# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_b
_database_code_depnum_ccdc_archive 'CCDC 1450418'
_audit_update_record             
;
2016-01-28 deposited with the CCDC.
2016-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'ciclesonide cyclohexane solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H50 O7'
_chemical_formula_weight         582.75
_chemical_absolute_configuration unk

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2

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'

_cell_length_a                   14.955(3)
_cell_length_b                   32.318(7)
_cell_length_c                   6.8184(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3295.5(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16588
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9802
_exptl_absorpt_correction_T_max  0.9881
_exptl_absorpt_process_details   ABSCOR

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'rigaku r-axis rapid IP'
_diffrn_measurement_method       oscillation
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27064
_diffrn_reflns_av_R_equivalents  0.1030
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         25.49
_reflns_number_total             6110
_reflns_number_gt                3839
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0650P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0135(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.6(16)
_refine_ls_number_reflns         6110
_refine_ls_number_parameters     350
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.0742
_refine_ls_wR_factor_ref         0.1654
_refine_ls_wR_factor_gt          0.1484
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O3 O 0.29937(16) 0.42571(6) 0.1994(3) 0.0470(6) Uani 1 1 d . . .
C9 C 0.4758(2) 0.30878(9) 0.3206(5) 0.0407(8) Uani 1 1 d . . .
H9A H 0.5166 0.3290 0.2615 0.049 Uiso 1 1 calc R . .
C12 C 0.3397(2) 0.34005(10) 0.1493(5) 0.0432(8) Uani 1 1 d . . .
H12A H 0.3708 0.3621 0.0813 0.052 Uiso 1 1 calc R . .
H12B H 0.2884 0.3323 0.0703 0.052 Uiso 1 1 calc R . .
O1 O 0.80021(18) 0.25604(9) 0.1744(4) 0.0740(8) Uani 1 1 d . . .
C11 C 0.4024(2) 0.30273(9) 0.1677(5) 0.0445(9) Uani 1 1 d . . .
H11A H 0.4320 0.2992 0.0406 0.053 Uiso 1 1 calc R . .
O2 O 0.35357(15) 0.26539(7) 0.2060(4) 0.0565(7) Uani 1 1 d . . .
H2A H 0.3342 0.2560 0.1026 0.085 Uiso 1 1 calc R . .
C5 C 0.6166(3) 0.28459(10) 0.4746(5) 0.0486(9) Uani 1 1 d . . .
O4 O 0.3219(2) 0.45833(7) 0.4843(4) 0.0680(8) Uani 1 1 d . . .
C13 C 0.3071(2) 0.35606(9) 0.3450(5) 0.0430(8) Uani 1 1 d . . .
C10 C 0.5362(2) 0.26949(10) 0.3626(5) 0.0446(8) Uani 1 1 d . . .
C17 C 0.2588(2) 0.39911(10) 0.3415(6) 0.0519(10) Uani 1 1 d . . .
C1 C 0.5648(3) 0.25013(10) 0.1701(6) 0.0513(9) Uani 1 1 d . . .
H1A H 0.5200 0.2403 0.0880 0.062 Uiso 1 1 calc R . .
C3 C 0.7220(3) 0.26056(11) 0.2284(6) 0.0556(10) Uani 1 1 d . . .
C14 C 0.3895(2) 0.36648(9) 0.4707(5) 0.0452(9) Uani 1 1 d . . .
H14A H 0.4269 0.3849 0.3913 0.054 Uiso 1 1 calc R . .
C7 C 0.5276(2) 0.34058(11) 0.6364(5) 0.0543(10) Uani 1 1 d . . .
H7A H 0.5582 0.3633 0.5722 0.065 Uiso 1 1 calc R . .
H7B H 0.5079 0.3503 0.7639 0.065 Uiso 1 1 calc R . .
C20 C 0.1589(3) 0.39729(11) 0.2998(7) 0.0614(11) Uani 1 1 d . . .
C4 C 0.7000(2) 0.28007(10) 0.4130(5) 0.0503(9) Uani 1 1 d . . .
H4A H 0.7463 0.2898 0.4916 0.060 Uiso 1 1 calc R . .
C16 C 0.2819(3) 0.41998(10) 0.5401(5) 0.0565(10) Uani 1 1 d . . .
H16A H 0.2290 0.4239 0.6228 0.068 Uiso 1 1 calc R . .
C22 C 0.2934(3) 0.46567(9) 0.2892(5) 0.0544(10) Uani 1 1 d . . .
H22A H 0.2311 0.4751 0.2891 0.065 Uiso 1 1 calc R . .
O6 O 0.0371(2) 0.39736(11) 0.0645(5) 0.0986(11) Uani 1 1 d . . .
C15 C 0.3530(3) 0.39274(11) 0.6398(5) 0.0563(10) Uani 1 1 d . . .
H15A H 0.3266 0.3755 0.7406 0.068 Uiso 1 1 calc R . .
H15B H 0.3999 0.4095 0.6980 0.068 Uiso 1 1 calc R . .
C8 C 0.4462(2) 0.32894(10) 0.5159(5) 0.0425(8) Uani 1 1 d . . .
H8A H 0.4102 0.3090 0.5901 0.051 Uiso 1 1 calc R . .
C6 C 0.5939(3) 0.30528(12) 0.6660(5) 0.0617(11) Uani 1 1 d . . .
H6A H 0.6481 0.3160 0.7253 0.074 Uiso 1 1 calc R . .
H6B H 0.5684 0.2850 0.7550 0.074 Uiso 1 1 calc R . .
O5 O 0.1041(2) 0.39376(9) 0.4303(5) 0.0858(10) Uani 1 1 d . . .
C2 C 0.6480(3) 0.24612(10) 0.1098(6) 0.0532(10) Uani 1 1 d . . .
H2B H 0.6594 0.2338 -0.0109 0.064 Uiso 1 1 calc R . .
C19 C 0.2437(2) 0.32501(10) 0.4490(6) 0.0587(11) Uani 1 1 d . . .
H19A H 0.2715 0.2983 0.4538 0.088 Uiso 1 1 calc R . .
H19B H 0.1885 0.3232 0.3776 0.088 Uiso 1 1 calc R . .
H19C H 0.2319 0.3344 0.5801 0.088 Uiso 1 1 calc R . .
C23 C 0.3509(3) 0.49688(10) 0.1883(6) 0.0595(10) Uani 1 1 d . . .
H23A H 0.4131 0.4875 0.1970 0.071 Uiso 1 1 calc R . .
C18 C 0.4907(3) 0.23518(11) 0.4786(6) 0.0643(11) Uani 1 1 d . . .
H18A H 0.5315 0.2125 0.4954 0.097 Uiso 1 1 calc R . .
H18B H 0.4388 0.2258 0.4087 0.097 Uiso 1 1 calc R . .
H18C H 0.4731 0.2456 0.6047 0.097 Uiso 1 1 calc R . .
