# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2017

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

data_285
_database_code_depnum_ccdc_archive 'CCDC 1501909'
_audit_update_record             
;
2016-08-31 deposited with the CCDC.
2017-02-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19.09 H34 Cl N O12.22'
_chemical_formula_weight         508.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Cmc21

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

_cell_length_a                   10.8029(4)
_cell_length_b                   15.9579(5)
_cell_length_c                   14.6015(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2517.18(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2054
_cell_measurement_theta_min      4.9050
_cell_measurement_theta_max      72.5610

_exptl_crystal_description       rodshape
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .35
_exptl_crystal_size_min          .35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1081
_exptl_absorpt_coefficient_mu    1.886
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  w/
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3723
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.94
_diffrn_reflns_theta_max         66.55
_reflns_number_total             1799
_reflns_number_gt                1610
_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)+(0.1000P)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    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.021(3)
_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   0.02(4)
_refine_ls_number_reflns         1799
_refine_ls_number_parameters     164
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0823
_refine_ls_wR_factor_ref         0.2538
_refine_ls_wR_factor_gt          0.2434
_refine_ls_goodness_of_fit_ref   1.944
_refine_ls_restrained_S_all      1.984
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.0000 0.05783(13) 0.43591(12) 0.0800(8) Uani 1 2 d S . .
O4 O 0.2322(4) 0.5169(3) 0.6713(4) 0.0959(15) Uani 1 1 d D . .
O5 O 0.1319(5) 0.3520(3) 0.6452(3) 0.1022(17) Uani 1 1 d D . .
C6 C 0.2979(7) 0.5852(6) 0.7142(8) 0.126(3) Uani 1 1 d D . .
H6A H 0.3173 0.5703 0.7785 0.152 Uiso 1 1 calc R . .
H6B H 0.3770 0.5950 0.6817 0.152 Uiso 1 1 calc R . .
C7 C 0.0615(8) 0.3017(10) 0.5925(12) 0.250(11) Uani 1 1 d D . .
H7A H 0.0871 0.3124 0.5285 0.300 Uiso 1 1 calc R . .
H7B H 0.0871 0.2436 0.6068 0.300 Uiso 1 1 calc R . .
O8 O 0.1269(7) 0.6541(4) 0.7695(7) 0.146(3) Uani 1 1 d D . .
C12 C 0.2360(9) 0.3884(6) 0.5971(5) 0.125(3) Uani 1 1 d D . .
H12A H 0.2920 0.3433 0.5757 0.150 Uiso 1 1 calc R . .
H12B H 0.2061 0.4195 0.5427 0.150 Uiso 1 1 calc R . .
C15 C 0.2248(9) 0.6603(5) 0.7123(8) 0.124(3) Uani 1 1 d D . .
H15A H 0.2766 0.7086 0.7306 0.149 Uiso 1 1 calc R . .
H15B H 0.1949 0.6703 0.6492 0.149 Uiso 1 1 calc R . .
C20 C 0.3021(8) 0.4441(5) 0.6565(8) 0.112(3) Uani 1 1 d D . .
H20A H 0.3185 0.4160 0.7157 0.135 Uiso 1 1 calc R . .
H20B H 0.3826 0.4590 0.6285 0.135 Uiso 1 1 calc R . .
O1 O 0.0000 0.5484(4) 0.5862(3) 0.0793(16) Uani 1 2 d S . .
C1 C 0.0616(8) 0.7220(5) 0.7720(19) 0.238(10) Uani 1 1 d D . .
H1A H 0.0877 0.7563 0.7189 0.286 Uiso 1 1 calc R . .
H1B H 0.0877 0.7529 0.8276 0.286 Uiso 1 1 calc R . .
N1 N 0.0000 0.5903(4) 0.4040(4) 0.080(2) Uani 1 2 d S . .
C5 C -0.1130(7) 0.6402(9) 0.3827(6) 0.128(4) Uani 1 1 d . B .
