# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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. 
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data_6a_DMF
_database_code_depnum_ccdc_archive 'CCDC 1519348'
_audit_update_record             
;
2017-01-22 deposited with the CCDC.
2017-01-27 downloaded from the CCDC.
;
_audit_creation_date             2017-01-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/4
# start Validation Reply Form
_vrf_PLAT029_6a_DMF              
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.917 Note
RESPONSE: This is slightly lower than ideal, 
 but the quality of the data and solution are excellent. 
;
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H30 N4 O8, C24 H32 O8, 1.6(C3 H7 N O)'
_chemical_formula_sum            'C76.80 H73.20 N5.60 O17.60'
_chemical_formula_weight         1356.21
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.0014(3)
_cell_length_b                   14.3032(6)
_cell_length_c                   15.5636(8)
_cell_angle_alpha                76.9517(16)
_cell_angle_beta                 79.6241(15)
_cell_angle_gamma                81.520(2)
_cell_volume                     1696.19(13)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4408
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.94
_shelx_estimated_absorpt_T_max   0.986
_shelx_estimated_absorpt_T_min   0.978
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7011
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_special_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0425 before and 0.0364 after correction.
The Ratio of minimum to maximum transmission is 0.9403.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rectanglar
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10864
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.346
_diffrn_ambient_temperature      173.2
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4784
_reflns_number_total             6336
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6336
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0449
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0542P)²+0.6939P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1179
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Sof(H04I)=Sof(H04J)=Sof(C0)=Sof(H0A)=Sof(H0B)=1-FVAR(1)
 Sof(H04G)=Sof(H04H)=Sof(C049)=Sof(H04K)=Sof(H04L)=FVAR(1)
 Fixed Sof: O047(0.8) N044(0.8) C048(0.8) H048(0.8) C050(0.8) H05A(0.8)
 H05B(0.8) H05C(0.8) C051(0.8) H05D(0.8) H05E(0.8) H05F(0.8)
3.a Secondary CH2 refined with riding coordinates:
 C038(H03A,H03B), C042(H04A,H04B), C043(H04C,H04D), C045(H04E,H04F), C046(H04G,
 H04H), C046(H04I,H04J), C049(H04K,H04L), C0(H0A,H0B)
3.b Aromatic/amide H refined with riding coordinates:
 N006(H006), C014(H014), C015(H015), C016(H016), C022(H022), C025(H025),
 C026(H026), C028(H028), C029(H029), C031(H031), C033(H033), C034(H034),
 C037(H037), C035(H035), C036(H036), C039(H039), C041(H041), C048(H048)
3.c Idealised Me refined as rotating group:
 C050(H05A,H05B,H05C), C051(H05D,H05E,H05F)
3.d Idealised tetrahedral OH refined as rotating group:
 O004(H004), O005(H005)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O002 O 0.84479(18) 0.58257(10) 0.33722(9) 0.0310(3) Uani 1 1 d . . . . .
O003 O 0.8199(2) 0.55132(11) -0.44594(9) 0.0361(4) Uani 1 1 d . . . . .
O004 O 0.6919(2) 0.47860(11) 0.43982(9) 0.0348(4) Uani 1 1 d . . . . .
H004 H 0.729334 0.504382 0.474883 0.052 Uiso 1 1 calc GR . . . .
O005 O 0.9660(2) 0.65788(10) -0.54896(9) 0.0347(4) Uani 1 1 d . . . . .
H005 H 0.930226 0.630982 -0.583762 0.052 Uiso 1 1 calc GR . . . .
N006 N 0.62016(18) 0.72608(10) 0.04190(9) 0.0161(3) Uani 1 1 d . . . . .
H006 H 0.571611 0.722897 0.097754 0.019 Uiso 1 1 calc R . . . .
N007 N 0.71470(18) 0.79062(10) -0.10091(9) 0.0165(3) Uani 1 1 d . . . . .
C009 C 0.9072(2) 0.67555(13) -0.24133(11) 0.0183(4) Uani 1 1 d . . . . .
C010 C 0.9467(2) 0.66745(13) -0.39793(12) 0.0217(4) Uani 1 1 d . . . . .
C011 C 0.6325(2) 0.80809(12) -0.02351(11) 0.0153(3) Uani 1 1 d . . . . .
C012 C 0.7464(2) 0.51947(13) 0.35729(12) 0.0228(4) Uani 1 1 d . . . . .
C014 C 0.7140(2) 0.53456(12) 0.19968(11) 0.0182(4) Uani 1 1 d . . . . .
H014 H 0.767532 0.592250 0.186468 0.022 Uiso 1 1 calc R . . . .
C015 C 0.9912(2) 0.75861(13) -0.26537(12) 0.0237(4) Uani 1 1 d . . . . .
H015 H 1.005221 0.791034 -0.220603 0.028 Uiso 1 1 calc R . . . .
C016 C 0.5873(2) 0.41667(13) 0.15227(12) 0.0229(4) Uani 1 1 d . . . . .
H016 H 0.555421 0.392547 0.106162 0.027 Uiso 1 1 calc R . . . .
C017 C 0.6679(2) 0.50094(12) 0.13073(11) 0.0171(4) Uani 1 1 d . . . . .
C018 C 0.7173(2) 0.54867(12) 0.03618(11) 0.0166(4) Uani 1 1 d . . . . .
C019 C 0.6823(2) 0.48437(13) 0.28776(12) 0.0215(4) Uani 1 1 d . . . . .
C020 C 0.8416(2) 0.63415(12) -0.14713(11) 0.0165(4) Uani 1 1 d . . . . .
C021 C 0.7579(2) 0.69149(12) -0.08582(11) 0.0155(3) Uani 1 1 d . . . . .
C022 C 0.8852(2) 0.63043(13) -0.30860(11) 0.0192(4) Uani 1 1 d . . . . .
H022 H 0.827867 0.573973 -0.293502 0.023 Uiso 1 1 calc R . . . .
C024 C 0.6985(2) 0.64921(12) 0.00348(11) 0.0159(3) Uani 1 1 d . . . . .
C025 C 0.6256(2) 0.98502(12) -0.07121(11) 0.0181(4) Uani 1 1 d . . . . .
H025 H 0.711563 0.974873 -0.119993 0.022 Uiso 1 1 calc R . . . .
C026 C 0.8570(2) 0.53488(12) -0.11467(12) 0.0189(4) Uani 1 1 d . . . . .
H026 H 0.910571 0.493591 -0.154061 0.023 Uiso 1 1 calc R . . . .
C027 C 0.9063(2) 0.61999(14) -0.46630(12) 0.0248(4) Uani 1 1 d . . . . .
C028 C 0.7968(2) 0.49363(12) -0.02633(12) 0.0191(4) Uani 1 1 d . . . . .
H028 H 0.810465 0.425291 -0.008057 0.023 Uiso 1 1 calc R . . . .
C029 C 1.0330(2) 0.74857(14) -0.42095(13) 0.0271(4) Uani 1 1 d . . . . .
H029 H 1.077094 0.772784 -0.481546 0.032 Uiso 1 1 calc R . . . .
C030 C 0.5641(2) 0.90578(12) -0.00982(11) 0.0163(3) Uani 1 1 d . . . . .
C031 C 0.5628(2) 1.07846(12) -0.06184(11) 0.0179(4) Uani 1 1 d . . . . .
H031 H 0.605834 1.131832 -0.104047 0.021 Uiso 1 1 calc R . . . .
C033 C 0.5999(2) 0.40125(14) 0.30829(13) 0.0257(4) Uani 1 1 d . . . . .
H033 H 0.575814 0.367723 0.368423 0.031 Uiso 1 1 calc R . . . .
C034 C 1.0546(3) 0.79446(14) -0.35425(13) 0.0279(4) Uani 1 1 d . . . . .
H034 H 1.112924 0.850553 -0.369567 0.034 Uiso 1 1 calc R . . . .
C037 C 0.5532(3) 0.36788(14) 0.23989(13) 0.0280(4) Uani 1 1 d . . . . .
H037 H 0.497248 0.311003 0.253374 0.034 Uiso 1 1 calc R . . . .
O001 O 0.39354(16) 0.70020(9) 0.21881(9) 0.0250(3) Uani 1 1 d . . . . .
O008 O 0.18910(17) 0.74812(10) 0.07305(9) 0.0325(3) Uani 1 1 d . . . . .
O013 O 0.58531(19) 0.84242(11) 0.23745(10) 0.0390(4) Uani 1 1 d . . . . .
O023 O 0.95420(18) 1.08788(11) 0.11709(10) 0.0351(4) Uani 1 1 d . . . . .
C032 C 0.8994(2) 1.01171(14) 0.18204(13) 0.0274(4) Uani 1 1 d . . . . .
C035 C 0.9412(3) 0.90955(16) 0.32250(14) 0.0326(5) Uani 1 1 d . . . . .
H035 H 1.001575 0.891528 0.372053 0.039 Uiso 1 1 calc R . . . .
C036 C 0.7675(3) 0.96130(15) 0.17738(14) 0.0303(5) Uani 1 1 d . . . . .
H036 H 0.709152 0.978275 0.127054 0.036 Uiso 1 1 calc R . . . .
C038 C 0.1198(2) 0.71358(15) 0.16291(14) 0.0296(4) Uani 1 1 d . . . . .
H03A H 0.023444 0.676261 0.165593 0.036 Uiso 1 1 calc R . . . .
H03B H 0.076164 0.768502 0.192752 0.036 Uiso 1 1 calc R . . . .
C039 C 0.8078(3) 0.85827(15) 0.32004(14) 0.0316(5) Uani 1 1 d . . . . .
H039 H 0.776926 0.805842 0.367162 0.038 Uiso 1 1 calc R . . . .
C040 C 0.7212(3) 0.88549(15) 0.24720(14) 0.0300(4) Uani 1 1 d . . . . .
C041 C 0.9876(2) 0.98563(15) 0.25502(13) 0.0288(4) Uani 1 1 d . . . . .
H041 H 1.078579 1.020034 0.258004 0.035 Uiso 1 1 calc R . . . .
C042 C 0.5134(3) 0.77522(15) 0.31245(13) 0.0312(5) Uani 1 1 d . . . . .
H04A H 0.487836 0.804133 0.366123 0.037 Uiso 1 1 calc R . . . .
H04B H 0.594767 0.716308 0.324453 0.037 Uiso 1 1 calc R . . . .
C043 C 0.2584(2) 0.64991(14) 0.20943(14) 0.0285(4) Uani 1 1 d . . . . .
H04C H 0.206422 0.617738 0.269469 0.034 Uiso 1 1 calc R . . . .
H04D H 0.307476 0.598935 0.175464 0.034 Uiso 1 1 calc R . . . .
C045 C 0.3523(3) 0.75049(16) 0.29085(14) 0.0320(5) Uani 1 1 d . . . . .
H04E H 0.292241 0.709423 0.343942 0.038 Uiso 1 1 calc R . . . .
H04F H 0.275579 0.810279 0.273847 0.038 Uiso 1 1 calc R . . . .
C046 C 0.0666(3) 0.80007(18) 0.01958(16) 0.0421(6) Uani 1 1 d . . . . .
H04G H -0.032453 0.828065 0.057429 0.051 Uiso 0.752(18) 1 calc R . P A 1
H04H H 0.025243 0.756155 -0.010835 0.051 Uiso 0.752(18) 1 calc R . P A 1
H04I H -0.002057 0.851266 0.048404 0.051 Uiso 0.248(18) 1 calc R . P A 2
H04J H -0.011594 0.756136 0.011665 0.051 Uiso 0.248(18) 1 calc R . P A 2
C049 C 0.8534(7) 1.1226(5) 0.0468(4) 0.0350(13) Uani 0.752(18) 1 d . . P A 1
H04K H 0.736854 1.147481 0.071687 0.042 Uiso 0.752(18) 1 calc R . P A 1
H04L H 0.843641 1.068994 0.017998 0.042 Uiso 0.752(18) 1 calc R . P A 1
C0 C 0.838(2) 1.1561(15) 0.0689(12) 0.040(4) Uani 0.248(18) 1 d . . P A 2
H0A H 0.789271 1.207103 0.102866 0.048 Uiso 0.248(18) 1 calc R . P A 2
H0B H 0.743548 1.123665 0.060070 0.048 Uiso 0.248(18) 1 calc R . P A 2
O047 O 0.7574(3) 1.06693(19) -0.43628(17) 0.0647(7) Uani 0.8 1 d . . P . .
N044 N 0.6280(3) 0.92945(17) -0.40245(15) 0.0367(5) Uani 0.8 1 d . . P . .
C048 C 0.7162(4) 0.9956(2) -0.4557(2) 0.0482(8) Uani 0.8 1 d . . P . .
H048 H 0.752041 0.987745 -0.515516 0.058 Uiso 0.8 1 calc R . P . .
C050 C 0.5881(4) 0.8483(2) -0.4330(2) 0.0503(8) Uani 0.8 1 d . . P . .
H05A H 0.463897 0.851222 -0.429251 0.076 Uiso 0.8 1 calc GR . P . .
H05B H 0.630888 0.788028 -0.395468 0.076 Uiso 0.8 1 calc GR . P . .
H05C H 0.642338 0.850765 -0.495057 0.076 Uiso 0.8 1 calc GR . P . .
C051 C 0.5764(5) 0.9301(3) -0.3079(2) 0.0556(9) Uani 0.8 1 d . . P . .
H05D H 0.642249 0.876649 -0.272616 0.083 Uiso 0.8 1 calc GR . P . .
H05E H 0.454224 0.922775 -0.291270 0.083 Uiso 0.8 1 calc GR . P . .
H05F H 0.597934 0.991481 -0.296218 0.083 Uiso 0.8 1 calc GR . P . .


_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
O002 C012 1.235(2) . ?
C0b C046 1.497(16) 2_675 ?
C049a C046 1.468(5) 2_675 ?
C049a H04K 0.9900 . ?
C049a H04L 0.9900 . ?
C0b H0A 0.9900 . ?
C0b H0B 0.9900 . ?
O003 C027 1.235(2) . ?
O004 H004 0.8400 . ?
O004 C012 1.310(2) . ?
O005 H005 0.8400 . ?
O005 C027 1.310(2) . ?
N006 H006 0.8800 . ?
N006 C011 1.371(2) . ?
N006 C024 1.385(2) . ?
N007 C011 1.322(2) . ?
N007 C021 1.385(2) . ?
C009 C015 1.395(3) . ?
C009 C020 1.483(2) . ?
C009 C022 1.396(2) . ?
C010 C022 1.398(2) . ?
C010 C027 1.487(2) . ?
C010 C029 1.382(3) . ?
C011 C030 1.471(2) . ?
C012 C019 1.486(3) . ?
C014 H014 0.9500 . ?
C014 C017 1.395(2) . ?
C014 C019 1.394(2) . ?
C015 H015 0.9500 . ?
C015 C034 1.392(3) . ?
C016 H016 0.9500 . ?
C016 C017 1.397(2) . ?
C016 C037 1.383(3) . ?
C017 C018 1.485(2) . ?
C018 C024 1.408(2) . ?
C018 C028 1.395(2) . ?
C019 C033 1.391(3) . ?
C020 C021 1.412(2) . ?
C020 C026 1.390(2) . ?
C021 C024 1.411(2) . ?
C022 H022 0.9500 . ?
C025 H025 0.9500 . ?
C025 C030 1.395(2) . ?
C025 C031 1.387(2) . ?
C026 H026 0.9500 . ?
C026 C028 1.396(2) . ?
C028 H028 0.9500 . ?
C029 H029 0.9500 . ?
C029 C034 1.394(3) . ?
C030 C031 1.401(2) 2_675 ?
C031 C030 1.401(2) 2_675 ?
C031 H031 0.9500 . ?
C033 H033 0.9500 . ?
C033 C037 1.388(3) . ?
C034 H034 0.9500 . ?
C037 H037 0.9500 . ?
O001 C043 1.429(2) . ?
O001 C045 1.430(2) . ?
O008 C038 1.413(2) . ?
O008 C046 1.416(3) . ?
O013 C040 1.372(2) . ?
O013 C042 1.426(2) . ?
O023 C032 1.373(2) . ?
O023 C049 1.431(5) . ?
O023 C0 1.424(14) . ?
C032 C036 1.384(3) . ?
C032 C041 1.396(3) . ?
C035 H035 0.9500 . ?
C035 C039 1.391(3) . ?
C035 C041 1.374(3) . ?
C036 H036 0.9500 . ?
C036 C040 1.391(3) . ?
C038 H03A 0.9900 . ?
C038 H03B 0.9900 . ?
C038 C043 1.509(3) . ?
C039 H039 0.9500 . ?
C039 C040 1.386(3) . ?
C041 H041 0.9500 . ?
C042 H04A 0.9900 . ?
C042 H04B 0.9900 . ?
C042 C045 1.497(3) . ?
C043 H04C 0.9900 . ?
C043 H04D 0.9900 . ?
C045 H04E 0.9900 . ?
C045 H04F 0.9900 . ?
C046 H04G 0.9900 . ?
C046 H04H 0.9900 . ?
C046 H04I 0.9900 . ?
C046 H04J 0.9900 . ?
C046 C049 1.468(5) 2_675 ?
C046 C0 1.497(16) 2_675 ?
O047 C048 1.232(4) . ?
N044 C048 1.308(4) . ?
N044 C050 1.445(4) . ?
N044 C051 1.457(4) . ?
C048 H048 0.9500 . ?
C050 H05A 0.9800 . ?
C050 H05B 0.9800 . ?
C050 H05C 0.9800 . ?
C051 H05D 0.9800 . ?
C051 H05E 0.9800 . ?
C051 H05F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C012 O004 H004 109.5 . . ?
H04Ka C049a H04L 108.2 . . ?
H0Ab C0b H0B 108.3 . . ?
C027 O005 H005 109.5 . . ?
C011 N006 H006 126.5 . . ?
C011 N006 C024 107.08(13) . . ?
C024 N006 H006 126.5 . . ?
C011 N007 C021 104.98(14) . . ?
C049a C046 H04G 109.9 2_675 . ?
H04Ga C046 H04H 108.3 . . ?
C049a C046 H04H 109.9 2_675 . ?
C0b C046 H04I 110.2 2_675 . ?
C0b C046 H04J 110.2 2_675 . ?
H04Ib C046 H04J 108.5 . . ?
C015 C009 C020 122.10(16) . . ?
C015 C009 C022 118.50(16) . . ?
C022 C009 C020 119.40(16) . . ?
C022 C010 C027 117.48(17) . . ?
C029 C010 C022 120.43(17) . . ?
C029 C010 C027 121.99(17) . . ?
N006 C011 C030 124.18(14) . . ?
N007 C011 N006 112.87(14) . . ?
N007 C011 C030 122.95(15) . . ?
O002 C012 O004 123.29(17) . . ?
O002 C012 C019 121.37(16) . . ?
O004 C012 C019 115.35(17) . . ?
C017 C014 H014 119.7 . . ?
C019 C014 H014 119.7 . . ?
C019 C014 C017 120.68(16) . . ?
C009 C015 H015 119.7 . . ?
C034 C015 C009 120.69(17) . . ?
C034 C015 H015 119.7 . . ?
C017 C016 H016 119.6 . . ?
C037 C016 H016 119.6 . . ?
C037 C016 C017 120.84(17) . . ?
C014 C017 C016 118.41(16) . . ?
C014 C017 C018 120.64(16) . . ?
C016 C017 C018 120.73(16) . . ?
C024 C018 C017 124.61(15) . . ?
C028 C018 C017 120.07(15) . . ?
C028 C018 C024 115.24(15) . . ?
C014 C019 C012 118.14(16) . . ?
C033 C019 C012 121.55(17) . . ?
C033 C019 C014 120.23(17) . . ?
C021 C020 C009 122.90(15) . . ?
C026 C020 C009 121.04(15) . . ?
C026 C020 C021 116.05(15) . . ?
N007 C021 C020 128.56(15) . . ?
N007 C021 C024 110.29(14) . . ?
C024 C021 C020 121.09(15) . . ?
C009 C022 C010 120.68(17) . . ?
C009 C022 H022 119.7 . . ?
C010 C022 H022 119.7 . . ?
N006 C024 C018 132.71(16) . . ?
N006 C024 C021 104.77(14) . . ?
C018 C024 C021 122.46(15) . . ?
C030 C025 H025 119.6 . . ?
C031 C025 H025 119.6 . . ?
C031 C025 C030 120.76(16) . . ?
C020 C026 H026 118.8 . . ?
C020 C026 C028 122.45(15) . . ?
C028 C026 H026 118.8 . . ?
O003 C027 O005 123.09(17) . . ?
O003 C027 C010 121.90(17) . . ?
O005 C027 C010 114.99(17) . . ?
C018 C028 C026 122.68(16) . . ?
C018 C028 H028 118.7 . . ?
C026 C028 H028 118.7 . . ?
C010 C029 H029 120.4 . . ?
C010 C029 C034 119.26(17) . . ?
C034 C029 H029 120.4 . . ?
C025 C030 C011 118.75(15) . . ?
C025 C030 C031 119.17(15) . 2_675 ?
C031 C030 C011 122.07(16) 2_675 . ?
C025 C031 C030 120.08(16) . 2_675 ?
C025 C031 H031 120.0 . . ?
C030 C031 H031 120.0 2_675 . ?
C019 C033 H033 120.4 . . ?
C037 C033 C019 119.21(17) . . ?
C037 C033 H033 120.4 . . ?
C015 C034 C029 120.42(18) . . ?
C015 C034 H034 119.8 . . ?
C029 C034 H034 119.8 . . ?
C016 C037 C033 120.62(18) . . ?
C016 C037 H037 119.7 . . ?
C033 C037 H037 119.7 . . ?
O023 C0b C046 108.6(10) . 2_675 ?
C043 O001 C045 113.66(14) . . ?
C038 O008 C046 113.96(16) . . ?
C040 O013 C042 117.56(16) . . ?
C032 O023 C049 116.4(2) . . ?
C032 O023 C0 121.8(7) . . ?
O023 C049a C046 109.8(3) . 2_675 ?
O023 C049a H04K 109.7 . . ?
O023 C049a H04L 109.7 . . ?
O023 C0b H0A 110.0 . . ?
O023 C0b H0B 110.0 . . ?
O023 C032 C036 123.85(18) . . ?
O023 C032 C041 115.66(17) . . ?
C036 C032 C041 120.48(19) . . ?
C039 C035 H035 119.2 . . ?
C041 C035 H035 119.2 . . ?
C041 C035 C039 121.60(19) . . ?
C032 C036 H036 120.4 . . ?
C032 C036 C040 119.28(19) . . ?
C040 C036 H036 120.4 . . ?
O008 C038 H03A 110.0 . . ?
O008 C038 H03B 110.0 . . ?
O008 C038 C043 108.57(15) . . ?
H03A C038 H03B 108.4 . . ?
C043 C038 H03A 110.0 . . ?
C043 C038 H03B 110.0 . . ?
C035 C039 H039 120.8 . . ?
C040 C039 C035 118.4(2) . . ?
C040 C039 H039 120.8 . . ?
O013 C040 C036 114.67(18) . . ?
O013 C040 C039 124.29(19) . . ?
C039 C040 C036 121.04(19) . . ?
C032 C041 H041 120.4 . . ?
C035 C041 C032 119.15(19) . . ?
C035 C041 H041 120.4 . . ?
O013 C042 H04A 110.2 . . ?
O013 C042 H04B 110.2 . . ?
O013 C042 C045 107.61(17) . . ?
H04A C042 H04B 108.5 . . ?
C045 C042 H04A 110.2 . . ?
C045 C042 H04B 110.2 . . ?
O001 C043 C038 114.09(16) . . ?
O001 C043 H04C 108.7 . . ?
O001 C043 H04D 108.7 . . ?
C038 C043 H04C 108.7 . . ?
C038 C043 H04D 108.7 . . ?
H04C C043 H04D 107.6 . . ?
O001 C045 C042 109.39(16) . . ?
O001 C045 H04E 109.8 . . ?
O001 C045 H04F 109.8 . . ?
C042 C045 H04E 109.8 . . ?
C042 C045 H04F 109.8 . . ?
H04E C045 H04F 108.2 . . ?
O008 C046 H04G 109.9 . . ?
O008 C046 H04H 109.9 . . ?
O008 C046 H04I 110.2 . . ?
O008 C046 H04J 110.2 . . ?
