# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_190325lyz_1_0m
_database_code_depnum_ccdc_archive 'CCDC 1960287'
loop_
_audit_author_name
_audit_author_address
'Yuezhou Liu'
;Zhejiang University
China
;
_audit_update_record             
;
2019-10-19 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_audit_creation_date             2019-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C H Cl3, C42 H38 N4 O6'
_chemical_formula_sum            'C43 H39 Cl3 N4 O6'
_chemical_formula_weight         814.13
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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 0.3281 0.5435 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.4017(2)
_cell_length_b                   11.9309(3)
_cell_length_c                   16.8327(4)
_cell_angle_alpha                95.0320(10)
_cell_angle_beta                 92.8350(10)
_cell_angle_gamma                92.8780(10)
_cell_volume                     1875.73(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.950
_cell_measurement_theta_min      4.597
_shelx_estimated_absorpt_T_max   0.871
_shelx_estimated_absorpt_T_min   0.777
_exptl_absorpt_coefficient_mu    1.770
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1223 before and 0.0626 after correction. The Ratio of minimum to maximum transmission is 0.6224. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22375
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.936
_diffrn_reflns_theta_min         4.595
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6452
_reflns_number_total             7014
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.531
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         7014
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0645
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0644P)²+2.9669P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1648
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C15(H15A,H15B), C25(H25A,H25B), C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C35(H35),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C28(H28A,H28B,
 H28C), C32(H32A,H32B,H32C), C43(H43A,H43B,H43C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.89725(9) 0.63788(9) 0.29654(7) 0.0680(3) Uani 1 1 d . . . . .
Cl2 Cl 0.60567(9) 0.69919(7) 0.27828(5) 0.0500(2) Uani 1 1 d . . . . .
Cl3 Cl 0.66942(17) 0.50615(15) 0.36132(12) 0.1226(7) Uani 1 1 d . . . . .
C1 C 0.7210(5) 0.6000(5) 0.3025(5) 0.131(3) Uani 1 1 d . . . . .
H1 H 0.708574 0.550721 0.251141 0.157 Uiso 1 1 calc R . . . .
O1 O 0.66315(18) 0.99434(15) 0.16395(11) 0.0306(4) Uani 1 1 d . . . . .
O2 O 0.1909(2) 0.74119(15) 0.26221(11) 0.0334(4) Uani 1 1 d . . . . .
O3 O 0.79781(19) 1.02865(16) 0.37489(12) 0.0353(4) Uani 1 1 d . . . . .
O4 O 0.32298(19) 0.78985(16) 0.47079(11) 0.0331(4) Uani 1 1 d . . . . .
O5 O 0.29026(17) 0.50541(14) 0.12134(10) 0.0273(4) Uani 1 1 d . . . . .
O6 O 0.74761(17) 0.76807(14) 0.02951(11) 0.0289(4) Uani 1 1 d . . . . .
N1 N 0.4374(2) 0.94679(16) 0.10758(12) 0.0244(4) Uani 1 1 d . . . . .
N2 N 0.2400(2) 0.83294(17) 0.15116(12) 0.0250(4) Uani 1 1 d . . . . .
N3 N 0.2518(2) 0.93166(17) 0.26998(12) 0.0258(4) Uani 1 1 d . . . . .
N4 N 0.4602(2) 1.03548(17) 0.22962(12) 0.0264(4) Uani 1 1 d . . . . .
C2 C 0.5334(2) 0.99078(19) 0.16763(15) 0.0242(5) Uani 1 1 d . . . . .
C3 C 0.2910(2) 0.9445(2) 0.13285(15) 0.0245(5) Uani 1 1 d . . . . .
C4 C 0.2260(2) 0.8261(2) 0.23130(15) 0.0250(5) Uani 1 1 d . . . . .
C5 C 0.3063(3) 1.0128(2) 0.21765(15) 0.0262(5) Uani 1 1 d . . . . .
C6 C 0.5297(3) 1.0759(2) 0.30658(16) 0.0297(5) Uani 1 1 d . . . . .
H6A H 0.473637 1.136151 0.331753 0.036 Uiso 1 1 calc R . . . .
H6B H 0.625262 1.109799 0.297716 0.036 Uiso 1 1 calc R . . . .
C7 C 0.5465(3) 0.9857(2) 0.36392(14) 0.0262(5) Uani 1 1 d . . . . .
C8 C 0.6797(3) 0.9654(2) 0.39424(15) 0.0283(5) Uani 1 1 d . . . . .
C9 C 0.8832(3) 0.9738(3) 0.31635(18) 0.0428(7) Uani 1 1 d . . . . .
H9A H 0.831006 0.966542 0.264136 0.064 Uiso 1 1 calc GR . . . .
H9B H 0.904171 0.898742 0.331706 0.064 Uiso 1 1 calc GR . . . .
H9C H 0.972675 1.018588 0.313250 0.064 Uiso 1 1 calc GR . . . .
C10 C 0.7008(3) 0.8837(2) 0.45012(15) 0.0278(5) Uani 1 1 d . . . . .
C11 C 0.5787(3) 0.8216(2) 0.47479(15) 0.0274(5) Uani 1 1 d . . . . .
C12 C 0.4402(3) 0.8448(2) 0.44202(15) 0.0271(5) Uani 1 1 d . . . . .
C13 C 0.2921(3) 0.6757(2) 0.43613(18) 0.0392(6) Uani 1 1 d . . . . .
H13A H 0.252761 0.676711 0.381203 0.059 Uiso 1 1 calc GR . . . .
H13B H 0.222508 0.637926 0.467704 0.059 Uiso 1 1 calc GR . . . .
H13C H 0.380056 0.634970 0.435958 0.059 Uiso 1 1 calc GR . . . .
C14 C 0.4233(3) 0.9231(2) 0.38853(14) 0.0256(5) Uani 1 1 d . . . . .
C15 C 0.2751(3) 0.9475(2) 0.35693(15) 0.0288(5) Uani 1 1 d . . . . .
H15A H 0.204668 0.898046 0.380940 0.035 Uiso 1 1 calc R . . . .
H15B H 0.256519 1.026417 0.374996 0.035 Uiso 1 1 calc R . . . .
C16 C 0.5983(3) 0.7414(2) 0.52899(15) 0.0304(5) Uani 1 1 d . . . . .
H16 H 0.517229 0.701962 0.546662 0.037 Uiso 1 1 calc R . . . .
C17 C 0.7347(3) 0.7174(2) 0.55822(15) 0.0323(6) Uani 1 1 d . . . . .
C18 C 0.8564(3) 0.7812(2) 0.53468(16) 0.0324(6) Uani 1 1 d . . . . .
C19 C 0.8361(3) 0.8637(2) 0.48238(16) 0.0310(5) Uani 1 1 d . . . . .
H19 H 0.916462 0.907622 0.468164 0.037 Uiso 1 1 calc R . . . .
C20 C 0.9950(3) 0.7579(3) 0.56587(18) 0.0412(7) Uani 1 1 d . . . . .
H20 H 1.076466 0.800762 0.551911 0.049 Uiso 1 1 calc R . . . .
C21 C 1.0108(4) 0.6753(3) 0.6150(2) 0.0514(8) Uani 1 1 d . . . . .
H21 H 1.103512 0.660748 0.635388 0.062 Uiso 1 1 calc R . . . .
C22 C 0.8915(4) 0.6101(3) 0.6366(2) 0.0508(8) Uani 1 1 d . . . . .
H22 H 0.905073 0.551222 0.670264 0.061 Uiso 1 1 calc R . . . .
C23 C 0.7571(3) 0.6309(3) 0.60970(18) 0.0412(7) Uani 1 1 d . . . . .
H23 H 0.677729 0.587315 0.625474 0.049 Uiso 1 1 calc R . . . .
C24 C 0.2292(3) 1.1220(2) 0.22635(18) 0.0372(6) Uani 1 1 d . . . . .
H24A H 0.126991 1.105932 0.213610 0.056 Uiso 1 1 calc GR . . . .
H24B H 0.267143 1.174013 0.189658 0.056 Uiso 1 1 calc GR . . . .
H24C H 0.243918 1.156388 0.281376 0.056 Uiso 1 1 calc GR . . . .
C25 C 0.2414(2) 0.7328(2) 0.09496(15) 0.0247(5) Uani 1 1 d . . . . .
H25A H 0.207878 0.752211 0.041449 0.030 Uiso 1 1 calc R . . . .
H25B H 0.172943 0.674539 0.111431 0.030 Uiso 1 1 calc R . . . .
C26 C 0.3861(2) 0.68344(19) 0.08872(13) 0.0220(5) Uani 1 1 d . . . . .
C27 C 0.4047(2) 0.5746(2) 0.10414(14) 0.0226(5) Uani 1 1 d . . . . .
C28 C 0.2806(3) 0.4890(2) 0.20441(16) 0.0350(6) Uani 1 1 d . . . . .
H28A H 0.212038 0.425870 0.210077 0.052 Uiso 1 1 calc GR . . . .
H28B H 0.248590 0.557557 0.232905 0.052 Uiso 1 1 calc GR . . . .
H28C H 0.374396 0.472194 0.226961 0.052 Uiso 1 1 calc GR . . . .
C29 C 0.5410(2) 0.52559(19) 0.09946(13) 0.0224(5) Uani 1 1 d . . . . .
C30 C 0.6594(2) 0.59464(19) 0.07684(13) 0.0220(5) Uani 1 1 d . . . . .
C31 C 0.6355(2) 0.70717(19) 0.05867(14) 0.0227(5) Uani 1 1 d . . . . .
C32 C 0.8571(3) 0.8127(2) 0.08834(19) 0.0356(6) Uani 1 1 d . . . . .
H32A H 0.949831 0.813111 0.064187 0.053 Uiso 1 1 calc GR . . . .
H32B H 0.859211 0.765484 0.133146 0.053 Uiso 1 1 calc GR . . . .
H32C H 0.836736 0.889778 0.107706 0.053 Uiso 1 1 calc GR . . . .
C33 C 0.5048(2) 0.75169(19) 0.06421(13) 0.0218(5) Uani 1 1 d . . . . .
C34 C 0.4826(2) 0.87031(19) 0.04242(14) 0.0241(5) Uani 1 1 d . . . . .
H34A H 0.572927 0.901833 0.023484 0.029 Uiso 1 1 calc R . . . .
H34B H 0.409907 0.866720 -0.002464 0.029 Uiso 1 1 calc R . . . .
C35 C 0.7927(2) 0.5488(2) 0.07265(14) 0.0241(5) Uani 1 1 d . . . . .
H35 H 0.870537 0.593272 0.056017 0.029 Uiso 1 1 calc R . . . .
C36 C 0.8152(2) 0.4398(2) 0.09212(14) 0.0247(5) Uani 1 1 d . . . . .
C37 C 0.6971(3) 0.3712(2) 0.11483(14) 0.0251(5) Uani 1 1 d . . . . .
C38 C 0.5622(3) 0.4154(2) 0.11621(14) 0.0251(5) Uani 1 1 d . . . . .
H38 H 0.483024 0.368967 0.128926 0.030 Uiso 1 1 calc R . . . .
C39 C 0.7220(3) 0.2601(2) 0.13503(16) 0.0312(5) Uani 1 1 d . . . . .
H39 H 0.644865 0.213809 0.150483 0.037 Uiso 1 1 calc R . . . .
C40 C 0.8548(3) 0.2191(2) 0.13256(17) 0.0351(6) Uani 1 1 d . . . . .
H40 H 0.869319 0.144883 0.146343 0.042 Uiso 1 1 calc R . . . .
C41 C 0.9713(3) 0.2871(2) 0.10945(17) 0.0347(6) Uani 1 1 d . . . . .
H41 H 1.063149 0.257584 0.107277 0.042 Uiso 1 1 calc R . . . .
C42 C 0.9527(3) 0.3941(2) 0.09039(15) 0.0295(5) Uani 1 1 d . . . . .
H42 H 1.031959 0.438813 0.075766 0.035 Uiso 1 1 calc R . . . .
C43 C 0.1921(3) 0.9915(2) 0.07119(16) 0.0309(5) Uani 1 1 d . . . . .
H43A H 0.191221 0.943893 0.020635 0.046 Uiso 1 1 calc GR . . . .
H43B H 0.226037 1.068360 0.062885 0.046 Uiso 1 1 calc GR . . . .
H43C H 0.095388 0.992414 0.090332 0.046 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C1 1.706(4) . ?
Cl2 C1 1.707(4) . ?
Cl3 C1 1.630(5) . ?
C1 H1 1.0000 . ?
O1 C2 1.223(3) . ?
O2 C4 1.217(3) . ?
O3 C8 1.380(3) . ?
O3 C9 1.436(4) . ?
O4 C12 1.384(3) . ?
O4 C13 1.443(3) . ?
O5 C27 1.380(3) . ?
O5 C28 1.436(3) . ?
O6 C31 1.384(3) . ?
O6 C32 1.441(3) . ?
N1 C2 1.371(3) . ?
N1 C3 1.460(3) . ?
N1 C34 1.458(3) . ?
N2 C3 1.455(3) . ?
N2 C4 1.371(3) . ?
N2 C25 1.458(3) . ?
N3 C4 1.371(3) . ?
N3 C5 1.456(3) . ?
N3 C15 1.463(3) . ?
N4 C2 1.363(3) . ?
N4 C5 1.460(3) . ?
N4 C6 1.454(3) . ?
C3 C5 1.577(3) . ?
C3 C43 1.522(3) . ?
C5 C24 1.522(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.517(3) . ?
C7 C8 1.369(4) . ?
C7 C14 1.444(3) . ?
C8 C10 1.426(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.433(3) . ?
C10 C19 1.399(4) . ?
C11 C12 1.438(4) . ?
C11 C16 1.391(4) . ?
C12 C14 1.363(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.518(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16 0.9500 . ?
C16 C17 1.403(4) . ?
C17 C18 1.434(4) . ?
C17 C23 1.421(4) . ?
C18 C19 1.390(4) . ?
C18 C20 1.430(4) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C20 C21 1.351(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.413(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.364(5) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.514(3) . ?
C26 C27 1.364(3) . ?
C26 C33 1.447(3) . ?
C27 C29 1.438(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.438(3) . ?
C29 C38 1.390(3) . ?
C30 C31 1.429(3) . ?
C30 C35 1.395(3) . ?
C31 C33 1.367(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.515(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35 0.9500 . ?
C35 C36 1.392(3) . ?
C36 C37 1.433(3) . ?
C36 C42 1.429(3) . ?
C37 C38 1.398(3) . ?
C37 C39 1.424(3) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C39 C40 1.365(4) . ?
C40 H40 0.9500 . ?
C40 C41 1.420(4) . ?
C41 H41 0.9500 . ?
C41 C42 1.360(4) . ?
C42 H42 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 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
Cl1 C1 Cl2 115.2(3) . . ?
Cl1 C1 H1 97.5 . . ?
Cl2 C1 H1 97.5 . . ?
Cl3 C1 Cl1 121.1(3) . . ?
Cl3 C1 Cl2 118.7(3) . . ?
Cl3 C1 H1 97.5 . . ?
C8 O3 C9 115.0(2) . . ?
C12 O4 C13 115.0(2) . . ?
C27 O5 C28 114.84(19) . . ?
C31 O6 C32 115.32(19) . . ?
C2 N1 C3 112.20(19) . . ?
C2 N1 C34 120.51(19) . . ?
C34 N1 C3 122.39(19) . . ?
C3 N2 C25 123.23(19) . . ?
C4 N2 C3 112.7(2) . . ?
C4 N2 C25 122.0(2) . . ?
C4 N3 C5 112.46(19) . . ?
C4 N3 C15 120.9(2) . . ?
C5 N3 C15 122.6(2) . . ?
C2 N4 C5 112.9(2) . . ?
C2 N4 C6 122.5(2) . . ?
C6 N4 C5 123.0(2) . . ?
O1 C2 N1 125.2(2) . . ?
O1 C2 N4 125.9(2) . . ?
N4 C2 N1 108.7(2) . . ?
N1 C3 C5 102.84(18) . . ?
N1 C3 C43 110.71(19) . . ?
N2 C3 N1 112.63(18) . . ?
N2 C3 C5 102.79(18) . . ?
N2 C3 C43 111.6(2) . . ?
C43 C3 C5 115.9(2) . . ?
O2 C4 N2 125.5(2) . . ?
O2 C4 N3 125.9(2) . . ?
N3 C4 N2 108.5(2) . . ?
N3 C5 N4 112.39(19) . . ?
N3 C5 C3 102.86(18) . . ?
N3 C5 C24 111.6(2) . . ?
N4 C5 C3 102.60(18) . . ?
N4 C5 C24 110.6(2) . . ?
C24 C5 C3 116.3(2) . . ?
N4 C6 H6A 108.7 . . ?
N4 C6 H6B 108.7 . . ?
N4 C6 C7 114.3(2) . . ?
H6A C6 H6B 107.6 . . ?
C7 C6 H6A 108.7 . . ?
C7 C6 H6B 108.7 . . ?
C8 C7 C6 119.6(2) . . ?
C8 C7 C14 119.7(2) . . ?
C14 C7 C6 120.7(2) . . ?
O3 C8 C10 117.7(2) . . ?
C7 C8 O3 120.5(2) . . ?
C7 C8 C10 121.8(2) . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 C11 118.7(2) . . ?
C19 C10 C8 122.2(2) . . ?
C19 C10 C11 119.1(2) . . ?
C10 C11 C12 118.3(2) . . ?
C16 C11 C10 119.1(2) . . ?
C16 C11 C12 122.6(2) . . ?
O4 C12 C11 117.4(2) . . ?
C14 C12 O4 120.7(2) . . ?
C14 C12 C11 121.7(2) . . ?
O4 C13 H13A 109.5 . . ?
O4 C13 H13B 109.5 . . ?
O4 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C14 C15 119.9(2) . . ?
C12 C14 C7 119.8(2) . . ?
C12 C14 C15 120.2(2) . . ?
N3 C15 C14 115.05(19) . . ?
N3 C15 H15A 108.5 . . ?
N3 C15 H15B 108.5 . . ?
C14 C15 H15A 108.5 . . ?
C14 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
C11 C16 H16 119.1 . . ?
C11 C16 C17 121.7(2) . . ?
C17 C16 H16 119.1 . . ?
C16 C17 C18 119.0(2) . . ?
C16 C17 C23 122.4(3) . . ?
C23 C17 C18 118.6(3) . . ?
C19 C18 C17 119.1(2) . . ?
C19 C18 C20 122.1(3) . . ?
C20 C18 C17 118.8(3) . . ?
C10 C19 H19 119.1 . . ?
C18 C19 C10 121.8(2) . . ?
C18 C19 H19 119.1 . . ?
C18 C20 H20 119.8 . . ?
C21 C20 C18 120.4(3) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 H21 119.5 . . ?
C20 C21 C22 120.9(3) . . ?
C22 C21 H21 119.5 . . ?
C21 C22 H22 119.7 . . ?
C23 C22 C21 120.7(3) . . ?
C23 C22 H22 119.7 . . ?
C17 C23 H23 119.7 . . ?
C22 C23 C17 120.5(3) . . ?
C22 C23 H23 119.7 . . ?
C5 C24 H24A 109.5 . . ?
C5 C24 H24B 109.5 . . ?
C5 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2 C25 H25A 108.7 . . ?
N2 C25 H25B 108.7 . . ?
N2 C25 C26 114.23(19) . . ?
H25A C25 H25B 107.6 . . ?
C26 C25 H25A 108.7 . . ?
C26 C25 H25B 108.7 . . ?
C27 C26 C25 120.7(2) . . ?
C27 C26 C33 119.8(2) . . ?
C33 C26 C25 119.5(2) . . ?
O5 C27 C29 117.3(2) . . ?
C26 C27 O5 120.6(2) . . ?
C26 C27 C29 122.0(2) . . ?
O5 C28 H28A 109.5 . . ?
O5 C28 H28B 109.5 . . ?
O5 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 C30 118.0(2) . . ?
C38 C29 C27 122.7(2) . . ?
C38 C29 C30 119.3(2) . . ?
C31 C30 C29 118.7(2) . . ?
C35 C30 C29 118.8(2) . . ?
C35 C30 C31 122.6(2) . . ?
O6 C31 C30 117.5(2) . . ?
C33 C31 O6 120.3(2) . . ?
C33 C31 C30 122.0(2) . . ?
O6 C32 H32A 109.5 . . ?
O6 C32 H32B 109.5 . . ?
O6 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C26 C33 C34 119.9(2) . . ?
C31 C33 C26 119.5(2) . . ?
C31 C33 C34 120.5(2) . . ?
N1 C34 C33 114.47(19) . . ?
N1 C34 H34A 108.6 . . ?
N1 C34 H34B 108.6 . . ?
C33 C34 H34A 108.6 . . ?
C33 C34 H34B 108.6 . . ?
H34A C34 H34B 107.6 . . ?
C30 C35 H35 119.0 . . ?
C36 C35 C30 122.0(2) . . ?
C36 C35 H35 119.0 . . ?
C35 C36 C37 119.2(2) . . ?
C35 C36 C42 122.0(2) . . ?
C42 C36 C37 118.8(2) . . ?
C38 C37 C36 119.0(2) . . ?
C38 C37 C39 122.5(2) . . ?
C39 C37 C36 118.5(2) . . ?
C29 C38 C37 121.7(2) . . ?
C29 C38 H38 119.1 . . ?
C37 C38 H38 119.1 . . ?
C37 C39 H39 119.4 . . ?
C40 C39 C37 121.1(2) . . ?
C40 C39 H39 119.4 . . ?
C39 C40 H40 119.9 . . ?
C39 C40 C41 120.2(2) . . ?
C41 C40 H40 119.9 . . ?
C40 C41 H41 119.7 . . ?
C42 C41 C40 120.7(2) . . ?
C42 C41 H41 119.7 . . ?
C36 C42 H42 119.6 . . ?
C41 C42 C36 120.7(2) . . ?
C41 C42 H42 119.6 . . ?
C3 C43 H43A 109.5 . . ?
C3 C43 H43B 109.5 . . ?
C3 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?

