# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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. 
# 
#######################################################################

data_1_sq
_database_code_depnum_ccdc_archive 'CCDC 1848123'
_audit_update_record             
;
2018-09-04 deposited with the CCDC.
2018-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H62 Cu2 N8 O15'
_chemical_formula_weight         1310.32

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   16.1213(6)
_cell_length_b                   8.9632(3)
_cell_length_c                   25.9147(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.817(3)
_cell_angle_gamma                90
_cell_volume                     3718.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13241
_cell_measurement_theta_min      5.1700
_cell_measurement_theta_max      72.2970

_exptl_crystal_description       plate-like
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_F_000             1360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    1.220
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.59609
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '?Ø scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42347
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         4.145
_diffrn_reflns_theta_max         75.065
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.738
_diffrn_reflns_point_group_measured_fraction_full 0.772
_reflns_number_total             11320
_reflns_number_gt                8859
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.425
_reflns_Friedel_fraction_max     0.472
_reflns_Friedel_fraction_full    0.511

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1097P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2334 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(3)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         11320
_refine_ls_number_parameters     808
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.1718
_refine_ls_wR_factor_gt          0.1623
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.25678(6) 0.50100(11) 0.47595(3) 0.0535(3) Uani 1 1 d . . . . .
Cu2 Cu 0.26828(5) 0.22149(10) 0.98017(3) 0.0431(2) Uani 1 1 d . . . . .
C1 C 0.3771(4) 0.7023(11) 0.4890(3) 0.0684(19) Uani 1 1 d . . . . .
C2 C 0.4631(5) 0.7756(11) 0.4969(4) 0.088(3) Uani 1 1 d . . . . .
H2A H 0.4557 0.8814 0.5048 0.105 Uiso 1 1 calc R U . . .
C3 C 0.5064(6) 0.7653(12) 0.4495(4) 0.095(3) Uani 1 1 d . . . . .
H3A H 0.4724 0.8109 0.4208 0.142 Uiso 1 1 calc R U . . .
H3B H 0.5591 0.8160 0.4554 0.142 Uiso 1 1 calc R U . . .
H3C H 0.5155 0.6623 0.4417 0.142 Uiso 1 1 calc R U . . .
C4 C 0.4898(5) 0.7168(12) 0.5878(4) 0.084(2) Uani 1 1 d . . . . .
C5 C 0.5388(5) 0.6323(10) 0.6334(3) 0.072(2) Uani 1 1 d . . . . .
C6 C 0.5034(6) 0.6220(12) 0.6788(4) 0.092(3) Uani 1 1 d . . . . .
H6A H 0.4511 0.6635 0.6813 0.110 Uiso 1 1 calc R U . . .
C7 C 0.5462(6) 0.5495(13) 0.7207(3) 0.096(3) Uani 1 1 d . . . . .
H7A H 0.5241 0.5471 0.7523 0.115 Uiso 1 1 calc R U . . .
C8 C 0.6204(4) 0.4814(11) 0.7163(3) 0.074(2) Uani 1 1 d . . . . .
C9 C 0.6550(5) 0.4919(13) 0.6716(3) 0.085(3) Uani 1 1 d . . . . .
H9A H 0.7057 0.4457 0.6680 0.102 Uiso 1 1 calc R U . . .
C10 C 0.6136(5) 0.5726(12) 0.6314(3) 0.087(3) Uani 1 1 d . . . . .
H10A H 0.6392 0.5860 0.6015 0.104 Uiso 1 1 calc R U . . .
C11 C 0.6294(4) 0.3368(10) 0.7936(3) 0.068(2) Uani 1 1 d . . . . .
C12 C 0.5632(4) 0.2433(12) 0.7806(3) 0.080(2) Uani 1 1 d . . . . .
H12A H 0.5399 0.2340 0.7462 0.096 Uiso 1 1 calc R U . . .
C13 C 0.5314(4) 0.1631(10) 0.8190(3) 0.071(2) Uani 1 1 d . . . . .
H13A H 0.4850 0.1028 0.8100 0.085 Uiso 1 1 calc R U . . .
C14 C 0.5660(4) 0.1685(8) 0.8707(2) 0.0574(16) Uani 1 1 d . . . . .
C15 C 0.6365(4) 0.2598(9) 0.8828(2) 0.0633(19) Uani 1 1 d . . . . .
H15A H 0.6618 0.2647 0.9170 0.076 Uiso 1 1 calc R U . . .
C16 C 0.6688(5) 0.3424(11) 0.8449(3) 0.074(2) Uani 1 1 d . . . . .
H16A H 0.7161 0.4010 0.8533 0.088 Uiso 1 1 calc R U . . .
C17 C 0.5300(4) 0.0766(8) 0.9107(3) 0.0564(16) Uani 1 1 d . . . . .
C18 C 0.5163(4) 0.0299(8) 1.0003(3) 0.0552(15) Uani 1 1 d . . . . .
H18A H 0.5328 -0.0745 0.9966 0.066 Uiso 1 1 calc R U . . .
C19 C 0.5545(5) 0.0894(11) 1.0540(3) 0.083(3) Uani 1 1 d . . . . .
H19A H 0.5342 0.0314 1.0810 0.125 Uiso 1 1 calc R U . . .
H19B H 0.6143 0.0819 1.0568 0.125 Uiso 1 1 calc R U . . .
H19C H 0.5389 0.1919 1.0575 0.125 Uiso 1 1 calc R U . . .
C20 C 0.4203(4) 0.0397(8) 0.9976(2) 0.0475(14) Uani 1 1 d . . . . .
C21 C 0.1455(4) 0.4338(8) 0.9920(2) 0.0517(15) Uani 1 1 d . . . . .
C22 C 0.0551(4) 0.4915(9) 0.9866(2) 0.0586(16) Uani 1 1 d . . . . .
H22A H 0.0563 0.6001 0.9912 0.070 Uiso 1 1 calc R U . . .
C23 C 0.0122(5) 0.4223(17) 1.0304(3) 0.116(5) Uani 1 1 d . . . . .
H23A H 0.0435 0.4457 1.0633 0.174 Uiso 1 1 calc R U . . .
H23B H -0.0433 0.4618 1.0295 0.174 Uiso 1 1 calc R U . . .
H23C H 0.0095 0.3160 1.0260 0.174 Uiso 1 1 calc R U . . .
C24 C 0.0319(4) 0.5237(8) 0.8935(3) 0.0565(16) Uani 1 1 d . . . . .
C25 C -0.0159(4) 0.4833(8) 0.8416(2) 0.0546(15) Uani 1 1 d . . . . .
C26 C 0.0161(5) 0.5405(10) 0.7988(3) 0.070(2) Uani 1 1 d . . . . .
H26A H 0.0649 0.5970 0.8029 0.084 Uiso 1 1 calc R U . . .
C27 C -0.0245(5) 0.5138(13) 0.7495(3) 0.088(3) Uani 1 1 d . . . . .
H27A H -0.0044 0.5559 0.7206 0.106 Uiso 1 1 calc R U . . .
C28 C -0.0939(4) 0.4255(10) 0.7434(2) 0.069(2) Uani 1 1 d . . . . .
C29 C -0.1269(4) 0.3686(9) 0.7856(3) 0.0659(19) Uani 1 1 d . . . . .
H29A H -0.1758 0.3128 0.7813 0.079 Uiso 1 1 calc R U . . .
C30 C -0.0859(4) 0.3960(8) 0.8349(2) 0.0549(15) Uani 1 1 d . . . . .
H30A H -0.1063 0.3543 0.8637 0.066 Uiso 1 1 calc R U . . .
C31 C -0.0973(4) 0.3564(10) 0.6537(2) 0.0642(19) Uani 1 1 d . . . . .
C32 C -0.0235(4) 0.2797(11) 0.6617(3) 0.076(2) Uani 1 1 d . . . . .
H32A H 0.0030 0.2652 0.6952 0.091 Uiso 1 1 calc R U . . .
C33 C 0.0108(4) 0.2247(10) 0.6199(2) 0.0649(17) Uani 1 1 d . . . . .
H33A H 0.0602 0.1703 0.6251 0.078 Uiso 1 1 calc R U . . .
C34 C -0.0275(4) 0.2492(7) 0.5691(3) 0.0524(15) Uani 1 1 d . . . . .
C35 C -0.1032(5) 0.3241(8) 0.5625(2) 0.0589(17) Uani 1 1 d . . . . .
H35A H -0.1304 0.3394 0.5292 0.071 Uiso 1 1 calc R U . . .
C36 C -0.1384(4) 0.3762(9) 0.6052(2) 0.0600(17) Uani 1 1 d . . . . .
H36A H -0.1898 0.4245 0.6009 0.072 Uiso 1 1 calc R U . . .
C37 C 0.0161(4) 0.1930(9) 0.5260(3) 0.0613(19) Uani 1 1 d . . . . .
C38 C 0.0490(4) 0.2315(9) 0.4369(2) 0.0600(16) Uani 1 1 d . . . . .
H38A H 0.0519 0.1224 0.4350 0.072 Uiso 1 1 calc R U . . .
C39 C 0.0058(6) 0.2864(11) 0.3875(3) 0.083(3) Uani 1 1 d . . . . .
H39A H 0.0374 0.2600 0.3597 0.125 Uiso 1 1 calc R U . . .
H39B H -0.0487 0.2422 0.3815 0.125 Uiso 1 1 calc R U . . .
H39C H 0.0005 0.3929 0.3890 0.125 Uiso 1 1 calc R U . . .
C40 C 0.1368(5) 0.2907(9) 0.4477(3) 0.0630(18) Uani 1 1 d . . . . .
C41 C 0.3362(5) 0.4831(12) 0.3796(3) 0.076(2) Uani 1 1 d . . . . .
H41A H 0.3852 0.4757 0.4024 0.091 Uiso 1 1 calc R U . . .
C42 C 0.3404(6) 0.4694(13) 0.3268(3) 0.090(3) Uani 1 1 d . . . . .
H42A H 0.3914 0.4497 0.3147 0.108 Uiso 1 1 calc R U . . .
C43 C 0.2686(5) 0.4852(10) 0.2916(2) 0.0673(19) Uani 1 1 d . . . . .
C44 C 0.1983(5) 0.5142(10) 0.3121(3) 0.074(2) Uani 1 1 d . . . . .
H44A H 0.1489 0.5275 0.2900 0.088 Uiso 1 1 calc R U . . .
C45 C 0.1967(4) 0.5251(10) 0.3645(2) 0.0643(19) Uani 1 1 d . . . . .
H45A H 0.1462 0.5464 0.3769 0.077 Uiso 1 1 calc R U . . .
C46 C 0.2744(6) 0.4576(11) 0.2347(3) 0.085(3) Uani 1 1 d . . . . .
H46A H 0.2318 0.5151 0.2139 0.102 Uiso 1 1 calc R U . . .
H46B H 0.3285 0.4908 0.2263 0.102 Uiso 1 1 calc R U . . .
C47 C 0.2636(6) 0.2985(11) 0.2217(3) 0.080(2) Uani 1 1 d . . . . .
H47A H 0.2108 0.2650 0.2320 0.095 Uiso 1 1 calc R U . . .
H47B H 0.3077 0.2424 0.2418 0.095 Uiso 1 1 calc R U . . .
C48 C 0.2651(5) 0.2624(8) 0.1632(2) 0.0592(18) Uani 1 1 d . . . . .
C49 C 0.3366(4) 0.2862(10) 0.1409(2) 0.067(2) Uani 1 1 d . . . . .
H49A H 0.3845 0.3184 0.1614 0.080 Uiso 1 1 calc R U . . .
C50 C 0.3387(4) 0.2634(9) 0.0888(2) 0.063(2) Uani 1 1 d . . . . .
H50A H 0.3879 0.2803 0.0743 0.076 Uiso 1 1 calc R U . . .
C51 C 0.2013(4) 0.1921(8) 0.0810(2) 0.0545(16) Uani 1 1 d . . . . .
H51A H 0.1538 0.1583 0.0605 0.065 Uiso 1 1 calc R U . . .
C52 C 0.1974(4) 0.2143(9) 0.1325(2) 0.0600(16) Uani 1 1 d . . . . .
H52A H 0.1478 0.1963 0.1466 0.072 Uiso 1 1 calc R U . . .
C53 C 0.2471(7) 0.6149(10) 0.5828(3) 0.115(3) Uani 1 1 d D U . . .
H53A H 0.2500 0.7100 0.5688 0.138 Uiso 1 1 calc R U . . .
C54 C 0.2396(8) 0.5948(11) 0.6357(3) 0.130(4) Uani 1 1 d D U . . .
H54A H 0.2380 0.6792 0.6565 0.156 Uiso 1 1 calc R U . . .
C55 C 0.2344(6) 0.4548(9) 0.6590(3) 0.083(2) Uani 1 1 d D U . . .
C56 C 0.2380(8) 0.3308(11) 0.6268(3) 0.118(3) Uani 1 1 d D U . . .
H56A H 0.2341 0.2354 0.6404 0.141 Uiso 1 1 calc R U . . .
C57 C 0.2476(7) 0.3489(10) 0.5741(3) 0.103(3) Uani 1 1 d D U . . .
H57A H 0.2524 0.2648 0.5537 0.124 Uiso 1 1 calc R U . . .
C58 C 0.2281(6) 0.4346(15) 0.7151(3) 0.101(4) Uani 1 1 d . . . . .
H58A H 0.2101 0.5283 0.7288 0.121 Uiso 1 1 calc R U . . .
H58B H 0.1849 0.3614 0.7188 0.121 Uiso 1 1 calc R U . . .
C59 C 0.3038(5) 0.3876(13) 0.7468(3) 0.086(3) Uani 1 1 d . . . . .
H59A H 0.3441 0.4681 0.7478 0.103 Uiso 1 1 calc R U . . .
H59B H 0.3270 0.3032 0.7299 0.103 Uiso 1 1 calc R U . . .
C60 C 0.2935(5) 0.3435(11) 0.8025(2) 0.072(2) Uani 1 1 d . . . . .
C61 C 0.2665(5) 0.4458(10) 0.8367(3) 0.0683(19) Uani 1 1 d . . . . .
H61A H 0.2544 0.5428 0.8254 0.082 Uiso 1 1 calc R U . . .
C62 C 0.2575(4) 0.4082(9) 0.8856(2) 0.0607(17) Uani 1 1 d . . . . .
H62A H 0.2371 0.4792 0.9070 0.073 Uiso 1 1 calc R U . . .
C63 C 0.3058(5) 0.1744(9) 0.8731(3) 0.0633(19) Uani 1 1 d . . . . .
H63A H 0.3209 0.0797 0.8855 0.076 Uiso 1 1 calc R U . . .
C64 C 0.3146(5) 0.2074(12) 0.8220(2) 0.073(2) Uani 1 1 d . . . . .
H64A H 0.3352 0.1355 0.8009 0.088 Uiso 1 1 calc R U . . .
N1 N 0.5139(4) 0.7060(9) 0.5421(2) 0.0754(18) Uani 1 1 d . . . . .
H1A H 0.5591 0.6588 0.5379 0.090 Uiso 1 1 calc R U . . .
N2 N 0.5477(3) 0.1186(7) 0.9601(2) 0.0551(13) Uani 1 1 d . . . . .
H2B H 0.5772 0.1970 0.9680 0.066 Uiso 1 1 calc R U . . .
N3 N 0.0085(3) 0.4573(7) 0.9366(2) 0.0583(15) Uani 1 1 d . . . . .
H3D H -0.0329 0.3963 0.9343 0.070 Uiso 1 1 calc R U . . .
N4 N 0.0010(4) 0.2713(8) 0.4804(2) 0.0654(16) Uani 1 1 d . . . . .
H4A H -0.0354 0.3418 0.4771 0.079 Uiso 1 1 calc R U . . .
N5 N 0.2646(3) 0.5065(8) 0.39875(17) 0.0539(13) Uani 1 1 d . . . . .
N6 N 0.2703(3) 0.2168(7) 0.05871(16) 0.0469(10) Uani 1 1 d . . . . .
N7 N 0.2499(4) 0.4894(8) 0.55183(19) 0.0698(16) Uani 1 1 d D U . . .
N8 N 0.2768(3) 0.2707(6) 0.90531(17) 0.0480(13) Uani 1 1 d . . . . .
O1 O 0.3122(4) 0.7848(7) 0.4777(2) 0.0913(18) Uani 1 1 d . . . . .
O2 O 0.3719(3) 0.5636(6) 0.49119(18) 0.0646(13) Uani 1 1 d . . . . .
O3 O 0.4272(5) 0.7908(10) 0.5969(3) 0.121(3) Uani 1 1 d . . . . .
O4 O 0.6679(3) 0.4175(9) 0.7581(2) 0.094(2) Uani 1 1 d . . . . .
O5 O 0.4867(3) -0.0320(6) 0.8973(2) 0.0706(13) Uani 1 1 d . . . . .
O6 O 0.3831(3) -0.0775(6) 1.0089(2) 0.0725(14) Uani 1 1 d . . . . .
O7 O 0.3868(2) 0.1637(5) 0.98521(14) 0.0471(10) Uani 1 1 d . . . . .
O8 O 0.2006(3) 0.5133(6) 1.0149(2) 0.0690(13) Uani 1 1 d . . . . .
O9 O 0.1558(3) 0.3072(6) 0.97241(15) 0.0528(10) Uani 1 1 d . . . . .
O10 O 0.0912(3) 0.6053(7) 0.8967(2) 0.0771(15) Uani 1 1 d . . . . .
O11 O -0.1404(3) 0.4033(9) 0.69446(17) 0.090(2) Uani 1 1 d . . . . .
O12 O 0.0630(3) 0.0825(6) 0.5306(2) 0.0684(13) Uani 1 1 d . . . . .
O13 O 0.1976(4) 0.2193(8) 0.4389(3) 0.105(2) Uani 1 1 d . . . . .
O14 O 0.1434(3) 0.4263(7) 0.46388(17) 0.0640(13) Uani 1 1 d . . . . .
O15 O 0.2217(3) -0.0289(6) 0.9751(2) 0.0621(12) Uani 1 1 d D . . . .
H15B H 0.237(4) 0.061(2) 0.980(3) 0.093 Uiso 1 1 d D U . . .
H15C H 0.265(3) -0.080(6) 0.984(3) 0.093 Uiso 1 1 d D U . . .


