# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 953617'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2014-12-23 downloaded from the CCDC.
;

_audit_creation_date             2013-07-23T13:00:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            DDJS-48
_chemical_formula_moiety         'C35 H41 Cu3 N5 O10, 2(Cl O4)'
_chemical_formula_sum            'C35 H41 Cl2 Cu3 N5 O18'
_chemical_formula_weight         1081.25
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   11.1962(5)
_cell_length_b                   15.1146(7)
_cell_length_c                   11.9446(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.215(2)
_cell_angle_gamma                90
_cell_volume                     2015.87(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7595
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      25.81
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1102
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1
;
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_T_max  0.875
_shelx_estimated_absorpt_T_min   0.775
_shelx_estimated_absorpt_T_max   0.9

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'sealed x-ray tube'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'APEX-II CCD'
_diffrn_orient_matrix_ub_11      -0.006636
_diffrn_orient_matrix_ub_12      -0.002115
_diffrn_orient_matrix_ub_13      0.08299
_diffrn_orient_matrix_ub_21      -0.023016
_diffrn_orient_matrix_ub_22      0.063934
_diffrn_orient_matrix_ub_23      -0.00059
_diffrn_orient_matrix_ub_31      -0.086295
_diffrn_orient_matrix_ub_32      -0.016889
_diffrn_orient_matrix_ub_33      -0.012627
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'φ or ω oscillation scans'
_diffrn_reflns_av_R_equivalents  0.09
_diffrn_reflns_number            19831
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.824
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.99
_reflns_number_total             19831
_reflns_number_gt                16358
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 software'
_computing_cell_refinement       'SAINT V8.32B integration software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_structure_solution    'SIR-2011 (Burla et al., 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refined as a 5-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0644P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         19831
_refine_ls_number_parameters     578
_refine_ls_number_restraints     1497
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0525
_refine_ls_wR_factor_ref         0.1314
_refine_ls_wR_factor_gt          0.1168
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.981
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Flack x determined using 2366 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.034(11)
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.146

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu -0.03123(12) 0.18756(9) 0.53217(12) 0.0080(4) Uani 1 d . .
Cu2 Cu 0.22985(12) 0.20639(9) 0.42918(12) 0.0082(4) Uani 1 d . .
Cu3 Cu 0.54531(12) 0.34033(10) 0.56131(12) 0.0071(4) Uani 1 d . .
N1 N -0.0086(8) 0.1309(7) 0.6752(8) 0.0090(17) Uani 1 d . .
C2 C 0.0972(10) 0.1362(8) 0.7348(10) 0.0093(19) Uani 1 d . .
C3 C 0.1116(10) 0.1059(8) 0.8442(10) 0.010(2) Uani 1 d . .
H3 H 0.1871 0.1082 0.8859 0.012 Uiso 1 calc . .
C4 C 0.0121(11) 0.0725(8) 0.8899(10) 0.012(2) Uani 1 d . .
H4 H 0.018 0.0539 0.9661 0.014 Uiso 1 calc . .
C5 C -0.0966(10) 0.0652(8) 0.8273(10) 0.009(2) Uani 1 d . .
H5 H -0.1646 0.0408 0.8591 0.01 Uiso 1 calc . .
C6 C -0.1037(10) 0.0942(8) 0.7183(10) 0.010(2) Uani 1 d . .
C7 C 0.1914(9) 0.1807(9) 0.6686(9) 0.010(2) Uani 1 d . .
H7A H 0.2224 0.2337 0.71 0.013 Uiso 1 calc . .
H7B H 0.2592 0.1395 0.6617 0.013 Uiso 1 calc . .
O8 O 0.1444(6) 0.2063(6) 0.5598(6) 0.0104(17) Uani 1 d . .
C9 C -0.2095(10) 0.0898(8) 0.6332(9) 0.009(2) Uani 1 d . .
H9A H -0.2119 0.0311 0.5963 0.011 Uiso 1 calc . .
H9B H -0.2844 0.0971 0.6716 0.011 Uiso 1 calc . .
O10 O -0.2022(7) 0.1574(5) 0.5505(6) 0.0090(17) Uani 1 d . .
H10 H -0.2255 0.2057 0.5763 0.014 Uiso 1 calc . .
N11 N -0.0519(8) 0.2478(7) 0.3823(8) 0.0088(18) Uani 1 d . .
C12 C -0.0559(9) 0.2014(8) 0.2866(9) 0.0094(19) Uani 1 d . .
C13 C -0.0610(11) 0.2412(8) 0.1832(10) 0.013(2) Uani 1 d . .
H13 H -0.0639 0.2067 0.1165 0.016 Uiso 1 calc . .
C14 C -0.0618(10) 0.3330(9) 0.1778(10) 0.016(2) Uani 1 d . .
H14 H -0.0644 0.3624 0.1074 0.019 Uiso 1 calc . .
C15 C -0.0589(10) 0.3798(8) 0.2743(10) 0.011(2) Uani 1 d . .
H15 H -0.0633 0.4426 0.272 0.014 Uiso 1 calc . .
C16 C -0.0496(10) 0.3361(8) 0.3764(9) 0.0099(19) Uani 1 d . .
C17 C -0.0658(10) 0.1017(8) 0.2995(10) 0.011(2) Uani 1 d . .
H17A H -0.1515 0.0848 0.2918 0.013 Uiso 1 calc . .
H17B H -0.026 0.0727 0.2379 0.013 Uiso 1 calc . .
O18 O -0.0144(7) 0.0698(6) 0.4031(7) 0.0125(18) Uani 1 d . .
H18 H 0.0606 0.0722 0.4035 0.019 Uiso 1 calc . .
C19 C -0.0376(11) 0.3898(8) 0.4826(10) 0.012(2) Uani 1 d . .
H19A H 0.0447 0.4139 0.4934 0.015 Uiso 1 calc . .
H19B H -0.0941 0.4403 0.4762 0.015 Uiso 1 calc . .
O20 O -0.0623(7) 0.3365(6) 0.5777(7) 0.0172(19) Uani 1 d . .
H20 H -0.0211 0.3546 0.6348 0.026 Uiso 1 calc . .
N21 N 0.2664(8) 0.2107(6) 0.2751(7) 0.0070(16) Uani 1 d . .
C22 C 0.2795(10) 0.2904(8) 0.2273(10) 0.0096(19) Uani 1 d . .
C23 C 0.3023(10) 0.2958(8) 0.1155(10) 0.011(2) Uani 1 d . .
H23 H 0.3102 0.3514 0.0796 0.013 Uiso 1 calc . .
C24 C 0.3134(10) 0.2176(8) 0.0577(10) 0.013(2) Uani 1 d . .
H24 H 0.3304 0.2196 -0.019 0.015 Uiso 1 calc . .
C25 C 0.3002(10) 0.1356(9) 0.1090(10) 0.011(2) Uani 1 d . .
H25 H 0.3077 0.0822 0.0682 0.013 Uiso 1 calc . .
C26 C 0.2763(10) 0.1343(8) 0.2193(10) 0.0094(19) Uani 1 d . .
C27 C 0.2634(10) 0.3664(7) 0.3054(9) 0.008(2) Uani 1 d . .
H27A H 0.337 0.4029 0.311 0.01 Uiso 1 calc . .
H27B H 0.1964 0.404 0.2747 0.01 Uiso 1 calc . .
O28 O 0.2395(6) 0.3368(6) 0.4125(6) 0.0098(16) Uani 1 d . .
C29 C 0.2550(11) 0.0548(8) 0.2890(10) 0.011(2) Uani 1 d . .
H29A H 0.1901 0.0189 0.251 0.013 Uiso 1 calc . .
H29B H 0.3285 0.0182 0.2954 0.013 Uiso 1 calc . .
O30 O 0.2222(7) 0.0781(5) 0.4012(7) 0.0089(17) Uani 1 d . .
N31 N 0.5686(8) 0.3037(6) 0.4049(8) 0.0081(17) Uani 1 d . .
C32 C 0.5528(10) 0.2194(8) 0.3692(9) 0.0089(19) Uani 1 d . .
C33 C 0.5747(9) 0.1936(9) 0.2621(9) 0.011(2) Uani 1 d . .
H33 H 0.5632 0.1337 0.2394 0.013 Uiso 1 calc . .
C34 C 0.6138(11) 0.2562(8) 0.1869(11) 0.013(2) Uani 1 d . .
H34 H 0.6288 0.2402 0.1124 0.015 Uiso 1 calc . .
C35 C 0.6299(10) 0.3425(9) 0.2242(10) 0.013(2) Uani 1 d . .
H35 H 0.6544 0.3868 0.1744 0.016 Uiso 1 calc . .
C36 C 0.6105(10) 0.3641(8) 0.3341(9) 0.0089(19) Uani 1 d . .
