# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_11paf013a _database_code_depnum_ccdc_archive 'CCDC 891789' #TrackingRef '- CaSr_all11_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-11-20 _audit_author_name 'Webster, M.' _chemical_name_systematic ; bis(acetonitrile)(1,4,7,10,13,16-hexaoxacyclooctadecane)calcium(II) bis(hexachloro)antimonate(V) ; # # C12H24O6 = 18-crown-6 # 1,4,7,10,13,16-hexaoxacyclooctadecane (Chemspider) # # MeCN = C2H3N # acetonitrile (Chemspider & iLab (defaults & selected options)) # methylcyanide # cyanomethane # _chemical_name_common ; bis(acetonitrile)(1,4,7,10,13,16- hexaoxacyclooctadecane)calcium(ii) bis(hexachloro)antimonate(V) ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H30 Ca N2 O6 2+, 2(Cl6 Sb 1-)' _chemical_formula_sum 'C16 H30 Ca Cl12 N2 O6 Sb2' _chemical_formula_structural '((C12 H24 O6) 2(C2 H3 N) Ca) (Cl6 Sb)2' _chemical_formula_weight 1055.40 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' 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 26.561(6) _cell_length_b 13.365(2) _cell_length_c 23.205(7) _cell_angle_alpha 90.00 _cell_angle_beta 115.331(10) _cell_angle_gamma 90.00 _cell_volume 7445(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 30624 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.883 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4112 _exptl_absorpt_coefficient_mu 2.482 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.411 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS conversion' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40678 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.49 _reflns_number_total 16579 _reflns_number_gt 13126 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+32.0895P] 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 'constr (CH2) noref (CH3)' # or mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16579 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1784 _refine_ls_wR_factor_gt 0.1574 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Sb1 Sb 0.215591(15) 0.21405(3) 0.11022(2) 0.02437(11) Uani 1 1 d . . . Sb2 Sb 0.447125(15) 0.64043(3) 0.229130(19) 0.02233(10) Uani 1 1 d . . . Sb3 Sb 0.281227(16) 0.70862(3) 0.87575(2) 0.02653(11) Uani 1 1 d . . . Sb4 Sb 0.052048(16) 0.13345(3) 0.77558(2) 0.02410(11) Uani 1 1 d . . . Cl1 Cl 0.29509(7) 0.31169(14) 0.17172(9) 0.0381(4) Uani 1 1 d . . . Cl2 Cl 0.18145(7) 0.34643(13) 0.03522(9) 0.0378(4) Uani 1 1 d . . . Cl3 Cl 0.26416(7) 0.14600(13) 0.05402(9) 0.0376(4) Uani 1 1 d . . . Cl4 Cl 0.24855(7) 0.08422(14) 0.18649(9) 0.0413(4) Uani 1 1 d . . . Cl5 Cl 0.16621(7) 0.28113(14) 0.16533(9) 0.0354(4) Uani 1 1 d . . . Cl6 Cl 0.13800(6) 0.11495(13) 0.04734(8) 0.0322(3) Uani 1 1 d . . . Cl7 Cl 0.52538(7) 0.71858(14) 0.22525(9) 0.0391(4) Uani 1 1 d . . . Cl8 Cl 0.40332(7) 0.63204(13) 0.11603(8) 0.0328(3) Uani 1 1 d . . . Cl9 Cl 0.40462(7) 0.79729(12) 0.22431(9) 0.0322(3) Uani 1 1 d . . . Cl10 Cl 0.48976(7) 0.65198(13) 0.34195(8) 0.0337(3) Uani 1 1 d . . . Cl11 Cl 0.48907(6) 0.48212(12) 0.23600(8) 0.0326(3) Uani 1 1 d . . . Cl12 Cl 0.36944(6) 0.55716(13) 0.23144(8) 0.0314(3) Uani 1 1 d . . . Cl13 Cl 0.34616(9) 0.77543(16) 0.84237(11) 0.0486(5) Uani 1 1 d . . . Cl14 Cl 0.24122(10) 0.6148(3) 0.78137(14) 0.0793(9) Uani 1 1 d . . . Cl15 Cl 0.21958(9) 0.84218(18) 0.83033(11) 0.0568(6) Uani 1 1 d . . . Cl16 Cl 0.32371(8) 0.80144(19) 0.97221(10) 0.0510(5) Uani 1 1 d . . . Cl17 Cl 0.34364(9) 0.57432(16) 0.92502(12) 0.0531(5) Uani 1 1 d . . . Cl18 Cl 0.21795(9) 0.63922(17) 0.91174(14) 0.0623(7) Uani 1 1 d . . . Cl19 Cl 0.08964(7) 0.29478(13) 0.77931(10) 0.0398(4) Uani 1 1 d . . . Cl20 Cl 0.14320(7) 0.06602(14) 0.81982(9) 0.0396(4) Uani 1 1 d . . . Cl21 Cl 0.04497(7) 0.11490(13) 0.67088(8) 0.0345(4) Uani 1 1 d . . . Cl22 Cl -0.03970(7) 0.19787(14) 0.73094(9) 0.0375(4) Uani 1 1 d . . . Cl23 Cl 0.05680(9) 0.15372(17) 0.87889(9) 0.0503(5) Uani 1 1 d . . . Cl24 Cl 0.01662(7) -0.02990(12) 0.76964(8) 0.0329(3) Uani 1 1 d . . . Ca1 Ca 0.38737(5) 0.24069(9) -0.04708(6) 0.0234(2) Uani 1 1 d . . . Ca2 Ca 0.12380(5) 0.73134(9) 1.05525(6) 0.0235(2) Uani 1 1 d . . . O1 O 0.28851(17) 0.2121(4) -0.1200(2) 0.0300(10) Uani 1 1 d . . . O2 O 0.31870(18) 0.3397(4) -0.0276(2) 0.0313(10) Uani 1 1 d . . . O3 O 0.42226(17) 0.3213(4) 0.0592(2) 0.0286(9) Uani 1 1 d . . . O4 O 0.47554(17) 0.3472(4) -0.0147(2) 0.0295(10) Uani 1 1 d . . . O5 O 0.47397(18) 0.1450(4) -0.0351(3) 0.0381(12) Uani 1 1 d . . . O6 O 0.37180(17) 0.1008(4) -0.1218(2) 0.0303(10) Uani 1 1 d . . . O7 O 0.21925(19) 0.7769(4) 1.0816(3) 0.0488(15) Uani 1 1 d . . . O8 O 0.19607(18) 0.5914(4) 1.0996(2) 0.0315(10) Uani 1 1 d . . . O9 O 0.13272(19) 0.6500(4) 1.1561(2) 0.0327(10) Uani 1 1 d . . . O10 O 0.03404(18) 0.6985(4) 1.0599(2) 0.0358(11) Uani 1 1 d . . . O11 O 0.03784(17) 0.7864(4) 0.9609(2) 0.0312(10) Uani 1 1 d . . . O12 O 0.13665(18) 0.8598(4) 0.9854(2) 0.0323(10) Uani 1 1 d . . . N1 N 0.3780(2) 0.3461(5) -0.1389(3) 0.0364(13) Uani 1 1 d . . . N2 N 0.3815(2) 0.0989(4) 0.0193(3) 0.0285(11) Uani 1 1 d . . . N3 N 0.1057(3) 0.6013(5) 0.9729(3) 0.0431(15) Uani 1 1 d . . . N4 N 0.1199(3) 0.8787(5) 1.1176(3) 0.0396(14) Uani 1 1 d . . . C1 C 0.2559(3) 0.3021(6) -0.1337(4) 0.0361(16) Uani 1 1 d . . . H1A H 0.2165 0.2877 -0.1626 0.043 Uiso 1 1 calc R . . H1B H 0.2704 0.3520 -0.1543 0.043 Uiso 1 1 calc R . . C2 C 0.2603(3) 0.3408(6) -0.0715(4) 0.0370(16) Uani 1 1 d . . . H2A H 0.2455 0.4098 -0.0765 0.044 Uiso 1 1 calc R . . H2B H 0.2388 0.2980 -0.0553 0.044 Uiso 1 1 calc R . . C3 C 0.3302(3) 0.3852(5) 0.0331(3) 0.0321(14) Uani 1 1 d . . . H3A H 0.2978 0.3774 0.0433 0.038 Uiso 1 1 calc R . . H3B H 0.3378 0.4575 0.0320 0.038 Uiso 1 1 calc R . . C4 C 0.3803(3) 0.3331(5) 0.0825(3) 0.0311(14) Uani 1 1 d . . . H4A H 0.3956 0.3729 0.1223 0.037 Uiso 1 1 calc R . . H4B H 0.3694 0.2667 0.0921 0.037 Uiso 1 1 calc R . . C5 C 0.4546(3) 0.4116(6) 0.0670(4) 0.0385(16) Uani 1 1 d . . . H5A H 0.4694 0.4359 0.1115 0.046 Uiso 1 1 calc R . . H5B H 0.4315 0.4649 0.0382 0.046 Uiso 1 1 calc R . . C6 C 0.5013(3) 0.3831(5) 0.0502(3) 0.0325(14) Uani 1 1 d . . . H6A H 0.5252 0.4418 0.0537 0.039 Uiso 1 1 calc R . . H6B H 0.5246 0.3301 0.0792 0.039 Uiso 1 1 calc R . . C7 C 0.5142(3) 0.3043(6) -0.0360(4) 0.0439(19) Uani 1 1 d . . . H7A H 0.5491 0.3436 -0.0192 0.053 Uiso 1 1 calc R . . H7B H 0.4982 0.3055 -0.0831 0.053 Uiso 1 1 calc R . . C8 C 0.5263(3) 0.1979(6) -0.0125(5) 0.055(3) Uani 1 1 d . . . H8A H 0.5511 0.1658 -0.0288 0.066 Uiso 1 1 calc R . . H8B H 0.5449 0.1967 0.0347 0.066 Uiso 1 1 calc R . . C9 C 0.4680(3) 0.0699(6) -0.0817(4) 0.0373(16) Uani 1 1 d . . . H9A H 0.4979 0.0191 -0.0634 0.045 Uiso 1 1 calc R . . H9B H 0.4704 0.1005 -0.1193 0.045 Uiso 1 1 calc R . . C10 C 0.4117(3) 0.0220(5) -0.1008(4) 0.0364(15) Uani 1 1 d . . . H10A H 0.4041 -0.0270 -0.1355 0.044 Uiso 1 1 calc R . . H10B H 0.4102 -0.0132 -0.0640 0.044 Uiso 1 1 calc R . . C11 C 0.3152(3) 0.0653(6) -0.1542(3) 0.0354(15) Uani 1 1 d . . . H11A H 0.3052 0.0253 -0.1248 0.042 Uiso 1 1 calc R . . H11B H 0.3110 0.0228 -0.1909 0.042 Uiso 1 1 calc R . . C12 C 0.2789(3) 0.1552(6) -0.1763(3) 0.0369(16) Uani 1 1 d . . . H12A H 0.2887 0.1951 -0.2060 0.044 Uiso 1 1 calc R . . H12B H 0.2393 0.1353 -0.1985 0.044 Uiso 1 1 calc R . . C13 C 0.3795(3) 0.4107(6) -0.1702(3) 0.0338(15) Uani 1 1 d . . . C14 C 0.3822(3) 0.4936(7) -0.2092(4) 0.046(2) Uani 1 1 d . . . H14A H 0.3636 0.5520 -0.2017 0.068 Uiso 1 1 d . . . H14B H 0.3637 0.4747 -0.2543 0.068 Uiso 1 1 d . . . H14C H 0.4213 0.5098 -0.1979 0.068 Uiso 1 1 d . . . C15 C 0.3836(2) 0.0445(5) 0.0581(3) 0.0293(13) Uani 1 1 d . . . C16 C 0.3872(3) -0.0244(6) 0.1085(3) 0.0407(17) Uani 1 1 d . . . H16A H 0.4245 -0.0211 0.1436 0.061 Uiso 1 1 d . . . H16B H 0.3798 -0.0927 0.0915 0.061 Uiso 1 1 d . . . H16C H 0.3595 -0.0056 0.1241 0.061 Uiso 1 1 d . . . C17 C 0.2661(3) 0.7103(6) 1.1051(4) 0.0411(18) Uani 1 1 d . . . H17A H 0.2860 0.7145 1.1522 0.049 Uiso 1 1 calc R . . H17B H 0.2924 0.7273 1.0867 0.049 Uiso 1 1 calc R . . C18 C 0.2424(3) 0.6069(6) 1.0847(4) 0.0372(16) Uani 1 1 d . . . H18A H 0.2302 0.5991 1.0382 0.045 Uiso 1 1 calc R . . H18B H 0.2714 0.5561 1.1069 0.045 Uiso 1 1 calc R . . C19 C 0.2107(3) 0.5606(6) 1.1635(4) 0.0384(16) Uani 1 1 d . . . H19A H 0.2352 0.6107 1.1940 0.046 Uiso 1 1 calc R . . H19B H 0.2303 0.4954 1.1722 0.046 Uiso 1 1 calc R . . C20 C 0.1572(3) 0.5519(5) 1.1692(4) 0.0370(16) Uani 1 1 d . . . H20A H 0.1324 0.5027 1.1382 0.044 Uiso 1 1 calc R . . H20B H 0.1639 0.5301 1.2127 0.044 Uiso 1 1 calc R . . C21 C 0.0846(3) 0.6598(6) 1.1682(4) 0.0401(17) Uani 1 1 d . . . H21A H 0.0822 0.7291 1.1818 0.048 Uiso 1 1 calc R . . H21B H 0.0878 0.6141 1.2032 0.048 Uiso 1 1 calc R . . C22 C 0.0328(3) 0.6355(6) 1.1096(4) 0.0430(18) Uani 1 1 d . . . H22A H 0.0324 0.5640 1.0983 0.052 Uiso 1 1 calc R . . H22B H -0.0008 0.6496 1.1167 0.052 Uiso 1 1 calc R . . C23 C -0.0159(3) 0.6965(6) 1.0014(4) 0.0417(18) Uani 1 1 d . . . H23A H -0.0491 0.6988 1.0103 0.050 Uiso 1 1 calc R . . H23B H -0.0174 0.6345 0.9773 0.050 Uiso 1 1 calc R . . C24 C -0.0144(3) 0.7860(6) 0.9638(4) 0.0358(16) Uani 1 1 d . . . H24A H -0.0450 0.7827 0.9203 0.043 Uiso 1 1 calc R . . H24B H -0.0189 0.8478 0.9846 0.043 Uiso 1 1 calc R . . C25 C 0.0408(3) 0.8639(7) 0.9200(4) 0.049(2) Uani 1 1 d . . . H25A H 0.0346 0.9299 0.9354 0.059 Uiso 1 1 calc R . . H25B H 0.0116 0.8538 0.8761 0.059 Uiso 1 1 calc R . . C26 C 0.0971(3) 0.8606(8) 0.9205(4) 0.050(2) Uani 1 1 d . . . H26A H 0.1010 0.7996 0.8985 0.060 Uiso 1 1 calc R . . H26B H 0.1028 0.9199 0.8984 0.060 Uiso 1 1 calc R . . C27 C 0.1915(3) 0.8866(6) 0.9934(4) 0.0366(16) Uani 1 1 d . . . H27A H 0.1921 0.9564 0.9793 0.044 Uiso 1 1 calc R . . H27B H 0.2040 0.8416 0.9682 0.044 Uiso 1 1 calc R . . C28 C 