# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jdk7862m
_database_code_depnum_ccdc_archive 'CCDC 1566555'
_audit_update_record             
;
2017-08-08 deposited with the CCDC.
2018-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C53 H49 Cl2 N3 O3'
_chemical_formula_weight         846.85

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

loop_
_symmetry_equiv_pos_as_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                   11.5660(10)
_cell_length_b                   31.513(3)
_cell_length_c                   12.0437(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.279(2)
_cell_angle_gamma                90.00
_cell_volume                     4386.3(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3864
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      28.23

_exptl_crystal_description       blocks
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9363
_exptl_absorpt_correction_T_max  0.9826
_exptl_absorpt_process_details   'BRUKER SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD DIFFARCTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19517
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_sigmaI/netI    0.1078
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.29
_diffrn_reflns_theta_max         24.00
_reflns_number_total             6883
_reflns_number_gt                5135
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER SMART'
_computing_cell_refinement       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0276P)²+13.0164P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6883
_refine_ls_number_parameters     551
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.1192
_refine_ls_wR_factor_ref         0.2111
_refine_ls_wR_factor_gt          0.1990
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_restrained_S_all      1.286
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl2 Cl 0.45089(17) 0.06162(8) 1.0304(2) 0.0652(7) Uani 1 1 d . . .
Cl1 Cl 0.56220(18) 0.07682(9) 0.82146(18) 0.0706(8) Uani 1 1 d . . .
O1 O 0.8357(3) 0.07573(13) 0.0022(3) 0.0220(10) Uani 1 1 d . . .
O2 O 0.9417(3) 0.18569(13) 0.1908(4) 0.0296(11) Uani 1 1 d . . .
O3 O 0.7388(4) 0.25160(14) 0.3208(4) 0.0392(13) Uani 1 1 d . . .
N1 N 1.0832(4) 0.12825(14) 0.0305(4) 0.0116(11) Uani 1 1 d . . .
N2 N 0.9576(4) 0.16221(15) -0.0737(4) 0.0141(11) Uani 1 1 d . . .
N3 N 0.8265(4) 0.19339(16) 0.3931(4) 0.0237(12) Uani 1 1 d . . .
H3 H 0.8638 0.1830 0.4500 0.028 Uiso 1 1 calc R . .
C40 C 0.6453(5) 0.11477(19) 0.4047(5) 0.0169(14) Uani 1 1 d . . .
C9 C 0.9704(4) 0.13228(18) 0.0057(4) 0.0107(12) Uiso 1 1 d . . .
C6 C 1.1361(4) 0.09780(18) 0.1065(5) 0.0148(13) Uani 1 1 d . . .
C41 C 0.5556(5) 0.1435(2) 0.4046(5) 0.0254(16) Uani 1 1 d . . .
H41 H 0.5617 0.1686 0.3643 0.031 Uiso 1 1 calc R . .
C27 C 0.8689(5) 0.1586(2) 0.2118(5) 0.0194(14) Uani 1 1 d . . .
C22 C 0.8743(4) 0.10649(19) 0.0576(5) 0.0146(13) Uani 1 1 d . . .
C24 C 0.7521(5) 0.09556(19) 0.2269(5) 0.0172(14) Uani 1 1 d . . .
H24 H 0.6759 0.0977 0.1888 0.021 Uiso 1 1 calc R . .
C23 C 0.8404(4) 0.11933(18) 0.1612(5) 0.0132(13) Uani 1 1 d . . .
C34 C 0.8476(5) -0.0784(2) 0.3654(5) 0.0195(14) Uani 1 1 d . . .
C25 C 0.7516(5) 0.12086(19) 0.3398(5) 0.0204(14) Uani 1 1 d . . .
H25 H 0.8167 0.1101 0.3861 0.024 Uiso 1 1 calc R . .
C46 C 0.8089(5) 0.2355(2) 0.3864(5) 0.0228(15) Uani 1 1 d . . .
C33 C 0.8900(5) 0.03655(19) 0.2854(5) 0.0183(14) Uani 1 1 d . . .
H33 H 0.9500 0.0562 0.2842 0.022 Uiso 1 1 calc R . .
C12 C 0.7211(5) 0.16418(19) -0.2898(5) 0.0210(15) Uani 1 1 d . . .
H12 H 0.6933 0.1478 -0.3493 0.025 Uiso 1 1 calc R . .
C5 C 1.1370(5) 0.0553(2) 0.0750(5) 0.0187(14) Uani 1 1 d . . .
C26 C 0.7832(5) 0.1654(2) 0.3056(5) 0.0220(15) Uani 1 1 d . . .
H26 H 0.7133 0.1785 0.2720 0.026 Uiso 1 1 calc R . .
C11 C 0.8149(5) 0.1495(2) -0.2259(5) 0.0198(15) Uani 1 1 d . . .
C31 C 0.8259(5) -0.03469(19) 0.3227(5) 0.0186(14) Uani 1 1 d . . .
C3 C 1.2286(5) 0.0388(2) 0.2545(5) 0.0283(16) Uani 1 1 d . . .
C30 C 0.7163(5) -0.02287(19) 0.2812(5) 0.0190(14) Uani 1 1 d . . .
H30 H 0.6575 -0.0430 0.2771 0.023 Uiso 1 1 calc R . .
C42 C 0.4567(5) 0.1362(2) 0.4626(5) 0.0266(16) Uani 1 1 d . . .
H42 H 0.3974 0.1562 0.4613 0.032 Uiso 1 1 calc R . .
C10 C 0.8526(4) 0.17435(19) -0.1356(5) 0.0157(14) Uani 1 1 d . . .
C29 C 0.6934(5) 0.01824(19) 0.2458(5) 0.0174(14) Uani 1 1 d . . .
H29 H 0.6194 0.0254 0.2191 0.021 Uiso 1 1 calc R . .
C32 C 0.9135(5) -0.00399(19) 0.3224(5) 0.0193(14) Uani 1 1 d . . .
H32 H 0.9881 -0.0111 0.3475 0.023 Uiso 1 1 calc R . .
C7 C 1.1430(5) 0.15736(19) -0.0326(5) 0.0207(15) Uani 1 1 d . . .
H7 H 1.2227 0.1614 -0.0307 0.025 Uiso 1 1 calc R . .
C28 C 0.7807(4) 0.04896(19) 0.2502(4) 0.0160(14) Uani 1 1 d . . .
C43 C 0.4467(5) 0.0995(2) 0.5218(5) 0.0282(17) Uani 1 1 d . . .
H43 H 0.3800 0.0943 0.5601 0.034 Uiso 1 1 calc R . .
C44 C 0.5341(5) 0.0706(2) 0.5249(5) 0.0293(17) Uani 1 1 d . . .
H44 H 0.5272 0.0457 0.5654 0.035 Uiso 1 1 calc R . .
C35 C 0.7999(5) -0.1142(2) 0.3111(5) 0.0244(15) Uani 1 1 d . . .
H35 H 0.7566 -0.1108 0.2450 0.029 Uiso 1 1 calc R . .
C4 C 1.1821(5) 0.0264(2) 0.1524(5) 0.0237(15) Uani 1 1 d . . .
H4 H 1.1808 -0.0024 0.1347 0.028 Uiso 1 1 calc R . .
C2 C 1.2347(5) 0.0818(2) 0.2769(5) 0.0256(16) Uani 1 1 d . . .
H2 H 1.2713 0.0906 0.3431 0.031 Uiso 1 1 calc R . .
C1 C 1.1890(4) 0.1125(2) 0.2055(5) 0.0183(14) Uani 1 1 d . . .
C18 C 1.0953(5) 0.0415(2) -0.0399(5) 0.0232(15) Uani 1 1 d . . .
H18A H 1.0122 0.0418 -0.0446 0.035 Uiso 1 1 calc R . .
H18B H 1.1226 0.0134 -0.0541 0.035 Uiso 1 1 calc R . .
H18C H 1.1245 0.0607 -0.0941 0.035 Uiso 1 1 calc R . .
C19 C 0.8742(5) 0.1085(2) -0.2530(5) 0.0260(16) Uani 1 1 d . . .
H19A H 0.9563 0.1131 -0.2539 0.039 Uiso 1 1 calc R . .
H19B H 0.8465 0.0987 -0.3247 0.039 Uiso 1 1 calc R . .
H19C H 0.8578 0.0876 -0.1978 0.039 Uiso 1 1 calc R . .
C13 C 0.6677(5) 0.2021(2) -0.2684(5) 0.0262(16) Uani 1 1 d . . .
C45 C 0.6332(5) 0.0784(2) 0.4674(5) 0.0217(15) Uani 1 1 d . . .
H45 H 0.6931 0.0586 0.4709 0.026 Uiso 1 1 calc R . .
C15 C 0.8013(5) 0.21312(19) -0.1115(5) 0.0217(15) Uani 1 1 d . . .
C8 C 1.0657(5) 0.17822(19) -0.0958(5) 0.0182(14) Uani 1 1 d . . .
H8 H 1.0813 0.1997 -0.1460 0.022 Uiso 1 1 calc R . .