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

data_190524lyz_17_0m
_database_code_depnum_ccdc_archive 'CCDC 1960288'
loop_
_audit_author_name
_audit_author_address
'Yuezhou Liu'
;Zhejiang University
China
;
_audit_update_record             
;
2019-10-19 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_audit_creation_date             2019-05-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H38 N4 O6, C9 H12'
_chemical_formula_sum            'C51 H50 N4 O6'
_chemical_formula_weight         814.95
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.2940(4)
_cell_length_b                   13.4087(5)
_cell_length_c                   16.3447(7)
_cell_angle_alpha                81.024(2)
_cell_angle_beta                 80.676(2)
_cell_angle_gamma                69.255(2)
_cell_volume                     2069.98(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      55.00
_cell_measurement_theta_min      4.02
_shelx_estimated_absorpt_T_max   0.974
_shelx_estimated_absorpt_T_min   0.949
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1073 before and 0.0728 after correction. The Ratio of minimum to maximum transmission is 0.7700. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0804
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20300
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.986
_diffrn_reflns_theta_min         4.022
_diffrn_ambient_temperature      169.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5665
_reflns_number_total             7603
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7603
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0616
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1235P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1805
_refine_ls_wR_factor_ref         0.1996
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B), C25(H25A,H25B), C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C29(H29),
 C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C45(H45), C47(H47), C49(H49)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 1.05260(16) 0.70929(12) 0.80514(9) 0.0417(4) Uani 1 1 d . . . . .
O2 O 0.49019(15) 0.99683(12) 0.82641(8) 0.0397(4) Uani 1 1 d . . . . .
O3 O 0.59198(14) 1.05855(11) 0.59208(8) 0.0353(3) Uani 1 1 d . . . . .
O4 O 1.15687(15) 0.82006(12) 0.59505(8) 0.0391(4) Uani 1 1 d . . . . .
O5 O 0.33852(15) 0.78611(12) 0.94390(9) 0.0413(4) Uani 1 1 d . . . . .
O6 O 0.87305(16) 0.49445(12) 0.87651(10) 0.0468(4) Uani 1 1 d . . . . .
N1 N 0.95812(17) 0.89101(13) 0.81844(9) 0.0313(4) Uani 1 1 d . . . . .
N2 N 0.86909(18) 0.77994(13) 0.90388(10) 0.0330(4) Uani 1 1 d . . . . .
N3 N 0.63993(17) 0.91181(13) 0.92708(9) 0.0321(4) Uani 1 1 d . . . . .
N4 N 0.71496(17) 1.00017(13) 0.81392(9) 0.0317(4) Uani 1 1 d . . . . .
C1 C 0.9673(2) 0.78495(17) 0.83867(11) 0.0331(5) Uani 1 1 d . . . . .
C2 C 0.7886(2) 0.88326(16) 0.93289(11) 0.0323(5) Uani 1 1 d . . . . .
C3 C 0.8338(2) 0.96157(16) 0.86230(11) 0.0310(4) Uani 1 1 d . . . . .
C4 C 0.8173(3) 0.88872(19) 1.02021(12) 0.0435(6) Uani 1 1 d . . . . .
H4A H 0.764757 0.960475 1.037102 0.065 Uiso 1 1 calc GR . . . .
H4B H 0.917550 0.873952 1.020445 0.065 Uiso 1 1 calc GR . . . .
H4C H 0.788109 0.835251 1.059319 0.065 Uiso 1 1 calc GR . . . .
C5 C 0.8611(2) 1.05390(17) 0.89188(12) 0.0375(5) Uani 1 1 d . . . . .
H5A H 0.880847 1.101766 0.843503 0.056 Uiso 1 1 calc GR . . . .
H5B H 0.941607 1.025330 0.923917 0.056 Uiso 1 1 calc GR . . . .
H5C H 0.778477 1.093969 0.927249 0.056 Uiso 1 1 calc GR . . . .
C6 C 0.6035(2) 0.97100(16) 0.85238(11) 0.0306(4) Uani 1 1 d . . . . .
C7 C 0.7172(2) 1.06110(16) 0.73242(11) 0.0322(4) Uani 1 1 d . . . . .
H7A H 0.758485 1.116852 0.734722 0.039 Uiso 1 1 calc R . . . .
H7B H 0.619594 1.098201 0.719826 0.039 Uiso 1 1 calc R . . . .
C8 C 0.7980(2) 0.99518(16) 0.66169(11) 0.0300(4) Uani 1 1 d . . . . .
C9 C 0.9433(2) 0.93077(16) 0.66393(11) 0.0296(4) Uani 1 1 d . . . . .
C10 C 1.0189(2) 0.92699(17) 0.73684(11) 0.0328(5) Uani 1 1 d . . . . .
H10A H 1.116688 0.878586 0.726507 0.039 Uiso 1 1 calc R . . . .
H10B H 1.021464 0.999628 0.739000 0.039 Uiso 1 1 calc R . . . .
C11 C 1.0149(2) 0.87631(16) 0.59721(11) 0.0319(4) Uani 1 1 d . . . . .
C12 C 0.9498(2) 0.88123(16) 0.52449(11) 0.0320(4) Uani 1 1 d . . . . .
C13 C 1.0224(2) 0.82717(17) 0.45589(12) 0.0352(5) Uani 1 1 d . . . . .
H13 H 1.118853 0.786235 0.456250 0.042 Uiso 1 1 calc R . . . .
C14 C 0.9558(2) 0.83197(17) 0.38633(11) 0.0340(5) Uani 1 1 d . . . . .
C15 C 1.0274(2) 0.77555(18) 0.31605(12) 0.0400(5) Uani 1 1 d . . . . .
H15 H 1.122989 0.731986 0.316012 0.048 Uiso 1 1 calc R . . . .
C16 C 0.9594(3) 0.78374(19) 0.24889(12) 0.0432(6) Uani 1 1 d . . . . .
H16 H 1.008175 0.745678 0.202533 0.052 Uiso 1 1 calc R . . . .
C17 C 0.8180(2) 0.84790(18) 0.24759(12) 0.0411(5) Uani 1 1 d . . . . .
H17 H 0.773257 0.854046 0.199667 0.049 Uiso 1 1 calc R . . . .
C18 C 0.7442(2) 0.90133(18) 0.31374(12) 0.0395(5) Uani 1 1 d . . . . .
H18 H 0.648181 0.943029 0.312254 0.047 Uiso 1 1 calc R . . . .
C19 C 0.8111(2) 0.89477(17) 0.38557(11) 0.0341(5) Uani 1 1 d . . . . .
C20 C 0.7388(2) 0.94889(17) 0.45418(11) 0.0338(5) Uani 1 1 d . . . . .
H20 H 0.642330 0.989923 0.453901 0.041 Uiso 1 1 calc R . . . .
C21 C 0.8053(2) 0.94401(16) 0.52328(11) 0.0305(4) Uani 1 1 d . . . . .
C22 C 0.7330(2) 1.00118(16) 0.59371(11) 0.0306(4) Uani 1 1 d . . . . .
C23 C 0.5618(3) 1.16650(19) 0.55308(14) 0.0490(6) Uani 1 1 d . . . . .
H23A H 0.614097 1.166152 0.497335 0.073 Uiso 1 1 calc GR . . . .
H23B H 0.589364 1.208374 0.586838 0.073 Uiso 1 1 calc GR . . . .
H23C H 0.461379 1.198745 0.548404 0.073 Uiso 1 1 calc GR . . . .
C24 C 1.1925(3) 0.7058(2) 0.61553(15) 0.0525(6) Uani 1 1 d . . . . .
H24A H 1.137889 0.679444 0.585796 0.079 Uiso 1 1 calc GR . . . .
H24B H 1.171353 0.689743 0.675759 0.079 Uiso 1 1 calc GR . . . .
H24C H 1.292438 0.670595 0.598989 0.079 Uiso 1 1 calc GR . . . .
C25 C 0.8524(2) 0.68069(17) 0.94472(12) 0.0372(5) Uani 1 1 d . . . . .
H25A H 0.847471 0.680692 1.005709 0.045 Uiso 1 1 calc R . . . .
H25B H 0.936379 0.620283 0.927363 0.045 Uiso 1 1 calc R . . . .
C26 C 0.7244(2) 0.66141(17) 0.92638(11) 0.0340(5) Uani 1 1 d . . . . .
C27 C 0.7405(2) 0.56683(17) 0.89733(13) 0.0376(5) Uani 1 1 d . . . . .
C28 C 0.6233(2) 0.53695(17) 0.88797(12) 0.0362(5) Uani 1 1 d . . . . .
C29 C 0.6399(2) 0.43663(17) 0.86575(13) 0.0402(5) Uani 1 1 d . . . . .
H29 H 0.731391 0.386158 0.856451 0.048 Uiso 1 1 calc R . . . .
C30 C 0.5255(2) 0.40880(17) 0.85688(12) 0.0361(5) Uani 1 1 d . . . . .
C31 C 0.5403(3) 0.30658(17) 0.83393(13) 0.0406(5) Uani 1 1 d . . . . .
H31 H 0.630666 0.253733 0.827689 0.049 Uiso 1 1 calc R . . . .
C32 C 0.4274(2) 0.28344(17) 0.82083(13) 0.0403(5) Uani 1 1 d . . . . .
H32 H 0.439492 0.215302 0.804796 0.048 Uiso 1 1 calc R . . . .
C33 C 0.2923(3) 0.36059(18) 0.83103(14) 0.0443(5) Uani 1 1 d . . . . .
H33 H 0.214142 0.344289 0.820733 0.053 Uiso 1 1 calc R . . . .
C34 C 0.2722(3) 0.45828(18) 0.85547(14) 0.0438(5) Uani 1 1 d . . . . .
H34 H 0.180280 0.508659 0.863252 0.053 Uiso 1 1 calc R . . . .
C35 C 0.3884(2) 0.48503(17) 0.86938(12) 0.0359(5) Uani 1 1 d . . . . .
C36 C 0.3710(2) 0.58537(18) 0.89389(13) 0.0392(5) Uani 1 1 d . . . . .
H36 H 0.279368 0.635437 0.903921 0.047 Uiso 1 1 calc R . . . .
C37 C 0.4860(2) 0.61265(16) 0.90372(12) 0.0342(5) Uani 1 1 d . . . . .
C38 C 0.4727(2) 0.71450(16) 0.92863(11) 0.0335(5) Uani 1 1 d . . . . .
C39 C 0.5860(2) 0.73878(16) 0.94126(11) 0.0337(5) Uani 1 1 d . . . . .
C40 C 0.5601(2) 0.84584(17) 0.97333(11) 0.0360(5) Uani 1 1 d . . . . .
H40A H 0.459384 0.888184 0.973508 0.043 Uiso 1 1 calc R . . . .
H40B H 0.581032 0.831427 1.031913 0.043 Uiso 1 1 calc R . . . .
C41 C 0.2840(3) 0.84726(19) 0.86858(15) 0.0488(6) Uani 1 1 d . . . . .
H41A H 0.289460 0.798160 0.828579 0.073 Uiso 1 1 calc GR . . . .
H41B H 0.339351 0.893193 0.844241 0.073 Uiso 1 1 calc GR . . . .
H41C H 0.186317 0.891929 0.881797 0.073 Uiso 1 1 calc GR . . . .
C42 C 0.9178(3) 0.5104(2) 0.78837(15) 0.0535(6) Uani 1 1 d . . . . .
H42A H 0.844056 0.512583 0.756311 0.080 Uiso 1 1 calc GR . . . .
H42B H 1.003225 0.451145 0.773362 0.080 Uiso 1 1 calc GR . . . .
H42C H 0.936521 0.578264 0.775717 0.080 Uiso 1 1 calc GR . . . .
C43 C 0.6387(5) 0.7683(3) 0.69073(19) 0.0926(12) Uani 1 1 d . . . . .
H43A H 0.729978 0.771339 0.697774 0.139 Uiso 1 1 calc GR . . . .
H43B H 0.590436 0.752826 0.745408 0.139 Uiso 1 1 calc GR . . . .
H43C H 0.582446 0.837458 0.664056 0.139 Uiso 1 1 calc GR . . . .
C44 C 0.6595(3) 0.6805(2) 0.63637(15) 0.0558(7) Uani 1 1 d . . . . .
C45 C 0.5882(3) 0.6087(2) 0.65821(14) 0.0527(6) Uani 1 1 d . . . . .
H45 H 0.525541 0.614769 0.708162 0.063 Uiso 1 1 calc R . . . .
C46 C 0.6050(3) 0.5280(2) 0.60978(14) 0.0516(6) Uani 1 1 d . . . . .
C47 C 0.6957(3) 0.5223(2) 0.53661(15) 0.0604(7) Uani 1 1 d . . . . .
H47 H 0.707658 0.468084 0.502120 0.072 Uiso 1 1 calc R . . . .
C48 C 0.7694(3) 0.5924(2) 0.51205(16) 0.0617(7) Uani 1 1 d . . . . .
C49 C 0.7509(3) 0.6704(2) 0.56296(16) 0.0583(7) Uani 1 1 d . . . . .
H49 H 0.801958 0.718533 0.547534 0.070 Uiso 1 1 calc R . . . .
C50 C 0.8625(4) 0.5866(3) 0.4299(2) 0.1011(13) Uani 1 1 d . . . . .
H50A H 0.815166 0.644224 0.389002 0.152 Uiso 1 1 calc GR . . . .
H50B H 0.882307 0.517035 0.409656 0.152 Uiso 1 1 calc GR . . . .
H50C H 0.950446 0.594629 0.437969 0.152 Uiso 1 1 calc GR . . . .
C51 C 0.5282(4) 0.4492(2) 0.63460(17) 0.0707(8) Uani 1 1 d . . . . .
H51A H 0.444996 0.479695 0.673411 0.106 Uiso 1 1 calc GR . . . .
H51B H 0.589664 0.382605 0.661720 0.106 Uiso 1 1 calc GR . . . .
H51C H 0.499939 0.433773 0.584837 0.106 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.219(2) . ?
O2 C6 1.220(2) . ?
O3 C22 1.384(2) . ?
O3 C23 1.434(3) . ?
O4 C11 1.384(2) . ?
O4 C24 1.440(3) . ?
O5 C38 1.384(2) . ?
O5 C41 1.444(3) . ?
O6 C27 1.391(3) . ?
O6 C42 1.446(3) . ?
N1 C1 1.381(3) . ?
N1 C3 1.450(3) . ?
N1 C10 1.465(2) . ?
N2 C1 1.356(3) . ?
N2 C2 1.447(3) . ?
N2 C25 1.447(2) . ?
N3 C2 1.455(3) . ?
N3 C6 1.377(3) . ?
N3 C40 1.461(2) . ?
N4 C3 1.459(2) . ?
N4 C6 1.368(2) . ?
N4 C7 1.451(2) . ?
C2 C3 1.564(3) . ?
C2 C4 1.521(2) . ?
C3 C5 1.524(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.515(3) . ?
C8 C9 1.441(3) . ?
C8 C22 1.365(3) . ?
C9 C10 1.510(2) . ?
C9 C11 1.368(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.438(3) . ?
C12 C13 1.393(3) . ?
C12 C21 1.428(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.402(3) . ?
C14 C15 1.427(3) . ?
C14 C19 1.429(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.365(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.406(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.360(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.431(3) . ?
C19 C20 1.393(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.394(3) . ?
C21 C22 1.435(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.512(3) . ?
C26 C27 1.369(3) . ?
C26 C39 1.444(3) . ?
C27 C28 1.436(3) . ?
C28 C29 1.393(3) . ?
C28 C37 1.429(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.389(3) . ?
C30 C31 1.427(3) . ?
C30 C35 1.424(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.360(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.412(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.365(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.425(3) . ?
C35 C36 1.406(3) . ?
C36 H36 0.9500 . ?
C36 C37 1.396(3) . ?
C37 C38 1.440(3) . ?
C38 C39 1.369(3) . ?
C39 C40 1.525(3) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C43 C44 1.520(4) . ?
C44 C45 1.378(4) . ?
C44 C49 1.392(4) . ?
C45 H45 0.9500 . ?
C45 C46 1.384(3) . ?
C46 C47 1.387(4) . ?
C46 C51 1.505(3) . ?
C47 H47 0.9500 . ?
C47 C48 1.382(4) . ?
C48 C49 1.379(4) . ?
C48 C50 1.513(4) . ?
C49 H49 0.9500 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 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
C22 O3 C23 114.44(15) . . ?
C11 O4 C24 114.74(17) . . ?
C38 O5 C41 112.45(16) . . ?
C27 O6 C42 110.96(17) . . ?
C1 N1 C3 111.10(16) . . ?
C1 N1 C10 120.69(16) . . ?
C3 N1 C10 121.27(16) . . ?
C1 N2 C2 113.35(16) . . ?
C1 N2 C25 123.67(17) . . ?
C25 N2 C2 122.83(16) . . ?
C2 N3 C40 121.10(17) . . ?
C6 N3 C2 111.56(15) . . ?
C6 N3 C40 121.52(16) . . ?
C6 N4 C3 113.16(15) . . ?
C6 N4 C7 123.89(16) . . ?
C7 N4 C3 122.93(15) . . ?
O1 C1 N1 125.42(18) . . ?
O1 C1 N2 126.45(18) . . ?
N2 C1 N1 108.08(17) . . ?
N2 C2 N3 112.12(15) . . ?
N2 C2 C3 101.76(15) . . ?
N2 C2 C4 111.35(17) . . ?
N3 C2 C3 103.02(15) . . ?
N3 C2 C4 112.12(16) . . ?
C4 C2 C3 115.84(15) . . ?
N1 C3 N4 112.42(14) . . ?
N1 C3 C2 102.97(15) . . ?
N1 C3 C5 112.17(16) . . ?
N4 C3 C2 101.69(15) . . ?
N4 C3 C5 111.54(17) . . ?
C5 C3 C2 115.40(14) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O2 C6 N3 126.29(18) . . ?
O2 C6 N4 125.81(18) . . ?
N4 C6 N3 107.84(16) . . ?
N4 C7 H7A 108.6 . . ?
N4 C7 H7B 108.6 . . ?
N4 C7 C8 114.82(17) . . ?
H7A C7 H7B 107.5 . . ?
C8 C7 H7A 108.6 . . ?
C8 C7 H7B 108.6 . . ?
C9 C8 C7 120.81(16) . . ?
C22 C8 C7 119.03(18) . . ?
C22 C8 C9 120.10(17) . . ?
C8 C9 C10 120.92(16) . . ?
C11 C9 C8 119.27(17) . . ?
C11 C9 C10 119.74(18) . . ?
N1 C10 C9 115.52(15) . . ?
N1 C10 H10A 108.4 . . ?
N1 C10 H10B 108.4 . . ?
C9 C10 H10A 108.4 . . ?
C9 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
O4 C11 C12 117.26(16) . . ?
C9 C11 O4 120.52(17) . . ?
C9 C11 C12 122.06(19) . . ?
C13 C12 C11 122.45(19) . . ?
C13 C12 C21 119.25(18) . . ?
C21 C12 C11 118.30(17) . . ?
C12 C13 H13 119.4 . . ?
C12 C13 C14 121.3(2) . . ?
C14 C13 H13 119.4 . . ?
C13 C14 C15 122.3(2) . . ?
C13 C14 C19 119.19(18) . . ?
C15 C14 C19 118.56(18) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.5(2) . . ?
C16 C15 H15 119.8 . . ?
C15 C16 H16 119.6 . . ?
C15 C16 C17 120.71(19) . . ?
C17 C16 H16 119.6 . . ?
C16 C17 H17 119.4 . . ?
C18 C17 C16 121.14(19) . . ?
C18 C17 H17 119.4 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.0(2) . . ?
C19 C18 H18 120.0 . . ?
C14 C19 C18 119.05(18) . . ?
C20 C19 C14 119.42(17) . . ?
C20 C19 C18 121.5(2) . . ?
C19 C20 H20 119.4 . . ?
C19 C20 C21 121.3(2) . . ?
C21 C20 H20 119.4 . . ?
C12 C21 C22 118.46(17) . . ?
C20 C21 C12 119.58(17) . . ?
C20 C21 C22 121.96(19) . . ?
O3 C22 C21 117.23(16) . . ?
C8 C22 O3 120.89(17) . . ?
C8 C22 C21 121.79(18) . . ?
O3 C23 H23A 109.5 . . ?
O3 C23 H23B 109.5 . . ?
O3 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O4 C24 H24A 109.5 . . ?
O4 C24 H24B 109.5 . . ?
O4 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2 C25 H25A 108.6 . . ?
N2 C25 H25B 108.6 . . ?
N2 C25 C26 114.54(16) . . ?
H25A C25 H25B 107.6 . . ?
C26 C25 H25A 108.6 . . ?
C26 C25 H25B 108.6 . . ?
C27 C26 C25 118.9(2) . . ?
C27 C26 C39 119.56(18) . . ?
C39 C26 C25 121.53(18) . . ?
O6 C27 C28 117.02(18) . . ?
C26 C27 O6 120.76(18) . . ?
C26 C27 C28 122.2(2) . . ?
C29 C28 C27 122.0(2) . . ?
C29 C28 C37 119.73(19) . . ?
C37 C28 C27 118.23(18) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 C28 121.4(2) . . ?
C30 C29 H29 119.3 . . ?
C29 C30 C31 122.3(2) . . ?
C29 C30 C35 119.36(19) . . ?
C35 C30 C31 118.34(19) . . ?
C30 C31 H31 119.4 . . ?
C32 C31 C30 121.2(2) . . ?
C32 C31 H31 119.4 . . ?
C31 C32 H32 120.0 . . ?
C31 C32 C33 120.1(2) . . ?
C33 C32 H32 120.0 . . ?
C32 C33 H33 119.5 . . ?
C34 C33 C32 121.0(2) . . ?
C34 C33 H33 119.5 . . ?
C33 C34 H34 119.9 . . ?
C33 C34 C35 120.3(2) . . ?
C35 C34 H34 119.9 . . ?
C30 C35 C34 119.09(19) . . ?
C36 C35 C30 119.38(19) . . ?
C36 C35 C34 121.5(2) . . ?
C35 C36 H36 119.5 . . ?
C37 C36 C35 121.1(2) . . ?
C37 C36 H36 119.5 . . ?
C28 C37 C38 118.19(18) . . ?
C36 C37 C28 118.95(19) . . ?
C36 C37 C38 122.9(2) . . ?
O5 C38 C37 116.97(17) . . ?
C39 C38 O5 120.60(18) . . ?
C39 C38 C37 122.3(2) . . ?
C26 C39 C40 122.45(18) . . ?
C38 C39 C26 119.21(18) . . ?
C38 C39 C40 118.31(19) . . ?
N3 C40 C39 116.52(16) . . ?
N3 C40 H40A 108.2 . . ?
N3 C40 H40B 108.2 . . ?
C39 C40 H40A 108.2 . . ?
C39 C40 H40B 108.2 . . ?
H40A C40 H40B 107.3 . . ?
O5 C41 H41A 109.5 . . ?
O5 C41 H41B 109.5 . . ?
O5 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O6 C42 H42A 109.5 . . ?
O6 C42 H42B 109.5 . . ?
O6 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C44 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
C44 C43 H43C 109.5 . . ?
C45 C44 C43 121.0(3) . . ?
C45 C44 C49 118.1(2) . . ?
C49 C44 C43 120.8(2) . . ?
C44 C45 H45 118.9 . . ?
C44 C45 C46 122.2(2) . . ?
C46 C45 H45 118.9 . . ?
C45 C46 C47 117.5(2) . . ?
C45 C46 C51 121.9(2) . . ?
C47 C46 C51 120.6(2) . . ?
C46 C47 H47 118.8 . . ?
C48 C47 C46 122.4(2) . . ?
C48 C47 H47 118.8 . . ?
C47 C48 C50 120.8(3) . . ?
C49 C48 C47 118.0(2) . . ?
C49 C48 C50 121.1(3) . . ?
C44 C49 H49 119.1 . . ?
C48 C49 C44 121.7(2) . . ?
C48 C49 H49 119.1 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C46 C51 H51A 109.5 . . ?
C46 C51 H51B 109.5 . . ?
C46 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.111 0.287 0.969 15.6 2.9 ?
2 0.111 0.713 0.031 15.6 2.9 ?

