# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

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

data_tt
_audit_block_doi                 10.5517/ccdc.csd.cc22hmgp
_database_code_depnum_ccdc_archive 'CCDC 1921642'
loop_
_audit_author_name
_audit_author_address
'John Low'
;University of Aberdeen
United Kingdom
;
_audit_update_record             
;
2019-06-11 deposited with the CCDC.	2019-08-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_tt                  
;
PROBLEM: Check Calcd Resid. Dens.  1.13A   From I4             -3.39 eA-3
RESPONSE: Thia is close to an I atom with a large ADP. An attempt to split the atom into two componenets was not successful.
;
# Added during the CSD deposition process: Tuesday 11 June 2019 06:13 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C57 H85 I3 O3'
_chemical_formula_weight         1198.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   6.12470(10)
_cell_length_b                   22.0786(2)
_cell_length_c                   22.7088(2)
_cell_angle_alpha                117.8960(10)
_cell_angle_beta                 90.6720(10)
_cell_angle_gamma                92.1240(10)
_cell_volume                     2710.63(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    41807
_cell_measurement_theta_min      2.1820
_cell_measurement_theta_max      70.1820

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_F_000             1220
_exptl_transmission_factor_min   0.0
_exptl_transmission_factor_max   1.0
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    13.885
_shelx_estimated_absorpt_T_min   0.068
_shelx_estimated_absorpt_T_max   0.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;



_diffrn_radiation_type           CuK\a
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'

_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter χ goniometer'
_diffrn_measurement_device_type  
;
Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer 
and HyPix 6000 detector
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'


_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Varimax focusing mirrors'
_diffrn_radiation_probe          x-ray

_diffrn_ambient_temperature      100(2)

_diffrn_source                   'Rotating anode'
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_source_current           30.0
_diffrn_source_target            Cu
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_number            48921
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.203
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             15680
_reflns_number_gt                15145
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_max     0.991
_reflns_Friedel_fraction_full    0.993

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

_computing_data_collection       
'CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)'
_computing_cell_refinement       
'CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)'
_computing_data_reduction        
'CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)'

_computing_structure_solution    
;
Oscail (McArdle et al., 2004)
SHELXT (Sheldrick, 2015)
OLEX2  (Dolmanov et al., 2009)
;
_computing_structure_refinement  
;
Oscail (McArdle et al., 2004),
ShelXle (Hübschle et al., 2011)
SHELXL-2017/1 (Sheldrick, 2017)
OLEX2  (Dolmanov et al., 2009)
;

_computing_molecular_graphics    ' Mercury (Macrae et al, 2006)'

_computing_publication_material  
;
Oscail (McArdle et al., 2004),
SHELXL-2017/1 (Sheldrick, 2017)
PLATON (Spek, 2009)
OLEX2  (Dolmanov et al., 2009)
;

