# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

data_Global
_publ_contact_author_name        'Prof. J. N. Moorthy'
_publ_contact_author_address     
;Departmet of chemistry
Indian Institute of Technology - Kanpur
Kanpur - 208 016
INDIA
;
_publ_contact_author_email       moorthy@iitk.ac.in
_publ_contact_author_phone       +915122597438
_publ_contact_author_fax         +915122597436
loop_
_publ_author_name
_publ_author_address


'Prof. J. N. Moorthy, '
;Departmet of chemistry
Indian Institute of Technology - Kanpur
Kanpur - 208 016
INDIA
;
'Alankriti Bajpai'
;Department of Chemistry
Indian Institute of Technology
Kanpur 208 016
INDIA
;
'Prof. P. Venugopalan'
;Department of Chemistry
Panjab University
Chandigrah 560017
INDIA
;
data_MeBTB-TCE-Without-Squeeze

_audit_creation_method           'Manual edit of SHELXL-97 CIF'
_chemical_name_systematic        
;
1,3,5-Tris(2,6-dimethyl-4-carboxyphenyl)benzene + 2*1,1,2,2-tetrachloroethane
;
_chemical_name_common            MeBTB
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H34 Cl8 O6'
_chemical_formula_weight         858.28

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   50.850(16)
_cell_length_b                   15.260(5)
_cell_length_c                   14.006(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10868(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3520
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER AXS KAPPA APEX-II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            53389
_diffrn_reflns_av_R_equivalents  0.1486
_diffrn_reflns_av_sigmaI/netI    0.1067
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9426
_reflns_number_gt                4559
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97

_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)+(0.1438P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9426
_refine_ls_number_parameters     548
_refine_ls_number_restraints     128
_refine_ls_R_factor_all          0.2673
_refine_ls_R_factor_gt           0.1833
_refine_ls_wR_factor_ref         0.4562
_refine_ls_wR_factor_gt          0.4279
_refine_ls_goodness_of_fit_ref   1.672
_refine_ls_restrained_S_all      1.689
_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 0.3262(3) -0.0215(13) 0.2216(13) 0.201(7) Uiso 0.27 1 d PDU A 1
Cl2 Cl 0.3677(4) 0.0231(14) 0.3431(14) 0.248(9) Uiso 0.27 1 d PDU A 1
Cl3 Cl 0.3709(9) 0.054(3) 0.0526(14) 0.45(2) Uiso 0.27 1 d PDU A 1
Cl4 Cl 0.3917(6) 0.1343(18) 0.216(2) 0.409(18) Uiso 0.27 1 d PDU A 1
C34 C 0.3598(3) 0.0008(12) 0.2245(13) 0.339(17) Uiso 0.27 1 d PDU A 1
H34A H 0.3705 -0.0485 0.1979 0.407 Uiso 0.27 1 calc PR A 1
C35 C 0.3637(4) 0.0841(15) 0.1699(16) 0.356(17) Uiso 0.27 1 d PDU A 1
H35A H 0.3479 0.1231 0.1737 0.427 Uiso 0.27 1 calc PR A 1
Cl21 Cl 0.3591(6) -0.1372(12) -0.068(3) 0.354(17) Uiso 0.23 1 d PDU B 2
Cl22 Cl 0.3383(3) -0.2955(10) -0.1363(11) 0.143(5) Uiso 0.23 1 d PDU B 2
Cl23 Cl 0.4025(5) -0.204(2) -0.020(3) 0.42(2) Uiso 0.23 1 d PDU B 2
Cl24 Cl 0.3855(5) -0.3446(18) -0.133(2) 0.282(13) Uiso 0.23 1 d PDU B 2
C44 C 0.3532(4) -0.2461(16) -0.0380(14) 0.290(17) Uiso 0.23 1 d PDU B 2
H44A H 0.3423 -0.2516 0.0211 0.349 Uiso 0.23 1 calc PR B 2
C45 C 0.3796(4) -0.2887(18) -0.0273(17) 0.302(17) Uiso 0.23 1 d PDU B 2
H45A H 0.3804 -0.3283 0.0296 0.363 Uiso 0.23 1 calc PR B 2
Cl1A Cl 0.4474(13) -0.142(4) 0.324(4) 0.74(3) Uiso 0.33 1 d PDU C 3
Cl2A Cl 0.4497(13) -0.201(3) 0.134(4) 0.77(3) Uiso 0.33 1 d PDU C 3
Cl3A Cl 0.4656(14) -0.001(3) 0.073(4) 0.72(3) Uiso 0.33 1 d PDU C 3
Cl4A Cl 0.4677(15) 0.039(3) 0.268(4) 0.75(3) Uiso 0.33 1 d PDU C 3
C34A C 0.4463(8) -0.108(3) 0.205(4) 0.75(3) Uiso 0.33 1 d PDU C 3
H34B H 0.4292 -0.0784 0.1913 0.897 Uiso 0.33 1 calc PR C 3
C35A C 0.4688(8) -0.047(2) 0.186(4) 0.74(3) Uiso 0.33 1 d PDU C 3
H35B H 0.4859 -0.0786 0.1917 0.893 Uiso 0.33 1 calc PR C 3
Cl17 Cl 0.4081(4) 0.2576(13) -0.2508(15) 0.164(8) Uiso 0.17 1 d PDU D 4
Cl18 Cl 0.4080(4) 0.1330(15) -0.1044(16) 0.179(9) Uiso 0.17 1 d PDU D 4
Cl19 Cl 0.4520(4) 0.2304(15) -0.0796(19) 0.184(9) Uiso 0.17 1 d PDU D 4
Cl20 Cl 0.4662(5) 0.0781(17) -0.178(2) 0.255(14) Uiso 0.17 1 d PDU D 4
C42 C 0.4226(4) 0.1610(13) -0.2120(14) 0.181(15) Uiso 0.17 1 d PDU D 4
H42A H 0.4207 0.1131 -0.2603 0.217 Uiso 0.17 1 calc PR D 4
C43 C 0.4509(3) 0.1801(15) -0.1914(15) 0.191(15) Uiso 0.17 1 d PDU D 4
H43A H 0.4593 0.2165 -0.2423 0.229 Uiso 0.17 1 calc PR D 4
Cl5 Cl 0.3915(11) 0.136(2) -0.068(3) 0.54(3) Uiso 0.28 1 d PDU E 5
Cl6 Cl 0.3632(6) 0.1306(17) 0.104(2) 0.316(15) Uiso 0.28 1 d PDU E 5
Cl7 Cl 0.4027(7) -0.001(2) 0.127(3) 0.49(2) Uiso 0.28 1 d PDU E 5
Cl8 Cl 0.3598(6) -0.0919(16) 0.050(2) 0.318(12) Uiso 0.28 1 d PDU E 5
C36 C 0.3706(6) 0.0719(15) 0.001(2) 0.392(19) Uiso 0.28 1 d PDU E 5
H36A H 0.3540 0.0603 -0.0356 0.471 Uiso 0.28 1 calc PR E 5
C37 C 0.3835(5) -0.0130(15) 0.025(2) 0.389(19) Uiso 0.28 1 d PDU E 5
H37A H 0.3947 -0.0329 -0.0293 0.467 Uiso 0.28 1 calc PR E 5
Cl13 Cl 0.4568(4) 0.2768(13) -0.1360(15) 0.182(7) Uiso 0.22 1 d PDU F 6
Cl14 Cl 0.4544(8) 0.179(3) 0.033(2) 0.45(2) Uiso 0.22 1 d PDU F 6
Cl15 Cl 0.4355(7) 0.0817(16) -0.149(3) 0.343(16) Uiso 0.22 1 d PDU F 6
Cl16 Cl 0.4012(5) 0.2192(16) -0.1938(19) 0.236(10) Uiso 0.22 1 d PDU F 6
C40 C 0.4356(5) 0.2313(16) -0.0525(14) 0.297(17) Uiso 0.22 1 d PDU F 6
H40A H 0.4250 0.2788 -0.0216 0.357 Uiso 0.22 1 calc PR F 6
C41 C 0.4175(4) 0.1675(15) -0.1003(17) 0.299(17) Uiso 0.22 1 d PDU F 6
H41A H 0.4045 0.1443 -0.0532 0.359 Uiso 0.22 1 calc PR F 6
Cl5A Cl 0.3246(3) -0.0665(11) 0.1986(11) 0.103(5) Uiso 0.17 1 d PDU G 7
Cl6A Cl 0.3716(6) -0.1002(18) 0.296(4) 0.40(2) Uiso 0.17 1 d PDU G 7
Cl7A Cl 0.3843(9) 0.070(2) 0.322(3) 0.35(2) Uiso 0.17 1 d PDU G 7
Cl8A Cl 0.3579(5) 0.1304(12) 0.1589(16) 0.142(7) Uiso 0.17 1 d PDU G 7
C36A C 0.3572(4) -0.0329(11) 0.211(2) 0.267(18) Uiso 0.17 1 d PDU G 7
H36B H 0.3669 -0.0338 0.1487 0.321 Uiso 0.17 1 calc PR G 7
C37A C 0.3560(5) 0.0574(12) 0.2537(16) 0.266(18) Uiso 0.17 1 d PDU G 7
H37B H 0.3397 0.0663 0.2925 0.320 Uiso 0.17 1 calc PR G 7
Cl9 Cl 0.3202(11) -0.229(3) -0.042(4) 0.69(3) Uiso 0.33 1 d PDU H 8
Cl10 Cl 0.3346(10) -0.352(3) -0.180(3) 0.51(2) Uiso 0.33 1 d PDU H 8
Cl11 Cl 0.3795(13) -0.250(4) 0.047(4) 0.73(3) Uiso 0.33 1 d PDU H 8
Cl12 Cl 0.3871(12) -0.388(4) -0.082(5) 0.73(4) Uiso 0.33 1 d PDU H 8
C38 C 0.3470(8) -0.278(3) -0.098(3) 0.65(3) Uiso 0.33 1 d PDU H 8
H38A H 0.3579 -0.2327 -0.1304 0.777 Uiso 0.33 1 calc PR H 8
C39 C 0.3632(8) -0.326(3) -0.025(3) 0.66(3) Uiso 0.33 1 d PDU H 8
H39A H 0.3517 -0.3645 0.0151 0.797 Uiso 0.33 1 calc PR H 8
O1 O 0.47880(15) -0.0619(7) 0.5676(7) 0.164(4) Uani 1 1 d . . .
H1A H 0.4940 -0.0540 0.5460 0.246 Uiso 1 1 calc R . .
O2 O 0.47269(15) 0.0627(7) 0.4906(7) 0.173(4) Uani 1 1 d . . .
O3 O 0.24191(9) -0.1479(3) 0.2559(3) 0.0539(12) Uani 1 1 d . . .
H4A H 0.2333 -0.1763 0.2151 0.081 Uiso 1 1 calc R . .
O4 O 0.24345(9) -0.2787(3) 0.3295(3) 0.0506(12) Uani 1 1 d . . .
O5 O 0.28366(9) 0.2639(3) 1.1274(3) 0.0588(13) Uani 1 1 d . . .
O6 O 0.27530(9) 0.1309(3) 1.1854(3) 0.0602(13) Uani 1 1 d . . .
H6A H 0.2696 0.1600 1.2317 0.090 Uiso 1 1 calc R . .
C1 C 0.35661(13) -0.0065(5) 0.6589(5) 0.0614(19) Uani 1 1 d . . .
C2 C 0.34802(14) 0.0264(4) 0.7460(5) 0.0582(18) Uani 1 1 d . . .
H2A H 0.3605 0.0485 0.7905 0.070 Uiso 1 1 calc R . .
C3 C 0.32159(13) 0.0276(4) 0.7687(4) 0.0486(16) Uani 1 1 d . . .
C4 C 0.30391(13) -0.0069(4) 0.7058(4) 0.0453(15) Uani 1 1 d . . .
H4B H 0.2857 -0.0076 0.7217 0.054 Uiso 1 1 calc R . .
C5 C 0.31230(13) -0.0413(4) 0.6176(4) 0.0469(16) Uani 1 1 d . . .
C6 C 0.33865(13) -0.0400(4) 0.5967(5) 0.0581(18) Uani 1 1 d . . .
H6B H 0.3445 -0.0629 0.5373 0.070 Uiso 1 1 calc R . .
C7 C 0.38498(14) -0.0027(6) 0.6326(5) 0.068(2) Uani 1 1 d . . .
C8 C 0.39363(17) 0.0652(7) 0.5737(8) 0.105(3) Uani 1 1 d . . .
C9 C 0.4202(2) 0.0635(8) 0.5437(9) 0.125(4) Uani 1 1 d . . .
H9A H 0.4265 0.1070 0.5009 0.150 Uiso 1 1 calc R . .
C10 C 0.43736(19) -0.0019(8) 0.5765(8) 0.106(3) Uani 1 1 d . . .
C11 C 0.42822(18) -0.0632(8) 0.6331(9) 0.122(4) Uani 1 1 d . . .
H11A H 0.4400 -0.1071 0.6550 0.147 Uiso 1 1 calc R . .
C12 C 0.40210(19) -0.0670(8) 0.6626(7) 0.114(4) Uani 1 1 d . . .
C13 C 0.4644(2) 0.0005(10) 0.5434(10) 0.129(4) Uani 1 1 d . . .
C14 C 0.3761(2) 0.1384(8) 0.5452(12) 0.184(7) Uani 1 1 d . . .
H14A H 0.3776 0.1483 0.4763 0.276 Uiso 1 1 calc R . .
H14B H 0.3812 0.1917 0.5795 0.276 Uiso 1 1 calc R . .
H14C H 0.3579 0.1236 0.5611 0.276 Uiso 1 1 calc R . .
C15 C 0.3925(2) -0.1385(10) 0.7247(14) 0.232(10) Uani 1 1 d . . .
H15A H 0.3829 -0.1135 0.7789 0.348 Uiso 1 1 calc R . .
H15B H 0.4075 -0.1726 0.7482 0.348 Uiso 1 1 calc R . .
H15C H 0.3808 -0.1768 0.6881 0.348 Uiso 1 1 calc R . .
C16 C 0.29381(12) -0.0791(4) 0.5463(4) 0.0447(15) Uani 1 1 d . . .
C17 C 0.28662(14) -0.0304(4) 0.4653(5) 0.0540(17) Uani 1 1 d . . .
C18 C 0.27092(13) -0.0699(4) 0.3961(4) 0.0476(16) Uani 1 1 d . . .
H18A H 0.2653 -0.0365 0.3426 0.057 Uiso 1 1 calc R . .
C19 C 0.26352(12) -0.1551(4) 0.4034(4) 0.0448(15) Uani 1 1 d . . .
C20 C 0.26969(12) -0.2035(4) 0.4831(4) 0.0498(16) Uani 1 1 d . . .
H20A H 0.2635 -0.2620 0.4889 0.060 Uiso 1 1 calc R . .
C21 C 0.28518(12) -0.1666(4) 0.5560(4) 0.0460(16) Uani 1 1 d . . .
C22 C 0.24817(12) -0.1994(4) 0.3268(4) 0.0478(16) Uani 1 1 d . . .
C23 C 0.29478(16) 0.0649(4) 0.4565(5) 0.069(2) Uani 1 1 d . . .
H23A H 0.3124 0.0683 0.4284 0.104 Uiso 1 1 calc R . .
H23B H 0.2949 0.0920 0.5199 0.104 Uiso 1 1 calc R . .
H23C H 0.2823 0.0959 0.4154 0.104 Uiso 1 1 calc R . .
C24 C 0.29328(14) -0.2197(4) 0.6433(4) 0.0566(18) Uani 1 1 d . . .
H24A H 0.2906 -0.1845 0.7010 0.085 Uiso 1 1 calc R . .
H24B H 0.3119 -0.2357 0.6380 0.085 Uiso 1 1 calc R . .
H24C H 0.2826 -0.2730 0.6470 0.085 Uiso 1 1 calc R . .
C25 C 0.31312(12) 0.0670(4) 0.8629(4) 0.0483(16) Uani 1 1 d . . .
C26 C 0.31648(12) 0.1565(4) 0.8794(4) 0.0456(16) Uani 1 1 d . . .
C27 C 0.30739(12) 0.1918(4) 0.9640(4) 0.0492(16) Uani 1 1 d . . .
H27A H 0.3098 0.2525 0.9763 0.059 Uiso 1 1 calc R . .
C28 C 0.29468(12) 0.1390(4) 1.0321(4) 0.0478(16) Uani 1 1 d . . .
C29 C 0.29199(13) 0.0511(4) 1.0148(4) 0.0492(16) Uani 1 1 d . . .
H29A H 0.2839 0.0155 1.0621 0.059 Uiso 1 1 calc R . .
C30 C 0.30051(13) 0.0120(4) 0.9312(4) 0.0476(16) Uani 1 1 d . . .
C31 C 0.28415(12) 0.1848(5) 1.1189(4) 0.0470(16) Uani 1 1 d . . .
C32 C 0.32928(15) 0.2168(4) 0.8083(5) 0.0605(19) Uani 1 1 d . . .
H32A H 0.3242 0.2774 0.8221 0.091 Uiso 1 1 calc R . .
H32B H 0.3236 0.2011 0.7437 0.091 Uiso 1 1 calc R . .
H32C H 0.3484 0.2110 0.8128 0.091 Uiso 1 1 calc R . .
C33 C 0.29688(16) -0.0859(4) 0.9162(5) 0.068(2) Uani 1 1 d . . .
H33A H 0.2976 -0.1160 0.9780 0.103 Uiso 1 1 calc R . .
H33B H 0.3109 -0.1082 0.8749 0.103 Uiso 1 1 calc R . .
H33C H 0.2798 -0.0968 0.8860 0.103 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
Cl1 C34 1.743(7) . ?
Cl2 C34 1.742(7) . ?
Cl3 C35 1.743(7) . ?
Cl4 C35 1.738(7) . ?
C34 C35 1.496(7) . ?
C34 H34A 1.0000 . ?
C35 H35A 1.0000 . ?
Cl21 C44 1.740(7) . ?
Cl22 C44 1.742(7) . ?
Cl23 C45 1.739(7) . ?
Cl24 C45 1.740(7) . ?
C44 C45 1.502(7) . ?
C44 H44A 1.0000 . ?
C45 H45A 1.0000 . ?
Cl1A C34A 1.742(7) . ?
Cl2A C34A 1.739(7) . ?
Cl3A C35A 1.738(7) . ?
Cl4A C35A 1.740(7) . ?
C34A C35A 1.502(7) . ?
C34A H34B 1.0000 . ?
C35A H35B 1.0000 . ?
Cl17 C42 1.735(7) . ?
Cl18 C42 1.734(7) . ?
Cl19 C43 1.744(7) . ?
Cl20 C43 1.749(7) . ?
C42 C43 1.495(7) . ?
C42 H42A 1.0000 . ?
C43 H43A 1.0000 . ?
Cl5 C36 1.736(7) . ?
Cl6 C36 1.735(7) . ?
Cl7 C37 1.738(7) . ?
Cl8 C37 1.740(7) . ?
C36 C37 1.492(7) . ?
C36 H36A 1.0000 . ?
C37 H37A 1.0000 . ?
Cl13 C40 1.737(7) . ?
Cl14 C40 1.731(7) . ?
Cl15 C41 1.738(7) . ?
Cl16 C41 1.738(7) . ?
C40 C41 1.497(7) . ?
C40 H40A 1.0000 . ?
C41 H41A 1.0000 . ?
Cl5A C36A 1.740(7) . ?
Cl6A C36A 1.738(7) . ?
Cl7A C37A 1.735(7) . ?
Cl8A C37A 1.736(7) . ?
C36A C37A 1.505(7) . ?
C36A H36B 1.0000 . ?
C37A H37B 1.0000 . ?
Cl9 C38 1.740(7) . ?
Cl10 C38 1.740(7) . ?
Cl11 C39 1.741(7) . ?
Cl12 C39 1.740(7) . ?
C38 C39 1.499(7) . ?
C38 H38A 1.0000 . ?
C39 H39A 1.0000 . ?
O1 C13 1.249(12) . ?
O1 H1A 0.8400 . ?
O2 C13 1.276(13) . ?
O3 C22 1.306(7) . ?
O3 H4A 0.8400 . ?
O4 C22 1.234(7) . ?
O5 C31 1.213(7) . ?
O6 C31 1.321(7) . ?
O6 H6A 0.8400 . ?
C1 C6 1.361(9) . ?
C1 C2 1.390(9) . ?
C1 C7 1.490(10) . ?
C2 C3 1.381(9) . ?
C2 H2A 0.9500 . ?
C3 C4 1.363(8) . ?
C3 C25 1.513(8) . ?
C4 C5 1.409(8) . ?
C4 H4B 0.9500 . ?
C5 C6 1.372(9) . ?
C5 C16 1.488(8) . ?
C6 H6B 0.9500 . ?
C7 C12 1.378(12) . ?
C7 C8 1.396(11) . ?
C8 C9 1.415(12) . ?
C8 C14 1.483(13) . ?
C9 C10 1.403(14) . ?
C9 H9A 0.9500 . ?
C10 C11 1.311(13) . ?
C10 C13 1.450(14) . ?
C11 C12 1.392(13) . ?
C11 H11A 0.9500 . ?
C12 C15 1.477(14) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.405(8) . ?
C16 C21 1.411(8) . ?
C17 C18 1.394(8) . ?
C17 C23 1.517(9) . ?
C18 C19 1.357(8) . ?
C18 H18A 0.9500 . ?
C19 C20 1.375(8) . ?
C19 C22 1.489(8) . ?
C20 C21 1.407(8) . ?
C20 H20A 0.9500 . ?
C21 C24 1.524(8) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.396(8) . ?
C25 C30 1.425(9) . ?
C26 C27 1.381(8) . ?
C26 C32 1.503(9) . ?
C27 C28 1.407(8) . ?
C27 H27A 0.9500 . ?
C28 C29 1.370(8) . ?
C28 C31 1.501(9) . ?
C29 C30 1.384(8) . ?
C29 H29A 0.9500 . ?
C30 C33 1.521(9) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C35 C34 Cl2 106.9(6) . . ?
C35 C34 Cl1 106.4(6) . . ?
Cl2 C34 Cl1 106.6(6) . . ?
C35 C34 H34A 112.2 . . ?
Cl2 C34 H34A 112.2 . . ?
Cl1 C34 H34A 112.2 . . ?
C34 C35 Cl4 107.0(6) . . ?
C34 C35 Cl3 106.6(7) . . ?
Cl4 C35 Cl3 107.1(6) . . ?
C34 C35 H35A 111.9 . . ?
Cl4 C35 H35A 111.9 . . ?
Cl3 C35 H35A 111.9 . . ?
C45 C44 Cl21 106.4(6) . . ?
C45 C44 Cl22 106.3(5) . . ?
Cl21 C44 Cl22 107.3(5) . . ?
C45 C44 H44A 112.2 . . ?
Cl21 C44 H44A 112.2 . . ?
Cl22 C44 H44A 112.2 . . ?
C44 C45 Cl23 106.5(6) . . ?
C44 C45 Cl24 106.3(5) . . ?
Cl23 C45 Cl24 107.2(5) . . ?
C44 C45 H45A 112.1 . . ?
Cl23 C45 H45A 112.1 . . ?
Cl24 C45 H45A 112.1 . . ?
C35A C34A Cl2A 109.5(7) . . ?
C35A C34A Cl1A 109.1(7) . . ?
Cl2A C34A Cl1A 107.2(6) . . ?
C35A C34A H34B 110.3 . . ?
Cl2A C34A H34B 110.3 . . ?
Cl1A C34A H34B 110.3 . . ?
C34A C35A Cl3A 109.6(7) . . ?
C34A C35A Cl4A 109.2(7) . . ?
Cl3A C35A Cl4A 107.2(6) . . ?
C34A C35A H35B 110.2 . . ?
Cl3A C35A H35B 110.2 . . ?
Cl4A C35A H35B 110.2 . . ?
C43 C42 Cl18 107.0(6) . . ?
C43 C42 Cl17 107.7(6) . . ?
Cl18 C42 Cl17 107.4(6) . . ?
C43 C42 H42A 111.5 . . ?
Cl18 C42 H42A 111.5 . . ?
Cl17 C42 H42A 111.5 . . ?
C42 C43 Cl19 106.9(6) . . ?
C42 C43 Cl20 106.0(6) . . ?
Cl19 C43 Cl20 106.3(6) . . ?
C42 C43 H43A 112.4 . . ?
Cl19 C43 H43A 112.4 . . ?
Cl20 C43 H43A 112.4 . . ?
C37 C36 Cl6 110.6(7) . . ?
C37 C36 Cl5 110.3(7) . . ?
Cl6 C36 Cl5 107.5(6) . . ?
C37 C36 H36A 109.5 . . ?
Cl6 C36 H36A 109.5 . . ?
Cl5 C36 H36A 109.5 . . ?
C36 C37 Cl7 110.3(7) . . ?
C36 C37 Cl8 110.0(7) . . ?
Cl7 C37 Cl8 107.2(6) . . ?
C36 C37 H37A 109.8 . . ?
Cl7 C37 H37A 109.8 . . ?
Cl8 C37 H37A 109.8 . . ?
C41 C40 Cl14 110.3(7) . . ?
C41 C40 Cl13 109.9(6) . . ?
Cl14 C40 Cl13 107.8(6) . . ?
C41 C40 H40A 109.6 . . ?
Cl14 C40 H40A 109.6 . . ?
Cl13 C40 H40A 109.6 . . ?
C40 C41 Cl15 110.1(6) . . ?
C40 C41 Cl16 109.5(6) . . ?
Cl15 C41 Cl16 107.2(6) . . ?
C40 C41 H41A 110.0 . . ?
Cl15 C41 H41A 110.0 . . ?
Cl16 C41 H41A 110.0 . . ?
C37A C36A Cl6A 106.4(6) . . ?
C37A C36A Cl5A 105.7(6) . . ?
Cl6A C36A Cl5A 107.2(6) . . ?
C37A C36A H36B 112.4 . . ?
Cl6A C36A H36B 112.4 . . ?
Cl5A C36A H36B 112.4 . . ?
C36A C37A Cl7A 106.6(6) . . ?
C36A C37A Cl8A 106.2(6) . . ?
Cl7A C37A Cl8A 107.6(6) . . ?
C36A C37A H37B 112.0 . . ?
Cl7A C37A H37B 112.0 . . ?
Cl8A C37A H37B 112.0 . . ?
C39 C38 Cl10 109.6(7) . . ?
C39 C38 Cl9 109.5(7) . . ?
Cl10 C38 Cl9 107.2(6) . . ?
C39 C38 H38A 110.2 . . ?
Cl10 C38 H38A 110.2 . . ?
Cl9 C38 H38A 110.2 . . ?
C38 C39 Cl12 109.5(7) . . ?
C38 C39 Cl11 109.5(7) . . ?
Cl12 C39 Cl11 107.1(6) . . ?
C38 C39 H39A 110.2 . . ?
Cl12 C39 H39A 110.2 . . ?
Cl11 C39 H39A 110.2 . . ?
C13 O1 H1A 109.5 . . ?
C22 O3 H4A 109.5 . . ?
C31 O6 H6A 109.5 . . ?
C6 C1 C2 119.1(6) . . ?
C6 C1 C7 120.4(6) . . ?
C2 C1 C7 120.5(7) . . ?
C3 C2 C1 120.8(6) . . ?
C3 C2 H2A 119.6 . . ?
C1 C2 H2A 119.6 . . ?
C4 C3 C2 119.2(6) . . ?
C4 C3 C25 121.9(6) . . ?
C2 C3 C25 118.8(6) . . ?
C3 C4 C5 120.7(6) . . ?
C3 C4 H4B 119.7 . . ?
C5 C4 H4B 119.7 . . ?
C6 C5 C4 118.5(6) . . ?
C6 C5 C16 118.6(5) . . ?
C4 C5 C16 122.8(6) . . ?
C1 C6 C5 121.6(6) . . ?
C1 C6 H6B 119.2 . . ?
C5 C6 H6B 119.2 . . ?
C12 C7 C8 120.7(8) . . ?
C12 C7 C1 120.6(7) . . ?
C8 C7 C1 118.7(7) . . ?
C7 C8 C9 117.5(9) . . ?
C7 C8 C14 121.9(8) . . ?
C9 C8 C14 120.5(9) . . ?
C10 C9 C8 120.7(10) . . ?
C10 C9 H9A 119.7 . . ?
C8 C9 H9A 119.7 . . ?
C11 C10 C9 119.0(9) . . ?
C11 C10 C13 123.2(11) . . ?
C9 C10 C13 117.8(11) . . ?
C10 C11 C12 123.2(10) . . ?
C10 C11 H11A 118.4 . . ?
C12 C11 H11A 118.4 . . ?
C7 C12 C11 118.8(9) . . ?
C7 C12 C15 119.9(8) . . ?
C11 C12 C15 121.3(10) . . ?
O1 C13 O2 122.0(10) . . ?
O1 C13 C10 116.7(12) . . ?
O2 C13 C10 121.2(12) . . ?
C8 C14 H14A 109.5 . . ?
C8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C21 119.8(6) . . ?
C17 C16 C5 120.1(6) . . ?
C21 C16 C5 119.9(5) . . ?
C18 C17 C16 118.8(6) . . ?
C18 C17 C23 121.0(6) . . ?
C16 C17 C23 120.2(6) . . ?
C19 C18 C17 121.4(6) . . ?
C19 C18 H18A 119.3 . . ?
C17 C18 H18A 119.3 . . ?
C18 C19 C20 120.9(6) . . ?
C18 C19 C22 121.7(6) . . ?
C20 C19 C22 117.4(6) . . ?
C19 C20 C21 120.1(6) . . ?
C19 C20 H20A 120.0 . . ?
C21 C20 H20A 120.0 . . ?
C20 C21 C16 118.9(5) . . ?
C20 C21 C24 121.4(6) . . ?
C16 C21 C24 119.7(5) . . ?
O4 C22 O3 124.4(6) . . ?
O4 C22 C19 121.7(6) . . ?
O3 C22 C19 113.7(6) . . ?
C17 C23 H23A 109.5 . . ?
C17 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C17 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C30 121.4(5) . . ?
C26 C25 C3 119.9(5) . . ?
C30 C25 C3 118.6(6) . . ?
C27 C26 C25 118.9(6) . . ?
C27 C26 C32 118.3(6) . . ?
C25 C26 C32 122.8(5) . . ?
C26 C27 C28 120.8(6) . . ?
C26 C27 H27A 119.6 . . ?
C28 C27 H27A 119.6 . . ?
C29 C28 C27 119.1(6) . . ?
C29 C28 C31 124.3(6) . . ?
C27 C28 C31 116.5(6) . . ?
C28 C29 C30 122.7(6) . . ?
C28 C29 H29A 118.6 . . ?
C30 C29 H29A 118.6 . . ?
C29 C30 C25 117.1(6) . . ?
C29 C30 C33 120.2(6) . . ?
C25 C30 C33 122.7(5) . . ?
O5 C31 O6 122.9(6) . . ?
O5 C31 C28 123.4(5) . . ?
O6 C31 C28 113.7(6) . . ?
C26 C32 H32A 109.5 . . ?
C26 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C26 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl2 C34 C35 Cl4 39.0(17) . . . . ?
Cl1 C34 C35 Cl4 152.6(17) . . . . ?
Cl2 C34 C35 Cl3 153.2(17) . . . . ?
Cl1 C34 C35 Cl3 -93.1(17) . . . . ?
Cl21 C44 C45 Cl23 14.6(16) . . . . ?
Cl22 C44 C45 Cl23 128.6(15) . . . . ?
Cl21 C44 C45 Cl24 -99.5(16) . . . . ?
Cl22 C44 C45 Cl24 14.6(15) . . . . ?
Cl2A C34A C35A Cl3A 71(3) . . . . ?
Cl1A C34A C35A Cl3A -172(3) . . . . ?
Cl2A C34A C35A Cl4A -172(3) . . . . ?
Cl1A C34A C35A Cl4A -55(3) . . . . ?
Cl18 C42 C43 Cl19 -35.8(13) . . . . ?
Cl17 C42 C43 Cl19 79.4(13) . . . . ?
Cl18 C42 C43 Cl20 77.3(13) . . . . ?
Cl17 C42 C43 Cl20 -167.5(14) . . . . ?
Cl6 C36 C37 Cl7 -33(2) . . . . ?
Cl5 C36 C37 Cl7 86(2) . . . . ?
Cl6 C36 C37 Cl8 85(2) . . . . ?
Cl5 C36 C37 Cl8 -156(2) . . . . ?
Cl14 C40 C41 Cl15 -56.3(17) . . . . ?
Cl13 C40 C41 Cl15 62.4(16) . . . . ?
Cl14 C40 C41 Cl16 -173.9(17) . . . . ?
Cl13 C40 C41 Cl16 -55.1(16) . . . . ?
Cl6A C36A C37A Cl7A 35.9(19) . . . . ?
Cl5A C36A C37A Cl7A 149.7(18) . . . . ?
Cl6A C36A C37A Cl8A 150.5(18) . . . . ?
Cl5A C36A C37A Cl8A -95.8(17) . . . . ?
Cl10 C38 C39 Cl12 54(3) . . . . ?
Cl9 C38 C39 Cl12 171(3) . . . . ?
Cl10 C38 C39 Cl11 171(3) . . . . ?
Cl9 C38 C39 Cl11 -72(3) . . . . ?
C6 C1 C2 C3 -1.6(10) . . . . ?
C7 C1 C2 C3 176.4(7) . . . . ?
C1 C2 C3 C4 2.2(10) . . . . ?
C1 C2 C3 C25 -177.9(6) . . . . ?
C2 C3 C4 C5 -1.5(9) . . . . ?
C25 C3 C4 C5 178.5(5) . . . . ?
C3 C4 C5 C6 0.4(9) . . . . ?
C3 C4 C5 C16 -179.6(6) . . . . ?
C2 C1 C6 C5 0.5(11) . . . . ?
C7 C1 C6 C5 -177.6(7) . . . . ?
C4 C5 C6 C1 0.2(10) . . . . ?
C16 C5 C6 C1 -179.8(6) . . . . ?
C6 C1 C7 C12 -97.4(10) . . . . ?
C2 C1 C7 C12 84.6(10) . . . . ?
C6 C1 C7 C8 80.0(10) . . . . ?
C2 C1 C7 C8 -98.0(9) . . . . ?
C12 C7 C8 C9 2.3(15) . . . . ?
C1 C7 C8 C9 -175.1(9) . . . . ?
C12 C7 C8 C14 -176.0(12) . . . . ?
C1 C7 C8 C14 6.5(16) . . . . ?
C7 C8 C9 C10 -3.3(17) . . . . ?
C14 C8 C9 C10 175.0(13) . . . . ?
C8 C9 C10 C11 2.2(19) . . . . ?
C8 C9 C10 C13 -179.6(11) . . . . ?
C9 C10 C11 C12 0(2) . . . . ?
C13 C10 C11 C12 -178.0(12) . . . . ?
C8 C7 C12 C11 -0.1(16) . . . . ?
C1 C7 C12 C11 177.2(10) . . . . ?
C8 C7 C12 C15 -179.9(12) . . . . ?
C1 C7 C12 C15 -2.5(17) . . . . ?
C10 C11 C12 C7 -1.1(19) . . . . ?
C10 C11 C12 C15 178.6(14) . . . . ?
C11 C10 C13 O1 3(2) . . . . ?
C9 C10 C13 O1 -174.7(12) . . . . ?
C11 C10 C13 O2 -178.0(13) . . . . ?
C9 C10 C13 O2 3.9(19) . . . . ?
C6 C5 C16 C17 -77.3(8) . . . . ?
C4 C5 C16 C17 102.7(7) . . . . ?
C6 C5 C16 C21 97.5(7) . . . . ?
C4 C5 C16 C21 -82.5(7) . . . . ?
C21 C16 C17 C18 0.2(9) . . . . ?
C5 C16 C17 C18 175.1(6) . . . . ?
C21 C16 C17 C23 177.2(6) . . . . ?
C5 C16 C17 C23 -7.9(9) . . . . ?
C16 C17 C18 C19 -3.0(9) . . . . ?
C23 C17 C18 C19 180.0(6) . . . . ?
C17 C18 C19 C20 4.8(9) . . . . ?
C17 C18 C19 C22 -176.1(6) . . . . ?
C18 C19 C20 C21 -3.8(9) . . . . ?
C22 C19 C20 C21 177.1(5) . . . . ?
C19 C20 C21 C16 1.0(8) . . . . ?
C19 C20 C21 C24 -177.5(6) . . . . ?
C17 C16 C21 C20 0.7(8) . . . . ?
C5 C16 C21 C20 -174.1(5) . . . . ?
C17 C16 C21 C24 179.3(6) . . . . ?
C5 C16 C21 C24 4.4(8) . . . . ?
C18 C19 C22 O4 173.5(6) . . . . ?
C20 C19 C22 O4 -7.4(8) . . . . ?
C18 C19 C22 O3 -2.5(8) . . . . ?
C20 C19 C22 O3 176.6(5) . . . . ?
C4 C3 C25 C26 -114.1(7) . . . . ?
C2 C3 C25 C26 66.0(8) . . . . ?
C4 C3 C25 C30 62.5(8) . . . . ?
C2 C3 C25 C30 -117.4(7) . . . . ?
C30 C25 C26 C27 0.2(9) . . . . ?
C3 C25 C26 C27 176.8(6) . . . . ?
C30 C25 C26 C32 -179.0(6) . . . . ?
C3 C25 C26 C32 -2.5(9) . . . . ?
C25 C26 C27 C28 -0.8(9) . . . . ?
C32 C26 C27 C28 178.5(6) . . . . ?
C26 C27 C28 C29 1.7(9) . . . . ?
C26 C27 C28 C31 -176.5(5) . . . . ?
C27 C28 C29 C30 -2.2(10) . . . . ?
C31 C28 C29 C30 175.9(6) . . . . ?
C28 C29 C30 C25 1.6(9) . . . . ?
C28 C29 C30 C33 -179.9(6) . . . . ?
C26 C25 C30 C29 -0.6(9) . . . . ?
C3 C25 C30 C29 -177.2(6) . . . . ?
C26 C25 C30 C33 -179.1(6) . . . . ?
C3 C25 C30 C33 4.3(9) . . . . ?
C29 C28 C31 O5 -170.0(6) . . . . ?
C27 C28 C31 O5 8.0(9) . . . . ?
C29 C28 C31 O6 9.7(9) . . . . ?
C27 C28 C31 O6 -172.3(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.109
_database_code_depnum_ccdc_archive 'CCDC 974555'
#END