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

data_190610lyz_0m
_database_code_depnum_ccdc_archive 'CCDC 1960291'
_audit_update_record             
;
2020-01-20 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_audit_creation_date             2020-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H38 N4 O6, C5.5 N, C12 H19 N'
_chemical_formula_sum            'C59.50 H57 N6 O6'
_chemical_formula_weight         952.11
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0150 0.0070 '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 0.0250 0.0140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0410 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.4161(2)
_cell_length_b                   14.2726(3)
_cell_length_c                   18.0403(4)
_cell_angle_alpha                106.7040(10)
_cell_angle_beta                 91.8020(10)
_cell_angle_gamma                100.7610(10)
_cell_volume                     2513.27(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.898
_cell_measurement_theta_min      4.136
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.967
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1099 before and 0.0594 after correction. The Ratio of minimum to maximum transmission is 0.8737. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22734
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.876
_diffrn_reflns_theta_min         3.068
_diffrn_ambient_temperature      169.97
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6560
_reflns_number_total             9191
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0074(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         9191
_refine_ls_number_restraints     318
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0751
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1128P)²+2.2428P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2041
_refine_ls_wR_factor_ref         0.2336
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C43-C47 = C47-C49 = C50-C47 = C46-C45 = C46-C49 = C46-C44 = C59-C57 = C60-C57
 = C60-C61 = C60-C63 = C59-C62 = C59-C63
 1.53 with sigma of 0.02
 C51-C49 = C52-C51 = C52-C58 = C58-C57 = C54-C57 = C54-C49 = C53-C49 = C53-C57
 = C56-C57 = C56-C55 = C48-C55 = C48-C49
 1.39 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C63 \\sim C57 \\sim C49 \\sim N6 \\sim C56 \\sim C59 \\sim C47 \\sim C43 \\sim
C62 \\sim C55 \\sim C50 \\sim C48 \\sim C53 \\sim N5 \\sim C46 \\sim C44 \\sim
C54 \\sim C51 \\sim C52 \\sim C58 \\sim C45 \\sim C61 \\sim C60: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C65(0.5) C64(0.5) C68(0.5) C67(0.5) C70(0.5) H63A(0.5) H63B(0.5)
 H63C(0.5) H63D(0.5) H63E(0.5) H63F(0.5) N6(0.5) H6A(0.5) H6B(0.5) C56(0.5)
 H56(0.5) C59(0.5) H59(0.5) C47(0.5) H47(0.5) C43(0.5) H43A(0.5) H43B(0.5)
 H43C(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5) C55(0.5) H55(0.5) C50(0.5)
 H50A(0.5) H50B(0.5) H50C(0.5) C48(0.5) H48(0.5) C53(0.5) N5(0.5) H5A(0.5)
 H5B(0.5) C46(0.5) H46(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5) C54(0.5)
 C51(0.5) H51(0.5) C52(0.5) H52(0.5) C58(0.5) H58(0.5) C45(0.5) H45A(0.5)
 H45B(0.5) H45C(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) C60(0.5) H60(0.5)
5.a Rotating group:
 N6(H6A,H6B), N5(H5A,H5B)
5.b Ternary CH refined with riding coordinates:
 C59(H59), C47(H47), C46(H46), C60(H60)
5.c Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C26(H26A,H26B), C25(H25A,H25B), C17(H17A,H17B)
5.d Aromatic/amide H refined with riding coordinates:
 C36(H36), C40(H40), C41(H41), C42(H42), C7(H7), C39(H39), C35(H35), C3(H3),
 C2(H2), C1(H1), C4(H4), C8(H8), C56(H56), C55(H55), C48(H48), C51(H51),
 C52(H52), C58(H58)
5.e Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C24(H24A,H24B,H24C), C14(H14A,H14B,H14C), C13(H13A,H13B,
 H13C), C31(H31A,H31B,H31C), C19(H19A,H19B,H19C), C63(H63A,H63B,H63C), C63(H63D,
 H63E,H63F), C43(H43A,H43B,H43C), C62(H62A,H62B,H62C), C50(H50A,H50B,H50C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C61(H61A,H61B,H61C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O3 O 0.35005(19) 0.31516(16) 0.20178(11) 0.0420(5) Uani 1 1 d . . . . .
O1 O -0.0683(2) 0.60410(16) 0.39436(12) 0.0435(5) Uani 1 1 d . . . . .
O5 O 0.27740(19) 0.70688(16) 0.08452(13) 0.0447(5) Uani 1 1 d . . . . .
O4 O 0.0019(2) 0.57089(16) 0.17950(12) 0.0448(5) Uani 1 1 d . . . . .
O6 O 0.59929(19) 0.44251(15) 0.09890(12) 0.0405(5) Uani 1 1 d . . . . .
O2 O 0.3029(2) 0.37713(17) 0.41324(12) 0.0476(6) Uani 1 1 d . . . . .
N1 N 0.0834(2) 0.44544(19) 0.09534(14) 0.0376(6) Uani 1 1 d . . . . .
N4 N 0.1280(2) 0.30898(19) 0.20395(13) 0.0382(6) Uani 1 1 d . . . . .
N3 N -0.0253(2) 0.41197(18) 0.19197(13) 0.0351(5) Uani 1 1 d . . . . .
N2 N 0.2222(2) 0.32912(18) 0.10002(13) 0.0343(5) Uani 1 1 d . . . . .
C23 C 0.0202(3) 0.3199(2) 0.15676(16) 0.0354(6) Uani 1 1 d . . . . .
C34 C 0.2121(3) 0.5216(2) 0.46974(16) 0.0366(6) Uani 1 1 d . . . . .
C28 C 0.1206(3) 0.4027(2) 0.34403(16) 0.0346(6) Uani 1 1 d . . . . .
C22 C 0.2454(3) 0.3193(2) 0.17238(15) 0.0326(6) Uani 1 1 d . . . . .
C21 C 0.0196(3) 0.4853(2) 0.15856(16) 0.0356(6) Uani 1 1 d . . . . .
C32 C 0.2647(5) 0.3049(3) 0.4536(2) 0.0672(11) Uani 1 1 d . . . . .
H32A H 0.192658 0.252250 0.422676 0.101 Uiso 1 1 calc GR . . . .
H32B H 0.235558 0.337513 0.503968 0.101 Uiso 1 1 calc GR . . . .
H32C H 0.339583 0.275335 0.461907 0.101 Uiso 1 1 calc GR . . . .
C24 C -0.0898(3) 0.2292(2) 0.13797(19) 0.0476(8) Uani 1 1 d . . . . .
H24A H -0.056742 0.169715 0.110718 0.071 Uiso 1 1 calc GR . . . .
H24B H -0.160204 0.237798 0.104751 0.071 Uiso 1 1 calc GR . . . .
H24C H -0.123999 0.221035 0.186229 0.071 Uiso 1 1 calc GR . . . .
C14 C 0.2322(3) 0.7588(3) 0.1573(2) 0.0520(8) Uani 1 1 d . . . . .
H14A H 0.178521 0.804585 0.148143 0.078 Uiso 1 1 calc GR . . . .
H14B H 0.307971 0.796769 0.194240 0.078 Uiso 1 1 calc GR . . . .
H14C H 0.179516 0.709989 0.178745 0.078 Uiso 1 1 calc GR . . . .
C18 C 0.3294(3) 0.3612(2) 0.05703(16) 0.0350(6) Uani 1 1 d . . . . .
H18A H 0.298284 0.338493 0.001110 0.042 Uiso 1 1 calc R . . . .
H18B H 0.401707 0.327136 0.063516 0.042 Uiso 1 1 calc R . . . .
C20 C 0.0893(3) 0.3413(2) 0.08530(15) 0.0350(6) Uani 1 1 d . . . . .
C16 C 0.3840(3) 0.4725(2) 0.08050(15) 0.0322(6) Uani 1 1 d . . . . .
C11 C 0.5153(3) 0.5079(2) 0.10241(15) 0.0321(6) Uani 1 1 d . . . . .
C36 C 0.3046(3) 0.5531(2) 0.53361(17) 0.0420(7) Uani 1 1 d . . . . .
H36 H 0.368331 0.514173 0.536341 0.050 Uiso 1 1 calc R . . . .
C40 C 0.4021(3) 0.6736(3) 0.65925(18) 0.0464(8) Uani 1 1 d . . . . .
H40 H 0.466165 0.635211 0.662643 0.056 Uiso 1 1 calc R . . . .
C13 C 0.6325(3) 0.4267(3) 0.1712(2) 0.0533(9) Uani 1 1 d . . . . .
H13A H 0.696081 0.382904 0.163874 0.080 Uiso 1 1 calc GR . . . .
H13B H 0.553170 0.395402 0.189779 0.080 Uiso 1 1 calc GR . . . .
H13C H 0.670896 0.491010 0.209457 0.080 Uiso 1 1 calc GR . . . .
C41 C 0.3093(3) 0.8178(3) 0.71183(19) 0.0511(8) Uani 1 1 d . . . . .
H41 H 0.311893 0.878462 0.751814 0.061 Uiso 1 1 calc R . . . .
C26 C 0.1186(3) 0.3041(2) 0.28325(16) 0.0393(7) Uani 1 1 d . . . . .
H26A H 0.192411 0.275947 0.297375 0.047 Uiso 1 1 calc R . . . .
H26B H 0.036245 0.257276 0.284636 0.047 Uiso 1 1 calc R . . . .
C37 C 0.2100(3) 0.6982(2) 0.58972(16) 0.0384(7) Uani 1 1 d . . . . .
C30 C 0.2091(3) 0.4319(2) 0.40746(16) 0.0374(7) Uani 1 1 d . . . . .
C27 C 0.0272(3) 0.4636(2) 0.33752(15) 0.0330(6) Uani 1 1 d . . . . .
C38 C 0.3062(3) 0.6402(2) 0.59376(16) 0.0385(7) Uani 1 1 d . . . . .
C10 C 0.5731(3) 0.6120(2) 0.12237(15) 0.0326(6) Uani 1 1 d . . . . .
C42 C 0.4026(3) 0.7594(3) 0.71655(19) 0.0495(8) Uani 1 1 d . . . . .
H42 H 0.466119 0.780188 0.760076 0.059 Uiso 1 1 calc R . . . .
C7 C 0.7065(3) 0.6499(2) 0.14688(15) 0.0349(6) Uani 1 1 d . . . . .
H7 H 0.761444 0.605499 0.151916 0.042 Uiso 1 1 calc R . . . .
C39 C 0.2155(3) 0.7886(2) 0.65085(18) 0.0452(7) Uani 1 1 d . . . . .
H39 H 0.153136 0.828881 0.649021 0.054 Uiso 1 1 calc R . . . .
C6 C 0.7602(3) 0.7518(2) 0.16405(16) 0.0366(6) Uani 1 1 d . . . . .
C35 C 0.1171(3) 0.6669(2) 0.52555(17) 0.0389(7) Uani 1 1 d . . . . .
H35 H 0.052507 0.705242 0.523301 0.047 Uiso 1 1 calc R . . . .
C3 C 0.8947(3) 0.7927(2) 0.19273(17) 0.0419(7) Uani 1 1 d . . . . .
H3 H 0.949428 0.750261 0.202157 0.050 Uiso 1 1 calc R . . . .
C29 C 0.0256(3) 0.5481(2) 0.39656(16) 0.0353(6) Uani 1 1 d . . . . .
C2 C 0.9448(3) 0.8914(3) 0.2066(2) 0.0519(8) Uani 1 1 d . . . . .
H2 H 1.033827 0.917602 0.226670 0.062 Uiso 1 1 calc R . . . .
C25 C -0.0753(3) 0.4327(2) 0.26846(16) 0.0368(7) Uani 1 1 d . . . . .
H25A H -0.137488 0.372061 0.270508 0.044 Uiso 1 1 calc R . . . .
H25B H -0.125385 0.486427 0.274096 0.044 Uiso 1 1 calc R . . . .
C1 C 0.8664(4) 0.9564(3) 0.1915(2) 0.0598(10) Uani 1 1 d . . . . .
H1 H 0.903581 1.025187 0.200274 0.072 Uiso 1 1 calc R . . . .
C31 C -0.0245(4) 0.6891(3) 0.3673(2) 0.0584(9) Uani 1 1 d . . . . .
H31A H -0.002586 0.666269 0.313487 0.088 Uiso 1 1 calc GR . . . .
H31B H 0.053368 0.731955 0.400195 0.088 Uiso 1 1 calc GR . . . .
H31C H -0.094462 0.726945 0.369742 0.088 Uiso 1 1 calc GR . . . .
C4 C 0.7378(4) 0.9201(3) 0.1643(2) 0.0562(9) Uani 1 1 d . . . . .
H4 H 0.686240 0.963662 0.153314 0.067 Uiso 1 1 calc R . . . .
C5 C 0.6798(3) 0.8180(2) 0.15223(17) 0.0410(7) Uani 1 1 d . . . . .
C19 C 0.0267(3) 0.2750(3) 0.00589(17) 0.0459(8) Uani 1 1 d . . . . .
H19A H -0.065569 0.279875 0.000480 0.069 Uiso 1 1 calc GR . . . .
H19B H 0.031974 0.205534 0.000519 0.069 Uiso 1 1 calc GR . . . .
H19C H 0.073161 0.296719 -0.034579 0.069 Uiso 1 1 calc GR . . . .
C8 C 0.5468(3) 0.7800(2) 0.12840(18) 0.0414(7) Uani 1 1 d . . . . .
H8 H 0.492877 0.823975 0.120973 0.050 Uiso 1 1 calc R . . . .
C9 C 0.4909(3) 0.6795(2) 0.11520(16) 0.0355(6) Uani 1 1 d . . . . .
C12 C 0.3540(3) 0.6403(2) 0.09271(16) 0.0363(6) Uani 1 1 d . . . . .
C15 C 0.3006(3) 0.5409(2) 0.07669(15) 0.0334(6) Uani 1 1 d . . . . .
C17 C 0.1555(3) 0.5038(2) 0.05017(17) 0.0386(7) Uani 1 1 d . . . . .
H17A H 0.115264 0.562193 0.052829 0.046 Uiso 1 1 calc R . . . .
H17B H 0.145920 0.462407 -0.004884 0.046 Uiso 1 1 calc R . . . .
C33 C 0.1167(3) 0.5805(2) 0.46459(16) 0.0355(6) Uani 1 1 d . . . . .
N7 N 0.4244(3) 0.8451(2) -0.0315(2) 0.0660(9) Uani 1 1 d . . . . .
C65 C 0.4787(6) 0.9571(4) -0.0076(4) 0.0450(15) Uani 0.5 1 d . . P . .
C71 C 0.8208(6) 0.9591(7) -0.0472(4) 0.144(3) Uani 1 1 d . . . . .
C66 C 0.5892(3) 0.9855(2) -0.0403(2) 0.0481(8) Uani 1 1 d . . . . .
C64 C 0.3600(7) 0.9027(5) 0.0176(4) 0.0478(15) Uani 0.5 1 d . . P . .
C68 C 0.6702(7) 0.9256(6) -0.0910(5) 0.062(2) Uani 0.5 1 d . . P . .
C69 C 0.6937(5) 0.9624(4) -0.1677(3) 0.0938(16) Uani 1 1 d . . . . .
C67 C 0.5362(6) 0.8746(5) -0.0633(4) 0.0469(15) Uani 0.5 1 d . . P . .
C70 C 0.7138(7) 1.0126(5) -0.0769(5) 0.0594(19) Uani 0.5 1 d . . P . .
C63 C 0.3361(5) 0.6609(5) 0.3138(4) 0.1115(17) Uani 1 1 d D U . . .
H63A H 0.288703 0.638481 0.353684 0.167 Uiso 0.5 1 calc GR . P A 1
H63B H 0.319509 0.606852 0.264562 0.167 Uiso 0.5 1 calc GR . P A 1
H63C H 0.305878 0.719160 0.306911 0.167 Uiso 0.5 1 calc GR . P A 1
H63D H 0.287235 0.714932 0.327815 0.167 Uiso 0.5 1 calc GR . P B 2
H63E H 0.275534 0.596483 0.304582 0.167 Uiso 0.5 1 calc GR . P B 2
H63F H 0.379135 0.662380 0.266474 0.167 Uiso 0.5 1 calc GR . P B 2
C57 C 0.5291(4) 0.7756(3) 0.4046(2) 0.0646(9) Uani 1 1 d D U . . .
C49 C 0.6708(5) 0.9193(3) 0.4957(2) 0.0789(11) Uani 1 1 d D U . . .
N6 N 0.7291(8) 0.8198(7) 0.3637(4) 0.0745(19) Uani 0.5 1 d . U P C 1
H6A H 0.683332 0.785447 0.317544 0.089 Uiso 0.5 1 d GR . P C 1
H6B H 0.773523 0.878176 0.358834 0.089 Uiso 0.5 1 d GR . P C 1
C56 C 0.4425(9) 0.7942(7) 0.4708(5) 0.0703(18) Uani 0.5 1 d D U P D 1
H56 H 0.357731 0.752605 0.464254 0.084 Uiso 0.5 1 calc R . P D 1
C59 C 0.4760(9) 0.6880(7) 0.3378(6) 0.080(2) Uani 0.5 1 d D U P D 1
H59 H 0.514875 0.707387 0.293051 0.097 Uiso 0.5 1 calc R . P D 1
C47 C 0.8274(10) 0.9731(6) 0.5029(5) 0.084(2) Uani 0.5 1 d D U P D 1
H47 H 0.878082 0.922032 0.476164 0.101 Uiso 0.5 1 calc R . P D 1
C43 C 0.8774(13) 1.0145(8) 0.5896(6) 0.110(4) Uani 0.5 1 d D U P D 1
H43A H 0.812190 1.047384 0.618874 0.165 Uiso 0.5 1 calc GR . P D 1
H43B H 0.960207 1.062998 0.596024 0.165 Uiso 0.5 1 calc GR . P D 1
H43C H 0.891787 0.959521 0.609040 0.165 Uiso 0.5 1 calc GR . P D 1
C62 C 0.5224(13) 0.5925(9) 0.3338(5) 0.070(3) Uani 0.5 1 d D U P D 1
H62A H 0.500230 0.545941 0.281234 0.104 Uiso 0.5 1 calc GR . P D 1
H62B H 0.479270 0.562152 0.371207 0.104 Uiso 0.5 1 calc GR . P D 1
H62C H 0.617648 0.607644 0.346255 0.104 Uiso 0.5 1 calc GR . P D 1
C55 C 0.4797(10) 0.8668(7) 0.5386(6) 0.067(2) Uani 0.5 1 d D U P D 1
H55 H 0.420740 0.876715 0.577946 0.080 Uiso 0.5 1 calc R . P D 1
C50 C 0.8440(13) 1.0556(8) 0.4649(7) 0.106(3) Uani 0.5 1 d D U P D 1
H50A H 0.796439 1.030558 0.413111 0.159 Uiso 0.5 1 calc GR . P D 1
H50B H 0.937440 1.078205 0.460358 0.159 Uiso 0.5 1 calc GR . P D 1
H50C H 0.809063 1.111706 0.496741 0.159 Uiso 0.5 1 calc GR . P D 1
C48 C 0.6060(9) 0.9281(7) 0.5512(6) 0.0780(19) Uani 0.5 1 d D U P D 1
H48 H 0.638788 0.974010 0.600668 0.094 Uiso 0.5 1 calc R . P D 1
C53 C 0.6479(8) 0.8368(6) 0.4215(4) 0.0667(16) Uani 0.5 1 d D U P C 1
N5 N 0.4769(9) 0.8060(7) 0.5287(5) 0.088(3) Uani 0.5 1 d . U P D 2
H5A H 0.511402 0.833028 0.578140 0.105 Uiso 0.5 1 d GR . P D 2
H5B H 0.399382 0.823447 0.525460 0.105 Uiso 0.5 1 d GR . P D 2
C46 C 0.6711(12) 0.9973(8) 0.5809(6) 0.103(3) Uani 0.5 1 d D U P D 2
H46 H 0.581207 1.010731 0.590007 0.123 Uiso 0.5 1 calc R . P D 2
C44 C 0.7161(16) 0.9592(10) 0.6382(8) 0.140(5) Uani 0.5 1 d D U P D 2
H44A H 0.642565 0.915453 0.651883 0.210 Uiso 0.5 1 calc GR . P D 2
H44B H 0.754044 1.014595 0.684391 0.210 Uiso 0.5 1 calc GR . P D 2
H44C H 0.783154 0.920975 0.618168 0.210 Uiso 0.5 1 calc GR . P D 2
C54 C 0.5572(6) 0.8393(5) 0.4758(3) 0.0456(13) Uani 0.5 1 d D U P D 2
C51 C 0.7296(10) 0.9496(6) 0.4419(5) 0.081(2) Uani 0.5 1 d D U P D 2
H51 H 0.795533 1.008953 0.455243 0.098 Uiso 0.5 1 calc R . P D 2
C52 C 0.6958(12) 0.8952(8) 0.3662(5) 0.101(3) Uani 0.5 1 d D U P D 2
H52 H 0.737502 0.917478 0.326424 0.121 Uiso 0.5 1 calc R . P D 2
C58 C 0.6014(11) 0.8081(7) 0.3464(5) 0.095(2) Uani 0.5 1 d D U P D 2
H58 H 0.583712 0.768819 0.293488 0.114 Uiso 0.5 1 calc R . P D 2
C45 C 0.7704(16) 1.0953(11) 0.5924(9) 0.166(6) Uani 0.5 1 d D U P D 2
H45A H 0.859496 1.082198 0.591689 0.249 Uiso 0.5 1 calc GR . P D 2
H45B H 0.761531 1.142718 0.642526 0.249 Uiso 0.5 1 calc GR . P D 2
H45C H 0.753615 1.123546 0.550476 0.249 Uiso 0.5 1 calc GR . P D 2
C61 C 0.5039(13) 0.5933(9) 0.3707(8) 0.095(3) Uani 0.5 1 d D U P D 2
H61A H 0.588106 0.608322 0.349483 0.142 Uiso 0.5 1 calc GR . P D 2
H61B H 0.449685 0.532046 0.335587 0.142 Uiso 0.5 1 calc GR . P D 2
H61C H 0.519328 0.584084 0.421809 0.142 Uiso 0.5 1 calc GR . P D 2
C60 C 0.4375(8) 0.6745(6) 0.3786(5) 0.0656(18) Uani 0.5 1 d D U P D 2
H60 H 0.385294 0.673643 0.424032 0.079 Uiso 0.5 1 calc R . P D 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
O3 C22 1.216(3) . ?
O1 C29 1.380(3) . ?
O1 C31 1.437(4) . ?
O5 C14 1.451(4) . ?
O5 C12 1.386(3) . ?
O4 C21 1.222(3) . ?
O6 C11 1.383(3) . ?
O6 C13 1.428(4) . ?
O2 C32 1.432(4) . ?
O2 C30 1.380(3) . ?
N1 C21 1.371(4) . ?
N1 C20 1.458(4) . ?
N1 C17 1.455(4) . ?
N4 C23 1.446(4) . ?
N4 C22 1.367(4) . ?
N4 C26 1.457(3) . ?
N3 C23 1.458(4) . ?
N3 C21 1.369(4) . ?
N3 C25 1.460(3) . ?
N2 C22 1.371(3) . ?
N2 C18 1.458(3) . ?
N2 C20 1.453(3) . ?
C23 C24 1.508(4) . ?
C23 C20 1.573(4) . ?
C34 C36 1.389(4) . ?
C34 C30 1.434(4) . ?
C34 C33 1.433(4) . ?
C28 C26 1.511(4) . ?
C28 C30 1.360(4) . ?
C28 C27 1.443(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C16 1.513(4) . ?
C20 C19 1.518(4) . ?
C16 C11 1.369(4) . ?
C16 C15 1.437(4) . ?
C11 C10 1.430(4) . ?
C36 H36 0.9500 . ?
C36 C38 1.393(4) . ?
C40 H40 0.9500 . ?
C40 C38 1.430(4) . ?
C40 C42 1.355(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C41 H41 0.9500 . ?
C41 C42 1.408(5) . ?
C41 C39 1.362(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C37 C38 1.426(4) . ?
C37 C39 1.427(4) . ?
C37 C35 1.395(4) . ?
C27 C29 1.364(4) . ?
C27 C25 1.520(4) . ?
C10 C7 1.401(4) . ?
C10 C9 1.432(4) . ?
C42 H42 0.9500 . ?
C7 H7 0.9500 . ?
C7 C6 1.397(4) . ?
C39 H39 0.9500 . ?
C6 C3 1.431(4) . ?
C6 C5 1.428(4) . ?
C35 H35 0.9500 . ?
C35 C33 1.395(4) . ?
C3 H3 0.9500 . ?
C3 C2 1.355(5) . ?
C29 C33 1.434(4) . ?
C2 H2 0.9500 . ?
C2 C1 1.420(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C1 H1 0.9500 . ?
C1 C4 1.363(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C4 H4 0.9500 . ?
C4 C5 1.421(4) . ?
C5 C8 1.395(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C8 H8 0.9500 . ?
C8 C9 1.392(4) . ?
C9 C12 1.430(4) . ?
C12 C15 1.365(4) . ?
C15 C17 1.518(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
N7 C65 1.520(6) . ?
N7 C64 1.316(7) . ?
N7 C67 1.365(7) . ?
C65 C65 1.170(12) 2_675 ?
C65 C66 1.330(7) 2_675 ?
C65 C66 1.358(7) . ?
C71 C68 1.655(9) . ?
C71 C70 1.620(10) . ?
C66 C64 1.513(7) 2_675 ?
C66 C68 1.465(8) . ?
C66 C67 1.505(7) . ?
C66 C70 1.510(8) . ?
C64 C70 1.689(10) 2_675 ?
C68 C69 1.624(10) . ?
C68 C67 1.613(10) . ?
C69 C70 1.578(10) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C63 H63D 0.9800 . ?
C63 H63E 0.9800 . ?
C63 H63F 0.9800 . ?
C63 C59 1.454(9) . ?
C63 C60 1.495(9) . ?
C57 C56 1.512(8) . ?
C57 C59 1.467(9) . ?
C57 C53 1.344(9) . ?
C57 C54 1.330(7) . ?
C57 C58 1.443(8) . ?
C57 C60 1.509(8) . ?
C49 C47 1.652(10) . ?
C49 C48 1.216(9) . ?
C49 C53 1.485(8) . ?
C49 C46 1.618(10) . ?
C49 C54 1.437(8) . ?
C49 C51 1.298(8) . ?
N6 H6A 0.9019 . ?
N6 H6B 0.9029 . ?
N6 C53 1.360(10) . ?
C56 H56 0.9500 . ?
C56 C55 1.346(12) . ?
C59 H59 1.0000 . ?
C59 C62 1.512(13) . ?
C47 H47 1.0000 . ?
C47 C43 1.540(11) . ?
C47 C50 1.511(11) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C55 H55 0.9500 . ?
C55 C48 1.409(12) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C48 H48 0.9500 . ?
N5 H5A 0.8969 . ?
N5 H5B 0.8934 . ?
N5 C54 1.413(10) . ?
C46 H46 1.0000 . ?
C46 C44 1.403(14) . ?
C46 C45 1.532(13) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C51 H51 0.9500 . ?
C51 C52 1.361(11) . ?
C52 H52 0.9500 . ?
C52 C58 1.380(11) . ?
C58 H58 0.9500 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C61 C60 1.433(12) . ?
C60 H60 1.0000 . ?

