O6 Cu2 N2 178.03(18) . . ?
N2 Cu2 O1 92.03(16) . . ?
N2 Cu2 O4 80.56(17) . . ?
O3 Cu3 Cl2 94.09(11) . . ?
O3 Cu3 O5 172.27(16) . . ?
O3 Cu3 N3 88.62(16) . . ?
O5 Cu3 Cl2 89.37(11) . . ?
O5 Cu3 N3 89.26(15) . . ?
N3 Cu3 Cl2 169.16(13) . . ?
O5 Cu4 O8 98.30(14) . . ?
O5 Cu4 N4 93.00(15) . . ?
O7 Cu4 O5 150.98(15) . . ?
O7 Cu4 O8 110.23(15) . . ?
O7 Cu4 N4 86.65(15) . . ?
O10 Cu4 O5 89.20(14) . . ?
O10 Cu4 O7 93.21(13) . . ?
O10 Cu4 O8 95.32(15) . . ?
O10 Cu4 N4 175.72(17) . . ?
N4 Cu4 O8 80.73(15) . . ?
O7 Cu5 Cl3 93.72(10) . . ?
O7 Cu5 O9 169.99(14) . . ?
O7 Cu5 N5 88.72(14) . . ?
O9 Cu5 Cl3 91.39(11) . . ?
O9 Cu5 N5 88.73(14) . . ?
N5 Cu5 Cl3 164.04(12) . . ?
O9 Cu6 O12 95.02(14) . . ?
O9 Cu6 N6 93.13(15) . . ?
O11 Cu6 O9 152.66(15) . . ?
O11 Cu6 O12 111.94(15) . . ?
O11 Cu6 N6 87.30(15) . . ?
O14 Cu6 O9 88.53(13) . . ?
O14 Cu6 O11 93.04(13) . . ?
O14 Cu6 O12 95.76(15) . . ?
O14 Cu6 N6 175.71(17) . . ?
N6 Cu6 O12 80.16(15) . . ?
O11 Cu7 Cl4 95.39(10) . . ?
O11 Cu7 O13 169.33(15) . . ?
O11 Cu7 N7 89.21(15) . . ?
O13 Cu7 Cl4 90.17(11) . . ?
O13 Cu7 N7 88.68(14) . . ?
N7 Cu7 Cl4 159.82(13) . . ?
O2 Cu8 O13 88.76(14) . . ?
O2 Cu8 O15 93.13(15) . . ?
O2 Cu8 O16 94.25(16) . . ?
O2 Cu8 N8 175.49(18) . . ?
O13 Cu8 O16 93.87(17) . . ?
O13 Cu8 N8 92.47(16) . . ?
O15 Cu8 O13 152.68(16) . . ?
O15 Cu8 O16 113.13(19) . . ?
O15 Cu8 N8 87.77(16) . . ?
N8 Cu8 O16 81.34(16) . . ?
Cu1 O1 Cu2 115.98(17) . . ?
C1 O1 Cu1 126.2(3) . . ?
C1 O1 Cu2 107.4(3) . . ?
N1 O2 Cu8 119.5(3) . . ?
Cu2 O3 Cu3 118.93(17) . . ?
C13 O3 Cu2 113.4(3) . . ?
C13 O3 Cu3 127.6(3) . . ?
Cu2 O4 H4 89(5) . . ?
C15 O4 Cu2 103.6(3) . . ?
C15 O4 H4 109(5) . . ?
Cu3 O5 Cu4 118.65(16) . . ?
C16 O5 Cu3 124.5(3) . . ?
C16 O5 Cu4 109.4(3) . . ?
N3 O6 Cu2 119.0(3) . . ?
Cu5 O7 Cu4 117.99(16) . . ?
C28 O7 Cu4 113.9(3) . . ?
C28 O7 Cu5 128.2(3) . . ?
Cu4 O8 H8 94(5) . . ?
C30 O8 Cu4 104.8(3) . . ?
C30 O8 H8 108(5) . . ?
Cu5 O9 Cu6 118.68(16) . . ?
C31 O9 Cu5 123.6(3) . . ?
C31 O9 Cu6 112.5(3) . . ?
N5 O10 Cu4 118.0(3) . . ?
Cu7 O11 Cu6 118.16(16) . . ?
C43 O11 Cu6 113.5(3) . . ?
C43 O11 Cu7 128.3(3) . . ?
Cu6 O12 H12 98(5) . . ?
C45 O12 Cu6 104.0(3) . . ?
C45 O12 H12 108(5) . . ?
Cu7 O13 Cu8 118.04(16) . . ?
C46 O13 Cu7 123.7(3) . . ?
C46 O13 Cu8 112.2(3) . . ?
N7 O14 Cu6 118.0(2) . . ?
Cu8 O15 Cu1 118.50(17) . . ?
C58 O15 Cu1 128.1(3) . . ?
C58 O15 Cu8 113.4(3) . . ?
Cu8 O16 H16 92(6) . . ?
C60 O16 Cu8 103.8(3) . . ?
C60 O16 H16 120(6) . . ?
O2 N1 Cu1 118.2(3) . . ?
C7 N1 Cu1 128.1(3) . . ?
C7 N1 O2 113.7(4) . . ?
C11 N2 Cu2 112.5(3) . . ?
C12 N2 Cu2 102.5(3) . . ?
C12 N2 C11 111.6(4) . . ?
C12 N2 C14 110.3(4) . . ?
C14 N2 Cu2 109.7(3) . . ?
C14 N2 C11 110.0(4) . . ?
O6 N3 Cu3 118.7(3) . . ?
C22 N3 Cu3 127.1(3) . . ?
C22 N3 O6 114.1(4) . . ?
C26 N4 Cu4 112.1(3) . . ?
C27 N4 Cu4 103.1(3) . . ?
C27 N4 C26 110.2(4) . . ?
C27 N4 C29 111.1(4) . . ?
C29 N4 Cu4 109.9(3) . . ?
C29 N4 C26 110.2(4) . . ?
O10 N5 Cu5 119.0(3) . . ?
C37 N5 Cu5 126.3(3) . . ?
C37 N5 O10 114.8(4) . . ?
C41 N6 Cu6 113.3(3) . . ?
C42 N6 Cu6 102.5(3) . . ?
C42 N6 C41 111.4(4) . . ?
C44 N6 Cu6 109.2(3) . . ?
C44 N6 C41 110.1(4) . . ?
C44 N6 C42 110.0(4) . . ?
O14 N7 Cu7 118.9(3) . . ?
C52 N7 Cu7 126.3(3) . . ?
C52 N7 O14 114.9(4) . . ?
C56 N8 Cu8 113.5(3) . . ?
C56 N8 C57 111.1(4) . . ?
C56 N8 C59 110.8(4) . . ?
C57 N8 Cu8 102.7(3) . . ?
C57 N8 C59 110.4(4) . . ?
C59 N8 Cu8 107.9(3) . . ?
O1 C1 C2 117.1(4) . . ?
O1 C1 C6 123.3(4) . . ?
C6 C1 C2 119.6(4) . . ?
C1 C2 C11 118.2(5) . . ?
C3 C2 C1 119.9(5) . . ?
C3 C2 C11 121.9(5) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.7(5) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C10 121.1(5) . . ?
C5 C4 C3 117.9(5) . . ?
C5 C4 C10 121.0(5) . . ?
C4 C5 H5 118.5 . . ?
C4 C5 C6 123.0(5) . . ?
C6 C5 H5 118.5 . . ?
C1 C6 C7 123.1(4) . . ?
C5 C6 C1 117.9(4) . . ?
C5 C6 C7 119.0(4) . . ?
N1 C7 C6 121.4(4) . . ?
N1 C7 C8 118.7(4) . . ?
C6 C7 C8 119.8(4) . . ?
C7 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
C7 C8 C9 111.1(4) . . ?
H8A C8 H8B 108.0 . . ?
C9 C8 H8A 109.4 . . ?
C9 C8 H8B 109.4 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C2 111.7(4) . . ?
N2 C11 H11A 109.3 . . ?
N2 C11 H11B 109.3 . . ?
C2 C11 H11A 109.3 . . ?
C2 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
N2 C12 C13 110.6(5) . . ?
H12A C12 H12B 108.1 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
O3 C13 C12 107.5(4) . . ?
O3 C13 H13A 110.2 . . ?
O3 C13 H13B 110.2 . . ?
C12 C13 H13A 110.2 . . ?
C12 C13 H13B 110.2 . . ?
H13A C13 H13B 108.5 . . ?
N2 C14 H14A 109.4 . . ?
N2 C14 H14B 109.4 . . ?
N2 C14 C15 111.4(5) . . ?
H14A C14 H14B 108.0 . . ?
C15 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
O4 C15 C14 108.9(5) . . ?
O4 C15 H15A 109.9 . . ?
O4 C15 H15B 109.9 . . ?
C14 C15 H15A 109.9 . . ?
C14 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
O5 C16 C17 116.9(4) . . ?
O5 C16 C21 122.7(4) . . ?
C21 C16 C17 120.4(4) . . ?
C16 C17 C26 118.8(4) . . ?
C18 C17 C16 119.5(5) . . ?
C18 C17 C26 121.6(5) . . ?
C17 C18 H18 119.3 . . ?
C17 C18 C19 121.3(5) . . ?
C19 C18 H18 119.3 . . ?
C18 C19 C25 119.7(5) . . ?
C20 C19 C18 118.0(5) . . ?
C20 C19 C25 122.3(5) . . ?
C19 C20 H20 118.6 . . ?
C19 C20 C21 122.7(5) . . ?
C21 C20 H20 118.6 . . ?
C16 C21 C20 117.9(4) . . ?
C16 C21 C22 123.3(4) . . ?
C20 C21 C22 118.8(4) . . ?
N3 C22 C21 121.4(4) . . ?
N3 C22 C23 119.3(4) . . ?
C21 C22 C23 119.3(4) . . ?
C22 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
C22 C23 C24 111.1(4) . . ?
H23A C23 H23B 108.0 . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C19 C25 H25A 109.5 . . ?
C19 C25 H25B 109.5 . . ?
C19 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N4 C26 H26A 109.1 . . ?
N4 C26 H26B 109.1 . . ?
C17 C26 N4 112.6(4) . . ?
C17 C26 H26A 109.1 . . ?
C17 C26 H26B 109.1 . . ?
H26A C26 H26B 107.8 . . ?
N4 C27 H27A 109.6 . . ?
N4 C27 H27B 109.6 . . ?
N4 C27 C28 110.1(4) . . ?
H27A C27 H27B 108.2 . . ?
C28 C27 H27A 109.6 . . ?
C28 C27 H27B 109.6 . . ?
O7 C28 C27 108.4(4) . . ?
O7 C28 H28A 110.0 . . ?
O7 C28 H28B 110.0 . . ?
C27 C28 H28A 110.0 . . ?
C27 C28 H28B 110.0 . . ?
H28A C28 H28B 108.4 . . ?
N4 C29 H29A 109.2 . . ?
N4 C29 H29B 109.2 . . ?
N4 C29 C30 112.0(4) . . ?
H29A C29 H29B 107.9 . . ?
C30 C29 H29A 109.2 . . ?
C30 C29 H29B 109.2 . . ?
O8 C30 C29 108.9(4) . . ?
O8 C30 H30A 109.9 . . ?
O8 C30 H30B 109.9 . . ?
C29 C30 H30A 109.9 . . ?
C29 C30 H30B 109.9 . . ?
H30A C30 H30B 108.3 . . ?
O9 C31 C32 117.9(4) . . ?
O9 C31 C36 122.1(4) . . ?
C36 C31 C32 120.0(4) . . ?
C31 C32 C41 119.0(4) . . ?
C33 C32 C31 119.6(5) . . ?
C33 C32 C41 121.0(4) . . ?
C32 C33 H33 119.0 . . ?
C32 C33 C34 122.0(5) . . ?
C34 C33 H33 119.0 . . ?
C33 C34 C40 121.5(5) . . ?
C35 C34 C33 117.7(5) . . ?
C35 C34 C40 120.8(5) . . ?
C34 C35 H35 118.5 . . ?
C34 C35 C36 122.9(5) . . ?
C36 C35 H35 118.5 . . ?
C31 C36 C35 117.4(4) . . ?
C31 C36 C37 123.3(4) . . ?
C35 C36 C37 119.3(4) . . ?
N5 C37 C36 120.7(4) . . ?
N5 C37 C38 118.4(4) . . ?
C36 C37 C38 120.9(4) . . ?
C37 C38 H38A 109.3 . . ?
C37 C38 H38B 109.3 . . ?
C37 C38 C39 111.7(4) . . ?
H38A C38 H38B 107.9 . . ?
C39 C38 H38A 109.3 . . ?
C39 C38 H38B 109.3 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C34 C40 H40A 109.5 . . ?
C34 C40 H40B 109.5 . . ?
C34 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N6 C41 H41A 108.6 . . ?
N6 C41 H41B 108.6 . . ?
C32 C41 N6 114.7(4) . . ?
C32 C41 H41A 108.6 . . ?
C32 C41 H41B 108.6 . . ?
H41A C41 H41B 107.6 . . ?
N6 C42 H42A 109.6 . . ?
N6 C42 H42B 109.6 . . ?
N6 C42 C43 110.3(4) . . ?
H42A C42 H42B 108.1 . . ?
C43 C42 H42A 109.6 . . ?
C43 C42 H42B 109.6 . . ?
O11 C43 C42 108.5(4) . . ?
O11 C43 H43A 110.0 . . ?
O11 C43 H43B 110.0 . . ?
C42 C43 H43A 110.0 . . ?
C42 C43 H43B 110.0 . . ?
H43A C43 H43B 108.4 . . ?
N6 C44 H44A 109.2 . . ?
N6 C44 H44B 109.2 . . ?
N6 C44 C45 111.9(4) . . ?
H44A C44 H44B 107.9 . . ?
C45 C44 H44A 109.2 . . ?
C45 C44 H44B 109.2 . . ?
O12 C45 C44 108.8(4) . . ?
O12 C45 H45A 109.9 . . ?
O12 C45 H45B 109.9 . . ?
C44 C45 H45A 109.9 . . ?
C44 C45 H45B 109.9 . . ?
H45A C45 H45B 108.3 . . ?
O13 C46 C47 116.9(4) . . ?
O13 C46 C51 122.7(4) . . ?
C51 C46 C47 120.3(4) . . ?
C46 C47 C56 119.0(4) . . ?
C48 C47 C46 119.2(4) . . ?
C48 C47 C56 121.4(4) . . ?
C47 C48 H48 119.0 . . ?
C47 C48 C49 122.0(4) . . ?
C49 C48 H48 119.0 . . ?
C48 C49 C55 121.0(4) . . ?
C50 C49 C48 117.5(4) . . ?
C50 C49 C55 121.5(5) . . ?
C49 C50 H50 118.6 . . ?
C49 C50 C51 122.9(5) . . ?
C51 C50 H50 118.6 . . ?
C46 C51 C50 117.8(4) . . ?
C46 C51 C52 123.0(4) . . ?
C50 C51 C52 119.1(4) . . ?
N7 C52 C51 121.1(4) . . ?
N7 C52 C53 118.3(4) . . ?
C51 C52 C53 120.6(4) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
C52 C53 C54 110.5(4) . . ?
H53A C53 H53B 108.1 . . ?
C54 C53 H53A 109.5 . . ?
C54 C53 H53B 109.5 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C49 C55 H55A 109.5 . . ?
C49 C55 H55B 109.5 . . ?
C49 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
N8 C56 C47 114.3(4) . . ?
N8 C56 H56A 108.7 . . ?
N8 C56 H56B 108.7 . . ?
C47 C56 H56A 108.7 . . ?
C47 C56 H56B 108.7 . . ?
H56A C56 H56B 107.6 . . ?
N8 C57 H57A 109.5 . . ?
N8 C57 H57B 109.5 . . ?
N8 C57 C58 110.8(4) . . ?
H57A C57 H57B 108.1 . . ?
C58 C57 H57A 109.5 . . ?
C58 C57 H57B 109.5 . . ?
O15 C58 C57 108.5(4) . . ?
O15 C58 H58A 110.0 . . ?
O15 C58 H58B 110.0 . . ?
C57 C58 H58A 110.0 . . ?
C57 C58 H58B 110.0 . . ?
H58A C58 H58B 108.4 . . ?
N8 C59 H59A 109.1 . . ?
N8 C59 H59B 109.1 . . ?
H59A C59 H59B 107.8 . . ?
C60 C59 N8 112.4(4) . . ?
C60 C59 H59A 109.1 . . ?
C60 C59 H59B 109.1 . . ?
O16 C60 C59 109.0(5) . . ?
O16 C60 H60A 109.9 . . ?
O16 C60 H60B 109.9 . . ?
C59 C60 H60A 109.9 . . ?
C59 C60 H60B 109.9 . . ?
H60A C60 H60B 108.3 . . ?
C69 O19 C69 126(2) 2_656 . ?
O19 C69 H69A 109.9 . . ?
O19 C69 H69B 109.9 . . ?
H69A C69 H69B 108.3 . . ?
C70 C69 O19 108.8(18) . . ?
C70 C69 H69A 109.9 . . ?
C70 C69 H69B 109.9 . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C63 O17 C62 123.3(16) . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C62 C61 H61A 109.5 . . ?
C62 C61 H61B 109.5 . . ?
C62 C61 H61C 109.5 . . ?
O17 C62 C61 111(2) . . ?
O17 C62 H62A 109.4 . . ?
O17 C62 H62B 109.4 . . ?
C61 C62 H62A 109.4 . . ?
C61 C62 H62B 109.4 . . ?
H62A C62 H62B 108.0 . . ?
O17 C63 H63A 109.4 . . ?
O17 C63 H63B 109.4 . . ?
O17 C63 C64 111.0(13) . . ?
H63A C63 H63B 108.0 . . ?
C64 C63 H63A 109.4 . . ?
C64 C63 H63B 109.4 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C67 O18 C66 119.7(11) . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C66 C65 H65A 109.5 . . ?
C66 C65 H65B 109.5 . . ?
C66 C65 H65C 109.5 . . ?
O18 C66 C65 117.4(13) . . ?
O18 C66 H66A 107.9 . . ?
O18 C66 H66B 107.9 . . ?
C65 C66 H66A 107.9 . . ?
C65 C66 H66B 107.9 . . ?
H66A C66 H66B 107.2 . . ?
O18 C67 H67A 108.6 . . ?
O18 C67 H67B 108.6 . . ?
H67A C67 H67B 107.6 . . ?
C68 C67 O18 114.4(10) . . ?
C68 C67 H67A 108.6 . . ?
C68 C67 H67B 108.6 . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 Cl1 0.84(2) 2.31(3) 3.130(5) 163(7) .
O8 H8 Cl2 0.84(2) 2.25(3) 3.062(4) 163(6) .
O12 H12 Cl3 0.84(2) 2.26(3) 3.078(4) 164(6) .
O16 H16 Cl4 0.85(2) 2.39(5) 3.136(6) 146(7) .

