# 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_ices15
_database_code_depnum_ccdc_archive 'CCDC 1476517'
_audit_update_record             
;
2016-04-26 deposited with the CCDC.
2016-11-17 downloaded from the CCDC.
;
_chemical_name_systematic        
'5-methyl-6,9-dioxobicyclo[3.3.1]nonan-2-yl 3,5-dinitrobenzoate'
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H16 N2 O8'
_chemical_formula_iupac          ?
_chemical_formula_weight         376.32
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   10.6964(11)
_cell_length_b                   25.365(3)
_cell_length_c                   6.2244(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1688.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4917
_cell_measurement_theta_min      2.4909
_cell_measurement_theta_max      33.9533
_cell_measurement_temperature    103.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.220
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784

_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_T_max  0.97

_exptl_special_details           
;
;

_diffrn_ambient_temperature      103.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker KappaCCD'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            24863
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_theta_min         2.49
_diffrn_reflns_theta_max         36.39
_diffrn_reflns_theta_full        36.39
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9

_refine_special_details          
;


;

_reflns_number_total             7597
_reflns_number_gt                6529
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1094
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_number_reflns         7597
_refine_ls_number_parameters     245
_refine_ls_number_restraints     1
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0599P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.241
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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

_computing_data_collection       'APEX3 (Bruker AXS Inc., 2015)'
_computing_cell_refinement       'SAINT V8.35A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.35A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2015)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2015)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.38301(12) 0.34246(5) 0.5566(3) 0.0129(2) Uani d . . . 1 . .
H H1 0.4042 0.3599 0.6868 0.015 Uiso calc U . R 1 . .
C C2 0.25873(13) 0.33553(5) 0.4970(3) 0.0139(3) Uani d . . . 1 . .
C C3 0.22264(13) 0.31081(6) 0.3091(3) 0.0148(3) Uani d . . . 1 . .
H H3 0.1372 0.3071 0.2705 0.018 Uiso calc U . R 1 . .
C C4 0.31810(13) 0.29169(6) 0.1799(3) 0.0130(3) Uani d . . . 1 . .
C C5 0.44350(13) 0.29715(5) 0.2303(3) 0.0129(2) Uani d . . . 1 . .
H H5 0.5063 0.2835 0.1379 0.015 Uiso calc U . R 1 . .
C C6 0.47544(12) 0.32319(5) 0.4202(2) 0.0115(2) Uani d . . . 1 . .
C C7 0.61114(12) 0.33025(5) 0.4694(2) 0.0117(2) Uani d . . . 1 . .
C C8 0.75872(12) 0.37397(6) 0.6975(3) 0.0130(3) Uani d . . . 1 . .
H H8 0.8146 0.3448 0.6479 0.016 Uiso calc U . R 1 . .
C C9 0.75618(13) 0.37592(6) 0.9422(3) 0.0128(2) Uani d . . . 1 . .
H H9 0.7169 0.3427 0.9961 0.015 Uiso calc U . R 1 . .
C C10 0.67713(12) 0.42200(6) 1.0154(3) 0.0130(2) Uani d . . . 1 . .
C C11 0.72476(13) 0.47527(6) 0.9367(3) 0.0151(3) Uani d . . . 1 . .
C C12 0.64170(16) 0.52061(6) 1.0100(4) 0.0253(4) Uani d . . . 1 . .
