# Copyright The Royal Society of Chemistry, 1998 data_sz288 # For cpd 4, paper ref 8/02681E _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H20 Ba2 O4 S8' _chemical_formula_weight 759.44 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ba' 'Ba' -0.3244 2.2819 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2864(11) _cell_length_b 11.3404(14) _cell_length_c 10.8724(14) _cell_angle_alpha 90.00 _cell_angle_beta 108.885(8) _cell_angle_gamma 90.00 _cell_volume 1200.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.28mm _exptl_crystal_size_mid 0.28mm _exptl_crystal_size_min 0.12mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 3.973 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.500 _exptl_absorpt_correction_T_max 0.861 _exptl_absorpt_process_details ? _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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2766 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2115 _reflns_number_gt 1882 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCAN' _computing_cell_refinement 'Siemens XSCAN' _computing_data_reduction 'Siemens XSCAN' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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/[\s^2^(Fo^2^)+(0.0311P)^2^+0.3023P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2115 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0534 _refine_ls_wR_factor_gt 0.0512 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.058 _refine_ls_shift/su_mean 0.004 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 Ba1 Ba 0.38332(2) 0.354767(16) 0.116936(17) 0.01910(8) Uani 1 1 d . . . S11 S 0.31202(9) 0.16560(8) -0.11489(8) 0.0247(2) Uani 1 1 d . . . S12 S 0.09665(9) 0.23548(9) -0.36175(8) 0.0324(2) Uani 1 1 d . . . O14 O 0.1566(2) 0.3449(2) -0.1346(2) 0.0244(5) Uani 1 1 d . . . C13 C 0.1822(3) 0.2547(3) -0.2046(3) 0.0215(7) Uani 1 1 d . . . C15 C 0.0431(4) 0.4267(3) -0.1946(3) 0.0292(8) Uani 1 1 d . . . H15A H 0.0345 0.4378 -0.2853 0.035 Uiso 1 1 calc R . . H15B H 0.0633 0.5027 -0.1516 0.035 Uiso 1 1 calc R . . C16 C -0.0906(4) 0.3808(4) -0.1848(4) 0.0370(9) Uani 1 1 d . . . H16A H -0.1627 0.4359 -0.2247 0.055 Uiso 1 1 calc R . . H16B H -0.0827 0.3710 -0.0949 0.055 Uiso 1 1 calc R . . H16C H -0.1115 0.3062 -0.2285 0.055 Uiso 1 1 calc R . . S21 S 0.50805(10) 0.10329(7) 0.24112(8) 0.0301(2) Uani 1 1 d . . . S22 S 0.66147(9) 0.11323(8) 0.52609(8) 0.02332(19) Uani 1 1 d . . . O24 O 0.6238(3) 0.2882(2) 0.3553(2) 0.0280(6) Uani 1 1 d . . . C23 C 0.6010(3) 0.1757(3) 0.3772(3) 0.0208(7) Uani 1 1 d . . . C25 C 0.7020(5) 0.3665(4) 0.4601(4) 0.0425(11) Uani 1 1 d . . . H25A H 0.7504 0.3206 0.5364 0.051 Uiso 1 1 calc R . . H25B H 0.6402 0.4203 0.4830 0.051 Uiso 1 1 calc R . . C26 C 0.8015(4) 0.4339(4) 0.4150(4) 