# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_comp1_x2986fin
_database_code_depnum_ccdc_archive 'CCDC 1980173'
loop_
_audit_author_name
_audit_author_address
'Peter Lonnecke'
;University of Leipzig
Germany
;
_audit_update_record             
;
2020-01-27 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H34 N2 O6 Zn'
_chemical_formula_sum            'C38 H34 N2 O6 Zn'
_chemical_formula_weight         680.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn 0.2839 1.4301 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P c'
_space_group_name_Hall           'P -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'

_cell_length_a                   17.6162(5)
_cell_length_b                   9.1037(2)
_cell_length_c                   10.3973(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.338(3)
_cell_angle_gamma                90
_cell_volume                     1608.05(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    8002
_cell_measurement_theta_min      2.2230
_cell_measurement_theta_max      31.6660

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_F_000             708
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.815
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3560
_diffrn_reflns_number            21936
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.237
_diffrn_reflns_theta_max         32.555
_diffrn_reflns_theta_full        30.510
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_point_group_measured_fraction_full 0.909
_reflns_number_total             9615
_reflns_number_gt                8163
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.766
_reflns_Friedel_fraction_max     0.715
_reflns_Friedel_fraction_full    0.818

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

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    SHELXT-2014-5
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
 ORTEP3 for Windows
 L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
 or
 DIAMOND Version 3.2k
 K. Brandenburg, Crystal Impact GbR, Bonn, Germany
;
_computing_publication_material  
;
 WINGX
 L.J. Farrugia,
 J. Appl. Cryst., 2012, 45, 849-854.
;
_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)+(0.0497P)²+0.0724P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2918 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         9615
_refine_ls_number_parameters     428
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1116
_refine_ls_wR_factor_gt          0.1043
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_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
Zn1 Zn 0.11976(4) 0.74239(4) 0.53745(5) 0.02290(10) Uani 1 1 d . . . . .
O1 O 0.19098(19) 0.6289(4) 0.4665(3) 0.0335(7) Uani 1 1 d . . . . .
O2 O 0.1326(2) 0.7066(4) 0.2616(3) 0.0389(7) Uani 1 1 d . . . . .
O3 O 0.99555(17) -0.6005(3) -0.0582(3) 0.0292(6) Uani 1 1 d . . . . .
O4 O 1.06364(18) -0.6339(3) 0.1491(3) 0.0280(6) Uani 1 1 d . . . . .
O5 O 0.07059(19) 0.9274(3) 0.4587(3) 0.0323(6) Uani 1 1 d . . . . .
O6 O 0.19332(18) 0.8460(3) 0.6973(3) 0.0296(6) Uani 1 1 d . . . . .
N1 N -0.0100(2) 1.0536(4) 0.2912(4) 0.0366(9) Uani 1 1 d . . . . .
N2 N 0.2353(2) 0.8738(4) 0.9214(3) 0.0329(8) Uani 1 1 d . . . . .
C1 C 0.1827(2) 0.6336(4) 0.3413(4) 0.0263(7) Uani 1 1 d . . . . .
C2 C 0.2394(2) 0.5439(4) 0.2903(4) 0.0266(8) Uani 1 1 d . . . . .
H2 H 0.229293 0.527779 0.197061 0.032 Uiso 1 1 calc R U . . .
C3 C 0.3039(2) 0.4859(4) 0.3717(4) 0.0269(8) Uani 1 1 d . . . . .
H3 H 0.310888 0.500281 0.464621 0.032 Uiso 1 1 calc R U . . .
C4 C 0.3654(2) 0.4017(4) 0.3318(4) 0.0232(7) Uani 1 1 d . . . . .
C5 C 0.4356(2) 0.3690(4) 0.4267(4) 0.0274(8) Uani 1 1 d . . . . .
H5 H 0.443242 0.401057 0.516214 0.033 Uiso 1 1 calc R U . . .
C6 C 0.4943(2) 0.2901(4) 0.3912(4) 0.0268(8) Uani 1 1 d . . . . .
H6 H 0.541496 0.266393 0.456682 0.032 Uiso 1 1 calc R U . . .
C7 C 0.4841(2) 0.2456(4) 0.2597(4) 0.0219(7) Uani 1 1 d . . . . .
C8 C 0.4182(3) 0.2766(4) 0.1701(4) 0.0305(9) Uani 1 1 d . . . . .
H8 H 0.412583 0.247397 0.080364 0.037 Uiso 1 1 calc R U . . .
C9 C 0.3553(2) 0.3519(4) 0.2020(4) 0.0264(7) Uani 1 1 d . . . . .
H9 H 0.307149 0.368022 0.136063 0.032 Uiso 1 1 calc R U . . .
C10 C 0.5449(2) 0.1471(4) 0.2250(3) 0.0186(6) Uani 1 1 d . . . . .
C11 C 0.5417(2) -0.0041(4) 0.2481(3) 0.0203(6) Uani 1 1 d . . . . .
C12 C 0.4808(2) -0.0676(4) 0.2960(4) 0.0261(8) Uani 1 1 d . . . . .
H12 H 0.441083 -0.005864 0.312945 0.031 Uiso 1 1 calc R U . . .
C13 C 0.4778(3) -0.2138(4) 0.3183(4) 0.0301(9) Uani 1 1 d . . . . .
H13 H 0.435867 -0.253376 0.348987 0.036 Uiso 1 1 calc R U . . .
C14 C 0.5372(3) -0.3078(4) 0.2960(4) 0.0275(8) Uani 1 1 d . . . . .
H14 H 0.535533 -0.410088 0.313001 0.033 Uiso 1 1 calc R U . . .
C15 C 0.5965(2) -0.2512(4) 0.2501(4) 0.0224(7) Uani 1 1 d . . . . .
H15 H 0.636041 -0.315380 0.236089 0.027 Uiso 1 1 calc R U . . .
C16 C 0.6012(2) -0.0993(4) 0.2224(3) 0.0191(6) Uani 1 1 d . . . . .
C17 C 0.6604(2) -0.0399(4) 0.1704(3) 0.0173(6) Uani 1 1 d . . . . .
C18 C 0.6620(2) 0.1112(4) 0.1438(3) 0.0182(6) Uani 1 1 d . . . . .
C19 C 0.7220(2) 0.1749(4) 0.0926(3) 0.0219(7) Uani 1 1 d . . . . .
H19 H 0.760768 0.113126 0.072537 0.026 Uiso 1 1 calc R U . . .
C20 C 0.7248(2) 0.3228(4) 0.0716(4) 0.0260(7) Uani 1 1 d . . . . .
H20 H 0.765647 0.362883 0.038149 0.031 Uiso 1 1 calc R U . . .
C21 C 0.6672(2) 0.4161(4) 0.0996(4) 0.0268(8) Uani 1 1 d . . . . .
H21 H 0.669359 0.518802 0.084773 0.032 Uiso 1 1 calc R U . . .
C22 C 0.6085(2) 0.3601(4) 0.1478(4) 0.0235(7) Uani 1 1 d . . . . .
H22 H 0.570092 0.424562 0.165507 0.028 Uiso 1 1 calc R U . . .
C23 C 0.6034(2) 0.2065(4) 0.1724(3) 0.0180(6) Uani 1 1 d . . . . .
C24 C 0.7209(2) -0.1386(4) 0.1391(3) 0.0186(6) Uani 1 1 d . . . . .
C25 C 0.7166(2) -0.1712(4) 0.0060(3) 0.0211(7) Uani 1 1 d . . . . .
H25 H 0.675844 -0.129904 -0.063211 0.025 Uiso 1 1 calc R U . . .
C26 C 0.7717(2) -0.2638(4) -0.0253(4) 0.0213(7) Uani 1 1 d . . . . .
H26 H 0.767796 -0.285959 -0.116097 0.026 Uiso 1 1 calc R U . . .