H5A H -0.1172 0.6499 0.3158 0.153 Uiso 1 1 calc R . .
H5B H -0.1871 0.6076 0.4007 0.153 Uiso 1 1 calc R . .
C4 C 0.0000 0.7617(13) 0.4097(16) 0.26(2) Uani 1 2 d S . .
H4A H 0.0000 0.8139 0.4463 0.310 Uiso 1 2 calc SR . .
H4B H 0.0000 0.7783 0.3443 0.310 Uiso 1 2 calc SR . .
C2 C -0.115(2) 0.7176(13) 0.4281(9) 0.259(14) Uani 1 1 d . . .
H2A H -0.1241 0.7087 0.4948 0.311 Uiso 1 1 calc R B .
H2B H -0.1858 0.7514 0.4064 0.311 Uiso 1 1 calc R . .
O6A O 0.0000 -0.0287(7) 0.4478(15) 0.162(14) Uani 0.65(5) 2 d SP A 1
O3 O 0.0000 0.0801(10) 0.3491(8) 0.256(12) Uani 1 2 d S . .
O2A O 0.073(3) 0.1059(13) 0.492(2) 0.276(14) Uani 0.75(4) 1 d P . 1
C3A C 0.0000 0.513(2) 0.343(3) 0.08(2) Uiso 0.27(9) 2 d SP B 1
O6B O 0.117(3) 0.009(3) 0.427(3) 0.356(15) Uiso 0.784(18) 1 d P A 2
O2B O 0.117(3) 0.085(3) 0.427(3) 0.14(2) Uiso 0.25(4) 1 d P A 2
C3B C 0.070(4) 0.5072(18) 0.3589(19) 0.216(9) Uiso 0.91(3) 1 d P . 2


_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
Cl1 O3 1.316(12) . ?
Cl1 O2B 1.34(3) 3 ?
Cl1 O2B 1.34(3) . ?
Cl1 O2A 1.375(12) 3 ?
Cl1 O2A 1.375(13) . ?
Cl1 O6A 1.391(12) . ?
Cl1 O6B 1.50(3) 3 ?
Cl1 O6B 1.50(3) . ?
O4 C20 1.402(9) . ?
O4 C6 1.444(10) . ?
O5 C7 1.347(10) . ?
O5 C12 1.448(10) . ?
C6 C15 1.435(11) . ?
C7 C7 1.329(17) 3 ?
O8 C1 1.294(10) . ?
O8 C15 1.351(11) . ?
C12 C20 1.433(12) . ?
C1 C1 1.330(17) 3 ?
N1 C5 1.490(11) 3 ?
N1 C5 1.490(11) . ?
N1 C3A 1.53(4) . ?
N1 C3B 1.66(3) 3 ?
N1 C3B 1.66(3) . ?
C5 C2 1.40(2) . ?
C4 C2 1.45(2) . ?
C4 C2 1.45(2) 3 ?
O3 O2B 1.70(4) . ?
O3 O2B 1.70(4) 3 ?
O2A O2A 1.57(6) 3 ?
O6B O2B 1.21(6) . ?
C3B C3B 1.51(8) 3 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cl1 O2B 79(2) . 3 ?
O3 Cl1 O2B 79(2) . . ?
O2B Cl1 O2B 141(3) 3 . ?
O3 Cl1 O2A 115.3(17) . 3 ?
O2B Cl1 O2A 48.9(18) 3 3 ?
O2B Cl1 O2A 115(3) . 3 ?
O3 Cl1 O2A 115.3(17) . . ?
O2B Cl1 O2A 115(3) 3 . ?
O2B Cl1 O2A 48.9(18) . . ?
O2A Cl1 O2A 70(3) 3 . ?
O3 Cl1 O6A 112.8(12) . . ?
O2B Cl1 O6A 109.4(18) 3 . ?
O2B Cl1 O6A 109.4(18) . . ?
O2A Cl1 O6A 118.6(12) 3 . ?
O2A Cl1 O6A 118.6(12) . . ?