C28 C 0.3270(4) 0.50026(15) -0.0227(6) 0.0992(18) Uani 1 1 d . . .
H28A H 0.2631 0.5050 -0.0341 0.119 Uiso 1 1 calc R . .
H28B H 0.3405 0.4743 -0.0873 0.119 Uiso 1 1 calc R . .
C21 C 0.1313(3) 0.40011(15) 0.0887(8) 0.0832(14) Uani 1 1 d . . .
H21A H 0.1521 0.4262 0.0349 0.100 Uiso 1 1 calc R . .
H21B H 0.1597 0.3780 0.0156 0.100 Uiso 1 1 calc R . .
O7 O 0.0519(3) 0.32965(12) 0.1135(7) 0.1241(14) Uani 1 1 d . . .
C24 C 0.3445(4) 0.53787(13) 0.2863(7) 0.1037(18) Uani 1 1 d . . .
H24A H 0.3685 0.5355 0.4181 0.124 Uiso 1 1 calc R . .
H24B H 0.2820 0.5455 0.2972 0.124 Uiso 1 1 calc R . .
C26 C 0.3650(5) 0.57575(16) -0.0241(9) 0.118(2) Uani 1 1 d . . .
H26A H 0.3997 0.5969 -0.0905 0.141 Uiso 1 1 calc R . .
H26B H 0.3025 0.5839 -0.0278 0.141 Uiso 1 1 calc R . .
C25 C 0.3944(5) 0.57219(14) 0.1786(9) 0.119(2) Uani 1 1 d . . .
H25A H 0.3843 0.5983 0.2455 0.143 Uiso 1 1 calc R . .
H25B H 0.4580 0.5664 0.1815 0.143 Uiso 1 1 calc R . .
C29 C 0.0051(4) 0.3591(3) 0.0871(9) 0.1051(19) Uani 1 1 d . . .
C30 C -0.0975(7) 0.3606(3) 0.0851(15) 0.184(3) Uiso 1 1 d . . .
H30A H -0.1007 0.3309 0.1123 0.221 Uiso 1 1 calc R . .
C27 C 0.3766(6) 0.53505(19) -0.1271(9) 0.154(3) Uani 1 1 d . . .
H27A H 0.4397 0.5283 -0.1335 0.185 Uiso 1 1 calc R . .
H27B H 0.3545 0.5374 -0.2604 0.185 Uiso 1 1 calc R . .
C32 C -0.1365(5) 0.3692(2) 0.2586(12) 0.161(3) Uiso 1 1 d . . .
H32A H -0.2003 0.3691 0.2432 0.242 Uiso 1 1 calc R . .
H32B H -0.1174 0.3960 0.3029 0.242 Uiso 1 1 calc R . .
H32C H -0.1196 0.3487 0.3532 0.242 Uiso 1 1 calc R . .
C31 C -0.1340(5) 0.3542(2) -0.1089(12) 0.163(3) Uiso 1 1 d . . .
H31A H -0.1981 0.3551 -0.1028 0.245 Uiso 1 1 calc R . .
H31B H -0.1152 0.3278 -0.1576 0.245 Uiso 1 1 calc R . .
H31C H -0.1130 0.3756 -0.1951 0.245 Uiso 1 1 calc R . .
C33 C 0.0439(5) 0.5089(3) 0.8112(11) 0.172(3) Uiso 1 1 d . . .
H33A H 0.0435 0.5321 0.9018 0.207 Uiso 1 1 calc R . .
H33B H 0.0850 0.4885 0.8633 0.207 Uiso 1 1 calc R . .
C35 C 0.0421(5) 0.5084(3) 0.4536(11) 0.164(3) Uiso 1 1 d . . .
H35A H 0.0826 0.4876 0.4023 0.197 Uiso 1 1 calc R . .
H35B H 0.0420 0.5312 0.3609 0.197 Uiso 1 1 calc R . .
C34 C 0.0788(7) 0.5232(3) 0.6299(15) 0.203(4) Uiso 1 1 d . . .
H34A H 0.1422 0.5168 0.6284 0.244 Uiso 1 1 calc R . .
H34B H 0.0735 0.5531 0.6288 0.244 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O3 C22 1.432(4) . ?
O3 C17 1.431(4) . ?
C9 C11 1.527(5) . ?
C9 C8 1.547(4) . ?
C9 C10 1.584(4) . ?
C9 H9A 0.9800 . ?
C12 C13 1.512(5) . ?
C12 C11 1.533(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
O1 C3 1.235(4) . ?
C11 O2 1.434(4) . ?
C11 H11A 0.9800 . ?
O2 H2A 0.8200 . ?
C5 C4 1.325(5) . ?
C5 C6 1.505(5) . ?
C5 C10 1.506(5) . ?
O4 C22 1.417(4) . ?
O4 C16 1.428(4) . ?
C13 C14 1.539(5) . ?
C13 C19 1.552(5) . ?
C13 C17 1.568(4) . ?
C10 C1 1.515(5) . ?
C10 C18 1.523(5) . ?
C17 C20 1.522(5) . ?
C17 C16 1.552(5) . ?
C1 C2 1.316(5) . ?
C1 H1A 0.9300 . ?
C3 C2 1.448(5) . ?
C3 C4 1.446(5) . ?
C14 C8 1.511(4) . ?
C14 C15 1.532(5) . ?
C14 H14A 0.9800 . ?
C7 C6 1.525(5) . ?
C7 C8 1.517(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C20 O5 1.215(5) . ?
C20 C21 1.500(6) . ?
C4 H4A 0.9300 . ?
C16 C15 1.539(5) . ?
C16 H16A 0.9800 . ?
C22 C23 1.493(5) . ?
C22 H22A 0.9800 . ?
O6 C29 1.334(7) . ?
O6 C21 1.422(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C8 H8A 0.9800 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C2 H2B 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C23 C24 1.487(6) . ?
C23 C28 1.486(5) . ?
C23 H23A 0.9800 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C28 C27 1.524(7) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
O7 C29 1.195(7) . ?
C24 C25 1.525(7) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C26 C25 1.455(7) . ?
C26 C27 1.501(8) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C29 C30 1.536(10) . ?
C30 C32 1.348(10) . ?
C30 C31 1.446(10) . ?
C30 H30A 0.9800 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C33 C34 1.419(10) . ?
C33 C33 1.434(15) 2_565 ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C35 C34 1.406(10) . ?
C35 C35 1.371(14) 2_565 ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C22 O3 C17 103.1(2) . . ?
C11 C9 C8 115.8(3) . . ?
C11 C9 C10 115.5(2) . . ?
C8 C9 C10 110.2(3) . . ?
C11 C9 H9A 104.6 . . ?
C8 C9 H9A 104.6 . . ?
C10 C9 H9A 104.6 . . ?
C13 C12 C11 113.2(3) . . ?