C27 C 0.8324(2) -0.3246(4) 0.0736(3) 0.0183(6) Uani 1 1 d . . . . .
C28 C 0.8374(2) -0.2897(4) 0.2073(3) 0.0216(7) Uani 1 1 d . . . . .
H28 H 0.878801 -0.329166 0.276691 0.026 Uiso 1 1 calc R U . . .
C29 C 0.7818(2) -0.1976(4) 0.2380(3) 0.0217(7) Uani 1 1 d . . . . .
H29 H 0.785702 -0.174634 0.328613 0.026 Uiso 1 1 calc R U . . .
C30 C 0.8896(2) -0.4211(4) 0.0350(3) 0.0205(7) Uani 1 1 d . . . . .
H30 H 0.878771 -0.446275 -0.056783 0.025 Uiso 1 1 calc R U . . .
C31 C 0.9551(2) -0.4770(4) 0.1153(4) 0.0219(7) Uani 1 1 d . . . . .
H31 H 0.968925 -0.453728 0.207626 0.026 Uiso 1 1 calc R U . . .
C32 C 1.0066(2) -0.5752(4) 0.0616(4) 0.0220(7) Uani 1 1 d . . . . .
C33 C -0.0123(4) 1.1821(5) 0.3734(6) 0.0553(15) Uani 1 1 d . . . . .
H33A H 0.024042 1.168098 0.461846 0.083 Uiso 1 1 calc R U . . .
H33B H -0.065871 1.195511 0.382421 0.083 Uiso 1 1 calc R U . . .
H33C H 0.003316 1.269205 0.331285 0.083 Uiso 1 1 calc R U . . .
C34 C -0.0579(3) 1.0557(6) 0.1550(5) 0.0455(12) Uani 1 1 d . . . . .
H34A H -0.041665 1.137692 0.107330 0.068 Uiso 1 1 calc R U . . .
H34B H -0.113343 1.067812 0.154138 0.068 Uiso 1 1 calc R U . . .
H34C H -0.051285 0.963075 0.111249 0.068 Uiso 1 1 calc R U . . .
C35 C 0.0309(2) 0.9371(4) 0.3416(4) 0.0294(8) Uani 1 1 d . . . . .
H35 H 0.030036 0.855139 0.284640 0.035 Uiso 1 1 calc R U . . .
C36 C 0.2898(4) 0.9923(6) 0.9182(6) 0.0549(16) Uani 1 1 d . . . . .
H36A H 0.289628 1.012596 0.825547 0.082 Uiso 1 1 calc R U . . .
H36B H 0.342873 0.963648 0.968929 0.082 Uiso 1 1 calc R U . . .
H36C H 0.273639 1.080649 0.957873 0.082 Uiso 1 1 calc R U . . .
C37 C 0.2299(3) 0.8257(6) 1.0525(4) 0.0466(12) Uani 1 1 d . . . . .
H37A H 0.190556 0.747425 1.042064 0.070 Uiso 1 1 calc R U . . .
H37B H 0.214325 0.908797 1.099813 0.070 Uiso 1 1 calc R U . . .
H37C H 0.281215 0.788636 1.103793 0.070 Uiso 1 1 calc R U . . .
C38 C 0.1918(2) 0.8126(4) 0.8131(4) 0.0285(8) Uani 1 1 d . . . . .
H38 H 0.156578 0.737233 0.823262 0.034 Uiso 1 1 calc 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
Zn1 O1 1.917(3) . ?
Zn1 O5 1.971(3) . ?
Zn1 O4 1.977(3) 2_455 ?
Zn1 O6 2.047(3) . ?
Zn1 C32 2.573(4) 2_455 ?
O1 C1 1.271(5) . ?
O2 C1 1.233(5) . ?
O3 C32 1.231(4) . ?
O4 C32 1.280(5) . ?
O5 C35 1.236(5) . ?
O6 C38 1.250(5) . ?
N1 C35 1.311(5) . ?
N1 C34 1.444(7) . ?
N1 C33 1.456(6) . ?
N2 C38 1.306(5) . ?
N2 C36 1.450(7) . ?
N2 C37 1.459(6) . ?
C1 C2 1.492(5) . ?
C2 C3 1.333(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.473(5) . ?
C3 H3 0.9500 . ?
C4 C9 1.390(5) . ?
C4 C5 1.395(5) . ?
C5 C6 1.388(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.391(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.313(6) . ?
C7 C10 1.511(5) . ?
C8 C9 1.416(5) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C23 1.398(5) . ?
C10 C11 1.401(5) . ?
C11 C12 1.420(5) . ?
C11 C16 1.439(4) . ?
C12 C13 1.354(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.417(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.360(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.419(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.404(5) . ?
C17 C18 1.405(5) . ?
C17 C24 1.494(4) . ?
C18 C19 1.425(5) . ?
C18 C23 1.439(4) . ?
C19 C20 1.368(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.412(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.361(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.428(5) . ?
C22 H22 0.9500 . ?
C24 C29 1.383(5) . ?
C24 C25 1.397(4) . ?
C25 C26 1.387(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.387(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.406(5) . ?
C27 C30 1.471(4) . ?
C28 C29 1.389(5) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C31 1.333(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.483(5) . ?
C31 H31 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O5 124.15(13) . . ?
O1 Zn1 O4 115.88(12) . 2_455 ?
O5 Zn1 O4 115.98(13) . 2_455 ?
O1 Zn1 O6 102.85(13) . . ?
O5 Zn1 O6 93.30(12) . . ?
O4 Zn1 O6 93.51(11) 2_455 . ?
O1 Zn1 C32 108.76(13) . 2_455 ?
O5 Zn1 C32 106.23(12) . 2_455 ?
O4 Zn1 C32 29.10(11) 2_455 2_455 ?
O6 Zn1 C32 122.27(11) . 2_455 ?
C1 O1 Zn1 117.8(3) . . ?
C32 O4 Zn1 102.2(2) . 2_654 ?
C35 O5 Zn1 122.8(3) . . ?
C38 O6 Zn1 120.0(3) . . ?
C35 N1 C34 121.3(4) . . ?
C35 N1 C33 120.9(4) . . ?
C34 N1 C33 117.7(4) . . ?
C38 N2 C36 122.5(4) . . ?
C38 N2 C37 120.6(4) . . ?
C36 N2 C37 116.8(4) . . ?
O2 C1 O1 125.1(4) . . ?
O2 C1 C2 118.9(3) . . ?
O1 C1 C2 116.0(3) . . ?
C3 C2 C1 122.0(4) . . ?
C3 C2 H2 119.0 . . ?
C1 C2 H2 119.0 . . ?
C2 C3 C4 126.4(4) . . ?
C2 C3 H3 116.8 . . ?
C4 C3 H3 116.8 . . ?
C9 C4 C5 118.6(3) . . ?
C9 C4 C3 121.9(4) . . ?
C5 C4 C3 119.5(3) . . ?
C6 C5 C4 120.4(3) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 120.1(4) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C8 C7 C6 119.6(3) . . ?
C8 C7 C10 120.5(3) . . ?
C6 C7 C10 119.5(3) . . ?
C7 C8 C9 122.6(3) . . ?
C7 C8 H8 118.7 . . ?
C9 C8 H8 118.7 . . ?
C4 C9 C8 118.6(4) . . ?
C4 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C23 C10 C11 120.9(3) . . ?
C23 C10 C7 120.4(3) . . ?
C11 C10 C7 118.7(3) . . ?
C10 C11 C12 121.9(3) . . ?
C10 C11 C16 119.8(3) . . ?
C12 C11 C16 118.3(3) . . ?
C13 C12 C11 121.8(3) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C12 C13 C14 120.1(3) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 119.8(3) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C16 122.2(3) . . ?
C14 C15 H15 118.9 . . ?
C16 C15 H15 118.9 . . ?
C17 C16 C15 122.9(3) . . ?