O3 Cl1 O6B 93.3(17) . 3 ?
O2B Cl1 O6B 50(2) 3 3 ?
O2B Cl1 O6B 163(3) . 3 ?
O2A Cl1 O6B 82(2) 3 3 ?
O2A Cl1 O6B 146(2) . 3 ?
O6A Cl1 O6B 59(2) . 3 ?
O3 Cl1 O6B 93.3(17) . . ?
O2B Cl1 O6B 163(3) 3 . ?
O2B Cl1 O6B 50(2) . . ?
O2A Cl1 O6B 146(2) 3 . ?
O2A Cl1 O6B 82(2) . . ?
O6A Cl1 O6B 59(2) . . ?
O6B Cl1 O6B 116(4) 3 . ?
C20 O4 C6 115.3(6) . . ?
C7 O5 C12 113.6(9) . . ?
C15 C6 O4 110.5(6) . . ?
C7 C7 O5 124.4(4) 3 . ?
C1 O8 C15 112.5(11) . . ?
C20 C12 O5 110.0(6) . . ?
O8 C15 C6 111.0(8) . . ?
O4 C20 C12 109.8(7) . . ?
O8 C1 C1 123.1(5) . 3 ?
C5 N1 C5 110.1(9) 3 . ?
C5 N1 C3A 108.1(10) 3 . ?
C5 N1 C3A 108.1(10) . . ?
C5 N1 C3B 135.6(15) 3 3 ?
C5 N1 C3B 88.4(13) . 3 ?
C3A N1 C3B 28.4(14) . 3 ?
C5 N1 C3B 88.4(13) 3 . ?
C5 N1 C3B 135.6(15) . . ?
C3A N1 C3B 28.4(14) . . ?
C3B N1 C3B 54(3) 3 . ?
C2 C5 N1 112.5(10) . . ?
C2 C4 C2 117(2) . 3 ?
C5 C2 C4 109.2(11) . . ?
Cl1 O3 O2B 50.9(13) . . ?
Cl1 O3 O2B 50.9(13) . 3 ?
O2B O3 O2B 96(3) . 3 ?
Cl1 O2A O2A 55.1(14) . 3 ?
O2B O6B Cl1 58(2) . . ?
O6B O2B Cl1 72(3) . . ?
O6B O2B O3 88(3) . . ?
Cl1 O2B O3 49.7(14) . . ?
C3B C3B N1 63.1(14) 3 . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        66.55
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.062
####################################################################### 
# 
# 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_220k
_database_code_depnum_ccdc_archive 'CCDC 1501910'
_audit_update_record             
;
2016-08-31 deposited with the CCDC.
2017-02-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H73 Cl2 N7 O18'
_chemical_formula_weight         950.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pn21a

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

_cell_length_a                   31.3826(3)
_cell_length_b                   14.50650(10)
_cell_length_c                   10.79330(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4913.67(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8385
_cell_measurement_theta_min      4.1400
_cell_measurement_theta_max      73.0870

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2040
_exptl_absorpt_coefficient_mu    1.820
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  /w
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15002
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.15
_diffrn_reflns_theta_max         73.28
_reflns_number_total             7264
_reflns_number_gt                6809
_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)+(0.1269P)²+2.3819P] 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   0.47(2)
_refine_ls_number_reflns         7264
_refine_ls_number_parameters     547
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0612
_refine_ls_wR_factor_ref         0.1836
_refine_ls_wR_factor_gt          0.1790
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl2 Cl 0.34907(2) 0.43202(7) 0.24497(7) 0.0408(2) Uani 1 1 d . . .
Cl7 Cl 0.59949(3) 0.43604(7) 0.77568(8) 0.0448(2) Uani 1 1 d . . .
O11 O 0.69382(9) 0.6274(2) 0.3769(3) 0.0476(6) Uani 1 1 d . . .
O29 O 0.29640(9) 0.7418(2) 0.8801(3) 0.0509(7) Uani 1 1 d . . .