0.0391(9) Uani 1 1 d . . . H26A H 0.8535 0.4857 0.4830 0.059 Uiso 1 1 calc R . . H26B H 0.7527 0.4795 0.3398 0.059 Uiso 1 1 calc R . . H26C H 0.8626 0.3802 0.3930 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.02028(13) 0.01786(12) 0.01917(12) -0.00013(7) 0.00640(8) -0.00127(8) S11 0.0270(5) 0.0258(4) 0.0201(4) 0.0007(3) 0.0062(3) 0.0047(4) S12 0.0250(5) 0.0470(6) 0.0210(4) -0.0066(4) 0.0018(4) 0.0072(4) O14 0.0194(12) 0.0270(13) 0.0258(12) -0.0040(10) 0.0060(10) 0.0052(10) C13 0.0163(17) 0.0271(18) 0.0223(16) -0.0034(13) 0.0079(13) -0.0053(14) C15 0.0217(18) 0.0290(19) 0.0350(19) -0.0016(16) 0.0068(16) 0.0053(16) C16 0.023(2) 0.052(2) 0.036(2) 0.0074(19) 0.0096(16) 0.0067(19) S21 0.0329(5) 0.0196(4) 0.0268(4) -0.0014(4) -0.0057(4) 0.0001(4) S22 0.0233(4) 0.0247(4) 0.0211(4) 0.0026(3) 0.0059(3) 0.0023(4) O24 0.0340(15) 0.0250(13) 0.0215(11) 0.0003(10) 0.0040(11) -0.0080(12) C23 0.0144(17) 0.0229(17) 0.0257(17) -0.0014(13) 0.0072(14) 0.0011(14) C25 0.062(3) 0.034(2) 0.0241(19) -0.0083(16) 0.0035(19) -0.026(2) C26 0.024(2) 0.031(2) 0.056(2) -0.0044(19) 0.0044(18) -0.0041(18) _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 Ba1 O14 2.967(2) . ? Ba1 O24 3.042(2) . ? Ba1 S12 3.1997(10) 4_566 ? Ba1 S11 3.2088(9) . ? Ba1 S21 3.2338(9) 2_655 ? Ba1 S11 3.2368(9) 4_566 ? Ba1 S21 3.2374(9) . ? Ba1 S22 3.2799(9) 2_655 ? Ba1 S22 3.3351(9) 4_565 ? S11 C13 1.707(3) . ? S11 Ba1 3.2368(9) 4_565 ? S12 C13 1.664(3) . ? S12 Ba1 3.1997(10) 4_565 ? O14 C13 1.350(4) . ? O14 C15 1.468(4) . ? C15 C16 1.506(5) . ? S21 C23 1.692(3) . ? S21 Ba1 3.2338(9) 2_645 ? S22 C23 1.690(3) . ? S22 Ba1 3.2799(9) 2_645 ? S22 Ba1 3.3351(9) 4_566 ? O24 C23 1.333(4) . ? O24 C25 1.463(4) . ? C25 C26 1.482(6) . ? 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 O14 Ba1 O24 162.88(6) . . ? O14 Ba1 S12 65.59(5) . 4_566 ? O24 Ba1 S12 111.92(5) . 4_566 ? O14 Ba1 S11 48.63(5) . . ? O24 Ba1 S11 114.79(5) . . ? S12 Ba1 S11 82.03(2) 4_566 . ? O14 Ba1 S21 121.33(5) . 2_655 ? O24 Ba1 S21 75.50(5) . 2_655 ? S12 Ba1 S21 115.37(3) 4_566 2_655 ? S11 Ba1 S21 155.97(2) . 2_655 ? O14 Ba1 S11 119.20(5) . 4_566 ? O24 Ba1 S11 64.78(5) . 4_566 ? S12 Ba1 S11 55.19(2) 4_566 4_566 ? S11 Ba1 S11 126.803(19) . 4_566 ? S21 Ba1 S11 77.08(2) 2_655 4_566 ? O14 Ba1 S21 116.00(5) . . ? O24 Ba1 S21 47.39(5) . . ? S12 Ba1 S21 86.45(3) 4_566 . ? S11 Ba1 S21 72.40(2) . . ? S21 Ba1 S21 122.658(10) 2_655 . ? S11 Ba1 S21 74.71(2) 4_566 . ? O14 Ba1 S22 69.45(5) . 2_655 ? O24 Ba1 S22 125.19(5) . 2_655 ? S12 Ba1 S22 109.20(2) 4_566 2_655 ? S11 Ba1 S22 105.29(2) . 2_655 ? S21 Ba1 S22 54.64(2) 2_655 2_655 ? S11 Ba1 S22 116.93(2) 4_566 2_655 ? S21 Ba1 S22 163.91(3) . 2_655 ? O14 Ba1 S22 103.00(5) . 4_565 ? O24 Ba1 S22 74.94(5) . 4_565 ? S12 Ba1 S22 162.80(2) 4_566 4_565 ? S11 Ba1 S22 80.79(2) . 