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0773P)²+4.1292P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.025(7)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         15680
_refine_ls_number_parameters     1153
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1214
_refine_ls_wR_factor_gt          0.1205
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.63735(9) -0.15785(3) 0.27430(3) 0.03279(15) Uani 1 1 d . . . . .
I2 I 0.64962(9) 0.69444(3) -0.10083(3) 0.03251(15) Uani 1 1 d . . . . .
I3 I 0.69675(17) 0.33975(5) 1.10077(4) 0.0625(3) Uani 1 1 d . . . . .
I4 I 0.2945(3) 1.09422(6) 0.86092(11) 0.1267(7) Uani 1 1 d . . . . .
I5 I 0.36373(9) 1.15761(3) 0.69711(3) 0.02900(14) Uani 1 1 d . . . . .
I6 I 0.87569(9) -0.09425(3) 0.05876(3) 0.03000(14) Uani 1 1 d . . . . .
O1 O 0.2024(12) 0.4236(3) 0.5641(4) 0.0374(16) Uani 1 1 d . . . . .
H1OA H 0.311051 0.451548 0.577979 0.056 Uiso 1 1 calc R U . . .
O2 O 0.1529(11) 0.5334(3) 0.3070(3) 0.0282(14) Uani 1 1 d . . . . .
H20A H 0.021946 0.525768 0.313861 0.042 Uiso 1 1 d R U . . .
O3 O 0.9054(14) 0.4654(4) 0.6579(4) 0.0444(18) Uani 1 1 d . . . . .
H3OA H 1.003725 0.450212 0.629842 0.067 Uiso 1 1 calc R U . . .
O4 O 0.5323(15) 0.5087(4) 0.6385(5) 0.054(2) Uani 1 1 d . . . . .
H4OA H 0.658077 0.496397 0.641841 0.081 Uiso 1 1 calc R U . . .
O5 O 0.8115(12) 0.5828(3) 0.3850(4) 0.0337(15) Uani 1 1 d . . . . .
H5OA H 0.714987 0.553365 0.360584 0.051 Uiso 1 1 calc R U . . .
O6 O 0.4778(12) 0.4886(3) 0.3544(3) 0.0302(14) Uani 1 1 d . . . . .
H6OA H 0.373900 0.502107 0.339817 0.045 Uiso 1 1 calc R U . . .
C1 C 0.4692(15) -0.0743(5) 0.2743(4) 0.0260(18) Uani 1 1 d . . . . .
H1 H 0.575929 -0.053185 0.255395 0.031 Uiso 1 1 calc R U . . .
C2 C 0.4152(14) -0.0144(4) 0.3424(4) 0.0168(16) Uani 1 1 d . . . . .
C3 C 0.2843(13) 0.0258(4) 0.3152(4) 0.0178(16) Uani 1 1 d . . . . .
H3 H 0.393956 0.042047 0.292763 0.021 Uiso 1 1 calc R U . . .
C4 C 0.1346(14) -0.0274(4) 0.2584(4) 0.0203(16) Uani 1 1 d . . . . .
H4A H 0.103403 -0.012478 0.224382 0.024 Uiso 1 1 calc R U . . .
H4AB H -0.005040 -0.035797 0.275461 0.024 Uiso 1 1 calc R U . . .
C5 C 0.2737(17) -0.0928(5) 0.2293(4) 0.0282(19) Uani 1 1 d . . . . .
H5A H 0.189557 -0.132316 0.228587 0.034 Uiso 1 1 calc R U . . .
H5AB H 0.316398 -0.104979 0.183291 0.034 Uiso 1 1 calc R U . . .
C6 C 0.1920(13) 0.0907(4) 0.3691(4) 0.0172(15) Uani 1 1 d . . . . .
H6 H 0.088075 0.077876 0.395506 0.021 Uiso 1 1 calc R U . . .
C7 C 0.3780(13) 0.1375(4) 0.4159(4) 0.0181(16) Uani 1 1 d . . . . .
H7 H 0.471357 0.151981 0.388418 0.022 Uiso 1 1 calc R U . . .
C8 C 0.5265(14) 0.0984(4) 0.4405(4) 0.0215(17) Uani 1 1 d . . . . .
H8A H 0.445495 0.087911 0.472353 0.026 Uiso 1 1 calc R U . . .
H8AB H 0.655629 0.128551 0.464768 0.026 Uiso 1 1 calc R U . . .
C9 C 0.6059(15) 0.0306(5) 0.3838(4) 0.0206(16) Uani 1 1 d . . . . .
H9A H 0.704930 0.041008 0.355251 0.025 Uiso 1 1 calc R U . . .
H9AB H 0.688829 0.006230 0.403275 0.025 Uiso 1 1 calc R U . . .
C10 C 0.2932(13) 0.2046(4) 0.4731(4) 0.0190(16) Uani 1 1 d . . . . .
C11 C 0.1256(14) 0.2351(4) 0.4460(4) 0.0209(16) Uani 1 1 d . . . . .
C12 C 0.0714(15) 0.3091(4) 0.4917(5) 0.0275(19) Uani 1 1 d . . . . .
H12A H -0.023354 0.325334 0.466907 0.033 Uiso 1 1 calc R U . . .
H12B H -0.011187 0.311058 0.529754 0.033 Uiso 1 1 calc R U . . .
C13 C 0.2732(16) 0.3560(5) 0.5179(5) 0.0284(19) Uani 1 1 d . . . . .
H13 H 0.348212 0.358340 0.480087 0.034 Uiso 1 1 calc R U . . .
C14 C 0.4278(15) 0.3295(5) 0.5523(5) 0.0276(19) Uani 1 1 d . . . . .
H14A H 0.355830 0.328891 0.590834 0.033 Uiso 1 1 calc R U . . .
H14B H 0.560391 0.360440 0.569099 0.033 Uiso 1 1 calc R U . . .
C15 C 0.4937(15) 0.2557(5) 0.5028(4) 0.0247(18) Uani 1 1 d . . . . .
H15A H 0.574749 0.257245 0.466004 0.030 Uiso 1 1 calc R U . . .
H15B H 0.592628 0.239020 0.526256 0.030 Uiso 1 1 calc R U . . .
C16 C 0.0313(14) 0.2013(4) 0.3862(4) 0.0215(17) Uani 1 1 d . . . . .
H16 H -0.067096 0.225401 0.373046 0.026 Uiso 1 1 calc R U . . .
C17 C 0.0667(15) 0.1281(4) 0.3372(4) 0.0205(16) Uani 1 1 d . . . . .
H17A H 0.150201 0.126747 0.299565 0.025 Uiso 1 1 calc R U . . .
H17B H -0.076712 0.103694 0.319148 0.025 Uiso 1 1 calc R U . . .
C18 C 0.1897(16) 0.1913(5) 0.5278(4) 0.0266(19) Uani 1 1 d . . . . .
H18A H 0.102774 0.230211 0.556255 0.040 Uiso 1 1 calc R U . . .
H18B H 0.305351 0.185887 0.554919 0.040 Uiso 1 1 calc R U . . .
H18C H 0.095017 0.149401 0.507046 0.040 Uiso 1 1 calc R U . . .
C19 C 0.2737(15) -0.0427(5) 0.3806(4) 0.0241(18) Uani 1 1 d . . . . .
H19A H 0.227612 -0.004559 0.422205 0.036 Uiso 1 1 calc R U . . .
H19B H 0.359270 -0.073440 0.390946 0.036 Uiso 1 1 calc R U . . .
H19C H 0.144496 -0.068184 0.353088 0.036 Uiso 1 1 calc R U . . .
C20 C 0.4841(17) 0.7222(5) -0.0097(5) 0.033(2) Uani 1 1 d . . . . .
H20 H 0.591170 0.753268 0.026356 0.039 Uiso 1 1 calc R U . . .
C21 C 0.4230(14) 0.6647(4) 0.0072(4) 0.0193(16) Uani 1 1 d . . . . .
C22 C 0.2926(13) 0.7082(4) 0.0700(4) 0.0180(16) Uani 1 1 d . . . . .
H22 H 0.400875 0.741851 0.103830 0.022 Uiso 1 1 calc R U . . .
C23 C 0.1470(14) 0.7499(5) 0.0488(4) 0.0225(17) Uani 1 1 d . . . . .
H23A H 0.110523 0.793359 0.087748 0.027 Uiso 1 1 calc R U . . .
H23B H 0.009761 0.723430 0.026595 0.027 Uiso 1 1 calc R U . . .
C24 C 0.2865(15) 0.7639(5) -0.0003(4) 0.0239(18) Uani 1 1 d . . . . .
H24A H 0.205348 0.748990 -0.043191 0.029 Uiso 1 1 calc R U . . .
H24B H 0.329118 0.813350 0.018731 0.029 Uiso 1 1 calc R U . . .
C25 C 0.1902(12) 0.6662(4) 0.1014(4) 0.0154(15) Uani 1 1 d . . . . .
H25 H 0.082112 0.630810 0.069113 0.019 Uiso 1 1 calc R U . . .
C26 C 0.3749(14) 0.6304(4) 0.1193(4) 0.0187(16) Uani 1 1 d . . . . .
H26 H 0.466876 0.667546 0.156002 0.022 Uiso 1 1 calc R U . . .
C27 C 0.5274(15) 0.5924(4) 0.0602(4) 0.0239(18) Uani 1 1 d . . . . .
H27A H 0.654265 0.577204 0.076422 0.029 Uiso 1 1 calc R U . . .
H27B H 0.447117 0.550903 0.025828 0.029 Uiso 1 1 calc R U . . .
C28 C 0.6112(14) 0.6355(5) 0.0281(5) 0.0233(17) Uani 1 1 d . . . . .
H28A H 0.709938 0.673466 0.060151 0.028 Uiso 1 1 calc R U . . .
H28B H 0.695815 0.606690 -0.011426 0.028 Uiso 1 1 calc R U . . .
C29 C 0.2807(14) 0.5824(4) 0.1471(4) 0.0190(16) Uani 1 1 d . . . . .
C30 C 0.1051(13) 0.6187(4) 0.1975(4) 0.0190(16) Uani 1 1 d . . . . .
C31 C 0.0323(13) 0.5837(4) 0.2381(4) 0.0208(16) Uani 1 1 d . . . . .
H31A H -0.071021 0.612815 0.271808 0.025 Uiso 1 1 calc R U . . .
H31B H -0.045872 0.539472 0.208342 0.025 Uiso 1 1 calc R U . . .
C32 C 0.2234(14) 0.5708(4) 0.2730(4) 0.0217(17) Uani 1 1 d . . . . .
H32 H 0.291600 0.615972 0.306401 0.026 Uiso 1 1 calc R U . . .
C33 C 0.3945(15) 0.5309(5) 0.2238(5) 0.0246(18) Uani 1 1 d . . . . .
H33A H 0.333250 0.484429 0.192666 0.029 Uiso 1 1 calc R U . . .
H33B H 0.522166 0.525946 0.248066 0.029 Uiso 1 1 calc R U . . .
C34 C 0.4677(13) 0.5681(4) 0.1843(4) 0.0206(17) Uani 1 1 d . . . . .
H34A H 0.574921 0.540148 0.151444 0.025 Uiso 1 1 calc R U . . .
H34B H 0.543286 0.612347 0.215437 0.025 Uiso 1 1 calc R U . . .
C35 C 0.0181(14) 0.6759(4) 0.2059(4) 0.0200(16) Uani 1 1 d . . . . .
H35 H -0.087987 0.695196 0.239034 0.024 Uiso 1 1 calc R U . . .
C36 C 0.0775(15) 0.7123(4) 0.1658(4) 0.0218(17) Uani 1 1 d . . . . .
H36A H 0.175771 0.752761 0.193365 0.026 Uiso 1 1 calc R U . . .
H36B H -0.056907 0.728921 0.154745 0.026 Uiso 1 1 calc R U . . .
C37 C 0.1779(15) 0.5145(4) 0.0901(4) 0.0224(17) Uani 1 1 d . . . . .
H37A H 0.093804 0.489793 0.109300 0.034 Uiso 1 1 calc R U . . .
H37B H 0.294193 0.485948 0.063268 0.034 Uiso 1 1 calc R U . . .
H37C H 0.080859 0.525000 0.061802 0.034 Uiso 1 1 calc R U . . .
C38 C 0.2766(16) 0.6084(5) -0.0490(4) 0.0286(19) Uani 1 1 d . . . . .
H38A H 0.210149 0.577885 -0.033068 0.043 Uiso 1 1 calc R U . . .
H38B H 0.365476 0.581730 -0.087519 0.043 Uiso 1 1 calc R U . . .
H38C H 0.161422 0.629734 -0.062099 0.043 Uiso 1 1 calc R U . . .
C39 C 0.803(3) 0.3043(8) 1.0020(6) 0.060(4) Uani 1 1 d . . . . .
H39 H 0.958887 0.322250 1.008794 0.072 Uiso 1 1 calc R U . . .
C40 C 0.7045(17) 0.3332(5) 0.9597(5) 0.035(2) Uani 1 1 d . . . . .
C41 C 0.8306(19) 0.2938(6) 0.8981(5) 0.038(2) Uani 1 1 d . . . . .
H41 H 0.986170 0.310646 0.911659 0.046 Uiso 1 1 calc R U . . .
C42 C 0.822(3) 0.2198(7) 0.8878(7) 0.062(4) Uani 1 1 d . . . . .
H42A H 0.951095 0.195121 0.864259 0.075 Uiso 1 1 calc R U . . .
H42B H 0.687469 0.194011 0.862297 0.075 Uiso 1 1 calc R U . . .
C43 C 0.821(3) 0.2303(8) 0.9597(7) 0.066(4) Uani 1 1 d . . . . .
H43A H 0.694732 0.204576 0.965780 0.080 Uiso 1 1 calc R U . . .
H43B H 0.957152 0.214626 0.970762 0.080 Uiso 1 1 calc R U . . .
C44 C 0.7814(16) 0.3071(4) 0.8399(4) 0.0276(19) Uani 1 1 d . . . . .
H44 H 0.625661 0.292108 0.824727 0.033 Uiso 1 1 calc R U . . .
C45 C 0.8104(17) 0.3851(5) 0.8631(5) 0.031(2) Uani 1 1 d . . . . .
H45 H 0.970832 0.396312 0.872416 0.037 Uiso 1 1 calc R U . . .
C46 C 0.704(2) 0.4278(6) 0.9291(5) 0.042(2) Uani 1 1 d . . . . .
H46A H 0.748175 0.476625 0.944957 0.050 Uiso 1 1 calc R U . . .
H46B H 0.543206 0.422849 0.921391 0.050 Uiso 1 1 calc R U . . .
C47 C 0.759(2) 0.4093(6) 0.9828(5) 0.044(3) Uani 1 1 d . . . . .
H47A H 0.675456 0.437336 1.022839 0.053 Uiso 1 1 calc R U . . .
H47B H 0.916561 0.419528 0.994995 0.053 Uiso 1 1 calc R U . . .
C48 C 0.7517(18) 0.4031(5) 0.8071(5) 0.035(2) Uani 1 1 d . . . . .
C49 C 0.8502(16) 0.3538(5) 0.7425(5) 0.032(2) Uani 1 1 d . . . . .
C50 C 0.8486(18) 0.3737(5) 0.6868(5) 0.038(2) Uani 1 1 d . . . . .
H50A H 0.696237 0.370094 0.669961 0.045 Uiso 1 1 calc R U . . .
H50B H 0.934025 0.340827 0.649496 0.045 Uiso 1 1 calc R U . . .
C51 C 0.9453(19) 0.4476(5) 0.7095(5) 0.037(2) Uani 1 1 d . . . . .
H51 H 1.106045 0.450038 0.719157 0.045 Uiso 1 1 calc R U . . .
C52 C 0.831(2) 0.4963(6) 0.7715(6) 0.049(3) Uani 1 1 d . . . . .
H52A H 0.894472 0.543389 0.787231 0.058 Uiso 1 1 calc R U . . .
H52B H 0.674223 0.496189 0.760155 0.058 Uiso 1 1 calc R U . . .
C53 C 0.850(2) 0.4774(5) 0.8266(5) 0.043(3) Uani 1 1 d . . . . .
H53A H 0.774040 0.511151 0.865793 0.052 Uiso 1 1 calc R U . . .
H53B H 1.006506 0.480274 0.839694 0.052 Uiso 1 1 calc R U . . .
C54 C 0.928(2) 0.2936(5) 0.7314(5) 0.040(2) Uani 1 1 d . . . . .
H54 H 0.987596 0.265622 0.689219 0.047 Uiso 1 1 calc R U . . .
C55 C 0.9270(19) 0.2687(5) 0.7810(5) 0.036(2) Uani 1 1 d . . . . .
H55A H 1.078598 0.271968 0.798289 0.044 Uiso 1 1 calc R U . . .
H55B H 0.878175 0.219546 0.758596 0.044 Uiso 1 1 calc R U . . .
C56 C 0.5009(18) 0.4007(7) 0.7964(7) 0.047(3) Uani 1 1 d . . . . .
H56A H 0.467426 0.401385 0.754483 0.070 Uiso 1 1 calc R U . . .
H56B H 0.440082 0.440527 0.833494 0.070 Uiso 1 1 calc R U . . .
H56C H 0.436410 0.358486 0.794597 0.070 Uiso 1 1 calc R U . . .
C57 C 0.458(2) 0.3168(7) 0.9486(7) 0.052(3) Uani 1 1 d . . . . .
H57A H 0.405524 0.325441 0.912393 0.078 Uiso 1 1 calc R U . . .
H57B H 0.383536 0.345881 0.989538 0.078 Uiso 1 1 calc R U . . .
H57C H 0.427595 0.268430 0.936559 0.078 Uiso 1 1 calc R U . . .
C58 C 0.1845(19) 1.0068(6) 0.8630(5) 0.038(2) Uani 1 1 d . . . . .
C59 C 0.2158(14) 0.9379(5) 0.8044(4) 0.0241(18) Uani 1 1 d . . . . .
C60 C 0.1598(15) 0.8927(5) 0.8392(4) 0.0246(18) Uani 1 1 d . . . . .
H60 H 0.285625 0.900333 0.870776 0.030 Uiso 1 1 calc R U . . .
C61 C -0.0316(17) 0.9263(5) 0.8823(5) 0.030(2) Uani 1 1 d . . . . .
H61A H -0.033664 0.919062 0.922125 0.036 Uiso 1 1 calc R U . . .
H61B H -0.172372 0.908674 0.856916 0.036 Uiso 1 1 calc R U . . .
C62 C 0.0154(19) 1.0035(6) 0.9019(6) 0.040(2) Uani 1 1 d . . . . .
H62 H -0.058080 1.041317 0.934397 0.048 Uiso 1 1 calc R U . . .
C63 C 0.1470(15) 0.8170(5) 0.7915(4) 0.0240(18) Uani 1 1 d . . . . .
H63 H 0.028963 0.806555 0.756822 0.029 Uiso 1 1 calc R U . . .
C64 C 0.3702(14) 0.7964(5) 0.7576(4) 0.0250(18) Uani 1 1 d . . . . .
H64 H 0.476775 0.801475 0.793477 0.030 Uiso 1 1 calc R U . . .
C65 C 0.4592(15) 0.8447(5) 0.7309(4) 0.0262(18) Uani 1 1 d . . . . .
H65A H 0.614240 0.835105 0.719895 0.031 Uiso 1 1 calc R U . . .
H65B H 0.377653 0.833807 0.688943 0.031 Uiso 1 1 calc R U . . .
C66 C 0.4452(15) 0.9206(5) 0.7778(5) 0.029(2) Uani 1 1 d . . . . .
H66A H 0.485034 0.946951 0.753927 0.035 Uiso 1 1 calc R U . . .
H66B H 0.551288 0.934272 0.815577 0.035 Uiso 1 1 calc R U . . .
C67 C 0.3657(15) 0.7191(5) 0.7043(4) 0.0239(18) Uani 1 1 d . . . . .
C68 C 0.2557(17) 0.6756(5) 0.7321(5) 0.034(2) Uani 1 1 d . . . . .
C69 C 0.2843(18) 0.5983(5) 0.6921(6) 0.040(2) Uani 1 1 d . . . . .
H69A H 0.222993 0.575062 0.716869 0.048 Uiso 1 1 calc R U . . .
H69B H 0.202562 0.580064 0.648894 0.048 Uiso 1 1 calc R U . . .
C70 C 0.5236(19) 0.5828(5) 0.6797(6) 0.041(2) Uani 1 1 d . . . . .
H70 H 0.603470 0.597101 0.723224 0.049 Uiso 1 1 calc R U . . .
C71 C 0.6248(18) 0.6201(5) 0.6454(6) 0.039(2) Uani 1 1 d . . . . .
H71A H 0.550724 0.604392 0.601356 0.047 Uiso 1 1 calc R U . . .
H71B H 0.780958 0.609654 0.638147 0.047 Uiso 1 1 calc R U . . .
C72 C 0.6049(16) 0.6974(5) 0.6873(5) 0.032(2) Uani 1 1 d . . . . .
H72A H 0.668492 0.720656 0.662893 0.039 Uiso 1 1 calc R U . . .
H72B H 0.691759 0.713278 0.729416 0.039 Uiso 1 1 calc R U . . .
C73 C 0.1418(16) 0.7011(5) 0.7866(5) 0.033(2) Uani 1 1 d . . . . .
H73 H 0.081221 0.669888 0.800599 0.040 Uiso 1 1 calc R U . . .
C74 C 0.0995(17) 0.7765(5) 0.8288(5) 0.033(2) Uani 1 1 d . . . . .
H74A H -0.055016 0.781263 0.841865 0.039 Uiso 1 1 calc R U . . .
H74B H 0.192822 0.795561 0.869985 0.039 Uiso 1 1 calc R U . . .
C75 C 0.2376(19) 0.7069(6) 0.6400(5) 0.038(2) Uani 1 1 d . . . . .
H75A H 0.196389 0.657954 0.613602 0.056 Uiso 1 1 calc R U . . .
H75B H 0.329996 0.721686 0.613707 0.056 Uiso 1 1 calc R U . . .
H75C H 0.105546 0.733312 0.652112 0.056 Uiso 1 1 calc R U . . .
C76 C 0.0533(16) 0.9263(5) 0.7479(5) 0.033(2) Uani 1 1 d . . . . .
H76A H 0.070294 0.880732 0.710243 0.049 Uiso 1 1 calc R U . . .
H76B H 0.081798 0.961362 0.733645 0.049 Uiso 1 1 calc R U . . .
H76C H -0.096076 0.929499 0.763777 0.049 Uiso 1 1 calc R U . . .
C77 C 0.5639(16) 1.0884(5) 0.6202(5) 0.032(2) Uani 1 1 d . . . . .
C78 C 0.6014(14) 1.0188(4) 0.6151(4) 0.0190(16) Uani 1 1 d . . . . .
C79 C 0.7201(12) 0.9894(4) 0.5494(4) 0.0146(15) Uani 1 1 d . . . . .
H79 H 0.606504 0.981448 0.514240 0.018 Uiso 1 1 calc R U . . .
C79A C 0.7426(15) 1.0285(5) 0.6755(4) 0.0258(18) Uani 1 1 d . . . . .
H79A H 0.777744 0.983579 0.670845 0.039 Uiso 1 1 calc R U . . .
H79B H 0.661984 1.053528 0.716380 0.039 Uiso 1 1 calc R U . . .
H79C H 0.878107 1.054734 0.677941 0.039 Uiso 1 1 calc R U . . .
C80 C 0.8698(14) 1.0484(4) 0.5546(4) 0.0219(17) Uani 1 1 d . . . . .
H80A H 0.897533 1.044366 0.510097 0.026 Uiso 1 1 calc R U . . .
H80B H 1.011070 1.050443 0.577268 0.026 Uiso 1 1 calc R U . . .
C81 C 0.7362(16) 1.1115(4) 0.5968(4) 0.0251(18) Uani 1 1 d . . . . .
H81 H 0.767160 1.157260 0.604964 0.030 Uiso 1 1 calc R U . . .
C82 C 0.8097(12) 0.9191(4) 0.5308(4) 0.0152(15) Uani 1 1 d . . . . .
H82 H 0.917792 0.923396 0.566004 0.018 Uiso 1 1 calc R U . . .
C83 C 0.6197(13) 0.8688(4) 0.5250(4) 0.0157(15) Uani 1 1 d . . . . .
H83 H 0.527720 0.861198 0.485238 0.019 Uiso 1 1 calc R U . . .
C84 C 0.4681(15) 0.8981(4) 0.5857(4) 0.0238(18) Uani 1 1 d . . . . .
H84A H 0.334989 0.867539 0.574895 0.029 Uiso 1 1 calc R U . . .
H84B H 0.544688 0.897991 0.624294 0.029 Uiso 1 1 calc R U . . .
C85 C 0.3993(15) 0.9721(5) 0.6058(5) 0.0247(18) Uani 1 1 d . . . . .
H85A H 0.300444 0.971521 0.570746 0.030 Uiso 1 1 calc R U . . .
H85B H 0.319373 0.990022 0.647888 0.030 Uiso 1 1 calc R U . . .
C86 C 0.7016(13) 0.7973(4) 0.5105(4) 0.0170(16) Uani 1 1 d . . . . .
C87 C 0.8720(14) 0.7747(4) 0.4563(4) 0.0204(16) Uani 1 1 d . . . . .
C88 C 0.9338(14) 0.7002(4) 0.4273(4) 0.0211(16) Uani 1 1 d . . . . .
H88A H 1.026491 0.688978 0.388455 0.025 Uiso 1 1 calc R U . . .
H88B H 1.020800 0.694420 0.461211 0.025 Uiso 1 1 calc R U . . .
C89 C 0.7350(14) 0.6507(4) 0.4057(4) 0.0218(17) Uani 1 1 d . . . . .
H89 H 0.660342 0.651527 0.366699 0.026 Uiso 1 1 calc R U . . .
C90 C 0.5736(16) 0.6699(5) 0.4614(5) 0.0281(19) Uani 1 1 d . . . . .
H90A H 0.640076 0.664372 0.498403 0.034 Uiso 1 1 calc R U . . .
H90B H 0.440740 0.639111 0.444593 0.034 Uiso 1 1 calc R U . . .
C91 C 0.5122(14) 0.7440(5) 0.4867(5) 0.0227(18) Uani 1 1 d . . . . .
H91A H 0.430611 0.747230 0.450407 0.027 Uiso 1 1 calc R U . . .
H91B H 0.411724 0.755763 0.523912 0.027 Uiso 1 1 calc R U . . .
C92 C 0.9630(15) 0.8152(4) 0.4345(4) 0.0231(17) Uani 1 1 d . . . . .
H92 H 1.060401 0.795779 0.398838 0.028 Uiso 1 1 calc R U . . .
C93 C 0.9217(15) 0.8908(4) 0.4630(4) 0.0237(18) Uani 1 1 d . . . . .
H93A H 0.828016 0.897803 0.431104 0.028 Uiso 1 1 calc R U . . .
H93B H 1.062547 0.916738 0.468793 0.028 Uiso 1 1 calc R U . . .
C94 C 0.8144(16) 0.8002(5) 0.5739(4) 0.0259(19) Uani 1 1 d . . . . .
H94A H 0.895063 0.758642 0.561241 0.039 Uiso 1 1 calc R U . . .
H94B H 0.702921 0.803366 0.605726 0.039 Uiso 1 1 calc R U . . .
H94C H 0.915790 0.840580 0.594607 0.039 Uiso 1 1 calc R U . . .
C95 C 0.7177(16) -0.0105(5) 0.0558(4) 0.0281(19) Uani 1 1 d . . . . .
H95 H 0.825119 0.007998 0.034707 0.034 Uiso 1 1 calc R U . . .
C96 C 0.6699(13) 0.0510(4) 0.1221(4) 0.0157(15) Uani 1 1 d . . . . .
C96A C 0.8664(14) 0.0959(4) 0.1623(4) 0.0218(17) Uani 1 1 d . . . . .
H96A H 0.963513 0.105264 0.132699 0.026 Uiso 1 1 calc R U . . .
H96B H 0.950053 0.071349 0.181478 0.026 Uiso 1 1 calc R U . . .
C97 C 0.5411(14) 0.0911(4) 0.0942(4) 0.0198(16) Uani 1 1 d . . . . .
H97 H 0.649232 0.105721 0.070083 0.024 Uiso 1 1 calc R U . . .
C98 C 0.3872(16) 0.0375(5) 0.0406(5) 0.030(2) Uani 1 1 d . . . . .
H98A H 0.352997 0.050559 0.005433 0.036 Uiso 1 1 calc R U . . .
H98B H 0.249067 0.031497 0.059887 0.036 Uiso 1 1 calc R U . . .
C99 C 0.5167(16) -0.0293(5) 0.0120(4) 0.030(2) Uani 1 1 d . . . . .
H99A H 0.430073 -0.067083 0.013896 0.036 Uiso 1 1 calc R U . . .
H99B H 0.554695 -0.043775 -0.034820 0.036 Uiso 1 1 calc R U . . .
C100 C 0.4517(14) 0.1574(4) 0.1483(4) 0.0200(16) Uani 1 1 d . . . . .
H100 H 0.346019 0.145352 0.174925 0.024 Uiso 1 1 calc R U . . .
C101 C 0.6409(13) 0.2036(4) 0.1954(4) 0.0178(16) Uani 1 1 d . . . . .
H101 H 0.732074 0.219214 0.168386 0.021 Uiso 1 1 calc R U . . .
C102 C 0.5627(14) 0.2700(4) 0.2555(4) 0.0189(16) Uani 1 1 d . . . . .
C103 C 0.3877(14) 0.3015(4) 0.2294(4) 0.0205(17) Uani 1 1 d . . . . .
C104 C 0.3329(14) 0.3742(4) 0.2776(4) 0.0233(17) Uani 1 1 d . . . . .
H10A H 0.235335 0.391861 0.254682 0.028 Uiso 1 1 calc R U . . .
H10B H 0.253880 0.374209 0.315354 0.028 Uiso 1 1 calc R U . . .
C105 C 0.5356(15) 0.4206(5) 0.3037(5) 0.0255(19) Uani 1 1 d . . . . .
H105 H 0.606402 0.424587 0.266145 0.031 Uiso 1 1 calc R U . . .
C106 C 0.6962(15) 0.3940(4) 0.3357(5) 0.0261(18) Uani 1 1 d . . . . .
H10C H 0.630993 0.392926 0.374905 0.031 Uiso 1 1 calc R U . . .
H10D H 0.829581 0.424713 0.351018 0.031 Uiso 1 1 calc R U . . .
C107 C 0.7559(14) 0.3210(4) 0.2845(5) 0.0237(18) Uani 1 1 d . . . . .
H10E H 0.832559 0.323673 0.247551 0.028 Uiso 1 1 calc R U . . .
H10F H 0.859168 0.303580 0.306231 0.028 Uiso 1 1 calc R U . . .
C108 C 0.2921(15) 0.2689(5) 0.1691(5) 0.0260(19) Uani 1 1 d . . . . .
H108 H 0.190560 0.293292 0.157347 0.031 Uiso 1 1 calc R U . . .
C109 C 0.3320(15) 0.1958(4) 0.1173(4) 0.0248(18) Uani 1 1 d . . . . .
H10G H 0.420218 0.196571 0.081389 0.030 Uiso 1 1 calc R U . . .
H10H H 0.190227 0.171263 0.097175 0.030 Uiso 1 1 calc R U . . .
C110 C 0.4568(16) 0.2549(5) 0.3080(4) 0.0246(18) Uani 1 1 d . . . . .
H11A H 0.378682 0.294904 0.338912 0.037 Uiso 1 1 calc R U . . .
H11B H 0.570046 0.244985 0.332615 0.037 Uiso 1 1 calc R U . . .
H11C H 0.353496 0.215182 0.286064 0.037 Uiso 1 1 calc R U . . .
C111 C 0.7941(15) 0.1638(4) 0.2187(5) 0.0257(18) Uani 1 1 d . . . . .
H11D H 0.925803 0.193563 0.241217 0.031 Uiso 1 1 calc R U . . .
H11E H 0.717826 0.154334 0.251888 0.031 Uiso 1 1 calc R U . . .
C112 C 0.5290(16) 0.0277(5) 0.1639(4) 0.0266(19) Uani 1 1 d . . . . .
H11G H 0.482506 0.068042 0.203630 0.040 Uiso 1 1 calc R U . . .
H11H H 0.614429 -0.000580 0.177484 0.040 Uiso 1 1 calc R U . . .
H11I H 0.399911 0.000838 0.137312 0.040 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C1 2.146(8) . ?
I2 C20 2.143(9) . ?
I3 C39 2.121(12) . ?
I4 C58 2.041(11) . ?
I5 C77 2.140(9) . ?
I6 C95 2.147(9) . ?
O1 C13 1.452(11) . ?
O1 H1OA 0.8400 . ?
O2 C32 1.429(10) . ?
O2 H20A 0.8449 . ?
O3 C51 1.418(13) . ?
O3 H3OA 0.8400 . ?
O4 C70 1.461(13) . ?
O4 H4OA 0.8400 . ?
O5 C89 1.444(10) . ?
O5 H5OA 0.8400 . ?
O6 C105 1.463(11) . ?
O6 H6OA 0.8400 . ?
C1 C5 1.480(12) . ?
C1 C2 1.543(12) . ?
C1 H1 1.0000 . ?
C2 C9 1.501(12) . ?
C2 C3 1.540(10) . ?
C2 C19 1.543(10) . ?
C3 C6 1.519(11) . ?
C3 C4 1.535(11) . ?
C3 H3 1.0000 . ?
C4 C5 1.568(12) . ?
C4 H4A 0.9900 . ?
C4 H4AB 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5AB 0.9900 . ?
C6 C7 1.533(11) . ?
C6 C17 1.545(10) . ?
C6 H6 1.0000 . ?
C7 C8 1.544(10) . ?
C7 C10 1.558(12) . ?
C7 H7 1.0000 . ?
C8 C9 1.548(12) . ?
C8 H8A 0.9900 . ?
C8 H8AB 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9AB 0.9900 . ?
C10 C11 1.519(11) . ?
C10 C18 1.542(11) . ?
C10 C15 1.549(12) . ?
C11 C16 1.318(12) . ?
C11 C12 1.523(12) . ?
C12 C13 1.505(13) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.517(13) . ?
C13 H13 1.0000 . ?
C14 C15 1.558(13) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.499(11) . ?
C16 H16 0.9500 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C24 1.504(12) . ?
C20 C21 1.526(11) . ?
C20 H20 1.0000 . ?
C21 C28 1.515(11) . ?
C21 C38 1.544(12) . ?
C21 C22 1.547(10) . ?
C22 C23 1.528(10) . ?
C22 C25 1.534(10) . ?
C22 H22 1.0000 . ?
C23 C24 1.548(11) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C36 1.528(11) . ?
C25 C26 1.556(10) . ?
C25 H25 1.0000 . ?
C26 C27 1.552(12) . ?
C26 C29 1.565(10) . ?
C26 H26 1.0000 . ?
C27 C28 1.523(11) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.531(11) . ?
C29 C34 1.542(11) . ?
C29 C37 1.554(12) . ?
C30 C35 1.318(12) . ?
C30 C31 1.516(10) . ?
C31 C32 1.514(11) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.515(12) . ?
C32 H32 1.0000 . ?
C33 C34 1.533(10) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.509(11) . ?
C35 H35 0.9500 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C43 1.47(2) . ?
C39 C40 1.511(17) . ?
C39 H39 1.0000 . ?
C40 C41 1.499(14) . ?
C40 C47 1.528(15) . ?
C40 C57 1.529(16) . ?
C41 C44 1.512(14) . ?
C41 C42 1.538(17) . ?
C41 H41 1.0000 . ?
C42 C43 1.539(19) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C55 1.525(13) . ?
C44 C45 1.549(12) . ?
C44 H44 1.0000 . ?
C45 C46 1.518(13) . ?
C45 C48 1.543(14) . ?
C45 H45 1.0000 . ?
C46 C47 1.494(16) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.509(13) . ?
C48 C56 1.547(15) . ?
C48 C53 1.578(15) . ?
C49 C54 1.339(15) . ?
C49 C50 1.521(14) . ?
C50 C51 1.555(15) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.514(15) . ?
C51 H51 1.0000 . ?
C52 C53 1.497(16) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.468(15) . ?
C54 H54 0.9500 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C62 1.391(15) . ?
C58 C59 1.502(14) . ?
C59 C66 1.527(13) . ?
C59 C76 1.532(12) . ?
C59 C60 1.567(11) . ?
C60 C63 1.506(13) . ?
C60 C61 1.514(13) . ?
C60 H60 1.0000 . ?
C61 C62 1.562(14) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62 0.9500 . ?
C63 C74 1.515(11) . ?
C63 C64 1.552(12) . ?
C63 H63 1.0000 . ?
C64 C65 1.540(11) . ?
C64 C67 1.563(13) . ?
C64 H64 1.0000 . ?
C65 C66 1.513(14) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 C68 1.519(12) . ?
C67 C75 1.552(12) . ?
C67 C72 1.554(13) . ?
C68 C73 1.316(15) . ?
C68 C69 1.531(15) . ?
C69 C70 1.517(16) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 C71 1.498(16) . ?
C70 H70 1.0000 . ?
C71 C72 1.526(14) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 C74 1.517(15) . ?
C73 H73 0.9500 . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 C81 1.371(14) . ?
C77 C78 1.513(11) . ?
C78 C79 1.526(11) . ?
C78 C85 1.527(12) . ?
C78 C79A 1.536(11) . ?
C79 C80 1.521(11) . ?
C79 C82 1.531(11) . ?
C79 H79 1.0000 . ?
C79A H79A 0.9800 . ?
C79A H79B 0.9800 . ?
C79A H79C 0.9800 . ?
C80 C81 1.543(12) . ?
C80 H80A 0.9900 . ?
C80 H80B 0.9900 . ?
C81 H81 0.9500 . ?
C82 C83 1.540(10) . ?
C82 C93 1.544(11) . ?
C82 H82 1.0000 . ?
C83 C84 1.556(11) . ?
C83 C86 1.558(11) . ?
C83 H83 1.0000 . ?
C84 C85 1.554(12) . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C85 H85A 0.9900 . ?
C85 H85B 0.9900 . ?
C86 C91 1.521(12) . ?
C86 C87 1.533(10) . ?
C86 C94 1.562(11) . ?
C87 C92 1.317(12) . ?
C87 C88 1.522(11) . ?
C88 C89 1.518(12) . ?
C88 H88A 0.9900 . ?
C88 H88B 0.9900 . ?
C89 C90 1.521(12) . ?
C89 H89 1.0000 . ?
C90 C91 1.522(12) . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 C93 1.515(12) . ?
C92 H92 0.9500 . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?
C95 C99 1.491(12) . ?
C95 C96 1.524(11) . ?
C95 H95 1.0000 . ?
C96 C96A 1.517(11) . ?
C96 C112 1.535(11) . ?
C96 C97 1.540(10) . ?
C96A C111 1.534(12) . ?
C96A H96A 0.9900 . ?
C96A H96B 0.9900 . ?
C97 C98 1.522(12) . ?
C97 C100 1.531(12) . ?
C97 H97 1.0000 . ?
C98 C99 1.558(13) . ?
C98 H98A 0.9900 . ?
C98 H98B 0.9900 . ?
C99 H99A 0.9900 . ?
C99 H99B 0.9900 . ?
C100 C109 1.532(10) . ?
C100 C101 1.546(11) . ?
C100 H100 1.0000 . ?
C101 C111 1.553(10) . ?
C101 C102 1.561(12) . ?
C101 H101 1.0000 . ?
C102 C107 1.513(12) . ?
C102 C110 1.526(11) . ?
C102 C103 1.551(11) . ?
C103 C108 1.329(13) . ?
C103 C104 1.513(12) . ?
C104 C105 1.504(12) . ?
C104 H10A 0.9900 . ?
C104 H10B 0.9900 . ?
C105 C106 1.505(11) . ?
C105 H105 1.0000 . ?
C106 C107 1.544(12) . ?
C106 H10C 0.9900 . ?
C106 H10D 0.9900 . ?
C107 H10E 0.9900 . ?
C107 H10F 0.9900 . ?
C108 C109 1.519(13) . ?
C108 H108 0.9500 . ?
C109 H10G 0.9900 . ?
C109 H10H 0.9900 . ?
C110 H11A 0.9800 . ?
C110 H11B 0.9800 . ?
C110 H11C 0.9800 . ?
C111 H11D 0.9900 . ?
C111 H11E 0.9900 . ?
C112 H11G 0.9800 . ?
C112 H11H 0.9800 . ?
C112 H11I 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 O1 H1OA 109.5 . . ?
C32 O2 H20A 125.9 . . ?
C51 O3 H3OA 109.5 . . ?
C70 O4 H4OA 109.5 . . ?
C89 O5 H5OA 109.5 . . ?
C105 O6 H6OA 109.5 . . ?
C5 C1 C2 108.6(7) . . ?
C5 C1 I1 116.5(6) . . ?
C2 C1 I1 117.6(5) . . ?
C5 C1 H1 104.1 . . ?
C2 C1 H1 104.1 . . ?
I1 C1 H1 104.1 . . ?
C9 C2 C3 108.4(6) . . ?
C9 C2 C19 112.6(7) . . ?
C3 C2 C19 113.0(7) . . ?
C9 C2 C1 116.1(7) . . ?
C3 C2 C1 96.9(6) . . ?
C19 C2 C1 109.0(7) . . ?
C6 C3 C4 120.3(7) . . ?
C6 C3 C2 113.8(6) . . ?
C4 C3 C2 106.3(6) . . ?
C6 C3 H3 105.0 . . ?
C4 C3 H3 105.0 . . ?
C2 C3 H3 105.0 . . ?
C3 C4 C5 102.6(7) . . ?
C3 C4 H4A 111.2 . . ?
C5 C4 H4A 111.2 . . ?
C3 C4 H4AB 111.2 . . ?
C5 C4 H4AB 111.2 . . ?
H4A C4 H4AB 109.2 . . ?
C1 C5 C4 105.5(7) . . ?
C1 C5 H5A 110.6 . . ?
C4 C5 H5A 110.6 . . ?
C1 C5 H5AB 110.6 . . ?
C4 C5 H5AB 110.6 . . ?
H5A C5 H5AB 108.8 . . ?
C3 C6 C7 109.7(6) . . ?
C3 C6 C17 110.1(6) . . ?
C7 C6 C17 110.7(6) . . ?
C3 C6 H6 108.8 . . ?
C7 C6 H6 108.8 . . ?
C17 C6 H6 108.8 . . ?
C6 C7 C8 111.8(6) . . ?
C6 C7 C10 112.2(6) . . ?
C8 C7 C10 113.7(6) . . ?
C6 C7 H7 106.2 . . ?
C8 C7 H7 106.2 . . ?
C10 C7 H7 106.2 . . ?
C7 C8 C9 113.8(7) . . ?
C7 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
C7 C8 H8AB 108.8 . . ?
C9 C8 H8AB 108.8 . . ?
H8A C8 H8AB 107.7 . . ?
C2 C9 C8 110.5(7) . . ?
C2 C9 H9A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C2 C9 H9AB 109.5 . . ?
C8 C9 H9AB 109.5 . . ?
H9A C9 H9AB 108.1 . . ?
C11 C10 C18 109.2(7) . . ?
C11 C10 C15 109.2(7) . . ?
C18 C10 C15 109.8(7) . . ?
C11 C10 C7 110.5(6) . . ?
C18 C10 C7 111.3(7) . . ?
C15 C10 C7 106.7(7) . . ?
C16 C11 C10 123.6(8) . . ?
C16 C11 C12 120.1(8) . . ?
C10 C11 C12 116.3(7) . . ?
C13 C12 C11 112.2(8) . . ?
