# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 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_180115_whh20180105_1
_database_code_depnum_ccdc_archive 'CCDC 1844325'
_audit_update_record             
;
2018-06-08 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H33 Cl N3 O Rh'
_chemical_formula_weight         553.92

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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.7346(13)
_cell_length_b                   11.0951(9)
_cell_length_c                   13.403(2)
_cell_angle_alpha                98.488(9)
_cell_angle_beta                 113.220(13)
_cell_angle_gamma                108.845(9)
_cell_volume                     1317.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2326
_cell_measurement_theta_min      3.1533
_cell_measurement_theta_max      29.3436

_exptl_crystal_description       Plate
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             572
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7373
_exptl_absorpt_correction_T_max  0.8734
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8089
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4612
_reflns_number_gt                3582
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0361P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4612
_refine_ls_number_parameters     306
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.0995
_refine_ls_wR_factor_gt          0.0864
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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
Rh1 Rh 0.59549(4) 0.83713(3) 0.73963(3) 0.04850(14) Uani 1 1 d . . .
Cl1 Cl 0.71350(14) 0.70870(13) 0.84027(11) 0.0703(3) Uani 1 1 d . . .
N1 N 0.4675(4) 0.6818(3) 0.5850(3) 0.0491(8) Uani 1 1 d . . .
N2 N 0.3291(4) 0.5891(3) 0.5359(3) 0.0526(9) Uani 1 1 d . . .
N3 N 0.3007(4) 0.5289(3) 0.4310(3) 0.0517(9) Uani 1 1 d . . .
C4 C 0.7383(4) 0.8657(4) 0.6702(4) 0.0471(10) Uani 1 1 d . . .
C5 C 0.6794(4) 0.7801(4) 0.5586(3) 0.0454(10) Uani 1 1 d . . .
C6 C 0.7672(5) 0.7877(4) 0.5043(4) 0.0524(10) Uani 1 1 d . . .
H6 H 0.7268 0.7311 0.4304 0.063 Uiso 1 1 calc R . .
C7 C 0.4181(4) 0.5821(4) 0.4119(4) 0.0509(10) Uani 1 1 d . . .
H7 H 0.4240 0.5565 0.3452 0.061 Uiso 1 1 calc R . .
C8 C 0.8880(5) 0.9558(4) 0.7241(4) 0.0533(10) Uani 1 1 d . . .
H8 H 0.9300 1.0123 0.7983 0.064 Uiso 1 1 calc R . .
C9 C 0.5259(4) 0.6813(4) 0.5110(3) 0.0434(9) Uani 1 1 d . . .
C10 C 0.9153(5) 0.8800(5) 0.5607(4) 0.0563(11) Uani 1 1 d . . .
H10 H 0.9738 0.8853 0.5242 0.068 Uiso 1 1 calc R . .
C11 C 0.0532(5) 0.4844(4) 0.2791(4) 0.0573(11) Uani 1 1 d . . .
C12 C 0.9769(4) 0.9642(4) 0.6705(4) 0.0524(11) Uani 1 1 d . . .
C13 C 0.5302(5) 0.8991(4) 0.8720(4) 0.0598(12) Uani 1 1 d . . .
C14 C 0.6649(6) 1.0031(5) 0.8837(5) 0.0675(13) Uani 1 1 d . . .
C15 C 0.4130(5) 0.8705(4) 0.7649(4) 0.0557(11) Uani 1 1 d . . .
C17 C 0.1518(5) 0.4261(4) 0.3500(4) 0.0603(12) Uani 1 1 d . . .
H17A H 0.1063 0.3808 0.3915 0.072 Uiso 1 1 calc R . .
H17B H 0.1598 0.3600 0.2997 0.072 Uiso 1 1 calc R . .
C18 C 0.0078(6) 0.4569(6) 0.1653(5) 0.0804(15) Uani 1 1 d . . .
H18 H 0.0394 0.4027 0.1307 0.097 Uiso 1 1 calc R . .
C19 C 0.6216(6) 1.0426(4) 0.7829(5) 0.0701(14) Uani 1 1 d . . .
C20 C 0.0056(6) 0.5640(6) 0.3285(5) 0.0957(18) Uani 1 1 d . . .
H20 H 0.0365 0.5845 0.4066 0.115 Uiso 1 1 calc R . .
C21 C 0.4694(6) 0.9546(5) 0.7058(4) 0.0655(13) Uani 1 1 d . . .
C22 C 0.2574(5) 0.7687(5) 0.7182(5) 0.0803(15) Uani 1 1 d . . .
H22A H 0.2588 0.6886 0.7366 0.120 Uiso 1 1 calc R . .
H22B H 0.2064 0.7482 0.6366 0.120 Uiso 1 1 calc R . .
H22C H 0.2064 0.8035 0.7511 0.120 Uiso 1 1 calc R . .
C23 C 0.5243(6) 0.8331(6) 0.9605(4) 0.0860(16) Uani 1 1 d . . .
H23A H 0.5397 0.8969 1.0257 0.129 Uiso 1 1 calc R . .
H23B H 0.6010 0.8010 0.9834 0.129 Uiso 1 1 calc R . .
H23C H 0.4285 0.7590 0.9292 0.129 Uiso 1 1 calc R . .
C24 C 0.7187(7) 1.1593(5) 0.7631(6) 0.112(2) Uani 1 1 d . . .
H24A H 0.6950 1.1365 0.6839 0.169 Uiso 1 1 calc R . .
H24B H 0.8218 1.1790 0.8097 0.169 Uiso 1 1 calc R . .
H24C H 0.7009 1.2366 0.7832 0.169 Uiso 1 1 calc R . .
C25 C 0.3745(7) 0.9573(7) 0.5900(5) 0.102(2) Uani 1 1 d . . .
H25A H 0.3153 1.0042 0.5961 0.153 Uiso 1 1 calc R . .
H25B H 0.3100 0.8671 0.5397 0.153 Uiso 1 1 calc R . .
H25C H 0.4372 1.0025 0.5600 0.153 Uiso 1 1 calc R . .
C26 C 0.8130(6) 1.0684(6) 0.9899(5) 0.106(2) Uani 1 1 d . . .
H26A H 0.8097 1.1319 1.0448 0.158 Uiso 1 1 calc R . .
H26B H 0.8894 1.1141 0.9713 0.158 Uiso 1 1 calc R . .
H26C H 0.8349 1.0012 1.0217 0.158 Uiso 1 1 calc R . .
C27 C -0.0859(7) 0.5089(7) 0.0993(6) 0.104(2) Uani 1 1 d . . .
H27 H -0.1158 0.4904 0.0214 0.125 Uiso 1 1 calc R . .
C28 C -0.1326(7) 0.5869(7) 0.1501(8) 0.119(2) Uani 1 1 d . . .
H28 H -0.1955 0.6212 0.1065 0.143 Uiso 1 1 calc R . .
C29 C -0.0892(8) 0.6148(8) 0.2621(7) 0.129(3) Uani 1 1 d . . .
H29 H -0.1223 0.6681 0.2959 0.155 Uiso 1 1 calc R . .
C33 C 1.1398(5) 1.0626(5) 0.7331(4) 0.0716(13) Uani 1 1 d . . .
H33A H 1.2007 1.0162 0.7623 0.107 Uiso 1 1 calc R . .
H33B H 1.1561 1.1314 0.7954 0.107 Uiso 1 1 calc R . .
H33C H 1.1658 1.1026 0.6813 0.107 Uiso 1 1 calc R . .
