data_04src0682

_exptl_special_details
;
 Two of the alkyl chains are partially disordered over two sites.
; 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. Paddy Murphy
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C52 H68 Br4 O4'
_chemical_formula_sum
 'C52 H68 Br4 O4'
_chemical_formula_weight          1076.70
 
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'
 'Br'  'Br'  -0.2901   2.4595
 '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   -P1
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    9.9105(9)
_cell_length_b                    13.1978(18)
_cell_length_c                    19.491(2)
_cell_angle_alpha                 72.837(9)
_cell_angle_beta                  87.908(8)
_cell_angle_gamma                 84.906(10)
_cell_volume                      2426.1(5)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     10667
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           0.38
_exptl_crystal_size_mid           0.29
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.474
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1104
_exptl_absorpt_coefficient_mu     3.361
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.3616
_exptl_absorpt_correction_T_max   0.8773
_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    'graphite'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             46540
_diffrn_reflns_av_R_equivalents   0.0759
_diffrn_reflns_av_sigmaI/netI     0.0924
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -25
_diffrn_reflns_limit_l_max        25
_diffrn_reflns_theta_min          2.94
_diffrn_reflns_theta_max          27.48
_reflns_number_total              11093
_reflns_number_gt                 6060
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_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)+(0.0588P)²+2.8909P] 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        0.0018(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          11093
_refine_ls_number_parameters      622
_refine_ls_number_restraints      178
_refine_ls_R_factor_all           0.1339
_refine_ls_R_factor_gt            0.0582
_refine_ls_wR_factor_ref          0.1477
_refine_ls_wR_factor_gt           0.1220
_refine_ls_goodness_of_fit_ref    1.017
_refine_ls_restrained_S_all       1.012
_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 0.3525(4) 0.1592(3) 0.6740(2) 0.0239(9) Uani 1 1 d U . .
C2 C 0.4337(4) 0.1340(3) 0.7340(2) 0.0231(9) Uani 1 1 d U . .
C3 C 0.4393(4) 0.2100(3) 0.7702(2) 0.0269(9) Uani 1 1 d U . .
H3 H 0.4958 0.1941 0.8109 0.032 Uiso 1 1 calc R . .
C4 C 0.3654(4) 0.3081(3) 0.7488(2) 0.0243(9) Uani 1 1 d U . .
C5 C 0.2857(4) 0.3298(3) 0.6883(2) 0.0248(9) Uani 1 1 d U . .
H5 H 0.2344 0.3967 0.6729 0.030 Uiso 1 1 calc R . .
C6 C 0.2780(4) 0.2577(3) 0.6494(2) 0.0222(9) Uani 1 1 d U . .
C7 C 0.1972(4) 0.2889(3) 0.5809(2) 0.0233(9) Uani 1 1 d U . .
H7A H 0.1625 0.2247 0.5739 0.028 Uiso 1 1 calc R . .
H7B H 0.1184 0.3384 0.5853 0.028 Uiso 1 1 calc R . .
C8 C 0.3575(4) 0.2839(3) 0.4768(2) 0.0195(8) Uani 1 1 d U . .
C9 C 0.2815(4) 0.3416(3) 0.5166(2) 0.0197(8) Uani 1 1 d U . .
C10 C 0.2903(4) 0.4514(3) 0.4961(2) 0.0222(9) Uani 1 1 d U . .
H10 H 0.2399 0.4921 0.5227 0.027 Uiso 1 1 calc R . .
C11 C 0.3693(4) 0.5034(3) 0.4387(2) 0.0211(8) Uani 1 1 d U . .
C12 C 0.4428(4) 0.4423(3) 0.4013(2) 0.0210(8) Uani 1 1 d U . .
H12 H 0.4981 0.4767 0.3620 0.025 Uiso 1 1 calc R . .
C13 C 0.4387(4) 0.3323(3) 0.4190(2) 0.0192(8) Uani 1 1 d U . .
C14 C 0.5251(4) 0.2702(3) 0.3771(2) 0.0228(9) Uani 1 1 d U . .
H14A H 0.5327 0.3141 0.3264 0.027 Uiso 1 1 calc R . .
H14B H 0.4810 0.2054 0.3777 0.027 Uiso 1 1 calc R . .
C15 C 0.6940(4) 0.1450(3) 0.4637(2) 0.0212(8) Uani 1 1 d U . .
C16 C 0.6658(4) 0.2385(3) 0.4088(2) 0.0206(8) Uani 1 1 d U . .