C37 C 0.5129(10) 0.1529(8) 0.4533(10) 0.010(2) Uani 1 d . .
H37A H 0.4718 0.103 0.413 0.012 Uiso 1 calc . .
H37B H 0.5839 0.129 0.4976 0.012 Uiso 1 calc . .
O38 O 0.4329(6) 0.1930(6) 0.5279(6) 0.0112(17) Uani 1 d . .
H38 H 0.451 0.176 0.5939 0.017 Uiso 1 calc . .
C39 C 0.6282(11) 0.4562(8) 0.3756(10) 0.013(2) Uani 1 d . .
H39A H 0.6957 0.484 0.3397 0.016 Uiso 1 calc . .
H39B H 0.5551 0.4916 0.3564 0.016 Uiso 1 calc . .
O40 O 0.6533(7) 0.4537(6) 0.4950(7) 0.0134(18) Uani 1 d . .
H40 H 0.7156 0.483 0.5126 0.02 Uiso 1 calc . .
N41 N 0.5264(8) 0.3690(6) 0.7141(8) 0.0100(17) Uani 1 d . .
C42 C 0.6145(10) 0.3469(9) 0.7918(10) 0.012(2) Uani 1 d . .
C43 C 0.6063(10) 0.3692(8) 0.9020(10) 0.012(2) Uani 1 d . .
H43 H 0.6678 0.3534 0.9574 0.014 Uiso 1 calc . .
C44 C 0.5051(11) 0.4159(8) 0.9310(11) 0.015(2) Uani 1 d . .
H44 H 0.4978 0.4322 1.007 0.018 Uiso 1 calc . .
C45 C 0.4158(11) 0.4384(9) 0.8503(10) 0.014(2) Uani 1 d . .
H45 H 0.3465 0.4695 0.8696 0.017 Uiso 1 calc . .
C46 C 0.4302(10) 0.4143(8) 0.7404(10) 0.011(2) Uani 1 d . .
C47 C 0.7141(10) 0.2940(9) 0.7433(10) 0.013(2) Uani 1 d . .
H47A H 0.7895 0.3284 0.7498 0.015 Uiso 1 calc . .
H47B H 0.7273 0.2381 0.7857 0.015 Uiso 1 calc . .
O48 O 0.6813(7) 0.2750(5) 0.6280(7) 0.0108(18) Uani 1 d . .
C49 C 0.3420(10) 0.4345(9) 0.6417(10) 0.013(2) Uani 1 d . .
H49A H 0.2659 0.4027 0.6502 0.015 Uiso 1 calc . .
H49B H 0.3247 0.4988 0.6389 0.015 Uiso 1 calc . .
O50 O 0.3916(7) 0.4074(5) 0.5395(7) 0.0090(17) Uani 1 d . .
H50 H 0.341 0.377 0.501 0.014 Uiso 1 calc . .
Cl1 Cl 0.5161(3) 0.0949(2) 0.8499(3) 0.0113(7) Uani 1 d . .
O51 O 0.5114(7) 0.1499(6) 0.7509(7) 0.020(2) Uani 1 d . .
O52 O 0.5642(7) 0.1444(6) 0.9439(7) 0.022(2) Uani 1 d . .
O53 O 0.5897(7) 0.0192(6) 0.8318(7) 0.018(2) Uani 1 d . .
O54 O 0.3963(7) 0.0648(6) 0.8688(7) 0.015(2) Uani 1 d . .
Cl2 Cl 0.0521(3) 0.3875(2) 0.8810(3) 0.0167(8) Uani 1 d . .
O55 O 0.1378(8) 0.4373(7) 0.9503(8) 0.030(2) Uani 1 d . .
O56 O -0.0620(8) 0.4294(6) 0.8838(8) 0.022(2) Uani 1 d . .
O57 O 0.0478(10) 0.3002(7) 0.9231(9) 0.037(3) Uani 1 d . .
O58 O 0.0875(8) 0.3854(7) 0.7667(7) 0.028(2) Uani 1 d . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 N1 1.911(10) . ?
Cu1 O8 1.990(7) . ?
Cu1 N11 2.006(10) . ?
Cu2 O8 1.889(7) . ?
Cu2 N21 1.915(9) . ?
Cu2 O30 1.968(8) . ?
Cu2 O28 1.984(9) . ?
Cu3 N41 1.903(10) . ?
Cu3 O48 1.936(8) . ?
Cu3 N31 1.984(10) . ?
N1 C6 1.338(13) . ?
N1 C2 1.339(13) . ?
C2 C3 1.383(15) . ?
C2 C7 1.521(14) . ?
C3 C4 1.372(15) . ?
C3 H3 0.95 . ?
C4 C5 1.386(14) . ?
C4 H4 0.95 . ?
C5 C6 1.369(14) . ?
C5 H5 0.95 . ?
C6 C9 1.505(14) . ?
C7 O8 1.420(12) . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C9 O10 1.427(12) . ?
C9 H9A 0.99 . ?
C9 H9B 0.99 . ?
O10 H10 0.84 . ?
N11 C16 1.338(14) . ?
N11 C12 1.339(13) . ?
C12 C13 1.372(14) . ?
C12 C17 1.520(15) . ?
C13 C14 1.389(16) . ?
C13 H13 0.95 . ?
C14 C15 1.351(15) . ?
C14 H14 0.95 . ?
C15 C16 1.385(14) . ?
C15 H15 0.95 . ?
C16 C19 1.503(15) . ?
C17 O18 1.411(12) . ?
C17 H17A 0.99 . ?
C17 H17B 0.99 . ?
O18 H18 0.84 . ?
C19 O20 1.436(13) . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
O20 H20 0.84 . ?
N21 C26 1.342(14) . ?
N21 C22 1.346(14) . ?
C22 C23 1.380(15) . ?
C22 C27 1.500(15) . ?
C23 C24 1.378(15) . ?
C23 H23 0.95 . ?
C24 C25 1.394(16) . ?
C24 H24 0.95 . ?
C25 C26 1.364(15) . ?
C25 H25 0.95 . ?
C26 C29 1.491(15) . ?
C27 O28 1.400(12) . ?
C27 H27A 0.99 . ?
C27 H27B 0.99 . ?
C29 O30 1.459(13) . ?
C29 H29A 0.99 . ?
C29 H29B 0.99 . ?
N31 C36 1.351(13) . ?
N31 C32 1.352(14) . ?
C32 C33 1.376(14) . ?
C32 C37 1.512(14) . ?
C33 C34 1.397(15) . ?
C33 H33 0.95 . ?
C34 C35 1.385(16) . ?
C34 H34 0.95 . ?
C35 C36 1.386(14) . ?
C35 H35 0.95 . ?
C36 C39 1.486(15) . ?
C37 O38 1.443(12) . ?
C37 H37A 0.99 . ?
C37 H37B 0.99 . ?
O38 H38 0.84 . ?
C39 O40 1.434(13) . ?
C39 H39A 0.99 . ?
C39 H39B 0.99 . ?
O40 H40 0.84 . ?
N41 C46 1.333(13) . ?
N41 C42 1.347(13) . ?
C42 C43 1.368(14) . ?
C42 C47 1.521(15) . ?
C43 C44 1.400(15) . ?
C43 H43 0.95 . ?
C44 C45 1.380(15) . ?
C44 H44 0.95 . ?
C45 C46 1.382(15) . ?
C45 H45 0.95 . ?
C46 C49 1.513(15) . ?
C47 O48 1.428(12) . ?
C47 H47A 0.99 . ?
C47 H47B 0.99 . ?
C49 O50 1.437(13) . ?
C49 H49A 0.99 . ?
C49 H49B 0.99 . ?
O50 H50 0.84 . ?
Cl1 O52 1.422(9) . ?
Cl1 O53 1.436(9) . ?
Cl1 O51 1.443(8) . ?
Cl1 O54 1.450(8) . ?
Cl2 O57 1.414(10) . ?
Cl2 O56 1.429(9) . ?
Cl2 O55 1.434(9) . ?
Cl2 O58 1.450(9) . ?

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
N1 Cu1 O8 81.4(3) . . ?
N1 Cu1 N11 179.0(4) . . ?
O8 Cu1 N11 97.6(4) . . ?
O8 Cu2 N21 161.9(3) . . ?
O8 Cu2 O30 96.9(4) . . ?
N21 Cu2 O30 83.1(4) . . ?
O8 Cu2 O28 96.8(3) . . ?
N21 Cu2 O28 81.5(4) . . ?
O30 Cu2 O28 164.4(3) . . ?
N41 Cu3 O48 82.0(4) . . ?
N41 Cu3 N31 176.7(4) . . ?
O48 Cu3 N31 95.2(4) . . ?
C6 N1 C2 121.2(10) . . ?
C6 N1 Cu1 118.2(7) . . ?
C2 N1 Cu1 120.2(8) . . ?