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
C29 O1 C31 114.0(2) . . ?
C12 O5 C14 112.9(2) . . ?
C11 O6 C13 115.1(2) . . ?
C30 O2 C32 113.8(3) . . ?
C21 N1 C20 112.7(2) . . ?
C21 N1 C17 124.0(3) . . ?
C17 N1 C20 122.7(2) . . ?
C23 N4 C26 123.5(2) . . ?
C22 N4 C23 113.7(2) . . ?
C22 N4 C26 122.0(2) . . ?
C23 N3 C25 121.8(2) . . ?
C21 N3 C23 112.6(2) . . ?
C21 N3 C25 122.9(2) . . ?
C22 N2 C18 121.4(2) . . ?
C22 N2 C20 112.6(2) . . ?
C20 N2 C18 122.2(2) . . ?
N4 C23 N3 111.9(2) . . ?
N4 C23 C24 111.3(2) . . ?
N4 C23 C20 102.4(2) . . ?
N3 C23 C24 112.0(2) . . ?
N3 C23 C20 102.9(2) . . ?
C24 C23 C20 115.8(2) . . ?
C36 C34 C30 122.2(3) . . ?
C36 C34 C33 119.6(3) . . ?
C33 C34 C30 118.2(3) . . ?
C30 C28 C26 118.8(3) . . ?
C30 C28 C27 119.8(3) . . ?
C27 C28 C26 121.3(2) . . ?
O3 C22 N4 125.8(3) . . ?
O3 C22 N2 126.4(3) . . ?
N4 C22 N2 107.6(2) . . ?
O4 C21 N1 125.4(3) . . ?
O4 C21 N3 126.0(3) . . ?
N3 C21 N1 108.6(2) . . ?
O2 C32 H32A 109.5 . . ?
O2 C32 H32B 109.5 . . ?
O2 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C18 H18A 108.4 . . ?
N2 C18 H18B 108.4 . . ?
N2 C18 C16 115.5(2) . . ?
H18A C18 H18B 107.5 . . ?
C16 C18 H18A 108.4 . . ?
C16 C18 H18B 108.4 . . ?
N1 C20 C23 102.8(2) . . ?
N1 C20 C19 111.0(2) . . ?
N2 C20 N1 112.0(2) . . ?
N2 C20 C23 102.8(2) . . ?
N2 C20 C19 112.0(2) . . ?
C19 C20 C23 115.7(2) . . ?
C11 C16 C18 119.5(2) . . ?
C11 C16 C15 119.8(3) . . ?
C15 C16 C18 120.6(2) . . ?
O6 C11 C10 117.2(2) . . ?
C16 C11 O6 120.6(3) . . ?
C16 C11 C10 121.9(2) . . ?
C34 C36 H36 119.2 . . ?
C34 C36 C38 121.6(3) . . ?
C38 C36 H36 119.2 . . ?
C38 C40 H40 119.6 . . ?
C42 C40 H40 119.6 . . ?
C42 C40 C38 120.7(3) . . ?
O6 C13 H13A 109.5 . . ?
O6 C13 H13B 109.5 . . ?
O6 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C42 C41 H41 119.5 . . ?
C39 C41 H41 119.5 . . ?
C39 C41 C42 121.1(3) . . ?
N4 C26 C28 115.3(2) . . ?
N4 C26 H26A 108.5 . . ?
N4 C26 H26B 108.5 . . ?
C28 C26 H26A 108.5 . . ?
C28 C26 H26B 108.5 . . ?
H26A C26 H26B 107.5 . . ?
C38 C37 C39 118.2(3) . . ?
C35 C37 C38 119.4(3) . . ?
C35 C37 C39 122.3(3) . . ?
O2 C30 C34 117.2(3) . . ?
C28 C30 O2 120.7(3) . . ?
C28 C30 C34 122.1(3) . . ?
C28 C27 C25 121.6(2) . . ?
C29 C27 C28 119.4(3) . . ?
C29 C27 C25 118.9(2) . . ?
C36 C38 C40 121.9(3) . . ?
C36 C38 C37 119.1(3) . . ?
C37 C38 C40 119.0(3) . . ?
C11 C10 C9 118.1(2) . . ?
C7 C10 C11 122.8(2) . . ?
C7 C10 C9 119.1(3) . . ?
C40 C42 C41 120.3(3) . . ?
C40 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
C10 C7 H7 119.4 . . ?
C6 C7 C10 121.2(3) . . ?
C6 C7 H7 119.4 . . ?
C41 C39 C37 120.7(3) . . ?
C41 C39 H39 119.7 . . ?
C37 C39 H39 119.7 . . ?
C7 C6 C3 122.0(3) . . ?
C7 C6 C5 119.6(3) . . ?
C5 C6 C3 118.4(3) . . ?
C37 C35 H35 119.2 . . ?
C37 C35 C33 121.6(3) . . ?
C33 C35 H35 119.2 . . ?
C6 C3 H3 119.7 . . ?
C2 C3 C6 120.6(3) . . ?
C2 C3 H3 119.7 . . ?
O1 C29 C33 117.1(2) . . ?
C27 C29 O1 120.7(3) . . ?
C27 C29 C33 122.1(3) . . ?
C3 C2 H2 119.5 . . ?
C3 C2 C1 121.1(3) . . ?
C1 C2 H2 119.5 . . ?
N3 C25 C27 116.0(2) . . ?
N3 C25 H25A 108.3 . . ?
N3 C25 H25B 108.3 . . ?
C27 C25 H25A 108.3 . . ?
C27 C25 H25B 108.3 . . ?
H25A C25 H25B 107.4 . . ?
C2 C1 H1 120.0 . . ?
C4 C1 C2 119.9(3) . . ?
C4 C1 H1 120.0 . . ?
O1 C31 H31A 109.5 . . ?
O1 C31 H31B 109.5 . . ?
O1 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C1 C4 H4 119.6 . . ?
C1 C4 C5 120.8(3) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 119.1(3) . . ?
C8 C5 C6 118.9(3) . . ?
C8 C5 C4 122.0(3) . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C5 C8 H8 119.1 . . ?
C9 C8 C5 121.8(3) . . ?
C9 C8 H8 119.1 . . ?
C8 C9 C10 119.2(3) . . ?
C8 C9 C12 122.3(3) . . ?
C12 C9 C10 118.5(3) . . ?
O5 C12 C9 117.2(3) . . ?
C15 C12 O5 120.7(2) . . ?
C15 C12 C9 122.1(3) . . ?
C16 C15 C17 121.1(3) . . ?
C12 C15 C16 119.5(2) . . ?
C12 C15 C17 119.3(2) . . ?
N1 C17 C15 114.4(2) . . ?
N1 C17 H17A 108.7 . . ?
N1 C17 H17B 108.7 . . ?
C15 C17 H17A 108.7 . . ?
C15 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
C34 C33 C29 118.3(3) . . ?
C35 C33 C34 118.7(3) . . ?
C35 C33 C29 123.0(3) . . ?
C64 N7 C65 62.8(4) . . ?
C64 N7 C67 127.2(5) . . ?
C67 N7 C65 64.3(4) . . ?
C65 C65 N7 177.2(10) 2_675 . ?
C65 C65 C66 65.5(6) 2_675 2_675 ?
C65 C65 C66 62.9(6) 2_675 . ?
C66 C65 N7 116.5(5) 2_675 . ?
C66 C65 N7 115.1(5) . . ?
C66 C65 C66 128.4(5) 2_675 . ?
C70 C71 C68 42.5(4) . . ?
C65 C66 C65 51.6(5) 2_675 . ?
C65 C66 C64 114.4(4) . 2_675 ?
C65 C66 C64 62.8(4) 2_675 2_675 ?
C65 C66 C68 130.5(5) . . ?
C65 C66 C68 177.1(5) 2_675 . ?
C65 C66 C67 116.5(4) 2_675 . ?
C65 C66 C67 64.9(4) . . ?
C65 C66 C70 130.7(5) 2_675 . ?
C65 C66 C70 177.3(5) . . ?
C68 C66 C64 115.0(5) . 2_675 ?
C68 C66 C67 65.8(4) . . ?
C68 C66 C70 47.1(4) . . ?
C67 C66 C64 178.9(4) . 2_675 ?
C67 C66 C70 112.8(4) . . ?
C70 C66 C64 68.0(4) . 2_675 ?
N7 C64 C66 117.9(5) . 2_675 ?
N7 C64 C70 173.5(6) . 2_675 ?
C66 C64 C70 56.0(3) 2_675 2_675 ?
C66 C68 C71 107.1(5) . . ?
C66 C68 C69 110.2(5) . . ?
C66 C68 C67 58.3(4) . . ?
C69 C68 C71 100.7(6) . . ?
C67 C68 C71 129.5(7) . . ?
C67 C68 C69 129.7(6) . . ?
C70 C69 C68 43.5(4) . . ?
N7 C67 C66 115.7(5) . . ?
N7 C67 C68 171.3(6) . . ?
C66 C67 C68 55.9(4) . . ?
C71 C70 C64 124.4(6) . 2_675 ?
C66 C70 C71 106.6(6) . . ?
C66 C70 C64 56.1(4) . 2_675 ?
C66 C70 C69 110.3(5) . . ?
C69 C70 C71 104.3(5) . . ?
C69 C70 C64 131.2(6) . 2_675 ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
H63D C63 H63E 109.5 . . ?
H63D C63 H63F 109.5 . . ?
H63E C63 H63F 109.5 . . ?
C59 C63 H63A 109.5 . . ?
C59 C63 H63B 109.5 . . ?
C59 C63 H63C 109.5 . . ?
C60 C63 H63D 109.5 . . ?
C60 C63 H63E 109.5 . . ?
C60 C63 H63F 109.5 . . ?
C59 C57 C56 115.3(6) . . ?
C53 C57 C56 113.0(5) . . ?
C53 C57 C59 131.2(6) . . ?
C54 C57 C58 113.9(5) . . ?
C54 C57 C60 128.6(5) . . ?
C58 C57 C60 117.4(5) . . ?
C48 C49 C47 122.9(7) . . ?
C48 C49 C53 127.7(7) . . ?
C53 C49 C47 105.7(5) . . ?
C54 C49 C46 112.9(6) . . ?
C51 C49 C46 119.9(6) . . ?
C51 C49 C54 120.6(6) . . ?
H6A N6 H6B 107.3 . . ?
C53 N6 H6A 111.1 . . ?
C53 N6 H6B 110.6 . . ?
C57 C56 H56 118.4 . . ?
C55 C56 C57 123.2(8) . . ?
C55 C56 H56 118.4 . . ?
C63 C59 C57 120.3(7) . . ?
C63 C59 H59 103.1 . . ?
C63 C59 C62 107.4(8) . . ?
C57 C59 H59 103.1 . . ?
C57 C59 C62 117.2(8) . . ?
C62 C59 H59 103.1 . . ?
C49 C47 H47 109.2 . . ?
C43 C47 C49 108.4(7) . . ?
C43 C47 H47 109.2 . . ?
C50 C47 C49 110.1(8) . . ?
C50 C47 H47 109.2 . . ?
C50 C47 C43 110.9(8) . . ?
C47 C43 H43A 109.5 . . ?
C47 C43 H43B 109.5 . . ?
C47 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C59 C62 H62A 109.5 . . ?
C59 C62 H62B 109.5 . . ?
C59 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C56 C55 H55 120.0 . . ?
C56 C55 C48 120.0(9) . . ?
C48 C55 H55 120.0 . . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C48 C55 116.6(9) . . ?
C49 C48 H48 121.7 . . ?
C55 C48 H48 121.7 . . ?
C57 C53 C49 117.7(6) . . ?
C57 C53 N6 114.3(7) . . ?
N6 C53 C49 127.7(7) . . ?
H5A N5 H5B 107.3 . . ?
C54 N5 H5A 112.6 . . ?
C54 N5 H5B 109.2 . . ?
C49 C46 H46 110.4 . . ?
C44 C46 C49 110.0(10) . . ?
C44 C46 H46 110.4 . . ?
C44 C46 C45 103.4(12) . . ?
C45 C46 C49 112.0(9) . . ?
C45 C46 H46 110.4 . . ?
C46 C44 H44A 109.5 . . ?
C46 C44 H44B 109.5 . . ?
C46 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C57 C54 C49 122.1(5) . . ?
C57 C54 N5 110.8(6) . . ?
N5 C54 C49 126.1(6) . . ?
C49 C51 H51 120.4 . . ?
C49 C51 C52 119.2(8) . . ?
C52 C51 H51 120.4 . . ?
C51 C52 H52 119.6 . . ?
C51 C52 C58 120.7(8) . . ?
C58 C52 H52 119.6 . . ?
C57 C58 H58 119.3 . . ?
C52 C58 C57 121.3(8) . . ?
C52 C58 H58 119.3 . . ?
C46 C45 H45A 109.5 . . ?
C46 C45 H45B 109.5 . . ?
C46 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
C63 C60 C57 115.1(6) . . ?
C63 C60 H60 103.8 . . ?
C57 C60 H60 103.8 . . ?
C61 C60 C63 115.4(8) . . ?
C61 C60 C57 113.1(8) . . ?
C61 C60 H60 103.8 . . ?

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

data_190522lyz_0m
_database_code_depnum_ccdc_archive 'CCDC 1960293'
loop_
_audit_author_name
_audit_author_address
'Yuezhou Liu'
;Zhejiang University
China
;
_audit_update_record             
;
2019-10-19 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_audit_creation_date             2019-05-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 F6, C42 H38 N4 O6'
_chemical_formula_sum            'C48 H38 F6 N4 O6'
_chemical_formula_weight         880.82
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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'
F F 0.0599 0.0411 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   16.0417(3)
_cell_length_b                   18.6338(3)
_cell_length_c                   13.7075(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.4420(10)
_cell_angle_gamma                90
_cell_volume                     4041.90(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.992
_cell_measurement_theta_min      3.19
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.940
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1220 before and 0.0523 after correction. The Ratio of minimum to maximum transmission is 0.6297. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21172
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.967
_diffrn_reflns_theta_min         3.188
_diffrn_ambient_temperature      170.02
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3182
_reflns_number_total             3806
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3806
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0520
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0671P)²+3.6579P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1473
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.56649(13) -0.03786(13) 0.68604(16) 0.1202(7) Uani 1 1 d . . . . .
F2 F 0.60372(12) 0.09172(12) 0.61619(16) 0.1152(7) Uani 1 1 d . . . . .
F3 F 0.53753(14) 0.12971(13) 0.42947(17) 0.1214(7) Uani 1 1 d . . . . .
C22 C 0.53358(18) -0.0192(2) 0.5931(2) 0.0909(10) Uani 1 1 d . . . . .
C23 C 0.55291(18) 0.0467(2) 0.5588(3) 0.0899(10) Uani 1 1 d . . . . .
C24 C 0.5184(2) 0.0658(2) 0.4645(3) 0.0942(10) Uani 1 1 d . . . . .
O1 O 0.39237(8) 0.36367(7) 0.06701(9) 0.0490(4) Uani 1 1 d . . . . .
O2 O 0.25847(9) 0.25049(8) 0.23202(11) 0.0618(4) Uani 1 1 d . . . . .
O3 O 0.45573(9) 0.31440(7) 0.59426(9) 0.0507(4) Uani 1 1 d . . . . .
N1 N 0.50187(10) 0.44137(8) 0.12508(11) 0.0430(4) Uani 1 1 d . . . . .
N2 N 0.40607(10) 0.41726(8) 0.22043(11) 0.0424(4) Uani 1 1 d . . . . .
C1 C 0.42971(12) 0.40264(9) 0.13146(13) 0.0415(4) Uani 1 1 d . . . . .
C2 C 0.46186(12) 0.46960(9) 0.27827(13) 0.0443(4) Uani 1 1 d . . . . .
C3 C 0.41890(15) 0.54158(10) 0.28481(16) 0.0585(6) Uani 1 1 d . . . . .
H3A H 0.457056 0.573921 0.327328 0.088 Uiso 1 1 calc GR . . . .
H3B H 0.367020 0.534864 0.312804 0.088 Uiso 1 1 calc GR . . . .
H3C H 0.404886 0.562450 0.218520 0.088 Uiso 1 1 calc GR . . . .
C4 C 0.55595(13) 0.42059(10) 0.05427(14) 0.0472(5) Uani 1 1 d . . . . .
H4A H 0.600170 0.457700 0.054649 0.057 Uiso 1 1 calc R . . . .
H4B H 0.521480 0.420273 -0.012614 0.057 Uiso 1 1 calc R . . . .
C5 C 0.33205(12) 0.38825(10) 0.25339(14) 0.0463(5) Uani 1 1 d . . . . .
H5A H 0.295068 0.366917 0.195765 0.056 Uiso 1 1 calc R . . . .
H5B H 0.300518 0.428255 0.277906 0.056 Uiso 1 1 calc R . . . .
C6 C 0.34926(11) 0.33206(10) 0.33370(13) 0.0423(4) Uani 1 1 d . . . . .
C7 C 0.31136(11) 0.26625(10) 0.31951(15) 0.0461(5) Uani 1 1 d . . . . .
C8 C 0.31917(11) 0.21355(10) 0.39614(15) 0.0458(5) Uani 1 1 d . . . . .
C9 C 0.27897(12) 0.14679(11) 0.38316(17) 0.0527(5) Uani 1 1 d . . . . .
H9 H 0.245809 0.135535 0.321086 0.063 Uiso 1 1 calc R . . . .
C10 C 0.28648(12) 0.09654(11) 0.45908(18) 0.0523(5) Uani 1 1 d . . . . .
C11 C 0.24920(13) 0.02669(12) 0.4467(2) 0.0632(6) Uani 1 1 d . . . . .
H11 H 0.217480 0.013752 0.384449 0.076 Uiso 1 1 calc R . . . .
C12 C 0.25815(13) -0.02116(12) 0.5215(2) 0.0656(6) Uani 1 1 d . . . . .
H12 H 0.232936 -0.067252 0.511109 0.079 Uiso 1 1 calc R . . . .
C13 C 0.30461(14) -0.00348(12) 0.6150(2) 0.0618(6) Uani 1 1 d . . . . .
H13 H 0.310546 -0.037635 0.667132 0.074 Uiso 1 1 calc R . . . .
C14 C 0.34097(13) 0.06262(12) 0.63057(18) 0.0568(5) Uani 1 1 d . . . . .
H14 H 0.371700 0.074264 0.693868 0.068 Uiso 1 1 calc R . . . .
C15 C 0.33349(12) 0.11418(11) 0.55348(16) 0.0492(5) Uani 1 1 d . . . . .
C16 C 0.37214(12) 0.18166(11) 0.56728(15) 0.0485(5) Uani 1 1 d . . . . .
H16 H 0.401951 0.194222 0.630688 0.058 Uiso 1 1 calc R . . . .
C17 C 0.36774(11) 0.23055(10) 0.49020(14) 0.0435(4) Uani 1 1 d . . . . .
C18 C 0.40959(12) 0.29868(10) 0.50210(14) 0.0439(4) Uani 1 1 d . . . . .
C19 C 0.40122(12) 0.34823(10) 0.42765(14) 0.0429(4) Uani 1 1 d . . . . .
C20 C 0.53851(14) 0.28090(11) 0.61373(16) 0.0560(5) Uani 1 1 d . . . . .
H20A H 0.575211 0.302673 0.571372 0.084 Uiso 1 1 calc GR . . . .
H20B H 0.532921 0.229402 0.599667 0.084 Uiso 1 1 calc GR . . . .
H20C H 0.563288 0.288017 0.683293 0.084 Uiso 1 1 calc GR . . . .
C21 C 0.30134(18) 0.21620(14) 0.16056(18) 0.0746(7) Uani 1 1 d . . . . .
H21A H 0.259738 0.199308 0.104853 0.112 Uiso 1 1 calc GR . . . .
H21B H 0.333953 0.175310 0.191390 0.112 Uiso 1 1 calc GR . . . .
H21C H 0.339594 0.250592 0.136660 0.112 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C22 1.343(4) . ?
F2 C23 1.333(3) . ?
F3 C24 1.339(4) . ?
C22 C23 1.368(5) . ?
C22 C24 1.363(4) 5_656 ?
C23 C24 1.366(5) . ?
O1 C1 1.222(2) . ?
O2 C7 1.382(2) . ?
O2 C21 1.436(3) . ?
O3 C18 1.387(2) . ?
O3 C20 1.452(3) . ?
N1 C1 1.379(2) . ?
N1 C2 1.455(2) 2_655 ?
N1 C4 1.456(3) . ?
N2 C1 1.363(2) . ?
N2 C2 1.466(2) . ?
N2 C5 1.443(3) . ?
C2 C2 1.552(4) 2_655 ?
C2 C3 1.517(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C19 1.515(3) 2_655 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.512(3) . ?
C6 C7 1.368(3) . ?
C6 C19 1.446(2) . ?
C7 C8 1.428(3) . ?
C8 C9 1.399(3) . ?
C8 C17 1.428(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.390(3) . ?
C10 C11 1.431(3) . ?
C10 C15 1.425(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.348(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.412(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.365(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.419(3) . ?
C15 C16 1.401(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.388(3) . ?
C17 C18 1.433(3) . ?
C18 C19 1.366(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 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
F1 C22 C23 118.9(3) . . ?
F1 C22 C24 119.5(4) . 5_656 ?
C24 C22 C23 121.6(4) 5_656 . ?
F2 C23 C22 120.8(3) . . ?
F2 C23 C24 120.6(4) . . ?
C24 C23 C22 118.6(3) . . ?
F3 C24 C22 120.9(4) . 5_656 ?
F3 C24 C23 119.3(3) . . ?
C22 C24 C23 119.8(4) 5_656 . ?
C7 O2 C21 113.07(16) . . ?
C18 O3 C20 114.33(14) . . ?
C1 N1 C2 110.24(15) . 2_655 ?
C1 N1 C4 120.07(15) . . ?
C2 N1 C4 120.66(15) 2_655 . ?
C1 N2 C2 112.48(16) . . ?
C1 N2 C5 124.70(15) . . ?
C5 N2 C2 122.73(15) . . ?
O1 C1 N1 125.61(18) . . ?
O1 C1 N2 126.20(18) . . ?
N2 C1 N1 108.16(15) . . ?
N1 C2 N2 111.68(14) 2_655 . ?
N1 C2 C2 102.96(16) 2_655 2_655 ?
N1 C2 C3 112.55(15) 2_655 . ?
N2 C2 C2 101.03(14) . 2_655 ?
N2 C2 C3 112.17(15) . . ?
C3 C2 C2 115.62(13) . 2_655 ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 108.4 . . ?
N1 C4 H4B 108.4 . . ?
N1 C4 C19 115.55(15) . 2_655 ?
H4A C4 H4B 107.5 . . ?
C19 C4 H4A 108.4 2_655 . ?
C19 C4 H4B 108.4 2_655 . ?
N2 C5 H5A 108.5 . . ?
N2 C5 H5B 108.5 . . ?
N2 C5 C6 115.22(15) . . ?
H5A C5 H5B 107.5 . . ?
C6 C5 H5A 108.5 . . ?
C6 C5 H5B 108.5 . . ?
C7 C6 C5 119.57(16) . . ?
C7 C6 C19 119.40(18) . . ?
C19 C6 C5 120.93(16) . . ?
O2 C7 C8 117.34(17) . . ?
C6 C7 O2 120.59(19) . . ?
C6 C7 C8 121.89(17) . . ?
C9 C8 C7 122.33(18) . . ?
C9 C8 C17 118.93(19) . . ?
C17 C8 C7 118.71(17) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 C8 121.48(19) . . ?
C10 C9 H9 119.3 . . ?
C9 C10 C11 122.7(2) . . ?
C9 C10 C15 119.49(18) . . ?
C15 C10 C11 117.8(2) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 C10 121.4(2) . . ?
C12 C11 H11 119.3 . . ?
C11 C12 H12 119.7 . . ?
C11 C12 C13 120.7(2) . . ?
C13 C12 H12 119.7 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.1(2) . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 119.6 . . ?
C13 C14 C15 120.9(2) . . ?
C15 C14 H14 119.6 . . ?
C14 C15 C10 119.19(18) . . ?
C16 C15 C10 119.1(2) . . ?
C16 C15 C14 121.7(2) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 C15 121.34(19) . . ?
C17 C16 H16 119.3 . . ?
C8 C17 C18 118.38(18) . . ?
C16 C17 C8 119.58(17) . . ?
C16 C17 C18 122.03(17) . . ?
O3 C18 C17 117.45(17) . . ?
C19 C18 O3 120.67(16) . . ?
C19 C18 C17 121.79(17) . . ?
C6 C19 C4 120.70(17) . 2_655 ?
C18 C19 C4 119.53(16) . 2_655 ?
C18 C19 C6 119.73(17) . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 C21 H21A 109.5 . . ?
O2 C21 H21B 109.5 . . ?
O2 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?

