# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1840385'
_audit_update_record             
;
2018-04-30 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_audit_creation_date             2018-01-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C90 H77 Co4 N14 O39.5'
_chemical_formula_sum            'C90 H77 Co4 N14 O39.50'
_chemical_formula_weight         2222.37
_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 0.0030 0.0020 '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'
Co Co 0.3570 0.9660 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0070 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0120 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                   15.060(3)
_cell_length_b                   17.240(3)
_cell_length_c                   18.790(4)
_cell_angle_alpha                92.09(3)
_cell_angle_beta                 100.49(3)
_cell_angle_gamma                115.21(3)
_cell_volume                     4304.1(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    128774
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      1.111
_shelx_estimated_absorpt_T_max   0.991
_shelx_estimated_absorpt_T_min   0.983
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2278
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1208
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            128774
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.111
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_source                   'MX1 Beamline Asutralian Synchrotron'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12145
_reflns_number_total             19677
_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       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluICE (McPhillips et al, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.839
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1387
_refine_ls_number_reflns         19677
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0880
_refine_ls_restrained_S_all      1.007
_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)+(0.1807P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2352
_refine_ls_wR_factor_ref         0.2699
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C79-O35
 1.3 with sigma of 0.02
 C84-N10
 1.45 with sigma of 0.02
 N10-O35
 2.27 with sigma of 0.04
3. Rigid body (RIGU) restrains
 N10, C79, C83, C84
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(N9)=Sof(C80)=Sof(H80)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C82)=
 Sof(H82A)=Sof(H82B)=Sof(H82C)=1-FVAR(1)
 Sof(N10)=Sof(C79)=Sof(H79)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=Sof(C84)=
 Sof(H84A)=Sof(H84B)=Sof(H84C)=FVAR(1)
 Fixed Sof: O34(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C17(H17A,H17B), C20(H20A,H20B), C35(H35A,H35B), C38(H38A,H38B),
 C53(H53A,H53B), C56(H56A,H56B), C71(H71A,H71B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C12(H12), C25(H25), C27(H27), C28(H28), C30(H30),
 C43(H43), C45(H45), C46(H46), C48(H48), C61(H61), C63(H63), C64(H64), C66(H66),
  C74(H74), C79(H79), C80(H80), C85(H85), C88(H88), C91(H91), C94(H94)
5.c Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C81(H81A,H81B,H81C), C82(H82A,H82B,
 H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C87(H87A,
 H87B,H87C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C92(H92A,H92B,H92C),
 C93(H93A,H93B,H93C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Co1 Co 1.000000 0.500000 0.000000 0.03658(19) Uani 1 2 d S T P . .
Co2 Co 1.00019(4) 0.46784(4) 0.25004(3) 0.04466(17) Uani 1 1 d . . . . .
Co3 Co 1.000000 0.500000 0.500000 0.0465(2) Uani 1 2 d S T P . .
Co4 Co -0.00185(4) 0.03000(4) 0.62268(3) 0.03676(16) Uani 1 1 d . . . . .
Co5 Co -0.00218(4) 0.02234(3) 0.87425(3) 0.03473(16) Uani 1 1 d . . . . .
O1 O 0.9282(2) 0.5127(2) 0.08295(16) 0.0445(7) Uani 1 1 d . . . . .
O2 O 0.8683(2) 0.4375(2) 0.17116(17) 0.0497(7) Uani 1 1 d . . . . .
O3 O 0.6339(3) 0.4688(2) 0.12035(19) 0.0574(9) Uani 1 1 d . . . . .
O4 O 0.7183(3) 0.2518(2) 0.06854(19) 0.0572(9) Uani 1 1 d . . . . .
O5 O 0.2750(2) 0.1904(2) 0.30734(16) 0.0432(7) Uani 1 1 d . . . . .
O6 O 0.3664(2) -0.02293(19) 0.25842(17) 0.0436(7) Uani 1 1 d . . . . .
O7 O 0.1303(2) -0.0094(2) 0.20619(15) 0.0434(7) Uani 1 1 d . . . . .
O8 O 0.0723(2) -0.0640(2) 0.30448(16) 0.0441(7) Uani 1 1 d . . . . .
O9 O 0.9328(2) 0.5079(2) 0.31914(17) 0.0478(7) Uani 1 1 d . . . . .
O10 O 0.8680(2) 0.4628(2) 0.41657(16) 0.0498(7) Uani 1 1 d . . . . .
O11 O 0.6456(2) 0.47672(19) 0.35185(17) 0.0441(7) Uani 1 1 d . . . . .
O12 O 0.7175(2) 0.2474(2) 0.32079(18) 0.0481(7) Uani 1 1 d . . . . .
O13 O 0.2889(2) 0.2387(2) 0.55437(17) 0.0477(7) Uani 1 1 d . . . . .
O14 O 0.3595(2) 0.0092(2) 0.52332(17) 0.0451(7) Uani 1 1 d . . . . .
O15 O 0.1342(2) 0.02353(19) 0.45815(15) 0.0387(6) Uani 1 1 d . . . . .
O16 O 0.0695(2) -0.01305(19) 0.55736(15) 0.0392(6) Uani 1 1 d . . . . .
O17 O 0.9335(3) 0.5356(2) 0.57581(18) 0.0543(8) Uani 1 1 d . . . . .
O18 O 0.8675(2) 0.4853(2) 0.67191(17) 0.0493(7) Uani 1 1 d . . . . .
O19 O 0.6464(3) 0.5149(2) 0.61044(19) 0.0534(8) Uani 1 1 d . . . . .
O20 O 0.7097(2) 0.2834(2) 0.56785(17) 0.0478(7) Uani 1 1 d . . . . .
O21 O 0.2829(2) 0.2682(2) 0.80582(18) 0.0498(8) Uani 1 1 d . . . . .
O22 O 0.3507(2) 0.0383(2) 0.76624(18) 0.0470(7) Uani 1 1 d . . . . .
O23 O 0.1320(2) 0.0728(2) 0.70309(15) 0.0426(7) Uani 1 1 d . . . . .
O24 O 0.0640(2) 0.00326(19) 0.79163(15) 0.0406(6) Uani 1 1 d . . . . .
O25 O 0.9299(2) 0.5467(2) 0.82886(18) 0.0538(8) Uani 1 1 d . . . . .
O26 O 0.8696(2) 0.4816(2) 0.92196(16) 0.0454(7) Uani 1 1 d . . . . .
O27 O 0.6353(2) 0.5096(2) 0.87453(18) 0.0488(7) Uani 1 1 d . . . . .
O28 O 0.7205(2) 0.2948(2) 0.81767(16) 0.0447(7) Uani 1 1 d . . . . .
O29 O 0.2762(2) 0.2275(2) 1.05609(17) 0.0500(7) Uani 1 1 d . . . . .
O30 O 0.3620(3) 0.0121(2) 1.00106(19) 0.0523(8) Uani 1 1 d . . . . .
O31 O 0.1288(2) 0.0361(2) 0.95022(15) 0.0400(6) Uani 1 1 d . . . . .
O32 O 0.0682(2) -0.03319(19) 1.04159(15) 0.0388(6) Uani 1 1 d . . . . .
O33 O 1.0661(2) 0.6341(2) 0.00472(19) 0.0511(8) Uani 1 1 d . . . . .
O34 O 1.0630(7) 0.6049(6) 0.2175(6) 0.097(3) Uani 0.5 1 d . . . . .
O35 O 0.9425(3) 0.3388(2) 0.2622(2) 0.0637(10) Uani 1 1 d D . . . .
O36 O 0.0567(2) 0.1583(2) 0.59814(18) 0.0496(7) Uani 1 1 d . . . . .
O37 O -0.0617(3) -0.0964(2) 0.66527(18) 0.0524(8) Uani 1 1 d . . . . .
O38 O 1.0633(3) 0.6321(3) 0.4851(2) 0.0749(13) Uani 1 1 d . . . . .
O39 O 0.0685(2) 0.1583(2) 0.88262(17) 0.0446(7) Uani 1 1 d . . . . .
O40 O -0.0756(3) -0.1118(2) 0.8540(2) 0.0599(9) Uani 1 1 d . . . . .
N1 N 0.6750(3) 0.3591(3) 0.0929(2) 0.0480(9) Uani 1 1 d . . . . .
N2 N 0.3228(3) 0.0848(2) 0.28407(18) 0.0370(7) Uani 1 1 d . . . . .
N3 N 0.6810(3) 0.3618(2) 0.33559(19) 0.0404(8) Uani 1 1 d . . . . .
N4 N 0.3235(2) 0.1235(2) 0.53802(18) 0.0378(7) Uani 1 1 d . . . . .
N5 N 0.6778(3) 0.3992(2) 0.5894(2) 0.0423(8) Uani 1 1 d . . . . .
N6 N 0.3186(3) 0.1541(2) 0.78780(18) 0.0383(7) Uani 1 1 d . . . . .
N7 N 0.6752(3) 0.4008(2) 0.84394(18) 0.0397(7) Uani 1 1 d . . . . .
N8 N 0.3214(3) 0.1216(2) 1.03107(19) 0.0411(8) Uani 1 1 d . . . . .
N9 N 0.8836(10) 0.2018(9) 0.2808(8) 0.052(3) Uani 0.447(10) 1 d . . . A 2
N10 N 0.8688(7) 0.1951(6) 0.2285(7) 0.054(2) Uani 0.553(10) 1 d D U . A 1
N11 N 1.1323(4) 0.7680(3) 0.0685(4) 0.0801(16) Uani 1 1 d . . . . .
N12 N 1.1207(4) 0.7517(3) 0.4345(5) 0.098(2) Uani 1 1 d . . . . .
N13 N 0.1116(3) 0.2679(2) 0.5272(3) 0.0542(10) Uani 1 1 d . . . . .
N14 N 0.1140(3) 0.2910(3) 0.8421(2) 0.0501(9) Uani 1 1 d . . . . .
N15 N -0.1065(4) -0.2486(3) 0.8700(3) 0.0730(14) Uani 1 1 d . . . . .
C0AA C 0.4515(3) 0.1098(3) 0.2130(2) 0.0362(8) Uani 1 1 d . . . . .
C1 C 0.8600(3) 0.4575(3) 0.1084(2) 0.0438(9) Uani 1 1 d . . . . .
C2 C 0.7539(3) 0.4160(3) 0.0577(2) 0.0513(11) Uani 1 1 d . . . . .
H2A H 0.736887 0.462468 0.040261 0.062 Uiso 1 1 calc R . . . .
H2B H 0.755252 0.382105 0.014522 0.062 Uiso 1 1 calc R . . . .
C3 C 0.6197(3) 0.3932(3) 0.1244(2) 0.0461(10) Uani 1 1 d . . . . .
C4 C 0.6663(3) 0.2753(3) 0.0974(2) 0.0444(9) Uani 1 1 d . . . . .
C5 C 0.5435(4) 0.3358(3) 0.1630(2) 0.0461(10) Uani 1 1 d . . . . .
C6 C 0.5918(3) 0.2186(3) 0.1375(2) 0.0393(8) Uani 1 1 d . . . . .
C7 C 0.4831(3) 0.3631(3) 0.1925(2) 0.0434(9) Uani 1 1 d . . . . .
H7 H 0.489066 0.419597 0.187280 0.052 Uiso 1 1 calc R . . . .
C8 C 0.5326(3) 0.2496(3) 0.1687(2) 0.0352(8) Uani 1 1 d . . . . .
C9 C 0.5804(3) 0.1350(3) 0.1435(2) 0.0421(9) Uani 1 1 d . . . . .
H9 H 0.619593 0.114277 0.121577 0.051 Uiso 1 1 calc R . . . .
C10 C 0.4125(3) 0.3090(3) 0.2304(2) 0.0414(9) Uani 1 1 d . . . . .
H10 H 0.372021 0.329562 0.250804 0.050 Uiso 1 1 calc R . . . .
C11 C 0.4610(3) 0.1948(2) 0.2065(2) 0.0330(7) Uani 1 1 d . . . . .
C12 C 0.5114(3) 0.0811(3) 0.1818(2) 0.0399(9) Uani 1 1 d . . . . .
H12 H 0.505224 0.024419 0.186690 0.048 Uiso 1 1 calc R . . . .
C13 C 0.4018(3) 0.2254(3) 0.2382(2) 0.0342(8) Uani 1 1 d . . . . .
C15 C 0.3282(3) 0.1684(3) 0.2787(2) 0.0381(8) Uani 1 1 d . . . . .
C16 C 0.3788(3) 0.0514(3) 0.2524(2) 0.0376(8) Uani 1 1 d . . . . .
C17 C 0.2468(3) 0.0264(3) 0.3211(2) 0.0411(9) Uani 1 1 d . . . . .
H17A H 0.245164 0.060012 0.364295 0.049 Uiso 1 1 calc R . . . .
H17B H 0.267321 -0.018203 0.338713 0.049 Uiso 1 1 calc R . . . .
C18 C 0.1400(3) -0.0189(3) 0.2723(2) 0.0392(8) Uani 1 1 d . . . . .
C19 C 0.8638(3) 0.4646(3) 0.3504(2) 0.0413(9) Uani 1 1 d . . . . .
C20 C 0.7606(3) 0.4121(3) 0.2980(2) 0.0419(9) Uani 1 1 d . . . . .
H20A H 0.740795 0.452256 0.270584 0.050 Uiso 1 1 calc R . . . .
H20B H 0.767055 0.372195 0.262287 0.050 Uiso 1 1 calc R . . . .
C21 C 0.6295(3) 0.4027(3) 0.3632(2) 0.0383(8) Uani 1 1 d . . . . .
C22 C 0.6682(3) 0.2772(3) 0.3463(2) 0.0382(8) Uani 1 1 d . . . . .
C23 C 0.5556(3) 0.3526(3) 0.4062(2) 0.0373(8) Uani 1 1 d . . . . .
C24 C 0.5922(3) 0.2280(3) 0.3877(2) 0.0341(8) Uani 1 1 d . . . . .
C25 C 0.5003(3) 0.3890(3) 0.4345(2) 0.0392(9) Uani 1 1 d . . . . .
H25 H 0.511143 0.446216 0.426782 0.047 Uiso 1 1 calc R . . . .
C26 C 0.5381(3) 0.2665(2) 0.41639(19) 0.0311(7) Uani 1 1 d . . . . .
C27 C 0.5742(3) 0.1428(3) 0.3988(2) 0.0366(8) Uani 1 1 d . . . . .
H27 H 0.610003 0.116702 0.378915 0.044 Uiso 1 1 calc R . . . .
C28 C 0.4293(3) 0.3419(3) 0.4740(2) 0.0392(9) Uani 1 1 d . . . . .
H28 H 0.392296 0.367465 0.493033 0.047 Uiso 1 1 calc R . . . .
C29 C 0.4660(3) 0.2189(2) 0.4567(2) 0.0322(7) Uani 1 1 d . . . . .
C30 C 0.5038(3) 0.0966(3) 0.4391(2) 0.0360(8) Uani 1 1 d . . . . .
H30 H 0.492855 0.039330 0.446714 0.043 Uiso 1 1 calc R . . . .
C31 C 0.4120(3) 0.2578(3) 0.4857(2) 0.0361(8) Uani 1 1 d . . . . .
C32 C 0.4494(3) 0.1327(3) 0.4682(2) 0.0345(8) Uani 1 1 d . . . . .
C33 C 0.3373(3) 0.2089(3) 0.5283(2) 0.0370(8) Uani 1 1 d . . . . .
C34 C 0.3752(3) 0.0831(3) 0.5107(2) 0.0373(8) Uani 1 1 d . . . . .
C35 C 0.2449(3) 0.0741(3) 0.5764(2) 0.0386(8) Uani 1 1 d . . . . .
H35A H 0.241418 0.114234 0.613681 0.046 Uiso 1 1 calc R . . . .
H35B H 0.263511 0.032299 0.602113 0.046 Uiso 1 1 calc R . . . .
C36 C 0.1402(3) 0.0247(3) 0.5253(2) 0.0345(8) Uani 1 1 d . . . . .
C37 C 0.8623(3) 0.4937(3) 0.6048(2) 0.0443(9) Uani 1 1 d . . . . .
C38 C 0.7585(3) 0.4510(3) 0.5532(2) 0.0482(10) Uani 1 1 d . . . . .
H38A H 0.742944 0.496404 0.531447 0.058 Uiso 1 1 calc R . . . .
H38B H 0.760244 0.413262 0.512972 0.058 Uiso 1 1 calc R . . . .
C39 C 0.6278(3) 0.4395(3) 0.6192(2) 0.0414(9) Uani 1 1 d . . . . .
C40 C 0.6633(3) 0.3135(3) 0.5969(2) 0.0385(9) Uani 1 1 d . . . . .
C41 C 0.5511(3) 0.3874(3) 0.6597(2) 0.0371(8) Uani 1 1 d . . . . .
C42 C 0.5902(3) 0.2638(3) 0.6399(2) 0.0342(8) Uani 1 1 d . . . . .
C43 C 0.4971(3) 0.4234(3) 0.6894(2) 0.0390(8) Uani 1 1 d . . . . .
H43 H 0.508886 0.481203 0.683487 0.047 Uiso 1 1 calc R . . . .
C44 C 0.5353(3) 0.3016(2) 0.6695(2) 0.0331(8) Uani 1 1 d . . . . .
C45 C 0.5744(3) 0.1800(3) 0.6512(2) 0.0383(8) Uani 1 1 d . . . . .
H45 H 0.612356 0.155537 0.632022 0.046 Uiso 1 1 calc R . . . .
C46 C 0.4252(3) 0.3745(3) 0.7281(2) 0.0393(9) Uani 1 1 d . . . . .
H46 H 0.387891 0.399340 0.747612 0.047 Uiso 1 1 calc R . . . .
C47 C 0.4628(3) 0.2522(3) 0.70884(19) 0.0328(7) Uani 1 1 d . . . . .
C48 C 0.5029(3) 0.1310(3) 0.6906(2) 0.0381(8) Uani 1 1 d . . . . .
H48 H 0.492922 0.073843 0.697981 0.046 Uiso 1 1 calc R . . . .
C49 C 0.4079(3) 0.2898(3) 0.7384(2) 0.0353(8) Uani 1 1 d . . . . .
C50 C 0.4469(3) 0.1661(3) 0.7189(2) 0.0351(8) Uani 1 1 d . . . . .
C51 C 0.3316(3) 0.2390(3) 0.7791(2) 0.0377(8) Uani 1 1 d . . . . .
C52 C 0.3699(3) 0.1138(3) 0.7588(2) 0.0375(8) Uani 1 1 d . . . . .
C53 C 0.2375(3) 0.1020(3) 0.8228(2) 0.0395(8) Uani 1 1 d . . . . .
H53A H 0.231835 0.139592 0.861059 0.047 Uiso 1 1 calc R . . . .
H53B H 0.253915 0.058047 0.846622 0.047 Uiso 1 1 calc R . . . .
C54 C 0.1359(3) 0.0564(3) 0.7675(2) 0.0362(8) Uani 1 1 d . . . . .
C55 C 0.8604(3) 0.4974(3) 0.8575(2) 0.0449(10) Uani 1 1 d . . . . .
C56 C 0.7540(3) 0.4593(3) 0.8092(2) 0.0440(9) Uani 1 1 d . . . . .
H56A H 0.737874 0.507391 0.795060 0.053 Uiso 1 1 calc R . . . .
H56B H 0.753053 0.427388 0.764012 0.053 Uiso 1 1 calc R . . . .
C57 C 0.6678(3) 0.3167(3) 0.8477(2) 0.0400(9) Uani 1 1 d . . . . .
C58 C 0.6205(3) 0.4344(3) 0.8773(2) 0.0412(9) Uani 1 1 d . . . . .
C59 C 0.5948(3) 0.2596(3) 0.8873(2) 0.0355(8) Uani 1 1 d . . . . .
C60 C 0.5456(3) 0.3747(3) 0.9152(2) 0.0390(8) Uani 1 1 d . . . . .
C61 C 0.5843(3) 0.1759(3) 0.8940(2) 0.0411(9) Uani 1 1 d . . . . .
H61 H 0.625165 0.156219 0.873190 0.049 Uiso 1 1 calc R . . . .
C62 C 0.5350(3) 0.2889(3) 0.9196(2) 0.0348(8) Uani 1 1 d . . . . .
C63 C 0.4855(3) 0.4020(3) 0.9460(2) 0.0409(9) Uani 1 1 d . . . . .
H63 H 0.491617 0.458754 0.941991 0.049 Uiso 1 1 calc R . . . .
C64 C 0.5139(3) 0.1204(3) 0.9311(2) 0.0406(9) Uani 1 1 d . . . . .
H64 H 0.508149 0.063828 0.935414 0.049 Uiso 1 1 calc R . . . .
C65 C 0.4636(3) 0.2328(3) 0.9566(2) 0.0347(8) Uani 1 1 d . . . . .
C66 C 0.4150(3) 0.3464(3) 0.9833(2) 0.0405(9) Uani 1 1 d . . . . .
H66 H 0.374786 0.366194 1.004732 0.049 Uiso 1 1 calc R . . . .
C67 C 0.4528(3) 0.1474(3) 0.9617(2) 0.0402(9) Uani 1 1 d . . . . .
C68 C 0.4042(3) 0.2631(3) 0.9888(2) 0.0376(8) Uani 1 1 d . . . . .
C69 C 0.3762(3) 0.0879(3) 0.9985(2) 0.0431(9) Uani 1 1 d . . . . .
C70 C 0.3287(3) 0.2054(3) 1.0272(2) 0.0411(9) Uani 1 1 d . . . . .
C71 C 0.2421(3) 0.0628(3) 1.0653(2) 0.0433(9) Uani 1 1 d . . . . .
H71A H 0.238916 0.095626 1.108268 0.052 Uiso 1 1 calc R . . . .
H71B H 0.260709 0.017133 1.082919 0.052 Uiso 1 1 calc R . . . .
C72 C 0.1364(3) 0.0192(3) 1.0139(2) 0.0360(8) Uani 1 1 d . . . . .
C74 C 1.0929(4) 0.6827(4) 0.0624(4) 0.0712(16) Uani 1 1 d . . . . .
H74 H 1.084605 0.656642 0.105973 0.085 Uiso 1 1 calc R . . . .
C77 C 1.1481(6) 0.8114(5) 0.0026(6) 0.124(4) Uani 1 1 d . . . . .
H77A H 1.121735 0.767909 -0.040468 0.186 Uiso 1 1 calc GR . . . .
H77B H 1.220216 0.847216 0.006770 0.186 Uiso 1 1 calc GR . . . .
H77C H 1.112909 0.848071 -0.002286 0.186 Uiso 1 1 calc GR . . . .
C78 C 1.1597(5) 0.8197(5) 0.1387(5) 0.124(3) Uani 1 1 d . . . . .
H78A H 1.139038 0.781557 0.175987 0.185 Uiso 1 1 calc GR . . . .
H78B H 1.125947 0.857480 0.135770 0.185 Uiso 1 1 calc GR . . . .
H78C H 1.232755 0.855073 0.151643 0.185 Uiso 1 1 calc GR . . . .
C79 C 0.9023(6) 0.2790(6) 0.2177(5) 0.053(2) Uani 0.553(10) 1 d D U . A 1
H79 H 0.891918 0.290292 0.168494 0.064 Uiso 0.553(10) 1 calc R . . A 1
C80 C 0.9230(7) 0.2873(7) 0.2988(7) 0.049(3) Uani 0.447(10) 1 d . . . A 2
H80 H 0.936129 0.306703 0.349284 0.059 Uiso 0.447(10) 1 calc R . . A 2
C81 C 0.8465(16) 0.1585(10) 0.2057(10) 0.090(7) Uani 0.447(10) 1 d . . . A 2
H81A H 0.844991 0.200379 0.172143 0.134 Uiso 0.447(10) 1 calc GR . . A 2
H81B H 0.778543 0.111872 0.200318 0.134 Uiso 0.447(10) 1 calc GR . . A 2
H81C H 0.891289 0.134306 0.194177 0.134 Uiso 0.447(10) 1 calc GR . . A 2
C82 C 0.8595(12) 0.1465(10) 0.3373(10) 0.076(5) Uani 0.447(10) 1 d . . . A 2
H82A H 0.888338 0.181758 0.385217 0.114 Uiso 0.447(10) 1 calc GR . . A 2
H82B H 0.887522 0.104851 0.334344 0.114 Uiso 0.447(10) 1 calc GR . . A 2
H82C H 0.786291 0.115375 0.330788 0.114 Uiso 0.447(10) 1 calc GR . . A 2
C83 C 0.8257(9) 0.1286(7) 0.1676(7) 0.061(3) Uani 0.553(10) 1 d . U . A 1
H83A H 0.814804 0.153527 0.122675 0.092 Uiso 0.553(10) 1 calc GR . . A 1
H83B H 0.761229 0.084173 0.174107 0.092 Uiso 0.553(10) 1 calc GR . . A 1
H83C H 0.871510 0.102509 0.164280 0.092 Uiso 0.553(10) 1 calc GR . . A 1
C84 C 0.8757(12) 0.1726(10) 0.3007(8) 0.069(4) Uani 0.553(10) 1 d D U . A 1
H84A H 0.900447 0.224731 0.335693 0.103 Uiso 0.553(10) 1 calc GR . . A 1
H84B H 0.922319 0.146351 0.309779 0.103 Uiso 0.553(10) 1 calc GR . . A 1
H84C H 0.809101 0.131319 0.306376 0.103 Uiso 0.553(10) 1 calc GR . . A 1
C85 C 1.0766(4) 0.6698(4) 0.4343(4) 0.0735(17) Uani 1 1 d . . . . .