O1 O 0.4455(8) 0.4277(8) 0.7857(7) 0.195(3) Uani 1 1 d . . .
H1 H 0.4402 0.4908 0.8216 0.293 Uiso 1 1 calc R . .
C34 C 0.5259(13) 0.3812(12) 0.8574(9) 0.247(7) Uani 1 1 d . . .
H34A H 0.6265 0.4191 0.8691 0.370 Uiso 1 1 calc R . .
H34B H 0.4844 0.2853 0.8264 0.370 Uiso 1 1 calc R . .
H34C H 0.5256 0.4052 0.9291 0.370 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
Rh1 C4 2.053(4) . ?
Rh1 N1 2.080(3) . ?
Rh1 C21 2.137(4) . ?
Rh1 C14 2.146(5) . ?
Rh1 C19 2.164(4) . ?
Rh1 C13 2.245(4) . ?
Rh1 C15 2.246(4) . ?
Rh1 Cl1 2.4168(11) . ?
N1 N2 1.320(4) . ?
N1 C9 1.367(5) . ?
N2 N3 1.330(4) . ?
N3 C7 1.350(5) . ?
N3 C17 1.457(5) . ?
C4 C8 1.392(6) . ?
C4 C5 1.409(6) . ?
C5 C6 1.391(5) . ?
C5 C9 1.456(5) . ?
C6 C10 1.385(6) . ?
C6 H6 0.9300 . ?
C7 C9 1.359(5) . ?
C7 H7 0.9300 . ?
C8 C12 1.392(5) . ?
C8 H8 0.9300 . ?
C10 C12 1.379(6) . ?
C10 H10 0.9300 . ?
C11 C18 1.356(6) . ?
C11 C20 1.366(6) . ?
C11 C17 1.507(6) . ?
C12 C33 1.514(6) . ?
C13 C15 1.388(6) . ?
C13 C14 1.462(6) . ?
C13 C23 1.494(6) . ?
C14 C19 1.429(7) . ?
C14 C26 1.499(7) . ?
C15 C21 1.449(6) . ?
C15 C22 1.485(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C27 1.397(7) . ?
C18 H18 0.9300 . ?
C19 C21 1.425(7) . ?
C19 C24 1.510(7) . ?
C20 C29 1.396(8) . ?
C20 H20 0.9300 . ?
C21 C25 1.495(7) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.356(9) . ?
C27 H27 0.9300 . ?
C28 C29 1.335(9) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
O1 C34 1.309(9) . ?
O1 H1 0.8200 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 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
C4 Rh1 N1 78.09(15) . . ?
C4 Rh1 C21 113.78(16) . . ?
N1 Rh1 C21 98.93(17) . . ?
C4 Rh1 C14 113.99(18) . . ?
N1 Rh1 C14 162.61(16) . . ?
C21 Rh1 C14 65.19(19) . . ?
C4 Rh1 C19 96.58(16) . . ?
N1 Rh1 C19 131.14(18) . . ?
C21 Rh1 C19 38.69(18) . . ?
C14 Rh1 C19 38.73(18) . . ?
C4 Rh1 C13 152.64(18) . . ?
N1 Rh1 C13 128.94(16) . . ?
C21 Rh1 C13 63.23(17) . . ?
C14 Rh1 C13 38.81(17) . . ?
C19 Rh1 C13 63.56(17) . . ?
C4 Rh1 C15 152.06(15) . . ?
N1 Rh1 C15 99.79(15) . . ?
C21 Rh1 C15 38.51(16) . . ?
C14 Rh1 C15 63.54(17) . . ?
C19 Rh1 C15 63.53(17) . . ?
C13 Rh1 C15 36.00(15) . . ?
C4 Rh1 Cl1 87.66(10) . . ?
N1 Rh1 Cl1 93.83(9) . . ?
C21 Rh1 Cl1 156.85(13) . . ?
C14 Rh1 Cl1 98.97(15) . . ?
C19 Rh1 Cl1 134.81(17) . . ?
C13 Rh1 Cl1 93.75(12) . . ?
C15 Rh1 Cl1 120.24(12) . . ?
N2 N1 C9 110.7(3) . . ?
N2 N1 Rh1 132.1(3) . . ?
C9 N1 Rh1 116.6(3) . . ?
N1 N2 N3 105.2(3) . . ?
N2 N3 C7 112.2(4) . . ?
N2 N3 C17 119.6(3) . . ?
C7 N3 C17 128.0(4) . . ?
C8 C4 C5 117.3(4) . . ?
C8 C4 Rh1 126.7(3) . . ?
C5 C4 Rh1 116.0(3) . . ?
C6 C5 C4 121.0(4) . . ?
C6 C5 C9 124.5(4) . . ?
C4 C5 C9 114.3(3) . . ?
C10 C6 C5 119.7(4) . . ?
C10 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
N3 C7 C9 105.2(4) . . ?
N3 C7 H7 127.4 . . ?
C9 C7 H7 127.4 . . ?
C12 C8 C4 122.2(4) . . ?
C12 C8 H8 118.9 . . ?
C4 C8 H8 118.9 . . ?
C7 C9 N1 106.7(3) . . ?
C7 C9 C5 139.0(4) . . ?
N1 C9 C5 114.4(4) . . ?
C12 C10 C6 120.8(4) . . ?
C12 C10 H10 119.6 . . ?
C6 C10 H10 119.6 . . ?
C18 C11 C20 118.8(4) . . ?
C18 C11 C17 120.9(4) . . ?
C20 C11 C17 120.3(5) . . ?
C10 C12 C8 119.1(4) . . ?
C10 C12 C33 120.6(4) . . ?
C8 C12 C33 120.3(4) . . ?
C15 C13 C14 108.5(4) . . ?
C15 C13 C23 126.8(5) . . ?
C14 C13 C23 124.7(5) . . ?
C15 C13 Rh1 72.0(2) . . ?
C14 C13 Rh1 66.9(2) . . ?
C23 C13 Rh1 125.3(3) . . ?
C19 C14 C13 107.0(4) . . ?
C19 C14 C26 127.4(5) . . ?
C13 C14 C26 125.0(5) . . ?
C19 C14 Rh1 71.3(3) . . ?
C13 C14 Rh1 74.3(3) . . ?
C26 C14 Rh1 126.8(3) . . ?
C13 C15 C21 108.3(4) . . ?
C13 C15 C22 125.8(4) . . ?
C21 C15 C22 125.9(5) . . ?
C13 C15 Rh1 72.0(2) . . ?
C21 C15 Rh1 66.7(2) . . ?
C22 C15 Rh1 125.9(3) . . ?
N3 C17 C11 112.0(3) . . ?
N3 C17 H17A 109.2 . . ?
C11 C17 H17A 109.2 . . ?
N3 C17 H17B 109.2 . . ?
C11 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C11 C18 C27 120.9(5) . . ?
C11 C18 H18 119.6 . . ?
C27 C18 H18 119.6 . . ?
C21 C19 C14 107.9(4) . . ?
C21 C19 C24 126.1(5) . . ?
C14 C19 C24 126.0(6) . . ?
C21 C19 Rh1 69.6(2) . . ?
C14 C19 Rh1 70.0(2) . . ?
C24 C19 Rh1 127.2(3) . . ?
C11 C20 C29 120.2(6) . . ?
C11 C20 H20 119.9 . . ?
C29 C20 H20 119.9 . . ?