C17 C 0.7682(4) 0.3065(3) 0.3873(2) 0.0220(9) Uani 1 1 d U . .
H17 H 0.7500 0.3712 0.3502 0.026 Uiso 1 1 calc R . .
C18 C 0.8951(4) 0.2846(3) 0.4172(2) 0.0226(9) Uani 1 1 d U . .
C19 C 0.9176(4) 0.1905(3) 0.4723(2) 0.0226(9) Uani 1 1 d U . .
H19 H 1.0039 0.1748 0.4944 0.027 Uiso 1 1 calc R . .
C20 C 0.8204(4) 0.1185(3) 0.4968(2) 0.0214(8) Uani 1 1 d U . .
C21 C 0.8505(4) 0.0161(3) 0.5573(2) 0.0236(9) Uani 1 1 d U . .
H21A H 0.7968 -0.0394 0.5499 0.028 Uiso 1 1 calc R . .
H21B H 0.9475 -0.0081 0.5547 0.028 Uiso 1 1 calc R . .
C22 C 0.6902(4) 0.0165(3) 0.6628(2) 0.0224(9) Uani 1 1 d U . .
C23 C 0.8195(4) 0.0267(3) 0.6318(2) 0.0234(9) Uani 1 1 d U . .
C24 C 0.9205(4) 0.0495(3) 0.6714(2) 0.0253(9) Uani 1 1 d U . .
H24 H 1.0097 0.0548 0.6519 0.030 Uiso 1 1 calc R . .
C25 C 0.8959(4) 0.0646(3) 0.7382(2) 0.0274(9) Uani 1 1 d U . .
C26 C 0.7652(4) 0.0546(3) 0.7662(2) 0.0281(9) Uani 1 1 d U . .
H26 H 0.7469 0.0638 0.8123 0.034 Uiso 1 1 calc R . .
C27 C 0.6606(4) 0.0318(3) 0.7293(2) 0.0240(9) Uani 1 1 d U . .
C28 C 0.5166(4) 0.0281(3) 0.7601(2) 0.0280(9) Uani 1 1 d U . .
H28A H 0.4709 -0.0266 0.7464 0.034 Uiso 1 1 calc R . .
H28B H 0.5207 0.0069 0.8132 0.034 Uiso 1 1 calc R . .
C29 C 0.3700(4) 0.3886(3) 0.7898(2) 0.0299(10) Uani 1 1 d U . .
H29A H 0.3934 0.4572 0.7561 0.036 Uiso 1 1 calc R . .
H29B H 0.4424 0.3640 0.8260 0.036 Uiso 1 1 calc R . .
C30 C 0.2372(4) 0.4060(4) 0.8272(3) 0.0372(11) Uani 1 1 d U . .
H30A H 0.2208 0.3401 0.8659 0.045 Uiso 1 1 calc R . .
H30B H 0.1628 0.4197 0.7922 0.045 Uiso 1 1 calc R . .
C31 C 0.2335(5) 0.4985(4) 0.8595(3) 0.0407(12) Uani 1 1 d U . .
H31A H 0.2422 0.5651 0.8202 0.049 Uiso 1 1 calc R . .
H31B H 0.1441 0.5048 0.8829 0.049 Uiso 1 1 calc R . .
C32 C 0.3429(5) 0.4878(4) 0.9138(3) 0.0419(12) Uani 1 1 d U . .
H32A H 0.4323 0.4896 0.8893 0.050 Uiso 1 1 calc R . .
H32B H 0.3406 0.4178 0.9506 0.050 Uiso 1 1 calc R . .
C33 C 0.3278(5) 0.5759(4) 0.9513(3) 0.0459(12) Uani 1 1 d U . .
H33A H 0.2469 0.5650 0.9831 0.055 Uiso 1 1 calc R . .
H33B H 0.4077 0.5679 0.9821 0.055 Uiso 1 1 calc R . .
C34 C 0.3147(5) 0.6874(4) 0.9020(3) 0.0421(12) Uani 1 1 d U . .
H34A H 0.3102 0.7378 0.9310 0.051 Uiso 1 1 calc R . .
H34B H 0.2289 0.6989 0.8753 0.051 Uiso 1 1 calc R . .
C35 C 0.3716(4) 0.6234(3) 0.4155(2) 0.0254(9) Uani 1 1 d U . .
H35A H 0.4360 0.6446 0.3747 0.031 Uiso 1 1 calc R . .
