# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_ar109
_database_code_depnum_ccdc_archive 'CCDC 1427187'
_audit_update_record             
;
2015-09-24 deposited with the CCDC.
2015-10-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H74 N2 O2'
_chemical_formula_sum            'C54 H74 N2 O2'
_chemical_formula_weight         783.15

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   14.9722(5)
_cell_length_b                   15.3987(5)
_cell_length_c                   21.4056(6)
_cell_angle_alpha                96.271(2)
_cell_angle_beta                 101.891(2)
_cell_angle_gamma                99.527(2)
_cell_volume                     4709.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    12990
_cell_measurement_theta_min      1.76
_cell_measurement_theta_max      25.42

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1712
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9838
_exptl_absorpt_correction_T_max  0.9935
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1.0 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            63231
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         25.42
_reflns_number_total             17278
_reflns_number_gt                12990
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint- Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

 The t-butyl groups reveal partial rotational disorder.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0616P)²+2.2885P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         17278
_refine_ls_number_parameters     1073
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1264
_refine_ls_wR_factor_gt          0.1126
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_restrained_S_all      0.993
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.30002(8) 0.95664(8) 0.45996(5) 0.0189(3) Uani 1 1 d . . .
H1 H 0.2742 1.0029 0.4412 0.068(8) Uiso 1 1 d R . .
O2 O 0.45925(8) 1.32166(7) 0.04998(6) 0.0220(3) Uani 1 1 d . . .
H2 H 0.5120 1.3092 0.0727 0.053(7) Uiso 1 1 d R . .
O3 O 0.40066(8) 1.26119(7) 0.23824(5) 0.0204(3) Uani 1 1 d . . .
H3 H 0.3462 1.2793 0.2223 0.049(7) Uiso 1 1 d R . .
O4 O 0.30916(8) 0.88273(8) 0.29416(5) 0.0211(3) Uani 1 1 d . . .
H4 H 0.3534 0.8543 0.3150 0.054(7) Uiso 1 1 d R . .
N5 N 0.23025(9) 1.07226(9) 0.37515(6) 0.0172(3) Uani 1 1 d . . .
N6 N 0.23734(9) 1.31539(9) 0.16554(7) 0.0183(3) Uani 1 1 d . . .
N7 N 0.43910(9) 0.80982(9) 0.38162(6) 0.0179(3) Uani 1 1 d . . .
N8 N 0.50854(10) 1.08522(9) 0.15148(7) 0.0205(3) Uani 1 1 d . . .
C9 C 0.44517(11) 1.40477(11) 0.30603(7) 0.0166(3) Uani 1 1 d . . .
C10 C 0.55113(11) 1.30158(11) 0.30604(7) 0.0167(3) Uani 1 1 d . . .
C11 C 0.39625(11) 1.24419(11) 0.02467(7) 0.0176(4) Uani 1 1 d . . .
C12 C 0.24720(11) 0.91766(10) 0.49805(7) 0.0151(3) Uani 1 1 d . . .
C13 C 0.31389(11) 0.74673(11) 0.43867(8) 0.0174(3) Uani 1 1 d . . .
C14 C 0.35512(11) 0.75107(11) 0.38530(8) 0.0174(3) Uani 1 1 d . . .
C15 C 0.30304(11) 1.38596(11) 0.15105(8) 0.0170(3) Uani 1 1 d . . .
C16 C 0.31674(11) 1.39960(11) 0.08924(8) 0.0174(3) Uani 1 1 d . . .
C17 C 0.46461(11) 1.32293(11) 0.28333(7) 0.0164(3) Uani 1 1 d . . .
C18 C 0.16790(11) 0.94798(11) 0.50849(7) 0.0168(3) Uani 1 1 d . . .
C19 C 0.42224(12) 1.16197(11) 0.01295(7) 0.0180(4) Uani 1 1 d . . .
C20 C 0.64699(11) 1.27273(11) 0.09757(8) 0.0186(4) Uani 1 1 d . . .
H20 H 0.6615 1.2865 0.0582 0.022 Uiso 1 1 calc R . .
C21 C 0.25135(11) 0.83027(11) 0.24049(8) 0.0179(4) Uani 1 1 d . . .
C22 C 0.09821(11) 0.98103(11) 0.39912(8) 0.0162(3) Uani 1 1 d . . .
C23 C 0.42027(11) 1.51845(11) 0.19795(8) 0.0173(3) Uani 1 1 d . . .
H23 H 0.4570 1.5570 0.2353 0.021 Uiso 1 1 calc R . .
C24 C 0.14970(11) 1.00090(11) 0.35172(8) 0.0157(3) Uani 1 1 d . . .
C25 C 0.27497(11) 0.84627(11) 0.52598(7) 0.0164(3) Uani 1 1 d . . .
C26 C 0.35085(11) 0.80330(11) 0.50532(8) 0.0175(3) Uani 1 1 d . . .
H26A H 0.3732 0.7653 0.5373 0.021 Uiso 1 1 calc R . .
H26B H 0.4040 0.8502 0.5040 0.021 Uiso 1 1 calc R . .
C27 C 0.57934(11) 1.19798(11) 0.09592(8) 0.0173(3) Uani 1 1 d . . .
C28 C 0.30262(12) 1.25215(11) 0.00966(7) 0.0181(4) Uani 1 1 d . . .
C29 C 0.26411(11) 0.74510(11) 0.22066(8) 0.0191(4) Uani 1 1 d . . .
C30 C 0.43156(11) 1.53658(11) 0.13768(8) 0.0176(4) Uani 1 1 d . . .
C31 C 0.59935(12) 1.44348(11) 0.37851(8) 0.0193(4) Uani 1 1 d . . .
C32 C 0.69411(11) 1.32803(11) 0.15480(8) 0.0180(4) Uani 1 1 d . . .
C33 C 0.66785(11) 1.30692(11) 0.21067(8) 0.0185(4) Uani 1 1 d . . .
H33 H 0.6956 1.3456 0.2501 0.022 Uiso 1 1 calc R . .
C34 C 0.11712(11) 0.95201(11) 0.28938(8) 0.0176(4) Uani 1 1 d . . .
C35 C 0.51231(12) 1.46269(11) 0.35355(8) 0.0185(4) Uani 1 1 d . . .
H35 H 0.4985 1.5176 0.3697 0.022 Uiso 1 1 calc R . .
C36 C 0.22475(11) 0.80893(11) 0.56780(8) 0.0187(4) Uani 1 1 d . . .
H36 H 0.2444 0.7611 0.5879 0.022 Uiso 1 1 calc R . .
C37 C 0.13399(11) 1.01860(11) 0.47094(8) 0.0178(4) Uani 1 1 d . . .
H37A H 0.1856 1.0702 0.4763 0.021 Uiso 1 1 calc R . .
H37B H 0.0834 1.0395 0.4880 0.021 Uiso 1 1 calc R . .
C38 C 0.03226(11) 0.89173(11) 0.27559(8) 0.0196(4) Uani 1 1 d . . .
H38 H 0.0107 0.8594 0.2332 0.024 Uiso 1 1 calc R . .
C39 C 0.35682(11) 1.44562(11) 0.20535(8) 0.0166(3) Uani 1 1 d . . .
C40 C 0.11959(11) 0.90838(11) 0.55018(8) 0.0184(4) Uani 1 1 d . . .
H40 H 0.0660 0.9294 0.5578 0.022 Uiso 1 1 calc R . .
C41 C 0.18048(11) 0.86651(11) 0.20649(8) 0.0187(4) Uani 1 1 d . . .
C42 C 0.14708(11) 0.83877(11) 0.58124(8) 0.0190(4) Uani 1 1 d . . .
C43 C 0.60227(11) 1.23112(11) 0.21149(8) 0.0168(3) Uani 1 1 d . . .
C44 C 0.16399(12) 0.95661(11) 0.23226(8) 0.0187(4) Uani 1 1 d . . .
H44A H 0.1242 0.9794 0.1973 0.022 Uiso 1 1 calc R . .
H44B H 0.2243 0.9990 0.2461 0.022 Uiso 1 1 calc R . .
C45 C 0.26941(12) 1.33887(11) 0.02540(8) 0.0190(4) Uani 1 1 d . . .
H45A H 0.2022 1.3234 0.0244 0.023 Uiso 1 1 calc R . .
H45B H 0.2756 1.3742 -0.0100 0.023 Uiso 1 1 calc R . .
C46 C 0.35273(12) 1.08836(11) -0.01716(8) 0.0201(4) Uani 1 1 d . . .
H46 H 0.3701 1.0324 -0.0255 0.024 Uiso 1 1 calc R . .
C47 C 0.49866(12) 1.61774(11) 0.12779(8) 0.0210(4) Uani 1 1 d . . .
C48 C 0.57528(12) 1.21766(11) 0.27547(8) 0.0181(4) Uani 1 1 d . . .
H48A H 0.5211 1.1681 0.2677 0.022 Uiso 1 1 calc R . .
H48B H 0.6277 1.2015 0.3054 0.022 Uiso 1 1 calc R . .
C49 C 0.18662(12) 0.62828(11) 0.37515(8) 0.0207(4) Uani 1 1 d . . .
C50 C 0.37901(11) 1.47560(11) 0.08483(8) 0.0183(4) Uani 1 1 d . . .
H50 H 0.3860 1.4864 0.0431 0.022 Uiso 1 1 calc R . .
C51 C 0.61636(12) 1.36199(11) 0.35348(8) 0.0184(4) Uani 1 1 d . . .
H51 H 0.6750 1.3471 0.3695 0.022 Uiso 1 1 calc R . .
C52 C 0.56145(11) 1.17300(11) 0.15409(8) 0.0169(3) Uani 1 1 d . . .
C53 C -0.02242(11) 0.87612(11) 0.31958(8) 0.0205(4) Uani 1 1 d . . .
C54 C 0.20616(12) 0.69697(12) 0.16359(8) 0.0225(4) Uani 1 1 d . . .
H54 H 0.2145 0.6388 0.1496 0.027 Uiso 1 1 calc R . .
C55 C 0.31235(11) 1.08121(11) 0.34683(8) 0.0196(4) Uani 1 1 d . . .
H55A H 0.2984 1.1052 0.3056 0.024 Uiso 1 1 calc R . .
H55B H 0.3287 1.0221 0.3378 0.024 Uiso 1 1 calc R . .
C56 C 0.52273(12) 1.14823(11) 0.03090(8) 0.0201(4) Uani 1 1 d . . .
H56A H 0.5219 1.0838 0.0308 0.024 Uiso 1 1 calc R . .
H56B H 0.5546 1.1671 -0.0030 0.024 Uiso 1 1 calc R . .
C57 C 0.30947(11) 0.69473(11) 0.32683(8) 0.0187(4) Uani 1 1 d . . .
C58 C 0.35529(11) 1.43136(11) 0.27475(8) 0.0179(4) Uani 1 1 d . . .
H58A H 0.3482 1.4869 0.2996 0.021 Uiso 1 1 calc R . .
H58B H 0.3018 1.3841 0.2748 0.021 Uiso 1 1 calc R . .
C59 C 0.23032(11) 0.68603(11) 0.43135(8) 0.0193(4) Uani 1 1 d . . .
H59 H 0.2019 0.6844 0.4671 0.023 Uiso 1 1 calc R . .
C60 C 0.01446(11) 0.92101(11) 0.38212(8) 0.0193(4) Uani 1 1 d . . .
H60 H -0.0193 0.9099 0.4144 0.023 Uiso 1 1 calc R . .
C61 C 0.25929(12) 1.09357(11) -0.03546(8) 0.0223(4) Uani 1 1 d . . .
C62 C 0.12473(12) 0.81616(12) 0.14964(8) 0.0228(4) Uani 1 1 d . . .
H62 H 0.0766 0.8404 0.1255 0.027 Uiso 1 1 calc R . .
