# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2019

####################################################################### 
# 
# 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_1e
_database_code_depnum_ccdc_archive 'CCDC 1937762'
loop_
_audit_author_name
_audit_author_address
'Chao-Guo Yan' 'Yangzhou University'
_audit_update_record             
;
2019-07-02 deposited with the CCDC.	2019-09-02 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         'C33 H29 Cl N2 O3'
_chemical_formula_sum            'C33 H29 Cl N2 O3'
_chemical_formula_weight         537.03

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'

_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                   17.7343(17)
_cell_length_b                   13.4538(11)
_cell_length_c                   24.680(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.670(3)
_cell_angle_gamma                90
_cell_volume                     5869.0(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    9921
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      22.94

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_F_000             2256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.165
_shelx_estimated_absorpt_T_min   0.961
_shelx_estimated_absorpt_T_max   0.968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            57372
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.902
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11528
_reflns_number_gt                5825
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_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)+(0.0999P)²+1.7769P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11528
_refine_ls_number_parameters     709
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0662
_refine_ls_wR_factor_ref         0.2067
_refine_ls_wR_factor_gt          0.1679
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_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 0.32194(17) 0.3500(2) 0.26445(12) 0.0428(8) Uani 1 1 d . . . . .
H1 H 0.2808 0.3646 0.2875 0.051 Uiso 1 1 calc R U . . .
C2 C 0.3177(2) 0.4206(2) 0.21574(14) 0.0601(9) Uani 1 1 d . . . . .
H2A H 0.2861 0.3931 0.1855 0.072 Uiso 1 1 calc R U . . .
H2B H 0.2975 0.4847 0.2253 0.072 Uiso 1 1 calc R U . . .
C3 C 0.3995(2) 0.4300(3) 0.20175(15) 0.0702(11) Uani 1 1 d . . . . .
H3A H 0.4125 0.3768 0.1777 0.084 Uiso 1 1 calc R U . . .
H3B H 0.4078 0.4933 0.1844 0.084 Uiso 1 1 calc R U . . .
C4 C 0.4453(2) 0.4229(3) 0.25573(15) 0.0620(10) Uani 1 1 d . . . . .
H4A H 0.4898 0.3818 0.2528 0.074 Uiso 1 1 calc R U . . .
H4B H 0.4615 0.4884 0.2685 0.074 Uiso 1 1 calc R U . . .
C5 C 0.40371(19) 0.3910(2) 0.34630(14) 0.0505(8) Uani 1 1 d . . . . .
H5 H 0.4453 0.4284 0.3595 0.061 Uiso 1 1 calc R U . . .
C6 C 0.3583(2) 0.3555(2) 0.38398(13) 0.0510(9) Uani 1 1 d . . . . .
C7 C 0.3711(3) 0.3981(3) 0.43833(16) 0.0705(11) Uani 1 1 d . . . . .
C8 C 0.3627(3) 0.3731(4) 0.53311(15) 0.1085(17) Uani 1 1 d . . . . .
H8A H 0.4123 0.4022 0.5355 0.163 Uiso 1 1 calc R U . . .
H8B H 0.3628 0.3160 0.5565 0.163 Uiso 1 1 calc R U . . .
H8C H 0.3269 0.4209 0.5442 0.163 Uiso 1 1 calc R U . . .
C9 C 0.2292(2) 0.1831(3) 0.16925(14) 0.0632(10) Uani 1 1 d . . . . .
H9 H 0.2706 0.1781 0.1485 0.076 Uiso 1 1 calc R U . . .
C10 C 0.1574(2) 0.1612(3) 0.14542(16) 0.0709(11) Uani 1 1 d . . . . .
H10 H 0.1507 0.1397 0.1095 0.085 Uiso 1 1 calc R U . . .
C11 C 0.0968(2) 0.1717(2) 0.17583(17) 0.0610(10) Uani 1 1 d . . . . .
C12 C 0.1061(2) 0.1997(2) 0.22907(16) 0.0599(9) Uani 1 1 d . . . . .
H12 H 0.0644 0.2059 0.2494 0.072 Uiso 1 1 calc R U . . .
C13 C 0.17794(19) 0.2187(2) 0.25232(14) 0.0508(8) Uani 1 1 d . . . . .
H13 H 0.1844 0.2365 0.2888 0.061 Uiso 1 1 calc R U . . .
C14 C 0.24045(17) 0.2121(2) 0.22268(12) 0.0424(8) Uani 1 1 d . . . . .
C15 C 0.31890(16) 0.2403(2) 0.24759(12) 0.0396(7) Uani 1 1 d . . . . .
H15 H 0.3531 0.2333 0.2186 0.047 Uiso 1 1 calc R U . . .
C16 C 0.34721(16) 0.1683(2) 0.29216(12) 0.0386(7) Uani 1 1 d . . . . .
C17 C 0.38267(16) 0.0781(2) 0.27624(13) 0.0434(8) Uani 1 1 d . . . . .
C18 C 0.40061(17) 0.0579(2) 0.22011(13) 0.0431(8) Uani 1 1 d . . . . .
C19 C 0.37254(19) -0.0259(3) 0.19326(16) 0.0623(10) Uani 1 1 d . . . . .
H19 H 0.3404 -0.0678 0.2105 0.075 Uiso 1 1 calc R U . . .
C20 C 0.3907(2) -0.0491(3) 0.14198(17) 0.0777(12) Uani 1 1 d . . . . .
H20 H 0.3700 -0.1056 0.1249 0.093 Uiso 1 1 calc R U . . .
C21 C 0.4391(2) 0.0097(3) 0.11521(15) 0.0689(11) Uani 1 1 d . . . . .
C22 C 0.4616(3) -0.0174(4) 0.05944(18) 0.1107(17) Uani 1 1 d . . . . .
H22A H 0.5080 -0.0545 0.0629 0.166 Uiso 1 1 calc R U . . .
H22B H 0.4687 0.0421 0.0390 0.166 Uiso 1 1 calc R U . . .
H22C H 0.4225 -0.0570 0.0409 0.166 Uiso 1 1 calc R U . . .
C23 C 0.46813(19) 0.0933(3) 0.14153(15) 0.0661(10) Uani 1 1 d . . . . .
H23 H 0.5010 0.1342 0.1243 0.079 Uiso 1 1 calc R U . . .
C24 C 0.44923(18) 0.1174(2) 0.19342(14) 0.0525(9) Uani 1 1 d . . . . .
H24 H 0.4695 0.1741 0.2104 0.063 Uiso 1 1 calc R U . . .
C25 C 0.3050(2) 0.2735(2) 0.37201(12) 0.0489(8) Uani 1 1 d . . . . .
C26 C 0.33664(17) 0.1816(2) 0.34657(13) 0.0431(8) Uani 1 1 d . . . . .
C27 C 0.35793(19) 0.1039(2) 0.38427(13) 0.0520(8) Uani 1 1 d . . . . .
C28 C 0.3494(2) 0.1109(3) 0.44065(15) 0.0707(11) Uani 1 1 d . . . . .
H28 H 0.3279 0.1680 0.4541 0.085 Uiso 1 1 calc R U . . .
C29 C 0.3717(3) 0.0364(4) 0.47578(18) 0.0995(15) Uani 1 1 d . . . . .
C30 C 0.3645(4) 0.0452(4) 0.53626(18) 0.150(3) Uani 1 1 d . . . . .
H30A H 0.3273 0.0946 0.5428 0.224 Uiso 1 1 calc R U . . .
H30B H 0.4124 0.0642 0.5542 0.224 Uiso 1 1 calc R U . . .
H30C H 0.3493 -0.0177 0.5502 0.224 Uiso 1 1 calc R U . . .
C31 C 0.4040(4) -0.0492(4) 0.4541(2) 0.130(2) Uani 1 1 d . . . . .
H31 H 0.4209 -0.0999 0.4777 0.156 Uiso 1 1 calc R U . . .
C32 C 0.4114(3) -0.0602(3) 0.39998(19) 0.0997(16) Uani 1 1 d . . . . .
H32 H 0.4309 -0.1189 0.3869 0.120 Uiso 1 1 calc R U . . .
C33 C 0.3897(2) 0.0171(2) 0.36414(15) 0.0596(9) Uani 1 1 d . . . . .
C34 C 0.19562(17) 0.5473(2) 0.75334(12) 0.0427(8) Uani 1 1 d . . . . .
H34 H 0.2396 0.5595 0.7326 0.051 Uiso 1 1 calc R U . . .
C35 C 0.19450(19) 0.6229(2) 0.79953(14) 0.0568(9) Uani 1 1 d . . . . .
H35A H 0.2231 0.5989 0.8321 0.068 Uiso 1 1 calc R U . . .
H35B H 0.2152 0.6862 0.7892 0.068 Uiso 1 1 calc R U . . .
C36 C 0.1107(2) 0.6320(3) 0.80820(16) 0.0720(11) Uani 1 1 d . . . . .
H36A H 0.0957 0.5811 0.8330 0.086 Uiso 1 1 calc R U . . .
H36B H 0.0998 0.6967 0.8231 0.086 Uiso 1 1 calc R U . . .
C37 C 0.06963(19) 0.6191(3) 0.75308(15) 0.0590(9) Uani 1 1 d . . . . .
H37A H 0.0258 0.5765 0.7550 0.071 Uiso 1 1 calc R U . . .
