# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_fb1314aa_a
_database_code_depnum_ccdc_archive 'CCDC 1529115'
_audit_update_record             
;
2017-01-22 deposited with the CCDC.
2017-10-16 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            'C18 H31.50 O1.12'
_chemical_formula_weight         265.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 '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'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_H-M_alt        'P 31'
_space_group_name_Hall           'P 31'

_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+1/3'
'-x+y, -x, z+2/3'

_cell_length_a                   23.112(4)
_cell_length_b                   23.112
_cell_length_c                   7.05320(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3262.78(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7106
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      23.16
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_F_000             1188
_exptl_transmission_factor_min   0.8630
_exptl_transmission_factor_max   0.9705
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.064
_shelx_estimated_absorpt_T_min   0.979
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker Photon CMOS Detector, D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29710
_diffrn_reflns_av_unetI/netI     0.0966
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.692
_diffrn_reflns_theta_max         26.419
_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 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8894
_reflns_number_gt                6809
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    0.997

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  'X-STEP32, Microsoft Word'
_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)+(0.0499P)²+10.2541P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0079(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 2388 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(8)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         8894
_refine_ls_number_parameters     477
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0958
_refine_ls_wR_factor_ref         0.2294
_refine_ls_wR_factor_gt          0.2161
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_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
C1 C 0.7699(4) 0.9216(4) 0.2225(10) 0.0188(15) Uani 1 1 d . . . . .
H1 H 0.8021 0.9399 0.1142 0.023 Uiso 1 1 calc R U . . .
C2 C 0.7984(4) 0.9780(4) 0.3714(11) 0.0242(17) Uani 1 1 d . . . . .
H2A H 0.7942 1.0162 0.3249 0.029 Uiso 1 1 calc R U . . .
H2B H 0.7727 0.9618 0.4908 0.029 Uiso 1 1 calc R U . . .
C3 C 0.8724(4) 1.0010(4) 0.4091(11) 0.0205(16) Uani 1 1 d . . . . .
H3A H 0.8982 1.0210 0.2916 0.025 Uiso 1 1 calc R U . . .
H3B H 0.8895 1.0363 0.5076 0.025 Uiso 1 1 calc R U . . .
C4 C 0.8845(4) 0.9453(4) 0.4733(10) 0.0194(16) Uani 1 1 d . . . . .
C5 C 0.8501(4) 0.8859(4) 0.3313(10) 0.0170(15) Uani 1 1 d . . . . .
H5 H 0.8736 0.9034 0.2077 0.020 Uiso 1 1 calc R U . . .
C6 C 0.7739(4) 0.8604(4) 0.2900(10) 0.0184(15) Uani 1 1 d . . . . .
C7 C 0.7518(4) 0.8095(4) 0.1280(11) 0.0250(17) Uani 1 1 d . . . . .
H7A H 0.7852 0.8281 0.0247 0.030 Uiso 1 1 calc R U . . .
H7B H 0.7503 0.7684 0.1747 0.030 Uiso 1 1 calc R U . . .
C8 C 0.6832(4) 0.7916(4) 0.0491(12) 0.0302(19) Uani 1 1 d . . . . .
H8A H 0.6726 0.7609 -0.0601 0.036 Uiso 1 1 calc R U . . .
H8B H 0.6489 0.7679 0.1477 0.036 Uiso 1 1 calc R U . . .
C9 C 0.6809(4) 0.8529(4) -0.0138(11) 0.0238(17) Uani 1 1 d . . . . .
H9A H 0.6347 0.8389 -0.0546 0.029 Uiso 1 1 calc R U . . .
H9B H 0.7103 0.8721 -0.1258 0.029 Uiso 1 1 calc R U . . .
C10 C 0.7022(4) 0.9084(4) 0.1378(10) 0.0197(16) Uani 1 1 d . . . . .
C11 C 0.8656(4) 0.9280(4) 0.6819(9) 0.0234(17) Uani 1 1 d . . . . .
H11A H 0.8194 0.9175 0.7014 0.035 Uiso 1 1 calc R U . . .
H11B H 0.8955 0.9663 0.7611 0.035 Uiso 1 1 calc R U . . .
H11C H 0.8699 0.8893 0.7167 0.035 Uiso 1 1 calc R U . . .
C12 C 0.8626(4) 0.8300(4) 0.3858(11) 0.0216(16) Uani 1 1 d . . . . .
H12 H 0.8438 0.8071 0.5013 0.026 Uiso 1 1 calc R U . . .
C13 C 0.8983(4) 0.8105(4) 0.2825(11) 0.0261(18) Uani 1 1 d . . . . .
H13A H 0.9177 0.8323 0.1663 0.031 Uiso 1 1 calc R U . . .
H13B H 0.9042 0.7748 0.3254 0.031 Uiso 1 1 calc R U . . .
C14 C 0.7300(4) 0.8255(4) 0.4650(11) 0.0262(18) Uani 1 1 d . . . . .
H14A H 0.6850 0.7922 0.4233 0.039 Uiso 1 1 calc R U . . .
H14B H 0.7274 0.8588 0.5452 0.039 Uiso 1 1 calc R U . . .
H14C H 0.7496 0.8034 0.5373 0.039 Uiso 1 1 calc R U . . .
C15 C 0.7118(4) 0.9702(4) 0.0335(14) 0.035(2) Uani 1 1 d . . . . .
H15A H 0.7499 0.9860 -0.0532 0.053 Uiso 1 1 calc R U . . .
H15B H 0.7204 1.0054 0.1254 0.053 Uiso 1 1 calc R U . . .
H15C H 0.6714 0.9591 -0.0391 0.053 Uiso 1 1 calc R U . . .
C16 C 0.6456(4) 0.8873(5) 0.2832(13) 0.036(2) Uani 1 1 d . . . . .
H16A H 0.6045 0.8783 0.2178 0.053 Uiso 1 1 calc R U . . .
H16B H 0.6580 0.9233 0.3756 0.053 Uiso 1 1 calc R U . . .
H16C H 0.6383 0.8468 0.3490 0.053 Uiso 1 1 calc R U . . .
C17 C 0.4395(4) 0.5423(4) 0.5236(11) 0.0260(18) Uani 1 1 d . . . . .
H17 H 0.4183 0.5546 0.4193 0.031 Uiso 1 1 calc R U . . .
C18 C 0.3842(4) 0.5071(4) 0.6697(12) 0.0293(19) Uani 1 1 d . . . . .
H18A H 0.4030 0.4989 0.7860 0.035 Uiso 1 1 calc R U . . .
H18B H 0.3498 0.4633 0.6189 0.035 Uiso 1 1 calc R U . . .
C19 C 0.3514(4) 0.5493(4) 0.7199(11) 0.0228(17) Uani 1 1 d . . . . .
H19A H 0.3277 0.5523 0.6067 0.027 Uiso 1 1 calc R U . . .
H19B H 0.3177 0.5260 0.8205 0.027 Uiso 1 1 calc R U . . .
C20 C 0.4003(4) 0.6191(4) 0.7867(11) 0.0213(17) Uani 1 1 d . . . . .
C21 C 0.4615(4) 0.6528(4) 0.6516(10) 0.0196(16) Uani 1 1 d . . . . .
H21 H 0.4429 0.6574 0.5282 0.023 Uiso 1 1 calc R U . . .
C22 C 0.4960(4) 0.6113(4) 0.6029(11) 0.0266(18) Uani 1 1 d . . . . .
C23 C 0.5473(5) 0.6482(5) 0.4452(12) 0.034(2) Uani 1 1 d . . . . .
H23A H 0.5845 0.6902 0.4968 0.040 Uiso 1 1 calc R U . . .
H23B H 0.5259 0.6601 0.3424 0.040 Uiso 1 1 calc R U . . .
C24 C 0.5754(5) 0.6054(5) 0.3628(15) 0.043(2) Uani 1 1 d . . . . .
H24A H 0.6071 0.6303 0.2594 0.052 Uiso 1 1 calc R U . . .
H24B H 0.6000 0.5965 0.4629 0.052 Uiso 1 1 calc R U . . .
C25 C 0.5191(5) 0.5392(6) 0.2863(13) 0.043(3) Uani 1 1 d . . . . .
H25A H 0.4992 0.5488 0.1748 0.051 Uiso 1 1 calc R U . . .
H25B H 0.5389 0.5123 0.2415 0.051 Uiso 1 1 calc R U . . .
C26 C 0.4631(5) 0.4970(5) 0.4257(12) 0.036(2) Uani 1 1 d . . . . .
C27 C 0.4175(4) 0.6189(4) 0.9951(10) 0.0217(17) Uani 1 1 d . . . . .
H27A H 0.4359 0.5892 1.0133 0.033 Uiso 1 1 calc R U . . .
H27B H 0.3771 0.6031 1.0720 0.033 Uiso 1 1 calc R U . . .
H27C H 0.4506 0.6643 1.0341 0.033 Uiso 1 1 calc R U . . .
C28 C 0.5111(4) 0.7238(4) 0.7105(11) 0.0273(18) Uani 1 1 d . . . . .
H28 H 0.5334 0.7297 0.8281 0.033 Uiso 1 1 calc R U . . .
C29 C 0.5259(4) 0.7779(4) 0.6136(12) 0.0297(19) Uani 1 1 d . . . . .
H29A H 0.5048 0.7745 0.4952 0.036 Uiso 1 1 calc R U . . .
H29B H 0.5577 0.8206 0.6619 0.036 Uiso 1 1 calc R U . . .
C30 C 0.5318(5) 0.6037(5) 0.7768(12) 0.034(2) Uani 1 1 d . . . . .
H30A H 0.5690 0.5980 0.7346 0.051 Uiso 1 1 calc R U . . .
H30B H 0.5003 0.5646 0.8505 0.051 Uiso 1 1 calc R U . . .
H30C H 0.5490 0.6438 0.8559 0.051 Uiso 1 1 calc R U . . .
C31 C 0.4063(6) 0.4433(5) 0.3137(15) 0.049(3) Uani 1 1 d . . . . .
H31A H 0.3856 0.4633 0.2365 0.073 Uiso 1 1 calc R U . . .
H31B H 0.3730 0.4105 0.4007 0.073 Uiso 1 1 calc R U . . .
H31C H 0.4233 0.4211 0.2308 0.073 Uiso 1 1 calc R U . . .
C32 C 0.4871(6) 0.4621(5) 0.5659(13) 0.046(3) Uani 1 1 d . . . . .
H32A H 0.4535 0.4398 0.6653 0.069 Uiso 1 1 calc R U . . .
H32B H 0.5294 0.4954 0.6236 0.069 Uiso 1 1 calc R U . . .
H32C H 0.4938 0.4289 0.4979 0.069 Uiso 1 1 calc R U . . .
C33 C 0.7475(4) 0.5624(4) 0.7709(10) 0.0158(15) Uani 1 1 d . . . . .
H33 H 0.7286 0.5289 0.8758 0.019 Uiso 1 1 calc R U . . .
C34 C 0.6924(4) 0.5361(3) 0.6216(10) 0.0170(15) Uani 1 1 d . . . . .
H34A H 0.7096 0.5630 0.5045 0.020 Uiso 1 1 calc R U . . .
H34B H 0.6545 0.5407 0.6685 0.020 Uiso 1 1 calc R U . . .
C35 C 0.6680(4) 0.4627(3) 0.5766(10) 0.0158(15) Uani 1 1 d . . . . .
H35A H 0.6468 0.4357 0.6914 0.019 Uiso 1 1 calc R U . . .
H35B H 0.6334 0.4477 0.4766 0.019 Uiso 1 1 calc R U . . .
C36 C 0.7233(3) 0.4494(3) 0.5104(9) 0.0133(14) Uani 1 1 d . . . . .
C37 C 0.7828(3) 0.4823(3) 0.6496(9) 0.0150(14) Uani 1 1 d . . . . .
H37 H 0.7652 0.4578 0.7720 0.018 Uiso 1 1 calc R U . . .
C38 C 0.8090(4) 0.5578(4) 0.6986(10) 0.0175(15) Uani 1 1 d . . . . .
C39 C 0.8592(4) 0.5785(4) 0.8589(11) 0.0212(16) Uani 1 1 d . . . . .
H39A H 0.9003 0.5804 0.8102 0.025 Uiso 1 1 calc R U . . .
H39B H 0.8405 0.5437 0.9587 0.025 Uiso 1 1 calc R U . . .
C40 C 0.8780(4) 0.6460(4) 0.9486(12) 0.0280(18) Uani 1 1 d . . . . .
H40A H 0.9081 0.6542 1.0578 0.034 Uiso 1 1 calc R U . . .
H40B H 0.9024 0.6820 0.8546 0.034 Uiso 1 1 calc R U . . .
C41 C 0.8168(4) 0.6479(4) 1.0148(11) 0.0254(18) Uani 1 1 d . . . . .
H41A H 0.8309 0.6935 1.0606 0.030 Uiso 1 1 calc R U . . .
H41B H 0.7972 0.6171 1.1238 0.030 Uiso 1 1 calc R U . . .
C42 C 0.7626(4) 0.6289(4) 0.8647(11) 0.0243(18) Uani 1 1 d . . . . .
C43 C 0.7414(4) 0.4679(4) 0.3013(10) 0.0211(16) Uani 1 1 d . . . . .
H43A H 0.7029 0.4390 0.2216 0.032 Uiso 1 1 calc R U . . .
H43B H 0.7792 0.4618 0.2674 0.032 Uiso 1 1 calc R U . . .
H43C H 0.7537 0.5146 0.2814 0.032 Uiso 1 1 calc R U . . .
C44 C 0.8388(4) 0.4701(4) 0.5956(10) 0.0203(16) Uani 1 1 d . . . . .
H44 H 0.8626 0.4907 0.4827 0.024 Uiso 1 1 calc R U . . .
C45 C 0.8573(4) 0.4337(4) 0.6911(12) 0.0280(18) Uani 1 1 d . . . . .
H45A H 0.8348 0.4123 0.8049 0.034 Uiso 1 1 calc R U . . .
H45B H 0.8933 0.4286 0.6468 0.034 Uiso 1 1 calc R U . . .
C46 C 0.8441(4) 0.6032(4) 0.5243(11) 0.0265(18) Uani 1 1 d . . . . .
H46A H 0.8694 0.5863 0.4556 0.040 Uiso 1 1 calc R U . . .
H46B H 0.8746 0.6489 0.5675 0.040 Uiso 1 1 calc R U . . .
H46C H 0.8103 0.6032 0.4400 0.040 Uiso 1 1 calc R U . . .
C47 C 0.6996(5) 0.6185(5) 0.9724(13) 0.035(2) Uani 1 1 d . . . . .
H47A H 0.6668 0.6169 0.8814 0.053 Uiso 1 1 calc R U . . .
H47B H 0.7121 0.6556 1.0608 0.053 Uiso 1 1 calc R U . . .
H47C H 0.6801 0.5764 1.0432 0.053 Uiso 1 1 calc R U . . .
C48 C 0.7816(5) 0.6873(4) 0.7251(12) 0.034(2) Uani 1 1 d . . . . .
H48A H 0.8255 0.7011 0.6697 0.051 Uiso 1 1 calc R U . . .
H48B H 0.7833 0.7251 0.7932 0.051 Uiso 1 1 calc R U . . .
H48C H 0.7482 0.6728 0.6241 0.051 Uiso 1 1 calc R U . . .
O1 O 0.9555(3) 0.9692(3) 0.4662(8) 0.0223(12) Uani 1 1 d . . . . .
H1A H 0.971(2) 0.990(5) 0.363(13) 0.033 Uiso 1 1 calc R U . . .
O2 O 0.3674(3) 0.6583(3) 0.7852(7) 0.0196(11) Uani 1 1 d . . . . .
H2 H 0.345(4) 0.652(3) 0.664(12) 0.029 Uiso 1 1 calc R U . . .
O3 O 0.6972(2) 0.3773(2) 0.5157(6) 0.0156(10) Uani 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
C1 C6 1.538(10) . ?
C1 C2 1.542(10) . ?
C1 C10 1.557(10) . ?
C1 H1 1.0000 . ?
C2 C3 1.539(11) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.518(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O1 1.447(9) . ?
C4 C11 1.529(10) . ?
C4 C5 1.558(10) . ?
C5 C12 1.508(10) . ?
C5 C6 1.580(10) . ?
C5 H5 1.0000 . ?
C6 C7 1.532(10) . ?
C6 C14 1.545(10) . ?
C7 C8 1.528(11) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.513(12) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.549(11) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C15 1.522(11) . ?
C10 C16 1.537(11) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.337(11) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9500 . ?
C13 H13B 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.522(12) . ?
C17 C26 1.563(11) . ?
C17 C22 1.574(12) . ?
C17 H17 1.0000 . ?
C18 C19 1.547(11) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.509(11) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 O2 1.445(9) . ?
C20 C27 1.523(10) . ?
C20 C21 1.554(10) . ?
C21 C28 1.517(11) . ?
C21 C22 1.559(11) . ?
C21 H21 1.0000 . ?
C22 C23 1.536(11) . ?
C22 C30 1.538(11) . ?
C23 C24 1.542(12) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.528(15) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.527(13) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C31 1.502(15) . ?
C26 C32 1.545(12) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.311(12) . ?
C28 H28 0.9500 . ?
C29 H29A 0.9500 . ?
C29 H29B 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.525(10) . ?
C33 C42 1.544(10) . ?
C33 C38 1.564(10) . ?
C33 H33 1.0000 . ?
C34 C35 1.529(9) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.529(10) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 O3 1.461(8) . ?
C36 C43 1.534(9) . ?
C36 C37 1.546(10) . ?
C37 C44 1.502(10) . ?
C37 C38 1.573(10) . ?
C37 H37 1.0000 . ?
C38 C39 1.516(10) . ?
C38 C46 1.556(10) . ?
C39 C40 1.531(11) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.511(12) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.527(11) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C48 1.547(11) . ?
C42 C47 1.551(12) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.307(12) . ?
C44 H44 0.9500 . ?
C45 H45A 0.9500 . ?
C45 H45B 0.9500 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
O1 H1A 0.85(9) . ?
O2 H2 0.98(9) . ?