C19 C21 C15 107.9(4) . . ?
C19 C21 C25 127.6(5) . . ?
C15 C21 C25 124.0(5) . . ?
C19 C21 Rh1 71.7(2) . . ?
C15 C21 Rh1 74.8(2) . . ?
C25 C21 Rh1 125.5(3) . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C13 C23 H23A 109.5 . . ?
C13 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C13 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25A 109.5 . . ?
C21 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C21 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C14 C26 H26A 109.5 . . ?
C14 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C14 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C18 119.2(6) . . ?
C28 C27 H27 120.4 . . ?
C18 C27 H27 120.4 . . ?
C29 C28 C27 120.7(6) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C28 C29 C20 120.1(6) . . ?
C28 C29 H29 119.9 . . ?
C20 C29 H29 119.9 . . ?
C12 C33 H33A 109.5 . . ?
C12 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C12 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C34 O1 H1 109.5 . . ?
O1 C34 H34A 109.5 . . ?
O1 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O1 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 Rh1 N1 N2 -177.4(3) . . . . ?
C21 Rh1 N1 N2 -64.8(3) . . . . ?
C14 Rh1 N1 N2 -41.6(7) . . . . ?
C19 Rh1 N1 N2 -89.1(4) . . . . ?
C13 Rh1 N1 N2 -2.2(4) . . . . ?
C15 Rh1 N1 N2 -25.8(3) . . . . ?
Cl1 Rh1 N1 N2 95.8(3) . . . . ?
C4 Rh1 N1 C9 -6.9(2) . . . . ?
C21 Rh1 N1 C9 105.7(3) . . . . ?
C14 Rh1 N1 C9 128.9(5) . . . . ?
C19 Rh1 N1 C9 81.4(3) . . . . ?
C13 Rh1 N1 C9 168.3(2) . . . . ?
C15 Rh1 N1 C9 144.7(3) . . . . ?
Cl1 Rh1 N1 C9 -93.7(2) . . . . ?
C9 N1 N2 N3 0.7(4) . . . . ?
Rh1 N1 N2 N3 171.6(2) . . . . ?
N1 N2 N3 C7 -0.5(4) . . . . ?
N1 N2 N3 C17 -175.7(3) . . . . ?
N1 Rh1 C4 C8 -172.2(4) . . . . ?
C21 Rh1 C4 C8 93.2(4) . . . . ?
C14 Rh1 C4 C8 21.0(4) . . . . ?
C19 Rh1 C4 C8 57.1(4) . . . . ?
C13 Rh1 C4 C8 15.9(5) . . . . ?
C15 Rh1 C4 C8 99.3(5) . . . . ?
Cl1 Rh1 C4 C8 -77.8(3) . . . . ?
N1 Rh1 C4 C5 4.5(3) . . . . ?
C21 Rh1 C4 C5 -90.2(3) . . . . ?
C14 Rh1 C4 C5 -162.4(3) . . . . ?
C19 Rh1 C4 C5 -126.3(3) . . . . ?
C13 Rh1 C4 C5 -167.5(3) . . . . ?
C15 Rh1 C4 C5 -84.0(4) . . . . ?
Cl1 Rh1 C4 C5 98.9(3) . . . . ?
C8 C4 C5 C6 -1.2(5) . . . . ?
Rh1 C4 C5 C6 -178.1(3) . . . . ?
C8 C4 C5 C9 175.3(3) . . . . ?
Rh1 C4 C5 C9 -1.7(4) . . . . ?
C4 C5 C6 C10 0.5(6) . . . . ?
C9 C5 C6 C10 -175.6(3) . . . . ?
N2 N3 C7 C9 0.1(4) . . . . ?
C17 N3 C7 C9 174.8(3) . . . . ?
C5 C4 C8 C12 1.1(6) . . . . ?
Rh1 C4 C8 C12 177.8(3) . . . . ?
N3 C7 C9 N1 0.3(4) . . . . ?
N3 C7 C9 C5 178.7(4) . . . . ?
N2 N1 C9 C7 -0.6(4) . . . . ?
Rh1 N1 C9 C7 -173.1(2) . . . . ?
N2 N1 C9 C5 -179.5(3) . . . . ?
Rh1 N1 C9 C5 8.0(4) . . . . ?
C6 C5 C9 C7 -6.1(7) . . . . ?
C4 C5 C9 C7 177.6(4) . . . . ?
C6 C5 C9 N1 172.2(3) . . . . ?
C4 C5 C9 N1 -4.1(5) . . . . ?
C5 C6 C10 C12 0.3(6) . . . . ?
C6 C10 C12 C8 -0.3(6) . . . . ?
C6 C10 C12 C33 178.5(4) . . . . ?
C4 C8 C12 C10 -0.4(6) . . . . ?
C4 C8 C12 C33 -179.2(4) . . . . ?
C4 Rh1 C13 C15 127.6(3) . . . . ?
N1 Rh1 C13 C15 -42.2(3) . . . . ?
C21 Rh1 C13 C15 37.2(3) . . . . ?
C14 Rh1 C13 C15 120.1(4) . . . . ?
C19 Rh1 C13 C15 80.7(3) . . . . ?
Cl1 Rh1 C13 C15 -140.2(2) . . . . ?
C4 Rh1 C13 C14 7.5(5) . . . . ?
N1 Rh1 C13 C14 -162.4(3) . . . . ?
C21 Rh1 C13 C14 -83.0(3) . . . . ?
C19 Rh1 C13 C14 -39.5(3) . . . . ?
C15 Rh1 C13 C14 -120.1(4) . . . . ?
Cl1 Rh1 C13 C14 99.7(3) . . . . ?
C4 Rh1 C13 C23 -109.6(5) . . . . ?
N1 Rh1 C13 C23 80.5(5) . . . . ?
C21 Rh1 C13 C23 159.9(5) . . . . ?
C14 Rh1 C13 C23 -117.1(6) . . . . ?
C19 Rh1 C13 C23 -156.6(5) . . . . ?
C15 Rh1 C13 C23 122.8(6) . . . . ?
Cl1 Rh1 C13 C23 -17.5(4) . . . . ?
C15 C13 C14 C19 4.1(4) . . . . ?
C23 C13 C14 C19 -177.8(4) . . . . ?
Rh1 C13 C14 C19 64.3(3) . . . . ?
C15 C13 C14 C26 175.6(4) . . . . ?
C23 C13 C14 C26 -6.3(7) . . . . ?
Rh1 C13 C14 C26 -124.2(4) . . . . ?
C15 C13 C14 Rh1 -60.2(3) . . . . ?
C23 C13 C14 Rh1 117.9(4) . . . . ?
C4 Rh1 C14 C19 69.2(3) . . . . ?
N1 Rh1 C14 C19 -62.4(6) . . . . ?
C21 Rh1 C14 C19 -37.0(3) . . . . ?
C13 Rh1 C14 C19 -114.5(4) . . . . ?
C15 Rh1 C14 C19 -79.9(3) . . . . ?
Cl1 Rh1 C14 C19 160.7(3) . . . . ?
C4 Rh1 C14 C13 -176.2(2) . . . . ?
N1 Rh1 C14 C13 52.1(7) . . . . ?
C21 Rh1 C14 C13 77.5(3) . . . . ?
C19 Rh1 C14 C13 114.5(4) . . . . ?
C15 Rh1 C14 C13 34.6(2) . . . . ?
Cl1 Rh1 C14 C13 -84.8(3) . . . . ?