H37B H 0.0531 0.6828 0.7380 0.071 Uiso 1 1 calc R U . . .
C38 C 0.12225(18) 0.5816(2) 0.66601(14) 0.0492(8) Uani 1 1 d . . . . .
H38 H 0.0827 0.6191 0.6496 0.059 Uiso 1 1 calc R U . . .
C39 C 0.17181(18) 0.5405(2) 0.63276(13) 0.0454(8) Uani 1 1 d . . . . .
C40 C 0.1725(2) 0.5821(3) 0.57777(15) 0.0591(9) Uani 1 1 d . . . . .
C41 C 0.2260(3) 0.5748(4) 0.49271(16) 0.1043(16) Uani 1 1 d . . . . .
H41A H 0.1785 0.5720 0.4711 0.157 Uiso 1 1 calc R U . . .
H41B H 0.2632 0.5374 0.4752 0.157 Uiso 1 1 calc R U . . .
H41C H 0.2422 0.6427 0.4966 0.157 Uiso 1 1 calc R U . . .
C42 C 0.2879(2) 0.3850(3) 0.85220(14) 0.0604(9) Uani 1 1 d . . . . .
H42 H 0.2474 0.3848 0.8739 0.073 Uiso 1 1 calc R U . . .
C43 C 0.3597(3) 0.3583(3) 0.87514(16) 0.0723(11) Uani 1 1 d . . . . .
H43 H 0.3670 0.3400 0.9115 0.087 Uiso 1 1 calc R U . . .
C44 C 0.4188(2) 0.3598(2) 0.84328(16) 0.0587(10) Uani 1 1 d . . . . .
C45 C 0.40882(19) 0.3857(2) 0.78988(15) 0.0577(9) Uani 1 1 d . . . . .
H45 H 0.4497 0.3866 0.7686 0.069 Uiso 1 1 calc R U . . .
C46 C 0.33753(18) 0.4106(2) 0.76775(13) 0.0511(8) Uani 1 1 d . . . . .
H46 H 0.3307 0.4275 0.7311 0.061 Uiso 1 1 calc R U . . .
C47 C 0.27563(17) 0.4112(2) 0.79861(12) 0.0399(7) Uani 1 1 d . . . . .
C48 C 0.19731(16) 0.43981(19) 0.77415(12) 0.0384(7) Uani 1 1 d . . . . .
H48 H 0.1639 0.4374 0.8038 0.046 Uiso 1 1 calc R U . . .
C49 C 0.16699(15) 0.36390(19) 0.73222(11) 0.0346(7) Uani 1 1 d . . . . .
C50 C 0.12897(15) 0.2772(2) 0.75062(12) 0.0367(7) Uani 1 1 d . . . . .
C51 C 0.11190(16) 0.2622(2) 0.80796(12) 0.0385(7) Uani 1 1 d . . . . .
C52 C 0.06581(17) 0.3254(2) 0.83516(13) 0.0463(8) Uani 1 1 d . . . . .
H52 H 0.0461 0.3821 0.8177 0.056 Uiso 1 1 calc R U . . .
C53 C 0.04866(18) 0.3051(2) 0.88792(13) 0.0497(8) Uani 1 1 d . . . . .
H53 H 0.0180 0.3488 0.9054 0.060 Uiso 1 1 calc R U . . .
C54 C 0.07633(18) 0.2210(2) 0.91508(13) 0.0488(8) Uani 1 1 d . . . . .
C55 C 0.0575(2) 0.1993(3) 0.97251(14) 0.0765(11) Uani 1 1 d . . . . .
H55A H 0.0473 0.1296 0.9761 0.115 Uiso 1 1 calc R U . . .
H55B H 0.0138 0.2369 0.9805 0.115 Uiso 1 1 calc R U . . .
H55C H 0.0996 0.2175 0.9975 0.115 Uiso 1 1 calc R U . . .
C56 C 0.1203(2) 0.1576(2) 0.88764(14) 0.0581(9) Uani 1 1 d . . . . .
H56 H 0.1389 0.1001 0.9048 0.070 Uiso 1 1 calc R U . . .
C57 C 0.13769(19) 0.1771(2) 0.83530(14) 0.0535(9) Uani 1 1 d . . . . .
H57 H 0.1674 0.1321 0.8179 0.064 Uiso 1 1 calc R U . . .
C58 C 0.21901(18) 0.4547(2) 0.65022(12) 0.0407(7) Uani 1 1 d . . . . .
C59 C 0.17869(15) 0.3702(2) 0.67779(12) 0.0365(7) Uani 1 1 d . . . . .
C60 C 0.15383(16) 0.2917(2) 0.64155(12) 0.0384(7) Uani 1 1 d . . . . .
C61 C 0.16204(18) 0.2912(2) 0.58511(13) 0.0500(8) Uani 1 1 d . . . . .
H61 H 0.1847 0.3455 0.5698 0.060 Uiso 1 1 calc R U . . .
C62 C 0.1380(2) 0.2143(3) 0.55229(14) 0.0594(9) Uani 1 1 d . . . . .
C63 C 0.1479(3) 0.2150(3) 0.49243(15) 0.0925(14) Uani 1 1 d . . . . .
H63A H 0.1795 0.2700 0.4841 0.139 Uiso 1 1 calc R U . . .
H63B H 0.0994 0.2216 0.4725 0.139 Uiso 1 1 calc R U . . .
H63C H 0.1712 0.1540 0.4825 0.139 Uiso 1 1 calc R U . . .
C64 C 0.1039(2) 0.1318(3) 0.57620(15) 0.0679(11) Uani 1 1 d . . . . .
H64 H 0.0874 0.0784 0.5544 0.082 Uiso 1 1 calc R U . . .
C65 C 0.0945(2) 0.1290(2) 0.63025(14) 0.0586(9) Uani 1 1 d . . . . .
H65 H 0.0719 0.0739 0.6449 0.070 Uiso 1 1 calc R U . . .
C66 C 0.11887(17) 0.2088(2) 0.66434(13) 0.0422(8) Uani 1 1 d . . . . .
Cl1 Cl 0.00560(6) 0.14833(8) 0.14642(5) 0.0947(4) Uani 1 1 d . . . . .
Cl2 Cl 0.50887(6) 0.32641(9) 0.87090(5) 0.1008(4) Uani 1 1 d . . . . .
N1 N 0.39468(14) 0.37784(18) 0.29277(11) 0.0464(7) Uani 1 1 d . . . . .
N2 N 0.40209(16) 0.00529(19) 0.31072(12) 0.0572(7) Uani 1 1 d . . . . .
N3 N 0.12557(14) 0.57269(17) 0.71971(11) 0.0449(6) Uani 1 1 d . . . . .
N4 N 0.10703(14) 0.20325(17) 0.71813(10) 0.0433(6) Uani 1 1 d . . . . .
O1 O 0.4065(2) 0.4736(2) 0.44911(11) 0.1003(10) Uani 1 1 d . . . . .
O2 O 0.34175(18) 0.3427(2) 0.47695(10) 0.0847(9) Uani 1 1 d . . . . .
O3 O 0.24088(14) 0.26998(18) 0.38687(9) 0.0643(7) Uani 1 1 d . . . . .
O4 O 0.13500(18) 0.65283(19) 0.56175(11) 0.0866(9) Uani 1 1 d . . . . .
O5 O 0.21718(15) 0.5329(2) 0.54583(10) 0.0742(7) Uani 1 1 d . . . . .
O6 O 0.28361(12) 0.44066(15) 0.63888(8) 0.0491(6) 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
C1 N1 1.465(4) . ?
C1 C2 1.529(4) . ?
C1 C15 1.533(4) . ?
C1 H1 0.9800 . ?
C2 C3 1.524(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.506(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.465(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N1 1.330(4) . ?
C5 C6 1.366(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.460(5) . ?
C6 C25 1.466(5) . ?
C7 O1 1.213(5) . ?
C7 O2 1.348(5) . ?
C8 O2 1.464(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C14 1.374(4) . ?
C9 C10 1.390(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.367(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.364(5) . ?
C11 Cl1 1.747(4) . ?
C12 C13 1.379(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.380(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.523(4) . ?
C15 C16 1.520(4) . ?
C15 H15 0.9800 . ?
C16 C26 1.383(4) . ?
C16 C17 1.436(4) . ?
C17 N2 1.325(4) . ?
C17 C18 1.472(4) . ?
C18 C19 1.380(4) . ?
C18 C24 1.382(4) . ?
C19 C20 1.367(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.375(5) . ?
C20 H20 0.9300 . ?
C21 C23 1.377(5) . ?
C21 C22 1.509(5) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.388(4) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O3 1.224(4) . ?
C25 C26 1.515(4) . ?
C26 C27 1.430(4) . ?
C27 C33 1.405(5) . ?
C27 C28 1.415(5) . ?
C28 C29 1.363(5) . ?
C28 H28 0.9300 . ?
C29 C31 1.411(6) . ?
C29 C30 1.513(6) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.361(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.399(5) . ?
C32 H32 0.9300 . ?
C33 N2 1.363(4) . ?
C34 N3 1.477(4) . ?
C34 C35 1.528(4) . ?
C34 C48 1.534(4) . ?
C34 H34 0.9800 . ?
C35 C36 1.524(5) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.500(5) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 N3 1.478(4) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 N3 1.327(4) . ?
C38 C39 1.367(4) . ?
C38 H38 0.9300 . ?
C39 C40 1.469(5) . ?
C39 C58 1.470(4) . ?
C40 O4 1.209(4) . ?
C40 O5 1.338(4) . ?
C41 O5 1.447(4) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 C47 1.369(4) . ?
C42 C43 1.398(5) . ?
C42 H42 0.9300 . ?
C43 C44 1.361(5) . ?
C43 H43 0.9300 . ?
C44 C45 1.361(5) . ?
C44 Cl2 1.744(4) . ?
C45 C46 1.377(4) . ?
C45 H45 0.9300 . ?
C46 C47 1.386(4) . ?
C46 H46 0.9300 . ?
C47 C48 1.518(4) . ?
C48 C49 1.521(4) . ?
C48 H48 0.9800 . ?
C49 C59 1.378(4) . ?
C49 C50 1.439(4) . ?
C50 N4 1.317(4) . ?