O008 C046 C049 108.8(2) . 2_675 ?
O008 C046 C0 107.6(6) . 2_675 ?
C046 C049a H04K 109.7 2_675 . ?
C046 C049a H04L 109.7 2_675 . ?
C048 N044 C050 121.6(3) . . ?
C046 C0b H0A 110.0 2_675 . ?
C048 N044 C051 121.6(3) . . ?
C050 N044 C051 116.7(3) . . ?
O047 C048 N044 126.7(3) . . ?
O047 C048 H048 116.7 . . ?
C046 C0b H0B 110.0 2_675 . ?
N044 C048 H048 116.7 . . ?
N044 C050 H05A 109.5 . . ?
N044 C050 H05B 109.5 . . ?
N044 C050 H05C 109.5 . . ?
H05A C050 H05B 109.5 . . ?
H05A C050 H05C 109.5 . . ?
H05B C050 H05C 109.5 . . ?
N044 C051 H05D 109.5 . . ?
N044 C051 H05E 109.5 . . ?
N044 C051 H05F 109.5 . . ?
H05D C051 H05E 109.5 . . ?
H05D C051 H05F 109.5 . . ?
H05E C051 H05F 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
O002 C012 C019 C014 -9.9(3) . . . . ?
O002 C012 C019 C033 167.13(18) . . . . ?
C038 O008 C046 C0b 171.8(10) . . . 2_675 ?
C038 O008 C046 C049a 145.7(4) . . . 2_675 ?
C032 O023 C0b C046 -154.7(8) . . . 2_675 ?
C0b O023 C032 C036 36.6(12) . . . . ?
C032 O023 C049a C046 -176.8(4) . . . 2_675 ?
C049a O023 C032 C036 7.7(5) . . . . ?
C049a O023 C032 C041 -173.2(4) . . . . ?
C0b O023 C032 C041 -144.3(12) . . . . ?
O004 C012 C019 C014 170.47(16) . . . . ?
O004 C012 C019 C033 -12.5(3) . . . . ?
N006 C011 C030 C025 161.34(16) . . . . ?
N006 C011 C030 C031 -19.9(3) . . . 2_675 ?
N007 C011 C030 C025 -17.8(2) . . . . ?
N007 C011 C030 C031 160.92(16) . . . 2_675 ?
N007 C021 C024 N006 -0.69(19) . . . . ?
N007 C021 C024 C018 176.85(15) . . . . ?
C009 C015 C034 C029 0.9(3) . . . . ?
C009 C020 C021 N007 3.5(3) . . . . ?
C009 C020 C021 C024 -179.49(16) . . . . ?
C009 C020 C026 C028 179.92(16) . . . . ?
C010 C029 C034 C015 0.5(3) . . . . ?
C011 N006 C024 C018 -176.25(18) . . . . ?
C011 N006 C024 C021 0.93(18) . . . . ?
C011 N007 C021 C020 177.43(16) . . . . ?
C011 N007 C021 C024 0.17(18) . . . . ?
C012 C019 C033 C037 -175.52(17) . . . . ?
C014 C017 C018 C024 -46.6(2) . . . . ?
C014 C017 C018 C028 129.78(18) . . . . ?
C014 C019 C033 C037 1.4(3) . . . . ?
C015 C009 C020 C021 41.6(2) . . . . ?
C015 C009 C020 C026 -139.58(18) . . . . ?
C015 C009 C022 C010 0.3(3) . . . . ?
C016 C017 C018 C024 138.90(18) . . . . ?
C016 C017 C018 C028 -44.7(2) . . . . ?
C017 C014 C019 C012 175.30(15) . . . . ?
C017 C014 C019 C033 -1.7(3) . . . . ?
C017 C016 C037 C033 -0.6(3) . . . . ?
C017 C018 C024 N006 -7.6(3) . . . . ?
C017 C018 C024 C021 175.67(16) . . . . ?
C017 C018 C028 C026 -175.36(16) . . . . ?
C019 C014 C017 C016 0.9(2) . . . . ?
C019 C014 C017 C018 -173.76(15) . . . . ?
C019 C033 C037 C016 -0.3(3) . . . . ?
C020 C009 C015 C034 178.60(17) . . . . ?
C020 C009 C022 C010 -179.60(16) . . . . ?
C020 C021 C024 N006 -178.20(14) . . . . ?
C020 C021 C024 C018 -0.7(3) . . . . ?
C020 C026 C028 C018 -0.3(3) . . . . ?
C021 N007 C011 N006 0.45(18) . . . . ?
C021 N007 C011 C030 179.72(15) . . . . ?
C021 C020 C026 C028 -1.2(2) . . . . ?
C022 C009 C015 C034 -1.3(3) . . . . ?
C022 C009 C020 C021 -138.46(17) . . . . ?
C022 C009 C020 C026 40.3(2) . . . . ?
C022 C010 C027 O003 1.0(3) . . . . ?
C022 C010 C027 O005 179.59(17) . . . . ?
C022 C010 C029 C034 -1.5(3) . . . . ?
C024 N006 C011 N007 -0.90(19) . . . . ?
C024 N006 C011 C030 179.84(15) . . . . ?
C024 C018 C028 C026 1.3(2) . . . . ?
C026 C020 C021 N007 -175.33(16) . . . . ?
C026 C020 C021 C024 1.7(2) . . . . ?
C027 C010 C022 C009 -175.27(16) . . . . ?
C027 C010 C029 C034 174.71(18) . . . . ?
C028 C018 C024 N006 175.90(17) . . . . ?
C028 C018 C024 C021 -0.9(2) . . . . ?
C029 C010 C022 C009 1.1(3) . . . . ?
C029 C010 C027 O003 -175.32(18) . . . . ?
C029 C010 C027 O005 3.3(3) . . . . ?
C030 C025 C031 C030 -0.1(3) . . . 2_675 ?
C031 C025 C030 C011 178.88(16) . . . . ?
C031 C025 C030 C031 0.1(3) . . . 2_675 ?
C037 C016 C017 C014 0.3(3) . . . . ?
C037 C016 C017 C018 174.90(17) . . . . ?
O008 C038 C043 O001 67.0(2) . . . . ?
O013 C042 C045 O001 65.6(2) . . . . ?
O023 C032 C036 C040 -179.61(18) . . . . ?
O023 C032 C041 C035 -179.49(17) . . . . ?
C032 C036 C040 O013 177.89(18) . . . . ?
C032 C036 C040 C039 -1.6(3) . . . . ?
C035 C039 C040 O013 -178.54(19) . . . . ?
C035 C039 C040 C036 0.9(3) . . . . ?
C036 C032 C041 C035 -0.4(3) . . . . ?
C039 C035 C041 C032 -0.3(3) . . . . ?
C040 O013 C042 C045 171.10(17) . . . . ?
C041 C032 C036 C040 1.3(3) . . . . ?
C041 C035 C039 C040 0.1(3) . . . . ?
C042 O013 C040 C036 -169.99(18) . . . . ?
C042 O013 C040 C039 9.5(3) . . . . ?
C043 O001 C045 C042 163.26(16) . . . . ?
C045 O001 C043 C038 79.4(2) . . . . ?
C046 O008 C038 C043 173.25(17) . . . . ?
C050 N044 C048 O047 -179.7(3) . . . . ?
C051 N044 C048 O047 -4.3(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
####################################################################### 
# 
# 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_Zn_6c
_database_code_depnum_ccdc_archive 'CCDC 1519350'
_audit_update_record             
;
2017-01-22 deposited with the CCDC.
2017-01-27 downloaded from the CCDC.
;
_audit_creation_date             2017-01-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/4
# start Validation Reply Form
_vrf_CHEMW03_Zn_6c               
; 
PROBLEM: ALERT: The ratio of given/expected molecular weight
RESPONSE: Masking of a DEF molecule but inclusion in the formula
;
_vrf_THETM01_Zn_6c               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: This was a weakly diffracting crystal and 
 no data was avaialbe at higher angles.
; # end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C164 H128 N12 O32 Zn4), 2(C5 H11 N O)'
_chemical_formula_sum            'C102 H108 N10 O20 Zn2'
_chemical_formula_weight         1924.72
_chemical_melting_point          ?
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'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   11.4221(4)
_cell_length_b                   21.2742(8)
_cell_length_c                   19.0647(7)
_cell_angle_alpha                90
_cell_angle_beta                 95.4192(19)
_cell_angle_gamma                90
_cell_volume                     4611.9(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9299
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      59.981
_cell_measurement_theta_min      3.120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  0.5818
_exptl_absorpt_correction_T_min  0.4908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1365 before and 0.1141 after correction.
The Ratio of minimum to maximum transmission is 0.8436.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24228
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        60.073
_diffrn_reflns_theta_max         60.073
_diffrn_reflns_theta_min         3.120
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5024
_reflns_number_total             6673
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         6673
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0683
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1120P)²+4.6528P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1957
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2S-C1S
 1.4 with sigma of 0.005
3. Restrained planarity
 N1S, C0AA, C1S, C3SA
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1S \\sim N1S \\sim C0AA \\sim C1S \\sim C2S \\sim C3SA \\sim C4SA \\sim C3SB
\\sim C4SB: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Same fragment restrains
{N1S, C0AA, C3SA, C4SA} sigma for 1-2: 0.02, 1-3: 0.02
{N1S, C0AA, C3SB, C4SB} sigma for 1-2: 0.02, 1-3: 0.02
as
{N1S, C0AA, C1S, C2S}
6. Others
 Sof(C3SB)=Sof(H3SC)=Sof(H3SD)=Sof(C4SB)=Sof(H4SD)=Sof(H4SE)=Sof(H4SF)=1-FVAR(1)
 Sof(C3SA)=Sof(H3SA)=Sof(H3SB)=Sof(C4SA)=Sof(H4SA)=Sof(H4SB)=Sof(H4SC)=FVAR(1)
7.a Riding coordinates:
 C4SA(H4SA,H4SB,H4SC)
7.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C1S(H1SA,H1SB), C3SA(H3SA,H3SB), C3SB(H3SC,H3SD)
7.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C19(H19), C23(H23), C24(H24), C26(H26), C28(H28), C30(H30),
  C38(H38), C39(H39), C40(H40), C41(H41), C0AA(H0AA)
7.d Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C4SB(H4SD,H4SE,H4SF)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn -0.38434(5) 0.98653(3) 1.08484(3) 0.0423(2) Uani 1 1 d . . . . .
O1 O -0.2256(3) 0.96465(15) 1.06814(15) 0.0533(8) Uani 1 1 d . . . . .
O2 O -0.2366(3) 0.90544(19) 1.16174(19) 0.0746(11) Uani 1 1 d . . . . .
O3 O 0.3972(3) 0.57302(14) 1.45043(17) 0.0587(9) Uani 1 1 d . . . . .
O4 O 0.5107(3) 0.58012(15) 1.54851(18) 0.0744(11) Uani 1 1 d . . . . .
O5 O -0.6452(2) 0.95399(13) 1.52815(15) 0.0479(7) Uani 1 1 d . . . . .
O6 O -0.7717(2) 0.85707(14) 1.58366(14) 0.0480(7) Uani 1 1 d . . . . .
O7 O -0.9895(3) 0.79453(15) 1.5916(2) 0.0722(11) Uani 1 1 d . . . . .
O8 O -0.7783(3) 1.15763(14) 1.45755(17) 0.0585(9) Uani 1 1 d . . . . .
N1 N 0.0952(3) 0.92197(14) 1.33609(15) 0.0316(7) Uani 1 1 d . . . . .
N2 N 0.1837(3) 0.87298(14) 1.43087(15) 0.0301(7) Uani 1 1 d . . . . .
H2 H 0.200875 0.862834 1.475399 0.036 Uiso 1 1 calc R . . . .
N3 N -0.4606(3) 1.00149(16) 1.17452(19) 0.0436(9) Uani 1 1 d . . . . .
C1 C -0.1800(4) 0.9283(2) 1.1163(2) 0.0470(11) Uani 1 1 d . . . . .
C2 C -0.0496(4) 0.91727(19) 1.1160(2) 0.0390(10) Uani 1 1 d . . . . .
C3 C 0.0136(4) 0.89488(17) 1.17787(19) 0.0358(9) Uani 1 1 d . . . . .
H3 H -0.027141 0.884887 1.217635 0.043 Uiso 1 1 calc R . . . .
C4 C 0.1350(3) 0.88717(17) 1.1815(2) 0.0332(9) Uani 1 1 d . . . . .
C5 C 0.1930(4) 0.9030(2) 1.1232(2) 0.0478(11) Uani 1 1 d . . . . .
H5 H 0.276146 0.899263 1.125395 0.057 Uiso 1 1 calc R . . . .
C6 C 0.1308(4) 0.9242(2) 1.0618(2) 0.0570(13) Uani 1 1 d . . . . .
H6 H 0.171176 0.933666 1.021722 0.068 Uiso 1 1 calc R . . . .
C7 C 0.0102(4) 0.9317(2) 1.0587(2) 0.0501(12) Uani 1 1 d . . . . .
H7 H -0.031679 0.946958 1.016759 0.060 Uiso 1 1 calc R . . . .
C8 C 0.1995(3) 0.86064(17) 1.24622(19) 0.0326(9) Uani 1 1 d . . . . .
C9 C 0.1733(3) 0.87653(16) 1.31432(19) 0.0299(9) Uani 1 1 d . . . . .
C10 C 0.2303(3) 0.84654(17) 1.37367(19) 0.0302(9) Uani 1 1 d . . . . .
C11 C 0.3161(3) 0.80002(17) 1.36915(19) 0.0318(9) Uani 1 1 d . . . . .
C12 C 0.3433(4) 0.78652(18) 1.3018(2) 0.0379(10) Uani 1 1 d . . . . .
H12 H 0.402395 0.756156 1.295545 0.045 Uiso 1 1 calc R . . . .
C13 C 0.2871(3) 0.81586(18) 1.2427(2) 0.0364(9) Uani 1 1 d . . . . .
H13 H 0.309745 0.804680 1.197700 0.044 Uiso 1 1 calc R . . . .
C14 C 0.3765(3) 0.76873(17) 1.43277(19) 0.0309(9) Uani 1 1 d . . . . .
C15 C 0.4312(3) 0.80325(18) 1.4877(2) 0.0388(10) Uani 1 1 d . . . . .
H15 H 0.428806 0.847851 1.485517 0.047 Uiso 1 1 calc R . . . .
C16 C 0.4898(4) 0.77399(19) 1.5462(2) 0.0420(10) Uani 1 1 d . . . . .
H16 H 0.524739 0.798590 1.584125 0.050 Uiso 1 1 calc R . . . .
C17 C 0.4971(3) 0.70959(19) 1.5490(2) 0.0375(10) Uani 1 1 d . . . . .
H17 H 0.540257 0.689604 1.587826 0.045 Uiso 1 1 calc R . . . .
C18 C 0.4413(3) 0.67389(17) 1.49493(19) 0.0296(9) Uani 1 1 d . . . . .
C19 C 0.3816(3) 0.70335(18) 1.43736(19) 0.0309(9) Uani 1 1 d . . . . .
H19 H 0.343467 0.678620 1.400482 0.037 Uiso 1 1 calc R . . . .
C20 C 0.4516(3) 0.60357(18) 1.4978(2) 0.0333(9) Uani 1 1 d . . . . .
C21 C 0.1061(3) 0.91767(17) 1.40543(19) 0.0305(9) Uani 1 1 d . . . . .
C22 C 0.0478(3) 0.95917(18) 1.45294(18) 0.0304(9) Uani 1 1 d . . . . .
C23 C 0.0304(3) 1.02203(17) 1.4358(2) 0.0327(9) Uani 1 1 d . . . . .
H23 H 0.050903 1.037260 1.391709 0.039 Uiso 1 1 calc R . . . .
C24 C 0.0166(3) 0.93733(18) 1.5178(2) 0.0344(9) Uani 1 1 d . . . . .
H24 H 0.027689 0.894311 1.530039 0.041 Uiso 1 1 calc R . . . .
C25 C -0.7194(4) 1.1045(2) 1.4406(3) 0.0475(11) Uani 1 1 d . . . . .
C26 C -0.6773(4) 1.0936(2) 1.3765(2) 0.0479(11) Uani 1 1 d . . . . .
H26 H -0.684380 1.124772 1.340635 0.057 Uiso 1 1 calc R . . . .
C27 C -0.6231(4) 1.0352(2) 1.3647(2) 0.0451(11) Uani 1 1 d . . . . .
C28 C -0.6135(3) 0.9904(2) 1.4166(2) 0.0425(11) Uani 1 1 d . . . . .
H28 H -0.577428 0.951236 1.408347 0.051 Uiso 1 1 calc R . . . .
C29 C -0.6564(4) 1.0021(2) 1.4814(2) 0.0416(11) Uani 1 1 d . . . . .
C30 C -0.7068(4) 1.0593(2) 1.4943(2) 0.0468(11) Uani 1 1 d . . . . .
H30 H -0.732791 1.068009 1.539217 0.056 Uiso 1 1 calc R . . . .
C31 C -0.6945(4) 0.9602(2) 1.5934(2) 0.0506(12) Uani 1 1 d . . . . .
H31A H -0.776107 0.976081 1.585670 0.061 Uiso 1 1 calc R . . . .
H31B H -0.647561 0.989900 1.624507 0.061 Uiso 1 1 calc R . . . .
C32 C -0.6928(4) 0.8964(2) 1.6258(2) 0.0565(13) Uani 1 1 d . . . . .
H32A H -0.612301 0.878714 1.628414 0.068 Uiso 1 1 calc R . . . .
H32B H -0.717055 0.898996 1.674212 0.068 Uiso 1 1 calc R . . . .
C33 C -0.7837(4) 0.7971(2) 1.6143(3) 0.0610(14) Uani 1 1 d . . . . .
H33A H -0.796893 0.801855 1.664604 0.073 Uiso 1 1 calc R . . . .
H33B H -0.710522 0.772629 1.611523 0.073 Uiso 1 1 calc R . . . .
C34 C -0.8842(5) 0.7633(2) 1.5765(3) 0.0689(16) Uani 1 1 d . . . . .
H34A H -0.877194 0.763618 1.525179 0.083 Uiso 1 1 calc R . . . .
H34B H -0.885462 0.719018 1.592536 0.083 Uiso 1 1 calc R . . . .
C35 C -1.0923(5) 0.7588(2) 1.5758(3) 0.0721(16) Uani 1 1 d . . . . .
H35A H -1.086826 0.718805 1.602427 0.086 Uiso 1 1 calc R . . . .
H35B H -1.102655 0.749003 1.524884 0.086 Uiso 1 1 calc R . . . .
C36 C -0.8064(4) 1.2034(2) 1.4039(3) 0.0676(15) Uani 1 1 d . . . . .
H36A H -0.827269 1.182413 1.358098 0.081 Uiso 1 1 calc R . . . .
H36B H -0.737826 1.231056 1.399285 0.081 Uiso 1 1 calc R . . . .
C37 C -0.5725(4) 1.02388(19) 1.2974(2) 0.0443(11) Uani 1 1 d . . . . .
C38 C -0.5384(4) 1.0725(2) 1.2552(2) 0.0483(11) Uani 1 1 d . . . . .
H38 H -0.553731 1.114780 1.267452 0.058 Uiso 1 1 calc R . . . .
C39 C -0.4833(4) 1.0602(2) 1.1965(2) 0.0489(11) Uani 1 1 d . . . . .
H39 H -0.459521 1.094724 1.169617 0.059 Uiso 1 1 calc R . . . .
C40 C -0.4958(4) 0.9545(2) 1.2135(2) 0.0486(11) Uani 1 1 d . . . . .
H40 H -0.481258 0.912692 1.198954 0.058 Uiso 1 1 calc R . . . .
C41 C -0.5515(4) 0.9627(2) 1.2730(3) 0.0508(12) Uani 1 1 d . . . . .
H41 H -0.576200 0.927256 1.298001 0.061 Uiso 1 1 calc R . . . .
O1S O -0.6093(5) 1.2773(2) 1.7747(2) 0.1016(14) Uani 1 1 d . U . . .
N1S N -0.7028(7) 1.2277(4) 1.6830(3) 0.148(3) Uani 1 1 d D U . . .
C0AA C -0.6674(9) 1.2347(3) 1.7493(4) 0.124(3) Uani 1 1 d D U . . .
H0AA H -0.689664 1.203098 1.780626 0.149 Uiso 1 1 calc R . . . .
C1S C -0.6642(9) 1.2719(6) 1.6289(5) 0.193(6) Uani 1 1 d D U . . .
H1SA H -0.585376 1.287960 1.646094 0.232 Uiso 1 1 calc R . . . .
H1SB H -0.655164 1.247385 1.585550 0.232 Uiso 1 1 calc R . . . .
C2S C -0.7361(10) 1.3235(7) 1.6102(9) 0.291(11) Uani 1 1 d D U . . .
H2SA H -0.742232 1.350114 1.651691 0.437 Uiso 1 1 calc GR . . . .
H2SB H -0.814576 1.308811 1.592278 0.437 Uiso 1 1 calc GR . . . .
H2SC H -0.701930 1.347911 1.573583 0.437 Uiso 1 1 calc GR . . . .
C3SA C -0.8059(14) 1.1865(9) 1.6573(11) 0.155(8) Uani 0.517(16) 1 d D U P A 1
H3SA H -0.782370 1.162877 1.616188 0.185 Uiso 0.517(16) 1 calc R . P A 1
H3SB H -0.815157 1.155202 1.694858 0.185 Uiso 0.517(16) 1 calc R . P A 1
C4SA C -0.9117(16) 1.2101(13) 1.6388(17) 0.34(2) Uani 0.517(16) 1 d D U P A 1
H4SA H -0.935433 1.238175 1.675677 0.513 Uiso 0.517(16) 1 d R . P A 1
H4SB H -0.968723 1.175715 1.631417 0.513 Uiso 0.517(16) 1 d R . P A 1
H4SC H -0.909003 1.233695 1.594877 0.513 Uiso 0.517(16) 1 d R . P A 1
C3SB C -0.7132(18) 1.1606(9) 1.6570(10) 0.170(9) Uani 0.483(16) 1 d D U P A 2
H3SC H -0.703579 1.162576 1.605954 0.204 Uiso 0.483(16) 1 calc R . P A 2
H3SD H -0.642846 1.138633 1.679150 0.204 Uiso 0.483(16) 1 calc R . P A 2
C4SB C -0.803(2) 1.1219(13) 1.6631(12) 0.278(17) Uani 0.483(16) 1 d D U P A 2
H4SD H -0.779727 1.089918 1.698745 0.417 Uiso 0.483(16) 1 calc GR . P A 2
H4SE H -0.824612 1.101376 1.617681 0.417 Uiso 0.483(16) 1 calc GR . P A 2
H4SF H -0.870026 1.145722 1.677271 0.417 Uiso 0.483(16) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.928(3) . ?
Zn1 O3 1.960(3) 2_557 ?
Zn1 O4 1.942(3) 4_475 ?
Zn1 N3 2.016(4) . ?
C3SAa H3SA 0.9900 . ?
C3SAa H3SB 0.9900 . ?
C3SAa C4SA 1.326(18) . ?
C4SAa H4SA 0.9799 . ?
C4SAa H4SB 0.9802 . ?
C4SAa H4SC 0.9800 . ?
C3SBb H3SC 0.9900 . ?
C3SBb H3SD 0.9900 . ?
C3SBb C4SB 1.327(16) . ?
C4SBb H4SD 0.9800 . ?
C4SBb H4SE 0.9800 . ?
C4SBb H4SF 0.9800 . ?
O1 C1 1.273(5) . ?
O2 C1 1.229(5) . ?
O3 Zn1 1.960(3) 2_547 ?
O3 C20 1.232(5) . ?
O4 Zn1 1.942(3) 4_676 ?
O4 C20 1.231(5) . ?
O5 C29 1.356(5) . ?
O5 C31 1.418(5) . ?
O6 C32 1.421(5) . ?
O6 C33 1.415(5) . ?
O7 C34 1.426(6) . ?
O7 C35 1.407(6) . ?
O8 C25 1.370(5) . ?
O8 C36 1.426(6) . ?
N1 C9 1.405(5) . ?
N1 C21 1.319(5) . ?
N2 H2 0.8800 . ?
N2 C10 1.378(5) . ?
N2 C21 1.357(5) . ?
N3 C39 1.351(5) . ?
N3 C40 1.330(6) . ?