0.2277(3) 0.8761(6) 1.0620(4) 0.0422(18) Uani 1 1 d . . . H28A H 0.2672 0.8850 1.0701 0.051 Uiso 1 1 calc R . . H28B H 0.2182 0.9275 1.0864 0.051 Uiso 1 1 calc R . . C29 C 0.1037(3) 0.5466(6) 0.9336(4) 0.0383(16) Uani 1 1 d . . . C30 C 0.1027(3) 0.4763(6) 0.8871(4) 0.0411(17) Uani 1 1 d . . . H30A H 0.1299 0.4958 0.8711 0.062 Uiso 1 1 d . . . H30B H 0.0654 0.4747 0.8517 0.062 Uiso 1 1 d . . . H30C H 0.1120 0.4096 0.9065 0.062 Uiso 1 1 d . . . C31 C 0.1163(3) 0.9387(6) 1.1499(4) 0.0357(15) Uani 1 1 d . . . C32 C 0.1114(3) 1.0154(6) 1.1918(4) 0.0408(17) Uani 1 1 d . . . H32A H 0.1199 1.0809 1.1793 0.061 Uiso 1 1 d . . . H32B H 0.1376 1.0010 1.2360 0.061 Uiso 1 1 d . . . H32C H 0.0733 1.0155 1.1884 0.061 Uiso 1 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 Sb1 0.02054(19) 0.0261(2) 0.0288(2) 0.00065(17) 0.01273(16) 0.00038(15) Sb2 0.02177(19) 0.0233(2) 0.0243(2) -0.00056(16) 0.01216(16) 0.00018(15) Sb3 0.0239(2) 0.0271(2) 0.0303(2) -0.00186(17) 0.01312(17) -0.00165(16) Sb4 0.0247(2) 0.0241(2) 0.0260(2) 0.00012(16) 0.01317(17) 0.00234(15) Cl1 0.0296(7) 0.0465(10) 0.0411(9) -0.0099(8) 0.0178(7) -0.0122(7) Cl2 0.0421(9) 0.0331(8) 0.0429(10) 0.0124(8) 0.0228(8) 0.0072(7) Cl3 0.0342(8) 0.0383(9) 0.0513(10) -0.0059(8) 0.0287(8) -0.0013(7) Cl4 0.0368(8) 0.0413(10) 0.0391(9) 0.0145(8) 0.0099(7) 0.0032(7) Cl5 0.0330(8) 0.0419(9) 0.0407(9) -0.0076(8) 0.0247(7) -0.0030(7) Cl6 0.0242(7) 0.0375(8) 0.0350(8) -0.0044(7) 0.0125(6) -0.0031(6) Cl7 0.0314(8) 0.0443(10) 0.0493(10) -0.0032(8) 0.0247(8) -0.0077(7) Cl8 0.0330(7) 0.0432(9) 0.0235(7) -0.0003(7) 0.0135(6) 0.0053(7) Cl9 0.0364(8) 0.0239(7) 0.0410(9) -0.0013(7) 0.0208(7) 0.0035(6) Cl10 0.0323(7) 0.0414(9) 0.0247(7) -0.0048(7) 0.0098(6) -0.0014(7) Cl11 0.0325(7) 0.0297(8) 0.0330(8) -0.0006(7) 0.0115(6) 0.0088(6) Cl12 0.0272(7) 0.0372(8) 0.0316(8) 0.0017(7) 0.0142(6) -0.0056(6) Cl13 0.0598(11) 0.0449(10) 0.0609(13) 0.0044(9) 0.0446(11) -0.0058(9) Cl14 0.0492(12) 0.109(2) 0.0686(16) -0.0587(17) 0.0148(11) -0.0112(13) Cl15 0.0503(11) 0.0555(13) 0.0559(13) 0.0137(11) 0.0145(10) 0.0237(10) Cl16 0.0360(9) 0.0766(15) 0.0383(10) -0.0237(10) 0.0137(8) -0.0034(9) Cl17 0.0490(10) 0.0447(11) 0.0723(15) 0.0163(11) 0.0324(11) 0.0158(9) Cl18 0.0552(12) 0.0519(12) 0.105(2) 0.0015(13) 0.0588(14) -0.0084(10) Cl19 0.0412(9) 0.0253(8) 0.0496(11) -0.0033(8) 0.0161(8) -0.0024(7) Cl20 0.0255(7) 0.0412(9) 0.0476(10) 0.0055(8) 0.0114(7) 0.0072(7) Cl21 0.0430(8) 0.0366(9) 0.0307(8) -0.0009(7) 0.0223(7) 0.0012(7) Cl22 0.0304(7) 0.0434(10) 0.0414(9) 0.0060(8) 0.0179(7) 0.0109(7) Cl23 0.0682(12) 0.0576(12) 0.0296(9) 0.0000(9) 0.0252(9) 0.0133(10) Cl24 0.0340(7) 0.0275(8) 0.0368(8) 0.0047(7) 0.0147(7) -0.0044(6) Ca1 0.0223(5) 0.0249(6) 0.0251(6) 0.0003(5) 0.0122(5) -0.0004(5) Ca2 0.0204(5) 0.0259(6) 0.0262(6) -0.0008(5) 0.0120(5) -0.0006(5) O1 0.023(2) 0.043(3) 0.023(2) 0.001(2) 0.0083(18) 0.0021(19) O2 0.028(2) 0.033(2) 0.038(3) 0.000(2) 0.019(2) 0.0037(19) O3 0.027(2) 0.035(2) 0.027(2) -0.002(2) 0.0145(18) 0.0002(19) O4 0.029(2) 0.036(2) 0.029(2) -0.006(2) 0.0173(19) -0.0040(19) O5 0.023(2) 0.038(3) 0.053(3) -0.015(2) 0.016(2) -0.001(2) O6 0.024(2) 0.038(3) 0.029(2) -0.006(2) 0.0107(18) -0.0027(19) O7 0.020(2) 0.051(3) 0.069(4) 0.022(3) 0.013(2) 0.000(2) O8 0.027(2) 0.031(2) 0.034(3) -0.002(2) 0.0116(19) -0.0009(19) O9 0.038(2) 0.033(3) 0.031(2) 0.006(2) 0.019(2) 0.004(2) O10 0.027(2) 0.047(3) 0.036(3) 0.013(2) 0.017(2) 0.002(2) O11 0.022(2) 0.039(3) 0.034(3) 0.007(2) 0.0141(19) 0.0002(19) O12 0.030(2) 0.039(3) 0.031(2) 0.002(2) 0.016(2) -0.005(2) N1 0.037(3) 0.037(3) 0.039(3) 0.004(3) 0.021(3) -0.004(3) N2 0.033(3) 0.027(3) 0.028(3) 0.000(2) 0.015(2) -0.002(2) N3 0.038(3) 0.047(4) 0.034(3) -0.008(3) 0.006(3) 0.013(3) N4 0.043(3) 0.036(3) 0.045(4) -0.005(3) 0.024(3) -0.003(3) C1 0.025(3) 0.047(4) 0.039(4) 0.010(3) 0.016(3) 0.004(3) C2 0.020(3) 0.041(4) 0.049(4) 0.011(3) 0.014(3) 0.006(3) C3 0.036(3) 0.032(3) 0.040(4) -0.001(3) 0.028(3) 0.000(3) C4 0.036(3) 0.040(4) 0.027(3) -0.003(3) 0.022(3) -0.004(3) C5 0.036(3) 0.047(4) 0.040(4) -0.014(3) 0.024(3) -0.010(3) C6 0.032(3) 0.038(4) 0.029(3) -0.007(3) 0.014(3) -0.001(3) C7 0.039(4) 0.060(5) 0.049(4) -0.015(4) 0.034(4) -0.013(4) C8 0.024(3) 0.039(4) 0.102(8) -0.018(5) 0.026(4) 0.001(3) C9 0.034(3) 0.042(4) 0.037(4) -0.014(3) 0.016(3) 0.003(3) C10 0.036(3) 0.035(4) 0.037(4) -0.007(3) 0.015(3) 0.005(3) C11 0.029(3) 0.044(4) 0.029(3) -0.019(3) 0.009(3) -0.013(3) C12 0.027(3) 0.058(5) 0.026(3) -0.007(3) 0.012(3) -0.002(3) C13 0.025(3) 0.048(4) 0.030(3) 0.008(3) 0.014(3) -0.001(3) C14 0.033(3) 0.057(5) 0.048(5) 0.021(4) 0.019(3) -0.001(3) C15 0.024(3) 0.035(3) 0.029(3) 0.001(3) 0.011(3) -0.005(3) C16 0.045(4) 0.049(4) 0.027(3) 0.011(3) 0.013(3) -0.007(3) C17 0.022(3) 0.058(5) 0.039(4) 0.009(4) 0.009(3) 0.004(3) C18 0.029(3) 0.048(4) 0.036(4) 0.000(3) 0.016(3) 0.010(3) C19 0.033(3) 0.039(4) 0.037(4) 0.002(3) 0.010(3) 0.002(3) C20 0.037(3) 0.033(4) 0.037(4) 0.015(3) 0.013(3) 0.013(3) C21 0.056(4) 0.036(4) 0.048(4) 0.004(3) 0.041(4) 0.001(3) C22 0.043(4) 0.045(4) 0.056(5) 0.016(4) 0.035(4) 0.009(3) C23 0.026(3) 0.047(4) 0.055(5) -0.012(4) 0.020(3) -0.009(3) C24 0.022(3) 0.045(4) 0.039(4) -0.006(3) 0.011(3) 0.002(3) C25 0.036(4) 0.056(5) 0.053(5) 0.029(4) 0.018(4) 0.009(4) C26 0.041(4) 0.074(6) 0.035(4) 0.021(4) 0.016(3) -0.006(4) C27 0.034(3) 0.038(4) 0.046(4) 0.002(3) 0.025(3) 0.000(3) C28 0.027(3) 0.041(4) 0.055(5) -0.003(4) 0.013(3) -0.010(3) C29 0.028(3) 0.040(4) 0.037(4) -0.005(3) 0.005(3) 0.004(3) C30 0.036(3) 0.044(4) 0.039(4) -0.012(4) 0.012(3) 0.000(3) C31 0.030(3) 0.037(4) 0.044(4) -0.002(3) 0.019(3) 0.002(3) C32 0.047(4) 0.043(4) 0.040(4) -0.010(3) 0.025(3) 0.003(3) _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 Sb1 Cl6 2.3574(16) . ? Sb1 Cl4 2.3629(18) . ? Sb1 Cl5 2.3655(16) . ? Sb1 Cl1 2.3707(17) . ? Sb1 Cl2 2.3729(18) . ? Sb1 Cl3 2.3730(17) . ? Sb2 Cl9 2.3609(16) . ? Sb2 Cl7 2.3621(16) . ? Sb2 Cl11 2.3645(16) . ? Sb2 Cl12 2.3651(15) . ? Sb2 Cl10 2.3713(18) . ? Sb2 Cl8 2.3750(18) . ? Sb3 Cl15 2.346(2) . ? Sb3 Cl14 2.347(2) . ? Sb3 Cl13 2.3485(18) . ? Sb3 Cl18 2.363(2) . ? Sb3 Cl17 2.378(2) . ? Sb3 Cl16 2.379(2) . ? Sb4 Cl24 2.3579(17) . ? Sb4 Cl23 2.362(2) . ? Sb4 Cl19 2.3620(18) . ? Sb4 Cl22 2.3650(17) . ? Sb4 Cl20 2.3666(17) . ? Sb4 Cl21 2.3681(18) . ? Ca1 O2 2.447(4) . ? Ca1 O6 2.462(5) . ? Ca1 O1 2.470(4) . ? Ca1 N1 2.477(6) . ? Ca1 O3 2.480(5) . ? Ca1 N2 2.488(6) . ? Ca1 O5 2.542(5) . ? Ca1 O4 2.563(4) . ? Ca2 O7 2.418(5) . ? Ca2 N4 2.471(6) . ? Ca2 O10 2.472(4) . ? Ca2 N3 2.474(7) . ? Ca2 O12 2.483(5) . ? Ca2 O9 2.499(5) . ? Ca2 O11 2.504(5) . ? Ca2 O8 2.559(5) . ? O1 C1 1.437(8) . ? O1 C12 1.438(8) . ? O2 C3 1.442(8) . ? O2 C2 1.446(8) . ? O3 C4 1.438(7) . ? O3 C5 1.448(8) . ? O4 C7 1.436(8) . ? O4 C6 1.444(8) . ? O5 C9 1.433(8) . ? O5 C8 1.443(8) . ? O6 C10 1.424(8) . ? O6 C11 1.442(7) . ? O7 C17 1.434(8) . ? O7 C28 1.450(9) . ? O8 C19 1.424(9) . ? O8 C18 1.428(8) . ? O9 C21 1.427(8) . ? O9 C20 1.437(8) . ? O10 C23 1.437(9) . ? O10 C22 1.440(8) . ? O11 C24 1.418(7) . ? O11 C25 1.429(9) . ? O12 C26 1.422(9) . ? O12 C27 1.435(8) . ? N1 C13 1.140(9) . ? N2 C15 1.140(9) . ? N3 C29 1.152(10) . ? N4 C31 1.130(9) . ? C1 C2 1.489(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.505(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.500(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.507(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.509(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.488(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.451(10) . ? C14 H14A 0.9788 . ? C14 H14B 0.9800 . ? C14 H14C 0.9811 . ? C15 C16 1.460(9) . ? C16 H16A 0.9797 . ? C16 H16B 0.9805 . ? C16 H16C 0.9796 . ? C17 C18 1.509(11) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.487(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.498(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.490(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.492(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.472(11) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.421(10) . ? C30 H30A 0.9803 . ? C30 H30B 0.9804 . ? C30 H30C 0.9806 . ? C31 C32 1.456(10) . ? C32 H32A 0.9788 . ? C32 H32B 0.9803 . ? C32 H32C 0.9809 . ? 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 Cl6 Sb1 Cl4 89.81(7) . . ? Cl6 Sb1 Cl5 90.43(6) . . ? Cl4 Sb1 Cl5 89.25(7) . . ? Cl6 Sb1 Cl1 178.25(6) . . ? Cl4 Sb1 Cl1 90.24(7) . . ? Cl5 Sb1 Cl1 91.32(6) . . ? Cl6 Sb1 Cl2 90.36(7) . . ? Cl4 Sb1 Cl2 178.53(7) . . ? Cl5 Sb1 Cl2 89.29(7) . . ? Cl1 Sb1 Cl2 89.63(7) . . ? Cl6 Sb1 Cl3 88.93(6) . . ? Cl4 Sb1 Cl3 90.91(7) . . ? Cl5 Sb1 Cl3 179.34(7) . . ? Cl1 Sb1 Cl3 89.32(6) . . ? Cl2 Sb1 Cl3 90.55(7) . . ? Cl9 Sb2 Cl7 90.93(6) . . ? Cl9 Sb2 Cl11 178.58(6) . . ? Cl7 Sb2 Cl11 90.08(6) . . ? Cl9 Sb2 Cl12 90.85(6) . . ? Cl7 Sb2 Cl12 178.02(6) . . ? Cl11 Sb2 Cl12 88.16(6) . . ? Cl9 Sb2 Cl10 89.27(6) . . ? Cl7 Sb2 Cl10 90.05(7) . . ? Cl11 Sb2 Cl10 89.72(6) . . ? Cl12 Sb2 Cl10 90.85(6) . . ? Cl9 Sb2 Cl8 89.50(6) . . ? Cl7 Sb2 Cl8 90.11(6) . . ? Cl11 Sb2 Cl8 91.50(6) . . ? Cl12 Sb2 Cl8 89.03(6) . . ? Cl10 Sb2 Cl8 178.77(6) . . ? Cl15 Sb3 Cl14 92.12(10) . . ? Cl15 Sb3 Cl13 91.86(8) . . ? Cl14 Sb3 Cl13 89.91(10) . . ? Cl15 Sb3 Cl18 89.56(9) . . ? Cl14 Sb3 Cl18 90.78(11) . . ? Cl13 Sb3 Cl18 178.40(9) . . ? Cl15 Sb3 Cl17 178.15(9) . . ? Cl14 Sb3 Cl17 89.40(10) . . ? Cl13 Sb3 Cl17 89.21(8) . . ? Cl18 Sb3 Cl17 89.36(8) . . ? Cl15 Sb3 Cl16 89.13(9) . . ? Cl14 Sb3 Cl16 178.66(9) . . ? Cl13 Sb3 Cl16 89.57(8) . . ? Cl18 Sb3 Cl16 89.71(9) . . ? Cl17 Sb3 Cl16 89.36(9) . . ? Cl24 Sb4 Cl23 90.70(7) . . ? Cl24 Sb4 Cl19 177.68(6) . . ? Cl23 Sb4 Cl19 91.14(8) . . ? Cl24 Sb4 Cl22 90.04(6) . . ? Cl23 Sb4 Cl22 90.02(7) . . ? Cl19 Sb4 Cl22 91.37(7) . . ? Cl24 Sb4 Cl20 88.93(6) . . ? Cl23 