# Electronic Supplementary Material (ESI) for Materials Chemistry Frontiers.
# This journal is © the Partner Organisations 2023

####################################################################### 
# 
# 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(2)*TBACl(2)
_audit_block_doi                 10.5517/cc7709r
_database_code_depnum_ccdc_archive 'CCDC 215273'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/b307849c 2003
_audit_update_record             
;
2003-07-14 deposited with the CCDC.	2023-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H26 Cl N2 O6 U * C16 H36 N'
_chemical_formula_sum            'C50 H62 Cl1 N3 O6 U'
_chemical_formula_weight         1074.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   13.3226(1)
_cell_length_b                   18.2936(1)
_cell_length_c                   20.3692(2)
_cell_angle_alpha                94.6846(3)
_cell_angle_beta                 104.4632(3)
_cell_angle_gamma                91.9727(3)
_cell_volume                     4783.22(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173.0(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2160
_exptl_absorpt_coefficient_mu    3.499
_exptl_absorpt_correction_type   platmulabs
_exptl_absorpt_correction_T_min  0.2736
_exptl_absorpt_correction_T_max  0.3350
_exptl_absorpt_process_details   
'R. H. Blessing, Acta Crystallogr.A 1995, 51, 33'


_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'nonius kappa ccd'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            56033
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         28.28
_reflns_number_total             23316
_reflns_number_gt                17779
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       collect
_computing_cell_refinement       denzo-smn
_computing_data_reduction        denzo-smn
_computing_structure_solution    shelxs-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0109P)²+7.1894P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         23316
_refine_ls_number_parameters     1107
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0678
_refine_ls_wR_factor_gt          0.0609
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C2A C 0.4826(3) 0.6474(2) 0.9798(2) 0.0377(10) Uani 1 1 d . . .
H2A H 0.5116 0.6562 1.0275 0.045 Uiso 1 1 calc R . .
C2B C 0.0039(3) 0.14445(19) 0.97634(19) 0.0297(8) Uani 1 1 d . . .
H2B H 0.0117 0.1524 1.0241 0.036 Uiso 1 1 calc R . .
C3A C 0.5339(3) 0.6854(2) 0.9373(2) 0.0381(10) Uani 1 1 d . . .
C3B C -0.0776(3) 0.18194(19) 0.9344(2) 0.0305(8) Uani 1 1 d . . .
C4A C 0.5095(3) 0.66839(19) 0.8659(2) 0.0358(9) Uani 1 1 d . . .
C4B C -0.1059(3) 0.16851(18) 0.86248(19) 0.0280(8) Uani 1 1 d . . .
C5A C 0.5656(3) 0.7078(2) 0.8280(3) 0.0420(11) Uani 1 1 d . . .
C5B C -0.1872(3) 0.20939(19) 0.8257(2) 0.0324(9) Uani 1 1 d . . .
C6A C 0.6408(3) 0.7621(2) 0.8612(3) 0.0512(13) Uani 1 1 d . . .
H6A H 0.6767 0.7891 0.8354 0.061 Uiso 1 1 calc R . .
C6B C -0.2351(3) 0.2597(2) 0.8594(2) 0.0410(10) Uani 1 1 d . . .
H6B H -0.2877 0.2874 0.8338 0.049 Uiso 1 1 calc R . .
C7A C 0.6647(3) 0.7776(2) 0.9319(3) 0.0569(14) Uani 1 1 d . . .
H7A H 0.7171 0.8143 0.9540 0.068 Uiso 1 1 calc R . .
C7B C -0.2084(3) 0.2711(2) 0.9301(3) 0.0439(11) Uani 1 1 d . . .
H7B H -0.2434 0.3055 0.9525 0.053 Uiso 1 1 calc R . .
C8A C 0.6123(3) 0.7395(2) 0.9687(3) 0.0482(12) Uani 1 1 d . . .
H8A H 0.6290 0.7498 1.0168 0.058 Uiso 1 1 calc R . .
C8B C -0.1315(3) 0.2325(2) 0.9670(2) 0.0388(9) Uani 1 1 d . . .
H8B H -0.1140 0.2398 1.0153 0.047 Uiso 1 1 calc R . .
C11A C 0.5438(3) 0.6241(2) 0.7275(2) 0.0444(11) Uani 1 1 d . . .
H11A H 0.4818 0.5945 0.7306 0.053 Uiso 1 1 calc R . .
H11B H 0.6065 0.6004 0.7516 0.053 Uiso 1 1 calc R . .
C11B C -0.2453(3) 0.1318(2) 0.7210(2) 0.0358(9) Uani 1 1 d . . .
H11C H -0.2850 0.1036 0.7466 0.043 Uiso 1 1 calc R . .
H11D H -0.1833 0.1048 0.7177 0.043 Uiso 1 1 calc R . .
C12A C 0.5440(4) 0.6285(3) 0.6546(3) 0.0494(12) Uani 1 1 d . . .
C12B C -0.3118(3) 0.1403(2) 0.6508(2) 0.0365(9) Uani 1 1 d . . .
C13A C 0.6103(4) 0.6787(3) 0.6365(3) 0.0675(15) Uani 1 1 d . . .
H13A H 0.6544 0.7127 0.6700 0.081 Uiso 1 1 calc R . .
C13B C -0.3832(3) 0.1944(2) 0.6396(2) 0.0456(11) Uani 1 1 d . . .
H13B H -0.3899 0.2276 0.6764 0.055 Uiso 1 1 calc R . .
C14A C 0.6112(6) 0.6784(4) 0.5675(4) 0.088(2) Uani 1 1 d . . .
H14A H 0.6569 0.7118 0.5542 0.106 Uiso 1 1 calc R . .
C14B C -0.4449(4) 0.1997(3) 0.5743(3) 0.0629(15) Uani 1 1 d . . .
H14B H -0.4935 0.2369 0.5665 0.075 Uiso 1 1 calc R . .
C15A C 0.5458(7) 0.6299(5) 0.5197(4) 0.095(2) Uani 1 1 d . . .
H15A H 0.5474 0.6298 0.4733 0.113 Uiso 1 1 calc R . .
C15B C -0.4360(5) 0.1518(4) 0.5211(3) 0.0822(19) Uani 1 1 d . . .
H15B H -0.4792 0.1553 0.4768 0.099 Uiso 1 1 calc R . .
C16A C 0.4784(6) 0.5815(4) 0.5371(3) 0.085(2) Uani 1 1 d . . .
H16A H 0.4326 0.5489 0.5032 0.101 Uiso 1 1 calc R . .
C16B C -0.3654(5) 0.0987(4) 0.5314(3) 0.0838(19) Uani 1 1 d . . .
H16B H -0.3589 0.0658 0.4943 0.101 Uiso 1 1 calc R . .
C17A C 0.4779(4) 0.5807(3) 0.6050(3) 0.0631(14) Uani 1 1 d . . .
H17A H 0.4318 0.5470 0.6177 0.076 Uiso 1 1 calc R . .
C17B C -0.3028(4) 0.0933(3) 0.5968(3) 0.0611(14) Uani 1 1 d . . .
H17B H -0.2535 0.0566 0.6039 0.073 Uiso 1 1 calc R . .
C18A C -0.0709(4) 0.5989(2) 0.5863(2) 0.0509(12) Uani 1 1 d . . .
C18B C 0.2290(3) 0.0944(2) 0.58739(19) 0.0329(8) Uani 1 1 d . . .
C19A C -0.1132(5) 0.6579(3) 0.5554(3) 0.0663(15) Uani 1 1 d . . .
H19A H -0.1015 0.7050 0.5802 0.080 Uiso 1 1 calc R . .
C19B C 0.1569(3) 0.0380(2) 0.5553(2) 0.0399(10) Uani 1 1 d . . .
H19B H 0.1245 0.0088 0.5816 0.048 Uiso 1 1 calc R . .
C20A C -0.1733(5) 0.6510(4) 0.4880(3) 0.0821(19) Uani 1 1 d . . .
H20A H -0.2016 0.6929 0.4673 0.099 Uiso 1 1 calc R . .
C20B C 0.1319(3) 0.0240(2) 0.4853(2) 0.0473(11) Uani 1 1 d . . .
H20B H 0.0833 -0.0153 0.4639 0.057 Uiso 1 1 calc R . .
C21A C -0.1908(5) 0.5838(4) 0.4527(3) 0.081(2) Uani 1 1 d . . .
H21A H -0.2324 0.5783 0.4071 0.098 Uiso 1 1 calc R . .
C21B C 0.1760(4) 0.0659(3) 0.4465(2) 0.0498(12) Uani 1 1 d . . .
H21B H 0.1578 0.0564 0.3984 0.060 Uiso 1 1 calc R . .
C22A C -0.1499(7) 0.5259(3) 0.4817(3) 0.125(4) Uani 1 1 d . . .
H22A H -0.1629 0.4789 0.4567 0.150 Uiso 1 1 calc R . .
C22B C 0.2472(4) 0.1221(3) 0.4780(3) 0.0616(14) Uani 1 1 d . . .
H22B H 0.2784 0.1517 0.4515 0.074 Uiso 1 1 calc R . .
C23A C -0.0876(7) 0.5327(3) 0.5488(3) 0.121(3) Uani 1 1 d . . .
H23A H -0.0569 0.4907 0.5681 0.145 Uiso 1 1 calc R . .
C23B C 0.2737(4) 0.1356(3) 0.5481(2) 0.0546(12) Uani 1 1 d . . .
H23B H 0.3236 0.1742 0.5693 0.066 Uiso 1 1 calc R . .
C24A C -0.0114(4) 0.6067(3) 0.6599(2) 0.0574(13) Uani 1 1 d . . .
H24A H 0.0573 0.5857 0.6650 0.069 Uiso 1 1 calc R . .
H24B H -0.0006 0.6592 0.6775 0.069 Uiso 1 1 calc R . .
C24B C 0.2558(3) 0.1120(3) 0.6632(2) 0.0440(10) Uani 1 1 d . . .
H24C H 0.2792 0.1645 0.6751 0.053 Uiso 1 1 calc R . .
H24D H 0.1941 0.1026 0.6807 0.053 Uiso 1 1 calc R . .
C26A C -0.0627(3) 0.5948(2) 0.7629(2) 0.0319(8) Uani 1 1 d . . .
C26B C 0.3844(3) 0.08872(18) 0.76050(18) 0.0270(8) Uani 1 1 d . . .
C27A C 0.0272(3) 0.58298(18) 0.81489(19) 0.0281(8) Uani 1 1 d . . .
C27B C 0.3319(3) 0.07783(17) 0.81219(17) 0.0234(7) Uani 1 1 d . . .
C28A C 0.0248(3) 0.6067(2) 0.88316(19) 0.0313(8) Uani 1 1 d . . .
C28B C 0.3882(3) 0.09967(18) 0.88042(19) 0.0274(8) Uani 1 1 d . . .
C29A C -0.0620(3) 0.6404(2) 0.8961(2) 0.0398(10) Uani 1 1 d . . .
H29A H -0.0625 0.6552 0.9418 0.048 Uiso 1 1 calc R . .
C29B C 0.4899(3) 0.1317(2) 0.8949(2) 0.0329(8) Uani 1 1 d . . .
H29B H 0.5262 0.1460 0.9408 0.040 Uiso 1 1 calc R . .
C30A C -0.1462(3) 0.6525(2) 0.8445(2) 0.0472(11) Uani 1 1 d . . .
H30A H -0.2039 0.6765 0.8540 0.057 Uiso 1 1 calc R . .
C30B C 0.5369(3) 0.1423(2) 0.8436(2) 0.0390(10) Uani 1 1 d . . .
H30B H 0.6052 0.1645 0.8539 0.047 Uiso 1 1 calc R . .
C31A C -0.1453(3) 0.6289(2) 0.7782(2) 0.0427(10) Uani 1 1 d . . .
H31A H -0.2037 0.6366 0.7422 0.051 Uiso 1 1 calc R . .
C31B C 0.4842(3) 0.1202(2) 0.7760(2) 0.0341(9) Uani 1 1 d . . .
H31B H 0.5174 0.1269 0.7405 0.041 Uiso 1 1 calc R . .
C33A C 0.1060(3) 0.59148(19) 0.94079(19) 0.0312(8) Uani 1 1 d . . .
H33A H 0.0909 0.5973 0.9840 0.037 Uiso 1 1 calc R . .
C33B C 0.3479(3) 0.08592(18) 0.93775(18) 0.0269(8) Uani 1 1 d . . .
H33B H 0.3959 0.0921 0.9812 0.032 Uiso 1 1 calc R . .
C35A C 0.2627(3) 0.55130(19) 1.00188(18) 0.0319(9) Uani 1 1 d . . .
C35B C 0.2320(3) 0.04786(18) 0.99854(17) 0.0269(8) Uani 1 1 d . . .
C36A C 0.2266(4) 0.5179(2) 1.0511(2) 0.0419(10) Uani 1 1 d . . .
H36A H 0.1543 0.5074 1.0446 0.050 Uiso 1 1 calc R . .
C36B C 0.3016(3) 0.0141(2) 1.04824(19) 0.0345(9) Uani 1 1 d . . .
H36B H 0.3671 0.0017 1.0413 0.041 Uiso 1 1 calc R . .
C37A C 0.2965(4) 0.4999(2) 1.1102(2) 0.0467(11) Uani 1 1 d . . .
H37A H 0.2715 0.4782 1.1443 0.056 Uiso 1 1 calc R . .
C37B C 0.2762(3) -0.0017(2) 1.1074(2) 0.0387(10) Uani 1 1 d . . .
H37B H 0.3249 -0.0236 1.1415 0.046 Uiso 1 1 calc R . .
C38A C 0.4014(4) 0.5134(2) 1.1189(2) 0.0498(12) Uani 1 1 d . . .
H38A H 0.4486 0.5005 1.1589 0.060 Uiso 1 1 calc R . .
C38B C 0.1807(3) 0.0142(2) 1.11716(19) 0.0379(10) Uani 1 1 d . . .
H38B H 0.1632 0.0026 1.1577 0.045 Uiso 1 1 calc R . .
C39A C 0.4385(3) 0.5457(2) 1.0702(2) 0.0421(10) Uani 1 1 d . . .
H39A H 0.5113 0.5537 1.0762 0.051 Uiso 1 1 calc R . .
C39B C 0.1098(3) 0.0472(2) 1.06814(19) 0.0343(9) Uani 1 1 d . . .
H39B H 0.0436 0.0576 1.0749 0.041 Uiso 1 1 calc R . .
C40A C 0.3696(3) 0.56677(19) 1.01171(18) 0.0321(9) Uani 1 1 d . . .
C40B C 0.1356(3) 0.06510(18) 1.00878(17) 0.0263(8) Uani 1 1 d . . .
C42A C 0.3727(3) 0.89014(19) 0.6970(2) 0.0337(9) Uani 1 1 d . . .
H42A H 0.3434 0.8953 0.6480 0.040 Uiso 1 1 calc R . .
H42B H 0.3704 0.9384 0.7222 0.040 Uiso 1 1 calc R . .
C42B C -0.0051(3) 0.25871(18) 0.68303(19) 0.0311(8) Uani 1 1 d . . .
H42C H 0.0386 0.2226 0.7087 0.037 Uiso 1 1 calc R . .
H42D H -0.0785 0.2437 0.6798 0.037 Uiso 1 1 calc R . .
C43A C 0.4848(3) 0.8719(2) 0.7073(2) 0.0394(10) Uani 1 1 d . . .
H43A H 0.4887 0.8247 0.6809 0.047 Uiso 1 1 calc R . .
H43B H 0.5152 0.8662 0.7561 0.047 Uiso 1 1 calc R . .
C43B C 0.0109(3) 0.2552(2) 0.6115(2) 0.0356(9) Uani 1 1 d . . .
H43C H 0.0862 0.2567 0.6141 0.043 Uiso 1 1 calc R . .
H43D H -0.0185 0.2984 0.5889 0.043 Uiso 1 1 calc R . .
C44A C 0.5472(4) 0.9317(2) 0.6848(3) 0.0507(12) Uani 1 1 d . . .
H44A H 0.5164 0.9375 0.6361 0.061 Uiso 1 1 calc R . .
H44B H 0.5429 0.9789 0.7112 0.061 Uiso 1 1 calc R . .
C44B C -0.0414(4) 0.1849(2) 0.5695(2) 0.0410(10) Uani 1 1 d . . .
H44C H -0.0132 0.1418 0.5927 0.049 Uiso 1 1 calc R . .
H44D H -0.1169 0.1840 0.5659 0.049 Uiso 1 1 calc R . .
C45A C 0.6600(4) 0.9147(3) 0.6946(3) 0.0626(14) Uani 1 1 d . . .
H45A H 0.6911 0.9096 0.7428 0.094 Uiso 1 1 calc R . .
H45B H 0.6972 0.9548 0.6798 0.094 Uiso 1 1 calc R . .
H45C H 0.6647 0.8688 0.6675 0.094 Uiso 1 1 calc R . .
C45B C -0.0233(4) 0.1800(2) 0.4984(2) 0.0522(12) Uani 1 1 d . . .
H45D H -0.0494 0.2233 0.4758 0.078 Uiso 1 1 calc R . .
H45E H -0.0601 0.1356 0.4719 0.078 Uiso 1 1 calc R . .
H45F H 0.0512 0.1779 0.5018 0.078 Uiso 1 1 calc R . .
C46A C 0.2999(3) 0.75939(19) 0.68096(19) 0.0330(9) Uani 1 1 d . . .
H46A H 0.3665 0.7368 0.6988 0.040 Uiso 1 1 calc R . .
H46B H 0.2443 0.7282 0.6909 0.040 Uiso 1 1 calc R . .
C46B C 0.1243(3) 0.36669(19) 0.71890(19) 0.0290(8) Uani 1 1 d . . .
H46C H 0.1338 0.4175 0.7411 0.035 Uiso 1 1 calc R . .
H46D H 0.1223 0.3695 0.6703 0.035 Uiso 1 1 calc R . .
C47A C 0.2808(4) 0.7589(2) 0.6041(2) 0.0470(11) Uani 1 1 d . . .
H47A H 0.2262 0.7931 0.5872 0.056 Uiso 1 1 calc R . .
H47B H 0.3452 0.7765 0.5930 0.056 Uiso 1 1 calc R . .
C47B C 0.2184(3) 0.3246(2) 0.7513(2) 0.0339(9) Uani 1 1 d . . .
H47C H 0.2351 0.3349 0.8014 0.041 Uiso 1 1 calc R . .
H47D H 0.2016 0.2712 0.7400 0.041 Uiso 1 1 calc R . .
C48A C 0.2480(4) 0.6840(2) 0.5688(2) 0.0534(12) Uani 1 1 d . . .
H48A H 0.1786 0.6699 0.5746 0.064 Uiso 1 1 calc R . .
H48B H 0.2970 0.6487 0.5913 0.064 Uiso 1 1 calc R . .
C48B C 0.3119(3) 0.3466(2) 0.7260(2) 0.0418(10) Uani 1 1 d . . .
H48C H 0.3194 0.4008 0.7284 0.050 Uiso 1 1 calc R . .
H48D H 0.3002 0.3273 0.6776 0.050 Uiso 1 1 calc R . .
C49A C 0.2432(4) 0.6767(3) 0.4944(2) 0.0572(13) Uani 1 1 d . . .
H49A H 0.1984 0.7134 0.4719 0.086 Uiso 1 1 calc R . .
H49B H 0.2148 0.6274 0.4746 0.086 Uiso 1 1 calc R . .
H49C H 0.3131 0.6844 0.4881 0.086 Uiso 1 1 calc R . .
C49B C 0.4114(4) 0.3179(3) 0.7671(3) 0.0618(14) Uani 1 1 d . . .
H49D H 0.4275 0.3412 0.8139 0.093 Uiso 1 1 calc R . .
H49E H 0.4684 0.3294 0.7465 0.093 Uiso 1 1 calc R . .
H49F H 0.4025 0.2645 0.7676 0.093 Uiso 1 1 calc R . .
C50A C 0.1952(3) 0.86479(19) 0.70540(19) 0.0318(9) Uani 1 1 d . . .
H50A H 0.2023 0.9176 0.7217 0.038 Uiso 1 1 calc R . .
H50B H 0.1655 0.8609 0.6555 0.038 Uiso 1 1 calc R . .
C50B C -0.0610(3) 0.38789(19) 0.69588(19) 0.0309(8) Uani 1 1 d . . .
H50C H -0.0395 0.4364 0.7219 0.037 Uiso 1 1 calc R . .
H50D H -0.0611 0.3935 0.6479 0.037 Uiso 1 1 calc R . .
C51A C 0.1184(3) 0.8274(2) 0.7374(2) 0.0403(10) Uani 1 1 d . . .
H51A H 0.1353 0.8430 0.7868 0.048 Uiso 1 1 calc R . .
H51B H 0.1230 0.7735 0.7316 0.048 Uiso 1 1 calc R . .
C51B C -0.1706(3) 0.3674(2) 0.6985(2) 0.0365(9) Uani 1 1 d . . .
H51C H -0.1703 0.3546 0.7448 0.044 Uiso 1 1 calc R . .
H51D H -0.1978 0.3237 0.6662 0.044 Uiso 1 1 calc R . .
C52A C 0.0087(3) 0.8476(2) 0.7038(3) 0.0484(11) Uani 1 1 d . . .
H52A H 0.0074 0.9016 0.7031 0.058 Uiso 1 1 calc R . .
H52B H -0.0116 0.8253 0.6561 0.058 Uiso 1 1 calc R . .
C52B C -0.2416(3) 0.4303(2) 0.6805(2) 0.0441(10) Uani 1 1 d . . .
H52C H -0.2142 0.4738 0.7131 0.053 Uiso 1 1 calc R . .
H52D H -0.2408 0.4434 0.6344 0.053 Uiso 1 1 calc R . .
C53A C -0.0693(4) 0.8214(3) 0.7412(4) 0.0770(18) Uani 1 1 d . . .
H53A H -0.0688 0.7679 0.7417 0.116 Uiso 1 1 calc R . .
H53B H -0.1389 0.8349 0.7180 0.116 Uiso 1 1 calc R . .
H53C H -0.0506 0.8445 0.7881 0.116 Uiso 1 1 calc R . .
C53B C -0.3527(4) 0.4118(3) 0.6821(3) 0.0642(15) Uani 1 1 d . . .
H53D H -0.3823 0.3712 0.6474 0.096 Uiso 1 1 calc R . .
H53E H -0.3937 0.4549 0.6727 0.096 Uiso 1 1 calc R . .
H53F H -0.3539 0.3972 0.7271 0.096 Uiso 1 1 calc R . .
C54A C 0.3451(3) 0.82520(18) 0.79476(18) 0.0290(8) Uani 1 1 d . . .
H54A H 0.2962 0.7911 0.8083 0.035 Uiso 1 1 calc R . .
H54B H 0.4123 0.8018 0.8011 0.035 Uiso 1 1 calc R . .
C54B C 0.0222(3) 0.32135(18) 0.79647(17) 0.0275(8) Uani 1 1 d . . .
H54C H 0.0796 0.2895 0.8139 0.033 Uiso 1 1 calc R . .
H54D H -0.0435 0.2946 0.7968 0.033 Uiso 1 1 calc R . .
C55A C 0.3608(3) 0.8952(2) 0.8419(2) 0.0352(9) Uani 1 1 d . . .
H55A H 0.2981 0.9239 0.8304 0.042 Uiso 1 1 calc R . .
H55B H 0.4203 0.9254 0.8358 0.042 Uiso 1 1 calc R . .
C55B C 0.0357(3) 0.39101(19) 0.84468(18) 0.0330(9) Uani 1 1 d . . .
H55C H -0.0289 0.4178 0.8345 0.040 Uiso 1 1 calc R . .
H55D H 0.0926 0.4234 0.8378 0.040 Uiso 1 1 calc R . .
C56A C 0.3814(3) 0.8773(2) 0.91600(19) 0.0344(9) Uani 1 1 d . . .
H56A H 0.4346 0.8403 0.9241 0.041 Uiso 1 1 calc R . .
H56B H 0.4102 0.9223 0.9462 0.041 Uiso 1 1 calc R . .
C56B C 0.0608(3) 0.3727(2) 0.91870(19) 0.0363(9) Uani 1 1 d . . .
H56C H 0.0543 0.4171 0.9482 0.044 Uiso 1 1 calc R . .
H56D H 0.0093 0.3345 0.9236 0.044 Uiso 1 1 calc R . .
C57A C 0.2861(4) 0.8483(2) 0.9351(2) 0.0484(11) Uani 1 1 d . . .
H57A H 0.2314 0.8833 0.9247 0.073 Uiso 1 1 calc R . .
H57B H 0.3034 0.8420 0.9839 0.073 Uiso 1 1 calc R . .
H57C H 0.2615 0.8009 0.9090 0.073 Uiso 1 1 calc R . .
C57B C 0.1694(4) 0.3454(3) 0.9428(2) 0.0483(11) Uani 1 1 d . . .
H57D H 0.1726 0.2970 0.9192 0.073 Uiso 1 1 calc R . .
H57E H 0.1854 0.3416 0.9920 0.073 Uiso 1 1 calc R . .
H57F H 0.2200 0.3800 0.9327 0.073 Uiso 1 1 calc R . .
N1A N 0.4016(2) 0.60257(16) 0.96045(16) 0.0305(7) Uani 1 1 d . . .
N1B N 0.0680(2) 0.10104(15) 0.95686(15) 0.0256(6) Uani 1 1 d . . .
N34A N 0.1972(2) 0.57078(15) 0.93988(15) 0.0284(7) Uani 1 1 d . . .
N34B N 0.2536(2) 0.06615(15) 0.93659(14) 0.0251(6) Uani 1 1 d . . .
N41A N 0.3036(2) 0.83523(15) 0.71923(15) 0.0289(7) Uani 1 1 d . . .
N41B N 0.0202(2) 0.33389(15) 0.72342(15) 0.0259(6) Uani 1 1 d . . .
O1A O 0.2463(2) 0.67208(13) 0.83868(14) 0.0351(6) Uani 1 1 d . . .
O1B O 0.06119(19) -0.01697(12) 0.84201(12) 0.0286(5) Uani 1 1 d . . .
O2A O 0.30762(19) 0.48443(13) 0.84573(13) 0.0306(6) Uani 1 1 d . . .
O2B O 0.14295(19) 0.16934(12) 0.83583(13) 0.0292(6) Uani 1 1 d . . .
O9A O 0.4396(2) 0.61645(14) 0.83507(14) 0.0375(6) Uani 1 1 d . . .
O9B O -0.06095(19) 0.12016(13) 0.83045(13) 0.0317(6) Uani 1 1 d . . .
O10A O 0.5427(2) 0.69819(15) 0.75835(17) 0.0449(7) Uani 1 1 d . . .
O10B O -0.2140(2) 0.20403(14) 0.75562(14) 0.0365(6) Uani 1 1 d . . .
O25A O -0.0709(2) 0.56829(14) 0.69656(13) 0.0380(7) Uani 1 1 d . . .
O25B O 0.3374(2) 0.06630(13) 0.69320(12) 0.0309(6) Uani 1 1 d . . .
O32A O 0.10429(18) 0.54862(12) 0.80024(12) 0.0255(5) Uani 1 1 d . . .
O32B O 0.23945(18) 0.04492(12) 0.79727(12) 0.0257(5) Uani 1 1 d . . .
Cl1A Cl 0.26174(8) 0.55641(6) 0.70196(5) 0.0390(2) Uani 1 1 d . . .
Cl1B Cl 0.00669(7) 0.05524(5) 0.69893(5) 0.0350(2) Uani 1 1 d . . .
U1A U 0.277894(10) 0.578083(6) 0.837862(7) 0.02458(4) Uani 1 1 d . . .
U1B U 0.097183(10) 0.076255(6) 0.834668(6) 0.02158(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2A N1A 1.292(5) . ?
C2A C3A 1.435(6) . ?
C2B N1B 1.298(5) . ?
C2B C3B 1.435(5) . ?
C3A C8A 1.404(5) . ?
C3A C4A 1.416(6) . ?
C3B C8B 1.413(5) . ?
C3B C4B 1.417(5) . ?
C4A O9A 1.308(4) . ?
C4A C5A 1.420(6) . ?
C4B O9B 1.305(4) . ?
C4B C5B 1.427(5) . ?
C5A O10A 1.370(6) . ?
C5A C6A 1.389(6) . ?
C5B C6B 1.372(6) . ?
C5B O10B 1.377(5) . ?
C6A C7A 1.397(7) . ?
C6B C7B 1.391(6) . ?
C7A C8A 1.360(7) . ?
C7B C8B 1.366(6) . ?
C11A O10A 1.449(5) . ?
C11A C12A 1.494(6) . ?
C11B O10B 1.443(5) . ?
C11B C12B 1.506(5) . ?
C12A C17A 1.386(7) . ?
C12A C13A 1.387(7) . ?
C12B C17B 1.373(6) . ?
C12B C13B 1.389(6) . ?
C13A C14A 1.407(8) . ?
C13B C14B 1.392(7) . ?
C14A C15A 1.370(10) . ?
C14B C15B 1.368(8) . ?
C15A C16A 1.369(10) . ?
C15B C16B 1.367(8) . ?
C16A C17A 1.386(8) . ?
C16B C17B 1.396(7) . ?
C18A C23A 1.359(8) . ?
C18A C19A 1.362(7) . ?
C18A C24A 1.503(6) . ?
C18B C23B 1.367(6) . ?
C18B C19B 1.387(6) . ?
C18B C24B 1.501(5) . ?
C19A C20A 1.400(8) . ?
C19B C20B 1.381(6) . ?
C20A C21A 1.354(8) . ?
C20B C21B 1.363(6) . ?
C21A C22A 1.323(9) . ?
C21B C22B 1.374(7) . ?
C22A C23A 1.405(8) . ?
C22B C23B 1.381(7) . ?
C24A O25A 1.422(5) . ?
C24B O25B 1.438(4) . ?
C26A C31A 1.372(6) . ?
C26A O25A 1.375(5) . ?
C26A C27A 1.423(5) . ?
C26B O25B 1.379(4) . ?
C26B C31B 1.382(5) . ?
C26B C27B 1.425(5) . ?
C27A O32A 1.306(4) . ?
C27A C28A 1.431(5) . ?
C27B O32B 1.305(4) . ?
C27B C28B 1.422(5) . ?
C28A C29A 1.401(5) . ?
C28A C33A 1.437(5) . ?
C28B C29B 1.407(5) . ?
C28B C33B 1.438(5) . ?
C29A C30A 1.370(6) . ?
C29B C30B 1.367(6) . ?
C30A C31A 1.387(6) . ?
C30B C31B 1.400(6) . ?
C33A N34A 1.289(5) . ?
C33B N34B 1.289(5) . ?
C35A C36A 1.390(6) . ?
C35A C40A 1.403(6) . ?
C35A N34A 1.424(4) . ?
C35B C36B 1.393(5) . ?
C35B C40B 1.393(5) . ?
C35B N34B 1.425(4) . ?
C36A C37A 1.395(6) . ?
C36B C37B 1.379(5) . ?
C37A C38A 1.375(7) . ?
C37B C38B 1.373(6) . ?
C38A C39A 1.378(6) . ?
C38B C39B 1.385(5) . ?
C39A C40A 1.401(5) . ?
C39B C40B 1.397(5) . ?
C40A N1A 1.420(5) . ?
C40B N1B 1.428(4) . ?
C42A C43A 1.508(5) . ?
C42A N41A 1.510(4) . ?
C42B C43B 1.522(5) . ?
C42B N41B 1.525(4) . ?
C43A C44A 1.520(5) . ?
C43B C44B 1.527(5) . ?
C44A C45A 1.512(7) . ?
C44B C45B 1.522(6) . ?
C46A C47A 1.522(5) . ?
C46A N41A 1.528(4) . ?
C46B N41B 1.518(4) . ?
C46B C47B 1.528(5) . ?
C47A C48A 1.492(6) . ?
C47B C48B 1.517(6) . ?
C48A C49A 1.494(6) . ?
C48B C49B 1.517(6) . ?
C50A C51A 1.516(5) . ?
C50A N41A 1.527(5) . ?
C50B C51B 1.511(5) . ?
C50B N41B 1.524(4) . ?
C51A C52A 1.524(6) . ?
C51B C52B 1.524(5) . ?
C52A C53A 1.520(7) . ?
C52B C53B 1.515(6) . ?
C54A C55A 1.512(5) . ?
C54A N41A 1.528(4) . ?
C54B N41B 1.518(4) . ?
C54B C55B 1.521(5) . ?
C55A C56A 1.530(5) . ?
C55B C56B 1.528(5) . ?
C56A C57A 1.510(6) . ?
C56B C57B 1.522(6) . ?
N1A U1A 2.619(3) . ?
N1B U1B 2.619(3) . ?
N34A U1A 2.577(3) . ?
N34B U1B 2.572(3) . ?
O1A U1A 1.784(2) . ?
O1B U1B 1.784(2) . ?
O2A U1A 1.783(2) . ?
O2B U1B 1.785(2) . ?
O9A U1A 2.259(3) . ?
O9B U1B 2.265(2) . ?
O32A U1A 2.278(2) . ?
O32B U1B 2.286(2) . ?
Cl1A U1A 2.7172(10) . ?
Cl1B U1B 2.7157(9) . ?