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
C6 C1 C2 111.8(6) . . ?
C6 C1 C10 117.0(6) . . ?
C2 C1 C10 112.9(6) . . ?
C6 C1 H1 104.5 . . ?
C2 C1 H1 104.5 . . ?
C10 C1 H1 104.5 . . ?
C3 C2 C1 109.9(6) . . ?
C3 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
C3 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C4 C3 C2 113.7(6) . . ?
C4 C3 H3A 108.8 . . ?
C2 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
C2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
O1 C4 C3 108.7(6) . . ?
O1 C4 C11 104.7(6) . . ?
C3 C4 C11 111.0(6) . . ?
O1 C4 C5 107.2(6) . . ?
C3 C4 C5 109.1(6) . . ?
C11 C4 C5 115.8(6) . . ?
C12 C5 C4 111.1(6) . . ?
C12 C5 C6 112.5(6) . . ?
C4 C5 C6 115.4(6) . . ?
C12 C5 H5 105.6 . . ?
C4 C5 H5 105.6 . . ?
C6 C5 H5 105.6 . . ?
C7 C6 C1 109.0(6) . . ?
C7 C6 C14 108.3(6) . . ?
C1 C6 C14 113.7(6) . . ?
C7 C6 C5 107.8(6) . . ?
C1 C6 C5 106.4(6) . . ?
C14 C6 C5 111.5(6) . . ?
C8 C7 C6 112.5(7) . . ?
C8 C7 H7A 109.1 . . ?
C6 C7 H7A 109.1 . . ?
C8 C7 H7B 109.1 . . ?
C6 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C9 C8 C7 111.7(7) . . ?
C9 C8 H8A 109.3 . . ?
C7 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
C8 C9 C10 115.3(6) . . ?
C8 C9 H9A 108.4 . . ?
C10 C9 H9A 108.4 . . ?
C8 C9 H9B 108.4 . . ?
C10 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
C15 C10 C16 108.8(7) . . ?
C15 C10 C9 106.3(6) . . ?
C16 C10 C9 109.3(7) . . ?
C15 C10 C1 109.9(6) . . ?
C16 C10 C1 114.7(6) . . ?
C9 C10 C1 107.5(6) . . ?
C4 C11 H11A 109.5 . . ?
C4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C5 124.4(7) . . ?
C13 C12 H12 117.8 . . ?
C5 C12 H12 117.8 . . ?
C12 C13 H13A 120.0 . . ?
C12 C13 H13B 120.0 . . ?
H13A C13 H13B 120.0 . . ?
C6 C14 H14A 109.5 . . ?
C6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C16 H16A 109.5 . . ?
C10 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C10 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C26 114.9(7) . . ?
C18 C17 C22 110.5(6) . . ?
C26 C17 C22 116.5(7) . . ?
C18 C17 H17 104.5 . . ?
C26 C17 H17 104.5 . . ?
C22 C17 H17 104.5 . . ?
C17 C18 C19 111.3(7) . . ?
C17 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 113.8(7) . . ?
C20 C19 H19A 108.8 . . ?
C18 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
O2 C20 C19 108.7(6) . . ?
O2 C20 C27 103.2(6) . . ?
C19 C20 C27 110.8(7) . . ?
O2 C20 C21 108.3(6) . . ?
C19 C20 C21 110.6(6) . . ?
C27 C20 C21 114.8(6) . . ?
C28 C21 C20 112.3(6) . . ?
C28 C21 C22 112.6(7) . . ?
C20 C21 C22 116.4(6) . . ?
C28 C21 H21 104.7 . . ?
C20 C21 H21 104.7 . . ?
C22 C21 H21 104.7 . . ?
C23 C22 C30 109.3(7) . . ?
C23 C22 C21 107.9(6) . . ?
C30 C22 C21 111.3(7) . . ?
C23 C22 C17 108.9(7) . . ?
C30 C22 C17 112.9(7) . . ?
C21 C22 C17 106.4(6) . . ?
C22 C23 C24 111.9(7) . . ?
C22 C23 H23A 109.2 . . ?
C24 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
C24 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C25 C24 C23 110.8(8) . . ?
C25 C24 H24A 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
C26 C25 C24 115.9(8) . . ?
C26 C25 H25A 108.3 . . ?
C24 C25 H25A 108.3 . . ?
C26 C25 H25B 108.3 . . ?
C24 C25 H25B 108.3 . . ?
H25A C25 H25B 107.4 . . ?
C31 C26 C25 107.5(8) . . ?
C31 C26 C32 107.4(8) . . ?
C25 C26 C32 109.5(8) . . ?
C31 C26 C17 109.5(7) . . ?
C25 C26 C17 108.9(7) . . ?
C32 C26 C17 113.8(7) . . ?
C20 C27 H27A 109.5 . . ?
C20 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C20 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C21 125.8(8) . . ?
C29 C28 H28 117.1 . . ?
C21 C28 H28 117.1 . . ?
C28 C29 H29A 120.0 . . ?
C28 C29 H29B 120.0 . . ?
H29A C29 H29B 120.0 . . ?
C22 C30 H30A 109.5 . . ?
C22 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C22 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C26 C31 H31A 109.5 . . ?
C26 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C26 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C26 C32 H32A 109.5 . . ?
C26 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C26 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C42 114.9(6) . . ?
C34 C33 C38 110.7(6) . . ?
C42 C33 C38 116.5(6) . . ?
C34 C33 H33 104.4 . . ?
C42 C33 H33 104.4 . . ?
C38 C33 H33 104.4 . . ?
C33 C34 C35 110.9(6) . . ?
C33 C34 H34A 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 108.0 . . ?
C36 C35 C34 113.9(6) . . ?
C36 C35 H35A 108.8 . . ?
C34 C35 H35A 108.8 . . ?
C36 C35 H35B 108.8 . . ?
C34 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
O3 C36 C35 108.2(5) . . ?
O3 C36 C43 104.0(5) . . ?
C35 C36 C43 112.1(6) . . ?
O3 C36 C37 107.6(5) . . ?
C35 C36 C37 109.6(6) . . ?
C43 C36 C37 114.9(6) . . ?
C44 C37 C36 112.6(6) . . ?
C44 C37 C38 111.9(6) . . ?
C36 C37 C38 116.0(6) . . ?
C44 C37 H37 105.0 . . ?
C36 C37 H37 105.0 . . ?
C38 C37 H37 105.0 . . ?
C39 C38 C46 108.6(6) . . ?
C39 C38 C33 108.2(6) . . ?
C46 C38 C33 113.3(6) . . ?
C39 C38 C37 108.9(6) . . ?
C46 C38 C37 111.0(6) . . ?
C33 C38 C37 106.8(6) . . ?
C38 C39 C40 114.4(7) . . ?
C38 C39 H39A 108.7 . . ?
C40 C39 H39A 108.7 . . ?
C38 C39 H39B 108.7 . . ?
C40 C39 H39B 108.7 . . ?
H39A C39 H39B 107.6 . . ?
C41 C40 C39 111.3(6) . . ?
C41 C40 H40A 109.4 . . ?
C39 C40 H40A 109.4 . . ?
C41 C40 H40B 109.4 . . ?
C39 C40 H40B 109.4 . . ?
H40A C40 H40B 108.0 . . ?
C40 C41 C42 115.0(6) . . ?
C40 C41 H41A 108.5 . . ?
C42 C41 H41A 108.5 . . ?
C40 C41 H41B 108.5 . . ?
C42 C41 H41B 108.5 . . ?
H41A C41 H41B 107.5 . . ?
C41 C42 C33 109.1(6) . . ?
C41 C42 C48 110.9(7) . . ?
C33 C42 C48 114.9(6) . . ?
C41 C42 C47 106.0(6) . . ?
C33 C42 C47 109.1(6) . . ?
C48 C42 C47 106.4(7) . . ?
C36 C43 H43A 109.5 . . ?
C36 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C36 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C44 C37 125.4(7) . . ?
C45 C44 H44 117.3 . . ?
C37 C44 H44 117.3 . . ?
C44 C45 H45A 120.0 . . ?
C44 C45 H45B 120.0 . . ?
H45A C45 H45B 120.0 . . ?
C38 C46 H46A 109.5 . . ?
C38 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C38 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C42 C47 H47A 109.5 . . ?
C42 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C42 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C42 C48 H48A 109.5 . . ?
C42 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C42 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C4 O1 H1A 109.5 . . ?
C20 O2 H2 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
C6 C1 C2 C3 60.6(8) . . . . ?
C10 C1 C2 C3 -164.9(6) . . . . ?
C1 C2 C3 C4 -56.9(8) . . . . ?
C2 C3 C4 O1 168.3(6) . . . . ?
C2 C3 C4 C11 -77.1(8) . . . . ?
C2 C3 C4 C5 51.7(8) . . . . ?
O1 C4 C5 C12 60.6(7) . . . . ?
C3 C4 C5 C12 178.2(6) . . . . ?
C11 C4 C5 C12 -55.7(9) . . . . ?
O1 C4 C5 C6 -169.7(6) . . . . ?
C3 C4 C5 C6 -52.2(8) . . . . ?
C11 C4 C5 C6 73.9(8) . . . . ?
C2 C1 C6 C7 -174.1(6) . . . . ?
C10 C1 C6 C7 53.5(8) . . . . ?
C2 C1 C6 C14 64.9(8) . . . . ?
C10 C1 C6 C14 -67.5(8) . . . . ?
C2 C1 C6 C5 -58.1(8) . . . . ?
C10 C1 C6 C5 169.4(6) . . . . ?
C12 C5 C6 C7 -59.1(8) . . . . ?
C4 C5 C6 C7 172.0(6) . . . . ?
C12 C5 C6 C1 -175.9(6) . . . . ?
C4 C5 C6 C1 55.2(8) . . . . ?
C12 C5 C6 C14 59.7(8) . . . . ?
C4 C5 C6 C14 -69.2(8) . . . . ?
C1 C6 C7 C8 -53.7(9) . . . . ?
C14 C6 C7 C8 70.5(8) . . . . ?
C5 C6 C7 C8 -168.7(6) . . . . ?
C6 C7 C8 C9 55.3(9) . . . . ?
C7 C8 C9 C10 -54.1(10) . . . . ?
C8 C9 C10 C15 167.1(7) . . . . ?
C8 C9 C10 C16 -75.7(9) . . . . ?
C8 C9 C10 C1 49.4(9) . . . . ?
C6 C1 C10 C15 -165.4(7) . . . . ?
C2 C1 C10 C15 62.7(8) . . . . ?
C6 C1 C10 C16 71.5(9) . . . . ?
C2 C1 C10 C16 -60.4(9) . . . . ?
C6 C1 C10 C9 -50.2(8) . . . . ?
C2 C1 C10 C9 177.9(6) . . . . ?
C4 C5 C12 C13 -114.2(8) . . . . ?
C6 C5 C12 C13 114.7(8) . . . . ?
C26 C17 C18 C19 -165.0(7) . . . . ?
C22 C17 C18 C19 60.6(8) . . . . ?
C17 C18 C19 C20 -55.2(9) . . . . ?
C18 C19 C20 O2 166.3(6) . . . . ?
C18 C19 C20 C27 -80.9(8) . . . . ?
C18 C19 C20 C21 47.6(8) . . . . ?
O2 C20 C21 C28 59.4(8) . . . . ?
C19 C20 C21 C28 178.4(6) . . . . ?
C27 C20 C21 C28 -55.3(9) . . . . ?
O2 C20 C21 C22 -168.7(6) . . . . ?
C19 C20 C21 C22 -49.8(9) . . . . ?
C27 C20 C21 C22 76.5(9) . . . . ?
C28 C21 C22 C23 -57.1(9) . . . . ?
C20 C21 C22 C23 171.1(7) . . . . ?
C28 C21 C22 C30 62.8(9) . . . . ?
C20 C21 C22 C30 -68.9(9) . . . . ?
C28 C21 C22 C17 -173.9(6) . . . . ?
C20 C21 C22 C17 54.4(8) . . . . ?
C18 C17 C22 C23 -174.6(7) . . . . ?
C26 C17 C22 C23 51.8(9) . . . . ?
C18 C17 C22 C30 63.9(9) . . . . ?
C26 C17 C22 C30 -69.7(9) . . . . ?
C18 C17 C22 C21 -58.5(8) . . . . ?
C26 C17 C22 C21 167.9(6) . . . . ?
C30 C22 C23 C24 68.7(10) . . . . ?
C21 C22 C23 C24 -170.1(8) . . . . ?
C17 C22 C23 C24 -55.1(10) . . . . ?
C22 C23 C24 C25 57.4(10) . . . . ?
C23 C24 C25 C26 -55.0(11) . . . . ?
C24 C25 C26 C31 167.1(8) . . . . ?
C24 C25 C26 C32 -76.5(10) . . . . ?
C24 C25 C26 C17 48.6(10) . . . . ?
C18 C17 C26 C31 63.7(9) . . . . ?
C22 C17 C26 C31 -164.8(7) . . . . ?
C18 C17 C26 C25 -179.0(7) . . . . ?
C22 C17 C26 C25 -47.5(10) . . . . ?
C18 C17 C26 C32 -56.5(11) . . . . ?
C22 C17 C26 C32 75.0(10) . . . . ?
C20 C21 C28 C29 -114.6(9) . . . . ?
C22 C21 C28 C29 111.6(9) . . . . ?
C42 C33 C34 C35 -164.6(6) . . . . ?
C38 C33 C34 C35 60.8(8) . . . . ?
C33 C34 C35 C36 -56.7(8) . . . . ?
C34 C35 C36 O3 166.8(5) . . . . ?
C34 C35 C36 C43 -79.1(7) . . . . ?
C34 C35 C36 C37 49.8(8) . . . . ?
O3 C36 C37 C44 61.5(7) . . . . ?
C35 C36 C37 C44 178.9(6) . . . . ?
C43 C36 C37 C44 -53.8(8) . . . . ?
O3 C36 C37 C38 -167.7(5) . . . . ?
C35 C36 C37 C38 -50.3(7) . . . . ?
C43 C36 C37 C38 77.0(8) . . . . ?
C34 C33 C38 C39 -174.8(6) . . . . ?
C42 C33 C38 C39 51.4(8) . . . . ?
C34 C33 C38 C46 64.7(8) . . . . ?
C42 C33 C38 C46 -69.1(8) . . . . ?
C34 C33 C38 C37 -57.8(7) . . . . ?
C42 C33 C38 C37 168.4(6) . . . . ?
C44 C37 C38 C39 -57.9(7) . . . . ?
C36 C37 C38 C39 170.9(6) . . . . ?
C44 C37 C38 C46 61.5(8) . . . . ?
C36 C37 C38 C46 -69.6(8) . . . . ?
C44 C37 C38 C33 -174.6(6) . . . . ?
C36 C37 C38 C33 54.3(7) . . . . ?
C46 C38 C39 C40 71.1(8) . . . . ?
C33 C38 C39 C40 -52.3(8) . . . . ?
C37 C38 C39 C40 -168.0(6) . . . . ?
C38 C39 C40 C41 54.7(9) . . . . ?
C39 C40 C41 C42 -53.1(9) . . . . ?
C40 C41 C42 C33 50.0(9) . . . . ?
C40 C41 C42 C48 -77.5(9) . . . . ?
C40 C41 C42 C47 167.5(7) . . . . ?
C34 C33 C42 C41 178.1(6) . . . . ?
C38 C33 C42 C41 -50.0(8) . . . . ?
C34 C33 C42 C48 -56.7(10) . . . . ?
C38 C33 C42 C48 75.2(9) . . . . ?
C34 C33 C42 C47 62.7(8) . . . . ?
C38 C33 C42 C47 -165.4(6) . . . . ?
C36 C37 C44 C45 -112.3(8) . . . . ?
C38 C37 C44 C45 114.8(8) . . . . ?

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
C19 H19A O2 0.99 2.63 3.454(9) 140.2 3_564
O1 H1A O1 0.85 1.98 2.833(5) 175.4 3_674

_refine_diff_density_max         0.437
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.081


#END===============================================
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: EtOAc / Hexan'
####################################################################### 
# 
# 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_FB9535Ab
_database_code_depnum_ccdc_archive 'CCDC 1529118'
_audit_update_record             
;
2017-01-22 deposited with the CCDC.
2017-10-16 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 H53 O2.50'
_chemical_formula_weight         453.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0192 0.0096 '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'
O O 0.0517 0.0336 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   6.52639(6)
_cell_length_b                   61.4400(5)
_cell_length_c                   7.08782(6)
_cell_angle_alpha                90
_cell_angle_beta                 113.2304(4)
_cell_angle_gamma                90
_cell_volume                     2611.67(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9876
_cell_measurement_theta_min      2.88
_cell_measurement_theta_max      66.71
_exptl_crystal_description       platelet
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_F_000             1012
_exptl_transmission_factor_min   0.8223
_exptl_transmission_factor_max   0.8955
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.513
_shelx_estimated_absorpt_T_min   0.883
_shelx_estimated_absorpt_T_max   0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
__diffrn_source                  'sealed tube'
_diffrn_measurement_device_type  'Bruker Photon CMOS Detector, D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26244
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -73
_diffrn_reflns_limit_k_max       73
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.877
_diffrn_reflns_theta_max         66.729
_diffrn_reflns_theta_full        66.729
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             9097
_reflns_number_gt                7869
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.981
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.995