O41 O 0.45236(9) 0.6485(2) 0.8526(3) 0.0469(6) Uani 1 1 d . . .
O47 O 0.60096(7) 0.5863(2) 0.2236(2) 0.0464(6) Uani 1 1 d G . .
H47A H 0.6136 0.6026 0.2898 0.070 Uiso 1 1 d G . .
H47B H 0.6088 0.6210 0.1643 0.070 Uiso 1 1 d G . .
O1 O 0.33907(8) 0.3459(2) 0.2995(3) 0.0689(9) Uani 1 1 d G . .
O48 O 0.34916(8) 0.58803(19) 0.7182(2) 0.0462(6) Uani 1 1 d G . .
H48A H 0.3530 0.6110 0.6466 0.069 Uiso 1 1 d G . .
H48B H 0.3731 0.5705 0.7473 0.069 Uiso 1 1 d G . .
O14 O 0.70571(4) 0.66614(15) 0.11769(16) 0.0488(7) Uani 1 1 d G . .
O17 O 0.62217(4) 0.67933(14) 0.00337(13) 0.0434(6) Uani 1 1 d G . .
O32 O 0.30123(6) 0.8140(2) 0.6297(2) 0.0575(8) Uani 1 1 d G . .
O20 O 0.55002(5) 0.77413(13) 0.09836(15) 0.0686(10) Uani 1 1 d G . .
N49 N 0.58260(6) 0.40229(12) 0.2105(2) 0.0363(6) Uani 1 1 d G . .
H49 H 0.5878 0.4653 0.2153 0.044 Uiso 1 1 calc R . .
O6 O 0.59222(15) 0.3443(3) 0.8148(4) 0.0834(12) Uani 1 1 d . . .
O26 O 0.60953(9) 0.6619(2) 0.4645(2) 0.0495(7) Uani 1 1 d . . .
O3 O 0.33440(18) 0.4325(4) 0.1214(3) 0.1036(16) Uani 1 1 d . . .
O44 O 0.36793(9) 0.6389(2) 0.9651(2) 0.0486(7) Uani 1 1 d . . .
O8 O 0.5781(2) 0.4993(4) 0.8493(7) 0.138(2) Uani 1 1 d . . .
N56 N 0.32927(9) 0.4058(2) 0.7425(3) 0.0382(6) Uani 1 1 d . . .
H56 H 0.3348 0.4681 0.7297 0.046 Uiso 1 1 calc R . .
O38 O 0.44391(10) 0.6407(2) 0.5861(3) 0.0523(7) Uani 1 1 d . . .
O35 O 0.36275(9) 0.6948(2) 0.5001(2) 0.0517(7) Uani 1 1 d . . .
O4 O 0.33003(17) 0.5059(3) 0.3122(5) 0.0925(14) Uani 1 1 d . . .
O23 O 0.54681(10) 0.7925(3) 0.3613(3) 0.0690(10) Uani 1 1 d . . .
O9 O 0.5828(2) 0.4474(6) 0.6569(5) 0.152(3) Uani 1 1 d . . .
C40 C 0.48378(13) 0.6142(3) 0.7642(5) 0.0542(10) Uani 1 1 d . . .
H40A H 0.5025 0.5691 0.8062 0.065 Uiso 1 1 calc R . .
H40B H 0.5018 0.6662 0.7360 0.065 Uiso 1 1 calc R . .
O5 O 0.39364(9) 0.4476(4) 0.2464(4) 0.0981(16) Uani 1 1 d . . .
C30 C 0.26188(9) 0.7371(3) 0.7977(4) 0.0545(11) Uani 1 1 d R . .
H30 H 0.2403 0.6912 0.7974 0.065 Uiso 1 1 calc R . .
C13 C 0.73606(13) 0.6213(3) 0.2007(5) 0.0565(11) Uani 1 1 d . . .
H13A H 0.7541 0.6691 0.2402 0.068 Uiso 1 1 calc R . .