C1 C2 1.508(6) . ?
C2 C3 1.406(5) . ?
C2 C7 1.377(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.392(5) . ?
C4 C5 1.388(6) . ?
C4 C8 1.486(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.386(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.382(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.401(5) . ?
C8 C13 1.388(5) . ?
C9 C10 1.404(5) . ?
C10 C11 1.401(5) . ?
C11 C12 1.380(5) . ?
C11 C14 1.494(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.390(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.379(5) . ?
C14 C19 1.395(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.392(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.373(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.386(5) . ?
C18 C19 1.386(5) . ?
C18 C20 1.501(5) . ?
C19 H19 0.9500 . ?
C21 C22 1.469(5) . ?
C22 C23 1.387(5) . ?
C22 C24 1.399(5) . ?
C23 H23 0.9500 . ?
C23 C24 1.381(5) 3_578 ?
C24 C23 1.381(5) 3_578 ?
C24 H24 0.9500 . ?
C25 C26 1.375(6) . ?
C25 C30 1.403(6) . ?
C26 H26 0.9500 . ?
C26 C27 1.416(6) . ?
C27 C28 1.370(6) . ?
C27 C37 1.476(6) . ?
C28 H28 0.9500 . ?
C28 C29 1.394(6) . ?
C29 C30 1.378(6) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.491(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.484(7) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.489(7) 3_378 ?
C36 C35 1.489(7) 3_378 ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.388(6) . ?
C37 C41 1.410(6) . ?
C38 H38 0.9500 . ?
C38 C39 1.360(6) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C40 C41 1.364(6) . ?
C41 H41 0.9500 . ?
O1S C0AA 1.198(8) . ?
N1S C0AA 1.299(9) . ?
N1S C1S 1.492(10) . ?
N1S C3SA 1.512(15) . ?
N1S C3SB 1.513(14) . ?
C0AA H0AA 0.9500 . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C1S C2S 1.398(5) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4SAa C3SAa N1S 122.0(16) . . ?
O1 Zn1 O3 102.19(14) . 2_557 ?
O1 Zn1 O4 108.88(16) . 4_475 ?
O1 Zn1 N3 131.82(13) . . ?
O3 Zn1 N3 96.81(14) 2_557 . ?
O4 Zn1 O3 122.65(13) 4_475 2_557 ?
C4SBb C3SBb N1S 126.5(16) . . ?
C4SAa C3SAa H3SA 106.8 . . ?
C4SAa C3SAa H3SB 106.8 . . ?
O4 Zn1 N3 96.66(16) 4_475 . ?
H3SAa C3SAa H3SB 106.7 . . ?
C3SAa C4SAa H4SA 110.3 . . ?
C3SAa C4SAa H4SB 109.4 . . ?
C1 O1 Zn1 110.8(3) . . ?
C20 O3 Zn1 139.7(3) . 2_547 ?
C20 O4 Zn1 148.2(3) . 4_676 ?
H4SAa C4SAa H4SB 109.5 . . ?
H4SAa C4SAa H4SC 109.5 . . ?
C3SAa C4SAa H4SC 108.7 . . ?
C29 O5 C31 119.1(3) . . ?
C33 O6 C32 112.2(3) . . ?
C35 O7 C34 114.0(4) . . ?
H4SBa C4SAa H4SC 109.5 . . ?
C4SBb C3SBb H3SC 105.7 . . ?
C4SBb C3SBb H3SD 105.7 . . ?
C25 O8 C36 118.4(4) . . ?
C21 N1 C9 104.2(3) . . ?
C10 N2 H2 126.5 . . ?
C21 N2 H2 126.5 . . ?
C21 N2 C10 106.9(3) . . ?
C39 N3 Zn1 121.4(3) . . ?
C40 N3 Zn1 122.1(3) . . ?
C40 N3 C39 116.4(4) . . ?
O1 C1 C2 115.4(4) . . ?
H3SCb C3SBb H3SD 106.1 . . ?
C3SBb C4SBb H4SD 109.5 . . ?
C3SBb C4SBb H4SE 109.5 . . ?
H4SDb C4SBb H4SE 109.5 . . ?
H4SEb C4SBb H4SF 109.5 . . ?
H4SDb C4SBb H4SF 109.5 . . ?
C3SBb C4SBb H4SF 109.5 . . ?
O2 C1 O1 122.8(4) . . ?
O2 C1 C2 121.7(4) . . ?
C3 C2 C1 118.6(4) . . ?
C7 C2 C1 122.2(4) . . ?
C7 C2 C3 119.1(4) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.8(4) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C8 120.0(3) . . ?
C5 C4 C3 118.7(4) . . ?
C5 C4 C8 121.4(4) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.7(4) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.1(4) . . ?
C7 C6 H6 119.9 . . ?
C2 C7 C6 120.6(4) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C9 C8 C4 123.0(3) . . ?
C13 C8 C4 121.6(3) . . ?
C13 C8 C9 115.3(3) . . ?
C8 C9 N1 129.6(3) . . ?
C8 C9 C10 121.0(3) . . ?
C10 C9 N1 109.5(3) . . ?
N2 C10 C9 105.6(3) . . ?
N2 C10 C11 131.4(3) . . ?
C11 C10 C9 123.0(3) . . ?
C10 C11 C14 122.5(3) . . ?
C12 C11 C10 115.1(3) . . ?
C12 C11 C14 122.4(3) . . ?
C11 C12 H12 118.9 . . ?
C11 C12 C13 122.2(4) . . ?
C13 C12 H12 118.9 . . ?
C8 C13 C12 123.3(4) . . ?
C8 C13 H13 118.3 . . ?
C12 C13 H13 118.3 . . ?
C15 C14 C11 121.3(3) . . ?
C15 C14 C19 118.1(3) . . ?
C19 C14 C11 120.6(3) . . ?
C14 C15 H15 119.4 . . ?
C14 C15 C16 121.3(4) . . ?
C16 C15 H15 119.4 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 C15 120.0(4) . . ?
C17 C16 H16 120.0 . . ?
C16 C17 H17 120.2 . . ?
C16 C17 C18 119.7(4) . . ?
C18 C17 H17 120.2 . . ?
C17 C18 C19 119.9(3) . . ?
C17 C18 C20 119.3(3) . . ?
C19 C18 C20 120.7(3) . . ?
C14 C19 H19 119.5 . . ?
C18 C19 C14 121.0(3) . . ?
C18 C19 H19 119.5 . . ?
O3 C20 C18 117.8(3) . . ?
O4 C20 O3 124.3(4) . . ?
O4 C20 C18 117.9(4) . . ?
N1 C21 N2 113.8(3) . . ?
N1 C21 C22 124.8(3) . . ?
N2 C21 C22 121.3(3) . . ?
C23 C22 C21 119.8(3) . . ?
C23 C22 C24 119.1(3) . . ?
C24 C22 C21 120.9(3) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 C22 120.5(3) 3_578 . ?
C24 C23 H23 119.7 3_578 . ?
C22 C24 H24 119.8 . . ?
C23 C24 C22 120.4(3) 3_578 . ?
C23 C24 H24 119.8 3_578 . ?
O8 C25 C26 124.8(4) . . ?
O8 C25 C30 114.3(4) . . ?
C26 C25 C30 120.9(4) . . ?
C25 C26 H26 120.5 . . ?
C25 C26 C27 119.0(4) . . ?
C27 C26 H26 120.5 . . ?
C26 C27 C37 119.6(4) . . ?
C28 C27 C26 120.1(4) . . ?
C28 C27 C37 120.3(4) . . ?
C27 C28 H28 119.8 . . ?
C27 C28 C29 120.4(4) . . ?
C29 C28 H28 119.8 . . ?
O5 C29 C28 115.4(4) . . ?
O5 C29 C30 124.3(4) . . ?
C30 C29 C28 120.3(4) . . ?
C25 C30 H30 120.3 . . ?
C29 C30 C25 119.3(4) . . ?
C29 C30 H30 120.3 . . ?
O5 C31 H31A 110.4 . . ?
O5 C31 H31B 110.4 . . ?
O5 C31 C32 106.8(4) . . ?
H31A C31 H31B 108.6 . . ?
C32 C31 H31A 110.4 . . ?
C32 C31 H31B 110.4 . . ?
O6 C32 C31 108.6(3) . . ?
O6 C32 H32A 110.0 . . ?
O6 C32 H32B 110.0 . . ?
C31 C32 H32A 110.0 . . ?
C31 C32 H32B 110.0 . . ?
H32A C32 H32B 108.4 . . ?
O6 C33 H33A 109.7 . . ?
O6 C33 H33B 109.7 . . ?
O6 C33 C34 109.7(4) . . ?
H33A C33 H33B 108.2 . . ?
C34 C33 H33A 109.7 . . ?
C34 C33 H33B 109.7 . . ?
O7 C34 C33 107.7(4) . . ?
O7 C34 H34A 110.2 . . ?
O7 C34 H34B 110.2 . . ?
C33 C34 H34A 110.2 . . ?
C33 C34 H34B 110.2 . . ?
H34A C34 H34B 108.5 . . ?
O7 C35 H35A 110.1 . . ?
O7 C35 H35B 110.1 . . ?
O7 C35 C36 107.9(4) . 3_378 ?
H35A C35 H35B 108.4 . . ?
C36 C35 H35A 110.1 3_378 . ?
C36 C35 H35B 110.1 3_378 . ?
O8 C36 C35 108.1(4) . 3_378 ?
O8 C36 H36A 110.1 . . ?
O8 C36 H36B 110.1 . . ?
C35 C36 H36A 110.1 3_378 . ?
C35 C36 H36B 110.1 3_378 . ?
H36A C36 H36B 108.4 . . ?
C38 C37 C27 122.5(4) . . ?
C38 C37 C41 115.5(4) . . ?
C41 C37 C27 122.0(4) . . ?
C37 C38 H38 119.7 . . ?
C39 C38 C37 120.7(4) . . ?
C39 C38 H38 119.7 . . ?
N3 C39 C38 123.4(4) . . ?
N3 C39 H39 118.3 . . ?
C38 C39 H39 118.3 . . ?
N3 C40 H40 118.1 . . ?
N3 C40 C41 123.8(4) . . ?
C41 C40 H40 118.1 . . ?
C37 C41 H41 120.0 . . ?
C40 C41 C37 120.1(4) . . ?
C40 C41 H41 120.0 . . ?
N1S C3SAa H3SA 106.8 . . ?
N1S C3SAa H3SB 106.8 . . ?
N1S C3SBb H3SC 105.7 . . ?
N1S C3SBb H3SD 105.7 . . ?
C0AA N1S C1S 121.1(7) . . ?
C0AA N1S C3SA 122.9(10) . . ?
C0AA N1S C3SB 115.8(10) . . ?
C1S N1S C3SA 114.4(11) . . ?
C1S N1S C3SB 112.7(10) . . ?
O1S C0AA N1S 126.1(7) . . ?
O1S C0AA H0AA 117.0 . . ?
N1S C0AA H0AA 117.0 . . ?
N1S C1S H1SA 107.9 . . ?
N1S C1S H1SB 107.9 . . ?
H1SA C1S H1SB 107.2 . . ?
C2S C1S N1S 117.8(9) . . ?
C2S C1S H1SA 107.9 . . ?
C2S C1S H1SB 107.9 . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 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
Zn1 O1 C1 O2 7.8(6) . . . . ?
Zn1 O1 C1 C2 -169.6(3) . . . . ?
Zn1 O3 C20 O4 -11.8(7) 2_547 . . . ?
Zn1 O3 C20 C18 170.6(3) 2_547 . . . ?
Zn1 O4 C20 O3 36.2(9) 4_676 . . . ?
Zn1 O4 C20 C18 -146.1(5) 4_676 . . . ?
Zn1 N3 C39 C38 177.5(3) . . . . ?
Zn1 N3 C40 C41 -177.5(3) . . . . ?
O1 C1 C2 C3 160.5(4) . . . . ?
O1 C1 C2 C7 -15.7(6) . . . . ?
O2 C1 C2 C3 -17.0(6) . . . . ?
O2 C1 C2 C7 166.8(5) . . . . ?
O5 C29 C30 C25 -176.5(4) . . . . ?
O5 C31 C32 O6 -66.7(4) . . . . ?
O6 C33 C34 O7 -68.8(5) . . . . ?
O8 C25 C26 C27 -176.8(4) . . . . ?
O8 C25 C30 C29 175.4(4) . . . . ?
N1 C9 C10 N2 1.6(4) . . . . ?
N1 C9 C10 C11 -178.2(3) . . . . ?
N1 C21 C22 C23 -34.8(6) . . . . ?
N1 C21 C22 C24 149.7(4) . . . . ?
N2 C10 C11 C12 -178.2(4) . . . . ?
N2 C10 C11 C14 0.0(6) . . . . ?
N2 C21 C22 C23 141.0(4) . . . . ?
N2 C21 C22 C24 -34.6(5) . . . . ?
N3 C40 C41 C37 -1.5(7) . . . . ?
C1 C2 C3 C4 -176.5(4) . . . . ?
C1 C2 C7 C6 176.3(4) . . . . ?
C2 C3 C4 C5 1.0(6) . . . . ?
C2 C3 C4 C8 -177.2(4) . . . . ?
C3 C2 C7 C6 0.1(7) . . . . ?
C3 C4 C5 C6 -2.0(6) . . . . ?
C3 C4 C8 C9 -40.4(5) . . . . ?
C3 C4 C8 C13 136.6(4) . . . . ?
C4 C5 C6 C7 2.0(7) . . . . ?
C4 C8 C9 N1 -6.7(6) . . . . ?
C4 C8 C9 C10 174.9(3) . . . . ?
C4 C8 C13 C12 -175.1(4) . . . . ?
C5 C4 C8 C9 141.4(4) . . . . ?
C5 C4 C8 C13 -41.5(6) . . . . ?
C5 C6 C7 C2 -1.1(8) . . . . ?
C7 C2 C3 C4 -0.1(6) . . . . ?
C8 C4 C5 C6 176.2(4) . . . . ?
C8 C9 C10 N2 -179.7(3) . . . . ?
C8 C9 C10 C11 0.5(6) . . . . ?
C9 N1 C21 N2 -0.6(4) . . . . ?
C9 N1 C21 C22 175.4(3) . . . . ?
C9 C8 C13 C12 2.2(6) . . . . ?
C9 C10 C11 C12 1.5(6) . . . . ?
C9 C10 C11 C14 179.6(3) . . . . ?
C10 N2 C21 N1 1.6(4) . . . . ?
C10 N2 C21 C22 -174.5(3) . . . . ?
C10 C11 C12 C13 -1.7(6) . . . . ?
C10 C11 C14 C15 -53.1(5) . . . . ?
C10 C11 C14 C19 128.5(4) . . . . ?
C11 C12 C13 C8 -0.2(6) . . . . ?
C11 C14 C15 C16 -178.5(4) . . . . ?
C11 C14 C19 C18 177.5(3) . . . . ?
C12 C11 C14 C15 124.9(4) . . . . ?
C12 C11 C14 C19 -53.4(5) . . . . ?
C13 C8 C9 N1 176.1(4) . . . . ?
C13 C8 C9 C10 -2.3(5) . . . . ?
C14 C11 C12 C13 -179.8(4) . . . . ?
C14 C15 C16 C17 2.0(6) . . . . ?
C15 C14 C19 C18 -1.0(5) . . . . ?
C15 C16 C17 C18 -3.0(6) . . . . ?
C16 C17 C18 C19 2.0(6) . . . . ?
C16 C17 C18 C20 178.9(4) . . . . ?
C17 C18 C19 C14 0.0(5) . . . . ?
C17 C18 C20 O3 177.2(4) . . . . ?
C17 C18 C20 O4 -0.6(6) . . . . ?
C19 C14 C15 C16 0.0(6) . . . . ?
C19 C18 C20 O3 -5.9(5) . . . . ?
C19 C18 C20 O4 176.4(4) . . . . ?
C20 C18 C19 C14 -176.9(3) . . . . ?
C21 N1 C9 C8 -179.2(4) . . . . ?
C21 N1 C9 C10 -0.6(4) . . . . ?
C21 N2 C10 C9 -1.9(4) . . . . ?
C21 N2 C10 C11 177.8(4) . . . . ?
C21 C22 C23 C24 -175.3(3) . . . 3_578 ?
C21 C22 C24 C23 175.2(3) . . . 3_578 ?
C23 C22 C24 C23 -0.3(6) . . . 3_578 ?
C24 C22 C23 C24 0.3(6) . . . 3_578 ?
C25 O8 C36 C35 157.0(4) . . . 3_378 ?
C25 C26 C27 C28 0.2(6) . . . . ?
C25 C26 C27 C37 -177.1(4) . . . . ?
C26 C25 C30 C29 -3.0(6) . . . . ?
C26 C27 C28 C29 -0.3(6) . . . . ?
C26 C27 C37 C38 22.8(6) . . . . ?
C26 C27 C37 C41 -159.6(4) . . . . ?
C27 C28 C29 O5 178.2(4) . . . . ?
C27 C28 C29 C30 -1.2(6) . . . . ?
C27 C37 C38 C39 174.6(4) . . . . ?
C27 C37 C41 C40 -174.6(4) . . . . ?
C28 C27 C37 C38 -154.5(4) . . . . ?
C28 C27 C37 C41 23.1(6) . . . . ?
C28 C29 C30 C25 2.9(6) . . . . ?
C29 O5 C31 C32 167.5(4) . . . . ?
C30 C25 C26 C27 1.5(6) . . . . ?
C31 O5 C29 C28 -175.3(3) . . . . ?
C31 O5 C29 C30 4.2(6) . . . . ?
C32 O6 C33 C34 168.2(4) . . . . ?
C33 O6 C32 C31 -174.5(4) . . . . ?
C34 O7 C35 C36 178.5(4) . . . 3_378 ?
C35 O7 C34 C33 -163.5(4) . . . . ?
C36 O8 C25 C26 4.9(6) . . . . ?
C36 O8 C25 C30 -173.5(4) . . . . ?
C37 C27 C28 C29 177.0(4) . . . . ?
C37 C38 C39 N3 1.5(7) . . . . ?
C38 C37 C41 C40 3.1(6) . . . . ?
C39 N3 C40 C41 -0.3(6) . . . . ?
C3SAa N1S C0AA O1S -159.3(11) . . . . ?
C3SBb N1S C0AA O1S 147.5(12) . . . . ?
C3SBb N1S C1S C2S 123.7(14) . . . . ?
C3SAa N1S C1S C2S 72.7(14) . . . . ?
C40 N3 C39 C38 0.3(6) . . . . ?
C41 C37 C38 C39 -3.2(6) . . . . ?
C0AA N1S C3SBb C4SBb 82(3) . . . . ?
C0AA N1S C3SAa C4SAa 100(3) . . . . ?
C0AA N1S C1S C2S -92.9(14) . . . . ?
C1S N1S C3SAa C4SAa -66(3) . . . . ?
C1S N1S C3SBb C4SBb -133(2) . . . . ?
C1S N1S C0AA O1S 5.2(15) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.009 0.098 0.185 200.5 49.3 C5H11NO
2 0.009 -0.098 0.815 200.5 49.5 C5H11NO
3 -0.009 0.402 0.685 200.5 49.3 C5H11NO
4 0.009 0.598 0.315 200.5 49.4 C5H11NO


_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'solvothermal DEF'
####################################################################### 
# 
# 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_Zn_6a
_database_code_depnum_ccdc_archive 'CCDC 1519349'
_audit_update_record             
;
2017-01-22 deposited with the CCDC.
2017-01-27 downloaded from the CCDC.
;
_audit_creation_date             2017-01-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/4
# start Validation Reply Form
_vrf_PLAT701_Zn_6a               
;
PROBLEM: Bond Calc 0.936(12), Rep 1.227(8), Dev.. 24.25 Sigma
RESPONSE: This is due to the disorder in the DEF molecule.
;
_vrf_PLAT702_Zn_6a               
;
PROBLEM: Angle Calc 96.4(7), Rep 127.6(5), Dev.. 44.57 Sigma
RESPONSE: This is due to the disorder in the DEF molecule.
;
_vrf_PLAT703_Zn_6a               
;
PROBLEM: Torsion Calc 112.9(18), Rep 123.5(11), Dev.. 5.89 Sigma
RESPONSE: This is due to the disorder in the DEF molecule.
;
_vrf_PLAT420_Zn_6a               
;
PROBLEM: D-H Without Acceptor O2W -- H2WA ... Please Check
RESPONSE: O2W is a metal bonded water and this is not unusual.
;
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C48 H30 N4 O10 Zn2, C24 H32 O8, 2(C5 H11 N O), 2(H2 O)'
_chemical_formula_sum            'C82 H88 N6 O22 Zn2'
_chemical_formula_weight         1640.32
_chemical_melting_point          ?
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2465(4)
_cell_length_b                   14.4619(6)
_cell_length_c                   16.5490(8)
_cell_angle_alpha                97.0926(17)
_cell_angle_beta                 94.778(2)
_cell_angle_gamma                102.6227(18)
_cell_volume                     1898.76(15)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      31.631
_cell_measurement_theta_min      2.942
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.7077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0488 before and 0.0397 after correction.
The Ratio of minimum to maximum transmission is 0.9483.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30083
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.398
_diffrn_reflns_theta_min         2.875
_diffrn_ambient_temperature      130.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6374
_reflns_number_total             7692
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         7692
_refine_ls_number_restraints     156
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0403
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0402P)²+3.0172P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1027
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O9 \\sim C40 \\sim N3 \\sim C36 \\sim C38 \\sim C40A \\sim C36A \\sim C38A
\\sim C37 \\sim C39 \\sim O9A \\sim C37A \\sim C39A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
3. Same fragment restrains
{O9A, C40A, N3, C36A, C37A, C38A, C39A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O9, C40, N3, C36, C37, C38, C39}
4. Others
 Sof(O9A)=Sof(C40A)=Sof(H40A)=Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C37A)=
 Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=
 Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(1)
 Sof(O9)=Sof(C40)=Sof(H40)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=
 Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=FVAR(1)
5.a Free rotating group:
 O1W(H1WA,H1WB)
5.b Rotating group:
 O2W(H2WA,H2WB)
5.c Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C49(H49A,H49B), C36(H36A,H36B), C38(H38A,H38B), C36A(H36C,H36D),
 C38A(H38C,H38D)
5.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C12(H12), C13(H13), C15(H15),
 C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28),
  C30(H30), C40(H40), C40A(H40A)
5.e Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C37A(H37D,H37E,H37F), C39A(H39D,
 H39E,H39F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.53158(4) -0.08064(2) 0.90374(2) 0.01690(9) Uani 1 1 d . . . . .
O1 O 0.5705(2) 0.16556(12) 1.02261(10) 0.0215(4) Uani 1 1 d . . . . .
O2 O 0.6598(2) 0.04830(12) 0.95371(10) 0.0189(4) Uani 1 1 d . . . . .
O2W O 0.7348(2) -0.13650(14) 0.89354(12) 0.0283(4) Uani 1 1 d . . . . .
H2WA H 0.725330 -0.173022 0.845454 0.043 Uiso 1 1 d GR . . . .
H2WB H 0.745547 -0.172114 0.932744 0.043 Uiso 1 1 d GR . . . .
O3 O 0.5481(2) 0.07891(12) 0.21195(10) 0.0209(4) Uani 1 1 d . . . . .
O4 O 0.6955(2) 0.00550(15) 0.13224(11) 0.0291(4) Uani 1 1 d . . . . .
N1 N 0.8218(2) 0.29633(13) 0.60913(11) 0.0107(4) Uani 1 1 d . . . . .
N2 N 0.8591(2) 0.22829(13) 0.48475(11) 0.0102(4) Uani 1 1 d . . . . .
H2 H 0.886314 0.223409 0.434357 0.012 Uiso 1 1 calc R . . . .
C1 C 0.6196(3) 0.12739(17) 0.95872(14) 0.0164(5) Uani 1 1 d . . . . .
C2 C 0.6256(3) 0.18041(17) 0.88662(14) 0.0159(5) Uani 1 1 d . . . . .
C3 C 0.5627(3) 0.26180(18) 0.88915(15) 0.0214(5) Uani 1 1 d . . . . .
H3 H 0.525591 0.287106 0.938165 0.026 Uiso 1 1 calc R . . . .
C4 C 0.5540(4) 0.30616(19) 0.82000(16) 0.0245(6) Uani 1 1 d . . . . .
