# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2015

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

data_2a
_database_code_depnum_ccdc_archive 'CCDC 1401765'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             13-04-26
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 041gwp12
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   15.6111(1)
_cell_length_b                   15.6111(1)
_cell_length_c                   10.5050(1)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2560.14(3)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P -4 '
_symmetry_space_group_name_Hall  'P -4'

_refine_special_details          
;
On initial refinement, some of the ADPs became very
prolate, suggesting the presence of disorder in one
adamantanol and one butyl chain.  The structure was
examined for the possibility of merohedral twinning,
however, the twin scale factor refined to 1, so the twin
law was removed and the disorder modeled.  The
occupancies for the disordered adamantanol were highly
correlated with the ADPs due to the very close proximity
of the two components and the large degree of overlap
between the models, so the occupancies were estimated
from size of the ADPs.
;

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C52 H136 F2 N2 O2 
# Dc =      1.12 Fooo =    968.00 Mu =      5.24 M =    429.83
# Found Formula = C56 H100.00 F1 N1 O4 
# Dc =      1.13 FOOO =    968.00 Mu =      5.46 M =    435.21

_chemical_formula_sum            'C56 H100 F1 N1 O4'
_chemical_formula_moiety         'C16 H36 N, 4(C10 H16 O), F'
_chemical_compound_source        .
_chemical_formula_weight         870.41


_cell_measurement_reflns_used    12745
_cell_measurement_theta_min      3
_cell_measurement_theta_max      77
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.20
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_max          0.23

_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             968
_exptl_absorpt_coefficient_mu    0.546

# Sheldrick geometric approximatio 0.89 0.90 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_T_max  0.90
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            5329
_reflns_number_total             5329
_diffrn_reflns_av_R_equivalents  0.022
# Number of reflections without Friedels Law is 5329 
# Number of reflections with Friedels Law is 2845 
# Theoretical number of reflections is about 2706 


_diffrn_reflns_theta_min         2.831
_diffrn_reflns_theta_max         76.964
_diffrn_measured_fraction_theta_max 0.993

_diffrn_reflns_theta_full        75.425
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       13
_reflns_limit_h_min              -19
_reflns_limit_h_max              19
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              13

_oxford_diffrn_Wilson_B_factor   3.48
_oxford_diffrn_Wilson_scale      0.03

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.26
_refine_diff_density_max         0.29


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         3520
_refine_ls_number_restraints     1255
_refine_ls_number_parameters     406
_oxford_refine_ls_R_factor_ref   0.0582
_refine_ls_wR_factor_ref         0.1565
_refine_ls_goodness_of_fit_ref   1.0106
_refine_ls_shift/su_max          0.0002767
_refine_ls_shift/su_mean         0.0000177


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3520
_refine_ls_R_factor_all          0.0582
_refine_ls_wR_factor_all         0.1565

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3442
_refine_ls_R_factor_gt           0.0574
_refine_ls_wR_factor_gt          0.1551

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration unk


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.11P)² + 1.04P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
F1 F 0.0000 0.0000 1.0000 0.0354 1.0000 Uani S T . . . .
O1 O 0.02580(14) 0.11973(12) 0.83372(17) 0.0685 1.0000 Uani D . . . . .
C11 C 0.03491(10) 0.20649(9) 0.87228(13) 0.0382 1.0000 Uani D . . . . .
C12 C 0.12517(13) 0.23753(14) 0.8441(2) 0.0531 1.0000 Uani D . . . . .
C13 C 0.13469(11) 0.33128(12) 0.8830(2) 0.0590 1.0000 Uani D . . . . .
C14 C 0.07107(18) 0.38465(12) 0.8110(2) 0.0565 1.0000 Uani D . . . . .
C15 C -0.01896(12) 0.35528(11) 0.84126(17) 0.0485 1.0000 Uani D . . . . .
C16 C -0.02846(12) 0.26221(14) 0.80068(17) 0.0451 1.0000 Uani D . . . . .
C17 C 0.01791(13) 0.21540(12) 1.01546(19) 0.0436 1.0000 Uani D . . . . .
C18 C 0.11815(14) 0.33891(14) 1.0258(2) 0.0543 1.0000 Uani D . . . . .
C19 C -0.03558(12) 0.36299(13) 0.9834(2) 0.0466 1.0000 Uani D . . . . .
C20 C 0.02833(12) 0.30938(11) 1.05589(15) 0.0395 1.0000 Uani D . . . . .
F2 F 0.5000 0.5000 0.5000 0.0510 1.0000 Uani S T . . . .
O2 O 0.51320(18) 0.36712(17) 0.6603(3) 0.0647 0.7500 Uani D . . 1 1 .
C21 C 0.46312(13) 0.29387(13) 0.6270(2) 0.0401 0.7500 Uani D . . 1 1 .
C22 C 0.47692(16) 0.27094(18) 0.4874(3) 0.0463 0.7500 Uani D . . 1 1 .
C23 C 0.42330(17) 0.19147(16) 0.4526(2) 0.0480 0.7500 Uani D . . 1 1 .
C24 C 0.4498(2) 0.11734(15) 0.5354(3) 0.0598 0.7500 Uani D . . 1 1 .
C25 C 0.43491(19) 0.13967(15) 0.6755(2) 0.0628 0.7500 Uani D . . 1 1 .
C26 C 0.48915(17) 0.21753(19) 0.7092(3) 0.0568 0.7500 Uani D . . 1 1 .
C27 C 0.36827(19) 0.31241(16) 0.6483(3) 0.0507 0.7500 Uani D . . 1 1 .
C28 C 0.32976(18) 0.21177(19) 0.4741(3) 0.0557 0.7500 Uani D . . 1 1 .
C29 C 0.3417(2) 0.1600(2) 0.6973(3) 0.0668 0.7500 Uani D . . 1 1 .
C30 C 0.31491(14) 0.23427(17) 0.6132(2) 0.0572 0.7500 Uani D . . 1 1 .
O102 O 0.4525(6) 0.3859(4) 0.6653(7) 0.0600 0.2500 Uani D . . 1 2 .
C121 C 0.4466(4) 0.2979(3) 0.6305(5) 0.0546 0.2500 Uani D . . 1 2 .
C122 C 0.4474(6) 0.2889(4) 0.4864(6) 0.0622 0.2500 Uani D . . 1 2 .
C123 C 0.4419(6) 0.1940(4) 0.4492(5) 0.0650 0.2500 Uani D . . 1 2 .
C124 C 0.5172(6) 0.1460(4) 0.5060(7) 0.0643 0.2500 Uani D . . 1 2 .
C125 C 0.5154(5) 0.1535(4) 0.6495(6) 0.0583 0.2500 Uani D . . 1 2 .
C126 C 0.5223(4) 0.2481(4) 0.6855(6) 0.0539 0.2500 Uani D . . 1 2 .
C127 C 0.3639(4) 0.2596(4) 0.6817(7) 0.0612 0.2500 Uani D . . 1 2 .
C128 C 0.3591(6) 0.1578(5) 0.5000(8) 0.0706 0.2500 Uani D . . 1 2 .
C129 C 0.4324(7) 0.1174(4) 0.7006(6) 0.0611 0.2500 Uani D . . 1 2 .
C130 C 0.3573(5) 0.1653(4) 0.6437(8) 0.0670 0.2500 Uani D . . 1 2 .
N31 N 0.0000 0.0000 0.5000 0.0328 1.0000 Uani DS T . . . .
C32 C 0.02463(18) 0.07272(11) 0.41222(11) 0.0381 0.259(9) Uani D . P 2 1 .
C33 C 0.0283(10) 0.1623(6) 0.4729(5) 0.0438 0.259(9) Uani D . P 2 1 .
C34 C 0.0561(7) 0.2260(6) 0.3753(8) 0.0545 0.259(9) Uani D . P 2 1 .
C35 C 0.1472(8) 0.2313(8) 0.3543(13) 0.0596 0.259(9) Uani D . P 2 1 .
C132 C 0.02463(18) 0.07272(11) 0.41222(11) 0.0381 0.741(9) Uani D . P 2 2 .
C133 C 0.0587(4) 0.1519(3) 0.4748(3) 0.0449 0.741(9) Uani D . P 2 2 .
C134 C 0.0854(5) 0.2153(3) 0.3740(3) 0.0645 0.741(9) Uani D . P 2 2 .
C135 C 0.1036(4) 0.3013(3) 0.4193(4) 0.0608 0.741(9) Uani D . P 2 2 .
N41 N 0.5000 0.5000 1.0000 0.0215 1.0000 Uani S T . . . .
C42 C 0.57648(14) 0.48748(16) 0.9119(2) 0.0263 1.0000 Uani . . . . . .
C43 C 0.66295(16) 0.48362(17) 0.9793(3) 0.0334 1.0000 Uani . . . . . .
C44 C 0.73163(17) 0.44714(17) 0.8922(3) 0.0361 1.0000 Uani . . . . . .
C45 C 0.72284(18) 0.35232(19) 0.8698(3) 0.0466 1.0000 Uani . . . . . .
H121 H 0.1647 0.2017 0.8884 0.0644 1.0000 Uiso R . . . . .
H122 H 0.1325 0.2337 0.7528 0.0629 1.0000 Uiso R . . . . .
H131 H 0.1925 0.3497 0.8604 0.0708 1.0000 Uiso R . . . . .
H142 H 0.0785 0.4458 0.8351 0.0685 1.0000 Uiso R . . . . .
H141 H 0.0801 0.3782 0.7214 0.0687 1.0000 Uiso R . . . . .
H151 H -0.0597 0.3907 0.7941 0.0586 1.0000 Uiso R . . . . .
H161 H -0.0848 0.2433 0.8223 0.0549 1.0000 Uiso R . . . . .
H162 H -0.0190 0.2556 0.7077 0.0537 1.0000 Uiso R . . . . .
H171 H 0.0598 0.1819 1.0620 0.0524 1.0000 Uiso R . . . . .
H172 H -0.0396 0.1979 1.0385 0.0529 1.0000 Uiso R . . . . .
H182 H 0.1262 0.3977 1.0541 0.0649 1.0000 Uiso R . . . . .
H181 H 0.1592 0.3012 1.0680 0.0636 1.0000 Uiso R . . . . .
H192 H -0.0274 0.4235 1.0084 0.0555 1.0000 Uiso R . . . . .
H191 H -0.0946 0.3420 1.0032 0.0564 1.0000 Uiso R . . . . .
H201 H 0.0181 0.3167 1.1478 0.0460 1.0000 Uiso R . . . . .
H221 H 0.5385 0.2588 0.4720 0.0558 0.7500 Uiso R . . 1 1 .
H222 H 0.4588 0.3196 0.4340 0.0552 0.7500 Uiso R . . 1 1 .
H231 H 0.4331 0.1765 0.3625 0.0579 0.7500 Uiso R . . 1 1 .
H241 H 0.5122 0.1077 0.5235 0.0718 0.7500 Uiso R . . 1 1 .
H242 H 0.4174 0.0664 0.5107 0.0724 0.7500 Uiso R . . 1 1 .
H251 H 0.4520 0.0929 0.7300 0.0762 0.7500 Uiso R . . 1 1 .
H262 H 0.4833 0.2329 0.7991 0.0677 0.7500 Uiso R . . 1 1 .
H261 H 0.5472 0.2059 0.6843 0.0666 0.7500 Uiso R . . 1 1 .
H271 H 0.3574 0.3219 0.7402 0.0604 0.7500 Uiso R . . 1 1 .
H272 H 0.3503 0.3622 0.5971 0.0610 0.7500 Uiso R . . 1 1 .
H281 H 0.3125 0.2611 0.4193 0.0670 0.7500 Uiso R . . 1 1 .
H282 H 0.2950 0.1612 0.4536 0.0669 0.7500 Uiso R . . 1 1 .
H291 H 0.3341 0.1736 0.7866 0.0803 0.7500 Uiso R . . 1 1 .
H292 H 0.3048 0.1106 0.6747 0.0805 0.7500 Uiso R . . 1 1 .
H301 H 0.2529 0.2486 0.6259 0.0695 0.7500 Uiso R . . 1 1 .
H1221 H 0.4993 0.3144 0.4505 0.0748 0.2500 Uiso R . . 1 2 .
H1222 H 0.3975 0.3179 0.4528 0.0748 0.2500 Uiso R . . 1 2 .
H1231 H 0.4438 0.1884 0.3562 0.0780 0.2500 Uiso R . . 1 2 .
H1241 H 0.5702 0.1706 0.4750 0.0771 0.2500 Uiso R . . 1 2 .
H1242 H 0.5139 0.0861 0.4819 0.0770 0.2500 Uiso R . . 1 2 .
H1251 H 0.5633 0.1213 0.6860 0.0701 0.2500 Uiso R . . 1 2 .
H1262 H 0.5233 0.2550 0.7774 0.0638 0.2500 Uiso R . . 1 2 .
H1261 H 0.5745 0.2708 0.6490 0.0641 0.2500 Uiso R . . 1 2 .
H1272 H 0.3625 0.2649 0.7730 0.0727 0.2500 Uiso R . . 1 2 .
H1271 H 0.3158 0.2904 0.6450 0.0729 0.2500 Uiso R . . 1 2 .
H1282 H 0.3560 0.0976 0.4770 0.0841 0.2500 Uiso R . . 1 2 .
H1281 H 0.3107 0.1877 0.4642 0.0841 0.2500 Uiso R . . 1 2 .
H1292 H 0.4311 0.1225 0.7923 0.0730 0.2500 Uiso R . . 1 2 .
H1291 H 0.4286 0.0575 0.6775 0.0729 0.2500 Uiso R . . 1 2 .
H1301 H 0.3030 0.1414 0.6761 0.0802 0.2500 Uiso R . . 1 2 .
H322 H -0.0195 0.0761 0.3486 0.0457 0.259(9) Uiso R . P 2 1 .
H321 H 0.0786 0.0587 0.3720 0.0459 0.259(9) Uiso R . P 2 1 .
H332 H 0.0715 0.1608 0.5402 0.0589 0.259(9) Uiso R . P 2 1 .
H331 H -0.0265 0.1785 0.5086 0.0591 0.259(9) Uiso R . P 2 1 .
H342 H 0.0357 0.2814 0.4038 0.0802 0.259(9) Uiso R . P 2 1 .
H341 H 0.0283 0.2120 0.2954 0.0801 0.259(9) Uiso R . P 2 1 .
H352 H 0.1593 0.2781 0.2970 0.0979 0.259(9) Uiso R . P 2 1 .
H351 H 0.1751 0.2419 0.4346 0.0980 0.259(9) Uiso R . P 2 1 .
H353 H 0.1691 0.1793 0.3189 0.0979 0.259(9) Uiso R . P 2 1 .
H1321 H 0.0668 0.0495 0.3532 0.0448 0.741(9) Uiso R . P 2 2 .
H1322 H -0.0261 0.0881 0.3676 0.0448 0.741(9) Uiso R . P 2 2 .
H1331 H 0.1078 0.1409 0.5283 0.0549 0.741(9) Uiso R . P 2 2 .
H1332 H 0.0131 0.1761 0.5252 0.0556 0.741(9) Uiso R . P 2 2 .
H1341 H 0.1346 0.1942 0.3252 0.0789 0.741(9) Uiso R . P 2 2 .
H1342 H 0.0344 0.2225 0.3184 0.0792 0.741(9) Uiso R . P 2 2 .
H1352 H 0.1077 0.3403 0.3498 0.0910 0.741(9) Uiso R . P 2 2 .
H1353 H 0.1568 0.3008 0.4655 0.0909 0.741(9) Uiso R . P 2 2 .
H1351 H 0.0577 0.3200 0.4757 0.0909 0.741(9) Uiso R . P 2 2 .
H421 H 0.5747 0.5368 0.8541 0.0307 1.0000 Uiso R . . . . .
H422 H 0.5664 0.4340 0.8675 0.0301 1.0000 Uiso R . . . . .
H431 H 0.6796 0.5421 1.0031 0.0390 1.0000 Uiso R . . . . .
H432 H 0.6592 0.4466 1.0562 0.0390 1.0000 Uiso R . . . . .
H441 H 0.7876 0.4544 0.9334 0.0441 1.0000 Uiso R . . . . .
H442 H 0.7306 0.4765 0.8089 0.0444 1.0000 Uiso R . . . . .
H452 H 0.7698 0.3353 0.8161 0.0706 1.0000 Uiso R . . . . .
H453 H 0.7235 0.3221 0.9510 0.0688 1.0000 Uiso R . . . . .
H451 H 0.6684 0.3404 0.8267 0.0688 1.0000 Uiso R . . . . .
H12 H 0.0146 0.0819 0.8912 0.1032 1.0000 Uiso R . . . . .
H21 H 0.4942 0.4081 0.6111 0.0972 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          6.5(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 . C11 . 1.421(2) yes
O1 . H12 . 0.862 no
C11 . C12 . 1.519(3) yes
C11 . C16 . 1.517(2) yes
C11 . C17 . 1.534(2) yes
C12 . C13 . 1.527(3) yes
C12 . H121 . 0.954 no
C12 . H122 . 0.968 no
C13 . C14 . 1.501(3) yes
C13 . C18 . 1.527(3) yes
C13 . H131 . 0.976 no
C14 . C15 . 1.512(3) yes
C14 . H142 . 0.995 no
C14 . H141 . 0.957 no
C15 . C16 . 1.521(2) yes
C15 . C19 . 1.520(2) yes
C15 . H151 . 0.977 no
C16 . H161 . 0.954 no
C16 . H162 . 0.993 no
C17 . C20 . 1.536(2) yes
C17 . H171 . 0.970 no
C17 . H172 . 0.969 no
C18 . C20 . 1.509(3) yes
C18 . H182 . 0.972 no
C18 . H181 . 0.976 no
C19 . C20 . 1.509(2) yes
C19 . H192 . 0.989 no
C19 . H191 . 0.999 no
C20 . H201 . 0.985 no
O2 . C21 . 1.429(3) yes
O2 . H21 . 0.874 no
C21 . C22 . 1.526(3) yes
C21 . C26 . 1.526(3) yes
C21 . C27 . 1.525(3) yes
C22 . C23 . 1.541(3) yes
C22 . H221 . 0.992 no
C22 . H222 . 0.985 no
C23 . C24 . 1.506(3) yes
C23 . C28 . 1.511(3) yes
C23 . H231 . 0.986 no
C24 . C25 . 1.531(3) yes
C24 . H241 . 0.994 no
C24 . H242 . 0.977 no
C25 . C26 . 1.523(3) yes
C25 . C29 . 1.506(3) yes
C25 . H251 . 0.965 no
C26 . H262 . 0.979 no
C26 . H261 . 0.961 no
C27 . C30 . 1.522(3) yes
C27 . H271 . 0.991 no
C27 . H272 . 0.986 no
C28 . C30 . 1.521(3) yes
C28 . H281 . 0.999 no
C28 . H282 . 0.982 no
C29 . C30 . 1.516(3) yes
C29 . H291 . 0.970 no
C29 . H292 . 0.993 no
C30 . H301 . 1.003 no
O102 . C121 . 1.425(5) yes
O102 . H21 . 0.932 no
C121 . C122 . 1.521(4) yes
C121 . C126 . 1.529(4) yes
C121 . C127 . 1.521(4) yes
C122 . C123 . 1.534(4) yes
C122 . H1221 . 0.979 no
C122 . H1222 . 0.969 no
C123 . C124 . 1.516(4) yes
C123 . C128 . 1.508(4) yes
C123 . H1231 . 0.982 no
C124 . C125 . 1.512(4) yes
C124 . H1241 . 0.969 no
C124 . H1242 . 0.971 no
C125 . C126 . 1.527(4) yes
C125 . C129 . 1.511(4) yes
C125 . H1251 . 0.979 no
C126 . H1262 . 0.971 no
C126 . H1261 . 0.968 no
C127 . C130 . 1.529(4) yes
C127 . H1272 . 0.963 no
C127 . H1271 . 0.971 no
C128 . C130 . 1.514(4) yes
C128 . H1282 . 0.971 no
C128 . H1281 . 0.966 no
C129 . C130 . 1.513(4) yes
C129 . H1292 . 0.967 no
C129 . H1291 . 0.969 no
C130 . H1301 . 0.987 no
N31 . C32 2_556 1.5122(19) yes
N31 . C32 3_555 1.5122(19) yes
N31 . C32 4_556 1.5122(19) yes
N31 . C32 . 1.5122(19) yes
N31 . C132 2_556 1.5122(19) yes
N31 . C132 3_555 1.5122(19) yes
N31 . C132 4_556 1.5122(19) yes
N31 . C132 . 1.5122(19) yes
C32 . C33 . 1.538(9) yes
C32 . H322 . 0.962 no
C32 . H321 . 0.967 no
C33 . C34 . 1.493(9) yes
C33 . H332 . 0.977 no
C33 . H331 . 0.968 no
C34 . C35 . 1.442(9) yes
C34 . H342 . 0.967 no
C34 . H341 . 0.969 no
C35 . H352 . 0.965 no
C35 . H351 . 0.964 no
C35 . H353 . 0.957 no
C132 . C133 . 1.498(4) yes
C132 . H1321 . 0.974 no
C132 . H1322 . 0.951 no
C133 . C134 . 1.508(5) yes
C133 . H1331 . 0.966 no
C133 . H1332 . 0.965 no
C134 . C135 . 1.453(6) yes
C134 . H1341 . 0.980 no
C134 . H1342 . 0.994 no
C135 . H1352 . 0.953 no
C135 . H1353 . 0.963 no
C135 . H1351 . 0.974 no
N41 . C42 2_567 1.523(2) yes
N41 . C42 4_657 1.523(2) yes
N41 . C42 3_665 1.523(2) yes
N41 . C42 . 1.523(2) yes
C42 . C43 . 1.525(3) yes
C42 . H421 . 0.981 no
C42 . H422 . 0.970 no
C43 . C44 . 1.520(4) yes
C43 . H431 . 0.981 no
C43 . H432 . 0.994 no
C44 . C45 . 1.505(4) yes
C44 . H441 . 0.981 no
C44 . H442 . 0.988 no
C45 . H452 . 0.963 no
C45 . H453 . 0.975 no
C45 . H451 . 0.981 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C11 . O1 . H12 . 118.3 no
O1 . C11 . C12 . 109.96(5) yes
O1 . C11 . C16 . 109.88(5) yes
C12 . C11 . C16 . 108.99(5) yes
O1 . C11 . C17 . 110.41(5) yes
C12 . C11 . C17 . 108.81(5) yes
C16 . C11 . C17 . 108.75(5) yes
C11 . C12 . C13 . 110.12(5) yes
C11 . C12 . H121 . 108.6 no
C13 . C12 . H121 . 111.6 no
C11 . C12 . H122 . 106.5 no
C13 . C12 . H122 . 108.2 no
H121 . C12 . H122 . 111.7 no
C12 . C13 . C14 . 109.44(5) yes
C12 . C13 . C18 . 108.74(5) yes
C14 . C13 . C18 . 109.90(5) yes
C12 . C13 . H131 . 107.9 no
C14 . C13 . H131 . 109.0 no
C18 . C13 . H131 . 111.9 no
C13 . C14 . C15 . 109.91(5) yes
C13 . C14 . H142 . 109.1 no
C15 . C14 . H142 . 110.3 no
C13 . C14 . H141 . 109.9 no
C15 . C14 . H141 . 108.2 no
H142 . C14 . H141 . 109.6 no
C14 . C15 . C16 . 108.73(5) yes
C14 . C15 . C19 . 109.96(5) yes
C16 . C15 . C19 . 109.52(5) yes
C14 . C15 . H151 . 109.1 no
C16 . C15 . H151 . 109.5 no
C19 . C15 . H151 . 110.0 no
C15 . C16 . C11 . 110.20(5) yes
C15 . C16 . H161 . 108.5 no
C11 . C16 . H161 . 107.8 no
C15 . C16 . H162 . 111.1 no
C11 . C16 . H162 . 109.3 no
H161 . C16 . H162 . 109.8 no
C11 . C17 . C20 . 109.85(5) yes
C11 . C17 . H171 . 109.2 no
C20 . C17 . H171 . 107.8 no
C11 . C17 . H172 . 112.3 no
C20 . C17 . H172 . 107.3 no
H171 . C17 . H172 . 110.3 no
C13 . C18 . C20 . 109.79(5) yes
C13 . C18 . H182 . 110.6 no
C20 . C18 . H182 . 110.1 no
C13 . C18 . H181 . 106.7 no
C20 . C18 . H181 . 109.3 no
H182 . C18 . H181 . 110.2 no
C15 . C19 . C20 . 109.83(5) yes
C15 . C19 . H192 . 108.3 no
C20 . C19 . H192 . 108.0 no
C15 . C19 . H191 . 109.6 no
C20 . C19 . H191 . 108.8 no
H192 . C19 . H191 . 112.2 no
C17 . C20 . C18 . 109.41(5) yes
C17 . C20 . C19 . 108.67(5) yes
C18 . C20 . C19 . 109.83(5) yes
C17 . C20 . H201 . 111.4 no
C18 . C20 . H201 . 108.7 no
C19 . C20 . H201 . 108.9 no
C21 . O2 . H21 . 104.8 no
O2 . C21 . C22 . 110.22(5) yes
O2 . C21 . C26 . 109.95(5) yes
C22 . C21 . C26 . 108.83(5) yes
O2 . C21 . C27 . 110.10(5) yes
C22 . C21 . C27 . 108.80(5) yes
C26 . C21 . C27 . 108.90(5) yes
C21 . C22 . C23 . 109.91(5) yes
C21 . C22 . H221 . 109.8 no
C23 . C22 . H221 . 109.5 no
C21 . C22 . H222 . 109.0 no
C23 . C22 . H222 . 109.2 no
H221 . C22 . H222 . 109.4 no
C22 . C23 . C24 . 109.43(6) yes
C22 . C23 . C28 . 108.70(6) yes
C24 . C23 . C28 . 109.86(6) yes
C22 . C23 . H231 . 109.5 no
C24 . C23 . H231 . 109.3 no
C28 . C23 . H231 . 110.1 no
C23 . C24 . C25 . 109.83(5) yes
C23 . C24 . H241 . 108.2 no
C25 . C24 . H241 . 107.7 no
C23 . C24 . H242 . 109.3 no
C25 . C24 . H242 . 111.2 no
H241 . C24 . H242 . 110.6 no
C24 . C25 . C26 . 108.70(6) yes
C24 . C25 . C29 . 109.90(6) yes
C26 . C25 . C29 . 109.46(6) yes
C24 . C25 . H251 . 110.9 no
C26 . C25 . H251 . 108.2 no
C29 . C25 . H251 . 109.7 no
C21 . C26 . C25 . 110.12(5) yes
C21 . C26 . H262 . 109.2 no
C25 . C26 . H262 . 111.6 no
C21 . C26 . H261 . 104.1 no
C25 . C26 . H261 . 108.2 no
H262 . C26 . H261 . 113.4 no
C21 . C27 . C30 . 110.11(5) yes
C21 . C27 . H271 . 109.7 no
C30 . C27 . H271 . 105.2 no
C21 . C27 . H272 . 110.2 no
C30 . C27 . H272 . 110.2 no
H271 . C27 . H272 . 111.4 no
C23 . C28 . C30 . 109.86(5) yes
C23 . C28 . H281 . 109.6 no
C30 . C28 . H281 . 109.6 no
C23 . C28 . H282 . 109.4 no
C30 . C28 . H282 . 108.2 no
H281 . C28 . H282 . 110.1 no
C25 . C29 . C30 . 109.87(5) yes
C25 . C29 . H291 . 108.1 no
C30 . C29 . H291 . 111.3 no
C25 . C29 . H292 . 111.1 no
C30 . C29 . H292 . 107.2 no
H291 . C29 . H292 . 109.2 no
C27 . C30 . C28 . 109.51(6) yes
C27 . C30 . C29 . 108.71(6) yes
C28 . C30 . C29 . 109.93(6) yes
C27 . C30 . H301 . 108.5 no
C28 . C30 . H301 . 109.1 no
C29 . C30 . H301 . 111.1 no
C121 . O102 . H21 . 104.3 no
O102 . C121 . C122 . 110.13(5) yes
O102 . C121 . C126 . 110.08(5) yes
C122 . C121 . C126 . 108.83(5) yes
O102 . C121 . C127 . 110.07(5) yes
C122 . C121 . C127 . 108.84(5) yes
C126 . C121 . C127 . 108.85(5) yes
C121 . C122 . C123 . 110.01(6) yes
C121 . C122 . H1221 . 110.7 no
C123 . C122 . H1221 . 110.0 no
C121 . C122 . H1222 . 108.2 no
C123 . C122 . H1222 . 108.3 no
H1221 . C122 . H1222 . 109.5 no
C122 . C123 . C124 . 109.47(6) yes
C122 . C123 . C128 . 108.69(6) yes
C124 . C123 . C128 . 109.88(6) yes
C122 . C123 . H1231 . 109.7 no
C124 . C123 . H1231 . 108.9 no
C128 . C123 . H1231 . 110.2 no
C123 . C124 . C125 . 109.84(6) yes
C123 . C124 . H1241 . 109.6 no
C125 . C124 . H1241 . 108.6 no
C123 . C124 . H1242 . 109.4 no
C125 . C124 . H1242 . 109.5 no
H1241 . C124 . H1242 . 109.8 no
C124 . C125 . C126 . 108.70(6) yes
C124 . C125 . C129 . 109.91(6) yes
C126 . C125 . C129 . 109.46(6) yes
C124 . C125 . H1251 . 109.6 no
C126 . C125 . H1251 . 110.2 no
C129 . C125 . H1251 . 108.9 no
C121 . C126 . C125 . 110.06(6) yes
C121 . C126 . H1262 . 109.3 no
C125 . C126 . H1262 . 110.8 no
C121 . C126 . H1261 . 108.3 no
C125 . C126 . H1261 . 108.4 no
H1262 . C126 . H1261 . 109.9 no
C121 . C127 . C130 . 110.06(6) yes
C121 . C127 . H1272 . 109.7 no
C130 . C127 . H1272 . 109.9 no
C121 . C127 . H1271 . 108.8 no
C130 . C127 . H1271 . 108.7 no
H1272 . C127 . H1271 . 109.7 no
C123 . C128 . C130 . 109.85(6) yes
C123 . C128 . H1282 . 108.5 no
C130 . C128 . H1282 . 108.8 no
C123 . C128 . H1281 . 110.6 no
C130 . C128 . H1281 . 109.6 no
H1282 . C128 . H1281 . 109.4 no
C125 . C129 . C130 . 109.86(6) yes
C125 . C129 . H1292 . 109.9 no
C130 . C129 . H1292 . 109.7 no
C125 . C129 . H1291 . 108.9 no
C130 . C129 . H1291 . 109.4 no
H1292 . C129 . H1291 . 109.1 no
C127 . C130 . C128 . 109.49(6) yes
C127 . C130 . C129 . 108.72(6) yes
C128 . C130 . C129 . 109.90(6) yes
C127 . C130 . H1301 . 109.4 no
C128 . C130 . H1301 . 109.3 no
C129 . C130 . H1301 . 110.1 no
C32 2_556 N31 . C32 3_555 111.83(2) yes
C32 2_556 N31 . C32 4_556 104.85(4) yes
C32 3_555 N31 . C32 4_556 111.83(2) yes
C32 2_556 N31 . C32 . 111.83(2) yes
C32 3_555 N31 . C32 . 104.85(4) yes
C32 4_556 N31 . C32 . 111.83(2) yes
C132 2_556 N31 . C132 3_555 111.83(2) yes
C132 2_556 N31 . C132 4_556 104.85(4) yes
C132 3_555 N31 . C132 4_556 111.83(2) yes
C132 2_556 N31 . C132 . 111.83(2) yes
C132 3_555 N31 . C132 . 104.85(4) yes
C132 4_556 N31 . C132 . 111.83(2) yes
N31 . C32 . C33 . 116.07(10) yes
N31 . C32 . H322 . 106.4 no
C33 . C32 . H322 . 105.4 no
N31 . C32 . H321 . 108.5 no
C33 . C32 . H321 . 110.7 no
H322 . C32 . H321 . 109.4 no
C32 . C33 . C34 . 109.42(10) yes
C32 . C33 . H332 . 107.7 no
C34 . C33 . H332 . 108.2 no
C32 . C33 . H331 . 111.4 no
C34 . C33 . H331 . 110.4 no
H332 . C33 . H331 . 109.6 no
C33 . C34 . C35 . 115.45(10) yes
C33 . C34 . H342 . 106.7 no
C35 . C34 . H342 . 108.6 no
C33 . C34 . H341 . 108.3 no
C35 . C34 . H341 . 108.7 no
H342 . C34 . H341 . 108.8 no
C34 . C35 . H352 . 109.4 no
C34 . C35 . H351 . 108.8 no
H352 . C35 . H351 . 109.1 no
C34 . C35 . H353 . 111.4 no
H352 . C35 . H353 . 109.3 no
H351 . C35 . H353 . 108.9 no
N31 . C132 . C133 . 116.25(8) yes
N31 . C132 . H1321 . 106.3 no
C133 . C132 . H1321 . 110.3 no
N31 . C132 . H1322 . 106.2 no
C133 . C132 . H1322 . 107.7 no
H1321 . C132 . H1322 . 110.1 no
C132 . C133 . C134 . 109.33(9) yes
C132 . C133 . H1331 . 113.0 no
C134 . C133 . H1331 . 107.8 no
C132 . C133 . H1332 . 107.5 no
C134 . C133 . H1332 . 109.5 no
H1331 . C133 . H1332 . 109.7 no
C133 . C134 . C135 . 115.46(10) yes
C133 . C134 . H1341 . 111.3 no
C135 . C134 . H1341 . 109.2 no
C133 . C134 . H1342 . 105.4 no
C135 . C134 . H1342 . 104.1 no
H1341 . C134 . H1342 . 111.0 no
C134 . C135 . H1352 . 110.7 no
C134 . C135 . H1353 . 109.0 no
H1352 . C135 . H1353 . 109.4 no
C134 . C135 . H1351 . 109.5 no
H1352 . C135 . H1351 . 108.9 no
H1353 . C135 . H1351 . 109.3 no
C42 2_567 N41 . C42 4_657 105.19(18) yes
C42 2_567 N41 . C42 3_665 111.65(9) yes
C42 4_657 N41 . C42 3_665 111.65(9) yes
C42 2_567 N41 . C42 . 111.65(9) yes
C42 4_657 N41 . C42 . 111.65(9) yes
C42 3_665 N41 . C42 . 105.19(18) yes
N41 . C42 . C43 . 114.64(17) yes
N41 . C42 . H421 . 104.7 no
C43 . C42 . H421 . 110.0 no
N41 . C42 . H422 . 106.0 no
C43 . C42 . H422 . 109.4 no
H421 . C42 . H422 . 111.9 no
C42 . C43 . C44 . 111.1(2) yes
C42 . C43 . H431 . 108.4 no
C44 . C43 . H431 . 108.3 no
C42 . C43 . H432 . 110.3 no
C44 . C43 . H432 . 108.2 no
H431 . C43 . H432 . 110.4 no
C43 . C44 . C45 . 113.5(2) yes
C43 . C44 . H441 . 108.6 no
C45 . C44 . H441 . 105.3 no
C43 . C44 . H442 . 110.4 no
C45 . C44 . H442 . 108.4 no
H441 . C44 . H442 . 110.5 no
C44 . C45 . H452 . 107.1 no
C44 . C45 . H453 . 109.8 no
H452 . C45 . H453 . 111.8 no
C44 . C45 . H451 . 109.7 no
H452 . C45 . H451 . 109.7 no
H453 . C45 . H451 . 108.8 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C125 . H261 . O2 . 130.0 1.025 2.584 3.336(6) yes
C125 . H1251 . C135 4_656 123.47 0.979 2.401 3.053(6) yes
C32 . H322 . O1 4_556 158.27 0.962 2.594 3.506(6) yes
C132 . H322 . O1 4_556 158.27 0.962 2.594 3.506(6) yes
C35 . H351 . C28 . 123.5 0.964 2.494 3.131(6) yes
C32 . H1321 . O1 2_556 157.34 0.974 2.433 3.353(6) yes
C132 . H1321 . O1 2_556 157.34 0.974 2.433 3.353(6) yes
C135 . H1352 . C125 2_566 128.90 0.953 2.363 3.053(6) yes
C42 . H421 . O102 3_665 157.90 0.981 2.360 3.290(6) yes
C42 . H422 . O2 . 144.63 0.970 2.553 3.391(6) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 26/04/13 at 17:05:52
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
REM EQUIV PART(1001,OCC) PART(1002,OCC) 
REM WEIGHT -1 PART(1002,OCC) 
EQUIV PART(2001,OCC) PART(2002,OCC) 
WEIGHT -1 PART(2002,OCC) 
RIDE C(32,U'S) C(132,U'S) 
RIDE O   (   1,X'S) H   (  12,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 142,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) 
RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 192,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE O   (   2,X'S) H   (  21,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 262,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) H   (1222,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) H   (1242,X'S) 
RIDE C   ( 125,X'S) H   (1251,X'S) 
RIDE C   ( 126,X'S) H   (1262,X'S) H   (1261,X'S) 
RIDE C   ( 127,X'S) H   (1272,X'S) H   (1271,X'S) 
RIDE C   ( 128,X'S) H   (1282,X'S) H   (1281,X'S) 
RIDE C   ( 129,X'S) H   (1292,X'S) H   (1291,X'S) 
RIDE C   ( 130,X'S) H   (1301,X'S) 
RIDE C   (  32,X'S) H   ( 322,X'S) H   ( 321,X'S) 
CONT C   ( 132,X'S) H   (1321,X'S) H   (1322,X'S) 
RIDE C   (  33,X'S) H   ( 332,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 342,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) H   ( 353,X'S) 
RIDE C   ( 133,X'S) H   (1331,X'S) H   (1332,X'S) 
RIDE C   ( 134,X'S) H   (1341,X'S) H   (1342,X'S) 
RIDE C   ( 135,X'S) H   (1352,X'S) H   (1353,X'S) H   (1351,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 452,X'S) H   ( 453,X'S) H   ( 451,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 26/04/13 at 17:05:52
#
#LIST     16                                                                    
SAME  N(31)  C(32)  C(33)  C(34)  C(35)  AND 
CONT  N(31)  C(132)  C(133)  C(134)  C(135) 
SIMU  0.01   N(31)  C(32)  C(33)  C(34)  C(35)  AND 
CONT  N(31)  C(132)  C(133)  C(134)  C(135) 
DELU  0.01   N(31)  C(32)  C(33)  C(34)  C(35)  AND 
CONT  N(31)  C(132)  C(133)  C(134)  C(135) 
REM CONT  N(41)  C(42)  C(43)  C(44)  C(45) 
SAME  O(1)  C(11)  C(12)  C(16)  C(17) 
CONT  C(13)  C(14)  C(15)  C(19)  C(20)  C(18)  AND 
CONT  O(1)  C(11)  C(16)  C(17)  C(12) 
CONT  C(15)  C(19)  C(20)  C(18)  C(13)  C(14)  AND 
CONT  O(1)  C(11)  C(17)  C(12)  C(16) 
CONT  C(20)  C(18)  C(13)  C(14)  C(15)  C(19)  AND 
CONT  O(2)  C(21)  C(22)  C(26)  C(27) 
CONT  C(23)  C(24)  C(25)  C(29)  C(30)  C(28)  AND 
CONT  O(2)  C(21)  C(26)  C(27)  C(22) 
CONT  C(25)  C(29)  C(30)  C(28)  C(23)  C(24)  AND 
CONT  O(2)  C(21)  C(27)  C(22)  C(26) 
CONT  C(30)  C(28)  C(23)  C(24)  C(25)  C(29)  AND 
CONT  O(102)  C(121)  C(122)  C(126)  C(127) 
CONT  C(123)  C(124)  C(125)  C(129)  C(130)  C(128)  AND 
CONT  O(102)  C(121)  C(126)  C(127)  C(122) 
CONT  C(125)  C(129)  C(130)  C(128)  C(123)  C(124)  AND 
CONT  O(102)  C(121)  C(127)  C(122)  C(126) 
CONT  C(130)  C(128)  C(123)  C(124)  C(125)  C(129) 
SIMU  0.01  O(1)  C(11)  C(12)  C(16)  C(17) 
CONT  C(13)  C(14)  C(15)  C(19)  C(20)  C(18)  AND 
CONT  O(1)  C(11)  C(16)  C(17)  C(12) 
CONT  C(15)  C(19)  C(20)  C(18)  C(13)  C(14)  AND 
CONT  O(1)  C(11)  C(17)  C(12)  C(16) 
CONT  C(20)  C(18)  C(13)  C(14)  C(15)  C(19)  AND 
CONT  O(2)  C(21)  C(22)  C(26)  C(27) 
CONT  C(23)  C(24)  C(25)  C(29)  C(30)  C(28)  AND 
CONT  O(2)  C(21)  C(26)  C(27)  C(22) 
CONT  C(25)  C(29)  C(30)  C(28)  C(23)  C(24)  AND 
CONT  O(2)  C(21)  C(27)  C(22)  C(26) 
CONT  C(30)  C(28)  C(23)  C(24)  C(25)  C(29)  AND 
CONT  O(102)  C(121)  C(122)  C(126)  C(127) 
CONT  C(123)  C(124)  C(125)  C(129)  C(130)  C(128)  AND 
CONT  O(102)  C(121)  C(126)  C(127)  C(122) 
CONT  C(125)  C(129)  C(130)  C(128)  C(123)  C(124)  AND 
CONT  O(102)  C(121)  C(127)  C(122)  C(126) 
CONT  C(130)  C(128)  C(123)  C(124)  C(125)  C(129) 
DELU  0.01  O(1)  C(11)  C(12)  C(16)  C(17) 
CONT  C(13)  C(14)  C(15)  C(19)  C(20)  C(18)  AND 
CONT  O(1)  C(11)  C(16)  C(17)  C(12) 
CONT  C(15)  C(19)  C(20)  C(18)  C(13)  C(14)  AND 
CONT  O(1)  C(11)  C(17)  C(12)  C(16) 
CONT  C(20)  C(18)  C(13)  C(14)  C(15)  C(19)  AND 
CONT  O(2)  C(21)  C(22)  C(26)  C(27) 
CONT  C(23)  C(24)  C(25)  C(29)  C(30)  C(28)  AND 
CONT  O(2)  C(21)  C(26)  C(27)  C(22) 
CONT  C(25)  C(29)  C(30)  C(28)  C(23)  C(24)  AND 
CONT  O(2)  C(21)  C(27)  C(22)  C(26) 
CONT  C(30)  C(28)  C(23)  C(24)  C(25)  C(29)  AND 
CONT  O(102)  C(121)  C(122)  C(126)  C(127) 
CONT  C(123)  C(124)  C(125)  C(129)  C(130)  C(128)  AND 
CONT  O(102)  C(121)  C(126)  C(127)  C(122) 
CONT  C(125)  C(129)  C(130)  C(128)  C(123)  C(124)  AND 
CONT  O(102)  C(121)  C(127)  C(122)  C(126) 
CONT  C(130)  C(128)  C(123)  C(124)  C(125)  C(129) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 1401766'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             13-04-24
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 043gwp12
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   9.9446(3)
_cell_length_b                   18.0891(7)
_cell_length_c                   15.7361(6)
_cell_angle_alpha                90
_cell_angle_beta                 103.523(4)
_cell_angle_gamma                90
_cell_volume                     2752.27(18)

_refine_special_details          
;
On first examination, it was found that there was solvent present
which was identified as dichloromethane (used in recrystallisation).
On refinement, the ADPs became prolate indicating disorder.
A two site model was used with restraints applied to maintain
sensible geometries and displacement parameters for the individual
components.  In order to ensure convergence, the ADPs of one
pair of chlorine atoms that were in close proximity were
constrained to the same shape.
;

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C22 H46 Cl2 F1 N1 O4 
# Dc =      1.15 Fooo =   1056.00 Mu =     23.80 M =    478.51
# Found Formula = C22 H50 Cl2 F1 N1 O4 
# Dc =      1.16 FOOO =   1056.00 Mu =     23.80 M =    482.55

_chemical_formula_sum            'C22 H50 Cl2 F1 N1 O4'
_chemical_formula_moiety         'C16 H36 N, C5 H12 O4, C H2 Cl2, F'
_chemical_compound_source        .
_chemical_formula_weight         482.55


_cell_measurement_reflns_used    6459
_cell_measurement_theta_min      3
_cell_measurement_theta_max      75
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.040
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.180

_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1056.000
_exptl_absorpt_coefficient_mu    2.380

# Sheldrick geometric approximatio 0.70 0.91 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_T_max  0.91
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            19286
_reflns_number_total             5597
_diffrn_reflns_av_R_equivalents  0.047
# Number of reflections with Friedels Law is 5597 
# Theoretical number of reflections is about 9141 


_diffrn_reflns_theta_min         3.784
_diffrn_reflns_theta_max         75.247
_diffrn_measured_fraction_theta_max 0.985

_diffrn_reflns_theta_full        72.237
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              19

_oxford_diffrn_Wilson_B_factor   4.37
_oxford_diffrn_Wilson_scale      0.05

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.47
_refine_diff_density_max         0.60


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         4548
_refine_ls_number_restraints     32
_refine_ls_number_parameters     293
_oxford_refine_ls_R_factor_ref   0.0693
_refine_ls_wR_factor_ref         0.1507
_refine_ls_goodness_of_fit_ref   0.9859
_refine_ls_shift/su_max          0.0002707
_refine_ls_shift/su_mean         0.0000298


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4548
_refine_ls_R_factor_all          0.0693
_refine_ls_wR_factor_all         0.1507

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3625
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_gt          0.1408

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.07P)² + 2.18P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C15 C 0.3401(2) 0.22442(14) 0.51870(16) 0.0372 1.0000 Uani . . . . . .
C16 C 0.4999(2) 0.17925(14) 0.65279(16) 0.0367 1.0000 Uani . . . . . .
C17 C 0.4146(3) 0.31148(15) 0.64459(17) 0.0402 1.0000 Uani . . . . . .
C18 C 0.5833(2) 0.27377(14) 0.56003(16) 0.0359 1.0000 Uani . . . . . .
C19 C 0.4598(2) 0.24753(13) 0.59429(14) 0.0303 1.0000 Uani . . . . . .
N21 N 0.94353(17) 0.29272(10) 0.83012(11) 0.0255 1.0000 Uani . . . . . .
C22 C 1.0718(2) 0.34140(12) 0.84625(15) 0.0295 1.0000 Uani . . . . . .
C23 C 1.0807(2) 0.39672(13) 0.77594(16) 0.0356 1.0000 Uani . . . . . .
C24 C 1.2065(3) 0.44576(16) 0.8077(2) 0.0506 1.0000 Uani . . . . . .
C25 C 1.2220(4) 0.5026(2) 0.7403(2) 0.0745 1.0000 Uani . . . . . .
C26 C 0.9264(2) 0.24858(12) 0.74660(14) 0.0290 1.0000 Uani . . . . . .
C27 C 1.0374(3) 0.19318(14) 0.74197(16) 0.0378 1.0000 Uani . . . . . .
C28 C 0.9987(4) 0.15681(19) 0.6518(2) 0.0659 1.0000 Uani . . . . . .
C29 C 1.0885(4) 0.09432(18) 0.6382(2) 0.0616 1.0000 Uani . . . . . .
C30 C 0.8117(2) 0.33796(13) 0.81902(15) 0.0298 1.0000 Uani . . . . . .
C31 C 0.8003(3) 0.38832(14) 0.89383(16) 0.0362 1.0000 Uani . . . . . .
C32 C 0.6616(3) 0.42858(16) 0.87052(19) 0.0489 1.0000 Uani . . . . . .
C33 C 0.6378(4) 0.47591(19) 0.9446(2) 0.0678 1.0000 Uani . . . . . .
C34 C 0.9635(2) 0.24205(12) 0.90935(14) 0.0281 1.0000 Uani . . . . . .
C35 C 0.8533(2) 0.18352(14) 0.90641(16) 0.0365 1.0000 Uani . . . . . .
C36 C 0.8837(3) 0.14019(16) 0.99208(17) 0.0461 1.0000 Uani . . . . . .
C37 C 1.0218(3) 0.10234(18) 1.0142(2) 0.0593 1.0000 Uani . . . . . .
C41 C 0.6347(7) 0.5624(5) 0.6058(7) 0.0863 0.644(12) Uani D . P 1 1 .
Cl42 Cl 0.4816(5) 0.5390(4) 0.6317(4) 0.1180 0.644(12) Uani D . P 1 1 .
Cl43 Cl 0.7433(8) 0.4874(4) 0.6317(6) 0.0653 0.356(12) Uani D . P 1 2 .
C51 C 0.6327(9) 0.5637(7) 0.6291(12) 0.0719 0.356(12) Uani D . P 1 2 .
Cl52 Cl 0.4749(7) 0.5180(5) 0.6017(6) 0.1078 0.356(12) Uani D . P 1 2 .
Cl53 Cl 0.7761(5) 0.5046(3) 0.6402(3) 0.0653 0.644(12) Uani D . P 1 1 .
F1 F 0.4633(2) 0.24550(12) 0.84601(10) 0.0689 1.0000 Uani . . . . . .
O11 O 0.30475(17) 0.27917(10) 0.45204(11) 0.0415 1.0000 Uani . . . . . .
O12 O 0.59920(17) 0.19404(10) 0.73180(11) 0.0424 1.0000 Uani . . . . . .
O13 O 0.3132(2) 0.29090(13) 0.69156(13) 0.0568 1.0000 Uani . . . . . .
O14 O 0.6277(2) 0.22220(12) 0.50429(13) 0.0523 1.0000 Uani . . . . . .
H121 H 0.5478 0.2076 0.7635 0.0643 1.0000 Uiso R . . . . .
H162 H 0.5372 0.1428 0.6190 0.0448 1.0000 Uiso R . . . . .
H161 H 0.4170 0.1576 0.6652 0.0437 1.0000 Uiso R . . . . .
H151 H 0.2573 0.2158 0.5395 0.0447 1.0000 Uiso R . . . . .
H152 H 0.3628 0.1780 0.4936 0.0452 1.0000 Uiso R . . . . .
H111 H 0.3539 0.2741 0.4172 0.0624 1.0000 Uiso R . . . . .
H181 H 0.6606 0.2824 0.6107 0.0426 1.0000 Uiso R . . . . .
H182 H 0.5587 0.3204 0.5301 0.0418 1.0000 Uiso R . . . . .
H141 H 0.5705 0.2305 0.4594 0.0774 1.0000 Uiso R . . . . .
H171 H 0.4953 0.3318 0.6850 0.0476 1.0000 Uiso R . . . . .
H172 H 0.3723 0.3497 0.6028 0.0477 1.0000 Uiso R . . . . .
H131 H 0.3499 0.2718 0.7389 0.0852 1.0000 Uiso R . . . . .
H261 H 0.8396 0.2237 0.7379 0.0343 1.0000 Uiso R . . . . .
H262 H 0.9200 0.2845 0.6996 0.0350 1.0000 Uiso R . . . . .
H272 H 1.0407 0.1543 0.7856 0.0449 1.0000 Uiso R . . . . .
H271 H 1.1281 0.2166 0.7518 0.0456 1.0000 Uiso R . . . . .
H281 H 0.9973 0.1936 0.6073 0.0790 1.0000 Uiso R . . . . .
H282 H 0.9093 0.1307 0.6422 0.0794 1.0000 Uiso R . . . . .
H291 H 1.1859 0.1107 0.6484 0.0922 1.0000 Uiso R . . . . .
H292 H 1.0619 0.0736 0.5785 0.0922 1.0000 Uiso R . . . . .
H293 H 1.0848 0.0528 0.6794 0.0922 1.0000 Uiso R . . . . .
H301 H 0.7374 0.3028 0.8106 0.0349 1.0000 Uiso R . . . . .
H302 H 0.8023 0.3657 0.7654 0.0360 1.0000 Uiso R . . . . .
H312 H 0.8743 0.4249 0.9053 0.0431 1.0000 Uiso R . . . . .
H311 H 0.8025 0.3586 0.9459 0.0435 1.0000 Uiso R . . . . .
H321 H 0.6571 0.4582 0.8191 0.0591 1.0000 Uiso R . . . . .
H322 H 0.5888 0.3915 0.8570 0.0587 1.0000 Uiso R . . . . .
H333 H 0.6396 0.4451 0.9951 0.1017 1.0000 Uiso R . . . . .
H331 H 0.7116 0.5127 0.9585 0.1011 1.0000 Uiso R . . . . .
H332 H 0.5493 0.5007 0.9287 0.1016 1.0000 Uiso R . . . . .
H222 H 1.1480 0.3076 0.8537 0.0349 1.0000 Uiso R . . . . .
H221 H 1.0756 0.3674 0.9017 0.0359 1.0000 Uiso R . . . . .
H231 H 0.9983 0.4263 0.7627 0.0435 1.0000 Uiso R . . . . .
H232 H 1.0881 0.3712 0.7226 0.0429 1.0000 Uiso R . . . . .
H241 H 1.2862 0.4151 0.8215 0.0615 1.0000 Uiso R . . . . .
H242 H 1.1975 0.4702 0.8610 0.0610 1.0000 Uiso R . . . . .
H253 H 1.2443 0.4768 0.6914 0.1121 1.0000 Uiso R . . . . .
H252 H 1.1356 0.5286 0.7200 0.1123 1.0000 Uiso R . . . . .
H251 H 1.2946 0.5367 0.7658 0.1118 1.0000 Uiso R . . . . .
H341 H 1.0521 0.2172 0.9147 0.0336 1.0000 Uiso R . . . . .
H342 H 0.9645 0.2735 0.9602 0.0348 1.0000 Uiso R . . . . .
H352 H 0.7640 0.2057 0.8993 0.0451 1.0000 Uiso R . . . . .
H351 H 0.8509 0.1498 0.8589 0.0437 1.0000 Uiso R . . . . .
H362 H 0.8132 0.1016 0.9899 0.0547 1.0000 Uiso R . . . . .
H361 H 0.8778 0.1743 1.0407 0.0562 1.0000 Uiso R . . . . .
H371 H 1.0353 0.0752 0.9637 0.0891 1.0000 Uiso R . . . . .
H373 H 1.0965 0.1389 1.0310 0.0894 1.0000 Uiso R . . . . .
H372 H 1.0253 0.0684 1.0628 0.0880 1.0000 Uiso R . . . . .
H411 H 0.6609 0.6085 0.6355 0.1037 0.644(12) Uiso R . P 1 1 .
H412 H 0.6204 0.5680 0.5442 0.1031 0.644(12) Uiso R . P 1 1 .
H511 H 0.6467 0.5889 0.6851 0.0869 0.356(12) Uiso R . P 1 2 .
H512 H 0.6419 0.5980 0.5831 0.0869 0.356(12) Uiso R . P 1 2 .

_refine_ls_extinction_coef       79.873
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          4.84(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C15 . C19 . 1.532(3) yes
C15 . O11 . 1.426(3) yes
C15 . H151 . 0.967 no
C15 . H152 . 0.977 no
C16 . C19 . 1.536(3) yes
C16 . O12 . 1.421(3) yes
C16 . H162 . 0.973 no
C16 . H161 . 0.973 no
C17 . C19 . 1.528(3) yes
C17 . O13 . 1.432(3) yes
C17 . H171 . 0.973 no
C17 . H172 . 0.978 no
C18 . C19 . 1.527(3) yes
C18 . O14 . 1.420(3) yes
C18 . H181 . 0.982 no
C18 . H182 . 0.968 no
N21 . C22 . 1.522(3) yes
N21 . C26 . 1.513(3) yes
N21 . C30 . 1.521(3) yes
N21 . C34 . 1.523(3) yes
C22 . C23 . 1.510(3) yes
C22 . H222 . 0.960 no
C22 . H221 . 0.984 no
C23 . C24 . 1.520(3) yes
C23 . H231 . 0.960 no
C23 . H232 . 0.976 no
C24 . C25 . 1.511(4) yes
C24 . H241 . 0.950 no
C24 . H242 . 0.970 no
C25 . H253 . 0.968 no
C25 . H252 . 0.966 no
C25 . H251 . 0.963 no
C26 . C27 . 1.505(3) yes
C26 . H261 . 0.955 no
C26 . H262 . 0.975 no
C27 . C28 . 1.530(4) yes
C27 . H272 . 0.979 no
C27 . H271 . 0.976 no
C28 . C29 . 1.487(4) yes
C28 . H281 . 0.964 no
C28 . H282 . 0.986 no
C29 . H291 . 0.989 no
C29 . H292 . 0.987 no
C29 . H293 . 1.000 no
C30 . C31 . 1.514(3) yes
C30 . H301 . 0.960 no
C30 . H302 . 0.966 no
C31 . C32 . 1.526(3) yes
C31 . H312 . 0.975 no
C31 . H311 . 0.976 no
C32 . C33 . 1.508(4) yes
C32 . H321 . 0.963 no
C32 . H322 . 0.973 no
C33 . H333 . 0.968 no
C33 . H331 . 0.977 no
C33 . H332 . 0.967 no
C34 . C35 . 1.517(3) yes
C34 . H341 . 0.975 no
C34 . H342 . 0.980 no
C35 . C36 . 1.527(3) yes
C35 . H352 . 0.956 no
C35 . H351 . 0.961 no
C36 . C37 . 1.501(4) yes
C36 . H362 . 0.985 no
C36 . H361 . 0.996 no
C37 . H371 . 0.971 no
C37 . H373 . 0.984 no
C37 . H372 . 0.974 no
C41 . Cl42 . 1.718(7) yes
C41 . Cl53 . 1.734(9) yes
C41 . H411 . 0.962 no
C41 . H412 . 0.952 no
Cl43 . C51 . 1.760(16) yes
C51 . Cl52 . 1.736(9) yes
C51 . H511 . 0.972 no
C51 . H512 . 0.975 no
O11 . H111 . 0.820 no
O12 . H121 . 0.830 no
O13 . H131 . 0.824 no
O14 . H141 . 0.810 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C19 . C15 . O11 . 113.26(19) yes
C19 . C15 . H151 . 110.5 no
O11 . C15 . H151 . 106.1 no
C19 . C15 . H152 . 109.7 no
O11 . C15 . H152 . 109.9 no
H151 . C15 . H152 . 107.1 no
C19 . C16 . O12 . 113.75(19) yes
C19 . C16 . H162 . 107.2 no
O12 . C16 . H162 . 109.3 no
C19 . C16 . H161 . 109.3 no
O12 . C16 . H161 . 110.4 no
H162 . C16 . H161 . 106.6 no
C19 . C17 . O13 . 113.5(2) yes
C19 . C17 . H171 . 109.1 no
O13 . C17 . H171 . 109.6 no
C19 . C17 . H172 . 108.6 no
O13 . C17 . H172 . 106.7 no
H171 . C17 . H172 . 109.3 no
C19 . C18 . O14 . 113.9(2) yes
C19 . C18 . H181 . 107.7 no
O14 . C18 . H181 . 108.0 no
C19 . C18 . H182 . 108.1 no
O14 . C18 . H182 . 110.6 no
H181 . C18 . H182 . 108.4 no
C16 . C19 . C15 . 106.95(18) yes
C16 . C19 . C17 . 111.4(2) yes
C15 . C19 . C17 . 109.8(2) yes
C16 . C19 . C18 . 110.14(19) yes
C15 . C19 . C18 . 110.73(19) yes
C17 . C19 . C18 . 107.82(19) yes
C22 . N21 . C26 . 111.70(17) yes
C22 . N21 . C30 . 111.98(17) yes
C26 . N21 . C30 . 105.40(15) yes
C22 . N21 . C34 . 105.55(15) yes
C26 . N21 . C34 . 111.12(16) yes
C30 . N21 . C34 . 111.22(16) yes
N21 . C22 . C23 . 116.85(17) yes
N21 . C22 . H222 . 105.0 no
C23 . C22 . H222 . 109.4 no
N21 . C22 . H221 . 106.4 no
C23 . C22 . H221 . 109.6 no
H222 . C22 . H221 . 109.4 no
C22 . C23 . C24 . 109.3(2) yes
C22 . C23 . H231 . 109.6 no
C24 . C23 . H231 . 110.0 no
C22 . C23 . H232 . 110.2 no
C24 . C23 . H232 . 109.7 no
H231 . C23 . H232 . 108.0 no
C23 . C24 . C25 . 112.2(2) yes
C23 . C24 . H241 . 108.3 no
C25 . C24 . H241 . 109.9 no
C23 . C24 . H242 . 108.4 no
C25 . C24 . H242 . 110.0 no
H241 . C24 . H242 . 108.0 no
C24 . C25 . H253 . 108.1 no
C24 . C25 . H252 . 109.5 no
H253 . C25 . H252 . 108.9 no
C24 . C25 . H251 . 109.4 no
H253 . C25 . H251 . 110.6 no
H252 . C25 . H251 . 110.3 no
N21 . C26 . C27 . 117.31(18) yes
N21 . C26 . H261 . 106.7 no
C27 . C26 . H261 . 109.1 no
N21 . C26 . H262 . 106.3 no
C27 . C26 . H262 . 109.0 no
H261 . C26 . H262 . 108.0 no
C26 . C27 . C28 . 107.6(2) yes
C26 . C27 . H272 . 110.5 no
C28 . C27 . H272 . 107.6 no
C26 . C27 . H271 . 111.4 no
C28 . C27 . H271 . 110.9 no
H272 . C27 . H271 . 108.9 no
C27 . C28 . C29 . 115.5(3) yes
C27 . C28 . H281 . 109.5 no
C29 . C28 . H281 . 109.1 no
C27 . C28 . H282 . 111.7 no
C29 . C28 . H282 . 99.5 no
H281 . C28 . H282 . 111.2 no
C28 . C29 . H291 . 110.3 no
C28 . C29 . H292 . 112.9 no
H291 . C29 . H292 . 107.7 no
C28 . C29 . H293 . 111.3 no
H291 . C29 . H293 . 107.6 no
H292 . C29 . H293 . 106.8 no
N21 . C30 . C31 . 117.01(18) yes
N21 . C30 . H301 . 105.9 no
C31 . C30 . H301 . 108.1 no
N21 . C30 . H302 . 106.5 no
C31 . C30 . H302 . 110.9 no
H301 . C30 . H302 . 108.0 no
C30 . C31 . C32 . 109.2(2) yes
C30 . C31 . H312 . 111.2 no
C32 . C31 . H312 . 108.8 no
C30 . C31 . H311 . 109.4 no
C32 . C31 . H311 . 107.8 no
H312 . C31 . H311 . 110.5 no
C31 . C32 . C33 . 112.4(3) yes
C31 . C32 . H321 . 109.2 no
C33 . C32 . H321 . 110.4 no
C31 . C32 . H322 . 107.9 no
C33 . C32 . H322 . 108.6 no
H321 . C32 . H322 . 108.3 no
C32 . C33 . H333 . 109.4 no
C32 . C33 . H331 . 108.4 no
H333 . C33 . H331 . 109.9 no
C32 . C33 . H332 . 111.2 no
H333 . C33 . H332 . 108.6 no
H331 . C33 . H332 . 109.4 no
N21 . C34 . C35 . 116.12(17) yes
N21 . C34 . H341 . 106.9 no
C35 . C34 . H341 . 108.2 no
N21 . C34 . H342 . 107.1 no
C35 . C34 . H342 . 107.4 no
H341 . C34 . H342 . 111.1 no
C34 . C35 . C36 . 109.80(19) yes
C34 . C35 . H352 . 110.8 no
C36 . C35 . H352 . 107.8 no
C34 . C35 . H351 . 110.7 no
C36 . C35 . H351 . 109.0 no
H352 . C35 . H351 . 108.8 no
C35 . C36 . C37 . 114.9(2) yes
C35 . C36 . H362 . 109.9 no
C37 . C36 . H362 . 106.9 no
C35 . C36 . H361 . 109.0 no
C37 . C36 . H361 . 108.6 no
H362 . C36 . H361 . 107.3 no
C36 . C37 . H371 . 109.6 no
C36 . C37 . H373 . 110.4 no
H371 . C37 . H373 . 108.7 no
C36 . C37 . H372 . 109.4 no
H371 . C37 . H372 . 109.7 no
H373 . C37 . H372 . 109.0 no
Cl42 . C41 . Cl53 . 118.5(5) yes
Cl42 . C41 . H411 . 104.6 no
Cl53 . C41 . H411 . 105.3 no
Cl42 . C41 . H412 . 109.8 no
Cl53 . C41 . H412 . 107.4 no
H411 . C41 . H412 . 111.0 no
Cl43 . C51 . Cl52 . 99.0(8) yes
Cl43 . C51 . H511 . 113.0 no
Cl52 . C51 . H511 . 112.2 no
Cl43 . C51 . H512 . 110.5 no
Cl52 . C51 . H512 . 110.8 no
H511 . C51 . H512 . 110.9 no
C15 . O11 . H111 . 109.3 no
C16 . O12 . H121 . 100.5 no
C17 . O13 . H131 . 111.0 no
C18 . O14 . H141 . 99.2 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C26 . H261 . O12 . 163.33 0.955 2.430 3.356(5) yes
C30 . H301 . O12 . 152.66 0.960 2.549 3.431(5) yes
C31 . H311 . O14 3_555 136.13 0.976 2.598 3.370(5) yes
C22 . H222 . O11 3_655 147.36 0.960 2.482 3.330(5) yes
C34 . H341 . O11 3_655 149.96 0.975 2.444 3.324(5) yes
C51 . H411 . O11 2_666 141.5 0.856 2.522 3.236(5) yes
C41 . H512 . O11 2_666 165 0.749 2.379 3.109(5) yes
C51 . H512 . O11 2_666 146.3 0.975 2.379 3.236(5) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 24/04/13 at 10:09:08
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE CL(43,U'S) CL(53,U'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 162,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) 
RIDE C   (  22,X'S) H   ( 222,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 253,X'S) H   ( 252,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  27,X'S) H   ( 272,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 312,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 333,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 373,X'S) H   ( 372,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) 
RIDE O   (  11,X'S) H   ( 111,X'S) 
RIDE O   (  12,X'S) H   ( 121,X'S) 
RIDE O   (  13,X'S) H   ( 131,X'S) 
RIDE O   (  14,X'S) H   ( 141,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 24/04/13 at 10:09:08
#
#LIST     16                                                                    
SAME CL(52) C(51) CL(53) AND 
CONT CL(53) C(51) CL(52) AND 
CONT CL(42) C(41) CL(43) AND 
CONT CL(43) C(41) CL(42) 
DELU 0.01 CL(52) C(51) CL(53) AND 
CONT CL(53) C(51) CL(52) AND 
CONT CL(42) C(41) CL(43) AND 
CONT CL(43) C(41) CL(42) 
SIMU 0.01 CL(52) C(51) CL(53) AND 
CONT CL(53) C(51) CL(52) AND 
CONT CL(42) C(41) CL(43) AND 
CONT CL(43) C(41) CL(42) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
1 1 3 x .
0 4 0 x .
####################################################################### 
# 
# 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_2c
_database_code_depnum_ccdc_archive 'CCDC 1401767'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             13-03-18
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 063ggke01
_chemical_name_systematic        .
_chemical_melting_point          .

