# 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_shelx
_audit_block_doi                 10.5517/cc133z9h
_database_code_depnum_ccdc_archive 'CCDC 1016716'
_audit_update_record             
;
2015-07-17 deposited with the CCDC.
2015-07-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 C69 H54 N10 O6, 3(H2 O)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C69 H60 N10 O9'
_chemical_formula_weight         1173.27

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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.68(2)
_cell_length_b                   16.44(2)
_cell_length_c                   17.69(2)
_cell_angle_alpha                91.408(12)
_cell_angle_beta                 115.658(13)
_cell_angle_gamma                117.999(12)
_cell_volume                     3477(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    302(2)
_cell_measurement_reflns_used    3990
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.3

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.076
_shelx_estimated_absorpt_T_min   0.985
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_process_details   
;
R. H. Blessing Acta Crystallogr., Section A 1995, 51, 33-38
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      302(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28426
_diffrn_reflns_av_unetI/netI     0.2520
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.998
_diffrn_reflns_theta_max         26.250
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             13667
_reflns_number_gt                3000
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r14k (Rigaku, 2012)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r14k (Rigaku, 2012)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r14k (Rigaku, 2012)
;
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Mercury 3.5'
_computing_publication_material  'Word 2010'

_refine_special_details          
;
 Diffuse, disordered solvent molecules could not be adequately modeled.  The
 bypass procedure in Platon (Spek, 1990) was used to remove the electronic
 contribution from these solvents. The cumulative potential solvent accessible void
 volume was 757 Α³ and the electron count/cell = 89. Based onthe electron count and
 TG results we assume that it could account for one molecule each of chloroform (58), methanol (18) and water (10).
 But, the reported formula reflects only the atoms used in the refinement.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0986P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13667
_refine_ls_number_parameters     799
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2087
_refine_ls_R_factor_gt           0.0886
_refine_ls_wR_factor_ref         0.2532
_refine_ls_wR_factor_gt          0.2216
_refine_ls_goodness_of_fit_ref   0.707
_refine_ls_restrained_S_all      0.707
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
C11 C 0.8288(4) 0.0892(4) 0.4287(3) 0.0646(15) Uani 1 1 d . . . . .
H11A H 0.8083 0.0849 0.3679 0.078 Uiso 1 1 calc R U . . .
H11B H 0.7791 0.0271 0.4315 0.078 Uiso 1 1 calc R U . . .
C12 C 0.9461(4) 0.1139(4) 0.4803(3) 0.0602(14) Uani 1 1 d . . . . .
C13 C 1.1233(5) 0.1729(4) 0.5320(4) 0.0772(16) Uani 1 1 d . . . . .
C14 C 1.2354(6) 0.2223(5) 0.5479(5) 0.097(2) Uani 1 1 d . . . . .
H14 H 1.2570 0.2587 0.5130 0.117 Uiso 1 1 calc R U . . .
C15 C 1.3093(5) 0.2113(6) 0.6203(6) 0.126(3) Uani 1 1 d . . . . .
H15 H 1.3833 0.2423 0.6335 0.151 Uiso 1 1 calc R U . . .
C16 C 1.2804(6) 0.1566(5) 0.6751(4) 0.103(2) Uani 1 1 d . . . . .
H16 H 1.3343 0.1519 0.7219 0.123 Uiso 1 1 calc R U . . .
C17 C 1.1738(6) 0.1110(4) 0.6592(3) 0.0826(17) Uani 1 1 d . . . . .
H17 H 1.1534 0.0748 0.6947 0.099 Uiso 1 1 calc R U . . .
C18 C 1.0935(5) 0.1203(4) 0.5861(3) 0.0733(16) Uani 1 1 d . . . . .
C19 C 0.9145(4) 0.0221(4) 0.5912(3) 0.0712(16) Uani 1 1 d . . . . .
H19A H 0.9308 -0.0276 0.6041 0.085 Uiso 1 1 calc R U . . .
H19B H 0.8355 -0.0089 0.5488 0.085 Uiso 1 1 calc R U . . .
C21 C 0.8597(4) 0.2496(4) 0.4322(3) 0.0629(15) Uani 1 1 d . . . . .
H21A H 0.9288 0.2634 0.4354 0.076 Uiso 1 1 calc R U . . .
H21B H 0.8058 0.2352 0.3713 0.076 Uiso 1 1 calc R U . . .
C22 C 0.8802(4) 0.3342(4) 0.4832(3) 0.0615(15) Uani 1 1 d . . . . .
C23 C 0.8614(5) 0.4428(5) 0.5317(4) 0.0668(15) Uani 1 1 d . . . . .
C24 C 0.8231(6) 0.4970(6) 0.5471(4) 0.094(2) Uani 1 1 d . . . . .
H24 H 0.7493 0.4795 0.5115 0.112 Uiso 1 1 calc R U . . .
C25 C 0.9008(9) 0.5816(6) 0.6199(6) 0.117(3) Uani 1 1 d . . . . .
H25 H 0.8764 0.6192 0.6324 0.140 Uiso 1 1 calc R U . . .
C26 C 1.0104(8) 0.6091(6) 0.6719(5) 0.107(2) Uani 1 1 d . . . . .
H26 H 1.0596 0.6670 0.7162 0.128 Uiso 1 1 calc R U . . .
C27 C 1.0483(6) 0.5541(5) 0.6602(3) 0.0853(19) Uani 1 1 d . . . . .
H27 H 1.1215 0.5707 0.6969 0.102 Uiso 1 1 calc R U . . .
C28 C 0.9707(5) 0.4701(4) 0.5894(3) 0.0698(16) Uani 1 1 d . . . . .
C29 C 1.0849(4) 0.3976(4) 0.5967(3) 0.0731(17) Uani 1 1 d . . . . .
H29A H 1.1497 0.4628 0.6228 0.088 Uiso 1 1 calc R U . . .
H29B H 1.0876 0.3662 0.5513 0.088 Uiso 1 1 calc R U . . .
C31 C 0.6967(4) 0.1238(4) 0.4358(3) 0.0654(14) Uani 1 1 d . . . . .
H31A H 0.6508 0.0906 0.3736 0.078 Uiso 1 1 calc R U . . .
H31B H 0.6870 0.1764 0.4453 0.078 Uiso 1 1 calc R U . . .
C32 C 0.6582(4) 0.0556(4) 0.4849(3) 0.0591(14) Uani 1 1 d . . . . .
C33 C 0.5980(4) -0.0727(5) 0.5214(4) 0.0699(15) Uani 1 1 d . . . . .
C34 C 0.5583(4) -0.1655(5) 0.5301(4) 0.097(2) Uani 1 1 d . . . . .
H34 H 0.5445 -0.2152 0.4912 0.117 Uiso 1 1 calc R U . . .
C35 C 0.5398(5) -0.1801(7) 0.6038(6) 0.119(3) Uani 1 1 d . . . . .
H35 H 0.5138 -0.2411 0.6118 0.143 Uiso 1 1 calc R U . . .
C36 C 0.5588(6) -0.1083(8) 0.6623(5) 0.113(3) Uani 1 1 d . . . . .
H36 H 0.5411 -0.1218 0.7062 0.135 Uiso 1 1 calc R U . . .
C37 C 0.6027(5) -0.0193(6) 0.6553(4) 0.100(2) Uani 1 1 d . . . . .
H37 H 0.6205 0.0307 0.6965 0.120 Uiso 1 1 calc R U . . .
C38 C 0.6225(4) -0.0009(5) 0.5846(3) 0.0671(15) Uani 1 1 d . . . . .
C39 C 0.6934(4) 0.1767(5) 0.6044(3) 0.0887(19) Uani 1 1 d . . . . .
H39A H 0.6601 0.1681 0.6410 0.106 Uiso 1 1 calc R U . . .
H39B H 0.6641 0.2057 0.5612 0.106 Uiso 1 1 calc R U . . .
C110 C 0.9412(4) 0.0813(4) 0.6742(3) 0.0684(15) Uani 1 1 d . . . . .
H11C H 0.9108 0.1219 0.6598 0.082 Uiso 1 1 calc R U . . .
H11D H 1.0217 0.1224 0.7119 0.082 Uiso 1 1 calc R U . . .
C111 C 0.8900(4) 0.0136(4) 0.7231(3) 0.0812(18) Uani 1 1 d . . . . .
H11E H 0.8173 0.0035 0.7061 0.097 Uiso 1 1 calc R U . . .
H11F H 0.8794 -0.0484 0.7057 0.097 Uiso 1 1 calc R U . . .
C112 C 0.9358(5) 0.1016(4) 0.8648(3) 0.0755(17) Uani 1 1 d . . . . .
C113 C 0.9989(6) 0.1291(4) 0.9601(4) 0.0777(17) Uani 1 1 d . . . . .
C114 C 0.9654(7) 0.1623(5) 1.0085(5) 0.129(3) Uani 1 1 d . . . . .
H114 H 0.9027 0.1667 0.9796 0.154 Uiso 1 1 calc R U . . .
C115 C 1.0269(10) 0.1899(7) 1.1031(6) 0.156(4) Uani 1 1 d . . . . .
H115 H 1.0039 0.2114 1.1352 0.187 Uiso 1 1 calc R U . . .
C116 C 1.1136(10) 0.1844(7) 1.1418(6) 0.143(4) Uani 1 1 d . . . . .
H116 H 1.1524 0.2037 1.2027 0.171 Uiso 1 1 calc R U . . .
C117 C 1.2534(10) 0.1455(9) 1.1402(6) 0.191(7) Uani 1 1 d . . . . .
H117 H 1.2970 0.1652 1.2009 0.230 Uiso 1 1 calc R U . . .
C118 C 1.2823(9) 0.1116(8) 1.0904(6) 0.159(4) Uani 1 1 d . . . . .
