data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr I. Butler
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C46 H49 Cl3 O6'
_chemical_formula_weight          804.20
 
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            triclinic
_symmetry_space_group_name_H-M    P-1
_symmetry_space_group_name_hall   '-P 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    6.179(3)
_cell_length_b                    17.150(7)
_cell_length_c                    20.284(7)
_cell_angle_alpha                 75.3973(18)
_cell_angle_beta                  89.419(2)
_cell_angle_gamma                 84.076(2)
_cell_volume                      2068.1(16)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     9150
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             'Light grey-green'
_exptl_crystal_size_max           0.18
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.291
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              848
_exptl_absorpt_coefficient_mu     0.270
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9531
_exptl_absorpt_correction_T_max   0.9920
_exptl_absorpt_process_details    'SORTAV Blessing (1997)'
 
_exptl_special_details
;
 PLEASE NOTE cell_measurement_ fields are not relevant to area detector data,
 the entire data set is used to refine the cell, which is indexed from all
 observed reflections in a 10 degree phi range.
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             40048
_diffrn_reflns_av_R_equivalents   0.1387
_diffrn_reflns_av_sigmaI/netI     0.1038
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -22
_diffrn_reflns_limit_k_max        22
_diffrn_reflns_limit_l_min        -26
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_theta_min          3.31
_diffrn_reflns_theta_max          27.48
_reflns_number_total              9380
_reflns_number_gt                 5546
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection
' DENZO (Otwinowski and Minor, 1997)'
_computing_cell_refinement        
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction         
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_computing_publication_material   ? 
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0675P)²+1.1000P] 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      SHELXL
_refine_ls_extinction_coef        0.0059(12)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          9380
_refine_ls_number_parameters      509
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1275
_refine_ls_R_factor_gt            0.0671
_refine_ls_wR_factor_ref          0.1751
_refine_ls_wR_factor_gt           0.1477
_refine_ls_goodness_of_fit_ref    1.019
_refine_ls_restrained_S_all       1.019
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C -0.2739(5) 0.53761(18) 0.33491(14) 0.0274(6) Uani 1 1 d . . .
C2 C -0.1720(5) 0.60941(18) 0.35009(15) 0.0303(7) Uani 1 1 d . . .
H2A H -0.2334 0.6204 0.3919 0.045 Uiso 1 1 calc R . .
H2B H -0.2034 0.6575 0.3120 0.045 Uiso 1 1 calc R . .
H2C H -0.0141 0.5961 0.3560 0.045 Uiso 1 1 calc R . .
C3 C -0.5199(5) 0.5625(2) 0.32324(16) 0.0345(7) Uani 1 1 d . . .
H3A H -0.5915 0.5163 0.3174 0.052 Uiso 1 1 calc R . .
H3B H -0.5443 0.6074 0.2822 0.052 Uiso 1 1 calc R . .
H3C H -0.5804 0.5798 0.3627 0.052 Uiso 1 1 calc R . .
C4 C -0.1835(4) 0.51641(18) 0.27037(14) 0.0269(6) Uani 1 1 d . . .
C5 C -0.0394(5) 0.56119(19) 0.22774(14) 0.0296(7) Uani 1 1 d . . .
H5 H 0.0080 0.6076 0.2384 0.036 Uiso 1 1 calc R . .
C6 C 0.0364(5) 0.53940(19) 0.16992(15) 0.0317(7) Uani 1 1 d . . .
H6 H 0.1360 0.5705 0.1415 0.038 Uiso 1 1 calc R . .
C7 C -0.0316(5) 0.47325(19) 0.15363(14) 0.0300(7) Uani 1 1 d . . .
C8 C -0.1770(5) 0.4279(2) 0.19456(16) 0.0338(7) Uani 1 1 d . . .
H8 H -0.2260 0.3822 0.1830 0.041 Uiso 1 1 calc R . .
C9 C -0.2498(5) 0.44970(19) 0.25233(15) 0.0303(7) Uani 1 1 d . . .
H9 H -0.3487 0.4181 0.2807 0.036 Uiso 1 1 calc R . .
C10 C -0.2244(4) 0.46465(17) 0.39608(14) 0.0247(6) Uani 1 1 d . . .
C11 C -0.3754(5) 0.43756(18) 0.44470(14) 0.0267(6) Uani 1 1 d . . .
H11 H -0.5197 0.4637 0.4395 0.032 Uiso 1 1 calc R . .