C17 C16 C11 119.4(3) . . ?
C15 C16 C11 117.7(3) . . ?
C16 C17 C18 120.6(3) . . ?
C16 C17 C24 119.8(3) . . ?
C18 C17 C24 119.6(3) . . ?
C17 C18 C19 121.8(3) . . ?
C17 C18 C23 119.8(3) . . ?
C19 C18 C23 118.4(3) . . ?
C20 C19 C18 121.5(3) . . ?
C20 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
C19 C20 C21 120.0(3) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 120.5(3) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 121.5(3) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C10 C23 C22 122.5(3) . . ?
C10 C23 C18 119.5(3) . . ?
C22 C23 C18 118.1(3) . . ?
C29 C24 C25 118.8(3) . . ?
C29 C24 C17 121.9(3) . . ?
C25 C24 C17 119.3(3) . . ?
C26 C25 C24 120.2(3) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C27 C26 C25 121.2(3) . . ?
C27 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C26 C27 C28 118.5(3) . . ?
C26 C27 C30 119.0(3) . . ?
C28 C27 C30 122.4(3) . . ?
C29 C28 C27 119.9(3) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C24 C29 C28 121.3(3) . . ?
C24 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C31 C30 C27 126.8(3) . . ?
C31 C30 H30 116.6 . . ?
C27 C30 H30 116.6 . . ?
C30 C31 C32 120.5(3) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
O3 C32 O4 121.7(3) . . ?
O3 C32 C31 123.0(3) . . ?
O4 C32 C31 115.3(3) . . ?
O3 C32 Zn1 73.1(2) . 2_654 ?
O4 C32 Zn1 48.66(17) . 2_654 ?
C31 C32 Zn1 163.7(3) . 2_654 ?
N1 C33 H33A 109.5 . . ?
N1 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N1 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N1 C34 H34A 109.5 . . ?
N1 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N1 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O5 C35 N1 124.0(4) . . ?
O5 C35 H35 118.0 . . ?
N1 C35 H35 118.0 . . ?
N2 C36 H36A 109.5 . . ?
N2 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N2 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N2 C37 H37A 109.5 . . ?
N2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O6 C38 N2 124.7(4) . . ?
O6 C38 H38 117.6 . . ?
N2 C38 H38 117.6 . . ?

_refine_diff_density_max         1.373
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.071

####################################################################### 
# 
# 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_comp2_x2972fin
_database_code_depnum_ccdc_archive 'CCDC 1980174'
loop_
_audit_author_name
_audit_author_address
'Peter Lonnecke'
;University of Leipzig
Germany
;
_audit_update_record             
;
2020-01-27 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT919_comp2_x2972fin      
;
PROBLEM: Reflection # Likely Affected by the Beamstop ...          1 Check
RESPONSE: All tested crystals had been twinned and with 41.9 \%A the c-axis is quite huge. As a consequence a lot of reflection are overlapped and especially for the second minor twin domain it was difficult to determine the  orientation within a reasonable accuracy. The reflection 0 -1 -1 has a  relatively high esd. However, the reflection is clearly not affected by  the beamstop and the esd value can be explained only as a result of the twinned data set.
;
# Added during the CSD deposition process: Monday 27 January 2020 05:02 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H27 Cd1 N1 O5, C3 H7 N1 O1'
_chemical_formula_sum            'C38 H34 Cd N2 O6'
_chemical_formula_weight         727.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cd Cd -0.8075 1.2024 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   8.0584(2)
_cell_length_b                   9.4051(2)
_cell_length_c                   41.9284(8)
_cell_angle_alpha                90
_cell_angle_beta                 91.246(2)
_cell_angle_gamma                90
_cell_volume                     3177.00(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    7340
_cell_measurement_theta_min      1.9430
_cell_measurement_theta_max      26.0870

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_F_000             1488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.739
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80567
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3560
_diffrn_reflns_number            7479
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         1.943
_diffrn_reflns_theta_max         26.406
_diffrn_reflns_theta_full        25.350
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7479
_reflns_number_gt                6268
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    SHELXT-2014-5
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
 ORTEP3 for Windows
 L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
 or
 DIAMOND Version 3.2k
 K. Brandenburg, Crystal Impact GbR, Bonn, Germany
;
_computing_publication_material  
;
 WINGX
 L.J. Farrugia,
 J. Appl. Cryst., 2012, 45, 849-854.
;
_refine_special_details          
;
 Refined as a 2-component twin.
 Twin law by rows for the first and second domain:
 1.0000  0.0000  0.0000  0.0000  1.0000  0.0000  0.0000  0.0000  1.0000
-1.0004 -0.0005  0.0000  0.0003 -1.0001  0.0000  0.2249  0.0047  1.0000
 Twin domain ratio: 0.775(1) : 0.225(1)
 Disordered solvent DMF molecule O6, N2, C36 to C38 on two positions with a 
 ratio of 0.65(1) : 0.35(1).

 All tested crystals had been twinned and with 41.9 Å the c-axis is quite 
 huge. As a consequence a lot of reflection are overlapped and especially
 for the second minor twin domain it was difficult to determine the
 orientation within a reasonable accuracy. The reflection 0 -1 -1 has a
 relatively high esd. However, the reflection is clearly not affected by
 the beamstop and the esd value can be explained only as a result of the
 twinned data set.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0541P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         7479
_refine_ls_number_parameters     465
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.0943
_refine_ls_wR_factor_gt          0.0860
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.982
_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
Cd1 Cd 0.23395(3) 0.47856(3) 0.49941(2) 0.02267(9) Uani 1 1 d . . . . .
O1 O 0.3496(3) 0.3534(3) 0.53803(7) 0.0291(7) Uani 1 1 d . . . . .
O2 O 0.5550(3) 0.5117(3) 0.53617(6) 0.0274(6) Uani 1 1 d . . . . .
O3 O 1.6403(3) 0.2177(3) 0.96713(7) 0.0324(7) Uani 1 1 d . . . . .
O4 O 1.5008(3) 0.0148(3) 0.96576(6) 0.0263(6) Uani 1 1 d . . . . .
C1 C 0.4789(5) 0.4146(5) 0.54994(9) 0.0249(9) Uani 1 1 d . . . . .
C2 C 0.5313(5) 0.3691(5) 0.58232(10) 0.0252(9) Uani 1 1 d . . . . .
H2 H 0.482977 0.286636 0.591359 0.030 Uiso 1 1 calc R U . . .
C3 C 0.6450(5) 0.4416(4) 0.59902(9) 0.0244(9) Uani 1 1 d . . . . .
H3 H 0.693928 0.520529 0.588660 0.029 Uiso 1 1 calc R U . . .
C4 C 0.7029(5) 0.4124(4) 0.63179(9) 0.0234(9) Uani 1 1 d . . . . .
C5 C 0.6479(5) 0.2972(4) 0.64936(9) 0.0267(9) Uani 1 1 d . . . . .
H5 H 0.566016 0.235527 0.640395 0.032 Uiso 1 1 calc R U . . .
C6 C 0.7109(5) 0.2711(4) 0.67987(9) 0.0256(9) Uani 1 1 d . . . . .
H6 H 0.675169 0.189839 0.691279 0.031 Uiso 1 1 calc R U . . .
C7 C 0.8266(5) 0.3637(4) 0.69388(9) 0.0223(9) Uani 1 1 d . . . . .
C8 C 0.8793(5) 0.4786(5) 0.67666(10) 0.0283(9) Uani 1 1 d . . . . .
H8 H 0.958618 0.541941 0.685904 0.034 Uiso 1 1 calc R U . . .
C9 C 0.8184(5) 0.5038(4) 0.64597(9) 0.0270(9) Uani 1 1 d . . . . .
H9 H 0.856064 0.584338 0.634513 0.032 Uiso 1 1 calc R U . . .
C10 C 0.9004(5) 0.3289(4) 0.72615(9) 0.0215(9) Uani 1 1 d . . . . .