C52 C 0.9123(6) 0.2500(2) 0.5705(6) 0.0417(19) Uani 1 1 d . . .
H52 H 0.8823 0.2252 0.5995 0.050 Uiso 1 1 calc R . .
C14 C 0.7084(5) 0.2260(2) -0.1790(5) 0.0285(16) Uani 1 1 d . . .
H14 H 0.6722 0.2515 -0.1637 0.034 Uiso 1 1 calc R . .
C48 C 0.9260(6) 0.3000(2) 0.4220(6) 0.0373(18) Uani 1 1 d . . .
H48 H 0.9049 0.3089 0.3504 0.045 Uiso 1 1 calc R . .
C38 C 0.9268(5) -0.1251(2) 0.5077(6) 0.0317(17) Uani 1 1 d . . .
H38 H 0.9701 -0.1289 0.5737 0.038 Uiso 1 1 calc R . .
C37 C 0.8792(5) -0.1593(2) 0.4532(6) 0.0319(17) Uani 1 1 d . . .
H37 H 0.8895 -0.1863 0.4831 0.038 Uiso 1 1 calc R . .
C36 C 0.8163(5) -0.1544(2) 0.3544(6) 0.0280(16) Uani 1 1 d . . .
H36 H 0.7851 -0.1779 0.3173 0.034 Uiso 1 1 calc R . .
C16 C 1.2018(5) 0.1587(2) 0.2327(6) 0.0317(17) Uani 1 1 d . . .
H16A H 1.2669 0.1701 0.1956 0.048 Uiso 1 1 calc R . .
H16B H 1.2139 0.1621 0.3115 0.048 Uiso 1 1 calc R . .
H16C H 1.1329 0.1735 0.2085 0.048 Uiso 1 1 calc R . .
C39 C 0.9104(5) -0.0846(2) 0.4645(5) 0.0258(15) Uani 1 1 d . . .
H39 H 0.9419 -0.0614 0.5025 0.031 Uiso 1 1 calc R . .
C21 C 0.8442(7) 0.2411(2) -0.0167(6) 0.046(2) Uani 1 1 d . . .
H21A H 0.8662 0.2238 0.0463 0.069 Uiso 1 1 calc R . .
H21B H 0.7837 0.2602 0.0031 0.069 Uiso 1 1 calc R . .
H21C H 0.9098 0.2572 -0.0392 0.069 Uiso 1 1 calc R . .
C20 C 0.5704(6) 0.2186(2) -0.3439(6) 0.043(2) Uani 1 1 d . . .
H20A H 0.5389 0.2439 -0.3126 0.065 Uiso 1 1 calc R . .
H20B H 0.5108 0.1974 -0.3515 0.065 Uiso 1 1 calc R . .
H20C H 0.5994 0.2249 -0.4156 0.065 Uiso 1 1 calc R . .
C17 C 1.2753(6) 0.0069(2) 0.3379(6) 0.044(2) Uani 1 1 d . . .
H17A H 1.2605 -0.0213 0.3104 0.066 Uiso 1 1 calc R . .
H17B H 1.2380 0.0107 0.4070 0.066 Uiso 1 1 calc R . .
H17C H 1.3572 0.0109 0.3494 0.066 Uiso 1 1 calc R . .
C51 C 0.9858(8) 0.2754(3) 0.6353(7) 0.068(3) Uani 1 1 d . . .
H51 H 1.0066 0.2673 0.7076 0.082 Uiso 1 1 calc R . .
C49 C 0.9987(7) 0.3242(3) 0.4881(8) 0.057(2) Uani 1 1 d . . .
H49 H 1.0286 0.3492 0.4599 0.068 Uiso 1 1 calc R . .
C50 C 1.0280(9) 0.3127(3) 0.5928(9) 0.080(3) Uani 1 1 d . . .
H50 H 1.0767 0.3298 0.6366 0.097 Uiso 1 1 calc R . .
C47 C 0.8838(5) 0.2619(2) 0.4626(5) 0.0228(15) Uani 1 1 d . . .
C62 C 0.5749(6) 0.0541(3) 0.9516(7) 0.061(3) Uani 1 1 d . . .
H62A H 0.6415 0.0662 0.9917 0.074 Uiso 1 1 calc R . .
H62B H 0.5887 0.0239 0.9436 0.074 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
Cl2 C62 1.767(8) . ?
Cl1 C62 1.725(9) . ?
O1 C22 1.249(7) . ?
O2 C27 1.232(7) . ?
O3 C46 1.220(7) . ?
N1 C9 1.333(6) . ?
N1 C7 1.393(7) . ?
N1 C6 1.445(7) . ?
N2 C9 1.347(7) . ?
N2 C8 1.385(6) . ?
N2 C10 1.451(7) . ?
N3 C46 1.346(8) . ?
N3 C26 1.449(7) . ?
N3 H3 0.8600 . ?
C40 C41 1.378(8) . ?
C40 C45 1.383(8) . ?
C40 C25 1.495(8) . ?
C9 C22 1.530(7) . ?
C6 C5 1.391(8) . ?
C6 C1 1.397(8) . ?
C41 C42 1.383(8) . ?
C41 H41 0.9300 . ?
C27 C23 1.412(8) . ?
C27 C26 1.547(8) . ?
C22 C23 1.383(8) . ?
C24 C23 1.515(7) . ?
C24 C28 1.529(8) . ?
C24 C25 1.576(8) . ?
C24 H24 0.9800 . ?
C34 C39 1.386(8) . ?
C34 C35 1.406(8) . ?
C34 C31 1.489(8) . ?
C25 C26 1.511(8) . ?
C25 H25 0.9800 . ?
C46 C47 1.489(8) . ?
C33 C28 1.374(7) . ?
C33 C32 1.377(8) . ?
C33 H33 0.9300 . ?
C12 C13 1.375(8) . ?
C12 C11 1.384(8) . ?
C12 H12 0.9300 . ?
C5 C4 1.391(8) . ?
C5 C18 1.512(8) . ?
C26 H26 0.9800 . ?
C11 C10 1.395(8) . ?
C11 C19 1.506(8) . ?
C31 C30 1.394(8) . ?
C31 C32 1.401(8) . ?
C3 C4 1.379(8) . ?
C3 C2 1.384(9) . ?
C3 C17 1.507(9) . ?
C30 C29 1.386(8) . ?
C30 H30 0.9300 . ?
C42 C43 1.366(9) . ?
C42 H42 0.9300 . ?
C10 C15 1.394(8) . ?
C29 C28 1.399(8) . ?
C29 H29 0.9300 . ?
C32 H32 0.9300 . ?
C7 C8 1.326(8) . ?
C7 H7 0.9300 . ?
C43 C44 1.360(8) . ?
C43 H43 0.9300 . ?
C44 C45 1.385(8) . ?
C44 H44 0.9300 . ?
C35 C36 1.378(9) . ?
C35 H35 0.9300 . ?
C4 H4 0.9300 . ?
C2 C1 1.385(8) . ?
C2 H2 0.9300 . ?
C1 C16 1.497(8) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C13 C14 1.380(9) . ?
C13 C20 1.511(8) . ?
C45 H45 0.9300 . ?
C15 C14 1.382(8) . ?
C15 C21 1.512(9) . ?
C8 H8 0.9300 . ?
C52 C47 1.378(9) . ?
C52 C51 1.386(10) . ?
C52 H52 0.9300 . ?
C14 H14 0.9300 . ?
C48 C49 1.368(10) . ?
C48 C47 1.392(9) . ?
C48 H48 0.9300 . ?
C38 C37 1.367(9) . ?
C38 C39 1.387(9) . ?
C38 H38 0.9300 . ?
C37 C36 1.379(9) . ?
C37 H37 0.9300 . ?
C36 H36 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C39 H39 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C51 C50 1.377(12) . ?
C51 H51 0.9300 . ?
C49 C50 1.343(11) . ?
C49 H49 0.9300 . ?
C50 H50 0.9300 . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?

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
C9 N1 C7 108.6(5) . . ?
C9 N1 C6 126.2(4) . . ?
C7 N1 C6 125.2(4) . . ?
C9 N2 C8 108.5(4) . . ?
C9 N2 C10 128.0(4) . . ?
C8 N2 C10 123.3(5) . . ?
C46 N3 C26 120.7(5) . . ?
C46 N3 H3 119.6 . . ?
C26 N3 H3 119.6 . . ?
C41 C40 C45 117.0(5) . . ?
C41 C40 C25 123.3(6) . . ?
C45 C40 C25 119.7(5) . . ?
N1 C9 N2 107.8(4) . . ?
N1 C9 C22 125.3(5) . . ?
N2 C9 C22 126.9(4) . . ?
C5 C6 C1 123.0(5) . . ?
C5 C6 N1 118.3(5) . . ?
C1 C6 N1 118.7(5) . . ?
C40 C41 C42 121.9(6) . . ?
C40 C41 H41 119.1 . . ?
C42 C41 H41 119.1 . . ?
O2 C27 C23 131.9(5) . . ?