data_Global3
_publ_contact_author_name        'Prof. J. N. Moorthy'
_publ_contact_author_address     
;Departmet of chemistry
Indian Institute of Technology - Kanpur
Kanpur - 208 016
INDIA
;
_publ_contact_author_email       moorthy@iitk.ac.in
_publ_contact_author_phone       +915122597438
_publ_contact_author_fax         +915122597436
loop_
_publ_author_name
_publ_author_address


'Prof. J. N. Moorthy, '
;Departmet of chemistry
Indian Institute of Technology - Kanpur
Kanpur - 208 016
INDIA
;
'Alankriti Bajpai'
;Department of Chemistry
Indian Institute of Technology
Kanpur 208 016
INDIA
;
'Prof. P. Venugopalan'
;Department of Chemistry
Panjab University
Chandigrah 560017
INDIA
;
data_MeBTB-TCE-After-Squeeze

_audit_creation_method           ' Manual edit of SHELXL-97 CIF'
_chemical_name_systematic        
;
1,3,5-Tris(2,6-dimethyl-4-carboxyphenyl)benzene + 2*1,1,2,2-tetrachloroethane
;
_chemical_name_common            MeBTB
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H34 Cl8 O6'
_chemical_formula_weight         858.28

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   50.850(16)
_cell_length_b                   15.260(5)
_cell_length_c                   14.006(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10868(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3520
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER AXS KAPPA APEX-II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            53394
_diffrn_reflns_av_R_equivalents  0.1341
_diffrn_reflns_av_sigmaI/netI    0.1170
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9426
_reflns_number_gt                4174
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97