C63 C 0.51789(12) 0.76410(12) 0.38093(9) 0.0237(4) Uani 1 1 d . . .
H63A H 0.4948 0.7037 0.3559 0.028 Uiso 1 1 calc R . .
H63B H 0.5472 0.7578 0.4257 0.028 Uiso 1 1 calc R . .
C64 C 0.33629(12) 0.70548(12) 0.26256(8) 0.0216(4) Uani 1 1 d . . .
H64A H 0.3980 0.7449 0.2704 0.026 Uiso 1 1 calc R . .
H64B H 0.3401 0.6468 0.2404 0.026 Uiso 1 1 calc R . .
C65 C 0.23676(12) 1.17674(11) -0.02124(8) 0.0215(4) Uani 1 1 d . . .
H65 H 0.1735 1.1822 -0.0332 0.026 Uiso 1 1 calc R . .
C66 C 0.53872(12) 0.95466(11) 0.38714(9) 0.0223(4) Uani 1 1 d . . .
H66A H 0.5065 0.9597 0.3428 0.027 Uiso 1 1 calc R . .
H66B H 0.5597 1.0154 0.4119 0.027 Uiso 1 1 calc R . .
C67 C 0.77201(12) 1.40715(12) 0.15631(8) 0.0238(4) Uani 1 1 d . . .
C68 C 0.22932(12) 0.63371(11) 0.32346(8) 0.0206(4) Uani 1 1 d . . .
H68 H 0.2023 0.5940 0.2844 0.025 Uiso 1 1 calc R . .
C69 C 0.40987(12) 1.07334(12) 0.15247(9) 0.0238(4) Uani 1 1 d . . .
H69A H 0.3799 1.1139 0.1259 0.029 Uiso 1 1 calc R . .
H69B H 0.4031 1.0879 0.1973 0.029 Uiso 1 1 calc R . .
C70 C 0.15353(12) 1.34472(12) 0.17886(8) 0.0227(4) Uani 1 1 d . . .
H70A H 0.1105 1.3476 0.1376 0.027 Uiso 1 1 calc R . .
H70B H 0.1712 1.4052 0.2042 0.027 Uiso 1 1 calc R . .
C71 C 0.67151(12) 1.50976(12) 0.43062(8) 0.0245(4) Uani 1 1 d . . .
C72 C 0.75980(14) 1.44321(13) 0.09172(9) 0.0303(4) Uani 1 1 d . . .
H72A H 0.7671 1.3981 0.0581 0.046 Uiso 1 1 calc R . .
H72B H 0.8069 1.4972 0.0956 0.046 Uiso 1 1 calc R . .
H72C H 0.6976 1.4574 0.0801 0.046 Uiso 1 1 calc R . .
C73 C 0.39367(12) 1.14383(12) 0.39383(9) 0.0253(4) Uani 1 1 d . . .
H73A H 0.4089 1.1183 0.4343 0.030 Uiso 1 1 calc R . .
H73B H 0.4490 1.1498 0.3749 0.030 Uiso 1 1 calc R . .
C74 C 0.47175(11) 0.89944(11) 0.41892(8) 0.0188(4) Uani 1 1 d . . .
H74A H 0.5035 0.8953 0.4636 0.023 Uiso 1 1 calc R . .
H74B H 0.4180 0.9286 0.4210 0.023 Uiso 1 1 calc R . .
C75 C 0.18267(13) 1.01275(12) -0.06729(9) 0.0265(4) Uani 1 1 d . . .
C76 C 0.08713(13) 0.79376(12) 0.62336(9) 0.0256(4) Uani 1 1 d . . .
C77 C 0.10469(13) 1.28118(12) 0.21612(9) 0.0280(4) Uani 1 1 d . . .
H77A H 0.0466 1.3001 0.2221 0.034 Uiso 1 1 calc R . .
H77B H 0.1452 1.2833 0.2593 0.034 Uiso 1 1 calc R . .
C78 C 0.16811(13) 1.15973(12) 0.16271(9) 0.0277(4) Uani 1 1 d . . .
H78A H 0.2135 1.1557 0.2026 0.033 Uiso 1 1 calc R . .
H78B H 0.1509 1.1004 0.1358 0.033 Uiso 1 1 calc R . .
C79 C 0.20294(13) 1.15947(11) 0.38418(9) 0.0238(4) Uani 1 1 d . . .
H79A H 0.1455 1.1530 0.4007 0.029 Uiso 1 1 calc R . .
H79B H 0.1896 1.1814 0.3421 0.029 Uiso 1 1 calc R . .
C80 C 0.58997(12) 0.81539(12) 0.35107(10) 0.0288(4) Uani 1 1 d . . .
H80A H 0.5628 0.8151 0.3048 0.035 Uiso 1 1 calc R . .
H80B H 0.6440 0.7855 0.3542 0.035 Uiso 1 1 calc R . .
C81 C 0.21286(12) 1.22718(11) 0.12610(8) 0.0220(4) Uani 1 1 d . . .
H81A H 0.2695 1.2095 0.1159 0.026 Uiso 1 1 calc R . .
H81B H 0.1691 1.2290 0.0850 0.026 Uiso 1 1 calc R . .
C82 C 0.62255(12) 0.91130(12) 0.38478(9) 0.0280(4) Uani 1 1 d . . .
H82A H 0.6588 0.9123 0.4292 0.034 Uiso 1 1 calc R . .
H82B H 0.6634 0.9450 0.3611 0.034 Uiso 1 1 calc R . .
C83 C 0.55811(13) 1.02758(12) 0.18962(9) 0.0267(4) Uani 1 1 d . . .
H83A H 0.5543 1.0402 0.2352 0.032 Uiso 1 1 calc R . .
H83B H 0.6245 1.0395 0.1879 0.032 Uiso 1 1 calc R . .
C84 C -0.11990(12) 0.81768(12) 0.30074(9) 0.0263(4) Uani 1 1 d . . .
C85 C 0.56802(13) 1.58721(13) 0.09103(9) 0.0303(4) Uani 1 1 d . . .
H85A H 0.6127 1.6391 0.0867 0.045 Uiso 1 1 calc R . .
H85B H 0.5346 1.5562 0.0481 0.045 Uiso 1 1 calc R . .
H85C H 0.6012 1.5468 0.1148 0.045 Uiso 1 1 calc R . .
C86 C 0.09359(13) 0.56418(13) 0.36642(9) 0.0302(4) Uani 1 1 d . . .
C87 C 0.51547(15) 0.93065(12) 0.16323(10) 0.0336(5) Uani 1 1 d . . .
H87A H 0.5470 0.8917 0.1905 0.040 Uiso 1 1 calc R . .
H87B H 0.5242 0.9167 0.1189 0.040 Uiso 1 1 calc R . .
C88 C 0.08170(14) 1.18580(13) 0.18034(10) 0.0326(5) Uani 1 1 d . . .
H88A H 0.0578 1.1445 0.2081 0.039 Uiso 1 1 calc R . .
H88B H 0.0326 1.1811 0.1406 0.039 Uiso 1 1 calc R . .
C89 C 0.55418(14) 1.67306(13) 0.19169(9) 0.0336(5) Uani 1 1 d . . .
H89A H 0.5114 1.6951 0.2158 0.050 Uiso 1 1 calc R . .
H89B H 0.5968 1.7236 0.1832 0.050 Uiso 1 1 calc R . .
H89C H 0.5900 1.6360 0.2172 0.050 Uiso 1 1 calc R . .
C90 C -0.13716(13) 0.75702(13) 0.23615(10) 0.0326(5) Uani 1 1 d . . .
H90A H -0.1348 0.7935 0.2015 0.049 Uiso 1 1 calc R . .
H90B H -0.1985 0.7182 0.2276 0.049 Uiso 1 1 calc R . .
H90C H -0.0892 0.7205 0.2379 0.049 Uiso 1 1 calc R . .
C91 C 0.44267(14) 1.67669(12) 0.08885(10) 0.0335(5) Uani 1 1 d . . .
H91A H 0.3978 1.6958 0.1123 0.050 Uiso 1 1 calc R . .
H91B H 0.4093 1.6429 0.0467 0.050 Uiso 1 1 calc R . .
H91C H 0.4850 1.7291 0.0827 0.050 Uiso 1 1 calc R . .
C92 C 0.13668(13) 0.73157(12) 0.12663(8) 0.0248(4) Uani 1 1 d . . .
C93 C -0.00663(13) 0.74576(13) 0.57940(10) 0.0319(5) Uani 1 1 d . . .
H93A H -0.0353 0.7882 0.5549 0.048 Uiso 1 1 calc R . .
H93B H -0.0478 0.7210 0.6058 0.048 Uiso 1 1 calc R . .
H93C H 0.0035 0.6975 0.5494 0.048 Uiso 1 1 calc R . .
C94 C 0.27932(14) 1.22636(12) 0.43120(9) 0.0308(4) Uani 1 1 d . . .
H94A H 0.2886 1.2071 0.4743 0.037 Uiso 1 1 calc R . .
H94B H 0.2605 1.2850 0.4350 0.037 Uiso 1 1 calc R . .
C95 C 0.41213(15) 0.91301(12) 0.16236(10) 0.0362(5) Uani 1 1 d . . .
H95A H 0.3839 0.8511 0.1417 0.043 Uiso 1 1 calc R . .
H95B H 0.4038 0.9196 0.2072 0.043 Uiso 1 1 calc R . .
C96 C 0.13193(14) 0.72437(15) 0.65743(11) 0.0379(5) Uani 1 1 d . . .
H96A H 0.1390 0.6773 0.6252 0.057 Uiso 1 1 calc R . .
H96B H 0.0923 0.6985 0.6845 0.057 Uiso 1 1 calc R . .
H96C H 0.1932 0.7528 0.6845 0.057 Uiso 1 1 calc R . .
C97 C 0.07196(15) 0.67793(14) 0.06438(9) 0.0371(5) Uani 1 1 d . . .
C98 C 0.37044(14) 1.23532(12) 0.40892(9) 0.0317(5) Uani 1 1 d . . .
H98A H 0.3648 1.2649 0.3699 0.038 Uiso 1 1 calc R . .
H98B H 0.4212 1.2726 0.4432 0.038 Uiso 1 1 calc R . .
C99 C 0.36313(14) 0.97710(12) 0.12575(9) 0.0327(5) Uani 1 1 d . . .
H99A H 0.2973 0.9677 0.1291 0.039 Uiso 1 1 calc R . .
H99B H 0.3641 0.9650 0.0795 0.039 Uiso 1 1 calc R . .
C100 C -0.19046(13) 0.87993(14) 0.29501(10) 0.0365(5) Uani 1 1 d . . .
H10A H -0.1821 0.9172 0.3367 0.055 Uiso 1 1 calc R . .
H10B H -0.2537 0.8444 0.2824 0.055 Uiso 1 1 calc R . .
H10C H -0.1806 0.9179 0.2622 0.055 Uiso 1 1 calc R . .
C101 C 0.77406(15) 1.48384(13) 0.20921(10) 0.0366(5) Uani 1 1 d . . .
H10D H 0.7126 1.5000 0.2033 0.055 Uiso 1 1 calc R . .
H10E H 0.8203 1.5355 0.2064 0.055 Uiso 1 1 calc R . .
H10F H 0.7906 1.4650 0.2517 0.055 Uiso 1 1 calc R . .
C102 C 0.67737(15) 1.60350(13) 0.41306(11) 0.0408(5) Uani 1 1 d . . .
H10G H 0.7304 1.6436 0.4428 0.061 Uiso 1 1 calc R . .
H10H H 0.6199 1.6244 0.4163 0.061 Uiso 1 1 calc R . .
H10I H 0.6856 1.6028 0.3688 0.061 Uiso 1 1 calc R . .
C103 C 0.07126(15) 0.86343(14) 0.67471(9) 0.0347(5) Uani 1 1 d . . .