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

data_190618lyz_1_0m
_database_code_depnum_ccdc_archive 'CCDC 1960294'
loop_
_audit_author_name
_audit_author_address
'Yuezhou Liu'
;Zhejiang University
China
;
_audit_update_record             
;
2019-10-19 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_audit_creation_date             2019-06-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H38 N4 O6, C9 H11 N O2'
_chemical_formula_sum            'C51 H49 N5 O8'
_chemical_formula_weight         859.95
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.6881(3)
_cell_length_b                   14.5217(4)
_cell_length_c                   16.4855(5)
_cell_angle_alpha                111.189(2)
_cell_angle_beta                 91.323(2)
_cell_angle_gamma                101.864(2)
_cell_volume                     2321.42(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.987
_cell_measurement_theta_min      2.918
_shelx_estimated_absorpt_T_max   0.991
_shelx_estimated_absorpt_T_min   0.978
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1214 before and 0.0689 after correction. The Ratio of minimum to maximum transmission is 0.7363. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28109
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.970
_diffrn_reflns_theta_min         2.917
_diffrn_ambient_temperature      169.97
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5928
_reflns_number_total             8695
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         8695
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0652
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0985P)²+1.4224P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1724
_refine_ls_wR_factor_ref         0.2005
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Rotating group:
 N5(H5D,H5E)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C22(H22A,H22B), C25(H25A,H25B), C40(H40A,H40B), C50(H50A,H50B)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C29(H29),
 C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C44(H44), C45(H45), C46(H46),
  C47(H47)
2.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C51(H51A,H51B,H51C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.28080(17) 0.41076(15) 0.08296(13) 0.0374(5) Uani 1 1 d . . . . .
O2 O 0.60355(18) 0.16815(15) 0.14085(13) 0.0380(5) Uani 1 1 d . . . . .
O3 O 0.80037(17) 0.36218(14) 0.31415(13) 0.0377(5) Uani 1 1 d . . . . .
O4 O 0.48137(18) 0.61492(14) 0.30007(13) 0.0399(5) Uani 1 1 d . . . . .
O5 O 0.00132(17) 0.24125(14) 0.07507(12) 0.0342(4) Uani 1 1 d . . . . .
O6 O 0.27791(17) -0.01258(14) 0.14376(13) 0.0367(5) Uani 1 1 d . . . . .
N1 N 0.3373(2) 0.26663(17) -0.01049(14) 0.0310(5) Uani 1 1 d . . . . .
N2 N 0.4914(2) 0.39556(17) 0.07570(15) 0.0337(5) Uani 1 1 d . . . . .
N3 N 0.6382(2) 0.29070(17) 0.07977(14) 0.0316(5) Uani 1 1 d . . . . .
N4 N 0.4618(2) 0.16690(17) 0.03222(14) 0.0314(5) Uani 1 1 d . . . . .
C1 C 0.3619(2) 0.3627(2) 0.05351(17) 0.0306(6) Uani 1 1 d . . . . .
C2 C 0.5700(2) 0.2052(2) 0.09035(17) 0.0317(6) Uani 1 1 d . . . . .
C3 C 0.5625(2) 0.3223(2) 0.02455(18) 0.0327(6) Uani 1 1 d . . . . .
C4 C 0.4523(2) 0.2261(2) -0.02160(17) 0.0308(6) Uani 1 1 d . . . . .
C5 C 0.6436(3) 0.3624(3) -0.0352(2) 0.0460(8) Uani 1 1 d . . . . .
H5A H 0.587794 0.376853 -0.074914 0.069 Uiso 1 1 calc GR . . . .
H5B H 0.688993 0.311414 -0.069451 0.069 Uiso 1 1 calc GR . . . .
H5C H 0.706290 0.424818 0.000110 0.069 Uiso 1 1 calc GR . . . .
C6 C 0.4637(3) 0.1658(3) -0.1169(2) 0.0469(8) Uani 1 1 d . . . . .
H6A H 0.391578 0.106262 -0.139528 0.070 Uiso 1 1 calc GR . . . .
H6B H 0.544828 0.143630 -0.121530 0.070 Uiso 1 1 calc GR . . . .
H6C H 0.462143 0.208505 -0.151117 0.070 Uiso 1 1 calc GR . . . .
C7 C 0.2093(2) 0.1993(2) -0.02441(18) 0.0338(6) Uani 1 1 d . . . . .
H7A H 0.202413 0.141758 -0.080942 0.041 Uiso 1 1 calc R . . . .
H7B H 0.144457 0.237117 -0.029821 0.041 Uiso 1 1 calc R . . . .
C8 C 0.1750(2) 0.1565(2) 0.04551(17) 0.0305(6) Uani 1 1 d . . . . .
C9 C 0.0679(2) 0.1738(2) 0.08710(18) 0.0316(6) Uani 1 1 d . . . . .
C10 C 0.0201(2) 0.1248(2) 0.14569(17) 0.0315(6) Uani 1 1 d . . . . .
C11 C -0.0931(2) 0.1369(2) 0.18412(18) 0.0348(6) Uani 1 1 d . . . . .
H11 H -0.138292 0.182762 0.174893 0.042 Uiso 1 1 calc R . . . .
C12 C -0.1416(2) 0.0830(2) 0.23594(18) 0.0343(6) Uani 1 1 d . . . . .
C13 C -0.2570(3) 0.0960(2) 0.2767(2) 0.0422(7) Uani 1 1 d . . . . .
H13 H -0.302267 0.142728 0.269192 0.051 Uiso 1 1 calc R . . . .
C14 C -0.3019(3) 0.0416(3) 0.3263(2) 0.0465(8) Uani 1 1 d . . . . .
H14 H -0.378505 0.050969 0.353066 0.056 Uiso 1 1 calc R . . . .
C15 C -0.2368(3) -0.0286(2) 0.3386(2) 0.0486(8) Uani 1 1 d . . . . .
H15 H -0.270016 -0.065773 0.373465 0.058 Uiso 1 1 calc R . . . .
C16 C -0.1274(3) -0.0432(2) 0.3011(2) 0.0430(7) Uani 1 1 d . . . . .
H16 H -0.085147 -0.091181 0.309315 0.052 Uiso 1 1 calc R . . . .
C17 C -0.0748(3) 0.0129(2) 0.24929(18) 0.0347(6) Uani 1 1 d . . . . .
C18 C 0.0415(3) 0.0036(2) 0.21305(18) 0.0357(6) Uani 1 1 d . . . . .
H18 H 0.087903 -0.040890 0.223601 0.043 Uiso 1 1 calc R . . . .
C19 C 0.0904(2) 0.0578(2) 0.16206(17) 0.0310(6) Uani 1 1 d . . . . .
C20 C 0.2090(2) 0.0491(2) 0.12349(18) 0.0327(6) Uani 1 1 d . . . . .
C21 C 0.2484(2) 0.0930(2) 0.06582(17) 0.0312(6) Uani 1 1 d . . . . .
C22 C 0.3686(2) 0.0741(2) 0.02200(19) 0.0337(6) Uani 1 1 d . . . . .
H22A H 0.409436 0.033505 0.047027 0.040 Uiso 1 1 calc R . . . .
H22B H 0.344080 0.033638 -0.041173 0.040 Uiso 1 1 calc R . . . .
C23 C -0.1006(3) 0.1952(2) 0.00548(19) 0.0405(7) Uani 1 1 d . . . . .
H23A H -0.067041 0.157833 -0.048453 0.061 Uiso 1 1 calc GR . . . .
H23B H -0.137427 0.247959 -0.003126 0.061 Uiso 1 1 calc GR . . . .
H23C H -0.167426 0.148366 0.020254 0.061 Uiso 1 1 calc GR . . . .
C24 C 0.3624(3) 0.0410(3) 0.2243(2) 0.0485(8) Uani 1 1 d . . . . .
H24A H 0.435671 0.087512 0.214709 0.073 Uiso 1 1 calc GR . . . .
H24B H 0.393417 -0.007935 0.242963 0.073 Uiso 1 1 calc GR . . . .
H24C H 0.315201 0.079684 0.269706 0.073 Uiso 1 1 calc GR . . . .
C25 C 0.5527(3) 0.4942(2) 0.14024(19) 0.0363(6) Uani 1 1 d . . . . .
H25A H 0.490728 0.538374 0.151280 0.044 Uiso 1 1 calc R . . . .
H25B H 0.626415 0.524940 0.115928 0.044 Uiso 1 1 calc R . . . .
C26 C 0.6005(2) 0.4917(2) 0.22664(19) 0.0333(6) Uani 1 1 d . . . . .
C27 C 0.5644(2) 0.5535(2) 0.30285(19) 0.0342(6) Uani 1 1 d . . . . .
C28 C 0.6059(2) 0.5561(2) 0.38640(19) 0.0328(6) Uani 1 1 d . . . . .
C29 C 0.5668(3) 0.6172(2) 0.46390(19) 0.0362(6) Uani 1 1 d . . . . .
H29 H 0.509017 0.657919 0.460985 0.043 Uiso 1 1 calc R . . . .
C30 C 0.6100(3) 0.6200(2) 0.54538(19) 0.0348(6) Uani 1 1 d . . . . .
C31 C 0.5747(3) 0.6842(2) 0.6249(2) 0.0419(7) Uani 1 1 d . . . . .
H31 H 0.518261 0.726432 0.623515 0.050 Uiso 1 1 calc R . . . .
C32 C 0.6207(3) 0.6860(2) 0.7031(2) 0.0464(8) Uani 1 1 d . . . . .
H32 H 0.595892 0.729343 0.755650 0.056 Uiso 1 1 calc R . . . .
C33 C 0.7052(3) 0.6240(3) 0.7074(2) 0.0478(8) Uani 1 1 d . . . . .
H33 H 0.737663 0.626914 0.762648 0.057 Uiso 1 1 calc R . . . .
C34 C 0.7397(3) 0.5608(2) 0.6331(2) 0.0425(7) Uani 1 1 d . . . . .
H34 H 0.795138 0.518592 0.636544 0.051 Uiso 1 1 calc R . . . .
C35 C 0.6939(3) 0.5567(2) 0.54933(19) 0.0366(6) Uani 1 1 d . . . . .
C36 C 0.7301(3) 0.4923(2) 0.47088(19) 0.0363(6) Uani 1 1 d . . . . .
H36 H 0.783893 0.448652 0.473441 0.044 Uiso 1 1 calc R . . . .
C37 C 0.6889(2) 0.4915(2) 0.39021(18) 0.0330(6) Uani 1 1 d . . . . .
C38 C 0.7259(2) 0.4278(2) 0.30965(19) 0.0327(6) Uani 1 1 d . . . . .
C39 C 0.6852(2) 0.4277(2) 0.23025(18) 0.0309(6) Uani 1 1 d . . . . .
C40 C 0.7358(2) 0.3649(2) 0.14890(18) 0.0345(6) Uani 1 1 d . . . . .
H40A H 0.788016 0.411361 0.124550 0.041 Uiso 1 1 calc R . . . .
H40B H 0.793777 0.328252 0.165880 0.041 Uiso 1 1 calc R . . . .
C41 C 0.9362(3) 0.4044(3) 0.3270(2) 0.0475(8) Uani 1 1 d . . . . .
H41A H 0.962354 0.423058 0.277441 0.071 Uiso 1 1 calc GR . . . .
H41B H 0.981859 0.354012 0.331372 0.071 Uiso 1 1 calc GR . . . .
H41C H 0.957294 0.464832 0.381132 0.071 Uiso 1 1 calc GR . . . .
C42 C 0.5472(3) 0.7133(2) 0.3051(2) 0.0480(8) Uani 1 1 d . . . . .
H42A H 0.592983 0.706865 0.253270 0.072 Uiso 1 1 calc GR . . . .
H42B H 0.608892 0.745538 0.357792 0.072 Uiso 1 1 calc GR . . . .
H42C H 0.484781 0.754953 0.307872 0.072 Uiso 1 1 calc GR . . . .
O7 O 0.1363(3) 0.64419(19) 0.39089(15) 0.0627(7) Uani 1 1 d . . . . .
O8 O -0.0329(2) 0.71391(19) 0.42064(15) 0.0623(7) Uani 1 1 d . . . . .
N5 N 0.1800(3) 0.5655(2) 0.22075(19) 0.0589(8) Uani 1 1 d . . . . .
H5D H 0.171962 0.548224 0.266787 0.071 Uiso 1 1 d GR . . . .
H5E H 0.187970 0.512496 0.175109 0.071 Uiso 1 1 d GR . . . .
C43 C 0.0736(3) 0.5970(2) 0.2058(2) 0.0407(7) Uani 1 1 d . . . . .
C44 C 0.0302(3) 0.5813(2) 0.1192(2) 0.0452(7) Uani 1 1 d . . . . .
H44 H 0.072373 0.544595 0.072304 0.054 Uiso 1 1 calc R . . . .
C45 C -0.0708(3) 0.6176(2) 0.1012(2) 0.0460(8) Uani 1 1 d . . . . .
H45 H -0.096175 0.607460 0.042456 0.055 Uiso 1 1 calc R . . . .
C46 C -0.1372(3) 0.6696(2) 0.1684(2) 0.0469(8) Uani 1 1 d . . . . .
H46 H -0.206670 0.695631 0.155858 0.056 Uiso 1 1 calc R . . . .
C47 C -0.1006(3) 0.6825(2) 0.2525(2) 0.0437(7) Uani 1 1 d . . . . .
H47 H -0.147850 0.715511 0.297901 0.052 Uiso 1 1 calc R . . . .
C48 C 0.0046(3) 0.6485(2) 0.27386(19) 0.0384(7) Uani 1 1 d . . . . .
C49 C 0.0442(3) 0.6674(2) 0.3655(2) 0.0479(8) Uani 1 1 d . . . . .
C50 C -0.0038(5) 0.7313(4) 0.5130(2) 0.0862(14) Uani 1 1 d . . . . .
H50A H 0.086830 0.768290 0.533474 0.103 Uiso 1 1 calc R . . . .
H50B H -0.017289 0.665857 0.521197 0.103 Uiso 1 1 calc R . . . .
C51 C -0.0909(5) 0.7918(4) 0.5625(3) 0.114(2) Uani 1 1 d . . . . .
H51A H -0.180095 0.753634 0.542870 0.171 Uiso 1 1 calc GR . . . .
H51B H -0.078149 0.855601 0.552699 0.171 Uiso 1 1 calc GR . . . .
H51C H -0.072468 0.806581 0.625046 0.171 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.223(3) . ?
O2 C2 1.225(3) . ?
O3 C38 1.381(3) . ?
O3 C41 1.433(3) . ?
O4 C27 1.393(3) . ?
O4 C42 1.428(4) . ?
O5 C9 1.388(3) . ?
O5 C23 1.428(3) . ?
O6 C20 1.390(3) . ?
O6 C24 1.446(3) . ?
N1 C1 1.379(3) . ?
N1 C4 1.457(3) . ?
N1 C7 1.467(3) . ?
N2 C1 1.363(3) . ?
N2 C3 1.461(3) . ?
N2 C25 1.447(4) . ?
N3 C2 1.376(4) . ?
N3 C3 1.454(3) . ?
N3 C40 1.464(3) . ?
N4 C2 1.366(3) . ?
N4 C4 1.456(3) . ?
N4 C22 1.454(4) . ?
C3 C4 1.559(4) . ?
C3 C5 1.519(4) . ?
C4 C6 1.519(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.514(4) . ?
C8 C9 1.369(4) . ?
C8 C21 1.445(3) . ?
C9 C10 1.438(4) . ?
C10 C11 1.392(4) . ?
C10 C19 1.437(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.396(4) . ?
C12 C13 1.433(4) . ?
C12 C17 1.430(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.359(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.415(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.355(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.431(4) . ?
C17 C18 1.402(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.390(4) . ?
C19 C20 1.439(4) . ?
C20 C21 1.354(4) . ?
C21 C22 1.514(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.517(4) . ?
C26 C27 1.371(4) . ?
C26 C39 1.440(3) . ?
C27 C28 1.422(4) . ?
C28 C29 1.397(4) . ?
C28 C37 1.434(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.394(4) . ?
C30 C31 1.419(4) . ?
C30 C35 1.427(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.358(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.417(4) . ?
C33 H33 0.9500 . ?
C33 C34 1.352(4) . ?
C34 H34 0.9500 . ?
C34 C35 1.431(4) . ?
C35 C36 1.412(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.386(4) . ?
C37 C38 1.436(4) . ?
C38 C39 1.369(4) . ?
C39 C40 1.508(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
O7 C49 1.215(4) . ?
O8 C49 1.335(4) . ?
O8 C50 1.466(5) . ?
N5 H5D 0.8823 . ?
N5 H5E 0.8819 . ?
N5 C43 1.358(4) . ?
C43 C44 1.413(4) . ?
C43 C48 1.421(4) . ?
C44 H44 0.9500 . ?
C44 C45 1.365(4) . ?
C45 H45 0.9500 . ?
C45 C46 1.398(4) . ?
C46 H46 0.9500 . ?
C46 C47 1.366(5) . ?
C47 H47 0.9500 . ?
C47 C48 1.403(4) . ?
C48 C49 1.469(4) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C51 1.468(7) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 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
C38 O3 C41 114.5(2) . . ?
C27 O4 C42 113.0(2) . . ?
C9 O5 C23 113.9(2) . . ?
C20 O6 C24 112.4(2) . . ?
C1 N1 C4 111.1(2) . . ?
C1 N1 C7 119.5(2) . . ?
C4 N1 C7 120.8(2) . . ?
C1 N2 C3 112.8(2) . . ?
C1 N2 C25 123.7(2) . . ?
C25 N2 C3 123.4(2) . . ?
C2 N3 C3 111.3(2) . . ?
C2 N3 C40 120.2(2) . . ?
C3 N3 C40 121.0(2) . . ?
C2 N4 C4 112.9(2) . . ?
C2 N4 C22 123.7(2) . . ?
C22 N4 C4 123.3(2) . . ?
O1 C1 N1 125.4(2) . . ?
O1 C1 N2 126.3(3) . . ?
N2 C1 N1 108.3(2) . . ?
O2 C2 N3 125.7(2) . . ?
O2 C2 N4 126.2(3) . . ?
N4 C2 N3 108.0(2) . . ?
N2 C3 C4 101.77(19) . . ?
N2 C3 C5 111.2(2) . . ?
N3 C3 N2 112.0(2) . . ?
N3 C3 C4 103.0(2) . . ?
N3 C3 C5 112.2(2) . . ?
C5 C3 C4 116.1(2) . . ?
N1 C4 C3 103.1(2) . . ?
N1 C4 C6 112.4(2) . . ?
N4 C4 N1 112.3(2) . . ?
N4 C4 C3 101.8(2) . . ?
N4 C4 C6 111.0(2) . . ?
C6 C4 C3 115.6(2) . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 H7A 108.2 . . ?
N1 C7 H7B 108.2 . . ?
N1 C7 C8 116.4(2) . . ?
H7A C7 H7B 107.3 . . ?
C8 C7 H7A 108.2 . . ?
C8 C7 H7B 108.2 . . ?
C9 C8 C7 119.3(2) . . ?
C9 C8 C21 119.1(2) . . ?
C21 C8 C7 121.5(2) . . ?
O5 C9 C10 116.9(2) . . ?
C8 C9 O5 120.8(2) . . ?
C8 C9 C10 122.2(2) . . ?
C11 C10 C9 122.8(2) . . ?
C11 C10 C19 119.2(3) . . ?
C19 C10 C9 118.0(2) . . ?
C10 C11 H11 119.3 . . ?
C10 C11 C12 121.4(2) . . ?
C12 C11 H11 119.3 . . ?
C11 C12 C13 121.7(3) . . ?
C11 C12 C17 119.6(2) . . ?
C17 C12 C13 118.7(3) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.1(3) . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 119.4 . . ?
C13 C14 C15 121.3(3) . . ?
C15 C14 H14 119.4 . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.5(3) . . ?
C16 C15 H15 119.8 . . ?
C15 C16 H16 119.7 . . ?
C15 C16 C17 120.7(3) . . ?
C17 C16 H16 119.7 . . ?
C12 C17 C16 118.8(3) . . ?
C18 C17 C12 118.9(3) . . ?
C18 C17 C16 122.3(3) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 C17 121.5(2) . . ?
C19 C18 H18 119.2 . . ?
C10 C19 C20 118.0(2) . . ?
C18 C19 C10 119.3(2) . . ?
C18 C19 C20 122.7(2) . . ?
O6 C20 C19 116.7(2) . . ?
C21 C20 O6 121.0(2) . . ?
C21 C20 C19 122.2(2) . . ?
C8 C21 C22 120.3(2) . . ?
C20 C21 C8 120.0(2) . . ?
C20 C21 C22 119.7(2) . . ?
N4 C22 C21 113.2(2) . . ?
N4 C22 H22A 108.9 . . ?
N4 C22 H22B 108.9 . . ?
C21 C22 H22A 108.9 . . ?
C21 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
O5 C23 H23A 109.5 . . ?
O5 C23 H23B 109.5 . . ?
O5 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O6 C24 H24A 109.5 . . ?
O6 C24 H24B 109.5 . . ?
O6 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2 C25 H25A 108.7 . . ?
N2 C25 H25B 108.7 . . ?
N2 C25 C26 114.1(2) . . ?
H25A C25 H25B 107.6 . . ?
C26 C25 H25A 108.7 . . ?
C26 C25 H25B 108.7 . . ?
C27 C26 C25 119.3(2) . . ?
C27 C26 C39 119.4(2) . . ?
C39 C26 C25 121.3(2) . . ?
O4 C27 C28 117.4(2) . . ?
C26 C27 O4 119.9(2) . . ?
C26 C27 C28 122.7(2) . . ?
C27 C28 C37 118.1(2) . . ?
C29 C28 C27 122.7(2) . . ?
C29 C28 C37 119.2(3) . . ?
C28 C29 H29 119.0 . . ?
C30 C29 C28 121.9(2) . . ?
C30 C29 H29 119.0 . . ?
C29 C30 C31 122.6(3) . . ?
C29 C30 C35 118.9(3) . . ?
C31 C30 C35 118.5(3) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 C30 120.8(3) . . ?
C32 C31 H31 119.6 . . ?
C31 C32 H32 119.5 . . ?
C31 C32 C33 121.0(3) . . ?
C33 C32 H32 119.5 . . ?
C32 C33 H33 119.9 . . ?
C34 C33 C32 120.1(3) . . ?
C34 C33 H33 119.9 . . ?
C33 C34 H34 119.6 . . ?
C33 C34 C35 120.8(3) . . ?
C35 C34 H34 119.6 . . ?
C30 C35 C34 118.8(3) . . ?
C36 C35 C30 119.3(3) . . ?
C36 C35 C34 121.9(3) . . ?
C35 C36 H36 119.3 . . ?
C37 C36 C35 121.4(2) . . ?
C37 C36 H36 119.3 . . ?
C28 C37 C38 118.4(2) . . ?
C36 C37 C28 119.2(3) . . ?
C36 C37 C38 122.5(2) . . ?
O3 C38 C37 117.6(2) . . ?
C39 C38 O3 120.3(2) . . ?
C39 C38 C37 122.1(2) . . ?
C26 C39 C40 121.3(2) . . ?
C38 C39 C26 119.3(2) . . ?
C38 C39 C40 119.3(2) . . ?
N3 C40 C39 115.7(2) . . ?
N3 C40 H40A 108.4 . . ?
N3 C40 H40B 108.4 . . ?
C39 C40 H40A 108.4 . . ?
C39 C40 H40B 108.4 . . ?
H40A C40 H40B 107.4 . . ?
O3 C41 H41A 109.5 . . ?
O3 C41 H41B 109.5 . . ?
O3 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O4 C42 H42A 109.5 . . ?
O4 C42 H42B 109.5 . . ?
O4 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C49 O8 C50 116.3(3) . . ?
H5D N5 H5E 109.0 . . ?
C43 N5 H5D 108.7 . . ?
C43 N5 H5E 110.3 . . ?
N5 C43 C44 119.4(3) . . ?
N5 C43 C48 123.1(3) . . ?
C44 C43 C48 117.5(3) . . ?
C43 C44 H44 119.2 . . ?
C45 C44 C43 121.7(3) . . ?
C45 C44 H44 119.2 . . ?
C44 C45 H45 119.7 . . ?
C44 C45 C46 120.7(3) . . ?
C46 C45 H45 119.7 . . ?
C45 C46 H46 120.5 . . ?
C47 C46 C45 119.0(3) . . ?
C47 C46 H46 120.5 . . ?
C46 C47 H47 119.0 . . ?
C46 C47 C48 122.0(3) . . ?
C48 C47 H47 119.0 . . ?
C43 C48 C49 120.5(3) . . ?
C47 C48 C43 119.1(3) . . ?
C47 C48 C49 120.4(3) . . ?
O7 C49 O8 121.8(3) . . ?
O7 C49 C48 125.4(3) . . ?
O8 C49 C48 112.7(3) . . ?
O8 C50 H50A 110.3 . . ?
O8 C50 H50B 110.3 . . ?
O8 C50 C51 107.2(4) . . ?
H50A C50 H50B 108.5 . . ?
C51 C50 H50A 110.3 . . ?
C51 C50 H50B 110.3 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 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
N5 H5D O7 0.88 2.11 2.712(4) 124.4 .