_cell_length_a                   9.9133(1)
_cell_length_b                   17.3454(3)
_cell_length_c                   18.3631(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3157.54(8)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n '
_symmetry_space_group_name_Hall  '-P 2n 2ab'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,-z+1/2
-x+1/2,-y+1/2,z+1/2
x+1/2,-y+1/2,-z
-x+1/2,y+1/2,z
-x,y,-z+1/2
x,-y,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C52 H120 F2 N2 O12 
# Dc =      2.11 Fooo =   1120.00 Mu =      1.53 M =    501.76
# Found Formula = C26 H60 F1 N1 O6 
# Dc =      1.06 FOOO =   1120.00 Mu =      0.76 M =    250.88

_chemical_formula_sum            'C26 H60 F1 N1 O6'
_chemical_formula_moiety         'C16 H36 N, 2(C5 H12 O3), F'
_chemical_compound_source        .
_chemical_formula_weight         501.76


_cell_measurement_reflns_used    4020
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.35

_exptl_crystal_density_diffrn    1.055
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1120
_exptl_absorpt_coefficient_mu    0.076

# Sheldrick geometric approximatio 0.98 0.99 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_T_max  0.99
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            46870
_reflns_number_total             3597
_diffrn_reflns_av_R_equivalents  0.020
# Number of reflections without Friedels Law is 6774 
# Number of reflections with Friedels Law is 3597 
# Theoretical number of reflections is about 3624 


_diffrn_reflns_theta_min         5.200
_diffrn_reflns_theta_max         27.492
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        26.942
_diffrn_measured_fraction_theta_full 0.992


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_reflns_limit_h_min              0
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              23

_oxford_diffrn_Wilson_B_factor   2.82
_oxford_diffrn_Wilson_scale      4.34

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.25
_refine_diff_density_max         0.34


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         3597
_refine_ls_number_restraints     0
_refine_ls_number_parameters     155
_oxford_refine_ls_R_factor_ref   0.0623
_refine_ls_wR_factor_ref         0.1057
_refine_ls_goodness_of_fit_ref   0.9619
_refine_ls_shift/su_max          0.0005402
_refine_ls_shift/su_mean         0.0000480


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3597
_refine_ls_R_factor_all          0.0623
_refine_ls_wR_factor_all         0.1057

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2751
_refine_ls_R_factor_gt           0.0431
_refine_ls_wR_factor_gt          0.0972

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 1.18P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
F1 F 0.5000 0.27953(8) 0.7500 0.0484 1.0000 Uani S T . . . .
O11 O 0.40012(9) 0.24409(6) 0.62274(5) 0.0429 1.0000 Uani . . . . . .
O12 O 0.65488(9) 0.36391(6) 0.66504(5) 0.0439 1.0000 Uani . . . . . .
O13 O 0.65601(9) 0.28057(7) 0.44334(5) 0.0482 1.0000 Uani . . . . . .
C14 C 0.51408(13) 0.25017(8) 0.57553(7) 0.0332 1.0000 Uani . . . . . .
C15 C 0.54159(12) 0.33180(8) 0.54877(6) 0.0308 1.0000 Uani . . . . . .
C16 C 0.55852(14) 0.38750(8) 0.61275(7) 0.0388 1.0000 Uani . . . . . .
C17 C 0.67155(13) 0.33030(9) 0.50427(7) 0.0397 1.0000 Uani . . . . . .
C18 C 0.42407(15) 0.36007(10) 0.50219(8) 0.0467 1.0000 Uani . . . . . .
N21 N 0.0000 0.27575(8) 0.7500 0.0241 1.0000 Uani S T . . . .
C22 C 0.01982(11) 0.32476(7) 0.81779(6) 0.0266 1.0000 Uani . . . . . .
C23 C -0.08660(12) 0.38576(7) 0.83215(6) 0.0301 1.0000 Uani . . . . . .
C24 C -0.05989(13) 0.42255(7) 0.90624(7) 0.0341 1.0000 Uani . . . . . .
C25 C -0.14602(16) 0.49324(8) 0.92037(8) 0.0440 1.0000 Uani . . . . . .
C26 C -0.12487(11) 0.22620(7) 0.76156(6) 0.0269 1.0000 Uani . . . . . .
C27 C -0.15489(12) 0.16644(7) 0.70371(7) 0.0323 1.0000 Uani . . . . . .
C28 C -0.27869(15) 0.12033(8) 0.72610(8) 0.0414 1.0000 Uani . . . . . .
C29 C -0.31618(18) 0.05819(9) 0.67198(9) 0.0546 1.0000 Uani . . . . . .
H111 H 0.4253 0.2553 0.6660 0.0641 1.0000 Uiso R . . . . .
H121 H 0.6118 0.3375 0.6967 0.0666 1.0000 Uiso R . . . . .
H131 H 0.7313 0.2742 0.4240 0.0718 1.0000 Uiso R . . . . .
H141 H 0.4945 0.2170 0.5324 0.0380 1.0000 Uiso R . . . . .
H142 H 0.5942 0.2301 0.6003 0.0408 1.0000 Uiso R . . . . .
H161 H 0.5907 0.4370 0.5930 0.0480 1.0000 Uiso R . . . . .
H162 H 0.4698 0.3945 0.6368 0.0465 1.0000 Uiso R . . . . .
H171 H 0.7453 0.3133 0.5354 0.0465 1.0000 Uiso R . . . . .
H172 H 0.6895 0.3825 0.4877 0.0488 1.0000 Uiso R . . . . .
H181 H 0.4369 0.4126 0.4860 0.0709 1.0000 Uiso R . . . . .
H182 H 0.3376 0.3570 0.5307 0.0683 1.0000 Uiso R . . . . .
H183 H 0.4180 0.3298 0.4580 0.0689 1.0000 Uiso R . . . . .
H221 H 0.0207 0.2877 0.8579 0.0313 1.0000 Uiso R . . . . .
H222 H 0.1080 0.3490 0.8134 0.0313 1.0000 Uiso R . . . . .
H231 H -0.1745 0.3624 0.8325 0.0358 1.0000 Uiso R . . . . .
H232 H -0.0839 0.4259 0.7938 0.0353 1.0000 Uiso R . . . . .
H241 H -0.0765 0.3843 0.9433 0.0423 1.0000 Uiso R . . . . .
H242 H 0.0356 0.4364 0.9084 0.0403 1.0000 Uiso R . . . . .
H251 H -0.1224 0.5335 0.8863 0.0639 1.0000 Uiso R . . . . .
H252 H -0.1315 0.5117 0.9704 0.0659 1.0000 Uiso R . . . . .
H253 H -0.2424 0.4810 0.9134 0.0649 1.0000 Uiso R . . . . .
H261 H -0.1147 0.2008 0.8090 0.0327 1.0000 Uiso R . . . . .
H262 H -0.2017 0.2616 0.7648 0.0306 1.0000 Uiso R . . . . .
H271 H -0.0794 0.1334 0.6975 0.0398 1.0000 Uiso R . . . . .
H272 H -0.1722 0.1914 0.6568 0.0398 1.0000 Uiso R . . . . .
H281 H -0.3556 0.1564 0.7307 0.0512 1.0000 Uiso R . . . . .
H282 H -0.2622 0.0955 0.7725 0.0530 1.0000 Uiso R . . . . .
H291 H -0.3313 0.0803 0.6221 0.0824 1.0000 Uiso R . . . . .
H292 H -0.2423 0.0196 0.6680 0.0828 1.0000 Uiso R . . . . .
H293 H -0.4022 0.0311 0.6863 0.0810 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.4964(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O11 . C14 . 1.4279(15) yes
O11 . H111 . 0.855 no
O12 . C16 . 1.4148(16) yes
O12 . H121 . 0.855 no
O13 . C17 . 1.4211(16) yes
O13 . H131 . 0.834 no
C14 . C15 . 1.5233(18) yes
C14 . H141 . 0.998 no
C14 . H142 . 0.980 no
C15 . C16 . 1.5304(17) yes
C15 . C17 . 1.5258(17) yes
C15 . C18 . 1.5263(17) yes
C16 . H161 . 0.985 no
C16 . H162 . 0.991 no
C17 . H171 . 0.973 no
C17 . H172 . 0.972 no
C18 . H181 . 0.967 no
C18 . H182 . 1.005 no
C18 . H183 . 0.968 no
N21 . C26 7_556 1.5219(13) yes
N21 . C22 7_556 1.5202(13) yes
N21 . C22 . 1.5202(13) yes
N21 . C26 . 1.5219(13) yes
C22 . C23 . 1.5172(16) yes
C22 . H221 . 0.978 no
C22 . H222 . 0.974 no
C23 . C24 . 1.5260(16) yes
C23 . H231 . 0.961 no
C23 . H232 . 0.990 no
C24 . C25 . 1.5165(18) yes
C24 . H241 . 0.964 no
C24 . H242 . 0.978 no
C25 . H251 . 0.967 no
C25 . H252 . 0.984 no
C25 . H253 . 0.987 no
C26 . C27 . 1.5137(16) yes
C26 . H261 . 0.981 no
C26 . H262 . 0.980 no
C27 . C28 . 1.5215(17) yes
C27 . H271 . 0.950 no
C27 . H272 . 0.980 no
C28 . C29 . 1.5124(19) yes
C28 . H281 . 0.990 no
C28 . H282 . 0.969 no
C29 . H291 . 1.004 no
C29 . H292 . 0.995 no
C29 . H293 . 1.009 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C14 . O11 . H111 . 108.4 no
C16 . O12 . H121 . 106.2 no
C17 . O13 . H131 . 108.6 no
O11 . C14 . C15 . 113.96(10) yes
O11 . C14 . H141 . 106.6 no
C15 . C14 . H141 . 108.3 no
O11 . C14 . H142 . 109.5 no
C15 . C14 . H142 . 109.6 no
H141 . C14 . H142 . 108.7 no
C14 . C15 . C16 . 111.03(10) yes
C14 . C15 . C17 . 107.94(11) yes
C16 . C15 . C17 . 109.23(10) yes
C14 . C15 . C18 . 110.04(11) yes
C16 . C15 . C18 . 108.13(11) yes
C17 . C15 . C18 . 110.48(11) yes
C15 . C16 . O12 . 114.36(11) yes
C15 . C16 . H161 . 107.7 no
O12 . C16 . H161 . 106.4 no
C15 . C16 . H162 . 108.7 no
O12 . C16 . H162 . 109.4 no
H161 . C16 . H162 . 110.2 no
C15 . C17 . O13 . 109.91(10) yes
C15 . C17 . H171 . 109.0 no
O13 . C17 . H171 . 111.1 no
C15 . C17 . H172 . 107.9 no
O13 . C17 . H172 . 109.8 no
H171 . C17 . H172 . 109.2 no
C15 . C18 . H181 . 112.0 no
C15 . C18 . H182 . 110.0 no
H181 . C18 . H182 . 108.7 no
C15 . C18 . H183 . 110.1 no
H181 . C18 . H183 . 105.2 no
H182 . C18 . H183 . 110.8 no
C26 7_556 N21 . C22 7_556 107.86(6) yes
C26 7_556 N21 . C22 . 108.96(6) yes
C22 7_556 N21 . C22 . 112.00(12) yes
C26 7_556 N21 . C26 . 111.23(12) yes
C22 7_556 N21 . C26 . 108.96(6) yes
C22 . N21 . C26 . 107.86(6) yes
N21 . C22 . C23 . 116.25(9) yes
N21 . C22 . H221 . 104.4 no
C23 . C22 . H221 . 109.5 no
N21 . C22 . H222 . 106.9 no
C23 . C22 . H222 . 109.7 no
H221 . C22 . H222 . 109.8 no
C22 . C23 . C24 . 109.02(10) yes
C22 . C23 . H231 . 109.7 no
C24 . C23 . H231 . 109.1 no
C22 . C23 . H232 . 110.3 no
C24 . C23 . H232 . 109.6 no
H231 . C23 . H232 . 109.0 no
C23 . C24 . C25 . 113.14(11) yes
C23 . C24 . H241 . 108.2 no
C25 . C24 . H241 . 109.8 no
C23 . C24 . H242 . 107.8 no
C25 . C24 . H242 . 109.9 no
H241 . C24 . H242 . 107.8 no
C24 . C25 . H251 . 109.7 no
C24 . C25 . H252 . 109.9 no
H251 . C25 . H252 . 109.5 no
C24 . C25 . H253 . 110.4 no
H251 . C25 . H253 . 107.9 no
H252 . C25 . H253 . 109.4 no
N21 . C26 . C27 . 116.66(9) yes
N21 . C26 . H261 . 107.1 no
C27 . C26 . H261 . 109.6 no
N21 . C26 . H262 . 106.7 no
C27 . C26 . H262 . 108.6 no
H261 . C26 . H262 . 107.9 no
C26 . C27 . C28 . 109.20(10) yes
C26 . C27 . H271 . 110.1 no
C28 . C27 . H271 . 110.5 no
C26 . C27 . H272 . 110.4 no
C28 . C27 . H272 . 109.2 no
H271 . C27 . H272 . 107.4 no
C27 . C28 . C29 . 113.29(12) yes
C27 . C28 . H281 . 108.2 no
C29 . C28 . H281 . 108.5 no
C27 . C28 . H282 . 109.6 no
C29 . C28 . H282 . 107.6 no
H281 . C28 . H282 . 109.6 no
C28 . C29 . H291 . 111.3 no
C28 . C29 . H292 . 110.3 no
H291 . C29 . H292 . 107.4 no
C28 . C29 . H293 . 111.7 no
H291 . C29 . H293 . 106.8 no
H292 . C29 . H293 . 109.1 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O13 . H131 . O11 5_556 177.42 0.834 1.908 2.7408(19) yes
C22 . H222 . O12 7_656 155.96 0.974 2.397 3.3106(19) yes
C26 . H261 . O13 4_555 142.56 0.981 2.522 3.3544(19) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 18/03/13 at 12:15:02
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE O   (  11,X'S) H   ( 111,X'S) 
RIDE O   (  12,X'S) H   ( 121,X'S) 
RIDE O   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 142,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) H   ( 183,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 252,X'S) H   ( 253,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   ( 282,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 293,X'S) H   ( 292,X'S) H   ( 291,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 18/03/13 at 12:15:02
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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_2d
_database_code_depnum_ccdc_archive 'CCDC 1401768'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             13-05-14
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 034kme12
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   22.5166(1)
_cell_length_b                   14.2863(1)
_cell_length_c                   19.8783(1)
_cell_angle_alpha                90
_cell_angle_beta                 103.6255(5)
_cell_angle_gamma                90
_cell_volume                     6214.47(6)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1 '
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C26 H60 F1 N1 O4.50 
# Dc =      1.02 Fooo =   2112.00 Mu =      5.68 M =    477.76
# Found Formula = C26 H60 F1 N1 O4 
# Dc =      1.00 FOOO =   2112.00 Mu =      5.49 M =    469.76

_chemical_formula_sum            'C26 H60 F1 N1 O4'
_chemical_formula_moiety         'C16 H36 N, 2(C5 H12 O2), F'
_chemical_compound_source        .
_chemical_formula_weight         469.76


_cell_measurement_reflns_used    39155
_cell_measurement_theta_min      4
_cell_measurement_theta_max      77
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.180
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.280

_exptl_crystal_density_diffrn    1.004
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2112
_exptl_absorpt_coefficient_mu    0.549

# Sheldrick geometric approximatio 0.90 0.91 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_T_max  0.91
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            66092
_reflns_number_total             6505
_diffrn_reflns_av_R_equivalents  0.023
# Number of reflections with Friedels Law is 6505 
# Theoretical number of reflections is about 11090 


_diffrn_reflns_theta_min         3.695
_diffrn_reflns_theta_max         76.711
_diffrn_measured_fraction_theta_max 0.994

_diffrn_reflns_theta_full        75.176
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       24
_reflns_limit_h_min              -28
_reflns_limit_h_max              27
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   3.73
_oxford_diffrn_Wilson_scale      0.13

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.24
_refine_diff_density_max         0.49


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         5509
_refine_ls_number_restraints     0
_refine_ls_number_parameters     289
_oxford_refine_ls_R_factor_ref   0.0582
_refine_ls_wR_factor_ref         0.1516
_refine_ls_goodness_of_fit_ref   0.9944
_refine_ls_shift/su_max          0.0005318
_refine_ls_shift/su_mean         0.0000441


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        5509
_refine_ls_R_factor_all          0.0582
_refine_ls_wR_factor_all         0.1516

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5097
_refine_ls_R_factor_gt           0.0556
_refine_ls_wR_factor_gt          0.1490

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.08P)² + 5.77P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
F1 F 0.27929(5) 0.55808(9) 0.84295(6) 0.0629 1.0000 Uani . . . . . .
O11 O 0.19226(6) 0.56868(9) 0.90730(6) 0.0512 1.0000 Uani . . . . . .
C12 C 0.17577(9) 0.47292(14) 0.90524(9) 0.0525 1.0000 Uani . . . . . .
C13 C 0.12471(7) 0.44455(13) 0.84337(9) 0.0468 1.0000 Uani . . . . . .
C14 C 0.06545(10) 0.4930(3) 0.84832(14) 0.0936 1.0000 Uani . . . . . .
C15 C 0.14046(8) 0.47872(15) 0.77642(9) 0.0543 1.0000 Uani . . . . . .
C16 C 0.11831(15) 0.33954(19) 0.84267(17) 0.0964 1.0000 Uani . . . . . .
O21 O 0.19725(6) 0.44414(10) 0.76830(7) 0.0583 1.0000 Uani . . . . . .
O31 O 0.36838(6) 0.64090(10) 0.93026(7) 0.0624 1.0000 Uani . . . . . .
C32 C 0.41744(9) 0.58453(19) 0.92155(9) 0.0637 1.0000 Uani . . . . . .
C33 C 0.44791(7) 0.61732(13) 0.86506(9) 0.0459 1.0000 Uani . . . . . .
C34 C 0.47911(13) 0.7110(2) 0.88439(19) 0.1093 1.0000 Uani . . . . . .
C35 C 0.40052(9) 0.62826(15) 0.79771(9) 0.0552 1.0000 Uani . . . . . .
C36 C 0.49523(10) 0.5444(2) 0.85677(14) 0.0776 1.0000 Uani . . . . . .
O41 O 0.36741(7) 0.54633(13) 0.77632(7) 0.0789 1.0000 Uani . . . . . .
N51 N 0.30616(5) 0.37557(8) 0.62249(5) 0.0277 1.0000 Uani . . . . . .
C52 C 0.30821(7) 0.35878(10) 0.69880(7) 0.0307 1.0000 Uani . . . . . .
C53 C 0.29169(8) 0.26154(11) 0.71804(8) 0.0422 1.0000 Uani . . . . . .
C54 C 0.30035(8) 0.25731(12) 0.79648(8) 0.0401 1.0000 Uani . . . . . .
C55 C 0.28373(13) 0.16493(14) 0.82282(10) 0.0678 1.0000 Uani . . . . . .
C56 C 0.24257(6) 0.35633(10) 0.57777(7) 0.0307 1.0000 Uani . . . . . .
C57 C 0.19228(7) 0.41868(12) 0.59140(8) 0.0395 1.0000 Uani . . . . . .
C58 C 0.13093(7) 0.38828(13) 0.54628(8) 0.0425 1.0000 Uani . . . . . .
C59 C 0.07871(8) 0.44949(17) 0.55641(11) 0.0619 1.0000 Uani . . . . . .
C60 C 0.32372(7) 0.47761(10) 0.61749(7) 0.0310 1.0000 Uani . . . . . .
C61 C 0.32710(8) 0.51198(11) 0.54635(8) 0.0401 1.0000 Uani . . . . . .
C62 C 0.33514(9) 0.61783(12) 0.54818(9) 0.0473 1.0000 Uani . . . . . .
C63 C 0.34632(12) 0.65723(16) 0.48130(11) 0.0705 1.0000 Uani . . . . . .
C64 C 0.34973(6) 0.31102(10) 0.59677(7) 0.0302 1.0000 Uani . . . . . .
C65 C 0.41536(7) 0.31184(12) 0.63904(8) 0.0404 1.0000 Uani . . . . . .
C66 C 0.45651(8) 0.25982(15) 0.60124(9) 0.0503 1.0000 Uani . . . . . .
C67 C 0.52172(9) 0.25000(19) 0.64297(14) 0.0748 1.0000 Uani . . . . . .
H121 H 0.1610 0.4576 0.9470 0.0631 1.0000 Uiso R . . . . .
H122 H 0.2115 0.4317 0.9047 0.0631 1.0000 Uiso R . . . . .
H142 H 0.0352 0.4729 0.8070 0.1396 1.0000 Uiso R . . . . .
H141 H 0.0528 0.4716 0.8897 0.1399 1.0000 Uiso R . . . . .
H143 H 0.0714 0.5626 0.8494 0.1401 1.0000 Uiso R . . . . .
H151 H 0.1401 0.5496 0.7771 0.0658 1.0000 Uiso R . . . . .
H152 H 0.1078 0.4545 0.7359 0.0657 1.0000 Uiso R . . . . .
H162 H 0.0838 0.3265 0.8025 0.1448 1.0000 Uiso R . . . . .
H163 H 0.1101 0.3239 0.8890 0.1448 1.0000 Uiso R . . . . .
H161 H 0.1571 0.3130 0.8353 0.1454 1.0000 Uiso R . . . . .
H322 H 0.4482 0.5840 0.9650 0.0778 1.0000 Uiso R . . . . .
H321 H 0.4030 0.5196 0.9094 0.0750 1.0000 Uiso R . . . . .
H341 H 0.4997 0.7300 0.8481 0.1634 1.0000 Uiso R . . . . .
H342 H 0.5092 0.7070 0.9291 0.1648 1.0000 Uiso R . . . . .
H343 H 0.4486 0.7592 0.8878 0.1632 1.0000 Uiso R . . . . .
H351 H 0.3718 0.6792 0.8051 0.0650 1.0000 Uiso R . . . . .
H352 H 0.4222 0.6461 0.7620 0.0664 1.0000 Uiso R . . . . .
H361 H 0.5206 0.5709 0.8270 0.1152 1.0000 Uiso R . . . . .
H362 H 0.5212 0.5277 0.9018 0.1162 1.0000 Uiso R . . . . .
H363 H 0.4727 0.4876 0.8347 0.1163 1.0000 Uiso R . . . . .
H522 H 0.3491 0.3748 0.7231 0.0361 1.0000 Uiso R . . . . .
H521 H 0.2801 0.4038 0.7114 0.0347 1.0000 Uiso R . . . . .
H531 H 0.3182 0.2181 0.7053 0.0529 1.0000 Uiso R . . . . .
H532 H 0.2501 0.2467 0.6960 0.0529 1.0000 Uiso R . . . . .
H541 H 0.3416 0.2721 0.8177 0.0498 1.0000 Uiso R . . . . .
H542 H 0.2753 0.3052 0.8096 0.0497 1.0000 Uiso R . . . . .
H551 H 0.2893 0.1652 0.8729 0.0996 1.0000 Uiso R . . . . .
H553 H 0.3094 0.1179 0.8114 0.1024 1.0000 Uiso R . . . . .
H552 H 0.2427 0.1478 0.8020 0.1035 1.0000 Uiso R . . . . .
H561 H 0.2342 0.2918 0.5857 0.0367 1.0000 Uiso R . . . . .
H562 H 0.2452 0.3631 0.5296 0.0359 1.0000 Uiso R . . . . .
H572 H 0.1915 0.4150 0.6386 0.0480 1.0000 Uiso R . . . . .
H571 H 0.2004 0.4827 0.5813 0.0476 1.0000 Uiso R . . . . .
H581 H 0.1243 0.3242 0.5564 0.0508 1.0000 Uiso R . . . . .
H582 H 0.1328 0.3923 0.4987 0.0500 1.0000 Uiso R . . . . .
H592 H 0.0410 0.4292 0.5262 0.0913 1.0000 Uiso R . . . . .
H591 H 0.0746 0.4434 0.6022 0.0920 1.0000 Uiso R . . . . .
H593 H 0.0854 0.5145 0.5468 0.0922 1.0000 Uiso R . . . . .
H602 H 0.3624 0.4857 0.6496 0.0353 1.0000 Uiso R . . . . .
H601 H 0.2943 0.5139 0.6337 0.0364 1.0000 Uiso R . . . . .
H611 H 0.3616 0.4828 0.5327 0.0488 1.0000 Uiso R . . . . .
H612 H 0.2913 0.4953 0.5132 0.0493 1.0000 Uiso R . . . . .
H622 H 0.3695 0.6350 0.5867 0.0567 1.0000 Uiso R . . . . .
H621 H 0.2985 0.6459 0.5572 0.0583 1.0000 Uiso R . . . . .
H631 H 0.3482 0.7240 0.4854 0.1045 1.0000 Uiso R . . . . .
H632 H 0.3848 0.6356 0.4739 0.1069 1.0000 Uiso R . . . . .
H633 H 0.3142 0.6405 0.4421 0.1057 1.0000 Uiso R . . . . .
H641 H 0.3336 0.2493 0.5967 0.0355 1.0000 Uiso R . . . . .
H642 H 0.3477 0.3300 0.5506 0.0345 1.0000 Uiso R . . . . .
H652 H 0.4295 0.3749 0.6472 0.0507 1.0000 Uiso R . . . . .
H651 H 0.4183 0.2821 0.6835 0.0497 1.0000 Uiso R . . . . .
H661 H 0.4564 0.2913 0.5574 0.0621 1.0000 Uiso R . . . . .
H662 H 0.4384 0.1982 0.5900 0.0613 1.0000 Uiso R . . . . .
H672 H 0.5464 0.2188 0.6159 0.1111 1.0000 Uiso R . . . . .
H671 H 0.5393 0.3084 0.6587 0.1118 1.0000 Uiso R . . . . .
H673 H 0.5219 0.2117 0.6834 0.1115 1.0000 Uiso R . . . . .
H111 H 0.2225 0.5718 0.8873 0.0771 1.0000 Uiso R . . . . .
H411 H 0.3374 0.5481 0.7956 0.1168 1.0000 Uiso R . . . . .
H311 H 0.3363 0.6269 0.9008 0.0932 1.0000 Uiso R . . . . .
H211 H 0.2227 0.4783 0.7924 0.0863 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.85(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O11 . C12 . 1.416(2) yes
O11 . H111 . 0.866 no
C12 . C13 . 1.527(2) yes
C12 . H121 . 0.989 no
C12 . H122 . 0.998 no
C13 . C14 . 1.527(3) yes
C13 . C15 . 1.536(2) yes
C13 . C16 . 1.507(3) yes
C14 . H142 . 0.979 no
C14 . H141 . 0.980 no
C14 . H143 . 1.003 no
C15 . O21 . 1.415(2) yes
C15 . H151 . 1.013 no
C15 . H152 . 1.015 no
C16 . H162 . 0.991 no
C16 . H163 . 1.006 no
C16 . H161 . 0.995 no
O21 . H211 . 0.816 no
O31 . C32 . 1.410(3) yes
O31 . H311 . 0.841 no
C32 . C33 . 1.521(2) yes
C32 . H322 . 0.971 no
C32 . H321 . 0.994 no
C33 . C34 . 1.518(3) yes
C33 . C35 . 1.511(3) yes
C33 . C36 . 1.526(3) yes
C34 . H341 . 0.984 no
C34 . H342 . 0.984 no
C34 . H343 . 0.986 no
C35 . O41 . 1.399(3) yes
C35 . H351 . 1.008 no
C35 . H352 . 0.985 no
C36 . H361 . 0.989 no
C36 . H362 . 0.976 no
C36 . H363 . 1.002 no
O41 . H411 . 0.853 no
N51 . C52 . 1.5255(16) yes
N51 . C56 . 1.5219(17) yes
N51 . C60 . 1.5198(17) yes
N51 . C64 . 1.5200(17) yes
C52 . C53 . 1.511(2) yes
C52 . H522 . 0.961 no
C52 . H521 . 0.976 no
C53 . C54 . 1.526(2) yes
C53 . H531 . 0.937 no
C53 . H532 . 0.960 no
C54 . C55 . 1.500(2) yes
C54 . H541 . 0.949 no
C54 . H542 . 0.961 no
C55 . H551 . 0.975 no
C55 . H553 . 0.947 no
C55 . H552 . 0.951 no
C56 . C57 . 1.515(2) yes
C56 . H561 . 0.961 no
C56 . H562 . 0.979 no
C57 . C58 . 1.522(2) yes
C57 . H572 . 0.944 no
C57 . H571 . 0.964 no
C58 . C59 . 1.516(2) yes
C58 . H581 . 0.956 no
C58 . H582 . 0.958 no
C59 . H592 . 0.962 no
C59 . H591 . 0.940 no
C59 . H593 . 0.967 no
C60 . C61 . 1.5158(19) yes
C60 . H602 . 0.958 no
C60 . H601 . 0.955 no
C61 . C62 . 1.522(2) yes
C61 . H611 . 0.975 no
C61 . H612 . 0.944 no
C62 . C63 . 1.518(2) yes
C62 . H622 . 0.983 no
C62 . H621 . 0.972 no
C63 . H631 . 0.957 no
C63 . H632 . 0.963 no
C63 . H633 . 0.961 no
C64 . C65 . 1.518(2) yes
C64 . H641 . 0.954 no
C64 . H642 . 0.948 no
C65 . C66 . 1.518(2) yes
C65 . H652 . 0.956 no
C65 . H651 . 0.969 no
C66 . C67 . 1.513(3) yes
C66 . H661 . 0.979 no
C66 . H662 . 0.973 no
C67 . H672 . 0.968 no
C67 . H671 . 0.945 no
C67 . H673 . 0.972 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C12 . O11 . H111 . 105.4 no
O11 . C12 . C13 . 114.98(15) yes
O11 . C12 . H121 . 109.1 no
C13 . C12 . H121 . 106.2 no
O11 . C12 . H122 . 111.4 no
C13 . C12 . H122 . 106.9 no
H121 . C12 . H122 . 108.0 no
C12 . C13 . C14 . 109.36(16) yes
C12 . C13 . C15 . 109.26(14) yes
C14 . C13 . C15 . 107.19(18) yes
C12 . C13 . C16 . 108.9(2) yes
C14 . C13 . C16 . 111.6(2) yes
C15 . C13 . C16 . 110.46(18) yes
C13 . C14 . H142 . 105.0 no
C13 . C14 . H141 . 110.2 no
H142 . C14 . H141 . 109.3 no
C13 . C14 . H143 . 109.6 no
H142 . C14 . H143 . 111.8 no
H141 . C14 . H143 . 110.8 no
C13 . C15 . O21 . 112.79(16) yes
C13 . C15 . H151 . 107.6 no
O21 . C15 . H151 . 111.1 no
C13 . C15 . H152 . 107.9 no
O21 . C15 . H152 . 107.2 no
H151 . C15 . H152 . 110.1 no
C13 . C16 . H162 . 104.5 no
C13 . C16 . H163 . 104.5 no
H162 . C16 . H163 . 114.7 no
C13 . C16 . H161 . 107.2 no
H162 . C16 . H161 . 111.0 no
H163 . C16 . H161 . 114.0 no
C15 . O21 . H211 . 104.6 no
C32 . O31 . H311 . 110.4 no
O31 . C32 . C33 . 114.67(18) yes
O31 . C32 . H322 . 108.0 no
C33 . C32 . H322 . 108.0 no
O31 . C32 . H321 . 110.0 no
C33 . C32 . H321 . 106.7 no
H322 . C32 . H321 . 109.4 no
C32 . C33 . C34 . 110.30(18) yes
C32 . C33 . C35 . 109.81(14) yes
C34 . C33 . C35 . 108.7(2) yes
C32 . C33 . C36 . 108.50(18) yes
C34 . C33 . C36 . 109.61(18) yes
C35 . C33 . C36 . 109.89(16) yes
C33 . C34 . H341 . 109.1 no
C33 . C34 . H342 . 110.9 no
H341 . C34 . H342 . 109.5 no
C33 . C34 . H343 . 110.1 no
H341 . C34 . H343 . 108.3 no
H342 . C34 . H343 . 108.8 no
C33 . C35 . O41 . 113.41(16) yes
C33 . C35 . H351 . 106.8 no
O41 . C35 . H351 . 109.5 no
C33 . C35 . H352 . 107.4 no
O41 . C35 . H352 . 108.5 no
H351 . C35 . H352 . 111.3 no
C33 . C36 . H361 . 108.6 no
C33 . C36 . H362 . 110.5 no
H361 . C36 . H362 . 109.6 no
C33 . C36 . H363 . 107.9 no
H361 . C36 . H363 . 110.6 no
H362 . C36 . H363 . 109.6 no
C35 . O41 . H411 . 105.1 no
C52 . N51 . C56 . 110.88(10) yes
C52 . N51 . C60 . 105.57(10) yes
C56 . N51 . C60 . 111.01(10) yes
C52 . N51 . C64 . 111.61(10) yes
C56 . N51 . C64 . 106.67(10) yes
C60 . N51 . C64 . 111.19(10) yes
N51 . C52 . C53 . 116.41(11) yes
N51 . C52 . H522 . 105.2 no
C53 . C52 . H522 . 110.9 no
N51 . C52 . H521 . 106.4 no
C53 . C52 . H521 . 109.1 no
H522 . C52 . H521 . 108.5 no
C52 . C53 . C54 . 108.38(12) yes
C52 . C53 . H531 . 109.2 no
C54 . C53 . H531 . 108.3 no
C52 . C53 . H532 . 111.0 no
C54 . C53 . H532 . 109.5 no
H531 . C53 . H532 . 110.3 no
C53 . C54 . C55 . 114.16(14) yes
C53 . C54 . H541 . 108.8 no
C55 . C54 . H541 . 109.8 no
C53 . C54 . H542 . 107.9 no
C55 . C54 . H542 . 108.7 no
H541 . C54 . H542 . 107.3 no
C54 . C55 . H551 . 111.8 no
C54 . C55 . H553 . 108.9 no
H551 . C55 . H553 . 108.0 no
C54 . C55 . H552 . 111.8 no
H551 . C55 . H552 . 108.9 no
H553 . C55 . H552 . 107.3 no
N51 . C56 . C57 . 115.43(11) yes
N51 . C56 . H561 . 105.8 no
C57 . C56 . H561 . 110.5 no
N51 . C56 . H562 . 106.7 no
C57 . C56 . H562 . 109.7 no
H561 . C56 . H562 . 108.3 no
C56 . C57 . C58 . 109.86(12) yes
C56 . C57 . H572 . 109.6 no
C58 . C57 . H572 . 110.0 no
C56 . C57 . H571 . 109.6 no
C58 . C57 . H571 . 109.7 no
H572 . C57 . H571 . 108.0 no
C57 . C58 . C59 . 112.43(15) yes
C57 . C58 . H581 . 108.3 no
C59 . C58 . H581 . 111.0 no
C57 . C58 . H582 . 108.6 no
C59 . C58 . H582 . 108.2 no
H581 . C58 . H582 . 108.2 no
C58 . C59 . H592 . 110.0 no
C58 . C59 . H591 . 109.3 no
H592 . C59 . H591 . 107.7 no
C58 . C59 . H593 . 111.4 no
H592 . C59 . H593 . 108.8 no
H591 . C59 . H593 . 109.5 no
N51 . C60 . C61 . 116.28(11) yes
N51 . C60 . H602 . 106.3 no
C61 . C60 . H602 . 110.2 no
N51 . C60 . H601 . 106.7 no
C61 . C60 . H601 . 109.3 no
H602 . C60 . H601 . 107.7 no
C60 . C61 . C62 . 109.35(13) yes
C60 . C61 . H611 . 109.9 no
C62 . C61 . H611 . 109.5 no
C60 . C61 . H612 . 110.3 no
C62 . C61 . H612 . 110.2 no
H611 . C61 . H612 . 107.7 no
C61 . C62 . C63 . 112.99(16) yes
C61 . C62 . H622 . 109.5 no
C63 . C62 . H622 . 109.2 no
C61 . C62 . H621 . 108.2 no
C63 . C62 . H621 . 109.4 no
H622 . C62 . H621 . 107.4 no
C62 . C63 . H631 . 107.9 no
C62 . C63 . H632 . 110.8 no
H631 . C63 . H632 . 108.1 no
C62 . C63 . H633 . 111.7 no
H631 . C63 . H633 . 109.0 no
H632 . C63 . H633 . 109.2 no
N51 . C64 . C65 . 115.49(11) yes
N51 . C64 . H641 . 106.6 no
C65 . C64 . H641 . 109.3 no
N51 . C64 . H642 . 105.3 no
C65 . C64 . H642 . 110.6 no
H641 . C64 . H642 . 109.3 no
C64 . C65 . C66 . 110.52(13) yes
C64 . C65 . H652 . 110.0 no
C66 . C65 . H652 . 109.1 no
C64 . C65 . H651 . 110.5 no
C66 . C65 . H651 . 108.6 no
H652 . C65 . H651 . 108.1 no
C65 . C66 . C67 . 113.62(15) yes
C65 . C66 . H661 . 109.9 no
C67 . C66 . H661 . 109.3 no
C65 . C66 . H662 . 106.5 no
C67 . C66 . H662 . 110.0 no
H661 . C66 . H662 . 107.3 no
C66 . C67 . H672 . 110.4 no
C66 . C67 . H671 . 112.1 no
H672 . C67 . H671 . 109.9 no
C66 . C67 . H673 . 108.7 no
H672 . C67 . H673 . 108.1 no
H671 . C67 . H673 . 107.6 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C52 . H521 . O21 . 151.40 0.976 2.467 3.356(3) yes
C57 . H572 . O21 . 166.98 0.944 2.584 3.511(3) yes
C58 . H582 . O11 6_564 150.01 0.958 2.559 3.423(3) yes
C64 . H642 . O31 6_564 165.30 0.948 2.576 3.501(3) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 14/05/13 at 12:04:27
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE O   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  14,X'S) H   ( 142,X'S) H   ( 141,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 162,X'S) H   ( 163,X'S) H   ( 161,X'S) 
RIDE O   (  21,X'S) H   ( 211,X'S) 
RIDE O   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 322,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) H   ( 343,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE O   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  52,X'S) H   ( 522,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 553,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) 
RIDE C   (  57,X'S) H   ( 572,X'S) H   ( 571,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) H   ( 582,X'S) 
RIDE C   (  59,X'S) H   ( 592,X'S) H   ( 591,X'S) H   ( 593,X'S) 
RIDE C   (  60,X'S) H   ( 602,X'S) H   ( 601,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) H   ( 612,X'S) 
RIDE C   (  62,X'S) H   ( 622,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) H   ( 632,X'S) H   ( 633,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) H   ( 642,X'S) 
RIDE C   (  65,X'S) H   ( 652,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 662,X'S) 
RIDE C   (  67,X'S) H   ( 672,X'S) H   ( 671,X'S) H   ( 673,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 14/05/13 at 12:04:27
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-2 2 3 x .
####################################################################### 
# 
# 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_2e
_database_code_depnum_ccdc_archive 'CCDC 1401769'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             13-05-16
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 066ggke01
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   18.9780(2)
_cell_length_b                   24.2645(2)
_cell_length_c                   10.3218(1)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4753.10(8)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2 '
_symmetry_space_group_name_Hall  'P 2 2ab'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,-y+1/2,-z
-x+1/2,y+1/2,-z
-x,-y,z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C39 H81 F1.50 N1.50 O9 
# Dc =      1.04 Fooo =   1679.68 Mu =      0.76 M =    743.57
# Found Formula = C38.39 H77.58 F1 N1 O12 
# Dc =      1.07 FOOO =   1679.68 Mu =      0.80 M =    764.30

_chemical_formula_sum            'C38.39 H77.58 F1 N1 O12'
_chemical_formula_moiety         '2(C10 H18 O6), C16 H36 N, 0.2(C12 H28), F'
_chemical_compound_source        .
_chemical_formula_weight         764.30


_cell_measurement_reflns_used    5976
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       prism
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_max          0.43

_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1679.681
_exptl_absorpt_coefficient_mu    0.080

# Sheldrick geometric approximatio 0.99 0.99 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_T_max  0.99
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            65091
_reflns_number_total             10799
_diffrn_reflns_av_R_equivalents  0.044
# Number of reflections without Friedels Law is 10799 
# Number of reflections with Friedels Law is 5965 
# Theoretical number of reflections is about 5449 


_diffrn_reflns_theta_min         5.098
_diffrn_reflns_theta_max         27.480
_diffrn_measured_fraction_theta_max 0.989

_diffrn_reflns_theta_full        26.381
_diffrn_measured_fraction_theta_full 0.990


_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_reflns_limit_h_min              0
_reflns_limit_h_max              24
_reflns_limit_k_min              0
_reflns_limit_k_max              31
_reflns_limit_l_min              -13
_reflns_limit_l_max              13

_oxford_diffrn_Wilson_B_factor   3.64
_oxford_diffrn_Wilson_scale      4.01

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.25
_refine_diff_density_max         0.30


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         10798
_refine_ls_number_restraints     201
_refine_ls_number_parameters     525
_oxford_refine_ls_R_factor_ref   0.0675
_refine_ls_wR_factor_ref         0.0978
_refine_ls_goodness_of_fit_ref   0.9807
_refine_ls_shift/su_max          0.0005858
_refine_ls_shift/su_mean         0.0000551


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        10798
_refine_ls_R_factor_all          0.0675
_refine_ls_wR_factor_all         0.0978

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8103
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_gt          0.0884

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration unk


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 1.09P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
F1 F 0.38987(6) 0.66501(4) 0.55042(11) 0.0562 1.0000 Uani . . . . . .
O1 O 0.41033(6) 0.76097(5) 0.64710(11) 0.0467 1.0000 Uani . . . . . .
O2 O 0.47328(6) 0.71936(5) 0.39319(11) 0.0418 1.0000 Uani . . . . . .
C11 C 0.47021(9) 0.78025(7) 0.58129(16) 0.0378 1.0000 Uani . . . . . .
C12 C 0.53757(10) 0.75258(7) 0.62622(15) 0.0403 1.0000 Uani . . . . . .
O13 O 0.54185(7) 0.71738(5) 0.70782(12) 0.0519 1.0000 Uani . . . . . .
O14 O 0.59264(6) 0.77369(5) 0.56172(12) 0.0448 1.0000 Uani . . . . . .
C15 C 0.66275(9) 0.75182(8) 0.59001(18) 0.0457 1.0000 Uani . . . . . .
C16 C 0.69355(12) 0.78477(12) 0.6989(2) 0.0734 1.0000 Uani . . . . . .
C17 C 0.70371(11) 0.75631(9) 0.46650(19) 0.0575 1.0000 Uani . . . . . .
C21 C 0.46447(9) 0.77395(7) 0.43383(15) 0.0367 1.0000 Uani . . . . . .
C22 C 0.39556(9) 0.79820(7) 0.38627(18) 0.0426 1.0000 Uani . . . . . .
O23 O 0.35312(7) 0.77425(6) 0.32158(14) 0.0577 1.0000 Uani . . . . . .
O24 O 0.38858(7) 0.85058(5) 0.42566(16) 0.0596 1.0000 Uani . . . . . .
C25 C 0.32136(12) 0.87790(9) 0.4010(3) 0.0744 1.0000 Uani . . . . . .
C26 C 0.30962(17) 0.91663(12) 0.5145(4) 0.1059 1.0000 Uani . . . . . .
C27 C 0.32673(18) 0.90662(15) 0.2725(3) 0.1128 1.0000 Uani . . . . . .
O3 O 0.29555(6) 0.61281(5) 0.41622(12) 0.0448 1.0000 Uani . . . . . .
O4 O 0.35730(6) 0.57468(5) 0.67130(11) 0.0434 1.0000 Uani . . . . . .
C31 C 0.29994(9) 0.55846(7) 0.46107(16) 0.0363 1.0000 Uani . . . . . .
C32 C 0.36461(9) 0.52865(7) 0.41062(17) 0.0389 1.0000 Uani . . . . . .
O33 O 0.41043(7) 0.54899(6) 0.34677(14) 0.0559 1.0000 Uani . . . . . .
O34 O 0.36194(6) 0.47567(5) 0.44535(13) 0.0502 1.0000 Uani D . . . . .
C35 C 0.42043(7) 0.43892(7) 0.41075(15) 0.0508 1.0000 Uani D . . . . .
C36 C 0.45195(17) 0.41837(14) 0.5328(3) 0.0817 0.829(5) Uani D . P 1 1 .
C37 C 0.39098(15) 0.39389(13) 0.3282(3) 0.0836 0.829(5) Uani D . P 1 1 .
C41 C 0.29656(8) 0.55510(7) 0.61007(16) 0.0352 1.0000 Uani . . . . . .
C42 C 0.23008(9) 0.58516(7) 0.65513(17) 0.0384 1.0000 Uani . . . . . .
O43 O 0.22842(7) 0.62320(5) 0.72902(13) 0.0490 1.0000 Uani . . . . . .
O44 O 0.17333(6) 0.56223(5) 0.59978(13) 0.0454 1.0000 Uani . . . . . .
C45 C 0.10487(9) 0.58799(8) 0.6218(2) 0.0524 1.0000 Uani . . . . . .
C46 C 0.07139(13) 0.56248(11) 0.7393(3) 0.0754 1.0000 Uani . . . . . .
C47 C 0.06346(12) 0.57784(10) 0.4992(3) 0.0729 1.0000 Uani . . . . . .
C136 C 0.4162(5) 0.3902(4) 0.4961(11) 0.0640 0.171(5) Uani D . P 1 2 .
C137 C 0.4131(5) 0.4253(5) 0.2735(7) 0.0691 0.171(5) Uani D . P 1 2 .
N51 N 0.40169(8) 0.67074(6) 1.00236(12) 0.0390 1.0000 Uani . . . . . .
C52 C 0.44769(10) 0.63533(8) 0.91481(17) 0.0476 1.0000 Uani . . . . . .
C53 C 0.50461(12) 0.60213(8) 0.9808(2) 0.0571 1.0000 Uani . . . . . .
C54 C 0.54774(14) 0.57168(10) 0.8789(3) 0.0813 1.0000 Uani . . . . . .
C55 C 0.60603(18) 0.53728(12) 0.9350(4) 0.1118 1.0000 Uani . . . . . .
C56 C 0.44696(9) 0.70737(7) 1.08770(16) 0.0397 1.0000 Uani . . . . . .
C57 C 0.49863(10) 0.74387(8) 1.01570(17) 0.0458 1.0000 Uani . . . . . .
C58 C 0.53989(10) 0.77993(8) 1.10932(18) 0.0517 1.0000 Uani . . . . . .
C59 C 0.59497(12) 0.81480(9) 1.0419(2) 0.0622 1.0000 Uani . . . . . .
C60 C 0.35509(10) 0.70491(8) 0.91370(16) 0.0461 1.0000 Uani . . . . . .
C61 C 0.30676(11) 0.74521(9) 0.98112(19) 0.0548 1.0000 Uani . . . . . .
C62 C 0.25904(12) 0.77342(11) 0.8840(2) 0.0730 1.0000 Uani . . . . . .
C63 C 0.21368(16) 0.81727(12) 0.9466(3) 0.0986 1.0000 Uani . . . . . .
C64 C 0.35733(9) 0.63501(7) 1.09236(16) 0.0417 1.0000 Uani . . . . . .
C65 C 0.30009(11) 0.60185(8) 1.02640(18) 0.0527 1.0000 Uani . . . . . .
C66 C 0.26653(12) 0.56089(10) 1.1176(2) 0.0629 1.0000 Uani . . . . . .
C67 C 0.20779(15) 0.52851(12) 1.0541(3) 0.0935 1.0000 Uani . . . . . .
C101 C 0.4168(6) 0.8875(4) 0.8986(8) 0.0999 0.398(4) Uani D . P 2 -1 .
C102 C 0.4533(4) 0.9371(2) 0.9509(6) 0.0865 0.398(4) Uani D . P 2 -1 .
C103 C 0.4804(5) 0.9787(3) 0.8486(5) 0.0892 0.398(4) Uani D . P 2 -1 .
C104 C 0.5174(4) 1.0298(3) 0.9155(5) 0.0858 0.398(4) Uani D . P 2 -1 .
C105 C 0.5433(4) 1.0721(2) 0.8128(6) 0.0933 0.398(4) Uani D . P 2 -1 .
C106 C 0.5957(7) 1.1135(4) 0.8596(8) 0.0951 0.398(4) Uani D . P 2 -1 .
H111 H 0.4736 0.8192 0.5995 0.0429 1.0000 Uiso R . . . . .
H151 H 0.6570 0.7132 0.6174 0.0534 1.0000 Uiso R . . . . .
H163 H 0.7413 0.7727 0.7154 0.1098 1.0000 Uiso R . . . . .
H162 H 0.6640 0.7803 0.7750 0.1085 1.0000 Uiso R . . . . .
H161 H 0.6926 0.8234 0.6744 0.1109 1.0000 Uiso R . . . . .
H172 H 0.7515 0.7421 0.4789 0.0855 1.0000 Uiso R . . . . .
H171 H 0.6800 0.7344 0.3979 0.0860 1.0000 Uiso R . . . . .
H173 H 0.7067 0.7957 0.4404 0.0852 1.0000 Uiso R . . . . .
H211 H 0.5026 0.7958 0.3945 0.0407 1.0000 Uiso R . . . . .
H251 H 0.2804 0.8511 0.4039 0.0883 1.0000 Uiso R . . . . .
H261 H 0.2635 0.9355 0.5038 0.1586 1.0000 Uiso R . . . . .
H263 H 0.3101 0.8942 0.5952 0.1593 1.0000 Uiso R . . . . .
H262 H 0.3493 0.9432 0.5111 0.1589 1.0000 Uiso R . . . . .
H273 H 0.2810 0.9245 0.2580 0.1689 1.0000 Uiso R . . . . .
H272 H 0.3368 0.8783 0.2090 0.1686 1.0000 Uiso R . . . . .
H271 H 0.3638 0.9342 0.2784 0.1681 1.0000 Uiso R . . . . .
H311 H 0.2603 0.5387 0.4276 0.0428 1.0000 Uiso R . . . . .
H361 H 0.4908 0.3946 0.5124 0.1217 0.829(5) Uiso R . P 1 1 .
H362 H 0.4657 0.4499 0.5822 0.1229 0.829(5) Uiso R . P 1 1 .
H363 H 0.4151 0.3972 0.5781 0.1220 0.829(5) Uiso R . P 1 1 .
H371 H 0.4311 0.3701 0.3057 0.1244 0.829(5) Uiso R . P 1 1 .
H373 H 0.3687 0.4097 0.2510 0.1248 0.829(5) Uiso R . P 1 1 .
H372 H 0.3559 0.3747 0.3788 0.1241 0.829(5) Uiso R . P 1 1 .
H411 H 0.2904 0.5164 0.6324 0.0392 1.0000 Uiso R . . . . .
H451 H 0.1138 0.6273 0.6319 0.0618 1.0000 Uiso R . . . . .
H461 H 0.0256 0.5803 0.7555 0.1117 1.0000 Uiso R . . . . .
H463 H 0.1011 0.5674 0.8172 0.1127 1.0000 Uiso R . . . . .
H462 H 0.0632 0.5233 0.7241 0.1106 1.0000 Uiso R . . . . .
H472 H 0.0156 0.5935 0.5136 0.1079 1.0000 Uiso R . . . . .
H471 H 0.0887 0.5958 0.4269 0.1082 1.0000 Uiso R . . . . .
H473 H 0.0623 0.5381 0.4845 0.1060 1.0000 Uiso R . . . . .
H1361 H 0.4597 0.3694 0.4895 0.0958 0.171(5) Uiso R . P 1 2 .
H1363 H 0.4093 0.4014 0.5841 0.0958 0.171(5) Uiso R . P 1 2 .
H1362 H 0.3770 0.3680 0.4701 0.0957 0.171(5) Uiso R . P 1 2 .
H1372 H 0.4547 0.4056 0.2474 0.1040 0.171(5) Uiso R . P 1 2 .
H1371 H 0.4093 0.4587 0.2250 0.1039 0.171(5) Uiso R . P 1 2 .
H1373 H 0.3715 0.4030 0.2606 0.1039 0.171(5) Uiso R . P 1 2 .
H522 H 0.4701 0.6600 0.8519 0.0559 1.0000 Uiso R . . . . .
H521 H 0.4155 0.6097 0.8687 0.0576 1.0000 Uiso R . . . . .
H532 H 0.5356 0.6280 1.0300 0.0681 1.0000 Uiso R . . . . .
H531 H 0.4841 0.5746 1.0405 0.0659 1.0000 Uiso R . . . . .
H541 H 0.5709 0.5990 0.8227 0.0979 1.0000 Uiso R . . . . .
H542 H 0.5158 0.5498 0.8270 0.0971 1.0000 Uiso R . . . . .
H551 H 0.6296 0.5166 0.8657 0.1676 1.0000 Uiso R . . . . .
H553 H 0.6393 0.5620 0.9808 0.1679 1.0000 Uiso R . . . . .
H552 H 0.5842 0.5104 0.9957 0.1677 1.0000 Uiso R . . . . .
H562 H 0.4140 0.7290 1.1402 0.0453 1.0000 Uiso R . . . . .
H561 H 0.4736 0.6826 1.1440 0.0463 1.0000 Uiso R . . . . .
H571 H 0.4726 0.7672 0.9567 0.0554 1.0000 Uiso R . . . . .
H572 H 0.5314 0.7210 0.9669 0.0549 1.0000 Uiso R . . . . .
H581 H 0.5049 0.8039 1.1544 0.0624 1.0000 Uiso R . . . . .
H582 H 0.5628 0.7559 1.1737 0.0622 1.0000 Uiso R . . . . .
H591 H 0.6223 0.8362 1.1060 0.0926 1.0000 Uiso R . . . . .
H593 H 0.5727 0.8397 0.9791 0.0917 1.0000 Uiso R . . . . .
H592 H 0.6285 0.7919 0.9935 0.0920 1.0000 Uiso R . . . . .
H602 H 0.3860 0.7254 0.8558 0.0535 1.0000 Uiso R . . . . .
H601 H 0.3276 0.6788 0.8635 0.0553 1.0000 Uiso R . . . . .
H612 H 0.3338 0.7738 1.0269 0.0654 1.0000 Uiso R . . . . .
H611 H 0.2781 0.7265 1.0427 0.0669 1.0000 Uiso R . . . . .
H621 H 0.2899 0.7906 0.8201 0.0882 1.0000 Uiso R . . . . .
H622 H 0.2289 0.7468 0.8452 0.0884 1.0000 Uiso R . . . . .
H632 H 0.1825 0.8327 0.8858 0.1477 1.0000 Uiso R . . . . .
H633 H 0.2456 0.8478 0.9736 0.1466 1.0000 Uiso R . . . . .
H631 H 0.1889 0.8038 1.0220 0.1466 1.0000 Uiso R . . . . .
H641 H 0.3372 0.6603 1.1549 0.0491 1.0000 Uiso R . . . . .
H642 H 0.3904 0.6113 1.1381 0.0485 1.0000 Uiso R . . . . .
H651 H 0.2631 0.6278 0.9938 0.0628 1.0000 Uiso R . . . . .
H652 H 0.3200 0.5815 0.9561 0.0633 1.0000 Uiso R . . . . .
H661 H 0.2517 0.5802 1.1978 0.0754 1.0000 Uiso R . . . . .
H662 H 0.3036 0.5348 1.1434 0.0751 1.0000 Uiso R . . . . .
H671 H 0.1872 0.5035 1.1168 0.1394 1.0000 Uiso R . . . . .
H672 H 0.1711 0.5505 1.0197 0.1402 1.0000 Uiso R . . . . .
H673 H 0.2278 0.5064 0.9822 0.1395 1.0000 Uiso R . . . . .
H11 H 0.4041 0.7289 0.6208 0.0686 1.0000 Uiso R . . . . .
H21 H 0.4454 0.6997 0.4341 0.0627 1.0000 Uiso R . . . . .
H41 H 0.3668 0.6044 0.6387 0.0652 1.0000 Uiso R . . . . .
H31 H 0.3271 0.6317 0.4531 0.0670 1.0000 Uiso R . . . . .
H1021 H 0.4212 0.9539 1.0112 0.1049 0.398(4) Uiso R . P 2 -1 .
H1022 H 0.4940 0.9233 0.9952 0.1050 0.398(4) Uiso R . P 2 -1 .
H1031 H 0.4402 0.9904 0.7937 0.1083 0.398(4) Uiso R . P 2 -1 .
H1032 H 0.5148 0.9573 0.7938 0.1076 0.398(4) Uiso R . P 2 -1 .
H1041 H 0.4831 1.0487 0.9719 0.1039 0.398(4) Uiso R . P 2 -1 .
H1042 H 0.5569 1.0160 0.9695 0.1039 0.398(4) Uiso R . P 2 -1 .
H1051 H 0.5033 1.0916 0.7874 0.1125 0.398(4) Uiso R . P 2 -1 .
H1052 H 0.5657 1.0549 0.7396 0.1116 0.398(4) Uiso R . P 2 -1 .
H351 H 0.4557 0.4596 0.3571 0.0606 0.829(5) Uiso R . P 1 1 .
H352 H 0.4652 0.4580 0.4255 0.0607 0.171(5) Uiso R . P 1 2 .
H1061 H 0.5797 1.1498 0.8412 0.1444 0.398(4) Uiso R . P 2 -1 .
H1062 H 0.6004 1.1076 0.9536 0.1435 0.398(4) Uiso R . P 2 -1 .
H1063 H 0.6390 1.1065 0.8128 0.1435 0.398(4) Uiso R . P 2 -1 .
H1011 H 0.3673 0.8926 0.9104 0.1517 0.398(4) Uiso R . P 2 -1 .
H1012 H 0.4314 0.8876 0.8095 0.1518 0.398(4) Uiso R . P 2 -1 .
H1013 H 0.4336 0.8574 0.9487 0.1522 0.398(4) Uiso R . P 2 -1 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.5272(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 . C11 . 1.4042(19) yes
O1 . H11 . 0.833 no
O2 . C21 . 1.3993(19) yes
O2 . H21 . 0.829 no
C11 . C12 . 1.517(2) yes
C11 . C21 . 1.534(2) yes
C11 . H111 . 0.965 no
C12 . O13 . 1.202(2) yes
C12 . O14 . 1.341(2) yes
O14 . C15 . 1.462(2) yes
C15 . C16 . 1.498(3) yes
C15 . C17 . 1.497(3) yes
C15 . H151 . 0.984 no
C16 . H163 . 0.968 no
C16 . H162 . 0.972 no
C16 . H161 . 0.972 no
C17 . H172 . 0.978 no
C17 . H171 . 0.993 no
C17 . H173 . 0.995 no
C21 . C22 . 1.516(2) yes
C21 . H211 . 0.985 no
C22 . O23 . 1.197(2) yes
C22 . O24 . 1.341(2) yes
O24 . C25 . 1.460(2) yes
C25 . C26 . 1.518(4) yes
C25 . C27 . 1.502(4) yes
C25 . H251 . 1.014 no
C26 . H261 . 0.993 no
C26 . H263 . 0.996 no
C26 . H262 . 0.992 no
C27 . H273 . 0.983 no
C27 . H272 . 0.968 no
C27 . H271 . 0.974 no
O3 . C31 . 1.4003(19) yes
O3 . H31 . 0.845 no
O4 . C41 . 1.3979(19) yes
O4 . H41 . 0.815 no
C31 . C32 . 1.517(2) yes
C31 . C41 . 1.541(2) yes
C31 . H311 . 0.957 no
C32 . O33 . 1.198(2) yes
C32 . O34 . 1.335(2) yes
O34 . C35 . 1.4679(18) yes
C35 . C36 . 1.481(3) yes
C35 . C37 . 1.494(3) yes
C35 . H351 . 1.003 no
C35 . C136 . 1.477(6) yes
C35 . C137 . 1.461(6) yes
C35 . H352 . 0.980 no
C36 . H361 . 0.959 no
C36 . H362 . 0.955 no
C36 . H363 . 0.986 no
C37 . H371 . 0.982 no
C37 . H373 . 0.980 no
C37 . H372 . 0.965 no
C41 . C42 . 1.530(2) yes
C41 . H411 . 0.974 no
C42 . O43 . 1.198(2) yes
C42 . O44 . 1.340(2) yes
O44 . C45 . 1.460(2) yes
C45 . C46 . 1.502(3) yes
C45 . C47 . 1.510(3) yes
C45 . H451 . 0.974 no
C46 . H461 . 0.985 no
C46 . H463 . 0.989 no
C46 . H462 . 0.976 no
C47 . H472 . 0.997 no
C47 . H471 . 0.988 no
C47 . H473 . 0.977 no
C136 . H1361 . 0.970 no
C136 . H1363 . 0.958 no
C136 . H1362 . 0.957 no
C137 . H1372 . 0.962 no
C137 . H1371 . 0.956 no
C137 . H1373 . 0.966 no
N51 . C52 . 1.522(2) yes
N51 . C56 . 1.518(2) yes
N51 . C60 . 1.519(2) yes
N51 . C64 . 1.524(2) yes
C52 . C53 . 1.510(3) yes
C52 . H522 . 0.981 no
C52 . H521 . 0.994 no
C53 . C54 . 1.524(3) yes
C53 . H532 . 1.000 no
C53 . H531 . 0.989 no
C54 . C55 . 1.502(4) yes
C54 . H541 . 0.985 no
C54 . H542 . 0.967 no
C55 . H551 . 0.982 no
C55 . H553 . 0.990 no
C55 . H552 . 0.995 no
C56 . C57 . 1.516(2) yes
C56 . H562 . 0.980 no
C56 . H561 . 0.978 no
C57 . C58 . 1.521(2) yes
C57 . H571 . 0.967 no
C57 . H572 . 0.973 no
C58 . C59 . 1.514(3) yes
C58 . H581 . 0.998 no
C58 . H582 . 0.986 no
C59 . H591 . 0.988 no
C59 . H593 . 0.981 no
C59 . H592 . 0.982 no
C60 . C61 . 1.511(3) yes
C60 . H602 . 0.974 no
C60 . H601 . 0.970 no
C61 . C62 . 1.515(3) yes
C61 . H612 . 0.984 no
C61 . H611 . 0.952 no
C62 . C63 . 1.513(4) yes
C62 . H621 . 0.975 no
C62 . H622 . 0.951 no
C63 . H632 . 0.940 no
C63 . H633 . 0.996 no
C63 . H631 . 0.966 no
C64 . C65 . 1.514(3) yes
C64 . H641 . 0.969 no
C64 . H642 . 0.973 no
C65 . C66 . 1.510(3) yes
C65 . H651 . 1.001 no
C65 . H652 . 0.956 no
C66 . C67 . 1.513(3) yes
C66 . H661 . 0.992 no
C66 . H662 . 0.982 no
C67 . H671 . 0.969 no
C67 . H672 . 0.947 no
C67 . H673 . 0.992 no
C101 . C102 . 1.489(5) yes
C101 . H1011 . 0.955 no
C101 . H1012 . 0.961 no
C101 . H1013 . 0.949 no
C102 . C103 . 1.549(5) yes
C102 . H1021 . 0.963 no
C102 . H1022 . 0.958 no
C103 . C104 . 1.584(5) yes
C103 . H1031 . 0.991 no
C103 . H1032 . 1.008 no
C104 . C105 . 1.555(5) yes
C104 . H1041 . 0.987 no
C104 . H1042 . 0.992 no
C105 . C106 . 1.494(5) yes
C105 . H1051 . 0.932 no
C105 . H1052 . 0.962 no
C106 . H1061 . 0.951 no
C106 . H1062 . 0.985 no
C106 . H1063 . 0.969 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C11 . O1 . H11 . 105.6 no
C21 . O2 . H21 . 108.4 no
O1 . C11 . C12 . 112.75(13) yes
O1 . C11 . C21 . 112.92(13) yes
C12 . C11 . C21 . 108.61(13) yes
O1 . C11 . H111 . 106.6 no
C12 . C11 . H111 . 108.5 no
C21 . C11 . H111 . 107.2 no
C11 . C12 . O13 . 125.86(15) yes
C11 . C12 . O14 . 109.64(14) yes
O13 . C12 . O14 . 124.50(17) yes
C12 . O14 . C15 . 118.14(13) yes
O14 . C15 . C16 . 108.14(16) yes
O14 . C15 . C17 . 106.02(15) yes
C16 . C15 . C17 . 113.41(17) yes
O14 . C15 . H151 . 107.6 no
C16 . C15 . H151 . 109.6 no
C17 . C15 . H151 . 111.8 no
C15 . C16 . H163 . 109.7 no
C15 . C16 . H162 . 108.8 no
H163 . C16 . H162 . 111.4 no
C15 . C16 . H161 . 108.2 no
H163 . C16 . H161 . 110.8 no
H162 . C16 . H161 . 107.8 no
C15 . C17 . H172 . 110.1 no
C15 . C17 . H171 . 109.5 no
H172 . C17 . H171 . 108.9 no
C15 . C17 . H173 . 109.3 no
H172 . C17 . H173 . 108.7 no
H171 . C17 . H173 . 110.4 no
C11 . C21 . O2 . 112.55(13) yes
C11 . C21 . C22 . 110.12(14) yes
O2 . C21 . C22 . 111.93(14) yes
C11 . C21 . H211 . 107.6 no
O2 . C21 . H211 . 107.4 no
C22 . C21 . H211 . 106.9 no
C21 . C22 . O23 . 124.95(16) yes
C21 . C22 . O24 . 110.79(16) yes
O23 . C22 . O24 . 124.25(17) yes
C22 . O24 . C25 . 117.63(16) yes
O24 . C25 . C26 . 106.0(2) yes
O24 . C25 . C27 . 107.8(2) yes
C26 . C25 . C27 . 113.8(2) yes
O24 . C25 . H251 . 111.9 no
C26 . C25 . H251 . 105.2 no
C27 . C25 . H251 . 112.1 no
C25 . C26 . H261 . 109.2 no
C25 . C26 . H263 . 107.8 no
H261 . C26 . H263 . 110.7 no
C25 . C26 . H262 . 105.3 no
H261 . C26 . H262 . 111.5 no
H263 . C26 . H262 . 112.2 no
C25 . C27 . H273 . 106.3 no
C25 . C27 . H272 . 106.4 no
H273 . C27 . H272 . 112.6 no
C25 . C27 . H271 . 108.3 no
H273 . C27 . H271 . 110.2 no
H272 . C27 . H271 . 112.7 no
C31 . O3 . H31 . 108.6 no
C41 . O4 . H41 . 107.2 no
O3 . C31 . C32 . 112.56(14) yes
O3 . C31 . C41 . 112.16(14) yes
C32 . C31 . C41 . 110.55(13) yes
O3 . C31 . H311 . 107.8 no
C32 . C31 . H311 . 105.9 no
C41 . C31 . H311 . 107.5 no
C31 . C32 . O33 . 125.44(16) yes
C31 . C32 . O34 . 109.64(14) yes
O33 . C32 . O34 . 124.89(16) yes
C32 . O34 . C35 . 119.39(12) yes
O34 . C35 . C36 . 107.64(7) yes
O34 . C35 . C37 . 107.46(7) yes
C36 . C35 . C37 . 112.95(7) yes
O34 . C35 . H351 . 109.5 no
C36 . C35 . H351 . 111.6 no
C37 . C35 . H351 . 107.5 no
O34 . C35 . C136 . 107.47(7) yes
O34 . C35 . C137 . 107.56(7) yes
C136 . C35 . C137 . 113.03(7) yes
O34 . C35 . H352 . 109.3 no
C136 . C35 . H352 . 109.5 no
C137 . C35 . H352 . 109.9 no
C35 . C36 . H361 . 109.0 no
C35 . C36 . H362 . 107.2 no
H361 . C36 . H362 . 112.8 no
C35 . C36 . H363 . 107.0 no
H361 . C36 . H363 . 109.7 no
H362 . C36 . H363 . 110.9 no
C35 . C37 . H371 . 105.9 no
C35 . C37 . H373 . 109.8 no
H371 . C37 . H373 . 111.8 no
C35 . C37 . H372 . 107.6 no
H371 . C37 . H372 . 112.3 no
H373 . C37 . H372 . 109.3 no
C31 . C41 . O4 . 113.50(13) yes
C31 . C41 . C42 . 108.21(13) yes
O4 . C41 . C42 . 112.37(13) yes
C31 . C41 . H411 . 107.0 no
O4 . C41 . H411 . 108.6 no
C42 . C41 . H411 . 106.8 no
C41 . C42 . O43 . 125.65(16) yes
C41 . C42 . O44 . 109.59(13) yes
O43 . C42 . O44 . 124.76(16) yes
C42 . O44 . C45 . 118.12(14) yes
O44 . C45 . C46 . 109.01(17) yes
O44 . C45 . C47 . 105.24(16) yes
C46 . C45 . C47 . 112.89(18) yes
O44 . C45 . H451 . 106.3 no
C46 . C45 . H451 . 113.0 no
C47 . C45 . H451 . 109.9 no
C45 . C46 . H461 . 109.2 no
C45 . C46 . H463 . 111.5 no
H461 . C46 . H463 . 108.1 no
C45 . C46 . H462 . 109.8 no
H461 . C46 . H462 . 108.4 no
H463 . C46 . H462 . 109.8 no
C45 . C47 . H472 . 106.7 no
C45 . C47 . H471 . 108.0 no
H472 . C47 . H471 . 112.8 no
C45 . C47 . H473 . 107.6 no
H472 . C47 . H473 . 112.3 no
H471 . C47 . H473 . 109.2 no
C35 . C136 . H1361 . 109.2 no
C35 . C136 . H1363 . 110.1 no
H1361 . C136 . H1363 . 109.3 no
C35 . C136 . H1362 . 109.0 no
H1361 . C136 . H1362 . 110.5 no
H1363 . C136 . H1362 . 108.7 no
C35 . C137 . H1372 . 107.9 no
C35 . C137 . H1371 . 108.8 no
H1372 . C137 . H1371 . 109.7 no
C35 . C137 . H1373 . 109.8 no
H1372 . C137 . H1373 . 110.7 no
H1371 . C137 . H1373 . 109.9 no
C52 . N51 . C56 . 110.51(13) yes
C52 . N51 . C60 . 106.52(13) yes
C56 . N51 . C60 . 111.08(13) yes
C52 . N51 . C64 . 110.94(13) yes
C56 . N51 . C64 . 106.98(12) yes
C60 . N51 . C64 . 110.86(13) yes
N51 . C52 . C53 . 116.34(15) yes
N51 . C52 . H522 . 107.2 no
C53 . C52 . H522 . 108.4 no
N51 . C52 . H521 . 106.6 no
C53 . C52 . H521 . 108.8 no
H522 . C52 . H521 . 109.4 no
C52 . C53 . C54 . 109.35(19) yes
C52 . C53 . H532 . 108.4 no
C54 . C53 . H532 . 109.8 no
C52 . C53 . H531 . 111.1 no
C54 . C53 . H531 . 108.3 no
H532 . C53 . H531 . 109.9 no
C53 . C54 . C55 . 113.5(2) yes
C53 . C54 . H541 . 108.6 no
C55 . C54 . H541 . 105.8 no
C53 . C54 . H542 . 108.2 no
C55 . C54 . H542 . 111.7 no
H541 . C54 . H542 . 108.9 no
C54 . C55 . H551 . 109.8 no
C54 . C55 . H553 . 108.5 no
H551 . C55 . H553 . 111.6 no
C54 . C55 . H552 . 107.5 no
H551 . C55 . H552 . 108.2 no
H553 . C55 . H552 . 111.2 no
N51 . C56 . C57 . 115.07(13) yes
N51 . C56 . H562 . 105.9 no
C57 . C56 . H562 . 111.7 no
N51 . C56 . H561 . 106.1 no
C57 . C56 . H561 . 108.4 no
H562 . C56 . H561 . 109.4 no
C56 . C57 . C58 . 110.96(14) yes
C56 . C57 . H571 . 108.7 no
C58 . C57 . H571 . 109.1 no
C56 . C57 . H572 . 109.5 no
C58 . C57 . H572 . 109.1 no
H571 . C57 . H572 . 109.4 no
C57 . C58 . C59 . 112.64(16) yes
C57 . C58 . H581 . 106.8 no
C59 . C58 . H581 . 110.4 no
C57 . C58 . H582 . 108.4 no
C59 . C58 . H582 . 109.6 no
H581 . C58 . H582 . 109.0 no
C58 . C59 . H591 . 110.3 no
C58 . C59 . H593 . 110.4 no
H591 . C59 . H593 . 110.2 no
C58 . C59 . H592 . 111.4 no
H591 . C59 . H592 . 107.4 no
H593 . C59 . H592 . 107.0 no
N51 . C60 . C61 . 115.42(14) yes
N51 . C60 . H602 . 107.3 no
C61 . C60 . H602 . 108.6 no
N51 . C60 . H601 . 106.2 no
C61 . C60 . H601 . 110.0 no
H602 . C60 . H601 . 109.2 no
C60 . C61 . C62 . 110.53(17) yes
C60 . C61 . H612 . 111.2 no
C62 . C61 . H612 . 108.1 no
C60 . C61 . H611 . 110.3 no
C62 . C61 . H611 . 108.4 no
H612 . C61 . H611 . 108.2 no
C61 . C62 . C63 . 112.1(2) yes
C61 . C62 . H621 . 106.4 no
C63 . C62 . H621 . 109.3 no
C61 . C62 . H622 . 109.4 no
C63 . C62 . H622 . 108.3 no
H621 . C62 . H622 . 111.5 no
C62 . C63 . H632 . 110.7 no
C62 . C63 . H633 . 107.3 no
H632 . C63 . H633 . 105.9 no
C62 . C63 . H631 . 112.5 no
H632 . C63 . H631 . 111.5 no
H633 . C63 . H631 . 108.7 no
N51 . C64 . C65 . 115.13(13) yes
N51 . C64 . H641 . 105.3 no
C65 . C64 . H641 . 110.7 no
N51 . C64 . H642 . 106.0 no
C65 . C64 . H642 . 111.5 no
H641 . C64 . H642 . 107.8 no
C64 . C65 . C66 . 111.85(15) yes
C64 . C65 . H651 . 108.6 no
C66 . C65 . H651 . 109.1 no
C64 . C65 . H652 . 109.5 no
C66 . C65 . H652 . 107.4 no
H651 . C65 . H652 . 110.3 no
C65 . C66 . C67 . 112.50(19) yes
C65 . C66 . H661 . 109.2 no
C67 . C66 . H661 . 113.5 no
C65 . C66 . H662 . 106.9 no
C67 . C66 . H662 . 108.1 no
H661 . C66 . H662 . 106.3 no
C66 . C67 . H671 . 109.4 no
C66 . C67 . H672 . 114.3 no
H671 . C67 . H672 . 107.9 no
C66 . C67 . H673 . 108.8 no
H671 . C67 . H673 . 108.4 no
H672 . C67 . H673 . 107.8 no
C102 . C101 . H1011 . 107.8 no
C102 . C101 . H1012 . 102.2 no
H1011 . C101 . H1012 . 113.9 no
C102 . C101 . H1013 . 105.5 no
H1011 . C101 . H1013 . 111.1 no
H1012 . C101 . H1013 . 115.2 no
C101 . C102 . C103 . 115.71(7) yes
C101 . C102 . H1021 . 106.4 no
C103 . C102 . H1021 . 112.0 no
C101 . C102 . H1022 . 105.4 no
C103 . C102 . H1022 . 106.6 no
H1021 . C102 . H1022 . 110.5 no
C102 . C103 . C104 . 111.08(7) yes
C102 . C103 . H1031 . 108.7 no
C104 . C103 . H1031 . 111.5 no
C102 . C103 . H1032 . 105.2 no
C104 . C103 . H1032 . 111.1 no
H1031 . C103 . H1032 . 109.0 no
C103 . C104 . C105 . 111.05(7) yes
C103 . C104 . H1041 . 109.2 no
C105 . C104 . H1041 . 107.6 no
C103 . C104 . H1042 . 108.4 no
C105 . C104 . H1042 . 111.5 no
H1041 . C104 . H1042 . 109.0 no
C104 . C105 . C106 . 115.72(7) yes
C104 . C105 . H1051 . 105.7 no
C106 . C105 . H1051 . 107.0 no
C104 . C105 . H1052 . 112.9 no
C106 . C105 . H1052 . 104.5 no
H1051 . C105 . H1052 . 111.0 no
C105 . C106 . H1061 . 110.2 no
C105 . C106 . H1062 . 106.3 no
H1061 . C106 . H1062 . 111.1 no
C105 . C106 . H1063 . 106.6 no
H1061 . C106 . H1063 . 109.5 no
H1062 . C106 . H1063 . 112.9 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C16 . H163 . O23 2_566 158.21 0.968 2.438 3.356(5) yes
C52 . H522 . O13 . 171.90 0.981 2.450 3.424(5) yes
C52 . H521 . O4 . 152.40 0.994 2.468 3.380(5) yes
C56 . H562 . O23 1_556 163.77 0.980 2.459 3.411(5) yes
C60 . H602 . O1 . 149.54 0.974 2.366 3.244(5) yes
C66 . H661 . O3 1_556 142.99 0.992 2.530 3.375(5) yes
C35 . H351 . O33 4_665 130.24 1.003 2.552 3.290(5) yes
C35 . H352 . O33 4_665 137.35 0.980 2.501 3.290(5) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 16/05/13 at 18:59:41
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIV PART(-2001,OCC) 
RIDE O   (   1,X'S) H   (  11,X'S) 
RIDE O   (   2,X'S) H   (  21,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 163,X'S) H   ( 162,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 172,X'S) H   ( 171,X'S) H   ( 173,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 263,X'S) H   ( 262,X'S) 
RIDE C   (  27,X'S) H   ( 273,X'S) H   ( 272,X'S) H   ( 271,X'S) 
RIDE O   (   3,X'S) H   (  31,X'S) 
RIDE O   (   4,X'S) H   (  41,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 373,X'S) H   ( 372,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 463,X'S) H   ( 462,X'S) 
RIDE C   (  47,X'S) H   ( 472,X'S) H   ( 471,X'S) H   ( 473,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) H   (1363,X'S) H   (1362,X'S) 
RIDE C   ( 137,X'S) H   (1372,X'S) H   (1371,X'S) H   (1373,X'S) 
RIDE C   (  52,X'S) H   ( 522,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 532,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 553,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 562,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) H   ( 572,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) H   ( 582,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) H   ( 593,X'S) H   ( 592,X'S) 
RIDE C   (  60,X'S) H   ( 602,X'S) H   ( 601,X'S) 
RIDE C   (  61,X'S) H   ( 612,X'S) H   ( 611,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) 
RIDE C   (  63,X'S) H   ( 632,X'S) H   ( 633,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) H   ( 642,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) H   ( 652,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 662,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) H   ( 672,X'S) H   ( 673,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) H   (1012,X'S) H   (1013,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) H   (1022,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) H   (1032,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) H   (1042,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) H   (1052,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) H   (1062,X'S) H   (1063,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 16/05/13 at 18:59:41
#
#LIST     16                                                                    
SAME  C(101)  C(102)  C(103)  C(104)  C(105)  C(106)  AND 
CONT  C(106)  C(105)  C(104)  C(103)  C(102)  C(101) 
SIMU  0.01    C(101)  C(102)  C(103)  C(104)  C(105)  C(106)  AND 
CONT  C(106)  C(105)  C(104)  C(103)  C(102)  C(101) 
DELU  0.01    C(101)  C(102)  C(103)  C(104)  C(105)  C(106)  AND 
CONT  C(106)  C(105)  C(104)  C(103)  C(102)  C(101) 
DIST 1.54,0.01 = 
CONT  C(101)  TO  C(102)  C(102)  TO  C(103)  C(103)  TO  C(104) 
CONT  C(104)  TO  C(105)  C(105)  TO  C(106) 
SAME  O(34)  C(35)  C(36)  C(37)  AND 
CONT  O(34)  C(35)  C(37)  C(36)  AND 
CONT  O(34)  C(35)  C(136)  C(137)  AND 
CONT  O(34)  C(35)  C(137)  C(136) 
SIMU  0.01   O(34)  C(35)  C(36)  C(37)  AND 
CONT  O(34)  C(35)  C(37)  C(36)  AND 
CONT  O(34)  C(35)  C(136)  C(137)  AND 
CONT  O(34)  C(35)  C(137)  C(136) 
DELU  0.01   O(34)  C(35)  C(36)  C(37)  AND 
CONT  O(34)  C(35)  C(37)  C(36)  AND 
CONT  O(34)  C(35)  C(136)  C(137)  AND 
CONT  O(34)  C(35)  C(137)  C(136) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
0 6 1 x .
####################################################################### 
# 
# 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_2f
_database_code_depnum_ccdc_archive 'CCDC 1401770'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             2014-12-19
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title 003lp14
_chemical_name_systematic        .
_chemical_melting_point          '362 K'