H13B H 0.7550 0.5809 0.1514 0.068 Uiso 1 1 calc R . .
O10 O 0.64277(14) 0.4579(5) 0.7700(6) 0.120(2) Uani 1 1 d . . .
C12 C 0.71547(15) 0.5663(3) 0.2979(4) 0.0573(11) Uani 1 1 d . . .
H12 H 0.7166 0.5011 0.3059 0.069 Uiso 1 1 calc R . .
C16 C 0.66154(13) 0.6678(3) -0.0619(4) 0.0499(10) Uani 1 1 d . . .
H16A H 0.6740 0.7289 -0.0807 0.060 Uiso 1 1 calc R . .
H16B H 0.6563 0.6354 -0.1412 0.060 Uiso 1 1 calc R . .
C57 C 0.29161(11) 0.3984(3) 0.8282(3) 0.0433(8) Uani 1 1 d . . .
H57A H 0.2979 0.4312 0.9065 0.052 Uiso 1 1 calc R . .
H57B H 0.2864 0.3328 0.8482 0.052 Uiso 1 1 calc R . .
C61 C 0.31993(15) 0.3635(3) 0.6206(4) 0.0569(11) Uani 1 1 d . . .
H61A H 0.3154 0.2964 0.6314 0.068 Uiso 1 1 calc R . .
H61B H 0.3447 0.3722 0.5649 0.068 Uiso 1 1 calc R . .
C31 C 0.26488(14) 0.8168(4) 0.7107(6) 0.0680(14) Uani 1 1 d . . .
H31A H 0.2387 0.8188 0.6596 0.082 Uiso 1 1 calc R . .
H31B H 0.2660 0.8745 0.7597 0.082 Uiso 1 1 calc R . .
C39 C 0.46380(14) 0.5696(3) 0.6544(5) 0.0575(11) Uani 1 1 d . . .
H39A H 0.4857 0.5384 0.6034 0.069 Uiso 1 1 calc R . .
H39B H 0.4425 0.5232 0.6810 0.069 Uiso 1 1 calc R . .
C28 C 0.67401(14) 0.5787(3) 0.4760(4) 0.0546(10) Uani 1 1 d . . .
H28A H 0.6961 0.5555 0.5337 0.065 Uiso 1 1 calc R . .
H28B H 0.6582 0.5252 0.4428 0.065 Uiso 1 1 calc R . .
C50 C 0.54481(12) 0.3890(3) 0.1301(3) 0.0482(9) Uani 1 1 d . . .
H50A H 0.5393 0.3222 0.1204 0.058 Uiso 1 1 calc R . .
H50B H 0.5508 0.4148 0.0470 0.058 Uiso 1 1 calc R . .
C18 C 0.59007(14) 0.7216(4) -0.0709(4) 0.0531(10) Uani 1 1 d . . .
H18A H 0.5878 0.6894 -0.1515 0.064 Uiso 1 1 calc R . .
H18B H 0.5976 0.7868 -0.0869 0.064 Uiso 1 1 calc R . .
C54 C 0.57475(15) 0.3689(3) 0.3373(4) 0.0568(11) Uani 1 1 d . . .
H54A H 0.5998 0.3829 0.3897 0.068 Uiso 1 1 calc R . .
H54B H 0.5710 0.3011 0.3357 0.068 Uiso 1 1 calc R . .
C21 C 0.51221(14) 0.7575(5) 0.1720(5) 0.0748(16) Uani 1 1 d . . .
H21 H 0.4900 0.7157 0.1513 0.090 Uiso 1 1 calc R . .
C46 C 0.29457(13) 0.6723(3) 0.9719(4) 0.0517(10) Uani 1 1 d . . .
H46 H 0.2710 0.6324 0.9857 0.062 Uiso 1 1 calc R . .
C36 C 0.39769(15) 0.6781(4) 0.4198(4) 0.0584(12) Uani 1 1 d . . .
H36 H 0.4029 0.7083 0.3432 0.070 Uiso 1 1 calc R . .