H85 H 1.051784 0.635769 0.387852 0.088 Uiso 1 1 calc R . . . .
C86 C 1.1740(6) 0.8194(5) 0.4930(7) 0.152(5) Uani 1 1 d . . . . .
H86A H 1.169762 0.795410 0.539465 0.228 Uiso 1 1 calc GR . . . .
H86B H 1.144462 0.860376 0.490387 0.228 Uiso 1 1 calc GR . . . .
H86C H 1.244642 0.849403 0.489810 0.228 Uiso 1 1 calc GR . . . .
C87 C 1.1303(7) 0.7789(6) 0.3607(7) 0.157(5) Uani 1 1 d . . . . .
H87A H 1.200982 0.802185 0.357233 0.236 Uiso 1 1 calc GR . . . .
H87B H 1.106782 0.823548 0.353053 0.236 Uiso 1 1 calc GR . . . .
H87C H 1.089615 0.728923 0.323355 0.236 Uiso 1 1 calc GR . . . .
C88 C 0.0679(3) 0.1847(3) 0.5382(3) 0.0461(10) Uani 1 1 d . . . . .
H88 H 0.043398 0.142398 0.496664 0.055 Uiso 1 1 calc R . . . .
C89 C 0.1611(5) 0.3367(3) 0.5865(3) 0.0681(15) Uani 1 1 d . . . . .
H89A H 0.127215 0.374432 0.583600 0.102 Uiso 1 1 calc GR . . . .
H89B H 0.231398 0.370285 0.583725 0.102 Uiso 1 1 calc GR . . . .
H89C H 0.158354 0.312444 0.632896 0.102 Uiso 1 1 calc GR . . . .
C90 C 0.1241(5) 0.2914(4) 0.4542(3) 0.0720(16) Uani 1 1 d . . . . .
H90A H 0.195822 0.318208 0.453531 0.108 Uiso 1 1 calc GR . . . .
H90B H 0.096013 0.332282 0.441958 0.108 Uiso 1 1 calc GR . . . .
H90C H 0.088867 0.239295 0.418414 0.108 Uiso 1 1 calc GR . . . .
C91 C -0.0774(4) -0.1619(4) 0.8935(3) 0.0673(15) Uani 1 1 d . . . . .
H91 H -0.058216 -0.143172 0.944438 0.081 Uiso 1 1 calc R . . . .
C92 C -0.1365(4) -0.2801(4) 0.7946(4) 0.0713(16) Uani 1 1 d . . . . .
H92A H -0.209104 -0.317440 0.782028 0.107 Uiso 1 1 calc GR . . . .
H92B H -0.100542 -0.313260 0.783592 0.107 Uiso 1 1 calc GR . . . .
H92C H -0.120725 -0.231297 0.766060 0.107 Uiso 1 1 calc GR . . . .
C93 C -0.1107(6) -0.3063(4) 0.9239(4) 0.095(2) Uani 1 1 d . . . . .
H93A H -0.181012 -0.346491 0.921808 0.142 Uiso 1 1 calc GR . . . .
H93B H -0.080353 -0.272917 0.972471 0.142 Uiso 1 1 calc GR . . . .
H93C H -0.073673 -0.339009 0.914021 0.142 Uiso 1 1 calc GR . . . .
C94 C 0.0702(3) 0.2046(3) 0.8324(3) 0.0450(9) Uani 1 1 d . . . . .
H94 H 0.038121 0.176249 0.784126 0.054 Uiso 1 1 calc R . . . .
C95 C 0.1166(5) 0.3385(4) 0.7801(4) 0.0804(18) Uani 1 1 d . . . . .
H95A H 0.186602 0.375726 0.778644 0.121 Uiso 1 1 calc GR . . . .
H95B H 0.081203 0.374187 0.784549 0.121 Uiso 1 1 calc GR . . . .
H95C H 0.083622 0.297815 0.735128 0.121 Uiso 1 1 calc GR . . . .
C96 C 0.1740(4) 0.3393(3) 0.9109(3) 0.0638(14) Uani 1 1 d . . . . .
H96A H 0.140442 0.370011 0.930890 0.096 Uiso 1 1 calc GR . . . .
H96B H 0.239854 0.381192 0.904327 0.096 Uiso 1 1 calc GR . . . .
H96C H 0.183024 0.299913 0.944622 0.096 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.107(3) 2_765 ?
Co1 O1 2.107(3) . ?
Co1 O26 2.120(3) 1_554 ?
Co1 O26 2.120(3) 2_766 ?
Co1 O33 2.082(3) . ?
Co1 O33 2.082(3) 2_765 ?
Co2 O2 2.098(3) . ?
Co2 O9 2.051(3) . ?
Co2 O18 2.062(4) 2_766 ?
Co2 O25 2.033(3) 2_766 ?
Co2 O34 2.294(9) . ?
Co2 O35 2.054(4) . ?
Co3 O10 2.127(3) 2_766 ?
Co3 O10 2.127(3) . ?
Co3 O17 2.095(3) . ?
Co3 O17 2.095(3) 2_766 ?
Co3 O38 2.113(4) 2_766 ?
Co3 O38 2.113(4) . ?
Co4 O8 2.084(3) 2_556 ?
Co4 O15 2.088(3) 2_556 ?
Co4 O16 2.075(3) . ?
Co4 O23 2.106(3) . ?
Co4 O36 2.109(3) . ?
Co4 O37 2.218(3) . ?
Co5 O7 2.146(3) 2_556 ?
Co5 O24 2.078(3) . ?
Co5 O31 2.130(3) . ?
Co5 O32 2.058(3) 2_557 ?
Co5 O39 2.107(3) . ?
Co5 O40 2.078(4) . ?
O1 C1 1.252(5) . ?
O2 C1 1.240(5) . ?
O3 C3 1.235(5) . ?
O4 C4 1.216(5) . ?
O5 C15 1.215(4) . ?
O6 C16 1.226(5) . ?
O7 C18 1.250(5) . ?
O8 C18 1.261(5) . ?
O9 C19 1.254(5) . ?
O10 C19 1.236(5) . ?
O11 C21 1.228(5) . ?
O12 C22 1.218(5) . ?
O13 C33 1.212(4) . ?
O14 C34 1.234(5) . ?
O15 C36 1.248(4) . ?
O16 C36 1.261(4) . ?
O17 C37 1.245(5) . ?
O18 C37 1.268(5) . ?
O19 C39 1.232(5) . ?
O20 C40 1.217(5) . ?
O21 C51 1.213(5) . ?
O22 C52 1.227(5) . ?
O23 C54 1.249(5) . ?
O24 C54 1.257(5) . ?
O25 C55 1.261(5) . ?
O26 C55 1.247(5) . ?
O27 C58 1.224(5) . ?
O28 C57 1.222(5) . ?
O29 C70 1.210(5) . ?
O30 C69 1.234(5) . ?
O31 C72 1.238(5) . ?
O32 C72 1.257(5) . ?
O33 C74 1.236(7) . ?
O35 C79 1.161(9) . ?
O35 C80 1.116(10) . ?
O36 C88 1.243(5) . ?
O38 C85 1.175(7) . ?
O39 C94 1.254(5) . ?
O40 C91 1.154(7) . ?
N1 C2 1.468(5) . ?
N1 C3 1.400(6) . ?
N1 C4 1.402(6) . ?
N2 C15 1.417(5) . ?
N2 C16 1.403(5) . ?
N2 C17 1.472(5) . ?
N3 C20 1.469(5) . ?
N3 C21 1.397(5) . ?
N3 C22 1.414(5) . ?
N4 C33 1.420(5) . ?
N4 C34 1.392(5) . ?
N4 C35 1.464(5) . ?
N5 C38 1.469(5) . ?
N5 C39 1.392(5) . ?
N5 C40 1.415(5) . ?
N6 C51 1.411(5) . ?
N6 C52 1.400(5) . ?
N6 C53 1.460(5) . ?
N7 C56 1.470(5) . ?
N7 C57 1.412(5) . ?
N7 C58 1.405(5) . ?
N8 C69 1.400(5) . ?
N8 C70 1.407(6) . ?
N8 C71 1.471(5) . ?
N9 C80 1.336(18) . ?
N9 C81 1.46(2) . ?
N9 C82 1.445(17) . ?
N10 C79 1.351(12) . ?
N10 C83 1.430(16) . ?
N10 C84 1.422(12) . ?
N11 C74 1.322(7) . ?
N11 C77 1.474(9) . ?
N11 C78 1.452(9) . ?
N12 C85 1.278(7) . ?
N12 C86 1.415(11) . ?
N12 C87 1.493(12) . ?
N13 C88 1.342(6) . ?
N13 C89 1.433(7) . ?
N13 C90 1.465(7) . ?
N14 C94 1.337(6) . ?
N14 C95 1.446(7) . ?
N14 C96 1.426(7) . ?
N15 C91 1.394(7) . ?
N15 C92 1.417(8) . ?
N15 C93 1.436(8) . ?
C0AA C11 1.423(5) . ?
C0AA C12 1.399(5) . ?
C0AA C16 1.472(5) . ?
C1 C2 1.547(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C5 1.486(6) . ?
C4 C6 1.486(6) . ?
C5 C7 1.374(6) . ?
C5 C8 1.433(6) . ?
C6 C8 1.415(5) . ?
C6 C9 1.389(6) . ?
C7 H7 0.9500 . ?
C7 C10 1.410(6) . ?
C8 C11 1.421(5) . ?
C9 H9 0.9500 . ?
C9 C12 1.400(5) . ?
C10 H10 0.9500 . ?
C10 C13 1.397(5) . ?
C11 C13 1.413(5) . ?
C12 H12 0.9500 . ?
C13 C15 1.486(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.542(6) . ?
C19 C20 1.544(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C23 1.483(5) . ?
C22 C24 1.476(5) . ?
C23 C25 1.397(5) . ?
C23 C26 1.421(5) . ?
C24 C26 1.409(5) . ?
C24 C27 1.406(5) . ?
C25 H25 0.9500 . ?
C25 C28 1.395(5) . ?
C26 C29 1.419(5) . ?
C27 H27 0.9500 . ?
C27 C30 1.395(5) . ?
C28 H28 0.9500 . ?
C28 C31 1.394(5) . ?
C29 C31 1.416(5) . ?
C29 C32 1.431(5) . ?
C30 H30 0.9500 . ?
C30 C32 1.390(5) . ?
C31 C33 1.479(5) . ?
C32 C34 1.475(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.542(6) . ?
C37 C38 1.530(7) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C41 1.484(5) . ?
C40 C42 1.474(5) . ?
C41 C43 1.388(5) . ?
C41 C44 1.420(5) . ?
C42 C44 1.419(5) . ?
C42 C45 1.393(5) . ?
C43 H43 0.9500 . ?
C43 C46 1.402(5) . ?
C44 C47 1.419(5) . ?
C45 H45 0.9500 . ?
C45 C48 1.409(5) . ?
C46 H46 0.9500 . ?
C46 C49 1.398(6) . ?
C47 C49 1.419(5) . ?
C47 C50 1.424(5) . ?
C48 H48 0.9500 . ?
C48 C50 1.391(5) . ?
C49 C51 1.478(5) . ?
C50 C52 1.483(5) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.541(6) . ?
C55 C56 1.534(6) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C59 1.470(5) . ?
C58 C60 1.482(5) . ?
C59 C61 1.395(6) . ?
C59 C62 1.414(5) . ?
C60 C62 1.425(5) . ?
C60 C63 1.383(5) . ?
C61 H61 0.9500 . ?
C61 C64 1.407(6) . ?
C62 C65 1.418(5) . ?
C63 H63 0.9500 . ?
C63 C66 1.410(6) . ?
C64 H64 0.9500 . ?
C64 C67 1.389(6) . ?
C65 C67 1.419(6) . ?
C65 C68 1.419(5) . ?
C66 H66 0.9500 . ?
C66 C68 1.384(6) . ?
C67 C69 1.483(6) . ?
C68 C70 1.481(5) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C71 C72 1.549(6) . ?
C74 H74 0.9500 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 H79 0.9500 . ?
C80 H80 0.9500 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C85 H85 0.9500 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C88 H88 0.9500 . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
C91 H91 0.9500 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?
C94 H94 0.9500 . ?
C95 H95A 0.9800 . ?
C95 H95B 0.9800 . ?
C95 H95C 0.9800 . ?
C96 H96A 0.9800 . ?
C96 H96B 0.9800 . ?
C96 H96C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O1 180.0 2_765 . ?
O1 Co1 O26 88.66(12) 2_765 2_766 ?
O1 Co1 O26 91.34(12) . 2_766 ?
O1 Co1 O26 88.66(12) . 1_554 ?
O1 Co1 O26 91.34(12) 2_765 1_554 ?
O26 Co1 O26 180.0(2) 1_554 2_766 ?
O33 Co1 O1 88.14(12) . . ?
O33 Co1 O1 91.86(12) . 2_765 ?
O33 Co1 O1 88.14(12) 2_765 2_765 ?
O33 Co1 O1 91.86(12) 2_765 . ?
O33 Co1 O26 94.26(13) . 1_554 ?
O33 Co1 O26 94.26(13) 2_765 2_766 ?
O33 Co1 O26 85.74(13) 2_765 1_554 ?
O33 Co1 O26 85.74(13) . 2_766 ?
O33 Co1 O33 180.0 . 2_765 ?
O2 Co2 O34 88.2(3) . . ?
O9 Co2 O2 85.39(13) . . ?
O9 Co2 O18 90.99(13) . 2_766 ?
O9 Co2 O34 87.7(3) . . ?
O9 Co2 O35 99.81(14) . . ?
O18 Co2 O2 172.25(13) 2_766 . ?
O18 Co2 O34 84.8(3) 2_766 . ?
O25 Co2 O2 90.44(13) 2_766 . ?
O25 Co2 O9 166.74(13) 2_766 . ?
O25 Co2 O18 91.58(13) 2_766 2_766 ?
O25 Co2 O34 79.6(3) 2_766 . ?
O25 Co2 O35 92.53(15) 2_766 . ?
O35 Co2 O2 87.23(15) . . ?
O35 Co2 O18 100.15(15) . 2_766 ?
O35 Co2 O34 170.9(3) . . ?
O10 Co3 O10 180.0 . 2_766 ?
O17 Co3 O10 88.82(13) 2_766 . ?
O17 Co3 O10 88.82(13) . 2_766 ?
O17 Co3 O10 91.18(13) 2_766 2_766 ?
O17 Co3 O10 91.18(13) . . ?
O17 Co3 O17 180.0(2) . 2_766 ?
O17 Co3 O38 94.60(14) 2_766 . ?
O17 Co3 O38 85.40(14) . . ?
O17 Co3 O38 94.60(14) . 2_766 ?
O17 Co3 O38 85.40(14) 2_766 2_766 ?
O38 Co3 O10 95.52(15) 2_766 2_766 ?
O38 Co3 O10 95.52(15) . . ?
O38 Co3 O10 84.48(15) . 2_766 ?
O38 Co3 O10 84.48(15) 2_766 . ?
O38 Co3 O38 180.0 2_766 . ?
O8 Co4 O15 91.87(11) 2_556 2_556 ?
O8 Co4 O23 91.17(12) 2_556 . ?
O8 Co4 O36 88.69(12) 2_556 . ?
O8 Co4 O37 83.95(12) 2_556 . ?
O15 Co4 O23 174.64(12) 2_556 . ?
O15 Co4 O36 99.01(13) 2_556 . ?
O15 Co4 O37 85.84(13) 2_556 . ?
O16 Co4 O8 174.00(11) . 2_556 ?
O16 Co4 O15 90.40(11) . 2_556 ?
O16 Co4 O23 86.15(11) . . ?
O16 Co4 O36 96.43(12) . . ?
O16 Co4 O37 90.69(12) . . ?
O23 Co4 O36 85.47(13) . . ?
O23 Co4 O37 90.09(13) . . ?
O36 Co4 O37 171.33(13) . . ?
O24 Co5 O7 89.76(11) . 2_556 ?
O24 Co5 O31 87.72(11) . . ?
O24 Co5 O39 95.14(12) . . ?
O24 Co5 O40 80.69(13) . . ?
O31 Co5 O7 177.36(9) . 2_556 ?
O32 Co5 O7 91.93(11) 2_557 2_556 ?
O32 Co5 O24 175.97(11) 2_557 . ?
O32 Co5 O31 90.64(11) 2_557 . ?
O32 Co5 O39 88.39(12) 2_557 . ?
O32 Co5 O40 95.93(13) 2_557 . ?
O39 Co5 O7 93.91(13) . 2_556 ?
O39 Co5 O31 85.55(12) . . ?
O40 Co5 O7 81.62(14) . 2_556 ?
O40 Co5 O31 98.72(14) . . ?
O40 Co5 O39 173.86(14) . . ?
C1 O1 Co1 131.3(3) . . ?
C1 O2 Co2 128.4(3) . . ?
C18 O7 Co5 131.2(3) . 2_556 ?
C18 O8 Co4 131.8(3) . 2_556 ?
C19 O9 Co2 130.2(3) . . ?
C19 O10 Co3 126.6(3) . . ?
C36 O15 Co4 126.2(3) . 2_556 ?
C36 O16 Co4 133.7(3) . . ?
C37 O17 Co3 133.1(3) . . ?
C37 O18 Co2 124.4(3) . 2_766 ?
C54 O23 Co4 124.3(3) . . ?
C54 O24 Co5 130.0(3) . . ?
C55 O25 Co2 136.0(3) . 2_766 ?
C55 O26 Co1 130.1(3) . 1_556 ?
C72 O31 Co5 128.5(2) . . ?
C72 O32 Co5 134.5(3) . 2_557 ?
C74 O33 Co1 122.6(4) . . ?
C79 O35 Co2 129.2(6) . . ?
C80 O35 Co2 149.0(8) . . ?
C88 O36 Co4 128.7(3) . . ?
C85 O38 Co3 134.7(5) . . ?
C94 O39 Co5 127.8(3) . . ?
C91 O40 Co5 129.0(4) . . ?
C3 N1 C2 118.9(4) . . ?
C3 N1 C4 124.6(4) . . ?
C4 N1 C2 116.3(4) . . ?
C15 N2 C17 117.0(3) . . ?
C16 N2 C15 125.1(3) . . ?
C16 N2 C17 117.7(3) . . ?
C21 N3 C20 118.1(3) . . ?
C21 N3 C22 124.9(3) . . ?
C22 N3 C20 116.7(3) . . ?
C33 N4 C35 116.4(3) . . ?
C34 N4 C33 124.8(3) . . ?
C34 N4 C35 118.7(3) . . ?
C39 N5 C38 118.2(4) . . ?
C39 N5 C40 124.9(3) . . ?
C40 N5 C38 116.7(3) . . ?
C51 N6 C53 116.7(3) . . ?
C52 N6 C51 125.0(3) . . ?
C52 N6 C53 117.9(3) . . ?
C57 N7 C56 116.5(3) . . ?
C58 N7 C56 118.4(4) . . ?
C58 N7 C57 124.7(3) . . ?
C69 N8 C70 125.1(3) . . ?
C69 N8 C71 118.0(4) . . ?
C70 N8 C71 116.6(3) . . ?
C80 N9 C81 124.1(13) . . ?
C80 N9 C82 118.8(13) . . ?
C82 N9 C81 116.2(15) . . ?
C79 N10 C83 120.2(10) . . ?
C79 N10 C84 120.0(12) . . ?
C84 N10 C83 119.8(10) . . ?
C74 N11 C77 119.4(6) . . ?
C74 N11 C78 121.3(7) . . ?
C78 N11 C77 119.3(6) . . ?
C85 N12 C86 130.9(9) . . ?
C85 N12 C87 113.8(8) . . ?
C86 N12 C87 114.6(7) . . ?
C88 N13 C89 121.9(5) . . ?
C88 N13 C90 120.8(5) . . ?
C89 N13 C90 116.7(4) . . ?
C94 N14 C95 120.3(5) . . ?
C94 N14 C96 121.8(4) . . ?
C96 N14 C95 117.0(5) . . ?
C91 N15 C92 120.7(5) . . ?
C91 N15 C93 118.6(6) . . ?
C92 N15 C93 120.6(5) . . ?
C11 C0AA C16 120.6(3) . . ?
C12 C0AA C11 120.0(3) . . ?
C12 C0AA C16 119.5(3) . . ?
O1 C1 C2 115.8(4) . . ?
O2 C1 O1 126.4(4) . . ?
O2 C1 C2 117.6(4) . . ?
N1 C2 C1 113.6(4) . . ?
N1 C2 H2A 108.8 . . ?
N1 C2 H2B 108.8 . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
O3 C3 N1 121.0(4) . . ?
O3 C3 C5 121.0(4) . . ?
N1 C3 C5 118.0(4) . . ?
O4 C4 N1 119.7(4) . . ?
O4 C4 C6 123.0(4) . . ?
N1 C4 C6 117.3(4) . . ?
C7 C5 C3 121.6(4) . . ?
C7 C5 C8 119.5(4) . . ?
C8 C5 C3 119.0(4) . . ?
C8 C6 C4 120.1(4) . . ?
C9 C6 C4 119.5(4) . . ?
C9 C6 C8 120.4(4) . . ?
C5 C7 H7 119.3 . . ?
C5 C7 C10 121.4(4) . . ?
C10 C7 H7 119.3 . . ?
C6 C8 C5 121.0(4) . . ?
C6 C8 C11 119.8(4) . . ?
C11 C8 C5 119.2(4) . . ?
C6 C9 H9 119.9 . . ?
C6 C9 C12 120.2(4) . . ?
C12 C9 H9 119.9 . . ?
C7 C10 H10 119.8 . . ?
C13 C10 C7 120.3(4) . . ?
C13 C10 H10 119.8 . . ?
C8 C11 C0AA 119.0(3) . . ?
C13 C11 C0AA 120.9(3) . . ?
C13 C11 C8 120.1(3) . . ?
C0AA C12 C9 120.6(4) . . ?
C0AA C12 H12 119.7 . . ?
C9 C12 H12 119.7 . . ?
C10 C13 C11 119.5(3) . . ?
C10 C13 C15 120.6(3) . . ?
C11 C13 C15 119.9(3) . . ?
O5 C15 N2 119.8(4) . . ?
O5 C15 C13 123.5(4) . . ?
N2 C15 C13 116.7(3) . . ?
O6 C16 N2 120.1(3) . . ?
O6 C16 C0AA 123.2(3) . . ?
N2 C16 C0AA 116.7(3) . . ?
N2 C17 H17A 108.8 . . ?
N2 C17 H17B 108.8 . . ?
N2 C17 C18 113.8(3) . . ?
H17A C17 H17B 107.7 . . ?
C18 C17 H17A 108.8 . . ?
C18 C17 H17B 108.8 . . ?
O7 C18 O8 127.5(4) . . ?
O7 C18 C17 117.6(3) . . ?
O8 C18 C17 114.9(3) . . ?
O9 C19 C20 114.1(4) . . ?
O10 C19 O9 128.1(4) . . ?
O10 C19 C20 117.7(4) . . ?
N3 C20 C19 113.3(3) . . ?
N3 C20 H20A 108.9 . . ?
N3 C20 H20B 108.9 . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
O11 C21 N3 120.8(4) . . ?
O11 C21 C23 122.3(4) . . ?
N3 C21 C23 116.9(3) . . ?
O12 C22 N3 120.1(3) . . ?
O12 C22 C24 122.8(4) . . ?
N3 C22 C24 117.1(3) . . ?
C25 C23 C21 120.0(3) . . ?
C25 C23 C26 119.9(3) . . ?
C26 C23 C21 120.1(3) . . ?
C26 C24 C22 120.1(3) . . ?
C27 C24 C22 119.9(3) . . ?
C27 C24 C26 120.0(3) . . ?
C23 C25 H25 119.8 . . ?
C28 C25 C23 120.5(4) . . ?
C28 C25 H25 119.8 . . ?
C24 C26 C23 120.9(3) . . ?
C24 C26 C29 119.7(3) . . ?
C29 C26 C23 119.4(3) . . ?
C24 C27 H27 119.9 . . ?
C30 C27 C24 120.2(3) . . ?
C30 C27 H27 119.9 . . ?
C25 C28 H28 119.7 . . ?
C31 C28 C25 120.7(3) . . ?
C31 C28 H28 119.7 . . ?
C26 C29 C32 119.6(3) . . ?
C31 C29 C26 119.6(3) . . ?
C31 C29 C32 120.8(3) . . ?
C27 C30 H30 119.4 . . ?
C32 C30 C27 121.2(3) . . ?
C32 C30 H30 119.4 . . ?
C28 C31 C29 120.0(3) . . ?
C28 C31 C33 120.2(3) . . ?