Sb4 Cl20 90.16(7) . . ? Cl19 Sb4 Cl20 89.64(7) . . ? Cl22 Sb4 Cl20 178.96(7) . . ? Cl24 Sb4 Cl21 89.35(6) . . ? Cl23 Sb4 Cl21 178.54(7) . . ? Cl19 Sb4 Cl21 88.85(7) . . ? Cl22 Sb4 Cl21 88.52(6) . . ? Cl20 Sb4 Cl21 91.30(7) . . ? O2 Ca1 O6 128.84(15) . . ? O2 Ca1 O1 63.41(16) . . ? O6 Ca1 O1 65.86(15) . . ? O2 Ca1 N1 92.48(18) . . ? O6 Ca1 N1 84.32(19) . . ? O1 Ca1 N1 79.23(18) . . ? O2 Ca1 O3 64.66(15) . . ? O6 Ca1 O3 155.40(17) . . ? O1 Ca1 O3 125.72(15) . . ? N1 Ca1 O3 117.80(19) . . ? O2 Ca1 N2 92.79(17) . . ? O6 Ca1 N2 79.70(18) . . ? O1 Ca1 N2 88.64(17) . . ? N1 Ca1 N2 162.9(2) . . ? O3 Ca1 N2 79.09(17) . . ? O2 Ca1 O5 164.46(18) . . ? O6 Ca1 O5 64.27(15) . . ? O1 Ca1 O5 130.09(16) . . ? N1 Ca1 O5 97.63(19) . . ? O3 Ca1 O5 100.06(16) . . ? N2 Ca1 O5 80.93(18) . . ? O2 Ca1 O4 107.77(15) . . ? O6 Ca1 O4 119.04(14) . . ? O1 Ca1 O4 148.98(16) . . ? N1 Ca1 O4 71.28(18) . . ? O3 Ca1 O4 63.99(14) . . ? N2 Ca1 O4 122.19(17) . . ? O5 Ca1 O4 64.97(15) . . ? O7 Ca2 N4 87.3(2) . . ? O7 Ca2 O10 163.8(2) . . ? N4 Ca2 O10 80.38(19) . . ? O7 Ca2 N3 102.0(2) . . ? N4 Ca2 N3 165.7(2) . . ? O10 Ca2 N3 92.1(2) . . ? O7 Ca2 O12 64.46(17) . . ? N4 Ca2 O12 83.27(19) . . ? O10 Ca2 O12 123.78(16) . . ? N3 Ca2 O12 91.0(2) . . ? O7 Ca2 O9 101.76(18) . . ? N4 Ca2 O9 79.01(19) . . ? O10 Ca2 O9 65.68(16) . . ? N3 Ca2 O9 109.1(2) . . ? O12 Ca2 O9 158.12(17) . . ? O7 Ca2 O11 127.74(18) . . ? N4 Ca2 O11 91.5(2) . . ? O10 Ca2 O11 63.58(15) . . ? N3 Ca2 O11 74.18(19) . . ? O12 Ca2 O11 63.54(15) . . ? O9 Ca2 O11 129.25(15) . . ? O7 Ca2 O8 63.72(17) . . ? N4 Ca2 O8 124.0(2) . . ? O10 Ca2 O8 115.09(16) . . ? N3 Ca2 O8 70.25(18) . . ? O12 Ca2 O8 118.62(15) . . ? O9 Ca2 O8 63.33(15) . . ? O11 Ca2 O8 144.36(17) . . ? C1 O1 C12 112.7(5) . . ? C1 O1 Ca1 112.7(4) . . ? C12 O1 Ca1 115.3(3) . . ? C3 O2 C2 113.5(5) . . ? C3 O2 Ca1 123.1(4) . . ? C2 O2 Ca1 122.3(4) . . ? C4 O3 C5 112.1(5) . . ? C4 O3 Ca1 113.6(4) . . ? C5 O3 Ca1 115.8(4) . . ? C7 O4 C6 113.7(5) . . ? C7 O4 Ca1 112.0(4) . . ? C6 O4 Ca1 117.2(4) . . ? C9 O5 C8 113.4(5) . . ? C9 O5 Ca1 117.9(4) . . ? C8 O5 Ca1 118.5(4) . . ? C10 O6 C11 113.1(5) . . ? C10 O6 Ca1 116.4(4) . . ? C11 O6 Ca1 116.1(4) . . ? C17 O7 C28 117.4(5) . . ? C17 O7 Ca2 125.8(4) . . ? C28 O7 Ca2 115.9(4) . . ? C19 O8 C18 114.5(5) . . ? C19 O8 Ca2 117.0(4) . . ? C18 O8 Ca2 111.9(4) . . ? C21 O9 C20 113.9(5) . . ? C21 O9 Ca2 114.2(4) . . ? C20 O9 Ca2 116.6(4) . . ? C23 O10 C22 114.8(5) . . ? C23 O10 Ca2 118.6(4) . . ? C22 O10 Ca2 119.5(4) . . ? C24 O11 C25 111.5(5) . . ? C24 O11 Ca2 120.1(4) . . ? C25 O11 Ca2 120.3(4) . . ? C26 O12 C27 112.6(5) . . ? C26 O12 Ca2 116.8(4) . . ? C27 O12 Ca2 120.3(4) . . ? C13 N1 Ca1 164.0(6) . . ? C15 N2 Ca1 168.4(5) . . ? C29 N3 Ca2 170.1(7) . . ? C31 N4 Ca2 172.3(6) . . ? O1 C1 C2 106.6(6) . . ? O1 C1 H1A 110.4 . . ? C2 C1 H1A 110.4 . . ? O1 C1 H1B 110.4 . . ? C2 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? O2 C2 C1 107.2(5) . . ? O2 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O2 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? O2 C3 C4 107.2(5) . . ? O2 C3 H3A 110.3 . . ? C4 C3 H3A 110.3 . . ? O2 C3 H3B 110.3 . . ? C4 C3 H3B 110.3 . . ? H3A C3 H3B 108.5 . . ? O3 C4 C3 109.9(5) . . ? O3 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? O3 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? O3 C5 C6 105.6(6) . . ? O3 C5 H5A 110.6 . . ? C6 C5 H5A 110.6 . . ? O3 C5 H5B 110.6 . . ? C6 C5 H5B 110.6 . . ? H5A C5 H5B 108.7 . . ? O4 C6 C5 106.2(5) . . ? O4 C6 H6A 110.5 . . ? C5 C6 H6A 110.5 . . ? O4 C6 H6B 110.5 . . ? C5 C6 H6B 110.5 . . ? H6A C6 H6B 108.7 . . ? O4 C7 C8 109.0(6) . . ? O4 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O4 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O5 C8 C7 108.0(6) . . ? O5 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? O5 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? O5 C9 C10 107.1(5) . . ? O5 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? O5 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? O6 C10 C9 106.6(6) . . ? O6 C10 H10A 110.4 . . ? C9 C10 H10A 110.4 . . ? O6 C10 H10B 110.4 . . ? C9 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? O6 C11 C12 107.0(6) . . ? O6 C11 H11A 110.3 . . ? C12 C11 H11A 110.3 . . ? O6 C11 H11B 110.3 . . ? C12 C11 H11B 110.3 . . ? H11A C11 H11B 108.6 . . ? O1 C12 C11 106.0(5) . . ? O1 C12 H12A 110.5 . . ? C11 C12 H12A 110.5 . . ? O1 C12 H12B 110.5 . . ? C11 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? N1 C13 C14 179.1(9) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.6 . . ? C13 C14 H14C 109.4 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.4 . . ? N2 C15 C16 179.1(8) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O7 C17 C18 105.7(5) . . ? O7 C17 H17A 110.6 . . ? C18 C17 H17A 110.6 . . ? O7 C17 H17B 110.6 . . ? C18 C17 H17B 110.6 . . ? H17A C17 H17B 108.7 . . ? O8 C18 C17 110.1(6) . . ? O8 C18 H18A 109.6 . . ? C17 C18 H18A 109.6 . . ? O8 C18 H18B 109.6 . . ? C17 C18 H18B 109.6 . . ? H18A C18 H18B 108.2 . . ? O8 C19 C20 105.7(5) . . ? O8 C19 H19A 110.6 . . ? C20 C19 H19A 110.6 . . ? O8 C19 H19B 110.6 . . ? C20 C19 H19B 110.6 . . ? H19A C19 H19B 108.7 . . ? O9 C20 C19 105.8(6) . . ? O9 C20 H20A 110.6 . . ? C19 C20 H20A 110.6 . . ? O9 C20 H20B 110.6 . . ? C19 C20 H20B 110.6 . . ? H20A C20 H20B 108.7 . . ? O9 C21 C22 110.8(6) . . ? O9 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? O9 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? O10 C22 C21 105.8(6) . . ? O10 C22 H22A 110.6 . . ? C21 C22 H22A 110.6 . . ? O10 C22 H22B 110.6 . . ? C21 C22 H22B 110.6 . . ? H22A C22 H22B 108.7 . . ? O10 C23 C24 107.1(6) . . ? O10 C23 H23A 110.3 . . ? C24 C23 H23A 110.3 . . ? O10 C23 H23B 110.3 . . ? C24 C23 H23B 110.3 . . ? H23A C23 H23B 108.5 . . ? O11 C24 C23 107.6(5) . . ? O11 C24 H24A 110.2 . . ? C23 C24 H24A 110.2 . . ? O11 C24 H24B 110.2 . . ? C23 C24 H24B 110.2 . . ? H24A C24 H24B 108.5 . . ? O11 C25 C26 108.2(6) . . ? O11 C25 H25A 110.1 . . ? C26 C25 H25A 110.1 . . ? O11 C25 H25B 110.1 . . ? C26 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? O12 C26 C25 107.0(6) . . ? O12 C26 H26A 110.3 . . ? C25 C26 H26A 110.3 . . ? O12 C26 H26B 110.3 . . ? C25 C26 H26B 110.3 . . ? H26A C26 H26B 108.6 . . ? O12 C27 C28 105.8(6) . . ? O12 C27 H27A 110.6 . . ? C28 C27 H27A 110.6 . . ? O12 C27 H27B 110.6 . . ? C28 C27 H27B 110.6 . . ? H27A C27 H27B 108.7 . . ? O7 C28 C27 108.1(6) . . ? O7 C28 H28A 110.1 . . ? C27 C28 H28A 110.1 . . ? O7 C28 H28B 110.1 . . ? C27 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? N3 C29 C30 177.7(9) . . ? C29 C30 H30A 109.6 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.4 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.4 . . ? H30B C30 H30C 109.4 . . ? N4 C31 C32 179.4(8) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.4 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # Ca1 O1 C1 C2 -59.5(5) . . . . ? # Ca1 O2 C2 C1 -17.8(7) . . . . ? # Ca1 O2 C3 C4 -18.6(7) . . . . ? # Ca1 O3 C4 C3 -52.4(6) . . . . ? # Ca1 O3 C5 C6 -55.8(6) . . . . ? # Ca1 O4 C6 C5 -39.0(7) . . . . ? # Ca1 O4 C7 C8 -54.1(7) . . . . ? # Ca1 O5 C8 C7 -32.6(9) . . . . ? # Ca1 O5 C9 C10 -34.9(7) . . . . ? # Ca1 O6 C10 C9 -54.2(6) . . . . ? # Ca1 O6 C11 C12 44.8(6) . . . . ? # Ca1 O1 C12 C11 48.8(6) . . . . ? # Ca1 N1 C13 C14 25(59) . . . . ? # Ca1 N2 C15 C16 -25(58) . . . . ? # Ca2 O7 C17 C18 22.6(8) . . . . ? # Ca2 O8 C18 C17 52.5(6) . . . . ? # Ca2 O8 C19 C20 44.6(7) . . . . ? # Ca2 O9 C20 C19 52.1(7) . . . . ? # Ca2 O9 C21 C22 46.9(7) . . . . ? # Ca2 O10 C22 C21 37.8(7) . . . . ? # Ca2 O10 C23 C24 -46.6(7) . . . . ? # Ca2 O11 C24 C23 -37.2(7) . . . . ? # Ca2 O11 C25 C26 30.1(9) . . . . ? # Ca2 O12 C26 C25 52.2(8) . . . . ? # Ca2 O12 C27 C28 -32.5(7) . . . . ? # Ca2 O7 C28 C27 -53.1(7) . . . . ? C12 O1 C1 C2 167.8(5) . . . . ? C3 O2 C2 C1 173.9(6) . . . . ? O1 C1 C2 O2 48.0(7) . . . . ? C2 O2 C3 C4 149.7(5) . . . . ? C5 O3 C4 C3 81.1(7) . . . . ? O2 C3 C4 O3 44.6(7) . . . . ? C4 O3 C5 C6 171.7(5) . . . . ? C7 O4 C6 C5 -172.3(6) . . . . ? O3 C5 C6 O4 59.2(7) . . . . ? C6 O4 C7 C8 81.6(8) . . . . ? C9 O5 C8 C7 112.0(7) . . . . ? O4 C7 C8 O5 56.4(9) . . . . ? C8 O5 C9 C10 -179.7(7) . . . . ? C11 O6 C10 C9 167.6(5) . . . . ? O5 C9 C10 O6 55.6(7) . . . . ? C10 O6 C11 C12 -176.9(5) . . . . ? C1 O1 C12 C11 -179.8(5) . . . . ? O6 C11 C12 O1 -59.4(7) . . . . ? C28 O7 C17 C18 -146.7(7) . . . . ? C19 O8 C18 C17 -83.6(7) . . . . ? O7 C17 C18 O8 -47.7(8) . . . . ? C18 O8 C19 C20 178.4(6) . . . . ? C21 O9 C20 C19 -171.6(6) . . . . ? O8 C19 C20 O9 -60.6(7) . . . . ? C20 O9 C21 C22 -90.5(7) . . . . ? C23 O10 C22 C21 -172.1(6) . . . . ? O9 C21 C22 O10 -53.9(8) . . . . ? C22 O10 C23 C24 163.0(6) . . . . ? C25 O11 C24 C23 173.9(7) . . . . ? O10 C23 C24 O11 51.3(7) . . . . ? C24 O11 C25 C26 179.0(7) . . . . ? C27 O12 C26 C25 -162.5(7) . . . . ? O11 C25 C26 O12 -50.8(10) . . . . ? C26 O12 C27 C28 -176.5(7) . . . . ? C17 O7 C28 C27 117.3(7) . . . . ? O12 C27 C28 O7 52.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.352 _refine_diff_density_min -2.262 _refine_diff_density_rms 0.206 data_11paf017a _database_code_depnum_ccdc_archive 'CCDC 891790' #TrackingRef '- CaSr_all11_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-11-21 _audit_author_name 'Webster, M.' _chemical_name_systematic ; aquo(1,4,7,10,13,16-hexaoxacyclooctadecane)- bis(trifluoromethanesulfonate)calcium(II) ; # C12H24O6 = 18-crown-6 # 1,4,7,10,13,16-hexaoxacyclooctadecane (Chemspider) # # [F3CSO3]- = triflate anion # trifluoromethanesulphonate (from CSD search - very few hits(2?)) # trifluoromethanesulfonate (from CSD search - many hits with 'f' spelling) # trifluoromethanesulfonate (iLab defaults & selected options) # (sodium) trifluoromethanesulfonate (chemspider) _chemical_name_common ; aquo(1,4,7,10,13,16-hexaoxacyclooctadecane)- bis(trifluoromethanesulfonate)calcium(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C14 H26 Ca F6 O13 S2' _chemical_formula_sum 'C14 H26 Ca F6 O13 S2' _chemical_formula_structural '((C12 H24 O6) (C F3 O3 S)2 (O H2) Ca' _chemical_formula_weight 620.55 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' F F 0.0171 0.0103 '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 'C 2/c' _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.570(4) _cell_length_b 8.595(2) _cell_length_c 19.596(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.51(3) _cell_angle_gamma 90.00 _cell_volume 2386.