N1 C2 C3 121.3(10) . . ?
N1 C2 C7 111.7(10) . . ?
C3 C2 C7 126.9(10) . . ?
C4 C3 C2 117.2(11) . . ?
C4 C3 H3 121.4 . . ?
C2 C3 H3 121.4 . . ?
C3 C4 C5 121.4(12) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C6 C5 C4 118.3(11) . . ?
C6 C5 H5 120.8 . . ?
C4 C5 H5 120.8 . . ?
N1 C6 C5 120.4(10) . . ?
N1 C6 C9 111.6(10) . . ?
C5 C6 C9 128.0(11) . . ?
O8 C7 C2 111.8(8) . . ?
O8 C7 H7A 109.3 . . ?
C2 C7 H7A 109.3 . . ?
O8 C7 H7B 109.3 . . ?
C2 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
C7 O8 Cu2 125.5(6) . . ?
C7 O8 Cu1 114.1(6) . . ?
Cu2 O8 Cu1 114.7(4) . . ?
O10 C9 C6 110.7(9) . . ?
O10 C9 H9A 109.5 . . ?
C6 C9 H9A 109.5 . . ?
O10 C9 H9B 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C9 O10 H10 109.5 . . ?
C16 N11 C12 118.5(10) . . ?
C16 N11 Cu1 119.9(8) . . ?
C12 N11 Cu1 121.2(8) . . ?
N11 C12 C13 122.4(12) . . ?
N11 C12 C17 115.5(10) . . ?
C13 C12 C17 121.8(11) . . ?
C12 C13 C14 118.6(12) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
C15 C14 C13 119.0(12) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 C16 119.9(12) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
N11 C16 C15 121.5(11) . . ?
N11 C16 C19 119.7(10) . . ?
C15 C16 C19 118.8(11) . . ?
O18 C17 C12 113.5(9) . . ?
O18 C17 H17A 108.9 . . ?
C12 C17 H17A 108.9 . . ?
O18 C17 H17B 108.9 . . ?
C12 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C17 O18 H18 109.5 . . ?
O20 C19 C16 110.7(10) . . ?
O20 C19 H19A 109.5 . . ?
C16 C19 H19A 109.5 . . ?
O20 C19 H19B 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
C19 O20 H20 109.5 . . ?
C26 N21 C22 122.9(10) . . ?
C26 N21 Cu2 118.7(7) . . ?
C22 N21 Cu2 118.4(8) . . ?
N21 C22 C23 119.8(11) . . ?
N21 C22 C27 113.6(10) . . ?
C23 C22 C27 126.6(11) . . ?
C24 C23 C22 117.6(12) . . ?
C24 C23 H23 121.2 . . ?
C22 C23 H23 121.2 . . ?
C23 C24 C25 121.7(11) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C26 C25 C24 118.1(11) . . ?
C26 C25 H25 120.9 . . ?
C24 C25 H25 120.9 . . ?
N21 C26 C25 119.8(11) . . ?
N21 C26 C29 113.2(10) . . ?
C25 C26 C29 127.0(11) . . ?
O28 C27 C22 111.3(9) . . ?
O28 C27 H27A 109.4 . . ?
C22 C27 H27A 109.4 . . ?
O28 C27 H27B 109.4 . . ?
C22 C27 H27B 109.4 . . ?
H27A C27 H27B 108 . . ?
C27 O28 Cu2 115.2(7) . . ?
O30 C29 C26 112.3(10) . . ?
O30 C29 H29A 109.1 . . ?
C26 C29 H29A 109.1 . . ?
O30 C29 H29B 109.1 . . ?
C26 C29 H29B 109.1 . . ?
H29A C29 H29B 107.9 . . ?
C29 O30 Cu2 112.5(7) . . ?
C36 N31 C32 118.8(10) . . ?
C36 N31 Cu3 118.5(8) . . ?
C32 N31 Cu3 122.5(8) . . ?
N31 C32 C33 122.2(11) . . ?
N31 C32 C37 117.1(10) . . ?
C33 C32 C37 120.7(11) . . ?
C32 C33 C34 119.4(12) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C35 C34 C33 118.1(12) . . ?
C35 C34 H34 120.9 . . ?
C33 C34 H34 120.9 . . ?
C34 C35 C36 120.0(12) . . ?
C34 C35 H35 120 . . ?
C36 C35 H35 120 . . ?
N31 C36 C35 121.3(11) . . ?
N31 C36 C39 117.9(10) . . ?
C35 C36 C39 120.7(11) . . ?
O38 C37 C32 111.0(10) . . ?
O38 C37 H37A 109.4 . . ?
C32 C37 H37A 109.4 . . ?
O38 C37 H37B 109.4 . . ?
C32 C37 H37B 109.4 . . ?
H37A C37 H37B 108 . . ?
C37 O38 H38 109.5 . . ?
O40 C39 C36 108.5(9) . . ?
O40 C39 H39A 110 . . ?
C36 C39 H39A 110 . . ?
O40 C39 H39B 110 . . ?
C36 C39 H39B 110 . . ?
H39A C39 H39B 108.4 . . ?
C39 O40 H40 109.5 . . ?
C46 N41 C42 121.9(10) . . ?
C46 N41 Cu3 119.5(8) . . ?
C42 N41 Cu3 118.5(8) . . ?
N41 C42 C43 120.3(11) . . ?
N41 C42 C47 112.8(10) . . ?
C43 C42 C47 126.8(10) . . ?
C42 C43 C44 118.4(11) . . ?
C42 C43 H43 120.8 . . ?
C44 C43 H43 120.8 . . ?
C45 C44 C43 120.6(12) . . ?
C45 C44 H44 119.7 . . ?
C43 C44 H44 119.7 . . ?
C44 C45 C46 118.0(12) . . ?
C44 C45 H45 121 . . ?
C46 C45 H45 121 . . ?
N41 C46 C45 120.8(11) . . ?
N41 C46 C49 114.3(10) . . ?
C45 C46 C49 124.9(11) . . ?
O48 C47 C42 109.3(9) . . ?
O48 C47 H47A 109.8 . . ?
C42 C47 H47A 109.8 . . ?
O48 C47 H47B 109.8 . . ?
C42 C47 H47B 109.8 . . ?
H47A C47 H47B 108.3 . . ?
C47 O48 Cu3 115.6(7) . . ?
O50 C49 C46 109.5(10) . . ?
O50 C49 H49A 109.8 . . ?
C46 C49 H49A 109.8 . . ?
O50 C49 H49B 109.8 . . ?
C46 C49 H49B 109.8 . . ?
H49A C49 H49B 108.2 . . ?
C49 O50 H50 109.5 . . ?
O52 Cl1 O53 110.5(5) . . ?
O52 Cl1 O51 109.5(6) . . ?
O53 Cl1 O51 108.8(5) . . ?
O52 Cl1 O54 110.1(5) . . ?
O53 Cl1 O54 108.7(5) . . ?
O51 Cl1 O54 109.2(5) . . ?
O57 Cl2 O56 110.6(6) . . ?
O57 Cl2 O55 108.8(7) . . ?
O56 Cl2 O55 108.4(6) . . ?
O57 Cl2 O58 109.5(6) . . ?
O56 Cl2 O58 109.8(6) . . ?
O55 Cl2 O58 109.7(6) . . ?

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
C6 N1 C2 C3 -1.7(18) . . . . ?
Cu1 N1 C2 C3 171.5(9) . . . . ?
C6 N1 C2 C7 -179.8(11) . . . . ?
Cu1 N1 C2 C7 -6.7(14) . . . . ?
N1 C2 C3 C4 -1.7(18) . . . . ?
C7 C2 C3 C4 176.2(12) . . . . ?
C2 C3 C4 C5 3.1(18) . . . . ?
C3 C4 C5 C6 -1.3(19) . . . . ?
C2 N1 C6 C5 3.6(18) . . . . ?
Cu1 N1 C6 C5 -169.7(9) . . . . ?
C2 N1 C6 C9 -175.9(11) . . . . ?
Cu1 N1 C6 C9 10.9(14) . . . . ?
C4 C5 C6 N1 -2.1(18) . . . . ?
C4 C5 C6 C9 177.3(12) . . . . ?
N1 C2 C7 O8 0.2(15) . . . . ?
C3 C2 C7 O8 -177.8(12) . . . . ?
C2 C7 O8 Cu2 -146.0(8) . . . . ?
C2 C7 O8 Cu1 5.7(12) . . . . ?
N21 Cu2 O8 C7 166.7(12) . . . . ?
O30 Cu2 O8 C7 77.6(9) . . . . ?
O28 Cu2 O8 C7 -109.8(9) . . . . ?
N21 Cu2 O8 Cu1 15.1(16) . . . . ?
O30 Cu2 O8 Cu1 -74.0(5) . . . . ?