_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 O2 1.935(5) . ?
Cu1 O14 1.937(5) . ?
Cu1 N7 1.986(5) . ?
Cu1 N5 2.020(5) . ?
Cu2 O9 1.958(4) . ?
Cu2 O7 1.969(4) . ?
Cu2 N8 2.010(5) . ?
Cu2 N6 2.033(4) 1_556 ?
Cu2 O15 2.365(5) . ?
Cu2 H15B 1.523(18) . ?
C1 O2 1.248(10) . ?
C1 O1 1.287(9) . ?
C1 C2 1.526(11) . ?
C2 C3 1.486(13) . ?
C2 N1 1.483(9) . ?
C2 H2A 0.9800 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 O3 1.252(11) . ?
C4 N1 1.294(11) . ?
C4 C5 1.542(11) . ?
C5 C10 1.325(11) . ?
C5 C6 1.371(12) . ?
C6 C7 1.378(12) . ?
C6 H6A 0.9300 . ?
C7 C8 1.361(12) . ?
C7 H7A 0.9300 . ?
C8 C9 1.348(10) . ?
C8 O4 1.374(8) . ?
C9 C10 1.374(11) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 O4 1.373(9) . ?
C11 C12 1.368(11) . ?
C11 C16 1.406(10) . ?
C12 C13 1.374(11) . ?
C12 H12A 0.9300 . ?
C13 C14 1.391(9) . ?
C13 H13A 0.9300 . ?
C14 C15 1.406(9) . ?
C14 C17 1.493(10) . ?
C15 C16 1.381(10) . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
C17 O5 1.223(8) . ?
C17 N2 1.333(8) . ?
C18 N2 1.449(9) . ?
C18 C20 1.542(8) . ?
C18 C19 1.548(9) . ?
C18 H18A 0.9800 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 O6 1.262(8) . ?
C20 O7 1.261(7) . ?
C21 O8 1.235(8) . ?
C21 O9 1.262(8) . ?
C21 C22 1.538(8) . ?
C22 N3 1.452(7) . ?
C22 C23 1.528(12) . ?
C22 H22A 0.9800 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 O10 1.198(8) . ?
C24 N3 1.357(9) . ?
C24 C25 1.514(8) . ?
C25 C30 1.367(9) . ?
C25 C26 1.378(10) . ?
C26 C27 1.385(10) . ?
C26 H26A 0.9300 . ?
C27 C28 1.364(12) . ?
C27 H27A 0.9300 . ?
C28 C29 1.369(10) . ?
C28 O11 1.409(7) . ?
C29 C30 1.389(8) . ?
C29 H29A 0.9300 . ?
C30 H30A 0.9300 . ?
C31 C36 1.361(9) . ?
C31 C32 1.368(10) . ?
C31 O11 1.396(8) . ?
C32 C33 1.365(10) . ?
C32 H32A 0.9300 . ?
C33 C34 1.403(8) . ?
C33 H33A 0.9300 . ?
C34 C35 1.385(9) . ?
C34 C37 1.476(9) . ?
C35 C36 1.386(9) . ?
C35 H35A 0.9300 . ?
C36 H36A 0.9300 . ?
C37 O12 1.243(9) . ?
C37 N4 1.371(9) . ?
C38 C39 1.468(10) . ?
C38 N4 1.486(8) . ?
C38 C40 1.506(10) . ?
C38 H38A 0.9800 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 O13 1.215(9) . ?
C40 O14 1.286(9) . ?
C41 N5 1.327(8) . ?
C41 C42 1.383(10) . ?
C41 H41A 0.9300 . ?
C42 C43 1.394(12) . ?
C42 H42A 0.9300 . ?
C43 C44 1.333(10) . ?
C43 C46 1.509(8) . ?
C44 C45 1.365(8) . ?
C44 H44A 0.9300 . ?
C45 N5 1.336(8) . ?
C45 H45A 0.9300 . ?
C46 C47 1.471(13) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.553(8) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 C52 1.342(9) . ?
C48 C49 1.366(10) . ?
C49 C50 1.370(8) . ?
C49 H49A 0.9300 . ?
C50 N6 1.341(7) . ?
C50 H50A 0.9300 . ?
C51 N6 1.331(7) . ?
C51 C52 1.359(8) . ?
C51 H51A 0.9300 . ?
C52 H52A 0.9300 . ?
C53 N7 1.386(6) . ?
C53 C54 1.402(6) . ?
C53 H53A 0.9300 . ?
C54 C55 1.399(6) . ?
C54 H54A 0.9300 . ?
C55 C56 1.395(6) . ?
C55 C58 1.479(10) . ?
C56 C57 1.401(6) . ?
C56 H56A 0.9300 . ?
C57 N7 1.388(6) . ?
C57 H57A 0.9300 . ?
C58 C59 1.450(11) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C59 C60 1.525(10) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 C64 1.348(13) . ?
C60 C61 1.381(11) . ?
C61 C62 1.338(9) . ?
C61 H61A 0.9300 . ?
C62 N8 1.356(9) . ?
C62 H62A 0.9300 . ?
C63 N8 1.324(8) . ?
C63 C64 1.380(9) . ?
C63 H63A 0.9300 . ?
C64 H64A 0.9300 . ?
N1 H1A 0.8600 . ?
N2 H2B 0.8600 . ?
N3 H3D 0.8600 . ?
N4 H4A 0.8600 . ?
N6 Cu2 2.032(4) 1_554 ?
O15 H15B 0.850(6) . ?
O15 H15C 0.850(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O14 175.9(2) . . ?
O2 Cu1 N7 88.7(2) . . ?
O14 Cu1 N7 88.8(2) . . ?
O2 Cu1 N5 91.4(2) . . ?
O14 Cu1 N5 91.0(2) . . ?
N7 Cu1 N5 178.3(3) . . ?
O9 Cu2 O7 171.8(2) . . ?
O9 Cu2 N8 89.06(18) . . ?
O7 Cu2 N8 86.82(18) . . ?
O9 Cu2 N6 90.88(18) . 1_556 ?
O7 Cu2 N6 91.62(17) . 1_556 ?
N8 Cu2 N6 167.5(2) . 1_556 ?
O9 Cu2 O15 94.73(19) . . ?
O7 Cu2 O15 93.06(18) . . ?
N8 Cu2 O15 102.3(2) . . ?
N6 Cu2 O15 90.1(2) 1_556 . ?
O9 Cu2 H15B 94(3) . . ?
O7 Cu2 H15B 94(3) . . ?
N8 Cu2 H15B 106(3) . . ?
N6 Cu2 H15B 87(3) 1_556 . ?
O15 Cu2 H15B 3(3) . . ?
O2 C1 O1 121.8(7) . . ?
O2 C1 C2 119.2(7) . . ?
O1 C1 C2 119.0(8) . . ?
C3 C2 N1 110.9(8) . . ?
C3 C2 C1 111.7(7) . . ?
N1 C2 C1 109.4(7) . . ?
C3 C2 H2A 108.2 . . ?
N1 C2 H2A 108.2 . . ?
C1 C2 H2A 108.2 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O3 C4 N1 123.3(8) . . ?
O3 C4 C5 117.8(9) . . ?
N1 C4 C5 118.9(8) . . ?
C10 C5 C6 118.7(8) . . ?
C10 C5 C4 123.7(8) . . ?
C6 C5 C4 117.6(8) . . ?
C5 C6 C7 119.2(9) . . ?
C5 C6 H6A 120.4 . . ?
C7 C6 H6A 120.4 . . ?
C8 C7 C6 120.6(8) . . ?
C8 C7 H7A 119.7 . . ?
C6 C7 H7A 119.7 . . ?
C7 C8 C9 119.9(7) . . ?
C7 C8 O4 122.3(7) . . ?
C9 C8 O4 117.3(7) . . ?
C8 C9 C10 118.3(8) . . ?
C8 C9 H9A 120.8 . . ?
C10 C9 H9A 120.8 . . ?
C5 C10 C9 123.1(8) . . ?
C5 C10 H10A 118.4 . . ?
C9 C10 H10A 118.4 . . ?
O4 C11 C12 124.0(7) . . ?
O4 C11 C16 115.2(7) . . ?
C12 C11 C16 120.3(7) . . ?
C11 C12 C13 119.4(7) . . ?
C11 C12 H12A 120.3 . . ?
C13 C12 H12A 120.3 . . ?
C12 C13 C14 122.6(7) . . ?
C12 C13 H13A 118.7 . . ?
C14 C13 H13A 118.7 . . ?
C13 C14 C15 117.1(6) . . ?
C13 C14 C17 120.3(7) . . ?
C15 C14 C17 122.5(6) . . ?
C16 C15 C14 121.1(6) . . ?
C16 C15 H15A 119.4 . . ?
C14 C15 H15A 119.4 . . ?
C15 C16 C11 119.2(7) . . ?
C15 C16 H16A 120.4 . . ?
C11 C16 H16A 120.4 . . ?
O5 C17 N2 123.1(7) . . ?
O5 C17 C14 119.9(6) . . ?
N2 C17 C14 117.0(6) . . ?
N2 C18 C20 111.7(5) . . ?
N2 C18 C19 108.7(6) . . ?
C20 C18 C19 108.2(6) . . ?
N2 C18 H18A 109.4 . . ?
C20 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O6 C20 O7 126.3(6) . . ?
O6 C20 C18 116.4(6) . . ?
O7 C20 C18 117.4(6) . . ?
O8 C21 O9 126.3(6) . . ?
O8 C21 C22 118.0(6) . . ?
O9 C21 C22 115.8(6) . . ?
N3 C22 C23 110.3(6) . . ?
N3 C22 C21 113.2(5) . . ?
C23 C22 C21 107.7(6) . . ?
N3 C22 H22A 108.5 . . ?
C23 C22 H22A 108.5 . . ?
C21 C22 H22A 108.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O10 C24 N3 120.6(6) . . ?
O10 C24 C25 121.6(7) . . ?
N3 C24 C25 117.7(6) . . ?
C30 C25 C26 119.6(6) . . ?
C30 C25 C24 125.1(6) . . ?
C26 C25 C24 115.3(6) . . ?
C25 C26 C27 119.8(7) . . ?
C25 C26 H26A 120.1 . . ?
C27 C26 H26A 120.1 . . ?
C28 C27 C26 119.9(7) . . ?
C28 C27 H27A 120.1 . . ?
C26 C27 H27A 120.1 . . ?
C27 C28 C29 121.0(6) . . ?
C27 C28 O11 121.8(7) . . ?
C29 C28 O11 116.7(7) . . ?
C28 C29 C30 118.8(7) . . ?
C28 C29 H29A 120.6 . . ?
C30 C29 H29A 120.6 . . ?
C25 C30 C29 120.9(7) . . ?
C25 C30 H30A 119.6 . . ?
C29 C30 H30A 119.6 . . ?
C36 C31 C32 121.7(7) . . ?
C36 C31 O11 115.3(6) . . ?
C32 C31 O11 122.6(6) . . ?
C33 C32 C31 119.2(6) . . ?
C33 C32 H32A 120.4 . . ?
C31 C32 H32A 120.4 . . ?
C32 C33 C34 120.9(7) . . ?
C32 C33 H33A 119.5 . . ?
C34 C33 H33A 119.5 . . ?
C35 C34 C33 118.3(6) . . ?
C35 C34 C37 124.3(6) . . ?
C33 C34 C37 117.4(6) . . ?
C36 C35 C34 120.2(6) . . ?
C36 C35 H35A 119.9 . . ?
C34 C35 H35A 119.9 . . ?
C31 C36 C35 119.5(7) . . ?
C31 C36 H36A 120.2 . . ?
C35 C36 H36A 120.2 . . ?
O12 C37 N4 122.3(6) . . ?
O12 C37 C34 122.6(6) . . ?
N4 C37 C34 115.1(7) . . ?
C39 C38 N4 110.2(7) . . ?
C39 C38 C40 112.5(7) . . ?
N4 C38 C40 109.6(5) . . ?
C39 C38 H38A 108.1 . . ?
N4 C38 H38A 108.1 . . ?
C40 C38 H38A 108.1 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O13 C40 O14 121.5(8) . . ?
O13 C40 C38 122.7(8) . . ?
O14 C40 C38 115.7(6) . . ?
N5 C41 C42 122.1(7) . . ?
N5 C41 H41A 119.0 . . ?
C42 C41 H41A 119.0 . . ?
C41 C42 C43 120.3(8) . . ?
C41 C42 H42A 119.9 . . ?
C43 C42 H42A 119.9 . . ?
C44 C43 C42 116.0(6) . . ?
C44 C43 C46 125.2(7) . . ?
C42 C43 C46 118.6(7) . . ?
C43 C44 C45 121.8(7) . . ?
C43 C44 H44A 119.1 . . ?
C45 C44 H44A 119.1 . . ?
N5 C45 C44 122.8(7) . . ?
N5 C45 H45A 118.6 . . ?
C44 C45 H45A 118.6 . . ?
C47 C46 C43 111.3(7) . . ?
C47 C46 H46A 109.4 . . ?
C43 C46 H46A 109.4 . . ?
C47 C46 H46B 109.4 . . ?
C43 C46 H46B 109.4 . . ?
H46A C46 H46B 108.0 . . ?
C46 C47 C48 114.2(6) . . ?
C46 C47 H47A 108.7 . . ?
C48 C47 H47A 108.7 . . ?
C46 C47 H47B 108.7 . . ?
C48 C47 H47B 108.7 . . ?
H47A C47 H47B 107.6 . . ?
C52 C48 C49 117.9(6) . . ?
C52 C48 C47 122.6(7) . . ?
C49 C48 C47 119.4(6) . . ?
C50 C49 C48 121.0(6) . . ?
C50 C49 H49A 119.5 . . ?
C48 C49 H49A 119.5 . . ?
N6 C50 C49 120.3(6) . . ?
N6 C50 H50A 119.9 . . ?
C49 C50 H50A 119.9 . . ?
N6 C51 C52 122.8(6) . . ?
N6 C51 H51A 118.6 . . ?
C52 C51 H51A 118.6 . . ?
C48 C52 C51 119.9(6) . . ?
C48 C52 H52A 120.0 . . ?
C51 C52 H52A 120.0 . . ?
N7 C53 C54 118.3(8) . . ?
N7 C53 H53A 120.8 . . ?
C54 C53 H53A 120.8 . . ?
C55 C54 C53 123.6(9) . . ?
C55 C54 H54A 118.2 . . ?
C53 C54 H54A 118.2 . . ?
C56 C55 C54 116.6(8) . . ?
C56 C55 C58 120.1(8) . . ?
C54 C55 C58 123.2(8) . . ?
C55 C56 C57 120.5(9) . . ?
C55 C56 H56A 119.7 . . ?
C57 C56 H56A 119.7 . . ?
N7 C57 C56 121.5(8) . . ?
N7 C57 H57A 119.3 . . ?
C56 C57 H57A 119.3 . . ?
C59 C58 C55 116.2(8) . . ?
C59 C58 H58A 108.2 . . ?
C55 C58 H58A 108.2 . . ?
C59 C58 H58B 108.2 . . ?
C55 C58 H58B 108.2 . . ?
H58A C58 H58B 107.4 . . ?
C58 C59 C60 115.7(7) . . ?
C58 C59 H59A 108.4 . . ?
C60 C59 H59A 108.4 . . ?
C58 C59 H59B 108.4 . . ?
C60 C59 H59B 108.4 . . ?
H59A C59 H59B 107.4 . . ?
C64 C60 C61 116.4(6) . . ?
C64 C60 C59 122.6(8) . . ?
C61 C60 C59 120.8(8) . . ?
C62 C61 C60 121.3(8) . . ?
C62 C61 H61A 119.4 . . ?
C60 C61 H61A 119.4 . . ?
C61 C62 N8 122.7(7) . . ?
C61 C62 H62A 118.7 . . ?
N8 C62 H62A 118.7 . . ?
N8 C63 C64 123.3(7) . . ?
N8 C63 H63A 118.3 . . ?
C64 C63 H63A 118.3 . . ?
C60 C64 C63 120.2(7) . . ?
C60 C64 H64A 119.9 . . ?
C63 C64 H64A 119.9 . . ?
C4 N1 C2 119.5(8) . . ?
C4 N1 H1A 120.2 . . ?
C2 N1 H1A 120.3 . . ?
C17 N2 C18 118.9(6) . . ?
C17 N2 H2B 120.6 . . ?
C18 N2 H2B 120.6 . . ?
C24 N3 C22 118.5(6) . . ?
C24 N3 H3D 120.7 . . ?
C22 N3 H3D 120.7 . . ?
C37 N4 C38 118.4(6) . . ?
C37 N4 H4A 120.8 . . ?
C38 N4 H4A 120.8 . . ?
C41 N5 C45 116.9(5) . . ?
C41 N5 Cu1 121.8(4) . . ?
C45 N5 Cu1 121.2(4) . . ?
C51 N6 C50 118.1(5) . . ?
C51 N6 Cu2 121.6(4) . 1_554 ?
C50 N6 Cu2 119.4(4) . 1_554 ?
C53 N7 C57 119.4(6) . . ?
C53 N7 Cu1 122.7(5) . . ?
C57 N7 Cu1 117.9(5) . . ?
C63 N8 C62 116.0(5) . . ?
C63 N8 Cu2 122.4(5) . . ?
C62 N8 Cu2 121.5(4) . . ?
C1 O2 Cu1 110.3(5) . . ?
C11 O4 C8 119.6(6) . . ?
C20 O7 Cu2 129.3(4) . . ?
C21 O9 Cu2 118.4(4) . . ?
C31 O11 C28 117.6(5) . . ?
C40 O14 Cu1 114.8(5) . . ?
Cu2 O15 H15B 6(6) . . ?
Cu2 O15 H15C 104(5) . . ?
H15B O15 H15C 104.1(10) . . ?

_refine_diff_density_max         0.581
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.059

_shelxl_version_number           2014-3


# SQUEEZE RESULTS (Version =  91117)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.202 -0.037 0.763 493 122 ' '
2 0.797 0.463 0.237 493 122 ' '
3 0.171 0.198 0.329 13 -1 ' '
4 0.829 0.698 0.671 13 -1 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 0 0 2.760
-1 0 1 3.073
0 0 1 1.717
1 0 1 3.420
0 0 2 3.435
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL exp_51_a.res in P2(1)
CELL   16.1213    8.9632   25.9147     90.00     96.82     90.00
SPGR P21
# Solvent Accessible Volume =      1013
# Electrons Found in S.A.V. =       243
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.846 0.287 0.948 !       8.50 eA-3
Q102 0.673 0.558 0.512 !       6.62 eA-3
C103 0.200 0.837 0.880 !       5.25 eA-3
C104 0.950 0.563 0.185 !       4.51 eA-3
C105 0.787 0.475 0.414 !       4.02 eA-3
C106 0.014 0.465 0.184 !       2.80 eA-3
C107 0.433 0.819 0.797 !       2.80 eA-3
C108 0.771 0.462 0.312 !       2.77 eA-3
C109 0.929 0.630 0.131 !       2.73 eA-3
C110 0.748 0.304 0.215 !       2.72 eA-3
C111 0.359 0.819 0.833 !       2.71 eA-3
C112 0.591 0.465 0.300 !       2.36 eA-3
C113 0.080 0.035 0.745 !       2.19 eA-3
C114 0.891 0.601 0.252 !       2.10 eA-3
C115 0.361 0.935 0.731 !       1.83 eA-3
C116 0.048 0.933 0.749 !       1.82 eA-3
C117 0.881 0.675 0.255 !       1.64 eA-3
C118 0.443 0.098 0.652 !       1.39 eA-3
C119 0.883 0.379 0.277 !       1.28 eA-3
Q120 0.345 0.024 0.594 !       1.10 eA-3
C121 0.309 0.935 0.656 !       0.94 eA-3
C122 0.721 0.383 0.183 !       0.93 eA-3
C123 0.300 0.832 0.844 !       0.92 eA-3
C124 0.298 0.900 0.669 !       0.90 eA-3
Q125 0.456 0.932 0.791 !       0.83 eA-3
Q126 0.300 0.069 0.561 !       0.82 eA-3
Q127 0.879 0.600 0.100 !       0.82 eA-3
Q128 0.751 0.971 0.448 !       0.81 eA-3
C129 0.911 0.943 0.796 !       0.81 eA-3
C130 0.375 0.063 0.631 !       0.78 eA-3
C131 0.282 0.967 0.724 !       0.78 eA-3
Q132 0.787 0.344 0.943 !       0.74 eA-3
Q133 0.185 0.928 0.075 !       0.74 eA-3
C134 0.862 0.503 0.336 !       0.71 eA-3
Q135 0.440 0.097 0.164 !       0.68 eA-3
Q136 0.058 0.590 0.170 !       0.66 eA-3
Q137 0.595 0.625 0.372 !       0.65 eA-3
Q138 0.377 0.902 0.021 !       0.64 eA-3
C139 0.720 0.409 0.227 !       0.64 eA-3
C140 0.471 0.191 0.673 !       0.63 eA-3
Q141 0.265 0.217 0.006 !       0.63 eA-3
Q142 0.210 0.460 0.725 !       0.63 eA-3
Q143 0.830 0.679 0.131 !       0.62 eA-3
Q144 0.485 0.628 0.300 !       0.62 eA-3
Q145 0.856 0.778 0.270 !       0.61 eA-3
Q146 0.890 0.403 0.320 !       0.61 eA-3
Q147 0.014 0.403 0.036 !       0.61 eA-3
Q148 0.011 0.256 0.491 !       0.61 eA-3
Q149 0.094 0.253 0.342 !       0.60 eA-3
Q150 0.050 0.258 0.725 !       0.60 eA-3
Q151 0.386 0.034 0.372 !       0.60 eA-3
Q152 0.990 0.719 0.483 !       0.60 eA-3
C153 0.911 0.439 0.146 !       0.59 eA-3
C154 0.658 0.370 0.212 !       0.59 eA-3
Q155 0.166 0.501 0.622 !       0.59 eA-3
Q156 0.348 0.498 0.328 !       0.59 eA-3
Q157 0.310 0.927 0.841 !       0.59 eA-3
Q158 0.824 1.001 0.422 !       0.58 eA-3
Q159 0.260 0.714 0.886 !       0.58 eA-3
Q160 0.470 0.034 0.273 !       0.58 eA-3
Q161 0.744 0.972 0.773 !       0.58 eA-3
Q162 0.844 0.186 0.147 !       0.58 eA-3
Q163 0.720 0.620 0.022 !       0.57 eA-3
Q164 0.231 0.784 0.699 !       0.57 eA-3
C165 0.142 0.913 0.760 !       0.57 eA-3
Q166 0.625 0.222 0.129 !       0.57 eA-3
Q167 0.715 0.723 0.112 !       0.57 eA-3
C168 0.425 0.186 0.697 !       0.57 eA-3
Q169 0.859 0.129 0.257 !       0.56 eA-3
Q170 0.733 0.151 0.187 !       0.55 eA-3
Q171 0.392 0.247 0.666 !       0.54 eA-3
Q172 0.096 0.931 0.643 !       0.54 eA-3
C173 0.451 0.278 0.667 !       0.53 eA-3
Q174 0.750 0.984 0.502 !       0.53 eA-3
Q175 0.302 0.653 0.848 !       0.53 eA-3
Q176 0.173 0.724 0.135 !       0.53 eA-3
Q177 0.012 0.937 0.059 !       0.53 eA-3
Q178 0.046 0.967 0.976 !       0.52 eA-3
Q179 0.063 0.560 0.075 !       0.52 eA-3
Q180 0.217 0.940 0.982 !       0.52 eA-3
Q181 0.829 0.740 0.279 !       0.52 eA-3
Q182 0.124 0.437 0.106 !       0.52 eA-3
C183 0.673 0.319 0.247 !       0.51 eA-3
C184 0.660 0.239 0.207 !       0.51 eA-3
Q185 0.266 0.494 0.396 !       0.50 eA-3
Q186 0.349 0.595 0.744 !       0.50 eA-3
C187 0.157 0.595 0.134 !       0.50 eA-3
Q188 0.388 0.681 0.744 !       0.50 eA-3
;

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1848124'
_audit_update_record             
;
2018-09-04 deposited with the CCDC.
2018-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H22 Mn N2 O9'
_chemical_formula_weight         489.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.5725(5)
_cell_length_b                   10.1493(7)
_cell_length_c                   31.853(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2124.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9962
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      27.27