H H12A 0.5556 0.5142 0.9629 0.038 Uiso calc U . R 1 . .
H H12B 0.672 0.5537 0.9471 0.038 Uiso calc U . R 1 . .
H H12C 0.6441 0.5232 1.167 0.038 Uiso calc U . R 1 . .
C C13 0.72708(14) 0.47290(6) 0.6864(3) 0.0170(3) Uani d . . . 1 . .
H H13A 0.6398 0.472 0.6335 0.02 Uiso calc U . R 1 . .
H H13B 0.766 0.5057 0.6316 0.02 Uiso calc U . R 1 . .
C C14 0.79741(13) 0.42571(6) 0.5929(3) 0.0155(3) Uani d . . . 1 . .
H H14A 0.7811 0.4237 0.4365 0.019 Uiso calc U . R 1 . .
H H14B 0.8883 0.431 0.6134 0.019 Uiso calc U . R 1 . .
C C15 0.88773(13) 0.38092(6) 1.0428(3) 0.0147(3) Uani d . . . 1 . .
H H15A 0.8824 0.3707 1.196 0.018 Uiso calc U . R 1 . .
H H15B 0.944 0.3554 0.9709 0.018 Uiso calc U . R 1 . .
C C16 0.94731(13) 0.43606(6) 1.0288(3) 0.0176(3) Uani d . . . 1 . .
H H16A 1.0019 0.4407 1.1558 0.021 Uiso calc U . R 1 . .
H H16B 1.0018 0.4368 0.9002 0.021 Uiso calc U . R 1 . .
C C17 0.86018(13) 0.48292(6) 1.0171(3) 0.0167(3) Uani d . . . 1 . .
N N1 0.16039(11) 0.35547(5) 0.6424(3) 0.0177(3) Uani d . . . 1 . .
N N2 0.28465(12) 0.26371(5) -0.0189(2) 0.0161(2) Uani d . . . 1 . .
O O1 0.19292(11) 0.37390(5) 0.8154(2) 0.0220(2) Uani d . . . 1 . .
O O2 0.05171(11) 0.35202(6) 0.5820(2) 0.0270(3) Uani d . . . 1 . .
O O3 0.17318(11) 0.26020(5) -0.0669(2) 0.0211(3) Uani d . . . 1 . .
O O4 0.37008(12) 0.24541(5) -0.1278(2) 0.0236(3) Uani d . . . 1 . .
O O5 0.69376(10) 0.30897(4) 0.3683(2) 0.0154(2) Uani d . . . 1 . .
O O6 0.62860(9) 0.36294(4) 0.6352(2) 0.0147(2) Uani d . . . 1 . .
O O7 0.58544(10) 0.41748(5) 1.1293(2) 0.0216(3) Uani d . . . 1 . .
O O8 0.89725(12) 0.52698(5) 1.0591(3) 0.0278(3) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.3913(19) ?
C1 C6 . 1.392(2) ?
C2 C3 . 1.382(2) ?
C2 N1 . 1.477(2) ?
C3 C4 . 1.387(2) ?
C4 C5 . 1.3846(19) ?
C4 N2 . 1.471(2) ?
C5 C6 . 1.396(2) ?
C6 C7 . 1.4942(18) ?
C7 O5 . 1.2117(17) ?
C7 O6 . 1.3371(18) ?
C8 O6 . 1.4717(17) ?
C8 C14 . 1.522(2) ?
C8 C9 . 1.524(2) ?
C9 C10 . 1.513(2) ?
C9 C15 . 1.545(2) ?
C10 O7 . 1.2156(18) ?
C10 C11 . 1.525(2) ?
C11 C12 . 1.523(2) ?
C11 C17 . 1.545(2) ?
C11 C13 . 1.559(3) ?
C13 C14 . 1.529(2) ?
C15 C16 . 1.539(2) ?
C16 C17 . 1.512(2) ?
C17 O8 . 1.2144(19) ?
N1 O1 . 1.224(2) ?
N1 O2 . 1.2250(18) ?
N2 O4 . 1.2288(19) ?
N2 O3 . 1.2325(16) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C6 . . 118.14(14) ?
C3 C2 C1 . . 123.37(14) ?
C3 C2 N1 . . 118.36(13) ?
C1 C2 N1 . . 118.27(15) ?
C2 C3 C4 . . 116.32(13) ?
C5 C4 C3 . . 123.15(15) ?
C5 C4 N2 . . 118.34(14) ?
C3 C4 N2 . . 118.51(12) ?
C4 C5 C6 . . 118.44(14) ?
C1 C6 C5 . . 120.57(12) ?
C1 C6 C7 . . 121.53(13) ?
C5 C6 C7 . . 117.89(12) ?
O5 C7 O6 . . 125.12(13) ?
O5 C7 C6 . . 123.28(14) ?
O6 C7 C6 . . 111.60(12) ?
O6 C8 C14 . . 107.96(12) ?
O6 C8 C9 . . 104.62(12) ?
C14 C8 C9 . . 113.86(12) ?
C10 C9 C8 . . 109.63(13) ?
C10 C9 C15 . . 108.87(12) ?
C8 C9 C15 . . 113.04(12) ?
O7 C10 C9 . . 123.62(13) ?
O7 C10 C11 . . 122.72(13) ?
C9 C10 C11 . . 113.65(12) ?
C12 C11 C10 . . 112.20(13) ?
C12 C11 C17 . . 110.79(13) ?
C10 C11 C17 . . 108.69(13) ?
C12 C11 C13 . . 109.74(15) ?
C10 C11 C13 . . 106.98(13) ?
C17 C11 C13 . . 108.29(13) ?
C14 C13 C11 . . 114.75(14) ?
C8 C14 C13 . . 112.22(13) ?
C16 C15 C9 . . 115.38(12) ?
C17 C16 C15 . . 117.49(12) ?
O8 C17 C16 . . 120.78(14) ?
O8 C17 C11 . . 119.44(14) ?
C16 C17 C11 . . 119.65(12) ?
O1 N1 O2 . . 124.56(14) ?
O1 N1 C2 . . 117.86(13) ?
O2 N1 C2 . . 117.58(15) ?
O4 N2 O3 . . 123.93(15) ?
O4 N2 C4 . . 117.75(12) ?
O3 N2 C4 . . 118.33(13) ?
C7 O6 C8 . . 116.95(11) ?