_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)+(0.0639P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9426
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1634
_refine_ls_R_factor_gt           0.0817
_refine_ls_wR_factor_ref         0.1970
_refine_ls_wR_factor_gt          0.1768
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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
O1 O 0.47925(7) -0.0605(3) 0.5702(3) 0.1643(16) Uani 1 1 d . . .
H1A H 0.4944 -0.0521 0.5484 0.246 Uiso 1 1 calc R . .
O2 O 0.47248(6) 0.0640(3) 0.4905(3) 0.1715(17) Uani 1 1 d . . .
O3 O 0.24189(4) -0.14776(12) 0.25590(13) 0.0578(6) Uani 1 1 d . . .
H4A H 0.2333 -0.1762 0.2151 0.087 Uiso 1 1 calc R . .
O4 O 0.24347(4) -0.27847(13) 0.33007(12) 0.0519(5) Uani 1 1 d . . .
O5 O 0.28382(4) 0.26396(14) 1.12671(13) 0.0615(6) Uani 1 1 d . . .
O6 O 0.27540(4) 0.13050(12) 1.18609(13) 0.0615(6) Uani 1 1 d . . .
H6A H 0.2697 0.1598 1.2324 0.092 Uiso 1 1 calc R . .
C1 C 0.35675(6) -0.0054(2) 0.6586(2) 0.0611(9) Uani 1 1 d . . .
C2 C 0.34776(7) 0.0275(2) 0.7466(2) 0.0623(9) Uani 1 1 d . . .
H2A H 0.3601 0.0504 0.7911 0.075 Uiso 1 1 calc R . .
C3 C 0.32167(6) 0.02714(18) 0.7691(2) 0.0504(8) Uani 1 1 d . . .
C4 C 0.30375(6) -0.00656(17) 0.70556(19) 0.0490(8) Uani 1 1 d . . .
H4B H 0.2855 -0.0064 0.7208 0.059 Uiso 1 1 calc R . .
C5 C 0.31244(6) -0.04157(18) 0.61707(19) 0.0474(8) Uani 1 1 d . . .
C6 C 0.33874(6) -0.0399(2) 0.5959(2) 0.0614(9) Uani 1 1 d . . .
H6B H 0.3446 -0.0630 0.5367 0.074 Uiso 1 1 calc R . .
C7 C 0.38504(7) -0.0010(3) 0.6319(2) 0.0682(10) Uani 1 1 d . . .
C8 C 0.39419(8) 0.0657(3) 0.5750(4) 0.1059(14) Uani 1 1 d . . .
C9 C 0.42016(10) 0.0643(3) 0.5444(4) 0.1219(17) Uani 1 1 d . . .
H9A H 0.4263 0.1082 0.5017 0.146 Uiso 1 1 calc R . .
C10 C 0.43717(8) -0.0001(4) 0.5754(3) 0.1044(14) Uani 1 1 d . . .
C11 C 0.42832(9) -0.0646(4) 0.6314(4) 0.1324(19) Uani 1 1 d . . .
H11A H 0.4399 -0.1100 0.6507 0.159 Uiso 1 1 calc R . .
C12 C 0.40170(9) -0.0659(3) 0.6623(3) 0.1130(16) Uani 1 1 d . . .
C13 C 0.46454(10) 0.0005(5) 0.5444(4) 0.1294(19) Uani 1 1 d . . .
C14 C 0.37582(10) 0.1380(3) 0.5426(5) 0.186(3) Uani 1 1 d . . .
H14A H 0.3777 0.1466 0.4736 0.279 Uiso 1 1 calc R . .
H14B H 0.3803 0.1925 0.5759 0.279 Uiso 1 1 calc R . .
H14C H 0.3576 0.1216 0.5573 0.279 Uiso 1 1 calc R . .
C15 C 0.39217(11) -0.1389(4) 0.7230(5) 0.227(4) Uani 1 1 d . . .
H15A H 0.3825 -0.1150 0.7777 0.340 Uiso 1 1 calc R . .
H15B H 0.4072 -0.1732 0.7459 0.340 Uiso 1 1 calc R . .
H15C H 0.3805 -0.1767 0.6856 0.340 Uiso 1 1 calc R . .
C16 C 0.29371(6) -0.0787(2) 0.54649(19) 0.0490(8) Uani 1 1 d . . .
C17 C 0.28662(6) -0.02909(19) 0.4656(2) 0.0544(8) Uani 1 1 d . . .
C18 C 0.27108(6) -0.0696(2) 0.39599(19) 0.0515(8) Uani 1 1 d . . .
H18A H 0.2656 -0.0366 0.3420 0.062 Uiso 1 1 calc R . .
C19 C 0.26354(6) -0.1557(2) 0.40348(19) 0.0475(7) Uani 1 1 d . . .
C20 C 0.26971(6) -0.20361(19) 0.4833(2) 0.0519(8) Uani 1 1 d . . .
H20A H 0.2635 -0.2620 0.4893 0.062 Uiso 1 1 calc R . .
C21 C 0.28521(5) -0.16691(19) 0.55622(18) 0.0448(7) Uani 1 1 d . . .
C22 C 0.24828(6) -0.2000(2) 0.3277(2) 0.0485(8) Uani 1 1 d . . .
C23 C 0.29465(7) 0.06454(19) 0.4559(2) 0.0701(10) Uani 1 1 d . . .
H23A H 0.3123 0.0677 0.4278 0.105 Uiso 1 1 calc R . .
H23B H 0.2948 0.0923 0.5190 0.105 Uiso 1 1 calc R . .
H23C H 0.2821 0.0952 0.4144 0.105 Uiso 1 1 calc R . .
C24 C 0.29323(6) -0.22059(19) 0.64287(18) 0.0585(9) Uani 1 1 d . . .
H24A H 0.2906 -0.1858 0.7009 0.088 Uiso 1 1 calc R . .
H24B H 0.3118 -0.2369 0.6374 0.088 Uiso 1 1 calc R . .
H24C H 0.2825 -0.2737 0.6462 0.088 Uiso 1 1 calc R . .
C25 C 0.31295(6) 0.0668(2) 0.86316(19) 0.0498(8) Uani 1 1 d . . .
C26 C 0.31648(6) 0.15644(19) 0.87879(19) 0.0477(7) Uani 1 1 d . . .
C27 C 0.30738(6) 0.19177(19) 0.96440(19) 0.0497(8) Uani 1 1 d . . .
H27A H 0.3098 0.2524 0.9771 0.060 Uiso 1 1 calc R . .
C28 C 0.29477(6) 0.1393(2) 1.03132(19) 0.0487(8) Uani 1 1 d . . .
C29 C 0.29206(6) 0.0517(2) 1.0151(2) 0.0527(8) Uani 1 1 d . . .
H29A H 0.2841 0.0162 1.0627 0.063 Uiso 1 1 calc R . .
C30 C 0.30063(6) 0.01254(19) 0.93117(19) 0.0475(8) Uani 1 1 d . . .
C31 C 0.28436(6) 0.1847(2) 1.11895(19) 0.0491(8) Uani 1 1 d . . .
C32 C 0.32916(6) 0.21676(19) 0.8089(2) 0.0627(9) Uani 1 1 d . . .
H32A H 0.3240 0.2773 0.8230 0.094 Uiso 1 1 calc R . .
H32B H 0.3235 0.2014 0.7441 0.094 Uiso 1 1 calc R . .
H32C H 0.3483 0.2112 0.8135 0.094 Uiso 1 1 calc R . .
C33 C 0.29682(7) -0.0850(2) 0.9172(2) 0.0702(10) Uani 1 1 d . . .
H33A H 0.2975 -0.1145 0.9793 0.105 Uiso 1 1 calc R . .
H33B H 0.3108 -0.1078 0.8759 0.105 Uiso 1 1 calc R . .
H33C H 0.2797 -0.0957 0.8874 0.105 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
O1 C13 1.247(6) . ?
O1 H1A 0.8400 . ?
O2 C13 1.293(6) . ?
O3 C22 1.323(3) . ?
O3 H4A 0.8400 . ?
O4 C22 1.223(3) . ?
O5 C31 1.215(3) . ?
O6 C31 1.333(3) . ?
O6 H6A 0.8400 . ?
C1 C6 1.373(4) . ?
C1 C2 1.408(4) . ?
C1 C7 1.488(5) . ?
C2 C3 1.364(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.374(4) . ?
C3 C25 1.516(4) . ?
C4 C5 1.420(4) . ?
C4 H4B 0.9500 . ?
C5 C6 1.370(4) . ?
C5 C16 1.485(4) . ?
C6 H6B 0.9500 . ?
C7 C12 1.372(5) . ?
C7 C8 1.374(5) . ?
C8 C9 1.388(5) . ?
C8 C14 1.515(6) . ?
C9 C10 1.380(6) . ?
C9 H9A 0.9500 . ?
C10 C11 1.336(6) . ?
C10 C13 1.458(6) . ?
C11 C12 1.422(6) . ?
C11 H11A 0.9500 . ?
C12 C15 1.482(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.410(4) . ?
C16 C21 1.420(4) . ?
C17 C18 1.399(4) . ?
C17 C23 1.492(4) . ?
C18 C19 1.373(4) . ?
C18 H18A 0.9500 . ?
C19 C20 1.372(4) . ?
C19 C22 1.479(4) . ?
C20 C21 1.407(4) . ?
C20 H20A 0.9500 . ?
C21 C24 1.520(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.397(4) . ?
C25 C30 1.409(4) . ?
C26 C27 1.394(4) . ?
C26 C32 1.491(4) . ?
C27 C28 1.389(4) . ?
C27 H27A 0.9500 . ?
C28 C29 1.364(4) . ?
C28 C31 1.505(4) . ?
C29 C30 1.388(4) . ?
C29 H29A 0.9500 . ?
C30 C33 1.513(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 O1 H1A 109.5 . . ?
C22 O3 H4A 109.5 . . ?
C31 O6 H6A 109.5 . . ?
C6 C1 C2 118.7(3) . . ?
C6 C1 C7 120.1(3) . . ?
C2 C1 C7 121.1(3) . . ?
C3 C2 C1 121.1(3) . . ?
C3 C2 H2A 119.5 . . ?
C1 C2 H2A 119.5 . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 C25 118.9(3) . . ?
C4 C3 C25 121.2(3) . . ?
C3 C4 C5 120.0(3) . . ?
C3 C4 H4B 120.0 . . ?
C5 C4 H4B 120.0 . . ?
C6 C5 C4 119.0(3) . . ?
C6 C5 C16 119.3(2) . . ?
C4 C5 C16 121.7(3) . . ?
C5 C6 C1 121.3(3) . . ?
C5 C6 H6B 119.3 . . ?
C1 C6 H6B 119.3 . . ?
C12 C7 C8 120.4(3) . . ?
C12 C7 C1 119.1(3) . . ?
C8 C7 C1 120.5(3) . . ?
C7 C8 C9 119.4(4) . . ?
C7 C8 C14 120.3(4) . . ?
C9 C8 C14 120.3(4) . . ?
C10 C9 C8 120.7(4) . . ?
C10 C9 H9A 119.7 . . ?
C8 C9 H9A 119.7 . . ?
C11 C10 C9 119.9(4) . . ?
C11 C10 C13 120.1(5) . . ?
C9 C10 C13 120.0(5) . . ?
C10 C11 C12 120.7(5) . . ?
C10 C11 H11A 119.7 . . ?
C12 C11 H11A 119.7 . . ?
C7 C12 C11 118.9(4) . . ?
C7 C12 C15 121.2(4) . . ?
C11 C12 C15 119.8(5) . . ?
O1 C13 O2 122.7(5) . . ?
O1 C13 C10 118.8(6) . . ?
O2 C13 C10 118.5(5) . . ?
C8 C14 H14A 109.5 . . ?
C8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C21 120.6(3) . . ?
C17 C16 C5 119.6(3) . . ?
C21 C16 C5 119.5(3) . . ?
C18 C17 C16 117.9(3) . . ?
C18 C17 C23 120.9(3) . . ?
C16 C17 C23 121.2(3) . . ?
C19 C18 C17 121.8(3) . . ?
C19 C18 H18A 119.1 . . ?
C17 C18 H18A 119.1 . . ?
C20 C19 C18 120.5(3) . . ?
C20 C19 C22 117.5(3) . . ?
C18 C19 C22 121.9(3) . . ?
C19 C20 C21 120.5(3) . . ?
C19 C20 H20A 119.7 . . ?
C21 C20 H20A 119.7 . . ?
C20 C21 C16 118.6(3) . . ?
C20 C21 C24 121.1(3) . . ?
C16 C21 C24 120.4(2) . . ?
O4 C22 O3 124.2(3) . . ?
O4 C22 C19 122.2(3) . . ?
O3 C22 C19 113.5(3) . . ?
C17 C23 H23A 109.5 . . ?
C17 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C17 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C30 121.8(3) . . ?
C26 C25 C3 119.3(2) . . ?
C30 C25 C3 118.9(3) . . ?
C27 C26 C25 118.1(3) . . ?
C27 C26 C32 118.0(3) . . ?
C25 C26 C32 123.9(2) . . ?
C28 C27 C26 120.7(3) . . ?
C28 C27 H27A 119.6 . . ?
C26 C27 H27A 119.6 . . ?
C29 C28 C27 119.9(3) . . ?
C29 C28 C31 123.5(3) . . ?
C27 C28 C31 116.6(3) . . ?
C28 C29 C30 122.1(3) . . ?
C28 C29 H29A 119.0 . . ?
C30 C29 H29A 119.0 . . ?
C29 C30 C25 117.3(3) . . ?
C29 C30 C33 119.5(3) . . ?
C25 C30 C33 123.2(3) . . ?
O5 C31 O6 123.2(3) . . ?
O5 C31 C28 122.6(3) . . ?
O6 C31 C28 114.2(3) . . ?
C26 C32 H32A 109.5 . . ?
C26 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C26 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -1.3(5) . . . . ?
C7 C1 C2 C3 176.9(3) . . . . ?
C1 C2 C3 C4 0.6(5) . . . . ?
C1 C2 C3 C25 -177.6(3) . . . . ?
C2 C3 C4 C5 0.6(4) . . . . ?
C25 C3 C4 C5 178.6(3) . . . . ?
C3 C4 C5 C6 -1.0(4) . . . . ?
C3 C4 C5 C16 179.9(3) . . . . ?
C4 C5 C6 C1 0.2(5) . . . . ?
C16 C5 C6 C1 179.4(3) . . . . ?
C2 C1 C6 C5 0.9(5) . . . . ?
C7 C1 C6 C5 -177.3(3) . . . . ?
C6 C1 C7 C12 -96.8(4) . . . . ?
C2 C1 C7 C12 85.0(5) . . . . ?
C6 C1 C7 C8 81.0(5) . . . . ?
C2 C1 C7 C8 -97.1(4) . . . . ?
C12 C7 C8 C9 3.3(7) . . . . ?
C1 C7 C8 C9 -174.5(4) . . . . ?
C12 C7 C8 C14 -179.2(5) . . . . ?
C1 C7 C8 C14 3.0(7) . . . . ?
C7 C8 C9 C10 -4.1(8) . . . . ?
C14 C8 C9 C10 178.4(5) . . . . ?
C8 C9 C10 C11 3.6(8) . . . . ?
C8 C9 C10 C13 -178.6(5) . . . . ?
C9 C10 C11 C12 -2.3(8) . . . . ?
C13 C10 C11 C12 179.9(5) . . . . ?
C8 C7 C12 C11 -2.0(7) . . . . ?
C1 C7 C12 C11 175.8(4) . . . . ?
C8 C7 C12 C15 -179.4(5) . . . . ?
C1 C7 C12 C15 -1.6(7) . . . . ?
C10 C11 C12 C7 1.5(8) . . . . ?
C10 C11 C12 C15 179.0(6) . . . . ?
C11 C10 C13 O1 0.8(9) . . . . ?
C9 C10 C13 O1 -177.0(5) . . . . ?
C11 C10 C13 O2 -179.8(5) . . . . ?
C9 C10 C13 O2 2.4(8) . . . . ?
C6 C5 C16 C17 -76.6(4) . . . . ?
C4 C5 C16 C17 102.5(3) . . . . ?
C6 C5 C16 C21 97.1(3) . . . . ?
C4 C5 C16 C21 -83.8(3) . . . . ?
C21 C16 C17 C18 0.0(4) . . . . ?
C5 C16 C17 C18 173.6(3) . . . . ?
C21 C16 C17 C23 178.0(3) . . . . ?
C5 C16 C17 C23 -8.4(4) . . . . ?
C16 C17 C18 C19 -2.2(4) . . . . ?
C23 C17 C18 C19 179.8(3) . . . . ?
C17 C18 C19 C20 4.1(4) . . . . ?
C17 C18 C19 C22 -176.8(3) . . . . ?
C18 C19 C20 C21 -3.8(4) . . . . ?
C22 C19 C20 C21 177.1(2) . . . . ?
C19 C20 C21 C16 1.6(4) . . . . ?
C19 C20 C21 C24 -177.2(3) . . . . ?
C17 C16 C21 C20 0.3(4) . . . . ?
C5 C16 C21 C20 -173.4(2) . . . . ?
C17 C16 C21 C24 179.1(3) . . . . ?
C5 C16 C21 C24 5.4(4) . . . . ?
C20 C19 C22 O4 -7.4(4) . . . . ?
C18 C19 C22 O4 173.5(3) . . . . ?
C20 C19 C22 O3 176.3(3) . . . . ?
C18 C19 C22 O3 -2.8(4) . . . . ?
C2 C3 C25 C26 64.4(4) . . . . ?
C4 C3 C25 C26 -113.7(3) . . . . ?
C2 C3 C25 C30 -117.8(3) . . . . ?
C4 C3 C25 C30 64.1(4) . . . . ?
C30 C25 C26 C27 -0.1(4) . . . . ?
C3 C25 C26 C27 177.6(3) . . . . ?
C30 C25 C26 C32 -179.5(3) . . . . ?
C3 C25 C26 C32 -1.7(4) . . . . ?
C25 C26 C27 C28 -1.1(4) . . . . ?
C32 C26 C27 C28 178.3(3) . . . . ?
C26 C27 C28 C29 2.4(4) . . . . ?
C26 C27 C28 C31 -176.7(3) . . . . ?
C27 C28 C29 C30 -2.6(4) . . . . ?
C31 C28 C29 C30 176.5(3) . . . . ?
C28 C29 C30 C25 1.4(4) . . . . ?
C28 C29 C30 C33 -179.5(3) . . . . ?
C26 C25 C30 C29 0.0(4) . . . . ?
C3 C25 C30 C29 -177.8(3) . . . . ?
C26 C25 C30 C33 -179.1(3) . . . . ?
C3 C25 C30 C33 3.2(4) . . . . ?
C29 C28 C31 O5 -170.0(3) . . . . ?
C27 C28 C31 O5 9.1(4) . . . . ?
C29 C28 C31 O6 8.8(4) . . . . ?
C27 C28 C31 O6 -172.1(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.041
#END
_database_code_depnum_ccdc_archive 'CCDC 974555'

Data_Global
_publ_contact_author_name        'Prof. J. N. Moorthy'
_publ_contact_author_address     
;Departmet of chemistry
Indian Institute of Technology - Kanpur
Kanpur - 208 016
INDIA
;
_publ_contact_author_email       moorthy@iitk.ac.in
_publ_contact_author_phone       +915122597438
_publ_contact_author_fax         +915122597436
loop_
_publ_author_name
_publ_author_address


'Prof. J. N. Moorthy, '
;Departmet of chemistry
Indian Institute of Technology - Kanpur
Kanpur - 208 016
INDIA
;
'Alankriti Bajpai'
;Department of Chemistry
Indian Institute of Technology
Kanpur 208 016
INDIA
;
'Prof. P. Venugopalan'
;Department of Chemistry
Panjab University
Chandigrah 560017
INDIA
;
data_MeBTB-DME

_audit_creation_method           'Manual edit of SHELXL-97 CIF'
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            
;
2*1,3,5-Tris(2,6-dimethyl-4-carboxyphenyl)benzene+2*Dimethoxyethane+2*H2O
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C74 H84 O18'
_chemical_formula_weight         1261.44

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           Hexagonal
_symmetry_space_group_name_H-M   P6(1)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'