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7252 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.728 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details 'Rigaku CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8352 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2710 _reflns_number_gt 2259 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+1.7491P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # 'geom (C-H) difmap (O-H)' _refine_ls_hydrogen_treatment 'constr (C-H) refxyz (O-H)' # mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2710 _refine_ls_number_parameters 167 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.0000 0.07533(5) 0.2500 0.01082(11) Uani 1 2 d S . . S1 S 0.04656(3) 0.44060(4) 0.35693(2) 0.01130(10) Uani 1 1 d . . . F1 F 0.11587(8) 0.55394(11) 0.48221(5) 0.0273(3) Uani 1 1 d . . . F2 F 0.07624(8) 0.31284(12) 0.48211(5) 0.0295(3) Uani 1 1 d . . . F3 F 0.20262(7) 0.37805(12) 0.45061(5) 0.0258(2) Uani 1 1 d . . . O1 O -0.16547(8) 0.12201(13) 0.26891(6) 0.0160(2) Uani 1 1 d . . . O2 O -0.02627(8) 0.00454(13) 0.37553(6) 0.0162(2) Uani 1 1 d . . . O3 O 0.14364(8) -0.03858(12) 0.34643(6) 0.0147(2) Uani 1 1 d . . . O4 O 0.0000 -0.19782(18) 0.2500 0.0205(4) Uani 1 2 d SD . . H4 H 0.0361(15) -0.256(2) 0.2782(11) 0.050 Uiso 1 1 d D . . O5 O 0.05392(8) 0.28773(12) 0.32792(6) 0.0175(3) Uani 1 1 d . . . O6 O 0.09914(8) 0.55956(12) 0.33063(6) 0.0158(2) Uani 1 1 d . . . O7 O -0.04573(8) 0.48451(14) 0.36336(6) 0.0198(3) Uani 1 1 d . . . C1 C -0.17093(12) 0.1299(2) 0.34118(9) 0.0187(4) Uani 1 1 d . . . H1A H -0.2379 0.1309 0.3440 0.022 Uiso 1 1 calc R . . H1B H -0.1409 0.2271 0.3626 0.022 Uiso 1 1 calc R . . C2 C -0.12167(12) -0.0080(2) 0.38061(9) 0.0189(4) Uani 1 1 d . . . H2A H -0.1259 -0.0051 0.4303 0.023 Uiso 1 1 calc R . . H2B H -0.1500 -0.1063 0.3592 0.023 Uiso 1 1 calc R . . C3 C 0.03397(12) -0.11291(18) 0.41349(8) 0.0173(3) Uani 1 1 d . . . H3A H 0.0210 -0.2145 0.3893 0.021 Uiso 1 1 calc R . . H3B H 0.0237 -0.1235 0.4615 0.021 Uiso 1 1 calc R . . C4 C 0.13285(12) -0.06274(18) 0.41647(8) 0.0173(3) Uani 1 1 d . . . H4A H 0.1468 0.0349 0.4438 0.021 Uiso 1 1 calc R . . H4B H 0.1776 -0.1436 0.4400 0.021 Uiso 1 1 calc R . . C5 C 0.23155(12) 0.03731(19) 0.34705(9) 0.0179(3) Uani 1 1 d . . . H5A H 0.2843 -0.0196 0.3780 0.021 Uiso 1 1 calc R . . H5B H 0.2308 0.1450 0.3649 0.021 Uiso 1 1 calc R . . C6 C 0.24399(12) 0.0391(2) 0.27333(9) 0.0198(4) Uani 1 1 d . . . H6A H 0.3039 0.0914 0.2716 0.024 Uiso 1 1 calc R . . H6B H 0.2458 -0.0685 0.2557 0.024 Uiso 1 1 calc R . . C7 C 0.11327(12) 0.41985(18) 0.44752(9) 0.0170(3) Uani 1 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 Ca1 0.0106(2) 0.0098(2) 0.0116(2) 0.000 0.00162(17) 0.000 S1 0.0103(2) 0.01137(18) 0.01135(19) -0.00026(13) 0.00070(15) -0.00035(14) F1 0.0387(7) 0.0228(5) 0.0160(5) -0.0070(4) -0.0022(5) 0.0030(5) F2 0.0420(7) 0.0283(5) 0.0190(5) 0.0091(4) 0.0088(5) -0.0039(5) F3 0.0168(5) 0.0326(6) 0.0228(6) 0.0016(4) -0.0060(4) 0.0063(4) O1 0.0117(6) 0.0219(6) 0.0141(6) -0.0030(4) 0.0022(5) -0.0037(5) O2 0.0140(6) 0.0169(5) 0.0183(6) 0.0026(5) 0.0048(5) 0.0000(5) O3 0.0135(6) 0.0167(5) 0.0133(6) 0.0002(4) 0.0017(5) -0.0001(4) O4 0.0270(10) 0.0110(8) 0.0170(9) 0.000 -0.0082(8) 0.000 O5 0.0203(6) 0.0131(5) 0.0171(6) -0.0028(4) 0.0007(5) -0.0005(5) O6 0.0154(6) 0.0147(5) 0.0168(6) 0.0040(4) 0.0026(5) -0.0015(4) O7 0.0115(6) 0.0232(6) 0.0241(6) -0.0014(5) 0.0029(5) 0.0014(5) C1 0.0140(8) 0.0250(8) 0.0176(8) -0.0061(7) 0.0050(7) -0.0023(7) C2 0.0142(9) 0.0277(9) 0.0155(8) -0.0021(7) 0.0050(7) -0.0069(7) C3 0.0231(9) 0.0152(7) 0.0132(8) 0.0025(6) 0.0031(7) 0.0004(7) C4 0.0212(9) 0.0188(8) 0.0102(8) 0.0020(6) 0.0005(7) 0.0016(7) C5 0.0109(8) 0.0249(8) 0.0165(8) -0.0006(6) 0.0007(7) 0.0015(7) C6 0.0114(8) 0.0288(9) 0.0181(9) 0.0030(7) 0.0009(7) 0.0053(7) C7 0.0189(9) 0.0155(7) 0.0152(8) 0.0017(6) 0.0012(7) -0.0003(6) _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 O4 2.3478(17) . ? Ca1 O5 2.3919(12) . ? Ca1 O5 2.3919(12) 2 ? Ca1 O1 2.5551(12) 2 ? Ca1 O1 2.5551(12) . ? Ca1 O2 2.6471(14) 2 ? Ca1 O2 2.6471(14) . ? Ca1 O3 2.6574(14) 2 ? Ca1 O3 2.6574(14) . ? S1 O7 1.4302(12) . ? S1 O6 1.4431(11) . ? S1 O5 1.4456(11) . ? S1 C7 1.8227(19) . ? F1 C7 1.3341(18) . ? F2 C7 1.3293(19) . ? F3 C7 1.338(2) . ? O1 C6 1.435(2) 2 ? O1 C1 1.438(2) . ? O2 C2 1.4207(19) . ? O2 C3 1.4275(19) . ? O3 C4 1.4326(19) . ? O3 C5 1.435(2) . ? O4 H4 0.833(15) . ? C1 C2 1.503(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.492(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.497(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O1 1.435(2) 2 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? 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 # added by hand O4 Ca1 O5 139.75(3) . . ? O4 Ca1 O5 139.75(3) . 2 ? O5 Ca1 O5 80.50(6) . 2 ? O4 Ca1 O1 99.03(3) . 2 ? O5 Ca1 O1 78.02(4) . 2 ? O5 Ca1 O1 88.16(4) 2 2 ? O4 Ca1 O1 99.03(3) . . ? O5 Ca1 O1 88.16(4) . . ? O5 Ca1 O1 78.02(4) 2 . ? O1 Ca1 O1 161.93(5) 2 . ? O4 Ca1 O2 76.71(3) . 2 ? O5 Ca1 O2 132.18(4) . 2 ? O5 Ca1 O2 71.31(4) 2 2 ? O1 Ca1 O2 63.59(4) 2 2 ? O1 Ca1 O2 121.13(4) . 2 ? O4 Ca1 O2 76.71(3) . . ? O5 Ca1 O2 71.31(4) . . ? O5 Ca1 O2 132.18(4) 2 . ? O1 Ca1 O2 121.13(4) 2 . ? O1 Ca1 O2 63.59(4) . . ? O2 Ca1 O2 153.42(5) 2 . ? O4 Ca1 O3 68.38(3) . 2 ? O5 Ca1 O3 145.27(4) . 2 ? O5 Ca1 O3 74.96(4) 2 2 ? O1 Ca1 O3 124.60(4) 2 2 ? O1 Ca1 O3 63.12(4) . 2 ? O2 Ca1 O3 61.01(4) 2 2 ? O2 Ca1 O3 108.38(4) . 2 ? O4 Ca1 O3 68.38(3) . . ? O5 Ca1 O3 74.96(4) . . ? O5 Ca1 O3 145.27(4) 2 . ? O1 Ca1 O3 63.12(4) 2 . ? O1 Ca1 O3 124.60(4) . . ? O2 Ca1 O3 108.38(4) 2 . ? O2 Ca1 O3 61.01(4) . . ? O3 Ca1 O3 136.76(5) 2 . ? O7 S1 O6 115.66(7) . . ? O7 S1 O5 115.61(7) . . ? O6 S1 O5 114.15(7) . . ? O7 S1 C7 103.80(8) . . ? O6 S1 C7 102.14(7) . . ? O5 S1 C7 102.85(7) . . ? C6 O1 C1 111.80(12) 2 . ? C6 O1 Ca1 119.37(9) 2 . ? C1 O1 Ca1 114.91(10) . . ? C2 O2 C3 113.73(12) . . ? C2 O2 Ca1 116.02(9) . . ? C3 O2 Ca1 116.24(9) . . ? C4 O3 C5 110.81(13) . . ? C4 O3 Ca1 119.36(10) . . ? C5 O3 Ca1 113.06(9) . . ? Ca1 O4 H4 126.6(16) . . ? H4 O4 H4 106.7(32) . 2 ? S1 O5 Ca1 154.33(8) . . ? O1 C1 C2 109.85(13) . . ? O1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? O1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? O2 C2 C1 105.17(13) . . ? O2 C2 H2A 110.7 . . ? C1 C2 H2A 110.7 . . ? O2 C2 H2B 110.7 . . ? C1 C2 H2B 110.7 . . ? H2A C2 H2B 108.8 . . ? O2 C3 C4 106.65(13) . . ? O2 C3 H3A 110.4 . . ? C4 C3 H3A 110.4 . . ? O2 C3 H3B 110.4 . . ? C4 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? O3 C4 C3 108.99(14) . . ? O3 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? O3 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? O3 C5 C6 107.79(14) . . ? O3 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? O3 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.5 . . ? O1 C6 C5 107.57(13) 2 . ? O1 C6 H6A 110.2 2 . ? C5 C6 H6A 110.2 . . ? O1 C6 H6B 110.2 2 . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? F2 C7 F1 107.73(13) . . ? F2 C7 F3 107.31(13) . . ? F1 C7 F3 107.30(14) . . ? F2 C7 S1 112.13(12) . . ? F1 C7 S1 110.91(11) . . ? F3 C7 S1 111.23(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 O1 C1 C2 89.97(16) 2 . . . ? Ca1 O1 C1 C2 -50.22(15) . . . . ? C3 O2 C2 C1 176.74(13) . . . . ? Ca1 O2 C2 C1 -44.49(14) . . . . ? O1 C1 C2 O2 61.42(17) . . . . ? C2 O2 C3 C4 -167.29(13) . . . . ? Ca1 O2 C3 C4 54.04(14) . . . . ? C5 O3 C4 C3 169.15(12) . . . . ? Ca1 O3 C4 C3 35.15(15) . . . . ? O2 C3 C4 O3 -56.25(16) . . . . ? C4 O3 C5 C6 172.42(13) . . . . ? Ca1 O3 C5 C6 -50.54(14) . . . . ? O3 C5 C6 O1 59.47(17) . . . 2 ? O7 S1 C7 F2 59.69(13) . . . . ? O6 S1 C7 F2 -179.72(11) . . . . ? O5 S1 C7 F2 -61.14(13) . . . . ? O7 S1 C7 F1 -60.80(13) . . . . ? O6 S1 C7 F1 59.80(13) . . . . ? O5 S1 C7 F1 178.37(11) . . . . ? O7 S1 C7 F3 179.86(11) . . . . ? O6 S1 C7 F3 -59.55(12) . . . . ? O5 S1 C7 F3 59.03(12) . . . . ? 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 O4 H4 O6 0.833(15) 1.995(16) 2.8046(17) 164(2) 1_545 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.351 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.059 data_11paf018a _database_code_depnum_ccdc_archive 'CCDC 891791' #TrackingRef '- CaSr_all11_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-11-23 _audit_author_name 'Webster, M.' _chemical_name_systematic ; 1,4,10,13-tetraoxa-7,16-dithiacyclooctadecane- bis(trifluoromethanesulfonate)calcium(II) ; # C12H24O4S2 = [18]aneO4S2 # 1,4,10,13-tetraoxo-7,16-dithia-cyclo-octadecane # 1,4,10,13-tetraoxa-7,16-dithiacyclooctadecane (iLab defaults) # 1,4,10,13-tetraoxa-7,16-dithiacyclooctadecane (iLab selected options) # # [F3CSO3]- = triflate anion # trifluoromethanesulphonate (from CSD search - very few hits(2?)) # trifluoromethanesulfonate (from CSD search - many hits with 'f' spelling) # trifluoromethanesulfonate (iLab defaults & selected options) _chemical_name_common ; 1,4,10,13-tetraoxa-7,16-dithiacyclooctadecane- bis(trifluoromethanesulfonate)calcium(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C14 H24 Ca F6 O10 S4' _chemical_formula_sum 'C14 H24 Ca F6 O10 S4' _chemical_formula_structural '(C12 H24 O4 S2) (C F3 O3 S)2 Ca' _chemical_formula_weight 634.65 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' F F 0.0171 0.0103 '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 orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 14.855(4) _cell_length_b 9.400(3) _cell_length_c 17.855(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2493.