H35B H 0.4053 0.6456 0.4556 0.031 Uiso 1 1 calc R . .
C36 C 0.2325(4) 0.6824(3) 0.3929(2) 0.0276(9) Uani 1 1 d U . .
H36A H 0.1754 0.6758 0.4365 0.033 Uiso 1 1 calc R . .
H36B H 0.2446 0.7589 0.3709 0.033 Uiso 1 1 calc R . .
C37 C 0.1574(4) 0.6433(3) 0.3406(2) 0.0289(10) Uani 1 1 d U . .
H37A H 0.0703 0.6872 0.3290 0.035 Uiso 1 1 calc R . .
H37B H 0.1361 0.5693 0.3648 0.035 Uiso 1 1 calc R . .
C38 C 0.2322(4) 0.6458(3) 0.2702(2) 0.0287(10) Uani 1 1 d U . .
H38A H 0.2580 0.7189 0.2466 0.034 Uiso 1 1 calc R . .
H38B H 0.3164 0.5980 0.2808 0.034 Uiso 1 1 calc R . .
C39 C 0.1457(5) 0.6115(4) 0.2191(2) 0.0392(11) Uani 1 1 d U . .
H39A H 0.1103 0.5427 0.2454 0.047 Uiso 1 1 calc R . .
H39B H 0.0671 0.6645 0.2045 0.047 Uiso 1 1 calc R . .
C40 C 0.2186(6) 0.5995(4) 0.1526(3) 0.0477(13) Uani 1 1 d U . .
H40A H 0.1583 0.5697 0.1254 0.057 Uiso 1 1 calc R . .
H40B H 0.2996 0.5488 0.1666 0.057 Uiso 1 1 calc R . .
C41 C 1.0062(4) 0.3588(3) 0.3906(2) 0.0287(10) Uani 1 1 d U . .
H41A H 1.0500 0.3696 0.4324 0.034 Uiso 1 1 calc R . .
H41B H 0.9653 0.4288 0.3615 0.034 Uiso 1 1 calc R . .
C42 C 1.1135(4) 0.3175(3) 0.3457(2) 0.0306(10) Uani 1 1 d U . .
H42A H 1.1855 0.3675 0.3332 0.037 Uiso 1 1 calc R . .
H42B H 1.1550 0.2481 0.3753 0.037 Uiso 1 1 calc R . .
C43 C 1.0624(5) 0.3035(4) 0.2771(2) 0.0358(11) Uani 1 1 d U B .
H43A H 0.9924 0.2517 0.2893 0.043 Uiso 1 1 calc R . .
H43B H 1.0193 0.3723 0.2475 0.043 Uiso 1 1 calc R . .
C44 C 1.1737(6) 0.2649(4) 0.2337(3) 0.0523(13) Uani 1 1 d DU . .
H44A H 1.2214 0.2001 0.2658 0.063 Uiso 1 1 calc R A 1
H44B H 1.2395 0.3198 0.2196 0.063 Uiso 1 1 calc R A 1
C45A C 1.1343(11) 0.2384(6) 0.1642(4) 0.050(2) Uani 0.752(15) 1 d PDU B 1
H45A H 1.2044 0.1874 0.1528 0.060 Uiso 0.752(15) 1 calc PR B 1
H45B H 1.0469 0.2056 0.1719 0.060 Uiso 0.752(15) 1 calc PR B 1
C46A C 1.1227(8) 0.3399(6) 0.1031(4) 0.047(2) Uani 0.752(15) 1 d PDU B 1
H46A H 1.2135 0.3659 0.0897 0.056 Uiso 0.752(15) 1 calc PR B 1
H46B H 1.0652 0.3954 0.1178 0.056 Uiso 0.752(15) 1 calc PR B 1
C45B C 1.0832(17) 0.279(3) 0.1660(9) 0.059(9) Uani 0.248(15) 1 d PDU B 2
H45C H 1.0163 0.2245 0.1790 0.071 Uiso 0.248(15) 1 calc PR B 2
H45D H 1.0321 0.3495 0.1545 0.071 Uiso 0.248(15) 1 calc PR B 2
C46B C 1.1585(19) 0.269(4) 0.1000(10) 0.076(12) Uani 0.248(15) 1 d PDU B 2
H46C H 1.2123 0.1994 0.1125 0.091 Uiso 0.248(15) 1 calc PR B 2
H46D H 1.2233 0.3248 0.0867 0.091 Uiso 0.248(15) 1 calc PR B 2
C47 C 1.0064(5) 0.0889(4) 0.7808(3) 0.0396(11) Uani 1 1 d U D .