C13 C12 H12A 108.9 . . ?
C11 C12 H12A 108.9 . . ?
C13 C12 H12B 108.9 . . ?
C11 C12 H12B 108.9 . . ?
H12A C12 H12B 107.8 . . ?
O2 C11 C9 110.5(3) . . ?
O2 C11 C12 111.5(3) . . ?
C9 C11 C12 113.3(3) . . ?
O2 C11 H11A 107.1 . . ?
C9 C11 H11A 107.1 . . ?
C12 C11 H11A 107.1 . . ?
C11 O2 H2A 109.5 . . ?
C4 C5 C6 122.4(3) . . ?
C4 C5 C10 123.8(3) . . ?
C6 C5 C10 113.8(3) . . ?
C22 O4 C16 105.6(3) . . ?
C12 C13 C14 108.0(3) . . ?
C12 C13 C19 112.3(3) . . ?
C14 C13 C19 112.1(3) . . ?
C12 C13 C17 116.0(3) . . ?
C14 C13 C17 100.6(2) . . ?
C19 C13 C17 107.4(3) . . ?
C1 C10 C5 110.3(3) . . ?
C1 C10 C18 106.0(3) . . ?
C5 C10 C18 109.2(3) . . ?
C1 C10 C9 109.6(3) . . ?
C5 C10 C9 106.7(3) . . ?
C18 C10 C9 115.0(3) . . ?
O3 C17 C20 108.3(3) . . ?
O3 C17 C16 103.6(3) . . ?
C20 C17 C16 113.5(3) . . ?
O3 C17 C13 110.3(3) . . ?
C20 C17 C13 114.9(3) . . ?
C16 C17 C13 105.6(3) . . ?
C2 C1 C10 125.4(3) . . ?
C2 C1 H1A 117.3 . . ?
C10 C1 H1A 117.3 . . ?
O1 C3 C2 121.3(4) . . ?
O1 C3 C4 121.7(4) . . ?
C2 C3 C4 117.0(3) . . ?
C8 C14 C13 112.8(2) . . ?
C8 C14 C15 119.4(3) . . ?
C13 C14 C15 104.8(3) . . ?
C8 C14 H14A 106.4 . . ?
C13 C14 H14A 106.4 . . ?
C15 C14 H14A 106.4 . . ?
C6 C7 C8 114.1(3) . . ?
C6 C7 H7A 108.7 . . ?
C8 C7 H7A 108.7 . . ?
C6 C7 H7B 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
O5 C20 C21 121.5(4) . . ?
O5 C20 C17 121.9(4) . . ?
C21 C20 C17 116.5(4) . . ?
C5 C4 C3 122.5(3) . . ?
C5 C4 H4A 118.7 . . ?
C3 C4 H4A 118.7 . . ?
O4 C16 C15 108.9(3) . . ?
O4 C16 C17 103.8(3) . . ?
C15 C16 C17 106.9(3) . . ?
O4 C16 H16A 112.2 . . ?
C15 C16 H16A 112.2 . . ?
C17 C16 H16A 112.2 . . ?
O4 C22 O3 103.4(3) . . ?
O4 C22 C23 111.9(3) . . ?
O3 C22 C23 112.1(3) . . ?
O4 C22 H22A 109.8 . . ?
O3 C22 H22A 109.8 . . ?
C23 C22 H22A 109.8 . . ?
C29 O6 C21 113.6(4) . . ?
C16 C15 C14 103.3(3) . . ?
C16 C15 H15A 111.1 . . ?
C14 C15 H15A 111.1 . . ?
C16 C15 H15B 111.1 . . ?
C14 C15 H15B 111.1 . . ?
H15A C15 H15B 109.1 . . ?
C14 C8 C7 111.2(3) . . ?
C14 C8 C9 108.8(3) . . ?
C7 C8 C9 109.9(3) . . ?
C14 C8 H8A 108.9 . . ?
C7 C8 H8A 108.9 . . ?
C9 C8 H8A 108.9 . . ?
C5 C6 C7 111.4(3) . . ?
C5 C6 H6A 109.4 . . ?
C7 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
C7 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C1 C2 C3 121.0(4) . . ?
C1 C2 H2B 119.5 . . ?
C3 C2 H2B 119.5 . . ?
C13 C19 H19A 109.5 . . ?
C13 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C13 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C24 C23 C28 110.7(4) . . ?
C24 C23 C22 111.0(3) . . ?
C28 C23 C22 110.9(4) . . ?
C24 C23 H23A 108.0 . . ?
C28 C23 H23A 108.0 . . ?
C22 C23 H23A 108.0 . . ?
C10 C18 H18A 109.5 . . ?
C10 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C10 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C23 C28 C27 112.9(4) . . ?
C23 C28 H28A 109.0 . . ?
C27 C28 H28A 109.0 . . ?
C23 C28 H28B 109.0 . . ?
C27 C28 H28B 109.0 . . ?
H28A C28 H28B 107.8 . . ?
O6 C21 C20 112.3(4) . . ?
O6 C21 H21A 109.1 . . ?
C20 C21 H21A 109.1 . . ?
O6 C21 H21B 109.1 . . ?
C20 C21 H21B 109.1 . . ?
H21A C21 H21B 107.9 . . ?
C23 C24 C25 113.6(4) . . ?
C23 C24 H24A 108.8 . . ?
C25 C24 H24A 108.8 . . ?
C23 C24 H24B 108.8 . . ?
C25 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
C25 C26 C27 109.9(5) . . ?
C25 C26 H26A 109.7 . . ?
C27 C26 H26A 109.7 . . ?
C25 C26 H26B 109.7 . . ?
C27 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
C26 C25 C24 111.5(5) . . ?
C26 C25 H25A 109.3 . . ?
C24 C25 H25A 109.3 . . ?
C26 C25 H25B 109.3 . . ?
C24 C25 H25B 109.3 . . ?
H25A C25 H25B 108.0 . . ?
O7 C29 O6 123.1(5) . . ?
O7 C29 C30 127.7(7) . . ?
O6 C29 C30 109.1(7) . . ?
C32 C30 C31 132.0(9) . . ?
C32 C30 C29 115.5(8) . . ?
C31 C30 C29 112.4(8) . . ?
C32 C30 H30A 90.9 . . ?
C31 C30 H30A 90.9 . . ?
C29 C30 H30A 90.9 . . ?
C26 C27 C28 111.8(5) . . ?
C26 C27 H27A 109.3 . . ?
C28 C27 H27A 109.3 . . ?
C26 C27 H27B 109.3 . . ?
C28 C27 H27B 109.3 . . ?
H27A C27 H27B 107.9 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C34 C33 C33 117.9(6) . 2_565 ?
C34 C33 H33A 107.8 . . ?
C33 C33 H33A 107.8 2_565 . ?
C34 C33 H33B 107.8 . . ?