O28 Cu2 O8 Cu1 98.6(4) . . . . ?
N1 C6 C9 O10 -26.0(14) . . . . ?
C5 C6 C9 O10 154.6(12) . . . . ?
C16 N11 C12 C13 -1.9(17) . . . . ?
Cu1 N11 C12 C13 -175.0(8) . . . . ?
C16 N11 C12 C17 -176.5(10) . . . . ?
Cu1 N11 C12 C17 10.3(13) . . . . ?
N11 C12 C13 C14 0.1(17) . . . . ?
C17 C12 C13 C14 174.4(11) . . . . ?
C12 C13 C14 C15 -0.7(18) . . . . ?
C13 C14 C15 C16 3.0(18) . . . . ?
C12 N11 C16 C15 4.2(17) . . . . ?
Cu1 N11 C16 C15 177.5(8) . . . . ?
C12 N11 C16 C19 -176.3(9) . . . . ?
Cu1 N11 C16 C19 -3.0(15) . . . . ?
C14 C15 C16 N11 -4.9(18) . . . . ?
C14 C15 C16 C19 175.6(10) . . . . ?
N11 C12 C17 O18 -28.4(14) . . . . ?
C13 C12 C17 O18 156.9(10) . . . . ?
N11 C16 C19 O20 -15.5(15) . . . . ?
C15 C16 C19 O20 164.0(10) . . . . ?
C26 N21 C22 C23 1.0(16) . . . . ?
Cu2 N21 C22 C23 -178.1(8) . . . . ?
C26 N21 C22 C27 179.4(10) . . . . ?
Cu2 N21 C22 C27 0.4(13) . . . . ?
N21 C22 C23 C24 -1.3(17) . . . . ?
C27 C22 C23 C24 -179.6(11) . . . . ?
C22 C23 C24 C25 1.0(17) . . . . ?
C23 C24 C25 C26 -0.3(18) . . . . ?
C22 N21 C26 C25 -0.2(17) . . . . ?
Cu2 N21 C26 C25 178.9(8) . . . . ?
C22 N21 C26 C29 -178.4(11) . . . . ?
Cu2 N21 C26 C29 0.6(13) . . . . ?
C24 C25 C26 N21 -0.2(18) . . . . ?
C24 C25 C26 C29 177.8(11) . . . . ?
N21 C22 C27 O28 0.7(14) . . . . ?
C23 C22 C27 O28 179.0(11) . . . . ?
C22 C27 O28 Cu2 -1.4(11) . . . . ?
N21 C26 C29 O30 2.9(14) . . . . ?
C25 C26 C29 O30 -175.3(11) . . . . ?
C26 C29 O30 Cu2 -4.9(12) . . . . ?
C36 N31 C32 C33 -2.0(16) . . . . ?
Cu3 N31 C32 C33 -176.8(8) . . . . ?
C36 N31 C32 C37 176.4(10) . . . . ?
Cu3 N31 C32 C37 1.5(13) . . . . ?
N31 C32 C33 C34 -0.4(16) . . . . ?
C37 C32 C33 C34 -178.7(10) . . . . ?
C32 C33 C34 C35 0.5(16) . . . . ?
C33 C34 C35 C36 1.7(17) . . . . ?
C32 N31 C36 C35 4.2(16) . . . . ?
Cu3 N31 C36 C35 179.3(8) . . . . ?
C32 N31 C36 C39 -179.4(10) . . . . ?
Cu3 N31 C36 C39 -4.4(14) . . . . ?
C34 C35 C36 N31 -4.2(17) . . . . ?
C34 C35 C36 C39 179.6(11) . . . . ?
N31 C32 C37 O38 34.9(14) . . . . ?
C33 C32 C37 O38 -146.7(10) . . . . ?
N31 C36 C39 O40 28.3(14) . . . . ?
C35 C36 C39 O40 -155.4(10) . . . . ?
C46 N41 C42 C43 1.3(19) . . . . ?
Cu3 N41 C42 C43 177.6(9) . . . . ?
C46 N41 C42 C47 179.0(11) . . . . ?
Cu3 N41 C42 C47 -4.7(14) . . . . ?
N41 C42 C43 C44 -0.5(18) . . . . ?
C47 C42 C43 C44 -177.8(12) . . . . ?
C42 C43 C44 C45 0.2(18) . . . . ?
C43 C44 C45 C46 -0.7(19) . . . . ?
C42 N41 C46 C45 -1.8(18) . . . . ?
Cu3 N41 C46 C45 -178.1(9) . . . . ?
C42 N41 C46 C49 178.9(11) . . . . ?
Cu3 N41 C46 C49 2.6(14) . . . . ?
C44 C45 C46 N41 1.4(19) . . . . ?
C44 C45 C46 C49 -179.3(12) . . . . ?
N41 C42 C47 O48 -5.3(15) . . . . ?
C43 C42 C47 O48 172.2(12) . . . . ?
C42 C47 O48 Cu3 12.8(12) . . . . ?
N41 C46 C49 O50 -6.4(15) . . . . ?
C45 C46 C49 O50 174.3(11) . . . . ?

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
O10 H10 O48 0.84 1.63 2.427(11) 156.8 1_455
O18 H18 O30 0.84 1.81 2.654(11) 178.8 .
O20 H20 O58 0.84 1.97 2.810(12) 173.6 .
O38 H38 O51 0.84 1.99 2.819(11) 171.5 .
O40 H40 O30 0.84 1.87 2.601(11) 144.3 2_656
O50 H50 O28 0.84 1.61 2.441(10) 168.4 .

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_DDJS-21
_database_code_depnum_ccdc_archive 'CCDC 1033744'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2014-12-23 downloaded from the CCDC.
;

_audit_creation_date             2012-07-30T11:22:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H17 Cu N2 O4, Cl O4'
_chemical_formula_sum            'C14 H17 Cl Cu N2 O8'
_chemical_formula_weight         440.29
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_Int_Tables_number      43
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'

_cell_length_a                   27.107(2)
_cell_length_b                   42.977(2)
_cell_length_c                   11.7228(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13656.8(16)
_cell_formula_units_Z            32
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1856
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      24.37
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7200
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_absorpt_correction_T_min  0.8778
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_number            41818
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         26.4
_diffrn_reflns_theta_full        26.4
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             6835
_reflns_number_gt                6114
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APPEX2 (BRUKER AXS, 2005)'
_computing_cell_refinement       'APPEX2 (BRUKER AXS, 2005)'
_computing_data_reduction        'APPEX2 (BRUKER AXS, 2005)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0302P)²+20.0804P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6835
_refine_ls_number_parameters     539
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0665
_refine_ls_wR_factor_gt          0.0635
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(8)
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.069

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
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'

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.29719(14) 0.11943(8) 0.2356(3) 0.0271(9) Uani 1 1 d . . .
H1A H 0.2632 0.1169 0.2059 0.033 Uiso 1 1 calc R . .
H1B H 0.3077 0.0995 0.27 0.033 Uiso 1 1 calc R . .
C2 C 0.33126(12) 0.12786(6) 0.1399(3) 0.0174(7) Uani 1 1 d . . .
C3 C 0.32092(14) 0.12055(8) 0.0280(3) 0.0257(8) Uani 1 1 d . . .
H3 H 0.2906 0.1108 0.0084 0.031 Uiso 1 1 calc R . .
C4 C 0.35532(15) 0.12761(8) -0.0553(3) 0.0303(9) Uani 1 1 d . . .
H4 H 0.3488 0.1227 -0.1329 0.036 Uiso 1 1 calc R . .
C5 C 0.39879(15) 0.14164(8) -0.0253(3) 0.0283(9) Uani 1 1 d . . .
H5 H 0.4231 0.146 -0.0814 0.034 Uiso 1 1 calc R . .
C6 C 0.40683(13) 0.14940(7) 0.0884(3) 0.0217(8) Uani 1 1 d . . .
C7 C 0.45255(14) 0.16733(9) 0.1230(3) 0.0344(9) Uani 1 1 d . . .
H7A H 0.4813 0.1594 0.0799 0.041 Uiso 1 1 calc R . .
H7B H 0.4482 0.1896 0.1034 0.041 Uiso 1 1 calc R . .
C8 C 0.41140(14) 0.11415(7) 0.5105(3) 0.0233(8) Uani 1 1 d . . .
H8A H 0.4434 0.1036 0.5235 0.028 Uiso 1 1 calc R . .
H8B H 0.3856 0.1025 0.5522 0.028 Uiso 1 1 calc R . .
C9 C 0.41392(12) 0.14707(7) 0.5555(3) 0.0174(7) Uani 1 1 d . . .
C10 C 0.42881(13) 0.15568(8) 0.6638(3) 0.0211(8) Uani 1 1 d . . .
H10 H 0.4395 0.1406 0.7177 0.025 Uiso 1 1 calc R . .