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
N1A C2A C3A 127.3(4) . . ?
N1B C2B C3B 127.8(3) . . ?
C8A C3A C4A 119.9(4) . . ?
C8A C3A C2A 118.2(4) . . ?
C4A C3A C2A 121.9(3) . . ?
C8B C3B C4B 119.9(4) . . ?
C8B C3B C2B 118.0(4) . . ?
C4B C3B C2B 122.0(3) . . ?
O9A C4A C3A 121.7(4) . . ?
O9A C4A C5A 120.2(4) . . ?
C3A C4A C5A 118.1(4) . . ?
O9B C4B C3B 122.0(3) . . ?
O9B C4B C5B 120.6(3) . . ?
C3B C4B C5B 117.4(3) . . ?
O10A C5A C6A 118.0(4) . . ?
O10A C5A C4A 122.0(4) . . ?
C6A C5A C4A 119.9(5) . . ?
C6B C5B O10B 117.9(3) . . ?
C6B C5B C4B 120.7(4) . . ?
O10B C5B C4B 121.2(3) . . ?
C5A C6A C7A 121.3(5) . . ?
C5B C6B C7B 121.4(4) . . ?
C8A C7A C6A 119.3(4) . . ?
C8B C7B C6B 119.6(4) . . ?
C7A C8A C3A 121.6(5) . . ?
C7B C8B C3B 121.0(4) . . ?
O10A C11A C12A 108.0(3) . . ?
O10B C11B C12B 108.3(3) . . ?
C17A C12A C13A 120.0(5) . . ?
C17A C12A C11A 119.0(4) . . ?
C13A C12A C11A 120.9(5) . . ?
C17B C12B C13B 119.2(4) . . ?
C17B C12B C11B 119.5(4) . . ?
C13B C12B C11B 121.3(4) . . ?
C12A C13A C14A 118.8(6) . . ?
C12B C13B C14B 119.7(5) . . ?
C15A C14A C13A 119.8(6) . . ?
C15B C14B C13B 120.4(5) . . ?
C16A C15A C14A 121.6(7) . . ?
C16B C15B C14B 120.4(5) . . ?
C15A C16A C17A 119.1(7) . . ?
C15B C16B C17B 119.6(6) . . ?
C12A C17A C16A 120.6(6) . . ?
C12B C17B C16B 120.7(5) . . ?
C23A C18A C19A 117.4(5) . . ?
C23A C18A C24A 121.6(5) . . ?
C19A C18A C24A 120.9(5) . . ?
C23B C18B C19B 118.5(4) . . ?
C23B C18B C24B 120.0(4) . . ?
C19B C18B C24B 121.4(4) . . ?
C18A C19A C20A 121.7(5) . . ?
C20B C19B C18B 120.2(4) . . ?
C21A C20A C19A 119.3(6) . . ?
C21B C20B C19B 120.9(4) . . ?
C22A C21A C20A 119.9(6) . . ?
C20B C21B C22B 119.1(4) . . ?
C21A C22A C23A 121.1(6) . . ?
C21B C22B C23B 120.2(4) . . ?
C18A C23A C22A 120.5(6) . . ?
C18B C23B C22B 121.0(4) . . ?
O25A C24A C18A 107.4(4) . . ?
O25B C24B C18B 108.2(3) . . ?
C31A C26A O25A 118.6(3) . . ?
C31A C26A C27A 121.1(4) . . ?
O25A C26A C27A 120.3(3) . . ?
O25B C26B C31B 117.9(3) . . ?
O25B C26B C27B 120.6(3) . . ?
C31B C26B C27B 121.5(3) . . ?
O32A C27A C26A 120.8(3) . . ?
O32A C27A C28A 122.8(3) . . ?
C26A C27A C28A 116.3(3) . . ?
O32B C27B C28B 122.3(3) . . ?
O32B C27B C26B 120.9(3) . . ?
C28B C27B C26B 116.6(3) . . ?
C29A C28A C27A 120.3(4) . . ?
C29A C28A C33A 117.6(4) . . ?
C27A C28A C33A 121.9(3) . . ?
C29B C28B C27B 120.8(3) . . ?
C29B C28B C33B 116.9(3) . . ?
C27B C28B C33B 122.2(3) . . ?
C30A C29A C28A 121.7(4) . . ?
C30B C29B C28B 120.8(4) . . ?
C29A C30A C31A 118.4(4) . . ?
C29B C30B C31B 119.9(4) . . ?
C26A C31A C30A 122.2(4) . . ?
C26B C31B C30B 120.4(4) . . ?
N34A C33A C28A 126.7(4) . . ?
N34B C33B C28B 127.1(3) . . ?
C36A C35A C40A 119.8(3) . . ?
C36A C35A N34A 123.8(4) . . ?
C40A C35A N34A 116.4(3) . . ?
C36B C35B C40B 119.3(3) . . ?
C36B C35B N34B 123.4(3) . . ?
C40B C35B N34B 117.2(3) . . ?
C35A C36A C37A 120.1(4) . . ?
C37B C36B C35B 120.6(4) . . ?
C38A C37A C36A 120.0(4) . . ?
C38B C37B C36B 120.2(4) . . ?
C37A C38A C39A 120.6(4) . . ?
C37B C38B C39B 120.2(4) . . ?
C38A C39A C40A 120.3(4) . . ?
C38B C39B C40B 120.1(4) . . ?
C39A C40A C35A 119.1(4) . . ?
C39A C40A N1A 123.7(4) . . ?
C35A C40A N1A 117.2(3) . . ?
C35B C40B C39B 119.5(3) . . ?
C35B C40B N1B 117.1(3) . . ?
C39B C40B N1B 123.5(3) . . ?
C43A C42A N41A 115.9(3) . . ?
C43B C42B N41B 114.9(3) . . ?
C42A C43A C44A 111.2(3) . . ?
C42B C43B C44B 110.8(3) . . ?
C45A C44A C43A 112.3(4) . . ?
C45B C44B C43B 111.1(4) . . ?
C47A C46A N41A 115.1(3) . . ?
N41B C46B C47B 115.2(3) . . ?
C48A C47A C46A 111.9(3) . . ?
C48B C47B C46B 111.0(3) . . ?
C47A C48A C49A 114.9(4) . . ?
C47B C48B C49B 112.3(4) . . ?
C51A C50A N41A 116.3(3) . . ?
C51B C50B N41B 115.9(3) . . ?
C50A C51A C52A 109.7(3) . . ?
C50B C51B C52B 111.4(3) . . ?
C53A C52A C51A 111.8(4) . . ?
C53B C52B C51B 113.1(4) . . ?
C55A C54A N41A 115.0(3) . . ?
N41B C54B C55B 114.7(3) . . ?
C54A C55A C56A 110.2(3) . . ?
C54B C55B C56B 110.7(3) . . ?
C57A C56A C55A 113.7(3) . . ?
C57B C56B C55B 112.8(3) . . ?
C2A N1A C40A 117.2(3) . . ?
C2A N1A U1A 127.3(3) . . ?
C40A N1A U1A 115.3(2) . . ?
C2B N1B C40B 116.5(3) . . ?
C2B N1B U1B 128.1(2) . . ?
C40B N1B U1B 115.3(2) . . ?
C33A N34A C35A 117.9(3) . . ?
C33A N34A U1A 124.3(2) . . ?
C35A N34A U1A 117.3(2) . . ?
C33B N34B C35B 118.1(3) . . ?
C33B N34B U1B 124.1(2) . . ?
C35B N34B U1B 117.1(2) . . ?
C42A N41A C50A 107.2(3) . . ?
C42A N41A C54A 110.5(3) . . ?
C50A N41A C54A 110.8(3) . . ?
C42A N41A C46A 111.7(3) . . ?
C50A N41A C46A 110.3(3) . . ?
C54A N41A C46A 106.3(3) . . ?
C54B N41B C46B 110.8(3) . . ?
C54B N41B C50B 110.9(3) . . ?
C46B N41B C50B 107.0(3) . . ?
C54B N41B C42B 105.9(2) . . ?
C46B N41B C42B 111.2(3) . . ?
C50B N41B C42B 111.1(3) . . ?
C4A O9A U1A 137.7(3) . . ?
C4B O9B U1B 140.8(2) . . ?
C5A O10A C11A 117.0(3) . . ?
C5B O10B C11B 116.8(3) . . ?
C26A O25A C24A 117.2(3) . . ?
C26B O25B C24B 113.3(3) . . ?
C27A O32A U1A 128.9(2) . . ?
C27B O32B U1B 129.2(2) . . ?
O2A U1A O1A 174.08(12) . . ?
O2A U1A O9A 94.82(11) . . ?
O1A U1A O9A 87.53(11) . . ?
O2A U1A O32A 92.49(10) . . ?
O1A U1A O32A 87.17(10) . . ?
O9A U1A O32A 158.93(9) . . ?
O2A U1A N34A 87.45(10) . . ?
O1A U1A N34A 86.88(11) . . ?
O9A U1A N34A 130.05(10) . . ?
O32A U1A N34A 69.94(9) . . ?
O2A U1A N1A 85.00(10) . . ?
O1A U1A N1A 90.84(10) . . ?
O9A U1A N1A 68.30(10) . . ?
O32A U1A N1A 132.15(9) . . ?
N34A U1A N1A 62.21(10) . . ?
O2A U1A Cl1A 89.49(8) . . ?
O1A U1A Cl1A 96.29(9) . . ?
O9A U1A Cl1A 79.74(7) . . ?
O32A U1A Cl1A 80.60(6) . . ?
N34A U1A Cl1A 150.21(7) . . ?
N1A U1A Cl1A 146.91(8) . . ?
O1B U1B O2B 173.92(11) . . ?
O1B U1B O9B 96.20(10) . . ?
O2B U1B O9B 86.83(10) . . ?
O1B U1B O32B 92.88(10) . . ?
O2B U1B O32B 86.15(10) . . ?
O9B U1B O32B 157.89(9) . . ?
O1B U1B N34B 87.40(10) . . ?
O2B U1B N34B 86.63(10) . . ?
O9B U1B N34B 130.58(9) . . ?
O32B U1B N34B 69.83(9) . . ?
O1B U1B N1B 84.80(10) . . ?
O2B U1B N1B 91.42(10) . . ?
O9B U1B N1B 68.72(9) . . ?
O32B U1B N1B 132.38(9) . . ?
N34B U1B N1B 62.55(9) . . ?
O1B U1B Cl1B 89.09(8) . . ?
O2B U1B Cl1B 96.67(8) . . ?
O9B U1B Cl1B 79.02(7) . . ?
O32B U1B Cl1B 81.02(6) . . ?
N34B U1B Cl1B 150.41(7) . . ?
N1B U1B Cl1B 146.21(7) . . ?