C33 C33 H33B 107.8 2_565 . ?
H33A C33 H33B 107.2 . . ?
C34 C35 C35 119.6(5) . 2_565 ?
C34 C35 H35A 107.4 . . ?
C35 C35 H35A 107.4 2_565 . ?
C34 C35 H35B 107.4 . . ?
C35 C35 H35B 107.4 2_565 . ?
H35A C35 H35B 107.0 . . ?
C33 C34 C35 119.4(8) . . ?
C33 C34 H34A 107.5 . . ?
C35 C34 H34A 107.5 . . ?
C33 C34 H34B 107.5 . . ?
C35 C34 H34B 107.5 . . ?
H34A C34 H34B 107.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 C9 C11 O2 -83.2(3) . . . . ?
C10 C9 C11 O2 47.8(4) . . . . ?
C8 C9 C11 C12 42.7(4) . . . . ?
C10 C9 C11 C12 173.7(3) . . . . ?
C13 C12 C11 O2 77.8(3) . . . . ?
C13 C12 C11 C9 -47.5(4) . . . . ?
C11 C12 C13 C14 56.3(3) . . . . ?
C11 C12 C13 C19 -67.8(4) . . . . ?
C11 C12 C13 C17 168.2(3) . . . . ?
C4 C5 C10 C1 -1.9(5) . . . . ?
C6 C5 C10 C1 178.6(3) . . . . ?
C4 C5 C10 C18 114.2(4) . . . . ?
C6 C5 C10 C18 -65.3(4) . . . . ?
C4 C5 C10 C9 -120.9(3) . . . . ?
C6 C5 C10 C9 59.6(4) . . . . ?
C11 C9 C10 C1 46.5(4) . . . . ?
C8 C9 C10 C1 -179.9(3) . . . . ?
C11 C9 C10 C5 165.9(3) . . . . ?
C8 C9 C10 C5 -60.4(3) . . . . ?
C11 C9 C10 C18 -72.8(4) . . . . ?
C8 C9 C10 C18 60.8(4) . . . . ?
C22 O3 C17 C20 88.9(3) . . . . ?
C22 O3 C17 C16 -31.9(3) . . . . ?
C22 O3 C17 C13 -144.5(3) . . . . ?
C12 C13 C17 O3 -36.0(4) . . . . ?
C14 C13 C17 O3 80.1(3) . . . . ?
C19 C13 C17 O3 -162.5(3) . . . . ?
C12 C13 C17 C20 86.7(4) . . . . ?
C14 C13 C17 C20 -157.2(3) . . . . ?
C19 C13 C17 C20 -39.8(4) . . . . ?
C12 C13 C17 C16 -147.4(3) . . . . ?
C14 C13 C17 C16 -31.2(3) . . . . ?
C19 C13 C17 C16 86.1(3) . . . . ?
C5 C10 C1 C2 1.4(5) . . . . ?
C18 C10 C1 C2 -116.8(4) . . . . ?
C9 C10 C1 C2 118.5(4) . . . . ?
C12 C13 C14 C8 -63.3(3) . . . . ?
C19 C13 C14 C8 60.9(4) . . . . ?
C17 C13 C14 C8 174.7(3) . . . . ?
C12 C13 C14 C15 165.4(2) . . . . ?
C19 C13 C14 C15 -70.5(3) . . . . ?
C17 C13 C14 C15 43.4(3) . . . . ?
O3 C17 C20 O5 -146.6(3) . . . . ?
C16 C17 C20 O5 -32.2(5) . . . . ?
C13 C17 C20 O5 89.5(4) . . . . ?
O3 C17 C20 C21 33.3(4) . . . . ?
C16 C17 C20 C21 147.8(3) . . . . ?
C13 C17 C20 C21 -90.5(4) . . . . ?
C6 C5 C4 C3 -179.4(3) . . . . ?
C10 C5 C4 C3 1.1(5) . . . . ?
O1 C3 C4 C5 -178.9(4) . . . . ?
C2 C3 C4 C5 0.5(5) . . . . ?
C22 O4 C16 C15 133.8(3) . . . . ?
C22 O4 C16 C17 20.2(4) . . . . ?
O3 C17 C16 O4 7.5(3) . . . . ?
C20 C17 C16 O4 -109.7(3) . . . . ?
C13 C17 C16 O4 123.5(3) . . . . ?
O3 C17 C16 C15 -107.6(3) . . . . ?
C20 C17 C16 C15 135.2(3) . . . . ?
C13 C17 C16 C15 8.5(4) . . . . ?
C16 O4 C22 O3 -41.2(4) . . . . ?
C16 O4 C22 C23 -162.0(3) . . . . ?
C17 O3 C22 O4 45.8(3) . . . . ?
C17 O3 C22 C23 166.4(3) . . . . ?
O4 C16 C15 C14 -93.5(3) . . . . ?
C17 C16 C15 C14 18.1(4) . . . . ?
C8 C14 C15 C16 -166.2(3) . . . . ?
C13 C14 C15 C16 -38.8(3) . . . . ?
C13 C14 C8 C7 178.9(3) . . . . ?
C15 C14 C8 C7 -57.5(4) . . . . ?
C13 C14 C8 C9 57.6(4) . . . . ?
C15 C14 C8 C9 -178.7(3) . . . . ?
C6 C7 C8 C14 -172.8(3) . . . . ?
C6 C7 C8 C9 -52.2(4) . . . . ?
C11 C9 C8 C14 -47.1(4) . . . . ?
C10 C9 C8 C14 179.5(3) . . . . ?
C11 C9 C8 C7 -169.1(3) . . . . ?
C10 C9 C8 C7 57.5(3) . . . . ?
C4 C5 C6 C7 125.6(4) . . . . ?
C10 C5 C6 C7 -54.8(4) . . . . ?
C8 C7 C6 C5 49.9(4) . . . . ?
C10 C1 C2 C3 0.0(6) . . . . ?
O1 C3 C2 C1 178.4(3) . . . . ?
C4 C3 C2 C1 -1.0(5) . . . . ?
O4 C22 C23 C24 -63.5(4) . . . . ?
O3 C22 C23 C24 -179.1(4) . . . . ?
O4 C22 C23 C28 173.0(4) . . . . ?
O3 C22 C23 C28 57.3(5) . . . . ?
C24 C23 C28 C27 49.9(7) . . . . ?
C22 C23 C28 C27 173.7(5) . . . . ?
C29 O6 C21 C20 -74.9(6) . . . . ?
O5 C20 C21 O6 -1.1(6) . . . . ?
C17 C20 C21 O6 178.9(3) . . . . ?
C28 C23 C24 C25 -50.6(7) . . . . ?
C22 C23 C24 C25 -174.3(5) . . . . ?
C27 C26 C25 C24 -56.7(8) . . . . ?
C23 C24 C25 C26 55.4(8) . . . . ?