H118 H 1.3469 0.1098 1.1181 0.191 Uiso 1 1 calc R U . . .
C119 C 1.2165(6) 0.0784(5) 0.9966(5) 0.128(3) Uani 1 1 d . . . . .
H119 H 1.2370 0.0537 0.9643 0.153 Uiso 1 1 calc R U . . .
C120 C 1.1249(5) 0.0833(5) 0.9559(4) 0.089(2) Uani 1 1 d . . . . .
C121 C 1.0885(5) 0.1209(4) 1.0022(3) 0.084(2) Uani 1 1 d . . . . .
C122 C 1.1563(8) 0.1508(5) 1.0991(4) 0.132(3) Uani 1 1 d . . . . .
C123 C 1.0555(5) 0.0472(5) 0.8575(4) 0.0790(17) Uani 1 1 d . . . . .
C210 C 1.0928(4) 0.3445(4) 0.6671(3) 0.0718(17) Uani 1 1 d . . . . .
H21C H 1.0340 0.2771 0.6393 0.086 Uiso 1 1 calc R U . . .
H21D H 1.0791 0.3698 0.7078 0.086 Uiso 1 1 calc R U . . .
C211 C 1.2060(4) 0.3523(4) 0.7191(3) 0.0769(17) Uani 1 1 d . . . . .
H21E H 1.1930 0.2882 0.7165 0.092 Uiso 1 1 calc R U . . .
H21F H 1.2508 0.3824 0.6921 0.092 Uiso 1 1 calc R U . . .
C212 C 1.2546(4) 0.3561(4) 0.8734(3) 0.0624(15) Uani 1 1 d . . . . .
C213 C 1.3208(4) 0.4124(4) 0.9653(3) 0.0673(15) Uani 1 1 d . . . . .
C214 C 1.3157(5) 0.3640(5) 1.0282(4) 0.098(2) Uani 1 1 d . . . . .
H214 H 1.2719 0.2973 1.0128 0.118 Uiso 1 1 calc R U . . .
C215 C 1.3809(6) 0.4214(7) 1.1179(4) 0.123(3) Uani 1 1 d . . . . .
H215 H 1.3762 0.3909 1.1609 0.147 Uiso 1 1 calc R U . . .
C216 C 1.4471(6) 0.5158(8) 1.1412(4) 0.126(3) Uani 1 1 d . . . . .
H216 H 1.4881 0.5494 1.2002 0.152 Uiso 1 1 calc R U . . .
C217 C 1.5277(6) 0.6672(7) 1.1052(5) 0.125(3) Uani 1 1 d . . . . .
H217 H 1.5702 0.7021 1.1640 0.150 Uiso 1 1 calc R U . . .
C218 C 1.5341(6) 0.7142(6) 1.0439(6) 0.144(3) Uani 1 1 d . . . . .
H218 H 1.5807 0.7807 1.0601 0.172 Uiso 1 1 calc R U . . .
C219 C 1.4683(5) 0.6597(5) 0.9547(5) 0.115(2) Uani 1 1 d . . . . .
H219 H 1.4728 0.6919 0.9128 0.138 Uiso 1 1 calc R U . . .
C220 C 1.3987(4) 0.5622(4) 0.9277(3) 0.0757(16) Uani 1 1 d . . . . .
C221 C 1.3908(4) 0.5133(5) 0.9904(3) 0.0690(16) Uani 1 1 d . . . . .
C222 C 1.4580(5) 0.5669(6) 1.0811(4) 0.0892(19) Uani 1 1 d . . . . .
C223 C 1.3341(4) 0.5094(5) 0.8335(4) 0.0768(16) Uani 1 1 d . . . . .
C310 C 0.8218(4) 0.2449(4) 0.6616(3) 0.0750(17) Uani 1 1 d . . . . .
H31C H 0.8514 0.2151 0.7035 0.090 Uiso 1 1 calc R U . . .
H31D H 0.8550 0.2553 0.6247 0.090 Uiso 1 1 calc R U . . .
C311 C 0.8538(5) 0.3414(4) 0.7103(3) 0.0769(17) Uani 1 1 d . . . . .
H31E H 0.9198 0.3920 0.7111 0.092 Uiso 1 1 calc R U . . .
H31F H 0.7936 0.3522 0.6788 0.092 Uiso 1 1 calc R U . . .
C312 C 0.9869(5) 0.3758(4) 0.8675(3) 0.0686(15) Uani 1 1 d . . . . .
C313 C 1.0131(5) 0.3895(4) 0.9578(3) 0.0659(15) Uani 1 1 d . . . . .
C314 C 1.1158(5) 0.4220(4) 1.0242(4) 0.0849(18) Uani 1 1 d . . . . .
H314 H 1.1721 0.4350 1.0120 0.102 Uiso 1 1 calc R U . . .
C315 C 1.1422(6) 0.4373(5) 1.1131(4) 0.099(2) Uani 1 1 d . . . . .
H315 H 1.2143 0.4586 1.1577 0.119 Uiso 1 1 calc R U . . .
C316 C 1.0635(7) 0.4212(4) 1.1319(4) 0.101(2) Uani 1 1 d . . . . .
H316 H 1.0818 0.4325 1.1902 0.121 Uiso 1 1 calc R U . . .
C317 C 0.8658(7) 0.3656(5) 1.0833(4) 0.111(2) Uani 1 1 d . . . . .
H317 H 0.8816 0.3718 1.1409 0.134 Uiso 1 1 calc R U . . .
C318 C 0.7594(7) 0.3355(6) 1.0186(5) 0.138(3) Uani 1 1 d . . . . .
H318 H 0.7049 0.3253 1.0324 0.165 Uiso 1 1 calc R U . . .
C319 C 0.7337(6) 0.3202(5) 0.9290(4) 0.118(2) Uani 1 1 d . . . . .
H319 H 0.6613 0.2980 0.8843 0.141 Uiso 1 1 calc R U . . .
C320 C 0.8170(5) 0.3385(4) 0.9084(3) 0.0762(17) Uani 1 1 d . . . . .
C321 C 0.9255(5) 0.3705(4) 0.9766(3) 0.0689(15) Uani 1 1 d . . . . .
C322 C 0.9513(5) 0.3871(4) 1.0652(3) 0.0795(17) Uani 1 1 d . . . . .
C323 C 0.7906(5) 0.3269(4) 0.8173(4) 0.0810(18) Uani 1 1 d . . . . .
N1 N 0.8165(3) 0.1632(3) 0.4637(2) 0.0564(11) Uani 1 1 d . . . . .
N12 N 1.0277(4) 0.1672(3) 0.4652(3) 0.0774(14) Uani 1 1 d . . . . .
N19 N 0.9815(3) 0.0838(3) 0.5532(2) 0.0628(12) Uani 1 1 d . . . . .
N22 N 0.8069(4) 0.3597(4) 0.4681(2) 0.0672(13) Uani 1 1 d . . . . .
N28 N 0.9839(3) 0.4011(3) 0.5565(2) 0.0624(12) Uani 1 1 d . . . . .
N32 N 0.6214(3) -0.0366(4) 0.4599(2) 0.0675(12) Uani 1 1 d . . . . .
N38 N 0.6617(3) 0.0808(4) 0.5588(3) 0.0694(12) Uani 1 1 d . . . . .
N111 N 0.9625(4) 0.0540(3) 0.8195(2) 0.0686(13) Uani 1 1 d . . . . .
N211 N 1.2694(3) 0.4094(3) 0.8129(2) 0.0612(11) Uani 1 1 d . . . . .
N311 N 0.8768(4) 0.3475(3) 0.8011(2) 0.0632(12) Uani 1 1 d . . . . .
O112 O 0.8590(4) 0.1143(3) 0.8225(3) 0.1072(15) Uani 1 1 d . . . . .
O123 O 1.0754(4) 0.0111(3) 0.8127(3) 0.1087(15) Uani 1 1 d . . . . .
O212 O 1.1906(3) 0.2705(3) 0.8479(2) 0.0958(14) Uani 1 1 d . . . . .
O223 O 1.3339(3) 0.5478(3) 0.7746(3) 0.1149(17) Uani 1 1 d . . . . .
O312 O 1.0558(3) 0.3909(3) 0.8459(2) 0.0937(13) Uani 1 1 d . . . . .
O323 O 0.6973(3) 0.3003(3) 0.7566(2) 0.1100(15) Uani 1 1 d . . . . .
O100 O 0.4986(4) 0.1280(4) 0.7244(3) 0.1294(17) Uani 1 1 d G . . . .
H10A H 0.4683 0.0937 0.6729 0.194 Uiso 1 1 d G U . . .
H10B H 0.5544 0.1823 0.7340 0.194 Uiso 1 1 d G U . . .
O101 O 1.3833(5) 0.7044(5) 0.7081(4) 0.210(3) Uani 1 1 d G . . . .
H10C H 1.3496 0.7015 0.6544 0.315 Uiso 1 1 d G U . . .
H10D H 1.3531 0.6485 0.7144 0.315 Uiso 1 1 d G U . . .
O102 O 1.0095(7) 0.1787(4) 0.2956(4) 0.233(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 N1 1.480(6) . ?
C11 C12 1.485(7) . ?
C12 N12 1.316(5) . ?
C12 N19 1.374(6) . ?
C13 C18 1.390(7) . ?
C13 N12 1.407(7) . ?
C13 C14 1.430(8) . ?
C14 C15 1.392(9) . ?
C15 C16 1.412(10) . ?
C16 C17 1.356(8) . ?
C17 C18 1.437(7) . ?
C18 N19 1.374(6) . ?
C19 N19 1.493(6) . ?
C19 C110 1.514(6) . ?
C21 C22 1.457(7) . ?
C21 N1 1.501(6) . ?
C22 N22 1.327(6) . ?