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10478 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.678 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.651 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12107 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5639 _reflns_number_gt 4479 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. C2 and C9 which had very elongated displacement ellipsoids were modelled as having two site (C2A/B and C9A/B) with isotropic displacement parameters, the proportions (A/B) was allowd to refine and H atoms were included. The DFIX command was used to control C-C distances in the disordered model. A TWIN/BASF command was also used. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+2.0503P] 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 constr _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 0.21(5) _refine_ls_number_reflns 5639 _refine_ls_number_parameters 317 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.046 _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 0.38132(5) 0.62396(8) 0.75193(5) 0.01879(17) Uani 1 1 d . A . S1 S 0.51507(7) 0.39561(11) 0.73089(6) 0.0284(3) Uani 1 1 d . . . S2 S 0.34309(7) 0.93305(11) 0.75499(7) 0.0265(2) Uani 1 1 d . . . S3 S 0.47895(6) 0.69971(11) 0.56423(6) 0.0198(2) Uani 1 1 d . A . S4 S 0.57616(6) 0.80737(11) 0.83919(6) 0.0206(2) Uani 1 1 d . A . F1 F 0.5774(3) 0.9065(4) 0.5108(2) 0.0811(13) Uani 1 1 d . A . F2 F 0.5886(3) 0.8746(5) 0.6302(3) 0.0903(14) Uani 1 1 d . A . F3 F 0.4727(3) 0.9739(3) 0.58463(17) 0.0643(11) Uani 1 1 d . A . F4 F 0.6359(2) 0.8470(4) 0.97542(18) 0.0547(9) Uani 1 1 d . A . F5 F 0.59349(18) 0.6324(3) 0.95258(16) 0.0448(8) Uani 1 1 d . A . F6 F 0.49490(19) 0.7966(3) 0.96966(16) 0.0474(8) Uani 1 1 d . A . O1 O 0.37080(19) 0.4423(3) 0.85079(18) 0.0280(7) Uani 1 1 d . . . O2 O 0.29174(19) 0.6967(3) 0.86119(19) 0.0316(8) Uani 1 1 d D . . O3 O 0.24126(19) 0.6869(3) 0.67815(19) 0.0341(8) Uani 1 1 d . . . O4 O 0.3226(2) 0.4203(4) 0.6773(3) 0.0529(11) Uani 1 1 d D . . O5 O 0.4372(2) 0.6862(4) 0.63684(18) 0.0375(8) Uani 1 1 d . . . O6 O 0.5511(2) 0.6044(4) 0.5514(2) 0.0452(10) Uani 1 1 d . . . O7 O 0.4169(2) 0.7166(3) 0.50408(19) 0.0358(8) Uani 1 1 d . . . O8 O 0.50723(18) 0.7102(3) 0.81237(17) 0.0253(7) Uani 1 1 d . . . O9 O 0.66565(18) 0.7711(3) 0.81721(17) 0.0306(7) Uani 1 1 d . . . O10 O 0.5525(2) 0.9545(3) 0.8346(2) 0.0377(8) Uani 1 1 d . . . C1A C 0.3028(3) 0.4599(5) 0.9047(2) 0.0280(10) Uani 0.50 1 d PD A 1 H1AW H 0.3189 0.4025 0.9492 0.034 Uiso 0.50 1 calc PR A 1 H1AX H 0.2463 0.4200 0.8841 0.034 Uiso 0.50 1 calc PR A 1 C2A C 0.2843(9) 0.6076(12) 0.9300(7) 0.033(4) Uiso 0.357(11) 1 d PD A 1 H2AY H 0.3289 0.6379 0.9680 0.040 Uiso 0.357(11) 1 calc PR A 1 H2AZ H 0.2232 0.6149 0.9519 0.040 Uiso 0.357(11) 1 calc PR A 1 C1B C 0.3028(3) 0.4599(5) 0.9047(2) 0.0280(10) Uani 0.50 1 d PD A 2 H1BW H 0.3301 0.4874 0.9531 0.034 Uiso 0.50 1 calc PR A 2 H1BX H 0.2705 0.3688 0.9119 0.034 Uiso 0.50 1 calc PR A 2 C2B C 0.2388(4) 0.5699(7) 0.8808(4) 0.0232(19) Uiso 0.643(11) 1 d PD A 2 H2BY H 0.2039 0.5367 0.8369 0.028 Uiso 0.643(11) 1 calc PR A 2 H2BZ H 0.1963 0.5921 0.9219 0.028 Uiso 0.643(11) 1 calc PR A 2 C3 C 0.2536(4) 0.8292(6) 0.8809(4) 0.0595(19) Uani 1 1 d . A . H3A H 0.2484 0.8362 0.9360 0.071 Uiso 1 1 calc R . . H3B H 0.1924 0.8372 0.8592 0.071 Uiso 1 1 calc R . . C4 C 0.3118(3) 0.9476(5) 0.8519(3) 0.0396(12) Uani 1 1 d . A . H4A H 0.3673 0.9515 0.8825 0.048 Uiso 1 1 calc R . . H4B H 0.2794 1.0387 0.8592 0.048 Uiso 1 1 calc R . . C5 C 0.2331(4) 0.9340(6) 0.7104(4) 0.0586(18) Uani 1 1 d . A . H5A H 0.1863 0.9123 0.7482 0.070 Uiso 1 1 calc R . . H5B H 0.2208 1.0299 0.6900 0.070 Uiso 1 1 calc R . . C6 C 0.2283(4) 0.8278(6) 0.6490(3) 0.0478(15) Uani 1 1 d . A . H6A H 0.1688 0.8339 0.6241 0.057 Uiso 1 1 calc R . . H6B H 0.2752 0.8488 0.6112 0.057 Uiso 1 1 calc R . . C7 C 0.2195(3) 0.5832(6) 0.6226(3) 0.0409(14) Uani 1 1 d . A . H7A H 0.2609 0.5920 0.5794 0.049 Uiso 1 1 calc R . . H7B H 0.1571 0.5977 0.6046 0.049 Uiso 1 1 calc R . . C8 C 0.2285(3) 0.4396(6) 0.6574(3) 0.0457(15) Uani 1 1 d . A . H8A H 0.1902 0.4329 0.7026 0.055 Uiso 1 1 calc R . . H8B H 0.2094 0.3651 0.6215 0.055 Uiso 1 1 calc R . . C9A C 0.3456(4) 0.2825(7) 0.6824(4) 0.028(2) Uiso 0.639(13) 1 d PD A 1 H9AY H 0.3160 0.2274 0.6421 0.033 Uiso 0.639(13) 1 calc PR A 1 H9AZ H 0.3260 0.2435 0.7313 0.033 Uiso 0.639(13) 1 calc PR A 1 C10A C 0.4527(3) 0.2709(5) 0.6747(3) 0.0419(13) Uani 0.50 1 d PD A 1 H10W H 0.4692 0.2853 0.6215 0.050 Uiso 0.50 1 calc PR A 1 H10X H 0.4713 0.1734 0.6888 0.050 Uiso 0.50 1 calc PR A 1 C9B C 0.3763(8) 0.3353(15) 0.6395(8) 0.036(4) Uiso 0.361(13) 1 d PD A 2 H9BY H 0.3990 0.3899 0.5959 0.043 Uiso 0.361(13) 1 calc PR A 2 H9BZ H 0.3387 0.2574 0.6192 0.043 Uiso 0.361(13) 1 calc PR A 2 C10B C 0.4527(3) 0.2709(5) 0.6747(3) 0.0419(13) Uani 0.50 1 d PD A 2 H10Y H 0.4928 0.2310 0.6357 0.050 Uiso 0.50 1 calc PR A 2 H10Z H 0.4321 0.1914 0.7068 0.050 Uiso 0.50 1 calc PR A 2 C11 C 0.5078(4) 0.3173(6) 0.8231(3) 0.0465(14) Uani 1 1 d . A . H11A H 0.5302 0.2182 0.8201 0.056 Uiso 1 1 calc R . . H11B H 0.5489 0.3701 0.8568 0.056 Uiso 1 1 calc R . . C12 C 0.4189(4) 0.3146(6) 0.8574(3) 0.0543(17) Uani 1 1 d . A . H12A H 0.3833 0.2374 0.8341 0.065 Uiso 1 1 calc R . . H12B H 0.4256 0.2916 0.9112 0.065 Uiso 1 1 calc R . . C13 C 0.5321(3) 0.8732(6) 0.5723(3) 0.0410(12) Uani 1 1 d . . . C14 C 0.5752(3) 0.7701(5) 0.9395(3) 0.0310(11) Uani 1 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 Ca1 0.0141(3) 0.0137(3) 0.0286(4) -0.0021(4) 0.0010(4) -0.0006(3) S1 0.0219(5) 0.0204(5) 0.0430(7) -0.0015(5) 0.0098(5) 0.0025(4) S2 0.0244(5) 0.0178(5) 0.0373(6) 0.0018(5) -0.0067(5) 0.0030(4) S3 0.0200(5) 0.0195(5) 0.0199(5) -0.0014(4) -0.0063(4) 0.0007(4) S4 0.0183(5) 0.0179(5) 0.0255(5) -0.0017(4) 0.0008(4) -0.0026(4) F1 0.109(3) 0.065(3) 0.069(3) -0.015(2) 0.053(2) -0.043(2) F2 0.079(3) 0.100(3) 0.091(3) -0.028(3) -0.031(2) -0.050(2) F3 0.128(3) 0.0199(16) 0.045(2) -0.0053(13) 0.0259(19) 0.0018(18) F4 0.0484(18) 0.079(2) 0.0371(17) -0.0227(17) -0.0103(14) -0.0086(17) F5 0.0435(17) 0.0486(19) 0.0422(18) 0.0179(14) 0.0066(13) 0.0129(14) F6 0.0407(16) 0.067(2) 0.0342(16) -0.0062(16) 0.0144(13) 0.0138(15) O1 0.0322(16) 0.0173(15) 0.0343(18) 0.0089(13) 0.0091(14) 0.0076(13) O2 0.0260(15) 0.0181(16) 0.051(2) 0.0086(15) 0.0167(14) 0.0065(13) O3 0.0187(15) 0.0377(19) 0.046(2) -0.0201(17) -0.0029(14) -0.0007(14) O4 0.0244(17) 0.043(2) 0.091(3) -0.044(2) 0.0000(19) -0.0080(16) O5 0.050(2) 0.039(2) 0.0242(17) 0.0026(16) 0.0004(15) -0.0035(17) O6 0.044(2) 0.044(2) 0.048(2) -0.0132(18) -0.0147(17) 0.0275(17) O7 0.0343(18) 0.040(2) 0.0335(19) -0.0011(15) -0.0150(15) 0.0018(15) O8 0.0209(15) 0.0221(16) 0.0329(17) -0.0003(13) -0.0032(12) -0.0043(12) O9 0.0189(14) 0.0409(19) 0.0321(18) -0.0005(14) 0.0030(13) -0.0033(14) O10 0.0429(18) 0.0164(15) 0.054(2) -0.0003(16) -0.0026(17) -0.0001(14) C1A 0.035(2) 0.031(3) 0.018(2) 0.0020(18) 0.0075(18) 0.001(2) C1B 0.035(2) 0.031(3) 0.018(2) 0.0020(18) 0.0075(18) 0.001(2) C3 0.053(3) 0.032(3) 0.093(5) 0.011(3) 0.044(3) 0.019(3) C4 0.040(3) 0.023(2) 0.056(3) -0.010(2) 0.006(3) 0.014(2) C5 0.051(3) 0.040(3) 0.085(5) -0.024(3) -0.041(3) 0.022(3) C6 0.041(3) 0.045(3) 0.057(4) -0.014(3) -0.029(3) 0.018(3) C7 0.023(2) 0.051(3) 0.049(3) -0.031(3) 0.001(2) -0.004(2) C8 0.023(2) 0.039(3) 0.075(4) -0.027(3) -0.004(2) -0.010(2) C10A 0.049(3) 0.025(3) 0.052(4) -0.018(2) 0.010(3) 0.006(2) C10B 0.049(3) 0.025(3) 0.052(4) -0.018(2) 0.010(3) 0.006(2) C11 0.051(3) 0.045(3) 0.043(3) 0.002(3) -0.009(3) 0.027(3) C12 0.091(4) 0.037(3) 0.035(3) 0.017(3) 0.024(3) 0.039(3) C13 0.049(3) 0.044(3) 0.030(3) -0.010(2) 0.009(2) -0.017(3) C14 0.026(2) 0.041(3) 0.026(2) -0.005(2) -0.002(2) 0.000(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 O5 2.292(3) . ? Ca1 O8 2.307(3) . ? Ca1 O2 2.458(3) . ? Ca1 O1 2.461(3) . ? Ca1 O4 2.491(3) . ? Ca1 O3 2.533(3) . ? Ca1 S1 2.9489(14) . ? Ca1 S2 2.9611(14) . ? S1 C10A 1.800(5) . ? S1 C11 1.808(6) . ? S2 C4 1.798(5) . ? S2 C5 1.817(5) . ? S3 O6 1.416(3) . ? S3 O7 1.424(3) . ? S3 O5 1.443(3) . ? S3 C13 1.818(5) . ? S4 O9 1.427(3) . ? S4 O10 1.430(3) . ? S4 O8 1.453(3) . ? S4 C14 1.825(5) . ? F1 C13 1.326(6) . ? F2 C13 1.331(7) . ? F3 C13 1.313(6) . ? F4 C14 1.322(5) . ? F5 C14 1.343(5) . ? F6 C14 1.332(5) . ? O1 C12 1.402(5) . ? O1 C1A 1.405(5) . ? O2 C3 1.413(6) . ? O2 C2B 1.470(7) . ? O2 C2A 1.491(11) . ? O3 C7 1.428(5) . ? O3 C6 1.436(6) . ? O4 C9B 1.315(11) . ? O4 C9A 1.342(7) . ? O4 C8 1.453(6) . ? C1A C2A 1.486(11) . ? C1A H1AW 0.9900 . ? C1A H1AX 0.9900 . ? C2A H2AY 0.9900 . ? C2A H2AZ 0.9900 . ? C2B H2BY 0.9900 . ? C2B H2BZ 0.9900 . ? C3 C4 1.501(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.484(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.492(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9A C10A 1.601(8) . ? C9A H9AY 0.9900 . ? C9A H9AZ 0.9900 . ? C10A H10W 0.9900 . ? C10A H10X 0.9900 . ? C9B H9BY 0.9900 . ? C9B H9BZ 0.9900 . ? C11 C12 1.456(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? 