4_565 ? S21 Ba1 S22 81.34(2) 2_655 4_565 ? S11 Ba1 S22 137.80(2) 4_566 4_565 ? S21 Ba1 S22 87.55(3) . 4_565 ? S22 Ba1 S22 76.39(2) 2_655 4_565 ? C13 S11 Ba1 89.45(11) . . ? C13 S11 Ba1 83.74(10) . 4_565 ? Ba1 S11 Ba1 133.98(3) . 4_565 ? C13 S12 Ba1 85.57(12) . 4_565 ? C13 O14 C15 120.0(3) . . ? C13 O14 Ba1 108.03(19) . . ? C15 O14 Ba1 131.32(19) . . ? O14 C13 S12 122.9(3) . . ? O14 C13 S11 112.7(2) . . ? S12 C13 S11 124.4(2) . . ? O14 C15 C16 111.3(3) . . ? C23 S21 Ba1 89.73(12) . 2_645 ? C23 S21 Ba1 88.44(12) . . ? Ba1 S21 Ba1 174.79(4) 2_645 . ? C23 S22 Ba1 88.20(12) . 2_645 ? C23 S22 Ba1 98.82(11) . 4_566 ? Ba1 S22 Ba1 103.61(2) 2_645 4_566 ? C23 O24 C25 121.8(3) . . ? C23 O24 Ba1 104.37(19) . . ? C25 O24 Ba1 127.1(2) . . ? O24 C23 S22 122.7(2) . . ? O24 C23 S21 113.0(2) . . ? S22 C23 S21 124.3(2) . . ? O24 C25 C26 108.7(3) . . ? _refine_diff_density_max 0.500 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.101 #=END data_sy170 # CIF file for cpd 6, paper ref 8/02681E _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C23 H54 Ca O7 S4' _chemical_formula_weight 610.98 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1- loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.611(2) _cell_length_b 12.741(3) _cell_length_c 16.012(3) _cell_angle_alpha 92.33(2) _cell_angle_beta 103.74(2) _cell_angle_gamma 112.00(2) _cell_volume 1747.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.56mm _exptl_crystal_size_mid 0.50mm _exptl_crystal_size_min 0.48mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method ? _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.451 _exptl_absorpt_correction_type 'Psi scan' _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 0.811 _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.98 _diffrn_reflns_number 7325 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6123 _reflns_number_observed 4433 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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 w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+0.6910P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6119 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_obs 0.0402 _refine_ls_wR_factor_all 0.0925 _refine_ls_wR_factor_obs 0.0731 _refine_ls_goodness_of_fit_all 1.026 _refine_ls_goodness_of_fit_obs 1.066 _refine_ls_restrained_S_all 1.137 _refine_ls_restrained_S_obs 1.066 _refine_ls_shift/esd_max -0.163 _refine_ls_shift/esd_mean 0.009 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ca Ca 0.08742(6) 0.18974(4) 0.18841(3) 0.02450(13) Uani 1 d . . S1A S -0.21017(8) 0.00863(6) 0.18743(5) 0.0396(2) Uani 1 d . . S2A S 0.02104(8) -0.04303(5) 0.11978(5) 0.0339(2) Uani 1 d . . C3A C -0.1464(3) -0.0845(2) 0.1500(2) 0.0269(6) Uani 1 d . . O4A O -0.2228(2) -0.19773(14) 0.14191(12) 0.0345(4) Uani 1 d . . C5A C -0.3682(3) -0.2482(2) 0.1668(2) 0.0366(7) Uani 1 d . . H5A H -0.4334(3) -0.2030(2) 0.1496(2) 0.044 Uiso 1 calc R . C6A C -0.4492(4) -0.3666(2) 0.1154(2) 0.0616(10) Uani 1 d . . H6A1 H -0.5506(12) -0.4052(7) 0.1270(11) 0.092 Uiso 1 calc R . H6A2 H -0.3849(13) -0.4105(7) 0.1326(11) 0.092 Uiso 1 calc R . H6A3 H -0.4647(24) -0.3610(3) 0.0533(2) 0.092 Uiso 1 calc R . C7A C -0.3337(4) -0.2499(3) 0.2630(2) 0.0593(9) Uani 1 d . . H7A1 H -0.4317(4) -0.2857(17) 0.2788(3) 0.089 Uiso 1 calc R . H7A2 H -0.2776(23) -0.1714(3) 0.2934(2) 0.089 Uiso 1 calc R . H7A3 H -0.2693(21) -0.2938(16) 0.2796(3) 0.089 Uiso 1 calc R . S1B S -0.05068(8) 0.30625(6) 0.27982(5) 0.0387(2) Uani 1 d . . S2B S 0.22311(8) 0.44365(6) 0.22068(5) 0.0355(2) Uani 1 d . . C3B C 0.0818(3) 0.4328(2) 0.2680(2) 0.0270(6) Uani 1 d . . O4B O 0.0613(2) 0.52322(14) 0.29921(12) 0.0345(4) Uani 1 d . . C5B C 0.1660(3) 0.6401(2) 0.2953(2) 0.0351(6) Uani 1 d . . H5B H 0.2063(3) 0.6410(2) 0.2431(2) 0.042 Uiso 1 calc R . C6B C 0.2992(3) 0.6800(2) 0.3759(2) 0.0487(8) Uani 1 d . . H6B1 H 0.3707(12) 0.7580(7) 0.3742(6) 0.073 Uiso 1 calc R . H6B2 H 0.3549(14) 0.6290(10) 0.3794(7) 0.073 Uiso 1 calc R . H6B3 H 0.2593(4) 0.6791(16) 0.4269(2) 0.073 Uiso 1 calc R . C7B C 0.0665(4) 0.7088(2) 0.2863(2) 0.0486(8) Uani 1 d . . H7B1 H 0.0387(19) 0.7162(14) 0.3406(5) 0.073 Uiso 1 calc R . H7B2 H -0.0287(11) 0.6698(9) 0.2388(9) 0.073 Uiso 1 calc R . H7B3 H 0.1247(9) 0.7849(6) 0.2735(13) 0.073 Uiso 1 calc R . O1C O 0.0077(2) 0.21691(15) 0.04361(11) 0.0360(4) Uani 1 d . . C2C C -0.0444(3) 0.3027(2) 0.0089(2) 0.0419(7) Uani 1 d . . H2C H -0.0494(3) 0.3500(2) 0.0586(2) 0.050 Uiso 1 calc R . C3C C -0.2050(4) 0.2475(3) -0.0515(2) 0.0734(11) Uani 1 d . . H3C1 H -0.2426(12) 0.3066(3) -0.0704(13) 0.110 Uiso 1 calc R . H3C2 H -0.2751(8) 0.1963(17) -0.0215(6) 0.110 Uiso 1 calc R . H3C3 H -0.2024(7) 0.2034(18) -0.1023(8) 0.110 Uiso 1 calc R . C4C C 0.0729(4) 0.3798(3) -0.0321(2) 0.0616(10) Uani 1 d . . H4C1 H 0.0364(13) 0.4371(12) -0.0568(13) 0.092 Uiso 1 calc R . H4C2 H 0.0858(20) 0.3344(4) -0.0783(10) 0.092 Uiso 1 calc R . H4C3 H 0.1731(8) 0.4183(14) 0.0119(4) 0.092 Uiso 1 calc R . O1D O 0.3382(2) 0.2155(2) 0.17448(11) 0.0348(4) Uani 1 d . . C2D C 0.4095(3) 0.2381(3) 0.1046(2) 0.0405(7) Uani 1 d . . H2D H 0.3442(3) 0.2642(3) 0.0588(2) 0.049 Uiso 1 calc R . C3D C 0.5688(4) 0.3333(3) 0.1367(2) 0.0695(11) Uani 1 d . . H3D1 H 0.6363(9) 0.3082(8) 0.1799(12) 0.104 Uiso 1 calc R . H3D2 H 0.5601(5) 0.4003(7) 0.1634(14) 0.104 Uiso 1 calc R . H3D3 H 0.6139(12) 0.3532(14) 0.0878(4) 0.104 Uiso 1 calc R . C4D C 0.4138(4) 0.1303(3) 0.0653(2) 0.0628(10) Uani 1 d . . H4D1 H 0.4514(25) 0.1446(6) 0.0134(9) 0.094 Uiso 1 calc R . H4D2 H 0.3086(6) 0.0696(6) 