_refine_special_details          
;
On first examination, it was found that there was solvent present
which was identified as diethyl ether.  On initial refinement, the 
ADPs became prolate indicating disorder so a two site model was 
used with restraints applied to maintain sensible geometries and 
displacement parameters for the individual components.  
;

_cell_length_a                   25.1923(1)
_cell_length_b                   9.6565(1)
_cell_length_c                   10.6715(1)
_cell_angle_alpha                90
_cell_angle_beta                 92.2457(5)
_cell_angle_gamma                90
_cell_volume                     2594.06(4)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2 '
_symmetry_space_group_name_Hall  'C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C40 H80 F1 N1 O12 
# Dc =      2.01 Fooo =    960.00 Mu =     12.29 M =    786.07
# Found Formula = C22 H44 F0.50 N0.50 O7 
# Dc =      1.12 FOOO =    960.00 Mu =      6.89 M =    437.09

_chemical_formula_sum            'C22 H44 F0.50 N0.50 O7'
_chemical_formula_moiety         
'C12 H22 O6, 0.5(C16 H36 N), 0.5(C4 H8 O3), 0.5(F)'
_chemical_compound_source        .
_chemical_formula_weight         437.09


_cell_measurement_reflns_used    43761
_cell_measurement_theta_min      4
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_max          0.20

_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    0.689

# Sheldrick geometric approximatio 1.00 1.00 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_T_max  1.00
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            49863
_reflns_number_total             5371
_diffrn_reflns_av_R_equivalents  0.020
# Number of reflections without Friedels Law is 5371 
# Number of reflections with Friedels Law is 2861 
# Theoretical number of reflections is about 2709 


_diffrn_reflns_theta_min         3.511
_diffrn_reflns_theta_max         76.028
_diffrn_measured_fraction_theta_max 0.996

_diffrn_reflns_theta_full        76.028
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_reflns_limit_h_min              -31
_reflns_limit_h_max              31
_reflns_limit_k_min              -12
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              13

_oxford_diffrn_Wilson_B_factor   3.21
_oxford_diffrn_Wilson_scale      0.07

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.20
_refine_diff_density_max         0.26


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         5353
_refine_ls_number_restraints     623
_refine_ls_number_parameters     321
_oxford_refine_ls_R_factor_ref   0.0327
_refine_ls_wR_factor_ref         0.0889
_refine_ls_goodness_of_fit_ref   1.0044
_refine_ls_shift/su_max          0.0003897
_refine_ls_shift/su_mean         0.0000321


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        5353
_refine_ls_R_factor_all          0.0327
_refine_ls_wR_factor_all         0.0889

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5330
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_gt          0.0889

_refine_ls_abs_structure_Flack   0.02(10)
_refine_ls_abs_structure_details 'Flack (1983), 2510 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.06P)² + 0.76P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
F1 F 0.5000 0.29093(14) 0.0000 0.0461 1.0000 Uani S T . . . .
O1 O 0.39970(3) 0.36457(9) -0.02106(7) 0.0289 1.0000 Uani . . . . . .
C11 C 0.37073(4) 0.24111(11) -0.04825(9) 0.0238 1.0000 Uani . . . . . .
C12 C 0.36889(4) 0.15315(12) 0.07075(10) 0.0265 1.0000 Uani . . . . . .
C13 C 0.33440(5) 0.21737(14) 0.16840(11) 0.0338 1.0000 Uani . . . . . .
O14 O 0.28256(3) 0.17026(12) 0.12972(9) 0.0407 1.0000 Uani . . . . . .
C15 C 0.28884(5) 0.03256(15) 0.08343(13) 0.0395 1.0000 Uani . . . . . .
O16 O 0.34320(3) 0.02270(10) 0.04716(8) 0.0329 1.0000 Uani . . . . . .
C17 C 0.25181(6) 0.0139(2) -0.03001(16) 0.0547 1.0000 Uani . . . . . .
C18 C 0.27987(7) -0.07335(18) 0.18547(17) 0.0561 1.0000 Uani . . . . . .
O2 O 0.44479(3) 0.10867(10) -0.13326(8) 0.0318 1.0000 Uani . . . . . .
C21 C 0.39232(4) 0.15886(12) -0.15711(10) 0.0248 1.0000 Uani . . . . . .
C22 C 0.39079(4) 0.23933(12) -0.27945(10) 0.0271 1.0000 Uani . . . . . .
C23 C 0.40659(5) 0.15158(14) -0.39095(11) 0.0341 1.0000 Uani . . . . . .
O24 O 0.37229(4) 0.19721(14) -0.49126(8) 0.0528 1.0000 Uani D . . . . .
C25 C 0.33256(11) 0.2785(3) -0.44719(18) 0.0307 0.4360(19) Uani D . P 1 1 .
O26 O 0.33829(17) 0.2781(4) -0.3145(5) 0.0400 0.4360(19) Uani D . P 1 1 .
C27 C 0.27893(15) 0.2152(5) -0.4848(4) 0.0846 0.4360(19) Uani D . P 1 1 .
C28 C 0.33989(19) 0.4187(4) -0.4930(3) 0.0696 0.4360(19) Uani D . P 1 1 .
C125 C 0.32378(8) 0.2419(2) -0.43703(14) 0.0307 0.5640(19) Uani D . P 1 2 .
O126 O 0.33653(13) 0.2787(4) -0.3103(4) 0.0400 0.5640(19) Uani D . P 1 2 .
C127 C 0.28570(12) 0.1246(4) -0.4376(3) 0.0712 0.5640(19) Uani D . P 1 2 .
C128 C 0.30319(12) 0.3697(3) -0.5081(2) 0.0625 0.5640(19) Uani D . P 1 2 .
N31 N 0.5000 -0.24066(14) 0.0000 0.0253 1.0000 Uani S T . . . .
C32 C 0.45881(4) -0.33339(12) -0.06582(11) 0.0298 1.0000 Uani . . . . . .
C33 C 0.41641(5) -0.25689(14) -0.14325(13) 0.0385 1.0000 Uani . . . . . .
C34 C 0.37746(7) -0.35030(18) -0.20783(19) 0.0627 1.0000 Uani . . . . . .
C35 C 0.33450(6) -0.27510(19) -0.28299(15) 0.0511 1.0000 Uani . . . . . .
C36 C 0.47339(4) -0.14636(12) 0.09303(10) 0.0273 1.0000 Uani . . . . . .
C37 C 0.44524(6) -0.21991(15) 0.19664(13) 0.0454 1.0000 Uani . . . . . .
C38 C 0.42908(7) -0.11923(17) 0.29698(13) 0.0495 1.0000 Uani . . . . . .
C39 C 0.40155(11) -0.1875(2) 0.40373(18) 0.0793 1.0000 Uani . . . . . .
O41 O 0.48812(13) 0.5447(3) 0.6335(3) 0.0769 0.5000 Uani . U . 2 -1 .
C42 C 0.50881(14) 0.4374(4) 0.6097(3) 0.0393 0.5000 Uani D U . 2 -1 .
C43 C 0.5414(3) 0.3449(10) 0.6957(8) 0.0484 0.5000 Uani D U . 2 -1 .
O44 O 0.5000 0.37571(16) 0.5000 0.0453 1.0000 Uani S TU . 2 -1 .
C45 C 0.4683(2) 0.4515(5) 0.4082(4) 0.0547 0.5000 Uani D U . 2 -1 .
C46 C 0.4565(4) 0.3685(10) 0.2943(9) 0.0559 0.5000 Uani D U . 2 -1 .
H11 H 0.4299 0.3441 -0.0092 0.0439 1.0000 Uiso R . . . . .
H21 H 0.4631 0.1662 -0.0954 0.0469 1.0000 Uiso R . . . . .
H111 H 0.3349 0.2669 -0.0714 0.0268 1.0000 Uiso R . . . . .
H121 H 0.4052 0.1366 0.1048 0.0310 1.0000 Uiso R . . . . .
H132 H 0.3446 0.1849 0.2519 0.0385 1.0000 Uiso R . . . . .
H131 H 0.3355 0.3200 0.1669 0.0384 1.0000 Uiso R . . . . .
H171 H 0.2559 -0.0795 -0.0655 0.0820 1.0000 Uiso R . . . . .
H173 H 0.2614 0.0790 -0.0950 0.0800 1.0000 Uiso R . . . . .
H172 H 0.2154 0.0306 -0.0068 0.0805 1.0000 Uiso R . . . . .
H181 H 0.2911 -0.1616 0.1550 0.0820 1.0000 Uiso R . . . . .
H182 H 0.3002 -0.0482 0.2599 0.0834 1.0000 Uiso R . . . . .
H183 H 0.2433 -0.0740 0.2037 0.0824 1.0000 Uiso R . . . . .
H211 H 0.3702 0.0745 -0.1676 0.0300 1.0000 Uiso R . . . . .
H231 H 0.4427 0.1702 -0.4122 0.0425 1.0000 Uiso R . . . . .
H232 H 0.4004 0.0509 -0.3703 0.0416 1.0000 Uiso R . . . . .
H271 H 0.2512 0.2663 -0.4467 0.1256 0.4360(19) Uiso R . P 1 1 .
H273 H 0.2735 0.2157 -0.5743 0.1257 0.4360(19) Uiso R . P 1 1 .
H272 H 0.2781 0.1217 -0.4543 0.1262 0.4360(19) Uiso R . P 1 1 .
H22 H 0.3137 0.4816 -0.4625 0.1059 0.4360(19) Uiso R . P 1 1 .
H282 H 0.3740 0.4538 -0.4643 0.1062 0.4360(19) Uiso R . P 1 1 .
H283 H 0.3378 0.4189 -0.5840 0.1050 0.4360(19) Uiso R . P 1 1 .
H1271 H 0.2536 0.1525 -0.3970 0.1039 0.5640(19) Uiso R . P 1 2 .
H1273 H 0.2772 0.1010 -0.5250 0.1051 0.5640(19) Uiso R . P 1 2 .
H1272 H 0.3024 0.0453 -0.3955 0.1039 0.5640(19) Uiso R . P 1 2 .
H1281 H 0.2733 0.4106 -0.4678 0.0918 0.5640(19) Uiso R . P 1 2 .
H1282 H 0.3338 0.4316 -0.5098 0.0939 0.5640(19) Uiso R . P 1 2 .
H1283 H 0.2937 0.3473 -0.5943 0.0924 0.5640(19) Uiso R . P 1 2 .
H221 H 0.4132 0.3226 -0.2704 0.0315 1.0000 Uiso R . . . . .
H321 H 0.4783 -0.3951 -0.1167 0.0365 1.0000 Uiso R . . . . .
H322 H 0.4445 -0.3873 0.0011 0.0353 1.0000 Uiso R . . . . .
H332 H 0.4345 -0.2104 -0.2090 0.0517 1.0000 Uiso R . . . . .
H331 H 0.3978 -0.1909 -0.0913 0.0516 1.0000 Uiso R . . . . .
H342 H 0.3977 -0.4146 -0.2612 0.0798 1.0000 Uiso R . . . . .
H341 H 0.3630 -0.4168 -0.1504 0.0789 1.0000 Uiso R . . . . .
H352 H 0.3086 -0.3364 -0.3214 0.0776 1.0000 Uiso R . . . . .
H353 H 0.3508 -0.2311 -0.3503 0.0774 1.0000 Uiso R . . . . .
H351 H 0.3157 -0.2083 -0.2342 0.0796 1.0000 Uiso R . . . . .
H362 H 0.5004 -0.0857 0.1267 0.0320 1.0000 Uiso R . . . . .
H361 H 0.4481 -0.0915 0.0458 0.0324 1.0000 Uiso R . . . . .
H372 H 0.4688 -0.2892 0.2354 0.0546 1.0000 Uiso R . . . . .
H371 H 0.4136 -0.2706 0.1620 0.0583 1.0000 Uiso R . . . . .
H381 H 0.4664 -0.0885 0.3497 0.0558 1.0000 Uiso R . . . . .
H382 H 0.4076 -0.0418 0.2605 0.0607 1.0000 Uiso R . . . . .
H391 H 0.3854 -0.1159 0.4615 0.1198 1.0000 Uiso R . . . . .
H393 H 0.4272 -0.2498 0.4531 0.1194 1.0000 Uiso R . . . . .
H392 H 0.3706 -0.2501 0.3669 0.1192 1.0000 Uiso R . . . . .
H431 H 0.5696 0.3017 0.6544 0.0718 0.5000 Uiso R . . 2 -1 .
H432 H 0.5569 0.3987 0.7659 0.0713 0.5000 Uiso R . . 2 -1 .
H433 H 0.5188 0.2731 0.7257 0.0725 0.5000 Uiso R . . 2 -1 .
H452 H 0.4844 0.5394 0.3908 0.0651 0.5000 Uiso R . . 2 -1 .
H451 H 0.4353 0.4759 0.4478 0.0667 0.5000 Uiso R . . 2 -1 .
H462 H 0.4279 0.4131 0.2460 0.0822 0.5000 Uiso R . . 2 -1 .
H461 H 0.4878 0.3666 0.2455 0.0830 0.5000 Uiso R . . 2 -1 .
H463 H 0.4469 0.2754 0.3193 0.0824 0.5000 Uiso R . . 2 -1 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          5.14(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 . C11 . 1.4218(12) yes
O1 . H11 . 0.791 no
C11 . C12 . 1.5300(14) yes
C11 . C21 . 1.5251(14) yes
C11 . H111 . 0.959 no
C12 . C13 . 1.5153(15) yes
C12 . O16 . 1.4339(13) yes
C12 . H121 . 0.984 no
C13 . O14 . 1.4287(15) yes
C13 . H132 . 0.970 no
C13 . H131 . 0.991 no
O14 . C15 . 1.4294(17) yes
C15 . O16 . 1.4407(14) yes
C15 . C17 . 1.510(2) yes
C15 . C18 . 1.517(2) yes
C17 . H171 . 0.986 no
C17 . H173 . 0.974 no
C17 . H172 . 0.973 no
C18 . H181 . 0.959 no
C18 . H182 . 0.959 no
C18 . H183 . 0.950 no
O2 . C21 . 1.4214(12) yes
O2 . H21 . 0.818 no
C21 . C22 . 1.5186(14) yes
C21 . H211 . 0.991 no
C22 . C23 . 1.5263(15) yes
C22 . O26 . 1.411(5) yes
C22 . H221 . 0.985 no
C22 . C23 . 1.5263(15) yes
C22 . O126 . 1.444(4) yes
C22 . H221 . 0.985 no
C23 . O24 . 1.4193(15) yes
C23 . H231 . 0.962 no
C23 . H232 . 1.010 no
O24 . C25 . 1.370(3) yes
O24 . C125 . 1.439(2) yes
C25 . O26 . 1.417(5) yes
C25 . C27 . 1.522(4) yes
C25 . C28 . 1.454(4) yes
C27 . H271 . 0.959 no
C27 . H273 . 0.960 no
C27 . H272 . 0.960 no
C28 . H22 . 0.963 no
C28 . H282 . 0.962 no
C28 . H283 . 0.971 no
C125 . O126 . 1.423(4) yes
C125 . C127 . 1.484(3) yes
C125 . C128 . 1.529(3) yes
C127 . H1271 . 0.970 no
C127 . H1273 . 0.976 no
C127 . H1272 . 0.975 no
C128 . H1281 . 0.967 no
C128 . H1282 . 0.977 no
C128 . H1283 . 0.966 no
N31 . C36 3_655 1.5219(12) yes
N31 . C32 3_655 1.5213(12) yes
N31 . C32 . 1.5213(12) yes
N31 . C36 . 1.5219(12) yes
C32 . C33 . 1.5167(16) yes
C32 . H321 . 0.955 no
C32 . H322 . 0.965 no
C33 . C34 . 1.4827(18) yes
C33 . H332 . 0.962 no
C33 . H331 . 0.977 no
C34 . C35 . 1.508(2) yes
C34 . H342 . 0.997 no
C34 . H341 . 0.969 no
C35 . H352 . 0.960 no
C35 . H353 . 0.941 no
C35 . H351 . 0.964 no
C36 . C37 . 1.5138(15) yes
C36 . H362 . 0.957 no
C36 . H361 . 0.956 no
C37 . C38 . 1.5138(19) yes
C37 . H372 . 0.976 no
C37 . H371 . 0.994 no
C38 . C39 . 1.509(2) yes
C38 . H381 . 1.117 no
C38 . H382 . 0.994 no
C39 . H391 . 1.022 no
C39 . H393 . 1.015 no
C39 . H392 . 1.050 no
O41 . C42 . 1.192(5) yes
C42 . C43 . 1.502(6) yes
C42 . O44 . 1.325(4) yes
C43 . H431 . 0.947 no
C43 . H432 . 0.980 no
C43 . H433 . 0.960 no
O44 . C45 . 1.440(4) yes
C45 . C46 . 1.477(7) yes
C45 . H452 . 0.962 no
C45 . H451 . 0.976 no
C46 . H462 . 0.969 no
C46 . H461 . 0.962 no
C46 . H463 . 0.971 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C11 . O1 . H11 . 107.8 no
O1 . C11 . C12 . 109.16(8) yes
O1 . C11 . C21 . 113.37(8) yes
C12 . C11 . C21 . 111.49(8) yes
O1 . C11 . H111 . 107.8 no
C12 . C11 . H111 . 107.4 no
C21 . C11 . H111 . 107.4 no
C11 . C12 . C13 . 112.36(9) yes
C11 . C12 . O16 . 111.73(8) yes
C13 . C12 . O16 . 102.32(8) yes
C11 . C12 . H121 . 109.8 no
C13 . C12 . H121 . 111.3 no
O16 . C12 . H121 . 109.2 no
C12 . C13 . O14 . 102.31(9) yes
C12 . C13 . H132 . 111.2 no
O14 . C13 . H132 . 111.7 no
C12 . C13 . H131 . 112.4 no
O14 . C13 . H131 . 109.9 no
H132 . C13 . H131 . 109.3 no
C13 . O14 . C15 . 106.48(9) yes
O14 . C15 . O16 . 105.88(9) yes
O14 . C15 . C17 . 108.33(12) yes
O16 . C15 . C17 . 109.92(11) yes
O14 . C15 . C18 . 110.94(12) yes
O16 . C15 . C18 . 108.55(12) yes
C17 . C15 . C18 . 112.98(13) yes
C15 . O16 . C12 . 108.78(9) yes
C15 . C17 . H171 . 110.3 no
C15 . C17 . H173 . 109.4 no
H171 . C17 . H173 . 106.6 no
C15 . C17 . H172 . 109.6 no
H171 . C17 . H172 . 111.2 no
H173 . C17 . H172 . 109.7 no
C15 . C18 . H181 . 107.5 no
C15 . C18 . H182 . 109.5 no
H181 . C18 . H182 . 110.5 no
C15 . C18 . H183 . 108.9 no
H181 . C18 . H183 . 111.4 no
H182 . C18 . H183 . 108.9 no
C21 . O2 . H21 . 111.1 no
C11 . C21 . O2 . 113.46(8) yes
C11 . C21 . C22 . 112.99(8) yes
O2 . C21 . C22 . 108.69(8) yes
C11 . C21 . H211 . 107.4 no
O2 . C21 . H211 . 104.8 no
C22 . C21 . H211 . 109.2 no
C21 . C22 . C23 . 112.80(9) yes
C21 . C22 . O26 . 110.8(2) yes
C23 . C22 . O26 . 102.2(2) yes
C21 . C22 . H221 . 109.7 no
C23 . C22 . H221 . 111.3 no
O26 . C22 . H221 . 109.7 no
C21 . C22 . C23 . 112.80(9) yes
C21 . C22 . O126 . 108.82(16) yes
C23 . C22 . O126 . 104.01(18) yes
C21 . C22 . H221 . 109.7 no
C23 . C22 . H221 . 111.3 no
O126 . C22 . H221 . 109.9 no
C22 . C23 . O24 . 104.23(9) yes
C22 . C23 . H231 . 111.0 no
O24 . C23 . H231 . 108.5 no
C22 . C23 . H232 . 108.4 no
O24 . C23 . H232 . 111.6 no
H231 . C23 . H232 . 112.8 no
C23 . O24 . C25 . 110.52(10) yes
C23 . O24 . C125 . 106.95(9) yes
O24 . C25 . O26 . 107.10(6) yes
O24 . C25 . C27 . 109.40(6) yes
O26 . C25 . C27 . 108.47(6) yes
O24 . C25 . C28 . 108.29(6) yes
O26 . C25 . C28 . 109.24(6) yes
C27 . C25 . C28 . 114.12(6) yes
C25 . O26 . C22 . 108.9(2) yes
C25 . C27 . H271 . 109.6 no
C25 . C27 . H273 . 110.5 no
H271 . C27 . H273 . 110.0 no
C25 . C27 . H272 . 108.6 no
H271 . C27 . H272 . 108.3 no
H273 . C27 . H272 . 109.7 no
C25 . C28 . H22 . 112.0 no
C25 . C28 . H282 . 110.2 no
H22 . C28 . H282 . 106.6 no
C25 . C28 . H283 . 109.6 no
H22 . C28 . H283 . 109.1 no
H282 . C28 . H283 . 109.3 no
O24 . C125 . O126 . 107.07(6) yes
O24 . C125 . C127 . 109.19(6) yes
O126 . C125 . C127 . 108.46(6) yes
O24 . C125 . C128 . 108.63(6) yes
O126 . C125 . C128 . 109.21(6) yes
C127 . C125 . C128 . 114.06(6) yes
C22 . O126 . C125 . 109.09(19) yes
C125 . C127 . H1271 . 109.6 no
C125 . C127 . H1273 . 107.4 no
H1271 . C127 . H1273 . 109.7 no
C125 . C127 . H1272 . 109.3 no
H1271 . C127 . H1272 . 111.5 no
H1273 . C127 . H1272 . 109.3 no
C125 . C128 . H1281 . 111.4 no
C125 . C128 . H1282 . 104.5 no
H1281 . C128 . H1282 . 112.8 no
C125 . C128 . H1283 . 111.0 no
H1281 . C128 . H1283 . 110.3 no
H1282 . C128 . H1283 . 106.6 no
C36 3_655 N31 . C32 3_655 110.09(6) yes
C36 3_655 N31 . C32 . 111.15(6) yes
C32 3_655 N31 . C32 . 107.89(11) yes
C36 3_655 N31 . C36 . 106.50(11) yes
C32 3_655 N31 . C36 . 111.15(6) yes
C32 . N31 . C36 . 110.09(6) yes
N31 . C32 . C33 . 114.70(9) yes
N31 . C32 . H321 . 105.9 no
C33 . C32 . H321 . 111.2 no
N31 . C32 . H322 . 104.1 no
C33 . C32 . H322 . 113.0 no
H321 . C32 . H322 . 107.4 no
C32 . C33 . C34 . 113.34(10) yes
C32 . C33 . H332 . 106.4 no
C34 . C33 . H332 . 105.5 no
C32 . C33 . H331 . 110.6 no
C34 . C33 . H331 . 109.7 no
H332 . C33 . H331 . 111.1 no
C33 . C34 . C35 . 113.73(13) yes
C33 . C34 . H342 . 107.5 no
C35 . C34 . H342 . 111.6 no
C33 . C34 . H341 . 111.6 no
C35 . C34 . H341 . 112.0 no
H342 . C34 . H341 . 99.4 no
C34 . C35 . H352 . 113.0 no
C34 . C35 . H353 . 107.3 no
H352 . C35 . H353 . 105.1 no
C34 . C35 . H351 . 113.1 no
H352 . C35 . H351 . 107.6 no
H353 . C35 . H351 . 110.3 no
N31 . C36 . C37 . 115.26(9) yes
N31 . C36 . H362 . 106.7 no
C37 . C36 . H362 . 111.0 no
N31 . C36 . H361 . 106.8 no
C37 . C36 . H361 . 108.9 no
H362 . C36 . H361 . 107.9 no
C36 . C37 . C38 . 111.23(11) yes
C36 . C37 . H372 . 109.7 no
C38 . C37 . H372 . 108.5 no
C36 . C37 . H371 . 110.6 no
C38 . C37 . H371 . 110.2 no
H372 . C37 . H371 . 106.5 no
C37 . C38 . C39 . 113.43(13) yes
C37 . C38 . H381 . 106.4 no
C39 . C38 . H381 . 98.0 no
C37 . C38 . H382 . 111.3 no
C39 . C38 . H382 . 111.4 no
H381 . C38 . H382 . 115.6 no
C38 . C39 . H391 . 111.4 no
C38 . C39 . H393 . 110.4 no
H391 . C39 . H393 . 110.3 no
C38 . C39 . H392 . 109.0 no
H391 . C39 . H392 . 107.9 no
H393 . C39 . H392 . 107.5 no
O41 . C42 . C43 . 128.3(5) yes
O41 . C42 . O44 . 121.3(3) yes
C43 . C42 . O44 . 110.0(5) yes
C42 . C43 . H431 . 112.3 no
C42 . C43 . H432 . 110.1 no
H431 . C43 . H432 . 107.8 no
C42 . C43 . H433 . 108.4 no
H431 . C43 . H433 . 107.6 no
H432 . C43 . H433 . 110.6 no
C42 . O44 . C45 . 116.2(2) yes
O44 . C45 . C46 . 111.9(5) yes
O44 . C45 . H452 . 110.7 no
C46 . C45 . H452 . 113.1 no
O44 . C45 . H451 . 106.8 no
C46 . C45 . H451 . 109.9 no
H452 . C45 . H451 . 104.2 no
C45 . C46 . H462 . 108.5 no
C45 . C46 . H461 . 108.2 no
H462 . C46 . H461 . 109.1 no
C45 . C46 . H463 . 108.7 no
H462 . C46 . H463 . 111.7 no
H461 . C46 . H463 . 110.5 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C36 . H362 . O2 3_655 156.39 0.957 2.330 3.229(4) yes
C37 . H372 . O41 3_646 166.84 0.976 2.364 3.321(4) yes
C43 . H431 . O24 3_655 163.99 0.947 2.528 3.449(4) yes
C46 3_656 H431 . O24 3_655 164.5 1.085 2.528 3.585(4) yes
O41 3_656 H452 . C45 . 122.0 0.750 0.962 1.501(4) yes
C45 . H451 . C28 1_556 151.12 0.976 2.568 3.455(4) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 19/12/14 at 10:04:00
#
#LIST     12                                                                    
BLOCK SCALE X'S U'S 
CONT ENANTIO 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
REM EQUIV PART(-2002,OCC) PART(-2003,OCC) 
REM WEIGHT -1 PART(-2003,OCC) 
RIDE  C(25,U'S) C(125,U'S) 
RIDE  O(26,U'S) O(126,U'S) 
RIDE O   (   1,X'S) H   (  11,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 173,X'S) H   ( 172,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) H   ( 183,X'S) 
RIDE O   (   2,X'S) H   (  21,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 273,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   (  22,X'S) H   ( 282,X'S) H   ( 283,X'S) 
RIDE C   ( 127,X'S) H   (1271,X'S) H   (1273,X'S) H   (1272,X'S) 
RIDE C   ( 128,X'S) H   (1281,X'S) H   (1282,X'S) H   (1283,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 332,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 342,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 353,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 372,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 393,X'S) H   ( 392,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) H   ( 433,X'S) 
RIDE C   (  45,X'S) H   ( 452,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 462,X'S) H   ( 461,X'S) H   ( 463,X'S) 
REM RIDE C   (  45,X'S) H   ( 453,X'S) H   ( 452,X'S) H   ( 451,X'S) 
REM RIDE C   ( 146,X'S) H   (1461,X'S) H   (1462,X'S) H   (1463,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 19/12/14 at 10:04:00
#
#LIST     16                                                                    
REM SAME  O(44)  C(45)  C(46)  C(146)  AND 
REM CONT  O(44)  C(45)  C(146)  C(46) 
REM SIMU  0.01   O(44)  C(45)  C(46)  C(146)  AND 
REM CONT  O(44)  C(45)  C(146)  C(46) 
REM DELU  0.01   O(44)  C(45)  C(46)  C(146)  AND 
REM CONT  O(44)  C(45)  C(146)  C(46) 
DIST  0,0.01 = MEAN 
CONT  C(42) TO  C(43)  C(45) TO  C(46) 
VIBR .0, 0.00200 = O(41) TO C(42) 
VIBR .0, 0.00200 = C(42) TO O(44) 
VIBR .0, 0.00200 = C(42) TO C(43) 
VIBR .0, 0.00500 = O(44) TO O(41) 
VIBR .0, 0.00500 = C(43) TO O(41) 
VIBR .0, 0.00500 = C(43) TO O(44) 
U(IJ) .0, 0.08000 = O(41) TO C(42) 
U(IJ) .0, 0.04000 = C(42) TO O(44) 
U(IJ) .0, 0.08000 = C(42) TO C(43) 
U(IJ) .0, 0.08000 = C(46) TO C(45) 
SAME  O(24)  C(25)  O(26)  C(27)  C(28)  AND 
CONT  O(26)  C(25)  O(24)  C(28)  C(27)  AND 
CONT  O(24)  C(125)  O(126)  C(127)  C(128)  AND 
CONT  O(126)  C(125)  O(24)  C(128)  C(127) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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_2g
_database_code_depnum_ccdc_archive 'CCDC 1401771'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             13-04-25
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 064ggke01
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_refine_special_details          
; 
On initial refinement there was a poor agreement 
between the observed and calculated structure factor
amplitudes.  Examination of the data and model using 
ROTAX (R. I. Cooper, R. O. Gould, S. Parsons & 
D. J. Watkin, J. Appl. Cryst. (2002), 35, 168-174) 
suggested the crystal was a pseudo-merohedral 
twin by 180.0° rotation about the -1  1  0 direct 
lattice direction: 

[  -0.001   -0.999    0.000]
[  -1.001    0.001    0.000]
[   0.000    0.000   -1.000]

Inclusion of this twin component in the refinement
gave a much better agreement and the twin scale 
factor indicated the crystal comprised a two component 
twin in a 60:40 ratio.
;

_cell_length_a                   18.6017(3)
_cell_length_b                   18.6158(3)
_cell_length_c                   19.1084(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6616.96(18)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a '
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
x+1/2,-y+1/2,-z
-x+1/2,y+1/2,z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C70 H160 F2.50 N2.50 O10 
# Dc =      2.50 Fooo =   2240.00 Mu =      1.70 M =   1244.55
# Found Formula = C28 H64 F1 N1 O4 
# Dc =      1.00 FOOO =   2240.00 Mu =      0.68 M =    497.82

_chemical_formula_sum            'C28 H64 F1 N1 O4'
_chemical_formula_moiety         'C16 H36 N, 2(C6 H14 O2), F'
_chemical_compound_source        .
_chemical_formula_weight         497.82


_cell_measurement_reflns_used    7082
_cell_measurement_theta_min      5
_cell_measurement_theta_max      26
_cell_measurement_temperature    150

_exptl_crystal_description       prism
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.080
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_max          0.490

_exptl_crystal_density_diffrn    0.999
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2240
_exptl_absorpt_coefficient_mu    0.068

# Sheldrick geometric approximatio 0.99 0.99 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_T_max  0.99
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            96568
_reflns_number_total             6466
_diffrn_reflns_av_R_equivalents  0.022
# Number of reflections without Friedels Law is 12342 
# Number of reflections with Friedels Law is 6466 
# Theoretical number of reflections is about 6518 


_diffrn_reflns_theta_min         5.115
_diffrn_reflns_theta_max         26.020
_diffrn_measured_fraction_theta_max 0.991

_diffrn_reflns_theta_full        26.020
_diffrn_measured_fraction_theta_full 0.991


_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_reflns_limit_h_min              0
_reflns_limit_h_max              22
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              -23
_reflns_limit_l_max              0

_oxford_diffrn_Wilson_B_factor   3.69
_oxford_diffrn_Wilson_scale      20.77

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.14
_refine_diff_density_max         0.20


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         6466
_refine_ls_number_restraints     0
_refine_ls_number_parameters     308
_oxford_refine_ls_R_factor_ref   0.0558
_refine_ls_wR_factor_ref         0.1038
_refine_ls_goodness_of_fit_ref   0.9864
_refine_ls_shift/su_max          0.0003659
_refine_ls_shift/su_mean         0.0000486


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6466
_refine_ls_R_factor_all          0.0558
_refine_ls_wR_factor_all         0.1038

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5368
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_gt          0.0979

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 1.37P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
O11 O 0.56788(7) 0.72138(8) 0.30033(6) 0.0513 1.0000 Uani . . . . . .
O12 O 0.54606(7) 0.65605(7) 0.44062(6) 0.0501 1.0000 Uani . . . . . .
C13 C 0.62234(10) 0.71496(12) 0.35288(9) 0.0477 1.0000 Uani . . . . . .
C14 C 0.62025(14) 0.78300(13) 0.39782(11) 0.0615 1.0000 Uani . . . . . .
C15 C 0.69275(13) 0.71186(18) 0.31307(11) 0.0764 1.0000 Uani . . . . . .
C16 C 0.60849(10) 0.64646(12) 0.39733(9) 0.0471 1.0000 Uani . . . . . .
C17 C 0.59632(15) 0.58091(14) 0.35078(12) 0.0698 1.0000 Uani . . . . . .
C18 C 0.66914(13) 0.63180(14) 0.44888(11) 0.0663 1.0000 Uani . . . . . .
O21 O 0.37360(8) 0.81345(7) 0.29469(6) 0.0539 1.0000 Uani . . . . . .
O22 O 0.41449(8) 0.83041(7) 0.44283(6) 0.0519 1.0000 Uani . . . . . .
C23 C 0.33862(10) 0.86068(10) 0.34234(9) 0.0412 1.0000 Uani . . . . . .
C24 C 0.27629(13) 0.82080(13) 0.37657(12) 0.0628 1.0000 Uani . . . . . .
C25 C 0.30923(14) 0.92073(12) 0.29649(10) 0.0597 1.0000 Uani . . . . . .
C26 C 0.39302(11) 0.88796(10) 0.39833(9) 0.0440 1.0000 Uani . . . . . .
C27 C 0.46051(14) 0.91905(16) 0.36375(13) 0.0755 1.0000 Uani . . . . . .
C28 C 0.35884(15) 0.94266(12) 0.44785(11) 0.0673 1.0000 Uani . . . . . .
F1 F 0.44450(6) 0.71655(6) 0.36576(6) 0.0533 1.0000 Uani . . . . . .
N31 N 0.48187(7) 0.73666(7) 0.62204(6) 0.0265 1.0000 Uani . . . . . .
C32 C 0.54096(8) 0.77609(9) 0.58261(7) 0.0293 1.0000 Uani . . . . . .
C33 C 0.59799(9) 0.81016(10) 0.62899(8) 0.0366 1.0000 Uani . . . . . .
C34 C 0.65669(10) 0.84451(10) 0.58584(9) 0.0389 1.0000 Uani . . . . . .
C35 C 0.71542(11) 0.87771(11) 0.63084(10) 0.0455 1.0000 Uani . . . . . .
C36 C 0.44411(9) 0.78604(9) 0.67381(7) 0.0295 1.0000 Uani . . . . . .
C37 C 0.41070(10) 0.85332(9) 0.64273(8) 0.0375 1.0000 Uani . . . . . .
C38 C 0.37834(11) 0.89881(10) 0.70092(9) 0.0449 1.0000 Uani . . . . . .
C39 C 0.34221(12) 0.96574(12) 0.67396(12) 0.0595 1.0000 Uani . . . . . .
C40 C 0.51289(9) 0.67500(8) 0.66476(7) 0.0295 1.0000 Uani . . . . . .
C41 C 0.55143(10) 0.61832(9) 0.62258(8) 0.0372 1.0000 Uani . . . . . .
C42 C 0.57587(13) 0.55634(11) 0.66721(10) 0.0540 1.0000 Uani . . . . . .
C43 C 0.61050(15) 0.49724(12) 0.62429(12) 0.0672 1.0000 Uani . . . . . .
C44 C 0.42948(8) 0.70879(9) 0.56737(7) 0.0287 1.0000 Uani . . . . . .
C45 C 0.37106(9) 0.66015(10) 0.59495(8) 0.0359 1.0000 Uani . . . . . .
C46 C 0.32062(11) 0.63635(11) 0.53737(10) 0.0461 1.0000 Uani . . . . . .
C47 C 0.26771(11) 0.58014(11) 0.56125(11) 0.0509 1.0000 Uani . . . . . .
H253 H 0.2823 0.9546 0.3239 0.0882 1.0000 Uiso R . . . . .
H252 H 0.3491 0.9470 0.2757 0.0894 1.0000 Uiso R . . . . .
H251 H 0.2792 0.9011 0.2605 0.0890 1.0000 Uiso R . . . . .
H241 H 0.2482 0.8543 0.4056 0.0934 1.0000 Uiso R . . . . .
H242 H 0.2463 0.7985 0.3411 0.0942 1.0000 Uiso R . . . . .
H243 H 0.2952 0.7846 0.4089 0.0925 1.0000 Uiso R . . . . .
H281 H 0.3939 0.9563 0.4844 0.0996 1.0000 Uiso R . . . . .
H282 H 0.3464 0.9858 0.4210 0.1003 1.0000 Uiso R . . . . .
H283 H 0.3141 0.9226 0.4689 0.1005 1.0000 Uiso R . . . . .
H273 H 0.4942 0.9343 0.3979 0.1127 1.0000 Uiso R . . . . .
H272 H 0.4459 0.9586 0.3339 0.1119 1.0000 Uiso R . . . . .
H271 H 0.4817 0.8829 0.3336 0.1129 1.0000 Uiso R . . . . .
H152 H 0.6963 0.7557 0.2818 0.1138 1.0000 Uiso R . . . . .
H153 H 0.7322 0.7111 0.3483 0.1132 1.0000 Uiso R . . . . .
H151 H 0.6932 0.6670 0.2838 0.1141 1.0000 Uiso R . . . . .
H142 H 0.6289 0.8272 0.3679 0.0912 1.0000 Uiso R . . . . .
H141 H 0.6585 0.7811 0.4327 0.0906 1.0000 Uiso R . . . . .
H143 H 0.5725 0.7851 0.4214 0.0911 1.0000 Uiso R . . . . .
H181 H 0.7114 0.6243 0.4234 0.0984 1.0000 Uiso R . . . . .
H183 H 0.6751 0.6721 0.4788 0.0985 1.0000 Uiso R . . . . .
H182 H 0.6569 0.5898 0.4757 0.0991 1.0000 Uiso R . . . . .
H173 H 0.6391 0.5717 0.3219 0.1019 1.0000 Uiso R . . . . .
H171 H 0.5848 0.5399 0.3801 0.1049 1.0000 Uiso R . . . . .
H172 H 0.5560 0.5910 0.3202 0.1046 1.0000 Uiso R . . . . .
H401 H 0.5443 0.6976 0.6980 0.0346 1.0000 Uiso R . . . . .
H402 H 0.4734 0.6541 0.6884 0.0345 1.0000 Uiso R . . . . .
H411 H 0.5933 0.6402 0.6022 0.0465 1.0000 Uiso R . . . . .
H412 H 0.5214 0.6010 0.5856 0.0460 1.0000 Uiso R . . . . .
H421 H 0.6111 0.5752 0.7029 0.0653 1.0000 Uiso R . . . . .
H422 H 0.5347 0.5374 0.6920 0.0665 1.0000 Uiso R . . . . .
H431 H 0.6260 0.4566 0.6545 0.1004 1.0000 Uiso R . . . . .
H433 H 0.6531 0.5160 0.6005 0.1016 1.0000 Uiso R . . . . .
H432 H 0.5764 0.4782 0.5908 0.1009 1.0000 Uiso R . . . . .
H321 H 0.5630 0.7430 0.5502 0.0333 1.0000 Uiso R . . . . .
H322 H 0.5167 0.8112 0.5557 0.0340 1.0000 Uiso R . . . . .
H331 H 0.6191 0.7730 0.6591 0.0462 1.0000 Uiso R . . . . .
H332 H 0.5768 0.8464 0.6582 0.0453 1.0000 Uiso R . . . . .
H341 H 0.6792 0.8082 0.5547 0.0476 1.0000 Uiso R . . . . .
H342 H 0.6345 0.8803 0.5565 0.0490 1.0000 Uiso R . . . . .
H351 H 0.7479 0.9054 0.6013 0.0665 1.0000 Uiso R . . . . .
H352 H 0.7405 0.8407 0.6547 0.0674 1.0000 Uiso R . . . . .
H353 H 0.6949 0.9107 0.6662 0.0669 1.0000 Uiso R . . . . .
H441 H 0.4554 0.6829 0.5334 0.0320 1.0000 Uiso R . . . . .
H442 H 0.4081 0.7512 0.5461 0.0327 1.0000 Uiso R . . . . .
H451 H 0.3922 0.6178 0.6148 0.0452 1.0000 Uiso R . . . . .
H452 H 0.3449 0.6835 0.6310 0.0447 1.0000 Uiso R . . . . .
H461 H 0.3497 0.6158 0.5014 0.0573 1.0000 Uiso R . . . . .
H462 H 0.2964 0.6761 0.5181 0.0583 1.0000 Uiso R . . . . .
H473 H 0.2346 0.5669 0.5245 0.0761 1.0000 Uiso R . . . . .
H472 H 0.2929 0.5372 0.5772 0.0764 1.0000 Uiso R . . . . .
H471 H 0.2410 0.5983 0.6030 0.0752 1.0000 Uiso R . . . . .
H362 H 0.4784 0.8000 0.7091 0.0347 1.0000 Uiso R . . . . .
H361 H 0.4086 0.7572 0.6972 0.0364 1.0000 Uiso R . . . . .
H372 H 0.4477 0.8820 0.6189 0.0453 1.0000 Uiso R . . . . .
H371 H 0.3727 0.8406 0.6095 0.0463 1.0000 Uiso R . . . . .
H382 H 0.4161 0.9120 0.7335 0.0554 1.0000 Uiso R . . . . .
H381 H 0.3440 0.8690 0.7247 0.0546 1.0000 Uiso R . . . . .
H393 H 0.3189 0.9945 0.7111 0.0884 1.0000 Uiso R . . . . .
H391 H 0.3785 0.9965 0.6506 0.0891 1.0000 Uiso R . . . . .
H392 H 0.3059 0.9529 0.6400 0.0890 1.0000 Uiso R . . . . .
H221 H 0.4255 0.7946 0.4187 0.0776 1.0000 Uiso R . . . . .
H121 H 0.5111 0.6693 0.4134 0.0755 1.0000 Uiso R . . . . .
H211 H 0.3955 0.7806 0.3148 0.0810 1.0000 Uiso R . . . . .
H111 H 0.5272 0.7217 0.3237 0.0768 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.3448(3)

loop_
_oxford_twin_element_scale_factors
0.6037(9)
0.3963(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O11 . C13 . 1.431(2) yes
O11 . H111 . 0.879 no
O12 . C16 . 1.437(2) yes
O12 . H121 . 0.869 no
C13 . C14 . 1.531(3) yes
C13 . C15 . 1.516(3) yes
C13 . C16 . 1.554(3) yes
C14 . H142 . 1.014 no
C14 . H141 . 0.976 no
C14 . H143 . 0.997 no
C15 . H152 . 1.013 no
C15 . H153 . 0.997 no
C15 . H151 . 1.004 no
C16 . C17 . 1.527(3) yes
C16 . C18 . 1.522(3) yes
C17 . H173 . 0.984 no
C17 . H171 . 0.971 no
C17 . H172 . 0.969 no
C18 . H181 . 0.935 no
C18 . H183 . 0.949 no
C18 . H182 . 0.962 no
O21 . C23 . 1.423(2) yes
O21 . H211 . 0.829 no
O22 . C26 . 1.425(2) yes
O22 . H221 . 0.836 no
C23 . C24 . 1.524(3) yes
C23 . C25 . 1.522(3) yes
C23 . C26 . 1.558(3) yes
C24 . H241 . 0.985 no
C24 . H242 . 0.971 no
C24 . H243 . 0.980 no
C25 . H253 . 0.959 no
C25 . H252 . 0.974 no
C25 . H251 . 0.959 no
C26 . C27 . 1.532(3) yes
C26 . C28 . 1.528(3) yes
C27 . H273 . 0.948 no
C27 . H272 . 0.970 no
C27 . H271 . 0.971 no
C28 . H281 . 0.989 no
C28 . H282 . 0.980 no
C28 . H283 . 0.997 no
N31 . C32 . 1.5216(19) yes
N31 . C36 . 1.5221(18) yes
N31 . C40 . 1.5222(19) yes
N31 . C44 . 1.5201(18) yes
C32 . C33 . 1.521(2) yes
C32 . H321 . 0.966 no
C32 . H322 . 0.946 no
C33 . C34 . 1.510(2) yes
C33 . H331 . 0.982 no
C33 . H332 . 0.960 no
C34 . C35 . 1.521(2) yes
C34 . H341 . 0.994 no
C34 . H342 . 0.964 no
C35 . H351 . 0.974 no
C35 . H352 . 0.949 no
C35 . H353 . 0.990 no
C36 . C37 . 1.519(2) yes
C36 . H362 . 0.963 no
C36 . H361 . 0.962 no
C37 . C38 . 1.522(2) yes
C37 . H372 . 0.983 no
C37 . H371 . 0.980 no
C38 . C39 . 1.507(3) yes
C38 . H382 . 0.971 no
C38 . H381 . 0.961 no
C39 . H393 . 0.988 no
C39 . H391 . 0.991 no
C39 . H392 . 0.967 no
C40 . C41 . 1.509(2) yes
C40 . H401 . 0.959 no
C40 . H402 . 0.946 no
C41 . C42 . 1.505(2) yes
C41 . H411 . 0.961 no
C41 . H412 . 0.957 no
C42 . C43 . 1.516(3) yes
C42 . H421 . 1.009 no
C42 . H422 . 0.967 no
C43 . H431 . 0.994 no
C43 . H433 . 0.978 no
C43 . H432 . 0.969 no
C44 . C45 . 1.509(2) yes
C44 . H441 . 0.941 no
C44 . H442 . 0.973 no
C45 . C46 . 1.512(2) yes
C45 . H451 . 0.959 no
C45 . H452 . 0.949 no
C46 . C47 . 1.507(3) yes
C46 . H461 . 0.954 no
C46 . H462 . 0.942 no
C47 . H473 . 0.966 no
C47 . H472 . 0.975 no
C47 . H471 . 0.998 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C13 . O11 . H111 . 104.7 no
C16 . O12 . H121 . 107.2 no
O11 . C13 . C14 . 107.84(17) yes
O11 . C13 . C15 . 105.23(14) yes
C14 . C13 . C15 . 109.6(2) yes
O11 . C13 . C16 . 109.55(16) yes
C14 . C13 . C16 . 111.61(15) yes
C15 . C13 . C16 . 112.74(19) yes
C13 . C14 . H142 . 110.6 no
C13 . C14 . H141 . 109.6 no
H142 . C14 . H141 . 107.4 no
C13 . C14 . H143 . 107.9 no
H142 . C14 . H143 . 111.4 no
H141 . C14 . H143 . 110.0 no
C13 . C15 . H152 . 108.7 no
C13 . C15 . H153 . 107.4 no
H152 . C15 . H153 . 111.2 no
C13 . C15 . H151 . 108.5 no
H152 . C15 . H151 . 109.9 no
H153 . C15 . H151 . 111.0 no
C13 . C16 . O12 . 110.29(15) yes
C13 . C16 . C17 . 111.23(15) yes
O12 . C16 . C17 . 108.35(18) yes
C13 . C16 . C18 . 112.21(18) yes
O12 . C16 . C18 . 104.40(14) yes
C17 . C16 . C18 . 110.09(18) yes
C16 . C17 . H173 . 110.2 no
C16 . C17 . H171 . 108.9 no
H173 . C17 . H171 . 111.4 no
C16 . C17 . H172 . 108.1 no
H173 . C17 . H172 . 108.7 no
H171 . C17 . H172 . 109.3 no
C16 . C18 . H181 . 108.3 no
C16 . C18 . H183 . 109.5 no
H181 . C18 . H183 . 109.5 no
C16 . C18 . H182 . 108.4 no
H181 . C18 . H182 . 110.7 no
H183 . C18 . H182 . 110.4 no
C23 . O21 . H211 . 112.5 no
C26 . O22 . H221 . 109.8 no
O21 . C23 . C24 . 108.76(17) yes
O21 . C23 . C25 . 104.46(14) yes
C24 . C23 . C25 . 109.36(18) yes
O21 . C23 . C26 . 110.11(15) yes
C24 . C23 . C26 . 110.99(15) yes
C25 . C23 . C26 . 112.91(16) yes
C23 . C24 . H241 . 109.7 no
C23 . C24 . H242 . 110.3 no
H241 . C24 . H242 . 111.1 no
C23 . C24 . H243 . 109.4 no
H241 . C24 . H243 . 105.8 no
H242 . C24 . H243 . 110.5 no
C23 . C25 . H253 . 110.8 no
C23 . C25 . H252 . 109.2 no
H253 . C25 . H252 . 106.9 no
C23 . C25 . H251 . 110.0 no
H253 . C25 . H251 . 109.7 no
H252 . C25 . H251 . 110.1 no
C23 . C26 . O22 . 110.29(15) yes
C23 . C26 . C27 . 111.05(15) yes
O22 . C26 . C27 . 108.16(18) yes
C23 . C26 . C28 . 111.85(17) yes
O22 . C26 . C28 . 104.36(14) yes
C27 . C26 . C28 . 110.9(2) yes
C26 . C27 . H273 . 111.0 no
C26 . C27 . H272 . 108.1 no
H273 . C27 . H272 . 111.2 no
C26 . C27 . H271 . 109.1 no
H273 . C27 . H271 . 110.4 no
H272 . C27 . H271 . 106.9 no
C26 . C28 . H281 . 109.5 no
C26 . C28 . H282 . 108.6 no
H281 . C28 . H282 . 108.4 no
C26 . C28 . H283 . 110.3 no
H281 . C28 . H283 . 111.2 no
H282 . C28 . H283 . 108.7 no
C32 . N31 . C36 . 111.34(12) yes
C32 . N31 . C40 . 110.82(11) yes
C36 . N31 . C40 . 106.37(10) yes
C32 . N31 . C44 . 106.71(10) yes
C36 . N31 . C44 . 110.92(11) yes
C40 . N31 . C44 . 110.74(12) yes
N31 . C32 . C33 . 114.61(11) yes
N31 . C32 . H321 . 108.5 no
C33 . C32 . H321 . 110.1 no
N31 . C32 . H322 . 105.0 no
C33 . C32 . H322 . 111.1 no
H321 . C32 . H322 . 107.2 no
C32 . C33 . C34 . 111.27(12) yes
C32 . C33 . H331 . 109.1 no
C34 . C33 . H331 . 109.3 no
C32 . C33 . H332 . 110.2 no
C34 . C33 . H332 . 108.4 no
H331 . C33 . H332 . 108.6 no
C33 . C34 . C35 . 112.49(13) yes
C33 . C34 . H341 . 110.1 no
C35 . C34 . H341 . 108.2 no
C33 . C34 . H342 . 107.5 no
C35 . C34 . H342 . 110.9 no
H341 . C34 . H342 . 107.6 no
C34 . C35 . H351 . 109.4 no
C34 . C35 . H352 . 109.3 no
H351 . C35 . H352 . 110.9 no
C34 . C35 . H353 . 111.2 no
H351 . C35 . H353 . 107.9 no
H352 . C35 . H353 . 108.1 no
N31 . C36 . C37 . 115.63(11) yes
N31 . C36 . H362 . 108.2 no
C37 . C36 . H362 . 108.8 no
N31 . C36 . H361 . 106.4 no
C37 . C36 . H361 . 111.2 no
H362 . C36 . H361 . 106.2 no
C36 . C37 . C38 . 109.57(13) yes
C36 . C37 . H372 . 110.0 no
C38 . C37 . H372 . 108.2 no
C36 . C37 . H371 . 110.4 no
C38 . C37 . H371 . 108.8 no
H372 . C37 . H371 . 109.8 no
C37 . C38 . C39 . 112.77(16) yes
C37 . C38 . H382 . 108.8 no
C39 . C38 . H382 . 109.5 no
C37 . C38 . H381 . 106.6 no
C39 . C38 . H381 . 110.1 no
H382 . C38 . H381 . 109.0 no
C38 . C39 . H393 . 113.5 no
C38 . C39 . H391 . 109.1 no
H393 . C39 . H391 . 108.1 no
C38 . C39 . H392 . 109.6 no
H393 . C39 . H392 . 108.0 no
H391 . C39 . H392 . 108.5 no
N31 . C40 . C41 . 114.90(11) yes
N31 . C40 . H401 . 104.7 no
C41 . C40 . H401 . 111.8 no
N31 . C40 . H402 . 105.8 no
C41 . C40 . H402 . 109.6 no
H401 . C40 . H402 . 109.7 no
C40 . C41 . C42 . 112.14(13) yes
C40 . C41 . H411 . 107.8 no
C42 . C41 . H411 . 108.0 no
C40 . C41 . H412 . 110.7 no
C42 . C41 . H412 . 109.6 no
H411 . C41 . H412 . 108.5 no
C41 . C42 . C43 . 112.23(15) yes
C41 . C42 . H421 . 108.2 no
C43 . C42 . H421 . 110.1 no
C41 . C42 . H422 . 108.6 no
C43 . C42 . H422 . 109.7 no
H421 . C42 . H422 . 108.0 no
C42 . C43 . H431 . 111.1 no
C42 . C43 . H433 . 109.6 no
H431 . C43 . H433 . 107.9 no
C42 . C43 . H432 . 110.2 no
H431 . C43 . H432 . 107.2 no
H433 . C43 . H432 . 110.7 no
N31 . C44 . C45 . 115.24(12) yes
N31 . C44 . H441 . 108.7 no
C45 . C44 . H441 . 107.6 no
N31 . C44 . H442 . 105.8 no
C45 . C44 . H442 . 109.8 no
H441 . C44 . H442 . 109.7 no
C44 . C45 . C46 . 111.61(13) yes
C44 . C45 . H451 . 109.6 no
C46 . C45 . H451 . 107.6 no
C44 . C45 . H452 . 110.3 no
C46 . C45 . H452 . 110.2 no
H451 . C45 . H452 . 107.5 no
C45 . C46 . C47 . 112.84(15) yes
C45 . C46 . H461 . 106.9 no
C47 . C46 . H461 . 108.0 no
C45 . C46 . H462 . 110.5 no
C47 . C46 . H462 . 110.6 no
H461 . C46 . H462 . 107.8 no
C46 . C47 . H473 . 111.9 no
C46 . C47 . H472 . 110.5 no
H473 . C47 . H472 . 108.9 no
C46 . C47 . H471 . 109.3 no
H473 . C47 . H471 . 110.5 no
H472 . C47 . H471 . 105.5 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C40 . H401 . O11 3_565 152.36 0.959 2.509 3.388(3) yes
C44 . H441 . O12 . 159.71 0.941 2.498 3.396(3) yes
C44 . H442 . O22 . 143.06 0.973 2.466 3.297(3) yes
C36 . H362 . O11 3_565 155.00 0.963 2.443 3.341(3) yes
C36 . H361 . O21 3_565 149.75 0.962 2.371 3.238(3) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 25/04/13 at 19:50:00
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
RIDE O   (  11,X'S) H   ( 111,X'S) 
RIDE O   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 142,X'S) H   ( 141,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 152,X'S) H   ( 153,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 173,X'S) H   ( 171,X'S) H   ( 172,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 183,X'S) H   ( 182,X'S) 
RIDE O   (  21,X'S) H   ( 211,X'S) 
RIDE O   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 253,X'S) H   ( 252,X'S) H   ( 251,X'S) 
RIDE C   (  27,X'S) H   ( 273,X'S) H   ( 272,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) H   ( 353,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 372,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 382,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 393,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 433,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) 
RIDE C   (  47,X'S) H   ( 473,X'S) H   ( 472,X'S) H   ( 471,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 25/04/13 at 19:50:00
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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_2h
_database_code_depnum_ccdc_archive 'CCDC 1401772'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             2015-04-20
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title 039lp14
_chemical_name_systematic        .
_chemical_melting_point          '433 K'

_cell_length_a                   10.68590(10)
_cell_length_b                   12.65280(10)
_cell_length_c                   34.7970(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4704.78(7)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21 '
_symmetry_space_group_name_Hall  'P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x+1/2,-y,z+1/2
x+1/2,-y+1/2,-z
-x,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C56 H64 F1 N1 O4 
# Dc =      1.18 Fooo =   1792.00 Mu =      5.92 M =    834.13
# Found Formula = C56 H64 F1 N1 O4 
# Dc =      1.18 FOOO =   1792.00 Mu =      5.92 M =    834.13

_chemical_formula_sum            'C56 H64 F1 N1 O4'
_chemical_formula_moiety         'C56 H64 F1 N1 O4'
_chemical_compound_source        .
_chemical_formula_weight         834.13


_cell_measurement_reflns_used    28738
_cell_measurement_theta_min      4
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.18
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.20

_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1792
_exptl_absorpt_coefficient_mu    0.592

# Sheldrick geometric approximatio 0.89 0.90 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_T_max  0.90
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            52468
_reflns_number_total             9770
_diffrn_reflns_av_R_equivalents  0.026
# Number of reflections without Friedels Law is 9770 
# Number of reflections with Friedels Law is 5476 
# Theoretical number of reflections is about 4921 


_diffrn_reflns_theta_min         3.717
_diffrn_reflns_theta_max         76.149
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        76.149
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       43
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              43

_oxford_diffrn_Wilson_B_factor   2.41
_oxford_diffrn_Wilson_scale      0.06

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.14
_refine_diff_density_max         0.15


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         9732
_refine_ls_number_restraints     0
_refine_ls_number_parameters     560
_oxford_refine_ls_R_factor_ref   0.0272
_refine_ls_wR_factor_ref         0.0670
_refine_ls_goodness_of_fit_ref   0.9641
_refine_ls_shift/su_max          0.0014078
_refine_ls_shift/su_mean         0.0000960


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        9732
_refine_ls_R_factor_all          0.0272
_refine_ls_wR_factor_all         0.0670

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                9487
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_gt          0.0662

