# Copyright The Royal Society of Chemistry, 1998 data_sy174 # Compound 3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H62 Mg O10 S2' _chemical_formula_weight 623.19 _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' 'Mg' 'Mg' 0.0486 0.0363 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.332(2) _cell_length_b 14.535(2) _cell_length_c 11.538(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.800(9) _cell_angle_gamma 90.00 _cell_volume 1896.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 4.90 _cell_measurement_theta_max 12.47 _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24mm _exptl_crystal_size_mid 0.40mm _exptl_crystal_size_min 0.50mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_method ? _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 0.200 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.982 _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_% 5.55 _diffrn_reflns_number 7028 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3342 _reflns_number_observed 2048 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 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^)+(0.0826P)^2^+1.0358P] 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 3339 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1094 _refine_ls_R_factor_obs 0.0631 _refine_ls_wR_factor_all 0.1836 _refine_ls_wR_factor_obs 0.1538 _refine_ls_goodness_of_fit_all 1.017 _refine_ls_goodness_of_fit_obs 1.122 _refine_ls_restrained_S_all 1.036 _refine_ls_restrained_S_obs 1.122 _refine_ls_shift/esd_max 0.010 _refine_ls_shift/esd_mean 0.001 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 Mg Mg 0.0000 0.0000 0.0000 0.0325(4) Uani 1 d S . O1A O 0.1179(2) -0.02392(15) 0.1404(2) 0.0366(6) Uani 1 d . . S1A S 0.13645(10) -0.19980(7) 0.19943(10) 0.0552(4) Uani 1 d . . C2A C 0.1654(3) -0.0842(2) 0.2033(3) 0.0356(8) Uani 1 d . . O3A O 0.2481(2) -0.0612(2) 0.2857(2) 0.0437(7) Uani 1 d . . C5A C 0.2879(3) 0.0343(2) 0.2930(3) 0.0402(9) Uani 1 d . . H5A H 0.2183(3) 0.0765(2) 0.2829(3) 0.048 Uiso 1 calc R . C6A C 0.3710(4) 0.0520(3) 0.2005(5) 0.0696(14) Uani 1 d . . H6A1 H 0.3965(23) 0.1164(7) 0.2041(19) 0.104 Uiso 1 calc R . H6A2 H 0.3308(10) 0.0395(22) 0.1243(5) 0.104 Uiso 1 calc R . H6A3 H 0.4401(14) 0.0118(16) 0.2123(17) 0.104 Uiso 1 calc R . C7A C 0.3447(5) 0.0436(3) 0.4137(4) 0.086(2) Uani 1 d . . H7A1 H 0.3738(31) 0.1066(8) 0.4255(12) 0.129 Uiso 1 calc R . H7A2 H 0.4110(22) 0.0005(19) 0.4241(12) 0.129 Uiso 1 calc R . H7A3 H 0.2864(10) 0.0299(26) 0.4703(4) 0.129 Uiso 1 calc R . O1B O 0.0482(2) 0.1363(2) -0.0103(2) 0.0450(7) Uani 1 d . . C2B C 0.1184(3) 0.2016(2) 0.0584(3) 0.0460(10) Uani 1 d . . H2B H 0.1754(3) 0.1668(2) 0.1118(3) 0.055 Uiso 1 calc R . C3B C 0.0419(5) 0.2591(3) 0.1302(4) 0.0697(14) Uani 1 d . . H3B1 H 0.0917(5) 0.2992(16) 0.1813(21) 0.104 Uiso 1 calc R . H3B2 H -0.0053(22) 0.2190(3) 0.1774(21) 0.104 Uiso 1 calc R . H3B3 H -0.0109(20) 0.2969(17) 0.0791(4) 0.104 Uiso 1 calc R . C4B C 0.1878(4) 0.2604(3) -0.0203(4) 0.0749(15) Uani 1 d . . H4B1 H 0.2387(23) 0.3026(17) 0.0266(5) 0.112 Uiso 1 calc R . H4B2 H 0.1331(4) 0.2960(18) -0.0722(21) 0.112 Uiso 1 calc R . H4B3 H 0.2367(23) 0.2210(4) -0.0666(22) 0.112 Uiso 1 calc R . O1C O 0.1298(2) -0.0345(2) -0.1099(2) 0.0491(7) Uani 1 d . . C2C C 0.1550(4) 0.0061(3) -0.2192(3) 0.0493(10) Uani 1 d . . H2C H 0.1119(4) 0.0661(3) -0.2265(3) 0.059 Uiso 1 calc R . C3C C 0.1090(5) -0.0550(4) -0.3173(4) 0.0768(15) Uani 1 d . . H3C1 H 0.1224(29) -0.0254(12) -0.3916(4) 0.115 Uiso 1 calc R . H3C2 H 0.0241(8) -0.0652(20) -0.3118(18) 0.115 Uiso 1 calc R . H3C3 H 0.1506(23) -0.1141(10) -0.3124(18) 0.115 Uiso 1 calc R . C4C C 0.2847(4) 0.0255(4) -0.2226(5) 0.080(2) Uani 1 d . . H4C1 H 0.2996(6) 0.0567(22) -0.2955(14) 0.119 Uiso 1 calc R . H4C2 H 0.3288(5) -0.0325(4) -0.2176(31) 0.119 Uiso 1 calc R . H4C3 H 0.3106(7) 0.0650(20) -0.1568(18) 0.119 Uiso 1 calc R . O1D O 0.2561(3) -0.1883(2) -0.0505(3) 0.0850(11) Uani 1 d . . C2D C 0.3780(4) -0.2108(3) -0.0586(5) 0.0708(14) Uani 1 d . . H2D H 0.3993(4) -0.1968(3) -0.1395(5) 0.085 Uiso 1 calc R . C3D C 0.4521(6) -0.1530(5) 0.0218(6) 0.115(2) Uani 1 d . . H3D1 H 0.5357(6) -0.1666(25) 0.0129(31) 0.172 Uiso 1 calc R . H3D2 H 0.4332(32) -0.1661(25) 0.1019(6) 0.172 Uiso 1 calc R . H3D3 H 0.4365(32) -0.0880(5) 0.0043(28) 0.172 Uiso 1 calc R . C4D C 0.3992(7) -0.3083(5) -0.0374(8) 0.142(3) Uani 1 d . . H4D1 H 0.4825(14) -0.3224(10) -0.0475(55) 0.214 Uiso 1 calc R . H4D2 H 0.3489(42) -0.3446(5) -0.0925(37) 0.214 Uiso 1 calc R . H4D3 H 0.3805(54) -0.3235(10) 0.0421(20) 0.214 Uiso 1 calc R . H1B H -0.0056 0.1730 -0.0600 0.171 Uiso 1 d . . H1C H 0.1886 -0.0895 -0.1000 0.171 Uiso 1 d . . H1D H 0.2307 -0.1974 0.0400 0.171 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 Mg 0.0331(9) 0.0271(8) 0.0357(9) 0.0048(7) -0.0104(7) -0.0031(7) O1A 0.0384(14) 0.0290(13) 0.0402(14) 0.0071(11) -0.0140(11) -0.0020(11) S1A 0.0634(7) 0.0310(5) 0.0667(7) 0.0149(5) -0.0296(6) -0.0094(5) C2A 0.032(2) 0.034(2) 0.039(2) 0.004(2) -0.008(2) -0.001(2) O3A 0.0452(15) 0.0333(13) 0.049(2) 0.0077(12) -0.0236(13) -0.0044(12) C5A 0.039(2) 0.029(2) 0.050(2) -0.003(2) -0.013(2) 0.000(2) C6A 0.055(3) 0.045(3) 0.111(4) -0.012(3) 0.020(3) -0.008(2) C7A 0.124(5) 0.059(3) 0.068(3) -0.003(2) -0.051(3) -0.012(3) O1B 0.051(2) 0.0268(13) 0.054(2) 0.0047(12) -0.0231(13) -0.0070(12) C2B 0.044(2) 0.031(2) 0.058(2) 0.003(2) -0.027(2) -0.010(2) C3B 0.080(3) 0.060(3) 