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  'Microsoft Word'
_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)+(0.0767P)²+0.7127P] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.2(3)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         9097
_refine_ls_number_parameters     614
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1444
_refine_ls_wR_factor_gt          0.1389
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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
C1 C 0.7589(7) 0.43121(7) 0.5864(7) 0.0182(9) Uani 1 1 d . . . . .
H1A H 0.7675 0.4265 0.7228 0.022 Uiso 1 1 calc R U . . .
H1B H 0.8720 0.4229 0.5553 0.022 Uiso 1 1 calc R U . . .
C2 C 0.8142(7) 0.45558(7) 0.5950(7) 0.0183(9) Uani 1 1 d . . . . .
H2A H 0.7114 0.4637 0.6409 0.022 Uiso 1 1 calc R U . . .
H2B H 0.9680 0.4580 0.6972 0.022 Uiso 1 1 calc R U . . .
C3 C 0.7949(7) 0.46428(6) 0.3895(7) 0.0185(9) Uani 1 1 d . . . . .
H3 H 0.9089 0.4563 0.3545 0.022 Uiso 1 1 calc R U . . .
C4 C 0.5694(7) 0.45996(7) 0.2121(7) 0.0176(9) Uani 1 1 d . . . . .
C5 C 0.5138(7) 0.43528(7) 0.2158(6) 0.0159(9) Uani 1 1 d . . . . .
H5 H 0.6358 0.4276 0.1907 0.019 Uiso 1 1 calc R U . . .
C6 C 0.5247(7) 0.42581(6) 0.4230(6) 0.0150(9) Uani 1 1 d . . . . .
C7 C 0.4996(7) 0.40031(7) 0.3950(6) 0.0156(9) Uani 1 1 d . . . . .
H7 H 0.6245 0.3956 0.3561 0.019 Uiso 1 1 calc R U . . .
C8 C 0.2844(7) 0.39323(7) 0.2142(7) 0.0182(9) Uani 1 1 d . . . . .
C9 C 0.2828(7) 0.40358(7) 0.0177(6) 0.0181(9) Uani 1 1 d . . . . .
H9A H 0.1433 0.3996 -0.0990 0.022 Uiso 1 1 calc R U . . .
H9B H 0.4095 0.3978 -0.0107 0.022 Uiso 1 1 calc R U . . .
C10 C 0.3002(7) 0.42846(7) 0.0357(7) 0.0186(9) Uani 1 1 d . . . . .
H10A H 0.3002 0.4347 -0.0933 0.022 Uiso 1 1 calc R U . . .
H10B H 0.1691 0.4343 0.0561 0.022 Uiso 1 1 calc R U . . .
C11 C 0.5329(8) 0.38751(7) 0.5916(6) 0.0183(9) Uani 1 1 d . . . . .
H11A H 0.3852 0.3843 0.5940 0.022 Uiso 1 1 calc R U . . .
H11B H 0.6166 0.3967 0.7125 0.022 Uiso 1 1 calc R U . . .
C12 C 0.6595(8) 0.36597(7) 0.6083(6) 0.0201(10) Uani 1 1 d . . . . .
H12A H 0.7167 0.3610 0.7527 0.024 Uiso 1 1 calc R U . . .
H12B H 0.7899 0.3688 0.5735 0.024 Uiso 1 1 calc R U . . .
C13 C 0.5202(7) 0.34748(6) 0.4694(7) 0.0159(9) Uani 1 1 d . . . . .
H13 H 0.3836 0.3466 0.5003 0.019 Uiso 1 1 calc R U . . .
C14 C 0.4313(7) 0.35299(7) 0.2370(7) 0.0182(9) Uani 1 1 d . . . . .
C15 C 0.2836(8) 0.33413(7) 0.1121(7) 0.0210(10) Uani 1 1 d . . . . .
H15A H 0.1441 0.3338 0.1360 0.025 Uiso 1 1 calc R U . . .
H15B H 0.2430 0.3369 -0.0359 0.025 Uiso 1 1 calc R U . . .
C16 C 0.3972(8) 0.31190(7) 0.1673(7) 0.0227(10) Uani 1 1 d . . . . .
H16A H 0.2955 0.3004 0.0830 0.027 Uiso 1 1 calc R U . . .
H16B H 0.5338 0.3118 0.1385 0.027 Uiso 1 1 calc R U . . .
C17 C 0.4573(7) 0.30734(7) 0.3950(7) 0.0163(9) Uani 1 1 d . . . . .
H17 H 0.3186 0.3108 0.4169 0.020 Uiso 1 1 calc R U . . .
C18 C 0.6335(7) 0.32437(7) 0.5301(7) 0.0168(9) Uani 1 1 d . . . . .
C19 C 0.6748(7) 0.31981(7) 0.7571(7) 0.0203(10) Uani 1 1 d . . . . .
H19A H 0.7975 0.3293 0.8463 0.024 Uiso 1 1 calc R U . . .
H19B H 0.5390 0.3237 0.7796 0.024 Uiso 1 1 calc R U . . .
C20 C 0.7342(8) 0.29615(7) 0.8207(7) 0.0236(10) Uani 1 1 d . . . . .
H20A H 0.8774 0.2925 0.8108 0.028 Uiso 1 1 calc R U . . .
H20B H 0.7537 0.2943 0.9655 0.028 Uiso 1 1 calc R U . . .
C21 C 0.5546(8) 0.28069(7) 0.6861(7) 0.0243(10) Uani 1 1 d . . . . .
H21A H 0.4159 0.2835 0.7075 0.029 Uiso 1 1 calc R U . . .
H21B H 0.6019 0.2656 0.7298 0.029 Uiso 1 1 calc R U . . .
C22 C 0.5046(8) 0.28286(7) 0.4562(7) 0.0230(10) Uani 1 1 d . . . . .
C23 C 0.3897(8) 0.47533(7) 0.2224(7) 0.0231(10) Uani 1 1 d . . . . .
H23A H 0.4220 0.4902 0.1931 0.035 Uiso 1 1 calc R U . . .
H23B H 0.3882 0.4747 0.3601 0.035 Uiso 1 1 calc R U . . .
H23C H 0.2437 0.4709 0.1207 0.035 Uiso 1 1 calc R U . . .
C24 C 0.6017(9) 0.46472(7) 0.0124(8) 0.0280(11) Uani 1 1 d . . . . .
H24A H 0.4557 0.4661 -0.1016 0.042 Uiso 1 1 calc R U . . .
H24B H 0.6852 0.4528 -0.0157 0.042 Uiso 1 1 calc R U . . .
H24C H 0.6848 0.4783 0.0274 0.042 Uiso 1 1 calc R U . . .
C25 C 0.3523(8) 0.43538(7) 0.4989(7) 0.0213(10) Uani 1 1 d . . . . .
H25A H 0.2145 0.4388 0.3807 0.032 Uiso 1 1 calc R U . . .
H25B H 0.4123 0.4487 0.5775 0.032 Uiso 1 1 calc R U . . .
H25C H 0.3204 0.4247 0.5866 0.032 Uiso 1 1 calc R U . . .
C26 C 0.0632(7) 0.39850(7) 0.2342(8) 0.0245(10) Uani 1 1 d . . . . .
H26A H 0.0373 0.4142 0.2216 0.037 Uiso 1 1 calc R U . . .
H26B H 0.0709 0.3936 0.3684 0.037 Uiso 1 1 calc R U . . .
H26C H -0.0595 0.3910 0.1253 0.037 Uiso 1 1 calc R U . . .
C27 C 0.6061(8) 0.35819(7) 0.1523(7) 0.0199(9) Uani 1 1 d . . . . .
H27A H 0.5331 0.3640 0.0130 0.030 Uiso 1 1 calc R U . . .
H27B H 0.6873 0.3449 0.1488 0.030 Uiso 1 1 calc R U . . .
H27C H 0.7106 0.3690 0.2405 0.030 Uiso 1 1 calc R U . . .
C28 C 0.8606(7) 0.32339(7) 0.5080(7) 0.0222(10) Uani 1 1 d . . . . .
H28A H 0.8358 0.3195 0.3666 0.033 Uiso 1 1 calc R U . . .
H28B H 0.9561 0.3124 0.6024 0.033 Uiso 1 1 calc R U . . .
H28C H 0.9334 0.3376 0.5411 0.033 Uiso 1 1 calc R U . . .
C29 C 0.6930(9) 0.27283(7) 0.4081(8) 0.0275(11) Uani 1 1 d . . . . .
H29A H 0.6649 0.2754 0.2635 0.041 Uiso 1 1 calc R U . . .
H29B H 0.6997 0.2571 0.4345 0.041 Uiso 1 1 calc R U . . .
H29C H 0.8351 0.2795 0.4955 0.041 Uiso 1 1 calc R U . . .
C30 C 0.2893(9) 0.26986(7) 0.3385(8) 0.0264(11) Uani 1 1 d . . . . .
H30A H 0.2620 0.2694 0.1923 0.040 Uiso 1 1 calc R U . . .
H30B H 0.1632 0.2769 0.3556 0.040 Uiso 1 1 calc R U . . .
H30C H 0.3059 0.2550 0.3928 0.040 Uiso 1 1 calc R U . . .
C31 C 0.6789(8) 0.57399(7) 0.6167(7) 0.0196(10) Uani 1 1 d . . . . .
H31A H 0.5646 0.5843 0.5287 0.023 Uiso 1 1 calc R U . . .
H31B H 0.8152 0.5761 0.5895 0.023 Uiso 1 1 calc R U . . .
C32 C 0.5944(7) 0.55076(7) 0.5581(7) 0.0197(10) Uani 1 1 d . . . . .
H32A H 0.4515 0.5490 0.5744 0.024 Uiso 1 1 calc R U . . .
H32B H 0.5657 0.5483 0.4118 0.024 Uiso 1 1 calc R U . . .
C33 C 0.7600(8) 0.53398(7) 0.6889(7) 0.0220(10) Uani 1 1 d . . . . .
H33 H 0.8990 0.5360 0.6635 0.026 Uiso 1 1 calc R U . . .
C34 C 0.8260(8) 0.53729(7) 0.9219(7) 0.0217(10) Uani 1 1 d . . . . .
C35 C 0.8965(7) 0.56156(7) 0.9750(7) 0.0174(9) Uani 1 1 d . . . . .
H35 H 1.0318 0.5633 0.9432 0.021 Uiso 1 1 calc R U . . .
C36 C 0.7322(7) 0.57934(7) 0.8434(7) 0.0173(9) Uani 1 1 d . . . . .
C37 C 0.8597(7) 0.60179(7) 0.8988(7) 0.0162(9) Uani 1 1 d . . . . .
H37 H 0.9912 0.5998 0.8615 0.019 Uiso 1 1 calc R U . . .
C38 C 0.9632(7) 0.60753(7) 1.1306(7) 0.0184(9) Uani 1 1 d . . . . .
C39 C 1.1032(7) 0.58831(7) 1.2499(7) 0.0186(9) Uani 1 1 d . . . . .
H39A H 1.1555 0.5914 1.3987 0.022 Uiso 1 1 calc R U . . .
H39B H 1.2364 0.5869 1.2167 0.022 Uiso 1 1 calc R U . . .
C40 C 0.9775(8) 0.56668(7) 1.2037(7) 0.0217(10) Uani 1 1 d . . . . .
H40A H 1.0770 0.5549 1.2845 0.026 Uiso 1 1 calc R U . . .
H40B H 0.8484 0.5675 1.2436 0.026 Uiso 1 1 calc R U . . .
C41 C 0.7258(7) 0.62053(7) 0.7582(6) 0.0188(9) Uani 1 1 d . . . . .
H41A H 0.6646 0.6153 0.6145 0.023 Uiso 1 1 calc R U . . .
H41B H 0.5980 0.6241 0.7946 0.023 Uiso 1 1 calc R U . . .
C42 C 0.8576(8) 0.64132(7) 0.7695(7) 0.0204(10) Uani 1 1 d . . . . .
H42A H 0.7749 0.6504 0.6477 0.024 Uiso 1 1 calc R U . . .
H42B H 1.0027 0.6375 0.7647 0.024 Uiso 1 1 calc R U . . .
C43 C 0.8998(7) 0.65473(7) 0.9647(6) 0.0167(9) Uani 1 1 d . . . . .
H43 H 0.7767 0.6505 1.0080 0.020 Uiso 1 1 calc R U . . .
C44 C 1.1171(7) 0.64733(6) 1.1444(7) 0.0180(9) Uani 1 1 d . . . . .
C45 C 1.1275(7) 0.65829(7) 1.3427(7) 0.0191(9) Uani 1 1 d . . . . .
H45A H 1.2683 0.6542 1.4575 0.023 Uiso 1 1 calc R U . . .
H45B H 1.0020 0.6531 1.3757 0.023 Uiso 1 1 calc R U . . .
C46 C 1.1150(8) 0.68317(7) 1.3204(7) 0.0205(10) Uani 1 1 d . . . . .
H46A H 1.1207 0.6898 1.4497 0.025 Uiso 1 1 calc R U . . .
H46B H 1.2453 0.6885 1.2953 0.025 Uiso 1 1 calc R U . . .
C47 C 0.8994(7) 0.69023(7) 1.1423(6) 0.0171(9) Uani 1 1 d . . . . .
H47 H 0.7780 0.6832 1.1731 0.021 Uiso 1 1 calc R U . . .
C48 C 0.8769(7) 0.67998(7) 0.9329(7) 0.0173(9) Uani 1 1 d . . . . .
C49 C 0.6381(8) 0.68525(7) 0.7760(7) 0.0199(10) Uani 1 1 d . . . . .
H49A H 0.6215 0.6800 0.6388 0.024 Uiso 1 1 calc R U . . .
H49B H 0.5290 0.6773 0.8157 0.024 Uiso 1 1 calc R U . . .
C50 C 0.5842(8) 0.70965(7) 0.7625(7) 0.0230(10) Uani 1 1 d . . . . .
H50A H 0.6820 0.7174 0.7080 0.028 Uiso 1 1 calc R U . . .
H50B H 0.4278 0.7119 0.6655 0.028 Uiso 1 1 calc R U . . .
C51 C 0.6162(8) 0.71915(7) 0.9704(7) 0.0225(10) Uani 1 1 d . . . . .
H51A H 0.5027 0.7128 1.0145 0.027 Uiso 1 1 calc R U . . .
H51B H 0.5900 0.7350 0.9552 0.027 Uiso 1 1 calc R U . . .
C52 C 0.8493(8) 0.71504(7) 1.1396(7) 0.0198(10) Uani 1 1 d . . . . .
C53 C 0.6382(8) 0.53021(7) 0.9863(7) 0.0215(10) Uani 1 1 d . . . . .
H53A H 0.4999 0.5377 0.9008 0.032 Uiso 1 1 calc R U . . .
H53B H 0.6776 0.5340 1.1307 0.032 Uiso 1 1 calc R U . . .
H53C H 0.6168 0.5144 0.9685 0.032 Uiso 1 1 calc R U . . .
C54 C 1.0281(8) 0.52228(7) 1.0339(8) 0.0259(11) Uani 1 1 d . . . . .
H54A H 0.9957 0.5076 0.9754 0.039 Uiso 1 1 calc R U . . .
H54B H 1.0567 0.5217 1.1803 0.039 Uiso 1 1 calc R U . . .
H54C H 1.1598 0.5280 1.0169 0.039 Uiso 1 1 calc R U . . .
C55 C 0.5103(7) 0.58033(7) 0.8736(7) 0.0209(10) Uani 1 1 d . . . . .
H55A H 0.4515 0.5952 0.8488 0.031 Uiso 1 1 calc R U . . .
H55B H 0.5365 0.5760 1.0144 0.031 Uiso 1 1 calc R U . . .
H55C H 0.4022 0.5704 0.7768 0.031 Uiso 1 1 calc R U . . .
C56 C 0.7977(8) 0.61378(7) 1.2243(7) 0.0212(10) Uani 1 1 d . . . . .
H56A H 0.6940 0.6247 1.1377 0.032 Uiso 1 1 calc R U . . .
H56B H 0.8785 0.6198 1.3620 0.032 Uiso 1 1 calc R U . . .
H56C H 0.7141 0.6008 1.2334 0.032 Uiso 1 1 calc R U . . .
C57 C 1.3332(7) 0.65201(7) 1.1178(7) 0.0238(10) Uani 1 1 d . . . . .
H57A H 1.3210 0.6467 0.9834 0.036 Uiso 1 1 calc R U . . .
H57B H 1.4571 0.6446 1.2263 0.036 Uiso 1 1 calc R U . . .
H57C H 1.3607 0.6677 1.1266 0.036 Uiso 1 1 calc R U . . .
C58 C 1.0443(8) 0.68878(7) 0.8468(7) 0.0209(10) Uani 1 1 d . . . . .
H58A H 1.0734 0.6776 0.7623 0.031 Uiso 1 1 calc R U . . .
H58B H 1.1841 0.6927 0.9608 0.031 Uiso 1 1 calc R U . . .
H58C H 0.9817 0.7017 0.7628 0.031 Uiso 1 1 calc R U . . .
C59 C 0.8351(9) 0.72157(7) 1.3439(7) 0.0274(11) Uani 1 1 d . . . . .
H59A H 0.7710 0.7362 1.3311 0.041 Uiso 1 1 calc R U . . .
H59B H 0.9849 0.7215 1.4535 0.041 Uiso 1 1 calc R U . . .
H59C H 0.7403 0.7112 1.3770 0.041 Uiso 1 1 calc R U . . .
C60 C 1.0232(8) 0.73006(7) 1.1120(8) 0.0240(10) Uani 1 1 d . . . . .
H60A H 1.0129 0.7290 0.9706 0.036 Uiso 1 1 calc R U . . .
H60B H 1.1728 0.7257 1.2071 0.036 Uiso 1 1 calc R U . . .
H60C H 0.9951 0.7451 1.1405 0.036 Uiso 1 1 calc R U . . .
O1 O 0.2601(5) 0.36977(4) 0.1917(4) 0.0183(7) Uani 1 1 d . . . . .
O2 O 0.8540(5) 0.48685(5) 0.4020(5) 0.0220(7) Uani 1 1 d . . . . .
H2O H 0.800(8) 0.4932(5) 0.472(8) 0.026 Uiso 1 1 calc R U . . .
O3 O 1.1349(5) 0.62384(4) 1.1683(5) 0.0202(7) Uani 1 1 d . . . . .
O4 O 0.6820(6) 0.51224(5) 0.6238(5) 0.0266(8) Uani 1 1 d . . . . .
H4O H 0.557(12) 0.5113(3) 0.609(10) 0.06(2) Uiso 1 1 calc R . . . .
O5 O 1.2574(7) 0.50494(8) 0.6117(7) 0.0445(11) Uani 1 1 d . . . . .
H51 H 1.243(12) 0.5054(11) 0.721(11) 0.053 Uiso 1 1 d . U . . .
H52 H 1.150(12) 0.4993(11) 0.527(11) 0.053 Uiso 1 1 d . 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
C1 C2 1.535(6) . ?
C1 C6 1.546(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.509(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O2 1.432(5) . ?
C3 C4 1.536(6) . ?
C3 H3 1.0000 . ?
C4 C23 1.530(6) . ?
C4 C24 1.539(7) . ?
C4 C5 1.562(6) . ?
C5 C10 1.531(6) . ?
C5 C6 1.555(6) . ?
C5 H5 1.0000 . ?
C6 C25 1.542(6) . ?
C6 C7 1.579(5) . ?
C7 C11 1.539(6) . ?
C7 C8 1.544(6) . ?
C7 H7 1.0000 . ?
C8 O1 1.452(5) . ?
C8 C9 1.527(6) . ?
C8 C26 1.540(6) . ?
C9 C10 1.535(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.540(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.543(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.552(6) . ?
C13 C18 1.580(6) . ?
C13 H13 1.0000 . ?
C14 O1 1.460(5) . ?
C14 C27 1.517(6) . ?
C14 C15 1.544(6) . ?
C15 C16 1.530(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.529(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C22 1.562(6) . ?
C17 C18 1.570(6) . ?
C17 H17 1.0000 . ?
C18 C19 1.548(6) . ?
C18 C28 1.552(6) . ?
C19 C20 1.526(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.518(7) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.536(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C29 1.529(7) . ?
C22 C30 1.544(6) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.527(6) . ?
C31 C36 1.540(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.517(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 O4 1.439(5) . ?
C33 C34 1.547(6) . ?
C33 H33 1.0000 . ?
C34 C53 1.530(7) . ?
C34 C54 1.547(6) . ?
C34 C35 1.562(6) . ?
C35 C40 1.527(6) . ?
C35 C36 1.557(6) . ?
C35 H35 1.0000 . ?
C36 C55 1.546(6) . ?
C36 C37 1.579(6) . ?
C37 C41 1.547(6) . ?
C37 C38 1.550(6) . ?
C37 H37 1.0000 . ?
C38 O3 1.447(5) . ?
C38 C56 1.524(6) . ?
C38 C39 1.528(6) . ?
C39 C40 1.528(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.524(6) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.539(6) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.554(6) . ?
C43 C48 1.566(6) . ?
C43 H43 1.0000 . ?
C44 O3 1.453(5) . ?
C44 C57 1.522(6) . ?
C44 C45 1.535(6) . ?
C45 C46 1.536(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.536(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C52 1.558(6) . ?
C47 C48 1.564(6) . ?
C47 H47 1.0000 . ?
C48 C58 1.544(6) . ?
C48 C49 1.550(6) . ?
C49 C50 1.534(6) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.521(6) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.542(6) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C60 1.534(6) . ?
C52 C59 1.540(6) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
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 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
O2 H2O 0.81(6) . ?
O4 H4O 0.78(7) . ?
O5 H51 0.81(7) . ?
O5 H52 0.80(8) . ?