C13 C12 H12A 109.2 . . ?
C11 C12 H12A 109.2 . . ?
C13 C12 H12B 109.2 . . ?
C11 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
O1 C13 C12 107.2(8) . . ?
O1 C13 C14 111.0(7) . . ?
C12 C13 C14 110.1(8) . . ?
O1 C13 H13 109.5 . . ?
C12 C13 H13 109.5 . . ?
C14 C13 H13 109.5 . . ?
C13 C14 C15 110.3(7) . . ?
C13 C14 H14A 109.6 . . ?
C15 C14 H14A 109.6 . . ?
C13 C14 H14B 109.6 . . ?
C15 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
C10 C15 C14 112.4(7) . . ?
C10 C15 H15A 109.1 . . ?
C14 C15 H15A 109.1 . . ?
C10 C15 H15B 109.1 . . ?
C14 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
C11 C16 C17 125.3(7) . . ?
C11 C16 H16 117.3 . . ?
C17 C16 H16 117.3 . . ?
C16 C17 C6 112.2(7) . . ?
C16 C17 H17A 109.2 . . ?
C6 C17 H17A 109.2 . . ?
C16 C17 H17B 109.2 . . ?
C6 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C10 C18 H18A 109.5 . . ?
C10 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C10 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C2 C19 H19A 109.5 . . ?
C2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C24 C20 C21 108.1(8) . . ?
C24 C20 I2 115.3(6) . . ?
C21 C20 I2 117.1(6) . . ?
C24 C20 H20 105.0 . . ?
C21 C20 H20 105.0 . . ?
I2 C20 H20 105.0 . . ?
C28 C21 C20 115.9(7) . . ?
C28 C21 C38 112.4(7) . . ?
C20 C21 C38 110.5(7) . . ?
C28 C21 C22 108.0(6) . . ?
C20 C21 C22 96.9(6) . . ?
C38 C21 C22 112.0(7) . . ?
C23 C22 C25 119.6(7) . . ?
C23 C22 C21 104.3(6) . . ?
C25 C22 C21 113.2(6) . . ?
C23 C22 H22 106.3 . . ?
C25 C22 H22 106.3 . . ?
C21 C22 H22 106.3 . . ?
C22 C23 C24 104.3(7) . . ?
C22 C23 H23A 110.9 . . ?
C24 C23 H23A 110.9 . . ?
C22 C23 H23B 110.9 . . ?
C24 C23 H23B 110.9 . . ?
H23A C23 H23B 108.9 . . ?
C20 C24 C23 104.2(7) . . ?
C20 C24 H24A 110.9 . . ?
C23 C24 H24A 110.9 . . ?
C20 C24 H24B 110.9 . . ?
C23 C24 H24B 110.9 . . ?
H24A C24 H24B 108.9 . . ?
C36 C25 C22 111.1(6) . . ?
C36 C25 C26 107.7(6) . . ?
C22 C25 C26 108.7(6) . . ?
C36 C25 H25 109.8 . . ?
C22 C25 H25 109.8 . . ?
C26 C25 H25 109.8 . . ?
C27 C26 C25 112.3(6) . . ?
C27 C26 C29 112.0(6) . . ?
C25 C26 C29 111.6(7) . . ?
C27 C26 H26 106.8 . . ?
C25 C26 H26 106.8 . . ?
C29 C26 H26 106.8 . . ?
C28 C27 C26 114.2(7) . . ?
C28 C27 H27A 108.7 . . ?
C26 C27 H27A 108.7 . . ?
C28 C27 H27B 108.7 . . ?
C26 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
C21 C28 C27 110.8(7) . . ?
C21 C28 H28A 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C21 C28 H28B 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 108.1 . . ?
C30 C29 C34 107.7(6) . . ?
C30 C29 C37 108.8(7) . . ?
C34 C29 C37 111.1(7) . . ?
C30 C29 C26 109.9(6) . . ?
C34 C29 C26 108.3(7) . . ?
C37 C29 C26 111.1(6) . . ?
C35 C30 C31 120.9(7) . . ?
C35 C30 C29 124.1(7) . . ?
C31 C30 C29 115.0(7) . . ?
C32 C31 C30 112.0(7) . . ?
C32 C31 H31A 109.2 . . ?
C30 C31 H31A 109.2 . . ?
C32 C31 H31B 109.2 . . ?
C30 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
O2 C32 C31 111.0(7) . . ?
O2 C32 C33 108.8(6) . . ?
C31 C32 C33 111.1(7) . . ?
O2 C32 H32 108.6 . . ?
C31 C32 H32 108.6 . . ?
C33 C32 H32 108.6 . . ?
C32 C33 C34 110.3(7) . . ?
C32 C33 H33A 109.6 . . ?
C34 C33 H33A 109.6 . . ?
C32 C33 H33B 109.6 . . ?
C34 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
C33 C34 C29 114.5(7) . . ?
C33 C34 H34A 108.6 . . ?
C29 C34 H34A 108.6 . . ?
C33 C34 H34B 108.6 . . ?
C29 C34 H34B 108.6 . . ?
H34A C34 H34B 107.6 . . ?
C30 C35 C36 123.7(7) . . ?
C30 C35 H35 118.1 . . ?
C36 C35 H35 118.1 . . ?
C35 C36 C25 112.6(7) . . ?
C35 C36 H36A 109.1 . . ?
C25 C36 H36A 109.1 . . ?
C35 C36 H36B 109.1 . . ?
C25 C36 H36B 109.1 . . ?
H36A C36 H36B 107.8 . . ?
C29 C37 H37A 109.5 . . ?
C29 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C29 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C21 C38 H38A 109.5 . . ?
C21 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C21 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C43 C39 C40 107.8(11) . . ?
C43 C39 I3 118.6(9) . . ?
C40 C39 I3 118.6(9) . . ?
C43 C39 H39 103.1 . . ?
C40 C39 H39 103.1 . . ?
I3 C39 H39 103.1 . . ?
C41 C40 C39 97.8(9) . . ?
C41 C40 C47 106.8(9) . . ?
C39 C40 C47 115.8(10) . . ?
C41 C40 C57 113.0(10) . . ?
C39 C40 C57 111.5(11) . . ?
C47 C40 C57 111.3(10) . . ?
C40 C41 C44 116.3(9) . . ?
C40 C41 C42 104.8(9) . . ?
C44 C41 C42 119.6(10) . . ?
C40 C41 H41 104.9 . . ?
C44 C41 H41 104.9 . . ?
C42 C41 H41 104.9 . . ?
C41 C42 C43 102.5(11) . . ?
C41 C42 H42A 111.3 . . ?
C43 C42 H42A 111.3 . . ?
C41 C42 H42B 111.3 . . ?
C43 C42 H42B 111.3 . . ?
H42A C42 H42B 109.2 . . ?
C39 C43 C42 105.4(11) . . ?
C39 C43 H43A 110.7 . . ?
C42 C43 H43A 110.7 . . ?
C39 C43 H43B 110.7 . . ?
C42 C43 H43B 110.7 . . ?
H43A C43 H43B 108.8 . . ?
C41 C44 C55 112.9(8) . . ?
C41 C44 C45 109.1(8) . . ?
C55 C44 C45 109.2(8) . . ?
C41 C44 H44 108.5 . . ?
C55 C44 H44 108.5 . . ?
C45 C44 H44 108.5 . . ?
C46 C45 C48 115.1(8) . . ?
C46 C45 C44 112.4(8) . . ?
C48 C45 C44 112.2(8) . . ?
C46 C45 H45 105.4 . . ?
C48 C45 H45 105.4 . . ?
C44 C45 H45 105.4 . . ?
C47 C46 C45 114.8(9) . . ?
C47 C46 H46A 108.6 . . ?
C45 C46 H46A 108.6 . . ?
C47 C46 H46B 108.6 . . ?
C45 C46 H46B 108.6 . . ?
H46A C46 H46B 107.5 . . ?
C46 C47 C40 110.9(9) . . ?
C46 C47 H47A 109.5 . . ?
C40 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C40 C47 H47B 109.5 . . ?
H47A C47 H47B 108.0 . . ?
C49 C48 C45 110.6(8) . . ?
C49 C48 C56 109.0(9) . . ?
C45 C48 C56 110.8(9) . . ?
C49 C48 C53 107.7(8) . . ?
C45 C48 C53 109.0(8) . . ?
C56 C48 C53 109.7(9) . . ?
C54 C49 C48 123.8(9) . . ?
C54 C49 C50 119.6(9) . . ?
C48 C49 C50 116.6(9) . . ?
C49 C50 C51 112.9(9) . . ?
C49 C50 H50A 109.0 . . ?
C51 C50 H50A 109.0 . . ?
C49 C50 H50B 109.0 . . ?
C51 C50 H50B 109.0 . . ?
H50A C50 H50B 107.8 . . ?
O3 C51 C52 109.4(9) . . ?
O3 C51 C50 108.7(9) . . ?
C52 C51 C50 108.4(9) . . ?
O3 C51 H51 110.1 . . ?
C52 C51 H51 110.1 . . ?
C50 C51 H51 110.1 . . ?
C53 C52 C51 112.6(9) . . ?
C53 C52 H52A 109.1 . . ?
C51 C52 H52A 109.1 . . ?
C53 C52 H52B 109.1 . . ?
C51 C52 H52B 109.1 . . ?
H52A C52 H52B 107.8 . . ?
C52 C53 C48 113.4(9) . . ?
C52 C53 H53A 108.9 . . ?
C48 C53 H53A 108.9 . . ?
C52 C53 H53B 108.9 . . ?
C48 C53 H53B 108.9 . . ?
H53A C53 H53B 107.7 . . ?
C49 C54 C55 123.4(9) . . ?
C49 C54 H54 118.3 . . ?
C55 C54 H54 118.3 . . ?
C54 C55 C44 114.7(9) . . ?
C54 C55 H55A 108.6 . . ?
C44 C55 H55A 108.6 . . ?
C54 C55 H55B 108.6 . . ?
C44 C55 H55B 108.6 . . ?
H55A C55 H55B 107.6 . . ?
C48 C56 H56A 109.5 . . ?
C48 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C48 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C40 C57 H57A 109.5 . . ?
C40 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C40 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C62 C58 C59 111.2(9) . . ?
C62 C58 I4 124.6(8) . . ?
C59 C58 I4 120.3(7) . . ?
C58 C59 C66 118.5(8) . . ?
C58 C59 C76 109.4(8) . . ?
C66 C59 C76 110.3(7) . . ?
C58 C59 C60 98.0(7) . . ?
C66 C59 C60 106.8(7) . . ?
C76 C59 C60 113.5(7) . . ?
C63 C60 C61 120.4(8) . . ?
C63 C60 C59 113.0(7) . . ?
C61 C60 C59 104.6(7) . . ?
C63 C60 H60 106.0 . . ?
C61 C60 H60 106.0 . . ?
C59 C60 H60 106.0 . . ?
C60 C61 C62 102.2(8) . . ?
C60 C61 H61A 111.3 . . ?
C62 C61 H61A 111.3 . . ?
C60 C61 H61B 111.3 . . ?
C62 C61 H61B 111.3 . . ?
H61A C61 H61B 109.2 . . ?
C58 C62 C61 107.4(9) . . ?
C58 C62 H62 126.3 . . ?
C61 C62 H62 126.3 . . ?
C60 C63 C74 110.1(7) . . ?
C60 C63 C64 108.8(7) . . ?
C74 C63 C64 108.9(7) . . ?
C60 C63 H63 109.7 . . ?
C74 C63 H63 109.7 . . ?
C64 C63 H63 109.7 . . ?
C65 C64 C63 113.5(7) . . ?
C65 C64 C67 113.0(7) . . ?
C63 C64 C67 111.8(7) . . ?
C65 C64 H64 105.9 . . ?
C63 C64 H64 105.9 . . ?
C67 C64 H64 105.9 . . ?
C66 C65 C64 115.4(8) . . ?
C66 C65 H65A 108.4 . . ?
C64 C65 H65A 108.4 . . ?
C66 C65 H65B 108.4 . . ?
C64 C65 H65B 108.4 . . ?
H65A C65 H65B 107.5 . . ?
C65 C66 C59 111.5(8) . . ?
C65 C66 H66A 109.3 . . ?
C59 C66 H66A 109.3 . . ?
C65 C66 H66B 109.3 . . ?
C59 C66 H66B 109.3 . . ?
H66A C66 H66B 108.0 . . ?
C68 C67 C75 108.6(8) . . ?
C68 C67 C72 109.2(8) . . ?
C75 C67 C72 109.7(8) . . ?
C68 C67 C64 109.7(7) . . ?
C75 C67 C64 111.0(8) . . ?
C72 C67 C64 108.7(7) . . ?
C73 C68 C67 123.5(9) . . ?
C73 C68 C69 121.0(9) . . ?
C67 C68 C69 115.4(9) . . ?
C70 C69 C68 111.1(9) . . ?
C70 C69 H69A 109.4 . . ?
C68 C69 H69A 109.4 . . ?
C70 C69 H69B 109.4 . . ?
C68 C69 H69B 109.4 . . ?
H69A C69 H69B 108.0 . . ?
O4 C70 C71 110.8(10) . . ?
O4 C70 C69 106.8(9) . . ?
C71 C70 C69 110.9(9) . . ?
O4 C70 H70 109.4 . . ?
C71 C70 H70 109.4 . . ?
C69 C70 H70 109.4 . . ?
C70 C71 C72 110.5(9) . . ?
C70 C71 H71A 109.6 . . ?
C72 C71 H71A 109.6 . . ?
C70 C71 H71B 109.6 . . ?
C72 C71 H71B 109.6 . . ?
H71A C71 H71B 108.1 . . ?
C71 C72 C67 113.7(8) . . ?
C71 C72 H72A 108.8 . . ?
C67 C72 H72A 108.8 . . ?
C71 C72 H72B 108.8 . . ?
C67 C72 H72B 108.8 . . ?
H72A C72 H72B 107.7 . . ?
C68 C73 C74 125.1(9) . . ?
C68 C73 H73 117.5 . . ?
C74 C73 H73 117.5 . . ?
C63 C74 C73 111.6(8) . . ?
C63 C74 H74A 109.3 . . ?
C73 C74 H74A 109.3 . . ?
C63 C74 H74B 109.3 . . ?
C73 C74 H74B 109.3 . . ?
H74A C74 H74B 108.0 . . ?
C67 C75 H75A 109.5 . . ?
C67 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C67 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C59 C76 H76A 109.5 . . ?
C59 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C59 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C81 C77 C78 111.9(8) . . ?
C81 C77 I5 121.8(7) . . ?
C78 C77 I5 119.2(6) . . ?
C77 C78 C79 96.9(6) . . ?
C77 C78 C85 117.1(7) . . ?
C79 C78 C85 108.1(7) . . ?
C77 C78 C79A 108.9(7) . . ?
C79 C78 C79A 114.5(7) . . ?
C85 C78 C79A 110.8(7) . . ?
C80 C79 C78 104.8(6) . . ?
C80 C79 C82 120.8(7) . . ?
C78 C79 C82 112.5(6) . . ?
C80 C79 H79 105.9 . . ?
C78 C79 H79 105.9 . . ?
C82 C79 H79 105.9 . . ?
C78 C79A H79A 109.5 . . ?
C78 C79A H79B 109.5 . . ?
H79A C79A H79B 109.5 . . ?
C78 C79A H79C 109.5 . . ?
H79A C79A H79C 109.5 . . ?
H79B C79A H79C 109.5 . . ?
C79 C80 C81 102.2(7) . . ?
C79 C80 H80A 111.3 . . ?
C81 C80 H80A 111.3 . . ?
C79 C80 H80B 111.3 . . ?
C81 C80 H80B 111.3 . . ?
H80A C80 H80B 109.2 . . ?
C77 C81 C80 106.5(7) . . ?
C77 C81 H81 126.7 . . ?
C80 C81 H81 126.7 . . ?
C79 C82 C83 109.3(6) . . ?
C79 C82 C93 110.4(6) . . ?
C83 C82 C93 108.6(6) . . ?
C79 C82 H82 109.5 . . ?
C83 C82 H82 109.5 . . ?
C93 C82 H82 109.5 . . ?
C82 C83 C84 113.2(6) . . ?
C82 C83 C86 111.9(6) . . ?
C84 C83 C86 111.8(6) . . ?
C82 C83 H83 106.5 . . ?
C84 C83 H83 106.5 . . ?
C86 C83 H83 106.5 . . ?
C85 C84 C83 113.5(7) . . ?
C85 C84 H84A 108.9 . . ?
C83 C84 H84A 108.9 . . ?
C85 C84 H84B 108.9 . . ?
C83 C84 H84B 108.9 . . ?
H84A C84 H84B 107.7 . . ?
C78 C85 C84 110.0(7) . . ?
C78 C85 H85A 109.7 . . ?
C84 C85 H85A 109.7 . . ?
C78 C85 H85B 109.7 . . ?
C84 C85 H85B 109.7 . . ?
H85A C85 H85B 108.2 . . ?
C91 C86 C87 108.7(7) . . ?
C91 C86 C83 110.4(7) . . ?
C87 C86 C83 109.9(6) . . ?
C91 C86 C94 109.5(7) . . ?
C87 C86 C94 107.2(7) . . ?
C83 C86 C94 111.1(7) . . ?
C92 C87 C88 120.3(8) . . ?
C92 C87 C86 124.1(8) . . ?
C88 C87 C86 115.6(7) . . ?
C89 C88 C87 112.4(7) . . ?
C89 C88 H88A 109.1 . . ?
C87 C88 H88A 109.1 . . ?
C89 C88 H88B 109.1 . . ?
C87 C88 H88B 109.1 . . ?
H88A C88 H88B 107.9 . . ?
O5 C89 C88 107.6(7) . . ?
O5 C89 C90 111.1(7) . . ?
C88 C89 C90 111.7(7) . . ?
O5 C89 H89 108.8 . . ?
C88 C89 H89 108.8 . . ?
C90 C89 H89 108.8 . . ?
C89 C90 C91 109.9(7) . . ?
C89 C90 H90A 109.7 . . ?
C91 C90 H90A 109.7 . . ?
C89 C90 H90B 109.7 . . ?
C91 C90 H90B 109.7 . . ?
H90A C90 H90B 108.2 . . ?
C86 C91 C90 115.8(7) . . ?
C86 C91 H91A 108.3 . . ?
C90 C91 H91A 108.3 . . ?
C86 C91 H91B 108.3 . . ?
C90 C91 H91B 108.3 . . ?
H91A C91 H91B 107.4 . . ?
C87 C92 C93 124.0(8) . . ?
C87 C92 H92 118.0 . . ?
C93 C92 H92 118.0 . . ?
C92 C93 C82 112.1(6) . . ?
C92 C93 H93A 109.2 . . ?
C82 C93 H93A 109.2 . . ?
C92 C93 H93B 109.2 . . ?
C82 C93 H93B 109.2 . . ?
H93A C93 H93B 107.9 . . ?
C86 C94 H94A 109.5 . . ?
C86 C94 H94B 109.5 . . ?
H94A C94 H94B 109.5 . . ?
C86 C94 H94C 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?
C99 C95 C96 108.0(7) . . ?
C99 C95 I6 115.8(7) . . ?
C96 C95 I6 117.7(6) . . ?
C99 C95 H95 104.6 . . ?
C96 C95 H95 104.6 . . ?
I6 C95 H95 104.6 . . ?
C96A C96 C95 116.2(7) . . ?
C96A C96 C112 111.4(7) . . ?
C95 C96 C112 110.0(7) . . ?
C96A C96 C97 108.2(6) . . ?
C95 C96 C97 97.8(6) . . ?
C112 C96 C97 112.5(7) . . ?
C96 C96A C111 110.7(7) . . ?
C96 C96A H96A 109.5 . . ?
C111 C96A H96A 109.5 . . ?
C96 C96A H96B 109.5 . . ?
C111 C96A H96B 109.5 . . ?
H96A C96A H96B 108.1 . . ?
C98 C97 C100 120.0(7) . . ?
C98 C97 C96 104.8(7) . . ?
C100 C97 C96 113.5(6) . . ?
C98 C97 H97 105.8 . . ?
C100 C97 H97 105.8 . . ?
C96 C97 H97 105.8 . . ?
C97 C98 C99 104.1(7) . . ?
C97 C98 H98A 110.9 . . ?
C99 C98 H98A 110.9 . . ?
C97 C98 H98B 110.9 . . ?
C99 C98 H98B 110.9 . . ?
H98A C98 H98B 109.0 . . ?
C95 C99 C98 104.6(7) . . ?
C95 C99 H99A 110.8 . . ?
C98 C99 H99A 110.8 . . ?
C95 C99 H99B 110.8 . . ?
C98 C99 H99B 110.8 . . ?
H99A C99 H99B 108.9 . . ?
C97 C100 C109 110.8(7) . . ?
C97 C100 C101 109.8(7) . . ?
C109 C100 C101 110.2(7) . . ?
C97 C100 H100 108.7 . . ?
C109 C100 H100 108.7 . . ?
C101 C100 H100 108.7 . . ?
C100 C101 C111 112.7(6) . . ?
C100 C101 C102 113.4(7) . . ?
C111 C101 C102 111.7(7) . . ?
C100 C101 H101 106.1 . . ?
C111 C101 H101 106.1 . . ?
C102 C101 H101 106.1 . . ?
C107 C102 C110 111.7(7) . . ?
C107 C102 C103 108.6(6) . . ?
C110 C102 C103 107.4(7) . . ?
C107 C102 C101 108.6(7) . . ?
C110 C102 C101 111.9(7) . . ?
C103 C102 C101 108.6(7) . . ?
C108 C103 C104 120.9(7) . . ?
C108 C103 C102 123.9(8) . . ?
C104 C103 C102 115.2(7) . . ?
C105 C104 C103 111.4(7) . . ?
C105 C104 H10A 109.3 . . ?
C103 C104 H10A 109.3 . . ?
C105 C104 H10B 109.3 . . ?
C103 C104 H10B 109.3 . . ?
H10A C104 H10B 108.0 . . ?
O6 C105 C104 109.8(7) . . ?
O6 C105 C106 107.4(7) . . ?
C104 C105 C106 111.7(7) . . ?
O6 C105 H105 109.3 . . ?
C104 C105 H105 109.3 . . ?
C106 C105 H105 109.3 . . ?
C105 C106 C107 109.2(7) . . ?
C105 C106 H10C 109.8 . . ?
C107 C106 H10C 109.8 . . ?
C105 C106 H10D 109.8 . . ?
C107 C106 H10D 109.8 . . ?
H10C C106 H10D 108.3 . . ?
C102 C107 C106 114.5(7) . . ?
C102 C107 H10E 108.6 . . ?
C106 C107 H10E 108.6 . . ?
C102 C107 H10F 108.6 . . ?
C106 C107 H10F 108.6 . . ?
H10E C107 H10F 107.6 . . ?
C103 C108 C109 125.3(7) . . ?
C103 C108 H108 117.4 . . ?
C109 C108 H108 117.4 . . ?
C108 C109 C100 111.3(7) . . ?
C108 C109 H10G 109.4 . . ?
C100 C109 H10G 109.4 . . ?
C108 C109 H10H 109.4 . . ?
C100 C109 H10H 109.4 . . ?
H10G C109 H10H 108.0 . . ?
C102 C110 H11A 109.5 . . ?
C102 C110 H11B 109.5 . . ?
H11A C110 H11B 109.5 . . ?
C102 C110 H11C 109.5 . . ?
H11A C110 H11C 109.5 . . ?
H11B C110 H11C 109.5 . . ?
C96A C111 C101 114.3(7) . . ?
C96A C111 H11D 108.7 . . ?
C101 C111 H11D 108.7 . . ?
C96A C111 H11E 108.7 . . ?
C101 C111 H11E 108.7 . . ?
H11D C111 H11E 107.6 . . ?
C96 C112 H11G 109.5 . . ?
C96 C112 H11H 109.5 . . ?
H11G C112 H11H 109.5 . . ?
C96 C112 H11I 109.5 . . ?
H11G C112 H11I 109.5 . . ?
H11H C112 H11I 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
C5 C1 C2 C9 -154.9(7) . . . . ?
I1 C1 C2 C9 70.2(8) . . . . ?
C5 C1 C2 C3 -40.5(8) . . . . ?
I1 C1 C2 C3 -175.4(6) . . . . ?
C5 C1 C2 C19 76.7(9) . . . . ?
I1 C1 C2 C19 -58.2(8) . . . . ?
C9 C2 C3 C6 -61.1(9) . . . . ?
C19 C2 C3 C6 64.4(9) . . . . ?
C1 C2 C3 C6 178.4(7) . . . . ?
C9 C2 C3 C4 164.1(7) . . . . ?
C19 C2 C3 C4 -70.3(8) . . . . ?
C1 C2 C3 C4 43.7(8) . . . . ?
C6 C3 C4 C5 -163.1(7) . . . . ?
C2 C3 C4 C5 -31.9(8) . . . . ?
C2 C1 C5 C4 22.5(9) . . . . ?
I1 C1 C5 C4 158.0(6) . . . . ?
C3 C4 C5 C1 5.7(9) . . . . ?
C4 C3 C6 C7 -175.2(6) . . . . ?
C2 C3 C6 C7 57.0(8) . . . . ?
C4 C3 C6 C17 -53.1(9) . . . . ?
C2 C3 C6 C17 179.1(7) . . . . ?
C3 C6 C7 C8 -50.0(8) . . . . ?
C17 C6 C7 C8 -171.7(7) . . . . ?
C3 C6 C7 C10 -179.1(6) . . . . ?
C17 C6 C7 C10 59.2(8) . . . . ?
C6 C7 C8 C9 50.1(9) . . . . ?
C10 C7 C8 C9 178.4(7) . . . . ?
C3 C2 C9 C8 57.0(8) . . . . ?
C19 C2 C9 C8 -68.8(9) . . . . ?
C1 C2 C9 C8 164.6(7) . . . . ?
C7 C8 C9 C2 -54.2(9) . . . . ?
C6 C7 C10 C11 -44.5(8) . . . . ?
C8 C7 C10 C11 -172.6(7) . . . . ?
C6 C7 C10 C18 77.1(8) . . . . ?
C8 C7 C10 C18 -51.1(9) . . . . ?
C6 C7 C10 C15 -163.1(6) . . . . ?
C8 C7 C10 C15 68.8(8) . . . . ?
C18 C10 C11 C16 -108.6(9) . . . . ?
C15 C10 C11 C16 131.2(9) . . . . ?
C7 C10 C11 C16 14.1(11) . . . . ?
C18 C10 C11 C12 72.3(9) . . . . ?
C15 C10 C11 C12 -47.8(10) . . . . ?
C7 C10 C11 C12 -164.9(7) . . . . ?
C16 C11 C12 C13 -127.7(9) . . . . ?
C10 C11 C12 C13 51.4(10) . . . . ?
C11 C12 C13 O1 -176.1(7) . . . . ?
C11 C12 C13 C14 -55.2(10) . . . . ?
O1 C13 C14 C15 177.5(8) . . . . ?
C12 C13 C14 C15 58.9(10) . . . . ?
C11 C10 C15 C14 50.6(9) . . . . ?
C18 C10 C15 C14 -69.2(9) . . . . ?
C7 C10 C15 C14 170.0(7) . . . . ?
C13 C14 C15 C10 -58.0(10) . . . . ?
C10 C11 C16 C17 2.5(14) . . . . ?
C12 C11 C16 C17 -178.6(8) . . . . ?
C11 C16 C17 C6 11.4(12) . . . . ?
C3 C6 C17 C16 -162.7(7) . . . . ?
C7 C6 C17 C16 -41.2(9) . . . . ?
C24 C20 C21 C28 -156.1(8) . . . . ?
I2 C20 C21 C28 71.7(10) . . . . ?
C24 C20 C21 C38 74.5(10) . . . . ?
I2 C20 C21 C38 -57.7(9) . . . . ?
C24 C20 C21 C22 -42.2(9) . . . . ?
I2 C20 C21 C22 -174.4(6) . . . . ?
C28 C21 C22 C23 165.8(7) . . . . ?
C20 C21 C22 C23 45.6(8) . . . . ?
C38 C21 C22 C23 -69.8(8) . . . . ?
C28 C21 C22 C25 -62.6(9) . . . . ?
C20 C21 C22 C25 177.3(7) . . . . ?
C38 C21 C22 C25 61.8(9) . . . . ?
C25 C22 C23 C24 -161.6(7) . . . . ?
C21 C22 C23 C24 -33.8(8) . . . . ?
C21 C20 C24 C23 22.9(10) . . . . ?
I2 C20 C24 C23 156.1(6) . . . . ?
C22 C23 C24 C20 7.0(10) . . . . ?
C23 C22 C25 C36 -60.5(10) . . . . ?
C21 C22 C25 C36 175.9(7) . . . . ?
C23 C22 C25 C26 -178.9(7) . . . . ?
C21 C22 C25 C26 57.5(9) . . . . ?
C36 C25 C26 C27 -169.8(7) . . . . ?
C22 C25 C26 C27 -49.3(9) . . . . ?
C36 C25 C26 C29 63.5(8) . . . . ?
C22 C25 C26 C29 -176.0(7) . . . . ?
C25 C26 C27 C28 49.4(10) . . . . ?
C29 C26 C27 C28 176.0(7) . . . . ?
C20 C21 C28 C27 165.6(8) . . . . ?
C38 C21 C28 C27 -65.9(9) . . . . ?
C22 C21 C28 C27 58.2(9) . . . . ?
C26 C27 C28 C21 -54.1(10) . . . . ?
C27 C26 C29 C30 -171.2(7) . . . . ?
C25 C26 C29 C30 -44.3(9) . . . . ?
C27 C26 C29 C34 71.4(8) . . . . ?
C25 C26 C29 C34 -161.7(7) . . . . ?
C27 C26 C29 C37 -50.8(9) . . . . ?
C25 C26 C29 C37 76.1(9) . . . . ?
C34 C29 C30 C35 129.8(9) . . . . ?
C37 C29 C30 C35 -109.7(9) . . . . ?
C26 C29 C30 C35 12.1(11) . . . . ?
C34 C29 C30 C31 -50.8(9) . . . . ?
C37 C29 C30 C31 69.6(9) . . . . ?
C26 C29 C30 C31 -168.6(7) . . . . ?
C35 C30 C31 C32 -126.7(9) . . . . ?
C29 C30 C31 C32 53.9(10) . . . . ?
C30 C31 C32 O2 -175.8(7) . . . . ?
C30 C31 C32 C33 -54.6(9) . . . . ?
O2 C32 C33 C34 177.8(7) . . . . ?
C31 C32 C33 C34 55.3(10) . . . . ?
C32 C33 C34 C29 -56.2(10) . . . . ?
C30 C29 C34 C33 52.2(9) . . . . ?
C37 C29 C34 C33 -66.8(9) . . . . ?
C26 C29 C34 C33 171.0(7) . . . . ?
C31 C30 C35 C36 -178.1(8) . . . . ?
C29 C30 C35 C36 1.2(14) . . . . ?
C30 C35 C36 C25 18.1(12) . . . . ?
C22 C25 C36 C35 -167.5(7) . . . . ?
C26 C25 C36 C35 -48.5(9) . . . . ?
C43 C39 C40 C41 -42.1(14) . . . . ?
I3 C39 C40 C41 179.5(10) . . . . ?
C43 C39 C40 C47 -155.0(12) . . . . ?
I3 C39 C40 C47 66.6(14) . . . . ?
C43 C39 C40 C57 76.5(14) . . . . ?
I3 C39 C40 C57 -61.9(14) . . . . ?
C39 C40 C41 C44 179.8(11) . . . . ?
C47 C40 C41 C44 -60.3(12) . . . . ?
C57 C40 C41 C44 62.4(13) . . . . ?
C39 C40 C41 C42 45.2(12) . . . . ?
C47 C40 C41 C42 165.2(10) . . . . ?
C57 C40 C41 C42 -72.1(13) . . . . ?
C40 C41 C42 C43 -33.0(14) . . . . ?
C44 C41 C42 C43 -165.8(12) . . . . ?
C40 C39 C43 C42 22.5(17) . . . . ?
I3 C39 C43 C42 161.0(11) . . . . ?
C41 C42 C43 C39 6.3(17) . . . . ?
C40 C41 C44 C55 176.2(9) . . . . ?
C42 C41 C44 C55 -56.2(14) . . . . ?
C40 C41 C44 C45 54.5(12) . . . . ?
C42 C41 C44 C45 -177.9(10) . . . . ?
C41 C44 C45 C46 -45.6(12) . . . . ?
C55 C44 C45 C46 -169.5(9) . . . . ?
C41 C44 C45 C48 -177.2(8) . . . . ?
C55 C44 C45 C48 59.0(11) . . . . ?
C48 C45 C46 C47 179.1(9) . . . . ?
C44 C45 C46 C47 49.1(13) . . . . ?
C45 C46 C47 C40 -55.4(14) . . . . ?
C41 C40 C47 C46 57.6(12) . . . . ?
C39 C40 C47 C46 165.2(10) . . . . ?
C57 C40 C47 C46 -66.2(13) . . . . ?
C46 C45 C48 C49 -175.1(9) . . . . ?
C44 C45 C48 C49 -44.9(11) . . . . ?
C46 C45 C48 C56 -54.1(12) . . . . ?
C44 C45 C48 C56 76.1(11) . . . . ?
C46 C45 C48 C53 66.7(12) . . . . ?
C44 C45 C48 C53 -163.2(8) . . . . ?
C45 C48 C49 C54 15.6(15) . . . . ?
C56 C48 C49 C54 -106.5(12) . . . . ?
C53 C48 C49 C54 134.6(12) . . . . ?
C45 C48 C49 C50 -167.3(9) . . . . ?
C56 C48 C49 C50 70.6(12) . . . . ?
C53 C48 C49 C50 -48.3(12) . . . . ?
C54 C49 C50 C51 -131.4(11) . . . . ?
C48 C49 C50 C51 51.3(12) . . . . ?
C49 C50 C51 O3 -170.8(8) . . . . ?
C49 C50 C51 C52 -52.1(12) . . . . ?
O3 C51 C52 C53 175.4(10) . . . . ?
C50 C51 C52 C53 57.0(14) . . . . ?
C51 C52 C53 C48 -59.2(14) . . . . ?
C49 C48 C53 C52 51.7(13) . . . . ?
C45 C48 C53 C52 171.7(10) . . . . ?
C56 C48 C53 C52 -66.8(12) . . . . ?
C48 C49 C54 C55 0.0(18) . . . . ?
C50 C49 C54 C55 -177.0(10) . . . . ?
C49 C54 C55 C44 14.3(17) . . . . ?
C41 C44 C55 C54 -164.1(10) . . . . ?
C45 C44 C55 C54 -42.5(12) . . . . ?
C62 C58 C59 C66 -149.0(9) . . . . ?
I4 C58 C59 C66 52.5(11) . . . . ?
C62 C58 C59 C76 83.4(11) . . . . ?
I4 C58 C59 C76 -75.0(10) . . . . ?
C62 C58 C59 C60 -35.0(11) . . . . ?
I4 C58 C59 C60 166.6(7) . . . . ?
C58 C59 C60 C63 172.7(8) . . . . ?
C66 C59 C60 C63 -64.2(9) . . . . ?
C76 C59 C60 C63 57.5(10) . . . . ?
C58 C59 C60 C61 40.1(9) . . . . ?
C66 C59 C60 C61 163.1(8) . . . . ?
C76 C59 C60 C61 -75.1(10) . . . . ?
C63 C60 C61 C62 -160.0(8) . . . . ?
C59 C60 C61 C62 -31.8(9) . . . . ?
C59 C58 C62 C61 16.5(12) . . . . ?
I4 C58 C62 C61 173.8(7) . . . . ?
C60 C61 C62 C58 10.4(11) . . . . ?
C61 C60 C63 C74 -57.4(10) . . . . ?
C59 C60 C63 C74 178.2(7) . . . . ?
C61 C60 C63 C64 -176.6(7) . . . . ?
C59 C60 C63 C64 59.0(9) . . . . ?
C60 C63 C64 C65 -47.7(9) . . . . ?
C74 C63 C64 C65 -167.7(8) . . . . ?
C60 C63 C64 C67 -176.9(6) . . . . ?
C74 C63 C64 C67 63.1(9) . . . . ?
C63 C64 C65 C66 45.1(10) . . . . ?
C67 C64 C65 C66 173.8(7) . . . . ?
C64 C65 C66 C59 -50.5(10) . . . . ?
C58 C59 C66 C65 166.2(8) . . . . ?
C76 C59 C66 C65 -66.7(9) . . . . ?
C60 C59 C66 C65 57.0(9) . . . . ?
C65 C64 C67 C68 -174.5(7) . . . . ?
C63 C64 C67 C68 -45.0(9) . . . . ?
C65 C64 C67 C75 -54.4(10) . . . . ?
C63 C64 C67 C75 75.1(9) . . . . ?
C65 C64 C67 C72 66.2(9) . . . . ?
C63 C64 C67 C72 -164.3(7) . . . . ?
C75 C67 C68 C73 -108.0(11) . . . . ?
C72 C67 C68 C73 132.4(10) . . . . ?
C64 C67 C68 C73 13.4(13) . . . . ?
C75 C67 C68 C69 71.6(11) . . . . ?
C72 C67 C68 C69 -47.9(11) . . . . ?
C64 C67 C68 C69 -166.9(8) . . . . ?
C73 C68 C69 C70 -128.1(11) . . . . ?
C67 C68 C69 C70 52.2(12) . . . . ?
C68 C69 C70 O4 -177.0(9) . . . . ?
C68 C69 C70 C71 -56.2(12) . . . . ?
O4 C70 C71 C72 177.2(9) . . . . ?
C69 C70 C71 C72 58.8(12) . . . . ?
C70 C71 C72 C67 -56.7(11) . . . . ?
C68 C67 C72 C71 49.9(11) . . . . ?
C75 C67 C72 C71 -69.0(11) . . . . ?
C64 C67 C72 C71 169.6(8) . . . . ?
C67 C68 C73 C74 1.1(16) . . . . ?
C69 C68 C73 C74 -178.5(10) . . . . ?
C60 C63 C74 C73 -165.6(8) . . . . ?
C64 C63 C74 C73 -46.4(11) . . . . ?
C68 C73 C74 C63 16.3(14) . . . . ?
C81 C77 C78 C79 -36.3(10) . . . . ?
I5 C77 C78 C79 172.5(6) . . . . ?
C81 C77 C78 C85 -150.7(8) . . . . ?
I5 C77 C78 C85 58.1(10) . . . . ?
C81 C77 C78 C79A 82.6(10) . . . . ?
I5 C77 C78 C79A -68.6(9) . . . . ?
C77 C78 C79 C80 40.6(8) . . . . ?
C85 C78 C79 C80 162.1(6) . . . . ?
C79A C78 C79 C80 -73.9(8) . . . . ?
C77 C78 C79 C82 173.7(7) . . . . ?
C85 C78 C79 C82 -64.8(8) . . . . ?
C79A C78 C79 C82 59.2(9) . . . . ?
C78 C79 C80 C81 -32.8(8) . . . . ?
C82 C79 C80 C81 -161.0(7) . . . . ?
C78 C77 C81 C80 17.1(11) . . . . ?
I5 C77 C81 C80 167.4(6) . . . . ?
C79 C80 C81 C77 10.1(9) . . . . ?
C80 C79 C82 C83 -176.4(6) . . . . ?
C78 C79 C82 C83 58.9(8) . . . . ?
C80 C79 C82 C93 -57.0(9) . . . . ?
C78 C79 C82 C93 178.2(7) . . . . ?
C79 C82 C83 C84 -48.9(8) . . . . ?
C93 C82 C83 C84 -169.4(7) . . . . ?
C79 C82 C83 C86 -176.3(6) . . . . ?
C93 C82 C83 C86 63.2(8) . . . . ?
C82 C83 C84 C85 47.4(10) . . . . ?
C86 C83 C84 C85 174.9(7) . . . . ?
C77 C78 C85 C84 167.2(8) . . . . ?
C79 C78 C85 C84 59.2(9) . . . . ?
C79A C78 C85 C84 -67.0(9) . . . . ?
C83 C84 C85 C78 -52.2(10) . . . . ?
C82 C83 C86 C91 -164.6(6) . . . . ?
C84 C83 C86 C91 67.2(8) . . . . ?
C82 C83 C86 C87 -44.8(9) . . . . ?
C84 C83 C86 C87 -173.0(7) . . . . ?
C82 C83 C86 C94 73.7(8) . . . . ?
C84 C83 C86 C94 -54.4(9) . . . . ?
C91 C86 C87 C92 132.3(9) . . . . ?
C83 C86 C87 C92 11.4(12) . . . . ?
C94 C86 C87 C92 -109.5(9) . . . . ?
C91 C86 C87 C88 -47.7(9) . . . . ?
C83 C86 C87 C88 -168.5(7) . . . . ?
C94 C86 C87 C88 70.6(9) . . . . ?
C92 C87 C88 C89 -129.6(9) . . . . ?
C86 C87 C88 C89 50.3(10) . . . . ?
C87 C88 C89 O5 -174.8(7) . . . . ?
C87 C88 C89 C90 -52.7(9) . . . . ?
O5 C89 C90 C91 174.7(7) . . . . ?
C88 C89 C90 C91 54.6(10) . . . . ?
C87 C86 C91 C90 51.1(9) . . . . ?
C83 C86 C91 C90 171.7(7) . . . . ?
C94 C86 C91 C90 -65.7(9) . . . . ?
C89 C90 C91 C86 -56.0(10) . . . . ?
C88 C87 C92 C93 -176.3(8) . . . . ?
C86 C87 C92 C93 3.8(14) . . . . ?
C87 C92 C93 C82 14.5(12) . . . . ?
C79 C82 C93 C92 -166.0(7) . . . . ?
C83 C82 C93 C92 -46.2(9) . . . . ?
C99 C95 C96 C96A -156.0(7) . . . . ?
I6 C95 C96 C96A 70.6(9) . . . . ?
C99 C95 C96 C112 76.3(9) . . . . ?
I6 C95 C96 C112 -57.1(9) . . . . ?
C99 C95 C96 C97 -41.2(9) . . . . ?
I6 C95 C96 C97 -174.6(6) . . . . ?
C95 C96 C96A C111 166.8(7) . . . . ?
C112 C96 C96A C111 -66.2(8) . . . . ?
C97 C96 C96A C111 58.1(8) . . . . ?
C96A C96 C97 C98 165.2(7) . . . . ?
C95 C96 C97 C98 44.2(8) . . . . ?
C112 C96 C97 C98 -71.2(9) . . . . ?
C96A C96 C97 C100 -62.0(9) . . . . ?
C95 C96 C97 C100 177.0(7) . . . . ?
C112 C96 C97 C100 61.5(9) . . . . ?
C100 C97 C98 C99 -161.1(7) . . . . ?
C96 C97 C98 C99 -32.1(9) . . . . ?
C96 C95 C99 C98 22.6(10) . . . . ?
I6 C95 C99 C98 157.0(6) . . . . ?
C97 C98 C99 C95 6.1(10) . . . . ?
C98 C97 C100 C109 -56.9(10) . . . . ?
C96 C97 C100 C109 178.2(7) . . . . ?
C98 C97 C100 C101 -178.8(7) . . . . ?
C96 C97 C100 C101 56.3(9) . . . . ?
C97 C100 C101 C111 -47.5(9) . . . . ?
C109 C100 C101 C111 -169.8(7) . . . . ?
C97 C100 C101 C102 -175.7(6) . . . . ?
C109 C100 C101 C102 62.0(9) . . . . ?
C100 C101 C102 C107 -161.8(6) . . . . ?
C111 C101 C102 C107 69.5(8) . . . . ?
C100 C101 C102 C110 74.5(8) . . . . ?
C111 C101 C102 C110 -54.2(9) . . . . ?
C100 C101 C102 C103 -43.9(8) . . . . ?
C111 C101 C102 C103 -172.6(7) . . . . ?
C107 C102 C103 C108 130.4(9) . . . . ?
C110 C102 C103 C108 -108.7(9) . . . . ?
C101 C102 C103 C108 12.5(11) . . . . ?
C107 C102 C103 C104 -48.5(9) . . . . ?
C110 C102 C103 C104 72.4(9) . . . . ?
C101 C102 C103 C104 -166.4(7) . . . . ?
C108 C103 C104 C105 -127.2(9) . . . . ?
C102 C103 C104 C105 51.7(9) . . . . ?
C103 C104 C105 O6 -174.9(6) . . . . ?
C103 C104 C105 C106 -55.8(10) . . . . ?
O6 C105 C106 C107 178.1(7) . . . . ?
C104 C105 C106 C107 57.6(10) . . . . ?
C110 C102 C107 C106 -67.0(9) . . . . ?
C103 C102 C107 C106 51.2(9) . . . . ?
C101 C102 C107 C106 169.2(7) . . . . ?
C105 C106 C107 C102 -57.2(10) . . . . ?
C104 C103 C108 C109 -179.0(8) . . . . ?
C102 C103 C108 C109 2.2(14) . . . . ?
C103 C108 C109 C100 14.3(13) . . . . ?
C97 C100 C109 C108 -165.9(7) . . . . ?
C101 C100 C109 C108 -44.2(10) . . . . ?
C96 C96A C111 C101 -53.2(10) . . . . ?
C100 C101 C111 C96A 47.7(10) . . . . ?
C102 C101 C111 C96A 176.7(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1OA O4 0.84 1.88 2.671(12) 157.0 . yes
O3 H3OA O1 0.84 1.82 2.660(11) 172.8 1_655 yes
O2 H20A O5 0.84 2.03 2.674(10) 132.4 1_455 yes
O4 H4OA O3 0.84 1.79 2.620(12) 170.4 . yes
O5 H5OA O6 0.84 1.96 2.699(10) 146.8 . yes
O6 H6OA O2 0.84 1.84 2.682(9) 178.0 . yes