C11 C 0.42762(12) 0.18712(7) 0.6911(3) 0.0210(8) Uani 1 1 d . . .
H11 H 0.4379 0.1937 0.7648 0.025 Uiso 1 1 calc R . .
C12 C 0.41179(12) 0.20887(7) 0.6135(3) 0.0184(7) Uani 1 1 d . . .
H12 H 0.411 0.2303 0.6326 0.022 Uiso 1 1 calc R . .
C13 C 0.39704(12) 0.19876(7) 0.5071(3) 0.0152(7) Uani 1 1 d . . .
C14 C 0.37704(13) 0.21896(7) 0.4140(3) 0.0210(8) Uani 1 1 d . . .
H14A H 0.3442 0.227 0.436 0.025 Uiso 1 1 calc R . .
H14B H 0.3993 0.2369 0.4016 0.025 Uiso 1 1 calc R . .
C15 C 0.43027(16) -0.03987(8) 0.3132(3) 0.0365(10) Uani 1 1 d . B .
H15A H 0.4001 -0.0528 0.3088 0.044 Uiso 1 1 calc R . .
H15B H 0.459 -0.0541 0.315 0.044 Uiso 1 1 calc R . .
C16 C 0.43350(12) -0.01957(7) 0.2080(3) 0.0194(8) Uani 1 1 d . B .
C17 C 0.43760(12) -0.02989(8) 0.0966(3) 0.0260(8) Uani 1 1 d . . .
H17 H 0.4398 -0.0515 0.0799 0.031 Uiso 1 1 calc R . .
C18 C 0.43847(13) -0.00819(9) 0.0107(3) 0.0300(9) Uani 1 1 d . . .
H18 H 0.4415 -0.0149 -0.0663 0.036 Uiso 1 1 calc R . .
C19 C 0.43497(14) 0.02300(9) 0.0344(3) 0.0291(9) Uani 1 1 d . . .
H19 H 0.4355 0.038 -0.0252 0.035 Uiso 1 1 calc R . .
C20 C 0.43067(12) 0.03219(8) 0.1473(3) 0.0194(7) Uani 1 1 d . B .
C21 C 0.42545(15) 0.06487(8) 0.1900(3) 0.0287(9) Uani 1 1 d . . .
H21A H 0.4543 0.0773 0.1654 0.034 Uiso 1 1 calc R A 1
H21B H 0.3954 0.0744 0.1569 0.034 Uiso 1 1 calc R A 1
N1 N 0.37355(9) 0.14238(6) 0.1686(2) 0.0131(6) Uani 1 1 d . . .
N2 N 0.39921(10) 0.16839(5) 0.4806(2) 0.0154(6) Uani 1 1 d . . .
N3 N 0.43041(9) 0.01073(6) 0.2304(2) 0.0139(6) Uani 1 1 d . . .
O1 O 0.46150(9) 0.16452(5) 0.2391(2) 0.0290(6) Uani 1 1 d D . .
H1O H 0.4670(14) 0.1807(6) 0.269(3) 0.035 Uiso 1 1 d D . .
O2 O 0.29798(10) 0.14318(5) 0.3194(2) 0.0263(6) Uani 1 1 d . . .
H2O H 0.2955(15) 0.1367(9) 0.377(3) 0.032 Uiso 1 1 d . . .
O3 O 0.37314(9) 0.20116(5) 0.31158(19) 0.0197(5) Uani 1 1 d D . .
H3O H 0.3607(14) 0.2092(8) 0.264(3) 0.024 Uiso 1 1 d D . .
O4 O 0.40048(11) 0.11409(5) 0.3928(2) 0.0365(7) Uani 1 1 d . . .
O5 O 0.42925(8) -0.02229(5) 0.41434(18) 0.0191(5) Uani 1 1 d . . .
O6 O 0.4220(4) 0.0652(4) 0.3158(13) 0.025(3) Uani 0.5 1 d PD B 1
H6O H 0.416(3) 0.0837(8) 0.331(8) 0.03 Uiso 0.5 1 d PD C 1
O9 O 0.29295(11) 0.17917(6) 0.5903(3) 0.0561(9) Uani 1 1 d . D .
O10 O 0.21973(18) 0.15359(12) 0.6013(8) 0.042(3) Uani 0.577(14) 1 d P D 1
O11 O 0.2891(3) 0.1253(2) 0.5478(9) 0.032(2) Uani 0.577(14) 1 d P D 1
O12 O 0.2765(4) 0.14057(17) 0.7382(5) 0.062(3) Uani 0.577(14) 1 d P D 1
O10B O 0.3114(6) 0.1422(2) 0.7057(12) 0.077(5) Uani 0.423(14) 1 d P D 2
O11B O 0.2295(4) 0.1571(2) 0.6916(13) 0.078(5) Uani 0.423(14) 1 d P D 2
O12B O 0.2650(7) 0.1289(4) 0.5452(11) 0.064(5) Uani 0.423(14) 1 d P D 2
O13 O 0.48661(10) 0.22223(6) 0.3321(3) 0.0575(9) Uani 1 1 d . . .
O14 O 0.55702(14) 0.20256(6) 0.4165(3) 0.0609(10) Uani 1 1 d . . .
O15 O 0.55165(10) 0.25520(5) 0.3778(2) 0.0386(7) Uani 1 1 d . . .
O16 O 0.55949(14) 0.21923(8) 0.2293(3) 0.0628(11) Uani 1 1 d . . .
Cl3 Cl 0.53908(3) 0.224722(17) 0.33790(7) 0.02121(18) Uani 1 1 d . . .
Cl4 Cl 0.27209(3) 0.150620(19) 0.62591(7) 0.02485(19) Uani 1 1 d . . .
Cu1 Cu 0.416802(14) 0.023199(8) 0.38408(3) 0.01298(9) Uani 1 1 d . B .
Cu2 Cu 0.384788(15) 0.154945(8) 0.32888(3) 0.01674(10) Uani 1 1 d . . .
O7 O 0.4832(3) 0.04165(13) 0.4747(6) 0.0225(16) Uani 0.5 1 d PD B 1
H7O H 0.5103(19) 0.033(2) 0.465(9) 0.027 Uiso 0.5 1 d PD E 1
C22 C 0.47341(14) 0.04115(8) 0.6032(3) 0.0314(10) Uani 1 1 d . . .
H22A H 0.4857 0.0215 0.6367 0.038 Uiso 1 1 calc R B 1
H22B H 0.4907 0.0587 0.6407 0.038 Uiso 1 1 calc R B 1
C23 C 0.41864(15) 0.04388(7) 0.6216(3) 0.0260(9) Uani 1 1 d . B .
C24 C 0.3992(2) 0.05303(8) 0.7271(3) 0.0494(14) Uani 1 1 d . . .
H24 H 0.4203 0.0575 0.7897 0.059 Uiso 1 1 calc R B .
C25 C 0.3484(3) 0.05533(9) 0.7379(4) 0.0625(17) Uani 1 1 d . B .
H25 H 0.3343 0.0614 0.8085 0.075 Uiso 1 1 calc R . .
C26 C 0.3193(2) 0.04895(9) 0.6486(4) 0.0517(14) Uani 1 1 d . . .
H26 H 0.2845 0.0505 0.656 0.062 Uiso 1 1 calc R B .
C27 C 0.33974(15) 0.04023(8) 0.5469(3) 0.0309(10) Uani 1 1 d . B .
N4 N 0.38955(11) 0.03769(5) 0.5343(2) 0.0179(6) Uani 1 1 d . . .
C28 C 0.30873(15) 0.03426(10) 0.4436(4) 0.0430(12) Uani 1 1 d . . .
H28A H 0.2754 0.0275 0.4673 0.052 Uiso 1 1 calc R B .
H28B H 0.3053 0.0537 0.399 0.052 Uiso 1 1 calc R . .
O8 O 0.33070(10) 0.01096(7) 0.3746(3) 0.0426(7) Uani 1 1 d . B .
H8O H 0.3234(16) 0.0118(10) 0.301(4) 0.051 Uiso 1 1 d . . .
O7B O 0.4826(3) 0.02708(17) 0.5062(6) 0.0307(16) Uani 0.5 1 d PD B 2
H7P H 0.5107(19) 0.025(2) 0.480(9) 0.037 Uiso 0.5 1 d PD F 2
O6B O 0.4046(4) 0.0635(4) 0.2994(13) 0.015(2) Uani 0.5 1 d P B 2
H6P H 0.404(3) 0.0793(13) 0.347(7) 0.018 Uiso 0.5 1 d PD G 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.417(4) . ?
C1 C2 1.497(5) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 N1 1.348(4) . ?
C2 C3 1.377(5) . ?
C3 C4 1.385(5) . ?
C3 H3 0.95 . ?
C4 C5 1.370(6) . ?
C4 H4 0.95 . ?