C22 N28 1.399(6) . ?
C23 N22 1.363(7) . ?
C23 C24 1.364(8) . ?
C23 C28 1.385(7) . ?
C24 C25 1.429(9) . ?
C25 C26 1.373(9) . ?
C26 C27 1.348(8) . ?
C27 C28 1.406(7) . ?
C28 N28 1.399(7) . ?
C29 N28 1.461(6) . ?
C29 C210 1.532(6) . ?
C31 N1 1.492(6) . ?
C31 C32 1.498(6) . ?
C32 N32 1.325(6) . ?
C32 N38 1.331(6) . ?
C33 N32 1.357(6) . ?
C33 C38 1.389(7) . ?
C33 C34 1.395(8) . ?
C34 C35 1.456(9) . ?
C35 C36 1.378(10) . ?
C36 C37 1.330(10) . ?
C37 C38 1.420(7) . ?
C38 N38 1.375(7) . ?
C39 N38 1.496(7) . ?
C39 C310 1.547(7) . ?
C110 C111 1.564(6) . ?
C111 N111 1.482(6) . ?
C112 O112 1.231(6) . ?
C112 N111 1.414(7) . ?
C112 C113 1.457(7) . ?
C113 C121 1.349(8) . ?
C113 C114 1.394(8) . ?
C114 C115 1.446(10) . ?
C115 C116 1.279(12) . ?
C116 C122 1.446(12) . ?
C117 C118 1.361(14) . ?
C117 C122 1.422(13) . ?
C118 C119 1.435(10) . ?
C119 C120 1.343(9) . ?
C120 C121 1.445(8) . ?
C120 C123 1.507(8) . ?
C121 C122 1.483(8) . ?
C123 O123 1.201(6) . ?
C123 N111 1.377(7) . ?
C210 C211 1.543(6) . ?
C211 N211 1.497(6) . ?
C212 O212 1.201(6) . ?
C212 N211 1.428(6) . ?
C212 C213 1.463(7) . ?
C213 C214 1.391(7) . ?
C213 C221 1.409(7) . ?
C214 C215 1.439(9) . ?
C215 C216 1.320(10) . ?
C216 C222 1.391(9) . ?
C217 C218 1.358(10) . ?
C217 C222 1.402(9) . ?
C218 C219 1.418(9) . ?
C219 C220 1.362(8) . ?
C220 C221 1.402(7) . ?
C220 C223 1.482(7) . ?
C221 C222 1.434(7) . ?
C223 O223 1.231(6) . ?
C223 N211 1.396(7) . ?
C310 C311 1.523(7) . ?
C311 N311 1.475(5) . ?
C312 O312 1.218(5) . ?
C312 N311 1.428(6) . ?
C312 C313 1.449(6) . ?
C313 C314 1.334(7) . ?
C313 C321 1.447(7) . ?
C314 C315 1.422(8) . ?
C315 C316 1.325(8) . ?
C316 C322 1.430(8) . ?
C317 C318 1.372(9) . ?
C317 C322 1.399(8) . ?
C318 C319 1.439(8) . ?
C319 C320 1.406(7) . ?
C320 C321 1.405(7) . ?
C320 C323 1.463(7) . ?
C321 C322 1.422(7) . ?
C323 O323 1.225(6) . ?
C323 N311 1.391(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
N1 C11 C12 110.2(4) . . ?
N12 C12 N19 112.1(5) . . ?
N12 C12 C11 126.2(5) . . ?
N19 C12 C11 121.6(4) . . ?
C18 C13 N12 108.5(5) . . ?
C18 C13 C14 121.8(6) . . ?
N12 C13 C14 129.8(6) . . ?
C15 C14 C13 114.3(6) . . ?
C14 C15 C16 125.0(6) . . ?
C17 C16 C15 119.8(7) . . ?
C16 C17 C18 118.1(6) . . ?
N19 C18 C13 106.8(5) . . ?
N19 C18 C17 132.1(6) . . ?
C13 C18 C17 121.1(6) . . ?
N19 C19 C110 110.9(4) . . ?
C22 C21 N1 112.4(4) . . ?
N22 C22 N28 110.6(5) . . ?
N22 C22 C21 126.4(5) . . ?
N28 C22 C21 123.0(5) . . ?
N22 C23 C24 130.0(7) . . ?
N22 C23 C28 111.4(6) . . ?
C24 C23 C28 118.6(7) . . ?
C23 C24 C25 117.3(7) . . ?
C26 C25 C24 122.0(8) . . ?
C27 C26 C25 121.4(8) . . ?
C26 C27 C28 116.1(7) . . ?
C23 C28 N28 104.8(5) . . ?
C23 C28 C27 124.4(7) . . ?
N28 C28 C27 130.6(7) . . ?
N28 C29 C210 113.9(4) . . ?
N1 C31 C32 112.0(4) . . ?
N32 C32 N38 113.3(4) . . ?
N32 C32 C31 122.1(5) . . ?
N38 C32 C31 124.6(5) . . ?
N32 C33 C38 110.7(6) . . ?
N32 C33 C34 130.3(6) . . ?
C38 C33 C34 118.9(6) . . ?
C33 C34 C35 115.9(7) . . ?
C36 C35 C34 123.5(8) . . ?
C37 C36 C35 119.1(8) . . ?
C36 C37 C38 119.8(8) . . ?
N38 C38 C33 104.7(5) . . ?
N38 C38 C37 132.7(7) . . ?
C33 C38 C37 122.5(6) . . ?
N38 C39 C310 111.6(5) . . ?
C19 C110 C111 110.0(4) . . ?
N111 C111 C110 112.0(4) . . ?
O112 C112 N111 119.0(5) . . ?
O112 C112 C113 123.9(7) . . ?
N111 C112 C113 117.1(6) . . ?
C121 C113 C114 119.5(6) . . ?
C121 C113 C112 120.6(6) . . ?
C114 C113 C112 119.9(7) . . ?
C113 C114 C115 120.7(8) . . ?
C116 C115 C114 118.9(11) . . ?
C115 C116 C122 125.6(10) . . ?
C118 C117 C122 119.8(10) . . ?
C117 C118 C119 122.2(11) . . ?
C120 C119 C118 119.2(9) . . ?
C119 C120 C121 123.1(6) . . ?
C119 C120 C123 118.9(7) . . ?
C121 C120 C123 118.0(6) . . ?
C113 C121 C120 122.3(5) . . ?
C113 C121 C122 121.9(8) . . ?
C120 C121 C122 115.9(8) . . ?
C117 C122 C116 127.0(8) . . ?
C117 C122 C121 119.6(10) . . ?
C116 C122 C121 113.4(10) . . ?
O123 C123 N111 120.0(5) . . ?
O123 C123 C120 123.6(6) . . ?
N111 C123 C120 116.3(6) . . ?
C29 C210 C211 114.5(4) . . ?
N211 C211 C210 112.2(4) . . ?
O212 C212 N211 120.3(4) . . ?
O212 C212 C213 123.9(5) . . ?
N211 C212 C213 115.8(5) . . ?
C214 C213 C221 120.4(5) . . ?
C214 C213 C212 118.6(6) . . ?
C221 C213 C212 121.0(5) . . ?
C213 C214 C215 117.3(6) . . ?
C216 C215 C214 122.1(7) . . ?
C215 C216 C222 122.6(6) . . ?
C218 C217 C222 120.9(7) . . ?
C217 C218 C219 118.6(8) . . ?
C220 C219 C218 122.9(7) . . ?
C219 C220 C221 118.9(6) . . ?
C219 C220 C223 120.2(6) . . ?
C221 C220 C223 120.9(5) . . ?
C220 C221 C213 120.7(5) . . ?
C220 C221 C222 119.0(6) . . ?
C213 C221 C222 120.2(6) . . ?
C216 C222 C217 123.0(7) . . ?
C216 C222 C221 117.3(7) . . ?
C217 C222 C221 119.7(7) . . ?
O223 C223 N211 119.7(5) . . ?
O223 C223 C220 124.5(6) . . ?
N211 C223 C220 115.8(5) . . ?
C311 C310 C39 111.5(5) . . ?
N311 C311 C310 113.2(4) . . ?
O312 C312 N311 118.3(5) . . ?
O312 C312 C313 123.0(5) . . ?
N311 C312 C313 118.6(5) . . ?
C314 C313 C321 119.0(5) . . ?
C314 C313 C312 122.4(5) . . ?
C321 C313 C312 118.6(5) . . ?
C313 C314 C315 122.5(6) . . ?
C316 C315 C314 119.6(6) . . ?
C315 C316 C322 122.0(6) . . ?
C318 C317 C322 122.1(6) . . ?
C317 C318 C319 118.7(6) . . ?
C320 C319 C318 120.6(6) . . ?
C321 C320 C319 119.1(5) . . ?
C321 C320 C323 121.2(5) . . ?
C319 C320 C323 119.7(6) . . ?
C320 C321 C322 120.4(5) . . ?
C320 C321 C313 120.6(4) . . ?
C322 C321 C313 119.0(5) . . ?
C317 C322 C321 119.0(6) . . ?
C317 C322 C316 122.9(6) . . ?
C321 C322 C316 118.0(6) . . ?
O323 C323 N311 120.1(5) . . ?
O323 C323 C320 122.7(5) . . ?
N311 C323 C320 117.2(5) . . ?
C11 N1 C31 110.4(4) . . ?
C11 N1 C21 110.0(4) . . ?
C31 N1 C21 109.8(4) . . ?
C12 N12 C13 105.8(4) . . ?
C12 N19 C18 106.8(4) . . ?
C12 N19 C19 128.3(4) . . ?
C18 N19 C19 124.8(4) . . ?
C22 N22 C23 106.5(5) . . ?
C22 N28 C28 106.7(5) . . ?
C22 N28 C29 127.8(5) . . ?