C29 C31 C33 119.8(3) . . ?
C29 C32 C34 120.0(3) . . ?
C30 C32 C29 119.3(3) . . ?
C30 C32 C34 120.7(3) . . ?
O13 C33 N4 120.1(3) . . ?
O13 C33 C31 122.8(4) . . ?
N4 C33 C31 117.1(3) . . ?
O14 C34 N4 120.0(3) . . ?
O14 C34 C32 122.5(3) . . ?
N4 C34 C32 117.4(3) . . ?
N4 C35 H35A 108.9 . . ?
N4 C35 H35B 108.9 . . ?
N4 C35 C36 113.3(3) . . ?
H35A C35 H35B 107.7 . . ?
C36 C35 H35A 108.9 . . ?
C36 C35 H35B 108.9 . . ?
O15 C36 O16 127.1(4) . . ?
O15 C36 C35 118.1(3) . . ?
O16 C36 C35 114.8(3) . . ?
O17 C37 O18 126.5(5) . . ?
O17 C37 C38 115.5(4) . . ?
O18 C37 C38 117.9(4) . . ?
N5 C38 C37 113.2(4) . . ?
N5 C38 H38A 108.9 . . ?
N5 C38 H38B 108.9 . . ?
C37 C38 H38A 108.9 . . ?
C37 C38 H38B 108.9 . . ?
H38A C38 H38B 107.7 . . ?
O19 C39 N5 120.1(4) . . ?
O19 C39 C41 122.6(4) . . ?
N5 C39 C41 117.3(3) . . ?
O20 C40 N5 120.1(3) . . ?
O20 C40 C42 122.7(4) . . ?
N5 C40 C42 117.2(3) . . ?
C43 C41 C39 120.1(4) . . ?
C43 C41 C44 120.3(3) . . ?
C44 C41 C39 119.7(3) . . ?
C44 C42 C40 119.8(3) . . ?
C45 C42 C40 120.2(3) . . ?
C45 C42 C44 120.1(3) . . ?
C41 C43 H43 119.9 . . ?
C41 C43 C46 120.1(4) . . ?
C46 C43 H43 119.9 . . ?
C42 C44 C41 121.1(3) . . ?
C42 C44 C47 119.2(3) . . ?
C47 C44 C41 119.7(3) . . ?
C42 C45 H45 119.6 . . ?
C42 C45 C48 120.8(3) . . ?
C48 C45 H45 119.6 . . ?
C43 C46 H46 119.6 . . ?
C49 C46 C43 120.8(3) . . ?
C49 C46 H46 119.6 . . ?
C44 C47 C49 119.3(3) . . ?
C44 C47 C50 119.8(3) . . ?
C49 C47 C50 120.9(3) . . ?
C45 C48 H48 120.0 . . ?
C50 C48 C45 120.1(4) . . ?
C50 C48 H48 120.0 . . ?
C46 C49 C47 119.8(3) . . ?
C46 C49 C51 120.2(3) . . ?
C47 C49 C51 120.0(3) . . ?
C47 C50 C52 119.9(3) . . ?
C48 C50 C47 120.1(3) . . ?
C48 C50 C52 120.1(3) . . ?
O21 C51 N6 120.2(3) . . ?
O21 C51 C49 122.7(4) . . ?
N6 C51 C49 117.1(3) . . ?
O22 C52 N6 120.7(4) . . ?
O22 C52 C50 122.2(4) . . ?
N6 C52 C50 117.1(3) . . ?
N6 C53 H53A 109.3 . . ?
N6 C53 H53B 109.3 . . ?
N6 C53 C54 111.8(3) . . ?
H53A C53 H53B 107.9 . . ?
C54 C53 H53A 109.3 . . ?
C54 C53 H53B 109.3 . . ?
O23 C54 O24 125.7(4) . . ?
O23 C54 C53 118.4(3) . . ?
O24 C54 C53 115.9(3) . . ?
O25 C55 C56 115.8(4) . . ?
O26 C55 O25 126.2(4) . . ?
O26 C55 C56 117.8(4) . . ?
N7 C56 C55 114.3(3) . . ?
N7 C56 H56A 108.7 . . ?
N7 C56 H56B 108.7 . . ?
C55 C56 H56A 108.7 . . ?
C55 C56 H56B 108.7 . . ?
H56A C56 H56B 107.6 . . ?
O28 C57 N7 119.1(4) . . ?
O28 C57 C59 123.7(4) . . ?
N7 C57 C59 117.2(3) . . ?
O27 C58 N7 120.6(4) . . ?
O27 C58 C60 122.6(4) . . ?
N7 C58 C60 116.8(4) . . ?
C61 C59 C57 120.3(3) . . ?
C61 C59 C62 119.2(3) . . ?
C62 C59 C57 120.5(4) . . ?
C62 C60 C58 120.2(3) . . ?
C63 C60 C58 120.0(4) . . ?
C63 C60 C62 119.9(4) . . ?
C59 C61 H61 119.6 . . ?
C59 C61 C64 120.7(4) . . ?
C64 C61 H61 119.6 . . ?
C59 C62 C60 120.5(3) . . ?
C59 C62 C65 120.0(4) . . ?
C65 C62 C60 119.5(3) . . ?
C60 C63 H63 119.7 . . ?
C60 C63 C66 120.6(4) . . ?
C66 C63 H63 119.7 . . ?
C61 C64 H64 119.6 . . ?
C67 C64 C61 120.8(4) . . ?
C67 C64 H64 119.6 . . ?
C62 C65 C67 119.9(4) . . ?
C62 C65 C68 119.4(4) . . ?
C68 C65 C67 120.7(3) . . ?
C63 C66 H66 119.8 . . ?
C68 C66 C63 120.5(4) . . ?
C68 C66 H66 119.8 . . ?
C64 C67 C65 119.3(4) . . ?
C64 C67 C69 120.8(4) . . ?
C65 C67 C69 120.0(4) . . ?
C65 C68 C70 120.3(4) . . ?
C66 C68 C65 120.2(3) . . ?
C66 C68 C70 119.5(4) . . ?
O30 C69 N8 121.3(4) . . ?
O30 C69 C67 121.6(4) . . ?
N8 C69 C67 117.1(4) . . ?
O29 C70 N8 119.8(4) . . ?
O29 C70 C68 123.4(4) . . ?
N8 C70 C68 116.8(4) . . ?
N8 C71 H71A 108.7 . . ?
N8 C71 H71B 108.7 . . ?
N8 C71 C72 114.1(3) . . ?
H71A C71 H71B 107.6 . . ?
C72 C71 H71A 108.7 . . ?
C72 C71 H71B 108.7 . . ?
O31 C72 O32 127.3(4) . . ?
O31 C72 C71 117.6(3) . . ?
O32 C72 C71 115.0(3) . . ?
O33 C74 N11 125.3(6) . . ?
O33 C74 H74 117.4 . . ?
N11 C74 H74 117.4 . . ?
N11 C77 H77A 109.5 . . ?
N11 C77 H77B 109.5 . . ?
N11 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
N11 C78 H78A 109.5 . . ?
N11 C78 H78B 109.5 . . ?
N11 C78 H78C 109.5 . . ?
H78A C78 H78B 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
O35 C79 N10 126.8(10) . . ?
O35 C79 H79 116.6 . . ?
N10 C79 H79 116.6 . . ?
O35 C80 N9 128.3(13) . . ?
O35 C80 H80 115.9 . . ?
N9 C80 H80 115.9 . . ?
N9 C81 H81A 109.5 . . ?
N9 C81 H81B 109.5 . . ?
N9 C81 H81C 109.5 . . ?
H81A C81 H81B 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
N9 C82 H82A 109.5 . . ?
N9 C82 H82B 109.5 . . ?
N9 C82 H82C 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
N10 C83 H83A 109.5 . . ?
N10 C83 H83B 109.5 . . ?
N10 C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
N10 C84 H84A 109.5 . . ?
N10 C84 H84B 109.5 . . ?
N10 C84 H84C 109.5 . . ?
H84A C84 H84B 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
O38 C85 N12 127.2(8) . . ?
O38 C85 H85 116.4 . . ?
N12 C85 H85 116.4 . . ?
N12 C86 H86A 109.5 . . ?
N12 C86 H86B 109.5 . . ?
N12 C86 H86C 109.5 . . ?
H86A C86 H86B 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
N12 C87 H87A 109.5 . . ?
N12 C87 H87B 109.5 . . ?
N12 C87 H87C 109.5 . . ?
H87A C87 H87B 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
O36 C88 N13 125.6(5) . . ?
O36 C88 H88 117.2 . . ?
N13 C88 H88 117.2 . . ?
N13 C89 H89A 109.5 . . ?
N13 C89 H89B 109.5 . . ?
N13 C89 H89C 109.5 . . ?
H89A C89 H89B 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
N13 C90 H90A 109.5 . . ?
N13 C90 H90B 109.5 . . ?
N13 C90 H90C 109.5 . . ?
H90A C90 H90B 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
O40 C91 N15 123.2(6) . . ?
O40 C91 H91 118.4 . . ?
N15 C91 H91 118.4 . . ?
N15 C92 H92A 109.5 . . ?
N15 C92 H92B 109.5 . . ?
N15 C92 H92C 109.5 . . ?
H92A C92 H92B 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
N15 C93 H93A 109.5 . . ?
N15 C93 H93B 109.5 . . ?
N15 C93 H93C 109.5 . . ?
H93A C93 H93B 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
O39 C94 N14 124.6(5) . . ?
O39 C94 H94 117.7 . . ?
N14 C94 H94 117.7 . . ?
N14 C95 H95A 109.5 . . ?
N14 C95 H95B 109.5 . . ?
N14 C95 H95C 109.5 . . ?
H95A C95 H95B 109.5 . . ?
H95A C95 H95C 109.5 . . ?
H95B C95 H95C 109.5 . . ?
N14 C96 H96A 109.5 . . ?
N14 C96 H96B 109.5 . . ?
N14 C96 H96C 109.5 . . ?
H96A C96 H96B 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_DIFMX02_1                   
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: Poor data quality leaves large residuals near metals
;
_vrf_RINTA01_1                   
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: Poor data quality was the best obtainable even with synchrotron radiation.
;
_vrf_PLAT020_1                   
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.121 Report
RESPONSE: Poor data quality was the best obtainable even with synchrotron radiation.
;
_vrf_PLAT041_1                   
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: H2O hydrogen atoms not in model, but included in formula.
;
_vrf_PLAT043_1                   
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       6.03 Check 
RESPONSE: H2O hydrogen atoms not in model, but included in formula.
;
_vrf_PLAT084_1                   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.27 Report
RESPONSE: Poor data quality was the best obtainable even with synchrotron radiation.
;
_vrf_PLAT094_1                   
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       3.07 Report
RESPONSE: Poor data quality leaves large residuals near metals
;
_vrf_PLAT220_1                   
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        5.1 Ratio 
RESPONSE: Some disorder in coordinated solvent molecules.
;
_vrf_PLAT222_1                   
;
PROBLEM: Non-Solv.  Resd 1  H   Uiso(max)/Uiso(min) Range        5.5 Ratio 
RESPONSE: ...
;
_vrf_PLAT242_1                   
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Co2 Check 
RESPONSE: Some disorder in coordinated solvent molecules.
;
_exptl_crystal_recrystallization_method 
'Crystallised at elevated temperature from synthesis'
####################################################################### 
# 
# 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_2Co
_database_code_depnum_ccdc_archive 'CCDC 1840386'
_audit_update_record             
;
2018-04-30 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_audit_creation_date             2018-01-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H16 Co N4 O16, 2(C2 H8 N)'
_chemical_formula_sum            'C40 H32 Co N6 O16'
_chemical_formula_weight         911.64
_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 0.0030 0.0020 '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'
Co Co 0.3570 0.9660 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0070 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0120 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.464(3)
_cell_length_b                   9.1800(18)
_cell_length_c                   25.501(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.94(3)
_cell_angle_gamma                90
_cell_volume                     3770.8(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    28009
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.498
_cell_measurement_theta_min      2.529
_shelx_estimated_absorpt_T_max   0.973
_shelx_estimated_absorpt_T_min   0.968
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28009
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.529
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3801
_reflns_number_total             4236
_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       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4236
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0508
_refine_ls_restrained_S_all      1.051
_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)+(0.0741P)²+6.6596P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1385
_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
 N3-H3A = N3-H3B
 0.84 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C11(H11A,H11B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C16(H16), C18(H18)
3.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Co1 Co 0.500000 0.18949(5) 0.750000 0.02779(14) Uani 1 2 d S T P . .
O1 O 0.57699(11) 0.3182(2) 0.72295(7) 0.0381(4) Uani 1 1 d . . . . .
O2 O 0.67945(13) 0.3753(3) 0.68347(9) 0.0580(6) Uani 1 1 d . . . . .
O3 O 0.54419(11) 0.3787(3) 0.56199(8) 0.0481(5) Uani 1 1 d . . . . .
O4 O 0.73217(12) 0.0479(2) 0.64486(8) 0.0468(5) Uani 1 1 d . . . . .
O5 O 0.44239(11) 0.0876(2) 0.68577(7) 0.0441(5) Uani 1 1 d . . . . .
O6 O 0.35492(12) -0.0003(3) 0.73355(7) 0.0525(5) Uani 1 1 d . . . . .
O7 O 0.29584(13) 0.1258(4) 0.56419(10) 0.0693(8) Uani 1 1 d . . . . .
O8 O 0.47266(17) -0.2352(3) 0.63630(9) 0.0656(7) Uani 1 1 d . . . . .
N1 N 0.63222(11) 0.1994(2) 0.59917(8) 0.0327(4) Uani 1 1 d . . . . .
N2 N 0.38151(14) -0.0602(3) 0.59782(9) 0.0508(7) Uani 1 1 d . . . . .
C1 C 0.61677(14) 0.3036(3) 0.68601(10) 0.0343(5) Uani 1 1 d . . . . .
C2 C 0.58714(14) 0.1891(3) 0.64304(9) 0.0351(5) Uani 1 1 d . . . . .
H2A H 0.595412 0.090895 0.659317 0.042 Uiso 1 1 calc R . . . .
H2B H 0.527014 0.202314 0.628521 0.042 Uiso 1 1 calc R . . . .
C3 C 0.70637(15) 0.1217(3) 0.60506(9) 0.0337(5) Uani 1 1 d . . . . .
C4 C 0.60567(14) 0.3060(3) 0.56074(9) 0.0346(5) Uani 1 1 d . . . . .
C5 C 0.75302(14) 0.1365(3) 0.56116(9) 0.0312(5) Uani 1 1 d . . . . .
C6 C 0.65528(13) 0.3268(3) 0.51867(9) 0.0307(5) Uani 1 1 d . . . . .
C7 C 0.82317(15) 0.0535(3) 0.56194(10) 0.0365(5) Uani 1 1 d . . . . .
H7 H 0.840407 -0.015837 0.589661 0.044 Uiso 1 1 calc R . . . .
C8 C 0.72666(13) 0.2408(3) 0.52024(8) 0.0280(4) Uani 1 1 d . . . . .
C9 C 0.63085(14) 0.4282(3) 0.47846(10) 0.0363(5) Uani 1 1 d . . . . .
H9 H 0.582814 0.485911 0.478051 0.044 Uiso 1 1 calc R . . . .
C10 C 0.38111(16) 0.0103(4) 0.69185(11) 0.0460(7) Uani 1 1 d . . . . .
C11 C 0.3380(2) -0.0745(5) 0.64231(12) 0.0661(11) Uani 1 1 d . . . . .
H11A H 0.335143 -0.178699 0.651733 0.079 Uiso 1 1 calc R . . . .
H11B H 0.280426 -0.038228 0.630680 0.079 Uiso 1 1 calc R . . . .
C12 C 0.45201(18) -0.1453(4) 0.60061(10) 0.0468(7) Uani 1 1 d . . . . .
C13 C 0.35602(15) 0.0517(4) 0.56152(11) 0.0494(7) Uani 1 1 d . . . . .
C14 C 0.50069(15) -0.1219(3) 0.55836(10) 0.0396(6) Uani 1 1 d . . . . .
C15 C 0.40592(14) 0.0763(3) 0.51970(10) 0.0396(6) Uani 1 1 d . . . . .
C16 C 0.56931(18) -0.2073(3) 0.55731(11) 0.0467(6) Uani 1 1 d . . . . .
H16 H 0.584633 -0.282387 0.583091 0.056 Uiso 1 1 calc R . . . .
C17 C 0.47629(13) -0.0112(3) 0.51994(8) 0.0337(5) Uani 1 1 d . . . . .
C18 C 0.38337(17) 0.1831(4) 0.48199(12) 0.0474(6) Uani 1 1 d . . . . .
H18 H 0.335669 0.241032 0.482344 0.057 Uiso 1 1 calc R . . . .
N3 N 0.69329(17) 0.6415(3) 0.73915(10) 0.0513(6) Uani 1 1 d D . . . .
H3A H 0.695(2) 0.5528(16) 0.7302(15) 0.062 Uiso 1 1 d DR . . . .
H3B H 0.730(2) 0.668(6) 0.7657(14) 0.107(18) Uiso 1 1 d D . . . .
C19 C 0.7100(3) 0.7406(4) 0.69732(18) 0.0768(12) Uani 1 1 d . . . . .
H19A H 0.673828 0.715589 0.662934 0.115 Uiso 1 1 calc GR . . . .
H19B H 0.768189 0.731146 0.694367 0.115 Uiso 1 1 calc GR . . . .
H19C H 0.699169 0.841193 0.706786 0.115 Uiso 1 1 calc GR . . . .
C20 C 0.6090(2) 0.6440(4) 0.7495(2) 0.0851(15) Uani 1 1 d . . . . .
H20A H 0.598188 0.739573 0.763777 0.128 Uiso 1 1 calc GR . . . .
H20B H 0.603678 0.568296 0.775675 0.128 Uiso 1 1 calc GR . . . .
H20C H 0.568870 0.625915 0.716028 0.128 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 1.9597(17) 2_656 ?
Co1 O1 1.9597(18) . ?
Co1 O5 1.9531(18) 2_656 ?
Co1 O5 1.9530(18) . ?
O1 C1 1.261(3) . ?
O2 C1 1.237(3) . ?
O3 C4 1.218(3) . ?
O4 C3 1.221(3) . ?
O5 C10 1.269(3) . ?
O6 C10 1.231(3) . ?
O7 C13 1.215(4) . ?
O8 C12 1.224(4) . ?
N1 C2 1.468(3) . ?
N1 C3 1.395(3) . ?
N1 C4 1.389(3) . ?
N2 C11 1.468(3) . ?
N2 C12 1.388(4) . ?
N2 C13 1.389(5) . ?
C1 C2 1.524(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C5 1.489(3) . ?
C4 C6 1.489(3) . ?
C5 C7 1.380(3) . ?
C5 C8 1.416(3) . ?
C6 C8 1.410(3) . ?
C6 C9 1.382(4) . ?
C7 H7 0.9500 . ?
C7 C9 1.409(3) 7_656 ?
C8 C8 1.419(4) 7_656 ?
C9 H9 0.9500 . ?
C10 C11 1.528(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C14 1.485(3) . ?
C13 C15 1.492(3) . ?
C14 C16 1.380(4) . ?
C14 C17 1.411(4) . ?
C15 C17 1.409(4) . ?
C15 C18 1.369(4) . ?
C16 H16 0.9500 . ?
C16 C18 1.408(4) 5_656 ?
C17 C17 1.420(4) 5_656 ?
C18 H18 0.9500 . ?
N3 H3A 0.848(10) . ?
N3 H3B 0.843(10) . ?
N3 C19 1.471(5) . ?
N3 C20 1.465(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O1 105.84(11) . 2_656 ?
O5 Co1 O1 103.34(7) 2_656 2_656 ?
O5 Co1 O1 103.34(7) . . ?
O5 Co1 O1 110.28(8) 2_656 . ?
O5 Co1 O1 110.29(8) . 2_656 ?
O5 Co1 O5 122.78(14) . 2_656 ?
C1 O1 Co1 132.28(17) . . ?
C10 O5 Co1 115.19(16) . . ?
C3 N1 C2 117.0(2) . . ?
C4 N1 C2 116.6(2) . . ?
C4 N1 C3 125.21(19) . . ?
C12 N2 C11 116.6(3) . . ?
C12 N2 C13 125.8(2) . . ?
C13 N2 C11 116.9(3) . . ?
O1 C1 C2 118.2(2) . . ?
O2 C1 O1 123.4(2) . . ?
O2 C1 C2 118.4(2) . . ?
N1 C2 C1 111.48(18) . . ?
N1 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
O4 C3 N1 121.3(2) . . ?
O4 C3 C5 122.1(2) . . ?
N1 C3 C5 116.6(2) . . ?
O3 C4 N1 120.6(2) . . ?
O3 C4 C6 122.1(2) . . ?
N1 C4 C6 117.3(2) . . ?
C7 C5 C3 119.9(2) . . ?
C7 C5 C8 120.8(2) . . ?
C8 C5 C3 119.3(2) . . ?
C8 C6 C4 119.1(2) . . ?
C9 C6 C4 120.2(2) . . ?
C9 C6 C8 120.8(2) . . ?
C5 C7 H7 120.1 . . ?
C5 C7 C9 119.9(2) . 7_656 ?
C9 C7 H7 120.1 7_656 . ?
C5 C8 C8 119.1(3) . 7_656 ?
C6 C8 C5 121.75(19) . . ?
C6 C8 C8 119.1(3) . 7_656 ?
C6 C9 C7 120.3(2) . 7_656 ?
C6 C9 H9 119.8 . . ?
C7 C9 H9 119.8 7_656 . ?
O5 C10 C11 115.4(2) . . ?
O6 C10 O5 125.4(2) . . ?
O6 C10 C11 119.2(2) . . ?
N2 C11 C10 112.1(2) . . ?
N2 C11 H11A 109.2 . . ?
N2 C11 H11B 109.2 . . ?
C10 C11 H11A 109.2 . . ?
C10 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
O8 C12 N2 121.2(3) . . ?
O8 C12 C14 121.9(3) . . ?
N2 C12 C14 116.9(3) . . ?
O7 C13 N2 121.0(3) . . ?
O7 C13 C15 122.1(3) . . ?
N2 C13 C15 117.0(3) . . ?
C16 C14 C12 119.9(3) . . ?
C16 C14 C17 120.8(2) . . ?
C17 C14 C12 119.3(3) . . ?
C17 C15 C13 119.0(3) . . ?
C18 C15 C13 120.1(3) . . ?
C18 C15 C17 121.0(2) . . ?
C14 C16 H16 120.0 . . ?
C14 C16 C18 120.0(3) . 5_656 ?
C18 C16 H16 120.0 5_656 . ?
C14 C17 C17 118.8(3) . 5_656 ?
C15 C17 C14 122.0(2) . . ?
C15 C17 C17 119.2(3) . 5_656 ?
C15 C18 C16 120.2(3) . 5_656 ?
C15 C18 H18 119.9 . . ?
C16 C18 H18 119.9 5_656 . ?
H3A N3 H3B 116(5) . . ?
C19 N3 H3A 112(3) . . ?
C19 N3 H3B 101(4) . . ?
C20 N3 H3A 99(3) . . ?
C20 N3 H3B 113(4) . . ?
C20 N3 C19 116.6(3) . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 H20A 109.5 . . ?
N3 C20 H20B 109.5 . . ?
N3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3A O2 0.848(10) 2.004(17) 2.812(4) 159(4) . yes
N3 H3B O2 0.843(10) 2.59(3) 3.344(4) 149(5) 4_656 yes
N3 H3B O4 0.843(10) 2.49(4) 3.081(3) 127(5) 4_656 yes

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
Co1 O1 C1 O2 -158.9(2) . . . . ?
Co1 O1 C1 C2 19.6(4) . . . . ?
Co1 O5 C10 O6 2.5(5) . . . . ?
Co1 O5 C10 C11 -177.6(3) . . . . ?
O1 C1 C2 N1 172.0(2) . . . . ?
O2 C1 C2 N1 -9.4(4) . . . . ?
O3 C4 C6 C8 178.8(2) . . . . ?
O3 C4 C6 C9 -1.9(4) . . . . ?
O4 C3 C5 C7 7.0(4) . . . . ?
O4 C3 C5 C8 -170.2(2) . . . . ?
O5 C10 C11 N2 5.4(5) . . . . ?
O6 C10 C11 N2 -174.7(3) . . . . ?
O7 C13 C15 C17 178.3(2) . . . . ?
O7 C13 C15 C18 -1.5(4) . . . . ?
O8 C12 C14 C16 2.9(4) . . . . ?
O8 C12 C14 C17 -176.6(2) . . . . ?
N1 C3 C5 C7 -174.6(2) . . . . ?
N1 C3 C5 C8 8.2(3) . . . . ?
N1 C4 C6 C8 -1.1(3) . . . . ?
N1 C4 C6 C9 178.2(2) . . . . ?
N2 C12 C14 C16 -177.0(2) . . . . ?
N2 C12 C14 C17 3.5(3) . . . . ?
N2 C13 C15 C17 -1.5(3) . . . . ?