####################################################################### 
# 
# 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_ices7
_database_code_depnum_ccdc_archive 'CCDC 1485262'
_audit_update_record             
;
2016-06-14 deposited with the CCDC.
2016-11-17 downloaded from the CCDC.
;
_chemical_name_systematic        
1,3,3,7-tetramethylbicyclo[3.3.1]nonane-2,6,9-trione
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H18 O3'
_chemical_formula_iupac          ?
_chemical_formula_weight         222.27

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.6185(16)
_cell_length_b                   6.4539(8)
_cell_length_c                   28.975(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.150(2)
_cell_angle_gamma                90
_cell_volume                     2322.8(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4832
_cell_measurement_theta_min      2.8567
_cell_measurement_theta_max      29.6159
_cell_measurement_temperature    103.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960

_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_T_max  0.99

_exptl_special_details           
;
;

_diffrn_ambient_temperature      103.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker KappaCCD'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            21935
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         29.70
_diffrn_reflns_theta_full        29.70
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40

_refine_special_details          
;
;

_reflns_number_total             6533
_reflns_number_gt                4743
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1786
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_number_reflns         6533
_refine_ls_number_parameters     297
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0843P)²+0.3771P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.329
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'APEX3 (Bruker AXS Inc., 2015)'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XS, VERSION 2013/1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2015)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2015)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 1.03027(11) 0.9962(2) 0.08830(5) 0.0135(3) Uani d . . . 1 . .
C C2 0.91030(11) 1.0361(2) 0.07301(5) 0.0144(3) Uani d . . . 1 . .
C C3 0.85744(11) 1.0727(2) 0.11667(5) 0.0141(3) Uani d . . . 1 . .
H H3A 0.7787 1.0537 0.1074 0.017 Uiso calc U . R 1 . .
H H3B 0.87 1.2186 0.1267 0.017 Uiso calc U . R 1 . .
C C4 0.89778(11) 0.9296(2) 0.15989(5) 0.0126(3) Uani d . . . 1 . .
H H4 0.8345 0.8698 0.1717 0.015 Uiso calc U . R 1 . .
C C5 0.96508(11) 1.0596(2) 0.19855(5) 0.0128(3) Uani d . . . 1 . .
C C6 1.07258(11) 1.1339(2) 0.18850(5) 0.0139(3) Uani d . . . 1 . .
H H6 1.0574 1.2392 0.1629 0.017 Uiso calc U . R 1 . .
C C7 1.13237(11) 0.9527(2) 0.16990(5) 0.0142(3) Uani d . . . 1 . .