O2 C27 C26 121.1(5) . . ?
C23 C27 C26 106.9(5) . . ?
O1 C22 C23 126.9(5) . . ?
O1 C22 C9 116.4(5) . . ?
C23 C22 C9 116.7(5) . . ?
C23 C24 C28 115.2(5) . . ?
C23 C24 C25 103.1(4) . . ?
C28 C24 C25 109.6(5) . . ?
C23 C24 H24 109.6 . . ?
C28 C24 H24 109.6 . . ?
C25 C24 H24 109.6 . . ?
C22 C23 C27 125.2(5) . . ?
C22 C23 C24 123.2(5) . . ?
C27 C23 C24 111.0(5) . . ?
C39 C34 C35 118.0(6) . . ?
C39 C34 C31 120.2(6) . . ?
C35 C34 C31 121.7(5) . . ?
C40 C25 C26 118.3(5) . . ?
C40 C25 C24 114.7(5) . . ?
C26 C25 C24 103.0(5) . . ?
C40 C25 H25 106.7 . . ?
C26 C25 H25 106.7 . . ?
C24 C25 H25 106.7 . . ?
O3 C46 N3 122.9(6) . . ?
O3 C46 C47 121.6(6) . . ?
N3 C46 C47 115.5(5) . . ?
C28 C33 C32 122.1(5) . . ?
C28 C33 H33 119.0 . . ?
C32 C33 H33 119.0 . . ?
C13 C12 C11 122.2(6) . . ?
C13 C12 H12 118.9 . . ?
C11 C12 H12 118.9 . . ?
C4 C5 C6 117.1(5) . . ?
C4 C5 C18 121.5(6) . . ?
C6 C5 C18 121.4(5) . . ?
N3 C26 C25 116.6(5) . . ?
N3 C26 C27 113.7(5) . . ?
C25 C26 C27 103.9(5) . . ?
N3 C26 H26 107.4 . . ?
C25 C26 H26 107.4 . . ?
C27 C26 H26 107.4 . . ?
C12 C11 C10 117.5(6) . . ?
C12 C11 C19 121.3(5) . . ?
C10 C11 C19 121.2(5) . . ?
C30 C31 C32 117.5(6) . . ?
C30 C31 C34 120.7(5) . . ?
C32 C31 C34 121.8(5) . . ?
C4 C3 C2 117.9(6) . . ?
C4 C3 C17 121.4(6) . . ?
C2 C3 C17 120.7(6) . . ?
C29 C30 C31 121.3(5) . . ?
C29 C30 H30 119.3 . . ?
C31 C30 H30 119.3 . . ?
C43 C42 C41 119.5(6) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C15 C10 C11 122.1(5) . . ?
C15 C10 N2 118.6(5) . . ?
C11 C10 N2 118.9(5) . . ?
C30 C29 C28 120.4(5) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C33 C32 C31 120.5(5) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C8 C7 N1 107.5(5) . . ?
C8 C7 H7 126.2 . . ?
N1 C7 H7 126.2 . . ?
C33 C28 C29 118.0(6) . . ?
C33 C28 C24 121.3(5) . . ?
C29 C28 C24 120.5(5) . . ?
C44 C43 C42 120.2(6) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 119.8(6) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C36 C35 C34 121.1(6) . . ?
C36 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C3 C4 C5 122.2(6) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C3 C2 C1 123.2(6) . . ?
C3 C2 H2 118.4 . . ?
C1 C2 H2 118.4 . . ?
C2 C1 C6 116.2(6) . . ?
C2 C1 C16 120.7(5) . . ?
C6 C1 C16 123.1(5) . . ?
C5 C18 H18A 109.5 . . ?
C5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C11 C19 H19A 109.5 . . ?
C11 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C11 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C12 C13 C14 118.5(6) . . ?
C12 C13 C20 121.0(6) . . ?
C14 C13 C20 120.4(6) . . ?
C40 C45 C44 121.5(6) . . ?
C40 C45 H45 119.2 . . ?
C44 C45 H45 119.2 . . ?
C14 C15 C10 117.5(6) . . ?
C14 C15 C21 119.8(6) . . ?
C10 C15 C21 122.7(5) . . ?
C7 C8 N2 107.6(5) . . ?
C7 C8 H8 126.2 . . ?
N2 C8 H8 126.2 . . ?
C47 C52 C51 119.6(7) . . ?
C47 C52 H52 120.2 . . ?
C51 C52 H52 120.2 . . ?
C13 C14 C15 122.2(6) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C49 C48 C47 119.5(7) . . ?
C49 C48 H48 120.2 . . ?
C47 C48 H48 120.2 . . ?
C37 C38 C39 119.9(6) . . ?
C37 C38 H38 120.0 . . ?
C39 C38 H38 120.0 . . ?
C38 C37 C36 121.0(6) . . ?
C38 C37 H37 119.5 . . ?
C36 C37 H37 119.5 . . ?
C35 C36 C37 119.3(6) . . ?
C35 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
C1 C16 H16A 109.5 . . ?
C1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C34 C39 C38 120.8(6) . . ?
C34 C39 H39 119.6 . . ?
C38 C39 H39 119.6 . . ?
C15 C21 H21A 109.5 . . ?
C15 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C15 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C13 C20 H20A 109.5 . . ?
C13 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C13 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C3 C17 H17A 109.5 . . ?
C3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C50 C51 C52 120.0(8) . . ?
C50 C51 H51 120.0 . . ?
C52 C51 H51 120.0 . . ?
C50 C49 C48 121.5(8) . . ?
C50 C49 H49 119.3 . . ?
C48 C49 H49 119.3 . . ?
C49 C50 C51 120.0(8) . . ?
C49 C50 H50 120.0 . . ?
C51 C50 H50 120.0 . . ?
C52 C47 C48 119.4(6) . . ?
C52 C47 C46 122.8(6) . . ?
C48 C47 C46 117.9(6) . . ?
Cl1 C62 Cl2 113.0(5) . . ?
Cl1 C62 H62A 109.0 . . ?
Cl2 C62 H62A 109.0 . . ?
Cl1 C62 H62B 109.0 . . ?
Cl2 C62 H62B 109.0 . . ?
H62A C62 H62B 107.8 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.072
####################################################################### 
# 
# 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_jdk851xm
_database_code_depnum_ccdc_archive 'CCDC 1568080'
_audit_update_record             
;
2017-08-10 deposited with the CCDC.
2018-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50.50 H49 Cl I N3 O5'
_chemical_formula_weight         940.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_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                   29.069(3)
_cell_length_b                   16.6470(18)
_cell_length_c                   23.834(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 124.203(2)
_cell_angle_gamma                90.00
_cell_volume                     9538.9(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5294
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      28.01

_exptl_crystal_description       BLOCKS
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3864
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.7896
_exptl_absorpt_correction_T_max  0.8993
_exptl_absorpt_process_details   'BRUKER SADABS'
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.194 0.250 243.1 45.3
2 0.155 0.093 0.414 7.4 -0.3
3 0.500 0.306 0.750 242.1 45.5
4 0.845 0.093 0.086 6.4 -0.2
5 0.345 0.406 0.586 6.7 -0.3
6 0.655 0.406 0.914 7.7 -0.2
7 0.500 0.694 0.250 243.1 45.3
8 0.000 0.806 0.750 242.1 45.5
9 0.345 0.593 0.086 6.4 -0.2
10 0.655 0.593 0.414 7.4 -0.3
11 0.155 0.906 0.914 7.7 -0.2
12 0.845 0.906 0.586 6.7 -0.3
_platon_squeeze_details          
; ?
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD DIFFARCTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28275
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         28.27
_reflns_number_total             11068
_reflns_number_gt                9292
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER SMART'
_computing_cell_refinement       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0494P)²+5.5501P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11068
_refine_ls_number_parameters     554
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0913
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.02359(5) 0.69101(6) 0.32277(6) 0.0828(3) Uani 1 1 d . . .
C54 C 0.0000 0.6330(3) 0.2500 0.0704(14) Uani 1 2 d S . .
H54A H -0.0300 0.5986 0.2421 0.084 Uiso 0.50 1 calc PR . .
H54B H 0.0300 0.5986 0.2579 0.084 Uiso 0.50 1 calc PR . .
I1 I 0.030665(6) 0.470735(9) 0.408600(7) 0.03148(6) Uani 1 1 d . . .
O3 O 0.13742(6) 0.57944(9) 0.66991(7) 0.0289(3) Uani 1 1 d . . .
O2 O 0.16486(6) 0.29207(9) 0.67919(7) 0.0280(3) Uani 1 1 d . . .
N3 N 0.11517(7) 0.45597(9) 0.62415(8) 0.0217(3) Uani 1 1 d . . .
C37 C 0.16222(9) 0.51980(12) 0.57254(11) 0.0252(4) Uani 1 1 d . . .
O1 O 0.08818(7) 0.13388(10) 0.50879(8) 0.0390(4) Uani 1 1 d . . .
C30 C 0.12601(8) 0.50950(12) 0.67364(10) 0.0227(4) Uani 1 1 d . . .