H4 H 0.511899 0.362420 0.821921 0.029 Uiso 1 1 calc R . . . .
C5 C 0.6063(3) 0.26910(17) 0.74774(15) 0.0179(5) Uani 1 1 d . . . . .
H5 H 0.599330 0.300160 0.700658 0.021 Uiso 1 1 calc R . . . .
C6 C 0.6691(3) 0.18669(16) 0.74372(14) 0.0130(5) Uani 1 1 d . . . . .
C7 C 0.6807(3) 0.14351(16) 0.81443(14) 0.0142(5) Uani 1 1 d . . . . .
H7 H 0.726506 0.088596 0.813422 0.017 Uiso 1 1 calc R . . . .
C8 C 0.7109(3) 0.14278(16) 0.66467(13) 0.0117(4) Uani 1 1 d . . . . .
C9 C 0.7713(3) 0.19758(15) 0.60388(13) 0.0103(4) Uani 1 1 d . . . . .
C10 C 0.7937(3) 0.15312(15) 0.52636(13) 0.0105(4) Uani 1 1 d . . . . .
C11 C 0.7588(3) 0.05338(16) 0.50473(13) 0.0111(4) Uani 1 1 d . . . . .
C12 C 0.7036(3) 0.00102(16) 0.56658(14) 0.0126(4) Uani 1 1 d . . . . .
H12 H 0.679866 -0.066908 0.555549 0.015 Uiso 1 1 calc R . . . .
C13 C 0.6817(3) 0.04389(16) 0.64378(14) 0.0127(4) Uani 1 1 d . . . . .
H13 H 0.645644 0.004209 0.683555 0.015 Uiso 1 1 calc R . . . .
C14 C 0.7740(3) 0.00556(16) 0.42240(14) 0.0124(4) Uani 1 1 d . . . . .
C15 C 0.7189(3) 0.03994(16) 0.35279(14) 0.0129(4) Uani 1 1 d . . . . .
H15 H 0.675231 0.095709 0.358498 0.015 Uiso 1 1 calc R . . . .
C16 C 0.7268(3) -0.00648(17) 0.27483(14) 0.0157(5) Uani 1 1 d . . . . .
C17 C 0.7931(3) -0.08709(18) 0.26599(15) 0.0195(5) Uani 1 1 d . . . . .
H17 H 0.801443 -0.117897 0.212879 0.023 Uiso 1 1 calc R . . . .
C18 C 0.8472(3) -0.12255(18) 0.33528(16) 0.0201(5) Uani 1 1 d . . . . .
H18 H 0.891348 -0.178134 0.329441 0.024 Uiso 1 1 calc R . . . .
C19 C 0.8368(3) -0.07695(16) 0.41281(14) 0.0152(5) Uani 1 1 d . . . . .
H19 H 0.872726 -0.101997 0.459836 0.018 Uiso 1 1 calc R . . . .
C20 C 0.6552(3) 0.02806(18) 0.20187(15) 0.0191(5) Uani 1 1 d . . . . .
C21 C 0.8729(3) 0.31117(15) 0.53715(13) 0.0100(4) Uani 1 1 d . . . . .
C22 C 0.9378(3) 0.40718(15) 0.51650(13) 0.0098(4) Uani 1 1 d . . . . .
C23 C 0.9071(3) 0.48584(16) 0.56566(13) 0.0115(4) Uani 1 1 d . . . . .
H23 H 0.843371 0.476148 0.610401 0.014 Uiso 1 1 calc R . . . .
C24 C 1.0307(3) 0.42198(15) 0.45050(13) 0.0109(4) Uani 1 1 d . . . . .
H24 H 1.051418 0.368771 0.416604 0.013 Uiso 1 1 calc R . . . .
O5 O 1.5024(2) 0.42407(12) 0.61736(11) 0.0209(4) Uani 1 1 d . . . . .
O6 O 1.2722(2) 0.25666(13) 0.44561(10) 0.0211(4) Uani 1 1 d . . . . .
O7 O 1.0002(2) 0.21457(11) 0.31193(10) 0.0160(3) Uani 1 1 d . . . . .
O8 O 1.1789(2) 0.63781(13) 0.72041(12) 0.0255(4) Uani 1 1 d . . . . .
C25 C 1.3208(3) 0.60488(17) 0.73169(16) 0.0193(5) Uani 1 1 d . . . . .
C26 C 1.4434(3) 0.63754(18) 0.79858(15) 0.0198(5) Uani 1 1 d . . . . .
H26 H 1.432757 0.686018 0.840757 0.024 Uiso 1 1 calc R . . . .
C27 C 1.5818(3) 0.59692(19) 0.80168(16) 0.0220(5) Uani 1 1 d . . . . .
H27 H 1.666426 0.618515 0.846822 0.026 Uiso 1 1 calc R . . . .
C28 C 1.5999(3) 0.52639(18) 0.74131(15) 0.0190(5) Uani 1 1 d . . . . .
H28 H 1.695770 0.500084 0.744752 0.023 Uiso 1 1 calc R . . . .
C29 C 1.4754(3) 0.49407(17) 0.67498(15) 0.0174(5) Uani 1 1 d . . . . .
C30 C 1.3358(3) 0.53310(17) 0.67012(16) 0.0206(5) Uani 1 1 d . . . . .
H30 H 1.251031 0.511041 0.625113 0.025 Uiso 1 1 calc R . . . .
C31 C 1.3673(3) 0.3807(2) 0.55480(18) 0.0292(6) Uani 1 1 d . . . . .
H31A H 1.333806 0.430477 0.525572 0.035 Uiso 1 1 calc R . . . .
H31B H 1.269612 0.348132 0.579859 0.035 Uiso 1 1 calc R . . . .
C32 C 1.4211(3) 0.3097(2) 0.49575(17) 0.0273(6) Uani 1 1 d . . . . .
H32A H 1.502136 0.342801 0.461843 0.033 Uiso 1 1 calc R . . . .
H32B H 1.474189 0.266561 0.525352 0.033 Uiso 1 1 calc R . . . .
C33 C 1.2953(3) 0.22785(18) 0.36300(15) 0.0183(5) Uani 1 1 d . . . . .
H33A H 1.384733 0.192002 0.361042 0.022 Uiso 1 1 calc R . . . .
H33B H 1.328139 0.284677 0.335056 0.022 Uiso 1 1 calc R . . . .
C34 C 1.1318(3) 0.16491(17) 0.32123(15) 0.0184(5) Uani 1 1 d . . . . .
H34A H 1.150129 0.135861 0.266375 0.022 Uiso 1 1 calc R . . . .
H34B H 1.095650 0.112226 0.353399 0.022 Uiso 1 1 calc R . . . .
C35 C 1.0089(3) 0.26494(19) 0.24288(16) 0.0216(5) Uani 1 1 d . . . . .
H35A H 1.039430 0.225211 0.196047 0.026 Uiso 1 1 calc R . . . .
H35B H 1.096919 0.324967 0.256320 0.026 Uiso 1 1 calc R . . . .
C49 C 1.1550(3) 0.71196(18) 0.78066(15) 0.0214(5) Uani 1 1 d . . . . .
H49A H 1.246803 0.769691 0.783720 0.026 Uiso 1 1 calc R . . . .
H49B H 1.155502 0.690405 0.835164 0.026 Uiso 1 1 calc R . . . .
O9 O 0.2101(6) 0.2737(3) 1.0174(2) 0.0519(15) Uani 0.648(9) 1 d D U P A 1
C40 C 0.1475(9) 0.2724(5) 0.9472(4) 0.0404(15) Uani 0.648(9) 1 d D U P A 1
H40 H 0.072472 0.214194 0.922645 0.049 Uiso 0.648(9) 1 calc R . P A 1
N3 N 0.1724(3) 0.34356(19) 0.90069(17) 0.0367(6) Uani 1 1 d D U . . .
C36 C 0.1008(15) 0.3406(7) 0.8166(5) 0.036(2) Uani 0.648(9) 1 d D U P A 1
H36A H 0.024737 0.276974 0.798061 0.043 Uiso 0.648(9) 1 calc R . P A 1
H36B H 0.192068 0.347972 0.781000 0.043 Uiso 0.648(9) 1 calc R . P A 1
C37 C 0.006(2) 0.4164(11) 0.8061(10) 0.044(3) Uani 0.648(9) 1 d D U P A 1
H37A H -0.040040 0.409697 0.748516 0.066 Uiso 0.648(9) 1 calc GR . P A 1
H37B H 0.080990 0.479745 0.822243 0.066 Uiso 0.648(9) 1 calc GR . P A 1
H37C H -0.085989 0.409175 0.840549 0.066 Uiso 0.648(9) 1 calc GR . P A 1
C38 C 0.2949(13) 0.4307(6) 0.9401(6) 0.039(2) Uani 0.648(9) 1 d D U P A 1
H38A H 0.339403 0.467840 0.897138 0.046 Uiso 0.648(9) 1 calc R . P A 1
H38B H 0.389519 0.412007 0.969451 0.046 Uiso 0.648(9) 1 calc R . P A 1
C39 C 0.2231(16) 0.4938(8) 0.9997(7) 0.058(3) Uani 0.648(9) 1 d D U P A 1
H39A H 0.142514 0.521621 0.969684 0.086 Uiso 0.648(9) 1 calc GR . P A 1
H39B H 0.313464 0.545345 1.029639 0.086 Uiso 0.648(9) 1 calc GR . P A 1
H39C H 0.166588 0.455665 1.038537 0.086 Uiso 0.648(9) 1 calc GR . P A 1
O9A O 0.1310(10) 0.2161(7) 0.9710(5) 0.048(3) Uani 0.352(9) 1 d D U P A 2
C40A C 0.0999(13) 0.2505(7) 0.9076(8) 0.032(3) Uani 0.352(9) 1 d D U P A 2
H40A H 0.024859 0.211742 0.863474 0.038 Uiso 0.352(9) 1 calc R . P A 2
C36A C 0.128(3) 0.3690(13) 0.8177(10) 0.046(5) Uani 0.352(9) 1 d D U P A 2
H36C H 0.232674 0.395296 0.794508 0.056 Uiso 0.352(9) 1 calc R . P A 2
H36D H 0.068301 0.310064 0.780851 0.056 Uiso 0.352(9) 1 calc R . P A 2
C37A C 0.021(4) 0.441(2) 0.8195(16) 0.042(6) Uani 0.352(9) 1 d D U P A 2
H37D H -0.002646 0.454614 0.763907 0.063 Uiso 0.352(9) 1 calc GR . P A 2
H37E H 0.080869 0.499772 0.855007 0.063 Uiso 0.352(9) 1 calc GR . P A 2
H37F H -0.083619 0.414470 0.840893 0.063 Uiso 0.352(9) 1 calc GR . P A 2
C38A C 0.287(3) 0.4132(13) 0.9589(10) 0.048(5) Uani 0.352(9) 1 d D U P A 2
H38C H 0.355611 0.460659 0.929961 0.057 Uiso 0.352(9) 1 calc R . P A 2
H38D H 0.362335 0.381537 0.989174 0.057 Uiso 0.352(9) 1 calc R . P A 2
C39A C 0.195(4) 0.4632(19) 1.0180(15) 0.090(10) Uani 0.352(9) 1 d D U P A 2
H39D H 0.137129 0.504485 0.989772 0.136 Uiso 0.352(9) 1 calc GR . P A 2
H39E H 0.274999 0.502238 1.063066 0.136 Uiso 0.352(9) 1 calc GR . P A 2
H39F H 0.113279 0.415601 1.039956 0.136 Uiso 0.352(9) 1 calc GR . P A 2
O1W O 0.9962(4) -0.00908(19) 0.0858(2) 0.0694(9) Uani 1 1 d . . . . .
H1WA H 1.062489 0.047104 0.087715 0.104 Uiso 1 1 d G . . . .
H1WB H 0.898634 -0.002408 0.098456 0.104 Uiso 1 1 d G . . . .


_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
Zn1 O1 1.9470(17) 2_657 ?
Zn1 O2 1.9726(17) . ?
Zn1 O2W 2.0239(19) . ?
Zn1 O3 1.9768(17) 2_656 ?
Zn1 O4 2.430(2) 2_656 ?
O9Ab C40A 1.246(11) . ?
C40Ab H40A 0.9500 . ?
C36Ab H36C 0.9900 . ?
C36Ab H36D 0.9900 . ?
C36Ab C37A 1.498(15) . ?
C37Ab H37D 0.9800 . ?
C37Ab H37E 0.9800 . ?
C37Ab H37F 0.9800 . ?
C38Ab H38C 0.9900 . ?
C38Ab H38D 0.9900 . ?
C38Ab C39A 1.496(15) . ?
C39Ab H39D 0.9800 . ?
C39Ab H39E 0.9800 . ?
C39Ab H39F 0.9800 . ?
O1 Zn1 1.9470(17) 2_657 ?
O1 C1 1.269(3) . ?
O2 C1 1.254(3) . ?
O2W H2WA 0.8866 . ?
O2W H2WB 0.8869 . ?
O3 Zn1 1.9768(17) 2_656 ?
O3 C20 1.275(3) . ?
O4 Zn1 2.430(2) 2_656 ?
O4 C20 1.250(3) . ?
N1 C9 1.387(3) . ?
N1 C21 1.323(3) . ?
N2 H2 0.8800 . ?
N2 C10 1.392(3) . ?
N2 C21 1.367(3) . ?
C1 C2 1.494(3) . ?
C2 C3 1.384(4) . ?
C2 C7 1.399(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.383(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.396(3) . ?
C6 C7 1.399(3) . ?
C6 C8 1.483(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.413(3) . ?
C8 C13 1.392(3) . ?
C9 C10 1.408(3) . ?
C10 C11 1.402(3) . ?
C11 C12 1.395(3) . ?
C11 C14 1.478(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.393(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.391(3) . ?
C14 C19 1.398(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.393(3) . ?
C16 C17 1.389(4) . ?
C16 C20 1.488(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.392(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.387(3) . ?
C19 H19 0.9500 . ?
C20 Zn1 2.529(3) 2_656 ?
C21 C22 1.468(3) . ?
C22 C23 1.397(3) . ?
C22 C24 1.397(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.387(3) 2_766 ?
C24 C23 1.387(3) 2_766 ?
C24 H24 0.9500 . ?
O5 C29 1.371(3) . ?
O5 C31 1.431(3) . ?
O6 C32 1.430(3) . ?
O6 C33 1.420(3) . ?
O7 C34 1.434(3) . ?
O7 C35 1.428(3) . ?
O8 C25 1.364(3) . ?
O8 C49 1.430(3) . ?
C25 C26 1.395(3) . ?
C25 C30 1.395(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.394(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.379(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.397(3) . ?
C29 C30 1.389(3) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.493(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.509(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C49 1.494(4) 2_766 ?
C49 C35 1.494(4) 2_766 ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
N3 C36 1.457(7) . ?
N3 C38 1.471(7) . ?
N3 C40A 1.371(9) . ?
N3 C36A 1.502(13) . ?
N3 C38A 1.422(13) . ?
O9A C40 1.227(8) . ?
C40A H40 0.9500 . ?
C40A N3 1.351(7) . ?
C36A H36A 0.9900 . ?
C36A H36B 0.9900 . ?
C36A C37 1.498(10) . ?
C37A H37A 0.9800 . ?
C37A H37B 0.9800 . ?
C37A H37C 0.9800 . ?
C38A H38A 0.9900 . ?
C38A H38B 0.9900 . ?
C38A C39 1.506(8) . ?
C39A H39A 0.9800 . ?
C39A H39B 0.9800 . ?
C39A H39C 0.9800 . ?
O1W H1WA 0.8699 . ?
O1W H1WB 0.8701 . ?

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 Zn1 O2 117.10(7) 2_657 . ?
O9Ab C40Ab N3 120.9(10) . . ?
C37Ab C36Ab N3 113.2(15) . . ?
O1 Zn1 O2W 95.95(8) 2_657 . ?
O1 Zn1 O3 127.53(8) 2_657 2_656 ?
O1 Zn1 O4 100.88(7) 2_657 2_656 ?
O2 Zn1 O2W 95.02(8) . . ?
O2 Zn1 O3 109.75(7) . 2_656 ?
O2 Zn1 O4 86.73(7) . 2_656 ?
O2W Zn1 O4 160.11(7) . 2_656 ?
O3 Zn1 O2W 102.37(8) 2_656 . ?
O3 Zn1 O4 58.75(7) 2_656 2_656 ?
O9Ab C40Ab H40A 119.5 . . ?
C37Ab C36Ab H36C 108.9 . . ?
H36Cb C36Ab H36D 107.7 . . ?
C37Ab C36Ab H36D 108.9 . . ?
C36Ab C37Ab H37D 109.5 . . ?
H37Db C37Ab H37E 109.5 . . ?
C36Ab C37Ab H37E 109.5 . . ?
H37Db C37Ab H37F 109.5 . . ?
H37Eb C37Ab H37F 109.5 . . ?
C1 O1 Zn1 117.39(15) . 2_657 ?
C1 O2 Zn1 130.35(16) . . ?
Zn1 O2W H2WA 110.5 . . ?
C36Ab C37Ab H37F 109.5 . . ?
C39Ab C38Ab H38C 109.5 . . ?
C39Ab C38Ab H38D 109.5 . . ?
Zn1 O2W H2WB 110.3 . . ?
H2WA O2W H2WB 108.4 . . ?
C20 O3 Zn1 99.85(15) . 2_656 ?
H38Cb C38Ab H38D 108.1 . . ?
C38Ab C39Ab H39D 109.5 . . ?
C38Ab C39Ab H39E 109.5 . . ?
C20 O4 Zn1 79.85(16) . 2_656 ?
C21 N1 C9 104.96(18) . . ?
H39Db C39Ab H39E 109.5 . . ?
C38Ab C39Ab H39F 109.5 . . ?
H39Db C39Ab H39F 109.5 . . ?
C10 N2 H2 126.6 . . ?
C21 N2 H2 126.6 . . ?
C21 N2 C10 106.86(18) . . ?
O1 C1 C2 117.0(2) . . ?
O2 C1 O1 123.2(2) . . ?
H39Eb C39Ab H39F 109.5 . . ?
C40Ab N3 C36A 112.6(9) . . ?
O2 C1 C2 119.8(2) . . ?
C38Ab N3 C36A 118.7(10) . . ?
C40Ab N3 C38A 128.5(9) . . ?
H36Aa C36A H36B 107.7 . . ?
C3 C2 C1 119.5(2) . . ?
C3 C2 C7 120.0(2) . . ?
H37Aa C37A H37B 109.5 . . ?
H37Ba C37A H37C 109.5 . . ?
C7 C2 C1 120.2(2) . . ?
H37Aa C37A H37C 109.5 . . ?
H38Aa C38A H38B 107.7 . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.7(2) . . ?
C4 C3 H3 120.1 . . ?
H39Aa C39A H39B 109.5 . . ?
H39Aa C39A H39C 109.5 . . ?
H39Ba C39A H39C 109.5 . . ?
C3 C4 H4 119.7 . . ?
C3 C4 C5 120.6(2) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.6(2) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C7 118.4(2) . . ?
C5 C6 C8 120.3(2) . . ?
C7 C6 C8 121.1(2) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 C2 120.6(2) . . ?
C6 C7 H7 119.7 . . ?
C9 C8 C6 122.5(2) . . ?
C13 C8 C6 121.5(2) . . ?
C13 C8 C9 115.9(2) . . ?
N1 C9 C8 128.7(2) . . ?
N1 C9 C10 110.24(18) . . ?
C10 C9 C8 121.0(2) . . ?
N2 C10 C9 104.84(18) . . ?
N2 C10 C11 132.3(2) . . ?
C11 C10 C9 122.8(2) . . ?
C10 C11 C14 123.5(2) . . ?
C12 C11 C10 115.0(2) . . ?
C12 C11 C14 121.5(2) . . ?
C11 C12 H12 118.5 . . ?
C13 C12 C11 122.9(2) . . ?
C13 C12 H12 118.5 . . ?
C8 C13 C12 122.3(2) . . ?
C8 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
C15 C14 C11 120.1(2) . . ?
C15 C14 C19 118.8(2) . . ?
C19 C14 C11 121.0(2) . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.7(2) . . ?
C16 C15 H15 119.6 . . ?
C15 C16 C20 119.2(2) . . ?
C17 C16 C15 120.0(2) . . ?
C17 C16 C20 120.7(2) . . ?
C16 C17 H17 120.1 . . ?
C16 C17 C18 119.7(2) . . ?
C18 C17 H17 120.1 . . ?
C17 C18 H18 119.9 . . ?
C19 C18 C17 120.2(2) . . ?
C19 C18 H18 119.9 . . ?
C14 C19 H19 119.7 . . ?
C18 C19 C14 120.6(2) . . ?
C18 C19 H19 119.7 . . ?
O3 C20 Zn1 50.36(11) . 2_656 ?
O3 C20 C16 118.2(2) . . ?
O4 C20 Zn1 71.04(14) . 2_656 ?
O4 C20 O3 121.0(2) . . ?
O4 C20 C16 120.8(2) . . ?
C16 C20 Zn1 165.61(18) . 2_656 ?
N1 C21 N2 113.10(19) . . ?
N1 C21 C22 122.95(19) . . ?
N2 C21 C22 123.95(19) . . ?
C23 C22 C21 118.4(2) . . ?
C23 C22 C24 119.5(2) . . ?
C24 C22 C21 122.1(2) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 C22 120.3(2) 2_766 . ?
C24 C23 H23 119.8 2_766 . ?
C22 C24 H24 119.9 . . ?
C23 C24 C22 120.2(2) 2_766 . ?
C23 C24 H24 119.9 2_766 . ?
C29 O5 C31 116.86(19) . . ?
C33 O6 C32 114.49(19) . . ?
C35 O7 C34 112.86(18) . . ?
C25 O8 C49 117.84(19) . . ?
O8 C25 C26 124.6(2) . . ?
O8 C25 C30 114.5(2) . . ?
C26 C25 C30 121.0(2) . . ?
C25 C26 H26 121.0 . . ?
C27 C26 C25 118.0(2) . . ?
C27 C26 H26 121.0 . . ?
C26 C27 H27 119.0 . . ?
C28 C27 C26 122.1(2) . . ?
C28 C27 H27 119.0 . . ?
C27 C28 H28 120.4 . . ?
C27 C28 C29 119.2(2) . . ?
C29 C28 H28 120.4 . . ?
O5 C29 C28 115.8(2) . . ?
O5 C29 C30 124.1(2) . . ?
C30 C29 C28 120.1(2) . . ?
C25 C30 H30 120.2 . . ?
C29 C30 C25 119.6(2) . . ?
C29 C30 H30 120.2 . . ?
O5 C31 H31A 109.8 . . ?
O5 C31 H31B 109.8 . . ?
O5 C31 C32 109.5(2) . . ?
H31A C31 H31B 108.2 . . ?
C32 C31 H31A 109.8 . . ?
C32 C31 H31B 109.8 . . ?
O6 C32 C31 105.9(2) . . ?
O6 C32 H32A 110.5 . . ?
O6 C32 H32B 110.5 . . ?
C31 C32 H32A 110.5 . . ?
C31 C32 H32B 110.5 . . ?
H32A C32 H32B 108.7 . . ?
O6 C33 H33A 110.2 . . ?
O6 C33 H33B 110.2 . . ?
O6 C33 C34 107.67(19) . . ?
H33A C33 H33B 108.5 . . ?
C34 C33 H33A 110.2 . . ?
C34 C33 H33B 110.2 . . ?
O7 C34 C33 113.89(19) . . ?
O7 C34 H34A 108.8 . . ?
O7 C34 H34B 108.8 . . ?
C33 C34 H34A 108.8 . . ?
C33 C34 H34B 108.8 . . ?
H34A C34 H34B 107.7 . . ?
O7 C35 H35A 109.5 . . ?
O7 C35 H35B 109.5 . . ?
O7 C35 C49 110.8(2) . 2_766 ?
H35A C35 H35B 108.1 . . ?
C49 C35 H35A 109.5 2_766 . ?
C49 C35 H35B 109.5 2_766 . ?
O8 C49 C35 108.7(2) . 2_766 ?
O8 C49 H49A 110.0 . . ?
O8 C49 H49B 110.0 . . ?
C35 C49 H49A 110.0 2_766 . ?
C35 C49 H49B 110.0 2_766 . ?