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.027 0.000 0.500 373.1 72.8 ?

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

data_190225lyz_0m
_database_code_depnum_ccdc_archive 'CCDC 1960289'
loop_
_audit_author_name
_audit_author_address
'Yuezhou Liu'
;Zhejiang University
China
;
_audit_update_record             
;
2019-10-19 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_audit_creation_date             2019-02-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H38 N4 O6, 3(C2 H3 N)'
_chemical_formula_sum            'C48 H47 N7 O6'
_chemical_formula_weight         817.92
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   14.1397(3)
_cell_length_b                   17.9442(4)
_cell_length_c                   17.0478(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.0650(10)
_cell_angle_gamma                90
_cell_volume                     4135.02(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.89
_cell_measurement_theta_min      4.896
_shelx_estimated_absorpt_T_max   0.964
_shelx_estimated_absorpt_T_min   0.934
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1368 before and 0.0581 after correction. The Ratio of minimum to maximum transmission is 0.8494. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38333
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.925
_diffrn_reflns_theta_min         3.117
_diffrn_ambient_temperature      170.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6615
_reflns_number_total             7729
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.519
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7729
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0884
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0500P)²+12.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2036
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C14(H14A,H14B), C24(H24A,H24B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C34(H34),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C27(H27A,H27B,
 H27C), C31(H31A,H31B,H31C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C46(H46A,
 H46B,H46C), C48(H48A,H48B,H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.34720(15) 0.73847(12) 0.31374(13) 0.0342(5) Uani 1 1 d . . . . .
O2 O 0.67063(15) 0.72755(13) 0.18789(13) 0.0349(5) Uani 1 1 d . . . . .
O3 O 0.15780(14) 0.67928(12) 0.12304(12) 0.0326(5) Uani 1 1 d . . . . .
O4 O 0.48531(13) 0.62051(11) 0.01571(11) 0.0272(4) Uani 1 1 d . . . . .
O5 O 0.85569(15) 0.66428(13) 0.37991(13) 0.0337(5) Uani 1 1 d . . . . .
O6 O 0.52248(13) 0.62426(11) 0.48501(11) 0.0269(4) Uani 1 1 d . . . . .
N1 N 0.50002(17) 0.79322(14) 0.33646(13) 0.0268(5) Uani 1 1 d . . . . .
N2 N 0.63852(17) 0.80848(13) 0.28275(14) 0.0270(5) Uani 1 1 d . . . . .
N3 N 0.52297(18) 0.79075(14) 0.16394(14) 0.0277(5) Uani 1 1 d . . . . .
N4 N 0.38640(17) 0.81421(13) 0.21770(14) 0.0268(5) Uani 1 1 d . . . . .
C1 C 0.4055(2) 0.77717(16) 0.29164(16) 0.0260(6) Uani 1 1 d . . . . .
C2 C 0.5504(2) 0.84306(16) 0.29456(16) 0.0274(6) Uani 1 1 d . . . . .
C3 C 0.6157(2) 0.77011(16) 0.20905(16) 0.0274(6) Uani 1 1 d . . . . .
C4 C 0.4765(2) 0.84393(16) 0.20558(16) 0.0277(6) Uani 1 1 d . . . . .
C5 C 0.3027(2) 0.79230(16) 0.14803(17) 0.0287(6) Uani 1 1 d . . . . .
H5A H 0.292241 0.831423 0.105387 0.034 Uiso 1 1 calc R . . . .
H5B H 0.242598 0.790371 0.166487 0.034 Uiso 1 1 calc R . . . .
C6 C 0.3140(2) 0.71790(16) 0.10935(15) 0.0241(6) Uani 1 1 d . . . . .
C7 C 0.24266(19) 0.66424(16) 0.10116(15) 0.0244(6) Uani 1 1 d . . . . .
C8 C 0.1555(3) 0.6485(2) 0.2009(2) 0.0446(9) Uani 1 1 d . . . . .
H8A H 0.157317 0.593981 0.198435 0.067 Uiso 1 1 calc GR . . . .
H8B H 0.094636 0.664295 0.212579 0.067 Uiso 1 1 calc GR . . . .
H8C H 0.212930 0.666401 0.244484 0.067 Uiso 1 1 calc GR . . . .
C9 C 0.24808(19) 0.59368(16) 0.06296(15) 0.0228(6) Uani 1 1 d . . . . .
C10 C 0.33100(19) 0.57939(16) 0.03302(15) 0.0222(5) Uani 1 1 d . . . . .
C11 C 0.40424(19) 0.63647(16) 0.04256(15) 0.0230(6) Uani 1 1 d . . . . .
C12 C 0.4730(2) 0.6405(2) -0.06825(18) 0.0359(7) Uani 1 1 d . . . . .
H12A H 0.418857 0.611329 -0.104179 0.054 Uiso 1 1 calc GR . . . .
H12B H 0.534371 0.630061 -0.081947 0.054 Uiso 1 1 calc GR . . . .
H12C H 0.457513 0.693704 -0.075937 0.054 Uiso 1 1 calc GR . . . .
C13 C 0.39697(19) 0.70346(16) 0.07831(15) 0.0236(6) Uani 1 1 d . . . . .
C14 C 0.4750(2) 0.76266(17) 0.08196(16) 0.0279(6) Uani 1 1 d . . . . .
H14A H 0.526097 0.741520 0.059254 0.033 Uiso 1 1 calc R . . . .
H14B H 0.443600 0.804925 0.046499 0.033 Uiso 1 1 calc R . . . .
C15 C 0.3366(2) 0.51191(16) -0.00628(16) 0.0246(6) Uani 1 1 d . . . . .
H15 H 0.392338 0.502168 -0.025091 0.030 Uiso 1 1 calc R . . . .
C16 C 0.2615(2) 0.45831(16) -0.01849(16) 0.0259(6) Uani 1 1 d . . . . .
C17 C 0.1790(2) 0.47251(16) 0.01207(16) 0.0257(6) Uani 1 1 d . . . . .
C18 C 0.1745(2) 0.53920(16) 0.05240(16) 0.0262(6) Uani 1 1 d . . . . .
H18 H 0.120151 0.548010 0.073294 0.031 Uiso 1 1 calc R . . . .
C19 C 0.1034(2) 0.41714(18) -0.00111(19) 0.0336(7) Uani 1 1 d . . . . .
H19 H 0.048628 0.425071 0.019467 0.040 Uiso 1 1 calc R . . . .
C20 C 0.1084(2) 0.35366(19) -0.0423(2) 0.0401(8) Uani 1 1 d . . . . .
H20 H 0.056757 0.317936 -0.051044 0.048 Uiso 1 1 calc R . . . .
C21 C 0.1901(3) 0.33982(19) -0.0728(2) 0.0397(8) Uani 1 1 d . . . . .
H21 H 0.192692 0.294907 -0.101607 0.048 Uiso 1 1 calc R . . . .
C22 C 0.2648(2) 0.39047(17) -0.06100(18) 0.0327(7) Uani 1 1 d . . . . .
H22 H 0.319414 0.380481 -0.081222 0.039 Uiso 1 1 calc R . . . .
C23 C 0.4608(3) 0.91924(18) 0.16358(19) 0.0403(8) Uani 1 1 d . . . . .
H23A H 0.524814 0.940109 0.163586 0.061 Uiso 1 1 calc GR . . . .
H23B H 0.428522 0.952914 0.193076 0.061 Uiso 1 1 calc GR . . . .
H23C H 0.418776 0.913413 0.106896 0.061 Uiso 1 1 calc GR . . . .
C24 C 0.7197(2) 0.78362(17) 0.35298(17) 0.0288(6) Uani 1 1 d . . . . .
H24A H 0.733357 0.823232 0.395252 0.035 Uiso 1 1 calc R . . . .
H24B H 0.779761 0.777927 0.334871 0.035 Uiso 1 1 calc R . . . .
C25 C 0.7024(2) 0.71102(16) 0.39253(15) 0.0245(6) Uani 1 1 d . . . . .
C26 C 0.7699(2) 0.65446(17) 0.40221(16) 0.0256(6) Uani 1 1 d . . . . .
C27 C 0.8541(3) 0.6301(2) 0.3024(2) 0.0458(9) Uani 1 1 d . . . . .
H27A H 0.805818 0.655969 0.257494 0.069 Uiso 1 1 calc GR . . . .
H27B H 0.835445 0.577567 0.302785 0.069 Uiso 1 1 calc GR . . . .
H27C H 0.919888 0.633812 0.294629 0.069 Uiso 1 1 calc GR . . . .
C28 C 0.75973(19) 0.58548(16) 0.44170(15) 0.0233(6) Uani 1 1 d . . . . .
C29 C 0.67440(19) 0.57564(16) 0.47017(15) 0.0227(6) Uani 1 1 d . . . . .
C30 C 0.60558(19) 0.63591(16) 0.45943(16) 0.0233(6) Uani 1 1 d . . . . .
C31 C 0.5346(2) 0.6427(2) 0.56928(18) 0.0366(7) Uani 1 1 d . . . . .
H31A H 0.554953 0.694925 0.579024 0.055 Uiso 1 1 calc GR . . . .
H31B H 0.585450 0.610529 0.604782 0.055 Uiso 1 1 calc GR . . . .
H31C H 0.471829 0.635231 0.581604 0.055 Uiso 1 1 calc GR . . . .
C32 C 0.61815(19) 0.70175(16) 0.42332(15) 0.0234(6) Uani 1 1 d . . . . .
C33 C 0.5452(2) 0.76444(16) 0.41897(16) 0.0271(6) Uani 1 1 d . . . . .
H33A H 0.492221 0.746432 0.441379 0.033 Uiso 1 1 calc R . . . .
H33B H 0.579721 0.805795 0.454373 0.033 Uiso 1 1 calc R . . . .
C34 C 0.6631(2) 0.50919(16) 0.50883(16) 0.0249(6) Uani 1 1 d . . . . .
H34 H 0.605580 0.502094 0.525978 0.030 Uiso 1 1 calc R . . . .
C35 C 0.7342(2) 0.45279(16) 0.52297(16) 0.0262(6) Uani 1 1 d . . . . .
C36 C 0.8201(2) 0.46325(16) 0.49561(17) 0.0266(6) Uani 1 1 d . . . . .
C37 C 0.8300(2) 0.52876(16) 0.45517(17) 0.0264(6) Uani 1 1 d . . . . .
H37 H 0.886264 0.535027 0.436171 0.032 Uiso 1 1 calc R . . . .
C38 C 0.8931(2) 0.40518(18) 0.51211(19) 0.0345(7) Uani 1 1 d . . . . .
H38 H 0.950670 0.411003 0.494701 0.041 Uiso 1 1 calc R . . . .
C39 C 0.8814(3) 0.34236(19) 0.5520(2) 0.0402(8) Uani 1 1 d . . . . .
H39 H 0.930995 0.304874 0.562721 0.048 Uiso 1 1 calc R . . . .
C40 C 0.7960(3) 0.33180(19) 0.5780(2) 0.0386(7) Uani 1 1 d . . . . .
H40 H 0.788494 0.287047 0.605320 0.046 Uiso 1 1 calc R . . . .
C41 C 0.7242(2) 0.38523(17) 0.56413(18) 0.0320(7) Uani 1 1 d . . . . .
H41 H 0.667365 0.377432 0.581975 0.038 Uiso 1 1 calc R . . . .
C42 C 0.5719(3) 0.91842(18) 0.33656(19) 0.0386(8) Uani 1 1 d . . . . .
H42A H 0.509476 0.942502 0.336002 0.058 Uiso 1 1 calc GR . . . .
H42B H 0.607204 0.949807 0.307360 0.058 Uiso 1 1 calc GR . . . .
H42C H 0.612802 0.911593 0.393426 0.058 Uiso 1 1 calc GR . . . .
N5 N 0.5257(6) 0.2859(3) 0.2502(3) 0.120(2) Uani 1 1 d . . . . .
C43 C 0.5998(5) 0.3230(3) 0.2838(3) 0.0764(15) Uani 1 1 d . . . . .
C44 C 0.6865(3) 0.3700(3) 0.3250(3) 0.0619(11) Uani 1 1 d . . . . .
H44A H 0.703778 0.401403 0.284231 0.093 Uiso 1 1 calc GR . . . .
H44B H 0.742804 0.337948 0.351984 0.093 Uiso 1 1 calc GR . . . .
H44C H 0.670290 0.401652 0.366119 0.093 Uiso 1 1 calc GR . . . .
N6 N 0.2447(10) 0.4711(4) 0.2663(6) 0.221(6) Uani 1 1 d . . . . .
C45 C 0.2753(5) 0.4278(4) 0.2287(4) 0.0917(18) Uani 1 1 d . . . . .
C46 C 0.3149(3) 0.3735(3) 0.1829(3) 0.0601(11) Uani 1 1 d . . . . .
H46A H 0.338374 0.399305 0.141527 0.090 Uiso 1 1 calc GR . . . .
H46B H 0.262961 0.337963 0.155848 0.090 Uiso 1 1 calc GR . . . .
H46C H 0.370149 0.346672 0.220733 0.090 Uiso 1 1 calc GR . . . .
N7 N 0.4517(5) 0.5600(7) 0.2772(5) 0.228(6) Uani 1 1 d . . . . .
C47 C 0.5250(8) 0.5616(8) 0.2418(4) 0.181(5) Uani 1 1 d . . . . .
C48 C 0.5888(7) 0.5195(4) 0.2025(4) 0.126(3) Uani 1 1 d . . . . .
H48A H 0.615938 0.553611 0.169665 0.188 Uiso 1 1 calc GR . . . .
H48B H 0.549640 0.480823 0.166906 0.188 Uiso 1 1 calc GR . . . .
H48C H 0.643123 0.496308 0.244908 0.188 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.219(4) . ?
O2 C3 1.218(4) . ?
O3 C7 1.384(3) . ?
O3 C8 1.447(4) . ?
O4 C11 1.383(3) . ?
O4 C12 1.436(3) . ?
O5 C26 1.385(3) . ?
O5 C27 1.450(4) . ?
O6 C30 1.384(3) . ?
O6 C31 1.434(3) . ?
N1 C1 1.362(4) . ?
N1 C2 1.455(4) . ?
N1 C33 1.458(3) . ?
N2 C2 1.458(4) . ?
N2 C3 1.385(4) . ?
N2 C24 1.464(4) . ?
N3 C3 1.362(4) . ?
N3 C4 1.456(4) . ?
N3 C14 1.453(3) . ?
N4 C1 1.380(4) . ?
N4 C4 1.451(4) . ?
N4 C5 1.463(3) . ?
C2 C4 1.570(4) . ?
C2 C42 1.518(4) . ?
C4 C23 1.515(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.518(4) . ?
C6 C7 1.372(4) . ?
C6 C13 1.445(4) . ?
C7 C9 1.436(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.433(4) . ?
C9 C18 1.401(4) . ?
C10 C11 1.431(4) . ?
C10 C15 1.397(4) . ?
C11 C13 1.365(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.520(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15 0.9500 . ?
C15 C16 1.402(4) . ?
C16 C17 1.433(4) . ?
C16 C22 1.425(4) . ?
C17 C18 1.391(4) . ?
C17 C19 1.428(4) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C19 C20 1.351(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.421(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.363(4) . ?
C22 H22 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.520(4) . ?
C25 C26 1.370(4) . ?
C25 C32 1.445(4) . ?
C26 C28 1.436(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.437(4) . ?
C28 C37 1.393(4) . ?
C29 C30 1.430(4) . ?
C29 C34 1.394(4) . ?
C30 C32 1.368(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.513(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34 0.9500 . ?
C34 C35 1.397(4) . ?
C35 C36 1.435(4) . ?
C35 C41 1.428(4) . ?
C36 C37 1.390(4) . ?
C36 C38 1.436(4) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C38 C39 1.352(5) . ?
C39 H39 0.9500 . ?
C39 C40 1.416(5) . ?
C40 H40 0.9500 . ?
C40 C41 1.365(4) . ?
C41 H41 0.9500 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
N5 C43 1.231(8) . ?
C43 C44 1.485(8) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
N6 C45 1.169(9) . ?
C45 C46 1.459(8) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
N7 C47 1.345(14) . ?
C47 C48 1.478(13) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 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
C7 O3 C8 115.3(2) . . ?
C11 O4 C12 114.1(2) . . ?
C26 O5 C27 114.5(2) . . ?
C30 O6 C31 114.7(2) . . ?
C1 N1 C2 113.4(2) . . ?
C1 N1 C33 123.1(2) . . ?
C2 N1 C33 123.5(2) . . ?
C2 N2 C24 120.9(2) . . ?
C3 N2 C2 110.8(2) . . ?
C3 N2 C24 120.6(2) . . ?
C3 N3 C4 113.6(2) . . ?
C3 N3 C14 123.3(2) . . ?
C14 N3 C4 123.1(2) . . ?
C1 N4 C4 111.3(2) . . ?
C1 N4 C5 120.4(2) . . ?
C4 N4 C5 121.2(2) . . ?
O1 C1 N1 126.1(3) . . ?
O1 C1 N4 126.1(3) . . ?
N1 C1 N4 107.9(2) . . ?
N1 C2 N2 111.6(2) . . ?
N1 C2 C4 101.4(2) . . ?
N1 C2 C42 112.0(2) . . ?
N2 C2 C4 103.0(2) . . ?
N2 C2 C42 112.6(2) . . ?
C42 C2 C4 115.5(2) . . ?
O2 C3 N2 125.5(3) . . ?
O2 C3 N3 126.6(3) . . ?
N3 C3 N2 107.9(3) . . ?
N3 C4 C2 101.3(2) . . ?
N3 C4 C23 112.3(2) . . ?
N4 C4 N3 111.7(2) . . ?
N4 C4 C2 102.8(2) . . ?
N4 C4 C23 112.5(3) . . ?
C23 C4 C2 115.4(2) . . ?
N4 C5 H5A 108.5 . . ?
N4 C5 H5B 108.5 . . ?
N4 C5 C6 115.2(2) . . ?
H5A C5 H5B 107.5 . . ?
C6 C5 H5A 108.5 . . ?
C6 C5 H5B 108.5 . . ?
C7 C6 C5 119.6(2) . . ?
C7 C6 C13 119.3(3) . . ?
C13 C6 C5 121.1(2) . . ?
O3 C7 C9 117.4(2) . . ?
C6 C7 O3 120.4(3) . . ?
C6 C7 C9 122.0(2) . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C7 118.5(2) . . ?
C18 C9 C7 122.5(2) . . ?
C18 C9 C10 119.0(3) . . ?
C11 C10 C9 118.1(2) . . ?
C15 C10 C9 119.6(2) . . ?
C15 C10 C11 122.2(2) . . ?
O4 C11 C10 117.2(2) . . ?
C13 C11 O4 120.6(2) . . ?
C13 C11 C10 122.3(2) . . ?
O4 C12 H12A 109.5 . . ?
O4 C12 H12B 109.5 . . ?
O4 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C6 C13 C14 121.2(2) . . ?
C11 C13 C6 119.8(2) . . ?
C11 C13 C14 119.0(2) . . ?
N3 C14 C13 114.2(2) . . ?
N3 C14 H14A 108.7 . . ?
N3 C14 H14B 108.7 . . ?
C13 C14 H14A 108.7 . . ?
C13 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C10 C15 H15 119.4 . . ?
C10 C15 C16 121.2(2) . . ?
C16 C15 H15 119.4 . . ?
C15 C16 C17 119.1(3) . . ?
C15 C16 C22 121.6(3) . . ?
C22 C16 C17 119.3(3) . . ?
C18 C17 C16 119.5(3) . . ?
C18 C17 C19 122.4(3) . . ?
C19 C17 C16 118.1(3) . . ?
C9 C18 H18 119.2 . . ?
C17 C18 C9 121.6(3) . . ?
C17 C18 H18 119.2 . . ?
C17 C19 H19 119.4 . . ?
C20 C19 C17 121.2(3) . . ?
C20 C19 H19 119.4 . . ?
C19 C20 H20 119.7 . . ?
C19 C20 C21 120.7(3) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 119.7 . . ?
C22 C21 C20 120.5(3) . . ?
C22 C21 H21 119.7 . . ?
C16 C22 H22 119.8 . . ?
C21 C22 C16 120.3(3) . . ?
C21 C22 H22 119.8 . . ?
C4 C23 H23A 109.5 . . ?
C4 C23 H23B 109.5 . . ?
C4 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C24 H24A 108.4 . . ?
N2 C24 H24B 108.4 . . ?
N2 C24 C25 115.7(2) . . ?
H24A C24 H24B 107.4 . . ?
C25 C24 H24A 108.4 . . ?
C25 C24 H24B 108.4 . . ?
C26 C25 C24 119.4(2) . . ?
C26 C25 C32 119.4(3) . . ?
C32 C25 C24 121.2(3) . . ?
O5 C26 C28 117.0(2) . . ?
C25 C26 O5 120.6(3) . . ?
C25 C26 C28 122.2(2) . . ?
O5 C27 H27A 109.5 . . ?
O5 C27 H27B 109.5 . . ?
O5 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 C29 118.3(2) . . ?
C37 C28 C26 122.8(2) . . ?
C37 C28 C29 118.9(3) . . ?
C30 C29 C28 118.1(2) . . ?
C34 C29 C28 119.3(2) . . ?
C34 C29 C30 122.6(2) . . ?
O6 C30 C29 117.0(2) . . ?
C32 C30 O6 120.5(2) . . ?
C32 C30 C29 122.5(2) . . ?
O6 C31 H31A 109.5 . . ?
O6 C31 H31B 109.5 . . ?
O6 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C25 C32 C33 121.3(2) . . ?
C30 C32 C25 119.5(2) . . ?
C30 C32 C33 119.2(2) . . ?
N1 C33 C32 114.2(2) . . ?
N1 C33 H33A 108.7 . . ?
N1 C33 H33B 108.7 . . ?
C32 C33 H33A 108.7 . . ?
C32 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
C29 C34 H34 119.2 . . ?
C29 C34 C35 121.7(2) . . ?
C35 C34 H34 119.2 . . ?
C34 C35 C36 118.9(3) . . ?
C34 C35 C41 122.0(3) . . ?
C41 C35 C36 119.0(3) . . ?
C35 C36 C38 118.0(3) . . ?
C37 C36 C35 119.3(3) . . ?
C37 C36 C38 122.7(3) . . ?
C28 C37 H37 119.0 . . ?
C36 C37 C28 121.9(2) . . ?
C36 C37 H37 119.0 . . ?
C36 C38 H38 119.5 . . ?
C39 C38 C36 121.1(3) . . ?
C39 C38 H38 119.5 . . ?
C38 C39 H39 119.6 . . ?
C38 C39 C40 120.7(3) . . ?
C40 C39 H39 119.6 . . ?
C39 C40 H40 119.6 . . ?
C41 C40 C39 120.7(3) . . ?
C41 C40 H40 119.6 . . ?
C35 C41 H41 119.8 . . ?
C40 C41 C35 120.4(3) . . ?
C40 C41 H41 119.8 . . ?
C2 C42 H42A 109.5 . . ?
C2 C42 H42B 109.5 . . ?
C2 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N5 C43 C44 177.7(6) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N6 C45 C46 179.0(9) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N7 C47 C48 147.8(13) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?