C12 C -0.3225(5) 0.37362(18) 0.50056(14) 0.0269(6) Uani 1 1 d . . .
H12 H -0.4294 0.3560 0.5334 0.032 Uiso 1 1 calc R . .
C13 C -0.1132(5) 0.33528(17) 0.50866(14) 0.0249(6) Uani 1 1 d . . .
C14 C 0.0412(4) 0.36060(19) 0.46091(15) 0.0287(7) Uani 1 1 d . . .
H14 H 0.1849 0.3340 0.4661 0.034 Uiso 1 1 calc R . .
C15 C -0.0142(4) 0.42461(18) 0.40573(15) 0.0290(7) Uani 1 1 d . . .
H15 H 0.0934 0.4422 0.3732 0.035 Uiso 1 1 calc R . .
O1 O 0.0441(4) 0.44753(13) 0.09717(10) 0.0360(5) Uani 1 1 d . . .
H1 H 0.1200 0.4819 0.0737 0.054 Uiso 1 1 calc R . .
O2 O -0.0519(3) 0.27000(12) 0.56265(10) 0.0306(5) Uani 1 1 d . . .
H2 H -0.1582 0.2599 0.5884 0.046 Uiso 1 1 calc R . .
C21 C 0.4903(5) 0.83124(19) 0.06855(14) 0.0293(7) Uani 1 1 d . . .
C22 C 0.3450(5) 0.90826(19) 0.03511(15) 0.0347(7) Uani 1 1 d . . .
H22A H 0.3596 0.9201 -0.0145 0.052 Uiso 1 1 calc R . .
H22B H 0.3887 0.9536 0.0514 0.052 Uiso 1 1 calc R . .
H22C H 0.1932 0.9006 0.0469 0.052 Uiso 1 1 calc R . .
C23 C 0.7228(5) 0.8446(2) 0.04521(16) 0.0368(8) Uani 1 1 d . . .
H23A H 0.7307 0.8505 -0.0041 0.055 Uiso 1 1 calc R . .
H23B H 0.8227 0.7980 0.0690 0.055 Uiso 1 1 calc R . .
H23C H 0.7640 0.8938 0.0558 0.055 Uiso 1 1 calc R . .
C24 C 0.4263(4) 0.75708(19) 0.04792(14) 0.0273(6) Uani 1 1 d . . .
C25 C 0.2546(5) 0.76011(19) 0.00358(14) 0.0301(7) Uani 1 1 d . . .
H25 H 0.1736 0.8108 -0.0160 0.036 Uiso 1 1 calc R . .
C26 C 0.1979(5) 0.6914(2) -0.01291(15) 0.0329(7) Uani 1 1 d . . .
H26 H 0.0787 0.6951 -0.0432 0.039 Uiso 1 1 calc R . .
C27 C 0.3139(5) 0.61803(19) 0.01457(15) 0.0329(7) Uani 1 1 d . . .
C28 C 0.4870(5) 0.6128(2) 0.05858(16) 0.0377(8) Uani 1 1 d . . .
H28 H 0.5691 0.5621 0.0772 0.045 Uiso 1 1 calc R . .
C29 C 0.5399(5) 0.6819(2) 0.07530(15) 0.0350(7) Uani 1 1 d . . .
H29 H 0.6572 0.6777 0.1064 0.042 Uiso 1 1 calc R . .
C30 C 0.4682(4) 0.81694(18) 0.14596(14) 0.0254(6) Uani 1 1 d . . .
C31 C 0.2838(4) 0.78529(18) 0.17790(15) 0.0276(7) Uani 1 1 d . . .
H31 H 0.1763 0.7708 0.1512 0.033 Uiso 1 1 calc R . .
C32 C 0.2530(5) 0.77440(18) 0.24663(15) 0.0283(7) Uani 1 1 d . . .
H32 H 0.1253 0.7532 0.2670 0.034 Uiso 1 1 calc R . .
C33 C 0.4098(4) 0.79460(17) 0.28576(14) 0.0247(6) Uani 1 1 d . . .
C34 C 0.5925(5) 0.82738(18) 0.25584(15) 0.0281(7) Uani 1 1 d . . .
H34 H 0.6982 0.8426 0.2827 0.034 Uiso 1 1 calc R . .
C35 C 0.6209(5) 0.83800(18) 0.18643(15) 0.0288(7) Uani 1 1 d . . .
H35 H 0.7475 0.8602 0.1661 0.035 Uiso 1 1 calc R . .