H H7A 1.1547 0.8529 0.1957 0.017 Uiso calc U . R 1 . .
H H7B 1.1984 1.0068 0.1601 0.017 Uiso calc U . R 1 . .
C C8 1.06459(11) 0.8366(2) 0.12795(5) 0.0134(3) Uani d . . . 1 . .
C C9 0.96649(11) 0.7559(2) 0.14603(5) 0.0133(3) Uani d . . . 1 . .
C C10 0.86228(12) 0.8422(2) 0.04593(5) 0.0177(3) Uani d . . . 1 . .
H H10A 0.8944 0.8249 0.0177 0.027 Uiso calc U . R 1 . .
H H10B 0.7842 0.8589 0.0369 0.027 Uiso calc U . R 1 . .
H H10C 0.8778 0.7197 0.066 0.027 Uiso calc U . R 1 . .
C C11 0.89014(14) 1.2259(2) 0.04104(5) 0.0232(3) Uani d . . . 1 . .
H H11A 0.9287 1.3454 0.0567 0.035 Uiso calc U . R 1 . .
H H11B 0.8128 1.256 0.0342 0.035 Uiso calc U . R 1 . .
H H11C 0.916 1.1981 0.0117 0.035 Uiso calc U . R 1 . .
C C12 1.14031(13) 1.2396(2) 0.23061(5) 0.0207(3) Uani d . . . 1 . .
H H12A 1.1021 1.3618 0.2392 0.031 Uiso calc U . R 1 . .
H H12B 1.2094 1.2821 0.2226 0.031 Uiso calc U . R 1 . .
H H12C 1.153 1.1428 0.2571 0.031 Uiso calc U . R 1 . .
C C13 1.13006(13) 0.6625(3) 0.11095(6) 0.0229(3) Uani d . . . 1 . .
H H13A 1.1504 0.5616 0.1362 0.034 Uiso calc U . R 1 . .
H H13B 1.1952 0.7204 0.1018 0.034 Uiso calc U . R 1 . .
H H13C 1.0867 0.5939 0.0839 0.034 Uiso calc U . R 1 . .
C C14 0.53166(11) 0.3206(2) 0.08657(5) 0.0151(3) Uani d . . . 1 . .
C C15 0.41215(12) 0.2724(2) 0.07185(5) 0.0148(3) Uani d . . . 1 . .
C C16 0.35713(11) 0.2468(2) 0.11523(5) 0.0146(3) Uani d . . . 1 . .
H H16A 0.367 0.1016 0.1262 0.018 Uiso calc U . R 1 . .
H H16B 0.2789 0.2697 0.1052 0.018 Uiso calc U . R 1 . .
C C17 0.39761(11) 0.3925(2) 0.15770(5) 0.0128(3) Uani d . . . 1 . .
H H17 0.3344 0.4538 0.1693 0.015 Uiso calc U . R 1 . .
C C18 0.46459(11) 0.2641(2) 0.19678(5) 0.0127(3) Uani d . . . 1 . .
C C19 0.57213(11) 0.1882(2) 0.18699(5) 0.0132(3) Uani d . . . 1 . .
H H19 0.557 0.0822 0.1615 0.016 Uiso calc U . R 1 . .
C C20 0.63205(11) 0.3682(2) 0.16822(5) 0.0144(3) Uani d . . . 1 . .
H H20A 0.6984 0.3137 0.1588 0.017 Uiso calc U . R 1 . .
H H20B 0.6539 0.4692 0.1939 0.017 Uiso calc U . R 1 . .
C C21 0.56476(11) 0.4828(2) 0.12579(5) 0.0139(3) Uani d . . . 1 . .
C C22 0.46622(11) 0.5643(2) 0.14309(5) 0.0131(3) Uani d . . . 1 . .
C C23 0.36199(13) 0.4568(2) 0.04157(5) 0.0192(3) Uani d . . . 1 . .
H H23A 0.3689 0.5831 0.0606 0.029 Uiso calc U . R 1 . .
H H23B 0.2856 0.4287 0.0299 0.029 Uiso calc U . R 1 . .
H H23C 0.3996 0.4754 0.015 0.029 Uiso calc U . R 1 . .
C C24 0.39585(13) 0.0734(2) 0.04305(5) 0.0223(3) Uani d . . . 1 . .
H H24A 0.4208 0.0943 0.0132 0.033 Uiso calc U . R 1 . .
H H24B 0.3192 0.0372 0.0369 0.033 Uiso calc U . R 1 . .
H H24C 0.437 -0.0391 0.0605 0.033 Uiso calc U . R 1 . .
C C25 0.63955(12) 0.0835(2) 0.22936(5) 0.0202(3) Uani d . . . 1 . .
H H25A 0.6539 0.1822 0.2554 0.03 Uiso calc U . R 1 . .
H H25B 0.7079 0.0368 0.2213 0.03 Uiso calc U . R 1 . .
H H25C 0.6003 -0.036 0.2387 0.03 Uiso calc U . R 1 . .
C C26 0.63129(13) 0.6556(3) 0.10886(6) 0.0240(4) Uani d . . . 1 . .
H H26A 0.5893 0.7216 0.0811 0.036 Uiso calc U . R 1 . .