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
Cu1 O1 C1 C2 154.9(3) . . . . ?
Cu1 O1 C1 C6 -27.3(6) . . . . ?
Cu1 O15 C58 C57 -159.8(4) . . . . ?
Cu1 N1 C7 C6 -0.2(7) . . . . ?
Cu1 N1 C7 C8 -177.3(3) . . . . ?
Cu2 O1 C1 C2 -62.2(5) . . . . ?
Cu2 O1 C1 C6 115.6(4) . . . . ?
Cu2 O3 C13 C12 -23.6(6) . . . . ?
Cu2 O4 C15 C14 -37.2(5) . . . . ?
Cu2 O6 N3 Cu3 -15.7(5) . . . . ?
Cu2 O6 N3 C22 167.3(3) . . . . ?
Cu2 N2 C11 C2 -45.7(5) . . . . ?
Cu2 N2 C12 C13 -43.3(5) . . . . ?
Cu2 N2 C14 C15 -47.2(6) . . . . ?
Cu3 O3 C13 C12 154.1(4) . . . . ?
Cu3 O5 C16 C17 -151.9(3) . . . . ?
Cu3 O5 C16 C21 31.6(6) . . . . ?
Cu3 N3 C22 C21 4.0(6) . . . . ?
Cu3 N3 C22 C23 -177.2(3) . . . . ?
Cu4 O5 C16 C17 58.7(4) . . . . ?
Cu4 O5 C16 C21 -117.7(4) . . . . ?
Cu4 O7 C28 C27 21.3(5) . . . . ?
Cu4 O8 C30 C29 35.6(5) . . . . ?
Cu4 O10 N5 Cu5 19.9(4) . . . . ?
Cu4 O10 N5 C37 -160.7(3) . . . . ?
Cu4 N4 C26 C17 45.1(5) . . . . ?
Cu4 N4 C27 C28 43.0(4) . . . . ?
Cu4 N4 C29 C30 44.9(5) . . . . ?
Cu5 O7 C28 C27 -158.0(3) . . . . ?
Cu5 O9 C31 C32 149.2(3) . . . . ?
Cu5 O9 C31 C36 -31.1(6) . . . . ?
Cu5 N5 C37 C36 1.7(6) . . . . ?
Cu5 N5 C37 C38 -178.0(3) . . . . ?
Cu6 O9 C31 C32 -56.7(5) . . . . ?
Cu6 O9 C31 C36 122.9(4) . . . . ?
Cu6 O11 C43 C42 -20.6(5) . . . . ?
Cu6 O12 C45 C44 -33.6(5) . . . . ?
Cu6 O14 N7 Cu7 -19.6(4) . . . . ?
Cu6 O14 N7 C52 159.1(3) . . . . ?
Cu6 N6 C41 C32 -42.5(5) . . . . ?
Cu6 N6 C42 C43 -43.2(4) . . . . ?
Cu6 N6 C44 C45 -50.2(5) . . . . ?
Cu7 O11 C43 C42 160.8(3) . . . . ?
Cu7 O13 C46 C47 -151.2(3) . . . . ?
Cu7 O13 C46 C51 30.2(6) . . . . ?
Cu7 N7 C52 C51 -4.5(6) . . . . ?
Cu7 N7 C52 C53 175.4(3) . . . . ?
Cu8 O2 N1 Cu1 13.5(5) . . . . ?
Cu8 O2 N1 C7 -167.6(3) . . . . ?
Cu8 O13 C46 C47 56.9(4) . . . . ?
Cu8 O13 C46 C51 -121.7(4) . . . . ?
Cu8 O15 C58 C57 20.8(6) . . . . ?
Cu8 O16 C60 C59 33.3(6) . . . . ?
Cu8 N8 C56 C47 41.7(5) . . . . ?
Cu8 N8 C57 C58 41.7(5) . . . . ?
Cu8 N8 C59 C60 49.8(5) . . . . ?
Cl4 Cu7 O11 Cu6 -167.23(18) . . . . ?
Cl4 Cu7 O11 C43 11.3(4) . . . . ?
O1 Cu2 O3 Cu3 -88.9(4) . . . . ?
O1 Cu2 O3 C13 89.0(5) . . . . ?
O1 Cu2 O6 N3 159.1(3) . . . . ?
O1 C1 C2 C3 178.5(4) . . . . ?
O1 C1 C2 C11 -1.7(7) . . . . ?
O1 C1 C6 C5 -179.0(4) . . . . ?
O1 C1 C6 C7 -2.1(7) . . . . ?
O2 Cu8 O15 Cu1 -1.7(2) . . . . ?
O2 Cu8 O15 C58 177.8(4) . . . . ?
O2 N1 C7 C6 -179.0(4) . . . . ?
O2 N1 C7 C8 3.9(6) . . . . ?
O3 Cu2 O6 N3 7.3(4) . . . . ?
O4 Cu2 O3 Cu3 103.1(2) . . . . ?
O4 Cu2 O3 C13 -79.0(4) . . . . ?
O4 Cu2 O6 N3 -104.1(3) . . . . ?
O5 Cu4 O10 N5 -161.4(3) . . . . ?
O5 C16 C17 C18 -178.1(4) . . . . ?
O5 C16 C17 C26 4.2(6) . . . . ?
O5 C16 C21 C20 -179.5(4) . . . . ?
O5 C16 C21 C22 2.3(7) . . . . ?
O6 Cu2 O3 Cu3 3.9(3) . . . . ?
O6 Cu2 O3 C13 -178.2(4) . . . . ?
O6 N3 C22 C21 -179.3(4) . . . . ?
O6 N3 C22 C23 -0.5(6) . . . . ?
O7 Cu4 O10 N5 -10.3(3) . . . . ?
O8 Cu4 O10 N5 100.3(3) . . . . ?
O9 Cu6 O14 N7 164.5(3) . . . . ?
O9 C31 C32 C33 -175.9(4) . . . . ?
O9 C31 C32 C41 -3.2(6) . . . . ?
O9 C31 C36 C35 174.2(4) . . . . ?
O9 C31 C36 C37 -7.5(7) . . . . ?
O10 N5 C37 C36 -177.7(4) . . . . ?
O10 N5 C37 C38 2.6(6) . . . . ?
O11 Cu6 O14 N7 11.8(3) . . . . ?
O12 Cu6 O14 N7 -100.6(3) . . . . ?
O13 Cu7 O11 Cu6 71.7(8) . . . . ?
O13 Cu7 O11 C43 -109.8(8) . . . . ?
O13 Cu8 O2 N1 -160.0(3) . . . . ?
O13 Cu8 O15 Cu1 91.6(4) . . . . ?
O13 Cu8 O15 C58 -88.9(5) . . . . ?
O13 C46 C47 C48 177.8(4) . . . . ?
O13 C46 C47 C56 4.6(6) . . . . ?
O13 C46 C51 C50 -175.8(4) . . . . ?
O13 C46 C51 C52 6.6(7) . . . . ?
O14 N7 C52 C51 176.9(4) . . . . ?
O14 N7 C52 C53 -3.3(6) . . . . ?
O15 Cu8 O2 N1 -7.2(4) . . . . ?
O16 Cu8 O2 N1 106.3(4) . . . . ?
O16 Cu8 O15 Cu1 -97.7(2) . . . . ?
O16 Cu8 O15 C58 81.8(4) . . . . ?
N1 C7 C8 C9 81.8(6) . . . . ?
N2 Cu2 O3 Cu3 -178.1(3) . . . . ?
N2 Cu2 O3 C13 -0.2(4) . . . . ?
N2 C12 C13 O3 45.6(6) . . . . ?
N2 C14 C15 O4 58.5(6) . . . . ?
N3 C22 C23 C24 -81.2(6) . . . . ?
N4 C27 C28 O7 -43.6(5) . . . . ?
N4 C29 C30 O8 -55.8(6) . . . . ?
N5 C37 C38 C39 77.5(6) . . . . ?
N6 C42 C43 O11 43.4(5) . . . . ?
N6 C44 C45 O12 57.8(6) . . . . ?
N7 Cu7 O11 Cu6 -6.9(2) . . . . ?
N7 Cu7 O11 C43 171.6(4) . . . . ?
N7 C52 C53 C54 -76.9(6) . . . . ?
N8 Cu8 O15 Cu1 -177.3(2) . . . . ?
N8 Cu8 O15 C58 2.2(4) . . . . ?
N8 C57 C58 O15 -42.5(6) . . . . ?
N8 C59 C60 O16 -57.5(7) . . . . ?
C1 C2 C3 C4 0.2(7) . . . . ?
C1 C2 C11 N2 64.6(6) . . . . ?
C1 C6 C7 N1 15.8(7) . . . . ?
C1 C6 C7 C8 -167.1(4) . . . . ?
C2 C1 C6 C5 -1.2(7) . . . . ?
C2 C1 C6 C7 175.7(4) . . . . ?
C2 C3 C4 C5 -0.2(7) . . . . ?
C2 C3 C4 C10 -178.9(5) . . . . ?
C3 C2 C11 N2 -115.6(5) . . . . ?
C3 C4 C5 C6 -0.5(7) . . . . ?
C4 C5 C6 C1 1.2(7) . . . . ?
C4 C5 C6 C7 -175.8(4) . . . . ?
C5 C6 C7 N1 -167.3(4) . . . . ?
C5 C6 C7 C8 9.8(6) . . . . ?
C6 C1 C2 C3 0.6(7) . . . . ?
C6 C1 C2 C11 -179.6(4) . . . . ?
C6 C7 C8 C9 -95.4(5) . . . . ?
C10 C4 C5 C6 178.2(5) . . . . ?
C11 N2 C12 C13 -163.9(4) . . . . ?
C11 N2 C14 C15 77.0(6) . . . . ?
C11 C2 C3 C4 -179.7(5) . . . . ?
C12 N2 C11 C2 68.9(5) . . . . ?
C12 N2 C14 C15 -159.4(5) . . . . ?
C14 N2 C11 C2 -168.3(4) . . . . ?
C14 N2 C12 C13 73.4(5) . . . . ?
C16 C17 C18 C19 -1.9(7) . . . . ?
C16 C17 C26 N4 -64.7(6) . . . . ?
C16 C21 C22 N3 -20.5(7) . . . . ?
C16 C21 C22 C23 160.7(4) . . . . ?
C17 C16 C21 C20 4.2(7) . . . . ?
C17 C16 C21 C22 -174.1(4) . . . . ?
C17 C18 C19 C20 2.3(7) . . . . ?
C17 C18 C19 C25 -176.5(5) . . . . ?
C18 C17 C26 N4 117.6(5) . . . . ?
C18 C19 C20 C21 0.6(8) . . . . ?
C19 C20 C21 C16 -3.8(7) . . . . ?
C19 C20 C21 C22 174.6(5) . . . . ?
C20 C21 C22 N3 161.3(4) . . . . ?
C20 C21 C22 C23 -17.5(6) . . . . ?
C21 C16 C17 C18 -1.5(7) . . . . ?
C21 C16 C17 C26 -179.3(4) . . . . ?
C21 C22 C23 C24 97.6(5) . . . . ?
C25 C19 C20 C21 179.3(5) . . . . ?
C26 N4 C27 C28 162.9(4) . . . . ?
C26 N4 C29 C30 -79.1(5) . . . . ?
C26 C17 C18 C19 175.8(5) . . . . ?
C27 N4 C26 C17 -69.2(5) . . . . ?
C27 N4 C29 C30 158.5(4) . . . . ?
C29 N4 C26 C17 167.8(4) . . . . ?
C29 N4 C27 C28 -74.7(5) . . . . ?
C31 C32 C33 C34 0.6(7) . . . . ?
C31 C32 C41 N6 59.7(6) . . . . ?
C31 C36 C37 N5 22.4(7) . . . . ?
C31 C36 C37 C38 -157.9(4) . . . . ?
C32 C31 C36 C35 -6.2(6) . . . . ?
C32 C31 C36 C37 172.1(4) . . . . ?
C32 C33 C34 C35 -3.7(7) . . . . ?
C32 C33 C34 C40 174.7(5) . . . . ?
C33 C32 C41 N6 -127.7(5) . . . . ?
C33 C34 C35 C36 1.8(7) . . . . ?
C34 C35 C36 C31 3.1(7) . . . . ?
C34 C35 C36 C37 -175.3(4) . . . . ?
C35 C36 C37 N5 -159.3(4) . . . . ?
C35 C36 C37 C38 20.4(6) . . . . ?
C36 C31 C32 C33 4.5(7) . . . . ?
C36 C31 C32 C41 177.2(4) . . . . ?
C36 C37 C38 C39 -102.2(5) . . . . ?
C40 C34 C35 C36 -176.6(5) . . . . ?
C41 N6 C42 C43 -164.7(4) . . . . ?
C41 N6 C44 C45 74.8(5) . . . . ?
C41 C32 C33 C34 -171.9(5) . . . . ?
C42 N6 C41 C32 72.5(5) . . . . ?
C42 N6 C44 C45 -162.0(4) . . . . ?
C44 N6 C41 C32 -165.1(4) . . . . ?
C44 N6 C42 C43 72.9(5) . . . . ?
C46 C47 C48 C49 -1.0(7) . . . . ?
C46 C47 C56 N8 -61.1(6) . . . . ?
C46 C51 C52 N7 -19.7(7) . . . . ?
C46 C51 C52 C53 160.4(4) . . . . ?
C47 C46 C51 C50 5.6(6) . . . . ?
C47 C46 C51 C52 -171.9(4) . . . . ?
C47 C48 C49 C50 3.1(8) . . . . ?
C47 C48 C49 C55 -175.9(5) . . . . ?
C48 C47 C56 N8 125.8(5) . . . . ?
C48 C49 C50 C51 -0.9(7) . . . . ?
C49 C50 C51 C46 -3.5(7) . . . . ?
C49 C50 C51 C52 174.2(4) . . . . ?
C50 C51 C52 N7 162.8(4) . . . . ?
C50 C51 C52 C53 -17.1(6) . . . . ?
C51 C46 C47 C48 -3.6(7) . . . . ?
C51 C46 C47 C56 -176.8(4) . . . . ?
C51 C52 C53 C54 103.0(5) . . . . ?
C55 C49 C50 C51 178.1(5) . . . . ?
C56 N8 C57 C58 163.4(4) . . . . ?
C56 N8 C59 C60 -75.1(6) . . . . ?
C56 C47 C48 C49 172.1(5) . . . . ?
C57 N8 C56 C47 -73.5(5) . . . . ?
C57 N8 C59 C60 161.3(5) . . . . ?
C59 N8 C56 C47 163.3(4) . . . . ?
C59 N8 C57 C58 -73.2(5) . . . . ?
C69 O19 C69 C70 177.2(19) 2_656 . . . ?
C62 O17 C63 C64 -175.9(18) . . . . ?
C63 O17 C62 C61 -173.3(18) . . . . ?
C66 O18 C67 C68 83.5(16) . . . . ?
C67 O18 C66 C65 171.2(12) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-7 -9 5 0.0565 -7.4683 -8.7826 5.3698 0.0374 0.2963 0.9544
-8 8 5 0.0399 -7.7127 8.4603 4.9872 0.1282 0.9765 -0.1733
8 -8 -5 0.0462 8.0808 -7.8648 -5.2570 -0.1292 -0.9849 0.1155
-5 -11 2 0.0706 -5.1057 -11.3096 2.0209 -0.0556 0.0000 0.9985
-1 -1 -33 0.0180 -0.5588 -0.7641 -33.3090 -0.9996 0.0255 -0.0091
5 11 -2 0.0377 5.1047 11.3089 -2.1221 0.0526 0.0000 -0.9986
1 1 33 0.0197 0.5588 0.7641 33.3090 0.9996 -0.0255 0.0091