H10J H 0.1312 0.8932 0.7029 0.052 Uiso 1 1 calc R . .
H10K H 0.0317 0.8341 0.7005 0.052 Uiso 1 1 calc R . .
H10L H 0.0407 0.9075 0.6536 0.052 Uiso 1 1 calc R . .
C104 C 0.86518(13) 1.37559(15) 0.16987(12) 0.0419(5) Uani 1 1 d . . .
H10M H 0.8754 1.3553 0.2121 0.063 Uiso 1 1 calc R . .
H10N H 0.9157 1.4249 0.1698 0.063 Uiso 1 1 calc R . .
H10O H 0.8640 1.3264 0.1364 0.063 Uiso 1 1 calc R . .
C105 C 0.05013(14) 0.57633(16) 0.42446(10) 0.0428(6) Uani 1 1 d . . .
H10P H 0.0920 0.5645 0.4629 0.064 Uiso 1 1 calc R . .
H10Q H -0.0095 0.5348 0.4163 0.064 Uiso 1 1 calc R . .
H10R H 0.0400 0.6376 0.4316 0.064 Uiso 1 1 calc R . .
C106 C -0.13613(16) 0.75917(15) 0.35270(11) 0.0444(6) Uani 1 1 d . . .
H10S H -0.0882 0.7226 0.3594 0.067 Uiso 1 1 calc R . .
H10T H -0.1976 0.7204 0.3385 0.067 Uiso 1 1 calc R . .
H10U H -0.1329 0.7972 0.3932 0.067 Uiso 1 1 calc R . .
C107 C 0.76810(15) 1.48721(16) 0.43841(12) 0.0506(6) Uani 1 1 d . . .
H10V H 0.8126 1.5319 0.4712 0.076 Uiso 1 1 calc R . .
H10W H 0.7869 1.4869 0.3972 0.076 Uiso 1 1 calc R . .
H101 H 0.7670 1.4283 0.4519 0.076 Uiso 1 1 calc R . .
C108 C 0.10895(18) 0.46830(14) 0.35555(12) 0.0524(7) Uani 1 1 d . . .
H102 H 0.1519 0.4569 0.3936 0.079 Uiso 1 1 calc R . .
H103 H 0.1354 0.4597 0.3176 0.079 Uiso 1 1 calc R . .
H104 H 0.0493 0.4269 0.3485 0.079 Uiso 1 1 calc R . .
C109 C 0.22166(17) 0.92766(15) -0.07919(13) 0.0539(7) Uani 1 1 d . . .
H105 H 0.2642 0.9364 -0.1081 0.081 Uiso 1 1 calc R . .
H106 H 0.1703 0.8778 -0.0990 0.081 Uiso 1 1 calc R . .
H107 H 0.2553 0.9146 -0.0380 0.081 Uiso 1 1 calc R . .
C110 C 0.64309(18) 1.50793(16) 0.49516(10) 0.0503(6) Uani 1 1 d . . .
H108 H 0.6404 1.4480 0.5069 0.075 Uiso 1 1 calc R . .
H109 H 0.5818 1.5241 0.4913 0.075 Uiso 1 1 calc R . .
H110 H 0.6889 1.5506 0.5286 0.075 Uiso 1 1 calc R . .
C111 C 0.10620(17) 0.59301(18) 0.04289(11) 0.0567(7) Uani 1 1 d . . .
H111 H 0.1705 0.6090 0.0385 0.085 Uiso 1 1 calc R . .
H112 H 0.0665 0.5632 0.0013 0.085 Uiso 1 1 calc R . .
H113 H 0.1034 0.5528 0.0752 0.085 Uiso 1 1 calc R . .
C112 C 0.11730(17) 0.99439(16) -0.02171(12) 0.0545(7) Uani 1 1 d . . .
H114 H 0.1526 0.9818 0.0191 0.082 Uiso 1 1 calc R . .
H115 H 0.0679 0.9429 -0.0417 0.082 Uiso 1 1 calc R . .
H116 H 0.0897 1.0467 -0.0134 0.082 Uiso 1 1 calc R . .
C113 C 0.02526(15) 0.5821(2) 0.30753(11) 0.0568(7) Uani 1 1 d . . .
H117 H -0.0362 0.5454 0.3038 0.085 Uiso 1 1 calc R . .
H118 H 0.0474 0.5672 0.2685 0.085 Uiso 1 1 calc R . .
H119 H 0.0209 0.6452 0.3127 0.085 Uiso 1 1 calc R . .
C114 C -0.02445(16) 0.64867(18) 0.07686(13) 0.0631(8) Uani 1 1 d . . .
H120 H -0.0199 0.6125 0.1119 0.095 Uiso 1 1 calc R . .
H121 H -0.0659 0.6134 0.0376 0.095 Uiso 1 1 calc R . .
H122 H -0.0495 0.7013 0.0891 0.095 Uiso 1 1 calc R . .
C115 C 0.1284(2) 1.03136(17) -0.13019(13) 0.0706(9) Uani 1 1 d . . .
H123 H 0.0971 1.0811 -0.1218 0.106 Uiso 1 1 calc R . .
H124 H 0.0818 0.9783 -0.1514 0.106 Uiso 1 1 calc R . .
H125 H 0.1708 1.0468 -0.1583 0.106 Uiso 1 1 calc R . .
C116 C 0.0678(3) 0.7342(2) 0.01049(12) 0.1165(17) Uani 1 1 d . . .
H126 H 0.0384 0.7846 0.0207 0.175 Uiso 1 1 calc R . .
H127 H 0.0314 0.6980 -0.0301 0.175 Uiso 1 1 calc R . .
H128 H 0.1311 0.7565 0.0060 0.175 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C12 1.3660(19) . ?
O2 C11 1.3719(19) . ?
O3 C17 1.3674(19) . ?
O4 C21 1.3703(19) . ?
N5 C24 1.451(2) . ?
N5 C55 1.472(2) . ?
N5 C79 1.472(2) . ?
N6 C15 1.446(2) . ?
N6 C81 1.466(2) . ?
N6 C70 1.472(2) . ?
N7 C14 1.444(2) . ?
N7 C74 1.468(2) . ?
N7 C63 1.472(2) . ?
N8 C52 1.438(2) . ?
N8 C83 1.460(2) . ?
N8 C69 1.463(2) . ?
C9 C35 1.387(2) . ?
C9 C17 1.398(2) . ?
C9 C58 1.516(2) . ?
C10 C51 1.391(2) . ?
C10 C17 1.392(2) . ?
C10 C48 1.515(2) . ?
C11 C19 1.397(2) . ?
C11 C28 1.401(2) . ?
C12 C25 1.390(2) . ?
C12 C18 1.396(2) . ?
C13 C59 1.401(2) . ?
C13 C14 1.409(2) . ?
C13 C26 1.531(2) . ?
C14 C57 1.414(2) . ?
C15 C39 1.407(2) . ?
C15 C16 1.412(2) . ?
C16 C50 1.395(2) . ?
C16 C45 1.532(2) . ?
C18 C40 1.389(2) . ?
C18 C37 1.514(2) . ?
C19 C46 1.399(2) . ?
C19 C56 1.530(2) . ?
C20 C27 1.394(2) . ?
C20 C32 1.393(2) . ?
C21 C29 1.390(2) . ?
C21 C41 1.391(2) . ?
C22 C60 1.383(2) . ?
C22 C24 1.425(2) . ?
C22 C37 1.533(2) . ?
C23 C30 1.387(2) . ?
C23 C39 1.391(2) . ?
C24 C34 1.406(2) . ?
C25 C36 1.394(2) . ?
C25 C26 1.522(2) . ?
C27 C52 1.406(2) . ?
C27 C56 1.519(2) . ?
C28 C65 1.394(2) . ?
C28 C45 1.528(2) . ?
C29 C54 1.395(2) . ?
C29 C64 1.511(2) . ?
C30 C50 1.392(2) . ?
C30 C47 1.532(2) . ?
C31 C51 1.393(2) . ?
C31 C35 1.395(2) . ?
C31 C71 1.531(2) . ?
C32 C33 1.388(2) . ?
C32 C67 1.533(2) . ?
C33 C43 1.400(2) . ?
C34 C38 1.399(2) . ?
C34 C44 1.533(2) . ?
C36 C42 1.390(2) . ?
C38 C53 1.384(2) . ?
C39 C58 1.529(2) . ?
C40 C42 1.396(2) . ?
C41 C62 1.393(2) . ?
C41 C44 1.514(2) . ?
C42 C76 1.537(2) . ?
C43 C52 1.398(2) . ?
C43 C48 1.531(2) . ?
C46 C61 1.391(3) . ?
C47 C85 1.528(2) . ?
C47 C89 1.526(2) . ?
C47 C91 1.533(3) . ?
C49 C59 1.384(2) . ?
C49 C68 1.391(2) . ?
C49 C86 1.532(2) . ?
C53 C60 1.393(2) . ?
C53 C84 1.532(2) . ?
C54 C92 1.389(3) . ?
C55 C73 1.523(2) . ?
C57 C68 1.380(2) . ?
C57 C64 1.528(2) . ?
C61 C65 1.395(2) . ?
C61 C75 1.533(2) . ?
C62 C92 1.395(3) . ?
C63 C80 1.520(2) . ?
C66 C82 1.523(3) . ?
C66 C74 1.522(2) . ?
C67 C104 1.535(3) . ?
C67 C72 1.533(2) . ?
C67 C101 1.536(3) . ?
C69 C99 1.523(2) . ?
C70 C77 1.517(2) . ?
C71 C107 1.523(3) . ?
C71 C102 1.524(3) . ?
C71 C110 1.529(3) . ?
C73 C98 1.523(3) . ?
C75 C115 1.505(3) . ?
C75 C112 1.534(3) . ?
C75 C109 1.538(3) . ?
C76 C96 1.526(3) . ?
C76 C103 1.533(3) . ?
C76 C93 1.537(3) . ?
C77 C88 1.530(3) . ?
C78 C81 1.519(2) . ?
C78 C88 1.522(3) . ?
C79 C94 1.514(3) . ?
C80 C82 1.524(2) . ?
C83 C87 1.519(2) . ?
C84 C90 1.530(3) . ?
C84 C106 1.538(3) . ?
C84 C100 1.535(3) . ?
C86 C105 1.525(3) . ?
C86 C108 1.532(3) . ?
C86 C113 1.533(3) . ?
C87 C95 1.522(3) . ?
C92 C97 1.536(2) . ?
C94 C98 1.526(3) . ?
C95 C99 1.516(3) . ?
C97 C116 1.514(3) . ?
C97 C114 1.526(3) . ?
C97 C111 1.540(3) . ?

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
C24 N5 C55 123.14(13) . . ?
C24 N5 C79 111.52(13) . . ?
C55 N5 C79 109.21(13) . . ?
C15 N6 C81 120.81(13) . . ?
C15 N6 C70 113.15(13) . . ?
C81 N6 C70 110.67(13) . . ?
C14 N7 C74 123.60(13) . . ?
C14 N7 C63 113.15(13) . . ?
C74 N7 C63 110.26(13) . . ?
C52 N8 C83 114.56(14) . . ?
C52 N8 C69 119.94(14) . . ?
C83 N8 C69 113.38(14) . . ?
C35 C9 C17 118.72(15) . . ?
C35 C9 C58 121.47(15) . . ?
C17 C9 C58 119.63(14) . . ?
C51 C10 C17 118.52(15) . . ?
C51 C10 C48 121.28(15) . . ?
C17 C10 C48 120.02(14) . . ?
O2 C11 C19 123.07(15) . . ?
O2 C11 C28 115.87(15) . . ?
C19 C11 C28 121.05(15) . . ?
O1 C12 C25 117.64(14) . . ?
O1 C12 C18 121.39(15) . . ?
C25 C12 C18 120.97(14) . . ?
C59 C13 C14 118.33(15) . . ?
C59 C13 C26 115.33(14) . . ?