_cell_length_a                   25.350(4)
_cell_length_b                   25.350(4)
_cell_length_c                   18.979(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     10562(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4032
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER AXS KAPPA APEX-II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            55064
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         24.99
_reflns_number_total             12237
_reflns_number_gt                8585
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97

_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. 
 The finally refined structure still has a void volume of 344Ang^3, probably 
 indicating that there may be very disordered water molecule present or the 
 thermal motions of the disordered atoms are very high. However, we could not 
 model any more   water molecules satisfactory due to very diffused electron 
 density observed.
;

_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)+(0.1159P)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    constr
_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   -0.4(12)
_refine_ls_number_reflns         12237
_refine_ls_number_parameters     817
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0728
_refine_ls_wR_factor_ref         0.1948
_refine_ls_wR_factor_gt          0.1768
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.075
_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
O1 O 0.2093(3) 0.1649(2) -0.4969(4) 0.144(2) Uani 1 1 d . . .
H1B H 0.1784 0.1643 -0.5111 0.216 Uiso 0.50 1 calc PR . .
O2 O 0.1564(3) 0.1375(3) -0.3959(4) 0.153(2) Uani 1 1 d . . .
H2B H 0.1319 0.1430 -0.4184 0.229 Uiso 0.50 1 calc PR . .
O3 O 0.42396(14) -0.16677(11) -0.17611(16) 0.0654(8) Uani 1 1 d . . .
O4 O 0.52044(15) -0.11692(12) -0.21332(17) 0.0673(8) Uani 1 1 d . . .
H4B H 0.5178 -0.1499 -0.2053 0.101 Uiso 1 1 calc R . .
O5 O 0.74962(16) 0.46886(14) -0.24444(19) 0.0788(9) Uani 1 1 d . . .
O6 O 0.71939(13) 0.46793(13) -0.13368(17) 0.0696(8) Uani 1 1 d . . .
H6B H 0.7543 0.4964 -0.1292 0.104 Uiso 1 1 calc R . .
C1 C 0.40322(17) 0.14795(16) -0.2927(2) 0.0477(9) Uani 1 1 d . . .
C2 C 0.40510(17) 0.09514(15) -0.27839(19) 0.0443(8) Uani 1 1 d . . .
H2A H 0.3722 0.0577 -0.2914 0.053 Uiso 1 1 calc R . .
C3 C 0.45490(16) 0.09680(15) -0.24515(18) 0.0424(8) Uani 1 1 d . . .
C4 C 0.50348(17) 0.15354(16) -0.22603(18) 0.0454(8) Uani 1 1 d . . .
H4A H 0.5368 0.1556 -0.2028 0.055 Uiso 1 1 calc R . .
C5 C 0.50319(16) 0.20665(15) -0.24077(19) 0.0439(8) Uani 1 1 d . . .
C6 C 0.45283(18) 0.20346(16) -0.2733(2) 0.0509(9) Uani 1 1 d . . .
H6A H 0.4522 0.2392 -0.2824 0.061 Uiso 1 1 calc R . .
C7 C 0.35010(19) 0.14651(16) -0.3290(2) 0.0542(10) Uani 1 1 d . . .
C8 C 0.3561(2) 0.16235(17) -0.4006(3) 0.0639(12) Uani 1 1 d . . .
C9 C 0.3071(2) 0.16332(19) -0.4338(3) 0.0768(15) Uani 1 1 d . . .
H9A H 0.3097 0.1739 -0.4811 0.092 Uiso 1 1 calc R . .
C10 C 0.2536(2) 0.1481(2) -0.3952(4) 0.0808(15) Uani 1 1 d . . .
C11 C 0.2500(2) 0.1332(2) -0.3268(4) 0.0769(14) Uani 1 1 d . . .
H11A H 0.2144 0.1235 -0.3025 0.092 Uiso 1 1 calc R . .
C12 C 0.2970(2) 0.13141(19) -0.2905(3) 0.0679(12) Uani 1 1 d . . .
C13 C 0.4113(2) 0.1752(2) -0.4418(3) 0.0732(13) Uani 1 1 d . . .
H13A H 0.4438 0.2155 -0.4312 0.110 Uiso 1 1 calc R . .
H13B H 0.4022 0.1722 -0.4913 0.110 Uiso 1 1 calc R . .
H13C H 0.4235 0.1461 -0.4296 0.110 Uiso 1 1 calc R . .
C14 C 0.2031(4) 0.1504(3) -0.4348(6) 0.115(3) Uani 1 1 d . . .
C15 C 0.2912(3) 0.1134(3) -0.2153(3) 0.0826(14) Uani 1 1 d . . .
H15A H 0.2518 0.1041 -0.1981 0.124 Uiso 1 1 calc R . .
H15B H 0.3222 0.1464 -0.1883 0.124 Uiso 1 1 calc R . .
H15C H 0.2957 0.0782 -0.2107 0.124 Uiso 1 1 calc R . .
C16 C 0.45850(16) 0.04067(15) -0.23246(18) 0.0420(8) Uani 1 1 d . . .
C17 C 0.41597(18) -0.00552(17) -0.1877(2) 0.0497(9) Uani 1 1 d . . .
C18 C 0.41999(18) -0.05781(16) -0.17838(19) 0.0497(9) Uani 1 1 d . . .
H18A H 0.3920 -0.0888 -0.1495 0.060 Uiso 1 1 calc R . .
C19 C 0.46523(17) -0.06434(15) -0.2117(2) 0.0481(9) Uani 1 1 d . . .
C20 C 0.50750(17) -0.01819(15) -0.25504(19) 0.0441(8) Uani 1 1 d . . .
H20A H 0.5381 -0.0225 -0.2767 0.053 Uiso 1 1 calc R . .
C21 C 0.50409(16) 0.03405(14) -0.26598(18) 0.0412(8) Uani 1 1 d . . .
C22 C 0.3680(2) 0.00101(19) -0.1482(2) 0.0592(10) Uani 1 1 d . . .
H22A H 0.3360 -0.0051 -0.1800 0.089 Uiso 1 1 calc R . .
H22B H 0.3859 0.0411 -0.1281 0.089 Uiso 1 1 calc R . .
H22C H 0.3516 -0.0288 -0.1112 0.089 Uiso 1 1 calc R . .
C23 C 0.4696(2) -0.12018(16) -0.1998(2) 0.0498(9) Uani 1 1 d . . .
C24 C 0.55041(17) 0.08281(16) -0.31405(19) 0.0466(8) Uani 1 1 d . . .
H24A H 0.5802 0.1160 -0.2862 0.070 Uiso 1 1 calc R . .
H24B H 0.5302 0.0973 -0.3446 0.070 Uiso 1 1 calc R . .
H24C H 0.5702 0.0661 -0.3418 0.070 Uiso 1 1 calc R . .
C25 C 0.55906(17) 0.26807(16) -0.2270(2) 0.0465(9) Uani 1 1 d . . .
C26 C 0.56590(17) 0.29711(16) -0.1616(2) 0.0468(8) Uani 1 1 d . . .
C28 C 0.65896(17) 0.38247(16) -0.2051(2) 0.0479(9) Uani 1 1 d . . .
C27 C 0.61666(19) 0.35443(18) -0.1522(2) 0.0536(10) Uani 1 1 d . . .
H27A H 0.6222 0.3743 -0.1094 0.064 Uiso 1 1 calc R . .
C29 C 0.65100(18) 0.35198(16) -0.2687(2) 0.0483(9) Uani 1 1 d . . .
H29A H 0.6795 0.3708 -0.3044 0.058 Uiso 1 1 calc R . .
C30 C 0.60211(17) 0.29478(16) -0.28011(19) 0.0452(8) Uani 1 1 d . . .
C32 C 0.7128(2) 0.44356(19) -0.1976(2) 0.0566(10) Uani 1 1 d . . .
C31 C 0.5207(2) 0.26655(18) -0.1027(2) 0.0548(10) Uani 1 1 d . . .
H31A H 0.5258 0.2345 -0.0830 0.082 Uiso 1 1 calc R . .
H31B H 0.4801 0.2498 -0.1209 0.082 Uiso 1 1 calc R . .
H31C H 0.5274 0.2959 -0.0668 0.082 Uiso 1 1 calc R . .
C33 C 0.59674(19) 0.26195(17) -0.3483(2) 0.0538(9) Uani 1 1 d . . .
H33A H 0.6302 0.2877 -0.3786 0.081 Uiso 1 1 calc R . .
H33B H 0.5591 0.2521 -0.3711 0.081 Uiso 1 1 calc R . .
H33C H 0.5975 0.2252 -0.3387 0.081 Uiso 1 1 calc R . .
O1A O 0.73807(12) 0.53316(13) 0.01047(15) 0.0609(7) Uani 1 1 d . . .
O2A O 0.69189(13) 0.43664(13) 0.04166(16) 0.0613(7) Uani 1 1 d . . .
H2AA H 0.6662 0.4354 0.0144 0.092 Uiso 1 1 calc R . .
O3A O 0.9824(3) 0.8261(4) 0.5399(5) 0.180(4) Uani 1 1 d . . .
H3AA H 0.9800 0.8463 0.5722 0.270 Uiso 0.50 1 calc PR . .
O4A O 0.9412(3) 0.7513(4) 0.6229(5) 0.205(4) Uani 1 1 d . . .
H4AA H 0.9426 0.7785 0.6476 0.307 Uiso 0.50 1 calc PR . .
O5A O 1.08825(17) 0.34826(15) 0.4151(2) 0.0979(12) Uani 1 1 d . . .
H5AA H 1.1095 0.3332 0.4245 0.147 Uiso 1 1 calc R . .
O6A O 1.17682(16) 0.42584(15) 0.3831(2) 0.0779(9) Uani 1 1 d . . .
C1A C 0.92111(15) 0.54367(17) 0.25254(19) 0.0450(8) Uani 1 1 d . . .
C2A C 0.92461(15) 0.58657(17) 0.3011(2) 0.0456(8) Uani 1 1 d . . .
H2AB H 0.9025 0.6062 0.2931 0.055 Uiso 1 1 calc R . .
C3A C 0.96023(15) 0.60051(17) 0.3607(2) 0.0468(8) Uani 1 1 d . . .
C4A C 0.99274(16) 0.57018(17) 0.3719(2) 0.0484(9) Uani 1 1 d . . .
H4AB H 1.0168 0.5790 0.4120 0.058 Uiso 1 1 calc R . .
C5A C 0.98994(16) 0.52735(18) 0.3248(2) 0.0504(9) Uani 1 1 d . . .
C6A C 0.95402(15) 0.51440(18) 0.2649(2) 0.0477(9) Uani 1 1 d . . .
H6AA H 0.9521 0.4858 0.2327 0.057 Uiso 1 1 calc R . .
C7A C 0.87673(15) 0.52708(17) 0.19208(19) 0.0440(8) Uani 1 1 d . . .
C8A C 0.82193(15) 0.47143(17) 0.19496(19) 0.0440(8) Uani 1 1 d . . .
C9A C 0.77822(16) 0.45877(17) 0.14303(19) 0.0449(8) Uani 1 1 d . . .
H9AA H 0.7420 0.4216 0.1436 0.054 Uiso 1 1 calc R . .
C10A C 0.78791(17) 0.50073(18) 0.0907(2) 0.0485(9) Uani 1 1 d . . .
C11A C 0.84337(16) 0.55471(18) 0.0874(2) 0.0461(8) Uani 1 1 d . . .
H11B H 0.8502 0.5823 0.0513 0.055 Uiso 1 1 calc R . .
C12A C 0.88846(16) 0.56821(17) 0.1366(2) 0.0471(8) Uani 1 1 d . . .
C13A C 0.80848(16) 0.42759(17) 0.2537(2) 0.0492(9) Uani 1 1 d . . .
H13D H 0.7668 0.3955 0.2509 0.074 Uiso 1 1 calc R . .
H13E H 0.8152 0.4484 0.2980 0.074 Uiso 1 1 calc R . .
H13F H 0.8348 0.4106 0.2503 0.074 Uiso 1 1 calc R . .
C14A C 0.73706(19) 0.4902(2) 0.0435(2) 0.0551(10) Uani 1 1 d . . .
C15A C 0.94895(18) 0.62727(19) 0.1315(2) 0.0582(10) Uani 1 1 d . . .
H15D H 0.9543 0.6431 0.0845 0.087 Uiso 1 1 calc R . .
H15E H 0.9815 0.6197 0.1427 0.087 Uiso 1 1 calc R . .
H15F H 0.9493 0.6564 0.1641 0.087 Uiso 1 1 calc R . .
C16A C 0.96220(17) 0.6453(2) 0.4127(2) 0.0569(10) Uani 1 1 d . . .
C17A C 0.99257(19) 0.7072(2) 0.3960(3) 0.0654(12) Uani 1 1 d . . .
C18A C 0.9917(2) 0.7472(3) 0.4480(4) 0.094(2) Uani 1 1 d . . .
H18B H 1.0120 0.7888 0.4390 0.112 Uiso 1 1 calc R . .
C19A C 0.9622(3) 0.7262(4) 0.5105(4) 0.097(2) Uani 1 1 d . . .
C20A C 0.9324(2) 0.6650(4) 0.5264(3) 0.0910(19) Uani 1 1 d . . .
H20B H 0.9127 0.6514 0.5695 0.109 Uiso 1 1 calc R . .
C21A C 0.93187(19) 0.6235(3) 0.4776(3) 0.0738(14) Uani 1 1 d . . .
C22A C 1.0242(2) 0.7303(2) 0.3267(3) 0.0763(14) Uani 1 1 d . . .
H22D H 1.0526 0.7162 0.3196 0.114 Uiso 1 1 calc R . .
H22E H 1.0455 0.7740 0.3268 0.114 Uiso 1 1 calc R . .
H22F H 0.9946 0.7154 0.2895 0.114 Uiso 1 1 calc R . .
C23A C 0.9629(4) 0.7730(7) 0.5602(8) 0.168(5) Uani 1 1 d . . .
C24A C 0.8974(2) 0.5560(3) 0.4953(3) 0.0807(15) Uani 1 1 d . . .
H24D H 0.8767 0.5500 0.5395 0.121 Uiso 1 1 calc R . .
H24E H 0.9255 0.5412 0.4986 0.121 Uiso 1 1 calc R . .
H24F H 0.8681 0.5342 0.4589 0.121 Uiso 1 1 calc R . .
C25A C 1.02342(18) 0.49387(18) 0.34045(19) 0.0506(9) Uani 1 1 d . . .
C26A C 1.08811(17) 0.52608(19) 0.33626(19) 0.0517(9) Uani 1 1 d . . .
C27A C 1.11855(18) 0.49484(19) 0.3513(2) 0.0536(9) Uani 1 1 d . . .
H27B H 1.1608 0.5149 0.3481 0.064 Uiso 1 1 calc R . .
C28A C 1.08769(19) 0.43526(19) 0.3708(2) 0.0563(10) Uani 1 1 d . . .
C29A C 1.0244(2) 0.4038(2) 0.3772(2) 0.0689(12) Uani 1 1 d . . .
H29B H 1.0040 0.3634 0.3920 0.083 Uiso 1 1 calc R . .
C30A C 0.99122(19) 0.43376(19) 0.3611(3) 0.0639(11) Uani 1 1 d . . .
C31A C 1.12375(19) 0.5923(2) 0.3203(2) 0.0635(11) Uani 1 1 d . . .
H31D H 1.1242 0.6151 0.3609 0.095 Uiso 1 1 calc R . .
H31E H 1.1053 0.6014 0.2815 0.095 Uiso 1 1 calc R . .
H31F H 1.1647 0.6032 0.3081 0.095 Uiso 1 1 calc R . .
C32A C 1.1227(2) 0.4036(2) 0.3899(3) 0.0660(11) Uani 1 1 d . . .
C33A C 0.9230(2) 0.3998(2) 0.3678(4) 0.102(2) Uani 1 1 d . . .
H33D H 0.9094 0.4278 0.3806 0.153 Uiso 1 1 calc R . .
H33E H 0.9109 0.3692 0.4036 0.153 Uiso 1 1 calc R . .
H33F H 0.9051 0.3809 0.3237 0.153 Uiso 1 1 calc R . .
O9 O 0.7778(7) 0.6026(7) -0.2988(10) 0.225(7) Uiso 0.606(15) 1 d PDU A 1
O10 O 0.7782(12) 0.7359(9) -0.3574(13) 0.318(10) Uiso 0.606(15) 1 d PDU A 1
C38 C 0.8251(6) 0.5872(7) -0.2964(8) 0.120(4) Uiso 0.606(15) 1 d PDU A 1
H38A H 0.8318 0.5769 -0.3429 0.180 Uiso 0.606(15) 1 calc PR A 1
H38B H 0.8130 0.5531 -0.2655 0.180 Uiso 0.606(15) 1 calc PR A 1
H38C H 0.8619 0.6214 -0.2791 0.180 Uiso 0.606(15) 1 calc PR A 1
C39 C 0.7912(12) 0.6483(11) -0.3505(12) 0.286(9) Uiso 0.606(15) 1 d PDU A 1
H39A H 0.7874 0.6313 -0.3972 0.343 Uiso 0.606(15) 1 calc PR A 1
H39B H 0.8327 0.6813 -0.3446 0.343 Uiso 0.606(15) 1 calc PR A 1
C40 C 0.7479(8) 0.6726(9) -0.3432(18) 0.311(10) Uiso 0.606(15) 1 d PDU A 1
H40A H 0.7142 0.6514 -0.3757 0.374 Uiso 0.606(15) 1 calc PR A 1
H40B H 0.7315 0.6651 -0.2957 0.374 Uiso 0.606(15) 1 calc PR A 1
C41 C 0.7999(19) 0.7707(14) -0.2944(18) 0.345(16) Uiso 0.606(15) 1 d PDU A 1
H41A H 0.7713 0.7504 -0.2570 0.517 Uiso 0.606(15) 1 calc PR A 1
H41B H 0.8045 0.8103 -0.3017 0.517 Uiso 0.606(15) 1 calc PR A 1
H41C H 0.8386 0.7750 -0.2820 0.517 Uiso 0.606(15) 1 calc PR A 1
O9A O 0.8224(8) 0.6209(7) -0.2956(12) 0.194(8) Uiso 0.394(15) 1 d PDU A 2
O10A O 0.7748(14) 0.6825(12) -0.3472(14) 0.255(11) Uiso 0.394(15) 1 d PDU A 2
C38A C 0.8385(5) 0.5761(5) -0.2833(7) 0.053(3) Uiso 0.394(15) 1 d PDU A 2
H38D H 0.8430 0.5726 -0.2336 0.080 Uiso 0.394(15) 1 calc PR A 2
H38E H 0.8763 0.5874 -0.3066 0.080 Uiso 0.394(15) 1 calc PR A 2
H38F H 0.8072 0.5377 -0.3014 0.080 Uiso 0.394(15) 1 calc PR A 2
C39A C 0.7646(10) 0.6052(12) -0.2663(19) 0.210(10) Uiso 0.394(15) 1 d PDU A 2
H39C H 0.7646 0.5982 -0.2160 0.252 Uiso 0.394(15) 1 calc PR A 2
H39D H 0.7330 0.5681 -0.2879 0.252 Uiso 0.394(15) 1 calc PR A 2
C40A C 0.7523(13) 0.6571(13) -0.2796(17) 0.246(11) Uiso 0.394(15) 1 d PDU A 2
H40C H 0.7089 0.6422 -0.2773 0.296 Uiso 0.394(15) 1 calc PR A 2
H40D H 0.7722 0.6882 -0.2438 0.296 Uiso 0.394(15) 1 calc PR A 2
C41A C 0.8336(16) 0.7349(17) -0.343(2) 0.274(17) Uiso 0.394(15) 1 d PDU A 2
H41D H 0.8297 0.7704 -0.3375 0.411 Uiso 0.394(15) 1 calc PR A 2
H41E H 0.8555 0.7385 -0.3861 0.411 Uiso 0.394(15) 1 calc PR A 2
H41F H 0.8553 0.7311 -0.3040 0.411 Uiso 0.394(15) 1 calc PR A 2
O7 O 1.2142(9) 0.2751(9) 0.3505(10) 0.257(7) Uiso 0.618(14) 1 d PDU B 3
O8 O 1.1416(6) 0.2905(6) 0.4697(7) 0.150(4) Uiso 0.618(14) 1 d PDU B 3
C34 C 1.1557(13) 0.2590(16) 0.323(2) 0.363(17) Uiso 0.618(14) 1 d PDU B 3
H34A H 1.1290 0.2158 0.3277 0.545 Uiso 0.618(14) 1 calc PR B 3
H34B H 1.1593 0.2702 0.2744 0.545 Uiso 0.618(14) 1 calc PR B 3
H34C H 1.1392 0.2800 0.3491 0.545 Uiso 0.618(14) 1 calc PR B 3
C35 C 1.2354(8) 0.3250(9) 0.3980(9) 0.199(6) Uiso 0.618(14) 1 d PDU B 3
H35A H 1.2294 0.3563 0.3761 0.239 Uiso 0.618(14) 1 calc PR B 3
H35B H 1.2789 0.3420 0.4043 0.239 Uiso 0.618(14) 1 calc PR B 3
C36 C 1.2058(6) 0.3113(9) 0.4699(7) 0.177(6) Uiso 0.618(14) 1 d PDU B 3
H36A H 1.2120 0.2804 0.4922 0.212 Uiso 0.618(14) 1 calc PR B 3
H36B H 1.2262 0.3478 0.4985 0.212 Uiso 0.618(14) 1 calc PR B 3
C37 C 1.1140(9) 0.2608(11) 0.5337(9) 0.214(9) Uiso 0.618(14) 1 d PDU B 3
H37A H 1.0922 0.2176 0.5264 0.322 Uiso 0.618(14) 1 calc PR B 3
H37B H 1.0863 0.2738 0.5493 0.322 Uiso 0.618(14) 1 calc PR B 3
H37C H 1.1449 0.2710 0.5688 0.322 Uiso 0.618(14) 1 calc PR B 3
O7A O 1.2688(13) 0.3172(14) 0.2998(11) 0.253(10) Uiso 0.382(14) 1 d PDU B 4
O8A O 1.1585(5) 0.2967(5) 0.4516(5) 0.080(4) Uiso 0.382(14) 1 d PDU B 4
C34A C 1.3316(14) 0.336(3) 0.308(3) 0.34(2) Uiso 0.382(14) 1 d PDU B 4
H34D H 1.3421 0.3128 0.2776 0.506 Uiso 0.382(14) 1 calc PR B 4
H34E H 1.3392 0.3303 0.3562 0.506 Uiso 0.382(14) 1 calc PR B 4
H34F H 1.3557 0.3786 0.2963 0.506 Uiso 0.382(14) 1 calc PR B 4
C35A C 1.2421(14) 0.3262(16) 0.3607(11) 0.184(8) Uiso 0.382(14) 1 d PDU B 4
H35C H 1.2033 0.3157 0.3394 0.221 Uiso 0.382(14) 1 calc PR B 4
H35D H 1.2645 0.3703 0.3595 0.221 Uiso 0.382(14) 1 calc PR B 4
C36A C 1.2215(6) 0.3200(10) 0.4358(9) 0.112(5) Uiso 0.382(14) 1 d PDU B 4
H36C H 1.2339 0.2942 0.4596 0.135 Uiso 0.382(14) 1 calc PR B 4
H36D H 1.2440 0.3600 0.4573 0.135 Uiso 0.382(14) 1 calc PR B 4
C37A C 1.1491(9) 0.2884(10) 0.5263(6) 0.118(6) Uiso 0.382(14) 1 d PDU B 4
H37D H 1.1480 0.2514 0.5401 0.177 Uiso 0.382(14) 1 calc PR B 4
H37E H 1.1112 0.2860 0.5384 0.177 Uiso 0.382(14) 1 calc PR B 4
H37F H 1.1818 0.3223 0.5504 0.177 Uiso 0.382(14) 1 calc PR B 4
O11 O 0.1324(8) 0.1633(8) -0.5861(10) 0.210(6) Uiso 0.50 1 d P C 1
O11A O 0.0587(9) 0.1141(10) -0.4737(12) 0.231(7) Uiso 0.50 1 d P D 2
O12 O 0.9875(18) 0.8855(18) 0.664(2) 0.351(16) Uiso 0.50 1 d P E 1
O12A O 0.9394(17) 0.8492(16) 0.685(2) 0.325(14) Uiso 0.50 1 d P F 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
O1 C14 1.221(11) . ?
O1 H1B 0.8200 . ?
O2 C14 1.291(11) . ?
O2 H2B 0.8200 . ?
O3 C23 1.253(5) . ?
O4 C23 1.275(5) . ?
O4 H4B 0.8200 . ?
O5 C32 1.215(5) . ?
O6 C32 1.333(5) . ?
O6 H6B 0.8200 . ?
C1 C6 1.388(5) . ?
C1 C2 1.390(5) . ?
C1 C7 1.497(6) . ?
C2 C3 1.393(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.395(5) . ?
C3 C16 1.490(5) . ?
C4 C5 1.379(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.384(5) . ?
C5 C25 1.514(5) . ?
C6 H6A 0.9300 . ?
C7 C8 1.404(6) . ?
C7 C12 1.406(6) . ?
C8 C9 1.406(6) . ?
C8 C13 1.489(7) . ?
C9 C10 1.414(8) . ?
C9 H9A 0.9300 . ?
C10 C11 1.341(8) . ?
C10 C14 1.513(9) . ?
C11 C12 1.396(7) . ?
C11 H11A 0.9300 . ?
C12 C15 1.483(8) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C21 1.401(5) . ?
C16 C17 1.412(5) . ?
C17 C18 1.390(5) . ?
C17 C22 1.506(6) . ?
C18 C19 1.390(6) . ?
C18 H18A 0.9300 . ?
C19 C20 1.393(5) . ?
C19 C23 1.491(5) . ?
C20 C21 1.385(5) . ?
C20 H20A 0.9300 . ?
C21 C24 1.512(5) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C30 1.388(5) . ?
C25 C26 1.410(5) . ?
C26 C27 1.389(6) . ?
C26 C31 1.508(6) . ?
C28 C27 1.379(6) . ?
C28 C29 1.391(5) . ?
C28 C32 1.472(6) . ?
C27 H27A 0.9300 . ?
C29 C30 1.374(5) . ?
C29 H29A 0.9300 . ?
C30 C33 1.508(5) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
O1A C14A 1.244(5) . ?
O2A C14A 1.266(5) . ?
O2A H2AA 0.8200 . ?
O3A C23A 1.240(17) . ?
O3A H3AA 0.8200 . ?
O4A C23A 1.311(18) . ?
O4A H4AA 0.8200 . ?
O5A C32A 1.316(6) . ?
O5A H5AA 0.8200 . ?
O6A C32A 1.201(5) . ?
C1A C6A 1.386(5) . ?
C1A C2A 1.394(5) . ?
C1A C7A 1.512(5) . ?
C2A C3A 1.378(5) . ?
C2A H2AB 0.9300 . ?
C3A C4A 1.396(5) . ?
C3A C16A 1.486(6) . ?
C4A C5A 1.380(5) . ?
C4A H4AB 0.9300 . ?
C5A C6A 1.390(5) . ?
C5A C25A 1.500(5) . ?
C6A H6AA 0.9300 . ?
C7A C8A 1.401(5) . ?
C7A C12A 1.405(5) . ?
C8A C9A 1.395(5) . ?
C8A C13A 1.489(5) . ?
C9A C10A 1.384(5) . ?
C9A H9AA 0.9300 . ?
C10A C11A 1.389(6) . ?
C10A C14A 1.481(5) . ?
C11A C12A 1.380(5) . ?
C11A H11B 0.9300 . ?
C12A C15A 1.519(6) . ?
C13A H13D 0.9600 . ?
C13A H13E 0.9600 . ?
C13A H13F 0.9600 . ?
C15A H15D 0.9600 . ?
C15A H15E 0.9600 . ?
C15A H15F 0.9600 . ?
C16A C17A 1.396(7) . ?
C16A C21A 1.411(7) . ?
C17A C18A 1.423(8) . ?
C17A C22A 1.497(7) . ?
C18A C19A 1.361(10) . ?
C18A H18B 0.9300 . ?
C19A C20A 1.378(9) . ?
C19A C23A 1.508(11) . ?
C20A C21A 1.398(8) . ?
C20A H20B 0.9300 . ?
C21A C24A 1.518(8) . ?
C22A H22D 0.9600 . ?
C22A H22E 0.9600 . ?
C22A H22F 0.9600 . ?
C24A H24D 0.9600 . ?
C24A H24E 0.9600 . ?
C24A H24F 0.9600 . ?
C25A C30A 1.378(6) . ?
C25A C26A 1.422(6) . ?
C26A C27A 1.384(6) . ?
C26A C31A 1.486(6) . ?
C27A C28A 1.359(6) . ?
C27A H27B 0.9300 . ?
C28A C29A 1.395(6) . ?
C28A C32A 1.509(6) . ?
C29A C30A 1.420(7) . ?
C29A H29B 0.9300 . ?
C30A C33A 1.504(7) . ?
C31A H31D 0.9600 . ?
C31A H31E 0.9600 . ?
C31A H31F 0.9600 . ?
C33A H33D 0.9600 . ?
C33A H33E 0.9600 . ?
C33A H33F 0.9600 . ?
O9 C39 1.424(7) . ?
O9 C38 1.436(7) . ?
O10 C40 1.417(7) . ?
O10 C41 1.423(7) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.507(7) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
O9A C38A 1.407(7) . ?
O9A C39A 1.424(7) . ?
O10A C41A 1.417(7) . ?
O10A C40A 1.421(7) . ?
C38A H38D 0.9600 . ?
C38A H38E 0.9600 . ?
C38A H38F 0.9600 . ?
C39A C40A 1.517(7) . ?
C39A H39C 0.9700 . ?
C39A H39D 0.9700 . ?
C40A H40C 0.9700 . ?
C40A H40D 0.9700 . ?
C41A H41D 0.9600 . ?
C41A H41E 0.9600 . ?
C41A H41F 0.9600 . ?
O7 C35 1.423(7) . ?
O7 C34 1.425(7) . ?
O8 C37 1.416(7) . ?
O8 C36 1.437(7) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.513(7) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
O7A C35A 1.415(7) . ?
O7A C34A 1.421(7) . ?
O8A C36A 1.430(7) . ?
O8A C37A 1.436(7) . ?
C34A H34D 0.9600 . ?
C34A H34E 0.9600 . ?
C34A H34F 0.9600 . ?
C35A C36A 1.499(7) . ?
C35A H35C 0.9700 . ?
C35A H35D 0.9700 . ?
C36A H36C 0.9700 . ?
C36A H36D 0.9700 . ?
C37A H37D 0.9600 . ?
C37A H37E 0.9600 . ?
C37A H37F 0.9600 . ?