C60 C 0.28132(17) 0.4050(4) 0.5629(4) 0.0675(13) Uani 1 1 d . . .
H60A H 0.2756 0.3742 0.4828 0.081 Uiso 1 1 calc R . .
H60B H 0.2866 0.4711 0.5462 0.081 Uiso 1 1 calc R . .
C42 C 0.43977(15) 0.5849(3) 0.9446(5) 0.0595(11) Uani 1 1 d . . .
H42 H 0.4501 0.5237 0.9518 0.071 Uiso 1 1 calc R . .
C59 C 0.24303(15) 0.3954(4) 0.6459(5) 0.0624(12) Uani 1 1 d . . .
H59A H 0.2363 0.3293 0.6576 0.075 Uiso 1 1 calc R . .
H59B H 0.2181 0.4254 0.6068 0.075 Uiso 1 1 calc R . .
C27 C 0.64455(14) 0.6400(4) 0.5430(4) 0.0542(10) Uani 1 1 d . . .
H27A H 0.6342 0.6090 0.6190 0.065 Uiso 1 1 calc R . .
H27B H 0.6595 0.6972 0.5677 0.065 Uiso 1 1 calc R . .
C55 C 0.62052(14) 0.3586(4) 0.1526(6) 0.0711(15) Uani 1 1 d . . .
H55A H 0.6162 0.2917 0.1480 0.107 Uiso 1 1 calc R . .
H55B H 0.6458 0.3718 0.2027 0.107 Uiso 1 1 calc R . .
H55C H 0.6245 0.3833 0.0689 0.107 Uiso 1 1 calc R . .
C58 C 0.25187(13) 0.4394(4) 0.7694(4) 0.0554(10) Uani 1 1 d . . .
H58A H 0.2272 0.4297 0.8250 0.066 Uiso 1 1 calc R . .
H58B H 0.2558 0.5066 0.7583 0.066 Uiso 1 1 calc R . .
C45 C 0.33464(15) 0.6713(4) 1.0427(4) 0.0574(11) Uani 1 1 d . . .
H45A H 0.3413 0.7342 1.0723 0.069 Uiso 1 1 calc R . .
H45B H 0.3317 0.6305 1.1157 0.069 Uiso 1 1 calc R . .
C15 C 0.69196(14) 0.6130(3) 0.0157(4) 0.0561(11) Uani 1 1 d . . .
H15A H 0.6778 0.5563 0.0457 0.067 Uiso 1 1 calc R . .
H15B H 0.7168 0.5946 -0.0350 0.067 Uiso 1 1 calc R . .
C34 C 0.33167(15) 0.7542(5) 0.4457(4) 0.0757(17) Uani 1 1 d . . .
H34A H 0.3239 0.7313 0.3623 0.091 Uiso 1 1 calc R . .
H34B H 0.3436 0.8171 0.4367 0.091 Uiso 1 1 calc R . .
C25 C 0.57592(14) 0.7066(4) 0.5300(4) 0.0588(12) Uani 1 1 d . . .
H25 H 0.5771 0.7262 0.6139 0.071 Uiso 1 1 calc R . .
C43 C 0.40713(15) 0.6290(4) 1.0305(4) 0.0592(12) Uani 1 1 d . . .
H43A H 0.4029 0.5897 1.1045 0.071 Uiso 1 1 calc R . .
H43B H 0.4174 0.6901 1.0582 0.071 Uiso 1 1 calc R . .
C33 C 0.29342(14) 0.7572(5) 0.5250(5) 0.0736(17) Uani 1 1 d . . .
H33 H 0.2675 0.7258 0.5084 0.088 Uiso 1 1 calc R . .
C62 C 0.36756(13) 0.3643(4) 0.8029(5) 0.0684(14) Uani 1 1 d . . .
H62A H 0.3704 0.3886 0.8872 0.103 Uiso 1 1 calc R . .