H47A H 1.0706 0.1325 0.7469 0.048 Uiso 1 1 calc R . .
H47B H 0.9653 0.1322 0.8110 0.048 Uiso 1 1 calc R . .
C48 C 1.0843(7) -0.0073(5) 0.8281(3) 0.081(2) Uani 1 1 d DU . .
H48A H 1.1550 -0.0383 0.8012 0.098 Uiso 1 1 calc R C 1
H48B H 1.0246 -0.0626 0.8545 0.098 Uiso 1 1 calc R C 1
C49A C 1.1464(17) 0.0507(10) 0.8789(6) 0.064(6) Uani 0.430(14) 1 d PDU D 1
H49A H 1.2167 0.0959 0.8518 0.076 Uiso 0.430(14) 1 calc PR D 1
H49B H 1.0741 0.0980 0.8926 0.076 Uiso 0.430(14) 1 calc PR D 1
C50A C 1.206(2) -0.0223(11) 0.9435(7) 0.064(6) Uani 0.430(14) 1 d PDU D 1
H50A H 1.2756 -0.0699 0.9282 0.076 Uiso 0.430(14) 1 calc PR D 1
H50B H 1.1340 -0.0672 0.9689 0.076 Uiso 0.430(14) 1 calc PR D 1
C51A C 1.271(2) 0.0185(19) 0.9985(9) 0.036(5) Uani 0.430(14) 1 d PDU D 1
H51A H 1.1995 0.0497 1.0248 0.043 Uiso 0.430(14) 1 calc PR D 1
H51B H 1.3208 -0.0418 1.0338 0.043 Uiso 0.430(14) 1 calc PR D 1
C52A C 1.367(2) 0.1009(17) 0.9635(9) 0.047(5) Uani 0.430(14) 1 d PDU D 1
H52A H 1.3225 0.1568 0.9233 0.057 Uiso 0.430(14) 1 calc PR D 1
H52B H 1.4484 0.0681 0.9449 0.057 Uiso 0.430(14) 1 calc PR D 1
C49B C 1.2050(8) -0.0032(8) 0.8767(5) 0.040(3) Uani 0.570(14) 1 d PDU D 2
H49C H 1.2580 -0.0731 0.8933 0.048 Uiso 0.570(14) 1 calc PR D 2
H49D H 1.2661 0.0516 0.8514 0.048 Uiso 0.570(14) 1 calc PR D 2
C50B C 1.1320(10) 0.0253(12) 0.9377(7) 0.057(3) Uani 0.570(14) 1 d PDU D 2
H50C H 1.0679 -0.0290 0.9596 0.069 Uiso 0.570(14) 1 calc PR D 2
H50D H 1.0784 0.0944 0.9188 0.069 Uiso 0.570(14) 1 calc PR D 2
C51B C 1.2282(19) 0.0331(17) 0.9963(8) 0.051(5) Uani 0.570(14) 1 d PDU D 2
H51C H 1.1738 0.0424 1.0379 0.061 Uiso 0.570(14) 1 calc PR D 2
H51D H 1.2866 -0.0341 1.0128 0.061 Uiso 0.570(14) 1 calc PR D 2
C52B C 1.3161(12) 0.1243(13) 0.9696(8) 0.042(3) Uani 0.570(14) 1 d PDU D 2
H52C H 1.2566 0.1902 0.9499 0.051 Uiso 0.570(14) 1 calc PR D 2
H52D H 1.3729 0.1122 0.9294 0.051 Uiso 0.570(14) 1 calc PR D 2
O1 O 0.3418(3) 0.0853(2) 0.63695(15) 0.0273(6) Uani 1 1 d U . .
H1 H 0.4190 0.0560 0.6322 0.041 Uiso 1 1 calc R . .
O2 O 0.3498(3) 0.1744(2) 0.49418(14) 0.0239(6) Uani 1 1 d U . .
H2 H 0.3339 0.1499 0.5384 0.036 Uiso 1 1 calc R . .
O3 O 0.5959(3) 0.0733(2) 0.48528(15) 0.0230(6) Uani 1 1 d U . .
H3A H 0.5196 0.1066 0.4848 0.035 Uiso 1 1 calc R . .
O4 O 0.5882(3) -0.0114(2) 0.62638(15) 0.0268(6) Uani 1 1 d U . .