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
C2 C1 C6 112.7(3) . . ?
C2 C1 H1A 109.0 . . ?
C6 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
C6 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C3 C2 C1 112.2(3) . . ?
C3 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
O2 C3 C2 111.4(3) . . ?
O2 C3 C4 111.5(3) . . ?
C2 C3 C4 114.7(4) . . ?
O2 C3 H3 106.2 . . ?
C2 C3 H3 106.2 . . ?
C4 C3 H3 106.2 . . ?
C23 C4 C3 111.1(4) . . ?
C23 C4 C24 108.2(4) . . ?
C3 C4 C24 106.6(4) . . ?
C23 C4 C5 114.3(4) . . ?
C3 C4 C5 107.9(3) . . ?
C24 C4 C5 108.5(3) . . ?
C10 C5 C6 111.9(3) . . ?
C10 C5 C4 113.1(3) . . ?
C6 C5 C4 117.1(3) . . ?
C10 C5 H5 104.4 . . ?
C6 C5 H5 104.4 . . ?
C4 C5 H5 104.4 . . ?
C25 C6 C1 107.4(3) . . ?
C25 C6 C5 114.8(3) . . ?
C1 C6 C5 106.9(3) . . ?
C25 C6 C7 111.6(3) . . ?
C1 C6 C7 109.2(3) . . ?
C5 C6 C7 106.8(3) . . ?
C11 C7 C8 111.4(4) . . ?
C11 C7 C6 115.0(3) . . ?
C8 C7 C6 113.5(3) . . ?
C11 C7 H7 105.3 . . ?
C8 C7 H7 105.3 . . ?
C6 C7 H7 105.3 . . ?
O1 C8 C9 110.6(3) . . ?
O1 C8 C26 98.8(3) . . ?
C9 C8 C26 109.1(4) . . ?
O1 C8 C7 113.3(3) . . ?
C9 C8 C7 108.5(4) . . ?
C26 C8 C7 116.3(4) . . ?
C8 C9 C10 111.4(4) . . ?
C8 C9 H9A 109.3 . . ?
C10 C9 H9A 109.3 . . ?
C8 C9 H9B 109.3 . . ?
C10 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
C5 C10 C9 110.8(3) . . ?
C5 C10 H10A 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C7 C11 C12 112.9(4) . . ?
C7 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
C7 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 C13 114.9(4) . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12B 108.5 . . ?
C13 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C12 C13 C14 113.3(3) . . ?
C12 C13 C18 113.2(3) . . ?
C14 C13 C18 115.1(3) . . ?
C12 C13 H13 104.6 . . ?
C14 C13 H13 104.6 . . ?
C18 C13 H13 104.6 . . ?
O1 C14 C27 113.2(3) . . ?
O1 C14 C15 98.8(3) . . ?
C27 C14 C15 109.1(4) . . ?
O1 C14 C13 108.7(3) . . ?
C27 C14 C13 116.2(4) . . ?
C15 C14 C13 109.4(3) . . ?
C16 C15 C14 113.2(4) . . ?
C16 C15 H15A 108.9 . . ?
C14 C15 H15A 108.9 . . ?
C16 C15 H15B 108.9 . . ?
C14 C15 H15B 108.9 . . ?
H15A C15 H15B 107.8 . . ?
C17 C16 C15 109.3(4) . . ?
C17 C16 H16A 109.8 . . ?
C15 C16 H16A 109.8 . . ?
C17 C16 H16B 109.8 . . ?
C15 C16 H16B 109.8 . . ?
H16A C16 H16B 108.3 . . ?
C16 C17 C22 114.2(3) . . ?
C16 C17 C18 110.1(3) . . ?
C22 C17 C18 117.1(3) . . ?
C16 C17 H17 104.7 . . ?
C22 C17 H17 104.7 . . ?
C18 C17 H17 104.7 . . ?
C19 C18 C28 108.4(4) . . ?
C19 C18 C17 107.4(3) . . ?
C28 C18 C17 114.3(3) . . ?
C19 C18 C13 108.5(3) . . ?
C28 C18 C13 111.7(3) . . ?
C17 C18 C13 106.3(3) . . ?
C20 C19 C18 113.5(3) . . ?
C20 C19 H19A 108.9 . . ?
C18 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C21 C20 C19 111.5(4) . . ?
C21 C20 H20A 109.3 . . ?
C19 C20 H20A 109.3 . . ?
C21 C20 H20B 109.3 . . ?
C19 C20 H20B 109.3 . . ?
H20A C20 H20B 108.0 . . ?
C20 C21 C22 113.6(4) . . ?
C20 C21 H21A 108.8 . . ?
C22 C21 H21A 108.8 . . ?
C20 C21 H21B 108.8 . . ?
C22 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C29 C22 C21 110.4(4) . . ?
C29 C22 C30 108.2(4) . . ?
C21 C22 C30 107.2(4) . . ?
C29 C22 C17 114.5(4) . . ?
C21 C22 C17 108.3(3) . . ?
C30 C22 C17 108.1(4) . . ?
C4 C23 H23A 109.5 . . ?
C4 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C4 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C4 C24 H24A 109.5 . . ?
C4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C4 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C6 C25 H25A 109.5 . . ?
C6 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C6 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C8 C26 H26A 109.5 . . ?
C8 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C8 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C14 C27 H27A 109.5 . . ?
C14 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C14 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C18 C28 H28A 109.5 . . ?
C18 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C18 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C22 C29 H29A 109.5 . . ?
C22 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C22 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C22 C30 H30A 109.5 . . ?
C22 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C22 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C36 113.1(4) . . ?
C32 C31 H31A 109.0 . . ?
C36 C31 H31A 109.0 . . ?
C32 C31 H31B 109.0 . . ?
C36 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
C33 C32 C31 112.0(4) . . ?
C33 C32 H32A 109.2 . . ?
C31 C32 H32A 109.2 . . ?
C33 C32 H32B 109.2 . . ?
C31 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
O4 C33 C32 111.0(4) . . ?
O4 C33 C34 112.2(4) . . ?
C32 C33 C34 113.3(4) . . ?
O4 C33 H33 106.6 . . ?
C32 C33 H33 106.6 . . ?
C34 C33 H33 106.6 . . ?
C53 C34 C33 111.2(4) . . ?
C53 C34 C54 107.4(4) . . ?
C33 C34 C54 107.0(4) . . ?
C53 C34 C35 113.2(4) . . ?
C33 C34 C35 108.3(3) . . ?
C54 C34 C35 109.6(4) . . ?
C40 C35 C36 111.1(3) . . ?
C40 C35 C34 113.5(4) . . ?
C36 C35 C34 117.2(3) . . ?
C40 C35 H35 104.5 . . ?
C36 C35 H35 104.5 . . ?
C34 C35 H35 104.5 . . ?
C31 C36 C55 108.3(4) . . ?
C31 C36 C35 107.1(3) . . ?
C55 C36 C35 113.9(4) . . ?
C31 C36 C37 109.1(3) . . ?
C55 C36 C37 111.2(3) . . ?
C35 C36 C37 107.0(3) . . ?
C41 C37 C38 114.4(3) . . ?
C41 C37 C36 112.4(3) . . ?
C38 C37 C36 115.4(3) . . ?
C41 C37 H37 104.4 . . ?
C38 C37 H37 104.4 . . ?
C36 C37 H37 104.4 . . ?
O3 C38 C56 112.1(3) . . ?
O3 C38 C39 100.5(3) . . ?
C56 C38 C39 109.0(4) . . ?
O3 C38 C37 109.6(3) . . ?
C56 C38 C37 115.6(4) . . ?
C39 C38 C37 109.0(3) . . ?
C38 C39 C40 113.6(4) . . ?
C38 C39 H39A 108.8 . . ?
C40 C39 H39A 108.8 . . ?
C38 C39 H39B 108.8 . . ?
C40 C39 H39B 108.8 . . ?
H39A C39 H39B 107.7 . . ?
C35 C40 C39 109.8(4) . . ?
C35 C40 H40A 109.7 . . ?
C39 C40 H40A 109.7 . . ?
C35 C40 H40B 109.7 . . ?
C39 C40 H40B 109.7 . . ?
H40A C40 H40B 108.2 . . ?
C42 C41 C37 115.2(4) . . ?
C42 C41 H41A 108.5 . . ?
C37 C41 H41A 108.5 . . ?
C42 C41 H41B 108.5 . . ?
C37 C41 H41B 108.5 . . ?
H41A C41 H41B 107.5 . . ?
C41 C42 C43 113.1(4) . . ?
C41 C42 H42A 109.0 . . ?
C43 C42 H42A 109.0 . . ?
C41 C42 H42B 108.9 . . ?
C43 C42 H42B 109.0 . . ?
H42A C42 H42B 107.8 . . ?
C42 C43 C44 111.2(4) . . ?
C42 C43 C48 115.3(3) . . ?
C44 C43 C48 114.3(3) . . ?
C42 C43 H43 104.9 . . ?
C44 C43 H43 104.9 . . ?
C48 C43 H43 104.9 . . ?
O3 C44 C57 99.6(3) . . ?
O3 C44 C45 110.9(3) . . ?
C57 C44 C45 108.8(4) . . ?
O3 C44 C43 113.0(3) . . ?
C57 C44 C43 115.7(4) . . ?
C45 C44 C43 108.6(3) . . ?
C44 C45 C46 111.1(4) . . ?
C44 C45 H45A 109.4 . . ?
C46 C45 H45A 109.4 . . ?
C44 C45 H45B 109.4 . . ?
C46 C45 H45B 109.4 . . ?
H45A C45 H45B 108.0 . . ?
C47 C46 C45 111.1(3) . . ?
C47 C46 H46A 109.4 . . ?
C45 C46 H46A 109.4 . . ?
C47 C46 H46B 109.4 . . ?
C45 C46 H46B 109.4 . . ?
H46A C46 H46B 108.0 . . ?
C46 C47 C52 114.0(3) . . ?
C46 C47 C48 112.3(4) . . ?
C52 C47 C48 116.2(3) . . ?
C46 C47 H47 104.3 . . ?
C52 C47 H47 104.3 . . ?
C48 C47 H47 104.3 . . ?
C58 C48 C49 108.1(4) . . ?
C58 C48 C47 114.7(3) . . ?
C49 C48 C47 106.8(4) . . ?
C58 C48 C43 111.2(4) . . ?
C49 C48 C43 108.8(3) . . ?
C47 C48 C43 107.1(3) . . ?
C50 C49 C48 112.9(4) . . ?
C50 C49 H49A 109.0 . . ?
C48 C49 H49A 109.0 . . ?
C50 C49 H49B 109.0 . . ?
C48 C49 H49B 109.0 . . ?
H49A C49 H49B 107.8 . . ?
C51 C50 C49 112.0(4) . . ?
C51 C50 H50A 109.2 . . ?
C49 C50 H50A 109.2 . . ?
C51 C50 H50B 109.2 . . ?
C49 C50 H50B 109.2 . . ?
H50A C50 H50B 107.9 . . ?
C50 C51 C52 114.0(4) . . ?
C50 C51 H51A 108.7 . . ?
C52 C51 H51A 108.7 . . ?
C50 C51 H51B 108.7 . . ?
C52 C51 H51B 108.7 . . ?
H51A C51 H51B 107.6 . . ?
C60 C52 C59 106.6(4) . . ?
C60 C52 C51 110.8(4) . . ?
C59 C52 C51 106.4(4) . . ?
C60 C52 C47 115.3(4) . . ?
C59 C52 C47 109.5(3) . . ?
C51 C52 C47 107.9(3) . . ?
C34 C53 H53A 109.5 . . ?
C34 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C34 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C34 C54 H54A 109.5 . . ?
C34 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C34 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C36 C55 H55A 109.5 . . ?
C36 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C36 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C38 C56 H56A 109.5 . . ?
C38 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C38 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C44 C57 H57A 109.5 . . ?
C44 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C44 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C48 C58 H58A 109.5 . . ?
C48 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C48 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C52 C59 H59A 109.5 . . ?
C52 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C52 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C52 C60 H60A 109.5 . . ?
C52 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C52 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C8 O1 C14 129.5(3) . . ?
C3 O2 H2O 109.5 . . ?
C38 O3 C44 130.2(3) . . ?
C33 O4 H4O 109.5 . . ?
H51 O5 H52 110(7) . . ?

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
C6 C1 C2 C3 -56.3(5) . . . . ?
C1 C2 C3 O2 -178.1(4) . . . . ?
C1 C2 C3 C4 54.1(5) . . . . ?
O2 C3 C4 C23 -51.7(5) . . . . ?
C2 C3 C4 C23 76.1(5) . . . . ?
O2 C3 C4 C24 66.0(4) . . . . ?
C2 C3 C4 C24 -166.2(3) . . . . ?
O2 C3 C4 C5 -177.6(3) . . . . ?
C2 C3 C4 C5 -49.9(5) . . . . ?
C23 C4 C5 C10 60.3(5) . . . . ?
C3 C4 C5 C10 -175.6(4) . . . . ?
C24 C4 C5 C10 -60.5(5) . . . . ?
C23 C4 C5 C6 -72.0(5) . . . . ?
C3 C4 C5 C6 52.1(5) . . . . ?
C24 C4 C5 C6 167.2(4) . . . . ?
C2 C1 C6 C25 -69.5(5) . . . . ?
C2 C1 C6 C5 54.1(5) . . . . ?
C2 C1 C6 C7 169.3(4) . . . . ?
C10 C5 C6 C25 -68.4(4) . . . . ?
C4 C5 C6 C25 64.5(5) . . . . ?
C10 C5 C6 C1 172.7(3) . . . . ?
C4 C5 C6 C1 -54.5(4) . . . . ?
C10 C5 C6 C7 55.8(4) . . . . ?
C4 C5 C6 C7 -171.3(3) . . . . ?
C25 C6 C7 C11 -60.5(5) . . . . ?
C1 C6 C7 C11 58.1(5) . . . . ?
C5 C6 C7 C11 173.3(4) . . . . ?
C25 C6 C7 C8 69.4(5) . . . . ?
C1 C6 C7 C8 -172.0(4) . . . . ?
C5 C6 C7 C8 -56.7(4) . . . . ?
C11 C7 C8 O1 -47.1(5) . . . . ?
C6 C7 C8 O1 -178.9(3) . . . . ?
C11 C7 C8 C9 -170.3(3) . . . . ?
C6 C7 C8 C9 58.0(5) . . . . ?
C11 C7 C8 C26 66.4(5) . . . . ?
C6 C7 C8 C26 -65.4(5) . . . . ?
O1 C8 C9 C10 178.0(3) . . . . ?
C26 C8 C9 C10 70.4(4) . . . . ?
C7 C8 C9 C10 -57.2(5) . . . . ?
C6 C5 C10 C9 -58.6(5) . . . . ?
C4 C5 C10 C9 166.6(4) . . . . ?
C8 C9 C10 C5 58.6(5) . . . . ?
C8 C7 C11 C12 87.6(4) . . . . ?
C6 C7 C11 C12 -141.4(4) . . . . ?
C7 C11 C12 C13 -76.0(5) . . . . ?
C11 C12 C13 C14 61.3(5) . . . . ?
C11 C12 C13 C18 -165.3(4) . . . . ?
C12 C13 C14 O1 -69.9(5) . . . . ?
C18 C13 C14 O1 157.7(3) . . . . ?
C12 C13 C14 C27 59.2(5) . . . . ?
C18 C13 C14 C27 -73.3(5) . . . . ?
C12 C13 C14 C15 -176.8(4) . . . . ?
C18 C13 C14 C15 50.8(5) . . . . ?
O1 C14 C15 C16 -165.2(4) . . . . ?
C27 C14 C15 C16 76.4(5) . . . . ?
C13 C14 C15 C16 -51.7(5) . . . . ?
C14 C15 C16 C17 59.5(5) . . . . ?
C15 C16 C17 C22 161.9(4) . . . . ?
C15 C16 C17 C18 -64.0(5) . . . . ?
C16 C17 C18 C19 176.3(3) . . . . ?
C22 C17 C18 C19 -51.1(5) . . . . ?
C16 C17 C18 C28 -63.4(5) . . . . ?
C22 C17 C18 C28 69.2(5) . . . . ?
C16 C17 C18 C13 60.3(4) . . . . ?
C22 C17 C18 C13 -167.1(4) . . . . ?
C12 C13 C18 C19 57.3(5) . . . . ?
C14 C13 C18 C19 -170.2(3) . . . . ?
C12 C13 C18 C28 -62.2(5) . . . . ?
C14 C13 C18 C28 70.3(5) . . . . ?
C12 C13 C18 C17 172.5(4) . . . . ?
C14 C13 C18 C17 -55.0(5) . . . . ?
C28 C18 C19 C20 -71.6(4) . . . . ?
C17 C18 C19 C20 52.4(5) . . . . ?
C13 C18 C19 C20 166.9(4) . . . . ?
C18 C19 C20 C21 -57.2(5) . . . . ?
C19 C20 C21 C22 56.8(5) . . . . ?
C20 C21 C22 C29 74.0(5) . . . . ?
C20 C21 C22 C30 -168.4(4) . . . . ?
C20 C21 C22 C17 -52.0(5) . . . . ?
C16 C17 C22 C29 58.3(5) . . . . ?
C18 C17 C22 C29 -72.5(5) . . . . ?
C16 C17 C22 C21 -178.1(4) . . . . ?
C18 C17 C22 C21 51.1(5) . . . . ?
C16 C17 C22 C30 -62.3(5) . . . . ?
C18 C17 C22 C30 166.9(4) . . . . ?
C36 C31 C32 C33 -57.9(5) . . . . ?
C31 C32 C33 O4 -177.0(4) . . . . ?
C31 C32 C33 C34 55.7(5) . . . . ?
O4 C33 C34 C53 -52.2(5) . . . . ?
C32 C33 C34 C53 74.5(4) . . . . ?
O4 C33 C34 C54 64.8(5) . . . . ?
C32 C33 C34 C54 -168.5(4) . . . . ?
O4 C33 C34 C35 -177.2(4) . . . . ?
C32 C33 C34 C35 -50.5(5) . . . . ?
C53 C34 C35 C40 59.1(5) . . . . ?
C33 C34 C35 C40 -177.0(4) . . . . ?
C54 C34 C35 C40 -60.6(5) . . . . ?
C53 C34 C35 C36 -72.5(5) . . . . ?
C33 C34 C35 C36 51.3(5) . . . . ?
C54 C34 C35 C36 167.7(4) . . . . ?
C32 C31 C36 C55 -69.4(5) . . . . ?
C32 C31 C36 C35 53.9(5) . . . . ?
C32 C31 C36 C37 169.4(4) . . . . ?
C40 C35 C36 C31 174.5(4) . . . . ?
C34 C35 C36 C31 -52.8(5) . . . . ?
C40 C35 C36 C55 -65.7(5) . . . . ?
C34 C35 C36 C55 67.0(5) . . . . ?
C40 C35 C36 C37 57.6(5) . . . . ?
C34 C35 C36 C37 -169.6(4) . . . . ?
C31 C36 C37 C41 57.1(5) . . . . ?
C55 C36 C37 C41 -62.4(5) . . . . ?
C35 C36 C37 C41 172.6(4) . . . . ?
C31 C36 C37 C38 -169.3(4) . . . . ?
C55 C36 C37 C38 71.2(5) . . . . ?
C35 C36 C37 C38 -53.8(5) . . . . ?
C41 C37 C38 O3 -67.1(5) . . . . ?
C36 C37 C38 O3 160.2(3) . . . . ?
C41 C37 C38 C56 60.7(5) . . . . ?
C36 C37 C38 C56 -72.0(5) . . . . ?
C41 C37 C38 C39 -176.2(4) . . . . ?
C36 C37 C38 C39 51.1(5) . . . . ?
O3 C38 C39 C40 -167.5(4) . . . . ?
C56 C38 C39 C40 74.6(5) . . . . ?
C37 C38 C39 C40 -52.4(5) . . . . ?
C36 C35 C40 C39 -61.5(5) . . . . ?
C34 C35 C40 C39 163.9(4) . . . . ?
C38 C39 C40 C35 58.9(5) . . . . ?
C38 C37 C41 C42 59.1(5) . . . . ?
C36 C37 C41 C42 -166.7(4) . . . . ?
C37 C41 C42 C43 -75.8(5) . . . . ?
C41 C42 C43 C44 87.9(5) . . . . ?
C41 C42 C43 C48 -139.8(4) . . . . ?
C42 C43 C44 O3 -46.4(5) . . . . ?
C48 C43 C44 O3 -179.2(4) . . . . ?
C42 C43 C44 C57 67.5(5) . . . . ?
C48 C43 C44 C57 -65.3(5) . . . . ?
C42 C43 C44 C45 -169.9(3) . . . . ?
C48 C43 C44 C45 57.3(5) . . . . ?
O3 C44 C45 C46 178.5(3) . . . . ?
C57 C44 C45 C46 70.0(4) . . . . ?
C43 C44 C45 C46 -56.8(5) . . . . ?
C44 C45 C46 C47 58.6(5) . . . . ?
C45 C46 C47 C52 167.3(4) . . . . ?
C45 C46 C47 C48 -58.0(5) . . . . ?
C46 C47 C48 C58 -69.4(5) . . . . ?
C52 C47 C48 C58 64.3(5) . . . . ?
C46 C47 C48 C49 170.9(3) . . . . ?
C52 C47 C48 C49 -55.5(5) . . . . ?
C46 C47 C48 C43 54.5(4) . . . . ?
C52 C47 C48 C43 -171.8(4) . . . . ?
C42 C43 C48 C58 -60.2(5) . . . . ?
C44 C43 C48 C58 70.6(5) . . . . ?
C42 C43 C48 C49 58.8(5) . . . . ?
C44 C43 C48 C49 -170.4(4) . . . . ?
C42 C43 C48 C47 173.8(4) . . . . ?
C44 C43 C48 C47 -55.4(5) . . . . ?
C58 C48 C49 C50 -69.4(5) . . . . ?
C47 C48 C49 C50 54.5(5) . . . . ?
C43 C48 C49 C50 169.7(4) . . . . ?
C48 C49 C50 C51 -56.2(5) . . . . ?
C49 C50 C51 C52 54.4(5) . . . . ?
C50 C51 C52 C60 75.7(5) . . . . ?
C50 C51 C52 C59 -168.9(4) . . . . ?
C50 C51 C52 C47 -51.5(5) . . . . ?
C46 C47 C52 C60 62.4(5) . . . . ?
C48 C47 C52 C60 -70.5(5) . . . . ?
C46 C47 C52 C59 -57.8(5) . . . . ?
C48 C47 C52 C59 169.3(4) . . . . ?
C46 C47 C52 C51 -173.2(4) . . . . ?
C48 C47 C52 C51 53.9(5) . . . . ?
C9 C8 O1 C14 90.0(5) . . . . ?
C26 C8 O1 C14 -155.7(4) . . . . ?
C7 C8 O1 C14 -32.0(6) . . . . ?
C27 C14 O1 C8 -47.2(5) . . . . ?
C15 C14 O1 C8 -162.4(4) . . . . ?
C13 C14 O1 C8 83.5(5) . . . . ?
C56 C38 O3 C44 -47.3(6) . . . . ?
C39 C38 O3 C44 -162.9(4) . . . . ?
C37 C38 O3 C44 82.4(5) . . . . ?
C57 C44 O3 C38 -156.1(4) . . . . ?
C45 C44 O3 C38 89.5(5) . . . . ?
C43 C44 O3 C38 -32.7(6) . . . . ?