C21 O6 C29 O7 -4.3(9) . . . . ?
C21 O6 C29 C30 172.6(6) . . . . ?
O7 C29 C30 C32 91.7(11) . . . . ?
O6 C29 C30 C32 -84.9(9) . . . . ?
O7 C29 C30 C31 -90.9(10) . . . . ?
O6 C29 C30 C31 92.4(8) . . . . ?
C25 C26 C27 C28 56.5(8) . . . . ?
C23 C28 C27 C26 -53.8(8) . . . . ?
C33 C33 C34 C35 -19.8(16) 2_565 . . . ?
C35 C35 C34 C33 20.6(16) 2_565 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2A O1 0.82 1.99 2.801(4) 167.5 4_455

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.043
####################################################################### 
# 
# 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_b
_database_code_depnum_ccdc_archive 'CCDC 1450419'
_audit_update_record             
;
2016-01-28 deposited with the CCDC.
2016-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'ciclesonide methanol solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H48 O8'
_chemical_formula_weight         572.71

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

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4(3)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+3/4'
'y, -x, z+1/4'

_cell_length_a                   11.0007(11)
_cell_length_b                   11.0007(11)
_cell_length_c                   25.559(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3093.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    386(2)
_cell_measurement_reflns_used    10369
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1240
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9787
_exptl_absorpt_correction_T_max  0.9871
_exptl_absorpt_process_details   ABSCOR

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      386(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'rigaku r-axis rapid IP'
_diffrn_measurement_method       oscillation
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27929
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         25.49
_reflns_number_total             5727
_reflns_number_gt                5511
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0900P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(6)
_refine_ls_number_reflns         5727
_refine_ls_number_parameters     386
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.1034
_refine_ls_wR_factor_gt          0.1011
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.127
_refine_ls_shift/su_mean         0.004

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 1.16123(11) 0.89973(13) 0.06634(5) 0.0337(3) Uani 1 1 d . . .
O2 O 0.56026(10) 1.01253(10) 0.08385(4) 0.0243(2) Uani 1 1 d . . .
H2A H 0.5520 0.9951 0.1148 0.036 Uiso 1 1 calc R . .
O6 O 0.13943(10) 0.64631(10) 0.01197(5) 0.0231(2) Uani 1 1 d . . .
O7 O 0.10808(11) 0.56298(12) -0.06699(5) 0.0302(3) Uani 1 1 d . . .
O5 O 0.18884(10) 0.82639(10) -0.05689(5) 0.0241(2) Uani 1 1 d . . .
O4 O 0.46473(11) 0.75894(10) -0.14455(4) 0.0232(2) Uani 1 1 d . . .
O3 O 0.47233(9) 0.68876(9) -0.06175(4) 0.0171(2) Uani 1 1 d . . .
O8 O 1.21375(19) 0.71047(16) 0.13503(8) 0.0620(5) Uani 1 1 d . . .
C4 C 1.02673(14) 1.01405(14) 0.01377(6) 0.0217(3) Uani 1 1 d . . .
H4A H 1.0856 1.0261 -0.0118 0.026 Uiso 1 1 calc R . .
C3 C 1.05932(14) 0.94663(14) 0.06095(7) 0.0231(3) Uani 1 1 d . . .
C2 C 0.96729(14) 0.93673(15) 0.10165(6) 0.0223(3) Uani 1 1 d . . .
H2B H 0.9858 0.8965 0.1327 0.027 Uiso 1 1 calc R . .
C1 C 0.85671(14) 0.98446(13) 0.09516(6) 0.0202(3) Uani 1 1 d . . .
H1A H 0.8021 0.9789 0.1228 0.024 Uiso 1 1 calc R . .
C10 C 0.81498(13) 1.04628(13) 0.04627(6) 0.0180(3) Uani 1 1 d . . .
C18 C 0.76820(15) 1.17451(13) 0.06164(7) 0.0232(3) Uani 1 1 d . . .
H18A H 0.8329 1.2198 0.0776 0.035 Uiso 1 1 calc R . .
H18B H 0.7021 1.1667 0.0859 0.035 Uiso 1 1 calc R . .
H18C H 0.7406 1.2164 0.0309 0.035 Uiso 1 1 calc R . .
C5 C 0.91511(13) 1.05918(13) 0.00610(6) 0.0183(3) Uani 1 1 d . . .
C6 C 0.87670(14) 1.11625(13) -0.04465(6) 0.0202(3) Uani 1 1 d . . .
H6A H 0.9455 1.1199 -0.0683 0.024 Uiso 1 1 calc R . .
H6B H 0.8488 1.1986 -0.0384 0.024 Uiso 1 1 calc R . .
C7 C 0.77454(14) 1.04181(13) -0.06950(6) 0.0192(3) Uani 1 1 d . . .
H7A H 0.8074 0.9646 -0.0812 0.023 Uiso 1 1 calc R . .
H7B H 0.7446 1.0847 -0.1000 0.023 Uiso 1 1 calc R . .
C8 C 0.66790(13) 1.01745(13) -0.03240(6) 0.0164(3) Uani 1 1 d . . .
H8A H 0.6247 1.0936 -0.0252 0.020 Uiso 1 1 calc R . .
C9 C 0.71572(13) 0.96274(13) 0.01949(6) 0.0163(3) Uani 1 1 d . . .
H9A H 0.7608 0.8901 0.0087 0.020 Uiso 1 1 calc R . .
C11 C 0.61840(13) 0.91429(13) 0.05724(6) 0.0181(3) Uani 1 1 d . . .
H11A H 0.6597 0.8646 0.0836 0.022 Uiso 1 1 calc R . .
C12 C 0.52549(13) 0.83273(14) 0.02927(6) 0.0178(3) Uani 1 1 d . . .
H12A H 0.5640 0.7561 0.0204 0.021 Uiso 1 1 calc R . .
H12B H 0.4589 0.8155 0.0530 0.021 Uiso 1 1 calc R . .
C13 C 0.47465(13) 0.89010(13) -0.02049(5) 0.0168(3) Uani 1 1 d . . .
C19 C 0.38988(14) 0.99842(14) -0.00873(6) 0.0209(3) Uani 1 1 d . . .
H19A H 0.4305 1.0545 0.0141 0.031 Uiso 1 1 calc R . .
H19B H 0.3172 0.9694 0.0079 0.031 Uiso 1 1 calc R . .
H19C H 0.3692 1.0387 -0.0408 0.031 Uiso 1 1 calc R . .
C14 C 0.58089(13) 0.92591(13) -0.05666(6) 0.0169(3) Uani 1 1 d . . .
H14A H 0.6280 0.8517 -0.0628 0.020 Uiso 1 1 calc R . .
C15 C 0.51734(13) 0.95663(14) -0.10855(6) 0.0194(3) Uani 1 1 d . . .
H15A H 0.4809 1.0369 -0.1074 0.023 Uiso 1 1 calc R . .