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
N1A C2A C3A C8A 171.3(4) . . . . ?
N1A C2A C3A C4A -10.4(6) . . . . ?
N1B C2B C3B C8B -173.7(3) . . . . ?
N1B C2B C3B C4B 7.5(6) . . . . ?
C8A C3A C4A O9A 177.4(3) . . . . ?
C2A C3A C4A O9A -0.8(6) . . . . ?
C8A C3A C4A C5A -0.5(5) . . . . ?
C2A C3A C4A C5A -178.7(3) . . . . ?
C8B C3B C4B O9B -177.3(3) . . . . ?
C2B C3B C4B O9B 1.5(5) . . . . ?
C8B C3B C4B C5B 1.9(5) . . . . ?
C2B C3B C4B C5B -179.4(3) . . . . ?
O9A C4A C5A O10A 6.2(6) . . . . ?
C3A C4A C5A O10A -175.8(3) . . . . ?
O9A C4A C5A C6A -178.9(3) . . . . ?
C3A C4A C5A C6A -1.0(5) . . . . ?
O9B C4B C5B C6B 179.4(3) . . . . ?
C3B C4B C5B C6B 0.2(5) . . . . ?
O9B C4B C5B O10B -6.0(5) . . . . ?
C3B C4B C5B O10B 174.9(3) . . . . ?
O10A C5A C6A C7A 176.8(4) . . . . ?
C4A C5A C6A C7A 1.8(6) . . . . ?
O10B C5B C6B C7B -176.6(3) . . . . ?
C4B C5B C6B C7B -1.8(6) . . . . ?
C5A C6A C7A C8A -1.0(6) . . . . ?
C5B C6B C7B C8B 1.3(6) . . . . ?
C6A C7A C8A C3A -0.6(7) . . . . ?
C4A C3A C8A C7A 1.3(6) . . . . ?
C2A C3A C8A C7A 179.6(4) . . . . ?
C6B C7B C8B C3B 0.9(6) . . . . ?
C4B C3B C8B C7B -2.5(6) . . . . ?
C2B C3B C8B C7B 178.7(3) . . . . ?
O10A C11A C12A C17A -134.7(4) . . . . ?
O10A C11A C12A C13A 46.3(5) . . . . ?
O10B C11B C12B C17B 142.0(4) . . . . ?
O10B C11B C12B C13B -38.8(5) . . . . ?
C17A C12A C13A C14A -1.9(7) . . . . ?
C11A C12A C13A C14A 177.0(5) . . . . ?
C17B C12B C13B C14B 0.5(7) . . . . ?
C11B C12B C13B C14B -178.7(4) . . . . ?
C12A C13A C14A C15A 1.1(9) . . . . ?
C12B C13B C14B C15B 0.4(8) . . . . ?
C13A C14A C15A C16A 0.6(10) . . . . ?
C13B C14B C15B C16B -0.9(10) . . . . ?
C14A C15A C16A C17A -1.4(10) . . . . ?
C14B C15B C16B C17B 0.6(11) . . . . ?
C13A C12A C17A C16A 1.1(7) . . . . ?
C11A C12A C17A C16A -177.8(4) . . . . ?
C15A C16A C17A C12A 0.5(8) . . . . ?
C13B C12B C17B C16B -0.8(8) . . . . ?
C11B C12B C17B C16B 178.3(5) . . . . ?
C15B C16B C17B C12B 0.3(10) . . . . ?
C23A C18A C19A C20A 1.2(9) . . . . ?
C24A C18A C19A C20A -176.6(5) . . . . ?
C23B C18B C19B C20B 0.5(6) . . . . ?
C24B C18B C19B C20B 178.5(4) . . . . ?
C18A C19A C20A C21A 0.6(10) . . . . ?
C18B C19B C20B C21B -1.1(7) . . . . ?
C19A C20A C21A C22A -1.0(11) . . . . ?
C19B C20B C21B C22B 0.8(7) . . . . ?
C20A C21A C22A C23A -0.4(13) . . . . ?
C20B C21B C22B C23B 0.2(8) . . . . ?
C19A C18A C23A C22A -2.6(12) . . . . ?
C24A C18A C23A C22A 175.2(7) . . . . ?
C21A C22A C23A C18A 2.3(14) . . . . ?
C19B C18B C23B C22B 0.5(7) . . . . ?
C24B C18B C23B C22B -177.6(4) . . . . ?
C21B C22B C23B C18B -0.8(8) . . . . ?
C23A C18A C24A O25A -65.9(8) . . . . ?
C19A C18A C24A O25A 111.9(5) . . . . ?
C23B C18B C24B O25B -95.1(5) . . . . ?
C19B C18B C24B O25B 86.9(5) . . . . ?
C31A C26A C27A O32A 178.0(3) . . . . ?
O25A C26A C27A O32A 1.8(5) . . . . ?
C31A C26A C27A C28A 1.7(5) . . . . ?
O25A C26A C27A C28A -174.6(3) . . . . ?
O25B C26B C27B O32B 1.6(5) . . . . ?
C31B C26B C27B O32B -176.8(3) . . . . ?
O25B C26B C27B C28B 177.2(3) . . . . ?
C31B C26B C27B C28B -1.2(5) . . . . ?
O32A C27A C28A C29A -177.1(3) . . . . ?
C26A C27A C28A C29A -0.9(5) . . . . ?
O32A C27A C28A C33A -2.5(5) . . . . ?
C26A C27A C28A C33A 173.7(3) . . . . ?
O32B C27B C28B C29B 176.7(3) . . . . ?
C26B C27B C28B C29B 1.2(5) . . . . ?
O32B C27B C28B C33B 1.0(5) . . . . ?
C26B C27B C28B C33B -174.5(3) . . . . ?
C27A C28A C29A C30A -0.7(6) . . . . ?
C33A C28A C29A C30A -175.5(4) . . . . ?
C27B C28B C29B C30B -0.2(5) . . . . ?
C33B C28B C29B C30B 175.7(3) . . . . ?
C28A C29A C30A C31A 1.5(6) . . . . ?
C28B C29B C30B C31B -0.9(6) . . . . ?
O25A C26A C31A C30A 175.3(4) . . . . ?
C27A C26A C31A C30A -1.0(6) . . . . ?
C29A C30A C31A C26A -0.7(7) . . . . ?
O25B C26B C31B C30B -178.3(3) . . . . ?
C27B C26B C31B C30B 0.1(5) . . . . ?
C29B C30B C31B C26B 0.9(6) . . . . ?
C29A C28A C33A N34A -169.4(4) . . . . ?
C27A C28A C33A N34A 15.9(6) . . . . ?
C29B C28B C33B N34B 170.4(3) . . . . ?
C27B C28B C33B N34B -13.7(6) . . . . ?
C40A C35A C36A C37A 0.0(6) . . . . ?
N34A C35A C36A C37A 179.2(4) . . . . ?
C40B C35B C36B C37B -0.6(5) . . . . ?
N34B C35B C36B C37B 179.5(3) . . . . ?
C35A C36A C37A C38A -1.6(6) . . . . ?
C35B C36B C37B C38B 1.6(6) . . . . ?
C36A C37A C38A C39A 0.8(7) . . . . ?
C36B C37B C38B C39B -0.9(6) . . . . ?
C37A C38A C39A C40A 1.6(6) . . . . ?
C37B C38B C39B C40B -0.7(6) . . . . ?
C38A C39A C40A C35A -3.2(6) . . . . ?
C38A C39A C40A N1A 177.7(4) . . . . ?
C36A C35A C40A C39A 2.3(5) . . . . ?
N34A C35A C40A C39A -176.9(3) . . . . ?
C36A C35A C40A N1A -178.5(3) . . . . ?
N34A C35A C40A N1A 2.3(5) . . . . ?
C36B C35B C40B C39B -1.0(5) . . . . ?
N34B C35B C40B C39B 178.9(3) . . . . ?
C36B C35B C40B N1B 178.8(3) . . . . ?
N34B C35B C40B N1B -1.3(4) . . . . ?
C38B C39B C40B C35B 1.7(5) . . . . ?
C38B C39B C40B N1B -178.1(3) . . . . ?
N41A C42A C43A C44A -178.6(3) . . . . ?
N41B C42B C43B C44B -165.7(3) . . . . ?
C42A C43A C44A C45A -180.0(4) . . . . ?
C42B C43B C44B C45B -178.5(3) . . . . ?
N41A C46A C47A C48A -163.5(4) . . . . ?
N41B C46B C47B C48B 162.5(3) . . . . ?
C46A C47A C48A C49A -171.3(4) . . . . ?
C46B C47B C48B C49B 168.5(3) . . . . ?
N41A C50A C51A C52A -164.4(3) . . . . ?
N41B C50B C51B C52B 170.9(3) . . . . ?
C50A C51A C52A C53A -171.1(4) . . . . ?
C50B C51B C52B C53B 179.6(4) . . . . ?
N41A C54A C55A C56A 168.8(3) . . . . ?
N41B C54B C55B C56B -167.4(3) . . . . ?
C54A C55A C56A C57A -73.9(4) . . . . ?
C54B C55B C56B C57B 70.7(4) . . . . ?
C3A C2A N1A C40A 174.9(3) . . . . ?
C3A C2A N1A U1A -10.9(6) . . . . ?
C39A C40A N1A C2A -33.8(5) . . . . ?
C35A C40A N1A C2A 147.1(3) . . . . ?
C39A C40A N1A U1A 151.4(3) . . . . ?
C35A C40A N1A U1A -27.8(4) . . . . ?
C3B C2B N1B C40B -174.2(3) . . . . ?
C3B C2B N1B U1B 9.6(5) . . . . ?
C35B C40B N1B C2B -150.7(3) . . . . ?
C39B C40B N1B C2B 29.1(5) . . . . ?
C35B C40B N1B U1B 26.0(4) . . . . ?
C39B C40B N1B U1B -154.2(3) . . . . ?
C28A C33A N34A C35A -173.7(3) . . . . ?
C28A C33A N34A U1A 14.6(5) . . . . ?
C36A C35A N34A C33A 33.7(5) . . . . ?
C40A C35A N34A C33A -147.1(3) . . . . ?
C36A C35A N34A U1A -154.0(3) . . . . ?
C40A C35A N34A U1A 25.2(4) . . . . ?
C28B C33B N34B C35B 173.5(3) . . . . ?
C28B C33B N34B U1B -16.3(5) . . . . ?
C36B C35B N34B C33B -34.1(5) . . . . ?
C40B C35B N34B C33B 146.0(3) . . . . ?
C36B C35B N34B U1B 155.0(3) . . . . ?
C40B C35B N34B U1B -24.9(4) . . . . ?
C43A C42A N41A C50A 179.1(3) . . . . ?
C43A C42A N41A C54A 58.2(4) . . . . ?
C43A C42A N41A C46A -59.9(4) . . . . ?
C51A C50A N41A C42A -167.3(3) . . . . ?
C51A C50A N41A C54A -46.6(4) . . . . ?
C51A C50A N41A C46A 70.9(4) . . . . ?
C55A C54A N41A C42A 55.2(4) . . . . ?
C55A C54A N41A C50A -63.5(4) . . . . ?
C55A C54A N41A C46A 176.6(3) . . . . ?
C47A C46A N41A C42A -47.9(4) . . . . ?
C47A C46A N41A C50A 71.2(4) . . . . ?
C47A C46A N41A C54A -168.6(3) . . . . ?
C55B C54B N41B C46B 65.1(4) . . . . ?
C55B C54B N41B C50B -53.5(4) . . . . ?
C55B C54B N41B C42B -174.2(3) . . . . ?
C47B C46B N41B C54B 52.8(4) . . . . ?
C47B C46B N41B C50B 173.7(3) . . . . ?
C47B C46B N41B C42B -64.8(4) . . . . ?
C51B C50B N41B C54B -56.6(4) . . . . ?
C51B C50B N41B C46B -177.4(3) . . . . ?
C51B C50B N41B C42B 61.0(4) . . . . ?
C43B C42B N41B C54B -167.8(3) . . . . ?
C43B C42B N41B C46B -47.4(4) . . . . ?
C43B C42B N41B C50B 71.7(4) . . . . ?
C3A C4A O9A U1A 44.9(5) . . . . ?
C5A C4A O9A U1A -137.3(3) . . . . ?
C3B C4B O9B U1B -38.4(5) . . . . ?
C5B C4B O9B U1B 142.4(3) . . . . ?
C6A C5A O10A C11A 129.2(4) . . . . ?
C4A C5A O10A C11A -55.9(5) . . . . ?
C12A C11A O10A C5A -165.8(3) . . . . ?
C6B C5B O10B C11B -127.4(4) . . . . ?
C4B C5B O10B C11B 57.9(4) . . . . ?
C12B C11B O10B C5B 156.6(3) . . . . ?
C31A C26A O25A C24A 108.2(4) . . . . ?
C27A C26A O25A C24A -75.5(5) . . . . ?
C18A C24A O25A C26A -148.9(4) . . . . ?
C31B C26B O25B C24B -108.4(4) . . . . ?
C27B C26B O25B C24B 73.1(4) . . . . ?
C18B C24B O25B C26B 166.2(3) . . . . ?
C26A C27A O32A U1A 135.5(3) . . . . ?
C28A C27A O32A U1A -48.4(4) . . . . ?
C28B C27B O32B U1B 48.9(4) . . . . ?
C26B C27B O32B U1B -135.7(3) . . . . ?
C4A O9A U1A O2A -129.6(4) . . . . ?
C4A O9A U1A O1A 45.0(4) . . . . ?
C4A O9A U1A O32A 120.5(4) . . . . ?
C4A O9A U1A N34A -38.8(4) . . . . ?
C4A O9A U1A N1A -46.9(4) . . . . ?
C4A O9A U1A Cl1A 141.8(4) . . . . ?
C27A O32A U1A O2A 140.5(3) . . . . ?
C27A O32A U1A O1A -33.6(3) . . . . ?
C27A O32A U1A O9A -109.2(3) . . . . ?
C27A O32A U1A N34A 54.1(3) . . . . ?
C27A O32A U1A N1A 54.9(3) . . . . ?
C27A O32A U1A Cl1A -130.5(3) . . . . ?
C33A N34A U1A O2A -129.9(3) . . . . ?
C35A N34A U1A O2A 58.3(2) . . . . ?
C33A N34A U1A O1A 51.8(3) . . . . ?
C35A N34A U1A O1A -120.0(2) . . . . ?
C33A N34A U1A O9A 135.9(3) . . . . ?
C35A N34A U1A O9A -35.9(3) . . . . ?
C33A N34A U1A O32A -36.4(3) . . . . ?
C35A N34A U1A O32A 151.9(3) . . . . ?
C33A N34A U1A N1A 144.4(3) . . . . ?
C35A N34A U1A N1A -27.4(2) . . . . ?
C33A N34A U1A Cl1A -45.4(3) . . . . ?
C35A N34A U1A Cl1A 142.8(2) . . . . ?
C2A N1A U1A O2A 124.0(3) . . . . ?
C40A N1A U1A O2A -61.8(2) . . . . ?
C2A N1A U1A O1A -60.2(3) . . . . ?
C40A N1A U1A O1A 114.0(2) . . . . ?
C2A N1A U1A O9A 26.8(3) . . . . ?
C40A N1A U1A O9A -159.0(3) . . . . ?
C2A N1A U1A O32A -147.1(3) . . . . ?
C40A N1A U1A O32A 27.1(3) . . . . ?
C2A N1A U1A N34A -146.2(3) . . . . ?
C40A N1A U1A N34A 28.0(2) . . . . ?
C2A N1A U1A Cl1A 42.7(4) . . . . ?
C40A N1A U1A Cl1A -143.1(2) . . . . ?
C4B O9B U1B O1B 121.7(4) . . . . ?
C4B O9B U1B O2B -53.0(4) . . . . ?
C4B O9B U1B O32B -124.6(3) . . . . ?
C4B O9B U1B N34B 29.8(4) . . . . ?
C4B O9B U1B N1B 39.8(3) . . . . ?
C4B O9B U1B Cl1B -150.4(4) . . . . ?
C27B O32B U1B O1B -140.5(3) . . . . ?
C27B O32B U1B O2B 33.5(3) . . . . ?
C27B O32B U1B O9B 105.3(3) . . . . ?
C27B O32B U1B N34B -54.3(3) . . . . ?
C27B O32B U1B N1B -54.9(3) . . . . ?
C27B O32B U1B Cl1B 130.9(3) . . . . ?
C33B N34B U1B O1B 130.7(3) . . . . ?
C35B N34B U1B O1B -59.0(2) . . . . ?
C33B N34B U1B O2B -50.5(3) . . . . ?
C35B N34B U1B O2B 119.8(2) . . . . ?
C33B N34B U1B O9B -133.4(3) . . . . ?
C35B N34B U1B O9B 36.9(3) . . . . ?
C33B N34B U1B O32B 36.6(3) . . . . ?
C35B N34B U1B O32B -153.0(2) . . . . ?
C33B N34B U1B N1B -143.9(3) . . . . ?
C35B N34B U1B N1B 26.5(2) . . . . ?
C33B N34B U1B Cl1B 47.1(3) . . . . ?
C35B N34B U1B Cl1B -142.57(19) . . . . ?
C2B N1B U1B O1B -120.7(3) . . . . ?
C40B N1B U1B O1B 63.1(2) . . . . ?
C2B N1B U1B O2B 64.1(3) . . . . ?
C40B N1B U1B O2B -112.2(2) . . . . ?
C2B N1B U1B O9B -22.0(3) . . . . ?
C40B N1B U1B O9B 161.8(2) . . . . ?
C2B N1B U1B O32B 150.1(3) . . . . ?
C40B N1B U1B O32B -26.1(3) . . . . ?
C2B N1B U1B N34B 149.5(3) . . . . ?
C40B N1B U1B N34B -26.7(2) . . . . ?
C2B N1B U1B Cl1B -40.2(3) . . . . ?
C40B N1B U1B Cl1B 143.58(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.109

#===END
####################################################################### 
# 
# 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_mo_20211226_0m
_database_code_depnum_ccdc_archive 'CCDC 2151869'
_audit_update_record             
;
2022-09-20 deposited with the CCDC.	2023-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H18 Cl2 N22 O15'
_chemical_formula_weight         757.36

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   33.372(4)
_cell_length_b                   6.9585(7)
_cell_length_c                   25.558(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.533(4)
_cell_angle_gamma                90
_cell_volume                     5520.8(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    1965
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      25.68