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 O5 Ca1 O8 92.05(12) . . ? O5 Ca1 O2 146.78(12) . . ? O8 Ca1 O2 88.28(11) . . ? O5 Ca1 O1 147.46(11) . . ? O8 Ca1 O1 87.71(11) . . ? O2 Ca1 O1 65.76(10) . . ? O5 Ca1 O4 80.97(14) . . ? O8 Ca1 O4 143.57(11) . . ? O2 Ca1 O4 116.68(12) . . ? O1 Ca1 O4 80.11(14) . . ? O5 Ca1 O3 76.81(12) . . ? O8 Ca1 O3 145.82(11) . . ? O2 Ca1 O3 84.44(11) . . ? O1 Ca1 O3 118.88(11) . . ? O4 Ca1 O3 67.27(11) . . ? O5 Ca1 S1 80.06(9) . . ? O8 Ca1 S1 76.66(8) . . ? O2 Ca1 S1 131.93(8) . . ? O1 Ca1 S1 68.22(7) . . ? O4 Ca1 S1 66.93(9) . . ? O3 Ca1 S1 131.09(8) . . ? O5 Ca1 S2 80.54(9) . . ? O8 Ca1 S2 78.57(8) . . ? O2 Ca1 S2 66.96(7) . . ? O1 Ca1 S2 130.96(8) . . ? O4 Ca1 S2 134.19(10) . . ? O3 Ca1 S2 67.84(7) . . ? S1 Ca1 S2 147.76(4) . . ? C10A S1 C11 102.2(3) . . ? C10A S1 Ca1 101.44(16) . . ? C11 S1 Ca1 98.07(16) . . ? C4 S2 C5 100.9(3) . . ? C4 S2 Ca1 98.18(16) . . ? C5 S2 Ca1 99.73(18) . . ? O6 S3 O7 116.0(2) . . ? O6 S3 O5 114.5(2) . . ? O7 S3 O5 114.2(2) . . ? O6 S3 C13 104.6(2) . . ? O7 S3 C13 104.0(2) . . ? O5 S3 C13 101.2(2) . . ? O9 S4 O10 116.38(19) . . ? O9 S4 O8 114.55(18) . . ? O10 S4 O8 114.58(18) . . ? O9 S4 C14 103.4(2) . . ? O10 S4 C14 103.9(2) . . ? O8 S4 C14 101.4(2) . . ? C12 O1 C1A 114.2(3) . . ? C12 O1 Ca1 128.5(3) . . ? C1A O1 Ca1 117.1(2) . . ? C3 O2 C2B 116.2(4) . . ? C3 O2 C2A 105.1(5) . . ? C2B O2 C2A 46.2(5) . . ? C3 O2 Ca1 131.3(3) . . ? C2B O2 Ca1 104.7(3) . . ? C2A O2 Ca1 122.5(5) . . ? C7 O3 C6 110.3(4) . . ? C7 O3 Ca1 112.8(3) . . ? C6 O3 Ca1 120.9(3) . . ? C9B O4 C9A 45.2(7) . . ? C9B O4 C8 122.3(6) . . ? C9A O4 C8 112.4(4) . . ? C9B O4 Ca1 121.9(6) . . ? C9A O4 Ca1 128.0(4) . . ? C8 O4 Ca1 111.8(3) . . ? S3 O5 Ca1 169.7(2) . . ? S4 O8 Ca1 161.18(18) . . ? O1 C1A C2A 116.8(6) . . ? O1 C1A H1AW 108.1 . . ? C2A C1A H1AW 108.1 . . ? O1 C1A H1AX 108.1 . . ? C2A C1A H1AX 108.1 . . ? H1AW C1A H1AX 107.3 . . ? C1A C2A O2 105.1(8) . . ? C1A C2A H2AY 110.7 . . ? O2 C2A H2AY 110.7 . . ? C1A C2A H2AZ 110.7 . . ? O2 C2A H2AZ 110.7 . . ? H2AY C2A H2AZ 108.8 . . ? O2 C2B H2BY 110.3 . . ? O2 C2B H2BZ 110.3 . . ? H2BY C2B H2BZ 108.5 . . ? O2 C3 C4 109.7(4) . . ? O2 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? O2 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C3 C4 S2 115.1(4) . . ? C3 C4 H4A 108.5 . . ? S2 C4 H4A 108.5 . . ? C3 C4 H4B 108.5 . . ? S2 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C6 C5 S2 111.3(4) . . ? C6 C5 H5A 109.4 . . ? S2 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? S2 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? O3 C6 C5 110.2(5) . . ? O3 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? O3 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? O3 C7 C8 107.9(4) . . ? O3 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? O3 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? O4 C8 C7 107.6(4) . . ? O4 C8 H8A 110.2 . . ? C7 C8 H8A 110.2 . . ? O4 C8 H8B 110.2 . . ? C7 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? O4 C9A C10A 108.2(5) . . ? O4 C9A H9AY 110.1 . . ? C10A C9A H9AY 110.1 . . ? O4 C9A H9AZ 110.1 . . ? C10A C9A H9AZ 110.1 . . ? H9AY C9A H9AZ 108.4 . . ? C9A C10A S1 114.8(4) . . ? C9A C10A H10W 108.6 . . ? S1 C10A H10W 108.6 . . ? C9A C10A H10X 108.6 . . ? S1 C10A H10X 108.6 . . ? H10W C10A H10X 107.5 . . ? O4 C9B H9BY 107.1 . . ? O4 C9B H9BZ 107.1 . . ? H9BY C9B H9BZ 106.8 . . ? C12 C11 S1 116.4(4) . . ? C12 C11 H11A 108.2 . . ? S1 C11 H11A 108.2 . . ? C12 C11 H11B 108.2 . . ? S1 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? O1 C12 C11 114.4(5) . . ? O1 C12 H12A 108.7 . . ? C11 C12 H12A 108.7 . . ? O1 C12 H12B 108.7 . . ? C11 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? F3 C13 F1 108.1(5) . . ? F3 C13 F2 106.7(4) . . ? F1 C13 F2 108.7(4) . . ? F3 C13 S3 111.6(3) . . ? F1 C13 S3 111.5(3) . . ? F2 C13 S3 110.1(4) . . ? F4 C14 F6 108.2(4) . . ? F4 C14 F5 107.7(4) . . ? F6 C14 F5 106.9(4) . . ? F4 C14 S4 111.4(3) . . ? F6 C14 S4 111.6(3) . . ? F5 C14 S4 110.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 O1 C1A C2A 147.1(7) . . . . ? Ca1 O1 C1A C2A -38.3(7) . . . . ? O1 C1A C2A O2 39.1(10) . . . . ? C3 O2 C2A C1A 166.3(6) . . . . ? C2B O2 C2A C1A 54.4(6) . . . . ? Ca1 O2 C2A C1A -24.4(10) . . . . ? C2B O2 C3 C4 -175.6(5) . . . . ? C2A O2 C3 C4 136.1(7) . . . . ? Ca1 O2 C3 C4 -31.8(8) . . . . ? O2 C3 C4 S2 49.5(6) . . . . ? C5 S2 C4 C3 60.1(4) . . . . ? Ca1 S2 C4 C3 -41.5(4) . . . . ? C4 S2 C5 C6 -138.2(5) . . . . ? Ca1 S2 C5 C6 -37.8(5) . . . . ? C7 O3 C6 C5 168.8(4) . . . . ? Ca1 O3 C6 C5 -56.4(5) . . . . ? S2 C5 C6 O3 62.1(6) . . . . ? C6 O3 C7 C8 -176.5(4) . . . . ? Ca1 O3 C7 C8 44.9(4) . . . . ? C9B O4 C8 C7 -106.5(9) . . . . ? C9A O4 C8 C7 -156.7(5) . . . . ? Ca1 O4 C8 C7 51.3(5) . . . . ? O3 C7 C8 O4 -64.2(5) . . . . ? C9B O4 C9A C10A 46.0(8) . . . . ? C8 O4 C9A C10A 159.8(5) . . . . ? Ca1 O4 C9A C10A -53.8(7) . . . . ? O4 C9A C10A S1 46.8(7) . . . . ? C11 S1 C10A C9A 77.1(5) . . . . ? Ca1 S1 C10A C9A -23.9(5) . . . . ? C10A S1 C11 C12 -67.3(5) . . . . ? Ca1 S1 C11 C12 36.3(5) . . . . ? C1A O1 C12 C11 -157.8(4) . . . . ? Ca1 O1 C12 C11 28.4(7) . . . . ? S1 C11 C12 O1 -44.9(7) . . . . ? O6 S3 C13 F3 -179.9(4) . . . . ? O7 S3 C13 F3 58.0(4) . . . . ? O5 S3 C13 F3 -60.6(4) . . . . ? O6 S3 C13 F1 59.2(5) . . . . ? O7 S3 C13 F1 -62.9(4) . . . . ? O5 S3 C13 F1 178.4(4) . . . . ? O6 S3 C13 F2 -61.6(4) . . . . ? O7 S3 C13 F2 176.3(4) . . . . ? O5 S3 C13 F2 57.7(4) . . . . ? O9 S4 C14 F4 59.8(4) . . . . ? O10 S4 C14 F4 -62.2(4) . . . . ? O8 S4 C14 F4 178.7(3) . . . . ? O9 S4 C14 F6 -179.1(3) . . . . ? O10 S4 C14 F6 58.9(4) . . . . ? O8 S4 C14 F6 -60.2(4) . . . . ? O9 S4 C14 F5 -60.1(3) . . . . ? O10 S4 C14 F5 177.9(3) . . . . ? O8 S4 C14 F5 58.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.469 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.082 data_11paf027a _database_code_depnum_ccdc_archive 'CCDC 891792' #TrackingRef '- CaSr_all11_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-11-25 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Diiodo(1,10-dioxa-4,7,13,16-tetrathiacyclooctadecane)calcium(II) dichloromethane solvate ; # C12H24O2S4 = [18]aneO2S4 # 1,10-dioxa-4,7,13,16-tetrathiacyclooctadecane # 1,10-dioxa-4,7,13,16-tetrathiacyclooctadecane (Chemspider) # SMILES: C1CSCCSCCOCCSCCSCCO1 _chemical_name_common ; Diiodo(1,10-dioxa-4,7,13,16- tetrathiacyclooctadecane)calcium(ii) dichloromethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Ca I2 O2 S4, 0.5(C H2 Cl2)' _chemical_formula_sum 'C12.50 H25 Ca Cl I2 O2 S4' _chemical_formula_weight 664.90 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' 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 17.076(4) _cell_length_b 8.2970(18) _cell_length_c 15.745(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.464(12) _cell_angle_gamma 90.00 _cell_volume 2230.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7259 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.6 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 3.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.254 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'confocal ' _diffrn_measurement_device_type 'Rigaku AFC12 (Right): Kappa 3-circle. Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10627 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0924 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5065 _reflns_number_gt 3498 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+4.7887P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5065 _refine_ls_number_parameters 208 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Ca1 Ca 0.23915(9) 0.49574(17) 0.29026(8) 0.0204(3) Uani 1 1 d . . . I1 I 0.37260(3) 0.28377(6) 0.21780(3) 0.02280(13) Uani 1 1 d . . . I2 I 0.11683(3) 0.41170(6) 0.14685(3) 0.02905(15) Uani 1 1 d . . . S1 S 0.17071(13) 0.1897(2) 0.34838(11) 0.0261(4) Uani 1 1 d . . . S2 S 0.13041(12) 0.5524(2) 0.43114(11) 0.0249(4) Uani 1 1 d . . . S3 S 0.30311(13) 0.7039(2) 0.15922(11) 0.0260(4) Uani 1 1 d . . . S4 S 0.33997(12) 0.7346(2) 0.37213(11) 0.0251(4) Uani 1 1 d . . . O1 O 0.3075(3) 0.3925(6) 0.4309(3) 0.0228(11) Uani 1 1 d . . . O2 O 0.1618(3) 0.7718(6) 0.2736(3) 0.0258(12) Uani 1 1 d . . . C1 C 0.2703(5) 0.2756(9) 0.4853(4) 0.0259(17) Uani 1 1 d . . . H1A H 0.2260 0.3266 0.5145 0.031 Uiso 1 1 calc R . . H1B H 0.3084 0.2365 0.5290 0.031 Uiso 1 1 calc R . . C2 C 0.2409(5) 0.1363(9) 0.4321(4) 0.0279(18) Uani 1 1 d . . . H2A H 0.2164 0.0567 0.4699 0.033 Uiso 1 1 calc R . . H2B H 0.2864 0.0834 0.4061 0.033 Uiso 1 1 calc R . . C3 C 0.0831(5) 0.2396(9) 0.4073(4) 0.0287(19) Uani 1 1 d . . . H3A H 0.0404 0.1650 0.3898 0.034 Uiso 1 1 calc R . . H3B H 0.0942 0.2222 0.4687 0.034 Uiso 1 1 calc R . . C4 C 0.0547(5) 0.4133(10) 0.3941(4) 0.0309(19) Uani 1 1 d . . . H4A H 0.0062 0.4314 0.4260 0.037 Uiso 1 1 calc R . . H4B H 0.0427 0.4323 0.3331 0.037 Uiso 1 1 calc R . . C5 C 0.0890(5) 0.7464(9) 0.4015(4) 0.0264(18) Uani 1 1 d . . . H5A H 0.0356 0.7539 0.4243 0.032 Uiso 1 1 calc R . . H5B H 0.1211 0.8322 0.4289 0.032 Uiso 1 1 calc R . . C6 C 0.0842(5) 0.7782(10) 0.3069(4) 0.0251(17) Uani 1 1 d . . . H6A H 0.0505 0.6962 0.2786 0.030 Uiso 1 1 calc R . . H6B H 0.0608 0.8857 0.2960 0.030 Uiso 1 1 calc R . . C7 C 0.1627(5) 0.8488(9) 0.1918(4) 0.0236(16) Uani 1 1 d . . . H7A H 0.1314 0.9491 0.1931 0.028 Uiso 1 1 calc R . . H7B H 0.1391 0.7764 0.1483 0.028 Uiso 1 1 calc R . . C8 C 0.2448(5) 0.8874(9) 0.1695(5) 0.0296(19) Uani 1 1 d . . . H8A H 0.2688 0.9570 0.2141 0.036 Uiso 1 1 calc R . . H8B H 0.2448 0.9476 0.1152 0.036 Uiso 1 1 calc R . . C9 C 0.3968(5) 0.7625(10) 0.2052(5) 0.0313(18) Uani 1 1 d . . . H9A H 0.4308 0.6658 0.2081 0.038 Uiso 1 1 calc R . . H9B H 0.4214 0.8399 0.1661 0.038 Uiso 1 1 calc R . . C10 C 0.3962(5) 0.8386(9) 0.2936(4) 0.0287(18) Uani 1 1 d . . . H10A H 0.3756 0.9497 0.2879 0.034 Uiso 1 1 calc R . . H10B H 0.4510 0.8468 0.3152 0.034 Uiso 1 1 calc R . . C11 C 0.4091(5) 0.5880(9) 0.4139(5) 0.0269(17) Uani 1 1 d . . . H11A H 0.4297 0.5215 0.3673 0.032 Uiso 1 1 calc R . . H11B H 0.4536 0.6429 0.4432 0.032 Uiso 1 1 calc R . . C12 C 0.3658(5) 0.4838(9) 0.4755(4) 0.0283(19) Uani 1 1 d . . . H12A H 0.4030 0.4102 0.5051 0.034 Uiso 1 1 calc R . . H12B H 0.3409 0.5524 0.5186 0.034 Uiso 1 1 calc R . . Cl1 Cl 0.53336(15) 0.8793(3) 0.55816(13) 0.0415(6) Uani 1 1 d D . . C13 C 0.5486(8) 1.0137(17) 0.4743(8) 0.029(4) Uani 0.50 1 d PD . . H13A H 0.5901 1.0910 0.4920 0.034 Uiso 0.50 1 calc PR . . H13B H 0.5680 0.9522 0.4253 0.034 Uiso 0.50 1 calc PR . . 