C4 Rh1 C14 C26 -53.9(5) . . . . ?
N1 Rh1 C14 C26 174.4(4) . . . . ?
C21 Rh1 C14 C26 -160.2(6) . . . . ?
C19 Rh1 C14 C26 -123.2(6) . . . . ?
C13 Rh1 C14 C26 122.3(6) . . . . ?
C15 Rh1 C14 C26 156.9(6) . . . . ?
Cl1 Rh1 C14 C26 37.5(5) . . . . ?
C14 C13 C15 C21 0.2(4) . . . . ?
C23 C13 C15 C21 -177.9(4) . . . . ?
Rh1 C13 C15 C21 -56.9(3) . . . . ?
C14 C13 C15 C22 178.8(4) . . . . ?
C23 C13 C15 C22 0.7(7) . . . . ?
Rh1 C13 C15 C22 121.7(4) . . . . ?
C14 C13 C15 Rh1 57.1(3) . . . . ?
C23 C13 C15 Rh1 -121.0(4) . . . . ?
C4 Rh1 C15 C13 -129.0(4) . . . . ?
N1 Rh1 C15 C13 148.0(3) . . . . ?
C21 Rh1 C15 C13 -120.0(4) . . . . ?
C14 Rh1 C15 C13 -37.3(3) . . . . ?
C19 Rh1 C15 C13 -80.7(3) . . . . ?
Cl1 Rh1 C15 C13 47.7(3) . . . . ?
C4 Rh1 C15 C21 -9.1(5) . . . . ?
N1 Rh1 C15 C21 -92.1(3) . . . . ?
C14 Rh1 C15 C21 82.7(3) . . . . ?
C19 Rh1 C15 C21 39.2(3) . . . . ?
C13 Rh1 C15 C21 120.0(4) . . . . ?
Cl1 Rh1 C15 C21 167.6(3) . . . . ?
C4 Rh1 C15 C22 109.4(5) . . . . ?
N1 Rh1 C15 C22 26.4(4) . . . . ?
C21 Rh1 C15 C22 118.5(5) . . . . ?
C14 Rh1 C15 C22 -158.8(5) . . . . ?
C19 Rh1 C15 C22 157.7(5) . . . . ?
C13 Rh1 C15 C22 -121.6(5) . . . . ?
Cl1 Rh1 C15 C22 -73.9(4) . . . . ?
N2 N3 C17 C11 91.0(5) . . . . ?
C7 N3 C17 C11 -83.3(5) . . . . ?
C18 C11 C17 N3 112.1(5) . . . . ?
C20 C11 C17 N3 -69.2(6) . . . . ?
C20 C11 C18 C27 0.1(8) . . . . ?
C17 C11 C18 C27 178.8(5) . . . . ?
C13 C14 C19 C21 -6.8(4) . . . . ?
C26 C14 C19 C21 -178.0(4) . . . . ?
Rh1 C14 C19 C21 59.5(3) . . . . ?
C13 C14 C19 C24 171.7(4) . . . . ?
C26 C14 C19 C24 0.5(7) . . . . ?
Rh1 C14 C19 C24 -122.0(4) . . . . ?
C13 C14 C19 Rh1 -66.3(3) . . . . ?
C26 C14 C19 Rh1 122.5(4) . . . . ?
C4 Rh1 C19 C21 120.4(3) . . . . ?
N1 Rh1 C19 C21 40.4(3) . . . . ?
C14 Rh1 C19 C21 -119.0(4) . . . . ?
C13 Rh1 C19 C21 -79.4(3) . . . . ?
C15 Rh1 C19 C21 -39.0(3) . . . . ?
Cl1 Rh1 C19 C21 -146.4(2) . . . . ?
C4 Rh1 C19 C14 -120.7(3) . . . . ?
N1 Rh1 C19 C14 159.4(2) . . . . ?
C21 Rh1 C19 C14 119.0(4) . . . . ?
C13 Rh1 C19 C14 39.6(3) . . . . ?
C15 Rh1 C19 C14 79.9(3) . . . . ?
Cl1 Rh1 C19 C14 -27.4(3) . . . . ?
C4 Rh1 C19 C24 -0.1(6) . . . . ?
N1 Rh1 C19 C24 -80.0(6) . . . . ?
C21 Rh1 C19 C24 -120.4(7) . . . . ?
C14 Rh1 C19 C24 120.6(7) . . . . ?
C13 Rh1 C19 C24 160.2(6) . . . . ?
C15 Rh1 C19 C24 -159.5(6) . . . . ?
Cl1 Rh1 C19 C24 93.2(6) . . . . ?
C18 C11 C20 C29 0.6(9) . . . . ?
C17 C11 C20 C29 -178.1(5) . . . . ?
C14 C19 C21 C15 6.9(4) . . . . ?
C24 C19 C21 C15 -171.6(4) . . . . ?
Rh1 C19 C21 C15 66.7(3) . . . . ?
C14 C19 C21 C25 179.1(4) . . . . ?
C24 C19 C21 C25 0.6(7) . . . . ?
Rh1 C19 C21 C25 -121.2(5) . . . . ?
C14 C19 C21 Rh1 -59.7(3) . . . . ?
C24 C19 C21 Rh1 121.8(4) . . . . ?
C13 C15 C21 C19 -4.4(4) . . . . ?
C22 C15 C21 C19 177.0(4) . . . . ?
Rh1 C15 C21 C19 -64.6(3) . . . . ?
C13 C15 C21 C25 -176.9(4) . . . . ?
C22 C15 C21 C25 4.5(6) . . . . ?
Rh1 C15 C21 C25 122.9(5) . . . . ?
C13 C15 C21 Rh1 60.2(3) . . . . ?
C22 C15 C21 Rh1 -118.5(4) . . . . ?
C4 Rh1 C21 C19 -69.5(3) . . . . ?
N1 Rh1 C21 C19 -150.4(3) . . . . ?
C14 Rh1 C21 C19 37.1(3) . . . . ?
C13 Rh1 C21 C19 80.3(3) . . . . ?
C15 Rh1 C21 C19 115.1(4) . . . . ?
Cl1 Rh1 C21 C19 87.0(5) . . . . ?
C4 Rh1 C21 C15 175.4(3) . . . . ?
N1 Rh1 C21 C15 94.5(3) . . . . ?
C14 Rh1 C21 C15 -78.0(3) . . . . ?
C19 Rh1 C21 C15 -115.1(4) . . . . ?
C13 Rh1 C21 C15 -34.8(3) . . . . ?
Cl1 Rh1 C21 C15 -28.1(6) . . . . ?
C4 Rh1 C21 C25 54.1(5) . . . . ?
N1 Rh1 C21 C25 -26.7(5) . . . . ?
C14 Rh1 C21 C25 160.7(5) . . . . ?
C19 Rh1 C21 C25 123.7(6) . . . . ?
C13 Rh1 C21 C25 -156.0(5) . . . . ?
C15 Rh1 C21 C25 -121.2(6) . . . . ?
Cl1 Rh1 C21 C25 -149.4(4) . . . . ?
C11 C18 C27 C28 -0.6(9) . . . . ?
C18 C27 C28 C29 0.5(12) . . . . ?
C27 C28 C29 C20 0.2(13) . . . . ?