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_F_000             3088
_exptl_transmission_factor_min   0.864
_exptl_transmission_factor_max   0.864
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.348
_shelx_estimated_absorpt_T_min   0.950
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ccd
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22759
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.512
_diffrn_reflns_theta_max         26.436
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             5612
_reflns_number_gt                3299
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0264P)²+13.4519P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5612
_refine_ls_number_parameters     442
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0538
_refine_ls_wR_factor_ref         0.1157
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.018
_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
C1 C 0.22102(11) 0.5277(5) 0.60850(15) 0.0203(8) Uani 1 1 d . . . A 1
C2 C 0.26602(11) 0.5176(5) 0.64635(14) 0.0185(8) Uani 1 1 d . . . A 1
C3 C 0.32985(11) 0.5762(5) 0.68910(15) 0.0219(8) Uani 1 1 d . . . A 1
C4 C 0.42322(12) 0.8680(6) 0.74034(15) 0.0283(9) Uani 1 1 d . . . A 1
C5 C 0.43734(12) 0.6838(6) 0.75702(15) 0.0289(10) Uani 1 1 d . . . A 1
N1 N 0.19118(9) 0.6058(4) 0.62646(12) 0.0218(7) Uani 1 1 d . . . A 1
N2 N 0.20915(10) 0.4441(4) 0.55505(13) 0.0260(7) Uani 1 1 d . . . A 1
N3 N 0.29593(9) 0.6538(4) 0.64863(12) 0.0218(7) Uani 1 1 d . . . A 1
N4 N 0.32415(10) 0.4124(5) 0.71142(14) 0.0326(8) Uani 1 1 d . . . A 1
N5 N 0.28111(10) 0.3721(5) 0.68206(13) 0.0308(8) Uani 1 1 d . . . A 1
N6 N 0.38049(10) 0.8497(5) 0.71039(12) 0.0242(7) Uani 1 1 d . . . A 1
N7 N 0.37168(9) 0.6567(4) 0.70887(12) 0.0244(7) Uani 1 1 d . . . A 1
N8 N 0.40640(10) 0.5528(5) 0.73786(13) 0.0287(8) Uani 1 1 d . . . A 1
N9 N 0.48022(11) 0.6213(6) 0.79221(13) 0.0359(9) Uani 1 1 d . . . A 1
O1 O 0.15145(8) 0.6053(4) 0.59875(11) 0.0307(6) Uani 1 1 d . . . A 1
O2 O 0.20518(8) 0.6830(4) 0.67581(10) 0.0255(6) Uani 1 1 d . . . A 1
O3 O 0.17169(9) 0.4449(4) 0.52010(11) 0.0343(7) Uani 1 1 d . . . A 1
O4 O 0.23943(9) 0.3701(4) 0.54397(11) 0.0323(7) Uani 1 1 d . . . A 1
O5 O 0.35203(8) 0.9781(4) 0.68932(11) 0.0289(6) Uani 1 1 d . . . A 1
O6 O 0.48672(9) 0.4478(5) 0.80005(12) 0.0420(8) Uani 1 1 d . . . A 1
O7 O 0.50697(9) 0.7477(5) 0.81123(12) 0.0478(8) Uani 1 1 d . . . A 1
Cl1 Cl 0.44644(3) 1.08561(15) 0.75087(4) 0.0364(3) Uani 1 1 d . . . A 1
C6 C 0.36917(11) 0.6297(5) 0.88919(14) 0.0210(8) Uani 1 1 d . . . B 2
C7 C 0.41622(12) 0.6171(5) 0.91208(14) 0.0222(8) Uani 1 1 d . . . B 2
C8 C 0.47851(11) 0.5367(5) 0.92514(15) 0.0213(8) Uani 1 1 d . . . B 2
C9 C 0.55896(12) 0.2297(6) 0.91040(15) 0.0261(9) Uani 1 1 d . . . B 2
C10 C 0.57578(12) 0.4131(6) 0.91485(15) 0.0248(9) Uani 1 1 d . . . B 2
Cl2 Cl 0.57638(3) 0.00961(14) 0.90256(4) 0.0331(2) Uani 1 1 d . . . B 2
N10 N 0.34964(10) 0.7219(4) 0.83805(12) 0.0229(7) Uani 1 1 d . . . B 2
N11 N 0.34536(10) 0.5544(4) 0.91898(12) 0.0239(7) Uani 1 1 d . . . B 2
N12 N 0.43823(10) 0.4799(4) 0.89556(12) 0.0239(7) Uani 1 1 d . . . B 2
N13 N 0.44156(9) 0.7453(5) 0.94819(13) 0.0271(7) Uani 1 1 d . . . B 2
N14 N 0.48326(10) 0.6901(4) 0.95708(13) 0.0259(7) Uani 1 1 d . . . B 2
N15 N 0.51553(10) 0.4476(4) 0.92112(12) 0.0246(7) Uani 1 1 d . . . B 2
N16 N 0.54968(10) 0.5470(4) 0.92125(12) 0.0256(7) Uani 1 1 d . . . B 2
N17 N 0.51961(10) 0.2526(5) 0.91453(12) 0.0251(7) Uani 1 1 d . . . B 2
N18 N 0.61592(10) 0.4729(5) 0.91007(13) 0.0295(8) Uani 1 1 d . . . B 2
O8 O 0.37504(8) 0.7960(4) 0.81679(11) 0.0305(7) Uani 1 1 d . . . B 2
O9 O 0.30991(8) 0.7342(4) 0.81324(10) 0.0302(6) Uani 1 1 d . . . B 2
O10 O 0.30530(8) 0.5569(4) 0.90085(11) 0.0289(6) Uani 1 1 d . . . B 2
O11 O 0.36669(8) 0.4817(4) 0.96613(10) 0.0303(6) Uani 1 1 d . . . B 2
O12 O 0.49147(8) 0.1292(4) 0.91332(11) 0.0331(7) Uani 1 1 d . . . B 2
O13 O 0.62189(9) 0.6450(4) 0.90612(12) 0.0369(7) Uani 1 1 d . . . B 2
O14 O 0.64106(9) 0.3442(4) 0.90953(12) 0.0405(8) Uani 1 1 d . . . B 2
N19 N 0.70984(11) 1.0096(5) 0.92644(13) 0.0413(9) Uani 1 1 d . . . . .
H19A H 0.7360 0.9618 0.9506 0.050 Uiso 1 1 d R U . . .
H19B H 0.6902 0.9912 0.9439 0.050 Uiso 1 1 d R U . . .
H19C H 0.7147 1.1270 0.9128 0.050 Uiso 1 1 d R U . . .
H19D H 0.6964 0.9228 0.8978 0.050 Uiso 1 1 d R U . . .
N20 N 0.23298(9) 0.4946(4) 0.78631(12) 0.0240(7) Uani 1 1 d . . . . .
H20A H 0.2350 0.6166 0.8004 0.029 Uiso 1 1 d R U . . .
H20B H 0.2272 0.5119 0.7487 0.029 Uiso 1 1 d R U . . .
H20C H 0.2584 0.4303 0.8035 0.029 Uiso 1 1 d R U . . .
H20D H 0.2093 0.4314 0.7879 0.029 Uiso 1 1 d R U . . .
N21 N 0.43421(9) 0.1335(4) 0.97634(12) 0.0270(8) Uani 1 1 d D . . . .
H21A H 0.4355 0.0028 0.9691 0.032 Uiso 1 1 d DR U . . .
H21B H 0.4589 0.1672 1.0062 0.032 Uiso 1 1 d DR U . . .
H21C H 0.4111 0.1739 0.9851 0.032 Uiso 1 1 d DR U . . .
H21D H 0.4324 0.1971 0.9437 0.032 Uiso 1 1 d DR U . . .
N22 N 0.37905(9) 0.2200(4) 0.81126(12) 0.0264(7) Uani 1 1 d D . . . .
H22A H 0.4020 0.2920 0.8344 0.032 Uiso 1 1 d DR U . . .
H22B H 0.3843 0.0892 0.8109 0.032 Uiso 1 1 d DR U . . .
H22C H 0.3665 0.2710 0.7754 0.032 Uiso 1 1 d DR U . . .
H22D H 0.3582 0.2245 0.8271 0.032 Uiso 1 1 d DR U . . .
O15 O 0.28941(9) 0.3530(4) 0.99727(12) 0.0406(8) Uani 1 1 d . . . . .
H15A H 0.2924 0.4200 1.0272 0.061 Uiso 1 1 d R U . . .
H15B H 0.3090 0.3980 0.9856 0.061 Uiso 1 1 d R 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
C1 N1 1.354(4) . ?
C1 N2 1.402(4) . ?
C1 C2 1.459(5) . ?
C2 N5 1.332(4) . ?
C2 N3 1.362(4) . ?
C3 N4 1.319(5) . ?
C3 N3 1.335(4) . ?
C3 N7 1.414(4) . ?
C4 N6 1.354(5) . ?
C4 C5 1.378(5) . ?
C4 Cl1 1.677(4) . ?
C5 N8 1.329(5) . ?
C5 N9 1.449(5) . ?
N1 O1 1.253(4) . ?
N1 O2 1.290(3) . ?
N2 O3 1.241(4) . ?
N2 O4 1.256(4) . ?
N4 N5 1.383(4) . ?
N6 O5 1.271(4) . ?
N6 N7 1.372(4) . ?
N7 N8 1.336(4) . ?
N9 O7 1.220(4) . ?
N9 O6 1.230(4) . ?
C6 N10 1.386(4) . ?
C6 N11 1.389(4) . ?
C6 C7 1.463(5) . ?
C7 N13 1.338(5) . ?
C7 N12 1.363(5) . ?
C8 N14 1.318(5) . ?
C8 N12 1.337(4) . ?
C8 N15 1.419(5) . ?
C9 N17 1.365(5) . ?
C9 C10 1.382(5) . ?
C9 Cl2 1.676(4) . ?
C10 N16 1.326(5) . ?
C10 N18 1.450(5) . ?
N10 O9 1.245(4) . ?
N10 O8 1.271(4) . ?
N11 O10 1.244(4) . ?
N11 O11 1.259(4) . ?
N13 N14 1.380(4) . ?
N15 N16 1.332(4) . ?
N15 N17 1.380(4) . ?
N17 O12 1.264(4) . ?
N18 O13 1.224(4) . ?
N18 O14 1.230(4) . ?
N19 H19A 0.9255 . ?
N19 H19B 0.9266 . ?
N19 H19C 0.9253 . ?
N19 H19D 0.9279 . ?
N20 H20A 0.9149 . ?
N20 H20B 0.9156 . ?
N20 H20C 0.9154 . ?
N20 H20D 0.9170 . ?
N21 H21A 0.9326 . ?
N21 H21B 0.9253 . ?
N21 H21C 0.9235 . ?
N21 H21D 0.9272 . ?
N22 H22A 0.9237 . ?
N22 H22B 0.9267 . ?
N22 H22C 0.9273 . ?
N22 H22D 0.9251 . ?
O15 H15A 0.8698 . ?
O15 H15B 0.8700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 121.1(3) . . ?
N1 C1 C2 120.0(3) . . ?
N2 C1 C2 118.7(3) . . ?
N5 C2 N3 114.4(3) . . ?
N5 C2 C1 122.0(3) . . ?
N3 C2 C1 123.7(3) . . ?
N4 C3 N3 118.0(3) . . ?
N4 C3 N7 117.9(3) . . ?
N3 C3 N7 124.1(3) . . ?
N6 C4 C5 104.9(3) . . ?
N6 C4 Cl1 120.3(3) . . ?
C5 C4 Cl1 134.8(3) . . ?
N8 C5 C4 113.1(3) . . ?
N8 C5 N9 118.7(4) . . ?
C4 C5 N9 128.2(4) . . ?
O1 N1 O2 118.8(3) . . ?
O1 N1 C1 124.4(3) . . ?
O2 N1 C1 116.8(3) . . ?
O3 N2 O4 121.4(3) . . ?
O3 N2 C1 123.3(3) . . ?
O4 N2 C1 115.3(3) . . ?
C3 N3 C2 98.7(3) . . ?
C3 N4 N5 103.1(3) . . ?
C2 N5 N4 105.9(3) . . ?
O5 N6 C4 129.9(3) . . ?
O5 N6 N7 123.8(3) . . ?
C4 N6 N7 106.2(3) . . ?
N8 N7 N6 112.4(3) . . ?
N8 N7 C3 121.7(3) . . ?
N6 N7 C3 124.8(3) . . ?
C5 N8 N7 103.4(3) . . ?
O7 N9 O6 125.7(4) . . ?
O7 N9 C5 116.3(4) . . ?
O6 N9 C5 118.0(4) . . ?
N10 C6 N11 121.8(3) . . ?
N10 C6 C7 118.0(3) . . ?
N11 C6 C7 120.3(3) . . ?
N13 C7 N12 113.9(3) . . ?
N13 C7 C6 123.4(3) . . ?
N12 C7 C6 122.6(3) . . ?
N14 C8 N12 117.2(3) . . ?
N14 C8 N15 119.3(3) . . ?
N12 C8 N15 123.4(3) . . ?
N17 C9 C10 105.0(3) . . ?
N17 C9 Cl2 120.1(3) . . ?
C10 C9 Cl2 134.8(3) . . ?
N16 C10 C9 113.2(3) . . ?
N16 C10 N18 118.5(3) . . ?
C9 C10 N18 128.2(3) . . ?
O9 N10 O8 120.5(3) . . ?
O9 N10 C6 123.8(3) . . ?
O8 N10 C6 115.7(3) . . ?
O10 N11 O11 121.0(3) . . ?
O10 N11 C6 122.9(3) . . ?
O11 N11 C6 116.1(3) . . ?
C8 N12 C7 99.3(3) . . ?
C7 N13 N14 105.8(3) . . ?
C8 N14 N13 103.8(3) . . ?
N16 N15 N17 112.9(3) . . ?
N16 N15 C8 122.6(3) . . ?
N17 N15 C8 124.5(3) . . ?
C10 N16 N15 103.6(3) . . ?
O12 N17 C9 130.2(3) . . ?
O12 N17 N15 124.4(3) . . ?
C9 N17 N15 105.4(3) . . ?
O13 N18 O14 125.4(3) . . ?
O13 N18 C10 118.1(3) . . ?
O14 N18 C10 116.6(3) . . ?
H19A N19 H19B 106.9 . . ?
H19A N19 H19C 108.5 . . ?
H19B N19 H19C 123.7 . . ?
H19A N19 H19D 110.9 . . ?
H19B N19 H19D 93.7 . . ?
H19C N19 H19D 112.2 . . ?
H20A N20 H20B 104.3 . . ?
H20A N20 H20C 110.1 . . ?
H20B N20 H20C 111.5 . . ?
H20A N20 H20D 111.6 . . ?
H20B N20 H20D 104.9 . . ?
H20C N20 H20D 113.8 . . ?
H21A N21 H21B 108.6 . . ?
H21A N21 H21C 116.7 . . ?
H21B N21 H21C 107.1 . . ?
H21A N21 H21D 106.1 . . ?
H21B N21 H21D 111.5 . . ?
H21C N21 H21D 106.8 . . ?
H22A N22 H22B 115.1 . . ?
H22A N22 H22C 113.1 . . ?
H22B N22 H22C 112.6 . . ?
H22A N22 H22D 106.4 . . ?
H22B N22 H22D 102.2 . . ?
H22C N22 H22D 106.1 . . ?
H15A O15 H15B 104.5 . . ?

_refine_diff_density_max         0.326
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.082

