# 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_abdulm03
_database_code_depnum_ccdc_archive 'CCDC 1035427'
_audit_update_record             
;
2014-11-21 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H36 N), C12 H10 N4 Ni O4'
_chemical_formula_sum            'C44 H82 N6 Ni O4'
_chemical_formula_weight         817.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7113(7)
_cell_length_b                   14.3928(7)
_cell_length_c                   15.4664(8)
_cell_angle_alpha                99.599(4)
_cell_angle_beta                 90.861(5)
_cell_angle_gamma                102.525(5)
_cell_volume                     2291.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    7179
_cell_measurement_theta_min      3.9265
_cell_measurement_theta_max      61.9984


_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_min  0.85378
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2879
_diffrn_standards_number         2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  10
_diffrn_standards_decay_%        0

_diffrn_reflns_number            12993
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.92
_diffrn_reflns_theta_max         62.00
_reflns_number_total             7077
_reflns_number_gt                5629
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
;

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2sigma(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.
 A short distance between two methyl groups (C11 and C12) is alerted. 
 The hydrogen atoms were here added on calculated positions as idealised
 methyl groups in staggered geometrie (HFIX 33). The comparatively close
 vicinity of C11 and C12 is thus regarded as responsible for this
 artefact. 
;

_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)+(0.0984P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7077
_refine_ls_number_parameters     496
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1360
_refine_ls_wR_factor_gt          0.1301
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2773(2) 0.11600(16) 0.16203(15) 0.0252(5) Uani 1 1 d . . .
C2 C 0.3448(2) 0.18309(17) 0.10139(15) 0.0259(5) Uani 1 1 d . . .
C3 C 0.0176(2) 0.35044(16) 0.30521(16) 0.0266(5) Uani 1 1 d . . .
C4 C 0.0720(2) 0.43066(17) 0.25250(16) 0.0290(5) Uani 1 1 d . . .
C5 C 0.1224(2) 0.12376(16) 0.27649(15) 0.0239(5) Uani 1 1 d . . .
C6 C 0.1115(2) 0.03422(17) 0.30250(16) 0.0279(5) Uani 1 1 d . . .
H6 H 0.1583 -0.0091 0.2761 0.033 Uiso 1 1 calc R . .
C7 C 0.0301(2) 0.01058(18) 0.36818(16) 0.0321(6) Uani 1 1 d . . .
H7 H 0.0226 -0.0490 0.3857 0.039 Uiso 1 1 calc R . .
C8 C -0.0403(2) 0.07468(18) 0.40815(16) 0.0304(5) Uani 1 1 d . . .
H8 H -0.0946 0.0575 0.4520 0.037 Uiso 1 1 calc R . .
C9 C -0.0302(2) 0.16429(17) 0.38317(15) 0.0276(5) Uani 1 1 d . . .
H9 H -0.0776 0.2069 0.4101 0.033 Uiso 1 1 calc R . .
C10 C 0.0511(2) 0.18985(16) 0.31767(15) 0.0236(5) Uani 1 1 d . . .
C11 C 0.3492(2) 0.32183(19) 0.03887(17) 0.0341(6) Uani 1 1 d . . .
H11A H 0.3125 0.3777 0.0460 0.051 Uiso 1 1 calc R . .
H11B H 0.3260 0.2847 -0.0189 0.051 Uiso 1 1 calc R . .
H11C H 0.4408 0.3420 0.0464 0.051 Uiso 1 1 calc R . .
C12 C 0.2242(3) 0.48644(18) 0.15375(18) 0.0339(6) Uani 1 1 d . . .
H12A H 0.2870 0.4642 0.1169 0.051 Uiso 1 1 calc R . .
H12B H 0.2655 0.5417 0.1961 0.051 Uiso 1 1 calc R . .
H12C H 0.1617 0.5040 0.1183 0.051 Uiso 1 1 calc R . .
C13 C -0.4102(2) -0.00678(16) 0.12269(15) 0.0246(5) Uani 1 1 d . . .
H13A H -0.4828 0.0236 0.1257 0.029 Uiso 1 1 calc R . .
H13B H -0.4073 -0.0382 0.0624 0.029 Uiso 1 1 calc R . .
C14 C -0.4324(2) -0.08358(17) 0.18065(16) 0.0301(5) Uani 1 1 d . . .
H14A H -0.4415 -0.0540 0.2407 0.036 Uiso 1 1 calc R . .
H14B H -0.3594 -0.1134 0.1799 0.036 Uiso 1 1 calc R . .
C15 C -0.5533(2) -0.16031(17) 0.14755(16) 0.0288(5) Uani 1 1 d . . .
H15A H -0.6277 -0.1333 0.1608 0.035 Uiso 1 1 calc R . .
H15B H -0.5528 -0.1780 0.0843 0.035 Uiso 1 1 calc R . .
C16 C -0.5644(3) -0.25056(18) 0.18864(18) 0.0368(6) Uani 1 1 d . . .
H16A H -0.6415 -0.2966 0.1659 0.055 Uiso 1 1 calc R . .
H16B H -0.5668 -0.2337 0.2512 0.055 Uiso 1 1 calc R . .
H16C H -0.4918 -0.2784 0.1747 0.055 Uiso 1 1 calc R . .
C17 C -0.1707(2) 0.02853(16) 0.15019(15) 0.0254(5) Uani 1 1 d . . .
H17A H -0.0950 0.0808 0.1598 0.030 Uiso 1 1 calc R . .
H17B H -0.1753 -0.0041 0.2005 0.030 Uiso 1 1 calc R . .
C18 C -0.1542(2) -0.04235(18) 0.06931(16) 0.0291(5) Uani 1 1 d . . .
H18A H -0.1313 -0.0076 0.0212 0.035 Uiso 1 1 calc R . .
H18B H -0.2349 -0.0883 0.0525 0.035 Uiso 1 1 calc R . .
C19 C -0.0508(2) -0.09700(18) 0.08533(17) 0.0321(5) Uani 1 1 d . . .
H19A H -0.0299 -0.1301 0.0294 0.038 Uiso 1 1 calc R . .
H19B H 0.0260 -0.0507 0.1109 0.038 Uiso 1 1 calc R . .
C20 C -0.0902(3) -0.17046(19) 0.14559(18) 0.0368(6) Uani 1 1 d . . .
H20A H -0.0216 -0.2021 0.1530 0.055 Uiso 1 1 calc R . .
H20B H -0.1650 -0.2175 0.1201 0.055 Uiso 1 1 calc R . .
H20C H -0.1090 -0.1381 0.2017 0.055 Uiso 1 1 calc R . .
C21 C -0.2794(2) 0.13351(16) 0.07499(15) 0.0255(5) Uani 1 1 d . . .
H21A H -0.3598 0.1535 0.0705 0.031 Uiso 1 1 calc R . .
H21B H -0.2702 0.0934 0.0195 0.031 Uiso 1 1 calc R . .
C22 C -0.1708(2) 0.22358(17) 0.08754(16) 0.0277(5) Uani 1 1 d . . .
H22A H -0.1818 0.2673 0.1404 0.033 Uiso 1 1 calc R . .
H22B H -0.0894 0.2057 0.0940 0.033 Uiso 1 1 calc R . .
C23 C -0.1717(2) 0.27358(18) 0.00816(17) 0.0322(6) Uani 1 1 d . . .
H23A H -0.2510 0.2953 0.0048 0.039 Uiso 1 1 calc R . .
H23B H -0.1688 0.2275 -0.0448 0.039 Uiso 1 1 calc R . .
C24 C -0.0585(3) 0.36005(19) 0.01290(19) 0.0411(7) Uani 1 1 d . . .
H24A H -0.0624 0.3893 -0.0382 0.062 Uiso 1 1 calc R . .
H24B H 0.0201 0.3387 0.0153 0.062 Uiso 1 1 calc R . .
H24C H -0.0622 0.4065 0.0646 0.062 Uiso 1 1 calc R . .
C25 C -0.2930(2) 0.13102(17) 0.23651(15) 0.0268(5) Uani 1 1 d . . .
H25A H -0.2148 0.1809 0.2482 0.032 Uiso 1 1 calc R . .
H25B H -0.2942 0.0893 0.2798 0.032 Uiso 1 1 calc R . .
C26 C -0.4059(2) 0.17880(17) 0.24952(16) 0.0288(5) Uani 1 1 d . . .
H26A H -0.4850 0.1298 0.2388 0.035 Uiso 1 1 calc R . .
H26B H -0.4049 0.2222 0.2077 0.035 Uiso 1 1 calc R . .
C27 C -0.4006(2) 0.23531(17) 0.34240(16) 0.0298(5) Uani 1 1 d . . .
H27A H -0.4018 0.1917 0.3841 0.036 Uiso 1 1 calc R . .
H27B H -0.3210 0.2838 0.3531 0.036 Uiso 1 1 calc R . .
C28 C -0.5126(2) 0.28448(18) 0.35693(17) 0.0338(6) Uani 1 1 d . . .
H28A H -0.5062 0.3192 0.4161 0.051 Uiso 1 1 calc R . .
H28B H -0.5915 0.2366 0.3473 0.051 Uiso 1 1 calc R . .
H28C H -0.5107 0.3287 0.3166 0.051 Uiso 1 1 calc R . .
C29 C 0.3039(2) 0.41828(17) 0.68064(16) 0.0272(5) Uani 1 1 d . . .
H29A H 0.3829 0.4312 0.6505 0.033 Uiso 1 1 calc R . .
H29B H 0.3147 0.3766 0.7221 0.033 Uiso 1 1 calc R . .
C30 C 0.2841(2) 0.51322(17) 0.73177(17) 0.0307(5) Uani 1 1 d . . .
H30A H 0.1955 0.5058 0.7472 0.037 Uiso 1 1 calc R . .
H30B H 0.3024 0.5627 0.6953 0.037 Uiso 1 1 calc R . .
C31 C 0.3714(3) 0.54456(18) 0.81516(17) 0.0342(6) Uani 1 1 d . . .
H31A H 0.4578 0.5403 0.8003 0.041 Uiso 1 1 calc R . .
H31B H 0.3728 0.6117 0.8385 0.041 Uiso 1 1 calc R . .
C32 C 0.3305(3) 0.4844(2) 0.88584(18) 0.0445(7) Uani 1 1 d . . .
H32A H 0.3890 0.5077 0.9363 0.067 Uiso 1 1 calc R . .
H32B H 0.3307 0.4181 0.8638 0.067 Uiso 1 1 calc R . .
H32C H 0.2458 0.4896 0.9021 0.067 Uiso 1 1 calc R . .
C33 C 0.2420(2) 0.28336(17) 0.55435(15) 0.0268(5) Uani 1 1 d . . .
H33A H 0.1745 0.2523 0.5097 0.032 Uiso 1 1 calc R . .
H33B H 0.3156 0.3124 0.5246 0.032 Uiso 1 1 calc R . .
C34 C 0.2785(2) 0.20581(17) 0.59865(16) 0.0284(5) Uani 1 1 d . . .
H34A H 0.2050 0.1732 0.6264 0.034 Uiso 1 1 calc R . .
H34B H 0.3461 0.2351 0.6436 0.034 Uiso 1 1 calc R . .
C35 C 0.3240(2) 0.13319(18) 0.53029(16) 0.0313(5) Uani 1 1 d . . .
H35A H 0.3916 0.1674 0.4987 0.038 Uiso 1 1 calc R . .
H35B H 0.2536 0.1006 0.4883 0.038 Uiso 1 1 calc R . .
C36 C 0.3739(2) 0.05800(18) 0.57120(17) 0.0328(6) Uani 1 1 d . . .
H36A H 0.4016 0.0139 0.5259 0.049 Uiso 1 1 calc R . .
H36B H 0.3067 0.0230 0.6015 0.049 Uiso 1 1 calc R . .
H36C H 0.4447 0.0898 0.6120 0.049 Uiso 1 1 calc R . .
C37 C 0.1583(2) 0.43090(17) 0.55657(15) 0.0266(5) Uani 1 1 d . . .
H37A H 0.1294 0.4823 0.5941 0.032 Uiso 1 1 calc R . .
H37B H 0.0865 0.3946 0.5172 0.032 Uiso 1 1 calc R . .
C38 C 0.2650(2) 0.47608(18) 0.50221(16) 0.0307(5) Uani 1 1 d . . .
H38A H 0.3415 0.5045 0.5399 0.037 Uiso 1 1 calc R . .
H38B H 0.2847 0.4262 0.4576 0.037 Uiso 1 1 calc R . .
C39 C 0.2265(2) 0.55342(17) 0.45833(16) 0.0293(5) Uani 1 1 d . . .
H39A H 0.1447 0.5268 0.4260 0.035 Uiso 1 1 calc R . .
H39B H 0.2162 0.6068 0.5030 0.035 Uiso 1 1 calc R . .
C40 C 0.3258(3) 0.59062(19) 0.39602(18) 0.0369(6) Uani 1 1 d . . .
H40A H 0.2986 0.6389 0.3692 0.055 Uiso 1 1 calc R . .
H40B H 0.3354 0.5381 0.3513 0.055 Uiso 1 1 calc R . .
H40C H 0.4064 0.6184 0.4281 0.055 Uiso 1 1 calc R . .
C41 C 0.0829(2) 0.32326(16) 0.66444(15) 0.0252(5) Uani 1 1 d . . .
H41A H 0.1109 0.2846 0.7033 0.030 Uiso 1 1 calc R . .
H41B H 0.0574 0.3769 0.7010 0.030 Uiso 1 1 calc R . .
C42 C -0.0335(2) 0.26216(17) 0.61014(16) 0.0282(5) Uani 1 1 d . . .
H42A H -0.0099 0.2089 0.5718 0.034 Uiso 1 1 calc R . .
H42B H -0.0672 0.3008 0.5738 0.034 Uiso 1 1 calc R . .
C43 C -0.1361(2) 0.22287(17) 0.67101(17) 0.0308(5) Uani 1 1 d . . .
H43A H -0.0995 0.1882 0.7099 0.037 Uiso 1 1 calc R . .
H43B H -0.1620 0.2767 0.7070 0.037 Uiso 1 1 calc R . .
C44 C -0.2531(2) 0.15576(19) 0.62087(19) 0.0381(6) Uani 1 1 d . . .
H44A H -0.3143 0.1330 0.6616 0.057 Uiso 1 1 calc R . .
H44B H -0.2283 0.1017 0.5860 0.057 Uiso 1 1 calc R . .
H44C H -0.2909 0.1901 0.5833 0.057 Uiso 1 1 calc R . .
N1 N 0.19666(18) 0.15928(13) 0.21064(12) 0.0236(4) Uani 1 1 d . . .
N2 N 0.30130(19) 0.26295(14) 0.10404(13) 0.0266(4) Uani 1 1 d . . .
N3 N 0.07310(18) 0.27564(13) 0.28334(13) 0.0254(4) Uani 1 1 d . . .
N4 N 0.16115(18) 0.40949(13) 0.19924(13) 0.0263(4) Uani 1 1 d . . .
N5 N -0.28794(18) 0.07187(13) 0.14650(12) 0.0241(4) Uani 1 1 d . . .
N6 N 0.19693(18) 0.36399(14) 0.61359(13) 0.0250(4) Uani 1 1 d . . .
O1 O 0.29859(16) 0.03506(12) 0.16236(12) 0.0338(4) Uani 1 1 d . . .
O2 O 0.42989(15) 0.15775(12) 0.05423(11) 0.0310(4) Uani 1 1 d . . .
O3 O -0.06397(17) 0.35977(12) 0.36052(12) 0.0368(4) Uani 1 1 d . . .
O4 O 0.03249(17) 0.50723(12) 0.26502(13) 0.0374(4) Uani 1 1 d . . .
Ni1 Ni 0.18715(3) 0.28224(3) 0.19473(2) 0.02314(14) 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 O1 1.236(3) . ?
C1 N1 1.340(3) . ?
C1 C2 1.534(3) . ?
C2 O2 1.254(3) . ?
C2 N2 1.325(3) . ?
C3 O3 1.244(3) . ?
C3 N3 1.338(3) . ?
C3 C4 1.541(3) . ?
C4 O4 1.251(3) . ?
C4 N4 1.323(3) . ?
C5 C6 1.395(3) . ?
C5 N1 1.397(3) . ?
C5 C10 1.422(3) . ?
C6 C7 1.386(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.388(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.390(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.390(3) . ?
C9 H9 0.9300 . ?
C10 N3 1.399(3) . ?
C11 N2 1.452(3) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N4 1.459(3) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.518(3) . ?
C13 N5 1.528(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.526(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.522(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.515(3) . ?
C17 N5 1.523(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.531(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.521(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 N5 1.521(3) . ?
C21 C22 1.525(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.524(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.529(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 N5 1.514(3) . ?
C25 C26 1.516(3) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.522(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.520(4) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 N6 1.518(3) . ?
C29 C30 1.519(3) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.526(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.517(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.518(3) . ?
C33 N6 1.524(3) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.522(3) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.525(3) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 N6 1.524(3) . ?
C37 C38 1.525(3) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.521(3) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.518(3) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C42 1.510(3) . ?
C41 N6 1.525(3) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.534(3) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.517(4) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
N1 Ni1 1.8508(18) . ?
N2 Ni1 1.900(2) . ?
N3 Ni1 1.850(2) . ?
N4 Ni1 1.9016(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N1 128.2(2) . . ?
O1 C1 C2 122.2(2) . . ?
N1 C1 C2 109.57(19) . . ?
O2 C2 N2 127.1(2) . . ?
O2 C2 C1 119.2(2) . . ?
N2 C2 C1 113.72(19) . . ?
O3 C3 N3 128.0(2) . . ?
O3 C3 C4 121.9(2) . . ?
N3 C3 C4 110.0(2) . . ?
O4 C4 N4 127.3(2) . . ?
O4 C4 C3 119.2(2) . . ?
N4 C4 C3 113.47(19) . . ?
C6 C5 N1 127.5(2) . . ?
C6 C5 C10 120.0(2) . . ?
N1 C5 C10 112.5(2) . . ?
C7 C6 C5 119.3(2) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C6 C7 C8 120.9(2) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C7 C8 C9 120.5(2) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C8 C9 C10 119.7(2) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C9 C10 N3 128.0(2) . . ?
C9 C10 C5 119.6(2) . . ?
N3 C10 C5 112.4(2) . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N5 114.94(18) . . ?
C14 C13 H13A 108.5 . . ?
N5 C13 H13A 108.5 . . ?
C14 C13 H13B 108.5 . . ?
N5 C13 H13B 108.5 . . ?
H13A C13 H13B 107.5 . . ?
C13 C14 C15 109.90(19) . . ?
C13 C14 H14A 109.7 . . ?
C15 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
C15 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
C16 C15 C14 112.5(2) . . ?
C16 C15 H15A 109.1 . . ?
C14 C15 H15A 109.1 . . ?
C16 C15 H15B 109.1 . . ?
C14 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 N5 115.43(18) . . ?
C18 C17 H17A 108.4 . . ?
N5 C17 H17A 108.4 . . ?
C18 C17 H17B 108.4 . . ?
N5 C17 H17B 108.4 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 111.8(2) . . ?
C17 C18 H18A 109.3 . . ?
C19 C18 H18A 109.3 . . ?
C17 C18 H18B 109.3 . . ?
C19 C18 H18B 109.3 . . ?
H18A C18 H18B 107.9 . . ?
C20 C19 C18 113.5(2) . . ?
C20 C19 H19A 108.9 . . ?
C18 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N5 C21 C22 116.14(18) . . ?
N5 C21 H21A 108.3 . . ?
C22 C21 H21A 108.3 . . ?
N5 C21 H21B 108.3 . . ?
C22 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
C23 C22 C21 109.30(19) . . ?
C23 C22 H22A 109.8 . . ?
C21 C22 H22A 109.8 . . ?
C23 C22 H22B 109.8 . . ?
C21 C22 H22B 109.8 . . ?
H22A C22 H22B 108.3 . . ?
C22 C23 C24 112.1(2) . . ?
C22 C23 H23A 109.2 . . ?
C24 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
C24 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N5 C25 C26 115.81(19) . . ?
N5 C25 H25A 108.3 . . ?
C26 C25 H25A 108.3 . . ?
N5 C25 H25B 108.3 . . ?
C26 C25 H25B 108.3 . . ?
H25A C25 H25B 107.4 . . ?
C25 C26 C27 110.8(2) . . ?
C25 C26 H26A 109.5 . . ?
C27 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C27 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
C28 C27 C26 111.8(2) . . ?
C28 C27 H27A 109.3 . . ?
C26 C27 H27A 109.3 . . ?
C28 C27 H27B 109.3 . . ?
C26 C27 H27B 109.3 . . ?
H27A C27 H27B 107.9 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N6 C29 C30 115.47(19) . . ?
N6 C29 H29A 108.4 . . ?
C30 C29 H29A 108.4 . . ?
N6 C29 H29B 108.4 . . ?
C30 C29 H29B 108.4 . . ?
H29A C29 H29B 107.5 . . ?
C29 C30 C31 110.8(2) . . ?
C29 C30 H30A 109.5 . . ?
C31 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C31 C30 H30B 109.5 . . ?
H30A C30 H30B 108.1 . . ?
C32 C31 C30 113.6(2) . . ?
C32 C31 H31A 108.9 . . ?
C30 C31 H31A 108.9 . . ?
C32 C31 H31B 108.9 . . ?
C30 C31 H31B 108.9 . . ?
H31A C31 H31B 107.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 N6 116.55(19) . . ?
C34 C33 H33A 108.2 . . ?
N6 C33 H33A 108.2 . . ?
C34 C33 H33B 108.2 . . ?
N6 C33 H33B 108.2 . . ?
H33A C33 H33B 107.3 . . ?
C33 C34 C35 109.29(19) . . ?
C33 C34 H34A 109.8 . . ?
C35 C34 H34A 109.8 . . ?
C33 C34 H34B 109.8 . . ?
C35 C34 H34B 109.8 . . ?
H34A C34 H34B 108.3 . . ?
C34 C35 C36 112.3(2) . . ?
C34 C35 H35A 109.1 . . ?
C36 C35 H35A 109.1 . . ?
C34 C35 H35B 109.1 . . ?
C36 C35 H35B 109.1 . . ?
H35A C35 H35B 107.9 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N6 C37 C38 114.28(19) . . ?
N6 C37 H37A 108.7 . . ?
C38 C37 H37A 108.7 . . ?
N6 C37 H37B 108.7 . . ?
C38 C37 H37B 108.7 . . ?
H37A C37 H37B 107.6 . . ?
C39 C38 C37 111.3(2) . . ?
C39 C38 H38A 109.4 . . ?
C37 C38 H38A 109.4 . . ?
C39 C38 H38B 109.4 . . ?
C37 C38 H38B 109.4 . . ?
H38A C38 H38B 108.0 . . ?
C40 C39 C38 111.5(2) . . ?
C40 C39 H39A 109.3 . . ?
C38 C39 H39A 109.3 . . ?
C40 C39 H39B 109.3 . . ?
C38 C39 H39B 109.3 . . ?
H39A C39 H39B 108.0 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 N6 116.27(19) . . ?
C42 C41 H41A 108.2 . . ?
N6 C41 H41A 108.2 . . ?
C42 C41 H41B 108.2 . . ?
N6 C41 H41B 108.2 . . ?
H41A C41 H41B 107.4 . . ?
C41 C42 C43 109.60(19) . . ?
C41 C42 H42A 109.8 . . ?
C43 C42 H42A 109.8 . . ?
C41 C42 H42B 109.8 . . ?
C43 C42 H42B 109.8 . . ?
H42A C42 H42B 108.2 . . ?
C44 C43 C42 112.6(2) . . ?
C44 C43 H43A 109.1 . . ?
C42 C43 H43A 109.1 . . ?
C44 C43 H43B 109.1 . . ?
C42 C43 H43B 109.1 . . ?
H43A C43 H43B 107.8 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C1 N1 C5 126.97(19) . . ?
C1 N1 Ni1 117.69(15) . . ?
C5 N1 Ni1 115.26(15) . . ?
C2 N2 C11 115.6(2) . . ?
C2 N2 Ni1 113.87(15) . . ?
C11 N2 Ni1 130.53(16) . . ?
C3 N3 C10 127.3(2) . . ?
C3 N3 Ni1 117.38(16) . . ?
C10 N3 Ni1 115.29(15) . . ?
C4 N4 C12 115.72(19) . . ?
C4 N4 Ni1 114.14(15) . . ?
C12 N4 Ni1 130.14(16) . . ?
C25 N5 C21 111.60(17) . . ?
C25 N5 C17 106.31(17) . . ?
C21 N5 C17 111.08(17) . . ?
C25 N5 C13 111.16(17) . . ?
C21 N5 C13 105.43(16) . . ?
C17 N5 C13 111.36(16) . . ?
C29 N6 C33 109.40(17) . . ?
C29 N6 C37 111.17(17) . . ?
C33 N6 C37 108.52(17) . . ?
C29 N6 C41 107.21(17) . . ?
C33 N6 C41 111.09(18) . . ?
C37 N6 C41 109.45(17) . . ?
N3 Ni1 N1 84.55(8) . . ?
N3 Ni1 N2 168.81(8) . . ?
N1 Ni1 N2 84.43(8) . . ?
N3 Ni1 N4 84.61(8) . . ?
N1 Ni1 N4 168.89(8) . . ?
N2 Ni1 N4 106.48(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 O2 -4.3(3) . . . . ?
N1 C1 C2 O2 175.8(2) . . . . ?
O1 C1 C2 N2 174.0(2) . . . . ?
N1 C1 C2 N2 -5.9(3) . . . . ?
O3 C3 C4 O4 -0.6(4) . . . . ?
N3 C3 C4 O4 -179.1(2) . . . . ?
O3 C3 C4 N4 177.6(2) . . . . ?
N3 C3 C4 N4 -1.0(3) . . . . ?
N1 C5 C6 C7 -178.4(2) . . . . ?
C10 C5 C6 C7 0.4(3) . . . . ?
C5 C6 C7 C8 0.0(4) . . . . ?
C6 C7 C8 C9 -0.2(4) . . . . ?
C7 C8 C9 C10 0.0(4) . . . . ?
C8 C9 C10 N3 179.4(2) . . . . ?
C8 C9 C10 C5 0.4(3) . . . . ?
C6 C5 C10 C9 -0.6(3) . . . . ?
N1 C5 C10 C9 178.38(19) . . . . ?
C6 C5 C10 N3 -179.7(2) . . . . ?
N1 C5 C10 N3 -0.7(3) . . . . ?
N5 C13 C14 C15 -177.17(18) . . . . ?
C13 C14 C15 C16 166.6(2) . . . . ?
N5 C17 C18 C19 -168.68(19) . . . . ?
C17 C18 C19 C20 71.3(3) . . . . ?
N5 C21 C22 C23 176.93(19) . . . . ?
C21 C22 C23 C24 -175.3(2) . . . . ?
N5 C25 C26 C27 179.61(19) . . . . ?
C25 C26 C27 C28 179.6(2) . . . . ?
N6 C29 C30 C31 161.5(2) . . . . ?
C29 C30 C31 C32 -72.7(3) . . . . ?
N6 C33 C34 C35 -178.6(2) . . . . ?
C33 C34 C35 C36 174.8(2) . . . . ?
N6 C37 C38 C39 -171.12(19) . . . . ?
C37 C38 C39 C40 -173.5(2) . . . . ?
N6 C41 C42 C43 177.10(18) . . . . ?
C41 C42 C43 C44 -176.6(2) . . . . ?
O1 C1 N1 C5 3.5(4) . . . . ?
C2 C1 N1 C5 -176.7(2) . . . . ?
O1 C1 N1 Ni1 179.8(2) . . . . ?
C2 C1 N1 Ni1 -0.4(2) . . . . ?
C6 C5 N1 C1 -3.5(4) . . . . ?
C10 C5 N1 C1 177.6(2) . . . . ?
C6 C5 N1 Ni1 -179.90(18) . . . . ?
C10 C5 N1 Ni1 1.2(2) . . . . ?
O2 C2 N2 C11 6.6(3) . . . . ?
C1 C2 N2 C11 -171.6(2) . . . . ?
O2 C2 N2 Ni1 -172.60(19) . . . . ?
C1 C2 N2 Ni1 9.3(2) . . . . ?
O3 C3 N3 C10 0.4(4) . . . . ?
C4 C3 N3 C10 178.9(2) . . . . ?
O3 C3 N3 Ni1 177.7(2) . . . . ?
C4 C3 N3 Ni1 -3.9(2) . . . . ?
C9 C10 N3 C3 -1.8(4) . . . . ?
C5 C10 N3 C3 177.3(2) . . . . ?
C9 C10 N3 Ni1 -179.05(19) . . . . ?
C5 C10 N3 Ni1 0.0(2) . . . . ?
O4 C4 N4 C12 3.3(4) . . . . ?
C3 C4 N4 C12 -174.6(2) . . . . ?
O4 C4 N4 Ni1 -176.9(2) . . . . ?
C3 C4 N4 Ni1 5.1(3) . . . . ?
C26 C25 N5 C21 60.8(3) . . . . ?
C26 C25 N5 C17 -177.94(19) . . . . ?
C26 C25 N5 C13 -56.6(2) . . . . ?
C22 C21 N5 C25 54.0(3) . . . . ?
C22 C21 N5 C17 -64.5(2) . . . . ?
C22 C21 N5 C13 174.77(19) . . . . ?
C18 C17 N5 C25 173.99(19) . . . . ?
C18 C17 N5 C21 -64.4(2) . . . . ?
C18 C17 N5 C13 52.8(2) . . . . ?
C14 C13 N5 C25 -64.5(2) . . . . ?
C14 C13 N5 C21 174.38(19) . . . . ?
C14 C13 N5 C17 53.8(2) . . . . ?
C30 C29 N6 C33 167.7(2) . . . . ?
C30 C29 N6 C37 47.8(3) . . . . ?
C30 C29 N6 C41 -71.8(2) . . . . ?
C34 C33 N6 C29 61.6(3) . . . . ?
C34 C33 N6 C37 -176.95(19) . . . . ?
C34 C33 N6 C41 -56.6(3) . . . . ?
C38 C37 N6 C29 61.9(3) . . . . ?
C38 C37 N6 C33 -58.5(3) . . . . ?
C38 C37 N6 C41 -179.9(2) . . . . ?
C42 C41 N6 C29 -177.33(18) . . . . ?
C42 C41 N6 C33 -57.8(2) . . . . ?
C42 C41 N6 C37 62.0(2) . . . . ?
C3 N3 Ni1 N1 -177.02(18) . . . . ?
C10 N3 Ni1 N1 0.56(16) . . . . ?
C3 N3 Ni1 N2 -166.8(4) . . . . ?
C10 N3 Ni1 N2 10.8(5) . . . . ?
C3 N3 Ni1 N4 5.44(18) . . . . ?
C10 N3 Ni1 N4 -176.98(17) . . . . ?
C1 N1 Ni1 N3 -177.72(18) . . . . ?
C5 N1 Ni1 N3 -0.98(16) . . . . ?
C1 N1 Ni1 N2 4.26(17) . . . . ?
C5 N1 Ni1 N2 -179.00(16) . . . . ?
C1 N1 Ni1 N4 -164.9(4) . . . . ?
C5 N1 Ni1 N4 11.8(5) . . . . ?
C2 N2 Ni1 N3 -17.9(5) . . . . ?
C11 N2 Ni1 N3 163.1(4) . . . . ?
C2 N2 Ni1 N1 -7.69(17) . . . . ?
C11 N2 Ni1 N1 173.3(2) . . . . ?
C2 N2 Ni1 N4 170.15(16) . . . . ?
C11 N2 Ni1 N4 -8.8(2) . . . . ?
C4 N4 Ni1 N3 -5.84(17) . . . . ?
C12 N4 Ni1 N3 173.8(2) . . . . ?
C4 N4 Ni1 N1 -18.7(5) . . . . ?
C12 N4 Ni1 N1 161.0(4) . . . . ?
C4 N4 Ni1 N2 172.60(16) . . . . ?
C12 N4 Ni1 N2 -7.7(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        62.00
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.063
####################################################################### 
# 
# 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 1035428'
_audit_update_record             
;
2015-03-09 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H14 N4 Ni O4, 2(C16 H36 N), 2(H2 O)'
_chemical_formula_sum            'C46 H90 N6 Ni O6'
_chemical_formula_weight         881.94

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'
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'
Ni Ni 0.3393 1.1124 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.3834(7)
_cell_length_b                   13.4528(3)
_cell_length_c                   15.9421(4)
_cell_angle_alpha                90
_cell_angle_beta                 110.328(3)
_cell_angle_gamma                90
_cell_volume                     4903.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    110
_cell_measurement_reflns_used    2563
_cell_measurement_theta_min      2.9551
_cell_measurement_theta_max      27.9879


_exptl_crystal_description       block
_exptl_crystal_colour            orange

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_F_000             1936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.446
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.94812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10287
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.960
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4298
_reflns_number_gt                3406
_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       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
;

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'

_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
A comparatively large unrefined electron density peak is observed with ca.
 0.7 e/A3 at a distance of ca. 1.8 A away from O3. That may indicate a 
 disorder of the respective water molecule, although this disorder could not
 be refined reliable.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0590P)²] 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         4298
_refine_ls_number_parameters     275
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0950
_refine_ls_wR_factor_gt          0.0927
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.10575(9) 0.14651(14) 0.35372(13) 0.0287(4) Uani 1 1 d . . . . .
C2 C 0.11337(9) 0.26012(15) 0.35985(13) 0.0305(5) Uani 1 1 d . . . . .
C3 C 0.02931(8) 0.02620(13) 0.27974(11) 0.0230(4) Uani 1 1 d . . . . .
C4 C 0.05814(8) -0.06332(14) 0.30925(12) 0.0264(4) Uani 1 1 d . . . . .
H4 H 0.0967 -0.0640 0.3484 0.032 Uiso 1 1 calc R U . . .
C5 C 0.02835(8) -0.15179(14) 0.27912(12) 0.0284(4) Uani 1 1 d . . . . .
H5 H 0.0472 -0.2120 0.2988 0.034 Uiso 1 1 calc R U . . .
C6 C 0.07197(9) 0.41687(14) 0.31088(13) 0.0319(5) Uani 1 1 d . . . . .
H6A H 0.0447 0.4440 0.2558 0.038 Uiso 1 1 calc R U . . .
H6B H 0.1112 0.4333 0.3133 0.038 Uiso 1 1 calc R U . . .
C7 C 0.06097(10) 0.46485(15) 0.38945(14) 0.0379(5) Uani 1 1 d . . . . .
H7A H 0.0664 0.5354 0.3878 0.057 Uiso 1 1 calc R U . . .
H7B H 0.0879 0.4385 0.4442 0.057 Uiso 1 1 calc R U . . .
H7C H 0.0217 0.4511 0.3862 0.057 Uiso 1 1 calc R U . . .
C8 C 0.15352(8) -0.00423(14) 0.66422(12) 0.0273(4) Uani 1 1 d . . . . .
H8A H 0.1744 -0.0595 0.7005 0.033 Uiso 1 1 calc R U . . .
H8B H 0.1300 0.0263 0.6954 0.033 Uiso 1 1 calc R U . . .
C9 C 0.11279(9) -0.04507(14) 0.57643(13) 0.0278(4) Uani 1 1 d . . . . .
H9A H 0.1341 -0.0890 0.5504 0.033 Uiso 1 1 calc R U . . .
H9B H 0.0967 0.0090 0.5349 0.033 Uiso 1 1 calc R U . . .
C10 C 0.06350(9) -0.10207(16) 0.59313(14) 0.0361(5) Uani 1 1 d . . . . .
H10A H 0.0803 -0.1484 0.6420 0.043 Uiso 1 1 calc R U . . .
H10B H 0.0393 -0.0556 0.6113 0.043 Uiso 1 1 calc R U . . .
C11 C 0.02546(10) -0.15873(19) 0.51216(15) 0.0499(6) Uani 1 1 d . . . . .
H11A H -0.0045 -0.1934 0.5266 0.075 Uiso 1 1 calc R U . . .
H11B H 0.0489 -0.2057 0.4943 0.075 Uiso 1 1 calc R U . . .
H11C H 0.0077 -0.1131 0.4640 0.075 Uiso 1 1 calc R U . . .
C12 C 0.16818(8) 0.16483(13) 0.60982(13) 0.0282(4) Uani 1 1 d . . . . .
H12A H 0.1981 0.2117 0.6085 0.034 Uiso 1 1 calc R U . . .
H12B H 0.1458 0.1474 0.5484 0.034 Uiso 1 1 calc R U . . .
C13 C 0.12777(9) 0.21662(14) 0.64929(13) 0.0318(5) Uani 1 1 d . . . . .
H13A H 0.1486 0.2313 0.7119 0.038 Uiso 1 1 calc R U . . .
H13B H 0.0951 0.1735 0.6454 0.038 Uiso 1 1 calc R U . . .
C14 C 0.10533(9) 0.31268(14) 0.59838(15) 0.0356(5) Uani 1 1 d . . . . .
H14A H 0.1381 0.3570 0.6063 0.043 Uiso 1 1 calc R U . . .
H14B H 0.0879 0.2978 0.5351 0.043 Uiso 1 1 calc R U . . .
C15 C 0.06036(10) 0.36528(15) 0.62888(16) 0.0413(5) Uani 1 1 d . . . . .
H15A H 0.0477 0.4251 0.5947 0.062 Uiso 1 1 calc R U . . .
H15B H 0.0776 0.3816 0.6912 0.062 Uiso 1 1 calc R U . . .
H15C H 0.0274 0.3224 0.6200 0.062 Uiso 1 1 calc R U . . .
C16 C 0.23347(8) 0.03197(13) 0.60335(12) 0.0256(4) Uani 1 1 d . . . . .
H16A H 0.2606 0.0833 0.6001 0.031 Uiso 1 1 calc R U . . .
H16B H 0.2069 0.0199 0.5429 0.031 Uiso 1 1 calc R U . . .
C17 C 0.26792(9) -0.06261(13) 0.63788(12) 0.0273(4) Uani 1 1 d . . . . .
H17A H 0.2428 -0.1120 0.6502 0.033 Uiso 1 1 calc R U . . .
H17B H 0.2999 -0.0489 0.6931 0.033 Uiso 1 1 calc R U . . .
C18 C 0.29185(9) -0.10215(14) 0.56801(13) 0.0308(5) Uani 1 1 d . . . . .
H18A H 0.2594 -0.1191 0.5143 0.037 Uiso 1 1 calc R U . . .
H18B H 0.3143 -0.0502 0.5527 0.037 Uiso 1 1 calc R U . . .
C19 C 0.33029(10) -0.19296(15) 0.59988(14) 0.0377(5) Uani 1 1 d . . . . .
H19A H 0.3447 -0.2143 0.5539 0.056 Uiso 1 1 calc R U . . .
H19B H 0.3079 -0.2455 0.6130 0.056 Uiso 1 1 calc R U . . .
H19C H 0.3626 -0.1766 0.6529 0.056 Uiso 1 1 calc R U . . .
C20 C 0.23719(9) 0.09482(14) 0.75287(12) 0.0295(4) Uani 1 1 d . . . . .
H20A H 0.2589 0.0353 0.7788 0.035 Uiso 1 1 calc R U . . .
H20B H 0.2126 0.1112 0.7874 0.035 Uiso 1 1 calc R U . . .
C21 C 0.28037(9) 0.17911(15) 0.76250(13) 0.0352(5) Uani 1 1 d . . . . .
H21A H 0.3027 0.1670 0.7237 0.042 Uiso 1 1 calc R U . . .
H21B H 0.2592 0.2411 0.7442 0.042 Uiso 1 1 calc R U . . .
C22 C 0.32172(10) 0.18785(15) 0.85863(14) 0.0371(5) Uani 1 1 d . . . . .
H22A H 0.3417 0.2514 0.8661 0.044 Uiso 1 1 calc R U . . .
H22B H 0.2989 0.1873 0.8978 0.044 Uiso 1 1 calc R U . . .
C23 C 0.36664(11) 0.10686(17) 0.88723(15) 0.0473(6) Uani 1 1 d . . . . .
H23A H 0.3900 0.1156 0.9492 0.071 Uiso 1 1 calc R U . . .
H23B H 0.3913 0.1097 0.8517 0.071 Uiso 1 1 calc R U . . .
H23C H 0.3474 0.0435 0.8792 0.071 Uiso 1 1 calc R U . . .
N1 N 0.05153(6) 0.12296(11) 0.30246(10) 0.0235(4) Uani 1 1 d . . . . .
N2 N 0.06553(7) 0.30853(11) 0.30976(10) 0.0279(4) Uani 1 1 d . . . . .
N3 N 0.19821(7) 0.07163(11) 0.65792(10) 0.0258(4) Uani 1 1 d . . . . .
O1 O 0.14703(6) 0.08947(10) 0.39277(9) 0.0356(3) Uani 1 1 d . . . . .
O2 O 0.16151(6) 0.29614(10) 0.40791(10) 0.0407(4) Uani 1 1 d . . . . .
O3 O 0.26701(7) 0.11466(13) 0.41763(12) 0.0481(4) Uani 1 1 d D U . . .
Ni1 Ni 0.0000 0.22520(2) 0.2500 0.02350(12) Uani 1 2 d S T P . .
H3A H 0.2308(12) 0.085(3) 0.384(3) 0.18(2) Uiso 1 1 d D . . . .
H3B H 0.2570(19) 0.171(2) 0.446(3) 0.175(17) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.247(2) . ?
C1 N1 1.329(2) . ?
C1 C2 1.539(3) . ?
C2 O2 1.255(2) . ?
C2 N2 1.332(3) . ?
C3 C4 1.391(2) . ?
C3 N1 1.408(2) . ?
C3 C3 1.414(4) 2 ?
C4 C5 1.390(3) . ?
C4 H4 0.9300 . ?
C5 C5 1.372(4) 2 ?
C5 H5 0.9300 . ?
C6 N2 1.465(2) . ?
C6 C7 1.513(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.510(3) . ?
C8 N3 1.522(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.525(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.509(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.511(3) . ?
C12 N3 1.519(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.523(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.520(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 N3 1.517(2) . ?
C16 C17 1.519(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.522(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.516(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 N3 1.514(2) . ?
C20 C21 1.518(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.518(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.499(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
N1 Ni1 1.8546(15) . ?
N2 Ni1 1.9130(16) . ?
O3 H3A 0.945(19) . ?
O3 H3B 0.954(19) . ?
Ni1 N1 1.8546(15) 2 ?
Ni1 N2 1.9130(16) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N1 128.22(18) . . ?
O1 C1 C2 121.40(18) . . ?
N1 C1 C2 110.38(16) . . ?
O2 C2 N2 128.00(19) . . ?
O2 C2 C1 119.27(18) . . ?
N2 C2 C1 112.72(17) . . ?
C4 C3 N1 127.53(17) . . ?
C4 C3 C3 120.06(11) . 2 ?
N1 C3 C3 112.42(10) . 2 ?
C5 C4 C3 118.83(18) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C5 C5 C4 121.11(11) 2 . ?
C5 C5 H5 119.4 2 . ?
C4 C5 H5 119.4 . . ?
N2 C6 C7 112.66(16) . . ?
N2 C6 H6A 109.1 . . ?
C7 C6 H6A 109.1 . . ?
N2 C6 H6B 109.1 . . ?
C7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 N3 115.99(14) . . ?
C9 C8 H8A 108.3 . . ?
N3 C8 H8A 108.3 . . ?
C9 C8 H8B 108.3 . . ?
N3 C8 H8B 108.3 . . ?
H8A C8 H8B 107.4 . . ?
C8 C9 C10 109.00(15) . . ?
C8 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
C8 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
C11 C10 C9 113.10(17) . . ?
C11 C10 H10A 109.0 . . ?
C9 C10 H10A 109.0 . . ?
C11 C10 H10B 109.0 . . ?
C9 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 N3 116.12(15) . . ?
C13 C12 H12A 108.3 . . ?
N3 C12 H12A 108.3 . . ?
C13 C12 H12B 108.3 . . ?
N3 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
C12 C13 C14 109.56(16) . . ?
C12 C13 H13A 109.8 . . ?
C14 C13 H13A 109.8 . . ?
C12 C13 H13B 109.8 . . ?
C14 C13 H13B 109.8 . . ?
H13A C13 H13B 108.2 . . ?
C15 C14 C13 112.96(17) . . ?
C15 C14 H14A 109.0 . . ?
C13 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
C13 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N3 C16 C17 116.05(14) . . ?
N3 C16 H16A 108.3 . . ?
C17 C16 H16A 108.3 . . ?
N3 C16 H16B 108.3 . . ?
C17 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C16 C17 C18 109.39(15) . . ?
C16 C17 H17A 109.8 . . ?
C18 C17 H17A 109.8 . . ?
C16 C17 H17B 109.8 . . ?
C18 C17 H17B 109.8 . . ?
H17A C17 H17B 108.2 . . ?
C19 C18 C17 112.70(16) . . ?
C19 C18 H18A 109.1 . . ?
C17 C18 H18A 109.1 . . ?
C19 C18 H18B 109.0 . . ?
C17 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 C21 115.30(15) . . ?
N3 C20 H20A 108.4 . . ?
C21 C20 H20A 108.4 . . ?
N3 C20 H20B 108.4 . . ?
C21 C20 H20B 108.4 . . ?
H20A C20 H20B 107.5 . . ?
C22 C21 C20 110.72(17) . . ?
C22 C21 H21A 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
C23 C22 C21 114.18(17) . . ?
C23 C22 H22A 108.7 . . ?
C21 C22 H22A 108.7 . . ?
C23 C22 H22B 108.7 . . ?
C21 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C1 N1 C3 126.18(16) . . ?
C1 N1 Ni1 118.29(13) . . ?
C3 N1 Ni1 115.45(12) . . ?
C2 N2 C6 114.27(17) . . ?
C2 N2 Ni1 114.70(13) . . ?
C6 N2 Ni1 131.02(13) . . ?
C20 N3 C16 111.21(14) . . ?
C20 N3 C12 111.09(14) . . ?
C16 N3 C12 105.71(13) . . ?
C20 N3 C8 106.71(13) . . ?
C16 N3 C8 111.33(14) . . ?
C12 N3 C8 110.87(14) . . ?
H3A O3 H3B 105(3) . . ?
N1 Ni1 N1 84.26(9) 2 . ?
N1 Ni1 N2 83.82(7) 2 2 ?
N1 Ni1 N2 167.67(6) . 2 ?
N1 Ni1 N2 167.66(6) 2 . ?
N1 Ni1 N2 83.81(7) . . ?
N2 Ni1 N2 108.25(10) 2 . ?

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
O1 C1 C2 O2 -2.7(3) . . . . ?
N1 C1 C2 O2 177.85(17) . . . . ?
O1 C1 C2 N2 176.43(17) . . . . ?
N1 C1 C2 N2 -3.0(2) . . . . ?
N1 C3 C4 C5 179.75(16) . . . . ?
C3 C3 C4 C5 0.1(3) 2 . . . ?
C3 C4 C5 C5 0.4(3) . . . 2 ?
N3 C8 C9 C10 -168.24(16) . . . . ?
C8 C9 C10 C11 -171.38(18) . . . . ?
N3 C12 C13 C14 175.28(16) . . . . ?
C12 C13 C14 C15 175.24(17) . . . . ?
N3 C16 C17 C18 170.13(16) . . . . ?
C16 C17 C18 C19 176.16(17) . . . . ?
N3 C20 C21 C22 -173.37(16) . . . . ?
C20 C21 C22 C23 73.0(2) . . . . ?
O1 C1 N1 C3 -1.4(3) . . . . ?
C2 C1 N1 C3 178.02(15) . . . . ?
O1 C1 N1 Ni1 -178.01(15) . . . . ?
C2 C1 N1 Ni1 1.37(19) . . . . ?
C4 C3 N1 C1 3.4(3) . . . . ?
C3 C3 N1 C1 -176.93(18) 2 . . . ?
C4 C3 N1 Ni1 -179.86(14) . . . . ?
C3 C3 N1 Ni1 -0.2(2) 2 . . . ?
O2 C2 N2 C6 1.6(3) . . . . ?
C1 C2 N2 C6 -177.49(15) . . . . ?
O2 C2 N2 Ni1 -177.67(16) . . . . ?
C1 C2 N2 Ni1 3.27(19) . . . . ?
C7 C6 N2 C2 -84.8(2) . . . . ?
C7 C6 N2 Ni1 94.27(19) . . . . ?
C21 C20 N3 C16 65.8(2) . . . . ?
C21 C20 N3 C12 -51.6(2) . . . . ?
C21 C20 N3 C8 -172.59(16) . . . . ?
C17 C16 N3 C20 59.5(2) . . . . ?
C17 C16 N3 C12 -179.81(16) . . . . ?
C17 C16 N3 C8 -59.3(2) . . . . ?
C13 C12 N3 C20 -61.8(2) . . . . ?
C13 C12 N3 C16 177.46(16) . . . . ?
C13 C12 N3 C8 56.7(2) . . . . ?
C9 C8 N3 C20 -175.05(15) . . . . ?
C9 C8 N3 C16 -53.5(2) . . . . ?
C9 C8 N3 C12 63.8(2) . . . . ?
C1 N1 Ni1 N1 177.08(17) . . . 2 ?
C3 N1 Ni1 N1 0.07(8) . . . 2 ?
C1 N1 Ni1 N2 -168.0(2) . . . 2 ?
C3 N1 Ni1 N2 15.0(4) . . . 2 ?
C1 N1 Ni1 N2 0.24(13) . . . . ?
C3 N1 Ni1 N2 -176.77(12) . . . . ?

_refine_diff_density_max         0.710
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.043

_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_abdulm81
_database_code_depnum_ccdc_archive 'CCDC 1035429'
_audit_update_record             
;
2014-11-21 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H36 N), C16 H18 N4 Ni O4'

_chemical_formula_sum            'C48 H90 N6 Ni O4'
_chemical_formula_weight         873.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)
_symmetry_space_group_name_Hall  'P 2yb'


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   13.5126(5)
_cell_length_b                   14.7246(4)
_cell_length_c                   25.4056(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.567(3)
_cell_angle_gamma                90.00
_cell_volume                     5031.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    110
_cell_measurement_reflns_used    9153
_cell_measurement_theta_min      2.9988
_cell_measurement_theta_max      64.0051


_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1920
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_min  0.88134
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  25
_diffrn_standards_decay_%        0

_diffrn_reflns_number            25119
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.47
_diffrn_reflns_theta_max         61.98
_reflns_number_total             14709
_reflns_number_gt                8552
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
;

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2sigma(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. Several atoms are alerted
 by the checkcif procedure by level A to C alerts to have large ADP max/min
 ratio's, high Ueq values when compared to neighbors or have large hirshfeld
 test differences. Furthermore, short intra H...H contacts are alerted.
 Most probably, all of these alerts are due to unresolved disorder. A number
 of atoms/groups could be refined disordered, however, trials to refine
 more atoms/groups as disordered did fail or gave non-reliable results.
 This is most probably due to the comparatively low number of observed vs.
 total reflections. The two highest unrefined electron density peaks Q1 
 (ca. 1.6 e/A3) and Q2 (ca. 1.2 e/A3) are located ca. 1.1 A away from Ni2 and
 ca. 1.1 A away from Ni1, respectively. 
 