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
O2 H2O O4 0.81 1.94 2.749(5) 171.9 .
O4 H4O O5 0.78 2.00 2.775(6) 169.6 1_455
O5 H52 O2 0.80(8) 1.94(8) 2.700(5) 159(7) .

_refine_diff_density_max         0.264
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.056


#END===============================================
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2, MeCN'
####################################################################### 
# 
# 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_FB5801Ba
_database_code_depnum_ccdc_archive 'CCDC 1529117'
_audit_update_record             
;
2017-01-22 deposited with the CCDC.
2017-10-16 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            'C37 H55 Br O3'
_chemical_formula_weight         627.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 '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'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2713 2.4705 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   16.9259(7)
_cell_length_b                   8.7979(3)
_cell_length_c                   23.0465(9)
_cell_angle_alpha                90
_cell_angle_beta                 107.5520(10)
_cell_angle_gamma                90
_cell_volume                     3272.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    101(2)
_cell_measurement_reflns_used    8520
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      24.16
_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   0.6763
_exptl_transmission_factor_max   0.7844
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.292
_shelx_estimated_absorpt_T_min   0.613
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      101(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker Photon CMOS Detector, D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54890
_diffrn_reflns_av_unetI/netI     0.1246
_diffrn_reflns_av_R_equivalents  0.1495
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.412
_diffrn_reflns_theta_max         25.045
_diffrn_reflns_theta_full        25.045
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             11547
_reflns_number_gt                8254
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.992