H49A C49 H49B 108.3 . . ?
N3 C40Ab H40A 119.5 . . ?
N3 C36Ab H36C 108.9 . . ?
N3 C36Ab H36D 108.9 . . ?
N3 C38Ab H38C 109.5 . . ?
N3 C38Ab H38D 109.5 . . ?
C40A N3 C36 127.6(5) . . ?
C40A N3 C38 114.0(6) . . ?
C36A N3 C38 118.3(6) . . ?
N3 C40A H40 116.0 . . ?
O9A C40A H40 116.0 . . ?
O9A C40A N3 127.9(6) . . ?
N3 C36A H36A 108.8 . . ?
N3 C36A H36B 108.8 . . ?
N3 C36A C37 113.8(8) . . ?
C37A C36A H36A 108.8 . . ?
C37A C36A H36B 108.8 . . ?
C36A C37A H37A 109.5 . . ?
C36A C37A H37B 109.5 . . ?
C36A C37A H37C 109.5 . . ?
N3 C38A H38A 108.9 . . ?
N3 C38A H38B 108.9 . . ?
N3 C38A C39 113.4(7) . . ?
N3 C38Ab C39A 110.7(17) . . ?
C39A C38A H38A 108.9 . . ?
C39A C38A H38B 108.9 . . ?
C38A C39A H39A 109.5 . . ?
C38A C39A H39B 109.5 . . ?
C38A C39A H39C 109.5 . . ?
H1WA O1W H1WB 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
Zn1 O1 C1 O2 -25.4(3) 2_657 . . . ?
Zn1 O1 C1 C2 153.55(17) 2_657 . . . ?
Zn1 O2 C1 O1 99.4(3) . . . . ?
Zn1 O2 C1 C2 -79.6(3) . . . . ?
Zn1 O3 C20 O4 8.6(3) 2_656 . . . ?
Zn1 O3 C20 C16 -169.42(17) 2_656 . . . ?
Zn1 O4 C20 O3 -7.0(2) 2_656 . . . ?
Zn1 O4 C20 C16 171.0(2) 2_656 . . . ?
C38Ab N3 C40Ab O9Ab -0.2(18) . . . . ?
C36Ab N3 C38Ab C39Ab 99(2) . . . . ?
C40Ab N3 C36Ab C37Ab 112.8(18) . . . . ?
C36Ab N3 C40Ab O9Ab 176.0(13) . . . . ?
C40Ab N3 C38Ab C39Ab -85(2) . . . . ?
C38Ab N3 C36Ab C37Ab -71(2) . . . . ?
O1 C1 C2 C3 -6.5(4) . . . . ?
O1 C1 C2 C7 179.1(2) . . . . ?
O2 C1 C2 C3 172.5(2) . . . . ?
O2 C1 C2 C7 -1.9(4) . . . . ?
N1 C9 C10 N2 -0.2(2) . . . . ?
N1 C9 C10 C11 177.6(2) . . . . ?
N1 C21 C22 C23 -16.1(3) . . . . ?
N1 C21 C22 C24 162.8(2) . . . . ?
N2 C10 C11 C12 175.7(2) . . . . ?
N2 C10 C11 C14 -5.9(4) . . . . ?
N2 C21 C22 C23 164.0(2) . . . . ?
N2 C21 C22 C24 -17.1(3) . . . . ?
C1 C2 C3 C4 -174.1(2) . . . . ?
C1 C2 C7 C6 172.7(2) . . . . ?
C2 C3 C4 C5 0.7(4) . . . . ?
C3 C2 C7 C6 -1.6(4) . . . . ?
C3 C4 C5 C6 -0.2(4) . . . . ?
C4 C5 C6 C7 -1.1(4) . . . . ?
C4 C5 C6 C8 174.7(2) . . . . ?
C5 C6 C7 C2 2.1(4) . . . . ?
C5 C6 C8 C9 32.5(3) . . . . ?
C5 C6 C8 C13 -142.9(2) . . . . ?
C6 C8 C9 N1 9.1(4) . . . . ?
C6 C8 C9 C10 -173.5(2) . . . . ?
C6 C8 C13 C12 173.1(2) . . . . ?
C7 C2 C3 C4 0.2(4) . . . . ?
C7 C6 C8 C9 -151.7(2) . . . . ?
C7 C6 C8 C13 32.8(3) . . . . ?
C8 C6 C7 C2 -173.8(2) . . . . ?
C8 C9 C10 N2 -178.0(2) . . . . ?
C8 C9 C10 C11 -0.2(3) . . . . ?
C9 N1 C21 N2 0.0(2) . . . . ?
C9 N1 C21 C22 -179.9(2) . . . . ?
C9 C8 C13 C12 -2.7(3) . . . . ?
C9 C10 C11 C12 -1.4(3) . . . . ?
C9 C10 C11 C14 177.0(2) . . . . ?
C10 N2 C21 N1 -0.1(3) . . . . ?
C10 N2 C21 C22 179.8(2) . . . . ?
C10 C11 C12 C13 1.0(3) . . . . ?
C10 C11 C14 C15 -41.7(3) . . . . ?
C10 C11 C14 C19 141.1(2) . . . . ?
C11 C12 C13 C8 1.1(4) . . . . ?
C11 C14 C15 C16 -177.6(2) . . . . ?
C11 C14 C19 C18 178.6(2) . . . . ?
C12 C11 C14 C15 136.7(2) . . . . ?
C12 C11 C14 C19 -40.5(3) . . . . ?
C13 C8 C9 N1 -175.2(2) . . . . ?
C13 C8 C9 C10 2.2(3) . . . . ?
C14 C11 C12 C13 -177.5(2) . . . . ?
C14 C15 C16 C17 -1.1(3) . . . . ?
C14 C15 C16 C20 175.5(2) . . . . ?
C15 C14 C19 C18 1.3(3) . . . . ?
C15 C16 C17 C18 1.7(4) . . . . ?
C15 C16 C20 Zn1 -54.8(8) . . . 2_656 ?
C15 C16 C20 O3 -20.1(3) . . . . ?
C15 C16 C20 O4 161.9(2) . . . . ?
C16 C17 C18 C19 -0.8(4) . . . . ?
C17 C16 C20 Zn1 121.8(7) . . . 2_656 ?
C17 C16 C20 O3 156.5(2) . . . . ?
C17 C16 C20 O4 -21.5(4) . . . . ?
C17 C18 C19 C14 -0.8(4) . . . . ?
C19 C14 C15 C16 -0.4(3) . . . . ?
C20 C16 C17 C18 -174.9(2) . . . . ?
C21 N1 C9 C8 177.7(2) . . . . ?
C21 N1 C9 C10 0.1(2) . . . . ?
C21 N2 C10 C9 0.2(2) . . . . ?
C21 N2 C10 C11 -177.3(2) . . . . ?
C21 C22 C23 C24 178.6(2) . . . 2_766 ?
C21 C22 C24 C23 -178.5(2) . . . 2_766 ?
C23 C22 C24 C23 0.4(4) . . . 2_766 ?
C24 C22 C23 C24 -0.4(4) . . . 2_766 ?
O5 C29 C30 C25 -179.4(2) . . . . ?
O5 C31 C32 O6 168.8(2) . . . . ?
O6 C33 C34 O7 67.4(2) . . . . ?
O8 C25 C26 C27 180.0(2) . . . . ?
O8 C25 C30 C29 179.9(2) . . . . ?
C25 O8 C49 C35 -178.7(2) . . . 2_766 ?
C25 C26 C27 C28 -0.1(4) . . . . ?
C26 C25 C30 C29 -0.6(4) . . . . ?
C26 C27 C28 C29 -0.3(4) . . . . ?
C27 C28 C29 O5 179.8(2) . . . . ?
C27 C28 C29 C30 0.3(4) . . . . ?
C28 C29 C30 C25 0.2(4) . . . . ?
C29 O5 C31 C32 177.5(2) . . . . ?
C30 C25 C26 C27 0.6(4) . . . . ?
C31 O5 C29 C28 171.8(2) . . . . ?
C31 O5 C29 C30 -8.6(4) . . . . ?
C32 O6 C33 C34 174.4(2) . . . . ?
C33 O6 C32 C31 145.7(2) . . . . ?
C34 O7 C35 C49 161.5(2) . . . 2_766 ?
C35 O7 C34 C33 81.4(2) . . . . ?
C49 O8 C25 C26 1.0(4) . . . . ?
C49 O8 C25 C30 -179.6(2) . . . . ?
O9A C40A N3 C36A 178.3(8) . . . . ?
O9A C40A N3 C38A 2.4(10) . . . . ?
C40A N3 C36A C37A 123.5(11) . . . . ?
C40A N3 C38A C39A -80.8(10) . . . . ?
C36A N3 C38A C39A 102.8(11) . . . . ?
C38A N3 C36A C37A -60.8(13) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'solvothermal DEF'
####################################################################### 
# 
# 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_cu_gg004_0m
_database_code_depnum_ccdc_archive 'CCDC 1519351'
_audit_update_record             
;
2016-11-25 deposited with the CCDC.
2017-01-27 downloaded from the CCDC.
;
_audit_creation_date             2016-11-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
# start Validation Reply Form
_vrf_REFNR01_cu_gg004_0m         
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: This was ignored in order to properly model the disorder.
 A solution in which this ratio was closer to 10:1 and the lesser 
 components of the disorder not modelled was also archived. 
;
_vrf_PLAT029_cu_gg004_0m         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.898 Note
RESPONSE: Weakly diffracting crystal with severe disorder.
;
_vrf_PLAT307_cu_gg004_0m         
;
PROBLEM: Isolated Metal Atom found in Structure (Unusual) Cu1 Check
RESPONSE: Due to the severe disorder.
;
_vrf_PLAT312_cu_gg004_0m         
;
PROBLEM: Strange C-O-H Geometry (C-O < 1.25 Ang) ..... O52A Check
RESPONSE:Due to the severe disorder.
;
_vrf_PLAT417_cu_gg004_0m         
;
PROBLEM: Short Inter D-H..H-D H0AA .. H53C .. 1.59 Ang.
RESPONSE:Due to the severe disorder.
;
_vrf_PLAT701_cu_gg004_0m         
;
PROBLEM: Bond Calc 5.78(5), Rep 1.198(19), Dev.. 91.64 Sigma
RESPONSE:Due to the severe disorder.
;
_vrf_PLAT702_cu_gg004_0m         
;
PROBLEM: Angle Calc 131(3), Rep 120.6(16), Dev.. 3.47 Sigma
RESPONSE: Due to the severe disorder.
;
_vrf_PLAT703_cu_gg004_0m         
;
PROBLEM: Torsion Calc 168(3), Rep -178(4), Dev.. 4.67 Sigma
RESPONSE: Due to the severe disorder.
;
_vrf_PLAT084_cu_gg004_0m         
;
PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.39 Report
RESPONSE: Due to the severe disorder.
;
_vrf_PLAT088_cu_gg004_0m         
;
PROBLEM: Poor Data / Parameter Ratio .................... 6.64 Note
RESPONSE: This was ignored in order to properly model the disorder.
 A solution in which this ratio was closer to 10:1 and the lesser 
 components of the disorder not modelled was also archived.
;
_vrf_PLAT245_cu_gg004_0m         
;
PROBLEM: U(iso) H0AB Smaller than U(eq) O0AA by ... 0.063 AngSq
RESPONSE:Due to the severe disorder
;
_vrf_PLAT415_cu_gg004_0m         
;
PROBLEM: Short Inter D-H..H-X H0AB .. H56B .. 2.09 Ang.
RESPONSE: Due to the severe disorder
;
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C48 H28 N4 O8, 2(H2 O), C34 H38 N2 O8, 1.5(C5 H11 N O), Cu'
_chemical_formula_sum            'C89.5 H86.5 Cu N7.5 O19.5'
_chemical_formula_weight         1641.03
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.2427(6)
_cell_length_b                   14.0544(5)
_cell_length_c                   17.5540(6)
_cell_angle_alpha                90
_cell_angle_beta                 103.263(2)
_cell_angle_gamma                90
_cell_volume                     4140.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      78.12
_cell_measurement_theta_min      2.63
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.6255
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1170 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.8294.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1727
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.898
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28562
_diffrn_reflns_point_group_measured_fraction_full 0.898
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        65.075
_diffrn_reflns_theta_max         65.075
_diffrn_reflns_theta_min         3.240
_diffrn_ambient_temperature      173.35
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3945
_reflns_number_total             6343
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.493
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         6343
_refine_ls_number_restraints     2324
_refine_ls_R_factor_all          0.1677
_refine_ls_R_factor_gt           0.1245
_refine_ls_restrained_S_all      1.314
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3433
_refine_ls_wR_factor_ref         0.3856
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H64A of C64A, H52C of C52B, H56B of C56B, H66A of C66A,
  H67A of C67A, H68A of C68A, H59B of C59B, H66B of C66B, H56A of C56A, H53D of
  C53B, H54B of C54B, H64B of C64B, H68B of C68B, H59A of C59A, H58A of C58A,
  H58B of C58B, H67B of C67B, H54A of C54A, H53B of C53A, H73 of C73, H72 of
  C72, H54 of C54, H52B of C52A, H53A of C53, H52 of C52, H64 of C64, H67 of
  C67, H59 of C59, H66 of C66, H68 of C68, H56 of C56, H58 of C58, H22A of C22A,
   H21 of C21, H24A of C24A, H23A of C23A, H23 of C23, H1E of C1E, H22 of C22,
  H21A of C21A, H24 of C24, H1D of C1D, H5 of C5, H3 of C3, H7 of C7, All N(H,H,
  H) groups, All Cu(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H0AA of C69B, All O(H) groups
2. Restrained distances
 N1D-C1D
 1.36 with sigma of 0.02
 C1D-O1D
 1.22 with sigma of 0.02
 N1E-C1E
 1.36 with sigma of 0.02
 C1E-O1E
 1.22 with sigma of 0.02
 N1D-C2D \\sim N1D-C4D
 with sigma of 0.02
 C2D-C3D \\sim C4D-C5D
 with sigma of 0.02
 N1E-C2E \\sim N1E-C4E
 with sigma of 0.02
 C2E-C3E \\sim C4E-C5E
 with sigma of 0.02
3. Restrained planarity
 N20, C20, C21, C22, C23, C24
 with sigma of 0.1
 N50, N51, C70, C57, C58, C59, C60, C61, C62
 with sigma of 0.1
 O50, O51, C50, C51
 with sigma of 0.1
 C50, C51, C52, C53, C54, C55, C56
 with sigma of 0.1
 O50A, O51A, C50A, C51A
 with sigma of 0.1
 C50A, C51A, C52A, C53A, C54A, C55A, C56A
 with sigma of 0.1
 O50B, O51B, C50B, C51B
 with sigma of 0.1
 C50B, C51B, C52B, C53B, C54B, C55B, C56B
 with sigma of 0.1
 C57A, C58A, C59A, C60A, C61A, C62A
 with sigma of 0.1
 C57B, C58B, C59B, C60B, C61B, C62B
 with sigma of 0.1
 O52, O53, C65, C69
 with sigma of 0.1
 O52A, O53A, C65A, C69A
 with sigma of 0.1
 O52B, O53B, C65B, C69B
 with sigma of 0.1
 C63A, C64A, C65A, C66A, C67A, C68A, C69A
 with sigma of 0.1
 C63B, C64B, C65B, C66B, C67B, C68B, C69B
 with sigma of 0.1
 C63, C64, C65, C66, C67, C68, C69
 with sigma of 0.1
 O1D, N1D, C1D, C2D, C4D
 with sigma of 0.1
 O1E, N1E, C1E, C2E, C4E
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N20 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim N20A \\sim C20A
\\sim C21A \\sim C22A \\sim C23A \\sim C24A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O50 \\sim O51 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim
C56 \\sim O50A \\sim O51A \\sim C50A \\sim C51A \\sim C52A \\sim C53A \\sim
C54A \\sim C55A \\sim C56A \\sim O50B \\sim O51B \\sim C50B \\sim C51B \\sim
C52B \\sim C53B \\sim C54B \\sim C55B \\sim C56B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
O52 \\sim O53 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim
C69 \\sim O52A \\sim O53A \\sim C63A \\sim C64A \\sim C65A \\sim C66A \\sim
C67A \\sim C68A \\sim C69A \\sim O52B \\sim O53B \\sim C63B \\sim C64B \\sim
C65B \\sim C66B \\sim C67B \\sim C68B \\sim C69B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C57A \\sim C58A
\\sim C59A \\sim C60A \\sim C61A \\sim C62A \\sim C57B \\sim C58B \\sim C59B
\\sim C60B \\sim C61B \\sim C62B: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O1D \\sim N1D \\sim C1D \\sim C2D \\sim C3D \\sim C4D \\sim C5D: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
O1E \\sim N1E \\sim C1E \\sim C2E \\sim C3E \\sim C4E \\sim C5E: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O51A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O52A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O53A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O52B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O53B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C3E) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C4E) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C50B) = Uanis(O51A) = Uanis(O51)
Uanis(C55A) = Uanis(C55) = Uanis(C55B)
Uanis(C54A) = Uanis(C54B) = Uanis(C54)
Uanis(C50) = Uanis(C50A)
5. Rigid body (RIGU) restrains
 O1D, N1D, C1D, C2D, C3D, C4D, C5D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1E, N1E, C1E, C2E, C3E, C4E, C5E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{N50, N51, C70, O50A, O51A, O52A, O53A, C50A, C51A, C52A, C53A, C54A, C55A,
C56A, C57A, C58A, C59A, C60A, C61A, C62A, C63A, C64A, C65A, C66A, C67A, C68A,
C69A} sigma for 1-2: 0.02, 1-3: 0.02
{N50, N51, C70, O50B, O51B, O52B, O53B, C50B, C51B, C52B, C53B, C54B, C55B,
C56B, C57B, C58B, C59B, C60B, C61B, C62B, C63B, C64B, C65B, C66B, C67B, C68B,
C69B} sigma for 1-2: 0.02, 1-3: 0.02
as
{N50, N51, C70, O50, O51, O52, O53, C50, C51, C52, C53, C54, C55, C56, C57,
C58, C59, C60, C61, C62, C63, C64, C65, C66, C67, C68, C69}
{N20A, C20A, C21A, C22A, C23A, C24A} sigma for 1-2: 0.02, 1-3: 0.02
as
{N20, C20, C21, C22, C23, C24}
{O1E, N1E, C1E, C2E, C3E, C4E, C5E} sigma for 1-2: 0.02, 1-3: 0.02
as
{O1D, N1D, C1D, C2D, C3D, C4D, C5D}
7. Others
 1*[Sof(H51)+Sof(O50)+Sof(O51)+Sof(O52)+Sof(O53)+Sof(H53)+Sof(C50)+Sof(C51)+
 Sof(C52)+Sof(H52)+Sof(C53)+Sof(H53A)+Sof(C54)+Sof(H54)+Sof(C55)+Sof(C56)+
 Sof(H56)+Sof(C57)+Sof(C58)+Sof(H58)+Sof(C59)+Sof(H59)+Sof(C60)+Sof(C61)+
 Sof(C62)+Sof(C63)+Sof(C64)+Sof(H64)+Sof(C65)+Sof(C66)+Sof(H66)+Sof(C67)+
 Sof(H67)+Sof(C68)+Sof(H68)+Sof(C69)+Sof(O1E)+Sof(N1E)+Sof(C1E)+Sof(H1E)+
 Sof(C2E)+Sof(H2EA)+Sof(H2EB)+Sof(C3E)+Sof(H3EA)+Sof(H3EB)+Sof(H3EC)+Sof(C4E)+
 Sof(H4EA)+Sof(H4EB)+Sof(C5E)+Sof(H5EA)+Sof(H5EB)+Sof(H5EC)]+1*[Sof(H51A)+
 Sof(O50A)+Sof(O51A)+Sof(O52A)+Sof(H52A)+Sof(O53A)+Sof(C50A)+Sof(C51A)+
 Sof(C52A)+Sof(H52B)+Sof(C53A)+Sof(H53B)+Sof(C54A)+Sof(H54A)+Sof(C55A)+
 Sof(C56A)+Sof(H56A)+Sof(C57A)+Sof(C58A)+Sof(H58A)+Sof(C59A)+Sof(H59A)+
 Sof(C60A)+Sof(C61A)+Sof(C62A)+Sof(C63A)+Sof(C64A)+Sof(H64A)+Sof(C65A)+
 Sof(C66A)+Sof(H66A)+Sof(C67A)+Sof(H67A)+Sof(C68A)+Sof(H68A)+Sof(C69A)]+1*
 [Sof(H51B)+Sof(O50B)+Sof(O51B)+Sof(O52B)+Sof(O53B)+Sof(H53C)+Sof(C50B)+
 Sof(C51B)+Sof(C52B)+Sof(H52C)+Sof(C53B)+Sof(H53D)+Sof(C54B)+Sof(H54B)+
 Sof(C55B)+Sof(C56B)+Sof(H56B)+Sof(C57B)+Sof(C58B)+Sof(H58B)+Sof(C59B)+
 Sof(H59B)+Sof(C60B)+Sof(C61B)+Sof(C62B)+Sof(C63B)+Sof(C64B)+Sof(H64B)+
 Sof(C65B)+Sof(C66B)+Sof(H66B)+Sof(C67B)+Sof(H67B)+Sof(C68B)+Sof(H68B)+
 Sof(C69B)+Sof(O1D)+Sof(N1D)+Sof(C1D)+Sof(H1D)+Sof(C2D)+Sof(H2DA)+Sof(H2DB)+
 Sof(C3D)+Sof(H3DA)+Sof(H3DB)+Sof(H3DC)+Sof(C4D)+Sof(H4DA)+Sof(H4DB)+Sof(C5D)+
 Sof(H5DA)+Sof(H5DB)+Sof(H5DC)]=1 with esd of 0.0001
 Sof(N20A)=Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=
 Sof(H23A)=Sof(C24A)=Sof(H24A)=1-FVAR(1)
 Sof(N20)=Sof(C20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=
 Sof(C24)=Sof(H24)=FVAR(1)
 Sof(H51)=Sof(O50)=Sof(O51)=Sof(O52)=Sof(O53)=Sof(H53)=Sof(C50)=Sof(C51)=
 Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53A)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(C56)=
 Sof(H56)=Sof(C57)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(C61)=
 Sof(C62)=Sof(C63)=Sof(C64)=Sof(H64)=Sof(C65)=Sof(C66)=Sof(H66)=Sof(C67)=
 Sof(H67)=Sof(C68)=Sof(H68)=Sof(C69)=Sof(O1E)=Sof(N1E)=Sof(C1E)=Sof(H1E)=
 Sof(C2E)=Sof(H2EA)=Sof(H2EB)=Sof(C3E)=Sof(H3EA)=Sof(H3EB)=Sof(H3EC)=Sof(C4E)=
 Sof(H4EA)=Sof(H4EB)=Sof(C5E)=Sof(H5EA)=Sof(H5EB)=Sof(H5EC)=FVAR(2)
 Sof(H51A)=Sof(O50A)=Sof(O51A)=Sof(O52A)=Sof(H52A)=Sof(O53A)=Sof(C50A)=
 Sof(C51A)=Sof(C52A)=Sof(H52B)=Sof(C53A)=Sof(H53B)=Sof(C54A)=Sof(H54A)=
 Sof(C55A)=Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(C58A)=Sof(H58A)=Sof(C59A)=
 Sof(H59A)=Sof(C60A)=Sof(C61A)=Sof(C62A)=Sof(C63A)=Sof(C64A)=Sof(H64A)=
 Sof(C65A)=Sof(C66A)=Sof(H66A)=Sof(C67A)=Sof(H67A)=Sof(C68A)=Sof(H68A)=
 Sof(C69A)=FVAR(3)
 Sof(H51B)=Sof(O50B)=Sof(O51B)=Sof(O52B)=Sof(O53B)=Sof(H53C)=Sof(C50B)=
 Sof(C51B)=Sof(C52B)=Sof(H52C)=Sof(C53B)=Sof(H53D)=Sof(C54B)=Sof(H54B)=
 Sof(C55B)=Sof(C56B)=Sof(H56B)=Sof(C57B)=Sof(C58B)=Sof(H58B)=Sof(C59B)=
 Sof(H59B)=Sof(C60B)=Sof(C61B)=Sof(C62B)=Sof(C63B)=Sof(C64B)=Sof(H64B)=
 Sof(C65B)=Sof(C66B)=Sof(H66B)=Sof(C67B)=Sof(H67B)=Sof(C68B)=Sof(H68B)=
 Sof(C69B)=Sof(O1D)=Sof(N1D)=Sof(C1D)=Sof(H1D)=Sof(C2D)=Sof(H2DA)=Sof(H2DB)=
 Sof(C3D)=Sof(H3DA)=Sof(H3DB)=Sof(H3DC)=Sof(C4D)=Sof(H4DA)=Sof(H4DB)=Sof(C5D)=
 Sof(H5DA)=Sof(H5DB)=Sof(H5DC)=FVAR(4)
 Fixed Sof: Cu1(0.5)
 Fixed X: H0AA(0.05464) H0AB(0.07598)
 Fixed Y: H0AA(0.50368) H0AB(0.53537)
 Fixed Z: H0AA(-0.273) H0AB(-0.195411)
8.a Riding coordinates:
 O53(H53), O52A(H52A), C3E(H3EA,H3EB,H3EC), C5E(H5EA,H5EB,H5EC), C3D(H3DA,H3DB,
 H3DC)
8.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C2E(H2EA,H2EB), C4E(H4EA,H4EB), C2D(H2DA,H2DB), C4D(H4DA,H4DB)
8.c Aromatic/amide H refined with riding coordinates:
 N51(H51), N51(H51A), N51(H51B), C52(H52), C53(H53A), C54(H54), C56(H56),
 C58(H58), C59(H59), C64(H64), C66(H66), C67(H67), C68(H68), C72(H72), C73(H73),
  C52A(H52B), C53A(H53B), C54A(H54A), C56A(H56A), C58A(H58A), C59A(H59A),
 C64A(H64A), C66A(H66A), C67A(H67A), C68A(H68A), C52B(H52C), C53B(H53D),
 C54B(H54B), C56B(H56B), C58B(H58B), C59B(H59B), C64B(H64B), C66B(H66B),
 C67B(H67B), C68B(H68B), C3(H3), C5(H5), C7(H7), C21(H21), C22(H22), C23(H23),
 C24(H24), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C1E(H1E), C1D(H1D)
8.d Idealised Me refined as rotating group:
 C5D(H5DA,H5DB,H5DC)
8.e Idealised tetrahedral OH refined as rotating group:
 O53B(H53C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N50 N 0.1692(2) 0.5369(4) -0.0999(3) 0.0809(13) Uani 1 1 d D . . . .