;

_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)+(0.1954P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_number_reflns         14709
_refine_ls_number_parameters     1094
_refine_ls_number_restraints     479
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0991
_refine_ls_wR_factor_ref         0.2794
_refine_ls_wR_factor_gt          0.2531
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_restrained_S_all      0.962
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001

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 0.6016(6) 1.3398(4) 0.5304(3) 0.0681(18) Uani 1 1 d . . .
C2 C 0.7134(6) 1.3537(5) 0.5306(3) 0.0721(19) Uani 1 1 d . . .
C3 C 0.5924(11) 1.3886(7) 0.7262(4) 0.140(5) Uani 1 1 d . . .
C4 C 0.6988(14) 1.3946(7) 0.7387(4) 0.163(7) Uani 1 1 d D A .
C5 C 0.4753(5) 1.3597(3) 0.6480(2) 0.102(3) Uani 1 1 d G . .
C6 C 0.3854(6) 1.3602(4) 0.6703(3) 0.135(5) Uani 1 1 d G . .
H6 H 0.3846 1.3661 0.7067 0.162 Uiso 1 1 calc R . .
C7 C 0.2965(5) 1.3518(4) 0.6382(4) 0.176(8) Uani 1 1 d G . .
H7 H 0.2363 1.3522 0.6531 0.211 Uiso 1 1 calc R . .
C8 C 0.2976(4) 1.3430(4) 0.5838(4) 0.140(5) Uani 1 1 d G . .
H8 H 0.2382 1.3374 0.5623 0.168 Uiso 1 1 calc R . .
C9 C 0.3876(5) 1.3425(3) 0.5615(2) 0.107(3) Uani 1 1 d G . .
H9 H 0.3883 1.3365 0.5251 0.128 Uiso 1 1 calc R . .
C10 C 0.4764(4) 1.3508(3) 0.5936(2) 0.087(2) Uani 1 1 d G . .
C12 C 0.8738(14) 1.3569(9) 0.5782(4) 0.183(8) Uani 1 1 d . . .
H12A H 0.9042 1.3372 0.6125 0.220 Uiso 1 1 calc R . .
H12B H 0.8937 1.3166 0.5509 0.220 Uiso 1 1 calc R . .
C11 C 0.8686(11) 1.3902(12) 0.7065(7) 0.156(5) Uani 0.84(2) 1 d PDU A 1
H11A H 0.8946 1.4162 0.6756 0.188 Uiso 0.84(2) 1 calc PR A 1
H11B H 0.8867 1.4306 0.7360 0.188 Uiso 0.84(2) 1 calc PR A 1
C13 C 0.9178(12) 1.3020(13) 0.7178(7) 0.174(7) Uani 0.84(2) 1 d PDU A 1
H13A H 0.8993 1.2611 0.6886 0.208 Uiso 0.84(2) 1 calc PR A 1
H13B H 0.8931 1.2762 0.7492 0.208 Uiso 0.84(2) 1 calc PR A 1
C14 C 1.0346(14) 1.3071(15) 0.7267(8) 0.208(8) Uani 0.84(2) 1 d PDU A 1
H14A H 1.0615 1.2468 0.7293 0.312 Uiso 0.84(2) 1 calc PR A 1
H14B H 1.0540 1.3396 0.7588 0.312 Uiso 0.84(2) 1 calc PR A 1
H14C H 1.0595 1.3381 0.6975 0.312 Uiso 0.84(2) 1 calc PR A 1
C11' C 0.8670(17) 1.398(5) 0.713(3) 0.156(5) Uani 0.16(2) 1 d PDU A 2
H11C H 0.8787 1.4464 0.7390 0.188 Uiso 0.16(2) 1 calc PR A 2
H11D H 0.9027 1.4119 0.6829 0.188 Uiso 0.16(2) 1 calc PR A 2
C13' C 0.900(5) 1.306(5) 0.737(4) 0.174(7) Uani 0.16(2) 1 d PDU A 2
H13C H 0.9234 1.2627 0.7124 0.208 Uiso 0.16(2) 1 calc PR A 2
H13D H 0.8526 1.2778 0.7588 0.208 Uiso 0.16(2) 1 calc PR A 2
C14' C 0.984(8) 1.360(8) 0.770(4) 0.208(8) Uani 0.16(2) 1 d PDU A 2
H14D H 1.0293 1.3182 0.7886 0.312 Uiso 0.16(2) 1 calc PR A 2
H14E H 0.9556 1.3992 0.7941 0.312 Uiso 0.16(2) 1 calc PR A 2
H14F H 1.0195 1.3953 0.7458 0.312 Uiso 0.16(2) 1 calc PR A 2
C15 C 0.8969(9) 1.4541(9) 0.5673(4) 0.137(4) Uani 1 1 d . . .
H15A H 0.8772 1.4930 0.5953 0.165 Uiso 1 1 calc R . .
H15B H 0.8622 1.4735 0.5340 0.165 Uiso 1 1 calc R . .
C16 C 1.0159(9) 1.4584(12) 0.5647(5) 0.178(7) Uani 1 1 d . . .
H16A H 1.0352 1.5196 0.5578 0.266 Uiso 1 1 calc R . .
H16B H 1.0341 1.4193 0.5370 0.266 Uiso 1 1 calc R . .
H16C H 1.0490 1.4387 0.5979 0.266 Uiso 1 1 calc R . .
C17 C 0.3535(7) 0.8612(5) 0.7692(2) 0.086(2) Uani 1 1 d . . .
C18 C 0.2431(7) 0.8626(6) 0.7578(3) 0.085(2) Uani 1 1 d . . .
C19 C 0.3484(9) 0.8969(8) 0.9682(3) 0.116(4) Uani 1 1 d . . .
C20 C 0.2440(7) 0.8827(7) 0.9666(3) 0.096(3) Uani 1 1 d . . .
C21 C 0.4739(3) 0.8898(4) 0.90158(18) 0.087(2) Uani 1 1 d G . .
C22 C 0.5621(5) 0.8975(5) 0.93429(19) 0.119(3) Uani 1 1 d G . .
H22 H 0.5605 0.9030 0.9707 0.142 Uiso 1 1 calc R . .
C23 C 0.6527(4) 0.8971(6) 0.9126(3) 0.144(5) Uani 1 1 d G . .
H23 H 0.7117 0.9023 0.9345 0.173 Uiso 1 1 calc R . .
C24 C 0.6551(4) 0.8890(5) 0.8583(3) 0.127(4) Uani 1 1 d G . .
H24 H 0.7157 0.8887 0.8438 0.153 Uiso 1 1 calc R . .
C25 C 0.5669(5) 0.8813(5) 0.8255(2) 0.116(3) Uani 1 1 d G . .
H25 H 0.5685 0.8758 0.7892 0.139 Uiso 1 1 calc R . .
C26 C 0.4763(4) 0.8817(4) 0.84720(17) 0.0745(18) Uani 1 1 d G . .
C27 C 0.0949(8) 0.8375(7) 0.9187(4) 0.113(3) Uani 1 1 d . . .
H27A H 0.0851 0.8017 0.9498 0.136 Uiso 1 1 calc R . .
H27B H 0.0775 0.8002 0.8877 0.136 Uiso 1 1 calc R . .
C28 C 0.0278(9) 0.9227(8) 0.9169(5) 0.128(4) Uani 1 1 d . . .
H28A H 0.0426 0.9586 0.9487 0.153 Uiso 1 1 calc R . .
H28B H 0.0392 0.9599 0.8866 0.153 Uiso 1 1 calc R . .
C29 C -0.0760(12) 0.8917(12) 0.9129(8) 0.222(9) Uani 1 1 d . . .
H29A H -0.1194 0.9434 0.9117 0.332 Uiso 1 1 calc R . .
H29B H -0.0864 0.8551 0.9432 0.332 Uiso 1 1 calc R . .
H29C H -0.0899 0.8564 0.8813 0.332 Uiso 1 1 calc R . .
C30 C 0.0925(10) 0.8763(9) 0.7879(5) 0.144(4) Uani 1 1 d . . .
H30A H 0.0582 0.8519 0.8166 0.173 Uiso 1 1 calc R . .
H30B H 0.0724 0.8401 0.7567 0.173 Uiso 1 1 calc R . .
C31 C 0.0532(13) 0.9760(9) 0.7767(7) 0.188(7) Uani 1 1 d . . .
H31A H 0.0715 1.0132 0.8077 0.226 Uiso 1 1 calc R . .
H31B H 0.0855 1.0012 0.7475 0.226 Uiso 1 1 calc R . .
C32 C -0.0591(11) 0.9805(12) 0.7635(8) 0.237(11) Uani 1 1 d . . .
H32A H -0.0784 1.0419 0.7551 0.356 Uiso 1 1 calc R . .
H32B H -0.0916 0.9601 0.7933 0.356 Uiso 1 1 calc R . .
H32C H -0.0780 0.9422 0.7336 0.356 Uiso 1 1 calc R . .
C33 C 0.2437(5) 1.0226(5) 0.6027(3) 0.076(2) Uani 1 1 d . . .
H33A H 0.2252 0.9894 0.6332 0.091 Uiso 1 1 calc R . .
H33B H 0.2356 0.9815 0.5727 0.091 Uiso 1 1 calc R . .
C34 C 0.1713(6) 1.0998(6) 0.5921(6) 0.122(4) Uani 1 1 d . . .
H34A H 0.1849 1.1303 0.5598 0.147 Uiso 1 1 calc R . .
H34B H 0.1811 1.1434 0.6208 0.147 Uiso 1 1 calc R . .
C35 C 0.0620(7) 1.0679(7) 0.5869(5) 0.125(4) Uani 1 1 d . . .
H35A H 0.0208 1.1164 0.5709 0.150 Uiso 1 1 calc R . .
H35B H 0.0556 1.0163 0.5631 0.150 Uiso 1 1 calc R . .
C36 C 0.0256(14) 1.0431(15) 0.6349(7) 0.229(7) Uani 1 1 d . . .
H36A H -0.0426 1.0247 0.6283 0.344 Uiso 1 1 calc R . .
H36B H 0.0303 1.0940 0.6586 0.344 Uiso 1 1 calc R . .
H36C H 0.0643 0.9936 0.6505 0.344 Uiso 1 1 calc R . .
C37 C 0.3856(6) 1.1016(5) 0.5665(3) 0.078(2) Uani 1 1 d . . .
H37A H 0.3444 1.1555 0.5618 0.094 Uiso 1 1 calc R . .
H37B H 0.4533 1.1215 0.5762 0.094 Uiso 1 1 calc R . .
C38 C 0.3824(6) 1.0528(5) 0.5138(3) 0.0755(19) Uani 1 1 d . . .
H38A H 0.3195 1.0209 0.5075 0.091 Uiso 1 1 calc R . .
H38B H 0.4352 1.0079 0.5155 0.091 Uiso 1 1 calc R . .
C39 C 0.3938(7) 1.1167(5) 0.4679(3) 0.095(3) Uani 1 1 d . . .
H39A H 0.4110 1.0818 0.4377 0.113 Uiso 1 1 calc R . .
H39B H 0.4480 1.1585 0.4777 0.113 Uiso 1 1 calc R . .
C40 C 0.2993(7) 1.1708(8) 0.4522(5) 0.132(5) Uani 1 1 d . . .
H40A H 0.3101 1.2105 0.4233 0.199 Uiso 1 1 calc R . .
H40B H 0.2825 1.2062 0.4818 0.199 Uiso 1 1 calc R . .
H40C H 0.2459 1.1298 0.4415 0.199 Uiso 1 1 calc R . .
C41 C 0.4118(5) 0.9570(4) 0.6184(3) 0.0660(17) Uani 1 1 d . . .
H41A H 0.3874 0.9220 0.6468 0.079 Uiso 1 1 calc R . .
H41B H 0.3981 0.9221 0.5861 0.079 Uiso 1 1 calc R . .
C42 C 0.5197(5) 0.9656(4) 0.6292(3) 0.0661(17) Uani 1 1 d . . .
H42A H 0.5345 1.0007 0.6613 0.079 Uiso 1 1 calc R . .
H42B H 0.5454 0.9986 0.6004 0.079 Uiso 1 1 calc R . .
C43 C 0.5716(5) 0.8754(5) 0.6355(3) 0.0733(17) Uani 1 1 d . . .
H43A H 0.5417 0.8407 0.6623 0.088 Uiso 1 1 calc R . .
H43B H 0.5603 0.8423 0.6025 0.088 Uiso 1 1 calc R . .
C44 C 0.6802(5) 0.8810(6) 0.6505(4) 0.097(3) Uani 1 1 d . . .
H44A H 0.7076 0.8209 0.6535 0.146 Uiso 1 1 calc R . .
H44B H 0.6924 0.9117 0.6839 0.146 Uiso 1 1 calc R . .
H44C H 0.7110 0.9141 0.6239 0.146 Uiso 1 1 calc R . .
C45 C 0.3696(7) 1.1060(5) 0.6598(3) 0.085(2) Uani 1 1 d . . .
H45A H 0.3269 1.1589 0.6547 0.102 Uiso 1 1 calc R . .
H45B H 0.4378 1.1271 0.6620 0.102 Uiso 1 1 calc R . .
C46 C 0.3516(9) 1.0615(6) 0.7124(4) 0.115(3) Uani 1 1 d . . .
H46A H 0.4046 1.0186 0.7223 0.138 Uiso 1 1 calc R . .
H46B H 0.2894 1.0283 0.7083 0.138 Uiso 1 1 calc R . .
C47 C 0.3477(11) 1.1326(7) 0.7564(4) 0.135(4) Uani 1 1 d . . .
H47A H 0.3821 1.1074 0.7884 0.162 Uiso 1 1 calc R . .
H47B H 0.3856 1.1850 0.7468 0.162 Uiso 1 1 calc R . .
C48 C 0.2673(18) 1.160(2) 0.7674(12) 0.42(3) Uani 1 1 d . . .
H48A H 0.2768 1.2043 0.7950 0.637 Uiso 1 1 calc R . .
H48B H 0.2295 1.1098 0.7791 0.637 Uiso 1 1 calc R . .
H48C H 0.2321 1.1867 0.7366 0.637 Uiso 1 1 calc R . .
C49 C 0.2654(7) 0.5877(4) 0.5739(3) 0.084(2) Uani 1 1 d . C .
H49A H 0.3054 0.5339 0.5823 0.101 Uiso 1 1 calc R . .
H49B H 0.1977 0.5678 0.5640 0.101 Uiso 1 1 calc R . .
C50 C 0.3041(11) 0.6352(7) 0.5268(4) 0.142(5) Uani 1 1 d . . .
H50A H 0.3727 0.6534 0.5358 0.170 Uiso 1 1 calc R . .
H50B H 0.2651 0.6894 0.5182 0.170 Uiso 1 1 calc R . .
C51 C 0.2974(13) 0.5706(7) 0.4784(4) 0.144(5) Uani 1 1 d . . .
H51A H 0.3613 0.5706 0.4639 0.172 Uiso 1 1 calc R . .
H51B H 0.2856 0.5095 0.4905 0.172 Uiso 1 1 calc R . .
C52 C 0.238(2) 0.5878(19) 0.4455(10) 0.44(3) Uani 1 1 d . . .
H52A H 0.2405 0.5451 0.4171 0.659 Uiso 1 1 calc R . .
H52B H 0.2489 0.6480 0.4328 0.659 Uiso 1 1 calc R . .
H52C H 0.1738 0.5849 0.4587 0.659 Uiso 1 1 calc R . .
C53 C 0.2073(8) 0.7338(5) 0.6112(3) 0.098(3) Uani 1 1 d . C .
H53A H 0.2389 0.7687 0.5851 0.118 Uiso 1 1 calc R . .
H53B H 0.2096 0.7700 0.6433 0.118 Uiso 1 1 calc R . .
C54 C 0.0982(6) 0.7179(5) 0.5907(3) 0.081(2) Uani 1 1 d . . .
H54A H 0.0939 0.6877 0.5566 0.097 Uiso 1 1 calc R . .
H54B H 0.0660 0.6799 0.6152 0.097 Uiso 1 1 calc R . .
C55 C 0.0490(7) 0.8084(6) 0.5857(4) 0.095(3) Uani 1 1 d . . .
H55A H 0.0522 0.8372 0.6202 0.113 Uiso 1 1 calc R . .
H55B H 0.0840 0.8468 0.5626 0.113 Uiso 1 1 calc R . .
C56 C -0.0527(9) 0.8000(7) 0.5647(4) 0.122(3) Uani 1 1 d . . .
H56A H -0.0829 0.8590 0.5622 0.184 Uiso 1 1 calc R . .
H56B H -0.0875 0.7623 0.5876 0.184 Uiso 1 1 calc R . .
H56C H -0.0558 0.7730 0.5302 0.184 Uiso 1 1 calc R . .
C57 C 0.3705(8) 0.6793(5) 0.6413(3) 0.108(3) Uani 1 1 d D C .
H57A H 0.3942 0.7167 0.6137 0.129 Uiso 1 1 calc R . .
H57B H 0.3674 0.7174 0.6723 0.129 Uiso 1 1 calc R . .
C58 C 0.4444(7) 0.6052(6) 0.6547(4) 0.122(4) Uani 1 1 d DU . .
H58A H 0.4392 0.5636 0.6250 0.146 Uiso 1 1 calc R B 1
H58B H 0.4219 0.5723 0.6844 0.146 Uiso 1 1 calc R B 1
C59 C 0.5537(15) 0.624(2) 0.6682(12) 0.117(5) Uani 0.430(17) 1 d PDU C 1
H59A H 0.5897 0.5674 0.6668 0.141 Uiso 0.430(17) 1 calc PR C 1
H59B H 0.5761 0.6638 0.6413 0.141 Uiso 0.430(17) 1 calc PR C 1
C60 C 0.5808(14) 0.6667(12) 0.7211(6) 0.084(6) Uani 0.430(17) 1 d PDU C 1
H60A H 0.6508 0.6797 0.7252 0.126 Uiso 0.430(17) 1 calc PR C 1
H60B H 0.5651 0.6256 0.7484 0.126 Uiso 0.430(17) 1 calc PR C 1
H60C H 0.5441 0.7221 0.7237 0.126 Uiso 0.430(17) 1 calc PR C 1
C59' C 0.5421(13) 0.6537(13) 0.6693(10) 0.117(5) Uani 0.570(17) 1 d PDU C 2
H59C H 0.5668 0.6784 0.6377 0.141 Uiso 0.570(17) 1 calc PR C 2
H59D H 0.5317 0.7038 0.6929 0.141 Uiso 0.570(17) 1 calc PR C 2
C60' C 0.6146(14) 0.5917(12) 0.6948(8) 0.130(6) Uani 0.570(17) 1 d PDU C 2
H60D H 0.6724 0.6251 0.7087 0.195 Uiso 0.570(17) 1 calc PR C 2
H60E H 0.6332 0.5480 0.6696 0.195 Uiso 0.570(17) 1 calc PR C 2
H60F H 0.5864 0.5610 0.7232 0.195 Uiso 0.570(17) 1 calc PR C 2
C61 C 0.2218(8) 0.5874(5) 0.6648(3) 0.094(3) Uani 1 1 d . C .
H61A H 0.1596 0.5619 0.6491 0.113 Uiso 1 1 calc R . .
H61B H 0.2667 0.5373 0.6742 0.113 Uiso 1 1 calc R . .
C62 C 0.2021(7) 0.6379(5) 0.7152(3) 0.089(2) Uani 1 1 d . . .
H62A H 0.1496 0.6822 0.7076 0.106 Uiso 1 1 calc R . .
H62B H 0.2617 0.6696 0.7295 0.106 Uiso 1 1 calc R . .
C63 C 0.1710(8) 0.5677(6) 0.7555(3) 0.095(2) Uani 1 1 d . . .
H63A H 0.1149 0.5327 0.7397 0.114 Uiso 1 1 calc R . .
H63B H 0.2256 0.5260 0.7647 0.114 Uiso 1 1 calc R . .
C64 C 0.1426(7) 0.6138(7) 0.8050(3) 0.102(3) Uani 1 1 d . . .
H64A H 0.1230 0.5689 0.8293 0.152 Uiso 1 1 calc R . .
H64B H 0.0883 0.6547 0.7959 0.152 Uiso 1 1 calc R . .
H64C H 0.1986 0.6472 0.8211 0.152 Uiso 1 1 calc R . .
C65 C 0.6288(12) 1.1403(9) 0.8348(4) 0.164(6) Uani 1 1 d U D .
H65A H 0.6590 1.0815 0.8427 0.197 Uiso 1 1 calc R . .
H65B H 0.5577 1.1312 0.8275 0.197 Uiso 1 1 calc R . .
C66 C 0.6687(17) 1.1783(11) 0.7871(5) 0.244(12) Uani 1 1 d . . .
H66A H 0.7366 1.1984 0.7961 0.293 Uiso 1 1 calc R . .
H66B H 0.6295 1.2307 0.7748 0.293 Uiso 1 1 calc R . .
C67 C 0.6663(12) 1.1072(9) 0.7428(4) 0.165(4) Uani 1 1 d . . .
H67A H 0.7028 1.0542 0.7565 0.199 Uiso 1 1 calc R . .
H67B H 0.5978 1.0888 0.7340 0.199 Uiso 1 1 calc R . .
C68 C 0.7055(13) 1.1342(11) 0.6956(5) 0.181(5) Uani 1 1 d . . .
H68A H 0.6981 1.0856 0.6704 0.272 Uiso 1 1 calc R . .
H68B H 0.7747 1.1487 0.7031 0.272 Uiso 1 1 calc R . .
H68C H 0.6703 1.1867 0.6814 0.272 Uiso 1 1 calc R . .
C69 C 0.614(2) 1.2977(14) 0.8855(18) 0.181(8) Uani 0.34(2) 1 d PDU D 1
H69A H 0.6298 1.3313 0.8546 0.217 Uiso 0.34(2) 1 calc PR D 1
H69B H 0.6413 1.3291 0.9172 0.217 Uiso 0.34(2) 1 calc PR D 1
C70 C 0.498(2) 1.282(2) 0.8854(13) 0.165(4) Uani 0.34(2) 1 d PDU D 1
H70A H 0.4716 1.2436 0.8561 0.199 Uiso 0.34(2) 1 calc PR D 1
H70B H 0.4807 1.2559 0.9184 0.199 Uiso 0.34(2) 1 calc PR D 1
C71 C 0.462(3) 1.378(2) 0.8786(18) 0.181(5) Uani 0.34(2) 1 d PDU D 1
H71A H 0.4943 1.4179 0.9057 0.217 Uiso 0.34(2) 1 calc PR D 1
H71B H 0.4728 1.4021 0.8439 0.217 Uiso 0.34(2) 1 calc PR D 1
C72 C 0.355(3) 1.366(5) 0.885(2) 0.229(7) Uani 0.34(2) 1 d PDU D 1
H72A H 0.3225 1.4239 0.8840 0.344 Uiso 0.34(2) 1 calc PR D 1
H72B H 0.3476 1.3365 0.9180 0.344 Uiso 0.34(2) 1 calc PR D 1
H72C H 0.3250 1.3288 0.8565 0.344 Uiso 0.34(2) 1 calc PR D 1
C69' C 0.5787(14) 1.2862(10) 0.8744(6) 0.166(5) Uani 0.66(2) 1 d PDU D 2
H69C H 0.6010 1.3187 0.8445 0.200 Uiso 0.66(2) 1 calc PR D 2
H69D H 0.5914 1.3257 0.9049 0.200 Uiso 0.66(2) 1 calc PR D 2
C70' C 0.4610(14) 1.2776(9) 0.8634(9) 0.168(5) Uani 0.66(2) 1 d PDU D 2
H70C H 0.4455 1.2479 0.8296 0.202 Uiso 0.66(2) 1 calc PR D 2
H70D H 0.4372 1.2389 0.8903 0.202 Uiso 0.66(2) 1 calc PR D 2
C71' C 0.4031(19) 1.3696(10) 0.8628(7) 0.183(7) Uani 0.66(2) 1 d PDU D 2
H71C H 0.4197 1.3990 0.8966 0.220 Uiso 0.66(2) 1 calc PR D 2
H71D H 0.4282 1.4081 0.8360 0.220 Uiso 0.66(2) 1 calc PR D 2
C72' C 0.292(2) 1.3671(13) 0.8525(8) 0.188(7) Uani 0.66(2) 1 d PDU D 2
H72D H 0.2658 1.4278 0.8529 0.281 Uiso 0.66(2) 1 calc PR D 2
H72E H 0.2646 1.3318 0.8795 0.281 Uiso 0.66(2) 1 calc PR D 2
H72F H 0.2732 1.3401 0.8186 0.281 Uiso 0.66(2) 1 calc PR D 2
C77 C 0.6211(14) 1.1419(11) 0.9299(4) 0.213(8) Uani 1 1 d U D .
H77A H 0.6741 1.0988 0.9394 0.255 Uiso 1 1 calc R . .
H77B H 0.5609 1.1081 0.9189 0.255 Uiso 1 1 calc R . .
C78 C 0.604(2) 1.2033(13) 0.9787(6) 0.38(2) Uani 1 1 d D . .
H78A H 0.5617 1.2544 0.9678 0.460 Uiso 1 1 calc R . .
H78B H 0.6672 1.2265 0.9949 0.460 Uiso 1 1 calc R . .
C79 C 0.5509(15) 1.1385(14) 1.0207(6) 0.217(10) Uani 1 1 d D . .
H79A H 0.5212 1.1725 1.0478 0.260 Uiso 1 1 calc R . .
H79B H 0.5039 1.0954 1.0037 0.260 Uiso 1 1 calc R . .
C80 C 0.6476(10) 1.0980(9) 1.0391(5) 0.154(5) Uani 1 1 d D . .
H80A H 0.6386 1.0528 1.0654 0.231 Uiso 1 1 calc R . .
H80B H 0.6916 1.1445 1.0540 0.231 Uiso 1 1 calc R . .
H80C H 0.6758 1.0703 1.0098 0.231 Uiso 1 1 calc R . .
C81 C 0.2145(9) 1.1554(7) 1.0591(4) 0.119(3) Uani 1 1 d . . .
H81A H 0.1491 1.1816 1.0506 0.143 Uiso 1 1 calc R . .
H81B H 0.2608 1.2051 1.0666 0.143 Uiso 1 1 calc R . .
C82 C 0.2434(9) 1.1051(7) 1.0110(4) 0.116(3) Uani 1 1 d . . .
H82A H 0.1962 1.0566 1.0020 0.139 Uiso 1 1 calc R . .
H82B H 0.3086 1.0780 1.0189 0.139 Uiso 1 1 calc R . .
C83 C 0.2452(8) 1.1703(7) 0.9635(4) 0.110(3) Uani 1 1 d . . .
H83A H 0.1822 1.2023 0.9583 0.132 Uiso 1 1 calc R . .
H83B H 0.2972 1.2151 0.9713 0.132 Uiso 1 1 calc R . .
C84 C 0.2631(9) 1.1206(8) 0.9132(4) 0.124(4) Uani 1 1 d . . .
H84A H 0.2652 1.1635 0.8849 0.187 Uiso 1 1 calc R . .
H84B H 0.2102 1.0780 0.9045 0.187 Uiso 1 1 calc R . .
H84C H 0.3252 1.0887 0.9183 0.187 Uiso 1 1 calc R . .
C85 C 0.1438(8) 1.0155(6) 1.1008(3) 0.101(3) Uani 1 1 d . . .
H85A H 0.1412 0.9824 1.1337 0.121 Uiso 1 1 calc R . .
H85B H 0.1720 0.9752 1.0760 0.121 Uiso 1 1 calc R . .
C86 C 0.0360(9) 1.0395(8) 1.0785(4) 0.119(4) Uani 1 1 d . . .
H86A H 0.0369 1.0701 1.0448 0.143 Uiso 1 1 calc R . .
H86B H 0.0067 1.0804 1.1027 0.143 Uiso 1 1 calc R . .
C87 C -0.0277(8) 0.9511(8) 1.0714(4) 0.117(3) Uani 1 1 d . . .
H87A H 0.0051 0.9088 1.0495 0.141 Uiso 1 1 calc R . .
H87B H -0.0312 0.9230 1.1057 0.141 Uiso 1 1 calc R . .
C88 C -0.1222(8) 0.9666(8) 1.0487(5) 0.135(4) Uani 1 1 d . . .
H88A H -0.1579 0.9102 1.0453 0.203 Uiso 1 1 calc R . .
H88B H -0.1193 0.9930 1.0143 0.203 Uiso 1 1 calc R . .
H88C H -0.1556 1.0075 1.0705 0.203 Uiso 1 1 calc R . .
C89 C 0.3090(6) 1.0638(7) 1.1269(4) 0.092(3) Uani 1 1 d . . .
H89A H 0.3291 1.0269 1.0982 0.110 Uiso 1 1 calc R . .
H89B H 0.3038 1.0233 1.1566 0.110 Uiso 1 1 calc R . .
C90 C 0.3936(7) 1.1283(9) 1.1426(5) 0.123(4) Uani 1 1 d . . .
H90A H 0.4011 1.1701 1.1137 0.148 Uiso 1 1 calc R . .
H90B H 0.3782 1.1636 1.1730 0.148 Uiso 1 1 calc R . .
C91 C 0.4896(9) 1.0782(7) 1.1560(5) 0.126(4) Uani 1 1 d . . .
H91A H 0.5070 1.0460 1.1249 0.151 Uiso 1 1 calc R . .
H91B H 0.4806 1.0336 1.1832 0.151 Uiso 1 1 calc R . .
C92 C 0.5757(8) 1.1431(7) 1.1756(6) 0.141(5) Uani 1 1 d . . .
H92A H 0.6364 1.1092 1.1817 0.212 Uiso 1 1 calc R . .
H92B H 0.5610 1.1716 1.2079 0.212 Uiso 1 1 calc R . .
H92C H 0.5831 1.1888 1.1493 0.212 Uiso 1 1 calc R . .
C93 C 0.1743(7) 1.1580(7) 1.1512(4) 0.098(3) Uani 1 1 d . . .
H93A H 0.1110 1.1826 1.1363 0.118 Uiso 1 1 calc R . .
H93B H 0.2202 1.2085 1.1570 0.118 Uiso 1 1 calc R . .
C94 C 0.1599(6) 1.1161(6) 1.2040(3) 0.092(2) Uani 1 1 d . . .
H94A H 0.1060 1.0724 1.1998 0.111 Uiso 1 1 calc R . .
H94B H 0.2200 1.0840 1.2173 0.111 Uiso 1 1 calc R . .
C95 C 0.1365(8) 1.1874(9) 1.2434(4) 0.126(4) Uani 1 1 d . . .
H95A H 0.0801 1.2227 1.2283 0.152 Uiso 1 1 calc R . .
H95B H 0.1928 1.2283 1.2492 0.152 Uiso 1 1 calc R . .
C96 C 0.1128(9) 1.1500(10) 1.2967(4) 0.145(5) Uani 1 1 d . . .
H96A H 0.0985 1.1993 1.3195 0.218 Uiso 1 1 calc R . .
H96B H 0.1689 1.1165 1.3125 0.218 Uiso 1 1 calc R . .
H96C H 0.0561 1.1106 1.2916 0.218 Uiso 1 1 calc R . .
N1 N 0.5740(5) 1.3525(3) 0.5783(2) 0.0747(16) Uani 1 1 d . . .
N2 N 0.7576(5) 1.3645(6) 0.5770(2) 0.0870(18) Uani 1 1 d . . .
N3 N 0.5675(7) 1.3706(5) 0.6741(3) 0.102(2) Uani 1 1 d . . .
N4 N 0.7583(7) 1.3875(6) 0.6970(2) 0.144(4) Uani 1 1 d D . .
N5 N 0.3849(5) 0.8734(5) 0.8206(2) 0.0819(16) Uani 1 1 d . . .
N6 N 0.1970(5) 0.8627(5) 0.8010(2) 0.0751(14) Uani 1 1 d . . .
C73 C 0.7617(11) 1.2248(14) 0.8901(6) 0.174(6) Uani 0.721(13) 1 d PDU D 1
H73A H 0.7759 1.2533 0.8572 0.209 Uiso 0.721(13) 1 calc PR D 1
H73B H 0.7719 1.2710 0.9173 0.209 Uiso 0.721(13) 1 calc PR D 1
C74 C 0.8417(12) 1.1545(15) 0.9027(8) 0.203(6) Uani 0.721(13) 1 d PDU D 1
H74A H 0.8349 1.1094 0.8747 0.244 Uiso 0.721(13) 1 calc PR D 1
H74B H 0.8275 1.1241 0.9350 0.244 Uiso 0.721(13) 1 calc PR D 1
C75 C 0.9530(14) 1.1844(13) 0.9098(7) 0.185(5) Uani 0.721(13) 1 d PDU D 1
H75A H 0.9591 1.2365 0.9332 0.222 Uiso 0.721(13) 1 calc PR D 1
H75B H 0.9919 1.1355 0.9270 0.222 Uiso 0.721(13) 1 calc PR D 1
C76 C 0.9964(12) 1.2081(11) 0.8606(5) 0.127(4) Uani 0.721(13) 1 d PDU D 1
H76A H 1.0670 1.2153 0.8678 0.190 Uiso 0.721(13) 1 calc PR D 1
H76B H 0.9678 1.2640 0.8468 0.190 Uiso 0.721(13) 1 calc PR D 1
H76C H 0.9826 1.1606 0.8350 0.190 Uiso 0.721(13) 1 calc PR D 1
C73' C 0.7524(19) 1.228(3) 0.906(2) 0.174(6) Uani 0.279(13) 1 d PDU D 2
H73C H 0.7500 1.2724 0.9339 0.209 Uiso 0.279(13) 1 calc PR D 2
H73D H 0.7871 1.2552 0.8780 0.209 Uiso 0.279(13) 1 calc PR D 2
C74' C 0.808(2) 1.144(3) 0.9272(18) 0.203(6) Uani 0.279(13) 1 d PDU D 2
H74C H 0.7857 1.0898 0.9076 0.244 Uiso 0.279(13) 1 calc PR D 2
H74D H 0.8006 1.1346 0.9644 0.244 Uiso 0.279(13) 1 calc PR D 2
C75' C 0.918(2) 1.167(3) 0.919(2) 0.185(5) Uani 0.279(13) 1 d PDU D 2
H75C H 0.9574 1.1716 0.9523 0.222 Uiso 0.279(13) 1 calc PR D 2
H75D H 0.9456 1.1192 0.8980 0.222 Uiso 0.279(13) 1 calc PR D 2
C76' C 0.916(3) 1.258(2) 0.8886(15) 0.127(4) Uani 0.279(13) 1 d PDU D 2
H76D H 0.9829 1.2807 0.8893 0.190 Uiso 0.279(13) 1 calc PR D 2
H76E H 0.8758 1.3005 0.9053 0.190 Uiso 0.279(13) 1 calc PR D 2
H76F H 0.8895 1.2486 0.8526 0.190 Uiso 0.279(13) 1 calc PR D 2
N8 N 0.1931(5) 0.8638(6) 0.9202(2) 0.0811(16) Uani 1 1 d . . .
N9 N 0.3514(4) 1.0465(4) 0.6123(2) 0.0645(14) Uani 1 1 d . . .
N10 N 0.2669(6) 0.6468(4) 0.6231(2) 0.089(2) Uani 1 1 d D . .
N11 N 0.2127(5) 1.0955(5) 1.1111(3) 0.097(2) Uani 1 1 d . . .
N12 N 0.6489(8) 1.2032(8) 0.8843(4) 0.179(3) Uani 1 1 d DU . .
O1 O 0.5456(4) 1.3235(3) 0.4894(2) 0.0853(14) Uani 1 1 d . . .
O2 O 0.7520(4) 1.3519(3) 0.48677(17) 0.0821(14) Uani 1 1 d . . .
O3 O 0.5365(10) 1.3923(8) 0.7610(3) 0.231(7) Uani 1 1 d . . .
O4 O 0.7463(10) 1.4005(7) 0.7861(2) 0.223(7) Uani 1 1 d . . .
O5 O 0.4113(6) 0.8462(3) 0.7337(2) 0.110(2) Uani 1 1 d . . .
O6 O 0.2067(5) 0.8664(4) 0.70971(18) 0.1028(17) Uani 1 1 d . . .
O7 O 0.4061(6) 0.9183(6) 1.0074(2) 0.136(3) Uani 1 1 d . . .
O8 O 0.2041(5) 0.8756(6) 1.0093(2) 0.119(2) Uani 1 1 d . . .
Ni1 Ni 0.67484(11) 1.36998(9) 0.63224(4) 0.0919(5) Uani 1 1 d . A .
Ni2 Ni 0.28130(9) 0.87169(9) 0.86398(4) 0.0773(4) Uani 1 1 d . . .
N7 N 0.3822(5) 0.8840(6) 0.9185(3) 0.101(2) 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 O1 1.250(8) . ?
C1 N1 1.319(8) . ?
C1 C2 1.524(11) . ?
C2 O2 1.275(8) . ?
C2 N2 1.279(8) . ?
C3 O3 1.217(12) . ?
C3 N3 1.361(12) . ?
C3 C4 1.44(2) . ?
C4 O4 1.312(15) . ?
C4 N4 1.394(14) . ?
C5 N3 1.363(10) . ?
C5 C6 1.3900 . ?
C5 C10 1.3900 . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 C9 1.3900 . ?
C8 H8 0.9300 . ?
C9 C10 1.3900 . ?
C9 H9 0.9300 . ?
C10 N1 1.412(8) . ?
C12 C15 1.498(18) . ?
C12 N2 1.572(19) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C11 C13 1.474(15) . ?
C11 N4 1.488(14) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C14 1.575(16) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C11' N4 1.49(2) . ?
C11' C13' 1.54(2) . ?
C11' H11C 0.9700 . ?
C11' H11D 0.9700 . ?
C13' C14' 1.55(2) . ?
C13' H13C 0.9700 . ?
C13' H13D 0.9700 . ?
C14' H14D 0.9600 . ?
C14' H14E 0.9600 . ?
C14' H14F 0.9600 . ?
C15 C16 1.617(17) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 O5 1.267(9) . ?
C17 N5 1.346(9) . ?
C17 C18 1.493(12) . ?
C18 O6 1.274(8) . ?
C18 N6 1.313(10) . ?
C19 O7 1.243(11) . ?
C19 N7 1.398(11) . ?
C19 C20 1.424(14) . ?
C20 O8 1.263(9) . ?
C20 N8 1.335(10) . ?
C21 N7 1.353(8) . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 C24 1.3900 . ?
C23 H23 0.9300 . ?
C24 C25 1.3900 . ?
C24 H24 0.9300 . ?
C25 C26 1.3900 . ?
C25 H25 0.9300 . ?
C26 N5 1.353(8) . ?
C27 N8 1.379(13) . ?
C27 C28 1.546(14) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.469(18) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 N6 1.433(15) . ?
C30 C31 1.577(19) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.52(2) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N9 1.494(10) . ?
C33 C34 1.507(11) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.543(14) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.407(19) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C38 1.516(11) . ?
C37 N9 1.528(8) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.518(10) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.525(13) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C42 1.462(10) . ?
C41 N9 1.550(8) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.503(9) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.483(10) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 N9 1.491(10) . ?
C45 C46 1.529(12) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.537(12) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.21(2) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 C50 1.522(12) . ?
C49 N10 1.523(9) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C50 C51 1.552(14) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 C52 1.130(19) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 N10 1.528(12) . ?
C53 C54 1.534(13) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 C55 1.490(11) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 C56 1.430(14) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 C58 1.495(12) . ?
C57 N10 1.509(12) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C58 C59 1.510(18) . ?
C58 C59' 1.516(16) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C59 C60 1.49(2) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C59' C60' 1.446(17) . ?
C59' H59C 0.9700 . ?
C59' H59D 0.9700 . ?
C60' H60D 0.9600 . ?
C60' H60E 0.9600 . ?
C60' H60F 0.9600 . ?
C61 C62 1.526(11) . ?
C61 N10 1.545(9) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 C63 1.543(11) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C63 C64 1.509(12) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C65 C66 1.483(14) . ?
C65 N12 1.564(12) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C66 C67 1.536(13) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C67 C68 1.412(15) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C69 N12 1.472(14) . ?
C69 C70 1.59(2) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C70 C71 1.50(2) . ?
C70 H70A 0.9700 . ?
C70 H70B 0.9700 . ?
C71 C72 1.49(2) . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C69' N12 1.553(16) . ?
C69' C70' 1.592(16) . ?
C69' H69C 0.9700 . ?
C69' H69D 0.9700 . ?
C70' C71' 1.563(16) . ?
C70' H70C 0.9700 . ?
C70' H70D 0.9700 . ?
C71' C72' 1.505(17) . ?
C71' H71C 0.9700 . ?
C71' H71D 0.9700 . ?
C72' H72D 0.9600 . ?
C72' H72E 0.9600 . ?
C72' H72F 0.9600 . ?
C77 N12 1.543(15) . ?
C77 C78 1.57(2) . ?
C77 H77A 0.9700 . ?
C77 H77B 0.9700 . ?
C78 C79 1.65(2) . ?
C78 H78A 0.9700 . ?
C78 H78B 0.9700 . ?
C79 C80 1.471(15) . ?
C79 H79A 0.9700 . ?
C79 H79B 0.9700 . ?
C80 H80A 0.9600 . ?
C80 H80B 0.9600 . ?
C80 H80C 0.9600 . ?
C81 C82 1.512(14) . ?
C81 N11 1.591(12) . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C82 C83 1.544(13) . ?
C82 H82A 0.9700 . ?
C82 H82B 0.9700 . ?
C83 C84 1.513(13) . ?
C83 H83A 0.9700 . ?
C83 H83B 0.9700 . ?
C84 H84A 0.9600 . ?
C84 H84B 0.9600 . ?
C84 H84C 0.9600 . ?
C85 N11 1.508(11) . ?
C85 C86 1.552(15) . ?
C85 H85A 0.9700 . ?
C85 H85B 0.9700 . ?
C86 C87 1.561(13) . ?
C86 H86A 0.9700 . ?
C86 H86B 0.9700 . ?
C87 C88 1.369(14) . ?
C87 H87A 0.9700 . ?
C87 H87B 0.9700 . ?
C88 H88A 0.9600 . ?
C88 H88B 0.9600 . ?
C88 H88C 0.9600 . ?
C89 N11 1.404(12) . ?
C89 C90 1.511(14) . ?
C89 H89A 0.9700 . ?
C89 H89B 0.9700 . ?
C90 C91 1.502(15) . ?
C90 H90A 0.9700 . ?
C90 H90B 0.9700 . ?
C91 C92 1.551(15) . ?
C91 H91A 0.9700 . ?
C91 H91B 0.9700 . ?
C92 H92A 0.9600 . ?
C92 H92B 0.9600 . ?
C92 H92C 0.9600 . ?
C93 N11 1.501(11) . ?
C93 C94 1.508(13) . ?
C93 H93A 0.9700 . ?
C93 H93B 0.9700 . ?
C94 C95 1.506(12) . ?
C94 H94A 0.9700 . ?
C94 H94B 0.9700 . ?
C95 C96 1.524(16) . ?
C95 H95A 0.9700 . ?
C95 H95B 0.9700 . ?
C96 H96A 0.9600 . ?
C96 H96B 0.9600 . ?
C96 H96C 0.9600 . ?
N1 Ni1 1.855(7) . ?
N2 Ni1 1.879(6) . ?
N3 Ni1 1.879(7) . ?
N4 Ni1 1.919(8) . ?
N5 Ni2 1.864(6) . ?
N6 Ni2 1.877(6) . ?
C73 C74 1.509(13) . ?
C73 N12 1.551(12) . ?
C73 H73A 0.9700 . ?
C73 H73B 0.9700 . ?
C74 C75 1.561(11) . ?
C74 H74A 0.9700 . ?
C74 H74B 0.9700 . ?
C75 C76 1.473(11) . ?
C75 H75A 0.9700 . ?
C75 H75B 0.9700 . ?
C76 H76A 0.9600 . ?
C76 H76B 0.9600 . ?
C76 H76C 0.9600 . ?
C73' N12 1.497(19) . ?
C73' C74' 1.53(2) . ?
C73' H73C 0.9700 . ?
C73' H73D 0.9700 . ?
C74' C75' 1.549(19) . ?
C74' H74C 0.9700 . ?
C74' H74D 0.9700 . ?
C75' C76' 1.542(19) . ?
C75' H75C 0.9700 . ?
C75' H75D 0.9700 . ?
C76' H76D 0.9600 . ?
C76' H76E 0.9600 . ?
C76' H76F 0.9600 . ?
N8 Ni2 1.950(6) . ?
Ni2 N7 1.855(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N1 126.4(7) . . ?
O1 C1 C2 123.2(6) . . ?
N1 C1 C2 110.3(6) . . ?
O2 C2 N2 127.8(7) . . ?
O2 C2 C1 119.0(6) . . ?
N2 C2 C1 113.1(6) . . ?
O3 C3 N3 127.1(14) . . ?
O3 C3 C4 120.9(11) . . ?
N3 C3 C4 111.8(9) . . ?
O4 C4 N4 115.8(15) . . ?
O4 C4 C3 126.4(11) . . ?
N4 C4 C3 117.7(9) . . ?
N3 C5 C6 126.6(5) . . ?
N3 C5 C10 113.3(5) . . ?
C6 C5 C10 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 120.0 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C10 C9 C8 120.0 . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C5 120.0 . . ?
C9 C10 N1 128.0(5) . . ?
C5 C10 N1 112.0(5) . . ?
C15 C12 N2 98.8(13) . . ?
C15 C12 H12A 112.0 . . ?
N2 C12 H12A 112.0 . . ?
C15 C12 H12B 112.0 . . ?
N2 C12 H12B 112.0 . . ?
H12A C12 H12B 109.7 . . ?
C13 C11 N4 115.8(11) . . ?
C13 C11 H11A 108.3 . . ?
N4 C11 H11A 108.3 . . ?
C13 C11 H11B 108.3 . . ?
N4 C11 H11B 108.3 . . ?
H11A C11 H11B 107.4 . . ?
C11 C13 C14 114.4(14) . . ?
C11 C13 H13A 108.7 . . ?
C14 C13 H13A 108.7 . . ?
C11 C13 H13B 108.7 . . ?
C14 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C11' C13' 105(3) . . ?
N4 C11' H11C 110.8 . . ?
C13' C11' H11C 110.8 . . ?
N4 C11' H11D 110.8 . . ?
C13' C11' H11D 110.8 . . ?
H11C C11' H11D 108.8 . . ?
C11' C13' C14' 86(6) . . ?
C11' C13' H13C 114.4 . . ?
C14' C13' H13C 114.4 . . ?
C11' C13' H13D 114.4 . . ?
C14' C13' H13D 114.4 . . ?
H13C C13' H13D 111.5 . . ?
C13' C14' H14D 109.5 . . ?
C13' C14' H14E 109.5 . . ?
H14D C14' H14E 109.5 . . ?
C13' C14' H14F 109.5 . . ?
H14D C14' H14F 109.5 . . ?
H14E C14' H14F 109.5 . . ?
C12 C15 C16 105.7(13) . . ?
C12 C15 H15A 110.6 . . ?
C16 C15 H15A 110.6 . . ?
C12 C15 H15B 110.6 . . ?
C16 C15 H15B 110.6 . . ?
H15A C15 H15B 108.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O5 C17 N5 123.8(9) . . ?
O5 C17 C18 122.5(7) . . ?
N5 C17 C18 113.6(7) . . ?
O6 C18 N6 129.1(8) . . ?
O6 C18 C17 118.1(8) . . ?
N6 C18 C17 112.7(6) . . ?
O7 C19 N7 121.6(11) . . ?
O7 C19 C20 127.2(9) . . ?
N7 C19 C20 111.2(7) . . ?
O8 C20 N8 121.1(9) . . ?
O8 C20 C19 119.4(8) . . ?
N8 C20 C19 118.8(7) . . ?
N7 C21 C22 125.0(5) . . ?
N7 C21 C26 114.8(5) . . ?
C22 C21 C26 120.0 . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C24 120.0 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 120.0 . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C26 C25 C24 120.0 . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
N5 C26 C25 126.7(4) . . ?
N5 C26 C21 113.3(4) . . ?
C25 C26 C21 120.0 . . ?
N8 C27 C28 109.4(9) . . ?
N8 C27 H27A 109.8 . . ?
C28 C27 H27A 109.8 . . ?
N8 C27 H27B 109.8 . . ?
C28 C27 H27B 109.8 . . ?
H27A C27 H27B 108.2 . . ?
C29 C28 C27 107.7(11) . . ?
C29 C28 H28A 110.2 . . ?
C27 C28 H28A 110.2 . . ?
C29 C28 H28B 110.2 . . ?
C27 C28 H28B 110.2 . . ?
H28A C28 H28B 108.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N6 C30 C31 118.6(10) . . ?
N6 C30 H30A 107.7 . . ?
C31 C30 H30A 107.7 . . ?
N6 C30 H30B 107.7 . . ?
C31 C30 H30B 107.7 . . ?
H30A C30 H30B 107.1 . . ?
C32 C31 C30 112.9(13) . . ?
C32 C31 H31A 109.0 . . ?
C30 C31 H31A 109.0 . . ?
C32 C31 H31B 109.0 . . ?
C30 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N9 C33 C34 117.2(6) . . ?
N9 C33 H33A 108.0 . . ?
C34 C33 H33A 108.0 . . ?
N9 C33 H33B 108.0 . . ?
C34 C33 H33B 108.0 . . ?
H33A C33 H33B 107.3 . . ?
C33 C34 C35 112.6(7) . . ?
C33 C34 H34A 109.1 . . ?
C35 C34 H34A 109.1 . . ?
C33 C34 H34B 109.1 . . ?
C35 C34 H34B 109.1 . . ?
H34A C34 H34B 107.8 . . ?
C36 C35 C34 114.6(12) . . ?
C36 C35 H35A 108.6 . . ?
C34 C35 H35A 108.6 . . ?
C36 C35 H35B 108.6 . . ?
C34 C35 H35B 108.6 . . ?
H35A C35 H35B 107.6 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 N9 115.9(6) . . ?
C38 C37 H37A 108.3 . . ?
N9 C37 H37A 108.3 . . ?
C38 C37 H37B 108.3 . . ?
N9 C37 H37B 108.3 . . ?
H37A C37 H37B 107.4 . . ?
C37 C38 C39 112.8(6) . . ?
C37 C38 H38A 109.0 . . ?
C39 C38 H38A 109.0 . . ?
C37 C38 H38B 109.0 . . ?
C39 C38 H38B 109.0 . . ?
H38A C38 H38B 107.8 . . ?
C38 C39 C40 112.3(8) . . ?
C38 C39 H39A 109.1 . . ?
C40 C39 H39A 109.1 . . ?
C38 C39 H39B 109.1 . . ?
C40 C39 H39B 109.1 . . ?
H39A C39 H39B 107.9 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 N9 116.8(5) . . ?
C42 C41 H41A 108.1 . . ?
N9 C41 H41A 108.1 . . ?
C42 C41 H41B 108.1 . . ?
N9 C41 H41B 108.1 . . ?
H41A C41 H41B 107.3 . . ?
C41 C42 C43 113.0(5) . . ?
C41 C42 H42A 109.0 . . ?
C43 C42 H42A 109.0 . . ?
C41 C42 H42B 109.0 . . ?
C43 C42 H42B 109.0 . . ?
H42A C42 H42B 107.8 . . ?
C44 C43 C42 114.7(6) . . ?
C44 C43 H43A 108.6 . . ?
C42 C43 H43A 108.6 . . ?
C44 C43 H43B 108.6 . . ?
C42 C43 H43B 108.6 . . ?
H43A C43 H43B 107.6 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N9 C45 C46 115.3(6) . . ?
N9 C45 H45A 108.5 . . ?
C46 C45 H45A 108.5 . . ?
N9 C45 H45B 108.5 . . ?
C46 C45 H45B 108.5 . . ?
H45A C45 H45B 107.5 . . ?
C45 C46 C47 111.4(7) . . ?
C45 C46 H46A 109.4 . . ?
C47 C46 H46A 109.4 . . ?
C45 C46 H46B 109.4 . . ?
C47 C46 H46B 109.4 . . ?
H46A C46 H46B 108.0 . . ?
C48 C47 C46 119.1(14) . . ?
C48 C47 H47A 107.5 . . ?
C46 C47 H47A 107.5 . . ?
C48 C47 H47B 107.5 . . ?
C46 C47 H47B 107.5 . . ?
H47A C47 H47B 107.0 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 N10 113.8(6) . . ?
C50 C49 H49A 108.8 . . ?
N10 C49 H49A 108.8 . . ?
C50 C49 H49B 108.8 . . ?
N10 C49 H49B 108.8 . . ?
H49A C49 H49B 107.7 . . ?
C49 C50 C51 110.1(8) . . ?
C49 C50 H50A 109.6 . . ?
C51 C50 H50A 109.6 . . ?
C49 C50 H50B 109.6 . . ?
C51 C50 H50B 109.6 . . ?
H50A C50 H50B 108.2 . . ?
C52 C51 C50 115.5(15) . . ?
C52 C51 H51A 108.4 . . ?
C50 C51 H51A 108.4 . . ?
C52 C51 H51B 108.4 . . ?
C50 C51 H51B 108.4 . . ?
H51A C51 H51B 107.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N10 C53 C54 114.2(6) . . ?
N10 C53 H53A 108.7 . . ?
C54 C53 H53A 108.7 . . ?
N10 C53 H53B 108.7 . . ?
C54 C53 H53B 108.7 . . ?
H53A C53 H53B 107.6 . . ?
C55 C54 C53 107.3(7) . . ?
C55 C54 H54A 110.2 . . ?
C53 C54 H54A 110.2 . . ?
C55 C54 H54B 110.2 . . ?
C53 C54 H54B 110.2 . . ?
H54A C54 H54B 108.5 . . ?
C56 C55 C54 111.0(8) . . ?
C56 C55 H55A 109.4 . . ?
C54 C55 H55A 109.4 . . ?
C56 C55 H55B 109.4 . . ?
C54 C55 H55B 109.4 . . ?
H55A C55 H55B 108.0 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C58 C57 N10 114.7(6) . . ?
C58 C57 H57A 108.6 . . ?
N10 C57 H57A 108.6 . . ?
C58 C57 H57B 108.6 . . ?
N10 C57 H57B 108.6 . . ?
H57A C57 H57B 107.6 . . ?
C57 C58 C59 122.2(14) . . ?
C57 C58 C59' 104.9(10) . . ?
C59 C58 C59' 17.7(16) . . ?
C57 C58 H58A 106.8 . . ?
C59 C58 H58A 106.8 . . ?
C59' C58 H58A 118.9 . . ?
C57 C58 H58B 106.8 . . ?
C59 C58 H58B 106.8 . . ?
C59' C58 H58B 112.1 . . ?
H58A C58 H58B 106.6 . . ?
C60 C59 C58 115.6(19) . . ?
C60 C59 H59A 108.4 . . ?
C58 C59 H59A 108.4 . . ?
C60 C59 H59B 108.4 . . ?
C58 C59 H59B 108.4 . . ?
H59A C59 H59B 107.5 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C60' C59' C58 110.4(15) . . ?
C60' C59' H59C 109.6 . . ?
C58 C59' H59C 109.6 . . ?
C60' C59' H59D 109.6 . . ?
C58 C59' H59D 109.6 . . ?
H59C C59' H59D 108.1 . . ?
C59' C60' H60D 109.5 . . ?
C59' C60' H60E 109.5 . . ?
H60D C60' H60E 109.5 . . ?
C59' C60' H60F 109.5 . . ?
H60D C60' H60F 109.5 . . ?
H60E C60' H60F 109.5 . . ?
C62 C61 N10 114.3(6) . . ?
C62 C61 H61A 108.7 . . ?
N10 C61 H61A 108.7 . . ?
C62 C61 H61B 108.7 . . ?
N10 C61 H61B 108.7 . . ?
H61A C61 H61B 107.6 . . ?
C61 C62 C63 108.1(6) . . ?
C61 C62 H62A 110.1 . . ?
C63 C62 H62A 110.1 . . ?
C61 C62 H62B 110.1 . . ?
C63 C62 H62B 110.1 . . ?
H62A C62 H62B 108.4 . . ?
C64 C63 C62 111.0(7) . . ?
C64 C63 H63A 109.4 . . ?
C62 C63 H63A 109.4 . . ?
C64 C63 H63B 109.4 . . ?
C62 C63 H63B 109.4 . . ?
H63A C63 H63B 108.0 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C66 C65 N12 112.7(7) . . ?
C66 C65 H65A 109.1 . . ?
N12 C65 H65A 109.1 . . ?
C66 C65 H65B 109.1 . . ?
N12 C65 H65B 109.1 . . ?
H65A C65 H65B 107.8 . . ?
C65 C66 C67 111.0(9) . . ?
C65 C66 H66A 109.4 . . ?
C67 C66 H66A 109.4 . . ?
C65 C66 H66B 109.4 . . ?
C67 C66 H66B 109.4 . . ?
H66A C66 H66B 108.0 . . ?
C68 C67 C66 116.5(10) . . ?
C68 C67 H67A 108.2 . . ?
C66 C67 H67A 108.2 . . ?
C68 C67 H67B 108.2 . . ?
C66 C67 H67B 108.2 . . ?
H67A C67 H67B 107.3 . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
N12 C69 C70 100(2) . . ?
N12 C69 H69A 111.7 . . ?
C70 C69 H69A 111.7 . . ?
N12 C69 H69B 111.7 . . ?
C70 C69 H69B 111.7 . . ?
H69A C69 H69B 109.5 . . ?
C71 C70 C69 99.4(19) . . ?
C71 C70 H70A 111.9 . . ?
C69 C70 H70A 111.9 . . ?
C71 C70 H70B 111.9 . . ?
C69 C70 H70B 111.9 . . ?
H70A C70 H70B 109.6 . . ?
C72 C71 C70 100(4) . . ?
C72 C71 H71A 111.8 . . ?
C70 C71 H71A 111.8 . . ?
C72 C71 H71B 111.8 . . ?
C70 C71 H71B 111.8 . . ?
H71A C71 H71B 109.5 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N12 C69' C70' 123.4(11) . . ?
N12 C69' H69C 106.5 . . ?
C70' C69' H69C 106.5 . . ?
N12 C69' H69D 106.5 . . ?
C70' C69' H69D 106.5 . . ?
H69C C69' H69D 106.5 . . ?
C71' C70' C69' 115.1(12) . . ?
C71' C70' H70C 108.5 . . ?
C69' C70' H70C 108.5 . . ?
C71' C70' H70D 108.5 . . ?
C69' C70' H70D 108.5 . . ?
H70C C70' H70D 107.5 . . ?
C72' C71' C70' 118.2(13) . . ?
C72' C71' H71C 107.8 . . ?
C70' C71' H71C 107.8 . . ?
C72' C71' H71D 107.8 . . ?
C70' C71' H71D 107.8 . . ?
H71C C71' H71D 107.1 . . ?
C71' C72' H72D 109.5 . . ?
C71' C72' H72E 109.5 . . ?
H72D C72' H72E 109.5 . . ?
C71' C72' H72F 109.5 . . ?
H72D C72' H72F 109.5 . . ?
H72E C72' H72F 109.5 . . ?
N12 C77 C78 108.7(11) . . ?
N12 C77 H77A 110.0 . . ?
C78 C77 H77A 110.0 . . ?
N12 C77 H77B 110.0 . . ?
C78 C77 H77B 110.0 . . ?
H77A C77 H77B 108.3 . . ?
C77 C78 C79 106.5(12) . . ?
C77 C78 H78A 110.4 . . ?
C79 C78 H78A 110.4 . . ?
C77 C78 H78B 110.4 . . ?
C79 C78 H78B 110.4 . . ?
H78A C78 H78B 108.6 . . ?
C80 C79 C78 90.6(16) . . ?
C80 C79 H79A 113.5 . . ?
C78 C79 H79A 113.5 . . ?
C80 C79 H79B 113.5 . . ?
C78 C79 H79B 113.5 . . ?
H79A C79 H79B 110.8 . . ?
C79 C80 H80A 109.5 . . ?
C79 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
C79 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C82 C81 N11 115.2(9) . . ?
C82 C81 H81A 108.5 . . ?
N11 C81 H81A 108.5 . . ?
C82 C81 H81B 108.5 . . ?
N11 C81 H81B 108.5 . . ?
H81A C81 H81B 107.5 . . ?
C81 C82 C83 110.5(9) . . ?
C81 C82 H82A 109.5 . . ?
C83 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
C83 C82 H82B 109.5 . . ?
H82A C82 H82B 108.1 . . ?
C84 C83 C82 112.0(9) . . ?
C84 C83 H83A 109.2 . . ?
C82 C83 H83A 109.2 . . ?
C84 C83 H83B 109.2 . . ?
C82 C83 H83B 109.2 . . ?
H83A C83 H83B 107.9 . . ?
C83 C84 H84A 109.5 . . ?
C83 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C83 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
N11 C85 C86 115.3(8) . . ?
N11 C85 H85A 108.5 . . ?
C86 C85 H85A 108.5 . . ?
N11 C85 H85B 108.5 . . ?
C86 C85 H85B 108.5 . . ?
H85A C85 H85B 107.5 . . ?
C85 C86 C87 109.9(10) . . ?
C85 C86 H86A 109.7 . . ?
C87 C86 H86A 109.7 . . ?
C85 C86 H86B 109.7 . . ?
C87 C86 H86B 109.7 . . ?
H86A C86 H86B 108.2 . . ?
C88 C87 C86 113.0(11) . . ?
C88 C87 H87A 109.0 . . ?
C86 C87 H87A 109.0 . . ?
C88 C87 H87B 109.0 . . ?
C86 C87 H87B 109.0 . . ?
H87A C87 H87B 107.8 . . ?
C87 C88 H88A 109.5 . . ?
C87 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C87 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
N11 C89 C90 121.5(9) . . ?
N11 C89 H89A 106.9 . . ?
C90 C89 H89A 106.9 . . ?
N11 C89 H89B 106.9 . . ?
C90 C89 H89B 106.9 . . ?
H89A C89 H89B 106.7 . . ?
C91 C90 C89 111.4(10) . . ?
C91 C90 H90A 109.3 . . ?
C89 C90 H90A 109.3 . . ?
C91 C90 H90B 109.3 . . ?
C89 C90 H90B 109.3 . . ?
H90A C90 H90B 108.0 . . ?
C90 C91 C92 112.0(9) . . ?
C90 C91 H91A 109.2 . . ?
C92 C91 H91A 109.2 . . ?
C90 C91 H91B 109.2 . . ?
C92 C91 H91B 109.2 . . ?
H91A C91 H91B 107.9 . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
N11 C93 C94 115.8(8) . . ?
N11 C93 H93A 108.3 . . ?
C94 C93 H93A 108.3 . . ?
N11 C93 H93B 108.3 . . ?
C94 C93 H93B 108.3 . . ?
H93A C93 H93B 107.4 . . ?
C95 C94 C93 111.1(9) . . ?
C95 C94 H94A 109.4 . . ?
C93 C94 H94A 109.4 . . ?
C95 C94 H94B 109.4 . . ?
C93 C94 H94B 109.4 . . ?
H94A C94 H94B 108.0 . . ?
C94 C95 C96 114.4(11) . . ?
C94 C95 H95A 108.7 . . ?
C96 C95 H95A 108.7 . . ?
C94 C95 H95B 108.7 . . ?
C96 C95 H95B 108.7 . . ?
H95A C95 H95B 107.6 . . ?
C95 C96 H96A 109.5 . . ?
C95 C96 H96B 109.5 . . ?
H96A C96 H96B 109.5 . . ?
C95 C96 H96C 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
C1 N1 C10 127.4(7) . . ?
C1 N1 Ni1 116.7(5) . . ?
C10 N1 Ni1 115.9(4) . . ?
C2 N2 C12 112.7(7) . . ?
C2 N2 Ni1 115.8(6) . . ?
C12 N2 Ni1 130.8(5) . . ?
C3 N3 C5 128.6(8) . . ?
C3 N3 Ni1 114.9(8) . . ?
C5 N3 Ni1 116.4(4) . . ?
C4 N4 C11 121.2(12) . . ?
C4 N4 C11' 114(3) . . ?
C11 N4 C11' 8(4) . . ?
C4 N4 Ni1 109.1(9) . . ?
C11 N4 Ni1 129.7(8) . . ?
C11' N4 Ni1 137(3) . . ?
C17 N5 C26 133.0(6) . . ?
C17 N5 Ni2 112.8(6) . . ?
C26 N5 Ni2 114.1(4) . . ?
C18 N6 C30 110.0(7) . . ?
C18 N6 Ni2 114.4(5) . . ?
C30 N6 Ni2 133.8(6) . . ?
C74 C73 N12 123.8(14) . . ?
C74 C73 H73A 106.4 . . ?
N12 C73 H73A 106.4 . . ?
C74 C73 H73B 106.4 . . ?
N12 C73 H73B 106.4 . . ?
H73A C73 H73B 106.4 . . ?
C73 C74 C75 119.6(16) . . ?
C73 C74 H74A 107.4 . . ?
C75 C74 H74A 107.4 . . ?
C73 C74 H74B 107.4 . . ?
C75 C74 H74B 107.4 . . ?
H74A C74 H74B 107.0 . . ?
C76 C75 C74 115.3(13) . . ?
C76 C75 H75A 108.5 . . ?
C74 C75 H75A 108.5 . . ?
C76 C75 H75B 108.5 . . ?
C74 C75 H75B 108.5 . . ?
H75A C75 H75B 107.5 . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
N12 C73' C74' 110(3) . . ?
N12 C73' H73C 109.7 . . ?
C74' C73' H73C 109.7 . . ?
N12 C73' H73D 109.7 . . ?
C74' C73' H73D 109.7 . . ?
H73C C73' H73D 108.2 . . ?
C73' C74' C75' 102.6(18) . . ?
C73' C74' H74C 111.3 . . ?
C75' C74' H74C 111.2 . . ?
C73' C74' H74D 111.2 . . ?
C75' C74' H74D 111.3 . . ?
H74C C74' H74D 109.2 . . ?
C76' C75' C74' 107.1(14) . . ?
C76' C75' H75C 110.3 . . ?
C74' C75' H75C 110.3 . . ?
C76' C75' H75D 110.3 . . ?
C74' C75' H75D 110.3 . . ?
H75C C75' H75D 108.5 . . ?
C75' C76' H76D 109.5 . . ?
C75' C76' H76E 109.5 . . ?
H76D C76' H76E 109.5 . . ?
C75' C76' H76F 109.5 . . ?
H76D C76' H76F 109.5 . . ?
H76E C76' H76F 109.5 . . ?
C20 N8 C27 119.6(7) . . ?
C20 N8 Ni2 109.6(6) . . ?
C27 N8 Ni2 130.7(6) . . ?
C45 N9 C33 110.7(6) . . ?
C45 N9 C37 105.4(5) . . ?
C33 N9 C37 111.2(6) . . ?
C45 N9 C41 112.1(5) . . ?
C33 N9 C41 108.1(5) . . ?
C37 N9 C41 109.3(5) . . ?
C57 N10 C49 111.8(7) . . ?
C57 N10 C53 104.5(6) . . ?
C49 N10 C53 110.6(6) . . ?
C57 N10 C61 112.7(7) . . ?
C49 N10 C61 105.3(5) . . ?
C53 N10 C61 112.0(7) . . ?
C89 N11 C93 112.5(7) . . ?
C89 N11 C85 109.2(8) . . ?
C93 N11 C85 110.4(7) . . ?
C89 N11 C81 109.4(7) . . ?
C93 N11 C81 104.9(8) . . ?
C85 N11 C81 110.3(7) . . ?
C69 N12 C73' 93(2) . . ?
C69 N12 C77 116(2) . . ?
C73' N12 C77 99(2) . . ?
C69 N12 C73 96.8(15) . . ?
C73' N12 C73 16(2) . . ?
C77 N12 C73 111.0(12) . . ?
C69 N12 C69' 21.0(13) . . ?
C73' N12 C69' 113.6(19) . . ?
C77 N12 C69' 113.2(12) . . ?
C73 N12 C69' 115.7(12) . . ?
C69 N12 C65 123.1(19) . . ?
C73' N12 C65 121(2) . . ?
C77 N12 C65 102.8(8) . . ?
C73 N12 C65 106.8(10) . . ?
C69' N12 C65 106.2(11) . . ?
N1 Ni1 N2 83.6(3) . . ?
N1 Ni1 N3 82.4(3) . . ?
N2 Ni1 N3 166.0(3) . . ?
N1 Ni1 N4 168.7(3) . . ?
N2 Ni1 N4 107.7(3) . . ?
N3 Ni1 N4 86.3(4) . . ?
N7 Ni2 N5 84.2(3) . . ?
N7 Ni2 N6 169.9(3) . . ?
N5 Ni2 N6 85.8(3) . . ?
N7 Ni2 N8 85.2(3) . . ?
N5 Ni2 N8 168.8(3) . . ?
N6 Ni2 N8 104.8(3) . . ?
C21 N7 C19 131.9(8) . . ?
C21 N7 Ni2 113.5(5) . . ?
C19 N7 Ni2 114.1(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
O1 C1 C2 O2 2.5(10) . . . . ?
N1 C1 C2 O2 -174.0(6) . . . . ?
O1 C1 C2 N2 -176.3(7) . . . . ?
N1 C1 C2 N2 7.2(9) . . . . ?
O3 C3 C4 O4 3(2) . . . . ?
N3 C3 C4 O4 -171.4(11) . . . . ?
O3 C3 C4 N4 178.4(11) . . . . ?
N3 C3 C4 N4 4.0(15) . . . . ?
N3 C5 C6 C7 177.3(6) . . . . ?
C10 C5 C6 C7 0.0 . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C8 C9 C10 C5 0.0 . . . . ?
C8 C9 C10 N1 -179.4(5) . . . . ?
N3 C5 C10 C9 -177.7(5) . . . . ?
C6 C5 C10 C9 0.0 . . . . ?
N3 C5 C10 N1 1.8(5) . . . . ?
C6 C5 C10 N1 179.5(4) . . . . ?
N4 C11 C13 C14 179.0(13) . . . . ?
N4 C11' C13' C14' -154(7) . . . . ?
N2 C12 C15 C16 -177.7(7) . . . . ?
O5 C17 C18 O6 -13.9(12) . . . . ?
N5 C17 C18 O6 168.9(7) . . . . ?
O5 C17 C18 N6 168.2(7) . . . . ?
N5 C17 C18 N6 -9.0(10) . . . . ?
O7 C19 C20 O8 -12.8(17) . . . . ?
N7 C19 C20 O8 167.5(9) . . . . ?
O7 C19 C20 N8 177.1(10) . . . . ?
N7 C19 C20 N8 -2.7(13) . . . . ?
N7 C21 C22 C23 175.9(7) . . . . ?
C26 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C24 0.0 . . . . ?
C22 C23 C24 C25 0.0 . . . . ?
C23 C24 C25 C26 0.0 . . . . ?
C24 C25 C26 N5 -178.9(7) . . . . ?
C24 C25 C26 C21 0.0 . . . . ?
N7 C21 C26 N5 2.8(6) . . . . ?
C22 C21 C26 N5 179.1(6) . . . . ?
N7 C21 C26 C25 -176.3(6) . . . . ?
C22 C21 C26 C25 0.0 . . . . ?
N8 C27 C28 C29 177.5(12) . . . . ?
N6 C30 C31 C32 -179.8(12) . . . . ?
N9 C33 C34 C35 -175.7(9) . . . . ?
C33 C34 C35 C36 73.7(17) . . . . ?
N9 C37 C38 C39 166.6(6) . . . . ?
C37 C38 C39 C40 -75.7(10) . . . . ?
N9 C41 C42 C43 178.8(6) . . . . ?
C41 C42 C43 C44 -175.6(7) . . . . ?
N9 C45 C46 C47 -166.4(9) . . . . ?
C45 C46 C47 C48 97(2) . . . . ?
N10 C49 C50 C51 -178.7(10) . . . . ?
C49 C50 C51 C52 108(3) . . . . ?
N10 C53 C54 C55 175.1(6) . . . . ?
C53 C54 C55 C56 177.7(7) . . . . ?
N10 C57 C58 C59 173.6(15) . . . . ?
N10 C57 C58 C59' 177.6(13) . . . . ?
C57 C58 C59 C60 72(3) . . . . ?
C59' C58 C59 C60 60(6) . . . . ?
C57 C58 C59' C60' 166.6(18) . . . . ?
C59 C58 C59' C60' -25(5) . . . . ?
N10 C61 C62 C63 -172.4(8) . . . . ?
C61 C62 C63 C64 -175.6(8) . . . . ?
N12 C65 C66 C67 168.7(15) . . . . ?
C65 C66 C67 C68 -178.0(18) . . . . ?
N12 C69 C70 C71 -172(3) . . . . ?
C69 C70 C71 C72 -174(3) . . . . ?
N12 C69' C70' C71' 171.3(12) . . . . ?
C69' C70' C71' C72' 179.9(14) . . . . ?
N12 C77 C78 C79 167.6(15) . . . . ?
C77 C78 C79 C80 79(2) . . . . ?
N11 C81 C82 C83 -178.6(8) . . . . ?
C81 C82 C83 C84 -173.9(9) . . . . ?
N11 C85 C86 C87 -178.3(7) . . . . ?
C85 C86 C87 C88 -176.1(9) . . . . ?
N11 C89 C90 C91 -178.0(9) . . . . ?
C89 C90 C91 C92 -176.4(10) . . . . ?
N11 C93 C94 C95 171.4(8) . . . . ?
C93 C94 C95 C96 175.4(9) . . . . ?
O1 C1 N1 C10 -0.2(10) . . . . ?
C2 C1 N1 C10 176.2(5) . . . . ?
O1 C1 N1 Ni1 177.1(5) . . . . ?
C2 C1 N1 Ni1 -6.6(7) . . . . ?
C9 C10 N1 C1 -5.5(8) . . . . ?
C5 C10 N1 C1 175.1(5) . . . . ?
C9 C10 N1 Ni1 177.3(3) . . . . ?
C5 C10 N1 Ni1 -2.2(4) . . . . ?
O2 C2 N2 C12 -11.5(13) . . . . ?
C1 C2 N2 C12 167.1(7) . . . . ?
O2 C2 N2 Ni1 176.7(6) . . . . ?
C1 C2 N2 Ni1 -4.7(9) . . . . ?
C15 C12 N2 C2 88.4(9) . . . . ?
C15 C12 N2 Ni1 -101.3(9) . . . . ?
O3 C3 N3 C5 6(2) . . . . ?
C4 C3 N3 C5 179.6(8) . . . . ?
O3 C3 N3 Ni1 -179.6(11) . . . . ?
C4 C3 N3 Ni1 -5.7(12) . . . . ?
C6 C5 N3 C3 -3.6(12) . . . . ?
C10 C5 N3 C3 173.9(9) . . . . ?
C6 C5 N3 Ni1 -178.2(3) . . . . ?
C10 C5 N3 Ni1 -0.7(7) . . . . ?
O4 C4 N4 C11 -2.2(16) . . . . ?
C3 C4 N4 C11 -178.1(12) . . . . ?
O4 C4 N4 C11' -6(3) . . . . ?
C3 C4 N4 C11' 178(3) . . . . ?
O4 C4 N4 Ni1 175.4(8) . . . . ?
C3 C4 N4 Ni1 -0.5(12) . . . . ?
C13 C11 N4 C4 88.2(15) . . . . ?
C13 C11 N4 C11' 116(23) . . . . ?
C13 C11 N4 Ni1 -88.9(17) . . . . ?
C13' C11' N4 C4 79(7) . . . . ?
C13' C11' N4 C11 -75(22) . . . . ?
C13' C11' N4 Ni1 -104(6) . . . . ?
O5 C17 N5 C26 6.9(14) . . . . ?
C18 C17 N5 C26 -175.9(7) . . . . ?
O5 C17 N5 Ni2 -168.9(6) . . . . ?
C18 C17 N5 Ni2 8.4(9) . . . . ?
C25 C26 N5 C17 1.5(12) . . . . ?
C21 C26 N5 C17 -177.5(8) . . . . ?
C25 C26 N5 Ni2 177.2(4) . . . . ?
C21 C26 N5 Ni2 -1.8(6) . . . . ?
O6 C18 N6 C30 -5.3(14) . . . . ?
C17 C18 N6 C30 172.3(8) . . . . ?
O6 C18 N6 Ni2 -172.3(7) . . . . ?
C17 C18 N6 Ni2 5.3(9) . . . . ?
C31 C30 N6 C18 -80.6(13) . . . . ?
C31 C30 N6 Ni2 82.9(14) . . . . ?
N12 C73 C74 C75 -177.6(13) . . . . ?
C73 C74 C75 C76 -74(2) . . . . ?
N12 C73' C74' C75' 150(4) . . . . ?
C73' C74' C75' C76' -5(6) . . . . ?
O8 C20 N8 C27 1.0(14) . . . . ?
C19 C20 N8 C27 171.0(9) . . . . ?
O8 C20 N8 Ni2 -174.9(8) . . . . ?
C19 C20 N8 Ni2 -4.9(11) . . . . ?
C28 C27 N8 C20 86.1(11) . . . . ?
C28 C27 N8 Ni2 -99.0(10) . . . . ?
C46 C45 N9 C33 66.1(9) . . . . ?
C46 C45 N9 C37 -173.5(8) . . . . ?
C46 C45 N9 C41 -54.7(9) . . . . ?
C34 C33 N9 C45 60.6(10) . . . . ?
C34 C33 N9 C37 -56.2(10) . . . . ?
C34 C33 N9 C41 -176.2(8) . . . . ?
C38 C37 N9 C45 175.4(6) . . . . ?
C38 C37 N9 C33 -64.6(8) . . . . ?
C38 C37 N9 C41 54.7(8) . . . . ?
C42 C41 N9 C45 -56.6(8) . . . . ?
C42 C41 N9 C33 -178.8(6) . . . . ?
C42 C41 N9 C37 60.0(8) . . . . ?
C58 C57 N10 C49 -59.3(9) . . . . ?
C58 C57 N10 C53 -179.0(7) . . . . ?
C58 C57 N10 C61 59.1(9) . . . . ?
C50 C49 N10 C57 -59.3(11) . . . . ?
C50 C49 N10 C53 56.8(11) . . . . ?
C50 C49 N10 C61 178.0(10) . . . . ?
C54 C53 N10 C57 178.9(6) . . . . ?
C54 C53 N10 C49 58.4(8) . . . . ?
C54 C53 N10 C61 -58.8(9) . . . . ?
C62 C61 N10 C57 66.3(10) . . . . ?
C62 C61 N10 C49 -171.6(8) . . . . ?
C62 C61 N10 C53 -51.3(11) . . . . ?
C90 C89 N11 C93 -54.0(12) . . . . ?
C90 C89 N11 C85 -177.0(9) . . . . ?
C90 C89 N11 C81 62.2(11) . . . . ?
C94 C93 N11 C89 -64.3(10) . . . . ?
C94 C93 N11 C85 58.0(10) . . . . ?
C94 C93 N11 C81 176.9(8) . . . . ?
C86 C85 N11 C89 -175.2(8) . . . . ?
C86 C85 N11 C93 60.6(10) . . . . ?
C86 C85 N11 C81 -54.9(10) . . . . ?
C82 C81 N11 C89 63.6(11) . . . . ?
C82 C81 N11 C93 -175.4(9) . . . . ?
C82 C81 N11 C85 -56.5(12) . . . . ?
C70 C69 N12 C73' -159(3) . . . . ?
C70 C69 N12 C77 -57(3) . . . . ?
C70 C69 N12 C73 -175(2) . . . . ?
C70 C69 N12 C69' 30(4) . . . . ?
C70 C69 N12 C65 70(3) . . . . ?
C74' C73' N12 C69 162(4) . . . . ?
C74' C73' N12 C77 46(4) . . . . ?
C74' C73' N12 C73 -93(8) . . . . ?
C74' C73' N12 C69' 166(3) . . . . ?
C74' C73' N12 C65 -65(5) . . . . ?
C78 C77 N12 C69 -25(2) . . . . ?
C78 C77 N12 C73' 73(3) . . . . ?
C78 C77 N12 C73 84(2) . . . . ?
C78 C77 N12 C69' -47.9(19) . . . . ?
C78 C77 N12 C65 -162.0(17) . . . . ?
C74 C73 N12 C69 167(2) . . . . ?
C74 C73 N12 C73' 90(9) . . . . ?
C74 C73 N12 C77 46.1(19) . . . . ?
C74 C73 N12 C69' 176.7(15) . . . . ?
C74 C73 N12 C65 -65.3(19) . . . . ?
C70' C69' N12 C69 -157(6) . . . . ?
C70' C69' N12 C73' -167(3) . . . . ?
C70' C69' N12 C77 -54.8(14) . . . . ?
C70' C69' N12 C73 175.6(12) . . . . ?
C70' C69' N12 C65 57.3(14) . . . . ?
C66 C65 N12 C69 58(3) . . . . ?
C66 C65 N12 C73' -60(3) . . . . ?
C66 C65 N12 C77 -168.9(17) . . . . ?
C66 C65 N12 C73 -52(2) . . . . ?
C66 C65 N12 C69' 72.0(17) . . . . ?
C1 N1 Ni1 N2 3.6(5) . . . . ?
C10 N1 Ni1 N2 -178.9(5) . . . . ?
C1 N1 Ni1 N3 -176.2(5) . . . . ?
C10 N1 Ni1 N3 1.4(4) . . . . ?
C1 N1 Ni1 N4 -174.4(16) . . . . ?
C10 N1 Ni1 N4 3.1(19) . . . . ?
C2 N2 Ni1 N1 1.0(7) . . . . ?
C12 N2 Ni1 N1 -169.0(9) . . . . ?
C2 N2 Ni1 N3 2(2) . . . . ?
C12 N2 Ni1 N3 -167.9(13) . . . . ?
C2 N2 Ni1 N4 -179.4(7) . . . . ?
C12 N2 Ni1 N4 10.6(10) . . . . ?
C3 N3 Ni1 N1 -175.8(8) . . . . ?
C5 N3 Ni1 N1 -0.4(5) . . . . ?
C3 N3 Ni1 N2 -176.9(13) . . . . ?
C5 N3 Ni1 N2 -1.5(19) . . . . ?
C3 N3 Ni1 N4 4.6(8) . . . . ?
C5 N3 Ni1 N4 180.0(6) . . . . ?
C4 N4 Ni1 N1 -4(2) . . . . ?
C11 N4 Ni1 N1 173.5(15) . . . . ?
C11' N4 Ni1 N1 179(4) . . . . ?
C4 N4 Ni1 N2 178.3(7) . . . . ?
C11 N4 Ni1 N2 -4.4(12) . . . . ?
C11' N4 Ni1 N2 1(4) . . . . ?
C4 N4 Ni1 N3 -2.1(8) . . . . ?
C11 N4 Ni1 N3 175.3(12) . . . . ?
C11' N4 Ni1 N3 -180(4) . . . . ?
C17 N5 Ni2 N7 176.9(6) . . . . ?
C26 N5 Ni2 N7 0.3(6) . . . . ?
C17 N5 Ni2 N6 -4.5(6) . . . . ?
C26 N5 Ni2 N6 178.9(5) . . . . ?
C17 N5 Ni2 N8 157.7(16) . . . . ?
C26 N5 Ni2 N8 -19(2) . . . . ?
C18 N6 Ni2 N7 8(2) . . . . ?
C30 N6 Ni2 N7 -155.4(18) . . . . ?
C18 N6 Ni2 N5 -0.7(6) . . . . ?
C30 N6 Ni2 N5 -163.7(10) . . . . ?
C18 N6 Ni2 N8 -177.2(6) . . . . ?
C30 N6 Ni2 N8 19.8(10) . . . . ?
C20 N8 Ni2 N7 8.1(7) . . . . ?
C27 N8 Ni2 N7 -167.3(9) . . . . ?
C20 N8 Ni2 N5 27(2) . . . . ?
C27 N8 Ni2 N5 -148.1(15) . . . . ?
C20 N8 Ni2 N6 -171.1(6) . . . . ?
C27 N8 Ni2 N6 13.6(9) . . . . ?
C22 C21 N7 C19 10.6(13) . . . . ?
C26 C21 N7 C19 -173.3(9) . . . . ?
C22 C21 N7 Ni2 -178.6(4) . . . . ?
C26 C21 N7 Ni2 -2.6(7) . . . . ?
O7 C19 N7 C21 0.5(17) . . . . ?
C20 C19 N7 C21 -179.7(9) . . . . ?
O7 C19 N7 Ni2 -170.2(8) . . . . ?
C20 C19 N7 Ni2 9.5(11) . . . . ?
N5 Ni2 N7 C21 1.3(6) . . . . ?
N6 Ni2 N7 C21 -7(2) . . . . ?
N8 Ni2 N7 C21 177.6(6) . . . . ?
N5 Ni2 N7 C19 173.7(8) . . . . ?
N6 Ni2 N7 C19 165.4(17) . . . . ?
N8 Ni2 N7 C19 -9.9(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        61.98
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         1.638
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.081
####################################################################### 
# 
# 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_meva13
_database_code_depnum_ccdc_archive 'CCDC 1035430'
_audit_update_record             
;
2014-11-21 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H10 Cu N4 O4, 2(C16 H36 N)'