C50 C51 1.485(4) . ?
C51 C57 1.388(4) . ?
C51 C52 1.389(4) . ?
C52 C53 1.388(4) . ?
C52 H52 0.9300 . ?
C53 C54 1.385(4) . ?
C53 H53 0.9300 . ?
C54 C56 1.371(4) . ?
C54 C55 1.511(5) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 C57 1.377(4) . ?
C56 H56 0.9300 . ?
C57 H57 0.9300 . ?
C58 O6 1.216(3) . ?
C58 C59 1.531(4) . ?
C59 C60 1.430(4) . ?
C60 C61 1.412(4) . ?
C60 C66 1.415(4) . ?
C61 C62 1.361(4) . ?
C61 H61 0.9300 . ?
C62 C64 1.416(5) . ?
C62 C63 1.502(5) . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C64 C65 1.358(5) . ?
C64 H64 0.9300 . ?
C65 C66 1.410(4) . ?
C65 H65 0.9300 . ?
C66 N4 1.363(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
N1 C1 C2 101.6(2) . . ?
N1 C1 C15 112.7(2) . . ?
C2 C1 C15 112.7(3) . . ?
N1 C1 H1 109.8 . . ?
C2 C1 H1 109.8 . . ?
C15 C1 H1 109.8 . . ?
C3 C2 C1 104.0(3) . . ?
C3 C2 H2A 110.9 . . ?
C1 C2 H2A 110.9 . . ?
C3 C2 H2B 110.9 . . ?
C1 C2 H2B 110.9 . . ?
H2A C2 H2B 109.0 . . ?
C4 C3 C2 104.5(3) . . ?
C4 C3 H3A 110.9 . . ?
C2 C3 H3A 110.9 . . ?
C4 C3 H3B 110.9 . . ?
C2 C3 H3B 110.9 . . ?
H3A C3 H3B 108.9 . . ?
N1 C4 C3 105.3(3) . . ?
N1 C4 H4A 110.7 . . ?
C3 C4 H4A 110.7 . . ?
N1 C4 H4B 110.7 . . ?
C3 C4 H4B 110.7 . . ?
H4A C4 H4B 108.8 . . ?
N1 C5 C6 126.9(3) . . ?
N1 C5 H5 116.6 . . ?
C6 C5 H5 116.6 . . ?
C5 C6 C7 115.6(4) . . ?
C5 C6 C25 122.2(3) . . ?
C7 C6 C25 122.0(3) . . ?
O1 C7 O2 122.1(4) . . ?
O1 C7 C6 124.8(4) . . ?
O2 C7 C6 113.1(4) . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C14 C9 C10 121.5(3) . . ?
C14 C9 H9 119.2 . . ?
C10 C9 H9 119.2 . . ?
C11 C10 C9 118.6(3) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C12 C11 C10 121.3(3) . . ?
C12 C11 Cl1 119.0(3) . . ?
C10 C11 Cl1 119.7(3) . . ?
C11 C12 C13 119.1(3) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C12 C13 C14 121.5(3) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
C9 C14 C13 117.9(3) . . ?
C9 C14 C15 121.0(3) . . ?
C13 C14 C15 121.1(3) . . ?
C16 C15 C14 111.7(2) . . ?
C16 C15 C1 114.5(2) . . ?
C14 C15 C1 111.1(2) . . ?
C16 C15 H15 106.3 . . ?
C14 C15 H15 106.3 . . ?
C1 C15 H15 106.3 . . ?
C26 C16 C17 118.2(3) . . ?
C26 C16 C15 123.9(2) . . ?
C17 C16 C15 117.8(3) . . ?
N2 C17 C16 123.1(3) . . ?
N2 C17 C18 113.8(3) . . ?
C16 C17 C18 123.1(3) . . ?
C19 C18 C24 117.3(3) . . ?
C19 C18 C17 120.4(3) . . ?
C24 C18 C17 122.2(3) . . ?
C20 C19 C18 121.9(3) . . ?
C20 C19 H19 119.1 . . ?
C18 C19 H19 119.1 . . ?
C19 C20 C21 121.1(3) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C20 C21 C23 117.9(3) . . ?
C20 C21 C22 121.4(4) . . ?
C23 C21 C22 120.7(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 C24 121.1(4) . . ?
C21 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C18 C24 C23 120.8(3) . . ?
C18 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
O3 C25 C6 124.6(3) . . ?
O3 C25 C26 118.5(3) . . ?
C6 C25 C26 116.3(3) . . ?
C16 C26 C27 119.2(3) . . ?
C16 C26 C25 126.3(3) . . ?
C27 C26 C25 114.5(3) . . ?
C33 C27 C28 118.8(3) . . ?
C33 C27 C26 118.0(3) . . ?
C28 C27 C26 123.2(3) . . ?
C29 C28 C27 121.8(4) . . ?
C29 C28 H28 119.1 . . ?
C27 C28 H28 119.1 . . ?
C28 C29 C31 117.7(4) . . ?
C28 C29 C30 121.8(4) . . ?
C31 C29 C30 120.5(4) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C29 122.4(4) . . ?
C32 C31 H31 118.8 . . ?
C29 C31 H31 118.8 . . ?
C31 C32 C33 119.7(4) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
N2 C33 C32 117.8(3) . . ?
N2 C33 C27 122.7(3) . . ?
C32 C33 C27 119.5(4) . . ?
N3 C34 C35 101.8(2) . . ?
N3 C34 C48 113.5(2) . . ?
C35 C34 C48 112.2(3) . . ?
N3 C34 H34 109.7 . . ?
C35 C34 H34 109.7 . . ?
C48 C34 H34 109.7 . . ?
C36 C35 C34 103.3(3) . . ?
C36 C35 H35A 111.1 . . ?
C34 C35 H35A 111.1 . . ?
C36 C35 H35B 111.1 . . ?
C34 C35 H35B 111.1 . . ?
H35A C35 H35B 109.1 . . ?
C37 C36 C35 105.7(3) . . ?
C37 C36 H36A 110.6 . . ?
C35 C36 H36A 110.6 . . ?
C37 C36 H36B 110.6 . . ?
C35 C36 H36B 110.6 . . ?
H36A C36 H36B 108.7 . . ?
N3 C37 C36 104.8(3) . . ?
N3 C37 H37A 110.8 . . ?
C36 C37 H37A 110.8 . . ?
N3 C37 H37B 110.8 . . ?
C36 C37 H37B 110.8 . . ?
H37A C37 H37B 108.9 . . ?
N3 C38 C39 125.8(3) . . ?
N3 C38 H38 117.1 . . ?
C39 C38 H38 117.1 . . ?
C38 C39 C40 117.0(3) . . ?
C38 C39 C58 121.3(3) . . ?
C40 C39 C58 121.5(3) . . ?
O4 C40 O5 122.2(3) . . ?
O4 C40 C39 123.8(4) . . ?
O5 C40 C39 113.9(3) . . ?
O5 C41 H41A 109.5 . . ?
O5 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O5 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C47 C42 C43 121.7(3) . . ?
C47 C42 H42 119.2 . . ?
C43 C42 H42 119.2 . . ?
C44 C43 C42 118.8(3) . . ?
C44 C43 H43 120.6 . . ?
C42 C43 H43 120.6 . . ?
C45 C44 C43 121.2(3) . . ?
C45 C44 Cl2 119.2(3) . . ?
C43 C44 Cl2 119.6(3) . . ?
C44 C45 C46 119.3(3) . . ?
C44 C45 H45 120.3 . . ?
C46 C45 H45 120.3 . . ?
C45 C46 C47 121.7(3) . . ?
C45 C46 H46 119.1 . . ?
C47 C46 H46 119.1 . . ?
C42 C47 C46 117.3(3) . . ?
C42 C47 C48 121.2(3) . . ?
C46 C47 C48 121.5(3) . . ?
C47 C48 C49 111.2(2) . . ?
C47 C48 C34 111.3(2) . . ?
C49 C48 C34 114.2(2) . . ?
C47 C48 H48 106.5 . . ?
C49 C48 H48 106.5 . . ?
C34 C48 H48 106.5 . . ?
C59 C49 C50 118.0(3) . . ?
C59 C49 C48 123.3(2) . . ?
C50 C49 C48 118.6(2) . . ?
N4 C50 C49 122.9(3) . . ?
N4 C50 C51 113.9(2) . . ?
C49 C50 C51 123.2(3) . . ?
C57 C51 C52 117.0(3) . . ?
C57 C51 C50 119.4(3) . . ?
C52 C51 C50 123.4(3) . . ?
C53 C52 C51 121.0(3) . . ?
C53 C52 H52 119.5 . . ?
C51 C52 H52 119.5 . . ?
C54 C53 C52 121.2(3) . . ?
C54 C53 H53 119.4 . . ?
C52 C53 H53 119.4 . . ?
C56 C54 C53 117.5(3) . . ?
C56 C54 C55 121.4(3) . . ?
C53 C54 C55 121.0(3) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 C57 121.7(3) . . ?
C54 C56 H56 119.2 . . ?
C57 C56 H56 119.2 . . ?
C56 C57 C51 121.5(3) . . ?
C56 C57 H57 119.2 . . ?
C51 C57 H57 119.2 . . ?
O6 C58 C39 125.4(3) . . ?
O6 C58 C59 118.0(3) . . ?
C39 C58 C59 116.0(3) . . ?
C49 C59 C60 120.1(3) . . ?
C49 C59 C58 126.2(3) . . ?
C60 C59 C58 113.7(2) . . ?
C61 C60 C66 118.1(3) . . ?
C61 C60 C59 124.7(3) . . ?
C66 C60 C59 117.1(3) . . ?
C62 C61 C60 122.6(3) . . ?
C62 C61 H61 118.7 . . ?
C60 C61 H61 118.7 . . ?
C61 C62 C64 118.1(3) . . ?
C61 C62 C63 121.6(3) . . ?
C64 C62 C63 120.2(3) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C65 C64 C62 121.5(3) . . ?
C65 C64 H64 119.3 . . ?
C62 C64 H64 119.3 . . ?
C64 C65 C66 120.6(3) . . ?
C64 C65 H65 119.7 . . ?
C66 C65 H65 119.7 . . ?
N4 C66 C65 118.4(3) . . ?
N4 C66 C60 122.5(3) . . ?
C65 C66 C60 119.1(3) . . ?
C5 N1 C4 122.3(3) . . ?
C5 N1 C1 122.6(3) . . ?
C4 N1 C1 111.7(3) . . ?
C17 N2 C33 118.7(3) . . ?
C38 N3 C34 123.3(3) . . ?
C38 N3 C37 122.7(3) . . ?
C34 N3 C37 110.9(3) . . ?
C50 N4 C66 119.4(2) . . ?
C7 O2 C8 115.6(4) . . ?
C40 O5 C41 117.0(3) . . ?