_refine_ls_abs_structure_Flack   -0.07(7)
_refine_ls_abs_structure_details 'Flack (1983), 4294 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 0.68P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
O1 O 0.80980(8) 0.56718(6) 0.61230(2) 0.0302 1.0000 Uani . . . . . .
O2 O 0.58394(7) 0.79160(6) 0.57334(2) 0.0277 1.0000 Uani . . . . . .
O3 O 0.39222(7) 0.82134(6) 0.50011(2) 0.0262 1.0000 Uani . . . . . .
O4 O 0.91297(9) 0.54106(7) 0.68124(3) 0.0415 1.0000 Uani . . . . . .
C10 C 0.85204(10) 0.47193(8) 0.59962(3) 0.0247 1.0000 Uani . . . . . .
C11 C 0.90590(11) 0.46256(8) 0.56248(3) 0.0277 1.0000 Uani . . . . . .
C12 C 0.95132(10) 0.36779(8) 0.55023(3) 0.0269 1.0000 Uani . . . . . .
C13 C 0.94909(9) 0.27766(8) 0.57447(3) 0.0243 1.0000 Uani . . . . . .
C14 C 0.99897(10) 0.17902(9) 0.56240(3) 0.0277 1.0000 Uani . . . . . .
C15 C 1.00027(10) 0.09370(9) 0.58656(4) 0.0308 1.0000 Uani . . . . . .
C16 C 0.95259(11) 0.10409(9) 0.62402(4) 0.0313 1.0000 Uani . . . . . .
C17 C 0.90313(10) 0.19762(9) 0.63635(3) 0.0278 1.0000 Uani . . . . . .
C18 C 0.89727(9) 0.28739(8) 0.61192(3) 0.0233 1.0000 Uani . . . . . .
C19 C 0.84340(9) 0.38576(8) 0.62409(3) 0.0237 1.0000 Uani . . . . . .
C20 C 0.82077(11) 0.46927(9) 0.68897(3) 0.0315 1.0000 Uani . . . . . .
C21 C 0.76936(13) 0.47383(10) 0.72649(3) 0.0391 1.0000 Uani . . . . . .
C22 C 0.67851(13) 0.40467(11) 0.73736(3) 0.0382 1.0000 Uani . . . . . .
C23 C 0.63197(11) 0.32853(10) 0.71132(3) 0.0319 1.0000 Uani . . . . . .
C24 C 0.53929(13) 0.25408(12) 0.72229(4) 0.0416 1.0000 Uani . . . . . .
C25 C 0.49681(13) 0.17956(12) 0.69724(4) 0.0450 1.0000 Uani . . . . . .
C26 C 0.54255(12) 0.17793(10) 0.65921(4) 0.0378 1.0000 Uani . . . . . .
C27 C 0.63022(10) 0.24978(9) 0.64745(3) 0.0285 1.0000 Uani . . . . . .
C28 C 0.68169(10) 0.32523(8) 0.67325(3) 0.0255 1.0000 Uani . . . . . .
C29 C 0.78124(10) 0.39513(8) 0.66244(3) 0.0248 1.0000 Uani . . . . . .
C30 C 0.57615(10) 0.89710(8) 0.56709(3) 0.0230 1.0000 Uani . . . . . .
C31 C 0.68619(10) 0.95982(9) 0.56528(3) 0.0283 1.0000 Uani . . . . . .
C32 C 0.67822(10) 1.06623(9) 0.55896(3) 0.0283 1.0000 Uani . . . . . .
C33 C 0.56067(10) 1.11570(8) 0.55423(3) 0.0235 1.0000 Uani . . . . . .
C34 C 0.55035(11) 1.22617(8) 0.54731(3) 0.0275 1.0000 Uani . . . . . .
C35 C 0.43598(11) 1.27247(8) 0.54237(3) 0.0300 1.0000 Uani . . . . . .
C36 C 0.32640(11) 1.21101(8) 0.54410(3) 0.0299 1.0000 Uani . . . . . .
C37 C 0.33270(10) 1.10426(8) 0.55087(3) 0.0259 1.0000 Uani . . . . . .
C38 C 0.44999(10) 1.05322(8) 0.55614(3) 0.0213 1.0000 Uani . . . . . .
C39 C 0.45913(9) 0.94205(7) 0.56284(3) 0.0209 1.0000 Uani . . . . . .
C40 C 0.31450(9) 0.81655(7) 0.53083(3) 0.0223 1.0000 Uani . . . . . .
C41 C 0.20433(10) 0.75376(8) 0.52963(3) 0.0263 1.0000 Uani . . . . . .
C42 C 0.12407(10) 0.75204(8) 0.56024(3) 0.0283 1.0000 Uani . . . . . .
C43 C 0.14985(10) 0.81133(8) 0.59377(3) 0.0258 1.0000 Uani . . . . . .
C44 C 0.06621(10) 0.81290(9) 0.62544(4) 0.0326 1.0000 Uani . . . . . .
C45 C 0.09246(12) 0.87012(10) 0.65763(4) 0.0366 1.0000 Uani . . . . . .
C46 C 0.20431(12) 0.92942(9) 0.65968(3) 0.0343 1.0000 Uani . . . . . .
C47 C 0.28691(11) 0.93042(8) 0.62949(3) 0.0280 1.0000 Uani . . . . . .
C48 C 0.26246(9) 0.87207(7) 0.59545(3) 0.0227 1.0000 Uani . . . . . .
C49 C 0.34461(9) 0.87457(7) 0.56310(3) 0.0210 1.0000 Uani . . . . . .
N50 N 0.38049(8) 0.56209(7) 0.64502(3) 0.0251 1.0000 Uani . . . . . .
C51 C 0.36556(10) 0.44284(8) 0.64945(3) 0.0260 1.0000 Uani . . . . . .
C52 C 0.24963(11) 0.39621(9) 0.63031(3) 0.0317 1.0000 Uani . . . . . .
C53 C 0.22871(12) 0.28179(10) 0.64330(4) 0.0363 1.0000 Uani . . . . . .
C54 C 0.18182(15) 0.27263(13) 0.68442(4) 0.0491 1.0000 Uani . . . . . .
C55 C 0.27029(11) 0.61932(9) 0.66346(3) 0.0294 1.0000 Uani . . . . . .
C56 C 0.24413(12) 0.58741(10) 0.70481(3) 0.0363 1.0000 Uani . . . . . .
C57 C 0.14892(12) 0.66030(11) 0.72353(4) 0.0390 1.0000 Uani . . . . . .
C58 C 0.10942(17) 0.61785(18) 0.76250(4) 0.0637 1.0000 Uani . . . . . .
C59 C 0.50271(10) 0.59339(9) 0.66449(3) 0.0277 1.0000 Uani . . . . . .
C60 C 0.52894(12) 0.71128(9) 0.66530(3) 0.0341 1.0000 Uani . . . . . .
C61 C 0.65858(13) 0.73404(12) 0.68134(5) 0.0458 1.0000 Uani . . . . . .
C62 C 0.68483(19) 0.85289(15) 0.68290(6) 0.0692 1.0000 Uani . . . . . .
C63 C 0.38325(10) 0.59218(8) 0.60262(3) 0.0263 1.0000 Uani . . . . . .
C64 C 0.49253(10) 0.54700(8) 0.58023(3) 0.0265 1.0000 Uani . . . . . .
C65 C 0.47640(11) 0.56620(8) 0.53715(3) 0.0291 1.0000 Uani . . . . . .
C66 C 0.58891(12) 0.52549(9) 0.51477(3) 0.0331 1.0000 Uani . . . . . .
F1 F 0.80280(6) 0.71497(5) 0.567107(18) 0.0273 1.0000 Uani . . . . . .
H111 H 0.9071 0.5222 0.5466 0.0345 1.0000 Uiso R . . . . .
H121 H 0.9862 0.3613 0.5244 0.0322 1.0000 Uiso R . . . . .
H141 H 1.0310 0.1729 0.5367 0.0326 1.0000 Uiso R . . . . .
H151 H 1.0321 0.0270 0.5781 0.0365 1.0000 Uiso R . . . . .
H161 H 0.9555 0.0436 0.6408 0.0375 1.0000 Uiso R . . . . .
H171 H 0.8736 0.2051 0.6618 0.0337 1.0000 Uiso R . . . . .
H211 H 0.8030 0.5263 0.7440 0.0466 1.0000 Uiso R . . . . .
H221 H 0.6446 0.4047 0.7630 0.0468 1.0000 Uiso R . . . . .
H241 H 0.5053 0.2566 0.7475 0.0485 1.0000 Uiso R . . . . .
H251 H 0.4347 0.1300 0.7051 0.0543 1.0000 Uiso R . . . . .
H261 H 0.5118 0.1284 0.6409 0.0461 1.0000 Uiso R . . . . .
H271 H 0.6578 0.2496 0.6210 0.0333 1.0000 Uiso R . . . . .
H311 H 0.7652 0.9253 0.5682 0.0337 1.0000 Uiso R . . . . .
H321 H 0.7543 1.1072 0.5575 0.0338 1.0000 Uiso R . . . . .
H341 H 0.6271 1.2671 0.5458 0.0320 1.0000 Uiso R . . . . .
H351 H 0.4298 1.3457 0.5372 0.0359 1.0000 Uiso R . . . . .
H361 H 0.2473 1.2447 0.5405 0.0357 1.0000 Uiso R . . . . .
H371 H 0.2569 1.0617 0.5522 0.0319 1.0000 Uiso R . . . . .
H411 H 0.1869 0.7146 0.5074 0.0332 1.0000 Uiso R . . . . .
H421 H 0.0506 0.7134 0.5589 0.0348 1.0000 Uiso R . . . . .
H441 H -0.0099 0.7712 0.6235 0.0390 1.0000 Uiso R . . . . .
H451 H 0.0367 0.8696 0.6788 0.0429 1.0000 Uiso R . . . . .
H461 H 0.2239 0.9695 0.6822 0.0408 1.0000 Uiso R . . . . .
H471 H 0.3622 0.9710 0.6318 0.0316 1.0000 Uiso R . . . . .
H512 H 0.4401 0.4113 0.6386 0.0293 1.0000 Uiso R . . . . .
H511 H 0.3651 0.4287 0.6768 0.0283 1.0000 Uiso R . . . . .
H522 H 0.2620 0.3991 0.6020 0.0366 1.0000 Uiso R . . . . .
H521 H 0.1776 0.4378 0.6364 0.0383 1.0000 Uiso R . . . . .
H532 H 0.1670 0.2506 0.6256 0.0431 1.0000 Uiso R . . . . .
H531 H 0.3078 0.2414 0.6396 0.0437 1.0000 Uiso R . . . . .
H542 H 0.1645 0.1971 0.6908 0.0728 1.0000 Uiso R . . . . .
H541 H 0.1029 0.3118 0.6881 0.0732 1.0000 Uiso R . . . . .
H543 H 0.2424 0.3003 0.7034 0.0716 1.0000 Uiso R . . . . .
H551 H 0.1984 0.6040 0.6473 0.0353 1.0000 Uiso R . . . . .
H552 H 0.2907 0.6937 0.6609 0.0347 1.0000 Uiso R . . . . .
H561 H 0.2128 0.5144 0.7062 0.0443 1.0000 Uiso R . . . . .
H562 H 0.3230 0.5904 0.7196 0.0444 1.0000 Uiso R . . . . .
H571 H 0.0752 0.6644 0.7065 0.0457 1.0000 Uiso R . . . . .
H572 H 0.1846 0.7324 0.7258 0.0470 1.0000 Uiso R . . . . .
H581 H 0.0529 0.6664 0.7746 0.0950 1.0000 Uiso R . . . . .
H583 H 0.0634 0.5495 0.7588 0.0962 1.0000 Uiso R . . . . .
H582 H 0.1813 0.6097 0.7795 0.0950 1.0000 Uiso R . . . . .
H592 H 0.5690 0.5576 0.6509 0.0334 1.0000 Uiso R . . . . .
H591 H 0.4976 0.5653 0.6902 0.0323 1.0000 Uiso R . . . . .
H602 H 0.5217 0.7391 0.6395 0.0412 1.0000 Uiso R . . . . .
H601 H 0.4651 0.7459 0.6812 0.0405 1.0000 Uiso R . . . . .
H612 H 0.7219 0.6971 0.6661 0.0549 1.0000 Uiso R . . . . .
H611 H 0.6649 0.7039 0.7075 0.0553 1.0000 Uiso R . . . . .
H623 H 0.7668 0.8676 0.6928 0.1029 1.0000 Uiso R . . . . .
H621 H 0.6782 0.8832 0.6575 0.1039 1.0000 Uiso R . . . . .
H622 H 0.6252 0.8883 0.7007 0.1033 1.0000 Uiso R . . . . .
H631 H 0.3036 0.5683 0.5916 0.0316 1.0000 Uiso R . . . . .
H632 H 0.3846 0.6680 0.6018 0.0325 1.0000 Uiso R . . . . .
H641 H 0.4985 0.4726 0.5846 0.0312 1.0000 Uiso R . . . . .
H642 H 0.5690 0.5797 0.5886 0.0314 1.0000 Uiso R . . . . .
H651 H 0.4006 0.5309 0.5282 0.0339 1.0000 Uiso R . . . . .
H652 H 0.4666 0.6435 0.5328 0.0344 1.0000 Uiso R . . . . .
H662 H 0.5802 0.5375 0.4871 0.0482 1.0000 Uiso R . . . . .
H663 H 0.6007 0.4481 0.5192 0.0481 1.0000 Uiso R . . . . .
H661 H 0.6695 0.5608 0.5231 0.0496 1.0000 Uiso R . . . . .
H21 H 0.6629 0.7680 0.5716 0.0452 1.0000 Uiso R . . . . .
H31 H 0.3548 0.8022 0.4784 0.0423 1.0000 Uiso R . . . . .
H41 H 0.8999 0.5620 0.6577 0.0638 1.0000 Uiso R . . . . .
H11 H 0.8110 0.6211 0.5946 0.0483 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.09(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 . C10 . 1.3605(13) yes
O1 . H11 . 0.920 no
O2 . C30 . 1.3551(12) yes
O2 . H21 . 0.897 no
O3 . C40 . 1.3549(13) yes
O3 . H31 . 0.888 no
O4 . C20 . 1.3668(15) yes
O4 . H41 . 0.871 no
C10 . C11 . 1.4197(15) yes
C10 . C19 . 1.3864(15) yes
C11 . C12 . 1.3621(15) yes
C11 . H111 . 0.936 no
C12 . C13 . 1.4186(14) yes
C12 . H121 . 0.975 no
C13 . C14 . 1.4206(15) yes
C13 . C18 . 1.4214(14) yes
C14 . C15 . 1.3684(16) yes
C14 . H141 . 0.962 no
C15 . C16 . 1.4055(17) yes
C15 . H151 . 0.956 no
C16 . C17 . 1.3654(16) yes
C16 . H161 . 0.963 no
C17 . C18 . 1.4200(14) yes
C17 . H171 . 0.946 no
C18 . C19 . 1.4352(14) yes
C19 . C29 . 1.4955(14) yes
C20 . C21 . 1.4175(17) yes
C20 . C29 . 1.3821(15) yes
C21 . C22 . 1.361(2) yes
C21 . H211 . 0.971 no
C22 . C23 . 1.4131(18) yes
C22 . H221 . 0.964 no
C23 . C24 . 1.4191(19) yes
C23 . C28 . 1.4278(15) yes
C24 . C25 . 1.362(2) yes
C24 . H241 . 0.949 no
C25 . C26 . 1.411(2) yes
C25 . H251 . 0.953 no
C26 . C27 . 1.3681(17) yes
C26 . H261 . 0.952 no
C27 . C28 . 1.4212(16) yes
C27 . H271 . 0.965 no
C28 . C29 . 1.4337(15) yes
C30 . C31 . 1.4200(14) yes
C30 . C39 . 1.3817(14) yes
C31 . C32 . 1.3669(15) yes
C31 . H311 . 0.956 no
C32 . C33 . 1.4131(15) yes
C32 . H321 . 0.966 no
C33 . C34 . 1.4225(14) yes
C33 . C38 . 1.4242(14) yes
C34 . C35 . 1.3662(17) yes
C34 . H341 . 0.972 no
C35 . C36 . 1.4070(16) yes
C35 . H351 . 0.946 no
C36 . C37 . 1.3728(15) yes
C36 . H361 . 0.955 no
C37 . C38 . 1.4217(14) yes
C37 . H371 . 0.974 no
C38 . C39 . 1.4291(13) yes
C39 . C49 . 1.4922(13) yes
C40 . C41 . 1.4209(14) yes
C40 . C49 . 1.3799(14) yes
C41 . C42 . 1.3677(16) yes
C41 . H411 . 0.938 no
C42 . C43 . 1.4142(16) yes
C42 . H421 . 0.926 no
C43 . C44 . 1.4192(15) yes
C43 . C48 . 1.4290(14) yes
C44 . C45 . 1.3630(19) yes
C44 . H441 . 0.972 no
C45 . C46 . 1.4130(19) yes
C45 . H451 . 0.946 no
C46 . C47 . 1.3723(16) yes
C46 . H461 . 0.955 no
C47 . C48 . 1.4200(15) yes
C47 . H471 . 0.957 no
C48 . C49 . 1.4277(14) yes
N50 . C51 . 1.5251(13) yes
N50 . C55 . 1.5241(13) yes
N50 . C59 . 1.5237(14) yes
N50 . C63 . 1.5240(13) yes
C51 . C52 . 1.5251(15) yes
C51 . H512 . 0.968 no
C51 . H511 . 0.970 no
C52 . C53 . 1.5330(16) yes
C52 . H522 . 0.994 no
C52 . H521 . 0.956 no
C53 . C54 . 1.521(2) yes
C53 . H532 . 0.985 no
C53 . H531 . 0.996 no
C54 . H542 . 0.999 no
C54 . H541 . 0.986 no
C54 . H543 . 0.988 no
C55 . C56 . 1.5201(16) yes
C55 . H551 . 0.972 no
C55 . H552 . 0.971 no
C56 . C57 . 1.5199(17) yes
C56 . H561 . 0.984 no
C56 . H562 . 0.989 no
C57 . C58 . 1.519(2) yes
C57 . H571 . 0.986 no
C57 . H572 . 0.991 no
C58 . H581 . 0.959 no
C58 . H583 . 1.003 no
C58 . H582 . 0.975 no
C59 . C60 . 1.5179(15) yes
C59 . H592 . 0.964 no
C59 . H591 . 0.963 no
C60 . C61 . 1.5211(18) yes
C60 . H602 . 0.967 no
C60 . H601 . 0.982 no
C61 . C62 . 1.531(2) yes
C61 . H612 . 0.978 no
C61 . H611 . 0.988 no
C62 . H623 . 0.960 no
C62 . H621 . 0.965 no
C62 . H622 . 0.996 no
C63 . C64 . 1.5157(14) yes
C63 . H631 . 0.981 no
C63 . H632 . 0.960 no
C64 . C65 . 1.5285(15) yes
C64 . H641 . 0.956 no
C64 . H642 . 0.961 no
C65 . C66 . 1.5221(16) yes
C65 . H651 . 0.976 no
C65 . H652 . 0.995 no
C66 . H662 . 0.978 no
C66 . H663 . 0.999 no
C66 . H661 . 1.013 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C10 . O1 . H11 . 115.8 no
C30 . O2 . H21 . 112.0 no
C40 . O3 . H31 . 112.4 no
C20 . O4 . H41 . 105.7 no
O1 . C10 . C11 . 120.25(9) yes
O1 . C10 . C19 . 118.38(9) yes
C11 . C10 . C19 . 121.36(9) yes
C10 . C11 . C12 . 120.19(9) yes
C10 . C11 . H111 . 118.4 no
C12 . C11 . H111 . 121.4 no
C11 . C12 . C13 . 121.04(9) yes
C11 . C12 . H121 . 119.9 no
C13 . C12 . H121 . 119.1 no
C12 . C13 . C14 . 121.61(10) yes
C12 . C13 . C18 . 118.82(9) yes
C14 . C13 . C18 . 119.56(9) yes
C13 . C14 . C15 . 121.01(10) yes
C13 . C14 . H141 . 118.6 no
C15 . C14 . H141 . 120.3 no
C14 . C15 . C16 . 119.49(10) yes
C14 . C15 . H151 . 120.7 no
C16 . C15 . H151 . 119.8 no
C15 . C16 . C17 . 120.86(10) yes
C15 . C16 . H161 . 118.4 no
C17 . C16 . H161 . 120.8 no
C16 . C17 . C18 . 121.48(10) yes
C16 . C17 . H171 . 120.7 no
C18 . C17 . H171 . 117.8 no
C13 . C18 . C17 . 117.54(9) yes
C13 . C18 . C19 . 120.12(9) yes
C17 . C18 . C19 . 122.33(10) yes
C18 . C19 . C10 . 118.31(9) yes
C18 . C19 . C29 . 120.67(9) yes
C10 . C19 . C29 . 121.02(9) yes
O4 . C20 . C21 . 115.69(10) yes
O4 . C20 . C29 . 122.68(10) yes
C21 . C20 . C29 . 121.62(11) yes
C20 . C21 . C22 . 120.43(11) yes
C20 . C21 . H211 . 117.6 no
C22 . C21 . H211 . 121.9 no
C21 . C22 . C23 . 120.74(11) yes
C21 . C22 . H221 . 121.7 no
C23 . C22 . H221 . 117.5 no
C22 . C23 . C24 . 121.71(11) yes
C22 . C23 . C28 . 118.95(11) yes
C24 . C23 . C28 . 119.32(11) yes
C23 . C24 . C25 . 121.34(12) yes
C23 . C24 . H241 . 119.6 no
C25 . C24 . H241 . 119.1 no
C24 . C25 . C26 . 119.66(12) yes
C24 . C25 . H251 . 120.2 no
C26 . C25 . H251 . 120.1 no
C25 . C26 . C27 . 120.54(12) yes
C25 . C26 . H261 . 121.2 no
C27 . C26 . H261 . 118.2 no
C26 . C27 . C28 . 121.50(11) yes
C26 . C27 . H271 . 119.5 no
C28 . C27 . H271 . 119.0 no
C23 . C28 . C27 . 117.50(10) yes
C23 . C28 . C29 . 120.09(10) yes
C27 . C28 . C29 . 122.40(10) yes
C19 . C29 . C28 . 120.98(9) yes
C19 . C29 . C20 . 120.94(10) yes
C28 . C29 . C20 . 118.05(10) yes
O2 . C30 . C31 . 120.45(9) yes
O2 . C30 . C39 . 118.57(9) yes
C31 . C30 . C39 . 120.97(9) yes
C30 . C31 . C32 . 120.40(10) yes
C30 . C31 . H311 . 118.1 no
C32 . C31 . H311 . 121.5 no
C31 . C32 . C33 . 120.70(9) yes
C31 . C32 . H321 . 119.0 no
C33 . C32 . H321 . 120.3 no
C32 . C33 . C34 . 121.59(10) yes
C32 . C33 . C38 . 119.13(9) yes
C34 . C33 . C38 . 119.27(10) yes
C33 . C34 . C35 . 120.79(10) yes
C33 . C34 . H341 . 117.9 no
C35 . C34 . H341 . 121.3 no
C34 . C35 . C36 . 120.15(9) yes
C34 . C35 . H351 . 120.4 no
C36 . C35 . H351 . 119.4 no
C35 . C36 . C37 . 120.68(10) yes
C35 . C36 . H361 . 119.0 no
C37 . C36 . H361 . 120.3 no
C36 . C37 . C38 . 120.82(10) yes
C36 . C37 . H371 . 120.7 no
C38 . C37 . H371 . 118.4 no
C33 . C38 . C37 . 118.29(9) yes
C33 . C38 . C39 . 119.82(9) yes
C37 . C38 . C39 . 121.89(9) yes
C38 . C39 . C30 . 118.98(9) yes
C38 . C39 . C49 . 120.54(9) yes
C30 . C39 . C49 . 120.40(8) yes
O3 . C40 . C41 . 120.65(9) yes
O3 . C40 . C49 . 118.38(9) yes
C41 . C40 . C49 . 120.97(9) yes
C40 . C41 . C42 . 120.37(10) yes
C40 . C41 . H411 . 118.9 no
C42 . C41 . H411 . 120.7 no
C41 . C42 . C43 . 120.79(9) yes
C41 . C42 . H421 . 120.0 no
C43 . C42 . H421 . 119.2 no
C42 . C43 . C44 . 121.70(10) yes
C42 . C43 . C48 . 118.89(10) yes
C44 . C43 . C48 . 119.41(10) yes
C43 . C44 . C45 . 121.07(11) yes
C43 . C44 . H441 . 117.8 no
C45 . C44 . H441 . 121.2 no
C44 . C45 . C46 . 119.84(11) yes
C44 . C45 . H451 . 120.3 no
C46 . C45 . H451 . 119.8 no
C45 . C46 . C47 . 120.69(11) yes
C45 . C46 . H461 . 120.5 no
C47 . C46 . H461 . 118.8 no
C46 . C47 . C48 . 121.03(11) yes
C46 . C47 . H471 . 118.8 no
C48 . C47 . H471 . 120.1 no
C43 . C48 . C47 . 117.95(10) yes
C43 . C48 . C49 . 119.83(9) yes
C47 . C48 . C49 . 122.20(9) yes
C39 . C49 . C48 . 121.45(9) yes
C39 . C49 . C40 . 119.39(9) yes
C48 . C49 . C40 . 119.11(9) yes
C51 . N50 . C55 . 110.28(8) yes
C51 . N50 . C59 . 107.57(8) yes
C55 . N50 . C59 . 110.58(8) yes
C51 . N50 . C63 . 110.30(8) yes
C55 . N50 . C63 . 107.70(8) yes
C59 . N50 . C63 . 110.42(8) yes
N50 . C51 . C52 . 115.06(9) yes
N50 . C51 . H512 . 106.4 no
C52 . C51 . H512 . 109.8 no
N50 . C51 . H511 . 106.4 no
C52 . C51 . H511 . 110.7 no
H512 . C51 . H511 . 108.1 no
C51 . C52 . C53 . 110.80(9) yes
C51 . C52 . H522 . 108.0 no
C53 . C52 . H522 . 110.3 no
C51 . C52 . H521 . 110.2 no
C53 . C52 . H521 . 109.7 no
H522 . C52 . H521 . 107.8 no
C52 . C53 . C54 . 113.42(11) yes
C52 . C53 . H532 . 106.9 no
C54 . C53 . H532 . 109.8 no
C52 . C53 . H531 . 108.9 no
C54 . C53 . H531 . 111.2 no
H532 . C53 . H531 . 106.4 no
C53 . C54 . H542 . 110.1 no
C53 . C54 . H541 . 111.5 no
H542 . C54 . H541 . 107.0 no
C53 . C54 . H543 . 112.6 no
H542 . C54 . H543 . 108.1 no
H541 . C54 . H543 . 107.2 no
N50 . C55 . C56 . 114.49(9) yes
N50 . C55 . H551 . 105.8 no
C56 . C55 . H551 . 110.4 no
N50 . C55 . H552 . 104.4 no
C56 . C55 . H552 . 112.7 no
H551 . C55 . H552 . 108.6 no
C55 . C56 . C57 . 111.56(10) yes
C55 . C56 . H561 . 111.0 no
C57 . C56 . H561 . 108.7 no
C55 . C56 . H562 . 109.1 no
C57 . C56 . H562 . 108.9 no
H561 . C56 . H562 . 107.5 no
C56 . C57 . C58 . 110.74(13) yes
C56 . C57 . H571 . 108.0 no
C58 . C57 . H571 . 109.4 no
C56 . C57 . H572 . 109.6 no
C58 . C57 . H572 . 111.1 no
H571 . C57 . H572 . 107.9 no
C57 . C58 . H581 . 109.9 no
C57 . C58 . H583 . 109.1 no
H581 . C58 . H583 . 107.5 no
C57 . C58 . H582 . 111.2 no
H581 . C58 . H582 . 107.3 no
H583 . C58 . H582 . 111.9 no
N50 . C59 . C60 . 114.96(9) yes
N50 . C59 . H592 . 106.9 no
C60 . C59 . H592 . 109.5 no
N50 . C59 . H591 . 105.5 no
C60 . C59 . H591 . 110.9 no
H592 . C59 . H591 . 108.8 no
C59 . C60 . C61 . 111.16(11) yes
C59 . C60 . H602 . 109.0 no
C61 . C60 . H602 . 110.1 no
C59 . C60 . H601 . 108.7 no
C61 . C60 . H601 . 110.0 no
H602 . C60 . H601 . 107.8 no
C60 . C61 . C62 . 111.47(14) yes
C60 . C61 . H612 . 109.9 no
C62 . C61 . H612 . 111.2 no
C60 . C61 . H611 . 109.1 no
C62 . C61 . H611 . 109.5 no
H612 . C61 . H611 . 105.5 no
C61 . C62 . H623 . 111.7 no
C61 . C62 . H621 . 110.2 no
H623 . C62 . H621 . 108.6 no
C61 . C62 . H622 . 110.3 no
H623 . C62 . H622 . 105.9 no
H621 . C62 . H622 . 110.1 no
N50 . C63 . C64 . 114.73(8) yes
N50 . C63 . H631 . 106.6 no
C64 . C63 . H631 . 110.5 no
N50 . C63 . H632 . 106.3 no
C64 . C63 . H632 . 110.5 no
H631 . C63 . H632 . 108.0 no
C63 . C64 . C65 . 110.94(9) yes
C63 . C64 . H641 . 109.9 no
C65 . C64 . H641 . 108.7 no
C63 . C64 . H642 . 109.7 no
C65 . C64 . H642 . 109.0 no
H641 . C64 . H642 . 108.5 no
C64 . C65 . C66 . 111.03(9) yes
C64 . C65 . H651 . 109.5 no
C66 . C65 . H651 . 109.7 no
C64 . C65 . H652 . 108.5 no
C66 . C65 . H652 . 109.8 no
H651 . C65 . H652 . 108.3 no
C65 . C66 . H662 . 112.0 no
C65 . C66 . H663 . 110.7 no
H662 . C66 . H663 . 108.3 no
C65 . C66 . H661 . 112.1 no
H662 . C66 . H661 . 107.2 no
H663 . C66 . H661 . 106.3 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C11 . H111 . O3 3_566 174.65 0.936 2.566 3.4987(16) yes
C57 . H571 . O4 1_455 137.25 0.986 2.493 3.2861(16) yes
C60 . H602 . O2 . 159.25 0.967 2.486 3.4082(16) yes
O4 . H41 . O1 . 153.64 0.871 1.852 2.6607(16) yes
O4 . H41 . C10 . 133.47 0.871 2.377 3.0424(16) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 20/04/15 at 20:24:33
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE O   (   1,X'S) H   (  11,X'S) 
RIDE O   (   2,X'S) H   (  21,X'S) 
RIDE O   (   3,X'S) H   (  31,X'S) 
RIDE O   (   4,X'S) H   (  41,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  51,X'S) H   ( 512,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 522,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 532,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 542,X'S) H   ( 541,X'S) H   ( 543,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) H   ( 572,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) H   ( 583,X'S) H   ( 582,X'S) 
RIDE C   (  59,X'S) H   ( 592,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 602,X'S) H   ( 601,X'S) 
RIDE C   (  61,X'S) H   ( 612,X'S) H   ( 611,X'S) 
RIDE C   (  62,X'S) H   ( 623,X'S) H   ( 621,X'S) H   ( 622,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) H   ( 632,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) H   ( 642,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) H   ( 652,X'S) 
RIDE C   (  66,X'S) H   ( 662,X'S) H   ( 663,X'S) H   ( 661,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 20/04/15 at 20:24:33
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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_2i
_database_code_depnum_ccdc_archive 'CCDC 1401773'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             13-04-24
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 008gwp12
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   8.75510(1)
_cell_length_b                   12.74630(1)
_cell_length_c                   22.1115(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.0698(6)
_cell_angle_gamma                90
_cell_volume                     2465.93(4)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P c '
_symmetry_space_group_name_Hall  'P -2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x,-y,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C60 H108 F1.50 N1.50 O6 
# Dc =      1.31 Fooo =    892.00 Mu =      6.73 M =    975.02
# Found Formula = C49 H80 F1 N1 O7 
# Dc =      1.10 FOOO =    892.00 Mu =      5.89 M =    814.17

_chemical_formula_sum            'C49 H80 F1 N1 O7'
_chemical_formula_moiety         'C16 H36 N, 3(C11 H14 O2), F, H2 O'
_chemical_compound_source        .
_chemical_formula_weight         814.17


_cell_measurement_reflns_used    35528
_cell_measurement_theta_min      3
_cell_measurement_theta_max      77
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.160
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_max          0.190

_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             892
_exptl_absorpt_coefficient_mu    0.589

# Sheldrick geometric approximatio 0.90 0.91 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_T_max  0.91
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            53899
_reflns_number_total             9870
_diffrn_reflns_av_R_equivalents  0.020
# Number of reflections without Friedels Law is 9870 
# Number of reflections with Friedels Law is 5165 
# Theoretical number of reflections is about 5197 


_diffrn_reflns_theta_min         3.467
_diffrn_reflns_theta_max         76.731
_diffrn_measured_fraction_theta_max 0.993

_diffrn_reflns_theta_full        75.196
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_reflns_limit_h_min              -11
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              -27
_reflns_limit_l_max              27

_oxford_diffrn_Wilson_B_factor   3.10
_oxford_diffrn_Wilson_scale      0.02

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.16
_refine_diff_density_max         0.33


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         9828
_refine_ls_number_restraints     2
_refine_ls_number_parameters     544
_oxford_refine_ls_R_factor_ref   0.0300
_refine_ls_wR_factor_ref         0.0797
_refine_ls_goodness_of_fit_ref   0.9982
_refine_ls_shift/su_max          0.0006168
_refine_ls_shift/su_mean         0.0000430


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        9828
_refine_ls_R_factor_all          0.0300
_refine_ls_wR_factor_all         0.0797

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                9682
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_gt          0.0793

_refine_ls_abs_structure_Flack   0.31(7)
_refine_ls_abs_structure_details 'Flack (1983), 4705 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 0.27P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
O4 O 0.50000(12) 0.66964(8) 0.50000(6) 0.0486 1.0000 Uani . . . . . .
C101 C 0.30115(14) 0.31495(9) 0.79767(6) 0.0307 1.0000 Uani . . . . . .
O102 O 0.44884(10) 0.28299(8) 0.77746(4) 0.0377 1.0000 Uani . . . . . .
C103 C 0.44920(14) 0.26684(10) 0.71267(6) 0.0340 1.0000 Uani . . . . . .
C104 C 0.29566(13) 0.30780(9) 0.69063(6) 0.0295 1.0000 Uani . . . . . .
C105 C 0.21146(13) 0.33600(9) 0.73947(6) 0.0289 1.0000 Uani . . . . . .
C106 C 0.06499(14) 0.37623(9) 0.73136(6) 0.0349 1.0000 Uani . . . . . .
C107 C 0.00506(15) 0.38810(10) 0.67265(7) 0.0382 1.0000 Uani . . . . . .
C108 C 0.08974(16) 0.35933(10) 0.62368(6) 0.0382 1.0000 Uani . . . . . .
C109 C 0.23644(15) 0.31882(10) 0.63185(6) 0.0347 1.0000 Uani . . . . . .
C110 C 0.46587(18) 0.15040(12) 0.69899(8) 0.0487 1.0000 Uani . . . . . .
C111 C 0.58127(17) 0.32992(15) 0.68869(8) 0.0528 1.0000 Uani . . . . . .
C112 C 0.32356(16) 0.40986(10) 0.83837(6) 0.0400 1.0000 Uani . . . . . .
C201 C 0.26486(13) 0.06898(8) 0.47213(6) 0.0290 1.0000 Uani . . . . . .
O202 O 0.12590(11) 0.10265(7) 0.44066(5) 0.0403 1.0000 Uani . . . . . .
C203 C 0.12543(15) 0.21257(10) 0.42660(6) 0.0366 1.0000 Uani . . . . . .
C204 C 0.27519(15) 0.25169(9) 0.45348(6) 0.0329 1.0000 Uani . . . . . .
C205 C 0.35522(13) 0.16944(8) 0.47991(6) 0.0284 1.0000 Uani . . . . . .
C206 C 0.49837(15) 0.18469(10) 0.50753(6) 0.0350 1.0000 Uani . . . . . .
C207 C 0.55869(16) 0.28618(11) 0.50860(7) 0.0417 1.0000 Uani . . . . . .
C208 C 0.47725(19) 0.36934(11) 0.48235(7) 0.0461 1.0000 Uani . . . . . .
C209 C 0.33523(18) 0.35236(10) 0.45422(7) 0.0418 1.0000 Uani . . . . . .
C210 C -0.01216(19) 0.26086(16) 0.45642(10) 0.0628 1.0000 Uani . . . . . .
C211 C 0.1145(2) 0.22622(14) 0.35816(7) 0.0542 1.0000 Uani . . . . . .
C212 C 0.22142(15) 0.01914(10) 0.53111(6) 0.0371 1.0000 Uani . . . . . .
C301 C 0.12003(13) 0.66340(8) 0.55218(6) 0.0281 1.0000 Uani . . . . . .
O302 O 0.25226(10) 0.67214(7) 0.59262(4) 0.0327 1.0000 Uani . . . . . .
C303 C 0.20962(14) 0.69262(9) 0.65431(6) 0.0317 1.0000 Uani . . . . . .
C304 C 0.04117(14) 0.66709(9) 0.65313(6) 0.0312 1.0000 Uani . . . . . .
C305 C -0.00963(13) 0.64851(9) 0.59417(6) 0.0295 1.0000 Uani . . . . . .
C306 C -0.16067(14) 0.62207(10) 0.58062(6) 0.0358 1.0000 Uani . . . . . .
C307 C -0.26035(15) 0.61388(12) 0.62790(7) 0.0418 1.0000 Uani . . . . . .
C308 C -0.20951(16) 0.63293(12) 0.68699(7) 0.0446 1.0000 Uani . . . . . .
C309 C -0.05831(16) 0.66035(11) 0.70011(6) 0.0399 1.0000 Uani . . . . . .
C310 C 0.30384(15) 0.61891(11) 0.69497(6) 0.0395 1.0000 Uani . . . . . .
C311 C 0.24051(19) 0.80753(11) 0.66936(7) 0.0480 1.0000 Uani . . . . . .
C312 C 0.14779(15) 0.57207(9) 0.50983(6) 0.0332 1.0000 Uani . . . . . .
N401 N 0.78499(11) 0.88504(8) 0.38629(5) 0.0281 1.0000 Uani . . . . . .
C402 C 0.92567(13) 0.90555(9) 0.34975(6) 0.0301 1.0000 Uani . . . . . .
C403 C 0.90361(15) 0.89348(12) 0.28170(6) 0.0394 1.0000 Uani . . . . . .
C404 C 1.03440(18) 0.94554(11) 0.24969(7) 0.0442 1.0000 Uani . . . . . .
C405 C 1.0245(2) 0.92720(13) 0.18188(7) 0.0546 1.0000 Uani . . . . . .
C406 C 0.65010(14) 0.95199(11) 0.36451(6) 0.0373 1.0000 Uani . . . . . .
C407 C 0.67812(17) 1.06756(12) 0.36302(7) 0.0460 1.0000 Uani . . . . . .
C408 C 0.55021(19) 1.12193(14) 0.32633(8) 0.0549 1.0000 Uani . . . . . .
C409 C 0.5705(2) 1.23960(16) 0.32652(10) 0.0670 1.0000 Uani . . . . . .
C410 C 0.83252(13) 0.91085(8) 0.45145(5) 0.0268 1.0000 Uani . . . . . .
C411 C 0.71240(13) 0.89379(9) 0.49797(6) 0.0313 1.0000 Uani . . . . . .
C412 C 0.77563(15) 0.92691(10) 0.56040(6) 0.0364 1.0000 Uani . . . . . .
C413 C 0.66102(19) 0.90926(12) 0.60932(7) 0.0454 1.0000 Uani . . . . . .
C414 C 0.72984(14) 0.77276(11) 0.37936(6) 0.0360 1.0000 Uani . . . . . .
C415 C 0.84226(17) 0.68791(11) 0.39804(8) 0.0457 1.0000 Uani . . . . . .
C416 C 0.7747(3) 0.57464(17) 0.40321(15) 0.0374 0.600(5) Uani . . P 1 1 .
C417 C 0.7434(3) 0.52824(17) 0.34121(11) 0.0428 0.600(5) Uani . . P 1 1 .
C418 C 0.7449(5) 0.5931(3) 0.3723(3) 0.0469 0.400(5) Uani . . P 1 2 .
C419 C 0.8350(5) 0.4944(3) 0.3844(2) 0.0608 0.400(5) Uani . . P 1 2 .
O1 O 0.22954(12) 0.23344(7) 0.82788(5) 0.0401 1.0000 Uani . . . . . .
O2 O 0.34577(11) 0.00067(7) 0.43625(5) 0.0385 1.0000 Uani . . . . . .
O3 O 0.09466(10) 0.75708(6) 0.52017(5) 0.0330 1.0000 Uani . . . . . .
F1 F 0.30143(10) 0.79919(5) 0.44099(4) 0.0372 1.0000 Uani . . . . . .
H3121 H 0.0523 0.5611 0.4851 0.0502 1.0000 Uiso R . . . . .
H3123 H 0.2292 0.5906 0.4837 0.0491 1.0000 Uiso R . . . . .
H3122 H 0.1750 0.5096 0.5334 0.0494 1.0000 Uiso R . . . . .
H3061 H -0.1965 0.6109 0.5402 0.0443 1.0000 Uiso R . . . . .
H3071 H -0.3653 0.5981 0.6193 0.0497 1.0000 Uiso R . . . . .
H3081 H -0.2792 0.6287 0.7198 0.0535 1.0000 Uiso R . . . . .
H3091 H -0.0231 0.6742 0.7411 0.0472 1.0000 Uiso R . . . . .
H3102 H 0.2755 0.6280 0.7378 0.0584 1.0000 Uiso R . . . . .
H3103 H 0.4126 0.6366 0.6917 0.0573 1.0000 Uiso R . . . . .
H3101 H 0.2862 0.5451 0.6825 0.0569 1.0000 Uiso R . . . . .
H3113 H 0.2165 0.8186 0.7108 0.0708 1.0000 Uiso R . . . . .
H3111 H 0.3479 0.8225 0.6646 0.0704 1.0000 Uiso R . . . . .
H3112 H 0.1796 0.8531 0.6424 0.0708 1.0000 Uiso R . . . . .
H1121 H 0.2234 0.4306 0.8522 0.0584 1.0000 Uiso R . . . . .
H1123 H 0.3860 0.3931 0.8742 0.0591 1.0000 Uiso R . . . . .
H1122 H 0.3706 0.4648 0.8147 0.0597 1.0000 Uiso R . . . . .
H1061 H 0.0087 0.3956 0.7655 0.0426 1.0000 Uiso R . . . . .
H1071 H -0.0925 0.4146 0.6651 0.0460 1.0000 Uiso R . . . . .
H1081 H 0.0467 0.3667 0.5830 0.0448 1.0000 Uiso R . . . . .
H1091 H 0.2931 0.3004 0.5964 0.0427 1.0000 Uiso R . . . . .
H1103 H 0.4582 0.1375 0.6565 0.0723 1.0000 Uiso R . . . . .
H1101 H 0.5637 0.1218 0.7140 0.0728 1.0000 Uiso R . . . . .
H1102 H 0.3820 0.1118 0.7179 0.0703 1.0000 Uiso R . . . . .
H1112 H 0.5804 0.3259 0.6451 0.0771 1.0000 Uiso R . . . . .
H1111 H 0.6760 0.3023 0.7057 0.0803 1.0000 Uiso R . . . . .
H1113 H 0.5706 0.4037 0.6993 0.0784 1.0000 Uiso R . . . . .
H2122 H 0.3099 -0.0061 0.5529 0.0559 1.0000 Uiso R . . . . .
H2123 H 0.1722 0.0687 0.5572 0.0554 1.0000 Uiso R . . . . .
H2121 H 0.1524 -0.0380 0.5239 0.0546 1.0000 Uiso R . . . . .
H2111 H 0.1189 0.3011 0.3504 0.0799 1.0000 Uiso R . . . . .
H2113 H 0.2010 0.1912 0.3406 0.0803 1.0000 Uiso R . . . . .
H2112 H 0.0171 0.1955 0.3403 0.0792 1.0000 Uiso R . . . . .
H2103 H -0.0097 0.3354 0.4507 0.0934 1.0000 Uiso R . . . . .
H2101 H -0.0073 0.2441 0.5000 0.0942 1.0000 Uiso R . . . . .
H2102 H -0.1059 0.2337 0.4379 0.0927 1.0000 Uiso R . . . . .
H2091 H 0.2790 0.4092 0.4369 0.0490 1.0000 Uiso R . . . . .
H2081 H 0.5223 0.4371 0.4829 0.0555 1.0000 Uiso R . . . . .
H2071 H 0.6518 0.2990 0.5257 0.0494 1.0000 Uiso R . . . . .
H2061 H 0.5526 0.1271 0.5264 0.0420 1.0000 Uiso R . . . . .
H4022 H 0.9613 0.9752 0.3593 0.0335 1.0000 Uiso R . . . . .
H4021 H 1.0005 0.8562 0.3640 0.0347 1.0000 Uiso R . . . . .
H4032 H 0.8077 0.9229 0.2680 0.0482 1.0000 Uiso R . . . . .
H4031 H 0.9046 0.8193 0.2705 0.0484 1.0000 Uiso R . . . . .
H4041 H 1.0296 1.0196 0.2589 0.0553 1.0000 Uiso R . . . . .
H4042 H 1.1324 0.9156 0.2676 0.0536 1.0000 Uiso R . . . . .
H4052 H 1.1127 0.9583 0.1621 0.0809 1.0000 Uiso R . . . . .
H4053 H 0.9330 0.9570 0.1650 0.0805 1.0000 Uiso R . . . . .
H4051 H 1.0260 0.8536 0.1727 0.0794 1.0000 Uiso R . . . . .
H4141 H 0.6974 0.7652 0.3370 0.0435 1.0000 Uiso R . . . . .
H4142 H 0.6396 0.7658 0.4037 0.0400 1.0000 Uiso R . . . . .
H4151 H 0.8879 0.7059 0.4386 0.0538 0.600(5) Uiso R . P 1 1 .
H4152 H 0.9268 0.6874 0.3688 0.0539 0.600(5) Uiso R . P 1 1 .
H4153 H 0.8636 0.6889 0.4423 0.0547 0.400(5) Uiso R . P 1 2 .
H4154 H 0.9393 0.6945 0.3771 0.0541 0.400(5) Uiso R . P 1 2 .
H4172 H 0.6914 0.4621 0.3454 0.0634 0.600(5) Uiso R . P 1 1 .
H4173 H 0.8365 0.5181 0.3217 0.0642 0.600(5) Uiso R . P 1 1 .
H4171 H 0.6743 0.5739 0.3185 0.0642 0.600(5) Uiso R . P 1 1 .
H4191 H 0.7759 0.4347 0.3711 0.0904 0.400(5) Uiso R . P 1 2 .
H4192 H 0.8615 0.4873 0.4267 0.0911 0.400(5) Uiso R . P 1 2 .
H4193 H 0.9282 0.4976 0.3627 0.0908 0.400(5) Uiso R . P 1 2 .
H4062 H 0.5692 0.9379 0.3907 0.0437 1.0000 Uiso R . . . . .
H4061 H 0.6230 0.9280 0.3234 0.0436 1.0000 Uiso R . . . . .
H4072 H 0.6863 1.0970 0.4016 0.0534 1.0000 Uiso R . . . . .
H4071 H 0.7739 1.0868 0.3464 0.0546 1.0000 Uiso R . . . . .
H4081 H 0.4493 1.1031 0.3435 0.0663 1.0000 Uiso R . . . . .
H4082 H 0.5560 1.1031 0.2817 0.0684 1.0000 Uiso R . . . . .
H4091 H 0.4867 1.2721 0.2994 0.1005 1.0000 Uiso R . . . . .
H4093 H 0.5637 1.2700 0.3688 0.1001 1.0000 Uiso R . . . . .
H4092 H 0.6710 1.2610 0.3099 0.1000 1.0000 Uiso R . . . . .
H4102 H 0.8685 0.9832 0.4524 0.0314 1.0000 Uiso R . . . . .
H4101 H 0.9198 0.8672 0.4614 0.0328 1.0000 Uiso R . . . . .
H4111 H 0.6216 0.9362 0.4873 0.0379 1.0000 Uiso R . . . . .
H4112 H 0.6850 0.8210 0.4990 0.0375 1.0000 Uiso R . . . . .
H4121 H 0.8062 1.0031 0.5597 0.0428 1.0000 Uiso R . . . . .
H4122 H 0.8687 0.8828 0.5708 0.0453 1.0000 Uiso R . . . . .
H4131 H 0.7031 0.9279 0.6484 0.0683 1.0000 Uiso R . . . . .
H4132 H 0.5684 0.9500 0.6010 0.0687 1.0000 Uiso R . . . . .
H4133 H 0.6347 0.8361 0.6101 0.0687 1.0000 Uiso R . . . . .
H4181 H 0.6475 0.5908 0.3927 0.0560 0.400(5) Uiso R . P 1 2 .
H4182 H 0.7235 0.5997 0.3297 0.0569 0.400(5) Uiso R . P 1 2 .
H4161 H 0.8413 0.5277 0.4268 0.0458 0.600(5) Uiso R . P 1 1 .
H4162 H 0.6754 0.5808 0.4231 0.0457 0.600(5) Uiso R . P 1 1 .
H21 H 0.3132 -0.0606 0.4415 0.0570 1.0000 Uiso R . . . . .
H11 H 0.2694 0.2285 0.8632 0.0593 1.0000 Uiso R . . . . .
H42 H 0.4554 0.6665 0.5338 0.0731 1.0000 Uiso R . . . . .
H31 H 0.1631 0.7667 0.4962 0.0494 1.0000 Uiso R . . . . .
H41 H 0.4479 0.7138 0.4804 0.0721 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       83(8)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          7.22(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O4 . H42 . 0.857 no
O4 . H41 . 0.835 no
C101 . O102 . 1.4419(15) yes
C101 . C105 . 1.5072(15) yes
C101 . C112 . 1.5164(17) yes
C101 . O1 . 1.3960(14) yes
O102 . C103 . 1.4475(15) yes
C103 . C104 . 1.5066(16) yes
C103 . C110 . 1.5228(19) yes
C103 . C111 . 1.5195(19) yes
C104 . C105 . 1.3771(17) yes
C104 . C109 . 1.3890(16) yes
C105 . C106 . 1.3867(17) yes
C106 . C107 . 1.3907(18) yes
C106 . H1061 . 0.949 no
C107 . C108 . 1.384(2) yes
C107 . H1071 . 0.928 no
C108 . C109 . 1.3899(19) yes
C108 . H1081 . 0.968 no
C109 . H1091 . 0.971 no
C110 . H1103 . 0.955 no
C110 . H1101 . 0.978 no
C110 . H1102 . 0.989 no
C111 . H1112 . 0.965 no
C111 . H1111 . 0.965 no
C111 . H1113 . 0.974 no
C112 . H1121 . 0.976 no
C112 . H1123 . 0.970 no
C112 . H1122 . 0.974 no
C201 . O202 . 1.4447(14) yes
C201 . C205 . 1.5118(15) yes
C201 . C212 . 1.5116(16) yes
C201 . O2 . 1.3892(14) yes
O202 . C203 . 1.4351(15) yes
C203 . C204 . 1.5049(18) yes
C203 . C210 . 1.524(2) yes
C203 . C211 . 1.5228(19) yes
C204 . C205 . 1.3791(16) yes
C204 . C209 . 1.3865(17) yes
C205 . C206 . 1.3878(17) yes
C206 . C207 . 1.3971(18) yes
C206 . H2061 . 0.961 no
C207 . C208 . 1.393(2) yes
C207 . H2071 . 0.901 no
C208 . C209 . 1.387(2) yes
C208 . H2081 . 0.950 no
C209 . H2091 . 0.949 no
C210 . H2103 . 0.959 no
C210 . H2101 . 0.985 no
C210 . H2102 . 0.968 no
C211 . H2111 . 0.971 no
C211 . H2113 . 0.972 no
C211 . H2112 . 1.007 no
C212 . H2122 . 0.954 no
C212 . H2123 . 0.966 no
C212 . H2121 . 0.955 no
C301 . O302 . 1.4414(13) yes
C301 . C305 . 1.5043(17) yes
C301 . C312 . 1.5191(16) yes
C301 . O3 . 1.4016(13) yes
O302 . C303 . 1.4507(14) yes
C303 . C304 . 1.5096(17) yes
C303 . C310 . 1.5226(17) yes
C303 . C311 . 1.5240(17) yes
C304 . C305 . 1.3825(16) yes
C304 . C309 . 1.3822(19) yes
C305 . C306 . 1.3869(17) yes
C306 . C307 . 1.3898(19) yes
C306 . H3061 . 0.947 no
C307 . C308 . 1.386(2) yes
C307 . H3071 . 0.953 no
C308 . C309 . 1.390(2) yes
C308 . H3081 . 0.965 no
C309 . H3091 . 0.963 no
C310 . H3102 . 0.994 no
C310 . H3103 . 0.983 no
C310 . H3101 . 0.991 no
C311 . H3113 . 0.957 no
C311 . H3111 . 0.969 no
C311 . H3112 . 0.977 no
C312 . H3121 . 0.992 no
C312 . H3123 . 0.964 no
C312 . H3122 . 0.976 no
N401 . C402 . 1.5199(14) yes
N401 . C406 . 1.5211(14) yes
N401 . C410 . 1.5211(13) yes
N401 . C414 . 1.5164(16) yes
C402 . C403 . 1.5179(16) yes
C402 . H4022 . 0.962 no
C402 . H4021 . 0.953 no
C403 . C404 . 1.520(2) yes
C403 . H4032 . 0.959 no
C403 . H4031 . 0.977 no
C404 . C405 . 1.517(2) yes
C404 . H4041 . 0.967 no
C404 . H4042 . 1.006 no
C405 . H4052 . 0.984 no
C405 . H4053 . 0.951 no
C405 . H4051 . 0.960 no
C406 . C407 . 1.494(2) yes
C406 . H4062 . 0.948 no
C406 . H4061 . 0.980 no
C407 . C408 . 1.5255(19) yes
C407 . H4072 . 0.933 no
C407 . H4071 . 0.960 no
C408 . C409 . 1.510(3) yes
C408 . H4081 . 1.003 no
C408 . H4082 . 1.019 no
C409 . H4091 . 1.018 no
C409 . H4093 . 1.017 no
C409 . H4092 . 1.003 no
C410 . C411 . 1.5131(16) yes
C410 . H4102 . 0.975 no
C410 . H4101 . 0.964 no
C411 . C412 . 1.5280(16) yes
C411 . H4111 . 0.983 no
C411 . H4112 . 0.959 no
C412 . C413 . 1.5187(19) yes
C412 . H4121 . 1.007 no
C412 . H4122 . 1.010 no
C413 . H4131 . 0.957 no
C413 . H4132 . 0.975 no
C413 . H4133 . 0.961 no
C414 . C415 . 1.510(2) yes
C414 . H4141 . 0.974 no
C414 . H4142 . 0.976 no
C415 . C416 . 1.566(2) yes
C415 . H4151 . 0.994 no
C415 . H4152 . 1.000 no
C415 . C418 . 1.574(4) yes
C415 . H4153 . 0.989 no
C415 . H4154 . 0.986 no
C416 . C417 . 1.509(4) yes
C416 . H4161 . 0.973 no
C416 . H4162 . 0.991 no
C417 . H4172 . 0.964 no
C417 . H4173 . 0.944 no
C417 . H4171 . 0.967 no
C418 . C419 . 1.504(6) yes
C418 . H4181 . 0.980 no
C418 . H4182 . 0.956 no
C419 . H4191 . 0.961 no
C419 . H4192 . 0.959 no
C419 . H4193 . 0.963 no
O1 . H11 . 0.846 no
O2 . H21 . 0.841 no
O3 . H31 . 0.824 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
H42 . O4 . H41 . 103.1 no
O102 . C101 . C105 . 103.37(9) yes
O102 . C101 . C112 . 108.12(10) yes
C105 . C101 . C112 . 114.64(10) yes
O102 . C101 . O1 . 111.18(10) yes
C105 . C101 . O1 . 108.18(9) yes
C112 . C101 . O1 . 111.13(10) yes
C101 . O102 . C103 . 112.38(9) yes
O102 . C103 . C104 . 103.72(10) yes
O102 . C103 . C110 . 109.81(11) yes
C104 . C103 . C110 . 111.36(10) yes
O102 . C103 . C111 . 107.40(11) yes
C104 . C103 . C111 . 112.65(11) yes
C110 . C103 . C111 . 111.51(13) yes
C103 . C104 . C105 . 109.47(10) yes
C103 . C104 . C109 . 129.52(11) yes
C105 . C104 . C109 . 121.01(11) yes
C101 . C105 . C104 . 110.24(10) yes
C101 . C105 . C106 . 128.84(11) yes
C104 . C105 . C106 . 120.91(11) yes
C105 . C106 . C107 . 118.49(12) yes
C105 . C106 . H1061 . 119.8 no
C107 . C106 . H1061 . 121.7 no
C106 . C107 . C108 . 120.45(12) yes
C106 . C107 . H1071 . 121.5 no
C108 . C107 . H1071 . 118.1 no
C107 . C108 . C109 . 121.04(11) yes
C107 . C108 . H1081 . 120.0 no
C109 . C108 . H1081 . 118.9 no
C108 . C109 . C104 . 118.10(12) yes
C108 . C109 . H1091 . 118.8 no
C104 . C109 . H1091 . 123.1 no
C103 . C110 . H1103 . 111.1 no
C103 . C110 . H1101 . 112.6 no
H1103 . C110 . H1101 . 107.4 no
C103 . C110 . H1102 . 108.8 no
H1103 . C110 . H1102 . 107.6 no
H1101 . C110 . H1102 . 109.1 no
C103 . C111 . H1112 . 110.0 no
C103 . C111 . H1111 . 109.0 no
H1112 . C111 . H1111 . 110.2 no
C103 . C111 . H1113 . 110.2 no
H1112 . C111 . H1113 . 107.2 no
H1111 . C111 . H1113 . 110.2 no
C101 . C112 . H1121 . 107.7 no
C101 . C112 . H1123 . 111.5 no
H1121 . C112 . H1123 . 106.9 no
C101 . C112 . H1122 . 107.6 no
H1121 . C112 . H1122 . 112.1 no
H1123 . C112 . H1122 . 111.2 no
O202 . C201 . C205 . 103.37(9) yes
O202 . C201 . C212 . 107.86(10) yes
C205 . C201 . C212 . 113.87(10) yes
O202 . C201 . O2 . 110.43(9) yes
C205 . C201 . O2 . 108.68(9) yes
C212 . C201 . O2 . 112.26(10) yes
C201 . O202 . C203 . 112.97(9) yes
O202 . C203 . C204 . 104.02(9) yes
O202 . C203 . C210 . 107.26(13) yes
C204 . C203 . C210 . 112.73(11) yes
O202 . C203 . C211 . 109.05(11) yes
C204 . C203 . C211 . 112.16(12) yes
C210 . C203 . C211 . 111.20(13) yes
C203 . C204 . C205 . 109.73(10) yes
C203 . C204 . C209 . 129.48(12) yes
C205 . C204 . C209 . 120.79(12) yes
C201 . C205 . C204 . 109.87(10) yes
C201 . C205 . C206 . 129.00(10) yes
C204 . C205 . C206 . 121.12(11) yes
C205 . C206 . C207 . 118.16(12) yes
C205 . C206 . H2061 . 120.5 no
C207 . C206 . H2061 . 121.3 no
C206 . C207 . C208 . 120.68(13) yes
C206 . C207 . H2071 . 120.7 no
C208 . C207 . H2071 . 118.6 no
C207 . C208 . C209 . 120.35(12) yes
C207 . C208 . H2081 . 118.7 no
C209 . C208 . H2081 . 120.9 no
C208 . C209 . C204 . 118.88(12) yes
C208 . C209 . H2091 . 120.4 no
C204 . C209 . H2091 . 120.7 no
C203 . C210 . H2103 . 108.7 no
C203 . C210 . H2101 . 109.2 no
H2103 . C210 . H2101 . 110.1 no
C203 . C210 . H2102 . 110.1 no
H2103 . C210 . H2102 . 108.7 no
H2101 . C210 . H2102 . 110.0 no
C203 . C211 . H2111 . 106.7 no
C203 . C211 . H2113 . 108.8 no
H2111 . C211 . H2113 . 110.1 no
C203 . C211 . H2112 . 111.5 no
H2111 . C211 . H2112 . 110.6 no
H2113 . C211 . H2112 . 109.1 no
C201 . C212 . H2122 . 110.7 no
C201 . C212 . H2123 . 111.8 no
H2122 . C212 . H2123 . 106.9 no
C201 . C212 . H2121 . 110.7 no
H2122 . C212 . H2121 . 108.9 no
H2123 . C212 . H2121 . 107.7 no
O302 . C301 . C305 . 103.52(9) yes
O302 . C301 . C312 . 107.39(9) yes
C305 . C301 . C312 . 115.14(10) yes
O302 . C301 . O3 . 110.89(9) yes
C305 . C301 . O3 . 108.05(9) yes
C312 . C301 . O3 . 111.57(9) yes
C301 . O302 . C303 . 111.65(8) yes
O302 . C303 . C304 . 103.26(9) yes
O302 . C303 . C310 . 106.97(10) yes
C304 . C303 . C310 . 112.66(10) yes
O302 . C303 . C311 . 109.19(10) yes
C304 . C303 . C311 . 112.12(11) yes
C310 . C303 . C311 . 112.09(11) yes
C303 . C304 . C305 . 109.51(10) yes
C303 . C304 . C309 . 129.95(11) yes
C305 . C304 . C309 . 120.54(12) yes
C301 . C305 . C304 . 109.65(10) yes
C301 . C305 . C306 . 129.20(11) yes
C304 . C305 . C306 . 121.14(12) yes
C305 . C306 . C307 . 118.38(12) yes
C305 . C306 . H3061 . 121.4 no
C307 . C306 . H3061 . 120.2 no
C306 . C307 . C308 . 120.46(12) yes
C306 . C307 . H3071 . 119.5 no
C308 . C307 . H3071 . 119.9 no
C307 . C308 . C309 . 120.79(13) yes
C307 . C308 . H3081 . 120.5 no
C309 . C308 . H3081 . 118.7 no
C308 . C309 . C304 . 118.69(13) yes
C308 . C309 . H3091 . 120.9 no
C304 . C309 . H3091 . 120.4 no
C303 . C310 . H3102 . 110.0 no
C303 . C310 . H3103 . 108.7 no
H3102 . C310 . H3103 . 108.6 no
C303 . C310 . H3101 . 110.2 no
H3102 . C310 . H3101 . 109.5 no
H3103 . C310 . H3101 . 109.8 no
C303 . C311 . H3113 . 107.9 no
C303 . C311 . H3111 . 109.4 no
H3113 . C311 . H3111 . 108.8 no
C303 . C311 . H3112 . 110.5 no
H3113 . C311 . H3112 . 111.2 no
H3111 . C311 . H3112 . 109.1 no
C301 . C312 . H3121 . 107.3 no
C301 . C312 . H3123 . 108.7 no
H3121 . C312 . H3123 . 109.3 no
C301 . C312 . H3122 . 109.7 no
H3121 . C312 . H3122 . 111.3 no
H3123 . C312 . H3122 . 110.4 no
C402 . N401 . C406 . 111.71(9) yes
C402 . N401 . C410 . 105.49(8) yes
C406 . N401 . C410 . 111.18(9) yes
C402 . N401 . C414 . 111.70(9) yes
C406 . N401 . C414 . 104.87(9) yes
C410 . N401 . C414 . 112.03(9) yes
N401 . C402 . C403 . 115.66(9) yes
N401 . C402 . H4022 . 107.7 no
C403 . C402 . H4022 . 109.9 no
N401 . C402 . H4021 . 105.8 no
C403 . C402 . H4021 . 108.7 no
H4022 . C402 . H4021 . 108.9 no
C402 . C403 . C404 . 110.26(11) yes
C402 . C403 . H4032 . 110.6 no
C404 . C403 . H4032 . 110.4 no
C402 . C403 . H4031 . 110.3 no
C404 . C403 . H4031 . 106.9 no
H4032 . C403 . H4031 . 108.3 no
C403 . C404 . C405 . 112.09(13) yes
C403 . C404 . H4041 . 106.8 no
C405 . C404 . H4041 . 110.9 no
C403 . C404 . H4042 . 107.3 no
C405 . C404 . H4042 . 110.3 no
H4041 . C404 . H4042 . 109.3 no
C404 . C405 . H4052 . 111.1 no
C404 . C405 . H4053 . 110.1 no
H4052 . C405 . H4053 . 109.2 no
C404 . C405 . H4051 . 111.1 no
H4052 . C405 . H4051 . 106.4 no
H4053 . C405 . H4051 . 108.9 no
N401 . C406 . C407 . 115.71(11) yes
N401 . C406 . H4062 . 106.8 no
C407 . C406 . H4062 . 109.1 no
N401 . C406 . H4061 . 106.1 no
C407 . C406 . H4061 . 108.8 no
H4062 . C406 . H4061 . 110.3 no
C406 . C407 . C408 . 109.98(13) yes
C406 . C407 . H4072 . 112.5 no
C408 . C407 . H4072 . 109.5 no
C406 . C407 . H4071 . 114.0 no
C408 . C407 . H4071 . 108.4 no
H4072 . C407 . H4071 . 102.1 no
C407 . C408 . C409 . 111.45(15) yes
C407 . C408 . H4081 . 109.2 no
C409 . C408 . H4081 . 110.0 no
C407 . C408 . H4082 . 110.3 no
C409 . C408 . H4082 . 103.1 no
H4081 . C408 . H4082 . 112.7 no
C408 . C409 . H4091 . 108.6 no
C408 . C409 . H4093 . 111.8 no
H4091 . C409 . H4093 . 108.8 no
C408 . C409 . H4092 . 111.9 no
H4091 . C409 . H4092 . 107.3 no
H4093 . C409 . H4092 . 108.3 no
N401 . C410 . C411 . 116.08(9) yes
N401 . C410 . H4102 . 107.5 no
C411 . C410 . H4102 . 110.7 no
N401 . C410 . H4101 . 106.1 no
C411 . C410 . H4101 . 109.1 no
H4102 . C410 . H4101 . 106.8 no
C410 . C411 . C412 . 109.65(10) yes
C410 . C411 . H4111 . 109.6 no
C412 . C411 . H4111 . 109.1 no
C410 . C411 . H4112 . 109.7 no
C412 . C411 . H4112 . 109.1 no
H4111 . C411 . H4112 . 109.7 no
C411 . C412 . C413 . 112.05(11) yes
C411 . C412 . H4121 . 109.9 no
C413 . C412 . H4121 . 109.6 no
C411 . C412 . H4122 . 108.3 no
C413 . C412 . H4122 . 107.7 no
H4121 . C412 . H4122 . 109.1 no
C412 . C413 . H4131 . 111.3 no
C412 . C413 . H4132 . 110.7 no
H4131 . C413 . H4132 . 109.2 no
C412 . C413 . H4133 . 108.7 no
H4131 . C413 . H4133 . 108.1 no
H4132 . C413 . H4133 . 108.7 no
N401 . C414 . C415 . 116.51(10) yes
N401 . C414 . H4141 . 105.8 no
C415 . C414 . H4141 . 110.9 no
N401 . C414 . H4142 . 107.0 no
C415 . C414 . H4142 . 108.4 no
H4141 . C414 . H4142 . 107.9 no
C414 . C415 . C416 . 115.87(15) yes
C414 . C415 . H4151 . 108.6 no
C416 . C415 . H4151 . 106.7 no
C414 . C415 . H4152 . 108.5 no
C416 . C415 . H4152 . 109.4 no
H4151 . C415 . H4152 . 107.6 no
C414 . C415 . C418 . 96.4(2) yes
C414 . C415 . H4153 . 111.1 no
C418 . C415 . H4153 . 116.6 no
C414 . C415 . H4154 . 112.0 no
C418 . C415 . H4154 . 111.1 no
H4153 . C415 . H4154 . 109.2 no
C415 . C416 . C417 . 110.6(2) yes
C415 . C416 . H4161 . 112.7 no
C417 . C416 . H4161 . 109.3 no
C415 . C416 . H4162 . 107.4 no
C417 . C416 . H4162 . 107.4 no
H4161 . C416 . H4162 . 109.2 no
C416 . C417 . H4172 . 109.1 no
C416 . C417 . H4173 . 109.6 no
H4172 . C417 . H4173 . 110.0 no
C416 . C417 . H4171 . 109.0 no
H4172 . C417 . H4171 . 106.7 no
H4173 . C417 . H4171 . 112.3 no
C415 . C418 . C419 . 107.6(3) yes
C415 . C418 . H4181 . 109.0 no
C419 . C418 . H4181 . 110.6 no
C415 . C418 . H4182 . 111.9 no
C419 . C418 . H4182 . 109.4 no
H4181 . C418 . H4182 . 108.3 no
C418 . C419 . H4191 . 109.5 no
C418 . C419 . H4192 . 111.2 no
H4191 . C419 . H4192 . 109.4 no
C418 . C419 . H4193 . 108.9 no
H4191 . C419 . H4193 . 109.7 no
H4192 . C419 . H4193 . 108.1 no
C101 . O1 . H11 . 108.7 no
C201 . O2 . H21 . 108.7 no
C301 . O3 . H31 . 110.2 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C312 . H3123 . O4 . 134.82 0.964 2.590 3.339(2) yes
C402 . H4021 . O1 2_664 139.17 0.953 2.466 3.247(2) yes
C404 . H4042 . O1 2_664 141.29 1.006 2.455 3.301(2) yes
C414 . H4141 . O102 2_564 136.62 0.974 2.576 3.352(2) yes
C415 . H4151 . O3 1_655 158.83 0.994 2.593 3.539(2) yes
C406 . H4062 . O2 1_565 147.33 0.948 2.371 3.210(2) yes
C410 . H4101 . O3 1_655 159.59 0.964 2.421 3.342(2) yes
C411 . H4112 . O4 . 154.49 0.959 2.520 3.410(2) yes
C417 . H4182 . C414 . 137.0 0.960 2.463 3.232(2) yes
C416 . H4162 . O4 . 151.02 0.991 2.593 3.494(2) yes
O4 . H42 . O302 . 154.28 0.857 2.242 3.037(2) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 24/04/13 at 11:32:31
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
CONT EXTPARAM 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE O   (   4,X'S) H   (  42,X'S) H   (  41,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 107,X'S) H   (1071,X'S) 
RIDE C   ( 108,X'S) H   (1081,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) 
RIDE C   ( 110,X'S) H   (1103,X'S) H   (1101,X'S) H   (1102,X'S) 
RIDE C   ( 111,X'S) H   (1112,X'S) H   (1111,X'S) H   (1113,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) H   (1123,X'S) H   (1122,X'S) 
RIDE C   ( 206,X'S) H   (2061,X'S) 
RIDE C   ( 207,X'S) H   (2071,X'S) 
RIDE C   ( 208,X'S) H   (2081,X'S) 
RIDE C   ( 209,X'S) H   (2091,X'S) 
RIDE C   ( 210,X'S) H   (2103,X'S) H   (2101,X'S) H   (2102,X'S) 
RIDE C   ( 211,X'S) H   (2111,X'S) H   (2113,X'S) H   (2112,X'S) 
RIDE C   ( 212,X'S) H   (2122,X'S) H   (2123,X'S) H   (2121,X'S) 
RIDE C   ( 306,X'S) H   (3061,X'S) 
RIDE C   ( 307,X'S) H   (3071,X'S) 
RIDE C   ( 308,X'S) H   (3081,X'S) 
RIDE C   ( 309,X'S) H   (3091,X'S) 
RIDE C   ( 310,X'S) H   (3102,X'S) H   (3103,X'S) H   (3101,X'S) 
RIDE C   ( 311,X'S) H   (3113,X'S) H   (3111,X'S) H   (3112,X'S) 
RIDE C   ( 312,X'S) H   (3121,X'S) H   (3123,X'S) H   (3122,X'S) 
RIDE C   ( 402,X'S) H   (4022,X'S) H   (4021,X'S) 
RIDE C   ( 403,X'S) H   (4032,X'S) H   (4031,X'S) 
RIDE C   ( 404,X'S) H   (4041,X'S) H   (4042,X'S) 
RIDE C   ( 405,X'S) H   (4052,X'S) H   (4053,X'S) H   (4051,X'S) 
RIDE C   ( 406,X'S) H   (4062,X'S) H   (4061,X'S) 
RIDE C   ( 407,X'S) H   (4072,X'S) H   (4071,X'S) 
RIDE C   ( 408,X'S) H   (4081,X'S) H   (4082,X'S) 
RIDE C   ( 409,X'S) H   (4091,X'S) H   (4093,X'S) H   (4092,X'S) 
RIDE C   ( 410,X'S) H   (4102,X'S) H   (4101,X'S) 
RIDE C   ( 411,X'S) H   (4111,X'S) H   (4112,X'S) 
RIDE C   ( 412,X'S) H   (4121,X'S) H   (4122,X'S) 
RIDE C   ( 413,X'S) H   (4131,X'S) H   (4132,X'S) H   (4133,X'S) 
RIDE C   ( 414,X'S) H   (4141,X'S) H   (4142,X'S) 
RIDE C   ( 415,X'S) H   (4151,X'S) H   (4152,X'S) 
CONT H   (4153,X'S) H   (4154,X'S) 
RIDE C   ( 416,X'S) H   (4161,X'S) H   (4162,X'S) 
RIDE C   ( 417,X'S) H   (4172,X'S) H   (4173,X'S) H   (4171,X'S) 
RIDE C   ( 418,X'S) H   (4181,X'S) H   (4182,X'S) 
RIDE C   ( 419,X'S) H   (4191,X'S) H   (4192,X'S) H   (4193,X'S) 
RIDE O   (   1,X'S) H   (  11,X'S) 
RIDE O   (   2,X'S) H   (  21,X'S) 
RIDE O   (   3,X'S) H   (  31,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 24/04/13 at 11:32:31
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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_2j
_database_code_depnum_ccdc_archive 'CCDC 1401774'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             12-11-30
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 004gwp12
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   14.5683(1)
_cell_length_b                   19.9837(2)
_cell_length_c                   20.7534(2)
_cell_angle_alpha                91.2454(7)
_cell_angle_beta                 94.4191(7)
_cell_angle_gamma                103.9009(8)
_cell_volume                     5842.46(9)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C73 H73 F1 N1 O3 
# Dc =      1.17 Fooo =   2224.00 Mu =      5.61 M =   2062.77
# Found Formula = C73 H78 F1 N1 O3 
# Dc =      1.18 FOOO =   2224.00 Mu =      5.61 M =   2072.85

_chemical_formula_sum            'C73 H78 F1 N1 O3'
_chemical_formula_moiety         '3(C19 H14 O), C16 H36 N, F'
_chemical_compound_source        .
_chemical_formula_weight         1036.43


_cell_measurement_reflns_used    141894
_cell_measurement_theta_min      3
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.21
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_max          0.26

_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2224
_exptl_absorpt_coefficient_mu    0.561

# Sheldrick geometric approximatio 0.87 0.89 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_T_max  0.89
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            227665
_reflns_number_total             24424
_diffrn_reflns_av_R_equivalents  0.026
# Number of reflections with Friedels Law is 24424 
# Theoretical number of reflections is about 41972 


_diffrn_reflns_theta_min         3.060
_diffrn_reflns_theta_max         76.656
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        75.122
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_reflns_limit_h_min              -18
_reflns_limit_h_max              18
_reflns_limit_k_min              -25
_reflns_limit_k_max              25
_reflns_limit_l_min              0
_reflns_limit_l_max              26

_oxford_diffrn_Wilson_B_factor   2.72
_oxford_diffrn_Wilson_scale      0.11

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.30
_refine_diff_density_max         0.52


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         20878
_refine_ls_number_restraints     0
_refine_ls_number_parameters     1406
_oxford_refine_ls_R_factor_ref   0.0429
_refine_ls_wR_factor_ref         0.0976
_refine_ls_goodness_of_fit_ref   0.9862
_refine_ls_shift/su_max          0.0005741
_refine_ls_shift/su_mean         0.0000404


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        20878
_refine_ls_R_factor_all          0.0429
_refine_ls_wR_factor_all         0.0976

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                19535
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_gt          0.0961