_chemical_formula_sum            'C44 H82 Cu N6 O4'
_chemical_formula_weight         822.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5836(13)
_cell_length_b                   14.534(3)
_cell_length_c                   15.6095(15)
_cell_angle_alpha                98.444(11)
_cell_angle_beta                 91.564(9)
_cell_angle_gamma                102.014(12)
_cell_volume                     2318.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    8005
_cell_measurement_theta_min      3.9064
_cell_measurement_theta_max      60.4463


_exptl_crystal_description       needle
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             898
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_min  0.51172
_exptl_absorpt_correction_T_max  1.22941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  10
_diffrn_standards_decay_%        0

_diffrn_reflns_number            17586
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.91
_diffrn_reflns_theta_max         60.63
_reflns_number_total             6824
_reflns_number_gt                5099
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2sigma(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)+(0.0596P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6824
_refine_ls_number_parameters     496
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0892
_refine_ls_wR_factor_gt          0.0850
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_restrained_S_all      0.939
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.30590(3) 0.21341(2) 0.806793(18) 0.02613(10) Uani 1 1 d . . .
O3 O 0.55286(15) 0.13812(11) 0.63288(10) 0.0397(4) Uani 1 1 d . . .
C4 C 0.4230(2) 0.06656(15) 0.74133(14) 0.0318(5) Uani 1 1 d . . .
O4 O 0.46538(15) -0.00807(10) 0.72767(10) 0.0413(4) Uani 1 1 d . . .
O1 O 0.20722(14) 0.46806(10) 0.84283(10) 0.0359(4) Uani 1 1 d . . .
N2 N 0.19298(16) 0.23863(12) 0.90030(10) 0.0283(4) Uani 1 1 d . . .
O2 O 0.07217(14) 0.34843(11) 0.94834(9) 0.0325(4) Uani 1 1 d . . .
N3 N 0.42532(16) 0.22394(12) 0.71500(10) 0.0256(4) Uani 1 1 d . . .
N5 N 0.78630(16) 0.43024(11) 0.85363(10) 0.0252(4) Uani 1 1 d . . .
N1 N 0.29942(16) 0.34165(11) 0.78917(11) 0.0254(4) Uani 1 1 d . . .
N4 N 0.33310(17) 0.08344(12) 0.79596(11) 0.0294(4) Uani 1 1 d . . .
N6 N 0.30279(16) 0.13641(12) 0.38819(10) 0.0262(4) Uani 1 1 d . . .
C17 C 0.91022(19) 0.50678(14) 0.87704(13) 0.0255(5) Uani 1 1 d . . .
H17A H 0.9076 0.5370 0.9365 0.031 Uiso 1 1 calc R . .
H17B H 0.9833 0.4760 0.8746 0.031 Uiso 1 1 calc R . .
C43 C 0.2680(2) -0.05747(15) 0.53925(14) 0.0323(5) Uani 1 1 d . . .
H43A H 0.2762 -0.1090 0.4941 0.039 Uiso 1 1 calc R . .
H43B H 0.3509 -0.0346 0.5716 0.039 Uiso 1 1 calc R . .
C13 C 0.66809(19) 0.47409(14) 0.84861(13) 0.0279(5) Uani 1 1 d . . .
H13A H 0.6734 0.5073 0.7988 0.033 Uiso 1 1 calc R . .
H13B H 0.5914 0.4231 0.8387 0.033 Uiso 1 1 calc R . .
C41 C 0.3408(2) 0.06803(15) 0.44525(13) 0.0292(5) Uani 1 1 d . . .
H41A H 0.3700 0.0177 0.4085 0.035 Uiso 1 1 calc R . .
H41B H 0.4131 0.1025 0.4848 0.035 Uiso 1 1 calc R . .
C14 C 0.6515(2) 0.54331(16) 0.92855(13) 0.0310(5) Uani 1 1 d . . .
H14A H 0.7329 0.5883 0.9451 0.037 Uiso 1 1 calc R . .
H14B H 0.6289 0.5084 0.9763 0.037 Uiso 1 1 calc R . .
C32 C 0.1270(2) 0.44099(15) 0.42896(14) 0.0349(5) Uani 1 1 d . . .
H32A H 0.0983 0.4834 0.4736 0.052 Uiso 1 1 calc R . .
H32B H 0.0566 0.4123 0.3870 0.052 Uiso 1 1 calc R . .
H32C H 0.1967 0.4761 0.4010 0.052 Uiso 1 1 calc R . .
C23 C 0.8959(2) 0.26749(15) 0.66163(13) 0.0331(5) Uani 1 1 d . . .
H23A H 0.8155 0.2200 0.6528 0.040 Uiso 1 1 calc R . .
H23B H 0.8952 0.3100 0.6192 0.040 Uiso 1 1 calc R . .
C30 C 0.2209(2) 0.29304(14) 0.40248(13) 0.0301(5) Uani 1 1 d . . .
H30A H 0.2963 0.3255 0.3765 0.036 Uiso 1 1 calc R . .
H30B H 0.1538 0.2662 0.3568 0.036 Uiso 1 1 calc R . .
C37 C 0.1949(2) 0.08398(15) 0.32071(13) 0.0292(5) Uani 1 1 d . . .
H37A H 0.1146 0.0711 0.3496 0.035 Uiso 1 1 calc R . .
H37B H 0.1847 0.1258 0.2791 0.035 Uiso 1 1 calc R . .
C1 C 0.22458(19) 0.38599(15) 0.84010(13) 0.0273(5) Uani 1 1 d . . .
C44 C 0.1662(2) -0.09436(16) 0.59971(15) 0.0398(6) Uani 1 1 d . . .
H44A H 0.1910 -0.1448 0.6250 0.060 Uiso 1 1 calc R . .
H44B H 0.0844 -0.1180 0.5676 0.060 Uiso 1 1 calc R . .
H44C H 0.1589 -0.0436 0.6449 0.060 Uiso 1 1 calc R . .
C21 C 0.7909(2) 0.37283(15) 0.76477(13) 0.0287(5) Uani 1 1 d . . .
H21A H 0.7116 0.3245 0.7531 0.034 Uiso 1 1 calc R . .
H21B H 0.7927 0.4149 0.7218 0.034 Uiso 1 1 calc R . .
C10 C 0.44473(19) 0.31048(14) 0.68215(13) 0.0260(5) Uani 1 1 d . . .
C6 C 0.3855(2) 0.46514(14) 0.69745(13) 0.0295(5) Uani 1 1 d . . .
H10 H 0.3391 0.5082 0.7239 0.035 Uiso 1 1 calc R . .
C15 C 0.5460(2) 0.59781(16) 0.91199(14) 0.0332(5) Uani 1 1 d . . .
H15A H 0.4686 0.5526 0.8867 0.040 Uiso 1 1 calc R . .
H15B H 0.5249 0.6297 0.9671 0.040 Uiso 1 1 calc R . .
C42 C 0.2321(2) 0.02302(16) 0.49794(14) 0.0339(5) Uani 1 1 d . . .
H42A H 0.2142 0.0713 0.5430 0.041 Uiso 1 1 calc R . .
H42B H 0.1542 -0.0016 0.4604 0.041 Uiso 1 1 calc R . .
C22 C 0.9043(2) 0.32438(15) 0.75281(13) 0.0298(5) Uani 1 1 d . . .
H22A H 0.9042 0.2821 0.7954 0.036 Uiso 1 1 calc R . .
H22B H 0.9846 0.3720 0.7619 0.036 Uiso 1 1 calc R . .
C25 C 0.77670(19) 0.36811(14) 0.92460(13) 0.0267(5) Uani 1 1 d . . .
H25A H 0.8576 0.3474 0.9297 0.032 Uiso 1 1 calc R . .
H25B H 0.7676 0.4071 0.9792 0.032 Uiso 1 1 calc R . .
C8 C 0.5350(2) 0.42602(16) 0.59210(13) 0.0330(5) Uani 1 1 d . . .
H8 H 0.5883 0.4433 0.5482 0.040 Uiso 1 1 calc R . .
C26 C 0.6670(2) 0.28057(15) 0.91219(13) 0.0310(5) Uani 1 1 d . . .
H26A H 0.6768 0.2387 0.8595 0.037 Uiso 1 1 calc R . .
H26B H 0.5849 0.2995 0.9064 0.037 Uiso 1 1 calc R . .
C33 C 0.41849(19) 0.17689(15) 0.33966(13) 0.0276(5) Uani 1 1 d . . .
H33A H 0.4468 0.1242 0.3058 0.033 Uiso 1 1 calc R . .
H33B H 0.3902 0.2142 0.2992 0.033 Uiso 1 1 calc R . .
C19 C 1.0555(2) 0.65782(15) 0.85271(14) 0.0314(5) Uani 1 1 d . . .
H19A H 1.1304 0.6301 0.8414 0.038 Uiso 1 1 calc R . .
H19B H 1.0539 0.6754 0.9150 0.038 Uiso 1 1 calc R . .
C27 C 0.6680(2) 0.22788(15) 0.98969(15) 0.0364(5) Uani 1 1 d . . .
H27A H 0.6649 0.2716 1.0425 0.044 Uiso 1 1 calc R . .
H27B H 0.7482 0.2059 0.9929 0.044 Uiso 1 1 calc R . .
C9 C 0.5258(2) 0.33636(15) 0.61667(12) 0.0292(5) Uani 1 1 d . . .
H7 H 0.5731 0.2943 0.5897 0.035 Uiso 1 1 calc R . .
C24 C 1.0090(2) 0.21832(16) 0.64750(14) 0.0364(5) Uani 1 1 d . . .
H24A H 1.0007 0.1835 0.5897 0.055 Uiso 1 1 calc R . .
H24B H 1.0089 0.1752 0.6886 0.055 Uiso 1 1 calc R . .
H24C H 1.0887 0.2652 0.6553 0.055 Uiso 1 1 calc R . .
C7 C 0.4663(2) 0.48906(15) 0.63201(13) 0.0330(5) Uani 1 1 d . . .
H9 H 0.4742 0.5486 0.6149 0.040 Uiso 1 1 calc R . .
C34 C 0.5339(2) 0.23859(15) 0.39455(13) 0.0296(5) Uani 1 1 d . . .
H34A H 0.5679 0.2013 0.4327 0.036 Uiso 1 1 calc R . .
H34B H 0.5075 0.2910 0.4302 0.036 Uiso 1 1 calc R . .
C11 C 0.1356(2) 0.18056(17) 0.96356(15) 0.0420(6) Uani 1 1 d . . .
H11A H 0.1680 0.1231 0.9581 0.063 Uiso 0.50 1 calc PR . .
H11B H 0.0432 0.1648 0.9533 0.063 Uiso 0.50 1 calc PR . .
H11C H 0.1577 0.2155 1.0210 0.063 Uiso 0.50 1 calc PR . .
H11D H 0.0780 0.2125 0.9969 0.063 Uiso 0.50 1 calc PR . .
H11E H 0.2027 0.1708 1.0016 0.063 Uiso 0.50 1 calc PR . .
H11F H 0.0882 0.1201 0.9339 0.063 Uiso 0.50 1 calc PR . .
C29 C 0.2556(2) 0.21384(15) 0.44594(13) 0.0291(5) Uani 1 1 d . . .
H29A H 0.3222 0.2425 0.4916 0.035 Uiso 1 1 calc R . .
H29B H 0.1799 0.1842 0.4734 0.035 Uiso 1 1 calc R . .
C28 C 0.5543(2) 0.14283(17) 0.98397(17) 0.0488(7) Uani 1 1 d . . .
H28A H 0.5588 0.1120 1.0339 0.073 Uiso 1 1 calc R . .
H28B H 0.5579 0.0986 0.9324 0.073 Uiso 1 1 calc R . .
H28C H 0.4746 0.1643 0.9819 0.073 Uiso 1 1 calc R . .
C39 C 0.1278(2) -0.04019(16) 0.18905(14) 0.0399(6) Uani 1 1 d . . .
H39A H 0.1270 -0.1063 0.1671 0.048 Uiso 1 1 calc R . .
H39B H 0.0403 -0.0360 0.2032 0.048 Uiso 1 1 calc R . .
C18 C 0.9334(2) 0.58360(15) 0.81961(13) 0.0319(5) Uani 1 1 d . . .
H18A H 0.8599 0.6138 0.8197 0.038 Uiso 1 1 calc R . .
H18B H 0.9427 0.5553 0.7605 0.038 Uiso 1 1 calc R . .
C12 C 0.2771(2) 0.00540(15) 0.84144(16) 0.0405(6) Uani 1 1 d . . .
H12A H 0.2137 0.0245 0.8790 0.061 Uiso 0.50 1 calc PR . .
H12B H 0.3441 -0.0107 0.8753 0.061 Uiso 0.50 1 calc PR . .
H12C H 0.2365 -0.0490 0.8000 0.061 Uiso 0.50 1 calc PR . .
H12D H 0.3158 -0.0480 0.8238 0.061 Uiso 0.50 1 calc PR . .
H12E H 0.1855 -0.0128 0.8276 0.061 Uiso 0.50 1 calc PR . .
H12F H 0.2930 0.0255 0.9029 0.061 Uiso 0.50 1 calc PR . .
C2 C 0.1553(2) 0.32045(15) 0.90170(13) 0.0279(5) Uani 1 1 d . . .
C16 C 0.5850(2) 0.67134(16) 0.85216(15) 0.0394(6) Uani 1 1 d . . .
H16A H 0.5153 0.7029 0.8444 0.059 Uiso 1 1 calc R . .
H16B H 0.6041 0.6402 0.7969 0.059 Uiso 1 1 calc R . .
H16C H 0.6604 0.7174 0.8774 0.059 Uiso 1 1 calc R . .
C36 C 0.7557(2) 0.34385(17) 0.38687(16) 0.0450(6) Uani 1 1 d . . .
H36A H 0.8187 0.3664 0.3474 0.068 Uiso 1 1 calc R . .
H36B H 0.7931 0.3100 0.4257 0.068 Uiso 1 1 calc R . .
H36C H 0.7291 0.3970 0.4197 0.068 Uiso 1 1 calc R . .
C20 C 1.0691(2) 0.74709(16) 0.81029(15) 0.0409(6) Uani 1 1 d . . .
H20A H 1.1472 0.7916 0.8332 0.061 Uiso 1 1 calc R . .
H20B H 0.9961 0.7755 0.8223 0.061 Uiso 1 1 calc R . .
H20C H 1.0727 0.7304 0.7487 0.061 Uiso 1 1 calc R . .
C31 C 0.1736(2) 0.36356(15) 0.46905(14) 0.0331(5) Uani 1 1 d . . .
H31A H 0.2434 0.3932 0.5122 0.040 Uiso 1 1 calc R . .
H31B H 0.1033 0.3294 0.4983 0.040 Uiso 1 1 calc R . .
C35 C 0.6387(2) 0.27745(16) 0.33584(15) 0.0352(5) Uani 1 1 d . . .
H35A H 0.6665 0.2246 0.3019 0.042 Uiso 1 1 calc R . .
H35B H 0.6025 0.3116 0.2959 0.042 Uiso 1 1 calc R . .
C40 C 0.1682(3) 0.01904(18) 0.11845(16) 0.0575(8) Uani 1 1 d . . .
H40A H 0.1091 -0.0038 0.0684 0.086 Uiso 1 1 calc R . .
H40B H 0.2540 0.0141 0.1030 0.086 Uiso 1 1 calc R . .
H40C H 0.1671 0.0844 0.1391 0.086 Uiso 1 1 calc R . .
C38 C 0.2162(2) -0.00938(15) 0.27146(14) 0.0342(5) Uani 1 1 d . . .
H38A H 0.1989 -0.0583 0.3082 0.041 Uiso 1 1 calc R . .
H38B H 0.3057 -0.0017 0.2565 0.041 Uiso 1 1 calc R . .
C5 C 0.37420(19) 0.37579(14) 0.72331(12) 0.0251(5) Uani 1 1 d . . .
C3 C 0.4753(2) 0.14853(15) 0.69003(13) 0.0298(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
Cu1 N3 1.9382(17) . ?
Cu1 N1 1.9383(16) . ?
Cu1 N2 1.9528(17) . ?
Cu1 N4 1.9531(17) . ?
O3 C3 1.243(2) . ?
C4 O4 1.250(3) . ?
C4 N4 1.332(3) . ?
C4 C3 1.548(3) . ?
O1 C1 1.239(2) . ?
N2 C2 1.328(3) . ?
N2 C11 1.456(3) . ?
O2 C2 1.251(2) . ?
N3 C3 1.326(3) . ?
N3 C10 1.405(3) . ?
N5 C21 1.518(2) . ?
N5 C25 1.521(3) . ?
N5 C13 1.523(3) . ?
N5 C17 1.529(2) . ?
N1 C1 1.331(3) . ?
N1 C5 1.400(3) . ?
N4 C12 1.457(3) . ?
N6 C29 1.513(3) . ?
N6 C33 1.517(3) . ?
N6 C37 1.527(2) . ?
N6 C41 1.533(2) . ?
C17 C18 1.517(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C43 C44 1.517(3) . ?
C43 C42 1.523(3) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C13 C14 1.522(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C41 C42 1.524(3) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C14 C15 1.534(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C32 C31 1.524(3) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C23 C24 1.522(3) . ?
C23 C22 1.528(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C30 C31 1.520(3) . ?
C30 C29 1.520(3) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C37 C38 1.521(3) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C1 C2 1.545(3) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C21 C22 1.515(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C10 C9 1.396(3) . ?
C10 C5 1.419(3) . ?
C6 C7 1.388(3) . ?
C6 C5 1.398(3) . ?
C6 H10 0.9300 . ?
C15 C16 1.521(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C25 C26 1.518(3) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C8 C7 1.375(3) . ?
C8 C9 1.397(3) . ?
C8 H8 0.9300 . ?
C26 C27 1.525(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C33 C34 1.514(3) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C19 C18 1.523(3) . ?
C19 C20 1.524(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C27 C28 1.525(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C9 H7 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C7 H9 0.9300 . ?
C34 C35 1.528(3) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C11 H11D 0.9600 . ?
C11 H11E 0.9600 . ?
C11 H11F 0.9600 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C39 C40 1.513(3) . ?
C39 C38 1.523(3) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C12 H12D 0.9600 . ?
C12 H12E 0.9600 . ?
C12 H12F 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C36 C35 1.524(3) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?