N51 N 0.2171(2) 0.4598(3) 0.0116(2) 0.0685(11) Uani 1 1 d D . . . .
H51 H 0.217942 0.431080 0.056338 0.082 Uiso 0.240(3) 1 calc R . P A 1
H51A H 0.217817 0.422574 0.052075 0.082 Uiso 0.228(3) 1 calc R . P A 2
H51B H 0.218138 0.433887 0.057468 0.082 Uiso 0.532(3) 1 calc R . P A 3
C70 C 0.1530(3) 0.4981(3) -0.0384(3) 0.0683(14) Uani 1 1 d D . . . .
O50 O 0.1034(17) 0.6655(19) -0.4589(13) 0.071(7) Uani 0.240(3) 1 d D U P A 1
O51 O 0.076(3) 0.550(4) -0.383(2) 0.080(5) Uani 0.240(3) 1 d D U P A 1
O52 O 0.4014(14) 0.1421(15) 0.1481(13) 0.129(7) Uani 0.240(3) 1 d D U P A 1
O53 O 0.505(2) 0.150(2) 0.240(2) 0.172(17) Uani 0.240(3) 1 d D U P A 1
H53 H 0.509552 0.092046 0.228916 0.258 Uiso 0.240(3) 1 d R . P A 1
C50 C 0.1190(16) 0.618(2) -0.3997(14) 0.082(4) Uani 0.240(3) 1 d D U P A 1
C51 C 0.1921(14) 0.6383(19) -0.3401(12) 0.101(7) Uani 0.240(3) 1 d D U P A 1
C52 C 0.2421(17) 0.709(2) -0.3531(15) 0.108(7) Uani 0.240(3) 1 d D U P A 1
H52 H 0.228385 0.745691 -0.399565 0.130 Uiso 0.240(3) 1 calc R . P A 1
C53 C 0.3141(19) 0.727(3) -0.2979(19) 0.131(8) Uani 0.240(3) 1 d D U P A 1
H53A H 0.350013 0.774702 -0.307221 0.157 Uiso 0.240(3) 1 calc R . P A 1
C54 C 0.3308(19) 0.674(3) -0.2297(17) 0.123(3) Uani 0.240(3) 1 d D U P A 1
H54 H 0.380766 0.681760 -0.193799 0.148 Uiso 0.240(3) 1 calc R . P A 1
C55 C 0.2777(14) 0.609(2) -0.2122(11) 0.104(3) Uani 0.240(3) 1 d D U P A 1
C56 C 0.211(2) 0.583(3) -0.2720(18) 0.095(7) Uani 0.240(3) 1 d D U P A 1
H56 H 0.180397 0.528628 -0.266235 0.114 Uiso 0.240(3) 1 calc R . P A 1
C57 C 0.3022(9) 0.548(3) -0.1407(13) 0.098(8) Uani 0.240(3) 1 d D U P A 1
C58 C 0.3835(10) 0.529(3) -0.1128(14) 0.089(7) Uani 0.240(3) 1 d D U P A 1
H58 H 0.420070 0.551474 -0.141918 0.107 Uiso 0.240(3) 1 calc R . P A 1
C59 C 0.4115(10) 0.481(3) -0.0452(14) 0.085(7) Uani 0.240(3) 1 d D U P A 1
H59 H 0.466853 0.467008 -0.030261 0.102 Uiso 0.240(3) 1 calc R . P A 1
C60 C 0.3621(8) 0.451(2) 0.0035(12) 0.087(9) Uani 0.240(3) 1 d D U P A 1
C61 C 0.2806(9) 0.475(4) -0.0223(19) 0.089(9) Uani 0.240(3) 1 d D U P A 1
C62 C 0.2512(10) 0.524(4) -0.0914(19) 0.090(9) Uani 0.240(3) 1 d D U P A 1
C63 C 0.3951(15) 0.4109(19) 0.0834(11) 0.078(8) Uani 0.240(3) 1 d D U P A 1
C64 C 0.4123(18) 0.3164(17) 0.0993(13) 0.080(8) Uani 0.240(3) 1 d D U P A 1
H64 H 0.397606 0.270313 0.058993 0.096 Uiso 0.240(3) 1 calc R . P A 1
C65 C 0.452(2) 0.2875(15) 0.1763(15) 0.084(8) Uani 0.240(3) 1 d D U P A 1
C66 C 0.477(2) 0.3545(19) 0.2311(15) 0.092(8) Uani 0.240(3) 1 d D U P A 1
H66 H 0.511128 0.336239 0.279301 0.110 Uiso 0.240(3) 1 calc R . P A 1
C67 C 0.455(2) 0.4462(19) 0.2209(14) 0.099(7) Uani 0.240(3) 1 d D U P A 1
H67 H 0.467786 0.490079 0.263021 0.119 Uiso 0.240(3) 1 calc R . P A 1
C68 C 0.412(2) 0.4760(19) 0.1453(14) 0.089(7) Uani 0.240(3) 1 d D U P A 1
H68 H 0.395584 0.540352 0.136884 0.106 Uiso 0.240(3) 1 calc R . P A 1
C69 C 0.4531(17) 0.1896(18) 0.1877(15) 0.127(10) Uani 0.240(3) 1 d D U P A 1
C71 C 0.0736(3) 0.4976(4) -0.0191(3) 0.0618(13) Uani 1 1 d . . . . .
C72 C 0.0223(3) 0.5723(4) -0.0433(3) 0.0659(13) Uani 1 1 d . . . . .
H72 H 0.037417 0.622332 -0.073259 0.079 Uiso 1 1 calc R . . . .
C73 C 0.0510(3) 0.4252(4) 0.0241(3) 0.0685(13) Uani 1 1 d . . . . .
H73 H 0.086033 0.373285 0.040821 0.082 Uiso 1 1 calc R . . . .
O50A O 0.123(2) 0.642(3) -0.4638(13) 0.112(13) Uani 0.228(3) 1 d D U P A 2
O51A O 0.085(3) 0.544(4) -0.380(2) 0.080(5) Uani 0.228(3) 1 d D U P A 2
O52A O 0.378(2) 0.552(3) 0.309(3) 0.34(3) Uani 0.228(3) 1 d D U P A 2
H52A H 0.378051 0.566096 0.355855 0.517 Uiso 0.228(3) 1 d R . P A 2
O53A O 0.497(3) 0.509(3) 0.358(2) 0.29(3) Uani 0.228(3) 1 d D U P A 2
C50A C 0.1271(17) 0.612(3) -0.3983(15) 0.082(4) Uani 0.228(3) 1 d D U P A 2
C51A C 0.1873(14) 0.652(2) -0.3331(11) 0.101(7) Uani 0.228(3) 1 d D U P A 2
C52A C 0.219(2) 0.739(2) -0.3436(15) 0.124(9) Uani 0.228(3) 1 d D U P A 2
H52B H 0.200821 0.771823 -0.391641 0.148 Uiso 0.228(3) 1 calc R . P A 2
C53A C 0.278(2) 0.780(2) -0.2842(16) 0.130(8) Uani 0.228(3) 1 d D U P A 2
H53B H 0.301082 0.840084 -0.291399 0.156 Uiso 0.228(3) 1 calc R . P A 2
C54A C 0.3018(17) 0.730(2) -0.2148(13) 0.123(3) Uani 0.228(3) 1 d D U P A 2
H54A H 0.343296 0.755654 -0.174902 0.148 Uiso 0.228(3) 1 calc R . P A 2
C55A C 0.2683(15) 0.645(2) -0.2007(11) 0.104(3) Uani 0.228(3) 1 d D U P A 2
C56A C 0.212(2) 0.602(3) -0.2624(14) 0.101(8) Uani 0.228(3) 1 d D U P A 2
H56A H 0.191242 0.541034 -0.256136 0.121 Uiso 0.228(3) 1 calc R . P A 2
C57A C 0.2992(9) 0.594(2) -0.1251(11) 0.092(7) Uani 0.228(3) 1 d D U P A 2
C58A C 0.3788(11) 0.6015(18) -0.0880(11) 0.107(7) Uani 0.228(3) 1 d D U P A 2
H58A H 0.412971 0.638816 -0.111520 0.128 Uiso 0.228(3) 1 calc R . P A 2
C59A C 0.4100(10) 0.5568(19) -0.0186(12) 0.101(7) Uani 0.228(3) 1 d D U P A 2
H59A H 0.464713 0.565884 0.005337 0.121 Uiso 0.228(3) 1 calc R . P A 2
C60A C 0.3639(8) 0.497(2) 0.0189(11) 0.096(7) Uani 0.228(3) 1 d D U P A 2
C61A C 0.2821(6) 0.493(3) -0.0164(18) 0.095(9) Uani 0.228(3) 1 d D U P A 2
C62A C 0.2509(7) 0.537(3) -0.0876(16) 0.089(9) Uani 0.228(3) 1 d D U P A 2
C63A C 0.3988(14) 0.4501(17) 0.0956(10) 0.079(7) Uani 0.228(3) 1 d D U P A 2
C64A C 0.4070(18) 0.4976(18) 0.1659(12) 0.120(9) Uani 0.228(3) 1 d D U P A 2
H64A H 0.397130 0.564050 0.166025 0.144 Uiso 0.228(3) 1 calc R . P A 2
C65A C 0.430(2) 0.448(2) 0.2380(13) 0.119(9) Uani 0.228(3) 1 d D U P A 2
C66A C 0.446(3) 0.354(2) 0.2367(14) 0.093(8) Uani 0.228(3) 1 d D U P A 2
H66A H 0.463885 0.322195 0.285230 0.111 Uiso 0.228(3) 1 calc R . P A 2
C67A C 0.437(2) 0.3037(19) 0.1705(17) 0.091(7) Uani 0.228(3) 1 d D U P A 2
H67A H 0.449181 0.237640 0.172016 0.109 Uiso 0.228(3) 1 calc R . P A 2
C68A C 0.410(3) 0.3519(18) 0.0973(15) 0.085(8) Uani 0.228(3) 1 d D U P A 2
H68A H 0.399527 0.316753 0.049784 0.102 Uiso 0.228(3) 1 calc R . P A 2
C69A C 0.434(2) 0.504(2) 0.3041(15) 0.157(11) Uani 0.228(3) 1 d D U P A 2
O50B O 0.0776(6) 0.6038(8) -0.4650(4) 0.088(2) Uani 0.532(3) 1 d D U P A 3
O51B O 0.0553(6) 0.5073(10) -0.3750(8) 0.128(5) Uani 0.532(3) 1 d D U P A 3
O52B O 0.4865(8) 0.1239(7) 0.1313(5) 0.139(4) Uani 0.532(3) 1 d D U P A 3
O53B O 0.5183(11) 0.1551(9) 0.2536(7) 0.117(5) Uani 0.532(3) 1 d D U P A 3
H53C H 0.529266 0.096813 0.255766 0.175 Uiso 0.532(3) 1 calc GR . P A 3
C50B C 0.0954(12) 0.5723(14) -0.3982(9) 0.080(5) Uani 0.532(3) 1 d D U P A 3
C51B C 0.1681(7) 0.6049(11) -0.3433(6) 0.087(4) Uani 0.532(3) 1 d D U P A 3
C52B C 0.2070(9) 0.6823(13) -0.3620(9) 0.105(5) Uani 0.532(3) 1 d D U P A 3
H52C H 0.185475 0.716544 -0.408711 0.126 Uiso 0.532(3) 1 calc R . P A 3
C53B C 0.2797(12) 0.7123(15) -0.3122(9) 0.133(5) Uani 0.532(3) 1 d D U P A 3
H53D H 0.308864 0.764187 -0.326268 0.160 Uiso 0.532(3) 1 calc R . P A 3
C54B C 0.3074(9) 0.6636(14) -0.2417(9) 0.123(3) Uani 0.532(3) 1 d D U P A 3
H54B H 0.353928 0.686248 -0.206304 0.148 Uiso 0.532(3) 1 calc R . P A 3
C55B C 0.2702(8) 0.5848(12) -0.2218(6) 0.104(3) Uani 0.532(3) 1 d D U P A 3
C56B C 0.1959(10) 0.5586(15) -0.2714(9) 0.096(4) Uani 0.532(3) 1 d D U P A 3
H56B H 0.165017 0.509575 -0.255726 0.115 Uiso 0.532(3) 1 calc R . P A 3
C57B C 0.2997(6) 0.5326(14) -0.1463(7) 0.104(5) Uani 0.532(3) 1 d D U P A 3
C58B C 0.3771(7) 0.4966(11) -0.1249(8) 0.108(6) Uani 0.532(3) 1 d D U P A 3
H58B H 0.411815 0.505555 -0.159302 0.130 Uiso 0.532(3) 1 calc R . P A 3
C59B C 0.4045(7) 0.4491(12) -0.0566(8) 0.108(6) Uani 0.532(3) 1 d D U P A 3
H59B H 0.456848 0.423615 -0.046691 0.129 Uiso 0.532(3) 1 calc R . P A 3
C60B C 0.3599(6) 0.4355(13) 0.0001(7) 0.084(4) Uani 0.532(3) 1 d D U P A 3
C61B C 0.2799(6) 0.469(2) -0.0235(10) 0.084(5) Uani 0.532(3) 1 d D U P A 3
C62B C 0.2501(6) 0.515(2) -0.0941(10) 0.088(5) Uani 0.532(3) 1 d D U P A 3
C63B C 0.3927(8) 0.3924(11) 0.0786(7) 0.077(4) Uani 0.532(3) 1 d D U P A 3
C64B C 0.4297(7) 0.3036(10) 0.0927(9) 0.083(4) Uani 0.532(3) 1 d D U P A 3
H64B H 0.433894 0.263988 0.049948 0.099 Uiso 0.532(3) 1 calc R . P A 3
C65B C 0.4608(9) 0.2727(10) 0.1700(9) 0.077(4) Uani 0.532(3) 1 d D U P A 3
C66B C 0.4579(15) 0.3316(15) 0.2307(9) 0.095(5) Uani 0.532(3) 1 d D U P A 3
H66B H 0.484594 0.313067 0.282109 0.114 Uiso 0.532(3) 1 calc R . P A 3
C67B C 0.4189(10) 0.4143(12) 0.2211(9) 0.099(4) Uani 0.532(3) 1 d D U P A 3
H67B H 0.413657 0.451072 0.265014 0.119 Uiso 0.532(3) 1 calc R . P A 3
C68B C 0.3856(8) 0.4463(11) 0.1442(9) 0.089(4) Uani 0.532(3) 1 d D U P A 3
H68B H 0.357974 0.505249 0.136647 0.107 Uiso 0.532(3) 1 calc R . P A 3
C69B C 0.4895(8) 0.1791(11) 0.1823(7) 0.101(4) Uani 0.532(3) 1 d D U P A 3
H0AA H 0.054640 0.503680 -0.273000 0.152 Uiso 1 1 d R . . . .
O1 O 0.2119(2) 0.5459(3) 0.1825(2) 0.0826(11) Uani 1 1 d . . . . .
O2 O 0.0077(2) 0.7681(3) 0.0769(2) 0.0904(12) Uani 1 1 d . . . . .
O3 O -0.1314(2) 0.7956(3) -0.0558(3) 0.0971(13) Uani 1 1 d . . . . .
O4 O -0.2042(2) 0.6508(3) -0.1569(2) 0.0791(11) Uani 1 1 d . . . . .
C1 C 0.1605(4) 0.4876(4) 0.2130(3) 0.0829(16) Uani 1 1 d . . . . .
H1A H 0.108746 0.480841 0.174816 0.099 Uiso 1 1 calc R . . . .
H1B H 0.150785 0.515365 0.261814 0.099 Uiso 1 1 calc R . . . .
C2 C 0.1844(3) 0.6285(4) 0.1458(3) 0.0712(14) Uani 1 1 d . . . . .
C3 C 0.1065(3) 0.6605(4) 0.1330(3) 0.0760(14) Uani 1 1 d . . . . .
H3 H 0.067525 0.625855 0.151946 0.091 Uiso 1 1 calc R . . . .
C4 C 0.0867(3) 0.7459(4) 0.0911(3) 0.0753(15) Uani 1 1 d . . . . .
C5 C 0.1438(4) 0.7987(4) 0.0677(3) 0.0802(16) Uani 1 1 d . . . . .
H5 H 0.129979 0.857300 0.041087 0.096 Uiso 1 1 calc R . . . .
C6 C 0.2221(4) 0.7665(4) 0.0830(3) 0.0840(16) Uani 1 1 d . . . . .
C7 C 0.2420(4) 0.6809(4) 0.1212(3) 0.0761(15) Uani 1 1 d . . . . .
H7 H 0.295175 0.658028 0.130587 0.091 Uiso 1 1 calc R . . . .
C8 C -0.0168(4) 0.8548(5) 0.0351(5) 0.108(2) Uani 1 1 d . . . . .
H8A H 0.006268 0.858894 -0.011488 0.129 Uiso 1 1 calc R . . . .
H8B H 0.001833 0.910335 0.069146 0.129 Uiso 1 1 calc R . . . .
C9 C -0.1050(4) 0.8542(5) 0.0111(4) 0.107(2) Uani 1 1 d . . . . .
H9A H -0.127177 0.830141 0.054721 0.128 Uiso 1 1 calc R . . . .
H9B H -0.124726 0.919920 -0.000982 0.128 Uiso 1 1 calc R . . . .
C10 C -0.2143(3) 0.7911(4) -0.0855(4) 0.0910(18) Uani 1 1 d . . . . .
H10A H -0.237519 0.855837 -0.089466 0.109 Uiso 1 1 calc R . . . .
H10B H -0.239326 0.752759 -0.050316 0.109 Uiso 1 1 calc R . . . .
C11 C -0.2289(4) 0.7455(4) -0.1656(4) 0.0890(18) Uani 1 1 d . . . . .
H11A H -0.286319 0.748623 -0.191349 0.107 Uiso 1 1 calc R . . . .
H11B H -0.198790 0.779827 -0.198746 0.107 Uiso 1 1 calc R . . . .
C12 C -0.2008(4) 0.6077(4) -0.2293(3) 0.0877(17) Uani 1 1 d . . . . .
H12A H -0.170444 0.648744 -0.257984 0.105 Uiso 1 1 calc R . . . .
H12B H -0.255272 0.599408 -0.262111 0.105 Uiso 1 1 calc R . . . .
N20 N 0.4091(6) 0.9116(8) -0.0038(8) 0.080(4) Uani 0.493(16) 1 d D U P B 1
C20 C 0.2883(11) 0.8193(15) 0.0478(15) 0.080(6) Uani 0.493(16) 1 d D U P B 1
C21 C 0.3405(10) 0.7704(11) 0.0097(11) 0.097(5) Uani 0.493(16) 1 d D U P B 1
H21 H 0.334837 0.704013 -0.000386 0.116 Uiso 0.493(16) 1 calc R . P B 1
C22 C 0.3996(8) 0.8219(8) -0.0121(10) 0.089(4) Uani 0.493(16) 1 d D U P B 1
H22 H 0.436151 0.788161 -0.035194 0.106 Uiso 0.493(16) 1 calc R . P B 1
C23 C 0.3589(12) 0.9595(12) 0.0349(13) 0.093(6) Uani 0.493(16) 1 d D U P B 1
H23 H 0.367960 1.025435 0.044962 0.111 Uiso 0.493(16) 1 calc R . P B 1
C24 C 0.2970(14) 0.9172(13) 0.0594(19) 0.087(6) Uani 0.493(16) 1 d D U P B 1
H24 H 0.262063 0.952836 0.083096 0.104 Uiso 0.493(16) 1 calc R . P B 1
N20A N 0.4125(6) 0.9346(8) 0.0472(10) 0.080(4) Uani 0.507(16) 1 d D U P B 2
C20A C 0.2835(11) 0.8255(13) 0.0672(16) 0.075(5) Uani 0.507(16) 1 d D U P B 2
C21A C 0.3536(10) 0.7853(9) 0.0524(12) 0.091(5) Uani 0.507(16) 1 d D U P B 2
H21A H 0.358618 0.718324 0.047736 0.109 Uiso 0.507(16) 1 calc R . P B 2
C22A C 0.4146(8) 0.8450(9) 0.0449(11) 0.089(4) Uani 0.507(16) 1 d D U P B 2
H22A H 0.462198 0.816450 0.037450 0.107 Uiso 0.507(16) 1 calc R . P B 2
C23A C 0.3429(13) 0.9752(12) 0.0617(14) 0.104(6) Uani 0.507(16) 1 d D U P B 2
H23A H 0.340592 1.042569 0.064761 0.124 Uiso 0.507(16) 1 calc R . P B 2
C24A C 0.2780(14) 0.9246(15) 0.072(2) 0.094(6) Uani 0.507(16) 1 d D U P B 2
H24A H 0.232006 0.955040 0.081423 0.113 Uiso 0.507(16) 1 calc R . P B 2
O1E O 0.645(3) 0.556(3) 0.356(3) 0.29(2) Uani 0.240(3) 1 d D U P A 1
N1E N 0.584(3) 0.697(3) 0.326(3) 0.30(2) Uani 0.240(3) 1 d D U P A 1
C1E C 0.583(3) 0.599(3) 0.330(3) 0.30(3) Uani 0.240(3) 1 d D U P A 1
H1E H 0.533954 0.565635 0.313664 0.363 Uiso 0.240(3) 1 calc R . P A 1
C2E C 0.656(3) 0.732(3) 0.351(4) 0.28(2) Uani 0.240(3) 1 d D U P A 1
H2EA H 0.661201 0.778422 0.309919 0.338 Uiso 0.240(3) 1 calc R . P A 1
H2EB H 0.651608 0.771078 0.396798 0.338 Uiso 0.240(3) 1 calc R . P A 1
C3E C 0.727(3) 0.694(3) 0.372(4) 0.27(2) Uani 0.240(3) 1 d D U P A 1
H3EA H 0.736213 0.678496 0.427598 0.404 Uiso 0.240(3) 1 d R . P A 1
H3EB H 0.766433 0.740576 0.363658 0.404 Uiso 0.240(3) 1 d R . P A 1
H3EC H 0.730673 0.636436 0.341808 0.404 Uiso 0.240(3) 1 d R . P A 1
C4E C 0.519(3) 0.748(4) 0.298(4) 0.29(2) Uani 0.240(3) 1 d D U P A 1
H4EA H 0.534025 0.815643 0.303089 0.345 Uiso 0.240(3) 1 calc R . P A 1
H4EB H 0.500545 0.733398 0.241877 0.345 Uiso 0.240(3) 1 calc R . P A 1
C5E C 0.459(3) 0.736(4) 0.331(4) 0.30(3) Uani 0.240(3) 1 d D U P A 1
H5EA H 0.427456 0.794372 0.323608 0.446 Uiso 0.240(3) 1 d R . P A 1
H5EB H 0.480406 0.724452 0.386688 0.446 Uiso 0.240(3) 1 d R . P A 1
H5EC H 0.425076 0.682082 0.308148 0.446 Uiso 0.240(3) 1 d R . P A 1
O1D O 0.5522(14) 0.5564(9) 0.3897(9) 0.210(8) Uani 0.532(3) 1 d D U P A 3
N1D N 0.5588(11) 0.6768(13) 0.3073(10) 0.168(6) Uani 0.532(3) 1 d D U P A 3
C1D C 0.5205(13) 0.6292(14) 0.3560(11) 0.186(7) Uani 0.532(3) 1 d D U P A 3
H1D H 0.470756 0.651120 0.363789 0.224 Uiso 0.532(3) 1 calc R . P A 3
C2D C 0.6291(15) 0.6356(14) 0.3061(11) 0.152(6) Uani 0.532(3) 1 d D U P A 3
H2DA H 0.617328 0.566652 0.306533 0.183 Uiso 0.532(3) 1 calc R . P A 3
H2DB H 0.635760 0.649024 0.252575 0.183 Uiso 0.532(3) 1 calc R . P A 3
C3D C 0.7002(16) 0.6419(18) 0.348(2) 0.244(15) Uani 0.532(3) 1 d D U P A 3
H3DA H 0.696104 0.686141 0.390490 0.366 Uiso 0.532(3) 1 d R . P A 3
H3DB H 0.738284 0.666841 0.319710 0.366 Uiso 0.532(3) 1 d R . P A 3
H3DC H 0.718604 0.579811 0.370990 0.366 Uiso 0.532(3) 1 d R . P A 3
C4D C 0.5324(12) 0.7522(16) 0.2665(13) 0.159(7) Uani 0.532(3) 1 d D U P A 3
H4DA H 0.496370 0.785620 0.294064 0.191 Uiso 0.532(3) 1 calc R . P A 3
H4DB H 0.578647 0.794654 0.268283 0.191 Uiso 0.532(3) 1 calc R . P A 3
C5D C 0.4952(14) 0.7446(17) 0.1939(12) 0.187(8) Uani 0.532(3) 1 d D U P A 3
H5DA H 0.481154 0.808132 0.171987 0.280 Uiso 0.532(3) 1 calc GR . P A 3
H5DB H 0.446547 0.707127 0.190205 0.280 Uiso 0.532(3) 1 calc GR . P A 3
H5DC H 0.529634 0.712836 0.164430 0.280 Uiso 0.532(3) 1 calc GR . P A 3
O0AA O 0.0349(4) 0.5181(6) -0.2321(3) 0.160(3) Uani 1 1 d . . . . .