C28 N28 C29 125.4(5) . . ?
C32 N32 C33 104.3(4) . . ?
C32 N38 C38 107.0(5) . . ?
C32 N38 C39 128.4(5) . . ?
C38 N38 C39 124.4(5) . . ?
C123 N111 C112 124.8(5) . . ?
C123 N111 C111 116.8(5) . . ?
C112 N111 C111 118.3(5) . . ?
C223 N211 C212 125.5(4) . . ?
C223 N211 C211 118.0(4) . . ?
C212 N211 C211 116.4(5) . . ?
C323 N311 C312 123.8(4) . . ?
C323 N311 C311 118.2(4) . . ?
C312 N311 C311 118.1(4) . . ?

_refine_diff_density_max         0.275
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.060

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 0.500 1.000 1.000 402 48 ' '
2 0.500 0.500 0.500 355 41 ' '
_platon_squeeze_details          
;
 Diffuse, disordered solvent molecules could not be adequately modeled.  The
 bypass procedure in Platon (Spek, 1990) was used to remove the electronic
 contribution from these solvents. The cumulative potential solvent accessible void
 volume was 757 Α³ and the electron count/cell = 89. Based onthe electron count and
 TG results we assume that it could account for one molecule each of chloroform (58), methanol (18) and water (10).
 But, the reported formula reflects only the atoms used in the refinement.
;
# start Validation Reply Form
_vrf_PLAT026_shelx               
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         22 %     
RESPONSE: The crystal diffraction for the ligand was poor. Only 6317 reflections out of the observed 28426 reflections 
(theta(max) = 13.5) were of I/sigma > 2, which is considered as relevant data. The compound diffracted weakly especially in the 
higher angles leading to a poor observed/unique reflections ratio (22%). 
;
# end Validation Reply Form

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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
_audit_block_doi                 10.5517/cc133zbj
_database_code_depnum_ccdc_archive 'CCDC 1016717'
_audit_update_record             
;
2015-07-17 deposited with the CCDC.
2015-07-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 C69 H56 Cu N10 O7, 2(Cl O4), 2(C3 H7 N O), 4(H2 O)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C75 H78 Cl2 Cu N12 O21'
_chemical_formula_weight         1617.93

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'
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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.244(8)
_cell_length_b                   15.370(9)
_cell_length_c                   17.480(9)
_cell_angle_alpha                82.582(8)
_cell_angle_beta                 80.483(19)
_cell_angle_gamma                88.567(19)
_cell_volume                     4005(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    5554
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_F_000             1686
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.418
_shelx_estimated_absorpt_T_min   0.921
_shelx_estimated_absorpt_T_max   0.921
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
R. H. Blessing Acta Crystallogr., Sect. A, 1995, 51, 33-38
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32463
_diffrn_reflns_av_unetI/netI     0.1288
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.001
_diffrn_reflns_theta_max         26.247
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             15656
_reflns_number_gt                9138
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r14k (Rigaku, 2012)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r14k (Rigaku, 2012)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r14k (Rigaku, 2012)
;

_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Mercury 3.5'
_computing_publication_material  'Word 2010'

_refine_special_details          
;
 Diffuse, disordered solvent molecules could not be adequately modeled.  The
 bypass procedure in Platon (Spek, 1990) was used to remove the electronic
 contribution from these solvents. The total potential solvent accessible void
 volume was 462 Α³ and the electron count/cell = 91. Though the exact
 solvent content is not known, from the electron count and the TG experimental results
 it is assumed to be one DMF and three water molecules. But the reported formula reflects
 only the atoms used in the refinement.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1088P)²+5.7295P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15656
_refine_ls_number_parameters     1025
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1486
_refine_ls_R_factor_gt           0.0941
_refine_ls_wR_factor_ref         0.2587
_refine_ls_wR_factor_gt          0.2206
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000

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
H6A H 0.404(4) 0.837(4) 0.387(3) 0.029(16) Uiso 1 1 d . . . . .
H6B H 0.414(4) 0.805(4) 0.465(3) 0.032(16) Uiso 1 1 d . . . . .
C1 C 0.1283(6) 0.3118(7) 0.0935(5) 0.072(3) Uani 1 1 d . . . . .
H1 H 0.0761 0.3375 0.0770 0.087 Uiso 1 1 calc R U . . .
C2 C 0.1661(7) 0.2390(7) 0.0614(4) 0.077(3) Uani 1 1 d . . . . .
H2 H 0.1396 0.2156 0.0230 0.093 Uiso 1 1 calc R U . . .
C3 C 0.5738(5) 0.3622(4) 0.1175(4) 0.0519(18) Uani 1 1 d . . . . .
H3 H 0.6164 0.3165 0.1105 0.062 Uiso 1 1 calc R U . . .
C4 C 0.2875(7) 0.1244(5) 0.0531(4) 0.065(3) Uani 1 1 d . . . . .
H4 H 0.2648 0.0990 0.0136 0.079 Uiso 1 1 calc R U . . .
C5 C 0.3600(6) 0.0903(5) 0.0786(4) 0.059(2) Uani 1 1 d . . . . .
H5 H 0.3875 0.0406 0.0575 0.071 Uiso 1 1 calc R U . . .
C6 C 0.1671(5) 0.9653(4) 0.1939(4) 0.0466(17) Uani 1 1 d . . . . .
H6 H 0.1520 1.0113 0.1565 0.056 Uiso 1 1 calc R U . . .
C7 C 0.1602(4) 0.7027(4) 0.7618(3) 0.0385(14) Uani 1 1 d . . . . .
H7 H 0.1076 0.6853 0.7973 0.046 Uiso 1 1 calc R U . . .
C8 C -0.0322(5) 1.0196(4) 0.3394(4) 0.0498(18) Uani 1 1 d . . . . .
H8 H 0.0063 1.0449 0.2940 0.060 Uiso 1 1 calc R U . . .
C9 C 0.1656(5) 0.3473(5) 0.1492(4) 0.0530(19) Uani 1 1 d . . . . .
H9 H 0.1392 0.3977 0.1701 0.064 Uiso 1 1 calc R U . . .
C10 C 0.4982(5) 0.3156(4) 0.0146(4) 0.0525(19) Uani 1 1 d . . . . .
H10 H 0.5390 0.2688 0.0061 0.063 Uiso 1 1 calc R U . . .
C11 C 0.3968(5) 0.1258(4) 0.1356(3) 0.0494(18) Uani 1 1 d . . . . .
H11 H 0.4497 0.1012 0.1515 0.059 Uiso 1 1 calc R U . . .
C12 C 0.1417(4) 0.8817(4) 0.1895(4) 0.0420(15) Uani 1 1 d . . . . .
H12 H 0.1099 0.8680 0.1502 0.050 Uiso 1 1 calc R U . . .
C13 C 0.2422(5) 0.1998(5) 0.0844(4) 0.054(2) Uani 1 1 d . . . . .
C14 C 0.4305(5) 0.3295(4) -0.0279(4) 0.0520(19) Uani 1 1 d . . . . .
H14 H 0.4262 0.2922 -0.0664 0.062 Uiso 1 1 calc R U . . .
C15 C 0.5797(5) 0.4176(4) 0.1729(4) 0.0505(18) Uani 1 1 d . . . . .
H15 H 0.6264 0.4102 0.2030 0.061 Uiso 1 1 calc R U . . .
C16 C 0.5074(5) 0.3718(4) 0.0721(3) 0.0424(16) Uani 1 1 d . . . . .
C17 C 0.2401(4) 0.3110(4) 0.1746(3) 0.0356(14) Uani 1 1 d . . . . .
C18 C 0.3568(5) 0.1961(3) 0.1688(3) 0.0352(15) Uani 1 1 d . . . . .
C19 C 0.3667(5) 0.3968(4) -0.0172(4) 0.0427(16) Uani 1 1 d . . . . .
H19 H 0.3201 0.4038 -0.0475 0.051 Uiso 1 1 calc R U . . .
C20 C -0.3240(4) 0.9960(4) 0.5000(4) 0.0452(17) Uani 1 1 d . . . . .
H20 H -0.3852 1.0119 0.5083 0.054 Uiso 1 1 calc R U . . .
C21 C -0.2692(5) 1.0323(3) 0.4339(4) 0.0433(16) Uani 1 1 d . . . . .
H21 H -0.2929 1.0734 0.3972 0.052 Uiso 1 1 calc R U . . .
C22 C -0.1187(5) 1.0450(4) 0.3521(4) 0.0460(17) Uani 1 1 d . . . . .
H22 H -0.1402 1.0873 0.3150 0.055 Uiso 1 1 calc R U . . .
C23 C 0.0016(5) 0.9552(4) 0.3940(4) 0.0439(16) Uani 1 1 d . . . . .
H23 H 0.0620 0.9368 0.3841 0.053 Uiso 1 1 calc R U . . .
C24 C 0.3725(4) 0.4521(4) 0.0374(3) 0.0373(15) Uani 1 1 d . . . . .
C25 C 0.2119(4) 0.8348(3) 0.3039(3) 0.0301(13) Uani 1 1 d . . . . .
C26 C 0.2140(4) 0.9858(4) 0.2509(4) 0.0425(16) Uani 1 1 d . . . . .
H26 H 0.2309 1.0450 0.2507 0.051 Uiso 1 1 calc R U . . .
C27 C 0.2807(4) 0.2354(4) 0.1432(3) 0.0359(14) Uani 1 1 d . . . . .
C28 C 0.2461(4) 0.6457(4) 0.1228(4) 0.0388(15) Uani 1 1 d . . . . .
H28A H 0.2294 0.6733 0.0728 0.047 Uiso 1 1 calc R U . . .
H28B H 0.2708 0.6919 0.1477 0.047 Uiso 1 1 calc R U . . .