_exptl_crystal_description       plate-like
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_F_000             1012
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.677
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29548
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.106
_diffrn_reflns_theta_max         28.545
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5341
_reflns_number_gt                4796
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.726
_reflns_Friedel_fraction_max     0.977
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0439P)²+0.1824P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1896 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(6)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         5341
_refine_ls_number_parameters     305
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0747
_refine_ls_wR_factor_gt          0.0718
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Mn1 Mn 0.15614(5) 0.25975(4) 0.99272(2) 0.02304(10) Uani 1 1 d . . . . .
N1 N -0.2428(3) 0.5877(2) 1.10794(6) 0.0278(4) Uani 1 1 d . . . . .
H1A H -0.2827 0.5531 1.1312 0.033 Uiso 1 1 calc R U . . .
N2 N -1.4005(3) 0.7330(2) 1.34448(6) 0.0306(5) Uani 1 1 d . . . . .
H2A H -1.3037 0.6819 1.3364 0.037 Uiso 1 1 calc R U . . .
O1 O 0.0736(3) 0.41531(19) 1.03310(6) 0.0327(4) Uani 1 1 d . . . . .
O2 O -0.2555(3) 0.38932(19) 1.04923(6) 0.0322(4) Uani 1 1 d . . . . .
O3 O -0.3161(3) 0.7261(2) 1.05490(5) 0.0371(4) Uani 1 1 d . . . . .
O4 O -0.9737(3) 0.9495(2) 1.17770(6) 0.0435(5) Uani 1 1 d . . . . .
O5 O -1.6070(3) 0.9015(2) 1.32611(6) 0.0475(6) Uani 1 1 d . . . . .
O6 O -1.1512(3) 0.66594(17) 1.40594(5) 0.0300(4) Uani 1 1 d . . . . .
O7 O -1.3806(2) 0.69757(18) 1.45641(5) 0.0276(4) Uani 1 1 d . . . . .
O8 O 0.4289(3) 0.37210(19) 0.97365(5) 0.0266(4) Uani 1 1 d D . . . .
O9 O 0.4804(4) 0.6252(2) 0.98486(7) 0.0521(6) Uani 1 1 d D . . . .
C1 C -0.0843(4) 0.4407(2) 1.05403(7) 0.0245(5) Uani 1 1 d . . . . .
C2 C -0.0537(4) 0.5419(2) 1.08893(8) 0.0264(5) Uani 1 1 d . . . . .
H2B H 0.0149 0.6186 1.0767 0.032 Uiso 1 1 calc R U . . .
C3 C 0.0835(5) 0.4865(3) 1.12297(9) 0.0397(7) Uani 1 1 d . . . . .
H3A H 0.2083 0.4562 1.1106 0.060 Uiso 1 1 calc R U . . .
H3B H 0.1127 0.5539 1.1432 0.060 Uiso 1 1 calc R U . . .
H3C H 0.0164 0.4141 1.1366 0.060 Uiso 1 1 calc R U . . .
C4 C -0.3550(4) 0.6816(2) 1.09025(7) 0.0256(5) Uani 1 1 d . . . . .
C5 C -0.5262(3) 0.7385(3) 1.11505(7) 0.0254(5) Uani 1 1 d . . . . .
C6 C -0.6869(4) 0.7973(2) 1.09378(8) 0.0289(5) Uani 1 1 d . . . . .
H6A H -0.6909 0.7942 1.0646 0.035 Uiso 1 1 calc R U . . .
C7 C -0.5203(4) 0.7456(3) 1.15872(7) 0.0294(5) Uani 1 1 d . . . . .
H7A H -0.4152 0.7048 1.1733 0.035 Uiso 1 1 calc R U . . .
C8 C -0.8406(4) 0.8602(2) 1.11544(7) 0.0306(5) Uani 1 1 d . . . . .
H8A H -0.9510 0.8958 1.1011 0.037 Uiso 1 1 calc R U . . .
C9 C -0.6699(4) 0.8132(3) 1.18054(8) 0.0333(5) Uani 1 1 d . . . . .
H9A H -0.6631 0.8204 1.2096 0.040 Uiso 1 1 calc R U . . .
C10 C -0.8284(4) 0.8695(2) 1.15884(8) 0.0306(5) Uani 1 1 d . . . . .
C11 C -1.0852(4) 0.9093(3) 1.21186(8) 0.0308(6) Uani 1 1 d . . . . .
C12 C -1.0864(4) 0.7832(3) 1.22819(8) 0.0348(6) Uani 1 1 d . . . . .
H12A H -1.0069 0.7174 1.2162 0.042 Uiso 1 1 calc R U . . .
C13 C -1.2084(4) 1.0066(3) 1.22891(8) 0.0343(6) Uani 1 1 d . . . . .
H13A H -1.2084 1.0911 1.2176 0.041 Uiso 1 1 calc R U . . .
C14 C -1.2081(4) 0.7560(3) 1.26276(8) 0.0329(5) Uani 1 1 d . . . . .
H14A H -1.2082 0.6716 1.2741 0.039 Uiso 1 1 calc R U . . .
C15 C -1.3309(4) 0.9769(3) 1.26286(8) 0.0332(6) Uani 1 1 d . . . . .
H15A H -1.4156 1.0416 1.2739 0.040 Uiso 1 1 calc R U . . .
C16 C -1.3294(4) 0.8525(3) 1.28066(7) 0.0289(5) Uani 1 1 d . . . . .
C17 C -1.4581(4) 0.8308(3) 1.31907(8) 0.0313(6) Uani 1 1 d . . . . .
C18 C -1.4943(4) 0.7091(3) 1.38526(7) 0.0267(5) Uani 1 1 d . . . . .
H18A H -1.5739 0.7870 1.3931 0.032 Uiso 1 1 calc R U . . .
C19 C -1.6363(4) 0.5907(3) 1.38384(8) 0.0396(6) Uani 1 1 d . . . . .
H19A H -1.6956 0.5774 1.4110 0.059 Uiso 1 1 calc R U . . .
H19B H -1.7420 0.6063 1.3637 0.059 Uiso 1 1 calc R U . . .
H19C H -1.5607 0.5137 1.3759 0.059 Uiso 1 1 calc R U . . .
C20 C -1.3268(4) 0.6896(2) 1.41783(7) 0.0231(4) Uani 1 1 d . . . . .
H8C H 0.480(6) 0.364(3) 0.9496(8) 0.056(11) Uiso 1 1 d D . . . .
H8B H 0.439(6) 0.446(2) 0.9809(10) 0.052(11) Uiso 1 1 d D . . . .
H9C H 0.377(5) 0.673(3) 0.9793(11) 0.069(13) Uiso 1 1 d D . . . .
H9B H 0.513(5) 0.649(3) 1.0088(7) 0.049(10) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O2 2.1005(18) 4_557 ?
Mn1 O1 2.1076(19) . ?
Mn1 O7 2.1917(16) 2_364 ?
Mn1 O8 2.2096(18) . ?
Mn1 O8 2.2737(19) 4_457 ?
Mn1 O7 2.2806(16) 3_447 ?
N1 C4 1.330(3) . ?
N1 C2 1.458(3) . ?
N1 H1A 0.8600 . ?
N2 C17 1.336(3) . ?
N2 C18 1.458(3) . ?
N2 H2A 0.8600 . ?
O1 C1 1.260(3) . ?
O2 C1 1.249(3) . ?
O2 Mn1 2.1004(18) 4_457 ?
O3 C4 1.240(3) . ?
O4 C11 1.374(3) . ?
O4 C10 1.390(3) . ?
O5 C17 1.234(3) . ?
O6 C20 1.238(3) . ?
O7 C20 1.281(3) . ?
O7 Mn1 2.1917(16) 2_365 ?
O7 Mn1 2.2807(16) 3_457 ?
O8 Mn1 2.2737(19) 4_557 ?
O8 H8C 0.84(2) . ?
O8 H8B 0.79(2) . ?
O9 H9C 0.85(2) . ?
O9 H9B 0.83(2) . ?
C1 C2 1.527(3) . ?
C2 C3 1.519(4) . ?
C2 H2B 0.9800 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 C5 1.491(3) . ?
C5 C6 1.390(3) . ?
C5 C7 1.393(3) . ?
C6 C8 1.380(4) . ?
C6 H6A 0.9300 . ?
C7 C9 1.386(4) . ?
C7 H7A 0.9300 . ?
C8 C10 1.388(3) . ?
C8 H8A 0.9300 . ?
C9 C10 1.375(4) . ?
C9 H9A 0.9300 . ?
C11 C12 1.382(4) . ?
C11 C13 1.388(4) . ?
C12 C14 1.389(4) . ?
C12 H12A 0.9300 . ?
C13 C15 1.382(4) . ?
C13 H13A 0.9300 . ?
C14 C16 1.385(4) . ?
C14 H14A 0.9300 . ?
C15 C16 1.385(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.504(3) . ?
C18 C19 1.522(4) . ?
C18 C20 1.526(3) . ?
C18 H18A 0.9800 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mn1 O1 177.53(8) 4_557 . ?
O2 Mn1 O7 92.02(7) 4_557 2_364 ?
O1 Mn1 O7 87.79(7) . 2_364 ?
O2 Mn1 O8 88.42(7) 4_557 . ?
O1 Mn1 O8 89.43(7) . . ?
O7 Mn1 O8 115.04(7) 2_364 . ?
O2 Mn1 O8 93.30(7) 4_557 4_457 ?
O1 Mn1 O8 89.09(7) . 4_457 ?
O7 Mn1 O8 79.76(6) 2_364 4_457 ?
O8 Mn1 O8 165.06(6) . 4_457 ?
O2 Mn1 O7 94.23(7) 4_557 3_447 ?
O1 Mn1 O7 86.57(7) . 3_447 ?
O7 Mn1 O7 164.60(6) 2_364 3_447 ?
O8 Mn1 O7 79.23(6) . 3_447 ?
O8 Mn1 O7 85.84(6) 4_457 3_447 ?
C4 N1 C2 121.6(2) . . ?
C4 N1 H1A 119.2 . . ?
C2 N1 H1A 119.2 . . ?
C17 N2 C18 122.9(2) . . ?
C17 N2 H2A 118.5 . . ?
C18 N2 H2A 118.5 . . ?
C1 O1 Mn1 133.48(17) . . ?
C1 O2 Mn1 128.87(15) . 4_457 ?
C11 O4 C10 122.4(2) . . ?
C20 O7 Mn1 138.30(16) . 2_365 ?
C20 O7 Mn1 121.35(15) . 3_457 ?
Mn1 O7 Mn1 96.02(6) 2_365 3_457 ?
Mn1 O8 Mn1 95.72(7) . 4_557 ?
Mn1 O8 H8C 122(3) . . ?
Mn1 O8 H8C 96(3) 4_557 . ?
Mn1 O8 H8B 119(3) . . ?
Mn1 O8 H8B 112(3) 4_557 . ?
H8C O8 H8B 109(3) . . ?
H9C O9 H9B 104(3) . . ?
O2 C1 O1 126.3(2) . . ?
O2 C1 C2 119.2(2) . . ?
O1 C1 C2 114.5(2) . . ?
N1 C2 C3 109.1(2) . . ?
N1 C2 C1 113.8(2) . . ?
C3 C2 C1 110.4(2) . . ?
N1 C2 H2B 107.8 . . ?
C3 C2 H2B 107.8 . . ?
C1 C2 H2B 107.8 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O3 C4 N1 122.1(2) . . ?
O3 C4 C5 119.7(2) . . ?
N1 C4 C5 118.1(2) . . ?
C6 C5 C7 119.1(2) . . ?
C6 C5 C4 118.8(2) . . ?
C7 C5 C4 121.9(2) . . ?
C8 C6 C5 120.7(2) . . ?
C8 C6 H6A 119.6 . . ?
C5 C6 H6A 119.6 . . ?
C9 C7 C5 120.4(2) . . ?
C9 C7 H7A 119.8 . . ?
C5 C7 H7A 119.8 . . ?
C6 C8 C10 119.2(2) . . ?
C6 C8 H8A 120.4 . . ?
C10 C8 H8A 120.4 . . ?
C10 C9 C7 119.4(2) . . ?
C10 C9 H9A 120.3 . . ?
C7 C9 H9A 120.3 . . ?
C9 C10 C8 121.1(2) . . ?
C9 C10 O4 123.1(2) . . ?
C8 C10 O4 115.5(2) . . ?
O4 C11 C12 125.2(2) . . ?
O4 C11 C13 114.2(2) . . ?
C12 C11 C13 120.6(2) . . ?
C11 C12 C14 119.1(2) . . ?
C11 C12 H12A 120.5 . . ?
C14 C12 H12A 120.5 . . ?
C15 C13 C11 119.4(3) . . ?
C15 C13 H13A 120.3 . . ?
C11 C13 H13A 120.3 . . ?
C16 C14 C12 121.2(3) . . ?
C16 C14 H14A 119.4 . . ?
C12 C14 H14A 119.4 . . ?
C13 C15 C16 121.0(2) . . ?
C13 C15 H15A 119.5 . . ?
C16 C15 H15A 119.5 . . ?
C14 C16 C15 118.7(2) . . ?
C14 C16 C17 123.8(2) . . ?
C15 C16 C17 117.5(2) . . ?
O5 C17 N2 123.2(2) . . ?
O5 C17 C16 120.6(2) . . ?
N2 C17 C16 116.2(2) . . ?
N2 C18 C19 111.4(2) . . ?
N2 C18 C20 108.79(19) . . ?
C19 C18 C20 111.1(2) . . ?
N2 C18 H18A 108.5 . . ?
C19 C18 H18A 108.5 . . ?
C20 C18 H18A 108.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O6 C20 O7 124.3(2) . . ?
O6 C20 C18 119.3(2) . . ?
O7 C20 C18 116.4(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mn1 O2 C1 O1 2.3(4) 4_457 . . . ?
Mn1 O2 C1 C2 -175.87(16) 4_457 . . . ?
Mn1 O1 C1 O2 -15.9(4) . . . . ?
Mn1 O1 C1 C2 162.38(17) . . . . ?
C4 N1 C2 C3 154.4(2) . . . . ?
C4 N1 C2 C1 -81.8(3) . . . . ?
O2 C1 C2 N1 -11.8(3) . . . . ?
O1 C1 C2 N1 169.8(2) . . . . ?
O2 C1 C2 C3 111.3(3) . . . . ?
O1 C1 C2 C3 -67.1(3) . . . . ?
C2 N1 C4 O3 7.1(4) . . . . ?
C2 N1 C4 C5 -169.8(2) . . . . ?
O3 C4 C5 C6 26.6(4) . . . . ?
N1 C4 C5 C6 -156.4(2) . . . . ?
O3 C4 C5 C7 -147.2(3) . . . . ?
N1 C4 C5 C7 29.7(3) . . . . ?
C7 C5 C6 C8 -1.0(4) . . . . ?
C4 C5 C6 C8 -175.0(2) . . . . ?
C6 C5 C7 C9 -1.6(4) . . . . ?
C4 C5 C7 C9 172.2(2) . . . . ?
C5 C6 C8 C10 3.0(4) . . . . ?
C5 C7 C9 C10 2.2(4) . . . . ?
C7 C9 C10 C8 -0.2(4) . . . . ?
C7 C9 C10 O4 -173.6(2) . . . . ?
C6 C8 C10 C9 -2.4(4) . . . . ?
C6 C8 C10 O4 171.5(2) . . . . ?
C11 O4 C10 C9 -54.6(4) . . . . ?
C11 O4 C10 C8 131.7(3) . . . . ?
C10 O4 C11 C12 -8.3(4) . . . . ?
C10 O4 C11 C13 174.0(3) . . . . ?
O4 C11 C12 C14 -179.5(3) . . . . ?
C13 C11 C12 C14 -1.9(4) . . . . ?
O4 C11 C13 C15 178.7(3) . . . . ?
C12 C11 C13 C15 0.9(4) . . . . ?
C11 C12 C14 C16 0.8(4) . . . . ?
C11 C13 C15 C16 1.4(4) . . . . ?
C12 C14 C16 C15 1.4(4) . . . . ?
C12 C14 C16 C17 -177.5(3) . . . . ?
C13 C15 C16 C14 -2.5(4) . . . . ?
C13 C15 C16 C17 176.5(3) . . . . ?
C18 N2 C17 O5 -6.8(4) . . . . ?
C18 N2 C17 C16 172.7(2) . . . . ?
C14 C16 C17 O5 -157.1(3) . . . . ?
C15 C16 C17 O5 24.0(4) . . . . ?
C14 C16 C17 N2 23.4(4) . . . . ?
C15 C16 C17 N2 -155.5(3) . . . . ?
C17 N2 C18 C19 104.6(3) . . . . ?
C17 N2 C18 C20 -132.6(2) . . . . ?
Mn1 O7 C20 O6 177.96(18) 2_365 . . . ?
Mn1 O7 C20 O6 27.7(3) 3_457 . . . ?
Mn1 O7 C20 C18 -2.9(4) 2_365 . . . ?
Mn1 O7 C20 C18 -153.21(16) 3_457 . . . ?
N2 C18 C20 O6 -16.3(3) . . . . ?
C19 C18 C20 O6 106.6(3) . . . . ?
N2 C18 C20 O7 164.5(2) . . . . ?
C19 C18 C20 O7 -72.5(3) . . . . ?

_refine_diff_density_max         0.301
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.047

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_4_sq
_database_code_depnum_ccdc_archive 'CCDC 1848126'
_audit_update_record             
;
2018-09-04 deposited with the CCDC.
2018-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H63 Cu2 N8 O14'
_chemical_formula_weight         1391.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.3695(15)
_cell_length_b                   19.989(2)
_cell_length_c                   15.6098(17)
_cell_angle_alpha                90
_cell_angle_beta                 96.395(4)
_cell_angle_gamma                90
_cell_volume                     4145.6(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3392
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      16.80

_exptl_crystal_description       plate-like
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_F_000             1444
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.571
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49024
_diffrn_reflns_av_unetI/netI     0.1305
_diffrn_reflns_av_R_equivalents  0.1172
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.019
_diffrn_reflns_theta_max         25.003
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.780
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.780
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.776
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             14529
_reflns_number_gt                7972
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_max     0.772
_reflns_Friedel_fraction_full    0.982