H H26B 0.6974 0.5971 0.1009 0.036 Uiso calc U . R 1 . .
H H26C 0.6498 0.7589 0.1338 0.036 Uiso calc U . R 1 . .
O O1 1.09870(9) 1.07941(18) 0.07015(4) 0.0234(3) Uani d . . . 1 . .
O O2 0.93081(9) 1.10021(17) 0.23394(3) 0.0198(2) Uani d . . . 1 . .
O O3 0.94673(9) 0.57402(15) 0.15044(4) 0.0202(2) Uani d . . . 1 . .
O O4 0.60001(9) 0.2422(2) 0.06782(4) 0.0267(3) Uani d . . . 1 . .
O O5 0.42986(9) 0.22410(17) 0.23212(3) 0.0201(2) Uani d . . . 1 . .
O O6 0.44557(9) 0.74665(16) 0.14610(4) 0.0207(3) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 . 1.2128(16) ?
C1 C2 . 1.523(2) ?
C1 C8 . 1.5468(19) ?
C2 C11 . 1.530(2) ?
C2 C10 . 1.543(2) ?
C2 C3 . 1.5487(18) ?
C3 C4 . 1.5669(19) ?
C4 C9 . 1.5140(19) ?
C4 C5 . 1.5314(19) ?
C5 O2 . 1.2099(16) ?
C5 C6 . 1.5146(19) ?
C6 C12 . 1.522(2) ?
C6 C7 . 1.5395(19) ?
C7 C8 . 1.5506(19) ?
C8 C9 . 1.5187(19) ?
C8 C13 . 1.5267(19) ?
C9 O3 . 1.2113(17) ?
C14 O4 . 1.2083(17) ?
C14 C15 . 1.525(2) ?
C14 C21 . 1.547(2) ?
C15 C24 . 1.526(2) ?
C15 C23 . 1.546(2) ?
C15 C16 . 1.5481(19) ?
C16 C17 . 1.5617(19) ?
C17 C22 . 1.5122(18) ?
C17 C18 . 1.5314(19) ?
C18 O5 . 1.2106(16) ?
C18 C19 . 1.5158(19) ?
C19 C25 . 1.523(2) ?
C19 C20 . 1.5367(19) ?
C20 C21 . 1.5529(19) ?
C21 C22 . 1.5145(19) ?
C21 C26 . 1.5277(19) ?
C22 O6 . 1.2121(17) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 C1 C2 . . 123.11(13) ?
O1 C1 C8 . . 119.31(13) ?
C2 C1 C8 . . 117.56(11) ?
C1 C2 C11 . . 111.24(12) ?
C1 C2 C10 . . 106.98(11) ?
C11 C2 C10 . . 109.45(12) ?
C1 C2 C3 . . 109.71(11) ?
C11 C2 C3 . . 108.84(12) ?
C10 C2 C3 . . 110.61(11) ?
C2 C3 C4 . . 115.91(11) ?
C9 C4 C5 . . 109.28(11) ?
C9 C4 C3 . . 110.18(10) ?
C5 C4 C3 . . 108.76(11) ?
O2 C5 C6 . . 124.09(13) ?
O2 C5 C4 . . 120.25(12) ?
C6 C5 C4 . . 115.65(11) ?
C5 C6 C12 . . 112.53(11) ?
C5 C6 C7 . . 109.74(11) ?
C12 C6 C7 . . 112.36(12) ?
C6 C7 C8 . . 113.88(11) ?
C9 C8 C13 . . 112.28(12) ?
C9 C8 C1 . . 110.24(11) ?
C13 C8 C1 . . 110.30(11) ?
C9 C8 C7 . . 105.43(10) ?
C13 C8 C7 . . 110.70(12) ?
C1 C8 C7 . . 107.69(11) ?
O3 C9 C4 . . 123.46(13) ?
O3 C9 C8 . . 124.35(13) ?
C4 C9 C8 . . 112.15(11) ?
O4 C14 C15 . . 122.52(13) ?
O4 C14 C21 . . 119.45(13) ?
C15 C14 C21 . . 117.98(11) ?
C14 C15 C24 . . 110.86(12) ?
C14 C15 C23 . . 106.69(12) ?
C24 C15 C23 . . 109.59(12) ?
C14 C15 C16 . . 110.95(11) ?
C24 C15 C16 . . 108.53(12) ?
C23 C15 C16 . . 110.22(11) ?
C15 C16 C17 . . 116.38(11) ?
C22 C17 C18 . . 109.57(11) ?
C22 C17 C16 . . 110.16(11) ?
C18 C17 C16 . . 108.54(11) ?
O5 C18 C19 . . 123.96(13) ?
O5 C18 C17 . . 120.39(12) ?
C19 C18 C17 . . 115.61(11) ?
C18 C19 C25 . . 112.58(11) ?
C18 C19 C20 . . 109.54(11) ?
C25 C19 C20 . . 112.40(12) ?
C19 C20 C21 . . 113.93(11) ?
C22 C21 C26 . . 112.48(12) ?
C22 C21 C14 . . 110.29(11) ?
C26 C21 C14 . . 110.51(11) ?
C22 C21 C20 . . 105.63(10) ?
C26 C21 C20 . . 110.30(12) ?
C14 C21 C20 . . 107.39(11) ?
O6 C22 C17 . . 123.41(13) ?
O6 C22 C21 . . 124.10(13) ?
C17 C22 C21 . . 112.47(11) ?