C44 C -0.01682(8) 0.25659(11) 0.48819(10) 0.0233(4) Uani 1 1 d . . .
O5 O -0.17427(7) 0.18431(11) 0.43441(9) 0.0432(4) Uani 1 1 d . . .
N1 N 0.20988(8) 0.13090(12) 0.65066(9) 0.0338(4) Uani 1 1 d . . .
C38 C 0.20997(9) 0.47221(13) 0.60585(11) 0.0295(4) Uani 1 1 d . . .
H38 H 0.2100 0.4240 0.6256 0.035 Uiso 1 1 calc R . .
O4 O 0.30665(7) 0.58752(11) 0.58775(9) 0.0462(4) Uani 1 1 d . . .
C29 C 0.07994(8) 0.42592(12) 0.51070(10) 0.0226(4) Uani 1 1 d . . .
H29 H 0.1086 0.3904 0.5149 0.027 Uiso 1 1 calc R . .
C24 C 0.11962(8) 0.30204(12) 0.62404(10) 0.0234(4) Uani 1 1 d . . .
C27 C 0.03891(8) 0.28916(12) 0.50714(10) 0.0224(4) Uani 1 1 d . . .
H27 H 0.0407 0.2858 0.4674 0.027 Uiso 1 1 calc R . .
C31 C 0.12558(8) 0.48450(12) 0.73407(10) 0.0241(4) Uani 1 1 d . . .
N2 N 0.14843(8) 0.09888(11) 0.67112(9) 0.0325(4) Uani 1 1 d . . .
C23 C 0.09051(8) 0.25045(12) 0.56673(10) 0.0235(4) Uani 1 1 d . . .
C34 C 0.13189(10) 0.45646(15) 0.85321(12) 0.0365(5) Uani 1 1 d . . .
H34 H 0.1345 0.4471 0.8934 0.044 Uiso 1 1 calc R . .
C46 C -0.11652(9) 0.25017(14) 0.40419(11) 0.0314(5) Uani 1 1 d . . .
H46 H -0.1470 0.2622 0.3608 0.038 Uiso 1 1 calc R . .
C22 C 0.10846(8) 0.17461(12) 0.56127(10) 0.0268(4) Uani 1 1 d . . .
C32 C 0.14326(8) 0.41033(13) 0.76597(10) 0.0283(4) Uani 1 1 d . . .
H32 H 0.1532 0.3700 0.7477 0.034 Uiso 1 1 calc R . .
C26 C 0.04584(8) 0.37821(11) 0.52954(10) 0.0210(4) Uani 1 1 d . . .
H26 H 0.0100 0.4038 0.5128 0.025 Uiso 1 1 calc R . .
C35 C 0.11389(11) 0.53018(15) 0.82132(13) 0.0376(5) Uani 1 1 d . . .
H35 H 0.1036 0.5701 0.8396 0.045 Uiso 1 1 calc R . .
C36 C 0.11107(10) 0.54482(14) 0.76223(12) 0.0322(5) Uani 1 1 d . . .
H36 H 0.0995 0.5948 0.7413 0.039 Uiso 1 1 calc R . .
C41 C 0.21041(10) 0.61612(14) 0.54696(12) 0.0364(5) Uani 1 1 d . . .
H41 H 0.2103 0.6642 0.5271 0.044 Uiso 1 1 calc R . .
C48 C -0.07767(10) 0.19305(14) 0.51372(12) 0.0356(5) Uani 1 1 d . . .
H48 H -0.0822 0.1662 0.5445 0.043 Uiso 1 1 calc R . .
C45 C -0.06338(8) 0.27278(13) 0.42410(11) 0.0299(5) Uani 1 1 d . . .
H45 H -0.0589 0.2998 0.3933 0.036 Uiso 1 1 calc R . .
C33 C 0.14603(9) 0.39682(15) 0.82541(11) 0.0336(5) Uani 1 1 d . . .
H33 H 0.1576 0.3470 0.8466 0.040 Uiso 1 1 calc R . .
C39 C 0.25736(9) 0.49640(15) 0.60971(12) 0.0330(5) Uani 1 1 d . . .
H39 H 0.2891 0.4644 0.6319 0.040 Uiso 1 1 calc R . .
C47 C -0.12361(9) 0.20965(13) 0.44934(11) 0.0292(4) Uani 1 1 d . . .
C49 C -0.02491(9) 0.21606(14) 0.53287(11) 0.0311(5) Uani 1 1 d . . .
H49 H 0.0055 0.2042 0.5763 0.037 Uiso 1 1 calc R . .
C28 C 0.10886(8) 0.49287(12) 0.56332(10) 0.0232(4) Uani 1 1 d . . .
H28 H 0.0836 0.5389 0.5488 0.028 Uiso 1 1 calc R . .
C15 C 0.08126(10) 0.12193(13) 0.70101(12) 0.0336(5) Uani 1 1 d . . .
C40 C 0.25744(9) 0.56862(15) 0.58031(12) 0.0341(5) Uani 1 1 d . . .
C21 C 0.11778(12) 0.18519(16) 0.75175(13) 0.0443(6) Uani 1 1 d . . .
H21A H 0.1444 0.1602 0.7944 0.066 Uiso 1 1 calc R . .
H21B H 0.0953 0.2220 0.7575 0.066 Uiso 1 1 calc R . .
H21C H 0.1370 0.2138 0.7358 0.066 Uiso 1 1 calc R . .
C9 C 0.15562(9) 0.13634(13) 0.62691(11) 0.0287(4) Uani 1 1 d . . .
C12 C 0.01399(13) -0.00002(18) 0.61153(15) 0.0532(7) Uani 1 1 d . . .
H12 H -0.0084 -0.0409 0.5821 0.064 Uiso 1 1 calc R . .
C42 C 0.16315(10) 0.59116(13) 0.54346(12) 0.0325(5) Uani 1 1 d . . .
H42 H 0.1315 0.6232 0.5211 0.039 Uiso 1 1 calc R . .
C17 C 0.33327(12) 0.2081(2) 0.53703(15) 0.0616(9) Uani 1 1 d . . .
H17A H 0.3687 0.1818 0.5643 0.092 Uiso 1 1 calc R . .
H17B H 0.3388 0.2651 0.5382 0.092 Uiso 1 1 calc R . .
H17C H 0.3143 0.1894 0.4911 0.092 Uiso 1 1 calc R . .
C6 C 0.23783(9) 0.15455(15) 0.61858(11) 0.0348(5) Uani 1 1 d . . .
C18 C 0.19748(14) 0.02947(17) 0.54546(17) 0.0581(8) Uani 1 1 d . . .
H18A H 0.2014 0.0010 0.5133 0.087 Uiso 1 1 calc R . .
H18B H 0.1592 0.0441 0.5245 0.087 Uiso 1 1 calc R . .
H18C H 0.2093 -0.0044 0.5839 0.087 Uiso 1 1 calc R . .
C10 C 0.09582(10) 0.08073(14) 0.66235(12) 0.0340(5) Uani 1 1 d . . .
C8 C 0.19940(11) 0.07107(17) 0.72488(13) 0.0456(6) Uani 1 1 d . . .
H8 H 0.2060 0.0433 0.7626 0.055 Uiso 1 1 calc R . .
C14 C 0.03120(11) 0.10123(16) 0.69203(13) 0.0429(6) Uani 1 1 d . . .
H14 H 0.0202 0.1286 0.7166 0.051 Uiso 1 1 calc R . .
C11 C 0.06346(12) 0.01826(15) 0.61820(13) 0.0433(6) Uani 1 1 d . . .
C1 C 0.27374(9) 0.22001(16) 0.64426(11) 0.0371(5) Uani 1 1 d . . .
C5 C 0.23268(11) 0.10397(16) 0.56829(12) 0.0424(6) Uani 1 1 d . . .
C50 C -0.22032(10) 0.1925(2) 0.36603(14) 0.0565(8) Uani 1 1 d . . .
H50A H -0.2274 0.2484 0.3545 0.085 Uiso 1 1 calc R . .
H50B H -0.2526 0.1683 0.3606 0.085 Uiso 1 1 calc R . .
H50C H -0.2122 0.1662 0.3367 0.085 Uiso 1 1 calc R . .
C13 C -0.00300(12) 0.04088(17) 0.64750(15) 0.0501(7) Uani 1 1 d . . .
C2 C 0.30311(10) 0.23684(17) 0.61541(12) 0.0418(6) Uani 1 1 d . . .
H2 H 0.3265 0.2813 0.6306 0.050 Uiso 1 1 calc R . .
C19 C 0.08201(15) -0.03033(16) 0.58107(17) 0.0582(8) Uani 1 1 d . . .
H19A H 0.0812 0.0027 0.5475 0.087 Uiso 1 1 calc R . .
H19B H 0.0575 -0.0753 0.5593 0.087 Uiso 1 1 calc R . .
H19C H 0.1192 -0.0494 0.6127 0.087 Uiso 1 1 calc R . .