H4 H 0.5981 0.0164 0.5820 0.040 Uiso 1 1 calc R . .
Br1 Br 0.46524(7) 0.71768(6) 0.83355(4) 0.0717(2) Uani 1 1 d U . .
Br2 Br 0.27402(7) 0.73455(5) 0.09125(3) 0.0591(2) Uani 1 1 d U . .
Br3A Br 1.0423(4) 0.3114(4) 0.0216(2) 0.0665(7) Uani 0.752(15) 1 d PDU B 1
Br3B Br 1.0515(13) 0.2807(13) 0.0153(5) 0.064(2) Uani 0.248(15) 1 d PDU B 2
Br4A Br 1.4155(11) 0.1607(7) 1.0393(6) 0.0454(12) Uani 0.430(14) 1 d PDU D 1
Br4B Br 1.4356(9) 0.1478(6) 1.0407(4) 0.0612(13) Uani 0.570(14) 1 d PDU D 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
C1 C2 1.384(6) . ?
C1 O1 1.388(5) . ?
C1 C6 1.397(6) . ?
C2 C3 1.392(6) . ?
C2 C28 1.514(6) . ?
C3 C4 1.386(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(6) . ?
C4 C29 1.510(6) . ?
C5 C6 1.390(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.512(5) . ?
C7 C9 1.506(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C13 1.387(5) . ?
C8 O2 1.391(4) . ?
C8 C9 1.398(5) . ?
C9 C10 1.394(5) . ?
C10 C11 1.384(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.385(5) . ?
C11 C35 1.515(5) . ?
C12 C13 1.394(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.514(5) . ?
C14 C16 1.520(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 O3 1.384(4) . ?
C15 C16 1.388(5) . ?
C15 C20 1.399(5) . ?
C16 C17 1.385(5) . ?
C17 C18 1.376(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(6) . ?
C18 C41 1.513(5) . ?
C19 C20 1.386(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.522(5) . ?
C21 C23 1.517(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C27 1.388(6) . ?
C22 O4 1.391(5) . ?
C22 C23 1.396(6) . ?
C23 C24 1.391(6) . ?
C24 C25 1.383(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.389(6) . ?
C25 C47 1.509(6) . ?
C26 C27 1.386(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.528(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.514(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.527(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.511(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.540(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.499(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 Br1 1.952(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.534(6) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.514(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.528(6) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.527(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.503(7) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 Br2 1.943(5) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.518(6) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.514(6) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.508(7) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45A 1.565(7) . ?
C44 C45B 1.579(8) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45A C46A 1.506(10) . ?
C45A H45A 0.9900 . ?
C45A H45B 0.9900 . ?
C46A Br3A 1.950(6) . ?
C46A H46A 0.9900 . ?
C46A H46B 0.9900 . ?
C45B C46B 1.496(18) . ?
C45B H45C 0.9900 . ?
C45B H45D 0.9900 . ?
C46B Br3B 1.956(7) . ?
C46B H46C 0.9900 . ?
C46B H46D 0.9900 . ?
C47 C48 1.498(7) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49B 1.568(7) . ?
C48 C49A 1.589(8) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49A C50A 1.449(15) . ?
C49A H49A 0.9900 . ?
C49A H49B 0.9900 . ?
C50A C51A 1.519(14) . ?
C50A H50A 0.9900 . ?
C50A H50B 0.9900 . ?
C51A C52A 1.500(14) . ?
C51A H51A 0.9900 . ?
C51A H51B 0.9900 . ?
C52A Br4A 1.960(7) . ?
C52A H52A 0.9900 . ?
C52A H52B 0.9900 . ?
C49B C50B 1.493(12) . ?
C49B H49C 0.9900 . ?
C49B H49D 0.9900 . ?
C50B C51B 1.546(13) . ?
C50B H50C 0.9900 . ?
C50B H50D 0.9900 . ?
C51B C52B 1.503(12) . ?
C51B H51C 0.9900 . ?
C51B H51D 0.9900 . ?
C52B Br4B 1.965(6) . ?
C52B H52C 0.9900 . ?
C52B H52D 0.9900 . ?
O1 H1 0.8400 . ?
O2 H2 0.8400 . ?
O3 H3A 0.8400 . ?
O4 H4 0.8400 . ?
 
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
C2 C1 O1 120.1(3) . . ?
C2 C1 C6 122.0(4) . . ?
O1 C1 C6 118.0(3) . . ?
C1 C2 C3 118.0(4) . . ?