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
C14 O1 H1B 109.5 . . ?
C14 O2 H2B 109.5 . . ?
C23 O4 H4B 109.5 . . ?
C32 O6 H6B 109.5 . . ?
C6 C1 C2 118.3(3) . . ?
C6 C1 C7 119.6(3) . . ?
C2 C1 C7 122.0(3) . . ?
C1 C2 C3 121.7(3) . . ?
C1 C2 H2A 119.1 . . ?
C3 C2 H2A 119.1 . . ?
C2 C3 C4 117.9(3) . . ?
C2 C3 C16 122.1(3) . . ?
C4 C3 C16 119.9(3) . . ?
C5 C4 C3 121.4(3) . . ?
C5 C4 H4A 119.3 . . ?
C3 C4 H4A 119.3 . . ?
C4 C5 C6 119.3(3) . . ?
C4 C5 C25 120.7(3) . . ?
C6 C5 C25 119.9(3) . . ?
C5 C6 C1 121.3(3) . . ?
C5 C6 H6A 119.4 . . ?
C1 C6 H6A 119.4 . . ?
C8 C7 C12 122.2(4) . . ?
C8 C7 C1 118.1(4) . . ?
C12 C7 C1 119.7(4) . . ?
C7 C8 C9 117.9(5) . . ?
C7 C8 C13 121.8(4) . . ?
C9 C8 C13 120.2(5) . . ?
C8 C9 C10 119.8(5) . . ?
C8 C9 H9A 120.1 . . ?
C10 C9 H9A 120.1 . . ?
C11 C10 C9 120.1(5) . . ?
C11 C10 C14 123.5(7) . . ?
C9 C10 C14 116.5(7) . . ?
C10 C11 C12 123.1(5) . . ?
C10 C11 H11A 118.4 . . ?
C12 C11 H11A 118.4 . . ?
C11 C12 C7 116.8(5) . . ?
C11 C12 C15 122.0(5) . . ?
C7 C12 C15 121.2(4) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C14 O2 126.4(7) . . ?
O1 C14 C10 120.5(9) . . ?
O2 C14 C10 113.1(9) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 120.5(3) . . ?
C21 C16 C3 119.3(3) . . ?
C17 C16 C3 120.2(3) . . ?
C18 C17 C16 118.5(4) . . ?
C18 C17 C22 119.3(3) . . ?
C16 C17 C22 122.1(3) . . ?
C19 C18 C17 120.9(3) . . ?
C19 C18 H18A 119.5 . . ?
C17 C18 H18A 119.5 . . ?
C18 C19 C20 120.2(3) . . ?
C18 C19 C23 120.1(3) . . ?
C20 C19 C23 119.7(4) . . ?
C21 C20 C19 120.1(3) . . ?
C21 C20 H20A 119.9 . . ?
C19 C20 H20A 119.9 . . ?
C20 C21 C16 119.7(3) . . ?
C20 C21 C24 118.5(3) . . ?
C16 C21 C24 121.7(3) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O3 C23 O4 124.1(3) . . ?
O3 C23 C19 118.5(4) . . ?
O4 C23 C19 117.4(3) . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 121.6(3) . . ?
C30 C25 C5 118.6(3) . . ?
C26 C25 C5 119.8(3) . . ?
C27 C26 C25 117.8(4) . . ?
C27 C26 C31 120.8(3) . . ?
C25 C26 C31 121.4(3) . . ?
C27 C28 C29 119.0(3) . . ?
C27 C28 C32 123.0(4) . . ?
C29 C28 C32 118.0(4) . . ?
C28 C27 C26 121.4(4) . . ?
C28 C27 H27A 119.3 . . ?
C26 C27 H27A 119.3 . . ?
C30 C29 C28 121.8(4) . . ?
C30 C29 H29A 119.1 . . ?
C28 C29 H29A 119.1 . . ?
C29 C30 C25 118.3(3) . . ?
C29 C30 C33 120.2(3) . . ?
C25 C30 C33 121.5(3) . . ?
O5 C32 O6 122.4(4) . . ?
O5 C32 C28 123.2(4) . . ?
O6 C32 C28 114.3(4) . . ?
C26 C31 H31A 109.5 . . ?
C26 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C26 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C14A O2A H2AA 109.5 . . ?
C23A O3A H3AA 109.5 . . ?
C23A O4A H4AA 109.5 . . ?
C32A O5A H5AA 109.5 . . ?
C6A C1A C2A 119.0(3) . . ?
C6A C1A C7A 122.9(3) . . ?
C2A C1A C7A 117.8(3) . . ?
C3A C2A C1A 121.3(3) . . ?
C3A C2A H2AB 119.3 . . ?
C1A C2A H2AB 119.3 . . ?
C2A C3A C4A 118.4(3) . . ?
C2A C3A C16A 120.5(3) . . ?
C4A C3A C16A 121.0(3) . . ?
C5A C4A C3A 121.5(3) . . ?
C5A C4A H4AB 119.3 . . ?
C3A C4A H4AB 119.3 . . ?
C4A C5A C6A 119.0(3) . . ?
C4A C5A C25A 119.7(3) . . ?
C6A C5A C25A 121.2(3) . . ?
C1A C6A C5A 120.7(4) . . ?
C1A C6A H6AA 119.7 . . ?
C5A C6A H6AA 119.7 . . ?
C8A C7A C12A 120.8(3) . . ?
C8A C7A C1A 118.4(3) . . ?
C12A C7A C1A 120.7(3) . . ?
C9A C8A C7A 118.5(3) . . ?
C9A C8A C13A 119.9(3) . . ?
C7A C8A C13A 121.5(3) . . ?
C10A C9A C8A 121.0(3) . . ?
C10A C9A H9AA 119.5 . . ?
C8A C9A H9AA 119.5 . . ?
C9A C10A C11A 119.5(3) . . ?
C9A C10A C14A 119.5(4) . . ?
C11A C10A C14A 120.7(4) . . ?
C12A C11A C10A 121.2(3) . . ?
C12A C11A H11B 119.4 . . ?
C10A C11A H11B 119.4 . . ?
C11A C12A C7A 118.8(3) . . ?
C11A C12A C15A 120.3(3) . . ?
C7A C12A C15A 120.9(3) . . ?
C8A C13A H13D 109.5 . . ?
C8A C13A H13E 109.5 . . ?
H13D C13A H13E 109.5 . . ?
C8A C13A H13F 109.5 . . ?
H13D C13A H13F 109.5 . . ?
H13E C13A H13F 109.5 . . ?
O1A C14A O2A 122.5(4) . . ?
O1A C14A C10A 120.8(4) . . ?
O2A C14A C10A 116.6(4) . . ?
C12A C15A H15D 109.5 . . ?
C12A C15A H15E 109.5 . . ?
H15D C15A H15E 109.5 . . ?
C12A C15A H15F 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
C17A C16A C21A 121.7(4) . . ?
C17A C16A C3A 119.8(4) . . ?
C21A C16A C3A 118.5(4) . . ?
C16A C17A C18A 116.5(5) . . ?
C16A C17A C22A 121.7(4) . . ?
C18A C17A C22A 121.8(5) . . ?
C19A C18A C17A 121.9(6) . . ?
C19A C18A H18B 119.0 . . ?
C17A C18A H18B 119.0 . . ?
C18A C19A C20A 121.0(5) . . ?
C18A C19A C23A 116.8(10) . . ?
C20A C19A C23A 122.2(10) . . ?
C19A C20A C21A 119.8(6) . . ?
C19A C20A H20B 120.1 . . ?
C21A C20A H20B 120.1 . . ?
C20A C21A C16A 119.1(6) . . ?
C20A C21A C24A 119.0(5) . . ?
C16A C21A C24A 121.9(4) . . ?
C17A C22A H22D 109.5 . . ?
C17A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C17A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
O3A C23A O4A 126.4(9) . . ?
O3A C23A C19A 120.1(14) . . ?
O4A C23A C19A 113.6(13) . . ?
C21A C24A H24D 109.5 . . ?
C21A C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
C21A C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C30A C25A C26A 121.7(3) . . ?
C30A C25A C5A 119.5(4) . . ?
C26A C25A C5A 118.7(3) . . ?
C27A C26A C25A 118.2(4) . . ?
C27A C26A C31A 119.4(4) . . ?
C25A C26A C31A 122.3(3) . . ?
C28A C27A C26A 121.1(4) . . ?
C28A C27A H27B 119.5 . . ?
C26A C27A H27B 119.5 . . ?
C27A C28A C29A 121.2(4) . . ?
C27A C28A C32A 119.5(4) . . ?
C29A C28A C32A 119.2(4) . . ?
C28A C29A C30A 119.6(4) . . ?
C28A C29A H29B 120.2 . . ?
C30A C29A H29B 120.2 . . ?
C25A C30A C29A 118.1(4) . . ?
C25A C30A C33A 122.2(4) . . ?
C29A C30A C33A 119.7(4) . . ?
C26A C31A H31D 109.5 . . ?
C26A C31A H31E 109.5 . . ?
H31D C31A H31E 109.5 . . ?
C26A C31A H31F 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
O6A C32A O5A 122.2(4) . . ?
O6A C32A C28A 124.2(4) . . ?
O5A C32A C28A 113.6(4) . . ?
C30A C33A H33D 109.5 . . ?
C30A C33A H33E 109.5 . . ?
H33D C33A H33E 109.5 . . ?
C30A C33A H33F 109.5 . . ?
H33D C33A H33F 109.5 . . ?
H33E C33A H33F 109.5 . . ?
C39 O9 C38 110.6(7) . . ?
C40 O10 C41 111.4(8) . . ?
O9 C38 H38A 109.5 . . ?
O9 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O9 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O9 C39 C40 110.0(7) . . ?
O9 C39 H39A 109.7 . . ?
C40 C39 H39A 109.7 . . ?
O9 C39 H39B 109.7 . . ?
C40 C39 H39B 109.7 . . ?
H39A C39 H39B 108.2 . . ?
O10 C40 C39 110.7(8) . . ?
O10 C40 H40A 109.5 . . ?
C39 C40 H40A 109.5 . . ?
O10 C40 H40B 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 108.1 . . ?
O10 C41 H41A 109.5 . . ?
O10 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O10 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C38A O9A C39A 112.5(8) . . ?
C41A O10A C40A 111.9(8) . . ?
O9A C38A H38D 109.5 . . ?
O9A C38A H38E 109.5 . . ?
H38D C38A H38E 109.5 . . ?
O9A C38A H38F 109.5 . . ?
H38D C38A H38F 109.5 . . ?
H38E C38A H38F 109.5 . . ?
O9A C39A C40A 108.6(7) . . ?
O9A C39A H39C 110.0 . . ?
C40A C39A H39C 110.0 . . ?
O9A C39A H39D 110.0 . . ?
C40A C39A H39D 110.0 . . ?
H39C C39A H39D 108.3 . . ?
O10A C40A C39A 109.5(7) . . ?
O10A C40A H40C 109.8 . . ?
C39A C40A H40C 109.8 . . ?
O10A C40A H40D 109.8 . . ?
C39A C40A H40D 109.8 . . ?
H40C C40A H40D 108.2 . . ?
O10A C41A H41D 109.5 . . ?
O10A C41A H41E 109.5 . . ?
H41D C41A H41E 109.5 . . ?
O10A C41A H41F 109.5 . . ?
H41D C41A H41F 109.5 . . ?
H41E C41A H41F 109.5 . . ?
C35 O7 C34 111.1(8) . . ?
C37 O8 C36 111.1(7) . . ?
O7 C34 H34A 109.5 . . ?
O7 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O7 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O7 C35 C36 116.3(10) . . ?
O7 C35 H35A 108.2 . . ?
C36 C35 H35A 108.2 . . ?
O7 C35 H35B 108.2 . . ?
C36 C35 H35B 108.2 . . ?
H35A C35 H35B 107.4 . . ?
O8 C36 C35 115.0(10) . . ?
O8 C36 H36A 108.5 . . ?
C35 C36 H36A 108.5 . . ?
O8 C36 H36B 108.5 . . ?
C35 C36 H36B 108.5 . . ?
H36A C36 H36B 107.5 . . ?
O8 C37 H37A 109.5 . . ?
O8 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O8 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35A O7A C34A 113.4(8) . . ?
C36A O8A C37A 109.6(7) . . ?
O7A C34A H34D 109.5 . . ?
O7A C34A H34E 109.5 . . ?
H34D C34A H34E 109.5 . . ?
O7A C34A H34F 109.5 . . ?
H34D C34A H34F 109.5 . . ?
H34E C34A H34F 109.5 . . ?
O7A C35A C36A 159(3) . . ?
O7A C35A H35C 96.6 . . ?
C36A C35A H35C 96.6 . . ?
O7A C35A H35D 96.6 . . ?
C36A C35A H35D 96.6 . . ?
H35C C35A H35D 103.5 . . ?
O8A C36A C35A 120.1(16) . . ?
O8A C36A H36C 107.3 . . ?
C35A C36A H36C 107.3 . . ?
O8A C36A H36D 107.3 . . ?
C35A C36A H36D 107.3 . . ?
H36C C36A H36D 106.9 . . ?
O8A C37A H37D 109.5 . . ?
O8A C37A H37E 109.5 . . ?
H37D C37A H37E 109.5 . . ?
O8A C37A H37F 109.5 . . ?
H37D C37A H37F 109.5 . . ?
H37E C37A H37F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.4(5) . . . . ?
C7 C1 C2 C3 179.4(4) . . . . ?
C1 C2 C3 C4 0.2(5) . . . . ?
C1 C2 C3 C16 -177.3(3) . . . . ?
C2 C3 C4 C5 -1.4(5) . . . . ?
C16 C3 C4 C5 176.1(3) . . . . ?
C3 C4 C5 C6 2.0(6) . . . . ?
C3 C4 C5 C25 -173.2(3) . . . . ?
C4 C5 C6 C1 -1.4(6) . . . . ?
C25 C5 C6 C1 173.9(4) . . . . ?
C2 C1 C6 C5 0.2(6) . . . . ?
C7 C1 C6 C5 -178.9(4) . . . . ?
C6 C1 C7 C8 76.4(5) . . . . ?
C2 C1 C7 C8 -102.6(4) . . . . ?
C6 C1 C7 C12 -101.7(4) . . . . ?
C2 C1 C7 C12 79.3(5) . . . . ?
C12 C7 C8 C9 0.5(6) . . . . ?
C1 C7 C8 C9 -177.5(3) . . . . ?
C12 C7 C8 C13 -176.8(4) . . . . ?
C1 C7 C8 C13 5.2(5) . . . . ?
C7 C8 C9 C10 -0.5(6) . . . . ?
C13 C8 C9 C10 176.8(4) . . . . ?
C8 C9 C10 C11 0.4(7) . . . . ?
C8 C9 C10 C14 179.9(4) . . . . ?
C9 C10 C11 C12 -0.3(7) . . . . ?
C14 C10 C11 C12 -179.7(5) . . . . ?
C10 C11 C12 C7 0.2(7) . . . . ?
C10 C11 C12 C15 -178.6(5) . . . . ?
C8 C7 C12 C11 -0.4(6) . . . . ?
C1 C7 C12 C11 177.6(3) . . . . ?
C8 C7 C12 C15 178.5(4) . . . . ?
C1 C7 C12 C15 -3.5(6) . . . . ?
C11 C10 C14 O1 179.3(6) . . . . ?
C9 C10 C14 O1 -0.1(8) . . . . ?
C11 C10 C14 O2 1.0(8) . . . . ?
C9 C10 C14 O2 -178.4(5) . . . . ?
C2 C3 C16 C21 115.7(4) . . . . ?
C4 C3 C16 C21 -61.8(4) . . . . ?
C2 C3 C16 C17 -63.7(5) . . . . ?
C4 C3 C16 C17 118.9(4) . . . . ?
C21 C16 C17 C18 -0.8(5) . . . . ?
C3 C16 C17 C18 178.6(3) . . . . ?
C21 C16 C17 C22 177.3(3) . . . . ?
C3 C16 C17 C22 -3.4(5) . . . . ?
C16 C17 C18 C19 0.7(5) . . . . ?
C22 C17 C18 C19 -177.3(4) . . . . ?
C17 C18 C19 C20 0.1(5) . . . . ?
C17 C18 C19 C23 178.7(3) . . . . ?
C18 C19 C20 C21 -1.0(5) . . . . ?
C23 C19 C20 C21 -179.5(3) . . . . ?
C19 C20 C21 C16 0.9(5) . . . . ?
C19 C20 C21 C24 -179.3(3) . . . . ?
C17 C16 C21 C20 -0.1(5) . . . . ?
C3 C16 C21 C20 -179.4(3) . . . . ?
C17 C16 C21 C24 -179.8(3) . . . . ?
C3 C16 C21 C24 0.8(5) . . . . ?
C18 C19 C23 O3 19.0(5) . . . . ?
C20 C19 C23 O3 -162.4(3) . . . . ?
C18 C19 C23 O4 -159.6(3) . . . . ?
C20 C19 C23 O4 19.0(5) . . . . ?
C4 C5 C25 C30 89.4(4) . . . . ?
C6 C5 C25 C30 -85.7(4) . . . . ?
C4 C5 C25 C26 -91.4(4) . . . . ?
C6 C5 C25 C26 93.4(4) . . . . ?
C30 C25 C26 C27 1.6(5) . . . . ?
C5 C25 C26 C27 -177.5(3) . . . . ?
C30 C25 C26 C31 -176.8(3) . . . . ?
C5 C25 C26 C31 4.0(5) . . . . ?
C29 C28 C27 C26 -1.2(5) . . . . ?
C32 C28 C27 C26 179.0(3) . . . . ?
C25 C26 C27 C28 0.4(5) . . . . ?
C31 C26 C27 C28 178.8(3) . . . . ?
C27 C28 C29 C30 0.1(5) . . . . ?
C32 C28 C29 C30 179.9(3) . . . . ?
C28 C29 C30 C25 1.8(5) . . . . ?
C28 C29 C30 C33 -176.9(3) . . . . ?
C26 C25 C30 C29 -2.7(5) . . . . ?
C5 C25 C30 C29 176.5(3) . . . . ?
C26 C25 C30 C33 176.1(3) . . . . ?
C5 C25 C30 C33 -4.8(5) . . . . ?
C27 C28 C32 O5 -178.8(4) . . . . ?
C29 C28 C32 O5 1.4(6) . . . . ?
C27 C28 C32 O6 4.2(5) . . . . ?
C29 C28 C32 O6 -175.5(3) . . . . ?
C6A C1A C2A C3A 0.3(5) . . . . ?
C7A C1A C2A C3A 174.7(3) . . . . ?
C1A C2A C3A C4A -0.5(5) . . . . ?
C1A C2A C3A C16A -178.5(3) . . . . ?
C2A C3A C4A C5A 0.3(5) . . . . ?
C16A C3A C4A C5A 178.3(4) . . . . ?
C3A C4A C5A C6A 0.2(5) . . . . ?
C3A C4A C5A C25A -177.3(4) . . . . ?
C2A C1A C6A C5A 0.2(5) . . . . ?
C7A C1A C6A C5A -174.0(3) . . . . ?
C4A C5A C6A C1A -0.4(5) . . . . ?
C25A C5A C6A C1A 177.1(4) . . . . ?
C6A C1A C7A C8A 70.7(4) . . . . ?
C2A C1A C7A C8A -103.5(4) . . . . ?
C6A C1A C7A C12A -113.4(4) . . . . ?
C2A C1A C7A C12A 72.4(4) . . . . ?
C12A C7A C8A C9A -2.5(5) . . . . ?
C1A C7A C8A C9A 173.5(3) . . . . ?
C12A C7A C8A C13A -179.4(3) . . . . ?
C1A C7A C8A C13A -3.4(5) . . . . ?
C7A C8A C9A C10A -1.6(5) . . . . ?
C13A C8A C9A C10A 175.3(3) . . . . ?
C8A C9A C10A C11A 3.8(5) . . . . ?
C8A C9A C10A C14A -170.2(3) . . . . ?
C9A C10A C11A C12A -2.0(5) . . . . ?
C14A C10A C11A C12A 172.0(3) . . . . ?
C10A C11A C12A C7A -2.0(5) . . . . ?
C10A C11A C12A C15A 179.5(3) . . . . ?
C8A C7A C12A C11A 4.3(5) . . . . ?
C1A C7A C12A C11A -171.6(3) . . . . ?
C8A C7A C12A C15A -177.2(3) . . . . ?
C1A C7A C12A C15A 6.9(5) . . . . ?
C9A C10A C14A O1A 159.2(4) . . . . ?
C11A C10A C14A O1A -14.8(6) . . . . ?
C9A C10A C14A O2A -17.2(5) . . . . ?
C11A C10A C14A O2A 168.8(3) . . . . ?
C2A C3A C16A C17A -72.2(5) . . . . ?
C4A C3A C16A C17A 109.8(4) . . . . ?
C2A C3A C16A C21A 106.5(4) . . . . ?
C4A C3A C16A C21A -71.5(5) . . . . ?
C21A C16A C17A C18A 0.5(6) . . . . ?
C3A C16A C17A C18A 179.1(4) . . . . ?
C21A C16A C17A C22A -179.3(4) . . . . ?
C3A C16A C17A C22A -0.7(6) . . . . ?
C16A C17A C18A C19A -0.9(7) . . . . ?
C22A C17A C18A C19A 178.9(5) . . . . ?
C17A C18A C19A C20A 0.9(8) . . . . ?
C17A C18A C19A C23A -177.9(5) . . . . ?
C18A C19A C20A C21A -0.6(8) . . . . ?
C23A C19A C20A C21A 178.2(6) . . . . ?
C19A C20A C21A C16A 0.2(7) . . . . ?
C19A C20A C21A C24A -178.4(4) . . . . ?
C17A C16A C21A C20A -0.1(6) . . . . ?
C3A C16A C21A C20A -178.8(3) . . . . ?
C17A C16A C21A C24A 178.4(4) . . . . ?
C3A C16A C21A C24A -0.3(6) . . . . ?
C18A C19A C23A O3A 9.4(10) . . . . ?
C20A C19A C23A O3A -169.5(7) . . . . ?
C18A C19A C23A O4A -171.1(6) . . . . ?
C20A C19A C23A O4A 10.1(10) . . . . ?
C4A C5A C25A C30A 106.2(4) . . . . ?
C6A C5A C25A C30A -71.3(5) . . . . ?
C4A C5A C25A C26A -71.3(5) . . . . ?
C6A C5A C25A C26A 111.3(4) . . . . ?
C30A C25A C26A C27A 2.1(6) . . . . ?
C5A C25A C26A C27A 179.5(3) . . . . ?
C30A C25A C26A C31A -174.4(4) . . . . ?
C5A C25A C26A C31A 3.0(5) . . . . ?
C25A C26A C27A C28A -1.1(6) . . . . ?
C31A C26A C27A C28A 175.6(4) . . . . ?
C26A C27A C28A C29A -1.0(6) . . . . ?
C26A C27A C28A C32A -177.3(4) . . . . ?
C27A C28A C29A C30A 2.0(6) . . . . ?
C32A C28A C29A C30A 178.4(4) . . . . ?
C26A C25A C30A C29A -1.1(6) . . . . ?
C5A C25A C30A C29A -178.5(4) . . . . ?
C26A C25A C30A C33A 178.1(5) . . . . ?
C5A C25A C30A C33A 0.7(7) . . . . ?
C28A C29A C30A C25A -1.0(7) . . . . ?
C28A C29A C30A C33A 179.8(5) . . . . ?
C27A C28A C32A O6A -7.1(7) . . . . ?
C29A C28A C32A O6A 176.5(5) . . . . ?
C27A C28A C32A O5A 172.9(4) . . . . ?
C29A C28A C32A O5A -3.5(6) . . . . ?
C38 O9 C39 C40 -169.3(19) . . . . ?
C41 O10 C40 C39 -94(3) . . . . ?
O9 C39 C40 O10 143(2) . . . . ?
C38A O9A C39A C40A 178(2) . . . . ?
C41A O10A C40A C39A -97(3) . . . . ?
O9A C39A C40A O10A 37(3) . . . . ?
C34 O7 C35 C36 75(3) . . . . ?
C37 O8 C36 C35 161.4(18) . . . . ?
O7 C35 C36 O8 -63(2) . . . . ?
C34A O7A C35A C36A -60(9) . . . . ?
C37A O8A C36A C35A 173(2) . . . . ?
O7A C35A C36A O8A -121(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.059
_database_code_depnum_ccdc_archive 'CCDC 974556'