C11 C 0.8073(5) 0.3500(4) 0.75362(9) 0.0205(8) Uani 1 1 d . . . . .
C12 C 0.6449(5) 0.4110(4) 0.75249(10) 0.0251(9) Uani 1 1 d . . . . .
H12 H 0.600889 0.444017 0.732640 0.030 Uiso 1 1 calc R U . . .
C13 C 0.5523(5) 0.4230(4) 0.77877(10) 0.0274(10) Uani 1 1 d . . . . .
H13 H 0.443548 0.461737 0.777138 0.033 Uiso 1 1 calc R U . . .
C14 C 0.6165(5) 0.3784(5) 0.80862(10) 0.0297(10) Uani 1 1 d . . . . .
H14 H 0.550031 0.385535 0.826988 0.036 Uiso 1 1 calc R U . . .
C15 C 0.7730(5) 0.3251(4) 0.81136(10) 0.0276(9) Uani 1 1 d . . . . .
H15 H 0.814996 0.297788 0.831805 0.033 Uiso 1 1 calc R U . . .
C16 C 0.8750(5) 0.3092(4) 0.78451(9) 0.0196(8) Uani 1 1 d . . . . .
C17 C 1.0353(5) 0.2499(4) 0.78660(9) 0.0214(9) Uani 1 1 d . . . . .
C18 C 1.1267(4) 0.2264(4) 0.75896(9) 0.0201(9) Uani 1 1 d . . . . .
C19 C 1.2865(5) 0.1603(4) 0.75961(10) 0.0248(9) Uani 1 1 d . . . . .
H19 H 1.334243 0.132906 0.779604 0.030 Uiso 1 1 calc R U . . .
C20 C 1.3721(5) 0.1353(4) 0.73285(10) 0.0267(9) Uani 1 1 d . . . . .
H20 H 1.477962 0.090923 0.734198 0.032 Uiso 1 1 calc R U . . .
C21 C 1.3037(5) 0.1753(4) 0.70276(10) 0.0263(9) Uani 1 1 d . . . . .
H21 H 1.363781 0.157375 0.683933 0.032 Uiso 1 1 calc R U . . .
C22 C 1.1532(5) 0.2391(4) 0.70069(9) 0.0228(9) Uani 1 1 d . . . . .
H22 H 1.109586 0.265618 0.680313 0.027 Uiso 1 1 calc R U . . .
C23 C 1.0585(5) 0.2676(4) 0.72830(9) 0.0203(9) Uani 1 1 d . . . . .
C24 C 1.1097(5) 0.2119(4) 0.81916(9) 0.0214(9) Uani 1 1 d . . . . .
C25 C 1.1356(5) 0.0723(5) 0.82766(9) 0.0252(9) Uani 1 1 d . . . . .
H25 H 1.103644 -0.001788 0.813404 0.030 Uiso 1 1 calc R U . . .
C26 C 1.2086(5) 0.0395(5) 0.85708(9) 0.0249(9) Uani 1 1 d . . . . .
H26 H 1.225988 -0.057181 0.862800 0.030 Uiso 1 1 calc R U . . .
C27 C 1.2566(5) 0.1463(4) 0.87825(9) 0.0253(9) Uani 1 1 d . . . . .
C28 C 1.2253(5) 0.2870(5) 0.86958(10) 0.0324(10) Uani 1 1 d . . . . .
H28 H 1.253734 0.361526 0.883992 0.039 Uiso 1 1 calc R U . . .
C29 C 1.1535(5) 0.3193(5) 0.84023(10) 0.0314(10) Uani 1 1 d . . . . .
H29 H 1.134048 0.415719 0.834516 0.038 Uiso 1 1 calc R U . . .
C30 C 1.3420(5) 0.1077(5) 0.90836(9) 0.0262(9) Uani 1 1 d . . . . .
H30 H 1.332780 0.011590 0.915040 0.031 Uiso 1 1 calc R U . . .
C31 C 1.4313(5) 0.1942(5) 0.92727(10) 0.0281(10) Uani 1 1 d . . . . .
H31 H 1.432354 0.293172 0.922732 0.034 Uiso 1 1 calc R U . . .
C32 C 1.5290(5) 0.1404(5) 0.95519(10) 0.0272(10) Uani 1 1 d . . . . .
O5 O 0.2599(3) 0.7181(3) 0.50378(7) 0.0317(7) Uani 1 1 d D . . . .
N1 N 0.3606(4) 0.9141(4) 0.52861(9) 0.0368(9) Uani 1 1 d D . . . .
C33 C 0.2191(6) 1.0008(5) 0.51959(17) 0.0608(16) Uani 1 1 d D . . . .
H33A H 0.229866 1.032271 0.497450 0.091 Uiso 1 1 calc R U . . .
H33B H 0.214477 1.083913 0.533633 0.091 Uiso 1 1 calc R U . . .
H33C H 0.117196 0.944963 0.521567 0.091 Uiso 1 1 calc R U . . .
C34 C 0.4891(6) 0.9790(6) 0.54909(13) 0.0519(14) Uani 1 1 d D . . . .
H34A H 0.579522 0.910839 0.552738 0.078 Uiso 1 1 calc R U . . .
H34B H 0.441367 1.005336 0.569562 0.078 Uiso 1 1 calc R U . . .
H34C H 0.532309 1.064126 0.538676 0.078 Uiso 1 1 calc R U . . .
C35 C 0.3690(5) 0.7793(4) 0.52034(11) 0.0319(10) Uani 1 1 d D . . . .
H35 H 0.463038 0.725883 0.527314 0.038 Uiso 1 1 calc R U . . .
O6 O -0.2386(14) 0.8412(17) 0.3803(5) 0.055(3) Uani 0.652(10) 1 d D . P A 1
N2 N 0.0048(11) 0.8702(13) 0.4083(3) 0.0406(18) Uani 0.652(10) 1 d D . P A 1
C36 C 0.0823(14) 0.9538(10) 0.3838(3) 0.073(4) Uani 0.652(10) 1 d D . P A 1
H36A H 0.190812 0.912962 0.379021 0.109 Uiso 0.652(10) 1 calc R U P A 1
H36B H 0.096752 1.051763 0.391307 0.109 Uiso 0.652(10) 1 calc R U P A 1
H36C H 0.011685 0.953246 0.364470 0.109 Uiso 0.652(10) 1 calc R U P A 1
C37 C 0.1003(11) 0.8394(11) 0.4373(2) 0.058(3) Uani 0.652(10) 1 d D . P A 1
H37A H 0.038931 0.771879 0.450414 0.086 Uiso 0.652(10) 1 calc R U P A 1
H37B H 0.118803 0.927546 0.449334 0.086 Uiso 0.652(10) 1 calc R U P A 1
H37C H 0.207419 0.797948 0.431766 0.086 Uiso 0.652(10) 1 calc R U P A 1
C38 C -0.1460(9) 0.8183(8) 0.40404(19) 0.044(2) Uani 0.652(10) 1 d D . P A 1
H38 H -0.187557 0.758651 0.420314 0.053 Uiso 0.652(10) 1 calc R U P A 1
O6F O -0.230(3) 0.812(4) 0.3802(10) 0.055(3) Uani 0.348(10) 1 d D . P A 2
N2F N 0.021(2) 0.873(2) 0.4027(5) 0.0406(18) Uani 0.348(10) 1 d D . P A 2
C36F C 0.005(2) 0.7709(18) 0.4282(4) 0.052(5) Uani 0.348(10) 1 d D . P A 2
H36D H -0.112542 0.750292 0.431433 0.078 Uiso 0.348(10) 1 calc R U P A 2
H36E H 0.054370 0.810136 0.447879 0.078 Uiso 0.348(10) 1 calc R U P A 2
H36F H 0.062986 0.683032 0.422594 0.078 Uiso 0.348(10) 1 calc R U P A 2
C37F C 0.1696(16) 0.9609(17) 0.4019(4) 0.048(4) Uani 0.348(10) 1 d D . P A 2
H37D H 0.267573 0.899726 0.400367 0.072 Uiso 0.348(10) 1 calc R U P A 2
H37E H 0.178079 1.017940 0.421393 0.072 Uiso 0.348(10) 1 calc R U P A 2
H37F H 0.163309 1.024124 0.383294 0.072 Uiso 0.348(10) 1 calc R U P A 2
C38F C -0.0987(18) 0.8820(15) 0.3807(3) 0.044(5) Uani 0.348(10) 1 d D . P A 2
H38F H -0.083355 0.947700 0.363828 0.053 Uiso 0.348(10) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O1 2.193(3) . ?