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

data_190530lyz_1_0m
_database_code_depnum_ccdc_archive 'CCDC 1960292'
loop_
_audit_author_name
_audit_author_address
'Yuezhou Liu'
;Zhejiang University
China
;
_audit_update_record             
;
2019-10-19 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_audit_creation_date             2019-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C H Cl3, C6 H3 N3 O7, C42 H38 N4 O6'
_chemical_formula_sum            'C49 H42 Cl3 N7 O13'
_chemical_formula_weight         1043.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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 0.3281 0.5435 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.2666(5)
_cell_length_b                   26.6723(14)
_cell_length_c                   18.5536(9)
_cell_angle_alpha                90
_cell_angle_beta                 101.541(2)
_cell_angle_gamma                90
_cell_volume                     4493.0(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.94
_cell_measurement_theta_min      4.47
_shelx_estimated_absorpt_T_max   0.922
_shelx_estimated_absorpt_T_min   0.879
_exptl_absorpt_coefficient_mu    1.659
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 57199 reflections, Rint = 0.1006
 (37369 with I > 3sig(I), Rint = 0.0968)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8322
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.043
_diffrn_reflns_theta_min         3.576
_diffrn_ambient_temperature      150.04
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6879
_reflns_number_total             8322
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         8322
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0626
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1330P)²+3.9774P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.2046
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.516(2)
 0.484(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C21(H21A,H21B), C31(H31A,H31B), C40(H40A,H40B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
 C41(H41), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48)
3.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C30(H30A,H30B,H30C), C34(H34A,H34B,
 H34C), C38(H38A,H38B,H38C), C49(H49A,H49B,H49C)
3.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.45723(13) 0.74519(3) 0.21579(6) 0.0349(3) Uani 1 1 d . . . . .
Cl2 Cl 0.14266(14) 0.74551(4) 0.16060(8) 0.0443(3) Uani 1 1 d . . . . .
Cl3 Cl 0.34739(15) 0.74561(4) 0.05902(7) 0.0442(3) Uani 1 1 d . . . . .
C1 C 0.3146(4) 0.72556(17) 0.1442(2) 0.0382(9) Uani 1 1 d . . . . .
H1 H 0.314456 0.688065 0.143932 0.046 Uiso 1 1 calc R . . . .
O1 O 0.3167(4) 0.50085(13) 0.3689(2) 0.0543(9) Uani 1 1 d . . . . .
O2 O 0.5286(4) 0.52573(12) 0.43042(17) 0.0442(8) Uani 1 1 d . . . . .
O3 O 0.7522(3) 0.52782(10) 0.37157(15) 0.0369(7) Uani 1 1 d . . . . .
H3 H 0.707347 0.528926 0.406642 0.055 Uiso 1 1 calc GR . . . .
O4 O 0.9388(3) 0.54433(11) 0.28347(17) 0.0416(7) Uani 1 1 d . . . . .
O5 O 0.9236(4) 0.48328(12) 0.20593(18) 0.0468(8) Uani 1 1 d . . . . .
O6 O 0.2479(3) 0.45599(11) 0.11739(18) 0.0448(8) Uani 1 1 d . . . . .
O7 O 0.4283(4) 0.45999(12) 0.05917(17) 0.0458(8) Uani 1 1 d . . . . .
N1 N 0.4457(4) 0.51048(12) 0.3727(2) 0.0359(8) Uani 1 1 d . . . . .
N2 N 0.8698(4) 0.51126(12) 0.24555(18) 0.0315(7) Uani 1 1 d . . . . .
N3 N 0.3759(4) 0.46477(12) 0.11467(19) 0.0340(8) Uani 1 1 d . . . . .
C2 C 0.5092(5) 0.50454(13) 0.3074(2) 0.0291(8) Uani 1 1 d . . . . .
C3 C 0.6603(4) 0.51376(12) 0.3111(2) 0.0266(8) Uani 1 1 d . . . . .
C4 C 0.7120(4) 0.50545(13) 0.2463(2) 0.0261(8) Uani 1 1 d . . . . .
C5 C 0.6221(4) 0.48959(13) 0.1818(2) 0.0286(8) Uani 1 1 d . . . . .
H5 H 0.660325 0.483966 0.138687 0.034 Uiso 1 1 calc R . . . .
C6 C 0.4741(5) 0.48213(13) 0.1820(2) 0.0289(9) Uani 1 1 d . . . . .
C7 C 0.4146(4) 0.48875(13) 0.2435(2) 0.0305(8) Uani 1 1 d . . . . .
H7 H 0.313074 0.482805 0.242347 0.037 Uiso 1 1 calc R . . . .
O8 O 0.8769(3) 0.74864(8) 0.23126(18) 0.0272(7) Uani 1 1 d . . . . .
O9 O 0.4837(3) 0.74362(9) 0.42700(18) 0.0287(7) Uani 1 1 d . . . . .
O10 O 0.7459(3) 0.62262(10) 0.16437(14) 0.0264(6) Uani 1 1 d . . . . .
O11 O 0.3566(3) 0.62204(10) 0.35572(14) 0.0249(6) Uani 1 1 d . . . . .
O12 O 0.3319(3) 0.86595(10) 0.35212(15) 0.0270(6) Uani 1 1 d . . . . .
O13 O 0.7182(3) 0.86936(10) 0.15920(15) 0.0262(6) Uani 1 1 d . . . . .
N4 N 0.8643(3) 0.79030(11) 0.33838(17) 0.0199(6) Uani 1 1 d . . . . .
N5 N 0.6958(3) 0.78843(11) 0.42207(18) 0.0208(6) Uani 1 1 d . . . . .
N6 N 0.7070(3) 0.70513(10) 0.42502(17) 0.0188(6) Uani 1 1 d . . . . .
N7 N 0.8735(3) 0.70733(11) 0.33987(17) 0.0211(6) Uani 1 1 d . . . . .
C8 C 0.8697(4) 0.74856(11) 0.2959(2) 0.0200(8) Uani 1 1 d . . . . .
C9 C 0.8453(4) 0.77865(12) 0.41211(18) 0.0190(7) Uani 1 1 d . . . . .
C10 C 0.6145(5) 0.74560(12) 0.4240(2) 0.0205(8) Uani 1 1 d . . . . .
C11 C 0.8525(4) 0.71913(12) 0.41320(18) 0.0184(6) Uani 1 1 d . . . . .
C12 C 0.8561(4) 0.65659(13) 0.3095(2) 0.0214(7) Uani 1 1 d . . . . .
H12A H 0.903029 0.632618 0.347881 0.026 Uiso 1 1 calc R . . . .
H12B H 0.908686 0.654289 0.268163 0.026 Uiso 1 1 calc R . . . .
C13 C 0.6965(4) 0.64118(13) 0.28230(19) 0.0190(7) Uani 1 1 d . . . . .
C14 C 0.6480(4) 0.62688(13) 0.2113(2) 0.0217(7) Uani 1 1 d . . . . .
C15 C 0.7427(5) 0.66358(17) 0.1131(2) 0.0344(10) Uani 1 1 d . . . . .
H15A H 0.794257 0.653656 0.074076 0.052 Uiso 1 1 calc GR . . . .
H15B H 0.791546 0.692898 0.139041 0.052 Uiso 1 1 calc GR . . . .
H15C H 0.640302 0.671974 0.091412 0.052 Uiso 1 1 calc GR . . . .
C16 C 0.4981(4) 0.61295(12) 0.18285(19) 0.0187(7) Uani 1 1 d . . . . .
C17 C 0.3974(4) 0.61292(12) 0.2328(2) 0.0200(7) Uani 1 1 d . . . . .
C18 C 0.4508(4) 0.62666(12) 0.30722(19) 0.0183(7) Uani 1 1 d . . . . .
C19 C 0.2518(4) 0.66231(16) 0.3539(2) 0.0324(9) Uani 1 1 d . . . . .
H19A H 0.211508 0.671525 0.302668 0.049 Uiso 1 1 calc GR . . . .
H19B H 0.301009 0.691413 0.380198 0.049 Uiso 1 1 calc GR . . . .
H19C H 0.171587 0.651308 0.377505 0.049 Uiso 1 1 calc GR . . . .
C20 C 0.5956(4) 0.64089(12) 0.33256(19) 0.0188(7) Uani 1 1 d . . . . .
C21 C 0.6486(4) 0.65445(12) 0.41270(19) 0.0196(7) Uani 1 1 d . . . . .
H21A H 0.565590 0.650627 0.438532 0.024 Uiso 1 1 calc R . . . .
H21B H 0.726267 0.630396 0.434900 0.024 Uiso 1 1 calc R . . . .
C22 C 0.2509(4) 0.59801(13) 0.2069(2) 0.0227(7) Uani 1 1 d . . . . .
H22 H 0.185831 0.595939 0.240403 0.027 Uiso 1 1 calc R . . . .
C23 C 0.1987(4) 0.58612(12) 0.1326(2) 0.0208(7) Uani 1 1 d . . . . .
C24 C 0.2994(4) 0.58666(13) 0.0831(2) 0.0231(7) Uani 1 1 d . . . . .
C25 C 0.4469(4) 0.59882(13) 0.1100(2) 0.0241(8) Uani 1 1 d . . . . .
H25 H 0.514290 0.597403 0.077606 0.029 Uiso 1 1 calc R . . . .
C26 C 0.2444(5) 0.57449(14) 0.0077(2) 0.0275(8) Uani 1 1 d . . . . .
H26 H 0.309213 0.574731 -0.026073 0.033 Uiso 1 1 calc R . . . .
C27 C 0.0990(5) 0.56248(14) -0.0165(2) 0.0300(9) Uani 1 1 d . . . . .
H27 H 0.063964 0.554452 -0.066856 0.036 Uiso 1 1 calc R . . . .
C28 C -0.0001(4) 0.56188(14) 0.0329(2) 0.0304(9) Uani 1 1 d . . . . .
H28 H -0.100537 0.553326 0.015473 0.036 Uiso 1 1 calc R . . . .
C29 C 0.0482(4) 0.57353(14) 0.1053(2) 0.0267(8) Uani 1 1 d . . . . .
H29 H -0.019044 0.573255 0.137761 0.032 Uiso 1 1 calc R . . . .
C30 C 0.9741(4) 0.69685(13) 0.4715(2) 0.0255(8) Uani 1 1 d . . . . .
H30A H 0.960897 0.707443 0.520338 0.038 Uiso 1 1 calc GR . . . .
H30B H 1.069950 0.708549 0.463490 0.038 Uiso 1 1 calc GR . . . .
H30C H 0.970105 0.660186 0.468303 0.038 Uiso 1 1 calc GR . . . .
C31 C 0.6266(4) 0.83757(13) 0.4092(2) 0.0217(7) Uani 1 1 d . . . . .
H31A H 0.698643 0.863420 0.431339 0.026 Uiso 1 1 calc R . . . .
H31B H 0.542603 0.839073 0.434743 0.026 Uiso 1 1 calc R . . . .
C32 C 0.5712(4) 0.85028(12) 0.3284(2) 0.0190(7) Uani 1 1 d . . . . .
C33 C 0.4256(4) 0.86226(13) 0.3031(2) 0.0204(7) Uani 1 1 d . . . . .
C34 C 0.2339(4) 0.82422(17) 0.3514(3) 0.0374(10) Uani 1 1 d . . . . .
H34A H 0.196163 0.813759 0.300469 0.056 Uiso 1 1 calc GR . . . .
H34B H 0.151490 0.834115 0.374143 0.056 Uiso 1 1 calc GR . . . .
H34C H 0.287166 0.796291 0.379032 0.056 Uiso 1 1 calc GR . . . .
C35 C 0.3691(4) 0.87577(12) 0.2285(2) 0.0207(7) Uani 1 1 d . . . . .
C36 C 0.4693(4) 0.87716(13) 0.17872(19) 0.0196(7) Uani 1 1 d . . . . .
C37 C 0.6208(4) 0.86456(13) 0.2065(2) 0.0211(7) Uani 1 1 d . . . . .
C38 C 0.7166(5) 0.82779(16) 0.1096(2) 0.0323(9) Uani 1 1 d . . . . .
H38A H 0.781034 0.835214 0.075011 0.048 Uiso 1 1 calc GR . . . .
H38B H 0.615868 0.822300 0.082227 0.048 Uiso 1 1 calc GR . . . .
H38C H 0.751733 0.797565 0.137696 0.048 Uiso 1 1 calc GR . . . .
C39 C 0.6721(4) 0.85155(12) 0.27856(19) 0.0189(7) Uani 1 1 d . . . . .
C40 C 0.8346(4) 0.84023(13) 0.3057(2) 0.0219(7) Uani 1 1 d . . . . .
H40A H 0.885732 0.843352 0.263886 0.026 Uiso 1 1 calc R . . . .
H40B H 0.876791 0.865712 0.342785 0.026 Uiso 1 1 calc R . . . .
C41 C 0.4168(4) 0.89296(13) 0.1066(2) 0.0230(8) Uani 1 1 d . . . . .
H41 H 0.482980 0.894587 0.073601 0.028 Uiso 1 1 calc R . . . .
C42 C 0.2689(4) 0.90652(13) 0.0813(2) 0.0236(7) Uani 1 1 d . . . . .
C43 C 0.1691(4) 0.90439(13) 0.1309(2) 0.0231(8) Uani 1 1 d . . . . .
C44 C 0.2214(4) 0.88932(13) 0.2039(2) 0.0229(8) Uani 1 1 d . . . . .
H44 H 0.155690 0.888275 0.237099 0.028 Uiso 1 1 calc R . . . .
C45 C 0.0196(4) 0.91984(14) 0.1061(2) 0.0274(8) Uani 1 1 d . . . . .
H45 H -0.047527 0.918420 0.138586 0.033 Uiso 1 1 calc R . . . .
C46 C -0.0267(5) 0.93655(14) 0.0360(2) 0.0295(9) Uani 1 1 d . . . . .
H46 H -0.126051 0.946934 0.020000 0.035 Uiso 1 1 calc R . . . .
C47 C 0.0726(5) 0.93866(14) -0.0138(2) 0.0317(9) Uani 1 1 d . . . . .
H47 H 0.038668 0.950337 -0.062590 0.038 Uiso 1 1 calc R . . . .
C48 C 0.2163(4) 0.92397(14) 0.0083(2) 0.0258(8) Uani 1 1 d . . . . .
H48 H 0.281207 0.925445 -0.025278 0.031 Uiso 1 1 calc R . . . .
C49 C 0.9579(4) 0.80487(13) 0.4705(2) 0.0254(7) Uani 1 1 d . . . . .
H49A H 1.057305 0.795515 0.464862 0.038 Uiso 1 1 calc GR . . . .
H49B H 0.943528 0.794804 0.519363 0.038 Uiso 1 1 calc GR . . . .
H49C H 0.945590 0.841256 0.464984 0.038 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C1 1.756(4) . ?
Cl2 C1 1.764(4) . ?
Cl3 C1 1.751(5) . ?
O1 N1 1.211(5) . ?
O2 N1 1.255(5) . ?
O3 C3 1.321(4) . ?
O4 N2 1.226(4) . ?
O5 N2 1.222(4) . ?
O6 N3 1.219(5) . ?
O7 N3 1.230(5) . ?
N1 C2 1.457(5) . ?
N2 C4 1.473(5) . ?
N3 C6 1.466(5) . ?
C2 C3 1.410(6) . ?
C2 C7 1.393(5) . ?
C3 C4 1.398(6) . ?
C4 C5 1.380(5) . ?
C5 C6 1.386(6) . ?
C6 C7 1.373(6) . ?
O8 C8 1.214(5) . ?
O9 C10 1.226(5) . ?
O10 C14 1.382(4) . ?
O10 C15 1.445(5) . ?
O11 C18 1.379(4) . ?
O11 C19 1.444(5) . ?
O12 C33 1.381(4) . ?
O12 C34 1.435(5) . ?
O13 C37 1.385(4) . ?
O13 C38 1.439(5) . ?
N4 C8 1.371(5) . ?
N4 C9 1.447(4) . ?
N4 C40 1.466(4) . ?
N5 C9 1.458(4) . ?
N5 C10 1.373(5) . ?
N5 C31 1.458(4) . ?
N6 C10 1.376(4) . ?
N6 C11 1.457(4) . ?
N6 C21 1.457(4) . ?
N7 C8 1.366(5) . ?
N7 C11 1.447(4) . ?
N7 C12 1.462(4) . ?
C9 C11 1.589(5) . ?
C9 C49 1.516(4) . ?
C11 C30 1.519(4) . ?
C12 C13 1.521(5) . ?
C13 C14 1.359(5) . ?
C13 C20 1.446(5) . ?
C14 C16 1.432(5) . ?
C16 C17 1.441(5) . ?
C16 C25 1.392(5) . ?
C17 C18 1.419(5) . ?
C17 C22 1.404(5) . ?
C18 C20 1.383(5) . ?
C20 C21 1.514(5) . ?
C22 C23 1.403(5) . ?
C23 C24 1.434(5) . ?
C23 C29 1.425(5) . ?
C24 C25 1.396(5) . ?
C24 C26 1.429(5) . ?
C26 C27 1.371(6) . ?
C27 C28 1.422(6) . ?
C28 C29 1.363(6) . ?
C31 C32 1.523(5) . ?
C32 C33 1.375(5) . ?
C32 C39 1.441(5) . ?
C33 C35 1.425(5) . ?
C35 C36 1.435(5) . ?
C35 C44 1.400(5) . ?
C36 C37 1.435(5) . ?
C36 C41 1.395(5) . ?
C37 C39 1.371(5) . ?
C39 C40 1.520(5) . ?
C41 C42 1.404(5) . ?
C42 C43 1.431(5) . ?
C42 C48 1.422(5) . ?
C43 C44 1.402(5) . ?
C43 C45 1.431(5) . ?
C45 C46 1.360(6) . ?
C46 C47 1.430(6) . ?
C47 C48 1.370(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 C1 Cl2 110.4(2) . . ?
Cl3 C1 Cl1 110.6(2) . . ?
Cl3 C1 Cl2 112.9(2) . . ?
O1 N1 O2 123.2(4) . . ?
O1 N1 C2 119.2(4) . . ?
O2 N1 C2 117.7(4) . . ?
O4 N2 C4 118.4(3) . . ?
O5 N2 O4 123.8(4) . . ?
O5 N2 C4 117.8(3) . . ?
O6 N3 O7 124.4(3) . . ?
O6 N3 C6 117.9(4) . . ?
O7 N3 C6 117.7(4) . . ?
C3 C2 N1 120.3(4) . . ?
C7 C2 N1 116.8(4) . . ?
C7 C2 C3 122.9(4) . . ?
O3 C3 C2 123.7(4) . . ?
O3 C3 C4 120.2(4) . . ?
C4 C3 C2 116.1(3) . . ?
C3 C4 N2 120.2(3) . . ?
C5 C4 N2 116.9(3) . . ?
C5 C4 C3 122.8(4) . . ?
C4 C5 C6 117.9(4) . . ?
C5 C6 N3 119.2(4) . . ?
C7 C6 N3 117.7(4) . . ?
C7 C6 C5 123.1(4) . . ?
C6 C7 C2 117.2(4) . . ?
C14 O10 C15 115.0(3) . . ?
C18 O11 C19 115.4(3) . . ?
C33 O12 C34 114.7(3) . . ?
C37 O13 C38 114.2(3) . . ?
C8 N4 C9 113.2(3) . . ?
C8 N4 C40 121.7(3) . . ?
C9 N4 C40 122.5(3) . . ?
C9 N5 C31 122.6(3) . . ?
C10 N5 C9 113.2(3) . . ?
C10 N5 C31 121.8(3) . . ?
C10 N6 C11 112.9(3) . . ?
C10 N6 C21 121.0(3) . . ?
C21 N6 C11 122.7(3) . . ?
C8 N7 C11 113.3(3) . . ?
C8 N7 C12 121.8(3) . . ?
C11 N7 C12 122.5(3) . . ?
O8 C8 N4 125.6(3) . . ?
O8 C8 N7 126.3(3) . . ?
N7 C8 N4 108.0(4) . . ?
N4 C9 N5 112.3(3) . . ?
N4 C9 C11 102.4(2) . . ?
N4 C9 C49 112.3(3) . . ?
N5 C9 C11 102.4(2) . . ?
N5 C9 C49 111.2(3) . . ?
C49 C9 C11 115.5(2) . . ?
O9 C10 N5 126.1(3) . . ?
O9 C10 N6 125.8(3) . . ?
N5 C10 N6 108.1(3) . . ?
N6 C11 C9 102.7(2) . . ?
N6 C11 C30 111.7(3) . . ?
N7 C11 N6 112.8(3) . . ?
N7 C11 C9 102.6(2) . . ?
N7 C11 C30 111.4(3) . . ?
C30 C11 C9 115.0(2) . . ?
N7 C12 C13 113.8(3) . . ?
C14 C13 C12 120.6(3) . . ?
C14 C13 C20 119.5(3) . . ?
C20 C13 C12 119.9(3) . . ?
O10 C14 C16 117.2(3) . . ?
C13 C14 O10 120.1(3) . . ?
C13 C14 C16 122.6(3) . . ?
C14 C16 C17 117.9(3) . . ?
C25 C16 C14 123.0(3) . . ?
C25 C16 C17 119.1(3) . . ?
C18 C17 C16 118.7(3) . . ?
C22 C17 C16 119.1(3) . . ?
C22 C17 C18 122.1(3) . . ?
O11 C18 C17 117.9(3) . . ?
O11 C18 C20 120.0(3) . . ?
C20 C18 C17 121.8(3) . . ?
C13 C20 C21 120.5(3) . . ?
C18 C20 C13 119.4(3) . . ?
C18 C20 C21 120.1(3) . . ?
N6 C21 C20 114.4(3) . . ?
C23 C22 C17 121.3(3) . . ?
C22 C23 C24 119.1(3) . . ?
C22 C23 C29 121.6(3) . . ?
C29 C23 C24 119.3(4) . . ?
C25 C24 C23 119.3(3) . . ?
C25 C24 C26 122.3(3) . . ?
C26 C24 C23 118.4(4) . . ?
C16 C25 C24 121.9(3) . . ?
C27 C26 C24 120.5(4) . . ?
C26 C27 C28 120.7(4) . . ?
C29 C28 C27 120.4(4) . . ?
C28 C29 C23 120.6(4) . . ?
N5 C31 C32 114.3(3) . . ?
C33 C32 C31 120.2(3) . . ?
C33 C32 C39 119.6(3) . . ?
C39 C32 C31 120.2(3) . . ?
O12 C33 C35 117.7(3) . . ?
C32 C33 O12 119.6(3) . . ?
C32 C33 C35 122.4(3) . . ?
C33 C35 C36 118.2(3) . . ?
C44 C35 C33 121.8(3) . . ?
C44 C35 C36 120.0(3) . . ?
C35 C36 C37 118.4(3) . . ?
C41 C36 C35 118.6(3) . . ?
C41 C36 C37 122.9(3) . . ?
O13 C37 C36 117.7(3) . . ?
C39 C37 O13 119.9(3) . . ?
C39 C37 C36 122.2(3) . . ?
C32 C39 C40 120.7(3) . . ?
C37 C39 C32 119.2(3) . . ?
C37 C39 C40 120.1(3) . . ?
N4 C40 C39 114.1(3) . . ?
C36 C41 C42 121.9(3) . . ?
C41 C42 C43 119.2(4) . . ?
C41 C42 C48 121.9(3) . . ?
C48 C42 C43 118.9(4) . . ?
C44 C43 C42 119.3(4) . . ?
C44 C43 C45 121.3(3) . . ?
C45 C43 C42 119.3(4) . . ?
C35 C44 C43 121.0(3) . . ?
C46 C45 C43 120.2(4) . . ?
C45 C46 C47 120.6(4) . . ?
C48 C47 C46 120.6(4) . . ?
C47 C48 C42 120.4(4) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.516(2)
2 0.484(2)