N2 C13 C15 C18 178.8(2) . . . . ?
C2 N1 C3 O4 0.3(3) . . . . ?
C2 N1 C3 C5 -178.13(19) . . . . ?
C2 N1 C4 O3 -5.2(3) . . . . ?
C2 N1 C4 C6 174.72(19) . . . . ?
C3 N1 C2 C1 87.7(3) . . . . ?
C3 N1 C4 O3 -172.5(2) . . . . ?
C3 N1 C4 C6 7.5(3) . . . . ?
C3 C5 C7 C9 -177.5(2) . . . 7_656 ?
C3 C5 C8 C6 -2.7(3) . . . . ?
C3 C5 C8 C8 177.3(2) . . . 7_656 ?
C4 N1 C2 C1 -80.6(3) . . . . ?
C4 N1 C3 O4 167.5(2) . . . . ?
C4 N1 C3 C5 -10.9(3) . . . . ?
C4 C6 C8 C5 -0.8(3) . . . . ?
C4 C6 C8 C8 179.1(2) . . . 7_656 ?
C4 C6 C9 C7 -178.9(2) . . . 7_656 ?
C7 C5 C8 C6 -180.0(2) . . . . ?
C7 C5 C8 C8 0.0(4) . . . 7_656 ?
C8 C5 C7 C9 -0.3(4) . . . 7_656 ?
C8 C6 C9 C7 0.4(4) . . . 7_656 ?
C9 C6 C8 C5 179.8(2) . . . . ?
C9 C6 C8 C8 -0.2(4) . . . 7_656 ?
C11 N2 C12 O8 5.4(4) . . . . ?
C11 N2 C12 C14 -174.7(2) . . . . ?
C11 N2 C13 O7 -6.1(4) . . . . ?
C11 N2 C13 C15 173.7(2) . . . . ?
C12 N2 C11 C10 78.5(4) . . . . ?
C12 N2 C13 O7 -175.7(3) . . . . ?
C12 N2 C13 C15 4.1(4) . . . . ?
C12 C14 C16 C18 -178.6(2) . . . 5_656 ?
C12 C14 C17 C15 -1.3(3) . . . . ?
C12 C14 C17 C17 179.4(2) . . . 5_656 ?
C13 N2 C11 C10 -92.0(4) . . . . ?
C13 N2 C12 O8 175.0(3) . . . . ?
C13 N2 C12 C14 -5.1(4) . . . . ?
C13 C15 C17 C14 0.3(3) . . . . ?
C13 C15 C17 C17 179.6(2) . . . 5_656 ?
C13 C15 C18 C16 179.6(2) . . . 5_656 ?
C16 C14 C17 C15 179.2(2) . . . . ?
C16 C14 C17 C17 -0.1(4) . . . 5_656 ?
C17 C14 C16 C18 0.9(4) . . . 5_656 ?
C17 C15 C18 C16 -0.1(4) . . . 5_656 ?
C18 C15 C17 C14 -180.0(2) . . . . ?
C18 C15 C17 C17 -0.7(4) . . . 5_656 ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Crystallised at elevated temperature from synthesis'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7
_database_code_depnum_ccdc_archive 'CCDC 1840392'
_audit_update_record             
;
2018-04-30 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_audit_creation_date             2018-02-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H18 N4 O8 Zn'
_chemical_formula_sum            'C30 H18 N4 O8 Zn'
_chemical_formula_weight         627.85
_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 0.0030 0.0020 '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 0.0070 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0120 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3120 1.4670 '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                   9.6690(19)
_cell_length_b                   13.649(3)
_cell_length_c                   14.082(3)
_cell_angle_alpha                109.91(3)
_cell_angle_beta                 106.20(3)
_cell_angle_gamma                99.92(3)
_cell_volume                     1602.8(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    60793
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.233
_cell_measurement_theta_min      1.652
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1879
_diffrn_reflns_av_unetI/netI     0.0866
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51444
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.497
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.652
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4111
_reflns_number_total             7354
_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       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         2.292
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_gt           0.0972
_refine_ls_restrained_S_all      1.058
_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)+(0.1990P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2803
_refine_ls_wR_factor_ref         0.3216
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C20(H20), C9(H9), C26(H26), C30(H30), C10(H10), C25(H25), C22(H22),
 C12(H12), C7(H7), C27(H27), C24(H24), C19(H19), C21(H21)
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.119 0.000 0.500 458 167 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?


_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Zn2 Zn 1.000000 0.500000 1.000000 0.0402(3) Uani 1 2 d S T P . .
Zn1 Zn -0.500000 0.500000 0.000000 0.0415(3) Uani 1 2 d S T P . .
O8 O 0.5520(4) 0.4661(3) 0.8562(3) 0.0399(9) Uani 1 1 d . . . . .
O7 O 0.7679(4) 0.4274(4) 0.9086(3) 0.0455(10) Uani 1 1 d . . . . .
O2 O -0.0417(4) 0.5537(3) 0.1509(3) 0.0418(9) Uani 1 1 d . . . . .
O4 O -0.1732(4) 0.3822(4) 0.2665(3) 0.0467(10) Uani 1 1 d . . . . .
O5 O 0.6933(4) 0.6307(4) 0.7458(4) 0.0558(12) Uani 1 1 d . . . . .
N4 N 0.9983(4) 0.6483(3) 0.9839(4) 0.0314(9) Uani 1 1 d . . . . .
O6 O 0.4338(5) 0.2721(4) 0.5907(4) 0.0622(13) Uani 1 1 d . . . . .
N3 N -0.5071(4) 0.3420(3) -0.0062(4) 0.0342(10) Uani 1 1 d . . . . .
O1 O -0.2747(4) 0.5695(4) 0.1033(4) 0.0508(11) Uani 1 1 d . . . . .
O3 O 0.0878(5) 0.7429(4) 0.4276(4) 0.0583(12) Uani 1 1 d . . . . .
N1 N -0.0439(5) 0.5618(4) 0.3496(4) 0.0450(11) Uani 1 1 d . . . . .
C6 C 0.0715(5) 0.4293(4) 0.3981(4) 0.0331(11) Uani 1 1 d . . . . .
N2 N 0.5667(5) 0.4520(5) 0.6623(4) 0.0473(12) Uani 1 1 d . . . . .
C8 C 0.1996(5) 0.5171(4) 0.4738(4) 0.0326(11) Uani 1 1 d . . . . .
C13 C 0.4499(6) 0.5811(5) 0.6124(4) 0.0363(12) Uani 1 1 d . . . . .
C4 C -0.0578(5) 0.4521(5) 0.3321(4) 0.0393(13) Uani 1 1 d . . . . .
C3 C 0.0829(6) 0.6502(5) 0.4203(5) 0.0469(14) Uani 1 1 d . . . . .
C18 C 0.6667(6) 0.4440(4) 0.8439(5) 0.0363(12) Uani 1 1 d . . . . .
C11 C 0.3215(5) 0.4937(4) 0.5377(4) 0.0334(11) Uani 1 1 d . . . . .
C28 C 1.1061(6) 0.7946(4) 0.9420(5) 0.0464(14) Uani 1 1 d . . . . .
H28 H 1.176367 0.822429 0.915086 0.056 Uiso 1 1 calc R . . . .
C15 C 0.5813(6) 0.5600(5) 0.6801(5) 0.0421(13) Uani 1 1 d . . . . .
C5 C 0.2108(6) 0.6267(5) 0.4890(5) 0.0431(13) Uani 1 1 d . . . . .
C14 C 0.3119(6) 0.3852(5) 0.5237(5) 0.0439(13) Uani 1 1 d . . . . .
C20 C -0.4808(6) 0.3169(5) 0.0774(5) 0.0420(13) Uani 1 1 d . . . . .
H20 H -0.457365 0.373710 0.146490 0.050 Uiso 1 1 calc R . . . .
C9 C 0.0649(6) 0.3236(5) 0.3839(4) 0.0373(12) Uani 1 1 d . . . . .
H9 H -0.020969 0.265427 0.330589 0.045 Uiso 1 1 calc R . . . .
C26 C 1.0967(6) 0.6946(4) 0.9482(5) 0.0415(13) Uani 1 1 d . . . . .
H26 H 1.163350 0.656286 0.926090 0.050 Uiso 1 1 calc R . . . .
C30 C 1.0267(7) 0.9628(5) 0.9741(6) 0.0481(15) Uani 1 1 d . . . . .
H30 H 1.079659 0.980739 0.931834 0.058 Uiso 1 1 calc R . . . .
C1 C -0.1587(6) 0.5664(5) 0.1680(5) 0.0395(12) Uani 1 1 d . . . . .
C29 C 1.0126(6) 0.8538(5) 0.9752(5) 0.0424(14) Uani 1 1 d . . . . .
C10 C 0.4570(6) 0.6880(5) 0.6264(5) 0.0413(13) Uani 1 1 d . . . . .
H10 H 0.542911 0.746260 0.679568 0.050 Uiso 1 1 calc R . . . .
C25 C 0.9001(6) 0.7035(4) 1.0081(5) 0.0469(15) Uani 1 1 d . . . . .
H25 H 0.823979 0.671072 1.027968 0.056 Uiso 1 1 calc R . . . .
C22 C -0.4845(7) 0.2126(5) 0.0726(5) 0.0496(15) Uani 1 1 d . . . . .
H22 H -0.462917 0.200416 0.137009 0.059 Uiso 1 1 calc R . . . .
C12 C 0.1853(6) 0.3011(5) 0.4482(5) 0.0403(12) Uani 1 1 d . . . . .
H12 H 0.179148 0.228125 0.439453 0.048 Uiso 1 1 calc R . . . .
C7 C 0.3379(6) 0.7098(5) 0.5623(5) 0.0449(13) Uani 1 1 d . . . . .
H7 H 0.345110 0.782423 0.569401 0.054 Uiso 1 1 calc R . . . .
C16 C 0.4392(6) 0.3628(5) 0.5937(5) 0.0474(15) Uani 1 1 d . . . . .
C27 C 0.9044(6) 0.8032(5) 1.0057(6) 0.0543(17) Uani 1 1 d . . . . .
H27 H 0.833461 0.838456 1.024896 0.065 Uiso 1 1 calc R . . . .
C23 C -0.5191(6) 0.1288(5) -0.0245(5) 0.0438(13) Uani 1 1 d . . . . .
C17 C 0.6898(7) 0.4325(6) 0.7367(5) 0.0535(17) Uani 1 1 d . . . . .
H17A H 0.786746 0.485201 0.753467 0.064 Uiso 1 1 calc R . . . .
H17B H 0.695902 0.358205 0.700057 0.064 Uiso 1 1 calc R . . . .
C24 C -0.5226(7) 0.0164(5) -0.0378(6) 0.0538(16) Uani 1 1 d . . . . .
H24 H -0.562727 -0.037777 -0.110149 0.065 Uiso 1 1 calc R . . . .
C19 C -0.5439(8) 0.2586(5) -0.1035(6) 0.0599(17) Uani 1 1 d . . . . .
H19 H -0.565461 0.272989 -0.166612 0.072 Uiso 1 1 calc R . . . .
C2 C -0.1647(7) 0.5853(6) 0.2808(5) 0.0520(16) Uani 1 1 d . . . . .
H2A H -0.160515 0.662322 0.318136 0.062 Uiso 1 1 calc R . . . .
H2B H -0.262522 0.538919 0.271448 0.062 Uiso 1 1 calc R . . . .
C21 C -0.5512(8) 0.1535(5) -0.1145(6) 0.0661(19) Uani 1 1 d . . . . .
H21 H -0.578680 0.097116 -0.184556 0.079 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn2 O7 2.104(4) 2_767 ?
Zn2 O7 2.104(4) . ?
Zn2 O2 2.176(4) 2_666 ?
Zn2 O2 2.176(4) 1_656 ?
Zn2 N4 2.115(4) . ?
Zn2 N4 2.115(4) 2_767 ?
Zn1 O8 2.139(4) 2_566 ?
Zn1 O8 2.139(4) 1_454 ?
Zn1 N3 2.116(4) 2_465 ?
Zn1 N3 2.116(4) . ?
Zn1 O1 2.083(4) . ?
Zn1 O1 2.083(4) 2_465 ?
O8 C18 1.240(6) . ?
O7 C18 1.248(6) . ?
O2 C1 1.248(6) . ?
O4 C4 1.211(7) . ?
O5 C15 1.196(7) . ?
N4 C26 1.354(6) . ?
N4 C25 1.355(6) . ?
O6 C16 1.216(7) . ?
N3 C20 1.307(6) . ?
N3 C19 1.351(8) . ?
O1 C1 1.251(7) . ?
O3 C3 1.225(7) . ?
N1 C4 1.408(8) . ?
N1 C3 1.393(8) . ?
N1 C2 1.454(7) . ?
C6 C8 1.410(8) . ?
C6 C4 1.485(7) . ?
C6 C9 1.375(8) . ?
N2 C15 1.383(8) . ?
N2 C16 1.398(8) . ?
N2 C17 1.479(7) . ?
C8 C11 1.425(7) . ?
C8 C5 1.417(8) . ?
C13 C11 1.406(8) . ?
C13 C15 1.499(7) . ?
C13 C10 1.391(8) . ?
C3 C5 1.501(8) . ?
C18 C17 1.546(8) . ?
C11 C14 1.409(8) . ?
C28 H28 0.9500 . ?
C28 C26 1.386(7) . ?
C28 C29 1.385(7) . ?
C5 C7 1.370(8) . ?
C14 C12 1.380(8) . ?
C14 C16 1.495(8) . ?
C20 H20 0.9500 . ?
C20 C22 1.395(8) . ?
C9 H9 0.9500 . ?
C9 C12 1.412(8) . ?
C26 H26 0.9500 . ?
C30 C30 1.310(12) 2_777 ?
C30 H30 0.9500 . ?
C30 C29 1.476(7) . ?
C1 C2 1.540(8) . ?
C29 C27 1.400(7) . ?
C10 H10 0.9500 . ?
C10 C7 1.396(8) . ?
C25 H25 0.9500 . ?
C25 C27 1.366(7) . ?
C22 H22 0.9500 . ?
C22 C23 1.356(9) . ?
C12 H12 0.9500 . ?
C7 H7 0.9500 . ?
C27 H27 0.9500 . ?
C23 C24 1.474(8) . ?
C23 C21 1.385(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C24 C24 1.289(12) 2_455 ?
C24 H24 0.9500 . ?
C19 H19 0.9500 . ?
C19 C21 1.377(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C21 H21 0.9500 . ?

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
O7 Zn2 O7 180.0 2_767 . ?
O7 Zn2 O2 91.48(15) 2_767 2_666 ?
O7 Zn2 O2 88.52(15) . 2_666 ?
O7 Zn2 O2 88.52(15) 2_767 1_656 ?
O7 Zn2 O2 91.48(15) . 1_656 ?
O7 Zn2 N4 93.00(16) 2_767 2_767 ?
O7 Zn2 N4 87.00(16) 2_767 . ?
O7 Zn2 N4 87.00(16) . 2_767 ?
O7 Zn2 N4 93.00(16) . . ?
O2 Zn2 O2 180.0 1_656 2_666 ?
N4 Zn2 O2 93.39(15) 2_767 2_666 ?
N4 Zn2 O2 86.61(15) 2_767 1_656 ?
N4 Zn2 O2 93.39(15) . 1_656 ?
N4 Zn2 O2 86.61(15) . 2_666 ?
N4 Zn2 N4 180.0(2) 2_767 . ?
O8 Zn1 O8 180.0(2) 1_454 2_566 ?
N3 Zn1 O8 87.42(16) . 2_566 ?
N3 Zn1 O8 87.42(16) 2_465 1_454 ?
N3 Zn1 O8 92.58(16) 2_465 2_566 ?
N3 Zn1 O8 92.58(16) . 1_454 ?
N3 Zn1 N3 180.0 . 2_465 ?
O1 Zn1 O8 86.30(15) 2_465 1_454 ?
O1 Zn1 O8 93.70(15) 2_465 2_566 ?
O1 Zn1 O8 86.30(15) . 2_566 ?
O1 Zn1 O8 93.70(15) . 1_454 ?
O1 Zn1 N3 94.22(17) 2_465 2_465 ?
O1 Zn1 N3 94.22(17) . . ?
O1 Zn1 N3 85.78(17) . 2_465 ?
O1 Zn1 N3 85.78(17) 2_465 . ?
O1 Zn1 O1 180.0 2_465 . ?
C18 O8 Zn1 126.5(4) . 1_656 ?
C18 O7 Zn2 137.4(3) . . ?
C1 O2 Zn2 130.4(4) . 1_454 ?
C26 N4 Zn2 121.6(3) . . ?
C26 N4 C25 115.4(4) . . ?
C25 N4 Zn2 123.0(3) . . ?
C20 N3 Zn1 125.2(4) . . ?
C20 N3 C19 115.9(5) . . ?
C19 N3 Zn1 118.9(4) . . ?
C1 O1 Zn1 151.0(4) . . ?
C4 N1 C2 118.0(5) . . ?
C3 N1 C4 125.6(5) . . ?
C3 N1 C2 116.0(5) . . ?
C8 C6 C4 119.0(5) . . ?
C9 C6 C8 121.2(5) . . ?
C9 C6 C4 119.7(5) . . ?
C15 N2 C16 126.7(5) . . ?
C15 N2 C17 115.6(5) . . ?
C16 N2 C17 116.9(5) . . ?
C6 C8 C11 118.2(5) . . ?
C6 C8 C5 122.6(5) . . ?
C5 C8 C11 119.3(5) . . ?
C11 C13 C15 119.9(5) . . ?
C10 C13 C11 121.3(5) . . ?
C10 C13 C15 118.8(5) . . ?
O4 C4 N1 119.3(5) . . ?
O4 C4 C6 123.6(5) . . ?
N1 C4 C6 117.1(5) . . ?
O3 C3 N1 121.5(5) . . ?
O3 C3 C5 121.8(6) . . ?
N1 C3 C5 116.7(5) . . ?
O8 C18 O7 127.2(5) . . ?
O8 C18 C17 118.4(5) . . ?
O7 C18 C17 114.4(4) . . ?
C13 C11 C8 118.1(5) . . ?
C13 C11 C14 121.9(5) . . ?
C14 C11 C8 119.9(5) . . ?
C26 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C29 C28 C26 119.8(4) . . ?
O5 C15 N2 120.9(5) . . ?
O5 C15 C13 123.3(6) . . ?
N2 C15 C13 115.8(5) . . ?
C8 C5 C3 118.8(5) . . ?
C7 C5 C8 121.0(5) . . ?
C7 C5 C3 120.1(5) . . ?
C11 C14 C16 119.1(5) . . ?
C12 C14 C11 120.4(5) . . ?
C12 C14 C16 120.5(5) . . ?
N3 C20 H20 117.6 . . ?
N3 C20 C22 124.8(6) . . ?
C22 C20 H20 117.6 . . ?
C6 C9 H9 119.9 . . ?
C6 C9 C12 120.3(5) . . ?
C12 C9 H9 119.9 . . ?
N4 C26 C28 123.9(5) . . ?
N4 C26 H26 118.1 . . ?
C28 C26 H26 118.1 . . ?
C30 C30 H30 116.9 2_777 . ?
C30 C30 C29 126.3(6) 2_777 . ?
C29 C30 H30 116.9 . . ?
O2 C1 O1 126.9(5) . . ?
O2 C1 C2 119.1(5) . . ?
O1 C1 C2 113.9(5) . . ?
C28 C29 C30 120.2(4) . . ?
C28 C29 C27 116.5(5) . . ?
C27 C29 C30 123.3(5) . . ?
C13 C10 H10 120.0 . . ?
C13 C10 C7 120.0(5) . . ?
C7 C10 H10 120.0 . . ?
N4 C25 H25 118.1 . . ?
N4 C25 C27 123.7(4) . . ?
C27 C25 H25 118.1 . . ?
C20 C22 H22 120.2 . . ?
C23 C22 C20 119.5(5) . . ?
C23 C22 H22 120.2 . . ?
C14 C12 C9 120.0(5) . . ?
C14 C12 H12 120.0 . . ?
C9 C12 H12 120.0 . . ?
C5 C7 C10 120.2(5) . . ?
C5 C7 H7 119.9 . . ?
C10 C7 H7 119.9 . . ?
O6 C16 N2 121.4(5) . . ?
O6 C16 C14 122.3(6) . . ?
N2 C16 C14 116.3(5) . . ?
C29 C27 H27 119.8 . . ?
C25 C27 C29 120.4(5) . . ?
C25 C27 H27 119.8 . . ?
C22 C23 C24 123.7(6) . . ?
C22 C23 C21 116.5(5) . . ?
C21 C23 C24 119.8(6) . . ?
N2 C17 C18 112.5(4) . . ?
N2 C17 H17A 109.1 . . ?
N2 C17 H17B 109.1 . . ?
C18 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
C23 C24 H24 116.4 . . ?
C24 C24 C23 127.2(9) 2_455 . ?
C24 C24 H24 116.4 2_455 . ?
N3 C19 H19 118.8 . . ?
N3 C19 C21 122.4(6) . . ?
C21 C19 H19 118.8 . . ?
N1 C2 C1 114.2(5) . . ?
N1 C2 H2A 108.7 . . ?
N1 C2 H2B 108.7 . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C23 C21 H21 119.6 . . ?
C19 C21 C23 120.8(7) . . ?
C19 C21 H21 119.6 . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_DIFMX02_7                   
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: Residual density close to Zn, low quality data.
;
_vrf_PLAT084_7                   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.32 Report
RESPONSE: Low quality data was best obtainable.
;
_vrf_PLAT094_7                   
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       2.14 Report
RESPONSE: Residual density close to Zn, low quality data.
;
_vrf_PLAT097_7                   
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       2.29 eA-3  
RESPONSE: Residual density close to Zn, low quality data.
;
_vrf_PLAT112_7                   
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem       a/2         84 %Fit  
RESPONSE: Checked through ADDSYM, P-1 is correct spacegroup.
;
_exptl_crystal_recrystallization_method 
'Crystallised at elevated temperature from synthesis'
####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1840394'
_audit_update_record             
;
2018-04-30 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_audit_creation_date             2016-12-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H54 Co2 N8 O18'
_chemical_formula_sum            'C60 H54 Co2 N8 O18'
_chemical_formula_weight         1292.96
_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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   26.660(5)
_cell_length_b                   7.2720(15)
_cell_length_c                   27.642(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5359.0(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3554
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.856
_cell_measurement_theta_min      1.660
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0920
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            56051
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         33.859
_diffrn_reflns_theta_min         1.660
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_device_type  'Quantum 210r'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7353
_reflns_number_total             9181
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.721
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         9181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0781
_refine_ls_restrained_S_all      1.032
_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)+(0.1052P)²+10.3369P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2057
_refine_ls_wR_factor_ref         0.2171
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C9(H9), C11(H11), C28(H28), C24(H24), C27(H27), C25(H25), C26(H26),
 C12(H12)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C3(H3A,H3B,H3C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C2(H2A,H2B,H2C)
;
_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
Co1 Co 0.38426(2) 0.63805(5) 0.47954(2) 0.02593(12) Uani 1 1 d . . . . .
O8 O 0.09564(7) 0.7043(3) 0.03569(7) 0.0257(4) Uani 1 1 d . . . . .
O5 O 0.19273(7) 0.6114(3) 0.09177(7) 0.0253(4) Uani 1 1 d . . . . .
O7 O 0.13699(7) 0.9315(3) 0.07159(7) 0.0250(4) Uani 1 1 d . . . . .
O2 O 0.36549(8) 0.5292(3) 0.37956(7) 0.0296(4) Uani 1 1 d . . . . .
O9 O 0.31138(8) 0.6470(4) 0.47085(8) 0.0350(5) Uani 1 1 d . . . . .
O3 O 0.41230(8) 0.7250(4) 0.22720(8) 0.0358(5) Uani 1 1 d . . . . .
O1 O 0.40811(9) 0.7502(4) 0.41782(8) 0.0341(5) Uani 1 1 d . . . . .
O4 O 0.31982(9) 0.8800(3) 0.35849(8) 0.0323(5) Uani 1 1 d . . . . .
O6 O 0.09961(9) 0.7139(4) 0.22547(8) 0.0378(5) Uani 1 1 d . . . . .
N3 N 0.42654(9) 0.4043(3) 0.48519(8) 0.0241(4) Uani 1 1 d . . . . .
N4 N 0.22836(9) 0.6760(4) 0.48292(8) 0.0263(4) Uani 1 1 d . . . . .
N2 N 0.14530(8) 0.7088(3) 0.15516(8) 0.0228(4) Uani 1 1 d . . . . .
N1 N 0.36517(9) 0.7547(4) 0.29663(9) 0.0274(5) Uani 1 1 d . . . . .
C10 C 0.27800(10) 0.7491(3) 0.23941(8) 0.0208(4) Uani 1 1 d . . . . .
C8 C 0.32478(10) 0.7176(4) 0.21716(9) 0.0223(4) Uani 1 1 d . . . . .
C16 C 0.23718(9) 0.6789(3) 0.16311(8) 0.0193(4) Uani 1 1 d . . . . .