H15B H 0.5739 0.9530 -0.1376 0.023 Uiso 1 1 calc R . .
C16 C 0.42019(14) 0.85782(13) -0.11306(6) 0.0183(3) Uani 1 1 d . . .
H16A H 0.3430 0.8900 -0.1263 0.022 Uiso 1 1 calc R . .
C17 C 0.40656(13) 0.80081(13) -0.05755(6) 0.0171(3) Uani 1 1 d . . .
C20 C 0.27607(13) 0.77175(13) -0.04086(6) 0.0178(3) Uani 1 1 d . . .
C21 C 0.26369(14) 0.66694(15) -0.00276(7) 0.0250(3) Uani 1 1 d . . .
H21A H 0.2962 0.5938 -0.0187 0.030 Uiso 1 1 calc R . .
H21B H 0.3112 0.6842 0.0283 0.030 Uiso 1 1 calc R . .
C29 C 0.07066(14) 0.59270(14) -0.02457(6) 0.0220(3) Uani 1 1 d . . .
C30 C -0.05776(14) 0.57482(14) -0.00547(6) 0.0223(3) Uani 1 1 d . . .
H30A H -0.0631 0.6002 0.0312 0.027 Uiso 1 1 calc R . .
C32 C -0.14467(19) 0.6523(2) -0.03835(9) 0.0436(5) Uani 1 1 d . . .
H32A H -0.1227 0.7364 -0.0352 0.065 Uiso 1 1 calc R . .
H32B H -0.2264 0.6410 -0.0261 0.065 Uiso 1 1 calc R . .
H32C H -0.1394 0.6280 -0.0744 0.065 Uiso 1 1 calc R . .
C31 C -0.09034(18) 0.44181(17) -0.00956(9) 0.0385(4) Uani 1 1 d . . .
H31A H -0.0351 0.3948 0.0113 0.058 Uiso 1 1 calc R . .
H31B H -0.0849 0.4164 -0.0454 0.058 Uiso 1 1 calc R . .
H31C H -0.1718 0.4297 0.0028 0.058 Uiso 1 1 calc R . .
C22 C 0.45657(14) 0.65100(13) -0.11450(6) 0.0188(3) Uani 1 1 d . . .
H22A H 0.3760 0.6144 -0.1189 0.023 Uiso 1 1 calc R . .
C23 C 0.55320(14) 0.56108(14) -0.12975(6) 0.0195(3) Uani 1 1 d . . .
H23A H 0.6326 0.5987 -0.1234 0.023 Uiso 1 1 calc R . .
C28 C 0.54454(17) 0.44649(15) -0.09591(7) 0.0282(4) Uani 1 1 d . . .
H28A H 0.5558 0.4684 -0.0595 0.034 Uiso 1 1 calc R . .
H28B H 0.4641 0.4114 -0.0996 0.034 Uiso 1 1 calc R . .
C27 C 0.6396(2) 0.35230(17) -0.11139(8) 0.0375(4) Uani 1 1 d . . .
H27A H 0.7201 0.3840 -0.1041 0.045 Uiso 1 1 calc R . .
H27B H 0.6284 0.2794 -0.0906 0.045 Uiso 1 1 calc R . .
C26 C 0.6299(2) 0.32054(18) -0.16903(8) 0.0412(5) Uani 1 1 d . . .
H26A H 0.5522 0.2818 -0.1757 0.049 Uiso 1 1 calc R . .
H26B H 0.6937 0.2636 -0.1783 0.049 Uiso 1 1 calc R . .
C25 C 0.6412(2) 0.43433(18) -0.20240(8) 0.0412(5) Uani 1 1 d . . .
H25A H 0.6323 0.4127 -0.2390 0.049 Uiso 1 1 calc R . .
H25B H 0.7215 0.4691 -0.1977 0.049 Uiso 1 1 calc R . .
C24 C 0.54510(17) 0.52911(16) -0.18790(7) 0.0293(4) Uani 1 1 d . . .
H24A H 0.5572 0.6019 -0.2087 0.035 Uiso 1 1 calc R . .
H24B H 0.4648 0.4974 -0.1957 0.035 Uiso 1 1 calc R . .
C33 C 1.2744(3) 0.7769(3) 0.17422(12) 0.0546(6) Uani 1 1 d . . .
H8B H 1.191(2) 0.771(2) 0.1073(10) 0.042(6) Uiso 1 1 d . . .
H33A H 1.312(5) 0.752(5) 0.203(3) 0.16(2) Uiso 1 1 d . . .
H33B H 1.236(4) 0.859(4) 0.190(2) 0.121(15) Uiso 1 1 d . . .
H33C H 1.344(5) 0.812(4) 0.157(2) 0.138(17) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C3 1.242(2) . ?
O2 C11 1.4282(18) . ?
O2 H2A 0.8200 . ?
O6 C29 1.339(2) . ?
O6 C21 1.4359(19) . ?
O7 C29 1.205(2) . ?
O5 C20 1.2042(19) . ?
O4 C22 1.4170(18) . ?
O4 C16 1.4389(18) . ?
O3 C22 1.4215(18) . ?
O3 C17 1.4333(17) . ?
O8 C33 1.408(3) . ?
O8 H8B 1.00(3) . ?
C4 C5 1.339(2) . ?
C4 C3 1.460(2) . ?
C4 H4A 0.9300 . ?
C3 C2 1.456(2) . ?
C2 C1 1.335(2) . ?
C2 H2B 0.9300 . ?
C1 C10 1.495(2) . ?
C1 H1A 0.9300 . ?
C10 C5 1.512(2) . ?
C10 C18 1.552(2) . ?
C10 C9 1.583(2) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C5 C6 1.502(2) . ?
C6 C7 1.529(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.532(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C14 1.521(2) . ?
C8 C9 1.549(2) . ?
C8 H8A 0.9800 . ?
C9 C11 1.536(2) . ?
C9 H9A 0.9800 . ?
C11 C12 1.536(2) . ?
C11 H11A 0.9800 . ?
C12 C13 1.526(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.541(2) . ?
C13 C19 1.543(2) . ?
C13 C17 1.557(2) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C14 C15 1.537(2) . ?
C14 H14A 0.9800 . ?
C15 C16 1.529(2) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.558(2) . ?
C16 H16A 0.9800 . ?
C17 C20 1.531(2) . ?
C20 C21 1.515(2) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C29 C30 1.508(2) . ?
C30 C31 1.510(2) . ?
C30 C32 1.532(3) . ?
C30 H30A 0.9800 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C22 C23 1.503(2) . ?
C22 H22A 0.9800 . ?
C23 C24 1.530(2) . ?
C23 C28 1.532(2) . ?
C23 H23A 0.9800 . ?
C28 C27 1.524(2) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C27 C26 1.518(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C26 C25 1.520(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C25 C24 1.531(2) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C33 H33A 0.88(7) . ?