C29 C 0.4414(5) 0.4411(4) 0.0838(3) 0.0402(16) Uani 1 1 d . . . . .
C30 C 0.3077(4) 0.7702(4) 0.7321(3) 0.0375(14) Uani 1 1 d . . . . .
H30 H 0.3541 0.7983 0.7497 0.045 Uiso 1 1 calc R U . . .
C31 C 0.6305(4) 0.5976(4) 0.3463(3) 0.0369(14) Uani 1 1 d . . . . .
H31 H 0.6808 0.6330 0.3242 0.044 Uiso 1 1 calc R U . . .
C32 C 0.1028(4) 0.6749(4) 0.2145(3) 0.0350(14) Uani 1 1 d . . . . .
H32A H 0.0804 0.7152 0.1731 0.042 Uiso 1 1 calc R U . . .
H32B H 0.0509 0.6452 0.2486 0.042 Uiso 1 1 calc R U . . .
C33 C -0.2904(4) 0.9351(3) 0.5558(4) 0.0365(14) Uani 1 1 d . . . . .
H33 H -0.3287 0.9104 0.6014 0.044 Uiso 1 1 calc R U . . .
C34 C 0.3063(5) 0.5230(4) 0.0492(3) 0.0382(14) Uani 1 1 d . . . . .
C35 C 0.4479(4) 0.4964(4) 0.1411(3) 0.0355(14) Uani 1 1 d . . . . .
C36 C 0.5698(4) 0.4509(4) 0.3912(3) 0.0363(14) Uani 1 1 d . . . . .
H36 H 0.5771 0.3891 0.4007 0.044 Uiso 1 1 calc R U . . .
C37 C 0.3937(4) 0.2309(4) 0.2316(3) 0.0359(14) Uani 1 1 d . . . . .
C38 C -0.1676(4) 0.8483(3) 0.6029(3) 0.0278(12) Uani 1 1 d . . . . .
C39 C 0.3944(4) 0.3453(3) 0.3182(3) 0.0327(13) Uani 1 1 d . . . . .
H39A H 0.3962 0.4100 0.3061 0.039 Uiso 1 1 calc R U . . .
H39B H 0.4562 0.3240 0.3178 0.039 Uiso 1 1 calc R U . . .
C40 C 0.2365(4) 0.9234(4) 0.3071(4) 0.0359(14) Uani 1 1 d . . . . .
H40 H 0.2672 0.9380 0.3468 0.043 Uiso 1 1 calc R U . . .
C41 C 0.1852(4) 0.6018(3) 0.3622(3) 0.0295(13) Uani 1 1 d . . . . .
H41A H 0.2298 0.5664 0.3317 0.035 Uiso 1 1 calc R U . . .
H41B H 0.1258 0.5756 0.3655 0.035 Uiso 1 1 calc R U . . .
C42 C 0.5156(5) 0.4854(4) 0.1846(4) 0.0457(16) Uani 1 1 d . . . . .
H42 H 0.5197 0.5234 0.2226 0.055 Uiso 1 1 calc R U . . .
C43 C 0.5475(4) 0.6369(4) 0.3643(3) 0.0311(13) Uani 1 1 d . . . . .
H43 H 0.5404 0.6987 0.3556 0.037 Uiso 1 1 calc R U . . .
C44 C -0.0408(4) 0.7677(3) 0.6471(3) 0.0345(13) Uani 1 1 d . . . . .
H44A H -0.0754 0.7747 0.6991 0.041 Uiso 1 1 calc R U . . .
H44B H 0.0215 0.7845 0.6471 0.041 Uiso 1 1 calc R U . . .
C45 C 0.2485(4) 0.5192(3) 0.4704(3) 0.0282(12) Uani 1 1 d . . . . .
H45A H 0.2373 0.5087 0.5283 0.034 Uiso 1 1 calc R U . . .
H45B H 0.2226 0.4701 0.4502 0.034 Uiso 1 1 calc R U . . .
C46 C 0.6406(4) 0.5051(4) 0.3605(3) 0.0363(14) Uani 1 1 d . . . . .
H46 H 0.6980 0.4800 0.3485 0.044 Uiso 1 1 calc R U . . .
C47 C 0.4751(4) 0.5820(4) 0.3956(3) 0.0299(12) Uani 1 1 d . . . . .
C48 C 0.3459(4) 0.5251(3) 0.4410(3) 0.0249(12) Uani 1 1 d . . . . .
C49 C -0.0434(4) 0.6701(4) 0.6329(3) 0.0325(13) Uani 1 1 d . . . . .
H49A H -0.1029 0.6457 0.6555 0.039 Uiso 1 1 calc R U . . .
H49B H -0.0340 0.6668 0.5759 0.039 Uiso 1 1 calc R U . . .
C50 C 0.3410(4) 0.3208(3) 0.3996(3) 0.0292(12) Uani 1 1 d . . . . .
H50A H 0.2787 0.3409 0.3999 0.035 Uiso 1 1 calc R U . . .
H50B H 0.3405 0.2561 0.4127 0.035 Uiso 1 1 calc R U . . .
C51 C -0.0536(4) 0.9197(4) 0.4610(4) 0.0368(14) Uani 1 1 d . . . . .
C52 C -0.1773(5) 1.0098(4) 0.4193(3) 0.0368(14) Uani 1 1 d . . . . .
C53 C 0.2315(5) 0.7438(4) 0.7852(4) 0.0409(15) Uani 1 1 d . . . . .
H53 H 0.2275 0.7538 0.8382 0.049 Uiso 1 1 calc R U . . .
C54 C 0.1862(4) 0.6949(3) 0.3239(3) 0.0261(12) Uani 1 1 d . . . . .
C55 C -0.0183(4) 0.8555(4) 0.5187(3) 0.0365(14) Uani 1 1 d . . . . .
C56 C 0.3174(4) 0.7565(3) 0.6548(3) 0.0328(13) Uani 1 1 d . . . . .
H56 H 0.3697 0.7746 0.6193 0.039 Uiso 1 1 calc R U . . .
C57 C 0.1274(4) 0.6263(3) 0.4982(3) 0.0277(12) Uani 1 1 d . . . . .
H57A H 0.0923 0.6733 0.4729 0.033 Uiso 1 1 calc R U . . .
H57B H 0.0890 0.5741 0.5158 0.033 Uiso 1 1 calc R U . . .
C58 C 0.1718(4) 0.6891(3) 0.6835(3) 0.0299(12) Uani 1 1 d . . . . .
C59 C 0.0274(4) 0.6146(4) 0.6693(3) 0.0339(13) Uani 1 1 d . . . . .
H59A H 0.0143 0.6130 0.7269 0.041 Uiso 1 1 calc R U . . .
H59B H 0.0246 0.5537 0.6571 0.041 Uiso 1 1 calc R U . . .
C60 C -0.2012(4) 0.9114(3) 0.5438(3) 0.0288(12) Uani 1 1 d . . . . .
C61 C 0.2485(4) 0.7153(3) 0.6297(3) 0.0272(12) Uani 1 1 d . . . . .
C62 C 0.2811(4) 0.3496(4) 0.2338(3) 0.0331(13) Uani 1 1 d . . . . .
C63 C 0.1639(4) 0.6056(4) 0.1765(3) 0.0347(14) Uani 1 1 d . . . . .
H63A H 0.1831 0.5632 0.2181 0.042 Uiso 1 1 calc R U . . .
H63B H 0.1299 0.5731 0.1459 0.042 Uiso 1 1 calc R U . . .
C64 C 0.3777(4) 0.5633(4) 0.1573(3) 0.0346(14) Uani 1 1 d . . . . .
C65 C -0.1440(4) 0.9470(3) 0.4744(3) 0.0317(13) Uani 1 1 d . . . . .
C66 C 0.4871(4) 0.4902(3) 0.4079(3) 0.0277(12) Uani 1 1 d . . . . .
C67 C 0.1605(4) 0.6562(3) 0.5657(3) 0.0250(12) Uani 1 1 d . . . . .
C68 C 0.1657(4) 0.8176(4) 0.2468(3) 0.0303(13) Uani 1 1 d . . . . .
C69 C 0.3801(4) 0.3619(3) 0.4607(3) 0.0303(13) Uani 1 1 d . . . . .
H69A H 0.3369 0.3558 0.5100 0.036 Uiso 1 1 calc R U . . .
H69B H 0.4345 0.3290 0.4710 0.036 Uiso 1 1 calc R U . . .
N2 N 0.2071(3) 0.6041(3) 0.4426(3) 0.0265(10) Uani 1 1 d . . . . .
N3 N 0.2408(3) 0.6944(3) 0.5560(3) 0.0266(10) Uani 1 1 d . . . . .
N4 N 0.2262(3) 0.7571(3) 0.3516(2) 0.0270(10) Uani 1 1 d . . . . .
N5 N 0.3853(3) 0.6019(3) 0.4173(3) 0.0277(10) Uani 1 1 d . . . . .
N70 N 0.1491(3) 0.7257(3) 0.2609(2) 0.0255(10) Uani 1 1 d . . . . .
N72 N 0.3154(3) 0.5763(3) 0.1069(3) 0.0378(12) Uani 1 1 d . . . . .
N78 N -0.0773(3) 0.8264(3) 0.5870(3) 0.0304(11) Uani 1 1 d . . . . .
N81 N 0.3563(3) 0.3080(3) 0.2569(2) 0.0276(10) Uani 1 1 d . . . . .
N82 N 0.1186(3) 0.6493(3) 0.6404(3) 0.0268(10) Uani 1 1 d . . . . .
N83 N 0.4031(3) 0.4565(3) 0.4380(3) 0.0291(10) Uani 1 1 d . . . . .
O6 O 0.3770(3) 0.8029(3) 0.4301(3) 0.0370(10) Uani 1 1 d . . . . .