_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'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  'Microsoft Word'
_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)+(0.0142P)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_abs_structure_details 
;
 Flack x determined using 2691 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(5)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         11547
_refine_ls_number_parameters     743
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.0835
_refine_ls_wR_factor_gt          0.0733
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_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
C1 C 0.9384(3) 0.4286(6) 0.9036(2) 0.0135(15) Uani 1 1 d . . . . .
H1A H 0.9921 0.4466 0.9350 0.016 Uiso 1 1 calc R U . . .
H1B H 0.9445 0.4593 0.8638 0.016 Uiso 1 1 calc R U . . .
C2 C 0.8725(3) 0.5273(7) 0.9174(3) 0.0177(15) Uani 1 1 d . . . . .
H2A H 0.8684 0.5024 0.9582 0.021 Uiso 1 1 calc R U . . .
H2B H 0.8879 0.6358 0.9171 0.021 Uiso 1 1 calc R U . . .
C3 C 0.7900(3) 0.4996(6) 0.8699(3) 0.0147(15) Uani 1 1 d . . . . .
H3 H 0.7946 0.5305 0.8293 0.018 Uiso 1 1 calc R U . . .
C4 C 0.7584(4) 0.3351(7) 0.8654(3) 0.0166(16) Uani 1 1 d . . . . .
C5 C 0.8290(3) 0.2292(7) 0.8579(3) 0.0151(15) Uani 1 1 d . . . . .
H5 H 0.8329 0.2518 0.8163 0.018 Uiso 1 1 calc R U . . .
C6 C 0.9178(3) 0.2569(7) 0.9017(3) 0.0150(15) Uani 1 1 d . . . . .
C7 C 0.9814(3) 0.1617(7) 0.8776(2) 0.0166(15) Uani 1 1 d . . . . .
C8 C 0.9602(4) -0.0091(7) 0.8785(3) 0.0228(16) Uani 1 1 d . . . . .
H8 H 0.9653 -0.0357 0.9217 0.027 Uiso 1 1 calc R U . . .
C9 C 0.8696(3) -0.0407(8) 0.8409(3) 0.0270(15) Uani 1 1 d . . . . .
H9A H 0.8644 -0.0275 0.7972 0.032 Uiso 1 1 calc R U . . .
H9B H 0.8565 -0.1480 0.8470 0.032 Uiso 1 1 calc R U . . .
C10 C 0.8062(4) 0.0604(7) 0.8564(3) 0.0267(18) Uani 1 1 d . . . . .
H10A H 0.8015 0.0306 0.8966 0.032 Uiso 1 1 calc R U . . .
H10B H 0.7514 0.0447 0.8259 0.032 Uiso 1 1 calc R U . . .
C11 C 0.9803(3) 0.2082(7) 0.8122(3) 0.0162(15) Uani 1 1 d . . . . .
H11A H 0.9480 0.1315 0.7832 0.019 Uiso 1 1 calc R U . . .
H11B H 0.9510 0.3066 0.8021 0.019 Uiso 1 1 calc R U . . .
C12 C 1.0653(3) 0.2233(7) 0.8028(3) 0.0172(15) Uani 1 1 d . . . . .
H12A H 1.0913 0.1219 0.8046 0.021 Uiso 1 1 calc R U . . .
H12B H 1.0596 0.2681 0.7623 0.021 Uiso 1 1 calc R U . . .
C13 C 1.1188(3) 0.3247(7) 0.8523(2) 0.0139(14) Uani 1 1 d . . . . .
H13 H 1.0811 0.4089 0.8562 0.017 Uiso 1 1 calc R U . . .
C14 C 1.1384(3) 0.2384(7) 0.9130(3) 0.0142(15) Uani 1 1 d . . . . .
C15 C 1.1771(3) 0.3491(7) 0.9648(3) 0.0168(15) Uani 1 1 d . . . . .
H15A H 1.1947 0.2930 1.0038 0.020 Uiso 1 1 calc R U . . .
H15B H 1.1353 0.4254 0.9673 0.020 Uiso 1 1 calc R U . . .
C16 C 1.2522(3) 0.4301(7) 0.9547(2) 0.0186(16) Uani 1 1 d . . . . .
H16A H 1.2748 0.5034 0.9882 0.022 Uiso 1 1 calc R U . . .
H16B H 1.2959 0.3542 0.9560 0.022 Uiso 1 1 calc R U . . .
C17 C 1.2302(3) 0.5146(6) 0.8939(2) 0.0149(15) Uani 1 1 d . . . . .
H17 H 1.1830 0.5821 0.8947 0.018 Uiso 1 1 calc R U . . .
C18 C 1.1929(3) 0.4055(6) 0.8402(3) 0.0134(8) Uani 1 1 d . . . . .
C19 C 1.1589(4) 0.5049(7) 0.7818(3) 0.0219(16) Uani 1 1 d . . . . .
H19A H 1.1383 0.4376 0.7460 0.026 Uiso 1 1 calc R U . . .
H19B H 1.1117 0.5663 0.7855 0.026 Uiso 1 1 calc R U . . .
C20 C 1.2253(4) 0.6109(8) 0.7719(2) 0.0231(15) Uani 1 1 d . . . . .
H20A H 1.2698 0.5494 0.7638 0.028 Uiso 1 1 calc R U . . .
H20B H 1.2004 0.6751 0.7357 0.028 Uiso 1 1 calc R U . . .
C21 C 1.2622(4) 0.7122(7) 0.8269(3) 0.0234(17) Uani 1 1 d . . . . .
H21A H 1.2188 0.7826 0.8313 0.028 Uiso 1 1 calc R U . . .
H21B H 1.3069 0.7744 0.8194 0.028 Uiso 1 1 calc R U . . .
C22 C 1.2978(3) 0.6255(7) 0.8869(3) 0.0188(15) Uani 1 1 d . . . . .
C23 C 0.7283(4) 0.2936(7) 0.9198(3) 0.0228(16) Uani 1 1 d . . . . .
H23A H 0.6834 0.3624 0.9212 0.034 Uiso 1 1 calc R U . . .
H23B H 0.7743 0.3034 0.9575 0.034 Uiso 1 1 calc R U . . .
H23C H 0.7080 0.1886 0.9155 0.034 Uiso 1 1 calc R U . . .
C24 C 0.6836(4) 0.3257(7) 0.8073(3) 0.0246(17) Uani 1 1 d . . . . .
H24A H 0.7017 0.3481 0.7717 0.037 Uiso 1 1 calc R U . . .
H24B H 0.6415 0.3997 0.8099 0.037 Uiso 1 1 calc R U . . .
H24C H 0.6600 0.2231 0.8035 0.037 Uiso 1 1 calc R U . . .
C25 C 0.9275(3) 0.2076(7) 0.9681(2) 0.0196(15) Uani 1 1 d . . . . .
H25A H 0.8994 0.1101 0.9680 0.029 Uiso 1 1 calc R U . . .
H25B H 0.9027 0.2847 0.9879 0.029 Uiso 1 1 calc R U . . .
H25C H 0.9865 0.1968 0.9905 0.029 Uiso 1 1 calc R U . . .
C26 C 1.0170(4) -0.1186(7) 0.8578(3) 0.0321(19) Uani 1 1 d . . . . .
H26A H 0.9996 -0.2236 0.8613 0.048 Uiso 1 1 calc R U . . .
H26B H 1.0744 -0.1049 0.8835 0.048 Uiso 1 1 calc R U . . .
H26C H 1.0134 -0.0972 0.8153 0.048 Uiso 1 1 calc R U . . .
C27 C 1.1938(3) 0.0972(7) 0.9193(3) 0.0202(15) Uani 1 1 d . . . . .
H27A H 1.1771 0.0392 0.8812 0.030 Uiso 1 1 calc R U . . .
H27B H 1.1880 0.0334 0.9526 0.030 Uiso 1 1 calc R U . . .
H27C H 1.2517 0.1289 0.9280 0.030 Uiso 1 1 calc R U . . .
C28 C 1.2538(4) 0.2874(7) 0.8273(3) 0.0188(15) Uani 1 1 d . . . . .
H28A H 1.2226 0.1987 0.8068 0.028 Uiso 1 1 calc R U . . .
H28B H 1.2937 0.2558 0.8658 0.028 Uiso 1 1 calc R U . . .
H28C H 1.2834 0.3334 0.8011 0.028 Uiso 1 1 calc R U . . .
C29 C 1.3809(3) 0.5497(7) 0.8885(3) 0.0241(17) Uani 1 1 d . . . . .
H29A H 1.3729 0.4872 0.8520 0.036 Uiso 1 1 calc R U . . .
H29B H 1.4000 0.4855 0.9248 0.036 Uiso 1 1 calc R U . . .
H29C H 1.4223 0.6285 0.8897 0.036 Uiso 1 1 calc R U . . .
C30 C 1.3170(4) 0.7426(7) 0.9385(3) 0.0259(17) Uani 1 1 d . . . . .
H30A H 1.3505 0.8250 0.9295 0.039 Uiso 1 1 calc R U . . .
H30B H 1.3477 0.6934 0.9769 0.039 Uiso 1 1 calc R U . . .
H30C H 1.2650 0.7843 0.9422 0.039 Uiso 1 1 calc R U . . .
C31 C 0.6898(4) 0.7015(7) 0.8437(3) 0.0170(15) Uani 1 1 d . . . . .
C32 C 0.6303(3) 0.7954(7) 0.8653(3) 0.0155(15) Uani 1 1 d . . . . .
C33 C 0.6085(4) 0.7599(7) 0.9171(3) 0.0181(16) Uani 1 1 d . . . . .
H33 H 0.6309 0.6720 0.9402 0.022 Uiso 1 1 calc R U . . .
C34 C 0.5538(4) 0.8534(7) 0.9353(3) 0.0242(17) Uani 1 1 d . . . . .
H34 H 0.5375 0.8289 0.9702 0.029 Uiso 1 1 calc R U . . .
C35 C 0.5239(3) 0.9822(8) 0.9016(3) 0.0296(17) Uani 1 1 d . . . . .
C36 C 0.5438(4) 1.0192(7) 0.8495(3) 0.0242(17) Uani 1 1 d . . . . .
H36 H 0.5217 1.1076 0.8266 0.029 Uiso 1 1 calc R U . . .
C37 C 0.5967(4) 0.9236(7) 0.8316(3) 0.0250(18) Uani 1 1 d . . . . .
H37 H 0.6105 0.9458 0.7955 0.030 Uiso 1 1 calc R U . . .
C38 C 0.5611(3) 0.5795(6) 0.5955(2) 0.0142(15) Uani 1 1 d . . . . .
H38A H 0.5736 0.5576 0.5571 0.017 Uiso 1 1 calc R U . . .
H38B H 0.6100 0.5492 0.6296 0.017 Uiso 1 1 calc R U . . .
C39 C 0.4870(3) 0.4847(7) 0.5978(2) 0.0147(14) Uani 1 1 d . . . . .
H39A H 0.4385 0.5097 0.5625 0.018 Uiso 1 1 calc R U . . .
H39B H 0.4996 0.3754 0.5956 0.018 Uiso 1 1 calc R U . . .
C40 C 0.4671(3) 0.5166(6) 0.6558(3) 0.0144(15) Uani 1 1 d . . . . .
H40 H 0.5152 0.4847 0.6910 0.017 Uiso 1 1 calc R U . . .
C41 C 0.4460(3) 0.6831(7) 0.6648(3) 0.0131(14) Uani 1 1 d . . . . .
C42 C 0.5178(3) 0.7848(7) 0.6564(3) 0.0136(14) Uani 1 1 d . . . . .
H42 H 0.5669 0.7620 0.6923 0.016 Uiso 1 1 calc R U . . .
C43 C 0.5466(3) 0.7516(7) 0.5996(2) 0.0134(8) Uani 1 1 d . . . . .
C44 C 0.6306(4) 0.8441(7) 0.6064(3) 0.0168(15) Uani 1 1 d . . . . .
C45 C 0.6121(4) 1.0170(7) 0.6093(3) 0.0213(16) Uani 1 1 d . . . . .
H45 H 0.5685 1.0432 0.5705 0.026 Uiso 1 1 calc R U . . .
C46 C 0.5757(4) 1.0512(7) 0.6610(3) 0.0237(16) Uani 1 1 d . . . . .
H46A H 0.6194 1.0354 0.7002 0.028 Uiso 1 1 calc R U . . .
H46B H 0.5597 1.1598 0.6588 0.028 Uiso 1 1 calc R U . . .
C47 C 0.5010(3) 0.9560(7) 0.6609(2) 0.0175(13) Uani 1 1 d . . . . .
H47A H 0.4532 0.9862 0.6260 0.021 Uiso 1 1 calc R U . . .
H47B H 0.4863 0.9758 0.6987 0.021 Uiso 1 1 calc R U . . .
C48 C 0.7001(3) 0.7961(7) 0.6644(3) 0.0176(15) Uani 1 1 d . . . . .
H48A H 0.7063 0.8768 0.6954 0.021 Uiso 1 1 calc R U . . .
H48B H 0.6822 0.7025 0.6807 0.021 Uiso 1 1 calc R U . . .
C49 C 0.7847(4) 0.7667(7) 0.6559(3) 0.0184(16) Uani 1 1 d . . . . .
H49A H 0.8111 0.8644 0.6511 0.022 Uiso 1 1 calc R U . . .
H49B H 0.8210 0.7141 0.6921 0.022 Uiso 1 1 calc R U . . .
C50 C 0.7738(3) 0.6689(7) 0.5997(3) 0.0159(15) Uani 1 1 d . . . . .
H50 H 0.7338 0.5879 0.6027 0.019 Uiso 1 1 calc R U . . .
C51 C 0.7273(4) 0.7625(7) 0.5432(3) 0.0175(15) Uani 1 1 d . . . . .
C52 C 0.7037(3) 0.6576(7) 0.4878(2) 0.0180(15) Uani 1 1 d . . . . .
H52A H 0.6630 0.5815 0.4925 0.022 Uiso 1 1 calc R U . . .
H52B H 0.6771 0.7181 0.4508 0.022 Uiso 1 1 calc R U . . .
C53 C 0.7792(3) 0.5760(7) 0.4799(3) 0.0197(16) Uani 1 1 d . . . . .
H53A H 0.7616 0.5081 0.4441 0.024 Uiso 1 1 calc R U . . .
H53B H 0.8182 0.6518 0.4724 0.024 Uiso 1 1 calc R U . . .
C54 C 0.8230(3) 0.4829(7) 0.5360(2) 0.0154(14) Uani 1 1 d . . . . .
H54 H 0.7782 0.4173 0.5425 0.018 Uiso 1 1 calc R U . . .
C55 C 0.8512(3) 0.5813(7) 0.5945(3) 0.0162(15) Uani 1 1 d . . . . .
C56 C 0.8806(3) 0.4706(9) 0.6492(3) 0.0282(16) Uani 1 1 d . . . . .
H56A H 0.9041 0.5304 0.6869 0.034 Uiso 1 1 calc R U . . .
H56B H 0.8320 0.4143 0.6536 0.034 Uiso 1 1 calc R U . . .
C57 C 0.9451(4) 0.3570(8) 0.6428(3) 0.0321(19) Uani 1 1 d . . . . .
H57A H 0.9580 0.2853 0.6775 0.039 Uiso 1 1 calc R U . . .
H57B H 0.9967 0.4119 0.6441 0.039 Uiso 1 1 calc R U . . .
C58 C 0.9152(4) 0.2676(8) 0.5833(3) 0.0271(18) Uani 1 1 d . . . . .
H58A H 0.9605 0.2000 0.5801 0.032 Uiso 1 1 calc R U . . .
H58B H 0.8681 0.2024 0.5848 0.032 Uiso 1 1 calc R U . . .
C59 C 0.8879(4) 0.3669(7) 0.5266(3) 0.0208(16) Uani 1 1 d . . . . .
C60 C 0.3597(3) 0.7255(7) 0.6221(3) 0.0202(16) Uani 1 1 d . . . . .
H60A H 0.3568 0.7011 0.5800 0.030 Uiso 1 1 calc R U . . .
H60B H 0.3502 0.8346 0.6255 0.030 Uiso 1 1 calc R U . . .
H60C H 0.3172 0.6679 0.6337 0.030 Uiso 1 1 calc R U . . .
C61 C 0.4422(4) 0.6974(7) 0.7306(3) 0.0208(16) Uani 1 1 d . . . . .
H61A H 0.4311 0.8034 0.7388 0.031 Uiso 1 1 calc R U . . .
H61B H 0.4952 0.6656 0.7591 0.031 Uiso 1 1 calc R U . . .
H61C H 0.3978 0.6324 0.7358 0.031 Uiso 1 1 calc R U . . .
C62 C 0.4825(3) 0.7999(7) 0.5385(2) 0.0185(15) Uani 1 1 d . . . . .
H62A H 0.5093 0.8014 0.5063 0.028 Uiso 1 1 calc R U . . .
H62B H 0.4613 0.9016 0.5429 0.028 Uiso 1 1 calc R U . . .
H62C H 0.4365 0.7273 0.5279 0.028 Uiso 1 1 calc R U . . .
C63 C 0.6849(4) 1.1233(8) 0.6145(3) 0.0343(18) Uani 1 1 d . . . . .
H63A H 0.7037 1.1122 0.5785 0.051 Uiso 1 1 calc R U . . .
H63B H 0.7304 1.0976 0.6510 0.051 Uiso 1 1 calc R U . . .
H63C H 0.6675 1.2286 0.6174 0.051 Uiso 1 1 calc R U . . .
C64 C 0.7727(4) 0.9010(7) 0.5287(3) 0.0277(17) Uani 1 1 d . . . . .
H64A H 0.8136 0.8675 0.5090 0.042 Uiso 1 1 calc R U . . .
H64B H 0.8010 0.9547 0.5666 0.042 Uiso 1 1 calc R U . . .
H64C H 0.7327 0.9693 0.5014 0.042 Uiso 1 1 calc R U . . .
C65 C 0.9234(4) 0.6924(8) 0.5974(3) 0.0287(18) Uani 1 1 d . . . . .
H65A H 0.9189 0.7287 0.5563 0.043 Uiso 1 1 calc R U . . .
H65B H 0.9764 0.6396 0.6142 0.043 Uiso 1 1 calc R U . . .
H65C H 0.9206 0.7790 0.6234 0.043 Uiso 1 1 calc R U . . .
C66 C 0.9626(3) 0.4401(8) 0.5125(3) 0.0321(18) Uani 1 1 d . . . . .
H66A H 0.9430 0.5154 0.4800 0.048 Uiso 1 1 calc R U . . .
H66B H 0.9945 0.3614 0.4993 0.048 Uiso 1 1 calc R U . . .
H66C H 0.9980 0.4902 0.5491 0.048 Uiso 1 1 calc R U . . .
C67 C 0.8467(4) 0.2603(7) 0.4730(3) 0.0256(18) Uani 1 1 d . . . . .
H67A H 0.8366 0.3159 0.4346 0.038 Uiso 1 1 calc R U . . .
H67B H 0.7939 0.2234 0.4769 0.038 Uiso 1 1 calc R U . . .
H67C H 0.8833 0.1737 0.4734 0.038 Uiso 1 1 calc R U . . .
C68 C 0.4034(4) 0.3137(6) 0.6963(3) 0.0130(14) Uani 1 1 d . . . . .
C69 C 0.3229(3) 0.2342(7) 0.6896(2) 0.0134(8) Uani 1 1 d . . . . .
C70 C 0.2473(3) 0.2948(7) 0.6557(2) 0.0136(15) Uani 1 1 d . . . . .
H70 H 0.2456 0.3898 0.6358 0.016 Uiso 1 1 calc R U . . .
C71 C 0.1740(4) 0.2162(7) 0.6508(3) 0.0171(15) Uani 1 1 d . . . . .
H71 H 0.1218 0.2585 0.6290 0.020 Uiso 1 1 calc R U . . .
C72 C 0.1787(3) 0.0756(7) 0.6783(3) 0.0150(15) Uani 1 1 d . . . . .
C73 C 0.2530(3) 0.0137(7) 0.7115(3) 0.0184(16) Uani 1 1 d . . . . .
H73 H 0.2548 -0.0836 0.7298 0.022 Uiso 1 1 calc R U . . .
C74 C 0.3248(3) 0.0946(7) 0.7179(2) 0.0156(14) Uani 1 1 d . . . . .
H74 H 0.3763 0.0543 0.7420 0.019 Uiso 1 1 calc R U . . .
O1 O 0.7291(2) 0.5991(5) 0.88492(17) 0.0174(10) Uani 1 1 d . . . . .
O2 O 1.0614(2) 0.1855(4) 0.92318(16) 0.0151(10) Uani 1 1 d . . . . .
O3 O 0.6997(3) 0.7185(5) 0.7947(2) 0.0348(12) Uani 1 1 d . . . . .
O4 O 0.3951(2) 0.4243(4) 0.65541(16) 0.0149(10) Uani 1 1 d . . . . .
O5 O 0.6489(2) 0.8171(5) 0.54971(18) 0.0185(10) Uani 1 1 d . . . . .
O6 O 0.4669(2) 0.2805(5) 0.73485(19) 0.0251(12) Uani 1 1 d . . . . .
Br1 Br 0.45322(4) 1.11410(9) 0.92824(4) 0.0463(3) Uani 1 1 d . . . . .
Br2 Br 0.08000(4) -0.03624(7) 0.67039(3) 0.02370(17) Uani 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
C1 C2 1.521(7) . ?
C1 C6 1.549(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.512(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O1 1.471(6) . ?
C3 C4 1.535(9) . ?
C3 H3 1.0000 . ?
C4 C23 1.533(8) . ?
C4 C24 1.542(8) . ?
C4 C5 1.566(8) . ?
C5 C10 1.532(8) . ?
C5 C6 1.556(8) . ?
C5 H5 1.0000 . ?
C6 C25 1.553(8) . ?
C6 C7 1.590(8) . ?
C7 O2 1.456(6) . ?
C7 C8 1.547(8) . ?
C7 C11 1.557(8) . ?
C8 C26 1.535(8) . ?
C8 C9 1.543(7) . ?
C8 H8 1.0000 . ?
C9 C10 1.518(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.524(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.515(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C18 1.538(8) . ?
C13 C14 1.539(7) . ?
C13 H13 1.0000 . ?
C14 O2 1.467(6) . ?
C14 C15 1.526(8) . ?
C14 C27 1.537(8) . ?
C15 C16 1.535(8) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.530(8) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.544(7) . ?
C17 C22 1.548(8) . ?
C17 H17 1.0000 . ?
C18 C28 1.553(8) . ?
C18 C19 1.561(7) . ?
C19 C20 1.529(8) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.522(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.534(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C30 1.533(8) . ?
C22 C29 1.546(8) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 O3 1.201(7) . ?
C31 O1 1.332(7) . ?
C31 C32 1.498(8) . ?
C32 C33 1.387(8) . ?
C32 C37 1.389(8) . ?
C33 C34 1.394(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.380(9) . ?
C34 H34 0.9500 . ?
C35 C36 1.382(9) . ?
C35 Br1 1.896(7) . ?
C36 C37 1.379(8) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39 1.520(7) . ?
C38 C43 1.542(8) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.501(7) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 O4 1.462(6) . ?
C40 C41 1.537(8) . ?
C40 H40 1.0000 . ?
C41 C60 1.541(8) . ?
C41 C61 1.543(8) . ?
C41 C42 1.567(8) . ?
C42 C47 1.542(8) . ?
C42 C43 1.557(8) . ?
C42 H42 1.0000 . ?
C43 C62 1.555(7) . ?
C43 C44 1.604(8) . ?
C44 O5 1.450(7) . ?
C44 C48 1.550(8) . ?
C44 C45 1.558(9) . ?
C45 C63 1.522(8) . ?
C45 C46 1.529(8) . ?
C45 H45 1.0000 . ?
C46 C47 1.516(8) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.525(8) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.519(8) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.541(8) . ?
C50 C55 1.555(8) . ?
C50 H50 1.0000 . ?
C51 O5 1.460(7) . ?
C51 C52 1.528(8) . ?
C51 C64 1.530(8) . ?
C52 C53 1.523(8) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.521(7) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.552(7) . ?
C54 C59 1.562(8) . ?
C54 H54 1.0000 . ?
C55 C65 1.551(8) . ?
C55 C56 1.552(8) . ?
C56 C57 1.521(8) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.527(9) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.523(8) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C66 1.539(8) . ?
C59 C67 1.541(8) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 O6 1.207(6) . ?
C68 O4 1.333(6) . ?
C68 C69 1.497(8) . ?
C69 C74 1.386(8) . ?
C69 C70 1.388(7) . ?
C70 C71 1.396(8) . ?
C70 H70 0.9500 . ?
C71 C72 1.381(8) . ?
C71 H71 0.9500 . ?
C72 C73 1.371(7) . ?
C72 Br2 1.900(6) . ?
C73 C74 1.378(7) . ?
C73 H73 0.9500 . ?
C74 H74 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
C2 C1 C6 113.0(5) . . ?
C2 C1 H1A 109.0 . . ?
C6 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
C6 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C3 C2 C1 109.4(5) . . ?
C3 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
C3 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
O1 C3 C2 107.0(4) . . ?
O1 C3 C4 108.8(5) . . ?
C2 C3 C4 115.3(5) . . ?
O1 C3 H3 108.5 . . ?
C2 C3 H3 108.5 . . ?
C4 C3 H3 108.5 . . ?
C23 C4 C3 111.3(5) . . ?
C23 C4 C24 108.0(5) . . ?
C3 C4 C24 106.7(5) . . ?
C23 C4 C5 113.7(5) . . ?
C3 C4 C5 107.9(5) . . ?
C24 C4 C5 109.0(5) . . ?
C10 C5 C6 110.7(5) . . ?
C10 C5 C4 112.5(5) . . ?
C6 C5 C4 117.1(5) . . ?
C10 C5 H5 105.1 . . ?
C6 C5 H5 105.1 . . ?
C4 C5 H5 105.1 . . ?
C1 C6 C25 106.8(5) . . ?
C1 C6 C5 109.6(5) . . ?
C25 C6 C5 113.0(5) . . ?
C1 C6 C7 110.7(5) . . ?
C25 C6 C7 108.4(5) . . ?
C5 C6 C7 108.3(5) . . ?
O2 C7 C8 107.4(5) . . ?
O2 C7 C11 113.5(5) . . ?
C8 C7 C11 109.4(5) . . ?
O2 C7 C6 104.7(4) . . ?
C8 C7 C6 108.8(5) . . ?
C11 C7 C6 112.8(5) . . ?
C26 C8 C9 108.8(5) . . ?
C26 C8 C7 115.8(5) . . ?
C9 C8 C7 111.3(5) . . ?
C26 C8 H8 106.8 . . ?
C9 C8 H8 106.8 . . ?
C7 C8 H8 106.8 . . ?
C10 C9 C8 114.6(6) . . ?
C10 C9 H9A 108.6 . . ?
C8 C9 H9A 108.6 . . ?
C10 C9 H9B 108.6 . . ?
C8 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 C5 112.4(5) . . ?
C9 C10 H10A 109.1 . . ?
C5 C10 H10A 109.1 . . ?
C9 C10 H10B 109.1 . . ?
C5 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
C12 C11 C7 115.1(5) . . ?
C12 C11 H11A 108.5 . . ?
C7 C11 H11A 108.5 . . ?
C12 C11 H11B 108.5 . . ?
C7 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
C13 C12 C11 108.6(5) . . ?
C13 C12 H12A 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C13 C12 H12B 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.3 . . ?
C12 C13 C18 118.1(5) . . ?
C12 C13 C14 108.1(5) . . ?
C18 C13 C14 115.4(5) . . ?
C12 C13 H13 104.6 . . ?
C18 C13 H13 104.6 . . ?
C14 C13 H13 104.6 . . ?
O2 C14 C15 105.7(4) . . ?
O2 C14 C27 106.0(4) . . ?
C15 C14 C27 109.7(5) . . ?
O2 C14 C13 110.1(4) . . ?
C15 C14 C13 108.7(5) . . ?
C27 C14 C13 116.2(5) . . ?
C14 C15 C16 111.0(5) . . ?
C14 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
C14 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C17 C16 C15 112.4(4) . . ?
C17 C16 H16A 109.1 . . ?
C15 C16 H16A 109.1 . . ?
C17 C16 H16B 109.1 . . ?
C15 C16 H16B 109.1 . . ?
H16A C16 H16B 107.9 . . ?
C16 C17 C18 111.1(5) . . ?
C16 C17 C22 114.7(5) . . ?
C18 C17 C22 116.4(5) . . ?
C16 C17 H17 104.3 . . ?
C18 C17 H17 104.3 . . ?
C22 C17 H17 104.3 . . ?
C13 C18 C17 107.5(5) . . ?
C13 C18 C28 110.5(5) . . ?
C17 C18 C28 115.8(5) . . ?
C13 C18 C19 107.8(4) . . ?
C17 C18 C19 107.3(5) . . ?
C28 C18 C19 107.7(5) . . ?
C20 C19 C18 112.0(5) . . ?
C20 C19 H19A 109.2 . . ?
C18 C19 H19A 109.2 . . ?
C20 C19 H19B 109.2 . . ?
C18 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C21 C20 C19 111.6(5) . . ?
C21 C20 H20A 109.3 . . ?
C19 C20 H20A 109.3 . . ?
C21 C20 H20B 109.3 . . ?
C19 C20 H20B 109.3 . . ?
H20A C20 H20B 108.0 . . ?
C20 C21 C22 114.3(5) . . ?
C20 C21 H21A 108.7 . . ?
C22 C21 H21A 108.7 . . ?
C20 C21 H21B 108.7 . . ?
C22 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C30 C22 C21 107.4(5) . . ?
C30 C22 C29 107.0(5) . . ?
C21 C22 C29 110.0(5) . . ?
C30 C22 C17 109.4(5) . . ?
C21 C22 C17 107.8(5) . . ?
C29 C22 C17 114.9(5) . . ?
C4 C23 H23A 109.5 . . ?
C4 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C4 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C4 C24 H24A 109.5 . . ?
C4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C4 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C6 C25 H25A 109.5 . . ?
C6 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C6 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C8 C26 H26A 109.5 . . ?
C8 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C8 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C14 C27 H27A 109.5 . . ?
C14 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C14 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C18 C28 H28A 109.5 . . ?
C18 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C18 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C22 C29 H29A 109.5 . . ?
C22 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C22 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C22 C30 H30A 109.5 . . ?
C22 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C22 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O3 C31 O1 125.0(6) . . ?
O3 C31 C32 122.8(6) . . ?
O1 C31 C32 112.2(5) . . ?
C33 C32 C37 119.5(6) . . ?
C33 C32 C31 122.8(6) . . ?
C37 C32 C31 117.7(6) . . ?
C32 C33 C34 119.9(6) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C35 C34 C33 118.7(7) . . ?
C35 C34 H34 120.7 . . ?
C33 C34 H34 120.7 . . ?
C34 C35 C36 122.5(6) . . ?
C34 C35 Br1 118.8(6) . . ?
C36 C35 Br1 118.7(5) . . ?
C37 C36 C35 117.8(6) . . ?
C37 C36 H36 121.1 . . ?
C35 C36 H36 121.1 . . ?
C36 C37 C32 121.5(6) . . ?
C36 C37 H37 119.3 . . ?
C32 C37 H37 119.3 . . ?
C39 C38 C43 112.9(5) . . ?
C39 C38 H38A 109.0 . . ?
C43 C38 H38A 109.0 . . ?
C39 C38 H38B 109.0 . . ?
C43 C38 H38B 109.0 . . ?
H38A C38 H38B 107.8 . . ?
C40 C39 C38 109.7(4) . . ?
C40 C39 H39A 109.7 . . ?
C38 C39 H39A 109.7 . . ?
C40 C39 H39B 109.7 . . ?
C38 C39 H39B 109.7 . . ?
H39A C39 H39B 108.2 . . ?
O4 C40 C39 107.5(4) . . ?
O4 C40 C41 107.7(4) . . ?
C39 C40 C41 114.9(5) . . ?
O4 C40 H40 108.9 . . ?
C39 C40 H40 108.9 . . ?
C41 C40 H40 108.9 . . ?
C40 C41 C60 111.0(5) . . ?
C40 C41 C61 106.9(5) . . ?
C60 C41 C61 107.1(5) . . ?
C40 C41 C42 107.9(5) . . ?
C60 C41 C42 113.8(5) . . ?
C61 C41 C42 109.8(5) . . ?
C47 C42 C43 110.5(5) . . ?
C47 C42 C41 112.6(5) . . ?
C43 C42 C41 116.6(5) . . ?
C47 C42 H42 105.4 . . ?
C43 C42 H42 105.4 . . ?
C41 C42 H42 105.4 . . ?
C38 C43 C62 107.1(5) . . ?
C38 C43 C42 109.3(5) . . ?
C62 C43 C42 113.6(5) . . ?
C38 C43 C44 110.6(5) . . ?
C62 C43 C44 107.8(5) . . ?
C42 C43 C44 108.4(4) . . ?
O5 C44 C48 114.8(5) . . ?
O5 C44 C45 107.4(5) . . ?
C48 C44 C45 109.8(5) . . ?
O5 C44 C43 104.7(4) . . ?
C48 C44 C43 111.4(5) . . ?
C45 C44 C43 108.4(5) . . ?
C63 C45 C46 108.9(5) . . ?
C63 C45 C44 115.8(5) . . ?
C46 C45 C44 111.1(5) . . ?
C63 C45 H45 106.9 . . ?
C46 C45 H45 106.9 . . ?
C44 C45 H45 106.9 . . ?
C47 C46 C45 114.9(5) . . ?
C47 C46 H46A 108.5 . . ?
C45 C46 H46A 108.5 . . ?
C47 C46 H46B 108.5 . . ?
C45 C46 H46B 108.5 . . ?
H46A C46 H46B 107.5 . . ?
C46 C47 C42 111.7(5) . . ?
C46 C47 H47A 109.3 . . ?
C42 C47 H47A 109.3 . . ?
C46 C47 H47B 109.3 . . ?
C42 C47 H47B 109.3 . . ?
H47A C47 H47B 108.0 . . ?
C49 C48 C44 115.7(5) . . ?
C49 C48 H48A 108.4 . . ?
C44 C48 H48A 108.4 . . ?
C49 C48 H48B 108.4 . . ?
C44 C48 H48B 108.4 . . ?
H48A C48 H48B 107.4 . . ?
C50 C49 C48 109.2(5) . . ?
C50 C49 H49A 109.8 . . ?
C48 C49 H49A 109.8 . . ?
C50 C49 H49B 109.8 . . ?
C48 C49 H49B 109.8 . . ?
H49A C49 H49B 108.3 . . ?
C49 C50 C51 108.5(5) . . ?
C49 C50 C55 117.2(5) . . ?
C51 C50 C55 115.3(5) . . ?
C49 C50 H50 104.8 . . ?
C51 C50 H50 104.8 . . ?
C55 C50 H50 104.8 . . ?
O5 C51 C52 105.6(4) . . ?
O5 C51 C64 107.0(5) . . ?
C52 C51 C64 108.7(5) . . ?
O5 C51 C50 109.7(5) . . ?
C52 C51 C50 108.8(5) . . ?
C64 C51 C50 116.5(5) . . ?
C53 C52 C51 111.6(5) . . ?
C53 C52 H52A 109.3 . . ?
C51 C52 H52A 109.3 . . ?
C53 C52 H52B 109.3 . . ?
C51 C52 H52B 109.3 . . ?
H52A C52 H52B 108.0 . . ?
C54 C53 C52 111.4(5) . . ?
C54 C53 H53A 109.4 . . ?
C52 C53 H53A 109.4 . . ?
C54 C53 H53B 109.4 . . ?
C52 C53 H53B 109.4 . . ?
H53A C53 H53B 108.0 . . ?
C53 C54 C55 112.4(5) . . ?
C53 C54 C59 114.7(5) . . ?
C55 C54 C59 116.1(4) . . ?
C53 C54 H54 103.9 . . ?
C55 C54 H54 103.9 . . ?
C59 C54 H54 103.9 . . ?
C65 C55 C54 114.8(5) . . ?
C65 C55 C56 107.8(5) . . ?
C54 C55 C56 107.2(5) . . ?
C65 C55 C50 110.9(5) . . ?
C54 C55 C50 107.3(4) . . ?
C56 C55 C50 108.6(5) . . ?
C57 C56 C55 113.4(5) . . ?
C57 C56 H56A 108.9 . . ?
C55 C56 H56A 108.9 . . ?
C57 C56 H56B 108.9 . . ?
C55 C56 H56B 108.9 . . ?
H56A C56 H56B 107.7 . . ?
C56 C57 C58 111.9(5) . . ?
C56 C57 H57A 109.2 . . ?
C58 C57 H57A 109.2 . . ?
C56 C57 H57B 109.2 . . ?
C58 C57 H57B 109.2 . . ?
H57A C57 H57B 107.9 . . ?
C59 C58 C57 114.0(6) . . ?
C59 C58 H58A 108.8 . . ?
C57 C58 H58A 108.8 . . ?
C59 C58 H58B 108.8 . . ?
C57 C58 H58B 108.8 . . ?
H58A C58 H58B 107.6 . . ?
C58 C59 C66 111.5(5) . . ?
C58 C59 C67 106.6(5) . . ?
C66 C59 C67 106.7(5) . . ?
C58 C59 C54 107.5(5) . . ?
C66 C59 C54 114.4(5) . . ?
C67 C59 C54 109.9(5) . . ?
C41 C60 H60A 109.5 . . ?
C41 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C41 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C41 C61 H61A 109.5 . . ?
C41 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C41 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C43 C62 H62A 109.5 . . ?
C43 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C43 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C45 C63 H63A 109.5 . . ?
C45 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C45 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C51 C64 H64A 109.5 . . ?
C51 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C51 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C55 C65 H65A 109.5 . . ?
C55 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C55 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C59 C66 H66A 109.5 . . ?
C59 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C59 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C59 C67 H67A 109.5 . . ?
C59 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C59 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
O6 C68 O4 125.2(5) . . ?
O6 C68 C69 123.0(5) . . ?
O4 C68 C69 111.7(5) . . ?
C74 C69 C70 119.5(5) . . ?
C74 C69 C68 118.3(5) . . ?
C70 C69 C68 122.2(5) . . ?
C69 C70 C71 120.1(6) . . ?
C69 C70 H70 120.0 . . ?
C71 C70 H70 120.0 . . ?
C72 C71 C70 118.6(6) . . ?
C72 C71 H71 120.7 . . ?
C70 C71 H71 120.7 . . ?
C73 C72 C71 121.9(5) . . ?
C73 C72 Br2 118.6(4) . . ?
C71 C72 Br2 119.4(4) . . ?
C72 C73 C74 119.0(5) . . ?
C72 C73 H73 120.5 . . ?
C74 C73 H73 120.5 . . ?
C73 C74 C69 120.8(5) . . ?
C73 C74 H74 119.6 . . ?
C69 C74 H74 119.6 . . ?
C31 O1 C3 118.0(5) . . ?
C7 O2 C14 127.4(4) . . ?
C68 O4 C40 119.4(4) . . ?
C44 O5 C51 126.5(4) . . ?

