 
data_porco7 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C48 H100 Br4 O12' 
_chemical_formula_weight          1188.92 
 
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            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                    9.8354(10) 
_cell_length_b                    9.7459(9) 
_cell_length_c                    12.7953(13) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  92.642(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      1225.2(2) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     223(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.30 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.611 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              624 
_exptl_absorpt_coefficient_mu     3.347 
_exptl_absorpt_correction_type    SADABS 
_exptl_absorpt_correction_T_min   0.495742 
_exptl_absorpt_correction_T_max   0.5541 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       223(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 1K CCD ' 
_diffrn_measurement_method        '0.3 deg. omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             8044 
_diffrn_reflns_av_R_equivalents   0.0393 
_diffrn_reflns_av_sigmaI/netI     0.0693 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          2.56 
_diffrn_reflns_theta_max          26.37 
_reflns_number_total              4610 
_reflns_number_gt                 3559 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        SMART 
_computing_cell_refinement        SAINT+ 
_computing_data_reduction         SAINT+ 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     SHELXTL 
_computing_publication_material   SHELXTL 
 
_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)+(0.0448P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.016(10) 
_refine_ls_number_reflns          4610 
_refine_ls_number_parameters      367 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0571 
_refine_ls_R_factor_gt            0.0362 
_refine_ls_wR_factor_ref          0.0819 
_refine_ls_wR_factor_gt           0.0737 
_refine_ls_goodness_of_fit_ref    0.867 
_refine_ls_restrained_S_all       0.867 
_refine_ls_shift/su_max           0.243 
_refine_ls_shift/su_mean          0.021 
 