_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.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1042P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2727 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.051(11)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         14529
_refine_ls_number_parameters     866
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.0654
_refine_ls_wR_factor_ref         0.2068
_refine_ls_wR_factor_gt          0.1616
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_restrained_S_all      0.982
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.11346(8) 0.44359(7) 0.16075(9) 0.0450(4) Uani 1 1 d . . . . .
Cu2 Cu 0.84910(9) 0.84538(7) 0.65659(9) 0.0486(4) Uani 1 1 d . . . . .
C1 C 0.1238(7) 0.5221(6) 0.3070(8) 0.045(3) Uani 1 1 d . . . . .
C2 C 0.1285(8) 0.5428(6) 0.3999(8) 0.050(3) Uani 1 1 d . . . . .
H2A H 0.1691 0.5102 0.4356 0.060 Uiso 1 1 calc R U . . .
C3 C 0.0256(10) 0.5491(7) 0.4328(9) 0.080(4) Uani 1 1 d . . . . .
H3A H -0.0270 0.5565 0.3857 0.096 Uiso 1 1 calc R U . . .
H3B H 0.0096 0.5095 0.4646 0.096 Uiso 1 1 calc R U . . .
C4 C 0.0393(14) 0.6086(7) 0.4902(10) 0.103(6) Uani 1 1 d . . . . .
H4A H -0.0248 0.6301 0.4956 0.124 Uiso 1 1 calc R U . . .
H4B H 0.0701 0.5960 0.5471 0.124 Uiso 1 1 calc R U . . .
C5 C 0.1056(11) 0.6533(8) 0.4478(10) 0.082(4) Uani 1 1 d . . . . .
H5A H 0.0680 0.6788 0.4021 0.098 Uiso 1 1 calc R U . . .
H5B H 0.1409 0.6840 0.4888 0.098 Uiso 1 1 calc R U . . .
C6 C 0.2635(9) 0.6202(7) 0.3981(8) 0.059(3) Uani 1 1 d . . . . .
C7 C 0.2965(9) 0.6905(6) 0.3977(8) 0.056(3) Uani 1 1 d D . . . .
C8 C 0.2417(10) 0.7365(8) 0.3499(10) 0.090(5) Uani 1 1 d D . . . .
H8A H 0.1818 0.7233 0.3184 0.108 Uiso 1 1 calc R U . . .
C9 C 0.2723(11) 0.8046(8) 0.3459(12) 0.098(5) Uani 1 1 d D . . . .
H9A H 0.2330 0.8365 0.3146 0.118 Uiso 1 1 calc R U . . .
C10 C 0.3600(10) 0.8197(7) 0.3893(11) 0.080(5) Uani 1 1 d D . . . .
C11 C 0.4158(10) 0.7771(7) 0.4379(9) 0.075(4) Uani 1 1 d D . . . .
H11A H 0.4762 0.7913 0.4678 0.090 Uiso 1 1 calc R U . . .
C12 C 0.3860(9) 0.7132(6) 0.4446(8) 0.067(4) Uani 1 1 d D . . . .
H12A H 0.4249 0.6839 0.4805 0.081 Uiso 1 1 calc R U . . .
C13 C 0.4856(12) 0.9040(8) 0.3764(12) 0.084(5) Uani 1 1 d . . . . .
C14 C 0.5318(12) 0.9550(7) 0.4257(10) 0.080(4) Uani 1 1 d . . . . .
H14A H 0.4955 0.9780 0.4639 0.096 Uiso 1 1 calc R U . . .
C15 C 0.6269(11) 0.9721(7) 0.4197(10) 0.075(4) Uani 1 1 d . . . . .
H15A H 0.6536 1.0091 0.4504 0.090 Uiso 1 1 calc R U . . .
C16 C 0.6880(10) 0.9364(8) 0.3687(9) 0.068(4) Uani 1 1 d . . . . .
C17 C 0.6416(12) 0.8844(8) 0.3205(9) 0.083(5) Uani 1 1 d . . . . .
H17A H 0.6791 0.8596 0.2851 0.099 Uiso 1 1 calc R U . . .
C18 C 0.5439(12) 0.8687(8) 0.3232(11) 0.095(5) Uani 1 1 d . . . . .
H18A H 0.5152 0.8340 0.2892 0.114 Uiso 1 1 calc R U . . .
C19 C 0.7881(12) 0.9577(8) 0.3647(9) 0.070(4) Uani 1 1 d . . . . .
C20 C 0.8604(12) 0.8431(10) 0.3936(9) 0.092(4) Uani 1 1 d D U . . .
H20A H 0.8108 0.8194 0.3538 0.111 Uiso 1 1 calc R U . . .
C21 C 0.966(3) 0.8194(19) 0.381(2) 0.22(2) Uani 1 1 d D . . . .
H21A H 0.9843 0.7776 0.3620 0.261 Uiso 1 1 calc R U . . .
C22 C 1.031(3) 0.874(2) 0.405(3) 0.23(2) Uani 1 1 d D . . . .
H22A H 1.0952 0.8692 0.3819 0.273 Uiso 1 1 calc R U . . .
H22B H 1.0434 0.8787 0.4674 0.273 Uiso 1 1 calc R U . . .
C23 C 0.9736(16) 0.9309(13) 0.3661(14) 0.157(12) Uani 1 1 d D . . . .
H23A H 0.9879 0.9371 0.3070 0.189 Uiso 1 1 calc R U . . .
H23B H 0.9917 0.9716 0.3980 0.189 Uiso 1 1 calc R U . . .
C24 C 0.8393(10) 0.8303(9) 0.4884(10) 0.070(4) Uani 1 1 d . U . . .
C25 C 0.8516(7) 0.7657(7) 0.7985(10) 0.054(4) Uani 1 1 d . . . . .
C26 C 0.8563(8) 0.7490(5) 0.8972(8) 0.051(3) Uani 1 1 d . . . . .
H26A H 0.8311 0.7865 0.9289 0.062 Uiso 1 1 calc R U . . .
C27 C 0.9664(8) 0.7305(6) 0.9345(8) 0.062(3) Uani 1 1 d . . . . .
H27A H 1.0055 0.7165 0.8888 0.075 Uiso 1 1 calc R U . . .
H27B H 0.9996 0.7683 0.9644 0.075 Uiso 1 1 calc R U . . .
C28 C 0.9543(10) 0.6738(6) 0.9959(10) 0.077(4) Uani 1 1 d . . . . .
H28A H 1.0143 0.6462 1.0034 0.092 Uiso 1 1 calc R U . . .
H28B H 0.9403 0.6904 1.0517 0.092 Uiso 1 1 calc R U . . .
C29 C 0.8663(10) 0.6352(7) 0.9529(10) 0.077(4) Uani 1 1 d . . . . .
H29A H 0.8875 0.6040 0.9108 0.092 Uiso 1 1 calc R U . . .
H29B H 0.8324 0.6107 0.9948 0.092 Uiso 1 1 calc R U . . .
C30 C 0.7029(10) 0.6886(6) 0.8945(9) 0.064(4) Uani 1 1 d D . . . .
C31 C 0.6521(10) 0.6188(8) 0.8998(11) 0.082(5) Uani 1 1 d D . . . .
C32 C 0.6734(10) 0.5656(8) 0.8503(10) 0.084(4) Uani 1 1 d . . . . .
H32A H 0.7217 0.5709 0.8123 0.101 Uiso 1 1 calc R U . . .
C33 C 0.6287(10) 0.5073(7) 0.8537(12) 0.091(5) Uani 1 1 d . . . . .
H33A H 0.6440 0.4721 0.8185 0.109 Uiso 1 1 calc R U . . .
C34 C 0.5570(10) 0.4997(7) 0.9123(11) 0.079(4) Uani 1 1 d . . . . .
C35 C 0.5259(10) 0.5522(8) 0.9576(10) 0.078(4) Uani 1 1 d . . . . .
H35A H 0.4724 0.5483 0.9906 0.094 Uiso 1 1 calc R U . . .
C36 C 0.5768(9) 0.6105(7) 0.9526(10) 0.076(4) Uani 1 1 d . . . . .
H36A H 0.5602 0.6464 0.9862 0.091 Uiso 1 1 calc R U . . .
C37 C 0.4184(9) 0.4199(6) 0.9047(9) 0.065(4) Uani 1 1 d . . . . .
C38 C 0.3941(9) 0.3563(7) 0.9321(10) 0.077(4) Uani 1 1 d . . . . .
H38A H 0.4436 0.3285 0.9593 0.093 Uiso 1 1 calc R U . . .
C39 C 0.2950(10) 0.3352(7) 0.9181(9) 0.071(4) Uani 1 1 d . . . . .
H39A H 0.2793 0.2916 0.9328 0.085 Uiso 1 1 calc R U . . .
C40 C 0.2206(8) 0.3756(6) 0.8840(8) 0.051(3) Uani 1 1 d . . . . .
C41 C 0.2457(8) 0.4390(6) 0.8583(8) 0.056(3) Uani 1 1 d . . . . .
H41A H 0.1955 0.4671 0.8329 0.067 Uiso 1 1 calc R U . . .
C42 C 0.3430(9) 0.4612(6) 0.8697(8) 0.062(3) Uani 1 1 d . . . . .
H42A H 0.3580 0.5045 0.8535 0.074 Uiso 1 1 calc R U . . .
C43 C 0.1169(9) 0.3438(8) 0.8650(8) 0.064(3) Uani 1 1 d . . . . .
C44 C -0.0640(8) 0.3477(8) 0.8489(8) 0.069(3) Uani 1 1 d . . . . .
H44A H -0.0711 0.3141 0.8926 0.082 Uiso 1 1 calc R U . . .
H44B H -0.0714 0.3265 0.7926 0.082 Uiso 1 1 calc R U . . .
C45 C -0.1380(12) 0.4016(9) 0.8529(13) 0.115(5) Uani 1 1 d . U . . .
H45A H -0.1593 0.4184 0.7955 0.138 Uiso 1 1 calc R U . . .
H45B H -0.1968 0.3849 0.8774 0.138 Uiso 1 1 calc R U . . .
C46 C -0.0911(10) 0.4539(8) 0.9059(11) 0.104(5) Uani 1 1 d . U . . .
H46A H -0.1056 0.4485 0.9650 0.125 Uiso 1 1 calc R U . . .
H46B H -0.1161 0.4972 0.8852 0.125 Uiso 1 1 calc R U . . .
C47 C 0.0226(7) 0.4489(6) 0.9007(7) 0.051(3) Uani 1 1 d . . . . .
H47A H 0.0437 0.4829 0.8611 0.061 Uiso 1 1 calc R U . . .
C48 C 0.0743(8) 0.4607(6) 0.9908(9) 0.055(3) Uani 1 1 d . . . . .
C49 C -0.0950(9) 0.4977(7) 0.1627(9) 0.060(4) Uani 1 1 d . . . . .
H49A H -0.0634 0.5390 0.1711 0.071 Uiso 1 1 calc R U . . .
C50 C -0.1953(9) 0.4954(7) 0.1568(11) 0.077(5) Uani 1 1 d . . . . .
H50A H -0.2310 0.5350 0.1606 0.092 Uiso 1 1 calc R U . . .
C51 C -0.2469(8) 0.4366(8) 0.1455(8) 0.057(3) Uani 1 1 d . . . . .
C52 C -0.1912(8) 0.3806(6) 0.1407(8) 0.050(3) Uani 1 1 d . . . . .
H52A H -0.2227 0.3391 0.1348 0.059 Uiso 1 1 calc R U . . .
C53 C -0.0867(8) 0.3846(6) 0.1447(8) 0.052(3) Uani 1 1 d . . . . .
H53A H -0.0498 0.3458 0.1386 0.062 Uiso 1 1 calc R U . . .
C54 C -0.3584(9) 0.4295(7) 0.1428(9) 0.066(4) Uani 1 1 d . . . . .
H54A H -0.3859 0.3882 0.1257 0.079 Uiso 1 1 calc R U . . .
C55 C -0.4198(8) 0.4750(7) 0.1619(9) 0.063(4) Uani 1 1 d . U . . .
H55A H -0.3924 0.5159 0.1805 0.076 Uiso 1 1 calc R U . . .
C56 C -0.5285(7) 0.4679(4) 0.1568(8) 0.052(3) Uani 1 1 d D . . . .
C57 C -0.5772(7) 0.4059(5) 0.1409(8) 0.048(3) Uani 1 1 d D U . . .
H57A H -0.5403 0.3677 0.1314 0.058 Uiso 1 1 calc R U . . .
C58 C -0.6834(9) 0.4025(7) 0.1396(9) 0.061(4) Uani 1 1 d . . . . .
H58A H -0.7157 0.3621 0.1257 0.073 Uiso 1 1 calc R U . . .
C59 C -0.6933(9) 0.5136(7) 0.1728(10) 0.069(4) Uani 1 1 d . . . . .
H59A H -0.7322 0.5508 0.1829 0.083 Uiso 1 1 calc R U . . .
C60 C -0.5910(8) 0.5214(6) 0.1743(9) 0.065(4) Uani 1 1 d D . . . .
H60A H -0.5626 0.5632 0.1872 0.078 Uiso 1 1 calc R U . . .
C61 C 1.0461(7) 0.7700(6) 0.6643(9) 0.053(3) Uani 1 1 d . . . . .
H61A H 1.0076 0.7322 0.6716 0.064 Uiso 1 1 calc R U . . .
C62 C 1.1463(9) 0.7623(6) 0.6637(8) 0.062(4) Uani 1 1 d . . . . .
H62A H 1.1758 0.7204 0.6726 0.074 Uiso 1 1 calc R U . . .
C63 C 1.2050(7) 0.8180(6) 0.6494(7) 0.040(3) Uani 1 1 d . . . . .
C64 C 1.1567(7) 0.8756(6) 0.6390(9) 0.056(4) Uani 1 1 d . . . . .
H64A H 1.1941 0.9136 0.6297 0.068 Uiso 1 1 calc R U . . .
C65 C 1.0599(9) 0.8826(7) 0.6410(9) 0.062(4) Uani 1 1 d . . . . .
H65A H 1.0312 0.9248 0.6328 0.075 Uiso 1 1 calc R U . . .
C66 C 1.3118(7) 0.8087(6) 0.6495(7) 0.047(3) Uani 1 1 d . . . . .
H66A H 1.3368 0.7653 0.6528 0.057 Uiso 1 1 calc R U . . .
C67 C 1.3788(7) 0.8601(6) 0.6450(7) 0.047(3) Uani 1 1 d . . . . .
H67A H 1.3524 0.9032 0.6408 0.057 Uiso 1 1 calc R U . . .
C68 C 1.4867(7) 0.8536(6) 0.6463(7) 0.045(3) Uani 1 1 d . . . . .
C69 C 1.5448(8) 0.9108(7) 0.6355(9) 0.063(4) Uani 1 1 d . . . . .
H69A H 1.5132 0.9519 0.6250 0.076 Uiso 1 1 calc R U . . .
C70 C 1.6502(9) 0.9068(6) 0.6403(9) 0.057(4) Uani 1 1 d . . . . .
H70A H 1.6867 0.9458 0.6346 0.068 Uiso 1 1 calc R U . . .
C71 C 1.6462(9) 0.7941(6) 0.6573(9) 0.054(3) Uani 1 1 d . . . . .
H71A H 1.6810 0.7537 0.6592 0.065 Uiso 1 1 calc R U . . .
C72 C 1.5409(7) 0.7931(6) 0.6599(8) 0.051(3) Uani 1 1 d . . . . .
H72A H 1.5079 0.7535 0.6703 0.062 Uiso 1 1 calc R U . . .
N1 N 0.1722(7) 0.6089(4) 0.4149(6) 0.050(2) Uani 1 1 d . . . . .
N2 N 0.8641(10) 0.9156(7) 0.3685(7) 0.078(3) Uani 1 1 d . . . . .
N3 N 0.7995(6) 0.6880(4) 0.9102(6) 0.048(2) Uani 1 1 d . . . . .
N4 N 0.0331(7) 0.3823(5) 0.8649(6) 0.055(3) Uani 1 1 d . . . . .
N5 N -0.0378(6) 0.4433(6) 0.1571(6) 0.047(2) Uani 1 1 d . . . . .
N6 N -0.7388(6) 0.4553(5) 0.1576(6) 0.042(2) Uani 1 1 d . . . . .
N7 N 0.9995(7) 0.8286(5) 0.6549(6) 0.052(3) Uani 1 1 d . . . . .
N8 N 1.6980(6) 0.8515(6) 0.6521(6) 0.050(2) Uani 1 1 d . . . . .
O1 O 0.1295(5) 0.4611(4) 0.2869(5) 0.048(2) Uani 1 1 d . . . . .
O2 O 0.1075(5) 0.5681(4) 0.2503(5) 0.058(2) Uani 1 1 d . . . . .
O3 O 0.3210(7) 0.5755(5) 0.3805(6) 0.082(3) Uani 1 1 d . . . . .
O4 O 0.3842(7) 0.8902(5) 0.3820(9) 0.112(4) Uani 1 1 d . . . . .
O5 O 0.8083(7) 1.0180(6) 0.3528(7) 0.096(3) Uani 1 1 d . . . . .
O6 O 0.8156(10) 0.7719(7) 0.5046(9) 0.124(4) Uani 1 1 d . U . . .
O7 O 0.8464(5) 0.8776(4) 0.5389(6) 0.055(2) Uani 1 1 d . U . . .
O8 O 0.8600(5) 0.8286(4) 0.7830(5) 0.049(2) Uani 1 1 d . . . . .
O9 O 0.8428(6) 0.7228(4) 0.7441(6) 0.065(2) Uani 1 1 d . . . . .
O10 O 0.6535(6) 0.7379(5) 0.8737(7) 0.082(3) Uani 1 1 d . . . . .
O11 O 0.5177(7) 0.4357(5) 0.9169(8) 0.104(4) Uani 1 1 d . . . . .
O12 O 0.1126(6) 0.2841(4) 0.8451(7) 0.075(3) Uani 1 1 d . . . . .
O13 O 0.0902(6) 0.5199(4) 1.0132(6) 0.067(2) Uani 1 1 d . . . . .
O14 O 0.0915(6) 0.4105(4) 1.0413(6) 0.053(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O14 1.969(8) 1_554 ?
Cu1 O1 1.989(8) . ?
Cu1 N6 1.995(8) 1_655 ?
Cu1 N5 2.017(8) . ?
Cu2 O7 1.944(9) . ?
Cu2 O8 1.992(8) . ?
Cu2 N8 2.017(8) 1_455 ?
Cu2 N7 2.042(10) . ?
C1 O1 1.264(13) . ?
C1 O2 1.279(14) . ?
C1 C2 1.502(16) . ?
C2 N1 1.453(14) . ?
C2 C3 1.526(16) . ?
C3 C4 1.489(19) . ?
C4 C5 1.467(19) . ?
C5 N1 1.395(16) . ?
C6 O3 1.230(13) . ?
C6 N1 1.296(14) . ?
C6 C7 1.473(17) . ?
C7 C8 1.348(17) . ?
C7 C12 1.407(15) . ?
C8 C9 1.426(19) . ?
C9 C10 1.323(18) . ?
C10 C11 1.315(18) . ?
C10 O4 1.454(16) . ?
C11 C12 1.345(17) . ?
C13 C14 1.38(2) . ?
C13 C18 1.39(2) . ?
C13 O4 1.395(17) . ?
C14 C15 1.330(18) . ?
C15 C16 1.398(18) . ?
C16 C17 1.388(18) . ?
C16 C19 1.412(18) . ?
C17 C18 1.349(18) . ?
C19 O5 1.253(16) . ?
C19 N2 1.316(17) . ?
C20 N2 1.50(2) . ?
C20 C21 1.52(3) . ?
C20 C24 1.56(2) . ?
C21 C22 1.42(4) . ?
C22 C23 1.47(3) . ?
C23 N2 1.50(2) . ?
C24 O7 1.227(16) . ?
C24 O6 1.245(18) . ?
C25 O9 1.204(15) . ?
C25 O8 1.287(13) . ?
C25 C26 1.570(18) . ?
C26 N3 1.462(13) . ?
C26 C27 1.565(15) . ?
C27 C28 1.506(17) . ?
C28 C29 1.501(17) . ?
C29 N3 1.490(15) . ?
C30 O10 1.212(14) . ?
C30 N3 1.287(14) . ?
C30 C31 1.557(18) . ?
C31 C32 1.36(2) . ?
C31 C36 1.380(18) . ?
C32 C33 1.314(19) . ?
C33 C34 1.40(2) . ?
C34 C35 1.36(2) . ?
C34 O11 1.388(16) . ?
C35 C36 1.356(17) . ?
C37 O11 1.357(13) . ?
C37 C42 1.370(16) . ?
C37 C38 1.389(17) . ?
C38 C39 1.386(17) . ?
C39 C40 1.344(17) . ?
C40 C41 1.381(16) . ?
C40 C43 1.524(16) . ?
C41 C42 1.367(15) . ?
C43 O12 1.231(17) . ?
C43 N4 1.360(16) . ?
C44 N4 1.467(14) . ?
C44 C45 1.47(2) . ?
C45 C46 1.43(2) . ?
C46 C47 1.535(17) . ?
C47 N4 1.457(15) . ?
C47 C48 1.516(16) . ?
C48 O13 1.246(13) . ?
C48 O14 1.281(14) . ?
C49 C50 1.334(17) . ?
C49 N5 1.336(15) . ?
C50 C51 1.365(19) . ?
C51 C52 1.351(17) . ?
C51 C54 1.494(15) . ?
C52 C53 1.394(15) . ?
C53 N5 1.346(15) . ?
C54 C55 1.282(16) . ?
C55 C56 1.454(14) . ?
C56 C60 1.403(6) . ?
C56 C57 1.409(6) . ?
C57 C58 1.420(15) . ?
C58 N6 1.336(15) . ?
C59 N6 1.324(15) . ?
C59 C60 1.374(15) . ?
C61 N7 1.326(14) . ?
C61 C62 1.350(15) . ?
C62 C63 1.394(16) . ?
C63 C64 1.320(14) . ?
C63 C66 1.440(14) . ?
C64 C65 1.305(16) . ?
C65 N7 1.380(14) . ?
C66 C67 1.370(15) . ?
C67 C68 1.447(13) . ?
C68 C69 1.404(17) . ?
C68 C72 1.413(16) . ?
C69 C70 1.405(16) . ?
C70 N8 1.280(15) . ?
C71 N8 1.347(15) . ?
C71 C72 1.413(15) . ?
N6 Cu1 1.995(8) 1_455 ?
N8 Cu2 2.017(8) 1_655 ?
O14 Cu1 1.969(8) 1_556 ?

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
O14 Cu1 O1 170.1(3) 1_554 . ?
O14 Cu1 N6 93.4(4) 1_554 1_655 ?
O1 Cu1 N6 90.3(3) . 1_655 ?
O14 Cu1 N5 86.0(3) 1_554 . ?
O1 Cu1 N5 91.5(3) . . ?
N6 Cu1 N5 172.8(5) 1_655 . ?
O7 Cu2 O8 169.9(3) . . ?
O7 Cu2 N8 91.9(3) . 1_455 ?
O8 Cu2 N8 90.4(3) . 1_455 ?
O7 Cu2 N7 87.6(3) . . ?
O8 Cu2 N7 91.2(3) . . ?
N8 Cu2 N7 173.4(5) 1_455 . ?
O1 C1 O2 122.2(12) . . ?
O1 C1 C2 120.5(11) . . ?
O2 C1 C2 117.2(11) . . ?
N1 C2 C1 112.2(10) . . ?
N1 C2 C3 103.4(10) . . ?
C1 C2 C3 113.9(10) . . ?
C4 C3 C2 102.3(12) . . ?
C5 C4 C3 104.8(12) . . ?
N1 C5 C4 102.8(12) . . ?
O3 C6 N1 123.1(12) . . ?
O3 C6 C7 119.8(11) . . ?
N1 C6 C7 117.1(11) . . ?
C8 C7 C12 116.4(12) . . ?
C8 C7 C6 120.6(11) . . ?
C12 C7 C6 123.0(11) . . ?
C7 C8 C9 122.4(13) . . ?
C10 C9 C8 115.9(15) . . ?
C11 C10 C9 124.2(14) . . ?
C11 C10 O4 123.8(13) . . ?
C9 C10 O4 111.9(13) . . ?
C10 C11 C12 120.4(12) . . ?
C11 C12 C7 120.6(12) . . ?
C14 C13 C18 117.4(15) . . ?
C14 C13 O4 119.2(16) . . ?
C18 C13 O4 123.4(16) . . ?
C15 C14 C13 121.5(15) . . ?
C14 C15 C16 122.2(14) . . ?
C17 C16 C15 115.9(13) . . ?
C17 C16 C19 124.8(15) . . ?
C15 C16 C19 119.2(14) . . ?
C18 C17 C16 122.2(15) . . ?
C17 C18 C13 120.6(15) . . ?
O5 C19 N2 116.3(15) . . ?
O5 C19 C16 121.2(14) . . ?
N2 C19 C16 122.4(14) . . ?
N2 C20 C21 102(2) . . ?
N2 C20 C24 114.9(13) . . ?
C21 C20 C24 109.7(17) . . ?
C22 C21 C20 106(3) . . ?
C21 C22 C23 102(4) . . ?
C22 C23 N2 108(2) . . ?
O7 C24 O6 126.5(16) . . ?
O7 C24 C20 118.3(15) . . ?
O6 C24 C20 115.1(16) . . ?
O9 C25 O8 124.6(13) . . ?
O9 C25 C26 122.0(11) . . ?
O8 C25 C26 113.4(12) . . ?
N3 C26 C27 103.5(8) . . ?
N3 C26 C25 110.4(10) . . ?
C27 C26 C25 110.4(9) . . ?
C28 C27 C26 104.5(9) . . ?
C29 C28 C27 103.7(11) . . ?
N3 C29 C28 103.7(10) . . ?
O10 C30 N3 124.3(11) . . ?
O10 C30 C31 121.0(12) . . ?
N3 C30 C31 114.6(11) . . ?
C32 C31 C36 117.2(14) . . ?
C32 C31 C30 123.2(13) . . ?
C36 C31 C30 119.4(15) . . ?
C33 C32 C31 122.9(14) . . ?
C32 C33 C34 118.0(14) . . ?
C35 C34 O11 123.0(14) . . ?
C35 C34 C33 121.8(13) . . ?
O11 C34 C33 115.1(14) . . ?
C36 C35 C34 116.8(13) . . ?
C35 C36 C31 122.8(15) . . ?
O11 C37 C42 125.5(11) . . ?
O11 C37 C38 115.3(11) . . ?
C42 C37 C38 119.1(11) . . ?
C39 C38 C37 118.9(13) . . ?
C40 C39 C38 122.1(13) . . ?
C39 C40 C41 118.3(11) . . ?
C39 C40 C43 116.3(12) . . ?
C41 C40 C43 124.9(11) . . ?
C42 C41 C40 121.3(11) . . ?
C41 C42 C37 120.2(11) . . ?
O12 C43 N4 122.2(12) . . ?
O12 C43 C40 118.0(12) . . ?
N4 C43 C40 119.7(13) . . ?
N4 C44 C45 103.6(12) . . ?
C46 C45 C44 107.8(13) . . ?
C45 C46 C47 107.1(13) . . ?
N4 C47 C48 116.4(10) . . ?
N4 C47 C46 102.5(10) . . ?
C48 C47 C46 107.0(10) . . ?
O13 C48 O14 124.0(12) . . ?
O13 C48 C47 117.0(12) . . ?
O14 C48 C47 118.9(10) . . ?
C50 C49 N5 123.1(12) . . ?
C49 C50 C51 121.9(13) . . ?
C52 C51 C50 116.6(10) . . ?
C52 C51 C54 118.3(12) . . ?
C50 C51 C54 125.0(13) . . ?
C51 C52 C53 120.3(11) . . ?
N5 C53 C52 121.7(11) . . ?
C55 C54 C51 126.1(13) . . ?
C54 C55 C56 125.5(13) . . ?
C60 C56 C57 115.6(9) . . ?
C60 C56 C55 121.9(10) . . ?
C57 C56 C55 122.3(9) . . ?
C56 C57 C58 119.1(10) . . ?
N6 C58 C57 122.4(11) . . ?
N6 C59 C60 122.7(13) . . ?
C59 C60 C56 121.5(11) . . ?
N7 C61 C62 123.6(11) . . ?
C61 C62 C63 119.2(11) . . ?
C64 C63 C62 116.0(10) . . ?
C64 C63 C66 125.8(10) . . ?
C62 C63 C66 118.2(10) . . ?
C65 C64 C63 124.3(11) . . ?
C64 C65 N7 121.2(13) . . ?
C67 C66 C63 123.8(10) . . ?
C66 C67 C68 126.0(11) . . ?
C69 C68 C72 115.7(9) . . ?
C69 C68 C67 119.3(11) . . ?
C72 C68 C67 125.0(10) . . ?
C68 C69 C70 120.8(12) . . ?
N8 C70 C69 122.6(12) . . ?
N8 C71 C72 122.3(11) . . ?
C71 C72 C68 118.7(10) . . ?
C6 N1 C5 128.1(11) . . ?
C6 N1 C2 119.7(10) . . ?
C5 N1 C2 112.1(10) . . ?
C19 N2 C20 125.5(13) . . ?
C19 N2 C23 128.3(17) . . ?
C20 N2 C23 105.3(16) . . ?
C30 N3 C26 119.5(9) . . ?
C30 N3 C29 129.0(10) . . ?
C26 N3 C29 110.9(8) . . ?
C43 N4 C47 129.1(10) . . ?
C43 N4 C44 116.6(11) . . ?
C47 N4 C44 112.1(10) . . ?
C49 N5 C53 116.5(9) . . ?
C49 N5 Cu1 125.1(9) . . ?
C53 N5 Cu1 118.4(8) . . ?
C59 N6 C58 118.6(10) . . ?
C59 N6 Cu1 122.3(8) . 1_455 ?
C58 N6 Cu1 119.1(8) . 1_455 ?
C61 N7 C65 115.6(10) . . ?
C61 N7 Cu2 126.5(8) . . ?
C65 N7 Cu2 117.9(8) . . ?
C70 N8 C71 119.5(9) . . ?
C70 N8 Cu2 122.6(9) . 1_655 ?
C71 N8 Cu2 117.8(8) . 1_655 ?
C1 O1 Cu1 114.4(8) . . ?
C13 O4 C10 114.9(11) . . ?
C24 O7 Cu2 110.1(9) . . ?
C25 O8 Cu2 110.6(8) . . ?
C37 O11 C34 125.3(11) . . ?
C48 O14 Cu1 108.5(8) . 1_556 ?

_refine_diff_density_max         0.420
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.123

_shelxl_version_number           2014-3


# SQUEEZE RESULTS (Version =  91117)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.075 0.147 0.242 734 175 ' '
2 -0.062 0.647 0.247 735 175 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 0 0 1.533
-6 0 1 9.181
-5 0 1 7.651
0 7 1 7.270
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL 2 in P2(1)
CELL   13.3695   19.9890   15.6098     90.00     96.39     90.00
SPGR P21
# Solvent Accessible Volume =      1468
# Electrons Found in S.A.V. =       349
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
Q101 0.139 0.093 0.274 !       3.42 eA-3
C102 0.817 0.108 0.098 !       3.34 eA-3
C103 0.076 0.617 0.727 !       3.26 eA-3
C104 0.067 0.590 0.755 !       3.25 eA-3
C105 0.875 0.569 0.742 !       3.10 eA-3
C106 0.439 0.728 0.864 !       3.07 eA-3
Q107 1.005 0.184 0.745 !       2.89 eA-3
C108 0.532 0.579 0.390 !       2.75 eA-3
C109 0.548 0.267 0.093 !       2.58 eA-3
C110 0.484 0.124 0.358 !       2.54 eA-3
C111 0.540 0.613 0.340 !       2.51 eA-3
C112 0.734 0.548 0.403 !       2.48 eA-3
C113 0.478 0.080 0.652 !       2.42 eA-3
C114 0.302 0.721 0.057 !       2.35 eA-3
C115 0.957 0.669 0.248 !       2.35 eA-3
C116 0.249 0.685 0.108 !       2.21 eA-3
C117 0.341 0.643 0.651 !       2.18 eA-3
C118 0.719 0.229 0.057 !       2.16 eA-3
Q119 0.178 0.174 0.604 !       2.15 eA-3
C120 0.315 0.766 0.078 !       2.08 eA-3
C121 0.377 0.746 0.098 !       2.08 eA-3
C122 0.642 0.274 0.941 !       2.07 eA-3
C123 0.815 0.651 0.344 !       2.05 eA-3
Q124 0.312 0.817 0.122 !       1.99 eA-3
C125 0.717 0.248 0.980 !       1.99 eA-3
C126 0.701 0.538 0.360 !       1.98 eA-3
C127 0.232 0.011 0.437 !       1.91 eA-3
C128 0.264 0.687 0.061 !       1.91 eA-3
C129 0.594 0.616 0.619 !       1.83 eA-3
C130 0.341 0.740-0.001 !       1.77 eA-3
C131 0.285 0.644 0.750 !       1.74 eA-3
C132 0.795 0.220 0.931 !       1.69 eA-3
Q133 0.530 0.190 0.097 !       1.69 eA-3
C134 0.648 0.270 0.859 !       1.66 eA-3
C135 0.313 0.080 0.688 !       1.66 eA-3
C136 0.516 0.174 0.783 !       1.65 eA-3
C137 0.298 0.706-0.005 !       1.64 eA-3
C138 0.345 0.064 0.620 !       1.64 eA-3
C139 0.391 0.139 0.643 !       1.63 eA-3
C140 0.629 0.188 0.977 !       1.62 eA-3
C141 0.376 0.181 0.530 !       1.60 eA-3
C142 0.594 0.718 0.220 !       1.57 eA-3
C143 0.573 0.691 0.177 !       1.56 eA-3
C144 0.184 0.060 0.316 !       1.56 eA-3
C145 0.331 0.653 0.051 !       1.56 eA-3
C146 0.343 0.172 0.623 !       1.56 eA-3
C147 0.348 0.177 0.463 !       1.55 eA-3
C148 0.511 0.128 0.693 !       1.55 eA-3
Q149 0.456 0.078 0.371 !       1.53 eA-3
C150 0.738 0.674 0.182 !       1.52 eA-3
Q151 0.484 0.088 0.704 !       1.48 eA-3
C152 0.829 0.641 0.278 !       1.48 eA-3
C153 0.015 0.090 0.295 !       1.47 eA-3
Q154 0.782 0.251 0.854 !       1.46 eA-3
C155 0.783 0.641 0.550 !       1.46 eA-3
Q156 0.393 0.752 0.796 !       1.46 eA-3
C157 0.343 0.201 0.762 !       1.45 eA-3
C158 0.655 0.642 0.490 !       1.45 eA-3
C159 0.356 0.639 0.690 !       1.44 eA-3
C160 0.313 0.673 0.817 !       1.44 eA-3
C161 0.671 0.671 0.442 !       1.43 eA-3
C162 0.761 0.250 0.920 !       1.43 eA-3
C163 0.389 0.744 0.174 !       1.43 eA-3
C164 0.613 0.207 0.944 !       1.43 eA-3
Q165 0.348 0.544 0.674 !       1.42 eA-3
C166 0.745 0.680 0.251 !       1.42 eA-3
C167 0.684 0.121 0.189 !       1.42 eA-3
C168 0.407 0.058 0.591 !       1.42 eA-3
Q169 0.779 0.709 0.208 !       1.42 eA-3
C170 0.436 0.076 0.546 !       1.40 eA-3
Q171 0.220 0.572 0.989 !       1.40 eA-3
C172 0.638 0.714 0.418 !       1.40 eA-3
C173 0.735 0.662 0.286 !       1.39 eA-3
Q174 0.423 0.680 0.860 !       1.37 eA-3
C175 0.407 0.128 0.493 !       1.37 eA-3
C176 0.702 0.173 0.083 !       1.37 eA-3
Q177 0.014 0.659 0.845 !       1.37 eA-3
C178 0.253 0.052 0.386 !       1.36 eA-3
Q179 0.361 0.684 0.660 !       1.35 eA-3
Q180 0.594 0.529 0.314 !       1.34 eA-3
C181 0.611 0.659 0.237 !       1.34 eA-3
C182 0.467 0.188 0.750 !       1.34 eA-3
C183 0.372 0.142 0.571 !       1.33 eA-3
C184 0.026 0.115 0.240 !       1.33 eA-3
C185 0.421 0.781 0.119 !       1.33 eA-3
Q186 0.855 0.099 0.059 !       1.33 eA-3
C187 0.312 0.059 0.395 !       1.32 eA-3
Q188 0.825 0.672 0.452 !       1.31 eA-3
C189 0.609 0.687 0.428 !       1.30 eA-3
C190 0.410 0.688 0.796 !       1.30 eA-3
C191 0.832 0.501 0.557 !       1.30 eA-3
C192 0.735 0.122 0.112 !       1.29 eA-3
C193 0.810 0.574 0.622 !       1.29 eA-3
C194 0.729 0.190 0.059 !       1.29 eA-3
C195 0.513 0.222 0.935 !       1.28 eA-3
C196 0.232 0.984 0.401 !       1.28 eA-3
C197 0.952 0.576 0.794 !       1.28 eA-3
C198 0.593 0.687 0.299 !       1.27 eA-3
C199 0.593 0.158 0.944 !       1.27 eA-3
;