C33 H33B 1.08(5) . ?
C33 H33C 0.98(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 O2 H2A 109.5 . . ?
C29 O6 C21 115.14(13) . . ?
C22 O4 C16 107.99(11) . . ?
C22 O3 C17 105.12(11) . . ?
C33 O8 H8B 106.0(14) . . ?
C5 C4 C3 122.30(15) . . ?
C5 C4 H4A 118.8 . . ?
C3 C4 H4A 118.8 . . ?
O1 C3 C2 121.16(16) . . ?
O1 C3 C4 121.63(15) . . ?
C2 C3 C4 117.22(14) . . ?
C1 C2 C3 121.02(15) . . ?
C1 C2 H2B 119.5 . . ?
C3 C2 H2B 119.5 . . ?
C2 C1 C10 124.23(14) . . ?
C2 C1 H1A 117.9 . . ?
C10 C1 H1A 117.9 . . ?
C1 C10 C5 112.74(12) . . ?
C1 C10 C18 107.67(13) . . ?
C5 C10 C18 109.15(12) . . ?
C1 C10 C9 108.01(12) . . ?
C5 C10 C9 105.28(11) . . ?
C18 C10 C9 114.11(12) . . ?
C10 C18 H18A 109.5 . . ?
C10 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C10 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C4 C5 C6 122.65(14) . . ?
C4 C5 C10 122.26(14) . . ?
C6 C5 C10 114.88(13) . . ?
C5 C6 C7 109.98(12) . . ?
C5 C6 H6A 109.7 . . ?
C7 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
C7 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C6 C7 C8 113.55(13) . . ?
C6 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
C8 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C14 C8 C7 110.20(12) . . ?
C14 C8 C9 107.79(11) . . ?
C7 C8 C9 109.76(12) . . ?
C14 C8 H8A 109.7 . . ?
C7 C8 H8A 109.7 . . ?
C9 C8 H8A 109.7 . . ?
C11 C9 C8 115.84(12) . . ?
C11 C9 C10 114.25(12) . . ?
C8 C9 C10 112.27(11) . . ?
C11 C9 H9A 104.3 . . ?
C8 C9 H9A 104.3 . . ?
C10 C9 H9A 104.3 . . ?
O2 C11 C9 110.40(12) . . ?
O2 C11 C12 111.45(12) . . ?
C9 C11 C12 111.96(12) . . ?
O2 C11 H11A 107.6 . . ?
C9 C11 H11A 107.6 . . ?
C12 C11 H11A 107.6 . . ?
C13 C12 C11 112.96(12) . . ?
C13 C12 H12A 109.0 . . ?
C11 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
C11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C12 C13 C14 109.12(12) . . ?
C12 C13 C19 112.25(12) . . ?
C14 C13 C19 112.20(12) . . ?
C12 C13 C17 114.99(12) . . ?
C14 C13 C17 99.28(11) . . ?
C19 C13 C17 108.37(12) . . ?
C13 C19 H19A 109.5 . . ?
C13 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C13 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C8 C14 C15 119.49(12) . . ?
C8 C14 C13 113.70(12) . . ?
C15 C14 C13 103.23(12) . . ?
C8 C14 H14A 106.5 . . ?
C15 C14 H14A 106.5 . . ?
C13 C14 H14A 106.5 . . ?
C16 C15 C14 103.10(12) . . ?
C16 C15 H15A 111.1 . . ?
C14 C15 H15A 111.1 . . ?
C16 C15 H15B 111.1 . . ?
C14 C15 H15B 111.1 . . ?
H15A C15 H15B 109.1 . . ?
O4 C16 C15 109.98(12) . . ?
O4 C16 C17 103.75(11) . . ?
C15 C16 C17 106.54(12) . . ?
O4 C16 H16A 112.0 . . ?
C15 C16 H16A 112.0 . . ?
C17 C16 H16A 112.0 . . ?
O3 C17 C20 108.33(11) . . ?
O3 C17 C13 110.21(11) . . ?
C20 C17 C13 114.41(12) . . ?
O3 C17 C16 103.26(11) . . ?
C20 C17 C16 115.33(12) . . ?
C13 C17 C16 104.70(11) . . ?
O5 C20 C21 121.80(14) . . ?
O5 C20 C17 123.23(14) . . ?
C21 C20 C17 114.97(12) . . ?
O6 C21 C20 111.98(13) . . ?
O6 C21 H21A 109.2 . . ?
C20 C21 H21A 109.2 . . ?
O6 C21 H21B 109.2 . . ?
C20 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
O7 C29 O6 123.65(14) . . ?
O7 C29 C30 125.18(14) . . ?
O6 C29 C30 111.17(13) . . ?
C29 C30 C31 109.05(14) . . ?
C29 C30 C32 109.54(14) . . ?
C31 C30 C32 110.67(16) . . ?
C29 C30 H30A 109.2 . . ?
C31 C30 H30A 109.2 . . ?
C32 C30 H30A 109.2 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O4 C22 O3 105.15(11) . . ?
O4 C22 C23 111.47(12) . . ?
O3 C22 C23 110.61(12) . . ?
O4 C22 H22A 109.8 . . ?
O3 C22 H22A 109.8 . . ?
C23 C22 H22A 109.8 . . ?
C22 C23 C24 111.22(13) . . ?
C22 C23 C28 110.55(13) . . ?
C24 C23 C28 110.84(14) . . ?
C22 C23 H23A 108.0 . . ?
C24 C23 H23A 108.0 . . ?
C28 C23 H23A 108.0 . . ?
C27 C28 C23 111.72(15) . . ?
C27 C28 H28A 109.3 . . ?
C23 C28 H28A 109.3 . . ?
C27 C28 H28B 109.3 . . ?
C23 C28 H28B 109.3 . . ?
H28A C28 H28B 107.9 . . ?
C26 C27 C28 111.10(16) . . ?
C26 C27 H27A 109.4 . . ?
C28 C27 H27A 109.4 . . ?
C26 C27 H27B 109.4 . . ?
C28 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
C27 C26 C25 110.44(16) . . ?
C27 C26 H26A 109.6 . . ?
C25 C26 H26A 109.6 . . ?
C27 C26 H26B 109.6 . . ?
C25 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
C26 C25 C24 111.60(17) . . ?
C26 C25 H25A 109.3 . . ?
C24 C25 H25A 109.3 . . ?
C26 C25 H25B 109.3 . . ?
C24 C25 H25B 109.3 . . ?
H25A C25 H25B 108.0 . . ?
C23 C24 C25 110.58(14) . . ?
C23 C24 H24A 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
O8 C33 H33A 130(4) . . ?
O8 C33 H33B 121(3) . . ?
H33A C33 H33B 98(4) . . ?
O8 C33 H33C 105(4) . . ?
H33A C33 H33C 98(5) . . ?