####################################################################### 
# 
# 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_190325lyz_2_0m
_database_code_depnum_ccdc_archive 'CCDC 1960290'
loop_
_audit_author_name
_audit_author_address
'Yuezhou Liu'
;Zhejiang University
China
;
_audit_update_record             
;
2019-10-19 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_audit_creation_date             2019-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C H Cl3, C42 H38 N4 O6, C6 H5 N O3'
_chemical_formula_sum            'C49 H44 Cl3 N5 O9'
_chemical_formula_weight         953.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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 0.3281 0.5435 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.3707(5)
_cell_length_b                   12.8735(7)
_cell_length_c                   17.6390(9)
_cell_angle_alpha                71.233(3)
_cell_angle_beta                 81.025(4)
_cell_angle_gamma                80.639(3)
_cell_volume                     2186.5(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.77
_cell_measurement_theta_min      3.179
_shelx_estimated_absorpt_T_max   0.968
_shelx_estimated_absorpt_T_min   0.855
_exptl_absorpt_coefficient_mu    1.614
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1234 before and 0.0751 after correction. The Ratio of minimum to maximum transmission is 0.7543. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31289
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.070
_diffrn_reflns_theta_min         3.177
_diffrn_ambient_temperature      169.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5431
_reflns_number_total             8221
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.960
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.0050(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.310
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         8221
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.1144
_refine_ls_restrained_S_all      1.310
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3102
_refine_ls_wR_factor_ref         0.3506
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C49(H49)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B), C38(H38A,H38B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C27(H27), C29(H29), C30(H30),
 C31(H31), C32(H32), C34(H34), C44(H44), C45(H45), C47(H47), C48(H48)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
2.e Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.1009(3) 1.1208(3) 0.9021(2) 0.1523(12) Uani 1 1 d . . . . .
Cl2 Cl -0.1793(2) 1.15137(18) 0.90733(14) 0.1099(8) Uani 1 1 d . . . . .
Cl3 Cl -0.0067(3) 1.2064(2) 0.75869(17) 0.1464(12) Uani 1 1 d . . . . .
C49 C -0.0392(8) 1.1144(6) 0.8529(5) 0.087(2) Uani 1 1 d . . . . .
H49 H -0.038567 1.038344 0.849237 0.105 Uiso 1 1 calc R . . . .
O1 O 0.2344(3) 0.6503(3) 1.00632(18) 0.0449(8) Uani 1 1 d . . . . .
O2 O 0.6157(3) 0.5534(3) 0.77257(18) 0.0444(8) Uani 1 1 d . . . . .
O3 O 0.0971(3) 0.8749(3) 0.82690(18) 0.0414(7) Uani 1 1 d . . . . .
O4 O 0.5335(3) 0.8000(2) 0.61411(18) 0.0410(7) Uani 1 1 d . . . . .
O5 O -0.1045(3) 0.8686(2) 0.68339(17) 0.0390(7) Uani 1 1 d . . . . .
O6 O 0.3196(3) 0.8220(2) 0.45685(17) 0.0386(7) Uani 1 1 d . . . . .
N1 N 0.3138(3) 0.9073(3) 0.8150(2) 0.0367(8) Uani 1 1 d . . . . .
N2 N 0.4979(3) 0.8676(3) 0.7230(2) 0.0354(8) Uani 1 1 d . . . . .
N3 N 0.2021(3) 0.9808(3) 0.7096(2) 0.0362(8) Uani 1 1 d . . . . .
N4 N 0.3914(3) 0.9570(3) 0.6167(2) 0.0342(8) Uani 1 1 d . . . . .
C1 C 0.4840(5) 0.3820(4) 0.8855(3) 0.0417(11) Uani 1 1 d . . . . .
H1 H 0.550176 0.364489 0.846292 0.050 Uiso 1 1 calc R . . . .
C2 C 0.4161(5) 0.2983(4) 0.9389(3) 0.0452(11) Uani 1 1 d . . . . .
C3 C 0.4375(5) 0.1869(4) 0.9351(3) 0.0539(13) Uani 1 1 d . . . . .
H3 H 0.500930 0.168382 0.895022 0.065 Uiso 1 1 calc R . . . .
C4 C 0.3680(6) 0.1074(5) 0.9884(4) 0.0649(16) Uani 1 1 d . . . . .
H4 H 0.383750 0.034189 0.984966 0.078 Uiso 1 1 calc R . . . .
C5 C 0.2714(6) 0.1328(5) 1.0498(4) 0.0600(14) Uani 1 1 d . . . . .
H5 H 0.224204 0.076532 1.086907 0.072 Uiso 1 1 calc R . . . .
C6 C 0.2481(5) 0.2365(4) 1.0544(3) 0.0503(12) Uani 1 1 d . . . . .
H6 H 0.183450 0.252763 1.094821 0.060 Uiso 1 1 calc R . . . .
C7 C 0.3180(5) 0.3230(4) 1.0002(3) 0.0443(11) Uani 1 1 d . . . . .
C8 C 0.2925(4) 0.4318(4) 1.0018(3) 0.0423(11) Uani 1 1 d . . . . .
H8 H 0.228108 0.449206 1.041968 0.051 Uiso 1 1 calc R . . . .
C9 C 0.3580(4) 0.5162(4) 0.9467(3) 0.0379(10) Uani 1 1 d . . . . .
C10 C 0.4586(4) 0.4900(4) 0.8875(3) 0.0418(11) Uani 1 1 d . . . . .
C11 C 0.5240(4) 0.5791(4) 0.8316(2) 0.0375(10) Uani 1 1 d . . . . .
C12 C 0.4929(4) 0.6851(4) 0.8333(3) 0.0380(10) Uani 1 1 d . . . . .
C13 C 0.3892(4) 0.7121(4) 0.8908(3) 0.0365(10) Uani 1 1 d . . . . .
C14 C 0.3243(4) 0.6282(4) 0.9466(2) 0.0375(10) Uani 1 1 d . . . . .
C15 C 0.3479(5) 0.8301(4) 0.8916(3) 0.0395(10) Uani 1 1 d . . . . .
H15A H 0.271132 0.831174 0.932585 0.047 Uiso 1 1 calc R . . . .
H15B H 0.420534 0.855949 0.908370 0.047 Uiso 1 1 calc R . . . .
C16 C 0.5724(4) 0.7736(4) 0.7775(3) 0.0380(10) Uani 1 1 d . . . . .
H16A H 0.617582 0.802371 0.810639 0.046 Uiso 1 1 calc R . . . .
H16B H 0.641109 0.739000 0.744458 0.046 Uiso 1 1 calc R . . . .
C17 C 0.4131(4) 0.9530(4) 0.7498(3) 0.0373(10) Uani 1 1 d . . . . .
C18 C 0.3330(4) 1.0123(3) 0.6762(3) 0.0332(9) Uani 1 1 d . . . . .
C19 C 0.4893(5) 1.0276(4) 0.7730(3) 0.0445(11) Uani 1 1 d . . . . .
H19A H 0.552399 0.982187 0.810024 0.067 Uiso 1 1 calc GR . . . .
H19B H 0.427998 1.075168 0.799396 0.067 Uiso 1 1 calc GR . . . .
H19C H 0.536561 1.073569 0.724454 0.067 Uiso 1 1 calc GR . . . .
C20 C 0.3301(5) 1.1361(4) 0.6422(3) 0.0469(11) Uani 1 1 d . . . . .
H20A H 0.419851 1.154782 0.622857 0.070 Uiso 1 1 calc GR . . . .
H20B H 0.292791 1.170245 0.684377 0.070 Uiso 1 1 calc GR . . . .
H20C H 0.275957 1.163849 0.597390 0.070 Uiso 1 1 calc GR . . . .
C21 C 0.1955(4) 0.9151(3) 0.7876(2) 0.0344(9) Uani 1 1 d . . . . .
C22 C 0.4782(4) 0.8675(3) 0.6479(3) 0.0330(9) Uani 1 1 d . . . . .
C23 C 0.0947(4) 1.0024(4) 0.6602(3) 0.0376(10) Uani 1 1 d . . . . .
H23A H 0.094666 1.078195 0.622173 0.045 Uiso 1 1 calc R . . . .
H23B H 0.010397 0.999667 0.695540 0.045 Uiso 1 1 calc R . . . .
C24 C 0.1015(4) 0.9228(3) 0.6128(3) 0.0344(9) Uani 1 1 d . . . . .
C25 C -0.0017(4) 0.8633(3) 0.6240(3) 0.0355(10) Uani 1 1 d . . . . .
C26 C -0.0095(4) 0.7945(3) 0.5757(3) 0.0343(9) Uani 1 1 d . . . . .
C27 C -0.1187(4) 0.7416(3) 0.5828(3) 0.0396(10) Uani 1 1 d . . . . .
H27 H -0.189258 0.746885 0.623279 0.047 Uiso 1 1 calc R . . . .
C28 C -0.1269(4) 0.6803(3) 0.5312(3) 0.0388(10) Uani 1 1 d . . . . .
C29 C -0.2397(4) 0.6258(4) 0.5372(3) 0.0466(12) Uani 1 1 d . . . . .
H29 H -0.310803 0.629641 0.577674 0.056 Uiso 1 1 calc R . . . .
C30 C -0.2456(5) 0.5691(4) 0.4857(3) 0.0504(13) Uani 1 1 d . . . . .
H30 H -0.321465 0.533976 0.490184 0.060 Uiso 1 1 calc R . . . .
C31 C -0.1427(5) 0.5610(4) 0.4260(3) 0.0545(14) Uani 1 1 d . . . . .
H31 H -0.149416 0.520681 0.390488 0.065 Uiso 1 1 calc R . . . .
C32 C -0.0308(5) 0.6112(4) 0.4179(3) 0.0482(12) Uani 1 1 d . . . . .
H32 H 0.038974 0.604785 0.377258 0.058 Uiso 1 1 calc R . . . .
C33 C -0.0204(4) 0.6723(3) 0.4706(3) 0.0411(11) Uani 1 1 d . . . . .
C34 C 0.0908(4) 0.7227(3) 0.4655(3) 0.0386(10) Uani 1 1 d . . . . .
H34 H 0.161879 0.715711 0.425689 0.046 Uiso 1 1 calc R . . . .
C35 C 0.1018(4) 0.7827(3) 0.5164(3) 0.0367(10) Uani 1 1 d . . . . .
C36 C 0.2129(4) 0.8371(3) 0.5123(3) 0.0357(9) Uani 1 1 d . . . . .
C37 C 0.2140(4) 0.9075(3) 0.5566(2) 0.0319(9) Uani 1 1 d . . . . .
C38 C 0.3317(4) 0.9701(4) 0.5444(3) 0.0367(10) Uani 1 1 d . . . . .
H38A H 0.399564 0.945598 0.505564 0.044 Uiso 1 1 calc R . . . .
H38B H 0.303781 1.049689 0.519614 0.044 Uiso 1 1 calc R . . . .
C39 C 0.3994(4) 0.7168(4) 0.4823(3) 0.0425(11) Uani 1 1 d . . . . .
H39A H 0.445706 0.697651 0.434916 0.064 Uiso 1 1 calc GR . . . .
H39B H 0.343032 0.659850 0.513367 0.064 Uiso 1 1 calc GR . . . .
H39C H 0.463587 0.721519 0.516047 0.064 Uiso 1 1 calc GR . . . .
C40 C -0.2037(4) 0.9578(4) 0.6604(3) 0.0449(11) Uani 1 1 d . . . . .
H40A H -0.244719 0.950741 0.616132 0.067 Uiso 1 1 calc GR . . . .
H40B H -0.165031 1.027485 0.642640 0.067 Uiso 1 1 calc GR . . . .
H40C H -0.270441 0.957277 0.706422 0.067 Uiso 1 1 calc GR . . . .
C41 C 0.7466(5) 0.5189(5) 0.7940(3) 0.0584(14) Uani 1 1 d . . . . .
H41A H 0.801300 0.492142 0.751931 0.088 Uiso 1 1 calc GR . . . .
H41B H 0.745470 0.459425 0.845311 0.088 Uiso 1 1 calc GR . . . .
H41C H 0.782878 0.581593 0.799364 0.088 Uiso 1 1 calc GR . . . .
C42 C 0.0990(5) 0.6600(4) 0.9930(3) 0.0537(13) Uani 1 1 d . . . . .
H42A H 0.077581 0.728720 0.950141 0.081 Uiso 1 1 calc GR . . . .
H42B H 0.042253 0.661114 1.042722 0.081 Uiso 1 1 calc GR . . . .
H42C H 0.084902 0.596925 0.976975 0.081 Uiso 1 1 calc GR . . . .
O7 O 0.0222(4) 0.6735(3) 0.8152(2) 0.0619(10) Uani 1 1 d . . . . .
H7 H 0.039815 0.738572 0.803901 0.093 Uiso 1 1 calc GR . . . .
O8 O 0.4339(5) 0.3161(3) 0.7163(3) 0.0748(12) Uani 1 1 d . . . . .
O9 O 0.5085(4) 0.4644(3) 0.6347(3) 0.0706(11) Uani 1 1 d . . . . .
N5 N 0.4284(5) 0.4171(4) 0.6885(3) 0.0551(11) Uani 1 1 d . . . . .
C43 C 0.3228(5) 0.4830(4) 0.7215(3) 0.0464(11) Uani 1 1 d . . . . .
C44 C 0.3300(5) 0.5969(4) 0.7016(3) 0.0458(11) Uani 1 1 d . . . . .
H44 H 0.402439 0.629434 0.667332 0.055 Uiso 1 1 calc R . . . .
C45 C 0.2291(5) 0.6600(4) 0.7332(3) 0.0454(11) Uani 1 1 d . . . . .
H45 H 0.231732 0.737253 0.719966 0.054 Uiso 1 1 calc R . . . .
C46 C 0.1237(5) 0.6127(4) 0.7839(3) 0.0500(12) Uani 1 1 d . . . . .
C47 C 0.1195(5) 0.5017(4) 0.8022(3) 0.0539(13) Uani 1 1 d . . . . .
H47 H 0.046655 0.469541 0.836293 0.065 Uiso 1 1 calc R . . . .
C48 C 0.2191(6) 0.4349(4) 0.7720(3) 0.0555(13) Uani 1 1 d . . . . .
H48 H 0.215949 0.357585 0.785969 0.067 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C49 1.830(9) . ?
Cl2 C49 1.701(7) . ?
Cl3 C49 1.722(8) . ?
C49 H49 1.0000 . ?
O1 C14 1.363(5) . ?
O1 C42 1.439(6) . ?
O2 C11 1.382(5) . ?
O2 C41 1.427(6) . ?
O3 C21 1.230(5) . ?
O4 C22 1.226(5) . ?
O5 C25 1.383(5) . ?
O5 C40 1.410(5) . ?
O6 C36 1.391(5) . ?
O6 C39 1.442(5) . ?
N1 C15 1.452(6) . ?
N1 C17 1.457(5) . ?
N1 C21 1.364(5) . ?
N2 C16 1.471(5) . ?
N2 C17 1.448(5) . ?
N2 C22 1.372(5) . ?
N3 C18 1.460(5) . ?
N3 C21 1.361(6) . ?
N3 C23 1.458(5) . ?
N4 C18 1.455(5) . ?
N4 C22 1.359(5) . ?
N4 C38 1.454(5) . ?
C1 H1 0.9500 . ?
C1 C2 1.390(7) . ?
C1 C10 1.383(6) . ?
C2 C3 1.435(7) . ?
C2 C7 1.442(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.364(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.437(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.345(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.428(7) . ?
C7 C8 1.392(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.393(6) . ?
C9 C10 1.437(6) . ?
C9 C14 1.427(6) . ?
C10 C11 1.437(7) . ?
C11 C12 1.359(6) . ?
C12 C13 1.439(6) . ?
C12 C16 1.509(6) . ?
C13 C14 1.391(6) . ?
C13 C15 1.514(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.565(6) . ?
C17 C19 1.522(6) . ?
C18 C20 1.510(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.505(6) . ?
C24 C25 1.368(6) . ?
C24 C37 1.439(6) . ?
C25 C26 1.431(6) . ?
C26 C27 1.384(6) . ?
C26 C35 1.455(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.403(6) . ?
C28 C29 1.432(6) . ?
C28 C33 1.428(7) . ?
C29 H29 0.9500 . ?
C29 C30 1.349(7) . ?
C30 H30 0.9500 . ?
C30 C31 1.393(8) . ?
C31 H31 0.9500 . ?
C31 C32 1.385(7) . ?
C32 H32 0.9500 . ?
C32 C33 1.422(6) . ?
C33 C34 1.390(6) . ?
C34 H34 0.9500 . ?
C34 C35 1.387(6) . ?
C35 C36 1.423(6) . ?
C36 C37 1.377(6) . ?
C37 C38 1.520(5) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
O7 H7 0.8400 . ?
O7 C46 1.362(6) . ?
O8 N5 1.228(6) . ?
O9 N5 1.228(6) . ?
N5 C43 1.441(7) . ?
C43 C44 1.406(7) . ?
C43 C48 1.377(7) . ?
C44 H44 0.9500 . ?
C44 C45 1.377(7) . ?
C45 H45 0.9500 . ?
C45 C46 1.389(7) . ?
C46 C47 1.366(7) . ?
C47 H47 0.9500 . ?
C47 C48 1.387(8) . ?
C48 H48 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
Cl1 C49 H49 110.7 . . ?
Cl2 C49 Cl1 108.0(4) . . ?
Cl2 C49 Cl3 114.9(5) . . ?
Cl2 C49 H49 110.7 . . ?
Cl3 C49 Cl1 101.2(4) . . ?
Cl3 C49 H49 110.7 . . ?
C14 O1 C42 115.3(3) . . ?
C11 O2 C41 115.4(3) . . ?
C25 O5 C40 114.8(3) . . ?
C36 O6 C39 114.1(3) . . ?
C15 N1 C17 122.3(3) . . ?
C21 N1 C15 122.7(4) . . ?
C21 N1 C17 111.7(3) . . ?
C17 N2 C16 123.1(3) . . ?
C22 N2 C16 121.9(3) . . ?
C22 N2 C17 113.3(3) . . ?
C21 N3 C18 113.7(3) . . ?
C21 N3 C23 123.0(4) . . ?
C23 N3 C18 122.6(3) . . ?
C22 N4 C18 111.9(3) . . ?
C22 N4 C38 121.8(3) . . ?
C38 N4 C18 122.8(3) . . ?
C2 C1 H1 118.8 . . ?
C10 C1 H1 118.8 . . ?
C10 C1 C2 122.3(4) . . ?
C1 C2 C3 122.8(5) . . ?
C1 C2 C7 119.5(4) . . ?
C3 C2 C7 117.7(4) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.9(5) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 H4 119.5 . . ?
C3 C4 C5 120.9(5) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.7(5) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 H6 119.1 . . ?
C5 C6 C7 121.7(5) . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C2 119.1(4) . . ?
C8 C7 C2 118.0(4) . . ?
C8 C7 C6 122.9(5) . . ?
C7 C8 H8 118.8 . . ?
C7 C8 C9 122.3(4) . . ?
C9 C8 H8 118.8 . . ?
C8 C9 C10 119.2(4) . . ?
C8 C9 C14 121.2(4) . . ?
C14 C9 C10 119.6(4) . . ?
C1 C10 C9 118.6(4) . . ?
C1 C10 C11 123.7(4) . . ?
C11 C10 C9 117.7(4) . . ?
O2 C11 C10 116.9(4) . . ?
C12 C11 O2 120.9(4) . . ?
C12 C11 C10 122.1(4) . . ?
C11 C12 C13 120.3(4) . . ?
C11 C12 C16 119.6(4) . . ?
C13 C12 C16 120.0(4) . . ?
C12 C13 C15 121.5(4) . . ?
C14 C13 C12 119.5(4) . . ?
C14 C13 C15 119.0(4) . . ?
O1 C14 C9 118.6(4) . . ?
O1 C14 C13 120.4(4) . . ?
C13 C14 C9 120.8(4) . . ?
N1 C15 C13 114.7(3) . . ?
N1 C15 H15A 108.6 . . ?
N1 C15 H15B 108.6 . . ?
C13 C15 H15A 108.6 . . ?
C13 C15 H15B 108.6 . . ?
H15A C15 H15B 107.6 . . ?
N2 C16 C12 115.8(3) . . ?
N2 C16 H16A 108.3 . . ?
N2 C16 H16B 108.3 . . ?
C12 C16 H16A 108.3 . . ?
C12 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
N1 C17 C18 103.9(3) . . ?
N1 C17 C19 110.9(4) . . ?
N2 C17 N1 111.9(3) . . ?
N2 C17 C18 102.0(3) . . ?
N2 C17 C19 112.7(4) . . ?
C19 C17 C18 114.8(4) . . ?
N3 C18 C17 101.4(3) . . ?
N3 C18 C20 111.4(3) . . ?
N4 C18 N3 110.9(3) . . ?
N4 C18 C17 103.7(3) . . ?
N4 C18 C20 111.8(4) . . ?
C20 C18 C17 116.9(3) . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 N1 126.6(4) . . ?
O3 C21 N3 125.1(4) . . ?
N3 C21 N1 108.2(4) . . ?
O4 C22 N2 125.3(4) . . ?
O4 C22 N4 126.4(4) . . ?
N4 C22 N2 108.3(3) . . ?
N3 C23 H23A 108.7 . . ?
N3 C23 H23B 108.7 . . ?
N3 C23 C24 114.3(3) . . ?
H23A C23 H23B 107.6 . . ?
C24 C23 H23A 108.7 . . ?
C24 C23 H23B 108.7 . . ?
C25 C24 C23 118.9(4) . . ?
C25 C24 C37 119.6(4) . . ?
C37 C24 C23 121.5(4) . . ?
O5 C25 C26 117.1(3) . . ?
C24 C25 O5 120.3(4) . . ?
C24 C25 C26 122.5(4) . . ?
C25 C26 C35 117.7(4) . . ?
C27 C26 C25 122.4(4) . . ?
C27 C26 C35 119.9(4) . . ?
C26 C27 H27 119.5 . . ?
C26 C27 C28 121.1(4) . . ?
C28 C27 H27 119.5 . . ?
C27 C28 C29 121.9(4) . . ?
C27 C28 C33 119.2(4) . . ?
C33 C28 C29 118.9(4) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.4(5) . . ?
C30 C29 H29 119.8 . . ?
C29 C30 H30 119.3 . . ?
C29 C30 C31 121.3(4) . . ?
C31 C30 H30 119.3 . . ?
C30 C31 H31 119.6 . . ?
C32 C31 C30 120.7(5) . . ?
C32 C31 H31 119.6 . . ?
C31 C32 H32 120.0 . . ?
C31 C32 C33 120.0(5) . . ?
C33 C32 H32 120.0 . . ?
C32 C33 C28 118.7(4) . . ?
C34 C33 C28 119.3(4) . . ?
C34 C33 C32 122.0(4) . . ?
C33 C34 H34 118.8 . . ?
C35 C34 C33 122.5(4) . . ?
C35 C34 H34 118.8 . . ?
C34 C35 C26 117.9(4) . . ?
C34 C35 C36 124.2(4) . . ?
C36 C35 C26 117.9(4) . . ?
O6 C36 C35 116.9(4) . . ?
C37 C36 O6 120.3(4) . . ?
C37 C36 C35 122.7(4) . . ?
C24 C37 C38 120.9(4) . . ?
C36 C37 C24 119.1(4) . . ?
C36 C37 C38 119.9(4) . . ?
N4 C38 C37 115.7(3) . . ?
N4 C38 H38A 108.4 . . ?
N4 C38 H38B 108.4 . . ?
C37 C38 H38A 108.4 . . ?
C37 C38 H38B 108.4 . . ?
H38A C38 H38B 107.4 . . ?
O6 C39 H39A 109.5 . . ?
O6 C39 H39B 109.5 . . ?
O6 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O5 C40 H40A 109.5 . . ?
O5 C40 H40B 109.5 . . ?
O5 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O2 C41 H41A 109.5 . . ?
O2 C41 H41B 109.5 . . ?
O2 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O1 C42 H42A 109.5 . . ?
O1 C42 H42B 109.5 . . ?
O1 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C46 O7 H7 109.5 . . ?
O8 N5 C43 117.9(5) . . ?
O9 N5 O8 123.5(5) . . ?
O9 N5 C43 118.6(4) . . ?
C44 C43 N5 118.0(5) . . ?
C48 C43 N5 120.7(5) . . ?
C48 C43 C44 121.3(5) . . ?
C43 C44 H44 121.0 . . ?
C45 C44 C43 118.1(5) . . ?
C45 C44 H44 121.0 . . ?
C44 C45 H45 119.4 . . ?
C44 C45 C46 121.2(5) . . ?
C46 C45 H45 119.4 . . ?
O7 C46 C45 122.2(5) . . ?
O7 C46 C47 118.4(5) . . ?
C47 C46 C45 119.3(5) . . ?
C46 C47 H47 119.3 . . ?
C46 C47 C48 121.4(5) . . ?
C48 C47 H47 119.3 . . ?
C43 C48 C47 118.6(5) . . ?
C43 C48 H48 120.7 . . ?
C47 C48 H48 120.7 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