####################################################################### 
# 
# 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_l4
_database_code_depnum_ccdc_archive 'CCDC 2151872'
_audit_update_record             
;
2022-09-20 deposited with the CCDC.	2023-02-13 downloaded from the CCDC.
;
_audit_creation_date             2022-09-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C5 H2 Cl N9 O6'
_chemical_formula_sum            'C5 H2 Cl N9 O6'
_chemical_formula_weight         319.61
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   37.714(5)
_cell_length_b                   6.7183(12)
_cell_length_c                   13.638(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3455.5(9)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    1548
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.61
_cell_measurement_theta_min      2.99
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0991
_diffrn_reflns_av_unetI/netI     0.1190
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15732
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.382
_diffrn_reflns_theta_min         2.160
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                3454
_reflns_number_total             6057
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    ?
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         6057
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.0784
_refine_ls_restrained_S_all      1.280
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1788
_refine_ls_wR_factor_ref         0.2217
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H4A(0.04) H4B(0.04) H11A(0.037) H11B(0.037) H27A(0.04) H27B(0.04)
 Fixed X: H4A(0.249055) H4B(0.278344) H11A(0.456778) H11B(0.432218)
 H27A(0.374707) H27B(0.349297)
 Fixed Y: H4A(0.043534) H4B(-0.098526) H11A(0.216115) H11B(0.280425)
 H27A(0.561937) H27B(0.641018)
 Fixed Z: H4A(0.207965) H4B(0.240135) H11A(0.554216) H11B(0.637146)
 H27A(0.902864) H27B(0.825184)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.17243(9) 0.3121(8) -0.1637(4) 0.0710(14) Uani 1 1 d . . . . .
Cl2 Cl 0.53583(10) -0.4834(7) 0.3923(4) 0.0704(13) Uani 1 1 d . . . . .
Cl3 Cl 0.42556(13) 0.1827(9) 1.1613(5) 0.101(2) Uani 1 1 d . . . . .
O1 O 0.3152(3) -0.5839(17) 0.1151(9) 0.074(3) Uani 1 1 d D . . . .
O2 O 0.3113(2) -0.3410(15) 0.2170(8) 0.045(2) Uani 1 1 d . . . . .
O3 O 0.1804(3) 0.4991(17) 0.0236(10) 0.073(3) Uani 1 1 d . . . . .
O4 O 0.1489(2) 0.2946(16) 0.0945(9) 0.056(3) Uani 1 1 d D . . . .
O5 O 0.1049(3) 0.189(2) -0.0788(8) 0.077(4) Uani 1 1 d . . . . .
O6 O 0.1284(3) -0.078(2) -0.0204(8) 0.066(3) Uani 1 1 d . . . . .
O7 O 0.4953(3) -0.490(2) 0.2111(11) 0.089(4) Uani 1 1 d . . . . .
O8 O 0.4485(3) -0.407(4) 0.2824(10) 0.152(9) Uani 1 1 d . . . . .
O9 O 0.4957(4) -0.0561(19) 0.2593(9) 0.083(4) Uani 1 1 d . . . . .
O10 O 0.5393(3) -0.0618(16) 0.3618(9) 0.069(3) Uani 1 1 d D . . . .
O11 O 0.3640(2) -0.0493(13) 0.7915(7) 0.040(2) Uani 1 1 d . . . . .
O12 O 0.3983(2) 0.2039(12) 0.7616(6) 0.035(2) Uani 1 1 d . . . . .
O13 O 0.4568(3) -0.164(2) 1.0730(9) 0.087(4) Uani 1 1 d . . . . .
O14 O 0.4144(2) -0.2034(15) 0.9693(9) 0.056(3) Uani 1 1 d . . . . .
O15 O 0.3877(4) -0.329(3) 1.1501(15) 0.127(6) Uani 1 1 d . U . . .
O16 O 0.3759(5) -0.095(3) 1.2422(12) 0.109(7) Uani 1 1 d . . . . .
O17 O 0.2629(2) 0.3942(13) 0.7085(7) 0.042(2) Uani 1 1 d . . . . .
O18 O 0.3029(2) 0.6184(14) 0.7389(7) 0.043(2) Uani 1 1 d . . . . .
N1 N 0.2499(3) -0.3500(17) -0.0754(8) 0.041(3) Uani 1 1 d . . . . .
N2 N 0.2730(3) -0.4169(16) -0.0080(8) 0.042(3) Uani 1 1 d . . . . .
N3 N 0.3030(3) -0.4234(18) 0.1400(10) 0.045(3) Uani 1 1 d . . . . .
N4 N 0.2624(2) -0.0612(15) 0.1966(8) 0.033(2) Uani 1 1 d . . . . .
H4A H 0.249055 0.043534 0.207965 0.040 Uiso 1 1 d R U . . .
H4B H 0.278344 -0.098526 0.240135 0.040 Uiso 1 1 d R U . . .
N5 N 0.2343(2) -0.1069(15) 0.0456(9) 0.036(3) Uani 1 1 d . . . . .
N6 N 0.2114(2) 0.0502(16) 0.0578(8) 0.034(2) Uani 1 1 d . . . . .
N7 N 0.2065(2) -0.0920(17) -0.0973(8) 0.040(3) Uani 1 1 d . . . . .
N8 N 0.1651(3) 0.3487(19) 0.0298(9) 0.046(3) Uani 1 1 d . . . . .
N9 N 0.1302(3) 0.090(2) -0.0522(9) 0.052(3) Uani 1 1 d . . . . .
N10 N 0.3894(2) 0.0287(15) 0.7487(8) 0.028(2) Uani 1 1 d . . . . .
N11 N 0.4417(2) 0.1856(13) 0.6012(8) 0.031(2) Uani 1 1 d . . . . .
H11A H 0.456778 0.216115 0.554216 0.037 Uiso 1 1 d R U . . .
H11B H 0.432218 0.280425 0.637146 0.037 Uiso 1 1 d R U . . .
N12 N 0.4716(2) -0.1062(14) 0.4796(8) 0.027(2) Uani 1 1 d . . . . .
N13 N 0.4494(2) -0.1403(13) 0.5602(8) 0.026(2) Uani 1 1 d . . . . .
N14 N 0.4615(2) -0.4425(15) 0.4998(7) 0.031(2) Uani 1 1 d . . . . .
N15 N 0.4219(2) -0.4186(15) 0.6380(8) 0.033(2) Uani 1 1 d . . . . .
N16 N 0.4051(2) -0.2866(15) 0.6927(8) 0.032(2) Uani 1 1 d . . . . .
N17 N 0.5145(3) -0.1300(19) 0.3252(10) 0.049(3) Uani 1 1 d . . . . .
N18 N 0.4802(3) -0.441(2) 0.2799(8) 0.041(3) Uani 1 1 d . U . . .
N19 N 0.4270(3) -0.1371(19) 1.0446(10) 0.055(3) Uani 1 1 d . . . . .
N20 N 0.3878(4) -0.142(3) 1.1918(16) 0.074(6) Uani 1 1 d . U . . .
N21 N 0.3420(2) -0.0318(14) 1.0287(8) 0.030(2) Uani 1 1 d . . . . .
N22 N 0.3767(2) 0.2449(15) 0.9933(8) 0.031(2) Uani 1 1 d . . . . .
N23 N 0.3458(2) 0.2427(13) 0.9397(7) 0.024(2) Uani 1 1 d . . . . .
N24 N 0.2943(2) 0.0434(14) 0.9188(8) 0.028(2) Uani 1 1 d . . . . .
N26 N 0.2889(2) 0.4562(15) 0.7536(8) 0.032(2) Uani 1 1 d . . . . .
N27 N 0.3554(2) 0.5479(14) 0.8673(8) 0.034(3) Uani 1 1 d . . . . .
H27A H 0.374707 0.561937 0.902864 0.040 Uiso 1 1 d R U . . .
H27B H 0.349297 0.641018 0.825184 0.040 Uiso 1 1 d R U . . .
C1 C 0.27801(17) -0.3300(7) 0.0772(6) 0.037(3) Uani 1 1 d D . . . .
C2 C 0.25841(16) -0.1594(6) 0.1140(6) 0.024(3) Uani 1 1 d D . . . .
C3 C 0.2313(3) -0.190(2) -0.0470(9) 0.033(3) Uani 1 1 d . . . . .
C4 C 0.19486(12) 0.0469(8) -0.0305(7) 0.031(3) Uani 1 1 d D . . . .
C5 C 0.16674(12) 0.1874(8) -0.0535(8) 0.043(3) Uani 1 1 d D . . . .
C6 C 0.41056(14) -0.0955(10) 0.6841(3) 0.025(3) Uani 1 1 d D . . . .
C7 C 0.43414(14) 0.0025(10) 0.6150(3) 0.024(2) Uani 1 1 d D . . . .
C8 C 0.4428(3) -0.3456(16) 0.5673(9) 0.025(2) Uani 1 1 d . . . . .
C9 C 0.47785(14) -0.2952(15) 0.4492(3) 0.027(3) Uani 1 1 d D . . . .
C10 C 0.50091(14) -0.3329(15) 0.3659(3) 0.031(3) Uani 1 1 d D . . . .
C11 C 0.40138(12) -0.0017(13) 1.1059(4) 0.041(3) Uani 1 1 d D . . . .
C12 C 0.37316(12) 0.0735(12) 1.0435(4) 0.030(3) Uani 1 1 d D . . . .
C13 C 0.3254(3) 0.0801(17) 0.9632(8) 0.026(3) Uani 1 1 d . . . . .
C14 C 0.30344(10) 0.3294(13) 0.8299(5) 0.028(3) Uani 1 1 d D . . . .
C15 C 0.33627(10) 0.3900(13) 0.8771(5) 0.024(2) Uani 1 1 d D . . . .
N25 N 0.2851(2) 0.1694(15) 0.8490(8) 0.030(2) Uani 1 1 d . . . A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C5 1.734(10) . ?
Cl2 C10 1.699(8) . ?
Cl3 C11 1.714(9) . ?
O1 N3 1.222(14) . ?
O2 N3 1.228(15) . ?
O3 N8 1.166(14) . ?
O4 N8 1.134(13) . ?
O5 N9 1.218(16) . ?
O6 N9 1.213(17) . ?
O7 N18 1.145(15) . ?
O8 N18 1.217(16) . ?
O9 N17 1.247(16) . ?
O10 N17 1.156(15) . ?
O11 N10 1.238(11) . ?
O12 N10 1.237(12) . ?
O13 N19 1.203(14) . ?
O14 N19 1.215(15) . ?
O15 N20 1.38(3) . ?
O16 N20 0.88(2) . ?
O17 N26 1.230(12) . ?
O18 N26 1.228(12) . ?
N1 N2 1.344(16) . ?
N1 C3 1.339(17) . ?
N2 C1 1.314(13) . ?
N3 C1 1.418(14) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N4 C2 1.314(12) . ?
N5 N6 1.375(14) . ?
N5 C2 1.350(12) . ?
N5 C3 1.387(16) . ?
N6 C4 1.357(13) . ?
N7 C3 1.337(16) . ?
N7 C4 1.375(13) . ?
N8 C5 1.570(16) . ?
N9 C5 1.523(12) . ?
N10 C6 1.452(11) . ?
N11 H11A 0.8802 . ?
N11 H11B 0.8800 . ?
N11 C7 1.277(11) . ?
N12 N13 1.399(12) . ?
N12 C9 1.356(13) . ?
N13 C7 1.346(11) . ?
N13 C8 1.406(13) . ?
N14 C8 1.330(14) . ?
N14 C9 1.355(13) . ?
N15 N16 1.319(13) . ?
N15 C8 1.338(15) . ?
N16 C6 1.305(11) . ?
N17 C10 1.558(16) . ?
N18 C10 1.587(12) . ?
N19 C11 1.568(14) . ?
N20 C11 1.588(17) . ?
N21 C12 1.388(11) . ?
N21 C13 1.325(14) . ?
N22 N23 1.374(12) . ?
N22 C12 1.346(12) . ?
N23 C13 1.375(14) . ?
N23 C15 1.356(12) . ?
N24 C13 1.341(14) . ?
N24 N25 1.321(13) . ?
N26 C14 1.454(13) . ?
N27 H27A 0.8801 . ?
N27 H27B 0.8799 . ?
N27 C15 1.290(11) . ?
C1 C2 1.454(3) . ?
C4 C5 1.454(3) . ?
C6 C7 1.454(3) . ?
C9 C10 1.454(3) . ?
C11 C12 1.454(3) . ?
C14 C15 1.454(3) . ?
C14 N25 1.305(12) . ?

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
C3 N1 N2 114.2(10) . . ?
C1 N2 N1 123.3(10) . . ?
O1 N3 O2 122.6(12) . . ?
O1 N3 C1 118.3(12) . . ?
O2 N3 C1 119.2(10) . . ?
H4A N4 H4B 120.0 . . ?
C2 N4 H4A 119.0 . . ?
C2 N4 H4B 120.9 . . ?
N6 N5 C3 111.7(10) . . ?
C2 N5 N6 122.7(9) . . ?
C2 N5 C3 125.3(9) . . ?
C4 N6 N5 99.7(9) . . ?
C3 N7 C4 102.7(9) . . ?
O3 N8 C5 121.8(11) . . ?
O4 N8 O3 126.9(15) . . ?
O4 N8 C5 111.2(11) . . ?
O5 N9 C5 118.1(14) . . ?
O6 N9 O5 124.8(13) . . ?
O6 N9 C5 117.0(12) . . ?
O11 N10 C6 117.9(9) . . ?
O12 N10 O11 123.1(9) . . ?
O12 N10 C6 118.9(8) . . ?
H11A N11 H11B 120.0 . . ?
C7 N11 H11A 118.4 . . ?
C7 N11 H11B 121.6 . . ?
C9 N12 N13 101.0(7) . . ?
N12 N13 C8 108.8(9) . . ?
C7 N13 N12 125.2(8) . . ?
C7 N13 C8 125.7(8) . . ?
C8 N14 C9 103.7(9) . . ?
N16 N15 C8 116.3(10) . . ?
C6 N16 N15 122.4(9) . . ?
O9 N17 C10 114.7(11) . . ?
O10 N17 O9 127.8(14) . . ?
O10 N17 C10 117.4(12) . . ?
O7 N18 O8 124.5(12) . . ?
O7 N18 C10 119.3(10) . . ?
O8 N18 C10 112.2(11) . . ?
O13 N19 O14 125.5(12) . . ?
O13 N19 C11 119.4(11) . . ?
O14 N19 C11 115.0(9) . . ?
O15 N20 C11 103.7(16) . . ?
O16 N20 O15 130(3) . . ?
O16 N20 C11 122(3) . . ?
C13 N21 C12 102.0(8) . . ?
C12 N22 N23 100.2(8) . . ?
N22 N23 C13 111.1(9) . . ?
C15 N23 N22 123.5(8) . . ?
C15 N23 C13 125.2(8) . . ?
N25 N24 C13 116.0(9) . . ?
O17 N26 C14 117.4(9) . . ?
O18 N26 O17 124.3(11) . . ?
O18 N26 C14 118.3(9) . . ?
H27A N27 H27B 120.0 . . ?
C15 N27 H27A 119.6 . . ?
C15 N27 H27B 120.4 . . ?
N2 C1 N3 115.6(8) . . ?
N2 C1 C2 125.7(8) . . ?
N3 C1 C2 118.5(8) . . ?
N4 C2 N5 122.6(7) . . ?
N4 C2 C1 129.2(7) . . ?
N5 C2 C1 108.1(7) . . ?
N1 C3 N5 123.0(12) . . ?
N7 C3 N1 128.0(11) . . ?
N7 C3 N5 108.9(11) . . ?
N6 C4 N7 117.0(7) . . ?
N6 C4 C5 121.0(8) . . ?
N7 C4 C5 122.0(8) . . ?
N8 C5 Cl1 107.3(5) . . ?
N9 C5 Cl1 109.2(7) . . ?
N9 C5 N8 104.6(8) . . ?
C4 C5 Cl1 114.2(6) . . ?
C4 C5 N8 108.7(7) . . ?
C4 C5 N9 112.3(7) . . ?
N10 C6 C7 118.0(6) . . ?
N16 C6 N10 115.1(7) . . ?
N16 C6 C7 126.8(7) . . ?
N11 C7 N13 120.6(7) . . ?
N11 C7 C6 132.0(7) . . ?
N13 C7 C6 107.5(6) . . ?
N14 C8 N13 109.7(10) . . ?
N14 C8 N15 129.2(10) . . ?
N15 C8 N13 121.0(10) . . ?
N12 C9 C10 120.4(8) . . ?
N14 C9 N12 116.7(7) . . ?
N14 C9 C10 122.9(9) . . ?
N17 C10 Cl2 110.0(6) . . ?
N17 C10 N18 107.5(8) . . ?
N18 C10 Cl2 105.4(7) . . ?
C9 C10 Cl2 113.7(5) . . ?
C9 C10 N17 108.8(8) . . ?
C9 C10 N18 111.3(6) . . ?
N19 C11 Cl3 109.1(6) . . ?
N19 C11 N20 104.4(10) . . ?
N20 C11 Cl3 106.0(10) . . ?
C12 C11 Cl3 113.3(6) . . ?
C12 C11 N19 109.9(6) . . ?
C12 C11 N20 113.7(7) . . ?
N21 C12 C11 121.9(7) . . ?
N22 C12 N21 116.5(6) . . ?
N22 C12 C11 121.5(7) . . ?
N21 C13 N23 110.1(9) . . ?
N21 C13 N24 127.7(10) . . ?
N24 C13 N23 122.1(10) . . ?
N26 C14 C15 118.4(7) . . ?
N25 C14 N26 115.2(6) . . ?
N25 C14 C15 126.5(8) . . ?
N23 C15 C14 107.5(7) . . ?
N27 C15 N23 121.1(7) . . ?
N27 C15 C14 131.4(8) . . ?
C14 N25 N24 122.2(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl3 C11 C12 N21 -149.9(7) . . . . ?
Cl3 C11 C12 N22 33.3(9) . . . . ?
O1 N3 C1 N2 -6.7(14) . . . . ?
O1 N3 C1 C2 168.7(9) . . . . ?
O2 N3 C1 N2 173.5(10) . . . . ?
O2 N3 C1 C2 -11.2(13) . . . . ?
O3 N8 C5 Cl1 -30.5(12) . . . . ?
O3 N8 C5 N9 -146.4(12) . . . . ?
O3 N8 C5 C4 93.5(12) . . . . ?
O4 N8 C5 Cl1 152.3(9) . . . . ?
O4 N8 C5 N9 36.4(12) . . . . ?
O4 N8 C5 C4 -83.7(10) . . . . ?
O5 N9 C5 Cl1 -45.9(13) . . . . ?
O5 N9 C5 N8 68.7(13) . . . . ?
O5 N9 C5 C4 -173.6(11) . . . . ?
O6 N9 C5 Cl1 137.3(10) . . . . ?
O6 N9 C5 N8 -108.1(11) . . . . ?
O6 N9 C5 C4 9.6(15) . . . . ?
O7 N18 C10 Cl2 -52.6(15) . . . . ?
O7 N18 C10 N17 64.7(16) . . . . ?
O7 N18 C10 C9 -176.2(13) . . . . ?
O8 N18 C10 Cl2 149.2(14) . . . . ?
O8 N18 C10 N17 -93.5(14) . . . . ?
O8 N18 C10 C9 25.6(17) . . . . ?
O9 N17 C10 Cl2 143.5(9) . . . . ?
O9 N17 C10 N18 29.3(12) . . . . ?
O9 N17 C10 C9 -91.4(11) . . . . ?
O10 N17 C10 Cl2 -39.8(12) . . . . ?
O10 N17 C10 N18 -154.1(10) . . . . ?
O10 N17 C10 C9 85.3(11) . . . . ?
O11 N10 C6 N16 -13.3(12) . . . . ?
O11 N10 C6 C7 164.3(8) . . . . ?
O12 N10 C6 N16 163.7(9) . . . . ?
O12 N10 C6 C7 -18.7(11) . . . . ?
O13 N19 C11 Cl3 32.9(16) . . . . ?
O13 N19 C11 N20 -80.0(16) . . . . ?
O13 N19 C11 C12 157.7(13) . . . . ?
O14 N19 C11 Cl3 -145.6(10) . . . . ?
O14 N19 C11 N20 101.5(14) . . . . ?
O14 N19 C11 C12 -20.8(14) . . . . ?
O15 N20 C11 Cl3 -146.1(11) . . . . ?
O15 N20 C11 N19 -31.0(13) . . . . ?
O15 N20 C11 C12 88.7(12) . . . . ?
O16 N20 C11 Cl3 54(3) . . . . ?
O16 N20 C11 N19 169(3) . . . . ?
O16 N20 C11 C12 -71(3) . . . . ?
O17 N26 C14 C15 173.7(8) . . . . ?
O17 N26 C14 N25 -6.4(13) . . . . ?
O18 N26 C14 C15 -7.1(12) . . . . ?
O18 N26 C14 N25 172.9(9) . . . . ?
N1 N2 C1 N3 178.8(10) . . . . ?
N1 N2 C1 C2 3.8(14) . . . . ?
N2 N1 C3 N5 -2.9(16) . . . . ?
N2 N1 C3 N7 -179.6(11) . . . . ?
N2 C1 C2 N4 -177.9(9) . . . . ?
N2 C1 C2 N5 0.2(10) . . . . ?
N3 C1 C2 N4 7.2(12) . . . . ?
N3 C1 C2 N5 -174.6(8) . . . . ?
N5 N6 C4 N7 -2.6(10) . . . . ?
N5 N6 C4 C5 178.7(7) . . . . ?
N6 N5 C2 N4 -1.7(14) . . . . ?
N6 N5 C2 C1 -180.0(8) . . . . ?
N6 N5 C3 N1 -177.6(10) . . . . ?
N6 N5 C3 N7 -0.3(12) . . . . ?
N6 C4 C5 Cl1 129.2(8) . . . . ?
N6 C4 C5 N8 9.4(10) . . . . ?
N6 C4 C5 N9 -105.8(9) . . . . ?
N7 C4 C5 Cl1 -49.5(8) . . . . ?
N7 C4 C5 N8 -169.3(8) . . . . ?
N7 C4 C5 N9 75.5(11) . . . . ?
N10 C6 C7 N11 3.7(11) . . . . ?
N10 C6 C7 N13 -176.9(7) . . . . ?
N12 N13 C7 N11 -6.2(14) . . . . ?
N12 N13 C7 C6 174.2(8) . . . . ?
N12 N13 C8 N14 4.2(12) . . . . ?
N12 N13 C8 N15 -179.3(10) . . . . ?
N12 C9 C10 Cl2 122.5(8) . . . . ?
N12 C9 C10 N17 -0.4(9) . . . . ?
N12 C9 C10 N18 -118.7(9) . . . . ?
N13 N12 C9 N14 1.7(10) . . . . ?
N13 N12 C9 C10 -178.8(6) . . . . ?
N14 C9 C10 Cl2 -58.0(9) . . . . ?
N14 C9 C10 N17 179.1(8) . . . . ?
N14 C9 C10 N18 60.8(10) . . . . ?
N15 N16 C6 N10 178.9(9) . . . . ?
N15 N16 C6 C7 1.5(15) . . . . ?
N16 N15 C8 N13 7.1(16) . . . . ?
N16 N15 C8 N14 -177.1(11) . . . . ?
N16 C6 C7 N11 -179.1(10) . . . . ?
N16 C6 C7 N13 0.4(10) . . . . ?
N19 C11 C12 N21 87.8(9) . . . . ?
N19 C11 C12 N22 -89.0(10) . . . . ?
N20 C11 C12 N21 -28.8(14) . . . . ?
N20 C11 C12 N22 154.4(12) . . . . ?
N22 N23 C13 N21 -2.2(12) . . . . ?
N22 N23 C13 N24 -178.5(10) . . . . ?
N22 N23 C15 N27 -2.9(13) . . . . ?
N22 N23 C15 C14 176.6(8) . . . . ?
N23 N22 C12 N21 -2.6(10) . . . . ?
N23 N22 C12 C11 174.4(7) . . . . ?
N26 C14 C15 N23 -175.6(8) . . . . ?
N26 C14 C15 N27 3.8(12) . . . . ?
N26 C14 N25 N24 -177.6(9) . . . . ?
C2 N5 N6 C4 176.7(8) . . . . ?
C2 N5 C3 N1 7.5(17) . . . . ?
C2 N5 C3 N7 -175.2(9) . . . . ?
C3 N1 N2 C1 -2.3(15) . . . . ?
C3 N5 N6 C4 1.6(11) . . . . ?
C3 N5 C2 N4 172.7(10) . . . . ?
C3 N5 C2 C1 -5.6(12) . . . . ?
C3 N7 C4 N6 2.5(11) . . . . ?
C3 N7 C4 C5 -178.8(7) . . . . ?
C4 N7 C3 N1 175.9(11) . . . . ?
C4 N7 C3 N5 -1.2(11) . . . . ?
C7 N13 C8 N14 177.7(9) . . . . ?
C7 N13 C8 N15 -5.7(17) . . . . ?
C8 N13 C7 N11 -178.8(10) . . . . ?
C8 N13 C7 C6 1.7(12) . . . . ?
C8 N14 C9 N12 0.8(11) . . . . ?
C8 N14 C9 C10 -178.8(7) . . . . ?
C8 N15 N16 C6 -5.2(16) . . . . ?
C9 N12 N13 C7 -177.0(8) . . . . ?
C9 N12 N13 C8 -3.3(10) . . . . ?
C9 N14 C8 N13 -2.9(11) . . . . ?
C9 N14 C8 N15 -179.1(11) . . . . ?
C12 N21 C13 N23 0.5(11) . . . . ?
C12 N21 C13 N24 176.6(10) . . . . ?
C12 N22 N23 C13 2.7(10) . . . . ?
C12 N22 N23 C15 178.6(8) . . . . ?
C13 N21 C12 N22 1.4(11) . . . . ?
C13 N21 C12 C11 -175.6(7) . . . . ?
C13 N23 C15 N27 172.4(9) . . . . ?
C13 N23 C15 C14 -8.1(11) . . . . ?
C13 N24 N25 C14 -5.7(15) . . . . ?
C15 N23 C13 N21 -178.0(9) . . . . ?
C15 N23 C13 N24 5.7(16) . . . . ?
C15 C14 N25 N24 2.4(14) . . . . ?
N25 N24 C13 N21 -173.6(10) . . . . ?
N25 N24 C13 N23 2.0(15) . . . . ?
N25 C14 C15 N23 4.4(10) . . . . ?
N25 C14 C15 N27 -176.2(10) . . . . ?