C14 C13 C26 126.34(14) . . ?
C13 C14 C57 118.32(14) . . ?
C13 C14 N7 127.55(14) . . ?
C57 C14 N7 114.08(14) . . ?
C39 C15 C16 118.97(14) . . ?
C39 C15 N6 114.53(14) . . ?
C16 C15 N6 126.51(14) . . ?
C50 C16 C15 117.81(15) . . ?
C50 C16 C45 115.81(14) . . ?
C15 C16 C45 126.39(14) . . ?
O3 C17 C10 117.39(14) . . ?
O3 C17 C9 122.00(15) . . ?
C10 C17 C9 120.61(15) . . ?
C40 C18 C12 118.68(15) . . ?
C40 C18 C37 122.19(15) . . ?
C12 C18 C37 119.02(14) . . ?
C11 C19 C46 118.23(15) . . ?
C11 C19 C56 123.51(14) . . ?
C46 C19 C56 118.25(15) . . ?
C27 C20 C32 122.48(15) . . ?
O4 C21 C29 121.22(15) . . ?
O4 C21 C41 117.05(15) . . ?
C29 C21 C41 121.72(15) . . ?
C60 C22 C24 120.27(15) . . ?
C60 C22 C37 116.57(14) . . ?
C24 C22 C37 123.03(14) . . ?
C30 C23 C39 122.06(15) . . ?
C34 C24 C22 117.98(14) . . ?
C34 C24 N5 128.24(14) . . ?
C22 C24 N5 113.78(13) . . ?
C12 C25 C36 118.30(15) . . ?
C12 C25 C26 120.57(14) . . ?
C36 C25 C26 120.75(15) . . ?
C25 C26 C13 110.61(13) . . ?
C20 C27 C52 119.58(15) . . ?
C20 C27 C56 118.94(14) . . ?
C52 C27 C56 121.40(14) . . ?
C65 C28 C11 117.94(16) . . ?
C65 C28 C45 118.64(15) . . ?
C11 C28 C45 123.42(14) . . ?
C21 C29 C54 118.42(16) . . ?
C21 C29 C64 119.66(14) . . ?
C54 C29 C64 121.85(15) . . ?
C23 C30 C50 116.43(15) . . ?
C23 C30 C47 123.33(14) . . ?
C50 C30 C47 120.23(14) . . ?
C51 C31 C35 116.63(15) . . ?
C51 C31 C71 122.59(15) . . ?
C35 C31 C71 120.78(15) . . ?
C33 C32 C20 116.47(15) . . ?
C33 C32 C67 121.64(15) . . ?
C20 C32 C67 121.88(15) . . ?
C32 C33 C43 122.86(15) . . ?
C38 C34 C24 118.56(15) . . ?
C38 C34 C44 114.02(14) . . ?
C24 C34 C44 127.42(14) . . ?
C9 C35 C31 122.63(15) . . ?
C42 C36 C25 122.68(16) . . ?
C18 C37 C22 110.40(13) . . ?
C53 C38 C34 124.37(16) . . ?
C23 C39 C15 120.38(15) . . ?
C23 C39 C58 116.29(14) . . ?
C15 C39 C58 123.16(14) . . ?
C18 C40 C42 122.24(15) . . ?
C21 C41 C62 117.72(16) . . ?
C21 C41 C44 120.28(14) . . ?
C62 C41 C44 121.98(16) . . ?
C36 C42 C40 117.04(15) . . ?
C36 C42 C76 123.05(15) . . ?
C40 C42 C76 119.70(15) . . ?
C52 C43 C33 119.33(15) . . ?
C52 C43 C48 122.67(14) . . ?
C33 C43 C48 117.95(14) . . ?
C41 C44 C34 111.98(13) . . ?
C28 C45 C16 118.99(14) . . ?
C61 C46 C19 122.88(16) . . ?
C85 C47 C89 107.72(15) . . ?
C85 C47 C91 109.57(15) . . ?
C89 C47 C91 108.68(15) . . ?
C85 C47 C30 109.73(14) . . ?
C89 C47 C30 112.18(14) . . ?
C91 C47 C30 108.93(14) . . ?
C10 C48 C43 110.88(13) . . ?
C59 C49 C68 116.36(15) . . ?
C59 C49 C86 123.94(16) . . ?
C68 C49 C86 119.62(15) . . ?
C30 C50 C16 124.19(15) . . ?
C31 C51 C10 122.84(16) . . ?
C43 C52 C27 118.62(14) . . ?
C43 C52 N8 123.65(14) . . ?
C27 C52 N8 117.49(14) . . ?
C38 C53 C60 115.84(15) . . ?
C38 C53 C84 122.80(15) . . ?
C60 C53 C84 121.27(15) . . ?
C92 C54 C29 122.00(16) . . ?
N5 C55 C73 109.32(13) . . ?
C27 C56 C19 115.16(13) . . ?
C68 C57 C14 120.55(15) . . ?
C68 C57 C64 115.76(15) . . ?
C14 C57 C64 123.15(14) . . ?
C9 C58 C39 109.52(13) . . ?
C49 C59 C13 123.96(16) . . ?
C22 C60 C53 122.67(15) . . ?
C65 C61 C46 116.60(15) . . ?
C65 C61 C75 120.32(16) . . ?
C46 C61 C75 123.04(16) . . ?
C92 C62 C41 122.66(17) . . ?
N7 C63 C80 111.19(15) . . ?
C29 C64 C57 109.37(13) . . ?
C61 C65 C28 123.20(16) . . ?
C82 C66 C74 110.21(15) . . ?
C32 C67 C104 108.36(15) . . ?
C32 C67 C72 111.56(14) . . ?
C104 C67 C72 108.63(16) . . ?
C32 C67 C101 111.15(14) . . ?
C104 C67 C101 109.26(16) . . ?
C72 C67 C101 107.84(16) . . ?
C57 C68 C49 122.35(15) . . ?
N8 C69 C99 109.13(15) . . ?
N6 C70 C77 110.85(15) . . ?
C107 C71 C102 107.79(17) . . ?
C107 C71 C110 108.46(18) . . ?
C102 C71 C110 109.36(17) . . ?
C107 C71 C31 111.81(15) . . ?
C102 C71 C31 110.19(15) . . ?
C110 C71 C31 109.19(15) . . ?
C98 C73 C55 111.07(16) . . ?
N7 C74 C66 109.72(13) . . ?
C115 C75 C61 109.93(16) . . ?
C115 C75 C112 109.5(2) . . ?
C61 C75 C112 108.85(15) . . ?
C115 C75 C109 109.61(19) . . ?
C61 C75 C109 112.34(16) . . ?
C112 C75 C109 106.54(18) . . ?
C96 C76 C103 108.41(16) . . ?
C96 C76 C93 107.73(16) . . ?
C103 C76 C93 109.91(16) . . ?
C96 C76 C42 112.16(15) . . ?
C103 C76 C42 110.30(15) . . ?
C93 C76 C42 108.29(15) . . ?
C70 C77 C88 111.00(15) . . ?
C81 C78 C88 111.23(16) . . ?
N5 C79 C94 110.92(15) . . ?
C63 C80 C82 111.50(15) . . ?
N6 C81 C78 109.53(14) . . ?
C66 C82 C80 109.73(14) . . ?
N8 C83 C87 109.81(16) . . ?
C90 C84 C53 112.49(14) . . ?
C90 C84 C106 108.38(16) . . ?
C53 C84 C106 111.08(16) . . ?
C90 C84 C100 108.63(16) . . ?
C53 C84 C100 107.53(15) . . ?
C106 C84 C100 108.64(16) . . ?
C105 C86 C108 109.15(18) . . ?
C105 C86 C49 112.55(15) . . ?
C108 C86 C49 109.02(17) . . ?
C105 C86 C113 107.59(18) . . ?
C108 C86 C113 109.80(19) . . ?
C49 C86 C113 108.70(16) . . ?
C83 C87 C95 109.99(16) . . ?
C78 C88 C77 110.30(15) . . ?
C54 C92 C62 117.39(16) . . ?
C54 C92 C97 121.93(17) . . ?
C62 C92 C97 120.62(17) . . ?
C79 C94 C98 111.10(15) . . ?
C99 C95 C87 111.02(16) . . ?
C116 C97 C114 111.0(3) . . ?
C116 C97 C92 109.76(18) . . ?
C114 C97 C92 108.95(17) . . ?
C116 C97 C111 108.2(2) . . ?
C114 C97 C111 107.26(19) . . ?
C92 C97 C111 111.68(18) . . ?
C73 C98 C94 110.16(15) . . ?
C95 C99 C69 111.10(16) . . ?

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
O1 H1 N5 0.95 1.94 2.8454(18) 158.6 .
O3 H3 N6 0.92 2.02 2.9135(18) 165.0 .
O4 H4 N7 0.92 1.97 2.8691(19) 163.7 .

# start Validation Reply Form
_vrf_PLAT220_ar109               
;
PROBLEM:  High Ueq. Of C(methyl) atoms
RESPONSE: The terminal t-Bu residues reveal partial rotational disorder
;
_vrf_PLAT222_ar109               
;
PROBLEM:  High Ueq. Of C(methyl) atoms
RESPONSE: The terminal t-Bu residues reveal partial rotational disorder
;
_vrf_PLAT230_ar109               
;
PROBLEM:  High Ueq. Of C(methyl) atoms
RESPONSE: The terminal t-Bu residues reveal partial rotational disorder
;
# end Validation Reply Form
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.42
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.044
####################################################################### 
# 
# 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_ar113
_database_code_depnum_ccdc_archive 'CCDC 1427188'
_audit_update_record             
;
2015-09-24 deposited with the CCDC.
2015-10-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H58 Cl2 N4 O2 Ti, 2(C6 H6)'
_chemical_formula_sum            'C62 H70 Cl2 N4 O2 Ti'
_chemical_formula_weight         1022.02

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   14.4979(13)
_cell_length_b                   12.8321(12)
_cell_length_c                   30.827(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.131(4)
_cell_angle_gamma                90.00
_cell_volume                     5662.4(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    10964
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      28.35

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2168
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9127
_exptl_absorpt_correction_T_max  0.9441
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            56350
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         28.35
_reflns_number_total             14102
_reflns_number_gt                10964
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0388P)²+3.5880P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14102
_refine_ls_number_parameters     652
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.1044
_refine_ls_wR_factor_gt          0.0949
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.44563(2) 0.89249(2) 0.228169(9) 0.01081(7) Uani 1 1 d . . .
Cl1 Cl 0.43488(3) 1.04982(3) 0.269576(13) 0.01819(9) Uani 1 1 d . . .
Cl2 Cl 0.54638(3) 0.82201(3) 0.290019(13) 0.01933(9) Uani 1 1 d . . .
O1 O 0.45935(8) 0.76807(8) 0.20111(4) 0.0133(2) Uani 1 1 d . . .
O2 O 0.37074(8) 0.94962(8) 0.18111(4) 0.0134(2) Uani 1 1 d . . .
N1 N 0.60232(9) 0.96286(10) 0.17434(4) 0.0133(3) Uani 1 1 d . . .
N2 N 0.57250(9) 0.96507(10) 0.21395(4) 0.0137(3) Uani 1 1 d . . .
N3 N 0.25968(9) 0.78396(10) 0.24560(4) 0.0128(3) Uani 1 1 d . . .
N4 N 0.33493(10) 0.84284(11) 0.26280(4) 0.0149(3) Uani 1 1 d . . .
C0 C 0.32908(13) 0.85228(14) 0.30564(5) 0.0196(4) Uani 1 1 d . . .
H21 H 0.3722 0.8900 0.3263 0.023 Uiso 1 1 calc R . .
C1 C 0.77820(15) 0.44550(17) 0.06903(7) 0.0333(5) Uani 1 1 d . . .
H1 H 0.7560 0.3868 0.0517 0.040 Uiso 1 1 calc R . .