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
C6 C1 C2 C3 -58.1(6) . . . . ?
C1 C2 C3 O1 -179.2(4) . . . . ?
C1 C2 C3 C4 59.6(7) . . . . ?
O1 C3 C4 C23 -47.3(6) . . . . ?
C2 C3 C4 C23 72.9(6) . . . . ?
O1 C3 C4 C24 70.3(6) . . . . ?
C2 C3 C4 C24 -169.5(5) . . . . ?
O1 C3 C4 C5 -172.7(4) . . . . ?
C2 C3 C4 C5 -52.5(7) . . . . ?
C23 C4 C5 C10 52.9(7) . . . . ?
C3 C4 C5 C10 176.9(5) . . . . ?
C24 C4 C5 C10 -67.7(7) . . . . ?
C23 C4 C5 C6 -77.1(7) . . . . ?
C3 C4 C5 C6 46.9(7) . . . . ?
C24 C4 C5 C6 162.4(5) . . . . ?
C2 C1 C6 C25 -70.5(5) . . . . ?
C2 C1 C6 C5 52.2(6) . . . . ?
C2 C1 C6 C7 171.6(4) . . . . ?
C10 C5 C6 C1 -178.5(5) . . . . ?
C4 C5 C6 C1 -47.8(7) . . . . ?
C10 C5 C6 C25 -59.5(7) . . . . ?
C4 C5 C6 C25 71.2(7) . . . . ?
C10 C5 C6 C7 60.6(6) . . . . ?
C4 C5 C6 C7 -168.6(5) . . . . ?
C1 C6 C7 O2 63.6(5) . . . . ?
C25 C6 C7 O2 -53.2(6) . . . . ?
C5 C6 C7 O2 -176.1(4) . . . . ?
C1 C6 C7 C8 178.2(5) . . . . ?
C25 C6 C7 C8 61.4(6) . . . . ?
C5 C6 C7 C8 -61.6(6) . . . . ?
C1 C6 C7 C11 -60.2(6) . . . . ?
C25 C6 C7 C11 -177.0(5) . . . . ?
C5 C6 C7 C11 60.1(6) . . . . ?
O2 C7 C8 C26 -66.0(7) . . . . ?
C11 C7 C8 C26 57.5(7) . . . . ?
C6 C7 C8 C26 -178.8(5) . . . . ?
O2 C7 C8 C9 169.1(5) . . . . ?
C11 C7 C8 C9 -67.4(6) . . . . ?
C6 C7 C8 C9 56.3(6) . . . . ?
C26 C8 C9 C10 -179.8(6) . . . . ?
C7 C8 C9 C10 -51.0(7) . . . . ?
C8 C9 C10 C5 49.4(8) . . . . ?
C6 C5 C10 C9 -54.4(7) . . . . ?
C4 C5 C10 C9 172.5(5) . . . . ?
O2 C7 C11 C12 17.9(7) . . . . ?
C8 C7 C11 C12 -102.1(6) . . . . ?
C6 C7 C11 C12 136.7(5) . . . . ?
C7 C11 C12 C13 -50.9(7) . . . . ?
C11 C12 C13 C18 -157.4(5) . . . . ?
C11 C12 C13 C14 69.3(6) . . . . ?
C12 C13 C14 O2 -53.4(6) . . . . ?
C18 C13 C14 O2 171.8(4) . . . . ?
C12 C13 C14 C15 -168.8(5) . . . . ?
C18 C13 C14 C15 56.5(6) . . . . ?
C12 C13 C14 C27 67.0(6) . . . . ?
C18 C13 C14 C27 -67.7(7) . . . . ?
O2 C14 C15 C16 -172.1(4) . . . . ?
C27 C14 C15 C16 74.1(6) . . . . ?
C13 C14 C15 C16 -53.9(6) . . . . ?
C14 C15 C16 C17 57.0(6) . . . . ?
C15 C16 C17 C18 -57.7(6) . . . . ?
C15 C16 C17 C22 167.7(5) . . . . ?
C12 C13 C18 C17 173.5(5) . . . . ?
C14 C13 C18 C17 -56.5(6) . . . . ?
C12 C13 C18 C28 -59.3(6) . . . . ?
C14 C13 C18 C28 70.7(6) . . . . ?
C12 C13 C18 C19 58.1(6) . . . . ?
C14 C13 C18 C19 -171.9(5) . . . . ?
C16 C17 C18 C13 54.8(6) . . . . ?
C22 C17 C18 C13 -171.4(5) . . . . ?
C16 C17 C18 C28 -69.2(6) . . . . ?
C22 C17 C18 C28 64.6(7) . . . . ?
C16 C17 C18 C19 170.6(5) . . . . ?
C22 C17 C18 C19 -55.6(6) . . . . ?
C13 C18 C19 C20 170.2(5) . . . . ?
C17 C18 C19 C20 54.7(6) . . . . ?
C28 C18 C19 C20 -70.6(6) . . . . ?
C18 C19 C20 C21 -56.2(7) . . . . ?
C19 C20 C21 C22 55.3(7) . . . . ?
C20 C21 C22 C30 -169.5(5) . . . . ?
C20 C21 C22 C29 74.3(7) . . . . ?
C20 C21 C22 C17 -51.7(7) . . . . ?
C16 C17 C22 C30 -57.6(7) . . . . ?
C18 C17 C22 C30 170.3(5) . . . . ?
C16 C17 C22 C21 -174.0(5) . . . . ?
C18 C17 C22 C21 53.8(7) . . . . ?
C16 C17 C22 C29 62.9(7) . . . . ?
C18 C17 C22 C29 -69.3(6) . . . . ?
O3 C31 C32 C33 168.9(6) . . . . ?
O1 C31 C32 C33 -11.0(8) . . . . ?
O3 C31 C32 C37 -11.5(9) . . . . ?
O1 C31 C32 C37 168.6(5) . . . . ?
C37 C32 C33 C34 -0.6(8) . . . . ?
C31 C32 C33 C34 179.0(5) . . . . ?
C32 C33 C34 C35 -1.4(9) . . . . ?
C33 C34 C35 C36 2.3(9) . . . . ?
C33 C34 C35 Br1 -177.3(4) . . . . ?
C34 C35 C36 C37 -1.0(9) . . . . ?
Br1 C35 C36 C37 178.6(4) . . . . ?
C35 C36 C37 C32 -1.1(8) . . . . ?
C33 C32 C37 C36 1.9(9) . . . . ?
C31 C32 C37 C36 -177.7(5) . . . . ?
C43 C38 C39 C40 -58.6(6) . . . . ?
C38 C39 C40 O4 179.3(4) . . . . ?
C38 C39 C40 C41 59.5(6) . . . . ?
O4 C40 C41 C60 -47.0(6) . . . . ?
C39 C40 C41 C60 72.8(6) . . . . ?
O4 C40 C41 C61 69.6(6) . . . . ?
C39 C40 C41 C61 -170.7(4) . . . . ?
O4 C40 C41 C42 -172.4(4) . . . . ?
C39 C40 C41 C42 -52.7(6) . . . . ?
C40 C41 C42 C47 176.8(5) . . . . ?
C60 C41 C42 C47 53.0(6) . . . . ?
C61 C41 C42 C47 -67.1(6) . . . . ?
C40 C41 C42 C43 47.6(6) . . . . ?
C60 C41 C42 C43 -76.2(6) . . . . ?
C61 C41 C42 C43 163.7(5) . . . . ?
C39 C38 C43 C62 -70.7(6) . . . . ?
C39 C38 C43 C42 52.8(6) . . . . ?
C39 C38 C43 C44 172.1(4) . . . . ?
C47 C42 C43 C38 -178.7(4) . . . . ?
C41 C42 C43 C38 -48.6(6) . . . . ?
C47 C42 C43 C62 -59.2(6) . . . . ?
C41 C42 C43 C62 71.0(6) . . . . ?
C47 C42 C43 C44 60.6(6) . . . . ?
C41 C42 C43 C44 -169.2(5) . . . . ?
C38 C43 C44 O5 64.8(6) . . . . ?
C62 C43 C44 O5 -52.0(6) . . . . ?
C42 C43 C44 O5 -175.4(4) . . . . ?
C38 C43 C44 C48 -59.9(6) . . . . ?
C62 C43 C44 C48 -176.7(5) . . . . ?
C42 C43 C44 C48 60.0(6) . . . . ?
C38 C43 C44 C45 179.1(5) . . . . ?
C62 C43 C44 C45 62.4(6) . . . . ?
C42 C43 C44 C45 -61.0(6) . . . . ?
O5 C44 C45 C63 -66.2(7) . . . . ?
C48 C44 C45 C63 59.2(7) . . . . ?
C43 C44 C45 C63 -178.8(5) . . . . ?
O5 C44 C45 C46 168.9(5) . . . . ?
C48 C44 C45 C46 -65.7(7) . . . . ?
C43 C44 C45 C46 56.3(7) . . . . ?
C63 C45 C46 C47 178.6(5) . . . . ?
C44 C45 C46 C47 -52.7(7) . . . . ?
C45 C46 C47 C42 51.4(7) . . . . ?
C43 C42 C47 C46 -55.3(6) . . . . ?
C41 C42 C47 C46 172.5(5) . . . . ?
O5 C44 C48 C49 15.2(8) . . . . ?
C45 C44 C48 C49 -105.9(6) . . . . ?
C43 C44 C48 C49 133.9(5) . . . . ?
C44 C48 C49 C50 -46.2(7) . . . . ?
C48 C49 C50 C51 67.2(6) . . . . ?
C48 C49 C50 C55 -160.0(5) . . . . ?
C49 C50 C51 O5 -55.9(6) . . . . ?
C55 C50 C51 O5 170.3(5) . . . . ?
C49 C50 C51 C52 -170.9(5) . . . . ?
C55 C50 C51 C52 55.3(6) . . . . ?
C49 C50 C51 C64 65.8(7) . . . . ?
C55 C50 C51 C64 -68.0(7) . . . . ?
O5 C51 C52 C53 -172.9(5) . . . . ?
C64 C51 C52 C53 72.6(6) . . . . ?
C50 C51 C52 C53 -55.2(6) . . . . ?
C51 C52 C53 C54 58.2(6) . . . . ?
C52 C53 C54 C55 -58.0(6) . . . . ?
C52 C53 C54 C59 166.5(5) . . . . ?
C53 C54 C55 C65 -70.0(6) . . . . ?
C59 C54 C55 C65 64.9(7) . . . . ?
C53 C54 C55 C56 170.3(5) . . . . ?
C59 C54 C55 C56 -54.8(6) . . . . ?
C53 C54 C55 C50 53.7(6) . . . . ?
C59 C54 C55 C50 -171.3(5) . . . . ?
C49 C50 C55 C65 -57.4(7) . . . . ?
C51 C50 C55 C65 72.3(6) . . . . ?
C49 C50 C55 C54 176.4(5) . . . . ?
C51 C50 C55 C54 -53.9(6) . . . . ?
C49 C50 C55 C56 60.9(7) . . . . ?
C51 C50 C55 C56 -169.5(5) . . . . ?
C65 C55 C56 C57 -71.1(7) . . . . ?
C54 C55 C56 C57 53.0(7) . . . . ?
C50 C55 C56 C57 168.7(5) . . . . ?
C55 C56 C57 C58 -54.8(8) . . . . ?
C56 C57 C58 C59 55.1(8) . . . . ?
C57 C58 C59 C66 73.2(7) . . . . ?
C57 C58 C59 C67 -170.7(5) . . . . ?
C57 C58 C59 C54 -52.9(7) . . . . ?
C53 C54 C59 C58 -171.2(5) . . . . ?
C55 C54 C59 C58 54.9(7) . . . . ?
C53 C54 C59 C66 64.5(7) . . . . ?
C55 C54 C59 C66 -69.4(7) . . . . ?
C53 C54 C59 C67 -55.5(7) . . . . ?
C55 C54 C59 C67 170.6(5) . . . . ?
O6 C68 C69 C74 -16.6(9) . . . . ?
O4 C68 C69 C74 164.1(5) . . . . ?
O6 C68 C69 C70 164.2(6) . . . . ?
O4 C68 C69 C70 -15.1(8) . . . . ?
C74 C69 C70 C71 0.7(8) . . . . ?
C68 C69 C70 C71 179.9(5) . . . . ?
C69 C70 C71 C72 -2.4(9) . . . . ?
C70 C71 C72 C73 1.8(9) . . . . ?
C70 C71 C72 Br2 -178.2(4) . . . . ?
C71 C72 C73 C74 0.5(9) . . . . ?
Br2 C72 C73 C74 -179.5(4) . . . . ?
C72 C73 C74 C69 -2.3(9) . . . . ?
C70 C69 C74 C73 1.6(9) . . . . ?
C68 C69 C74 C73 -177.6(5) . . . . ?
O3 C31 O1 C3 0.6(8) . . . . ?
C32 C31 O1 C3 -179.6(5) . . . . ?
C2 C3 O1 C31 120.0(5) . . . . ?
C4 C3 O1 C31 -114.7(5) . . . . ?
C8 C7 O2 C14 117.5(6) . . . . ?
C11 C7 O2 C14 -3.6(8) . . . . ?
C6 C7 O2 C14 -127.0(5) . . . . ?
C15 C14 O2 C7 139.0(5) . . . . ?
C27 C14 O2 C7 -104.6(6) . . . . ?
C13 C14 O2 C7 21.8(7) . . . . ?
O6 C68 O4 C40 -0.5(8) . . . . ?
C69 C68 O4 C40 178.8(4) . . . . ?
C39 C40 O4 C68 114.4(5) . . . . ?
C41 C40 O4 C68 -121.3(5) . . . . ?
C48 C44 O5 C51 -5.4(8) . . . . ?
C45 C44 O5 C51 117.0(6) . . . . ?
C43 C44 O5 C51 -127.9(5) . . . . ?
C52 C51 O5 C44 143.1(5) . . . . ?
C64 C51 O5 C44 -101.2(6) . . . . ?
C50 C51 O5 C44 26.0(7) . . . . ?

_refine_diff_density_max         0.327
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.072


#END===============================================
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: C6H6, (CH2Cl)2, iPrOH'
####################################################################### 
# 
# 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_FB1412Ba
_database_code_depnum_ccdc_archive 'CCDC 1529116'
_audit_update_record             
;
2017-01-22 deposited with the CCDC.
2017-10-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            Cupacinoxepin
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H50 O3'
_chemical_formula_weight         458.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0192 0.0096 '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'
O O 0.0517 0.0336 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           77
_space_group_name_H-M_alt        'P 42'
_space_group_name_Hall           'P 4c'

_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'
'-y, x, z+1/2'
'y, -x, z+1/2'

_cell_length_a                   18.4576(2)
_cell_length_b                   18.4576
_cell_length_c                   7.45850(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2540.98(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5731
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      66.64
_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   0.7160
_exptl_transmission_factor_max   0.7923
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.550
_shelx_estimated_absorpt_T_min   0.814
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker Photon CMOS Detector, D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24885
_diffrn_reflns_av_unetI/netI     0.1067
_diffrn_reflns_av_R_equivalents  0.1428
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.386
_diffrn_reflns_theta_max         66.757
_diffrn_reflns_theta_full        66.757
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4490
_reflns_number_gt                3149
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.841
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.995