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 2.94P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
F1 F 0.61935(5) 0.85750(4) 0.25220(4) 0.0359 1.0000 Uani . . . . . .
F2 F 0.19771(5) 0.41171(5) 0.29033(4) 0.0417 1.0000 Uani . . . . . .
O11 O 0.45609(6) 0.83384(4) 0.29473(4) 0.0282 1.0000 Uani . . . . . .
O12 O 0.51011(6) 0.79247(4) 0.15152(4) 0.0273 1.0000 Uani . . . . . .
O13 O 0.79470(6) 0.91174(4) 0.24144(5) 0.0309 1.0000 Uani . . . . . .
O14 O 0.36029(6) 0.42842(4) 0.25275(4) 0.0285 1.0000 Uani . . . . . .
O15 O 0.02598(6) 0.37027(4) 0.27411(4) 0.0248 1.0000 Uani . . . . . .
O16 O -0.05571(6) 0.30606(4) 0.15706(4) 0.0305 1.0000 Uani . . . . . .
C101 C 0.43484(9) 0.86095(6) 0.35367(6) 0.0257 1.0000 Uani . . . . . .
C102 C 0.47445(9) 0.82896(6) 0.41257(6) 0.0272 1.0000 Uani . . . . . .
C103 C 0.56831(10) 0.83423(7) 0.43346(7) 0.0361 1.0000 Uani . . . . . .
C104 C 0.58839(12) 0.80008(8) 0.48850(8) 0.0449 1.0000 Uani . . . . . .
C105 C 0.51622(12) 0.76217(8) 0.52206(7) 0.0440 1.0000 Uani . . . . . .
C106 C 0.42188(11) 0.75666(7) 0.50122(7) 0.0374 1.0000 Uani . . . . . .
C107 C 0.40110(10) 0.79022(6) 0.44576(6) 0.0291 1.0000 Uani . . . . . .
C108 C 0.30992(9) 0.79335(6) 0.41168(6) 0.0284 1.0000 Uani . . . . . .
C109 C 0.32832(9) 0.83423(6) 0.35819(6) 0.0260 1.0000 Uani . . . . . .
C110 C 0.25541(10) 0.84589(7) 0.31706(7) 0.0332 1.0000 Uani . . . . . .
C111 C 0.16243(10) 0.81616(8) 0.32954(7) 0.0379 1.0000 Uani . . . . . .
C112 C 0.14373(10) 0.77540(7) 0.38256(8) 0.0387 1.0000 Uani . . . . . .
C113 C 0.21703(10) 0.76344(7) 0.42393(7) 0.0358 1.0000 Uani . . . . . .
C114 C 0.46352(9) 0.93981(6) 0.35986(6) 0.0278 1.0000 Uani . . . . . .
C115 C 0.51315(11) 0.97950(7) 0.31417(7) 0.0368 1.0000 Uani . . . . . .
C116 C 0.53611(13) 1.05105(8) 0.32155(8) 0.0480 1.0000 Uani . . . . . .
C117 C 0.50972(13) 1.08338(8) 0.37380(8) 0.0483 1.0000 Uani . . . . . .
C118 C 0.46148(13) 1.04431(8) 0.41987(8) 0.0475 1.0000 Uani . . . . . .
C119 C 0.43912(12) 0.97333(7) 0.41305(7) 0.0411 1.0000 Uani . . . . . .
C120 C 0.50458(9) 0.82856(6) 0.09374(6) 0.0246 1.0000 Uani . . . . . .
C121 C 0.60209(8) 0.86367(6) 0.07264(6) 0.0243 1.0000 Uani . . . . . .
C122 C 0.66987(9) 0.91684(7) 0.10439(6) 0.0279 1.0000 Uani . . . . . .
C123 C 0.75475(9) 0.94084(7) 0.07660(7) 0.0351 1.0000 Uani . . . . . .
C124 C 0.77100(10) 0.91248(8) 0.01826(7) 0.0399 1.0000 Uani . . . . . .
C125 C 0.70247(10) 0.85947(8) -0.01406(7) 0.0365 1.0000 Uani . . . . . .
C126 C 0.61746(9) 0.83533(7) 0.01333(6) 0.0284 1.0000 Uani . . . . . .
C127 C 0.53224(9) 0.78139(7) -0.00917(6) 0.0299 1.0000 Uani . . . . . .
C128 C 0.46676(9) 0.77575(6) 0.03755(6) 0.0277 1.0000 Uani . . . . . .
C129 C 0.38039(10) 0.72804(7) 0.02904(7) 0.0349 1.0000 Uani . . . . . .
C130 C 0.35929(11) 0.68611(8) -0.02738(8) 0.0427 1.0000 Uani . . . . . .
C131 C 0.42336(11) 0.69305(8) -0.07444(8) 0.0439 1.0000 Uani . . . . . .
C132 C 0.51055(11) 0.74022(8) -0.06583(7) 0.0387 1.0000 Uani . . . . . .
C133 C 0.44273(8) 0.88043(6) 0.09774(6) 0.0241 1.0000 Uani . . . . . .
C134 C 0.39453(10) 0.88666(7) 0.15146(6) 0.0336 1.0000 Uani . . . . . .
C135 C 0.33905(12) 0.93441(9) 0.15307(7) 0.0435 1.0000 Uani . . . . . .
C136 C 0.33056(10) 0.97554(7) 0.10161(7) 0.0361 1.0000 Uani . . . . . .
C137 C 0.37837(9) 0.96941(7) 0.04772(7) 0.0323 1.0000 Uani . . . . . .
C138 C 0.43416(9) 0.92250(7) 0.04603(6) 0.0295 1.0000 Uani . . . . . .
C139 C 0.86191(9) 0.87399(6) 0.26143(7) 0.0302 1.0000 Uani . . . . . .
C140 C 0.88268(10) 0.87826(7) 0.33487(7) 0.0334 1.0000 Uani . . . . . .
C141 C 0.82260(11) 0.85150(7) 0.38114(7) 0.0396 1.0000 Uani . . . . . .
C142 C 0.85635(14) 0.86421(8) 0.44595(8) 0.0525 1.0000 Uani . . . . . .
C143 C 0.94928(16) 0.90324(9) 0.46274(9) 0.0623 1.0000 Uani . . . . . .
C144 C 1.00863(13) 0.92968(9) 0.41656(10) 0.0540 1.0000 Uani . . . . . .
C145 C 0.97530(11) 0.91734(7) 0.35232(8) 0.0427 1.0000 Uani . . . . . .
C146 C 1.02189(10) 0.93885(7) 0.29313(9) 0.0421 1.0000 Uani . . . . . .
C147 C 0.95814(9) 0.91293(7) 0.23983(8) 0.0359 1.0000 Uani . . . . . .
C148 C 0.98457(11) 0.92315(7) 0.17719(9) 0.0443 1.0000 Uani . . . . . .
C149 C 1.07563(12) 0.96134(8) 0.16830(11) 0.0542 1.0000 Uani . . . . . .
C150 C 1.13846(12) 0.98820(9) 0.22054(11) 0.0584 1.0000 Uani . . . . . .
C151 C 1.11397(11) 0.97765(8) 0.28318(11) 0.0561 1.0000 Uani . . . . . .
C152 C 0.83492(9) 0.80008(6) 0.23232(7) 0.0292 1.0000 Uani . . . . . .
C153 C 0.76752(10) 0.78241(7) 0.17999(7) 0.0336 1.0000 Uani . . . . . .
C154 C 0.74454(11) 0.71603(7) 0.15192(7) 0.0387 1.0000 Uani . . . . . .
C155 C 0.78912(11) 0.66694(7) 0.17586(8) 0.0412 1.0000 Uani . . . . . .
C156 C 0.85678(11) 0.68406(7) 0.22784(8) 0.0416 1.0000 Uani . . . . . .
C157 C 0.87972(10) 0.75025(7) 0.25598(8) 0.0360 1.0000 Uani . . . . . .
C158 C 0.42158(8) 0.38946(6) 0.27920(6) 0.0254 1.0000 Uani . . . . . .
C159 C 0.43657(9) 0.39591(6) 0.35311(6) 0.0275 1.0000 Uani . . . . . .
C160 C 0.36967(10) 0.37883(7) 0.39753(7) 0.0326 1.0000 Uani . . . . . .
C161 C 0.39969(11) 0.38949(8) 0.46307(7) 0.0419 1.0000 Uani . . . . . .
C162 C 0.49458(12) 0.41662(8) 0.48347(8) 0.0462 1.0000 Uani . . . . . .
C163 C 0.56151(11) 0.43444(8) 0.43926(8) 0.0422 1.0000 Uani . . . . . .
C164 C 0.53222(9) 0.42415(7) 0.37361(7) 0.0320 1.0000 Uani . . . . . .
C165 C 0.58529(9) 0.44051(6) 0.31631(7) 0.0324 1.0000 Uani . . . . . .
C166 C 0.52186(9) 0.42232(6) 0.26108(7) 0.0286 1.0000 Uani . . . . . .
C167 C 0.55218(10) 0.43465(7) 0.20004(7) 0.0353 1.0000 Uani . . . . . .
C168 C 0.64784(11) 0.46592(7) 0.19480(9) 0.0442 1.0000 Uani . . . . . .
C169 C 0.71073(10) 0.48317(7) 0.24955(9) 0.0467 1.0000 Uani . . . . . .
C170 C 0.68060(10) 0.47049(7) 0.31051(9) 0.0415 1.0000 Uani . . . . . .
C171 C 0.39170(8) 0.31355(6) 0.25491(6) 0.0246 1.0000 Uani . . . . . .
C172 C 0.30859(9) 0.28814(7) 0.21580(6) 0.0309 1.0000 Uani . . . . . .
C173 C 0.28542(11) 0.22001(7) 0.19176(7) 0.0379 1.0000 Uani . . . . . .
C174 C 0.34440(11) 0.17692(7) 0.20659(7) 0.0401 1.0000 Uani . . . . . .
C175 C 0.42696(11) 0.20178(7) 0.24638(8) 0.0392 1.0000 Uani . . . . . .
C176 C 0.45012(9) 0.26928(7) 0.27052(7) 0.0320 1.0000 Uani . . . . . .
C177 C -0.02015(8) 0.38010(6) 0.32984(6) 0.0221 1.0000 Uani . . . . . .
C178 C 0.01826(8) 0.34971(6) 0.39036(6) 0.0227 1.0000 Uani . . . . . .
C179 C 0.10865(9) 0.36809(7) 0.42166(6) 0.0277 1.0000 Uani . . . . . .
C180 C 0.12750(10) 0.33364(7) 0.47692(6) 0.0321 1.0000 Uani . . . . . .
C181 C 0.05785(10) 0.28165(7) 0.49989(6) 0.0325 1.0000 Uani . . . . . .
C182 C -0.03297(10) 0.26318(7) 0.46866(6) 0.0295 1.0000 Uani . . . . . .
C183 C -0.05278(9) 0.29849(6) 0.41428(6) 0.0244 1.0000 Uani . . . . . .
C184 C -0.14136(9) 0.29197(6) 0.37277(6) 0.0239 1.0000 Uani . . . . . .
C185 C -0.12305(8) 0.33730(6) 0.32236(6) 0.0227 1.0000 Uani . . . . . .
C186 C -0.19432(9) 0.34149(6) 0.27576(6) 0.0264 1.0000 Uani . . . . . .
C187 C -0.28537(9) 0.30059(7) 0.28061(7) 0.0306 1.0000 Uani . . . . . .
C188 C -0.30396(9) 0.25635(7) 0.33122(7) 0.0316 1.0000 Uani . . . . . .
C189 C -0.23232(9) 0.25126(6) 0.37770(6) 0.0286 1.0000 Uani . . . . . .
C190 C -0.01887(8) 0.45622(6) 0.34364(6) 0.0237 1.0000 Uani . . . . . .
C191 C 0.02483(10) 0.50809(7) 0.30523(6) 0.0310 1.0000 Uani . . . . . .
C192 C 0.02268(11) 0.57628(7) 0.31885(8) 0.0402 1.0000 Uani . . . . . .
C193 C -0.02300(11) 0.59288(7) 0.37031(8) 0.0404 1.0000 Uani . . . . . .
C194 C -0.06545(11) 0.54163(7) 0.40941(8) 0.0417 1.0000 Uani . . . . . .
C195 C -0.06327(10) 0.47401(7) 0.39625(7) 0.0351 1.0000 Uani . . . . . .
C196 C -0.03124(9) 0.33444(7) 0.09638(6) 0.0273 1.0000 Uani . . . . . .
C197 C 0.07545(9) 0.35082(7) 0.08884(6) 0.0271 1.0000 Uani . . . . . .
C198 C 0.14815(9) 0.39727(7) 0.12481(6) 0.0318 1.0000 Uani . . . . . .
C199 C 0.24079(10) 0.40356(8) 0.10892(7) 0.0393 1.0000 Uani . . . . . .
C200 C 0.26010(10) 0.36424(9) 0.05832(8) 0.0439 1.0000 Uani . . . . . .
C201 C 0.18765(11) 0.31765(8) 0.02204(7) 0.0412 1.0000 Uani . . . . . .
C202 C 0.09488(10) 0.31140(7) 0.03756(6) 0.0321 1.0000 Uani . . . . . .
C203 C 0.00487(10) 0.26648(7) 0.00920(7) 0.0355 1.0000 Uani . . . . . .
C204 C -0.06850(10) 0.27770(7) 0.04412(6) 0.0315 1.0000 Uani . . . . . .
C205 C -0.16093(11) 0.24029(8) 0.02918(7) 0.0402 1.0000 Uani . . . . . .
C206 C -0.17963(12) 0.19226(9) -0.02263(9) 0.0524 1.0000 Uani . . . . . .
C207 C -0.10738(14) 0.18251(9) -0.05823(9) 0.0568 1.0000 Uani . . . . . .
C208 C -0.01417(13) 0.21890(9) -0.04274(8) 0.0490 1.0000 Uani . . . . . .
C209 C -0.06968(9) 0.39843(7) 0.08376(6) 0.0304 1.0000 Uani . . . . . .
C210 C -0.07503(11) 0.44350(8) 0.13419(7) 0.0401 1.0000 Uani . . . . . .
C211 C -0.10616(13) 0.50301(9) 0.12268(9) 0.0532 1.0000 Uani . . . . . .
C212 C -0.13256(12) 0.51845(9) 0.06110(10) 0.0574 1.0000 Uani . . . . . .
C213 C -0.12733(14) 0.47456(10) 0.01088(10) 0.0629 1.0000 Uani . . . . . .
C214 C -0.09597(13) 0.41500(9) 0.02161(8) 0.0489 1.0000 Uani . . . . . .
N501 N 0.39356(8) 0.62633(5) 0.25215(5) 0.0298 1.0000 Uani . . . . . .
C502 C 0.40806(10) 0.58019(6) 0.19655(7) 0.0320 1.0000 Uani . . . . . .
C503 C 0.47422(10) 0.61455(7) 0.14753(7) 0.0341 1.0000 Uani . . . . . .
C504 C 0.46065(11) 0.56716(7) 0.08719(7) 0.0400 1.0000 Uani . . . . . .
C505 C 0.53697(13) 0.59150(8) 0.04125(8) 0.0476 1.0000 Uani . . . . . .
C506 C 0.48760(10) 0.66945(6) 0.28295(7) 0.0326 1.0000 Uani . . . . . .
C507 C 0.55709(10) 0.62999(7) 0.31036(7) 0.0357 1.0000 Uani . . . . . .
C508 C 0.64785(11) 0.68117(8) 0.33734(8) 0.0419 1.0000 Uani . . . . . .
C509 C 0.72310(12) 0.64693(9) 0.36535(8) 0.0472 1.0000 Uani . . . . . .
C510 C 0.34140(10) 0.57764(6) 0.30012(6) 0.0313 1.0000 Uani . . . . . .
C511 C 0.30912(10) 0.61050(7) 0.35815(7) 0.0332 1.0000 Uani . . . . . .
C512 C 0.26507(10) 0.55260(7) 0.40149(6) 0.0337 1.0000 Uani . . . . . .
C513 C 0.21872(11) 0.57707(8) 0.45754(7) 0.0421 1.0000 Uani . . . . . .
C514 C 0.33713(10) 0.67721(7) 0.22857(7) 0.0337 1.0000 Uani . . . . . .
C515 C 0.23974(11) 0.64581(8) 0.19568(7) 0.0417 1.0000 Uani . . . . . .
C516 C 0.18237(12) 0.69886(10) 0.18863(10) 0.0561 1.0000 Uani . . . . . .
C517 C 0.08371(14) 0.67016(13) 0.15643(9) 0.0686 1.0000 Uani . . . . . .
N521 N 0.91099(8) 0.12775(5) 0.25054(5) 0.0295 1.0000 Uani . . . . . .
C522 C 0.95255(10) 0.09809(7) 0.19449(7) 0.0356 1.0000 Uani . . . . . .
C523 C 0.99814(12) 0.15182(8) 0.14763(8) 0.0446 1.0000 Uani . . . . . .
C524 C 1.04692(11) 0.12134(8) 0.09573(8) 0.0443 1.0000 Uani . . . . . .
C525 C 0.97611(13) 0.06964(11) 0.05057(9) 0.0591 1.0000 Uani . . . . . .
C526 C 0.98754(10) 0.18358(7) 0.28712(7) 0.0327 1.0000 Uani . . . . . .
C527 C 1.07731(11) 0.16121(8) 0.30862(8) 0.0419 1.0000 Uani . . . . . .
C528 C 1.14766(11) 0.21693(8) 0.34841(8) 0.0448 1.0000 Uani . . . . . .
C529 C 1.23624(12) 0.19414(9) 0.37079(8) 0.0501 1.0000 Uani . . . . . .
C530 C 0.87384(10) 0.06891(6) 0.29456(7) 0.0321 1.0000 Uani . . . . . .
C531 C 0.82498(11) 0.08747(7) 0.35193(7) 0.0366 1.0000 Uani . . . . . .
C532 C 0.79489(12) 0.02516(8) 0.39314(8) 0.0460 1.0000 Uani . . . . . .
C533 C 0.74752(14) 0.04120(11) 0.45190(9) 0.0605 1.0000 Uani . . . . . .
C534 C 0.83161(10) 0.16069(7) 0.22590(7) 0.0315 1.0000 Uani . . . . . .
C535 C 0.74787(11) 0.11178(8) 0.18870(8) 0.0421 1.0000 Uani . . . . . .
C536 C 0.66803(11) 0.14674(8) 0.17063(8) 0.0419 1.0000 Uani . . . . . .
C537 C 0.58118(14) 0.09706(11) 0.13624(9) 0.0623 1.0000 Uani . . . . . .
H1031 H 0.6190 0.8610 0.4103 0.0441 1.0000 Uiso R . . . . .
H1041 H 0.6529 0.8023 0.5036 0.0543 1.0000 Uiso R . . . . .
H1051 H 0.5314 0.7393 0.5595 0.0531 1.0000 Uiso R . . . . .
H1061 H 0.3717 0.7298 0.5237 0.0439 1.0000 Uiso R . . . . .
H1101 H 0.2687 0.8736 0.2804 0.0400 1.0000 Uiso R . . . . .
H1111 H 0.1117 0.8227 0.3015 0.0455 1.0000 Uiso R . . . . .
H1121 H 0.0793 0.7559 0.3905 0.0451 1.0000 Uiso R . . . . .
H1131 H 0.2035 0.7342 0.4604 0.0433 1.0000 Uiso R . . . . .
H1151 H 0.5310 0.9572 0.2767 0.0446 1.0000 Uiso R . . . . .
H1161 H 0.5702 1.0777 0.2890 0.0587 1.0000 Uiso R . . . . .
H1171 H 0.5244 1.1330 0.3785 0.0578 1.0000 Uiso R . . . . .
H1181 H 0.4428 1.0659 0.4557 0.0570 1.0000 Uiso R . . . . .
H1191 H 0.4055 0.9468 0.4450 0.0497 1.0000 Uiso R . . . . .
H1221 H 0.6594 0.9362 0.1444 0.0327 1.0000 Uiso R . . . . .
H1231 H 0.8027 0.9763 0.0985 0.0420 1.0000 Uiso R . . . . .
H1241 H 0.8303 0.9306 0.0002 0.0481 1.0000 Uiso R . . . . .
H1251 H 0.7138 0.8402 -0.0543 0.0442 1.0000 Uiso R . . . . .
H1291 H 0.3352 0.7246 0.0608 0.0415 1.0000 Uiso R . . . . .
H1301 H 0.3006 0.6534 -0.0339 0.0507 1.0000 Uiso R . . . . .
H1311 H 0.4069 0.6641 -0.1132 0.0531 1.0000 Uiso R . . . . .
H1321 H 0.5548 0.7445 -0.0982 0.0470 1.0000 Uiso R . . . . .
H1341 H 0.4011 0.8591 0.1871 0.0410 1.0000 Uiso R . . . . .
H1351 H 0.3063 0.9390 0.1907 0.0528 1.0000 Uiso R . . . . .
H1361 H 0.2923 1.0083 0.1024 0.0428 1.0000 Uiso R . . . . .
H1371 H 0.3729 0.9972 0.0126 0.0387 1.0000 Uiso R . . . . .
H1381 H 0.4675 0.9183 0.0096 0.0361 1.0000 Uiso R . . . . .
H1411 H 0.7598 0.8260 0.3698 0.0452 1.0000 Uiso R . . . . .
H1421 H 0.8149 0.8473 0.4770 0.0595 1.0000 Uiso R . . . . .
H1431 H 0.9676 0.9108 0.5061 0.0750 1.0000 Uiso R . . . . .
H1441 H 1.0735 0.9565 0.4298 0.0653 1.0000 Uiso R . . . . .
H1481 H 0.9382 0.9015 0.1393 0.0550 1.0000 Uiso R . . . . .
H1491 H 1.0974 0.9686 0.1231 0.0668 1.0000 Uiso R . . . . .
H1501 H 1.2021 1.0149 0.2129 0.0697 1.0000 Uiso R . . . . .
H1511 H 1.1517 0.9917 0.3213 0.0647 1.0000 Uiso R . . . . .
H1531 H 0.7362 0.8159 0.1639 0.0395 1.0000 Uiso R . . . . .
H1541 H 0.6971 0.7055 0.1157 0.0462 1.0000 Uiso R . . . . .
H1551 H 0.7740 0.6213 0.1565 0.0493 1.0000 Uiso R . . . . .
H1561 H 0.8875 0.6503 0.2451 0.0504 1.0000 Uiso R . . . . .
H1571 H 0.9261 0.7618 0.2922 0.0435 1.0000 Uiso R . . . . .
H1601 H 0.3039 0.3606 0.3841 0.0377 1.0000 Uiso R . . . . .
H1611 H 0.3536 0.3775 0.4951 0.0506 1.0000 Uiso R . . . . .
H1621 H 0.5139 0.4240 0.5295 0.0557 1.0000 Uiso R . . . . .
H1631 H 0.6267 0.4541 0.4526 0.0506 1.0000 Uiso R . . . . .
H1671 H 0.5083 0.4229 0.1623 0.0404 1.0000 Uiso R . . . . .
H1681 H 0.6678 0.4747 0.1533 0.0529 1.0000 Uiso R . . . . .
H1691 H 0.7767 0.5037 0.2451 0.0557 1.0000 Uiso R . . . . .
H1701 H 0.7242 0.4815 0.3483 0.0505 1.0000 Uiso R . . . . .
H1721 H 0.2678 0.3183 0.2050 0.0377 1.0000 Uiso R . . . . .
H1731 H 0.2276 0.2040 0.1638 0.0469 1.0000 Uiso R . . . . .
H1741 H 0.3291 0.1306 0.1890 0.0485 1.0000 Uiso R . . . . .
H1751 H 0.4684 0.1729 0.2578 0.0476 1.0000 Uiso R . . . . .
H1761 H 0.5072 0.2857 0.2982 0.0387 1.0000 Uiso R . . . . .
H1791 H 0.1575 0.4028 0.4049 0.0330 1.0000 Uiso R . . . . .
H1801 H 0.1898 0.3458 0.4982 0.0388 1.0000 Uiso R . . . . .
H1811 H 0.0725 0.2585 0.5371 0.0387 1.0000 Uiso R . . . . .
H1821 H -0.0808 0.2268 0.4840 0.0343 1.0000 Uiso R . . . . .
H1861 H -0.1824 0.3721 0.2408 0.0317 1.0000 Uiso R . . . . .
H1871 H -0.3354 0.3033 0.2493 0.0370 1.0000 Uiso R . . . . .
H1881 H -0.3673 0.2289 0.3339 0.0373 1.0000 Uiso R . . . . .
H1891 H -0.2446 0.2206 0.4123 0.0337 1.0000 Uiso R . . . . .
H1911 H 0.0568 0.4971 0.2694 0.0370 1.0000 Uiso R . . . . .
H1921 H 0.0544 0.6118 0.2921 0.0493 1.0000 Uiso R . . . . .
H1931 H -0.0254 0.6396 0.3789 0.0478 1.0000 Uiso R . . . . .
H1941 H -0.0955 0.5534 0.4458 0.0508 1.0000 Uiso R . . . . .
H1951 H -0.0925 0.4387 0.4238 0.0428 1.0000 Uiso R . . . . .
H1981 H 0.1353 0.4248 0.1606 0.0380 1.0000 Uiso R . . . . .
H1991 H 0.2923 0.4351 0.1339 0.0476 1.0000 Uiso R . . . . .
H2001 H 0.3246 0.3691 0.0490 0.0531 1.0000 Uiso R . . . . .
H2011 H 0.2003 0.2895 -0.0122 0.0489 1.0000 Uiso R . . . . .
H2051 H -0.2113 0.2470 0.0544 0.0474 1.0000 Uiso R . . . . .
H2061 H -0.2435 0.1660 -0.0331 0.0632 1.0000 Uiso R . . . . .
H2071 H -0.1213 0.1493 -0.0944 0.0681 1.0000 Uiso R . . . . .
H2081 H 0.0360 0.2107 -0.0669 0.0587 1.0000 Uiso R . . . . .
H2101 H -0.0575 0.4334 0.1776 0.0492 1.0000 Uiso R . . . . .
H2111 H -0.1104 0.5337 0.1582 0.0656 1.0000 Uiso R . . . . .
H2121 H -0.1542 0.5595 0.0530 0.0696 1.0000 Uiso R . . . . .
H2131 H -0.1441 0.4846 -0.0316 0.0777 1.0000 Uiso R . . . . .
H2141 H -0.0915 0.3849 -0.0124 0.0587 1.0000 Uiso R . . . . .
H5021 H 0.4310 0.5428 0.2164 0.0371 1.0000 Uiso R . . . . .
H5022 H 0.3440 0.5613 0.1755 0.0364 1.0000 Uiso R . . . . .
H5031 H 0.4623 0.6588 0.1356 0.0405 1.0000 Uiso R . . . . .
H5032 H 0.5414 0.6238 0.1661 0.0415 1.0000 Uiso R . . . . .
H5041 H 0.3975 0.5652 0.0644 0.0472 1.0000 Uiso R . . . . .
H5042 H 0.4619 0.5206 0.1004 0.0478 1.0000 Uiso R . . . . .
H5052 H 0.5229 0.5636 0.0009 0.0700 1.0000 Uiso R . . . . .
H5053 H 0.5410 0.6394 0.0319 0.0693 1.0000 Uiso R . . . . .
H5051 H 0.5988 0.5875 0.0611 0.0700 1.0000 Uiso R . . . . .
H5061 H 0.4714 0.6977 0.3166 0.0376 1.0000 Uiso R . . . . .
H5062 H 0.5147 0.6989 0.2492 0.0380 1.0000 Uiso R . . . . .
H5071 H 0.5303 0.6008 0.3449 0.0439 1.0000 Uiso R . . . . .
H5072 H 0.5724 0.6000 0.2765 0.0428 1.0000 Uiso R . . . . .
H5081 H 0.6314 0.7105 0.3703 0.0505 1.0000 Uiso R . . . . .
H5082 H 0.6717 0.7097 0.3025 0.0502 1.0000 Uiso R . . . . .
H5093 H 0.7787 0.6822 0.3842 0.0698 1.0000 Uiso R . . . . .
H5092 H 0.6981 0.6152 0.3989 0.0703 1.0000 Uiso R . . . . .
H5091 H 0.7438 0.6205 0.3306 0.0696 1.0000 Uiso R . . . . .
H5101 H 0.3849 0.5490 0.3141 0.0374 1.0000 Uiso R . . . . .
H5102 H 0.2865 0.5486 0.2756 0.0368 1.0000 Uiso R . . . . .
H5111 H 0.3626 0.6434 0.3824 0.0400 1.0000 Uiso R . . . . .
H5112 H 0.2615 0.6358 0.3443 0.0398 1.0000 Uiso R . . . . .
H5121 H 0.3140 0.5297 0.4178 0.0396 1.0000 Uiso R . . . . .
H5122 H 0.2171 0.5182 0.3754 0.0401 1.0000 Uiso R . . . . .
H5133 H 0.1925 0.5385 0.4841 0.0623 1.0000 Uiso R . . . . .
H5131 H 0.2646 0.6120 0.4852 0.0614 1.0000 Uiso R . . . . .
H5132 H 0.1668 0.5974 0.4418 0.0621 1.0000 Uiso R . . . . .
H5141 H 0.3317 0.7048 0.2666 0.0395 1.0000 Uiso R . . . . .
H5142 H 0.3767 0.7070 0.1993 0.0395 1.0000 Uiso R . . . . .
H5151 H 0.2063 0.6077 0.2196 0.0502 1.0000 Uiso R . . . . .
H5152 H 0.2444 0.6262 0.1527 0.0518 1.0000 Uiso R . . . . .
H5161 H 0.1763 0.7175 0.2333 0.0701 1.0000 Uiso R . . . . .
H5162 H 0.2126 0.7370 0.1648 0.0671 1.0000 Uiso R . . . . .
H5172 H 0.0454 0.7043 0.1589 0.1023 1.0000 Uiso R . . . . .
H5171 H 0.0498 0.6264 0.1746 0.1028 1.0000 Uiso R . . . . .
H5173 H 0.0876 0.6601 0.1108 0.1039 1.0000 Uiso R . . . . .
H5221 H 0.9983 0.0744 0.2149 0.0408 1.0000 Uiso R . . . . .
H5222 H 0.8989 0.0643 0.1759 0.0394 1.0000 Uiso R . . . . .
H5231 H 1.0481 0.1914 0.1732 0.0557 1.0000 Uiso R . . . . .
H5232 H 0.9445 0.1687 0.1259 0.0554 1.0000 Uiso R . . . . .
H5241 H 1.0936 0.0999 0.1169 0.0450 1.0000 Uiso R . . . . .
H5242 H 1.0831 0.1598 0.0705 0.0537 1.0000 Uiso R . . . . .
H5261 H 1.0011 0.2224 0.2601 0.0381 1.0000 Uiso R . . . . .
H5262 H 0.9595 0.1974 0.3237 0.0371 1.0000 Uiso R . . . . .
H5271 H 1.1084 0.1497 0.2703 0.0512 1.0000 Uiso R . . . . .
H5272 H 1.0642 0.1214 0.3374 0.0524 1.0000 Uiso R . . . . .
H5281 H 1.1623 0.2583 0.3207 0.0548 1.0000 Uiso R . . . . .
H5282 H 1.1144 0.2292 0.3873 0.0559 1.0000 Uiso R . . . . .
H5291 H 1.2814 0.2311 0.3988 0.0755 1.0000 Uiso R . . . . .
H5292 H 1.2683 0.1834 0.3336 0.0753 1.0000 Uiso R . . . . .
H5293 H 1.2197 0.1518 0.3930 0.0709 1.0000 Uiso R . . . . .
H5301 H 0.9285 0.0524 0.3098 0.0386 1.0000 Uiso R . . . . .
H5302 H 0.8306 0.0323 0.2665 0.0384 1.0000 Uiso R . . . . .
H5311 H 0.8669 0.1242 0.3785 0.0447 1.0000 Uiso R . . . . .
H5312 H 0.7687 0.1033 0.3371 0.0443 1.0000 Uiso R . . . . .
H5321 H 0.8505 0.0092 0.4065 0.0557 1.0000 Uiso R . . . . .
H5322 H 0.7495 -0.0105 0.3665 0.0565 1.0000 Uiso R . . . . .
H5331 H 0.7305 0.0010 0.4779 0.0899 1.0000 Uiso R . . . . .
H5332 H 0.7884 0.0787 0.4791 0.0892 1.0000 Uiso R . . . . .
H5333 H 0.6899 0.0557 0.4392 0.0898 1.0000 Uiso R . . . . .
H5342 H 0.8587 0.1984 0.1984 0.0378 1.0000 Uiso R . . . . .
H5341 H 0.8107 0.1803 0.2641 0.0355 1.0000 Uiso R . . . . .
H5352 H 0.7672 0.0947 0.1494 0.0531 1.0000 Uiso R . . . . .
H5351 H 0.7206 0.0729 0.2141 0.0510 1.0000 Uiso R . . . . .
H5361 H 0.6918 0.1848 0.1447 0.0525 1.0000 Uiso R . . . . .
H5362 H 0.6492 0.1658 0.2104 0.0505 1.0000 Uiso R . . . . .
H5371 H 0.5326 0.1218 0.1226 0.0929 1.0000 Uiso R . . . . .
H5372 H 0.5987 0.0754 0.0984 0.0946 1.0000 Uiso R . . . . .
H5373 H 0.5526 0.0601 0.1659 0.0953 1.0000 Uiso R . . . . .
H151 H 0.0895 0.3855 0.2809 0.0407 1.0000 Uiso R . . . . .
H131 H 0.7366 0.8897 0.2487 0.0482 1.0000 Uiso R . . . . .
H121 H 0.5470 0.8184 0.1808 0.0428 1.0000 Uiso R . . . . .
H161 H -0.0247 0.3312 0.1886 0.0468 1.0000 Uiso R . . . . .
H141 H 0.3051 0.4178 0.2685 0.0445 1.0000 Uiso R . . . . .
H111 H 0.5157 0.8460 0.2890 0.0444 1.0000 Uiso R . . . . .
H5251 H 1.0075 0.0599 0.0092 0.0894 1.0000 Uiso R . . . . .
H5252 H 0.9677 0.0262 0.0763 0.0857 1.0000 Uiso R . . . . .
H5253 H 0.9136 0.0852 0.0395 0.0898 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       170(9)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          3.079(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O11 . C101 . 1.4126(14) yes
O11 . H111 . 0.863 no
O12 . C120 . 1.4197(14) yes
O12 . H121 . 0.854 no
O13 . C139 . 1.4163(15) yes
O13 . H131 . 0.882 no
O14 . C158 . 1.4079(15) yes
O14 . H141 . 0.871 no
O15 . C177 . 1.4146(14) yes
O15 . H151 . 0.901 no
O16 . C196 . 1.4274(14) yes
O16 . H161 . 0.846 no
C101 . C102 . 1.5292(17) yes
C101 . C109 . 1.5260(17) yes
C101 . C114 . 1.5301(17) yes
C102 . C103 . 1.3806(19) yes
C102 . C107 . 1.3981(18) yes
C103 . C104 . 1.391(2) yes
C103 . H1031 . 0.969 no
C104 . C105 . 1.385(2) yes
C104 . H1041 . 0.957 no
C105 . C106 . 1.386(2) yes
C105 . H1051 . 0.948 no
C106 . C107 . 1.3940(19) yes
C106 . H1061 . 0.956 no
C107 . C108 . 1.4717(19) yes
C108 . C109 . 1.3970(17) yes
C108 . C113 . 1.3871(19) yes
C109 . C110 . 1.3780(19) yes
C110 . C111 . 1.3888(19) yes
C110 . H1101 . 0.955 no
C111 . C112 . 1.388(2) yes
C111 . H1111 . 0.941 no
C112 . C113 . 1.387(2) yes
C112 . H1121 . 0.954 no
C113 . H1131 . 0.970 no
C114 . C115 . 1.3834(18) yes
C114 . C119 . 1.3914(19) yes
C115 . C116 . 1.390(2) yes
C115 . H1151 . 0.971 no
C116 . C117 . 1.376(2) yes
C116 . H1161 . 0.963 no
C117 . C118 . 1.375(2) yes
C117 . H1171 . 0.964 no
C118 . C119 . 1.379(2) yes
C118 . H1181 . 0.942 no
C119 . H1191 . 0.950 no
C120 . C121 . 1.5271(16) yes
C120 . C128 . 1.5314(17) yes
C120 . C133 . 1.5328(17) yes
C121 . C122 . 1.3797(18) yes
C121 . C126 . 1.3996(17) yes
C122 . C123 . 1.3888(18) yes
C122 . H1221 . 0.948 no
C123 . C124 . 1.386(2) yes
C123 . H1231 . 0.947 no
C124 . C125 . 1.388(2) yes
C124 . H1241 . 0.961 no
C125 . C126 . 1.3867(18) yes
C125 . H1251 . 0.954 no
C126 . C127 . 1.4722(18) yes
C127 . C128 . 1.3993(18) yes
C127 . C132 . 1.3911(19) yes
C128 . C129 . 1.3804(18) yes
C129 . C130 . 1.395(2) yes
C129 . H1291 . 0.960 no
C130 . C131 . 1.389(2) yes
C130 . H1301 . 0.942 no
C131 . C132 . 1.384(2) yes
C131 . H1311 . 0.959 no
C132 . H1321 . 0.956 no
C133 . C134 . 1.3815(18) yes
C133 . C138 . 1.3938(18) yes
C134 . C135 . 1.392(2) yes
C134 . H1341 . 0.945 no
C135 . C136 . 1.378(2) yes
C135 . H1351 . 0.959 no
C136 . C137 . 1.3806(19) yes
C136 . H1361 . 0.958 no
C137 . C138 . 1.3819(19) yes
C137 . H1371 . 0.937 no
C138 . H1381 . 0.942 no
C139 . C140 . 1.527(2) yes
C139 . C147 . 1.5361(18) yes
C139 . C152 . 1.5319(17) yes
C140 . C141 . 1.379(2) yes
C140 . C145 . 1.403(2) yes
C141 . C142 . 1.392(2) yes
C141 . H1411 . 0.943 no
C142 . C143 . 1.404(3) yes
C142 . H1421 . 0.930 no
C143 . C144 . 1.370(3) yes
C143 . H1431 . 0.917 no
C144 . C145 . 1.379(2) yes
C144 . H1441 . 0.983 no
C145 . C146 . 1.472(2) yes
C146 . C147 . 1.393(2) yes
C146 . C151 . 1.412(2) yes
C147 . C148 . 1.390(2) yes
C148 . C149 . 1.391(2) yes
C148 . H1481 . 1.012 no
C149 . C150 . 1.374(3) yes
C149 . H1491 . 1.015 no
C150 . C151 . 1.382(3) yes
C150 . H1501 . 0.978 no
C151 . H1511 . 0.925 no
C152 . C153 . 1.386(2) yes
C152 . C157 . 1.3940(19) yes
C153 . C154 . 1.3907(19) yes
C153 . H1531 . 0.949 no
C154 . C155 . 1.382(2) yes
C154 . H1541 . 0.964 no
C155 . C156 . 1.382(2) yes
C155 . H1551 . 0.956 no
C156 . C157 . 1.388(2) yes
C156 . H1561 . 0.957 no
C157 . H1571 . 0.956 no
C158 . C159 . 1.5308(18) yes
C158 . C166 . 1.5301(16) yes
C158 . C171 . 1.5363(17) yes
C159 . C160 . 1.3814(19) yes
C159 . C164 . 1.4005(18) yes
C160 . C161 . 1.392(2) yes
C160 . H1601 . 0.956 no
C161 . C162 . 1.387(2) yes
C161 . H1611 . 0.974 no
C162 . C163 . 1.380(2) yes
C162 . H1621 . 0.973 no
C163 . C164 . 1.392(2) yes
C163 . H1631 . 0.953 no
C164 . C165 . 1.468(2) yes
C165 . C166 . 1.3990(19) yes
C165 . C170 . 1.3895(19) yes
C166 . C167 . 1.381(2) yes
C167 . C168 . 1.397(2) yes
C167 . H1671 . 0.960 no
C168 . C169 . 1.386(2) yes
C168 . H1681 . 0.936 no
C169 . C170 . 1.380(2) yes
C169 . H1691 . 0.962 no
C170 . H1701 . 0.957 no
C171 . C172 . 1.3847(18) yes
C171 . C176 . 1.3942(18) yes
C172 . C173 . 1.3928(19) yes
C172 . H1721 . 0.962 no
C173 . C174 . 1.379(2) yes
C173 . H1731 . 0.967 no
C174 . C175 . 1.385(2) yes
C174 . H1741 . 0.955 no
C175 . C176 . 1.3821(19) yes
C175 . H1751 . 0.951 no
C176 . H1761 . 0.956 no
C177 . C178 . 1.5321(16) yes
C177 . C185 . 1.5314(16) yes
C177 . C190 . 1.5371(16) yes
C178 . C179 . 1.3843(17) yes
C178 . C183 . 1.3992(17) yes
C179 . C180 . 1.3933(18) yes
C179 . H1791 . 0.960 no
C180 . C181 . 1.388(2) yes
C180 . H1801 . 0.952 no
C181 . C182 . 1.3891(19) yes
C181 . H1811 . 0.945 no
C182 . C183 . 1.3918(18) yes
C182 . H1821 . 0.957 no
C183 . C184 . 1.4723(17) yes
C184 . C185 . 1.3980(17) yes
C184 . C189 . 1.3910(17) yes
C185 . C186 . 1.3823(18) yes
C186 . C187 . 1.3931(18) yes
C186 . H1861 . 0.958 no
C187 . C188 . 1.3883(19) yes
C187 . H1871 . 0.951 no
C188 . C189 . 1.3894(19) yes
C188 . H1881 . 0.960 no
C189 . H1891 . 0.953 no
C190 . C191 . 1.3829(17) yes
C190 . C195 . 1.3926(18) yes
C191 . C192 . 1.3939(19) yes
C191 . H1911 . 0.956 no
C192 . C193 . 1.376(2) yes
C192 . H1921 . 0.961 no
C193 . C194 . 1.378(2) yes
C193 . H1931 . 0.955 no
C194 . C195 . 1.3812(19) yes
C194 . H1941 . 0.954 no
C195 . H1951 . 0.957 no
C196 . C197 . 1.5307(17) yes
C196 . C204 . 1.5222(18) yes
C196 . C209 . 1.5340(19) yes
C197 . C198 . 1.3843(18) yes
C197 . C202 . 1.3965(19) yes
C198 . C199 . 1.391(2) yes
C198 . H1981 . 0.970 no
C199 . C200 . 1.384(2) yes
C199 . H1991 . 0.963 no
C200 . C201 . 1.387(2) yes
C200 . H2001 . 0.956 no
C201 . C202 . 1.390(2) yes
C201 . H2011 . 0.953 no
C202 . C203 . 1.4712(19) yes
C203 . C204 . 1.395(2) yes
C203 . C208 . 1.388(2) yes
C204 . C205 . 1.3822(19) yes
C205 . C206 . 1.391(2) yes
C205 . H2051 . 0.966 no
C206 . C207 . 1.380(3) yes
C206 . H2061 . 0.958 no
C207 . C208 . 1.387(2) yes
C207 . H2071 . 0.967 no
C208 . H2081 . 0.960 no
C209 . C210 . 1.385(2) yes
C209 . C214 . 1.387(2) yes
C210 . C211 . 1.390(2) yes
C210 . H2101 . 0.956 no
C211 . C212 . 1.369(3) yes
C211 . H2111 . 0.964 no
C212 . C213 . 1.366(3) yes
C212 . H2121 . 0.961 no
C213 . C214 . 1.390(3) yes
C213 . H2131 . 0.935 no
C214 . H2141 . 0.934 no
N501 . C502 . 1.5203(16) yes
N501 . C506 . 1.5172(17) yes
N501 . C510 . 1.5229(16) yes
N501 . C514 . 1.5199(18) yes
C502 . C503 . 1.5163(17) yes
C502 . H5021 . 0.975 no
C502 . H5022 . 0.983 no
C503 . C504 . 1.5246(19) yes
C503 . H5031 . 0.974 no
C503 . H5032 . 0.996 no
C504 . C505 . 1.518(2) yes
C504 . H5041 . 0.993 no
C504 . H5042 . 0.979 no
C505 . H5052 . 0.975 no
C505 . H5053 . 0.970 no
C505 . H5051 . 0.982 no
C506 . C507 . 1.512(2) yes
C506 . H5061 . 0.966 no
C506 . H5062 . 0.971 no
C507 . C508 . 1.523(2) yes
C507 . H5071 . 0.979 no
C507 . H5072 . 0.987 no
C508 . C509 . 1.512(2) yes
C508 . H5081 . 0.971 no
C508 . H5082 . 0.965 no
C509 . H5093 . 0.986 no
C509 . H5092 . 0.982 no
C509 . H5091 . 0.991 no
C510 . C511 . 1.5179(18) yes
C510 . H5101 . 0.983 no
C510 . H5102 . 0.968 no
C511 . C512 . 1.5287(18) yes
C511 . H5111 . 0.986 no
C511 . H5112 . 0.982 no
C512 . C513 . 1.5175(19) yes
C512 . H5121 . 0.979 no
C512 . H5122 . 0.974 no
C513 . H5133 . 0.976 no
C513 . H5131 . 0.981 no
C513 . H5132 . 0.980 no
C514 . C515 . 1.509(2) yes
C514 . H5141 . 0.972 no
C514 . H5142 . 0.980 no
C515 . C516 . 1.502(2) yes
C515 . H5151 . 0.968 no
C515 . H5152 . 0.980 no
C516 . C517 . 1.510(3) yes
C516 . H5161 . 1.009 no
C516 . H5162 . 0.953 no
C517 . H5172 . 0.983 no
C517 . H5171 . 0.993 no
C517 . H5173 . 0.972 no
N521 . C522 . 1.5238(16) yes
N521 . C526 . 1.5163(17) yes
N521 . C530 . 1.5256(17) yes
N521 . C534 . 1.5236(16) yes
C522 . C523 . 1.530(2) yes
C522 . H5221 . 0.983 no
C522 . H5222 . 0.951 no
C523 . C524 . 1.528(2) yes
C523 . H5231 . 1.040 no
C523 . H5232 . 1.004 no
C524 . C525 . 1.519(2) yes
C524 . H5241 . 0.970 no
C524 . H5242 . 1.003 no
C525 . H5251 . 1.039 no
C525 . H5252 . 1.016 no
C525 . H5253 . 1.043 no
C526 . C527 . 1.519(2) yes
C526 . H5261 . 0.958 no
C526 . H5262 . 0.955 no
C527 . C528 . 1.501(2) yes
C527 . H5271 . 0.995 no
C527 . H5272 . 0.996 no
C528 . C529 . 1.513(2) yes
C528 . H5281 . 1.007 no
C528 . H5282 . 1.027 no
C529 . H5291 . 1.003 no
C529 . H5292 . 0.978 no
C529 . H5293 . 0.960 no
C530 . C531 . 1.5166(19) yes
C530 . H5301 . 0.966 no
C530 . H5302 . 0.988 no
C531 . C532 . 1.5219(19) yes
C531 . H5311 . 0.964 no
C531 . H5312 . 0.978 no
C532 . C533 . 1.512(2) yes
C532 . H5321 . 0.963 no
C532 . H5322 . 0.975 no
C533 . H5331 . 0.971 no
C533 . H5332 . 0.974 no
C533 . H5333 . 0.972 no
C534 . C535 . 1.513(2) yes
C534 . H5342 . 0.980 no
C534 . H5341 . 0.977 no
C535 . C536 . 1.522(2) yes
C535 . H5352 . 0.965 no
C535 . H5351 . 0.970 no
C536 . C537 . 1.524(2) yes
C536 . H5361 . 0.953 no
C536 . H5362 . 0.985 no
C537 . H5371 . 0.983 no
C537 . H5372 . 0.969 no
C537 . H5373 . 1.005 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C101 . O11 . H111 . 112.6 no
C120 . O12 . H121 . 110.4 no
C139 . O13 . H131 . 111.7 no
C158 . O14 . H141 . 111.9 no
C177 . O15 . H151 . 112.0 no
C196 . O16 . H161 . 111.9 no
O11 . C101 . C102 . 112.45(10) yes
O11 . C101 . C109 . 106.99(10) yes
C102 . C101 . C109 . 101.02(10) yes
O11 . C101 . C114 . 113.59(10) yes
C102 . C101 . C114 . 111.27(10) yes
C109 . C101 . C114 . 110.72(10) yes
C101 . C102 . C103 . 128.08(12) yes
C101 . C102 . C107 . 110.93(11) yes
C103 . C102 . C107 . 120.99(12) yes
C102 . C103 . C104 . 118.42(14) yes
C102 . C103 . H1031 . 120.8 no
C104 . C103 . H1031 . 120.8 no
C103 . C104 . C105 . 120.99(14) yes
C103 . C104 . H1041 . 120.0 no
C105 . C104 . H1041 . 119.0 no
C104 . C105 . C106 . 120.79(14) yes
C104 . C105 . H1051 . 119.7 no
C106 . C105 . H1051 . 119.5 no
C105 . C106 . C107 . 118.59(14) yes
C105 . C106 . H1061 . 121.2 no
C107 . C106 . H1061 . 120.2 no
C102 . C107 . C106 . 120.22(13) yes
C102 . C107 . C108 . 108.48(11) yes
C106 . C107 . C108 . 131.31(13) yes
C107 . C108 . C109 . 108.49(11) yes
C107 . C108 . C113 . 131.50(12) yes
C109 . C108 . C113 . 120.01(13) yes
C101 . C109 . C108 . 111.08(11) yes
C101 . C109 . C110 . 127.83(11) yes
C108 . C109 . C110 . 121.09(12) yes
C109 . C110 . C111 . 118.85(12) yes
C109 . C110 . H1101 . 120.5 no
C111 . C110 . H1101 . 120.7 no
C110 . C111 . C112 . 120.31(13) yes
C110 . C111 . H1111 . 120.1 no
C112 . C111 . H1111 . 119.6 no
C111 . C112 . C113 . 120.95(13) yes
C111 . C112 . H1121 . 119.0 no
C113 . C112 . H1121 . 120.1 no
C112 . C113 . C108 . 118.80(13) yes
C112 . C113 . H1131 . 120.5 no
C108 . C113 . H1131 . 120.7 no
C101 . C114 . C115 . 122.27(11) yes
C101 . C114 . C119 . 119.39(11) yes
C115 . C114 . C119 . 118.34(12) yes
C114 . C115 . C116 . 119.98(13) yes
C114 . C115 . H1151 . 119.8 no
C116 . C115 . H1151 . 120.2 no
C115 . C116 . C117 . 120.89(14) yes
C115 . C116 . H1161 . 118.6 no
C117 . C116 . H1161 . 120.5 no
C116 . C117 . C118 . 119.49(14) yes
C116 . C117 . H1171 . 121.0 no
C118 . C117 . H1171 . 119.5 no
C117 . C118 . C119 . 119.88(14) yes
C117 . C118 . H1181 . 120.1 no
C119 . C118 . H1181 . 120.0 no
C114 . C119 . C118 . 121.40(13) yes
C114 . C119 . H1191 . 119.3 no
C118 . C119 . H1191 . 119.2 no
O12 . C120 . C121 . 112.73(10) yes
O12 . C120 . C128 . 108.49(10) yes
C121 . C120 . C128 . 100.91(10) yes
O12 . C120 . C133 . 112.70(10) yes
C121 . C120 . C133 . 110.55(10) yes
C128 . C120 . C133 . 110.83(10) yes
C120 . C121 . C122 . 127.82(11) yes
C120 . C121 . C126 . 111.14(10) yes
C122 . C121 . C126 . 121.03(11) yes
C121 . C122 . C123 . 118.32(12) yes
C121 . C122 . H1221 . 121.1 no
C123 . C122 . H1221 . 120.6 no
C122 . C123 . C124 . 121.00(13) yes
C122 . C123 . H1231 . 119.3 no
C124 . C123 . H1231 . 119.7 no
C123 . C124 . C125 . 120.73(13) yes
C123 . C124 . H1241 . 118.9 no
C125 . C124 . H1241 . 120.4 no
C124 . C125 . C126 . 118.59(13) yes
C124 . C125 . H1251 . 120.5 no
C126 . C125 . H1251 . 120.9 no
C121 . C126 . C125 . 120.31(12) yes
C121 . C126 . C127 . 108.45(11) yes
C125 . C126 . C127 . 131.24(12) yes
C126 . C127 . C128 . 108.46(11) yes
C126 . C127 . C132 . 130.91(12) yes
C128 . C127 . C132 . 120.62(13) yes
C120 . C128 . C127 . 111.00(11) yes
C120 . C128 . C129 . 128.34(12) yes
C127 . C128 . C129 . 120.64(12) yes
C128 . C129 . C130 . 118.66(13) yes
C128 . C129 . H1291 . 120.7 no
C130 . C129 . H1291 . 120.7 no
C129 . C130 . C131 . 120.58(13) yes
C129 . C130 . H1301 . 119.7 no
C131 . C130 . H1301 . 119.8 no
C130 . C131 . C132 . 121.00(13) yes
C130 . C131 . H1311 . 119.1 no
C132 . C131 . H1311 . 119.9 no
C127 . C132 . C131 . 118.45(13) yes
C127 . C132 . H1321 . 120.8 no
C131 . C132 . H1321 . 120.8 no
C120 . C133 . C134 . 121.70(11) yes
C120 . C133 . C138 . 119.65(11) yes
C134 . C133 . C138 . 118.65(12) yes
C133 . C134 . C135 . 119.83(12) yes
C133 . C134 . H1341 . 119.2 no
C135 . C134 . H1341 . 120.9 no
C134 . C135 . C136 . 121.15(13) yes
C134 . C135 . H1351 . 119.6 no
C136 . C135 . H1351 . 119.3 no
C135 . C136 . C137 . 119.27(13) yes
C135 . C136 . H1361 . 121.4 no
C137 . C136 . H1361 . 119.3 no
C136 . C137 . C138 . 119.87(12) yes
C136 . C137 . H1371 . 119.7 no
C138 . C137 . H1371 . 120.4 no
C133 . C138 . C137 . 121.23(12) yes
C133 . C138 . H1381 . 118.4 no
C137 . C138 . H1381 . 120.4 no
O13 . C139 . C140 . 111.66(10) yes
O13 . C139 . C147 . 107.26(10) yes
C140 . C139 . C147 . 101.23(11) yes
O13 . C139 . C152 . 112.10(11) yes
C140 . C139 . C152 . 113.69(11) yes
C147 . C139 . C152 . 110.18(10) yes
C139 . C140 . C141 . 128.35(12) yes
C139 . C140 . C145 . 110.46(13) yes
C141 . C140 . C145 . 121.15(14) yes
C140 . C141 . C142 . 118.19(15) yes
C140 . C141 . H1411 . 121.7 no
C142 . C141 . H1411 . 120.1 no
C141 . C142 . C143 . 120.07(18) yes
C141 . C142 . H1421 . 117.8 no
C143 . C142 . H1421 . 122.1 no
C142 . C143 . C144 . 121.47(16) yes
C142 . C143 . H1431 . 116.6 no
C144 . C143 . H1431 . 121.9 no
C143 . C144 . C145 . 118.58(16) yes
C143 . C144 . H1441 . 119.6 no
C145 . C144 . H1441 . 121.8 no
C140 . C145 . C144 . 120.53(17) yes
C140 . C145 . C146 . 108.83(13) yes
C144 . C145 . C146 . 130.65(15) yes
C145 . C146 . C147 . 108.56(12) yes
C145 . C146 . C151 . 132.10(16) yes
C147 . C146 . C151 . 119.33(17) yes
C139 . C147 . C146 . 110.81(13) yes
C139 . C147 . C148 . 128.14(14) yes
C146 . C147 . C148 . 121.05(14) yes
C147 . C148 . C149 . 118.81(17) yes
C147 . C148 . H1481 . 119.6 no
C149 . C148 . H1481 . 121.6 no
C148 . C149 . C150 . 120.57(18) yes
C148 . C149 . H1491 . 120.5 no
C150 . C149 . H1491 . 118.9 no
C149 . C150 . C151 . 121.44(15) yes
C149 . C150 . H1501 . 118.9 no
C151 . C150 . H1501 . 119.6 no
C146 . C151 . C150 . 118.77(17) yes
C146 . C151 . H1511 . 113.1 no
C150 . C151 . H1511 . 128.0 no
C139 . C152 . C153 . 120.07(12) yes
C139 . C152 . C157 . 121.10(12) yes
C153 . C152 . C157 . 118.78(12) yes
C152 . C153 . C154 . 120.58(13) yes
C152 . C153 . H1531 . 119.3 no
C154 . C153 . H1531 . 120.1 no
C153 . C154 . C155 . 120.20(14) yes
C153 . C154 . H1541 . 118.3 no
C155 . C154 . H1541 . 121.5 no
C154 . C155 . C156 . 119.74(13) yes
C154 . C155 . H1551 . 120.6 no
C156 . C155 . H1551 . 119.7 no
C155 . C156 . C157 . 120.16(14) yes
C155 . C156 . H1561 . 120.4 no
C157 . C156 . H1561 . 119.5 no
C152 . C157 . C156 . 120.54(14) yes
C152 . C157 . H1571 . 119.5 no
C156 . C157 . H1571 . 119.9 no
O14 . C158 . C159 . 113.50(10) yes
O14 . C158 . C166 . 108.08(10) yes
C159 . C158 . C166 . 100.83(10) yes
O14 . C158 . C171 . 112.34(10) yes
C159 . C158 . C171 . 111.43(10) yes
C166 . C158 . C171 . 109.96(10) yes
C158 . C159 . C160 . 128.40(12) yes
C158 . C159 . C164 . 110.91(11) yes
C160 . C159 . C164 . 120.69(13) yes
C159 . C160 . C161 . 118.50(13) yes
C159 . C160 . H1601 . 121.5 no
C161 . C160 . H1601 . 120.0 no
C160 . C161 . C162 . 120.88(14) yes
C160 . C161 . H1611 . 119.7 no
C162 . C161 . H1611 . 119.5 no
C161 . C162 . C163 . 120.82(14) yes
C161 . C162 . H1621 . 119.5 no
C163 . C162 . H1621 . 119.7 no
C162 . C163 . C164 . 118.76(14) yes
C162 . C163 . H1631 . 121.6 no
C164 . C163 . H1631 . 119.6 no
C159 . C164 . C163 . 120.35(13) yes
C159 . C164 . C165 . 108.59(12) yes
C163 . C164 . C165 . 131.02(13) yes
C164 . C165 . C166 . 108.52(11) yes
C164 . C165 . C170 . 131.17(14) yes
C166 . C165 . C170 . 120.29(14) yes
C158 . C166 . C165 . 111.04(11) yes
C158 . C166 . C167 . 128.06(12) yes
C165 . C166 . C167 . 120.90(12) yes
C166 . C167 . C168 . 118.34(14) yes
C166 . C167 . H1671 . 120.7 no
C168 . C167 . H1671 . 121.0 no
C167 . C168 . C169 . 120.64(15) yes
C167 . C168 . H1681 . 118.0 no
C169 . C168 . H1681 . 121.4 no
C168 . C169 . C170 . 121.04(13) yes
C168 . C169 . H1691 . 119.6 no
C170 . C169 . H1691 . 119.3 no
C165 . C170 . C169 . 118.77(15) yes
C165 . C170 . H1701 . 120.1 no
C169 . C170 . H1701 . 121.1 no
C158 . C171 . C172 . 121.32(11) yes
C158 . C171 . C176 . 119.99(11) yes
C172 . C171 . C176 . 118.66(12) yes
C171 . C172 . C173 . 120.22(13) yes
C171 . C172 . H1721 . 119.1 no
C173 . C172 . H1721 . 120.7 no
C172 . C173 . C174 . 120.72(13) yes
C172 . C173 . H1731 . 118.4 no
C174 . C173 . H1731 . 120.9 no
C173 . C174 . C175 . 119.32(13) yes
C173 . C174 . H1741 . 120.4 no
C175 . C174 . H1741 . 120.3 no
C174 . C175 . C176 . 120.18(14) yes
C174 . C175 . H1751 . 120.9 no
C176 . C175 . H1751 . 118.9 no
C171 . C176 . C175 . 120.89(13) yes
C171 . C176 . H1761 . 119.8 no
C175 . C176 . H1761 . 119.3 no
O15 . C177 . C178 . 113.31(9) yes
O15 . C177 . C185 . 109.98(9) yes
C178 . C177 . C185 . 100.94(9) yes
O15 . C177 . C190 . 112.61(9) yes
C178 . C177 . C190 . 110.04(9) yes
C185 . C177 . C190 . 109.30(9) yes
C177 . C178 . C179 . 128.34(11) yes
C177 . C178 . C183 . 110.93(10) yes
C179 . C178 . C183 . 120.71(11) yes
C178 . C179 . C180 . 118.41(12) yes
C178 . C179 . H1791 . 120.7 no
C180 . C179 . H1791 . 120.9 no
C179 . C180 . C181 . 121.03(12) yes
C179 . C180 . H1801 . 118.6 no
C181 . C180 . H1801 . 120.3 no
C180 . C181 . C182 . 120.69(12) yes
C180 . C181 . H1811 . 119.6 no
C182 . C181 . H1811 . 119.7 no
C181 . C182 . C183 . 118.51(12) yes
C181 . C182 . H1821 . 120.8 no
C183 . C182 . H1821 . 120.7 no
C178 . C183 . C182 . 120.60(12) yes
C178 . C183 . C184 . 108.52(11) yes
C182 . C183 . C184 . 130.88(11) yes
C183 . C184 . C185 . 108.58(10) yes
C183 . C184 . C189 . 130.92(12) yes
C185 . C184 . C189 . 120.49(12) yes
C177 . C185 . C184 . 110.94(10) yes
C177 . C185 . C186 . 128.24(11) yes
C184 . C185 . C186 . 120.76(11) yes
C185 . C186 . C187 . 118.75(12) yes
C185 . C186 . H1861 . 121.4 no
C187 . C186 . H1861 . 119.8 no
C186 . C187 . C188 . 120.54(12) yes
C186 . C187 . H1871 . 119.8 no
C188 . C187 . H1871 . 119.6 no
C187 . C188 . C189 . 120.95(12) yes
C187 . C188 . H1881 . 119.2 no
C189 . C188 . H1881 . 119.8 no
C184 . C189 . C188 . 118.50(12) yes
C184 . C189 . H1891 . 120.3 no
C188 . C189 . H1891 . 121.2 no
C177 . C190 . C191 . 122.12(11) yes
C177 . C190 . C195 . 119.40(11) yes
C191 . C190 . C195 . 118.49(12) yes
C190 . C191 . C192 . 120.16(13) yes
C190 . C191 . H1911 . 119.8 no
C192 . C191 . H1911 . 120.0 no
C191 . C192 . C193 . 120.67(13) yes
C191 . C192 . H1921 . 119.1 no
C193 . C192 . H1921 . 120.3 no
C192 . C193 . C194 . 119.52(13) yes
C192 . C193 . H1931 . 120.3 no
C194 . C193 . H1931 . 120.1 no
C193 . C194 . C195 . 120.04(13) yes
C193 . C194 . H1941 . 119.4 no
C195 . C194 . H1941 . 120.6 no
C190 . C195 . C194 . 121.11(13) yes
C190 . C195 . H1951 . 119.3 no
C194 . C195 . H1951 . 119.6 no
O16 . C196 . C197 . 113.27(10) yes
O16 . C196 . C204 . 107.68(10) yes
C197 . C196 . C204 . 101.17(10) yes
O16 . C196 . C209 . 111.81(10) yes
C197 . C196 . C209 . 110.27(10) yes
C204 . C196 . C209 . 112.19(11) yes
C196 . C197 . C198 . 128.68(12) yes
C196 . C197 . C202 . 110.73(11) yes
C198 . C197 . C202 . 120.59(12) yes
C197 . C198 . C199 . 118.57(13) yes
C197 . C198 . H1981 . 121.2 no
C199 . C198 . H1981 . 120.3 no
C198 . C199 . C200 . 120.85(13) yes
C198 . C199 . H1991 . 119.7 no
C200 . C199 . H1991 . 119.5 no
C199 . C200 . C201 . 120.91(14) yes
C199 . C200 . H2001 . 119.0 no
C201 . C200 . H2001 . 120.1 no
C200 . C201 . C202 . 118.45(14) yes
C200 . C201 . H2011 . 121.6 no
C202 . C201 . H2011 . 119.9 no
C197 . C202 . C201 . 120.63(13) yes
C197 . C202 . C203 . 108.43(12) yes
C201 . C202 . C203 . 130.92(13) yes
C202 . C203 . C204 . 108.64(12) yes
C202 . C203 . C208 . 130.94(14) yes
C204 . C203 . C208 . 120.42(14) yes
C196 . C204 . C203 . 110.92(11) yes
C196 . C204 . C205 . 128.16(13) yes
C203 . C204 . C205 . 120.92(13) yes
C204 . C205 . C206 . 118.46(15) yes
C204 . C205 . H2051 . 120.8 no
C206 . C205 . H2051 . 120.7 no
C205 . C206 . C207 . 120.56(15) yes
C205 . C206 . H2061 . 118.9 no
C207 . C206 . H2061 . 120.6 no
C206 . C207 . C208 . 121.30(15) yes
C206 . C207 . H2071 . 119.8 no
C208 . C207 . H2071 . 118.9 no
C203 . C208 . C207 . 118.31(16) yes
C203 . C208 . H2081 . 120.9 no
C207 . C208 . H2081 . 120.8 no
C196 . C209 . C210 . 120.74(12) yes
C196 . C209 . C214 . 121.53(13) yes
C210 . C209 . C214 . 117.66(14) yes
C209 . C210 . C211 . 120.94(15) yes
C209 . C210 . H2101 . 119.6 no
C211 . C210 . H2101 . 119.5 no
C210 . C211 . C212 . 120.75(17) yes
C210 . C211 . H2111 . 120.2 no
C212 . C211 . H2111 . 119.0 no
C211 . C212 . C213 . 118.94(16) yes
C211 . C212 . H2121 . 120.9 no
C213 . C212 . H2121 . 120.1 no
C212 . C213 . C214 . 120.97(17) yes
C212 . C213 . H2131 . 120.2 no
C214 . C213 . H2131 . 118.8 no
C213 . C214 . C209 . 120.75(17) yes
C213 . C214 . H2141 . 121.7 no
C209 . C214 . H2141 . 117.6 no
C502 . N501 . C506 . 111.28(10) yes
C502 . N501 . C510 . 105.51(9) yes
C506 . N501 . C510 . 111.27(10) yes
C502 . N501 . C514 . 111.05(10) yes
C506 . N501 . C514 . 106.1(1) yes
C510 . N501 . C514 . 111.71(10) yes
N501 . C502 . C503 . 116.32(10) yes
N501 . C502 . H5021 . 106.0 no
C503 . C502 . H5021 . 110.5 no
N501 . C502 . H5022 . 104.4 no
C503 . C502 . H5022 . 110.3 no
H5021 . C502 . H5022 . 109.0 no
C502 . C503 . C504 . 109.20(11) yes
C502 . C503 . H5031 . 111.6 no
C504 . C503 . H5031 . 109.3 no
C502 . C503 . H5032 . 110.1 no
C504 . C503 . H5032 . 109.5 no
H5031 . C503 . H5032 . 107.0 no
C503 . C504 . C505 . 112.23(12) yes
C503 . C504 . H5041 . 109.0 no
C505 . C504 . H5041 . 109.2 no
C503 . C504 . H5042 . 108.8 no
C505 . C504 . H5042 . 109.3 no
H5041 . C504 . H5042 . 108.2 no
C504 . C505 . H5052 . 110.8 no
C504 . C505 . H5053 . 109.7 no
H5052 . C505 . H5053 . 109.3 no
C504 . C505 . H5051 . 110.0 no
H5052 . C505 . H5051 . 108.2 no
H5053 . C505 . H5051 . 108.8 no
N501 . C506 . C507 . 116.16(10) yes
N501 . C506 . H5061 . 105.4 no
C507 . C506 . H5061 . 110.3 no
N501 . C506 . H5062 . 105.1 no
C507 . C506 . H5062 . 110.4 no
H5061 . C506 . H5062 . 109.0 no
C506 . C507 . C508 . 108.95(11) yes
C506 . C507 . H5071 . 110.7 no
C508 . C507 . H5071 . 109.4 no
C506 . C507 . H5072 . 110.7 no
C508 . C507 . H5072 . 109.1 no
H5071 . C507 . H5072 . 108.0 no
C507 . C508 . C509 . 113.32(13) yes
C507 . C508 . H5081 . 108.0 no
C509 . C508 . H5081 . 110.1 no
C507 . C508 . H5082 . 107.4 no
C509 . C508 . H5082 . 109.8 no
H5081 . C508 . H5082 . 108.0 no
C508 . C509 . H5093 . 109.9 no
C508 . C509 . H5092 . 110.5 no
H5093 . C509 . H5092 . 109.5 no
C508 . C509 . H5091 . 109.7 no
H5093 . C509 . H5091 . 108.2 no
H5092 . C509 . H5091 . 108.9 no
N501 . C510 . C511 . 116.89(10) yes
N501 . C510 . H5101 . 105.3 no
C511 . C510 . H5101 . 110.6 no
N501 . C510 . H5102 . 106.0 no
C511 . C510 . H5102 . 109.1 no
H5101 . C510 . H5102 . 108.6 no
C510 . C511 . C512 . 107.70(11) yes
C510 . C511 . H5111 . 111.3 no
C512 . C511 . H5111 . 110.1 no
C510 . C511 . H5112 . 110.5 no
C512 . C511 . H5112 . 109.4 no
H5111 . C511 . H5112 . 107.8 no
C511 . C512 . C513 . 113.51(12) yes
C511 . C512 . H5121 . 109.0 no
C513 . C512 . H5121 . 110.0 no
C511 . C512 . H5122 . 108.7 no
C513 . C512 . H5122 . 108.4 no
H5121 . C512 . H5122 . 107.0 no
C512 . C513 . H5133 . 110.5 no
C512 . C513 . H5131 . 111.2 no
H5133 . C513 . H5131 . 108.2 no
C512 . C513 . H5132 . 110.8 no
H5133 . C513 . H5132 . 108.0 no
H5131 . C513 . H5132 . 108.0 no
N501 . C514 . C515 . 115.76(11) yes
N501 . C514 . H5141 . 105.8 no
C515 . C514 . H5141 . 109.7 no
N501 . C514 . H5142 . 105.9 no
C515 . C514 . H5142 . 110.7 no
H5141 . C514 . H5142 . 108.6 no
C514 . C515 . C516 . 110.93(13) yes
C514 . C515 . H5151 . 110.9 no
C516 . C515 . H5151 . 109.6 no
C514 . C515 . H5152 . 110.7 no
C516 . C515 . H5152 . 108.8 no
H5151 . C515 . H5152 . 105.8 no
C515 . C516 . C517 . 113.27(17) yes
C515 . C516 . H5161 . 108.0 no
C517 . C516 . H5161 . 108.1 no
C515 . C516 . H5162 . 112.2 no
C517 . C516 . H5162 . 108.0 no
H5161 . C516 . H5162 . 107.0 no
C516 . C517 . H5172 . 110.7 no
C516 . C517 . H5171 . 113.5 no
H5172 . C517 . H5171 . 109.4 no
C516 . C517 . H5173 . 109.4 no
H5172 . C517 . H5173 . 107.0 no
H5171 . C517 . H5173 . 106.6 no
C522 . N521 . C526 . 109.46(10) yes
C522 . N521 . C530 . 107.74(10) yes
C526 . N521 . C530 . 110.54(10) yes
C522 . N521 . C534 . 110.83(10) yes
C526 . N521 . C534 . 107.55(10) yes
C530 . N521 . C534 . 110.72(10) yes
N521 . C522 . C523 . 114.17(11) yes
N521 . C522 . H5221 . 105.1 no
C523 . C522 . H5221 . 112.1 no
N521 . C522 . H5222 . 101.5 no
C523 . C522 . H5222 . 114.4 no
H5221 . C522 . H5222 . 108.6 no
C522 . C523 . C524 . 112.64(13) yes
C522 . C523 . H5231 . 109.7 no
C524 . C523 . H5231 . 108.6 no
C522 . C523 . H5232 . 105.6 no
C524 . C523 . H5232 . 108.5 no
H5231 . C523 . H5232 . 111.9 no
C523 . C524 . C525 . 111.76(14) yes
C523 . C524 . H5241 . 108.6 no
C525 . C524 . H5241 . 110.8 no
C523 . C524 . H5242 . 109.0 no
C525 . C524 . H5242 . 110.2 no
H5241 . C524 . H5242 . 106.3 no
C524 . C525 . H5251 . 110.0 no
C524 . C525 . H5252 . 101.4 no
H5251 . C525 . H5252 . 106.3 no
C524 . C525 . H5253 . 112.3 no
H5251 . C525 . H5253 . 111.9 no
H5252 . C525 . H5253 . 114.3 no
N521 . C526 . C527 . 114.34(11) yes
N521 . C526 . H5261 . 107.5 no
C527 . C526 . H5261 . 111.1 no
N521 . C526 . H5262 . 106.0 no
C527 . C526 . H5262 . 110.5 no
H5261 . C526 . H5262 . 107.0 no
C526 . C527 . C528 . 111.89(12) yes
C526 . C527 . H5271 . 110.2 no
C528 . C527 . H5271 . 107.8 no
C526 . C527 . H5272 . 111.8 no
C528 . C527 . H5272 . 104.6 no
H5271 . C527 . H5272 . 110.4 no
C527 . C528 . C529 . 111.82(14) yes
C527 . C528 . H5281 . 106.7 no
C529 . C528 . H5281 . 111.8 no
C527 . C528 . H5282 . 107.2 no
C529 . C528 . H5282 . 110.7 no
H5281 . C528 . H5282 . 108.4 no
C528 . C529 . H5291 . 111.0 no
C528 . C529 . H5292 . 110.3 no
H5291 . C529 . H5292 . 108.8 no
C528 . C529 . H5293 . 110.2 no
H5291 . C529 . H5293 . 111.1 no
H5292 . C529 . H5293 . 105.3 no
N521 . C530 . C531 . 115.78(10) yes
N521 . C530 . H5301 . 105.7 no
C531 . C530 . H5301 . 109.5 no
N521 . C530 . H5302 . 106.0 no
C531 . C530 . H5302 . 111.0 no
H5301 . C530 . H5302 . 108.4 no
C530 . C531 . C532 . 110.46(12) yes
C530 . C531 . H5311 . 110.7 no
C532 . C531 . H5311 . 108.7 no
C530 . C531 . H5312 . 110.3 no
C532 . C531 . H5312 . 108.8 no
H5311 . C531 . H5312 . 107.9 no
C531 . C532 . C533 . 112.68(14) yes
C531 . C532 . H5321 . 108.1 no
C533 . C532 . H5321 . 109.8 no
C531 . C532 . H5322 . 107.9 no
C533 . C532 . H5322 . 108.1 no
H5321 . C532 . H5322 . 110.2 no
C532 . C533 . H5331 . 111.1 no
C532 . C533 . H5332 . 111.8 no
H5331 . C533 . H5332 . 108.4 no
C532 . C533 . H5333 . 110.8 no
H5331 . C533 . H5333 . 107.8 no
H5332 . C533 . H5333 . 106.8 no
N521 . C534 . C535 . 114.80(11) yes
N521 . C534 . H5342 . 107.9 no
C535 . C534 . H5342 . 109.5 no
N521 . C534 . H5341 . 106.1 no
C535 . C534 . H5341 . 109.8 no
H5342 . C534 . H5341 . 108.6 no
C534 . C535 . C536 . 111.84(12) yes
C534 . C535 . H5352 . 110.1 no
C536 . C535 . H5352 . 108.2 no
C534 . C535 . H5351 . 111.6 no
C536 . C535 . H5351 . 106.0 no
H5352 . C535 . H5351 . 108.9 no
C535 . C536 . C537 . 112.37(14) yes
C535 . C536 . H5361 . 108.6 no
C537 . C536 . H5361 . 111.4 no
C535 . C536 . H5362 . 108.8 no
C537 . C536 . H5362 . 108.7 no
H5361 . C536 . H5362 . 106.9 no
C536 . C537 . H5371 . 110.4 no
C536 . C537 . H5372 . 110.3 no
H5371 . C537 . H5372 . 108.8 no
C536 . C537 . H5373 . 110.5 no
H5371 . C537 . H5373 . 108.1 no
H5372 . C537 . H5373 . 108.7 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C134 . H1341 . O11 . 156.68 0.945 2.419 3.308(2) yes
C502 . H5021 . O14 . 136.35 0.975 2.433 3.210(2) yes
C514 . H5142 . O12 . 164.19 0.980 2.541 3.494(2) yes
C530 . H5302 . O13 1_545 142.08 0.988 2.376 3.213(2) yes
C534 . H5342 . O16 1_655 165.11 0.980 2.424 3.380(2) yes
O16 . H161 . O15 . 164.73 0.846 1.941 2.766(2) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 30/11/12 at 11:50:50
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE O   (  11,X'S) H   ( 111,X'S) 
RIDE O   (  12,X'S) H   ( 121,X'S) 
RIDE O   (  13,X'S) H   ( 131,X'S) 
RIDE O   (  14,X'S) H   ( 141,X'S) 
RIDE O   (  15,X'S) H   ( 151,X'S) 
RIDE O   (  16,X'S) H   ( 161,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) 
RIDE C   ( 117,X'S) H   (1171,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 119,X'S) H   (1191,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) 
RIDE C   ( 125,X'S) H   (1251,X'S) 
RIDE C   ( 129,X'S) H   (1291,X'S) 
RIDE C   ( 130,X'S) H   (1301,X'S) 
RIDE C   ( 131,X'S) H   (1311,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) 
RIDE C   ( 134,X'S) H   (1341,X'S) 
RIDE C   ( 135,X'S) H   (1351,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) 
RIDE C   ( 137,X'S) H   (1371,X'S) 
RIDE C   ( 138,X'S) H   (1381,X'S) 
RIDE C   ( 141,X'S) H   (1411,X'S) 
RIDE C   ( 142,X'S) H   (1421,X'S) 
RIDE C   ( 143,X'S) H   (1431,X'S) 
RIDE C   ( 144,X'S) H   (1441,X'S) 
RIDE C   ( 148,X'S) H   (1481,X'S) 
RIDE C   ( 149,X'S) H   (1491,X'S) 
RIDE C   ( 150,X'S) H   (1501,X'S) 
RIDE C   ( 151,X'S) H   (1511,X'S) 
RIDE C   ( 153,X'S) H   (1531,X'S) 
RIDE C   ( 154,X'S) H   (1541,X'S) 
RIDE C   ( 155,X'S) H   (1551,X'S) 
RIDE C   ( 156,X'S) H   (1561,X'S) 
RIDE C   ( 157,X'S) H   (1571,X'S) 
RIDE C   ( 160,X'S) H   (1601,X'S) 
RIDE C   ( 161,X'S) H   (1611,X'S) 
RIDE C   ( 162,X'S) H   (1621,X'S) 
RIDE C   ( 163,X'S) H   (1631,X'S) 
RIDE C   ( 167,X'S) H   (1671,X'S) 
RIDE C   ( 168,X'S) H   (1681,X'S) 
RIDE C   ( 169,X'S) H   (1691,X'S) 
RIDE C   ( 170,X'S) H   (1701,X'S) 
RIDE C   ( 172,X'S) H   (1721,X'S) 
RIDE C   ( 173,X'S) H   (1731,X'S) 
RIDE C   ( 174,X'S) H   (1741,X'S) 
RIDE C   ( 175,X'S) H   (1751,X'S) 
RIDE C   ( 176,X'S) H   (1761,X'S) 
RIDE C   ( 179,X'S) H   (1791,X'S) 
RIDE C   ( 180,X'S) H   (1801,X'S) 
RIDE C   ( 181,X'S) H   (1811,X'S) 
RIDE C   ( 182,X'S) H   (1821,X'S) 
RIDE C   ( 186,X'S) H   (1861,X'S) 
RIDE C   ( 187,X'S) H   (1871,X'S) 
RIDE C   ( 188,X'S) H   (1881,X'S) 
RIDE C   ( 189,X'S) H   (1891,X'S) 
RIDE C   ( 191,X'S) H   (1911,X'S) 
RIDE C   ( 192,X'S) H   (1921,X'S) 
RIDE C   ( 193,X'S) H   (1931,X'S) 
RIDE C   ( 194,X'S) H   (1941,X'S) 
RIDE C   ( 195,X'S) H   (1951,X'S) 
RIDE C   ( 198,X'S) H   (1981,X'S) 
RIDE C   ( 199,X'S) H   (1991,X'S) 
RIDE C   ( 200,X'S) H   (2001,X'S) 
RIDE C   ( 201,X'S) H   (2011,X'S) 
RIDE C   ( 205,X'S) H   (2051,X'S) 
RIDE C   ( 206,X'S) H   (2061,X'S) 
RIDE C   ( 207,X'S) H   (2071,X'S) 
RIDE C   ( 208,X'S) H   (2081,X'S) 
RIDE C   ( 210,X'S) H   (2101,X'S) 
RIDE C   ( 211,X'S) H   (2111,X'S) 
RIDE C   ( 212,X'S) H   (2121,X'S) 
RIDE C   ( 213,X'S) H   (2131,X'S) 
RIDE C   ( 214,X'S) H   (2141,X'S) 
RIDE C   ( 502,X'S) H   (5021,X'S) H   (5022,X'S) 
RIDE C   ( 503,X'S) H   (5031,X'S) H   (5032,X'S) 
RIDE C   ( 504,X'S) H   (5041,X'S) H   (5042,X'S) 
RIDE C   ( 505,X'S) H   (5052,X'S) H   (5053,X'S) H   (5051,X'S) 
RIDE C   ( 506,X'S) H   (5061,X'S) H   (5062,X'S) 
RIDE C   ( 507,X'S) H   (5071,X'S) H   (5072,X'S) 
RIDE C   ( 508,X'S) H   (5081,X'S) H   (5082,X'S) 
RIDE C   ( 509,X'S) H   (5093,X'S) H   (5092,X'S) H   (5091,X'S) 
RIDE C   ( 510,X'S) H   (5101,X'S) H   (5102,X'S) 
RIDE C   ( 511,X'S) H   (5111,X'S) H   (5112,X'S) 
RIDE C   ( 512,X'S) H   (5121,X'S) H   (5122,X'S) 
RIDE C   ( 513,X'S) H   (5133,X'S) H   (5131,X'S) H   (5132,X'S) 
RIDE C   ( 514,X'S) H   (5141,X'S) H   (5142,X'S) 
RIDE C   ( 515,X'S) H   (5151,X'S) H   (5152,X'S) 
RIDE C   ( 516,X'S) H   (5161,X'S) H   (5162,X'S) 
RIDE C   ( 517,X'S) H   (5172,X'S) H   (5171,X'S) H   (5173,X'S) 
RIDE C   ( 522,X'S) H   (5221,X'S) H   (5222,X'S) 
RIDE C   ( 523,X'S) H   (5231,X'S) H   (5232,X'S) 
RIDE C   ( 524,X'S) H   (5241,X'S) H   (5242,X'S) 
RIDE C   ( 525,X'S) H   (5251,X'S) H   (5252,X'S) H   (5253,X'S) 
RIDE C   ( 526,X'S) H   (5261,X'S) H   (5262,X'S) 
RIDE C   ( 527,X'S) H   (5271,X'S) H   (5272,X'S) 
RIDE C   ( 528,X'S) H   (5281,X'S) H   (5282,X'S) 
RIDE C   ( 529,X'S) H   (5291,X'S) H   (5292,X'S) H   (5293,X'S) 
RIDE C   ( 530,X'S) H   (5301,X'S) H   (5302,X'S) 
RIDE C   ( 531,X'S) H   (5311,X'S) H   (5312,X'S) 
RIDE C   ( 532,X'S) H   (5321,X'S) H   (5322,X'S) 
RIDE C   ( 533,X'S) H   (5331,X'S) H   (5332,X'S) H   (5333,X'S) 
RIDE C   ( 534,X'S) H   (5342,X'S) H   (5341,X'S) 
RIDE C   ( 535,X'S) H   (5352,X'S) H   (5351,X'S) 
RIDE C   ( 536,X'S) H   (5361,X'S) H   (5362,X'S) 
RIDE C   ( 537,X'S) H   (5371,X'S) H   (5372,X'S) H   (5373,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 30/11/12 at 11:50:50
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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_2k
_database_code_depnum_ccdc_archive 'CCDC 1401775'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             13-04-30
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 065ggke01
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   9.4953(1)
_cell_length_b                   12.1501(2)
_cell_length_c                   21.4618(4)
_cell_angle_alpha                81.8444(6)
_cell_angle_beta                 89.1604(6)
_cell_angle_gamma                78.5486(7)
_cell_volume                     2401.96(7)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C45 H72 F1 N1 O3 
# Dc =      0.96 Fooo =    884.00 Mu =      0.61 M =    694.07
# Found Formula = C55 H72 F1 N1 O3 
# Dc =      1.13 FOOO =    884.00 Mu =      0.70 M =    814.18