C11 C20 C29 C28 -0.7(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.394
_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_170930_whh20170612_1
_database_code_depnum_ccdc_archive 'CCDC 1844326'
_audit_update_record             
;
2018-05-21 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H27 N3 O8'
_chemical_formula_weight         509.51

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   P2(1)/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                   13.7264(8)
_cell_length_b                   8.0434(4)
_cell_length_c                   22.4695(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.451(6)
_cell_angle_gamma                90.00
_cell_volume                     2459.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3043
_cell_measurement_theta_min      2.9357
_cell_measurement_theta_max      29.2780

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.38
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9521
_exptl_absorpt_correction_T_max  0.9618
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9889
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4331
_reflns_number_gt                3405
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0625P)²+0.7516P] 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         4331
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1281
_refine_ls_wR_factor_gt          0.1145
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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
O4 O 0.68139(10) 0.62338(17) 0.20207(7) 0.0336(4) Uani 1 1 d . . .
O2 O 0.46839(10) 0.90429(16) 0.16210(6) 0.0277(3) Uani 1 1 d . . .
O5 O 0.27531(11) 0.06017(18) 0.08252(7) 0.0375(4) Uani 1 1 d . . .
O6 O 0.13123(10) 0.09302(18) 0.02481(7) 0.0341(4) Uani 1 1 d . . .
C12 C 0.39845(14) 0.4753(2) 0.23063(9) 0.0222(4) Uani 1 1 d . . .
H12 H 0.4420 0.5064 0.2640 0.027 Uiso 1 1 calc R . .
O1 O 0.52754(12) 0.81229(17) 0.25328(7) 0.0372(4) Uani 1 1 d . . .
C11 C 0.41768(14) 0.5242(2) 0.17382(8) 0.0198(4) Uani 1 1 d . . .
C1 C 0.36839(13) 0.5355(2) 0.06190(8) 0.0196(4) Uani 1 1 d . . .
N1 N 0.40009(11) 0.66983(19) -0.01649(7) 0.0229(4) Uani 1 1 d . . .
N3 N 0.37223(12) 0.4257(2) 0.01577(7) 0.0249(4) Uani 1 1 d . . .
C13 C 0.31661(15) 0.3818(2) 0.23912(9) 0.0242(4) Uani 1 1 d . . .
C2 C 0.38550(14) 0.6918(2) 0.04093(8) 0.0220(4) Uani 1 1 d . . .
H2 H 0.3867 0.7914 0.0620 0.026 Uiso 1 1 calc R . .
O3 O 0.60469(10) 0.38288(17) 0.21072(8) 0.0416(4) Uani 1 1 d . . .
N2 N 0.39128(12) 0.5080(2) -0.03202(7) 0.0259(4) Uani 1 1 d . . .
C26 C 0.60298(14) 0.5264(2) 0.19749(9) 0.0220(4) Uani 1 1 d . . .
O7 O 0.04254(11) 0.2651(2) 0.11630(8) 0.0471(4) Uani 1 1 d . . .
C17 C 0.51215(13) 0.6212(2) 0.17000(9) 0.0200(4) Uani 1 1 d . . .
H17 H 0.5178 0.6412 0.1276 0.024 Uiso 1 1 calc R . .
C23 C 0.19489(14) 0.3287(2) 0.07819(9) 0.0237(4) Uani 1 1 d . . .
H23 H 0.2058 0.3946 0.0430 0.028 Uiso 1 1 calc R . .
C16 C 0.26857(14) 0.3848(2) 0.13104(9) 0.0212(4) Uani 1 1 d . . .
C10 C 0.35112(13) 0.4816(2) 0.12276(8) 0.0187(4) Uani 1 1 d . . .
C15 C 0.25245(14) 0.3374(2) 0.18855(9) 0.0243(4) Uani 1 1 d . . .
H15 H 0.1972 0.2743 0.1933 0.029 Uiso 1 1 calc R . .
C4 C 0.33372(14) 0.8945(2) -0.08488(8) 0.0243(4) Uani 1 1 d . . .
C19 C 0.50581(13) 0.7881(2) 0.20065(9) 0.0222(4) Uani 1 1 d . . .
C3 C 0.42286(15) 0.7937(3) -0.06054(9) 0.0287(5) Uani 1 1 d . . .
H3A H 0.4484 0.7377 -0.0935 0.034 Uiso 1 1 calc R . .
H3B H 0.4735 0.8679 -0.0418 0.034 Uiso 1 1 calc R . .
C21 C 0.20720(14) 0.1457(3) 0.06336(9) 0.0250(5) Uani 1 1 d . . .
C14 C 0.29939(17) 0.3267(3) 0.30090(10) 0.0348(5) Uani 1 1 d . . .
H14A H 0.2463 0.3898 0.3135 0.052 Uiso 1 1 calc R . .
H14B H 0.3579 0.3446 0.3285 0.052 Uiso 1 1 calc R . .
H14C H 0.2829 0.2107 0.3001 0.052 Uiso 1 1 calc R . .
O8 O 0.05937(12) 0.5095(2) 0.07197(9) 0.0500(5) Uani 1 1 d . . .
C9 C 0.25329(15) 0.8148(3) -0.11671(9) 0.0293(5) Uani 1 1 d . . .
H9 H 0.2552 0.7004 -0.1226 0.035 Uiso 1 1 calc R . .
C18 C 0.77456(15) 0.5499(3) 0.22624(10) 0.0323(5) Uani 1 1 d . . .
H18A H 0.7653 0.4794 0.2595 0.048 Uiso 1 1 calc R . .
H18B H 0.8205 0.6364 0.2396 0.048 Uiso 1 1 calc R . .
H18C H 0.7996 0.4853 0.1957 0.048 Uiso 1 1 calc R . .
C8 C 0.17060(16) 0.9033(3) -0.13961(9) 0.0344(5) Uani 1 1 d . . .
H8 H 0.1171 0.8489 -0.1607 0.041 Uiso 1 1 calc R . .
C5 C 0.32936(15) 1.0641(3) -0.07583(9) 0.0292(5) Uani 1 1 d . . .
H5 H 0.3823 1.1187 -0.0542 0.035 Uiso 1 1 calc R . .
C24 C 0.09030(15) 0.3601(3) 0.09132(10) 0.0303(5) Uani 1 1 d . . .
C6 C 0.24646(17) 1.1535(3) -0.09885(10) 0.0354(5) Uani 1 1 d . . .
H6 H 0.2439 1.2677 -0.0926 0.043 Uiso 1 1 calc R . .
C7 C 0.16804(16) 1.0734(3) -0.13095(10) 0.0364(5) Uani 1 1 d . . .
H7 H 0.1130 1.1339 -0.1469 0.044 Uiso 1 1 calc R . .
C20 C 0.45349(17) 1.0653(2) 0.18855(11) 0.0368(6) Uani 1 1 d . . .
H20A H 0.4158 1.0520 0.2214 0.055 Uiso 1 1 calc R . .
H20B H 0.4188 1.1368 0.1588 0.055 Uiso 1 1 calc R . .
H20C H 0.5160 1.1138 0.2030 0.055 Uiso 1 1 calc R . .
C22 C 0.12992(17) -0.0832(3) 0.01131(11) 0.0399(6) Uani 1 1 d . . .
H22A H 0.1901 -0.1136 -0.0034 0.060 Uiso 1 1 calc R . .
H22B H 0.0754 -0.1075 -0.0187 0.060 Uiso 1 1 calc R . .
H22C H 0.1234 -0.1452 0.0471 0.060 Uiso 1 1 calc R . .
C25 C -0.0384(2) 0.5526(4) 0.08539(17) 0.0780(10) Uani 1 1 d . . .