_refine_diff_density_max         0.343
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.049



####################################################################### 
# 
# 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_2f
_database_code_depnum_ccdc_archive 'CCDC 1937764'
loop_
_audit_author_name
_audit_author_address
'Chao-Guo Yan' 'Yangzhou University'
_audit_update_record             
;
2019-07-02 deposited with the CCDC.	2019-09-02 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         'C44 H39 N3 O7'
_chemical_formula_sum            'C44 H39 N3 O7'
_chemical_formula_weight         721.78

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                   9.8530(14)
_cell_length_b                   14.0452(18)
_cell_length_c                   15.201(2)
_cell_angle_alpha                111.663(4)
_cell_angle_beta                 93.543(5)
_cell_angle_gamma                102.840(4)
_cell_volume                     1882.0(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    3871
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      23.06

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_F_000             760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.087
_shelx_estimated_absorpt_T_min   0.979
_shelx_estimated_absorpt_T_max   0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27139
_diffrn_reflns_av_unetI/netI     0.1423
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.147
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             7339
_reflns_number_gt                3409
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_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)+(0.0742P)²+0.5858P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7339
_refine_ls_number_parameters     491
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1855
_refine_ls_R_factor_gt           0.0718
_refine_ls_wR_factor_ref         0.1845
_refine_ls_wR_factor_gt          0.1451
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_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 0.4811(3) 0.0270(2) 0.1391(2) 0.0333(8) Uani 1 1 d . . . . .
H1 H 0.4214 -0.0134 0.0764 0.040 Uiso 1 1 calc R U . . .
C2 C 0.6343(4) 0.0570(3) 0.1254(2) 0.0464(9) Uani 1 1 d . . . . .
H2A H 0.6522 0.0040 0.0683 0.056 Uiso 1 1 calc R U . . .
H2B H 0.6582 0.1254 0.1204 0.056 Uiso 1 1 calc R U . . .
C3 C 0.7164(4) 0.0613(3) 0.2139(3) 0.0636(12) Uani 1 1 d . . . . .
H3A H 0.7354 0.1315 0.2647 0.076 Uiso 1 1 calc R U . . .
H3B H 0.8054 0.0450 0.2006 0.076 Uiso 1 1 calc R U . . .
C4 C 0.6261(4) -0.0203(3) 0.2429(3) 0.0525(10) Uani 1 1 d . . . . .
H4A H 0.6598 -0.0837 0.2251 0.063 Uiso 1 1 calc R U . . .
H4B H 0.6257 0.0078 0.3116 0.063 Uiso 1 1 calc R U . . .
C5 C 0.3911(4) -0.1355(3) 0.1681(2) 0.0435(9) Uani 1 1 d . . . . .
H5 H 0.4181 -0.1842 0.1886 0.052 Uiso 1 1 calc R U . . .
C6 C 0.2587(4) -0.1655(2) 0.1181(2) 0.0396(9) Uani 1 1 d . . . . .
C7 C 0.1795(5) -0.2770(3) 0.0800(3) 0.0532(11) Uani 1 1 d . . . . .
C8 C 0.1790(6) -0.4488(3) 0.0749(4) 0.109(2) Uani 1 1 d . . . . .
H8A H 0.1050 -0.4526 0.1128 0.164 Uiso 1 1 calc R U . . .
H8B H 0.2439 -0.4859 0.0873 0.164 Uiso 1 1 calc R U . . .
H8C H 0.1391 -0.4810 0.0082 0.164 Uiso 1 1 calc R U . . .
C9 C 0.1867(4) -0.0870(2) 0.1107(2) 0.0359(8) Uani 1 1 d . . . . .
C10 C 0.1970(3) 0.0067(2) 0.2051(2) 0.0283(8) Uani 1 1 d . . . . .
C11 C 0.0849(3) -0.0139(2) 0.2600(2) 0.0299(8) Uani 1 1 d . . . . .
C12 C -0.0116(3) -0.1133(3) 0.2322(2) 0.0376(9) Uani 1 1 d . . . . .
H12 H -0.0068 -0.1672 0.1752 0.045 Uiso 1 1 calc R U . . .
C13 C -0.1136(4) -0.1350(3) 0.2854(3) 0.0407(9) Uani 1 1 d . . . . .
C14 C -0.2164(4) -0.2437(3) 0.2514(3) 0.0661(12) Uani 1 1 d . . . . .
H14A H -0.2962 -0.2468 0.2099 0.099 Uiso 1 1 calc R U . . .
H14B H -0.2472 -0.2564 0.3057 0.099 Uiso 1 1 calc R U . . .
H14C H -0.1708 -0.2968 0.2170 0.099 Uiso 1 1 calc R U . . .
C15 C -0.1196(4) -0.0540(3) 0.3690(3) 0.0436(9) Uani 1 1 d . . . . .
H15 H -0.1868 -0.0666 0.4065 0.052 Uiso 1 1 calc R U . . .
C16 C -0.0276(4) 0.0462(3) 0.3987(2) 0.0407(9) Uani 1 1 d . . . . .
H16 H -0.0350 0.0995 0.4554 0.049 Uiso 1 1 calc R U . . .
C17 C 0.0753(3) 0.0685(2) 0.3456(2) 0.0317(8) Uani 1 1 d . . . . .
C18 C 0.1681(3) 0.2479(2) 0.4686(2) 0.0378(9) Uani 1 1 d . . . . .
H18A H 0.2567 0.3024 0.4865 0.045 Uiso 1 1 calc R U . . .
H18B H 0.1678 0.2122 0.5125 0.045 Uiso 1 1 calc R U . . .
C19 C 0.0499(4) 0.3013(3) 0.4825(2) 0.0403(9) Uani 1 1 d . . . . .
C20 C 0.0350(4) 0.3609(3) 0.5741(3) 0.0639(12) Uani 1 1 d . . . . .
H20 H 0.0953 0.3647 0.6256 0.077 Uiso 1 1 calc R U . . .
C21 C -0.0674(5) 0.4152(4) 0.5915(3) 0.0825(15) Uani 1 1 d . . . . .
H21 H -0.0764 0.4546 0.6542 0.099 Uiso 1 1 calc R U . . .
C22 C -0.1554(5) 0.4110(3) 0.5169(4) 0.0706(13) Uani 1 1 d . . . . .
H22 H -0.2246 0.4477 0.5285 0.085 Uiso 1 1 calc R U . . .
C23 C -0.1425(4) 0.3536(3) 0.4256(3) 0.0639(12) Uani 1 1 d . . . . .
H23 H -0.2025 0.3511 0.3746 0.077 Uiso 1 1 calc R U . . .
C24 C -0.0395(4) 0.2983(3) 0.4082(3) 0.0500(10) Uani 1 1 d . . . . .
H24 H -0.0311 0.2589 0.3453 0.060 Uiso 1 1 calc R U . . .
C25 C 0.5189(4) 0.2738(3) 0.1443(2) 0.0428(9) Uani 1 1 d . . . . .
H25 H 0.6023 0.2916 0.1859 0.051 Uiso 1 1 calc R U . . .
C26 C 0.5025(5) 0.3338(3) 0.0926(3) 0.0505(10) Uani 1 1 d . . . . .
C27 C 0.3827(5) 0.3099(3) 0.0295(3) 0.0637(12) Uani 1 1 d . . . . .
H27 H 0.3736 0.3515 -0.0048 0.076 Uiso 1 1 calc R U . . .
C28 C 0.2766(5) 0.2229(3) 0.0184(3) 0.0592(11) Uani 1 1 d . . . . .
H28 H 0.1946 0.2046 -0.0246 0.071 Uiso 1 1 calc R U . . .
C29 C 0.2900(4) 0.1617(3) 0.0705(2) 0.0436(9) Uani 1 1 d . . . . .
H29 H 0.2168 0.1031 0.0624 0.052 Uiso 1 1 calc R U . . .
C30 C 0.4112(4) 0.1872(2) 0.1343(2) 0.0334(8) Uani 1 1 d . . . . .
C31 C 0.4275(3) 0.1232(2) 0.1949(2) 0.0297(8) Uani 1 1 d . . . . .
H31 H 0.5030 0.1697 0.2485 0.036 Uiso 1 1 calc R U . . .
C32 C 0.2988(3) 0.0970(2) 0.2396(2) 0.0269(7) Uani 1 1 d . . . . .
C33 C 0.3019(3) 0.1821(2) 0.3393(2) 0.0282(8) Uani 1 1 d . . . . .
C34 C 0.3467(3) 0.2930(2) 0.3375(2) 0.0303(8) Uani 1 1 d . . . . .
C35 C 0.2554(4) 0.3215(3) 0.2844(2) 0.0379(9) Uani 1 1 d . . . . .
H35 H 0.1675 0.2752 0.2541 0.045 Uiso 1 1 calc R U . . .
C36 C 0.2948(4) 0.4182(3) 0.2767(3) 0.0468(10) Uani 1 1 d . . . . .
H36 H 0.2330 0.4360 0.2404 0.056 Uiso 1 1 calc R U . . .
C37 C 0.4239(5) 0.4893(3) 0.3214(3) 0.0507(10) Uani 1 1 d . . . . .
C38 C 0.4646(5) 0.5957(3) 0.3119(3) 0.0878(15) Uani 1 1 d . . . . .
H38A H 0.3837 0.6235 0.3137 0.132 Uiso 1 1 calc R U . . .
H38B H 0.4983 0.5863 0.2521 0.132 Uiso 1 1 calc R U . . .
H38C H 0.5375 0.6446 0.3639 0.132 Uiso 1 1 calc R U . . .
C39 C 0.5133(4) 0.4603(3) 0.3735(3) 0.0543(11) Uani 1 1 d . . . . .
H39 H 0.6012 0.5067 0.4038 0.065 Uiso 1 1 calc R U . . .
C40 C 0.4757(4) 0.3638(3) 0.3822(2) 0.0402(9) Uani 1 1 d . . . . .
H40 H 0.5380 0.3463 0.4184 0.048 Uiso 1 1 calc R U . . .
C41 C 0.4054(3) 0.1682(2) 0.4072(2) 0.0326(8) Uani 1 1 d . . . . .
C42 C 0.4751(4) 0.1523(3) 0.4633(2) 0.0400(9) Uani 1 1 d . . . . .
C43 C 0.5510(4) 0.1385(3) 0.5403(3) 0.0431(9) Uani 1 1 d . . . . .