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 0.0204(8) 0.0234(7) 0.0175(6) 0.0010(5) 0.0043(6) -0.0017(7) I1 0.0262(3) 0.0210(2) 0.0215(2) -0.00043(18) 0.00643(19) 0.0007(2) I2 0.0246(3) 0.0429(3) 0.0199(2) -0.0075(2) 0.00367(19) -0.0050(3) S1 0.0360(12) 0.0237(9) 0.0190(8) -0.0019(7) 0.0072(8) -0.0057(9) S2 0.0262(11) 0.0271(9) 0.0215(8) 0.0007(7) 0.0044(8) 0.0009(9) S3 0.0281(11) 0.0275(10) 0.0228(8) 0.0022(7) 0.0094(8) 0.0004(10) S4 0.0264(11) 0.0222(9) 0.0268(9) -0.0013(7) 0.0020(8) 0.0009(9) O1 0.020(3) 0.028(3) 0.021(2) 0.002(2) 0.003(2) -0.003(2) O2 0.023(3) 0.030(3) 0.025(2) 0.004(2) 0.006(2) 0.005(3) C1 0.027(4) 0.031(4) 0.021(3) 0.005(3) 0.007(3) 0.000(4) C2 0.035(5) 0.030(4) 0.020(3) 0.003(3) 0.010(3) 0.009(4) C3 0.031(5) 0.032(4) 0.023(3) 0.002(3) -0.001(3) -0.014(4) C4 0.027(5) 0.048(5) 0.018(3) -0.005(3) 0.006(3) -0.001(4) C5 0.032(5) 0.029(4) 0.019(3) -0.001(3) 0.009(3) 0.009(4) C6 0.017(4) 0.033(4) 0.026(3) 0.006(3) 0.007(3) 0.015(4) C7 0.020(4) 0.021(4) 0.030(4) 0.008(3) 0.003(3) 0.004(4) C8 0.036(5) 0.023(4) 0.030(4) 0.007(3) 0.009(4) -0.002(4) C9 0.022(4) 0.028(4) 0.044(4) 0.005(3) 0.016(4) -0.008(4) C10 0.035(5) 0.019(4) 0.032(4) 0.003(3) 0.001(4) -0.003(4) C11 0.018(4) 0.029(4) 0.033(4) -0.002(3) -0.002(3) -0.001(4) C12 0.033(5) 0.024(4) 0.027(4) -0.005(3) -0.004(4) 0.007(4) Cl1 0.0464(15) 0.0418(12) 0.0366(10) -0.0021(9) 0.0063(10) -0.0003(12) C13 0.009(7) 0.038(9) 0.040(8) -0.009(7) 0.003(6) -0.001(7) _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 O1 2.621(5) . ? Ca1 O2 2.653(5) . ? Ca1 S4 2.905(2) . ? Ca1 S3 2.923(2) . ? Ca1 S1 2.951(2) . ? Ca1 S2 2.966(3) . ? Ca1 I2 3.1155(15) . ? Ca1 I1 3.1178(17) . ? S1 C2 1.814(7) . ? S1 C3 1.829(9) . ? S2 C5 1.814(7) . ? S2 C4 1.818(8) . ? S3 C9 1.807(8) . ? S3 C8 1.828(8) . ? S4 C10 1.805(8) . ? S4 C11 1.807(8) . ? O1 C12 1.422(8) . ? O1 C1 1.450(9) . ? O2 C7 1.438(8) . ? O2 C6 1.440(9) . ? C1 C2 1.505(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.533(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.513(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.488(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.528(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.507(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? Cl1 C13 1.752(12) . ? C13 Cl1 1.724(12) 3_676 ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? 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 O1 Ca1 O2 125.13(15) . . ? O1 Ca1 S4 66.55(12) . . ? O2 Ca1 S4 75.09(12) . . ? O1 Ca1 S3 128.56(13) . . ? O2 Ca1 S3 67.31(13) . . ? S4 Ca1 S3 71.48(6) . . ? O1 Ca1 S1 68.15(12) . . ? O2 Ca1 S1 125.00(14) . . ? S4 Ca1 S1 133.19(7) . . ? S3 Ca1 S1 152.29(7) . . ? O1 Ca1 S2 72.15(13) . . ? O2 Ca1 S2 67.53(12) . . ? S4 Ca1 S2 86.29(7) . . ? S3 Ca1 S2 133.34(8) . . ? S1 Ca1 S2 69.15(6) . . ? O1 Ca1 I2 144.59(12) . . ? O2 Ca1 I2 78.39(11) . . ? S4 Ca1 I2 148.54(6) . . ? S3 Ca1 I2 82.90(5) . . ? S1 Ca1 I2 76.62(5) . . ? S2 Ca1 I2 99.01(6) . . ? O1 Ca1 I1 79.12(12) . . ? O2 Ca1 I1 144.80(12) . . ? S4 Ca1 I1 96.71(6) . . ? S3 Ca1 I1 77.60(6) . . ? S1 Ca1 I1 85.82(6) . . ? S2 Ca1 I1 147.18(6) . . ? I2 Ca1 I1 95.24(4) . . ? C2 S1 C3 102.8(3) . . ? C2 S1 Ca1 100.1(3) . . ? C3 S1 Ca1 107.4(2) . . ? C5 S2 C4 102.2(4) . . ? C5 S2 Ca1 101.3(3) . . ? C4 S2 Ca1 96.5(3) . . ? C9 S3 C8 102.6(4) . . ? C9 S3 Ca1 102.7(3) . . ? C8 S3 Ca1 102.4(3) . . ? C10 S4 C11 102.5(4) . . ? C10 S4 Ca1 110.0(2) . . ? C11 S4 Ca1 94.4(2) . . ? C12 O1 C1 112.2(5) . . ? C12 O1 Ca1 122.2(4) . . ? C1 O1 Ca1 121.7(4) . . ? C7 O2 C6 110.0(5) . . ? C7 O2 Ca1 117.1(4) . . ? C6 O2 Ca1 117.2(4) . . ? O1 C1 C2 109.3(5) . . ? O1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? O1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? C1 C2 S1 114.9(5) . . ? C1 C2 H2A 108.5 . . ? S1 C2 H2A 108.5 . . ? C1 C2 H2B 108.5 . . ? S1 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? C4 C3 S1 113.8(5) . . ? C4 C3 H3A 108.8 . . ? S1 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? S1 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 C4 S2 109.5(5) . . ? C3 C4 H4A 109.8 . . ? S2 C4 H4A 109.8 . . ? C3 C4 H4B 109.8 . . ? S2 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? C6 C5 S2 114.8(5) . . ? C6 C5 H5A 108.6 . . ? S2 C5 H5A 108.6 . . ? C6 C5 H5B 108.6 . . ? S2 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? O2 C6 C5 108.9(6) . . ? O2 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? O2 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? O2 C7 C8 109.8(6) . . ? O2 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? O2 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C7 C8 S3 111.1(5) . . ? C7 C8 H8A 109.4 . . ? S3 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? S3 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 S3 116.7(6) . . ? C10 C9 H9A 108.1 . . ? S3 C9 H9A 108.1 . . ? C10 C9 H9B 108.1 . . ? S3 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? C9 C10 S4 116.3(5) . . ? C9 C10 H10A 108.2 . . ? S4 C10 H10A 108.2 . . ? C9 C10 H10B 108.2 . . ? S4 C10 H10B 108.2 . . ? H10A C10 H10B 107.4 . . ? C12 C11 S4 107.1(6) . . ? C12 C11 H11A 110.3 . . ? S4 C11 H11A 110.3 . . ? C12 C11 H11B 110.3 . . ? S4 C11 H11B 110.3 . . ? H11A C11 H11B 108.6 . . ? O1 C12 C11 109.7(5) . . ? O1 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? O1 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? Cl1 C13 Cl1 114.6(8) 3_676 . ? Cl1 C13 H13A 108.6 3_676 . ? Cl1 C13 H13A 108.6 . . ? Cl1 C13 H13B 108.6 3_676 . ? Cl1 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 O1 C1 C2 -152.8(6) . . . . ? Ca1 O1 C1 C2 49.0(8) . . . . ? O1 C1 C2 S1 -59.1(8) . . . . ? C3 S1 C2 C1 -71.3(6) . . . . ? Ca1 S1 C2 C1 39.3(6) . . . . ? C2 S1 C3 C4 119.5(5) . . . . ? Ca1 S1 C3 C4 14.5(5) . . . . ? S1 C3 C4 S2 -61.4(6) . . . . ? C5 S2 C4 C3 175.2(5) . . . . ? Ca1 S2 C4 C3 72.2(5) . . . . ? C4 S2 C5 C6 -69.3(7) . . . . ? Ca1 S2 C5 C6 30.0(6) . . . . ? C7 O2 C6 C5 -162.3(6) . . . . ? Ca1 O2 C6 C5 60.8(7) . . . . ? S2 C5 C6 O2 -59.8(8) . . . . ? C6 O2 C7 C8 162.7(6) . . . . ? Ca1 O2 C7 C8 -60.3(7) . . . . ? O2 C7 C8 S3 63.3(7) . . . . ? C9 S3 C8 C7 -141.7(5) . . . . ? Ca1 S3 C8 C7 -35.4(5) . . . . ? C8 S3 C9 C10 51.8(6) . . . . ? Ca1 S3 C9 C10 -54.3(6) . . . . ? S3 C9 C10 S4 48.1(8) . . . . ? C11 S4 C10 C9 85.9(6) . . . . ? Ca1 S4 C10 C9 -13.5(7) . . . . ? C10 S4 C11 C12 -175.3(5) . . . . ? Ca1 S4 C11 C12 -63.6(5) . . . . ? C1 O1 C12 C11 173.0(6) . . . . ? Ca1 O1 C12 C11 -29.0(8) . . . . ? S4 C11 C12 O1 66.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.168 _refine_diff_density_min -1.612 _refine_diff_density_rms 0.219 data_11paf033a _database_code_depnum_ccdc_archive 'CCDC 891793' #TrackingRef '- CaSr_all11_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-11-25 _audit_author_name 'Webster, M.' _chemical_name_systematic ; diiodo(1,4,7-trioxa-10,13-dithiacyclopentadecane)calcium(II) ; # C10H20O3S2 = [15]aneO3S2 # 1,4,7-trioxa-10,13-dithiacyclopentadecane (iLab defaults) # 1,4,7-trioxa-10,13-dithiacyclopentadecane (iLab selected options) # 1,4,7-trioxa-10,13-dithiacyclopentadecane (Chemspider) _chemical_name_common diiodo(1,4,7-trioxa-10,13-dithiacyclopentadecane)calcium(ii) _chemical_melting_point ? _chemical_formula_moiety 'C10 H20 Ca I2 O3 S2' _chemical_formula_sum 'C10 H20 Ca I2 O3 S2' _chemical_formula_weight 546.26 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' 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 10.027(4) _cell_length_b 13.924(5) _cell_length_c 12.848(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.82(4) _cell_angle_gamma 90.00 _cell_volume 1755.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7438 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 4.110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.568 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'AFC12 (Right): Kappa 3-circle' _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8699 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4003 _reflns_number_gt 3329 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+6.0370P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4003 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _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 Ca1 Ca 0.18431(11) 0.20358(8) 0.96650(9) 0.0182(2) Uani 1 1 d . . . I1 I 0.23678(4) 0.08598(3) 0.77577(3) 0.02258(12) Uani 1 1 d . . . I2 I -0.12155(4) 0.23913(3) 0.84691(3) 0.02180(12) Uani 1 1 d . . . S1 S 0.41478(15) 0.33358(11) 0.94789(12) 0.0231(3) Uani 1 1 d . . . S2 S 0.12354(15) 0.40957(10) 0.99725(12) 0.0233(3) Uani 1 1 d . . . O1 O 0.0756(4) 0.2246(3) 1.1176(3) 0.0212(8) Uani 1 1 d . . . O2 O 0.1629(4) 0.0553(3) 1.0569(3) 0.0212(8) Uani 1 1 d . . . O3 O 0.4112(4) 0.1408(3) 1.0598(3) 0.0206(8) Uani 1 1 d . . . C1 C 0.0045(6) 0.1383(5) 1.1383(5) 0.0269(13) Uani 1 1 d . . . H1A H -0.0717 0.1244 1.0780 0.032 Uiso 1 1 calc R . . H1B H -0.0328 0.1461 1.2034 0.032 Uiso 1 1 calc R . . C2 C 0.1068(7) 0.0585(5) 1.1523(5) 0.0276(13) Uani 1 1 d . . . H2A H 0.1800 0.0706 1.2154 0.033 Uiso 1 1 calc R . . H2B H 0.0625 -0.0034 1.1624 0.033 Uiso 1 1 calc