H25A H -0.0853 0.4753 0.0659 0.117 Uiso 1 1 calc R . .
H25B H -0.0547 0.6630 0.0712 0.117 Uiso 1 1 calc R . .
H25C H -0.0396 0.5480 0.1280 0.117 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
O4 C26 1.322(2) . ?
O4 C18 1.449(2) . ?
O2 C19 1.331(2) . ?
O2 C20 1.451(2) . ?
O5 C21 1.195(2) . ?
O6 C21 1.335(2) . ?
O6 C22 1.449(2) . ?
C12 C13 1.385(3) . ?
C12 C11 1.393(3) . ?
C12 H12 0.9300 . ?
O1 C19 1.197(2) . ?
C11 C10 1.413(3) . ?
C11 C17 1.525(3) . ?
C1 N3 1.368(2) . ?
C1 C2 1.373(3) . ?
C1 C10 1.483(3) . ?
N1 C2 1.343(2) . ?
N1 N2 1.349(2) . ?
N1 C3 1.467(3) . ?
N3 N2 1.316(2) . ?
C13 C15 1.391(3) . ?
C13 C14 1.505(3) . ?
C2 H2 0.9300 . ?
O3 C26 1.191(2) . ?
C26 C17 1.522(3) . ?
O7 C24 1.193(3) . ?
C17 C19 1.517(3) . ?
C17 H17 0.9800 . ?
C23 C21 1.523(3) . ?
C23 C24 1.524(3) . ?
C23 C16 1.525(3) . ?
C23 H23 0.9800 . ?
C16 C15 1.392(3) . ?
C16 C10 1.407(3) . ?
C15 H15 0.9300 . ?
C4 C5 1.382(3) . ?
C4 C9 1.392(3) . ?
C4 C3 1.510(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
O8 C24 1.329(3) . ?
O8 C25 1.455(3) . ?
C9 C8 1.382(3) . ?
C9 H9 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C8 C7 1.383(3) . ?
C8 H8 0.9300 . ?
C5 C6 1.388(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.376(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 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
C26 O4 C18 117.28(15) . . ?
C19 O2 C20 115.05(16) . . ?
C21 O6 C22 115.71(16) . . ?
C13 C12 C11 122.19(18) . . ?
C13 C12 H12 118.9 . . ?
C11 C12 H12 118.9 . . ?
C12 C11 C10 119.73(17) . . ?
C12 C11 C17 117.36(16) . . ?
C10 C11 C17 122.91(17) . . ?
N3 C1 C2 107.80(17) . . ?
N3 C1 C10 122.46(16) . . ?
C2 C1 C10 129.72(17) . . ?
C2 N1 N2 110.85(15) . . ?
C2 N1 C3 129.10(16) . . ?
N2 N1 C3 120.05(16) . . ?
N2 N3 C1 108.95(15) . . ?
C12 C13 C15 117.77(18) . . ?
C12 C13 C14 120.92(18) . . ?
C15 C13 C14 121.29(18) . . ?
N1 C2 C1 105.24(16) . . ?
N1 C2 H2 127.4 . . ?
C1 C2 H2 127.4 . . ?
N3 N2 N1 107.15(15) . . ?
O3 C26 O4 124.24(18) . . ?
O3 C26 C17 125.11(17) . . ?
O4 C26 C17 110.58(16) . . ?
C19 C17 C26 110.57(15) . . ?
C19 C17 C11 109.14(15) . . ?
C26 C17 C11 112.24(15) . . ?
C19 C17 H17 108.3 . . ?
C26 C17 H17 108.3 . . ?
C11 C17 H17 108.3 . . ?
C21 C23 C24 109.66(16) . . ?
C21 C23 C16 112.03(16) . . ?
C24 C23 C16 110.28(16) . . ?
C21 C23 H23 108.3 . . ?
C24 C23 H23 108.3 . . ?
C16 C23 H23 108.3 . . ?
C15 C16 C10 120.12(17) . . ?
C15 C16 C23 118.22(16) . . ?
C10 C16 C23 121.67(17) . . ?
C16 C10 C11 118.30(17) . . ?
C16 C10 C1 120.77(16) . . ?
C11 C10 C1 120.93(16) . . ?
C13 C15 C16 121.87(18) . . ?
C13 C15 H15 119.1 . . ?
C16 C15 H15 119.1 . . ?
C5 C4 C9 118.94(18) . . ?
C5 C4 C3 121.68(18) . . ?
C9 C4 C3 119.38(18) . . ?
O1 C19 O2 123.66(18) . . ?
O1 C19 C17 124.80(17) . . ?
O2 C19 C17 111.47(16) . . ?
N1 C3 C4 112.05(16) . . ?
N1 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
N1 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
O5 C21 O6 124.02(19) . . ?
O5 C21 C23 125.53(18) . . ?
O6 C21 C23 110.45(17) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C24 O8 C25 114.3(2) . . ?
C8 C9 C4 120.8(2) . . ?
C8 C9 H9 119.6 . . ?
C4 C9 H9 119.6 . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C9 C8 C7 119.5(2) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C4 C5 C6 120.37(19) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
O7 C24 O8 124.1(2) . . ?
O7 C24 C23 125.0(2) . . ?
O8 C24 C23 110.82(19) . . ?
C7 C6 C5 120.0(2) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 120.3(2) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
O2 C20 H20A 109.5 . . ?
O2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O6 C22 H22A 109.5 . . ?
O6 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O6 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O8 C25 H25A 109.5 . . ?
O8 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O8 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.052
####################################################################### 
# 
# 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_170420_whh20170329_1
_database_code_depnum_ccdc_archive 'CCDC 1844334'
_audit_update_record             
;
2018-05-21 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H45 N3 O6'
_chemical_formula_weight         651.78

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.6158(11)
_cell_length_b                   14.3878(19)
_cell_length_c                   15.7308(15)
_cell_angle_alpha                63.487(11)
_cell_angle_beta                 72.881(9)
_cell_angle_gamma                74.459(11)
_cell_volume                     1837.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1655
_cell_measurement_theta_min      3.1680
_cell_measurement_theta_max      29.2082

_exptl_crystal_description       colorless
_exptl_crystal_colour            block
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.38
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9628
_exptl_absorpt_correction_T_max  0.9704
_exptl_absorpt_process_details   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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10782
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_sigmaI/netI    0.1121
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6457
_reflns_number_gt                2472
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1943P)²+0.2427P] 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         6457
_refine_ls_number_parameters     437
_refine_ls_number_restraints     164
_refine_ls_R_factor_all          0.2250
_refine_ls_R_factor_gt           0.1104
_refine_ls_wR_factor_ref         0.4014
_refine_ls_wR_factor_gt          0.2908
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.492
_refine_ls_shift/su_mean         0.009

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
O6 O 0.5894(4) -0.1658(3) 0.4672(2) 0.0784(12) Uani 1 1 d . . .
O5 O 0.3925(4) -0.0392(3) 0.4507(3) 0.0847(13) Uani 1 1 d . . .
C21 C 0.3971(6) 0.1141(4) 0.2335(4) 0.0674(15) Uani 1 1 d . . .
H21 H 0.3228 0.0708 0.2598 0.081 Uiso 1 1 calc R . .
N1 N 0.9690(5) 0.0024(4) 0.3208(3) 0.0771(14) Uani 1 1 d . . .
C22 C 0.5382(5) 0.0692(4) 0.2508(3) 0.0596(14) Uani 1 1 d . . .