Cd1 O5 2.270(3) . ?
Cd1 O2 2.288(3) 3_666 ?
Cd1 O4 2.326(2) 4_465 ?
Cd1 O3 2.400(3) 4_465 ?
Cd1 O4 2.439(3) 2_656 ?
Cd1 C32 2.699(4) 4_465 ?
O1 C1 1.282(5) . ?
O2 C1 1.249(5) . ?
O3 C32 1.250(5) . ?
O4 C32 1.284(5) . ?
C1 C2 1.476(5) . ?
C2 C3 1.330(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.467(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(6) . ?
C4 C9 1.391(5) . ?
C5 C6 1.388(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.395(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.372(6) . ?
C7 C10 1.502(5) . ?
C8 C9 1.388(5) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C23 1.399(5) . ?
C10 C11 1.403(6) . ?
C11 C12 1.429(5) . ?
C11 C16 1.446(5) . ?
C12 C13 1.349(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.408(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.359(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.416(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.408(5) . ?
C17 C18 1.404(5) . ?
C17 C24 1.522(5) . ?
C18 C19 1.430(5) . ?
C18 C23 1.440(5) . ?
C19 C20 1.350(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.417(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.354(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.426(6) . ?
C22 H22 0.9500 . ?
C24 C25 1.375(6) . ?
C24 C29 1.383(6) . ?
C25 C26 1.390(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.389(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.394(6) . ?
C27 C30 1.470(5) . ?
C28 C29 1.382(5) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C31 1.335(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.485(5) . ?
C31 H31 0.9500 . ?
O5 C35 1.249(5) . ?
N1 C35 1.316(5) . ?
N1 C33 1.445(6) . ?
N1 C34 1.464(5) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35 0.9500 . ?
O6 C38 1.249(18) . ?
N2 C38 1.318(10) . ?
N2 C36 1.447(14) . ?
N2 C37 1.454(11) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38 0.9500 . ?
O6F C38F 1.25(2) . ?
N2F C38F 1.319(15) . ?
N2F C36F 1.45(2) . ?
N2F C37F 1.458(17) . ?
C36F H36D 0.9800 . ?
C36F H36E 0.9800 . ?
C36F H36F 0.9800 . ?
C37F H37D 0.9800 . ?
C37F H37E 0.9800 . ?
C37F H37F 0.9800 . ?
C38F H38F 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cd1 O5 115.84(10) . . ?
O1 Cd1 O2 101.12(10) . 3_666 ?
O5 Cd1 O2 86.82(10) . 3_666 ?
O1 Cd1 O4 141.91(10) . 4_465 ?
O5 Cd1 O4 95.41(10) . 4_465 ?
O2 Cd1 O4 101.86(9) 3_666 4_465 ?
O1 Cd1 O3 97.30(10) . 4_465 ?
O5 Cd1 O3 146.72(10) . 4_465 ?
O2 Cd1 O3 83.81(10) 3_666 4_465 ?
O4 Cd1 O3 55.86(10) 4_465 4_465 ?
O1 Cd1 O4 87.45(10) . 2_656 ?
O5 Cd1 O4 83.36(10) . 2_656 ?
O2 Cd1 O4 169.10(10) 3_666 2_656 ?
O4 Cd1 O4 74.49(10) 4_465 2_656 ?
O3 Cd1 O4 101.92(10) 4_465 2_656 ?
O1 Cd1 C32 121.91(13) . 4_465 ?
O5 Cd1 C32 121.41(12) . 4_465 ?
O2 Cd1 C32 91.21(11) 3_666 4_465 ?
O4 Cd1 C32 28.38(11) 4_465 4_465 ?
O3 Cd1 C32 27.60(11) 4_465 4_465 ?
O4 Cd1 C32 89.90(11) 2_656 4_465 ?
C1 O1 Cd1 112.0(3) . . ?
C1 O2 Cd1 135.3(3) . 3_666 ?
C32 O3 Cd1 89.6(2) . 4_766 ?
C32 O4 Cd1 92.2(2) . 4_766 ?
C32 O4 Cd1 118.7(3) . 2_646 ?
Cd1 O4 Cd1 105.51(10) 4_766 2_646 ?
O2 C1 O1 123.5(4) . . ?
O2 C1 C2 120.3(4) . . ?
O1 C1 C2 116.2(4) . . ?
C3 C2 C1 121.0(4) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 126.8(4) . . ?
C2 C3 H3 116.6 . . ?
C4 C3 H3 116.6 . . ?
C5 C4 C9 118.3(3) . . ?
C5 C4 C3 123.0(4) . . ?
C9 C4 C3 118.7(4) . . ?
C6 C5 C4 120.8(4) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 120.4(4) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C8 C7 C6 118.8(3) . . ?
C8 C7 C10 121.6(3) . . ?
C6 C7 C10 119.4(4) . . ?
C7 C8 C9 121.0(4) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C8 C9 C4 120.7(4) . . ?
C8 C9 H9 119.6 . . ?
C4 C9 H9 119.6 . . ?
C23 C10 C11 120.5(3) . . ?
C23 C10 C7 119.3(4) . . ?
C11 C10 C7 120.0(3) . . ?
C10 C11 C12 122.4(3) . . ?
C10 C11 C16 120.0(3) . . ?
C12 C11 C16 117.6(4) . . ?
C13 C12 C11 122.0(4) . . ?
C13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C12 C13 C14 120.1(4) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 120.5(4) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 121.7(4) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C17 C16 C15 122.7(3) . . ?
C17 C16 C11 119.2(4) . . ?
C15 C16 C11 118.0(3) . . ?
C18 C17 C16 120.6(3) . . ?
C18 C17 C24 120.0(3) . . ?
C16 C17 C24 119.5(4) . . ?
C17 C18 C19 122.8(3) . . ?
C17 C18 C23 119.8(3) . . ?
C19 C18 C23 117.4(3) . . ?
C20 C19 C18 122.4(3) . . ?
C20 C19 H19 118.8 . . ?
C18 C19 H19 118.8 . . ?
C19 C20 C21 119.9(4) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C22 C21 C20 120.4(4) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C23 121.7(4) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C10 C23 C22 121.8(3) . . ?
C10 C23 C18 119.9(4) . . ?
C22 C23 C18 118.3(3) . . ?
C25 C24 C29 119.8(4) . . ?
C25 C24 C17 120.8(4) . . ?
C29 C24 C17 119.4(4) . . ?
C24 C25 C26 120.1(4) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C27 C26 C25 120.9(4) . . ?
C27 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
C26 C27 C28 118.3(3) . . ?
C26 C27 C30 119.3(4) . . ?
C28 C27 C30 122.5(4) . . ?
C29 C28 C27 120.7(4) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C28 C29 C24 120.3(4) . . ?
C28 C29 H29 119.9 . . ?
C24 C29 H29 119.9 . . ?
C31 C30 C27 126.6(4) . . ?
C31 C30 H30 116.7 . . ?
C27 C30 H30 116.7 . . ?
C30 C31 C32 122.0(4) . . ?
C30 C31 H31 119.0 . . ?