C14 C 0.28340(10) 0.6457(4) 0.14186(9) 0.0216(4) Uani 1 1 d . . . . .
H14 H 0.2853 0.6087 0.1089 0.026 Uiso 1 1 calc R . . . .
C13 C 0.23373(9) 0.7295(3) 0.21194(8) 0.0198(4) Uani 1 1 d . . . . .
C18 C 0.19104(10) 0.6625(3) 0.13378(9) 0.0209(4) Uani 1 1 d . . . . .
C15 C 0.18681(10) 0.7556(4) 0.23424(9) 0.0220(4) Uani 1 1 d . . . . .
C9 C 0.22797(11) 0.8339(4) 0.30917(9) 0.0253(5) Uani 1 1 d . . . . .
H9 H 0.2259 0.8742 0.3418 0.030 Uiso 1 1 calc R . . . .
C6 C 0.37152(11) 0.7331(4) 0.24631(10) 0.0267(5) Uani 1 1 d . . . . .
C11 C 0.32743(10) 0.6668(4) 0.16909(9) 0.0228(4) Uani 1 1 d . . . . .
H11 H 0.3592 0.6461 0.1544 0.027 Uiso 1 1 calc R . . . .
C7 C 0.27457(11) 0.8018(4) 0.28831(9) 0.0234(5) Uani 1 1 d . . . . .
C23 C 0.48511(9) 0.0845(4) 0.49685(9) 0.0217(4) Uani 1 1 d . . . . .
C28 C 0.27441(11) 0.6515(4) 0.49872(10) 0.0273(5) Uani 1 1 d . . . . .
H28 H 0.2798 0.6368 0.5325 0.033 Uiso 1 1 calc R . . . .
C22 C 0.11401(9) 0.7834(4) 0.07318(9) 0.0228(5) Uani 1 1 d . . . . .
C24 C 0.48609(10) 0.2277(4) 0.53031(10) 0.0259(5) Uani 1 1 d . . . . .
H24 H 0.5074 0.2198 0.5578 0.031 Uiso 1 1 calc R . . . .
C27 C 0.42614(10) 0.2693(4) 0.45177(10) 0.0266(5) Uani 1 1 d . . . . .
H27 H 0.4059 0.2843 0.4238 0.032 Uiso 1 1 calc R . . . .
C25 C 0.45398(11) 0.1101(4) 0.45653(10) 0.0267(5) Uani 1 1 d . . . . .
H25 H 0.4520 0.0175 0.4324 0.032 Uiso 1 1 calc R . . . .
C17 C 0.14002(10) 0.7256(4) 0.20586(10) 0.0258(5) Uani 1 1 d . . . . .
C26 C 0.45636(11) 0.3807(4) 0.52381(10) 0.0279(5) Uani 1 1 d . . . . .
H26 H 0.4570 0.4741 0.5478 0.033 Uiso 1 1 calc R . . . .
C12 C 0.18395(11) 0.8070(4) 0.28218(9) 0.0255(5) Uani 1 1 d . . . . .
H12 H 0.1521 0.8243 0.2970 0.031 Uiso 1 1 calc R . . . .
C21 C 0.09998(10) 0.6979(4) 0.12281(10) 0.0245(5) Uani 1 1 d . . . . .
C20 C 0.05634(10) 0.8191(5) 0.14039(11) 0.0299(6) Uani 1 1 d . . . . .
H20A H 0.0403 0.7612 0.1684 0.045 Uiso 1 1 calc GR . . . .
H20B H 0.0317 0.8328 0.1143 0.045 Uiso 1 1 calc GR . . . .
H20C H 0.0692 0.9404 0.1496 0.045 Uiso 1 1 calc GR . . . .
C19 C 0.08330(12) 0.4974(4) 0.11901(11) 0.0311(6) Uani 1 1 d . . . . .
H19A H 0.1090 0.4262 0.1020 0.047 Uiso 1 1 calc GR . . . .
H19B H 0.0516 0.4906 0.1011 0.047 Uiso 1 1 calc GR . . . .
H19C H 0.0785 0.4468 0.1515 0.047 Uiso 1 1 calc GR . . . .
C5 C 0.32066(11) 0.8182(4) 0.31746(10) 0.0257(5) Uani 1 1 d . . . . .
C1 C 0.39120(11) 0.6696(5) 0.37967(10) 0.0301(6) Uani 1 1 d . . . . .
C3 C 0.45023(12) 0.6102(6) 0.31420(12) 0.0389(7) Uani 1 1 d . . . . .
H3A H 0.4340 0.4961 0.3036 0.058 Uiso 1 1 calc GR . . . .
H3B H 0.4726 0.5839 0.3415 0.058 Uiso 1 1 calc GR . . . .
H3C H 0.4698 0.6621 0.2874 0.058 Uiso 1 1 calc GR . . . .
C29 C 0.18566(12) 0.6798(5) 0.51609(11) 0.0306(6) Uani 1 1 d . . . . .
H29A H 0.1619 0.5829 0.5072 0.046 Uiso 1 1 calc GR . . . .
H29B H 0.1690 0.7998 0.5141 0.046 Uiso 1 1 calc GR . . . .
H29C H 0.1975 0.6594 0.5492 0.046 Uiso 1 1 calc GR . . . .
C30 C 0.21744(13) 0.7020(6) 0.43176(11) 0.0418(8) Uani 1 1 d . . . . .
H30A H 0.2489 0.7019 0.4133 0.063 Uiso 1 1 calc GR . . . .
H30B H 0.2002 0.8197 0.4271 0.063 Uiso 1 1 calc GR . . . .
H30C H 0.1959 0.6018 0.4203 0.063 Uiso 1 1 calc GR . . . .
C4 C 0.40959(11) 0.7501(5) 0.33018(10) 0.0305(6) Uani 1 1 d . . . . .
C2 C 0.43194(14) 0.9441(6) 0.33278(13) 0.0419(8) Uani 1 1 d . . . . .
H2A H 0.4427 0.9825 0.3004 0.063 Uiso 1 1 calc GR . . . .
H2B H 0.4609 0.9439 0.3547 0.063 Uiso 1 1 calc GR . . . .
H2C H 0.4065 1.0299 0.3449 0.063 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O8 2.003(2) 2_565 ?
Co1 O9 1.959(2) . ?
Co1 O1 1.995(2) . ?
Co1 N3 2.046(2) . ?
O8 Co1 2.003(2) 2_564 ?
O8 C22 1.282(3) . ?
O5 C18 1.220(3) . ?
O7 C22 1.240(4) . ?
O2 C1 1.229(4) . ?
O9 C28 1.251(4) . ?
O3 C6 1.210(4) . ?
O1 C1 1.288(4) . ?
O4 C5 1.220(3) . ?
O6 C17 1.209(3) . ?
N3 C27 1.348(4) . ?
N3 C26 1.342(4) . ?
N4 C28 1.315(4) . ?
N4 C29 1.462(4) . ?
N4 C30 1.456(4) . ?
N2 C18 1.396(3) . ?
N2 C17 1.414(3) . ?
N2 C21 1.505(3) . ?
N1 C6 1.410(4) . ?
N1 C5 1.398(4) . ?
N1 C4 1.504(3) . ?
C10 C8 1.409(4) . ?
C10 C13 1.411(3) . ?
C10 C7 1.408(3) . ?
C8 C6 1.488(4) . ?
C8 C11 1.381(4) . ?
C16 C14 1.386(3) . ?
C16 C13 1.402(3) . ?
C16 C18 1.478(3) . ?
C14 H14 0.9500 . ?
C14 C11 1.403(3) . ?
C13 C15 1.407(3) . ?
C15 C17 1.490(4) . ?
C15 C12 1.379(3) . ?
C9 H9 0.9500 . ?
C9 C7 1.390(4) . ?
C9 C12 1.404(4) . ?
C11 H11 0.9500 . ?
C7 C5 1.474(4) . ?
C23 C23 1.474(5) 5_656 ?
C23 C24 1.393(4) . ?
C23 C25 1.402(4) . ?
C28 H28 0.9500 . ?
C22 C21 1.552(4) . ?
C24 H24 0.9500 . ?
C24 C26 1.378(4) . ?
C27 H27 0.9500 . ?
C27 C25 1.382(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C12 H12 0.9500 . ?
C21 C20 1.538(4) . ?
C21 C19 1.528(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C1 C4 1.567(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C3 C4 1.551(5) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C4 C2 1.533(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 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
O8 Co1 N3 105.61(9) 2_565 . ?
O9 Co1 O8 109.96(9) . 2_565 ?
O9 Co1 O1 101.40(10) . . ?
O9 Co1 N3 125.69(11) . . ?
O1 Co1 O8 110.09(9) . 2_565 ?
O1 Co1 N3 103.27(10) . . ?
C22 O8 Co1 105.52(17) . 2_564 ?
C28 O9 Co1 135.0(2) . . ?
C1 O1 Co1 113.7(2) . . ?
C27 N3 Co1 123.26(18) . . ?
C26 N3 Co1 119.55(19) . . ?
C26 N3 C27 117.2(2) . . ?
C28 N4 C29 121.4(2) . . ?
C28 N4 C30 121.8(3) . . ?
C30 N4 C29 116.8(2) . . ?
C18 N2 C17 121.8(2) . . ?
C18 N2 C21 115.9(2) . . ?
C17 N2 C21 120.9(2) . . ?
C6 N1 C4 120.8(2) . . ?
C5 N1 C6 123.0(2) . . ?
C5 N1 C4 114.9(2) . . ?
C8 C10 C13 119.3(2) . . ?
C7 C10 C8 121.4(2) . . ?
C7 C10 C13 119.3(2) . . ?
C10 C8 C6 119.5(2) . . ?
C11 C8 C10 120.6(2) . . ?
C11 C8 C6 119.9(2) . . ?
C14 C16 C13 120.8(2) . . ?
C14 C16 C18 119.6(2) . . ?
C13 C16 C18 119.6(2) . . ?
C16 C14 H14 120.1 . . ?
C16 C14 C11 119.8(2) . . ?
C11 C14 H14 120.1 . . ?
C16 C13 C10 119.3(2) . . ?
C16 C13 C15 121.0(2) . . ?
C15 C13 C10 119.6(2) . . ?
O5 C18 N2 120.6(2) . . ?
O5 C18 C16 121.1(2) . . ?
N2 C18 C16 118.4(2) . . ?
C13 C15 C17 119.6(2) . . ?
C12 C15 C13 120.4(2) . . ?
C12 C15 C17 120.0(2) . . ?
C7 C9 H9 119.9 . . ?
C7 C9 C12 120.2(2) . . ?
C12 C9 H9 119.9 . . ?
O3 C6 N1 122.9(3) . . ?
O3 C6 C8 120.8(3) . . ?
N1 C6 C8 116.2(2) . . ?
C8 C11 C14 120.2(2) . . ?
C8 C11 H11 119.9 . . ?
C14 C11 H11 119.9 . . ?
C10 C7 C5 119.5(2) . . ?
C9 C7 C10 120.1(2) . . ?
C9 C7 C5 120.3(2) . . ?
C24 C23 C23 122.3(3) . 5_656 ?
C24 C23 C25 116.1(2) . . ?
C25 C23 C23 121.6(3) . 5_656 ?
O9 C28 N4 122.3(3) . . ?
O9 C28 H28 118.8 . . ?
N4 C28 H28 118.8 . . ?
O8 C22 C21 116.3(2) . . ?
O7 C22 O8 123.3(2) . . ?
O7 C22 C21 119.9(2) . . ?
C23 C24 H24 119.8 . . ?
C26 C24 C23 120.4(2) . . ?
C26 C24 H24 119.8 . . ?
N3 C27 H27 118.6 . . ?
N3 C27 C25 122.7(2) . . ?
C25 C27 H27 118.6 . . ?
C23 C25 H25 119.8 . . ?
C27 C25 C23 120.3(3) . . ?
C27 C25 H25 119.8 . . ?
O6 C17 N2 121.8(3) . . ?
O6 C17 C15 121.4(3) . . ?
N2 C17 C15 116.8(2) . . ?
N3 C26 C24 123.2(3) . . ?
N3 C26 H26 118.4 . . ?
C24 C26 H26 118.4 . . ?
C15 C12 C9 120.1(3) . . ?
C15 C12 H12 119.9 . . ?
C9 C12 H12 119.9 . . ?
N2 C21 C22 108.1(2) . . ?
N2 C21 C20 112.9(2) . . ?
N2 C21 C19 108.9(2) . . ?
C20 C21 C22 103.4(2) . . ?
C19 C21 C22 113.0(2) . . ?
C19 C21 C20 110.4(2) . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C21 C19 H19A 109.5 . . ?
C21 C19 H19B 109.5 . . ?
C21 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O4 C5 N1 121.4(2) . . ?
O4 C5 C7 121.5(3) . . ?
N1 C5 C7 117.1(2) . . ?
O2 C1 O1 125.1(3) . . ?
O2 C1 C4 118.9(3) . . ?
O1 C1 C4 115.8(3) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
N4 C29 H29A 109.5 . . ?
N4 C29 H29B 109.5 . . ?
N4 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N4 C30 H30A 109.5 . . ?
N4 C30 H30B 109.5 . . ?
N4 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N1 C4 C1 107.5(2) . . ?
N1 C4 C3 112.9(2) . . ?
N1 C4 C2 108.3(3) . . ?
C3 C4 C1 102.8(3) . . ?
C2 C4 C1 115.1(3) . . ?
C2 C4 C3 110.2(3) . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_shelx_SHELXL_version_number     2014/7

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Crystallised at elevated temperature from synthesis'
####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 1840393'
_audit_update_record             
;
2018-04-30 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_audit_creation_date             2017-05-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H30 Cu N4 O10'
_chemical_formula_sum            'C28 H30 Cu N4 O10'
_chemical_formula_weight         646.10
_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 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3410 1.2900 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0070 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0120 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.105(5)
_cell_length_b                   14.012(3)
_cell_length_c                   7.4950(15)
_cell_angle_alpha                90
_cell_angle_beta                 94.37(3)
_cell_angle_gamma                90
_cell_volume                     2838.3(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13310
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.818
_cell_measurement_theta_min      1.507
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0978
_diffrn_reflns_av_unetI/netI     0.0850
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13310
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         31.821
_diffrn_reflns_theta_min         1.507
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_source                   'MX1 beamline Australian Synchrotron'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2264
_reflns_number_total             4072
_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       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.975
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4072
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1425
_refine_ls_R_factor_gt           0.0849
_refine_ls_restrained_S_all      1.045
_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)+(0.1638P)²+1.5130P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2502
_refine_ls_wR_factor_ref         0.2917
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C9(H9), C11(H11)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_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
Cu1 Cu 0.7500 0.2500 0.0000 0.0537(3) Uani 1 2 d S T P . .
O1 O 0.69099(12) 0.1974(2) 0.0992(5) 0.0566(8) Uani 1 1 d . . . . .
O4 O 0.62643(14) 0.3665(3) 0.2411(5) 0.0609(9) Uani 1 1 d . . . . .
O5 O 0.76456(14) 0.3344(3) 0.2061(5) 0.0658(10) Uani 1 1 d . . . . .
O2 O 0.65680(13) 0.3033(3) -0.0930(5) 0.0587(9) Uani 1 1 d . . . . .
O3 O 0.49729(15) 0.2018(3) -0.0099(7) 0.0732(11) Uani 1 1 d . . . . .
N1 N 0.56786(15) 0.2869(3) 0.0616(6) 0.0523(9) Uani 1 1 d . . . . .
N2 N 0.74761(14) 0.4018(3) 0.4648(6) 0.0539(10) Uani 1 1 d . . . . .
C10 C 0.51229(16) 0.4567(3) 0.0191(6) 0.0474(10) Uani 1 1 d . . . . .
C1 C 0.65352(18) 0.2407(3) 0.0192(7) 0.0503(10) Uani 1 1 d . . . . .
C12 C 0.73746(18) 0.3447(3) 0.3295(7) 0.0543(11) Uani 1 1 d . . . . .
H12 H 0.7076 0.3092 0.3258 0.065 Uiso 1 1 calc R . . . .
C8 C 0.56141(16) 0.4601(4) 0.1082(6) 0.0509(11) Uani 1 1 d . . . . .
C9 C 0.44233(18) 0.3691(4) -0.1084(7) 0.0548(11) Uani 1 1 d . . . . .
H9 H 0.4265 0.3099 -0.1363 0.066 Uiso 1 1 calc R . . . .
C6 C 0.58784(18) 0.3694(4) 0.1435(7) 0.0543(11) Uani 1 1 d . . . . .
C7 C 0.48965(17) 0.3701(4) -0.0252(6) 0.0516(11) Uani 1 1 d . . . . .
C11 C 0.58261(17) 0.5449(4) 0.1521(6) 0.0533(11) Uani 1 1 d . . . . .
H11 H 0.6146 0.5465 0.2131 0.064 Uiso 1 1 calc R . . . .
C4 C 0.60192(19) 0.2015(4) 0.0619(7) 0.0564(12) Uani 1 1 d . . . . .
C5 C 0.5170(2) 0.2788(4) 0.0087(7) 0.0567(12) Uani 1 1 d . . . . .
C2 C 0.5881(2) 0.1327(4) -0.0900(9) 0.0716(16) Uani 1 1 d . . . . .
H2A H 0.5601 0.0933 -0.0593 0.107 Uiso 1 1 calc GR . . . .
H2B H 0.6164 0.0915 -0.1092 0.107 Uiso 1 1 calc GR . . . .
H2C H 0.5789 0.1688 -0.1995 0.107 Uiso 1 1 calc GR . . . .
C3 C 0.6015(2) 0.1507(5) 0.2433(9) 0.0757(17) Uani 1 1 d . . . . .
H3A H 0.6175 0.1913 0.3372 0.114 Uiso 1 1 calc GR . . . .
H3B H 0.6195 0.0902 0.2387 0.114 Uiso 1 1 calc GR . . . .
H3C H 0.5673 0.1381 0.2697 0.114 Uiso 1 1 calc GR . . . .
C13 C 0.7124(3) 0.4169(5) 0.5996(10) 0.0796(18) Uani 1 1 d . . . . .
H13A H 0.6992 0.4819 0.5889 0.119 Uiso 1 1 calc GR . . . .
H13B H 0.7292 0.4081 0.7191 0.119 Uiso 1 1 calc GR . . . .
H13C H 0.6853 0.3709 0.5816 0.119 Uiso 1 1 calc GR . . . .
C14 C 0.7932(2) 0.4567(5) 0.4877(8) 0.0731(16) Uani 1 1 d . . . . .
H14A H 0.8165 0.4337 0.4037 0.110 Uiso 1 1 calc GR . . . .
H14B H 0.8078 0.4491 0.6106 0.110 Uiso 1 1 calc GR . . . .
H14C H 0.7859 0.5243 0.4644 0.110 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.958(4) . ?
Cu1 O1 1.959(4) 7_655 ?
Cu1 O5 1.962(4) 7_655 ?
Cu1 O5 1.962(4) . ?
O1 C1 1.291(6) . ?
O4 C6 1.230(6) . ?
O5 C12 1.232(6) . ?
O2 C1 1.223(6) . ?
O3 C5 1.207(7) . ?
N1 C6 1.399(7) . ?
N1 C4 1.510(6) . ?
N1 C5 1.410(7) . ?
N2 C12 1.304(7) . ?
N2 C13 1.457(7) . ?
N2 C14 1.454(7) . ?
C10 C10 1.403(9) 5_665 ?
C10 C8 1.444(6) . ?
C10 C7 1.388(7) . ?
C1 C4 1.558(7) . ?
C12 H12 0.9500 . ?
C8 C6 1.473(7) . ?
C8 C11 1.349(7) . ?
C9 H9 0.9500 . ?
C9 C7 1.383(7) . ?
C9 C11 1.408(7) 5_665 ?
C7 C5 1.491(7) . ?
C11 C9 1.408(7) 5_665 ?
C11 H11 0.9500 . ?
C4 C2 1.517(8) . ?
C4 C3 1.536(8) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 180.0 . 7_655 ?
O1 Cu1 O5 92.82(15) 7_655 7_655 ?
O1 Cu1 O5 92.82(15) . . ?
O1 Cu1 O5 87.18(15) . 7_655 ?
O1 Cu1 O5 87.18(15) 7_655 . ?
O5 Cu1 O5 180.0 . 7_655 ?
C1 O1 Cu1 106.5(3) . . ?
C12 O5 Cu1 124.4(3) . . ?
C6 N1 C4 116.0(4) . . ?
C6 N1 C5 121.8(4) . . ?
C5 N1 C4 121.4(5) . . ?
C12 N2 C13 121.2(5) . . ?
C12 N2 C14 122.9(5) . . ?
C14 N2 C13 115.9(5) . . ?
C10 C10 C8 118.2(6) 5_665 . ?
C7 C10 C10 120.8(5) . 5_665 ?
C7 C10 C8 121.0(4) . . ?
O1 C1 C4 115.2(4) . . ?
O2 C1 O1 124.1(5) . . ?
O2 C1 C4 120.5(4) . . ?
O5 C12 N2 123.5(5) . . ?
O5 C12 H12 118.2 . . ?
N2 C12 H12 118.2 . . ?
C10 C8 C6 118.2(5) . . ?
C11 C8 C10 120.2(4) . . ?
C11 C8 C6 121.5(4) . . ?
C7 C9 H9 119.7 . . ?
C7 C9 C11 120.6(5) . 5_665 ?
C11 C9 H9 119.7 5_665 . ?
O4 C6 N1 121.1(4) . . ?
O4 C6 C8 121.0(5) . . ?
N1 C6 C8 117.9(4) . . ?
C10 C7 C5 120.3(4) . . ?
C9 C7 C10 119.7(5) . . ?
C9 C7 C5 120.0(5) . . ?
C8 C11 C9 120.6(5) . 5_665 ?
C8 C11 H11 119.7 . . ?
C9 C11 H11 119.7 5_665 . ?
N1 C4 C1 106.2(4) . . ?
N1 C4 C2 112.7(4) . . ?
N1 C4 C3 108.9(4) . . ?
C2 C4 C1 104.1(4) . . ?
C2 C4 C3 110.6(5) . . ?
C3 C4 C1 114.4(4) . . ?
O3 C5 N1 121.2(5) . . ?
O3 C5 C7 122.6(5) . . ?
N1 C5 C7 116.2(5) . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
N2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C14 H14A 109.5 . . ?
N2 C14 H14B 109.5 . . ?
N2 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Crystallised at elevated temperature from synthesis'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 1840390'
_audit_update_record             
;
2018-04-30 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_audit_creation_date             2018-01-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H18 Cu N4 O8'
_chemical_formula_sum            'C30 H18 Cu N4 O8'
_chemical_formula_weight         626.02
_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 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3410 1.2900 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0070 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0120 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                   11.713(2)
_cell_length_b                   11.938(2)
_cell_length_c                   12.993(3)
_cell_angle_alpha                115.19(3)
_cell_angle_beta                 105.01(3)
_cell_angle_gamma                96.15(3)
_cell_volume                     1538.0(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    58526
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.026
_cell_measurement_theta_min      1.841
_shelx_estimated_absorpt_T_max   0.985
_shelx_estimated_absorpt_T_min   0.970
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             638
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1499
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            58512
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         32.029
_diffrn_reflns_theta_min         1.841
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'phi scnas'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6408
_reflns_number_total             9276
_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       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.672
_refine_diff_density_min         -1.977
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         9276
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0775
_refine_ls_restrained_S_all      1.055
_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)+(0.1032P)²+1.7322P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.2173
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C30(H30), C28(H28), C29(H29), C9(H9), C19(H19), C24(H24), C21(H21),
 C12(H12), C25(H25), C22(H22), C27(H27), C7(H7), C10(H10)
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 1.020 0.857 372 94 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu -0.09065(4) 0.38823(4) 0.01323(3) 0.03497(14) Uani 1 1 d . . . . .
O8 O 0.8819(2) 0.4961(2) 0.9315(2) 0.0389(5) Uani 1 1 d . . . . .
O2 O -0.0321(2) 0.2978(2) 0.1014(2) 0.0384(5) Uani 1 1 d . . . . .
O4 O -0.0279(2) 0.3409(3) 0.3615(2) 0.0502(7) Uani 1 1 d . . . . .
O7 O 0.6844(3) 0.4003(3) 0.8608(3) 0.0522(7) Uani 1 1 d . . . . .
O3 O 0.1440(3) 0.0628(3) 0.1245(3) 0.0535(7) Uani 1 1 d . . . . .
N3 N -0.1162(3) 0.5213(3) 0.1577(3) 0.0420(7) Uani 1 1 d . . . . .
N1 N 0.0570(3) 0.1980(3) 0.2471(3) 0.0379(6) Uani 1 1 d . . . . .
N4 N -0.0867(3) 1.2406(3) 0.8626(2) 0.0388(6) Uani 1 1 d . . . . .
O5 O 0.7139(3) 0.3557(3) 0.5999(3) 0.0601(8) Uani 1 1 d . . . . .
O1 O -0.2244(3) 0.1970(3) 0.0536(3) 0.0609(8) Uani 1 1 d . . . . .
O6 O 0.5444(3) 0.6477(3) 0.8279(3) 0.0662(9) Uani 1 1 d . . . . .