_refine_diff_density_max         1.450
_refine_diff_density_min         -3.365
_refine_diff_density_rms         0.115

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1921637'
loop_
_audit_author_name
_audit_author_address
'Stephan Hohloch'
;University of Paderborn
Germany
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H90 N6 O4'
_chemical_formula_weight         983.39

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.116(3)
_cell_length_b                   15.693(3)
_cell_length_c                   16.506(3)
_cell_angle_alpha                69.462(4)
_cell_angle_beta                 82.703(4)
_cell_angle_gamma                81.560(4)
_cell_volume                     3375.6(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    8416
_cell_measurement_theta_min      1.39
_cell_measurement_theta_max      25.47

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.967
_exptl_crystal_F_000             1072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.060
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            65353
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.394
_diffrn_reflns_theta_max         25.471
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12374
_reflns_number_gt                8416
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker ApexIII suite, 2018'
_computing_cell_refinement       'Bruker ApexIII suite, 2018'
_computing_data_reduction        'Bruker ApexIII suite, 2018'
_computing_structure_solution    ShelXT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  WinGX
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0584P)²+3.3213P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12374
_refine_ls_number_parameters     683
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0681
_refine_ls_wR_factor_ref         0.1756
_refine_ls_wR_factor_gt          0.1524
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O2A O 0.59152(12) 0.12894(13) 0.61208(11) 0.0326(4) Uani 1 1 d . . . . .
O1 O 0.58263(13) 0.29177(12) 0.50821(11) 0.0347(4) Uani 1 1 d . . . . .
O2 O 0.20164(12) 0.19493(12) 0.51983(11) 0.0321(4) Uani 1 1 d . . . . .
O1A O 0.22356(14) 0.21287(14) 0.36100(13) 0.0443(5) Uani 1 1 d . . . . .
N1A N 0.41029(15) 0.11095(14) 0.57886(13) 0.0283(5) Uani 1 1 d . . . . .
N1 N 0.25208(15) 0.34523(14) 0.54282(13) 0.0300(5) Uani 1 1 d . . . . .
N3A N 0.34479(15) 0.05939(14) 0.50258(13) 0.0293(5) Uani 1 1 d . . . . .
N2A N 0.35239(15) 0.04891(14) 0.58430(13) 0.0304(5) Uani 1 1 d . . . . .
N2 N 0.30134(15) 0.36031(14) 0.59962(14) 0.0318(5) Uani 1 1 d . . . . .
N3 N 0.38633(15) 0.37759(14) 0.55662(14) 0.0301(5) Uani 1 1 d . . . . .
C16A C 0.51714(18) 0.13140(16) 0.67336(16) 0.0289(6) Uani 1 1 d . . . . .
C11A C 0.42482(18) 0.12610(17) 0.65728(15) 0.0285(6) Uani 1 1 d . . . . .
C2 C 0.39337(18) 0.37323(16) 0.47469(16) 0.0287(6) Uani 1 1 d . . . . .
C2A C 0.39458(18) 0.12710(17) 0.44495(16) 0.0298(6) Uani 1 1 d . . . . .
C16 C 0.13588(18) 0.24142(17) 0.55595(16) 0.0304(6) Uani 1 1 d . . . . .
C1 C 0.30425(18) 0.35174(17) 0.46772(17) 0.0310(6) Uani 1 1 d . . . . .
H1 H 0.2841 0.3433 0.4198 0.037 Uiso 1 1 calc R U . . .
C13A C 0.35508(19) 0.15123(17) 0.78754(16) 0.0314(6) Uani 1 1 d . . . . .
C7 C 0.52488(19) 0.46570(17) 0.25800(17) 0.0327(6) Uani 1 1 d . . . . .
C11 C 0.15601(18) 0.32065(17) 0.56847(17) 0.0309(6) Uani 1 1 d . . . . .
C10 C 0.56881(18) 0.34891(17) 0.42973(16) 0.0304(6) Uani 1 1 d . . . . .
C6A C 0.47697(19) 0.14911(17) 0.29978(17) 0.0338(6) Uani 1 1 d . . . . .
H6A H 0.5335 0.1231 0.3264 0.041 Uiso 1 1 calc R U . . .
C5 C 0.47445(18) 0.39138(17) 0.40929(16) 0.0299(6) Uani 1 1 d . . . . .
C9 C 0.64271(18) 0.37208(17) 0.36105(17) 0.0316(6) Uani 1 1 d . . . . .
C1A C 0.43901(18) 0.15872(17) 0.49628(15) 0.0300(6) Uani 1 1 d . . . . .
H1A H 0.4805 0.2039 0.4779 0.036 Uiso 1 1 calc R U . . .
C14A C 0.44880(19) 0.14864(18) 0.80720(16) 0.0330(6) Uani 1 1 d . . . . .
H14A H 0.4569 0.1546 0.8599 0.040 Uiso 1 1 calc R U . . .
C5A C 0.39193(19) 0.15751(17) 0.35086(16) 0.0324(6) Uani 1 1 d . . . . .
C6 C 0.45408(19) 0.44677(17) 0.32515(16) 0.0314(6) Uani 1 1 d . . . . .
H6 H 0.3910 0.4715 0.3142 0.038 Uiso 1 1 calc R U . . .
C12A C 0.34369(19) 0.13681(17) 0.71122(16) 0.0311(6) Uani 1 1 d . . . . .
H12A H 0.2829 0.1344 0.6966 0.037 Uiso 1 1 calc R U . . .
C15 C 0.04213(18) 0.21497(18) 0.58935(17) 0.0321(6) Uani 1 1 d . . . . .
C10A C 0.30563(19) 0.19826(19) 0.31347(17) 0.0344(6) Uani 1 1 d . . . . .
C15A C 0.53128(18) 0.13785(17) 0.75411(16) 0.0308(6) Uani 1 1 d . . . . .
C12 C 0.09241(19) 0.37385(18) 0.60740(18) 0.0363(6) Uani 1 1 d . . . . .
H12 H 0.1113 0.4255 0.6134 0.044 Uiso 1 1 calc R U . . .
C8 C 0.61839(19) 0.42818(17) 0.27890(17) 0.0331(6) Uani 1 1 d . . . . .
H8 H 0.6676 0.4417 0.2348 0.040 Uiso 1 1 calc R U . . .
C29A C 0.63254(19) 0.12860(18) 0.78221(17) 0.0336(6) Uani 1 1 d . . . . .
C7A C 0.4787(2) 0.17859(18) 0.21074(17) 0.0356(6) Uani 1 1 d . . . . .
C17 C 0.4999(2) 0.52661(19) 0.16576(17) 0.0370(6) Uani 1 1 d . . . . .
C9A C 0.3037(2) 0.22418(19) 0.22256(18) 0.0378(7) Uani 1 1 d . . . . .
C13 C 0.00127(19) 0.34969(19) 0.63702(19) 0.0388(7) Uani 1 1 d . . . . .
C25A C 0.2691(2) 0.1704(2) 0.84769(17) 0.0378(6) Uani 1 1 d . . . . .
C29 C 0.01298(19) 0.12667(19) 0.58405(19) 0.0375(6) Uani 1 1 d . . . . .
C21 C 0.74776(19) 0.33339(19) 0.37831(18) 0.0381(7) Uani 1 1 d . . . . .
C8A C 0.3901(2) 0.21410(19) 0.17541(17) 0.0391(7) Uani 1 1 d . . . . .
H8A H 0.3895 0.2323 0.1154 0.047 Uiso 1 1 calc R U . . .
C14 C -0.0203(2) 0.27002(19) 0.62750(18) 0.0379(6) Uani 1 1 d . . . . .
H14 H -0.0813 0.2522 0.6483 0.045 Uiso 1 1 calc R U . . .
C17A C 0.5702(2) 0.17264(19) 0.15158(17) 0.0399(7) Uani 1 1 d . . . . .
C61 C 0.45742(19) 0.39936(19) 0.60170(18) 0.0375(6) Uani 1 1 d . . . . .
H61A H 0.4319 0.4517 0.6180 0.056 Uiso 1 1 calc R U . . .
H61B H 0.5149 0.4126 0.5639 0.056 Uiso 1 1 calc R U . . .
H61C H 0.4721 0.3480 0.6528 0.056 Uiso 1 1 calc R U . . .
C32A C 0.6860(2) 0.2092(2) 0.72280(19) 0.0420(7) Uani 1 1 d . . . . .
H32A H 0.6913 0.2093 0.6642 0.063 Uiso 1 1 calc R U . . .
H32B H 0.7490 0.2031 0.7415 0.063 Uiso 1 1 calc R U . . .
H32C H 0.6511 0.2655 0.7255 0.063 Uiso 1 1 calc R U . . .
C30A C 0.6878(2) 0.03758(19) 0.77835(19) 0.0413(7) Uani 1 1 d . . . . .
H30A H 0.6532 -0.0124 0.8148 0.062 Uiso 1 1 calc R U . . .
H30B H 0.7505 0.0305 0.7982 0.062 Uiso 1 1 calc R U . . .
H30C H 0.6941 0.0380 0.7196 0.062 Uiso 1 1 calc R U . . .
C61A C 0.2836(2) 0.00293(19) 0.48264(18) 0.0373(6) Uani 1 1 d . . . . .
H61D H 0.2646 -0.0445 0.5351 0.056 Uiso 1 1 calc R U . . .
H61E H 0.3185 -0.0242 0.4423 0.056 Uiso 1 1 calc R U . . .
H61F H 0.2274 0.0404 0.4575 0.056 Uiso 1 1 calc R U . . .
C21A C 0.2088(2) 0.2621(2) 0.17955(19) 0.0476(8) Uani 1 1 d . . . . .
C30 C 0.0190(2) 0.1333(2) 0.4889(2) 0.0448(7) Uani 1 1 d . . . . .
H30D H -0.0217 0.1861 0.4574 0.067 Uiso 1 1 calc R U . . .
H30E H -0.0017 0.0792 0.4853 0.067 Uiso 1 1 calc R U . . .
H30F H 0.0841 0.1386 0.4643 0.067 Uiso 1 1 calc R U . . .
C31 C 0.0809(2) 0.04498(19) 0.6357(2) 0.0460(7) Uani 1 1 d . . . . .
H31A H 0.1463 0.0557 0.6152 0.069 Uiso 1 1 calc R U . . .
H31B H 0.0677 -0.0098 0.6279 0.069 Uiso 1 1 calc R U . . .
H31C H 0.0711 0.0381 0.6962 0.069 Uiso 1 1 calc R U . . .
C31A C 0.6305(2) 0.1268(2) 0.87545(18) 0.0434(7) Uani 1 1 d . . . . .
H31D H 0.5995 0.1840 0.8796 0.065 Uiso 1 1 calc R U . . .
H31E H 0.6951 0.1176 0.8919 0.065 Uiso 1 1 calc R U . . .
H31F H 0.5957 0.0778 0.9135 0.065 Uiso 1 1 calc R U . . .
C22 C 0.7568(2) 0.2287(2) 0.4050(2) 0.0448(7) Uani 1 1 d . . . . .
H22A H 0.7185 0.2042 0.4584 0.067 Uiso 1 1 calc R U . . .
H22B H 0.8228 0.2045 0.4127 0.067 Uiso 1 1 calc R U . . .
H22C H 0.7348 0.2121 0.3604 0.067 Uiso 1 1 calc R U . . .
C25 C -0.0728(2) 0.4055(2) 0.6798(2) 0.0489(8) Uani 1 1 d . . . . .
C32 C -0.0894(2) 0.1095(2) 0.6226(2) 0.0504(8) Uani 1 1 d . . . . .
H32D H -0.0951 0.1048 0.6826 0.076 Uiso 1 1 calc R U . . .
H32E H -0.1040 0.0536 0.6181 0.076 Uiso 1 1 calc R U . . .
H32F H -0.1336 0.1595 0.5915 0.076 Uiso 1 1 calc R U . . .
C26A C 0.2767(2) 0.1013(2) 0.93960(18) 0.0506(8) Uani 1 1 d . . . . .
H26A H 0.2769 0.0406 0.9384 0.076 Uiso 1 1 calc R U . . .
H26B H 0.2228 0.1144 0.9768 0.076 Uiso 1 1 calc R U . . .
H26C H 0.3351 0.1057 0.9612 0.076 Uiso 1 1 calc R U . . .
C23 C 0.7781(2) 0.3616(2) 0.4502(2) 0.0473(8) Uani 1 1 d . . . . .
H23A H 0.7359 0.3399 0.5017 0.071 Uiso 1 1 calc R U . . .
H23B H 0.7747 0.4271 0.4317 0.071 Uiso 1 1 calc R U . . .
H23C H 0.8428 0.3354 0.4624 0.071 Uiso 1 1 calc R U . . .
C28A C 0.1737(2) 0.1648(3) 0.8159(2) 0.0560(9) Uani 1 1 d . . . . .
H28A H 0.1671 0.2090 0.7589 0.084 Uiso 1 1 calc R U . . .
H28B H 0.1215 0.1774 0.8549 0.084 Uiso 1 1 calc R U . . .
H28C H 0.1725 0.1045 0.8141 0.084 Uiso 1 1 calc R U . . .
C27A C 0.2694(3) 0.2676(2) 0.8500(2) 0.0575(9) Uani 1 1 d . . . . .
H27A H 0.3273 0.2711 0.8729 0.086 Uiso 1 1 calc R U . . .
H27B H 0.2148 0.2812 0.8862 0.086 Uiso 1 1 calc R U . . .
H27C H 0.2662 0.3111 0.7922 0.086 Uiso 1 1 calc R U . . .
C18 C 0.5879(3) 0.5341(2) 0.09978(19) 0.0568(9) Uani 1 1 d . . . . .
H18A H 0.6361 0.5612 0.1159 0.085 Uiso 1 1 calc R U . . .
H18B H 0.5694 0.5717 0.0431 0.085 Uiso 1 1 calc R U . . .
H18C H 0.6135 0.4742 0.0991 0.085 Uiso 1 1 calc R U . . .
C23A C 0.1687(3) 0.3526(2) 0.1932(2) 0.0613(10) Uani 1 1 d . . . . .
H23D H 0.1585 0.3429 0.2543 0.092 Uiso 1 1 calc R U . . .
H23E H 0.1088 0.3747 0.1672 0.092 Uiso 1 1 calc R U . . .
H23F H 0.2136 0.3968 0.1668 0.092 Uiso 1 1 calc R U . . .
C24 C 0.8179(2) 0.3688(2) 0.2979(2) 0.0562(9) Uani 1 1 d . . . . .
H24A H 0.8823 0.3437 0.3122 0.084 Uiso 1 1 calc R U . . .
H24B H 0.8131 0.4344 0.2792 0.084 Uiso 1 1 calc R U . . .
H24C H 0.8020 0.3504 0.2521 0.084 Uiso 1 1 calc R U . . .
C20 C 0.4604(3) 0.6212(2) 0.1661(2) 0.0592(9) Uani 1 1 d . . . . .
H20A H 0.4038 0.6173 0.2056 0.089 Uiso 1 1 calc R U . . .
H20B H 0.4445 0.6592 0.1087 0.089 Uiso 1 1 calc R U . . .
H20C H 0.5079 0.6472 0.1843 0.089 Uiso 1 1 calc R U . . .
C19 C 0.4246(3) 0.4855(2) 0.1365(2) 0.0599(9) Uani 1 1 d . . . . .
H19A H 0.4482 0.4240 0.1394 0.090 Uiso 1 1 calc R U . . .
H19B H 0.4116 0.5218 0.0779 0.090 Uiso 1 1 calc R U . . .
H19C H 0.3665 0.4849 0.1738 0.090 Uiso 1 1 calc R U . . .
C20A C 0.6580(2) 0.1292(2) 0.2024(2) 0.0575(9) Uani 1 1 d . . . . .
H20D H 0.7134 0.1266 0.1627 0.086 Uiso 1 1 calc R U . . .
H20E H 0.6477 0.0684 0.2402 0.086 Uiso 1 1 calc R U . . .
H20F H 0.6683 0.1653 0.2362 0.086 Uiso 1 1 calc R U . . .
C27 C -0.1660(2) 0.4299(2) 0.6337(2) 0.0634(10) Uani 1 1 d . . . . .
H27D H -0.2131 0.4631 0.6620 0.095 Uiso 1 1 calc R U . . .
H27E H -0.1899 0.3747 0.6363 0.095 Uiso 1 1 calc R U . . .
H27F H -0.1533 0.4670 0.5742 0.095 Uiso 1 1 calc R U . . .
C22A C 0.1360(2) 0.1922(3) 0.2169(2) 0.0649(10) Uani 1 1 d . . . . .
H22D H 0.1610 0.1366 0.2060 0.097 Uiso 1 1 calc R U . . .
H22E H 0.0769 0.2164 0.1898 0.097 Uiso 1 1 calc R U . . .
H22F H 0.1242 0.1797 0.2783 0.097 Uiso 1 1 calc R U . . .
C24A C 0.2236(3) 0.2810(3) 0.0809(2) 0.0713(11) Uani 1 1 d . . . . .
H24D H 0.2686 0.3254 0.0553 0.107 Uiso 1 1 calc R U . . .
H24E H 0.1633 0.3042 0.0558 0.107 Uiso 1 1 calc R U . . .
H24F H 0.2482 0.2253 0.0702 0.107 Uiso 1 1 calc R U . . .
C28 C -0.0968(3) 0.3465(3) 0.7743(2) 0.0750(12) Uani 1 1 d . . . . .
H28D H -0.0398 0.3300 0.8049 0.112 Uiso 1 1 calc R U . . .
H28E H -0.1213 0.2921 0.7757 0.112 Uiso 1 1 calc R U . . .
H28F H -0.1444 0.3805 0.8013 0.112 Uiso 1 1 calc R U . . .
C18A C 0.5577(3) 0.1143(3) 0.0972(2) 0.0692(11) Uani 1 1 d . . . . .
H18D H 0.5046 0.1420 0.0622 0.104 Uiso 1 1 calc R U . . .
H18E H 0.5453 0.0540 0.1350 0.104 Uiso 1 1 calc R U . . .
H18F H 0.6152 0.1103 0.0603 0.104 Uiso 1 1 calc R U . . .
C26 C -0.0382(3) 0.4936(3) 0.6748(4) 0.116(2) Uani 1 1 d . . . . .
H26D H 0.0183 0.4802 0.7058 0.174 Uiso 1 1 calc R U . . .
H26E H -0.0876 0.5276 0.7002 0.174 Uiso 1 1 calc R U . . .
H26F H -0.0232 0.5291 0.6151 0.174 Uiso 1 1 calc R U . . .
C19A C 0.5888(3) 0.2684(2) 0.0913(2) 0.0676(11) Uani 1 1 d . . . . .
H19D H 0.5340 0.2968 0.0588 0.101 Uiso 1 1 calc R U . . .
H19E H 0.6443 0.2645 0.0521 0.101 Uiso 1 1 calc R U . . .
H19F H 0.5999 0.3044 0.1251 0.101 Uiso 1 1 calc R U . . .
H1O H 0.221(3) 0.206(3) 0.424(3) 0.090(13) Uiso 1 1 d . . . . .
H2O H 0.592(3) 0.191(3) 0.569(3) 0.101(14) 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
O2A C16A 1.368(3) . ?
O2A H2O 0.99(4) . ?
O1 C10 1.311(3) . ?
O2 C16 1.310(3) . ?
O1A C10A 1.352(3) . ?
O1A H1O 1.00(4) . ?
N1A N2A 1.333(3) . ?
N1A C1A 1.348(3) . ?
N1A C11A 1.439(3) . ?
N1 N2 1.337(3) . ?
N1 C1 1.338(3) . ?
N1 C11 1.435(3) . ?
N3A N2A 1.317(3) . ?
N3A C2A 1.367(3) . ?
N3A C61A 1.464(3) . ?
N2 N3 1.327(3) . ?
N3 C2 1.368(3) . ?
N3 C61 1.465(3) . ?
C16A C11A 1.382(4) . ?
C16A C15A 1.412(3) . ?
C11A C12A 1.386(3) . ?
C2 C1 1.378(4) . ?
C2 C5 1.457(3) . ?
C2A C1A 1.371(4) . ?
C2A C5A 1.460(3) . ?
C16 C11 1.403(4) . ?
C16 C15 1.429(4) . ?
C1 H1 0.9300 . ?
C13A C12A 1.388(3) . ?
C13A C14A 1.393(4) . ?
C13A C25A 1.532(4) . ?
C7 C6 1.375(4) . ?
C7 C8 1.398(4) . ?
C7 C17 1.540(4) . ?
C11 C12 1.388(3) . ?
C10 C9 1.424(4) . ?
C10 C5 1.424(4) . ?
C6A C7A 1.375(4) . ?
C6A C5A 1.394(4) . ?
C6A H6A 0.9300 . ?
C5 C6 1.396(3) . ?
C9 C8 1.387(4) . ?
C9 C21 1.540(4) . ?
C1A H1A 0.9300 . ?
C14A C15A 1.393(4) . ?
C14A H14A 0.9300 . ?
C5A C10A 1.400(4) . ?
C6 H6 0.9300 . ?
C12A H12A 0.9300 . ?
C15 C14 1.392(4) . ?
C15 C29 1.536(4) . ?
C10A C9A 1.413(4) . ?
C15A C29A 1.530(4) . ?
C12 C13 1.375(4) . ?
C12 H12 0.9300 . ?
C8 H8 0.9300 . ?
C29A C31A 1.526(4) . ?
C29A C32A 1.533(4) . ?
C29A C30A 1.542(4) . ?
C7A C8A 1.403(4) . ?
C7A C17A 1.528(4) . ?
C17 C20 1.508(4) . ?
C17 C19 1.526(4) . ?
C17 C18 1.534(4) . ?
C9A C8A 1.380(4) . ?
C9A C21A 1.538(4) . ?
C13 C14 1.394(4) . ?
C13 C25 1.528(4) . ?
C25A C26A 1.530(4) . ?
C25A C28A 1.530(4) . ?
C25A C27A 1.539(4) . ?
C29 C32 1.526(4) . ?
C29 C30 1.529(4) . ?
C29 C31 1.540(4) . ?
C21 C23 1.530(4) . ?
C21 C22 1.534(4) . ?
C21 C24 1.536(4) . ?
C8A H8A 0.9300 . ?
C14 H14 0.9300 . ?
C17A C19A 1.522(4) . ?
C17A C20A 1.523(4) . ?
C17A C18A 1.529(4) . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C32A H32A 0.9600 . ?
C32A H32B 0.9600 . ?
C32A H32C 0.9600 . ?
C30A H30A 0.9600 . ?
C30A H30B 0.9600 . ?
C30A H30C 0.9600 . ?
C61A H61D 0.9600 . ?
C61A H61E 0.9600 . ?
C61A H61F 0.9600 . ?
C21A C22A 1.529(5) . ?
C21A C23A 1.531(4) . ?
C21A C24A 1.541(4) . ?
C30 H30D 0.9600 . ?
C30 H30E 0.9600 . ?
C30 H30F 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C31A H31D 0.9600 . ?
C31A H31E 0.9600 . ?
C31A H31F 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C25 C26 1.504(5) . ?
C25 C28 1.532(5) . ?
C25 C27 1.536(5) . ?
C32 H32D 0.9600 . ?
C32 H32E 0.9600 . ?
C32 H32F 0.9600 . ?
C26A H26A 0.9600 . ?
C26A H26B 0.9600 . ?
C26A H26C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C28A H28A 0.9600 . ?
C28A H28B 0.9600 . ?
C28A H28C 0.9600 . ?
C27A H27A 0.9600 . ?
C27A H27B 0.9600 . ?
C27A H27C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C23A H23D 0.9600 . ?
C23A H23E 0.9600 . ?
C23A H23F 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20A H20D 0.9600 . ?
C20A H20E 0.9600 . ?
C20A H20F 0.9600 . ?
C27 H27D 0.9600 . ?
C27 H27E 0.9600 . ?
C27 H27F 0.9600 . ?
C22A H22D 0.9600 . ?
C22A H22E 0.9600 . ?
C22A H22F 0.9600 . ?
C24A H24D 0.9600 . ?
C24A H24E 0.9600 . ?
C24A H24F 0.9600 . ?
C28 H28D 0.9600 . ?
C28 H28E 0.9600 . ?
C28 H28F 0.9600 . ?
C18A H18D 0.9600 . ?
C18A H18E 0.9600 . ?
C18A H18F 0.9600 . ?
C26 H26D 0.9600 . ?
C26 H26E 0.9600 . ?
C26 H26F 0.9600 . ?
C19A H19D 0.9600 . ?
C19A H19E 0.9600 . ?
C19A H19F 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
C16A O2A H2O 108(2) . . ?
C10A O1A H1O 124(2) . . ?
N2A N1A C1A 112.8(2) . . ?
N2A N1A C11A 118.2(2) . . ?
C1A N1A C11A 128.5(2) . . ?
N2 N1 C1 112.4(2) . . ?
N2 N1 C11 119.3(2) . . ?
C1 N1 C11 128.2(2) . . ?
N2A N3A C2A 113.5(2) . . ?
N2A N3A C61A 119.1(2) . . ?
C2A N3A C61A 127.4(2) . . ?
N3A N2A N1A 103.39(19) . . ?
N3 N2 N1 103.45(19) . . ?
N2 N3 C2 113.6(2) . . ?
N2 N3 C61 116.8(2) . . ?
C2 N3 C61 129.6(2) . . ?
O2A C16A C11A 119.7(2) . . ?
O2A C16A C15A 122.2(2) . . ?
C11A C16A C15A 118.1(2) . . ?
C16A C11A C12A 124.1(2) . . ?
C16A C11A N1A 118.8(2) . . ?
C12A C11A N1A 117.1(2) . . ?
N3 C2 C1 103.5(2) . . ?
N3 C2 C5 128.0(2) . . ?
C1 C2 C5 128.5(2) . . ?
N3A C2A C1A 104.2(2) . . ?
N3A C2A C5A 124.5(2) . . ?
C1A C2A C5A 131.2(2) . . ?
O2 C16 C11 120.7(2) . . ?
O2 C16 C15 124.4(2) . . ?
C11 C16 C15 114.8(2) . . ?
N1 C1 C2 107.2(2) . . ?
N1 C1 H1 126.4 . . ?
C2 C1 H1 126.4 . . ?
C12A C13A C14A 117.1(2) . . ?
C12A C13A C25A 122.0(2) . . ?
C14A C13A C25A 120.8(2) . . ?
C6 C7 C8 116.5(2) . . ?
C6 C7 C17 120.3(2) . . ?
C8 C7 C17 123.2(2) . . ?
C12 C11 C16 125.4(2) . . ?
C12 C11 N1 117.8(2) . . ?
C16 C11 N1 116.7(2) . . ?
O1 C10 C9 124.3(2) . . ?
O1 C10 C5 119.5(2) . . ?
C9 C10 C5 116.2(2) . . ?
C7A C6A C5A 121.2(3) . . ?
C7A C6A H6A 119.4 . . ?
C5A C6A H6A 119.4 . . ?
C6 C5 C10 122.0(2) . . ?
C6 C5 C2 116.9(2) . . ?
C10 C5 C2 120.9(2) . . ?
C8 C9 C10 119.2(2) . . ?
C8 C9 C21 121.0(2) . . ?
C10 C9 C21 119.9(2) . . ?
N1A C1A C2A 106.0(2) . . ?
N1A C1A H1A 127.0 . . ?
C2A C1A H1A 127.0 . . ?
C15A C14A C13A 125.1(2) . . ?
C15A C14A H14A 117.4 . . ?
C13A C14A H14A 117.4 . . ?
C6A C5A C10A 121.3(2) . . ?
C6A C5A C2A 118.9(2) . . ?
C10A C5A C2A 119.7(2) . . ?
C7 C6 C5 121.6(2) . . ?
C7 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
C11A C12A C13A 118.6(2) . . ?
C11A C12A H12A 120.7 . . ?
C13A C12A H12A 120.7 . . ?
C14 C15 C16 118.5(2) . . ?
C14 C15 C29 121.5(2) . . ?
C16 C15 C29 120.0(2) . . ?
O1A C10A C5A 122.6(2) . . ?
O1A C10A C9A 118.6(2) . . ?
C5A C10A C9A 118.8(2) . . ?
C14A C15A C16A 116.4(2) . . ?
C14A C15A C29A 122.6(2) . . ?
C16A C15A C29A 120.9(2) . . ?
C13 C12 C11 119.6(2) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C9 C8 C7 124.4(2) . . ?
C9 C8 H8 117.8 . . ?
C7 C8 H8 117.8 . . ?
C31A C29A C15A 111.8(2) . . ?
C31A C29A C32A 108.2(2) . . ?
C15A C29A C32A 110.2(2) . . ?
C31A C29A C30A 107.2(2) . . ?
C15A C29A C30A 109.4(2) . . ?
C32A C29A C30A 110.0(2) . . ?
C6A C7A C8A 116.1(2) . . ?
C6A C7A C17A 123.4(2) . . ?
C8A C7A C17A 120.5(2) . . ?
C20 C17 C19 109.4(3) . . ?
C20 C17 C18 108.9(3) . . ?
C19 C17 C18 107.7(3) . . ?
C20 C17 C7 109.3(2) . . ?
C19 C17 C7 109.6(2) . . ?
C18 C17 C7 111.9(2) . . ?
C8A C9A C10A 117.0(2) . . ?
C8A C9A C21A 122.4(2) . . ?
C10A C9A C21A 120.5(2) . . ?
C12 C13 C14 116.5(2) . . ?
C12 C13 C25 122.4(3) . . ?
C14 C13 C25 121.1(3) . . ?
C26A C25A C28A 108.6(3) . . ?
C26A C25A C13A 110.2(2) . . ?
C28A C25A C13A 111.8(2) . . ?
C26A C25A C27A 109.2(2) . . ?
C28A C25A C27A 108.6(3) . . ?
C13A C25A C27A 108.5(2) . . ?
C32 C29 C30 107.7(2) . . ?
C32 C29 C15 112.7(2) . . ?
C30 C29 C15 109.3(2) . . ?
C32 C29 C31 107.6(2) . . ?
C30 C29 C31 110.8(2) . . ?
C15 C29 C31 108.7(2) . . ?
C23 C21 C22 110.4(2) . . ?
C23 C21 C24 107.4(2) . . ?
C22 C21 C24 107.6(2) . . ?
C23 C21 C9 109.7(2) . . ?
C22 C21 C9 109.1(2) . . ?
C24 C21 C9 112.6(2) . . ?
C9A C8A C7A 125.2(2) . . ?
C9A C8A H8A 117.4 . . ?
C7A C8A H8A 117.4 . . ?
C15 C14 C13 125.2(3) . . ?
C15 C14 H14 117.4 . . ?
C13 C14 H14 117.4 . . ?
C19A C17A C20A 108.4(3) . . ?
C19A C17A C7A 109.4(2) . . ?
C20A C17A C7A 112.5(2) . . ?
C19A C17A C18A 109.2(3) . . ?
C20A C17A C18A 107.8(3) . . ?
C7A C17A C18A 109.5(3) . . ?
N3 C61 H61A 109.5 . . ?
N3 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
N3 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C29A C32A H32A 109.5 . . ?
C29A C32A H32B 109.5 . . ?
H32A C32A H32B 109.5 . . ?
C29A C32A H32C 109.5 . . ?
H32A C32A H32C 109.5 . . ?
H32B C32A H32C 109.5 . . ?
C29A C30A H30A 109.5 . . ?
C29A C30A H30B 109.5 . . ?
H30A C30A H30B 109.5 . . ?
C29A C30A H30C 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
N3A C61A H61D 109.5 . . ?
N3A C61A H61E 109.5 . . ?
H61D C61A H61E 109.5 . . ?
N3A C61A H61F 109.5 . . ?
H61D C61A H61F 109.5 . . ?
H61E C61A H61F 109.5 . . ?
C22A C21A C23A 110.3(3) . . ?
C22A C21A C9A 110.0(3) . . ?
C23A C21A C9A 110.4(3) . . ?
C22A C21A C24A 107.4(3) . . ?
C23A C21A C24A 107.5(3) . . ?
C9A C21A C24A 111.2(3) . . ?
C29 C30 H30D 109.5 . . ?
C29 C30 H30E 109.5 . . ?
H30D C30 H30E 109.5 . . ?
C29 C30 H30F 109.5 . . ?
H30D C30 H30F 109.5 . . ?
H30E C30 H30F 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29A C31A H31D 109.5 . . ?
C29A C31A H31E 109.5 . . ?
H31D C31A H31E 109.5 . . ?
C29A C31A H31F 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C26 C25 C13 112.1(3) . . ?
C26 C25 C28 111.0(3) . . ?
C13 C25 C28 108.8(3) . . ?
C26 C25 C27 107.7(3) . . ?
C13 C25 C27 109.6(3) . . ?
C28 C25 C27 107.4(3) . . ?
C29 C32 H32D 109.5 . . ?
C29 C32 H32E 109.5 . . ?
H32D C32 H32E 109.5 . . ?
C29 C32 H32F 109.5 . . ?
H32D C32 H32F 109.5 . . ?
H32E C32 H32F 109.5 . . ?
C25A C26A H26A 109.5 . . ?
C25A C26A H26B 109.5 . . ?
H26A C26A H26B 109.5 . . ?
C25A C26A H26C 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25A C28A H28A 109.5 . . ?
C25A C28A H28B 109.5 . . ?
H28A C28A H28B 109.5 . . ?
C25A C28A H28C 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
C25A C27A H27A 109.5 . . ?
C25A C27A H27B 109.5 . . ?
H27A C27A H27B 109.5 . . ?
C25A C27A H27C 109.5 . . ?
H27A C27A H27C 109.5 . . ?
H27B C27A H27C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21A C23A H23D 109.5 . . ?
C21A C23A H23E 109.5 . . ?
H23D C23A H23E 109.5 . . ?
C21A C23A H23F 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17A C20A H20D 109.5 . . ?
C17A C20A H20E 109.5 . . ?
H20D C20A H20E 109.5 . . ?
C17A C20A H20F 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C25 C27 H27D 109.5 . . ?
C25 C27 H27E 109.5 . . ?
H27D C27 H27E 109.5 . . ?
C25 C27 H27F 109.5 . . ?
H27D C27 H27F 109.5 . . ?
H27E C27 H27F 109.5 . . ?
C21A C22A H22D 109.5 . . ?
C21A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C21A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
C21A C24A H24D 109.5 . . ?
C21A C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
C21A C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C25 C28 H28D 109.5 . . ?
C25 C28 H28E 109.5 . . ?
H28D C28 H28E 109.5 . . ?
C25 C28 H28F 109.5 . . ?
H28D C28 H28F 109.5 . . ?
H28E C28 H28F 109.5 . . ?
C17A C18A H18D 109.5 . . ?
C17A C18A H18E 109.5 . . ?
H18D C18A H18E 109.5 . . ?
C17A C18A H18F 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C25 C26 H26D 109.5 . . ?
C25 C26 H26E 109.5 . . ?
H26D C26 H26E 109.5 . . ?
C25 C26 H26F 109.5 . . ?
H26D C26 H26F 109.5 . . ?
H26E C26 H26F 109.5 . . ?
C17A C19A H19D 109.5 . . ?
C17A C19A H19E 109.5 . . ?
H19D C19A H19E 109.5 . . ?
C17A C19A H19F 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?

_refine_diff_density_max         0.514
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.048