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 
Br1 Br 0.26070(4) 0.92741(6) 0.26122(4) 0.05254(16) Uani 1 1 d . . . 
Br2 Br -0.29644(6) 0.13339(5) 0.46807(5) 0.06547(19) Uani 1 1 d . . . 
O1 O -0.0220(3) 0.7164(4) 0.0088(3) 0.0467(8) Uani 1 1 d . . . 
O2 O 0.2483(3) 0.9358(5) 0.0276(2) 0.0629(10) Uani 1 1 d . . . 
O3 O -0.0714(3) 0.7714(3) 0.3627(2) 0.0390(7) Uani 1 1 d . . . 
O4 O -0.2834(4) 0.8307(4) 0.4095(3) 0.0509(9) Uani 1 1 d . . . 
O5 O -0.2122(3) 0.9971(3) 0.1268(3) 0.0421(8) Uani 1 1 d . . . 
O6 O -0.2186(3) 0.7646(3) 0.1721(2) 0.0363(7) Uani 1 1 d . . . 
C1 C 0.1064(4) 0.9008(4) 0.1688(3) 0.0353(10) Uani 1 1 d . . . 
C2 C 0.1394(4) 0.8991(5) 0.0563(3) 0.0403(11) Uani 1 1 d . . . 
C3 C 0.0303(4) 0.8501(5) -0.0191(3) 0.0379(10) Uani 1 1 d . . . 
C4 C -0.1061(4) 0.8342(5) 0.0187(3) 0.0368(10) Uani 1 1 d . . . 
C5 C -0.1413(4) 0.8699(4) 0.1297(3) 0.0339(10) Uani 1 1 d . . . 
C6 C -0.0186(4) 0.8891(4) 0.2051(3) 0.0315(10) Uani 1 1 d . . . 
C7 C -0.0516(5) 0.9059(5) 0.3176(3) 0.0395(10) Uani 1 1 d . . . 
C8 C -0.1967(5) 0.7448(5) 0.3997(3) 0.0383(11) Uani 1 1 d . . . 
C9 C -0.2128(5) 0.5980(4) 0.4226(3) 0.0365(11) Uani 1 1 d . . . 
C10 C -0.3384(5) 0.5549(5) 0.4569(4) 0.0418(12) Uani 1 1 d . . . 
C11 C -0.3640(5) 0.4169(6) 0.4718(3) 0.0444(11) Uani 1 1 d . . . 
C12 C -0.2632(5) 0.3229(5) 0.4533(4) 0.0421(11) Uani 1 1 d . . . 
C13 C -0.1372(5) 0.3647(5) 0.4229(4) 0.0445(13) Uani 1 1 d . . . 
C14 C -0.1120(5) 0.5022(5) 0.4081(4) 0.0414(11) Uani 1 1 d . . . 
C15 C -0.3557(4) 0.9865(5) 0.1473(4) 0.0433(12) Uani 1 1 d . . . 
C16 C -0.4168(5) 0.8700(6) 0.0832(5) 0.0513(14) Uani 1 1 d . . . 
C17 C -0.3451(4) 0.7341(6) 0.1110(4) 0.0451(12) Uani 1 1 d . . . 
C18 C -0.4237(6) 0.6423(9) 0.1814(5) 0.0609(15) Uani 1 1 d . . . 
C19 C -0.4161(6) 1.1250(9) 0.1219(6) 0.0663(16) Uani 1 1 d . . . 
C20 C 0.0547(6) 0.8683(8) -0.1350(4) 0.0523(13) Uani 1 1 d . . . 
C21 C -0.0612(5) 0.8203(6) -0.2047(4) 0.0488(12) Uani 1 1 d . . . 
C22 C -0.1645(5) 0.8939(5) -0.2404(3) 0.0431(11) Uani 1 1 d . . . 
C23 C -0.1850(6) 1.0421(6) -0.2162(5) 0.0617(16) Uani 1 1 d . . . 
H23A H -0.255(3) 1.0511(7) -0.1694(17) 0.093 Uiso 1 1 calc R . . 
H23B H -0.2086(10) 1.0895(18) -0.278(2) 0.093 Uiso 1 1 calc R . . 
H23C H -0.104(3) 1.0785(15) -0.1860(12) 0.093 Uiso 1 1 calc R . . 
C24 C -0.2785(7) 0.8313(7) -0.3110(5) 0.078(2) Uani 1 1 d . . . 
H24A H -0.2697(8) 0.8612(14) -0.380(3) 0.117 Uiso 1 1 calc R . . 
H24B H -0.363(4) 0.8589(13) -0.2875(11) 0.117 Uiso 1 1 calc R . . 
H24C H -0.2723(7) 0.735(4) -0.3086(5) 0.117 Uiso 1 1 calc R . . 
H16B H -0.508(4) 0.867(4) 0.088(3) 0.023(10) Uiso 1 1 d . . . 
H15 H -0.359(4) 0.962(5) 0.217(3) 0.034(12) Uiso 1 1 d . . . 
H14 H -0.034(5) 0.535(5) 0.383(4) 0.038(12) Uiso 1 1 d . . . 
H7B H -0.133(4) 0.953(5) 0.320(3) 0.039(12) Uiso 1 1 d . . . 
H13 H -0.078(5) 0.305(6) 0.411(4) 0.053(16) Uiso 1 1 d . . . 
H7A H 0.023(4) 0.950(5) 0.357(3) 0.028(10) Uiso 1 1 d . . . 
H20B H 0.070(3) 0.950(4) -0.144(3) 0.000(9) Uiso 1 1 d . . . 
H19C H -0.374(5) 1.187(5) 0.163(4) 0.036(14) Uiso 1 1 d . . . 
H11 H -0.450(5) 0.392(6) 0.485(4) 0.061(16) Uiso 1 1 d . . . 
H10 H -0.421(5) 0.615(6) 0.467(4) 0.054(14) Uiso 1 1 d . . . 
H20A H 0.141(6) 0.820(6) -0.147(4) 0.060(15) Uiso 1 1 d . . . 
H19B H -0.507(6) 1.126(7) 0.136(4) 0.067(16) Uiso 1 1 d . . . 
H19A H -0.385(5) 1.163(6) 0.049(5) 0.063(16) Uiso 1 1 d . . . 
H21 H -0.074(5) 0.711(7) -0.222(4) 0.066(15) Uiso 1 1 d . . . 
H4 H -0.184(4) 0.840(4) -0.031(3) 0.026(10) Uiso 1 1 d . . . 
H16A H -0.413(4) 0.881(4) 0.006(4) 0.040(13) Uiso 1 1 d . . . 
H18C H -0.439(4) 0.692(4) 0.232(3) 0.019(11) Uiso 1 1 d . . . 
H18B H -0.522(6) 0.620(7) 0.150(4) 0.078(17) Uiso 1 1 d . . . 
H18A H -0.378(6) 0.553(7) 0.201(5) 0.08(2) Uiso 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 
Br1 C1 1.898(4) . ? 
Br2 C12 1.887(5) . ? 
O1 C4 1.424(6) . ? 
O1 C3 1.452(6) . ? 
O2 C2 1.202(5) . ? 
O3 C8 1.365(5) . ? 
O3 C7 1.449(6) . ? 
O4 C8 1.206(6) . ? 
O5 C5 1.422(5) . ? 
O5 C15 1.452(5) . ? 
O6 C5 1.402(5) . ? 
O6 C17 1.468(5) . ? 
C1 C6 1.339(6) . ? 
C1 C2 1.491(6) . ? 
C2 C3 1.487(6) . ? 
C3 C4 1.455(6) . ? 
C3 C20 1.523(7) . ? 
C4 C5 1.518(6) . ? 
C5 C6 1.521(5) . ? 
C6 C7 1.500(6) . ? 
C8 C9 1.471(7) . ? 
C9 C14 1.380(7) . ? 
C9 C10 1.395(7) . ? 
C10 C11 1.383(8) . ? 
C11 C12 1.378(7) . ? 
C12 C13 1.377(7) . ? 
C13 C14 1.378(7) . ? 
C15 C16 1.509(7) . ? 
C15 C19 1.504(9) . ? 
C16 C17 1.534(8) . ? 
C17 C18 1.508(8) . ? 
C20 C21 1.490(8) . ? 
C21 C22 1.309(7) . ? 
C22 C23 1.493(8) . ? 
C22 C24 1.533(7) . ? 
 