H33B C33 H33C 99(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C4 C3 O1 176.12(15) . . . . ?
C5 C4 C3 C2 -4.0(2) . . . . ?
O1 C3 C2 C1 -178.20(16) . . . . ?
C4 C3 C2 C1 1.9(2) . . . . ?
C3 C2 C1 C10 2.7(2) . . . . ?
C2 C1 C10 C5 -5.0(2) . . . . ?
C2 C1 C10 C18 -125.48(16) . . . . ?
C2 C1 C10 C9 110.86(16) . . . . ?
C3 C4 C5 C6 -172.95(14) . . . . ?
C3 C4 C5 C10 1.4(2) . . . . ?
C1 C10 C5 C4 2.9(2) . . . . ?
C18 C10 C5 C4 122.48(15) . . . . ?
C9 C10 C5 C4 -114.64(15) . . . . ?
C1 C10 C5 C6 177.66(12) . . . . ?
C18 C10 C5 C6 -62.74(16) . . . . ?
C9 C10 C5 C6 60.14(15) . . . . ?
C4 C5 C6 C7 116.42(16) . . . . ?
C10 C5 C6 C7 -58.34(16) . . . . ?
C5 C6 C7 C8 52.13(16) . . . . ?
C6 C7 C8 C14 -170.45(12) . . . . ?
C6 C7 C8 C9 -51.89(15) . . . . ?
C14 C8 C9 C11 -50.48(16) . . . . ?
C7 C8 C9 C11 -170.52(12) . . . . ?
C14 C8 C9 C10 175.77(11) . . . . ?
C7 C8 C9 C10 55.73(15) . . . . ?
C1 C10 C9 C11 46.62(15) . . . . ?
C5 C10 C9 C11 167.28(12) . . . . ?
C18 C10 C9 C11 -73.07(16) . . . . ?
C1 C10 C9 C8 -178.87(12) . . . . ?
C5 C10 C9 C8 -58.20(15) . . . . ?
C18 C10 C9 C8 61.44(16) . . . . ?
C8 C9 C11 O2 -76.97(15) . . . . ?
C10 C9 C11 O2 55.87(16) . . . . ?
C8 C9 C11 C12 47.82(17) . . . . ?
C10 C9 C11 C12 -179.34(11) . . . . ?
O2 C11 C12 C13 74.94(15) . . . . ?
C9 C11 C12 C13 -49.27(16) . . . . ?
C11 C12 C13 C14 54.72(16) . . . . ?
C11 C12 C13 C19 -70.30(15) . . . . ?
C11 C12 C13 C17 165.21(12) . . . . ?
C7 C8 C14 C15 -61.13(17) . . . . ?
C9 C8 C14 C15 179.11(12) . . . . ?
C7 C8 C14 C13 176.50(12) . . . . ?
C9 C8 C14 C13 56.74(16) . . . . ?
C12 C13 C14 C8 -60.34(16) . . . . ?
C19 C13 C14 C8 64.71(16) . . . . ?
C17 C13 C14 C8 179.01(11) . . . . ?
C12 C13 C14 C15 168.71(11) . . . . ?
C19 C13 C14 C15 -66.24(15) . . . . ?
C17 C13 C14 C15 48.06(13) . . . . ?
C8 C14 C15 C16 -168.12(12) . . . . ?
C13 C14 C15 C16 -40.73(14) . . . . ?
C22 O4 C16 C15 123.54(12) . . . . ?
C22 O4 C16 C17 9.91(15) . . . . ?
C14 C15 C16 O4 -95.27(13) . . . . ?
C14 C15 C16 C17 16.56(15) . . . . ?
C22 O3 C17 C20 90.43(13) . . . . ?
C22 O3 C17 C13 -143.70(12) . . . . ?
C22 O3 C17 C16 -32.33(14) . . . . ?
C12 C13 C17 O3 -42.79(16) . . . . ?
C14 C13 C17 O3 73.47(13) . . . . ?
C19 C13 C17 O3 -169.30(11) . . . . ?
C12 C13 C17 C20 79.56(15) . . . . ?
C14 C13 C17 C20 -164.18(12) . . . . ?
C19 C13 C17 C20 -46.95(16) . . . . ?
C12 C13 C17 C16 -153.23(12) . . . . ?
C14 C13 C17 C16 -36.97(13) . . . . ?
C19 C13 C17 C16 80.26(14) . . . . ?
O4 C16 C17 O3 13.76(14) . . . . ?
C15 C16 C17 O3 -102.32(13) . . . . ?
O4 C16 C17 C20 -104.21(14) . . . . ?
C15 C16 C17 C20 139.72(12) . . . . ?
O4 C16 C17 C13 129.14(12) . . . . ?
C15 C16 C17 C13 13.07(15) . . . . ?
O3 C17 C20 O5 -142.95(14) . . . . ?
C13 C17 C20 O5 93.69(17) . . . . ?
C16 C17 C20 O5 -27.9(2) . . . . ?
O3 C17 C20 C21 36.29(17) . . . . ?
C13 C17 C20 C21 -87.08(16) . . . . ?
C16 C17 C20 C21 151.38(13) . . . . ?
C29 O6 C21 C20 74.72(17) . . . . ?
O5 C20 C21 O6 -1.9(2) . . . . ?
C17 C20 C21 O6 178.86(12) . . . . ?
C21 O6 C29 O7 0.0(2) . . . . ?
C21 O6 C29 C30 179.91(13) . . . . ?
O7 C29 C30 C31 56.0(2) . . . . ?
O6 C29 C30 C31 -123.89(16) . . . . ?
O7 C29 C30 C32 -65.3(2) . . . . ?
O6 C29 C30 C32 114.86(16) . . . . ?
C16 O4 C22 O3 -30.56(14) . . . . ?
C16 O4 C22 C23 -150.45(12) . . . . ?
C17 O3 C22 O4 39.76(14) . . . . ?
C17 O3 C22 C23 160.22(12) . . . . ?
O4 C22 C23 C24 -57.78(17) . . . . ?
O3 C22 C23 C24 -174.39(13) . . . . ?
O4 C22 C23 C28 178.64(13) . . . . ?
O3 C22 C23 C28 62.03(16) . . . . ?
C22 C23 C28 C27 178.63(14) . . . . ?
C24 C23 C28 C27 54.8(2) . . . . ?
C23 C28 C27 C26 -55.8(2) . . . . ?
C28 C27 C26 C25 56.4(3) . . . . ?
C27 C26 C25 C24 -57.2(2) . . . . ?
C22 C23 C24 C25 -178.09(14) . . . . ?
C28 C23 C24 C25 -54.7(2) . . . . ?
C26 C25 C24 C23 56.5(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2A O7 0.82 2.08 2.8607(17) 158.2 4_565
O8 H8B O1 1.00(3) 1.79(3) 2.784(2) 169(2) .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.035