C2 C 0.84708(15) 0.43321(17) 0.10499(7) 0.0343(5) Uani 1 1 d . . .
H5 H 0.8724 0.3660 0.1123 0.041 Uiso 1 1 calc R . .
C3 C 0.87950(15) 0.51853(18) 0.13047(7) 0.0329(5) Uani 1 1 d . . .
H4 H 0.9271 0.5101 0.1552 0.040 Uiso 1 1 calc R . .
C4 C 0.84235(15) 0.61574(17) 0.11970(7) 0.0323(5) Uani 1 1 d . . .
H2 H 0.8641 0.6744 0.1372 0.039 Uiso 1 1 calc R . .
C5 C 0.74129(15) 0.54314(16) 0.05818(7) 0.0316(5) Uani 1 1 d . . .
H3 H 0.6939 0.5517 0.0334 0.038 Uiso 1 1 calc R . .
C6 C 0.77356(14) 0.62808(16) 0.08349(7) 0.0316(5) Uani 1 1 d . . .
H6 H 0.7485 0.6953 0.0760 0.038 Uiso 1 1 calc R . .
C7 C 0.49101(11) 0.66938(12) 0.19735(5) 0.0126(3) Uani 1 1 d . . .
C8 C 0.57650(11) 0.65265(12) 0.18234(5) 0.0134(3) Uani 1 1 d . . .
C9 C 0.63375(11) 0.74281(12) 0.16928(5) 0.0149(3) Uani 1 1 d . . .
H66 H 0.6514 0.7895 0.1948 0.018 Uiso 1 1 calc R . .
H65 H 0.6919 0.7159 0.1603 0.018 Uiso 1 1 calc R . .
C10 C 0.57874(11) 0.80374(12) 0.13169(5) 0.0139(3) Uani 1 1 d . . .
C11 C 0.55467(11) 0.90750(12) 0.13679(5) 0.0126(3) Uani 1 1 d . . .
C12 C 0.63942(12) 1.01563(13) 0.24088(6) 0.0175(3) Uani 1 1 d . . .
H9 H 0.6376 1.0294 0.2710 0.021 Uiso 1 1 calc R . .
C13 C 0.71172(12) 1.04515(13) 0.21891(6) 0.0193(4) Uani 1 1 d . . .
H8 H 0.7671 1.0818 0.2306 0.023 Uiso 1 1 calc R . .
C14 C 0.68597(11) 1.00994(13) 0.17658(6) 0.0173(3) Uani 1 1 d . . .
H7 H 0.7209 1.0175 0.1532 0.021 Uiso 1 1 calc R . .
C15 C 0.49027(11) 0.96009(12) 0.10659(5) 0.0137(3) Uani 1 1 d . . .
C16 C 0.45391(11) 1.06617(12) 0.11704(5) 0.0138(3) Uani 1 1 d . . .
H53 H 0.4659 1.1163 0.0942 0.017 Uiso 1 1 calc R . .
H52 H 0.4886 1.0904 0.1455 0.017 Uiso 1 1 calc R . .
C17 C 0.35052(11) 1.06558(12) 0.11946(5) 0.0126(3) Uani 1 1 d . . .
C18 C 0.31368(11) 1.00735(12) 0.15120(5) 0.0122(3) Uani 1 1 d . . .
C19 C 0.21639(11) 1.00525(12) 0.15094(5) 0.0127(3) Uani 1 1 d . . .
C20 C 0.15885(11) 1.06419(12) 0.11995(5) 0.0144(3) Uani 1 1 d . . .
H10 H 0.0934 1.0635 0.1203 0.017 Uiso 1 1 calc R . .
C21 C 0.19340(11) 1.12464(12) 0.08821(5) 0.0138(3) Uani 1 1 d . . .
C22 C 0.12541(12) 1.18563(13) 0.05430(5) 0.0168(3) Uani 1 1 d . . .
C23 C 0.17667(13) 1.24599(15) 0.02236(6) 0.0246(4) Uani 1 1 d . . .
H11 H 0.2200 1.2959 0.0388 0.037 Uiso 1 1 calc R . .
H12 H 0.1311 1.2836 0.0011 0.037 Uiso 1 1 calc R . .
H13 H 0.2117 1.1971 0.0067 0.037 Uiso 1 1 calc R . .
C24 C 0.05758(14) 1.10866(15) 0.02760(6) 0.0273(4) Uani 1 1 d . . .
H16 H 0.0931 1.0578 0.0132 0.041 Uiso 1 1 calc R . .
H15 H 0.0149 1.1469 0.0053 0.041 Uiso 1 1 calc R . .
H14 H 0.0216 1.0722 0.0473 0.041 Uiso 1 1 calc R . .
C25 C 0.06948(13) 1.26347(14) 0.07768(6) 0.0243(4) Uani 1 1 d . . .
H17 H 0.0362 1.2259 0.0982 0.037 Uiso 1 1 calc R . .
H18 H 0.0243 1.2999 0.0559 0.037 Uiso 1 1 calc R . .
H19 H 0.1122 1.3142 0.0939 0.037 Uiso 1 1 calc R . .
C26 C 0.28914(12) 1.12316(12) 0.08887(5) 0.0138(3) Uani 1 1 d . . .
H20 H 0.3143 1.1631 0.0676 0.017 Uiso 1 1 calc R . .
C27 C 0.17447(11) 0.93393(12) 0.18153(5) 0.0144(3) Uani 1 1 d . . .
H50 H 0.1066 0.9473 0.1789 0.017 Uiso 1 1 calc R . .
H51 H 0.2034 0.9478 0.2123 0.017 Uiso 1 1 calc R . .
C28 C 0.19097(11) 0.82144(12) 0.16997(5) 0.0131(3) Uani 1 1 d . . .
C29 C 0.24163(11) 0.75441(12) 0.20020(5) 0.0121(3) Uani 1 1 d . . .
C30 C 0.20901(12) 0.75674(13) 0.27676(5) 0.0164(3) Uani 1 1 d . . .
H25 H 0.1539 0.7155 0.2726 0.020 Uiso 1 1 calc R . .
C31 C 0.25184(12) 0.79980(14) 0.31577(6) 0.0196(4) Uani 1 1 d . . .
H24 H 0.2324 0.7946 0.3437 0.024 Uiso 1 1 calc R . .
C32 C 0.27470(11) 0.65891(12) 0.18841(5) 0.0134(3) Uani 1 1 d . . .
C33 C 0.34214(11) 0.59569(12) 0.22058(5) 0.0150(3) Uani 1 1 d . . .
H37 H 0.3152 0.5257 0.2237 0.018 Uiso 1 1 calc R . .
H38 H 0.3501 0.6300 0.2497 0.018 Uiso 1 1 calc R . .
C34 C 0.43693(11) 0.58369(12) 0.20647(5) 0.0138(3) Uani 1 1 d . . .
C35 C 0.47172(12) 0.48360(12) 0.20195(5) 0.0152(3) Uani 1 1 d . . .
H26 H 0.4355 0.4258 0.2086 0.018 Uiso 1 1 calc R . .
C36 C 0.55679(12) 0.46419(12) 0.18814(5) 0.0155(3) Uani 1 1 d . . .
C37 C 0.60755(12) 0.55106(12) 0.17799(5) 0.0152(3) Uani 1 1 d . . .
H27 H 0.6653 0.5404 0.1678 0.018 Uiso 1 1 calc R . .
C38 C 0.59223(12) 0.35361(13) 0.18192(6) 0.0212(4) Uani 1 1 d . . .
C39 C 0.69484(14) 0.34323(16) 0.20217(10) 0.0476(7) Uani 1 1 d . . .
H29 H 0.7020 0.3572 0.2338 0.071 Uiso 1 1 calc R . .
H28 H 0.7321 0.3934 0.1883 0.071 Uiso 1 1 calc R . .
H30 H 0.7164 0.2724 0.1974 0.071 Uiso 1 1 calc R . .
C40 C 0.58246(19) 0.33088(17) 0.13225(7) 0.0413(6) Uani 1 1 d . . .
H33 H 0.6195 0.3814 0.1185 0.062 Uiso 1 1 calc R . .
H31 H 0.5167 0.3365 0.1189 0.062 Uiso 1 1 calc R . .
H32 H 0.6050 0.2603 0.1278 0.062 Uiso 1 1 calc R . .
C41 C 0.53614(14) 0.27167(14) 0.20236(7) 0.0263(4) Uani 1 1 d . . .
H34 H 0.5634 0.2027 0.1993 0.039 Uiso 1 1 calc R . .
H36 H 0.4713 0.2723 0.1873 0.039 Uiso 1 1 calc R . .
H35 H 0.5377 0.2874 0.2336 0.039 Uiso 1 1 calc R . .
C42 C 0.24746(12) 0.62532(12) 0.14520(5) 0.0151(3) Uani 1 1 d . . .
H49 H 0.2691 0.5599 0.1365 0.018 Uiso 1 1 calc R . .
C43 C 0.18930(11) 0.68548(13) 0.11450(5) 0.0155(3) Uani 1 1 d . . .
C44 C 0.16407(11) 0.78447(13) 0.12752(5) 0.0153(3) Uani 1 1 d . . .
H39 H 0.1273 0.8279 0.1066 0.018 Uiso 1 1 calc R . .
C45 C 0.15360(13) 0.64843(14) 0.06774(6) 0.0214(4) Uani 1 1 d . . .
C46 C 0.17840(16) 0.72934(16) 0.03474(6) 0.0308(5) Uani 1 1 d . . .
H42 H 0.1476 0.7956 0.0392 0.046 Uiso 1 1 calc R . .
H41 H 0.1571 0.7045 0.0048 0.046 Uiso 1 1 calc R . .
H40 H 0.2462 0.7396 0.0392 0.046 Uiso 1 1 calc R . .
C47 C 0.19548(16) 0.54341(15) 0.05761(6) 0.0296(4) Uani 1 1 d . . .
H45 H 0.2637 0.5489 0.0619 0.044 Uiso 1 1 calc R . .
H43 H 0.1723 0.5240 0.0271 0.044 Uiso 1 1 calc R . .
H44 H 0.1772 0.4900 0.0773 0.044 Uiso 1 1 calc R . .
C48 C 0.04671(15) 0.63680(19) 0.06202(7) 0.0378(5) Uani 1 1 d . . .
H46 H 0.0304 0.5855 0.0831 0.057 Uiso 1 1 calc R . .
H47 H 0.0230 0.6134 0.0321 0.057 Uiso 1 1 calc R . .
H48 H 0.0186 0.7042 0.0673 0.057 Uiso 1 1 calc R . .
C49 C 0.45855(11) 0.91004(13) 0.06670(5) 0.0145(3) Uani 1 1 d . . .
H64 H 0.4148 0.9446 0.0453 0.017 Uiso 1 1 calc R . .
C50 C 0.48957(11) 0.81060(13) 0.05764(5) 0.0148(3) Uani 1 1 d . . .
C51 C 0.54592(12) 0.75706(13) 0.09162(5) 0.0155(3) Uani 1 1 d . . .
H54 H 0.5621 0.6866 0.0871 0.019 Uiso 1 1 calc R . .
C52 C 0.46975(12) 0.76189(13) 0.01173(5) 0.0180(3) Uani 1 1 d . . .
C53 C 0.43741(14) 0.64821(14) 0.01344(6) 0.0266(4) Uani 1 1 d . . .
H55 H 0.4859 0.6073 0.0316 0.040 Uiso 1 1 calc R . .
H56 H 0.4260 0.6194 -0.0164 0.040 Uiso 1 1 calc R . .
H57 H 0.3796 0.6454 0.0261 0.040 Uiso 1 1 calc R . .
C54 C 0.56213(13) 0.76424(15) -0.00691(6) 0.0250(4) Uani 1 1 d . . .
H59 H 0.5832 0.8365 -0.0085 0.037 Uiso 1 1 calc R . .