O71 O 0.3746(3) 0.6063(3) 0.2125(3) 0.0472(11) Uani 1 1 d . . . . .
O73 O 0.0581(3) 0.8268(3) 0.5077(3) 0.0447(11) Uani 1 1 d . . . . .
O74 O 0.2463(3) 0.5374(3) 0.0110(2) 0.0493(12) Uani 1 1 d . . . . .
O80 O 0.4550(3) 0.1952(3) 0.2611(2) 0.0446(11) Uani 1 1 d . . . . .
O84 O 0.2513(3) 0.4154(2) 0.2622(2) 0.0412(11) Uani 1 1 d . . . . .
O85 O -0.2129(3) 0.8182(2) 0.6643(2) 0.0361(9) Uani 1 1 d . . . . .
Cu1 Cu 0.29621(4) 0.70593(4) 0.43645(4) 0.0265(2) Uani 1 1 d . . . . .
C101 C 0.5367(6) 0.9019(5) 0.1147(4) 0.063(2) Uani 1 1 d . . . . .
H10A H 0.5599 0.9617 0.1078 0.095 Uiso 1 1 calc R U . . .
H10B H 0.4979 0.8969 0.0761 0.095 Uiso 1 1 calc R U . . .
H10C H 0.5863 0.8603 0.1074 0.095 Uiso 1 1 calc R U . . .
C102 C 0.4374(5) 0.7999(5) 0.2096(4) 0.059(2) Uani 1 1 d . . . . .
H10D H 0.3986 0.7978 0.2605 0.088 Uiso 1 1 calc R U . . .
H10E H 0.4794 0.7506 0.2108 0.088 Uiso 1 1 calc R U . . .
H10F H 0.4012 0.7960 0.1688 0.088 Uiso 1 1 calc R U . . .
C104 C 0.4889(4) 0.9358(4) 0.2468(3) 0.0386(15) Uani 1 1 d . . . . .
H104 H 0.5229 0.9878 0.2308 0.046 Uiso 1 1 calc R U . . .
N106 N 0.4863(4) 0.8819(3) 0.1931(3) 0.0444(14) Uani 1 1 d . . . . .
O108 O 0.4514(3) 0.9241(3) 0.3150(2) 0.0456(11) Uani 1 1 d . . . . .
C115 C 0.2716(9) 0.0604(15) 0.7645(9) 0.225(11) Uani 1 1 d . . . . .
H11A H 0.3261 0.0320 0.7413 0.337 Uiso 1 1 calc R U . . .
H11B H 0.2238 0.0170 0.7794 0.337 Uiso 1 1 calc R U . . .
H11C H 0.2823 0.0853 0.8110 0.337 Uiso 1 1 calc R U . . .
C116 C 0.1467(9) 0.1489(8) 0.7266(7) 0.124(5) Uani 1 1 d . . . . .
H11D H 0.1234 0.1199 0.7791 0.186 Uiso 1 1 calc R U . . .
H11E H 0.1160 0.1263 0.6883 0.186 Uiso 1 1 calc R U . . .
H11F H 0.1368 0.2123 0.7248 0.186 Uiso 1 1 calc R U . . .
C117 C 0.2933(13) 0.1581(9) 0.6441(6) 0.159(8) Uani 1 1 d . . . . .
H117 H 0.2553 0.1800 0.6081 0.191 Uiso 1 1 calc R U . . .
N119 N 0.2457(7) 0.1304(7) 0.7075(5) 0.103(3) Uani 1 1 d . . . . .
O119 O 0.3602(5) 0.1665(6) 0.6152(6) 0.139(4) Uani 1 1 d . . . . .
O103 O 0.1318(4) 0.3860(4) 0.6519(4) 0.0861(19) Uani 1 1 d . . . . .
O105 O 0.1596(4) 0.3216(3) 0.5387(3) 0.0714(16) Uani 1 1 d . . . . .
O107 O 0.0495(4) 0.4295(3) 0.5547(4) 0.0785(18) Uani 1 1 d . . . . .
O109 O 0.0277(3) 0.2899(3) 0.6240(3) 0.0625(14) Uani 1 1 d . . . . .
Cl90 Cl 0.09239(10) 0.35663(10) 0.59320(9) 0.0395(4) Uani 1 1 d . . . . .
O9 O 0.3747(5) 0.8845(4) 1.0044(4) 0.109(3) Uani 1 1 d . . . . .
O11 O 0.2724(4) 0.7978(3) 0.9630(3) 0.0769(18) Uani 1 1 d . . . . .
O13 O 0.3628(5) 0.8917(5) 0.8727(3) 0.105(3) Uani 1 1 d . . . . .
O17 O 0.2551(5) 0.9506(4) 0.9592(4) 0.097(2) Uani 1 1 d . . . . .
Cl91 Cl 0.31461(13) 0.88147(11) 0.95124(10) 0.0510(4) Uani 1 1 d . . . . .
H11G H 0.515(6) 0.108(6) 0.339(5) 0.07(3) Uiso 1 1 d . . . . .
H11H H 0.510(5) 0.027(5) 0.366(4) 0.04(2) Uiso 1 1 d . . . . .
O110 O 0.5188(4) 0.0726(4) 0.3733(3) 0.0467(13) Uani 1 1 d . . . . .
O111 O 0.5057(3) 0.8225(3) 0.5078(3) 0.0466(11) Uani 1 1 d G . . . .
H11I H 0.5376 0.8491 0.4658 0.070 Uiso 1 1 d G U . . .
H11J H 0.5066 0.8526 0.5465 0.070 Uiso 1 1 d G U . . .
O118 O 0.0916(7) 0.6240(8) 0.9762(7) 0.148(4) Uani 1 1 d G . . . .
H11K H 0.0783 0.6762 0.9889 0.222 Uiso 1 1 d G U . . .
H11L H 0.1288 0.5991 1.0051 0.222 Uiso 1 1 d G U . . .
O130 O 0.9842(8) 0.4776(9) 0.1148(6) 0.199(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C9 1.381(11) . ?
C1 C2 1.387(13) . ?
C1 H1 0.9500 . ?
C2 C13 1.389(12) . ?
C2 H2 0.9500 . ?
C3 C16 1.379(10) . ?
C3 C15 1.385(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.330(12) . ?
C4 C13 1.456(11) . ?
C4 H4 0.9500 . ?
C5 C11 1.393(10) . ?
C5 H5 0.9500 . ?
C6 C12 1.367(9) . ?
C6 C26 1.391(9) . ?
C6 H6 0.9500 . ?
C7 C58 1.393(8) . ?
C7 C53 1.414(9) . ?
C7 H7 0.9500 . ?
C8 C22 1.357(10) . ?
C8 C23 1.432(10) . ?
C8 H8 0.9500 . ?
C9 C17 1.368(9) . ?
C9 H9 0.9500 . ?
C10 C14 1.364(10) . ?
C10 C16 1.433(9) . ?
C10 H10 0.9500 . ?
C11 C18 1.375(9) . ?
C11 H11 0.9500 . ?
C12 C68 1.398(8) . ?
C12 H12 0.9500 . ?
C13 C27 1.435(9) . ?
C14 C19 1.412(9) . ?
C14 H14 0.9500 . ?
C15 C42 1.422(9) . ?
C15 H15 0.9500 . ?
C16 C29 1.457(9) . ?
C17 C27 1.432(9) . ?
C17 C62 1.484(8) . ?
C18 C27 1.407(9) . ?
C18 C37 1.474(8) . ?
C19 C24 1.372(8) . ?
C19 H19 0.9500 . ?
C20 C21 1.372(9) . ?
C20 C33 1.413(9) . ?
C20 H20 0.9500 . ?
C21 C52 1.424(9) . ?
C21 H21 0.9500 . ?
C22 C52 1.408(9) . ?
C22 H22 0.9500 . ?
C23 C51 1.382(8) . ?
C23 H23 0.9500 . ?
C24 C29 1.424(9) . ?
C24 C34 1.478(9) . ?
C25 C68 1.368(8) . ?
C25 N4 1.399(7) . ?
C25 C40 1.433(7) . ?
C26 C40 1.362(8) . ?
C26 H26 0.9500 . ?
C28 N72 1.501(8) . ?
C28 C63 1.527(8) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C35 1.410(9) . ?
C30 C56 1.378(8) . ?
C30 C53 1.395(9) . ?
C30 H30 0.9500 . ?
C31 C43 1.393(8) . ?
C31 C46 1.421(8) . ?
C31 H31 0.9500 . ?
C32 N70 1.466(7) . ?
C32 C63 1.540(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C60 1.387(8) . ?
C33 H33 0.9500 . ?
C34 O74 1.218(8) . ?
C34 N72 1.405(8) . ?
C35 C42 1.375(9) . ?
C35 C64 1.484(8) . ?
C36 C46 1.373(8) . ?
C36 C66 1.388(8) . ?
C36 H36 0.9500 . ?
C37 O80 1.225(7) . ?
C37 N81 1.394(7) . ?
C38 O85 1.220(6) . ?
C38 N78 1.400(7) . ?
C38 C60 1.470(8) . ?
C39 N81 1.482(7) . ?
C39 C50 1.523(8) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40 0.9500 . ?
C41 C54 1.499(7) . ?
C41 N2 1.503(7) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42 0.9500 . ?
C43 C47 1.399(8) . ?
C43 H43 0.9500 . ?
C44 N78 1.467(7) . ?
C44 C49 1.556(7) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C48 1.491(8) . ?
C45 N2 1.494(7) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46 0.9500 . ?
C47 N5 1.397(7) . ?
C47 C66 1.411(7) . ?
C48 N5 1.324(6) . ?
C48 N83 1.352(7) . ?
C49 C59 1.529(8) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C69 1.518(8) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C65 1.420(8) . ?