####################################################################### 
# 
# 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 1848125'
_audit_update_record             
;
2018-09-04 deposited with the CCDC.
2018-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H22 Co N2 O9'
_chemical_formula_weight         493.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.3508(9)
_cell_length_b                   10.4298(14)
_cell_length_c                   31.772(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2104.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5692
_cell_measurement_theta_min      5.129
_cell_measurement_theta_max      44.522

_exptl_crystal_description       needle-like
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_F_000             1020
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.872
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29106
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.055
_diffrn_reflns_theta_max         28.694
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5060
_reflns_number_gt                4038
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.680
_reflns_Friedel_fraction_max     0.889
_reflns_Friedel_fraction_full    0.996

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0273P)²+0.8428P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1436 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(11)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         5060
_refine_ls_number_parameters     305
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0766
_refine_ls_wR_factor_gt          0.0698
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.15195(6) 0.25191(5) 0.99464(2) 0.02266(11) Uani 1 1 d . . . . .
N1 N -0.2440(5) 0.5831(3) 1.10424(9) 0.0277(7) Uani 1 1 d . . . . .
H1A H -0.2869 0.5491 1.1274 0.033 Uiso 1 1 calc R U . . .
N2 N -1.4112(5) 0.7302(3) 1.34594(9) 0.0319(8) Uani 1 1 d . . . . .
H2A H -1.3133 0.6801 1.3371 0.038 Uiso 1 1 calc R U . . .
O1 O 0.0799(4) 0.4029(2) 1.03200(8) 0.0304(6) Uani 1 1 d . . . . .
O2 O -0.2667(4) 0.3908(2) 1.04534(8) 0.0290(6) Uani 1 1 d . . . . .
O3 O -0.3173(4) 0.7190(2) 1.05140(8) 0.0366(7) Uani 1 1 d . . . . .
O4 O -0.9738(5) 0.9451(3) 1.17870(9) 0.0451(8) Uani 1 1 d . . . . .
O5 O -1.6159(5) 0.9005(3) 1.32978(9) 0.0477(8) Uani 1 1 d . . . . .
O6 O -1.1492(4) 0.6656(2) 1.40673(7) 0.0316(6) Uani 1 1 d . . . . .
O7 O -1.3831(4) 0.7003(2) 1.45793(7) 0.0258(5) Uani 1 1 d . . . . .
O8 O 0.4154(4) 0.3613(2) 0.97391(9) 0.0261(6) Uani 1 1 d D . . . .
H8C H 0.475(8) 0.355(4) 0.9509(10) 0.065(18) Uiso 1 1 d D . . . .
H8B H 0.425(7) 0.435(3) 0.9822(13) 0.052(15) Uiso 1 1 d D . . . .
O9 O 0.4585(7) 0.6076(3) 0.98488(12) 0.0585(9) Uani 1 1 d D . . . .
H9C H 0.371(7) 0.662(4) 0.9753(13) 0.071(18) Uiso 1 1 d D . . . .
H9B H 0.492(9) 0.634(5) 1.0086(10) 0.10(2) Uiso 1 1 d D . . . .
C1 C -0.0848(6) 0.4342(3) 1.05127(11) 0.0246(8) Uani 1 1 d . . . . .
C2 C -0.0510(5) 0.5357(3) 1.08519(12) 0.0268(8) Uani 1 1 d . . . . .
H2B H 0.0198 0.6088 1.0719 0.032 Uiso 1 1 calc R U . . .
C3 C 0.0941(6) 0.4845(4) 1.11932(13) 0.0394(10) Uani 1 1 d . . . . .
H3A H 0.2215 0.4532 1.1067 0.059 Uiso 1 1 calc R U . . .
H3B H 0.1272 0.5521 1.1387 0.059 Uiso 1 1 calc R U . . .
H3C H 0.0253 0.4159 1.1341 0.059 Uiso 1 1 calc R U . . .
C4 C -0.3562(6) 0.6770(3) 1.08720(11) 0.0262(8) Uani 1 1 d . . . . .
C5 C -0.5272(5) 0.7356(4) 1.11295(11) 0.0264(8) Uani 1 1 d . . . . .
C6 C -0.6937(6) 0.7955(3) 1.09263(12) 0.0305(9) Uani 1 1 d . . . . .
H6A H -0.7020 0.7927 1.0634 0.037 Uiso 1 1 calc R U . . .
C7 C -0.5166(5) 0.7412(4) 1.15663(11) 0.0306(8) Uani 1 1 d . . . . .
H7A H -0.4081 0.6993 1.1706 0.037 Uiso 1 1 calc R U . . .
C8 C -0.8467(6) 0.8592(3) 1.11508(12) 0.0319(8) Uani 1 1 d . . . . .
H8A H -0.9595 0.8975 1.1013 0.038 Uiso 1 1 calc R U . . .
C9 C -0.6650(6) 0.8082(4) 1.17940(12) 0.0349(9) Uani 1 1 d . . . . .
H9A H -0.6538 0.8147 1.2085 0.042 Uiso 1 1 calc R U . . .
C10 C -0.8303(6) 0.8653(4) 1.15844(12) 0.0327(9) Uani 1 1 d . . . . .
C11 C -1.0872(6) 0.9062(4) 1.21336(12) 0.0320(9) Uani 1 1 d . . . . .
C12 C -1.0913(6) 0.7832(4) 1.22899(12) 0.0358(10) Uani 1 1 d . . . . .
H12A H -1.0124 0.7189 1.2163 0.043 Uiso 1 1 calc R U . . .
C13 C -1.2101(6) 1.0006(4) 1.23138(12) 0.0367(10) Uani 1 1 d . . . . .
H13A H -1.2092 1.0831 1.2203 0.044 Uiso 1 1 calc R U . . .
C14 C -1.2143(5) 0.7563(4) 1.26393(11) 0.0351(8) Uani 1 1 d . . . . .
H14A H -1.2158 0.6736 1.2749 0.042 Uiso 1 1 calc R U . . .
C15 C -1.3336(7) 0.9727(4) 1.26568(11) 0.0350(9) Uani 1 1 d . . . . .
H15A H -1.4172 1.0365 1.2775 0.042 Uiso 1 1 calc R U . . .
C16 C -1.3351(6) 0.8510(4) 1.28282(11) 0.0299(8) Uani 1 1 d . . . . .
C17 C -1.4666(6) 0.8293(4) 1.32133(12) 0.0311(9) Uani 1 1 d . . . . .
C18 C -1.5061(6) 0.7020(4) 1.38672(11) 0.0284(8) Uani 1 1 d . . . . .
H18A H -1.5973 0.7736 1.3949 0.034 Uiso 1 1 calc R U . . .
C19 C -1.6374(7) 0.5799(4) 1.38487(13) 0.0411(10) Uani 1 1 d . . . . .
H19A H -1.6979 0.5636 1.4120 0.062 Uiso 1 1 calc R U . . .
H19B H -1.7477 0.5901 1.3645 0.062 Uiso 1 1 calc R U . . .
H19C H -1.5492 0.5092 1.3769 0.062 Uiso 1 1 calc R U . . .
C20 C -1.3315(6) 0.6883(3) 1.41909(11) 0.0241(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2 2.023(2) 4_557 ?
Co1 O1 2.025(3) . ?
Co1 O7 2.127(2) 2_364 ?
Co1 O8 2.130(3) . ?
Co1 O8 2.156(3) 4_457 ?
Co1 O7 2.171(2) 3_447 ?
N1 C4 1.327(4) . ?
N1 C2 1.454(4) . ?
N1 H1A 0.8600 . ?
N2 C17 1.343(5) . ?
N2 C18 1.459(4) . ?
N2 H2A 0.8600 . ?
O1 C1 1.255(4) . ?
O2 C1 1.255(4) . ?
O2 Co1 2.023(2) 4_457 ?
O3 C4 1.243(4) . ?
O4 C11 1.377(5) . ?
O4 C10 1.392(4) . ?
O5 C17 1.234(4) . ?
O6 C20 1.245(4) . ?
O7 C20 1.283(4) . ?
O7 Co1 2.127(2) 2_365 ?
O7 Co1 2.171(2) 3_457 ?
O8 Co1 2.156(3) 4_557 ?
O8 H8C 0.83(2) . ?
O8 H8B 0.82(2) . ?
O9 H9C 0.85(2) . ?
O9 H9B 0.83(2) . ?
C1 C2 1.526(5) . ?
C2 C3 1.520(5) . ?
C2 H2B 0.9800 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 C5 1.490(5) . ?
C5 C6 1.388(5) . ?
C5 C7 1.390(5) . ?
C6 C8 1.376(5) . ?
C6 H6A 0.9300 . ?
C7 C9 1.378(5) . ?
C7 H7A 0.9300 . ?
C8 C10 1.383(5) . ?
C8 H8A 0.9300 . ?
C9 C10 1.378(5) . ?
C9 H9A 0.9300 . ?
C11 C12 1.376(5) . ?
C11 C13 1.380(5) . ?
C12 C14 1.386(5) . ?
C12 H12A 0.9300 . ?
C13 C15 1.374(5) . ?
C13 H13A 0.9300 . ?
C14 C16 1.387(5) . ?
C14 H14A 0.9300 . ?
C15 C16 1.382(5) . ?
C15 H15A 0.9300 . ?
C16 C17 1.499(5) . ?
C18 C20 1.519(5) . ?
C18 C19 1.523(5) . ?
C18 H18A 0.9800 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O1 176.20(11) 4_557 . ?
O2 Co1 O7 91.89(10) 4_557 2_364 ?
O1 Co1 O7 87.59(10) . 2_364 ?
O2 Co1 O8 89.95(11) 4_557 . ?
O1 Co1 O8 86.68(11) . . ?
O7 Co1 O8 109.62(10) 2_364 . ?
O2 Co1 O8 93.80(11) 4_557 4_457 ?
O1 Co1 O8 89.82(10) . 4_457 ?
O7 Co1 O8 79.81(9) 2_364 4_457 ?
O8 Co1 O8 169.76(7) . 4_457 ?
O2 Co1 O7 94.64(10) 4_557 3_447 ?
O1 Co1 O7 86.48(10) . 3_447 ?
O7 Co1 O7 168.89(8) 2_364 3_447 ?
O8 Co1 O7 79.41(10) . 3_447 ?
O8 Co1 O7 90.78(9) 4_457 3_447 ?
C4 N1 C2 122.3(3) . . ?
C4 N1 H1A 118.8 . . ?
C2 N1 H1A 118.8 . . ?
C17 N2 C18 124.3(3) . . ?
C17 N2 H2A 117.8 . . ?
C18 N2 H2A 117.8 . . ?
C1 O1 Co1 132.5(2) . . ?
C1 O2 Co1 126.5(2) . 4_457 ?
C11 O4 C10 122.4(3) . . ?
C20 O7 Co1 139.1(2) . 2_365 ?
C20 O7 Co1 121.3(2) . 3_457 ?
Co1 O7 Co1 95.97(9) 2_365 3_457 ?
Co1 O8 Co1 96.36(10) . 4_557 ?
Co1 O8 H8C 126(3) . . ?
Co1 O8 H8C 93(4) 4_557 . ?
Co1 O8 H8B 118(3) . . ?
Co1 O8 H8B 108(3) 4_557 . ?
H8C O8 H8B 109(3) . . ?
H9C O9 H9B 106(3) . . ?
O2 C1 O1 126.9(3) . . ?
O2 C1 C2 119.1(3) . . ?
O1 C1 C2 114.0(3) . . ?
N1 C2 C3 109.5(3) . . ?
N1 C2 C1 114.3(3) . . ?
C3 C2 C1 110.2(3) . . ?
N1 C2 H2B 107.5 . . ?
C3 C2 H2B 107.5 . . ?
C1 C2 H2B 107.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O3 C4 N1 121.7(3) . . ?
O3 C4 C5 120.2(3) . . ?
N1 C4 C5 118.0(3) . . ?
C6 C5 C7 118.8(3) . . ?
C6 C5 C4 119.0(3) . . ?
C7 C5 C4 122.0(3) . . ?
C8 C6 C5 120.9(3) . . ?
C8 C6 H6A 119.5 . . ?
C5 C6 H6A 119.5 . . ?
C9 C7 C5 120.8(3) . . ?
C9 C7 H7A 119.6 . . ?
C5 C7 H7A 119.6 . . ?
C6 C8 C10 119.0(4) . . ?
C6 C8 H8A 120.5 . . ?
C10 C8 H8A 120.5 . . ?
C7 C9 C10 119.1(3) . . ?
C7 C9 H9A 120.5 . . ?
C10 C9 H9A 120.5 . . ?
C9 C10 C8 121.2(3) . . ?
C9 C10 O4 122.2(3) . . ?
C8 C10 O4 116.0(3) . . ?
C12 C11 O4 125.0(3) . . ?
C12 C11 C13 120.3(4) . . ?
O4 C11 C13 114.7(4) . . ?
C11 C12 C14 119.3(4) . . ?
C11 C12 H12A 120.4 . . ?
C14 C12 H12A 120.4 . . ?
C15 C13 C11 120.0(4) . . ?
C15 C13 H13A 120.0 . . ?
C11 C13 H13A 120.0 . . ?
C12 C14 C16 120.9(4) . . ?
C12 C14 H14A 119.5 . . ?
C16 C14 H14A 119.5 . . ?
C13 C15 C16 120.7(4) . . ?
C13 C15 H15A 119.6 . . ?
C16 C15 H15A 119.6 . . ?
C15 C16 C14 118.7(4) . . ?
C15 C16 C17 117.6(3) . . ?
C14 C16 C17 123.7(3) . . ?
O5 C17 N2 122.5(4) . . ?
O5 C17 C16 121.0(4) . . ?
N2 C17 C16 116.4(3) . . ?
N2 C18 C20 108.6(3) . . ?
N2 C18 C19 111.1(3) . . ?
C20 C18 C19 110.3(3) . . ?
N2 C18 H18A 108.9 . . ?
C20 C18 H18A 108.9 . . ?
C19 C18 H18A 108.9 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O6 C20 O7 124.0(3) . . ?
O6 C20 C18 118.9(3) . . ?
O7 C20 C18 117.1(3) . . ?

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 O2 C1 O1 4.3(6) 4_457 . . . ?
Co1 O2 C1 C2 -175.5(2) 4_457 . . . ?
Co1 O1 C1 O2 -15.9(6) . . . . ?
Co1 O1 C1 C2 163.9(2) . . . . ?
C4 N1 C2 C3 151.1(3) . . . . ?
C4 N1 C2 C1 -84.7(4) . . . . ?
O2 C1 C2 N1 -7.0(5) . . . . ?
O1 C1 C2 N1 173.2(3) . . . . ?
O2 C1 C2 C3 116.9(4) . . . . ?
O1 C1 C2 C3 -63.0(4) . . . . ?
C2 N1 C4 O3 9.1(5) . . . . ?
C2 N1 C4 C5 -168.5(3) . . . . ?
O3 C4 C5 C6 26.6(5) . . . . ?
N1 C4 C5 C6 -155.7(3) . . . . ?
O3 C4 C5 C7 -148.0(4) . . . . ?
N1 C4 C5 C7 29.6(5) . . . . ?
C7 C5 C6 C8 -0.3(6) . . . . ?
C4 C5 C6 C8 -175.1(3) . . . . ?
C6 C5 C7 C9 -1.9(6) . . . . ?
C4 C5 C7 C9 172.8(4) . . . . ?
C5 C6 C8 C10 1.4(6) . . . . ?
C5 C7 C9 C10 2.8(6) . . . . ?
C7 C9 C10 C8 -1.6(6) . . . . ?
C7 C9 C10 O4 -173.3(4) . . . . ?
C6 C8 C10 C9 -0.5(6) . . . . ?
C6 C8 C10 O4 171.7(3) . . . . ?
C11 O4 C10 C9 -55.8(6) . . . . ?
C11 O4 C10 C8 132.1(4) . . . . ?
C10 O4 C11 C12 -7.6(6) . . . . ?
C10 O4 C11 C13 175.3(4) . . . . ?
O4 C11 C12 C14 -179.3(4) . . . . ?
C13 C11 C12 C14 -2.3(6) . . . . ?
C12 C11 C13 C15 1.5(6) . . . . ?
O4 C11 C13 C15 178.7(4) . . . . ?
C11 C12 C14 C16 1.0(6) . . . . ?
C11 C13 C15 C16 0.7(6) . . . . ?
C13 C15 C16 C14 -2.0(6) . . . . ?
C13 C15 C16 C17 177.4(4) . . . . ?
C12 C14 C16 C15 1.1(6) . . . . ?
C12 C14 C16 C17 -178.2(4) . . . . ?
C18 N2 C17 O5 -5.7(6) . . . . ?
C18 N2 C17 C16 173.5(3) . . . . ?
C15 C16 C17 O5 22.6(6) . . . . ?
C14 C16 C17 O5 -158.1(4) . . . . ?
C15 C16 C17 N2 -156.7(4) . . . . ?
C14 C16 C17 N2 22.6(5) . . . . ?
C17 N2 C18 C20 -127.6(4) . . . . ?
C17 N2 C18 C19 110.8(4) . . . . ?
Co1 O7 C20 O6 175.2(3) 2_365 . . . ?
Co1 O7 C20 O6 22.8(5) 3_457 . . . ?
Co1 O7 C20 C18 -5.2(5) 2_365 . . . ?
Co1 O7 C20 C18 -157.6(2) 3_457 . . . ?
N2 C18 C20 O6 -20.1(5) . . . . ?
C19 C18 C20 O6 101.9(4) . . . . ?
N2 C18 C20 O7 160.4(3) . . . . ?
C19 C18 C20 O7 -77.6(4) . . . . ?

_refine_diff_density_max         0.455
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.059

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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 1848127'
_audit_update_record             
;
2018-09-04 deposited with the CCDC.
2018-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8.84 H8.14 Cd0.18 N0.91 O1.96'
_chemical_formula_weight         178.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   42.4758(9)
_cell_length_b                   13.9687(3)
_cell_length_c                   23.1291(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.610(3)
_cell_angle_gamma                90
_cell_volume                     13217.1(6)
_cell_formula_units_Z            57
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    17887
_cell_measurement_theta_min      4.5170
_cell_measurement_theta_max      73.9030

_exptl_crystal_description       plate-like
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_F_000             5228
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    3.811
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.42774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '?Ø scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            63646
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_av_R_equivalents  0.1300
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.737
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_point_group_measured_fraction_full 0.870
_reflns_number_total             20801
_reflns_number_gt                15514
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.687
_reflns_Friedel_fraction_max     0.751
_reflns_Friedel_fraction_full    0.741