H60 H 0.5524 0.7336 -0.0364 0.037 Uiso 1 1 calc R . .
H58 H 0.6096 0.7241 0.0123 0.037 Uiso 1 1 calc R . .
C55 C 0.39636(13) 0.82295(15) -0.01971(6) 0.0245(4) Uani 1 1 d . . .
H62 H 0.3379 0.8261 -0.0075 0.037 Uiso 1 1 calc R . .
H63 H 0.3851 0.7879 -0.0483 0.037 Uiso 1 1 calc R . .
H61 H 0.4191 0.8938 -0.0234 0.037 Uiso 1 1 calc R . .
C56 C 0.59136(18) 0.4291(2) 0.35711(12) 0.0616(8) Uani 1 1 d . . .
H67 H 0.5663 0.3702 0.3407 0.074 Uiso 1 1 calc R . .
C57 C 0.58436(15) 0.5306(2) 0.33790(9) 0.0503(7) Uani 1 1 d . . .
H72 H 0.5546 0.5407 0.3085 0.060 Uiso 1 1 calc R . .
C58 C 0.62172(16) 0.61329(18) 0.36305(8) 0.0396(6) Uani 1 1 d . . .
H69 H 0.6171 0.6816 0.3510 0.048 Uiso 1 1 calc R . .
C59 C 0.66532(19) 0.5984(2) 0.40505(9) 0.0483(6) Uani 1 1 d . . .
H68 H 0.6914 0.6563 0.4219 0.058 Uiso 1 1 calc R . .
C60 C 0.63503(19) 0.4183(2) 0.39973(11) 0.0589(8) Uani 1 1 d . . .
H70 H 0.6393 0.3512 0.4129 0.071 Uiso 1 1 calc R . .
C61 C 0.6721(2) 0.5014(2) 0.42326(9) 0.0551(7) Uani 1 1 d . . .
H71 H 0.7029 0.4921 0.4526 0.066 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O2 1.8222(11) . ?
Ti1 O1 1.8267(11) . ?
Ti1 N4 2.1600(14) . ?
Ti1 N2 2.1676(14) . ?
Ti1 Cl2 2.3881(5) . ?
Ti1 Cl1 2.4067(5) . ?
O1 C7 1.3583(18) . ?
O2 C18 1.3570(18) . ?
N1 C14 1.347(2) . ?
N1 N2 1.3587(18) . ?
N1 C11 1.438(2) . ?
N2 C12 1.340(2) . ?
N3 C30 1.345(2) . ?
N3 N4 1.3633(19) . ?
N3 C29 1.433(2) . ?
N4 C0 1.342(2) . ?
C0 C31 1.384(2) . ?
C0 H21 0.9500 . ?
C1 C2 1.378(3) . ?
C1 C5 1.382(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.385(3) . ?
C2 H5 0.9500 . ?
C3 C4 1.378(3) . ?
C3 H4 0.9500 . ?
C4 C6 1.383(3) . ?
C4 H2 0.9500 . ?
C5 C6 1.378(3) . ?
C5 H3 0.9500 . ?
C6 H6 0.9500 . ?
C7 C34 1.405(2) . ?
C7 C8 1.407(2) . ?
C8 C37 1.393(2) . ?
C8 C9 1.515(2) . ?
C9 C10 1.516(2) . ?
C9 H66 0.9900 . ?
C9 H65 0.9900 . ?
C10 C51 1.387(2) . ?
C10 C11 1.392(2) . ?
C11 C15 1.385(2) . ?
C12 C13 1.388(2) . ?
C12 H9 0.9500 . ?
C13 C14 1.375(2) . ?
C13 H8 0.9500 . ?
C14 H7 0.9500 . ?
C15 C49 1.399(2) . ?
C15 C16 1.513(2) . ?
C16 C17 1.513(2) . ?
C16 H53 0.9900 . ?
C16 H52 0.9900 . ?
C17 C26 1.400(2) . ?
C17 C18 1.402(2) . ?
C18 C19 1.410(2) . ?
C19 C20 1.389(2) . ?
C19 C27 1.509(2) . ?
C20 C21 1.402(2) . ?
C20 H10 0.9500 . ?
C21 C26 1.385(2) . ?
C21 C22 1.533(2) . ?
C22 C23 1.534(2) . ?
C22 C24 1.537(2) . ?
C22 C25 1.536(2) . ?
C23 H11 0.9800 . ?
C23 H12 0.9800 . ?
C23 H13 0.9800 . ?
C24 H16 0.9800 . ?
C24 H15 0.9800 . ?
C24 H14 0.9800 . ?
C25 H17 0.9800 . ?
C25 H18 0.9800 . ?
C25 H19 0.9800 . ?
C26 H20 0.9500 . ?
C27 C28 1.515(2) . ?
C27 H50 0.9900 . ?
C27 H51 0.9900 . ?
C28 C29 1.389(2) . ?
C28 C44 1.389(2) . ?
C29 C32 1.385(2) . ?
C30 C31 1.379(2) . ?
C30 H25 0.9500 . ?
C31 H24 0.9500 . ?
C32 C42 1.396(2) . ?
C32 C33 1.513(2) . ?
C33 C34 1.514(2) . ?
C33 H37 0.9900 . ?
C33 H38 0.9900 . ?
C34 C35 1.395(2) . ?
C35 C36 1.389(2) . ?
C35 H26 0.9500 . ?
C36 C37 1.398(2) . ?
C36 C38 1.532(2) . ?
C37 H27 0.9500 . ?
C38 C41 1.525(3) . ?
C38 C39 1.525(3) . ?
C38 C40 1.543(3) . ?
C39 H29 0.9800 . ?
C39 H28 0.9800 . ?
C39 H30 0.9800 . ?
C40 H33 0.9800 . ?
C40 H31 0.9800 . ?
C40 H32 0.9800 . ?
C41 H34 0.9800 . ?
C41 H36 0.9800 . ?
C41 H35 0.9800 . ?
C42 C43 1.396(2) . ?
C42 H49 0.9500 . ?
C43 C44 1.398(2) . ?
C43 C45 1.528(2) . ?
C44 H39 0.9500 . ?
C45 C47 1.531(3) . ?
C45 C46 1.536(3) . ?
C45 C48 1.539(3) . ?
C46 H42 0.9800 . ?
C46 H41 0.9800 . ?
C46 H40 0.9800 . ?
C47 H45 0.9800 . ?
C47 H43 0.9800 . ?
C47 H44 0.9800 . ?
C48 H46 0.9800 . ?
C48 H47 0.9800 . ?
C48 H48 0.9800 . ?
C49 C50 1.396(2) . ?
C49 H64 0.9500 . ?
C50 C51 1.402(2) . ?
C50 C52 1.532(2) . ?
C51 H54 0.9500 . ?
C52 C55 1.536(2) . ?
C52 C53 1.536(2) . ?
C52 C54 1.539(2) . ?
C53 H55 0.9800 . ?
C53 H56 0.9800 . ?
C53 H57 0.9800 . ?
C54 H59 0.9800 . ?
C54 H60 0.9800 . ?
C54 H58 0.9800 . ?
C55 H62 0.9800 . ?
C55 H63 0.9800 . ?
C55 H61 0.9800 . ?
C56 C60 1.372(4) . ?
C56 C57 1.428(4) . ?
C56 H67 0.9500 . ?
C57 C58 1.373(4) . ?
C57 H72 0.9500 . ?
C58 C59 1.361(3) . ?
C58 H69 0.9500 . ?
C59 C61 1.363(3) . ?
C59 H68 0.9500 . ?
C60 C61 1.352(4) . ?
C60 H70 0.9500 . ?
C61 H71 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ti1 O1 94.73(5) . . ?
O2 Ti1 N4 96.69(5) . . ?
O1 Ti1 N4 96.38(5) . . ?
O2 Ti1 N2 94.80(5) . . ?
O1 Ti1 N2 97.23(5) . . ?
N4 Ti1 N2 161.37(5) . . ?
O2 Ti1 Cl2 178.38(4) . . ?
O1 Ti1 Cl2 86.35(4) . . ?
N4 Ti1 Cl2 84.37(4) . . ?
N2 Ti1 Cl2 83.86(4) . . ?
O2 Ti1 Cl1 90.24(4) . . ?
O1 Ti1 Cl1 175.01(4) . . ?
N4 Ti1 Cl1 82.50(4) . . ?
N2 Ti1 Cl1 82.84(4) . . ?
Cl2 Ti1 Cl1 88.690(18) . . ?
C7 O1 Ti1 156.44(10) . . ?
C18 O2 Ti1 169.28(10) . . ?
C14 N1 N2 110.91(13) . . ?
C14 N1 C11 125.20(14) . . ?
N2 N1 C11 123.57(13) . . ?
C12 N2 N1 105.33(13) . . ?
C12 N2 Ti1 129.56(12) . . ?
N1 N2 Ti1 125.03(10) . . ?
C30 N3 N4 111.11(13) . . ?
C30 N3 C29 126.36(14) . . ?
N4 N3 C29 122.50(13) . . ?
C0 N4 N3 105.14(13) . . ?
C0 N4 Ti1 128.88(11) . . ?
N3 N4 Ti1 125.64(10) . . ?
N4 C0 C31 110.96(15) . . ?
N4 C0 H21 124.5 . . ?
C31 C0 H21 124.5 . . ?
C2 C1 C5 120.1(2) . . ?
C2 C1 H1 119.9 . . ?
C5 C1 H1 119.9 . . ?
C1 C2 C3 120.2(2) . . ?
C1 C2 H5 119.9 . . ?
C3 C2 H5 119.9 . . ?
C4 C3 C2 119.62(19) . . ?
C4 C3 H4 120.2 . . ?
C2 C3 H4 120.2 . . ?
C3 C4 C6 120.1(2) . . ?
C3 C4 H2 119.9 . . ?
C6 C4 H2 119.9 . . ?
C6 C5 C1 119.73(19) . . ?
C6 C5 H3 120.1 . . ?
C1 C5 H3 120.1 . . ?
C5 C6 C4 120.2(2) . . ?
C5 C6 H6 119.9 . . ?
C4 C6 H6 119.9 . . ?
O1 C7 C34 120.39(14) . . ?
O1 C7 C8 119.85(14) . . ?
C34 C7 C8 119.70(14) . . ?
C37 C8 C7 119.32(15) . . ?
C37 C8 C9 119.36(15) . . ?
C7 C8 C9 121.29(14) . . ?
C10 C9 C8 110.68(13) . . ?
C10 C9 H66 109.5 . . ?
C8 C9 H66 109.5 . . ?
C10 C9 H65 109.5 . . ?
C8 C9 H65 109.5 . . ?
H66 C9 H65 108.1 . . ?
C51 C10 C11 117.20(15) . . ?
C51 C10 C9 121.51(15) . . ?
C11 C10 C9 121.21(15) . . ?
C15 C11 C10 122.99(15) . . ?
C15 C11 N1 119.14(14) . . ?
C10 C11 N1 117.81(14) . . ?
N2 C12 C13 111.01(15) . . ?
N2 C12 H9 124.5 . . ?
C13 C12 H9 124.5 . . ?
C14 C13 C12 105.13(15) . . ?
C14 C13 H8 127.4 . . ?
C12 C13 H8 127.4 . . ?
N1 C14 C13 107.61(15) . . ?
N1 C14 H7 126.2 . . ?
C13 C14 H7 126.2 . . ?
C11 C15 C49 117.38(15) . . ?
C11 C15 C16 121.05(14) . . ?
C49 C15 C16 121.55(14) . . ?
C15 C16 C17 112.81(13) . . ?
C15 C16 H53 109.0 . . ?
C17 C16 H53 109.0 . . ?
C15 C16 H52 109.0 . . ?
C17 C16 H52 109.0 . . ?
H53 C16 H52 107.8 . . ?