H62B H 0.3931 0.3799 0.7548 0.103 Uiso 1 1 calc R . .
H62C H 0.3643 0.2972 0.8062 0.103 Uiso 1 1 calc R . .
C37 C 0.42410(16) 0.6069(4) 0.4744(4) 0.0620(12) Uani 1 1 d . . .
H37A H 0.4064 0.5523 0.4939 0.074 Uiso 1 1 calc R . .
H37B H 0.4463 0.5879 0.4146 0.074 Uiso 1 1 calc R . .
C24 C 0.53885(14) 0.7178(4) 0.4460(4) 0.0608(12) Uani 1 1 d . . .
H24A H 0.5341 0.6600 0.3991 0.073 Uiso 1 1 calc R . .
H24B H 0.5129 0.7309 0.4952 0.073 Uiso 1 1 calc R . .
C51 C 0.50564(13) 0.4348(4) 0.1825(5) 0.0635(11) Uani 1 1 d . . .
H51A H 0.4808 0.4213 0.1289 0.076 Uiso 1 1 calc R . .
H51B H 0.5098 0.5024 0.1841 0.076 Uiso 1 1 calc R . .
C53 C 0.53562(18) 0.4130(4) 0.3934(4) 0.0698(14) Uani 1 1 d . . .
H53A H 0.5303 0.3857 0.4760 0.084 Uiso 1 1 calc R . .
H53B H 0.5409 0.4797 0.4048 0.084 Uiso 1 1 calc R . .
C19 C 0.54893(13) 0.7164(4) -0.0041(4) 0.0594(12) Uani 1 1 d . . .
H19A H 0.5255 0.7352 -0.0600 0.071 Uiso 1 1 calc R . .
H19B H 0.5436 0.6522 0.0228 0.071 Uiso 1 1 calc R . .
C22 C 0.51346(16) 0.8125(6) 0.2784(6) 0.093(2) Uani 1 1 d . . .
H22 H 0.4933 0.8600 0.2935 0.112 Uiso 1 1 calc R . .
C52 C 0.49682(16) 0.4000(4) 0.3139(5) 0.0696(13) Uani 1 1 d . . .
H52A H 0.4726 0.4345 0.3499 0.083 Uiso 1 1 calc R . .
H52B H 0.4891 0.3339 0.3112 0.083 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
Cl2 O3 1.411(3) . ?
Cl2 O1 1.416(3) . ?
Cl2 O5 1.417(3) . ?
Cl2 O4 1.426(4) . ?
Cl7 O8 1.387(5) . ?
Cl7 O10 1.396(4) . ?
Cl7 O9 1.395(4) . ?
Cl7 O6 1.415(4) . ?
O11 C12 1.406(5) . ?
O11 C28 1.424(5) . ?
O29 C30 1.403(5) . ?
O29 C46 1.414(5) . ?
O41 C42 1.411(6) . ?
O41 C40 1.459(5) . ?
O14 C15 1.412(5) . ?
O14 C13 1.460(5) . ?
O17 C18 1.426(4) . ?
O17 C16 1.432(4) . ?
O32 C33 1.420(6) . ?
O32 C31 1.438(5) . ?
O20 C19 1.388(5) . ?
O20 C21 1.449(5) . ?
N49 C54 1.473(5) . ?
N49 C50 1.482(4) . ?
N49 C55 1.486(4) . ?
O26 C27 1.423(5) . ?
O26 C25 1.426(5) . ?
O44 C45 1.419(5) . ?
O44 C43 1.425(5) . ?
N56 C61 1.482(5) . ?
N56 C62 1.494(5) . ?
N56 C57 1.504(4) . ?
O38 C39 1.414(6) . ?
O38 C37 1.442(5) . ?
O35 C36 1.419(5) . ?
O35 C34 1.428(6) . ?
O23 C22 1.408(6) . ?
O23 C24 1.440(7) . ?
C40 C39 1.489(7) . ?
C30 C31 1.493(7) . ?
C13 C12 1.468(7) . ?