0.068(3) -0.018(2) -0.002(3) -0.024(3) C4B 0.070(3) 0.070(3) 0.085(4) -0.008(3) 0.000(3) -0.036(3) O1C 0.048(2) 0.054(2) 0.046(2) 0.0145(13) 0.0042(13) 0.0109(13) C2C 0.049(2) 0.049(2) 0.050(2) 0.010(2) 0.004(2) 0.000(2) C3C 0.088(4) 0.085(4) 0.058(3) -0.007(3) 0.010(3) -0.016(3) C4C 0.054(3) 0.103(4) 0.082(4) 0.026(3) 0.005(3) -0.008(3) O1D 0.056(2) 0.088(3) 0.111(3) 0.029(2) 0.007(2) 0.025(2) C2D 0.056(3) 0.073(3) 0.081(3) -0.004(3) -0.008(3) 0.014(3) C3D 0.093(5) 0.142(6) 0.109(5) -0.036(5) 0.012(4) -0.032(4) C4D 0.121(6) 0.089(5) 0.219(10) -0.020(5) 0.026(6) 0.018(5) _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 Mg O1B 2.060(2) 3 ? Mg O1B 2.060(2) . ? Mg O1A 2.060(2) . ? Mg O1A 2.060(2) 3 ? Mg O1C 2.067(3) . ? Mg O1C 2.067(3) 3 ? O1A C2A 1.238(4) . ? S1A C2A 1.712(4) . ? C2A O3A 1.333(4) . ? O3A C5A 1.459(4) . ? C5A C6A 1.492(6) . ? C5A C7A 1.501(5) . ? 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 . ? O1B C2B 1.442(4) . ? O1B H1B 0.970(2) . ? C2B C3B 1.494(6) . ? C2B C4B 1.507(6) . ? C2B H2B 1.00 . ? C3B H3B1 0.98 . ? C3B H3B2 0.98 . ? C3B H3B3 0.98 . ? C4B H4B1 0.98 . ? C4B H4B2 0.98 . ? C4B H4B3 0.98 . ? O1C C2C 1.438(5) . ? O1C H1C 1.041(3) . ? C2C C4C 1.500(6) . ? C2C C3C 1.505(6) . ? 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 1.429(6) . ? O1D H1D 1.109(4) . ? C2D C4D 1.455(8) . ? C2D C3D 1.472(7) . ? 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 . ? 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 O1B Mg O1B 180.0 3 . ? O1B Mg O1A 87.32(9) 3 . ? O1B Mg O1A 92.68(9) . . ? O1B Mg O1A 92.68(9) 3 3 ? O1B Mg O1A 87.32(9) . 3 ? O1A Mg O1A 180.0 . 3 ? O1B Mg O1C 90.24(11) 3 . ? O1B Mg O1C 89.76(11) . . ? O1A Mg O1C 89.46(10) . . ? O1A Mg O1C 90.54(10) 3 . ? O1B Mg O1C 89.76(11) 3 3 ? O1B Mg O1C 90.24(11) . 3 ? O1A Mg O1C 90.54(10) . 3 ? O1A Mg O1C 89.46(10) 3 3 ? O1C Mg O1C 180.0 . 3 ? C2A O1A Mg 144.5(2) . . ? O1A C2A O3A 119.9(3) . . ? O1A C2A S1A 127.2(3) . . ? O3A C2A S1A 112.9(2) . . ? C2A O3A C5A 118.7(3) . . ? O3A C5A C6A 109.3(3) . . ? O3A C5A C7A 104.6(3) . . ? C6A C5A C7A 113.3(4) . . ? O3A C5A H5A 109.8(2) . . ? C6A C5A H5A 109.8(2) . . ? C7A C5A H5A 109.8(3) . . ? 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(3) . . ? H7A1 C7A H7A2 109.5 . . ? C5A C7A H7A3 109.5(3) . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C2B O1B Mg 137.8(2) . . ? C2B O1B H1B 105.4(2) . . ? Mg O1B H1B 113.9(2) . . ? O1B C2B C3B 110.8(3) . . ? O1B C2B C4B 109.4(3) . . ? C3B C2B C4B 111.2(4) . . ? O1B C2B H2B 108.4(2) . . ? C3B C2B H2B 108.4(2) . . ? C4B C2B H2B 108.4(2) . . ? C2B C3B H3B1 109.5(2) . . ? C2B C3B H3B2 109.5(2) . . ? H3B1 C3B H3B2 109.5 . . ? C2B C3B H3B3 109.5(2) . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C2B C4B H4B1 109.5(2) . . ? C2B C4B H4B2 109.5(2) . . ? H4B1 C4B H4B2 109.5 . . ? C2B C4B H4B3 109.5(3) . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C2C O1C Mg 128.9(2) . . ? C2C O1C H1C 104.4(3) . . ? Mg O1C H1C 126.5(2) . . ? O1C C2C C4C 110.6(3) . . ? O1C C2C C3C 109.7(4) . . ? C4C C2C C3C 112.5(4) . . ? O1C C2C H2C 108.0(2) . . ? C4C C2C H2C 108.0(3) . . ? C3C C2C H2C 108.0(3) . . ? C2C C3C H3C1 109.5(3) . . ? C2C C3C H3C2 109.5(3) . . ? H3C1 C3C H3C2 109.5 . . ? C2C C3C H3C3 109.5(3) . . ? H3C1 C3C H3C3 109.5 . . ? H3C2 C3C H3C3 109.5 . . ? C2C C4C H4C1 109.5(2) . . ? C2C C4C H4C2 109.5(3) . . ? H4C1 C4C H4C2 109.5 . . ? C2C C4C H4C3 109.5(3) . . ? H4C1 C4C H4C3 109.5 . . ? H4C2 C4C H4C3 109..5 . . ? C2D O1D H1D 110.3(3) . . ? O1D C2D C4D 111.2(5) . . ? O1D C2D C3D 109.9(5) . . ? C4D C2D C3D 111.6(6) . . ? O1D C2D H2D 108.0(3) . . ? C4D C2D H2D 108.0(4) . . ? C3D C2D H2D 108.0(4) . . ? C2D C3D H3D1 109.5(3) . . ? C2D C3D H3D2 109.5(4) . . ? H3D1 C3D H3D2 109.5 . . ? C2D C3D H3D3 109.5(4) . . ? H3D1 C3D H3D3 109.5 . . ? H3D2 C3D H3D3 109.5 . . ? C2D C4D H4D1 109.5(4) . . ? C2D C4D H4D2 109.5(4) . . ? H4D1 C4D H4D2 109.5 . . ? C2D C4D H4D3 109.5(4) . . ? H4D1 C4D H4D3 109.5 . . ? H4D2 C4D H4D3 109.5 . . ? _refine_diff_density_max 0.609 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.057 #=END data_sx175 # Compound 4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H30 O6 S2 Sr' _chemical_formula_weight 446.12 _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' 'Sr' 'Sr' -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 17.283(3) _cell_length_b 15.544(5) _cell_length_c 15.769(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4236.3(23) _cell_formula_units_Z 8 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.56mm _exptl_crystal_size_mid 0.38mm _exptl_crystal_size_min 0.36mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method ? _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 2.764 _exptl_absorpt_correction_type 'Psi scans' _exptl_absorpt_correction_T_min 0.254 _exptl_absorpt_correction_T_max 0.356 _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_% 1.72 _diffrn_reflns_number 1964 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.09 _reflns_number_total 1890 _reflns_number_observed 1718 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 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^)+(0.0499P)^2^+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(9) _refine_ls_number_reflns 1889 _refine_ls_number_parameters 110 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_obs 0.0338 _refine_ls_wR_factor_all 0.0765 _refine_ls_wR_factor_obs 0.0735 _refine_ls_goodness_of_fit_all 1.039 _refine_ls_goodness_of_fit_obs 