_olex2_exptl_crystal_mounting_method 'Mitegen tip, Paratone oil'
_olex2_submission_original_sample_id JF3243.1
_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_7
_database_code_depnum_ccdc_archive 'CCDC 1029556'
_audit_update_record             
;
2014-10-16 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
# local name eb4182
_audit_creation_date             2014-09-04
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C60 H84 Br4 Cu8 N8 O16), 3(C4 H10 O)'
_chemical_formula_sum            'C132 H198 Br8 Cu16 N16 O35'
_chemical_formula_weight         4224.97
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40 H40 N8 O20 Cu'
_chemical_oxdiff_usercomment     '@ 120 K JF3041'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   15.8200(4)
_cell_length_b                   20.0425(4)
_cell_length_c                   51.3059(14)
_cell_angle_alpha                90
_cell_angle_beta                 93.223(2)
_cell_angle_gamma                90
_cell_volume                     16242.0(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14644
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      74.4260
_cell_measurement_theta_min      3.5410
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.106
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.995
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             8504
_exptl_crystal_size_max          0.0813
_exptl_crystal_size_mid          0.0534
_exptl_crystal_size_min          0.0357
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1203
_diffrn_reflns_av_unetI/netI     0.0603
_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       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            125018
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         3.400
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -70.00   27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   57.0000   60.0000 97

#__ type_ start__ end____ width___ exp.time_
  2 omega  -50.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000 -150.0000 79

#__ type_ start__ end____ width___ exp.time_
  3 omega  -50.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000 -180.0000 79

#__ type_ start__ end____ width___ exp.time_
  4 omega -113.00  -17.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000  -90.0000 96

#__ type_ start__ end____ width___ exp.time_
  5 omega    1.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686  -99.0000 -180.0000 82

#__ type_ start__ end____ width___ exp.time_
  6 omega    1.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686  -99.0000  120.0000 82

#__ type_ start__ end____ width___ exp.time_
  7 omega   37.00  142.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -150.0000 105

#__ type_ start__ end____ width___ exp.time_
  8 omega   39.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   60.0000 82

#__ type_ start__ end____ width___ exp.time_
  9 omega   41.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000    0.0000 98

#__ type_ start__ end____ width___ exp.time_
 10 omega   39.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -30.0000 82

#__ type_ start__ end____ width___ exp.time_
 11 omega   87.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  120.0000 91

#__ type_ start__ end____ width___ exp.time_
 12 omega   36.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -180.0000 55

#__ type_ start__ end____ width___ exp.time_
 13 omega   66.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  -30.0000 112

#__ type_ start__ end____ width___ exp.time_
 14 omega   66.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  120.0000 112

#__ type_ start__ end____ width___ exp.time_
 15 omega   87.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000    0.0000 91

#__ type_ start__ end____ width___ exp.time_
 16 omega   30.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 79

#__ type_ start__ end____ width___ exp.time_
 17 omega   36.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000    0.0000 55

#__ type_ start__ end____ width___ exp.time_
 18 omega   39.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  150.0000 82

#__ type_ start__ end____ width___ exp.time_
 19 omega   40.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000    0.0000 58

#__ type_ start__ end____ width___ exp.time_
 20 omega   40.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -90.0000 58

#__ type_ start__ end____ width___ exp.time_
 21 omega   30.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 79

#__ type_ start__ end____ width___ exp.time_
 22 omega   37.00  142.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -120.0000 105

#__ type_ start__ end____ width___ exp.time_
 23 omega   94.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
 24 omega   30.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 79

#__ type_ start__ end____ width___ exp.time_
 25 omega   39.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 82

#__ type_ start__ end____ width___ exp.time_
 26 omega   87.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000 -180.0000 91

#__ type_ start__ end____ width___ exp.time_
 27 omega   41.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 68

#__ type_ start__ end____ width___ exp.time_
 28 omega   84.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   67.0000  -50.4806 93

#__ type_ start__ end____ width___ exp.time_
 29 omega   96.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 30 omega   51.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   30.0000 40

#__ type_ start__ end____ width___ exp.time_
 31 omega   58.00  125.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -131.0000 -155.4745 67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0776751000
_diffrn_orient_matrix_UB_12      0.0232622000
_diffrn_orient_matrix_UB_13      -0.0143554000
_diffrn_orient_matrix_UB_21      -0.0008510000
_diffrn_orient_matrix_UB_22      -0.0660826000
_diffrn_orient_matrix_UB_23      -0.0153655000
_diffrn_orient_matrix_UB_31      -0.0589677000
_diffrn_orient_matrix_UB_32      0.0316671000
_diffrn_orient_matrix_UB_33      -0.0214963000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11336
_reflns_number_total             14848
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_refine_diff_density_max         1.451
_refine_diff_density_min         -2.800
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     962
_refine_ls_number_reflns         14848
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0769
_refine_ls_restrained_S_all      1.066
_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)+(0.1205P)²+168.8881P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2035
_refine_ls_wR_factor_ref         0.2205
_refine_special_details          
;
O-bound H atoms were located in a difference Fourier map and refined with 
geometric restraints (AFIX 83 in SHELXL). Two molecules of diethyl ether 
were located. One (containing O17) is located entirely on general 
positions. The second (containing O18) was modelled as disordered around 
a crystallographic twofold rotation axis. Displacement ellipsoid similarity 
restraints were used on this molecule, and C69 was refined using an 
isotropic model. The deepest hole is 2.8 electrons deep located 0.14 A 
from Br3.