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1769P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 4840 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(9)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         20801
_refine_ls_number_parameters     1563
_refine_ls_number_restraints     884
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0922
_refine_ls_wR_factor_ref         0.2636
_refine_ls_wR_factor_gt          0.2483
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      2.982
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.46326(2) 0.81452(8) 0.93442(4) 0.0452(2) Uani 1 1 d . . . . .
Cd2 Cd 0.0000 0.63638(11) 0.5000 0.0489(3) Uani 1 2 d S T P . .
Cd3 Cd 0.08625(2) 0.67437(9) 0.44439(5) 0.0545(3) Uani 1 1 d . . . . .
C1 C 0.5477(3) 0.8154(13) 0.9518(7) 0.061(3) Uani 1 1 d . U . . .
C2 C 0.5509(3) 0.8080(11) 0.8860(8) 0.069(3) Uani 1 1 d D U . . .
H2A H 0.5309 0.8327 0.8580 0.083 Uiso 1 1 calc R U . . .
C3 C 0.5562(4) 0.7145(12) 0.8703(10) 0.084(3) Uani 1 1 d D U . . .
H3A H 0.5491 0.6687 0.8958 0.101 Uiso 1 1 calc R U . . .
H3B H 0.5449 0.7015 0.8287 0.101 Uiso 1 1 calc R U . . .
C4 C 0.5899(4) 0.7112(13) 0.8795(11) 0.095(4) Uani 1 1 d D U . . .
H4A H 0.6001 0.6926 0.9207 0.114 Uiso 1 1 calc R U . . .
H4B H 0.5952 0.6631 0.8534 0.114 Uiso 1 1 calc R U . . .
C5 C 0.6022(4) 0.7988(11) 0.8682(10) 0.093(4) Uani 1 1 d D U . . .
H5A H 0.6039 0.8034 0.8273 0.112 Uiso 1 1 calc R U . . .
H5B H 0.6233 0.8123 0.8960 0.112 Uiso 1 1 calc R U . . .
C6 C 0.5824(3) 0.9562(13) 0.8908(7) 0.059(3) Uani 1 1 d . U . . .
C7 C 0.6108(4) 1.0073(14) 0.8804(8) 0.065(3) Uani 1 1 d . U . . .
C8 C 0.6185(4) 1.0057(15) 0.8275(8) 0.072(3) Uani 1 1 d . U . . .
H8A H 0.6064 0.9682 0.7961 0.086 Uiso 1 1 calc R U . . .
C9 C 0.6449(4) 1.0607(15) 0.8198(9) 0.073(3) Uani 1 1 d . U . . .
H9A H 0.6506 1.0567 0.7837 0.088 Uiso 1 1 calc R U . . .
C10 C 0.6616(4) 1.1170(15) 0.8621(9) 0.075(3) Uani 1 1 d . U . . .
C11 C 0.6548(4) 1.1221(15) 0.9202(9) 0.078(3) Uani 1 1 d . U . . .
H11A H 0.6669 1.1596 0.9516 0.094 Uiso 1 1 calc R U . . .
C12 C 0.6281(4) 1.0647(14) 0.9248(9) 0.073(3) Uani 1 1 d . U . . .
H12A H 0.6220 1.0665 0.9606 0.088 Uiso 1 1 calc R U . . .
C13 C 0.7137(4) 1.1336(15) 0.8450(8) 0.072(3) Uani 1 1 d . U . . .
C14 C 0.7220(4) 1.0400(14) 0.8562(8) 0.071(3) Uani 1 1 d . U . . .
H14A H 0.7089 0.9996 0.8718 0.086 Uiso 1 1 calc R U . . .
C15 C 0.7497(3) 1.0060(14) 0.8443(8) 0.067(3) Uani 1 1 d . U . . .
H15A H 0.7550 0.9415 0.8500 0.081 Uiso 1 1 calc R U . . .
C16 C 0.7700(3) 1.0678(14) 0.8237(7) 0.065(3) Uani 1 1 d . U . . .
C17 C 0.7615(3) 1.1607(14) 0.8119(8) 0.070(3) Uani 1 1 d . U . . .
H17A H 0.7748 1.2003 0.7964 0.084 Uiso 1 1 calc R U . . .
C18 C 0.7323(4) 1.1991(14) 0.8227(8) 0.073(3) Uani 1 1 d . U . . .
H18A H 0.7263 1.2628 0.8155 0.087 Uiso 1 1 calc R U . . .
C19 C 0.8011(3) 1.0267(14) 0.8101(7) 0.063(3) Uani 1 1 d . U . . .
C20 C 0.8368(3) 1.1432(15) 0.8751(8) 0.090(4) Uani 1 1 d D U . . .
H20A H 0.8281 1.1252 0.9083 0.108 Uiso 1 1 calc R U . . .
H20B H 0.8280 1.2052 0.8601 0.108 Uiso 1 1 calc R U . . .
C21 C 0.8707(3) 1.1462(17) 0.8933(7) 0.087(3) Uani 1 1 d D U . . .
H21A H 0.8789 1.1056 0.9281 0.105 Uiso 1 1 calc R U . . .
H21B H 0.8782 1.2111 0.9037 0.105 Uiso 1 1 calc R U . . .
C22 C 0.8817(3) 1.1135(13) 0.8454(7) 0.075(3) Uani 1 1 d D U . . .
H22A H 0.9027 1.0818 0.8595 0.090 Uiso 1 1 calc R U . . .
H22B H 0.8838 1.1660 0.8191 0.090 Uiso 1 1 calc R U . . .
C23 C 0.8577(2) 1.0495(11) 0.8159(7) 0.063(3) Uani 1 1 d D U . . .
H23A H 0.8545 1.0548 0.7724 0.076 Uiso 1 1 calc R U . . .
C24 C 0.8666(3) 0.9465(13) 0.8356(8) 0.064(3) Uani 1 1 d D U . . .
C25 C 0.4371(3) 0.8485(13) 0.8147(8) 0.067(3) Uani 1 1 d . U . . .
C26 C 0.4218(4) 0.8889(14) 0.7515(8) 0.075(3) Uani 1 1 d . U . . .
H26A H 0.4368 0.8800 0.7262 0.090 Uiso 1 1 calc R U . . .
C27 C 0.4138(4) 0.9970(15) 0.7553(9) 0.084(3) Uani 1 1 d . U . . .
H27A H 0.4105 1.0127 0.7942 0.101 Uiso 1 1 calc R U . . .
H27B H 0.4311 1.0369 0.7484 0.101 Uiso 1 1 calc R U . . .
C28 C 0.3833(5) 1.0092(17) 0.7072(10) 0.091(4) Uani 1 1 d . U . . .
H28A H 0.3881 1.0179 0.6688 0.110 Uiso 1 1 calc R U . . .
H28B H 0.3713 1.0647 0.7150 0.110 Uiso 1 1 calc R U . . .
C29 C 0.3637(5) 0.9199(17) 0.7066(11) 0.097(4) Uani 1 1 d . U . . .
H29A H 0.3512 0.9234 0.7359 0.116 Uiso 1 1 calc R U . . .
H29B H 0.3489 0.9087 0.6672 0.116 Uiso 1 1 calc R U . . .
C30 C 0.3884(4) 0.7510(17) 0.7062(8) 0.073(3) Uani 1 1 d . U . . .
C31 C 0.3562(4) 0.7126(15) 0.6794(7) 0.069(3) Uani 1 1 d . U . . .
C32 C 0.3548(4) 0.6405(15) 0.6357(7) 0.072(3) Uani 1 1 d . U . . .
H32A H 0.3738 0.6231 0.6258 0.087 Uiso 1 1 calc R U . . .
C33 C 0.3260(4) 0.5955(16) 0.6077(8) 0.074(3) Uani 1 1 d . U . . .
H33A H 0.3253 0.5540 0.5759 0.089 Uiso 1 1 calc R U . . .
C34 C 0.2981(4) 0.6110(15) 0.6259(8) 0.072(3) Uani 1 1 d . U . . .
C35 C 0.2984(4) 0.6773(15) 0.6719(7) 0.071(3) Uani 1 1 d . U . . .
H35A H 0.2799 0.6865 0.6853 0.085 Uiso 1 1 calc R U . . .
C36 C 0.3274(4) 0.7297(14) 0.6976(7) 0.067(3) Uani 1 1 d . U . . .
H36A H 0.3275 0.7758 0.7267 0.080 Uiso 1 1 calc R U . . .
C37 C 0.2424(4) 0.5689(14) 0.6179(8) 0.068(3) Uani 1 1 d . U . . .
C38 C 0.2380(4) 0.5181(13) 0.6638(8) 0.068(3) Uani 1 1 d . U . . .
H38A H 0.2550 0.4815 0.6873 0.082 Uiso 1 1 calc R U . . .
C39 C 0.2085(4) 0.5204(14) 0.6758(8) 0.071(3) Uani 1 1 d . U . . .
H39A H 0.2053 0.4832 0.7070 0.086 Uiso 1 1 calc R U . . .
C40 C 0.1827(4) 0.5772(14) 0.6426(8) 0.067(3) Uani 1 1 d . U . . .
C41 C 0.1875(4) 0.6273(14) 0.5959(8) 0.069(3) Uani 1 1 d . U . . .
H41A H 0.1705 0.6639 0.5725 0.083 Uiso 1 1 calc R U . . .
C42 C 0.2187(4) 0.6250(14) 0.5817(8) 0.070(3) Uani 1 1 d . U . . .
H42A H 0.2224 0.6597 0.5498 0.084 Uiso 1 1 calc R U . . .
C43 C 0.1496(4) 0.5764(15) 0.6525(8) 0.067(3) Uani 1 1 d . U . . .
C44 C 0.1495(5) 0.7435(14) 0.6746(12) 0.123(5) Uani 1 1 d D U . . .
H44A H 0.1535 0.7774 0.6408 0.147 Uiso 1 1 calc R U . . .
H44B H 0.1701 0.7339 0.7046 0.147 Uiso 1 1 calc R U . . .
C45 C 0.1279(4) 0.794(2) 0.6986(11) 0.122(5) Uani 1 1 d D U . . .
H45A H 0.1343 0.7890 0.7420 0.146 Uiso 1 1 calc R U . . .
H45B H 0.1281 0.8616 0.6881 0.146 Uiso 1 1 calc R U . . .
C46 C 0.0970(4) 0.7569(16) 0.6755(11) 0.111(4) Uani 1 1 d D U . . .
H46A H 0.0839 0.7992 0.6451 0.134 Uiso 1 1 calc R U . . .
H46B H 0.0861 0.7486 0.7070 0.134 Uiso 1 1 calc R U . . .
C47 C 0.1012(3) 0.6695(16) 0.6505(9) 0.095(4) Uani 1 1 d D U . . .
H47A H 0.0944 0.6198 0.6745 0.114 Uiso 1 1 calc R U . . .
C48 C 0.0814(4) 0.6530(17) 0.5829(8) 0.082(4) Uani 1 1 d . U . . .
C49 C -0.0233(4) 0.6440(12) 0.6306(7) 0.062(3) Uani 1 1 d . U . . .
C50 C 0.0111(5) 0.6156(14) 0.6704(8) 0.075(3) Uani 1 1 d . U . . .
H50A H 0.0276 0.6332 0.6497 0.090 Uiso 1 1 calc R U . . .
C51 C 0.0132(6) 0.5072(17) 0.6833(9) 0.090(3) Uani 1 1 d . U . . .
H51A H -0.0048 0.4736 0.6563 0.108 Uiso 1 1 calc R U . . .
H51B H 0.0336 0.4811 0.6790 0.108 Uiso 1 1 calc R U . . .
C52 C 0.0115(6) 0.4990(19) 0.7448(9) 0.100(4) Uani 1 1 d . U . . .
H52A H 0.0251 0.4464 0.7644 0.120 Uiso 1 1 calc R U . . .
H52B H -0.0109 0.4857 0.7453 0.120 Uiso 1 1 calc R U . . .
C53 C 0.0225(6) 0.5882(18) 0.7771(10) 0.100(5) Uani 1 1 d . U . . .
H53A H 0.0086 0.6055 0.8027 0.119 Uiso 1 1 calc R U . . .
H53B H 0.0449 0.5828 0.8015 0.119 Uiso 1 1 calc R U . . .
C54 C 0.0242(5) 0.750(2) 0.7353(9) 0.095(4) Uani 1 1 d . U . . .
C55 C 0.0434(4) 0.7961(15) 0.7914(8) 0.102(4) Uani 1 1 d D U . . .
C56 C 0.0350(5) 0.8852(15) 0.8114(9) 0.109(4) Uani 1 1 d D U . . .
H56A H 0.0151 0.9124 0.7910 0.130 Uiso 1 1 calc R U . . .
C57 C 0.0548(4) 0.9356(17) 0.8604(9) 0.112(4) Uani 1 1 d D U . . .
H57A H 0.0486 0.9948 0.8721 0.135 Uiso 1 1 calc R U . . .
C58 C 0.0845(5) 0.8920(16) 0.8909(10) 0.114(4) Uani 1 1 d D U . . .
C59 C 0.0933(5) 0.8005(16) 0.8751(10) 0.119(4) Uani 1 1 d D U . . .
H59A H 0.1122 0.7708 0.8976 0.143 Uiso 1 1 calc R U . . .
C60 C 0.0729(4) 0.7546(18) 0.8247(9) 0.114(4) Uani 1 1 d D U . . .
H60A H 0.0791 0.6954 0.8129 0.137 Uiso 1 1 calc R U . . .
C61 C 0.1361(5) 0.949(2) 0.9359(7) 0.112(4) Uani 1 1 d D U . . .
C62 C 0.1586(4) 0.954(2) 0.9930(8) 0.112(4) Uani 1 1 d D U . . .
H62A H 0.1507 0.9607 1.0266 0.135 Uiso 1 1 calc R U . . .
C63 C 0.1927(4) 0.951(2) 1.0010(8) 0.112(4) Uani 1 1 d D U . . .
H63A H 0.2069 0.9458 1.0393 0.134 Uiso 1 1 calc R U . . .
C64 C 0.2050(5) 0.955(2) 0.9503(7) 0.109(4) Uani 1 1 d D U . . .
C65 C 0.1826(4) 0.956(2) 0.8930(9) 0.118(4) Uani 1 1 d D U . . .
H65A H 0.1904 0.9624 0.8593 0.141 Uiso 1 1 calc R U . . .
C66 C 0.1487(5) 0.947(2) 0.8855(9) 0.118(4) Uani 1 1 d D U . . .
H66A H 0.1346 0.9405 0.8472 0.142 Uiso 1 1 calc R U . . .
C67 C 0.2415(6) 0.964(2) 0.9587(10) 0.106(5) Uani 1 1 d . U . . .
O19 O 0.2520(6) 1.042(2) 0.9438(13) 0.186(11) Uani 1 1 d . . . . .
C68 C 0.2467(7) 0.787(2) 0.9899(14) 0.124(6) Uani 1 1 d . U . . .
H68A H 0.2387 0.7850 1.0254 0.149 Uiso 1 1 calc R U . . .
H68B H 0.2296 0.7656 0.9555 0.149 Uiso 1 1 calc R U . . .
C69 C 0.2752(7) 0.730(2) 0.9976(14) 0.127(5) Uani 1 1 d . U . . .
H69A H 0.2764 0.7030 0.9598 0.153 Uiso 1 1 calc R U . . .
H69B H 0.2757 0.6791 1.0261 0.153 Uiso 1 1 calc R U . . .
C70 C 0.3013(7) 0.797(2) 1.0203(13) 0.127(5) Uani 1 1 d . U . . .
H70A H 0.3213 0.7724 1.0135 0.153 Uiso 1 1 calc R U . . .
H70B H 0.3047 0.8051 1.0632 0.153 Uiso 1 1 calc R U . . .
C71 C 0.2939(6) 0.891(2) 0.9906(13) 0.120(5) Uani 1 1 d . U . . .
H71A H 0.3033 0.9437 1.0178 0.144 Uiso 1 1 calc R U . . .
C72 C 0.3069(6) 0.888(2) 0.9394(14) 0.115(5) Uani 1 1 d D U . . .
C73 C 0.1453(6) 0.7218(19) 0.4234(10) 0.095(4) Uani 1 1 d . U . . .
C74 C 0.1783(5) 0.7421(11) 0.4075(7) 0.090(4) Uani 1 1 d D U . . .
H74A H 0.1968 0.7214 0.4405 0.108 Uiso 1 1 calc R U . . .
C75 C 0.1789(5) 0.8407(12) 0.4006(7) 0.097(4) Uani 1 1 d D U . . .
H75A H 0.1670 0.8721 0.4255 0.117 Uiso 1 1 calc R U . . .
H75B H 0.2013 0.8640 0.4118 0.117 Uiso 1 1 calc R U . . .
C76 C 0.1644(5) 0.8586(16) 0.3405(7) 0.103(4) Uani 1 1 d D U . . .
H76A H 0.1727 0.9173 0.3278 0.123 Uiso 1 1 calc R U . . .
H76B H 0.1408 0.8638 0.3329 0.123 Uiso 1 1 calc R U . . .
C77 C 0.1727(6) 0.7803(13) 0.3109(8) 0.104(5) Uani 1 1 d D U . . .
H77A H 0.1541 0.7602 0.2785 0.125 Uiso 1 1 calc R U . . .
H77B H 0.1906 0.7961 0.2942 0.125 Uiso 1 1 calc R U . . .
C78 C 0.1958(5) 0.6243(18) 0.3425(10) 0.097(4) Uani 1 1 d D U . . .
C79 C 0.2062(4) 0.5551(17) 0.3866(9) 0.097(3) Uani 1 1 d D U . . .
C80 C 0.2341(5) 0.500(2) 0.3938(10) 0.102(4) Uani 1 1 d . U . . .
H80A H 0.2472 0.5158 0.3690 0.123 Uiso 1 1 calc R U . . .
C81 C 0.2443(5) 0.429(2) 0.4308(10) 0.104(4) Uani 1 1 d . U . . .
H81A H 0.2646 0.4021 0.4336 0.124 Uiso 1 1 calc R U . . .
C82 C 0.2250(5) 0.394(2) 0.4661(10) 0.101(4) Uani 1 1 d . U . . .
C83 C 0.1973(5) 0.438(2) 0.4612(10) 0.099(4) Uani 1 1 d . U . . .
H83A H 0.1837 0.4169 0.4840 0.119 Uiso 1 1 calc R U . . .
C84 C 0.1876(5) 0.5152(19) 0.4228(9) 0.099(4) Uani 1 1 d D U . . .
H84A H 0.1674 0.5426 0.4207 0.119 Uiso 1 1 calc R U . . .
C85 C 0.2174(5) 0.2781(13) 0.5352(7) 0.123(5) Uani 1 1 d DG U . . .
C86 C 0.2072(5) 0.3302(11) 0.5781(8) 0.131(5) Uani 1 1 d DG U . . .
H86A H 0.2111 0.3958 0.5818 0.158 Uiso 1 1 calc R U . . .
C87 C 0.1912(5) 0.2844(13) 0.6154(7) 0.131(4) Uani 1 1 d DG U . . .
H87A H 0.1844 0.3192 0.6441 0.157 Uiso 1 1 calc R U . . .
C89 C 0.1854(5) 0.1864(13) 0.6099(7) 0.119(4) Uani 1 1 d DG U . . .
C90 C 0.1956(5) 0.1343(11) 0.5670(8) 0.126(4) Uani 1 1 d DG U . . .
H90A H 0.1918 0.0688 0.5633 0.151 Uiso 1 1 calc R U . . .
C88 C 0.2116(5) 0.1802(13) 0.5296(7) 0.128(5) Uani 1 1 d DG U . . .
H88A H 0.2184 0.1453 0.5009 0.153 Uiso 1 1 calc R U . . .
C91 C 0.1660(7) 0.132(2) 0.6444(11) 0.115(5) Uani 1 1 d . U . . .
C92 C 0.1806(10) 0.248(2) 0.7282(15) 0.185(8) Uani 1 1 d D U . . .
H92A H 0.2041 0.2398 0.7423 0.222 Uiso 1 1 calc R U . . .
H92B H 0.1759 0.3039 0.7025 0.222 Uiso 1 1 calc R U . . .
C93 C 0.1671(11) 0.257(3) 0.7759(15) 0.181(8) Uani 1 1 d D U . . .
H93A H 0.1825 0.2892 0.8088 0.217 Uiso 1 1 calc R U . . .
H93B H 0.1475 0.2962 0.7640 0.217 Uiso 1 1 calc R U . . .
C94 C 0.1594(10) 0.169(2) 0.7946(13) 0.173(8) Uani 1 1 d D U . . .
H94A H 0.1404 0.1710 0.8104 0.208 Uiso 1 1 calc R U . . .
H94B H 0.1776 0.1396 0.8238 0.208 Uiso 1 1 calc R U . . .
C95 C 0.1528(9) 0.124(2) 0.7394(11) 0.168(8) Uani 1 1 d D U . . .
H95A H 0.1627 0.0605 0.7467 0.201 Uiso 1 1 calc R U . . .
C96 C 0.1150(10) 0.107(3) 0.7106(16) 0.169(8) Uani 1 1 d D U . . .
C97 C 0.4516(5) 0.5970(13) 0.9690(8) 0.071(4) Uani 1 1 d . U . . .
H97A H 0.4428 0.6269 0.9971 0.085 Uiso 1 1 calc R U . . .
C98 C 0.4520(5) 0.4989(14) 0.9682(9) 0.080(3) Uani 1 1 d . U . . .
H98A H 0.4433 0.4638 0.9945 0.096 Uiso 1 1 calc R U . . .
C99 C 0.4669(5) 0.4483(11) 0.9235(9) 0.080(3) Uani 1 1 d D U . . .
C100 C 0.4764(4) 0.5077(14) 0.8866(8) 0.075(3) Uani 1 1 d . U . . .
H10A H 0.4849 0.4810 0.8572 0.090 Uiso 1 1 calc R U . . .
C101 C 0.4746(4) 0.6047(12) 0.8886(8) 0.068(3) Uani 1 1 d . U . . .
H10B H 0.4813 0.6405 0.8601 0.081 Uiso 1 1 calc R U . . .
C102 C 0.4691(5) 0.3495(11) 0.9191(9) 0.084(3) Uani 1 1 d D U . . .
H10C H 0.4819 0.3263 0.8953 0.100 Uiso 1 1 calc R U . . .
C103 C 0.4552(5) 0.2871(14) 0.9446(9) 0.085(3) Uani 1 1 d . U . . .
H10D H 0.4417 0.3084 0.9676 0.102 Uiso 1 1 calc R U . . .
C104 C 0.4598(5) 0.1783(15) 0.9388(8) 0.077(3) Uani 1 1 d . U . . .
C105 C 0.4360(5) 0.1266(13) 0.9527(9) 0.077(3) Uani 1 1 d . U . . .
H10E H 0.4183 0.1564 0.9617 0.092 Uiso 1 1 calc R U . . .
C106 C 0.4388(5) 0.0256(12) 0.9532(9) 0.074(4) Uani 1 1 d . U . . .
H10F H 0.4236 -0.0126 0.9645 0.089 Uiso 1 1 calc R U . . .
C107 C 0.4857(4) 0.0292(11) 0.9205(8) 0.065(3) Uani 1 1 d . U . . .
H10G H 0.5015 -0.0050 0.9082 0.078 Uiso 1 1 calc R U . . .
C108 C 0.4857(5) 0.1306(13) 0.9210(8) 0.074(3) Uani 1 1 d . U . . .
H10H H 0.5020 0.1651 0.9102 0.088 Uiso 1 1 calc R U . . .
C109 C 0.0749(5) 0.4513(14) 0.4091(9) 0.080(4) Uani 1 1 d . U . . .
H10I H 0.0633 0.4793 0.3732 0.096 Uiso 1 1 calc R U . . .
C110 C 0.0729(5) 0.3486(13) 0.4157(9) 0.078(3) Uani 1 1 d . U . . .
H11B H 0.0596 0.3119 0.3852 0.093 Uiso 1 1 calc R U . . .
C111 C 0.0910(4) 0.3059(13) 0.4682(8) 0.070(3) Uani 1 1 d . U . . .
C112 C 0.1090(5) 0.3709(13) 0.5112(9) 0.074(3) Uani 1 1 d . U . . .
H11C H 0.1213 0.3468 0.5478 0.089 Uiso 1 1 calc R U . . .
C113 C 0.1092(5) 0.4659(12) 0.5020(9) 0.072(3) Uani 1 1 d . U . . .
H11D H 0.1218 0.5036 0.5328 0.086 Uiso 1 1 calc R U . . .