C5 C6 1.391(5) . ?
C5 H5 0.95 . ?
C6 N1 1.337(4) . ?
C6 C7 1.515(5) . ?
C7 O1 1.388(5) . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C8 O4 1.411(4) . ?
C8 C9 1.512(4) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C9 N2 1.330(4) . ?
C9 C10 1.382(5) . ?
C10 C11 1.389(4) . ?
C10 H10 0.95 . ?
C11 C12 1.373(4) . ?
C11 H11 0.95 . ?
C12 C13 1.381(4) . ?
C12 H12 0.95 . ?
C13 N2 1.343(4) . ?
C13 C14 1.496(4) . ?
C14 O3 1.427(4) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 O5 1.406(4) . ?
C15 C16 1.513(5) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 N3 1.331(4) . ?
C16 C17 1.384(5) . ?
C17 C18 1.373(5) . ?
C17 H17 0.95 . ?
C18 C19 1.372(5) . ?
C18 H18 0.95 . ?
C19 C20 1.386(5) . ?
C19 H19 0.95 . ?
C20 N3 1.341(4) . ?
C20 C21 1.497(5) . ?
C21 O6B 1.403(17) . ?
C21 O6 1.478(16) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
N1 Cu2 1.979(3) . ?
N2 Cu2 1.911(3) . ?
N3 Cu1 1.916(2) . ?
O1 Cu2 2.367(3) . ?
O1 H1O 0.794(18) . ?
O2 Cu2 2.410(3) . ?
O2 H2O 0.73(4) . ?
O3 Cu2 2.021(2) . ?
O3 H3O 0.74(3) . ?
O4 Cu2 1.956(2) . ?
O5 Cu1 2.015(2) . ?
O6 Cu1 1.979(16) . ?
O6 H6O 0.83(2) . ?
O6 H6P 0.86(4) . ?
O9 Cl4 1.414(3) . ?
O10 Cl4 1.454(5) . ?
O11 Cl4 1.493(9) . ?
O12 Cl4 1.390(6) . ?
O10B Cl4 1.463(8) . ?
O11B Cl4 1.415(8) . ?
O12B Cl4 1.342(13) . ?
O13 Cl3 1.428(3) . ?
O14 Cl3 1.412(3) . ?
O15 Cl3 1.432(2) . ?
O16 Cl3 1.408(3) . ?
Cu1 N4 2.009(3) . ?
Cu1 O6B 2.024(16) . ?
Cu1 O7 2.237(7) . ?
Cu1 O7B 2.293(7) . ?
Cu1 O8 2.395(3) . ?
O7 C22 1.530(8) . ?
O7 H7O 0.83(3) . ?
O7 H7P 1.05(6) . ?
C22 O7B 1.312(7) . ?
C22 C23 1.505(5) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
C23 N4 1.318(4) . ?
C23 C24 1.401(6) . ?
C24 C25 1.386(8) . ?
C24 H24 0.95 . ?
C25 C26 1.339(8) . ?
C25 H25 0.95 . ?
C26 C27 1.367(5) . ?
C26 H26 0.95 . ?
C27 N4 1.363(5) . ?
C27 C28 1.497(6) . ?
C28 O8 1.418(5) . ?
C28 H28A 0.99 . ?
C28 H28B 0.99 . ?
O8 H8O 0.88(5) . ?
O7B H7O 0.93(5) . ?
O7B H7P 0.829(15) . ?
O6B H6O 1.00(6) . ?
O6B H6P 0.88(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 C2 109.6(3) . . ?
O2 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
O2 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N1 C2 C3 121.1(3) . . ?
N1 C2 C1 116.7(3) . . ?
C3 C2 C1 122.2(3) . . ?
C2 C3 C4 119.0(3) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 119.7(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 119.1(4) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
N1 C6 C5 120.9(3) . . ?
N1 C6 C7 118.6(3) . . ?
C5 C6 C7 120.4(3) . . ?
O1 C7 C6 111.2(3) . . ?
O1 C7 H7A 109.4 . . ?
C6 C7 H7A 109.4 . . ?
O1 C7 H7B 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108 . . ?
O4 C8 C9 110.7(3) . . ?
O4 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
O4 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
N2 C9 C10 120.6(3) . . ?
N2 C9 C8 113.6(3) . . ?
C10 C9 C8 125.8(3) . . ?
C9 C10 C11 117.7(3) . . ?
C9 C10 H10 121.1 . . ?
C11 C10 H10 121.1 . . ?
C12 C11 C10 121.1(3) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 118.4(3) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
N2 C13 C12 120.1(3) . . ?
N2 C13 C14 114.3(3) . . ?
C12 C13 C14 125.6(3) . . ?
O3 C14 C13 109.2(2) . . ?
O3 C14 H14A 109.8 . . ?
C13 C14 H14A 109.8 . . ?
O3 C14 H14B 109.8 . . ?
C13 C14 H14B 109.8 . . ?
H14A C14 H14B 108.3 . . ?
O5 C15 C16 112.3(3) . . ?
O5 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
O5 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
N3 C16 C17 120.3(3) . . ?
N3 C16 C15 113.5(3) . . ?
C17 C16 C15 126.1(3) . . ?
C18 C17 C16 118.4(3) . . ?
C18 C17 H17 120.8 . . ?
C16 C17 H17 120.8 . . ?
C19 C18 C17 120.9(3) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 118.6(3) . . ?
C18 C19 H19 120.7 . . ?
C20 C19 H19 120.7 . . ?
N3 C20 C19 119.8(3) . . ?
N3 C20 C21 113.7(3) . . ?
C19 C20 C21 126.5(3) . . ?
O6B C21 C20 107.7(7) . . ?
O6 C21 C20 110.3(7) . . ?
O6B C21 H21A 127.3 . . ?
O6 C21 H21A 109.6 . . ?
C20 C21 H21A 109.6 . . ?
O6B C21 H21B 92.5 . . ?
O6 C21 H21B 109.6 . . ?
C20 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C6 N1 C2 120.2(3) . . ?
C6 N1 Cu2 120.1(2) . . ?
C2 N1 Cu2 119.6(2) . . ?
C9 N2 C13 122.0(3) . . ?
C9 N2 Cu2 117.9(2) . . ?
C13 N2 Cu2 120.0(2) . . ?
C16 N3 C20 122.0(3) . . ?
C16 N3 Cu1 118.1(2) . . ?
C20 N3 Cu1 119.4(2) . . ?
C7 O1 Cu2 107.3(2) . . ?
C7 O1 H1O 113(3) . . ?
Cu2 O1 H1O 97(3) . . ?
C1 O2 Cu2 101.42(19) . . ?
C1 O2 H2O 111(3) . . ?
Cu2 O2 H2O 97(3) . . ?
C14 O3 Cu2 115.50(18) . . ?
C14 O3 H3O 115(3) . . ?
Cu2 O3 H3O 127(3) . . ?
C8 O4 Cu2 114.75(19) . . ?
C15 O5 Cu1 112.1(2) . . ?
C21 O6 Cu1 113.6(9) . . ?
C21 O6 H6O 104(7) . . ?
Cu1 O6 H6O 140(6) . . ?
C21 O6 H6P 118(6) . . ?
Cu1 O6 H6P 116(5) . . ?
O16 Cl3 O14 110.0(2) . . ?
O16 Cl3 O13 109.6(2) . . ?
O14 Cl3 O13 108.9(2) . . ?
O16 Cl3 O15 110.79(18) . . ?
O14 Cl3 O15 108.80(17) . . ?
O13 Cl3 O15 108.73(16) . . ?
O12B Cl4 O12 117.6(8) . . ?
O12B Cl4 O9 116.9(6) . . ?
O12 Cl4 O9 121.0(4) . . ?
O12B Cl4 O11B 113.7(7) . . ?
O12 Cl4 O11B 67.4(6) . . ?
O9 Cl4 O11B 108.5(4) . . ?
O12B Cl4 O10 77.3(7) . . ?
O12 Cl4 O10 107.4(4) . . ?
O9 Cl4 O10 104.8(3) . . ?
O11B Cl4 O10 45.1(5) . . ?
O12B Cl4 O10B 112.6(8) . . ?
O9 Cl4 O10B 96.5(6) . . ?
O11B Cl4 O10B 107.1(7) . . ?
O10 Cl4 O10B 149.2(7) . . ?
O12 Cl4 O11 109.2(5) . . ?
O9 Cl4 O11 109.1(4) . . ?
O11B Cl4 O11 136.7(5) . . ?
O10 Cl4 O11 104.1(4) . . ?
O10B Cl4 O11 89.3(6) . . ?
N3 Cu1 O6 82.0(5) . . ?
N3 Cu1 N4 169.16(12) . . ?
O6 Cu1 N4 95.6(5) . . ?
N3 Cu1 O5 82.06(10) . . ?
