Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Dirk Volkmer' 'Marc Fricke' 'Norbert Mayr' _publ_contact_author_name 'Dirk Volkmer' _publ_contact_author_address ; Institut fur Anorganische Chemie II Universitat Ulm Fakultat fur Chemie Albert-Einstein-Allee 11 Ulm D-89081 GERMANY ; _publ_contact_author_email DIRK.VOLKMER@UNI-ULM.DE _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Crystal Structure Analysis of [Ca(O3SC18H37)2(DMSO)2], a Lamellar Coordination Polymer and its Relevance for Model Studies in Biomineralization ; data_casulf _database_code_depnum_ccdc_archive 'CCDC 611718' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H86 Ca O8 S4' _chemical_formula_weight 863.41 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 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 5.4085(4) _cell_length_b 8.1350(7) _cell_length_c 54.718(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.4900(10) _cell_angle_gamma 90.00 _cell_volume 2405.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 7724 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.96 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13005 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -69 _diffrn_reflns_limit_l_max 69 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.03 _reflns_number_total 5157 _reflns_number_gt 4600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0000P)^2^+16.0624P] 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 5157 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0997 _refine_ls_wR_factor_ref 0.2298 _refine_ls_wR_factor_gt 0.2274 _refine_ls_goodness_of_fit_ref 1.309 _refine_ls_restrained_S_all 1.309 _refine_ls_shift/su_max 0.000 _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 Ca1 Ca 1.0000 1.0000 0.0000 0.0149(3) Uani 1 2 d S . . S1 S 0.5075(2) 1.11062(15) 0.04149(2) 0.0161(3) Uani 1 1 d . . . O1 O 0.7015(7) 1.0214(5) 0.02916(7) 0.0271(9) Uani 1 1 d . . . O2 O 0.2892(6) 1.1370(4) 0.02520(6) 0.0215(8) Uani 1 1 d . . . O3 O 0.5954(7) 1.2595(5) 0.05321(7) 0.0272(9) Uani 1 1 d . . . C1 C 0.4141(9) 0.9796(7) 0.06524(9) 0.0209(10) Uani 1 1 d . . . H1A H 0.3493 0.8756 0.0581 0.025 Uiso 1 1 calc R . . H1B H 0.5591 0.9530 0.0762 0.025 Uiso 1 1 calc R . . C2 C 0.2148(11) 1.0603(8) 0.08006(10) 0.0311(13) Uani 1 1 d . . . H2A H 0.0626 1.0740 0.0695 0.037 Uiso 1 1 calc R . . H2B H 0.2717 1.1710 0.0853 0.037 Uiso 1 1 calc R . . C3 C 0.1542(13) 0.9597(8) 0.10260(11) 0.0380(15) Uani 1 1 d . . . H3A H 0.3085 0.9391 0.1125 0.046 Uiso 1 1 calc R . . H3B H 0.0855 0.8520 