C44 C 0.7676(4) 0.1398(4) 0.6117(3) 0.0788(14) Uani 1 1 d . . . . .
H44A H 0.7722 0.1990 0.6704 0.118 Uiso 1 1 calc R U . . .
H44B H 0.8611 0.1399 0.5973 0.118 Uiso 1 1 calc R U . . .
H44C H 0.7252 0.0749 0.6185 0.118 Uiso 1 1 calc R U . . .
N1 N 0.4847(3) -0.0436(2) 0.18998(18) 0.0358(7) Uani 1 1 d . . . . .
N2 N 0.1638(3) 0.17047(19) 0.37170(17) 0.0319(7) Uani 1 1 d . . . . .
N3 N 0.6149(5) 0.4302(3) 0.1109(3) 0.0813(12) Uani 1 1 d . . . . .
O1 O 0.1079(3) -0.09812(18) 0.04069(16) 0.0521(7) Uani 1 1 d . . . . .
O2 O 0.0598(3) -0.3126(2) 0.0376(2) 0.0764(9) Uani 1 1 d . . . . .
O3 O 0.2528(3) -0.3383(2) 0.1000(2) 0.0853(10) Uani 1 1 d . . . . .
O4 O 0.7278(4) 0.4441(3) 0.1578(3) 0.1137(13) Uani 1 1 d . . . . .
O5 O 0.5916(4) 0.4937(3) 0.0799(3) 0.1233(14) Uani 1 1 d . . . . .
O6 O 0.4954(3) 0.1217(3) 0.6022(2) 0.0821(10) Uani 1 1 d . . . . .
O7 O 0.6835(3) 0.1483(2) 0.53445(18) 0.0634(8) 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
C1 N1 1.470(4) . ?
C1 C2 1.523(4) . ?
C1 C31 1.534(4) . ?
C1 H1 0.9800 . ?
C2 C3 1.501(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.506(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.470(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N1 1.320(4) . ?
C5 C6 1.362(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.460(5) . ?
C6 C9 1.469(4) . ?
C7 O2 1.210(4) . ?
C7 O3 1.341(4) . ?
C8 O3 1.453(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 O1 1.217(3) . ?
C9 C10 1.527(4) . ?
C10 C32 1.330(4) . ?
C10 C11 1.467(4) . ?
C11 C12 1.398(4) . ?
C11 C17 1.412(4) . ?
C12 C13 1.379(5) . ?
C12 H12 0.9300 . ?
C13 C15 1.373(5) . ?
C13 C14 1.513(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.384(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.387(4) . ?
C16 H16 0.9300 . ?
C17 N2 1.398(4) . ?
C18 N2 1.465(4) . ?
C18 C19 1.505(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C24 1.371(5) . ?
C19 C20 1.372(5) . ?
C20 C21 1.376(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.360(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.353(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.391(5) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.374(5) . ?
C25 C30 1.378(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.368(5) . ?
C26 N3 1.467(5) . ?
C27 C28 1.367(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.387(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.380(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.529(4) . ?
C31 C32 1.513(4) . ?
C31 H31 0.9800 . ?
C32 C33 1.538(4) . ?
C33 N2 1.470(4) . ?
C33 C41 1.499(4) . ?
C33 C34 1.534(4) . ?
C34 C40 1.378(4) . ?
C34 C35 1.388(4) . ?
C35 C36 1.379(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.380(5) . ?
C36 H36 0.9300 . ?
C37 C39 1.372(5) . ?
C37 C38 1.522(5) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.381(5) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 C42 1.178(4) . ?
C42 C43 1.445(5) . ?
C43 O6 1.188(4) . ?
C43 O7 1.295(4) . ?
C44 O7 1.451(4) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
N3 O5 1.208(4) . ?
N3 O4 1.220(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 102.0(2) . . ?
N1 C1 C31 113.1(2) . . ?
C2 C1 C31 113.2(3) . . ?
N1 C1 H1 109.4 . . ?
C2 C1 H1 109.4 . . ?
C31 C1 H1 109.4 . . ?
C3 C2 C1 103.9(3) . . ?
C3 C2 H2A 111.0 . . ?
C1 C2 H2A 111.0 . . ?
C3 C2 H2B 111.0 . . ?
C1 C2 H2B 111.0 . . ?
H2A C2 H2B 109.0 . . ?
C2 C3 C4 106.3(3) . . ?
C2 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
C2 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
N1 C4 C3 104.3(3) . . ?
N1 C4 H4A 110.9 . . ?
C3 C4 H4A 110.9 . . ?
N1 C4 H4B 110.9 . . ?
C3 C4 H4B 110.9 . . ?
H4A C4 H4B 108.9 . . ?
N1 C5 C6 126.0(3) . . ?
N1 C5 H5 117.0 . . ?
C6 C5 H5 117.0 . . ?
C5 C6 C7 119.4(3) . . ?
C5 C6 C9 121.7(3) . . ?
C7 C6 C9 118.5(3) . . ?
O2 C7 O3 122.1(4) . . ?
O2 C7 C6 125.5(4) . . ?
O3 C7 C6 112.4(3) . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 C9 C6 125.6(3) . . ?
O1 C9 C10 119.1(3) . . ?
C6 C9 C10 114.6(3) . . ?
C32 C10 C11 121.2(3) . . ?
C32 C10 C9 125.7(3) . . ?
C11 C10 C9 113.0(3) . . ?
C12 C11 C17 118.3(3) . . ?
C12 C11 C10 122.5(3) . . ?
C17 C11 C10 119.2(3) . . ?
C13 C12 C11 123.1(3) . . ?
C13 C12 H12 118.4 . . ?
C11 C12 H12 118.4 . . ?
C15 C13 C12 117.5(3) . . ?
C15 C13 C14 121.6(3) . . ?
C12 C13 C14 120.9(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 C16 121.5(3) . . ?
C13 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C15 C16 C17 121.3(3) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 H16 119.3 . . ?
C16 C17 N2 122.1(3) . . ?
C16 C17 C11 118.3(3) . . ?
N2 C17 C11 119.5(3) . . ?
N2 C18 C19 115.9(3) . . ?
N2 C18 H18A 108.3 . . ?
C19 C18 H18A 108.3 . . ?
N2 C18 H18B 108.3 . . ?
C19 C18 H18B 108.3 . . ?
H18A C18 H18B 107.4 . . ?
C24 C19 C20 117.9(3) . . ?
C24 C19 C18 123.5(3) . . ?
C20 C19 C18 118.5(3) . . ?
C19 C20 C21 121.4(4) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C22 C21 C20 119.9(4) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C23 C22 C21 120.1(4) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 119.9(4) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C19 C24 C23 120.8(4) . . ?
C19 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C26 C25 C30 119.7(3) . . ?
C26 C25 H25 120.2 . . ?
C30 C25 H25 120.2 . . ?
C27 C26 C25 122.3(4) . . ?
C27 C26 N3 119.6(4) . . ?
C25 C26 N3 118.0(4) . . ?
C28 C27 C26 118.1(4) . . ?
C28 C27 H27 121.0 . . ?
C26 C27 H27 121.0 . . ?
C27 C28 C29 120.7(4) . . ?
C27 C28 H28 119.6 . . ?
C29 C28 H28 119.6 . . ?
C30 C29 C28 120.5(4) . . ?
C30 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C25 C30 C29 118.7(3) . . ?
C25 C30 C31 119.5(3) . . ?
C29 C30 C31 121.8(3) . . ?
C32 C31 C30 113.7(2) . . ?
C32 C31 C1 114.2(3) . . ?
C30 C31 C1 110.7(2) . . ?
C32 C31 H31 105.8 . . ?
C30 C31 H31 105.8 . . ?
C1 C31 H31 105.8 . . ?
C10 C32 C31 126.3(3) . . ?
C10 C32 C33 120.2(3) . . ?
C31 C32 C33 113.2(3) . . ?
N2 C33 C41 109.0(2) . . ?
N2 C33 C34 107.6(2) . . ?
C41 C33 C34 111.3(2) . . ?
N2 C33 C32 112.7(2) . . ?
C41 C33 C32 106.3(2) . . ?
C34 C33 C32 109.9(2) . . ?
C40 C34 C35 118.5(3) . . ?
C40 C34 C33 123.2(3) . . ?
C35 C34 C33 118.3(3) . . ?
C36 C35 C34 120.1(3) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C35 C36 C37 121.6(3) . . ?
C35 C36 H36 119.2 . . ?
C37 C36 H36 119.2 . . ?
C39 C37 C36 117.8(3) . . ?
C39 C37 C38 121.7(4) . . ?
C36 C37 C38 120.5(4) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 C40 121.5(4) . . ?
C37 C39 H39 119.3 . . ?
C40 C39 H39 119.3 . . ?
C34 C40 C39 120.5(3) . . ?
C34 C40 H40 119.7 . . ?
C39 C40 H40 119.7 . . ?
C42 C41 C33 173.3(4) . . ?
C41 C42 C43 173.3(4) . . ?
O6 C43 O7 124.9(3) . . ?
O6 C43 C42 122.4(4) . . ?
O7 C43 C42 112.7(3) . . ?
O7 C44 H44A 109.5 . . ?
O7 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O7 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C5 N1 C4 121.4(3) . . ?
C5 N1 C1 124.1(3) . . ?
C4 N1 C1 111.3(3) . . ?
C17 N2 C18 117.2(3) . . ?
C17 N2 C33 118.8(2) . . ?
C18 N2 C33 112.8(2) . . ?
O5 N3 O4 122.3(5) . . ?
O5 N3 C26 118.7(5) . . ?
O4 N3 C26 119.0(4) . . ?
C7 O3 C8 117.1(3) . . ?
C43 O7 C44 115.8(3) . . ?