####################################################################### 
# 
# 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_sh_0093m
_database_code_depnum_ccdc_archive 'CCDC 1921636'
loop_
_audit_author_name
_audit_author_address
'Stephan Hohloch'
;University of Paderborn
Germany
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-08-19 downloaded from the CCDC.
;
_audit_creation_date             2019-03-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C F3 O3 S, C31 H46 N3 O2, C3 H3'
_chemical_formula_sum            'C35 H49 F3 N3 O5 S'
_chemical_formula_weight         680.83
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   16.821(5)
_cell_length_b                   12.129(3)
_cell_length_c                   19.288(5)
_cell_angle_alpha                90
_cell_angle_beta                 111.467(5)
_cell_angle_gamma                90
_cell_volume                     3662.3(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3211
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      1.30
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0971 before and 0.0500 after correction.
The Ratio of minimum to maximum transmission is 0.9283.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   'Blessing, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1385
_diffrn_reflns_av_unetI/netI     0.1619
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19822
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.619
_diffrn_reflns_theta_min         1.301
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker Smart AXS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3211
_reflns_number_total             6767
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker ApexIII suite, 2019'
_computing_data_collection       'Bruker ApexIII suite, 2019'
_computing_data_reduction        'Bruker ApexIII suite, 2019'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.335
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6767
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.0941
_refine_ls_restrained_S_all      0.947
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1691P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2557
_refine_ls_wR_factor_ref         0.2904
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F10A) \\sim Ueq, Uanis(F10B) \\sim Ueq, Uanis(F11A) \\sim Ueq,
Uanis(F11B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: F10A(0.5) F11A(0.5) F10B(0.5) F11B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C12(H12), C1(H1), C6(H6), C202(H202), C200(H200), C201(H201)
4.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C22(H22A,H22B,
 H22C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C23(H23A,
 H23B,H23C), C28(H28A,H28B,H28C), C61(H61A,H61B,H61C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S100 S 0.50446(13) 0.49941(13) 0.64439(8) 0.0506(5) Uani 1 1 d . . . . .
O1 O 0.3589(2) 0.2795(3) 0.51405(19) 0.0340(9) Uani 1 1 d . . . . .
H1A H 0.400130 0.307153 0.546831 0.051 Uiso 1 1 calc GR . . . .
O101 O 0.5093(2) 0.3939(3) 0.61257(19) 0.0354(9) Uani 1 1 d . . . . .
O2 O 0.6573(2) 0.2793(3) 0.60834(19) 0.0344(9) Uani 1 1 d . . . . .
H2 H 0.615925 0.303478 0.616310 0.052 Uiso 1 1 calc GR . . . .
N2 N 0.5593(3) 0.2446(3) 0.7530(2) 0.0253(10) Uani 1 1 d . . . . .
N1 N 0.5818(2) 0.1891(3) 0.7038(2) 0.0221(9) Uani 1 1 d . . . . .
N3 N 0.4746(3) 0.2451(3) 0.7254(2) 0.0254(10) Uani 1 1 d . . . . .
C2 C 0.4426(3) 0.1891(4) 0.6594(2) 0.0177(10) Uani 1 1 d . . . . .
C11 C 0.6707(3) 0.1690(4) 0.7160(2) 0.0196(11) Uani 1 1 d . . . . .
C16 C 0.7039(3) 0.2116(4) 0.6661(2) 0.0195(11) Uani 1 1 d . . . . .
C14 C 0.8332(3) 0.1185(4) 0.7333(3) 0.0235(11) Uani 1 1 d . . . . .
H14 H 0.888922 0.100353 0.738909 0.028 Uiso 1 1 calc R . . . .
C10 C 0.3148(3) 0.2152(4) 0.5457(3) 0.0206(11) Uani 1 1 d . . . . .
C5 C 0.3518(3) 0.1718(4) 0.6165(3) 0.0217(11) Uani 1 1 d . . . . .
C7 C 0.2213(3) 0.0798(4) 0.6075(3) 0.0231(11) Uani 1 1 d . . . . .
C9 C 0.2290(3) 0.1901(4) 0.5021(3) 0.0216(11) Uani 1 1 d . . . . .
C8 C 0.1863(3) 0.1228(4) 0.5354(3) 0.0243(11) Uani 1 1 d . . . . .
H8 H 0.129887 0.104913 0.507345 0.029 Uiso 1 1 calc R . . . .
C12 C 0.7175(3) 0.1026(4) 0.7748(3) 0.0231(11) Uani 1 1 d . . . . .
H12 H 0.692711 0.075260 0.807239 0.028 Uiso 1 1 calc R . . . .
C13 C 0.8016(3) 0.0764(4) 0.7856(3) 0.0220(11) Uani 1 1 d . . . . .
C21 C 0.1845(3) 0.2362(4) 0.4224(3) 0.0274(12) Uani 1 1 d . . . . .
C1 C 0.5127(3) 0.1535(4) 0.6462(3) 0.0221(11) Uani 1 1 d . . . . .
H1 H 0.512906 0.112643 0.605507 0.027 Uiso 1 1 calc R . . . .
C25 C 0.8553(3) 0.0061(4) 0.8515(3) 0.0288(12) Uani 1 1 d . . . . .
C15 C 0.7876(3) 0.1856(4) 0.6734(3) 0.0228(11) Uani 1 1 d . . . . .
C29 C 0.8284(3) 0.2291(4) 0.6187(3) 0.0278(12) Uani 1 1 d . . . . .
C17 C 0.1714(3) 0.0079(4) 0.6425(3) 0.0288(12) Uani 1 1 d . . . . .
C6 C 0.3052(3) 0.1067(4) 0.6480(3) 0.0233(11) Uani 1 1 d . . . . .
H6 H 0.330942 0.081422 0.696644 0.028 Uiso 1 1 calc R . . . .
C202 C 0.4584(3) 0.0859(4) 0.4546(3) 0.0296(13) Uani 1 1 d . . . . .
H202 H 0.430025 0.143959 0.424077 0.036 Uiso 1 1 calc R . . . .
C200 C 0.5877(3) -0.0077(4) 0.5232(3) 0.0298(12) Uani 1 1 d . . . . .
H200 H 0.646880 -0.013214 0.539152 0.036 Uiso 1 1 calc R . . . .
C201 C 0.5460(3) 0.0777(4) 0.4775(3) 0.0284(12) Uani 1 1 d . . . . .
H201 H 0.576729 0.129791 0.462178 0.034 Uiso 1 1 calc R . . . .
C31 C 0.8316(4) 0.3570(4) 0.6225(3) 0.0406(15) Uani 1 1 d . . . . .
H31A H 0.774674 0.385494 0.609121 0.061 Uiso 1 1 calc GR . . . .
H31B H 0.856550 0.384698 0.588454 0.061 Uiso 1 1 calc GR . . . .
H31C H 0.865475 0.379857 0.672197 0.061 Uiso 1 1 calc GR . . . .
C27 C 0.8727(4) 0.0722(5) 0.9234(3) 0.0427(15) Uani 1 1 d . . . . .
H27A H 0.902154 0.139096 0.921300 0.064 Uiso 1 1 calc GR . . . .
H27B H 0.907245 0.029072 0.965372 0.064 Uiso 1 1 calc GR . . . .
H27C H 0.819462 0.089713 0.928636 0.064 Uiso 1 1 calc GR . . . .
O102 O 0.4923(5) 0.5124(4) 0.7078(3) 0.102(2) Uani 1 1 d . . . . .
C24 C 0.1824(4) 0.3638(4) 0.4257(3) 0.0403(15) Uani 1 1 d . . . . .
H24A H 0.151603 0.386185 0.456537 0.060 Uiso 1 1 calc GR . . . .
H24B H 0.154625 0.392639 0.376365 0.060 Uiso 1 1 calc GR . . . .
H24C H 0.239784 0.391576 0.446306 0.060 Uiso 1 1 calc GR . . . .
C22 C 0.0913(3) 0.1989(5) 0.3873(3) 0.0454(16) Uani 1 1 d . . . . .
H22A H 0.088966 0.119872 0.384527 0.068 Uiso 1 1 calc GR . . . .
H22B H 0.066100 0.229248 0.338105 0.068 Uiso 1 1 calc GR . . . .
H22C H 0.060261 0.224189 0.417316 0.068 Uiso 1 1 calc GR . . . .
C26 C 0.8071(4) -0.1000(4) 0.8553(3) 0.0415(15) Uani 1 1 d . . . . .
H26A H 0.755140 -0.081403 0.862408 0.062 Uiso 1 1 calc GR . . . .
H26B H 0.842219 -0.144529 0.896161 0.062 Uiso 1 1 calc GR . . . .
H26C H 0.793833 -0.140375 0.809607 0.062 Uiso 1 1 calc GR . . . .
C30 C 0.9202(3) 0.1869(5) 0.6378(3) 0.0417(15) Uani 1 1 d . . . . .
H30A H 0.955108 0.210705 0.686983 0.063 Uiso 1 1 calc GR . . . .
H30B H 0.942903 0.215765 0.602481 0.063 Uiso 1 1 calc GR . . . .
H30C H 0.919947 0.107774 0.635738 0.063 Uiso 1 1 calc GR . . . .
C32 C 0.7764(4) 0.1916(5) 0.5398(3) 0.0416(15) Uani 1 1 d . . . . .
H32A H 0.770540 0.112834 0.538904 0.062 Uiso 1 1 calc GR . . . .
H32B H 0.804957 0.213284 0.507046 0.062 Uiso 1 1 calc GR . . . .
H32C H 0.720846 0.225041 0.523689 0.062 Uiso 1 1 calc GR . . . .
C23 C 0.2290(4) 0.1978(5) 0.3706(3) 0.0417(15) Uani 1 1 d . . . . .
H23A H 0.286906 0.223749 0.388961 0.062 Uiso 1 1 calc GR . . . .
H23B H 0.199418 0.226704 0.321532 0.062 Uiso 1 1 calc GR . . . .
H23C H 0.228617 0.118684 0.368669 0.062 Uiso 1 1 calc GR . . . .
C28 C 0.9408(3) -0.0280(6) 0.8476(3) 0.0486(17) Uani 1 1 d . . . . .
H28A H 0.931029 -0.070548 0.803294 0.073 Uiso 1 1 calc GR . . . .
H28B H 0.971893 -0.071530 0.890534 0.073 Uiso 1 1 calc GR . . . .
H28C H 0.973177 0.036702 0.846531 0.073 Uiso 1 1 calc GR . . . .
C61 C 0.4319(4) 0.2988(5) 0.7682(3) 0.0461(16) Uani 1 1 d . . . . .
H61A H 0.415889 0.244994 0.797194 0.069 Uiso 1 1 calc GR . . . .
H61B H 0.381625 0.335315 0.735204 0.069 Uiso 1 1 calc GR . . . .
H61C H 0.469497 0.352029 0.800791 0.069 Uiso 1 1 calc GR . . . .
C18 C 0.1606(4) 0.0717(5) 0.7064(4) 0.0541(18) Uani 1 1 d . . . . .
H18A H 0.215701 0.093592 0.741052 0.081 Uiso 1 1 calc GR . . . .
H18B H 0.133025 0.025666 0.731372 0.081 Uiso 1 1 calc GR . . . .
H18C H 0.126378 0.135983 0.687247 0.081 Uiso 1 1 calc GR . . . .
C19 C 0.2219(4) -0.0976(5) 0.6730(4) 0.0538(18) Uani 1 1 d . . . . .
H19A H 0.230876 -0.136656 0.633192 0.081 Uiso 1 1 calc GR . . . .
H19B H 0.190335 -0.143396 0.694451 0.081 Uiso 1 1 calc GR . . . .
H19C H 0.276054 -0.079053 0.710454 0.081 Uiso 1 1 calc GR . . . .
C20 C 0.0846(4) -0.0255(6) 0.5875(3) 0.0573(19) Uani 1 1 d . . . . .
H20A H 0.052260 0.039321 0.565949 0.086 Uiso 1 1 calc GR . . . .
H20B H 0.054901 -0.067242 0.612735 0.086 Uiso 1 1 calc GR . . . .
H20C H 0.091629 -0.069764 0.548861 0.086 Uiso 1 1 calc GR . . . .
O100 O 0.5849(4) 0.5667(6) 0.6516(6) 0.163(4) Uani 1 1 d . . . . .
C100 C 0.4352(7) 0.5768(6) 0.5704(5) 0.099(3) Uani 1 1 d . . . . .
F100 F 0.4171(3) 0.6757(3) 0.5892(2) 0.0773(13) Uani 1 1 d . . . . .
F10A F 0.4909(8) 0.6105(7) 0.5312(5) 0.108(4) Uani 0.5 1 d . U P A 1
F11A F 0.4040(17) 0.479(2) 0.6300(16) 0.299(11) Uani 0.5 1 d . U P A 1
F10B F 0.4112(5) 0.5493(6) 0.5047(4) 0.0523(19) Uani 0.5 1 d . U P A 2
F11B F 0.3516(6) 0.5263(8) 0.5621(5) 0.080(3) Uani 0.5 1 d . U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S100 O101 1.434(4) . ?
S100 O102 1.321(5) . ?
S100 O100 1.542(7) . ?
S100 C100 1.749(9) . ?
S100 F11A 1.63(3) . ?
O1 H1A 0.8200 . ?
O1 C10 1.365(6) . ?
O2 H2 0.8200 . ?
O2 C16 1.374(5) . ?
N2 N1 1.326(5) . ?
N2 N3 1.325(6) . ?
N1 C11 1.447(6) . ?
N1 C1 1.352(6) . ?
N3 C2 1.367(6) . ?
N3 C61 1.434(7) . ?
C2 C5 1.462(6) . ?
C2 C1 1.364(6) . ?
C11 C16 1.379(6) . ?
C11 C12 1.378(6) . ?
C16 C15 1.399(7) . ?
C14 H14 0.9300 . ?
C14 C13 1.398(7) . ?
C14 C15 1.390(7) . ?
C10 C5 1.381(6) . ?
C10 C9 1.412(6) . ?
C5 C6 1.398(7) . ?
C7 C8 1.398(6) . ?
C7 C17 1.528(7) . ?
C7 C6 1.378(6) . ?
C9 C8 1.390(6) . ?
C9 C21 1.547(6) . ?
C8 H8 0.9300 . ?
C12 H12 0.9300 . ?
C12 C13 1.390(7) . ?
C13 C25 1.523(7) . ?
C21 C24 1.550(7) . ?
C21 C22 1.532(7) . ?
C21 C23 1.524(7) . ?
C1 H1 0.9300 . ?
C25 C27 1.535(7) . ?
C25 C26 1.536(7) . ?
C25 C28 1.524(7) . ?
C15 C29 1.548(7) . ?
C29 C31 1.553(7) . ?
C29 C30 1.538(7) . ?
C29 C32 1.520(7) . ?
C17 C18 1.522(8) . ?
C17 C19 1.529(8) . ?
C17 C20 1.513(7) . ?
C6 H6 0.9300 . ?
C202 H202 0.9300 . ?
C202 C200 1.388(7) 3_656 ?
C202 C201 1.379(7) . ?
C200 H200 0.9300 . ?
C200 C201 1.375(7) . ?
C201 H201 0.9300 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
O102 F11A 1.73(3) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C100 F100 1.321(7) . ?
C100 F10A 1.461(13) . ?
C100 F11A 1.86(3) . ?
C100 F10B 1.226(10) . ?
C100 F11B 1.488(13) . ?
F10B F11B 1.766(12) . ?

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
O101 S100 O100 109.1(3) . . ?
O101 S100 C100 104.7(3) . . ?
O101 S100 F11A 90.4(10) . . ?
O102 S100 O101 123.7(3) . . ?
O102 S100 O100 106.3(5) . . ?
O102 S100 C100 114.2(4) . . ?
O102 S100 F11A 70.9(10) . . ?
O100 S100 C100 95.1(5) . . ?
O100 S100 F11A 156.7(11) . . ?
F11A S100 C100 66.7(11) . . ?
C10 O1 H1A 109.5 . . ?
C16 O2 H2 109.5 . . ?
N3 N2 N1 105.2(4) . . ?
N2 N1 C11 121.2(4) . . ?
N2 N1 C1 111.4(4) . . ?
C1 N1 C11 127.4(4) . . ?
N2 N3 C2 111.8(4) . . ?
N2 N3 C61 117.5(4) . . ?
C2 N3 C61 130.7(4) . . ?
N3 C2 C5 124.9(4) . . ?
C1 C2 N3 104.9(4) . . ?
C1 C2 C5 130.1(4) . . ?
C16 C11 N1 118.8(4) . . ?
C12 C11 N1 118.5(4) . . ?
C12 C11 C16 122.6(4) . . ?
O2 C16 C11 122.3(4) . . ?
O2 C16 C15 118.1(4) . . ?
C11 C16 C15 119.6(4) . . ?
C13 C14 H14 117.5 . . ?
C15 C14 H14 117.5 . . ?
C15 C14 C13 125.0(5) . . ?
O1 C10 C5 122.6(4) . . ?
O1 C10 C9 117.4(4) . . ?
C5 C10 C9 119.9(4) . . ?
C10 C5 C2 120.3(4) . . ?
C10 C5 C6 121.6(4) . . ?
C6 C5 C2 118.1(4) . . ?
C8 C7 C17 123.6(4) . . ?
C6 C7 C8 116.5(5) . . ?
C6 C7 C17 119.9(4) . . ?
C10 C9 C21 122.1(4) . . ?
C8 C9 C10 116.1(4) . . ?
C8 C9 C21 121.8(4) . . ?
C7 C8 H8 117.3 . . ?
C9 C8 C7 125.3(4) . . ?
C9 C8 H8 117.3 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0(5) . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C25 122.8(4) . . ?
C12 C13 C14 116.3(4) . . ?
C12 C13 C25 120.8(4) . . ?
C9 C21 C24 109.3(4) . . ?
C22 C21 C9 112.2(4) . . ?
C22 C21 C24 106.2(4) . . ?
C23 C21 C9 111.4(4) . . ?
C23 C21 C24 110.9(4) . . ?
C23 C21 C22 106.8(5) . . ?
N1 C1 C2 106.8(4) . . ?
N1 C1 H1 126.6 . . ?
C2 C1 H1 126.6 . . ?
C13 C25 C27 108.7(4) . . ?
C13 C25 C26 110.3(4) . . ?
C13 C25 C28 113.1(4) . . ?
C27 C25 C26 108.9(4) . . ?
C28 C25 C27 108.4(4) . . ?
C28 C25 C26 107.4(5) . . ?
C16 C15 C29 122.4(4) . . ?
C14 C15 C16 116.4(4) . . ?
C14 C15 C29 121.2(4) . . ?
C15 C29 C31 108.9(4) . . ?
C30 C29 C15 112.3(4) . . ?
C30 C29 C31 107.9(4) . . ?
C32 C29 C15 110.1(4) . . ?
C32 C29 C31 110.1(4) . . ?
C32 C29 C30 107.4(4) . . ?
C7 C17 C19 109.3(4) . . ?
C18 C17 C7 108.4(4) . . ?
C18 C17 C19 109.2(5) . . ?
C20 C17 C7 112.8(4) . . ?
C20 C17 C18 109.5(5) . . ?
C20 C17 C19 107.6(5) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.5(4) . . ?
C7 C6 H6 119.7 . . ?
C200 C202 H202 119.8 3_656 . ?
C201 C202 H202 119.8 . . ?
C201 C202 C200 120.3(5) . 3_656 ?
C202 C200 H200 120.0 3_656 . ?
C201 C200 C202 120.0(5) . 3_656 ?
C201 C200 H200 120.0 . . ?
C202 C201 H201 120.2 . . ?
C200 C201 C202 119.6(5) . . ?
C200 C201 H201 120.2 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
S100 O102 F11A 62.8(9) . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C61 H61A 109.5 . . ?
N3 C61 H61B 109.5 . . ?
N3 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
S100 C100 F11A 53.5(9) . . ?
F100 C100 S100 114.5(6) . . ?
F100 C100 F10A 98.4(8) . . ?
F100 C100 F11A 105.3(11) . . ?
F100 C100 F11B 95.7(8) . . ?
F10A C100 S100 102.2(7) . . ?
F10A C100 F11A 151.5(11) . . ?
F10B C100 S100 124.5(6) . . ?
F10B C100 F100 120.6(8) . . ?
F10B C100 F11B 80.5(8) . . ?
F11B C100 S100 100.8(7) . . ?
S100 F11A O102 46.2(8) . . ?
S100 F11A C100 59.8(10) . . ?
O102 F11A C100 92.2(13) . . ?
C100 F10B F11B 56.2(7) . . ?
C100 F11B F10B 43.2(5) . . ?

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

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1921635'
loop_
_audit_author_name
_audit_author_address
'Stephan Hohloch'
;University of Paderborn
Germany
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H43 N3 O2'
_chemical_formula_weight         477.67

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'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                   26.760(5)
_cell_length_b                   10.170(2)
_cell_length_c                   11.170(2)
_cell_angle_alpha                90
_cell_angle_beta                 114.10(3)
_cell_angle_gamma                90
_cell_volume                     2774.9(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    1720
_cell_measurement_theta_min      1.66
_cell_measurement_theta_max      25.52

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_F_000             1040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.071
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart AXS'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6109
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.667
_diffrn_reflns_theta_max         25.528
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             2532
_reflns_number_gt                1720
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Apex3 suite, 2019'
_computing_cell_refinement       'Bruker Apex3 suite, 2019'
_computing_data_reduction        'Bruker Apex3 suite, 2019'
_computing_structure_solution    WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0601P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    refU
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2532
_refine_ls_number_parameters     188
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0535
_refine_ls_wR_factor_ref         0.1273
_refine_ls_wR_factor_gt          0.1164
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.40477(6) 0.32436(12) 0.34785(14) 0.0320(4) Uani 1 1 d . . . . .
H1 H 0.4285 0.3150 0.3200 0.051(8) Uiso 1 1 calc R . . . .
C6 C 0.43333(8) 0.67935(18) 0.39614(19) 0.0227(5) Uani 1 1 d . . . . .
H6 H 0.4572 0.7408 0.3867 0.014(5) Uiso 1 1 calc R . . . .
C5 C 0.43638(8) 0.54919(18) 0.36099(19) 0.0200(5) Uani 1 1 d . . . . .
C7 C 0.39623(8) 0.71960(18) 0.44412(19) 0.0220(5) Uani 1 1 d . . . . .
C9 C 0.36368(8) 0.49126(18) 0.4272(2) 0.0226(5) Uani 1 1 d . . . . .
C10 C 0.40216(8) 0.45419(18) 0.3787(2) 0.0229(5) Uani 1 1 d . . . . .
C17 C 0.39199(9) 0.86543(18) 0.4749(2) 0.0240(5) Uani 1 1 d . . . . .
C8 C 0.36207(8) 0.62353(18) 0.45843(19) 0.0235(5) Uani 1 1 d . . . . .
H8 H 0.3366 0.6491 0.4908 0.024(5) Uiso 1 1 calc R . . . .
C1 C 0.5000 0.5956(3) 0.2500 0.0274(7) Uani 1 2 d S T P . .
C21 C 0.32381(9) 0.39011(19) 0.4421(2) 0.0267(5) Uani 1 1 d . . . . .
C18 C 0.37706(10) 0.9455(2) 0.3486(2) 0.0349(6) Uani 1 1 d . . . . .
H18A H 0.4052 0.9353 0.3168 0.048(7) Uiso 1 1 calc R . . . .
H18B H 0.3738 1.0367 0.3665 0.045(7) Uiso 1 1 calc R . . . .
H18C H 0.3429 0.9147 0.2835 0.065(9) Uiso 1 1 calc R . . . .
C19 C 0.34874(9) 0.8889(2) 0.5281(2) 0.0315(6) Uani 1 1 d . . . . .
H19A H 0.3136 0.8630 0.4635 0.027(6) Uiso 1 1 calc R . . . .
H19B H 0.3480 0.9806 0.5479 0.039(6) Uiso 1 1 calc R . . . .
H19C H 0.3574 0.8380 0.6064 0.035(6) Uiso 1 1 calc R . . . .
C22 C 0.35486(9) 0.2824(2) 0.5387(2) 0.0325(6) Uani 1 1 d . . . . .
H22A H 0.3750 0.3204 0.6235 0.040(7) Uiso 1 1 calc R . . . .
H22B H 0.3798 0.2400 0.5089 0.056(8) Uiso 1 1 calc R . . . .
H22C H 0.3294 0.2189 0.5444 0.038(6) Uiso 1 1 calc R . . . .
C20 C 0.44701(9) 0.9132(2) 0.5782(2) 0.0354(6) Uani 1 1 d . . . . .
H20A H 0.4559 0.8645 0.6579 0.049(7) Uiso 1 1 calc R . . . .
H20B H 0.4445 1.0051 0.5949 0.036(6) Uiso 1 1 calc R . . . .
H20C H 0.4750 0.9001 0.5465 0.038(7) Uiso 1 1 calc R . . . .
C24 C 0.28831(9) 0.3311(2) 0.3077(2) 0.0365(6) Uani 1 1 d . . . . .
H24A H 0.3112 0.2846 0.2744 0.052(7) Uiso 1 1 calc R . . . .
H24B H 0.2693 0.4003 0.2480 0.048(7) Uiso 1 1 calc R . . . .
H24C H 0.2622 0.2714 0.3164 0.057(8) Uiso 1 1 calc R . . . .
C23 C 0.28550(10) 0.4549(2) 0.4949(3) 0.0423(7) Uani 1 1 d . . . . .
H23A H 0.2608 0.3902 0.5025 0.058(8) Uiso 1 1 calc R . . . .
H23B H 0.2649 0.5230 0.4358 0.064(9) Uiso 1 1 calc R . . . .
H23C H 0.3066 0.4923 0.5795 0.047(8) Uiso 1 1 calc R . . . .
N2 N 0.48366(7) 0.39027(15) 0.28032(18) 0.0301(5) Uani 1 1 d . . . . .
N1 N 0.47273(7) 0.51586(16) 0.29967(17) 0.0202(4) Uani 0.5 1 d . . P . .
C2 C 0.47273(7) 0.51586(16) 0.29967(17) 0.0202(4) Uani 0.5 1 d . . P . .
H1A H 0.5000 0.685(3) 0.2500 0.039(9) Uiso 1 2 d S . P . .


_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 C10 1.374(2) . ?
O1 H1 0.8200 . ?
C6 C7 1.369(3) . ?
C6 C5 1.393(3) . ?
C6 H6 0.9300 . ?
C5 C10 1.400(3) . ?
C5 N1 1.440(3) . ?
C7 C8 1.391(3) . ?
C7 C17 1.537(3) . ?
C9 C8 1.395(3) . ?
C9 C10 1.397(3) . ?
C9 C21 1.539(3) . ?
C17 C19 1.520(3) . ?
C17 C20 1.532(3) . ?
C17 C18 1.534(3) . ?
C8 H8 0.9300 . ?
C1 N1 1.352(2) . ?
C1 C2 1.352(2) 2_655 ?
C1 N1 1.352(2) 2_655 ?
C1 H1A 0.91(3) . ?
C21 C22 1.524(3) . ?
C21 C23 1.525(3) . ?
C21 C24 1.534(3) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
N2 N2 1.306(3) 2_655 ?
N2 N1 1.347(2) . ?

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
C10 O1 H1 109.5 . . ?
C7 C6 C5 122.00(18) . . ?
C7 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C6 C5 C10 119.95(18) . . ?
C6 C5 N1 119.12(17) . . ?
C10 C5 N1 120.83(17) . . ?
C6 C7 C8 116.78(18) . . ?
C6 C7 C17 120.50(17) . . ?
C8 C7 C17 122.68(18) . . ?
C8 C9 C10 117.41(18) . . ?
C8 C9 C21 121.59(18) . . ?
C10 C9 C21 120.99(17) . . ?
O1 C10 C9 118.53(17) . . ?
O1 C10 C5 121.67(18) . . ?
C9 C10 C5 119.79(17) . . ?
C19 C17 C20 107.85(17) . . ?
C19 C17 C18 108.78(17) . . ?
C20 C17 C18 109.48(18) . . ?
C19 C17 C7 112.12(16) . . ?
C20 C17 C7 109.78(17) . . ?
C18 C17 C7 108.79(17) . . ?
C7 C8 C9 124.03(19) . . ?
C7 C8 H8 118.0 . . ?
C9 C8 H8 118.0 . . ?
N1 C1 C2 106.3 . 2_655 ?
N1 C1 N1 106.3(3) . 2_655 ?
C2 C1 N1 0.0 2_655 2_655 ?
N1 C1 H1A 126.86(13) . . ?
C2 C1 H1A 126.86(12) 2_655 . ?
N1 C1 H1A 126.86(12) 2_655 . ?
C22 C21 C23 107.17(18) . . ?
C22 C21 C24 110.64(17) . . ?
C23 C21 C24 107.59(19) . . ?
C22 C21 C9 110.81(17) . . ?
C23 C21 C9 110.98(17) . . ?
C24 C21 C9 109.58(17) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 N2 N1 108.55(10) 2_655 . ?
N2 N1 C1 108.31(18) . . ?
N2 N1 C5 122.17(16) . . ?
C1 N1 C5 129.51(17) . . ?

_refine_diff_density_max         0.221
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.042