0.0492(13) 0.094 Uiso 1 calc R . H4D3 H 0.4840(21) 0.1066(11) 0.1077(6) 0.094 Uiso 1 calc R . O1E O 0.2125(2) 0.15888(15) 0.32497(11) 0.0332(4) Uani 1 d . . C2E C 0.1542(3) 0.1230(2) 0.3987(2) 0.0354(6) Uani 1 d . . H2E H 0.0604(3) 0.1411(2) 0.3948(2) 0.042 Uiso 1 calc R . C3E C 0.1046(4) -0.0047(2) 0.3960(2) 0.0512(8) Uani 1 d . . H3E1 H 0.1962(5) -0.0238(3) 0.4037(13) 0.077 Uiso 1 calc R . H3E2 H 0.0301(18) -0.0437(3) 0.3397(5) 0.077 Uiso 1 calc R . H3E3 H 0.0551(21) -0.0297(4) 0.4427(8) 0.077 Uiso 1 calc R . C4E C 0.2752(4) 0.1887(3) 0.4808(2) 0.0576(9) Uani 1 d . . H4E1 H 0.2328(9) 0.1678(14) 0.5305(2) 0.086 Uiso 1 calc R . H4E2 H 0.3050(19) 0.2708(3) 0.4790(6) 0.086 Uiso 1 calc R . H4E3 H 0.3671(11) 0.1703(14) 0.4867(7) 0.086 Uiso 1 calc R . O1F O 0.5081(2) 0.17715(14) 0.32860(12) 0.0343(4) Uani 1 d . . C2F C 0.5743(3) 0.0941(2) 0.3195(2) 0.0342(6) Uani 1 d . . H2F H 0.6386(3) 0.1170(2) 0.2774(2) 0.041 Uiso 1 calc R . C3F C 0.6776(4) 0.0910(3) 0.4043(2) 0.0677(10) Uani 1 d . . H3F1 H 0.7250(22) 0.0367(15) 0.3961(4) 0.101 Uiso 1 calc R . H3F2 H 0.6158(7) 0.0668(19) 0.4460(5) 0.101 Uiso 1 calc R . H3F3 H 0.7597(16) 0.1674(6) 0.4266(8) 0.101 Uiso 1 calc R . C4F C 0.4411(4) -0.0182(2) 0.2813(2) 0.0539(9) Uani 1 d . . H4F1 H 0.4817(4) -0.0750(5) 0.2678(12) 0.081 Uiso 1 calc R . H4F2 H 0.3743(14) -0.0091(5) 0.2279(7) 0.081 Uiso 1 calc R . H4F3 H 0.3801(14) -0.0441(9) 0.3231(6) 0.081 Uiso 1 calc R . O1G O -0.2490(2) 0.3772(2) 0.39380(13) 0.0410(5) Uani 1 d . . C2G C -0.2602(3) 0.4864(2) 0.3891(2) 0.0376(7) Uani 1 d . . H2G H -0.2519(3) 0.5096(2) 0.3310(2) 0.045 Uiso 1 calc R . C3G C -0.1311(3) 0.5751(2) 0.4589(2) 0.0492(8) Uani 1 d . . H3G1 H -0.1367(14) 0.6498(4) 0.4533(8) 0.074 Uiso 1 calc R . H3G2 H -0.0303(4) 0.5787(12) 0.4530(8) 0.074 Uiso 1 calc R . H3G3 H -0.1421(13) 0.5545(9) 0.5160(2) 0.074 Uiso 1 calc R . C4G C -0.4186(3) 0.4699(3) 0.3984(2) 0.0588(9) Uani 1 d . . H4G1 H -0.4322(10) 0.5423(5) 0.3949(14) 0.088 Uiso 1 calc R . H4G2 H -0.4281(10) 0.4452(18) 0.4547(6) 0.088 Uiso 1 calc R . H4G3 H -0.4990(4) 0.4116(13) 0.3516(8) 0.088 Uiso 1 calc R . H1E H 0.2990 0.1384 0.3339 0.088 Uiso 1 d . . H1D H 0.4051 0.1982 0.2218 0.088 Uiso 1 d . . H1C H -0.0017 0.1619 -0.0080 0.088 Uiso 1 d . . H1F H 0.5906 0.2384 0.3524 0.088 Uiso 1 d . . H1G H -0.1810 0.3785 0.3648 0.088 Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.0259(3) 0.0243(3) 0.0256(3) 0.0004(2) 0.0086(2) 0.0119(2) S1A 0.0329(4) 0..0315(4) 0.0576(5) -0.0051(3) 0.0205(4) 0.0125(3) S2A 0.0346(4) 0.0265(3) 0.0441(4) -0.0024(3) 0.0212(3) 0.0102(3) C3A 0.0312(14) 0.0277(14) 0.0230(13) 0.0022(11) 0.0085(11) 0.0124(12) O4A 0.0364(11) 0.0251(9) 0.0475(12) 0.0071(8) 0.0228(9) 0.0112(8) C5A 0.030(2) 0.0338(15) 0.049(2) 0.0127(13) 0.0208(14) 0.0098(13) C6A 0.061(2) 