Cu1 Cu 0.50289(10) 0.01782(11) 0.03412(9) 0.0807(6) Uani 0.5 1 d . . P C -1
H0AB H 0.075980 0.535370 -0.195411 0.097 Uiso 1 1 d R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N50 C70 1.297(6) . ?
N50 C62 1.398(12) . ?
O52Ab H52A 0.8399 . ?
O51Ab C50A 1.28(2) . ?
O50Ab C50A 1.216(19) . ?
C50Ab C51A 1.47(2) . ?
C51Ab C52A 1.37(2) . ?
C52Ab H52B 0.9500 . ?
C52Ab C53A 1.41(2) . ?
C53Ab H53B 0.9500 . ?
C53Ab C54A 1.39(2) . ?
C54Ab H54A 0.9500 . ?
C54Ab C55A 1.369(19) . ?
C51Ab C56A 1.401(17) . ?
C55Ab C56A 1.414(18) . ?
C56Ab H56A 0.9500 . ?
C55Ab C57A 1.495(15) . ?
C57Ab C58A 1.382(16) . ?
C58Ab H58A 0.9500 . ?
C58Ab C59A 1.367(18) . ?
C59Ab H59A 0.9500 . ?
C59Ab C60A 1.415(18) . ?
C60Ab C61A 1.406(15) . ?
C57Ab C62A 1.419(16) . ?
N50 C62A 1.375(12) . ?
C61Ab C62A 1.388(14) . ?
C60Ab C63A 1.499(15) . ?
C63Ab C64A 1.381(19) . ?
C64Ab H64A 0.9500 . ?
C64Ab C65A 1.42(2) . ?
C65Ab C66A 1.34(2) . ?
C66Ab H66A 0.9500 . ?
C66Ab C67A 1.34(2) . ?
C67Ab H67A 0.9500 . ?
C63Ab C68A 1.39(2) . ?
C67Ab C68A 1.43(2) . ?
C68Ab H68A 0.9500 . ?
O53Ab C69A 1.27(2) . ?
O52Ab C69A 1.19(2) . ?
C65Ab C69A 1.40(2) . ?
O53Bc H53C 0.8400 . ?
O51Bc C50B 1.27(2) . ?
O50Bc C50B 1.226(18) . ?
C50Bc C51B 1.47(2) . ?
C51Bc C52B 1.357(18) . ?
C52Bc H52C 0.9500 . ?
C52Bc C53B 1.418(18) . ?
C53Bc H53D 0.9500 . ?
C53Bc C54B 1.398(17) . ?
C54Bc H54B 0.9500 . ?
C54Bc C55B 1.364(15) . ?
C55Bc C56B 1.422(14) . ?
C51Bc C56B 1.403(13) . ?
C56Bc H56B 0.9500 . ?
C55Bc C57B 1.498(13) . ?
C57Bc C58B 1.397(13) . ?
C58Bc H58B 0.9500 . ?
C58Bc C59B 1.359(14) . ?
C59Bc H59B 0.9500 . ?
C59Bc C60B 1.403(14) . ?
C60Bc C61B 1.428(11) . ?
C57Bc C62B 1.412(12) . ?
C61Bc C62B 1.382(11) . ?
N50 C62B 1.410(10) . ?
C60Bc C63B 1.493(13) . ?
C63Bc C64B 1.398(15) . ?
C64Bc H64B 0.9500 . ?
C64Bc C65B 1.410(15) . ?
C65Bc C66B 1.360(18) . ?
C66Bc H66B 0.9500 . ?
C66Bc C67B 1.334(18) . ?
C67Bc H67B 0.9500 . ?
C63Bc C68B 1.406(16) . ?
C67Bc C68B 1.413(17) . ?
C68Bc H68B 0.9500 . ?
O53Bc C69B 1.282(16) . ?
O52Bc C69B 1.177(14) . ?
C65Bc C69B 1.403(18) . ?
C20Ab C21A 1.412(15) . ?
C21Ab H21A 0.9500 . ?
C21Ab C22A 1.375(14) . ?
N20Ab C22A 1.260(13) . ?
C22Ab H22A 0.9500 . ?
N20Ab C23A 1.40(2) . ?
C23Ab H23A 0.9500 . ?
C20Ab C24A 1.400(15) . ?
C23Ab C24A 1.371(18) . ?
C24Ab H24A 0.9500 . ?
N1Ea C1E 1.376(16) . ?
O1Ea C1E 1.223(17) . ?
C1Ea H1E 0.9500 . ?
N1Ea C2E 1.32(2) . ?
C2Ea H2EA 0.9900 . ?
C2Ea H2EB 0.9900 . ?
C2Ea C3E 1.30(2) . ?
C3Ea H3EA 0.9798 . ?
C3Ea H3EB 0.9798 . ?
C3Ea H3EC 0.9801 . ?
N1Ea C4E 1.32(2) . ?
C4Ea H4EA 0.9900 . ?
C4Ea H4EB 0.9900 . ?
C4Ea C5E 1.30(2) . ?
C5Ea H5EA 0.9801 . ?
C5Ea H5EB 0.9800 . ?
C5Ea H5EC 0.9803 . ?
O1Dc C1D 1.243(15) . ?
N1Dc C1D 1.369(15) . ?
C1Dc H1D 0.9500 . ?
N1Dc C2D 1.348(19) . ?
C2Dc H2DA 0.9900 . ?
C2Dc H2DB 0.9900 . ?
C2Dc C3D 1.28(2) . ?
C3Dc H3DA 0.9800 . ?
C3Dc H3DB 0.9801 . ?
C3Dc H3DC 0.9802 . ?
N1Dc C4D 1.302(18) . ?
C4Dc H4DA 0.9900 . ?
C4Dc H4DB 0.9900 . ?
C4Dc C5D 1.29(2) . ?
C5Dc H5DA 0.9800 . ?
C5Dc H5DB 0.9800 . ?
C5Dc H5DC 0.9800 . ?
N51 H51 0.8800 . ?
N51 H51A 0.8800 . ?
N51 H51B 0.8800 . ?
N51 C70 1.354(6) . ?
N51 C61 1.379(13) . ?
N51 C61A 1.406(13) . ?
N51 C61B 1.371(10) . ?
C70 C71 1.484(7) . ?
C71 C72 1.375(7) . ?
C71 C73 1.377(7) . ?
C72 H72 0.9500 . ?
C72 C73 1.381(7) 3_565 ?
C73 C72 1.381(7) 3_565 ?
C73 H73 0.9500 . ?
O50A C50 1.209(19) . ?
O51A C50 1.29(2) . ?
O52A C69 1.198(19) . ?
O53A H53 0.8402 . ?
O53A C69 1.26(2) . ?
C50A C51 1.47(2) . ?
C51A C52 1.37(2) . ?
C51A C56 1.402(17) . ?
C52A H52 0.9500 . ?
C52A C53 1.41(2) . ?
C53A H53A 0.9500 . ?
C53A C54 1.39(2) . ?
C54A H54 0.9500 . ?
C54A C55 1.372(18) . ?
C55A C56 1.412(17) . ?
C55A C57 1.501(15) . ?
C56A H56 0.9500 . ?
C57A C58 1.399(16) . ?
C57A C62 1.407(15) . ?
C58A H58 0.9500 . ?
C58A C59 1.356(17) . ?
C59A H59 0.9500 . ?
C59A C60 1.405(17) . ?
C60A C61 1.417(13) . ?
C60A C63 1.496(15) . ?
C61A C62 1.386(14) . ?
C63A C64 1.375(18) . ?
C63A C68 1.399(19) . ?
C64A H64 0.9500 . ?
C64A C65 1.428(19) . ?
C65A C66 1.34(2) . ?
C65A C69 1.39(2) . ?
C66A H66 0.9500 . ?
C66A C67 1.34(2) . ?
C67A H67 0.9500 . ?
C67A C68 1.42(2) . ?
C68A H68 0.9500 . ?
O1 C1 1.401(7) . ?
O1 C2 1.358(6) . ?
O2 C4 1.365(6) . ?
O2 C8 1.434(7) . ?
O3 C9 1.422(7) . ?
O3 C10 1.406(7) . ?
O4 C11 1.395(6) . ?
O4 C12 1.422(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C12 1.505(8) 3_565 ?
C2 C3 1.386(8) . ?
C2 C7 1.381(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.408(7) . ?
C4 C5 1.368(8) . ?
C5 H5 0.9500 . ?
C5 C6 1.390(8) . ?
C6 C7 1.383(8) . ?
C6 C20 1.599(17) . ?
C6 C20A 1.421(15) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.484(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.514(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C1 1.505(8) 3_565 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N20A C22 1.275(13) . ?
N20A C23 1.39(2) . ?
C20A C21 1.416(16) . ?
C20A C24 1.395(15) . ?
C21A H21 0.9500 . ?
C21A C22 1.375(15) . ?
C22A H22 0.9500 . ?
C23A H23 0.9500 . ?
C23A C24 1.374(18) . ?
C24A H24 0.9500 . ?
O0AA H0AA 0.886(6) . ?
O0AA H0AB 0.875(5) . ?

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
C70 N50 C62 105.3(6) . . ?
C70 N50 C62A 106.3(6) . . ?
C70 N50 C62B 104.2(5) . . ?
C70 N51 H51 127.2 . . ?
C70 N51 H51A 128.1 . . ?
C70 N51 H51B 126.8 . . ?
C70 N51 C61 105.6(6) . . ?
C70 N51 C61A 103.7(6) . . ?
C70 N51 C61B 106.3(5) . . ?
C61A N51 H51 127.2 . . ?
N50 C70 N51 114.0(4) . . ?
N50 C70 C71 125.3(4) . . ?
N51 C70 C71 120.6(4) . . ?
C61Bc C62Bc N50 109.0(7) . . ?
C62Ab C61Ab N51 106.9(8) . . ?
O50Ab C50Ab O51A 126(2) . . ?
C69Ab O52Ab H52A 112.5 . . ?
O52Ab C69Ab O53A 119(2) . . ?
C52Ab C51Ab C50A 118.2(16) . . ?
C56Ab C51Ab C50A 120.9(18) . . ?
O50Ab C50Ab C51A 118.6(19) . . ?
O51Ab C50Ab C51A 115.7(18) . . ?
C54Ab C53Ab C52A 117.3(18) . . ?
C53Ab C52Ab H52B 119.5 . . ?
C51Ab C52Ab H52B 119.5 . . ?
C55Ab C54Ab C53A 123.4(16) . . ?
C51Ab C52Ab C53A 120.9(16) . . ?
C54Ab C53Ab H53B 121.4 . . ?
C52Ab C53Ab H53B 121.4 . . ?
C53Ab C54Ab H54A 118.3 . . ?
C55Ab C54Ab H54A 118.3 . . ?
C58Ab C57Ab C55A 119.7(13) . . ?
C72 C71 C70 119.2(5) . . ?
C72 C71 C73 119.4(5) . . ?
C51Ab C56Ab C55A 118.8(16) . . ?
C73 C71 C70 121.4(4) . . ?
C62Ab C57Ab C55A 123.6(12) . . ?
C52Ab C51Ab C56A 120.9(16) . . ?
C71 C72 H72 119.9 . . ?
C71 C72 C73 120.2(5) . 3_565 ?
C73 C72 H72 119.9 3_565 . ?
C71 C73 C72 120.4(4) . 3_565 ?
C71 C73 H73 119.8 . . ?
C72 C73 H73 119.8 3_565 . ?
C69A O53A H53 110.0 . . ?
O50A C50A O51 125(2) . . ?
O50A C50A C51 119.4(19) . . ?
O51A C50A C51 115.1(17) . . ?
C52A C51A C50 119.5(15) . . ?
C52A C51A C56 120.6(16) . . ?
C56A C51A C50 119.8(17) . . ?
C51A C52A H52 119.7 . . ?
C51A C52A C53 120.5(16) . . ?
C53A C52A H52 119.7 . . ?
C52A C53A H53A 121.0 . . ?
C54A C53A C52 117.9(18) . . ?
C54A C53A H53A 121.0 . . ?
C53A C54A H54 118.8 . . ?
C55A C54A C53 122.3(16) . . ?
C55A C54A H54 118.8 . . ?
C54A C55A C56 118.3(14) . . ?
C54A C55A C57 119.5(14) . . ?
C56A C55A C57 119.8(16) . . ?
C51A C56A C55 118.9(16) . . ?
C51A C56A H56 120.6 . . ?
C55A C56A H56 120.6 . . ?
C58A C57A C55 117.7(12) . . ?
C58A C57A C62 117.4(11) . . ?
C62A C57A C55 123.6(14) . . ?
C57A C58A H58 119.2 . . ?
C59A C58A C57 121.7(13) . . ?
C59A C58A H58 119.2 . . ?
C58A C59A H59 118.6 . . ?
C58A C59A C60 122.7(13) . . ?
C60A C59A H59 118.6 . . ?
C59A C60A C61 115.3(11) . . ?
C59A C60A C63 122.1(13) . . ?
C61A C60A C63 121.8(13) . . ?
N51 C61A C60 130.7(11) . . ?
N51 C61A C62 106.7(8) . . ?
C62A C61A C60 122.5(11) . . ?
N50 C62A C57 131.6(11) . . ?
C61A C62A N50 108.4(9) . . ?
C61A C62A C57 120.0(11) . . ?
C64A C63A C60 124.6(15) . . ?
C64A C63A C68 118.5(13) . . ?
C68A C63A C60 116.8(14) . . ?
C63A C64A H64 120.0 . . ?
C63A C64A C65 120.1(15) . . ?
C65A C64A H64 120.0 . . ?
C66A C65A C64 118.8(14) . . ?
C54Ab C55Ab C56A 118.4(13) . . ?
C51Ab C56Ab H56A 120.6 . . ?
C55Ab C56Ab H56A 120.6 . . ?
C61Ab C62Ab C57A 121.4(13) . . ?
N50 C62Ab C57A 128.3(14) . . ?
C56Ab C55Ab C57A 121.2(16) . . ?
C54Ab C55Ab C57A 119.9(14) . . ?
C59Ab C58Ab C57A 122.0(14) . . ?
C59Ab C58Ab H58A 119.0 . . ?
C57Ab C58Ab H58A 119.0 . . ?
C61Ab C60Ab C59A 115.6(12) . . ?
C58Ab C59Ab H59A 118.7 . . ?
C60Ab C59Ab H59A 118.7 . . ?
C62Ab C61Ab C60A 121.5(11) . . ?
C64Ab C63Ab C60A 121.8(16) . . ?
C58Ab C59Ab C60A 122.6(13) . . ?
C68Ab C63Ab C60A 118.9(14) . . ?
N50 C62Ab C61A 108.0(9) . . ?
C58Ab C57Ab C62A 116.7(12) . . ?
C61Ab C60Ab C63A 122.3(13) . . ?
C59Ab C60Ab C63A 121.8(13) . . ?
C69Ab C65Ab C64A 114.0(18) . . ?
C66Ab C65Ab C64A 118.9(15) . . ?
C63Ab C64Ab H64A 119.7 . . ?
C65Ab C64Ab H64A 119.7 . . ?
C63Ab C64Ab C65A 120.5(16) . . ?
O53Ab C69Ab C65A 121(2) . . ?
C67Ab C66Ab C65A 123.3(16) . . ?
C66A C65A C69 126.9(17) . . ?
C69A C65A C64 113.9(16) . . ?
C65A C66A H66 118.5 . . ?
C67A C66A C65 123.0(15) . . ?
C67A C66A H66 118.5 . . ?
C66A C67A H67 120.8 . . ?
C66A C67A C68 118.5(16) . . ?
C68A C67A H67 120.8 . . ?
C63A C68A C67 120.1(15) . . ?
C63A C68A H68 119.9 . . ?
C67A C68A H68 119.9 . . ?
O52A C69A O53 119(2) . . ?
O52A C69A C65 119.1(18) . . ?
O53A C69A C65 121.9(19) . . ?
C2 O1 C1 119.9(5) . . ?
C4 O2 C8 116.8(5) . . ?
C10 O3 C9 115.9(5) . . ?
C11 O4 C12 112.5(4) . . ?
O1 C1 H1A 110.4 . . ?
O1 C1 H1B 110.4 . . ?
O1 C1 C12 106.8(5) . 3_565 ?
O52Ab C69Ab C65A 120(2) . . ?
C67Ab C66Ab H66A 118.3 . . ?
C65Ab C66Ab H66A 118.3 . . ?
C63Ab C68Ab C67A 120.2(17) . . ?
C68Ab C67Ab H67A 120.8 . . ?
C66Ab C67Ab H67A 120.8 . . ?
C64Ab C63Ab C68A 118.3(14) . . ?
C66Ab C67Ab C68A 118.4(17) . . ?
C63Ab C68Ab H68A 119.9 . . ?
C67Ab C68Ab H68A 119.9 . . ?
C66Ab C65Ab C69A 127.0(19) . . ?
O50Bc C50Bc O51B 122.2(19) . . ?
O52Bc C69Bc O53B 120.6(14) . . ?
C69Bc O53Bc H53C 109.5 . . ?
C56Bc C51Bc C50B 120.6(14) . . ?
C52Bc C51Bc C50B 119.1(12) . . ?
O51Bc C50Bc C51B 117.4(16) . . ?
O50Bc C50Bc C51B 120.2(18) . . ?
C54Bc C53Bc C52B 118.3(14) . . ?
C51Bc C52Bc H52C 119.8 . . ?
C53Bc C52Bc H52C 119.8 . . ?
C51Bc C52Bc C53B 120.4(13) . . ?
C55Bc C54Bc C53B 122.6(12) . . ?
C52Bc C53Bc H53D 120.9 . . ?
C54Bc C53Bc H53D 120.9 . . ?
C53Bc C54Bc H54B 118.7 . . ?
C55Bc C54Bc H54B 118.7 . . ?
C58Bc C57Bc C55B 121.6(10) . . ?
C51Bc C56Bc C55B 120.3(13) . . ?
C62Bc C57Bc C55B 121.9(9) . . ?
C52Bc C51Bc C56B 120.2(12) . . ?
C54Bc C55Bc C56B 117.6(10) . . ?
C51Bc C56Bc H56B 119.9 . . ?
C55Bc C56Bc H56B 119.9 . . ?
C54Bc C55Bc C57B 122.7(10) . . ?
N50 C62Bc C57B 130.5(8) . . ?
C59Bc C58Bc C57B 122.1(10) . . ?
C61Bc C62Bc C57B 120.5(8) . . ?
C56Bc C55Bc C57B 119.3(10) . . ?
C57Bc C58Bc H58B 118.9 . . ?
C59Bc C58Bc H58B 118.9 . . ?
C58Bc C59Bc H59B 118.0 . . ?
C60Bc C59Bc H59B 118.0 . . ?
C62Bc C61Bc C60B 123.4(8) . . ?
C64Bc C63Bc C60B 125.9(12) . . ?
C58Bc C59Bc C60B 123.9(10) . . ?
C68Bc C63Bc C60B 116.9(10) . . ?
C59Bc C60Bc C61B 113.4(8) . . ?
C58Bc C57Bc C62B 116.4(9) . . ?
C59Bc C60Bc C63B 123.9(9) . . ?
H1A C1 H1B 108.6 . . ?
C12 C1 H1A 110.4 3_565 . ?
C12 C1 H1B 110.4 3_565 . ?
O1 C2 C3 125.0(5) . . ?
O1 C2 C7 114.0(5) . . ?
C7 C2 C3 121.0(5) . . ?
C2 C3 H3 120.9 . . ?
C2 C3 C4 118.1(5) . . ?
C4 C3 H3 120.9 . . ?
O2 C4 C3 113.7(5) . . ?
O2 C4 C5 125.4(5) . . ?
C5 C4 C3 120.9(5) . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 119.9(5) . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C20 121.4(10) . . ?
C5 C6 C20A 120.4(10) . . ?
C7 C6 C5 119.9(6) . . ?
C7 C6 C20 118.2(10) . . ?
C7 C6 C20A 119.3(10) . . ?
C2 C7 C6 120.0(6) . . ?
C2 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
O2 C8 H8A 110.2 . . ?
O2 C8 H8B 110.2 . . ?
O2 C8 C9 107.6(6) . . ?
H8A C8 H8B 108.5 . . ?
C9 C8 H8A 110.2 . . ?
C9 C8 H8B 110.2 . . ?
O3 C9 C8 110.6(6) . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
O3 C10 H10A 110.2 . . ?
O3 C10 H10B 110.2 . . ?
O3 C10 C11 107.6(5) . . ?
H10A C10 H10B 108.5 . . ?
C11 C10 H10A 110.2 . . ?
C11 C10 H10B 110.2 . . ?
O4 C11 C10 108.7(5) . . ?
O4 C11 H11A 110.0 . . ?
O4 C11 H11B 110.0 . . ?
C10 C11 H11A 110.0 . . ?
C10 C11 H11B 110.0 . . ?
H11A C11 H11B 108.3 . . ?
O4 C12 C1 108.7(4) . 3_565 ?
O4 C12 H12A 109.9 . . ?
O4 C12 H12B 109.9 . . ?
C1 C12 H12A 109.9 3_565 . ?