O21 O 0.2603(4) 0.54704(14) 0.00201(11) 0.0416(6) Uani 1 1 d . . .
H21 H 0.1703 0.5579 -0.0307 0.062 Uiso 1 1 calc R . .
O22 O 0.3758(3) 0.78120(13) 0.35473(9) 0.0299(5) Uani 1 1 d . . .
H22 H 0.4809 0.7954 0.3733 0.045 Uiso 1 1 calc R . .
C41 C -0.2779(5) 1.16709(19) 0.37641(15) 0.0292(7) Uani 1 1 d . . .
C42 C -0.0461(5) 1.1923(2) 0.37666(18) 0.0392(8) Uani 1 1 d . . .
H42A H 0.0384 1.1744 0.3411 0.059 Uiso 1 1 calc R . .
H42B H 0.0239 1.1671 0.4212 0.059 Uiso 1 1 calc R . .
H42C H -0.0529 1.2514 0.3678 0.059 Uiso 1 1 calc R . .
C43 C -0.4030(5) 1.1933(2) 0.43381(16) 0.0355(7) Uani 1 1 d . . .
H43A H -0.4005 1.2517 0.4277 0.053 Uiso 1 1 calc R . .
H43B H -0.3347 1.1642 0.4778 0.053 Uiso 1 1 calc R . .
H43C H -0.5540 1.1808 0.4327 0.053 Uiso 1 1 calc R . .
C44 C -0.3804(5) 1.20734(18) 0.30665(15) 0.0284(7) Uani 1 1 d . . .
C45 C -0.5590(5) 1.26504(19) 0.29632(16) 0.0333(7) Uani 1 1 d . . .
H45 H -0.6197 1.2816 0.3344 0.040 Uiso 1 1 calc R . .
C46 C -0.6518(5) 1.2993(2) 0.23278(16) 0.0360(7) Uani 1 1 d . . .
H46 H -0.7735 1.3391 0.2273 0.043 Uiso 1 1 calc R . .
C47 C -0.5664(5) 1.2752(2) 0.17698(16) 0.0372(8) Uani 1 1 d . . .
C48 C -0.3853(5) 1.21901(19) 0.18545(16) 0.0375(8) Uani 1 1 d . . .
H48 H -0.3233 1.2033 0.1472 0.045 Uiso 1 1 calc R . .
C49 C -0.2954(5) 1.18599(19) 0.24908(15) 0.0335(7) Uani 1 1 d . . .
H49 H -0.1712 1.1473 0.2542 0.040 Uiso 1 1 calc R . .
C50 C -0.2780(4) 1.07551(18) 0.38914(14) 0.0270(6) Uani 1 1 d . . .
C51 C -0.4689(5) 1.04417(19) 0.37589(16) 0.0323(7) Uani 1 1 d . . .
H51 H -0.5935 1.0805 0.3583 0.039 Uiso 1 1 calc R . .
C52 C -0.4807(5) 0.96205(19) 0.38774(16) 0.0321(7) Uani 1 1 d . . .
H52 H -0.6121 0.9421 0.3785 0.039 Uiso 1 1 calc R . .
C53 C -0.3006(4) 0.90919(18) 0.41304(14) 0.0258(6) Uani 1 1 d . . .
C54 C -0.1113(5) 0.93799(19) 0.42777(14) 0.0297(7) Uani 1 1 d . . .
H54 H 0.0121 0.9013 0.4461 0.036 Uiso 1 1 calc R . .
C55 C -0.1022(5) 1.02040(18) 0.41574(14) 0.0285(7) Uani 1 1 d . . .
H55 H 0.0288 1.0398 0.4260 0.034 Uiso 1 1 calc R . .
O41 O -0.6547(4) 1.30480(16) 0.11285(11) 0.0492(6) Uani 1 1 d . . .
H41 H -0.7437 1.3455 0.1120 0.074 Uiso 1 1 calc R . .
O42 O -0.3179(3) 0.82719(12) 0.42267(10) 0.0300(5) Uani 1 1 d . . .
H42 H -0.1949 0.8012 0.4328 0.045 Uiso 1 1 calc R . .
C61 C 0.1532(5) 0.9952(2) 0.18866(16) 0.0347(7) Uani 1 1 d . . .
H61 H 0.2379 0.9446 0.1828 0.042 Uiso 1 1 calc R . .
Cl61 Cl 0.02590(14) 0.97305(5) 0.26801(4) 0.0434(2) Uani 1 1 d . . .