0.036(2) 0.079(3) 0.010(2) 0.032(2) 0.001(2) C7A 0.056(2) 0.076(2) 0.053(2) 0.027(2) 0.028(2) 0.024(2) S1B 0.0364(4) 0.0239(3) 0.0606(5) -0.0006(3) 0.0272(4) 0.0094(3) S2B 0.0347(4) 0.0294(4) 0.0444(4) -0.0007(3) 0.0206(3) 0.0094(3) C3B 0.0275(14) 0.0269(13) 0.0259(14) -0.0010(11) 0.0051(11) 0.0120(12) O4B 0.0396(11) 0.0238(9) 0.0457(11) 0.0001(8) 0.0219(9) 0.0127(8) C5B 0.039(2) 0.0225(13) 0.044(2) 0.0055(12) 0.0170(14) 0.0094(12) C6B 0.046(2) 0.036(2) 0.055(2) 0.0026(14) 0.008(2) 0.0091(15) C7B 0.058(2) 0.034(2) 0.061(2) 0.0089(15) 0.020(2) 0.023(2) O1C 0.0515(12) 0.0352(10) 0.0270(10) 0.0004(8) 0.0073(9) 0.0259(9) C2C 0.057(2) 0.043(2) 0.035(2) 0.0008(13) 0.0080(15) 0.033(2) C3C 0.062(2) 0.092(3) 0.072(3) -0.005(2) -0.004(2) 0.052(2) C4C 0.094(3) 0.046(2) 0.056(2) 0.015(2) 0.029(2) 0.034(2) O1D 0.0312(10) 0.0479(11) 0.0334(10) 0.0101(9) 0.0134(9) 0.0213(9) C2D 0.032(2) 0.062(2) 0.035(2) 0.0186(14) 0.0157(13) 0.0214(15) C3D 0.055(2) 0.070(2) 0.079(3) 0.029(2) 0.032(2) 0.009(2) C4D 0.065(2) 0.084(3) 0.047(2) -0.002(2) 0.026(2) 0.031(2) O1E 0.0338(10) 0.0452(11) 0.0292(10) 0.0092(8) 0.0131(8) 0.0217(9) C2E 0.037(2) 0.048(2) 0.031(2) 0.0082(13) 0.0176(13) 0.0230(14) C3E 0.055(2) 0.050(2) 0.042(2) 0.0096(15) 0.016(2) 0.011(2) C4E 0.074(2) 0.056(2) 0.035(2) -0.005(2) 0.018(2) 0.016(2) O1F 0.0253(10) 0.0323(10) 0.0463(12) 0.0021(9) 0.0083(9) 0.0140(8) C2F 0.0308(15) 0.0336(15) 0.046(2) 0.0077(13) 0.0145(13) 0.0185(13) C3F 0.075(3) 0.072(2) 0.064(2) 0.014(2) 0.000(2) 0.050(2) C4F 0.045(2) 0.029(2) 0.089(3) 0.004(2) 0.024(2) 0.0120(14) O1G 0.0374(11) 0.0361(11) 0.0536(13) -0.0030(9) 0.0185(10) 0.0164(9) C2G 0.039(2) 0.038(2) 0.038(2) 0.0033(13) 0.0094(14) 0.0181(14) C3G 0.047(2) 0.037(2) 0.057(2) -0.0017(15) 0.011(2) 0.0124(15) C4G 0.041(2) 0.053(2) 0.086(3) -0.002(2) 0.012(2) 0.028(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 Ca O1C 2.346(2) . ? Ca O1E 2.357(2) . ? Ca O1D 2.374(2) . ? Ca S1B 2.8862(9) . ? Ca S2A 2.8974(11) . ? Ca S1A 2.9218(11) . ? Ca S2B 2.9694(11) . ? S1A C3A 1.675(2) . ? S2A C3A 1.690(3) . ? C3A O4A 1..335(3) . ? O4A C5A 1.462(3) . ? C5A C7A 1.498(4) . ? C5A C6A 1.507(4) . ? C5A H5A 1.00 . ? C6A H6A1 0.98 . ? C6A H6A2 0.98 . ? C6A H6A3 0.98 . ? C7A H7A1 0.98 . ? C7A H7A2 0.98 . ? C7A H7A3 0.98 . ? S1B C3B 1.691(3) . ? S2B C3B 1.671(3) . ? C3B O4B 1.337(3) . ? O4B C5B 1.466(3) . ? C5B C6B 1.496(4) . ? C5B C7B 1.507(4) . ? C5B H5B 1.00 . ? C6B H6B1 0.98 . ? C6B H6B2 0.98 . ? C6B H6B3 0.98 . ? C7B H7B1 0.98 . ? C7B H7B2 0.98 . ? C7B H7B3 0.98 . ? O1C C2C 1.442(3) . ? O1C H1C 1.026(2) . ? C2C C3C 1.495(4) . ? C2C C4C 1.498(4) . ? C2C H2C 1.00 . ? C3C H3C1 0.98 . ? C3C H3C2 0.98 . ? C3C H3C3 0.98 . ? C4C H4C1 0.98 . ? C4C H4C2 0.98 . ? C4C H4C3 0.98 . ? O1D C2D 1.431(3) . ? O1D H1D 0.961(2) . ? C2D