_shelx_SHELXL_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_20211841_0m
_database_code_depnum_ccdc_archive 'CCDC 2151874'
_audit_update_record             
;
2022-09-20 deposited with the CCDC.	2023-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H8 N10 O7'
_chemical_formula_weight         320.21

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

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

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

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

_cell_length_a                   10.2673(4)
_cell_length_b                   10.8434(5)
_cell_length_c                   11.9935(5)
_cell_angle_alpha                80.6090(10)
_cell_angle_beta                 70.4600(10)
_cell_angle_gamma                80.229(2)
_cell_volume                     1231.95(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4477
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      26.36

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_F_000             656
_exptl_transmission_factor_min   0.864
_exptl_transmission_factor_max   0.864
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.158
_shelx_estimated_absorpt_T_min   0.977
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ccd
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14147
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.918
_diffrn_reflns_theta_max         26.446
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5000
_reflns_number_gt                3656
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0415P)²+0.2956P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5000
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1077
_refine_ls_wR_factor_gt          0.0933
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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
C1 C 0.03364(19) 0.6170(2) 0.58146(17) 0.0150(4) Uani 1 1 d . . . A 1
C2 C 0.1749(2) 0.6035(2) 0.49556(17) 0.0155(4) Uani 1 1 d . . . A 1
C3 C 0.3849(2) 0.6307(2) 0.41179(18) 0.0185(5) Uani 1 1 d . . . A 1
C4 C 0.4321(2) 0.5081(2) 0.24849(17) 0.0168(5) Uani 1 1 d . . . A 1
C5 C 0.5632(2) 0.5540(2) 0.21397(18) 0.0175(5) Uani 1 1 d . . . A 1
N1 N 0.01521(17) 0.55473(18) 0.69357(15) 0.0188(4) Uani 1 1 d . . . A 1
N2 N -0.06810(17) 0.70356(17) 0.55265(15) 0.0175(4) Uani 1 1 d . . . A 1
N3 N 0.27796(17) 0.66096(18) 0.50572(15) 0.0207(4) Uani 1 1 d . . . A 1
N4 N 0.20887(16) 0.53715(17) 0.40429(15) 0.0177(4) Uani 1 1 d . . . A 1
N5 N 0.34569(16) 0.55506(16) 0.35012(14) 0.0151(4) Uani 1 1 d . . . A 1
N6 N 0.51263(18) 0.6695(2) 0.37376(17) 0.0278(5) Uani 1 1 d . . . A 1
N7 N 0.59716(17) 0.62965(19) 0.27331(16) 0.0234(4) Uani 1 1 d . . . A 1
N8 N 0.38677(17) 0.43330(18) 0.19906(15) 0.0208(4) Uani 1 1 d . . . A 1
H8A H 0.3013 0.4136 0.2313 0.025 Uiso 1 1 calc R U . A 1
H8B H 0.4416 0.4024 0.1334 0.025 Uiso 1 1 calc R U . A 1
N9 N 0.67124(17) 0.52376(19) 0.10457(15) 0.0217(4) Uani 1 1 d . . . A 1
O3 O -0.09633(14) 0.56867(16) 0.77917(12) 0.0245(4) Uani 1 1 d . . . A 1
O4 O 0.11696(15) 0.48118(16) 0.70840(14) 0.0294(4) Uani 1 1 d . . . A 1
O5 O -0.18455(14) 0.73020(14) 0.62475(13) 0.0240(4) Uani 1 1 d . . . A 1
O6 O -0.03525(14) 0.75673(15) 0.44614(12) 0.0223(4) Uani 1 1 d . . . A 1
O7 O 0.77755(15) 0.57399(17) 0.07256(13) 0.0303(4) Uani 1 1 d . . . A 1
O8 O 0.64746(15) 0.44884(16) 0.04890(13) 0.0259(4) Uani 1 1 d . . . A 1
C6 C 0.2507(2) 0.0002(2) 0.50296(18) 0.0176(4) Uani 1 1 d . . . B 2
C7 C 0.26880(19) -0.0291(2) 0.38744(17) 0.0162(4) Uani 1 1 d . . . B 2
C8 C 0.4579(2) 0.0968(2) 0.33786(18) 0.0174(5) Uani 1 1 d . . . B 2
C9 C 0.6258(2) 0.0996(2) 0.02975(18) 0.0172(4) Uani 1 1 d . . . B 2
C10 C 0.5370(2) 0.0816(2) 0.15378(18) 0.0170(4) Uani 1 1 d . . . B 2
N10 N 0.13776(18) -0.04371(17) 0.60402(15) 0.0201(4) Uani 1 1 d . . . B 2
N11 N 0.43074(17) 0.12300(18) 0.45075(15) 0.0221(4) Uani 1 1 d . . . B 2
N12 N 0.32658(17) 0.07177(18) 0.53059(15) 0.0209(4) Uani 1 1 d . . . B 2
N13 N 0.20046(17) -0.09334(17) 0.34830(15) 0.0198(4) Uani 1 1 d . . . B 2
H13A H 0.2269 -0.1026 0.2721 0.024 Uiso 1 1 calc R U . B 2
H13B H 0.1278 -0.1275 0.3980 0.024 Uiso 1 1 calc R U . B 2
N14 N 0.38187(16) 0.02305(16) 0.30736(14) 0.0156(4) Uani 1 1 d . . . B 2
N15 N 0.43125(17) 0.01293(17) 0.18810(14) 0.0184(4) Uani 1 1 d . . . B 2
N16 N 0.55752(17) 0.13438(18) 0.24094(15) 0.0187(4) Uani 1 1 d . . . B 2
N17 N 0.59402(17) 0.20584(17) -0.04063(15) 0.0184(4) Uani 1 1 d . . . B 2
N18 N 0.74355(17) 0.01519(18) -0.00735(16) 0.0224(4) Uani 1 1 d . . . B 2
O9 O 0.76027(17) -0.07600(17) 0.06730(15) 0.0381(4) Uani 1 1 d . . . B 2
O10 O 0.82968(15) 0.02524(16) -0.10951(13) 0.0287(4) Uani 1 1 d . . . B 2
O11 O 0.48055(15) 0.27147(15) 0.00323(13) 0.0240(4) Uani 1 1 d . . . B 2
O12 O 0.67331(15) 0.23787(14) -0.14281(12) 0.0229(4) Uani 1 1 d . . . B 2
O13 O 0.12323(16) -0.01633(15) 0.70302(13) 0.0271(4) Uani 1 1 d . . . B 2
O14 O 0.06029(15) -0.10725(15) 0.58451(13) 0.0244(4) Uani 1 1 d . . . B 2
N19 N 0.99295(19) 0.7555(2) 0.89446(17) 0.0307(5) Uani 1 1 d . . . . .
H19A H 1.0061 0.7343 0.9747 0.037 Uiso 1 1 d R U . . .
H19B H 1.0779 0.7497 0.8373 0.037 Uiso 1 1 d R U . . .
H19C H 0.9492 0.8409 0.8880 0.037 Uiso 1 1 d R U . . .
H19D H 0.9357 0.7054 0.8879 0.037 Uiso 1 1 d R U . . .
N20 N 0.19101(18) 0.22415(18) 0.73327(15) 0.0224(4) Uani 1 1 d . . . . .
H20A H 0.2463 0.2771 0.7364 0.027 Uiso 1 1 d R U . . .
H20B H 0.1042 0.2376 0.7839 0.027 Uiso 1 1 d R U . . .
H20C H 0.1896 0.2309 0.6598 0.027 Uiso 1 1 d R U . . .
H20D H 0.2119 0.1461 0.7569 0.027 Uiso 1 1 d R U . . .
O1 O 0.92495(15) 0.30141(17) 0.89147(14) 0.0335(4) Uani 1 1 d . . . . .
H1A H 0.8601 0.2708 0.8828 0.050 Uiso 1 1 d R U . . .
H1B H 0.9117 0.3852 0.8791 0.050 Uiso 1 1 d R U . . .
O2 O 0.25744(15) 0.70469(15) 0.74131(13) 0.0236(4) Uani 1 1 d . . . . .
H2A H 0.3136 0.7512 0.7448 0.035 Uiso 1 1 d R U . . .
H2B H 0.2742 0.6964 0.6657 0.035 Uiso 1 1 d R 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
C1 N1 1.370(3) . ?
C1 N2 1.376(3) . ?
C1 C2 1.471(3) . ?
C2 N4 1.325(3) . ?
C2 N3 1.362(2) . ?
C3 N3 1.324(3) . ?
C3 N6 1.352(3) . ?
C3 N5 1.375(3) . ?
C4 N8 1.302(3) . ?
C4 N5 1.363(3) . ?
C4 C5 1.421(3) . ?
C5 N7 1.325(3) . ?
C5 N9 1.450(3) . ?
N1 O4 1.247(2) . ?
N1 O3 1.262(2) . ?
N2 O5 1.238(2) . ?
N2 O6 1.271(2) . ?
N4 N5 1.369(2) . ?
N6 N7 1.317(2) . ?
N8 H8A 0.8800 . ?
N8 H8B 0.8800 . ?
N9 O7 1.220(2) . ?
N9 O8 1.232(2) . ?
C6 N12 1.335(3) . ?
C6 C7 1.416(3) . ?
C6 N10 1.449(2) . ?
C7 N13 1.300(3) . ?
C7 N14 1.375(2) . ?
C8 N16 1.325(2) . ?
C8 N11 1.356(3) . ?
C8 N14 1.372(3) . ?
C9 N17 1.373(3) . ?
C9 N18 1.376(3) . ?
C9 C10 1.463(3) . ?
C10 N15 1.333(2) . ?
C10 N16 1.360(3) . ?
N10 O13 1.225(2) . ?
N10 O14 1.235(2) . ?
N11 N12 1.309(2) . ?
N13 H13A 0.8800 . ?
N13 H13B 0.8800 . ?
N14 N15 1.365(2) . ?
N17 O11 1.254(2) . ?
N17 O12 1.255(2) . ?
N18 O10 1.249(2) . ?
N18 O9 1.251(2) . ?
N19 H19A 1.0005 . ?
N19 H19B 0.9112 . ?
N19 H19C 0.9609 . ?
N19 H19D 0.8950 . ?
N20 H20A 0.8860 . ?
N20 H20B 0.8983 . ?
N20 H20C 0.8773 . ?
N20 H20D 0.8623 . ?
O1 H1A 0.8341 . ?
O1 H1B 0.8905 . ?
O2 H2A 0.8427 . ?
O2 H2B 0.8819 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 122.58(17) . . ?
N1 C1 C2 117.26(17) . . ?
N2 C1 C2 119.50(17) . . ?
N4 C2 N3 116.47(17) . . ?
N4 C2 C1 122.54(17) . . ?
N3 C2 C1 120.99(18) . . ?
N3 C3 N6 128.2(2) . . ?
N3 C3 N5 109.24(16) . . ?
N6 C3 N5 122.50(19) . . ?
N8 C4 N5 119.20(18) . . ?
N8 C4 C5 130.6(2) . . ?
N5 C4 C5 110.17(18) . . ?
N7 C5 C4 124.82(19) . . ?
N7 C5 N9 114.05(17) . . ?
C4 C5 N9 121.09(18) . . ?
O4 N1 O3 120.18(17) . . ?
O4 N1 C1 116.05(17) . . ?
O3 N1 C1 123.77(17) . . ?
O5 N2 O6 121.07(17) . . ?
O5 N2 C1 123.15(16) . . ?
O6 N2 C1 115.78(16) . . ?
C3 N3 C2 102.89(17) . . ?
C2 N4 N5 101.19(15) . . ?
C4 N5 N4 125.99(17) . . ?
C4 N5 C3 123.80(16) . . ?
N4 N5 C3 110.19(16) . . ?
N7 N6 C3 115.29(18) . . ?
N6 N7 C5 123.34(17) . . ?
C4 N8 H8A 120.0 . . ?
C4 N8 H8B 120.0 . . ?
H8A N8 H8B 120.0 . . ?
O7 N9 O8 124.27(18) . . ?
O7 N9 C5 119.10(19) . . ?
O8 N9 C5 116.62(16) . . ?
N12 C6 C7 125.98(18) . . ?
N12 C6 N10 113.52(17) . . ?
C7 C6 N10 120.44(18) . . ?
N13 C7 N14 118.51(18) . . ?
N13 C7 C6 132.07(18) . . ?
N14 C7 C6 109.41(18) . . ?
N16 C8 N11 128.00(19) . . ?
N16 C8 N14 108.82(17) . . ?
N11 C8 N14 123.18(18) . . ?
N17 C9 N18 123.25(18) . . ?
N17 C9 C10 118.18(18) . . ?
N18 C9 C10 118.31(18) . . ?
N15 C10 N16 116.04(18) . . ?
N15 C10 C9 122.19(18) . . ?
N16 C10 C9 121.76(17) . . ?
O13 N10 O14 123.50(17) . . ?
O13 N10 C6 119.35(17) . . ?
O14 N10 C6 117.14(17) . . ?
N12 N11 C8 115.36(17) . . ?
N11 N12 C6 122.53(18) . . ?
C7 N13 H13A 120.0 . . ?
C7 N13 H13B 120.0 . . ?
H13A N13 H13B 120.0 . . ?
N15 N14 C8 110.83(15) . . ?
N15 N14 C7 125.69(17) . . ?
C8 N14 C7 123.45(17) . . ?
C10 N15 N14 100.96(16) . . ?
C8 N16 C10 103.34(16) . . ?
O11 N17 O12 120.91(17) . . ?
O11 N17 C9 116.24(16) . . ?
O12 N17 C9 122.85(17) . . ?
O10 N18 O9 120.38(18) . . ?
O10 N18 C9 123.46(18) . . ?
O9 N18 C9 116.16(17) . . ?
H19A N19 H19B 109.0 . . ?
H19A N19 H19C 108.7 . . ?
H19B N19 H19C 108.5 . . ?
H19A N19 H19D 109.2 . . ?
H19B N19 H19D 113.5 . . ?
H19C N19 H19D 107.8 . . ?
H20A N20 H20B 113.0 . . ?
H20A N20 H20C 108.2 . . ?
H20B N20 H20C 110.5 . . ?
H20A N20 H20D 116.1 . . ?
H20B N20 H20D 99.5 . . ?
H20C N20 H20D 109.3 . . ?
H1A O1 H1B 110.5 . . ?
H2A O2 H2B 107.7 . . ?

_refine_diff_density_max         0.307
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.064

####################################################################### 
# 
# 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_mo_20211050_0m
_database_code_depnum_ccdc_archive 'CCDC 2151871'
_audit_update_record             
;
2022-09-20 deposited with the CCDC.	2023-02-13 downloaded from the CCDC.
;
_audit_creation_date             2021-07-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C5 H3 Cl N8 O3), C H4 O, C2 H3 N'
_chemical_formula_sum            'C13 H13 Cl2 N17 O7'
_chemical_formula_weight         590.30
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   17.345(3)
_cell_length_b                   5.5381(9)
_cell_length_c                   25.004(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.662(5)
_cell_angle_gamma                90
_cell_volume                     2312.6(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    943
_cell_measurement_temperature    140
_cell_measurement_theta_max      24.53
_cell_measurement_theta_min      2.44
_shelx_estimated_absorpt_T_max   0.989
_shelx_estimated_absorpt_T_min   0.962
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1230 before and 0.0674 after correction. The Ratio of minimum to maximum transmission is 0.8209. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1202
_diffrn_reflns_av_unetI/netI     0.1678
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11145
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.770
_diffrn_reflns_theta_min         2.439
_diffrn_ambient_temperature      140.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2177
_reflns_number_total             4383
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4383
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1786
_refine_ls_R_factor_gt           0.0768
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0438P)²+2.7648P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1758
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Tetrahedral OH refined with riding coordinates:
 O1(H1)
2.b X=CH2 refined with riding coordinates:
 N15(H15A,H15B), N4(H4A,H4B)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl2 Cl 0.31654(9) 0.8184(3) 0.27011(6) 0.0305(4) Uani 1 1 d . . . . .
Cl1 Cl -0.07887(9) 1.2506(3) 0.36163(7) 0.0375(5) Uani 1 1 d . . . . .
O4 O 0.3644(2) 0.7456(8) 0.47201(16) 0.0252(10) Uani 1 1 d . . . . .
O6 O 0.7300(2) 1.6051(8) 0.48115(16) 0.0274(11) Uani 1 1 d . . . . .
O2 O 0.4441(2) 0.9848(8) 0.44276(16) 0.0260(10) Uani 1 1 d . . . . .
O5 O 0.6113(2) 1.7646(8) 0.45785(15) 0.0264(10) Uani 1 1 d . . . . .
O007 O 0.6357(3) 1.4724(9) 0.28619(19) 0.0300(12) Uani 1 1 d . . . . .
O3 O 0.3723(3) 0.4372(8) 0.21730(17) 0.0317(11) Uani 1 1 d . . . . .
H3 H 0.389396 0.315952 0.203878 0.048 Uiso 1 1 calc GR . . . .
O1 O -0.1107(2) 1.6607(8) 0.29147(18) 0.0354(12) Uani 1 1 d . . . . .
H1 H -0.135928 1.531240 0.282016 0.053 Uiso 1 1 calc R . . . .
N8 N 0.3772(3) 0.9297(9) 0.44760(19) 0.0204(12) Uani 1 1 d . . . . .
N5 N 0.1780(3) 1.1869(9) 0.39896(19) 0.0188(11) Uani 1 1 d . . . . .
N10 N 0.5311(3) 1.1809(9) 0.35993(19) 0.0211(12) Uani 1 1 d . . . . .
N3 N 0.0977(3) 1.1763(9) 0.39286(19) 0.0224(12) Uani 1 1 d . . . . .
N7 N 0.3283(3) 1.2801(9) 0.39732(18) 0.0228(12) Uani 1 1 d . . . . .
N11 N 0.4565(3) 1.0984(9) 0.33198(19) 0.0208(12) Uani 1 1 d . . . . .
N16 N 0.6592(3) 1.6045(9) 0.45363(19) 0.0225(12) Uani 1 1 d . . . . .
N15 N 0.4856(3) 1.4916(9) 0.4047(2) 0.0240(12) Uani 1 1 d . . . . .
H15A H 0.436355 1.442513 0.389233 0.029 Uiso 1 1 calc R . . . .
H15B H 0.494047 1.617795 0.426942 0.029 Uiso 1 1 calc R . . . .
N6 N 0.2741(3) 1.4377(9) 0.37194(19) 0.0231(12) Uani 1 1 d . . . . .
N2 N 0.1311(3) 1.5036(9) 0.3472(2) 0.0243(12) Uani 1 1 d . . . . .
N14 N 0.6867(3) 1.2620(10) 0.40725(19) 0.0252(12) Uani 1 1 d . . . . .
N4 N 0.2077(3) 0.8507(9) 0.45473(19) 0.0226(12) Uani 1 1 d . . . . .
H4A H 0.156689 0.842280 0.453933 0.027 Uiso 1 1 calc R . . . .
H4B H 0.241655 0.743235 0.473595 0.027 Uiso 1 1 calc R . . . .
N1 N -0.0304(3) 1.6133(9) 0.3084(2) 0.0264(13) Uani 1 1 d . . . . .
N9 N 0.4364(3) 0.5695(10) 0.2487(2) 0.0272(13) Uani 1 1 d . . . . .
N13 N 0.6697(3) 1.0730(10) 0.3745(2) 0.0269(13) Uani 1 1 d . . . . .
N12 N 0.5562(3) 0.8594(9) 0.3165(2) 0.0253(13) Uani 1 1 d . . . . .
C10 C 0.2330(3) 1.0240(11) 0.4277(2) 0.0200(14) Uani 1 1 d . . . . .
C9 C 0.1972(4) 1.3797(11) 0.3713(2) 0.0202(14) Uani 1 1 d . . . . .
C16 C 0.6298(3) 1.4100(11) 0.4153(2) 0.0177(13) Uani 1 1 d . . . . .
C8 C 0.0737(3) 1.3713(11) 0.3613(2) 0.0204(14) Uani 1 1 d . . . . .
C15 C 0.5459(3) 1.3776(11) 0.3948(2) 0.0202(14) Uani 1 1 d . . . . .
N17 N 1.0460(4) 0.7379(11) 0.4644(2) 0.0419(16) Uani 1 1 d . . . . .
C13 C 0.4761(4) 0.9036(11) 0.3072(2) 0.0200(14) Uani 1 1 d . . . . .
C12 C 0.4130(3) 0.7477(12) 0.2731(2) 0.0208(14) Uani 1 1 d . . . . .
C11 C 0.3098(3) 1.0831(11) 0.4225(2) 0.0217(14) Uani 1 1 d . . . . .
C14 C 0.5897(4) 1.0375(11) 0.3497(2) 0.0251(15) Uani 1 1 d . . . . .
C7 C -0.0119(3) 1.4305(12) 0.3405(2) 0.0242(15) Uani 1 1 d . . . . .
C19 C 0.9789(4) 0.7465(13) 0.4575(3) 0.0358(18) Uani 1 1 d . . . . .
C17 C 0.7153(4) 1.5678(13) 0.2965(3) 0.0374(18) Uani 1 1 d . . . . .
H17A H 0.723897 1.627076 0.261607 0.056 Uiso 1 1 calc GR . . . .
H17B H 0.754274 1.440432 0.311746 0.056 Uiso 1 1 calc GR . . . .
H17C H 0.722165 1.701105 0.323140 0.056 Uiso 1 1 calc GR . . . .
C18 C 0.8914(4) 0.7530(14) 0.4473(3) 0.047(2) Uani 1 1 d . . . . .
H18A H 0.866034 0.718605 0.408017 0.070 Uiso 1 1 calc GR . . . .
H18B H 0.875037 0.913468 0.456581 0.070 Uiso 1 1 calc GR . . . .
H18C H 0.874896 0.631347 0.470406 0.070 Uiso 1 1 calc GR . . . .
H007 H 0.608(4) 1.582(13) 0.287(3) 0.04(3) Uiso 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
Cl2 C12 1.700(6) . ?
Cl1 C7 1.718(6) . ?
O4 N8 1.239(6) . ?
O6 N16 1.235(6) . ?
O2 N8 1.237(6) . ?
O5 N16 1.239(6) . ?
O007 C17 1.435(7) . ?
O3 N9 1.385(6) . ?
O1 N1 1.368(6) . ?
N8 C11 1.444(7) . ?
N5 N3 1.360(6) . ?
N5 C10 1.367(7) . ?
N5 C9 1.361(7) . ?
N10 N11 1.373(6) . ?
N10 C15 1.375(7) . ?
N10 C14 1.366(7) . ?
N3 C8 1.336(7) . ?
N7 N6 1.314(6) . ?
N7 C11 1.342(7) . ?
N11 C13 1.333(7) . ?
N16 C16 1.440(7) . ?
N15 C15 1.302(7) . ?
N6 C9 1.369(7) . ?
N2 C9 1.332(7) . ?
N2 C8 1.356(7) . ?
N14 N13 1.312(7) . ?
N14 C16 1.340(7) . ?
N4 C10 1.316(7) . ?
N1 C7 1.277(7) . ?
N9 C12 1.282(7) . ?
N13 C14 1.373(7) . ?
N12 C13 1.368(7) . ?
N12 C14 1.319(8) . ?
C10 C11 1.411(8) . ?
C16 C15 1.417(8) . ?
C8 C7 1.473(8) . ?
N17 C19 1.130(8) . ?
C13 C12 1.472(8) . ?
C19 C18 1.469(9) . ?