N2 N 0.6297(3) 0.5047(3) 0.7091(3) 0.0467(7) Uani 1 1 d . . . . .
C6 C 0.1863(3) 0.3761(3) 0.4446(3) 0.0379(7) Uani 1 1 d . . . . .
C3 C 0.1568(3) 0.1526(3) 0.2220(3) 0.0401(7) Uani 1 1 d . . . . .
C4 C 0.0656(3) 0.3077(3) 0.3514(3) 0.0388(7) Uani 1 1 d . . . . .
C5 C 0.2771(3) 0.2166(3) 0.3215(3) 0.0404(7) Uani 1 1 d . . . . .
C8 C 0.2879(3) 0.3257(3) 0.4287(3) 0.0373(7) Uani 1 1 d . . . . .
C20 C -0.0224(4) 0.5848(3) 0.2628(3) 0.0446(8) Uani 1 1 d . . . . .
H20 H 0.051665 0.558327 0.268823 0.053 Uiso 1 1 calc R . . . .
C11 C 0.4015(3) 0.3856(3) 0.5227(3) 0.0390(7) Uani 1 1 d . . . . .
C18 C 0.7703(4) 0.4766(3) 0.8696(3) 0.0425(8) Uani 1 1 d . . . . .
C30 C 0.0178(4) 1.2047(3) 0.8617(3) 0.0433(8) Uani 1 1 d . . . . .
H30 H 0.088392 1.251283 0.931841 0.052 Uiso 1 1 calc R . . . .
C13 C 0.5033(3) 0.3340(4) 0.5073(4) 0.0440(8) Uani 1 1 d . . . . .
C26 C -0.0745(4) 1.0305(3) 0.6605(3) 0.0464(9) Uani 1 1 d . . . . .
C28 C 0.0271(4) 1.1026(3) 0.7628(4) 0.0467(8) Uani 1 1 d . . . . .
H28 H 0.103548 1.081992 0.765237 0.056 Uiso 1 1 calc R . . . .
C14 C 0.4124(3) 0.4951(4) 0.6307(3) 0.0425(7) Uani 1 1 d . . . . .
C1 C -0.1123(3) 0.2163(3) 0.0992(3) 0.0390(7) Uani 1 1 d . . . . .
C29 C -0.1867(4) 1.1720(4) 0.7625(3) 0.0472(8) Uani 1 1 d . . . . .
H29 H -0.261366 1.196614 0.761542 0.057 Uiso 1 1 calc R . . . .
C9 C 0.1994(4) 0.4854(4) 0.5487(3) 0.0435(8) Uani 1 1 d . . . . .
H9 H 0.131263 0.520366 0.557407 0.052 Uiso 1 1 calc R . . . .
C23 C -0.1367(4) 0.7285(3) 0.3565(3) 0.0478(9) Uani 1 1 d . . . . .
C15 C 0.6227(4) 0.3953(4) 0.6058(4) 0.0491(9) Uani 1 1 d . . . . .
C19 C -0.2225(4) 0.5580(4) 0.1526(3) 0.0462(8) Uani 1 1 d . . . . .
H19 H -0.290523 0.511586 0.080097 0.055 Uiso 1 1 calc R . . . .
C24 C -0.1530(4) 0.8396(3) 0.4560(3) 0.0491(9) Uani 1 1 d . . . . .
H24 H -0.232031 0.854948 0.446862 0.059 Uiso 1 1 calc R . . . .
C21 C -0.2358(4) 0.6597(4) 0.2484(4) 0.0496(9) Uani 1 1 d . . . . .
H21 H -0.311432 0.682843 0.241191 0.060 Uiso 1 1 calc R . . . .
C12 C 0.3133(4) 0.5454(4) 0.6420(3) 0.0437(8) Uani 1 1 d . . . . .
H12 H 0.321717 0.620971 0.713186 0.052 Uiso 1 1 calc R . . . .
C25 C -0.0613(5) 0.9195(3) 0.5583(4) 0.0498(9) Uani 1 1 d . . . . .
H25 H 0.017531 0.903994 0.565901 0.060 Uiso 1 1 calc R . . . .
C2 C -0.0646(3) 0.1347(3) 0.1564(3) 0.0404(7) Uani 1 1 d . . . . .
H2A H -0.121649 0.115644 0.194678 0.049 Uiso 1 1 calc R . . . .
H2B H -0.062041 0.052491 0.092410 0.049 Uiso 1 1 calc R . . . .
C22 C -0.0302(4) 0.6884(3) 0.3635(3) 0.0482(9) Uani 1 1 d . . . . .
H22 H 0.037643 0.730963 0.436509 0.058 Uiso 1 1 calc R . . . .
C16 C 0.5310(4) 0.5566(4) 0.7307(4) 0.0480(9) Uani 1 1 d . . . . .
C27 C -0.1842(4) 1.0668(4) 0.6609(3) 0.0496(9) Uani 1 1 d . . . . .
H27 H -0.256276 1.020069 0.592500 0.060 Uiso 1 1 calc R . . . .
C7 C 0.3777(4) 0.1697(4) 0.3070(4) 0.0519(9) Uani 1 1 d . . . . .
H7 H 0.370642 0.097490 0.233634 0.062 Uiso 1 1 calc R . . . .
C17 C 0.7472(4) 0.5611(4) 0.8086(4) 0.0511(10) Uani 1 1 d . . . . .
H17A H 0.747214 0.646874 0.869010 0.061 Uiso 1 1 calc R . . . .
H17B H 0.813703 0.571213 0.776918 0.061 Uiso 1 1 calc R . . . .
C10 C 0.4909(4) 0.2295(4) 0.4017(4) 0.0563(10) Uani 1 1 d . . . . .
H10 H 0.559776 0.196391 0.391790 0.068 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O8 2.434(3) 2_666 ?
Cu1 O8 1.992(2) 1_454 ?
Cu1 O2 1.937(2) . ?
Cu1 N3 1.998(3) . ?
Cu1 N4 2.016(3) 1_544 ?
O8 C18 1.280(5) . ?
O2 C1 1.263(5) . ?
O4 C4 1.222(4) . ?
O7 C18 1.229(5) . ?
O3 C3 1.220(4) . ?
N3 C20 1.345(5) . ?
N3 C19 1.357(5) . ?
N1 C3 1.397(4) . ?
N1 C4 1.397(5) . ?
N1 C2 1.460(5) . ?
N4 C30 1.341(5) . ?
N4 C29 1.354(5) . ?
O5 C15 1.221(5) . ?
O1 C1 1.243(4) . ?
O6 C16 1.222(5) . ?
N2 C15 1.394(6) . ?
N2 C16 1.404(5) . ?
N2 C17 1.469(5) . ?
C6 C4 1.469(5) . ?
C6 C8 1.413(5) . ?
C6 C9 1.379(5) . ?
C3 C5 1.492(5) . ?
C5 C8 1.407(5) . ?
C5 C7 1.380(5) . ?
C8 C11 1.409(5) . ?
C20 H20 0.9500 . ?
C20 C22 1.401(5) . ?
C11 C13 1.421(5) . ?
C11 C14 1.415(5) . ?
C18 C17 1.531(5) . ?
C30 H30 0.9500 . ?
C30 C28 1.385(5) . ?
C13 C15 1.479(5) . ?
C13 C10 1.364(6) . ?
C26 C28 1.382(6) . ?
C26 C25 1.481(5) . ?
C26 C27 1.400(6) . ?
C28 H28 0.9500 . ?
C14 C12 1.376(5) . ?
C14 C16 1.480(5) . ?
C1 C2 1.528(4) . ?
C29 H29 0.9500 . ?
C29 C27 1.392(5) . ?
C9 H9 0.9500 . ?
C9 C12 1.407(5) . ?
C23 C24 1.479(5) . ?
C23 C21 1.401(6) . ?
C23 C22 1.378(6) . ?
C19 H19 0.9500 . ?
C19 C21 1.379(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.338(6) . ?
C21 H21 0.9500 . ?
C12 H12 0.9500 . ?
C25 H25 0.9500 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C22 H22 0.9500 . ?
C27 H27 0.9500 . ?
C7 H7 0.9500 . ?
C7 C10 1.409(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C10 H10 0.9500 . ?

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
O8 Cu1 O8 79.28(10) 1_454 2_666 ?
O8 Cu1 N3 89.87(11) 1_454 . ?
O8 Cu1 N4 92.08(11) 1_454 1_544 ?
O2 Cu1 O8 90.07(10) . 2_666 ?
O2 Cu1 O8 169.35(11) . 1_454 ?
O2 Cu1 N3 91.18(11) . . ?
O2 Cu1 N4 88.24(11) . 1_544 ?
N3 Cu1 O8 93.34(12) . 2_666 ?
N3 Cu1 N4 172.52(13) . 1_544 ?
N4 Cu1 O8 94.12(12) 1_544 2_666 ?
Cu1 O8 Cu1 100.72(10) 1_656 2_666 ?
C18 O8 Cu1 114.5(2) . 1_656 ?
C18 O8 Cu1 144.7(2) . 2_666 ?
C1 O2 Cu1 116.2(2) . . ?
C20 N3 Cu1 119.3(3) . . ?
C20 N3 C19 117.8(3) . . ?
C19 N3 Cu1 122.7(2) . . ?
C3 N1 C4 124.3(3) . . ?
C3 N1 C2 119.3(3) . . ?
C4 N1 C2 116.1(3) . . ?
C30 N4 Cu1 119.3(2) . 1_566 ?
C30 N4 C29 117.8(3) . . ?
C29 N4 Cu1 122.9(3) . 1_566 ?
C15 N2 C16 125.4(3) . . ?
C15 N2 C17 116.7(3) . . ?
C16 N2 C17 117.6(4) . . ?
C8 C6 C4 119.2(3) . . ?
C9 C6 C4 120.3(3) . . ?
C9 C6 C8 120.4(3) . . ?
O3 C3 N1 120.9(3) . . ?
O3 C3 C5 122.6(3) . . ?
N1 C3 C5 116.5(3) . . ?
O4 C4 N1 118.5(3) . . ?
O4 C4 C6 123.2(3) . . ?
N1 C4 C6 118.3(3) . . ?
C8 C5 C3 119.9(3) . . ?
C7 C5 C3 119.7(3) . . ?
C7 C5 C8 120.4(3) . . ?
C5 C8 C6 121.2(3) . . ?
C5 C8 C11 119.8(3) . . ?
C11 C8 C6 119.0(3) . . ?
N3 C20 H20 118.9 . . ?
N3 C20 C22 122.2(4) . . ?
C22 C20 H20 118.9 . . ?
C8 C11 C13 119.0(3) . . ?
C8 C11 C14 119.9(3) . . ?
C14 C11 C13 121.1(3) . . ?
O8 C18 C17 115.2(3) . . ?
O7 C18 O8 124.6(3) . . ?
O7 C18 C17 120.2(3) . . ?
N4 C30 H30 118.7 . . ?
N4 C30 C28 122.7(4) . . ?
C28 C30 H30 118.7 . . ?
C11 C13 C15 119.5(4) . . ?
C10 C13 C11 120.0(4) . . ?
C10 C13 C15 120.5(4) . . ?
C28 C26 C25 118.4(4) . . ?
C28 C26 C27 117.4(3) . . ?
C27 C26 C25 124.1(4) . . ?
C30 C28 H28 119.9 . . ?
C26 C28 C30 120.2(4) . . ?
C26 C28 H28 119.9 . . ?
C11 C14 C16 120.0(3) . . ?
C12 C14 C11 120.0(3) . . ?
C12 C14 C16 120.0(4) . . ?
O2 C1 C2 115.9(3) . . ?
O1 C1 O2 125.5(3) . . ?
O1 C1 C2 118.5(3) . . ?
N4 C29 H29 118.8 . . ?
N4 C29 C27 122.4(4) . . ?
C27 C29 H29 118.8 . . ?
C6 C9 H9 119.8 . . ?
C6 C9 C12 120.3(3) . . ?
C12 C9 H9 119.8 . . ?
C21 C23 C24 118.0(4) . . ?
C22 C23 C24 124.1(4) . . ?
C22 C23 C21 117.9(3) . . ?
O5 C15 N2 119.5(4) . . ?
O5 C15 C13 123.3(4) . . ?
N2 C15 C13 117.2(3) . . ?
N3 C19 H19 118.6 . . ?
N3 C19 C21 122.8(4) . . ?
C21 C19 H19 118.6 . . ?
C23 C24 H24 118.5 . . ?
C25 C24 C23 122.9(4) . . ?
C25 C24 H24 118.5 . . ?
C23 C21 H21 120.3 . . ?
C19 C21 C23 119.4(4) . . ?
C19 C21 H21 120.3 . . ?
C14 C12 C9 120.3(3) . . ?
C14 C12 H12 119.8 . . ?
C9 C12 H12 119.8 . . ?
C26 C25 H25 117.8 . . ?
C24 C25 C26 124.5(4) . . ?
C24 C25 H25 117.8 . . ?
N1 C2 C1 112.2(3) . . ?
N1 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C20 C22 H22 120.1 . . ?
C23 C22 C20 119.8(4) . . ?
C23 C22 H22 120.1 . . ?
O6 C16 N2 120.6(4) . . ?
O6 C16 C14 122.8(4) . . ?
N2 C16 C14 116.6(4) . . ?
C26 C27 H27 120.3 . . ?
C29 C27 C26 119.4(4) . . ?
C29 C27 H27 120.3 . . ?
C5 C7 H7 120.2 . . ?
C5 C7 C10 119.6(4) . . ?
C10 C7 H7 120.2 . . ?
N2 C17 C18 110.9(3) . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 108.0 . . ?
C13 C10 C7 121.2(4) . . ?
C13 C10 H10 119.4 . . ?
C7 C10 H10 119.4 . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_RINTA01_5                   
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: Best quality data that could be obtained.
;
_vrf_PLAT020_5                   
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.150 Report
RESPONSE: Best quality data that could be obtained.
;
_vrf_PLAT430_5                   
;
PROBLEM: Short Inter D...A Contact O8     ..N4      .       2.89 Ang.      
RESPONSE: Donor atoms within coodination sphere.
;
_exptl_crystal_recrystallization_method 
'Crystallised at elevated temperature from synthesis'
####################################################################### 
# 
# 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_merge_pl
_database_code_depnum_ccdc_archive 'CCDC 1840389'
_audit_update_record             
;
2018-04-30 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_audit_creation_date             2018-01-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H16 Co N4 O8'
_chemical_formula_sum            'C28 H16 Co N4 O8'
_chemical_formula_weight         595.38
_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 0.0030 0.0020 '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'
Co Co 0.3570 0.9660 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0070 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0120 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           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                   7.2510(15)
_cell_length_b                   18.380(4)
_cell_length_c                   17.791(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.74(3)
_cell_angle_gamma                90
_cell_volume                     2368.4(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    42489
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.746
_cell_measurement_theta_min      1.594
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.969
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.3037
_diffrn_reflns_av_unetI/netI     0.1461
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30307
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.594
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4992
_reflns_number_total             5398
_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       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.728
_refine_diff_density_min         -2.359
_refine_diff_density_rms         0.202
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5398
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0657
_refine_ls_restrained_S_all      1.218
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0610P)²+0.3263P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1444
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
 C25(H25), C26(H26), C27(H27), C28(H28)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Co1 Co 0.26709(4) 0.37802(2) 0.61144(2) 0.01372(13) Uani 1 1 d . . . . .
O1 O 0.3555(2) 0.26019(8) 0.60469(8) 0.0182(3) Uani 1 1 d . . . . .
O2 O 0.5411(2) 0.35040(8) 0.63805(8) 0.0181(3) Uani 1 1 d . . . . .
O3 O 0.6348(2) 0.21988(8) 0.47518(9) 0.0223(3) Uani 1 1 d . . . . .
O4 O 0.6437(3) 0.10678(10) 0.70280(9) 0.0270(4) Uani 1 1 d . . . . .
O5 O 0.0138(2) 0.34383(8) 0.64573(8) 0.0188(3) Uani 1 1 d . . . . .
O6 O 0.2072(2) 0.38540(8) 0.73487(9) 0.0186(3) Uani 1 1 d . . . . .
O7 O 0.0572(2) 0.29310(8) 0.90319(9) 0.0224(3) Uani 1 1 d . . . . .
O8 O -0.1521(2) 0.48914(9) 0.76977(8) 0.0225(3) Uani 1 1 d . . . . .
N1 N 0.6362(2) 0.16365(9) 0.58899(10) 0.0179(4) Uani 1 1 d . . . . .
N2 N -0.0638(3) 0.39040(10) 0.83853(9) 0.0160(3) Uani 1 1 d . . . . .
N3 N 0.2888(2) 0.38950(10) 0.49541(10) 0.0153(3) Uani 1 1 d . . . . .
N4 N 0.2181(2) 0.48937(9) 0.59765(10) 0.0155(3) Uani 1 1 d . . . . .
C1 C 0.5126(3) 0.28412(11) 0.62189(11) 0.0165(4) Uani 1 1 d . . . . .
C2 C 0.6796(3) 0.23362(11) 0.62475(13) 0.0220(4) Uani 1 1 d . . . . .
H2A H 0.781879 0.257058 0.598880 0.026 Uiso 1 1 calc R . . . .
H2B H 0.721358 0.225404 0.677870 0.026 Uiso 1 1 calc R . . . .
C3 C 0.6189(3) 0.10277(11) 0.63467(12) 0.0172(4) Uani 1 1 d . . . . .
C4 C 0.6065(3) 0.16479(11) 0.51077(12) 0.0163(4) Uani 1 1 d . . . . .
C5 C 0.5696(3) 0.03343(10) 0.59633(10) 0.0137(4) Uani 1 1 d . . . . .
C6 C 0.5417(3) 0.09658(10) 0.47411(10) 0.0134(4) Uani 1 1 d . . . . .
C7 C 0.5590(3) -0.02976(11) 0.63799(11) 0.0161(4) Uani 1 1 d . . . . .
H7 H 0.589218 -0.029073 0.690535 0.019 Uiso 1 1 calc R . . . .
C8 C 0.5281(2) 0.03266(10) 0.51770(10) 0.0120(4) Uani 1 1 d . . . . .
C9 C 0.4967(3) 0.09520(11) 0.39751(11) 0.0157(4) Uani 1 1 d . . . . .
H9 H 0.503504 0.138620 0.368807 0.019 Uiso 1 1 calc R . . . .
C10 C 0.0534(3) 0.36019(11) 0.71397(11) 0.0154(4) Uani 1 1 d . . . . .
C11 C -0.0949(3) 0.34674(11) 0.77046(11) 0.0189(4) Uani 1 1 d . . . . .
H11A H -0.217418 0.358748 0.746785 0.023 Uiso 1 1 calc R . . . .
H11B H -0.095247 0.294550 0.784194 0.023 Uiso 1 1 calc R . . . .
C12 C 0.0131(3) 0.35726(11) 0.90339(10) 0.0149(4) Uani 1 1 d . . . . .
C13 C -0.0986(3) 0.46465(11) 0.83075(11) 0.0162(4) Uani 1 1 d . . . . .
C14 C 0.0325(3) 0.40306(10) 0.97186(10) 0.0133(4) Uani 1 1 d . . . . .
C15 C -0.0725(3) 0.51046(11) 0.89859(10) 0.0133(4) Uani 1 1 d . . . . .
C16 C 0.0929(3) 0.37242(10) 1.03975(12) 0.0166(4) Uani 1 1 d . . . . .
H16 H 0.121343 0.322013 1.042508 0.020 Uiso 1 1 calc R . . . .
C17 C -0.0100(2) 0.47794(10) 0.96743(10) 0.0120(4) Uani 1 1 d . . . . .
C18 C -0.1121(3) 0.58400(11) 0.89543(10) 0.0157(4) Uani 1 1 d . . . . .
H18 H -0.152761 0.605333 0.848901 0.019 Uiso 1 1 calc R . . . .
C19 C 0.3693(3) 0.34924(13) 0.37352(11) 0.0220(4) Uani 1 1 d . . . . .
H19 H 0.398164 0.310374 0.340898 0.026 Uiso 1 1 calc R . . . .
C20 C 0.3665(3) 0.42027(12) 0.34799(11) 0.0210(4) Uani 1 1 d . . . . .
H20 H 0.396231 0.430925 0.297743 0.025 Uiso 1 1 calc R . . . .
C21 C 0.3292(3) 0.33577(11) 0.44788(11) 0.0185(4) Uani 1 1 d . . . . .
H21 H 0.330311 0.286996 0.465575 0.022 Uiso 1 1 calc R . . . .
C22 C 0.3198(3) 0.47611(12) 0.39644(11) 0.0190(4) Uani 1 1 d . . . . .
H22 H 0.313634 0.525106 0.379509 0.023 Uiso 1 1 calc R . . . .
C23 C 0.2823(3) 0.45848(11) 0.47028(10) 0.0151(4) Uani 1 1 d . . . . .
C24 C 0.2326(3) 0.51425(11) 0.52646(11) 0.0151(4) Uani 1 1 d . . . . .
C25 C 0.1987(3) 0.58645(11) 0.50748(12) 0.0194(4) Uani 1 1 d . . . . .
H25 H 0.210838 0.602852 0.457323 0.023 Uiso 1 1 calc R . . . .
C26 C 0.1465(3) 0.63443(12) 0.56323(14) 0.0216(4) Uani 1 1 d . . . . .
H26 H 0.122057 0.684044 0.551592 0.026 Uiso 1 1 calc R . . . .
C27 C 0.1682(3) 0.53601(11) 0.65101(12) 0.0182(4) Uani 1 1 d . . . . .
H27 H 0.157961 0.518534 0.700889 0.022 Uiso 1 1 calc R . . . .
C28 C 0.1308(3) 0.60873(12) 0.63614(13) 0.0211(4) Uani 1 1 d . . . . .
H28 H 0.095197 0.640413 0.675066 0.025 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.2633(16) . ?
Co1 O2 2.0834(17) . ?
Co1 O5 2.0609(15) . ?
Co1 O6 2.2628(16) . ?
Co1 N3 2.0885(17) . ?
Co1 N4 2.0897(18) . ?
Co1 C1 2.480(2) . ?
Co1 C10 2.4712(19) . ?
O1 C1 1.246(3) . ?
O2 C1 1.267(3) . ?
O3 C4 1.217(2) . ?
O4 C3 1.219(3) . ?
O5 C10 1.270(3) . ?
O6 C10 1.248(3) . ?
O7 C12 1.222(3) . ?
O8 C13 1.220(3) . ?
N1 C2 1.462(3) . ?
N1 C3 1.392(3) . ?
N1 C4 1.398(3) . ?
N2 C11 1.461(3) . ?
N2 C12 1.397(3) . ?
N2 C13 1.393(3) . ?
N3 C21 1.342(2) . ?
N3 C23 1.344(3) . ?
N4 C24 1.355(2) . ?
N4 C27 1.341(2) . ?
C1 C2 1.525(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C5 1.481(3) . ?
C4 C6 1.480(3) . ?
C5 C7 1.382(3) . ?
C5 C8 1.417(3) . ?
C6 C8 1.414(2) . ?
C6 C9 1.386(3) . ?
C7 H7 0.9500 . ?
C7 C9 1.409(3) 3_656 ?
C8 C8 1.407(4) 3_656 ?
C9 H9 0.9500 . ?
C10 C11 1.526(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C14 1.482(3) . ?
C13 C15 1.476(3) . ?
C14 C16 1.385(3) . ?
C14 C17 1.412(3) . ?
C15 C17 1.418(3) . ?
C15 C18 1.383(3) . ?
C16 H16 0.9500 . ?
C16 C18 1.406(3) 3_567 ?
C17 C17 1.416(4) 3_567 ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C19 C20 1.382(3) . ?
C19 C21 1.390(3) . ?
C20 H20 0.9500 . ?
C20 C22 1.392(3) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C22 C23 1.392(2) . ?
C23 C24 1.488(3) . ?
C24 C25 1.388(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.393(3) . ?
C26 H26 0.9500 . ?
C26 C28 1.390(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.387(3) . ?
C28 H28 0.9500 . ?

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 Co1 C1 30.01(6) . . ?
O1 Co1 C10 95.82(6) . . ?
O2 Co1 O1 60.63(6) . . ?
O2 Co1 O6 91.10(6) . . ?
O2 Co1 N3 97.64(7) . . ?
O2 Co1 N4 114.85(7) . . ?
O2 Co1 C1 30.68(6) . . ?
O2 Co1 C10 115.15(7) . . ?
O5 Co1 O1 89.00(6) . . ?
O5 Co1 O2 135.42(6) . . ?
O5 Co1 O6 61.05(6) . . ?
O5 Co1 N3 115.71(7) . . ?
O5 Co1 N4 100.63(6) . . ?
O5 Co1 C1 114.35(7) . . ?
O5 Co1 C10 30.89(7) . . ?
O6 Co1 O1 100.19(5) . . ?
O6 Co1 C1 98.01(6) . . ?
O6 Co1 C10 30.17(7) . . ?
N3 Co1 O1 90.53(6) . . ?
N3 Co1 O6 168.58(7) . . ?
N3 Co1 N4 78.78(7) . . ?