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 
C4 O1 C3 60.8(3) . . ? 
C8 O3 C7 116.7(4) . . ? 
C5 O5 C15 114.4(3) . . ? 
C5 O6 C17 113.8(3) . . ? 
C6 C1 C2 125.3(3) . . ? 
C6 C1 Br1 121.1(3) . . ? 
C2 C1 Br1 113.6(3) . . ? 
O2 C2 C1 121.9(4) . . ? 
O2 C2 C3 121.6(4) . . ? 
C1 C2 C3 116.5(3) . . ? 
O1 C3 C4 58.7(3) . . ? 
O1 C3 C2 112.5(3) . . ? 
C4 C3 C2 117.9(4) . . ? 
O1 C3 C20 114.7(4) . . ? 
C4 C3 C20 121.6(4) . . ? 
C2 C3 C20 116.9(4) . . ? 
O1 C4 C3 60.5(3) . . ? 
O1 C4 C5 115.2(4) . . ? 
C3 C4 C5 122.7(4) . . ? 
O6 C5 O5 112.0(3) . . ? 
O6 C5 C4 110.2(4) . . ? 
O5 C5 C4 107.9(3) . . ? 
O6 C5 C6 105.9(3) . . ? 
O5 C5 C6 106.4(3) . . ? 
C4 C5 C6 114.4(3) . . ? 
C1 C6 C7 124.5(4) . . ? 
C1 C6 C5 120.4(4) . . ? 
C7 C6 C5 114.9(3) . . ? 
O3 C7 C6 108.8(4) . . ? 
O4 C8 O3 123.9(4) . . ? 
O4 C8 C9 124.9(4) . . ? 
O3 C8 C9 111.2(4) . . ? 
C14 C9 C10 119.4(4) . . ? 
C14 C9 C8 123.1(4) . . ? 
C10 C9 C8 117.4(4) . . ? 
C11 C10 C9 120.3(4) . . ? 
C12 C11 C10 119.1(5) . . ? 
C13 C12 C11 121.0(5) . . ? 
C13 C12 Br2 118.7(4) . . ? 
C11 C12 Br2 120.3(4) . . ? 
C12 C13 C14 119.8(5) . . ? 
C9 C14 C13 120.3(5) . . ? 
O5 C15 C16 108.8(4) . . ? 
O5 C15 C19 106.0(4) . . ? 
C16 C15 C19 114.5(5) . . ? 
C15 C16 C17 110.9(4) . . ? 
O6 C17 C18 104.3(4) . . ? 
O6 C17 C16 108.5(4) . . ? 
C18 C17 C16 114.0(5) . . ? 
C21 C20 C3 113.3(4) . . ? 
C22 C21 C20 126.6(5) . . ? 
C21 C22 C23 124.6(5) . . ? 
C21 C22 C24 121.5(5) . . ? 
C23 C22 C24 113.9(5) . . ? 
 
_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              26.37 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    0.353 
_refine_diff_density_min   -0.294 
_refine_diff_density_rms    0.059 