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
N3 Cu1 N1 82.20(7) . . ?
N3 Cu1 N2 165.05(7) . . ?
N1 Cu1 N2 83.30(7) . . ?
N3 Cu1 N4 83.50(7) . . ?
N1 Cu1 N4 165.23(7) . . ?
N2 Cu1 N4 111.18(7) . . ?
O4 C4 N4 126.3(2) . . ?
O4 C4 C3 119.0(2) . . ?
N4 C4 C3 114.74(18) . . ?
C2 N2 C11 115.01(18) . . ?
C2 N2 Cu1 113.43(14) . . ?
C11 N2 Cu1 131.35(15) . . ?
C3 N3 C10 128.59(18) . . ?
C3 N3 Cu1 116.38(14) . . ?
C10 N3 Cu1 115.00(13) . . ?
C21 N5 C25 111.60(15) . . ?
C21 N5 C13 105.94(14) . . ?
C25 N5 C13 111.09(15) . . ?
C21 N5 C17 111.06(15) . . ?
C25 N5 C17 105.82(14) . . ?
C13 N5 C17 111.44(15) . . ?
C1 N1 C5 128.06(17) . . ?
C1 N1 Cu1 116.66(14) . . ?
C5 N1 Cu1 115.28(13) . . ?
C4 N4 C12 115.86(18) . . ?
C4 N4 Cu1 113.54(14) . . ?
C12 N4 Cu1 130.48(15) . . ?
C29 N6 C33 111.76(16) . . ?
C29 N6 C37 109.22(15) . . ?
C33 N6 C37 107.51(15) . . ?
C29 N6 C41 108.27(15) . . ?
C33 N6 C41 109.37(15) . . ?
C37 N6 C41 110.72(15) . . ?
C18 C17 N5 115.29(16) . . ?
C18 C17 H17A 108.5 . . ?
N5 C17 H17A 108.5 . . ?
C18 C17 H17B 108.5 . . ?
N5 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C44 C43 C42 111.04(18) . . ?
C44 C43 H43A 109.4 . . ?
C42 C43 H43A 109.4 . . ?
C44 C43 H43B 109.4 . . ?
C42 C43 H43B 109.4 . . ?
H43A C43 H43B 108.0 . . ?
C14 C13 N5 115.16(16) . . ?
C14 C13 H13A 108.5 . . ?
N5 C13 H13A 108.5 . . ?
C14 C13 H13B 108.5 . . ?
N5 C13 H13B 108.5 . . ?
H13A C13 H13B 107.5 . . ?
C42 C41 N6 114.28(16) . . ?
C42 C41 H41A 108.7 . . ?
N6 C41 H41A 108.7 . . ?
C42 C41 H41B 108.7 . . ?
N6 C41 H41B 108.7 . . ?
H41A C41 H41B 107.6 . . ?
C13 C14 C15 111.69(17) . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14B 109.3 . . ?
C15 C14 H14B 109.3 . . ?
H14A C14 H14B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C24 C23 C22 111.74(17) . . ?
C24 C23 H23A 109.3 . . ?
C22 C23 H23A 109.3 . . ?
C24 C23 H23B 109.3 . . ?
C22 C23 H23B 109.3 . . ?
H23A C23 H23B 107.9 . . ?
C31 C30 C29 109.85(17) . . ?
C31 C30 H30A 109.7 . . ?
C29 C30 H30A 109.7 . . ?
C31 C30 H30B 109.7 . . ?
C29 C30 H30B 109.7 . . ?
H30A C30 H30B 108.2 . . ?
C38 C37 N6 115.14(16) . . ?
C38 C37 H37A 108.5 . . ?
N6 C37 H37A 108.5 . . ?
C38 C37 H37B 108.5 . . ?
N6 C37 H37B 108.5 . . ?
H37A C37 H37B 107.5 . . ?
O1 C1 N1 128.7(2) . . ?
O1 C1 C2 120.50(18) . . ?
N1 C1 C2 110.79(18) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C22 C21 N5 115.77(16) . . ?
C22 C21 H21A 108.3 . . ?
N5 C21 H21A 108.3 . . ?
C22 C21 H21B 108.3 . . ?
N5 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
C9 C10 N3 126.53(19) . . ?
C9 C10 C5 119.65(19) . . ?
N3 C10 C5 113.81(18) . . ?
C7 C6 C5 119.5(2) . . ?
C7 C6 H10 120.3 . . ?
C5 C6 H10 120.3 . . ?
C16 C15 C14 113.51(19) . . ?
C16 C15 H15A 108.9 . . ?
C14 C15 H15A 108.9 . . ?
C16 C15 H15B 108.9 . . ?
C14 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C43 C42 C41 111.36(18) . . ?
C43 C42 H42A 109.4 . . ?
C41 C42 H42A 109.4 . . ?
C43 C42 H42B 109.4 . . ?
C41 C42 H42B 109.4 . . ?
H42A C42 H42B 108.0 . . ?
C21 C22 C23 110.51(17) . . ?
C21 C22 H22A 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C26 C25 N5 116.28(16) . . ?
C26 C25 H25A 108.2 . . ?
N5 C25 H25A 108.2 . . ?
C26 C25 H25B 108.2 . . ?
N5 C25 H25B 108.2 . . ?
H25A C25 H25B 107.4 . . ?
C7 C8 C9 120.9(2) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C25 C26 C27 109.90(17) . . ?
C25 C26 H26A 109.7 . . ?
C27 C26 H26A 109.7 . . ?
C25 C26 H26B 109.7 . . ?
C27 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
C34 C33 N6 116.34(16) . . ?
C34 C33 H33A 108.2 . . ?
N6 C33 H33A 108.2 . . ?
C34 C33 H33B 108.2 . . ?
N6 C33 H33B 108.2 . . ?
H33A C33 H33B 107.4 . . ?
C18 C19 C20 112.55(18) . . ?
C18 C19 H19A 109.1 . . ?
C20 C19 H19A 109.1 . . ?
C18 C19 H19B 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
C26 C27 C28 112.40(18) . . ?
C26 C27 H27A 109.1 . . ?
C28 C27 H27A 109.1 . . ?
C26 C27 H27B 109.1 . . ?
C28 C27 H27B 109.1 . . ?
H27A C27 H27B 107.9 . . ?
C10 C9 C8 119.3(2) . . ?
C10 C9 H7 120.3 . . ?
C8 C9 H7 120.3 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C8 C7 C6 120.9(2) . . ?
C8 C7 H9 119.5 . . ?
C6 C7 H9 119.5 . . ?
C33 C34 C35 109.70(17) . . ?
C33 C34 H34A 109.7 . . ?
C35 C34 H34A 109.7 . . ?
C33 C34 H34B 109.7 . . ?
C35 C34 H34B 109.7 . . ?
H34A C34 H34B 108.2 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C11 H11D 109.5 . . ?
H11A C11 H11D 141.1 . . ?
H11B C11 H11D 56.3 . . ?
H11C C11 H11D 56.3 . . ?
N2 C11 H11E 109.5 . . ?
H11A C11 H11E 56.3 . . ?
H11B C11 H11E 141.1 . . ?
H11C C11 H11E 56.3 . . ?
H11D C11 H11E 109.5 . . ?
N2 C11 H11F 109.5 . . ?
H11A C11 H11F 56.3 . . ?
H11B C11 H11F 56.3 . . ?
H11C C11 H11F 141.1 . . ?
H11D C11 H11F 109.5 . . ?
H11E C11 H11F 109.5 . . ?
N6 C29 C30 116.67(16) . . ?
N6 C29 H29A 108.1 . . ?
C30 C29 H29A 108.1 . . ?
N6 C29 H29B 108.1 . . ?
C30 C29 H29B 108.1 . . ?
H29A C29 H29B 107.3 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C40 C39 C38 113.4(2) . . ?
C40 C39 H39A 108.9 . . ?
C38 C39 H39A 108.9 . . ?
C40 C39 H39B 108.9 . . ?
C38 C39 H39B 108.9 . . ?
H39A C39 H39B 107.7 . . ?
C17 C18 C19 109.96(16) . . ?
C17 C18 H18A 109.7 . . ?
C19 C18 H18A 109.7 . . ?
C17 C18 H18B 109.7 . . ?
C19 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C12 H12D 109.5 . . ?
H12A C12 H12D 141.1 . . ?
H12B C12 H12D 56.3 . . ?
H12C C12 H12D 56.3 . . ?
N4 C12 H12E 109.5 . . ?
H12A C12 H12E 56.3 . . ?
H12B C12 H12E 141.1 . . ?
H12C C12 H12E 56.3 . . ?
H12D C12 H12E 109.5 . . ?
N4 C12 H12F 109.5 . . ?
H12A C12 H12F 56.3 . . ?
H12B C12 H12F 56.3 . . ?
H12C C12 H12F 141.1 . . ?
H12D C12 H12F 109.5 . . ?
H12E C12 H12F 109.5 . . ?
O2 C2 N2 126.2(2) . . ?
O2 C2 C1 118.68(19) . . ?
N2 C2 C1 115.10(18) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C30 C31 C32 112.88(18) . . ?
C30 C31 H31A 109.0 . . ?
C32 C31 H31A 109.0 . . ?
C30 C31 H31B 109.0 . . ?
C32 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
C36 C35 C34 112.50(19) . . ?
C36 C35 H35A 109.1 . . ?
C34 C35 H35A 109.1 . . ?
C36 C35 H35B 109.1 . . ?
C34 C35 H35B 109.1 . . ?
H35A C35 H35B 107.8 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C37 C38 C39 110.85(18) . . ?
C37 C38 H38A 109.5 . . ?
C39 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 108.1 . . ?
C6 C5 N1 126.52(19) . . ?
C6 C5 C10 119.8(2) . . ?
N1 C5 C10 113.68(18) . . ?
O3 C3 N3 128.3(2) . . ?
O3 C3 C4 120.31(19) . . ?
N3 C3 C4 111.42(18) . . ?

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
N3 Cu1 N2 C2 21.0(4) . . . . ?
N1 Cu1 N2 C2 6.88(14) . . . . ?
N4 Cu1 N2 C2 -170.12(13) . . . . ?
N3 Cu1 N2 C11 -164.5(2) . . . . ?
N1 Cu1 N2 C11 -178.68(19) . . . . ?
N4 Cu1 N2 C11 4.3(2) . . . . ?
N1 Cu1 N3 C3 -179.73(15) . . . . ?
N2 Cu1 N3 C3 166.1(2) . . . . ?
N4 Cu1 N3 C3 -3.45(14) . . . . ?
N1 Cu1 N3 C10 -1.31(13) . . . . ?
N2 Cu1 N3 C10 -15.5(3) . . . . ?
N4 Cu1 N3 C10 174.97(14) . . . . ?
N3 Cu1 N1 C1 -178.92(15) . . . . ?
N2 Cu1 N1 C1 -2.57(14) . . . . ?
N4 Cu1 N1 C1 166.4(2) . . . . ?
N3 Cu1 N1 C5 1.53(13) . . . . ?
N2 Cu1 N1 C5 177.88(14) . . . . ?
N4 Cu1 N1 C5 -13.1(4) . . . . ?
O4 C4 N4 C12 -2.1(3) . . . . ?
C3 C4 N4 C12 176.67(17) . . . . ?
O4 C4 N4 Cu1 174.39(17) . . . . ?
C3 C4 N4 Cu1 -6.9(2) . . . . ?
N3 Cu1 N4 C4 5.78(14) . . . . ?
N1 Cu1 N4 C4 20.4(4) . . . . ?
N2 Cu1 N4 C4 -171.34(13) . . . . ?
N3 Cu1 N4 C12 -178.41(19) . . . . ?
N1 Cu1 N4 C12 -163.8(2) . . . . ?
N2 Cu1 N4 C12 4.5(2) . . . . ?
C21 N5 C17 C18 64.5(2) . . . . ?
C25 N5 C17 C18 -174.24(17) . . . . ?
C13 N5 C17 C18 -53.4(2) . . . . ?
C21 N5 C13 C14 -174.23(17) . . . . ?
C25 N5 C13 C14 64.4(2) . . . . ?
C17 N5 C13 C14 -53.3(2) . . . . ?
C29 N6 C41 C42 57.6(2) . . . . ?
C33 N6 C41 C42 179.64(17) . . . . ?
C37 N6 C41 C42 -62.1(2) . . . . ?
N5 C13 C14 C15 169.43(17) . . . . ?
C29 N6 C37 C38 -166.65(18) . . . . ?
C33 N6 C37 C38 71.9(2) . . . . ?
C41 N6 C37 C38 -47.5(2) . . . . ?
C5 N1 C1 O1 -2.5(3) . . . . ?
Cu1 N1 C1 O1 177.99(17) . . . . ?
C5 N1 C1 C2 177.82(17) . . . . ?
Cu1 N1 C1 C2 -1.7(2) . . . . ?
C25 N5 C21 C22 -60.9(2) . . . . ?
C13 N5 C21 C22 178.10(17) . . . . ?
C17 N5 C21 C22 57.0(2) . . . . ?
C3 N3 C10 C9 -2.2(3) . . . . ?
Cu1 N3 C10 C9 179.63(15) . . . . ?
C3 N3 C10 C5 179.05(18) . . . . ?
Cu1 N3 C10 C5 0.9(2) . . . . ?
C13 C14 C15 C16 -71.4(2) . . . . ?
C44 C43 C42 C41 173.53(18) . . . . ?
N6 C41 C42 C43 169.13(17) . . . . ?
N5 C21 C22 C23 178.78(17) . . . . ?
C24 C23 C22 C21 179.73(18) . . . . ?
C21 N5 C25 C26 -53.8(2) . . . . ?
C13 N5 C25 C26 64.2(2) . . . . ?
C17 N5 C25 C26 -174.75(17) . . . . ?
N5 C25 C26 C27 -178.22(17) . . . . ?
C29 N6 C33 C34 55.6(2) . . . . ?
C37 N6 C33 C34 175.44(17) . . . . ?
C41 N6 C33 C34 -64.3(2) . . . . ?
C25 C26 C27 C28 176.1(2) . . . . ?
N3 C10 C9 C8 -179.36(18) . . . . ?
C5 C10 C9 C8 -0.7(3) . . . . ?
C7 C8 C9 C10 0.5(3) . . . . ?
C9 C8 C7 C6 -0.3(3) . . . . ?
C5 C6 C7 C8 0.3(3) . . . . ?
N6 C33 C34 C35 -177.20(16) . . . . ?
C33 N6 C29 C30 55.7(2) . . . . ?
C37 N6 C29 C30 -63.1(2) . . . . ?
C41 N6 C29 C30 176.24(17) . . . . ?
C31 C30 C29 N6 179.10(18) . . . . ?
N5 C17 C18 C19 176.96(17) . . . . ?
C20 C19 C18 C17 -167.86(18) . . . . ?
C11 N2 C2 O2 -3.8(3) . . . . ?
Cu1 N2 C2 O2 171.57(15) . . . . ?
C11 N2 C2 C1 175.05(17) . . . . ?
Cu1 N2 C2 C1 -9.6(2) . . . . ?
O1 C1 C2 O2 6.7(3) . . . . ?
N1 C1 C2 O2 -173.57(17) . . . . ?
O1 C1 C2 N2 -172.22(18) . . . . ?
N1 C1 C2 N2 7.5(2) . . . . ?
C29 C30 C31 C32 -175.52(18) . . . . ?
C33 C34 C35 C36 177.51(18) . . . . ?
N6 C37 C38 C39 -162.61(18) . . . . ?
C40 C39 C38 C37 73.0(3) . . . . ?
C7 C6 C5 N1 178.54(18) . . . . ?
C7 C6 C5 C10 -0.4(3) . . . . ?
C1 N1 C5 C6 0.1(3) . . . . ?
Cu1 N1 C5 C6 179.54(15) . . . . ?
C1 N1 C5 C10 179.04(18) . . . . ?
Cu1 N1 C5 C10 -1.5(2) . . . . ?
C9 C10 C5 C6 0.6(3) . . . . ?
N3 C10 C5 C6 179.45(16) . . . . ?
C9 C10 C5 N1 -178.47(16) . . . . ?
N3 C10 C5 N1 0.4(2) . . . . ?
C10 N3 C3 O3 1.6(3) . . . . ?
Cu1 N3 C3 O3 179.78(17) . . . . ?
C10 N3 C3 C4 -177.46(17) . . . . ?
Cu1 N3 C3 C4 0.7(2) . . . . ?
O4 C4 C3 O3 3.8(3) . . . . ?
N4 C4 C3 O3 -175.02(18) . . . . ?
O4 C4 C3 N3 -177.02(18) . . . . ?
N4 C4 C3 N3 4.1(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        60.63
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.045
####################################################################### 
# 
# 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 1035431'
_audit_update_record             
;
2015-03-09 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H14 Cu N4 O4, 2(C16 H36 N), 2(H2 O)'
_chemical_formula_sum            'C46 H90 Cu N6 O6'
_chemical_formula_weight         886.77

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.396(5)
_cell_length_b                   13.432(3)
_cell_length_c                   15.919(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.80(3)
_cell_angle_gamma                90
_cell_volume                     4908.4(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    15712
_cell_measurement_theta_min      2.9542
_cell_measurement_theta_max      25.9999

_exptl_crystal_description       block
_exptl_crystal_colour            purple

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_F_000             1940
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    0.495
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.93353
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET)
(compiled Jun 12 2006,17:01:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21633
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.964
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4293
_reflns_number_gt                3662
_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       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET)
(compiled Jun 12 2006,17:01:16)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET)
(compiled Jun 12 2006,17:01:16)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET)
(compiled Jun 12 2006,17:01:16)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'

_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0495P)²+8.6116P] 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         4293
_refine_ls_number_parameters     274
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.1013
_refine_ls_wR_factor_gt          0.0933
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.10607(9) 0.35661(16) -0.14605(14) 0.0227(5) Uani 1 1 d . . . . .
C2 C 0.11482(10) 0.24213(17) -0.13912(15) 0.0270(5) Uani 1 1 d . . . . .
C3 C 0.02910(8) 0.47580(14) -0.21919(12) 0.0167(4) Uani 1 1 d . . . . .
C4 C 0.05694(9) 0.56601(16) -0.19001(13) 0.0198(4) Uani 1 1 d . . . . .
H4 H 0.0950 0.5667 -0.1501 0.024 Uiso 1 1 calc R U . . .
C5 C 0.02820(9) 0.65528(16) -0.22027(14) 0.0219(4) Uani 1 1 d . . . . .
H5 H 0.0471 0.7154 -0.2003 0.026 Uiso 1 1 calc R U . . .
C6 C 0.07550(10) 0.08212(17) -0.18607(15) 0.0278(5) Uani 1 1 d . . . . .
H6A H 0.1149 0.0657 -0.1825 0.033 Uiso 1 1 calc R U . . .
H6B H 0.0491 0.0542 -0.2411 0.033 Uiso 1 1 calc R U . . .
C7 C 0.06324(11) 0.03505(17) -0.10791(16) 0.0331(5) Uani 1 1 d . . . . .
H7A H 0.0685 -0.0357 -0.1090 0.050 Uiso 1 1 calc R U . . .
H7B H 0.0239 0.0493 -0.1120 0.050 Uiso 1 1 calc R U . . .
H7C H 0.0896 0.0617 -0.0531 0.050 Uiso 1 1 calc R U . . .
C8 C 0.23239(9) 0.46898(15) 0.10240(14) 0.0202(4) Uani 1 1 d . . . . .
H8A H 0.2593 0.4174 0.0988 0.024 Uiso 1 1 calc R U . . .
H8B H 0.2061 0.4814 0.0422 0.024 Uiso 1 1 calc R U . . .
C9 C 0.26688(9) 0.56321(15) 0.13687(14) 0.0210(4) Uani 1 1 d . . . . .
H9A H 0.2988 0.5490 0.1916 0.025 Uiso 1 1 calc R U . . .
H9B H 0.2420 0.6128 0.1499 0.025 Uiso 1 1 calc R U . . .
C10 C 0.29069(9) 0.60300(16) 0.06666(14) 0.0242(5) Uani 1 1 d . . . . .
H10A H 0.3126 0.5508 0.0502 0.029 Uiso 1 1 calc R U . . .
H10B H 0.2584 0.6211 0.0137 0.029 Uiso 1 1 calc R U . . .
C11 C 0.32975(10) 0.69297(18) 0.09897(16) 0.0309(5) Uani 1 1 d . . . . .
H11A H 0.3439 0.7150 0.0527 0.046 Uiso 1 1 calc R U . . .
H11B H 0.3621 0.6753 0.1510 0.046 Uiso 1 1 calc R U . . .
H11C H 0.3080 0.7456 0.1137 0.046 Uiso 1 1 calc R U . . .
C12 C 0.23564(9) 0.40619(17) 0.25204(14) 0.0247(5) Uani 1 1 d . . . . .
H12A H 0.2110 0.3897 0.2868 0.030 Uiso 1 1 calc R U . . .
H12B H 0.2574 0.4656 0.2779 0.030 Uiso 1 1 calc R U . . .
C13 C 0.27846(10) 0.32128(17) 0.26032(16) 0.0295(5) Uani 1 1 d . . . . .
H13A H 0.3007 0.3335 0.2212 0.035 Uiso 1 1 calc R U . . .
H13B H 0.2573 0.2594 0.2421 0.035 Uiso 1 1 calc R U . . .
C14 C 0.31961(10) 0.31232(17) 0.35622(16) 0.0308(5) Uani 1 1 d . . . . .
H14A H 0.2968 0.3123 0.3957 0.037 Uiso 1 1 calc R U . . .
H14B H 0.3397 0.2489 0.3633 0.037 Uiso 1 1 calc R U . . .
C15 C 0.36426(12) 0.39440(19) 0.38452(17) 0.0392(6) Uani 1 1 d . . . . .
H15A H 0.3883 0.3845 0.4456 0.059 Uiso 1 1 calc R U . . .
H15B H 0.3448 0.4575 0.3786 0.059 Uiso 1 1 calc R U . . .
H15C H 0.3881 0.3935 0.3473 0.059 Uiso 1 1 calc R U . . .
C16 C 0.15279(9) 0.50556(16) 0.16450(13) 0.0209(4) Uani 1 1 d . . . . .
H16A H 0.1292 0.4751 0.1959 0.025 Uiso 1 1 calc R U . . .
H16B H 0.1737 0.5607 0.2007 0.025 Uiso 1 1 calc R U . . .
C17 C 0.11242(9) 0.54678(16) 0.07687(14) 0.0218(4) Uani 1 1 d . . . . .
H17A H 0.0963 0.4927 0.0355 0.026 Uiso 1 1 calc R U . . .
H17B H 0.1339 0.5905 0.0506 0.026 Uiso 1 1 calc R U . . .
C18 C 0.06342(10) 0.60456(19) 0.09427(15) 0.0294(5) Uani 1 1 d . . . . .
H18A H 0.0394 0.5585 0.1135 0.035 Uiso 1 1 calc R U . . .
H18B H 0.0802 0.6516 0.1423 0.035 Uiso 1 1 calc R U . . .
C19 C 0.02557(11) 0.6601(2) 0.01293(17) 0.0439(7) Uani 1 1 d . . . . .
H19A H -0.0045 0.6949 0.0271 0.066 Uiso 1 1 calc R U . . .
H19B H 0.0082 0.6138 -0.0346 0.066 Uiso 1 1 calc R U . . .
H19C H 0.0489 0.7070 -0.0055 0.066 Uiso 1 1 calc R U . . .
C20 C 0.16713(9) 0.33600(16) 0.10945(14) 0.0236(5) Uani 1 1 d . . . . .
H20A H 0.1451 0.3533 0.0481 0.028 Uiso 1 1 calc R U . . .
H20B H 0.1970 0.2889 0.1081 0.028 Uiso 1 1 calc R U . . .
C21 C 0.12662(10) 0.28475(16) 0.14955(15) 0.0259(5) Uani 1 1 d . . . . .
H21A H 0.0937 0.3276 0.1450 0.031 Uiso 1 1 calc R U . . .
H21B H 0.1470 0.2709 0.2122 0.031 Uiso 1 1 calc R U . . .
C22 C 0.10517(10) 0.18758(17) 0.09932(17) 0.0305(5) Uani 1 1 d . . . . .
H22A H 0.0881 0.2018 0.0360 0.037 Uiso 1 1 calc R U . . .
H22B H 0.1382 0.1437 0.1076 0.037 Uiso 1 1 calc R U . . .
C23 C 0.06041(10) 0.13472(18) 0.13035(18) 0.0350(6) Uani 1 1 d . . . . .
H23A H 0.0485 0.0742 0.0971 0.052 Uiso 1 1 calc R U . . .
H23B H 0.0271 0.1771 0.1208 0.052 Uiso 1 1 calc R U . . .
H23C H 0.0773 0.1195 0.1928 0.052 Uiso 1 1 calc R U . . .
N1 N 0.05167(7) 0.38024(13) -0.19454(11) 0.0192(4) Uani 1 1 d . . . . .
N2 N 0.06885(8) 0.18998(13) -0.18866(12) 0.0239(4) Uani 1 1 d . . . . .
N3 N 0.19698(7) 0.42958(13) 0.15729(11) 0.0203(4) Uani 1 1 d . . . . .
O1 O 0.14768(7) 0.41335(12) -0.10975(11) 0.0337(4) Uani 1 1 d . . . . .
O2 O 0.16314(7) 0.20859(13) -0.08979(12) 0.0397(4) Uani 1 1 d . . . . .
O3 O 0.26750(8) 0.38599(15) -0.08328(14) 0.0439(5) Uani 1 1 d D U . . .
Cu1 Cu 0.0000 0.27137(3) -0.2500 0.01843(12) Uani 1 2 d S T P . .
H1 H 0.2366(14) 0.421(3) -0.124(2) 0.106(11) Uiso 1 1 d D . . . .
H2 H 0.2507(17) 0.336(2) -0.059(3) 0.106(11) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.244(3) . ?
C1 N1 1.328(3) . ?
C1 C2 1.551(3) . ?
C2 O2 1.258(3) . ?
C2 N2 1.331(3) . ?
C3 C4 1.390(3) . ?
C3 N1 1.399(3) . ?
C3 C3 1.426(4) 2_554 ?
C4 C5 1.390(3) . ?
C4 H4 0.9300 . ?
C5 C5 1.381(4) 2_554 ?
C5 H5 0.9300 . ?
C6 N2 1.457(3) . ?
C6 C7 1.513(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.516(3) . ?
C8 N3 1.517(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.521(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.517(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N3 1.516(3) . ?
C12 C13 1.522(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.521(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.508(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.514(3) . ?
C16 N3 1.517(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.527(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.509(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.512(3) . ?
C20 N3 1.521(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.528(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.518(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
N1 Cu1 1.9374(17) . ?
N2 Cu1 1.9645(18) . ?
O3 H1 0.939(18) . ?
O3 H2 0.944(18) . ?
Cu1 N1 1.9374(17) 2_554 ?
Cu1 N2 1.9645(18) 2_554 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N1 128.4(2) . . ?
O1 C1 C2 120.22(19) . . ?
N1 C1 C2 111.38(18) . . ?
O2 C2 N2 127.2(2) . . ?
O2 C2 C1 118.5(2) . . ?
N2 C2 C1 114.31(18) . . ?
C4 C3 N1 127.19(18) . . ?
C4 C3 C3 119.33(12) . 2_554 ?
N1 C3 C3 113.48(10) . 2_554 ?
C5 C4 C3 120.27(19) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C5 C5 C4 120.40(12) 2_554 . ?
C5 C5 H5 119.8 2_554 . ?
C4 C5 H5 119.8 . . ?
N2 C6 C7 112.81(19) . . ?
N2 C6 H6A 109.0 . . ?
C7 C6 H6A 109.0 . . ?
N2 C6 H6B 109.0 . . ?
C7 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 N3 115.93(16) . . ?
C9 C8 H8A 108.3 . . ?
N3 C8 H8A 108.3 . . ?
C9 C8 H8B 108.3 . . ?
N3 C8 H8B 108.3 . . ?
H8A C8 H8B 107.4 . . ?
C8 C9 C10 109.31(17) . . ?
C8 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
C8 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.3 . . ?
C11 C10 C9 112.54(18) . . ?
C11 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
C11 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C13 114.76(18) . . ?
N3 C12 H12A 108.6 . . ?
C13 C12 H12A 108.6 . . ?
N3 C12 H12B 108.6 . . ?
C13 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
C12 C13 C14 110.28(19) . . ?
C12 C13 H13A 109.6 . . ?
C14 C13 H13A 109.6 . . ?
C12 C13 H13B 109.6 . . ?
C14 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C15 C14 C13 114.0(2) . . ?
C15 C14 H14A 108.8 . . ?
C13 C14 H14A 108.8 . . ?
C15 C14 H14B 108.8 . . ?
C13 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N3 115.69(16) . . ?
C17 C16 H16A 108.4 . . ?
N3 C16 H16A 108.4 . . ?
C17 C16 H16B 108.4 . . ?
N3 C16 H16B 108.4 . . ?
H16A C16 H16B 107.4 . . ?
C16 C17 C18 108.88(17) . . ?
C16 C17 H17A 109.9 . . ?
C18 C17 H17A 109.9 . . ?
C16 C17 H17B 109.9 . . ?
C18 C17 H17B 109.9 . . ?
H17A C17 H17B 108.3 . . ?
C19 C18 C17 112.63(19) . . ?
C19 C18 H18A 109.1 . . ?
C17 C18 H18A 109.1 . . ?
C19 C18 H18B 109.1 . . ?
C17 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 N3 115.81(17) . . ?
C21 C20 H20A 108.3 . . ?
N3 C20 H20A 108.3 . . ?
C21 C20 H20B 108.3 . . ?
N3 C20 H20B 108.3 . . ?
H20A C20 H20B 107.4 . . ?
C20 C21 C22 108.97(18) . . ?
C20 C21 H21A 109.9 . . ?
C22 C21 H21A 109.9 . . ?
C20 C21 H21B 109.9 . . ?
C22 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
C23 C22 C21 112.7(2) . . ?
C23 C22 H22A 109.1 . . ?
C21 C22 H22A 109.1 . . ?
C23 C22 H22B 109.1 . . ?
C21 C22 H22B 109.1 . . ?
H22A C22 H22B 107.8 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C1 N1 C3 127.09(17) . . ?
C1 N1 Cu1 116.89(14) . . ?
C3 N1 Cu1 115.53(13) . . ?
C2 N2 C6 116.32(18) . . ?
C2 N2 Cu1 114.12(15) . . ?
C6 N2 Cu1 129.47(15) . . ?
C8 N3 C16 111.53(15) . . ?
C8 N3 C12 111.20(15) . . ?
C16 N3 C12 106.42(15) . . ?
C8 N3 C20 105.62(15) . . ?
C16 N3 C20 111.21(16) . . ?
C12 N3 C20 110.96(16) . . ?
H1 O3 H2 107(3) . . ?
N1 Cu1 N1 81.97(10) . 2_554 ?
N1 Cu1 N2 83.03(8) . . ?
N1 Cu1 N2 164.04(7) 2_554 . ?
N1 Cu1 N2 164.04(7) . 2_554 ?
N1 Cu1 N2 83.03(8) 2_554 2_554 ?
N2 Cu1 N2 112.38(11) . 2_554 ?

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
O1 C1 C2 O2 6.2(3) . . . . ?
N1 C1 C2 O2 -174.9(2) . . . . ?
O1 C1 C2 N2 -173.0(2) . . . . ?
N1 C1 C2 N2 5.8(3) . . . . ?
N1 C3 C4 C5 -179.33(19) . . . . ?
C3 C3 C4 C5 0.3(3) 2_554 . . . ?
C3 C4 C5 C5 -0.2(3) . . . 2_554 ?
N3 C8 C9 C10 -169.78(17) . . . . ?
C8 C9 C10 C11 -175.53(18) . . . . ?
N3 C12 C13 C14 173.32(18) . . . . ?
C12 C13 C14 C15 -72.5(3) . . . . ?
N3 C16 C17 C18 168.46(18) . . . . ?
C16 C17 C18 C19 172.2(2) . . . . ?
N3 C20 C21 C22 -174.54(17) . . . . ?
C20 C21 C22 C23 -175.54(19) . . . . ?
O1 C1 N1 C3 2.9(4) . . . . ?
C2 C1 N1 C3 -175.88(18) . . . . ?
O1 C1 N1 Cu1 174.47(18) . . . . ?
C2 C1 N1 Cu1 -4.3(2) . . . . ?
C4 C3 N1 C1 -7.8(3) . . . . ?
C3 C3 N1 C1 172.5(2) 2_554 . . . ?
C4 C3 N1 Cu1 -179.52(15) . . . . ?
C3 C3 N1 Cu1 0.8(3) 2_554 . . . ?
O2 C2 N2 C6 -0.7(3) . . . . ?
C1 C2 N2 C6 178.52(18) . . . . ?
O2 C2 N2 Cu1 176.2(2) . . . . ?
C1 C2 N2 Cu1 -4.6(2) . . . . ?
C7 C6 N2 C2 84.6(2) . . . . ?
C7 C6 N2 Cu1 -91.7(2) . . . . ?
C9 C8 N3 C16 59.2(2) . . . . ?
C9 C8 N3 C12 -59.4(2) . . . . ?
C9 C8 N3 C20 -179.83(17) . . . . ?
C17 C16 N3 C8 53.6(2) . . . . ?
C17 C16 N3 C12 175.00(17) . . . . ?
C17 C16 N3 C20 -64.1(2) . . . . ?
C13 C12 N3 C8 -65.7(2) . . . . ?
C13 C12 N3 C16 172.65(17) . . . . ?
C13 C12 N3 C20 51.5(2) . . . . ?
C21 C20 N3 C8 -177.40(17) . . . . ?
C21 C20 N3 C16 -56.3(2) . . . . ?
C21 C20 N3 C12 62.0(2) . . . . ?

_refine_diff_density_max         1.188
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.052

_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_abdulm89
_database_code_depnum_ccdc_archive 'CCDC 1035432'
_audit_update_record             
;
2014-11-21 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H36 N), C16 H18 Cu N4 O4'
_chemical_formula_sum            'C48 H90 Cu N6 O4'
_chemical_formula_weight         878.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.4875(6)
_cell_length_b                   14.6748(7)
_cell_length_c                   25.6140(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.346(4)
_cell_angle_gamma                90.00
_cell_volume                     5047.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    6867
_cell_measurement_theta_min      3.2883
_cell_measurement_theta_max      61.9929


_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1924
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_min  0.50473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  25
_diffrn_standards_decay_%        0
_diffrn_reflns_number            14520
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         59.99
_reflns_number_total             7383
_reflns_number_gt                3309
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
;

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2sigma(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. Several atoms are alerted
 by level A to C alerts by the checkcif procedure to have large ADP max/min
 ratio's, large hirshfeld test difference and/or high Ueq values when compared
 to neighbors. Furthermore, short intra and/or inter H...H contacts are 
 alerted. Most probably, all of these alerts are due to further unresolveable
 disorder of atoms/groups. The best suitable crystal of this compound chosen
 for measurement was, due to its plate-like shape weakly diffractive only.
 Although long measurement times of individual frames have been applied the
 ratio between observed/unique reflections is with ca. 45 % still poor. 
 Furthermore, due to icing problems, the measurement has been stopped at
 a resolution of theta = ca. 60 degree. 
;