#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .        239 Ang3

The largest residual peak is 1.45 electrons high located 0.34 A from H69C.

#===============================================================================

098_ALERT_2_C Large Reported Min.  (Negative) Residual Density      -2.80 eA-3

The deepest hole is 2.8 electrons deep located 0.14 A 
from Br3.


241_ALERT_2_C High      Ueq as Compared to Neighbors for .....        O16 Check
243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors of         C61 Check
244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors of         O17 Check
244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors of         C63 Check
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0122 Ang.
410_ALERT_2_C Short Intra H...H Contact  H5     ..  H8A     ..       1.96 Ang.

Noted.

#===============================================================================





;





# start Validation Reply Form
_vrf_PLAT601_eb4182              
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        225 Ang3  
RESPONSE: Please see the _refine_special_details section of the CIF.
;
# end Validation Reply Form

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C62, C61, O17, C63, C64
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C68
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C61) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 O17, C63, C62, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C67, O18, C68
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C69, C68
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O18(0.5) C66(0.5) H66A(0.5) H66B(0.5) C67(0.5) H67A(0.5) H67B(0.5)
 H67C(0.5) C68(0.5) H68A(0.5) H68B(0.5) C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
  C29(H29A,H29B), C30(H30A,H30B), C38(H38A,H38B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C53(H53A,H53B),
 C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B),
  C66(H66A,H66B), C68(H68A,H68B), C61(H61A,H61B), C63(H63A,H63B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C18(H18), C20(H20), C33(H33), C35(H35), C48(H48), C50(H50)
6.c Tetrahedral OH refined with riding coordinates:
 O4(H4), O8(H8), O12(H12), O16(H16)
6.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C62(H62A,H62B,H62C),
 C64(H64A,H64B,H64C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Br1 Br 0.85101(7) 0.96243(5) 0.54348(2) 0.0445(2) Uani 1 1 d . . . . .
Br2 Br 0.38698(8) 0.85632(7) 0.61984(3) 0.0612(3) Uani 1 1 d . . . . .
Br3 Br 0.64568(7) 0.52669(6) 0.70122(2) 0.0517(3) Uani 1 1 d . . . . .
Br4 Br 1.13235(8) 0.66681(7) 0.64446(5) 0.0863(6) Uani 1 1 d . . . . .
Cu1 Cu 0.85044(7) 0.86118(6) 0.56828(2) 0.0252(2) Uani 1 1 d . . . . .
Cu2 Cu 0.64041(7) 0.87371(6) 0.56653(2) 0.0265(3) Uani 1 1 d . . . . .
Cu3 Cu 0.53427(7) 0.85768(6) 0.61905(2) 0.0245(2) Uani 1 1 d . . . . .
Cu4 Cu 0.53044(7) 0.74525(5) 0.66738(2) 0.0228(2) Uani 1 1 d . . . . .
Cu5 Cu 0.63917(7) 0.60710(5) 0.66732(2) 0.0216(2) Uani 1 1 d . . . . .
Cu6 Cu 0.84230(7) 0.57384(5) 0.65624(2) 0.0219(2) Uani 1 1 d . . . . .
Cu7 Cu 0.98807(7) 0.68613(5) 0.65048(2) 0.0266(3) Uani 1 1 d . . . . .
Cu8 Cu 0.99555(7) 0.82323(6) 0.61334(2) 0.0256(2) Uani 1 1 d . . . . .
O1 O 0.7448(3) 0.8369(3) 0.55099(11) 0.0281(11) Uani 1 1 d . . . . .
O2 O 0.9179(4) 0.7571(3) 0.60291(11) 0.0305(12) Uani 1 1 d . . . . .
O3 O 0.5354(3) 0.8628(3) 0.58239(11) 0.0306(12) Uani 1 1 d . . . . .
O4 O 0.6577(4) 0.9866(3) 0.55436(11) 0.0344(13) Uani 1 1 d . . . . .
H4 H 0.7011 1.0105 0.5567 0.041 Uiso 1 1 calc R . . . .
O5 O 0.5418(3) 0.8395(3) 0.65573(11) 0.0271(11) Uani 1 1 d . . . . .
O6 O 0.7011(4) 0.8773(3) 0.59906(11) 0.0323(12) Uani 1 1 d . . . . .
O7 O 0.5752(3) 0.6695(3) 0.68587(10) 0.0251(11) Uani 1 1 d . . . . .
O8 O 0.3860(4) 0.7279(3) 0.65491(12) 0.0334(13) Uani 1 1 d . . . . .
H8 H 0.3802 0.7524 0.6417 0.040 Uiso 1 1 calc R . . . .
O9 O 0.7191(3) 0.5587(3) 0.64856(10) 0.0236(10) Uani 1 1 d . . . . .
O10 O 0.5698(4) 0.7167(3) 0.63553(11) 0.0290(12) Uani 1 1 d . . . . .
O11 O 0.9528(3) 0.5967(3) 0.64660(11) 0.0263(11) Uani 1 1 d . . . . .
O12 O 0.8467(4) 0.5299(3) 0.69978(12) 0.0340(13) Uani 1 1 d . . . . .
H12 H 0.7952 0.5387 0.7011 0.041 Uiso 1 1 calc R . . . .
O13 O 1.0068(3) 0.7794(3) 0.64805(11) 0.0268(11) Uani 1 1 d . . . . .
O14 O 0.8168(3) 0.6610(3) 0.66599(11) 0.0278(11) Uani 1 1 d . . . . .
O15 O 0.9474(4) 0.8868(3) 0.58971(12) 0.0309(12) Uani 1 1 d . . . . .
O16 O 1.1117(4) 0.7666(4) 0.59629(18) 0.058(2) Uani 1 1 d . . . . .
H16 H 1.1008 0.7395 0.6081 0.069 Uiso 1 1 calc R . . . .
N1 N 0.8632(4) 0.7680(3) 0.58192(13) 0.0263(13) Uani 1 1 d . . . . .
N2 N 0.5753(4) 0.8725(4) 0.53179(13) 0.0304(14) Uani 1 1 d . . . . .
N3 N 0.6587(4) 0.8814(3) 0.62103(13) 0.0263(13) Uani 1 1 d . . . . .
N4 N 0.4794(4) 0.7719(3) 0.70044(13) 0.0251(13) Uani 1 1 d . . . . .
N5 N 0.6029(4) 0.6538(3) 0.63393(12) 0.0231(12) Uani 1 1 d . . . . .
N6 N 0.8723(4) 0.4803(3) 0.64899(13) 0.0253(13) Uani 1 1 d . . . . .
N7 N 0.8816(4) 0.7054(3) 0.66796(13) 0.0251(13) Uani 1 1 d . . . . .
N8 N 1.0857(4) 0.8905(4) 0.62287(14) 0.0304(15) Uani 1 1 d . . . . .
C1 C 0.7248(5) 0.7763(4) 0.54130(15) 0.0252(15) Uani 1 1 d . . . . .
C2 C 0.6602(5) 0.7735(4) 0.52069(15) 0.0287(16) Uani 1 1 d . . . . .
C3 C 0.6339(5) 0.7130(4) 0.51066(15) 0.0291(16) Uani 1 1 d . . . . .
H3 H 0.5902 0.7120 0.4972 0.035 Uiso 1 1 calc R . . . .
C4 C 0.6691(5) 0.6534(4) 0.51966(16) 0.0300(17) Uani 1 1 d . . . . .
C5 C 0.7322(5) 0.6563(4) 0.53975(15) 0.0279(16) Uani 1 1 d . . . . .
H5 H 0.7570 0.6158 0.5460 0.033 Uiso 1 1 calc R . . . .
C6 C 0.7605(5) 0.7161(4) 0.55101(15) 0.0265(16) Uani 1 1 d . . . . .
C7 C 0.8240(5) 0.7135(4) 0.57345(15) 0.0253(15) Uani 1 1 d . . . . .
C8 C 0.8467(5) 0.6480(4) 0.58595(16) 0.0299(17) Uani 1 1 d . . . . .
H8A H 0.7997 0.6159 0.5827 0.036 Uiso 1 1 calc R . . . .
H8B H 0.8558 0.6539 0.6051 0.036 Uiso 1 1 calc R . . . .
C9 C 0.9271(6) 0.6208(5) 0.57474(19) 0.0374(19) Uani 1 1 d . . . . .
H9A H 0.9172 0.6136 0.5559 0.056 Uiso 1 1 calc GR . . . .
H9B H 0.9426 0.5785 0.5833 0.056 Uiso 1 1 calc GR . . . .
H9C H 0.9732 0.6530 0.5778 0.056 Uiso 1 1 calc GR . . . .
C10 C 0.6390(6) 0.5871(5) 0.50865(17) 0.038(2) Uani 1 1 d . . . . .
H10A H 0.5800 0.5799 0.5128 0.057 Uiso 1 1 calc GR . . . .
H10B H 0.6744 0.5513 0.5163 0.057 Uiso 1 1 calc GR . . . .
H10C H 0.6429 0.5872 0.4897 0.057 Uiso 1 1 calc GR . . . .
C11 C 0.6215(5) 0.8375(4) 0.51135(16) 0.0306(17) Uani 1 1 d . . . . .
H11A H 0.6666 0.8671 0.5054 0.037 Uiso 1 1 calc R . . . .
H11B H 0.5818 0.8284 0.4962 0.037 Uiso 1 1 calc R . . . .
C12 C 0.4974(5) 0.8346(5) 0.53782(17) 0.0335(18) Uani 1 1 d . . . . .
H12A H 0.5104 0.7864 0.5389 0.040 Uiso 1 1 calc R . . . .
H12B H 0.4531 0.8413 0.5237 0.040 Uiso 1 1 calc R . . . .
C13 C 0.4651(5) 0.8587(5) 0.56365(16) 0.0329(18) Uani 1 1 d . . . . .
H13A H 0.4382 0.9030 0.5613 0.040 Uiso 1 1 calc R . . . .
H13B H 0.4224 0.8271 0.5698 0.040 Uiso 1 1 calc R . . . .
C14 C 0.5550(6) 0.9424(5) 0.52377(18) 0.037(2) Uani 1 1 d . . . . .
H14A H 0.5085 0.9590 0.5342 0.045 Uiso 1 1 calc R . . . .
H14B H 0.5343 0.9425 0.5052 0.045 Uiso 1 1 calc R . . . .
C15 C 0.6284(6) 0.9891(4) 0.52715(17) 0.037(2) Uani 1 1 d . . . . .
H15A H 0.6742 0.9753 0.5159 0.044 Uiso 1 1 calc R . . . .
H15B H 0.6108 1.0351 0.5223 0.044 Uiso 1 1 calc R . . . .
C16 C 0.5906(5) 0.8739(3) 0.67359(15) 0.0228(15) Uani 1 1 d . . . . .
C17 C 0.5626(5) 0.8775(4) 0.69909(16) 0.0260(15) Uani 1 1 d . . . . .
C18 C 0.6113(5) 0.9101(4) 0.71840(16) 0.0290(16) Uani 1 1 d . . . . .
H18 H 0.5936 0.9101 0.7358 0.035 Uiso 1 1 calc R . . . .
C19 C 0.6862(5) 0.9429(4) 0.71269(16) 0.0286(16) Uani 1 1 d . . . . .
C20 C 0.7126(5) 0.9386(4) 0.68761(17) 0.0305(17) Uani 1 1 d . . . . .
H20 H 0.7638 0.9604 0.6837 0.037 Uiso 1 1 calc R . . . .
C21 C 0.6678(5) 0.9037(4) 0.66748(14) 0.0239(15) Uani 1 1 d . . . . .