_refine_diff_density_max         0.302
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.047



####################################################################### 
# 
# 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_1i
_database_code_depnum_ccdc_archive 'CCDC 1937763'
loop_
_audit_author_name
_audit_author_address
'Chao-Guo Yan' 'Yangzhou University'
_audit_update_record             
;
2019-07-02 deposited with the CCDC.	2019-09-02 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         'C33 H29 N3 O5'
_chemical_formula_sum            'C33 H29 N3 O5'
_chemical_formula_weight         547.59

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      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                   12.847(3)
_cell_length_b                   12.739(3)
_cell_length_c                   20.208(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.730(6)
_cell_angle_gamma                90
_cell_volume                     3284.5(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    6614
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      22.87

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_F_000             1152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.075
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.982
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29223
_diffrn_reflns_av_unetI/netI     0.0922
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.399
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6442
_reflns_number_gt                3432
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_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)+(0.1563P)²+0.9137P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6442
_refine_ls_number_parameters     373
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1512
_refine_ls_R_factor_gt           0.0833
_refine_ls_wR_factor_ref         0.2858
_refine_ls_wR_factor_gt          0.2481
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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 0.8047(3) 0.0578(3) -0.05744(18) 0.0498(9) Uani 1 1 d . . . . .
H1 H 0.8771 0.0547 -0.0361 0.060 Uiso 1 1 calc R U . . .
C2 C 0.8029(3) 0.0906(4) -0.1291(2) 0.0640(11) Uani 1 1 d . . . . .
H2A H 0.8644 0.0654 -0.1477 0.077 Uiso 1 1 calc R U . . .
H2B H 0.7992 0.1664 -0.1335 0.077 Uiso 1 1 calc R U . . .
C3 C 0.7023(4) 0.0383(4) -0.1633(2) 0.0767(13) Uani 1 1 d . . . . .
H3A H 0.6408 0.0791 -0.1564 0.092 Uiso 1 1 calc R U . . .
H3B H 0.7054 0.0308 -0.2108 0.092 Uiso 1 1 calc R U . . .
C4 C 0.6998(4) -0.0661(4) -0.1308(2) 0.0740(13) Uani 1 1 d . . . . .
H4A H 0.7337 -0.1188 -0.1555 0.089 Uiso 1 1 calc R U . . .
H4B H 0.6282 -0.0879 -0.1274 0.089 Uiso 1 1 calc R U . . .
C5 C 0.7927(3) -0.1291(3) -0.0244(2) 0.0551(10) Uani 1 1 d . . . . .
H5 H 0.7720 -0.1957 -0.0395 0.066 Uiso 1 1 calc R U . . .
C6 C 0.8548(3) -0.1240(3) 0.0354(2) 0.0519(10) Uani 1 1 d . . . . .
C7 C 0.9018(3) -0.2239(3) 0.0603(2) 0.0566(11) Uani 1 1 d . . . . .
C8 C 1.0080(4) -0.3099(3) 0.1471(3) 0.0830(14) Uani 1 1 d . . . . .
H8A H 0.9542 -0.3583 0.1562 0.125 Uiso 1 1 calc R U . . .
H8B H 1.0517 -0.2940 0.1877 0.125 Uiso 1 1 calc R U . . .
H8C H 1.0498 -0.3407 0.1158 0.125 Uiso 1 1 calc R U . . .
C9 C 0.8873(3) 0.2437(3) 0.04007(19) 0.0512(10) Uani 1 1 d . . . . .
H9 H 0.9186 0.1829 0.0585 0.061 Uiso 1 1 calc R U . . .
C10 C 0.9327(3) 0.3410(3) 0.0547(2) 0.0583(11) Uani 1 1 d . . . . .
C11 C 0.8909(4) 0.4331(3) 0.0289(3) 0.0728(14) Uani 1 1 d . . . . .
H11 H 0.9229 0.4972 0.0402 0.087 Uiso 1 1 calc R U . . .
C12 C 0.8005(4) 0.4278(3) -0.0139(3) 0.0801(15) Uani 1 1 d . . . . .
H12 H 0.7706 0.4890 -0.0326 0.096 Uiso 1 1 calc R U . . .
C13 C 0.7525(3) 0.3313(3) -0.0299(2) 0.0703(12) Uani 1 1 d . . . . .
H13 H 0.6912 0.3289 -0.0594 0.084 Uiso 1 1 calc R U . . .
C14 C 0.7952(3) 0.2384(3) -0.0022(2) 0.0523(10) Uani 1 1 d . . . . .
C15 C 0.7391(3) 0.1337(3) -0.01815(18) 0.0459(9) Uani 1 1 d . . . . .
H15 H 0.6758 0.1504 -0.0483 0.055 Uiso 1 1 calc R U . . .
C16 C 0.7018(3) 0.0894(2) 0.04400(17) 0.0403(8) Uani 1 1 d . . . . .
C17 C 0.6030(2) 0.1255(2) 0.06280(17) 0.0392(8) Uani 1 1 d . . . . .
C18 C 0.5301(2) 0.1932(2) 0.01771(17) 0.0384(8) Uani 1 1 d . . . . .
C19 C 0.4861(3) 0.1593(3) -0.04477(19) 0.0519(10) Uani 1 1 d . . . . .
H19 H 0.5021 0.0925 -0.0592 0.062 Uiso 1 1 calc R U . . .
C20 C 0.4196(3) 0.2220(3) -0.0858(2) 0.0577(10) Uani 1 1 d . . . . .
H20 H 0.3908 0.1961 -0.1270 0.069 Uiso 1 1 calc R U . . .
C21 C 0.3948(3) 0.3221(3) -0.0675(2) 0.0574(11) Uani 1 1 d . . . . .
C22 C 0.3226(4) 0.3932(4) -0.1133(3) 0.0859(15) Uani 1 1 d . . . . .
H22A H 0.3565 0.4116 -0.1516 0.129 Uiso 1 1 calc R U . . .
H22B H 0.3077 0.4558 -0.0897 0.129 Uiso 1 1 calc R U . . .
H22C H 0.2584 0.3568 -0.1274 0.129 Uiso 1 1 calc R U . . .
C23 C 0.4362(3) 0.3551(3) -0.0039(2) 0.0703(13) Uani 1 1 d . . . . .
H23 H 0.4184 0.4211 0.0110 0.084 Uiso 1 1 calc R U . . .
C24 C 0.5027(3) 0.2922(3) 0.0374(2) 0.0629(11) Uani 1 1 d . . . . .
H24 H 0.5296 0.3168 0.0793 0.075 Uiso 1 1 calc R U . . .
C25 C 0.8653(3) -0.0278(3) 0.0756(2) 0.0473(9) Uani 1 1 d . . . . .
C26 C 0.7610(3) 0.0231(2) 0.08857(18) 0.0410(8) Uani 1 1 d . . . . .
C27 C 0.7244(3) -0.0055(2) 0.14937(18) 0.0425(9) Uani 1 1 d . . . . .
C28 C 0.7782(3) -0.0765(3) 0.19722(19) 0.0511(10) Uani 1 1 d . . . . .
H28 H 0.8424 -0.1045 0.1892 0.061 Uiso 1 1 calc R U . . .
C29 C 0.7370(3) -0.1037(3) 0.25392(19) 0.0567(10) Uani 1 1 d . . . . .
C30 C 0.7926(4) -0.1825(4) 0.3019(2) 0.0886(15) Uani 1 1 d . . . . .
H30A H 0.7626 -0.2508 0.2932 0.133 Uiso 1 1 calc R U . . .
H30B H 0.7848 -0.1623 0.3468 0.133 Uiso 1 1 calc R U . . .
H30C H 0.8657 -0.1843 0.2962 0.133 Uiso 1 1 calc R U . . .
C31 C 0.6413(4) -0.0587(4) 0.2668(2) 0.0661(12) Uani 1 1 d . . . . .
H31 H 0.6135 -0.0761 0.3059 0.079 Uiso 1 1 calc R U . . .
C32 C 0.5880(3) 0.0103(3) 0.22281(19) 0.0583(10) Uani 1 1 d . . . . .
H32 H 0.5251 0.0392 0.2325 0.070 Uiso 1 1 calc R U . . .
C33 C 0.6274(3) 0.0373(3) 0.16379(17) 0.0426(8) Uani 1 1 d . . . . .
N1 N 0.7590(2) -0.0493(2) -0.06281(16) 0.0528(8) Uani 1 1 d . . . . .
N2 N 1.0295(3) 0.3453(3) 0.1009(2) 0.0755(11) Uani 1 1 d . . . . .
N3 N 0.5684(2) 0.1023(2) 0.11979(14) 0.0435(7) Uani 1 1 d . . . . .
O1 O 0.8877(2) -0.3080(2) 0.03193(15) 0.0728(9) Uani 1 1 d . . . . .
O2 O 0.9608(2) -0.21556(19) 0.11961(16) 0.0671(8) Uani 1 1 d . . . . .
O3 O 1.0714(3) 0.2624(3) 0.12034(19) 0.0944(11) Uani 1 1 d . . . . .
O4 O 1.0647(3) 0.4314(3) 0.1184(2) 0.1116(13) Uani 1 1 d . . . . .
O5 O 0.9467(2) 0.00608(19) 0.10629(15) 0.0621(8) 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
C1 N1 1.483(5) . ?
C1 C2 1.504(5) . ?
C1 C15 1.560(5) . ?
C1 H1 0.9800 . ?
C2 C3 1.544(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.485(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.506(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N1 1.321(5) . ?
C5 C6 1.369(6) . ?
C5 H5 0.9300 . ?
C6 C25 1.468(5) . ?
C6 C7 1.472(5) . ?
C7 O1 1.219(5) . ?
C7 O2 1.345(5) . ?
C8 O2 1.428(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C14 1.377(5) . ?
C9 C10 1.387(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.368(6) . ?
C10 N2 1.466(6) . ?
C11 C12 1.367(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.396(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.394(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.532(5) . ?
C15 C16 1.506(5) . ?
C15 H15 0.9800 . ?
C16 C26 1.394(5) . ?
C16 C17 1.441(4) . ?
C17 N3 1.316(4) . ?
C17 C18 1.501(5) . ?
C18 C24 1.380(5) . ?
C18 C19 1.390(5) . ?
C19 C20 1.374(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.376(6) . ?
C20 H20 0.9300 . ?
C21 C23 1.396(6) . ?
C21 C22 1.529(5) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.380(6) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O5 1.230(4) . ?
C25 C26 1.538(5) . ?
C26 C27 1.414(5) . ?
C27 C33 1.422(5) . ?
C27 C28 1.440(5) . ?
C28 C29 1.362(5) . ?
C28 H28 0.9300 . ?
C29 C31 1.408(6) . ?
C29 C30 1.516(6) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.375(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.392(5) . ?
C32 H32 0.9300 . ?
C33 N3 1.376(4) . ?
N2 O4 1.222(4) . ?
N2 O3 1.228(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 103.0(3) . . ?
N1 C1 C15 112.0(3) . . ?
C2 C1 C15 111.6(3) . . ?
N1 C1 H1 110.0 . . ?
C2 C1 H1 110.0 . . ?
C15 C1 H1 110.0 . . ?
C1 C2 C3 103.2(3) . . ?
C1 C2 H2A 111.1 . . ?
C3 C2 H2A 111.1 . . ?
C1 C2 H2B 111.1 . . ?
C3 C2 H2B 111.1 . . ?
H2A C2 H2B 109.1 . . ?
C4 C3 C2 104.4(4) . . ?
C4 C3 H3A 110.9 . . ?
C2 C3 H3A 110.9 . . ?
C4 C3 H3B 110.9 . . ?
C2 C3 H3B 110.9 . . ?
H3A C3 H3B 108.9 . . ?
C3 C4 N1 104.0(4) . . ?
C3 C4 H4A 111.0 . . ?
N1 C4 H4A 111.0 . . ?
C3 C4 H4B 111.0 . . ?
N1 C4 H4B 111.0 . . ?
H4A C4 H4B 109.0 . . ?
N1 C5 C6 126.9(4) . . ?
N1 C5 H5 116.6 . . ?
C6 C5 H5 116.6 . . ?
C5 C6 C25 122.3(3) . . ?
C5 C6 C7 115.8(4) . . ?
C25 C6 C7 121.7(4) . . ?
O1 C7 O2 121.7(4) . . ?
O1 C7 C6 124.5(4) . . ?
O2 C7 C6 113.7(4) . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C14 C9 C10 119.0(4) . . ?
C14 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C11 C10 C9 123.3(5) . . ?
C11 C10 N2 118.5(4) . . ?
C9 C10 N2 118.3(4) . . ?
C12 C11 C10 117.7(4) . . ?
C12 C11 H11 121.1 . . ?
C10 C11 H11 121.1 . . ?
C11 C12 C13 120.7(4) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C14 C13 C12 120.8(5) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C9 C14 C13 118.5(4) . . ?
C9 C14 C15 121.4(3) . . ?
C13 C14 C15 120.1(4) . . ?
C16 C15 C14 109.8(3) . . ?
C16 C15 C1 115.8(3) . . ?
C14 C15 C1 112.2(3) . . ?
C16 C15 H15 106.1 . . ?
C14 C15 H15 106.1 . . ?
C1 C15 H15 106.1 . . ?
C26 C16 C17 117.0(3) . . ?
C26 C16 C15 124.3(3) . . ?
C17 C16 C15 118.4(3) . . ?
N3 C17 C16 123.9(3) . . ?
N3 C17 C18 114.1(3) . . ?
C16 C17 C18 122.0(3) . . ?
C24 C18 C19 117.1(3) . . ?
C24 C18 C17 120.8(3) . . ?
C19 C18 C17 122.1(3) . . ?
C20 C19 C18 121.7(3) . . ?
C20 C19 H19 119.1 . . ?
C18 C19 H19 119.1 . . ?
C19 C20 C21 121.5(4) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C20 C21 C23 116.9(3) . . ?
C20 C21 C22 121.9(4) . . ?
C23 C21 C22 121.2(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C21 121.6(4) . . ?
C24 C23 H23 119.2 . . ?
C21 C23 H23 119.2 . . ?
C23 C24 C18 121.1(4) . . ?
C23 C24 H24 119.4 . . ?
C18 C24 H24 119.4 . . ?
O5 C25 C6 126.1(3) . . ?
O5 C25 C26 118.2(3) . . ?
C6 C25 C26 114.9(3) . . ?
C16 C26 C27 120.4(3) . . ?
C16 C26 C25 124.5(3) . . ?
C27 C26 C25 115.1(3) . . ?
C26 C27 C33 117.9(3) . . ?
C26 C27 C28 124.3(3) . . ?
C33 C27 C28 117.8(3) . . ?
C29 C28 C27 121.4(4) . . ?
C29 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
C28 C29 C31 119.1(4) . . ?
C28 C29 C30 120.4(4) . . ?
C31 C29 C30 120.5(4) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C29 121.3(4) . . ?
C32 C31 H31 119.3 . . ?
C29 C31 H31 119.3 . . ?
C31 C32 C33 120.6(4) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
N3 C33 C32 118.3(3) . . ?
N3 C33 C27 121.9(3) . . ?
C32 C33 C27 119.8(3) . . ?
C5 N1 C1 124.4(3) . . ?
C5 N1 C4 121.5(3) . . ?
C1 N1 C4 110.5(3) . . ?
O4 N2 O3 123.1(5) . . ?
O4 N2 C10 118.3(4) . . ?
O3 N2 C10 118.6(4) . . ?
C17 N3 C33 118.9(3) . . ?
C7 O2 C8 116.7(3) . . ?