data_Global
_publ_contact_author_name        'Prof. J. N. Moorthy'
_publ_contact_author_address     
;Departmet of chemistry
Indian Institute of Technology - Kanpur
Kanpur - 208 016
INDIA
;
_publ_contact_author_email       moorthy@iitk.ac.in
_publ_contact_author_phone       +915122597438
_publ_contact_author_fax         +915122597436
loop_
_publ_author_name
_publ_author_address


'Prof. J. N. Moorthy, '
;Departmet of chemistry
Indian Institute of Technology - Kanpur
Kanpur - 208 016
INDIA
;
'Alankriti Bajpai'
;Department of Chemistry
Indian Institute of Technology
Kanpur 208 016
INDIA
;
'Prof. P. Venugopalan'
;Department of Chemistry
Panjab University
Chandigrah 560017
INDIA
;
data_MeBTB-DBC

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            
;
1,3,5-Tris(2,6-dimethyl-4-carboxyphenyl)benzene + 2*dibenzocrown + 1.5K+
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C73 H80 K1.5 O20'
_chemical_formula_weight         1336.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   8.6821(8)
_cell_length_b                   29.796(3)
_cell_length_c                   12.8045(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.432(2)
_cell_angle_gamma                90.00
_cell_volume                     3291.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       cube
_exptl_crystal_colour            colorss
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1414
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER AXS KAPPA APEX-II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17091
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         25.00
_reflns_number_total             10384
_reflns_number_gt                6817
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97