C22 C 0.7046(4) 0.8957(4) 0.64195(15) 0.0233(15) Uani 1 1 d . . . . .
C23 C 0.7977(5) 0.9086(4) 0.63971(16) 0.0304(17) Uani 1 1 d . . . . .
H23A H 0.8206 0.8766 0.6272 0.036 Uiso 1 1 calc R . . . .
H23B H 0.8279 0.9015 0.6569 0.036 Uiso 1 1 calc R . . . .
C24 C 0.8132(6) 0.9793(5) 0.63052(19) 0.039(2) Uani 1 1 d . . . . .
H24A H 0.7880 0.9850 0.6128 0.058 Uiso 1 1 calc GR . . . .
H24B H 0.8743 0.9876 0.6306 0.058 Uiso 1 1 calc GR . . . .
H24C H 0.7874 1.0110 0.6423 0.058 Uiso 1 1 calc GR . . . .
C25 C 0.7374(6) 0.9810(6) 0.7338(2) 0.048(3) Uani 1 1 d . . . . .
H25A H 0.7007 1.0133 0.7420 0.072 Uiso 1 1 calc GR . . . .
H25B H 0.7840 1.0046 0.7260 0.072 Uiso 1 1 calc GR . . . .
H25C H 0.7604 0.9496 0.7470 0.072 Uiso 1 1 calc GR . . . .
C26 C 0.4796(5) 0.8460(4) 0.70478(16) 0.0291(16) Uani 1 1 d . . . . .
H26A H 0.4340 0.8664 0.6934 0.035 Uiso 1 1 calc R . . . .
H26B H 0.4673 0.8552 0.7231 0.035 Uiso 1 1 calc R . . . .
C27 C 0.5369(5) 0.7389(4) 0.72113(15) 0.0269(16) Uani 1 1 d . . . . .
H27A H 0.5086 0.7374 0.7378 0.032 Uiso 1 1 calc R . . . .
H27B H 0.5898 0.7650 0.7239 0.032 Uiso 1 1 calc R . . . .
C28 C 0.5576(5) 0.6684(4) 0.71250(15) 0.0257(15) Uani 1 1 d . . . . .
H28A H 0.6073 0.6512 0.7230 0.031 Uiso 1 1 calc R . . . .
H28B H 0.5090 0.6385 0.7151 0.031 Uiso 1 1 calc R . . . .
C29 C 0.3905(5) 0.7450(4) 0.70100(18) 0.0335(18) Uani 1 1 d . . . . .
H29A H 0.3928 0.6966 0.7048 0.040 Uiso 1 1 calc R . . . .
H29B H 0.3612 0.7671 0.7152 0.040 Uiso 1 1 calc R . . . .
C30 C 0.3413(5) 0.7561(5) 0.67553(18) 0.0366(19) Uani 1 1 d . . . . .
H30A H 0.2848 0.7351 0.6760 0.044 Uiso 1 1 calc R . . . .
H30B H 0.3333 0.8046 0.6725 0.044 Uiso 1 1 calc R . . . .
C31 C 0.7020(5) 0.5326(4) 0.62463(14) 0.0230(15) Uani 1 1 d . . . . .
C32 C 0.7422(5) 0.4728(4) 0.61833(17) 0.0280(16) Uani 1 1 d . . . . .
C33 C 0.7225(5) 0.4428(4) 0.59466(17) 0.0312(17) Uani 1 1 d . . . . .
H33 H 0.7499 0.4023 0.5905 0.037 Uiso 1 1 calc R . . . .
C34 C 0.6626(5) 0.4707(4) 0.57654(15) 0.0290(16) Uani 1 1 d . . . . .
C35 C 0.6257(5) 0.5312(4) 0.58250(15) 0.0282(16) Uani 1 1 d . . . . .
H35 H 0.5860 0.5509 0.5702 0.034 Uiso 1 1 calc R . . . .
C36 C 0.6454(5) 0.5641(4) 0.60627(16) 0.0257(15) Uani 1 1 d . . . . .
C37 C 0.6086(5) 0.6307(4) 0.61067(15) 0.0236(15) Uani 1 1 d . . . . .
C38 C 0.5751(5) 0.6725(4) 0.58772(16) 0.0292(16) Uani 1 1 d . . . . .
H38A H 0.5997 0.6562 0.5716 0.035 Uiso 1 1 calc R . . . .
H38B H 0.5931 0.7194 0.5905 0.035 Uiso 1 1 calc R . . . .
C39 C 0.4776(5) 0.6698(5) 0.58423(17) 0.0357(19) Uani 1 1 d . . . . .
H39A H 0.4582 0.7000 0.5701 0.053 Uiso 1 1 calc GR . . . .
H39B H 0.4530 0.6834 0.6005 0.053 Uiso 1 1 calc GR . . . .
H39C H 0.4598 0.6241 0.5798 0.053 Uiso 1 1 calc GR . . . .
C40 C 0.6374(7) 0.4336(5) 0.55169(18) 0.042(2) Uani 1 1 d . . . . .
H40A H 0.6862 0.4308 0.5408 0.063 Uiso 1 1 calc GR . . . .
H40B H 0.5913 0.4575 0.5422 0.063 Uiso 1 1 calc GR . . . .
H40C H 0.6186 0.3886 0.5560 0.063 Uiso 1 1 calc GR . . . .
C41 C 0.7984(5) 0.4386(4) 0.63871(17) 0.0289(16) Uani 1 1 d . . . . .
H41A H 0.8204 0.3969 0.6312 0.035 Uiso 1 1 calc R . . . .
H41B H 0.7641 0.4260 0.6535 0.035 Uiso 1 1 calc R . . . .
C42 C 0.9377(5) 0.4862(4) 0.62908(17) 0.0282(16) Uani 1 1 d . . . . .
H42A H 0.9099 0.4968 0.6118 0.034 Uiso 1 1 calc R . . . .
H42B H 0.9681 0.4434 0.6276 0.034 Uiso 1 1 calc R . . . .
C43 C 1.0000(5) 0.5413(4) 0.63727(16) 0.0270(16) Uani 1 1 d . . . . .
H43A H 1.0405 0.5249 0.6512 0.032 Uiso 1 1 calc R . . . .
H43B H 1.0323 0.5552 0.6222 0.032 Uiso 1 1 calc R . . . .
C44 C 0.9102(5) 0.4488(4) 0.67341(17) 0.0321(18) Uani 1 1 d . . . . .
H44A H 0.9671 0.4679 0.6774 0.039 Uiso 1 1 calc R . . . .
H44B H 0.9171 0.4003 0.6704 0.039 Uiso 1 1 calc R . . . .
C45 C 0.8569(6) 0.4590(4) 0.69646(18) 0.0346(18) Uani 1 1 d . . . . .
H45A H 0.8009 0.4374 0.6933 0.042 Uiso 1 1 calc R . . . .
H45B H 0.8850 0.4392 0.7124 0.042 Uiso 1 1 calc R . . . .
C46 C 0.9932(5) 0.8224(4) 0.66768(15) 0.0250(15) Uani 1 1 d . . . . .
C47 C 1.0455(5) 0.8800(4) 0.66950(15) 0.0249(15) Uani 1 1 d . . . . .
C48 C 1.0351(5) 0.9252(4) 0.68964(17) 0.0292(17) Uani 1 1 d . . . . .
H48 H 1.0681 0.9648 0.6904 0.035 Uiso 1 1 calc R . . . .
C49 C 0.9774(5) 0.9137(4) 0.70869(16) 0.0286(16) Uani 1 1 d . . . . .
C50 C 0.9250(5) 0.8585(4) 0.70600(15) 0.0253(15) Uani 1 1 d . . . . .
H50 H 0.8840 0.8513 0.7185 0.030 Uiso 1 1 calc R . . . .
C51 C 0.9301(5) 0.8125(4) 0.68532(16) 0.0254(15) Uani 1 1 d . . . . .
C52 C 0.8682(5) 0.7579(4) 0.68253(16) 0.0248(15) Uani 1 1 d . . . . .
C53 C 0.7866(5) 0.7607(4) 0.69624(18) 0.0310(17) Uani 1 1 d . . . . .
H53A H 0.7391 0.7471 0.6840 0.037 Uiso 1 1 calc R . . . .
H53B H 0.7761 0.8071 0.7019 0.037 Uiso 1 1 calc R . . . .
C54 C 0.7904(6) 0.7147(5) 0.71992(18) 0.039(2) Uani 1 1 d . . . . .
H54A H 0.8034 0.6692 0.7144 0.059 Uiso 1 1 calc GR . . . .
H54B H 0.7357 0.7151 0.7280 0.059 Uiso 1 1 calc GR . . . .
H54C H 0.8347 0.7302 0.7326 0.059 Uiso 1 1 calc GR . . . .
C55 C 0.9708(6) 0.9616(4) 0.73138(17) 0.0342(18) Uani 1 1 d . . . . .
H55A H 1.0275 0.9704 0.7393 0.051 Uiso 1 1 calc GR . . . .
H55B H 0.9354 0.9418 0.7444 0.051 Uiso 1 1 calc GR . . . .
H55C H 0.9453 1.0035 0.7250 0.051 Uiso 1 1 calc GR . . . .
C56 C 1.1153(5) 0.8870(5) 0.65077(18) 0.0340(18) Uani 1 1 d . . . . .
H56A H 1.1480 0.9279 0.6553 0.041 Uiso 1 1 calc R . . . .
H56B H 1.1542 0.8485 0.6532 0.041 Uiso 1 1 calc R . . . .
C57 C 1.0433(5) 0.9544(4) 0.61648(17) 0.0316(17) Uani 1 1 d . . . . .
H57A H 1.0863 0.9900 0.6155 0.038 Uiso 1 1 calc R . . . .
H57B H 1.0054 0.9662 0.6305 0.038 Uiso 1 1 calc R . . . .
C58 C 0.9920(5) 0.9499(4) 0.59066(18) 0.0344(19) Uani 1 1 d . . . . .
H58A H 0.9511 0.9872 0.5891 0.041 Uiso 1 1 calc R . . . .
H58B H 1.0300 0.9528 0.5760 0.041 Uiso 1 1 calc R . . . .
C59 C 1.1567(6) 0.8795(5) 0.6057(2) 0.040(2) Uani 1 1 d . . . . .
H59A H 1.2055 0.9072 0.6120 0.048 Uiso 1 1 calc R . . . .
H59B H 1.1392 0.8945 0.5878 0.048 Uiso 1 1 calc R . . . .
C60 C 1.1848(6) 0.8061(5) 0.6046(2) 0.047(2) Uani 1 1 d . . . . .
H60A H 1.2300 0.8009 0.5922 0.056 Uiso 1 1 calc R . . . .
H60B H 1.2073 0.7914 0.6221 0.056 Uiso 1 1 calc R . . . .
O18 O 0.3330(11) 0.8315(10) 0.4916(4) 0.066(4) Uani 0.5 1 d . . P A -1
C66 C 0.255(4) 0.8416(17) 0.4981(17) 0.081(14) Uani 0.5 1 d . . P A -1
H66A H 0.2206 0.8024 0.4925 0.097 Uiso 0.5 1 calc R . P A -1
H66B H 0.2322 0.8806 0.4881 0.097 Uiso 0.5 1 calc R . P A -1
C67 C 0.244(2) 0.8542(16) 0.5278(6) 0.077(8) Uani 0.5 1 d . . P A -1
H67A H 0.1860 0.8697 0.5303 0.116 Uiso 0.5 1 calc GR . P A -1
H67B H 0.2843 0.8882 0.5343 0.116 Uiso 0.5 1 calc GR . P A -1
H67C H 0.2540 0.8126 0.5375 0.116 Uiso 0.5 1 calc GR . P A -1
C68 C 0.341(2) 0.817(2) 0.4666(6) 0.083(9) Uani 0.5 1 d . U P A -1
H68A H 0.3163 0.8542 0.4557 0.100 Uiso 0.5 1 calc R . P A -1
H68B H 0.3085 0.7762 0.4621 0.100 Uiso 0.5 1 calc R . P A -1
C69 C 0.4366(17) 0.8073(15) 0.4607(5) 0.066(6) Uiso 0.5 1 d . . P A -1
H69A H 0.4403 0.7888 0.4431 0.100 Uiso 0.5 1 calc GR . P A -1
H69B H 0.4632 0.7764 0.4735 0.100 Uiso 0.5 1 calc GR . P A -1
H69C H 0.4660 0.8503 0.4618 0.100 Uiso 0.5 1 calc GR . P A -1
O17 O 0.3674(11) 0.7929(8) 0.7623(3) 0.117(4) Uani 1 1 d . U . . .
C61 C 0.3775(17) 0.8522(15) 0.7778(8) 0.199(15) Uani 1 1 d . U . . .
H61A H 0.3538 0.8443 0.7950 0.239 Uiso 1 1 calc R . . . .
H61B H 0.3448 0.8888 0.7691 0.239 Uiso 1 1 calc R . . . .
C62 C 0.4750(11) 0.8747(12) 0.7822(3) 0.109(6) Uani 1 1 d . U . . .
H62A H 0.5060 0.8619 0.7670 0.163 Uiso 1 1 calc GR . . . .
H62B H 0.5003 0.8527 0.7978 0.163 Uiso 1 1 calc GR . . . .
H62C H 0.4779 0.9232 0.7845 0.163 Uiso 1 1 calc GR . . . .
C63 C 0.3587(12) 0.7366(11) 0.7808(4) 0.101(5) Uani 1 1 d . U . . .
H63A H 0.4138 0.7276 0.7902 0.121 Uiso 1 1 calc R . . . .
H63B H 0.3171 0.7483 0.7938 0.121 Uiso 1 1 calc R . . . .
C64 C 0.3298(15) 0.6763(12) 0.7661(4) 0.121(7) Uani 1 1 d . U . . .
H64A H 0.3691 0.6667 0.7525 0.181 Uiso 1 1 calc GR . . . .
H64B H 0.2731 0.6841 0.7581 0.181 Uiso 1 1 calc GR . . . .