C23 C 0.6492(6) 0.1306(4) 0.2132(3) 0.0636(15) Uani 1 1 d . . .
O4 O 0.4090(4) -0.1549(4) 0.3178(3) 0.0943(14) Uani 1 1 d . . .
C20 C 0.3621(7) 0.2202(5) 0.1789(4) 0.0766(17) Uani 1 1 d . . .
C35 C 0.5708(5) -0.0497(4) 0.3085(3) 0.0593(14) Uani 1 1 d . . .
H35 H 0.6802 -0.0712 0.3005 0.071 Uiso 1 1 calc R . .
C19 C 0.4777(8) 0.2802(4) 0.1377(4) 0.0798(18) Uani 1 1 d . . .
H19 H 0.4572 0.3528 0.0977 0.096 Uiso 1 1 calc R . .
C33 C 0.7961(6) 0.0829(4) 0.2402(4) 0.0635(15) Uani 1 1 d . . .
C36 C 0.5127(6) -0.1084(4) 0.2690(4) 0.0665(15) Uani 1 1 d . . .
C18 C 0.6197(6) 0.2374(4) 0.1532(4) 0.0669(15) Uani 1 1 d . . .
N2 N 1.0263(6) 0.0161(5) 0.2293(4) 0.0941(17) Uani 1 1 d . . .
C9 C 0.5813(6) -0.1055(4) 0.1715(4) 0.0650(15) Uani 1 1 d . . .
N3 N 0.9216(6) 0.0660(4) 0.1792(4) 0.0912(17) Uani 1 1 d . . .
C39 C 0.5054(7) -0.0813(5) 0.4160(4) 0.0672(15) Uani 1 1 d . . .
C34 C 0.8275(6) 0.0426(5) 0.3295(4) 0.0733(16) Uani 1 1 d . . .
H34 H 0.7605 0.0432 0.3874 0.088 Uiso 1 1 calc R . .
C37 C 0.5407(7) -0.2089(5) 0.5719(4) 0.092(2) Uani 1 1 d D . .
H37A H 0.4434 -0.2310 0.5900 0.110 Uiso 1 1 calc R . .
H37B H 0.5313 -0.1551 0.5971 0.110 Uiso 1 1 calc R . .
C8 C 0.7135(6) -0.0698(5) 0.1193(4) 0.0830(18) Uani 1 1 d . . .
H8 H 0.7645 -0.0445 0.1459 0.100 Uiso 1 1 calc R . .
C14 C 0.7366(7) 0.3080(4) 0.1054(4) 0.0812(18) Uani 1 1 d . . .
H14 H 0.8342 0.2613 0.1025 0.097 Uiso 1 1 calc R . .
O1 O 0.6781(7) 0.4753(4) -0.0148(4) 0.132(2) Uani 1 1 d . . .
O2 O 0.8574(7) 0.4151(5) 0.1267(4) 0.134(2) Uani 1 1 d . . .
C24 C 0.2063(7) 0.2693(6) 0.1658(5) 0.106(2) Uani 1 1 d . . .
H24A H 0.1484 0.2138 0.1851 0.159 Uiso 1 1 calc R . .
H24B H 0.2069 0.3162 0.0975 0.159 Uiso 1 1 calc R . .
H24C H 0.1622 0.3097 0.2062 0.159 Uiso 1 1 calc R . .
C17 C 0.7380(9) 0.3684(6) 0.1604(5) 0.098(2) Uani 1 1 d . . .
C6 C 0.7565(8) 0.3392(6) -0.0737(4) 0.093(2) Uani 1 1 d . . .
C10 C 0.5145(8) -0.1436(6) 0.1290(5) 0.099(2) Uani 1 1 d . . .
H10 H 0.4265 -0.1725 0.1643 0.119 Uiso 1 1 calc R . .
C25 C 1.0588(7) -0.0579(6) 0.3952(5) 0.101(2) Uani 1 1 d DU . .
H25A H 1.0718 -0.0107 0.4216 0.121 Uiso 1 1 calc R . .
H25B H 1.1576 -0.0847 0.3648 0.121 Uiso 1 1 calc R . .
C7 C 0.7716(8) -0.0712(6) 0.0275(5) 0.099(2) Uani 1 1 d . . .
H7 H 0.8624 -0.0464 -0.0074 0.118 Uiso 1 1 calc R . .
C13 C 0.7236(8) 0.3801(6) 0.0028(5) 0.097(2) Uani 1 1 d . . .
C11 C 0.5733(10) -0.1405(7) 0.0362(6) 0.114(2) Uani 1 1 d . . .
H11 H 0.5219 -0.1623 0.0070 0.136 Uiso 1 1 calc R . .
C1 C 0.8343(9) 0.2435(7) -0.0647(5) 0.110(2) Uani 1 1 d . . .
H1 H 0.8682 0.1977 -0.0064 0.132 Uiso 1 1 calc R . .
C3 C 0.8103(15) 0.2756(12) -0.2225(8) 0.158(4) Uani 1 1 d . . .
H3 H 0.8265 0.2531 -0.2733 0.190 Uiso 1 1 calc R . .
C12 C 0.7049(10) -0.1060(7) -0.0133(5) 0.114(3) Uani 1 1 d . . .
H12 H 0.7481 -0.1068 -0.0757 0.137 Uiso 1 1 calc R . .
C40 C 0.6507(10) -0.2996(7) 0.6131(5) 0.147(4) Uani 1 1 d D . .
H40A H 0.6527 -0.3550 0.5923 0.221 Uiso 1 1 calc R . .
H40B H 0.6247 -0.3265 0.6840 0.221 Uiso 1 1 calc R . .
H40C H 0.7480 -0.2781 0.5903 0.221 Uiso 1 1 calc R . .
O3 O 0.6511(9) 0.3757(6) 0.2270(5) 0.177(3) Uani 1 1 d . . .
C2 C 0.8650(11) 0.2118(8) -0.1398(8) 0.137(3) Uani 1 1 d . . .
H2 H 0.9240 0.1456 -0.1345 0.165 Uiso 1 1 calc R . .
C4 C 0.7326(16) 0.3719(12) -0.2295(8) 0.169(5) Uani 1 1 d . . .
H4 H 0.6970 0.4179 -0.2871 0.203 Uiso 1 1 calc R . .
C5 C 0.7053(11) 0.4031(8) -0.1576(7) 0.138(3) Uani 1 1 d . . .
H5 H 0.6496 0.4705 -0.1644 0.166 Uiso 1 1 calc R . .
C26 C 0.9922(11) -0.1468(7) 0.4749(7) 0.146(3) Uani 1 1 d DU . .
H26A H 0.9751 -0.1915 0.4471 0.175 Uiso 1 1 calc R . .
H26B H 0.8947 -0.1188 0.5057 0.175 Uiso 1 1 calc R . .
C27 C 1.0786(14) -0.2139(10) 0.5511(8) 0.175(4) Uani 1 1 d DU . .
H27A H 1.1318 -0.1677 0.5571 0.210 Uiso 1 1 calc R . .
H27B H 1.0072 -0.2401 0.6131 0.210 Uiso 1 1 calc R . .
C15 C 0.8694(15) 0.4845(8) 0.1664(8) 0.167(4) Uani 1 1 d D . .
H15A H 0.8018 0.4695 0.2305 0.200 Uiso 1 1 calc R . .
H15B H 0.9712 0.4701 0.1767 0.200 Uiso 1 1 calc R . .