C1 C12 H12B 109.9 3_565 . ?
H12A C12 H12B 108.3 . . ?
C22A N20A C23 117.2(10) . . ?
C21A C20A C6 123.0(13) . . ?
C24A C20A C6 117.6(15) . . ?
C24A C20A C21 119.3(12) . . ?
C20A C21A H21 121.0 . . ?
C22A C21A C20 117.9(12) . . ?
C22A C21A H21 121.0 . . ?
N20A C22A C21 124.9(12) . . ?
N20A C22A H22 117.6 . . ?
C21A C22A H22 117.6 . . ?
N20A C23A H23 118.0 . . ?
C24A C23A N20 124.0(12) . . ?
C24A C23A H23 118.0 . . ?
C20A C24A H24 121.7 . . ?
C23A C24A C20 116.5(14) . . ?
C23A C24A H24 121.7 . . ?
H0AA O0AA H0AB 105.3(6) . . ?
C61Bc C60Bc C63B 122.6(9) . . ?
C66Bc C65Bc C64B 119.5(11) . . ?
C69Bc C65Bc C64B 118.7(12) . . ?
C63Bc C64Bc H64B 119.9 . . ?
C65Bc C64Bc H64B 119.9 . . ?
O53Bc C69Bc C65B 116.1(12) . . ?
C67Bc C66Bc C65B 122.6(11) . . ?
C63Bc C64Bc C65B 120.2(12) . . ?
O52Bc C69Bc C65B 123.3(13) . . ?
C65Bc C66Bc H66B 118.7 . . ?
C67Bc C66Bc H66B 118.7 . . ?
C63Bc C68Bc C67B 121.2(12) . . ?
C68Bc C67Bc H67B 120.6 . . ?
C66Bc C67Bc H67B 120.6 . . ?
C64Bc C63Bc C68B 117.3(10) . . ?
C66Bc C67Bc C68B 118.8(13) . . ?
C67Bc C68Bc H68B 119.4 . . ?
C63Bc C68Bc H68B 119.4 . . ?
C66Bc C65Bc C69B 121.7(12) . . ?
C24Ab C20Ab C6 120.4(15) . . ?
C21Ab C20Ab C6 120.7(14) . . ?
C24Ab C23Ab N20A 124.7(13) . . ?
C23Ab C24Ab C20A 116.1(14) . . ?
C22Ab C21Ab C20A 118.6(11) . . ?
C24Ab C20Ab C21A 118.8(11) . . ?
N20Ab C22Ab C21A 125.4(11) . . ?
C20Ab C21Ab H21A 120.7 . . ?
C22Ab C21Ab H21A 120.7 . . ?
C21Ab C22Ab H22A 117.3 . . ?
N20Ab C22Ab H22A 117.3 . . ?
C22Ab N20Ab C23A 116.3(11) . . ?
C24Ab C23Ab H23A 117.6 . . ?
N20Ab C23Ab H23A 117.6 . . ?
C20Ab C24Ab H24A 121.9 . . ?
C23Ab C24Ab H24A 121.9 . . ?
C3Ea C2Ea N1E 134(3) . . ?
C5Ea C4Ea N1E 118(3) . . ?
O1Ea C1Ea N1E 120(3) . . ?
C2Ea N1Ea C1E 112(2) . . ?
C4Ea N1Ea C1E 123(2) . . ?
O1Ea C1Ea H1E 120.1 . . ?
N1Ea C1Ea H1E 120.1 . . ?
C4Ea N1Ea C2E 125(3) . . ?
C3Ea C2Ea H2EA 103.8 . . ?
N1Ea C2Ea H2EA 103.8 . . ?
C3Ea C2Ea H2EB 103.8 . . ?
N1Ea C2Ea H2EB 103.8 . . ?
H2EAa C2Ea H2EB 105.4 . . ?
C2Ea C3Ea H3EA 107.8 . . ?
C2Ea C3Ea H3EB 109.2 . . ?
H3EAa C3Ea H3EB 109.5 . . ?
C2Ea C3Ea H3EC 111.4 . . ?
H3EAa C3Ea H3EC 109.5 . . ?
H3EBa C3Ea H3EC 109.5 . . ?
C5Ea C4Ea H4EA 107.9 . . ?
N1Ea C4Ea H4EA 107.9 . . ?
H4EAa C4Ea H4EB 107.2 . . ?
N1Ea C4Ea H4EB 107.9 . . ?
C5Ea C4Ea H4EB 107.9 . . ?
C4Ea C5Ea H5EA 108.1 . . ?
C4Ea C5Ea H5EB 107.7 . . ?
H5EAa C5Ea H5EB 109.5 . . ?
C4Ea C5Ea H5EC 112.5 . . ?
H5EAa C5Ea H5EC 109.4 . . ?
H5EBa C5Ea H5EC 109.5 . . ?
C5Dc C4Dc N1D 120(2) . . ?
O1Dc C1Dc N1D 118(2) . . ?
C3Dc C2Dc N1D 135(2) . . ?
C2Dc N1Dc C1D 111.4(18) . . ?
C4Dc N1Dc C1D 126(2) . . ?
N1Dc C1Dc H1D 120.8 . . ?
O1Dc C1Dc H1D 120.8 . . ?
C4Dc N1Dc C2D 123(2) . . ?
C3Dc C2Dc H2DA 103.5 . . ?
N1Dc C2Dc H2DA 103.5 . . ?
C3Dc C2Dc H2DB 103.5 . . ?
N1Dc C2Dc H2DB 103.5 . . ?
H2DAc C2Dc H2DB 105.3 . . ?
C2Dc C3Dc H3DA 104.8 . . ?
C2Dc C3Dc H3DB 113.0 . . ?
H3DAc C3Dc H3DB 109.5 . . ?
C2Dc C3Dc H3DC 110.5 . . ?
H3DBc C3Dc H3DC 109.5 . . ?
H3DAc C3Dc H3DC 109.5 . . ?
C5Dc C4Dc H4DA 107.2 . . ?
N1Dc C4Dc H4DA 107.2 . . ?
C5Dc C4Dc H4DB 107.2 . . ?
H4DAc C4Dc H4DB 106.8 . . ?
N1Dc C4Dc H4DB 107.2 . . ?
C4Dc C5Dc H5DA 109.5 . . ?
H5DAc C5Dc H5DB 109.5 . . ?
C4Dc C5Dc H5DB 109.5 . . ?
H5DBc C5Dc H5DC 109.5 . . ?
H5DAc C5Dc H5DC 109.5 . . ?
C4Dc C5Dc H5DC 109.5 . . ?
C61Ab N51 H51A 128.1 . . ?
C61Bc N51 H51B 126.8 . . ?
N51 C61Ab C60A 131.2(12) . . ?
N51 C61Bc C60B 130.3(8) . . ?
N51 C61Bc C62B 106.1(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
C62Ab N50 C70 N51 -8(2) . . . . ?
C50Bc C51Bc C56Bc C55Bc 174.1(15) . . . . ?
C60Bc C63Bc C68Bc C67Bc -176.2(13) . . . . ?
C62Bc N50 C70 N51 5.9(15) . . . . ?
C58Bc C57Bc C62Bc C61Bc 5(3) . . . . ?
C62Ab N50 C70 C71 169(2) . . . . ?
C4Dc N1Dc C1Dc O1Dc 178.1(19) . . . . ?
C62Bc N50 C70 C71 -177.0(14) . . . . ?
C55Bc C57Bc C58Bc C59Bc -180.0(16) . . . . ?
C61Bc N51 C70 N50 -4.2(15) . . . . ?
C68Bc C63Bc C64Bc C65Bc -2.3(14) . . . . ?
C61Ab N51 C70 N50 11(2) . . . . ?
N20Ab C23Ab C24Ab C20Ab 0(3) . . . . ?
C61Bc N51 C70 C71 178.6(14) . . . . ?
C52Bc C53Bc C54Bc C55Bc 5(3) . . . . ?
C61Ab N51 C70 C71 -166(2) . . . . ?
C56Bc C55Bc C57Bc C58Bc 130.8(18) . . . . ?
O50Ab C50Ab C51Ab C52Ab 19(3) . . . . ?
C59Bc C60Bc C61Bc C62Bc -2(3) . . . . ?
O51Ab C50Ab C51Ab C52Ab -163(3) . . . . ?
C59Bc C60Bc C63Bc C64Bc -55(2) . . . . ?
O50Ab C50Ab C51Ab C56Ab -160(4) . . . . ?
C69Bc C65Bc C66Bc C67Bc -168.4(19) . . . . ?
O51Ab C50Ab C51Ab C56Ab 18(3) . . . . ?
C56Ab C51Ab C52Ab C53Ab 1(3) . . . . ?
C4 C5 C6 C20Ab -172.7(13) . . . . ?
C20Ab C6 C7 C2 171.8(12) . . . . ?
C66Bc C65Bc C69Bc O53Bc -5(2) . . . . ?
C4Ea N1Ea C2Ea C3Ea -172(8) . . . . ?
C24Ab C20Ab C21Ab C22Ab 1(3) . . . . ?
C2Dc N1Dc C4Dc C5Dc 84(3) . . . . ?
C52Ab C53Ab C54Ab C55Ab -3(5) . . . . ?
C53Bc C54Bc C55Bc C57Bc -179.9(18) . . . . ?
C53Ab C54Ab C55Ab C56Ab 6(5) . . . . ?
C57Bc C55Bc C56Bc C51Bc -178.4(17) . . . . ?
C53Ab C54Ab C55Ab C57Ab 178(3) . . . . ?
C56Bc C55Bc C57Bc C62Bc -47(3) . . . . ?
C52Ab C51Ab C56Ab C55Ab 2(4) . . . . ?
C58Bc C59Bc C60Bc C61Bc 5(3) . . . . ?
C50Ab C51Ab C56Ab C55Ab -178(3) . . . . ?
C60Bc C61Bc C62Bc N50 179(2) . . . . ?
C54Ab C55Ab C56Ab C51Ab -6(5) . . . . ?
C58Bc C57Bc C62Bc N50 -177(2) . . . . ?
C57Ab C55Ab C56Ab C51Ab -178(3) . . . . ?
C59Bc C60Bc C63Bc C68Bc 124.5(17) . . . . ?
C54Ab C55Ab C57Ab C58Ab -32(4) . . . . ?
C63Bc C64Bc C65Bc C66Bc -3.0(16) . . . . ?
C56Ab C55Ab C57Ab C58Ab 140(3) . . . . ?
C65Bc C66Bc C67Bc C68Bc -6(3) . . . . ?
C54Ab C55Ab C57Ab C62Ab 148(4) . . . . ?
C66Bc C65Bc C69Bc O52Bc 173.2(18) . . . . ?
C56Ab C55Ab C57Ab C62Ab -40(5) . . . . ?
C50Ab C51Ab C52Ab C53Ab -178(2) . . . . ?
C62Ab C57Ab C58Ab C59Ab 0(2) . . . . ?
C20Ab C21Ab C22Ab N20Ab -3(3) . . . . ?
C51Ab C52Ab C53Ab C54Ab -1(4) . . . . ?
C4Ea N1Ea C1Ea O1Ea 179(3) . . . . ?
C57Ab C58Ab C59Ab C60Ab 2(2) . . . . ?
C2Ea N1Ea C4Ea C5Ea -125(7) . . . . ?
C58Ab C59Ab C60Ab C61Ab -5(4) . . . . ?
C4Dc N1Dc C2Dc C3Dc 95(4) . . . . ?
C58Ab C59Ab C60Ab C63Ab -179(2) . . . . ?
C51Bc C52Bc C53Bc C54Bc -4(3) . . . . ?
C59Ab C60Ab C61Ab C62Ab 6(6) . . . . ?
C53Bc C54Bc C55Bc C56Bc -7(3) . . . . ?
C63Ab C60Ab C61Ab C62Ab -180(3) . . . . ?
C52Bc C51Bc C56Bc C55Bc -8(3) . . . . ?
C60Ab C61Ab C62Ab N50 -169(4) . . . . ?
C54Bc C55Bc C56Bc C51Bc 8(3) . . . . ?
C60Ab C61Ab C62Ab C57Ab -5(6) . . . . ?
C54Bc C55Bc C57Bc C58Bc -56(2) . . . . ?
C58Ab C57Ab C62Ab N50 162(4) . . . . ?
C54Bc C55Bc C57Bc C62Bc 126(2) . . . . ?
C55Ab C57Ab C62Ab N50 -18(6) . . . . ?
C62Bc C57Bc C58Bc C59Bc -2.0(19) . . . . ?
C58Ab C57Ab C62Ab C61Ab 2(5) . . . . ?
C57Bc C58Bc C59Bc C60Bc -3.1(17) . . . . ?
C55Ab C57Ab C62Ab C61Ab -178(4) . . . . ?
C58Bc C59Bc C60Bc C63Bc -173.3(14) . . . . ?
C61Ab C60Ab C63Ab C64Ab -91(4) . . . . ?
C63Bc C60Bc C61Bc C62Bc 176(2) . . . . ?
C59Ab C60Ab C63Ab C64Ab 82(3) . . . . ?
C60Bc C61Bc C62Bc C57Bc -2(4) . . . . ?
C61Ab C60Ab C63Ab C68Ab 77(4) . . . . ?
C55Bc C57Bc C62Bc C61Bc -177(2) . . . . ?
C59Ab C60Ab C63Ab C68Ab -110(3) . . . . ?
C55Bc C57Bc C62Bc N50 1(4) . . . . ?
C68Ab C63Ab C64Ab C65Ab 3(2) . . . . ?
C61Bc C60Bc C63Bc C64Bc 126.4(19) . . . . ?
C60Ab C63Ab C64Ab C65Ab 171(2) . . . . ?
C61Bc C60Bc C63Bc C68Bc -54(2) . . . . ?
C63Ab C64Ab C65Ab C66Ab 2(3) . . . . ?
C60Bc C63Bc C64Bc C65Bc 177.6(13) . . . . ?
C63Ab C64Ab C65Ab C69Ab -178(2) . . . . ?
C63Bc C64Bc C65Bc C69Bc 172.9(13) . . . . ?
C69Ab C65Ab C66Ab C67Ab 176(4) . . . . ?
C64Bc C65Bc C66Bc C67Bc 7(3) . . . . ?
C64Ab C65Ab C66Ab C67Ab -3(5) . . . . ?
C64Bc C63Bc C68Bc C67Bc 3.7(19) . . . . ?
C1Dc N1Dc C4Dc C5Dc -96(3) . . . . ?
C66Bc C67Bc C68Bc C63Bc 0(2) . . . . ?
C64Ab C63Ab C68Ab C67Ab -6(4) . . . . ?
C64Bc C65Bc C69Bc O52Bc -2.6(19) . . . . ?
C60Ab C63Ab C68Ab C67Ab -175(3) . . . . ?
C64Bc C65Bc C69Bc O53Bc 179.0(15) . . . . ?
C66Ab C67Ab C68Ab C63Ab 5(5) . . . . ?
C55Ab C57Ab C58Ab C59Ab 180(3) . . . . ?
C66Ab C65Ab C69Ab O52Ab -127(4) . . . . ?
C23Ab N20Ab C22Ab C21Ab 3(3) . . . . ?
C64Ab C65Ab C69Ab O52Ab 52(4) . . . . ?
C22Ab N20Ab C23Ab C24Ab -1(3) . . . . ?
C66Ab C65Ab C69Ab O53Ab 56(4) . . . . ?
C21Ab C20Ab C24Ab C23Ab 0(3) . . . . ?
C64Ab C65Ab C69Ab O53Ab -124(3) . . . . ?
C2Ea N1Ea C1Ea O1Ea 0(3) . . . . ?
O50Bc C50Bc C51Bc C52Bc 12.3(16) . . . . ?
C1Ea N1Ea C2Ea C3Ea 8(10) . . . . ?
O51Bc C50Bc C51Bc C52Bc -171.7(16) . . . . ?
C1Ea N1Ea C4Ea C5Ea 55(7) . . . . ?
O50Bc C50Bc C51Bc C56Bc -169.6(17) . . . . ?
C2Dc N1Dc C1Dc O1Dc -2(2) . . . . ?
O51Bc C50Bc C51Bc C56Bc 6.5(19) . . . . ?
C1Dc N1Dc C2Dc C3Dc -86(4) . . . . ?
C56Bc C51Bc C52Bc C53Bc 5(2) . . . . ?
C50Bc C51Bc C52Bc C53Bc -176.5(14) . . . . ?
C65Ab C66Ab C67Ab C68Ab 0(6) . . . . ?
C59Bc C60Bc C61Bc N51 172(2) . . . . ?
C63Ab C60Ab C61Ab N51 9(7) . . . . ?
C63Bc C60Bc C61Bc N51 -9(4) . . . . ?
C59Ab C60Ab C61Ab N51 -165(4) . . . . ?
N50 C70 C71 C72 -30.5(7) . . . . ?
N50 C70 C71 C73 151.3(5) . . . . ?
N51 C61Bc C62Bc C57Bc -178(2) . . . . ?
N51 C61Bc C62Bc N50 3(3) . . . . ?
N51 C61Ab C62Ab C57Ab 168(4) . . . . ?
N51 C61Ab C62Ab N50 4(4) . . . . ?
N51 C70 C71 C72 146.4(4) . . . . ?
N51 C70 C71 C73 -31.9(7) . . . . ?
N51 C61A C62A N50 -1(6) . . . . ?
N51 C61A C62A C57A -178(4) . . . . ?
C70 N50 C62Ab C57Ab -160(4) . . . . ?
C70 N50 C62Ab C61Ab 2(4) . . . . ?
C70 N50 C62Bc C61Bc -5(2) . . . . ?
C70 N50 C62Bc C57Bc 176(2) . . . . ?
C70 N50 C62A C57A 177(5) . . . . ?
C70 N50 C62A C61A 1(5) . . . . ?
C70 N51 C61Bc C60Bc -175(2) . . . . ?
C70 N51 C61Ab C62Ab -9(4) . . . . ?
C70 N51 C61Bc C62Bc 0(2) . . . . ?
C70 N51 C61Ab C60Ab 164(4) . . . . ?
C70 N51 C61A C60A 180(5) . . . . ?
C70 N51 C61A C62A 1(5) . . . . ?
C70 C71 C72 C73 -178.1(4) . . . 3_565 ?
C70 C71 C73 C72 178.1(4) . . . 3_565 ?
C72 C71 C73 C72 -0.2(8) . . . 3_565 ?
C73 C71 C72 C73 0.2(8) . . . 3_565 ?
O50A C50A C51A C52A -1(3) . . . . ?
O50A C50A C51A C56A -179(3) . . . . ?
O51A C50A C51A C52A 179(3) . . . . ?
O51A C50A C51A C56A 2(4) . . . . ?
C50A C51A C52A C53A -178(2) . . . . ?
C50A C51A C56A C55A -174(3) . . . . ?
C51A C52A C53A C54A -2(5) . . . . ?
C52A C51A C56A C55A 8(5) . . . . ?
C52A C53A C54A C55A -5(6) . . . . ?
C53A C54A C55A C56A 13(6) . . . . ?
C53A C54A C55A C57A 175(4) . . . . ?
C54A C55A C56A C51A -15(6) . . . . ?
C54A C55A C57A C58A -26(5) . . . . ?
C54A C55A C57A C62A 141(4) . . . . ?
C55A C57A C58A C59A 175(3) . . . . ?
C55A C57A C62A N50 10(8) . . . . ?
C55A C57A C62A C61A -174(4) . . . . ?
C56A C51A C52A C53A 0(3) . . . . ?
C56A C55A C57A C58A 136(4) . . . . ?
C56A C55A C57A C62A -57(5) . . . . ?
C57A C55A C56A C51A -177(3) . . . . ?
C57A C58A C59A C60A -4(5) . . . . ?
C58A C57A C62A N50 177(5) . . . . ?
C58A C57A C62A C61A -7(7) . . . . ?
C58A C59A C60A C61A -1(6) . . . . ?
C58A C59A C60A C63A -170(3) . . . . ?
C59A C60A C61A N51 -178(5) . . . . ?
C59A C60A C61A C62A 1(7) . . . . ?
C59A C60A C63A C64A -88(3) . . . . ?
C59A C60A C63A C68A 89(4) . . . . ?
C60A C61A C62A N50 180(5) . . . . ?
C60A C61A C62A C57A 3(9) . . . . ?
C60A C63A C64A C65A 173(2) . . . . ?
C60A C63A C68A C67A -170(3) . . . . ?
C61A N51 C70 N50 -1(3) . . . . ?
C61A N51 C70 C71 -178(3) . . . . ?
C61A C60A C63A C64A 103(4) . . . . ?
C61A C60A C63A C68A -80(4) . . . . ?
C62A N50 C70 N51 0(3) . . . . ?
C62A N50 C70 C71 177(3) . . . . ?
C62A C57A C58A C59A 8(6) . . . . ?
C63A C60A C61A N51 -8(8) . . . . ?
C63A C60A C61A C62A 171(4) . . . . ?
C63A C64A C65A C66A -4(2) . . . . ?
C63A C64A C65A C69A 169(2) . . . . ?
C64A C63A C68A C67A 7(4) . . . . ?
C64A C65A C66A C67A 11(5) . . . . ?
C64A C65A C69A O52A -26(3) . . . . ?
C64A C65A C69A O53A 157(3) . . . . ?
C65A C66A C67A C68A -8(6) . . . . ?
C66A C65A C69A O52A 147(4) . . . . ?
C66A C65A C69A O53A -31(4) . . . . ?
C66A C67A C68A C63A -1(5) . . . . ?
C68A C63A C64A C65A -5(2) . . . . ?
C69A C65A C66A C67A -161(3) . . . . ?
O1 C2 C3 C4 -177.4(4) . . . . ?
O1 C2 C7 C6 180.0(4) . . . . ?
O2 C4 C5 C6 -177.4(5) . . . . ?
O2 C8 C9 O3 -78.7(7) . . . . ?
O3 C10 C11 O4 66.9(6) . . . . ?
C1 O1 C2 C3 -2.2(7) . . . . ?
C1 O1 C2 C7 177.6(5) . . . . ?
C2 O1 C1 C12 165.0(4) . . . 3_565 ?
C2 C3 C4 O2 175.8(4) . . . . ?
C2 C3 C4 C5 -3.8(7) . . . . ?
C3 C2 C7 C6 -0.2(8) . . . . ?
C3 C4 C5 C6 2.2(8) . . . . ?
C4 O2 C8 C9 167.7(5) . . . . ?
C4 C5 C6 C7 0.5(8) . . . . ?
C4 C5 C6 C20A 172.4(11) . . . . ?
C5 C6 C20Ab C21Ab -154.8(17) . . . . ?
C5 C6 C20Ab C24Ab 30(2) . . . . ?
C5 C6 C7 C2 -1.5(8) . . . . ?
C5 C6 C20A C21A -131.8(14) . . . . ?
C5 C6 C20A C24A 51.8(18) . . . . ?
C6 C20Ab C21Ab C22Ab -173.8(17) . . . . ?
C6 C20Ab C24Ab C23Ab 175(2) . . . . ?
C6 C20A C21A C22A -174.4(18) . . . . ?
C6 C20A C24A C23A 174(2) . . . . ?
C7 C2 C3 C4 2.8(7) . . . . ?
C7 C6 C20Ab C21Ab 32(3) . . . . ?
C7 C6 C20Ab C24Ab -143.3(17) . . . . ?
C7 C6 C20A C21A 40(2) . . . . ?
C7 C6 C20A C24A -136.1(14) . . . . ?
C8 O2 C4 C3 179.3(5) . . . . ?
C8 O2 C4 C5 -1.1(8) . . . . ?
C9 O3 C10 C11 167.0(5) . . . . ?
C10 O3 C9 C8 -178.5(6) . . . . ?
C11 O4 C12 C1 170.4(5) . . . 3_565 ?
C12 O4 C11 C10 -168.2(5) . . . . ?
N20A C23A C24A C20A 4(3) . . . . ?
C20A C6 C7 C2 -173.7(11) . . . . ?
C20A C21A C22A N20A -3(2) . . . . ?
C21A C20A C24A C23A -2(2) . . . . ?
C22A N20A C23A C24A -5(2) . . . . ?
C23A N20A C22A C21A 4(2) . . . . ?
C24A C20A C21A C22A 1.9(17) . . . . ?

_shelx_SHELXL_version_number     2016/4

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'solvothermal from DEF, EtOH, H2O'