C3 C 0.29865(11) 0.18933(18) 0.56460(13) 0.0467(7) Uani 1 1 d . . .
C7 C 0.23736(11) 0.09152(17) 0.71261(13) 0.0461(6) Uani 1 1 d . . .
H7 H 0.2753 0.0812 0.7405 0.055 Uiso 1 1 calc R . .
C4 C 0.26351(11) 0.12428(18) 0.54219(13) 0.0479(7) Uani 1 1 d . . .
H4 H 0.2602 0.0924 0.5080 0.057 Uiso 1 1 calc R . .
C16 C 0.28377(10) 0.26911(18) 0.70342(13) 0.0456(6) Uani 1 1 d . . .
H16A H 0.3088 0.2408 0.7449 0.068 Uiso 1 1 calc R . .
H16B H 0.2491 0.2779 0.6987 0.068 Uiso 1 1 calc R . .
H16C H 0.2998 0.3199 0.7043 0.068 Uiso 1 1 calc R . .
C25 C 0.08442(8) 0.37940(11) 0.60724(10) 0.0212(4) Uani 1 1 d . . .
H25 H 0.0628 0.3772 0.6273 0.025 Uiso 1 1 calc R . .
C43 C 0.30799(13) 0.6608(2) 0.55786(17) 0.0608(8) Uani 1 1 d . . .
H43A H 0.2809 0.6589 0.5097 0.091 Uiso 1 1 calc R . .
H43B H 0.3443 0.6682 0.5669 0.091 Uiso 1 1 calc R . .
H43C H 0.2997 0.7048 0.5768 0.091 Uiso 1 1 calc R . .
C20 C -0.05682(15) 0.0196(2) 0.6401(2) 0.0752(11) Uani 1 1 d . . .
H20A H -0.0491 -0.0155 0.6763 0.113 Uiso 1 1 calc R . .
H20B H -0.0813 -0.0068 0.5974 0.113 Uiso 1 1 calc R . .
H20C H -0.0742 0.0678 0.6418 0.113 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 C54 1.754(3) . ?
C54 Cl1 1.754(3) 2 ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
I1 C29 2.1474(19) . ?
O3 C30 1.227(2) . ?
O2 C24 1.241(2) . ?
N3 C30 1.366(2) . ?
N3 C25 1.477(2) . ?
N3 C28 1.488(2) . ?
C37 C42 1.383(3) . ?
C37 C38 1.395(3) . ?
C37 C28 1.507(3) . ?
O1 C22 1.242(2) . ?
C30 C31 1.506(3) . ?
C44 C45 1.383(3) . ?
C44 C49 1.388(3) . ?
C44 C27 1.516(3) . ?
O5 C47 1.373(2) . ?
O5 C50 1.419(3) . ?
N1 C9 1.346(3) . ?
N1 C7 1.386(3) . ?
N1 C6 1.448(3) . ?
C38 C39 1.388(3) . ?
C38 H38 0.9300 . ?
O4 C40 1.375(3) . ?
O4 C43 1.425(3) . ?
C29 C26 1.522(3) . ?
C29 C28 1.528(3) . ?
C29 H29 0.9800 . ?
C24 C23 1.421(3) . ?
C24 C25 1.551(3) . ?
C27 C23 1.512(3) . ?
C27 C26 1.550(3) . ?
C27 H27 0.9800 . ?
C31 C32 1.388(3) . ?
C31 C36 1.398(3) . ?
N2 C9 1.338(3) . ?
N2 C8 1.385(3) . ?
N2 C10 1.454(3) . ?
C23 C22 1.400(3) . ?
C34 C33 1.379(3) . ?
C34 C35 1.382(3) . ?
C34 H34 0.9300 . ?
C46 C47 1.380(3) . ?
C46 C45 1.389(3) . ?
C46 H46 0.9300 . ?
C22 C9 1.524(3) . ?
C32 C33 1.391(3) . ?
C32 H32 0.9300 . ?
C26 C25 1.534(3) . ?
C26 H26 0.9800 . ?
C35 C36 1.386(3) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C41 C40 1.380(3) . ?
C41 C42 1.392(3) . ?
C41 H41 0.9300 . ?
C48 C47 1.382(3) . ?
C48 C49 1.386(3) . ?
C48 H48 0.9300 . ?
C45 H45 0.9300 . ?
C33 H33 0.9300 . ?
C39 C40 1.392(3) . ?
C39 H39 0.9300 . ?
C49 H49 0.9300 . ?
C28 H28 0.9800 . ?
C15 C14 1.390(3) . ?
C15 C10 1.392(3) . ?
C15 C21 1.502(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C12 C13 1.385(4) . ?
C12 C11 1.389(4) . ?
C12 H12 0.9300 . ?
C42 H42 0.9300 . ?
C17 C3 1.512(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C6 C1 1.391(4) . ?
C6 C5 1.402(3) . ?
C18 C5 1.502(4) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C10 C11 1.400(3) . ?
C8 C7 1.335(4) . ?
C8 H8 0.9300 . ?
C14 C13 1.392(4) . ?
C14 H14 0.9300 . ?
C11 C19 1.505(4) . ?
C1 C2 1.393(3) . ?
C1 C16 1.510(3) . ?
C5 C4 1.390(4) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C13 C20 1.514(4) . ?
C2 C3 1.390(4) . ?
C2 H2 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C3 C4 1.374(4) . ?
C7 H7 0.9300 . ?
C4 H4 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C25 H25 0.9800 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 C54 Cl1 113.1(2) . 2 ?
Cl1 C54 H54A 109.0 . . ?
Cl1 C54 H54A 109.0 2 . ?
Cl1 C54 H54B 109.0 . . ?
Cl1 C54 H54B 109.0 2 . ?
H54A C54 H54B 107.8 . . ?
C30 N3 C25 127.51(16) . . ?
C30 N3 C28 114.47(16) . . ?
C25 N3 C28 111.48(15) . . ?
C42 C37 C38 118.66(19) . . ?
C42 C37 C28 119.39(19) . . ?
C38 C37 C28 121.81(19) . . ?
O3 C30 N3 119.78(18) . . ?
O3 C30 C31 118.63(18) . . ?
N3 C30 C31 121.57(18) . . ?
C45 C44 C49 117.35(19) . . ?
C45 C44 C27 118.52(18) . . ?
C49 C44 C27 123.97(18) . . ?
C47 O5 C50 116.77(18) . . ?
C9 N1 C7 108.48(19) . . ?
C9 N1 C6 129.20(18) . . ?
C7 N1 C6 122.16(19) . . ?
C39 C38 C37 120.4(2) . . ?
C39 C38 H38 119.8 . . ?
C37 C38 H38 119.8 . . ?
C40 O4 C43 116.8(2) . . ?
C26 C29 C28 106.71(15) . . ?
C26 C29 I1 112.68(12) . . ?
C28 C29 I1 112.66(13) . . ?
C26 C29 H29 108.2 . . ?
C28 C29 H29 108.2 . . ?
I1 C29 H29 108.2 . . ?
O2 C24 C23 129.85(18) . . ?
O2 C24 C25 122.47(17) . . ?
C23 C24 C25 107.67(16) . . ?
C23 C27 C44 117.18(17) . . ?
C23 C27 C26 102.47(15) . . ?
C44 C27 C26 110.79(15) . . ?
C23 C27 H27 108.7 . . ?
C44 C27 H27 108.7 . . ?
C26 C27 H27 108.7 . . ?
C32 C31 C36 119.64(19) . . ?
C32 C31 C30 124.74(18) . . ?
C36 C31 C30 115.32(19) . . ?
C9 N2 C8 109.0(2) . . ?
C9 N2 C10 126.93(18) . . ?
C8 N2 C10 123.7(2) . . ?
C22 C23 C24 125.64(18) . . ?
C22 C23 C27 121.45(18) . . ?
C24 C23 C27 112.67(17) . . ?
C33 C34 C35 119.9(2) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C47 C46 C45 119.4(2) . . ?
C47 C46 H46 120.3 . . ?
C45 C46 H46 120.3 . . ?
O1 C22 C23 126.53(19) . . ?
O1 C22 C9 116.70(18) . . ?
C23 C22 C9 116.68(18) . . ?
C31 C32 C33 119.5(2) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 . . ?
C29 C26 C25 101.20(15) . . ?
C29 C26 C27 112.19(15) . . ?
C25 C26 C27 107.06(15) . . ?
C29 C26 H26 111.9 . . ?
C25 C26 H26 111.9 . . ?
C27 C26 H26 111.9 . . ?
C34 C35 C36 120.2(2) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C35 C36 C31 120.0(2) . . ?
C35 C36 H36 120.0 . . ?
C31 C36 H36 120.0 . . ?
C40 C41 C42 119.2(2) . . ?
C40 C41 H41 120.4 . . ?
C42 C41 H41 120.4 . . ?
C47 C48 C49 120.7(2) . . ?
C47 C48 H48 119.7 . . ?
C49 C48 H48 119.7 . . ?
C44 C45 C46 122.3(2) . . ?
C44 C45 H45 118.9 . . ?