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  'Microsoft Word'
_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)+(0.0396P)²+0.5688P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1034 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(2)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         4490
_refine_ls_number_parameters     307
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0571
_refine_ls_wR_factor_ref         0.1122
_refine_ls_wR_factor_gt          0.0986
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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
C1 C 0.6678(2) 1.0230(2) 0.2953(6) 0.0149(11) Uani 1 1 d . . . . .
H1A H 0.6618 0.9982 0.1786 0.018 Uiso 1 1 calc R U . . .
H1B H 0.6186 1.0342 0.3407 0.018 Uiso 1 1 calc R U . . .
C2 C 0.7063(2) 1.0949(2) 0.2602(7) 0.0188(11) Uani 1 1 d . . . . .
H2A H 0.6755 1.1253 0.1821 0.023 Uiso 1 1 calc R U . . .
H2B H 0.7126 1.1208 0.3755 0.023 Uiso 1 1 calc R U . . .
C3 C 0.7784(3) 1.0859(2) 0.1743(7) 0.0198(11) Uani 1 1 d . . . . .
C4 C 0.8301(2) 1.0384(2) 0.4621(7) 0.0179(11) Uani 1 1 d . . . . .
C5 C 0.7585(2) 1.0089(2) 0.5492(6) 0.0153(11) Uani 1 1 d . . . . .
H5 H 0.7321 1.0527 0.5938 0.018 Uiso 1 1 calc R U . . .
C6 C 0.7038(2) 0.9680(2) 0.4289(6) 0.0131(10) Uani 1 1 d . . . . .
C7 C 0.6387(2) 0.9385(2) 0.5465(6) 0.0125(10) Uani 1 1 d . . . . .
H7 H 0.6127 0.9832 0.5865 0.015 Uiso 1 1 calc R U . . .
C8 C 0.6577(2) 0.8987(2) 0.7229(6) 0.0130(10) Uani 1 1 d . . . . .
C9 C 0.7109(2) 0.9462(2) 0.8260(6) 0.0161(11) Uani 1 1 d . . . . .
H9A H 0.6862 0.9914 0.8625 0.019 Uiso 1 1 calc R U . . .
H9B H 0.7261 0.9205 0.9363 0.019 Uiso 1 1 calc R U . . .
C10 C 0.7779(2) 0.9653(2) 0.7166(6) 0.0145(11) Uani 1 1 d . . . . .
H10A H 0.8030 0.9202 0.6804 0.017 Uiso 1 1 calc R U . . .
H10B H 0.8117 0.9939 0.7918 0.017 Uiso 1 1 calc R U . . .
C11 C 0.5834(2) 0.8985(2) 0.4287(6) 0.0164(11) Uani 1 1 d . . . . .
H11A H 0.5770 0.9260 0.3158 0.020 Uiso 1 1 calc R U . . .
H11B H 0.6034 0.8504 0.3972 0.020 Uiso 1 1 calc R U . . .
C12 C 0.5090(2) 0.8878(2) 0.5152(6) 0.0165(11) Uani 1 1 d . . . . .
H12A H 0.4936 0.9339 0.5712 0.020 Uiso 1 1 calc R U . . .
H12B H 0.4734 0.8756 0.4206 0.020 Uiso 1 1 calc R U . . .
C13 C 0.5083(2) 0.8282(2) 0.6570(7) 0.0149(11) Uani 1 1 d . . . . .
H13 H 0.5490 0.7953 0.6219 0.018 Uiso 1 1 calc R U . . .
C14 C 0.5296(2) 0.8562(2) 0.8447(7) 0.0151(11) Uani 1 1 d . . . . .
C15 C 0.5396(2) 0.7924(2) 0.9722(7) 0.0158(11) Uani 1 1 d . . . . .
H15A H 0.5495 0.8108 1.0945 0.019 Uiso 1 1 calc R U . . .
H15B H 0.5819 0.7633 0.9335 0.019 Uiso 1 1 calc R U . . .
C16 C 0.4720(2) 0.7440(2) 0.9761(7) 0.0180(11) Uani 1 1 d . . . . .
H16A H 0.4803 0.7029 1.0588 0.022 Uiso 1 1 calc R U . . .
H16B H 0.4303 0.7722 1.0216 0.022 Uiso 1 1 calc R U . . .
C17 C 0.4545(2) 0.7150(2) 0.7887(7) 0.0160(11) Uani 1 1 d . . . . .
H17 H 0.5011 0.6935 0.7459 0.019 Uiso 1 1 calc R U . . .
C18 C 0.4392(2) 0.7780(2) 0.6555(6) 0.0145(11) Uani 1 1 d . . . . .
C19 C 0.4324(2) 0.7445(2) 0.4659(7) 0.0203(11) Uani 1 1 d . . . . .
H19A H 0.4185 0.7830 0.3801 0.024 Uiso 1 1 calc R U . . .
H19B H 0.4802 0.7254 0.4287 0.024 Uiso 1 1 calc R U . . .
C20 C 0.3766(2) 0.6834(2) 0.4567(7) 0.0244(12) Uani 1 1 d . . . . .
H20A H 0.3277 0.7033 0.4806 0.029 Uiso 1 1 calc R U . . .
H20B H 0.3764 0.6623 0.3346 0.029 Uiso 1 1 calc R U . . .
C21 C 0.3934(2) 0.6244(2) 0.5924(7) 0.0232(13) Uani 1 1 d . . . . .
H21A H 0.4395 0.6007 0.5579 0.028 Uiso 1 1 calc R U . . .
H21B H 0.3548 0.5873 0.5865 0.028 Uiso 1 1 calc R U . . .
C22 C 0.3999(2) 0.6506(2) 0.7857(7) 0.0196(11) Uani 1 1 d . . . . .
C23 C 0.8499(3) 1.1107(2) 0.5449(7) 0.0221(12) Uani 1 1 d . . . . .
H23A H 0.8989 1.1244 0.5072 0.033 Uiso 1 1 calc R U . . .
H23B H 0.8483 1.1068 0.6759 0.033 Uiso 1 1 calc R U . . .
H23C H 0.8154 1.1477 0.5051 0.033 Uiso 1 1 calc R U . . .
C24 C 0.8944(2) 0.9872(3) 0.4792(7) 0.0235(12) Uani 1 1 d . . . . .
H24A H 0.8807 0.9390 0.4357 0.035 Uiso 1 1 calc R U . . .
H24B H 0.9091 0.9839 0.6052 0.035 Uiso 1 1 calc R U . . .
H24C H 0.9349 1.0057 0.4076 0.035 Uiso 1 1 calc R U . . .
C25 C 0.7410(2) 0.9072(2) 0.3227(6) 0.0175(11) Uani 1 1 d . . . . .
H25A H 0.7047 0.8811 0.2518 0.026 Uiso 1 1 calc R U . . .
H25B H 0.7645 0.8736 0.4061 0.026 Uiso 1 1 calc R U . . .
H25C H 0.7774 0.9282 0.2424 0.026 Uiso 1 1 calc R U . . .
C26 C 0.6888(2) 0.8224(2) 0.7068(7) 0.0171(11) Uani 1 1 d . . . . .
H26A H 0.6565 0.7926 0.6332 0.026 Uiso 1 1 calc R U . . .
H26B H 0.6932 0.8009 0.8265 0.026 Uiso 1 1 calc R U . . .
H26C H 0.7367 0.8247 0.6505 0.026 Uiso 1 1 calc R U . . .
C27 C 0.4760(2) 0.9093(2) 0.9307(7) 0.0194(11) Uani 1 1 d . . . . .
H27A H 0.4613 0.9456 0.8421 0.029 Uiso 1 1 calc R U . . .
H27B H 0.4991 0.9334 1.0328 0.029 Uiso 1 1 calc R U . . .
H27C H 0.4332 0.8827 0.9722 0.029 Uiso 1 1 calc R U . . .
C28 C 0.3695(2) 0.8217(2) 0.6936(7) 0.0209(12) Uani 1 1 d . . . . .
H28A H 0.3754 0.8713 0.6496 0.031 Uiso 1 1 calc R U . . .
H28B H 0.3603 0.8226 0.8230 0.031 Uiso 1 1 calc R U . . .
H28C H 0.3285 0.7988 0.6323 0.031 Uiso 1 1 calc R U . . .
C29 C 0.3254(2) 0.6689(2) 0.8644(8) 0.0261(13) Uani 1 1 d . . . . .
H29A H 0.3006 0.7035 0.7859 0.039 Uiso 1 1 calc R U . . .
H29B H 0.3314 0.6902 0.9837 0.039 Uiso 1 1 calc R U . . .
H29C H 0.2964 0.6245 0.8737 0.039 Uiso 1 1 calc R U . . .
C30 C 0.4308(3) 0.5874(2) 0.8940(8) 0.0286(14) Uani 1 1 d . . . . .
H30A H 0.4024 0.5436 0.8699 0.043 Uiso 1 1 calc R U . . .
H30B H 0.4285 0.5988 1.0221 0.043 Uiso 1 1 calc R U . . .
H30C H 0.4813 0.5791 0.8592 0.043 Uiso 1 1 calc R U . . .
O1 O 0.59502(15) 0.90154(15) 0.8423(4) 0.0149(7) Uani 1 1 d . . . . .
O2 O 0.79219(17) 1.10647(18) 0.0238(5) 0.0281(8) Uani 1 1 d . . . . .
O3 O 0.82904(16) 1.04814(16) 0.2643(4) 0.0201(8) Uani 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
C1 C2 1.528(6) . ?
C1 C6 1.571(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.485(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O2 1.212(6) . ?
C3 O3 1.346(5) . ?
C4 O3 1.487(6) . ?
C4 C23 1.516(6) . ?
C4 C24 1.523(6) . ?
C4 C5 1.569(6) . ?
C5 C10 1.528(6) . ?
C5 C6 1.548(6) . ?
C5 H5 1.0000 . ?
C6 C25 1.535(6) . ?
C6 C7 1.583(6) . ?
C7 C11 1.537(6) . ?
C7 C8 1.547(6) . ?
C7 H7 1.0000 . ?
C8 O1 1.461(5) . ?
C8 C26 1.525(6) . ?
C8 C9 1.526(6) . ?
C9 C10 1.523(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.529(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.527(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.543(7) . ?
C13 C18 1.576(6) . ?
C13 H13 1.0000 . ?
C14 O1 1.469(5) . ?
C14 C15 1.526(6) . ?
C14 C27 1.533(6) . ?
C15 C16 1.535(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.531(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.555(6) . ?
C17 C22 1.557(6) . ?
C17 H17 1.0000 . ?
C18 C28 1.545(6) . ?
C18 C19 1.549(6) . ?
C19 C20 1.530(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.519(7) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.526(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C30 1.530(6) . ?
C22 C29 1.533(6) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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
C2 C1 C6 118.2(4) . . ?
C2 C1 H1A 107.7 . . ?
C6 C1 H1A 107.7 . . ?
C2 C1 H1B 107.7 . . ?
C6 C1 H1B 107.7 . . ?
H1A C1 H1B 107.1 . . ?
C3 C2 C1 113.1(4) . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.8 . . ?
O2 C3 O3 118.5(4) . . ?
O2 C3 C2 123.6(5) . . ?
O3 C3 C2 117.7(4) . . ?
O3 C4 C23 107.5(4) . . ?
O3 C4 C24 99.6(4) . . ?
C23 C4 C24 108.9(4) . . ?
O3 C4 C5 116.3(4) . . ?
C23 C4 C5 109.9(4) . . ?
C24 C4 C5 114.1(4) . . ?
C10 C5 C6 111.7(3) . . ?
C10 C5 C4 108.8(3) . . ?
C6 C5 C4 118.6(4) . . ?
C10 C5 H5 105.6 . . ?
C6 C5 H5 105.6 . . ?
C4 C5 H5 105.6 . . ?
C25 C6 C5 111.3(3) . . ?
C25 C6 C1 109.5(4) . . ?
C5 C6 C1 109.1(3) . . ?
C25 C6 C7 111.9(3) . . ?
C5 C6 C7 110.0(4) . . ?
C1 C6 C7 104.7(3) . . ?
C11 C7 C8 114.0(3) . . ?
C11 C7 C6 110.7(4) . . ?
C8 C7 C6 117.6(3) . . ?
C11 C7 H7 104.3 . . ?
C8 C7 H7 104.3 . . ?
C6 C7 H7 104.3 . . ?
O1 C8 C26 112.3(3) . . ?
O1 C8 C9 100.5(3) . . ?
C26 C8 C9 109.1(3) . . ?
O1 C8 C7 108.8(3) . . ?
C26 C8 C7 117.2(4) . . ?
C9 C8 C7 107.5(3) . . ?
C10 C9 C8 112.7(4) . . ?
C10 C9 H9A 109.0 . . ?
C8 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
C8 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 C5 111.7(3) . . ?
C9 C10 H10A 109.3 . . ?
C5 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C5 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
C12 C11 C7 114.7(4) . . ?
C12 C11 H11A 108.6 . . ?
C7 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
C7 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
C13 C12 C11 113.1(4) . . ?
C13 C12 H12A 109.0 . . ?
C11 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
C11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C12 C13 C14 112.6(3) . . ?
C12 C13 C18 115.2(4) . . ?
C14 C13 C18 114.2(4) . . ?
C12 C13 H13 104.5 . . ?
C14 C13 H13 104.5 . . ?
C18 C13 H13 104.5 . . ?
O1 C14 C15 110.3(3) . . ?
O1 C14 C27 99.9(3) . . ?
C15 C14 C27 108.1(4) . . ?
O1 C14 C13 112.9(4) . . ?
C15 C14 C13 109.7(3) . . ?
C27 C14 C13 115.4(4) . . ?
C14 C15 C16 111.2(4) . . ?
C14 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
C14 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C17 C16 C15 111.0(4) . . ?
C17 C16 H16A 109.4 . . ?
C15 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C16 C17 C18 111.1(4) . . ?
C16 C17 C22 114.6(4) . . ?
C18 C17 C22 116.4(4) . . ?
C16 C17 H17 104.4 . . ?
C18 C17 H17 104.4 . . ?
C22 C17 H17 104.4 . . ?
C28 C18 C19 107.9(4) . . ?
C28 C18 C17 115.0(4) . . ?
C19 C18 C17 107.4(4) . . ?
C28 C18 C13 111.5(3) . . ?
C19 C18 C13 107.9(4) . . ?
C17 C18 C13 106.8(3) . . ?
C20 C19 C18 113.0(4) . . ?
C20 C19 H19A 109.0 . . ?
C18 C19 H19A 109.0 . . ?
C20 C19 H19B 109.0 . . ?
C18 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C21 C20 C19 111.1(4) . . ?
C21 C20 H20A 109.4 . . ?
C19 C20 H20A 109.4 . . ?
C21 C20 H20B 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C20 C21 C22 114.7(4) . . ?
C20 C21 H21A 108.6 . . ?
C22 C21 H21A 108.6 . . ?
C20 C21 H21B 108.6 . . ?
C22 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
C21 C22 C30 106.6(4) . . ?
C21 C22 C29 111.1(4) . . ?
C30 C22 C29 107.4(4) . . ?
C21 C22 C17 107.9(4) . . ?
C30 C22 C17 109.5(4) . . ?
C29 C22 C17 114.0(4) . . ?
C4 C23 H23A 109.5 . . ?
C4 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C4 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C4 C24 H24A 109.5 . . ?
C4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C4 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C6 C25 H25A 109.5 . . ?
C6 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C6 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C8 C26 H26A 109.5 . . ?
C8 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C8 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C14 C27 H27A 109.5 . . ?
C14 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C14 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C18 C28 H28A 109.5 . . ?
C18 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C18 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C22 C29 H29A 109.5 . . ?
C22 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C22 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C22 C30 H30A 109.5 . . ?
C22 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C22 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C8 O1 C14 129.6(3) . . ?
C3 O3 C4 124.5(4) . . ?

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
C6 C1 C2 C3 63.4(6) . . . . ?
C1 C2 C3 O2 114.0(5) . . . . ?
C1 C2 C3 O3 -61.1(6) . . . . ?
O3 C4 C5 C10 150.0(4) . . . . ?
C23 C4 C5 C10 -87.7(5) . . . . ?
C24 C4 C5 C10 34.8(5) . . . . ?
O3 C4 C5 C6 20.9(6) . . . . ?
C23 C4 C5 C6 143.2(4) . . . . ?
C24 C4 C5 C6 -94.3(5) . . . . ?
C10 C5 C6 C25 -76.4(5) . . . . ?
C4 C5 C6 C25 51.3(5) . . . . ?
C10 C5 C6 C1 162.5(3) . . . . ?
C4 C5 C6 C1 -69.7(5) . . . . ?
C10 C5 C6 C7 48.2(5) . . . . ?
C4 C5 C6 C7 176.0(4) . . . . ?
C2 C1 C6 C25 -102.5(5) . . . . ?
C2 C1 C6 C5 19.6(5) . . . . ?
C2 C1 C6 C7 137.3(4) . . . . ?
C25 C6 C7 C11 -56.4(5) . . . . ?
C5 C6 C7 C11 179.3(4) . . . . ?
C1 C6 C7 C11 62.2(4) . . . . ?
C25 C6 C7 C8 77.1(5) . . . . ?
C5 C6 C7 C8 -47.2(5) . . . . ?
C1 C6 C7 C8 -164.3(4) . . . . ?
C11 C7 C8 O1 -70.3(4) . . . . ?
C6 C7 C8 O1 157.7(3) . . . . ?
C11 C7 C8 C26 58.5(5) . . . . ?
C6 C7 C8 C26 -73.5(5) . . . . ?
C11 C7 C8 C9 -178.3(4) . . . . ?
C6 C7 C8 C9 49.7(5) . . . . ?
O1 C8 C9 C10 -169.2(3) . . . . ?
C26 C8 C9 C10 72.6(5) . . . . ?
C7 C8 C9 C10 -55.4(4) . . . . ?
C8 C9 C10 C5 62.0(5) . . . . ?
C6 C5 C10 C9 -57.1(5) . . . . ?
C4 C5 C10 C9 170.1(4) . . . . ?
C8 C7 C11 C12 62.1(5) . . . . ?
C6 C7 C11 C12 -162.6(4) . . . . ?
C7 C11 C12 C13 -75.6(5) . . . . ?
C11 C12 C13 C14 87.3(5) . . . . ?
C11 C12 C13 C18 -139.4(4) . . . . ?
C12 C13 C14 O1 -47.4(5) . . . . ?
C18 C13 C14 O1 178.8(3) . . . . ?
C12 C13 C14 C15 -170.9(3) . . . . ?
C18 C13 C14 C15 55.3(5) . . . . ?
C12 C13 C14 C27 66.7(5) . . . . ?
C18 C13 C14 C27 -67.1(5) . . . . ?
O1 C14 C15 C16 -179.7(3) . . . . ?
C27 C14 C15 C16 72.0(5) . . . . ?
C13 C14 C15 C16 -54.7(5) . . . . ?
C14 C15 C16 C17 58.5(5) . . . . ?
C15 C16 C17 C18 -60.5(4) . . . . ?
C15 C16 C17 C22 165.0(3) . . . . ?
C16 C17 C18 C28 -67.3(5) . . . . ?
C22 C17 C18 C28 66.3(5) . . . . ?
C16 C17 C18 C19 172.5(3) . . . . ?
C22 C17 C18 C19 -53.9(5) . . . . ?
C16 C17 C18 C13 57.0(4) . . . . ?
C22 C17 C18 C13 -169.4(4) . . . . ?
C12 C13 C18 C28 -61.8(5) . . . . ?
C14 C13 C18 C28 70.8(5) . . . . ?
C12 C13 C18 C19 56.6(5) . . . . ?
C14 C13 C18 C19 -170.9(4) . . . . ?
C12 C13 C18 C17 171.7(4) . . . . ?
C14 C13 C18 C17 -55.7(5) . . . . ?
C28 C18 C19 C20 -70.7(5) . . . . ?
C17 C18 C19 C20 53.9(5) . . . . ?
C13 C18 C19 C20 168.6(4) . . . . ?
C18 C19 C20 C21 -56.0(5) . . . . ?
C19 C20 C21 C22 55.4(5) . . . . ?
C20 C21 C22 C30 -169.5(4) . . . . ?
C20 C21 C22 C29 73.8(5) . . . . ?
C20 C21 C22 C17 -51.9(5) . . . . ?
C16 C17 C22 C21 -175.3(4) . . . . ?
C18 C17 C22 C21 52.7(5) . . . . ?
C16 C17 C22 C30 -59.7(5) . . . . ?
C18 C17 C22 C30 168.3(4) . . . . ?
C16 C17 C22 C29 60.7(5) . . . . ?
C18 C17 C22 C29 -71.2(6) . . . . ?
C26 C8 O1 C14 -50.1(5) . . . . ?
C9 C8 O1 C14 -166.0(4) . . . . ?
C7 C8 O1 C14 81.3(5) . . . . ?
C15 C14 O1 C8 92.7(5) . . . . ?
C27 C14 O1 C8 -153.6(4) . . . . ?
C13 C14 O1 C8 -30.4(5) . . . . ?
O2 C3 O3 C4 160.8(4) . . . . ?
C2 C3 O3 C4 -23.8(6) . . . . ?
C23 C4 O3 C3 -71.1(5) . . . . ?
C24 C4 O3 C3 175.5(4) . . . . ?
C5 C4 O3 C3 52.4(5) . . . . ?

_refine_diff_density_max         0.190
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.050


#END===============================================
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Aceton/ Hexan'