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1921638'
loop_
_audit_author_name
_audit_author_address
'Stephan Hohloch'
;University of Paderborn
Germany
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H94 Cl2 N6 O6 Ti2'
_chemical_formula_weight         1234.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'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                   37.210(2)
_cell_length_b                   16.6867(8)
_cell_length_c                   27.0170(16)
_cell_angle_alpha                90
_cell_angle_beta                 108.543(5)
_cell_angle_gamma                90
_cell_volume                     15904.3(16)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9142
_cell_measurement_theta_min      2.06
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.031
_exptl_crystal_F_000             5264
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    0.312
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.963
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_measurement_method       'omega + phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42122
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.060
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             13941
_reflns_number_gt                9142
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Stoe X-Area suite, 2019'
_computing_cell_refinement       'Stoe X-Area suite, 2019'
_computing_data_reduction        'Stoe X-Area suite, 2019'
_computing_structure_solution    ShelXT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  WinGX
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1186P)²+60.0851P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13941
_refine_ls_number_parameters     765
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0780
_refine_ls_wR_factor_ref         0.2479
_refine_ls_wR_factor_gt          0.2160
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti2 Ti 0.30378(2) 0.30895(5) 0.28205(3) 0.0409(2) Uani 1 1 d . . . . .
Ti1 Ti 0.32754(2) 0.21306(5) 0.40644(3) 0.0415(2) Uani 1 1 d . . . . .
Cl2 Cl 0.29159(3) 0.22332(8) 0.20884(5) 0.0526(3) Uani 1 1 d . . . . .
Cl1 Cl 0.34839(6) 0.14419(11) 0.48754(6) 0.0819(5) Uani 1 1 d . . . . .
O1A O 0.25223(8) 0.33107(19) 0.27153(12) 0.0417(7) Uani 1 1 d . . . . .
O10 O 0.31873(8) 0.2478(2) 0.33638(12) 0.0439(8) Uani 1 1 d . . . . .
O2A O 0.34828(8) 0.3469(2) 0.27059(12) 0.0467(8) Uani 1 1 d . . . . .
O2 O 0.28327(9) 0.1543(2) 0.38884(13) 0.0486(8) Uani 1 1 d . . . . .
O1 O 0.36288(9) 0.2938(2) 0.43321(13) 0.0510(9) Uani 1 1 d . . . . .
O100 O 0.36453(10) 0.1270(2) 0.38471(13) 0.0570(9) Uani 1 1 d . . . . .
N3A N 0.29630(11) 0.5369(2) 0.35190(14) 0.0422(9) Uani 1 1 d . . . . .
N1A N 0.33710(10) 0.4766(2) 0.32855(14) 0.0425(9) Uani 1 1 d . . . . .
N2A N 0.33101(11) 0.5454(2) 0.35029(15) 0.0450(9) Uani 1 1 d . . . . .
N1 N 0.25543(12) 0.2850(3) 0.42676(15) 0.0502(10) Uani 1 1 d . . . . .
C2 C 0.30230(12) 0.3707(3) 0.45005(16) 0.0376(10) Uani 1 1 d . . . . .
C2A C 0.28015(13) 0.4647(3) 0.33230(17) 0.0418(11) Uani 1 1 d . . . . .
C9A C 0.18869(12) 0.3559(3) 0.26887(18) 0.0416(11) Uani 1 1 d . . . . .
N2 N 0.24385(16) 0.3465(3) 0.44976(17) 0.0666(14) Uani 1 1 d . . . . .
C13 C 0.17012(13) 0.1523(3) 0.38225(17) 0.0410(11) Uani 1 1 d . . . . .
C11 C 0.23115(12) 0.2169(3) 0.40643(17) 0.0390(10) Uani 1 1 d . . . . .
C12 C 0.19290(13) 0.2175(3) 0.40263(17) 0.0421(11) Uani 1 1 d . . . . .
H12 H 0.1827 0.2621 0.4139 0.051 Uiso 1 1 calc R U . . .
C16 C 0.24722(13) 0.1515(3) 0.38848(18) 0.0444(11) Uani 1 1 d . . . . .
C1A C 0.30767(12) 0.4243(3) 0.31722(17) 0.0411(11) Uani 1 1 d . . . . .
C8A C 0.16538(13) 0.3992(3) 0.28996(18) 0.0459(12) Uani 1 1 d . . . . .
H8A H 0.1397 0.3865 0.2788 0.055 Uiso 1 1 calc R U . . .
C1 C 0.29216(13) 0.2968(3) 0.42693(17) 0.0420(11) Uani 1 1 d . . . . .
C14 C 0.18741(13) 0.0853(3) 0.36761(18) 0.0439(11) Uani 1 1 d . . . . .
H14 H 0.1726 0.0400 0.3556 0.053 Uiso 1 1 calc R U . . .
C10A C 0.22799(13) 0.3744(3) 0.28799(17) 0.0423(11) Uani 1 1 d . . . . .
C5A C 0.24087(12) 0.4392(3) 0.32209(17) 0.0407(11) Uani 1 1 d . . . . .
C15 C 0.22501(14) 0.0828(3) 0.37004(19) 0.0462(11) Uani 1 1 d . . . . .
N3 N 0.27236(17) 0.3978(3) 0.46435(17) 0.0711(15) Uani 1 1 d . . . . .
C6 C 0.34337(15) 0.4911(3) 0.47845(18) 0.0488(12) Uani 1 1 d . . . . .
H6 H 0.3232 0.5190 0.4837 0.059 Uiso 1 1 calc R U . . .
C11A C 0.37154(13) 0.4688(3) 0.31541(17) 0.0455(12) Uani 1 1 d . . . . .
C6A C 0.21543(13) 0.4796(3) 0.34200(18) 0.0442(11) Uani 1 1 d . . . . .
H6A H 0.2245 0.5204 0.3662 0.053 Uiso 1 1 calc R U . . .
C21 C 0.43846(14) 0.3561(3) 0.46033(19) 0.0527(13) Uani 1 1 d . . . . .
C21A C 0.17336(13) 0.2914(3) 0.22702(19) 0.0460(12) Uani 1 1 d . . . . .
C9 C 0.40424(14) 0.4053(3) 0.46382(18) 0.0480(12) Uani 1 1 d . . . . .
C7 C 0.37810(14) 0.5280(3) 0.48912(18) 0.0481(12) Uani 1 1 d . . . . .
C5 C 0.33793(14) 0.4117(3) 0.45971(18) 0.0479(12) Uani 1 1 d . . . . .
C15A C 0.40660(13) 0.4015(4) 0.26666(19) 0.0579(15) Uani 1 1 d . . . . .
C16A C 0.37454(12) 0.4042(3) 0.28405(17) 0.0464(12) Uani 1 1 d . . . . .
C7A C 0.17734(13) 0.4607(3) 0.32678(19) 0.0466(12) Uani 1 1 d . . . . .
C10 C 0.36791(14) 0.3694(3) 0.45145(18) 0.0486(12) Uani 1 1 d . . . . .
C25 C 0.12690(13) 0.1544(3) 0.37255(18) 0.0458(11) Uani 1 1 d . . . . .
C8 C 0.40762(15) 0.4832(3) 0.48161(19) 0.0525(13) Uani 1 1 d . . . . .
H8 H 0.4312 0.5077 0.4891 0.063 Uiso 1 1 calc R U . . .
C12A C 0.40013(13) 0.5260(3) 0.33389(19) 0.0503(13) Uani 1 1 d . . . . .
H12A H 0.3974 0.5669 0.3558 0.060 Uiso 1 1 calc R U . . .
C23A C 0.18495(14) 0.3101(3) 0.17831(19) 0.0524(13) Uani 1 1 d . . . . .
H23A H 0.1766 0.3631 0.1660 0.079 Uiso 1 1 calc R U . . .
H23B H 0.1735 0.2719 0.1514 0.079 Uiso 1 1 calc R U . . .
H23C H 0.2120 0.3072 0.1872 0.079 Uiso 1 1 calc R U . . .
C22A C 0.18885(14) 0.2090(3) 0.2489(2) 0.0512(12) Uani 1 1 d . . . . .
H22A H 0.2160 0.2098 0.2595 0.077 Uiso 1 1 calc R U . . .
H22B H 0.1794 0.1689 0.2225 0.077 Uiso 1 1 calc R U . . .
H22C H 0.1809 0.1968 0.2786 0.077 Uiso 1 1 calc R U . . .
C13A C 0.43240(14) 0.5216(4) 0.31953(19) 0.0546(14) Uani 1 1 d . . . . .
C29A C 0.41109(15) 0.3335(4) 0.2311(2) 0.0659(17) Uani 1 1 d . . . . .
C14A C 0.43422(14) 0.4605(4) 0.2852(2) 0.0641(17) Uani 1 1 d . . . . .
H14A H 0.4553 0.4590 0.2738 0.077 Uiso 1 1 calc R U . . .
C17 C 0.38529(16) 0.6146(3) 0.5097(2) 0.0588(14) Uani 1 1 d . . . . .
C29 C 0.24229(15) 0.0084(3) 0.3523(2) 0.0557(13) Uani 1 1 d . . . . .
C25A C 0.46546(14) 0.5806(4) 0.3396(2) 0.0640(17) Uani 1 1 d . . . . .
C31A C 0.37734(15) 0.3301(4) 0.1805(2) 0.0696(18) Uani 1 1 d . . . . .
H31A H 0.3546 0.3187 0.1887 0.104 Uiso 1 1 calc R U . . .
H31B H 0.3816 0.2887 0.1583 0.104 Uiso 1 1 calc R U . . .
H31C H 0.3748 0.3807 0.1628 0.104 Uiso 1 1 calc R U . . .
C24 C 0.47471(14) 0.4061(4) 0.4763(2) 0.0620(15) Uani 1 1 d . . . . .
H24A H 0.4716 0.4514 0.4534 0.093 Uiso 1 1 calc R U . . .
H24B H 0.4955 0.3739 0.4739 0.093 Uiso 1 1 calc R U . . .
H24C H 0.4799 0.4244 0.5115 0.093 Uiso 1 1 calc R U . . .
C61A C 0.28152(15) 0.6063(3) 0.3725(2) 0.0568(13) Uani 1 1 d . . . . .
H61A H 0.2999 0.6487 0.3799 0.085 Uiso 1 1 calc R U . . .
H61B H 0.2765 0.5914 0.4040 0.085 Uiso 1 1 calc R U . . .
H61C H 0.2585 0.6243 0.3471 0.085 Uiso 1 1 calc R U . . .
C23 C 0.44482(15) 0.2854(4) 0.4992(2) 0.0592(14) Uani 1 1 d . . . . .
H23D H 0.4508 0.3059 0.5341 0.089 Uiso 1 1 calc R U . . .
H23E H 0.4654 0.2529 0.4965 0.089 Uiso 1 1 calc R U . . .
H23F H 0.4222 0.2537 0.4911 0.089 Uiso 1 1 calc R U . . .
C30 C 0.27711(16) -0.0211(3) 0.3963(2) 0.0646(15) Uani 1 1 d . . . . .
H30A H 0.2956 0.0210 0.4060 0.097 Uiso 1 1 calc R U . . .
H30B H 0.2878 -0.0667 0.3844 0.097 Uiso 1 1 calc R U . . .
H30C H 0.2697 -0.0359 0.4259 0.097 Uiso 1 1 calc R U . . .
C17A C 0.14909(15) 0.5052(4) 0.3478(2) 0.0584(14) Uani 1 1 d . . . . .
C22 C 0.43260(15) 0.3251(4) 0.40436(19) 0.0589(14) Uani 1 1 d . . . . .
H22D H 0.4087 0.2978 0.3917 0.088 Uiso 1 1 calc R U . . .
H22E H 0.4527 0.2887 0.4048 0.088 Uiso 1 1 calc R U . . .
H22F H 0.4328 0.3695 0.3819 0.088 Uiso 1 1 calc R U . . .
C32 C 0.25298(17) 0.0294(4) 0.3033(2) 0.0646(15) Uani 1 1 d . . . . .
H32A H 0.2304 0.0417 0.2750 0.097 Uiso 1 1 calc R U . . .
H32B H 0.2656 -0.0154 0.2939 0.097 Uiso 1 1 calc R U . . .
H32C H 0.2696 0.0750 0.3104 0.097 Uiso 1 1 calc R U . . .
C20 C 0.41900(16) 0.6169(4) 0.5596(2) 0.0654(16) Uani 1 1 d . . . . .
H20A H 0.4133 0.5861 0.5862 0.098 Uiso 1 1 calc R U . . .
H20B H 0.4241 0.6714 0.5711 0.098 Uiso 1 1 calc R U . . .
H20C H 0.4409 0.5948 0.5530 0.098 Uiso 1 1 calc R U . . .
C26A C 0.46044(15) 0.6369(4) 0.3807(3) 0.0727(18) Uani 1 1 d . . . . .
H26A H 0.4388 0.6706 0.3655 0.109 Uiso 1 1 calc R U . . .
H26B H 0.4827 0.6695 0.3939 0.109 Uiso 1 1 calc R U . . .
H26C H 0.4566 0.6064 0.4087 0.109 Uiso 1 1 calc R U . . .
C24A C 0.12971(14) 0.2876(4) 0.2083(2) 0.0583(14) Uani 1 1 d . . . . .
H24D H 0.1210 0.2778 0.2376 0.087 Uiso 1 1 calc R U . . .
H24E H 0.1213 0.2450 0.1834 0.087 Uiso 1 1 calc R U . . .
H24F H 0.1196 0.3376 0.1923 0.087 Uiso 1 1 calc R U . . .
C18 C 0.35099(17) 0.6504(4) 0.5215(2) 0.0682(16) Uani 1 1 d . . . . .
H18A H 0.3299 0.6532 0.4899 0.102 Uiso 1 1 calc R U . . .
H18B H 0.3571 0.7033 0.5357 0.102 Uiso 1 1 calc R U . . .
H18C H 0.3445 0.6172 0.5464 0.102 Uiso 1 1 calc R U . . .
C31 C 0.21386(18) -0.0607(3) 0.3374(3) 0.0706(17) Uani 1 1 d . . . . .
H31D H 0.2063 -0.0752 0.3670 0.106 Uiso 1 1 calc R U . . .
H31E H 0.2255 -0.1060 0.3267 0.106 Uiso 1 1 calc R U . . .
H31F H 0.1920 -0.0442 0.3092 0.106 Uiso 1 1 calc R U . . .
C27A C 0.50244(15) 0.5336(4) 0.3640(2) 0.0711(18) Uani 1 1 d . . . . .
H27A H 0.5230 0.5705 0.3779 0.107 Uiso 1 1 calc R U . . .
H27B H 0.5076 0.5010 0.3378 0.107 Uiso 1 1 calc R U . . .
H27C H 0.4999 0.5000 0.3915 0.107 Uiso 1 1 calc R U . . .
C32A C 0.41506(18) 0.2540(5) 0.2606(3) 0.084(2) Uani 1 1 d . . . . .
H32D H 0.4349 0.2584 0.2935 0.126 Uiso 1 1 calc R U . . .
H32E H 0.4212 0.2121 0.2403 0.126 Uiso 1 1 calc R U . . .
H32F H 0.3916 0.2415 0.2666 0.126 Uiso 1 1 calc R U . . .
C19 C 0.3938(2) 0.6659(4) 0.4675(3) 0.083(2) Uani 1 1 d . . . . .
H19A H 0.4164 0.6464 0.4616 0.125 Uiso 1 1 calc R U . . .
H19B H 0.3975 0.7206 0.4788 0.125 Uiso 1 1 calc R U . . .
H19C H 0.3730 0.6626 0.4356 0.125 Uiso 1 1 calc R U . . .
C28A C 0.4687(2) 0.6339(5) 0.2942(3) 0.108(3) Uani 1 1 d . . . . .
H28A H 0.4451 0.6613 0.2785 0.162 Uiso 1 1 calc R U . . .
H28B H 0.4743 0.6010 0.2685 0.162 Uiso 1 1 calc R U . . .
H28C H 0.4885 0.6725 0.3075 0.162 Uiso 1 1 calc R U . . .
C20A C 0.1680(2) 0.5701(4) 0.3877(3) 0.091(2) Uani 1 1 d . . . . .
H20D H 0.1491 0.5971 0.3988 0.136 Uiso 1 1 calc R U . . .
H20E H 0.1805 0.6080 0.3719 0.136 Uiso 1 1 calc R U . . .
H20F H 0.1863 0.5458 0.4173 0.136 Uiso 1 1 calc R U . . .
C30A C 0.44698(18) 0.3441(6) 0.2151(3) 0.105(3) Uani 1 1 d . . . . .
H30D H 0.4471 0.3966 0.2007 0.157 Uiso 1 1 calc R U . . .
H30E H 0.4473 0.3045 0.1895 0.157 Uiso 1 1 calc R U . . .
H30F H 0.4690 0.3377 0.2453 0.157 Uiso 1 1 calc R U . . .
C18A C 0.1210(2) 0.5493(6) 0.3019(3) 0.120(3) Uani 1 1 d . . . . .
H18D H 0.1042 0.5112 0.2795 0.180 Uiso 1 1 calc R U . . .
H18E H 0.1346 0.5777 0.2827 0.180 Uiso 1 1 calc R U . . .
H18F H 0.1065 0.5866 0.3149 0.180 Uiso 1 1 calc R U . . .
C100 C 0.3999(2) 0.0950(6) 0.4190(3) 0.113(3) Uani 1 1 d . . . . .
H10A H 0.4181 0.1378 0.4314 0.136 Uiso 1 1 calc R U . . .
H10B H 0.3957 0.0695 0.4490 0.136 Uiso 1 1 calc R U . . .
C103 C 0.3577(2) 0.0972(5) 0.3325(3) 0.102(3) Uani 1 1 d . . . . .
H10C H 0.3607 0.1397 0.3097 0.122 Uiso 1 1 calc R U . . .
H10D H 0.3322 0.0758 0.3187 0.122 Uiso 1 1 calc R U . . .
C19A C 0.1280(3) 0.4482(5) 0.3715(4) 0.123(3) Uani 1 1 d . . . . .
H19D H 0.1156 0.4083 0.3462 0.185 Uiso 1 1 calc R U . . .
H19E H 0.1094 0.4771 0.3821 0.185 Uiso 1 1 calc R U . . .
H19F H 0.1455 0.4226 0.4013 0.185 Uiso 1 1 calc R U . . .
C26 C 0.1080(2) 0.1879(9) 0.3212(3) 0.164(6) Uani 1 1 d . . . . .
H26D H 0.0811 0.1879 0.3148 0.247 Uiso 1 1 calc R U . . .
H26E H 0.1138 0.1561 0.2952 0.247 Uiso 1 1 calc R U . . .
H26F H 0.1165 0.2419 0.3198 0.247 Uiso 1 1 calc R U . . .
C28 C 0.1172(2) 0.1992(7) 0.4143(3) 0.139(4) Uani 1 1 d . . . . .
H28D H 0.1218 0.2553 0.4113 0.208 Uiso 1 1 calc R U . . .
H28E H 0.1325 0.1801 0.4479 0.208 Uiso 1 1 calc R U . . .
H28F H 0.0909 0.1910 0.4105 0.208 Uiso 1 1 calc R U . . .
C27 C 0.1112(2) 0.0708(5) 0.3727(6) 0.180(6) Uani 1 1 d . . . . .
H27D H 0.0845 0.0738 0.3671 0.270 Uiso 1 1 calc R U . . .
H27E H 0.1235 0.0458 0.4058 0.270 Uiso 1 1 calc R U . . .
H27F H 0.1157 0.0397 0.3454 0.270 Uiso 1 1 calc R U . . .
C61 C 0.2610(3) 0.4588(6) 0.4939(4) 0.125(3) Uani 1 1 d . . . . .
H61D H 0.2586 0.5091 0.4759 0.187 Uiso 1 1 calc R U . . .
H61E H 0.2798 0.4636 0.5277 0.187 Uiso 1 1 calc R U . . .
H61F H 0.2371 0.4445 0.4979 0.187 Uiso 1 1 calc R U . . .
C102 C 0.3863(4) 0.0330(8) 0.3370(5) 0.196(7) Uani 1 1 d . . . . .
H10E H 0.3740 -0.0191 0.3313 0.235 Uiso 1 1 calc R U . . .
H10F H 0.3989 0.0407 0.3110 0.235 Uiso 1 1 calc R U . . .
C101 C 0.4141(6) 0.0371(13) 0.3901(8) 0.272(9) Uani 1 1 d . U . . .
H10G H 0.4168 -0.0150 0.4069 0.327 Uiso 1 1 calc R U . . .
H10H H 0.4387 0.0537 0.3884 0.327 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti2 O10 1.728(3) . ?
Ti2 O1A 1.884(3) . ?
Ti2 O2A 1.888(3) . ?
Ti2 C1A 2.130(5) . ?
Ti2 Cl2 2.3641(15) . ?
Ti1 O2 1.845(3) . ?
Ti1 O1 1.861(4) . ?
Ti1 O10 1.905(3) . ?
Ti1 C1 2.111(5) . ?
Ti1 O100 2.194(3) . ?
Ti1 Cl1 2.3756(17) . ?
O1A C10A 1.338(5) . ?
O2A C16A 1.331(6) . ?
O2 C16 1.339(5) . ?
O1 C10 1.344(6) . ?
O100 C103 1.439(7) . ?
O100 C100 1.449(8) . ?
N3A N2A 1.314(5) . ?
N3A C2A 1.375(6) . ?
N3A C61A 1.466(6) . ?
N1A N2A 1.341(6) . ?
N1A C1A 1.357(6) . ?
N1A C11A 1.441(6) . ?
N1 N2 1.340(6) . ?
N1 C1 1.380(6) . ?
N1 C11 1.446(6) . ?
C2 N3 1.367(6) . ?
C2 C1 1.379(6) . ?
C2 C5 1.441(7) . ?
C2A C1A 1.391(6) . ?
C2A C5A 1.462(6) . ?
C9A C8A 1.383(7) . ?
C9A C10A 1.421(6) . ?
C9A C21A 1.534(7) . ?
N2 N3 1.322(7) . ?
C13 C12 1.381(7) . ?
C13 C14 1.409(7) . ?
C13 C25 1.546(6) . ?
C11 C12 1.394(6) . ?
C11 C16 1.403(6) . ?
C12 H12 0.9300 . ?
C16 C15 1.409(7) . ?
C8A C7A 1.399(7) . ?
C8A H8A 0.9300 . ?
C14 C15 1.380(6) . ?
C14 H14 0.9300 . ?
C10A C5A 1.403(7) . ?
C5A C6A 1.401(6) . ?
C15 C29 1.542(7) . ?
N3 C61 1.439(10) . ?
C6 C7 1.377(7) . ?
C6 C5 1.410(7) . ?
C6 H6 0.9300 . ?
C11A C16A 1.397(7) . ?
C11A C12A 1.398(7) . ?
C6A C7A 1.381(6) . ?
C6A H6A 0.9300 . ?
C21 C24 1.527(7) . ?
C21 C9 1.543(7) . ?
C21 C23 1.546(8) . ?
C21 C22 1.547(7) . ?
C21A C22A 1.534(7) . ?
C21A C24A 1.541(6) . ?
C21A C23A 1.542(7) . ?
C9 C8 1.378(7) . ?
C9 C10 1.419(7) . ?
C7 C8 1.396(7) . ?
C7 C17 1.540(7) . ?
C5 C10 1.397(7) . ?
C15A C14A 1.397(8) . ?
C15A C16A 1.415(6) . ?
C15A C29A 1.528(8) . ?
C7A C17A 1.536(7) . ?
C25 C26 1.453(9) . ?
C25 C28 1.490(9) . ?
C25 C27 1.512(10) . ?
C8 H8 0.9300 . ?
C12A C13A 1.376(7) . ?
C12A H12A 0.9300 . ?
C23A H23A 0.9600 . ?
C23A H23B 0.9600 . ?
C23A H23C 0.9600 . ?
C22A H22A 0.9600 . ?
C22A H22B 0.9600 . ?
C22A H22C 0.9600 . ?
C13A C14A 1.395(8) . ?
C13A C25A 1.533(7) . ?
C29A C32A 1.532(10) . ?
C29A C31A 1.535(8) . ?
C29A C30A 1.539(7) . ?
C14A H14A 0.9300 . ?
C17 C20 1.523(8) . ?
C17 C18 1.533(8) . ?
C17 C19 1.538(8) . ?
C29 C31 1.529(8) . ?
C29 C30 1.534(8) . ?
C29 C32 1.539(7) . ?
C25A C26A 1.511(9) . ?
C25A C27A 1.538(8) . ?
C25A C28A 1.550(8) . ?
C31A H31A 0.9600 . ?
C31A H31B 0.9600 . ?
C31A H31C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C61A H61A 0.9600 . ?
C61A H61B 0.9600 . ?
C61A H61C 0.9600 . ?
C23 H23D 0.9600 . ?
C23 H23E 0.9600 . ?
C23 H23F 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C17A C19A 1.499(8) . ?
C17A C20A 1.531(9) . ?
C17A C18A 1.532(9) . ?
C22 H22D 0.9600 . ?
C22 H22E 0.9600 . ?
C22 H22F 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C26A H26A 0.9600 . ?
C26A H26B 0.9600 . ?
C26A H26C 0.9600 . ?
C24A H24D 0.9600 . ?
C24A H24E 0.9600 . ?
C24A H24F 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C31 H31D 0.9600 . ?
C31 H31E 0.9600 . ?
C31 H31F 0.9600 . ?
C27A H27A 0.9600 . ?
C27A H27B 0.9600 . ?
C27A H27C 0.9600 . ?
C32A H32D 0.9600 . ?
C32A H32E 0.9600 . ?
C32A H32F 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C28A H28A 0.9600 . ?
C28A H28B 0.9600 . ?
C28A H28C 0.9600 . ?
C20A H20D 0.9600 . ?
C20A H20E 0.9600 . ?
C20A H20F 0.9600 . ?
C30A H30D 0.9600 . ?
C30A H30E 0.9600 . ?
C30A H30F 0.9600 . ?
C18A H18D 0.9600 . ?
C18A H18E 0.9600 . ?
C18A H18F 0.9600 . ?
C100 C101 1.445(17) . ?
C100 H10A 0.9700 . ?
C100 H10B 0.9700 . ?
C103 C102 1.488(11) . ?
C103 H10C 0.9700 . ?
C103 H10D 0.9700 . ?
C19A H19D 0.9600 . ?
C19A H19E 0.9600 . ?
C19A H19F 0.9600 . ?
C26 H26D 0.9600 . ?
C26 H26E 0.9600 . ?
C26 H26F 0.9600 . ?
C28 H28D 0.9600 . ?
C28 H28E 0.9600 . ?
C28 H28F 0.9600 . ?
C27 H27D 0.9600 . ?
C27 H27E 0.9600 . ?
C27 H27F 0.9600 . ?
C61 H61D 0.9600 . ?
C61 H61E 0.9600 . ?
C61 H61F 0.9600 . ?
C102 C101 1.481(19) . ?
C102 H10E 0.9700 . ?
C102 H10F 0.9700 . ?
C101 H10G 0.9700 . ?
C101 H10H 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
O10 Ti2 O1A 106.32(14) . . ?
O10 Ti2 O2A 105.98(15) . . ?
O1A Ti2 O2A 144.43(15) . . ?
O10 Ti2 C1A 101.36(16) . . ?
O1A Ti2 C1A 79.16(15) . . ?
O2A Ti2 C1A 80.28(16) . . ?
O10 Ti2 Cl2 106.13(12) . . ?
O1A Ti2 Cl2 94.41(10) . . ?
O2A Ti2 Cl2 90.61(10) . . ?
C1A Ti2 Cl2 152.47(13) . . ?
O2 Ti1 O1 161.39(15) . . ?
O2 Ti1 O10 92.76(15) . . ?
O1 Ti1 O10 92.47(15) . . ?
O2 Ti1 C1 80.76(17) . . ?
O1 Ti1 C1 80.84(17) . . ?
O10 Ti1 C1 97.74(16) . . ?
O2 Ti1 O100 99.66(14) . . ?
O1 Ti1 O100 98.75(15) . . ?
O10 Ti1 O100 81.81(13) . . ?
C1 Ti1 O100 179.38(17) . . ?
O2 Ti1 Cl1 89.05(12) . . ?
O1 Ti1 Cl1 90.50(12) . . ?
O10 Ti1 Cl1 164.99(11) . . ?
C1 Ti1 Cl1 97.26(13) . . ?
O100 Ti1 Cl1 83.20(11) . . ?
C10A O1A Ti2 144.8(3) . . ?
Ti2 O10 Ti1 158.5(2) . . ?
C16A O2A Ti2 143.3(3) . . ?
C16 O2 Ti1 146.1(3) . . ?
C10 O1 Ti1 145.1(3) . . ?
C103 O100 C100 110.0(5) . . ?
C103 O100 Ti1 123.9(4) . . ?
C100 O100 Ti1 126.1(4) . . ?
N2A N3A C2A 113.3(4) . . ?
N2A N3A C61A 114.8(4) . . ?
C2A N3A C61A 131.9(4) . . ?
N2A N1A C1A 114.4(4) . . ?
N2A N1A C11A 118.2(4) . . ?
C1A N1A C11A 127.1(4) . . ?
N3A N2A N1A 103.1(4) . . ?
N2 N1 C1 110.7(5) . . ?
N2 N1 C11 121.6(4) . . ?
C1 N1 C11 127.8(4) . . ?
N3 C2 C1 107.1(5) . . ?
N3 C2 C5 125.3(5) . . ?
C1 C2 C5 127.6(4) . . ?
N3A C2A C1A 105.4(4) . . ?
N3A C2A C5A 128.0(4) . . ?
C1A C2A C5A 126.1(4) . . ?
C8A C9A C10A 116.4(4) . . ?
C8A C9A C21A 122.4(4) . . ?
C10A C9A C21A 121.2(4) . . ?
N3 N2 N1 106.8(5) . . ?
C12 C13 C14 117.4(4) . . ?
C12 C13 C25 121.6(4) . . ?
C14 C13 C25 120.9(4) . . ?
C12 C11 C16 121.2(4) . . ?
C12 C11 N1 121.5(4) . . ?
C16 C11 N1 117.3(4) . . ?
C13 C12 C11 120.4(4) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
O2 C16 C11 120.5(4) . . ?
O2 C16 C15 120.3(4) . . ?
C11 C16 C15 119.3(4) . . ?
N1A C1A C2A 103.8(4) . . ?
N1A C1A Ti2 128.1(3) . . ?
C2A C1A Ti2 128.1(3) . . ?
C9A C8A C7A 125.2(4) . . ?
C9A C8A H8A 117.4 . . ?
C7A C8A H8A 117.4 . . ?
C2 C1 N1 104.9(4) . . ?
C2 C1 Ti1 127.4(3) . . ?
N1 C1 Ti1 127.1(4) . . ?
C15 C14 C13 123.8(5) . . ?
C15 C14 H14 118.1 . . ?
C13 C14 H14 118.1 . . ?
O1A C10A C5A 120.6(4) . . ?
O1A C10A C9A 119.1(4) . . ?
C5A C10A C9A 120.2(4) . . ?
C6A C5A C10A 119.5(4) . . ?
C6A C5A C2A 123.0(4) . . ?
C10A C5A C2A 117.4(4) . . ?
C14 C15 C16 117.6(4) . . ?
C14 C15 C29 121.7(5) . . ?
C16 C15 C29 120.6(4) . . ?
N2 N3 C2 110.5(5) . . ?
N2 N3 C61 105.9(6) . . ?
C2 N3 C61 143.2(7) . . ?
C7 C6 C5 120.9(5) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C16A C11A C12A 123.0(4) . . ?
C16A C11A N1A 117.9(4) . . ?
C12A C11A N1A 119.1(5) . . ?
C7A C6A C5A 122.0(5) . . ?
C7A C6A H6A 119.0 . . ?
C5A C6A H6A 119.0 . . ?
C24 C21 C9 111.3(5) . . ?
C24 C21 C23 107.1(4) . . ?
C9 C21 C23 108.4(4) . . ?
C24 C21 C22 107.2(4) . . ?
C9 C21 C22 112.0(4) . . ?
C23 C21 C22 110.6(5) . . ?
C9A C21A C22A 109.8(4) . . ?
C9A C21A C24A 112.1(4) . . ?
C22A C21A C24A 108.5(4) . . ?
C9A C21A C23A 110.3(4) . . ?
C22A C21A C23A 109.8(4) . . ?
C24A C21A C23A 106.3(4) . . ?
C8 C9 C10 117.1(5) . . ?
C8 C9 C21 122.6(5) . . ?
C10 C9 C21 120.2(5) . . ?
C6 C7 C8 117.4(5) . . ?
C6 C7 C17 122.6(5) . . ?
C8 C7 C17 120.0(5) . . ?
C10 C5 C6 120.1(5) . . ?
C10 C5 C2 117.8(5) . . ?
C6 C5 C2 122.0(5) . . ?
C14A C15A C16A 117.4(5) . . ?
C14A C15A C29A 122.2(5) . . ?
C16A C15A C29A 120.3(5) . . ?
O2A C16A C11A 121.7(4) . . ?
O2A C16A C15A 120.6(5) . . ?
C11A C16A C15A 117.7(5) . . ?
C6A C7A C8A 116.3(4) . . ?
C6A C7A C17A 122.5(5) . . ?
C8A C7A C17A 121.2(4) . . ?
O1 C10 C5 120.5(4) . . ?
O1 C10 C9 119.6(5) . . ?
C5 C10 C9 119.9(5) . . ?
C26 C25 C28 111.6(7) . . ?
C26 C25 C27 106.7(8) . . ?
C28 C25 C27 105.9(7) . . ?
C26 C25 C13 109.4(4) . . ?
C28 C25 C13 111.9(5) . . ?
C27 C25 C13 111.2(5) . . ?
C9 C8 C7 124.6(5) . . ?
C9 C8 H8 117.7 . . ?
C7 C8 H8 117.7 . . ?
C13A C12A C11A 119.7(5) . . ?
C13A C12A H12A 120.1 . . ?
C11A C12A H12A 120.1 . . ?
C21A C23A H23A 109.5 . . ?
C21A C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
C21A C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C21A C22A H22A 109.5 . . ?
C21A C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C21A C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C12A C13A C14A 117.2(5) . . ?
C12A C13A C25A 122.7(6) . . ?
C14A C13A C25A 120.1(5) . . ?
C15A C29A C32A 109.1(5) . . ?
C15A C29A C31A 111.4(5) . . ?
C32A C29A C31A 110.3(5) . . ?
C15A C29A C30A 111.7(5) . . ?
C32A C29A C30A 107.3(6) . . ?
C31A C29A C30A 107.0(5) . . ?
C13A C14A C15A 124.6(5) . . ?
C13A C14A H14A 117.7 . . ?
C15A C14A H14A 117.7 . . ?
C20 C17 C18 108.1(5) . . ?
C20 C17 C19 109.7(5) . . ?
C18 C17 C19 108.7(5) . . ?
C20 C17 C7 110.1(5) . . ?
C18 C17 C7 112.4(4) . . ?
C19 C17 C7 107.9(5) . . ?
C31 C29 C30 107.8(5) . . ?
C31 C29 C32 107.0(5) . . ?
C30 C29 C32 110.7(5) . . ?
C31 C29 C15 111.5(4) . . ?
C30 C29 C15 110.5(4) . . ?
C32 C29 C15 109.4(4) . . ?
C26A C25A C13A 112.7(5) . . ?
C26A C25A C27A 107.7(4) . . ?
C13A C25A C27A 109.4(5) . . ?
C26A C25A C28A 106.4(6) . . ?
C13A C25A C28A 110.1(4) . . ?
C27A C25A C28A 110.4(5) . . ?
C29A C31A H31A 109.5 . . ?
C29A C31A H31B 109.5 . . ?
H31A C31A H31B 109.5 . . ?
C29A C31A H31C 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3A C61A H61A 109.5 . . ?
N3A C61A H61B 109.5 . . ?
H61A C61A H61B 109.5 . . ?
N3A C61A H61C 109.5 . . ?
H61A C61A H61C 109.5 . . ?
H61B C61A H61C 109.5 . . ?
C21 C23 H23D 109.5 . . ?
C21 C23 H23E 109.5 . . ?
H23D C23 H23E 109.5 . . ?
C21 C23 H23F 109.5 . . ?
H23D C23 H23F 109.5 . . ?
H23E C23 H23F 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C19A C17A C20A 109.6(6) . . ?
C19A C17A C18A 109.5(7) . . ?
C20A C17A C18A 105.8(6) . . ?
C19A C17A C7A 111.3(5) . . ?
C20A C17A C7A 112.7(5) . . ?
C18A C17A C7A 107.7(5) . . ?
C21 C22 H22D 109.5 . . ?
C21 C22 H22E 109.5 . . ?
H22D C22 H22E 109.5 . . ?
C21 C22 H22F 109.5 . . ?
H22D C22 H22F 109.5 . . ?
H22E C22 H22F 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C25A C26A H26A 109.5 . . ?
C25A C26A H26B 109.5 . . ?
H26A C26A H26B 109.5 . . ?
C25A C26A H26C 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
C21A C24A H24D 109.5 . . ?
C21A C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
C21A C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C29 C31 H31D 109.5 . . ?
C29 C31 H31E 109.5 . . ?
H31D C31 H31E 109.5 . . ?
C29 C31 H31F 109.5 . . ?
H31D C31 H31F 109.5 . . ?
H31E C31 H31F 109.5 . . ?
C25A C27A H27A 109.5 . . ?
C25A C27A H27B 109.5 . . ?
H27A C27A H27B 109.5 . . ?
C25A C27A H27C 109.5 . . ?
H27A C27A H27C 109.5 . . ?
H27B C27A H27C 109.5 . . ?
C29A C32A H32D 109.5 . . ?
C29A C32A H32E 109.5 . . ?
H32D C32A H32E 109.5 . . ?
C29A C32A H32F 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C25A C28A H28A 109.5 . . ?
C25A C28A H28B 109.5 . . ?
H28A C28A H28B 109.5 . . ?
C25A C28A H28C 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
C17A C20A H20D 109.5 . . ?
C17A C20A H20E 109.5 . . ?
H20D C20A H20E 109.5 . . ?
C17A C20A H20F 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C29A C30A H30D 109.5 . . ?
C29A C30A H30E 109.5 . . ?
H30D C30A H30E 109.5 . . ?
C29A C30A H30F 109.5 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 109.5 . . ?
C17A C18A H18D 109.5 . . ?
C17A C18A H18E 109.5 . . ?
H18D C18A H18E 109.5 . . ?
C17A C18A H18F 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C101 C100 O100 108.4(10) . . ?
C101 C100 H10A 110.0 . . ?
O100 C100 H10A 110.0 . . ?
C101 C100 H10B 110.0 . . ?
O100 C100 H10B 110.0 . . ?
H10A C100 H10B 108.4 . . ?
O100 C103 C102 105.7(7) . . ?
O100 C103 H10C 110.6 . . ?
C102 C103 H10C 110.6 . . ?
O100 C103 H10D 110.6 . . ?
C102 C103 H10D 110.6 . . ?
H10C C103 H10D 108.7 . . ?
C17A C19A H19D 109.5 . . ?
C17A C19A H19E 109.5 . . ?
H19D C19A H19E 109.5 . . ?
C17A C19A H19F 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C25 C26 H26D 109.5 . . ?
C25 C26 H26E 109.5 . . ?
H26D C26 H26E 109.5 . . ?
C25 C26 H26F 109.5 . . ?
H26D C26 H26F 109.5 . . ?
H26E C26 H26F 109.5 . . ?
C25 C28 H28D 109.5 . . ?
C25 C28 H28E 109.5 . . ?
H28D C28 H28E 109.5 . . ?
C25 C28 H28F 109.5 . . ?
H28D C28 H28F 109.5 . . ?
H28E C28 H28F 109.5 . . ?
C25 C27 H27D 109.5 . . ?
C25 C27 H27E 109.5 . . ?
H27D C27 H27E 109.5 . . ?
C25 C27 H27F 109.5 . . ?
H27D C27 H27F 109.5 . . ?
H27E C27 H27F 109.5 . . ?
N3 C61 H61D 109.5 . . ?
N3 C61 H61E 109.5 . . ?
H61D C61 H61E 109.5 . . ?
N3 C61 H61F 109.5 . . ?
H61D C61 H61F 109.5 . . ?
H61E C61 H61F 109.5 . . ?
C101 C102 C103 107.9(10) . . ?
C101 C102 H10E 110.1 . . ?
C103 C102 H10E 110.1 . . ?
C101 C102 H10F 110.1 . . ?
C103 C102 H10F 110.1 . . ?
H10E C102 H10F 108.4 . . ?
C100 C101 C102 106.9(13) . . ?
C100 C101 H10G 110.3 . . ?
C102 C101 H10G 110.3 . . ?
C100 C101 H10H 110.3 . . ?
C102 C101 H10H 110.3 . . ?
H10G C101 H10H 108.6 . . ?