C26 C17 C18 118.64(15) . . ?
C26 C17 C16 119.53(14) . . ?
C18 C17 C16 121.82(14) . . ?
O2 C18 C17 120.43(14) . . ?
O2 C18 C19 119.66(14) . . ?
C17 C18 C19 119.86(14) . . ?
C20 C19 C18 119.00(15) . . ?
C20 C19 C27 120.18(15) . . ?
C18 C19 C27 120.66(14) . . ?
C19 C20 C21 122.64(15) . . ?
C19 C20 H10 118.7 . . ?
C21 C20 H10 118.7 . . ?
C26 C21 C20 116.77(14) . . ?
C26 C21 C22 123.47(14) . . ?
C20 C21 C22 119.74(15) . . ?
C21 C22 C23 111.77(14) . . ?
C21 C22 C24 108.94(13) . . ?
C23 C22 C24 108.35(15) . . ?
C21 C22 C25 110.01(14) . . ?
C23 C22 C25 108.56(14) . . ?
C24 C22 C25 109.17(15) . . ?
C22 C23 H11 109.5 . . ?
C22 C23 H12 109.5 . . ?
H11 C23 H12 109.5 . . ?
C22 C23 H13 109.5 . . ?
H11 C23 H13 109.5 . . ?
H12 C23 H13 109.5 . . ?
C22 C24 H16 109.5 . . ?
C22 C24 H15 109.5 . . ?
H16 C24 H15 109.5 . . ?
C22 C24 H14 109.5 . . ?
H16 C24 H14 109.5 . . ?
H15 C24 H14 109.5 . . ?
C22 C25 H17 109.5 . . ?
C22 C25 H18 109.5 . . ?
H17 C25 H18 109.5 . . ?
C22 C25 H19 109.5 . . ?
H17 C25 H19 109.5 . . ?
H18 C25 H19 109.5 . . ?
C21 C26 C17 123.05(15) . . ?
C21 C26 H20 118.5 . . ?
C17 C26 H20 118.5 . . ?
C19 C27 C28 109.68(13) . . ?
C19 C27 H50 109.7 . . ?
C28 C27 H50 109.7 . . ?
C19 C27 H51 109.7 . . ?
C28 C27 H51 109.7 . . ?
H50 C27 H51 108.2 . . ?
C29 C28 C44 117.39(15) . . ?
C29 C28 C27 121.25(14) . . ?
C44 C28 C27 121.07(14) . . ?
C32 C29 C28 122.68(15) . . ?
C32 C29 N3 118.23(14) . . ?
C28 C29 N3 119.08(14) . . ?
N3 C30 C31 107.32(15) . . ?
N3 C30 H25 126.3 . . ?
C31 C30 H25 126.3 . . ?
C30 C31 C0 105.47(15) . . ?
C30 C31 H24 127.3 . . ?
C0 C31 H24 127.3 . . ?
C29 C32 C42 117.78(15) . . ?
C29 C32 C33 121.13(14) . . ?
C42 C32 C33 121.02(14) . . ?
C32 C33 C34 112.83(13) . . ?
C32 C33 H37 109.0 . . ?
C34 C33 H37 109.0 . . ?
C32 C33 H38 109.0 . . ?
C34 C33 H38 109.0 . . ?
H37 C33 H38 107.8 . . ?
C35 C34 C7 118.59(15) . . ?
C35 C34 C33 118.80(14) . . ?
C7 C34 C33 122.61(14) . . ?
C36 C35 C34 123.26(15) . . ?
C36 C35 H26 118.4 . . ?
C34 C35 H26 118.4 . . ?
C35 C36 C37 116.73(15) . . ?
C35 C36 C38 122.42(15) . . ?
C37 C36 C38 120.78(15) . . ?
C8 C37 C36 122.36(15) . . ?
C8 C37 H27 118.8 . . ?
C36 C37 H27 118.8 . . ?
C41 C38 C39 108.67(17) . . ?
C41 C38 C36 112.06(15) . . ?
C39 C38 C36 110.76(14) . . ?
C41 C38 C40 107.98(15) . . ?
C39 C38 C40 108.64(19) . . ?
C36 C38 C40 108.64(15) . . ?
C38 C39 H29 109.5 . . ?
C38 C39 H28 109.5 . . ?
H29 C39 H28 109.5 . . ?
C38 C39 H30 109.5 . . ?
H29 C39 H30 109.5 . . ?
H28 C39 H30 109.5 . . ?
C38 C40 H33 109.5 . . ?
C38 C40 H31 109.5 . . ?
H33 C40 H31 109.5 . . ?
C38 C40 H32 109.5 . . ?
H33 C40 H32 109.5 . . ?
H31 C40 H32 109.5 . . ?
C38 C41 H34 109.5 . . ?
C38 C41 H36 109.5 . . ?
H34 C41 H36 109.5 . . ?
C38 C41 H35 109.5 . . ?
H34 C41 H35 109.5 . . ?
H36 C41 H35 109.5 . . ?
C43 C42 C32 121.67(15) . . ?
C43 C42 H49 119.2 . . ?
C32 C42 H49 119.2 . . ?
C42 C43 C44 117.72(15) . . ?
C42 C43 C45 123.03(15) . . ?
C44 C43 C45 119.25(15) . . ?
C28 C44 C43 122.27(15) . . ?
C28 C44 H39 118.9 . . ?
C43 C44 H39 118.9 . . ?
C43 C45 C47 112.37(15) . . ?
C43 C45 C46 109.55(15) . . ?
C47 C45 C46 108.54(15) . . ?
C43 C45 C48 108.80(15) . . ?
C47 C45 C48 108.43(16) . . ?
C46 C45 C48 109.09(17) . . ?
C45 C46 H42 109.5 . . ?
C45 C46 H41 109.5 . . ?
H42 C46 H41 109.5 . . ?
C45 C46 H40 109.5 . . ?
H42 C46 H40 109.5 . . ?
H41 C46 H40 109.5 . . ?
C45 C47 H45 109.5 . . ?
C45 C47 H43 109.5 . . ?
H45 C47 H43 109.5 . . ?
C45 C47 H44 109.5 . . ?
H45 C47 H44 109.5 . . ?
H43 C47 H44 109.5 . . ?
C45 C48 H46 109.5 . . ?
C45 C48 H47 109.5 . . ?
H46 C48 H47 109.5 . . ?
C45 C48 H48 109.5 . . ?
H46 C48 H48 109.5 . . ?
H47 C48 H48 109.5 . . ?
C50 C49 C15 121.62(15) . . ?
C50 C49 H64 119.2 . . ?
C15 C49 H64 119.2 . . ?
C49 C50 C51 117.81(15) . . ?
C49 C50 C52 122.60(15) . . ?
C51 C50 C52 119.47(15) . . ?
C10 C51 C50 122.05(15) . . ?
C10 C51 H54 119.0 . . ?
C50 C51 H54 119.0 . . ?
C50 C52 C55 112.61(14) . . ?
C50 C52 C53 111.69(14) . . ?
C55 C52 C53 108.75(15) . . ?
C50 C52 C54 106.86(14) . . ?
C55 C52 C54 108.13(14) . . ?
C53 C52 C54 108.66(15) . . ?
C52 C53 H55 109.5 . . ?
C52 C53 H56 109.5 . . ?
H55 C53 H56 109.5 . . ?
C52 C53 H57 109.5 . . ?
H55 C53 H57 109.5 . . ?
H56 C53 H57 109.5 . . ?
C52 C54 H59 109.5 . . ?
C52 C54 H60 109.5 . . ?
H59 C54 H60 109.5 . . ?
C52 C54 H58 109.5 . . ?
H59 C54 H58 109.5 . . ?
H60 C54 H58 109.5 . . ?
C52 C55 H62 109.5 . . ?
C52 C55 H63 109.5 . . ?
H62 C55 H63 109.5 . . ?
C52 C55 H61 109.5 . . ?
H62 C55 H61 109.5 . . ?
H63 C55 H61 109.5 . . ?
C60 C56 C57 118.8(3) . . ?
C60 C56 H67 120.6 . . ?
C57 C56 H67 120.6 . . ?
C58 C57 C56 118.3(2) . . ?
C58 C57 H72 120.8 . . ?
C56 C57 H72 120.8 . . ?
C59 C58 C57 120.7(2) . . ?
C59 C58 H69 119.7 . . ?
C57 C58 H69 119.7 . . ?
C58 C59 C61 120.8(3) . . ?
C58 C59 H68 119.6 . . ?
C61 C59 H68 119.6 . . ?
C61 C60 C56 121.1(2) . . ?
C61 C60 H70 119.4 . . ?
C56 C60 H70 119.4 . . ?
C60 C61 C59 120.2(3) . . ?
C60 C61 H71 119.9 . . ?
C59 C61 H71 119.9 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.35
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.058
####################################################################### 
# 
# 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_ar114
_database_code_depnum_ccdc_archive 'CCDC 1427189'
_audit_update_record             
;
2015-09-24 deposited with the CCDC.
2015-10-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H60 N4 O2'
_chemical_formula_sum            'C50 H60 N4 O2'
_chemical_formula_weight         749.02

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   21.9820(10)
_cell_length_b                   12.4352(6)
_cell_length_c                   19.3445(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 123.7240(10)
_cell_angle_gamma                90.00
_cell_volume                     4398.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    3393
_cell_measurement_theta_min      1.98
_cell_measurement_theta_max      25.04

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9756
_exptl_absorpt_correction_T_max  0.9895
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'ApexDuo. Bruker-AXS'
_diffrn_measurement_method       '1.0 deg. φ and ω scan'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16769
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         25.04
_reflns_number_total             3883
_reflns_number_gt                3393
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

 The terminal t-butyl residues are partly disordered.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1352P)²+13.2560P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3883
_refine_ls_number_parameters     266
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0705
_refine_ls_wR_factor_ref         0.2185
_refine_ls_wR_factor_gt          0.2080
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.92203(9) 0.45888(14) 0.23866(10) 0.0225(4) Uani 1 1 d . A .
H44 H 0.9548 0.489 0.282 0.027 Uiso 1 1 d . . .
N1 N 0.91207(10) 0.50623(16) 0.07331(12) 0.0201(5) Uani 1 1 d . . .
N2 N 0.96420(11) 0.57062(17) 0.13326(13) 0.0245(5) Uani 1 1 d . . .
C1 C 0.6763(3) 0.2989(4) 0.2856(3) 0.0790(14) Uani 1 1 d . A .
H24 H 0.6378 0.2643 0.2888 0.119 Uiso 1 1 calc R . .
H1 H 0.6554 0.3594 0.2467 0.119 Uiso 1 1 calc R . .
H23 H 0.7148 0.3253 0.3408 0.119 Uiso 1 1 calc R . .
C2 C 0.71151(19) 0.2102(3) 0.2527(2) 0.0606(12) Uani 1 1 d . . .
C3 C 0.77133(14) 0.2694(2) 0.24984(16) 0.0289(6) Uani 1 1 d . A .
C4 C 0.83462(13) 0.3053(2) 0.32289(15) 0.0250(6) Uani 1 1 d . . .
H27 H 0.8416 0.2867 0.3745 0.030 Uiso 1 1 calc R A .
C5 C 0.88806(12) 0.36690(18) 0.32410(14) 0.0190(5) Uani 1 1 d . A .
C6 C 0.95807(12) 0.39760(19) 0.40663(14) 0.0204(5) Uani 1 1 d . . .
H13 H 0.9657 0.4763 0.4085 0.024 Uiso 1 1 calc R A .
H20 H 0.9535 0.3780 0.4532 0.024 Uiso 1 1 calc R . .
C7 C 0.97666(12) 0.33909(19) 0.08387(13) 0.0181(5) Uani 1 1 d . . .
C8 C 0.91831(12) 0.39100(18) 0.08022(13) 0.0174(5) Uani 1 1 d . . .