_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)+(0.0567P)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    constr
_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   0.00(6)
_refine_ls_number_reflns         10384
_refine_ls_number_parameters     856
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0710
_refine_ls_wR_factor_ref         0.1556
_refine_ls_wR_factor_gt          0.1380
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.114
_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
K1 K 0.33297(15) 0.61791(4) 0.79750(10) 0.0403(3) Uani 1 1 d . . .
K2 K -0.3675(4) 0.62706(15) 0.7736(3) 0.0950(13) Uani 0.50 1 d P . .
O1 O 0.7485(5) 0.58379(13) 1.2264(3) 0.0498(11) Uani 1 1 d . . .
O2 O 0.9921(5) 0.56379(13) 1.2142(3) 0.0505(11) Uani 1 1 d . . .
O3 O 1.6933(5) 0.92189(14) 1.7911(3) 0.0488(11) Uani 1 1 d . . .
O4 O 1.4956(5) 0.91996(13) 1.8877(3) 0.0457(10) Uani 1 1 d . . .
O5 O 0.8477(5) 0.98549(13) 0.8852(3) 0.0444(10) Uani 1 1 d . . .
O6 O 1.0994(5) 0.99547(13) 0.8841(3) 0.0492(11) Uani 1 1 d . . .
O7 O 0.2269(5) 0.57212(16) 0.6205(4) 0.0623(14) Uani 1 1 d . . .
O8 O 0.1593(4) 0.66602(14) 0.6350(3) 0.0440(10) Uani 1 1 d . . .
O9 O 0.2827(4) 0.70895(12) 0.8241(3) 0.0375(10) Uani 1 1 d . . .
O10 O 0.4248(5) 0.66386(12) 0.9790(3) 0.0444(11) Uani 1 1 d . . .
O11 O 0.4821(5) 0.57085(14) 0.9599(4) 0.0586(13) Uani 1 1 d . . .
O12 O 0.3852(6) 0.52687(15) 0.7719(5) 0.0695(15) Uani 1 1 d . . .
O13 O -0.3024(6) 0.58038(15) 0.5689(3) 0.0586(12) Uani 1 1 d . . .
O14 O -0.3685(4) 0.67630(14) 0.5529(3) 0.0460(11) Uani 1 1 d . . .
O15 O -0.2799(5) 0.72502(13) 0.7461(3) 0.0468(11) Uani 1 1 d . . .
O16 O -0.1224(7) 0.68530(15) 0.9025(3) 0.0742(15) Uani 1 1 d DU . .
O17 O 0.0425(5) 0.60211(14) 0.8816(3) 0.0500(11) Uani 1 1 d U . .
O18 O -0.1644(8) 0.54833(16) 0.7356(4) 0.098(2) Uani 1 1 d DU . .
O19 O 0.5984(7) 0.5041(2) 1.2233(5) 0.105(2) Uani 1 1 d . . .
O20 O 1.3278(8) 0.5544(2) 1.2586(6) 0.120(2) Uani 1 1 d . . .
C1 C 1.0911(6) 0.77421(17) 1.3285(4) 0.0293(12) Uani 1 1 d . . .
C2 C 1.0593(6) 0.80535(17) 1.2472(4) 0.0302(12) Uani 1 1 d . . .
H2A H 1.0031 0.7960 1.1830 0.036 Uiso 1 1 calc R . .
C3 C 1.1079(6) 0.84940(17) 1.2585(4) 0.0298(13) Uani 1 1 d . . .
C4 C 1.1857(6) 0.86235(18) 1.3546(4) 0.0314(13) Uani 1 1 d . . .
H4A H 1.2194 0.8926 1.3638 0.038 Uiso 1 1 calc R . .
C5 C 1.2159(6) 0.83235(18) 1.4379(4) 0.0323(13) Uani 1 1 d . . .
C6 C 1.1675(6) 0.78810(18) 1.4228(4) 0.0339(13) Uani 1 1 d . . .
H6A H 1.1876 0.7671 1.4785 0.041 Uiso 1 1 calc R . .
C7 C 1.0394(6) 0.72621(17) 1.3096(4) 0.0274(12) Uani 1 1 d . . .
C8 C 1.1473(6) 0.69432(18) 1.2849(4) 0.0338(13) Uani 1 1 d . . .
C9 C 1.1000(6) 0.65000(17) 1.2637(4) 0.0308(13) Uani 1 1 d . . .
H9A H 1.1734 0.6279 1.2488 0.037 Uiso 1 1 calc R . .
C10 C 0.9456(6) 0.63853(17) 1.2644(4) 0.0290(12) Uani 1 1 d . . .
C11 C 0.8402(6) 0.67069(17) 1.2905(4) 0.0327(13) Uani 1 1 d . . .
H11A H 0.7346 0.6626 1.2916 0.039 Uiso 1 1 calc R . .
C12 C 0.8860(6) 0.71420(17) 1.3146(4) 0.0303(13) Uani 1 1 d . . .
C13 C 0.8860(8) 0.59129(18) 1.2331(4) 0.0382(14) Uani 1 1 d . . .
C14 C 1.3156(6) 0.7076(2) 1.2759(5) 0.0470(16) Uani 1 1 d . . .
H14A H 1.3776 0.6805 1.2688 0.071 Uiso 1 1 calc R . .
H14B H 1.3571 0.7241 1.3390 0.071 Uiso 1 1 calc R . .
H14C H 1.3197 0.7267 1.2139 0.071 Uiso 1 1 calc R . .
C15 C 0.7684(6) 0.74776(19) 1.3458(5) 0.0409(15) Uani 1 1 d . . .
H15A H 0.7439 0.7694 1.2887 0.061 Uiso 1 1 calc R . .
H15B H 0.8114 0.7637 1.4095 0.061 Uiso 1 1 calc R . .
H15C H 0.6737 0.7319 1.3595 0.061 Uiso 1 1 calc R . .
C16 C 1.3028(6) 0.84858(16) 1.5387(4) 0.0303(13) Uani 1 1 d . . .
C17 C 1.4648(6) 0.85262(17) 1.5457(4) 0.0331(13) Uani 1 1 d . . .
C18 C 1.5434(6) 0.87190(16) 1.6343(4) 0.0323(13) Uani 1 1 d . . .
H18A H 1.6526 0.8756 1.6384 0.039 Uiso 1 1 calc R . .
C19 C 1.4657(6) 0.88581(17) 1.7169(4) 0.0307(13) Uani 1 1 d . . .
C20 C 1.3077(7) 0.88047(17) 1.7121(4) 0.0356(14) Uani 1 1 d . . .
H20A H 1.2549 0.8891 1.7700 0.043 Uiso 1 1 calc R . .
C21 C 1.2255(6) 0.86242(18) 1.6228(4) 0.0367(14) Uani 1 1 d . . .
C22 C 1.5507(7) 0.91035(19) 1.8080(5) 0.0360(14) Uani 1 1 d . . .
C23 C 1.5513(6) 0.8380(2) 1.4541(5) 0.0429(15) Uani 1 1 d . . .
H23A H 1.5340 0.8600 1.3972 0.064 Uiso 1 1 calc R . .
H23B H 1.5131 0.8086 1.4287 0.064 Uiso 1 1 calc R . .
H23C H 1.6624 0.8360 1.4777 0.064 Uiso 1 1 calc R . .
C24 C 1.0479(7) 0.8578(2) 1.6159(5) 0.0483(16) Uani 1 1 d . . .
H24A H 1.0017 0.8666 1.5456 0.072 Uiso 1 1 calc R . .
H24B H 1.0083 0.8773 1.6685 0.072 Uiso 1 1 calc R . .
H24C H 1.0208 0.8266 1.6292 0.072 Uiso 1 1 calc R . .
C25 C 1.0758(6) 0.88189(17) 1.1698(4) 0.0275(12) Uani 1 1 d . . .
C26 C 0.9274(6) 0.89855(17) 1.1432(4) 0.0307(13) Uani 1 1 d . . .
C27 C 0.8984(6) 0.92769(17) 1.0592(4) 0.0318(13) Uani 1 1 d . . .
H27A H 0.7960 0.9385 1.0408 0.038 Uiso 1 1 calc R . .
C28 C 1.0169(6) 0.94151(17) 1.0008(4) 0.0312(13) Uani 1 1 d . . .
C29 C 1.1662(7) 0.92449(17) 1.0291(4) 0.0341(13) Uani 1 1 d . . .
H29A H 1.2480 0.9338 0.9906 0.041 Uiso 1 1 calc R . .
C30 C 1.1984(6) 0.89446(17) 1.1114(4) 0.0296(12) Uani 1 1 d . . .
C31 C 0.9849(7) 0.97581(18) 0.9167(4) 0.0337(13) Uani 1 1 d . . .
C32 C 0.7943(6) 0.88609(19) 1.2073(5) 0.0408(15) Uani 1 1 d . . .
H32A H 0.7031 0.9044 1.1841 0.061 Uiso 1 1 calc R . .
H32B H 0.8262 0.8917 1.2821 0.061 Uiso 1 1 calc R . .
H32C H 0.7686 0.8543 1.1968 0.061 Uiso 1 1 calc R . .
C33 C 1.3576(6) 0.87595(19) 1.1373(4) 0.0385(14) Uani 1 1 d . . .
H33A H 1.4232 0.8855 1.0839 0.058 Uiso 1 1 calc R . .
H33B H 1.3529 0.8431 1.1387 0.058 Uiso 1 1 calc R . .
H33C H 1.4016 0.8871 1.2063 0.058 Uiso 1 1 calc R . .
C34 C 0.3958(10) 0.5123(3) 0.6750(9) 0.078(3) Uani 1 1 d . . .
C35 C 0.4901(11) 0.4758(2) 0.6499(9) 0.095(3) Uani 1 1 d . . .
H35A H 0.5497 0.4605 0.7057 0.114 Uiso 1 1 calc R . .
C36 C 0.4987(15) 0.4618(3) 0.5513(11) 0.114(4) Uani 1 1 d . . .
H36A H 0.5648 0.4376 0.5378 0.137 Uiso 1 1 calc R . .
C37 C 0.4116(11) 0.4828(3) 0.4707(8) 0.079(3) Uani 1 1 d . . .
H37A H 0.4119 0.4719 0.4010 0.095 Uiso 1 1 calc R . .
C38 C 0.3194(10) 0.5213(3) 0.4901(8) 0.087(3) Uani 1 1 d . . .
H38A H 0.2629 0.5370 0.4337 0.105 Uiso 1 1 calc R . .
C39 C 0.3151(9) 0.5346(3) 0.5917(7) 0.067(2) Uani 1 1 d . . .
C40 C 0.1382(8) 0.5966(3) 0.5383(6) 0.069(2) Uani 1 1 d . . .
H40A H 0.0647 0.5762 0.4970 0.083 Uiso 1 1 calc R . .
H40B H 0.2080 0.6098 0.4904 0.083 Uiso 1 1 calc R . .
C41 C 0.0515(7) 0.6330(2) 0.5859(5) 0.062(2) Uani 1 1 d . . .
H41A H -0.0209 0.6475 0.5309 0.074 Uiso 1 1 calc R . .
H41B H -0.0101 0.6201 0.6392 0.074 Uiso 1 1 calc R . .
C42 C 0.0832(7) 0.7017(2) 0.6827(5) 0.0462(16) Uani 1 1 d . . .
H42A H 0.0142 0.6891 0.7318 0.055 Uiso 1 1 calc R . .
H42B H 0.0183 0.7187 0.6277 0.055 Uiso 1 1 calc R . .
C43 C 0.1963(7) 0.7325(2) 0.7406(5) 0.0421(15) Uani 1 1 d . . .
H43A H 0.2674 0.7446 0.6922 0.050 Uiso 1 1 calc R . .
H43B H 0.1410 0.7579 0.7691 0.050 Uiso 1 1 calc R . .
C44 C 0.3858(6) 0.73303(18) 0.8911(4) 0.0348(14) Uani 1 1 d . . .
C45 C 0.4173(7) 0.77819(19) 0.8821(5) 0.0457(16) Uani 1 1 d . . .
H45A H 0.3642 0.7951 0.8264 0.055 Uiso 1 1 calc R . .
C46 C 0.5250(8) 0.7988(2) 0.9532(6) 0.0526(18) Uani 1 1 d . . .
H46A H 0.5451 0.8299 0.9470 0.063 Uiso 1 1 calc R . .
C47 C 0.6020(9) 0.7750(2) 1.0317(6) 0.0600(19) Uani 1 1 d . . .
H47A H 0.6774 0.7894 1.0800 0.072 Uiso 1 1 calc R . .
C48 C 0.5727(8) 0.7302(2) 1.0426(6) 0.0603(19) Uani 1 1 d . . .
H48A H 0.6281 0.7139 1.0985 0.072 Uiso 1 1 calc R . .
C49 C 0.4633(7) 0.7083(2) 0.9733(5) 0.0407(15) Uani 1 1 d . . .
C50 C 0.5076(9) 0.6377(2) 1.0591(6) 0.069(2) Uani 1 1 d . . .
H50A H 0.4958 0.6509 1.1288 0.082 Uiso 1 1 calc R . .
H50B H 0.6192 0.6375 1.0497 0.082 Uiso 1 1 calc R . .
C51 C 0.4456(9) 0.5906(2) 1.0536(6) 0.069(2) Uani 1 1 d . . .
H51A H 0.4925 0.5731 1.1148 0.083 Uiso 1 1 calc R . .
H51B H 0.3318 0.5910 1.0550 0.083 Uiso 1 1 calc R . .
C52 C 0.4478(10) 0.5243(2) 0.9576(8) 0.084(3) Uani 1 1 d . . .
H52A H 0.3364 0.5196 0.9642 0.101 Uiso 1 1 calc R . .
H52B H 0.5088 0.5090 1.0173 0.101 Uiso 1 1 calc R . .
C53 C 0.4861(12) 0.5053(2) 0.8583(8) 0.093(3) Uani 1 1 d . . .
H53A H 0.4689 0.4725 0.8573 0.112 Uiso 1 1 calc R . .
H53B H 0.5964 0.5111 0.8500 0.112 Uiso 1 1 calc R . .
C54 C -0.1370(11) 0.5251(2) 0.6444(6) 0.073(2) Uani 1 1 d . . .
C55 C -0.0429(10) 0.4880(2) 0.6427(7) 0.072(2) Uani 1 1 d . . .
H55A H 0.0112 0.4764 0.7055 0.086 Uiso 1 1 calc R . .
C56 C -0.0294(10) 0.4679(3) 0.5449(8) 0.077(2) Uani 1 1 d . . .
H56A H 0.0344 0.4422 0.5410 0.092 Uiso 1 1 calc R . .
C57 C -0.1070(9) 0.4850(3) 0.4560(7) 0.068(2) Uani 1 1 d . . .
H57A H -0.0974 0.4709 0.3904 0.081 Uiso 1 1 calc R . .
C58 C -0.2009(9) 0.5229(3) 0.4594(6) 0.065(2) Uani 1 1 d . . .
H58A H -0.2548 0.5346 0.3966 0.078 Uiso 1 1 calc R . .
C59 C -0.2148(9) 0.5432(2) 0.5539(6) 0.0568(19) Uani 1 1 d . . .
C60 C -0.3757(8) 0.6031(2) 0.4768(5) 0.0546(19) Uani 1 1 d . . .
H60A H -0.4429 0.5819 0.4331 0.065 Uiso 1 1 calc R . .
H60B H -0.2960 0.6146 0.4342 0.065 Uiso 1 1 calc R . .
C61 C -0.4690(7) 0.6404(2) 0.5107(6) 0.0583(19) Uani 1 1 d . . .
H61A H -0.5393 0.6516 0.4501 0.070 Uiso 1 1 calc R . .
H61B H -0.5331 0.6298 0.5649 0.070 Uiso 1 1 calc R . .
C62 C -0.4579(8) 0.7095(2) 0.5980(5) 0.0545(18) Uani 1 1 d . . .
H62A H -0.5217 0.6952 0.6481 0.065 Uiso 1 1 calc R . .
H62B H -0.5287 0.7240 0.5420 0.065 Uiso 1 1 calc R . .
C63 C -0.3563(7) 0.7440(2) 0.6537(5) 0.0477(17) Uani 1 1 d . . .
H63A H -0.2792 0.7546 0.6078 0.057 Uiso 1 1 calc R . .
H63B H -0.4192 0.7701 0.6715 0.057 Uiso 1 1 calc R . .
C64 C -0.1842(7) 0.7527(2) 0.8127(5) 0.0435(16) Uani 1 1 d . . .
C65 C -0.1695(8) 0.7983(2) 0.8001(6) 0.0528(18) Uani 1 1 d . . .
H65A H -0.2268 0.8134 0.7431 0.063 Uiso 1 1 calc R . .
C66 C -0.0694(8) 0.8216(2) 0.8723(5) 0.0548(19) Uani 1 1 d . . .
H66A H -0.0601 0.8532 0.8652 0.066 Uiso 1 1 calc R . .
C67 C 0.0156(9) 0.8006(2) 0.9528(5) 0.0602(19) Uani 1 1 d . . .
H67A H 0.0852 0.8174 1.0002 0.072 Uiso 1 1 calc R . .
C68 C 0.0019(9) 0.7545(2) 0.9666(5) 0.063(2) Uani 1 1 d . . .
H68A H 0.0605 0.7398 1.0237 0.075 Uiso 1 1 calc R . .
C69 C -0.0970(8) 0.7308(2) 0.8969(5) 0.0521(18) Uani 1 1 d . . .
C70 C -0.0140(12) 0.6627(3) 0.9831(6) 0.107(3) Uani 1 1 d DU . .
H70A H 0.0918 0.6747 0.9804 0.128 Uiso 1 1 calc R . .
H70B H -0.0449 0.6691 1.0537 0.128 Uiso 1 1 calc R . .
C71 C -0.0134(14) 0.6142(3) 0.9663(8) 0.134(4) Uani 1 1 d DU . .
H71A H 0.0480 0.5999 1.0271 0.161 Uiso 1 1 calc R . .
H71B H -0.1211 0.6030 0.9637 0.161 Uiso 1 1 calc R . .
C72 C 0.0221(12) 0.5523(3) 0.8712(9) 0.129(4) Uani 1 1 d DU . .
H72A H 0.0990 0.5423 0.8246 0.155 Uiso 1 1 calc R . .
H72B H 0.0567 0.5398 0.9415 0.155 Uiso 1 1 calc R . .
C73 C -0.1163(13) 0.5296(3) 0.8360(7) 0.130(4) Uani 1 1 d DU . .
H73A H -0.1956 0.5346 0.8846 0.155 Uiso 1 1 calc R . .
H73B H -0.0977 0.4970 0.8305 0.155 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
K1 K2 2.666(4) 1_655 ?
K1 O11 2.714(4) . ?
K1 O7 2.716(5) . ?
K1 O10 2.737(4) . ?
K1 O9 2.775(4) . ?
K1 O12 2.776(5) . ?
K1 O8 2.821(4) . ?
K1 O17 2.890(4) . ?
K1 C51 3.414(8) . ?
K1 C41 3.468(7) . ?
K1 C42 3.519(6) . ?
K1 C52 3.539(8) . ?
K2 K1 2.666(4) 1_455 ?
K2 O18 3.007(7) . ?
K2 O15 3.046(6) . ?
K2 O13 3.075(7) . ?
K2 O16 3.078(7) . ?
K2 O14 3.183(6) . ?
K2 O11 3.302(6) 1_455 ?
K2 C62 3.363(7) . ?
K2 C61 3.406(8) . ?
O1 C13 1.208(7) . ?
O2 C13 1.276(7) . ?
O3 C22 1.326(7) . ?
O4 C22 1.209(7) . ?
O5 C31 1.248(7) . ?
O6 C31 1.264(6) . ?
O7 C39 1.427(8) . ?
O7 C40 1.433(9) . ?
O8 C42 1.424(7) . ?
O8 C41 1.452(7) . ?
O9 C44 1.371(7) . ?
O9 C43 1.420(6) . ?
O10 C49 1.369(7) . ?
O10 C50 1.418(7) . ?
O11 C51 1.405(8) . ?
O11 C52 1.419(8) . ?
O11 K2 3.302(6) 1_655 ?
O12 C34 1.327(10) . ?
O12 C53 1.479(10) . ?
O13 C59 1.370(8) . ?
O13 C60 1.444(7) . ?
O14 C62 1.420(7) . ?
O14 C61 1.446(7) . ?
O15 C64 1.392(7) . ?
O15 C63 1.409(7) . ?
O16 C69 1.377(8) . ?
O16 C70 1.479(6) . ?
O17 C71 1.288(10) . ?
O17 C72 1.498(10) . ?
O18 C54 1.401(9) . ?
O18 C73 1.420(7) . ?
C1 C6 1.374(7) . ?
C1 C2 1.399(7) . ?
C1 C7 1.510(7) . ?
C2 C3 1.381(7) . ?
C2 H2A 0.9500 . ?
C3 C4 1.391(7) . ?
C3 C25 1.494(7) . ?
C4 C5 1.393(7) . ?
C4 H4A 0.9500 . ?
C5 C6 1.391(7) . ?
C5 C16 1.501(7) . ?
C6 H6A 0.9500 . ?
C7 C12 1.388(7) . ?
C7 C8 1.395(7) . ?
C8 C9 1.401(7) . ?
C8 C14 1.530(8) . ?
C9 C10 1.385(7) . ?
C9 H9A 0.9500 . ?
C10 C11 1.391(7) . ?
C10 C13 1.537(7) . ?
C11 C12 1.381(7) . ?
C11 H11A 0.9500 . ?
C12 C15 1.515(7) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.394(7) . ?
C16 C17 1.405(7) . ?
C17 C18 1.382(7) . ?
C17 C23 1.525(7) . ?
C18 C19 1.381(7) . ?
C18 H18A 0.9500 . ?
C19 C20 1.375(7) . ?
C19 C22 1.498(8) . ?
C20 C21 1.386(7) . ?
C20 H20A 0.9500 . ?
C21 C24 1.540(8) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.387(7) . ?
C25 C30 1.418(7) . ?
C26 C27 1.383(7) . ?
C26 C32 1.536(8) . ?
C27 C28 1.400(7) . ?
C27 H27A 0.9500 . ?
C28 C29 1.401(8) . ?
C28 C31 1.489(7) . ?
C29 C30 1.387(7) . ?
C29 H29A 0.9500 . ?
C30 C33 1.491(7) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C39 1.378(12) . ?
C34 C35 1.421(11) . ?
C35 C36 1.339(14) . ?
C35 H35A 0.9500 . ?
C36 C37 1.361(13) . ?
C36 H36A 0.9500 . ?
C37 C38 1.435(11) . ?
C37 H37A 0.9500 . ?
C38 C39 1.365(10) . ?
C38 H38A 0.9500 . ?
C40 C41 1.488(9) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.481(8) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.381(8) . ?
C44 C49 1.395(8) . ?
C45 C46 1.374(9) . ?
C45 H45A 0.9500 . ?
C46 C47 1.345(9) . ?
C46 H46A 0.9500 . ?
C47 C48 1.368(9) . ?
C47 H47A 0.9500 . ?
C48 C49 1.389(9) . ?
C48 H48A 0.9500 . ?
C50 C51 1.501(9) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.463(12) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.376(11) . ?
C54 C59 1.384(10) . ?
C55 C56 1.405(11) . ?
C55 H55A 0.9500 . ?
C56 C57 1.355(10) . ?
C56 H56A 0.9500 . ?
C57 C58 1.399(10) . ?
C57 H57A 0.9500 . ?
C58 C59 1.369(10) . ?
C58 H58A 0.9500 . ?
C60 C61 1.469(9) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.484(9) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C65 1.376(9) . ?
C64 C69 1.407(9) . ?
C65 C66 1.383(9) . ?
C65 H65A 0.9500 . ?
C66 C67 1.352(9) . ?
C66 H66A 0.9500 . ?
C67 C68 1.391(10) . ?
C67 H67A 0.9500 . ?
C68 C69 1.364(9) . ?
C68 H68A 0.9500 . ?
C70 C71 1.460(7) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 C73 1.408(7) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?