C16 C 0.837(2) 0.5889(10) 0.1078(9) 0.234(8) Uani 1 1 d D . .
H16A H 0.8751 0.5992 0.0397 0.351 Uiso 1 1 calc R . .
H16B H 0.8820 0.6313 0.1234 0.351 Uiso 1 1 calc R . .
H16C H 0.7295 0.6108 0.1185 0.351 Uiso 1 1 calc R . .
C30 C 1.233(3) -0.485(2) 0.551(2) 0.419(16) Uani 1 1 d DU . .
H30A H 1.2126 -0.4959 0.4980 0.503 Uiso 1 1 calc R . .
H30B H 1.3229 -0.4521 0.5200 0.503 Uiso 1 1 calc R . .
C38 C 1.174(3) -0.638(3) 0.6513(19) 0.376(15) Uani 1 1 d DU . .
H38A H 1.0901 -0.5921 0.6219 0.564 Uiso 1 1 calc R . .
H38B H 1.1563 -0.6450 0.7183 0.564 Uiso 1 1 calc R . .
H38C H 1.1851 -0.7076 0.6509 0.564 Uiso 1 1 calc R . .
C28 C 1.1865(18) -0.3051(14) 0.5435(12) 0.229(7) Uani 1 1 d DU . .
H28A H 1.2656 -0.2794 0.4861 0.275 Uiso 1 1 calc R . .
H28B H 1.2319 -0.3393 0.6014 0.275 Uiso 1 1 calc R . .
C29 C 1.129(2) -0.3840(16) 0.5354(15) 0.256(8) Uani 1 1 d DU . .
H29A H 1.1063 -0.3555 0.4702 0.307 Uiso 1 1 calc R . .
H29B H 1.0360 -0.3980 0.5837 0.307 Uiso 1 1 calc R . .
C31 C 1.310(3) -0.592(2) 0.595(3) 0.475(19) Uani 1 1 d DU . .
H31A H 1.3740 -0.5976 0.6368 0.570 Uiso 1 1 calc R . .
H31B H 1.3674 -0.6215 0.5465 0.570 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
O6 C39 1.328(7) . ?
O6 C37 1.452(6) . ?
O5 C39 1.198(6) . ?
C21 C20 1.381(8) . ?
C21 C22 1.387(7) . ?
N1 C34 1.321(7) . ?
N1 N2 1.323(7) . ?
N1 C25 1.468(8) . ?
C22 C23 1.391(7) . ?
C22 C35 1.530(7) . ?
C23 C18 1.402(7) . ?
C23 C33 1.490(7) . ?
O4 C36 1.216(6) . ?
C20 C19 1.412(9) . ?
C20 C24 1.507(9) . ?
C35 C39 1.517(7) . ?
C35 C36 1.530(8) . ?
C19 C18 1.384(8) . ?
C33 N3 1.343(6) . ?
C33 C34 1.353(8) . ?
C36 C9 1.467(7) . ?
C18 C14 1.513(8) . ?
N2 N3 1.313(7) . ?
C9 C8 1.383(7) . ?
C9 C10 1.389(9) . ?
C37 C40 1.467(8) . ?
C8 C7 1.395(9) . ?
C14 C17 1.479(10) . ?
C14 C13 1.501(9) . ?
O1 C13 1.247(8) . ?
O2 C17 1.337(9) . ?
O2 C15 1.436(11) . ?
C17 O3 1.159(8) . ?
C6 C1 1.346(10) . ?
C6 C5 1.374(11) . ?
C6 C13 1.484(10) . ?
C10 C11 1.385(10) . ?
C25 C26 1.468(9) . ?
C7 C12 1.331(10) . ?
C11 C12 1.366(10) . ?
C1 C2 1.377(12) . ?
C3 C4 1.359(15) . ?
C3 C2 1.374(15) . ?
C4 C5 1.328(14) . ?
C26 C27 1.478(10) . ?
C27 C28 1.466(12) . ?
C15 C16 1.374(11) . ?
C30 C31 1.464(14) . ?
C30 C29 1.487(14) . ?
C38 C31 1.484(15) . ?
C28 C29 1.454(13) . ?

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
C39 O6 C37 117.3(4) . . ?
C20 C21 C22 121.5(5) . . ?
C34 N1 N2 109.4(5) . . ?
C34 N1 C25 130.2(5) . . ?
N2 N1 C25 120.2(5) . . ?
C21 C22 C23 120.5(5) . . ?
C21 C22 C35 118.7(5) . . ?
C23 C22 C35 120.7(5) . . ?
C22 C23 C18 119.5(5) . . ?
C22 C23 C33 119.6(4) . . ?
C18 C23 C33 120.8(5) . . ?
C21 C20 C19 117.1(5) . . ?
C21 C20 C24 121.0(6) . . ?
C19 C20 C24 121.9(5) . . ?
C39 C35 C36 109.6(4) . . ?
C39 C35 C22 112.2(4) . . ?
C36 C35 C22 110.4(4) . . ?
C18 C19 C20 122.6(5) . . ?
N3 C33 C34 107.3(5) . . ?
N3 C33 C23 125.1(5) . . ?
C34 C33 C23 127.5(4) . . ?
O4 C36 C9 121.1(6) . . ?
O4 C36 C35 119.8(5) . . ?
C9 C36 C35 119.1(5) . . ?
C19 C18 C23 118.6(5) . . ?
C19 C18 C14 118.8(5) . . ?
C23 C18 C14 122.7(5) . . ?
N3 N2 N1 108.2(4) . . ?
C8 C9 C10 117.0(5) . . ?
C8 C9 C36 123.7(6) . . ?
C10 C9 C36 119.3(5) . . ?
N2 N3 C33 108.3(5) . . ?
O5 C39 O6 124.2(5) . . ?
O5 C39 C35 125.9(6) . . ?
O6 C39 C35 109.9(5) . . ?
N1 C34 C33 106.8(5) . . ?
O6 C37 C40 107.9(5) . . ?
C9 C8 C7 119.7(7) . . ?
C17 C14 C13 110.7(5) . . ?
C17 C14 C18 113.6(5) . . ?
C13 C14 C18 111.2(6) . . ?
C17 O2 C15 119.4(8) . . ?
O3 C17 O2 120.6(8) . . ?
O3 C17 C14 126.9(7) . . ?
O2 C17 C14 112.4(6) . . ?
C1 C6 C5 119.0(8) . . ?
C1 C6 C13 123.2(7) . . ?
C5 C6 C13 117.8(8) . . ?
C11 C10 C9 121.5(7) . . ?
N1 C25 C26 112.4(6) . . ?
C12 C7 C8 122.7(7) . . ?
O1 C13 C6 121.3(7) . . ?
O1 C13 C14 117.3(7) . . ?
C6 C13 C14 121.4(7) . . ?
C12 C11 C10 120.3(8) . . ?
C6 C1 C2 120.2(8) . . ?
C4 C3 C2 118.3(10) . . ?
C7 C12 C11 118.7(7) . . ?
C3 C2 C1 120.1(10) . . ?
C5 C4 C3 121.5(11) . . ?
C4 C5 C6 120.9(10) . . ?
C25 C26 C27 115.8(8) . . ?
C28 C27 C26 120.9(12) . . ?
C16 C15 O2 112.9(10) . . ?
C31 C30 C29 163(3) . . ?
C29 C28 C27 115.8(16) . . ?
C28 C29 C30 114(2) . . ?
C30 C31 C38 95(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.057