H64C H 0.3282 0.6383 0.7781 0.181 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Cu1 2.3955(15) . ?
Br2 Cu3 2.3328(16) . ?
Br3 Cu5 2.3691(15) . ?
Br4 Cu7 2.3527(17) . ?
Cu1 O1 1.910(6) . ?
Cu1 O15 1.907(6) . ?
Cu1 N1 2.001(7) . ?
Cu2 O1 2.014(6) . ?
Cu2 O3 1.903(6) . ?
Cu2 O4 2.367(6) . ?
Cu2 O6 1.879(6) . ?
Cu2 N2 2.008(7) . ?
Cu3 O3 1.885(6) . ?
Cu3 O5 1.914(6) . ?
Cu3 N3 2.023(7) . ?
Cu4 O5 1.993(6) . ?
Cu4 O7 1.905(5) . ?
Cu4 O8 2.363(6) . ?
Cu4 O10 1.870(6) . ?
Cu4 N4 1.992(7) . ?
Cu5 O7 1.898(5) . ?
Cu5 O9 1.899(5) . ?
Cu5 N5 2.008(6) . ?
Cu6 O9 1.990(5) . ?
Cu6 O11 1.900(6) . ?
Cu6 O12 2.399(6) . ?
Cu6 O14 1.867(5) . ?
Cu6 N6 1.974(7) . ?
Cu7 O11 1.884(5) . ?
Cu7 O13 1.898(6) . ?
Cu7 N7 1.991(7) . ?
Cu8 O2 1.865(6) . ?
Cu8 O13 1.984(6) . ?
Cu8 O15 1.890(6) . ?
Cu8 O16 2.369(7) . ?
Cu8 N8 2.003(7) . ?
O1 C1 1.344(10) . ?
O2 N1 1.360(8) . ?
O3 C13 1.431(9) . ?
O4 H4 0.8400 . ?
O4 C15 1.447(10) . ?
O5 C16 1.353(9) . ?
O6 N3 1.345(9) . ?
O7 C28 1.410(9) . ?
O8 H8 0.8400 . ?
O8 C30 1.422(11) . ?
O9 C31 1.348(9) . ?
O10 N5 1.369(8) . ?
O11 C43 1.435(9) . ?
O12 H12 0.8400 . ?
O12 C45 1.440(10) . ?
O13 C46 1.351(10) . ?
O14 N7 1.357(8) . ?
O15 C58 1.447(10) . ?
O16 H16 0.8400 . ?
O16 C60 1.447(11) . ?
N1 C7 1.316(11) . ?
N2 C11 1.487(11) . ?
N2 C12 1.495(11) . ?
N2 C14 1.491(11) . ?
N3 C22 1.294(10) . ?
N4 C26 1.502(10) . ?
N4 C27 1.511(10) . ?
N4 C29 1.508(10) . ?
N5 C37 1.288(10) . ?
N6 C41 1.509(9) . ?
N6 C42 1.498(10) . ?
N6 C44 1.499(10) . ?
N7 C52 1.315(10) . ?
N8 C56 1.483(11) . ?
N8 C57 1.474(11) . ?
N8 C59 1.483(11) . ?
C1 C2 1.430(11) . ?
C1 C6 1.411(11) . ?
C2 C3 1.373(12) . ?
C2 C11 1.488(12) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(12) . ?
C4 C5 1.395(11) . ?
C4 C10 1.511(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(12) . ?
C6 C7 1.486(11) . ?
C7 C8 1.496(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.526(13) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.524(12) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.495(14) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.406(11) . ?
C16 C21 1.411(11) . ?
C17 C18 1.383(12) . ?
C17 C26 1.500(11) . ?
C18 H18 0.9500 . ?
C18 C19 1.401(12) . ?
C19 C20 1.378(13) . ?
C19 C25 1.521(11) . ?
C20 H20 0.9500 . ?
C20 C21 1.406(11) . ?
C21 C22 1.472(11) . ?
C22 C23 1.506(11) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.519(12) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.522(11) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.500(13) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.402(11) . ?
C31 C36 1.412(11) . ?
C32 C33 1.376(12) . ?
C32 C41 1.500(12) . ?
C33 H33 0.9500 . ?
C33 C34 1.406(12) . ?
C34 C35 1.386(12) . ?
C34 C40 1.510(11) . ?
C35 H35 0.9500 . ?
C35 C36 1.406(11) . ?
C36 C37 1.479(11) . ?
C37 C38 1.517(11) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.543(11) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.523(11) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.505(13) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.422(11) . ?
C46 C51 1.398(12) . ?
C47 C48 1.391(12) . ?
C47 C56 1.510(12) . ?
C48 H48 0.9500 . ?
C48 C49 1.393(13) . ?
C49 C50 1.385(11) . ?
C49 C55 1.517(11) . ?
C50 H50 0.9500 . ?
C50 C51 1.411(11) . ?
C51 C52 1.469(11) . ?
C52 C53 1.506(11) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.524(13) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.517(12) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.538(14) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
O18 C66 1.31(8) . ?
O18 C68 1.32(3) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C66 C67 1.57(9) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C68 C69 1.58(4) . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
O17 C61 1.43(3) . ?
O17 C63 1.49(2) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.61(3) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.48(3) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 Br1 89.92(18) . . ?
O1 Cu1 N1 89.6(3) . . ?
O15 Cu1 Br1 92.92(18) . . ?
O15 Cu1 O1 172.2(3) . . ?
O15 Cu1 N1 89.3(3) . . ?
N1 Cu1 Br1 166.7(2) . . ?
O1 Cu2 O4 97.8(2) . . ?
O3 Cu2 O1 151.9(3) . . ?
O3 Cu2 O4 109.8(2) . . ?
O3 Cu2 N2 87.8(3) . . ?
O6 Cu2 O1 88.6(2) . . ?
O6 Cu2 O3 92.2(2) . . ?
O6 Cu2 O4 97.9(2) . . ?
O6 Cu2 N2 178.5(3) . . ?
N2 Cu2 O1 92.0(3) . . ?
N2 Cu2 O4 80.7(3) . . ?
O3 Cu3 Br2 94.78(18) . . ?
O3 Cu3 O5 171.1(3) . . ?
O3 Cu3 N3 88.5(3) . . ?
O5 Cu3 Br2 89.31(17) . . ?
O5 Cu3 N3 89.4(2) . . ?
N3 Cu3 Br2 166.5(2) . . ?
O5 Cu4 O8 99.2(2) . . ?
O7 Cu4 O5 150.1(2) . . ?
O7 Cu4 O8 110.1(2) . . ?
O7 Cu4 N4 86.9(2) . . ?
O10 Cu4 O5 89.3(2) . . ?
O10 Cu4 O7 93.4(2) . . ?
O10 Cu4 O8 94.7(2) . . ?
O10 Cu4 N4 175.2(3) . . ?
N4 Cu4 O5 92.8(3) . . ?
N4 Cu4 O8 80.7(2) . . ?
O7 Cu5 Br3 94.75(17) . . ?
O7 Cu5 O9 168.6(2) . . ?
O7 Cu5 N5 89.2(2) . . ?
O9 Cu5 Br3 91.24(17) . . ?
O9 Cu5 N5 88.4(2) . . ?
N5 Cu5 Br3 160.5(2) . . ?
O9 Cu6 O12 96.0(2) . . ?
O11 Cu6 O9 153.0(2) . . ?
O11 Cu6 O12 110.6(2) . . ?
O11 Cu6 N6 86.9(2) . . ?
O14 Cu6 O9 88.4(2) . . ?
O14 Cu6 O11 93.4(2) . . ?
O14 Cu6 O12 95.1(2) . . ?
O14 Cu6 N6 175.2(3) . . ?
N6 Cu6 O9 93.5(2) . . ?
N6 Cu6 O12 80.3(2) . . ?
O11 Cu7 Br4 96.49(16) . . ?
O11 Cu7 O13 167.5(2) . . ?
O11 Cu7 N7 88.8(3) . . ?
O13 Cu7 Br4 89.86(17) . . ?
O13 Cu7 N7 88.7(3) . . ?
N7 Cu7 Br4 160.6(2) . . ?
O2 Cu8 O13 88.1(2) . . ?
O2 Cu8 O15 93.4(2) . . ?
O2 Cu8 O16 93.8(3) . . ?
O2 Cu8 N8 175.4(3) . . ?
O13 Cu8 O16 95.0(3) . . ?
O13 Cu8 N8 93.0(3) . . ?
O15 Cu8 O13 152.4(3) . . ?
O15 Cu8 O16 112.3(3) . . ?
O15 Cu8 N8 87.6(3) . . ?
N8 Cu8 O16 81.7(3) . . ?
Cu1 O1 Cu2 116.0(3) . . ?
C1 O1 Cu1 125.7(5) . . ?
C1 O1 Cu2 107.2(5) . . ?
N1 O2 Cu8 119.6(5) . . ?
Cu3 O3 Cu2 119.4(3) . . ?
C13 O3 Cu2 112.5(5) . . ?
C13 O3 Cu3 128.1(5) . . ?
Cu2 O4 H4 127.8 . . ?
C15 O4 Cu2 104.6(5) . . ?
C15 O4 H4 109.5 . . ?
Cu3 O5 Cu4 118.2(3) . . ?
C16 O5 Cu3 124.8(5) . . ?
C16 O5 Cu4 109.7(4) . . ?
N3 O6 Cu2 119.5(5) . . ?
Cu5 O7 Cu4 118.0(3) . . ?
C28 O7 Cu4 114.1(5) . . ?
C28 O7 Cu5 127.9(5) . . ?
Cu4 O8 H8 101.1 . . ?
C30 O8 Cu4 104.7(5) . . ?
C30 O8 H8 109.5 . . ?
Cu5 O9 Cu6 119.6(3) . . ?
C31 O9 Cu5 123.7(5) . . ?
C31 O9 Cu6 112.6(5) . . ?
N5 O10 Cu4 118.7(4) . . ?
Cu7 O11 Cu6 118.3(3) . . ?
C43 O11 Cu6 113.7(5) . . ?
C43 O11 Cu7 128.0(5) . . ?
Cu6 O12 H12 91.2 . . ?
C45 O12 Cu6 104.5(5) . . ?
C45 O12 H12 109.5 . . ?
Cu7 O13 Cu8 119.2(3) . . ?
C46 O13 Cu7 123.1(5) . . ?
C46 O13 Cu8 112.2(5) . . ?
N7 O14 Cu6 117.4(4) . . ?
Cu8 O15 Cu1 118.1(3) . . ?
C58 O15 Cu1 129.1(5) . . ?
C58 O15 Cu8 112.9(5) . . ?
Cu8 O16 H16 81.1 . . ?
C60 O16 Cu8 104.6(6) . . ?
C60 O16 H16 109.5 . . ?
O2 N1 Cu1 118.2(5) . . ?
C7 N1 Cu1 128.5(5) . . ?
C7 N1 O2 113.3(6) . . ?
C11 N2 Cu2 112.6(5) . . ?
C11 N2 C12 110.5(7) . . ?
C11 N2 C14 110.9(7) . . ?
C12 N2 Cu2 102.1(5) . . ?
C14 N2 Cu2 109.0(5) . . ?
C14 N2 C12 111.5(7) . . ?
O6 N3 Cu3 118.2(5) . . ?
C22 N3 Cu3 126.4(6) . . ?
C22 N3 O6 115.2(6) . . ?
C26 N4 Cu4 113.2(5) . . ?
C26 N4 C27 109.4(6) . . ?
C26 N4 C29 110.2(6) . . ?
C27 N4 Cu4 103.0(5) . . ?
C29 N4 Cu4 110.1(5) . . ?
C29 N4 C27 110.8(6) . . ?
O10 N5 Cu5 118.1(5) . . ?
C37 N5 Cu5 126.2(5) . . ?
C37 N5 O10 115.7(6) . . ?
C41 N6 Cu6 113.7(5) . . ?
C42 N6 Cu6 103.7(5) . . ?
C42 N6 C41 110.9(6) . . ?
C42 N6 C44 110.2(6) . . ?
C44 N6 Cu6 109.4(5) . . ?
C44 N6 C41 108.9(6) . . ?
O14 N7 Cu7 119.6(5) . . ?
C52 N7 Cu7 125.3(5) . . ?
C52 N7 O14 115.0(7) . . ?
C56 N8 Cu8 112.7(5) . . ?
C56 N8 C59 111.1(7) . . ?
C57 N8 Cu8 102.8(5) . . ?
C57 N8 C56 111.8(7) . . ?
C57 N8 C59 110.3(7) . . ?
C59 N8 Cu8 107.9(5) . . ?
O1 C1 C2 116.9(7) . . ?
O1 C1 C6 124.2(7) . . ?
C6 C1 C2 118.9(7) . . ?
C1 C2 C11 118.0(7) . . ?
C3 C2 C1 120.0(8) . . ?
C3 C2 C11 122.0(7) . . ?
C2 C3 H3 119.0 . . ?
C2 C3 C4 121.9(7) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 C5 117.9(8) . . ?
C3 C4 C10 121.4(7) . . ?
C5 C4 C10 120.7(8) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 C4 122.8(8) . . ?