C32 C31 H31 119.0 . . ?
O3 C32 O4 121.8(3) . . ?
O3 C32 C31 118.7(4) . . ?
O4 C32 C31 119.4(4) . . ?
O3 C32 Cd1 62.8(2) . 4_766 ?
O4 C32 Cd1 59.44(18) . 4_766 ?
C31 C32 Cd1 171.3(3) . 4_766 ?
C35 O5 Cd1 124.4(3) . . ?
C35 N1 C33 121.3(4) . . ?
C35 N1 C34 121.1(4) . . ?
C33 N1 C34 117.5(4) . . ?
N1 C33 H33A 109.5 . . ?
N1 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N1 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N1 C34 H34A 109.5 . . ?
N1 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N1 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O5 C35 N1 123.4(4) . . ?
O5 C35 H35 118.3 . . ?
N1 C35 H35 118.3 . . ?
C38 N2 C36 121.0(10) . . ?
C38 N2 C37 120.6(10) . . ?
C36 N2 C37 118.3(9) . . ?
N2 C36 H36A 109.5 . . ?
N2 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N2 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N2 C37 H37A 109.5 . . ?
N2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O6 C38 N2 125.3(12) . . ?
O6 C38 H38 117.3 . . ?
N2 C38 H38 117.3 . . ?
C38F N2F C36F 119.0(15) . . ?
C38F N2F C37F 122.4(18) . . ?
C36F N2F C37F 118.5(14) . . ?
N2F C36F H36D 109.5 . . ?
N2F C36F H36E 109.5 . . ?
H36D C36F H36E 109.5 . . ?
N2F C36F H36F 109.5 . . ?
H36D C36F H36F 109.5 . . ?
H36E C36F H36F 109.5 . . ?
N2F C37F H37D 109.5 . . ?
N2F C37F H37E 109.5 . . ?
H37D C37F H37E 109.5 . . ?
N2F C37F H37F 109.5 . . ?
H37D C37F H37F 109.5 . . ?
H37E C37F H37F 109.5 . . ?
O6F C38F N2F 126(2) . . ?
O6F C38F H38F 117.2 . . ?
N2F C38F H38F 117.2 . . ?

_refine_diff_density_max         1.386
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.183

####################################################################### 
# 
# 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_H2L_x3040fin
_database_code_depnum_ccdc_archive 'CCDC 1980175'
loop_
_audit_author_name
_audit_author_address
'Peter Lonnecke'
;University of Leipzig
Germany
;
_audit_update_record             
;
2020-01-27 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H22 O4, 2(C4 H9 N O)'
_chemical_formula_sum            'C40 H40 N2 O6'
_chemical_formula_weight         644.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
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'

_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                   7.8864(4)
_cell_length_b                   9.2043(4)
_cell_length_c                   11.9198(6)
_cell_angle_alpha                76.155(4)
_cell_angle_beta                 81.642(4)
_cell_angle_gamma                75.045(4)
_cell_volume                     808.42(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    3865
_cell_measurement_theta_min      2.3350
_cell_measurement_theta_max      30.3180

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_F_000             342
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.089
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.99331
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3560
_diffrn_reflns_number            11121
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.767
_diffrn_reflns_theta_max         30.623
_diffrn_reflns_theta_full        28.285
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4475
_reflns_number_gt                3434
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    SHELXT-2018-2
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
 ORTEP3 for Windows
 L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
 or
 DIAMOND Version 3.2k
 K. Brandenburg, Crystal Impact GbR, Bonn, Germany
;
_computing_publication_material  
;
 WINGX
 L.J. Farrugia,
 J. Appl. Cryst., 2012, 45, 849-854.
;
_refine_special_details          
;
Disordered molecule with ratio 0.933(2):0.067(2)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0550P)²+0.3265P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4475
_refine_ls_number_parameters     352
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1291
_refine_ls_wR_factor_gt          0.1172
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.013
_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 0.09173(17) 0.54491(15) 0.07539(11) 0.0168(3) Uani 1 1 d . . . . .
C2 C -0.04704(17) 0.65181(15) 0.01812(11) 0.0173(3) Uani 1 1 d . . . . .
C3 C -0.10007(18) 0.80758(16) 0.03310(12) 0.0210(3) Uani 1 1 d . . . . .
C4 C -0.23275(19) 0.91082(16) -0.02386(13) 0.0234(3) Uani 1 1 d . . . . .
C5 C -0.32162(19) 0.86693(16) -0.10090(13) 0.0232(3) Uani 1 1 d . . . . .
C6 C -0.27644(18) 0.72050(16) -0.11778(12) 0.0202(3) Uani 1 1 d . . . . .
C7 C -0.13936(17) 0.60710(15) -0.05868(11) 0.0172(3) Uani 1 1 d . . . . .
O1 O 0.57184(18) 0.81758(19) 0.61307(12) 0.0374(3) Uani 0.9331(18) 1 d D . P A
1
O2 O 0.7798(2) 0.74621(17) 0.47505(12) 0.0328(3) Uani 0.9331(18) 1 d D . P A 1
C8 C 0.1968(4) 0.5942(5) 0.1495(2) 0.0172(4) Uani 0.9331(18) 1 d D . P A 1
C9 C 0.1481(2) 0.5875(2) 0.26731(15) 0.0231(4) Uani 0.9331(18) 1 d D . P A 1
C10 C 0.2511(2) 0.62798(19) 0.33454(14) 0.0237(3) Uani 0.9331(18) 1 d D . P A 1
C11 C 0.4046(2) 0.67644(17) 0.28536(14) 0.0201(3) Uani 0.9331(18) 1 d D . P A 1
C12 C 0.4508(2) 0.68320(19) 0.16699(14) 0.0211(3) Uani 0.9331(18) 1 d D . P A 1
C13 C 0.3480(2) 0.6424(2) 0.10024(14) 0.0203(4) Uani 0.9331(18) 1 d D . P A 1
C14 C 0.5235(2) 0.71319(18) 0.35294(14) 0.0232(3) Uani 0.9331(18) 1 d D . P A 1
C15 C 0.4859(2) 0.74208(19) 0.45837(14) 0.0266(3) Uani 0.9331(18) 1 d D . P A 1
C16 C 0.6147(3) 0.7736(2) 0.52274(19) 0.0272(4) Uani 0.9331(18) 1 d D . P A 1
O1F O 0.597(3) 0.773(3) 0.576(2) 0.030 Uiso 0.0669(18) 1 d D U P A 2
O2F O 0.853(3) 0.741(2) 0.4587(18) 0.030 Uiso 0.0669(18) 1 d D U P A 2
H1OF H 0.897041 0.757332 0.513299 0.045 Uiso 0.0669(18) 1 calc R U P A 2
C8F C 0.175(9) 0.589(11) 0.160(4) 0.030 Uiso 0.0669(18) 1 d D U P A 2
C9F C 0.318(4) 0.649(4) 0.123(2) 0.030 Uiso 0.0669(18) 1 d D U P A 2
H9F H 0.358352 0.667063 0.043175 0.036 Uiso 0.0669(18) 1 calc R U P A 2
C10F C 0.407(3) 0.686(3) 0.204(2) 0.030 Uiso 0.0669(18) 1 d D U P A 2
H10F H 0.511445 0.722179 0.179736 0.036 Uiso 0.0669(18) 1 calc R U P A 2
C11F C 0.339(3) 0.6682(19) 0.3189(18) 0.030 Uiso 0.0669(18) 1 d D U P A 2
C12F C 0.186(3) 0.617(3) 0.351(2) 0.030 Uiso 0.0669(18) 1 d D U P A 2
H12F H 0.138706 0.607199 0.429618 0.036 Uiso 0.0669(18) 1 calc R U P A 2
C13F C 0.099(4) 0.580(4) 0.274(3) 0.030 Uiso 0.0669(18) 1 d D U P A 2
H13F H -0.009502 0.549712 0.297401 0.036 Uiso 0.0669(18) 1 calc R U P A 2
C14F C 0.434(3) 0.705(3) 0.4025(19) 0.030 Uiso 0.0669(18) 1 d D U P A 2
H14F H 0.371118 0.710194 0.476338 0.036 Uiso 0.0669(18) 1 calc R U P A 2
C15F C 0.593(3) 0.733(3) 0.3905(18) 0.030 Uiso 0.0669(18) 1 d D U P A 2
H15F H 0.657132 0.736105 0.316281 0.036 Uiso 0.0669(18) 1 calc R U P A 2
C16F C 0.679(3) 0.760(3) 0.484(2) 0.030 Uiso 0.0669(18) 1 d D U P A 2
H3 H -0.037(2) 0.8382(19) 0.0854(14) 0.024(4) Uiso 1 1 d . . . . .