C51 C55 1.476(8) . ?
C52 C65 1.418(8) . ?
C53 H53 0.9500 . ?
C54 N4 1.329(6) . ?
C54 N70 1.348(7) . ?
C55 O73 1.228(7) . ?
C55 N78 1.401(7) . ?
C56 C61 1.397(8) . ?
C56 H56 0.9500 . ?
C57 C67 1.484(7) . ?
C57 N2 1.488(7) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 N82 1.394(7) . ?
C58 C61 1.406(8) . ?
C59 N82 1.487(7) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 C65 1.426(8) . ?
C61 N3 1.390(7) . ?
C62 O84 1.229(7) . ?
C62 N81 1.391(8) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 O71 1.232(7) . ?
C64 N72 1.392(8) . ?
C66 N83 1.387(7) . ?
C67 N3 1.347(7) . ?
C67 N82 1.348(6) . ?
C68 N70 1.423(7) . ?
C69 N83 1.491(6) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
N2 Cu1 2.078(4) . ?
N3 Cu1 2.107(5) . ?
N4 Cu1 2.034(4) . ?
N5 Cu1 2.095(5) . ?
O6 Cu1 1.937(4) . ?
O6 H6A 0.90(6) . ?
O6 H6B 0.90(6) . ?
C101 N106 1.455(8) . ?
C101 H10A 0.9800 . ?
C101 H10B 0.9800 . ?
C101 H10C 0.9800 . ?
C102 N106 1.453(8) . ?
C102 H10D 0.9800 . ?
C102 H10E 0.9800 . ?
C102 H10F 0.9800 . ?
C104 O108 1.226(7) . ?
C104 N106 1.336(8) . ?
C104 H104 0.9500 . ?
C115 N119 1.463(16) . ?
C115 H11A 0.9800 . ?
C115 H11B 0.9800 . ?
C115 H11C 0.9800 . ?
C116 N119 1.518(14) . ?
C116 H11D 0.9800 . ?
C116 H11E 0.9800 . ?
C116 H11F 0.9800 . ?
C117 O119 1.064(17) . ?
C117 N119 1.251(13) . ?
C117 H117 0.9500 . ?
O103 Cl90 1.398(5) . ?
O105 Cl90 1.424(5) . ?
O107 Cl90 1.431(5) . ?
O109 Cl90 1.430(4) . ?
O9 Cl91 1.414(6) . ?
O11 Cl91 1.428(5) . ?
O13 Cl91 1.438(6) . ?
O17 Cl91 1.386(6) . ?
O110 H11G 0.76(9) . ?
O110 H11H 0.75(7) . ?
O111 H11I 0.8702 . ?
O111 H11J 0.8700 . ?
O118 H11K 0.8699 . ?
O118 H11L 0.8699 . ?

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
C9 C1 C2 120.7(8) . . ?
C9 C1 H1 119.6 . . ?
C2 C1 H1 119.6 . . ?
C1 C2 C13 121.0(7) . . ?
C1 C2 H2 119.5 . . ?
C13 C2 H2 119.5 . . ?
C16 C3 C15 121.5(7) . . ?
C16 C3 H3 119.3 . . ?
C15 C3 H3 119.3 . . ?
C5 C4 C13 121.2(7) . . ?
C5 C4 H4 119.4 . . ?
C13 C4 H4 119.4 . . ?
C4 C5 C11 121.7(7) . . ?
C4 C5 H5 119.1 . . ?
C11 C5 H5 119.1 . . ?
C12 C6 C26 122.6(6) . . ?
C12 C6 H6 118.7 . . ?
C26 C6 H6 118.7 . . ?
C58 C7 C53 115.9(6) . . ?
C58 C7 H7 122.1 . . ?
C53 C7 H7 122.1 . . ?
C22 C8 C23 120.5(6) . . ?
C22 C8 H8 119.8 . . ?
C23 C8 H8 119.8 . . ?
C17 C9 C1 120.8(8) . . ?
C17 C9 H9 119.6 . . ?
C1 C9 H9 119.6 . . ?
C14 C10 C16 119.8(7) . . ?
C14 C10 H10 120.1 . . ?
C16 C10 H10 120.1 . . ?
C18 C11 C5 120.3(8) . . ?
C18 C11 H11 119.9 . . ?
C5 C11 H11 119.9 . . ?
C6 C12 C68 115.5(6) . . ?
C6 C12 H12 122.3 . . ?
C68 C12 H12 122.3 . . ?
C2 C13 C27 118.7(8) . . ?
C2 C13 C4 124.9(8) . . ?
C27 C13 C4 116.4(8) . . ?
C10 C14 C19 122.9(7) . . ?
C10 C14 H14 118.5 . . ?
C19 C14 H14 118.5 . . ?
C3 C15 C42 119.8(7) . . ?
C3 C15 H15 120.1 . . ?
C42 C15 H15 120.1 . . ?
C3 C16 C10 123.5(7) . . ?
C3 C16 C29 119.0(6) . . ?
C10 C16 C29 117.5(7) . . ?
C9 C17 C27 120.0(6) . . ?
C9 C17 C62 121.1(6) . . ?
C27 C17 C62 118.9(6) . . ?
C11 C18 C27 120.3(6) . . ?
C11 C18 C37 120.1(6) . . ?
C27 C18 C37 119.6(5) . . ?
C24 C19 C14 119.4(7) . . ?
C24 C19 H19 120.3 . . ?
C14 C19 H19 120.3 . . ?
C21 C20 C33 120.5(6) . . ?
C21 C20 H20 119.7 . . ?
C33 C20 H20 119.7 . . ?
C20 C21 C52 121.3(6) . . ?
C20 C21 H21 119.3 . . ?
C52 C21 H21 119.3 . . ?
C8 C22 C52 121.2(6) . . ?
C8 C22 H22 119.4 . . ?
C52 C22 H22 119.4 . . ?
C51 C23 C8 119.9(7) . . ?
C51 C23 H23 120.1 . . ?
C8 C23 H23 120.1 . . ?
C19 C24 C29 120.5(6) . . ?
C19 C24 C34 120.0(6) . . ?
C29 C24 C34 119.5(5) . . ?
C68 C25 N4 110.1(4) . . ?
C68 C25 C40 119.1(5) . . ?
N4 C25 C40 130.7(5) . . ?
C40 C26 C6 121.8(5) . . ?
C40 C26 H26 119.1 . . ?
C6 C26 H26 119.1 . . ?
C18 C27 C17 121.3(5) . . ?
C18 C27 C13 120.0(6) . . ?
C17 C27 C13 118.7(6) . . ?
N72 C28 C63 110.3(4) . . ?
N72 C28 H28A 109.6 . . ?
C63 C28 H28A 109.6 . . ?
N72 C28 H28B 109.6 . . ?
C63 C28 H28B 109.6 . . ?
H28A C28 H28B 108.1 . . ?
C35 C29 C24 121.4(6) . . ?
C35 C29 C16 118.8(6) . . ?
C24 C29 C16 119.8(6) . . ?
C56 C30 C53 121.6(6) . . ?
C56 C30 H30 119.2 . . ?
C53 C30 H30 119.2 . . ?
C43 C31 C46 120.7(6) . . ?
C43 C31 H31 119.7 . . ?
C46 C31 H31 119.7 . . ?
N70 C32 C63 111.9(5) . . ?
N70 C32 H32A 109.2 . . ?
C63 C32 H32A 109.2 . . ?
N70 C32 H32B 109.2 . . ?
C63 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
C60 C33 C20 119.9(6) . . ?
C60 C33 H33 120.0 . . ?
C20 C33 H33 120.0 . . ?
O74 C34 N72 119.7(6) . . ?
O74 C34 C24 123.3(6) . . ?
N72 C34 C24 117.0(6) . . ?
C42 C35 C29 120.5(6) . . ?
C42 C35 C64 120.1(6) . . ?
C29 C35 C64 119.3(6) . . ?
C46 C36 C66 117.2(5) . . ?
C46 C36 H36 121.4 . . ?
C66 C36 H36 121.4 . . ?
O80 C37 N81 119.9(5) . . ?
O80 C37 C18 122.8(5) . . ?
N81 C37 C18 117.3(6) . . ?
O85 C38 N78 120.1(5) . . ?
O85 C38 C60 123.6(6) . . ?
N78 C38 C60 116.2(5) . . ?
N81 C39 C50 112.5(4) . . ?
N81 C39 H39A 109.1 . . ?
C50 C39 H39A 109.1 . . ?
N81 C39 H39B 109.1 . . ?
C50 C39 H39B 109.1 . . ?
H39A C39 H39B 107.8 . . ?
C26 C40 C25 117.1(6) . . ?
C26 C40 H40 121.4 . . ?
C25 C40 H40 121.4 . . ?
C54 C41 N2 106.7(4) . . ?
C54 C41 H41A 110.4 . . ?
N2 C41 H41A 110.4 . . ?
C54 C41 H41B 110.4 . . ?
N2 C41 H41B 110.4 . . ?
H41A C41 H41B 108.6 . . ?
C35 C42 C15 120.3(6) . . ?
C35 C42 H42 119.8 . . ?
C15 C42 H42 119.8 . . ?
C31 C43 C47 117.6(5) . . ?
C31 C43 H43 121.2 . . ?
C47 C43 H43 121.2 . . ?
N78 C44 C49 111.8(5) . . ?
N78 C44 H44A 109.3 . . ?
C49 C44 H44A 109.3 . . ?
N78 C44 H44B 109.3 . . ?
C49 C44 H44B 109.3 . . ?
H44A C44 H44B 107.9 . . ?
C48 C45 N2 107.7(4) . . ?
C48 C45 H45A 110.2 . . ?
N2 C45 H45A 110.2 . . ?
C48 C45 H45B 110.2 . . ?