N3 Co1 C1 93.24(7) . . ?
N3 Co1 C10 145.35(8) . . ?
N4 Co1 O1 167.93(5) . . ?
N4 Co1 O6 90.90(6) . . ?
N4 Co1 C1 143.87(7) . . ?
N4 Co1 C10 96.17(6) . . ?
C10 Co1 C1 109.00(7) . . ?
C1 O1 Co1 84.67(12) . . ?
C1 O2 Co1 92.24(13) . . ?
C10 O5 Co1 92.69(12) . . ?
C10 O6 Co1 84.19(12) . . ?
C3 N1 C2 118.45(18) . . ?
C3 N1 C4 125.40(18) . . ?
C4 N1 C2 116.07(17) . . ?
C12 N2 C11 118.99(17) . . ?
C13 N2 C11 115.82(17) . . ?
C13 N2 C12 124.91(18) . . ?
C21 N3 Co1 125.29(14) . . ?
C21 N3 C23 119.33(17) . . ?
C23 N3 Co1 114.90(13) . . ?
C24 N4 Co1 114.82(13) . . ?
C27 N4 Co1 126.36(14) . . ?
C27 N4 C24 118.77(18) . . ?
O1 C1 Co1 65.33(11) . . ?
O1 C1 O2 122.21(19) . . ?
O1 C1 C2 120.59(18) . . ?
O2 C1 Co1 57.08(11) . . ?
O2 C1 C2 117.20(19) . . ?
C2 C1 Co1 172.87(14) . . ?
N1 C2 C1 111.51(19) . . ?
N1 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
O4 C3 N1 121.2(2) . . ?
O4 C3 C5 122.06(19) . . ?
N1 C3 C5 116.69(18) . . ?
O3 C4 N1 120.58(19) . . ?
O3 C4 C6 122.25(19) . . ?
N1 C4 C6 117.17(17) . . ?
C7 C5 C3 119.64(18) . . ?
C7 C5 C8 120.43(18) . . ?
C8 C5 C3 119.90(17) . . ?
C8 C6 C4 119.43(18) . . ?
C9 C6 C4 120.25(17) . . ?
C9 C6 C8 120.32(18) . . ?
C5 C7 H7 120.0 . . ?
C5 C7 C9 119.95(18) . 3_656 ?
C9 C7 H7 120.0 3_656 . ?
C6 C8 C5 121.08(18) . . ?
C8 C8 C5 119.6(2) 3_656 . ?
C8 C8 C6 119.3(2) 3_656 . ?
C6 C9 C7 120.36(17) . 3_656 ?
C6 C9 H9 119.8 . . ?
C7 C9 H9 119.8 3_656 . ?
O5 C10 Co1 56.42(9) . . ?
O5 C10 C11 117.20(18) . . ?
O6 C10 Co1 65.64(10) . . ?
O6 C10 O5 122.04(17) . . ?
O6 C10 C11 120.76(18) . . ?
C11 C10 Co1 173.58(16) . . ?
N2 C11 C10 111.80(17) . . ?
N2 C11 H11A 109.3 . . ?
N2 C11 H11B 109.3 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
O7 C12 N2 120.84(19) . . ?
O7 C12 C14 122.41(19) . . ?
N2 C12 C14 116.72(17) . . ?
O8 C13 N2 119.85(19) . . ?
O8 C13 C15 122.63(18) . . ?
N2 C13 C15 117.50(18) . . ?
C16 C14 C12 119.98(17) . . ?
C16 C14 C17 120.28(17) . . ?
C17 C14 C12 119.74(17) . . ?
C17 C15 C13 119.29(17) . . ?
C18 C15 C13 120.40(18) . . ?
C18 C15 C17 120.30(18) . . ?
C14 C16 H16 120.0 . . ?
C14 C16 C18 119.92(18) . 3_567 ?
C18 C16 H16 120.0 3_567 . ?
C14 C17 C15 121.27(17) . . ?
C14 C17 C17 119.9(2) . 3_567 ?
C17 C17 C15 118.8(2) 3_567 . ?
C15 C18 C16 120.76(18) . 3_567 ?
C15 C18 H18 119.6 . . ?
C16 C18 H18 119.6 3_567 . ?
C20 C19 H19 120.6 . . ?
C20 C19 C21 118.71(19) . . ?
C21 C19 H19 120.6 . . ?
C19 C20 H20 120.2 . . ?
C19 C20 C22 119.54(18) . . ?
C22 C20 H20 120.2 . . ?
N3 C21 C19 122.0(2) . . ?
N3 C21 H21 119.0 . . ?
C19 C21 H21 119.0 . . ?
C20 C22 H22 120.8 . . ?
C23 C22 C20 118.47(19) . . ?
C23 C22 H22 120.8 . . ?
N3 C23 C22 121.87(18) . . ?
N3 C23 C24 115.59(16) . . ?
C22 C23 C24 122.55(18) . . ?
N4 C24 C23 115.31(17) . . ?
N4 C24 C25 121.94(18) . . ?
C25 C24 C23 122.74(18) . . ?
C24 C25 H25 120.6 . . ?
C24 C25 C26 118.87(19) . . ?
C26 C25 H25 120.6 . . ?
C25 C26 H26 120.4 . . ?
C28 C26 C25 119.1(2) . . ?
C28 C26 H26 120.4 . . ?
N4 C27 H27 118.7 . . ?
N4 C27 C28 122.53(19) . . ?
C28 C27 H27 118.7 . . ?
C26 C28 H28 120.6 . . ?
C27 C28 C26 118.78(19) . . ?
C27 C28 H28 120.6 . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT020_merge_pl            
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.298 Report
RESPONSE: This is the best data that could be obtained. Structure unambiguous.
;
# start Validation Reply Form
_vrf_RINTA01_merge_pl            
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: This is the best data that could be obtained. Structure unambiguous.
;
_exptl_crystal_recrystallization_method 
'Crystallised at elevated temperature from synthesis'
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1840388'
_audit_update_record             
;
2018-04-30 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_audit_creation_date             2018-01-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H11 N2 O10 Zn, 0.25(H2 O)'
_chemical_formula_sum            'C18 H11.50 N2 O10.25 Zn'
_chemical_formula_weight         485.16
_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 0.0030 0.0020 '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 0.0070 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0120 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3120 1.4670 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.827(3)
_cell_length_b                   28.485(6)
_cell_length_c                   7.4000(15)
_cell_angle_alpha                90
_cell_angle_beta                 90.71(3)
_cell_angle_gamma                90
_cell_volume                     3546.7(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    28533
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.497
_cell_measurement_theta_min      1.406
_shelx_estimated_absorpt_T_max   0.986
_shelx_estimated_absorpt_T_min   0.944
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   none
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            28533
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.497
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.406
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3395
_reflns_number_total             4081
_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       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.533
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4081
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0866
_refine_ls_restrained_S_all      1.079
_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)+(0.1198P)²+79.4398P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2614
_refine_ls_wR_factor_ref         0.2687
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O11(0.25)
3.a Rotating group:
 O9(H9A,H9B), O10(H10A,H10B)
3.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C12(H12)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.28183(5) 0.53415(3) 0.28866(12) 0.0287(3) Uani 1 1 d . . . . .
O1 O 0.3276(4) 0.57595(18) 0.4792(8) 0.0379(13) Uani 1 1 d . . . . .
O2 O 0.3343(4) 0.64213(18) 0.3167(8) 0.0368(12) Uani 1 1 d . . . . .
O3 O 0.5188(3) 0.65261(16) 0.4973(7) 0.0301(11) Uani 1 1 d . . . . .
O4 O 0.2927(3) 0.72592(18) 0.6711(7) 0.0318(11) Uani 1 1 d . . . . .
O5 O 0.6981(3) 0.87436(17) 0.3447(7) 0.0283(10) Uani 1 1 d . . . . .
O6 O 0.4686(3) 0.94572(17) 0.5066(8) 0.0324(11) Uani 1 1 d . . . . .
O7 O 0.7261(3) 1.00070(16) 0.4995(7) 0.0298(11) Uani 1 1 d . . . . .
O8 O 0.6837(4) 0.94247(17) 0.6649(7) 0.0349(12) Uani 1 1 d . . . . .
O9 O 0.3546(7) 0.5708(3) 0.0891(12) 0.089(4) Uani 1 1 d . . . . .
H9A H 0.398820 0.554044 0.060715 0.134 Uiso 1 1 d GR . . . .
H9B H 0.375751 0.597723 0.135750 0.134 Uiso 1 1 d GR . . . .
O10 O 0.3544(4) 0.4772(2) 0.2685(9) 0.0451(14) Uani 1 1 d . . . . .
H10A H 0.339204 0.454123 0.343868 0.068 Uiso 1 1 d GR . . . .
H10B H 0.404063 0.483596 0.307946 0.068 Uiso 1 1 d GR . . . .
N1 N 0.4082(3) 0.68993(19) 0.5937(7) 0.0227(11) Uani 1 1 d . . . . .
N2 N 0.5809(3) 0.90922(17) 0.4132(7) 0.0211(10) Uani 1 1 d . . . . .
C1 C 0.3424(4) 0.6203(2) 0.4579(10) 0.0282(14) Uani 1 1 d . . . . .
C2 C 0.3727(4) 0.6439(2) 0.6309(10) 0.0281(14) Uani 1 1 d . . . . .
H2 H 0.330(6) 0.650(3) 0.704(13) 0.034 Uiso 1 1 d R . . . .
C3 C 0.4847(4) 0.6897(2) 0.5234(8) 0.0208(12) Uani 1 1 d . . . . .
C4 C 0.3610(4) 0.7298(2) 0.6183(8) 0.0208(12) Uani 1 1 d . . . . .
C5 C 0.5214(3) 0.7358(2) 0.4893(8) 0.0170(11) Uani 1 1 d . . . . .
C6 C 0.3982(4) 0.7758(2) 0.5814(8) 0.0183(11) Uani 1 1 d . . . . .
C7 C 0.5991(4) 0.7387(2) 0.4281(8) 0.0193(11) Uani 1 1 d . . . . .
H7 H 0.628240 0.710779 0.406304 0.023 Uiso 1 1 calc R . . . .
C8 C 0.4769(3) 0.7773(2) 0.5201(7) 0.0152(10) Uani 1 1 d . . . . .
C9 C 0.3554(4) 0.8164(2) 0.6082(8) 0.0210(12) Uani 1 1 d . . . . .
H9 H 0.302012 0.814651 0.647843 0.025 Uiso 1 1 calc R . . . .
C10 C 0.6347(4) 0.7825(2) 0.3982(8) 0.0212(12) Uani 1 1 d . . . . .
H10 H 0.688103 0.784096 0.358186 0.025 Uiso 1 1 calc R . . . .
C11 C 0.5124(3) 0.8215(2) 0.4878(7) 0.0160(11) Uani 1 1 d . . . . .
C12 C 0.3905(4) 0.8603(2) 0.5772(8) 0.0207(12) Uani 1 1 d . . . . .
H12 H 0.361373 0.888350 0.597462 0.025 Uiso 1 1 calc R . . . .
C13 C 0.5922(4) 0.8235(2) 0.4270(8) 0.0175(11) Uani 1 1 d . . . . .
C14 C 0.4680(4) 0.8625(2) 0.5168(8) 0.0184(11) Uani 1 1 d . . . . .
C15 C 0.6292(4) 0.8696(2) 0.3918(8) 0.0198(12) Uani 1 1 d . . . . .
C16 C 0.5041(4) 0.9092(2) 0.4819(8) 0.0206(12) Uani 1 1 d . . . . .
C17 C 0.6193(4) 0.9542(2) 0.3800(9) 0.0267(13) Uani 1 1 d . . . . .
H17A H 0.578466 0.979192 0.376463 0.032 Uiso 1 1 calc R . . . .
H17B H 0.645025 0.953272 0.260443 0.032 Uiso 1 1 calc R . . . .
C18 C 0.6808(4) 0.9662(2) 0.5223(9) 0.0264(13) Uani 1 1 d . . . . .
O11 O 0.500000 0.5664(11) 0.250000 0.088(8) Uiso 0.5 2 d S T 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
Zn1 O1 1.993(5) . ?
Zn1 O7 2.063(5) 3_445 ?
Zn1 O8 1.993(6) 8_465 ?
Zn1 O9 2.194(8) . ?
Zn1 O10 2.038(6) . ?
Zn1 C18 2.587(7) 8_465 ?
O1 C1 1.297(8) . ?
O2 C1 1.222(9) . ?
O3 C3 1.221(8) . ?
O4 C4 1.223(8) . ?
O5 C15 1.222(8) . ?
O6 C16 1.214(8) . ?
O7 C18 1.257(8) . ?
O8 C18 1.253(9) . ?
O9 H9A 0.9115 . ?
O9 H9B 0.9115 . ?
O10 H10A 0.9006 . ?
O10 H10B 0.9002 . ?
N1 C2 1.469(8) . ?
N1 C3 1.394(8) . ?
N1 C4 1.399(8) . ?
N2 C15 1.401(8) . ?
N2 C16 1.394(8) . ?
N2 C17 1.457(7) . ?
C1 C2 1.528(10) . ?
C2 H2 0.92(10) . ?
C3 C5 1.474(8) . ?
C4 C6 1.481(8) . ?
C5 C7 1.390(8) . ?
C5 C8 1.419(8) . ?
C6 C8 1.405(8) . ?
C6 C9 1.377(9) . ?
C7 H7 0.9500 . ?
C7 C10 1.403(8) . ?
C8 C11 1.415(8) . ?
C9 H9 0.9500 . ?
C9 C12 1.404(9) . ?
C10 H10 0.9500 . ?
C10 C13 1.387(8) . ?
C11 C13 1.422(8) . ?
C11 C14 1.404(8) . ?
C12 H12 0.9500 . ?
C12 C14 1.385(8) . ?
C13 C15 1.479(8) . ?
C14 C16 1.487(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.506(10) . ?

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 O7 85.2(2) . 3_445 ?
O1 Zn1 O8 115.9(2) . 8_465 ?
O1 Zn1 O9 88.7(3) . . ?
O1 Zn1 O10 107.5(3) . . ?
O1 Zn1 C18 141.8(2) . 8_465 ?
O7 Zn1 O9 172.4(3) 3_445 . ?
O7 Zn1 C18 105.9(2) 3_445 8_465 ?
O8 Zn1 O7 96.9(2) 8_465 3_445 ?
O8 Zn1 O9 89.9(4) 8_465 . ?
O8 Zn1 O10 136.6(2) 8_465 . ?
O8 Zn1 C18 28.1(2) 8_465 8_465 ?
O9 Zn1 C18 81.7(3) . 8_465 ?
O10 Zn1 O7 88.0(2) . 3_445 ?
O10 Zn1 O9 89.4(4) . . ?
O10 Zn1 C18 109.3(2) . 8_465 ?
C1 O1 Zn1 124.7(5) . . ?
C18 O7 Zn1 138.1(5) . 3 ?
C18 O8 Zn1 103.3(4) . 8_566 ?
Zn1 O9 H9A 111.7 . . ?
Zn1 O9 H9B 111.4 . . ?
H9A O9 H9B 102.2 . . ?
Zn1 O10 H10A 111.1 . . ?
Zn1 O10 H10B 111.6 . . ?
H10A O10 H10B 102.6 . . ?
C3 N1 C2 116.5(5) . . ?
C3 N1 C4 125.4(5) . . ?
C4 N1 C2 117.9(5) . . ?
C15 N2 C17 115.4(5) . . ?
C16 N2 C15 125.7(5) . . ?
C16 N2 C17 118.5(5) . . ?
O1 C1 C2 112.9(6) . . ?
O2 C1 O1 125.5(7) . . ?
O2 C1 C2 121.7(6) . . ?
N1 C2 C1 111.6(6) . . ?
N1 C2 H2 104(6) . . ?
C1 C2 H2 109(6) . . ?
O3 C3 N1 120.1(6) . . ?
O3 C3 C5 123.0(6) . . ?
N1 C3 C5 116.9(5) . . ?
O4 C4 N1 120.4(6) . . ?
O4 C4 C6 122.7(6) . . ?
N1 C4 C6 116.9(5) . . ?
C7 C5 C3 120.5(5) . . ?
C7 C5 C8 120.2(5) . . ?
C8 C5 C3 119.3(5) . . ?
C8 C6 C4 119.2(5) . . ?
C9 C6 C4 119.5(5) . . ?
C9 C6 C8 121.2(5) . . ?
C5 C7 H7 119.7 . . ?
C5 C7 C10 120.7(5) . . ?
C10 C7 H7 119.7 . . ?
C6 C8 C5 121.9(5) . . ?
C6 C8 C11 118.8(5) . . ?
C11 C8 C5 119.3(5) . . ?
C6 C9 H9 119.9 . . ?
C6 C9 C12 120.1(6) . . ?
C12 C9 H9 119.9 . . ?
C7 C10 H10 120.0 . . ?
C13 C10 C7 120.0(6) . . ?
C13 C10 H10 120.0 . . ?
C8 C11 C13 119.4(5) . . ?
C14 C11 C8 119.2(5) . . ?
C14 C11 C13 121.4(5) . . ?
C9 C12 H12 120.2 . . ?
C14 C12 C9 119.5(6) . . ?
C14 C12 H12 120.2 . . ?
C10 C13 C11 120.5(5) . . ?
C10 C13 C15 120.1(5) . . ?
C11 C13 C15 119.5(5) . . ?
C11 C14 C16 119.9(5) . . ?
C12 C14 C11 121.1(5) . . ?
C12 C14 C16 119.0(5) . . ?
O5 C15 N2 119.8(5) . . ?
O5 C15 C13 123.5(6) . . ?
N2 C15 C13 116.7(5) . . ?
O6 C16 N2 121.0(6) . . ?
O6 C16 C14 122.5(6) . . ?
N2 C16 C14 116.5(5) . . ?
N2 C17 H17A 109.1 . . ?
N2 C17 H17B 109.1 . . ?
N2 C17 C18 112.6(6) . . ?
H17A C17 H17B 107.8 . . ?
C18 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
O7 C18 Zn1 73.2(4) . 8_566 ?
O7 C18 C17 119.7(6) . . ?
O8 C18 Zn1 48.6(4) . 8_566 ?
O8 C18 O7 121.2(7) . . ?
O8 C18 C17 119.0(6) . . ?
C17 C18 Zn1 166.2(5) . 8_566 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O9 H9A O11 0.91 2.22 2.711(12) 113.2 . yes
O9 H9B O2 0.91 1.98 2.663(10) 131.0 . yes
O9 H9B O3 0.91 2.57 3.226(9) 129.4 2_655 yes
O10 H10A O9 0.90 1.96 2.738(10) 143.2 6_566 yes

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT041_3                   
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: H atoms of lattice water not included in model, but are in formula.
;
_vrf_PLAT220_3                   
;
PROBLEM: Non-Solvent  Resd  O   Ueq(max)/Ueq(min) Range        3.1 Ratio   
RESPONSE: One aqua ligand appears to have disorder that could not be modelled.
;
_vrf_PLAT222_3                   
;
PROBLEM: Non-Solv.  Resd  H   Uiso(max)/Uiso(min) Range        5.8 Ratio   
RESPONSE: As for PLAT220_3.
;
_exptl_crystal_recrystallization_method 
'Crystallised at elevated temperature from synthesis'
####################################################################### 
# 
# 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_2zn
_database_code_depnum_ccdc_archive 'CCDC 1840387'
_audit_update_record             
;
2018-04-30 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_audit_creation_date             2018-01-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H16 N4 O16 Zn, 2(C2 H8 N)'
_chemical_formula_sum            'C40 H32 N6 O16 Zn'
_chemical_formula_weight         918.08
_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 0.0030 0.0020 '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 0.0070 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0120 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3120 1.4670 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.468(3)
_cell_length_b                   9.1690(18)
_cell_length_c                   25.512(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.04(3)
_cell_angle_gamma                90
_cell_volume                     3767.4(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    31341
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      .632
_shelx_estimated_absorpt_T_max   0.993
_shelx_estimated_absorpt_T_min   0.985
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1468
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31341
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.632
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_source                   'MX1 beamline Australian Synchrotron'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2826
_reflns_number_total             4324
_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       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.769
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4324
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1341
_refine_ls_R_factor_gt           0.0901
_refine_ls_restrained_S_all      1.043
_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)+(0.1543P)²+6.4826P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2220
_refine_ls_wR_factor_ref         0.2552
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C11(H11A,H11B), N3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C16(H16), C18(H18)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.500000 0.18835(10) 0.750000 0.0359(3) Uani 1 2 d S T P . .
O1 O 0.5762(2) 0.3168(4) 0.72266(16) 0.0445(9) Uani 1 1 d . . . . .
O2 O 0.6796(3) 0.3731(6) 0.6838(2) 0.0639(14) Uani 1 1 d . . . . .
O3 O 0.7313(3) 0.0453(5) 0.64414(17) 0.0523(10) Uani 1 1 d . . . . .
O4 O 0.5440(2) 0.3790(5) 0.56211(17) 0.0502(10) Uani 1 1 d . . . . .
O5 O 0.4421(2) 0.0862(5) 0.68670(15) 0.0465(10) Uani 1 1 d . . . . .
O6 O 0.3531(3) -0.0022(6) 0.73337(17) 0.0610(13) Uani 1 1 d . . . . .
O7 O 0.2959(2) 0.1266(7) 0.5644(2) 0.0689(14) Uani 1 1 d . . . . .
O8 O 0.4732(3) -0.2362(6) 0.63613(18) 0.0635(13) Uani 1 1 d . . . . .
N1 N 0.6318(2) 0.1991(5) 0.59874(16) 0.0337(9) Uani 1 1 d . . . . .
N2 N 0.3815(3) -0.0608(6) 0.59772(19) 0.0507(13) Uani 1 1 d . . . . .
C1 C 0.6165(3) 0.3015(6) 0.6859(2) 0.0378(11) Uani 1 1 d . . . . .
C2 C 0.5866(3) 0.1883(6) 0.6425(2) 0.0379(11) Uani 1 1 d . . . . .
H2A H 0.594373 0.089576 0.658475 0.045 Uiso 1 1 calc R . . . .
H2B H 0.526499 0.202492 0.627949 0.045 Uiso 1 1 calc R . . . .
C3 C 0.7061(3) 0.1201(6) 0.6046(2) 0.0366(11) Uani 1 1 d . . . . .
C4 C 0.6056(3) 0.3056(6) 0.5607(2) 0.0363(11) Uani 1 1 d . . . . .
C5 C 0.7530(3) 0.1361(6) 0.5607(2) 0.0350(11) Uani 1 1 d . . . . .
C6 C 0.6550(3) 0.3276(5) 0.5185(2) 0.0312(10) Uani 1 1 d . . . . .
C7 C 0.8231(3) 0.0525(6) 0.5614(2) 0.0389(11) Uani 1 1 d . . . . .
H7 H 0.840081 -0.017279 0.589073 0.047 Uiso 1 1 calc R . . . .
C8 C 0.7267(3) 0.2408(5) 0.52040(18) 0.0280(9) Uani 1 1 d . . . . .
C9 C 0.6310(3) 0.4293(6) 0.4786(2) 0.0378(11) Uani 1 1 d . . . . .
H9 H 0.583024 0.487259 0.478164 0.045 Uiso 1 1 calc R . . . .
C10 C 0.3794(3) 0.0096(7) 0.6918(2) 0.0493(15) Uani 1 1 d . . . . .
C11 C 0.3377(4) -0.0753(10) 0.6420(2) 0.066(2) Uani 1 1 d . . . . .
H11A H 0.335104 -0.179715 0.651402 0.079 Uiso 1 1 calc R . . . .
H11B H 0.279990 -0.039823 0.630028 0.079 Uiso 1 1 calc R . . . .
C12 C 0.4524(4) -0.1470(7) 0.6004(2) 0.0471(15) Uani 1 1 d . . . . .
C13 C 0.3561(3) 0.0513(8) 0.5618(2) 0.0497(16) Uani 1 1 d . . . . .
C14 C 0.5010(3) -0.1228(7) 0.5580(2) 0.0408(12) Uani 1 1 d . . . . .
C15 C 0.4055(3) 0.0760(6) 0.5195(2) 0.0395(12) Uani 1 1 d . . . . .
C16 C 0.5702(4) -0.2072(7) 0.5569(2) 0.0491(14) Uani 1 1 d . . . . .
H16 H 0.586254 -0.281814 0.582794 0.059 Uiso 1 1 calc R . . . .
C17 C 0.4768(3) -0.0109(6) 0.52021(19) 0.0343(11) Uani 1 1 d . . . . .
C18 C 0.3833(3) 0.1824(7) 0.4826(3) 0.0481(13) Uani 1 1 d . . . . .
H18 H 0.335943 0.240906 0.483413 0.058 Uiso 1 1 calc R . . . .
N3 N 0.6927(3) 0.6438(7) 0.7394(2) 0.0573(14) Uani 1 1 d . . . . .
H3A H 0.704851 0.550793 0.731175 0.069 Uiso 1 1 calc R . . . .
H3B H 0.728978 0.668586 0.770068 0.069 Uiso 1 1 calc R . . . .