Cl62 Cl 0.33150(17) 1.06819(7) 0.18502(6) 0.0658(3) Uani 1 1 d . . .
Cl63 Cl -0.04398(15) 1.02799(6) 0.12313(4) 0.0493(3) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 C10 1.529(4) . ?
C1 C4 1.532(4) . ?
C1 C2 1.537(4) . ?
C1 C3 1.540(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.386(4) . ?
C4 C9 1.386(4) . ?
C5 C6 1.383(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.365(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.380(4) . ?
C7 O1 1.390(4) . ?
C8 C9 1.377(4) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.379(4) . ?
C10 C15 1.396(4) . ?
C11 C12 1.377(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.376(4) . ?
C13 O2 1.376(4) . ?
C14 C15 1.372(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O1 H1 0.8400 . ?
O2 H2 0.8400 . ?
C21 C22 1.525(4) . ?
C21 C24 1.525(4) . ?
C21 C23 1.530(4) . ?
C21 C30 1.534(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.385(4) . ?
C24 C29 1.387(4) . ?
C25 C26 1.382(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.369(5) . ?
C26 H26 0.9500 . ?
C27 O21 1.378(4) . ?
C27 C28 1.380(5) . ?
C28 C29 1.382(5) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C35 1.388(4) . ?
C30 C31 1.396(4) . ?
C31 C32 1.373(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.382(4) . ?
C32 H32 0.9500 . ?
C33 O22 1.377(3) . ?
C33 C34 1.381(4) . ?
C34 C35 1.385(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
O21 H21 0.8400 . ?
O22 H22 0.8400 . ?
C41 C44 1.520(4) . ?
C41 C50 1.526(4) . ?
C41 C43 1.528(4) . ?
C41 C42 1.539(4) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.385(4) . ?
C44 C49 1.393(4) . ?
C45 C46 1.376(4) . ?
C45 H45 0.9500 . ?
C46 C47 1.383(5) . ?
C46 H46 0.9500 . ?
C47 O41 1.366(4) . ?
C47 C48 1.383(5) . ?
C48 C49 1.368(4) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 C55 1.381(4) . ?
C50 C51 1.400(4) . ?
C51 C52 1.377(4) . ?
C51 H51 0.9500 . ?
C52 C53 1.375(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.379(4) . ?
C53 O42 1.385(4) . ?
C54 C55 1.379(4) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
O41 H41 0.8400 . ?
O42 H42 0.8400 . ?
C61 Cl62 1.739(3) . ?
C61 Cl63 1.753(3) . ?
C61 Cl61 1.756(3) . ?
C61 H61 1.0000 . ?
 
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
C10 C1 C4 109.4(2) . . ?
C10 C1 C2 107.6(2) . . ?
C4 C1 C2 112.3(2) . . ?
C10 C1 C3 112.3(2) . . ?
C4 C1 C3 107.8(2) . . ?
C2 C1 C3 107.5(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 C9 117.4(3) . . ?
C5 C4 C1 123.5(3) . . ?
C9 C4 C1 119.1(3) . . ?
C6 C5 C4 121.1(3) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C7 C6 C5 120.1(3) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C8 120.3(3) . . ?
C6 C7 O1 122.4(3) . . ?
C8 C7 O1 117.3(3) . . ?
C9 C8 C7 119.1(3) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C4 122.0(3) . . ?
C8 C9 H9 119.0 . . ?
C4 C9 H9 119.0 . . ?
C11 C10 C15 117.3(3) . . ?
C11 C10 C1 123.3(3) . . ?
C15 C10 C1 119.4(3) . . ?
C12 C11 C10 121.7(3) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C11 C12 C13 119.7(3) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C14 C13 O2 117.6(3) . . ?
C14 C13 C12 120.1(3) . . ?
O2 C13 C12 122.3(3) . . ?
C15 C14 C13 119.4(3) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C10 121.8(3) . . ?
C14 C15 H15 119.1 . . ?
C10 C15 H15 119.1 . . ?
C7 O1 H1 109.5 . . ?
C13 O2 H2 109.5 . . ?
C22 C21 C24 112.6(2) . . ?
C22 C21 C23 107.4(3) . . ?
C24 C21 C23 108.3(3) . . ?
C22 C21 C30 107.5(3) . . ?
C24 C21 C30 108.7(2) . . ?
C23 C21 C30 112.4(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C29 117.1(3) . . ?
C25 C24 C21 123.2(3) . . ?