_refine_diff_density_max         0.304
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.067



####################################################################### 
# 
# 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_3f
_database_code_depnum_ccdc_archive 'CCDC 1937765'
loop_
_audit_author_name
_audit_author_address
'Chao-Guo Yan' 'Yangzhou University'
_audit_update_record             
;
2019-07-02 deposited with the CCDC.	2019-09-02 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         'C34 H28 Cl2 N2 O3'
_chemical_formula_sum            'C34 H28 Cl2 N2 O3'
_chemical_formula_weight         583.48

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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   10.1992(10)
_cell_length_b                   17.1094(19)
_cell_length_c                   33.448(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5836.8(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    4347
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      20.74

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_F_000             2432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.261
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48740
_diffrn_reflns_av_unetI/netI     0.1106
_diffrn_reflns_av_R_equivalents  0.1926
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.381
_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_full        24.711
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4957
_reflns_number_gt                2619
_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)+(0.0477P)²+5.8331P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4957
_refine_ls_number_parameters     372
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1643
_refine_ls_R_factor_gt           0.0727
_refine_ls_wR_factor_ref         0.1624
_refine_ls_wR_factor_gt          0.1324
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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 0.2243(4) 0.3044(3) 0.10230(13) 0.0462(12) Uani 1 1 d . . . . .
H1A H 0.2366 0.3589 0.0953 0.055 Uiso 1 1 calc R U . . .
H1B H 0.2030 0.3009 0.1305 0.055 Uiso 1 1 calc R U . . .
C2 C 0.1170(4) 0.2674(3) 0.07686(15) 0.0595(14) Uani 1 1 d . . . . .
H2A H 0.0656 0.3073 0.0634 0.071 Uiso 1 1 calc R U . . .
H2B H 0.0590 0.2359 0.0932 0.071 Uiso 1 1 calc R U . . .
C3 C 0.1893(4) 0.2165(3) 0.04648(13) 0.0501(13) Uani 1 1 d . . . . .
H3A H 0.1353 0.1728 0.0381 0.060 Uiso 1 1 calc R U . . .
H3B H 0.2138 0.2467 0.0231 0.060 Uiso 1 1 calc R U . . .
C4 C 0.3105(4) 0.1882(2) 0.06894(11) 0.0342(10) Uani 1 1 d . . . . .
H4 H 0.3814 0.1776 0.0499 0.041 Uiso 1 1 calc R U . . .
C5 C 0.4617(4) 0.2892(2) 0.09367(11) 0.0368(11) Uani 1 1 d . . . . .
H5 H 0.4684 0.3415 0.1010 0.044 Uiso 1 1 calc R U . . .
C6 C 0.5761(4) 0.2505(2) 0.08463(11) 0.0356(10) Uani 1 1 d . . . . .
C7 C 0.6958(4) 0.2933(3) 0.07564(14) 0.0513(13) Uani 1 1 d . . . . .
C8 C 0.7919(5) 0.4186(3) 0.0683(2) 0.106(2) Uani 1 1 d . . . . .
H8A H 0.8515 0.4106 0.0901 0.160 Uiso 1 1 calc R U . . .
H8B H 0.7671 0.4727 0.0672 0.160 Uiso 1 1 calc R U . . .
H8C H 0.8337 0.4041 0.0436 0.160 Uiso 1 1 calc R U . . .
C9 C 0.1297(4) 0.0185(3) 0.05981(12) 0.0398(11) Uani 1 1 d . . . . .
C10 C 0.1082(4) -0.0429(3) 0.03356(12) 0.0439(12) Uani 1 1 d . . . . .
H10 H 0.0233 -0.0607 0.0291 0.053 Uiso 1 1 calc R U . . .
C11 C 0.2120(4) -0.0776(3) 0.01410(12) 0.0454(12) Uani 1 1 d . . . . .
H11 H 0.1975 -0.1178 -0.0041 0.054 Uiso 1 1 calc R U . . .
C12 C 0.3383(4) -0.0521(3) 0.02187(12) 0.0455(12) Uani 1 1 d . . . . .
H12 H 0.4090 -0.0754 0.0090 0.055 Uiso 1 1 calc R U . . .
C13 C 0.3597(4) 0.0079(2) 0.04872(11) 0.0386(11) Uani 1 1 d . . . . .
H13 H 0.4452 0.0236 0.0540 0.046 Uiso 1 1 calc R U . . .
C14 C 0.2570(4) 0.0455(2) 0.06799(11) 0.0338(10) Uani 1 1 d . . . . .
C15 C 0.2857(4) 0.1155(2) 0.09493(11) 0.0322(10) Uani 1 1 d . . . . .
H15 H 0.2057 0.1256 0.1103 0.039 Uiso 1 1 calc R U . . .
C16 C 0.3940(4) 0.0976(2) 0.12516(11) 0.0302(10) Uani 1 1 d . . . . .
C17 C 0.3619(4) 0.0500(2) 0.15932(12) 0.0376(10) Uani 1 1 d . . . . .
C18 C 0.2349(4) 0.0090(3) 0.16175(12) 0.0442(11) Uani 1 1 d . . . . .
H18 H 0.1655 0.0279 0.1465 0.053 Uiso 1 1 calc R U . . .
C19 C 0.2141(5) -0.0539(3) 0.18466(12) 0.0506(13) Uani 1 1 d . . . . .
H19 H 0.2838 -0.0722 0.2000 0.061 Uiso 1 1 calc R U . . .
C20 C 0.0892(5) -0.0959(3) 0.18728(13) 0.0530(13) Uani 1 1 d . . . . .
C21 C 0.0785(6) -0.1726(3) 0.19967(13) 0.0642(15) Uani 1 1 d . . . . .
C22 C -0.0399(8) -0.2114(4) 0.20175(16) 0.088(2) Uani 1 1 d . . . . .
H22 H -0.0432 -0.2633 0.2100 0.105 Uiso 1 1 calc R U . . .
C23 C -0.1532(8) -0.1725(5) 0.1915(2) 0.099(2) Uani 1 1 d . . . . .
H23 H -0.2338 -0.1977 0.1930 0.119 Uiso 1 1 calc R U . . .
C24 C -0.1465(6) -0.0981(4) 0.17935(19) 0.0865(19) Uani 1 1 d . . . . .
H24 H -0.2230 -0.0719 0.1723 0.104 Uiso 1 1 calc R U . . .
C25 C -0.0287(5) -0.0599(3) 0.17710(16) 0.0729(16) Uani 1 1 d . . . . .
H25 H -0.0273 -0.0082 0.1685 0.087 Uiso 1 1 calc R U . . .
C26 C 0.5826(4) 0.1651(3) 0.08642(12) 0.0344(10) Uani 1 1 d . . . . .
C27 C 0.5206(4) 0.1242(2) 0.12226(11) 0.0301(10) Uani 1 1 d . . . . .
C28 C 0.6112(4) 0.1105(2) 0.15422(11) 0.0323(10) Uani 1 1 d . . . . .
C29 C 0.7410(4) 0.1400(2) 0.15489(12) 0.0392(11) Uani 1 1 d . . . . .
H29 H 0.7735 0.1655 0.1324 0.047 Uiso 1 1 calc R U . . .
C30 C 0.8204(4) 0.1319(3) 0.18810(14) 0.0477(12) Uani 1 1 d . . . . .
C31 C 0.9549(4) 0.1689(3) 0.18966(14) 0.0611(14) Uani 1 1 d . . . . .
H31A H 1.0185 0.1302 0.1970 0.092 Uiso 1 1 calc R U . . .
H31B H 0.9551 0.2102 0.2091 0.092 Uiso 1 1 calc R U . . .
H31C H 0.9764 0.1899 0.1639 0.092 Uiso 1 1 calc R U . . .
C32 C 0.7711(5) 0.0901(3) 0.22116(13) 0.0552(13) Uani 1 1 d . . . . .
H32 H 0.8238 0.0838 0.2436 0.066 Uiso 1 1 calc R U . . .
C33 C 0.6497(5) 0.0588(3) 0.22113(12) 0.0514(12) Uani 1 1 d . . . . .
H33 H 0.6208 0.0308 0.2433 0.062 Uiso 1 1 calc R U . . .
C34 C 0.5659(4) 0.0682(2) 0.18781(12) 0.0388(11) Uani 1 1 d . . . . .
Cl1 Cl -0.00723(10) 0.06124(8) 0.08194(4) 0.0593(4) Uani 1 1 d . . . . .
Cl2 Cl 0.21886(19) -0.22637(9) 0.21209(5) 0.1066(6) Uani 1 1 d . . . . .
N1 N 0.3428(3) 0.25806(19) 0.09282(9) 0.0341(8) Uani 1 1 d . . . . .
N2 N 0.4436(4) 0.0363(2) 0.18927(10) 0.0428(9) Uani 1 1 d . . . . .
O1 O 0.8021(3) 0.2651(2) 0.07047(13) 0.0875(13) Uani 1 1 d . . . . .
O2 O 0.6765(3) 0.3710(2) 0.07411(11) 0.0697(10) Uani 1 1 d . . . . .
O3 O 0.6476(3) 0.12469(18) 0.06404(8) 0.0481(8) 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
C1 N1 1.480(5) . ?
C1 C2 1.524(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.528(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.525(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.474(5) . ?
C4 C15 1.540(5) . ?
C4 H4 0.9800 . ?
C5 N1 1.325(4) . ?
C5 C6 1.376(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.455(6) . ?
C6 C26 1.463(6) . ?
C7 O1 1.199(5) . ?
C7 O2 1.345(5) . ?
C8 O2 1.444(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.387(5) . ?
C9 C14 1.405(5) . ?
C9 Cl1 1.741(4) . ?
C10 C11 1.378(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.385(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.381(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.387(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.527(5) . ?
C15 C16 1.528(5) . ?
C15 H15 0.9800 . ?
C16 C27 1.373(5) . ?
C16 C17 1.441(5) . ?
C17 N2 1.324(5) . ?
C17 C18 1.475(6) . ?
C18 C19 1.337(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.466(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.380(6) . ?
C20 C25 1.393(7) . ?
C21 C22 1.380(7) . ?
C21 Cl2 1.752(6) . ?
C22 C23 1.377(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.337(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.370(7) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 O3 1.216(4) . ?
C26 C27 1.525(5) . ?
C27 C28 1.432(5) . ?
C28 C34 1.414(5) . ?
C28 C29 1.418(5) . ?
C29 C30 1.382(5) . ?
C29 H29 0.9300 . ?
C30 C32 1.410(6) . ?
C30 C31 1.512(6) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.349(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.414(5) . ?
C33 H33 0.9300 . ?
C34 N2 1.362(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 104.1(3) . . ?
N1 C1 H1A 110.9 . . ?
C2 C1 H1A 110.9 . . ?
N1 C1 H1B 110.9 . . ?
C2 C1 H1B 110.9 . . ?
H1A C1 H1B 109.0 . . ?
C1 C2 C3 105.2(3) . . ?
C1 C2 H2A 110.7 . . ?
C3 C2 H2A 110.7 . . ?
C1 C2 H2B 110.7 . . ?
C3 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
C4 C3 C2 104.1(3) . . ?
C4 C3 H3A 110.9 . . ?
C2 C3 H3A 110.9 . . ?
C4 C3 H3B 110.9 . . ?
C2 C3 H3B 110.9 . . ?
H3A C3 H3B 108.9 . . ?
N1 C4 C3 101.0(3) . . ?
N1 C4 C15 112.7(3) . . ?
C3 C4 C15 113.7(3) . . ?
N1 C4 H4 109.7 . . ?
C3 C4 H4 109.7 . . ?
C15 C4 H4 109.7 . . ?
N1 C5 C6 125.3(4) . . ?
N1 C5 H5 117.4 . . ?
C6 C5 H5 117.4 . . ?
C5 C6 C7 120.9(4) . . ?
C5 C6 C26 120.7(4) . . ?
C7 C6 C26 118.3(4) . . ?
O1 C7 O2 121.6(4) . . ?
O1 C7 C6 125.8(5) . . ?
O2 C7 C6 112.5(4) . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C14 121.2(4) . . ?
C10 C9 Cl1 117.4(3) . . ?
C14 C9 Cl1 121.4(3) . . ?
C11 C10 C9 120.3(4) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 119.4(4) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 120.2(4) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 121.8(4) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C13 C14 C9 117.1(4) . . ?
C13 C14 C15 119.5(3) . . ?
C9 C14 C15 123.3(4) . . ?
C14 C15 C16 111.9(3) . . ?
C14 C15 C4 109.4(3) . . ?
C16 C15 C4 114.6(3) . . ?
C14 C15 H15 106.8 . . ?
C16 C15 H15 106.8 . . ?
C4 C15 H15 106.8 . . ?
C27 C16 C17 117.2(3) . . ?
C27 C16 C15 124.5(3) . . ?
C17 C16 C15 118.3(3) . . ?
N2 C17 C16 123.8(4) . . ?
N2 C17 C18 115.3(4) . . ?
C16 C17 C18 120.8(4) . . ?
C19 C18 C17 123.6(4) . . ?
C19 C18 H18 118.2 . . ?
C17 C18 H18 118.2 . . ?
C18 C19 C20 124.5(5) . . ?
C18 C19 H19 117.8 . . ?
C20 C19 H19 117.8 . . ?
C21 C20 C25 115.2(5) . . ?
C21 C20 C19 123.6(5) . . ?
C25 C20 C19 121.2(5) . . ?
C20 C21 C22 122.8(6) . . ?
C20 C21 Cl2 120.4(4) . . ?
C22 C21 Cl2 116.7(5) . . ?
C23 C22 C21 119.2(6) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C24 C23 C22 119.6(7) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 121.0(7) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C24 C25 C20 122.2(6) . . ?
C24 C25 H25 118.9 . . ?
C20 C25 H25 118.9 . . ?
O3 C26 C6 124.6(4) . . ?
O3 C26 C27 116.7(4) . . ?
C6 C26 C27 118.1(3) . . ?
C16 C27 C28 120.0(3) . . ?
C16 C27 C26 126.7(3) . . ?
C28 C27 C26 113.3(3) . . ?
C34 C28 C29 118.4(4) . . ?
C34 C28 C27 117.8(4) . . ?
C29 C28 C27 123.7(4) . . ?
C30 C29 C28 121.6(4) . . ?
C30 C29 H29 119.2 . . ?
C28 C29 H29 119.2 . . ?
C29 C30 C32 118.2(4) . . ?
C29 C30 C31 121.2(4) . . ?
C32 C30 C31 120.6(4) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C30 121.9(4) . . ?
C33 C32 H32 119.1 . . ?
C30 C32 H32 119.1 . . ?
C32 C33 C34 120.7(4) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
N2 C34 C33 118.7(4) . . ?
N2 C34 C28 122.2(4) . . ?
C33 C34 C28 119.1(4) . . ?
C5 N1 C4 122.8(3) . . ?
C5 N1 C1 121.8(3) . . ?
C4 N1 C1 111.6(3) . . ?
C17 N2 C34 118.6(3) . . ?
C7 O2 C8 116.3(4) . . ?