H4 H -0.268(2) 1.016(2) -0.0129(15) 0.031(5) Uiso 1 1 d . . . . .
H5 H -0.415(2) 0.941(2) -0.1420(15) 0.030(4) Uiso 1 1 d . . . . .
H6 H -0.335(2) 0.6925(18) -0.1716(14) 0.018(4) Uiso 1 1 d . . . . .
H1O2 H 0.857(4) 0.749(3) 0.535(3) 0.075(8) Uiso 0.9331(18) 1 d . . P A 1
H9 H 0.044(3) 0.552(2) 0.3023(18) 0.035(6) Uiso 0.9331(18) 1 d . . P A 1
H10 H 0.216(3) 0.618(2) 0.4180(18) 0.033(5) Uiso 0.9331(18) 1 d . . P A 1
H12 H 0.561(2) 0.714(2) 0.1317(15) 0.024(4) Uiso 0.9331(18) 1 d . . P A 1
H13 H 0.388(2) 0.645(2) 0.0174(17) 0.027(5) Uiso 0.9331(18) 1 d . . P A 1
H14 H 0.648(3) 0.717(2) 0.3161(17) 0.036(5) Uiso 0.9331(18) 1 d . . P A 1
H15 H 0.363(3) 0.748(2) 0.4989(18) 0.043(6) Uiso 0.9331(18) 1 d . . P A 1
O3 O 1.0173(2) 0.7294(2) 0.60967(12) 0.0274(4) Uani 0.9331(18) 1 d D . P A 1
N1 N 1.16353(17) 0.79855(15) 0.72791(11) 0.0236(3) Uani 0.9331(18) 1 d D . P A
1
C17 C 1.2730(2) 0.6441(2) 0.75615(17) 0.0265(4) Uani 0.9331(18) 1 d D . P A 1
C18 C 1.2043(5) 0.9130(6) 0.7791(3) 0.0356(5) Uani 0.9331(18) 1 d D . P A 1
C19 C 1.03422(19) 0.82956(17) 0.6586(1) 0.0213(3) Uani 0.9331(18) 1 d D . P A 1
C20 C 0.9118(3) 0.9864(2) 0.64121(18) 0.0295(4) Uani 0.9331(18) 1 d D . P A 1
O3F O 0.993(4) 0.721(4) 0.634(2) 0.030 Uiso 0.0669(18) 1 d D U P A 2
N1F N 1.089(2) 0.8811(19) 0.7043(15) 0.030 Uiso 0.0669(18) 1 d D U P A 2
C17F C 0.948(3) 1.010(3) 0.656(3) 0.030 Uiso 0.0669(18) 1 d D U P A 2
H17D H 0.948379 1.014165 0.572724 0.045 Uiso 0.0669(18) 1 calc R U P A 2
H17E H 0.967516 1.106325 0.666511 0.045 Uiso 0.0669(18) 1 calc R U P A 2
H17F H 0.833895 0.995036 0.695454 0.045 Uiso 0.0669(18) 1 calc R U P A 2
C18F C 1.212(6) 0.915(7) 0.769(4) 0.030 Uiso 0.0669(18) 1 d D U P A 2
H18D H 1.295758 0.819569 0.799719 0.045 Uiso 0.0669(18) 1 calc R U P A 2
H18E H 1.146224 0.960487 0.833765 0.045 Uiso 0.0669(18) 1 calc R U P A 2
H18F H 1.275160 0.987471 0.717897 0.045 Uiso 0.0669(18) 1 calc R U P A 2
C19F C 1.103(2) 0.742(2) 0.6883(15) 0.030 Uiso 0.0669(18) 1 d D U P A 2
C20F C 1.248(3) 0.610(3) 0.739(3) 0.030 Uiso 0.0669(18) 1 d D U P A 2
H20D H 1.199262 0.519811 0.773721 0.045 Uiso 0.0669(18) 1 calc R U P A 2
H20E H 1.296450 0.639476 0.799490 0.045 Uiso 0.0669(18) 1 calc R U P A 2
H20F H 1.340735 0.585912 0.678191 0.045 Uiso 0.0669(18) 1 calc R U P A 2
H17A H 1.396(3) 0.645(3) 0.736(2) 0.048(6) Uiso 0.9331(18) 1 d . . P A 1
H17B H 1.248(4) 0.577(3) 0.704(3) 0.075(10) Uiso 0.9331(18) 1 d . . P A 1
H17C H 1.251(3) 0.597(3) 0.840(2) 0.047(7) Uiso 0.9331(18) 1 d . . P A 1
H18A H 1.173(3) 0.890(3) 0.864(2) 0.055(7) Uiso 0.9331(18) 1 d . . P A 1
H18B H 1.330(4) 0.909(3) 0.760(2) 0.066(8) Uiso 0.9331(18) 1 d . . P A 1
H18C H 1.149(3) 1.018(3) 0.737(2) 0.051(7) Uiso 0.9331(18) 1 d . . P A 1
H20A H 0.869(3) 1.024(2) 0.7185(19) 0.042(6) Uiso 0.9331(18) 1 d . . P A 1
H20B H 0.973(3) 1.068(3) 0.589(2) 0.042(6) Uiso 0.9331(18) 1 d . . P A 1
H20C H 0.812(3) 0.982(3) 0.605(2) 0.049(6) Uiso 0.9331(18) 1 d . . P A 1


_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 C2 1.4042(18) . ?
C1 C7 1.4067(18) 2_565 ?
C1 C8F 1.47(3) . ?
C1 C8 1.508(2) . ?
C2 C3 1.4331(18) . ?
C2 C7 1.4374(17) . ?
C3 C4 1.358(2) . ?
C3 H3 0.980(17) . ?
C4 C5 1.417(2) . ?
C4 H4 0.968(18) . ?
C5 C6 1.358(2) . ?
C5 H5 0.966(18) . ?
C6 C7 1.4288(18) . ?
C6 H6 0.958(16) . ?
O1 C16 1.212(2) . ?
O2 C16 1.329(2) . ?
O2 H1O2 1.02(3) . ?
C8 C13 1.381(2) . ?
C8 C9 1.392(2) . ?
C9 C10 1.388(2) . ?
C9 H9 0.97(2) . ?
C10 C11 1.399(2) . ?
C10 H10 0.98(2) . ?
C11 C12 1.396(2) . ?
C11 C14 1.468(2) . ?
C12 C13 1.385(2) . ?
C12 H12 0.990(18) . ?
C13 H13 0.989(19) . ?
C14 C15 1.322(2) . ?
C14 H14 1.02(2) . ?
C15 C16 1.480(2) . ?
C15 H15 1.01(2) . ?
O1F C16F 1.212(17) . ?
O2F C16F 1.332(18) . ?
O2F H1OF 0.8400 . ?
C8F C9F 1.352(19) . ?
C8F C13F 1.395(19) . ?
C9F C10F 1.418(18) . ?
C9F H9F 0.9500 . ?
C10F C11F 1.382(17) . ?
C10F H10F 0.9500 . ?