C6 C5 H5 118.6 . . ?
C1 C6 C7 122.8(7) . . ?
C5 C6 C1 118.5(7) . . ?
C5 C6 C7 118.7(7) . . ?
N1 C7 C6 120.8(7) . . ?
N1 C7 C8 119.3(7) . . ?
C6 C7 C8 119.8(7) . . ?
C7 C8 H8A 109.7 . . ?
C7 C8 H8B 109.7 . . ?
C7 C8 C9 109.7(7) . . ?
H8A C8 H8B 108.2 . . ?
C9 C8 H8A 109.7 . . ?
C9 C8 H8B 109.7 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C2 112.9(7) . . ?
N2 C11 H11A 109.0 . . ?
N2 C11 H11B 109.0 . . ?
C2 C11 H11A 109.0 . . ?
C2 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N2 C12 H12A 109.7 . . ?
N2 C12 H12B 109.7 . . ?
N2 C12 C13 109.9(7) . . ?
H12A C12 H12B 108.2 . . ?
C13 C12 H12A 109.7 . . ?
C13 C12 H12B 109.7 . . ?
O3 C13 C12 108.5(7) . . ?
O3 C13 H13A 110.0 . . ?
O3 C13 H13B 110.0 . . ?
C12 C13 H13A 110.0 . . ?
C12 C13 H13B 110.0 . . ?
H13A C13 H13B 108.4 . . ?
N2 C14 H14A 108.8 . . ?
N2 C14 H14B 108.8 . . ?
N2 C14 C15 113.7(7) . . ?
H14A C14 H14B 107.7 . . ?
C15 C14 H14A 108.8 . . ?
C15 C14 H14B 108.8 . . ?
O4 C15 C14 107.1(7) . . ?
O4 C15 H15A 110.3 . . ?
O4 C15 H15B 110.3 . . ?
C14 C15 H15A 110.3 . . ?
C14 C15 H15B 110.3 . . ?
H15A C15 H15B 108.5 . . ?
O5 C16 C17 117.4(7) . . ?
O5 C16 C21 122.2(7) . . ?
C17 C16 C21 120.4(7) . . ?
C16 C17 C26 118.9(7) . . ?
C18 C17 C16 119.9(7) . . ?
C18 C17 C26 121.1(7) . . ?
C17 C18 H18 119.5 . . ?
C17 C18 C19 121.0(8) . . ?
C19 C18 H18 119.5 . . ?
C18 C19 C25 120.7(8) . . ?
C20 C19 C18 118.1(7) . . ?
C20 C19 C25 121.2(8) . . ?
C19 C20 H20 118.3 . . ?
C19 C20 C21 123.3(8) . . ?
C21 C20 H20 118.3 . . ?
C16 C21 C22 122.8(7) . . ?
C20 C21 C16 117.0(7) . . ?
C20 C21 C22 120.0(7) . . ?
N3 C22 C21 122.1(7) . . ?
N3 C22 C23 118.7(7) . . ?
C21 C22 C23 119.1(7) . . ?
C22 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
C22 C23 C24 111.1(7) . . ?
H23A C23 H23B 108.0 . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C19 C25 H25A 109.5 . . ?
C19 C25 H25B 109.5 . . ?
C19 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N4 C26 H26A 109.1 . . ?
N4 C26 H26B 109.1 . . ?
C17 C26 N4 112.5(6) . . ?
C17 C26 H26A 109.1 . . ?
C17 C26 H26B 109.1 . . ?
H26A C26 H26B 107.8 . . ?
N4 C27 H27A 109.8 . . ?
N4 C27 H27B 109.8 . . ?
N4 C27 C28 109.4(6) . . ?
H27A C27 H27B 108.2 . . ?
C28 C27 H27A 109.8 . . ?
C28 C27 H27B 109.8 . . ?
O7 C28 C27 108.9(6) . . ?
O7 C28 H28A 109.9 . . ?
O7 C28 H28B 109.9 . . ?
C27 C28 H28A 109.9 . . ?
C27 C28 H28B 109.9 . . ?
H28A C28 H28B 108.3 . . ?
N4 C29 H29A 109.3 . . ?
N4 C29 H29B 109.3 . . ?
H29A C29 H29B 108.0 . . ?
C30 C29 N4 111.6(7) . . ?
C30 C29 H29A 109.3 . . ?
C30 C29 H29B 109.3 . . ?
O8 C30 C29 109.5(7) . . ?
O8 C30 H30A 109.8 . . ?
O8 C30 H30B 109.8 . . ?
C29 C30 H30A 109.8 . . ?
C29 C30 H30B 109.8 . . ?
H30A C30 H30B 108.2 . . ?
O9 C31 C32 118.1(7) . . ?
O9 C31 C36 121.4(7) . . ?
C32 C31 C36 120.5(7) . . ?
C31 C32 C41 119.3(7) . . ?
C33 C32 C31 119.6(8) . . ?
C33 C32 C41 120.7(7) . . ?
C32 C33 H33 119.3 . . ?
C32 C33 C34 121.3(8) . . ?
C34 C33 H33 119.3 . . ?
C33 C34 C40 119.9(8) . . ?
C35 C34 C33 118.6(7) . . ?
C35 C34 C40 121.5(8) . . ?
C34 C35 H35 119.1 . . ?
C34 C35 C36 121.7(7) . . ?
C36 C35 H35 119.1 . . ?
C31 C36 C37 122.9(7) . . ?
C35 C36 C31 118.1(7) . . ?
C35 C36 C37 119.0(7) . . ?
N5 C37 C36 121.0(7) . . ?
N5 C37 C38 118.7(7) . . ?
C36 C37 C38 120.3(7) . . ?
C37 C38 H38A 109.2 . . ?
C37 C38 H38B 109.2 . . ?
C37 C38 C39 111.9(7) . . ?
H38A C38 H38B 107.9 . . ?
C39 C38 H38A 109.2 . . ?
C39 C38 H38B 109.2 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C34 C40 H40A 109.5 . . ?
C34 C40 H40B 109.5 . . ?
C34 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N6 C41 H41A 108.8 . . ?
N6 C41 H41B 108.8 . . ?
C32 C41 N6 114.0(6) . . ?
C32 C41 H41A 108.8 . . ?
C32 C41 H41B 108.8 . . ?
H41A C41 H41B 107.6 . . ?
N6 C42 H42A 109.8 . . ?
N6 C42 H42B 109.8 . . ?
N6 C42 C43 109.2(6) . . ?
H42A C42 H42B 108.3 . . ?
C43 C42 H42A 109.8 . . ?
C43 C42 H42B 109.8 . . ?
O11 C43 C42 108.2(6) . . ?
O11 C43 H43A 110.1 . . ?
O11 C43 H43B 110.1 . . ?
C42 C43 H43A 110.1 . . ?
C42 C43 H43B 110.1 . . ?
H43A C43 H43B 108.4 . . ?
N6 C44 H44A 109.1 . . ?
N6 C44 H44B 109.1 . . ?
N6 C44 C45 112.6(7) . . ?
H44A C44 H44B 107.8 . . ?
C45 C44 H44A 109.1 . . ?
C45 C44 H44B 109.1 . . ?
O12 C45 C44 107.4(7) . . ?
O12 C45 H45A 110.2 . . ?
O12 C45 H45B 110.2 . . ?
C44 C45 H45A 110.2 . . ?
C44 C45 H45B 110.2 . . ?
H45A C45 H45B 108.5 . . ?
O13 C46 C47 116.7(7) . . ?
O13 C46 C51 122.8(7) . . ?
C51 C46 C47 120.5(7) . . ?
C46 C47 C56 118.5(7) . . ?
C48 C47 C46 119.0(8) . . ?
C48 C47 C56 122.3(7) . . ?
C47 C48 H48 119.2 . . ?
C47 C48 C49 121.5(7) . . ?
C49 C48 H48 119.2 . . ?
C48 C49 C55 120.6(7) . . ?
C50 C49 C48 118.3(8) . . ?
C50 C49 C55 121.0(8) . . ?
C49 C50 H50 118.7 . . ?
C49 C50 C51 122.5(8) . . ?
C51 C50 H50 118.7 . . ?
C46 C51 C50 117.8(7) . . ?
C46 C51 C52 122.6(7) . . ?
C50 C51 C52 119.6(7) . . ?
N7 C52 C51 121.6(7) . . ?
N7 C52 C53 117.7(7) . . ?
C51 C52 C53 120.7(7) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
C52 C53 C54 110.7(7) . . ?
H53A C53 H53B 108.1 . . ?
C54 C53 H53A 109.5 . . ?
C54 C53 H53B 109.5 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C49 C55 H55A 109.5 . . ?
C49 C55 H55B 109.5 . . ?
C49 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
N8 C56 C47 114.6(6) . . ?
N8 C56 H56A 108.6 . . ?
N8 C56 H56B 108.6 . . ?
C47 C56 H56A 108.6 . . ?
C47 C56 H56B 108.6 . . ?
H56A C56 H56B 107.6 . . ?
N8 C57 H57A 109.5 . . ?
N8 C57 H57B 109.5 . . ?
N8 C57 C58 110.9(7) . . ?
H57A C57 H57B 108.0 . . ?
C58 C57 H57A 109.5 . . ?
C58 C57 H57B 109.5 . . ?
O15 C58 C57 108.5(7) . . ?
O15 C58 H58A 110.0 . . ?
O15 C58 H58B 110.0 . . ?
C57 C58 H58A 110.0 . . ?
C57 C58 H58B 110.0 . . ?
H58A C58 H58B 108.4 . . ?
N8 C59 H59A 109.0 . . ?
N8 C59 H59B 109.0 . . ?
N8 C59 C60 113.1(8) . . ?
H59A C59 H59B 107.8 . . ?
C60 C59 H59A 109.0 . . ?
C60 C59 H59B 109.0 . . ?
O16 C60 C59 107.8(8) . . ?
O16 C60 H60A 110.1 . . ?
O16 C60 H60B 110.1 . . ?
C59 C60 H60A 110.1 . . ?
C59 C60 H60B 110.1 . . ?
H60A C60 H60B 108.5 . . ?
C66 O18 C68 115(4) . . ?
O18 C66 H66A 108.4 . . ?
O18 C66 H66B 108.4 . . ?
O18 C66 C67 116(5) . . ?
H66A C66 H66B 107.4 . . ?
C67 C66 H66A 108.4 . . ?
C67 C66 H66B 108.4 . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
O18 C68 H68A 109.5 . . ?
O18 C68 H68B 109.5 . . ?
O18 C68 C69 111(2) . . ?
H68A C68 H68B 108.1 . . ?
C69 C68 H68A 109.5 . . ?
C69 C68 H68B 109.5 . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C61 O17 C63 107(2) . . ?
O17 C61 H61A 109.1 . . ?
O17 C61 H61B 109.1 . . ?
O17 C61 C62 113(2) . . ?
H61A C61 H61B 107.8 . . ?
C62 C61 H61A 109.1 . . ?
C62 C61 H61B 109.1 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O17 C63 H63A 109.8 . . ?
O17 C63 H63B 109.8 . . ?
H63A C63 H63B 108.2 . . ?
C64 C63 O17 109.4(16) . . ?
C64 C63 H63A 109.8 . . ?
C64 C63 H63B 109.8 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 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
Br2 Cu3 O3 Cu2 174.6(3) . . . . ?
Br2 Cu3 O3 C13 -6.3(7) . . . . ?
Br3 Cu5 O7 Cu4 -170.6(3) . . . . ?
Br3 Cu5 O7 C28 11.3(6) . . . . ?
Br3 Cu5 O9 Cu6 -86.5(3) . . . . ?
Br3 Cu5 O9 C31 118.0(5) . . . . ?
Br4 Cu7 O11 Cu6 167.6(3) . . . . ?
Br4 Cu7 O11 C43 -11.6(6) . . . . ?
Br4 Cu7 O13 Cu8 89.6(3) . . . . ?
Br4 Cu7 O13 C46 -118.6(5) . . . . ?
Cu1 O1 C1 C2 -155.6(5) . . . . ?
Cu1 O1 C1 C6 27.6(11) . . . . ?
Cu1 O15 C58 C57 160.3(6) . . . . ?
Cu1 N1 C7 C6 -0.4(11) . . . . ?
Cu1 N1 C7 C8 177.1(6) . . . . ?
Cu2 O1 C1 C2 62.3(7) . . . . ?
Cu2 O1 C1 C6 -114.5(7) . . . . ?
Cu2 O3 C13 C12 24.1(8) . . . . ?
Cu2 O4 C15 C14 36.5(8) . . . . ?
Cu2 O6 N3 Cu3 16.9(7) . . . . ?
Cu2 O6 N3 C22 -168.0(5) . . . . ?
Cu2 N2 C11 C2 44.6(8) . . . . ?
Cu2 N2 C12 C13 43.5(7) . . . . ?
Cu2 N2 C14 C15 46.3(9) . . . . ?
Cu3 O3 C13 C12 -155.1(6) . . . . ?
Cu3 O5 C16 C17 150.9(5) . . . . ?
Cu3 O5 C16 C21 -30.8(9) . . . . ?
Cu3 N3 C22 C21 -6.9(10) . . . . ?
Cu3 N3 C22 C23 176.8(5) . . . . ?
Cu4 O5 C16 C17 -59.6(7) . . . . ?
Cu4 O5 C16 C21 118.7(6) . . . . ?