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
K2 K1 O11 75.70(13) 1_655 . ?
K2 K1 O7 101.50(14) 1_655 . ?
O11 K1 O7 117.89(16) . . ?
K2 K1 O10 81.46(14) 1_655 . ?
O11 K1 O10 62.58(13) . . ?
O7 K1 O10 177.04(14) . . ?
K2 K1 O9 94.75(13) 1_655 . ?
O11 K1 O9 118.64(14) . . ?
O7 K1 O9 123.39(15) . . ?
O10 K1 O9 56.06(11) . . ?
K2 K1 O12 84.94(14) 1_655 . ?
O11 K1 O12 61.01(17) . . ?
O7 K1 O12 56.98(18) . . ?
O10 K1 O12 123.59(16) . . ?
O9 K1 O12 179.58(17) . . ?
K2 K1 O8 108.12(12) 1_655 . ?
O11 K1 O8 176.14(14) . . ?
O7 K1 O8 62.39(14) . . ?
O10 K1 O8 116.92(12) . . ?
O9 K1 O8 61.00(12) . . ?
O12 K1 O8 119.37(16) . . ?
K2 K1 O17 164.28(13) 1_655 . ?
O11 K1 O17 89.52(13) . . ?
O7 K1 O17 90.05(13) . . ?
O10 K1 O17 87.03(13) . . ?
O9 K1 O17 87.58(12) . . ?
O12 K1 O17 92.64(13) . . ?
O8 K1 O17 86.62(11) . . ?
K2 K1 C51 87.52(16) 1_655 . ?
O11 K1 C51 23.09(15) . . ?
O7 K1 C51 135.71(18) . . ?
O10 K1 C51 43.84(15) . . ?
O9 K1 C51 98.44(16) . . ?
O12 K1 C51 81.26(18) . . ?
O8 K1 C51 154.37(16) . . ?
O17 K1 C51 76.76(16) . . ?
K2 K1 C41 120.53(15) 1_655 . ?
O11 K1 C41 154.08(16) . . ?
O7 K1 C41 43.12(17) . . ?
O10 K1 C41 135.30(15) . . ?
O9 K1 C41 82.10(15) . . ?
O12 K1 C41 98.30(18) . . ?
O8 K1 C41 23.98(14) . . ?
O17 K1 C41 75.18(14) . . ?
C51 K1 C41 151.89(18) . . ?
K2 K1 C42 116.28(14) 1_655 . ?
O11 K1 C42 154.91(16) . . ?
O7 K1 C42 82.66(16) . . ?
O10 K1 C42 96.15(13) . . ?
O9 K1 C42 42.24(13) . . ?
O12 K1 C42 138.17(17) . . ?
O8 K1 C42 22.73(12) . . ?
O17 K1 C42 75.44(13) . . ?
C51 K1 C42 131.84(17) . . ?
C41 K1 C42 40.04(16) . . ?
K2 K1 C52 86.11(17) 1_655 . ?
O11 K1 C52 21.47(18) . . ?
O7 K1 C52 97.7(2) . . ?
O10 K1 C52 82.32(18) . . ?
O9 K1 C52 137.54(19) . . ?
O12 K1 C52 42.2(2) . . ?
O8 K1 C52 157.03(18) . . ?
O17 K1 C52 81.76(16) . . ?
C51 K1 C52 39.1(2) . . ?
C41 K1 C52 133.0(2) . . ?
C42 K1 C52 157.20(18) . . ?
K1 K2 O18 122.4(2) 1_455 . ?
K1 K2 O15 111.75(17) 1_455 . ?
O18 K2 O15 124.78(19) . . ?
K1 K2 O13 109.06(16) 1_455 . ?
O18 K2 O13 48.86(15) . . ?
O15 K2 O13 105.24(16) . . ?
K1 K2 O16 128.4(2) 1_455 . ?
O18 K2 O16 98.27(18) . . ?
O15 K2 O16 49.86(13) . . ?
O13 K2 O16 122.00(18) . . ?
K1 K2 O14 104.08(14) 1_455 . ?
O18 K2 O14 99.18(18) . . ?
O15 K2 O14 55.38(13) . . ?
O13 K2 O14 55.55(13) . . ?
O16 K2 O14 98.59(16) . . ?
K1 K2 O11 52.80(10) 1_455 1_455 ?
O18 K2 O11 90.43(18) . 1_455 ?
O15 K2 O11 133.90(19) . 1_455 ?
O13 K2 O11 120.79(19) . 1_455 ?
O16 K2 O11 101.77(17) . 1_455 ?
O14 K2 O11 155.97(17) . 1_455 ?
K1 K2 C62 89.66(15) 1_455 . ?
O18 K2 C62 124.0(2) . . ?
O15 K2 C62 42.74(16) . . ?
O13 K2 C62 79.17(17) . . ?
O16 K2 C62 92.42(19) . . ?
O14 K2 C62 24.85(13) . . ?
O11 K2 C62 140.55(19) 1_455 . ?
K1 K2 C61 88.73(16) 1_455 . ?
O18 K2 C61 91.3(2) . . ?
O15 K2 C61 79.30(17) . . ?
O13 K2 C61 42.47(16) . . ?
O16 K2 C61 123.43(19) . . ?
O14 K2 C61 25.06(13) . . ?
O11 K2 C61 133.95(19) 1_455 . ?
C62 K2 C61 40.44(18) . . ?
C39 O7 C40 118.0(6) . . ?
C39 O7 K1 117.9(5) . . ?
C40 O7 K1 117.4(4) . . ?
C42 O8 C41 112.6(5) . . ?
C42 O8 K1 107.3(3) . . ?
C41 O8 K1 103.9(4) . . ?
C44 O9 C43 117.8(4) . . ?
C44 O9 K1 119.2(3) . . ?
C43 O9 K1 117.8(3) . . ?
C49 O10 C50 117.5(5) . . ?
C49 O10 K1 119.2(3) . . ?
C50 O10 K1 114.5(4) . . ?
C51 O11 C52 111.2(6) . . ?
C51 O11 K1 107.7(4) . . ?
C52 O11 K1 114.1(5) . . ?
C51 O11 K2 123.3(4) . 1_655 ?
C52 O11 K2 125.5(5) . 1_655 ?
K1 O11 K2 51.50(10) . 1_655 ?
C34 O12 C53 117.5(7) . . ?
C34 O12 K1 117.3(5) . . ?
C53 O12 K1 115.3(4) . . ?
C59 O13 C60 117.8(5) . . ?
C59 O13 K2 130.0(4) . . ?
C60 O13 K2 112.2(4) . . ?
C62 O14 C61 109.5(5) . . ?
C62 O14 K2 84.7(3) . . ?
C61 O14 K2 86.2(3) . . ?
C64 O15 C63 117.9(5) . . ?
C64 O15 K2 129.6(3) . . ?
C63 O15 K2 112.4(4) . . ?
C69 O16 C70 113.1(6) . . ?
C69 O16 K2 129.2(4) . . ?
C70 O16 K2 117.7(4) . . ?
C71 O17 C72 107.5(7) . . ?
C71 O17 K1 134.0(6) . . ?
C72 O17 K1 103.1(5) . . ?
C54 O18 C73 120.0(7) . . ?
C54 O18 K2 132.7(5) . . ?
C73 O18 K2 106.2(6) . . ?
C6 C1 C2 119.3(5) . . ?
C6 C1 C7 122.1(5) . . ?
C2 C1 C7 118.6(5) . . ?
C3 C2 C1 121.3(5) . . ?
C3 C2 H2A 119.3 . . ?
C1 C2 H2A 119.3 . . ?
C2 C3 C4 117.9(5) . . ?
C2 C3 C25 120.5(5) . . ?
C4 C3 C25 121.6(5) . . ?
C3 C4 C5 122.0(5) . . ?
C3 C4 H4A 119.0 . . ?
C5 C4 H4A 119.0 . . ?
C6 C5 C4 118.3(5) . . ?
C6 C5 C16 122.7(5) . . ?
C4 C5 C16 119.0(5) . . ?
C1 C6 C5 121.1(5) . . ?
C1 C6 H6A 119.5 . . ?
C5 C6 H6A 119.5 . . ?
C12 C7 C8 120.5(5) . . ?
C12 C7 C1 120.4(5) . . ?
C8 C7 C1 119.1(5) . . ?
C7 C8 C9 119.8(5) . . ?
C7 C8 C14 120.8(5) . . ?
C9 C8 C14 119.4(5) . . ?
C10 C9 C8 119.6(5) . . ?
C10 C9 H9A 120.2 . . ?
C8 C9 H9A 120.2 . . ?
C9 C10 C11 119.7(5) . . ?
C9 C10 C13 121.5(5) . . ?
C11 C10 C13 118.8(5) . . ?
C12 C11 C10 121.3(5) . . ?
C12 C11 H11A 119.3 . . ?
C10 C11 H11A 119.3 . . ?
C11 C12 C7 119.0(5) . . ?
C11 C12 C15 119.5(5) . . ?
C7 C12 C15 121.4(4) . . ?
O1 C13 O2 126.6(5) . . ?
O1 C13 C10 119.3(5) . . ?
O2 C13 C10 114.1(5) . . ?
C8 C14 H14A 109.5 . . ?
C8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 119.4(5) . . ?
C21 C16 C5 121.4(5) . . ?
C17 C16 C5 119.1(5) . . ?
C18 C17 C16 119.1(5) . . ?
C18 C17 C23 120.6(5) . . ?
C16 C17 C23 120.2(5) . . ?
C19 C18 C17 121.0(5) . . ?
C19 C18 H18A 119.5 . . ?
C17 C18 H18A 119.5 . . ?
C20 C19 C18 120.1(5) . . ?
C20 C19 C22 119.6(5) . . ?
C18 C19 C22 120.2(5) . . ?
C19 C20 C21 120.1(5) . . ?
C19 C20 H20A 120.0 . . ?
C21 C20 H20A 120.0 . . ?
C20 C21 C16 120.3(5) . . ?
C20 C21 C24 120.1(5) . . ?
C16 C21 C24 119.6(5) . . ?
O4 C22 O3 122.8(5) . . ?
O4 C22 C19 124.4(5) . . ?
O3 C22 C19 112.8(5) . . ?
C17 C23 H23A 109.5 . . ?
C17 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C17 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C30 120.5(5) . . ?
C26 C25 C3 120.5(5) . . ?
C30 C25 C3 119.0(5) . . ?
C27 C26 C25 119.9(5) . . ?
C27 C26 C32 119.0(5) . . ?
C25 C26 C32 121.1(5) . . ?
C26 C27 C28 121.3(5) . . ?
C26 C27 H27A 119.4 . . ?
C28 C27 H27A 119.4 . . ?
C27 C28 C29 118.0(5) . . ?
C27 C28 C31 120.0(5) . . ?
C29 C28 C31 121.8(5) . . ?
C30 C29 C28 122.1(5) . . ?
C30 C29 H29A 119.0 . . ?
C28 C29 H29A 119.0 . . ?
C29 C30 C25 118.2(5) . . ?
C29 C30 C33 120.7(5) . . ?
C25 C30 C33 121.1(5) . . ?
O5 C31 O6 122.9(5) . . ?
O5 C31 C28 119.1(5) . . ?
O6 C31 C28 117.9(6) . . ?
C26 C32 H32A 109.5 . . ?
C26 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C26 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O12 C34 C39 118.9(7) . . ?
O12 C34 C35 124.3(10) . . ?
C39 C34 C35 116.7(9) . . ?
C36 C35 C34 123.0(12) . . ?
C36 C35 H35A 118.5 . . ?
C34 C35 H35A 118.5 . . ?
C35 C36 C37 119.1(11) . . ?
C35 C36 H36A 120.4 . . ?
C37 C36 H36A 120.4 . . ?
C36 C37 C38 120.6(9) . . ?
C36 C37 H37A 119.7 . . ?
C38 C37 H37A 119.7 . . ?
C39 C38 C37 118.2(10) . . ?
C39 C38 H38A 120.9 . . ?
C37 C38 H38A 120.9 . . ?
C38 C39 C34 122.1(9) . . ?
C38 C39 O7 123.2(9) . . ?
C34 C39 O7 114.7(7) . . ?
O7 C40 C41 109.0(5) . . ?
O7 C40 H40A 109.9 . . ?
C41 C40 H40A 109.9 . . ?
O7 C40 H40B 109.9 . . ?
C41 C40 H40B 109.9 . . ?
H40A C40 H40B 108.3 . . ?
O8 C41 C40 109.8(5) . . ?
O8 C41 K1 52.1(3) . . ?
C40 C41 K1 83.2(4) . . ?
O8 C41 H41A 109.7 . . ?
C40 C41 H41A 109.7 . . ?
K1 C41 H41A 161.4 . . ?
O8 C41 H41B 109.7 . . ?
C40 C41 H41B 109.7 . . ?
K1 C41 H41B 78.4 . . ?
H41A C41 H41B 108.2 . . ?
O8 C42 C43 111.3(5) . . ?
O8 C42 K1 49.9(2) . . ?
C43 C42 K1 83.5(3) . . ?
O8 C42 H42A 109.4 . . ?
C43 C42 H42A 109.4 . . ?
K1 C42 H42A 81.6 . . ?
O8 C42 H42B 109.4 . . ?
C43 C42 H42B 109.4 . . ?
K1 C42 H42B 159.2 . . ?
H42A C42 H42B 108.0 . . ?
O9 C43 C42 109.6(5) . . ?
O9 C43 H43A 109.7 . . ?
C42 C43 H43A 109.7 . . ?
O9 C43 H43B 109.7 . . ?
C42 C43 H43B 109.7 . . ?
H43A C43 H43B 108.2 . . ?
O9 C44 C45 125.4(5) . . ?
O9 C44 C49 114.9(5) . . ?
C45 C44 C49 119.7(6) . . ?
C46 C45 C44 120.4(6) . . ?
C46 C45 H45A 119.8 . . ?
C44 C45 H45A 119.8 . . ?
C47 C46 C45 120.3(6) . . ?
C47 C46 H46A 119.8 . . ?
C45 C46 H46A 119.8 . . ?
C46 C47 C48 120.5(7) . . ?
C46 C47 H47A 119.8 . . ?
C48 C47 H47A 119.8 . . ?
C47 C48 C49 121.0(7) . . ?
C47 C48 H48A 119.5 . . ?
C49 C48 H48A 119.5 . . ?
O10 C49 C48 125.1(6) . . ?
O10 C49 C44 116.8(5) . . ?
C48 C49 C44 118.1(6) . . ?
O10 C50 C51 109.2(6) . . ?
O10 C50 H50A 109.8 . . ?
C51 C50 H50A 109.8 . . ?
O10 C50 H50B 109.8 . . ?
C51 C50 H50B 109.8 . . ?
H50A C50 H50B 108.3 . . ?
O11 C51 C50 108.6(7) . . ?
O11 C51 K1 49.2(3) . . ?
C50 C51 K1 83.4(4) . . ?
O11 C51 H51A 110.0 . . ?
C50 C51 H51A 110.0 . . ?
K1 C51 H51A 159.0 . . ?
O11 C51 H51B 110.0 . . ?
C50 C51 H51B 110.0 . . ?
K1 C51 H51B 80.6 . . ?
H51A C51 H51B 108.4 . . ?
O11 C52 C53 109.1(7) . . ?
O11 C52 K1 44.4(4) . . ?
C53 C52 K1 83.0(5) . . ?
O11 C52 H52A 109.9 . . ?
C53 C52 H52A 109.9 . . ?
K1 C52 H52A 86.8 . . ?
O11 C52 H52B 109.9 . . ?
C53 C52 H52B 109.9 . . ?
K1 C52 H52B 154.2 . . ?
H52A C52 H52B 108.3 . . ?
C52 C53 O12 108.0(7) . . ?
C52 C53 H53A 110.1 . . ?
O12 C53 H53A 110.1 . . ?
C52 C53 H53B 110.1 . . ?
O12 C53 H53B 110.1 . . ?
H53A C53 H53B 108.4 . . ?
C55 C54 C59 122.3(8) . . ?
C55 C54 O18 124.5(7) . . ?
C59 C54 O18 113.1(7) . . ?
C54 C55 C56 117.7(8) . . ?
C54 C55 H55A 121.1 . . ?
C56 C55 H55A 121.1 . . ?
C57 C56 C55 120.3(8) . . ?
C57 C56 H56A 119.8 . . ?
C55 C56 H56A 119.8 . . ?
C56 C57 C58 121.0(8) . . ?
C56 C57 H57A 119.5 . . ?
C58 C57 H57A 119.5 . . ?
C59 C58 C57 119.5(8) . . ?
C59 C58 H58A 120.2 . . ?
C57 C58 H58A 120.2 . . ?
C58 C59 O13 125.8(7) . . ?
C58 C59 C54 119.0(8) . . ?
O13 C59 C54 115.1(7) . . ?
O13 C60 C61 108.7(5) . . ?
O13 C60 H60A 109.9 . . ?
C61 C60 H60A 109.9 . . ?
O13 C60 H60B 109.9 . . ?
C61 C60 H60B 109.9 . . ?
H60A C60 H60B 108.3 . . ?
O14 C61 C60 109.9(5) . . ?
O14 C61 K2 68.8(3) . . ?
C60 C61 K2 96.5(4) . . ?
O14 C61 H61A 109.7 . . ?
C60 C61 H61A 109.7 . . ?
K2 C61 H61A 151.9 . . ?
O14 C61 H61B 109.7 . . ?
C60 C61 H61B 109.7 . . ?
K2 C61 H61B 51.1 . . ?
H61A C61 H61B 108.2 . . ?
O14 C62 C63 110.8(5) . . ?
O14 C62 K2 70.4(3) . . ?
C63 C62 K2 95.9(4) . . ?
O14 C62 H62A 109.5 . . ?
C63 C62 H62A 109.5 . . ?
K2 C62 H62A 50.0 . . ?
O14 C62 H62B 109.5 . . ?
C63 C62 H62B 109.5 . . ?
K2 C62 H62B 151.9 . . ?
H62A C62 H62B 108.1 . . ?
O15 C63 C62 108.9(5) . . ?
O15 C63 H63A 109.9 . . ?
C62 C63 H63A 109.9 . . ?
O15 C63 H63B 109.9 . . ?
C62 C63 H63B 109.9 . . ?
H63A C63 H63B 108.3 . . ?
C65 C64 O15 124.8(6) . . ?
C65 C64 C69 119.9(7) . . ?
O15 C64 C69 115.3(6) . . ?
C64 C65 C66 118.5(7) . . ?
C64 C65 H65A 120.7 . . ?
C66 C65 H65A 120.7 . . ?
C67 C66 C65 121.7(7) . . ?
C67 C66 H66A 119.2 . . ?
C65 C66 H66A 119.2 . . ?
C66 C67 C68 120.4(7) . . ?
C66 C67 H67A 119.8 . . ?
C68 C67 H67A 119.8 . . ?
C69 C68 C67 119.0(7) . . ?
C69 C68 H68A 120.5 . . ?
C67 C68 H68A 120.5 . . ?
C68 C69 O16 124.7(6) . . ?
C68 C69 C64 120.4(6) . . ?
O16 C69 C64 114.9(6) . . ?
C71 C70 O16 111.1(7) . . ?
C71 C70 H70A 109.4 . . ?
O16 C70 H70A 109.4 . . ?
C71 C70 H70B 109.4 . . ?
O16 C70 H70B 109.4 . . ?
H70A C70 H70B 108.0 . . ?
O17 C71 C70 114.2(9) . . ?
O17 C71 H71A 108.7 . . ?
C70 C71 H71A 108.7 . . ?
O17 C71 H71B 108.7 . . ?
C70 C71 H71B 108.7 . . ?
H71A C71 H71B 107.6 . . ?
C73 C72 O17 126.3(8) . . ?
C73 C72 H72A 105.7 . . ?
O17 C72 H72A 105.7 . . ?
C73 C72 H72B 105.7 . . ?
O17 C72 H72B 105.7 . . ?
H72A C72 H72B 106.2 . . ?
C72 C73 O18 104.8(8) . . ?
C72 C73 H73A 110.8 . . ?
O18 C73 H73A 110.8 . . ?
C72 C73 H73B 110.8 . . ?
O18 C73 H73B 110.8 . . ?
H73A C73 H73B 108.9 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.060
_database_code_depnum_ccdc_archive 'CCDC 974557'