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
O4 N8 C11 117.8(5) . . ?
O2 N8 O4 123.3(5) . . ?
O2 N8 C11 118.9(5) . . ?
N3 N5 C10 125.3(5) . . ?
N3 N5 C9 111.1(5) . . ?
C9 N5 C10 123.6(5) . . ?
N11 N10 C15 125.1(5) . . ?
C14 N10 N11 111.0(5) . . ?
C14 N10 C15 123.9(5) . . ?
C8 N3 N5 100.2(5) . . ?
N6 N7 C11 122.4(5) . . ?
C13 N11 N10 100.5(5) . . ?
O6 N16 O5 122.6(5) . . ?
O6 N16 C16 119.6(5) . . ?
O5 N16 C16 117.8(5) . . ?
N7 N6 C9 114.7(5) . . ?
C9 N2 C8 101.9(5) . . ?
N13 N14 C16 122.1(5) . . ?
C7 N1 O1 114.0(5) . . ?
C12 N9 O3 111.6(5) . . ?
N14 N13 C14 115.2(5) . . ?
C14 N12 C13 103.1(5) . . ?
N5 C10 C11 110.0(5) . . ?
N4 C10 N5 117.9(5) . . ?
N4 C10 C11 132.1(6) . . ?
N5 C9 N6 123.3(5) . . ?
N2 C9 N5 109.6(5) . . ?
N2 C9 N6 127.0(6) . . ?
N14 C16 N16 114.5(5) . . ?
N14 C16 C15 126.4(5) . . ?
C15 C16 N16 118.8(5) . . ?
N3 C8 N2 117.2(5) . . ?
N3 C8 C7 120.8(5) . . ?
N2 C8 C7 121.9(5) . . ?
N10 C15 C16 109.1(5) . . ?
N15 C15 N10 118.9(5) . . ?
N15 C15 C16 131.9(6) . . ?
N11 C13 N12 116.2(5) . . ?
N11 C13 C12 120.1(5) . . ?
N12 C13 C12 123.7(6) . . ?
N9 C12 Cl2 126.2(5) . . ?
N9 C12 C13 116.5(5) . . ?
C13 C12 Cl2 117.3(5) . . ?
N7 C11 N8 114.5(5) . . ?
N7 C11 C10 125.7(5) . . ?
C10 C11 N8 119.8(6) . . ?
N10 C14 N13 122.9(5) . . ?
N12 C14 N10 109.2(5) . . ?
N12 C14 N13 127.7(6) . . ?
N1 C7 Cl1 125.3(5) . . ?
N1 C7 C8 117.1(5) . . ?
C8 C7 Cl1 117.6(5) . . ?
N17 C19 C18 178.5(8) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_20211860_0m
_database_code_depnum_ccdc_archive 'CCDC 2151873'
_audit_update_record             
;
2022-09-20 deposited with the CCDC.	2023-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H10 K2 N18 O15'
_chemical_formula_weight         700.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   43.231(8)
_cell_length_b                   9.0006(15)
_cell_length_c                   12.327(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.157(5)
_cell_angle_gamma                90
_cell_volume                     4689.0(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    1909
_cell_measurement_theta_min      2.686
_cell_measurement_theta_max      24.101

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_F_000             2832
_exptl_transmission_factor_min   0.864
_exptl_transmission_factor_max   0.864
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.522
_shelx_estimated_absorpt_T_min   0.959
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ccd
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18926
_diffrn_reflns_av_unetI/netI     0.0944
_diffrn_reflns_av_R_equivalents  0.1119
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.314
_diffrn_reflns_theta_max         25.376
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             4254
_reflns_number_gt                2497
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0469P)²+10.6122P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4254
_refine_ls_number_parameters     412
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0593
_refine_ls_wR_factor_ref         0.1456
_refine_ls_wR_factor_gt          0.1144
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
C1 C 0.68182(12) 1.2058(5) 0.4129(4) 0.0262(12) Uani 1 1 d . . . . .
C2 C 0.65671(12) 1.3042(5) 0.4217(4) 0.0224(12) Uani 1 1 d . . . . .
C3 C 0.63230(12) 1.5053(5) 0.4269(4) 0.0221(11) Uani 1 1 d . . . . .
C4 C 0.57961(12) 1.4072(5) 0.4073(4) 0.0211(11) Uani 1 1 d . . . . .
C5 C 0.57225(12) 1.5604(5) 0.4101(4) 0.0217(11) Uani 1 1 d . . . . .
C6 C 0.54655(12) -0.0575(5) 0.6410(4) 0.0223(12) Uani 1 1 d . . . . .
C7 C 0.55416(11) 0.0971(5) 0.6442(4) 0.0200(11) Uani 1 1 d . . . . .
C8 C 0.60687(11) 0.9974(5) 0.6702(4) 0.0191(11) Uani 1 1 d . . . . .
C9 C 0.63219(12) 0.1972(5) 0.6808(4) 0.0198(11) Uani 1 1 d . . . . .
C10 C 0.65956(12) 0.2937(5) 0.6957(4) 0.0237(12) Uani 1 1 d . . . . .
K1 K 0.66483(3) 0.80292(12) 0.61579(10) 0.0344(3) Uani 1 1 d . . . . .
K2 K 0.74502(3) 0.53369(12) 0.69524(11) 0.0360(3) Uani 1 1 d . . . . .
N1 N 0.68121(10) 1.0560(4) 0.4211(3) 0.0266(10) Uani 1 1 d . . . . .
N2 N 0.71112(11) 1.2692(5) 0.3969(4) 0.0366(12) Uani 1 1 d . . . . .
N3 N 0.66101(10) 1.4548(4) 0.4312(3) 0.0247(10) Uani 1 1 d . . . . .
N4 N 0.61116(9) 1.3899(4) 0.4161(3) 0.0200(9) Uani 1 1 d . . . . .
N5 N 0.62642(10) 1.2573(4) 0.4136(3) 0.0218(10) Uani 1 1 d . . . . .
N6 N 0.56107(9) 1.2912(4) 0.3977(3) 0.0228(10) Uani 1 1 d . . . . .
H6A H 0.5691 1.2014 0.3970 0.027 Uiso 1 1 calc R U . . .
H6B H 0.5406 1.3029 0.3920 0.027 Uiso 1 1 calc R U . . .
N7 N 0.59282(10) 1.6717(4) 0.4226(3) 0.0223(10) Uani 1 1 d . . . . .
N8 N 0.62333(10) 1.6486(4) 0.4319(3) 0.0246(10) Uani 1 1 d . . . . .
N9 N 0.53975(10) 1.6093(5) 0.3969(3) 0.0270(10) Uani 1 1 d . . . . .
N10 N 0.53596(10) 0.2127(4) 0.6354(3) 0.0257(10) Uani 1 1 d . . . . .
H10A H 0.5442 0.3024 0.6381 0.031 Uiso 1 1 calc R U . . .
H10B H 0.5154 0.2015 0.6266 0.031 Uiso 1 1 calc R U . . .
N11 N 0.51449(10) -0.1069(4) 0.6282(3) 0.0265(10) Uani 1 1 d . . . . .
N12 N 0.59771(10) 0.8529(4) 0.6637(3) 0.0240(10) Uani 1 1 d . . . . .
N13 N 0.56722(10) -0.1691(4) 0.6497(3) 0.0248(10) Uani 1 1 d . . . . .
N14 N 0.58615(9) 0.1144(4) 0.6578(3) 0.0191(9) Uani 1 1 d . . . . .
N15 N 0.60211(9) 0.2457(4) 0.6642(3) 0.0199(9) Uani 1 1 d . . . . .
N16 N 0.63596(9) 1.0464(4) 0.6854(3) 0.0223(10) Uani 1 1 d . . . . .
N17 N 0.65759(10) 0.4446(4) 0.6920(3) 0.0234(10) Uani 1 1 d . . . . .
N18 N 0.69043(10) 0.2303(4) 0.7111(4) 0.0258(10) Uani 1 1 d . . . . .
O1 O 0.70572(9) 0.9795(4) 0.4177(3) 0.0346(9) Uani 1 1 d . . . . .
O2 O 0.65662(9) 0.9924(4) 0.4359(3) 0.0307(9) Uani 1 1 d . . . . .
O3 O 0.71106(11) 0.6851(4) 0.5201(3) 0.0437(11) Uani 1 1 d D . . . .
H3A H 0.7044(15) 0.604(4) 0.485(5) 0.066 Uiso 1 1 d D U . . .
H3B H 0.7121(15) 0.762(4) 0.479(4) 0.066 Uiso 1 1 d D U . . .
O4 O 0.72157(10) 1.2269(4) 0.3157(4) 0.0484(11) Uani 1 1 d . . . . .
O5 O 0.72362(10) 1.3674(5) 0.4603(4) 0.0706(16) Uani 1 1 d . . . . .
O7 O 0.51900(8) 1.5144(4) 0.3851(3) 0.0382(10) Uani 1 1 d . . . . .
O8 O 0.53443(8) 1.7429(4) 0.3968(3) 0.0357(10) Uani 1 1 d . . . . .
O9 O 0.49366(8) -0.0128(4) 0.6178(3) 0.0363(10) Uani 1 1 d . . . . .
O10 O 0.50930(9) -0.2404(4) 0.6297(3) 0.0431(11) Uani 1 1 d . . . . .
O11 O 0.63094(8) 0.5053(3) 0.6781(3) 0.0278(8) Uani 1 1 d . . . . .
O12 O 0.68167(8) 0.5259(3) 0.6984(3) 0.0301(9) Uani 1 1 d . . . . .
O13 O 0.71334(8) 0.2919(4) 0.7733(3) 0.0338(9) Uani 1 1 d . . . . .
O14 O 0.69391(8) 1.1115(4) 0.6644(3) 0.0373(10) Uani 1 1 d . . . . .
O15 O 0.43880(8) 0.4981(3) 0.3453(3) 0.0341(9) Uani 1 1 d . . . . .
H15A H 0.4184 0.5019 0.3397 0.051 Uiso 1 1 d R U . . .
H15B H 0.4426 0.4239 0.3440 0.051 Uiso 1 1 d R U . . .
O6 O 0.58625(8) 1.0000(3) 0.4064(3) 0.0341(9) Uani 1 1 d . . . . .
H6C H 0.6067 1.0105 0.4259 0.051 Uiso 1 1 d R U . . .
H6D H 0.5830 0.9177 0.4094 0.051 Uiso 1 1 d R 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
C1 N1 1.353(6) . ?
C1 C2 1.423(7) . ?
C1 N2 1.440(7) . ?
C2 N5 1.359(6) . ?
C2 N3 1.370(6) . ?
C3 N3 1.312(6) . ?
C3 N8 1.352(6) . ?
C3 N4 1.372(6) . ?
C4 N6 1.307(6) . ?
C4 N4 1.354(6) . ?
C4 C5 1.417(6) . ?
C5 N7 1.327(6) . ?
C5 N9 1.448(6) . ?
C6 N13 1.334(6) . ?
C6 C7 1.428(6) . ?
C6 N11 1.432(6) . ?
C7 N10 1.295(6) . ?
C7 N14 1.366(6) . ?
C8 N16 1.308(6) . ?
C8 N12 1.357(6) . ?
C8 N14 1.371(6) 1_565 ?
C9 N15 1.346(6) . ?
C9 N16 1.367(6) 1_545 ?
C9 C10 1.448(7) . ?
C10 N17 1.361(6) . ?
C10 N18 1.427(6) . ?
K1 O12 2.734(3) . ?
K1 O3 2.739(5) . ?
K1 N16 2.747(4) . ?
K1 O2 2.760(4) . ?
K1 N8 2.928(4) 1_545 ?
K1 O14 3.056(4) . ?
K1 O4 3.101(5) 6_576 ?
K1 N12 3.113(4) . ?
K1 O11 3.222(3) . ?
K1 N17 3.392(4) . ?
K1 K2 4.1736(17) . ?
K1 K2 4.5943(18) 4_656 ?
K1 H3B 2.94(6) . ?
K2 O3 2.709(4) . ?
K2 O12 2.748(4) . ?
K2 O4 2.773(4) 7_666 ?
K2 O1 2.782(4) 7_666 ?
K2 O13 2.845(4) . ?
K2 O13 2.915(4) 4_656 ?
K2 O4 2.917(4) 6_576 ?
K2 O14 2.921(4) 4_646 ?
K2 O5 3.218(5) 1_545 ?
K2 N18 3.301(4) 4_656 ?
K2 K1 4.5943(18) 4_646 ?
K2 H3A 2.88(6) . ?
N1 O2 1.254(5) . ?
N1 O1 1.272(5) . ?
N2 O5 1.227(6) . ?
N2 O4 1.242(6) . ?
N4 N5 1.367(5) . ?
N6 H6A 0.8800 . ?
N6 H6B 0.8800 . ?
N7 N8 1.316(5) . ?
N8 K1 2.928(4) 1_565 ?
N9 O8 1.225(5) . ?
N9 O7 1.225(5) . ?
N10 H10A 0.8800 . ?
N10 H10B 0.8800 . ?
N11 O9 1.223(5) . ?
N11 O10 1.224(5) . ?
N12 N13 1.308(5) 1_565 ?
N13 N12 1.308(5) 1_545 ?
N14 N15 1.362(5) . ?
N14 C8 1.371(6) 1_545 ?
N16 C9 1.367(6) 1_565 ?
N17 O11 1.254(5) . ?
N17 O12 1.261(5) . ?
N18 O14 1.239(5) 1_545 ?
N18 O13 1.248(5) . ?
N18 K2 3.301(4) 4_646 ?
O1 K2 2.782(4) 7_666 ?
O3 H3A 0.87(2) . ?
O3 H3B 0.87(2) . ?
O4 K2 2.773(4) 7_666 ?
O4 K2 2.917(4) 6_575 ?
O4 K1 3.101(5) 6_575 ?
O5 K2 3.218(5) 1_565 ?
O13 K2 2.915(4) 4_646 ?
O14 N18 1.239(5) 1_565 ?
O14 K2 2.921(4) 4_656 ?
O15 H15A 0.8699 . ?
O15 H15B 0.6889 . ?
O6 H6C 0.8706 . ?
O6 H6D 0.7565 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 126.0(5) . . ?
N1 C1 N2 115.9(4) . . ?
C2 C1 N2 118.1(4) . . ?
N5 C2 N3 115.2(4) . . ?
N5 C2 C1 122.6(4) . . ?
N3 C2 C1 122.0(5) . . ?
N3 C3 N8 127.3(4) . . ?
N3 C3 N4 110.3(4) . . ?
N8 C3 N4 122.4(4) . . ?
N6 C4 N4 120.2(4) . . ?
N6 C4 C5 130.0(5) . . ?
N4 C4 C5 109.7(4) . . ?
N7 C5 C4 126.1(5) . . ?
N7 C5 N9 113.2(4) . . ?
C4 C5 N9 120.7(4) . . ?
N13 C6 C7 125.8(5) . . ?
N13 C6 N11 113.0(4) . . ?
C7 C6 N11 121.1(4) . . ?
N10 C7 N14 120.0(4) . . ?
N10 C7 C6 130.4(5) . . ?
N14 C7 C6 109.6(4) . . ?
N16 C8 N12 126.3(4) . . ?
N16 C8 N14 110.0(4) . 1_565 ?
N12 C8 N14 123.7(4) . 1_565 ?
N15 C9 N16 115.6(4) . 1_545 ?
N15 C9 C10 124.2(4) . . ?
N16 C9 C10 120.2(4) 1_545 . ?
N17 C10 N18 117.0(4) . . ?
N17 C10 C9 123.4(5) . . ?
N18 C10 C9 119.6(4) . . ?
O12 K1 O3 69.26(11) . . ?
O12 K1 N16 135.59(12) . . ?
O3 K1 N16 149.76(13) . . ?
O12 K1 O2 147.33(11) . . ?
O3 K1 O2 82.84(12) . . ?
N16 K1 O2 76.58(11) . . ?
O12 K1 N8 85.84(11) . 1_545 ?
O3 K1 N8 82.35(13) . 1_545 ?
N16 K1 N8 112.06(12) . 1_545 ?
O2 K1 N8 73.56(11) . 1_545 ?
O12 K1 O14 133.62(11) . . ?
O3 K1 O14 97.41(12) . . ?
N16 K1 O14 53.76(11) . . ?
O2 K1 O14 64.77(10) . . ?
N8 K1 O14 137.95(11) 1_545 . ?
O12 K1 O4 61.38(10) . 6_576 ?
O3 K1 O4 77.40(12) . 6_576 ?
N16 K1 O4 98.98(12) . 6_576 ?
O2 K1 O4 129.65(11) . 6_576 ?
N8 K1 O4 145.84(11) 1_545 6_576 ?
O14 K1 O4 72.48(10) . 6_576 ?
O12 K1 N12 104.30(11) . . ?
O3 K1 N12 158.65(12) . . ?
N16 K1 N12 47.37(11) . . ?
O2 K1 N12 95.50(11) . . ?
N8 K1 N12 76.80(11) 1_545 . ?
O14 K1 N12 101.12(10) . . ?
O4 K1 N12 118.34(11) 6_576 . ?
O12 K1 O11 41.56(9) . . ?
O3 K1 O11 100.97(11) . . ?
N16 K1 O11 109.25(11) . . ?
O2 K1 O11 135.81(10) . . ?
N8 K1 O11 63.58(10) 1_545 . ?
O14 K1 O11 153.87(10) . . ?
O4 K1 O11 93.55(10) 6_576 . ?
N12 K1 O11 65.56(9) . . ?
O12 K1 N17 20.35(10) . . ?
O3 K1 N17 82.49(11) . . ?
N16 K1 N17 126.70(12) . . ?
O2 K1 N17 143.72(10) . . ?
N8 K1 N17 71.72(10) 1_545 . ?
O14 K1 N17 150.25(10) . . ?
O4 K1 N17 78.54(10) 6_576 . ?
N12 K1 N17 86.61(10) . . ?
O11 K1 N17 21.66(9) . . ?
O12 K1 K2 40.54(8) . . ?
O3 K1 K2 39.72(9) . . ?
N16 K1 K2 143.07(9) . . ?
O2 K1 K2 120.47(9) . . ?
N8 K1 K2 104.46(9) 1_545 . ?
O14 K1 K2 101.22(8) . . ?
O4 K1 K2 44.30(7) 6_576 . ?
N12 K1 K2 143.20(8) . . ?
O11 K1 K2 81.85(7) . . ?
N17 K1 K2 60.23(8) . . ?
O12 K1 K2 95.31(8) . 4_656 ?
O3 K1 K2 77.02(9) . 4_656 ?
N16 K1 K2 82.74(9) . 4_656 ?
O2 K1 K2 94.58(8) . 4_656 ?
N8 K1 K2 157.38(9) 1_545 4_656 ?
O14 K1 K2 38.70(7) . 4_656 ?
O4 K1 K2 36.05(8) 6_576 4_656 ?
N12 K1 K2 124.30(8) . 4_656 ?
O11 K1 K2 129.40(7) . 4_656 ?
N17 K1 K2 114.04(8) . 4_656 ?
K2 K1 K2 64.50(2) . 4_656 ?
O12 K1 H3B 86.3(6) . . ?
O3 K1 H3B 17.1(6) . . ?
N16 K1 H3B 134.2(7) . . ?
O2 K1 H3B 66.6(7) . . ?
N8 K1 H3B 83.2(12) 1_545 . ?
O14 K1 H3B 85.4(10) . . ?
O4 K1 H3B 85.2(11) 6_576 . ?
N12 K1 H3B 156.5(11) . . ?
O11 K1 H3B 116.0(8) . . ?
N17 K1 H3B 99.0(6) . . ?
K2 K1 H3B 54.4(8) . . ?
K2 K1 H3B 74.3(12) 4_656 . ?
O3 K2 O12 69.49(12) . . ?
O3 K2 O4 125.97(14) . 7_666 ?
O12 K2 O4 120.66(11) . 7_666 ?
O3 K2 O1 88.06(13) . 7_666 ?
O12 K2 O1 151.20(12) . 7_666 ?
O4 K2 O1 58.53(11) 7_666 7_666 ?
O3 K2 O13 115.83(12) . . ?
O12 K2 O13 54.80(10) . . ?
O4 K2 O13 70.25(11) 7_666 . ?
O1 K2 O13 127.62(11) 7_666 . ?
O3 K2 O13 85.46(12) . 4_656 ?
O12 K2 O13 127.44(10) . 4_656 ?
O4 K2 O13 111.55(12) 7_666 4_656 ?
O1 K2 O13 65.43(10) 7_666 4_656 ?
O13 K2 O13 153.21(6) . 4_656 ?
O3 K2 O4 81.13(13) . 6_576 ?
O12 K2 O4 63.74(11) . 6_576 ?
O4 K2 O4 152.88(7) 7_666 6_576 ?
O1 K2 O4 132.15(11) 7_666 6_576 ?
O13 K2 O4 98.59(12) . 6_576 ?
O13 K2 O4 67.32(11) 4_656 6_576 ?
O3 K2 O14 128.47(12) . 4_646 ?
O12 K2 O14 140.98(12) . 4_646 ?
O4 K2 O14 79.43(12) 7_666 4_646 ?
O1 K2 O14 67.36(11) 7_666 4_646 ?
O13 K2 O14 114.99(11) . 4_646 ?
O13 K2 O14 43.46(10) 4_656 4_646 ?
O4 K2 O14 83.62(12) 6_576 4_646 ?
O3 K2 O5 60.80(12) . 1_545 ?
O12 K2 O5 84.39(11) . 1_545 ?
O4 K2 O5 67.46(12) 7_666 1_545 ?
O1 K2 O5 68.59(11) 7_666 1_545 ?
O13 K2 O5 83.15(12) . 1_545 ?
O13 K2 O5 122.90(12) 4_656 1_545 ?
O4 K2 O5 137.46(12) 6_576 1_545 ?
O14 K2 O5 134.23(11) 4_646 1_545 ?
O3 K2 N18 106.59(12) . 4_656 ?
O12 K2 N18 141.30(11) . 4_656 ?
O4 K2 N18 93.43(12) 7_666 4_656 ?
O1 K2 N18 61.19(11) 7_666 4_656 ?
O13 K2 N18 136.35(11) . 4_656 ?
O13 K2 N18 22.05(9) 4_656 4_656 ?
O4 K2 N18 77.57(11) 6_576 4_656 ?
O14 K2 N18 21.89(9) 4_646 4_656 ?
O5 K2 N18 128.75(12) 1_545 4_656 ?
O3 K2 K1 40.26(10) . . ?
O12 K2 K1 40.29(7) . . ?
O4 K2 K1 153.54(10) 7_666 . ?
O1 K2 K1 126.37(8) 7_666 . ?
O13 K2 K1 95.07(8) . . ?
O13 K2 K1 91.58(8) 4_656 . ?
O4 K2 K1 47.94(9) 6_576 . ?
O14 K2 K1 127.03(8) 4_646 . ?
O5 K2 K1 89.53(8) 1_545 . ?
N18 K2 K1 111.72(8) 4_656 . ?
O3 K2 K1 153.01(10) . 4_646 ?
O12 K2 K1 136.29(8) . 4_646 ?
O4 K2 K1 41.16(10) 7_666 4_646 ?
O1 K2 K1 65.00(8) 7_666 4_646 ?
O13 K2 K1 84.26(8) . 4_646 ?
O13 K2 K1 81.88(8) 4_656 4_646 ?
O4 K2 K1 115.12(10) 6_576 4_646 ?
O14 K2 K1 40.85(7) 4_646 4_646 ?
O5 K2 K1 107.36(8) 1_545 4_646 ?
N18 K2 K1 60.04(8) 4_656 4_646 ?
K1 K2 K1 162.84(4) . 4_646 ?
O3 K2 H3A 17.5(6) . . ?
O12 K2 H3A 66.2(13) . . ?
O4 K2 H3A 111.6(9) 7_666 . ?
O1 K2 H3A 86.9(13) 7_666 . ?
O13 K2 H3A 103.1(10) . . ?
O13 K2 H3A 100.8(8) 4_656 . ?
O4 K2 H3A 94.8(9) 6_576 . ?
O14 K2 H3A 141.7(11) 4_646 . ?
O5 K2 H3A 44.5(8) 1_545 . ?
N18 K2 H3A 120.6(10) 4_656 . ?
K1 K2 H3A 48.8(11) . . ?
K1 K2 H3A 148.0(12) 4_646 . ?
O2 N1 O1 119.7(4) . . ?
O2 N1 C1 119.7(4) . . ?
O1 N1 C1 120.5(4) . . ?
O5 N2 O4 123.3(5) . . ?
O5 N2 C1 118.7(5) . . ?
O4 N2 C1 117.9(5) . . ?
C3 N3 C2 103.2(4) . . ?
C4 N4 N5 125.6(4) . . ?
C4 N4 C3 124.1(4) . . ?
N5 N4 C3 110.4(4) . . ?
C2 N5 N4 100.9(4) . . ?
C4 N6 H6A 120.0 . . ?
C4 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
N8 N7 C5 121.7(4) . . ?
N7 N8 C3 116.0(4) . . ?
N7 N8 K1 115.6(3) . 1_565 ?
C3 N8 K1 110.6(3) . 1_565 ?
O8 N9 O7 123.5(4) . . ?
O8 N9 C5 118.4(4) . . ?
O7 N9 C5 118.1(4) . . ?
C7 N10 H10A 120.0 . . ?
C7 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
O9 N11 O10 123.2(4) . . ?
O9 N11 C6 118.1(4) . . ?
O10 N11 C6 118.7(4) . . ?
N13 N12 C8 115.2(4) 1_565 . ?
N13 N12 K1 155.1(3) 1_565 . ?
C8 N12 K1 83.0(3) . . ?
N12 N13 C6 122.4(4) 1_545 . ?
N15 N14 C7 126.4(4) . . ?
N15 N14 C8 110.4(4) . 1_545 ?
C7 N14 C8 123.1(4) . 1_545 ?
C9 N15 N14 100.9(3) . . ?
C8 N16 C9 103.1(4) . 1_565 ?
C8 N16 K1 99.9(3) . . ?
C9 N16 K1 146.9(3) 1_565 . ?
O11 N17 O12 118.6(4) . . ?
O11 N17 C10 119.3(4) . . ?
O12 N17 C10 122.1(4) . . ?
O11 N17 K1 71.5(2) . . ?
O12 N17 K1 48.9(2) . . ?
C10 N17 K1 161.7(3) . . ?
O14 N18 O13 120.7(4) 1_545 . ?
O14 N18 C10 119.0(4) 1_545 . ?
O13 N18 C10 120.3(4) . . ?
O14 N18 K2 61.5(2) 1_545 4_646 ?
O13 N18 K2 61.3(2) . 4_646 ?
C10 N18 K2 163.6(3) . 4_646 ?
N1 O1 K2 140.4(3) . 7_666 ?
N1 O2 K1 115.4(3) . . ?
K2 O3 K1 100.02(14) . . ?
K2 O3 H3A 92(4) . . ?
K1 O3 H3A 110(4) . . ?
K2 O3 H3B 142(4) . . ?
K1 O3 H3B 95(4) . . ?
H3A O3 H3B 116(6) . . ?
N2 O4 K2 125.5(3) . 7_666 ?
N2 O4 K2 114.1(3) . 6_575 ?
K2 O4 K2 111.08(14) 7_666 6_575 ?
N2 O4 K1 107.8(3) . 6_575 ?
K2 O4 K1 102.79(14) 7_666 6_575 ?
K2 O4 K1 87.76(12) 6_575 6_575 ?
N2 O5 K2 155.9(4) . 1_565 ?
N17 O11 K1 86.8(2) . . ?
N17 O12 K1 110.8(3) . . ?
N17 O12 K2 145.7(3) . . ?
K1 O12 K2 99.17(11) . . ?
N18 O13 K2 120.5(3) . . ?
N18 O13 K2 96.7(3) . 4_646 ?
K2 O13 K2 109.10(12) . 4_646 ?
N18 O14 K2 96.6(3) 1_565 4_656 ?
N18 O14 K1 142.2(3) 1_565 . ?
K2 O14 K1 100.44(11) 4_656 . ?
H15A O15 H15B 106.0 . . ?
H6C O6 H6D 106.2 . . ?