_refine_diff_density_max         2.379
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.074



####################################################################### 
# 
# 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_sh_0198_0m
_database_code_depnum_ccdc_archive 'CCDC 1921640'
loop_
_audit_author_name
_audit_author_address
'Stephan Hohloch'
;University of Paderborn
Germany
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-08-19 downloaded from the CCDC.
;
_audit_creation_date             2019-06-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H57 Cl N5 Nb O2, C4 H10 O'
_chemical_formula_sum            'C44 H67 Cl N5 Nb O3'
_chemical_formula_weight         842.38
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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'

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

_cell_length_a                   11.0086(16)
_cell_length_b                   15.840(2)
_cell_length_c                   15.982(2)
_cell_angle_alpha                103.559(3)
_cell_angle_beta                 93.800(3)
_cell_angle_gamma                108.092(3)
_cell_volume                     2545.9(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7628
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.53
_cell_measurement_theta_min      1.32
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1171 before and 0.0475 after correction.
The Ratio of minimum to maximum transmission is 0.8190.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.32
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29018
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.538
_diffrn_reflns_theta_min         1.326
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Smart AXS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7628
_reflns_number_total             9465
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker Apex3 software, 2019'
_computing_data_collection       'Bruker Apex3 software, 2019'
_computing_data_reduction        'Bruker Apex3 software, 2019'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.299
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         9465
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0470
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0518P)²+1.9857P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1184
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C102(H10D,H10E), C101(H10I,H10J)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C12(H12), C53(H53), C14(H14), C54(H54), C50(H50), C52(H52),
 C51(H51)
4.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C19(H19A,H19B,H19C), C24(H24A,H24B,H24C), C61(H61A,H61B,
 H61C), C32(H32A,H32B,H32C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C22(H22A,
 H22B,H22C), C43(H43A,H43B,H43C), C41(H41A,H41B,H41C), C18(H18A,H18B,H18C),
 C30(H30A,H30B,H30C), C20(H20A,H20B,H20C), C103(H10A,H10B,H10C), C100(H10F,H10G,
 H10H), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C),
 C28A(H28D,H28E,H28F), C27A(H27D,H27E,H27F), C26A(H26D,H26E,H26F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.52481(2) 0.79644(2) 0.23443(2) 0.02007(9) Uani 1 1 d . . . . .
Cl1 Cl 0.33424(7) 0.84537(6) 0.24432(5) 0.03084(19) Uani 1 1 d . . . . .
O1 O 0.66467(18) 0.91668(13) 0.25432(13) 0.0231(5) Uani 1 1 d . . . . .
O2 O 0.44626(19) 0.67823(14) 0.26402(13) 0.0244(5) Uani 1 1 d . . . . .
N3 N 0.8979(2) 0.77381(18) 0.30992(17) 0.0271(6) Uani 1 1 d . . . . .
N1 N 0.7058(2) 0.69469(17) 0.30640(16) 0.0230(6) Uani 1 1 d . . . . .
N2 N 0.8267(2) 0.69954(18) 0.33056(17) 0.0288(6) Uani 1 1 d . . . . .
N40 N 0.5247(2) 0.75465(17) 0.12250(16) 0.0245(6) Uani 1 1 d . . . . .
N50 N 0.5473(2) 0.85634(17) 0.39513(16) 0.0260(6) Uani 1 1 d . . . . .
C5 C 0.8695(3) 0.8969(2) 0.24004(18) 0.0219(6) Uani 1 1 d . . . . .
C11 C 0.6017(3) 0.6171(2) 0.3137(2) 0.0249(7) Uani 1 1 d . . . . .
C6 C 0.9908(3) 0.9265(2) 0.21367(19) 0.0258(7) Uani 1 1 d . . . . .
H6 H 1.046805 0.893644 0.217986 0.031 Uiso 1 1 calc R . . . .
C10 C 0.7829(3) 0.9454(2) 0.23123(18) 0.0218(6) Uani 1 1 d . . . . .
C2 C 0.8248(3) 0.8157(2) 0.27291(18) 0.0217(6) Uani 1 1 d . . . . .
C1 C 0.6974(3) 0.7640(2) 0.27141(19) 0.0214(6) Uani 1 1 d . . . . .
C8 C 0.9439(3) 1.0499(2) 0.1763(2) 0.0272(7) Uani 1 1 d . . . . .
H8 H 0.969852 1.101678 0.155198 0.033 Uiso 1 1 calc R . . . .
C9 C 0.8207(3) 1.0249(2) 0.20062(19) 0.0240(7) Uani 1 1 d . . . . .
C7 C 1.0300(3) 1.0026(2) 0.1815(2) 0.0297(7) Uani 1 1 d . . . . .
C12 C 0.6298(3) 0.5478(2) 0.3425(2) 0.0316(8) Uani 1 1 d . . . . .
H12 H 0.715143 0.554932 0.361180 0.038 Uiso 1 1 calc R . . . .
C21 C 0.7308(3) 1.0806(2) 0.1936(2) 0.0288(7) Uani 1 1 d . . . . .
C16 C 0.4735(3) 0.6099(2) 0.28717(19) 0.0245(7) Uani 1 1 d . . . . .
C53 C 0.6459(3) 0.9706(3) 0.5291(2) 0.0400(9) Uani 1 1 d . . . . .
H53 H 0.714331 1.023107 0.559173 0.048 Uiso 1 1 calc R . . . .
C14 C 0.4065(3) 0.4606(2) 0.3135(2) 0.0368(8) Uani 1 1 d . . . . .
H14 H 0.340520 0.406642 0.312568 0.044 Uiso 1 1 calc R . . . .
C15 C 0.3738(3) 0.5277(2) 0.2849(2) 0.0296(7) Uani 1 1 d . . . . .
C40 C 0.5427(3) 0.7196(2) 0.0336(2) 0.0301(7) Uani 1 1 d . . . . .
C42 C 0.6879(3) 0.7529(3) 0.0287(2) 0.0402(9) Uani 1 1 d . . . . .
H42A H 0.720257 0.819025 0.043610 0.060 Uiso 1 1 calc GR . . . .
H42B H 0.702044 0.728595 -0.029292 0.060 Uiso 1 1 calc GR . . . .
H42C H 0.732322 0.731809 0.068871 0.060 Uiso 1 1 calc GR . . . .
C54 C 0.6425(3) 0.9319(2) 0.4420(2) 0.0345(8) Uani 1 1 d . . . . .
H54 H 0.709595 0.959560 0.414437 0.041 Uiso 1 1 calc R . . . .
C50 C 0.4528(3) 0.8185(2) 0.4376(2) 0.0320(8) Uani 1 1 d . . . . .
H50 H 0.385503 0.765715 0.406689 0.038 Uiso 1 1 calc R . . . .
C19 C 1.2661(3) 1.0591(2) 0.2348(2) 0.0385(9) Uani 1 1 d . . . . .
H19A H 1.254493 1.107393 0.279081 0.058 Uiso 1 1 calc GR . . . .
H19B H 1.350881 1.080044 0.219118 0.058 Uiso 1 1 calc GR . . . .
H19C H 1.256596 1.006104 0.256377 0.058 Uiso 1 1 calc GR . . . .
C24 C 0.6095(3) 1.0225(2) 0.1273(2) 0.0374(8) Uani 1 1 d . . . . .
H24A H 0.634184 1.002309 0.071533 0.056 Uiso 1 1 calc GR . . . .
H24B H 0.555380 1.058904 0.122669 0.056 Uiso 1 1 calc GR . . . .
H24C H 0.563027 0.969752 0.146027 0.056 Uiso 1 1 calc GR . . . .
C61 C 1.0378(3) 0.7969(3) 0.3298(2) 0.0409(9) Uani 1 1 d . . . . .
H61A H 1.056912 0.770813 0.375391 0.061 Uiso 1 1 calc GR . . . .
H61B H 1.078087 0.862712 0.348356 0.061 Uiso 1 1 calc GR . . . .
H61C H 1.070172 0.772393 0.278661 0.061 Uiso 1 1 calc GR . . . .
C52 C 0.5485(3) 0.9316(3) 0.5711(2) 0.0382(9) Uani 1 1 d . . . . .
H52 H 0.548649 0.957085 0.629814 0.046 Uiso 1 1 calc R . . . .
C13 C 0.5323(4) 0.4691(2) 0.3436(2) 0.0379(9) Uani 1 1 d . . . . .
C32 C 0.2279(4) 0.5148(3) 0.1525(2) 0.0446(9) Uani 1 1 d . . . . .
H32A H 0.281569 0.574310 0.149101 0.067 Uiso 1 1 calc GR . . . .
H32B H 0.140258 0.503738 0.128592 0.067 Uiso 1 1 calc GR . . . .
H32C H 0.257992 0.468152 0.119971 0.067 Uiso 1 1 calc GR . . . .
C51 C 0.4503(4) 0.8538(2) 0.5242(2) 0.0386(9) Uani 1 1 d . . . . .
H51 H 0.382657 0.825192 0.550951 0.046 Uiso 1 1 calc R . . . .
C17 C 1.1651(3) 1.0334(3) 0.1551(2) 0.0405(9) Uani 1 1 d . . . . .
C23 C 0.6935(4) 1.1130(2) 0.2836(2) 0.0433(9) Uani 1 1 d . . . . .
H23A H 0.649715 1.060397 0.303375 0.065 Uiso 1 1 calc GR . . . .
H23B H 0.637320 1.148182 0.279497 0.065 Uiso 1 1 calc GR . . . .
H23C H 0.770099 1.150813 0.324152 0.065 Uiso 1 1 calc GR . . . .
C29 C 0.2341(3) 0.5122(2) 0.2479(2) 0.0384(9) Uani 1 1 d . . . . .
C31 C 0.1843(3) 0.5858(3) 0.3001(3) 0.0481(10) Uani 1 1 d . . . . .
H31A H 0.197757 0.588796 0.360836 0.072 Uiso 1 1 calc GR . . . .
H31B H 0.093705 0.569943 0.280636 0.072 Uiso 1 1 calc GR . . . .
H31C H 0.230383 0.644624 0.291414 0.072 Uiso 1 1 calc GR . . . .
C25 C 0.5618(4) 0.3909(2) 0.3737(3) 0.0531(11) Uani 1 1 d . . . . .
C22 C 0.7965(4) 1.1676(2) 0.1648(3) 0.0420(9) Uani 1 1 d . . . . .
H22A H 0.872406 1.205858 0.205791 0.063 Uiso 1 1 calc GR . . . .
H22B H 0.737720 1.201097 0.162246 0.063 Uiso 1 1 calc GR . . . .
H22C H 0.820521 1.150288 0.108248 0.063 Uiso 1 1 calc GR . . . .
C43 C 0.4709(4) 0.7559(3) -0.0268(2) 0.0482(10) Uani 1 1 d . . . . .
H43A H 0.380269 0.734748 -0.022948 0.072 Uiso 1 1 calc GR . . . .
H43B H 0.483818 0.733684 -0.085599 0.072 Uiso 1 1 calc GR . . . .
H43C H 0.503452 0.822085 -0.009778 0.072 Uiso 1 1 calc GR . . . .
C41 C 0.4919(4) 0.6151(3) 0.0105(3) 0.0558(12) Uani 1 1 d . . . . .
H41A H 0.535865 0.594367 0.051175 0.084 Uiso 1 1 calc GR . . . .
H41B H 0.506957 0.590703 -0.047234 0.084 Uiso 1 1 calc GR . . . .
H41C H 0.400869 0.594204 0.012990 0.084 Uiso 1 1 calc GR . . . .
C18 C 1.1820(4) 0.9536(3) 0.0866(3) 0.0620(13) Uani 1 1 d . . . . .
H18A H 1.170416 0.901565 0.110135 0.093 Uiso 1 1 calc GR . . . .
H18B H 1.267180 0.972486 0.071159 0.093 Uiso 1 1 calc GR . . . .
H18C H 1.118910 0.936653 0.035806 0.093 Uiso 1 1 calc GR . . . .
O100 O 0.9549(4) 0.6056(4) 0.1103(3) 0.1263(18) Uani 1 1 d . . . . .
C30 C 0.1417(4) 0.4183(3) 0.2500(3) 0.0657(14) Uani 1 1 d . . . . .
H30A H 0.169598 0.370385 0.217458 0.099 Uiso 1 1 calc GR . . . .
H30B H 0.056010 0.410456 0.224710 0.099 Uiso 1 1 calc GR . . . .
H30C H 0.141348 0.414946 0.309232 0.099 Uiso 1 1 calc GR . . . .
C20 C 1.1887(4) 1.1168(4) 0.1194(4) 0.0839(19) Uani 1 1 d . . . . .
H20A H 1.127325 1.101804 0.068029 0.126 Uiso 1 1 calc GR . . . .
H20B H 1.274731 1.134534 0.104971 0.126 Uiso 1 1 calc GR . . . .
H20C H 1.179147 1.166987 0.162435 0.126 Uiso 1 1 calc GR . . . .
C103 C 1.1118(5) 0.6789(4) 0.0347(3) 0.0821(16) Uani 1 1 d . . . . .
H10A H 1.131006 0.719408 -0.002548 0.123 Uiso 1 1 calc GR . . . .
H10B H 1.109460 0.618595 0.003611 0.123 Uiso 1 1 calc GR . . . .
H10C H 1.177476 0.702403 0.084960 0.123 Uiso 1 1 calc GR . . . .
C102 C 0.9876(5) 0.6736(4) 0.0620(4) 0.0954(19) Uani 1 1 d . . . . .
H10D H 0.991624 0.733086 0.098232 0.114 Uiso 1 1 calc R . . . .
H10E H 0.922259 0.656332 0.011522 0.114 Uiso 1 1 calc R . . . .
C100 C 0.8055(5) 0.5023(4) 0.1647(4) 0.0883(18) Uani 1 1 d . . . . .
H10F H 0.821130 0.447752 0.134037 0.132 Uiso 1 1 calc GR . . . .
H10G H 0.716220 0.487117 0.172238 0.132 Uiso 1 1 calc GR . . . .
H10H H 0.858914 0.527371 0.220609 0.132 Uiso 1 1 calc GR . . . .
C101 C 0.8359(6) 0.5693(4) 0.1155(4) 0.102(2) Uani 1 1 d . . . . .
H10I H 0.789282 0.540080 0.056821 0.123 Uiso 1 1 calc R . . . .
H10J H 0.803463 0.618324 0.141044 0.123 Uiso 1 1 calc R . . . .
C28 C 0.4563(7) 0.3561(5) 0.4356(5) 0.054(2) Uani 0.552(7) 1 d . U P A 1
H28A H 0.468948 0.404756 0.487541 0.081 Uiso 0.552(7) 1 calc GR . P A 1
H28B H 0.466896 0.303380 0.450790 0.081 Uiso 0.552(7) 1 calc GR . P A 1
H28C H 0.370706 0.339542 0.404919 0.081 Uiso 0.552(7) 1 calc GR . P A 1
C27 C 0.5327(12) 0.3104(6) 0.2977(6) 0.077(4) Uani 0.552(7) 1 d . . P A 1
H27A H 0.443379 0.291090 0.273041 0.116 Uiso 0.552(7) 1 calc GR . P A 1
H27B H 0.549675 0.260878 0.315674 0.116 Uiso 0.552(7) 1 calc GR . P A 1
H27C H 0.586142 0.326779 0.254987 0.116 Uiso 0.552(7) 1 calc GR . P A 1
C26 C 0.6867(9) 0.4164(7) 0.4215(7) 0.071(3) Uani 0.552(7) 1 d . U P A 1
H26A H 0.750556 0.444291 0.388970 0.106 Uiso 0.552(7) 1 calc GR . P A 1
H26B H 0.701062 0.362559 0.431469 0.106 Uiso 0.552(7) 1 calc GR . P A 1
H26C H 0.693236 0.459603 0.476289 0.106 Uiso 0.552(7) 1 calc GR . P A 1
C28A C 0.6321(13) 0.4259(7) 0.4644(6) 0.069(4) Uani 0.448(7) 1 d . . P A 2
H28D H 0.705404 0.479785 0.468825 0.103 Uiso 0.448(7) 1 calc GR . P A 2
H28E H 0.660790 0.379121 0.479090 0.103 Uiso 0.448(7) 1 calc GR . P A 2
H28F H 0.575296 0.441389 0.503771 0.103 Uiso 0.448(7) 1 calc GR . P A 2
C27A C 0.4721(14) 0.3015(9) 0.3382(10) 0.086(4) Uani 0.448(7) 1 d . U P A 2
H27D H 0.397977 0.294146 0.367816 0.129 Uiso 0.448(7) 1 calc GR . P A 2
H27E H 0.511462 0.256877 0.345225 0.129 Uiso 0.448(7) 1 calc GR . P A 2
H27F H 0.445774 0.292659 0.277409 0.129 Uiso 0.448(7) 1 calc GR . P A 2
C26A C 0.6896(13) 0.3720(7) 0.3209(8) 0.078(4) Uani 0.448(7) 1 d . . P A 2
H26D H 0.668266 0.363003 0.259549 0.117 Uiso 0.448(7) 1 calc GR . P A 2
H26E H 0.703654 0.318084 0.331034 0.117 Uiso 0.448(7) 1 calc GR . P A 2
H26F H 0.766652 0.424426 0.343408 0.117 Uiso 0.448(7) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 Cl1 2.4542(8) . ?
Nb1 O1 1.9823(19) . ?
Nb1 O2 1.985(2) . ?
Nb1 N40 1.756(3) . ?
Nb1 N50 2.487(3) . ?
Nb1 C1 2.196(3) . ?
O1 C10 1.346(3) . ?
O2 C16 1.331(3) . ?
N3 N2 1.323(3) . ?
N3 C2 1.376(4) . ?
N3 C61 1.461(4) . ?
N1 N2 1.335(3) . ?
N1 C11 1.431(4) . ?
N1 C1 1.368(4) . ?
N40 C40 1.449(4) . ?
N50 C54 1.338(4) . ?
N50 C50 1.341(4) . ?
C5 C6 1.400(4) . ?
C5 C10 1.416(4) . ?
C5 C2 1.460(4) . ?
C11 C12 1.393(4) . ?
C11 C16 1.408(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.379(4) . ?
C10 C9 1.409(4) . ?
C2 C1 1.382(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.399(4) . ?
C8 C7 1.388(4) . ?
C9 C21 1.532(4) . ?
C7 C17 1.535(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.375(5) . ?
C21 C24 1.531(5) . ?
C21 C23 1.538(4) . ?
C21 C22 1.535(4) . ?
C16 C15 1.410(4) . ?
C53 H53 0.9300 . ?
C53 C54 1.376(5) . ?
C53 C52 1.364(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.383(4) . ?
C14 C13 1.390(5) . ?
C15 C29 1.534(5) . ?
C40 C42 1.533(5) . ?
C40 C43 1.526(5) . ?
C40 C41 1.516(5) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C54 H54 0.9300 . ?
C50 H50 0.9300 . ?
C50 C51 1.372(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C19 C17 1.520(5) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C52 H52 0.9300 . ?
C52 C51 1.372(5) . ?
C13 C25 1.542(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C32 C29 1.534(5) . ?
C51 H51 0.9300 . ?
C17 C18 1.535(6) . ?
C17 C20 1.517(5) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C29 C31 1.534(5) . ?
C29 C30 1.529(5) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C25 C28 1.625(8) . ?
C25 C27 1.473(9) . ?
C25 C26 1.417(10) . ?
C25 C28A 1.488(10) . ?
C25 C27A 1.407(13) . ?
C25 C26A 1.755(13) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
O100 C102 1.438(7) . ?
O100 C101 1.274(7) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C103 H10A 0.9600 . ?
C103 H10B 0.9600 . ?
C103 H10C 0.9600 . ?
C103 C102 1.446(7) . ?
C102 H10D 0.9700 . ?
C102 H10E 0.9700 . ?
C100 H10F 0.9600 . ?
C100 H10G 0.9600 . ?
C100 H10H 0.9600 . ?
C100 C101 1.435(8) . ?
C101 H10I 0.9700 . ?
C101 H10J 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C28A H28D 0.9600 . ?
C28A H28E 0.9600 . ?
C28A H28F 0.9600 . ?
C27A H27D 0.9600 . ?
C27A H27E 0.9600 . ?
C27A H27F 0.9600 . ?
C26A H26D 0.9600 . ?
C26A H26E 0.9600 . ?
C26A H26F 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 Nb1 N50 80.24(6) . . ?
O1 Nb1 Cl1 101.07(6) . . ?
O1 Nb1 O2 151.02(8) . . ?
O1 Nb1 N50 79.25(8) . . ?
O1 Nb1 C1 77.66(9) . . ?
O2 Nb1 Cl1 96.08(6) . . ?
O2 Nb1 N50 80.86(8) . . ?
O2 Nb1 C1 78.67(9) . . ?
N40 Nb1 Cl1 105.13(8) . . ?
N40 Nb1 O1 97.98(10) . . ?
N40 Nb1 O2 99.89(10) . . ?
N40 Nb1 N50 174.41(10) . . ?
N40 Nb1 C1 93.37(11) . . ?
C1 Nb1 Cl1 161.42(8) . . ?
C1 Nb1 N50 81.32(10) . . ?
C10 O1 Nb1 135.64(18) . . ?
C16 O2 Nb1 143.31(19) . . ?
N2 N3 C2 112.8(2) . . ?
N2 N3 C61 115.7(3) . . ?
C2 N3 C61 131.5(3) . . ?
N2 N1 C11 118.5(2) . . ?
N2 N1 C1 114.1(2) . . ?
C1 N1 C11 127.3(2) . . ?
N3 N2 N1 103.4(2) . . ?
C40 N40 Nb1 171.8(2) . . ?
C54 N50 Nb1 123.6(2) . . ?
C54 N50 C50 116.4(3) . . ?
C50 N50 Nb1 119.6(2) . . ?
C6 C5 C10 118.9(3) . . ?
C6 C5 C2 123.2(3) . . ?
C10 C5 C2 117.8(3) . . ?
C12 C11 N1 119.1(3) . . ?
C12 C11 C16 121.4(3) . . ?
C16 C11 N1 119.4(3) . . ?
C5 C6 H6 118.9 . . ?
C7 C6 C5 122.1(3) . . ?
C7 C6 H6 118.9 . . ?
O1 C10 C5 119.7(3) . . ?
O1 C10 C9 119.7(3) . . ?
C9 C10 C5 120.6(3) . . ?
N3 C2 C5 128.1(3) . . ?
N3 C2 C1 105.8(3) . . ?
C1 C2 C5 126.1(3) . . ?
N1 C1 Nb1 128.7(2) . . ?
N1 C1 C2 103.9(2) . . ?
C2 C1 Nb1 127.0(2) . . ?
C9 C8 H8 117.8 . . ?
C7 C8 H8 117.8 . . ?
C7 C8 C9 124.4(3) . . ?
C10 C9 C21 121.6(3) . . ?
C8 C9 C10 116.7(3) . . ?
C8 C9 C21 121.6(3) . . ?
C6 C7 C8 117.2(3) . . ?
C6 C7 C17 120.2(3) . . ?
C8 C7 C17 122.5(3) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.4(3) . . ?
C13 C12 H12 119.8 . . ?
C9 C21 C23 109.2(3) . . ?
C9 C21 C22 112.1(3) . . ?
C24 C21 C9 110.6(3) . . ?
C24 C21 C23 110.3(3) . . ?
C24 C21 C22 107.7(3) . . ?
C22 C21 C23 106.8(3) . . ?
O2 C16 C11 121.4(3) . . ?
O2 C16 C15 120.4(3) . . ?
C11 C16 C15 118.2(3) . . ?
C54 C53 H53 120.2 . . ?
C52 C53 H53 120.2 . . ?
C52 C53 C54 119.6(3) . . ?
C15 C14 H14 118.1 . . ?
C15 C14 C13 123.8(3) . . ?
C13 C14 H14 118.1 . . ?
C16 C15 C29 120.4(3) . . ?
C14 C15 C16 118.1(3) . . ?
C14 C15 C29 121.4(3) . . ?
N40 C40 C42 108.2(3) . . ?
N40 C40 C43 109.2(3) . . ?
N40 C40 C41 108.3(3) . . ?
C43 C40 C42 110.3(3) . . ?
C41 C40 C42 109.4(3) . . ?
C41 C40 C43 111.3(3) . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N50 C54 C53 123.2(3) . . ?
N50 C54 H54 118.4 . . ?
C53 C54 H54 118.4 . . ?
N50 C50 H50 118.3 . . ?
N50 C50 C51 123.3(3) . . ?
C51 C50 H50 118.3 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C61 H61A 109.5 . . ?
N3 C61 H61B 109.5 . . ?
N3 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C53 C52 H52 121.0 . . ?
C53 C52 C51 118.1(3) . . ?
C51 C52 H52 121.0 . . ?
C12 C13 C14 117.8(3) . . ?
C12 C13 C25 121.2(3) . . ?
C14 C13 C25 121.0(3) . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
C50 C51 H51 120.3 . . ?
C52 C51 C50 119.4(3) . . ?
C52 C51 H51 120.3 . . ?
C19 C17 C7 108.9(3) . . ?
C19 C17 C18 108.5(3) . . ?
C18 C17 C7 109.6(3) . . ?
C20 C17 C7 112.3(3) . . ?
C20 C17 C19 107.9(3) . . ?
C20 C17 C18 109.5(4) . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C29 C32 109.1(3) . . ?
C15 C29 C31 111.2(3) . . ?
C32 C29 C31 109.8(3) . . ?
C30 C29 C15 112.1(3) . . ?
C30 C29 C32 107.3(3) . . ?
C30 C29 C31 107.2(3) . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C13 C25 C28 107.5(4) . . ?
C13 C25 C26A 106.2(4) . . ?
C27 C25 C13 108.6(4) . . ?
C27 C25 C28 103.9(6) . . ?
C26 C25 C13 114.8(5) . . ?
C26 C25 C28 108.0(6) . . ?
C26 C25 C27 113.3(7) . . ?
C28A C25 C13 110.5(4) . . ?
C28A C25 C26A 97.7(7) . . ?
C27A C25 C13 116.3(6) . . ?
C27A C25 C28A 124.4(8) . . ?
C27A C25 C26A 96.6(8) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C101 O100 C102 117.5(5) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
H10A C103 H10B 109.5 . . ?
H10A C103 H10C 109.5 . . ?
H10B C103 H10C 109.5 . . ?
C102 C103 H10A 109.5 . . ?
C102 C103 H10B 109.5 . . ?
C102 C103 H10C 109.5 . . ?
O100 C102 C103 108.5(6) . . ?
O100 C102 H10D 110.0 . . ?
O100 C102 H10E 110.0 . . ?
C103 C102 H10D 110.0 . . ?
C103 C102 H10E 110.0 . . ?
H10D C102 H10E 108.4 . . ?
H10F C100 H10G 109.5 . . ?
H10F C100 H10H 109.5 . . ?
H10G C100 H10H 109.5 . . ?
C101 C100 H10F 109.5 . . ?
C101 C100 H10G 109.5 . . ?
C101 C100 H10H 109.5 . . ?
O100 C101 C100 116.6(6) . . ?
O100 C101 H10I 108.1 . . ?
O100 C101 H10J 108.1 . . ?
C100 C101 H10I 108.1 . . ?
C100 C101 H10J 108.1 . . ?
H10I C101 H10J 107.3 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C28A H28D 109.5 . . ?
C25 C28A H28E 109.5 . . ?
C25 C28A H28F 109.5 . . ?
H28D C28A H28E 109.5 . . ?
H28D C28A H28F 109.5 . . ?
H28E C28A H28F 109.5 . . ?
C25 C27A H27D 109.5 . . ?
C25 C27A H27E 109.5 . . ?
C25 C27A H27F 109.5 . . ?
H27D C27A H27E 109.5 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 109.5 . . ?
C25 C26A H26D 109.5 . . ?
C25 C26A H26E 109.5 . . ?
C25 C26A H26F 109.5 . . ?
H26D C26A H26E 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.632 0.500 389.9 80.0 Et2O
2 0.037 0.235 0.081 11.9 0.0 ?
3 -0.037 0.765 0.919 11.9 0.0 ?


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

data_sh_0167m
_database_code_depnum_ccdc_archive 'CCDC 1921639'
loop_
_audit_author_name
_audit_author_address
'Stephan Hohloch'
;University of Paderborn
Germany
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-08-19 downloaded from the CCDC.
;
_audit_creation_date             2019-03-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H57 N5 O2 Ti'
_chemical_formula_sum            'C40 H57 N5 O2 Ti'
_chemical_formula_weight         687.80
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.374(3)
_cell_length_b                   16.810(5)
_cell_length_c                   25.014(8)
_cell_angle_alpha                90
_cell_angle_beta                 90.800(6)
_cell_angle_gamma                90
_cell_volume                     3941(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4175
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.46
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.542117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1272 before and 0.0462 after correction.
The Ratio of minimum to maximum transmission is 0.5421.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0976
_diffrn_reflns_av_unetI/netI     0.0918
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26363
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.460
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart AXS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4175
_reflns_number_total             6902
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker ApexIII suite, 2019'
_computing_data_collection       'Bruker ApexIII suite, 2019'
_computing_data_reduction        'Bruker ApexIII suite, 2019'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.097
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6902
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.0899
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0851P)²+15.4015P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2126
_refine_ls_wR_factor_ref         0.2468
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N1, C2A}
{N1A, C2}
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uiso(N1) = Uiso(C2A)
Uiso(N1A) = Uiso(C2)
4. Others
 Sof(C61B)=Sof(H61D)=Sof(H61E)=Sof(H61F)=1-FVAR(1)
 Sof(C61A)=Sof(H61A)=Sof(H61B)=Sof(H61C)=FVAR(1)
 Fixed Sof: N1(0.5) C2A(0.5) C2(0.5) N1A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C14(H14), C104(H104), C12(H12), C100(H100), C103(H103),
 C102(H102), C101(H101)
5.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C31(H31A,H31B,
 H31C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C),
 C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C61A(H61A,H61B,H61C), C61B(H61D,H61E,
 H61F), C42(H42A,H42B,H42C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.58177(11) 0.34276(6) 0.64223(4) 0.0250(3) Uani 1 1 d . . . . .
O1 O 0.7037(4) 0.4341(2) 0.62448(14) 0.0271(9) Uani 1 1 d . . . . .
O2 O 0.4904(4) 0.2537(2) 0.60548(14) 0.0300(9) Uani 1 1 d . . . . .
N100 N 0.7732(5) 0.2700(3) 0.66308(18) 0.0271(11) Uani 1 1 d . . . . .
N3 N 0.3480(5) 0.5030(3) 0.54107(18) 0.0351(12) Uani 1 1 d . . . . .
N40 N 0.5058(5) 0.3606(3) 0.70155(18) 0.0289(11) Uani 1 1 d . . . . .
N2 N 0.2777(5) 0.4371(3) 0.52822(19) 0.0363(12) Uani 1 1 d . . . . .
C10 C 0.6745(6) 0.5121(3) 0.6243(2) 0.0241(12) Uani 1 1 d . . . . .
C1 C 0.4384(6) 0.4059(3) 0.5921(2) 0.0269(13) Uani 1 1 d . . . . .
C5 C 0.5458(6) 0.5415(3) 0.6022(2) 0.0251(12) Uani 1 1 d . . . . .
C9 C 0.7755(6) 0.5679(3) 0.6436(2) 0.0260(12) Uani 1 1 d . . . . .
C11 C 0.2845(6) 0.2959(3) 0.5553(2) 0.0287(13) Uani 1 1 d . . . . .
C21 C 0.9224(6) 0.5405(3) 0.6650(2) 0.0312(13) Uani 1 1 d . . . . .
C16 C 0.3681(6) 0.2371(3) 0.5804(2) 0.0289(13) Uani 1 1 d . . . . .
C7 C 0.6070(6) 0.6777(3) 0.6238(2) 0.0304(14) Uani 1 1 d . . . . .
C6 C 0.5130(6) 0.6223(3) 0.6033(2) 0.0285(13) Uani 1 1 d . . . . .
H6 H 0.425175 0.639215 0.589755 0.034 Uiso 1 1 calc R . . . .
C8 C 0.7376(6) 0.6482(3) 0.6433(2) 0.0313(13) Uani 1 1 d . . . . .
H8 H 0.803261 0.684528 0.657052 0.038 Uiso 1 1 calc R . . . .
C15 C 0.3182(6) 0.1567(4) 0.5776(2) 0.0337(14) Uani 1 1 d . . . . .
C29 C 0.3994(7) 0.0895(4) 0.6066(2) 0.0386(15) Uani 1 1 d . . . . .
C14 C 0.1945(7) 0.1415(4) 0.5483(2) 0.0410(16) Uani 1 1 d . . . . .
H14 H 0.163699 0.088961 0.545905 0.049 Uiso 1 1 calc R . . . .
C40 C 0.4279(7) 0.3876(4) 0.7482(3) 0.0424(16) Uani 1 1 d . . . . .
C22 C 1.0041(6) 0.4990(4) 0.6199(2) 0.0383(15) Uani 1 1 d . . . . .
H22A H 0.949659 0.454431 0.606941 0.058 Uiso 1 1 calc GR . . . .
H22B H 1.094690 0.480806 0.633389 0.058 Uiso 1 1 calc GR . . . .
H22C H 1.018762 0.535904 0.591191 0.058 Uiso 1 1 calc GR . . . .
C104 C 0.9040(7) 0.2800(4) 0.6437(3) 0.0420(16) Uani 1 1 d . . . . .
H104 H 0.917853 0.318828 0.617814 0.050 Uiso 1 1 calc R . . . .
C24 C 0.9030(7) 0.4845(4) 0.7126(2) 0.0375(15) Uani 1 1 d . . . . .
H24A H 0.861155 0.513214 0.741572 0.056 Uiso 1 1 calc GR . . . .
H24B H 0.994197 0.463889 0.723733 0.056 Uiso 1 1 calc GR . . . .
H24C H 0.841608 0.441284 0.702258 0.056 Uiso 1 1 calc GR . . . .
C17 C 0.5636(7) 0.7652(3) 0.6254(2) 0.0369(15) Uani 1 1 d . . . . .
C13 C 0.1132(7) 0.1993(4) 0.5222(2) 0.0435(17) Uani 1 1 d . . . . .
C12 C 0.1607(7) 0.2766(4) 0.5273(2) 0.0408(16) Uani 1 1 d . . . . .
H12 H 0.107731 0.317209 0.511448 0.049 Uiso 1 1 calc R . . . .
C23 C 1.0147(6) 0.6099(4) 0.6836(3) 0.0414(16) Uani 1 1 d . . . . .
H23A H 1.028859 0.645896 0.654337 0.062 Uiso 1 1 calc GR . . . .
H23B H 1.105338 0.590360 0.696133 0.062 Uiso 1 1 calc GR . . . .
H23C H 0.967965 0.637397 0.712108 0.062 Uiso 1 1 calc GR . . . .
C31 C 0.4046(7) 0.1075(4) 0.6664(3) 0.0462(17) Uani 1 1 d . . . . .
H31A H 0.309964 0.105108 0.680482 0.069 Uiso 1 1 calc GR . . . .
H31B H 0.443242 0.159796 0.672079 0.069 Uiso 1 1 calc GR . . . .
H31C H 0.463976 0.069027 0.684300 0.069 Uiso 1 1 calc GR . . . .
C20 C 0.6720(7) 0.8170(4) 0.6543(3) 0.0526(19) Uani 1 1 d . . . . .
H20A H 0.684009 0.798621 0.690368 0.079 Uiso 1 1 calc GR . . . .
H20B H 0.639030 0.871076 0.654455 0.079 Uiso 1 1 calc GR . . . .
H20C H 0.761574 0.814150 0.636239 0.079 Uiso 1 1 calc GR . . . .
C18 C 0.4210(7) 0.7739(4) 0.6548(3) 0.0515(18) Uani 1 1 d . . . . .
H18A H 0.431624 0.753860 0.690621 0.077 Uiso 1 1 calc GR . . . .
H18B H 0.348371 0.744109 0.636226 0.077 Uiso 1 1 calc GR . . . .
H18C H 0.394290 0.828949 0.655990 0.077 Uiso 1 1 calc GR . . . .
C100 C 0.7584(8) 0.2132(4) 0.7011(3) 0.0520(19) Uani 1 1 d . . . . .
H100 H 0.669549 0.207407 0.716768 0.062 Uiso 1 1 calc R . . . .
C19 C 0.5449(8) 0.7959(4) 0.5684(3) 0.0517(19) Uani 1 1 d . . . . .
H19A H 0.517123 0.850817 0.569155 0.077 Uiso 1 1 calc GR . . . .
H19B H 0.472381 0.765368 0.550232 0.077 Uiso 1 1 calc GR . . . .
H19C H 0.633309 0.790685 0.549783 0.077 Uiso 1 1 calc GR . . . .
C30 C 0.5510(7) 0.0829(4) 0.5843(3) 0.0553(19) Uani 1 1 d . . . . .
H30A H 0.601221 0.131852 0.590507 0.083 Uiso 1 1 calc GR . . . .
H30B H 0.545759 0.072395 0.546635 0.083 Uiso 1 1 calc GR . . . .
H30C H 0.600772 0.040176 0.602005 0.083 Uiso 1 1 calc GR . . . .
C32 C 0.3273(8) 0.0091(4) 0.5991(3) 0.059(2) Uani 1 1 d . . . . .
H32A H 0.379747 -0.030710 0.618573 0.089 Uiso 1 1 calc GR . . . .
H32B H 0.324997 -0.004354 0.561779 0.089 Uiso 1 1 calc GR . . . .
H32C H 0.231587 0.011726 0.612140 0.089 Uiso 1 1 calc GR . . . .
C103 C 1.0182(8) 0.2355(4) 0.6602(3) 0.057(2) Uani 1 1 d . . . . .
H103 H 1.108240 0.245469 0.646521 0.069 Uiso 1 1 calc R . . . .
C102 C 0.9992(8) 0.1759(4) 0.6971(3) 0.057(2) Uani 1 1 d . . . . .
H102 H 1.075339 0.144071 0.708024 0.068 Uiso 1 1 calc R . . . .
C101 C 0.8650(8) 0.1644(5) 0.7176(3) 0.067(2) Uani 1 1 d . . . . .
H101 H 0.848238 0.124099 0.742238 0.080 Uiso 1 1 calc R . . . .
C25 C -0.0203(9) 0.1755(5) 0.4900(3) 0.066(2) Uani 1 1 d . . . . .
C41 C 0.4246(9) 0.3239(6) 0.7905(3) 0.073(3) Uani 1 1 d . . . . .
H41A H 0.378827 0.344203 0.821778 0.109 Uiso 1 1 calc GR . . . .
H41B H 0.520323 0.308096 0.799549 0.109 Uiso 1 1 calc GR . . . .
H41C H 0.372417 0.278752 0.777164 0.109 Uiso 1 1 calc GR . . . .
C43 C 0.5204(11) 0.4548(6) 0.7760(4) 0.094(3) Uani 1 1 d . . . . .
H43A H 0.531923 0.498431 0.751663 0.141 Uiso 1 1 calc GR . . . .
H43B H 0.612406 0.433730 0.785665 0.141 Uiso 1 1 calc GR . . . .
H43C H 0.473201 0.473031 0.807500 0.141 Uiso 1 1 calc GR . . . .
C28 C -0.1276(9) 0.1375(7) 0.5253(4) 0.098(4) Uani 1 1 d . . . . .
H28A H -0.172508 0.177601 0.546625 0.146 Uiso 1 1 calc GR . . . .
H28B H -0.080815 0.099627 0.548311 0.146 Uiso 1 1 calc GR . . . .
H28C H -0.198382 0.110905 0.503771 0.146 Uiso 1 1 calc GR . . . .
C27 C 0.0239(11) 0.1109(7) 0.4482(3) 0.104(4) Uani 1 1 d . . . . .
H27A H -0.058055 0.095780 0.427079 0.156 Uiso 1 1 calc GR . . . .
H27B H 0.061071 0.065115 0.466566 0.156 Uiso 1 1 calc GR . . . .
H27C H 0.095703 0.132258 0.425232 0.156 Uiso 1 1 calc GR . . . .
C61A C 0.2997(13) 0.5677(6) 0.5099(4) 0.036(3) Uani 0.534(12) 1 d . . P A 1
H61A H 0.252264 0.548071 0.478261 0.054 Uiso 0.534(12) 1 calc GR . P A 1
H61B H 0.379508 0.599917 0.499910 0.054 Uiso 0.534(12) 1 calc GR . P A 1
H61C H 0.234252 0.599055 0.530209 0.054 Uiso 0.534(12) 1 calc GR . P A 1
C61B C 0.1780(13) 0.4543(8) 0.4900(5) 0.035(4) Uani 0.466(12) 1 d . . P A 2
H61D H 0.084578 0.444516 0.503834 0.053 Uiso 0.466(12) 1 calc GR . P A 2
H61E H 0.193000 0.421316 0.459301 0.053 Uiso 0.466(12) 1 calc GR . P A 2
H61F H 0.185938 0.509235 0.480001 0.053 Uiso 0.466(12) 1 calc GR . P A 2
C42 C 0.2883(10) 0.4172(7) 0.7356(4) 0.106(3) Uani 1 1 d . U . . .
H42A H 0.295789 0.461711 0.711743 0.158 Uiso 1 1 calc GR . . . .
H42B H 0.242563 0.433715 0.767820 0.158 Uiso 1 1 calc GR . . . .
H42C H 0.233004 0.375954 0.718696 0.158 Uiso 1 1 calc GR . . . .
C26 C -0.0713(13) 0.2415(7) 0.4563(5) 0.133(4) Uani 1 1 d . U . . .
H26A H -0.120479 0.279507 0.477930 0.200 Uiso 1 1 calc GR . . . .
H26B H -0.135203 0.221344 0.429175 0.200 Uiso 1 1 calc GR . . . .
H26C H 0.008512 0.266800 0.439639 0.200 Uiso 1 1 calc GR . . . .
N1 N 0.3324(5) 0.3769(3) 0.55864(19) 0.0261(11) Uiso 0.5 1 d . . P A .
C2A C 0.3324(5) 0.3769(3) 0.55864(19) 0.0261(11) Uiso 0.5 1 d . . P A .
C2 C 0.4449(5) 0.4854(3) 0.57972(19) 0.0287(12) Uiso 0.5 1 d . . P A .
N1A N 0.4449(5) 0.4854(3) 0.57972(19) 0.0287(12) Uiso 0.5 1 d . . P A .