C46 C45 H45 118.9 . . ?
C34 C33 C32 120.7(2) . . ?
C34 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C38 C39 C40 120.0(2) . . ?
C38 C39 H39 120.0 . . ?
C40 C39 H39 120.0 . . ?
O5 C47 C46 123.8(2) . . ?
O5 C47 C48 116.9(2) . . ?
C46 C47 C48 119.27(19) . . ?
C48 C49 C44 121.0(2) . . ?
C48 C49 H49 119.5 . . ?
C44 C49 H49 119.5 . . ?
N3 C28 C37 115.32(16) . . ?
N3 C28 C29 102.01(15) . . ?
C37 C28 C29 112.51(16) . . ?
N3 C28 H28 108.9 . . ?
C37 C28 H28 108.9 . . ?
C29 C28 H28 108.9 . . ?
C14 C15 C10 117.2(2) . . ?
C14 C15 C21 120.2(2) . . ?
C10 C15 C21 122.6(2) . . ?
O4 C40 C41 124.4(2) . . ?
O4 C40 C39 115.4(2) . . ?
C41 C40 C39 120.2(2) . . ?
C15 C21 H21A 109.5 . . ?
C15 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C15 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C9 N1 107.59(18) . . ?
N2 C9 C22 123.70(19) . . ?
N1 C9 C22 128.7(2) . . ?
C13 C12 C11 121.9(3) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C37 C42 C41 121.5(2) . . ?
C37 C42 H42 119.2 . . ?
C41 C42 H42 119.2 . . ?
C3 C17 H17A 109.5 . . ?
C3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C1 C6 C5 122.7(2) . . ?
C1 C6 N1 119.1(2) . . ?
C5 C6 N1 117.8(2) . . ?
C5 C18 H18A 109.5 . . ?
C5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C10 C11 122.5(2) . . ?
C15 C10 N2 119.3(2) . . ?
C11 C10 N2 118.0(2) . . ?
C7 C8 N2 107.4(2) . . ?
C7 C8 H8 126.3 . . ?
N2 C8 H8 126.3 . . ?
C15 C14 C13 122.2(2) . . ?
C15 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?
C12 C11 C10 117.6(2) . . ?
C12 C11 C19 120.3(3) . . ?
C10 C11 C19 122.0(3) . . ?
C6 C1 C2 117.2(2) . . ?
C6 C1 C16 122.6(2) . . ?
C2 C1 C16 120.1(2) . . ?
C4 C5 C6 116.8(3) . . ?
C4 C5 C18 121.2(2) . . ?
C6 C5 C18 122.0(2) . . ?
O5 C50 H50A 109.5 . . ?
O5 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
O5 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C12 C13 C14 118.5(3) . . ?
C12 C13 C20 121.2(3) . . ?
C14 C13 C20 120.4(3) . . ?
C3 C2 C1 122.2(3) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C11 C19 H19A 109.5 . . ?
C11 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C11 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C4 C3 C2 118.2(2) . . ?
C4 C3 C17 121.7(3) . . ?
C2 C3 C17 120.1(3) . . ?
C8 C7 N1 107.6(2) . . ?
C8 C7 H7 126.2 . . ?
N1 C7 H7 126.2 . . ?
C3 C4 C5 122.9(2) . . ?
C3 C4 H4 118.5 . . ?
C5 C4 H4 118.5 . . ?
C1 C16 H16A 109.5 . . ?
C1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C25 C26 105.07(15) . . ?
N3 C25 C24 115.84(15) . . ?
C26 C25 C24 103.27(15) . . ?
N3 C25 H25 110.7 . . ?
C26 C25 H25 110.7 . . ?
C24 C25 H25 110.7 . . ?
O4 C43 H43A 109.5 . . ?
O4 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O4 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C13 C20 H20A 109.5 . . ?
C13 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C13 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.934
_diffrn_reflns_theta_full        28.27
_diffrn_measured_fraction_theta_full 0.934
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.068
####################################################################### 
# 
# 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_786jdkm
_database_code_depnum_ccdc_archive 'CCDC 1568078'
_audit_update_record             
;
2017-08-10 deposited with the CCDC.
2018-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H47 N3 O3'
_chemical_formula_weight         761.93

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

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   P21/n

loop_
_symmetry_equiv_pos_as_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                   13.605(3)
_cell_length_b                   13.333(3)
_cell_length_c                   23.507(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.393(6)
_cell_angle_gamma                90.00
_cell_volume                     4180.0(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1741
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      24.66

_exptl_crystal_description       PLATES
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9874
_exptl_absorpt_correction_T_max  0.9978
_exptl_absorpt_process_details   'BRUKER SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17563
_diffrn_reflns_av_R_equivalents  0.0958
_diffrn_reflns_av_sigmaI/netI    0.1437
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7310
_reflns_number_gt                3754
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER SMART'
_computing_cell_refinement       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0566P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7310
_refine_ls_number_parameters     533
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1650
_refine_ls_R_factor_gt           0.0784
_refine_ls_wR_factor_ref         0.1724
_refine_ls_wR_factor_gt          0.1391
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.20076(18) 0.94851(18) 0.18861(10) 0.0293(6) Uani 1 1 d . . .
O2 O 0.32889(19) 0.70119(19) 0.11167(11) 0.0342(7) Uani 1 1 d . . .
N1 N 0.1312(2) 0.7156(2) 0.16606(12) 0.0238(7) Uani 1 1 d . . .
N2 N 0.2579(2) 0.7271(2) 0.23769(12) 0.0246(7) Uani 1 1 d . . .
N3 N 0.4178(3) 0.7586(3) 0.02190(14) 0.0340(9) Uani 1 1 d . . .
C22 C 0.2374(3) 0.8744(3) 0.16762(15) 0.0227(9) Uani 1 1 d . . .
C23 C 0.3017(3) 0.8761(3) 0.12909(15) 0.0210(8) Uani 1 1 d . . .
C24 C 0.3363(3) 0.9715(3) 0.10481(15) 0.0257(9) Uani 1 1 d . . .
H24 H 0.2788 1.0167 0.0942 0.031 Uiso 1 1 calc R . .
C33 C 0.4438(3) 1.1247(3) 0.13529(16) 0.0320(10) Uani 1 1 d . . .
H33 H 0.4079 1.1576 0.1029 0.038 Uiso 1 1 calc R . .
C28 C 0.4194(3) 1.0261(3) 0.14589(15) 0.0237(9) Uani 1 1 d . . .
C31 C 0.5769(3) 1.1280(3) 0.22056(16) 0.0309(10) Uani 1 1 d . . .
O3 O 0.5733(2) 0.7980(2) 0.00994(12) 0.0513(9) Uani 1 1 d . . .
C6 C 0.3448(3) 0.7668(3) 0.27715(15) 0.0267(9) Uani 1 1 d . . .
C7 C 0.2096(3) 0.7733(3) 0.18894(15) 0.0223(9) Uani 1 1 d . . .
C12 C -0.0231(3) 0.7067(3) 0.01759(17) 0.0338(10) Uani 1 1 d . . .
H12 H -0.0251 0.6725 -0.0171 0.041 Uiso 1 1 calc R . .
C29 C 0.4752(3) 0.9791(3) 0.19483(16) 0.0293(10) Uani 1 1 d . . .
H29 H 0.4608 0.9132 0.2033 0.035 Uiso 1 1 calc R . .
C11 C 0.0536(3) 0.6851(3) 0.06380(16) 0.0278(9) Uani 1 1 d . . .
C9 C 0.2095(3) 0.6385(3) 0.24466(16) 0.0291(10) Uani 1 1 d . . .
H9 H 0.2281 0.5920 0.2743 0.035 Uiso 1 1 calc R . .
C15 C -0.0191(3) 0.8074(3) 0.12147(17) 0.0300(10) Uani 1 1 d . . .
C25 C 0.3701(3) 0.9364(3) 0.04855(16) 0.0316(10) Uani 1 1 d . . .
H25 H 0.4247 0.9795 0.0413 0.038 Uiso 1 1 calc R . .
C32 C 0.5195(3) 1.1746(3) 0.17153(17) 0.0360(11) Uani 1 1 d . . .
H32 H 0.5331 1.2409 0.1634 0.043 Uiso 1 1 calc R . .
C46 C 0.5007(3) 0.7430(3) -0.00064(17) 0.0332(10) Uani 1 1 d . . .
C10 C 0.0551(3) 0.7380(3) 0.11507(16) 0.0258(9) Uani 1 1 d . . .
C47 C 0.4931(3) 0.6549(3) -0.04059(17) 0.0335(10) Uani 1 1 d . . .
C8 C 0.1311(3) 0.6322(3) 0.20085(16) 0.0286(9) Uani 1 1 d . . .
H8 H 0.0844 0.5805 0.1947 0.034 Uiso 1 1 calc R . .
C18 C 0.2262(3) 0.8744(3) 0.32148(17) 0.0418(11) Uani 1 1 d . . .
H18A H 0.1977 0.9137 0.2881 0.063 Uiso 1 1 calc R . .