C1 C2 C28 122.2(4) . . ?
C3 C2 C28 119.8(4) . . ?
C4 C3 C2 122.3(4) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
C3 C4 C5 117.5(4) . . ?
C3 C4 C29 121.7(4) . . ?
C5 C4 C29 120.8(4) . . ?
C4 C5 C6 122.6(4) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C5 C6 C1 117.5(4) . . ?
C5 C6 C7 120.2(3) . . ?
C1 C6 C7 122.2(3) . . ?
C9 C7 C6 111.7(3) . . ?
C9 C7 H7A 109.3 . . ?
C6 C7 H7A 109.3 . . ?
C9 C7 H7B 109.3 . . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
C13 C8 O2 118.4(3) . . ?
C13 C8 C9 122.2(3) . . ?
O2 C8 C9 119.4(3) . . ?
C10 C9 C8 117.3(4) . . ?
C10 C9 C7 120.3(3) . . ?
C8 C9 C7 122.4(3) . . ?
C11 C10 C9 122.7(4) . . ?
C11 C10 H10 118.7 . . ?
C9 C10 H10 118.7 . . ?
C10 C11 C12 117.6(3) . . ?
C10 C11 C35 121.5(3) . . ?
C12 C11 C35 120.8(4) . . ?
C11 C12 C13 122.6(4) . . ?
C11 C12 H12 118.7 . . ?
C13 C12 H12 118.7 . . ?
C8 C13 C12 117.6(3) . . ?
C8 C13 C14 122.7(3) . . ?
C12 C13 C14 119.7(4) . . ?
C13 C14 C16 111.0(3) . . ?
C13 C14 H14A 109.4 . . ?
C16 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
C16 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
O3 C15 C16 119.4(3) . . ?
O3 C15 C20 118.3(3) . . ?
C16 C15 C20 122.2(4) . . ?
C17 C16 C15 117.6(3) . . ?
C17 C16 C14 120.6(3) . . ?
C15 C16 C14 121.6(3) . . ?
C18 C17 C16 123.1(4) . . ?
C18 C17 H17 118.5 . . ?
C16 C17 H17 118.5 . . ?
C17 C18 C19 117.1(4) . . ?
C17 C18 C41 121.7(4) . . ?
C19 C18 C41 121.2(3) . . ?
C20 C19 C18 123.3(4) . . ?
C20 C19 H19 118.4 . . ?
C18 C19 H19 118.4 . . ?
C19 C20 C15 116.8(4) . . ?
C19 C20 C21 121.2(3) . . ?
C15 C20 C21 122.0(3) . . ?
C23 C21 C20 114.1(3) . . ?
C23 C21 H21A 108.7 . . ?
C20 C21 H21A 108.7 . . ?
C23 C21 H21B 108.7 . . ?
C20 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C27 C22 O4 118.8(4) . . ?
C27 C22 C23 122.1(4) . . ?
O4 C22 C23 119.1(3) . . ?
C24 C23 C22 117.4(4) . . ?
C24 C23 C21 120.3(4) . . ?
C22 C23 C21 122.3(3) . . ?
C25 C24 C23 122.5(4) . . ?
C25 C24 H24 118.7 . . ?
C23 C24 H24 118.7 . . ?
C24 C25 C26 117.8(4) . . ?
C24 C25 C47 122.0(4) . . ?
C26 C25 C47 120.2(4) . . ?
C27 C26 C25 122.3(4) . . ?
C27 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
C26 C27 C22 117.9(4) . . ?
C26 C27 C28 120.6(4) . . ?
C22 C27 C28 121.5(4) . . ?
C2 C28 C27 112.6(3) . . ?
C2 C28 H28A 109.1 . . ?
C27 C28 H28A 109.1 . . ?
C2 C28 H28B 109.1 . . ?
C27 C28 H28B 109.1 . . ?
H28A C28 H28B 107.8 . . ?
C4 C29 C30 112.9(3) . . ?
C4 C29 H29A 109.0 . . ?
C30 C29 H29A 109.0 . . ?
C4 C29 H29B 109.0 . . ?
C30 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
C29 C30 C31 113.4(4) . . ?
C29 C30 H30A 108.9 . . ?
C31 C30 H30A 108.9 . . ?
C29 C30 H30B 108.9 . . ?
C31 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C32 C31 C30 114.3(4) . . ?
C32 C31 H31A 108.7 . . ?
C30 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
C30 C31 H31B 108.7 . . ?