C114 C 0.0907(5) 0.2050(13) 0.4789(9) 0.070(3) Uani 1 1 d . U . . .
H11E H 0.1025 0.1825 0.5163 0.084 Uiso 1 1 calc R U . . .
C115 C 0.0747(4) 0.1408(13) 0.4387(8) 0.068(3) Uani 1 1 d . U . . .
H11F H 0.0617 0.1644 0.4025 0.081 Uiso 1 1 calc R U . . .
C116 C 0.0758(5) 0.0394(14) 0.4463(8) 0.071(3) Uani 1 1 d . U . . .
C117 C 0.0558(5) -0.0167(14) 0.4020(9) 0.079(3) Uani 1 1 d . U . . .
H11G H 0.0404 0.0119 0.3704 0.095 Uiso 1 1 calc R U . . .
C118 C 0.0587(5) -0.1136(13) 0.4045(9) 0.078(4) Uani 1 1 d . U . . .
H11H H 0.0461 -0.1489 0.3725 0.094 Uiso 1 1 calc R U . . .
C119 C 0.0952(6) -0.1099(15) 0.4918(9) 0.085(4) Uani 1 1 d . U . . .
H11I H 0.1092 -0.1418 0.5238 0.102 Uiso 1 1 calc R U . . .
C120 C 0.0943(5) -0.0147(14) 0.4930(9) 0.080(3) Uani 1 1 d . U . . .
H12B H 0.1067 0.0168 0.5270 0.096 Uiso 1 1 calc R U . . .
N13 N -0.0041(7) 0.4726(9) 0.4944(16) 0.067(8) Uani 0.5 1 d G U P A -1
C123 C 0.0203(5) 0.4176(14) 0.5319(12) 0.057(5) Uani 0.5 1 d G U P A -1
H12C H 0.0374 0.4473 0.5600 0.069 Uiso 0.5 1 calc R U P A -1
C125 C 0.0192(4) 0.3184(13) 0.5274(8) 0.058(4) Uani 0.5 1 d G U P A -1
H12D H 0.0355 0.2816 0.5525 0.070 Uiso 0.5 1 calc R U P A -1
C124 C -0.0063(5) 0.2741(9) 0.4854(10) 0.059(4) Uani 0.5 1 d G U P A -1
C122 C -0.0307(4) 0.3291(14) 0.4480(8) 0.060(4) Uani 0.5 1 d G U P A -1
H12E H -0.0478 0.2995 0.4199 0.072 Uiso 0.5 1 calc R U P A -1
C121 C -0.0296(6) 0.4283(13) 0.4525(12) 0.057(5) Uani 0.5 1 d G U P A -1
H12F H -0.0459 0.4651 0.4274 0.068 Uiso 0.5 1 calc R U P A -1
C126 C -0.0059(8) 0.169(3) 0.4801(13) 0.062(4) Uani 0.5 1 d . U P A -1
H12G H -0.0180 0.1445 0.4433 0.075 Uiso 0.5 1 calc R U P A -1
C127 C 0.0080(8) 0.107(3) 0.5170(14) 0.063(4) Uani 0.5 1 d . U P A -1
H12J H 0.0213 0.1311 0.5528 0.076 Uiso 0.5 1 calc R U P A -1
C128 C 0.0068(7) -0.0010(9) 0.5128(10) 0.067(4) Uani 0.5 1 d G U P A -1
C129 C 0.0219(6) -0.0562(15) 0.5626(8) 0.073(5) Uani 0.5 1 d G U P A -1
H12H H 0.0338 -0.0268 0.5977 0.088 Uiso 0.5 1 calc R U P A -1
C130 C 0.0191(9) -0.1554(14) 0.5598(11) 0.075(6) Uani 0.5 1 d G U P A -1
H13A H 0.0292 -0.1923 0.5931 0.090 Uiso 0.5 1 calc R U P A -1
N14 N 0.0012(11) -0.1993(9) 0.5073(14) 0.047(6) Uani 0.5 1 d G U P A -1
C131 C -0.0139(8) -0.1442(14) 0.4576(10) 0.066(5) Uani 0.5 1 d G U P A -1
H13B H -0.0258 -0.1736 0.4224 0.079 Uiso 0.5 1 calc R U P A -1
C132 C -0.0111(6) -0.0450(14) 0.4603(8) 0.067(5) Uani 0.5 1 d G U P A -1
H13C H -0.0212 -0.0081 0.4270 0.080 Uiso 0.5 1 calc R U P A -1
N8 N 0.2589(4) 0.8868(18) 0.9797(8) 0.100(6) Uani 1 1 d . . . . .
N1 N 0.5777(3) 0.8576(9) 0.8780(6) 0.064(4) Uani 1 1 d D . . . .
N2 N 0.8289(2) 1.0750(10) 0.8299(6) 0.064(3) Uani 1 1 d D . . . .
N3 N 0.3892(3) 0.8438(14) 0.7225(7) 0.081(5) Uani 1 1 d . . . . .
N4 N 0.1344(3) 0.6567(12) 0.6565(7) 0.076(4) Uani 1 1 d D . . . .
N5 N 0.1817(4) 0.7081(11) 0.3531(5) 0.086(6) Uani 1 1 d D . . . .
N6 N 0.1661(5) 0.1673(16) 0.6976(9) 0.113(7) Uani 1 1 d D . . . .
N7 N 0.0198(4) 0.6574(13) 0.7298(5) 0.077(5) Uani 1 1 d . . . . .
N9 N 0.4630(3) 0.6528(9) 0.9318(5) 0.050(3) Uani 1 1 d . . . . .
N10 N 0.4634(3) -0.0131(11) 0.9374(6) 0.056(4) Uani 1 1 d . . . . .
N11 N 0.0931(4) 0.5087(12) 0.4530(7) 0.068(4) Uani 1 1 d . . . . .
N12 N 0.0777(3) -0.1595(10) 0.4485(7) 0.063(4) Uani 1 1 d . . . . .
O1 O 0.51963(19) 0.8057(9) 0.9597(4) 0.055(2) Uani 1 1 d . . . . .
O2 O 0.5738(2) 0.8129(9) 0.9943(4) 0.059(2) Uani 1 1 d . . . . .
O3 O 0.5607(3) 0.9996(9) 0.9090(5) 0.070(3) Uani 1 1 d . . . . .
O4 O 0.6851(3) 1.1737(11) 0.8530(8) 0.105(5) Uani 1 1 d . . . . .
O5 O 0.7997(3) 0.9512(10) 0.7805(5) 0.074(3) Uani 1 1 d . . . . .
O6 O 0.8621(3) 0.9086(13) 0.8788(7) 0.099(5) Uani 1 1 d D . . . .
O7 O 0.8843(3) 0.9017(11) 0.8049(6) 0.090(4) Uani 1 1 d D . . . .
H7A H 0.895(4) 0.850(10) 0.828(5) 0.134 Uiso 1 1 d D U . . .
O8 O 0.4192(2) 0.8331(9) 0.8488(5) 0.063(3) Uani 1 1 d . . . . .
O9 O 0.4670(2) 0.8345(7) 0.8301(5) 0.060(3) Uani 1 1 d . . . . .
O10 O 0.4123(3) 0.7081(11) 0.7162(6) 0.085(4) Uani 1 1 d . . . . .
O11 O 0.2715(3) 0.5615(12) 0.5973(6) 0.086(4) Uani 1 1 d . . . . .
O12 O 0.1351(3) 0.4942(12) 0.6486(6) 0.096(4) Uani 1 1 d . . . . .
O13 O 0.0959(3) 0.6737(11) 0.5463(5) 0.074(3) Uani 1 1 d . . . . .
O14 O 0.0502(2) 0.6331(11) 0.5744(5) 0.076(3) Uani 1 1 d . . . . .
O15 O -0.0279(2) 0.6412(9) 0.5752(4) 0.057(3) Uani 1 1 d . . . . .
O16 O -0.0457(3) 0.6602(10) 0.6545(4) 0.073(3) Uani 1 1 d . . . . .
O17 O 0.0158(3) 0.8069(11) 0.6904(5) 0.090(4) Uani 1 1 d . . . . .
O18 O 0.1052(3) 0.9470(13) 0.9350(6) 0.106(5) Uani 1 1 d . . . . .
O20 O 0.2883(4) 0.8791(15) 0.8842(8) 0.121(6) Uani 1 1 d D . . . .
O21 O 0.3384(4) 0.9022(17) 0.9501(8) 0.129(7) Uani 1 1 d D . . . .
H21C H 0.3436(17) 0.91(2) 0.9099(17) 0.194 Uiso 1 1 d D U . . .
O22 O 0.1452(4) 0.7226(13) 0.4763(7) 0.107(4) Uani 1 1 d . U . . .
O23 O 0.1233(3) 0.6901(12) 0.3855(8) 0.103(4) Uani 1 1 d . U . . .
O24 O 0.1993(4) 0.6116(15) 0.2902(6) 0.123(6) Uani 1 1 d . . . . .
O25 O 0.2380(4) 0.3226(16) 0.5027(8) 0.130(7) Uani 1 1 d . . . . .
O26 O 0.1537(6) 0.0593(16) 0.6255(11) 0.160(9) Uani 1 1 d . . . . .
O27 O 0.0991(6) 0.171(3) 0.6794(17) 0.250(19) Uani 1 1 d D . . . .
H27C H 0.075(3) 0.171(19) 0.679(19) 0.375 Uiso 1 1 d D U . . .
O28 O 0.1005(5) 0.0379(18) 0.7299(9) 0.149(8) Uani 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N9 2.260(13) . ?
Cd1 O1 2.310(8) . ?
Cd1 O8 2.344(10) . ?
Cd1 O1 2.362(9) 2_657 ?
Cd1 N10 2.408(15) 1_565 ?
Cd1 O9 2.477(10) . ?
Cd1 O2 2.567(9) 2_657 ?
Cd1 C25 2.733(16) . ?
Cd2 N13 2.295(13) . ?
Cd2 O14 2.352(10) . ?
Cd2 O14 2.352(10) 2_556 ?
Cd2 O15 2.353(9) . ?
Cd2 O15 2.353(9) 2_556 ?
Cd3 O13 2.281(10) . ?
Cd3 N11 2.334(17) . ?
Cd3 O23 2.352(16) . ?
Cd3 N12 2.355(13) 1_565 ?
Cd3 O15 2.443(10) 2_556 ?
Cd3 O16 2.474(10) 2_556 ?
Cd3 O22 2.506(16) . ?
C1 O1 1.261(15) . ?
C1 O2 1.269(17) . ?
C1 C2 1.57(2) . ?
C2 N1 1.388(7) . ?
C2 C3 1.391(7) . ?
C2 H2A 0.9800 . ?
C3 C4 1.388(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.383(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N1 1.391(7) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 O3 1.266(18) . ?
C6 N1 1.41(2) . ?
C6 C7 1.48(2) . ?
C7 C8 1.35(2) . ?
C7 C12 1.35(3) . ?
C8 C9 1.41(2) . ?
C8 H8A 0.9300 . ?
C9 C10 1.31(3) . ?
C9 H9A 0.9300 . ?
C10 O4 1.34(2) . ?
C10 C11 1.45(3) . ?
C11 C12 1.42(2) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C13 C14 1.36(3) . ?
C13 C18 1.39(2) . ?
C13 O4 1.396(19) . ?
C14 C15 1.36(2) . ?
C14 H14A 0.9300 . ?
C15 C16 1.39(2) . ?
C15 H15A 0.9300 . ?
C16 C17 1.36(3) . ?
C16 C19 1.548(19) . ?
C17 C18 1.43(2) . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9300 . ?
C19 O5 1.25(2) . ?
C19 N2 1.329(19) . ?
C20 N2 1.388(7) . ?
C20 C21 1.388(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.390(7) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.391(7) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 N2 1.392(6) . ?
C23 C24 1.53(2) . ?
C23 H23A 0.9800 . ?
C24 O6 1.19(2) . ?
C24 O7 1.322(19) . ?
C25 O9 1.238(17) . ?
C25 O8 1.252(18) . ?
C25 C26 1.54(2) . ?
C26 N3 1.51(2) . ?
C26 C27 1.56(3) . ?
C26 H26A 0.9800 . ?
C27 C28 1.47(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.50(3) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 N3 1.49(3) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 O10 1.15(2) . ?
C30 N3 1.35(3) . ?
C30 C31 1.45(2) . ?
C31 C36 1.42(2) . ?
C31 C32 1.42(3) . ?
C32 C33 1.37(2) . ?
C32 H32A 0.9300 . ?
C33 C34 1.38(2) . ?
C33 H33A 0.9300 . ?
C34 O11 1.34(2) . ?
C34 C35 1.41(2) . ?
C35 C36 1.42(2) . ?
C35 H35A 0.9300 . ?
C36 H36A 0.9300 . ?
C37 C38 1.33(2) . ?
C37 C42 1.37(2) . ?
C37 O11 1.446(19) . ?
C38 C39 1.35(2) . ?
C38 H38A 0.9300 . ?
C39 C40 1.40(2) . ?
C39 H39A 0.9300 . ?
C40 C41 1.35(2) . ?
C40 C43 1.49(2) . ?
C41 C42 1.45(2) . ?
C41 H41A 0.9300 . ?
C42 H42A 0.9300 . ?
C43 O12 1.29(2) . ?
C43 N4 1.31(2) . ?
C44 N4 1.383(7) . ?
C44 C45 1.388(7) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 C46 1.380(7) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.382(7) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 N4 1.390(7) . ?
C47 C48 1.58(3) . ?
C47 H47A 0.9800 . ?
C48 O13 1.21(2) . ?
C48 O14 1.319(19) . ?
C49 O16 1.241(18) . ?
C49 O15 1.244(17) . ?
C49 C50 1.56(2) . ?
C50 N7 1.45(2) . ?
C50 C51 1.54(3) . ?
C50 H50A 0.9800 . ?
C51 C52 1.45(3) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 C53 1.46(3) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 N7 1.44(2) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 O17 1.28(3) . ?
C54 N7 1.30(3) . ?
C54 C55 1.49(3) . ?
C55 C56 1.406(7) . ?
C55 C60 1.408(7) . ?
C56 C57 1.406(7) . ?
C56 H56A 0.9300 . ?
C57 C58 1.407(7) . ?
C57 H57A 0.9300 . ?
C58 O18 1.38(2) . ?
C58 C59 1.408(7) . ?
C59 C60 1.405(7) . ?
C59 H59A 0.9300 . ?
C60 H60A 0.9300 . ?
C61 O18 1.31(2) . ?
C61 C62 1.408(7) . ?
C61 C66 1.408(7) . ?
C62 C63 1.410(7) . ?
C62 H62A 0.9300 . ?
C63 C64 1.406(7) . ?
C63 H63A 0.9300 . ?
C64 C65 1.408(7) . ?
C64 C67 1.52(3) . ?
C65 C66 1.407(7) . ?
C65 H65A 0.9300 . ?
C66 H66A 0.9300 . ?
C67 O19 1.27(3) . ?
C67 N8 1.32(3) . ?
C68 C69 1.41(4) . ?
C68 N8 1.53(4) . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C69 C70 1.44(4) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C70 C71 1.47(4) . ?
C70 H70A 0.9700 . ?
C70 H70B 0.9700 . ?
C71 C72 1.44(3) . ?
C71 N8 1.44(3) . ?
C71 H71A 0.9800 . ?
C72 O21 1.31(3) . ?
C72 O20 1.31(3) . ?
C73 O23 1.18(3) . ?
C73 O22 1.23(3) . ?
C73 C74 1.57(3) . ?
C74 C75 1.388(7) . ?
C74 N5 1.389(7) . ?
C74 H74A 0.9800 . ?
C75 C76 1.383(7) . ?
C75 H75A 0.9700 . ?
C75 H75B 0.9700 . ?
C76 C77 1.386(7) . ?
C76 H76A 0.9700 . ?
C76 H76B 0.9700 . ?
C77 N5 1.384(7) . ?
C77 H77A 0.9700 . ?
C77 H77B 0.9700 . ?
C78 O24 1.27(3) . ?
C78 N5 1.37(3) . ?
C78 C79 1.388(7) . ?
C79 C80 1.38(3) . ?
C79 C84 1.409(7) . ?
C80 C81 1.30(3) . ?
C80 H80A 0.9300 . ?
C81 C82 1.39(3) . ?
C81 H81A 0.9300 . ?
C82 C83 1.31(3) . ?
C82 O25 1.33(3) . ?
C83 C84 1.39(3) . ?
C83 H83A 0.9300 . ?
C84 H84A 0.9300 . ?
C85 C86 1.3900 . ?
C85 C88 1.3900 . ?
C85 O25 1.439(18) . ?
C86 C87 1.3900 . ?
C86 H86A 0.9300 . ?
C87 C89 1.3900 . ?
C87 H87A 0.9300 . ?
C89 C90 1.3900 . ?
C89 C91 1.50(3) . ?
C90 C88 1.3900 . ?
C90 H90A 0.9300 . ?
C88 H88A 0.9300 . ?
C91 O26 1.17(3) . ?
C91 N6 1.33(3) . ?
C92 C93 1.379(7) . ?
C92 N6 1.382(7) . ?
C92 H92A 0.9700 . ?
C92 H92B 0.9700 . ?
C93 C94 1.378(7) . ?
C93 H93A 0.9700 . ?
C93 H93B 0.9700 . ?
C94 C95 1.380(7) . ?
C94 H94A 0.9700 . ?
C94 H94B 0.9700 . ?
C95 N6 1.381(7) . ?
C95 C96 1.58(5) . ?
C95 H95A 0.9800 . ?
C96 O27 1.23(4) . ?
C96 O28 1.29(4) . ?
C97 N9 1.35(2) . ?
C97 C98 1.37(3) . ?
C97 H97A 0.9300 . ?
C98 C99 1.52(3) . ?
C98 H98A 0.9300 . ?
C99 C100 1.33(3) . ?
C99 C102 1.389(7) . ?
C100 C101 1.36(2) . ?
C100 H10A 0.9300 . ?
C101 N9 1.40(2) . ?
C101 H10B 0.9300 . ?
C102 C103 1.28(3) . ?
C102 H10C 0.9300 . ?
C103 C104 1.54(3) . ?
C103 H10D 0.9300 . ?
C104 C105 1.35(3) . ?
C104 C108 1.44(3) . ?
C105 C106 1.42(2) . ?
C105 H10E 0.9300 . ?
C106 N10 1.31(2) . ?
C106 H10F 0.9300 . ?
C107 N10 1.265(19) . ?
C107 C108 1.42(2) . ?
C107 H10G 0.9300 . ?
C108 H10H 0.9300 . ?
C109 N11 1.36(2) . ?
C109 C110 1.45(3) . ?
C109 H10I 0.9300 . ?
C110 C111 1.38(3) . ?
C110 H11B 0.9300 . ?
C111 C112 1.41(3) . ?
C111 C114 1.43(2) . ?
C112 C113 1.34(2) . ?
C112 H11C 0.9300 . ?
C113 N11 1.30(2) . ?
C113 H11D 0.9300 . ?
C114 C115 1.34(2) . ?
C114 H11E 0.9300 . ?
C115 C116 1.43(3) . ?
C115 H11F 0.9300 . ?
C116 C120 1.38(3) . ?
C116 C117 1.38(3) . ?
C117 C118 1.36(3) . ?
C117 H11G 0.9300 . ?
C118 N12 1.29(2) . ?
C118 H11H 0.9300 . ?
C119 N12 1.28(2) . ?
C119 C120 1.33(3) . ?
C119 H11I 0.9300 . ?
C120 H12B 0.9300 . ?
N13 C123 1.3900 . ?
N13 C121 1.3900 . ?
C123 C125 1.3900 . ?
C123 H12C 0.9300 . ?
C125 C124 1.3900 . ?
C125 H12D 0.9300 . ?
C124 C122 1.3900 . ?
C124 C126 1.48(4) . ?
C122 C121 1.3900 . ?
C122 H12E 0.9300 . ?
C121 H12F 0.9300 . ?
C126 C127 1.24(4) . ?
C126 H12G 0.9300 . ?
C127 C128 1.51(4) . ?
C127 H12J 0.9300 . ?
C128 C129 1.3900 . ?
C128 C132 1.3900 . ?
C129 C130 1.3900 . ?
C129 H12H 0.9300 . ?
C130 N14 1.3900 . ?
C130 H13A 0.9300 . ?
N14 C131 1.3900 . ?
C131 C132 1.3900 . ?
C131 H13B 0.9300 . ?
C132 H13C 0.9300 . ?
N10 Cd1 2.408(15) 1_545 ?
N12 Cd3 2.355(13) 1_545 ?
O1 Cd1 2.362(9) 2_657 ?
O2 Cd1 2.567(9) 2_657 ?
O7 H7A 0.94(3) . ?
O15 Cd3 2.443(10) 2_556 ?
O16 Cd3 2.474(10) 2_556 ?
O21 H21C 1.02(3) . ?
O27 H27C 1.03(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N9 Cd1 O1 87.2(4) . . ?
N9 Cd1 O8 95.2(4) . . ?
O1 Cd1 O8 139.2(3) . . ?
N9 Cd1 O1 88.5(4) . 2_657 ?
O1 Cd1 O1 74.1(3) . 2_657 ?
O8 Cd1 O1 146.6(3) . 2_657 ?
N9 Cd1 N10 179.8(4) . 1_565 ?
O1 Cd1 N10 93.0(4) . 1_565 ?
O8 Cd1 N10 84.7(4) . 1_565 ?
O1 Cd1 N10 91.4(4) 2_657 1_565 ?
N9 Cd1 O9 95.0(4) . . ?
O1 Cd1 O9 85.4(3) . . ?
O8 Cd1 O9 53.8(3) . . ?
O1 Cd1 O9 159.0(3) 2_657 . ?
N10 Cd1 O9 85.2(4) 1_565 . ?
N9 Cd1 O2 90.5(4) . 2_657 ?
O1 Cd1 O2 127.6(3) . 2_657 ?
O8 Cd1 O2 93.2(3) . 2_657 ?
O1 Cd1 O2 53.5(3) 2_657 2_657 ?
N10 Cd1 O2 89.3(4) 1_565 2_657 ?
O9 Cd1 O2 146.9(3) . 2_657 ?
N9 Cd1 C25 98.6(5) . . ?
O1 Cd1 C25 112.1(4) . . ?
O8 Cd1 C25 27.2(4) . . ?
O1 Cd1 C25 170.7(5) 2_657 . ?
N10 Cd1 C25 81.5(5) 1_565 . ?
O9 Cd1 C25 26.9(4) . . ?
O2 Cd1 C25 120.0(4) 2_657 . ?
N13 Cd2 O14 93.5(7) . . ?
N13 Cd2 O14 84.2(7) . 2_556 ?
O14 Cd2 O14 177.8(7) . 2_556 ?
N13 Cd2 O15 91.4(11) . . ?
O14 Cd2 O15 89.8(3) . . ?
O14 Cd2 O15 90.3(3) 2_556 . ?
N13 Cd2 O15 91.9(11) . 2_556 ?
O14 Cd2 O15 90.3(3) . 2_556 ?
O14 Cd2 O15 89.8(3) 2_556 2_556 ?
O15 Cd2 O15 176.7(6) . 2_556 ?
O13 Cd3 N11 85.6(5) . . ?
O13 Cd3 O23 129.5(5) . . ?
N11 Cd3 O23 93.1(5) . . ?
O13 Cd3 N12 87.1(5) . 1_565 ?
N11 Cd3 N12 172.1(5) . 1_565 ?
O23 Cd3 N12 93.8(6) . 1_565 ?
O13 Cd3 O15 94.7(4) . 2_556 ?
N11 Cd3 O15 85.7(5) . 2_556 ?
O23 Cd3 O15 135.6(4) . 2_556 ?
N12 Cd3 O15 91.9(5) 1_565 2_556 ?
O13 Cd3 O16 147.4(4) . 2_556 ?
N11 Cd3 O16 92.3(5) . 2_556 ?
O23 Cd3 O16 83.1(4) . 2_556 ?
N12 Cd3 O16 92.3(5) 1_565 2_556 ?
O15 Cd3 O16 52.7(3) 2_556 2_556 ?
O13 Cd3 O22 79.0(4) . . ?
N11 Cd3 O22 98.6(6) . . ?
O23 Cd3 O22 51.2(5) . . ?
N12 Cd3 O22 82.9(5) 1_565 . ?
O15 Cd3 O22 172.0(5) 2_556 . ?
O16 Cd3 O22 133.4(4) 2_556 . ?
O1 C1 O2 123.1(13) . . ?
O1 C1 C2 117.8(12) . . ?
O2 C1 C2 117.7(12) . . ?
N1 C2 C3 103.7(13) . . ?
N1 C2 C1 112.7(12) . . ?
C3 C2 C1 112.2(16) . . ?
N1 C2 H2A 109.4 . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
C4 C3 C2 103.0(15) . . ?
C4 C3 H3A 111.2 . . ?
C2 C3 H3A 111.2 . . ?
C4 C3 H3B 111.2 . . ?
C2 C3 H3B 111.2 . . ?
H3A C3 H3B 109.1 . . ?
C5 C4 C3 111.6(16) . . ?