1.053 _refine_ls_restrained_S_all 1.042 _refine_ls_restrained_S_obs 1.053 _refine_ls_shift/esd_max -2.818 _refine_ls_shift/esd_mean 0.275 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 Sr Sr 0.0000 0.0000 0.26646(3) 0.02191(14) Uani 1 d S . S1A S -0.04423(7) 0.16810(7) 0.17778(8) 0.0377(3) Uani 1 d . . C2A C -0.1089(2) 0.1109(3) 0.1190(2) 0.0266(10) Uani 1 d . . O3A O -0.1571(2) 0.1390(2) 0.0704(2) 0.0338(7) Uani 1 d . . O4A O -0.1033(2) 0.0240(2) 0.1321(2) 0.0328(7) Uani 1 d . . C5A C -0.1521(3) -0.0322(3) 0.0787(3) 0.0369(11) Uani 1 d . . H5A H -0.1968(3) 0.0014(3) 0.0559(3) 0.044 Uiso 1 calc R . C6A C -0.1044(3) -0.0646(3) 0.0075(4) 0.0520(14) Uani 1 d . . H6A1 H -0.0626(14) -0.1007(21) 0.0298(4) 0.078 Uiso 1 calc R . H6A2 H -0.0822(19) -0.0159(3) -0.0236(15) 0.078 Uiso 1 calc R . H6A3 H -0.1368(6) -0.0988(21) -0.0308(14) 0.078 Uiso 1 calc R . C7A C -0.1810(3) -0.1013(4) 0.1363(4) 0.0545(15) Uani 1 d . . H7A1 H -0.2130(21) -0.1417(16) 0.1041(7) 0.082 Uiso 1 calc R . H7A2 H -0.2121(21) -0.0754(5) 0.1817(16) 0.082 Uiso 1 calc R . H7A3 H -0.1370(3) -0.1319(18) 0.1612(22) 0.082 Uiso 1 calc R . O1B O -0.0846(2) 0.0670(2) 0.3805(2) 0.0458(9) Uani 1 d . . H1B H -0.1045 0.0189 0.4153 0.069 Uiso 1 d . . C2B C -0.0813(3) 0.1435(3) 0.4299(3) 0.0448(13) Uani 1 d . . H2B H -0.0531(3) 0.1878(3) 0.3959(3) 0.054 Uiso 1 calc R . C3B C -0.0367(4) 0.1287(5) 0.5081(4) 0.090(2) Uani 1 d . . H3B1 H -0.0281(29) 0.1837(7) 0.5371(19) 0.135 Uiso 1 calc R . H3B2 H 0.0134(15) 0.1028(35) 0.4938(6) 0.135 Uiso 1 calc R . H3B3 H -0.0655(16) 0.0899(30) 0.5455(17) 0.135 Uiso 1 calc R . C4B C -0.1601(4) 0.1770(4) 0.4467(5) 0.081(2) Uani 1 d . . H4B1 H -0.1564(4) 0.2318(18) 0.4771(30) 0.122 Uiso 1 calc R . H4B2 H -0.1888(11) 0.1354(17) 0.4812(29) 0.122 Uiso 1 calc R . H4B3 H -0.1871(11) 0.1859(32) 0.3928(5) 0.122 Uiso 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 Sr 0.0226(2) 0.0176(2) 0.0255(2) 0.000 0.000 -0.0002(3) S1A 0.0394(7) 0.0253(6) 0.0484(7) 0.0022(5) -0.0177(6) 0.0018(5) C2A 0.026(2) 0.025(2) 0.029(2) 0.002(2) 0.005(2) 0.004(2) O3A 0.037(2) 0.028(2) 0.036(2) 0.0019(13) -0.013(2) 0.0069(15) O4A 0.034(2) 0.024(2) 0.041(2) -0.0013(12) -0.0149(15) 0.0023(13) C5A 0.037(3) 0.028(2) 0.045(3) 0.001(2) -0.014(2) -0.002(2) C6A 0.068(4) 0.045(3) 0.043(3) -0.009(3) 0.004(3) -0.010(3) C7A 0.050(3) 0.052(3) 0.061(3) 0.003(3) -0.007(3) -0.019(3) O1B 0.052(2) 0.032(2) 0.053(2) -0.011(2) 0.023(2) -0.007(2) C2B 0.056(3) 0.031(3) 0.048(3) -0.014(2) 0.013(3) -0.009(2) C3B 0.102(6) 0.092(5) 0.076(5) -0.023(5) -0.019(5) 0.014(5) C4B 0.062(4) 0.061(4) 0.121(6) -0.037(4) -0.002(4) 0.017(4) _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 Sr O3A 2.505(3) 3 ? Sr O3A 2.505(3) 16_445 ? Sr O1B 2.540(3) 2 ? Sr O1B 2.540(3) . ? Sr O4A 2.796(3) . ? Sr O4A 2.796(3) 2 ? Sr S1A 3.0607(13) . ? Sr S1A 3.0607(13) 2 ? S1A C2A 1.703(4) . ? C2A O3A 1.213(5) . ? C2A O4A 1.370(5) . ? O3A Sr 2.505(3) 11_454 ? O4A C5A 1.478(5) . ? C5A C6A 1.481(7) . ? C5A C7A 1.492(7) . ? 