O6 Cu1 O5 160.7(5) . . ?
N4 Cu1 O5 102.01(9) . . ?
N3 Cu1 O6B 79.0(5) . . ?
O6 Cu1 O6B 14.7(4) . . ?
N4 Cu1 O6B 96.0(5) . . ?
O5 Cu1 O6B 160.7(4) . . ?
N3 Cu1 O7 113.0(2) . . ?
O6 Cu1 O7 79.1(3) . . ?
N4 Cu1 O7 76.7(2) . . ?
O5 Cu1 O7 97.21(15) . . ?
O6B Cu1 O7 93.5(3) . . ?
N3 Cu1 O7B 117.2(2) . . ?
O6 Cu1 O7B 97.5(3) . . ?
N4 Cu1 O7B 73.5(2) . . ?
O5 Cu1 O7B 80.2(2) . . ?
O6B Cu1 O7B 111.8(3) . . ?
O7 Cu1 O7B 18.42(17) . . ?
N3 Cu1 O8 94.74(11) . . ?
O6 Cu1 O8 104.5(3) . . ?
N4 Cu1 O8 75.54(11) . . ?
O5 Cu1 O8 87.61(10) . . ?
O6B Cu1 O8 90.3(3) . . ?
O7 Cu1 O8 152.2(2) . . ?
O7B Cu1 O8 143.4(2) . . ?
N2 Cu2 O4 82.54(10) . . ?
N2 Cu2 N1 176.47(12) . . ?
O4 Cu2 N1 98.78(10) . . ?
N2 Cu2 O3 80.11(10) . . ?
O4 Cu2 O3 162.65(9) . . ?
N1 Cu2 O3 98.55(10) . . ?
N2 Cu2 O1 100.47(11) . . ?
O4 Cu2 O1 97.79(11) . . ?
N1 Cu2 O1 76.13(10) . . ?
O3 Cu2 O1 85.51(9) . . ?
N2 Cu2 O2 107.84(10) . . ?
O4 Cu2 O2 92.39(10) . . ?
N1 Cu2 O2 75.43(9) . . ?
O3 Cu2 O2 92.81(9) . . ?
O1 Cu2 O2 150.92(9) . . ?
C22 O7 Cu1 108.8(4) . . ?
C22 O7 H7O 107(7) . . ?
Cu1 O7 H7O 119(8) . . ?
C22 O7 H7P 93(5) . . ?
Cu1 O7 H7P 110(6) . . ?
O7B C22 C23 110.3(4) . . ?
C23 C22 O7 108.1(4) . . ?
O7B C22 H22A 83.5 . . ?
C23 C22 H22A 110.1 . . ?
O7 C22 H22A 110.1 . . ?
O7B C22 H22B 130.2 . . ?
C23 C22 H22B 110.1 . . ?
O7 C22 H22B 110.1 . . ?
H22A C22 H22B 108.4 . . ?
N4 C23 C24 121.1(4) . . ?
N4 C23 C22 117.6(3) . . ?
C24 C23 C22 121.2(4) . . ?
C25 C24 C23 118.2(4) . . ?
C25 C24 H24 120.9 . . ?
C23 C24 H24 120.9 . . ?
C26 C25 C24 120.0(4) . . ?
C26 C25 H25 120 . . ?
C24 C25 H25 120 . . ?
C25 C26 C27 119.9(5) . . ?
C25 C26 H26 120 . . ?
C27 C26 H26 120 . . ?
N4 C27 C26 121.2(4) . . ?
N4 C27 C28 117.1(3) . . ?
C26 C27 C28 121.7(4) . . ?
C23 N4 C27 119.5(3) . . ?
C23 N4 Cu1 121.5(2) . . ?
C27 N4 Cu1 119.0(2) . . ?
O8 C28 C27 110.3(3) . . ?
O8 C28 H28A 109.6 . . ?
C27 C28 H28A 109.6 . . ?
O8 C28 H28B 109.6 . . ?
C27 C28 H28B 109.6 . . ?
H28A C28 H28B 108.1 . . ?
C28 O8 Cu1 103.2(2) . . ?
C28 O8 H8O 116(3) . . ?
Cu1 O8 H8O 105(3) . . ?
C22 O7B Cu1 115.3(5) . . ?
C22 O7B H7O 119(7) . . ?
Cu1 O7B H7O 109(7) . . ?
C22 O7B H7P 124(9) . . ?
Cu1 O7B H7P 118(8) . . ?
C21 O6B Cu1 114.7(10) . . ?
C21 O6B H6O 100(5) . . ?
Cu1 O6B H6O 121(6) . . ?
C21 O6B H6P 124(5) . . ?
Cu1 O6B H6P 110(6) . . ?


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
O2 C1 C2 N1 37.1(4) . . . . ?
O2 C1 C2 C3 -144.4(3) . . . . ?
N1 C2 C3 C4 1.7(5) . . . . ?
C1 C2 C3 C4 -176.6(3) . . . . ?
C2 C3 C4 C5 0.0(5) . . . . ?
C3 C4 C5 C6 -2.0(5) . . . . ?
C4 C5 C6 N1 2.3(5) . . . . ?
C4 C5 C6 C7 -174.9(3) . . . . ?
N1 C6 C7 O1 21.1(4) . . . . ?
C5 C6 C7 O1 -161.7(3) . . . . ?
O4 C8 C9 N2 8.3(4) . . . . ?
O4 C8 C9 C10 -172.9(3) . . . . ?
N2 C9 C10 C11 0.3(5) . . . . ?
C8 C9 C10 C11 -178.5(3) . . . . ?
C9 C10 C11 C12 0.6(5) . . . . ?
C10 C11 C12 C13 -0.1(5) . . . . ?
C11 C12 C13 N2 -1.2(5) . . . . ?
C11 C12 C13 C14 177.6(3) . . . . ?
N2 C13 C14 O3 -10.1(4) . . . . ?
C12 C13 C14 O3 171.1(3) . . . . ?
O5 C15 C16 N3 -5.5(5) . . . . ?
O5 C15 C16 C17 176.6(3) . . . . ?
N3 C16 C17 C18 0.1(5) . . . . ?
C15 C16 C17 C18 177.9(4) . . . . ?
C16 C17 C18 C19 -0.5(5) . . . . ?
C17 C18 C19 C20 0.2(6) . . . . ?
C18 C19 C20 N3 0.5(5) . . . . ?
C18 C19 C20 C21 -178.7(3) . . . . ?
N3 C20 C21 O6B -20.5(5) . . . . ?
C19 C20 C21 O6B 158.8(5) . . . . ?
N3 C20 C21 O6 0.8(6) . . . . ?
C19 C20 C21 O6 -179.9(5) . . . . ?
C5 C6 N1 C2 -0.6(5) . . . . ?
C7 C6 N1 C2 176.6(3) . . . . ?
C5 C6 N1 Cu2 -177.9(2) . . . . ?
C7 C6 N1 Cu2 -0.7(4) . . . . ?
C3 C2 N1 C6 -1.4(4) . . . . ?
C1 C2 N1 C6 177.0(3) . . . . ?
C3 C2 N1 Cu2 175.9(2) . . . . ?
C1 C2 N1 Cu2 -5.7(4) . . . . ?
C10 C9 N2 C13 -1.6(5) . . . . ?
C8 C9 N2 C13 177.3(3) . . . . ?
C10 C9 N2 Cu2 174.6(3) . . . . ?
C8 C9 N2 Cu2 -6.5(4) . . . . ?
C12 C13 N2 C9 2.1(5) . . . . ?
C14 C13 N2 C9 -176.8(3) . . . . ?
C12 C13 N2 Cu2 -174.0(2) . . . . ?
C14 C13 N2 Cu2 7.0(4) . . . . ?
C17 C16 N3 C20 0.6(5) . . . . ?
C15 C16 N3 C20 -177.4(3) . . . . ?
C17 C16 N3 Cu1 172.6(3) . . . . ?
C15 C16 N3 Cu1 -5.5(4) . . . . ?
C19 C20 N3 C16 -1.0(5) . . . . ?
C21 C20 N3 C16 178.4(3) . . . . ?
C19 C20 N3 Cu1 -172.8(3) . . . . ?
C21 C20 N3 Cu1 6.6(4) . . . . ?
C6 C7 O1 Cu2 -26.6(3) . . . . ?
C2 C1 O2 Cu2 -42.1(3) . . . . ?
C13 C14 O3 Cu2 9.0(3) . . . . ?
C9 C8 O4 Cu2 -6.6(4) . . . . ?
C16 C15 O5 Cu1 13.1(4) . . . . ?
O6B C21 O6 Cu1 79(3) . . . . ?
C20 C21 O6 Cu1 -7.3(7) . . . . ?
C16 N3 Cu1 O6 179.2(4) . . . . ?
C20 N3 Cu1 O6 -8.6(4) . . . . ?