C29 C24 C21 119.6(3) . . ?
C26 C25 C24 121.8(3) . . ?
C26 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
C27 C26 C25 119.8(3) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C26 C27 O21 122.4(3) . . ?
C26 C27 C28 120.0(3) . . ?
O21 C27 C28 117.5(3) . . ?
C27 C28 C29 119.5(3) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C28 C29 C24 121.8(3) . . ?
C28 C29 H29 119.1 . . ?
C24 C29 H29 119.1 . . ?
C35 C30 C31 117.3(3) . . ?
C35 C30 C21 122.6(2) . . ?
C31 C30 C21 120.0(2) . . ?
C32 C31 C30 122.1(3) . . ?
C32 C31 H31 119.0 . . ?
C30 C31 H31 119.0 . . ?
C31 C32 C33 119.2(3) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
O22 C33 C34 121.9(2) . . ?
O22 C33 C32 117.7(2) . . ?
C34 C33 C32 120.4(3) . . ?
C33 C34 C35 119.6(3) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C34 C35 C30 121.4(3) . . ?
C34 C35 H35 119.3 . . ?
C30 C35 H35 119.3 . . ?
C27 O21 H21 109.5 . . ?
C33 O22 H22 109.5 . . ?
C44 C41 C50 108.6(2) . . ?
C44 C41 C43 112.4(3) . . ?
C50 C41 C43 107.9(2) . . ?
C44 C41 C42 107.8(3) . . ?
C50 C41 C42 112.0(3) . . ?
C43 C41 C42 108.2(3) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C44 C49 116.7(3) . . ?
C45 C44 C41 123.4(3) . . ?
C49 C44 C41 119.9(3) . . ?
C46 C45 C44 122.3(3) . . ?
C46 C45 H45 118.9 . . ?
C44 C45 H45 118.9 . . ?
C45 C46 C47 119.5(3) . . ?
C45 C46 H46 120.3 . . ?
C47 C46 H46 120.3 . . ?
O41 C47 C48 117.9(3) . . ?
O41 C47 C46 122.5(3) . . ?
C48 C47 C46 119.6(3) . . ?
C49 C48 C47 119.9(3) . . ?
C49 C48 H48 120.1 . . ?
C47 C48 H48 120.1 . . ?
C48 C49 C44 122.1(3) . . ?
C48 C49 H49 119.0 . . ?
C44 C49 H49 119.0 . . ?
C55 C50 C51 117.1(3) . . ?
C55 C50 C41 123.9(3) . . ?
C51 C50 C41 119.0(3) . . ?
C52 C51 C50 121.7(3) . . ?
C52 C51 H51 119.1 . . ?
C50 C51 H51 119.1 . . ?
C53 C52 C51 119.4(3) . . ?
C53 C52 H52 120.3 . . ?
C51 C52 H52 120.3 . . ?
C52 C53 C54 120.4(3) . . ?
C52 C53 O42 117.5(2) . . ?
C54 C53 O42 122.1(3) . . ?
C53 C54 C55 119.5(3) . . ?
C53 C54 H54 120.2 . . ?
C55 C54 H54 120.2 . . ?
C54 C55 C50 121.9(3) . . ?
C54 C55 H55 119.1 . . ?
C50 C55 H55 119.1 . . ?
C47 O41 H41 109.5 . . ?
C53 O42 H42 109.5 . . ?
Cl62 C61 Cl63 110.65(19) . . ?
Cl62 C61 Cl61 110.53(18) . . ?
Cl63 C61 Cl61 109.80(18) . . ?
Cl62 C61 H61 108.6 . . ?
Cl63 C61 H61 108.6 . . ?
Cl61 C61 H61 108.6 . . ?
 
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_angle_DHA
 _geom_hbond_site_symmetry_A
O1 H1 O21  0.84 1.86 2.679(4) 164.0 .
O2 H2 O22  0.84 1.84 2.673(3) 169.8 2_566
O21 H21 O1  0.84 1.92 2.743(3) 164.8 2_565
O22 H22 O42  0.84 1.81 2.646(3) 172.1 1_655
O41 H41 O1  0.84 2.03 2.870(4) 172.9 1_465
O42 H42 O2  0.84 1.84 2.659(3) 164.2 2_566
 
_diffrn_measured_fraction_theta_max    0.992
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.992
_refine_diff_density_max    0.357
_refine_diff_density_min   -0.392
_refine_diff_density_rms    0.073