C4D 1.506(4) . ? C2D C3D 1.505(4) . ? C2D H2D 1.00 . ? C3D H3D1 0.98 . ? C3D H3D2 0.98 . ? C3D H3D3 0.98 . ? C4D H4D1 0.98 . ? C4D H4D2 0.98 . ? C4D H4D3 0.98 . ? O1E C2E 1.443(3) . ? O1E H1E 0.943(2) . ? C2E C4E 1.495(4) .. ? C2E C3E 1.510(4) . ? C2E H2E 1.00 . ? C3E H3E1 0.98 . ? C3E H3E2 0.98 . ? C3E H3E3 0.98 . ? C4E H4E1 0.98 . ? C4E H4E2 0.98 . ? C4E H4E3 0.98 . ? O1F C2F 1.443(3) . ? O1F H1F 0.867(2) . ? C2F C3F 1.491(4) . ? C2F C4F 1.499(4) . ? C2F H2F 1.00 . ? C3F H3F1 0.98 . ? C3F H3F2 0.98 . ? C3F H3F3 0.98 . ? C4F H4F1 0.98 . ? C4F H4F2 0.98 . ? C4F H4F3 0.98 . ? O1G C2G 1.438(3) . ? O1G H1G 0.884(2) . ? C2G C3G 1.501(4) . ? C2G C4G 1.501(4) . ? C2G H2G 1.00 . ? C3G H3G1 0.98 . ? C3G H3G2 0.98 . ? C3G H3G3 0.98 . ? C4G H4G1 0.98 . ? C4G H4G2 0.98 . ? C4G H4G3 0.98 . ? 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 O1C Ca O1E 167.77(6) . . ? O1C Ca O1D 91.18(7) . . ? O1E Ca O1D 76.91(6) . . ? O1C Ca S1B 103.75(5) . . ? O1E Ca S1B 87.30(5) . . ? O1D Ca S1B 138.48(5) . . ? O1C Ca S2A 86.40(5) . . ? O1E Ca S2A 88.92(5) . . ? O1D Ca S2A 81.02(5) . . ? S1B Ca S2A 137.51(3) . . ? O1C Ca S1A 95.50(6) . . ? O1E Ca S1A 92.10(5) . . ? O1D Ca S1A 140.80(5) . . ? S1B Ca S1A 76.85(3) . . ? S2A Ca S1A 61.01(3) . . ? O1C Ca S2B 83.48(5) . . ? O1E Ca S2B 97.74(5) . . ? O1D Ca S2B 83.45(5) . . ? S1B Ca S2B 60.68(3) . . ? S2A Ca S2B 161.26(3) . . ? S1A Ca S2B 135.65(3) . . ? C3A S1A Ca 87.56(9) . . ? C3A S2A Ca 88.10(9) . . ? O4A C3A S1A 123.0(2) . . ? O4A C3A S2A 114.3(2) . . ? S1A C3A S2A 122.76(15) . . ? C3A O4A C5A 121.4(2) . . ? O4A C5A C7A 110.1(2) . . ? O4A C5A C6A 104.6(2) . . ? C7A C5A C6A 112.6(3) . . ? O4A C5A H5A 109.80(13) . . ? C7A C5A H5A 109.8(2) . . ? C6A C5A H5A 109.8(2) . . ? C5A C6A H6A1 109.5(2) . . ? C5A C6A H6A2 109.5(2) . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5(2) . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C5A C7A H7A1 109.5(2) . . ? C5A C7A H7A2 109.5(2) . . ? H7A1 C7A H7A2 109.5 . . ? C5A C7A H7A3 109.5(2) . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C3B S1B Ca 89.20(9) . . ? C3B S2B Ca 86.78(9) . . ? O4B C3B S2B 123.3(2) . . ? O4B C3B S1B 113.4(2) . . ? S2B C3B S1B 123.30(14) . . ? C3B O4B C5B 121.1(2) . . ? O4B C5B C6B 108.4(2) . . ? O4B C5B C7B 105.3(2) . . ? C6B C5B C7B 113.8(2) . . ? O4B C5B H5B 109.73(13) . . ? C6B C5B H5B 109.7(2) . . ? C7B C5B H5B 109.7(2) . . ? C5B C6B H6B1 109.5(2) . . ? C5B C6B H6B2 109.5(2) . . ? H6B1 C6B H6B2 109.5 . . ? C5B C6B H6B3 109.5(2) . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C5B C7B H7B1 109.5(2) . . ? C5B C7B H7B2 109.5(2) . . ? H7B1 C7B H7B2 109.5 . . ? C5B C7B H7B3 109.47(15) . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C2C O1C Ca 129.71(15) . . ? C2C O1C H1C 107.5(2) . . ? Ca O1C H1C 122.65(12) . . ? O1C C2C C3C 110.3(2) . . ? O1C C2C C4C 109.5(2) . . ? C3C C2C C4C 113.4(3) . . ? O1C C2C H2C 107.81(13) . . ? C3C C2C H2C 107.8(2) . . ? C4C C2C H2C 107.8(2) . . ? C2C C3C H3C1 109.5(2) . . ? C2C C3C H3C2 109.5(2) . . ? H3C1 C3C H3C2 109.5 . . ? C2C C3C H3C3 109.5(2) . . ? H3C1 C3C H3C3 109.5 . . ? H3C2 C3C H3C3 109.5 . . ? C2C C4C H4C1 109.5(2) . . ? C2C C4C H4C2 109.5(2) . . ? H4C1 C4C H4C2 109.5 . . ? C2C C4C H4C3 109.5(2) . . ? H4C1 C4C H4C3 109.5 . . ? H4C2 C4C H4C3 109.5 . . ? C2D O1D Ca 133.7(2) . . ? C2D O1D H1D 109.3(2) . . ? Ca O1D H1D 116.44(12) . . ? O1D C2D C4D 110.2(2) . . ? O1D C2D C3D 109.5(2) . . ? C4D C2D C3D 112.7(3) . . ? O1D C2D H2D 108.12(13) . . ? C4D C2D H2D 108.1(2) . . ? C3D C2D H2D 108.1(2) . . ? C2D C3D H3D1 109.5(2) . . ? C2D C3D H3D2 109.5(2) . . ? H3D1 C3D H3D2 109.5 . . ? C2D C3D H3D3 109.5(2) . . ? H3D1 C3D H3D3 109.5 . . ? H3D2 C3D H3D3 109.5 . . ? C2D C4D H4D1 109.5(2) . . ? C2D C4D H4D2 109.5(2) . . ? H4D1 C4D H4D2 109.5 . . ? C2D C4D H4D3 109.5(2) . . ? H4D1 C4D H4D3 109.5 . . ? H4D2 C4D H4D3 109.5 . . ? C2E O1E Ca 130.84(15) . . ? C2E O1E H1E 102.3(2) . . ? Ca O1E H1E 122.91(13) . . ? O1E C2E C4E 109.7(2) . . ? O1E C2E C3E 109.9(2) . . ? C4E C2E C3E 112.5(2) . . ? O1E C2E H2E 108.21(13) . . ? C4E C2E H2E 108.2(2) . . ? C3E C2E H2E 108.2(2) . . ? C2E C3E H3E1 109.5(2) . . ? C2E C3E H3E2 109.5(2) . . ? H3E1 C3E H3E2 109.5 . . ? C2E C3E H3E3 109.5(2) . . ? H3E1 C3E H3E3 109.5 . . ? H3E2 C3E H3E3 109.5 . . ? C2E C4E H4E1 109.5(2) . . ? C2E C4E H4E2 109.5(2) . . ? H4E1 C4E H4E2 109.5 . . ? C2E C4E H4E3 109.5(2) . . ? H4E1 C4E H4E3 109.5 . . ? H4E2 C4E H4E3 109.5 . . ? C2F O1F H1F 101.9(2) . . ? O1F C2F C3F 110.9(2) . . ? O1F C2F C4F 107.1(2) . . ? C3F C2F C4F 113.6(3) . . ? O1F C2F H2F 108.37(13) . . ? C3F C2F H2F 108.4(2) . . ? C4F C2F H2F 108.4(2) . . ? C2F C3F H3F1 109.5(2) . . ? C2F C3F H3F2 109.5(2) . . ? H3F1 C3F H3F2 109.5 . . ? C2F C3F H3F3 109.5(2) . . ? H3F1 C3F H3F3 109.5 . . ? H3F2 C3F H3F3 109.5 . . ? C2F C4F H4F1 109.47(15) . . ? C2F C4F H4F2 109.5(2) . . ? H4F1 C4F H4F2 109.5 . . ? C2F C4F H4F3 109.5(2) . . ? H4F1 C4F H4F3 109.5 . . ? H4F2 C4F H4F3 109.5 . . ? C2G O1G H1G 104.9(2) . . ? O1G C2G C3G 110.2(2) . . ? O1G C2G C4G 106.5(2) . . ? C3G C2G C4G 112.3(3) . . ? O1G C2G H2G 109.27(14) . . ? C3G C2G H2G 109.3(2) . . ? C4G C2G H2G 109.3(2) . . ? C2G C3G H3G1 109.5(2) . . ? C2G C3G H3G2 109.5(2) . . ? H3G1 C3G H3G2 109.5 . . ? C2G C3G H3G3 109.5(2) . . ? H3G1 C3G H3G3 109.5 . . ? H3G2 C3G H3G3 109.5 . . ? C2G C4G H4G1 109.5(2) . . ? C2G C4G H4G2 109.5(2) . . ? H4G1 C4G H4G2 109.5 . . ? C2G C4G H4G3 109.5(2) . . ? H4G1 C4G H4G3 109.5 . . ? H4G2 C4G H4G3 109.5 . . ? _refine_diff_density_max 0.248 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.049