Cu4 O7 C28 C27 -21.0(7) . . . . ?
Cu4 O8 C30 C29 -35.2(8) . . . . ?
Cu4 O10 N5 Cu5 -18.0(7) . . . . ?
Cu4 O10 N5 C37 162.7(5) . . . . ?
Cu4 N4 C26 C17 -44.6(8) . . . . ?
Cu4 N4 C27 C28 -42.8(7) . . . . ?
Cu4 N4 C29 C30 -45.3(8) . . . . ?
Cu5 O7 C28 C27 157.2(5) . . . . ?
Cu5 O9 C31 C32 -147.1(6) . . . . ?
Cu5 O9 C31 C36 33.0(9) . . . . ?
Cu5 N5 C37 C36 -0.9(10) . . . . ?
Cu5 N5 C37 C38 178.0(5) . . . . ?
Cu6 O9 C31 C32 55.9(8) . . . . ?
Cu6 O9 C31 C36 -124.0(6) . . . . ?
Cu6 O11 C43 C42 19.4(8) . . . . ?
Cu6 O12 C45 C44 33.8(7) . . . . ?
Cu6 O14 N7 Cu7 18.9(7) . . . . ?
Cu6 O14 N7 C52 -158.9(5) . . . . ?
Cu6 N6 C41 C32 43.5(8) . . . . ?
Cu6 N6 C42 C43 44.1(7) . . . . ?
Cu6 N6 C44 C45 50.3(8) . . . . ?
Cu7 O11 C43 C42 -161.3(5) . . . . ?
Cu7 O13 C46 C47 149.3(5) . . . . ?
Cu7 O13 C46 C51 -32.0(9) . . . . ?
Cu7 N7 C52 C51 6.2(10) . . . . ?
Cu7 N7 C52 C53 -174.3(5) . . . . ?
Cu8 O2 N1 Cu1 -13.8(7) . . . . ?
Cu8 O2 N1 C7 167.1(5) . . . . ?
Cu8 O13 C46 C47 -57.2(7) . . . . ?
Cu8 O13 C46 C51 121.6(7) . . . . ?
Cu8 O15 C58 C57 -20.1(9) . . . . ?
Cu8 O16 C60 C59 -32.2(10) . . . . ?
Cu8 N8 C56 C47 -44.0(9) . . . . ?
Cu8 N8 C57 C58 -42.6(8) . . . . ?
Cu8 N8 C59 C60 -49.5(9) . . . . ?
O1 Cu2 O6 N3 -161.2(6) . . . . ?
O1 C1 C2 C3 -177.1(7) . . . . ?
O1 C1 C2 C11 1.1(11) . . . . ?
O1 C1 C6 C5 177.9(7) . . . . ?
O1 C1 C6 C7 0.7(12) . . . . ?
O2 Cu8 O15 Cu1 1.1(4) . . . . ?
O2 Cu8 O15 C58 -178.5(6) . . . . ?
O2 N1 C7 C6 178.7(7) . . . . ?
O2 N1 C7 C8 -3.9(10) . . . . ?
O3 Cu2 O6 N3 -9.3(6) . . . . ?
O4 Cu2 O6 N3 101.1(6) . . . . ?
O5 Cu4 O10 N5 159.1(5) . . . . ?
O5 C16 C17 C18 177.8(7) . . . . ?
O5 C16 C17 C26 -2.4(10) . . . . ?
O5 C16 C21 C20 179.5(7) . . . . ?
O5 C16 C21 C22 -4.8(11) . . . . ?
O6 N3 C22 C21 178.4(6) . . . . ?
O6 N3 C22 C23 2.2(10) . . . . ?
O7 Cu4 O10 N5 8.9(5) . . . . ?
O7 Cu5 O9 Cu6 35.2(13) . . . . ?
O7 Cu5 O9 C31 -120.3(11) . . . . ?
O8 Cu4 O10 N5 -101.6(5) . . . . ?
O9 Cu5 O7 Cu4 68.1(12) . . . . ?
O9 Cu5 O7 C28 -110.1(12) . . . . ?
O9 Cu6 O14 N7 -164.4(5) . . . . ?
O9 C31 C32 C33 176.2(7) . . . . ?
O9 C31 C32 C41 3.4(11) . . . . ?
O9 C31 C36 C35 -175.1(7) . . . . ?
O9 C31 C36 C37 6.9(11) . . . . ?
O10 N5 C37 C36 178.3(6) . . . . ?
O10 N5 C37 C38 -2.8(10) . . . . ?
O11 Cu6 O14 N7 -11.4(5) . . . . ?
O11 Cu7 O13 Cu8 -31.1(13) . . . . ?
O11 Cu7 O13 C46 120.7(11) . . . . ?
O12 Cu6 O14 N7 99.7(5) . . . . ?
O13 Cu7 O11 Cu6 -72.3(12) . . . . ?
O13 Cu7 O11 C43 108.5(12) . . . . ?
O13 Cu8 O2 N1 160.2(6) . . . . ?
O13 Cu8 O15 Cu1 -91.4(6) . . . . ?
O13 Cu8 O15 C58 89.0(7) . . . . ?
O13 C46 C47 C48 -178.9(7) . . . . ?
O13 C46 C47 C56 -3.9(10) . . . . ?
O13 C46 C51 C50 176.2(7) . . . . ?
O13 C46 C51 C52 -5.8(11) . . . . ?
O14 N7 C52 C51 -176.2(6) . . . . ?
O14 N7 C52 C53 3.3(10) . . . . ?
O15 Cu8 O2 N1 7.7(6) . . . . ?
O16 Cu8 O2 N1 -104.9(6) . . . . ?
O16 Cu8 O15 Cu1 96.7(4) . . . . ?
O16 Cu8 O15 C58 -83.0(6) . . . . ?
N1 C7 C8 C9 -80.8(9) . . . . ?
N2 C12 C13 O3 -46.3(9) . . . . ?
N2 C14 C15 O4 -57.5(10) . . . . ?
N3 Cu3 O3 Cu2 7.7(4) . . . . ?
N3 Cu3 O3 C13 -173.2(7) . . . . ?
N3 C22 C23 C24 80.9(9) . . . . ?
N4 C27 C28 O7 43.1(8) . . . . ?
N4 C29 C30 O8 55.4(9) . . . . ?
N5 Cu5 O7 Cu4 -9.8(3) . . . . ?
N5 Cu5 O7 C28 172.1(6) . . . . ?
N5 Cu5 O9 Cu6 113.1(3) . . . . ?
N5 Cu5 O9 C31 -42.4(6) . . . . ?
N5 C37 C38 C39 -77.3(9) . . . . ?
N6 C42 C43 O11 -42.6(9) . . . . ?
N6 C44 C45 O12 -57.4(9) . . . . ?
N7 Cu7 O11 Cu6 6.3(3) . . . . ?
N7 Cu7 O11 C43 -172.9(6) . . . . ?
N7 Cu7 O13 Cu8 -109.7(3) . . . . ?
N7 Cu7 O13 C46 42.1(5) . . . . ?
N7 C52 C53 C54 76.3(9) . . . . ?
N8 Cu8 O15 Cu1 176.7(4) . . . . ?
N8 Cu8 O15 C58 -2.9(6) . . . . ?
N8 C57 C58 O15 42.9(9) . . . . ?
N8 C59 C60 O16 56.6(11) . . . . ?
C1 C2 C3 C4 -1.0(12) . . . . ?
C1 C2 C11 N2 -63.6(10) . . . . ?
C1 C6 C7 N1 -14.3(12) . . . . ?
C1 C6 C7 C8 168.3(7) . . . . ?
C2 C1 C6 C5 1.2(11) . . . . ?
C2 C1 C6 C7 -176.1(7) . . . . ?
C2 C3 C4 C5 0.9(12) . . . . ?
C2 C3 C4 C10 179.3(8) . . . . ?
C3 C2 C11 N2 114.6(9) . . . . ?
C3 C4 C5 C6 0.3(12) . . . . ?
C4 C5 C6 C1 -1.3(12) . . . . ?
C4 C5 C6 C7 176.1(7) . . . . ?
C5 C6 C7 N1 168.4(7) . . . . ?
C5 C6 C7 C8 -9.0(11) . . . . ?
C6 C1 C2 C3 -0.1(12) . . . . ?
C6 C1 C2 C11 178.0(7) . . . . ?
C6 C7 C8 C9 96.7(9) . . . . ?
C10 C4 C5 C6 -178.2(8) . . . . ?
C11 N2 C12 C13 163.5(7) . . . . ?
C11 N2 C14 C15 -78.2(9) . . . . ?
C11 C2 C3 C4 -179.1(8) . . . . ?
C12 N2 C11 C2 -68.9(9) . . . . ?
C12 N2 C14 C15 158.3(7) . . . . ?
C14 N2 C11 C2 167.0(7) . . . . ?
C14 N2 C12 C13 -72.7(8) . . . . ?
C16 C17 C18 C19 3.6(11) . . . . ?
C16 C17 C26 N4 62.3(9) . . . . ?
C16 C21 C22 N3 24.1(11) . . . . ?
C16 C21 C22 C23 -159.6(7) . . . . ?
C17 C16 C21 C20 -2.2(10) . . . . ?
C17 C16 C21 C22 173.5(7) . . . . ?
C17 C18 C19 C20 -3.6(12) . . . . ?
C17 C18 C19 C25 177.4(8) . . . . ?
C18 C17 C26 N4 -118.0(8) . . . . ?
C18 C19 C20 C21 0.7(12) . . . . ?
C19 C20 C21 C16 2.2(12) . . . . ?
C19 C20 C21 C22 -173.7(7) . . . . ?
C20 C21 C22 N3 -160.3(7) . . . . ?
C20 C21 C22 C23 15.9(10) . . . . ?
C21 C16 C17 C18 -0.5(11) . . . . ?
C21 C16 C17 C26 179.2(7) . . . . ?
C21 C22 C23 C24 -95.5(8) . . . . ?
C25 C19 C20 C21 179.7(8) . . . . ?
C26 N4 C27 C28 -163.4(6) . . . . ?
C26 N4 C29 C30 80.2(8) . . . . ?
C26 C17 C18 C19 -176.2(7) . . . . ?
C27 N4 C26 C17 69.6(8) . . . . ?
C27 N4 C29 C30 -158.6(7) . . . . ?
C29 N4 C26 C17 -168.4(7) . . . . ?
C29 N4 C27 C28 75.0(8) . . . . ?
C31 C32 C33 C34 0.1(12) . . . . ?
C31 C32 C41 N6 -59.9(10) . . . . ?
C31 C36 C37 N5 -23.1(11) . . . . ?
C31 C36 C37 C38 158.0(7) . . . . ?
C32 C31 C36 C35 5.1(11) . . . . ?
C32 C31 C36 C37 -173.0(7) . . . . ?
C32 C33 C34 C35 2.5(13) . . . . ?
C32 C33 C34 C40 -175.2(8) . . . . ?
C33 C32 C41 N6 127.4(8) . . . . ?
C33 C34 C35 C36 -1.3(12) . . . . ?
C34 C35 C36 C31 -2.4(12) . . . . ?
C34 C35 C36 C37 175.7(7) . . . . ?
C35 C36 C37 N5 158.9(7) . . . . ?
C35 C36 C37 C38 -20.0(11) . . . . ?
C36 C31 C32 C33 -3.9(12) . . . . ?
C36 C31 C32 C41 -176.8(7) . . . . ?
C36 C37 C38 C39 101.6(8) . . . . ?
C40 C34 C35 C36 176.4(8) . . . . ?
C41 N6 C42 C43 166.5(6) . . . . ?
C41 N6 C44 C45 -74.6(9) . . . . ?
C41 C32 C33 C34 172.8(8) . . . . ?
C42 N6 C41 C32 -72.8(9) . . . . ?
C42 N6 C44 C45 163.6(7) . . . . ?
C44 N6 C41 C32 165.8(7) . . . . ?
C44 N6 C42 C43 -72.9(8) . . . . ?
C46 C47 C48 C49 3.0(11) . . . . ?
C46 C47 C56 N8 62.0(10) . . . . ?
C46 C51 C52 N7 18.8(12) . . . . ?
C46 C51 C52 C53 -160.7(7) . . . . ?
C47 C46 C51 C50 -5.0(11) . . . . ?
C47 C46 C51 C52 172.9(7) . . . . ?
C47 C48 C49 C50 -5.3(12) . . . . ?
C47 C48 C49 C55 176.4(7) . . . . ?
C48 C47 C56 N8 -123.2(8) . . . . ?
C48 C49 C50 C51 2.4(12) . . . . ?
C49 C50 C51 C46 2.7(11) . . . . ?
C49 C50 C51 C52 -175.3(7) . . . . ?
C50 C51 C52 N7 -163.3(7) . . . . ?
C50 C51 C52 C53 17.2(11) . . . . ?
C51 C46 C47 C48 2.3(11) . . . . ?
C51 C46 C47 C56 177.3(7) . . . . ?
C51 C52 C53 C54 -104.1(8) . . . . ?
C55 C49 C50 C51 -179.2(7) . . . . ?
C56 N8 C57 C58 -163.6(7) . . . . ?
C56 N8 C59 C60 74.5(9) . . . . ?
C56 C47 C48 C49 -171.8(7) . . . . ?
C57 N8 C56 C47 71.1(9) . . . . ?
C57 N8 C59 C60 -161.0(8) . . . . ?
C59 N8 C56 C47 -165.2(7) . . . . ?
C59 N8 C57 C58 72.3(9) . . . . ?
C66 O18 C68 C69 179(3) . . . . ?
C68 O18 C66 C67 176(3) . . . . ?
C61 O17 C63 C64 167.9(19) . . . . ?
C63 O17 C61 C62 99(3) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5 6 -23 0.0279 -5.4249 5.7765 -23.0713 0.0442 -0.0226 0.9988
-8 -8 6 0.0132 -8.1797 -7.6935 5.7555 -0.8969 0.4269 0.1150
6 -5 23 0.0246 5.8760 -5.2915 22.6038 0.0088 -0.0026 -1.0000
8 8 -7 0.0214 7.9374 7.9841 -6.8667 0.9008 -0.4289 -0.0676
-4 -3 -29 0.0197 -4.0878 -3.2422 -28.6099 0.0178 0.6573 0.7534
4 5 28 0.0174 3.5404 4.7003 28.1610 -0.0199 -0.7463 -0.6653
3 -12 -3 0.0155 3.3812 -12.2433 -3.0136 0.0211 0.8525 -0.5223
-4 -1 5 0.0171 -4.0000 -1.0000 4.9993 -0.4057 -0.0073 0.0967

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id JF3041
_olex2_submission_special_instructions 'No special instructions were received'