_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)+(0.1870P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7383
_refine_ls_number_parameters     715
_refine_ls_number_restraints     804
_refine_ls_R_factor_all          0.1498
_refine_ls_R_factor_gt           0.0883
_refine_ls_wR_factor_ref         0.2980
_refine_ls_wR_factor_gt          0.2625
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.963
_refine_ls_shift/su_max          0.005
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3787(8) 0.7191(4) 0.2179(2) 0.136(3) Uani 1 1 d . . .
C2 C 0.2645(8) 0.7346(4) 0.2192(2) 0.133(3) Uani 1 1 d . C .
C3 C 0.3805(10) 0.7625(4) 0.0192(3) 0.162(4) Uani 1 1 d . C .
C4 C 0.2652(12) 0.7597(4) 0.0070(2) 0.182(5) Uani 1 1 d . C .
C5 C 0.4977(7) 0.7306(3) 0.1517(3) 0.168(4) Uani 1 1 d G . .
C6 C 0.5864(9) 0.7233(3) 0.1837(2) 0.176(4) Uani 1 1 d G . .
H6 H 0.5853 0.7178 0.2198 0.211 Uiso 1 1 calc R . .
C7 C 0.6769(7) 0.7242(3) 0.1618(4) 0.237(6) Uani 1 1 d G . .
H7 H 0.7362 0.7193 0.1832 0.285 Uiso 1 1 calc R . .
C8 C 0.6786(6) 0.7324(3) 0.1078(4) 0.210(7) Uani 1 1 d G . .
H8 H 0.7392 0.7330 0.0931 0.252 Uiso 1 1 calc R . .
C9 C 0.5900(8) 0.7397(3) 0.0758(2) 0.208(7) Uani 1 1 d G . .
H9 H 0.5911 0.7452 0.0397 0.249 Uiso 1 1 calc R . .
C10 C 0.4995(6) 0.7388(3) 0.0977(3) 0.147(3) Uani 1 1 d G C .
C12 C 0.0993(9) 0.7530(4) 0.0355(3) 0.171(4) Uani 1 1 d D C .
H12A H 0.0811 0.7870 0.0036 0.205 Uiso 1 1 calc R . .
H12B H 0.0675 0.7823 0.0636 0.205 Uiso 1 1 calc R . .
C15 C 0.0582(7) 0.6545(5) 0.0284(3) 0.169(3) Uani 1 1 d D . .
H15A H 0.0907 0.6243 0.0010 0.203 Uiso 1 1 calc R . .
H15B H 0.0737 0.6208 0.0607 0.203 Uiso 1 1 calc R . .
C16 C -0.0532(7) 0.6538(7) 0.0144(3) 0.203(4) Uani 1 1 d D . .
H16A H -0.0761 0.5919 0.0109 0.305 Uiso 1 1 calc R . .
H16B H -0.0686 0.6854 -0.0182 0.305 Uiso 1 1 calc R . .
H16C H -0.0856 0.6835 0.0415 0.305 Uiso 1 1 calc R . .
C17 C 0.192(4) 0.614(3) 0.343(3) 0.199(10) Uani 0.17(4) 1 d PDU A 1
H17A H 0.2143 0.6660 0.3645 0.239 Uiso 0.17(4) 1 calc PR A 1
H17B H 0.2132 0.6216 0.3086 0.239 Uiso 0.17(4) 1 calc PR A 1
C18 C 0.079(4) 0.606(4) 0.341(6) 0.202(4) Uani 0.17(4) 1 d PDU A 1
H18A H 0.0610 0.5675 0.3690 0.243 Uiso 0.17(4) 1 calc PR A 1
H18B H 0.0550 0.5772 0.3077 0.243 Uiso 0.17(4) 1 calc PR A 1
C19 C 0.031(5) 0.699(4) 0.344(3) 0.212(6) Uani 0.17(4) 1 d PDU A 1
H19A H 0.0353 0.7180 0.3808 0.255 Uiso 0.17(4) 1 calc PR A 1
H19B H 0.0677 0.7434 0.3254 0.255 Uiso 0.17(4) 1 calc PR A 1
C20 C -0.077(4) 0.699(5) 0.322(3) 0.209(16) Uani 0.17(4) 1 d PDU A 1
H20A H -0.1016 0.7604 0.3208 0.313 Uiso 0.17(4) 1 calc PR A 1
H20B H -0.1151 0.6629 0.3441 0.313 Uiso 0.17(4) 1 calc PR A 1
H20C H -0.0819 0.6739 0.2874 0.313 Uiso 0.17(4) 1 calc PR A 1
C17' C 0.1741(10) 0.6080(6) 0.3575(4) 0.181(4) Uani 0.83(4) 1 d PDU A 2
H17C H 0.1720 0.6418 0.3899 0.217 Uiso 0.83(4) 1 calc PR A 2
H17D H 0.2052 0.6469 0.3331 0.217 Uiso 0.83(4) 1 calc PR A 2
C18' C 0.0691(12) 0.5894(9) 0.3355(12) 0.202(4) Uani 0.83(4) 1 d PDU A 2
H18C H 0.0366 0.5507 0.3594 0.243 Uiso 0.83(4) 1 calc PR A 2
H18D H 0.0695 0.5575 0.3023 0.243 Uiso 0.83(4) 1 calc PR A 2
C19' C 0.0114(13) 0.6777(10) 0.3271(7) 0.212(6) Uani 0.83(4) 1 d PDU A 2
H19C H 0.0104 0.7088 0.3605 0.255 Uiso 0.83(4) 1 calc PR A 2
H19D H 0.0454 0.7169 0.3040 0.255 Uiso 0.83(4) 1 calc PR A 2
C20' C -0.0910(13) 0.6632(14) 0.3045(7) 0.244(8) Uani 0.83(4) 1 d PDU A 2
H20D H -0.1250 0.7207 0.3011 0.365 Uiso 0.83(4) 1 calc PR A 2
H20E H -0.1248 0.6240 0.3270 0.365 Uiso 0.83(4) 1 calc PR A 2
H20F H -0.0905 0.6355 0.2706 0.365 Uiso 0.83(4) 1 calc PR A 2
C21 C 0.275(3) 0.4602(16) 0.3264(8) 0.133(9) Uani 0.320(14) 1 d PDU A 1
H21A H 0.3193 0.4152 0.3434 0.160 Uiso 0.320(14) 1 calc PR A 1
H21B H 0.2170 0.4281 0.3100 0.160 Uiso 0.320(14) 1 calc PR A 1
C22 C 0.327(2) 0.5081(13) 0.2842(6) 0.122(7) Uani 0.320(14) 1 d PDU A 1
H22A H 0.3966 0.5159 0.2965 0.147 Uiso 0.320(14) 1 calc PR A 1
H22B H 0.2981 0.5682 0.2783 0.147 Uiso 0.320(14) 1 calc PR A 1
C23 C 0.3193(17) 0.4562(12) 0.2327(6) 0.112(7) Uani 0.320(14) 1 d PDU A 1
H23A H 0.3669 0.4816 0.2106 0.134 Uiso 0.320(14) 1 calc PR A 1
H23B H 0.3378 0.3932 0.2398 0.134 Uiso 0.320(14) 1 calc PR A 1
C24 C 0.2178(19) 0.4582(18) 0.2032(9) 0.118(8) Uani 0.320(14) 1 d PDU A 1
H24A H 0.2180 0.4215 0.1722 0.177 Uiso 0.320(14) 1 calc PR A 1
H24B H 0.2009 0.5199 0.1935 0.177 Uiso 0.320(14) 1 calc PR A 1
H24C H 0.1697 0.4347 0.2250 0.177 Uiso 0.320(14) 1 calc PR A 1
C21' C 0.2258(17) 0.4669(8) 0.3165(5) 0.176(7) Uani 0.680(14) 1 d PDU A 2
H21C H 0.2677 0.4133 0.3212 0.211 Uiso 0.680(14) 1 calc PR A 2
H21D H 0.1573 0.4461 0.3119 0.211 Uiso 0.680(14) 1 calc PR A 2
C22' C 0.2488(16) 0.5134(8) 0.2664(5) 0.179(7) Uani 0.680(14) 1 d PDU A 2
H22C H 0.3155 0.5387 0.2705 0.215 Uiso 0.680(14) 1 calc PR A 2
H22D H 0.2021 0.5627 0.2581 0.215 Uiso 0.680(14) 1 calc PR A 2
C23' C 0.2406(15) 0.4420(12) 0.2219(5) 0.178(8) Uani 0.680(14) 1 d PDU A 2
H23C H 0.2886 0.3935 0.2296 0.214 Uiso 0.680(14) 1 calc PR A 2
H23D H 0.1744 0.4155 0.2182 0.214 Uiso 0.680(14) 1 calc PR A 2
C24' C 0.2613(12) 0.4911(8) 0.1715(5) 0.193(7) Uani 0.680(14) 1 d PDU A 2
H24D H 0.2587 0.4482 0.1431 0.289 Uiso 0.680(14) 1 calc PR A 2
H24E H 0.3263 0.5184 0.1760 0.289 Uiso 0.680(14) 1 calc PR A 2
H24F H 0.2121 0.5376 0.1638 0.289 Uiso 0.680(14) 1 calc PR A 2
C25 C 0.343(2) 0.552(3) 0.3939(19) 0.183(9) Uani 0.244(13) 1 d PDU A 1
H25A H 0.3751 0.5863 0.3678 0.219 Uiso 0.244(13) 1 calc PR A 1
H25B H 0.3327 0.5938 0.4222 0.219 Uiso 0.244(13) 1 calc PR A 1
C26 C 0.416(3) 0.483(3) 0.4154(19) 0.192(12) Uani 0.244(13) 1 d PDU A 1
H26A H 0.3995 0.4263 0.3969 0.230 Uiso 0.244(13) 1 calc PR A 1
H26B H 0.4032 0.4729 0.4517 0.230 Uiso 0.244(13) 1 calc PR A 1
C27 C 0.528(3) 0.498(2) 0.4145(10) 0.192(11) Uani 0.244(13) 1 d PDU A 1
H27A H 0.5594 0.4416 0.4054 0.230 Uiso 0.244(13) 1 calc PR A 1
H27B H 0.5394 0.5429 0.3878 0.230 Uiso 0.244(13) 1 calc PR A 1
C28 C 0.575(2) 0.5314(19) 0.4676(8) 0.167(10) Uani 0.244(13) 1 d PDU A 1
H28A H 0.6094 0.5879 0.4630 0.250 Uiso 0.244(13) 1 calc PR A 1
H28B H 0.6220 0.4868 0.4821 0.250 Uiso 0.244(13) 1 calc PR A 1
H28C H 0.5245 0.5405 0.4909 0.250 Uiso 0.244(13) 1 calc PR A 1
C25' C 0.3391(10) 0.5619(8) 0.3819(6) 0.183(5) Uani 0.756(13) 1 d PDU A 2
H25C H 0.3383 0.6023 0.4118 0.220 Uiso 0.756(13) 1 calc PR A 2
H25D H 0.3592 0.5970 0.3526 0.220 Uiso 0.756(13) 1 calc PR A 2
C26' C 0.4120(10) 0.4873(10) 0.3946(7) 0.189(5) Uani 0.756(13) 1 d PDU A 2
H26C H 0.4192 0.4489 0.3644 0.226 Uiso 0.756(13) 1 calc PR A 2
H26D H 0.3932 0.4500 0.4234 0.226 Uiso 0.756(13) 1 calc PR A 2
C27' C 0.5052(10) 0.5404(6) 0.4099(5) 0.197(5) Uani 0.756(13) 1 d PDU A 2
H27C H 0.4930 0.5834 0.4374 0.236 Uiso 0.756(13) 1 calc PR A 2
H27D H 0.5235 0.5748 0.3799 0.236 Uiso 0.756(13) 1 calc PR A 2
C28' C 0.5893(9) 0.4783(7) 0.4289(6) 0.202(6) Uani 0.756(13) 1 d PDU A 2
H28D H 0.6516 0.5071 0.4239 0.304 Uiso 0.756(13) 1 calc PR A 2
H28E H 0.5839 0.4223 0.4095 0.304 Uiso 0.756(13) 1 calc PR A 2
H28F H 0.5862 0.4657 0.4655 0.304 Uiso 0.756(13) 1 calc PR A 2
C29 C 0.1987(6) 0.4663(3) 0.4100(2) 0.155(3) Uani 1 1 d . A .
H29A H 0.2431 0.4150 0.4173 0.185 Uiso 1 1 calc R . .
H29B H 0.1348 0.4423 0.3958 0.185 Uiso 1 1 calc R . .
C30 C 0.1846(6) 0.5140(4) 0.4615(2) 0.150(3) Uani 1 1 d . . .
H30A H 0.1336 0.5605 0.4561 0.180 Uiso 1 1 calc R . .
H30B H 0.2463 0.5429 0.4752 0.180 Uiso 1 1 calc R . .
C31 C 0.1534(6) 0.4415(4) 0.5003(2) 0.150(3) Uani 1 1 d . . .
H31A H 0.2067 0.3977 0.5074 0.180 Uiso 1 1 calc R . .
H31B H 0.0950 0.4092 0.4850 0.180 Uiso 1 1 calc R . .
C32 C 0.1300(6) 0.4877(5) 0.5518(3) 0.158(3) Uani 1 1 d . . .
H32A H 0.1108 0.4423 0.5759 0.236 Uiso 1 1 calc R . .
H32B H 0.0764 0.5304 0.5447 0.236 Uiso 1 1 calc R . .
H32C H 0.1880 0.5193 0.5670 0.236 Uiso 1 1 calc R . .
C33 C 0.4128(13) 0.6661(7) -0.1278(6) 0.134(4) Uani 0.65(4) 1 d PDU B 1
H33A H 0.3916 0.6945 -0.0965 0.161 Uiso 0.65(4) 1 calc PR B 1
H33B H 0.3958 0.7073 -0.1569 0.161 Uiso 0.65(4) 1 calc PR B 1
C34 C 0.5294(14) 0.6544(9) -0.1207(8) 0.143(5) Uani 0.65(4) 1 d PDU B 1
H34A H 0.5477 0.6178 -0.0898 0.172 Uiso 0.65(4) 1 calc PR B 1
H34B H 0.5510 0.6225 -0.1508 0.172 Uiso 0.65(4) 1 calc PR B 1
C35 C 0.5810(16) 0.7441(7) -0.1151(6) 0.149(5) Uani 0.65(4) 1 d PDU B 1
H35A H 0.5533 0.7780 -0.0873 0.179 Uiso 0.65(4) 1 calc PR B 1
H35B H 0.5661 0.7781 -0.1474 0.179 Uiso 0.65(4) 1 calc PR B 1
C36 C 0.6937(19) 0.7403(10) -0.1030(8) 0.179(7) Uani 0.65(4) 1 d PDU B 1
H36A H 0.7201 0.8011 -0.1012 0.268 Uiso 0.65(4) 1 calc PR B 1
H36B H 0.7224 0.7072 -0.1303 0.268 Uiso 0.65(4) 1 calc PR B 1
H36C H 0.7097 0.7102 -0.0701 0.268 Uiso 0.65(4) 1 calc PR B 1
C33' C 0.403(2) 0.6655(15) -0.1389(14) 0.134(8) Uani 0.35(4) 1 d PDU B 2
H33C H 0.3687 0.7084 -0.1182 0.161 Uiso 0.35(4) 1 calc PR B 2
H33D H 0.3989 0.6878 -0.1746 0.161 Uiso 0.35(4) 1 calc PR B 2
C34' C 0.515(2) 0.661(2) -0.1169(16) 0.142(9) Uani 0.35(4) 1 d PDU B 2
H34C H 0.5210 0.6364 -0.0815 0.170 Uiso 0.35(4) 1 calc PR B 2
H34D H 0.5519 0.6222 -0.1388 0.170 Uiso 0.35(4) 1 calc PR B 2
C35' C 0.5513(19) 0.757(2) -0.1175(16) 0.126(7) Uani 0.35(4) 1 d PDU B 2
H35C H 0.5126 0.7946 -0.0958 0.152 Uiso 0.35(4) 1 calc PR B 2
H35D H 0.5430 0.7806 -0.1530 0.152 Uiso 0.35(4) 1 calc PR B 2
C36' C 0.6598(17) 0.761(2) -0.0970(13) 0.126(7) Uani 0.35(4) 1 d PDU B 2
H36D H 0.6823 0.8230 -0.0968 0.190 Uiso 0.35(4) 1 calc PR B 2
H36E H 0.6982 0.7251 -0.1192 0.190 Uiso 0.35(4) 1 calc PR B 2
H36F H 0.6679 0.7370 -0.0620 0.190 Uiso 0.35(4) 1 calc PR B 2
C37 C 0.395(3) 0.523(3) -0.0898(8) 0.124(9) Uani 0.37(5) 1 d PDU B 1
H37A H 0.3686 0.4620 -0.0926 0.149 Uiso 0.37(5) 1 calc PR B 1
H37B H 0.4667 0.5196 -0.0893 0.149 Uiso 0.37(5) 1 calc PR B 1
C38 C 0.369(3) 0.5643(18) -0.0385(9) 0.127(9) Uani 0.37(5) 1 d PDU B 1
H38A H 0.3086 0.6002 -0.0442 0.153 Uiso 0.37(5) 1 calc PR B 1
H38B H 0.4225 0.6038 -0.0242 0.153 Uiso 0.37(5) 1 calc PR B 1
C39 C 0.354(3) 0.4841(14) 0.0003(11) 0.131(9) Uani 0.37(5) 1 d PDU B 1
H39A H 0.3145 0.4369 -0.0182 0.157 Uiso 0.37(5) 1 calc PR B 1
H39B H 0.4183 0.4582 0.0120 0.157 Uiso 0.37(5) 1 calc PR B 1
C40 C 0.304(3) 0.5123(13) 0.0467(13) 0.167(14) Uani 0.37(5) 1 d PDU B 1
H40A H 0.2993 0.4610 0.0696 0.250 Uiso 0.37(5) 1 calc PR B 1
H40B H 0.2385 0.5344 0.0357 0.250 Uiso 0.37(5) 1 calc PR B 1
H40C H 0.3420 0.5597 0.0650 0.250 Uiso 0.37(5) 1 calc PR B 1
C37' C 0.361(3) 0.5124(12) -0.0905(5) 0.139(7) Uani 0.63(5) 1 d PDU B 2
H37C H 0.3217 0.4586 -0.1003 0.166 Uiso 0.63(5) 1 calc PR B 2
H37D H 0.4297 0.4930 -0.0835 0.166 Uiso 0.63(5) 1 calc PR B 2
C38' C 0.327(3) 0.5489(13) -0.0401(6) 0.163(8) Uani 0.63(5) 1 d PDU B 2
H38C H 0.2599 0.5724 -0.0471 0.196 Uiso 0.63(5) 1 calc PR B 2
H38D H 0.3698 0.5994 -0.0282 0.196 Uiso 0.63(5) 1 calc PR B 2
C39' C 0.328(3) 0.4765(14) 0.0050(7) 0.178(9) Uani 0.63(5) 1 d PDU B 2
H39C H 0.2779 0.4308 -0.0047 0.214 Uiso 0.63(5) 1 calc PR B 2
H39D H 0.3924 0.4462 0.0082 0.214 Uiso 0.63(5) 1 calc PR B 2
C40' C 0.309(3) 0.5152(17) 0.0584(10) 0.263(16) Uani 0.63(5) 1 d PDU B 2
H40D H 0.3069 0.4663 0.0831 0.395 Uiso 0.63(5) 1 calc PR B 2
H40E H 0.2471 0.5474 0.0555 0.395 Uiso 0.63(5) 1 calc PR B 2
H40F H 0.3622 0.5563 0.0700 0.395 Uiso 0.63(5) 1 calc PR B 2
C41 C 0.2387(7) 0.5990(5) -0.1491(3) 0.147(3) Uani 1 1 d . B .
H41A H 0.2170 0.6296 -0.1186 0.177 Uiso 1 1 calc R . .
H41B H 0.2300 0.6414 -0.1782 0.177 Uiso 1 1 calc R . .
C42 C 0.1730(8) 0.5210(6) -0.1611(5) 0.201(4) Uani 1 1 d . . .
H42A H 0.1845 0.4758 -0.1336 0.241 Uiso 1 1 calc R . .
H42B H 0.1889 0.4935 -0.1938 0.241 Uiso 1 1 calc R . .
C43 C 0.0540(9) 0.5510(6) -0.1665(4) 0.194(4) Uani 1 1 d . . .
H43A H 0.0438 0.6010 -0.1912 0.233 Uiso 1 1 calc R . .
H43B H 0.0136 0.5000 -0.1800 0.233 Uiso 1 1 calc R . .
C44 C 0.0223(8) 0.5789(7) -0.1159(4) 0.236(5) Uani 1 1 d . . .
H44A H -0.0469 0.5955 -0.1201 0.353 Uiso 1 1 calc R . .
H44B H 0.0611 0.6303 -0.1028 0.353 Uiso 1 1 calc R . .
H44C H 0.0316 0.5293 -0.0915 0.353 Uiso 1 1 calc R . .
C45 C 0.3858(7) 0.5212(4) -0.1841(2) 0.156(3) Uani 1 1 d . B .
H45A H 0.4514 0.4959 -0.1744 0.187 Uiso 1 1 calc R . .
H45B H 0.3399 0.4706 -0.1902 0.187 Uiso 1 1 calc R . .
C46 C 0.3886(7) 0.5742(5) -0.2351(2) 0.188(4) Uani 1 1 d . . .
H46A H 0.3247 0.6030 -0.2444 0.226 Uiso 1 1 calc R . .
H46B H 0.4390 0.6215 -0.2307 0.226 Uiso 1 1 calc R . .
C47 C 0.4123(11) 0.5096(6) -0.2778(4) 0.224(6) Uani 1 1 d . . .
H47A H 0.4375 0.5429 -0.3065 0.268 Uiso 1 1 calc R . .
H47B H 0.4626 0.4661 -0.2645 0.268 Uiso 1 1 calc R . .
C48 C 0.3206(11) 0.4627(9) -0.2958(5) 0.273(8) Uani 1 1 d . . .
H48A H 0.3346 0.4155 -0.3200 0.410 Uiso 1 1 calc R . .
H48B H 0.2744 0.5053 -0.3130 0.410 Uiso 1 1 calc R . .
H48C H 0.2921 0.4362 -0.2664 0.410 Uiso 1 1 calc R . .
N1 N 0.4056(5) 0.7319(3) 0.1692(2) 0.134(2) Uani 1 1 d . . .
N2 N 0.2154(6) 0.7485(4) 0.17355(19) 0.149(2) Uani 1 1 d DU . .
N3 N 0.4043(8) 0.7457(3) 0.0707(2) 0.170(4) Uani 1 1 d . . .
N4 N 0.2129(7) 0.7587(3) 0.04821(19) 0.145(2) Uani 1 1 d D . .
N5 N 0.2399(6) 0.5249(3) 0.3687(2) 0.170(2) Uani 1 1 d DU . .
N6 N 0.3544(5) 0.5774(3) -0.13795(19) 0.1392(18) Uani 1 1 d DU . .
O1 O 0.4317(4) 0.6986(3) 0.25765(19) 0.1576(19) Uani 1 1 d . . .
O2 O 0.2314(5) 0.7353(3) 0.26280(14) 0.156(2) Uani 1 1 d . . .
O3 O 0.4286(7) 0.7734(3) -0.0160(2) 0.245(4) Uani 1 1 d . . .
O4 O 0.2226(6) 0.7586(3) -0.04115(16) 0.193(3) Uani 1 1 d . . .
Cu1 Cu 0.29467(10) 0.74718(4) 0.11441(3) 0.1452(6) Uani 1 1 d U C .
C11 C 0.1055(12) 0.7264(9) 0.1740(6) 0.122(4) Uani 0.467(9) 1 d PDU C 1
H11A H 0.0908 0.6873 0.2028 0.146 Uiso 0.467(9) 1 calc PR C 1
H11B H 0.0753 0.7028 0.1409 0.146 Uiso 0.467(9) 1 calc PR C 1
C13 C 0.0829(15) 0.8269(9) 0.1828(8) 0.159(6) Uani 0.467(9) 1 d PDU C 1
H13A H 0.1193 0.8486 0.2148 0.191 Uiso 0.467(9) 1 calc PR C 1
H13B H 0.1017 0.8634 0.1537 0.191 Uiso 0.467(9) 1 calc PR C 1
C14 C -0.0274(14) 0.8325(12) 0.1867(7) 0.195(8) Uani 0.467(9) 1 d PDU C 1
H14A H -0.0483 0.7814 0.2064 0.293 Uiso 0.467(9) 1 calc PR C 1
H14B H -0.0617 0.8316 0.1521 0.293 Uiso 0.467(9) 1 calc PR C 1
H14C H -0.0426 0.8880 0.2040 0.293 Uiso 0.467(9) 1 calc PR C 1
C11' C 0.1059(10) 0.7822(9) 0.1729(5) 0.126(4) Uani 0.533(9) 1 d PDU C 2
H11C H 0.0980 0.8182 0.2040 0.151 Uiso 0.533(9) 1 calc PR C 2
H11D H 0.0893 0.8204 0.1424 0.151 Uiso 0.533(9) 1 calc PR C 2
C13' C 0.0373(12) 0.7010(8) 0.1712(7) 0.143(5) Uani 0.533(9) 1 d PDU C 2
H13C H 0.0532 0.6647 0.2025 0.172 Uiso 0.533(9) 1 calc PR C 2
H13D H 0.0494 0.6635 0.1412 0.172 Uiso 0.533(9) 1 calc PR C 2
C14' C -0.0725(11) 0.7259(10) 0.1675(7) 0.165(5) Uani 0.533(9) 1 d PDU C 2
H14D H -0.1119 0.6713 0.1656 0.247 Uiso 0.533(9) 1 calc PR C 2
H14E H -0.0890 0.7619 0.1367 0.247 Uiso 0.533(9) 1 calc PR C 2
H14F H -0.0860 0.7602 0.1980 0.247 Uiso 0.533(9) 1 calc PR C 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.227(8) . ?
C1 N1 1.343(7) . ?
C1 C2 1.561(11) . ?
C2 O2 1.240(7) . ?
C2 N2 1.306(9) . ?
C3 O3 1.171(8) . ?
C3 N3 1.351(10) . ?
C3 C4 1.559(14) . ?
C4 O4 1.312(10) . ?
C4 N4 1.322(10) . ?
C5 N1 1.360(8) . ?
C5 C6 1.3900 . ?
C5 C10 1.3900 . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 C9 1.3900 . ?
C8 H8 0.9300 . ?
C9 C10 1.3900 . ?
C9 H9 0.9300 . ?
C10 N3 1.404(10) . ?
C12 N4 1.538(10) . ?
C12 C15 1.553(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C15 C16 1.512(9) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.52(2) . ?
C17 N5 1.56(2) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.53(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.51(2) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C17' C18' 1.500(13) . ?
C17' N5 1.519(10) . ?
C17' H17C 0.9700 . ?
C17' H17D 0.9700 . ?
C18' C19' 1.516(12) . ?
C18' H18C 0.9700 . ?
C18' H18D 0.9700 . ?
C19' C20' 1.463(14) . ?
C19' H19C 0.9700 . ?
C19' H19D 0.9700 . ?
C20' H20D 0.9600 . ?
C20' H20E 0.9600 . ?
C20' H20F 0.9600 . ?
C21 C22 1.517(17) . ?
C21 N5 1.544(17) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.518(15) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.501(18) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C21' C22' 1.511(12) . ?
C21' N5 1.581(12) . ?
C21' H21C 0.9700 . ?
C21' H21D 0.9700 . ?
C22' C23' 1.545(15) . ?
C22' H22C 0.9700 . ?
C22' H22D 0.9700 . ?
C23' C24' 1.526(15) . ?
C23' H23C 0.9700 . ?
C23' H23D 0.9700 . ?
C24' H24D 0.9600 . ?
C24' H24E 0.9600 . ?
C24' H24F 0.9600 . ?
C25 C26 1.48(2) . ?
C25 N5 1.530(19) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.54(2) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.53(2) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C25' N5 1.455(12) . ?
C25' C26' 1.487(13) . ?
C25' H25C 0.9700 . ?
C25' H25D 0.9700 . ?
C26' C27' 1.500(13) . ?
C26' H26C 0.9700 . ?
C26' H26D 0.9700 . ?
C27' C28' 1.501(14) . ?
C27' H27C 0.9700 . ?
C27' H27D 0.9700 . ?
C28' H28D 0.9600 . ?
C28' H28E 0.9600 . ?
C28' H28F 0.9600 . ?
C29 N5 1.510(7) . ?
C29 C30 1.519(8) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.540(7) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.544(9) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N6 1.532(13) . ?
C33 C34 1.576(13) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.489(13) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.525(14) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C33' N6 1.453(16) . ?
C33' C34' 1.555(18) . ?
C33' H33C 0.9700 . ?
C33' H33D 0.9700 . ?
C34' C35' 1.498(18) . ?
C34' H34C 0.9700 . ?
C34' H34D 0.9700 . ?
C35' C36' 1.508(17) . ?
C35' H35C 0.9700 . ?
C35' H35D 0.9700 . ?
C36' H36D 0.9600 . ?
C36' H36E 0.9600 . ?
C36' H36F 0.9600 . ?
C37 C38 1.513(18) . ?
C37 N6 1.523(18) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.568(15) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.478(17) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C37' C38' 1.506(13) . ?
C37' N6 1.542(13) . ?
C37' H37C 0.9700 . ?
C37' H37D 0.9700 . ?
C38' C39' 1.570(14) . ?
C38' H38C 0.9700 . ?
C38' H38D 0.9700 . ?
C39' C40' 1.522(16) . ?
C39' H39C 0.9700 . ?
C39' H39D 0.9700 . ?
C40' H40D 0.9600 . ?
C40' H40E 0.9600 . ?
C40' H40F 0.9600 . ?
C41 C42 1.462(11) . ?
C41 N6 1.592(9) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.658(12) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.461(12) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C46 1.524(9) . ?
C45 N6 1.533(7) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.505(9) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.453(16) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
N1 Cu1 1.967(7) . ?
N2 C11 1.518(15) . ?
N2 C11' 1.556(13) . ?
N2 Cu1 1.934(6) . ?
N3 Cu1 1.936(7) . ?
N4 Cu1 1.942(7) . ?
C11 C13 1.527(14) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C14 1.503(16) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C11' C13' 1.508(14) . ?
C11' H11C 0.9700 . ?
C11' H11D 0.9700 . ?
C13' C14' 1.520(15) . ?
C13' H13C 0.9700 . ?
C13' H13D 0.9700 . ?
C14' H14D 0.9600 . ?
C14' H14E 0.9600 . ?
C14' H14F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N1 128.2(10) . . ?
O1 C1 C2 121.1(6) . . ?
N1 C1 C2 110.7(7) . . ?
O2 C2 N2 127.6(9) . . ?
O2 C2 C1 117.4(7) . . ?
N2 C2 C1 115.0(6) . . ?
O3 C3 N3 132.8(13) . . ?
O3 C3 C4 117.7(10) . . ?
N3 C3 C4 109.4(7) . . ?
O4 C4 N4 122.1(13) . . ?
O4 C4 C3 122.0(8) . . ?
N4 C4 C3 115.9(8) . . ?
N1 C5 C6 124.7(7) . . ?
N1 C5 C10 115.3(7) . . ?
C6 C5 C10 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 120.0 . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 120.0 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 C5 120.0 . . ?
C9 C10 N3 126.7(6) . . ?
C5 C10 N3 113.3(6) . . ?
N4 C12 C15 114.4(6) . . ?
N4 C12 H12A 108.7 . . ?
C15 C12 H12A 108.7 . . ?
N4 C12 H12B 108.7 . . ?
C15 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
C16 C15 C12 111.8(7) . . ?
C16 C15 H15A 109.3 . . ?
C12 C15 H15A 109.3 . . ?
C16 C15 H15B 109.3 . . ?
C12 C15 H15B 109.3 . . ?
H15A C15 H15B 107.9 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 N5 109(3) . . ?
C18 C17 H17A 109.8 . . ?
N5 C17 H17A 109.8 . . ?
C18 C17 H17B 109.8 . . ?
N5 C17 H17B 109.8 . . ?
H17A C17 H17B 108.3 . . ?
C17 C18 C19 111(3) . . ?
C17 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 112(3) . . ?
C20 C19 H19A 109.2 . . ?
C18 C19 H19A 109.2 . . ?
C20 C19 H19B 109.2 . . ?
C18 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18' C17' N5 116.1(9) . . ?
C18' C17' H17C 108.3 . . ?
N5 C17' H17C 108.3 . . ?
C18' C17' H17D 108.3 . . ?
N5 C17' H17D 108.3 . . ?
H17C C17' H17D 107.4 . . ?
C17' C18' C19' 110.6(11) . . ?
C17' C18' H18C 109.5 . . ?
C19' C18' H18C 109.5 . . ?
C17' C18' H18D 109.5 . . ?
C19' C18' H18D 109.5 . . ?
H18C C18' H18D 108.1 . . ?
C20' C19' C18' 112.6(12) . . ?
C20' C19' H19C 109.1 . . ?
C18' C19' H19C 109.1 . . ?
C20' C19' H19D 109.1 . . ?
C18' C19' H19D 109.1 . . ?
H19C C19' H19D 107.8 . . ?
C19' C20' H20D 109.5 . . ?
C19' C20' H20E 109.5 . . ?
H20D C20' H20E 109.5 . . ?
C19' C20' H20F 109.5 . . ?
H20D C20' H20F 109.5 . . ?
H20E C20' H20F 109.5 . . ?
C22 C21 N5 113.9(16) . . ?
C22 C21 H21A 108.8 . . ?
N5 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
N5 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C21 C22 C23 112.9(14) . . ?
C21 C22 H22A 109.0 . . ?
C23 C22 H22A 109.0 . . ?
C21 C22 H22B 109.0 . . ?
C23 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C24 C23 C22 114.4(16) . . ?
C24 C23 H23A 108.7 . . ?
C22 C23 H23A 108.7 . . ?
C24 C23 H23B 108.7 . . ?
C22 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22' C21' N5 117.2(10) . . ?
C22' C21' H21C 108.0 . . ?
N5 C21' H21C 108.0 . . ?
C22' C21' H21D 108.0 . . ?
N5 C21' H21D 108.0 . . ?
H21C C21' H21D 107.2 . . ?
C21' C22' C23' 108.3(10) . . ?
C21' C22' H22C 110.0 . . ?
C23' C22' H22C 110.0 . . ?
C21' C22' H22D 110.0 . . ?
C23' C22' H22D 110.0 . . ?
H22C C22' H22D 108.4 . . ?
C24' C23' C22' 107.3(12) . . ?
C24' C23' H23C 110.3 . . ?
C22' C23' H23C 110.3 . . ?
C24' C23' H23D 110.3 . . ?
C22' C23' H23D 110.3 . . ?
H23C C23' H23D 108.5 . . ?
C23' C24' H24D 109.5 . . ?
C23' C24' H24E 109.5 . . ?
H24D C24' H24E 109.5 . . ?
C23' C24' H24F 109.5 . . ?
H24D C24' H24F 109.5 . . ?
H24E C24' H24F 109.5 . . ?
C26 C25 N5 122(3) . . ?
C26 C25 H25A 106.9 . . ?
N5 C25 H25A 106.9 . . ?
C26 C25 H25B 106.9 . . ?
N5 C25 H25B 106.9 . . ?
H25A C25 H25B 106.7 . . ?
C25 C26 C27 121(3) . . ?
C25 C26 H26A 107.1 . . ?
C27 C26 H26A 107.1 . . ?
C25 C26 H26B 107.1 . . ?
C27 C26 H26B 107.1 . . ?
H26A C26 H26B 106.8 . . ?
C28 C27 C26 111(3) . . ?
C28 C27 H27A 109.3 . . ?
C26 C27 H27A 109.3 . . ?
C28 C27 H27B 109.3 . . ?
C26 C27 H27B 109.3 . . ?
H27A C27 H27B 108.0 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N5 C25' C26' 110.6(8) . . ?
N5 C25' H25C 109.5 . . ?
C26' C25' H25C 109.5 . . ?
N5 C25' H25D 109.5 . . ?
C26' C25' H25D 109.5 . . ?
H25C C25' H25D 108.1 . . ?
C25' C26' C27' 101.3(11) . . ?
C25' C26' H26C 111.5 . . ?
C27' C26' H26C 111.5 . . ?
C25' C26' H26D 111.5 . . ?
C27' C26' H26D 111.5 . . ?
H26C C26' H26D 109.3 . . ?
C26' C27' C28' 111.0(9) . . ?
C26' C27' H27C 109.4 . . ?
C28' C27' H27C 109.4 . . ?
C26' C27' H27D 109.4 . . ?
C28' C27' H27D 109.4 . . ?
H27C C27' H27D 108.0 . . ?
C27' C28' H28D 109.5 . . ?
C27' C28' H28E 109.5 . . ?
H28D C28' H28E 109.5 . . ?
C27' C28' H28F 109.5 . . ?
H28D C28' H28F 109.5 . . ?
H28E C28' H28F 109.5 . . ?
N5 C29 C30 115.5(4) . . ?
N5 C29 H29A 108.4 . . ?
C30 C29 H29A 108.4 . . ?
N5 C29 H29B 108.4 . . ?
C30 C29 H29B 108.4 . . ?
H29A C29 H29B 107.5 . . ?
C29 C30 C31 107.8(5) . . ?
C29 C30 H30A 110.1 . . ?
C31 C30 H30A 110.1 . . ?
C29 C30 H30B 110.1 . . ?
C31 C30 H30B 110.1 . . ?
H30A C30 H30B 108.5 . . ?
C30 C31 C32 109.8(5) . . ?
C30 C31 H31A 109.7 . . ?
C32 C31 H31A 109.7 . . ?
C30 C31 H31B 109.7 . . ?
C32 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N6 C33 C34 114.8(10) . . ?
N6 C33 H33A 108.6 . . ?
C34 C33 H33A 108.6 . . ?
N6 C33 H33B 108.6 . . ?
C34 C33 H33B 108.6 . . ?
H33A C33 H33B 107.6 . . ?
C35 C34 C33 111.5(12) . . ?
C35 C34 H34A 109.3 . . ?
C33 C34 H34A 109.3 . . ?
C35 C34 H34B 109.3 . . ?
C33 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?
C34 C35 C36 115.8(10) . . ?
C34 C35 H35A 108.3 . . ?
C36 C35 H35A 108.3 . . ?
C34 C35 H35B 108.3 . . ?
C36 C35 H35B 108.3 . . ?
H35A C35 H35B 107.4 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N6 C33' C34' 112(2) . . ?
N6 C33' H33C 109.2 . . ?
C34' C33' H33C 109.2 . . ?
N6 C33' H33D 109.2 . . ?
C34' C33' H33D 109.2 . . ?
H33C C33' H33D 107.9 . . ?
C35' C34' C33' 105.2(18) . . ?
C35' C34' H34C 110.7 . . ?
C33' C34' H34C 110.7 . . ?
C35' C34' H34D 110.7 . . ?
C33' C34' H34D 110.7 . . ?
H34C C34' H34D 108.8 . . ?
C34' C35' C36' 110.1(18) . . ?
C34' C35' H35C 109.6 . . ?
C36' C35' H35C 109.6 . . ?
C34' C35' H35D 109.6 . . ?
C36' C35' H35D 109.6 . . ?
H35C C35' H35D 108.2 . . ?
C35' C36' H36D 109.5 . . ?
C35' C36' H36E 109.5 . . ?
H36D C36' H36E 109.5 . . ?
C35' C36' H36F 109.5 . . ?
H36D C36' H36F 109.5 . . ?
H36E C36' H36F 109.5 . . ?
C38 C37 N6 113.8(19) . . ?
C38 C37 H37A 108.8 . . ?
N6 C37 H37A 108.8 . . ?
C38 C37 H37B 108.8 . . ?
N6 C37 H37B 108.8 . . ?
H37A C37 H37B 107.7 . . ?
C37 C38 C39 107.9(16) . . ?
C37 C38 H38A 110.1 . . ?
C39 C38 H38A 110.1 . . ?
C37 C38 H38B 110.1 . . ?
C39 C38 H38B 110.1 . . ?
H38A C38 H38B 108.4 . . ?
C40 C39 C38 113.4(16) . . ?
C40 C39 H39A 108.9 . . ?
C38 C39 H39A 108.9 . . ?
C40 C39 H39B 108.9 . . ?
C38 C39 H39B 108.9 . . ?
H39A C39 H39B 107.7 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38' C37' N6 117.1(12) . . ?
C38' C37' H37C 108.0 . . ?
N6 C37' H37C 108.0 . . ?
C38' C37' H37D 108.0 . . ?
N6 C37' H37D 108.0 . . ?
H37C C37' H37D 107.3 . . ?
C37' C38' C39' 114.0(12) . . ?
C37' C38' H38C 108.7 . . ?
C39' C38' H38C 108.7 . . ?
C37' C38' H38D 108.7 . . ?
C39' C38' H38D 108.7 . . ?
H38C C38' H38D 107.6 . . ?
C40' C39' C38' 114.7(14) . . ?
C40' C39' H39C 108.6 . . ?
C38' C39' H39C 108.6 . . ?
C40' C39' H39D 108.6 . . ?
C38' C39' H39D 108.6 . . ?
H39C C39' H39D 107.6 . . ?
C39' C40' H40D 109.5 . . ?
C39' C40' H40E 109.5 . . ?
H40D C40' H40E 109.5 . . ?
C39' C40' H40F 109.5 . . ?
H40D C40' H40F 109.5 . . ?
H40E C40' H40F 109.5 . . ?
C42 C41 N6 116.5(6) . . ?
C42 C41 H41A 108.2 . . ?
N6 C41 H41A 108.2 . . ?
C42 C41 H41B 108.2 . . ?
N6 C41 H41B 108.2 . . ?
H41A C41 H41B 107.3 . . ?
C41 C42 C43 111.9(7) . . ?
C41 C42 H42A 109.2 . . ?
C43 C42 H42A 109.2 . . ?
C41 C42 H42B 109.2 . . ?
C43 C42 H42B 109.2 . . ?
H42A C42 H42B 107.9 . . ?
C44 C43 C42 111.3(9) . . ?
C44 C43 H43A 109.4 . . ?
C42 C43 H43A 109.4 . . ?
C44 C43 H43B 109.4 . . ?
C42 C43 H43B 109.4 . . ?
H43A C43 H43B 108.0 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 N6 114.6(4) . . ?
C46 C45 H45A 108.6 . . ?
N6 C45 H45A 108.6 . . ?
C46 C45 H45B 108.6 . . ?
N6 C45 H45B 108.6 . . ?
H45A C45 H45B 107.6 . . ?
C47 C46 C45 109.0(6) . . ?
C47 C46 H46A 109.9 . . ?
C45 C46 H46A 109.9 . . ?
C47 C46 H46B 109.9 . . ?
C45 C46 H46B 109.9 . . ?
H46A C46 H46B 108.3 . . ?
C48 C47 C46 107.3(11) . . ?
C48 C47 H47A 110.3 . . ?
C46 C47 H47A 110.3 . . ?
C48 C47 H47B 110.3 . . ?
C46 C47 H47B 110.3 . . ?
H47A C47 H47B 108.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C1 N1 C5 129.7(8) . . ?
C1 N1 Cu1 115.1(6) . . ?
C5 N1 Cu1 115.1(5) . . ?
C2 N2 C11 112.0(8) . . ?
C2 N2 C11' 117.5(7) . . ?
C11 N2 C11' 30.9(5) . . ?
C2 N2 Cu1 115.4(6) . . ?
C11 N2 Cu1 127.9(7) . . ?
C11' N2 Cu1 126.0(6) . . ?
C3 N3 C10 128.1(8) . . ?
C3 N3 Cu1 116.0(8) . . ?
C10 N3 Cu1 115.4(4) . . ?
C4 N4 C12 115.3(8) . . ?
C4 N4 Cu1 113.3(8) . . ?
C12 N4 Cu1 130.8(4) . . ?
C25' N5 C29 116.1(8) . . ?
C25' N5 C17' 104.7(8) . . ?
C29 N5 C17' 110.0(6) . . ?
C25' N5 C25 13(2) . . ?
C29 N5 C25 103.4(17) . . ?
C17' N5 C25 111.3(19) . . ?
C25' N5 C21 93.5(15) . . ?
C29 N5 C21 107.3(9) . . ?
C17' N5 C21 124.8(13) . . ?
C25 N5 C21 98(3) . . ?
C25' N5 C17 97(2) . . ?
C29 N5 C17 127(3) . . ?
C17' N5 C17 17(3) . . ?
C25 N5 C17 106(2) . . ?
C21 N5 C17 111(3) . . ?
C25' N5 C21' 115.7(11) . . ?
C29 N5 C21' 105.3(7) . . ?
C17' N5 C21' 104.5(9) . . ?
C25 N5 C21' 122(2) . . ?
C21 N5 C21' 25.4(18) . . ?
C17 N5 C21' 95(3) . . ?
C33' N6 C37 110(2) . . ?
C33' N6 C33 11.1(16) . . ?
C37 N6 C33 99.5(19) . . ?
C33' N6 C45 108.0(14) . . ?
C37 N6 C45 104.0(12) . . ?
C33 N6 C45 114.4(8) . . ?
C33' N6 C37' 124.8(18) . . ?
C37 N6 C37' 18(2) . . ?
C33 N6 C37' 113.7(12) . . ?
C45 N6 C37' 106.0(7) . . ?
C33' N6 C41 105.0(13) . . ?
C37 N6 C41 121.3(17) . . ?
C33 N6 C41 109.9(7) . . ?
C45 N6 C41 107.8(6) . . ?
C37' N6 C41 104.3(13) . . ?
N2 Cu1 N3 163.9(3) . . ?
N2 Cu1 N4 111.9(3) . . ?
N3 Cu1 N4 84.2(3) . . ?
N2 Cu1 N1 83.2(3) . . ?
N3 Cu1 N1 80.8(3) . . ?
N4 Cu1 N1 164.9(3) . . ?
N2 C11 C13 90.2(12) . . ?
N2 C11 H11A 113.6 . . ?
C13 C11 H11A 113.6 . . ?
N2 C11 H11B 113.6 . . ?
C13 C11 H11B 113.6 . . ?
H11A C11 H11B 110.9 . . ?
C14 C13 C11 106.0(13) . . ?
C14 C13 H13A 110.5 . . ?
C11 C13 H13A 110.5 . . ?
C14 C13 H13B 110.5 . . ?
C11 C13 H13B 110.5 . . ?
H13A C13 H13B 108.7 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13' C11' N2 109.1(11) . . ?
C13' C11' H11C 109.9 . . ?
N2 C11' H11C 109.9 . . ?
C13' C11' H11D 109.9 . . ?
N2 C11' H11D 109.9 . . ?
H11C C11' H11D 108.3 . . ?
C11' C13' C14' 113.8(12) . . ?
C11' C13' H13C 108.8 . . ?
C14' C13' H13C 108.8 . . ?
C11' C13' H13D 108.8 . . ?
C14' C13' H13D 108.8 . . ?
H13C C13' H13D 107.7 . . ?
C13' C14' H14D 109.5 . . ?
C13' C14' H14E 109.5 . . ?
H14D C14' H14E 109.5 . . ?
C13' C14' H14F 109.5 . . ?
H14D C14' H14F 109.5 . . ?
H14E C14' H14F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 O2 7.7(9) . . . . ?
N1 C1 C2 O2 -172.0(5) . . . . ?
O1 C1 C2 N2 -174.4(6) . . . . ?
N1 C1 C2 N2 5.9(7) . . . . ?
O3 C3 C4 O4 8.0(10) . . . . ?
N3 C3 C4 O4 -168.4(5) . . . . ?
O3 C3 C4 N4 -171.9(5) . . . . ?
N3 C3 C4 N4 11.7(8) . . . . ?
N1 C5 C6 C7 -178.9(4) . . . . ?
C10 C5 C6 C7 0.0 . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C8 C9 C10 C5 0.0 . . . . ?
C8 C9 C10 N3 179.9(5) . . . . ?
N1 C5 C10 C9 179.0(4) . . . . ?
C6 C5 C10 C9 0.0 . . . . ?
N1 C5 C10 N3 -0.9(4) . . . . ?
C6 C5 C10 N3 -179.9(5) . . . . ?
N4 C12 C15 C16 -178.2(6) . . . . ?
N5 C17 C18 C19 150(8) . . . . ?
C17 C18 C19 C20 159(7) . . . . ?
N5 C17' C18' C19' 179.0(13) . . . . ?
C17' C18' C19' C20' 178.7(17) . . . . ?
N5 C21 C22 C23 -154(2) . . . . ?
C21 C22 C23 C24 72(3) . . . . ?
N5 C21' C22' C23' 174.3(16) . . . . ?
C21' C22' C23' C24' 178.5(15) . . . . ?
N5 C25 C26 C27 148(4) . . . . ?
C25 C26 C27 C28 100(4) . . . . ?
N5 C25' C26' C27' -176.7(11) . . . . ?
C25' C26' C27' C28' 175.3(11) . . . . ?
N5 C29 C30 C31 -173.9(7) . . . . ?
C29 C30 C31 C32 -175.5(6) . . . . ?
N6 C33 C34 C35 175.6(11) . . . . ?
C33 C34 C35 C36 174.7(14) . . . . ?
N6 C33' C34' C35' -176(3) . . . . ?
C33' C34' C35' C36' -180(3) . . . . ?
N6 C37 C38 C39 146(4) . . . . ?
C37 C38 C39 C40 -165(3) . . . . ?
N6 C37' C38' C39' 175(2) . . . . ?
C37' C38' C39' C40' 171(3) . . . . ?
N6 C41 C42 C43 174.7(6) . . . . ?
C41 C42 C43 C44 -68.3(10) . . . . ?
N6 C45 C46 C47 -175.5(9) . . . . ?
C45 C46 C47 C48 80.1(12) . . . . ?
O1 C1 N1 C5 -4.0(10) . . . . ?
C2 C1 N1 C5 175.6(5) . . . . ?
O1 C1 N1 Cu1 171.7(5) . . . . ?
C2 C1 N1 Cu1 -8.7(6) . . . . ?
C6 C5 N1 C1 -6.3(7) . . . . ?
C10 C5 N1 C1 174.8(4) . . . . ?
C6 C5 N1 Cu1 178.0(2) . . . . ?
C10 C5 N1 Cu1 -1.0(4) . . . . ?
O2 C2 N2 C11 -24.8(10) . . . . ?
C1 C2 N2 C11 157.6(7) . . . . ?
O2 C2 N2 C11' 8.9(11) . . . . ?
C1 C2 N2 C11' -168.8(7) . . . . ?
O2 C2 N2 Cu1 177.4(5) . . . . ?
C1 C2 N2 Cu1 -0.2(7) . . . . ?
O3 C3 N3 C10 2.0(11) . . . . ?
C4 C3 N3 C10 177.7(6) . . . . ?
O3 C3 N3 Cu1 173.1(6) . . . . ?
C4 C3 N3 Cu1 -11.3(7) . . . . ?
C9 C10 N3 C3 -6.4(8) . . . . ?
C5 C10 N3 C3 173.5(5) . . . . ?
C9 C10 N3 Cu1 -177.5(2) . . . . ?
C5 C10 N3 Cu1 2.4(5) . . . . ?
O4 C4 N4 C12 1.9(8) . . . . ?
C3 C4 N4 C12 -178.2(5) . . . . ?
O4 C4 N4 Cu1 173.6(4) . . . . ?
C3 C4 N4 Cu1 -6.5(7) . . . . ?
C15 C12 N4 C4 86.7(7) . . . . ?
C15 C12 N4 Cu1 -83.2(7) . . . . ?
C26' C25' N5 C29 57.8(12) . . . . ?
C26' C25' N5 C17' 179.3(10) . . . . ?
C26' C25' N5 C25 56(11) . . . . ?
C26' C25' N5 C21 -53.3(15) . . . . ?
C26' C25' N5 C17 -165(3) . . . . ?
C26' C25' N5 C21' -66.3(13) . . . . ?
C30 C29 N5 C25' 62.3(10) . . . . ?
C30 C29 N5 C17' -56.3(10) . . . . ?
C30 C29 N5 C25 63(2) . . . . ?
C30 C29 N5 C21 165.2(16) . . . . ?
C30 C29 N5 C17 -60(3) . . . . ?
C30 C29 N5 C21' -168.4(10) . . . . ?
C18' C17' N5 C25' 171.8(17) . . . . ?
C18' C17' N5 C29 -62.8(18) . . . . ?
C18' C17' N5 C25 -177(3) . . . . ?
C18' C17' N5 C21 67(2) . . . . ?
C18' C17' N5 C17 107(10) . . . . ?
C18' C17' N5 C21' 49.8(18) . . . . ?
C26 C25 N5 C25' -129(14) . . . . ?
C26 C25 N5 C29 53(5) . . . . ?
C26 C25 N5 C17' 171(4) . . . . ?
C26 C25 N5 C21 -57(4) . . . . ?
C26 C25 N5 C17 -172(5) . . . . ?
C26 C25 N5 C21' -65(5) . . . . ?
C22 C21 N5 C25' -56(2) . . . . ?
C22 C21 N5 C29 -175(2) . . . . ?
C22 C21 N5 C17' 55(3) . . . . ?
C22 C21 N5 C25 -68(3) . . . . ?
C22 C21 N5 C17 43(4) . . . . ?
C22 C21 N5 C21' 96(4) . . . . ?
C18 C17 N5 C25' -163(7) . . . . ?
C18 C17 N5 C29 -33(8) . . . . ?
C18 C17 N5 C17' -44(7) . . . . ?
C18 C17 N5 C25 -154(7) . . . . ?
C18 C17 N5 C21 101(7) . . . . ?
C18 C17 N5 C21' 81(7) . . . . ?
C22' C21' N5 C25' -57.9(16) . . . . ?
C22' C21' N5 C29 172.5(13) . . . . ?
C22' C21' N5 C17' 56.6(16) . . . . ?
C22' C21' N5 C25 -71(2) . . . . ?
C22' C21' N5 C21 -89(3) . . . . ?
C22' C21' N5 C17 42(3) . . . . ?
C34' C33' N6 C37 35(3) . . . . ?
C34' C33' N6 C33 50(9) . . . . ?
C34' C33' N6 C45 -78(3) . . . . ?
C34' C33' N6 C37' 48(4) . . . . ?
C34' C33' N6 C41 168(3) . . . . ?
C38 C37 N6 C33' 67(3) . . . . ?
C38 C37 N6 C33 64(3) . . . . ?
C38 C37 N6 C45 -178(2) . . . . ?
C38 C37 N6 C37' -79(5) . . . . ?
C38 C37 N6 C41 -56(3) . . . . ?
C34 C33 N6 C33' -110(10) . . . . ?
C34 C33 N6 C37 56.2(19) . . . . ?
C34 C33 N6 C45 -54.0(15) . . . . ?
C34 C33 N6 C37' 68.1(18) . . . . ?
C34 C33 N6 C41 -175.4(12) . . . . ?
C46 C45 N6 C33' -41.8(16) . . . . ?
C46 C45 N6 C37 -159(2) . . . . ?
C46 C45 N6 C33 -51.5(11) . . . . ?
C46 C45 N6 C37' -177.6(15) . . . . ?
C46 C45 N6 C41 71.1(8) . . . . ?
C38' C37' N6 C33' 58(3) . . . . ?
C38' C37' N6 C37 98(6) . . . . ?
C38' C37' N6 C33 57(2) . . . . ?
C38' C37' N6 C45 -176.0(15) . . . . ?
C38' C37' N6 C41 -62.3(19) . . . . ?
C42 C41 N6 C33' 167.7(16) . . . . ?
C42 C41 N6 C37 -67(2) . . . . ?
C42 C41 N6 C33 178.1(9) . . . . ?
C42 C41 N6 C45 52.8(8) . . . . ?
C42 C41 N6 C37' -59.6(11) . . . . ?
C2 N2 Cu1 N3 -9.8(11) . . . . ?
C11 N2 Cu1 N3 -163.4(8) . . . . ?
C11' N2 Cu1 N3 157.7(8) . . . . ?
C2 N2 Cu1 N4 175.4(4) . . . . ?
C11 N2 Cu1 N4 21.8(8) . . . . ?
C11' N2 Cu1 N4 -17.1(8) . . . . ?
C2 N2 Cu1 N1 -3.5(5) . . . . ?
C11 N2 Cu1 N1 -157.2(8) . . . . ?
C11' N2 Cu1 N1 163.9(7) . . . . ?
C3 N3 Cu1 N2 -168.2(7) . . . . ?
C10 N3 Cu1 N2 4.0(11) . . . . ?
C3 N3 Cu1 N4 6.9(5) . . . . ?
C10 N3 Cu1 N4 179.2(4) . . . . ?
C3 N3 Cu1 N1 -174.5(5) . . . . ?
C10 N3 Cu1 N1 -2.3(4) . . . . ?
C4 N4 Cu1 N2 178.8(4) . . . . ?
C12 N4 Cu1 N2 -11.1(6) . . . . ?
C4 N4 Cu1 N3 0.3(4) . . . . ?
C12 N4 Cu1 N3 170.4(5) . . . . ?
C4 N4 Cu1 N1 -5.1(10) . . . . ?
C12 N4 Cu1 N1 164.9(6) . . . . ?
C1 N1 Cu1 N2 7.2(4) . . . . ?
C5 N1 Cu1 N2 -176.5(4) . . . . ?
C1 N1 Cu1 N3 -174.6(4) . . . . ?
C5 N1 Cu1 N3 1.8(3) . . . . ?
C1 N1 Cu1 N4 -169.1(6) . . . . ?
C5 N1 Cu1 N4 7.2(9) . . . . ?
C2 N2 C11 C13 96.7(11) . . . . ?
C11' N2 C11 C13 -10.4(14) . . . . ?
Cu1 N2 C11 C13 -108.9(11) . . . . ?
N2 C11 C13 C14 -178.8(13) . . . . ?
C2 N2 C11' C13' -90.7(11) . . . . ?
C11 N2 C11' C13' -3.4(16) . . . . ?
Cu1 N2 C11' C13' 102.1(11) . . . . ?
N2 C11' C13' C14' -177.0(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        59.99
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.052
####################################################################### 
# 
# 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_abdul306
_database_code_depnum_ccdc_archive 'CCDC 1035433'
_audit_update_record             
;
2014-11-21 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H56 Cu3 N10 O4, 2(C24 H20 B)'
_chemical_formula_sum            'C78 H96 B2 Cu3 N10 O4'
_chemical_formula_weight         1449.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.7472(5)
_cell_length_b                   14.0699(5)
_cell_length_c                   19.3586(8)
_cell_angle_alpha                103.343(3)
_cell_angle_beta                 100.238(3)
_cell_angle_gamma                91.599(3)
_cell_volume                     3576.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7876
_cell_measurement_theta_min      3.1849
_cell_measurement_theta_max      64.1050


_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1526
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Gemini S'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  10
_diffrn_standards_decay_%        0

_diffrn_reflns_number            21468
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.24
_diffrn_reflns_theta_max         62.00
_reflns_number_total             11034
_reflns_number_gt                9937
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2sigma(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.
 In case this compound the trinuclear and dicationic complex fragment has been 
refined disordered on two positions with all of its non-hydrogen atoms. 
This disorder resembles a statistical disorder, whereby the complex fragments 
are arranged in top versus down orientation with respect to each other. 
The finally obtained, freely calculated occupation factors amounts to 0.68 
versus 0.32. Several atoms appear as disordered further as indicated by 
level A to C alerts by the checkcif procedure due to high Ueq values and 
large Hirshfeld Test differences when compared to neighbours. Their disorder 
could not be solved and refined reliable, which is mostly attributed to the 
already poor ratio of reflections to parameters. 