_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
Ti1 O1 1.968(4) . ?
Ti1 O2 1.948(4) . ?
Ti1 N100 2.227(5) . ?
Ti1 N40 1.682(5) . ?
Ti1 C1 2.112(5) . ?
O1 C10 1.341(6) . ?
O2 C16 1.330(6) . ?
N100 C104 1.335(8) . ?
N100 C100 1.357(8) . ?
N3 N2 1.326(7) . ?
N3 C61A 1.409(10) . ?
N3 N1A 1.350(6) . ?
N40 C40 1.457(7) . ?
N2 C61B 1.358(12) . ?
N2 N1 1.363(6) . ?
C10 C5 1.408(7) . ?
C10 C9 1.413(7) . ?
C1 N1 1.379(7) . ?
C1 N1A 1.373(7) . ?
C5 C6 1.393(7) . ?
C5 N1A 1.444(7) . ?
C9 C21 1.541(8) . ?
C9 C8 1.395(7) . ?
C11 C16 1.404(8) . ?
C11 C12 1.385(8) . ?
C11 N1 1.435(7) . ?
C21 C22 1.538(8) . ?
C21 C24 1.530(8) . ?
C21 C23 1.523(8) . ?
C16 C15 1.432(8) . ?
C7 C6 1.377(8) . ?
C7 C8 1.403(8) . ?
C7 C17 1.527(8) . ?
C6 H6 0.9300 . ?
C8 H8 0.9300 . ?
C15 C29 1.538(8) . ?
C15 C14 1.387(8) . ?
C29 C31 1.528(9) . ?
C29 C30 1.538(9) . ?
C29 C32 1.521(9) . ?
C14 H14 0.9300 . ?
C14 C13 1.393(9) . ?
C40 C41 1.507(10) . ?
C40 C43 1.579(11) . ?
C40 C42 1.431(10) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C104 H104 0.9300 . ?
C104 C103 1.364(9) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C17 C20 1.513(9) . ?
C17 C18 1.542(9) . ?
C17 C19 1.524(9) . ?
C13 C12 1.378(9) . ?
C13 C25 1.532(9) . ?
C12 H12 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C100 H100 0.9300 . ?
C100 C101 1.353(9) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C103 H103 0.9300 . ?
C103 C102 1.377(10) . ?
C102 H102 0.9300 . ?
C102 C101 1.379(10) . ?
C101 H101 0.9300 . ?
C25 C28 1.492(12) . ?
C25 C27 1.567(13) . ?
C25 C26 1.469(13) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C61A H61A 0.9600 . ?
C61A H61B 0.9600 . ?
C61A H61C 0.9600 . ?
C61B H61D 0.9600 . ?
C61B H61E 0.9600 . ?
C61B H61F 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 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
O1 Ti1 N100 90.69(16) . . ?
O1 Ti1 C1 80.85(18) . . ?
O2 Ti1 O1 138.19(16) . . ?
O2 Ti1 N100 92.07(16) . . ?
O2 Ti1 C1 80.46(19) . . ?
N40 Ti1 O1 108.32(19) . . ?
N40 Ti1 O2 111.4(2) . . ?
N40 Ti1 N100 103.95(19) . . ?
N40 Ti1 C1 99.2(2) . . ?
C1 Ti1 N100 156.79(19) . . ?
C10 O1 Ti1 130.1(3) . . ?
C16 O2 Ti1 139.0(4) . . ?
C104 N100 Ti1 126.0(4) . . ?
C104 N100 C100 116.5(5) . . ?
C100 N100 Ti1 117.4(4) . . ?
N2 N3 C61A 110.8(6) . . ?
N2 N3 N1A 108.5(4) . . ?
N1A N3 C61A 140.7(7) . . ?
C40 N40 Ti1 170.0(4) . . ?
N3 N2 C61B 109.1(7) . . ?
N3 N2 N1 107.7(4) . . ?
C61B N2 N1 143.2(8) . . ?
O1 C10 C5 121.2(5) . . ?
O1 C10 C9 120.8(5) . . ?
C5 C10 C9 117.9(5) . . ?
N1 C1 Ti1 129.0(4) . . ?
N1A C1 Ti1 126.4(4) . . ?
N1A C1 N1 104.0(5) . . ?
C10 C5 N1A 118.5(5) . . ?
C6 C5 C10 121.5(5) . . ?
C6 C5 N1A 120.0(5) . . ?
C10 C9 C21 120.7(5) . . ?
C8 C9 C10 118.1(5) . . ?
C8 C9 C21 121.2(5) . . ?
C16 C11 N1 118.0(5) . . ?
C12 C11 C16 121.3(5) . . ?
C12 C11 N1 120.7(5) . . ?
C22 C21 C9 109.4(5) . . ?
C24 C21 C9 109.8(5) . . ?
C24 C21 C22 111.0(5) . . ?
C23 C21 C9 112.2(5) . . ?
C23 C21 C22 106.6(5) . . ?
C23 C21 C24 107.8(5) . . ?
O2 C16 C11 122.4(5) . . ?
O2 C16 C15 120.0(5) . . ?
C11 C16 C15 117.6(5) . . ?
C6 C7 C8 116.2(5) . . ?
C6 C7 C17 119.5(5) . . ?
C8 C7 C17 124.3(5) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 C5 121.8(5) . . ?
C7 C6 H6 119.1 . . ?
C9 C8 C7 124.4(5) . . ?
C9 C8 H8 117.8 . . ?
C7 C8 H8 117.8 . . ?
C16 C15 C29 120.7(5) . . ?
C14 C15 C16 118.1(5) . . ?
C14 C15 C29 121.2(5) . . ?
C31 C29 C15 109.0(5) . . ?
C31 C29 C30 110.6(6) . . ?
C30 C29 C15 109.7(5) . . ?
C32 C29 C15 112.2(5) . . ?
C32 C29 C31 107.8(5) . . ?
C32 C29 C30 107.6(6) . . ?
C15 C14 H14 117.7 . . ?
C15 C14 C13 124.5(6) . . ?
C13 C14 H14 117.7 . . ?
N40 C40 C41 110.9(5) . . ?
N40 C40 C43 107.3(5) . . ?
C41 C40 C43 102.5(7) . . ?
C42 C40 N40 113.5(6) . . ?
C42 C40 C41 111.9(7) . . ?
C42 C40 C43 110.1(7) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N100 C104 H104 118.6 . . ?
N100 C104 C103 122.8(6) . . ?
C103 C104 H104 118.6 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C7 C17 C18 109.7(5) . . ?
C20 C17 C7 112.9(5) . . ?
C20 C17 C18 107.4(5) . . ?
C20 C17 C19 108.7(6) . . ?
C19 C17 C7 109.1(5) . . ?
C19 C17 C18 109.0(5) . . ?
C14 C13 C25 120.1(6) . . ?
C12 C13 C14 116.2(5) . . ?
C12 C13 C25 123.7(6) . . ?
C11 C12 H12 118.8 . . ?
C13 C12 C11 122.4(6) . . ?
C13 C12 H12 118.8 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N100 C100 H100 118.0 . . ?
C101 C100 N100 123.9(7) . . ?
C101 C100 H100 118.0 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C104 C103 H103 120.2 . . ?
C104 C103 C102 119.5(7) . . ?
C102 C103 H103 120.2 . . ?
C103 C102 H102 120.7 . . ?
C103 C102 C101 118.6(7) . . ?
C101 C102 H102 120.7 . . ?
C100 C101 C102 118.4(7) . . ?
C100 C101 H101 120.8 . . ?
C102 C101 H101 120.8 . . ?
C13 C25 C27 108.1(7) . . ?
C28 C25 C13 110.6(6) . . ?
C28 C25 C27 106.6(7) . . ?
C26 C25 C13 111.2(7) . . ?
C26 C25 C28 116.5(9) . . ?
C26 C25 C27 103.1(8) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N3 C61A H61A 109.5 . . ?
N3 C61A H61B 109.5 . . ?
N3 C61A H61C 109.5 . . ?
H61A C61A H61B 109.5 . . ?
H61A C61A H61C 109.5 . . ?
H61B C61A H61C 109.5 . . ?
N2 C61B H61D 109.5 . . ?
N2 C61B H61E 109.5 . . ?
N2 C61B H61F 109.5 . . ?
H61D C61B H61E 109.5 . . ?
H61D C61B H61F 109.5 . . ?
H61E C61B H61F 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N2 N1 C1 109.7(5) . . ?
N2 N1 C11 123.9(5) . . ?
C1 N1 C11 126.4(5) . . ?
N3 N1A C1 110.1(5) . . ?
N3 N1A C5 124.5(5) . . ?
C1 N1A C5 125.3(5) . . ?

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

data_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1921641'
loop_
_audit_author_name
_audit_author_address
'Stephan Hohloch'
;University of Paderborn
Germany
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H61 Mo N5 O2'
_chemical_formula_weight         727.86

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   39.691(11)
_cell_length_b                   39.691(11)
_cell_length_c                   14.511(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     19798(12)
_cell_formula_units_Z            18
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    4993
_cell_measurement_theta_min      1.52
_cell_measurement_theta_max      25.40

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_F_000             6984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    0.332
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Buker D8'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24804
_diffrn_reflns_av_unetI/netI     0.1376
_diffrn_reflns_av_R_equivalents  0.1092
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.523
_diffrn_reflns_theta_max         25.401
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8090
_reflns_number_gt                4993
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker ApexIII suite, 2018'
_computing_cell_refinement       'Bruker ApexIII suite, 2018'
_computing_data_reduction        'Bruker ApexIII suite, 2018'
_computing_structure_solution    ShelXT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  WinGX
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0796P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8090
_refine_ls_number_parameters     443
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0664
_refine_ls_wR_factor_ref         0.1764
_refine_ls_wR_factor_gt          0.1547
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.58069(2) 0.48751(2) 0.66437(3) 0.01840(16) Uani 1 1 d . . . . .
O1 O 0.52827(9) 0.47925(9) 0.7000(2) 0.0205(8) Uani 1 1 d . . . . .
O2 O 0.62629(9) 0.51551(10) 0.5786(2) 0.0234(8) Uani 1 1 d . . . . .
N1 N 0.56721(11) 0.48155(11) 0.4444(3) 0.0190(10) Uani 1 1 d . . . . .
N3 N 0.50751(12) 0.45762(12) 0.4189(3) 0.0197(10) Uani 1 1 d . . . . .
N2 N 0.54159(12) 0.47091(12) 0.3755(3) 0.0209(10) Uani 1 1 d . . . . .
N50 N 0.60379(11) 0.52069(12) 0.7540(3) 0.0226(10) Uani 1 1 d . . . . .
N40 N 0.57805(12) 0.44330(12) 0.6887(3) 0.0260(11) Uani 1 1 d . . . . .
C5 C 0.48040(14) 0.44687(14) 0.5810(4) 0.0190(12) Uani 1 1 d . . . . .
C2 C 0.51132(14) 0.46017(14) 0.5121(4) 0.0176(11) Uani 1 1 d . . . . .
C1 C 0.55108(14) 0.47632(14) 0.5300(4) 0.0195(12) Uani 1 1 d . . . . .
C10 C 0.49077(13) 0.45644(13) 0.6740(4) 0.0167(11) Uani 1 1 d . . . . .
C9 C 0.46169(14) 0.44316(13) 0.7427(4) 0.0183(11) Uani 1 1 d . . . . .
C6 C 0.44090(14) 0.42402(14) 0.5567(4) 0.0221(12) Uani 1 1 d . . . . .
H6 H 0.4341 0.4177 0.4952 0.027 Uiso 1 1 calc R U . . .
C11 C 0.60691(13) 0.49496(14) 0.4229(4) 0.0201(12) Uani 1 1 d . . . . .
C17 C 0.36923(14) 0.38425(14) 0.5964(4) 0.0227(12) Uani 1 1 d . . . . .
C8 C 0.42343(14) 0.42071(14) 0.7143(4) 0.0230(12) Uani 1 1 d . . . . .
H8 H 0.4041 0.4117 0.7591 0.028 Uiso 1 1 calc R U . . .
C7 C 0.41211(14) 0.41088(14) 0.6231(4) 0.0209(12) Uani 1 1 d . . . . .
C21 C 0.47152(15) 0.45407(15) 0.8439(4) 0.0228(12) Uani 1 1 d . . . . .
C50 C 0.62108(15) 0.55043(16) 0.8251(4) 0.0254(13) Uani 1 1 d . . . . .
C29 C 0.70658(15) 0.54269(15) 0.5414(4) 0.0246(13) Uani 1 1 d . . . . .
C16 C 0.63452(14) 0.51047(14) 0.4931(4) 0.0218(12) Uani 1 1 d . . . . .
C15 C 0.67410(14) 0.52372(14) 0.4685(4) 0.0222(12) Uani 1 1 d . . . . .
C13 C 0.65530(15) 0.50674(15) 0.3060(4) 0.0265(13) Uani 1 1 d . . . . .
C19 C 0.34305(14) 0.39618(16) 0.6490(4) 0.0287(14) Uani 1 1 d . . . . .
H19A H 0.3509 0.4227 0.6349 0.043 Uiso 1 1 calc R U . . .
H19B H 0.3455 0.3935 0.7140 0.043 Uiso 1 1 calc R U . . .
H19C H 0.3165 0.3797 0.6307 0.043 Uiso 1 1 calc R U . . .
C22 C 0.43589(15) 0.43494(16) 0.9054(4) 0.0267(13) Uani 1 1 d . . . . .
H22A H 0.4172 0.4420 0.8848 0.040 Uiso 1 1 calc R U . . .
H22B H 0.4433 0.4435 0.9678 0.040 Uiso 1 1 calc R U . . .
H22C H 0.4246 0.4072 0.9025 0.040 Uiso 1 1 calc R U . . .
C12 C 0.61660(15) 0.49312(15) 0.3310(4) 0.0250(13) Uani 1 1 d . . . . .
H12 H 0.5972 0.4828 0.2864 0.030 Uiso 1 1 calc R U . . .
C23 C 0.50038(15) 0.44175(16) 0.8809(4) 0.0257(13) Uani 1 1 d . . . . .
H23A H 0.4885 0.4139 0.8783 0.039 Uiso 1 1 calc R U . . .
H23B H 0.5071 0.4503 0.9435 0.039 Uiso 1 1 calc R U . . .
H23C H 0.5235 0.4534 0.8437 0.039 Uiso 1 1 calc R U . . .
C14 C 0.68255(15) 0.52137(15) 0.3778(4) 0.0250(13) Uani 1 1 d . . . . .
H14 H 0.7084 0.5302 0.3629 0.030 Uiso 1 1 calc R U . . .
C30 C 0.71040(15) 0.58137(15) 0.5699(4) 0.0283(13) Uani 1 1 d . . . . .
H30A H 0.7173 0.5981 0.5171 0.043 Uiso 1 1 calc R U . . .
H30B H 0.7303 0.5934 0.6160 0.043 Uiso 1 1 calc R U . . .
H30C H 0.6861 0.5770 0.5943 0.043 Uiso 1 1 calc R U . . .
C32 C 0.74582(15) 0.55065(17) 0.5030(4) 0.0344(15) Uani 1 1 d . . . . .
H32A H 0.7437 0.5267 0.4822 0.052 Uiso 1 1 calc R U . . .
H32B H 0.7652 0.5617 0.5505 0.052 Uiso 1 1 calc R U . . .
H32C H 0.7532 0.5685 0.4523 0.052 Uiso 1 1 calc R U . . .
C61 C 0.47380(14) 0.44317(15) 0.3585(4) 0.0257(13) Uani 1 1 d . . . . .
H61A H 0.4823 0.4513 0.2964 0.039 Uiso 1 1 calc R U . . .
H61B H 0.4576 0.4534 0.3780 0.039 Uiso 1 1 calc R U . . .
H61C H 0.4593 0.4153 0.3613 0.039 Uiso 1 1 calc R U . . .
C24 C 0.49015(17) 0.49860(15) 0.8541(4) 0.0314(14) Uani 1 1 d . . . . .
H24A H 0.5141 0.5113 0.8200 0.047 Uiso 1 1 calc R U . . .
H24B H 0.4953 0.5056 0.9179 0.047 Uiso 1 1 calc R U . . .
H24C H 0.4726 0.5066 0.8305 0.047 Uiso 1 1 calc R U . . .
C40 C 0.58514(17) 0.41774(16) 0.7486(4) 0.0338(15) Uani 1 1 d . . . . .
C20 C 0.36243(16) 0.38616(17) 0.4939(4) 0.0333(14) Uani 1 1 d . . . . .
H20A H 0.3714 0.4127 0.4766 0.050 Uiso 1 1 calc R U . . .
H20B H 0.3352 0.3706 0.4808 0.050 Uiso 1 1 calc R U . . .
H20C H 0.3765 0.3764 0.4596 0.050 Uiso 1 1 calc R U . . .
C43 C 0.54613(17) 0.38095(16) 0.7645(4) 0.0393(16) Uani 1 1 d . . . . .
H43A H 0.5279 0.3878 0.7890 0.059 Uiso 1 1 calc R U . . .
H43B H 0.5494 0.3644 0.8073 0.059 Uiso 1 1 calc R U . . .
H43C H 0.5365 0.3675 0.7071 0.059 Uiso 1 1 calc R U . . .
C25 C 0.66705(16) 0.50701(18) 0.2069(4) 0.0371(15) Uani 1 1 d . . . . .
C18 C 0.35761(16) 0.34223(15) 0.6218(5) 0.0381(16) Uani 1 1 d . . . . .
H18A H 0.3307 0.3253 0.6072 0.057 Uiso 1 1 calc R U . . .
H18B H 0.3616 0.3407 0.6866 0.057 Uiso 1 1 calc R U . . .
H18C H 0.3733 0.3345 0.5876 0.057 Uiso 1 1 calc R U . . .
C31 C 0.69786(16) 0.51600(18) 0.6257(4) 0.0346(15) Uani 1 1 d . . . . .
H31A H 0.6739 0.5111 0.6536 0.052 Uiso 1 1 calc R U . . .
H31B H 0.7186 0.5284 0.6695 0.052 Uiso 1 1 calc R U . . .
H31C H 0.6956 0.4918 0.6064 0.052 Uiso 1 1 calc R U . . .
C53 C 0.6113(2) 0.53166(19) 0.9191(4) 0.0505(19) Uani 1 1 d . . . . .
H53A H 0.5837 0.5185 0.9282 0.076 Uiso 1 1 calc R U . . .
H53B H 0.6239 0.5513 0.9656 0.076 Uiso 1 1 calc R U . . .
H53C H 0.6202 0.5132 0.9234 0.076 Uiso 1 1 calc R U . . .
C42 C 0.6022(2) 0.43739(18) 0.8404(5) 0.052(2) Uani 1 1 d . . . . .
H42A H 0.6267 0.4606 0.8300 0.078 Uiso 1 1 calc R U . . .
H42B H 0.6060 0.4200 0.8791 0.078 Uiso 1 1 calc R U . . .
H42C H 0.5846 0.4440 0.8699 0.078 Uiso 1 1 calc R U . . .
C51 C 0.6058(2) 0.57835(18) 0.8166(5) 0.055(2) Uani 1 1 d . . . . .
H51A H 0.6114 0.5896 0.7561 0.082 Uiso 1 1 calc R U . . .
H51B H 0.6182 0.5986 0.8618 0.082 Uiso 1 1 calc R U . . .
H51C H 0.5782 0.5646 0.8265 0.082 Uiso 1 1 calc R U . . .
C41 C 0.6127(2) 0.4080(2) 0.6974(6) 0.060(2) Uani 1 1 d . . . . .
H41A H 0.6018 0.3968 0.6386 0.090 Uiso 1 1 calc R U . . .
H41B H 0.6165 0.3898 0.7329 0.090 Uiso 1 1 calc R U . . .
H41C H 0.6373 0.4313 0.6884 0.090 Uiso 1 1 calc R U . . .
C52 C 0.66483(18) 0.5715(2) 0.8118(5) 0.068(3) Uani 1 1 d . . . . .
H52A H 0.6736 0.5529 0.8116 0.102 Uiso 1 1 calc R U . . .
H52B H 0.6772 0.5896 0.8613 0.102 Uiso 1 1 calc R U . . .
H52C H 0.6714 0.5852 0.7543 0.102 Uiso 1 1 calc R U . . .
C27 C 0.7057(3) 0.5110(3) 0.1957(8) 0.109(4) Uani 1 1 d . U . . .
H27A H 0.7059 0.4893 0.2239 0.164 Uiso 1 1 calc R U . . .
H27B H 0.7249 0.5347 0.2245 0.164 Uiso 1 1 calc R U . . .
H27C H 0.7115 0.5118 0.1312 0.164 Uiso 1 1 calc R U . . .
C26 C 0.6378(3) 0.4763(3) 0.1478(8) 0.122(4) Uani 1 1 d . U . . .
H26A H 0.6462 0.4814 0.0847 0.182 Uiso 1 1 calc R U . . .
H26B H 0.6135 0.4758 0.1538 0.182 Uiso 1 1 calc R U . . .
H26C H 0.6345 0.4516 0.1660 0.182 Uiso 1 1 calc R U . . .
C28 C 0.6732(4) 0.5445(3) 0.1617(9) 0.138(5) Uani 1 1 d . U . . .
H28A H 0.7005 0.5619 0.1522 0.207 Uiso 1 1 calc R U . . .
H28B H 0.6630 0.5567 0.2011 0.207 Uiso 1 1 calc R U . . .
H28C H 0.6600 0.5385 0.1035 0.207 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 N40 1.741(4) . ?
Mo1 N50 1.749(4) . ?
Mo1 O1 2.005(3) . ?
Mo1 O2 2.013(3) . ?
Mo1 C1 2.204(5) . ?
O1 C10 1.353(5) . ?
O2 C16 1.323(6) . ?
N1 N2 1.336(6) . ?
N1 C1 1.365(7) . ?
N1 C11 1.423(6) . ?
N3 N2 1.339(6) . ?
N3 C2 1.359(6) . ?
N3 C61 1.456(6) . ?
N50 C50 1.455(7) . ?
N40 C40 1.466(7) . ?
C5 C10 1.406(7) . ?
C5 C6 1.409(7) . ?
C5 C2 1.462(7) . ?
C2 C1 1.399(7) . ?
C10 C9 1.412(7) . ?
C9 C8 1.384(7) . ?
C9 C21 1.527(7) . ?
C6 C7 1.382(7) . ?
C6 H6 0.9300 . ?
C11 C16 1.394(7) . ?
C11 C12 1.400(7) . ?
C17 C20 1.520(8) . ?
C17 C18 1.536(7) . ?
C17 C7 1.538(7) . ?
C17 C19 1.543(7) . ?
C8 C7 1.389(7) . ?
C8 H8 0.9300 . ?
C21 C22 1.516(7) . ?
C21 C24 1.544(7) . ?
C21 C23 1.549(7) . ?
C50 C53 1.510(8) . ?
C50 C51 1.510(8) . ?
C50 C52 1.516(8) . ?
C29 C30 1.522(7) . ?
C29 C32 1.531(7) . ?
C29 C31 1.539(7) . ?
C29 C15 1.543(7) . ?
C16 C15 1.430(7) . ?
C15 C14 1.372(7) . ?
C13 C12 1.397(7) . ?
C13 C14 1.402(7) . ?
C13 C25 1.510(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C12 H12 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C14 H14 0.9300 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C40 C42 1.521(9) . ?
C40 C43 1.524(8) . ?
C40 C41 1.525(8) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C25 C26 1.468(11) . ?
C25 C27 1.470(10) . ?
C25 C28 1.531(12) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 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
N40 Mo1 N50 110.7(2) . . ?
N40 Mo1 O1 104.38(17) . . ?
N50 Mo1 O1 92.39(16) . . ?
N40 Mo1 O2 105.41(18) . . ?
N50 Mo1 O2 93.23(17) . . ?
O1 Mo1 O2 145.41(14) . . ?
N40 Mo1 C1 102.62(19) . . ?
N50 Mo1 C1 146.69(19) . . ?
O1 Mo1 C1 77.89(16) . . ?
O2 Mo1 C1 78.80(16) . . ?
C10 O1 Mo1 137.9(3) . . ?
C16 O2 Mo1 135.9(3) . . ?
N2 N1 C1 114.1(4) . . ?
N2 N1 C11 118.6(4) . . ?
C1 N1 C11 127.2(4) . . ?
N2 N3 C2 112.7(4) . . ?
N2 N3 C61 114.9(4) . . ?
C2 N3 C61 132.4(4) . . ?
N1 N2 N3 103.4(4) . . ?
C50 N50 Mo1 174.1(4) . . ?
C40 N40 Mo1 151.9(4) . . ?
C10 C5 C6 119.7(5) . . ?
C10 C5 C2 118.7(4) . . ?
C6 C5 C2 121.6(5) . . ?
N3 C2 C1 106.1(4) . . ?
N3 C2 C5 127.7(4) . . ?
C1 C2 C5 126.1(5) . . ?
N1 C1 C2 103.7(4) . . ?
N1 C1 Mo1 127.7(3) . . ?
C2 C1 Mo1 128.5(4) . . ?
O1 C10 C5 121.6(4) . . ?
O1 C10 C9 118.2(5) . . ?
C5 C10 C9 120.1(4) . . ?
C8 C9 C10 117.3(5) . . ?
C8 C9 C21 120.7(5) . . ?
C10 C9 C21 121.9(4) . . ?
C7 C6 C5 120.8(5) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C16 C11 C12 122.9(5) . . ?
C16 C11 N1 118.9(5) . . ?
C12 C11 N1 118.1(4) . . ?
C20 C17 C18 109.0(5) . . ?
C20 C17 C7 112.1(4) . . ?
C18 C17 C7 108.3(4) . . ?
C20 C17 C19 107.8(4) . . ?
C18 C17 C19 109.4(5) . . ?
C7 C17 C19 110.4(4) . . ?
C9 C8 C7 124.1(5) . . ?
C9 C8 H8 118.0 . . ?
C7 C8 H8 118.0 . . ?
C6 C7 C8 117.9(5) . . ?
C6 C7 C17 120.3(5) . . ?
C8 C7 C17 121.6(5) . . ?
C22 C21 C9 112.5(4) . . ?
C22 C21 C24 108.1(4) . . ?
C9 C21 C24 108.9(4) . . ?
C22 C21 C23 106.9(4) . . ?
C9 C21 C23 111.6(4) . . ?
C24 C21 C23 108.8(4) . . ?
N50 C50 C53 109.9(5) . . ?
N50 C50 C51 109.8(5) . . ?
C53 C50 C51 109.7(5) . . ?
N50 C50 C52 107.6(5) . . ?
C53 C50 C52 109.1(6) . . ?
C51 C50 C52 110.7(5) . . ?
C30 C29 C32 108.2(4) . . ?
C30 C29 C31 110.7(5) . . ?
C32 C29 C31 106.7(4) . . ?
C30 C29 C15 108.4(4) . . ?
C32 C29 C15 111.5(5) . . ?
C31 C29 C15 111.3(4) . . ?
O2 C16 C11 123.6(4) . . ?
O2 C16 C15 119.2(5) . . ?
C11 C16 C15 117.2(5) . . ?
C14 C15 C16 118.4(5) . . ?
C14 C15 C29 121.2(5) . . ?
C16 C15 C29 120.3(5) . . ?
C12 C13 C14 116.0(5) . . ?
C12 C13 C25 121.7(5) . . ?
C14 C13 C25 122.2(5) . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C13 C12 C11 120.3(5) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C14 C13 125.2(5) . . ?
C15 C14 H14 117.4 . . ?
C13 C14 H14 117.4 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C61 H61A 109.5 . . ?
N3 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
N3 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N40 C40 C42 110.8(5) . . ?
N40 C40 C43 107.3(5) . . ?
C42 C40 C43 109.7(5) . . ?
N40 C40 C41 107.3(5) . . ?
C42 C40 C41 111.4(6) . . ?
C43 C40 C41 110.2(5) . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C26 C25 C27 112.0(7) . . ?
C26 C25 C13 116.0(6) . . ?
C27 C25 C13 114.1(6) . . ?
C26 C25 C28 103.4(8) . . ?
C27 C25 C28 101.3(7) . . ?
C13 C25 C28 108.3(7) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

_refine_diff_density_max         1.258
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.108