0.0973 0.046 Uiso 1 1 calc R . . C4 C -0.0328(13) 1.0476(10) 0.11841(11) 0.0457(18) Uani 1 1 d . . . H4A H 0.0307 1.1589 0.1225 0.055 Uiso 1 1 calc R . . H4B H -0.1904 1.0608 0.1087 0.055 Uiso 1 1 calc R . . C5 C -0.0840(15) 0.9583(11) 0.14199(13) 0.053(2) Uani 1 1 d . . . H5A H 0.0737 0.9449 0.1517 0.063 Uiso 1 1 calc R . . H5B H -0.1479 0.8471 0.1379 0.063 Uiso 1 1 calc R . . C6 C -0.2685(15) 1.0455(12) 0.15766(12) 0.058(2) Uani 1 1 d . . . H6A H -0.4286 1.0545 0.1483 0.069 Uiso 1 1 calc R . . H6B H -0.2083 1.1585 0.1611 0.069 Uiso 1 1 calc R . . C7 C -0.3113(17) 0.9592(13) 0.18187(14) 0.066(3) Uani 1 1 d . . . H7A H -0.3688 0.8457 0.1785 0.079 Uiso 1 1 calc R . . H7B H -0.1520 0.9522 0.1914 0.079 Uiso 1 1 calc R . . C8 C -0.4992(17) 1.0455(13) 0.19719(14) 0.070(3) Uani 1 1 d . . . H8A H -0.6595 1.0502 0.1878 0.084 Uiso 1 1 calc R . . H8B H -0.4437 1.1599 0.2003 0.084 Uiso 1 1 calc R . . C9 C -0.5382(18) 0.9612(13) 0.22178(14) 0.073(3) Uani 1 1 d . . . H9A H -0.5933 0.8467 0.2187 0.088 Uiso 1 1 calc R . . H9B H -0.3780 0.9567 0.2312 0.088 Uiso 1 1 calc R . . C10 C -0.7275(18) 1.0476(14) 0.23710(14) 0.076(3) Uani 1 1 d . . . H10A H -0.8872 1.0531 0.2276 0.092 Uiso 1 1 calc R . . H10B H -0.6715 1.1617 0.2403 0.092 Uiso 1 1 calc R . . C11 C -0.7679(18) 0.9623(14) 0.26146(14) 0.074(3) Uani 1 1 d . . . H11A H -0.8234 0.8481 0.2582 0.089 Uiso 1 1 calc R . . H11B H -0.6081 0.9570 0.2710 0.089 Uiso 1 1 calc R . . C12 C -0.9573(18) 1.0479(14) 0.27685(14) 0.075(3) Uani 1 1 d . . . H12A H -1.1171 1.0531 0.2674 0.090 Uiso 1 1 calc R . . H12B H -0.9019 1.1621 0.2801 0.090 Uiso 1 1 calc R . . C13 C -0.9979(17) 0.9633(13) 0.30117(14) 0.068(3) Uani 1 1 d . . . H13A H -1.0542 0.8492 0.2979 0.082 Uiso 1 1 calc R . . H13B H -0.8379 0.9575 0.3106 0.082 Uiso 1 1 calc R . . C14 C -1.1862(17) 1.0494(13) 0.31661(14) 0.067(3) Uani 1 1 d . . . H14A H -1.3465 1.0549 0.3072 0.080 Uiso 1 1 calc R . . H14B H -1.1303 1.1635 0.3199 0.080 Uiso 1 1 calc R . . C15 C -1.2250(16) 0.9637(12) 0.34097(13) 0.061(2) Uani 1 1 d . . . H15A H -1.2818 0.8498 0.3377 0.073 Uiso 1 1 calc R . . H15B H -1.0641 0.9573 0.3503 0.073 Uiso 1 1 calc R . . C16 C -1.4103(15) 1.0483(11) 0.35672(13) 0.057(2) Uani 1 1 d . . . H16A H -1.5723 1.0530 0.3476 0.068 Uiso 1 1 calc R . . H16B H -1.3551 1.1626 0.3599 0.068 Uiso 1 1 calc R . . C17 C -1.4433(15) 0.9629(11) 0.38097(12) 0.054(2) Uani 1 1 d . . . H17A H -1.2815 0.9593 0.3901 0.064 Uiso 1 1 calc R . . H17B H -1.4960 0.8481 0.3778 0.064 Uiso 1 1 calc R . . C18 C -1.6326(15) 1.0455(11) 0.39701(13) 