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 . ? O1B C2B 1.422(5) . ? O1B H1B 0.989(3) . ? C2B C3B 1.473(8) . ? C2B C4B 1.482(8) . ? C2B H2B 1.00 . ? C3B H3B1 0.98 . ? C3B H3B2 0.98 . ? C3B H3B3 0.98 . ? C4B H4B1 0.98 . ? C4B H4B2 0.98 . ? C4B H4B3 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 O3A Sr O3A 140.28(15) 3 16_445 ? O3A Sr O1B 70.92(11) 3 2 ? O3A Sr O1B 81.14(11) 16_445 2 ? O3A Sr O1B 81.14(11) 3 . ? O3A Sr O1B 70.92(11) 16_445 . ? O1B Sr O1B 89.9(2) 2 . ? O3A Sr O4A 125.10(9) 3 . ? O3A Sr O4A 86.56(10) 16_445 . ? O1B Sr O4A 163.43(9) 2 . ? O1B Sr O4A 96.57(11) . . ? O3A Sr O4A 86.56(10) 3 2 ? O3A Sr O4A 125.10(9) 16_445 2 ? O1B Sr O4A 96.57(11) 2 2 ? O1B Sr O4A 163.43(9) . 2 ? O4A Sr O4A 81.45(14) . 2 ? O3A Sr S1A 74.18(7) 3 . ? O3A Sr S1A 125.66(8) 16_445 . ? O1B Sr S1A 144.78(8) 2 . ? O1B Sr S1A 80.21(9) . . ? O4A Sr S1A 51.72(6) . . ? O4A Sr S1A 85.81(7) 2 . ? O3A Sr S1A 125.66(8) 3 2 ? O3A Sr S1A 74.18(7) 16_445 2 ? O1B Sr S1A 80.21(9) 2 2 ? O1B Sr S1A 144.78(8) . 2 ? O4A Sr S1A 85.81(7) . 2 ? O4A Sr S1A 51.72(6) 2 2 ? S1A Sr S1A 125.62(5) . 2 ? C2A S1A Sr 88.10(15) . . ? O3A C2A O4A 119.9(4) . . ? O3A C2A S1A 127.3(3) . . ? O4A C2A S1A 112.8(3) . . ? C2A O3A Sr 154.5(3) . 11_454 ? C2A O4A C5A 117.2(3) . . ? C2A O4A Sr 106.9(2) . . ? C5A O4A Sr 135.9(2) . . ? O4A C5A C6A 108.3(4) . . ? O4A C5A C7A 105.6(4) . . ? C6A C5A C7A 113.8(5) . . ? O4A C5A H5A 109.7(2) . . ? C6A C5A H5A 109.7(3) . . ? C7A C5A H5A 109.6(3) . . ? C5A C6A H6A1 109.6(3) . . ? C5A C6A H6A2 109.5(3) . . ? H6A1 C6A H6A2 109.4 . . ? C5A C6A H6A3 109.5(3) . . ? H6A1 C6A H6A3 109.4 . . ? H6A2 C6A H6A3 109.4 . . ? C5A C7A H7A1 109.4(3) . . ? C5A C7A H7A2 109.5(3) . . ? H7A1 C7A H7A2 109.5 . . ? C5A C7A H7A3 109.4(3) . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C2B O1B Sr 135.0(3) . . ? C2B O1B H1B 110.0(3) . . ? Sr O1B H1B 106.4(2) . . ? O1B C2B C3B 110.5(5) . . ? O1B C2B C4B 110.8(4) . . ? C3B C2B C4B 112.7(5) . . ? O1B C2B H2B 107.5(2) . . ? C3B C2B H2B 107.6(4) . . ? C4B C2B H2B 107.5(4) . . ? C2B C3B H3B1 109.5(4) . . ? C2B C3B H3B2 109.3(4) . . ? H3B1 C3B H3B2 109.5 . . ? C2B C3B H3B3 109.6(4) . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C2B C4B H4B1 109.5(3) . . ? C2B C4B H4B2 109.5(4) . . ? H4B1 C4B H4B2 109.5 . . ? C2B C4B H4B3 109.4(4) . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? _refine_diff_density_max 0.739 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.070