_chemical_formula_sum            'C55 H72 F1 N1 O3'
_chemical_formula_moiety         '3(C13 H12 O), C16 H36 N, F'
_chemical_compound_source        .
_chemical_formula_weight         814.18


_cell_measurement_reflns_used    10032
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.14
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_max          0.65

_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             884.000
_exptl_absorpt_coefficient_mu    0.070

# Sheldrick geometric approximatio 0.99 0.99 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.99
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            40263
_reflns_number_total             10827
_diffrn_reflns_av_R_equivalents  0.022
# Number of reflections without Friedels Law is 19337 
# Number of reflections with Friedels Law is 10827 
# Theoretical number of reflections is about 11112 


_diffrn_reflns_theta_min         5.114
_diffrn_reflns_theta_max         27.568
_diffrn_measured_fraction_theta_max 0.974

_diffrn_reflns_theta_full        25.087
_diffrn_measured_fraction_theta_full 0.986


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              -15
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              27

_oxford_diffrn_Wilson_B_factor   3.44
_oxford_diffrn_Wilson_scale      0.55

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.35
_refine_diff_density_max         0.53


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         8998
_refine_ls_number_restraints     256
_refine_ls_number_parameters     597
_oxford_refine_ls_R_factor_ref   0.0611
_refine_ls_wR_factor_ref         0.1277
_refine_ls_goodness_of_fit_ref   0.9966
_refine_ls_shift/su_max          0.0005931
_refine_ls_shift/su_mean         0.0000687


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        8999
_refine_ls_R_factor_all          0.0611
_refine_ls_wR_factor_all         0.1278

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7316
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_gt          0.1166

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 0.96P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
O1 O 0.55996(14) 0.19758(12) 0.69367(6) 0.0598 1.0000 Uani . . . . . .
O2 O 0.26656(12) 0.55784(9) 0.70626(5) 0.0440 1.0000 Uani . . . . . .
O3 O 0.25801(12) 0.30950(11) 0.82809(5) 0.0500 1.0000 Uani . . . . . .
C11 C 0.51437(18) 0.21305(13) 0.63082(7) 0.0450 1.0000 Uani D . . . . .
C59 C 0.49700(19) 0.13028(15) 0.85187(9) 0.0488 1.0000 Uani . . . . . .
C13 C 0.6203(10) 0.3094(9) 0.5355(4) 0.0565 0.50(3) Uani D . P 1 1 .
C61 C 0.6831(2) 0.01465(18) 0.92049(12) 0.0678 1.0000 Uani . . . . . .
C15 C 0.8553(10) 0.2382(12) 0.5010(3) 0.0551 0.50(3) Uani D . P 1 1 .
C16 C 0.8727(8) 0.1522(11) 0.5506(4) 0.0530 0.50(3) Uani D . P 1 1 .
C17 C 0.7619(9) 0.1440(10) 0.5927(5) 0.0469 0.50(3) Uani D . P 1 1 .
C18 C 0.42759(17) 0.12389(13) 0.61968(7) 0.0391 1.0000 Uani . . . . . .
C19 C 0.3601(2) 0.07012(18) 0.66890(9) 0.0571 1.0000 Uani . . . . . .
C20 C 0.2756(2) -0.0059(2) 0.65850(10) 0.0660 1.0000 Uani . . . . . .
C21 C 0.25578(19) -0.02951(16) 0.59881(9) 0.0531 1.0000 Uani . . . . . .
C22 C 0.32217(19) 0.02300(15) 0.54951(8) 0.0485 1.0000 Uani . . . . . .
C23 C 0.40794(18) 0.09849(14) 0.55984(7) 0.0423 1.0000 Uani . . . . . .
C31 C 0.20272(16) 0.59655(13) 0.76102(7) 0.0371 1.0000 Uani . . . . . .
C32 C 0.06383(16) 0.68016(12) 0.74281(7) 0.0359 1.0000 Uani . . . . . .
C33 C 0.03781(18) 0.73647(14) 0.68196(8) 0.0448 1.0000 Uani . . . . . .
C34 C -0.0877(2) 0.81644(15) 0.66739(10) 0.0537 1.0000 Uani . . . . . .
C35 C -0.18808(19) 0.84033(15) 0.71303(10) 0.0551 1.0000 Uani . . . . . .
C36 C -0.16380(18) 0.78465(15) 0.77340(10) 0.0518 1.0000 Uani . . . . . .
C37 C -0.03885(17) 0.70527(14) 0.78811(8) 0.0420 1.0000 Uani . . . . . .
C38 C 0.29970(15) 0.65427(13) 0.79561(7) 0.0354 1.0000 Uani . . . . . .
C39 C 0.37417(18) 0.73045(16) 0.76215(8) 0.0463 1.0000 Uani . . . . . .
C40 C 0.45436(19) 0.78969(18) 0.79291(9) 0.0549 1.0000 Uani . . . . . .
C41 C 0.46330(19) 0.77379(17) 0.85775(9) 0.0537 1.0000 Uani . . . . . .
C42 C 0.3913(2) 0.69763(17) 0.89143(8) 0.0534 1.0000 Uani . . . . . .
C43 C 0.30978(18) 0.63857(14) 0.86068(8) 0.0441 1.0000 Uani . . . . . .
C51 C 0.31863(16) 0.29157(13) 0.88924(7) 0.0395 1.0000 Uani . . . . . .
C52 C 0.19986(16) 0.27592(13) 0.93566(7) 0.0366 1.0000 Uani . . . . . .
C53 C 0.12801(17) 0.18789(14) 0.93460(8) 0.0406 1.0000 Uani . . . . . .
C54 C 0.01791(18) 0.17422(16) 0.97642(9) 0.0529 1.0000 Uani . . . . . .
C55 C -0.0186(2) 0.24727(18) 1.02038(9) 0.0609 1.0000 Uani . . . . . .
C56 C 0.0525(2) 0.33431(19) 1.02167(9) 0.0641 1.0000 Uani . . . . . .
C57 C 0.1605(2) 0.34891(16) 0.97951(9) 0.0528 1.0000 Uani . . . . . .
C58 C 0.44577(15) 0.19159(13) 0.89947(7) 0.0360 1.0000 Uani . . . . . .
C81 C 0.75296(17) 0.39829(14) 0.83219(7) 0.0399 1.0000 Uani . . . . . .
C60 C 0.6157(2) 0.04210(17) 0.86237(11) 0.0652 1.0000 Uani . . . . . .
C83 C 0.6519(2) 0.43151(17) 0.93853(8) 0.0527 1.0000 Uani . . . . . .
C62 C 0.6322(2) 0.07420(18) 0.96799(11) 0.0619 1.0000 Uani . . . . . .
C63 C 0.51450(18) 0.16207(15) 0.95808(8) 0.0468 1.0000 Uani . . . . . .
F1 F 0.43490(11) 0.36839(8) 0.74413(5) 0.0513 1.0000 Uani . . . . . .
N71 N 0.87553(13) 0.37386(10) 0.72580(5) 0.0317 1.0000 Uani . . . . . .
C72 C 1.01109(15) 0.39787(13) 0.69277(7) 0.0335 1.0000 Uani . . . . . .
C73 C 1.03410(18) 0.36276(14) 0.62773(7) 0.0410 1.0000 Uani . . . . . .
C74 C 1.14053(18) 0.42431(16) 0.59186(8) 0.0475 1.0000 Uani . . . . . .
C75 C 1.1729(2) 0.38915(18) 0.52742(8) 0.0563 1.0000 Uani . . . . . .
C76 C 0.74142(16) 0.43273(13) 0.68705(7) 0.0343 1.0000 Uani . . . . . .
C77 C 0.72701(17) 0.55884(13) 0.66730(8) 0.0407 1.0000 Uani . . . . . .
C78 C 0.59162(16) 0.60566(14) 0.62740(7) 0.0401 1.0000 Uani . . . . . .
C79 C 0.57277(19) 0.73214(15) 0.60606(8) 0.0484 1.0000 Uani . . . . . .
C80 C 0.87532(16) 0.41747(12) 0.78863(6) 0.0324 1.0000 Uani . . . . . .
C117 C 0.7658(7) 0.1228(9) 0.6018(5) 0.0397 0.50(3) Uani D . P 1 2 .
C82 C 0.76057(18) 0.45768(15) 0.88926(7) 0.0435 1.0000 Uani . . . . . .
C115 C 0.8855(10) 0.1985(12) 0.5113(5) 0.0532 0.50(3) Uani D . P 1 2 .
C84 C 0.87347(17) 0.24787(12) 0.73452(7) 0.0380 1.0000 Uani . . . . . .
C85 C 0.98957(19) 0.17241(13) 0.77734(8) 0.0437 1.0000 Uani . . . . . .
C86 C 0.9823(2) 0.04878(14) 0.77733(9) 0.0503 1.0000 Uani . . . . . .
C87 C 1.0880(2) -0.03090(15) 0.82321(10) 0.0626 1.0000 Uani . . . . . .
C112 C 0.6470(9) 0.2081(9) 0.5890(5) 0.0405 0.50(3) Uani D . P 1 2 .
C116 C 0.8858(6) 0.1179(10) 0.5636(5) 0.0474 0.50(3) Uani D . P 1 2 .
C12 C 0.6335(9) 0.2214(9) 0.5853(5) 0.0414 0.50(3) Uani D . P 1 1 .
C14 C 0.7296(12) 0.3160(11) 0.4928(3) 0.0617 0.50(3) Uani D . P 1 1 .
C114 C 0.7694(13) 0.2840(9) 0.4975(4) 0.0548 0.50(3) Uani D . P 1 2 .
C113 C 0.6494(11) 0.2889(9) 0.5354(4) 0.0511 0.50(3) Uani D . P 1 2 .
H591 H 0.4533 0.1495 0.8111 0.0587 1.0000 Uiso R . . . . .
H131 H 0.5355 0.3652 0.5312 0.0681 0.50(3) Uiso R . P 1 1 .
H611 H 0.7628 -0.0441 0.9275 0.0813 1.0000 Uiso R . . . . .
H151 H 0.9299 0.2449 0.4714 0.0664 0.50(3) Uiso R . P 1 1 .
H161 H 0.9591 0.0988 0.5565 0.0639 0.50(3) Uiso R . P 1 1 .
H171 H 0.7728 0.0861 0.6263 0.0556 0.50(3) Uiso R . P 1 1 .
H191 H 0.3752 0.0839 0.7096 0.0696 1.0000 Uiso R . . . . .
H201 H 0.2311 -0.0417 0.6923 0.0799 1.0000 Uiso R . . . . .
H211 H 0.1964 -0.0803 0.5914 0.0633 1.0000 Uiso R . . . . .
H221 H 0.3112 0.0070 0.5084 0.0578 1.0000 Uiso R . . . . .
H231 H 0.4511 0.1346 0.5249 0.0508 1.0000 Uiso R . . . . .
H311 H 0.1819 0.5323 0.7894 0.0433 1.0000 Uiso R . . . . .
H331 H 0.1062 0.7209 0.6503 0.0540 1.0000 Uiso R . . . . .
H341 H -0.1054 0.8521 0.6252 0.0641 1.0000 Uiso R . . . . .
H351 H -0.2725 0.8931 0.7028 0.0663 1.0000 Uiso R . . . . .
H361 H -0.2336 0.8005 0.8049 0.0621 1.0000 Uiso R . . . . .
H371 H -0.0240 0.6680 0.8303 0.0495 1.0000 Uiso R . . . . .
H391 H 0.3689 0.7428 0.7179 0.0552 1.0000 Uiso R . . . . .
H401 H 0.5021 0.8439 0.7692 0.0668 1.0000 Uiso R . . . . .
H411 H 0.5171 0.8159 0.8790 0.0639 1.0000 Uiso R . . . . .
H421 H 0.3985 0.6848 0.9360 0.0641 1.0000 Uiso R . . . . .
H431 H 0.2596 0.5856 0.8836 0.0529 1.0000 Uiso R . . . . .
H511 H 0.3535 0.3630 0.8942 0.0472 1.0000 Uiso R . . . . .
H531 H 0.1545 0.1376 0.9050 0.0471 1.0000 Uiso R . . . . .
H541 H -0.0297 0.1158 0.9738 0.0628 1.0000 Uiso R . . . . .
H551 H -0.0896 0.2368 1.0492 0.0724 1.0000 Uiso R . . . . .
H561 H 0.0294 0.3852 1.0528 0.0775 1.0000 Uiso R . . . . .
H571 H 0.2080 0.4095 0.9811 0.0642 1.0000 Uiso R . . . . .
H811 H 0.7604 0.3177 0.8467 0.0494 1.0000 Uiso R . . . . .
H812 H 0.6629 0.4269 0.8110 0.0491 1.0000 Uiso R . . . . .
H601 H 0.6509 0.0026 0.8287 0.0784 1.0000 Uiso R . . . . .
H831 H 0.6572 0.4712 0.9746 0.0783 1.0000 Uiso R . . . . .
H832 H 0.6682 0.3495 0.9523 0.0787 1.0000 Uiso R . . . . .
H833 H 0.5555 0.4548 0.9204 0.0787 1.0000 Uiso R . . . . .
H621 H 0.6751 0.0548 1.0078 0.0751 1.0000 Uiso R . . . . .
H631 H 0.4793 0.2019 0.9912 0.0560 1.0000 Uiso R . . . . .
H721 H 1.0894 0.3592 0.7202 0.0382 1.0000 Uiso R . . . . .
H722 H 1.0055 0.4799 0.6900 0.0380 1.0000 Uiso R . . . . .
H731 H 1.0712 0.2816 0.6310 0.0514 1.0000 Uiso R . . . . .
H732 H 0.9456 0.3808 0.6045 0.0492 1.0000 Uiso R . . . . .
H741 H 1.2268 0.4134 0.6167 0.0583 1.0000 Uiso R . . . . .
H742 H 1.0991 0.5056 0.5877 0.0581 1.0000 Uiso R . . . . .
H753 H 1.2412 0.4305 0.5057 0.0847 1.0000 Uiso R . . . . .
H752 H 1.2140 0.3095 0.5306 0.0832 1.0000 Uiso R . . . . .
H751 H 1.0855 0.4032 0.5009 0.0825 1.0000 Uiso R . . . . .
H762 H 0.6615 0.4165 0.7125 0.0393 1.0000 Uiso R . . . . .
H761 H 0.7437 0.3947 0.6507 0.0395 1.0000 Uiso R . . . . .
H771 H 0.7200 0.5982 0.7042 0.0495 1.0000 Uiso R . . . . .
H772 H 0.8106 0.5732 0.6432 0.0502 1.0000 Uiso R . . . . .
H781 H 0.5082 0.5887 0.6518 0.0474 1.0000 Uiso R . . . . .
H782 H 0.5978 0.5659 0.5904 0.0473 1.0000 Uiso R . . . . .
H793 H 0.4848 0.7608 0.5813 0.0723 1.0000 Uiso R . . . . .
H792 H 0.5681 0.7737 0.6425 0.0709 1.0000 Uiso R . . . . .
H791 H 0.6536 0.7491 0.5794 0.0719 1.0000 Uiso R . . . . .
H801 H 0.9673 0.3818 0.8092 0.0374 1.0000 Uiso R . . . . .
H802 H 0.8720 0.4973 0.7787 0.0372 1.0000 Uiso R . . . . .
H1171 H 0.7647 0.0690 0.6361 0.0475 0.50(3) Uiso R . P 1 2 .
H821 H 0.8578 0.4343 0.9083 0.0523 1.0000 Uiso R . . . . .
H822 H 0.7421 0.5391 0.8757 0.0520 1.0000 Uiso R . . . . .
H1151 H 0.9670 0.1942 0.4846 0.0649 0.50(3) Uiso R . P 1 2 .
H841 H 0.7772 0.2411 0.7504 0.0454 1.0000 Uiso R . . . . .
H842 H 0.8829 0.2254 0.6923 0.0453 1.0000 Uiso R . . . . .
H851 H 0.9788 0.1896 0.8197 0.0517 1.0000 Uiso R . . . . .
H852 H 1.0822 0.1844 0.7633 0.0530 1.0000 Uiso R . . . . .
H862 H 0.8836 0.0394 0.7872 0.0607 1.0000 Uiso R . . . . .
H861 H 1.0029 0.0317 0.7350 0.0608 1.0000 Uiso R . . . . .
H873 H 1.0892 -0.1065 0.8173 0.0928 1.0000 Uiso R . . . . .
H872 H 1.0587 -0.0211 0.8663 0.0928 1.0000 Uiso R . . . . .
H871 H 1.1861 -0.0167 0.8170 0.0929 1.0000 Uiso R . . . . .
H1161 H 0.9649 0.0590 0.5737 0.0570 0.50(3) Uiso R . P 1 2 .
H141 H 0.7165 0.3736 0.4585 0.0740 0.50(3) Uiso R . P 1 1 .
H1141 H 0.7712 0.3398 0.4615 0.0663 0.50(3) Uiso R . P 1 2 .
H1131 H 0.5698 0.3469 0.5250 0.0615 0.50(3) Uiso R . P 1 2 .
H111 H 0.4497 0.2958 0.6300 0.0481 1.0000 Uiso R . . . . .
H31 H 0.3246 0.3260 0.7998 0.0760 1.0000 Uiso R . . . . .
H21 H 0.3267 0.4987 0.7202 0.0671 1.0000 Uiso R . . . . .
H11 H 0.5128 0.2606 0.7154 0.0919 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       450(90)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          1.317(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 . C11 . 1.3982(19) yes
O1 . H11 . 0.982 no
O2 . C31 . 1.4116(18) yes
O2 . H21 . 0.845 no
O3 . C51 . 1.4117(19) yes
O3 . H31 . 0.901 no
C11 . C18 . 1.531(2) yes
C11 . C12 . 1.493(5) yes
C11 . H111 . 1.067 no
C11 . C18 . 1.531(2) yes
C11 . C112 . 1.532(4) yes
C11 . H111 . 1.067 no
C59 . C58 . 1.376(2) yes
C59 . C60 . 1.389(3) yes
C59 . H591 . 0.953 no
C13 . C12 . 1.388(4) yes
C13 . C14 . 1.382(4) yes
C13 . H131 . 0.941 no
C61 . C60 . 1.378(3) yes
C61 . C62 . 1.361(3) yes
C61 . H611 . 0.929 no
C15 . C16 . 1.369(4) yes
C15 . C14 . 1.364(4) yes
C15 . H151 . 0.952 no
C16 . C17 . 1.385(5) yes
C16 . H161 . 0.937 no
C17 . C12 . 1.379(4) yes
C17 . H171 . 0.926 no
C18 . C19 . 1.380(2) yes
C18 . C23 . 1.386(2) yes
C19 . C20 . 1.380(3) yes
C19 . H191 . 0.930 no
C20 . C21 . 1.375(3) yes
C20 . H201 . 0.931 no
C21 . C22 . 1.368(3) yes
C21 . H211 . 0.945 no
C22 . C23 . 1.383(2) yes
C22 . H221 . 0.942 no
C23 . H231 . 0.944 no
C31 . C32 . 1.515(2) yes
C31 . C38 . 1.522(2) yes
C31 . H311 . 0.970 no
C32 . C33 . 1.387(2) yes
C32 . C37 . 1.388(2) yes
C33 . C34 . 1.388(2) yes
C33 . H331 . 0.945 no
C34 . C35 . 1.377(3) yes
C34 . H341 . 0.948 no
C35 . C36 . 1.374(3) yes
C35 . H351 . 0.929 no
C36 . C37 . 1.381(2) yes
C36 . H361 . 0.952 no
C37 . H371 . 0.952 no
C38 . C39 . 1.389(2) yes
C38 . C43 . 1.384(2) yes
C39 . C40 . 1.379(2) yes
C39 . H391 . 0.941 no
C40 . C41 . 1.379(3) yes
C40 . H401 . 0.956 no
C41 . C42 . 1.376(3) yes
C41 . H411 . 0.953 no
C42 . C43 . 1.386(2) yes
C42 . H421 . 0.948 no
C43 . H431 . 0.953 no
C51 . C52 . 1.516(2) yes
C51 . C58 . 1.527(2) yes
C51 . H511 . 1.008 no
C52 . C53 . 1.381(2) yes
C52 . C57 . 1.381(2) yes
C53 . C54 . 1.387(2) yes
C53 . H531 . 0.940 no
C54 . C55 . 1.380(3) yes
C54 . H541 . 0.923 no
C55 . C56 . 1.366(3) yes
C55 . H551 . 0.924 no
C56 . C57 . 1.379(3) yes
C56 . H561 . 0.967 no
C57 . H571 . 0.941 no
C58 . C63 . 1.393(2) yes
C81 . C80 . 1.514(2) yes
C81 . C82 . 1.517(2) yes
C81 . H811 . 0.973 no
C81 . H812 . 0.953 no
C60 . H601 . 0.945 no
C83 . C82 . 1.512(2) yes
C83 . H831 . 0.975 no
C83 . H832 . 0.980 no
C83 . H833 . 0.972 no
C62 . C63 . 1.380(3) yes
C62 . H621 . 0.930 no
C63 . H631 . 0.937 no
N71 . C72 . 1.5193(18) yes
N71 . C76 . 1.5249(18) yes
N71 . C80 . 1.5170(17) yes
N71 . C84 . 1.5197(18) yes
C72 . C73 . 1.517(2) yes
C72 . H721 . 0.957 no
C72 . H722 . 0.981 no
C73 . C74 . 1.512(2) yes
C73 . H731 . 0.972 no
C73 . H732 . 0.955 no
C74 . C75 . 1.514(2) yes
C74 . H741 . 0.960 no
C74 . H742 . 0.980 no
C75 . H753 . 0.972 no
C75 . H752 . 0.962 no
C75 . H751 . 0.986 no
C76 . C77 . 1.510(2) yes
C76 . H762 . 0.964 no
C76 . H761 . 0.959 no
C77 . C78 . 1.521(2) yes
C77 . H771 . 0.977 no
C77 . H772 . 0.972 no
C78 . C79 . 1.516(2) yes
C78 . H781 . 0.983 no
C78 . H782 . 0.981 no
C79 . H793 . 0.973 no
C79 . H792 . 0.985 no
C79 . H791 . 0.987 no
C80 . H801 . 0.976 no
C80 . H802 . 0.957 no
C117 . C112 . 1.374(4) yes
C117 . C116 . 1.390(4) yes
C117 . H1171 . 0.915 no
C82 . H821 . 0.987 no
C82 . H822 . 0.972 no
C115 . C116 . 1.381(4) yes
C115 . C114 . 1.360(4) yes
C115 . H1151 . 0.954 no
C84 . C85 . 1.513(2) yes
C84 . H841 . 0.986 no
C84 . H842 . 0.981 no
C85 . C86 . 1.517(2) yes
C85 . H851 . 0.961 no
C85 . H852 . 0.957 no
C86 . C87 . 1.512(3) yes
C86 . H862 . 0.983 no
C86 . H861 . 0.969 no
C87 . H873 . 0.942 no
C87 . H872 . 0.979 no
C87 . H871 . 0.985 no
C112 . C113 . 1.405(4) yes
C116 . H1161 . 0.932 no
C14 . H141 . 0.932 no
C114 . C113 . 1.387(4) yes
C114 . H1141 . 0.954 no
C113 . H1131 . 0.931 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C11 . O1 . H11 . 111.5 no
C31 . O2 . H21 . 103.8 no
C51 . O3 . H31 . 109.2 no
O1 . C11 . C18 . 110.71(14) yes
O1 . C11 . C12 . 113.1(5) yes
C18 . C11 . C12 . 113.6(7) yes
O1 . C11 . H111 . 97.2 no
C18 . C11 . H111 . 113.1 no
C12 . C11 . H111 . 108.1 no
O1 . C11 . C18 . 110.71(14) yes
O1 . C11 . C112 . 108.4(5) yes
C18 . C11 . C112 . 111.8(6) yes
O1 . C11 . H111 . 97.2 no
C18 . C11 . H111 . 113.1 no
C112 . C11 . H111 . 114.6 no
C58 . C59 . C60 . 120.24(18) yes
C58 . C59 . H591 . 120.3 no
C60 . C59 . H591 . 119.4 no
C12 . C13 . C14 . 121.01(6) yes
C12 . C13 . H131 . 119.1 no
C14 . C13 . H131 . 119.9 no
C60 . C61 . C62 . 119.58(18) yes
C60 . C61 . H611 . 120.6 no
C62 . C61 . H611 . 119.8 no
C16 . C15 . C14 . 120.36(6) yes
C16 . C15 . H151 . 121.1 no
C14 . C15 . H151 . 118.6 no
C15 . C16 . C17 . 119.82(6) yes
C15 . C16 . H161 . 120.5 no
C17 . C16 . H161 . 119.6 no
C16 . C17 . C12 . 120.98(6) yes
C16 . C17 . H171 . 120.3 no
C12 . C17 . H171 . 118.7 no
C11 . C18 . C19 . 120.66(15) yes
C11 . C18 . C23 . 121.53(14) yes
C19 . C18 . C23 . 117.73(16) yes
C18 . C19 . C20 . 120.81(17) yes
C18 . C19 . H191 . 118.8 no
C20 . C19 . H191 . 120.3 no
C19 . C20 . C21 . 120.91(18) yes
C19 . C20 . H201 . 119.7 no
C21 . C20 . H201 . 119.4 no
C20 . C21 . C22 . 118.99(17) yes
C20 . C21 . H211 . 121.1 no
C22 . C21 . H211 . 119.9 no
C21 . C22 . C23 . 120.26(17) yes
C21 . C22 . H221 . 120.3 no
C23 . C22 . H221 . 119.5 no
C18 . C23 . C22 . 121.30(16) yes
C18 . C23 . H231 . 120.1 no
C22 . C23 . H231 . 118.5 no
O2 . C31 . C32 . 109.01(12) yes
O2 . C31 . C38 . 112.49(12) yes
C32 . C31 . C38 . 108.77(12) yes
O2 . C31 . H311 . 109.0 no
C32 . C31 . H311 . 109.3 no
C38 . C31 . H311 . 108.3 no
C31 . C32 . C33 . 121.67(14) yes
C31 . C32 . C37 . 119.93(14) yes
C33 . C32 . C37 . 118.36(15) yes
C32 . C33 . C34 . 120.31(16) yes
C32 . C33 . H331 . 119.9 no
C34 . C33 . H331 . 119.8 no
C33 . C34 . C35 . 120.45(18) yes
C33 . C34 . H341 . 119.2 no
C35 . C34 . H341 . 120.3 no
C34 . C35 . C36 . 119.76(17) yes
C34 . C35 . H351 . 120.0 no
C36 . C35 . H351 . 120.2 no
C35 . C36 . C37 . 119.96(17) yes
C35 . C36 . H361 . 119.9 no
C37 . C36 . H361 . 120.2 no
C32 . C37 . C36 . 121.17(17) yes
C32 . C37 . H371 . 120.3 no
C36 . C37 . H371 . 118.6 no
C31 . C38 . C39 . 120.06(14) yes
C31 . C38 . C43 . 121.74(14) yes
C39 . C38 . C43 . 118.07(15) yes
C38 . C39 . C40 . 120.91(15) yes
C38 . C39 . H391 . 119.8 no
C40 . C39 . H391 . 119.3 no
C39 . C40 . C41 . 120.59(16) yes
C39 . C40 . H401 . 119.9 no
C41 . C40 . H401 . 119.5 no
C40 . C41 . C42 . 119.06(16) yes
C40 . C41 . H411 . 120.6 no
C42 . C41 . H411 . 120.4 no
C41 . C42 . C43 . 120.50(16) yes
C41 . C42 . H421 . 119.7 no
C43 . C42 . H421 . 119.8 no
C42 . C43 . C38 . 120.87(16) yes
C42 . C43 . H431 . 121.1 no
C38 . C43 . H431 . 118.1 no
O3 . C51 . C52 . 107.60(12) yes
O3 . C51 . C58 . 113.19(13) yes
C52 . C51 . C58 . 111.51(12) yes
O3 . C51 . H511 . 106.0 no
C52 . C51 . H511 . 109.8 no
C58 . C51 . H511 . 108.6 no
C51 . C52 . C53 . 120.27(14) yes
C51 . C52 . C57 . 121.21(15) yes
C53 . C52 . C57 . 118.53(15) yes
C52 . C53 . C54 . 120.44(16) yes
C52 . C53 . H531 . 119.0 no
C54 . C53 . H531 . 120.5 no
C53 . C54 . C55 . 120.11(18) yes
C53 . C54 . H541 . 118.4 no
C55 . C54 . H541 . 121.5 no
C54 . C55 . C56 . 119.62(17) yes
C54 . C55 . H551 . 120.2 no
C56 . C55 . H551 . 120.1 no
C55 . C56 . C57 . 120.28(18) yes
C55 . C56 . H561 . 120.5 no
C57 . C56 . H561 . 119.2 no
C52 . C57 . C56 . 121.01(18) yes
C52 . C57 . H571 . 120.0 no
C56 . C57 . H571 . 118.9 no
C51 . C58 . C59 . 121.85(14) yes
C51 . C58 . C63 . 119.67(15) yes
C59 . C58 . C63 . 118.47(15) yes
C80 . C81 . C82 . 109.29(12) yes
C80 . C81 . H811 . 110.5 no
C82 . C81 . H811 . 108.2 no
C80 . C81 . H812 . 110.4 no
C82 . C81 . H812 . 109.7 no
H811 . C81 . H812 . 108.7 no
C59 . C60 . C61 . 120.5(2) yes
C59 . C60 . H601 . 118.9 no
C61 . C60 . H601 . 120.6 no
C82 . C83 . H831 . 111.4 no
C82 . C83 . H832 . 109.6 no
H831 . C83 . H832 . 110.0 no
C82 . C83 . H833 . 109.6 no
H831 . C83 . H833 . 108.6 no
H832 . C83 . H833 . 107.5 no
C61 . C62 . C63 . 120.40(19) yes
C61 . C62 . H621 . 120.3 no
C63 . C62 . H621 . 119.3 no
C58 . C63 . C62 . 120.77(18) yes
C58 . C63 . H631 . 119.4 no
C62 . C63 . H631 . 119.8 no
C72 . N71 . C76 . 111.28(11) yes
C72 . N71 . C80 . 106.13(10) yes
C76 . N71 . C80 . 110.89(11) yes
C72 . N71 . C84 . 111.10(11) yes
C76 . N71 . C84 . 106.17(10) yes
C80 . N71 . C84 . 111.35(11) yes
N71 . C72 . C73 . 115.89(12) yes
N71 . C72 . H721 . 106.0 no
C73 . C72 . H721 . 110.1 no
N71 . C72 . H722 . 106.1 no
C73 . C72 . H722 . 109.5 no
H721 . C72 . H722 . 109.0 no
C72 . C73 . C74 . 110.37(13) yes
C72 . C73 . H731 . 110.3 no
C74 . C73 . H731 . 108.6 no
C72 . C73 . H732 . 110.3 no
C74 . C73 . H732 . 108.4 no
H731 . C73 . H732 . 108.8 no
C73 . C74 . C75 . 112.91(15) yes
C73 . C74 . H741 . 109.4 no
C75 . C74 . H741 . 111.3 no
C73 . C74 . H742 . 107.1 no
C75 . C74 . H742 . 110.0 no
H741 . C74 . H742 . 105.9 no
C74 . C75 . H753 . 110.6 no
C74 . C75 . H752 . 111.1 no
H753 . C75 . H752 . 107.7 no
C74 . C75 . H751 . 111.9 no
H753 . C75 . H751 . 108.2 no
H752 . C75 . H751 . 107.1 no
N71 . C76 . C77 . 115.78(11) yes
N71 . C76 . H762 . 105.5 no
C77 . C76 . H762 . 110.9 no
N71 . C76 . H761 . 105.9 no
C77 . C76 . H761 . 110.2 no
H762 . C76 . H761 . 108.1 no
C76 . C77 . C78 . 110.20(13) yes
C76 . C77 . H771 . 110.4 no
C78 . C77 . H771 . 108.0 no
C76 . C77 . H772 . 109.4 no
C78 . C77 . H772 . 109.6 no
H771 . C77 . H772 . 109.1 no
C77 . C78 . C79 . 112.20(14) yes
C77 . C78 . H781 . 108.9 no
C79 . C78 . H781 . 110.3 no
C77 . C78 . H782 . 108.3 no
C79 . C78 . H782 . 109.4 no
H781 . C78 . H782 . 107.6 no
C78 . C79 . H793 . 111.0 no
C78 . C79 . H792 . 110.8 no
H793 . C79 . H792 . 108.1 no
C78 . C79 . H791 . 110.6 no
H793 . C79 . H791 . 107.5 no
H792 . C79 . H791 . 108.7 no
N71 . C80 . C81 . 116.36(11) yes
N71 . C80 . H801 . 106.7 no
C81 . C80 . H801 . 110.1 no
N71 . C80 . H802 . 105.6 no
C81 . C80 . H802 . 109.0 no
H801 . C80 . H802 . 108.7 no
C112 . C117 . C116 . 121.04(6) yes
C112 . C117 . H1171 . 118.7 no
C116 . C117 . H1171 . 120.3 no
C81 . C82 . C83 . 112.41(13) yes
C81 . C82 . H821 . 109.5 no
C83 . C82 . H821 . 108.9 no
C81 . C82 . H822 . 108.7 no
C83 . C82 . H822 . 108.7 no
H821 . C82 . H822 . 108.6 no
C116 . C115 . C114 . 120.37(6) yes
C116 . C115 . H1151 . 119.9 no
C114 . C115 . H1151 . 119.7 no
N71 . C84 . C85 . 115.82(12) yes
N71 . C84 . H841 . 105.8 no
C85 . C84 . H841 . 110.9 no
N71 . C84 . H842 . 105.9 no
C85 . C84 . H842 . 109.3 no
H841 . C84 . H842 . 108.7 no
C84 . C85 . C86 . 110.08(13) yes
C84 . C85 . H851 . 110.9 no
C86 . C85 . H851 . 109.0 no
C84 . C85 . H852 . 110.1 no
C86 . C85 . H852 . 109.2 no
H851 . C85 . H852 . 107.6 no
C85 . C86 . C87 . 112.78(15) yes
C85 . C86 . H862 . 108.4 no
C87 . C86 . H862 . 110.5 no
C85 . C86 . H861 . 107.3 no
C87 . C86 . H861 . 109.6 no
H862 . C86 . H861 . 108.1 no
C86 . C87 . H873 . 109.6 no
C86 . C87 . H872 . 109.5 no
H873 . C87 . H872 . 109.0 no
C86 . C87 . H871 . 111.5 no
H873 . C87 . H871 . 108.1 no
H872 . C87 . H871 . 109.1 no
C11 . C112 . C117 . 121.00(6) yes
C11 . C112 . C113 . 121.07(6) yes
C117 . C112 . C113 . 117.91(6) yes
C117 . C116 . C115 . 119.89(6) yes
C117 . C116 . H1161 . 118.9 no
C115 . C116 . H1161 . 121.2 no
C11 . C12 . C13 . 121.02(6) yes
C11 . C12 . C17 . 121.02(6) yes
C13 . C12 . C17 . 117.93(6) yes
C13 . C14 . C15 . 119.82(6) yes
C13 . C14 . H141 . 119.6 no
C15 . C14 . H141 . 120.6 no
C115 . C114 . C113 . 119.79(6) yes
C115 . C114 . H1141 . 119.5 no
C113 . C114 . H1141 . 120.7 no
C112 . C113 . C114 . 120.98(6) yes
C112 . C113 . H1131 . 120.0 no
C114 . C113 . H1131 . 119.0 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C84 . H841 . O1 . 129.95 0.986 2.589 3.310(5) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 30/04/13 at 12:19:52
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE O   (   1,X'S) H   (  11,X'S) 
RIDE O   (   2,X'S) H   (  21,X'S) 
RIDE O   (   3,X'S) H   (  31,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) H   ( 812,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) H   ( 832,X'S) H   ( 833,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) H   ( 732,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) H   ( 742,X'S) 
RIDE C   (  75,X'S) H   ( 753,X'S) H   ( 752,X'S) H   ( 751,X'S) 
RIDE C   (  76,X'S) H   ( 762,X'S) H   ( 761,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) H   ( 772,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) H   ( 782,X'S) 
RIDE C   (  79,X'S) H   ( 793,X'S) H   ( 792,X'S) H   ( 791,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) H   ( 802,X'S) 
RIDE C   ( 117,X'S) H   (1171,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) H   ( 822,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) H   ( 842,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) H   ( 852,X'S) 
RIDE C   (  86,X'S) H   ( 862,X'S) H   ( 861,X'S) 
RIDE C   (  87,X'S) H   ( 873,X'S) H   ( 872,X'S) H   ( 871,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 30/04/13 at 12:19:52
#
#LIST     16                                                                    
SAME C(11)  C(12)  C(17)  C(16)  C(15)  C(14)  C(13) AND 
CONT C(11)  C(12)  C(13)  C(14)  C(15)  C(16)  C(17) AND 
CONT C(11)  C(112)  C(117)  C(116)  C(115)  C(114)  C(113) AND 
CONT C(11)  C(112)  C(113)  C(114)  C(115)  C(116)  C(117) 
SIMU 0.01   C(11)  C(12)  C(17)  C(16)  C(15)  C(14)  C(13) AND 
CONT C(11)  C(12)  C(13)  C(14)  C(15)  C(16)  C(17) AND 
CONT C(11)  C(112)  C(117)  C(116)  C(115)  C(114)  C(113) AND 
CONT C(11)  C(112)  C(113)  C(114)  C(115)  C(116)  C(117) 
DELU 0.01   C(11)  C(12)  C(17)  C(16)  C(15)  C(14)  C(13) AND 
CONT C(11)  C(12)  C(13)  C(14)  C(15)  C(16)  C(17) AND 
CONT C(11)  C(112)  C(117)  C(116)  C(115)  C(114)  C(113) AND 
CONT C(11)  C(112)  C(113)  C(114)  C(115)  C(116)  C(117) 
END                                                                             
;
####################################################################### 
# 
# 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_2l
_database_code_depnum_ccdc_archive 'CCDC 1401776'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             13-04-25
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 010gwp12
_chemical_name_systematic        .
_chemical_melting_point          'not measured'


_refine_special_details          
; 
After the initial structure solution, a difference Fourier map 
indicated the presence of residual electron density, clearly 
indicating the presence of a partially occupied hexane disordered 
around the inversion centre.  Despite copious use of restraints
and constraints, several different attempts to model it were 
unsuccessful giving problems including poor convergence and 
significant residual electron density.  Thus, SQUEEZE was used 
leaving a void from which the electron density was removed.
This model converged readily and R1 was 2% lower than the best
atomic model.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 154 47 ' '
2 0.500 0.500 0.000 154 47 ' '
_platon_squeeze_details          
; 
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure 
factors.
;

_cell_length_a                   11.2887(1)
_cell_length_b                   17.6025(1)
_cell_length_c                   24.9660(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.4318(7)
_cell_angle_gamma                90
_cell_volume                     4907.35(7)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C54 H68 F1 N1 O2 
# Dc =      1.06 Fooo =   1696.00 Mu =      5.04 M =    782.14
# Found Formula = C54.00 H68 F1 N1 O2 
# Dc =      1.06 FOOO =   1696.00 Mu =      5.04 M =    782.14

_chemical_formula_sum            'C54 H68 F1 N1 O2'
_chemical_formula_moiety         '2(C19 H16 O), C16 H36 N, F'
_chemical_compound_source        .
_chemical_formula_weight         782.14


_cell_measurement_reflns_used    49297
_cell_measurement_theta_min      3
_cell_measurement_theta_max      77
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.220
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_max          0.300

_exptl_crystal_density_diffrn    1.059
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1696.000
_exptl_absorpt_coefficient_mu    0.504

# Sheldrick geometric approximatio 0.89 0.90 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_T_max  0.90
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            117478
_reflns_number_total             10345
_diffrn_reflns_av_R_equivalents  0.035
# Number of reflections with Friedels Law is 10345 
# Theoretical number of reflections is about 20732 


_diffrn_reflns_theta_min         3.083
_diffrn_reflns_theta_max         76.917
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        76.917
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       31
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              31

_oxford_diffrn_Wilson_B_factor   4.03
_oxford_diffrn_Wilson_scale      0.10

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.60
_refine_diff_density_max         0.69


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         10304
_refine_ls_number_restraints     1269
_refine_ls_number_parameters     836
_oxford_refine_ls_R_factor_ref   0.0614
_refine_ls_wR_factor_ref         0.1454
_refine_ls_goodness_of_fit_ref   0.9822
_refine_ls_shift/su_max          0.0008927
_refine_ls_shift/su_mean         0.0000764


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        10304
_refine_ls_R_factor_all          0.0614
_refine_ls_wR_factor_all         0.1454

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8934
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_gt          0.1394