C9 C 0.86649(12) 0.33236(19) 0.08499(13) 0.0174(5) Uani 1 1 d . . .
C10 C 0.80767(12) 0.38407(19) 0.09272(13) 0.0189(5) Uani 1 1 d . . .
H14 H 0.8101 0.4632 0.0888 0.023 Uiso 1 1 calc R . .
H25 H 0.7590 0.3600 0.0459 0.023 Uiso 1 1 calc R . .
C11 C 0.81621(12) 0.35588(18) 0.17381(14) 0.0180(5) Uani 1 1 d . A .
C12 C 0.76452(12) 0.29462(19) 0.17551(14) 0.0217(5) Uani 1 1 d . . .
H26 H 0.7232 0.2690 0.1246 0.026 Uiso 1 1 calc R A .
C13 C 0.64771(17) 0.1775(3) 0.1704(2) 0.0501(9) Uani 1 1 d . A .
H21 H 0.6126 0.1390 0.1774 0.075 Uiso 1 1 calc R . .
H22 H 0.6640 0.1303 0.1431 0.075 Uiso 1 1 calc R . .
H2 H 0.6243 0.2416 0.1361 0.075 Uiso 1 1 calc R . .
C14 C 0.86943(15) 0.6706(2) 0.03696(17) 0.0304(6) Uani 1 1 d . . .
H3 H 0.8395 0.7313 0.0086 0.036 Uiso 1 1 calc R . .
C15 C 0.93810(15) 0.6699(2) 0.11087(17) 0.0283(6) Uani 1 1 d . . .
H16 H 0.9633 0.7326 0.1416 0.034 Uiso 1 1 calc R . .
C17 C 0.87116(12) 0.22032(19) 0.08745(13) 0.0192(5) Uani 1 1 d . . .
H18 H 0.8364 0.1800 0.0912 0.023 Uiso 1 1 calc R . .
C18 C 0.92473(12) 0.16568(19) 0.08458(13) 0.0198(5) Uani 1 1 d . . .
C19 C 0.92754(13) 0.0422(2) 0.08097(16) 0.0269(6) Uani 1 1 d . . .
C20 C 0.87423(15) -0.0125(2) 0.09760(19) 0.0348(7) Uani 1 1 d . . .
H6 H 0.8852 0.0104 0.1519 0.052 Uiso 1 1 calc R . .
H4 H 0.8795 -0.0907 0.0974 0.052 Uiso 1 1 calc R . .
H5 H 0.8240 0.0080 0.0542 0.052 Uiso 1 1 calc R . .
C21 C 0.90667(17) 0.0109(2) -0.00655(18) 0.0381(7) Uani 1 1 d . . .
H7 H 0.8567 0.0349 -0.0478 0.057 Uiso 1 1 calc R . .
H8 H 0.9095 -0.0674 -0.0099 0.057 Uiso 1 1 calc R . .
H9 H 0.9405 0.0452 -0.0177 0.057 Uiso 1 1 calc R . .
C22 C 1.00541(15) 0.0019(2) 0.14603(19) 0.0373(7) Uani 1 1 d . . .
H11 H 1.0195 0.0247 0.2016 0.056 Uiso 1 1 calc R . .
H12 H 1.0397 0.0321 0.1339 0.056 Uiso 1 1 calc R . .
H10 H 1.0065 -0.0768 0.1440 0.056 Uiso 1 1 calc R . .
C23 C 0.97751(12) 0.22753(19) 0.08402(14) 0.0202(5) Uani 1 1 d . . .
H19 H 1.0155 0.1917 0.0837 0.024 Uiso 1 1 calc R . .
C24 C 0.87721(12) 0.39492(18) 0.24789(14) 0.0171(5) Uani 1 1 d . . .
C25 C 0.85413(14) 0.5649(2) 0.01372(15) 0.0258(6) Uani 1 1 d . . .
H17 H 0.8112 0.5376 -0.0348 0.031 Uiso 1 1 calc R . .
C16 C 0.7365(2) 0.1368(5) 0.3182(3) 0.066(2) Uani 1 1 d . . .
H16A H 0.6948 0.0984 0.3118 0.099 Uiso 1 1 calc R . .
H16B H 0.7625 0.1756 0.3712 0.099 Uiso 1 1 calc R . .
H16C H 0.7698 0.0851 0.3173 0.099 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C24 1.353(3) . ?
O1 H44 0.84 . ?
N1 N2 1.350(3) . ?
N1 C25 1.361(3) . ?
N1 C8 1.439(3) . ?
N2 C15 1.328(3) . ?
C1 C2 1.665(7) . ?
C1 H24 0.9800 . ?
C1 H1 0.9800 . ?
C1 H23 0.9800 . ?
C2 C16 1.402(5) . ?
C2 C13 1.479(4) . ?
C2 C3 1.535(4) . ?
C3 C4 1.396(3) . ?
C3 C12 1.396(4) . ?
C4 C5 1.392(3) . ?
C4 H27 0.9500 . ?
C5 C24 1.400(3) . ?
C5 C6 1.528(3) . ?
C6 C7 1.526(3) 2_755 ?
C6 H13 0.9900 . ?
C6 H20 0.9900 . ?
C7 C23 1.387(3) . ?
C7 C8 1.402(3) . ?
C7 C6 1.526(3) 2_755 ?
C8 C9 1.398(3) . ?
C9 C17 1.396(3) . ?
C9 C10 1.524(3) . ?
C10 C11 1.514(3) . ?
C10 H14 0.9900 . ?
C10 H25 0.9900 . ?
C11 C12 1.384(3) . ?
C11 C24 1.398(3) . ?
C12 H26 0.9500 . ?
C13 H21 0.9800 . ?
C13 H22 0.9800 . ?
C13 H2 0.9800 . ?
C14 C25 1.369(4) . ?
C14 C15 1.388(4) . ?
C14 H3 0.9500 . ?
C15 H16 0.9500 . ?
C17 C18 1.387(3) . ?
C17 H18 0.9500 . ?
C18 C23 1.397(3) . ?
C18 C19 1.539(3) . ?
C19 C20 1.536(4) . ?
C19 C21 1.538(4) . ?
C19 C22 1.541(4) . ?
C20 H6 0.9800 . ?
C20 H4 0.9800 . ?
C20 H5 0.9800 . ?
C21 H7 0.9800 . ?
C21 H8 0.9800 . ?
C21 H9 0.9800 . ?
C22 H11 0.9800 . ?
C22 H12 0.9800 . ?
C22 H10 0.9800 . ?
C23 H19 0.9500 . ?
C25 H17 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 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
C24 O1 H44 115 . . ?
N2 N1 C25 111.0(2) . . ?
N2 N1 C8 121.28(19) . . ?
C25 N1 C8 127.5(2) . . ?
C15 N2 N1 105.3(2) . . ?
C2 C1 H24 109.5 . . ?
C2 C1 H1 109.5 . . ?
H24 C1 H1 109.5 . . ?
C2 C1 H23 109.5 . . ?
H24 C1 H23 109.5 . . ?
H1 C1 H23 109.5 . . ?
C16 C2 C13 117.1(3) . . ?
C16 C2 C3 115.5(3) . . ?
C13 C2 C3 114.3(3) . . ?
C16 C2 C1 96.8(4) . . ?
C13 C2 C1 103.3(3) . . ?
C3 C2 C1 106.6(3) . . ?
C4 C3 C12 116.6(2) . . ?
C4 C3 C2 120.6(2) . . ?
C12 C3 C2 122.7(2) . . ?
C5 C4 C3 123.4(2) . . ?
C5 C4 H27 118.3 . . ?
C3 C4 H27 118.3 . . ?
C4 C5 C24 118.1(2) . . ?
C4 C5 C6 120.4(2) . . ?
C24 C5 C6 121.5(2) . . ?
C7 C6 C5 109.92(18) 2_755 . ?
C7 C6 H13 109.7 2_755 . ?
C5 C6 H13 109.7 . . ?
C7 C6 H20 109.7 2_755 . ?
C5 C6 H20 109.7 . . ?
H13 C6 H20 108.2 . . ?
C23 C7 C8 118.1(2) . . ?
C23 C7 C6 117.8(2) . 2_755 ?
C8 C7 C6 124.0(2) . 2_755 ?
C9 C8 C7 120.8(2) . . ?
C9 C8 N1 119.1(2) . . ?
C7 C8 N1 120.0(2) . . ?
C17 C9 C8 118.4(2) . . ?
C17 C9 C10 117.9(2) . . ?
C8 C9 C10 123.6(2) . . ?
C11 C10 C9 112.34(18) . . ?
C11 C10 H14 109.1 . . ?
C9 C10 H14 109.1 . . ?
C11 C10 H25 109.1 . . ?
C9 C10 H25 109.1 . . ?
H14 C10 H25 107.9 . . ?
C12 C11 C24 120.0(2) . . ?
C12 C11 C10 121.4(2) . . ?
C24 C11 C10 118.6(2) . . ?
C11 C12 C3 121.9(2) . . ?
C11 C12 H26 119.1 . . ?
C3 C12 H26 119.1 . . ?
C2 C13 H21 109.5 . . ?
C2 C13 H22 109.5 . . ?
H21 C13 H22 109.5 . . ?
C2 C13 H2 109.5 . . ?
H21 C13 H2 109.5 . . ?
H22 C13 H2 109.5 . . ?
C25 C14 C15 105.1(2) . . ?
C25 C14 H3 127.4 . . ?
C15 C14 H3 127.4 . . ?
N2 C15 C14 111.6(2) . . ?
N2 C15 H16 124.2 . . ?
C14 C15 H16 124.2 . . ?
C18 C17 C9 122.4(2) . . ?
C18 C17 H18 118.8 . . ?
C9 C17 H18 118.8 . . ?
C17 C18 C23 117.2(2) . . ?
C17 C18 C19 123.1(2) . . ?
C23 C18 C19 119.6(2) . . ?
C20 C19 C21 108.8(2) . . ?
C20 C19 C18 112.2(2) . . ?
C21 C19 C18 107.9(2) . . ?
C20 C19 C22 108.4(2) . . ?
C21 C19 C22 109.5(2) . . ?
C18 C19 C22 110.0(2) . . ?
C19 C20 H6 109.5 . . ?
C19 C20 H4 109.5 . . ?
H6 C20 H4 109.5 . . ?
C19 C20 H5 109.5 . . ?
H6 C20 H5 109.5 . . ?
H4 C20 H5 109.5 . . ?
C19 C21 H7 109.5 . . ?
C19 C21 H8 109.5 . . ?
H7 C21 H8 109.5 . . ?
C19 C21 H9 109.5 . . ?
H7 C21 H9 109.5 . . ?
H8 C21 H9 109.5 . . ?
C19 C22 H11 109.5 . . ?
C19 C22 H12 109.5 . . ?
H11 C22 H12 109.5 . . ?
C19 C22 H10 109.5 . . ?
H11 C22 H10 109.5 . . ?
H12 C22 H10 109.5 . . ?
C7 C23 C18 122.7(2) . . ?
C7 C23 H19 118.7 . . ?
C18 C23 H19 118.7 . . ?
O1 C24 C11 115.0(2) . . ?
O1 C24 C5 125.0(2) . . ?
C11 C24 C5 119.9(2) . . ?
N1 C25 C14 107.0(2) . . ?
N1 C25 H17 126.5 . . ?
C14 C25 H17 126.5 . . ?
C2 C16 H16A 109.5 . . ?
C2 C16 H16B 109.5 . . ?
C2 C16 H16C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H44 N2 0.84 1.91 2.728(3) 168 2_755

# start Validation Reply Form
_vrf_PLAT220_ar114               
;
PROBLEM
RESPONSE:  The t-butyl groups are partly disordered.
;
_vrf_PLAT230_ar114               
;
PROBLEM
RESPONSE:  The t-butyl groups are partly disordered.
;
# end Validation Reply Form
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.030