C16 N3 Cu1 N4 -102.7(6) . . . . ?
C20 N3 Cu1 N4 69.4(6) . . . . ?
C16 N3 Cu1 O5 10.2(2) . . . . ?
C20 N3 Cu1 O5 -177.7(3) . . . . ?
C16 N3 Cu1 O6B -166.2(4) . . . . ?
C20 N3 Cu1 O6B 6.0(4) . . . . ?
C16 N3 Cu1 O7 104.7(3) . . . . ?
C20 N3 Cu1 O7 -83.2(3) . . . . ?
C16 N3 Cu1 O7B 84.9(3) . . . . ?
C20 N3 Cu1 O7B -103.0(3) . . . . ?
C16 N3 Cu1 O8 -76.7(2) . . . . ?
C20 N3 Cu1 O8 95.4(2) . . . . ?
C21 O6 Cu1 N3 8.5(6) . . . . ?
C21 O6 Cu1 N4 -160.9(6) . . . . ?
C21 O6 Cu1 O5 43.2(13) . . . . ?
C21 O6 Cu1 O6B -69(3) . . . . ?
C21 O6 Cu1 O7 123.9(7) . . . . ?
C21 O6 Cu1 O7B 125.1(6) . . . . ?
C21 O6 Cu1 O8 -84.4(7) . . . . ?
C15 O5 Cu1 N3 -12.7(2) . . . . ?
C15 O5 Cu1 O6 -47.4(10) . . . . ?
C15 O5 Cu1 N4 157.1(2) . . . . ?
C15 O5 Cu1 O6B -1.8(10) . . . . ?
C15 O5 Cu1 O7 -125.1(3) . . . . ?
C15 O5 Cu1 O7B -132.3(3) . . . . ?
C15 O5 Cu1 O8 82.4(2) . . . . ?
C9 N2 Cu2 O4 2.3(3) . . . . ?
C13 N2 Cu2 O4 178.6(3) . . . . ?
C9 N2 Cu2 O3 -177.8(3) . . . . ?
C13 N2 Cu2 O3 -1.5(2) . . . . ?
C9 N2 Cu2 O1 -94.3(2) . . . . ?
C13 N2 Cu2 O1 82.0(3) . . . . ?
C9 N2 Cu2 O2 92.4(3) . . . . ?
C13 N2 Cu2 O2 -91.3(3) . . . . ?
C8 O4 Cu2 N1 179.5(3) . . . . ?
C8 O4 Cu2 O3 2.4(5) . . . . ?
C8 O4 Cu2 O1 102.4(3) . . . . ?
C8 O4 Cu2 O2 -104.9(3) . . . . ?
C6 N1 Cu2 O4 -106.9(2) . . . . ?
C2 N1 Cu2 O4 75.8(2) . . . . ?
C6 N1 Cu2 O3 72.2(2) . . . . ?
C2 N1 Cu2 O3 -105.1(2) . . . . ?
C6 N1 Cu2 O1 -11.0(2) . . . . ?
C2 N1 Cu2 O1 171.7(2) . . . . ?
C6 N1 Cu2 O2 162.9(2) . . . . ?
C2 N1 Cu2 O2 -14.4(2) . . . . ?
C14 O3 Cu2 N2 -4.6(2) . . . . ?
C14 O3 Cu2 O4 -4.3(5) . . . . ?
C14 O3 Cu2 N1 178.7(2) . . . . ?
C14 O3 Cu2 O1 -106.1(2) . . . . ?
C14 O3 Cu2 O2 103.0(2) . . . . ?
C7 O1 Cu2 N2 -157.7(2) . . . . ?
C7 O1 Cu2 O4 118.5(2) . . . . ?
C7 O1 Cu2 N1 21.3(2) . . . . ?
C7 O1 Cu2 O3 -78.6(2) . . . . ?
C7 O1 Cu2 O2 9.1(3) . . . . ?
C1 O2 Cu2 N2 -149.7(2) . . . . ?
C1 O2 Cu2 O4 -66.8(2) . . . . ?
C1 O2 Cu2 N1 31.7(2) . . . . ?
C1 O2 Cu2 O3 129.8(2) . . . . ?
C1 O2 Cu2 O1 44.0(3) . . . . ?
N3 Cu1 O7 C22 -162.2(3) . . . . ?
O6 Cu1 O7 C22 121.4(6) . . . . ?
N4 Cu1 O7 C22 22.9(3) . . . . ?
O5 Cu1 O7 C22 -77.8(3) . . . . ?
O6B Cu1 O7 C22 118.2(6) . . . . ?
O7B Cu1 O7 C22 -54.8(9) . . . . ?
O8 Cu1 O7 C22 20.8(6) . . . . ?
Cu1 O7 C22 O7B 72.0(11) . . . . ?
Cu1 O7 C22 C23 -27.3(4) . . . . ?
O7B C22 C23 N4 -12.0(5) . . . . ?
O7 C22 C23 N4 17.9(4) . . . . ?
O7B C22 C23 C24 168.7(4) . . . . ?
O7 C22 C23 C24 -161.3(4) . . . . ?
N4 C23 C24 C25 0.2(5) . . . . ?
C22 C23 C24 C25 179.4(3) . . . . ?
C23 C24 C25 C26 -0.2(6) . . . . ?
C24 C25 C26 C27 -0.1(6) . . . . ?
C25 C26 C27 N4 0.3(6) . . . . ?
C25 C26 C27 C28 -177.2(4) . . . . ?
C24 C23 N4 C27 0.0(4) . . . . ?
C22 C23 N4 C27 -179.3(3) . . . . ?
C24 C23 N4 Cu1 -178.0(2) . . . . ?
C22 C23 N4 Cu1 2.8(4) . . . . ?
C26 C27 N4 C23 -0.3(5) . . . . ?
C28 C27 N4 C23 177.4(3) . . . . ?
C26 C27 N4 Cu1 177.7(3) . . . . ?
C28 C27 N4 Cu1 -4.6(4) . . . . ?
N3 Cu1 N4 C23 -169.2(5) . . . . ?
O6 Cu1 N4 C23 -92.4(4) . . . . ?
O5 Cu1 N4 C23 79.6(2) . . . . ?
O6B Cu1 N4 C23 -107.2(3) . . . . ?
O7 Cu1 N4 C23 -15.0(3) . . . . ?
O7B Cu1 N4 C23 3.7(3) . . . . ?
O8 Cu1 N4 C23 164.0(2) . . . . ?
N3 Cu1 N4 C27 12.8(7) . . . . ?
O6 Cu1 N4 C27 89.6(3) . . . . ?
O5 Cu1 N4 C27 -98.3(2) . . . . ?
O6B Cu1 N4 C27 74.8(3) . . . . ?
O7 Cu1 N4 C27 167.0(3) . . . . ?
O7B Cu1 N4 C27 -174.2(3) . . . . ?
O8 Cu1 N4 C27 -14.0(2) . . . . ?
N4 C27 C28 O8 34.0(4) . . . . ?
C26 C27 C28 O8 -148.3(3) . . . . ?
C27 C28 O8 Cu1 -39.8(3) . . . . ?
N3 Cu1 O8 C28 -145.1(2) . . . . ?
O6 Cu1 O8 C28 -62.1(5) . . . . ?
N4 Cu1 O8 C28 30.0(2) . . . . ?
O5 Cu1 O8 C28 133.1(2) . . . . ?
O6B Cu1 O8 C28 -66.1(5) . . . . ?
O7 Cu1 O8 C28 32.1(4) . . . . ?
O7B Cu1 O8 C28 63.0(4) . . . . ?
C23 C22 O7B Cu1 14.5(6) . . . . ?
O7 C22 O7B Cu1 -76.2(11) . . . . ?
N3 Cu1 O7B C22 167.7(4) . . . . ?
O6 Cu1 O7B C22 82.9(7) . . . . ?
N4 Cu1 O7B C22 -10.8(4) . . . . ?
O5 Cu1 O7B C22 -116.6(5) . . . . ?
O6B Cu1 O7B C22 79.1(7) . . . . ?
O7 Cu1 O7B C22 86.6(11) . . . . ?
O8 Cu1 O7B C22 -44.2(7) . . . . ?
O6 C21 O6B Cu1 -75(3) . . . . ?
C20 C21 O6B Cu1 25.4(6) . . . . ?
N3 Cu1 O6B C21 -18.4(5) . . . . ?
O6 Cu1 O6B C21 82(4) . . . . ?
N4 Cu1 O6B C21 171.3(5) . . . . ?
O5 Cu1 O6B C21 -29.5(13) . . . . ?
O7 Cu1 O6B C21 94.4(6) . . . . ?
O7B Cu1 O6B C21 96.7(6) . . . . ?
O8 Cu1 O6B C21 -113.2(5) . . . . ?

# END of CIF