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.07P)² + 1.96P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
F1 F 0.70392(8) 0.66013(5) 0.69178(3) 0.0436 1.0000 Uani . . . . . .
O1 O 0.57356(9) 0.72725(6) 0.74912(4) 0.0376 1.0000 Uani . . . . . .
C101 C 0.55234(12) 0.69143(8) 0.79752(5) 0.0368 1.0000 Uani D . . . . .
C102 C 0.47219(13) 0.62057(8) 0.78477(6) 0.0373 1.0000 Uani . . . . . .
C103 C 0.47379(14) 0.58051(9) 0.73709(6) 0.0393 1.0000 Uani . . . . . .
C104 C 0.40159(16) 0.51694(10) 0.72553(8) 0.0510 1.0000 Uani . . . . . .
C105 C 0.32842(16) 0.49216(11) 0.76173(10) 0.0609 1.0000 Uani . . . . . .
C106 C 0.32726(19) 0.53095(11) 0.80915(10) 0.0652 1.0000 Uani . . . . . .
C107 C 0.39740(18) 0.59467(10) 0.82057(8) 0.0538 1.0000 Uani . . . . . .
C108 C 0.4744(5) 0.7485(4) 0.8236(2) 0.0468 0.63(2) Uani D . P 1 1 .
C109 C 0.3612(5) 0.7663(5) 0.79861(18) 0.0451 0.63(2) Uani D . P 1 1 .
C110 C 0.2942(6) 0.8225(4) 0.8197(3) 0.0527 0.63(2) Uani D . P 1 1 .
C111 C 0.3398(8) 0.8602(3) 0.8669(4) 0.0527 0.63(2) Uani D . P 1 1 .
C112 C 0.4520(8) 0.8433(3) 0.8922(3) 0.0533 0.63(2) Uani D . P 1 1 .
C113 C 0.5210(6) 0.7886(4) 0.8706(3) 0.0496 0.63(2) Uani D . P 1 1 .
C114 C 0.6649(3) 0.6654(5) 0.8344(3) 0.0428 0.60(2) Uani D . P 2 1 .
C115 C 0.6569(7) 0.6206(4) 0.8798(3) 0.0582 0.60(2) Uani D . P 2 1 .
C116 C 0.7589(9) 0.6008(4) 0.9149(2) 0.0687 0.60(2) Uani D . P 2 1 .
C117 C 0.8696(7) 0.6256(5) 0.9056(3) 0.0654 0.60(2) Uani D . P 2 1 .
C118 C 0.8787(4) 0.6700(5) 0.8614(3) 0.0609 0.60(2) Uani D . P 2 1 .
C119 C 0.7765(4) 0.6893(5) 0.8254(3) 0.0507 0.60(2) Uani D . P 2 1 .
O2 O 0.70003(10) 0.74871(6) 0.61047(4) 0.0449 1.0000 Uani . . . . . .
C201 C 0.65432(15) 0.71905(8) 0.55807(5) 0.0451 1.0000 Uani D . . . . .
C202 C 0.51994(16) 0.70406(8) 0.55372(6) 0.0417 1.0000 Uani . . . . . .
C203 C 0.4382(2) 0.72169(10) 0.50784(7) 0.0551 1.0000 Uani . . . . . .
C204 C 0.3181(2) 0.70540(12) 0.50516(8) 0.0669 1.0000 Uani . . . . . .
C205 C 0.2754(2) 0.67142(12) 0.54800(9) 0.0663 1.0000 Uani . . . . . .
C206 C 0.35483(19) 0.65287(11) 0.59360(8) 0.0595 1.0000 Uani . . . . . .
C207 C 0.47535(17) 0.66902(10) 0.59648(7) 0.0492 1.0000 Uani . . . . . .
C208 C 0.6734(3) 0.78135(11) 0.51717(10) 0.0425 0.746(10) Uani D . P 3 1 .
C209 C 0.7009(4) 0.76293(16) 0.46545(11) 0.0529 0.746(10) Uani D . P 3 1 .
C210 C 0.7154(3) 0.8197(2) 0.42869(12) 0.0602 0.746(10) Uani D . P 3 1 .
C211 C 0.7003(3) 0.8945(2) 0.44176(14) 0.0614 0.746(10) Uani D . P 3 1 .
C212 C 0.6700(6) 0.91285(16) 0.4917(2) 0.0549 0.746(10) Uani D . P 3 1 .
C213 C 0.6548(5) 0.85634(17) 0.52874(16) 0.0425 0.746(10) Uani D . P 3 1 .
C214 C 0.7298(4) 0.6513(3) 0.5466(3) 0.0553 0.538(14) Uani D . P 4 1 .
C215 C 0.8455(5) 0.6420(4) 0.5740(3) 0.0570 0.538(14) Uani D . P 4 1 .
C216 C 0.9165(5) 0.5819(4) 0.5613(3) 0.0576 0.538(14) Uani D . P 4 1 .
C217 C 0.8711(7) 0.5290(3) 0.5239(2) 0.0524 0.538(14) Uani D . P 4 1 .
C218 C 0.7582(9) 0.5378(3) 0.49665(16) 0.0638 0.538(14) Uani D . P 4 1 .
C219 C 0.6880(7) 0.6000(4) 0.50756(18) 0.0611 0.538(14) Uani D . P 4 1 .
C308 C 0.4915(8) 0.7551(5) 0.8270(3) 0.0288 0.37(2) Uani D . P 1 2 .
C309 C 0.3841(11) 0.7852(7) 0.8044(3) 0.0470 0.37(2) Uani D . P 1 2 .
C310 C 0.3248(13) 0.8377(6) 0.8329(6) 0.0574 0.37(2) Uani D . P 1 2 .
C311 C 0.3783(15) 0.8648(5) 0.8821(6) 0.0536 0.37(2) Uani D . P 1 2 .
C312 C 0.4872(14) 0.8373(6) 0.9044(5) 0.0558 0.37(2) Uani D . P 1 2 .
C313 C 0.5441(11) 0.7821(7) 0.8777(4) 0.0450 0.37(2) Uani D . P 1 2 .
C314 C 0.6779(5) 0.6747(8) 0.8301(5) 0.0465 0.40(2) Uani D . P 2 2 .
C315 C 0.6914(10) 0.6230(6) 0.8730(4) 0.0603 0.40(2) Uani D . P 2 2 .
C316 C 0.8032(13) 0.6108(5) 0.9036(5) 0.0682 0.40(2) Uani D . P 2 2 .
C317 C 0.9029(9) 0.6462(7) 0.8901(5) 0.0657 0.40(2) Uani D . P 2 2 .
C318 C 0.8916(5) 0.6955(8) 0.8467(5) 0.0588 0.40(2) Uani D . P 2 2 .
C319 C 0.7792(5) 0.7098(7) 0.8168(4) 0.0471 0.40(2) Uani D . P 2 2 .
C408 C 0.6890(12) 0.7898(3) 0.5254(4) 0.0652 0.254(10) Uani D . P 3 2 .
C409 C 0.7540(13) 0.7811(4) 0.4818(5) 0.0696 0.254(10) Uani D . P 3 2 .
C410 C 0.7681(15) 0.8421(5) 0.4476(5) 0.0808 0.254(10) Uani D . P 3 2 .
C411 C 0.7227(14) 0.9120(5) 0.4574(5) 0.0736 0.254(10) Uani D . P 3 2 .
C412 C 0.665(2) 0.9223(5) 0.5023(6) 0.0596 0.254(10) Uani D . P 3 2 .
C413 C 0.6516(18) 0.8612(4) 0.5369(6) 0.0556 0.254(10) Uani D . P 3 2 .
C414 C 0.7130(3) 0.6418(3) 0.5462(3) 0.0494 0.462(14) Uani D . P 4 2 .
C415 C 0.8326(5) 0.6293(4) 0.5628(4) 0.0561 0.462(14) Uani D . P 4 2 .
C416 C 0.8870(5) 0.5615(4) 0.5494(3) 0.0528 0.462(14) Uani D . P 4 2 .
C417 C 0.8227(7) 0.5086(3) 0.5157(2) 0.0504 0.462(14) Uani D . P 4 2 .
C418 C 0.7025(7) 0.5198(3) 0.49874(17) 0.0488 0.462(14) Uani D . P 4 2 .
C419 C 0.6459(5) 0.5847(3) 0.51440(18) 0.0453 0.462(14) Uani D . P 4 2 .
N501 N 0.85385(12) 0.46070(6) 0.75228(6) 0.0468 1.0000 Uani D . . . . .
C502 C 0.75633(13) 0.46358(7) 0.78823(6) 0.0398 1.0000 Uani D . . . . .
C503 C 0.69081(16) 0.38999(8) 0.79425(7) 0.0484 1.0000 Uani D . . . . .
C504 C 0.60346(15) 0.40073(8) 0.83410(7) 0.0480 1.0000 Uani D . . . . .
C505 C 0.51875(18) 0.33445(11) 0.83462(8) 0.0631 1.0000 Uani D . . . . .
C506 C 0.8954(12) 0.5434(3) 0.7506(7) 0.0456 0.56(3) Uani D . P 5 1 .
C507 C 1.0013(7) 0.5581(4) 0.7204(5) 0.0522 0.56(3) Uani D . P 5 1 .
C508 C 1.0400(7) 0.6410(4) 0.7282(6) 0.0569 0.56(3) Uani D . P 5 1 .
C509 C 1.1365(7) 0.6631(6) 0.6952(6) 0.0640 0.56(3) Uani D . P 5 1 .
C510 C 0.9597(10) 0.4092(5) 0.7812(3) 0.0590 0.491(15) Uani D . P 6 1 .
C511 C 1.0172(7) 0.4343(4) 0.8390(3) 0.0583 0.491(15) Uani D . P 6 1 .
C512 C 1.1097(6) 0.3722(3) 0.8636(5) 0.0732 0.491(15) Uani D . P 6 1 .
C513 C 1.1669(6) 0.3896(5) 0.9186(5) 0.0781 0.491(15) Uani D . P 6 1 .
C514 C 0.80564(18) 0.42998(8) 0.69679(7) 0.0595 1.0000 Uani D . . . . .
C515 C 0.70087(18) 0.47211(9) 0.66620(7) 0.0623 1.0000 Uani D . . . . .
C516 C 0.6733(4) 0.4383(2) 0.61267(17) 0.0744 0.468(5) Uani D . P 7 1 .
C517 C 0.5662(5) 0.4600(3) 0.58572(18) 0.0758 0.468(5) Uani D . P 7 1 .
C606 C 0.9004(15) 0.5402(4) 0.7470(8) 0.0468 0.44(3) Uani D . P 5 2 .
C607 C 0.9913(10) 0.5500(5) 0.7089(5) 0.0527 0.44(3) Uani D . P 5 2 .
C608 C 1.0307(9) 0.6323(5) 0.7096(7) 0.0595 0.44(3) Uani D . P 5 2 .
C609 C 1.1278(9) 0.6466(7) 0.6763(6) 0.0610 0.44(3) Uani D . P 5 2 .
C610 C 0.9485(9) 0.4064(5) 0.7703(3) 0.0566 0.509(15) Uani D . P 6 2 .
C611 C 1.0125(7) 0.4176(4) 0.8259(3) 0.0569 0.509(15) Uani D . P 6 2 .
C612 C 1.1082(5) 0.3590(3) 0.8377(4) 0.0622 0.509(15) Uani D . P 6 2 .
C613 C 1.1733(5) 0.3638(4) 0.8936(4) 0.0684 0.509(15) Uani D . P 6 2 .
C617 C 0.6383(4) 0.4219(2) 0.61637(12) 0.0791 0.532(5) Uani D . P 7 2 .
C618 C 0.5413(4) 0.3712(2) 0.63072(14) 0.0629 0.532(5) Uani D . P 7 2 .
H1031 H 0.5241 0.5969 0.7127 0.0463 1.0000 Uiso R . . . . .
H1041 H 0.4029 0.4912 0.6926 0.0614 1.0000 Uiso R . . . . .
H1051 H 0.2794 0.4487 0.7538 0.0732 1.0000 Uiso R . . . . .
H1061 H 0.2779 0.5131 0.8346 0.0780 1.0000 Uiso R . . . . .
H1071 H 0.3936 0.6218 0.8533 0.0658 1.0000 Uiso R . . . . .
H1091 H 0.3287 0.7396 0.7669 0.0536 0.63(2) Uiso R . P 1 1 .
H1101 H 0.2171 0.8341 0.8016 0.0631 0.63(2) Uiso R . P 1 1 .
H1111 H 0.2917 0.8968 0.8818 0.0628 0.63(2) Uiso R . P 1 1 .
H1121 H 0.4825 0.8689 0.9243 0.0644 0.63(2) Uiso R . P 1 1 .
H1131 H 0.5985 0.7787 0.8888 0.0600 0.63(2) Uiso R . P 1 1 .
H1151 H 0.5817 0.6034 0.8870 0.0695 0.60(2) Uiso R . P 2 1 .
H1161 H 0.7509 0.5708 0.9456 0.0820 0.60(2) Uiso R . P 2 1 .
H1171 H 0.9388 0.6118 0.9295 0.0778 0.60(2) Uiso R . P 2 1 .
H1181 H 0.9535 0.6869 0.8548 0.0736 0.60(2) Uiso R . P 2 1 .
H1191 H 0.7818 0.7190 0.7945 0.0606 0.60(2) Uiso R . P 2 1 .
H2031 H 0.4677 0.7447 0.4790 0.0658 1.0000 Uiso R . . . . .
H2041 H 0.2650 0.7188 0.4745 0.0799 1.0000 Uiso R . . . . .
H2051 H 0.1921 0.6611 0.5455 0.0794 1.0000 Uiso R . . . . .
H2061 H 0.3255 0.6282 0.6237 0.0713 1.0000 Uiso R . . . . .
H2071 H 0.5292 0.6549 0.6275 0.0589 1.0000 Uiso R . . . . .
H2091 H 0.7138 0.7116 0.4556 0.0634 0.746(10) Uiso R . P 3 1 .
H2101 H 0.7363 0.8073 0.3936 0.0713 0.746(10) Uiso R . P 3 1 .
H2111 H 0.7099 0.9342 0.4167 0.0743 0.746(10) Uiso R . P 3 1 .
H2121 H 0.6570 0.9637 0.5016 0.0664 0.746(10) Uiso R . P 3 1 .
H2131 H 0.6317 0.8669 0.5631 0.0507 0.746(10) Uiso R . P 3 1 .
H2151 H 0.8745 0.6766 0.6014 0.0681 0.538(14) Uiso R . P 4 1 .
H2161 H 0.9968 0.5766 0.5791 0.0700 0.538(14) Uiso R . P 4 1 .
H2171 H 0.9172 0.4866 0.5162 0.0628 0.538(14) Uiso R . P 4 1 .
H2181 H 0.7257 0.5022 0.4705 0.0762 0.538(14) Uiso R . P 4 1 .
H2191 H 0.6098 0.6067 0.4887 0.0732 0.538(14) Uiso R . P 4 1 .
H3091 H 0.3521 0.7701 0.7691 0.0562 0.37(2) Uiso R . P 1 2 .
H3101 H 0.2480 0.8541 0.8181 0.0695 0.37(2) Uiso R . P 1 2 .
H3111 H 0.3388 0.9022 0.9001 0.0642 0.37(2) Uiso R . P 1 2 .
H3121 H 0.5235 0.8561 0.9382 0.0671 0.37(2) Uiso R . P 1 2 .
H3131 H 0.6173 0.7629 0.8945 0.0539 0.37(2) Uiso R . P 1 2 .
H3151 H 0.6241 0.5974 0.8812 0.0718 0.40(2) Uiso R . P 2 2 .
H3161 H 0.8115 0.5779 0.9332 0.0823 0.40(2) Uiso R . P 2 2 .
H3171 H 0.9789 0.6364 0.9101 0.0790 0.40(2) Uiso R . P 2 2 .
H3181 H 0.9600 0.7193 0.8369 0.0712 0.40(2) Uiso R . P 2 2 .
H3191 H 0.7718 0.7435 0.7872 0.0565 0.40(2) Uiso R . P 2 2 .
H4091 H 0.7887 0.7341 0.4753 0.0840 0.254(10) Uiso R . P 3 2 .
H4101 H 0.8080 0.8349 0.4177 0.0971 0.254(10) Uiso R . P 3 2 .
H4111 H 0.7310 0.9527 0.4341 0.0880 0.254(10) Uiso R . P 3 2 .
H4121 H 0.6345 0.9700 0.5096 0.0708 0.254(10) Uiso R . P 3 2 .
H4131 H 0.6163 0.8687 0.5682 0.0669 0.254(10) Uiso R . P 3 2 .
H4151 H 0.8744 0.6666 0.5830 0.0669 0.462(14) Uiso R . P 4 2 .
H4161 H 0.9667 0.5528 0.5637 0.0631 0.462(14) Uiso R . P 4 2 .
H4171 H 0.8630 0.4652 0.5050 0.0598 0.462(14) Uiso R . P 4 2 .
H4181 H 0.6590 0.4823 0.4774 0.0595 0.462(14) Uiso R . P 4 2 .
H4191 H 0.5619 0.5904 0.5034 0.0540 0.462(14) Uiso R . P 4 2 .
H5022 H 0.7949 0.4814 0.8241 0.0483 1.0000 Uiso R . . . . .
H5021 H 0.6993 0.5017 0.7728 0.0458 1.0000 Uiso R . . . . .
H5031 H 0.7477 0.3491 0.8061 0.0589 1.0000 Uiso R . . . . .
H5032 H 0.6441 0.3755 0.7591 0.0593 1.0000 Uiso R . . . . .
H5042 H 0.6472 0.4089 0.8700 0.0582 1.0000 Uiso R . . . . .
H5041 H 0.5588 0.4473 0.8265 0.0581 1.0000 Uiso R . . . . .
H5053 H 0.4643 0.3434 0.8620 0.0944 1.0000 Uiso R . . . . .
H5052 H 0.5633 0.2883 0.8448 0.0940 1.0000 Uiso R . . . . .
H5051 H 0.4712 0.3269 0.7982 0.0949 1.0000 Uiso R . . . . .
H5061 H 0.9151 0.5590 0.7890 0.0547 0.56(3) Uiso R . P 5 1 .
H5062 H 0.8265 0.5720 0.7336 0.0539 0.56(3) Uiso R . P 5 1 .
H5071 H 1.0684 0.5256 0.7343 0.0627 0.56(3) Uiso R . P 5 1 .
H5072 H 0.9780 0.5473 0.6821 0.0634 0.56(3) Uiso R . P 5 1 .
H5082 H 1.0766 0.6499 0.7661 0.0677 0.56(3) Uiso R . P 5 1 .
H5081 H 0.9705 0.6737 0.7202 0.0671 0.56(3) Uiso R . P 5 1 .
H5093 H 1.1608 0.7159 0.7025 0.0956 0.56(3) Uiso R . P 5 1 .
H5092 H 1.2066 0.6315 0.7052 0.0953 0.56(3) Uiso R . P 5 1 .
H5091 H 1.1074 0.6585 0.6557 0.0963 0.56(3) Uiso R . P 5 1 .
H5101 H 1.0219 0.4091 0.7571 0.0707 0.491(15) Uiso R . P 6 1 .
H5102 H 0.9257 0.3596 0.7843 0.0708 0.491(15) Uiso R . P 6 1 .
H5112 H 1.0573 0.4822 0.8373 0.0697 0.491(15) Uiso R . P 6 1 .
H5111 H 0.9542 0.4413 0.8617 0.0696 0.491(15) Uiso R . P 6 1 .
H5122 H 1.1758 0.3564 0.8426 0.0849 0.491(15) Uiso R . P 6 1 .
H5121 H 1.0614 0.3270 0.8658 0.0872 0.491(15) Uiso R . P 6 1 .
H5131 H 1.2274 0.3506 0.9313 0.1166 0.491(15) Uiso R . P 6 1 .
H5132 H 1.2053 0.4393 0.9196 0.1168 0.491(15) Uiso R . P 6 1 .
H5133 H 1.1041 0.3906 0.9419 0.1172 0.491(15) Uiso R . P 6 1 .
H5142 H 0.8722 0.4296 0.6764 0.0701 1.0000 Uiso R . . . . .
H5141 H 0.7819 0.3778 0.7022 0.0697 1.0000 Uiso R . . . . .
H5161 H 0.7393 0.4514 0.5925 0.0889 0.468(5) Uiso R . P 7 1 .
H5162 H 0.6734 0.3797 0.6192 0.0901 0.468(5) Uiso R . P 7 1 .
H5172 H 0.5608 0.4414 0.5491 0.1135 0.468(5) Uiso R . P 7 1 .
H5171 H 0.5620 0.5141 0.5876 0.1135 0.468(5) Uiso R . P 7 1 .
H5173 H 0.5085 0.4356 0.6042 0.1128 0.468(5) Uiso R . P 7 1 .
H6062 H 0.9354 0.5551 0.7838 0.0563 0.44(3) Uiso R . P 5 2 .
H6061 H 0.8307 0.5717 0.7348 0.0551 0.44(3) Uiso R . P 5 2 .
H6071 H 1.0597 0.5177 0.7192 0.0627 0.44(3) Uiso R . P 5 2 .
H6072 H 0.9560 0.5365 0.6718 0.0630 0.44(3) Uiso R . P 5 2 .
H6082 H 1.0631 0.6478 0.7475 0.0713 0.44(3) Uiso R . P 5 2 .
H6081 H 0.9600 0.6629 0.6958 0.0704 0.44(3) Uiso R . P 5 2 .
H6091 H 1.1486 0.7012 0.6764 0.0917 0.44(3) Uiso R . P 5 2 .
H6092 H 1.1973 0.6167 0.6900 0.0915 0.44(3) Uiso R . P 5 2 .
H6093 H 1.0997 0.6309 0.6392 0.0920 0.44(3) Uiso R . P 5 2 .
H6102 H 1.0052 0.4094 0.7436 0.0670 0.509(15) Uiso R . P 6 2 .
H6101 H 0.9109 0.3570 0.7676 0.0673 0.509(15) Uiso R . P 6 2 .
H6112 H 1.0449 0.4681 0.8301 0.0678 0.509(15) Uiso R . P 6 2 .
H6111 H 0.9551 0.4114 0.8507 0.0681 0.509(15) Uiso R . P 6 2 .
H6121 H 1.1709 0.3661 0.8153 0.0750 0.509(15) Uiso R . P 6 2 .
H6122 H 1.0760 0.3085 0.8328 0.0747 0.509(15) Uiso R . P 6 2 .
H6133 H 1.2345 0.3234 0.8982 0.1027 0.509(15) Uiso R . P 6 2 .
H6132 H 1.2132 0.4133 0.8985 0.1030 0.509(15) Uiso R . P 6 2 .
H6131 H 1.1156 0.3560 0.9186 0.1031 0.509(15) Uiso R . P 6 2 .
H6172 H 0.7001 0.3937 0.5989 0.0959 0.532(5) Uiso R . P 7 2 .
H6171 H 0.5905 0.4548 0.5914 0.0933 0.532(5) Uiso R . P 7 2 .
H6181 H 0.4990 0.3486 0.5988 0.0938 0.532(5) Uiso R . P 7 2 .
H6182 H 0.5793 0.3314 0.6538 0.0941 0.532(5) Uiso R . P 7 2 .
H6183 H 0.4872 0.3986 0.6500 0.0945 0.532(5) Uiso R . P 7 2 .
H11 H 0.6208 0.6995 0.7321 0.0574 1.0000 Uiso R . . . . .
H21 H 0.6985 0.7158 0.6352 0.0670 1.0000 Uiso R . . . . .
H5151 H 0.7198 0.5252 0.6628 0.0745 0.468(5) Uiso R . P 7 1 .
H5152 H 0.6345 0.4677 0.6870 0.0748 0.468(5) Uiso R . P 7 1 .
H5153 H 0.6431 0.4851 0.6901 0.0745 0.532(5) Uiso R . P 7 2 .
H5154 H 0.7296 0.5191 0.6521 0.0745 0.532(5) Uiso R . P 7 2 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.35(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 . C101 . 1.4142(16) yes
O1 . H11 . 0.878 no
C101 . C102 . 1.546(2) yes
C101 . C108 . 1.541(4) yes
C101 . C114 . 1.526(3) yes
C101 . C102 . 1.546(2) yes
C101 . C114 . 1.526(3) yes
C101 . C308 . 1.555(4) yes
C101 . C102 . 1.546(2) yes
C101 . C108 . 1.541(4) yes
C101 . C314 . 1.556(5) yes
C101 . C102 . 1.546(2) yes
C101 . C308 . 1.555(4) yes
C101 . C314 . 1.556(5) yes
C102 . C103 . 1.386(2) yes
C102 . C107 . 1.393(2) yes
C103 . C104 . 1.390(2) yes
C103 . H1031 . 0.937 no
C104 . C105 . 1.381(3) yes
C104 . H1041 . 0.940 no
C105 . C106 . 1.368(3) yes
C105 . H1051 . 0.947 no
C106 . C107 . 1.378(3) yes
C106 . H1061 . 0.957 no
C107 . H1071 . 0.953 no
C108 . C109 . 1.373(4) yes
C108 . C113 . 1.405(4) yes
C109 . C110 . 1.394(4) yes
C109 . H1091 . 0.947 no
C110 . C111 . 1.384(4) yes
C110 . H1101 . 0.942 no
C111 . C112 . 1.363(4) yes
C111 . H1111 . 0.954 no
C112 . C113 . 1.395(4) yes
C112 . H1121 . 0.941 no
C113 . H1131 . 0.942 no
C114 . C115 . 1.396(4) yes
C114 . C119 . 1.377(4) yes
C115 . C116 . 1.385(4) yes
C115 . H1151 . 0.943 no
C116 . C117 . 1.376(4) yes
C116 . H1161 . 0.947 no
C117 . C118 . 1.368(4) yes
C117 . H1171 . 0.943 no
C118 . C119 . 1.396(4) yes
C118 . H1181 . 0.933 no
C119 . H1191 . 0.940 no
O2 . C201 . 1.4325(18) yes
O2 . H21 . 0.848 no
C201 . C202 . 1.528(2) yes
C201 . C208 . 1.535(3) yes
C201 . C214 . 1.517(3) yes
C201 . C202 . 1.528(2) yes
C201 . C214 . 1.517(3) yes
C201 . C408 . 1.570(5) yes
C201 . C202 . 1.528(2) yes
C201 . C208 . 1.535(3) yes
C201 . C414 . 1.560(4) yes
C201 . C202 . 1.528(2) yes
C201 . C408 . 1.570(5) yes
C201 . C414 . 1.560(4) yes
C202 . C203 . 1.396(2) yes
C202 . C207 . 1.390(2) yes
C203 . C204 . 1.378(3) yes
C203 . H2031 . 0.930 no
C204 . C205 . 1.373(3) yes
C204 . H2041 . 0.931 no
C205 . C206 . 1.381(3) yes
C205 . H2051 . 0.951 no
C206 . C207 . 1.381(3) yes
C206 . H2061 . 0.968 no
C207 . H2071 . 0.944 no
C208 . C209 . 1.409(3) yes
C208 . C213 . 1.374(3) yes
C209 . C210 . 1.383(3) yes
C209 . H2091 . 0.954 no
C210 . C211 . 1.374(3) yes
C210 . H2101 . 0.964 no
C211 . C212 . 1.379(3) yes
C211 . H2111 . 0.954 no
C212 . C213 . 1.386(3) yes
C212 . H2121 . 0.945 no
C213 . H2131 . 0.951 no
C214 . C215 . 1.393(4) yes
C214 . C219 . 1.362(4) yes
C215 . C216 . 1.391(4) yes
C215 . H2151 . 0.938 no
C216 . C217 . 1.364(4) yes
C216 . H2161 . 0.954 no
C217 . C218 . 1.363(4) yes
C217 . H2171 . 0.945 no
C218 . C219 . 1.402(4) yes
C218 . H2181 . 0.940 no
C219 . H2191 . 0.945 no
C308 . C309 . 1.367(5) yes
C308 . C313 . 1.399(5) yes
C309 . C310 . 1.395(5) yes
C309 . H3091 . 0.941 no
C310 . C311 . 1.372(5) yes
C310 . H3101 . 0.937 no
C311 . C312 . 1.362(5) yes
C311 . H3111 . 0.945 no
C312 . C313 . 1.389(5) yes
C312 . H3121 . 0.942 no
C313 . H3131 . 0.934 no
C314 . C315 . 1.396(5) yes
C314 . C319 . 1.382(5) yes
C315 . C316 . 1.393(5) yes
C315 . H3151 . 0.932 no
C316 . C317 . 1.371(5) yes
C316 . H3161 . 0.934 no
C317 . C318 . 1.378(5) yes
C317 . H3171 . 0.944 no
C318 . C319 . 1.397(5) yes
C318 . H3181 . 0.943 no
C319 . H3191 . 0.942 no
C408 . C409 . 1.408(5) yes
C408 . C413 . 1.370(6) yes
C409 . C410 . 1.395(5) yes
C409 . H4091 . 0.939 no
C410 . C411 . 1.367(6) yes
C410 . H4101 . 0.936 no
C411 . C412 . 1.386(6) yes
C411 . H4111 . 0.937 no
C412 . C413 . 1.401(6) yes
C412 . H4121 . 0.938 no
C413 . H4131 . 0.938 no
C414 . C415 . 1.371(5) yes
C414 . C419 . 1.427(4) yes
C415 . C416 . 1.404(5) yes
C415 . H4151 . 0.916 no
C416 . C417 . 1.387(4) yes
C416 . H4161 . 0.931 no
C417 . C418 . 1.376(4) yes
C417 . H4171 . 0.948 no
C418 . C419 . 1.393(4) yes
C418 . H4181 . 0.939 no
C419 . H4191 . 0.953 no
N501 . C502 . 1.5199(18) yes
N501 . C506 . 1.531(6) yes
N501 . C510 . 1.587(6) yes
N501 . C514 . 1.512(2) yes
N501 . C502 . 1.5199(18) yes
N501 . C510 . 1.587(6) yes
N501 . C514 . 1.512(2) yes
N501 . C606 . 1.507(7) yes
N501 . C502 . 1.5199(18) yes
N501 . C506 . 1.531(6) yes
N501 . C514 . 1.512(2) yes
N501 . C610 . 1.456(6) yes
N501 . C502 . 1.5199(18) yes
N501 . C514 . 1.512(2) yes
N501 . C606 . 1.507(7) yes
N501 . C610 . 1.456(6) yes
C502 . C503 . 1.510(2) yes
C502 . H5022 . 0.987 no
C502 . H5021 . 0.971 no
C503 . C504 . 1.512(2) yes
C503 . H5031 . 0.981 no
C503 . H5032 . 0.988 no
C504 . C505 . 1.510(2) yes
C504 . H5042 . 0.969 no
C504 . H5041 . 0.968 no
C505 . H5053 . 0.996 no
C505 . H5052 . 0.970 no
C505 . H5051 . 0.994 no
C506 . C507 . 1.527(6) yes
C506 . H5061 . 0.991 no
C506 . H5062 . 0.971 no
C507 . C508 . 1.527(6) yes
C507 . H5071 . 0.972 no
C507 . H5072 . 0.972 no
C508 . C509 . 1.510(6) yes
C508 . H5082 . 0.989 no
C508 . H5081 . 0.970 no
C509 . H5093 . 0.977 no
C509 . H5092 . 0.969 no
C509 . H5091 . 0.996 no
C510 . C511 . 1.557(6) yes
C510 . H5101 . 0.990 no
C510 . H5102 . 0.962 no
C511 . C512 . 1.574(6) yes
C511 . H5112 . 0.961 no
C511 . H5111 . 0.979 no
C512 . C513 . 1.461(6) yes
C512 . H5122 . 1.012 no
C512 . H5121 . 0.971 no
C513 . H5131 . 0.988 no
C513 . H5132 . 0.975 no
C513 . H5133 . 0.981 no
C514 . C515 . 1.506(3) yes
C514 . H5142 . 0.967 no
C514 . H5141 . 0.972 no
C515 . C516 . 1.454(4) yes
C515 . H5151 . 0.965 no
C515 . H5152 . 0.974 no
C515 . C617 . 1.603(4) yes
C515 . H5153 . 0.974 no
C515 . H5154 . 0.974 no
C516 . C517 . 1.350(6) yes
C516 . H5161 . 0.985 no
C516 . H5162 . 1.045 no
C517 . H5172 . 0.964 no
C517 . H5171 . 0.955 no
C517 . H5173 . 0.955 no
C606 . C607 . 1.508(8) yes
C606 . H6062 . 0.980 no
C606 . H6061 . 0.975 no
C607 . C608 . 1.514(7) yes
C607 . H6071 . 0.964 no
C607 . H6072 . 0.983 no
C608 . C609 . 1.491(7) yes
C608 . H6082 . 1.001 no
C608 . H6081 . 0.982 no
C609 . H6091 . 0.990 no
C609 . H6092 . 0.965 no
C609 . H6093 . 0.973 no
C610 . C611 . 1.482(6) yes
C610 . H6102 . 0.991 no
C610 . H6101 . 0.965 no
C611 . C612 . 1.491(6) yes
C611 . H6112 . 0.960 no
C611 . H6111 . 0.965 no
C612 . C613 . 1.482(5) yes
C612 . H6121 . 0.974 no
C612 . H6122 . 0.962 no
C613 . H6133 . 0.987 no
C613 . H6132 . 0.980 no
C613 . H6131 . 0.975 no
C617 . C618 . 1.495(5) yes
C617 . H6172 . 1.006 no
C617 . H6171 . 0.958 no
C618 . H6181 . 0.954 no
C618 . H6182 . 0.967 no
C618 . H6183 . 0.962 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C101 . O1 . H11 . 110.9 no
O1 . C101 . C102 . 110.56(11) yes
O1 . C101 . C108 . 104.4(3) yes
C102 . C101 . C108 . 105.1(3) yes
O1 . C101 . C114 . 114.7(2) yes
C102 . C101 . C114 . 107.0(3) yes
C108 . C101 . C114 . 114.7(4) yes
O1 . C101 . C102 . 110.56(11) yes
O1 . C101 . C114 . 114.7(2) yes
C102 . C101 . C114 . 107.0(3) yes
O1 . C101 . C308 . 103.0(4) yes
C102 . C101 . C308 . 113.1(5) yes
C114 . C101 . C308 . 108.5(5) yes
O1 . C101 . C102 . 110.56(11) yes
O1 . C101 . C108 . 104.4(3) yes
C102 . C101 . C108 . 105.1(3) yes
O1 . C101 . C314 . 106.0(3) yes
C102 . C101 . C314 . 114.6(5) yes
C108 . C101 . C314 . 115.8(6) yes
O1 . C101 . C102 . 110.56(11) yes
O1 . C101 . C308 . 103.0(4) yes
C102 . C101 . C308 . 113.1(5) yes
O1 . C101 . C314 . 106.0(3) yes
C102 . C101 . C314 . 114.6(5) yes
C308 . C101 . C314 . 108.7(7) yes
C101 . C102 . C103 . 120.40(13) yes
C101 . C102 . C107 . 121.56(14) yes
C103 . C102 . C107 . 118.03(15) yes
C102 . C103 . C104 . 120.46(15) yes
C102 . C103 . H1031 . 119.2 no
C104 . C103 . H1031 . 120.3 no
C103 . C104 . C105 . 120.48(18) yes
C103 . C104 . H1041 . 119.1 no
C105 . C104 . H1041 . 120.5 no
C104 . C105 . C106 . 119.41(17) yes
C104 . C105 . H1051 . 120.3 no
C106 . C105 . H1051 . 120.2 no
C105 . C106 . C107 . 120.45(17) yes
C105 . C106 . H1061 . 119.4 no
C107 . C106 . H1061 . 120.1 no
C102 . C107 . C106 . 121.16(18) yes
C102 . C107 . H1071 . 119.6 no
C106 . C107 . H1071 . 119.2 no
C101 . C108 . C109 . 120.54(7) yes
C101 . C108 . C113 . 120.92(7) yes
C109 . C108 . C113 . 118.29(6) yes
C108 . C109 . C110 . 120.73(7) yes
C108 . C109 . H1091 . 119.1 no
C110 . C109 . H1091 . 120.2 no
C109 . C110 . C111 . 120.43(7) yes
C109 . C110 . H1101 . 119.1 no
C111 . C110 . H1101 . 120.5 no
C110 . C111 . C112 . 119.66(7) yes
C110 . C111 . H1111 . 119.7 no
C112 . C111 . H1111 . 120.6 no
C111 . C112 . C113 . 120.31(7) yes
C111 . C112 . H1121 . 119.4 no
C113 . C112 . H1121 . 120.3 no
C108 . C113 . C112 . 120.53(7) yes
C108 . C113 . H1131 . 121.2 no
C112 . C113 . H1131 . 118.3 no
C101 . C114 . C115 . 120.80(7) yes
C101 . C114 . C119 . 120.72(6) yes
C115 . C114 . C119 . 118.36(6) yes
C114 . C115 . C116 . 120.58(7) yes
C114 . C115 . H1151 . 120.2 no
C116 . C115 . H1151 . 119.2 no
C115 . C116 . C117 . 120.36(7) yes
C115 . C116 . H1161 . 118.9 no
C117 . C116 . H1161 . 120.7 no
C116 . C117 . C118 . 119.66(7) yes
C116 . C117 . H1171 . 120.0 no
C118 . C117 . H1171 . 120.4 no
C117 . C118 . C119 . 120.38(7) yes
C117 . C118 . H1181 . 120.1 no
C119 . C118 . H1181 . 119.5 no
C118 . C119 . C114 . 120.65(7) yes
C118 . C119 . H1191 . 121.1 no
C114 . C119 . H1191 . 118.2 no
C201 . O2 . H21 . 111.9 no
O2 . C201 . C202 . 110.42(11) yes
O2 . C201 . C208 . 106.28(14) yes
C202 . C201 . C208 . 108.08(16) yes
O2 . C201 . C214 . 108.75(17) yes
C202 . C201 . C214 . 115.4(3) yes
C208 . C201 . C214 . 107.4(4) yes
O2 . C201 . C202 . 110.42(11) yes
O2 . C201 . C214 . 108.75(17) yes
C202 . C201 . C214 . 115.4(3) yes
O2 . C201 . C408 . 95.9(5) yes
C202 . C201 . C408 . 114.9(5) yes
C214 . C201 . C408 . 109.7(4) yes
O2 . C201 . C202 . 110.42(11) yes
O2 . C201 . C208 . 106.28(14) yes
C202 . C201 . C208 . 108.08(16) yes
O2 . C201 . C414 . 112.6(2) yes
C202 . C201 . C414 . 106.3(2) yes
C208 . C201 . C414 . 113.1(4) yes
O2 . C201 . C202 . 110.42(11) yes
O2 . C201 . C408 . 95.9(5) yes
C202 . C201 . C408 . 114.9(5) yes
O2 . C201 . C414 . 112.6(2) yes
C202 . C201 . C414 . 106.3(2) yes
C408 . C201 . C414 . 116.6(4) yes
C201 . C202 . C203 . 123.34(15) yes
C201 . C202 . C207 . 119.32(14) yes
C203 . C202 . C207 . 117.31(17) yes
C202 . C203 . C204 . 121.37(17) yes
C202 . C203 . H2031 . 117.7 no
C204 . C203 . H2031 . 120.9 no
C203 . C204 . C205 . 120.56(18) yes
C203 . C204 . H2041 . 119.8 no
C205 . C204 . H2041 . 119.6 no
C204 . C205 . C206 . 119.0(2) yes
C204 . C205 . H2051 . 119.4 no
C206 . C205 . H2051 . 121.6 no
C205 . C206 . C207 . 120.67(18) yes
C205 . C206 . H2061 . 119.5 no
C207 . C206 . H2061 . 119.9 no
C202 . C207 . C206 . 121.08(17) yes
C202 . C207 . H2071 . 118.9 no
C206 . C207 . H2071 . 120.0 no
C201 . C208 . C209 . 121.08(6) yes
C201 . C208 . C213 . 120.40(6) yes
C209 . C208 . C213 . 118.33(6) yes
C208 . C209 . C210 . 120.36(6) yes
C208 . C209 . H2091 . 121.1 no
C210 . C209 . H2091 . 118.4 no
C209 . C210 . C211 . 120.28(6) yes
C209 . C210 . H2101 . 120.5 no
C211 . C210 . H2101 . 119.2 no
C210 . C211 . C212 . 119.68(6) yes
C210 . C211 . H2111 . 121.1 no
C212 . C211 . H2111 . 119.2 no
C211 . C212 . C213 . 120.45(7) yes
C211 . C212 . H2121 . 121.8 no
C213 . C212 . H2121 . 117.7 no
C212 . C213 . C208 . 120.80(6) yes
C212 . C213 . H2131 . 122.6 no
C208 . C213 . H2131 . 116.6 no
C201 . C214 . C215 . 120.83(6) yes
C201 . C214 . C219 . 120.73(6) yes
C215 . C214 . C219 . 118.36(6) yes
C214 . C215 . C216 . 120.52(7) yes
C214 . C215 . H2151 . 118.9 no
C216 . C215 . H2151 . 120.6 no
C215 . C216 . C217 . 120.27(7) yes
C215 . C216 . H2161 . 120.5 no
C217 . C216 . H2161 . 119.2 no
C216 . C217 . C218 . 119.59(7) yes
C216 . C217 . H2171 . 121.0 no
C218 . C217 . H2171 . 119.4 no
C217 . C218 . C219 . 120.40(7) yes
C217 . C218 . H2181 . 120.8 no
C219 . C218 . H2181 . 118.8 no
C218 . C219 . C214 . 120.70(7) yes
C218 . C219 . H2191 . 120.9 no
C214 . C219 . H2191 . 118.4 no
C101 . C308 . C309 . 120.70(6) yes
C101 . C308 . C313 . 120.97(6) yes
C309 . C308 . C313 . 118.32(6) yes
C308 . C309 . C310 . 120.61(7) yes
C308 . C309 . H3091 . 118.2 no
C310 . C309 . H3091 . 121.2 no
C309 . C310 . C311 . 120.37(7) yes
C309 . C310 . H3101 . 119.3 no
C311 . C310 . H3101 . 120.4 no
C310 . C311 . C312 . 119.66(7) yes
C310 . C311 . H3111 . 119.4 no
C312 . C311 . H3111 . 120.9 no
C311 . C312 . C313 . 120.32(7) yes
C311 . C312 . H3121 . 119.4 no
C313 . C312 . H3121 . 120.3 no
C308 . C313 . C312 . 120.50(7) yes
C308 . C313 . H3131 . 120.9 no
C312 . C313 . H3131 . 118.6 no
C101 . C314 . C315 . 120.83(6) yes
C101 . C314 . C319 . 120.80(6) yes
C315 . C314 . C319 . 118.36(6) yes
C314 . C315 . C316 . 120.59(7) yes
C314 . C315 . H3151 . 119.0 no
C316 . C315 . H3151 . 120.4 no
C315 . C316 . C317 . 120.34(7) yes
C315 . C316 . H3161 . 120.5 no
C317 . C316 . H3161 . 119.1 no
C316 . C317 . C318 . 119.65(7) yes
C316 . C317 . H3171 . 120.1 no
C318 . C317 . H3171 . 120.2 no
C317 . C318 . C319 . 120.36(7) yes
C317 . C318 . H3181 . 119.9 no
C319 . C318 . H3181 . 119.7 no
C318 . C319 . C314 . 120.60(7) yes
C318 . C319 . H3191 . 120.1 no
C314 . C319 . H3191 . 119.3 no
C201 . C408 . C409 . 120.90(7) yes
C201 . C408 . C413 . 120.72(7) yes
C409 . C408 . C413 . 118.30(6) yes
C408 . C409 . C410 . 120.49(7) yes
C408 . C409 . H4091 . 120.4 no
C410 . C409 . H4091 . 119.1 no
C409 . C410 . C411 . 120.26(7) yes
C409 . C410 . H4101 . 119.7 no
C411 . C410 . H4101 . 120.1 no
C410 . C411 . C412 . 119.60(7) yes
C410 . C411 . H4111 . 120.2 no
C412 . C411 . H4111 . 120.2 no
C411 . C412 . C413 . 120.34(7) yes
C411 . C412 . H4121 . 120.3 no
C413 . C412 . H4121 . 119.4 no
C412 . C413 . C408 . 120.59(7) yes
C412 . C413 . H4131 . 120.4 no
C408 . C413 . H4131 . 119.0 no
C201 . C414 . C415 . 120.65(7) yes
C201 . C414 . C419 . 120.90(7) yes
C415 . C414 . C419 . 118.27(6) yes
C414 . C415 . C416 . 120.69(7) yes
C414 . C415 . H4151 . 117.1 no
C416 . C415 . H4151 . 122.2 no
C415 . C416 . C417 . 120.46(7) yes
C415 . C416 . H4161 . 118.8 no
C417 . C416 . H4161 . 120.8 no
C416 . C417 . C418 . 119.68(7) yes
C416 . C417 . H4171 . 119.0 no
C418 . C417 . H4171 . 121.4 no
C417 . C418 . C419 . 120.23(7) yes
C417 . C418 . H4181 . 118.9 no
C419 . C418 . H4181 . 120.8 no
C414 . C419 . C418 . 120.41(7) yes
C414 . C419 . H4191 . 120.8 no
C418 . C419 . H4191 . 118.8 no
C502 . N501 . C506 . 103.62(19) yes
C502 . N501 . C510 . 108.2(5) yes
C506 . N501 . C510 . 110.0(8) yes
C502 . N501 . C514 . 111.00(12) yes
C506 . N501 . C514 . 112.7(7) yes
C510 . N501 . C514 . 111.0(2) yes
C502 . N501 . C510 . 108.2(5) yes
C502 . N501 . C514 . 111.00(12) yes
C510 . N501 . C514 . 111.0(2) yes
C502 . N501 . C606 . 108.2(2) yes
C510 . N501 . C606 . 108.7(10) yes
C514 . N501 . C606 . 109.6(8) yes
C502 . N501 . C506 . 103.62(19) yes
C502 . N501 . C514 . 111.00(12) yes
C506 . N501 . C514 . 112.7(7) yes
C502 . N501 . C610 . 113.7(4) yes
C506 . N501 . C610 . 114.8(7) yes
C514 . N501 . C610 . 101.39(19) yes
C502 . N501 . C514 . 111.00(12) yes
C502 . N501 . C606 . 108.2(2) yes
C514 . N501 . C606 . 109.6(8) yes
C502 . N501 . C610 . 113.7(4) yes
C514 . N501 . C610 . 101.39(19) yes
C606 . N501 . C610 . 112.8(9) yes
N501 . C502 . C503 . 115.97(8) yes
N501 . C502 . H5022 . 106.5 no
C503 . C502 . H5022 . 109.9 no
N501 . C502 . H5021 . 106.5 no
C503 . C502 . H5021 . 109.1 no
H5022 . C502 . H5021 . 108.6 no
C502 . C503 . C504 . 109.54(7) yes
C502 . C503 . H5031 . 110.5 no
C504 . C503 . H5031 . 110.8 no
C502 . C503 . H5032 . 109.8 no
C504 . C503 . H5032 . 107.6 no
H5031 . C503 . H5032 . 108.5 no
C503 . C504 . C505 . 112.59(9) yes
C503 . C504 . H5042 . 109.6 no
C505 . C504 . H5042 . 110.1 no
C503 . C504 . H5041 . 110.4 no
C505 . C504 . H5041 . 110.1 no
H5042 . C504 . H5041 . 103.7 no
C504 . C505 . H5053 . 109.8 no
C504 . C505 . H5052 . 110.2 no
H5053 . C505 . H5052 . 107.6 no
C504 . C505 . H5051 . 110.7 no
H5053 . C505 . H5051 . 110.0 no
H5052 . C505 . H5051 . 108.5 no
N501 . C506 . C507 . 116.10(10) yes
N501 . C506 . H5061 . 105.3 no
C507 . C506 . H5061 . 110.5 no
N501 . C506 . H5062 . 106.1 no
C507 . C506 . H5062 . 109.2 no
H5061 . C506 . H5062 . 109.4 no
C506 . C507 . C508 . 109.22(10) yes
C506 . C507 . H5071 . 110.3 no
C508 . C507 . H5071 . 108.9 no
C506 . C507 . H5072 . 109.5 no
C508 . C507 . H5072 . 110.1 no
H5071 . C507 . H5072 . 108.8 no
C507 . C508 . C509 . 113.12(10) yes
C507 . C508 . H5082 . 110.2 no
C509 . C508 . H5082 . 104.4 no
C507 . C508 . H5081 . 109.5 no
C509 . C508 . H5081 . 111.2 no
H5082 . C508 . H5081 . 108.3 no
C508 . C509 . H5093 . 110.4 no
C508 . C509 . H5092 . 109.8 no
H5093 . C509 . H5092 . 107.5 no
C508 . C509 . H5091 . 111.0 no
H5093 . C509 . H5091 . 107.8 no
H5092 . C509 . H5091 . 110.2 no
N501 . C510 . C511 . 116.30(10) yes
N501 . C510 . H5101 . 106.1 no
C511 . C510 . H5101 . 109.2 no
N501 . C510 . H5102 . 105.8 no
C511 . C510 . H5102 . 107.5 no
H5101 . C510 . H5102 . 112.0 no
C510 . C511 . C512 . 109.06(10) yes
C510 . C511 . H5112 . 110.1 no
C512 . C511 . H5112 . 109.7 no
C510 . C511 . H5111 . 109.4 no
C512 . C511 . H5111 . 111.0 no
H5112 . C511 . H5111 . 107.5 no
C511 . C512 . C513 . 113.42(10) yes
C511 . C512 . H5122 . 119.1 no
C513 . C512 . H5122 . 106.6 no
C511 . C512 . H5121 . 104.2 no
C513 . C512 . H5121 . 107.1 no
H5122 . C512 . H5121 . 105.6 no
C512 . C513 . H5131 . 110.3 no
C512 . C513 . H5132 . 110.2 no
H5131 . C513 . H5132 . 109.4 no
C512 . C513 . H5133 . 107.6 no
H5131 . C513 . H5133 . 110.2 no
H5132 . C513 . H5133 . 109.0 no
N501 . C514 . C515 . 116.03(6) yes
N501 . C514 . H5142 . 106.4 no
C515 . C514 . H5142 . 110.4 no
N501 . C514 . H5141 . 106.3 no
C515 . C514 . H5141 . 108.9 no
H5142 . C514 . H5141 . 108.5 no
C514 . C515 . C516 . 108.11(9) yes
C514 . C515 . H5151 . 110.7 no
C516 . C515 . H5151 . 109.6 no
C514 . C515 . H5152 . 107.4 no
C516 . C515 . H5152 . 112.3 no
H5151 . C515 . H5152 . 108.8 no
C514 . C515 . C617 . 110.21(10) yes
C514 . C515 . H5153 . 110.6 no
C617 . C515 . H5153 . 110.3 no
C514 . C515 . H5154 . 108.9 no
C617 . C515 . H5154 . 108.6 no
H5153 . C515 . H5154 . 108.1 no
C515 . C516 . C517 . 113.44(10) yes
C515 . C516 . H5161 . 107.4 no
C517 . C516 . H5161 . 111.6 no
C515 . C516 . H5162 . 105.4 no
C517 . C516 . H5162 . 109.7 no
H5161 . C516 . H5162 . 109.0 no
C516 . C517 . H5172 . 107.6 no
C516 . C517 . H5171 . 107.7 no
H5172 . C517 . H5171 . 112.9 no
C516 . C517 . H5173 . 104.9 no
H5172 . C517 . H5173 . 110.7 no
H5171 . C517 . H5173 . 112.5 no
N501 . C606 . C607 . 116.09(10) yes
N501 . C606 . H6062 . 105.3 no
C607 . C606 . H6062 . 110.0 no
N501 . C606 . H6061 . 106.2 no
C607 . C606 . H6061 . 109.2 no
H6062 . C606 . H6061 . 109.7 no
C606 . C607 . C608 . 109.18(10) yes
C606 . C607 . H6071 . 110.9 no
C608 . C607 . H6071 . 109.9 no
C606 . C607 . H6072 . 110.3 no
C608 . C607 . H6072 . 108.7 no
H6071 . C607 . H6072 . 107.8 no
C607 . C608 . C609 . 113.15(10) yes
C607 . C608 . H6082 . 109.7 no
C609 . C608 . H6082 . 106.6 no
C607 . C608 . H6081 . 107.3 no
C609 . C608 . H6081 . 109.8 no
H6082 . C608 . H6081 . 110.3 no
C608 . C609 . H6091 . 110.8 no
C608 . C609 . H6092 . 109.6 no
H6091 . C609 . H6092 . 110.4 no
C608 . C609 . H6093 . 108.6 no
H6091 . C609 . H6093 . 108.8 no
H6092 . C609 . H6093 . 108.5 no
N501 . C610 . C611 . 115.88(10) yes
N501 . C610 . H6102 . 105.9 no
C611 . C610 . H6102 . 110.5 no
N501 . C610 . H6101 . 106.0 no
C611 . C610 . H6101 . 109.6 no
H6102 . C610 . H6101 . 108.8 no
C610 . C611 . C612 . 109.36(10) yes
C610 . C611 . H6112 . 110.5 no
C612 . C611 . H6112 . 111.4 no
C610 . C611 . H6111 . 107.8 no
C612 . C611 . H6111 . 109.3 no
H6112 . C611 . H6111 . 108.5 no
C611 . C612 . C613 . 113.01(10) yes
C611 . C612 . H6121 . 111.4 no
C613 . C612 . H6121 . 103.5 no
C611 . C612 . H6122 . 111.4 no
C613 . C612 . H6122 . 107.3 no
H6121 . C612 . H6122 . 109.8 no
C612 . C613 . H6133 . 108.1 no
C612 . C613 . H6132 . 108.8 no
H6133 . C613 . H6132 . 108.9 no
C612 . C613 . H6131 . 107.9 no
H6133 . C613 . H6131 . 110.3 no
H6132 . C613 . H6131 . 112.7 no
C515 . C617 . C618 . 113.42(10) yes
C515 . C617 . H6172 . 110.8 no
C618 . C617 . H6172 . 112.9 no
C515 . C617 . H6171 . 108.3 no
C618 . C617 . H6171 . 98.9 no
H6172 . C617 . H6171 . 112.0 no
C617 . C618 . H6181 . 110.0 no
C617 . C618 . H6182 . 107.4 no
H6181 . C618 . H6182 . 108.6 no
C617 . C618 . H6183 . 111.3 no
H6181 . C618 . H6183 . 110.5 no
H6182 . C618 . H6183 . 108.9 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C115 . H1151 . C107 . 125.94 0.943 2.467 3.115(10) yes
C209 . H2091 . C219 . 127.02 0.954 2.395 3.066(10) yes
C317 . H3171 . C211 3_565 166.1 0.944 2.566 3.490(10) yes
C510 . H5102 . O1 4_646 143.8 0.962 2.475 3.300(10) yes
C610 . H5102 . O1 4_646 132.9 0.945 2.475 3.194(10) yes
C516 . H5161 . C417 . 153.37 0.985 2.471 3.381(10) yes
C510 . H6101 . O1 4_646 145.7 1.100 2.332 3.300(10) yes
C610 . H6101 . O1 4_646 148.2 0.965 2.332 3.194(10) yes
C618 . H6182 . C318 4_646 139.9 0.967 2.415 3.215(10) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 25/04/13 at 18:39:32
#
#LIST     12                                                                    
BLOCK SCALE X'S U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIV PART(2001,OCC) PART(2002,OCC) 
WEIGHT -1 PART(2002,OCC) 
EQUIV PART(3001,OCC) PART(3002,OCC) 
WEIGHT -1 PART(3002,OCC) 
EQUIV PART(4001,OCC) PART(4002,OCC) 
WEIGHT -1 PART(4002,OCC) 
EQUIV PART(5001,OCC) PART(5002,OCC) 
WEIGHT -1 PART(5002,OCC) 
EQUIV PART(6001,OCC) PART(6002,OCC) 
WEIGHT -1 PART(6002,OCC) 
EQUIV PART(7001,OCC) PART(7002,OCC) 
WEIGHT -1 PART(7002,OCC) 
RIDE O   (   1,X'S) H   (  11,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 107,X'S) H   (1071,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) 
RIDE C   ( 117,X'S) H   (1171,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 119,X'S) H   (1191,X'S) 
RIDE O   (   2,X'S) H   (  21,X'S) 
RIDE C   ( 203,X'S) H   (2031,X'S) 
RIDE C   ( 204,X'S) H   (2041,X'S) 
RIDE C   ( 205,X'S) H   (2051,X'S) 
RIDE C   ( 206,X'S) H   (2061,X'S) 
RIDE C   ( 207,X'S) H   (2071,X'S) 
RIDE C   ( 209,X'S) H   (2091,X'S) 
RIDE C   ( 210,X'S) H   (2101,X'S) 
RIDE C   ( 211,X'S) H   (2111,X'S) 
RIDE C   ( 212,X'S) H   (2121,X'S) 
RIDE C   ( 213,X'S) H   (2131,X'S) 
RIDE C   ( 215,X'S) H   (2151,X'S) 
RIDE C   ( 216,X'S) H   (2161,X'S) 
RIDE C   ( 217,X'S) H   (2171,X'S) 
RIDE C   ( 218,X'S) H   (2181,X'S) 
RIDE C   ( 219,X'S) H   (2191,X'S) 
RIDE C   ( 309,X'S) H   (3091,X'S) 
RIDE C   ( 310,X'S) H   (3101,X'S) 
RIDE C   ( 311,X'S) H   (3111,X'S) 
RIDE C   ( 312,X'S) H   (3121,X'S) 
RIDE C   ( 313,X'S) H   (3131,X'S) 
RIDE C   ( 315,X'S) H   (3151,X'S) 
RIDE C   ( 316,X'S) H   (3161,X'S) 
RIDE C   ( 317,X'S) H   (3171,X'S) 
RIDE C   ( 318,X'S) H   (3181,X'S) 
RIDE C   ( 319,X'S) H   (3191,X'S) 
RIDE C   ( 409,X'S) H   (4091,X'S) 
RIDE C   ( 410,X'S) H   (4101,X'S) 
RIDE C   ( 411,X'S) H   (4111,X'S) 
RIDE C   ( 412,X'S) H   (4121,X'S) 
RIDE C   ( 413,X'S) H   (4131,X'S) 
RIDE C   ( 415,X'S) H   (4151,X'S) 
RIDE C   ( 416,X'S) H   (4161,X'S) 
RIDE C   ( 417,X'S) H   (4171,X'S) 
RIDE C   ( 418,X'S) H   (4181,X'S) 
RIDE C   ( 419,X'S) H   (4191,X'S) 
RIDE C   ( 502,X'S) H   (5022,X'S) H   (5021,X'S) 
RIDE C   ( 503,X'S) H   (5031,X'S) H   (5032,X'S) 
RIDE C   ( 504,X'S) H   (5042,X'S) H   (5041,X'S) 
RIDE C   ( 505,X'S) H   (5053,X'S) H   (5052,X'S) H   (5051,X'S) 
RIDE C   ( 506,X'S) H   (5061,X'S) H   (5062,X'S) 
RIDE C   ( 507,X'S) H   (5071,X'S) H   (5072,X'S) 
RIDE C   ( 508,X'S) H   (5082,X'S) H   (5081,X'S) 
RIDE C   ( 509,X'S) H   (5093,X'S) H   (5092,X'S) H   (5091,X'S) 
RIDE C   ( 510,X'S) H   (5101,X'S) H   (5102,X'S) 
RIDE C   ( 511,X'S) H   (5112,X'S) H   (5111,X'S) 
RIDE C   ( 512,X'S) H   (5122,X'S) H   (5121,X'S) 
RIDE C   ( 513,X'S) H   (5131,X'S) H   (5132,X'S) H   (5133,X'S) 
RIDE C   ( 514,X'S) H   (5142,X'S) H   (5141,X'S) 
RIDE C   ( 515,X'S) H   (5151,X'S) H   (5152,X'S) 
CONT H   (5153,X'S) H   (5154,X'S) 
RIDE C   ( 516,X'S) H   (5161,X'S) H   (5162,X'S) 
RIDE C   ( 517,X'S) H   (5172,X'S) H   (5171,X'S) H   (5173,X'S) 
RIDE C   ( 606,X'S) H   (6062,X'S) H   (6061,X'S) 
RIDE C   ( 607,X'S) H   (6071,X'S) H   (6072,X'S) 
RIDE C   ( 608,X'S) H   (6082,X'S) H   (6081,X'S) 
RIDE C   ( 609,X'S) H   (6091,X'S) H   (6092,X'S) H   (6093,X'S) 
RIDE C   ( 610,X'S) H   (6102,X'S) H   (6101,X'S) 
RIDE C   ( 611,X'S) H   (6112,X'S) H   (6111,X'S) 
RIDE C   ( 612,X'S) H   (6121,X'S) H   (6122,X'S) 
RIDE C   ( 613,X'S) H   (6133,X'S) H   (6132,X'S) H   (6131,X'S) 
RIDE C   ( 617,X'S) H   (6172,X'S) H   (6171,X'S) 
RIDE C   ( 618,X'S) H   (6181,X'S) H   (6182,X'S) H   (6183,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 25/04/13 at 18:39:32
#
#LIST     16                                                                    
REM 
REM ALCOHOL 
REM 
SAME  C(101)  C(108)  C(109)  C(110)  C(111)  C(112)  C(113)  AND 
CONT  C(101)  C(108)  C(113)  C(112)  C(111)  C(110)  C(109)  AND 
CONT  C(101)  C(114)  C(115)  C(116)  C(117)  C(118)  C(119)  AND 
CONT  C(101)  C(114)  C(119)  C(118)  C(117)  C(116)  C(115)  AND 
CONT  C(201)  C(208)  C(209)  C(210)  C(211)  C(212)  C(213)  AND 
CONT  C(201)  C(208)  C(213)  C(212)  C(211)  C(210)  C(209)  AND 
CONT  C(201)  C(214)  C(215)  C(216)  C(217)  C(218)  C(219)  AND 
CONT  C(201)  C(214)  C(219)  C(218)  C(217)  C(216)  C(215)  AND 
CONT  C(101)  C(308)  C(309)  C(310)  C(311)  C(312)  C(313)  AND 
CONT  C(101)  C(308)  C(313)  C(312)  C(311)  C(310)  C(309)  AND 
CONT  C(101)  C(314)  C(315)  C(316)  C(317)  C(318)  C(319)  AND 
CONT  C(101)  C(314)  C(319)  C(318)  C(317)  C(316)  C(315)  AND 
CONT  C(201)  C(408)  C(409)  C(410)  C(411)  C(412)  C(413)  AND 
CONT  C(201)  C(408)  C(413)  C(412)  C(411)  C(410)  C(409)  AND 
CONT  C(201)  C(414)  C(415)  C(416)  C(417)  C(418)  C(419)  AND 
CONT  C(201)  C(414)  C(419)  C(418)  C(417)  C(416)  C(415) 
SIMU  0.01    C(101)  C(108)  C(109)  C(110)  C(111)  C(112)  C(113)  AND 
CONT  C(101)  C(108)  C(113)  C(112)  C(111)  C(110)  C(109)  AND 
CONT  C(101)  C(114)  C(115)  C(116)  C(117)  C(118)  C(119)  AND 
CONT  C(101)  C(114)  C(119)  C(118)  C(117)  C(116)  C(115)  AND 
CONT  C(201)  C(208)  C(209)  C(210)  C(211)  C(212)  C(213)  AND 
CONT  C(201)  C(208)  C(213)  C(212)  C(211)  C(210)  C(209)  AND 
CONT  C(201)  C(214)  C(215)  C(216)  C(217)  C(218)  C(219)  AND 
CONT  C(201)  C(214)  C(219)  C(218)  C(217)  C(216)  C(215)  AND 
CONT  C(101)  C(308)  C(309)  C(310)  C(311)  C(312)  C(313)  AND 
CONT  C(101)  C(308)  C(313)  C(312)  C(311)  C(310)  C(309)  AND 
CONT  C(101)  C(314)  C(315)  C(316)  C(317)  C(318)  C(319)  AND 
CONT  C(101)  C(314)  C(319)  C(318)  C(317)  C(316)  C(315)  AND 
CONT  C(201)  C(408)  C(409)  C(410)  C(411)  C(412)  C(413)  AND 
CONT  C(201)  C(408)  C(413)  C(412)  C(411)  C(410)  C(409)  AND 
CONT  C(201)  C(414)  C(415)  C(416)  C(417)  C(418)  C(419)  AND 
CONT  C(201)  C(414)  C(419)  C(418)  C(417)  C(416)  C(415) 
DELU  0.01    C(101)  C(108)  C(109)  C(110)  C(111)  C(112)  C(113)  AND 
CONT  C(101)  C(108)  C(113)  C(112)  C(111)  C(110)  C(109)  AND 
CONT  C(101)  C(114)  C(115)  C(116)  C(117)  C(118)  C(119)  AND 
CONT  C(101)  C(114)  C(119)  C(118)  C(117)  C(116)  C(115)  AND 
CONT  C(201)  C(208)  C(209)  C(210)  C(211)  C(212)  C(213)  AND 
CONT  C(201)  C(208)  C(213)  C(212)  C(211)  C(210)  C(209)  AND 
CONT  C(201)  C(214)  C(215)  C(216)  C(217)  C(218)  C(219)  AND 
CONT  C(201)  C(214)  C(219)  C(218)  C(217)  C(216)  C(215)  AND 
CONT  C(101)  C(308)  C(309)  C(310)  C(311)  C(312)  C(313)  AND 
CONT  C(101)  C(308)  C(313)  C(312)  C(311)  C(310)  C(309)  AND 
CONT  C(101)  C(314)  C(315)  C(316)  C(317)  C(318)  C(319)  AND 
CONT  C(101)  C(314)  C(319)  C(318)  C(317)  C(316)  C(315)  AND 
CONT  C(201)  C(408)  C(409)  C(410)  C(411)  C(412)  C(413)  AND 
CONT  C(201)  C(408)  C(413)  C(412)  C(411)  C(410)  C(409)  AND 
CONT  C(201)  C(414)  C(415)  C(416)  C(417)  C(418)  C(419)  AND 
CONT  C(201)  C(414)  C(419)  C(418)  C(417)  C(416)  C(415) 
REM 
REM TBA 
REM 
SAME  N(501)  C(502)  C(503)  C(504)  C(505)  AND 
CONT  N(501)  C(506)  C(507)  C(508)  C(509)  AND 
CONT  N(501)  C(510)  C(511)  C(512)  C(513)  AND 
CONT  N(501)  C(514)  C(515)  C(516)  C(517)  AND 
CONT  N(501)  C(606)  C(607)  C(608)  C(609)  AND 
CONT  N(501)  C(610)  C(611)  C(612)  C(613)  AND 
CONT  N(501)  C(514)  C(515)  C(617)  C(618) 
SIMU  0.005   N(501)  C(502)  C(503)  C(504)  C(505)  AND 
CONT  N(501)  C(506)  C(507)  C(508)  C(509)  AND 
CONT  N(501)  C(510)  C(511)  C(512)  C(513)  AND 
CONT  N(501)  C(514)  C(515)  C(516)  C(517)  AND 
CONT  N(501)  C(606)  C(607)  C(608)  C(609)  AND 
CONT  N(501)  C(610)  C(611)  C(612)  C(613)  AND 
CONT  N(501)  C(514)  C(515)  C(617)  C(618) 
DELU  0.005   N(501)  C(502)  C(503)  C(504)  C(505)  AND 
CONT  N(501)  C(506)  C(507)  C(508)  C(509)  AND 
CONT  N(501)  C(510)  C(511)  C(512)  C(513)  AND 
CONT  N(501)  C(514)  C(515)  C(516)  C(517)  AND 
CONT  N(501)  C(606)  C(607)  C(608)  C(609)  AND 
CONT  N(501)  C(610)  C(611)  C(612)  C(613)  AND 
CONT  N(501)  C(514)  C(515)  C(617)  C(618) 
END                                                                             
;
####################################################################### 
# 
# 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_2m
_database_code_depnum_ccdc_archive 'CCDC 1401777'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             13-04-25
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 048gwp12
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_refine_special_details          
; 
On completion of the model, it became apparent that there
was a small solvent accessible void.  Careful examination 
of the difference Fourier map showed no evidence of 
significant residual electron density.  PLATON/SQUEEZE was 
used to evaluate the magnitude of the void space and 
the associated electron density (see below).  However, 
refinement including the contributions to the A and B 
parts of the calculated structure factors determined by 
discrete Fourier transform of the electron density in the 
void region (using SQUEEZE) made minimal difference to the 
agreement factors and no perceptible change to the model 
so these were omitted for the final refinement.

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.500        32         1 ' '
   2  0.180  0.066  0.234        81         2 ' '
   3 -0.180  0.934  0.766        82         2 ' '
   4  0.160  0.357  0.342         8         0 ' '
   5  0.190  0.057  0.366         6         0 ' '
   6  0.451  0.724  0.255        33         1 ' '
   7  0.548  0.276  0.745        33         1 ' '
   8  0.810  0.943  0.634         5         0 ' '
   9  0.840  0.643  0.658         8         0 ' '
;


_cell_length_a                   13.4717(3)
_cell_length_b                   17.5643(4)
_cell_length_c                   24.8506(5)
_cell_angle_alpha                78.8655(19)
_cell_angle_beta                 80.5422(17)
_cell_angle_gamma                69.645(2)
_cell_volume                     5379.0(2)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C60 H80 F1 N1 O2 
# Dc =      1.07 Fooo =   1888.00 Mu =      5.00 M =   1732.60
# Found Formula = C60 H80 F1 N1 O2 
# Dc =      1.07 FOOO =   1888.00 Mu =      5.00 M =   1732.60

_chemical_formula_sum            'C60 H80 F1 N1 O2'
_chemical_formula_moiety         '2(C22 H22 O), C16 H36 N, F'
_chemical_compound_source        .
_chemical_formula_weight         866.30


_cell_measurement_reflns_used    46180
_cell_measurement_theta_min      3
_cell_measurement_theta_max      77
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.180
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.210

_exptl_crystal_density_diffrn    1.070
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1888
_exptl_absorpt_coefficient_mu    0.500

# Sheldrick geometric approximatio 0.90 0.91 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_T_max  0.91
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            110583
_reflns_number_total             22463
_diffrn_reflns_av_R_equivalents  0.033
# Number of reflections with Friedels Law is 22463 
# Theoretical number of reflections is about 45586 


_diffrn_reflns_theta_min         3.038
_diffrn_reflns_theta_max         77.166
_diffrn_measured_fraction_theta_max 0.986

_diffrn_reflns_theta_full        74.851
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_reflns_limit_h_min              -16
_reflns_limit_h_max              17
_reflns_limit_k_min              -21
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              31

_oxford_diffrn_Wilson_B_factor   3.11
_oxford_diffrn_Wilson_scale      0.08

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.21
_refine_diff_density_max         0.33


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         22370
_refine_ls_number_restraints     0
_refine_ls_number_parameters     1154
_oxford_refine_ls_R_factor_ref   0.0502
_refine_ls_wR_factor_ref         0.1203
_refine_ls_goodness_of_fit_ref   0.9911
_refine_ls_shift/su_max          0.0008843
_refine_ls_shift/su_mean         0.0001389


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        22373
_refine_ls_R_factor_all          0.0502
_refine_ls_wR_factor_all         0.1204

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                19453
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_gt          0.1141