C11F C12F 1.378(17) . ?
C11F C14F 1.477(16) . ?
C12F C13F 1.372(18) . ?
C12F H12F 0.9500 . ?
C13F H13F 0.9500 . ?
C14F C15F 1.327(17) . ?
C14F H14F 0.9500 . ?
C15F C16F 1.481(17) . ?
C15F H15F 0.9500 . ?
O3 C19 1.245(2) . ?
N1 C19 1.3364(19) . ?
N1 C17 1.450(2) . ?
N1 C18 1.458(3) . ?
C17 H17A 0.96(2) . ?
C17 H17B 1.05(3) . ?
C17 H17C 1.00(2) . ?
C18 H18A 0.99(2) . ?
C18 H18B 0.98(3) . ?
C18 H18C 0.99(2) . ?
C19 C20 1.502(2) . ?
C20 H20A 1.04(2) . ?
C20 H20B 1.03(2) . ?
C20 H20C 0.97(2) . ?
O3F C19F 1.235(17) . ?
N1F C19F 1.313(16) . ?
N1F C18F 1.457(18) . ?
N1F C17F 1.466(17) . ?
C17F H17D 0.9800 . ?
C17F H17E 0.9800 . ?
C17F H17F 0.9800 . ?
C18F H18D 0.9800 . ?
C18F H18E 0.9800 . ?
C18F H18F 0.9800 . ?
C19F C20F 1.508(17) . ?
C20F H20D 0.9800 . ?
C20F H20E 0.9800 . ?
C20F H20F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C7 119.91(11) . 2_565 ?
C2 C1 C8F 120(4) . . ?
C7 C1 C8F 120(4) 2_565 . ?
C2 C1 C8 120.4(2) . . ?
C7 C1 C8 119.6(2) 2_565 . ?
C1 C2 C3 121.66(12) . . ?
C1 C2 C7 120.28(11) . . ?
C3 C2 C7 118.05(12) . . ?
C4 C3 C2 121.31(13) . . ?
C4 C3 H3 120.6(10) . . ?
C2 C3 H3 118.1(10) . . ?
C3 C4 C5 120.47(13) . . ?
C3 C4 H4 120.7(11) . . ?
C5 C4 H4 118.9(11) . . ?
C6 C5 C4 120.42(13) . . ?
C6 C5 H5 119.5(11) . . ?
C4 C5 H5 120.1(11) . . ?
C5 C6 C7 121.23(12) . . ?
C5 C6 H6 119.9(10) . . ?
C7 C6 H6 118.9(10) . . ?
C1 C7 C6 121.68(12) 2_565 . ?
C1 C7 C2 119.80(12) 2_565 . ?
C6 C7 C2 118.51(12) . . ?
C16 O2 H1O2 106.7(16) . . ?
C13 C8 C9 119.24(15) . . ?
C13 C8 C1 119.25(16) . . ?
C9 C8 C1 121.47(16) . . ?
C10 C9 C8 120.30(15) . . ?
C10 C9 H9 120.3(12) . . ?
C8 C9 H9 119.4(12) . . ?
C9 C10 C11 120.80(14) . . ?
C9 C10 H10 118.6(12) . . ?
C11 C10 H10 120.6(12) . . ?
C12 C11 C10 118.06(13) . . ?
C12 C11 C14 118.57(14) . . ?
C10 C11 C14 123.31(14) . . ?
C13 C12 C11 120.99(14) . . ?
C13 C12 H12 120.1(10) . . ?
C11 C12 H12 118.8(10) . . ?
C8 C13 C12 120.61(15) . . ?
C8 C13 H13 121.3(11) . . ?
C12 C13 H13 118.1(11) . . ?
C15 C14 C11 126.43(15) . . ?
C15 C14 H14 115.8(12) . . ?
C11 C14 H14 117.8(11) . . ?
C14 C15 C16 123.39(17) . . ?
C14 C15 H15 120.8(12) . . ?
C16 C15 H15 115.7(12) . . ?
O1 C16 O2 123.31(15) . . ?
O1 C16 C15 122.03(18) . . ?
O2 C16 C15 114.64(18) . . ?
C16F O2F H1OF 109.5 . . ?
C9F C8F C13F 121(2) . . ?
C9F C8F C1 119(2) . . ?
C13F C8F C1 120(2) . . ?
C8F C9F C10F 120(2) . . ?
C8F C9F H9F 120.1 . . ?
C10F C9F H9F 120.1 . . ?
C11F C10F C9F 119.0(18) . . ?
C11F C10F H10F 120.5 . . ?
C9F C10F H10F 120.5 . . ?
C12F C11F C10F 118.9(17) . . ?
C12F C11F C14F 122.5(18) . . ?
C10F C11F C14F 118.5(18) . . ?
C13F C12F C11F 123(2) . . ?
C13F C12F H12F 118.6 . . ?
C11F C12F H12F 118.6 . . ?
C12F C13F C8F 117(2) . . ?
C12F C13F H13F 121.3 . . ?
C8F C13F H13F 121.3 . . ?
C15F C14F C11F 130.0(19) . . ?
C15F C14F H14F 115.0 . . ?
C11F C14F H14F 115.0 . . ?
C14F C15F C16F 125.0(18) . . ?
C14F C15F H15F 117.5 . . ?
C16F C15F H15F 117.5 . . ?
O1F C16F O2F 127(2) . . ?
O1F C16F C15F 120(2) . . ?
O2F C16F C15F 112.0(19) . . ?
C19 N1 C17 120.26(14) . . ?
C19 N1 C18 123.7(2) . . ?
C17 N1 C18 116.0(2) . . ?
N1 C17 H17A 110.6(14) . . ?
N1 C17 H17B 109.6(16) . . ?
H17A C17 H17B 104(2) . . ?
N1 C17 H17C 110.8(13) . . ?
H17A C17 H17C 111.0(18) . . ?
H17B C17 H17C 110(2) . . ?
N1 C18 H18A 109.7(15) . . ?
N1 C18 H18B 107.2(16) . . ?
H18A C18 H18B 112(2) . . ?
N1 C18 H18C 109.5(14) . . ?
H18A C18 H18C 115.6(19) . . ?
H18B C18 H18C 103(2) . . ?
O3 C19 N1 120.01(16) . . ?
O3 C19 C20 121.29(17) . . ?
N1 C19 C20 118.70(14) . . ?
C19 C20 H20A 112.7(12) . . ?
C19 C20 H20B 111.3(13) . . ?
H20A C20 H20B 105.8(17) . . ?
C19 C20 H20C 108.0(14) . . ?
H20A C20 H20C 109.9(18) . . ?
H20B C20 H20C 109.0(18) . . ?
C19F N1F C18F 122(3) . . ?
C19F N1F C17F 120.8(18) . . ?
C18F N1F C17F 117(3) . . ?
N1F C17F H17D 109.5 . . ?
N1F C17F H17E 109.5 . . ?
H17D C17F H17E 109.5 . . ?
N1F C17F H17F 109.5 . . ?
H17D C17F H17F 109.5 . . ?
H17E C17F H17F 109.5 . . ?
N1F C18F H18D 109.5 . . ?
N1F C18F H18E 109.5 . . ?
H18D C18F H18E 109.5 . . ?
N1F C18F H18F 109.5 . . ?
H18D C18F H18F 109.5 . . ?
H18E C18F H18F 109.5 . . ?
O3F C19F N1F 119(2) . . ?
O3F C19F C20F 121(2) . . ?
N1F C19F C20F 120.3(19) . . ?
C19F C20F H20D 109.5 . . ?
C19F C20F H20E 109.5 . . ?
H20D C20F H20E 109.5 . . ?
C19F C20F H20F 109.5 . . ?
H20D C20F H20F 109.5 . . ?
H20E C20F H20F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H1O2 O3 1.02(3) 1.60(3) 2.591(2) 165(3) . yes
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.047