N2 C45 H45B 110.2 . . ?
H45A C45 H45B 108.5 . . ?
C36 C46 C31 121.9(6) . . ?
C36 C46 H46 119.1 . . ?
C31 C46 H46 119.1 . . ?
N5 C47 C43 130.4(5) . . ?
N5 C47 C66 109.2(5) . . ?
C43 C47 C66 120.3(5) . . ?
N5 C48 N83 113.3(5) . . ?
N5 C48 C45 121.1(5) . . ?
N83 C48 C45 125.5(5) . . ?
C59 C49 C44 112.1(5) . . ?
C59 C49 H49A 109.2 . . ?
C44 C49 H49A 109.2 . . ?
C59 C49 H49B 109.2 . . ?
C44 C49 H49B 109.2 . . ?
H49A C49 H49B 107.9 . . ?
C69 C50 C39 111.2(4) . . ?
C69 C50 H50A 109.4 . . ?
C39 C50 H50A 109.4 . . ?
C69 C50 H50B 109.4 . . ?
C39 C50 H50B 109.4 . . ?
H50A C50 H50B 108.0 . . ?
C23 C51 C65 119.4(6) . . ?
C23 C51 C55 120.1(6) . . ?
C65 C51 C55 120.5(5) . . ?
C22 C52 C65 118.7(6) . . ?
C22 C52 C21 123.2(6) . . ?
C65 C52 C21 118.1(6) . . ?
C30 C53 C7 121.4(6) . . ?
C30 C53 H53 119.3 . . ?
C7 C53 H53 119.3 . . ?
N4 C54 N70 112.8(4) . . ?
N4 C54 C41 120.7(5) . . ?
N70 C54 C41 126.5(5) . . ?
O73 C55 N78 120.8(5) . . ?
O73 C55 C51 122.7(6) . . ?
N78 C55 C51 116.5(6) . . ?
C30 C56 C61 118.6(6) . . ?
C30 C56 H56 120.7 . . ?
C61 C56 H56 120.7 . . ?
C67 C57 N2 106.7(4) . . ?
C67 C57 H57A 110.4 . . ?
N2 C57 H57A 110.4 . . ?
C67 C57 H57B 110.4 . . ?
N2 C57 H57B 110.4 . . ?
H57A C57 H57B 108.6 . . ?
C7 C58 N82 132.3(5) . . ?
C7 C58 C61 123.0(5) . . ?
N82 C58 C61 104.7(5) . . ?
N82 C59 C49 112.3(4) . . ?
N82 C59 H59A 109.1 . . ?
C49 C59 H59A 109.1 . . ?
N82 C59 H59B 109.1 . . ?
C49 C59 H59B 109.1 . . ?
H59A C59 H59B 107.9 . . ?
C33 C60 C65 120.1(5) . . ?
C33 C60 C38 118.9(5) . . ?
C65 C60 C38 121.0(5) . . ?
N3 C61 C56 130.3(5) . . ?
N3 C61 C58 110.2(5) . . ?
C56 C61 C58 119.5(5) . . ?
O84 C62 N81 120.1(5) . . ?
O84 C62 C17 122.7(6) . . ?
N81 C62 C17 117.2(5) . . ?
C28 C63 C32 112.8(5) . . ?
C28 C63 H63A 109.0 . . ?
C32 C63 H63A 109.0 . . ?
C28 C63 H63B 109.0 . . ?
C32 C63 H63B 109.0 . . ?
H63A C63 H63B 107.8 . . ?
O71 C64 N72 121.0(6) . . ?
O71 C64 C35 121.8(6) . . ?
N72 C64 C35 117.2(5) . . ?
C52 C65 C51 120.3(6) . . ?
C52 C65 C60 120.0(6) . . ?
C51 C65 C60 119.8(5) . . ?
N83 C66 C36 132.5(5) . . ?
N83 C66 C47 105.2(5) . . ?
C36 C66 C47 122.2(5) . . ?
N3 C67 N82 112.4(4) . . ?
N3 C67 C57 120.5(5) . . ?
N82 C67 C57 127.1(5) . . ?
C25 C68 C12 123.8(5) . . ?
C25 C68 N70 105.5(5) . . ?
C12 C68 N70 130.7(5) . . ?
N83 C69 C50 114.0(4) . . ?
N83 C69 H69A 108.8 . . ?
C50 C69 H69A 108.8 . . ?
N83 C69 H69B 108.8 . . ?
C50 C69 H69B 108.8 . . ?
H69A C69 H69B 107.6 . . ?
C57 N2 C45 111.9(4) . . ?
C57 N2 C41 111.3(4) . . ?
C45 N2 C41 110.2(4) . . ?
C57 N2 Cu1 105.5(3) . . ?
C45 N2 Cu1 109.6(3) . . ?
C41 N2 Cu1 108.0(3) . . ?
C67 N3 C61 104.7(4) . . ?
C67 N3 Cu1 108.5(3) . . ?
C61 N3 Cu1 146.6(4) . . ?
C54 N4 C25 105.2(4) . . ?
C54 N4 Cu1 111.7(3) . . ?
C25 N4 Cu1 142.6(4) . . ?
C48 N5 C47 105.0(4) . . ?
C48 N5 Cu1 111.4(4) . . ?
C47 N5 Cu1 143.2(4) . . ?
C54 N70 C68 106.4(4) . . ?
C54 N70 C32 127.1(4) . . ?
C68 N70 C32 126.5(5) . . ?
C64 N72 C34 124.9(5) . . ?
C64 N72 C28 116.7(5) . . ?
C34 N72 C28 117.9(5) . . ?
C38 N78 C55 125.9(5) . . ?
C38 N78 C44 117.4(5) . . ?
C55 N78 C44 116.7(5) . . ?
C62 N81 C37 125.2(5) . . ?
C62 N81 C39 116.5(5) . . ?
C37 N81 C39 118.0(5) . . ?
C67 N82 C58 107.9(4) . . ?
C67 N82 C59 125.6(4) . . ?
C58 N82 C59 126.2(5) . . ?
C48 N83 C66 107.2(4) . . ?
C48 N83 C69 126.5(5) . . ?
C66 N83 C69 126.2(5) . . ?
Cu1 O6 H6A 128(3) . . ?
Cu1 O6 H6B 122(4) . . ?
H6A O6 H6B 104(5) . . ?
O6 Cu1 N4 98.35(18) . . ?
O6 Cu1 N2 178.59(19) . . ?
N4 Cu1 N2 80.48(17) . . ?
O6 Cu1 N5 101.45(18) . . ?
N4 Cu1 N5 120.19(18) . . ?
N2 Cu1 N5 79.85(18) . . ?
O6 Cu1 N3 100.25(18) . . ?
N4 Cu1 N3 121.89(18) . . ?
N2 Cu1 N3 79.76(17) . . ?
N5 Cu1 N3 109.08(17) . . ?
N106 C101 H10A 109.5 . . ?
N106 C101 H10B 109.5 . . ?
H10A C101 H10B 109.5 . . ?
N106 C101 H10C 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
N106 C102 H10D 109.5 . . ?
N106 C102 H10E 109.5 . . ?
H10D C102 H10E 109.5 . . ?
N106 C102 H10F 109.5 . . ?
H10D C102 H10F 109.5 . . ?
H10E C102 H10F 109.5 . . ?
O108 C104 N106 125.9(6) . . ?
O108 C104 H104 117.1 . . ?
N106 C104 H104 117.1 . . ?
C104 N106 C102 122.9(5) . . ?
C104 N106 C101 120.5(5) . . ?
C102 N106 C101 116.6(5) . . ?
N119 C115 H11A 109.5 . . ?
N119 C115 H11B 109.5 . . ?
H11A C115 H11B 109.5 . . ?
N119 C115 H11C 109.5 . . ?
H11A C115 H11C 109.5 . . ?
H11B C115 H11C 109.5 . . ?
N119 C116 H11D 109.5 . . ?
N119 C116 H11E 109.5 . . ?
H11D C116 H11E 109.5 . . ?
N119 C116 H11F 109.5 . . ?
H11D C116 H11F 109.5 . . ?
H11E C116 H11F 109.5 . . ?
O119 C117 N119 143.9(19) . . ?
O119 C117 H117 108.0 . . ?
N119 C117 H117 108.0 . . ?
C117 N119 C115 124.4(14) . . ?
C117 N119 C116 124.0(13) . . ?
C115 N119 C116 110.1(9) . . ?
O103 Cl90 O105 109.0(4) . . ?
O103 Cl90 O109 111.9(4) . . ?
O105 Cl90 O109 108.6(3) . . ?
O103 Cl90 O107 108.6(4) . . ?
O105 Cl90 O107 109.9(4) . . ?
O109 Cl90 O107 108.8(3) . . ?
O17 Cl91 O9 108.5(4) . . ?
O17 Cl91 O11 113.4(4) . . ?
O9 Cl91 O11 110.5(4) . . ?
O17 Cl91 O13 108.6(5) . . ?
O9 Cl91 O13 109.4(5) . . ?
O11 Cl91 O13 106.4(3) . . ?
H11G O110 H11H 115(8) . . ?
H11I O111 H11J 109.5 . . ?
H11K O118 H11L 109.5 . . ?

_refine_diff_density_max         1.224
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.092

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 462 91 ' '
_platon_squeeze_details          
;
 Diffuse, disordered solvent molecules could not be adequately modeled.  The
 bypass procedure in Platon (Spek, 1990) was used to remove the electronic
 contribution from these solvents. The total potential solvent accessible void
 volume was 462 Α³ and the electron count/cell = 91. Though the exact
 solvent content is not known, from the electron count and the TG experimental results
 it is assumed to be one DMF and three water molecules. But the reported formula reflects
 only the atoms used in the refinement.
;


_shelxl_version_number           2013-4