0.053(2) Uani 1 1 d . . . H18A H -1.6426 0.9846 0.4124 0.079 Uiso 1 1 calc R . . H18B H -1.7952 1.0459 0.3884 0.079 Uiso 1 1 calc R . . H18C H -1.5810 1.1588 0.4005 0.079 Uiso 1 1 calc R . . S2 S 0.9270(2) 0.67481(16) 0.03969(2) 0.0236(3) Uani 1 1 d . . . O4 O 1.0918(6) 0.7560(4) 0.02116(7) 0.0235(8) Uani 1 1 d . . . C19 C 1.0805(10) 0.4906(7) 0.04903(11) 0.0284(12) Uani 1 1 d . . . H19A H 1.1217 0.4269 0.0346 0.043 Uiso 1 1 calc R . . H19B H 0.9717 0.4255 0.0591 0.043 Uiso 1 1 calc R . . H19C H 1.2327 0.5178 0.0585 0.043 Uiso 1 1 calc R . . C20 C 0.6792(10) 0.5863(8) 0.02186(12) 0.0368(15) Uani 1 1 d . . . H20A H 0.5696 0.6736 0.0154 0.055 Uiso 1 1 calc R . . H20B H 0.5857 0.5118 0.0321 0.055 Uiso 1 1 calc R . . H20C H 0.7456 0.5247 0.0082 0.055 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 Ca1 0.0121(6) 0.0136(6) 0.0196(7) 0.0031(5) 0.0051(5) 0.0007(5) S1 0.0131(5) 0.0171(6) 0.0186(6) 0.0020(5) 0.0053(4) -0.0004(5) O1 0.0239(19) 0.030(2) 0.028(2) 0.0056(16) 0.0150(15) 0.0084(16) O2 0.0207(18) 0.0215(19) 0.0224(18) 0.0012(15) 0.0019(14) 0.0006(15) O3 0.028(2) 0.0205(19) 0.033(2) -0.0002(16) 0.0005(16) -0.0075(16) C1 0.019(2) 0.023(3) 0.022(2) 0.004(2) 0.0091(19) 0.000(2) C2 0.031(3) 0.043(3) 0.021(3) 0.003(2) 0.015(2) 0.003(3) C3 0.045(4) 0.041(4) 0.030(3) 0.001(3) 0.021(3) -0.003(3) C4 0.044(4) 0.069(5) 0.026(3) -0.004(3) 0.021(3) -0.008(4) C5 0.057(5) 0.069(5) 0.036(4) 0.001(4) 0.028(3) -0.005(4) C6 0.054(5) 0.091(7) 0.030(3) -0.008(4) 0.025(3) -0.010(4) C7 0.070(6) 0.093(7) 0.038(4) -0.003(4) 0.038(4) -0.006(5) C8 0.071(6) 0.103(8) 0.040(4) -0.006(5) 0.039(4) -0.013(5) C9 0.085(6) 0.099(8) 0.040(4) -0.004(5) 0.042(4) -0.012(6) C10 0.082(6) 0.112(8) 0.039(4) -0.004(5) 0.040(4) -0.009(6) C11 0.076(6) 0.107(8) 0.042(4) -0.001(5) 0.039(4) -0.008(6) C12 0.080(6) 0.105(8) 0.044(4) 0.003(5) 0.045(4) 0.000(6) C13 0.076(6) 0.093(7) 0.040(4) -0.002(4) 0.038(4) -0.004(5) C14 0.072(6) 0.093(7) 0.039(4) 0.002(4) 0.035(4) -0.003(5) C15 0.067(5) 0.080(6) 0.038(4) -0.002(4) 0.030(4) -0.002(5) C16 0.061(5) 0.075(6) 0.036(4) 0.003(4) 0.030(3) 0.000(4) C17 0.060(5) 0.068(5) 0.035(4) 0.006(4) 0.026(3) 0.007(4) C18 0.057(5) 0.068(5) 0.035(4) 0.006(4) 0.024(3) 0.002(4) S2 0.0224(6) 0.0204(6) 0.0286(7) 0.0057(5) 0.0067(5) 0.0028(5) O4 0.0165(17) 0.0188(18) 0.036(2) 0.0098(16) 0.0068(15) 0.0028(14) C19 0.019(3) 0.023(3) 0.043(3) 0.011(2) 0.003(2) 0.001(2) C20 0.016(3) 0.037(4) 0.056(4) 0.021(3) -0.001(2) -0.005(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 Ca1 O2 2.325(4) 3_675 ? Ca1 O2 2.325(4) 1_655 ? Ca1 O1 2.325(3) . ? Ca1 O1 2.325(3) 3_775 ? Ca1 O4 2.340(3) 3_775 ? Ca1 O4 2.340(3) . ? Ca1 S2 3.4563(13) . ? Ca1 S2 3.4563(13) 3_775 ? S1 O3 1.441(4) . ? S1 O2 1.464(4) . ? S1 O1 1.465(4) . ? S1 C1 1.771(5) . ? O2 Ca1 2.325(4) 1_455 ? C1 C2 1.525(7) . ? C2 C3 1.528(8) . ? C3 C4 1.536(8) . ? C4 C5 1.517(9) . ? C5 C6 1.520(10) . ? C6 C7 1.526(10) . ? C7 C8 1.517(10) . ? C8 C9 1.533(11) . ? C9 C10 1.523(11) . ? C10 C11 1.527(11) . ? C11 C12 1.522(11) . ? C12 C13 1.523(11) . ? C13 C14 1.522(11) . ? C14 C15 1.527(10) . ? C15 C16 1.515(10) . ? C16 C17 1.515(9) . ? C17 C18 1.532(9) . ? S2 O4 1.529(4) . ? S2 C20 1.776(6) . ? S2 C19 1.777(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 O2 Ca1 O2 180.00(14) 3_675 1_655 ? O2 Ca1 O1 88.49(13) 3_675 . ? O2 Ca1 O1 91.51(13) 1_655 . ? O2 Ca1 O1 91.51(13) 3_675 3_775 ? O2 Ca1 O1 88.49(13) 1_655 3_775 ? O1 Ca1 O1 180.00(13) . 3_775 ? O2 Ca1 O4 89.45(13) 3_675 3_775 ? O2 Ca1 O4 90.55(13) 1_655 3_775 ? O1 Ca1 O4 97.89(13) . 3_775 ? O1 Ca1 O4 82.11(13) 3_775 3_775 ? O2 Ca1 O4 90.55(13) 3_675 . ? O2 Ca1 O4 89.45(13) 1_655 . ? O1 Ca1 O4 82.11(13) . . ? O1 Ca1 O4 97.89(13) 3_775 . ? O4 Ca1 O4 180.00(16) 3_775 . ? O2 Ca1 S2 85.04(9) 3_675 . ? O2 Ca1 S2 94.96(9) 1_655 . ? O1 Ca1 S2 61.59(10) . . ? O1 Ca1 S2 118.41(10) 3_775 . ? O4 Ca1 S2 158.82(9) 3_775 . ? O4 Ca1 S2 21.18(9) . . ? O2 Ca1 S2 94.96(9) 3_675 3_775 ? O2 Ca1 S2 85.04(9) 1_655 3_775 ? O1 Ca1 S2 118.41(10) . 3_775 ? O1 Ca1 S2 61.59(10) 3_775 3_775 ? O4 Ca1 S2 21.18(9) 3_775 3_775 ? O4 Ca1 S2 158.82(9) . 3_775 ? S2 Ca1 S2 180.00(4) . 3_775 ? O3 S1 O2 112.9(2) . . ? O3 S1 O1 113.1(2) . . ? O2 S1 O1 111.5(2) . . ? O3 S1 C1 106.2(2) . . ? O2 S1 C1 106.7(2) . . ? O1 S1 C1 105.8(2) . . ? S1 O1 Ca1 152.4(2) . . ? S1 O2 Ca1 142.7(2) . 1_455 ? C2 C1 S1 111.2(4) . . ? C1 C2 C3 112.3(5) . . ? C2 C3 C4 112.0(6) . . ? C5 C4 C3 113.9(6) . . ? C4 C5 C6 113.9(7) . . ? C5 C6 C7 113.8(8) . . ? C8 C7 C6 113.4(8) . . ? C7 C8 C9 113.5(9) . . ? C10 C9 C8 113.4(9) . . ? C9 C10 C11 113.3(9) . . ? C12 C11 C10 113.6(9) . . ? C11 C12 C13 113.8(9) . . ? C14 C13 C12 113.8(8) . . ? C13 C14 C15 113.3(8) . . ? C16 C15 C14 114.1(8) . . ? C15 C16 C17 113.3(7) . . ? C16 C17 C18 114.1(7) . . ? O4 S2 C20 105.0(3) . . ? O4 S2 C19 106.0(2) . . ? C20 S2 C19 98.5(3) . . ? O4 S2 Ca1 33.57(13) . . ? C20 S2 Ca1 94.0(2) . . ? C19 S2 Ca1 139.57(19) . . ? S2 O4 Ca1 125.2(2) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.03 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.399 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.106