_refine_diff_density_max         0.414
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.094

####################################################################### 
# 
# 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_mo_20211139_0m
_database_code_depnum_ccdc_archive 'CCDC 2151868'
_audit_update_record             
;
2022-09-20 deposited with the CCDC.	2023-02-13 downloaded from the CCDC.
;
_audit_creation_date             2021-07-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C5 H2 Cl K N9 O7.5'
_chemical_formula_sum            'C5 H2 Cl K N9 O7.50'
_chemical_formula_weight         382.71
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   21.576(4)
_cell_length_b                   7.2159(11)
_cell_length_c                   15.648(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.847(5)
_cell_angle_gamma                90
_cell_volume                     2427.5(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2748
_cell_measurement_temperature    170
_cell_measurement_theta_max      26.352
_cell_measurement_theta_min      2.613
_shelx_estimated_absorpt_T_max   0.971
_shelx_estimated_absorpt_T_min   0.918
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0835 before and 0.0666 after correction. The Ratio of minimum to maximum transmission is 0.8882. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.094
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8788
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.450
_diffrn_reflns_theta_min         1.894
_diffrn_ambient_temperature      170
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1771
_reflns_number_total             2486
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2486
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0482
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0417P)²+4.5816P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1129
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N7-H7 = O4-H4
 0.87 with sigma of 0.02
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.41531(4) -0.04551(10) 0.69521(5) 0.0261(2) Uani 1 1 d . . . . .
Cl1 Cl 0.26252(5) 0.60088(13) 0.90649(6) 0.0406(3) Uani 1 1 d . . . . .
O4 O 0.500000 0.2434(5) 0.750000 0.0279(8) Uani 1 2 d DS T P . .
O5 O 0.43298(12) -0.0149(3) 0.52409(16) 0.0325(6) Uani 1 1 d . . . . .
O8 O 0.44755(12) 0.5322(3) 0.38748(15) 0.0301(6) Uani 1 1 d . . . . .
O3 O 0.31938(12) 0.7272(3) 0.74124(17) 0.0369(7) Uani 1 1 d . . . . .
O6 O 0.42743(13) -0.0188(3) 0.38650(17) 0.0401(7) Uani 1 1 d . . . . .
O7 O 0.47089(12) 0.2761(4) 0.32472(15) 0.0376(7) Uani 1 1 d . . . . .
N8 N 0.44995(13) 0.3559(4) 0.38598(17) 0.0259(7) Uani 1 1 d . . . . .
N7 N 0.41118(14) 0.5489(4) 0.53747(18) 0.0241(7) Uani 1 1 d D . . . .
N2 N 0.34608(13) 0.4192(4) 0.72076(17) 0.0243(7) Uani 1 1 d . . . . .
N6 N 0.38739(13) 0.6019(4) 0.61172(17) 0.0248(7) Uani 1 1 d . . . . .
N5 N 0.38430(13) 0.2882(4) 0.59576(17) 0.0224(6) Uani 1 1 d . . . . .
O1 O 0.30507(14) 0.1971(4) 0.96374(18) 0.0487(8) Uani 1 1 d . . . . .
N9 N 0.43071(13) 0.0670(4) 0.45453(18) 0.0259(7) Uani 1 1 d . . . . .
N3 N 0.34027(13) 0.2558(4) 0.75842(17) 0.0264(7) Uani 1 1 d . . . . .
N1 N 0.32113(13) 0.5616(4) 0.76521(18) 0.0256(7) Uani 1 1 d . . . . .
N4 N 0.29951(15) 0.1538(4) 0.8889(2) 0.0349(8) Uani 1 1 d . . . . .
O2 O 0.28447(17) 0.0024(4) 0.8598(2) 0.0585(9) Uani 1 1 d . . . . .
C3 C 0.37276(15) 0.4401(4) 0.6417(2) 0.0206(7) Uani 1 1 d . . . . .
C2 C 0.31254(16) 0.2965(5) 0.8278(2) 0.0262(8) Uani 1 1 d . . . . .
C5 C 0.43041(16) 0.2637(5) 0.4559(2) 0.0228(8) Uani 1 1 d . . . . .
C4 C 0.40948(15) 0.3632(4) 0.5282(2) 0.0206(7) Uani 1 1 d . . . . .
C1 C 0.29988(16) 0.4822(5) 0.8352(2) 0.0263(8) Uani 1 1 d . . . . .
H7 H 0.4256(15) 0.630(4) 0.5061(19) 0.026(10) Uiso 1 1 d D . . . .
H4 H 0.4901(17) 0.314(4) 0.7877(19) 0.033(11) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 K1 3.9034(18) 2_656 ?
K1 O4 2.856(3) . ?
K1 O5 2.745(2) . ?
K1 O3 2.783(3) 1_545 ?
K1 O6 3.018(3) 6_556 ?
K1 O7 2.811(3) 6_556 ?
K1 O7 3.004(3) 5_656 ?
K1 N6 2.900(3) 1_545 ?
K1 N5 2.914(3) . ?
K1 N3 2.932(3) . ?
Cl1 C1 1.667(3) . ?
O4 H4 0.822(18) . ?
O4 H4 0.822(18) 2_656 ?
O5 N9 1.236(4) . ?
O8 N8 1.273(4) . ?
O3 N1 1.252(3) . ?
O6 N9 1.229(4) . ?
O7 N8 1.236(3) . ?
N8 C5 1.376(4) . ?
N7 N6 1.364(4) . ?
N7 C4 1.348(4) . ?
N7 H7 0.838(18) . ?
N2 N3 1.329(4) . ?
N2 N1 1.375(4) . ?
N2 C3 1.416(4) . ?
N6 C3 1.307(4) . ?
N5 C3 1.346(4) . ?
N5 C4 1.342(4) . ?
O1 N4 1.208(4) . ?
N9 C5 1.419(4) . ?
N3 C2 1.317(4) . ?
N1 C1 1.350(4) . ?
N4 O2 1.217(4) . ?
N4 C2 1.448(4) . ?
C2 C1 1.375(5) . ?
C5 C4 1.445(4) . ?

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
O4 K1 K1 46.89(5) . 2_656 ?
O4 K1 O6 65.82(6) . 6_556 ?
O4 K1 O7 85.85(7) . 5_656 ?
O4 K1 N6 151.52(7) . 1_545 ?
O4 K1 N5 70.69(7) . . ?
O4 K1 N3 73.44(7) . . ?
O5 K1 K1 103.09(6) . 2_656 ?
O5 K1 O4 95.51(6) . . ?
O5 K1 O3 117.87(8) . 1_545 ?
O5 K1 O6 161.32(8) . 6_556 ?
O5 K1 O7 131.67(7) . 6_556 ?
O5 K1 O7 76.18(7) . 5_656 ?
O5 K1 N6 70.85(7) . 1_545 ?
O5 K1 N5 57.13(7) . . ?
O5 K1 N3 113.30(8) . . ?
O3 K1 K1 125.13(6) 1_545 2_656 ?
O3 K1 O4 145.44(6) 1_545 . ?
O3 K1 O6 80.68(8) 1_545 6_556 ?
O3 K1 O7 109.44(7) 1_545 5_656 ?
O3 K1 O7 75.28(8) 1_545 6_556 ?
O3 K1 N6 57.91(7) 1_545 1_545 ?
O3 K1 N5 118.88(8) 1_545 . ?
O3 K1 N3 84.59(7) 1_545 . ?
O6 K1 K1 64.21(6) 6_556 2_656 ?
O7 K1 K1 49.97(6) 6_556 2_656 ?
O7 K1 K1 45.77(5) 5_656 2_656 ?
O7 K1 O4 89.57(8) 6_556 . ?
O7 K1 O6 51.70(7) 6_556 6_556 ?
O7 K1 O6 100.66(7) 5_656 6_556 ?
O7 K1 O7 56.25(8) 6_556 5_656 ?
O7 K1 N6 82.25(8) 6_556 1_545 ?
O7 K1 N5 159.84(8) 6_556 . ?
O7 K1 N3 114.19(8) 6_556 . ?
N6 K1 K1 110.42(6) 1_545 2_656 ?
N6 K1 O6 125.37(8) 1_545 6_556 ?
N6 K1 O7 66.91(8) 1_545 5_656 ?
N6 K1 N5 117.06(8) 1_545 . ?
N6 K1 N3 134.66(9) 1_545 . ?
N5 K1 K1 113.50(6) . 2_656 ?
N5 K1 O6 113.53(7) . 6_556 ?
N5 K1 O7 123.71(7) . 5_656 ?
N5 K1 N3 57.25(7) . . ?
N3 K1 K1 112.03(6) . 2_656 ?
N3 K1 O6 63.61(8) . 6_556 ?
N3 K1 O7 157.70(8) . 5_656 ?
K1 O4 K1 86.22(10) 2_656 . ?
K1 O4 H4 116(3) 2_656 . ?
K1 O4 H4 118(3) 2_656 2_656 ?
K1 O4 H4 118(3) . . ?
K1 O4 H4 116(3) . 2_656 ?
H4 O4 H4 103(5) . 2_656 ?
N9 O5 K1 154.0(2) . . ?
N1 O3 K1 129.5(2) . 1_565 ?
N9 O6 K1 140.9(2) . 6 ?
K1 O7 K1 84.26(7) 6 5_656 ?
N8 O7 K1 132.3(2) . 6 ?
N8 O7 K1 134.0(2) . 5_656 ?
O8 N8 C5 116.9(3) . . ?
O7 N8 O8 119.9(3) . . ?
O7 N8 C5 123.2(3) . . ?
N6 N7 H7 119(2) . . ?
C4 N7 N6 111.2(3) . . ?
C4 N7 H7 129(2) . . ?
N3 N2 N1 112.5(2) . . ?
N3 N2 C3 122.8(2) . . ?
N1 N2 C3 124.6(3) . . ?
N7 N6 K1 123.43(19) . 1_565 ?
C3 N6 K1 132.0(2) . 1_565 ?
C3 N6 N7 100.1(2) . . ?
C3 N5 K1 115.6(2) . . ?
C4 N5 K1 131.6(2) . . ?
C4 N5 C3 101.4(3) . . ?
O5 N9 C5 117.7(3) . . ?
O6 N9 O5 121.1(3) . . ?
O6 N9 C5 121.1(3) . . ?
N2 N3 K1 115.66(17) . . ?
C2 N3 K1 138.2(2) . . ?
C2 N3 N2 103.5(3) . . ?
O3 N1 N2 124.4(3) . . ?
O3 N1 C1 130.1(3) . . ?
C1 N1 N2 105.5(3) . . ?
O1 N4 O2 126.6(3) . . ?
O1 N4 C2 116.5(3) . . ?
O2 N4 C2 116.9(3) . . ?
N6 C3 N2 122.5(3) . . ?
N6 C3 N5 118.3(3) . . ?
N5 C3 N2 119.2(3) . . ?
N3 C2 N4 120.9(3) . . ?
N3 C2 C1 113.2(3) . . ?
C1 C2 N4 125.9(3) . . ?
N8 C5 N9 118.0(3) . . ?
N8 C5 C4 121.3(3) . . ?
N9 C5 C4 120.7(3) . . ?
N7 C4 C5 124.8(3) . . ?
N5 C4 N7 109.0(3) . . ?
N5 C4 C5 126.2(3) . . ?
N1 C1 Cl1 122.8(3) . . ?
N1 C1 C2 105.2(3) . . ?
C2 C1 Cl1 131.9(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