C5 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
C5 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
C4 C5 N1 98.9(14) . . ?
C4 C5 H5A 112.0 . . ?
N1 C5 H5A 112.0 . . ?
C4 C5 H5B 112.0 . . ?
N1 C5 H5B 112.0 . . ?
H5A C5 H5B 109.7 . . ?
O3 C6 N1 117.6(13) . . ?
O3 C6 C7 121.4(16) . . ?
N1 C6 C7 120.9(13) . . ?
C8 C7 C12 118.9(16) . . ?
C8 C7 C6 123.2(17) . . ?
C12 C7 C6 117.6(14) . . ?
C7 C8 C9 120.1(19) . . ?
C7 C8 H8A 119.9 . . ?
C9 C8 H8A 119.9 . . ?
C10 C9 C8 121.5(17) . . ?
C10 C9 H9A 119.3 . . ?
C8 C9 H9A 119.3 . . ?
C9 C10 O4 121.1(17) . . ?
C9 C10 C11 121.5(16) . . ?
O4 C10 C11 117.3(18) . . ?
C12 C11 C10 113.8(18) . . ?
C12 C11 H11A 123.1 . . ?
C10 C11 H11A 123.1 . . ?
C7 C12 C11 124.0(17) . . ?
C7 C12 H12A 118.0 . . ?
C11 C12 H12A 118.0 . . ?
C14 C13 C18 123.8(15) . . ?
C14 C13 O4 123.4(14) . . ?
C18 C13 O4 112.7(17) . . ?
C15 C14 C13 119.3(15) . . ?
C15 C14 H14A 120.4 . . ?
C13 C14 H14A 120.4 . . ?
C14 C15 C16 120.1(17) . . ?
C14 C15 H15A 119.9 . . ?
C16 C15 H15A 119.9 . . ?
C17 C16 C15 120.4(14) . . ?
C17 C16 C19 120.7(14) . . ?
C15 C16 C19 118.8(16) . . ?
C16 C17 C18 121.3(15) . . ?
C16 C17 H17A 119.3 . . ?
C18 C17 H17A 119.3 . . ?
C13 C18 C17 115.0(17) . . ?
C13 C18 H18A 122.5 . . ?
C17 C18 H18A 122.5 . . ?
O5 C19 N2 121.4(13) . . ?
O5 C19 C16 120.5(14) . . ?
N2 C19 C16 118.1(15) . . ?
N2 C20 C21 105.7(13) . . ?
N2 C20 H20A 110.6 . . ?
C21 C20 H20A 110.6 . . ?
N2 C20 H20B 110.6 . . ?
C21 C20 H20B 110.6 . . ?
H20A C20 H20B 108.7 . . ?
C20 C21 C22 107.0(13) . . ?
C20 C21 H21A 110.3 . . ?
C22 C21 H21A 110.3 . . ?
C20 C21 H21B 110.3 . . ?
C22 C21 H21B 110.3 . . ?
H21A C21 H21B 108.6 . . ?
C21 C22 C23 104.0(13) . . ?
C21 C22 H22A 111.0 . . ?
C23 C22 H22A 111.0 . . ?
C21 C22 H22B 111.0 . . ?
C23 C22 H22B 111.0 . . ?
H22A C22 H22B 109.0 . . ?
C22 C23 N2 107.2(11) . . ?
C22 C23 C24 111.7(14) . . ?
N2 C23 C24 109.5(13) . . ?
C22 C23 H23A 109.5 . . ?
N2 C23 H23A 109.5 . . ?
C24 C23 H23A 109.5 . . ?
O6 C24 O7 118.9(17) . . ?
O6 C24 C23 126.0(15) . . ?
O7 C24 C23 114.6(15) . . ?
O9 C25 O8 122.8(14) . . ?
O9 C25 C26 118.0(14) . . ?
O8 C25 C26 119.3(13) . . ?
O9 C25 Cd1 64.9(8) . . ?
O8 C25 Cd1 58.8(8) . . ?
C26 C25 Cd1 168.2(14) . . ?
N3 C26 C25 111.8(13) . . ?
N3 C26 C27 103.9(14) . . ?
C25 C26 C27 110.2(17) . . ?
N3 C26 H26A 110.2 . . ?
C25 C26 H26A 110.2 . . ?
C27 C26 H26A 110.2 . . ?
C28 C27 C26 103.4(18) . . ?
C28 C27 H27A 111.1 . . ?
C26 C27 H27A 111.1 . . ?
C28 C27 H27B 111.1 . . ?
C26 C27 H27B 111.1 . . ?
H27A C27 H27B 109.1 . . ?
C27 C28 C29 106.5(17) . . ?
C27 C28 H28A 110.4 . . ?
C29 C28 H28A 110.4 . . ?
C27 C28 H28B 110.4 . . ?
C29 C28 H28B 110.4 . . ?
H28A C28 H28B 108.6 . . ?
N3 C29 C28 103.2(16) . . ?
N3 C29 H29A 111.1 . . ?
C28 C29 H29A 111.1 . . ?
N3 C29 H29B 111.1 . . ?
C28 C29 H29B 111.1 . . ?
H29A C29 H29B 109.1 . . ?
O10 C30 N3 119.5(18) . . ?
O10 C30 C31 125(2) . . ?
N3 C30 C31 115.2(17) . . ?
C36 C31 C32 117.4(15) . . ?
C36 C31 C30 127.0(17) . . ?
C32 C31 C30 115.0(15) . . ?
C33 C32 C31 121.5(15) . . ?
C33 C32 H32A 119.3 . . ?
C31 C32 H32A 119.3 . . ?
C32 C33 C34 120.9(17) . . ?
C32 C33 H33A 119.5 . . ?
C34 C33 H33A 119.5 . . ?
O11 C34 C33 116.6(16) . . ?
O11 C34 C35 123.4(15) . . ?
C33 C34 C35 120.0(16) . . ?
C34 C35 C36 119.2(14) . . ?
C34 C35 H35A 120.4 . . ?
C36 C35 H35A 120.4 . . ?
C31 C36 C35 120.6(16) . . ?
C31 C36 H36A 119.7 . . ?
C35 C36 H36A 119.7 . . ?
C38 C37 C42 123.8(16) . . ?
C38 C37 O11 122.7(15) . . ?
C42 C37 O11 113.2(16) . . ?
C37 C38 C39 119.0(16) . . ?
C37 C38 H38A 120.5 . . ?
C39 C38 H38A 120.5 . . ?
C38 C39 C40 122.0(18) . . ?
C38 C39 H39A 119.0 . . ?
C40 C39 H39A 119.0 . . ?
C41 C40 C39 118.0(16) . . ?
C41 C40 C43 118.7(15) . . ?
C39 C40 C43 123.0(16) . . ?
C40 C41 C42 121.0(16) . . ?
C40 C41 H41A 119.5 . . ?
C42 C41 H41A 119.5 . . ?
C37 C42 C41 116.1(17) . . ?
C37 C42 H42A 122.0 . . ?
C41 C42 H42A 122.0 . . ?
O12 C43 N4 122.0(16) . . ?
O12 C43 C40 116.7(18) . . ?
N4 C43 C40 120.6(16) . . ?
N4 C44 C45 105.6(19) . . ?
N4 C44 H44A 110.6 . . ?
C45 C44 H44A 110.6 . . ?
N4 C44 H44B 110.6 . . ?
C45 C44 H44B 110.6 . . ?
H44A C44 H44B 108.8 . . ?
C46 C45 C44 108.2(18) . . ?
C46 C45 H45A 110.1 . . ?
C44 C45 H45A 110.1 . . ?
C46 C45 H45B 110.1 . . ?
C44 C45 H45B 110.1 . . ?
H45A C45 H45B 108.4 . . ?
C45 C46 C47 106.3(18) . . ?
C45 C46 H46A 110.5 . . ?
C47 C46 H46A 110.5 . . ?
C45 C46 H46B 110.5 . . ?
C47 C46 H46B 110.5 . . ?
H46A C46 H46B 108.7 . . ?
C46 C47 N4 108.3(16) . . ?
C46 C47 C48 116.6(19) . . ?
N4 C47 C48 109.5(13) . . ?
C46 C47 H47A 107.3 . . ?
N4 C47 H47A 107.3 . . ?
C48 C47 H47A 107.3 . . ?
O13 C48 O14 129.1(17) . . ?
O13 C48 C47 115.0(15) . . ?
O14 C48 C47 115.0(13) . . ?
O16 C49 O15 122.7(14) . . ?
O16 C49 C50 119.5(14) . . ?
O15 C49 C50 117.5(13) . . ?
N7 C50 C51 103.1(15) . . ?
N7 C50 C49 114.8(15) . . ?
C51 C50 C49 111.2(17) . . ?
N7 C50 H50A 109.2 . . ?
C51 C50 H50A 109.2 . . ?
C49 C50 H50A 109.2 . . ?
C52 C51 C50 104.6(19) . . ?
C52 C51 H51A 110.8 . . ?
C50 C51 H51A 110.8 . . ?
C52 C51 H51B 110.8 . . ?
C50 C51 H51B 110.8 . . ?
H51A C51 H51B 108.9 . . ?
C51 C52 C53 110(2) . . ?
C51 C52 H52A 109.7 . . ?
C53 C52 H52A 109.7 . . ?
C51 C52 H52B 109.7 . . ?
C53 C52 H52B 109.7 . . ?
H52A C52 H52B 108.2 . . ?
N7 C53 C52 103.5(17) . . ?
N7 C53 H53A 111.1 . . ?
C52 C53 H53A 111.1 . . ?
N7 C53 H53B 111.1 . . ?
C52 C53 H53B 111.1 . . ?
H53A C53 H53B 109.0 . . ?
O17 C54 N7 122.5(19) . . ?
O17 C54 C55 114(2) . . ?
N7 C54 C55 123(2) . . ?
C56 C55 C60 117.0(18) . . ?
C56 C55 C54 123.1(15) . . ?
C60 C55 C54 119.7(15) . . ?
C55 C56 C57 123.8(19) . . ?
C55 C56 H56A 118.1 . . ?
C57 C56 H56A 118.1 . . ?
C56 C57 C58 116.8(19) . . ?
C56 C57 H57A 121.6 . . ?
C58 C57 H57A 121.6 . . ?
O18 C58 C57 115.8(16) . . ?
O18 C58 C59 122.4(15) . . ?
C57 C58 C59 122(2) . . ?
C60 C59 C58 119.0(19) . . ?
C60 C59 H59A 120.5 . . ?
C58 C59 H59A 120.5 . . ?
C59 C60 C55 121.5(19) . . ?
C59 C60 H60A 119.2 . . ?
C55 C60 H60A 119.2 . . ?
O18 C61 C62 116.3(14) . . ?
O18 C61 C66 126.1(17) . . ?
C62 C61 C66 117.7(19) . . ?
C61 C62 C63 122.4(18) . . ?
C61 C62 H62A 118.8 . . ?
C63 C62 H62A 118.8 . . ?
C64 C63 C62 119.1(19) . . ?
C64 C63 H63A 120.4 . . ?
C62 C63 H63A 120.4 . . ?
C63 C64 C65 118.5(19) . . ?
C63 C64 C67 119.5(16) . . ?
C65 C64 C67 121.9(16) . . ?
C66 C65 C64 122(2) . . ?
C66 C65 H65A 119.2 . . ?
C64 C65 H65A 119.2 . . ?
C65 C66 C61 120(2) . . ?
C65 C66 H66A 120.0 . . ?
C61 C66 H66A 120.0 . . ?
O19 C67 N8 127(3) . . ?
O19 C67 C64 117(3) . . ?
N8 C67 C64 115(3) . . ?
C69 C68 N8 102(2) . . ?
C69 C68 H68A 111.3 . . ?
N8 C68 H68A 111.3 . . ?
C69 C68 H68B 111.3 . . ?
N8 C68 H68B 111.3 . . ?
H68A C68 H68B 109.2 . . ?
C68 C69 C70 104(3) . . ?
C68 C69 H69A 111.1 . . ?
C70 C69 H69A 111.1 . . ?
C68 C69 H69B 111.1 . . ?
C70 C69 H69B 111.1 . . ?
H69A C69 H69B 109.0 . . ?
C69 C70 C71 111(3) . . ?
C69 C70 H70A 109.4 . . ?
C71 C70 H70A 109.4 . . ?
C69 C70 H70B 109.4 . . ?
C71 C70 H70B 109.4 . . ?
H70A C70 H70B 108.0 . . ?
C72 C71 N8 118(2) . . ?
C72 C71 C70 106(3) . . ?
N8 C71 C70 97(2) . . ?
C72 C71 H71A 111.7 . . ?
N8 C71 H71A 111.7 . . ?
C70 C71 H71A 111.7 . . ?
O21 C72 O20 121(2) . . ?
O21 C72 C71 116(3) . . ?
O20 C72 C71 123(2) . . ?
O23 C73 O22 122(2) . . ?
O23 C73 C74 118(2) . . ?
O22 C73 C74 118.3(19) . . ?
C75 C74 N5 102.9(15) . . ?
C75 C74 C73 104.7(18) . . ?
N5 C74 C73 117.9(17) . . ?
C75 C74 H74A 110.3 . . ?
N5 C74 H74A 110.3 . . ?
C73 C74 H74A 110.3 . . ?
C76 C75 C74 106.2(17) . . ?
C76 C75 H75A 110.5 . . ?
C74 C75 H75A 110.5 . . ?
C76 C75 H75B 110.5 . . ?
C74 C75 H75B 110.5 . . ?
H75A C75 H75B 108.7 . . ?
C75 C76 C77 104.4(19) . . ?
C75 C76 H76A 110.9 . . ?
C77 C76 H76A 110.9 . . ?
C75 C76 H76B 110.9 . . ?
C77 C76 H76B 110.9 . . ?
H76A C76 H76B 108.9 . . ?
N5 C77 C76 106.6(17) . . ?
N5 C77 H77A 110.4 . . ?
C76 C77 H77A 110.4 . . ?
N5 C77 H77B 110.4 . . ?
C76 C77 H77B 110.4 . . ?
H77A C77 H77B 108.6 . . ?
O24 C78 N5 117.4(16) . . ?
O24 C78 C79 120(2) . . ?
N5 C78 C79 122(2) . . ?
C80 C79 C78 124.5(18) . . ?
C80 C79 C84 107.8(19) . . ?
C78 C79 C84 126.5(19) . . ?
C81 C80 C79 129(2) . . ?
C81 C80 H80A 115.7 . . ?
C79 C80 H80A 115.7 . . ?
C80 C81 C82 121(2) . . ?
C80 C81 H81A 119.7 . . ?
C82 C81 H81A 119.7 . . ?
C83 C82 O25 128(2) . . ?
C83 C82 C81 116(2) . . ?
O25 C82 C81 116(2) . . ?
C82 C83 C84 122(2) . . ?
C82 C83 H83A 119.2 . . ?
C84 C83 H83A 119.2 . . ?
C83 C84 C79 125(2) . . ?
C83 C84 H84A 117.5 . . ?
C79 C84 H84A 117.5 . . ?
C86 C85 C88 120.0 . . ?
C86 C85 O25 119.7(15) . . ?
C88 C85 O25 119.6(15) . . ?
C87 C86 C85 120.0 . . ?
C87 C86 H86A 120.0 . . ?
C85 C86 H86A 120.0 . . ?
C86 C87 C89 120.0 . . ?
C86 C87 H87A 120.0 . . ?
C89 C87 H87A 120.0 . . ?
C90 C89 C87 120.0 . . ?
C90 C89 C91 115.7(15) . . ?
C87 C89 C91 124.1(15) . . ?
C89 C90 C88 120.0 . . ?
C89 C90 H90A 120.0 . . ?
C88 C90 H90A 120.0 . . ?
C90 C88 C85 120.0 . . ?
C90 C88 H88A 120.0 . . ?
C85 C88 H88A 120.0 . . ?
O26 C91 N6 124(3) . . ?
O26 C91 C89 120(2) . . ?
N6 C91 C89 116(2) . . ?
C93 C92 N6 105(2) . . ?
C93 C92 H92A 110.7 . . ?
N6 C92 H92A 110.7 . . ?
C93 C92 H92B 110.7 . . ?
N6 C92 H92B 110.7 . . ?
H92A C92 H92B 108.8 . . ?
C94 C93 C92 111(3) . . ?
C94 C93 H93A 109.5 . . ?
C92 C93 H93A 109.5 . . ?
C94 C93 H93B 109.5 . . ?
C92 C93 H93B 109.5 . . ?
H93A C93 H93B 108.1 . . ?
C93 C94 C95 97(3) . . ?
C93 C94 H94A 112.4 . . ?
C95 C94 H94A 112.4 . . ?
C93 C94 H94B 112.4 . . ?
C95 C94 H94B 112.4 . . ?
H94A C94 H94B 110.0 . . ?
C94 C95 N6 116(2) . . ?
C94 C95 C96 113(3) . . ?
N6 C95 C96 109(3) . . ?
C94 C95 H95A 106.1 . . ?
N6 C95 H95A 106.1 . . ?
C96 C95 H95A 106.1 . . ?
O27 C96 O28 121(4) . . ?
O27 C96 C95 118(4) . . ?
O28 C96 C95 119(3) . . ?
N9 C97 C98 124.2(19) . . ?
N9 C97 H97A 117.9 . . ?
C98 C97 H97A 117.9 . . ?
C97 C98 C99 118.8(18) . . ?
C97 C98 H98A 120.6 . . ?
C99 C98 H98A 120.6 . . ?
C100 C99 C102 122(2) . . ?
C100 C99 C98 113.5(16) . . ?
C102 C99 C98 124(2) . . ?
C99 C100 C101 124.8(19) . . ?
C99 C100 H10A 117.6 . . ?
C101 C100 H10A 117.6 . . ?
C100 C101 N9 122.5(17) . . ?
C100 C101 H10B 118.7 . . ?
N9 C101 H10B 118.7 . . ?
C103 C102 C99 126(2) . . ?
C103 C102 H10C 116.8 . . ?
C99 C102 H10C 116.8 . . ?
C102 C103 C104 123(2) . . ?
C102 C103 H10D 118.5 . . ?
C104 C103 H10D 118.5 . . ?
C105 C104 C108 120.0(18) . . ?
C105 C104 C103 112.8(18) . . ?
C108 C104 C103 127.2(19) . . ?
C104 C105 C106 117.9(19) . . ?
C104 C105 H10E 121.1 . . ?
C106 C105 H10E 121.1 . . ?
N10 C106 C105 118.8(19) . . ?
N10 C106 H10F 120.6 . . ?
C105 C106 H10F 120.6 . . ?
N10 C107 C108 117.7(17) . . ?
N10 C107 H10G 121.1 . . ?
C108 C107 H10G 121.1 . . ?
C107 C108 C104 117.7(17) . . ?
C107 C108 H10H 121.1 . . ?
C104 C108 H10H 121.1 . . ?
N11 C109 C110 122.9(19) . . ?
N11 C109 H10I 118.6 . . ?
C110 C109 H10I 118.6 . . ?
C111 C110 C109 119.0(19) . . ?
C111 C110 H11B 120.5 . . ?
C109 C110 H11B 120.5 . . ?
C110 C111 C112 114.1(17) . . ?
C110 C111 C114 123.2(18) . . ?
C112 C111 C114 122.7(17) . . ?
C113 C112 C111 123.4(19) . . ?
C113 C112 H11C 118.3 . . ?
C111 C112 H11C 118.3 . . ?
N11 C113 C112 124.5(19) . . ?
N11 C113 H11D 117.8 . . ?
C112 C113 H11D 117.8 . . ?
C115 C114 C111 124.5(19) . . ?
C115 C114 H11E 117.8 . . ?
C111 C114 H11E 117.8 . . ?
C114 C115 C116 125.9(18) . . ?
C114 C115 H11F 117.0 . . ?
C116 C115 H11F 117.0 . . ?
C120 C116 C117 112.2(18) . . ?
C120 C116 C115 129.3(18) . . ?
C117 C116 C115 118.5(18) . . ?
C118 C117 C116 120.1(19) . . ?
C118 C117 H11G 120.0 . . ?
C116 C117 H11G 120.0 . . ?
N12 C118 C117 124.1(19) . . ?
N12 C118 H11H 117.9 . . ?
C117 C118 H11H 117.9 . . ?
N12 C119 C120 123(2) . . ?
N12 C119 H11I 118.5 . . ?
C120 C119 H11I 118.5 . . ?
C119 C120 C116 123(2) . . ?
C119 C120 H12B 118.5 . . ?
C116 C120 H12B 118.5 . . ?
C123 N13 C121 120.0 . . ?
C123 N13 Cd2 118.9(12) . . ?
C121 N13 Cd2 121.1(12) . . ?
C125 C123 N13 120.0 . . ?
C125 C123 H12C 120.0 . . ?
N13 C123 H12C 120.0 . . ?
C123 C125 C124 120.0 . . ?
C123 C125 H12D 120.0 . . ?
C124 C125 H12D 120.0 . . ?
C122 C124 C125 120.0 . . ?
C122 C124 C126 121.4(16) . . ?
C125 C124 C126 118.6(16) . . ?
C124 C122 C121 120.0 . . ?
C124 C122 H12E 120.0 . . ?
C121 C122 H12E 120.0 . . ?
C122 C121 N13 120.0 . . ?
C122 C121 H12F 120.0 . . ?
N13 C121 H12F 120.0 . . ?
C127 C126 C124 130(3) . . ?
C127 C126 H12G 114.9 . . ?
C124 C126 H12G 114.9 . . ?
C126 C127 C128 130(3) . . ?
C126 C127 H12J 114.9 . . ?
C128 C127 H12J 114.9 . . ?
C129 C128 C132 120.0 . . ?
C129 C128 C127 120.0(17) . . ?
C132 C128 C127 119.9(17) . . ?
C128 C129 C130 120.0 . . ?
C128 C129 H12H 120.0 . . ?
C130 C129 H12H 120.0 . . ?
C129 C130 N14 120.0 . . ?
C129 C130 H13A 120.0 . . ?
N14 C130 H13A 120.0 . . ?
C131 N14 C130 120.0 . . ?
N14 C131 C132 120.0 . . ?
N14 C131 H13B 120.0 . . ?
C132 C131 H13B 120.0 . . ?
C131 C132 C128 120.0 . . ?
C131 C132 H13C 120.0 . . ?
C128 C132 H13C 120.0 . . ?
C67 N8 C71 119(2) . . ?
C67 N8 C68 128(2) . . ?
C71 N8 C68 113(2) . . ?
C2 N1 C5 113.8(13) . . ?
C2 N1 C6 122.3(12) . . ?
C5 N1 C6 122.7(12) . . ?
C19 N2 C20 128.3(12) . . ?
C19 N2 C23 123.0(12) . . ?
C20 N2 C23 107.6(11) . . ?
C30 N3 C29 131.0(17) . . ?
C30 N3 C26 118.5(15) . . ?
C29 N3 C26 109.3(17) . . ?
C43 N4 C44 125.1(14) . . ?
C43 N4 C47 127.5(16) . . ?
C44 N4 C47 107.0(16) . . ?
C78 N5 C77 123.3(15) . . ?
C78 N5 C74 127.8(15) . . ?
C77 N5 C74 108.3(16) . . ?
C91 N6 C95 126(2) . . ?
C91 N6 C92 132(2) . . ?
C95 N6 C92 102(2) . . ?
C54 N7 C53 127.5(17) . . ?
C54 N7 C50 119.0(16) . . ?
C53 N7 C50 113.5(18) . . ?
C97 N9 C101 115.9(15) . . ?
C97 N9 Cd1 124.1(11) . . ?
C101 N9 Cd1 120.0(10) . . ?
C107 N10 C106 127.7(18) . . ?
C107 N10 Cd1 117.0(11) . 1_545 ?
C106 N10 Cd1 115.2(12) . 1_545 ?
C113 N11 C109 116.1(17) . . ?
C113 N11 Cd3 123.7(12) . . ?
C109 N11 Cd3 119.2(14) . . ?
C119 N12 C118 117.3(17) . . ?
C119 N12 Cd3 120.1(13) . 1_545 ?
C118 N12 Cd3 122.0(12) . 1_545 ?
C1 O1 Cd1 156.0(10) . . ?
C1 O1 Cd1 96.1(8) . 2_657 ?
Cd1 O1 Cd1 105.6(3) . 2_657 ?
C1 O2 Cd1 86.5(7) . 2_657 ?
C10 O4 C13 119.9(16) . . ?
C24 O7 H7A 109(3) . . ?
C25 O8 Cd1 94.0(8) . . ?
C25 O9 Cd1 88.2(9) . . ?
C34 O11 C37 119.0(14) . . ?
C48 O13 Cd3 137.7(12) . . ?
C48 O14 Cd2 141.5(11) . . ?
C49 O15 Cd2 142.5(10) . . ?
C49 O15 Cd3 93.0(9) . 2_556 ?
Cd2 O15 Cd3 123.8(4) . 2_556 ?
C49 O16 Cd3 91.6(9) . 2_556 ?
C61 O18 C58 117.4(15) . . ?
C72 O21 H21C 108(3) . . ?
C73 O22 Cd3 88.5(14) . . ?
C73 O23 Cd3 97.2(15) . . ?
C82 O25 C85 116.8(17) . . ?
C96 O27 H27C 113(4) . . ?

_refine_diff_density_max         1.097
_refine_diff_density_min         -1.779
_refine_diff_density_rms         0.120

_shelxl_version_number           2014-3