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.06P)² + 1.56P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C91 C 0.03783(13) 0.59782(8) 0.51970(6) 0.0465 1.0000 Uani . . . . . .
C11 C 0.34783(9) 0.67176(7) 0.84329(4) 0.0289 1.0000 Uani . . . . . .
C12 C 0.22826(10) 0.68207(7) 0.84943(5) 0.0299 1.0000 Uani . . . . . .
C13 C 0.16170(10) 0.73928(8) 0.81269(5) 0.0353 1.0000 Uani . . . . . .
C14 C 0.05323(11) 0.74962(9) 0.81826(6) 0.0416 1.0000 Uani . . . . . .
C15 C 0.00784(11) 0.70327(9) 0.86007(6) 0.0432 1.0000 Uani . . . . . .
C16 C 0.07434(11) 0.64644(9) 0.89678(6) 0.0428 1.0000 Uani . . . . . .
C17 C 0.18239(10) 0.63581(8) 0.89172(5) 0.0360 1.0000 Uani . . . . . .
C18 C -0.10973(13) 0.71478(12) 0.86618(8) 0.0608 1.0000 Uani . . . . . .
C19 C 0.41380(9) 0.57990(7) 0.85390(5) 0.0314 1.0000 Uani . . . . . .
C20 C 0.45336(10) 0.53465(8) 0.81028(6) 0.0368 1.0000 Uani . . . . . .
C21 C 0.51105(11) 0.45139(8) 0.82029(7) 0.0452 1.0000 Uani . . . . . .
C22 C 0.53031(10) 0.41072(8) 0.87306(7) 0.0458 1.0000 Uani . . . . . .
C23 C 0.49131(11) 0.45607(8) 0.91630(6) 0.0435 1.0000 Uani . . . . . .
C24 C 0.43436(10) 0.53958(8) 0.90690(6) 0.0375 1.0000 Uani . . . . . .
C25 C 0.59102(13) 0.32011(9) 0.88310(10) 0.0651 1.0000 Uani . . . . . .
C26 C 0.37441(10) 0.71668(7) 0.88340(5) 0.0304 1.0000 Uani . . . . . .
C27 C 0.47830(11) 0.71902(8) 0.87763(5) 0.0362 1.0000 Uani . . . . . .
C28 C 0.50768(12) 0.76052(8) 0.91090(6) 0.0420 1.0000 Uani . . . . . .
C29 C 0.43556(13) 0.80012(9) 0.95165(6) 0.0451 1.0000 Uani . . . . . .
C30 C 0.33356(13) 0.79619(9) 0.95807(6) 0.0473 1.0000 Uani . . . . . .
C31 C 0.30246(11) 0.75551(8) 0.92416(5) 0.0395 1.0000 Uani . . . . . .
C32 C 0.46746(18) 0.84628(12) 0.98764(8) 0.0661 1.0000 Uani . . . . . .
C41 C 0.52119(9) 0.71831(7) 0.60481(5) 0.0304 1.0000 Uani . . . . . .
C42 C 0.45812(9) 0.71932(7) 0.55810(5) 0.0302 1.0000 Uani . . . . . .
C43 C 0.36209(10) 0.70350(8) 0.57052(6) 0.0382 1.0000 Uani . . . . . .
C44 C 0.30725(11) 0.70073(9) 0.52868(6) 0.0427 1.0000 Uani . . . . . .
C45 C 0.34603(11) 0.71282(7) 0.47343(6) 0.0378 1.0000 Uani . . . . . .
C46 C 0.44210(11) 0.72812(8) 0.46129(5) 0.0382 1.0000 Uani . . . . . .
C47 C 0.49710(10) 0.73196(8) 0.50266(5) 0.0350 1.0000 Uani . . . . . .
C48 C 0.28886(13) 0.70763(10) 0.42788(7) 0.0521 1.0000 Uani . . . . . .
C49 C 0.58817(9) 0.62931(7) 0.62422(5) 0.0306 1.0000 Uani . . . . . .
C50 C 0.60049(10) 0.60176(8) 0.67981(5) 0.0347 1.0000 Uani . . . . . .
C51 C 0.66022(10) 0.52115(8) 0.69737(5) 0.0376 1.0000 Uani . . . . . .
C52 C 0.71043(10) 0.46557(8) 0.66064(5) 0.0360 1.0000 Uani . . . . . .
C53 C 0.70002(12) 0.49392(8) 0.60506(6) 0.0421 1.0000 Uani . . . . . .
C54 C 0.63885(12) 0.57400(8) 0.58726(5) 0.0395 1.0000 Uani . . . . . .
C55 C 0.77009(12) 0.37741(9) 0.68107(7) 0.0472 1.0000 Uani . . . . . .
C56 C 0.59118(10) 0.77284(7) 0.58356(5) 0.0310 1.0000 Uani . . . . . .
C57 C 0.54124(11) 0.85719(8) 0.57504(6) 0.0399 1.0000 Uani . . . . . .
C58 C 0.59864(12) 0.91018(8) 0.55344(6) 0.0429 1.0000 Uani . . . . . .
C59 C 0.70799(11) 0.88087(8) 0.53971(5) 0.0379 1.0000 Uani . . . . . .
C60 C 0.75734(10) 0.79663(8) 0.54753(5) 0.0382 1.0000 Uani . . . . . .
C61 C 0.70030(10) 0.74318(8) 0.56935(5) 0.0357 1.0000 Uani . . . . . .
C62 C 0.77081(13) 0.93848(10) 0.51741(7) 0.0522 1.0000 Uani . . . . . .
C71 C 0.14929(9) 0.27551(7) 0.65868(4) 0.0278 1.0000 Uani . . . . . .
C72 C 0.08264(9) 0.22584(7) 0.64714(5) 0.0303 1.0000 Uani . . . . . .
C73 C 0.04644(10) 0.17482(8) 0.69016(6) 0.0380 1.0000 Uani . . . . . .
C74 C -0.01132(11) 0.12836(9) 0.67951(7) 0.0482 1.0000 Uani . . . . . .
C75 C -0.03417(11) 0.13024(9) 0.62689(8) 0.0498 1.0000 Uani . . . . . .
C76 C 0.00172(11) 0.18141(9) 0.58423(7) 0.0458 1.0000 Uani . . . . . .
C77 C 0.05891(10) 0.22855(8) 0.59424(6) 0.0368 1.0000 Uani . . . . . .
C78 C -0.09467(15) 0.07777(12) 0.61574(11) 0.0767 1.0000 Uani . . . . . .
C79 C 0.26836(9) 0.22437(7) 0.65235(5) 0.0286 1.0000 Uani . . . . . .
C80 C 0.33592(10) 0.22677(8) 0.68817(5) 0.0352 1.0000 Uani . . . . . .
C81 C 0.44400(11) 0.18101(9) 0.68287(6) 0.0420 1.0000 Uani . . . . . .
C82 C 0.48776(10) 0.13126(8) 0.64226(6) 0.0422 1.0000 Uani . . . . . .
C83 C 0.42040(10) 0.12931(8) 0.60620(6) 0.0402 1.0000 Uani . . . . . .
C84 C 0.31261(10) 0.17475(7) 0.61114(5) 0.0334 1.0000 Uani . . . . . .
C85 C 0.60529(12) 0.08204(11) 0.63613(8) 0.0608 1.0000 Uani . . . . . .
C86 C 0.12463(9) 0.35769(7) 0.61947(4) 0.0277 1.0000 Uani . . . . . .
C87 C 0.02339(10) 0.41506(7) 0.62743(5) 0.0318 1.0000 Uani . . . . . .
C88 C -0.00460(10) 0.49183(7) 0.59535(5) 0.0347 1.0000 Uani . . . . . .
C89 C 0.06792(11) 0.51396(7) 0.55413(5) 0.0349 1.0000 Uani . . . . . .
C90 C 0.16768(11) 0.45658(8) 0.54571(5) 0.0394 1.0000 Uani . . . . . .
C238 C 0.19643(10) 0.37917(7) 0.57799(5) 0.0350 1.0000 Uani . . . . . .
C101 C -0.01223(9) 0.27858(7) 0.89457(5) 0.0291 1.0000 Uani . . . . . .
C102 C 0.04948(9) 0.22036(7) 0.94166(5) 0.0301 1.0000 Uani . . . . . .
C103 C 0.14655(10) 0.16118(8) 0.92963(6) 0.0388 1.0000 Uani . . . . . .
C104 C 0.20360(11) 0.10934(9) 0.97177(6) 0.0451 1.0000 Uani . . . . . .
C105 C 0.16604(12) 0.11470(8) 1.02673(6) 0.0421 1.0000 Uani . . . . . .
C106 C 0.06742(12) 0.17175(8) 1.03866(5) 0.0418 1.0000 Uani . . . . . .
C107 C 0.01002(11) 0.22422(8) 0.99679(5) 0.0362 1.0000 Uani . . . . . .
C108 C 0.23118(17) 0.06159(10) 1.07220(8) 0.0630 1.0000 Uani . . . . . .
C109 C -0.07834(9) 0.23716(7) 0.87328(5) 0.0292 1.0000 Uani . . . . . .
C110 C -0.09583(10) 0.25448(7) 0.81790(5) 0.0326 1.0000 Uani . . . . . .
C111 C -0.15419(10) 0.21696(8) 0.79765(5) 0.0346 1.0000 Uani . . . . . .
C112 C -0.19756(10) 0.16130(8) 0.83180(6) 0.0358 1.0000 Uani . . . . . .
C113 C -0.18085(11) 0.14456(8) 0.88711(6) 0.0384 1.0000 Uani . . . . . .
C114 C -0.12172(10) 0.18127(8) 0.90751(5) 0.0345 1.0000 Uani . . . . . .
C115 C -0.26102(14) 0.12167(10) 0.80874(7) 0.0532 1.0000 Uani . . . . . .
C116 C -0.08167(9) 0.35902(7) 0.91566(5) 0.0297 1.0000 Uani . . . . . .
C117 C -0.03104(10) 0.41025(8) 0.92645(6) 0.0368 1.0000 Uani . . . . . .
C118 C -0.08824(11) 0.48211(8) 0.94800(6) 0.0384 1.0000 Uani . . . . . .
C119 C -0.19818(11) 0.50549(8) 0.95951(5) 0.0363 1.0000 Uani . . . . . .
C120 C -0.24848(11) 0.45442(9) 0.94886(6) 0.0422 1.0000 Uani . . . . . .
C121 C -0.19142(10) 0.38218(8) 0.92726(6) 0.0382 1.0000 Uani . . . . . .
C122 C -0.26056(13) 0.58408(9) 0.98219(7) 0.0505 1.0000 Uani . . . . . .
O1 O 0.37936(7) 0.70867(5) 0.79038(3) 0.0333 1.0000 Uani . . . . . .
O2 O 0.45136(7) 0.75422(5) 0.64912(4) 0.0357 1.0000 Uani . . . . . .
O3 O 0.11807(7) 0.29878(5) 0.71198(3) 0.0334 1.0000 Uani . . . . . .
O4 O 0.05955(7) 0.30119(5) 0.85101(3) 0.0328 1.0000 Uani . . . . . .
F1 F 0.33533(6) 0.67338(5) 0.70647(3) 0.0388 1.0000 Uani . . . . . .
F2 F 0.16882(6) 0.18923(4) 0.79331(3) 0.0383 1.0000 Uani . . . . . .
H41 H 0.0965 0.2595 0.8349 0.0512 1.0000 Uiso R . . . . .
H31 H 0.1362 0.2561 0.7372 0.0521 1.0000 Uiso R . . . . .
H11 H 0.3640 0.6905 0.7635 0.0521 1.0000 Uiso R . . . . .
H21 H 0.4114 0.7242 0.6654 0.0559 1.0000 Uiso R . . . . .
N201 N 0.33695(8) -0.04113(6) 0.76782(4) 0.0298 1.0000 Uani . . . . . .
C202 C 0.43463(10) -0.11765(7) 0.76764(5) 0.0331 1.0000 Uani . . . . . .
C203 C 0.53261(11) -0.10901(8) 0.73085(6) 0.0397 1.0000 Uani . . . . . .
C204 C 0.62333(12) -0.19013(10) 0.73690(7) 0.0507 1.0000 Uani . . . . . .
C205 C 0.72639(13) -0.18611(13) 0.70340(8) 0.0654 1.0000 Uani . . . . . .
C206 C 0.36077(10) 0.03019(7) 0.78247(5) 0.0324 1.0000 Uani . . . . . .
C207 C 0.40576(11) 0.01575(8) 0.83697(6) 0.0402 1.0000 Uani . . . . . .
C208 C 0.43767(13) 0.08928(9) 0.84106(7) 0.0479 1.0000 Uani . . . . . .
C209 C 0.48530(14) 0.08102(12) 0.89373(7) 0.0587 1.0000 Uani . . . . . .
C210 C 0.29834(10) -0.01204(7) 0.71102(5) 0.0329 1.0000 Uani . . . . . .
C211 C 0.26187(11) -0.07072(8) 0.68831(5) 0.0375 1.0000 Uani . . . . . .
C212 C 0.23208(10) -0.03449(8) 0.63002(5) 0.0373 1.0000 Uani . . . . . .
C213 C 0.18700(14) -0.08776(10) 0.60672(7) 0.0531 1.0000 Uani . . . . . .
C214 C 0.25274(10) -0.06445(7) 0.81007(5) 0.0346 1.0000 Uani . . . . . .
C215 C 0.14295(11) 0.00001(9) 0.81273(6) 0.0435 1.0000 Uani . . . . . .
C216 C 0.06756(12) -0.02967(10) 0.85836(7) 0.0526 1.0000 Uani . . . . . .
C217 C 0.08626(14) -0.02625(11) 0.91598(7) 0.0588 1.0000 Uani . . . . . .
N221 N 0.16323(8) 0.51952(6) 0.73344(4) 0.0330 1.0000 Uani . . . . . .
C222 C 0.06297(10) 0.49709(8) 0.73613(5) 0.0363 1.0000 Uani . . . . . .
C223 C -0.03160(11) 0.54199(8) 0.77347(6) 0.0390 1.0000 Uani . . . . . .
C224 C -0.12620(12) 0.51360(11) 0.77384(7) 0.0510 1.0000 Uani . . . . . .
C225 C -0.22525(13) 0.56337(12) 0.80653(7) 0.0562 1.0000 Uani . . . . . .
C226 C 0.14120(10) 0.61127(7) 0.71751(5) 0.0351 1.0000 Uani . . . . . .
C227 C 0.09193(12) 0.65011(8) 0.66395(6) 0.0423 1.0000 Uani . . . . . .
C228 C 0.06400(13) 0.74255(9) 0.65776(7) 0.0503 1.0000 Uani . . . . . .
C229 C 0.01023(15) 0.78796(11) 0.60666(8) 0.0580 1.0000 Uani . . . . . .
C230 C 0.20417(10) 0.49725(8) 0.78967(5) 0.0345 1.0000 Uani . . . . . .
C231 C 0.23796(11) 0.40700(8) 0.81312(6) 0.0399 1.0000 Uani . . . . . .
H1031 H 0.1741 0.1575 0.8916 0.0465 1.0000 Uiso R . . . . .
C232 C 0.26681(11) 0.39568(9) 0.87157(6) 0.0394 1.0000 Uani . . . . . .
C233 C 0.30821(14) 0.30587(10) 0.89584(7) 0.0539 1.0000 Uani . . . . . .
C234 C 0.24553(11) 0.47243(8) 0.69120(5) 0.0386 1.0000 Uani . . . . . .
C235 C 0.35653(12) 0.47822(10) 0.68786(7) 0.0488 1.0000 Uani . . . . . .
C236 C 0.43247(14) 0.43223(10) 0.64245(7) 0.0558 1.0000 Uani . . . . . .
C237 C 0.41682(15) 0.47783(11) 0.58505(7) 0.0603 1.0000 Uani . . . . . .
H1041 H 0.2704 0.0691 0.9623 0.0551 1.0000 Uiso R . . . . .
H1061 H 0.0385 0.1766 1.0764 0.0496 1.0000 Uiso R . . . . .
H1071 H -0.0574 0.2635 1.0064 0.0432 1.0000 Uiso R . . . . .
H1081 H 0.1865 0.0478 1.1048 0.0958 1.0000 Uiso R . . . . .
H1083 H 0.2705 0.0917 1.0836 0.0953 1.0000 Uiso R . . . . .
H1082 H 0.2812 0.0109 1.0600 0.0945 1.0000 Uiso R . . . . .
H1171 H 0.0462 0.3944 0.9188 0.0458 1.0000 Uiso R . . . . .
H1181 H -0.0512 0.5167 0.9556 0.0473 1.0000 Uiso R . . . . .
H1201 H -0.3249 0.4700 0.9560 0.0521 1.0000 Uiso R . . . . .
H1211 H -0.2276 0.3471 0.9212 0.0474 1.0000 Uiso R . . . . .
H1223 H -0.3003 0.5747 1.0181 0.0764 1.0000 Uiso R . . . . .
H1221 H -0.3118 0.6213 0.9579 0.0783 1.0000 Uiso R . . . . .
H1222 H -0.2137 0.6144 0.9869 0.0766 1.0000 Uiso R . . . . .
H1101 H -0.0669 0.2924 0.7932 0.0391 1.0000 Uiso R . . . . .
H1111 H -0.1651 0.2298 0.7596 0.0418 1.0000 Uiso R . . . . .
H1131 H -0.2096 0.1065 0.9111 0.0469 1.0000 Uiso R . . . . .
H1141 H -0.1103 0.1691 0.9464 0.0414 1.0000 Uiso R . . . . .
H1151 H -0.3137 0.1086 0.8341 0.0822 1.0000 Uiso R . . . . .
H1152 H -0.2864 0.1509 0.7759 0.0831 1.0000 Uiso R . . . . .
H1153 H -0.2166 0.0695 0.7994 0.0828 1.0000 Uiso R . . . . .
H731 H 0.0602 0.1726 0.7274 0.0456 1.0000 Uiso R . . . . .
H741 H -0.0346 0.0938 0.7094 0.0584 1.0000 Uiso R . . . . .
H761 H -0.0125 0.1844 0.5477 0.0554 1.0000 Uiso R . . . . .
H771 H 0.0823 0.2634 0.5636 0.0445 1.0000 Uiso R . . . . .
H781 H -0.1280 0.0994 0.5824 0.1157 1.0000 Uiso R . . . . .
H782 H -0.1504 0.0760 0.6441 0.1153 1.0000 Uiso R . . . . .
H783 H -0.0520 0.0218 0.6136 0.1165 1.0000 Uiso R . . . . .
H801 H 0.3089 0.2601 0.7163 0.0417 1.0000 Uiso R . . . . .
H811 H 0.4876 0.1860 0.7073 0.0504 1.0000 Uiso R . . . . .
H831 H 0.4480 0.0954 0.5770 0.0488 1.0000 Uiso R . . . . .
H841 H 0.2677 0.1709 0.5856 0.0402 1.0000 Uiso R . . . . .
H853 H 0.6406 0.1039 0.6029 0.0911 1.0000 Uiso R . . . . .
H852 H 0.6155 0.0247 0.6344 0.0915 1.0000 Uiso R . . . . .
H851 H 0.6357 0.0860 0.6670 0.0910 1.0000 Uiso R . . . . .
H871 H -0.0277 0.4013 0.6555 0.0386 1.0000 Uiso R . . . . .
H881 H -0.0740 0.5307 0.6020 0.0414 1.0000 Uiso R . . . . .
H901 H 0.2191 0.4697 0.5175 0.0472 1.0000 Uiso R . . . . .
H2381 H 0.2662 0.3413 0.5715 0.0424 1.0000 Uiso R . . . . .
H912 H 0.0338 0.6409 0.5387 0.0726 1.0000 Uiso R . . . . .
H911 H -0.0324 0.6129 0.5086 0.0740 1.0000 Uiso R . . . . .
H913 H 0.0804 0.6001 0.4862 0.0738 1.0000 Uiso R . . . . .
H201 H 0.4417 0.5606 0.7743 0.0434 1.0000 Uiso R . . . . .
H211 H 0.5369 0.4220 0.7897 0.0546 1.0000 Uiso R . . . . .
H231 H 0.5019 0.4287 0.9545 0.0526 1.0000 Uiso R . . . . .
H241 H 0.4088 0.5694 0.9372 0.0449 1.0000 Uiso R . . . . .
H253 H 0.5565 0.2894 0.8691 0.0986 1.0000 Uiso R . . . . .
H252 H 0.5965 0.3007 0.9218 0.0994 1.0000 Uiso R . . . . .
H251 H 0.6618 0.3088 0.8643 0.0975 1.0000 Uiso R . . . . .
H131 H 0.1919 0.7696 0.7832 0.0411 1.0000 Uiso R . . . . .
H141 H 0.0095 0.7902 0.7931 0.0505 1.0000 Uiso R . . . . .
H161 H 0.0433 0.6144 0.9272 0.0514 1.0000 Uiso R . . . . .
H171 H 0.2271 0.5955 0.9182 0.0438 1.0000 Uiso R . . . . .
H181 H -0.1472 0.7404 0.8984 0.0913 1.0000 Uiso R . . . . .
H183 H -0.1404 0.7501 0.8348 0.0914 1.0000 Uiso R . . . . .
H182 H -0.1235 0.6636 0.8683 0.0929 1.0000 Uiso R . . . . .
H271 H 0.5281 0.6922 0.8511 0.0429 1.0000 Uiso R . . . . .
H281 H 0.5779 0.7628 0.9045 0.0511 1.0000 Uiso R . . . . .
H301 H 0.2821 0.8232 0.9861 0.0581 1.0000 Uiso R . . . . .
H311 H 0.2296 0.7552 0.9296 0.0486 1.0000 Uiso R . . . . .
H321 H 0.4204 0.8546 1.0209 0.1002 1.0000 Uiso R . . . . .
H322 H 0.5357 0.8156 0.9987 0.1003 1.0000 Uiso R . . . . .
H323 H 0.4698 0.8986 0.9694 0.1004 1.0000 Uiso R . . . . .
H431 H 0.3333 0.6949 0.6086 0.0448 1.0000 Uiso R . . . . .
H441 H 0.2413 0.6895 0.5386 0.0516 1.0000 Uiso R . . . . .
H461 H 0.4704 0.7374 0.4233 0.0467 1.0000 Uiso R . . . . .
H471 H 0.5625 0.7434 0.4924 0.0418 1.0000 Uiso R . . . . .
H481 H 0.2199 0.7027 0.4416 0.0788 1.0000 Uiso R . . . . .
H482 H 0.3281 0.6583 0.4114 0.0787 1.0000 Uiso R . . . . .
H483 H 0.2803 0.7547 0.3999 0.0807 1.0000 Uiso R . . . . .
H501 H 0.5654 0.6385 0.7059 0.0430 1.0000 Uiso R . . . . .
H511 H 0.6641 0.5034 0.7360 0.0455 1.0000 Uiso R . . . . .
H531 H 0.7359 0.4577 0.5787 0.0505 1.0000 Uiso R . . . . .
H541 H 0.6316 0.5911 0.5485 0.0470 1.0000 Uiso R . . . . .
H552 H 0.8201 0.3506 0.6519 0.0715 1.0000 Uiso R . . . . .
H551 H 0.7216 0.3466 0.6940 0.0709 1.0000 Uiso R . . . . .
H553 H 0.8082 0.3732 0.7117 0.0697 1.0000 Uiso R . . . . .
H571 H 0.4659 0.8792 0.5844 0.0490 1.0000 Uiso R . . . . .
H581 H 0.5617 0.9681 0.5476 0.0515 1.0000 Uiso R . . . . .
H601 H 0.8339 0.7740 0.5376 0.0473 1.0000 Uiso R . . . . .
H611 H 0.7372 0.6853 0.5747 0.0434 1.0000 Uiso R . . . . .
H623 H 0.7241 0.9942 0.5088 0.0776 1.0000 Uiso R . . . . .
H622 H 0.8124 0.9411 0.5443 0.0799 1.0000 Uiso R . . . . .
H621 H 0.8168 0.9240 0.4839 0.0791 1.0000 Uiso R . . . . .
H2021 H 0.4512 -0.1341 0.8054 0.0402 1.0000 Uiso R . . . . .
H2022 H 0.4130 -0.1598 0.7570 0.0398 1.0000 Uiso R . . . . .
H2031 H 0.5183 -0.0929 0.6932 0.0490 1.0000 Uiso R . . . . .
H2032 H 0.5547 -0.0670 0.7407 0.0489 1.0000 Uiso R . . . . .
H2041 H 0.6022 -0.2331 0.7265 0.0640 1.0000 Uiso R . . . . .
H2042 H 0.6369 -0.2051 0.7757 0.0626 1.0000 Uiso R . . . . .
H2051 H 0.7497 -0.1464 0.7161 0.0980 1.0000 Uiso R . . . . .
H2052 H 0.7156 -0.1682 0.6637 0.0972 1.0000 Uiso R . . . . .
H2053 H 0.7832 -0.2400 0.7076 0.0970 1.0000 Uiso R . . . . .
H2061 H 0.2954 0.0757 0.7822 0.0379 1.0000 Uiso R . . . . .
H2062 H 0.4134 0.0417 0.7530 0.0377 1.0000 Uiso R . . . . .
H2071 H 0.3527 0.0080 0.8680 0.0499 1.0000 Uiso R . . . . .
H2072 H 0.4674 -0.0339 0.8397 0.0496 1.0000 Uiso R . . . . .
H2081 H 0.3757 0.1384 0.8377 0.0586 1.0000 Uiso R . . . . .
H2082 H 0.4908 0.0947 0.8099 0.0591 1.0000 Uiso R . . . . .
H2091 H 0.5456 0.0305 0.8974 0.0871 1.0000 Uiso R . . . . .
H2092 H 0.5101 0.1272 0.8949 0.0867 1.0000 Uiso R . . . . .
H2093 H 0.4343 0.0772 0.9252 0.0887 1.0000 Uiso R . . . . .
H2101 H 0.2405 0.0405 0.7128 0.0369 1.0000 Uiso R . . . . .
H2102 H 0.3573 0.0005 0.6870 0.0363 1.0000 Uiso R . . . . .
H2111 H 0.3165 -0.1241 0.6873 0.0462 1.0000 Uiso R . . . . .
H2112 H 0.1986 -0.0800 0.7120 0.0449 1.0000 Uiso R . . . . .
H2121 H 0.1792 0.0204 0.6301 0.0439 1.0000 Uiso R . . . . .
H2122 H 0.2964 -0.0278 0.6059 0.0452 1.0000 Uiso R . . . . .
H2133 H 0.2384 -0.1424 0.6055 0.0803 1.0000 Uiso R . . . . .
H2132 H 0.1247 -0.0941 0.6302 0.0786 1.0000 Uiso R . . . . .
H2131 H 0.1675 -0.0634 0.5689 0.0784 1.0000 Uiso R . . . . .
H2141 H 0.2486 -0.1156 0.8014 0.0391 1.0000 Uiso R . . . . .
H2142 H 0.2819 -0.0775 0.8461 0.0404 1.0000 Uiso R . . . . .
H2151 H 0.1149 0.0095 0.7768 0.0520 1.0000 Uiso R . . . . .
H2152 H 0.1471 0.0519 0.8192 0.0516 1.0000 Uiso R . . . . .
H2161 H 0.0723 -0.0863 0.8549 0.0627 1.0000 Uiso R . . . . .
H2162 H -0.0054 0.0040 0.8517 0.0628 1.0000 Uiso R . . . . .
H2173 H 0.0383 -0.0460 0.9444 0.0870 1.0000 Uiso R . . . . .
H2172 H 0.0753 0.0304 0.9202 0.0862 1.0000 Uiso R . . . . .
H2171 H 0.1600 -0.0583 0.9238 0.0876 1.0000 Uiso R . . . . .
H2221 H 0.0451 0.5077 0.6989 0.0440 1.0000 Uiso R . . . . .
H2222 H 0.0822 0.4387 0.7483 0.0441 1.0000 Uiso R . . . . .
H2231 H -0.0523 0.6006 0.7618 0.0478 1.0000 Uiso R . . . . .
H2232 H -0.0120 0.5304 0.8113 0.0476 1.0000 Uiso R . . . . .
H2241 H -0.1404 0.5195 0.7364 0.0623 1.0000 Uiso R . . . . .
H2242 H -0.1040 0.4537 0.7896 0.0643 1.0000 Uiso R . . . . .
H2253 H -0.2465 0.6195 0.7891 0.0848 1.0000 Uiso R . . . . .
H2252 H -0.2102 0.5619 0.8440 0.0828 1.0000 Uiso R . . . . .
H2251 H -0.2841 0.5411 0.8102 0.0841 1.0000 Uiso R . . . . .
H2261 H 0.0925 0.6360 0.7477 0.0411 1.0000 Uiso R . . . . .
H2262 H 0.2094 0.6203 0.7164 0.0426 1.0000 Uiso R . . . . .
H2271 H 0.0275 0.6375 0.6630 0.0520 1.0000 Uiso R . . . . .
H2272 H 0.1409 0.6311 0.6329 0.0515 1.0000 Uiso R . . . . .
H2281 H 0.1291 0.7551 0.6579 0.0605 1.0000 Uiso R . . . . .
H2282 H 0.0128 0.7619 0.6897 0.0616 1.0000 Uiso R . . . . .
H2291 H 0.0568 0.7695 0.5734 0.0875 1.0000 Uiso R . . . . .
H2292 H -0.0076 0.8491 0.6034 0.0862 1.0000 Uiso R . . . . .
H2293 H -0.0560 0.7753 0.6069 0.0866 1.0000 Uiso R . . . . .
H2301 H 0.2630 0.5183 0.7859 0.0401 1.0000 Uiso R . . . . .
H2302 H 0.1474 0.5285 0.8146 0.0405 1.0000 Uiso R . . . . .
H2311 H 0.1800 0.3856 0.8134 0.0484 1.0000 Uiso R . . . . .
H2312 H 0.3007 0.3758 0.7896 0.0474 1.0000 Uiso R . . . . .
H2321 H 0.2023 0.4246 0.8950 0.0466 1.0000 Uiso R . . . . .
H2322 H 0.3192 0.4215 0.8719 0.0464 1.0000 Uiso R . . . . .
H2331 H 0.2525 0.2813 0.8983 0.0811 1.0000 Uiso R . . . . .
H2332 H 0.3276 0.2985 0.9334 0.0801 1.0000 Uiso R . . . . .
H2333 H 0.3701 0.2760 0.8727 0.0779 1.0000 Uiso R . . . . .
H2341 H 0.2471 0.4150 0.7006 0.0444 1.0000 Uiso R . . . . .
H2342 H 0.2165 0.4939 0.6560 0.0461 1.0000 Uiso R . . . . .
H2351 H 0.3847 0.4526 0.7242 0.0599 1.0000 Uiso R . . . . .
H2352 H 0.3521 0.5357 0.6814 0.0574 1.0000 Uiso R . . . . .
H2361 H 0.5077 0.4250 0.6468 0.0687 1.0000 Uiso R . . . . .
H2362 H 0.4252 0.3764 0.6448 0.0665 1.0000 Uiso R . . . . .
H2373 H 0.3407 0.4916 0.5788 0.0903 1.0000 Uiso R . . . . .
H2372 H 0.4653 0.4457 0.5566 0.0889 1.0000 Uiso R . . . . .
H2371 H 0.4328 0.5298 0.5823 0.0896 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       111(12)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          3.56(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C91 . C89 . 1.5093(16) yes
C91 . H912 . 0.949 no
C91 . H911 . 0.961 no
C91 . H913 . 0.933 no
C11 . C12 . 1.5421(16) yes
C11 . C19 . 1.5419(16) yes
C11 . C26 . 1.5369(15) yes
C11 . O1 . 1.4172(13) yes
C12 . C13 . 1.3911(17) yes
C12 . C17 . 1.3973(16) yes
C13 . C14 . 1.3951(19) yes
C13 . H131 . 0.942 no
C14 . C15 . 1.388(2) yes
C14 . H141 . 0.950 no
C15 . C16 . 1.388(2) yes
C15 . C18 . 1.511(2) yes
C16 . C17 . 1.3891(19) yes
C16 . H161 . 0.979 no
C17 . H171 . 0.975 no
C18 . H181 . 0.973 no
C18 . H183 . 0.952 no
C18 . H182 . 0.969 no
C19 . C20 . 1.3926(17) yes
C19 . C24 . 1.3914(18) yes
C20 . C21 . 1.3918(19) yes
C20 . H201 . 0.933 no
C21 . C22 . 1.385(2) yes
C21 . H211 . 0.952 no
C22 . C23 . 1.385(2) yes
C22 . C25 . 1.5074(19) yes
C23 . C24 . 1.3923(19) yes
C23 . H231 . 0.987 no
C24 . H241 . 0.950 no
C25 . H253 . 0.963 no
C25 . H252 . 0.962 no
C25 . H251 . 0.962 no
C26 . C27 . 1.3974(18) yes
C26 . C31 . 1.3837(18) yes
C27 . C28 . 1.3829(18) yes
C27 . H271 . 0.928 no
C28 . C29 . 1.390(2) yes
C28 . H281 . 0.947 no
C29 . C30 . 1.381(2) yes
C29 . C32 . 1.5133(19) yes
C30 . C31 . 1.3976(19) yes
C30 . H301 . 0.966 no
C31 . H311 . 0.971 no
C32 . H321 . 0.958 no
C32 . H322 . 0.945 no
C32 . H323 . 0.951 no
C41 . C42 . 1.5413(17) yes
C41 . C49 . 1.5365(16) yes
C41 . C56 . 1.5345(15) yes
C41 . O2 . 1.4179(13) yes
C42 . C43 . 1.3899(17) yes
C42 . C47 . 1.3957(16) yes
C43 . C44 . 1.388(2) yes
C43 . H431 . 0.965 no
C44 . C45 . 1.390(2) yes
C44 . H441 . 0.959 no
C45 . C46 . 1.3860(19) yes
C45 . C48 . 1.5024(19) yes
C46 . C47 . 1.3866(18) yes
C46 . H461 . 0.965 no
C47 . H471 . 0.954 no
C48 . H481 . 0.963 no
C48 . H482 . 0.972 no
C48 . H483 . 0.959 no
C49 . C50 . 1.3898(17) yes
C49 . C54 . 1.3894(17) yes
C50 . C51 . 1.3881(19) yes
C50 . H501 . 0.953 no
C51 . C52 . 1.388(2) yes
C51 . H511 . 0.956 no
C52 . C53 . 1.3874(18) yes
C52 . C55 . 1.5054(18) yes
C53 . C54 . 1.3880(18) yes
C53 . H531 . 0.954 no
C54 . H541 . 0.962 no
C55 . H552 . 0.975 no
C55 . H551 . 0.966 no
C55 . H553 . 0.963 no
C56 . C57 . 1.3873(17) yes
C56 . C61 . 1.3874(17) yes
C57 . C58 . 1.3869(18) yes
C57 . H571 . 0.958 no
C58 . C59 . 1.388(2) yes
C58 . H581 . 0.958 no
C59 . C60 . 1.3842(19) yes
C59 . C62 . 1.5075(18) yes
C60 . C61 . 1.3908(17) yes
C60 . H601 . 0.975 no
C61 . H611 . 0.957 no
C62 . H623 . 0.966 no
C62 . H622 . 0.958 no
C62 . H621 . 0.972 no
C71 . C72 . 1.5414(16) yes
C71 . C79 . 1.5407(16) yes
C71 . C86 . 1.5405(15) yes
C71 . O3 . 1.4160(13) yes
C72 . C73 . 1.3952(17) yes
C72 . C77 . 1.3913(18) yes
C73 . C74 . 1.391(2) yes
C73 . H731 . 0.964 no
C74 . C75 . 1.384(2) yes
C74 . H741 . 0.950 no
C75 . C76 . 1.390(2) yes
C75 . C78 . 1.512(2) yes
C76 . C77 . 1.3883(19) yes
C76 . H761 . 0.946 no
C77 . H771 . 0.964 no
C78 . H781 . 0.956 no
C78 . H782 . 0.947 no
C78 . H783 . 0.957 no
C79 . C80 . 1.3892(17) yes
C79 . C84 . 1.3951(17) yes
C80 . C81 . 1.3954(19) yes
C80 . H801 . 0.944 no
C81 . C82 . 1.384(2) yes
C81 . H811 . 0.945 no
C82 . C83 . 1.389(2) yes
C82 . C85 . 1.5156(19) yes
C83 . C84 . 1.3906(18) yes
C83 . H831 . 0.971 no
C84 . H841 . 0.972 no
C85 . H853 . 0.964 no
C85 . H852 . 0.976 no
C85 . H851 . 0.951 no
C86 . C87 . 1.3954(16) yes
C86 . C238 . 1.3844(16) yes
C87 . C88 . 1.3878(17) yes
C87 . H871 . 0.954 no
C88 . C89 . 1.3914(18) yes
C88 . H881 . 0.957 no
C89 . C90 . 1.3830(19) yes
C90 . C238 . 1.3988(17) yes
C90 . H901 . 0.957 no
C238 . H2381 . 0.953 no
C101 . C102 . 1.5402(16) yes
C101 . C109 . 1.5351(16) yes
C101 . C116 . 1.5334(16) yes
C101 . O4 . 1.4219(13) yes
C102 . C103 . 1.3877(17) yes
C102 . C107 . 1.3913(17) yes
C103 . C104 . 1.388(2) yes
C103 . H1031 . 0.963 no
C104 . C105 . 1.385(2) yes
C104 . H1041 . 0.957 no
C105 . C106 . 1.384(2) yes
C105 . C108 . 1.506(2) yes
C106 . C107 . 1.3885(18) yes
C106 . H1061 . 0.962 no
C107 . H1071 . 0.956 no
C108 . H1081 . 0.970 no
C108 . H1083 . 0.970 no
C108 . H1082 . 0.979 no
C109 . C110 . 1.3919(17) yes
C109 . C114 . 1.3936(16) yes
C110 . C111 . 1.3871(17) yes
C110 . H1101 . 0.957 no
C111 . C112 . 1.3898(18) yes
C111 . H1111 . 0.953 no
C112 . C113 . 1.3877(19) yes
C112 . C115 . 1.5076(18) yes
C113 . C114 . 1.3872(18) yes
C113 . H1131 . 0.951 no
C114 . H1141 . 0.974 no
C115 . H1151 . 0.930 no
C115 . H1152 . 0.924 no
C115 . H1153 . 0.952 no
C116 . C117 . 1.3881(17) yes
C116 . C121 . 1.3862(17) yes
C117 . C118 . 1.3866(18) yes
C117 . H1171 . 0.974 no
C118 . C119 . 1.3882(19) yes
C118 . H1181 . 0.970 no
C119 . C120 . 1.3811(19) yes
C119 . C122 . 1.5059(18) yes
C120 . C121 . 1.3920(19) yes
C120 . H1201 . 0.964 no
C121 . H1211 . 0.953 no
C122 . H1223 . 0.979 no
C122 . H1221 . 0.969 no
C122 . H1222 . 0.989 no
O1 . H11 . 0.875 no
O2 . H21 . 0.880 no
O3 . H31 . 0.869 no
O4 . H41 . 0.860 no
N201 . C202 . 1.5192(14) yes
N201 . C206 . 1.5162(14) yes
N201 . C210 . 1.5173(15) yes
N201 . C214 . 1.5239(15) yes
C202 . C203 . 1.5134(18) yes
C202 . H2021 . 0.965 no
C202 . H2022 . 0.976 no
C203 . C204 . 1.5207(19) yes
C203 . H2031 . 0.955 no
C203 . H2032 . 0.969 no
C204 . C205 . 1.514(2) yes
C204 . H2041 . 0.983 no
C204 . H2042 . 0.980 no
C205 . H2051 . 0.976 no
C205 . H2052 . 0.995 no
C205 . H2053 . 0.988 no
C206 . C207 . 1.5151(18) yes
C206 . H2061 . 0.962 no
C206 . H2062 . 0.975 no
C207 . C208 . 1.5213(19) yes
C207 . H2071 . 0.985 no
C207 . H2072 . 0.973 no
C208 . C209 . 1.511(2) yes
C208 . H2081 . 0.970 no
C208 . H2082 . 0.979 no
C209 . H2091 . 0.973 no
C209 . H2092 . 0.986 no
C209 . H2093 . 0.960 no
C210 . C211 . 1.5134(17) yes
C210 . H2101 . 0.983 no
C210 . H2102 . 0.975 no
C211 . C212 . 1.5236(18) yes
C211 . H2111 . 0.971 no
C211 . H2112 . 0.997 no
C212 . C213 . 1.5164(19) yes
C212 . H2121 . 0.979 no
C212 . H2122 . 0.998 no
C213 . H2133 . 0.971 no
C213 . H2132 . 0.968 no
C213 . H2131 . 0.991 no
C214 . C215 . 1.5184(18) yes
C214 . H2141 . 0.985 no
C214 . H2142 . 0.991 no
C215 . C216 . 1.5331(19) yes
C215 . H2151 . 0.988 no
C215 . H2152 . 0.977 no
C216 . C217 . 1.510(3) yes
C216 . H2161 . 0.994 no
C216 . H2162 . 0.977 no
C217 . H2173 . 0.974 no
C217 . H2172 . 0.978 no
C217 . H2171 . 0.986 no
N221 . C222 . 1.5213(15) yes
N221 . C226 . 1.5170(15) yes
N221 . C230 . 1.5172(15) yes
N221 . C234 . 1.5265(16) yes
C222 . C223 . 1.5170(19) yes
C222 . H2221 . 0.962 no
C222 . H2222 . 0.964 no
C223 . C224 . 1.5195(18) yes
C223 . H2231 . 0.967 no
C223 . H2232 . 0.981 no
C224 . C225 . 1.520(2) yes
C224 . H2241 . 0.960 no
C224 . H2242 . 1.005 no
C225 . H2253 . 0.959 no
C225 . H2252 . 0.977 no
C225 . H2251 . 0.984 no
C226 . C227 . 1.5172(19) yes
C226 . H2261 . 0.974 no
C226 . H2262 . 0.981 no
C227 . C228 . 1.5163(19) yes
C227 . H2271 . 0.971 no
C227 . H2272 . 0.961 no
C228 . C229 . 1.511(2) yes
C228 . H2281 . 0.977 no
C228 . H2282 . 0.992 no
C229 . H2291 . 0.986 no
C229 . H2292 . 1.005 no
C229 . H2293 . 0.990 no
C230 . C231 . 1.5127(18) yes
C230 . H2301 . 0.969 no
C230 . H2302 . 0.977 no
C231 . C232 . 1.5236(18) yes
C231 . H2311 . 0.975 no
C231 . H2312 . 0.998 no
C232 . C233 . 1.515(2) yes
C232 . H2321 . 0.996 no
C232 . H2322 . 0.965 no
C233 . H2331 . 0.977 no
C233 . H2332 . 0.982 no
C233 . H2333 . 0.978 no
C234 . C235 . 1.522(2) yes
C234 . H2341 . 0.983 no
C234 . H2342 . 0.971 no
C235 . C236 . 1.540(2) yes
C235 . H2351 . 1.000 no
C235 . H2352 . 0.974 no
C236 . C237 . 1.504(3) yes
C236 . H2361 . 0.998 no
C236 . H2362 . 1.009 no
C237 . H2373 . 1.000 no
C237 . H2372 . 0.995 no
C237 . H2371 . 0.997 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C89 . C91 . H912 . 114.1 no
C89 . C91 . H911 . 110.9 no
H912 . C91 . H911 . 103.9 no
C89 . C91 . H913 . 113.4 no
H912 . C91 . H913 . 110.5 no
H911 . C91 . H913 . 103.2 no
C12 . C11 . C19 . 109.90(9) yes
C12 . C11 . C26 . 112.26(9) yes
C19 . C11 . C26 . 108.66(9) yes
C12 . C11 . O1 . 110.69(9) yes
C19 . C11 . O1 . 111.03(9) yes
C26 . C11 . O1 . 104.17(8) yes
C11 . C12 . C13 . 120.36(10) yes
C11 . C12 . C17 . 122.07(11) yes
C13 . C12 . C17 . 117.56(11) yes
C12 . C13 . C14 . 120.76(12) yes
C12 . C13 . H131 . 118.6 no
C14 . C13 . H131 . 120.6 no
C13 . C14 . C15 . 121.65(13) yes
C13 . C14 . H141 . 118.8 no
C15 . C14 . H141 . 119.6 no
C14 . C15 . C16 . 117.47(12) yes
C14 . C15 . C18 . 121.58(15) yes
C16 . C15 . C18 . 120.94(14) yes
C15 . C16 . C17 . 121.37(13) yes
C15 . C16 . H161 . 118.6 no
C17 . C16 . H161 . 120.0 no
C12 . C17 . C16 . 121.19(13) yes
C12 . C17 . H171 . 119.3 no
C16 . C17 . H171 . 119.5 no
C15 . C18 . H181 . 112.0 no
C15 . C18 . H183 . 109.1 no
H181 . C18 . H183 . 107.1 no
C15 . C18 . H182 . 112.4 no
H181 . C18 . H182 . 108.8 no
H183 . C18 . H182 . 107.1 no
C11 . C19 . C20 . 120.42(11) yes
C11 . C19 . C24 . 121.46(11) yes
C20 . C19 . C24 . 118.11(12) yes
C19 . C20 . C21 . 120.10(13) yes
C19 . C20 . H201 . 119.7 no
C21 . C20 . H201 . 120.2 no
C20 . C21 . C22 . 121.99(13) yes
C20 . C21 . H211 . 118.2 no
C22 . C21 . H211 . 119.8 no
C21 . C22 . C23 . 117.71(12) yes
C21 . C22 . C25 . 121.12(16) yes
C23 . C22 . C25 . 121.17(16) yes
C22 . C23 . C24 . 120.98(14) yes
C22 . C23 . H231 . 119.9 no
C24 . C23 . H231 . 119.1 no
C23 . C24 . C19 . 121.09(13) yes
C23 . C24 . H241 . 119.4 no
C19 . C24 . H241 . 119.5 no
C22 . C25 . H253 . 110.6 no
C22 . C25 . H252 . 111.3 no
H253 . C25 . H252 . 108.8 no
C22 . C25 . H251 . 110.4 no
H253 . C25 . H251 . 107.4 no
H252 . C25 . H251 . 108.3 no
C11 . C26 . C27 . 117.35(11) yes
C11 . C26 . C31 . 124.55(11) yes
C27 . C26 . C31 . 118.09(11) yes
C26 . C27 . C28 . 120.92(13) yes
C26 . C27 . H271 . 119.3 no
C28 . C27 . H271 . 119.8 no
C27 . C28 . C29 . 121.23(13) yes
C27 . C28 . H281 . 118.3 no
C29 . C28 . H281 . 120.5 no
C28 . C29 . C30 . 117.72(12) yes
C28 . C29 . C32 . 121.19(15) yes
C30 . C29 . C32 . 121.08(15) yes
C29 . C30 . C31 . 121.57(13) yes
C29 . C30 . H301 . 119.1 no
C31 . C30 . H301 . 119.3 no
C30 . C31 . C26 . 120.43(13) yes
C30 . C31 . H311 . 118.9 no
C26 . C31 . H311 . 120.7 no
C29 . C32 . H321 . 112.3 no
C29 . C32 . H322 . 109.9 no
H321 . C32 . H322 . 106.1 no
C29 . C32 . H323 . 112.9 no
H321 . C32 . H323 . 107.6 no
H322 . C32 . H323 . 107.7 no
C42 . C41 . C49 . 109.08(9) yes
C42 . C41 . C56 . 109.02(9) yes
C49 . C41 . C56 . 111.61(10) yes
C42 . C41 . O2 . 110.69(10) yes
C49 . C41 . O2 . 110.96(9) yes
C56 . C41 . O2 . 105.44(9) yes
C41 . C42 . C43 . 120.18(10) yes
C41 . C42 . C47 . 121.76(10) yes
C43 . C42 . C47 . 117.99(12) yes
C42 . C43 . C44 . 120.46(12) yes
C42 . C43 . H431 . 119.4 no
C44 . C43 . H431 . 120.1 no
C43 . C44 . C45 . 121.77(12) yes
C43 . C44 . H441 . 118.5 no
C45 . C44 . H441 . 119.7 no
C44 . C45 . C46 . 117.52(12) yes
C44 . C45 . C48 . 122.21(13) yes
C46 . C45 . C48 . 120.25(13) yes
C45 . C46 . C47 . 121.29(12) yes
C45 . C46 . H461 . 119.2 no
C47 . C46 . H461 . 119.5 no
C42 . C47 . C46 . 120.96(12) yes
C42 . C47 . H471 . 120.5 no
C46 . C47 . H471 . 118.5 no
C45 . C48 . H481 . 111.6 no
C45 . C48 . H482 . 110.0 no
H481 . C48 . H482 . 105.4 no
C45 . C48 . H483 . 111.3 no
H481 . C48 . H483 . 109.0 no
H482 . C48 . H483 . 109.3 no
C41 . C49 . C50 . 120.57(11) yes
C41 . C49 . C54 . 121.66(10) yes
C50 . C49 . C54 . 117.77(11) yes
C49 . C50 . C51 . 120.55(12) yes
C49 . C50 . H501 . 119.1 no
C51 . C50 . H501 . 120.3 no
C50 . C51 . C52 . 121.86(11) yes
C50 . C51 . H511 . 118.4 no
C52 . C51 . H511 . 119.7 no
C51 . C52 . C53 . 117.36(12) yes
C51 . C52 . C55 . 120.74(12) yes
C53 . C52 . C55 . 121.86(13) yes
C52 . C53 . C54 . 121.12(12) yes
C52 . C53 . H531 . 119.2 no
C54 . C53 . H531 . 119.7 no
C49 . C54 . C53 . 121.30(12) yes
C49 . C54 . H541 . 119.8 no
C53 . C54 . H541 . 118.9 no
C52 . C55 . H552 . 111.5 no
C52 . C55 . H551 . 110.8 no
H552 . C55 . H551 . 107.2 no
C52 . C55 . H553 . 111.3 no
H552 . C55 . H553 . 109.1 no
H551 . C55 . H553 . 106.8 no
C41 . C56 . C57 . 117.82(11) yes
C41 . C56 . C61 . 124.24(11) yes
C57 . C56 . C61 . 117.83(11) yes
C56 . C57 . C58 . 121.10(12) yes
C56 . C57 . H571 . 119.4 no
C58 . C57 . H571 . 119.5 no
C57 . C58 . C59 . 121.30(12) yes
C57 . C58 . H581 . 119.1 no
C59 . C58 . H581 . 119.6 no
C58 . C59 . C60 . 117.45(12) yes
C58 . C59 . C62 . 121.35(13) yes
C60 . C59 . C62 . 121.20(13) yes
C59 . C60 . C61 . 121.52(12) yes
C59 . C60 . H601 . 119.5 no
C61 . C60 . H601 . 119.0 no
C60 . C61 . C56 . 120.79(12) yes
C60 . C61 . H611 . 119.2 no
C56 . C61 . H611 . 120.0 no
C59 . C62 . H623 . 111.1 no
C59 . C62 . H622 . 111.5 no
H623 . C62 . H622 . 104.7 no
C59 . C62 . H621 . 112.7 no
H623 . C62 . H621 . 107.1 no
H622 . C62 . H621 . 109.5 no
C72 . C71 . C79 . 109.53(9) yes
C72 . C71 . C86 . 109.38(9) yes
C79 . C71 . C86 . 112.02(9) yes
C72 . C71 . O3 . 110.95(9) yes
C79 . C71 . O3 . 110.76(9) yes
C86 . C71 . O3 . 104.12(8) yes
C71 . C72 . C73 . 120.01(11) yes
C71 . C72 . C77 . 121.88(10) yes
C73 . C72 . C77 . 118.09(12) yes
C72 . C73 . C74 . 120.01(14) yes
C72 . C73 . H731 . 120.0 no
C74 . C73 . H731 . 120.0 no
C73 . C74 . C75 . 122.09(14) yes
C73 . C74 . H741 . 118.4 no
C75 . C74 . H741 . 119.5 no
C74 . C75 . C76 . 117.64(13) yes
C74 . C75 . C78 . 121.48(17) yes
C76 . C75 . C78 . 120.87(17) yes
C75 . C76 . C77 . 120.96(14) yes
C75 . C76 . H761 . 120.1 no
C77 . C76 . H761 . 118.9 no
C72 . C77 . C76 . 121.20(13) yes
C72 . C77 . H771 . 120.2 no
C76 . C77 . H771 . 118.6 no
C75 . C78 . H781 . 111.9 no
C75 . C78 . H782 . 110.9 no
H781 . C78 . H782 . 105.8 no
C75 . C78 . H783 . 114.0 no
H781 . C78 . H783 . 107.7 no
H782 . C78 . H783 . 106.0 no
C71 . C79 . C80 . 120.20(10) yes
C71 . C79 . C84 . 122.24(10) yes
C80 . C79 . C84 . 117.57(11) yes
C79 . C80 . C81 . 120.89(12) yes
C79 . C80 . H801 . 119.9 no
C81 . C80 . H801 . 119.2 no
C80 . C81 . C82 . 121.56(13) yes
C80 . C81 . H811 . 118.1 no
C82 . C81 . H811 . 120.3 no
C81 . C82 . C83 . 117.56(12) yes
C81 . C82 . C85 . 121.65(14) yes
C83 . C82 . C85 . 120.77(15) yes
C82 . C83 . C84 . 121.28(13) yes
C82 . C83 . H831 . 120.2 no
C84 . C83 . H831 . 118.6 no
C79 . C84 . C83 . 121.14(12) yes
C79 . C84 . H841 . 120.0 no
C83 . C84 . H841 . 118.9 no
C82 . C85 . H853 . 110.6 no
C82 . C85 . H852 . 110.6 no
H853 . C85 . H852 . 108.5 no
C82 . C85 . H851 . 108.0 no
H853 . C85 . H851 . 108.8 no
H852 . C85 . H851 . 110.3 no
C71 . C86 . C87 . 117.33(10) yes
C71 . C86 . C238 . 124.66(10) yes
C87 . C86 . C238 . 117.99(10) yes
C86 . C87 . C88 . 121.31(11) yes
C86 . C87 . H871 . 119.4 no
C88 . C87 . H871 . 119.3 no
C87 . C88 . C89 . 120.79(11) yes
C87 . C88 . H881 . 119.9 no
C89 . C88 . H881 . 119.3 no
C91 . C89 . C88 . 120.75(12) yes
C91 . C89 . C90 . 121.40(12) yes
C88 . C89 . C90 . 117.85(11) yes
C89 . C90 . C238 . 121.62(12) yes
C89 . C90 . H901 . 119.9 no
C238 . C90 . H901 . 118.5 no
C90 . C238 . C86 . 120.43(12) yes
C90 . C238 . H2381 . 119.5 no
C86 . C238 . H2381 . 120.0 no
C102 . C101 . C109 . 110.10(9) yes
C102 . C101 . C116 . 108.78(9) yes
C109 . C101 . C116 . 112.11(9) yes
C102 . C101 . O4 . 110.21(9) yes
C109 . C101 . O4 . 110.36(9) yes
C116 . C101 . O4 . 105.16(9) yes
C101 . C102 . C103 . 120.01(11) yes
C101 . C102 . C107 . 121.84(11) yes
C103 . C102 . C107 . 118.14(11) yes
C102 . C103 . C104 . 120.45(12) yes
C102 . C103 . H1031 . 118.8 no
C104 . C103 . H1031 . 120.8 no
C103 . C104 . C105 . 121.53(13) yes
C103 . C104 . H1041 . 118.7 no
C105 . C104 . H1041 . 119.8 no
C104 . C105 . C106 . 117.93(12) yes
C104 . C105 . C108 . 121.24(15) yes
C106 . C105 . C108 . 120.81(14) yes
C105 . C106 . C107 . 120.93(13) yes
C105 . C106 . H1061 . 120.1 no
C107 . C106 . H1061 . 118.9 no
C102 . C107 . C106 . 120.95(12) yes
C102 . C107 . H1071 . 120.2 no
C106 . C107 . H1071 . 118.9 no
C105 . C108 . H1081 . 111.7 no
C105 . C108 . H1083 . 109.4 no
H1081 . C108 . H1083 . 106.0 no
C105 . C108 . H1082 . 111.1 no
H1081 . C108 . H1082 . 109.1 no
H1083 . C108 . H1082 . 109.4 no
C101 . C109 . C110 . 119.94(10) yes
C101 . C109 . C114 . 122.31(11) yes
C110 . C109 . C114 . 117.74(11) yes
C109 . C110 . C111 . 120.89(11) yes
C109 . C110 . H1101 . 119.8 no
C111 . C110 . H1101 . 119.3 no
C110 . C111 . C112 . 121.37(12) yes
C110 . C111 . H1111 . 119.3 no
C112 . C111 . H1111 . 119.3 no
C111 . C112 . C113 . 117.73(11) yes
C111 . C112 . C115 . 120.25(12) yes
C113 . C112 . C115 . 122.01(12) yes
C112 . C113 . C114 . 121.18(11) yes
C112 . C113 . H1131 . 119.0 no
C114 . C113 . H1131 . 119.8 no
C109 . C114 . C113 . 121.08(12) yes
C109 . C114 . H1141 . 118.3 no
C113 . C114 . H1141 . 120.7 no
C112 . C115 . H1151 . 113.8 no
C112 . C115 . H1152 . 112.5 no
H1151 . C115 . H1152 . 112.6 no
C112 . C115 . H1153 . 110.1 no
H1151 . C115 . H1153 . 102.6 no
H1152 . C115 . H1153 . 104.2 no
C101 . C116 . C117 . 117.95(10) yes
C101 . C116 . C121 . 124.31(10) yes
C117 . C116 . C121 . 117.65(11) yes
C116 . C117 . C118 . 121.18(12) yes
C116 . C117 . H1171 . 118.4 no
C118 . C117 . H1171 . 120.4 no
C117 . C118 . C119 . 121.23(12) yes
C117 . C118 . H1181 . 119.8 no
C119 . C118 . H1181 . 119.0 no
C118 . C119 . C120 . 117.56(12) yes
C118 . C119 . C122 . 121.29(12) yes
C120 . C119 . C122 . 121.14(13) yes
C119 . C120 . C121 . 121.43(12) yes
C119 . C120 . H1201 . 118.9 no
C121 . C120 . H1201 . 119.7 no
C120 . C121 . C116 . 120.94(12) yes
C120 . C121 . H1211 . 120.0 no
C116 . C121 . H1211 . 119.1 no
C119 . C122 . H1223 . 112.5 no
C119 . C122 . H1221 . 112.1 no
H1223 . C122 . H1221 . 106.9 no
C119 . C122 . H1222 . 111.6 no
H1223 . C122 . H1222 . 107.1 no
H1221 . C122 . H1222 . 106.1 no
C11 . O1 . H11 . 113.1 no
C41 . O2 . H21 . 111.1 no
C71 . O3 . H31 . 110.6 no
C101 . O4 . H41 . 109.9 no
C202 . N201 . C206 . 111.83(9) yes
C202 . N201 . C210 . 111.01(9) yes
C206 . N201 . C210 . 105.67(8) yes
C202 . N201 . C214 . 106.27(8) yes
C206 . N201 . C214 . 110.85(9) yes
C210 . N201 . C214 . 111.30(9) yes
N201 . C202 . C203 . 116.56(10) yes
N201 . C202 . H2021 . 105.8 no
C203 . C202 . H2021 . 109.1 no
N201 . C202 . H2022 . 106.5 no
C203 . C202 . H2022 . 109.8 no
H2021 . C202 . H2022 . 108.7 no
C202 . C203 . C204 . 109.68(11) yes
C202 . C203 . H2031 . 110.7 no
C204 . C203 . H2031 . 109.8 no
C202 . C203 . H2032 . 110.8 no
C204 . C203 . H2032 . 108.8 no
H2031 . C203 . H2032 . 107.0 no
C203 . C204 . C205 . 113.32(14) yes
C203 . C204 . H2041 . 109.5 no
C205 . C204 . H2041 . 109.9 no
C203 . C204 . H2042 . 108.2 no
C205 . C204 . H2042 . 107.3 no
H2041 . C204 . H2042 . 108.5 no
C204 . C205 . H2051 . 109.3 no
C204 . C205 . H2052 . 110.3 no
H2051 . C205 . H2052 . 108.6 no
C204 . C205 . H2053 . 111.3 no
H2051 . C205 . H2053 . 108.4 no
H2052 . C205 . H2053 . 108.9 no
N201 . C206 . C207 . 116.45(10) yes
N201 . C206 . H2061 . 106.9 no
C207 . C206 . H2061 . 109.5 no
N201 . C206 . H2062 . 105.2 no
C207 . C206 . H2062 . 108.1 no
H2061 . C206 . H2062 . 110.7 no
C206 . C207 . C208 . 108.82(11) yes
C206 . C207 . H2071 . 110.6 no
C208 . C207 . H2071 . 110.0 no
C206 . C207 . H2072 . 110.7 no
C208 . C207 . H2072 . 109.7 no
H2071 . C207 . H2072 . 106.9 no
C207 . C208 . C209 . 113.45(13) yes
C207 . C208 . H2081 . 108.9 no
C209 . C208 . H2081 . 110.1 no
C207 . C208 . H2082 . 107.7 no
C209 . C208 . H2082 . 108.3 no
H2081 . C208 . H2082 . 108.3 no
C208 . C209 . H2091 . 109.3 no
C208 . C209 . H2092 . 112.9 no
H2091 . C209 . H2092 . 108.3 no
C208 . C209 . H2093 . 110.5 no
H2091 . C209 . H2093 . 107.2 no
H2092 . C209 . H2093 . 108.5 no
N201 . C210 . C211 . 116.16(9) yes
N201 . C210 . H2101 . 107.1 no
C211 . C210 . H2101 . 110.2 no
N201 . C210 . H2102 . 105.3 no
C211 . C210 . H2102 . 111.2 no
H2101 . C210 . H2102 . 106.3 no
C210 . C211 . C212 . 109.43(10) yes
C210 . C211 . H2111 . 112.2 no
C212 . C211 . H2111 . 108.8 no
C210 . C211 . H2112 . 110.1 no
C212 . C211 . H2112 . 109.2 no
H2111 . C211 . H2112 . 107.0 no
C211 . C212 . C213 . 111.76(11) yes
C211 . C212 . H2121 . 109.8 no
C213 . C212 . H2121 . 108.9 no
C211 . C212 . H2122 . 109.1 no
C213 . C212 . H2122 . 110.2 no
H2121 . C212 . H2122 . 106.9 no
C212 . C213 . H2133 . 110.8 no
C212 . C213 . H2132 . 109.9 no
H2133 . C213 . H2132 . 107.1 no
C212 . C213 . H2131 . 111.0 no
H2133 . C213 . H2131 . 108.6 no
H2132 . C213 . H2131 . 109.4 no
N201 . C214 . C215 . 115.73(10) yes
N201 . C214 . H2141 . 106.7 no
C215 . C214 . H2141 . 110.2 no
N201 . C214 . H2142 . 105.6 no
C215 . C214 . H2142 . 110.6 no
H2141 . C214 . H2142 . 107.6 no
C214 . C215 . C216 . 110.36(12) yes
C214 . C215 . H2151 . 108.4 no
C216 . C215 . H2151 . 109.2 no
C214 . C215 . H2152 . 110.6 no
C216 . C215 . H2152 . 110.1 no
H2151 . C215 . H2152 . 108.1 no
C215 . C216 . C217 . 114.14(13) yes
C215 . C216 . H2161 . 109.7 no
C217 . C216 . H2161 . 110.2 no
C215 . C216 . H2162 . 107.9 no
C217 . C216 . H2162 . 109.6 no
H2161 . C216 . H2162 . 104.8 no
C216 . C217 . H2173 . 112.9 no
C216 . C217 . H2172 . 109.9 no
H2173 . C217 . H2172 . 107.2 no
C216 . C217 . H2171 . 111.8 no
H2173 . C217 . H2171 . 108.1 no
H2172 . C217 . H2171 . 106.5 no
C222 . N221 . C226 . 111.38(10) yes
C222 . N221 . C230 . 110.40(9) yes
C226 . N221 . C230 . 106.06(9) yes
C222 . N221 . C234 . 107.31(9) yes
C226 . N221 . C234 . 110.84(10) yes
C230 . N221 . C234 . 110.90(10) yes
N221 . C222 . C223 . 115.57(10) yes
N221 . C222 . H2221 . 106.3 no
C223 . C222 . H2221 . 110.2 no
N221 . C222 . H2222 . 106.6 no
C223 . C222 . H2222 . 109.8 no
H2221 . C222 . H2222 . 108.1 no
C222 . C223 . C224 . 111.01(11) yes
C222 . C223 . H2231 . 111.0 no
C224 . C223 . H2231 . 109.0 no
C222 . C223 . H2232 . 109.1 no
C224 . C223 . H2232 . 108.4 no
H2231 . C223 . H2232 . 108.3 no
C223 . C224 . C225 . 112.05(13) yes
C223 . C224 . H2241 . 108.2 no
C225 . C224 . H2241 . 109.1 no
C223 . C224 . H2242 . 106.8 no
C225 . C224 . H2242 . 111.8 no
H2241 . C224 . H2242 . 108.8 no
C224 . C225 . H2253 . 109.4 no
C224 . C225 . H2252 . 110.1 no
H2253 . C225 . H2252 . 108.3 no
C224 . C225 . H2251 . 111.9 no
H2253 . C225 . H2251 . 110.3 no
H2252 . C225 . H2251 . 106.7 no
N221 . C226 . C227 . 116.37(10) yes
N221 . C226 . H2261 . 105.3 no
C227 . C226 . H2261 . 108.7 no
N221 . C226 . H2262 . 106.1 no
C227 . C226 . H2262 . 110.7 no
H2261 . C226 . H2262 . 109.3 no
C226 . C227 . C228 . 109.28(11) yes
C226 . C227 . H2271 . 111.8 no
C228 . C227 . H2271 . 108.5 no
C226 . C227 . H2272 . 110.9 no
C228 . C227 . H2272 . 108.3 no
H2271 . C227 . H2272 . 108.0 no
C227 . C228 . C229 . 113.80(13) yes
C227 . C228 . H2281 . 108.4 no
C229 . C228 . H2281 . 110.4 no
C227 . C228 . H2282 . 107.9 no
C229 . C228 . H2282 . 106.5 no
H2281 . C228 . H2282 . 109.8 no
C228 . C229 . H2291 . 110.1 no
C228 . C229 . H2292 . 112.5 no
H2291 . C229 . H2292 . 108.3 no
C228 . C229 . H2293 . 109.9 no
H2291 . C229 . H2293 . 106.9 no
H2292 . C229 . H2293 . 108.9 no
N221 . C230 . C231 . 115.96(10) yes
N221 . C230 . H2301 . 105.9 no
C231 . C230 . H2301 . 110.8 no
N221 . C230 . H2302 . 106.5 no
C231 . C230 . H2302 . 110.0 no
H2301 . C230 . H2302 . 107.3 no
C230 . C231 . C232 . 109.55(11) yes
C230 . C231 . H2311 . 109.6 no
C232 . C231 . H2311 . 110.0 no
C230 . C231 . H2312 . 109.9 no
C232 . C231 . H2312 . 109.7 no
H2311 . C231 . H2312 . 108.1 no
C231 . C232 . C233 . 111.90(12) yes
C231 . C232 . H2321 . 108.6 no
C233 . C232 . H2321 . 109.7 no
C231 . C232 . H2322 . 110.1 no
C233 . C232 . H2322 . 109.8 no
H2321 . C232 . H2322 . 106.5 no
C232 . C233 . H2331 . 109.3 no
C232 . C233 . H2332 . 111.9 no
H2331 . C233 . H2332 . 107.0 no
C232 . C233 . H2333 . 111.0 no
H2331 . C233 . H2333 . 108.4 no
H2332 . C233 . H2333 . 109.0 no
N221 . C234 . C235 . 115.21(10) yes
N221 . C234 . H2341 . 106.3 no
C235 . C234 . H2341 . 111.0 no
N221 . C234 . H2342 . 105.8 no
C235 . C234 . H2342 . 110.8 no
H2341 . C234 . H2342 . 107.3 no
C234 . C235 . C236 . 111.45(13) yes
C234 . C235 . H2351 . 107.9 no
C236 . C235 . H2351 . 108.8 no
C234 . C235 . H2352 . 109.4 no
C236 . C235 . H2352 . 110.7 no
H2351 . C235 . H2352 . 108.6 no
C235 . C236 . C237 . 113.92(14) yes
C235 . C236 . H2361 . 110.2 no
C237 . C236 . H2361 . 104.1 no
C235 . C236 . H2362 . 110.2 no
C237 . C236 . H2362 . 109.4 no
H2361 . C236 . H2362 . 108.7 no
C236 . C237 . H2373 . 108.8 no
C236 . C237 . H2372 . 112.0 no
H2373 . C237 . H2372 . 110.8 no
C236 . C237 . H2371 . 108.1 no
H2373 . C237 . H2371 . 108.9 no
H2372 . C237 . H2371 . 108.3 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C202 . H2022 . O1 1_545 144.03 0.976 2.470 3.310(2) yes
C211 . H2111 . O2 1_545 159.64 0.971 2.507 3.435(2) yes
C231 . H2311 . O4 . 156.45 0.975 2.520 3.436(2) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 25/04/13 at 19:05:31
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE C   (  91,X'S) H   ( 912,X'S) H   ( 911,X'S) H   ( 913,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 183,X'S) H   ( 182,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 253,X'S) H   ( 252,X'S) H   ( 251,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) H   ( 323,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 482,X'S) H   ( 483,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 552,X'S) H   ( 551,X'S) H   ( 553,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  62,X'S) H   ( 623,X'S) H   ( 622,X'S) H   ( 621,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) H   ( 782,X'S) H   ( 783,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) 
RIDE C   (  85,X'S) H   ( 853,X'S) H   ( 852,X'S) H   ( 851,X'S) 
RIDE C   (  87,X'S) H   ( 871,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) 
RIDE C   ( 238,X'S) H   (2381,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 107,X'S) H   (1071,X'S) 
RIDE C   ( 108,X'S) H   (1081,X'S) H   (1083,X'S) H   (1082,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) H   (1152,X'S) H   (1153,X'S) 
RIDE C   ( 117,X'S) H   (1171,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 120,X'S) H   (1201,X'S) 
RIDE C   ( 121,X'S) H   (1211,X'S) 
RIDE C   ( 122,X'S) H   (1223,X'S) H   (1221,X'S) H   (1222,X'S) 
RIDE O   (   1,X'S) H   (  11,X'S) 
RIDE O   (   2,X'S) H   (  21,X'S) 
RIDE O   (   3,X'S) H   (  31,X'S) 
RIDE O   (   4,X'S) H   (  41,X'S) 
RIDE C   ( 202,X'S) H   (2021,X'S) H   (2022,X'S) 
RIDE C   ( 203,X'S) H   (2031,X'S) H   (2032,X'S) 
RIDE C   ( 204,X'S) H   (2041,X'S) H   (2042,X'S) 
RIDE C   ( 205,X'S) H   (2051,X'S) H   (2052,X'S) H   (2053,X'S) 
RIDE C   ( 206,X'S) H   (2061,X'S) H   (2062,X'S) 
RIDE C   ( 207,X'S) H   (2071,X'S) H   (2072,X'S) 
RIDE C   ( 208,X'S) H   (2081,X'S) H   (2082,X'S) 
RIDE C   ( 209,X'S) H   (2091,X'S) H   (2092,X'S) H   (2093,X'S) 
RIDE C   ( 210,X'S) H   (2101,X'S) H   (2102,X'S) 
RIDE C   ( 211,X'S) H   (2111,X'S) H   (2112,X'S) 
RIDE C   ( 212,X'S) H   (2121,X'S) H   (2122,X'S) 
RIDE C   ( 213,X'S) H   (2133,X'S) H   (2132,X'S) H   (2131,X'S) 
RIDE C   ( 214,X'S) H   (2141,X'S) H   (2142,X'S) 
RIDE C   ( 215,X'S) H   (2151,X'S) H   (2152,X'S) 
RIDE C   ( 216,X'S) H   (2161,X'S) H   (2162,X'S) 
RIDE C   ( 217,X'S) H   (2173,X'S) H   (2172,X'S) H   (2171,X'S) 
RIDE C   ( 222,X'S) H   (2221,X'S) H   (2222,X'S) 
RIDE C   ( 223,X'S) H   (2231,X'S) H   (2232,X'S) 
RIDE C   ( 224,X'S) H   (2241,X'S) H   (2242,X'S) 
RIDE C   ( 225,X'S) H   (2253,X'S) H   (2252,X'S) H   (2251,X'S) 
RIDE C   ( 226,X'S) H   (2261,X'S) H   (2262,X'S) 
RIDE C   ( 227,X'S) H   (2271,X'S) H   (2272,X'S) 
RIDE C   ( 228,X'S) H   (2281,X'S) H   (2282,X'S) 
RIDE C   ( 229,X'S) H   (2291,X'S) H   (2292,X'S) H   (2293,X'S) 
RIDE C   ( 230,X'S) H   (2301,X'S) H   (2302,X'S) 
RIDE C   ( 231,X'S) H   (2311,X'S) H   (2312,X'S) 
RIDE C   ( 232,X'S) H   (2321,X'S) H   (2322,X'S) 
RIDE C   ( 233,X'S) H   (2331,X'S) H   (2332,X'S) H   (2333,X'S) 
RIDE C   ( 234,X'S) H   (2341,X'S) H   (2342,X'S) 
RIDE C   ( 235,X'S) H   (2351,X'S) H   (2352,X'S) 
RIDE C   ( 236,X'S) H   (2361,X'S) H   (2362,X'S) 
RIDE C   ( 237,X'S) H   (2373,X'S) H   (2372,X'S) H   (2371,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 25/04/13 at 19:05:31
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-3 0 1 x .
-5 0 5 x .
####################################################################### 
# 
# 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_2n
_database_code_depnum_ccdc_archive 'CCDC 1401778'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
#============================================================================
_audit_creation_date             2015-04-21
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title 013lp14
_chemical_name_systematic        .
_chemical_melting_point          '416 K'

_cell_length_a                   27.7157(6)
_cell_length_b                   9.7374(2)
_cell_length_c                   25.2072(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.664(2)
_cell_angle_gamma                90
_cell_volume                     6550.2(2)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c '
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
x,-y,z+1/2
-x,y,-z+1/2
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C46 H65 F1 N2 O2 
# Dc =      1.41 Fooo =   2488.00 Mu =      6.88 M =    697.03
# Found Formula = C38.00 H48.00 F0.50 N1.50 O2.50 
# Dc =      1.17 FOOO =   2488.00 Mu =      5.76 M =    575.31

_chemical_formula_sum            'C76 H96 F N3 O5'
_chemical_formula_moiety         '2(C30 H29 N O2), C16 H36 N, F, H2 O'
_chemical_compound_source        .
_chemical_formula_weight         1150.62


_cell_measurement_reflns_used    14243
_cell_measurement_theta_min      3
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.24

_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2488.000
_exptl_absorpt_coefficient_mu    0.576

# Sheldrick geometric approximatio 1.00 1.00 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_T_max  1.00
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            26899
_reflns_number_total             6786
_diffrn_reflns_av_R_equivalents  0.021
# Number of reflections with Friedels Law is 6786 
# Theoretical number of reflections is about 13674 


_diffrn_reflns_theta_min         3.312
_diffrn_reflns_theta_max         75.982
_diffrn_measured_fraction_theta_max 0.989

_diffrn_reflns_theta_full        74.463
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       23
_reflns_limit_h_min              -34
_reflns_limit_h_max              33
_reflns_limit_k_min              0
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              31

_oxford_diffrn_Wilson_B_factor   2.92
_oxford_diffrn_Wilson_scale      0.19

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.17
_refine_diff_density_max         0.94


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         6762
_refine_ls_number_restraints     950
_refine_ls_number_parameters     443
_oxford_refine_ls_R_factor_ref   0.0499
_refine_ls_wR_factor_ref         0.1351
_refine_ls_goodness_of_fit_ref   0.9935
_refine_ls_shift/su_max          0.0011275
_refine_ls_shift/su_mean         0.0000431


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6762
_refine_ls_R_factor_all          0.0499
_refine_ls_wR_factor_all         0.1351

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6179
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_gt          0.1322

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.08P)² + 5.66P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
F1 F 0.45229(13) 0.5999(3) 0.25239(15) 0.0405 0.5000 Uani . . . 1 -1 .
O101 O 0.45895(17) 0.6530(4) 0.2501(2) 0.0465 0.5000 Uani . . . 1 -2 .
O1 O 0.37449(3) 0.56255(9) 0.16975(4) 0.0288 1.0000 Uani . . . . . .
C11 C 0.32924(4) 0.63746(12) 0.16000(5) 0.0241 1.0000 Uani . . . . . .
C12 C 0.29100(4) 0.56363(13) 0.11301(5) 0.0257 1.0000 Uani . . . . . .
C13 C 0.24832(5) 0.62896(14) 0.08115(6) 0.0356 1.0000 Uani . . . . . .
C14 C 0.21211(6) 0.55626(16) 0.04246(7) 0.0420 1.0000 Uani . . . . . .
C15 C 0.21764(5) 0.41697(15) 0.03510(6) 0.0370 1.0000 Uani . . . . . .
C16 C 0.26043(6) 0.35169(14) 0.06574(5) 0.0349 1.0000 Uani . . . . . .
C17 C 0.29672(5) 0.42415(13) 0.10404(5) 0.0311 1.0000 Uani . . . . . .
C18 C 0.33708(4) 0.78629(13) 0.14438(5) 0.0243 1.0000 Uani . . . . . .
C19 C 0.37606(5) 0.81880(14) 0.12169(6) 0.0328 1.0000 Uani . . . . . .
C20 C 0.38230(6) 0.95204(15) 0.10498(7) 0.0420 1.0000 Uani . . . . . .
C21 C 0.35070(5) 1.05604(14) 0.11163(6) 0.0345 1.0000 Uani . . . . . .
C22 C 0.31243(5) 1.02594(14) 0.13482(6) 0.0341 1.0000 Uani . . . . . .
C23 C 0.30546(5) 0.89246(14) 0.15064(6) 0.0323 1.0000 Uani . . . . . .
C31 C 0.30827(4) 0.63211(12) 0.21123(5) 0.0244 1.0000 Uani . . . . . .
N32 N 0.34347(4) 0.69243(11) 0.25980(4) 0.0269 1.0000 Uani . . . . . .
C33 C 0.33213(4) 0.63933(13) 0.30991(5) 0.0260 1.0000 Uani . . . . . .
C34 C 0.29931(5) 0.51156(15) 0.29023(5) 0.0332 1.0000 Uani . . . . . .
C35 C 0.30134(5) 0.48761(13) 0.23094(5) 0.0287 1.0000 Uani . . . . . .
O2 O 0.41185(4) 0.52309(10) 0.33064(4) 0.0355 1.0000 Uani . . . . . .
C41 C 0.38150(4) 0.60742(13) 0.35429(5) 0.0266 1.0000 Uani D . . . . .
C42 C 0.37189(5) 0.52590(13) 0.40250(5) 0.0283 1.0000 Uani . . . . . .
C43 C 0.33121(5) 0.55450(16) 0.42311(6) 0.0362 1.0000 Uani . . . . . .
C44 C 0.32379(6) 0.48259(18) 0.46780(6) 0.0453 1.0000 Uani . . . . . .
C45 C 0.35686(8) 0.38256(17) 0.49283(6) 0.0509 1.0000 Uani . . . . . .
C46 C 0.39730(8) 0.35262(18) 0.47281(7) 0.0539 1.0000 Uani . . . . . .
C47 C 0.40481(6) 0.42348(15) 0.42774(6) 0.0405 1.0000 Uani . . . . . .
C48 C 0.41007(11) 0.7390(4) 0.3765(2) 0.0306 0.515(2) Uani D . P 2 1 .
C49 C 0.38879(16) 0.8397(5) 0.4022(2) 0.0371 0.515(2) Uani D . P 2 1 .
C50 C 0.4161(2) 0.9551(5) 0.4250(2) 0.0518 0.515(2) Uani D . P 2 1 .
C51 C 0.4643(2) 0.9711(5) 0.4236(2) 0.0577 0.515(2) Uani D . P 2 1 .
C52 C 0.48561(16) 0.8740(5) 0.39814(18) 0.0595 0.515(2) Uani D . P 2 1 .
C53 C 0.45893(14) 0.7579(5) 0.37494(17) 0.0446 0.515(2) Uani D . P 2 1 .
N61 N 0.0000 0.73586(16) 0.2500 0.0286 1.0000 Uani S T . . . .
C62 C 0.04163(5) 0.64042(14) 0.24474(6) 0.0335 1.0000 Uani . . . . . .
C63 C 0.08831(5) 0.70373(16) 0.23542(6) 0.0381 1.0000 Uani . . . . . .
C64 C 0.11961(6) 0.58686(17) 0.22116(7) 0.0428 1.0000 Uani . . . . . .
C65 C 0.16636(6) 0.6354(2) 0.20649(9) 0.0606 1.0000 Uani . . . . . .
C66 C 0.01664(5) 0.82998(13) 0.29982(5) 0.0296 1.0000 Uani . . . . . .
C67 C 0.02766(5) 0.76038(14) 0.35559(5) 0.0339 1.0000 Uani . . . . . .
C68 C 0.04923(6) 0.86323(15) 0.40129(6) 0.0369 1.0000 Uani . . . . . .
C69 C 0.05961(7) 0.79982(19) 0.45814(6) 0.0490 1.0000 Uani . . . . . .
C148 C 0.40806(11) 0.7402(4) 0.3798(2) 0.0306 0.485(2) Uani D . P 2 2 .
C149 C 0.38118(16) 0.8497(5) 0.3935(2) 0.0342 0.485(2) Uani D . P 2 2 .
C150 C 0.4058(2) 0.9661(5) 0.4193(2) 0.0438 0.485(2) Uani D . P 2 2 .
C151 C 0.4568(2) 0.9770(6) 0.4311(3) 0.0597 0.485(2) Uani D . P 2 2 .
C152 C 0.48385(18) 0.8698(6) 0.4183(2) 0.0654 0.485(2) Uani D . P 2 2 .
C153 C 0.45995(16) 0.7527(5) 0.3924(2) 0.0536 0.485(2) Uani D . P 2 2 .
H131 H 0.2438 0.7244 0.0854 0.0430 1.0000 Uiso R . . . . .
H141 H 0.1836 0.6054 0.0213 0.0502 1.0000 Uiso R . . . . .
H151 H 0.1925 0.3672 0.0083 0.0435 1.0000 Uiso R . . . . .
H161 H 0.2654 0.2554 0.0607 0.0410 1.0000 Uiso R . . . . .
H171 H 0.3259 0.3815 0.1253 0.0379 1.0000 Uiso R . . . . .
H191 H 0.3984 0.7474 0.1174 0.0395 1.0000 Uiso R . . . . .
H201 H 0.4088 0.9739 0.0887 0.0512 1.0000 Uiso R . . . . .
H211 H 0.3549 1.1488 0.1001 0.0420 1.0000 Uiso R . . . . .
H221 H 0.2901 1.0998 0.1401 0.0409 1.0000 Uiso R . . . . .
H231 H 0.2784 0.8758 0.1663 0.0377 1.0000 Uiso R . . . . .
H311 H 0.2755 0.6797 0.2026 0.0282 1.0000 Uiso R . . . . .
H331 H 0.3127 0.7057 0.3255 0.0307 1.0000 Uiso R . . . . .
H341 H 0.3110 0.4315 0.3136 0.0404 1.0000 Uiso R . . . . .
H342 H 0.2644 0.5335 0.2910 0.0395 1.0000 Uiso R . . . . .
H352 H 0.3310 0.4317 0.2305 0.0337 1.0000 Uiso R . . . . .
H351 H 0.2714 0.4460 0.2082 0.0337 1.0000 Uiso R . . . . .
H431 H 0.3076 0.6230 0.4063 0.0431 1.0000 Uiso R . . . . .
H441 H 0.2959 0.5025 0.4811 0.0543 1.0000 Uiso R . . . . .
H451 H 0.3520 0.3350 0.5237 0.0596 1.0000 Uiso R . . . . .
H461 H 0.4201 0.2841 0.4893 0.0650 1.0000 Uiso R . . . . .
H471 H 0.4321 0.4017 0.4140 0.0479 1.0000 Uiso R . . . . .
H491 H 0.3545 0.8282 0.4038 0.0423 0.515(2) Uiso R . P 2 1 .
H501 H 0.4002 1.0206 0.4412 0.0616 0.515(2) Uiso R . P 2 1 .
H511 H 0.4835 1.0469 0.4406 0.0743 0.515(2) Uiso R . P 2 1 .
H521 H 0.5195 0.8840 0.3980 0.0765 0.515(2) Uiso R . P 2 1 .
H531 H 0.4743 0.6900 0.3577 0.0572 0.515(2) Uiso R . P 2 1 .
H621 H 0.0501 0.5867 0.2789 0.0392 1.0000 Uiso R . . . . .
H622 H 0.0264 0.5813 0.2127 0.0393 1.0000 Uiso R . . . . .
H632 H 0.1071 0.7521 0.2688 0.0436 1.0000 Uiso R . . . . .
H631 H 0.0795 0.7698 0.2051 0.0455 1.0000 Uiso R . . . . .
H642 H 0.1289 0.5227 0.2528 0.0514 1.0000 Uiso R . . . . .
H641 H 0.0980 0.5392 0.1885 0.0516 1.0000 Uiso R . . . . .
H651 H 0.1853 0.5593 0.1962 0.0895 1.0000 Uiso R . . . . .
H653 H 0.1886 0.6851 0.2381 0.0895 1.0000 Uiso R . . . . .
H652 H 0.1565 0.6986 0.1756 0.0919 1.0000 Uiso R . . . . .
H661 H -0.0096 0.8970 0.2967 0.0350 1.0000 Uiso R . . . . .
H662 H 0.0459 0.8778 0.2957 0.0357 1.0000 Uiso R . . . . .
H672 H -0.0033 0.7182 0.3613 0.0411 1.0000 Uiso R . . . . .
H671 H 0.0517 0.6878 0.3570 0.0422 1.0000 Uiso R . . . . .
H681 H 0.0260 0.9394 0.3986 0.0454 1.0000 Uiso R . . . . .
H682 H 0.0803 0.9008 0.3954 0.0454 1.0000 Uiso R . . . . .
H692 H 0.0733 0.8709 0.4858 0.0722 1.0000 Uiso R . . . . .
H691 H 0.0289 0.7660 0.4658 0.0725 1.0000 Uiso R . . . . .
H693 H 0.0837 0.7246 0.4633 0.0733 1.0000 Uiso R . . . . .
H1491 H 0.3454 0.8466 0.3838 0.0410 0.485(2) Uiso R . P 2 2 .
H1501 H 0.3863 1.0389 0.4275 0.0519 0.485(2) Uiso R . P 2 2 .
H1511 H 0.4733 1.0569 0.4481 0.0692 0.485(2) Uiso R . P 2 2 .
H1521 H 0.5192 0.8723 0.4290 0.0710 0.485(2) Uiso R . P 2 2 .
H1531 H 0.4790 0.6799 0.3837 0.0587 0.485(2) Uiso R . P 2 2 .
H11 H 0.3954 0.5931 0.1979 0.0444 1.0000 Uiso R . . . . .
H321 H 0.3445 0.7800 0.2591 0.0337 1.0000 Uiso R . . . . .
H21 H 0.4180 0.5699 0.3051 0.0535 1.0000 Uiso R . . . . .
H1011 H 0.4592 0.7504 0.2482 0.0600 0.5000 Uiso R . . 1 -2 .
H1012 H 0.4924 0.6314 0.2501 0.0600 0.5000 Uiso R . . 1 -2 .

_refine_ls_extinction_coef       91(13)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          2.49(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O101 . H1011 . 0.950 no
O101 . H1012 . 0.950 no
O1 . C11 . 1.4139(13) yes
O1 . H11 . 0.840 no
C11 . C12 . 1.5379(17) yes
C11 . C18 . 1.5326(17) yes
C11 . C31 . 1.5535(15) yes
C12 . C13 . 1.3914(18) yes
C12 . C17 . 1.3929(18) yes
C13 . C14 . 1.389(2) yes
C13 . H131 . 0.948 no
C14 . C15 . 1.383(2) yes
C14 . H141 . 0.954 no
C15 . C16 . 1.383(2) yes
C15 . H151 . 0.961 no
C16 . C17 . 1.3846(19) yes
C16 . H161 . 0.962 no
C17 . H171 . 0.938 no
C18 . C19 . 1.3886(17) yes
C18 . C23 . 1.3914(17) yes
C19 . C20 . 1.389(2) yes
C19 . H191 . 0.957 no
C20 . C21 . 1.378(2) yes
C20 . H201 . 0.957 no
C21 . C22 . 1.374(2) yes
C21 . H211 . 0.966 no
C22 . C23 . 1.3882(19) yes
C22 . H221 . 0.981 no
C23 . H231 . 0.952 no
C31 . N32 . 1.4665(15) yes
C31 . C35 . 1.5215(17) yes
C31 . H311 . 0.990 no
N32 . C33 . 1.4752(14) yes
N32 . H321 . 0.854 no
C33 . C34 . 1.5421(17) yes
C33 . C41 . 1.5471(16) yes
C33 . H331 . 0.988 no
C34 . C35 . 1.5288(17) yes
C34 . H341 . 0.978 no
C34 . H342 . 0.997 no
C35 . H352 . 0.988 no
C35 . H351 . 0.962 no
O2 . C41 . 1.4169(14) yes
O2 . H21 . 0.843 no
C41 . C42 . 1.5338(16) yes
C41 . C48 . 1.531(4) yes
C41 . C42 . 1.5338(16) yes
C41 . C148 . 1.540(4) yes
C42 . C43 . 1.3909(19) yes
C42 . C47 . 1.385(2) yes
C43 . C44 . 1.388(2) yes
C43 . H431 . 0.950 no
C44 . C45 . 1.369(3) yes
C44 . H441 . 0.941 no
C45 . C46 . 1.379(3) yes
C45 . H451 . 0.946 no
C46 . C47 . 1.392(2) yes
C46 . H461 . 0.935 no
C47 . H471 . 0.938 no
C48 . C49 . 1.391(4) yes
C48 . C53 . 1.377(4) yes
C49 . C50 . 1.390(4) yes
C49 . H491 . 0.967 no
C50 . C51 . 1.357(4) yes
C50 . H501 . 0.929 no
C51 . C52 . 1.363(4) yes
C51 . H511 . 0.942 no
C52 . C53 . 1.391(4) yes
C52 . H521 . 0.946 no
C53 . H531 . 0.953 no
N61 . C66 6_555 1.5221(15) yes
N61 . C62 6_555 1.5149(16) yes
N61 . C62 . 1.5149(16) yes
N61 . C66 . 1.5221(15) yes
C62 . C63 . 1.508(2) yes
C62 . H621 . 0.981 no
C62 . H622 . 0.989 no
C63 . C64 . 1.531(2) yes
C63 . H632 . 0.983 no
C63 . H631 . 0.979 no
C64 . C65 . 1.516(2) yes
C64 . H642 . 0.991 no
C64 . H641 . 0.993 no
C65 . H651 . 0.982 no
C65 . H653 . 0.992 no
C65 . H652 . 0.972 no
C66 . C67 . 1.5156(18) yes
C66 . H661 . 0.963 no
C66 . H662 . 0.966 no
C67 . C68 . 1.5217(19) yes
C67 . H672 . 0.995 no
C67 . H671 . 0.965 no
C68 . C69 . 1.515(2) yes
C68 . H681 . 0.972 no
C68 . H682 . 0.983 no
C69 . H692 . 0.983 no
C69 . H691 . 0.978 no
C69 . H693 . 0.975 no
C148 . C149 . 1.397(4) yes
C148 . C153 . 1.392(4) yes
C149 . C150 . 1.390(4) yes
C149 . H1491 . 0.956 no
C150 . C151 . 1.369(4) yes
C150 . H1501 . 0.947 no
C151 . C152 . 1.373(4) yes
C151 . H1511 . 0.944 no
C152 . C153 . 1.390(4) yes
C152 . H1521 . 0.943 no
C153 . H1531 . 0.944 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
H1011 . O101 . H1012 . 101.6 no
C11 . O1 . H11 . 109.9 no
O1 . C11 . C12 . 106.69(9) yes
O1 . C11 . C18 . 110.60(9) yes
C12 . C11 . C18 . 111.11(9) yes
O1 . C11 . C31 . 110.59(9) yes
C12 . C11 . C31 . 106.85(9) yes
C18 . C11 . C31 . 110.86(9) yes
C11 . C12 . C13 . 122.18(11) yes
C11 . C12 . C17 . 119.73(11) yes
C13 . C12 . C17 . 117.93(12) yes
C12 . C13 . C14 . 120.83(13) yes
C12 . C13 . H131 . 120.1 no
C14 . C13 . H131 . 119.1 no
C13 . C14 . C15 . 120.57(13) yes
C13 . C14 . H141 . 118.0 no
C15 . C14 . H141 . 121.4 no
C14 . C15 . C16 . 119.02(13) yes
C14 . C15 . H151 . 120.2 no
C16 . C15 . H151 . 120.7 no
C15 . C16 . C17 . 120.47(13) yes
C15 . C16 . H161 . 120.4 no
C17 . C16 . H161 . 119.2 no
C12 . C17 . C16 . 121.13(12) yes
C12 . C17 . H171 . 117.2 no
C16 . C17 . H171 . 121.7 no
C11 . C18 . C19 . 120.10(11) yes
C11 . C18 . C23 . 122.42(10) yes
C19 . C18 . C23 . 117.46(12) yes
C18 . C19 . C20 . 120.81(12) yes
C18 . C19 . H191 . 118.8 no
C20 . C19 . H191 . 120.4 no
C19 . C20 . C21 . 120.94(13) yes
C19 . C20 . H201 . 120.7 no
C21 . C20 . H201 . 118.4 no
C20 . C21 . C22 . 118.94(13) yes
C20 . C21 . H211 . 121.2 no
C22 . C21 . H211 . 119.9 no
C21 . C22 . C23 . 120.34(12) yes
C21 . C22 . H221 . 119.3 no
C23 . C22 . H221 . 120.4 no
C18 . C23 . C22 . 121.49(12) yes
C18 . C23 . H231 . 120.8 no
C22 . C23 . H231 . 117.7 no
C11 . C31 . N32 . 111.51(9) yes
C11 . C31 . C35 . 114.26(10) yes
N32 . C31 . C35 . 102.24(9) yes
C11 . C31 . H311 . 109.2 no
N32 . C31 . H311 . 111.1 no
C35 . C31 . H311 . 108.4 no
C31 . N32 . C33 . 109.09(9) yes
C31 . N32 . H321 . 113.7 no
C33 . N32 . H321 . 112.7 no
N32 . C33 . C34 . 104.53(9) yes
N32 . C33 . C41 . 109.77(9) yes
C34 . C33 . C41 . 113.61(10) yes
N32 . C33 . H331 . 112.1 no
C34 . C33 . H331 . 108.6 no
C41 . C33 . H331 . 108.3 no
C33 . C34 . C35 . 105.27(10) yes
C33 . C34 . H341 . 112.3 no
C35 . C34 . H341 . 111.9 no
C33 . C34 . H342 . 108.2 no
C35 . C34 . H342 . 110.2 no
H341 . C34 . H342 . 108.9 no
C34 . C35 . C31 . 102.67(10) yes
C34 . C35 . H352 . 110.2 no
C31 . C35 . H352 . 109.1 no
C34 . C35 . H351 . 113.2 no
C31 . C35 . H351 . 111.1 no
H352 . C35 . H351 . 110.4 no
C41 . O2 . H21 . 105.9 no
C33 . C41 . O2 . 108.76(9) yes
C33 . C41 . C42 . 111.58(9) yes
O2 . C41 . C42 . 106.45(10) yes
C33 . C41 . C48 . 111.43(19) yes
O2 . C41 . C48 . 109.38(11) yes
C42 . C41 . C48 . 109.1(2) yes
C33 . C41 . O2 . 108.76(9) yes
C33 . C41 . C42 . 111.58(9) yes
O2 . C41 . C42 . 106.45(10) yes
C33 . C41 . C148 . 111.31(17) yes
O2 . C41 . C148 . 113.04(13) yes
C42 . C41 . C148 . 105.6(2) yes
C41 . C42 . C43 . 121.60(12) yes
C41 . C42 . C47 . 120.18(12) yes
C43 . C42 . C47 . 118.20(12) yes
C42 . C43 . C44 . 120.98(14) yes
C42 . C43 . H431 . 120.3 no
C44 . C43 . H431 . 118.7 no
C43 . C44 . C45 . 120.34(15) yes
C43 . C44 . H441 . 120.0 no
C45 . C44 . H441 . 119.6 no
C44 . C45 . C46 . 119.41(14) yes
C44 . C45 . H451 . 120.1 no
C46 . C45 . H451 . 120.5 no
C45 . C46 . C47 . 120.61(16) yes
C45 . C46 . H461 . 120.4 no
C47 . C46 . H461 . 119.0 no
C46 . C47 . C42 . 120.44(15) yes
C46 . C47 . H471 . 120.2 no
C42 . C47 . H471 . 119.4 no
C41 . C48 . C49 . 121.18(6) yes
C41 . C48 . C53 . 121.09(5) yes
C49 . C48 . C53 . 117.59(5) yes
C48 . C49 . C50 . 120.72(6) yes
C48 . C49 . H491 . 118.8 no
C50 . C49 . H491 . 120.4 no
C49 . C50 . C51 . 120.81(6) yes
C49 . C50 . H501 . 117.8 no
C51 . C50 . H501 . 121.4 no
C50 . C51 . C52 . 119.19(6) yes
C50 . C51 . H511 . 121.0 no
C52 . C51 . H511 . 119.8 no
C51 . C52 . C53 . 120.90(6) yes
C51 . C52 . H521 . 119.2 no
C53 . C52 . H521 . 119.8 no
C52 . C53 . C48 . 120.77(6) yes
C52 . C53 . H531 . 120.3 no
C48 . C53 . H531 . 119.0 no
C66 6_555 N61 . C62 6_555 111.92(7) yes
C66 6_555 N61 . C62 . 111.43(7) yes
C62 6_555 N61 . C62 . 104.32(14) yes
C66 6_555 N61 . C66 . 105.96(13) yes
C62 6_555 N61 . C66 . 111.43(7) yes
C62 . N61 . C66 . 111.92(7) yes
N61 . C62 . C63 . 117.95(12) yes
N61 . C62 . H621 . 105.0 no
C63 . C62 . H621 . 110.0 no
N61 . C62 . H622 . 105.2 no
C63 . C62 . H622 . 107.7 no
H621 . C62 . H622 . 110.9 no
C62 . C63 . C64 . 107.28(12) yes
C62 . C63 . H632 . 110.0 no
C64 . C63 . H632 . 110.7 no
C62 . C63 . H631 . 110.3 no
C64 . C63 . H631 . 110.1 no
H632 . C63 . H631 . 108.5 no
C63 . C64 . C65 . 113.65(14) yes
C63 . C64 . H642 . 108.7 no
C65 . C64 . H642 . 109.8 no
C63 . C64 . H641 . 106.8 no
C65 . C64 . H641 . 107.9 no
H642 . C64 . H641 . 110.0 no
C64 . C65 . H651 . 112.5 no
C64 . C65 . H653 . 110.0 no
H651 . C65 . H653 . 108.6 no
C64 . C65 . H652 . 108.7 no
H651 . C65 . H652 . 108.7 no
H653 . C65 . H652 . 108.3 no
N61 . C66 . C67 . 115.87(11) yes
N61 . C66 . H661 . 106.6 no
C67 . C66 . H661 . 109.8 no
N61 . C66 . H662 . 106.1 no
C67 . C66 . H662 . 110.5 no
H661 . C66 . H662 . 107.6 no
C66 . C67 . C68 . 110.34(11) yes
C66 . C67 . H672 . 110.6 no
C68 . C67 . H672 . 109.9 no
C66 . C67 . H671 . 109.1 no
C68 . C67 . H671 . 109.1 no
H672 . C67 . H671 . 107.7 no
C67 . C68 . C69 . 112.54(12) yes
C67 . C68 . H681 . 109.3 no
C69 . C68 . H681 . 109.3 no
C67 . C68 . H682 . 108.2 no
C69 . C68 . H682 . 110.1 no
H681 . C68 . H682 . 107.2 no
C68 . C69 . H692 . 108.8 no
C68 . C69 . H691 . 111.8 no
H692 . C69 . H691 . 106.6 no
C68 . C69 . H693 . 112.4 no
H692 . C69 . H693 . 108.4 no
H691 . C69 . H693 . 108.7 no
C41 . C148 . C149 . 121.19(5) yes
C41 . C148 . C153 . 121.13(6) yes
C149 . C148 . C153 . 117.62(5) yes
C148 . C149 . C150 . 120.75(6) yes
C148 . C149 . H1491 . 119.9 no
C150 . C149 . H1491 . 119.3 no
C149 . C150 . C151 . 120.82(6) yes
C149 . C150 . H1501 . 118.4 no
C151 . C150 . H1501 . 120.8 no
C150 . C151 . C152 . 119.19(6) yes
C150 . C151 . H1511 . 120.4 no
C152 . C151 . H1511 . 120.4 no
C151 . C152 . C153 . 120.85(6) yes
C151 . C152 . H1521 . 120.3 no
C153 . C152 . H1521 . 118.8 no
C148 . C153 . C152 . 120.75(6) yes
C148 . C153 . H1531 . 119.3 no
C152 . C153 . H1531 . 120.0 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O1 . H11 . O101 . 162.16 0.840 1.981 2.793(3) yes
O2 . H21 . O101 . 159.72 0.843 2.170 2.975(3) yes
O101 . H1012 . O101 6_655 158.34 0.950 1.368 2.278(3) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 21/04/15 at 00:52:00
#
#LIST     12                                                                    
BLOCK SCALE X'S U'S 
CONT EXTPARAM 
RIDE C(48,U'S) C(148,U'S) 
EQUIV PART(2001,OCC) PART(2002,OCC) 
WEIGHT -1 PART(2002,OCC) 
RIDE O   ( 101,X'S) H   (1012,X'S) H   (1011,X'S) 
RIDE O   (   1,X'S) H   (  11,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE N   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) 
RIDE O   (   2,X'S) H   (  21,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) 
RIDE C   (  63,X'S) H   ( 632,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 642,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) H   ( 653,X'S) H   ( 652,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 662,X'S) 
RIDE C   (  67,X'S) H   ( 672,X'S) H   ( 671,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) H   ( 682,X'S) 
RIDE C   (  69,X'S) H   ( 692,X'S) H   ( 691,X'S) H   ( 693,X'S) 
RIDE C   ( 149,X'S) H   (1491,X'S) 
RIDE C   ( 150,X'S) H   (1501,X'S) 
RIDE C   ( 151,X'S) H   (1511,X'S) 
RIDE C   ( 152,X'S) H   (1521,X'S) 
RIDE C   ( 153,X'S) H   (1531,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 21/04/15 at 00:52:00
#
#LIST     16                                                                    
SAME  C(41)  C(48)  C(49)  C(50)  C(51)  C(52)  C(53)  AND 
CONT  C(41)  C(48)  C(53)  C(52)  C(51)  C(50)  C(49)  AND 
CONT  C(41)  C(148)  C(149)  C(150)  C(151)  C(152)  C(153)  AND 
CONT  C(41)  C(148)  C(153)  C(152)  C(151)  C(150)  C(149) 
SIMU  0.01   C(41)  C(48)  C(49)  C(50)  C(51)  C(52)  C(53)  AND 
CONT  C(41)  C(48)  C(53)  C(52)  C(51)  C(50)  C(49)  AND 
CONT  C(41)  C(148)  C(149)  C(150)  C(151)  C(152)  C(153)  AND 
CONT  C(41)  C(148)  C(153)  C(152)  C(151)  C(150)  C(149) 
DELU  0.01  C(41)  C(48)  C(49)  C(50)  C(51)  C(52)  C(53)  AND 
CONT  C(41)  C(48)  C(53)  C(52)  C(51)  C(50)  C(49)  AND 
CONT  C(41)  C(148)  C(149)  C(150)  C(151)  C(152)  C(153)  AND 
CONT  C(41)  C(148)  C(153)  C(152)  C(151)  C(150)  C(149) 
PLANAR  C(41)  C(48)  C(49)  C(50)  C(51)  C(52)  C(53) 
PLANAR  C(41)  C(148)  C(149)  C(150)  C(151)  C(152)  C(153) 
END                                                                             
;


#============================================================================
# start Validation Reply Form
#============================================================================
_vrf_PLAT043_2f                  
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      15.97 Check
RESPONSE: PLATON/CheckCIF appears to be mis-calculating the occupancy 
for O44 which is located on a special position.  The author of the software 
has been contacted to discuss the issue.
;
_vrf_PLAT049_2g                  
;
PROBLEM: Calculated Density less than 1.0 gcm-3 .........     0.9994 Check  
RESPONSE: This appears to be an artefact of the structure rather than
an error.
;
_vrf_STRVA01_2i                  
;
PROBLEM:  Flack test results are ambiguous.
RESPONSE: The Flack x parameter was refined as part of the full-matrix 
least-squares indicating that the structure was twinned by inversion.
;
_vrf_PLAT601_2m                  
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 82 A**3 
RESPONSE: PLATON/SQUEEZE was used to evaluate the magnitude 
of the void space and the associated electron density.  However, 
refinement including the contributions to the A and B 
parts of the calculated structure factors determined by 
discrete Fourier transform of the electron density in the 
void region (using SQUEEZE) made minimal difference to the 
agreement factors and no perceptible change to the model 
so these were omitted for the final refinement.

See _refine_special_details for full details
;
_vrf_DIFMX01_2n                  
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00 
RESPONSE: This peak is close to the disordered fluoride/water
molecule and is thought to be an partially occupied disordered
water molecule.  Due to its close proximity to the water, 
PLATON/SQUEEZE has little/no effect so was not used.
;
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