 The following restraints have been used for refinement:
DFIX     2.200   0.020 CU3A N8A
DFIX     1.500   0.020 C22A N8A
DFIX     1.500   0.020 N8A C23A
DFIX     1.500   0.020 N9A C26A
DFIX     1.500   0.020 C24A C25A
DFIX     1.500   0.020 N8A C24A
DFIX     1.500   0.020 N9A C25A
DFIX     1.500   0.020 N9A C27A
DFIX     1.500   0.020 C27A C28A
DFIX     1.500   0.020 N10 C29A
DFIX     1.450   0.020 N2A C11A
DFIX     1.500   0.020 N5A C14A
DFIX     1.500   0.020 N5A C13A
DFIX     1.500   0.020 C15A C16A
DFIX     1.500   0.020 C18A C19A
DFIX     1.500   0.020 N6A C18A
DFIX     1.500   0.020 C19A N7
DFIX     1.500   0.020 N7 C20A
DFIX     1.500   0.020 C21A N7
DANG     2.500   0.040 C13A C14A
DANG     2.500   0.040 C22A C23A
DANG     2.500   0.040 C22A C24A
DANG     2.500   0.040 C23A C24A
DANG     2.500   0.040 C25A C26A
DANG     2.500   0.040 C25A C27A
DANG     2.500   0.040 C26A C27A
DANG     2.500   0.040 C28A C29A
DELU     0.002   0.002 C5A C6A C7A C8A C9A C10A C11A C12A N1A N2A N3A
DELU     0.002   0.002 C4A CU1A C4A C3A C3A C4A O4A O3A O3A O4A
SIMU     0.005   0.010   1.700 C5A C6A C7A C8A C9A C10A C11A C12A N1A
SIMU     0.005   0.010 1.700 N2A N3A C4A CU1A C4A C3A C3A C4A O4A O3A O3A O4A
ISOR     0.100 C5A C6A C7A C8A C9A C10A C11A C12A N1A N2A N3A C4A CU1A
ISOR     0.100 C1A C2A C3A C4A O1A O2A O3A O4A
DELU     0.010   0.010 C13A C14A C15A C16A C17A C18A C19A C20A C21A
DELU     0.010   0.010 N5A N6A CU2A
SIMU     0.040   0.080   1.700 C13A C14A C15A C16A C17A C18A C19A C20A
SIMU     0.040   0.080   1.700 C21A N5A N6A CU2A
ISOR     0.100 C13A C14A C15A C16A C17A C18A C19A C20A C21A N5A N6A
ISOR     0.100 CU2A
DELU     0.010   0.010 C22A C23A C24A C25A C26A C27A C28A C29A C30A
DELU     0.010   0.010 N8A N9A CU3A
SIMU     0.040   0.080   1.700 C22A C23A C24A C25A C26A C27A C28A C29A
SIMU     0.040   0.080   1.700 C30A N8A N9A CU3A
ISOR     0.100 C22A C23A C24A C25A C26A C27A C28A C29A C30A N8A N9A
ISOR     0.100 CU3A
DFIX     1.400   0.020 C3A C4A
DFIX     1.400   0.020 N2A C2A
DFIX     1.200   0.020 C3A O3A
DFIX     1.200   0.020 C4A O4A
DFIX     1.400   0.020 C4A N4A
DFIX     1.400   0.020 C3A N3A
DFIX     1.200   0.020 C3A O3A
DFIX     1.200   0.020 C4A O4A
DFIX     1.400   0.020 C4A N4A
DANG     2.250   0.040 N4A O4A
DANG     2.250   0.040 N1 O1
DANG     2.250   0.040 N1A O1A
DFIX     1.400   0.020 C4A C3A
EADP C1A C3A
EADP C2A C4A
EADP O1A O4A
EADP C17A C23A
EADP C26A C27A


;

_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)+(0.0914P)²+15.8424P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11034
_refine_ls_number_parameters     1238
_refine_ls_number_restraints     434
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0987
_refine_ls_wR_factor_ref         0.2479
_refine_ls_wR_factor_gt          0.2442
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.004

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
B1 B 0.6654(5) 0.2725(5) 0.8773(4) 0.0540(17) Uani 1 1 d . . .
B2 B 0.1677(5) 0.3002(6) 0.3648(4) 0.060(2) Uani 1 1 d . . .
C31 C 0.6033(4) 0.3364(5) 0.8266(3) 0.0540(15) Uani 1 1 d . . .
C32 C 0.5003(5) 0.3415(5) 0.8194(3) 0.0564(15) Uani 1 1 d . . .
H32 H 0.4667 0.3034 0.8423 0.068 Uiso 1 1 calc R . .
C33 C 0.4468(5) 0.3982(6) 0.7814(3) 0.0652(18) Uani 1 1 d . . .
H33 H 0.3784 0.3962 0.7779 0.078 Uiso 1 1 calc R . .
C34 C 0.4921(5) 0.4596(6) 0.7473(3) 0.071(2) Uani 1 1 d . . .
H34 H 0.4559 0.5003 0.7224 0.085 Uiso 1 1 calc R . .
C35 C 0.5938(5) 0.4569(6) 0.7524(3) 0.0637(18) Uani 1 1 d . . .
H35 H 0.6271 0.4963 0.7303 0.076 Uiso 1 1 calc R . .
C36 C 0.6464(5) 0.3967(6) 0.7898(3) 0.0653(19) Uani 1 1 d . . .
H36 H 0.7142 0.3957 0.7907 0.078 Uiso 1 1 calc R . .
C37 C 0.6928(5) 0.3422(5) 0.9608(3) 0.0584(16) Uani 1 1 d . . .
C38 C 0.6249(4) 0.4026(4) 0.9906(3) 0.0463(13) Uani 1 1 d . . .
H38 H 0.5655 0.4088 0.9608 0.056 Uiso 1 1 calc R . .
C39 C 0.6412(5) 0.4542(5) 1.0623(3) 0.0583(16) Uani 1 1 d . . .
H39 H 0.5936 0.4940 1.0795 0.070 Uiso 1 1 calc R . .
C40 C 0.7273(6) 0.4465(8) 1.1078(4) 0.107(4) Uani 1 1 d . . .
H40 H 0.7392 0.4807 1.1560 0.129 Uiso 1 1 calc R . .
C41 C 0.7966(7) 0.3859(10) 1.0800(5) 0.164(7) Uani 1 1 d . . .
H41 H 0.8565 0.3813 1.1096 0.196 Uiso 1 1 calc R . .
C42 C 0.7776(6) 0.3333(8) 1.0098(4) 0.112(4) Uani 1 1 d . . .
H42 H 0.8230 0.2896 0.9940 0.135 Uiso 1 1 calc R . .
C43 C 0.6000(4) 0.1739(5) 0.8780(4) 0.0600(17) Uani 1 1 d . . .
C44 C 0.5327(4) 0.1199(5) 0.8168(4) 0.0631(18) Uani 1 1 d . . .
H44 H 0.5203 0.1443 0.7756 0.076 Uiso 1 1 calc R . .
C45 C 0.4849(5) 0.0320(5) 0.8161(5) 0.070(2) Uani 1 1 d . . .
H45 H 0.4411 -0.0016 0.7747 0.084 Uiso 1 1 calc R . .
C46 C 0.5014(5) -0.0069(6) 0.8766(5) 0.073(2) Uani 1 1 d . . .
H46 H 0.4683 -0.0654 0.8767 0.088 Uiso 1 1 calc R . .
C47 C 0.5663(6) 0.0423(6) 0.9350(5) 0.075(2) Uani 1 1 d . . .
H47 H 0.5792 0.0161 0.9754 0.090 Uiso 1 1 calc R . .
C48 C 0.6146(5) 0.1303(6) 0.9372(4) 0.0686(19) Uani 1 1 d . . .
H48 H 0.6583 0.1619 0.9792 0.082 Uiso 1 1 calc R . .
C49 C 0.7686(5) 0.2361(5) 0.8498(3) 0.0618(18) Uani 1 1 d . . .
C50 C 0.8501(5) 0.3033(5) 0.8542(3) 0.0622(17) Uani 1 1 d . . .
H50 H 0.8462 0.3693 0.8747 0.075 Uiso 1 1 calc R . .
C51 C 0.9364(5) 0.2726(6) 0.8284(4) 0.071(2) Uani 1 1 d . . .
H51 H 0.9876 0.3188 0.8311 0.086 Uiso 1 1 calc R . .
C52 C 0.9460(5) 0.1753(5) 0.7994(4) 0.0683(19) Uani 1 1 d . . .
H52 H 1.0033 0.1556 0.7826 0.082 Uiso 1 1 calc R . .
C53 C 0.8693(5) 0.1071(5) 0.7953(4) 0.072(2) Uani 1 1 d . . .
H53 H 0.8748 0.0410 0.7760 0.087 Uiso 1 1 calc R . .
C54 C 0.7840(5) 0.1383(5) 0.8203(4) 0.0676(19) Uani 1 1 d . . .
H54 H 0.7338 0.0909 0.8173 0.081 Uiso 1 1 calc R . .
C55 C 0.1958(4) 0.3671(5) 0.4495(3) 0.0545(15) Uani 1 1 d . . .
C56 C 0.1215(4) 0.4108(4) 0.4842(3) 0.0450(13) Uani 1 1 d . . .
H56 H 0.0565 0.4011 0.4587 0.054 Uiso 1 1 calc R . .
C57 C 0.1394(5) 0.4672(4) 0.5538(3) 0.0533(15) Uani 1 1 d . . .
H57 H 0.0871 0.4941 0.5744 0.064 Uiso 1 1 calc R . .
C58 C 0.2329(6) 0.4839(7) 0.5925(4) 0.087(3) Uani 1 1 d . . .
H58 H 0.2457 0.5226 0.6395 0.105 Uiso 1 1 calc R . .
C59 C 0.3097(6) 0.4420(9) 0.5608(4) 0.116(4) Uani 1 1 d . . .
H59 H 0.3747 0.4530 0.5863 0.139 Uiso 1 1 calc R . .
C60 C 0.2889(6) 0.3844(9) 0.4914(5) 0.116(4) Uani 1 1 d . . .
H60 H 0.3410 0.3555 0.4717 0.139 Uiso 1 1 calc R . .
C61 C 0.1030(5) 0.3659(5) 0.3159(3) 0.0583(16) Uani 1 1 d . . .
C62 C -0.0002(5) 0.3708(5) 0.3099(3) 0.0593(16) Uani 1 1 d . . .
H62 H -0.0333 0.3305 0.3315 0.071 Uiso 1 1 calc R . .
C63 C -0.0552(5) 0.4313(6) 0.2744(3) 0.069(2) Uani 1 1 d . . .
H63 H -0.1234 0.4302 0.2720 0.082 Uiso 1 1 calc R . .
C64 C -0.0093(5) 0.4943(6) 0.2419(3) 0.0617(17) Uani 1 1 d . . .
H64 H -0.0450 0.5362 0.2180 0.074 Uiso 1 1 calc R . .
C65 C 0.0920(5) 0.4911(6) 0.2472(3) 0.0625(17) Uani 1 1 d . . .
H65 H 0.1249 0.5320 0.2260 0.075 Uiso 1 1 calc R . .
C66 C 0.1447(5) 0.4315(5) 0.2815(3) 0.0589(17) Uani 1 1 d . . .
H66 H 0.2127 0.4332 0.2830 0.071 Uiso 1 1 calc R . .
C67 C 0.2686(5) 0.2667(5) 0.3335(3) 0.0606(17) Uani 1 1 d . . .
C68 C 0.3497(5) 0.3316(5) 0.3382(4) 0.0651(18) Uani 1 1 d . . .
H68 H 0.3463 0.3974 0.3599 0.078 Uiso 1 1 calc R . .
C69 C 0.4362(5) 0.3030(6) 0.3118(4) 0.0682(19) Uani 1 1 d . . .
H69 H 0.4871 0.3496 0.3150 0.082 Uiso 1 1 calc R . .
C70 C 0.4450(5) 0.2062(6) 0.2815(4) 0.077(2) Uani 1 1 d . . .
H70 H 0.5021 0.1867 0.2644 0.092 Uiso 1 1 calc R . .
C71 C 0.3678(5) 0.1374(6) 0.2763(4) 0.076(2) Uani 1 1 d . . .
H71 H 0.3731 0.0715 0.2561 0.091 Uiso 1 1 calc R . .
C72 C 0.2819(5) 0.1681(5) 0.3020(4) 0.071(2) Uani 1 1 d . . .
H72 H 0.2310 0.1211 0.2979 0.086 Uiso 1 1 calc R . .
C73 C 0.1014(4) 0.2012(5) 0.3642(3) 0.0532(15) Uani 1 1 d . . .
C74 C 0.0352(4) 0.1484(5) 0.3043(4) 0.0601(17) Uani 1 1 d . . .
H74 H 0.0231 0.1740 0.2636 0.072 Uiso 1 1 calc R . .
C75 C -0.0132(5) 0.0617(6) 0.3011(5) 0.072(2) Uani 1 1 d . . .
H75 H -0.0566 0.0294 0.2592 0.086 Uiso 1 1 calc R . .
C76 C 0.0026(5) 0.0214(5) 0.3614(5) 0.077(2) Uani 1 1 d . . .
H76 H -0.0312 -0.0372 0.3606 0.092 Uiso 1 1 calc R . .
C77 C 0.0698(5) 0.0706(5) 0.4226(4) 0.0715(19) Uani 1 1 d . . .
H77 H 0.0828 0.0446 0.4630 0.086 Uiso 1 1 calc R . .
C78 C 0.1174(5) 0.1591(5) 0.4225(4) 0.066(2) Uani 1 1 d . . .
H78 H 0.1621 0.1914 0.4638 0.079 Uiso 1 1 calc R . .
N7 N 0.3437(4) 1.2676(3) 1.0460(3) 0.0478(11) Uani 1 1 d D . .
N10 N 0.1523(4) 0.7458(4) 0.4461(3) 0.0548(13) Uani 1 1 d D . .
C1 C 0.2130(13) 1.1358(9) 0.8564(7) 0.052(3) Uani 0.676(2) 1 d P A 1
C2 C 0.2178(8) 1.0512(7) 0.8937(7) 0.045(2) Uani 0.676(2) 1 d P A 1
C3 C 0.2747(8) 0.9458(10) 0.6177(6) 0.043(3) Uani 0.676(2) 1 d P A 1
C4 C 0.2833(7) 0.8468(9) 0.6369(5) 0.041(3) Uani 0.676(2) 1 d P A 1
C5 C 0.2189(6) 1.1653(7) 0.7372(5) 0.049(2) Uani 0.676(2) 1 d P A 1
C6 C 0.1889(13) 1.2624(15) 0.7458(7) 0.045(3) Uani 0.676(2) 1 d P A 1
H6 H 0.1700 1.2954 0.7882 0.054 Uiso 0.676(2) 1 calc PR A 1
C7 C 0.1889(7) 1.3063(7) 0.6888(5) 0.059(2) Uani 0.676(2) 1 d P A 1
H7 H 0.1729 1.3710 0.6937 0.071 Uiso 0.676(2) 1 calc PR A 1
C8 C 0.2126(7) 1.2545(7) 0.6242(5) 0.056(2) Uani 0.676(2) 1 d P A 1
H8 H 0.2089 1.2839 0.5855 0.067 Uiso 0.676(2) 1 calc PR A 1
C9 C 0.2404(18) 1.1640(12) 0.6171(11) 0.068(5) Uani 0.676(2) 1 d P A 1
H9 H 0.2596 1.1327 0.5743 0.081 Uiso 0.676(2) 1 calc PR A 1
C10 C 0.2419(6) 1.1115(7) 0.6745(5) 0.049(2) Uani 0.676(2) 1 d P A 1
C11 C 0.2296(8) 0.8802(8) 0.8872(5) 0.061(3) Uani 0.676(2) 1 d P A 1
H11A H 0.2380 0.8226 0.8516 0.092 Uiso 0.676(2) 1 calc PR A 1
H11B H 0.1678 0.8725 0.9026 0.092 Uiso 0.676(2) 1 calc PR A 1
H11C H 0.2831 0.8895 0.9280 0.092 Uiso 0.676(2) 1 calc PR A 1
C12 C 0.2776(10) 0.7490(8) 0.7211(6) 0.076(4) Uani 0.676(2) 1 d P A 1
H12A H 0.2693 0.7579 0.7703 0.113 Uiso 0.676(2) 1 calc PR A 1
H12B H 0.3400 0.7220 0.7158 0.113 Uiso 0.676(2) 1 calc PR A 1
H12C H 0.2248 0.7050 0.6898 0.113 Uiso 0.676(2) 1 calc PR A 1
C13 C -0.0005(11) 1.1338(11) 0.9996(7) 0.075(4) Uani 0.676(2) 1 d P A 1
H13A H -0.0271 1.1790 0.9721 0.112 Uiso 0.676(2) 1 calc PR A 1
H13B H -0.0493 1.1152 1.0247 0.112 Uiso 0.676(2) 1 calc PR A 1
H13C H 0.0169 1.0766 0.9675 0.112 Uiso 0.676(2) 1 calc PR A 1
C14 C 0.1229(9) 1.1120(11) 1.0944(7) 0.089(4) Uani 0.676(2) 1 d P A 1
H14A H 0.1810 1.1398 1.1297 0.133 Uiso 0.676(2) 1 calc PR A 1
H14B H 0.1385 1.0535 1.0628 0.133 Uiso 0.676(2) 1 calc PR A 1
H14C H 0.0715 1.0963 1.1185 0.133 Uiso 0.676(2) 1 calc PR A 1
C15 C 0.071(2) 1.273(2) 1.1017(13) 0.065(5) Uani 0.676(2) 1 d P A 1
H15A H 0.1235 1.2887 1.1442 0.078 Uiso 0.676(2) 1 calc PR A 1
H15B H 0.0088 1.2647 1.1174 0.078 Uiso 0.676(2) 1 calc PR A 1
C16 C 0.0670(7) 1.3568(9) 1.0626(6) 0.067(3) Uani 0.676(2) 1 d P A 1
H16A H 0.0084 1.3464 1.0248 0.080 Uiso 0.676(2) 1 calc PR A 1
H16B H 0.0640 1.4187 1.0965 0.080 Uiso 0.676(2) 1 calc PR A 1
C17 C 0.1403(8) 1.4139(8) 0.9734(5) 0.069(3) Uani 0.676(2) 1 d P A 1
H17A H 0.1987 1.4147 0.9527 0.103 Uiso 0.676(2) 1 calc PR A 1
H17B H 0.1264 1.4799 0.9939 0.103 Uiso 0.676(2) 1 calc PR A 1
H17C H 0.0852 1.3827 0.9365 0.103 Uiso 0.676(2) 1 calc PR A 1
C18 C 0.2442(7) 1.4067(7) 1.0863(5) 0.059(3) Uani 0.676(2) 1 d P A 1
H18A H 0.2428 1.3881 1.1314 0.071 Uiso 0.676(2) 1 calc PR A 1
H18B H 0.2425 1.4773 1.0952 0.071 Uiso 0.676(2) 1 calc PR A 1
C19 C 0.3408(9) 1.3747(8) 1.0589(7) 0.042(3) Uani 0.676(2) 1 d P A 1
H19A H 0.3430 1.3948 1.0145 0.050 Uiso 0.676(2) 1 calc PR A 1
H19B H 0.3981 1.4063 1.0947 0.050 Uiso 0.676(2) 1 calc PR A 1
C20 C 0.4141(15) 1.2235(14) 1.0002(12) 0.056(4) Uani 0.676(2) 1 d P A 1
H20A H 0.4110 1.1540 0.9952 0.084 Uiso 0.676(2) 1 calc PR A 1
H20B H 0.4801 1.2508 1.0225 0.084 Uiso 0.676(2) 1 calc PR A 1
H20C H 0.3969 1.2372 0.9534 0.084 Uiso 0.676(2) 1 calc PR A 1
C21 C 0.3716(9) 1.2402(15) 1.1136(9) 0.071(7) Uani 0.676(2) 1 d P A 1
H21A H 0.3259 1.2642 1.1446 0.107 Uiso 0.676(2) 1 calc PR A 1
H21B H 0.4373 1.2679 1.1364 0.107 Uiso 0.676(2) 1 calc PR A 1
H21C H 0.3703 1.1701 1.1049 0.107 Uiso 0.676(2) 1 calc PR A 1
C22 C 0.5081(8) 0.8125(9) 0.5340(6) 0.074(3) Uani 0.676(2) 1 d P A 1
H22A H 0.5075 0.8733 0.5195 0.111 Uiso 0.676(2) 1 calc PR A 1
H22B H 0.5707 0.7851 0.5303 0.111 Uiso 0.676(2) 1 calc PR A 1
H22C H 0.4985 0.8239 0.5831 0.111 Uiso 0.676(2) 1 calc PR A 1
C23 C 0.4283(8) 0.6508(9) 0.5061(6) 0.066(3) Uani 0.676(2) 1 d P A 1
H23A H 0.3756 0.6078 0.4738 0.099 Uiso 0.676(2) 1 calc PR A 1
H23B H 0.4182 0.6595 0.5549 0.099 Uiso 0.676(2) 1 calc PR A 1
H23C H 0.4905 0.6227 0.5018 0.099 Uiso 0.676(2) 1 calc PR A 1
C24 C 0.4403(10) 0.7242(8) 0.4087(5) 0.057(3) Uani 0.676(2) 1 d P A 1
H24A H 0.5092 0.7166 0.4051 0.069 Uiso 0.676(2) 1 calc PR A 1
H24B H 0.4020 0.6639 0.3818 0.069 Uiso 0.676(2) 1 calc PR A 1
C25 C 0.4040(9) 0.8071(9) 0.3784(5) 0.053(3) Uani 0.676(2) 1 d P A 1
H25A H 0.4506 0.8639 0.3992 0.064 Uiso 0.676(2) 1 calc PR A 1
H25B H 0.4016 0.7902 0.3266 0.064 Uiso 0.676(2) 1 calc PR A 1
C26 C 0.2870(8) 0.9375(8) 0.3888(6) 0.063(3) Uani 0.676(2) 1 d P A 1
H26A H 0.3383 0.9810 0.4222 0.094 Uiso 0.676(2) 1 calc PR A 1
H26B H 0.2238 0.9536 0.4012 0.094 Uiso 0.676(2) 1 calc PR A 1
H26C H 0.2876 0.9442 0.3406 0.094 Uiso 0.676(2) 1 calc PR A 1
C27 C 0.2271(7) 0.7640(8) 0.3420(4) 0.051(2) Uani 0.676(2) 1 d P A 1
H27A H 0.2487 0.6980 0.3356 0.061 Uiso 0.676(2) 1 calc PR A 1
H27B H 0.2160 0.7802 0.2953 0.061 Uiso 0.676(2) 1 calc PR A 1
C28 C 0.1291(11) 0.7690(13) 0.3719(8) 0.047(3) Uani 0.676(2) 1 d P A 1
H28A H 0.1050 0.8339 0.3761 0.057 Uiso 0.676(2) 1 calc PR A 1
H28B H 0.0786 0.7218 0.3397 0.057 Uiso 0.676(2) 1 calc PR A 1
C29 C 0.1506(10) 0.6440(10) 0.4363(8) 0.054(3) Uani 0.676(2) 1 d P A 1
H29A H 0.2010 0.6189 0.4100 0.081 Uiso 0.676(2) 1 calc PR A 1
H29B H 0.0869 0.6149 0.4097 0.081 Uiso 0.676(2) 1 calc PR A 1
H29C H 0.1626 0.6282 0.4826 0.081 Uiso 0.676(2) 1 calc PR A 1
C30 C 0.0762(17) 0.7912(13) 0.4853(10) 0.058(4) Uani 0.676(2) 1 d P A 1
H30A H 0.0811 0.8606 0.4899 0.086 Uiso 0.676(2) 1 calc PR A 1
H30B H 0.0864 0.7782 0.5325 0.086 Uiso 0.676(2) 1 calc PR A 1
H30C H 0.0117 0.7643 0.4591 0.086 Uiso 0.676(2) 1 calc PR A 1
N1 N 0.2239(5) 1.1104(7) 0.7906(3) 0.0457(18) Uani 0.676(2) 1 d PD A 1
N2 N 0.2293(5) 0.9655(5) 0.8559(3) 0.0456(16) Uani 0.676(2) 1 d P A 1
N3 N 0.2596(5) 1.0144(5) 0.6715(4) 0.0457(17) Uani 0.676(2) 1 d P A 1
N4 N 0.2756(5) 0.8418(5) 0.7020(4) 0.0417(16) Uani 0.676(2) 1 d P A 1
N5 N 0.0897(6) 1.1812(7) 1.0529(4) 0.064(2) Uani 0.676(2) 1 d P A 1
N6 N 0.1566(5) 1.3588(6) 1.0310(4) 0.0530(19) Uani 0.676(2) 1 d P A 1
N8 N 0.4295(6) 0.7453(6) 0.4875(4) 0.058(2) Uani 0.676(2) 1 d P A 1
N9 N 0.3045(5) 0.8331(5) 0.3926(3) 0.0426(15) Uani 0.676(2) 1 d P A 1
O1 O 0.1994(15) 1.2200(8) 0.8962(9) 0.068(4) Uani 0.676(2) 1 d PD A 1
O2 O 0.2073(7) 1.0733(8) 0.9607(4) 0.058(2) Uani 0.676(2) 1 d P A 1
O3 O 0.2880(15) 0.9519(10) 0.5471(11) 0.066(7) Uani 0.676(2) 1 d P A 1
O4 O 0.3007(10) 0.7763(7) 0.5854(7) 0.060(3) Uani 0.676(2) 1 d P A 1
Cu1 Cu 0.24839(8) 0.97273(9) 0.75794(6) 0.0423(4) Uani 0.676(2) 1 d P A 1
Cu2 Cu 0.1893(2) 1.2183(2) 0.99490(17) 0.0399(7) Uani 0.676(2) 1 d P A 1
Cu3 Cu 0.3042(5) 0.8117(4) 0.4938(3) 0.0522(15) Uani 0.676(2) 1 d P A 1
C1A C 0.2820(19) 0.887(3) 0.6281(12) 0.043(2) Uani 0.324(2) 1 d PU A 2
C2A C 0.282(3) 0.964(2) 0.5984(16) 0.043(3) Uani 0.324(2) 1 d PDU A 2
C3A C 0.222(2) 1.0768(17) 0.8762(10) 0.043(2) Uani 0.324(2) 1 d PDU A 2
C4A C 0.208(3) 1.1661(19) 0.8573(13) 0.043(3) Uani 0.324(2) 1 d PDU A 2
C5A C 0.2742(11) 0.8537(8) 0.7508(5) 0.046(2) Uani 0.324(2) 1 d PGU A 2
C6A C 0.2972(13) 0.7565(8) 0.7405(5) 0.050(2) Uani 0.324(2) 1 d PGU A 2
H6A H 0.3081 0.7223 0.6956 0.061 Uiso 0.324(2) 1 calc PR A 2
C7A C 0.3039(11) 0.7103(7) 0.7971(6) 0.054(2) Uani 0.324(2) 1 d PGU A 2
H7A H 0.3192 0.6452 0.7902 0.065 Uiso 0.324(2) 1 calc PR A 2
C8A C 0.2875(11) 0.7613(8) 0.8642(5) 0.055(2) Uani 0.324(2) 1 d PGU A 2
H8A H 0.2920 0.7304 0.9021 0.066 Uiso 0.324(2) 1 calc PR A 2
C9A C 0.2646(12) 0.8586(8) 0.8745(5) 0.051(2) Uani 0.324(2) 1 d PGU A 2
H9A H 0.2536 0.8927 0.9194 0.061 Uiso 0.324(2) 1 calc PR A 2
C10A C 0.2579(10) 0.9048(6) 0.8178(6) 0.047(2) Uani 0.324(2) 1 d PGU A 2
C11A C 0.256(4) 1.139(2) 0.6058(17) 0.056(10) Uani 0.324(2) 1 d PDU A 2
H11D H 0.2478 1.1965 0.6413 0.085 Uiso 0.324(2) 1 calc PR A 2
H11E H 0.1988 1.1252 0.5676 0.085 Uiso 0.324(2) 1 calc PR A 2
H11F H 0.3139 1.1487 0.5863 0.085 Uiso 0.324(2) 1 calc PR A 2
C12A C 0.212(3) 1.263(3) 0.7699(18) 0.056(9) Uani 0.324(2) 1 d PU A 2
H12D H 0.2195 1.2561 0.7206 0.085 Uiso 0.324(2) 1 calc PR A 2
H12E H 0.2650 1.3076 0.8012 0.085 Uiso 0.324(2) 1 calc PR A 2
H12F H 0.1497 1.2893 0.7762 0.085 Uiso 0.324(2) 1 calc PR A 2
C13A C 0.002(3) 1.188(3) 0.971(3) 0.21(3) Uani 0.324(2) 1 d PDU A 2
H13D H 0.0136 1.1325 0.9912 0.322 Uiso 0.324(2) 1 calc PR A 2
H13E H 0.0075 1.1706 0.9207 0.322 Uiso 0.324(2) 1 calc PR A 2
H13F H -0.0627 1.2090 0.9751 0.322 Uiso 0.324(2) 1 calc PR A 2
C14A C 0.082(3) 1.368(2) 0.9957(19) 0.117(12) Uani 0.324(2) 1 d PDU A 2
H14D H 0.0853 1.3616 0.9457 0.175 Uiso 0.324(2) 1 calc PR A 2
H14E H 0.1406 1.4052 1.0254 0.175 Uiso 0.324(2) 1 calc PR A 2
H14F H 0.0246 1.4002 1.0065 0.175 Uiso 0.324(2) 1 calc PR A 2
C15A C 0.063(6) 1.291(4) 1.086(3) 0.062(11) Uani 0.324(2) 1 d PDU A 2
H15C H 0.0987 1.3531 1.1126 0.075 Uiso 0.324(2) 1 calc PR A 2
H15D H -0.0069 1.2975 1.0872 0.075 Uiso 0.324(2) 1 calc PR A 2
C16A C 0.0990(19) 1.2121(19) 1.1216(12) 0.063(6) Uani 0.324(2) 1 d PDU A 2
H16C H 0.0512 1.1558 1.1051 0.076 Uiso 0.324(2) 1 calc PR A 2
H16D H 0.1048 1.2349 1.1736 0.076 Uiso 0.324(2) 1 calc PR A 2
C17A C 0.197(4) 1.073(2) 1.101(2) 0.136(11) Uani 0.324(2) 1 d PU A 2
H17D H 0.2582 1.0483 1.0896 0.204 Uiso 0.324(2) 1 calc PR A 2
H17E H 0.1427 1.0388 1.0647 0.204 Uiso 0.324(2) 1 calc PR A 2
H17F H 0.1896 1.0618 1.1472 0.204 Uiso 0.324(2) 1 calc PR A 2
C18A C 0.2806(15) 1.2540(17) 1.1531(11) 0.078(7) Uani 0.324(2) 1 d PDU A 2
H18C H 0.2612 1.3207 1.1581 0.093 Uiso 0.324(2) 1 calc PR A 2
H18D H 0.2955 1.2408 1.2007 0.093 Uiso 0.324(2) 1 calc PR A 2
C19A C 0.369(2) 1.240(3) 1.1177(13) 0.071(13) Uani 0.324(2) 1 d PDU A 2
H19C H 0.3854 1.1728 1.1103 0.085 Uiso 0.324(2) 1 calc PR A 2
H19D H 0.4250 1.2817 1.1480 0.085 Uiso 0.324(2) 1 calc PR A 2
C20A C 0.415(4) 1.256(3) 0.995(3) 0.09(2) Uani 0.324(2) 1 d PDU A 2
H20D H 0.3882 1.2794 0.9533 0.139 Uiso 0.324(2) 1 calc PR A 2
H20E H 0.4270 1.1878 0.9798 0.139 Uiso 0.324(2) 1 calc PR A 2
H20F H 0.4768 1.2925 1.0188 0.139 Uiso 0.324(2) 1 calc PR A 2
C21A C 0.318(5) 1.371(2) 1.068(3) 0.18(3) Uani 0.324(2) 1 d PDU A 2
H21D H 0.2869 1.3920 1.0255 0.272 Uiso 0.324(2) 1 calc PR A 2
H21E H 0.3770 1.4127 1.0905 0.272 Uiso 0.324(2) 1 calc PR A 2
H21F H 0.2729 1.3763 1.1008 0.272 Uiso 0.324(2) 1 calc PR A 2
C22A C 0.491(3) 0.893(4) 0.498(3) 0.24(3) Uani 0.324(2) 1 d PDU A 2
H22D H 0.4740 0.9449 0.5353 0.358 Uiso 0.324(2) 1 calc PR A 2
H22E H 0.5430 0.9180 0.4783 0.358 Uiso 0.324(2) 1 calc PR A 2
H22F H 0.5139 0.8403 0.5190 0.358 Uiso 0.324(2) 1 calc PR A 2
C23A C 0.349(3) 0.934(2) 0.407(2) 0.136(11) Uani 0.324(2) 1 d PDU A 2
H23D H 0.3332 0.9852 0.4454 0.204 Uiso 0.324(2) 1 calc PR A 2
H23E H 0.2891 0.9050 0.3750 0.204 Uiso 0.324(2) 1 calc PR A 2
H23F H 0.3913 0.9619 0.3814 0.204 Uiso 0.324(2) 1 calc PR A 2
C24A C 0.425(4) 0.773(3) 0.384(2) 0.24(3) Uani 0.324(2) 1 d PDU A 2
H24C H 0.4872 0.7861 0.3693 0.283 Uiso 0.324(2) 1 calc PR A 2
H24D H 0.3725 0.7555 0.3419 0.283 Uiso 0.324(2) 1 calc PR A 2
C25A C 0.433(3) 0.696(5) 0.427(3) 0.24(3) Uani 0.324(2) 1 d PDU A 2
H25C H 0.4529 0.6371 0.3970 0.287 Uiso 0.324(2) 1 calc PR A 2
H25D H 0.4870 0.7181 0.4682 0.287 Uiso 0.324(2) 1 calc PR A 2
C26A C 0.367(3) 0.615(3) 0.5131(17) 0.133(10) Uani 0.324(2) 1 d PDU A 2
H26D H 0.3065 0.6047 0.5300 0.199 Uiso 0.324(2) 1 calc PR A 2
H26E H 0.4148 0.6540 0.5523 0.199 Uiso 0.324(2) 1 calc PR A 2
H26F H 0.3917 0.5536 0.4948 0.199 Uiso 0.324(2) 1 calc PR A 2
C27A C 0.257(2) 0.618(3) 0.3996(17) 0.133(10) Uani 0.324(2) 1 d PDU A 2
H27C H 0.2469 0.6457 0.3577 0.159 Uiso 0.324(2) 1 calc PR A 2
H27D H 0.2649 0.5484 0.3839 0.159 Uiso 0.324(2) 1 calc PR A 2
C28A C 0.171(4) 0.634(4) 0.438(3) 0.136(15) Uani 0.324(2) 1 d PDU A 2
H28C H 0.1869 0.6199 0.4854 0.163 Uiso 0.324(2) 1 calc PR A 2
H28D H 0.1126 0.5935 0.4105 0.163 Uiso 0.324(2) 1 calc PR A 2
C29A C 0.088(4) 0.774(4) 0.502(3) 0.13(2) Uani 0.324(2) 1 d PDU A 2
H29D H 0.1166 0.7546 0.5449 0.201 Uiso 0.324(2) 1 calc PR A 2
H29E H 0.0231 0.7408 0.4830 0.201 Uiso 0.324(2) 1 calc PR A 2
H29F H 0.0826 0.8432 0.5124 0.201 Uiso 0.324(2) 1 calc PR A 2
C30A C 0.146(5) 0.771(4) 0.377(3) 0.16(3) Uani 0.324(2) 1 d PU A 2
H30D H 0.1522 0.8411 0.3848 0.237 Uiso 0.324(2) 1 calc PR A 2
H30E H 0.0838 0.7457 0.3467 0.237 Uiso 0.324(2) 1 calc PR A 2
H30F H 0.1991 0.7435 0.3545 0.237 Uiso 0.324(2) 1 calc PR A 2
N1A N 0.2696(11) 0.9077(12) 0.7006(7) 0.043(2) Uani 0.324(2) 1 d PDU A 2
N2A N 0.2670(12) 1.0572(11) 0.6390(9) 0.049(4) Uani 0.324(2) 1 d PDU A 2
N3A N 0.2380(10) 1.0018(10) 0.8198(7) 0.040(2) Uani 0.324(2) 1 d PDU A 2
N4A N 0.2163(11) 1.1725(12) 0.7871(9) 0.048(4) Uani 0.324(2) 1 d PD A 2
N5A N 0.078(2) 1.269(2) 1.0103(17) 0.149(13) Uani 0.324(2) 1 d PDU A 2
N6A N 0.1982(17) 1.1821(18) 1.1046(9) 0.098(7) Uani 0.324(2) 1 d PDU A 2
N8A N 0.4018(19) 0.858(2) 0.4396(17) 0.207(19) Uani 0.324(2) 1 d PDU A 2
N9A N 0.3455(17) 0.6684(16) 0.4543(13) 0.140(11) Uani 0.324(2) 1 d PDU A 2
O1A O 0.285(2) 0.7979(18) 0.5933(14) 0.044(3) Uani 0.324(2) 1 d PDU A 2
O2A O 0.283(3) 0.948(3) 0.549(3) 0.082(16) Uani 0.324(2) 1 d PU A 2
O3A O 0.2161(15) 1.0708(16) 0.9361(11) 0.045(3) Uani 0.324(2) 1 d PDU A 2
O4A O 0.190(3) 1.2411(19) 0.8962(13) 0.044(3) Uani 0.324(2) 1 d PDU A 2
Cu1A Cu 0.24707(19) 1.0452(2) 0.73404(13) 0.0485(9) Uani 0.324(2) 1 d PU A 2
Cu2A Cu 0.2044(6) 1.1954(5) 1.0044(4) 0.059(2) Uani 0.324(2) 1 d PU A 2
Cu3A Cu 0.2884(9) 0.7997(7) 0.4899(4) 0.0276(12) Uani 0.324(2) 1 d PDU A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 C31 1.629(10) . ?
B1 C43 1.635(10) . ?
B1 C37 1.658(9) . ?
B1 C49 1.656(9) . ?
B2 C73 1.639(11) . ?
B2 C61 1.641(11) . ?
B2 C67 1.648(9) . ?
B2 C55 1.662(9) . ?
C31 C32 1.403(9) . ?
C31 C36 1.406(10) . ?
C32 C33 1.353(10) . ?
C32 H32 0.9300 . ?
C33 C34 1.397(10) . ?
C33 H33 0.9300 . ?
C34 C35 1.387(10) . ?
C34 H34 0.9300 . ?
C35 C36 1.376(10) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 C38 1.391(8) . ?
C37 C42 1.394(10) . ?
C38 C39 1.385(8) . ?
C38 H38 0.9300 . ?
C39 C40 1.367(10) . ?
C39 H39 0.9300 . ?
C40 C41 1.393(11) . ?
C40 H40 0.9300 . ?
C41 C42 1.364(11) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C43 C48 1.408(10) . ?
C43 C44 1.412(9) . ?
C44 C45 1.381(10) . ?
C44 H44 0.9300 . ?
C45 C46 1.391(11) . ?
C45 H45 0.9300 . ?
C46 C47 1.341(11) . ?
C46 H46 0.9300 . ?
C47 C48 1.377(11) . ?
C47 H47 0.9300 . ?
C48 H48 0.9300 . ?
C49 C54 1.400(9) . ?
C49 C50 1.423(9) . ?
C50 C51 1.408(9) . ?
C50 H50 0.9300 . ?
C51 C52 1.374(10) . ?
C51 H51 0.9300 . ?
C52 C53 1.385(10) . ?
C52 H52 0.9300 . ?
C53 C54 1.391(9) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C55 C60 1.370(10) . ?
C55 C56 1.401(8) . ?
C56 C57 1.373(8) . ?
C56 H56 0.9300 . ?
C57 C58 1.352(10) . ?
C57 H57 0.9300 . ?
C58 C59 1.392(11) . ?
C58 H58 0.9300 . ?
C59 C60 1.376(10) . ?
C59 H59 0.9300 . ?
C60 H60 0.9300 . ?
C61 C62 1.408(9) . ?
C61 C66 1.418(10) . ?
C62 C63 1.374(10) . ?
C62 H62 0.9300 . ?
C63 C64 1.395(10) . ?
C63 H63 0.9300 . ?
C64 C65 1.381(9) . ?
C64 H64 0.9300 . ?
C65 C66 1.337(10) . ?
C65 H65 0.9300 . ?
C66 H66 0.9300 . ?
C67 C68 1.398(10) . ?
C67 C72 1.412(9) . ?
C68 C69 1.409(9) . ?
C68 H68 0.9300 . ?
C69 C70 1.371(10) . ?
C69 H69 0.9300 . ?
C70 C71 1.391(10) . ?
C70 H70 0.9300 . ?
C71 C72 1.402(9) . ?
C71 H71 0.9300 . ?
C72 H72 0.9300 . ?
C73 C78 1.380(10) . ?
C73 C74 1.384(8) . ?
C74 C75 1.356(10) . ?
C74 H74 0.9300 . ?
C75 C76 1.398(12) . ?
C75 H75 0.9300 . ?
C76 C77 1.390(11) . ?
C76 H76 0.9300 . ?
C77 C78 1.391(10) . ?
C77 H77 0.9300 . ?
C78 H78 0.9300 . ?
N7 C21 1.440(16) . ?
N7 C19 1.473(12) . ?
N7 C20 1.479(14) . ?
N7 C21A 1.50(2) . ?
N7 C20A 1.50(2) . ?
N7 C19A 1.507(18) . ?
N7 Cu2A 2.076(10) . ?
N7 Cu2 2.195(6) . ?
N10 C29 1.401(16) . ?
N10 C30A 1.45(6) . ?
N10 C30 1.475(15) . ?
N10 C29A 1.503(19) . ?
N10 C28 1.526(17) . ?
N10 C28A 1.57(5) . ?
N10 Cu3A 1.963(13) . ?
N10 Cu3 2.209(8) . ?
C1 N1 1.277(13) . ?
C1 O1 1.294(13) . ?
C1 C2 1.527(17) . ?
C2 N2 1.287(12) . ?
C2 O2 1.297(13) . ?
C3 N3 1.298(11) . ?
C3 O3 1.43(3) . ?
C3 C4 1.525(14) . ?
C4 O4 1.296(14) . ?
C4 N4 1.301(12) . ?
C5 C10 1.368(12) . ?
C5 N1 1.420(13) . ?
C5 C6 1.42(2) . ?
C6 C7 1.38(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.392(13) . ?
C7 H7 0.9300 . ?
C8 C9 1.32(2) . ?
C8 H8 0.9300 . ?
C9 C10 1.47(2) . ?
C9 H9 0.9300 . ?
C10 N3 1.384(12) . ?
C11 N2 1.464(13) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N4 1.437(14) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N5 1.494(15) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 N5 1.434(16) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N5 1.47(3) . ?
C15 C16 1.54(2) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 N6 1.470(13) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 N6 1.489(14) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N6 1.489(11) . ?
C18 C19 1.555(15) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 N8 1.441(13) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 N8 1.456(14) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C25 1.483(16) . ?
C24 N8 1.520(12) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 N9 1.481(14) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 N9 1.511(13) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 N9 1.473(11) . ?
C27 C28 1.556(15) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
N1 Cu1 1.953(9) . ?
N2 Cu1 1.985(7) . ?
N3 Cu1 1.926(9) . ?
N4 Cu1 1.991(7) . ?
N5 Cu2 2.046(8) . ?
N6 Cu2 2.031(8) . ?
N8 Cu3 1.992(9) . ?
N9 Cu3 2.050(7) . ?
O1 Cu2 1.946(16) . ?
O2 Cu2 2.030(10) . ?
O3 Cu3 2.043(12) . ?
O4 Cu3 1.957(14) . ?
C1A O1A 1.28(4) . ?
C1A C2A 1.34(4) . ?
C1A N1A 1.41(3) . ?
C1A O2A 1.92(6) . ?
C2A O2A 0.93(5) . ?
C2A N2A 1.403(19) . ?
C3A O3A 1.198(13) . ?
C3A N3A 1.387(17) . ?
C3A C4A 1.396(13) . ?
C4A O4A 1.206(14) . ?
C4A N4A 1.406(14) . ?
C5A N1A 1.359(17) . ?
C5A C6A 1.3900 . ?
C5A C10A 1.3900 . ?
C6A C7A 1.3900 . ?
C6A H6A 0.9300 . ?
C7A C8A 1.3900 . ?
C7A H7A 0.9300 . ?
C8A C9A 1.3900 . ?
C8A H8A 0.9300 . ?
C9A C10A 1.3900 . ?
C9A H9A 0.9300 . ?
C10A N3A 1.393(16) . ?
C11A N2A 1.436(18) . ?
C11A H11D 0.9600 . ?
C11A H11E 0.9600 . ?
C11A H11F 0.9600 . ?
C12A N4A 1.39(5) . ?
C12A H12D 0.9600 . ?
C12A H12E 0.9600 . ?
C12A H12F 0.9600 . ?
C13A N5A 1.488(19) . ?
C13A H13D 0.9600 . ?
C13A H13E 0.9600 . ?
C13A H13F 0.9600 . ?
C14A N5A 1.475(19) . ?
C14A H14D 0.9600 . ?
C14A H14E 0.9600 . ?
C14A H14F 0.9600 . ?
C15A C16A 1.490(19) . ?
C15A N5A 1.48(7) . ?
C15A H15C 0.9700 . ?
C15A H15D 0.9700 . ?
C16A N6A 1.51(3) . ?
C16A H16C 0.9700 . ?
C16A H16D 0.9700 . ?
C17A N6A 1.53(4) . ?
C17A H17D 0.9600 . ?
C17A H17E 0.9600 . ?
C17A H17F 0.9600 . ?
C18A C19A 1.489(19) . ?
C18A N6A 1.520(18) . ?
C18A H18C 0.9700 . ?
C18A H18D 0.9700 . ?
C19A H19C 0.9700 . ?
C19A H19D 0.9700 . ?
C20A H20D 0.9600 . ?
C20A H20E 0.9600 . ?
C20A H20F 0.9600 . ?
C21A H21D 0.9600 . ?
C21A H21E 0.9600 . ?
C21A H21F 0.9600 . ?
C22A N8A 1.505(19) . ?
C22A H22D 0.9600 . ?
C22A H22E 0.9600 . ?
C22A H22F 0.9600 . ?
C23A N8A 1.508(19) . ?
C23A H23D 0.9600 . ?
C23A H23E 0.9600 . ?
C23A H23F 0.9600 . ?
C24A N8A 1.493(19) . ?
C24A C25A 1.51(2) . ?
C24A H24C 0.9700 . ?
C24A H24D 0.9700 . ?
C25A N9A 1.478(18) . ?
C25A H25C 0.9700 . ?
C25A H25D 0.9700 . ?
C26A N9A 1.490(18) . ?
C26A H26D 0.9600 . ?
C26A H26E 0.9600 . ?
C26A H26F 0.9600 . ?
C27A C28A 1.50(2) . ?
C27A N9A 1.503(18) . ?
C27A H27C 0.9700 . ?
C27A H27D 0.9700 . ?
C28A H28C 0.9700 . ?
C28A H28D 0.9700 . ?
C29A H29D 0.9600 . ?
C29A H29E 0.9600 . ?
C29A H29F 0.9600 . ?
C30A H30D 0.9600 . ?
C30A H30E 0.9600 . ?
C30A H30F 0.9600 . ?
N1A Cu1A 1.946(16) . ?
N2A Cu1A 1.952(16) . ?
N3A Cu1A 1.918(14) . ?
N4A Cu1A 1.948(17) . ?
N5A Cu2A 2.06(3) . ?
N6A Cu2A 2.007(19) . ?
N8A Cu3A 2.208(16) . ?
N9A Cu3A 2.05(2) . ?
O1A Cu3A 2.02(3) . ?
O2A Cu3A 2.15(4) . ?
O3A Cu2A 1.97(3) . ?
O4A Cu2A 2.31(3) . ?