H31A C31 H31B 107.6 . . ?
C31 C32 C33 113.2(4) . . ?
C31 C32 H32A 108.9 . . ?
C33 C32 H32A 108.9 . . ?
C31 C32 H32B 108.9 . . ?
C33 C32 H32B 108.9 . . ?
H32A C32 H32B 107.8 . . ?
C34 C33 C32 115.3(4) . . ?
C34 C33 H33A 108.5 . . ?
C32 C33 H33A 108.5 . . ?
C34 C33 H33B 108.5 . . ?
C32 C33 H33B 108.5 . . ?
H33A C33 H33B 107.5 . . ?
C33 C34 Br1 112.7(3) . . ?
C33 C34 H34A 109.1 . . ?
Br1 C34 H34A 109.1 . . ?
C33 C34 H34B 109.1 . . ?
Br1 C34 H34B 109.1 . . ?
H34A C34 H34B 107.8 . . ?
C11 C35 C36 113.3(3) . . ?
C11 C35 H35A 108.9 . . ?
C36 C35 H35A 108.9 . . ?
C11 C35 H35B 108.9 . . ?
C36 C35 H35B 108.9 . . ?
H35A C35 H35B 107.7 . . ?
C37 C36 C35 115.0(3) . . ?
C37 C36 H36A 108.5 . . ?
C35 C36 H36A 108.5 . . ?
C37 C36 H36B 108.5 . . ?
C35 C36 H36B 108.5 . . ?
H36A C36 H36B 107.5 . . ?
C36 C37 C38 115.6(3) . . ?
C36 C37 H37A 108.4 . . ?
C38 C37 H37A 108.4 . . ?
C36 C37 H37B 108.4 . . ?
C38 C37 H37B 108.4 . . ?
H37A C37 H37B 107.4 . . ?
C39 C38 C37 112.0(4) . . ?
C39 C38 H38A 109.2 . . ?
C37 C38 H38A 109.2 . . ?
C39 C38 H38B 109.2 . . ?
C37 C38 H38B 109.2 . . ?
H38A C38 H38B 107.9 . . ?
C40 C39 C38 114.8(4) . . ?
C40 C39 H39A 108.6 . . ?
C38 C39 H39A 108.6 . . ?
C40 C39 H39B 108.6 . . ?
C38 C39 H39B 108.6 . . ?
H39A C39 H39B 107.6 . . ?
C39 C40 Br2 111.9(3) . . ?
C39 C40 H40A 109.2 . . ?
Br2 C40 H40A 109.2 . . ?
C39 C40 H40B 109.2 . . ?
Br2 C40 H40B 109.2 . . ?
H40A C40 H40B 107.9 . . ?
C18 C41 C42 113.2(3) . . ?
C18 C41 H41A 108.9 . . ?
C42 C41 H41A 108.9 . . ?
C18 C41 H41B 108.9 . . ?
C42 C41 H41B 108.9 . . ?
H41A C41 H41B 107.7 . . ?
C43 C42 C41 114.9(4) . . ?
C43 C42 H42A 108.5 . . ?
C41 C42 H42A 108.5 . . ?
C43 C42 H42B 108.5 . . ?
C41 C42 H42B 108.5 . . ?
H42A C42 H42B 107.5 . . ?
C44 C43 C42 112.7(4) . . ?
C44 C43 H43A 109.1 . . ?
C42 C43 H43A 109.1 . . ?
C44 C43 H43B 109.1 . . ?
C42 C43 H43B 109.1 . . ?
H43A C43 H43B 107.8 . . ?
C43 C44 C45A 118.4(5) . . ?
C43 C44 C45B 95.3(9) . . ?
C45A C44 C45B 26.0(9) . . ?
C43 C44 H44A 107.7 . . ?
C45A C44 H44A 107.7 . . ?
C45B C44 H44A 130.0 . . ?
C43 C44 H44B 107.7 . . ?
C45A C44 H44B 107.7 . . ?
C45B C44 H44B 107.0 . . ?
H44A C44 H44B 107.1 . . ?
C46A C45A C44 108.7(5) . . ?
C46A C45A H45A 109.9 . . ?
C44 C45A H45A 109.9 . . ?
C46A C45A H45B 109.9 . . ?
C44 C45A H45B 109.9 . . ?
H45A C45A H45B 108.3 . . ?
C45A C46A Br3A 108.6(5) . . ?
C45A C46A H46A 110.0 . . ?
Br3A C46A H46A 110.0 . . ?