H18B H 0.2307 0.9143 0.3559 0.063 Uiso 1 1 calc R . .
H18C H 0.1844 0.8171 0.3238 0.063 Uiso 1 1 calc R . .
C27 C 0.3424(3) 0.7919(3) 0.10571(15) 0.0272(9) Uani 1 1 d . . .
C1 C 0.4397(3) 0.7286(3) 0.27492(15) 0.0298(10) Uani 1 1 d . . .
C21 C -0.0211(3) 0.8583(3) 0.17827(16) 0.0371(11) Uani 1 1 d . . .
H21A H -0.0019 0.8113 0.2094 0.056 Uiso 1 1 calc R . .
H21B H -0.0875 0.8826 0.1783 0.056 Uiso 1 1 calc R . .
H21C H 0.0250 0.9137 0.1834 0.056 Uiso 1 1 calc R . .
C26 C 0.4119(3) 0.8310(3) 0.06696(16) 0.0298(10) Uani 1 1 d . . .
H26 H 0.4791 0.8390 0.0909 0.036 Uiso 1 1 calc R . .
C5 C 0.3294(3) 0.8398(3) 0.31625(16) 0.0314(10) Uani 1 1 d . . .
C14 C -0.0933(3) 0.8263(3) 0.07298(18) 0.0361(11) Uani 1 1 d . . .
H14 H -0.1423 0.8737 0.0757 0.043 Uiso 1 1 calc R . .
C20 C -0.1787(3) 0.7997(4) -0.03108(18) 0.0537(13) Uani 1 1 d . . .
H20A H -0.2391 0.8166 -0.0180 0.081 Uiso 1 1 calc R . .
H20B H -0.1903 0.7419 -0.0558 0.081 Uiso 1 1 calc R . .
H20C H -0.1586 0.8551 -0.0523 0.081 Uiso 1 1 calc R . .
C34 C 0.6591(3) 1.1810(3) 0.26030(19) 0.0389(11) Uani 1 1 d . . .
C3 C 0.5112(3) 0.8471(3) 0.35031(17) 0.0385(11) Uani 1 1 d . . .
C13 C -0.0973(3) 0.7770(3) 0.02032(18) 0.0388(11) Uani 1 1 d . . .
C19 C 0.1317(3) 0.6087(3) 0.05652(16) 0.0356(11) Uani 1 1 d . . .
H19A H 0.0994 0.5504 0.0373 0.053 Uiso 1 1 calc R . .
H19B H 0.1695 0.5900 0.0939 0.053 Uiso 1 1 calc R . .
H19C H 0.1759 0.6369 0.0336 0.053 Uiso 1 1 calc R . .
C4 C 0.4143(3) 0.8788(3) 0.35223(16) 0.0379(11) Uani 1 1 d . . .
H4 H 0.4061 0.9283 0.3788 0.045 Uiso 1 1 calc R . .
C40 C 0.2892(3) 0.9315(3) -0.00533(17) 0.0353(10) Uani 1 1 d . . .
C30 C 0.5522(3) 1.0300(3) 0.23091(16) 0.0334(10) Uani 1 1 d . . .
H30 H 0.5884 0.9970 0.2632 0.040 Uiso 1 1 calc R . .
C52 C 0.4044(4) 0.6245(3) -0.07374(18) 0.0490(12) Uani 1 1 d . . .
H52 H 0.3465 0.6618 -0.0742 0.059 Uiso 1 1 calc R . .
C16 C 0.4534(3) 0.6407(3) 0.23703(17) 0.0489(12) Uani 1 1 d . . .
H16A H 0.5220 0.6377 0.2326 0.073 Uiso 1 1 calc R . .
H16B H 0.4105 0.6485 0.1996 0.073 Uiso 1 1 calc R . .
H16C H 0.4365 0.5798 0.2547 0.073 Uiso 1 1 calc R . .
C42 C 0.2424(5) 0.9394(4) -0.10959(19) 0.0683(17) Uani 1 1 d . . .
H42 H 0.2605 0.9489 -0.1453 0.082 Uiso 1 1 calc R . .
C2 C 0.5214(3) 0.7715(3) 0.31135(17) 0.0380(11) Uani 1 1 d . . .
H2 H 0.5854 0.7489 0.3096 0.046 Uiso 1 1 calc R . .
C41 C 0.3138(4) 0.9467(3) -0.05945(18) 0.0527(13) Uani 1 1 d . . .
H41 H 0.3796 0.9621 -0.0617 0.063 Uiso 1 1 calc R . .
C17 C 0.6023(3) 0.8901(4) 0.38918(19) 0.0621(15) Uani 1 1 d . . .
H17A H 0.6278 0.8430 0.4194 0.093 Uiso 1 1 calc R . .
H17B H 0.5847 0.9514 0.4061 0.093 Uiso 1 1 calc R . .
H17C H 0.6529 0.9035 0.3669 0.093 Uiso 1 1 calc R . .
C48 C 0.5807(3) 0.6009(3) -0.04132(19) 0.0494(13) Uani 1 1 d . . .
H48 H 0.6417 0.6229 -0.0198 0.059 Uiso 1 1 calc R . .
C45 C 0.1898(3) 0.9099(3) -0.00392(19) 0.0508(13) Uani 1 1 d . . .
H45 H 0.1714 0.8996 0.0317 0.061 Uiso 1 1 calc R . .
C35 C 0.6842(3) 1.1583(3) 0.3193(2) 0.0526(13) Uani 1 1 d . . .
H35 H 0.6508 1.1066 0.3341 0.063 Uiso 1 1 calc R . .
C44 C 0.1173(4) 0.9033(4) -0.0546(2) 0.0715(17) Uani 1 1 d . . .
H44 H 0.0511 0.8890 -0.0528 0.086 Uiso 1 1 calc R . .
C39 C 0.7116(3) 1.2569(4) 0.2396(2) 0.0618(15) Uani 1 1 d . . .
H39 H 0.6983 1.2722 0.2003 0.074 Uiso 1 1 calc R . .
C43 C 0.1443(5) 0.9182(4) -0.1074(2) 0.0744(19) Uani 1 1 d . . .
H43 H 0.0963 0.9140 -0.1415 0.089 Uiso 1 1 calc R . .
C37 C 0.8066(4) 1.2880(5) 0.3351(3) 0.079(2) Uani 1 1 d . . .
H37 H 0.8550 1.3248 0.3600 0.095 Uiso 1 1 calc R . .
C49 C 0.5762(4) 0.5141(4) -0.0745(2) 0.0613(15) Uani 1 1 d . . .
H49 H 0.6340 0.4769 -0.0748 0.074 Uiso 1 1 calc R . .
C50 C 0.4865(5) 0.4839(4) -0.1065(2) 0.0629(15) Uani 1 1 d . . .
H50 H 0.4837 0.4257 -0.1285 0.076 Uiso 1 1 calc R . .
C36 C 0.7578(4) 1.2111(4) 0.3562(2) 0.0680(16) Uani 1 1 d . . .
H36 H 0.7741 1.1944 0.3953 0.082 Uiso 1 1 calc R . .
C51 C 0.4003(4) 0.5373(4) -0.1071(2) 0.0619(15) Uani 1 1 d . . .
H51 H 0.3398 0.5158 -0.1295 0.074 Uiso 1 1 calc R . .
C38 C 0.7844(4) 1.3106(5) 0.2777(3) 0.087(2) Uani 1 1 d . . .
H38 H 0.8183 1.3626 0.2635 0.104 Uiso 1 1 calc R . .
H1C H 0.375(3) 0.704(4) 0.0172(19) 0.076(17) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C22 1.252(4) . ?
O2 C27 1.235(4) . ?
N1 C7 1.339(4) . ?
N1 C8 1.380(4) . ?
N1 C10 1.452(4) . ?
N2 C7 1.351(4) . ?
N2 C9 1.378(4) . ?
N2 C6 1.450(4) . ?
N3 C46 1.354(5) . ?
N3 C26 1.447(4) . ?
N3 H1C 0.92(4) . ?
C22 C23 1.378(5) . ?
C22 C7 1.511(5) . ?
C23 C27 1.411(5) . ?
C23 C24 1.507(5) . ?
C24 C28 1.520(5) . ?
C24 C25 1.556(5) . ?
C24 H24 0.9800 . ?
C33 C32 1.372(5) . ?
C33 C28 1.390(5) . ?
C33 H33 0.9300 . ?
C28 C29 1.396(5) . ?
C31 C30 1.383(5) . ?
C31 C32 1.403(5) . ?
C31 C34 1.487(5) . ?
O3 C46 1.217(4) . ?
C6 C5 1.383(5) . ?
C6 C1 1.399(5) . ?
C12 C11 1.379(5) . ?
C12 C13 1.388(5) . ?
C12 H12 0.9300 . ?
C29 C30 1.387(5) . ?
C29 H29 0.9300 . ?
C11 C10 1.393(5) . ?
C11 C19 1.506(5) . ?
C9 C8 1.331(5) . ?
C9 H9 0.9300 . ?
C15 C14 1.388(5) . ?