C19 C 0.7085(6) 0.7389(9) 0.6966(4) 0.087(3) Uani 1 1 d . . . . .
H19A H 0.718270 0.838639 0.710267 0.131 Uiso 1 1 calc GR . . . .
H19B H 0.660271 0.737761 0.666684 0.131 Uiso 1 1 calc GR . . . .
H19C H 0.757511 0.704061 0.684217 0.131 Uiso 1 1 calc GR . . . .
C20 C 0.6096(4) 0.6436(9) 0.7507(5) 0.090(3) Uani 1 1 d . . . . .
H20A H 0.568763 0.624959 0.717483 0.135 Uiso 1 1 calc GR . . . .
H20B H 0.598419 0.738591 0.765255 0.135 Uiso 1 1 calc GR . . . .
H20C H 0.605747 0.567043 0.776837 0.135 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.952(4) 2_656 ?
Zn1 O1 1.952(4) . ?
Zn1 O5 1.937(4) 2_656 ?
Zn1 O5 1.937(4) . ?
O1 C1 1.265(6) . ?
O2 C1 1.239(6) . ?
O3 C3 1.218(7) . ?
O4 C4 1.224(6) . ?
O5 C10 1.278(6) . ?
O6 C10 1.231(6) . ?
O7 C13 1.221(8) . ?
O8 C12 1.218(8) . ?
N1 C2 1.470(6) . ?
N1 C3 1.402(7) . ?
N1 C4 1.381(7) . ?
N2 C11 1.468(6) . ?
N2 C12 1.400(9) . ?
N2 C13 1.383(9) . ?
C1 C2 1.522(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C5 1.497(7) . ?
C4 C6 1.492(6) . ?
C5 C7 1.381(7) . ?
C5 C8 1.407(7) . ?
C6 C8 1.416(7) . ?
C6 C9 1.377(7) . ?
C7 H7 0.9500 . ?
C7 C9 1.403(7) 7_656 ?
C8 C8 1.427(8) 7_656 ?
C9 H9 0.9500 . ?
C10 C11 1.525(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C14 1.491(7) . ?
C13 C15 1.498(7) . ?
C14 C16 1.383(9) . ?
C14 C17 1.407(8) . ?
C15 C17 1.416(7) . ?
C15 C18 1.351(9) . ?
C16 H16 0.9500 . ?
C16 C18 1.406(8) 5_656 ?
C17 C17 1.421(9) 5_656 ?
C18 H18 0.9500 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 C19 1.462(10) . ?
N3 C20 1.455(9) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O1 105.8(2) . 2_656 ?
O5 Zn1 O1 103.58(16) 2_656 2_656 ?
O5 Zn1 O1 103.58(16) . . ?
O5 Zn1 O1 110.39(17) 2_656 . ?
O5 Zn1 O1 110.39(17) . 2_656 ?
O5 Zn1 O5 122.2(3) . 2_656 ?
C1 O1 Zn1 132.4(4) . . ?
C10 O5 Zn1 116.6(3) . . ?
C3 N1 C2 116.9(4) . . ?
C4 N1 C2 116.6(4) . . ?
C4 N1 C3 125.4(4) . . ?
C12 N2 C11 116.7(6) . . ?
C13 N2 C11 116.6(6) . . ?
C13 N2 C12 125.9(4) . . ?
O1 C1 C2 118.3(4) . . ?
O2 C1 O1 123.3(5) . . ?
O2 C1 C2 118.5(4) . . ?
N1 C2 C1 111.6(4) . . ?
N1 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
O3 C3 N1 121.3(4) . . ?
O3 C3 C5 122.4(5) . . ?
N1 C3 C5 116.4(5) . . ?
O4 C4 N1 120.5(4) . . ?
O4 C4 C6 121.8(5) . . ?
N1 C4 C6 117.7(4) . . ?
C7 C5 C3 119.7(5) . . ?
C7 C5 C8 121.3(4) . . ?
C8 C5 C3 119.0(4) . . ?
C8 C6 C4 118.4(5) . . ?
C9 C6 C4 120.6(4) . . ?
C9 C6 C8 121.0(4) . . ?
C5 C7 H7 120.0 . . ?
C5 C7 C9 119.9(5) . 7_656 ?
C9 C7 H7 120.0 7_656 . ?
C5 C8 C6 122.4(4) . . ?
C5 C8 C8 118.8(5) . 7_656 ?
C6 C8 C8 118.8(6) . 7_656 ?
C6 C9 C7 120.3(4) . 7_656 ?
C6 C9 H9 119.9 . . ?
C7 C9 H9 119.9 7_656 . ?
O5 C10 C11 115.4(4) . . ?
O6 C10 O5 124.9(5) . . ?
O6 C10 C11 119.6(5) . . ?
N2 C11 C10 112.7(4) . . ?
N2 C11 H11A 109.1 . . ?
N2 C11 H11B 109.1 . . ?
C10 C11 H11A 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
O8 C12 N2 121.2(5) . . ?
O8 C12 C14 122.2(6) . . ?
N2 C12 C14 116.6(5) . . ?
O7 C13 N2 121.4(5) . . ?
O7 C13 C15 121.6(7) . . ?
N2 C13 C15 117.1(5) . . ?
C16 C14 C12 120.0(6) . . ?
C16 C14 C17 120.7(5) . . ?
C17 C14 C12 119.2(5) . . ?
C17 C15 C13 118.6(6) . . ?
C18 C15 C13 120.1(5) . . ?
C18 C15 C17 121.3(5) . . ?
C14 C16 H16 120.0 . . ?
C14 C16 C18 120.0(6) . 5_656 ?
C18 C16 H16 120.0 5_656 . ?
C14 C17 C15 122.3(4) . . ?
C14 C17 C17 118.8(6) . 5_656 ?
C15 C17 C17 118.8(6) . 5_656 ?
C15 C18 C16 120.4(5) . 5_656 ?
C15 C18 H18 119.8 . . ?
C16 C18 H18 119.8 5_656 . ?
H3A N3 H3B 107.1 . . ?
C19 N3 H3A 107.8 . . ?
C19 N3 H3B 107.8 . . ?
C20 N3 H3A 107.8 . . ?
C20 N3 H3B 107.8 . . ?
C20 N3 C19 118.0(7) . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 H20A 109.5 . . ?
N3 C20 H20B 109.5 . . ?
N3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3A O2 0.91 2.02 2.844(7) 149.9 . yes
N3 H3A O6 0.91 2.48 2.994(7) 116.2 3 yes
N3 H3B O3 0.91 2.43 3.109(7) 131.7 4_656 yes

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_DIFMX02_2zn                 
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: Low quality data. No atom site in isostructural material.
;
_vrf_RINTA01_2zn                 
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: Best quality dtaa that could be obtained.
;
_vrf_PLAT020_2zn                 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.147 Report
RESPONSE: Best quality dtaa that could be obtained.
;
_vrf_PLAT084_2zn                 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.26 Report
RESPONSE: Best quality dtaa that could be obtained.
;
_vrf_PLAT094_2zn                 
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       2.76 Report
RESPONSE: Low quality data. No atom site in isostructural material.
;
_vrf_PLAT097_2zn                 
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       2.77 eA-3  
RESPONSE: Low quality data. No atom site in isostructural material.
;
_exptl_crystal_recrystallization_method 
'Crystallised at elevated temperature from synthesis'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 1840391'
_audit_update_record             
;
2018-04-30 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_audit_creation_date             2018-01-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H12 Cu N3 O12, C3 H7 N O, C2 H8 N'
_chemical_formula_sum            'C32 H27 Cu N5 O13'
_chemical_formula_weight         753.12
_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 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3410 1.2900 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0070 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0120 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                   9.864(2)
_cell_length_b                   13.216(3)
_cell_length_c                   13.312(3)
_cell_angle_alpha                113.74(3)
_cell_angle_beta                 98.29(3)
_cell_angle_gamma                92.58(3)
_cell_volume                     1561.7(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    57978
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.652
_cell_measurement_theta_min      1.694
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.985
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57978
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         31.656
_diffrn_reflns_theta_min         1.694
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7041
_reflns_number_total             8771
_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       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.810
_refine_diff_density_min         -1.495
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8771
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0684
_refine_ls_restrained_S_all      1.039
_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)+(0.1225P)²+1.7457P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1913
_refine_ls_wR_factor_ref         0.2073
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H) groups
2. Restrained distances
 N4-C30
 1.45 with sigma of 0.01
 O13-C28
 1.25 with sigma of 0.005
 N5-H5A = N5-H5B
 0.91 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C17(H17A,H17B), C20(H20A,H20B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C12(H12), C25(H25), C27(H27), C28(H28)
3.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.62324(3) 0.05255(3) 0.53632(3) 0.03530(13) Uani 1 1 d . . . . .
O1 O 0.3202(2) 0.09313(19) 0.55762(18) 0.0406(5) Uani 1 1 d . . . . .
O2 O 0.5335(2) 0.18223(18) 0.61970(18) 0.0384(5) Uani 1 1 d . . . . .
O3 O 0.4574(3) 0.4814(3) 0.6944(2) 0.0613(7) Uani 1 1 d . . . . .
O4 O 0.4379(3) 0.2401(2) 0.8563(2) 0.0511(6) Uani 1 1 d . . . . .
O5 O 1.0245(3) 0.7981(3) 1.1029(3) 0.0659(8) Uani 1 1 d . . . . .
O6 O 1.0338(3) 0.5404(3) 1.2448(3) 0.0732(10) Uani 1 1 d . . . . .
O7 O 0.9668(2) 0.8060(2) 1.3456(2) 0.0466(6) Uani 1 1 d . . . . .
O8 O 1.1800(2) 0.8692(2) 1.4363(2) 0.0476(6) Uani 1 1 d . . . . .
O9 O 0.3642(2) -0.0095(2) 0.33704(19) 0.0434(5) Uani 1 1 d . . . . .
O10 O 0.5778(3) 0.0798(2) 0.40104(19) 0.0461(5) Uani 1 1 d . . . . .
O11 O 0.3999(4) -0.0920(3) 0.0277(3) 0.0720(9) Uani 1 1 d . . . . .
O12 O 0.2649(4) 0.2073(3) 0.2945(2) 0.0701(9) Uani 1 1 d . . . . .
N1 N 0.4498(3) 0.3595(2) 0.7754(2) 0.0368(5) Uani 1 1 d . . . . .
N2 N 1.0385(3) 0.6609(3) 1.1635(3) 0.0516(8) Uani 1 1 d . . . . .
N3 N 0.3297(4) 0.0560(3) 0.1643(3) 0.0596(9) Uani 1 1 d . . . . .
C1 C 0.4058(3) 0.1775(3) 0.6149(2) 0.0360(6) Uani 1 1 d . . . . .
C2 C 0.3467(3) 0.2829(3) 0.6825(3) 0.0418(7) Uani 1 1 d . . . . .
H2A H 0.312993 0.319881 0.633705 0.050 Uiso 1 1 calc R . . . .
H2B H 0.267271 0.263361 0.711625 0.050 Uiso 1 1 calc R . . . .
C3 C 0.5044(3) 0.4554(3) 0.7687(3) 0.0438(7) Uani 1 1 d . . . . .
C4 C 0.4954(3) 0.3236(3) 0.8575(3) 0.0385(6) Uani 1 1 d . . . . .
C5 C 0.6219(3) 0.5226(3) 0.8573(3) 0.0419(7) Uani 1 1 d . . . . .
C6 C 0.6164(3) 0.3889(2) 0.9423(2) 0.0370(6) Uani 1 1 d . . . . .
C7 C 0.6792(5) 0.6192(3) 0.8572(3) 0.0570(10) Uani 1 1 d . . . . .
H7 H 0.640929 0.644280 0.802796 0.068 Uiso 1 1 calc R . . . .
C8 C 0.6772(3) 0.4852(2) 0.9379(2) 0.0356(6) Uani 1 1 d . . . . .
C9 C 0.6714(4) 0.3549(3) 1.0223(3) 0.0481(8) Uani 1 1 d . . . . .
H9 H 0.628788 0.290763 1.025682 0.058 Uiso 1 1 calc R . . . .
C10 C 0.7940(5) 0.6802(3) 0.9374(3) 0.0592(10) Uani 1 1 d . . . . .
H10 H 0.831340 0.748290 0.938591 0.071 Uiso 1 1 calc R . . . .
C11 C 0.7958(3) 0.5453(2) 1.0163(2) 0.0381(6) Uani 1 1 d . . . . .
C12 C 0.7908(4) 0.4146(3) 1.0995(3) 0.0530(9) Uani 1 1 d . . . . .
H12 H 0.828715 0.390522 1.154749 0.064 Uiso 1 1 calc R . . . .
C13 C 0.8532(3) 0.6443(3) 1.0135(3) 0.0468(8) Uani 1 1 d . . . . .
C14 C 0.8523(3) 0.5074(3) 1.0952(3) 0.0450(7) Uani 1 1 d . . . . .
C15 C 0.9777(4) 0.7078(3) 1.0964(3) 0.0523(9) Uani 1 1 d . . . . .
C16 C 0.9812(4) 0.5686(3) 1.1743(3) 0.0533(9) Uani 1 1 d . . . . .
C17 C 1.1516(3) 0.7291(3) 1.2530(3) 0.0573(10) Uani 1 1 d . . . . .
H17A H 1.208421 0.773552 1.226415 0.069 Uiso 1 1 calc R . . . .
H17B H 1.211121 0.680507 1.275087 0.069 Uiso 1 1 calc R . . . .
C18 C 1.0934(3) 0.8068(3) 1.3536(3) 0.0430(7) Uani 1 1 d . . . . .
C19 C 0.4664(4) 0.0472(3) 0.3325(3) 0.0454(7) Uani 1 1 d . . . . .
C20 C 0.4646(5) 0.0776(5) 0.2339(4) 0.0668(12) Uani 1 1 d . . . . .
H20A H 0.497592 0.157684 0.262101 0.080 Uiso 1 1 calc R . . . .
H20B H 0.529883 0.035082 0.187549 0.080 Uiso 1 1 calc R . . . .
C21 C 0.3088(5) -0.0358(4) 0.0601(4) 0.0582(10) Uani 1 1 d . . . . .
C22 C 0.2347(5) 0.1280(4) 0.2049(3) 0.0591(10) Uani 1 1 d . . . . .
C23 C 0.1677(4) -0.0590(3) -0.0063(3) 0.0523(8) Uani 1 1 d . . . . .
C24 C 0.0948(4) 0.1050(3) 0.1353(3) 0.0503(8) Uani 1 1 d . . . . .
C25 C 0.1374(5) -0.1500(3) -0.1075(3) 0.0558(9) Uani 1 1 d . . . . .
H25 H 0.206233 -0.197007 -0.134082 0.067 Uiso 1 1 calc R . . . .
C26 C 0.0666(4) 0.0117(3) 0.0329(3) 0.0480(8) Uani 1 1 d . . . . .
C27 C -0.0048(5) 0.1728(3) 0.1707(3) 0.0560(9) Uani 1 1 d . . . . .
H27 H 0.016388 0.236592 0.239594 0.067 Uiso 1 1 calc R . . . .
O13 O 0.1901(11) 0.6811(7) 0.6784(6) 0.213(4) Uani 1 1 d D . . . .
N4 N 0.2371(6) 0.5607(4) 0.5222(3) 0.0813(13) Uani 1 1 d D . . . .
C28 C 0.1921(15) 0.5806(7) 0.6124(7) 0.193(7) Uani 1 1 d D . . . .
H28 H 0.160783 0.521595 0.629888 0.232 Uiso 1 1 calc R . . . .
C29 C 0.2570(11) 0.4547(8) 0.4420(6) 0.147(4) Uani 1 1 d . . . . .
H29A H 0.235744 0.453146 0.367083 0.220 Uiso 1 1 calc GR . . . .
H29B H 0.195813 0.396942 0.446778 0.220 Uiso 1 1 calc GR . . . .
H29C H 0.353086 0.441024 0.456703 0.220 Uiso 1 1 calc GR . . . .
C30 C 0.2965(16) 0.6531(9) 0.5073(12) 0.260(11) Uani 1 1 d D . . . .
H30A H 0.395188 0.667599 0.538692 0.391 Uiso 1 1 calc GR . . . .
H30B H 0.251175 0.718946 0.545492 0.391 Uiso 1 1 calc GR . . . .
H30C H 0.283906 0.636106 0.427576 0.391 Uiso 1 1 calc GR . . . .
N5 N 0.9028(3) 1.0116(3) 1.3638(2) 0.0445(6) Uani 1 1 d D . . . .
H5A H 0.879(5) 1.070(3) 1.421(3) 0.067 Uiso 1 1 d DR . . . .
H5B H 0.920(5) 0.942(2) 1.358(4) 0.067 Uiso 1 1 d DR . . . .
C31 C 0.8127(4) 0.9876(4) 1.2569(3) 0.0508(8) Uani 1 1 d . . . . .
H31A H 0.858993 0.944247 1.195445 0.076 Uiso 1 1 calc GR . . . .
H31B H 0.792701 1.057599 1.252065 0.076 Uiso 1 1 calc GR . . . .
H31C H 0.726265 0.944835 1.251988 0.076 Uiso 1 1 calc GR . . . .
C32 C 1.0379(4) 1.0724(4) 1.3779(3) 0.0533(9) Uani 1 1 d . . . . .
H32A H 1.087797 1.027342 1.319798 0.080 Uiso 1 1 calc GR . . . .
H32B H 1.091322 1.087594 1.451399 0.080 Uiso 1 1 calc GR . . . .
H32C H 1.024412 1.142885 1.371695 0.080 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cu1 2.5907(12) 2_656 ?
Cu1 O1 1.985(2) 2_656 ?
Cu1 O2 1.960(2) . ?
Cu1 O8 2.070(2) 2_767 ?
Cu1 O9 1.974(2) 2_656 ?
Cu1 O10 1.969(2) . ?
O1 C1 1.258(3) . ?
O2 C1 1.250(3) . ?
O3 C3 1.211(4) . ?
O4 C4 1.211(4) . ?
O5 C15 1.225(5) . ?
O6 C16 1.202(5) . ?
O7 C18 1.237(4) . ?
O8 C18 1.246(4) . ?
O9 C19 1.252(4) . ?
O10 C19 1.255(4) . ?
O11 C21 1.209(6) . ?
O12 C22 1.214(5) . ?
N1 C2 1.458(4) . ?
N1 C3 1.396(4) . ?
N1 C4 1.384(4) . ?
N2 C15 1.367(6) . ?
N2 C16 1.390(6) . ?
N2 C17 1.462(4) . ?
N3 C20 1.452(5) . ?
N3 C21 1.406(6) . ?
N3 C22 1.373(6) . ?
C1 C2 1.518(4) . ?
C3 C5 1.481(4) . ?
C4 C6 1.476(4) . ?
C5 C7 1.372(5) . ?
C5 C8 1.406(5) . ?
C6 C8 1.408(4) . ?
C6 C9 1.367(5) . ?
C7 C10 1.396(5) . ?
C8 C11 1.409(4) . ?
C9 C12 1.408(5) . ?
C10 C13 1.355(6) . ?
C11 C13 1.419(5) . ?
C11 C14 1.394(5) . ?
C12 C14 1.369(6) . ?
C13 C15 1.484(4) . ?
C14 C16 1.488(4) . ?
C17 C18 1.531(5) . ?
C19 C20 1.518(5) . ?
C21 C23 1.483(6) . ?
C22 C24 1.491(6) . ?
C23 C25 1.378(5) . ?
C23 C26 1.407(6) . ?
C24 C26 1.401(5) . ?
C24 C27 1.364(6) . ?
C25 C27 1.398(6) 2 ?
C26 C26 1.414(7) 2 ?
O13 C28 1.267(5) . ?
N4 C28 1.273(11) . ?
N4 C29 1.421(8) . ?
N4 C30 1.427(8) . ?
N5 C31 1.470(5) . ?
N5 C32 1.472(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
O1 Cu1 Cu1 83.97(7) 2_656 2_656 ?
O1 Cu1 O8 91.36(10) 2_656 2_767 ?
O2 Cu1 Cu1 85.67(7) . 2_656 ?
O2 Cu1 O1 169.64(8) . 2_656 ?
O2 Cu1 O8 98.88(10) . 2_767 ?
O2 Cu1 O9 89.40(10) . 2_656 ?
O2 Cu1 O10 90.18(11) . . ?
O8 Cu1 Cu1 169.36(7) 2_767 2_656 ?
O9 Cu1 Cu1 88.52(7) 2_656 2_656 ?
O9 Cu1 O1 90.18(11) 2_656 2_656 ?
O9 Cu1 O8 101.08(11) 2_656 2_767 ?
O10 Cu1 Cu1 81.18(8) . 2_656 ?
O10 Cu1 O1 88.39(11) . 2_656 ?
O10 Cu1 O8 89.17(11) . 2_767 ?
O10 Cu1 O9 169.69(9) . 2_656 ?
C1 O1 Cu1 122.4(2) . 2_656 ?
C1 O2 Cu1 122.0(2) . . ?
C18 O8 Cu1 136.4(2) . 2_767 ?
C19 O9 Cu1 117.6(2) . 2_656 ?
C19 O10 Cu1 126.3(2) . . ?
C3 N1 C2 118.1(3) . . ?
C4 N1 C2 115.8(3) . . ?
C4 N1 C3 125.6(2) . . ?
C15 N2 C16 125.4(3) . . ?
C15 N2 C17 117.0(3) . . ?
C16 N2 C17 115.3(4) . . ?
C21 N3 C20 117.0(4) . . ?
C22 N3 C20 117.3(4) . . ?
C22 N3 C21 125.8(4) . . ?
O1 C1 C2 116.3(3) . . ?
O2 C1 O1 125.9(3) . . ?
O2 C1 C2 117.8(2) . . ?
N1 C2 C1 111.3(2) . . ?
O3 C3 N1 121.4(3) . . ?
O3 C3 C5 122.5(3) . . ?
N1 C3 C5 116.1(3) . . ?
O4 C4 N1 119.9(3) . . ?
O4 C4 C6 122.6(3) . . ?
N1 C4 C6 117.5(3) . . ?
C7 C5 C3 119.3(3) . . ?
C7 C5 C8 120.6(3) . . ?
C8 C5 C3 120.0(3) . . ?
C8 C6 C4 119.1(3) . . ?
C9 C6 C4 120.6(3) . . ?
C9 C6 C8 120.3(3) . . ?
C5 C7 C10 119.6(4) . . ?
C5 C8 C6 121.4(3) . . ?
C5 C8 C11 119.4(3) . . ?
C6 C8 C11 119.2(3) . . ?
C6 C9 C12 120.3(3) . . ?
C13 C10 C7 121.3(4) . . ?
C8 C11 C13 118.6(3) . . ?
C14 C11 C8 119.6(3) . . ?
C14 C11 C13 121.8(3) . . ?
C14 C12 C9 120.1(3) . . ?
C10 C13 C11 120.3(3) . . ?
C10 C13 C15 121.1(3) . . ?
C11 C13 C15 118.6(3) . . ?
C11 C14 C16 119.2(3) . . ?
C12 C14 C11 120.5(3) . . ?
C12 C14 C16 120.3(3) . . ?
O5 C15 N2 121.7(3) . . ?
O5 C15 C13 120.9(4) . . ?
N2 C15 C13 117.4(3) . . ?
O6 C16 N2 121.1(3) . . ?
O6 C16 C14 122.1(4) . . ?
N2 C16 C14 116.8(3) . . ?
N2 C17 C18 109.8(3) . . ?
O7 C18 O8 125.5(3) . . ?
O7 C18 C17 118.4(3) . . ?
O8 C18 C17 116.1(3) . . ?
O9 C19 O10 126.4(3) . . ?
O9 C19 C20 119.7(3) . . ?
O10 C19 C20 113.9(3) . . ?
N3 C20 C19 114.0(4) . . ?
O11 C21 N3 121.9(4) . . ?
O11 C21 C23 122.6(4) . . ?
N3 C21 C23 115.5(4) . . ?
O12 C22 N3 120.6(4) . . ?
O12 C22 C24 121.7(5) . . ?
N3 C22 C24 117.7(3) . . ?
C25 C23 C21 119.0(4) . . ?
C25 C23 C26 120.4(4) . . ?
C26 C23 C21 120.6(4) . . ?
C26 C24 C22 118.8(4) . . ?
C27 C24 C22 120.9(4) . . ?
C27 C24 C26 120.3(4) . . ?
C23 C25 C27 119.6(4) . 2 ?
C23 C26 C26 119.3(4) . 2 ?
C24 C26 C23 121.6(4) . . ?
C24 C26 C26 119.2(5) . 2 ?
C24 C27 C25 121.2(4) . 2 ?
C28 N4 C29 126.7(7) . . ?
C28 N4 C30 117.6(9) . . ?
C29 N4 C30 114.7(9) . . ?
O13 C28 N4 118.3(9) . . ?
C31 N5 C32 113.8(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N5 H5A O8 0.911(10) 1.93(3) 2.756(4) 150(4) 2_778 yes
N5 H5B O7 0.914(10) 1.829(12) 2.741(4) 176(5) . yes

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Crystallised at elevated temperature from synthesis'