C45A C46A H46B 110.0 . . ?
Br3A C46A H46B 110.0 . . ?
H46A C46A H46B 108.4 . . ?
C46B C45B C44 115.4(11) . . ?
C46B C45B H45C 108.4 . . ?
C44 C45B H45C 108.4 . . ?
C46B C45B H45D 108.4 . . ?
C44 C45B H45D 108.4 . . ?
H45C C45B H45D 107.5 . . ?
C45B C46B Br3B 117.4(11) . . ?
C45B C46B H46C 108.0 . . ?
Br3B C46B H46C 108.0 . . ?
C45B C46B H46D 108.0 . . ?
Br3B C46B H46D 108.0 . . ?
H46C C46B H46D 107.2 . . ?
C48 C47 C25 114.5(4) . . ?
C48 C47 H47A 108.6 . . ?
C25 C47 H47A 108.6 . . ?
C48 C47 H47B 108.6 . . ?
C25 C47 H47B 108.6 . . ?
H47A C47 H47B 107.6 . . ?
C47 C48 C49B 124.3(6) . . ?
C47 C48 C49A 96.8(6) . . ?
C49B C48 C49A 32.7(6) . . ?
C47 C48 H48A 112.4 . . ?
C49B C48 H48A 84.1 . . ?
C49A C48 H48A 112.4 . . ?
C47 C48 H48B 112.4 . . ?
C49B C48 H48B 110.1 . . ?
C49A C48 H48B 112.4 . . ?
H48A C48 H48B 109.9 . . ?
C50A C49A C48 113.4(10) . . ?
C50A C49A H49A 108.9 . . ?
C48 C49A H49A 108.9 . . ?
C50A C49A H49B 108.9 . . ?
C48 C49A H49B 108.9 . . ?
H49A C49A H49B 107.7 . . ?
C49A C50A C51A 121.0(13) . . ?
C49A C50A H50A 107.1 . . ?
C51A C50A H50A 107.1 . . ?
C49A C50A H50B 107.1 . . ?
C51A C50A H50B 107.1 . . ?
H50A C50A H50B 106.8 . . ?
C52A C51A C50A 111.4(12) . . ?
C52A C51A H51A 109.4 . . ?
C50A C51A H51A 109.4 . . ?
C52A C51A H51B 109.4 . . ?
C50A C51A H51B 109.4 . . ?
H51A C51A H51B 108.0 . . ?
C51A C52A Br4A 105.3(11) . . ?
C51A C52A H52A 110.7 . . ?
Br4A C52A H52A 110.7 . . ?
C51A C52A H52B 110.7 . . ?
Br4A C52A H52B 110.7 . . ?
H52A C52A H52B 108.8 . . ?
C50B C49B C48 101.6(7) . . ?
C50B C49B H49C 111.5 . . ?
C48 C49B H49C 111.5 . . ?
C50B C49B H49D 111.5 . . ?
C48 C49B H49D 111.5 . . ?
H49C C49B H49D 109.3 . . ?
C49B C50B C51B 113.1(11) . . ?
C49B C50B H50C 109.0 . . ?
C51B C50B H50C 109.0 . . ?
C49B C50B H50D 109.0 . . ?
C51B C50B H50D 109.0 . . ?
H50C C50B H50D 107.8 . . ?
C52B C51B C50B 112.2(10) . . ?
C52B C51B H51C 109.2 . . ?
C50B C51B H51C 109.2 . . ?
C52B C51B H51D 109.2 . . ?
C50B C51B H51D 109.2 . . ?
H51C C51B H51D 107.9 . . ?
C51B C52B Br4B 116.1(10) . . ?
C51B C52B H52C 108.3 . . ?
Br4B C52B H52C 108.3 . . ?
C51B C52B H52D 108.3 . . ?
Br4B C52B H52D 108.3 . . ?
H52C C52B H52D 107.4 . . ?
C1 O1 H1 109.5 . . ?
C8 O2 H2 109.5 . . ?
C15 O3 H3A 109.5 . . ?
C22 O4 H4 109.5 . . ?
 
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 O4  0.84 1.84 2.682(4) 177.3 .
O2 H2 O1  0.84 1.86 2.684(4) 166.5 .
O3 H3A O2  0.84 1.86 2.700(4) 174.1 .
O4 H4 O3  0.84 1.81 2.647(4) 172.3 .
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    0.985
_refine_diff_density_min   -1.038
_refine_diff_density_rms    0.088