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
C31 B1 C43 111.5(5) . . ?
C31 B1 C37 107.6(5) . . ?
C43 B1 C37 108.7(5) . . ?
C31 B1 C49 112.6(6) . . ?
C43 B1 C49 106.9(5) . . ?
C37 B1 C49 109.6(5) . . ?
C73 B2 C61 110.3(5) . . ?
C73 B2 C67 108.3(5) . . ?
C61 B2 C67 111.2(6) . . ?
C73 B2 C55 108.1(6) . . ?
C61 B2 C55 107.8(5) . . ?
C67 B2 C55 111.1(5) . . ?
C32 C31 C36 113.0(6) . . ?
C32 C31 B1 122.4(6) . . ?
C36 C31 B1 124.5(6) . . ?
C33 C32 C31 124.3(7) . . ?
C33 C32 H32 117.9 . . ?
C31 C32 H32 117.9 . . ?
C32 C33 C34 121.4(7) . . ?
C32 C33 H33 119.3 . . ?
C34 C33 H33 119.3 . . ?
C35 C34 C33 116.5(7) . . ?
C35 C34 H34 121.7 . . ?
C33 C34 H34 121.7 . . ?
C36 C35 C34 121.0(7) . . ?
C36 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C35 C36 C31 123.7(6) . . ?
C35 C36 H36 118.1 . . ?
C31 C36 H36 118.1 . . ?
C38 C37 C42 114.7(6) . . ?
C38 C37 B1 121.7(6) . . ?
C42 C37 B1 122.8(6) . . ?
C39 C38 C37 123.3(6) . . ?
C39 C38 H38 118.4 . . ?
C37 C38 H38 118.4 . . ?
C40 C39 C38 120.0(6) . . ?
C40 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
C39 C40 C41 118.2(7) . . ?
C39 C40 H40 120.9 . . ?
C41 C40 H40 120.9 . . ?
C42 C41 C40 120.8(8) . . ?
C42 C41 H41 119.6 . . ?
C40 C41 H41 119.6 . . ?
C41 C42 C37 122.7(8) . . ?
C41 C42 H42 118.6 . . ?
C37 C42 H42 118.6 . . ?
C48 C43 C44 114.5(7) . . ?
C48 C43 B1 122.3(6) . . ?
C44 C43 B1 122.8(7) . . ?
C45 C44 C43 122.2(8) . . ?
C45 C44 H44 118.9 . . ?
C43 C44 H44 118.9 . . ?
C44 C45 C46 120.7(7) . . ?
C44 C45 H45 119.7 . . ?
C46 C45 H45 119.7 . . ?
C47 C46 C45 118.2(8) . . ?
C47 C46 H46 120.9 . . ?
C45 C46 H46 120.9 . . ?
C46 C47 C48 122.2(8) . . ?
C46 C47 H47 118.9 . . ?
C48 C47 H47 118.9 . . ?
C47 C48 C43 122.2(7) . . ?
C47 C48 H48 118.9 . . ?
C43 C48 H48 118.9 . . ?
C54 C49 C50 114.1(6) . . ?
C54 C49 B1 123.9(6) . . ?
C50 C49 B1 122.0(6) . . ?
C51 C50 C49 122.0(6) . . ?
C51 C50 H50 119.0 . . ?
C49 C50 H50 119.0 . . ?
C52 C51 C50 120.8(7) . . ?
C52 C51 H51 119.6 . . ?
C50 C51 H51 119.6 . . ?
C51 C52 C53 119.2(6) . . ?
C51 C52 H52 120.4 . . ?
C53 C52 H52 120.4 . . ?
C52 C53 C54 119.5(6) . . ?
C52 C53 H53 120.2 . . ?
C54 C53 H53 120.2 . . ?
C53 C54 C49 124.4(7) . . ?
C53 C54 H54 117.8 . . ?
C49 C54 H54 117.8 . . ?
C60 C55 C56 114.2(6) . . ?
C60 C55 B2 125.4(6) . . ?
C56 C55 B2 120.4(5) . . ?
C57 C56 C55 123.5(6) . . ?
C57 C56 H56 118.3 . . ?
C55 C56 H56 118.3 . . ?
C58 C57 C56 120.1(6) . . ?
C58 C57 H57 119.9 . . ?
C56 C57 H57 119.9 . . ?
C57 C58 C59 118.9(6) . . ?
C57 C58 H58 120.6 . . ?
C59 C58 H58 120.6 . . ?
C60 C59 C58 119.5(8) . . ?
C60 C59 H59 120.3 . . ?
C58 C59 H59 120.3 . . ?
C55 C60 C59 123.8(7) . . ?
C55 C60 H60 118.1 . . ?
C59 C60 H60 118.1 . . ?
C62 C61 C66 112.3(7) . . ?
C62 C61 B2 122.9(6) . . ?
C66 C61 B2 124.5(6) . . ?
C63 C62 C61 124.3(7) . . ?
C63 C62 H62 117.9 . . ?
C61 C62 H62 117.9 . . ?
C62 C63 C64 120.4(6) . . ?
C62 C63 H63 119.8 . . ?
C64 C63 H63 119.8 . . ?
C65 C64 C63 116.4(7) . . ?
C65 C64 H64 121.8 . . ?
C63 C64 H64 121.8 . . ?
C66 C65 C64 122.6(7) . . ?
C66 C65 H65 118.7 . . ?
C64 C65 H65 118.7 . . ?
C65 C66 C61 123.9(6) . . ?
C65 C66 H66 118.0 . . ?
C61 C66 H66 118.0 . . ?
C68 C67 C72 114.0(6) . . ?
C68 C67 B2 123.6(6) . . ?
C72 C67 B2 122.3(6) . . ?
C67 C68 C69 123.7(6) . . ?
C67 C68 H68 118.1 . . ?
C69 C68 H68 118.1 . . ?
C70 C69 C68 119.7(7) . . ?
C70 C69 H69 120.1 . . ?
C68 C69 H69 120.1 . . ?
C69 C70 C71 119.6(6) . . ?
C69 C70 H70 120.2 . . ?
C71 C70 H70 120.2 . . ?
C70 C71 C72 119.5(7) . . ?
C70 C71 H71 120.3 . . ?
C72 C71 H71 120.3 . . ?
C71 C72 C67 123.5(7) . . ?
C71 C72 H72 118.3 . . ?
C67 C72 H72 118.3 . . ?
C78 C73 C74 115.3(6) . . ?
C78 C73 B2 120.6(6) . . ?
C74 C73 B2 123.7(6) . . ?
C75 C74 C73 124.1(7) . . ?
C75 C74 H74 117.9 . . ?
C73 C74 H74 117.9 . . ?
C74 C75 C76 119.6(7) . . ?
C74 C75 H75 120.2 . . ?
C76 C75 H75 120.2 . . ?
C77 C76 C75 118.6(7) . . ?
C77 C76 H76 120.7 . . ?
C75 C76 H76 120.7 . . ?
C76 C77 C78 119.2(8) . . ?
C76 C77 H77 120.4 . . ?
C78 C77 H77 120.4 . . ?
C73 C78 C77 123.1(7) . . ?
C73 C78 H78 118.4 . . ?
C77 C78 H78 118.4 . . ?
C21 N7 C19 110.0(11) . . ?
C21 N7 C20 106.0(13) . . ?
C19 N7 C20 115.6(10) . . ?
C21 N7 C21A 104(3) . . ?
C19 N7 C21A 15(3) . . ?
C20 N7 C21A 130(3) . . ?
C21 N7 C20A 119(3) . . ?
C19 N7 C20A 97.2(19) . . ?
C20 N7 C20A 19(2) . . ?
C21A N7 C20A 112(3) . . ?
C21 N7 C19A 2.6(15) . . ?
C19 N7 C19A 109.0(18) . . ?
C20 N7 C19A 108.6(14) . . ?
C21A N7 C19A 102(3) . . ?
C20A N7 C19A 121(3) . . ?
C21 N7 Cu2A 102.9(7) . . ?
C19 N7 Cu2A 112.2(6) . . ?
C20 N7 Cu2A 109.1(9) . . ?
C21A N7 Cu2A 101(3) . . ?
C20A N7 Cu2A 116(3) . . ?
C19A N7 Cu2A 101.4(16) . . ?
C21 N7 Cu2 111.8(6) . . ?
C19 N7 Cu2 101.6(6) . . ?
C20 N7 Cu2 111.9(10) . . ?
C21A N7 Cu2 92(2) . . ?
C20A N7 Cu2 115(3) . . ?
C19A N7 Cu2 110.0(15) . . ?
Cu2A N7 Cu2 11.5(2) . . ?
C29 N10 C30A 110(2) . . ?
C29 N10 C30 113.6(10) . . ?
C30A N10 C30 112(3) . . ?
C29 N10 C29A 102(2) . . ?
C30A N10 C29A 129(4) . . ?
C30 N10 C29A 18(3) . . ?
C29 N10 C28 108.5(9) . . ?
C30A N10 C28 9(3) . . ?
C30 N10 C28 105.5(9) . . ?
C29A N10 C28 123(2) . . ?
C29 N10 C28A 10(2) . . ?
C30A N10 C28A 111(3) . . ?
C30 N10 C28A 121.1(18) . . ?
C29A N10 C28A 108(3) . . ?
C28 N10 C28A 111(2) . . ?
C29 N10 Cu3A 107.7(7) . . ?
C30A N10 Cu3A 98(2) . . ?
C30 N10 Cu3A 114.3(10) . . ?
C29A N10 Cu3A 109(2) . . ?
C28 N10 Cu3A 106.8(7) . . ?
C28A N10 Cu3A 98(2) . . ?
C29 N10 Cu3 109.8(7) . . ?
C30A N10 Cu3 97(2) . . ?
C30 N10 Cu3 113.7(10) . . ?
C29A N10 Cu3 109(2) . . ?
C28 N10 Cu3 105.1(7) . . ?
C28A N10 Cu3 100(2) . . ?
Cu3A N10 Cu3 2.2(3) . . ?
N1 C1 O1 131.3(14) . . ?
N1 C1 C2 113.4(11) . . ?
O1 C1 C2 115.3(11) . . ?
N2 C2 O2 126.6(11) . . ?
N2 C2 C1 117.6(11) . . ?
O2 C2 C1 115.7(9) . . ?
N3 C3 O3 129.5(14) . . ?
N3 C3 C4 112.2(11) . . ?
O3 C3 C4 118.2(9) . . ?
O4 C4 N4 127.1(11) . . ?
O4 C4 C3 114.5(9) . . ?
N4 C4 C3 118.4(10) . . ?
C10 C5 N1 111.8(9) . . ?
C10 C5 C6 123.5(11) . . ?
N1 C5 C6 124.6(10) . . ?
C7 C6 C5 117.6(12) . . ?
C7 C6 H6 121.2 . . ?
C5 C6 H6 121.2 . . ?
C6 C7 C8 120.6(11) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C9 C8 C7 120.9(12) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.6 . . ?
C8 C9 C10 122.1(15) . . ?
C8 C9 H9 118.9 . . ?
C10 C9 H9 118.9 . . ?
C5 C10 N3 117.0(9) . . ?
C5 C10 C9 115.0(11) . . ?
N3 C10 C9 128.0(10) . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N5 C15 C16 110.0(17) . . ?
N5 C15 H15A 109.4 . . ?
C16 C15 H15A 109.5 . . ?
N5 C15 H15B 109.9 . . ?
C16 C15 H15B 109.9 . . ?
H15A C15 H15B 108.1 . . ?
N6 C16 C15 108.5(14) . . ?
N6 C16 H16A 110.1 . . ?
C15 C16 H16A 109.9 . . ?
N6 C16 H16B 110.1 . . ?
C15 C16 H16B 109.9 . . ?
H16A C16 H16B 108.4 . . ?
N6 C17 H17A 109.5 . . ?
N6 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N6 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N6 C18 C19 109.6(7) . . ?
N6 C18 H18A 109.8 . . ?
C19 C18 H18A 109.8 . . ?
N6 C18 H18B 109.8 . . ?
C19 C18 H18B 109.8 . . ?
H18A C18 H18B 108.2 . . ?
N7 C19 C18 109.7(9) . . ?
N7 C19 H19A 109.7 . . ?
C18 C19 H19A 109.7 . . ?
N7 C19 H19B 109.7 . . ?
C18 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
N7 C20 H20A 109.5 . . ?
N7 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N7 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N7 C21 H21A 109.5 . . ?
N7 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N7 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N8 C22 H22A 109.5 . . ?
N8 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N8 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N8 C23 H23A 109.5 . . ?
N8 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N8 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 N8 108.5(9) . . ?
C25 C24 H24A 110.0 . . ?
N8 C24 H24A 110.0 . . ?
C25 C24 H24B 110.0 . . ?
N8 C24 H24B 110.0 . . ?
H24A C24 H24B 108.4 . . ?
N9 C25 C24 112.9(10) . . ?
N9 C25 H25A 109.0 . . ?
C24 C25 H25A 109.0 . . ?
N9 C25 H25B 109.0 . . ?
C24 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
N9 C26 H26A 109.5 . . ?
N9 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N9 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N9 C27 C28 110.0(8) . . ?
N9 C27 H27A 109.7 . . ?
C28 C27 H27A 109.6 . . ?
N9 C27 H27B 109.7 . . ?
C28 C27 H27B 109.7 . . ?
H27A C27 H27B 108.2 . . ?
N10 C28 C27 107.0(10) . . ?
N10 C28 H28A 110.3 . . ?
C27 C28 H28A 110.3 . . ?
N10 C28 H28B 110.3 . . ?
C27 C28 H28B 110.3 . . ?
H28A C28 H28B 108.6 . . ?
N10 C29 H29A 109.5 . . ?
N10 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N10 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N10 C30 H30A 109.5 . . ?
N10 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N10 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C1 N1 C5 130.6(10) . . ?
C1 N1 Cu1 114.4(9) . . ?
C5 N1 Cu1 115.0(5) . . ?
C2 N2 C11 120.5(9) . . ?
C2 N2 Cu1 110.5(8) . . ?
C11 N2 Cu1 129.0(6) . . ?
C3 N3 C10 129.8(11) . . ?
C3 N3 Cu1 115.3(9) . . ?
C10 N3 Cu1 114.6(5) . . ?
C4 N4 C12 120.1(8) . . ?
C4 N4 Cu1 109.5(7) . . ?
C12 N4 Cu1 130.1(6) . . ?
C14 N5 C15 109.5(12) . . ?
C14 N5 C13 106.8(9) . . ?
C15 N5 C13 113.2(15) . . ?
C14 N5 Cu2 114.3(8) . . ?
C15 N5 Cu2 106.3(14) . . ?
C13 N5 Cu2 106.9(6) . . ?
C16 N6 C17 109.7(9) . . ?
C16 N6 C18 111.7(7) . . ?
C17 N6 C18 108.4(8) . . ?
C16 N6 Cu2 108.0(6) . . ?
C17 N6 Cu2 113.4(6) . . ?
C18 N6 Cu2 105.7(6) . . ?
C22 N8 C23 111.8(8) . . ?
C22 N8 C24 112.1(9) . . ?
C23 N8 C24 106.0(8) . . ?
C22 N8 Cu3 106.6(7) . . ?
C23 N8 Cu3 113.7(7) . . ?
C24 N8 Cu3 106.7(6) . . ?
C27 N9 C25 110.4(7) . . ?
C27 N9 C26 111.1(7) . . ?
C25 N9 C26 111.3(8) . . ?
C27 N9 Cu3 107.1(5) . . ?
C25 N9 Cu3 104.4(5) . . ?
C26 N9 Cu3 112.3(6) . . ?
C1 O1 Cu2 114.4(10) . . ?
C2 O2 Cu2 111.3(7) . . ?
C3 O3 Cu3 105.4(13) . . ?
C4 O4 Cu3 115.1(9) . . ?
N3 Cu1 N1 81.3(3) . . ?
N3 Cu1 N2 165.1(3) . . ?
N1 Cu1 N2 83.9(3) . . ?
N3 Cu1 N4 84.5(3) . . ?
N1 Cu1 N4 165.8(3) . . ?
N2 Cu1 N4 110.3(3) . . ?
O1 Cu2 O2 83.3(4) . . ?
O1 Cu2 N6 99.6(4) . . ?
O2 Cu2 N6 173.7(4) . . ?
O1 Cu2 N5 140.6(7) . . ?
O2 Cu2 N5 88.0(4) . . ?
N6 Cu2 N5 86.2(4) . . ?
O1 Cu2 N7 97.9(6) . . ?
O2 Cu2 N7 98.4(3) . . ?
N6 Cu2 N7 86.8(3) . . ?
N5 Cu2 N7 121.5(3) . . ?
O4 Cu3 N8 89.8(4) . . ?
O4 Cu3 O3 86.5(7) . . ?
N8 Cu3 O3 127.8(7) . . ?
O4 Cu3 N9 173.9(5) . . ?
N8 Cu3 N9 88.1(4) . . ?
O3 Cu3 N9 99.4(7) . . ?
O4 Cu3 N10 92.4(5) . . ?
N8 Cu3 N10 126.5(4) . . ?
O3 Cu3 N10 105.7(6) . . ?
N9 Cu3 N10 84.2(3) . . ?
O1A C1A C2A 124(2) . . ?
O1A C1A N1A 120(3) . . ?
C2A C1A N1A 116(3) . . ?
O1A C1A O2A 98(2) . . ?
C2A C1A O2A 26.2(16) . . ?
N1A C1A O2A 142(3) . . ?
O2A C2A C1A 114(3) . . ?
O2A C2A N2A 126(4) . . ?
C1A C2A N2A 120(3) . . ?
O3A C3A N3A 127(2) . . ?
O3A C3A C4A 119.4(18) . . ?
N3A C3A C4A 113.7(17) . . ?
O4A C4A C3A 126(2) . . ?
O4A C4A N4A 115.0(19) . . ?
C3A C4A N4A 118.9(17) . . ?
N1A C5A C6A 125.3(10) . . ?
N1A C5A C10A 114.6(10) . . ?
C6A C5A C10A 120.0 . . ?
C7A C6A C5A 120.0 . . ?
C7A C6A H6A 120.0 . . ?
C5A C6A H6A 120.0 . . ?
C6A C7A C8A 120.0 . . ?
C6A C7A H7A 120.0 . . ?
C8A C7A H7A 120.0 . . ?
C7A C8A C9A 120.0 . . ?
C7A C8A H8A 120.0 . . ?
C9A C8A H8A 120.0 . . ?
C10A C9A C8A 120.0 . . ?
C10A C9A H9A 120.0 . . ?
C8A C9A H9A 120.0 . . ?
C9A C10A C5A 120.0 . . ?
C9A C10A N3A 127.1(9) . . ?
C5A C10A N3A 112.9(9) . . ?
N2A C11A H11D 109.5 . . ?
N2A C11A H11E 109.5 . . ?
H11D C11A H11E 109.5 . . ?
N2A C11A H11F 109.4 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
N4A C12A H12D 109.5 . . ?
N4A C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
N4A C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
N5A C13A H13D 109.5 . . ?
N5A C13A H13E 109.5 . . ?
H13D C13A H13E 109.5 . . ?
N5A C13A H13F 109.4 . . ?
H13D C13A H13F 109.5 . . ?
H13E C13A H13F 109.5 . . ?
N5A C14A H14D 109.5 . . ?
N5A C14A H14E 109.5 . . ?
H14D C14A H14E 109.5 . . ?
N5A C14A H14F 109.4 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
C16A C15A N5A 111(4) . . ?
C16A C15A H15C 109.8 . . ?
N5A C15A H15C 110.1 . . ?
C16A C15A H15D 108.9 . . ?
N5A C15A H15D 109.1 . . ?
H15C C15A H15D 108.3 . . ?
C15A C16A N6A 111(4) . . ?
C15A C16A H16C 109.5 . . ?
N6A C16A H16C 109.2 . . ?
C15A C16A H16D 109.9 . . ?
N6A C16A H16D 109.2 . . ?
H16C C16A H16D 107.9 . . ?
N6A C17A H17D 109.5 . . ?
N6A C17A H17E 109.5 . . ?
H17D C17A H17E 109.5 . . ?
N6A C17A H17F 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
C19A C18A N6A 106(2) . . ?
C19A C18A H18C 110.4 . . ?
N6A C18A H18C 110.4 . . ?
C19A C18A H18D 110.4 . . ?
N6A C18A H18D 110.4 . . ?
H18C C18A H18D 108.6 . . ?
C18A C19A N7 108.4(17) . . ?
C18A C19A H19C 110.0 . . ?
N7 C19A H19C 110.0 . . ?
C18A C19A H19D 110.0 . . ?
N7 C19A H19D 110.0 . . ?
H19C C19A H19D 108.4 . . ?
N7 C20A H20D 109.5 . . ?
N7 C20A H20E 109.5 . . ?
H20D C20A H20E 109.5 . . ?
N7 C20A H20F 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
N7 C21A H21D 109.4 . . ?
N7 C21A H21E 109.5 . . ?
H21D C21A H21E 109.5 . . ?
N7 C21A H21F 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
N8A C22A H22D 109.5 . . ?
N8A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
N8A C22A H22F 109.4 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
N8A C23A H23D 109.4 . . ?
N8A C23A H23E 109.5 . . ?
H23D C23A H23E 109.5 . . ?
N8A C23A H23F 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
N8A C24A C25A 100(4) . . ?
N8A C24A H24C 111.8 . . ?
C25A C24A H24C 111.8 . . ?
N8A C24A H24D 111.8 . . ?
C25A C24A H24D 111.8 . . ?
H24C C24A H24D 109.5 . . ?
N9A C25A C24A 119(4) . . ?
N9A C25A H25C 107.6 . . ?
C24A C25A H25C 107.6 . . ?
N9A C25A H25D 107.7 . . ?
C24A C25A H25D 107.7 . . ?
H25C C25A H25D 107.1 . . ?
N9A C26A H26D 109.5 . . ?
N9A C26A H26E 109.5 . . ?
H26D C26A H26E 109.5 . . ?
N9A C26A H26F 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?
C28A C27A N9A 105(3) . . ?
C28A C27A H27C 110.7 . . ?
N9A C27A H27C 110.8 . . ?
C28A C27A H27D 110.8 . . ?
N9A C27A H27D 110.7 . . ?
H27C C27A H27D 108.8 . . ?
C27A C28A N10 105(4) . . ?
C27A C28A H28C 110.6 . . ?
N10 C28A H28C 110.6 . . ?
C27A C28A H28D 110.7 . . ?
N10 C28A H28D 110.7 . . ?
H28C C28A H28D 108.8 . . ?
N10 C29A H29D 109.5 . . ?
N10 C29A H29E 109.5 . . ?
H29D C29A H29E 109.5 . . ?
N10 C29A H29F 109.5 . . ?
H29D C29A H29F 109.5 . . ?
H29E C29A H29F 109.5 . . ?
N10 C30A H30D 109.6 . . ?
N10 C30A H30E 109.4 . . ?
H30D C30A H30E 109.5 . . ?
N10 C30A H30F 109.4 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 109.5 . . ?
C5A N1A C1A 134(2) . . ?
C5A N1A Cu1A 115.6(9) . . ?
C1A N1A Cu1A 110.6(18) . . ?
C2A N2A C11A 120(2) . . ?
C2A N2A Cu1A 108.6(16) . . ?
C11A N2A Cu1A 130.5(17) . . ?
C3A N3A C10A 130.7(15) . . ?
C3A N3A Cu1A 112.9(13) . . ?
C10A N3A Cu1A 116.0(9) . . ?
C12A N4A C4A 119(2) . . ?
C12A N4A Cu1A 132(2) . . ?
C4A N4A Cu1A 108.5(12) . . ?
C14A N5A C13A 125(3) . . ?
C14A N5A C15A 102(3) . . ?
C13A N5A C15A 105(4) . . ?
C14A N5A Cu2A 115(2) . . ?
C13A N5A Cu2A 99(2) . . ?
C15A N5A Cu2A 108(3) . . ?
C16A N6A C18A 110.1(19) . . ?
C16A N6A C17A 105(2) . . ?
C18A N6A C17A 122(3) . . ?
C16A N6A Cu2A 108.7(16) . . ?
C18A N6A Cu2A 104.3(13) . . ?
C17A N6A Cu2A 106.1(16) . . ?
C24A N8A C22A 110(2) . . ?
C24A N8A C23A 113(2) . . ?
C22A N8A C23A 116(2) . . ?
C24A N8A Cu3A 106(3) . . ?
C22A N8A Cu3A 107(2) . . ?
C23A N8A Cu3A 102.7(17) . . ?
C25A N9A C26A 115(2) . . ?
C25A N9A C27A 118(2) . . ?
C26A N9A C27A 109(2) . . ?
C25A N9A Cu3A 104(3) . . ?
C26A N9A Cu3A 111.0(19) . . ?
C27A N9A Cu3A 98.8(19) . . ?
C1A O1A Cu3A 107(2) . . ?
C2A O2A C1A 40(2) . . ?
C2A O2A Cu3A 123(4) . . ?
C1A O2A Cu3A 82.8(18) . . ?
C3A O3A Cu2A 115.4(17) . . ?
C4A O4A Cu2A 100.5(17) . . ?
N3A Cu1A N1A 80.6(6) . . ?
N3A Cu1A N4A 85.9(6) . . ?
N1A Cu1A N4A 166.3(6) . . ?
N3A Cu1A N2A 165.9(6) . . ?
N1A Cu1A N2A 85.5(6) . . ?
N4A Cu1A N2A 108.1(6) . . ?
O3A Cu2A N6A 113.9(9) . . ?
O3A Cu2A N5A 126.2(12) . . ?
N6A Cu2A N5A 85.8(12) . . ?
O3A Cu2A N7 109.8(7) . . ?
N6A Cu2A N7 87.9(7) . . ?
N5A Cu2A N7 121.0(10) . . ?
O3A Cu2A O4A 77.7(8) . . ?
N6A Cu2A O4A 166.8(11) . . ?
N5A Cu2A O4A 82.2(12) . . ?
N7 Cu2A O4A 93.8(10) . . ?
N10 Cu3A O1A 98.5(9) . . ?
N10 Cu3A N9A 92.2(8) . . ?
O1A Cu3A N9A 101.3(11) . . ?
N10 Cu3A O2A 108.3(12) . . ?
O1A Cu3A O2A 72.0(17) . . ?
N9A Cu3A O2A 159.0(15) . . ?
N10 Cu3A N8A 129.1(9) . . ?
O1A Cu3A N8A 132.1(13) . . ?
N9A Cu3A N8A 83.7(12) . . ?
O2A Cu3A N8A 86.5(18) . . ?

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
C43 B1 C31 C32 33.5(7) . . . . ?
C37 B1 C31 C32 -85.5(7) . . . . ?
C49 B1 C31 C32 153.6(5) . . . . ?
C43 B1 C31 C36 -150.9(5) . . . . ?
C37 B1 C31 C36 90.0(7) . . . . ?
C49 B1 C31 C36 -30.9(8) . . . . ?
C36 C31 C32 C33 -0.1(9) . . . . ?
B1 C31 C32 C33 175.9(6) . . . . ?
C31 C32 C33 C34 -1.9(10) . . . . ?
C32 C33 C34 C35 2.1(10) . . . . ?
C33 C34 C35 C36 -0.3(10) . . . . ?
C34 C35 C36 C31 -1.8(10) . . . . ?
C32 C31 C36 C35 2.0(9) . . . . ?
B1 C31 C36 C35 -174.0(6) . . . . ?
C31 B1 C37 C38 40.5(8) . . . . ?
C43 B1 C37 C38 -80.3(8) . . . . ?
C49 B1 C37 C38 163.3(6) . . . . ?
C31 B1 C37 C42 -150.1(8) . . . . ?
C43 B1 C37 C42 89.1(9) . . . . ?
C49 B1 C37 C42 -27.4(11) . . . . ?
C42 C37 C38 C39 3.0(11) . . . . ?
B1 C37 C38 C39 173.2(6) . . . . ?
C37 C38 C39 C40 -0.5(11) . . . . ?
C38 C39 C40 C41 -0.1(16) . . . . ?
C39 C40 C41 C42 -2(2) . . . . ?
C40 C41 C42 C37 5(2) . . . . ?
C38 C37 C42 C41 -5.3(17) . . . . ?
B1 C37 C42 C41 -175.3(12) . . . . ?
C31 B1 C43 C48 -151.7(6) . . . . ?
C37 B1 C43 C48 -33.3(8) . . . . ?
C49 B1 C43 C48 84.9(7) . . . . ?
C31 B1 C43 C44 35.5(7) . . . . ?
C37 B1 C43 C44 153.9(5) . . . . ?
C49 B1 C43 C44 -87.9(7) . . . . ?
C48 C43 C44 C45 0.6(9) . . . . ?
B1 C43 C44 C45 173.9(6) . . . . ?
C43 C44 C45 C46 0.1(9) . . . . ?
C44 C45 C46 C47 -1.3(10) . . . . ?
C45 C46 C47 C48 1.6(11) . . . . ?
C46 C47 C48 C43 -0.9(11) . . . . ?
C44 C43 C48 C47 -0.3(9) . . . . ?
B1 C43 C48 C47 -173.6(6) . . . . ?
C31 B1 C49 C54 -111.8(8) . . . . ?
C43 B1 C49 C54 10.9(9) . . . . ?
C37 B1 C49 C54 128.5(7) . . . . ?
C31 B1 C49 C50 68.0(8) . . . . ?
C43 B1 C49 C50 -169.4(6) . . . . ?
C37 B1 C49 C50 -51.8(9) . . . . ?
C54 C49 C50 C51 2.1(11) . . . . ?
B1 C49 C50 C51 -177.7(7) . . . . ?
C49 C50 C51 C52 -1.5(12) . . . . ?
C50 C51 C52 C53 0.2(12) . . . . ?
C51 C52 C53 C54 0.4(12) . . . . ?
C52 C53 C54 C49 0.4(13) . . . . ?
C50 C49 C54 C53 -1.6(11) . . . . ?
B1 C49 C54 C53 178.2(7) . . . . ?
C73 B2 C55 C60 112.3(9) . . . . ?
C61 B2 C55 C60 -128.5(9) . . . . ?
C67 B2 C55 C60 -6.4(12) . . . . ?
C73 B2 C55 C56 -67.3(8) . . . . ?
C61 B2 C55 C56 52.0(8) . . . . ?
C67 B2 C55 C56 174.0(6) . . . . ?
C60 C55 C56 C57 0.7(11) . . . . ?
B2 C55 C56 C57 -179.7(6) . . . . ?
C55 C56 C57 C58 0.6(10) . . . . ?
C56 C57 C58 C59 -0.7(13) . . . . ?
C57 C58 C59 C60 -0.5(18) . . . . ?
C56 C55 C60 C59 -2.0(17) . . . . ?
B2 C55 C60 C59 178.4(11) . . . . ?
C58 C59 C60 C55 2(2) . . . . ?
C73 B2 C61 C62 33.2(8) . . . . ?
C67 B2 C61 C62 153.4(6) . . . . ?
C55 B2 C61 C62 -84.7(7) . . . . ?
C73 B2 C61 C66 -153.9(5) . . . . ?
C67 B2 C61 C66 -33.7(8) . . . . ?
C55 B2 C61 C66 88.2(7) . . . . ?
C66 C61 C62 C63 0.6(9) . . . . ?
B2 C61 C62 C63 174.3(6) . . . . ?
C61 C62 C63 C64 -0.9(10) . . . . ?
C62 C63 C64 C65 0.6(9) . . . . ?
C63 C64 C65 C66 -0.2(10) . . . . ?
C64 C65 C66 C61 0.0(10) . . . . ?
C62 C61 C66 C65 -0.2(8) . . . . ?
B2 C61 C66 C65 -173.8(6) . . . . ?
C73 B2 C67 C68 -168.4(6) . . . . ?
C61 B2 C67 C68 70.2(8) . . . . ?
C55 B2 C67 C68 -49.9(10) . . . . ?
C73 B2 C67 C72 9.0(9) . . . . ?
C61 B2 C67 C72 -112.4(8) . . . . ?
C55 B2 C67 C72 127.6(7) . . . . ?
C72 C67 C68 C69 2.0(11) . . . . ?
B2 C67 C68 C69 179.7(7) . . . . ?
C67 C68 C69 C70 -2.0(12) . . . . ?
C68 C69 C70 C71 0.7(12) . . . . ?
C69 C70 C71 C72 0.4(13) . . . . ?
C70 C71 C72 C67 -0.2(13) . . . . ?
C68 C67 C72 C71 -0.9(11) . . . . ?
B2 C67 C72 C71 -178.6(7) . . . . ?
C61 B2 C73 C78 -150.4(5) . . . . ?
C67 B2 C73 C78 87.7(7) . . . . ?
C55 B2 C73 C78 -32.7(8) . . . . ?
C61 B2 C73 C74 37.1(8) . . . . ?
C67 B2 C73 C74 -84.8(7) . . . . ?
C55 B2 C73 C74 154.8(6) . . . . ?
C78 C73 C74 C75 0.8(9) . . . . ?
B2 C73 C74 C75 173.7(6) . . . . ?
C73 C74 C75 C76 0.4(10) . . . . ?
C74 C75 C76 C77 -1.6(10) . . . . ?
C75 C76 C77 C78 1.4(10) . . . . ?
C74 C73 C78 C77 -1.0(9) . . . . ?
B2 C73 C78 C77 -174.1(6) . . . . ?
C76 C77 C78 C73 -0.1(10) . . . . ?
N1 C1 C2 N2 -1.7(19) . . . . ?
O1 C1 C2 N2 178.7(14) . . . . ?
N1 C1 C2 O2 179.9(12) . . . . ?
O1 C1 C2 O2 0(2) . . . . ?
N3 C3 C4 O4 -178.5(11) . . . . ?
O3 C3 C4 O4 -1.1(17) . . . . ?
N3 C3 C4 N4 -0.3(13) . . . . ?
O3 C3 C4 N4 177.0(12) . . . . ?
C10 C5 C6 C7 -4.0(19) . . . . ?
N1 C5 C6 C7 179.4(10) . . . . ?
C5 C6 C7 C8 3.3(19) . . . . ?
C6 C7 C8 C9 -3(2) . . . . ?
C7 C8 C9 C10 4(3) . . . . ?
N1 C5 C10 N3 3.8(11) . . . . ?
C6 C5 C10 N3 -173.3(11) . . . . ?
N1 C5 C10 C9 -178.7(12) . . . . ?
C6 C5 C10 C9 4.2(17) . . . . ?
C8 C9 C10 C5 -4(2) . . . . ?
C8 C9 C10 N3 173.0(13) . . . . ?
N5 C15 C16 N6 -52(2) . . . . ?
C21 N7 C19 C18 -77.3(11) . . . . ?
C20 N7 C19 C18 162.6(13) . . . . ?
C21A N7 C19 C18 -9(10) . . . . ?
C20A N7 C19 C18 158(3) . . . . ?
C19A N7 C19 C18 -74.8(15) . . . . ?
Cu2A N7 C19 C18 36.7(11) . . . . ?
Cu2 N7 C19 C18 41.2(9) . . . . ?
N6 C18 C19 N7 -59.8(12) . . . . ?
N8 C24 C25 N9 -50.5(11) . . . . ?
C29 N10 C28 C27 -81.8(12) . . . . ?
C30A N10 C28 C27 20(18) . . . . ?
C30 N10 C28 C27 156.1(12) . . . . ?
C29A N10 C28 C27 160(3) . . . . ?
C28A N10 C28 C27 -71(2) . . . . ?
Cu3A N10 C28 C27 34.1(11) . . . . ?
Cu3 N10 C28 C27 35.7(11) . . . . ?
N9 C27 C28 N10 -57.7(12) . . . . ?
O1 C1 N1 C5 -4(3) . . . . ?
C2 C1 N1 C5 176.2(9) . . . . ?
O1 C1 N1 Cu1 177.3(17) . . . . ?
C2 C1 N1 Cu1 -2.2(16) . . . . ?
C10 C5 N1 C1 175.8(13) . . . . ?
C6 C5 N1 C1 -7.1(18) . . . . ?
C10 C5 N1 Cu1 -5.8(9) . . . . ?
C6 C5 N1 Cu1 171.2(10) . . . . ?
O2 C2 N2 C11 1.3(16) . . . . ?
C1 C2 N2 C11 -176.9(11) . . . . ?
O2 C2 N2 Cu1 -177.3(10) . . . . ?
C1 C2 N2 Cu1 4.5(13) . . . . ?
O3 C3 N3 C10 7(2) . . . . ?
C4 C3 N3 C10 -175.6(8) . . . . ?
O3 C3 N3 Cu1 -178.8(13) . . . . ?
C4 C3 N3 Cu1 -1.8(11) . . . . ?
C5 C10 N3 C3 173.8(10) . . . . ?
C9 C10 N3 C3 -3.4(19) . . . . ?
C5 C10 N3 Cu1 0.0(10) . . . . ?
C9 C10 N3 Cu1 -177.2(13) . . . . ?
O4 C4 N4 C12 -5.7(17) . . . . ?
C3 C4 N4 C12 176.4(10) . . . . ?
O4 C4 N4 Cu1 -179.9(10) . . . . ?
C3 C4 N4 Cu1 2.1(10) . . . . ?
C16 C15 N5 C14 162.6(15) . . . . ?
C16 C15 N5 C13 -78(2) . . . . ?
C16 C15 N5 Cu2 39(2) . . . . ?
C15 C16 N6 C17 161.0(13) . . . . ?
C15 C16 N6 C18 -78.9(14) . . . . ?
C15 C16 N6 Cu2 37.0(14) . . . . ?
C19 C18 N6 C16 159.6(10) . . . . ?
C19 C18 N6 C17 -79.5(11) . . . . ?
C19 C18 N6 Cu2 42.4(10) . . . . ?
C25 C24 N8 C22 -79.3(11) . . . . ?
C25 C24 N8 C23 158.5(9) . . . . ?
C25 C24 N8 Cu3 37.0(11) . . . . ?
C28 C27 N9 C25 161.3(10) . . . . ?
C28 C27 N9 C26 -74.6(11) . . . . ?
C28 C27 N9 Cu3 48.3(10) . . . . ?
C24 C25 N9 C27 -78.6(9) . . . . ?
C24 C25 N9 C26 157.5(8) . . . . ?
C24 C25 N9 Cu3 36.2(8) . . . . ?
N1 C1 O1 Cu2 -179.1(16) . . . . ?
C2 C1 O1 Cu2 0(2) . . . . ?
N2 C2 O2 Cu2 -179.1(9) . . . . ?
C1 C2 O2 Cu2 -0.8(14) . . . . ?
N3 C3 O3 Cu3 -178.6(10) . . . . ?
C4 C3 O3 Cu3 4.5(16) . . . . ?
N4 C4 O4 Cu3 178.7(8) . . . . ?
C3 C4 O4 Cu3 -3.3(14) . . . . ?
C3 N3 Cu1 N1 -177.3(7) . . . . ?
C10 N3 Cu1 N1 -2.5(6) . . . . ?
C3 N3 Cu1 N2 -175.8(10) . . . . ?
C10 N3 Cu1 N2 -1.0(14) . . . . ?
C3 N3 Cu1 N4 2.4(7) . . . . ?
C10 N3 Cu1 N4 177.2(6) . . . . ?
C1 N1 Cu1 N3 -176.8(10) . . . . ?
C5 N1 Cu1 N3 4.6(6) . . . . ?
C1 N1 Cu1 N2 3.6(10) . . . . ?
C5 N1 Cu1 N2 -175.0(6) . . . . ?
C1 N1 Cu1 N4 -178.1(13) . . . . ?
C5 N1 Cu1 N4 3.3(15) . . . . ?
C2 N2 Cu1 N3 -5.9(15) . . . . ?
C11 N2 Cu1 N3 175.7(10) . . . . ?
C2 N2 Cu1 N1 -4.4(7) . . . . ?
C11 N2 Cu1 N1 177.2(8) . . . . ?
C2 N2 Cu1 N4 176.0(6) . . . . ?
C11 N2 Cu1 N4 -2.4(8) . . . . ?
C4 N4 Cu1 N3 -2.4(6) . . . . ?
C12 N4 Cu1 N3 -175.9(9) . . . . ?
C4 N4 Cu1 N1 -1.1(15) . . . . ?
C12 N4 Cu1 N1 -174.6(11) . . . . ?
C4 N4 Cu1 N2 177.1(6) . . . . ?
C12 N4 Cu1 N2 3.6(10) . . . . ?
C1 O1 Cu2 O2 -0.7(14) . . . . ?
C1 O1 Cu2 N6 -175.0(14) . . . . ?
C1 O1 Cu2 N5 -79.2(16) . . . . ?
C1 O1 Cu2 N7 96.9(14) . . . . ?
C2 O2 Cu2 O1 0.8(10) . . . . ?
C2 O2 Cu2 N6 119(3) . . . . ?
C2 O2 Cu2 N5 142.3(8) . . . . ?
C2 O2 Cu2 N7 -96.2(8) . . . . ?
C16 N6 Cu2 O1 127.7(9) . . . . ?
C17 N6 Cu2 O1 5.9(9) . . . . ?
C18 N6 Cu2 O1 -112.6(9) . . . . ?
C16 N6 Cu2 O2 11(4) . . . . ?
C17 N6 Cu2 O2 -111(3) . . . . ?
C18 N6 Cu2 O2 130(3) . . . . ?
C16 N6 Cu2 N5 -13.1(7) . . . . ?
C17 N6 Cu2 N5 -134.8(7) . . . . ?
C18 N6 Cu2 N5 106.6(7) . . . . ?
C16 N6 Cu2 N7 -134.9(6) . . . . ?
C17 N6 Cu2 N7 103.4(6) . . . . ?
C18 N6 Cu2 N7 -15.2(6) . . . . ?
C14 N5 Cu2 O1 124.0(9) . . . . ?
C15 N5 Cu2 O1 -115.1(12) . . . . ?
C13 N5 Cu2 O1 6.1(12) . . . . ?
C14 N5 Cu2 O2 47.1(8) . . . . ?
C15 N5 Cu2 O2 168.0(11) . . . . ?
C13 N5 Cu2 O2 -70.8(9) . . . . ?
C14 N5 Cu2 N6 -135.4(8) . . . . ?
C15 N5 Cu2 N6 -14.5(11) . . . . ?
C13 N5 Cu2 N6 106.7(9) . . . . ?
C14 N5 Cu2 N7 -51.5(9) . . . . ?
C15 N5 Cu2 N7 69.3(11) . . . . ?
C13 N5 Cu2 N7 -169.5(8) . . . . ?
C21 N7 Cu2 O1 -158.3(10) . . . . ?
C19 N7 Cu2 O1 84.5(7) . . . . ?
C20 N7 Cu2 O1 -39.5(10) . . . . ?
C21A N7 Cu2 O1 96(3) . . . . ?
C20A N7 Cu2 O1 -19(2) . . . . ?
C19A N7 Cu2 O1 -160.2(16) . . . . ?
Cu2A N7 Cu2 O1 -117.2(16) . . . . ?
C21 N7 Cu2 O2 -73.9(10) . . . . ?
C19 N7 Cu2 O2 168.8(6) . . . . ?
C20 N7 Cu2 O2 44.9(10) . . . . ?
C21A N7 Cu2 O2 -180(3) . . . . ?
C20A N7 Cu2 O2 65(2) . . . . ?
C19A N7 Cu2 O2 -75.9(16) . . . . ?
Cu2A N7 Cu2 O2 -32.8(15) . . . . ?
C21 N7 Cu2 N6 102.5(10) . . . . ?
C19 N7 Cu2 N6 -14.8(6) . . . . ?
C20 N7 Cu2 N6 -138.7(10) . . . . ?
C21A N7 Cu2 N6 -3(3) . . . . ?
C20A N7 Cu2 N6 -118(2) . . . . ?
C19A N7 Cu2 N6 100.5(16) . . . . ?
Cu2A N7 Cu2 N6 143.6(17) . . . . ?
C21 N7 Cu2 N5 18.9(11) . . . . ?
C19 N7 Cu2 N5 -98.4(7) . . . . ?
C20 N7 Cu2 N5 137.7(10) . . . . ?
C21A N7 Cu2 N5 -87(3) . . . . ?
C20A N7 Cu2 N5 158(2) . . . . ?
C19A N7 Cu2 N5 16.9(16) . . . . ?
Cu2A N7 Cu2 N5 60.0(15) . . . . ?
C4 O4 Cu3 N8 132.8(10) . . . . ?
C4 O4 Cu3 O3 4.8(11) . . . . ?
C4 O4 Cu3 N9 -158(4) . . . . ?
C4 O4 Cu3 N10 -100.8(10) . . . . ?
C22 N8 Cu3 O4 -80.0(8) . . . . ?
C23 N8 Cu3 O4 43.6(8) . . . . ?
C24 N8 Cu3 O4 160.1(8) . . . . ?
C22 N8 Cu3 O3 5.4(12) . . . . ?
C23 N8 Cu3 O3 129.0(11) . . . . ?
C24 N8 Cu3 O3 -114.6(11) . . . . ?
C22 N8 Cu3 N9 105.8(7) . . . . ?
C23 N8 Cu3 N9 -130.6(7) . . . . ?
C24 N8 Cu3 N9 -14.2(7) . . . . ?
C22 N8 Cu3 N10 -172.8(6) . . . . ?
C23 N8 Cu3 N10 -49.3(8) . . . . ?
C24 N8 Cu3 N10 67.2(8) . . . . ?
C3 O3 Cu3 O4 -4.8(12) . . . . ?
C3 O3 Cu3 N8 -91.8(13) . . . . ?
C3 O3 Cu3 N9 173.3(11) . . . . ?
C3 O3 Cu3 N10 86.7(12) . . . . ?
C27 N9 Cu3 O4 36(5) . . . . ?
C25 N9 Cu3 O4 -81(5) . . . . ?
C26 N9 Cu3 O4 159(5) . . . . ?
C27 N9 Cu3 N8 106.1(6) . . . . ?
C25 N9 Cu3 N8 -11.0(6) . . . . ?
C26 N9 Cu3 N8 -131.7(6) . . . . ?
C27 N9 Cu3 O3 -125.9(8) . . . . ?
C25 N9 Cu3 O3 117.0(8) . . . . ?
C26 N9 Cu3 O3 -3.6(9) . . . . ?
C27 N9 Cu3 N10 -20.9(6) . . . . ?
C25 N9 Cu3 N10 -138.0(6) . . . . ?
C26 N9 Cu3 N10 101.4(6) . . . . ?
C29 N10 Cu3 O4 -67.4(7) . . . . ?
C30A N10 Cu3 O4 178(3) . . . . ?
C30 N10 Cu3 O4 61.1(8) . . . . ?
C29A N10 Cu3 O4 43(2) . . . . ?
C28 N10 Cu3 O4 176.0(7) . . . . ?
C28A N10 Cu3 O4 -69(2) . . . . ?
Cu3A N10 Cu3 O4 -45(9) . . . . ?
C29 N10 Cu3 N8 24.1(8) . . . . ?
C30A N10 Cu3 N8 -90(3) . . . . ?
C30 N10 Cu3 N8 152.6(8) . . . . ?
C29A N10 Cu3 N8 135(2) . . . . ?
C28 N10 Cu3 N8 -92.5(7) . . . . ?
C28A N10 Cu3 N8 22(2) . . . . ?
Cu3A N10 Cu3 N8 46(9) . . . . ?
C29 N10 Cu3 O3 -154.4(10) . . . . ?
C30A N10 Cu3 O3 91(3) . . . . ?
C30 N10 Cu3 O3 -25.9(10) . . . . ?
C29A N10 Cu3 O3 -44(2) . . . . ?
C28 N10 Cu3 O3 89.0(10) . . . . ?
C28A N10 Cu3 O3 -156(2) . . . . ?
Cu3A N10 Cu3 O3 -132(10) . . . . ?
C29 N10 Cu3 N9 107.4(7) . . . . ?
C30A N10 Cu3 N9 -7(3) . . . . ?
C30 N10 Cu3 N9 -124.1(8) . . . . ?
C29A N10 Cu3 N9 -142(2) . . . . ?
C28 N10 Cu3 N9 -9.2(7) . . . . ?
C28A N10 Cu3 N9 105(2) . . . . ?
Cu3A N10 Cu3 N9 129(10) . . . . ?
O1A C1A C2A O2A 2(7) . . . . ?
N1A C1A C2A O2A -173(4) . . . . ?
O1A C1A C2A N2A 172(2) . . . . ?
N1A C1A C2A N2A -2(4) . . . . ?
O2A C1A C2A N2A 171(7) . . . . ?
O3A C3A C4A O4A 0(7) . . . . ?
N3A C3A C4A O4A 178(4) . . . . ?
O3A C3A C4A N4A 179(3) . . . . ?
N3A C3A C4A N4A -3(6) . . . . ?
N1A C5A C6A C7A 177.2(15) . . . . ?
C10A C5A C6A C7A 0.0 . . . . ?
C5A C6A C7A C8A 0.0 . . . . ?
C6A C7A C8A C9A 0.0 . . . . ?
C7A C8A C9A C10A 0.0 . . . . ?
C8A C9A C10A C5A 0.0 . . . . ?
C8A C9A C10A N3A -178.4(14) . . . . ?
N1A C5A C10A C9A -177.5(14) . . . . ?
C6A C5A C10A C9A 0.0 . . . . ?
N1A C5A C10A N3A 1.1(15) . . . . ?
C6A C5A C10A N3A 178.6(12) . . . . ?
N5A C15A C16A N6A 44(7) . . . . ?
N6A C18A C19A N7 63(3) . . . . ?
C21 N7 C19A C18A -174(58) . . . . ?
C19 N7 C19A C18A 72(3) . . . . ?
C20 N7 C19A C18A -161(2) . . . . ?
C21A N7 C19A C18A 58(4) . . . . ?
C20A N7 C19A C18A -176(3) . . . . ?
Cu2A N7 C19A C18A -46(3) . . . . ?
Cu2 N7 C19A C18A -38(3) . . . . ?
N8A C24A C25A N9A 61(6) . . . . ?
N9A C27A C28A N10 72(4) . . . . ?
C29 N10 C28A C27A 139(17) . . . . ?
C30A N10 C28A C27A 50(5) . . . . ?
C30 N10 C28A C27A -177(2) . . . . ?
C29A N10 C28A C27A -164(4) . . . . ?
C28 N10 C28A C27A 59(4) . . . . ?
Cu3A N10 C28A C27A -52(4) . . . . ?
Cu3 N10 C28A C27A -51(4) . . . . ?
C6A C5A N1A C1A 2(3) . . . . ?
C10A C5A N1A C1A 179.3(19) . . . . ?
C6A C5A N1A Cu1A -174.8(7) . . . . ?
C10A C5A N1A Cu1A 2.5(16) . . . . ?
O1A C1A N1A C5A 12(4) . . . . ?
C2A C1A N1A C5A -173(2) . . . . ?
O2A C1A N1A C5A -178(3) . . . . ?
O1A C1A N1A Cu1A -171(2) . . . . ?
C2A C1A N1A Cu1A 4(3) . . . . ?
O2A C1A N1A Cu1A -1(4) . . . . ?
O2A C2A N2A C11A -3(7) . . . . ?
C1A C2A N2A C11A -173(3) . . . . ?
O2A C2A N2A Cu1A 169(5) . . . . ?
C1A C2A N2A Cu1A -1(4) . . . . ?
O3A C3A N3A C10A -5(5) . . . . ?
C4A C3A N3A C10A 177(3) . . . . ?
O3A C3A N3A Cu1A -178(3) . . . . ?
C4A C3A N3A Cu1A 5(4) . . . . ?
C9A C10A N3A C3A 1(3) . . . . ?
C5A C10A N3A C3A -177(2) . . . . ?
C9A C10A N3A Cu1A 174.1(7) . . . . ?
C5A C10A N3A Cu1A -4.4(14) . . . . ?
O4A C4A N4A C12A 6(5) . . . . ?
C3A C4A N4A C12A -174(4) . . . . ?
O4A C4A N4A Cu1A 179(3) . . . . ?
C3A C4A N4A Cu1A 0(5) . . . . ?
C16A C15A N5A C14A -155(5) . . . . ?
C16A C15A N5A C13A 72(6) . . . . ?
C16A C15A N5A Cu2A -33(6) . . . . ?
C15A C16A N6A C18A 81(4) . . . . ?
C15A C16A N6A C17A -146(4) . . . . ?
C15A C16A N6A Cu2A -33(4) . . . . ?
C19A C18A N6A C16A -161(2) . . . . ?
C19A C18A N6A C17A 75(3) . . . . ?
C19A C18A N6A Cu2A -45(2) . . . . ?
C25A C24A N8A C22A 71(4) . . . . ?
C25A C24A N8A C23A -157(3) . . . . ?
C25A C24A N8A Cu3A -45(4) . . . . ?
C24A C25A N9A C26A -163(4) . . . . ?
C24A C25A N9A C27A 66(6) . . . . ?
C24A C25A N9A Cu3A -41(5) . . . . ?
C28A C27A N9A C25A -159(4) . . . . ?
C28A C27A N9A C26A 68(4) . . . . ?
C28A C27A N9A Cu3A -48(3) . . . . ?
C2A C1A O1A Cu3A 0(4) . . . . ?
N1A C1A O1A Cu3A 174.0(18) . . . . ?
O2A C1A O1A Cu3A 0(2) . . . . ?
N2A C2A O2A C1A -170(8) . . . . ?
C1A C2A O2A Cu3A -2(7) . . . . ?
N2A C2A O2A Cu3A -172(2) . . . . ?
O1A C1A O2A C2A -179(5) . . . . ?
N1A C1A O2A C2A 10(6) . . . . ?
O1A C1A O2A Cu3A 0(2) . . . . ?
C2A C1A O2A Cu3A 178(6) . . . . ?
N1A C1A O2A Cu3A -172(3) . . . . ?
N3A C3A O3A Cu2A 175(2) . . . . ?
C4A C3A O3A Cu2A -8(5) . . . . ?
C3A C4A O4A Cu2A 6(6) . . . . ?
N4A C4A O4A Cu2A -173(3) . . . . ?
C3A N3A Cu1A N1A 178.4(17) . . . . ?
C10A N3A Cu1A N1A 4.5(11) . . . . ?
C3A N3A Cu1A N4A -3.9(17) . . . . ?
C10A N3A Cu1A N4A -177.9(12) . . . . ?
C3A N3A Cu1A N2A 170(3) . . . . ?
C10A N3A Cu1A N2A -4(3) . . . . ?
C5A N1A Cu1A N3A -3.9(12) . . . . ?
C1A N1A Cu1A N3A 178.7(15) . . . . ?
C5A N1A Cu1A N4A -14(3) . . . . ?
C1A N1A Cu1A N4A 169(3) . . . . ?
C5A N1A Cu1A N2A 174.1(13) . . . . ?
C1A N1A Cu1A N2A -3.4(14) . . . . ?
C12A N4A Cu1A N3A 175(3) . . . . ?
C4A N4A Cu1A N3A 2(2) . . . . ?
C12A N4A Cu1A N1A -176(3) . . . . ?
C4A N4A Cu1A N1A 12(4) . . . . ?
C12A N4A Cu1A N2A -4(3) . . . . ?
C4A N4A Cu1A N2A -176(2) . . . . ?
C2A N2A Cu1A N3A 11(4) . . . . ?
C11A N2A Cu1A N3A -178(3) . . . . ?
C2A N2A Cu1A N1A 2.2(17) . . . . ?
C11A N2A Cu1A N1A 174(3) . . . . ?
C2A N2A Cu1A N4A -175.8(17) . . . . ?
C11A N2A Cu1A N4A -4(3) . . . . ?
C3A O3A Cu2A N6A -179(2) . . . . ?
C3A O3A Cu2A N5A 79(3) . . . . ?
C3A O3A Cu2A N7 -82(2) . . . . ?
C3A O3A Cu2A O4A 8(2) . . . . ?
C16A N6A Cu2A O3A -116.5(17) . . . . ?
C18A N6A Cu2A O3A 126.0(16) . . . . ?
C17A N6A Cu2A O3A -4(3) . . . . ?
C16A N6A Cu2A N5A 11.4(18) . . . . ?
C18A N6A Cu2A N5A -106.1(18) . . . . ?
C17A N6A Cu2A N5A 124(2) . . . . ?
C16A N6A Cu2A N7 132.7(16) . . . . ?
C18A N6A Cu2A N7 15.2(16) . . . . ?
C17A N6A Cu2A N7 -115(2) . . . . ?
C16A N6A Cu2A O4A 35(6) . . . . ?
C18A N6A Cu2A O4A -83(6) . . . . ?
C17A N6A Cu2A O4A 147(5) . . . . ?
C14A N5A Cu2A O3A -117(2) . . . . ?
C13A N5A Cu2A O3A 19(3) . . . . ?
C15A N5A Cu2A O3A 128(3) . . . . ?
C14A N5A Cu2A N6A 126(2) . . . . ?
C13A N5A Cu2A N6A -98(3) . . . . ?
C15A N5A Cu2A N6A 12(3) . . . . ?
C14A N5A Cu2A N7 41(3) . . . . ?
C13A N5A Cu2A N7 177(2) . . . . ?
C15A N5A Cu2A N7 -73(3) . . . . ?
C14A N5A Cu2A O4A -49(2) . . . . ?
C13A N5A Cu2A O4A 87(3) . . . . ?
C15A N5A Cu2A O4A -163(3) . . . . ?
C21 N7 Cu2A O3A -96.5(11) . . . . ?
C19 N7 Cu2A O3A 145.2(8) . . . . ?
C20 N7 Cu2A O3A 15.8(12) . . . . ?
C21A N7 Cu2A O3A 156(3) . . . . ?
C20A N7 Cu2A O3A 35(3) . . . . ?
C19A N7 Cu2A O3A -98.6(15) . . . . ?
Cu2 N7 Cu2A O3A 122.3(18) . . . . ?
C21 N7 Cu2A N6A 18.2(12) . . . . ?
C19 N7 Cu2A N6A -100.1(10) . . . . ?
C20 N7 Cu2A N6A 130.5(13) . . . . ?
C21A N7 Cu2A N6A -89(3) . . . . ?
C20A N7 Cu2A N6A 150(3) . . . . ?
C19A N7 Cu2A N6A 16.1(16) . . . . ?
Cu2 N7 Cu2A N6A -123.0(19) . . . . ?
C21 N7 Cu2A N5A 102.0(14) . . . . ?
C19 N7 Cu2A N5A -16.3(13) . . . . ?
C20 N7 Cu2A N5A -145.7(15) . . . . ?
C21A N7 Cu2A N5A -5(3) . . . . ?
C20A N7 Cu2A N5A -127(3) . . . . ?
C19A N7 Cu2A N5A 99.9(17) . . . . ?
Cu2 N7 Cu2A N5A -39.2(16) . . . . ?
C21 N7 Cu2A O4A -174.8(11) . . . . ?
C19 N7 Cu2A O4A 66.9(9) . . . . ?
C20 N7 Cu2A O4A -62.5(12) . . . . ?
C21A N7 Cu2A O4A 78(3) . . . . ?
C20A N7 Cu2A O4A -44(3) . . . . ?
C19A N7 Cu2A O4A -176.9(15) . . . . ?
Cu2 N7 Cu2A O4A 43.9(15) . . . . ?
C4A O4A Cu2A O3A -7(3) . . . . ?
C4A O4A Cu2A N6A -160(5) . . . . ?
C4A O4A Cu2A N5A -137(3) . . . . ?
C4A O4A Cu2A N7 102(3) . . . . ?
C29 N10 Cu3A O1A -80.2(10) . . . . ?
C30A N10 Cu3A O1A 166(3) . . . . ?
C30 N10 Cu3A O1A 47.1(10) . . . . ?
C29A N10 Cu3A O1A 29(2) . . . . ?
C28 N10 Cu3A O1A 163.4(9) . . . . ?
C28A N10 Cu3A O1A -82(2) . . . . ?
Cu3 N10 Cu3A O1A 122(10) . . . . ?
C29 N10 Cu3A N9A 21.6(11) . . . . ?
C30A N10 Cu3A N9A -93(3) . . . . ?
C30 N10 Cu3A N9A 148.8(11) . . . . ?
C29A N10 Cu3A N9A 131(2) . . . . ?
C28 N10 Cu3A N9A -94.9(10) . . . . ?
C28A N10 Cu3A N9A 20(2) . . . . ?
Cu3 N10 Cu3A N9A -137(10) . . . . ?
C29 N10 Cu3A O2A -154.0(18) . . . . ?
C30A N10 Cu3A O2A 92(3) . . . . ?
C30 N10 Cu3A O2A -26.7(19) . . . . ?
C29A N10 Cu3A O2A -44(3) . . . . ?
C28 N10 Cu3A O2A 89.6(18) . . . . ?
C28A N10 Cu3A O2A -156(3) . . . . ?
Cu3 N10 Cu3A O2A 48(10) . . . . ?
C29 N10 Cu3A N8A 105.3(14) . . . . ?
C30A N10 Cu3A N8A -9(3) . . . . ?
C30 N10 Cu3A N8A -127.4(14) . . . . ?
C29A N10 Cu3A N8A -145(3) . . . . ?
C28 N10 Cu3A N8A -11.1(14) . . . . ?
C28A N10 Cu3A N8A 103(2) . . . . ?
Cu3 N10 Cu3A N8A -53(9) . . . . ?
C1A O1A Cu3A N10 -106.9(19) . . . . ?
C1A O1A Cu3A N9A 159.1(19) . . . . ?
C1A O1A Cu3A O2A 0(2) . . . . ?
C1A O1A Cu3A N8A 67(2) . . . . ?
C25A N9A Cu3A N10 136(2) . . . . ?
C26A N9A Cu3A N10 -99.6(19) . . . . ?
C27A N9A Cu3A N10 15.0(17) . . . . ?
C25A N9A Cu3A O1A -124(2) . . . . ?
C26A N9A Cu3A O1A 0(2) . . . . ?
C27A N9A Cu3A O1A 114.2(19) . . . . ?
C25A N9A Cu3A O2A -55(6) . . . . ?
C26A N9A Cu3A O2A 69(5) . . . . ?
C27A N9A Cu3A O2A -177(5) . . . . ?
C25A N9A Cu3A N8A 7(2) . . . . ?
C26A N9A Cu3A N8A 131(2) . . . . ?
C27A N9A Cu3A N8A -114.1(19) . . . . ?
C2A O2A Cu3A N10 95(5) . . . . ?
C1A O2A Cu3A N10 93.4(15) . . . . ?
C2A O2A Cu3A O1A 1(5) . . . . ?
C1A O2A Cu3A O1A 0.2(13) . . . . ?
C2A O2A Cu3A N9A -73(8) . . . . ?
C1A O2A Cu3A N9A -74(5) . . . . ?
C2A O2A Cu3A N8A -135(5) . . . . ?
C1A O2A Cu3A N8A -136.4(16) . . . . ?
C24A N8A Cu3A N10 -65(2) . . . . ?
C22A N8A Cu3A N10 178(2) . . . . ?
C23A N8A Cu3A N10 54(2) . . . . ?
C24A N8A Cu3A O1A 123(2) . . . . ?
C22A N8A Cu3A O1A 5(3) . . . . ?
C23A N8A Cu3A O1A -118(2) . . . . ?
C24A N8A Cu3A N9A 23(2) . . . . ?
C22A N8A Cu3A N9A -95(2) . . . . ?
C23A N8A Cu3A N9A 142(2) . . . . ?
C24A N8A Cu3A O2A -176(3) . . . . ?
C22A N8A Cu3A O2A 67(3) . . . . ?
C23A N8A Cu3A O2A -56(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        62.00
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.085
####################################################################### 
# 
# 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 1035435'
_audit_update_record             
;
2015-03-12 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'4(C34 H64 Cu3 N10 O4), 3(C4 H10 O), 8(N O3), 2(C H2 Cl2)'
_chemical_formula_sum            'C150 H290 Cl4 Cu12 N48 O43'
_chemical_formula_weight         4358.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.1788(11)
_cell_length_b                   29.4709(15)
_cell_length_c                   11.2788(7)
_cell_angle_alpha                90
_cell_angle_beta                 91.797(7)
_cell_angle_gamma                90
_cell_volume                     5375.1(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100
_cell_measurement_reflns_used    2177
_cell_measurement_theta_min      8.7690
_cell_measurement_theta_max      61.2200
_cell_oxdiff_twin_number         4
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 0.9988 -0.0001 0.0825 0.0028 -0.9999 0.0010 -0.0029 -0.0005 -1.0008
3 -0.9981 0.0021 0.0402 0.0043 0.9991 0.0056 -0.0188 0.0003 -1.0017
4 -1.0018 -0.0004 -0.0532 0.0030 -1.0005 -0.0073 0.0163 -0.0005 0.9998