C16 C15 1.498(7) . ?
C57 C58 1.520(6) . ?
C61 C60 1.490(7) . ?
C28 C27 1.472(7) . ?
C50 C51 1.507(6) . ?
C18 C19 1.480(6) . ?
C54 C53 1.511(7) . ?
C21 C22 1.399(9) . ?
C46 C45 1.472(6) . ?
C36 C37 1.449(8) . ?
C60 C59 1.505(7) . ?
C42 C43 1.522(7) . ?
C59 C58 1.504(7) . ?
C34 C33 1.474(7) . ?
C25 C24 1.483(6) . ?
C51 C52 1.530(7) . ?
C53 C52 1.501(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cl2 O1 109.0(2) . . ?
O3 Cl2 O5 109.3(3) . . ?
O1 Cl2 O5 110.8(3) . . ?
O3 Cl2 O4 109.9(3) . . ?
O1 Cl2 O4 111.0(2) . . ?
O5 Cl2 O4 106.7(3) . . ?
O8 Cl7 O10 110.3(4) . . ?
O8 Cl7 O9 105.4(5) . . ?
O10 Cl7 O9 107.4(4) . . ?
O8 Cl7 O6 111.9(3) . . ?
O10 Cl7 O6 112.6(3) . . ?
O9 Cl7 O6 108.9(4) . . ?
C12 O11 C28 110.7(3) . . ?
C30 O29 C46 112.2(3) . . ?
C42 O41 C40 115.3(3) . . ?
C15 O14 C13 115.8(3) . . ?
C18 O17 C16 112.5(3) . . ?
C33 O32 C31 111.3(4) . . ?
C19 O20 C21 108.5(3) . . ?
C54 N49 C50 111.6(3) . . ?
C54 N49 C55 112.6(3) . . ?
C50 N49 C55 109.8(3) . . ?
C27 O26 C25 112.2(3) . . ?
C45 O44 C43 112.1(3) . . ?
C61 N56 C62 112.3(4) . . ?
C61 N56 C57 111.1(3) . . ?
C62 N56 C57 109.6(3) . . ?
C39 O38 C37 112.2(4) . . ?
C36 O35 C34 112.3(3) . . ?
C22 O23 C24 115.5(5) . . ?
O41 C40 C39 112.6(3) . . ?
O29 C30 C31 108.2(3) . . ?
O14 C13 C12 113.2(3) . . ?
O11 C12 C13 107.6(4) . . ?
O17 C16 C15 109.7(3) . . ?
N56 C57 C58 111.1(3) . . ?
N56 C61 C60 111.4(3) . . ?
O32 C31 C30 114.2(4) . . ?
O38 C39 C40 106.5(4) . . ?
O11 C28 C27 110.1(3) . . ?
N49 C50 C51 112.0(3) . . ?
O17 C18 C19 108.7(3) . . ?
N49 C54 C53 111.6(3) . . ?
C22 C21 O20 109.4(5) . . ?
O29 C46 C45 109.7(3) . . ?
O35 C36 C37 108.4(4) . . ?
C61 C60 C59 111.3(4) . . ?
O41 C42 C43 110.0(4) . . ?
C60 C59 C58 109.9(4) . . ?
O26 C27 C28 109.1(3) . . ?
C59 C58 C57 110.8(4) . . ?
O44 C45 C46 109.0(3) . . ?
O14 C15 C16 109.9(3) . . ?
O35 C34 C33 109.6(4) . . ?
O26 C25 C24 109.1(3) . . ?
O44 C43 C42 108.8(4) . . ?
O32 C33 C34 109.8(4) . . ?
O38 C37 C36 110.1(4) . . ?
O23 C24 C25 109.5(4) . . ?
C50 C51 C52 110.5(4) . . ?
C52 C53 C54 112.2(4) . . ?
O20 C19 C18 109.6(3) . . ?
C21 C22 O23 115.2(6) . . ?
C53 C52 C51 110.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        73.28
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.062