C15 C10 1.400(5) . ?
C15 C21 1.502(5) . ?
C25 C40 1.506(5) . ?
C25 C26 1.545(5) . ?
C25 H25 0.9800 . ?
C32 H32 0.9300 . ?
C46 C47 1.494(5) . ?
C47 C52 1.362(5) . ?
C47 C48 1.396(5) . ?
C8 H8 0.9300 . ?
C18 C5 1.505(5) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C27 C26 1.529(5) . ?
C1 C2 1.386(5) . ?
C1 C16 1.506(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C26 H26 0.9800 . ?
C5 C4 1.391(5) . ?
C14 C13 1.393(5) . ?
C14 H14 0.9300 . ?
C20 C13 1.500(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C34 C39 1.381(6) . ?
C34 C35 1.395(6) . ?
C3 C2 1.387(5) . ?
C3 C4 1.393(5) . ?
C3 C17 1.502(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C4 H4 0.9300 . ?
C40 C45 1.389(6) . ?
C40 C41 1.393(5) . ?
C30 H30 0.9300 . ?
C52 C51 1.397(6) . ?
C52 H52 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C42 C43 1.375(7) . ?
C42 C41 1.375(6) . ?
C42 H42 0.9300 . ?
C2 H2 0.9300 . ?
C41 H41 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C48 C49 1.390(6) . ?
C48 H48 0.9300 . ?
C45 C44 1.391(6) . ?
C45 H45 0.9300 . ?
C35 C36 1.381(6) . ?
C35 H35 0.9300 . ?
C44 C43 1.377(7) . ?
C44 H44 0.9300 . ?
C39 C38 1.395(6) . ?
C39 H39 0.9300 . ?
C43 H43 0.9300 . ?
C37 C38 1.357(7) . ?
C37 C36 1.368(7) . ?
C37 H37 0.9300 . ?
C49 C50 1.363(6) . ?
C49 H49 0.9300 . ?
C50 C51 1.369(6) . ?
C50 H50 0.9300 . ?
C36 H36 0.9300 . ?
C51 H51 0.9300 . ?
C38 H38 0.9300 . ?

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 N1 C8 108.6(3) . . ?
C7 N1 C10 126.5(3) . . ?
C8 N1 C10 124.8(3) . . ?
C7 N2 C9 109.1(3) . . ?
C7 N2 C6 125.1(3) . . ?
C9 N2 C6 125.8(3) . . ?
C46 N3 C26 124.1(4) . . ?
C46 N3 H1C 113(3) . . ?
C26 N3 H1C 119(3) . . ?
O1 C22 C23 126.8(3) . . ?
O1 C22 C7 115.4(3) . . ?
C23 C22 C7 117.8(3) . . ?
C22 C23 C27 126.3(3) . . ?
C22 C23 C24 123.3(3) . . ?
C27 C23 C24 110.4(3) . . ?
C23 C24 C28 114.4(3) . . ?
C23 C24 C25 103.6(3) . . ?
C28 C24 C25 112.1(3) . . ?
C23 C24 H24 108.9 . . ?
C28 C24 H24 108.9 . . ?
C25 C24 H24 108.9 . . ?
C32 C33 C28 121.6(4) . . ?
C32 C33 H33 119.2 . . ?
C28 C33 H33 119.2 . . ?
C33 C28 C29 117.5(4) . . ?
C33 C28 C24 120.9(3) . . ?
C29 C28 C24 121.6(3) . . ?
C30 C31 C32 116.6(4) . . ?
C30 C31 C34 121.2(4) . . ?
C32 C31 C34 122.2(4) . . ?
C5 C6 C1 122.9(4) . . ?
C5 C6 N2 118.1(3) . . ?
C1 C6 N2 119.0(3) . . ?
N1 C7 N2 107.1(3) . . ?
N1 C7 C22 127.6(3) . . ?
N2 C7 C22 125.1(3) . . ?
C11 C12 C13 123.2(4) . . ?
C11 C12 H12 118.4 . . ?
C13 C12 H12 118.4 . . ?
C30 C29 C28 120.4(4) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C12 C11 C10 117.1(3) . . ?
C12 C11 C19 119.5(3) . . ?
C10 C11 C19 123.4(3) . . ?
C8 C9 N2 106.9(3) . . ?
C8 C9 H9 126.5 . . ?
N2 C9 H9 126.5 . . ?
C14 C15 C10 117.0(4) . . ?
C14 C15 C21 120.7(4) . . ?
C10 C15 C21 122.3(4) . . ?
C40 C25 C26 111.4(3) . . ?
C40 C25 C24 116.0(3) . . ?
C26 C25 C24 100.9(3) . . ?
C40 C25 H25 109.4 . . ?
C26 C25 H25 109.4 . . ?
C24 C25 H25 109.4 . . ?
C33 C32 C31 121.5(4) . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
O3 C46 N3 122.2(4) . . ?
O3 C46 C47 123.8(4) . . ?
N3 C46 C47 114.0(4) . . ?
C11 C10 C15 122.7(4) . . ?
C11 C10 N1 119.8(3) . . ?
C15 C10 N1 117.3(3) . . ?
C52 C47 C48 120.1(4) . . ?
C52 C47 C46 122.5(4) . . ?
C48 C47 C46 117.3(4) . . ?
C9 C8 N1 108.2(3) . . ?
C9 C8 H8 125.9 . . ?
N1 C8 H8 125.9 . . ?
C5 C18 H18A 109.5 . . ?
C5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O2 C27 C23 131.0(3) . . ?
O2 C27 C26 121.7(3) . . ?
C23 C27 C26 107.3(3) . . ?
C2 C1 C6 117.4(4) . . ?
C2 C1 C16 120.6(4) . . ?
C6 C1 C16 121.9(4) . . ?
C15 C21 H21A 109.5 . . ?
C15 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C15 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N3 C26 C27 109.8(3) . . ?
N3 C26 C25 118.2(3) . . ?
C27 C26 C25 103.9(3) . . ?
N3 C26 H26 108.2 . . ?
C27 C26 H26 108.2 . . ?
C25 C26 H26 108.2 . . ?
C6 C5 C4 116.8(4) . . ?
C6 C5 C18 122.4(4) . . ?
C4 C5 C18 120.8(4) . . ?
C15 C14 C13 122.6(4) . . ?
C15 C14 H14 118.7 . . ?
C13 C14 H14 118.7 . . ?
C13 C20 H20A 109.5 . . ?
C13 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C13 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C39 C34 C35 117.9(4) . . ?
C39 C34 C31 120.3(4) . . ?
C35 C34 C31 121.8(4) . . ?
C2 C3 C4 117.5(4) . . ?
C2 C3 C17 120.0(4) . . ?
C4 C3 C17 122.5(4) . . ?
C12 C13 C14 117.3(4) . . ?
C12 C13 C20 121.8(4) . . ?
C14 C13 C20 120.9(4) . . ?
C11 C19 H19A 109.5 . . ?
C11 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C11 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C5 C4 C3 123.0(4) . . ?
C5 C4 H4 118.5 . . ?
C3 C4 H4 118.5 . . ?
C45 C40 C41 117.6(4) . . ?
C45 C40 C25 122.8(4) . . ?
C41 C40 C25 119.6(4) . . ?
C31 C30 C29 122.3(4) . . ?
C31 C30 H30 118.8 . . ?
C29 C30 H30 118.8 . . ?
C47 C52 C51 120.1(5) . . ?
C47 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
C1 C16 H16A 109.5 . . ?
C1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C43 C42 C41 120.6(5) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C1 C2 C3 122.4(4) . . ?
C1 C2 H2 118.8 . . ?
C3 C2 H2 118.8 . . ?
C42 C41 C40 121.0(5) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C3 C17 H17A 109.5 . . ?
C3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C49 C48 C47 119.6(5) . . ?
C49 C48 H48 120.2 . . ?
C47 C48 H48 120.2 . . ?
C40 C45 C44 121.5(5) . . ?
C40 C45 H45 119.3 . . ?
C44 C45 H45 119.3 . . ?
C36 C35 C34 121.2(5) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C43 C44 C45 119.5(5) . . ?
C43 C44 H44 120.2 . . ?
C45 C44 H44 120.2 . . ?
C34 C39 C38 120.1(5) . . ?
C34 C39 H39 119.9 . . ?
C38 C39 H39 119.9 . . ?
C42 C43 C44 119.8(5) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C38 C37 C36 119.9(5) . . ?
C38 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?
C50 C49 C48 119.4(5) . . ?
C50 C49 H49 120.3 . . ?
C48 C49 H49 120.3 . . ?
C49 C50 C51 121.6(5) . . ?
C49 C50 H50 119.2 . . ?
C51 C50 H50 119.2 . . ?
C37 C36 C35 119.9(5) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C50 C51 C52 119.1(5) . . ?
C50 C51 H51 120.4 . . ?
C52 C51 H51 120.4 . . ?
C37 C38 C39 121.0(6) . . ?
C37 C38 H38 119.5 . . ?
C39 C38 H38 119.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.050