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
N1 C1 C2 C3 -14.6(4) . . . . ?
C1 C2 C3 C4 32.5(4) . . . . ?
C2 C3 C4 N1 -36.9(4) . . . . ?
C2 C3 C4 C15 84.0(4) . . . . ?
N1 C5 C6 C7 162.8(4) . . . . ?
N1 C5 C6 C26 -21.3(6) . . . . ?
C5 C6 C7 O1 173.9(5) . . . . ?
C26 C6 C7 O1 -2.1(7) . . . . ?
C5 C6 C7 O2 -5.2(6) . . . . ?
C26 C6 C7 O2 178.8(4) . . . . ?
C14 C9 C10 C11 -1.6(6) . . . . ?
Cl1 C9 C10 C11 178.0(3) . . . . ?
C9 C10 C11 C12 1.8(6) . . . . ?
C10 C11 C12 C13 -0.3(6) . . . . ?
C11 C12 C13 C14 -1.4(6) . . . . ?
C12 C13 C14 C9 1.5(6) . . . . ?
C12 C13 C14 C15 -175.4(4) . . . . ?
C10 C9 C14 C13 0.0(6) . . . . ?
Cl1 C9 C14 C13 -179.6(3) . . . . ?
C10 C9 C14 C15 176.7(4) . . . . ?
Cl1 C9 C14 C15 -2.9(5) . . . . ?
C13 C14 C15 C16 -50.5(5) . . . . ?
C9 C14 C15 C16 132.8(4) . . . . ?
C13 C14 C15 C4 77.6(4) . . . . ?
C9 C14 C15 C4 -99.1(4) . . . . ?
N1 C4 C15 C14 -178.3(3) . . . . ?
C3 C4 C15 C14 67.5(4) . . . . ?
N1 C4 C15 C16 -51.8(4) . . . . ?
C3 C4 C15 C16 -166.0(3) . . . . ?
C14 C15 C16 C27 104.2(4) . . . . ?
C4 C15 C16 C27 -21.1(5) . . . . ?
C14 C15 C16 C17 -76.2(4) . . . . ?
C4 C15 C16 C17 158.5(3) . . . . ?
C27 C16 C17 N2 5.9(6) . . . . ?
C15 C16 C17 N2 -173.7(4) . . . . ?
C27 C16 C17 C18 -170.5(4) . . . . ?
C15 C16 C17 C18 9.8(5) . . . . ?
N2 C17 C18 C19 -19.1(6) . . . . ?
C16 C17 C18 C19 157.6(4) . . . . ?
C17 C18 C19 C20 -179.5(4) . . . . ?
C18 C19 C20 C21 157.8(4) . . . . ?
C18 C19 C20 C25 -22.1(7) . . . . ?
C25 C20 C21 C22 0.3(7) . . . . ?
C19 C20 C21 C22 -179.6(4) . . . . ?
C25 C20 C21 Cl2 178.2(4) . . . . ?
C19 C20 C21 Cl2 -1.7(6) . . . . ?
C20 C21 C22 C23 -0.7(8) . . . . ?
Cl2 C21 C22 C23 -178.6(5) . . . . ?
C21 C22 C23 C24 0.7(9) . . . . ?
C22 C23 C24 C25 -0.3(10) . . . . ?
C23 C24 C25 C20 -0.1(9) . . . . ?
C21 C20 C25 C24 0.1(7) . . . . ?
C19 C20 C25 C24 -180.0(5) . . . . ?
C5 C6 C26 O3 145.4(4) . . . . ?
C7 C6 C26 O3 -38.6(6) . . . . ?
C5 C6 C26 C27 -44.2(5) . . . . ?
C7 C6 C26 C27 131.8(4) . . . . ?
C17 C16 C27 C28 -5.8(5) . . . . ?
C15 C16 C27 C28 173.9(3) . . . . ?
C17 C16 C27 C26 170.6(4) . . . . ?
C15 C16 C27 C26 -9.8(6) . . . . ?
O3 C26 C27 C16 -98.0(5) . . . . ?
C6 C26 C27 C16 90.8(5) . . . . ?
O3 C26 C27 C28 78.5(4) . . . . ?
C6 C26 C27 C28 -92.6(4) . . . . ?
C16 C27 C28 C34 1.0(5) . . . . ?
C26 C27 C28 C34 -175.8(3) . . . . ?
C16 C27 C28 C29 -175.8(4) . . . . ?
C26 C27 C28 C29 7.3(5) . . . . ?
C34 C28 C29 C30 -3.5(6) . . . . ?
C27 C28 C29 C30 173.4(4) . . . . ?
C28 C29 C30 C32 2.8(6) . . . . ?
C28 C29 C30 C31 -175.3(4) . . . . ?
C29 C30 C32 C33 -0.5(7) . . . . ?
C31 C30 C32 C33 177.6(4) . . . . ?
C30 C32 C33 C34 -1.1(7) . . . . ?
C32 C33 C34 N2 -179.3(4) . . . . ?
C32 C33 C34 C28 0.4(6) . . . . ?
C29 C28 C34 N2 -178.5(4) . . . . ?
C27 C28 C34 N2 4.5(6) . . . . ?
C29 C28 C34 C33 1.8(6) . . . . ?
C27 C28 C34 C33 -175.2(4) . . . . ?
C6 C5 N1 C4 -22.6(6) . . . . ?
C6 C5 N1 C1 -178.9(4) . . . . ?
C3 C4 N1 C5 -129.2(4) . . . . ?
C15 C4 N1 C5 109.1(4) . . . . ?
C3 C4 N1 C1 29.3(4) . . . . ?
C15 C4 N1 C1 -92.4(4) . . . . ?
C2 C1 N1 C5 149.2(4) . . . . ?
C2 C1 N1 C4 -9.5(4) . . . . ?
C16 C17 N2 C34 -0.7(6) . . . . ?
C18 C17 N2 C34 175.9(4) . . . . ?
C33 C34 N2 C17 175.1(4) . . . . ?
C28 C34 N2 C17 -4.6(6) . . . . ?
O1 C7 O2 C8 -3.5(7) . . . . ?
C6 C7 O2 C8 175.6(4) . . . . ?

_refine_diff_density_max         0.248
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.052





#===================================================================================