_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_F_000             2286
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    2.338
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.84544
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;



_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21200
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_av_R_equivalents  0.1117
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.059
_diffrn_reflns_theta_max         63.132
_diffrn_reflns_theta_full        63.500
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_orient_matrix_UB_11      -0.0074575000
_diffrn_orient_matrix_UB_12      -0.0468922000
_diffrn_orient_matrix_UB_13      0.0590717000
_diffrn_orient_matrix_UB_21      -0.0046929000
_diffrn_orient_matrix_UB_22      0.0229563000
_diffrn_orient_matrix_UB_23      0.1224125000
_diffrn_orient_matrix_UB_31      -0.0949269000
_diffrn_orient_matrix_UB_32      0.0024640000
_diffrn_orient_matrix_UB_33      -0.0153308000
_diffrn_oxdiff_twin_integration_method simultaneous
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.3638 747 18003
2 0.3155 712 17991
3 0.1543 925 17942
4 0.1664 711 17990


_reflns_number_total             11546
_reflns_number_gt                6685
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;

_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 4-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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11546
_refine_ls_number_parameters     691
_refine_ls_number_restraints     716
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0994
_refine_ls_wR_factor_ref         0.2894
_refine_ls_wR_factor_gt          0.2628
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_restrained_S_all      0.939
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.003

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
C2 C 0.3574(8) 0.5755(4) 0.1236(10) 0.050(3) Uani 1 1 d . U . . .
C3 C 0.1554(7) 0.4312(4) 0.0177(10) 0.042(2) Uani 1 1 d . U . . .
C4 C 0.1419(6) 0.4322(4) 0.1515(9) 0.039(2) Uani 1 1 d . U . . .
C5 C 0.2713(5) 0.5148(2) -0.1421(5) 0.043(2) Uani 1 1 d G U . . .
C6 C 0.2950(5) 0.5301(2) -0.2526(6) 0.059(3) Uani 1 1 d G U . . .
H6 H 0.3267 0.5563 -0.2584 0.070 Uiso 1 1 calc R U . . .
C7 C 0.2713(7) 0.5062(3) -0.3544(5) 0.085(5) Uani 1 1 d G U . . .
H7 H 0.2871 0.5164 -0.4283 0.102 Uiso 1 1 calc R U . . .
C8 C 0.2239(6) 0.4671(3) -0.3457(5) 0.077(4) Uani 1 1 d G U . . .
H8 H 0.2081 0.4511 -0.4138 0.092 Uiso 1 1 calc R U . . .
C9 C 0.2002(5) 0.4518(2) -0.2352(6) 0.058(3) Uani 1 1 d G U . . .
H9 H 0.1685 0.4257 -0.2294 0.069 Uiso 1 1 calc R U . . .
C10 C 0.2239(5) 0.4757(2) -0.1334(5) 0.042(2) Uani 1 1 d G U . . .
C1 C 0.3415(7) 0.5679(4) -0.0072(9) 0.043(2) Uani 1 1 d . U . . .
C11 C 0.3404(17) 0.5482(8) 0.321(2) 0.060(6) Uani 0.60(3) 1 d D U P A 1
H11A H 0.3364 0.5795 0.3469 0.072 Uiso 0.60(3) 1 calc R U P A 1
H11B H 0.2982 0.5312 0.3615 0.072 Uiso 0.60(3) 1 calc R U P A 1
C12 C 0.4183(19) 0.5314(12) 0.360(2) 0.114(12) Uani 0.60(3) 1 d D U P A 1
H12A H 0.4197 0.5318 0.4461 0.136 Uiso 0.60(3) 1 calc R U P A 1
H12B H 0.4596 0.5528 0.3347 0.136 Uiso 0.60(3) 1 calc R U P A 1
C13 C 0.445(4) 0.4868(14) 0.324(3) 0.17(2) Uani 0.60(3) 1 d D U P A 1
H13A H 0.5028 0.4834 0.3413 0.259 Uiso 0.60(3) 1 calc R U P A 1
H13B H 0.4340 0.4832 0.2403 0.259 Uiso 0.60(3) 1 calc R U P A 1
H13C H 0.4147 0.4642 0.3663 0.259 Uiso 0.60(3) 1 calc R U P A 1
C11' C 0.325(5) 0.5628(16) 0.327(4) 0.112(14) Uani 0.40(3) 1 d D U P A 2
H11C H 0.3716 0.5832 0.3391 0.134 Uiso 0.40(3) 1 calc R U P A 2
H11D H 0.2750 0.5792 0.3450 0.134 Uiso 0.40(3) 1 calc R U P A 2
C12' C 0.335(4) 0.524(2) 0.406(3) 0.16(2) Uani 0.40(3) 1 d D U P A 2
H12C H 0.2817 0.5089 0.4118 0.194 Uiso 0.40(3) 1 calc R U P A 2
H12D H 0.3511 0.5349 0.4847 0.194 Uiso 0.40(3) 1 calc R U P A 2
C13' C 0.397(3) 0.4919(14) 0.364(3) 0.093(14) Uani 0.40(3) 1 d D U P A 2
H13D H 0.4443 0.4924 0.4168 0.140 Uiso 0.40(3) 1 calc R U P A 2
H13E H 0.4124 0.5003 0.2857 0.140 Uiso 0.40(3) 1 calc R U P A 2
H13F H 0.3734 0.4619 0.3623 0.140 Uiso 0.40(3) 1 calc R U P A 2
C14 C 0.1688(8) 0.4700(4) 0.3353(10) 0.054(3) Uani 1 1 d . U . . .
H14A H 0.2220 0.4727 0.3769 0.065 Uiso 1 1 calc R U . . .
H14B H 0.1419 0.4430 0.3645 0.065 Uiso 1 1 calc R U . . .
C15 C 0.1168(10) 0.5108(6) 0.3636(14) 0.081(4) Uani 1 1 d . U . . .
H15A H 0.1193 0.5151 0.4489 0.097 Uiso 1 1 calc R U . . .
H15B H 0.1421 0.5372 0.3284 0.097 Uiso 1 1 calc R U . . .
C16 C 0.0342(12) 0.5099(8) 0.3270(17) 0.118(7) Uani 1 1 d . U . . .
H16A H 0.0077 0.5373 0.3517 0.177 Uiso 1 1 calc R U . . .
H16B H 0.0076 0.4842 0.3618 0.177 Uiso 1 1 calc R U . . .
H16C H 0.0302 0.5075 0.2421 0.177 Uiso 1 1 calc R U . . .
C17 C 0.5514(9) 0.5528(4) 0.0295(15) 0.071(4) Uani 1 1 d . U . . .
H17A H 0.5202 0.5441 -0.0407 0.106 Uiso 1 1 calc R U . . .
H17B H 0.5219 0.5440 0.0983 0.106 Uiso 1 1 calc R U . . .
H17C H 0.6043 0.5380 0.0304 0.106 Uiso 1 1 calc R U . . .
C18 C 0.6122(10) 0.6165(5) 0.1417(15) 0.077(4) Uani 1 1 d . U . . .
H18A H 0.6212 0.6487 0.1417 0.115 Uiso 1 1 calc R U . . .
H18B H 0.6645 0.6011 0.1440 0.115 Uiso 1 1 calc R U . . .
H18C H 0.5816 0.6082 0.2101 0.115 Uiso 1 1 calc R U . . .
C19 C 0.6099(9) 0.6160(4) -0.0783(15) 0.066(3) Uani 1 1 d . U . . .
H19A H 0.5888 0.5991 -0.1466 0.079 Uiso 1 1 calc R U . . .
H19B H 0.6681 0.6090 -0.0665 0.079 Uiso 1 1 calc R U . . .
C20 C 0.5985(7) 0.6666(4) -0.0993(13) 0.057(3) Uani 1 1 d . U . . .
H20A H 0.6281 0.6835 -0.0376 0.069 Uiso 1 1 calc R U . . .
H20B H 0.6211 0.6749 -0.1750 0.069 Uiso 1 1 calc R U . . .
C21 C 0.4704(9) 0.6679(4) -0.2187(11) 0.061(3) Uani 1 1 d . U . . .
H21A H 0.4124 0.6746 -0.2175 0.092 Uiso 1 1 calc R U . . .
H21B H 0.4778 0.6363 -0.2367 0.092 Uiso 1 1 calc R U . . .
H21C H 0.4958 0.6860 -0.2780 0.092 Uiso 1 1 calc R U . . .
C22 C 0.4971(8) 0.7257(4) -0.0656(11) 0.058(3) Uani 1 1 d . U . . .
H22A H 0.5084 0.7454 -0.1321 0.069 Uiso 1 1 calc R U . . .
H22B H 0.5345 0.7338 0.0000 0.069 Uiso 1 1 calc R U . . .
C23 C 0.4077(8) 0.7317(4) -0.0293(14) 0.063(3) Uani 1 1 d . U . . .
H23A H 0.4000 0.7617 0.0034 0.076 Uiso 1 1 calc R U . . .
H23B H 0.3707 0.7283 -0.0980 0.076 Uiso 1 1 calc R U . . .
C24 C 0.4163(9) 0.7105(5) 0.1827(14) 0.074(4) Uani 1 1 d . U . . .
H24A H 0.4744 0.7172 0.1846 0.110 Uiso 1 1 calc R U . . .
H24B H 0.4057 0.6860 0.2363 0.110 Uiso 1 1 calc R U . . .
H24C H 0.3862 0.7369 0.2062 0.110 Uiso 1 1 calc R U . . .
C25 C 0.3002(8) 0.6893(6) 0.0563(13) 0.071(4) Uani 1 1 d . U . . .
H25A H 0.2828 0.6795 -0.0218 0.106 Uiso 1 1 calc R U . . .
H25B H 0.2721 0.7169 0.0753 0.106 Uiso 1 1 calc R U . . .
H25C H 0.2871 0.6663 0.1129 0.106 Uiso 1 1 calc R U . . .
C26 C 0.2025(8) 0.3183(4) 0.1335(14) 0.065(3) Uani 1 1 d . U . . .
H26A H 0.2145 0.3442 0.1824 0.097 Uiso 1 1 calc R U . . .
H26B H 0.2177 0.3245 0.0535 0.097 Uiso 1 1 calc R U . . .
H26C H 0.2334 0.2926 0.1632 0.097 Uiso 1 1 calc R U . . .
C27 C 0.0891(9) 0.2989(4) 0.2562(12) 0.063(3) Uani 1 1 d . U . . .
H27A H 0.0983 0.3252 0.3048 0.094 Uiso 1 1 calc R U . . .
H27B H 0.1204 0.2739 0.2885 0.094 Uiso 1 1 calc R U . . .
H27C H 0.0313 0.2913 0.2543 0.094 Uiso 1 1 calc R U . . .
C28 C 0.0959(8) 0.2702(4) 0.0567(12) 0.055(3) Uani 1 1 d . U . . .
H28A H 0.1071 0.2420 0.0986 0.066 Uiso 1 1 calc R U . . .
H28B H 0.1316 0.2714 -0.0108 0.066 Uiso 1 1 calc R U . . .
C29 C 0.0062(8) 0.2707(4) 0.0126(13) 0.056(3) Uani 1 1 d . U . . .
H29A H -0.0031 0.2476 -0.0475 0.067 Uiso 1 1 calc R U . . .
H29B H -0.0302 0.2649 0.0776 0.067 Uiso 1 1 calc R U . . .
C30 C 0.0265(9) 0.3203(4) -0.1596(13) 0.068(3) Uani 1 1 d . U . . .
H30A H 0.0842 0.3127 -0.1545 0.101 Uiso 1 1 calc R U . . .
H30B H 0.0200 0.3508 -0.1885 0.101 Uiso 1 1 calc R U . . .
H30C H -0.0017 0.2997 -0.2130 0.101 Uiso 1 1 calc R U . . .
C31 C -0.0994(8) 0.3270(4) -0.0438(14) 0.062(3) Uani 1 1 d . U . . .
H31A H -0.1259 0.3147 0.0252 0.075 Uiso 1 1 calc R U . . .
H31B H -0.1251 0.3136 -0.1142 0.075 Uiso 1 1 calc R U . . .
C32 C -0.1089(10) 0.3911(5) 0.1667(15) 0.078(4) Uani 1 1 d . U . . .
H32A H -0.1194 0.3593 0.1765 0.116 Uiso 1 1 calc R U . . .
H32B H -0.1604 0.4073 0.1637 0.116 Uiso 1 1 calc R U . . .
H32C H -0.0753 0.4019 0.2324 0.116 Uiso 1 1 calc R U . . .
C33 C -0.1092(10) 0.3782(5) -0.0471(16) 0.076(4) Uani 1 1 d . U . . .
H33A H -0.0872 0.3900 -0.1198 0.091 Uiso 1 1 calc R U . . .
H33B H -0.1674 0.3860 -0.0456 0.091 Uiso 1 1 calc R U . . .
C34 C -0.0518(9) 0.4457(4) 0.0384(16) 0.077(4) Uani 1 1 d . U . . .
H34A H -0.0264 0.4505 -0.0364 0.115 Uiso 1 1 calc R U . . .
H34B H -0.0161 0.4570 0.1012 0.115 Uiso 1 1 calc R U . . .
H34C H -0.1037 0.4614 0.0389 0.115 Uiso 1 1 calc R U . . .
N1 N 0.2934(6) 0.5339(3) -0.0303(8) 0.042(2) Uani 1 1 d . U . . .
N3 N 0.2040(6) 0.4635(3) -0.0186(8) 0.0412(19) Uani 1 1 d . U . . .
N2 N 0.3205(7) 0.5467(4) 0.1943(8) 0.059(3) Uani 1 1 d D U . . .
N4 N 0.1824(6) 0.4645(3) 0.2094(8) 0.046(2) Uani 1 1 d . U . . .
N7 N 0.5634(6) 0.6030(3) 0.0301(10) 0.055(2) Uani 1 1 d . U . . .
N6 N 0.5099(6) 0.6782(3) -0.0989(9) 0.053(2) Uani 1 1 d . U . . .
N5 N 0.3891(6) 0.6972(3) 0.0597(9) 0.054(2) Uani 1 1 d . U . . .
N10 N -0.0653(7) 0.3985(3) 0.0551(11) 0.061(2) Uani 1 1 d . U . . .
N9 N -0.0098(7) 0.3166(3) -0.0382(10) 0.061(2) Uani 1 1 d . U . . .
N8 N 0.1153(6) 0.3083(3) 0.1355(9) 0.051(2) Uani 1 1 d . U . . .
N11 N 0.1920(9) 0.7688(6) 0.2622(14) 0.081(5) Uani 0.78(2) 1 d D U P B 1
O5 O 0.1198(8) 0.7737(6) 0.2356(15) 0.092(5) Uani 0.78(2) 1 d D U P B 1
O6 O 0.2109(13) 0.7296(7) 0.302(2) 0.139(7) Uani 0.78(2) 1 d D U P B 1
O7 O 0.2469(9) 0.7940(7) 0.2493(19) 0.119(6) Uani 0.78(2) 1 d D U P B 1
N11' N 0.201(4) 0.783(2) 0.253(8) 0.34(6) Uani 0.22(2) 1 d D U P B 2
O5' O 0.167(5) 0.783(3) 0.156(9) 0.32(6) Uani 0.22(2) 1 d D U P B 2
O6' O 0.266(5) 0.763(3) 0.263(10) 0.35(6) Uani 0.22(2) 1 d D U P B 2
O7' O 0.172(7) 0.801(3) 0.334(9) 0.35(6) Uani 0.22(2) 1 d D U P B 2
O1 O 0.3777(5) 0.5946(2) -0.0780(7) 0.0478(17) Uani 1 1 d . U . . .
O2 O 0.4081(6) 0.6064(3) 0.1577(8) 0.063(2) Uani 1 1 d . U . . .
O3 O 0.1199(5) 0.4010(3) -0.0438(7) 0.0536(19) Uani 1 1 d . U . . .
O4 O 0.0930(5) 0.4040(3) 0.1913(7) 0.0493(18) Uani 1 1 d . U . . .
N12 N 0.699(3) 0.7455(18) 0.183(4) 0.18(2) Uani 0.34(3) 1 d D U P C 3
O8 O 0.635(4) 0.741(3) 0.236(8) 0.23(4) Uani 0.34(3) 1 d D U P C 3
O9 O 0.721(4) 0.7780(19) 0.143(6) 0.22(3) Uani 0.34(3) 1 d D U P C 3
O10 O 0.743(4) 0.7117(19) 0.182(5) 0.21(3) Uani 0.34(3) 1 d D U P C 3
N12' N 0.6976(9) 0.7267(5) 0.1874(16) 0.051(4) Uani 0.66(3) 1 d D U P C 4
O8' O 0.6272(10) 0.7365(9) 0.206(2) 0.079(6) Uani 0.66(3) 1 d D U P C 4
O9' O 0.7226(11) 0.7329(8) 0.0951(16) 0.102(8) Uani 0.66(3) 1 d D U P C 4
O10' O 0.7485(11) 0.7064(6) 0.2555(19) 0.090(6) Uani 0.66(3) 1 d D U P C 4
Cu2 Cu 0.45634(11) 0.64067(5) 0.02542(15) 0.0474(4) Uani 1 1 d . U . . .
Cu1 Cu 0.25034(12) 0.50277(5) 0.10566(14) 0.0434(4) Uani 1 1 d . U . . .
Cu3 Cu 0.04337(11) 0.36126(5) 0.07304(16) 0.0490(5) Uani 1 1 d . U . . .
C35 C 0.6419(10) 0.8317(7) -0.009(2) 0.069(5) Uani 0.5 1 d D U P . .
H35A H 0.6689 0.8268 -0.0831 0.082 Uiso 0.5 1 calc R U P . .
H35B H 0.6408 0.8030 0.0331 0.082 Uiso 0.5 1 calc R U P . .
Cl1 Cl 0.5429(6) 0.8489(2) -0.0381(6) 0.0765(19) Uani 0.5 1 d D U P . .
Cl2 Cl 0.7000(7) 0.8707(3) 0.0764(8) 0.110(3) Uani 0.5 1 d D U P . .
O11 O -0.063(2) 0.1474(11) 0.025(3) 0.110(6) Uani 0.391(17) 1 d D U P D 1
C36 C -0.198(3) 0.1401(13) 0.122(4) 0.110(6) Uani 0.391(17) 1 d D U P D 1
H36A H -0.2526 0.1274 0.1111 0.165 Uiso 0.391(17) 1 calc R U P D 1
H36B H -0.2027 0.1723 0.1343 0.165 Uiso 0.391(17) 1 calc R U P D 1
H36C H -0.1713 0.1265 0.1905 0.165 Uiso 0.391(17) 1 calc R U P D 1
C37 C -0.150(2) 0.1312(14) 0.017(3) 0.110(6) Uani 0.391(17) 1 d D U P D 1
H37A H -0.1770 0.1457 -0.0512 0.132 Uiso 0.391(17) 1 calc R U P D 1
H37B H -0.1494 0.0988 0.0019 0.132 Uiso 0.391(17) 1 calc R U P D 1
C38 C 0.007(2) 0.1177(11) 0.010(4) 0.110(6) Uani 0.391(17) 1 d D U P D 1
H38A H 0.0084 0.1083 -0.0726 0.132 Uiso 0.391(17) 1 calc R U P D 1
H38B H 0.0006 0.0907 0.0579 0.132 Uiso 0.391(17) 1 calc R U P D 1
C39 C 0.087(3) 0.1402(15) 0.044(5) 0.110(6) Uani 0.391(17) 1 d D U P D 1
H39A H 0.1303 0.1276 -0.0017 0.165 Uiso 0.391(17) 1 calc R U P D 1
H39B H 0.0988 0.1353 0.1268 0.165 Uiso 0.391(17) 1 calc R U P D 1
H39C H 0.0823 0.1722 0.0286 0.165 Uiso 0.391(17) 1 calc R U P D 1
O11' O -0.099(3) 0.1434(10) 0.063(3) 0.110(6) Uani 0.359(17) 1 d D U P D 2
C36' C -0.243(3) 0.1341(14) 0.046(4) 0.110(6) Uani 0.359(17) 1 d D U P D 2
H36D H -0.2904 0.1237 -0.0001 0.165 Uiso 0.359(17) 1 calc R U P D 2
H36E H -0.2427 0.1666 0.0473 0.165 Uiso 0.359(17) 1 calc R U P D 2
H36F H -0.2459 0.1227 0.1254 0.165 Uiso 0.359(17) 1 calc R U P D 2
C37' C -0.168(3) 0.1177(14) -0.007(4) 0.110(6) Uani 0.359(17) 1 d D U P D 2
H37C H -0.1676 0.1250 -0.0912 0.132 Uiso 0.359(17) 1 calc R U P D 2
H37D H -0.1622 0.0851 0.0025 0.132 Uiso 0.359(17) 1 calc R U P D 2
C38' C -0.024(3) 0.143(2) 0.003(4) 0.110(6) Uani 0.359(17) 1 d D U P D 2
H38C H -0.0194 0.1727 -0.0337 0.132 Uiso 0.359(17) 1 calc R U P D 2
H38D H -0.0319 0.1217 -0.0622 0.132 Uiso 0.359(17) 1 calc R U P D 2
C39' C 0.059(3) 0.1332(17) 0.052(5) 0.110(6) Uani 0.359(17) 1 d D U P D 2
H39D H 0.0992 0.1389 -0.0062 0.165 Uiso 0.359(17) 1 calc R U P D 2
H39E H 0.0616 0.1020 0.0764 0.165 Uiso 0.359(17) 1 calc R U P D 2
H39F H 0.0696 0.1523 0.1201 0.165 Uiso 0.359(17) 1 calc R U P D 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 O2 1.277(14) . ?
C2 N2 1.320(15) . ?
C2 C1 1.507(16) . ?
C3 O3 1.256(13) . ?
C3 N3 1.308(14) . ?
C3 C4 1.532(16) . ?
C4 O4 1.241(13) . ?
C4 N4 1.317(14) . ?
C5 C6 1.3900 . ?
C5 C10 1.3900 . ?
C5 N1 1.416(10) . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 C9 1.3900 . ?
C8 H8 0.9300 . ?
C9 C10 1.3900 . ?
C9 H9 0.9300 . ?
C10 N3 1.391(10) . ?
C1 O1 1.277(13) . ?
C1 N1 1.292(14) . ?
C11 C12 1.41(2) . ?
C11 N2 1.46(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.44(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C11' C12' 1.45(2) . ?
C11' N2 1.57(5) . ?
C11' H11C 0.9700 . ?
C11' H11D 0.9700 . ?
C12' C13' 1.47(2) . ?
C12' H12C 0.9700 . ?
C12' H12D 0.9700 . ?
C13' H13D 0.9600 . ?
C13' H13E 0.9600 . ?
C13' H13F 0.9600 . ?
C14 N4 1.452(15) . ?
C14 C15 1.507(19) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.39(2) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N7 1.492(15) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N7 1.517(19) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 N7 1.505(18) . ?
C19 C20 1.520(17) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N6 1.474(15) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 N6 1.506(17) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 N6 1.466(15) . ?
C22 C23 1.526(18) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 N5 1.467(17) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 N5 1.494(18) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 N5 1.457(17) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 N8 1.443(16) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 N8 1.465(17) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 N8 1.459(16) . ?
C28 C29 1.519(18) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 N9 1.490(16) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 N9 1.510(18) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 N9 1.482(16) . ?
C31 C33 1.516(18) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 N10 1.48(2) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N10 1.463(19) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 N10 1.422(16) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
N1 Cu1 1.935(9) . ?
N3 Cu1 1.949(10) . ?
N2 Cu1 1.972(10) . ?
N4 Cu1 1.982(9) . ?
N7 Cu2 2.056(10) . ?
N6 Cu2 2.004(10) . ?
N5 Cu2 2.032(10) . ?
N10 Cu3 2.077(11) . ?
N9 Cu3 1.994(11) . ?
N8 Cu3 2.058(10) . ?
N11 O7 1.172(18) . ?
N11 O5 1.205(15) . ?
N11 O6 1.271(18) . ?
N11' O7' 1.16(2) . ?
N11' O5' 1.21(2) . ?
N11' O6' 1.21(2) . ?
O1 Cu2 2.174(8) . ?
O2 Cu2 1.982(9) . ?
O3 Cu3 2.179(8) . ?
O4 Cu3 1.987(8) . ?
N12 O9 1.12(2) . ?
N12 O8 1.22(2) . ?
N12 O10 1.22(2) . ?
N12' O9' 1.143(17) . ?
N12' O8' 1.202(16) . ?
N12' O10' 1.259(17) . ?
C35 Cl1 1.703(15) . ?
C35 Cl2 1.752(14) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
O11 C38 1.44(2) . ?
O11 C37 1.49(2) . ?
C36 C37 1.47(2) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.49(2) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
O11' C38' 1.41(2) . ?
O11' C37' 1.55(2) . ?
C36' C37' 1.45(2) . ?
C36' H36D 0.9600 . ?
C36' H36E 0.9600 . ?
C36' H36F 0.9600 . ?
C37' H37C 0.9700 . ?
C37' H37D 0.9700 . ?
C38' C39' 1.46(2) . ?
C38' H38C 0.9700 . ?
C38' H38D 0.9700 . ?
C39' H39D 0.9600 . ?
C39' H39E 0.9600 . ?
C39' H39F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C2 N2 125.1(10) . . ?
O2 C2 C1 119.2(10) . . ?
N2 C2 C1 115.5(10) . . ?
O3 C3 N3 127.6(10) . . ?
O3 C3 C4 118.8(10) . . ?
N3 C3 C4 113.6(10) . . ?
O4 C4 N4 128.1(10) . . ?
O4 C4 C3 117.1(10) . . ?
N4 C4 C3 114.7(9) . . ?
C6 C5 C10 120.0 . . ?
C6 C5 N1 127.0(5) . . ?
C10 C5 N1 113.0(5) . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 120.0 . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 120.0 . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C5 120.0 . . ?
C9 C10 N3 124.9(5) . . ?
C5 C10 N3 115.1(5) . . ?
O1 C1 N1 129.7(10) . . ?
O1 C1 C2 117.0(9) . . ?
N1 C1 C2 113.3(9) . . ?
C12 C11 N2 117(2) . . ?
C12 C11 H11A 107.9 . . ?
N2 C11 H11A 107.9 . . ?
C12 C11 H11B 107.9 . . ?
N2 C11 H11B 108.0 . . ?
H11A C11 H11B 107.2 . . ?
C11 C12 C13 120(3) . . ?
C11 C12 H12A 107.3 . . ?
C13 C12 H12A 107.3 . . ?
C11 C12 H12B 107.3 . . ?
C13 C12 H12B 107.3 . . ?
H12A C12 H12B 106.9 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.4 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12' C11' N2 110(3) . . ?
C12' C11' H11C 109.6 . . ?
N2 C11' H11C 109.6 . . ?
C12' C11' H11D 109.5 . . ?
N2 C11' H11D 109.5 . . ?
H11C C11' H11D 108.1 . . ?
C11' C12' C13' 112(3) . . ?
C11' C12' H12C 109.3 . . ?
C13' C12' H12C 109.3 . . ?
C11' C12' H12D 109.2 . . ?
C13' C12' H12D 109.3 . . ?
H12C C12' H12D 107.9 . . ?
C12' C13' H13D 109.5 . . ?
C12' C13' H13E 109.5 . . ?
H13D C13' H13E 109.5 . . ?
C12' C13' H13F 109.4 . . ?
H13D C13' H13F 109.5 . . ?
H13E C13' H13F 109.5 . . ?
N4 C14 C15 113.4(11) . . ?
N4 C14 H14A 108.9 . . ?
C15 C14 H14A 108.9 . . ?
N4 C14 H14B 108.9 . . ?
C15 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C16 C15 C14 117.5(16) . . ?
C16 C15 H15A 107.9 . . ?
C14 C15 H15A 107.9 . . ?
C16 C15 H15B 107.9 . . ?
C14 C15 H15B 107.9 . . ?
H15A C15 H15B 107.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N7 C17 H17A 109.5 . . ?
N7 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N7 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N7 C18 H18A 109.5 . . ?
N7 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N7 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N7 C19 C20 108.4(11) . . ?
N7 C19 H19A 110.0 . . ?
C20 C19 H19A 110.0 . . ?
N7 C19 H19B 110.0 . . ?
C20 C19 H19B 110.0 . . ?
H19A C19 H19B 108.4 . . ?
N6 C20 C19 109.8(10) . . ?
N6 C20 H20A 109.7 . . ?
C19 C20 H20A 109.7 . . ?
N6 C20 H20B 109.7 . . ?
C19 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
N6 C21 H21A 109.5 . . ?
N6 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N6 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N6 C22 C23 108.8(10) . . ?
N6 C22 H22A 109.9 . . ?
C23 C22 H22A 109.9 . . ?
N6 C22 H22B 109.9 . . ?
C23 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
N5 C23 C22 108.6(10) . . ?
N5 C23 H23A 110.0 . . ?
C22 C23 H23A 110.0 . . ?
N5 C23 H23B 110.0 . . ?
C22 C23 H23B 110.0 . . ?
H23A C23 H23B 108.3 . . ?
N5 C24 H24A 109.5 . . ?
N5 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N5 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N5 C25 H25A 109.5 . . ?
N5 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N5 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N8 C26 H26A 109.5 . . ?
N8 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N8 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N8 C27 H27A 109.5 . . ?
N8 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N8 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N8 C28 C29 112.1(10) . . ?
N8 C28 H28A 109.2 . . ?
C29 C28 H28A 109.2 . . ?
N8 C28 H28B 109.2 . . ?
C29 C28 H28B 109.2 . . ?
H28A C28 H28B 107.9 . . ?
N9 C29 C28 106.7(10) . . ?
N9 C29 H29A 110.4 . . ?
C28 C29 H29A 110.4 . . ?
N9 C29 H29B 110.4 . . ?
C28 C29 H29B 110.4 . . ?
H29A C29 H29B 108.6 . . ?
N9 C30 H30A 109.5 . . ?
N9 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N9 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N9 C31 C33 108.0(11) . . ?
N9 C31 H31A 110.1 . . ?
C33 C31 H31A 110.1 . . ?
N9 C31 H31B 110.1 . . ?
C33 C31 H31B 110.1 . . ?
H31A C31 H31B 108.4 . . ?
N10 C32 H32A 109.5 . . ?
N10 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N10 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N10 C33 C31 109.9(12) . . ?
N10 C33 H33A 109.7 . . ?
C31 C33 H33A 109.7 . . ?
N10 C33 H33B 109.7 . . ?
C31 C33 H33B 109.7 . . ?
H33A C33 H33B 108.2 . . ?
N10 C34 H34A 109.5 . . ?
N10 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N10 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C1 N1 C5 128.4(8) . . ?
C1 N1 Cu1 116.0(7) . . ?
C5 N1 Cu1 115.5(6) . . ?
C3 N3 C10 129.7(9) . . ?
C3 N3 Cu1 115.3(7) . . ?
C10 N3 Cu1 114.9(6) . . ?
C2 N2 C11 118.9(14) . . ?
C2 N2 C11' 112(2) . . ?
C2 N2 Cu1 112.3(7) . . ?
C11 N2 Cu1 128.6(12) . . ?
C11' N2 Cu1 134(3) . . ?
C4 N4 C14 118.5(10) . . ?
C4 N4 Cu1 113.2(7) . . ?
C14 N4 Cu1 128.2(8) . . ?
C17 N7 C19 108.5(10) . . ?
C17 N7 C18 109.1(11) . . ?
C19 N7 C18 110.4(10) . . ?
C17 N7 Cu2 115.2(8) . . ?
C19 N7 Cu2 106.5(8) . . ?
C18 N7 Cu2 107.2(8) . . ?
C22 N6 C20 111.5(10) . . ?
C22 N6 C21 111.3(10) . . ?
C20 N6 C21 109.6(10) . . ?
C22 N6 Cu2 106.2(7) . . ?
C20 N6 Cu2 108.5(8) . . ?
C21 N6 Cu2 109.6(7) . . ?
C25 N5 C23 108.4(11) . . ?
C25 N5 C24 109.2(10) . . ?
C23 N5 C24 113.1(11) . . ?
C25 N5 Cu2 113.5(9) . . ?
C23 N5 Cu2 108.4(8) . . ?
C24 N5 Cu2 104.4(8) . . ?
C34 N10 C33 111.6(12) . . ?
C34 N10 C32 109.7(12) . . ?
C33 N10 C32 112.1(11) . . ?
C34 N10 Cu3 113.4(9) . . ?
C33 N10 Cu3 104.4(8) . . ?
C32 N10 Cu3 105.3(9) . . ?
C31 N9 C29 111.3(10) . . ?
C31 N9 C30 110.7(11) . . ?
C29 N9 C30 110.3(10) . . ?
C31 N9 Cu3 107.0(8) . . ?
C29 N9 Cu3 106.9(8) . . ?
C30 N9 Cu3 110.6(8) . . ?
C26 N8 C28 109.8(10) . . ?
C26 N8 C27 111.4(11) . . ?
C28 N8 C27 111.0(9) . . ?
C26 N8 Cu3 112.5(7) . . ?
C28 N8 Cu3 105.5(8) . . ?
C27 N8 Cu3 106.5(8) . . ?
O7 N11 O5 129(2) . . ?
O7 N11 O6 116.4(18) . . ?
O5 N11 O6 114.6(19) . . ?
O7' N11' O5' 122(4) . . ?
O7' N11' O6' 121(4) . . ?
O5' N11' O6' 117(4) . . ?
C1 O1 Cu2 108.7(7) . . ?
C2 O2 Cu2 113.7(7) . . ?
C3 O3 Cu3 107.8(7) . . ?
C4 O4 Cu3 115.5(7) . . ?
O9 N12 O8 125(4) . . ?
O9 N12 O10 120(4) . . ?
O8 N12 O10 115(4) . . ?
O9' N12' O8' 119.1(19) . . ?
O9' N12' O10' 112.8(18) . . ?
O8' N12' O10' 128(2) . . ?
O2 Cu2 N6 175.6(4) . . ?
O2 Cu2 N5 92.8(4) . . ?
N6 Cu2 N5 85.8(4) . . ?
O2 Cu2 N7 93.2(4) . . ?
N6 Cu2 N7 86.2(4) . . ?
N5 Cu2 N7 153.2(4) . . ?
O2 Cu2 O1 81.3(3) . . ?
N6 Cu2 O1 103.1(4) . . ?
N5 Cu2 O1 107.8(4) . . ?
N7 Cu2 O1 98.9(4) . . ?
N1 Cu1 N3 81.4(3) . . ?
N1 Cu1 N2 82.8(4) . . ?
N3 Cu1 N2 163.0(4) . . ?
N1 Cu1 N4 163.2(4) . . ?
N3 Cu1 N4 83.1(4) . . ?
N2 Cu1 N4 113.2(4) . . ?
O4 Cu3 N9 176.8(4) . . ?
O4 Cu3 N8 92.3(4) . . ?
N9 Cu3 N8 86.7(4) . . ?
O4 Cu3 N10 93.0(4) . . ?
N9 Cu3 N10 86.6(4) . . ?
N8 Cu3 N10 154.4(4) . . ?
O4 Cu3 O3 80.7(3) . . ?
N9 Cu3 O3 102.5(4) . . ?
N8 Cu3 O3 106.8(4) . . ?
N10 Cu3 O3 98.7(4) . . ?
Cl1 C35 Cl2 113.4(11) . . ?
Cl1 C35 H35A 108.9 . . ?
Cl2 C35 H35A 108.9 . . ?
Cl1 C35 H35B 108.9 . . ?
Cl2 C35 H35B 108.9 . . ?
H35A C35 H35B 107.7 . . ?
C38 O11 C37 123(3) . . ?
C37 C36 H36A 109.5 . . ?
C37 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C37 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C36 C37 O11 115(3) . . ?
C36 C37 H37A 108.6 . . ?
O11 C37 H37A 108.6 . . ?
C36 C37 H37B 108.6 . . ?
O11 C37 H37B 108.6 . . ?
H37A C37 H37B 107.6 . . ?
O11 C38 C39 112(3) . . ?
O11 C38 H38A 109.1 . . ?
C39 C38 H38A 109.2 . . ?
O11 C38 H38B 109.4 . . ?
C39 C38 H38B 109.4 . . ?
H38A C38 H38B 108.0 . . ?
C38 C39 H39A 109.6 . . ?
C38 C39 H39B 109.3 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38' O11' C37' 112(3) . . ?
C37' C36' H36D 109.4 . . ?
C37' C36' H36E 109.5 . . ?
H36D C36' H36E 109.5 . . ?
C37' C36' H36F 109.5 . . ?
H36D C36' H36F 109.5 . . ?
H36E C36' H36F 109.5 . . ?
C36' C37' O11' 103(3) . . ?
C36' C37' H37C 111.2 . . ?
O11' C37' H37C 111.1 . . ?
C36' C37' H37D 111.1 . . ?
O11' C37' H37D 111.1 . . ?
H37C C37' H37D 109.1 . . ?
O11' C38' C39' 127(4) . . ?
O11' C38' H38C 105.4 . . ?
C39' C38' H38C 105.4 . . ?
O11' C38' H38D 105.5 . . ?
C39' C38' H38D 105.5 . . ?
H38C C38' H38D 106.0 . . ?
C38' C39' H39D 109.5 . . ?
C38' C39' H39E 109.4 . . ?
H39D C39' H39E 109.5 . . ?
C38' C39' H39F 109.5 . . ?
H39D C39' H39F 109.5 . . ?
H39E C39' H39F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 C3 C4 O4 -3.3(16) . . . . ?
N3 C3 C4 O4 176.3(9) . . . . ?
O3 C3 C4 N4 179.0(10) . . . . ?
N3 C3 C4 N4 -1.3(14) . . . . ?
C10 C5 C6 C7 0.0 . . . . ?
N1 C5 C6 C7 176.8(9) . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C8 C9 C10 C5 0.0 . . . . ?
C8 C9 C10 N3 -179.8(9) . . . . ?
C6 C5 C10 C9 0.0 . . . . ?
N1 C5 C10 C9 -177.2(8) . . . . ?
C6 C5 C10 N3 179.8(8) . . . . ?
N1 C5 C10 N3 2.6(8) . . . . ?
O2 C2 C1 O1 -3.0(17) . . . . ?
N2 C2 C1 O1 -178.5(11) . . . . ?
O2 C2 C1 N1 175.6(11) . . . . ?
N2 C2 C1 N1 0.1(16) . . . . ?
N2 C11 C12 C13 -52(4) . . . . ?
N2 C11' C12' C13' 45(7) . . . . ?
N4 C14 C15 C16 68(2) . . . . ?
N7 C19 C20 N6 -51.1(15) . . . . ?
N6 C22 C23 N5 51.8(13) . . . . ?
N8 C28 C29 N9 52.4(14) . . . . ?
N9 C31 C33 N10 -55.7(16) . . . . ?
O1 C1 N1 C5 4(2) . . . . ?
C2 C1 N1 C5 -174.1(10) . . . . ?
O1 C1 N1 Cu1 -179.2(10) . . . . ?
C2 C1 N1 Cu1 2.3(13) . . . . ?
C6 C5 N1 C1 -2.4(15) . . . . ?
C10 C5 N1 C1 174.5(10) . . . . ?
C6 C5 N1 Cu1 -178.9(5) . . . . ?
C10 C5 N1 Cu1 -1.9(9) . . . . ?
O3 C3 N3 C10 6.2(19) . . . . ?
C4 C3 N3 C10 -173.4(10) . . . . ?
O3 C3 N3 Cu1 -178.0(9) . . . . ?
C4 C3 N3 Cu1 2.4(12) . . . . ?
C9 C10 N3 C3 -6.5(15) . . . . ?
C5 C10 N3 C3 173.7(10) . . . . ?
C9 C10 N3 Cu1 177.6(5) . . . . ?
C5 C10 N3 Cu1 -2.1(9) . . . . ?
O2 C2 N2 C11 -2(2) . . . . ?
C1 C2 N2 C11 172.7(14) . . . . ?
O2 C2 N2 C11' 17(3) . . . . ?
C1 C2 N2 C11' -168(3) . . . . ?
O2 C2 N2 Cu1 -177.6(10) . . . . ?
C1 C2 N2 Cu1 -2.4(14) . . . . ?
C12 C11 N2 C2 -73(3) . . . . ?
C12 C11 N2 C11' -145(12) . . . . ?
C12 C11 N2 Cu1 101(3) . . . . ?
C12' C11' N2 C2 -144(4) . . . . ?
C12' C11' N2 C11 -28(7) . . . . ?
C12' C11' N2 Cu1 54(6) . . . . ?
O4 C4 N4 C14 -1.5(17) . . . . ?
C3 C4 N4 C14 175.8(10) . . . . ?
O4 C4 N4 Cu1 -177.7(9) . . . . ?
C3 C4 N4 Cu1 -0.4(12) . . . . ?
C15 C14 N4 C4 -105.8(14) . . . . ?
C15 C14 N4 Cu1 69.7(15) . . . . ?
C20 C19 N7 C17 162.2(11) . . . . ?
C20 C19 N7 C18 -78.3(14) . . . . ?
C20 C19 N7 Cu2 37.7(12) . . . . ?
C23 C22 N6 C20 -162.5(11) . . . . ?
C23 C22 N6 C21 74.7(13) . . . . ?
C23 C22 N6 Cu2 -44.5(11) . . . . ?
C19 C20 N6 C22 154.5(11) . . . . ?
C19 C20 N6 C21 -81.8(13) . . . . ?
C19 C20 N6 Cu2 37.8(13) . . . . ?
C22 C23 N5 C25 -155.4(11) . . . . ?
C22 C23 N5 C24 83.4(13) . . . . ?
C22 C23 N5 Cu2 -31.9(12) . . . . ?
C31 C33 N10 C34 162.7(12) . . . . ?
C31 C33 N10 C32 -73.7(15) . . . . ?
C31 C33 N10 Cu3 39.8(14) . . . . ?
C33 C31 N9 C29 157.3(12) . . . . ?
C33 C31 N9 C30 -79.7(14) . . . . ?
C33 C31 N9 Cu3 40.9(13) . . . . ?
C28 C29 N9 C31 -159.3(11) . . . . ?
C28 C29 N9 C30 77.4(13) . . . . ?
C28 C29 N9 Cu3 -42.9(11) . . . . ?
C29 C28 N8 C26 -155.1(10) . . . . ?
C29 C28 N8 C27 81.3(13) . . . . ?
C29 C28 N8 Cu3 -33.6(11) . . . . ?
N1 C1 O1 Cu2 -175.6(11) . . . . ?
C2 C1 O1 Cu2 2.8(12) . . . . ?
N2 C2 O2 Cu2 176.4(11) . . . . ?
C1 C2 O2 Cu2 1.3(15) . . . . ?
N3 C3 O3 Cu3 -176.8(10) . . . . ?
C4 C3 O3 Cu3 2.8(12) . . . . ?
N4 C4 O4 Cu3 179.0(9) . . . . ?
C3 C4 O4 Cu3 1.8(12) . . . . ?
C38 O11 C37 C36 123(5) . . . . ?
C37 O11 C38 C39 -170(3) . . . . ?
C38' O11' C37' C36' -162(4) . . . . ?
C37' O11' C38' C39' -134(6) . . . . ?

_refine_diff_density_max         1.564
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.166

# start Validation Reply Form
_vrf_PLAT410_shelx               
;
PROBLEM: Short Intra H...H Contact  H14A   ..  H12C    ..       1.48 Ang.  
RESPONSE: Alerted short Intra and/or Inter H...H contacts refer to such
H atoms, which belong to the n-Propyl groups (H12C, H12D and H16A). 
The C atoms of the n-Propyl groups have comparatively large Ueq values -
and one n-Propyl group (C11-C13) could be refined disordered. Obviously,
the chosen model of disorder is not sufficient to avoid the alerted
H...H contacts. Trials to refine the other n-Propyl group as being 
disordered gave then only non-reliable results. Most likely, this is
due to the multicrystalline nature of the crystal, cf.:
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.3638 747 18003
2 0.3155 712 17991
3 0.1543 925 17942
4 0.1664 711 17990

;
_vrf_PLAT411_shelx               
;
PROBLEM: Short Inter H...H Contact  H7     ..  H12D    ..       1.55 Ang.  
RESPONSE: cf. above
;
_vrf_PLAT413_shelx               
;
PROBLEM: Short Inter XH3 .. XHn     H16A   ..  H38B    ..       1.88 Ang.  
RESPONSE: cf. above
;
_vrf_PLAT341_shelx               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0151 Ang.  
RESPONSE: This alert is attributed to the multicrystalline nature of
the crystal, cf. above.
;
# end Validation Reply Form

_shelxl_version_number           2013-4