R . . C3 C 0.2848(6) -0.0002(4) 1.0712(5) 0.0239(12) Uani 1 1 d . . . H3A H 0.2983 -0.0229 1.0011 0.029 Uiso 1 1 calc R . . H3B H 0.2754 -0.0573 1.1150 0.029 Uiso 1 1 calc R . . C4 C 0.4078(6) 0.0569(4) 1.1245(5) 0.0234(12) Uani 1 1 d . . . H4A H 0.3998 0.0756 1.1973 0.028 Uiso 1 1 calc R . . H4B H 0.4919 0.0186 1.1290 0.028 Uiso 1 1 calc R . . C5 C 0.5358(6) 0.1944(4) 1.0941(5) 0.0228(12) Uani 1 1 d . . . H5A H 0.6134 0.1496 1.1145 0.027 Uiso 1 1 calc R . . H5B H 0.5293 0.2339 1.1569 0.027 Uiso 1 1 calc R . . C6 C 0.5589(7) 0.2583(4) 1.0048(5) 0.0262(13) Uani 1 1 d . . . H6A H 0.5818 0.2175 0.9478 0.031 Uiso 1 1 calc R . . H6B H 0.6384 0.3000 1.0316 0.031 Uiso 1 1 calc R . . C7 C 0.4067(6) 0.4132(4) 1.0591(5) 0.0242(12) Uani 1 1 d . . . H7A H 0.3990 0.3753 1.1228 0.029 Uiso 1 1 calc R . . H7B H 0.4901 0.4531 1.0765 0.029 Uiso 1 1 calc R . . C8 C 0.2815(6) 0.4769(4) 1.0255(5) 0.0248(12) Uani 1 1 d . . . H8A H 0.2905 0.5136 0.9612 0.030 Uiso 1 1 calc R . . H8B H 0.2778 0.5237 1.0828 0.030 Uiso 1 1 calc R . . C9 C 0.0939(7) 0.3947(4) 1.1324(5) 0.0257(13) Uani 1 1 d . . . H9A H 0.1824 0.3867 1.1825 0.031 Uiso 1 1 calc R . . H9B H 0.0498 0.4532 1.1532 0.031 Uiso 1 1 calc R . . C10 C 0.0053(6) 0.3092(5) 1.1402(5) 0.0283(13) Uani 1 1 d . . . H10A H -0.0143 0.3051 1.2125 0.034 Uiso 1 1 calc R . . H10B H -0.0823 0.3154 1.0885 0.034 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 0.0114(5) 0.0248(6) 0.0186(5) 0.0002(4) 0.0039(4) 0.0005(4) I1 0.01506(19) 0.0338(2) 0.0194(2) -0.00224(14) 0.00467(14) 0.00225(14) I2 0.01230(18) 0.0310(2) 0.0214(2) 0.00141(14) 0.00191(14) -0.00041(13) S1 0.0185(7) 0.0280(7) 0.0236(7) 0.0022(6) 0.0060(5) -0.0024(5) S2 0.0207(7) 0.0275(7) 0.0211(7) -0.0003(5) 0.0025(5) 0.0053(5) O1 0.0142(19) 0.031(2) 0.019(2) -0.0032(17) 0.0050(15) 0.0015(16) O2 0.0167(19) 0.027(2) 0.022(2) 0.0004(16) 0.0084(16) -0.0007(16) O3 0.0150(18) 0.024(2) 0.022(2) 0.0042(16) 0.0017(15) -0.0025(16) C1 0.016(3) 0.039(3) 0.028(3) 0.001(3) 0.009(2) -0.002(2) C2 0.027(3) 0.033(3) 0.025(3) 0.004(3) 0.010(2) -0.001(3) C3 0.019(3) 0.026(3) 0.027(3) 0.005(2) 0.007(2) -0.004(2) C4 0.017(3) 0.026(3) 0.026(3) 0.006(2) 0.001(2) 0.002(2) C5 0.011(2) 0.030(3) 0.025(3) -0.001(2) -0.002(2) 0.001(2) C6 0.021(3) 0.031(3) 0.029(3) -0.006(2) 0.009(2) -0.002(2) C7 0.021(3) 0.025(3) 0.025(3) 0.001(2) 0.001(2) -0.004(2) C8 0.028(3) 0.022(3) 0.024(3) 0.003(2) 0.001(2) -0.004(2) C9 0.028(3) 0.031(3) 0.018(3) -0.001(2) 0.004(2) 0.008(3) C10 0.021(3) 0.036(3) 0.029(3) 0.001(3) 0.008(2) 0.011(3) _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 C3 3.212(6) . ? Ca1 O2 2.400(4) . ? Ca1 O1 2.432(4) . ? Ca1 O3 2.502(4) . ? Ca1 S2 2.975(2) . ? Ca1 S1 2.9834(19) . ? Ca1 I1 3.0808(14) . ? Ca1 I2 3.1751(17) . ? S1 C6 1.813(7) . ? S1 C7 1.824(6) . ? S2 C8 1.812(6) . ? S2 C9 1.832(6) . ? O1 C10 1.432(7) . ? O1 C1 1.450(7) . ? O2 C3 1.426(7) . ? O2 C2 1.450(7) . ? O3 C4 1.438(7) . ? O3 C5 1.444(7) . ? C1 C2 1.498(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.509(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.506(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.526(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.501(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? 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 O1 67.54(14) . . ? O2 Ca1 O3 68.32(13) . . ? O1 Ca1 O3 99.91(14) . . ? O2 Ca1 S2 136.38(11) . . ? O1 Ca1 S2 68.91(11) . . ? O3 Ca1 S2 117.64(10) . . ? O2 Ca1 S1 135.10(11) . . ? O1 Ca1 S1 118.18(11) . . ? O3 Ca1 S1 66.86(10) . . ? S2 Ca1 S1 66.98(5) . . ? O2 Ca1 I1 88.54(10) . . ? O1 Ca1 I1 151.27(11) . . ? O3 Ca1 I1 84.76(10) . . ? S2 Ca1 I1 133.71(5) . . ? S1 Ca1 I1 89.85(5) . . ? O2 Ca1 I2 101.23(10) . . ? O1 Ca1 I2 79.69(10) . . ? O3 Ca1 I2 168.45(10) . . ? S2 Ca1 I2 73.15(4) . . ? S1 Ca1 I2 123.64(5) . . ? I1 Ca1 I2 90.19(4) . . ? C6 S1 C7 101.3(3) . . ? C6 S1 Ca1 100.6(2) . . ? C7 S1 Ca1 98.4(2) . . ? C8 S2 C9 100.0(3) . . ? C8 S2 Ca1 109.3(2) . . ? C9 S2 Ca1 95.4(2) . . ? C10 O1 C1 111.3(5) . . ? C10 O1 Ca1 125.5(4) . . ? C1 O1 Ca1 111.3(3) . . ? C3 O2 C2 112.2(4) . . ? C3 O2 Ca1 111.7(3) . . ? C2 O2 Ca1 118.1(3) . . ? C4 O3 C5 111.4(4) . . ? C4 O3 Ca1 115.7(3) . . ? C5 O3 Ca1 127.6(3) . . ? O1 C1 C2 106.7(5) . . ? O1 C1 H1A 110.4 . . ? C2 C1 H1A 110.4 . . ? O1 C1 H1B 110.4 . . ? C2 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? O2 C2 C1 107.2(5) . . ? O2 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O2 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? O2 C3 C4 111.9(5) . . ? O2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? O2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O3 C4 C3 106.3(4) . . ? O3 C4 H4A 110.5 . . ? C3 C4 H4A 110.5 . . ? O3 C4 H4B 110.5 . . ? C3 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? O3 C5 C6 109.4(5) . . ? O3 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? O3 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? C5 C6 S1 114.5(4) . . ? C5 C6 H6A 108.6 . . ? S1 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 . . ? S1 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C8 C7 S1 107.3(4) . . ? C8 C7 H7A 110.3 . . ? S1 C7 H7A 110.3 . . ? C8 C7 H7B 110.3 . . ? S1 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? C7 C8 S2 113.0(4) . . ? C7 C8 H8A 109.0 . . ? S2 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? S2 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C10 C9 S2 111.4(4) . . ? C10 C9 H9A 109.3 . . ? S2 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? S2 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? O1 C10 C9 108.4(5) . . ? O1 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? O1 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 O1 C1 C2 -159.3(5) . . . . ? Ca1 O1 C1 C2 55.4(5) . . . . ? C3 O2 C2 C1 164.8(5) . . . . ? Ca1 O2 C2 C1 32.7(6) . . . . ? O1 C1 C2 O2 -56.5(6) . . . . ? C2 O2 C3 C4 -82.1(6) . . . . ? Ca1 O2 C3 C4 53.2(5) . . . . ? C2 O2 C3 Ca1 -135.3(5) . . . . ? C5 O3 C4 C3 -171.6(5) . . . . ? Ca1 O3 C4 C3 32.1(6) . . . . ? O2 C3 C4 O3 -56.1(6) . . . . ? C4 O3 C5 C6 159.8(5) . . . . ? Ca1 O3 C5 C6 -47.3(6) . . . . ? O3 C5 C6 S1 51.9(6) . . . . ? C7 S1 C6 C5 66.4(5) . . . . ? Ca1 S1 C6 C5 -34.5(5) . . . . ? C6 S1 C7 C8 -175.8(4) . . . . ? Ca1 S1 C7 C8 -73.1(4) . . . . ? S1 C7 C8 S2 62.2(5) . . . . ? C9 S2 C8 C7 82.5(5) . . . . ? Ca1 S2 C8 C7 -16.9(5) . . . . ? C8 S2 C9 C10 -156.2(4) . . . . ? Ca1 S2 C9 C10 -45.5(4) . . . . ? C1 O1 C10 C9 171.9(5) . . . . ? Ca1 O1 C10 C9 -48.8(6) . . . . ? S2 C9 C10 O1 63.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.424 _refine_diff_density_min -3.032 _refine_diff_density_rms 0.212 data_12paf080ra _database_code_depnum_ccdc_archive 'CCDC 891794' #TrackingRef '- CaSr_all11_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-03-27 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Diaqua-1,4,10,13-tetraoxa-7,16-dithiacyclooctadecane-calcium diiodide ; # C12H24O4S2 = [18]aneO4S2 # 1,4,10,13-tetraoxo-7,16-dithia-cyclooctadecane # 1,4,10,13-tetraoxa-7,16-dithiacyclooctadecane (iLab defaults) # 1,4,10,13-tetraoxa-7,16-dithiacyclooctadecane (iLab selected options) _chemical_name_common ;Diaqua-1,4,10,13-tetraoxa-7,16-dithiacyclooctadecane-calcium diiodide ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H28 Ca O6 S2 2+, 2(I 1-)' _chemical_formula_sum 'C12 H28 Ca I2 O6 S2' _chemical_formula_structural '((C12 H24 O4 S2) 2(H2 O) Ca) 2(I)' _chemical_formula_weight 626.34 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.313(3) _cell_length_b 11.947(4) _cell_length_c 19.736(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2195.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8068 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 3.309 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.722 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10240 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.1730 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4991 _reflns_number_gt 3126 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0137P)^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 (C-H) difmap (O-H)' _refine_ls_hydrogen_treatment 'constr (C-H) refxyz (O-H)' # 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 0.47(3) _chemical_absolute_configuration ad _refine_ls_number_reflns 4991 _refine_ls_number_parameters 217 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1102 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _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 0.3443(2) 0.01559(14) 0.15801(6) 0.0152(4) Uani 1 1 d . . . S1 S 0.5257(3) -0.1181(2) 0.06428(9) 0.0363(7) Uani 1 1 d . . . S2 S 0.2578(2) 0.0773(2) 0.30068(9) 0.0219(6) Uani 1 1 d . . . O1 O 0.2125(6) -0.0609(5) 0.0575(2) 0.0284(17) Uani 1 1 d . . . O2 O 0.0795(6) 0.0108(5) 0.1739(2) 0.0235(16) Uani 1 1 d . . . O3 O 0.3117(7) 0.2156(4) 0.1718(2) 0.0232(15) Uani 1 1 d . . . O4 O 0.4442(6) 0.1290(5) 0.0652(2) 0.0210(15) Uani 1 1 d . . . O5 O 0.3353(8) -0.1578(5) 0.2104(3) 0.0276(15) Uani 1 1 d D . . H1 H 0.294(9) -0.209(5) 0.189(3) 0.04(3) Uiso 1 1 d D . . H2 H 0.310(8) -0.169(6) 0.2508(15) 0.02(2) Uiso 1 1 d D . . O6 O 0.5755(6) 0.0493(5) 0.2038(2) 0.0207(15) Uani 1 1 d . . . C1 C 0.4035(13) -0.1470(9) -0.0057(4) 0.048(4) Uani 1 1 d . . . H1A H 0.4575 -0.1418 -0.0488 0.058 Uiso 1 1 calc R . . H1B H 0.3680 -0.2248 -0.0014 0.058 Uiso 1 1 calc R . . C2 C 0.2753(11) -0.0684(9) -0.0092(3) 0.038(3) Uani 1 1 d . . . H2A H 0.3065 0.0066 -0.0246 0.045 Uiso 1 1 calc R . . H2B H 0.2036 -0.0974 -0.0418 0.045 Uiso 1 1 calc R . . C3 C 0.0662(11) -0.0292(9) 0.0575(4) 0.037(3) Uani 1 1 d . . . H3A H 0.0137 -0.0714 0.0222 0.044 Uiso 1 1 calc R . . H3B H 0.0576 0.0517 0.0473 0.044 Uiso 1 1 calc R . . C4 C 0.0037(9) -0.0531(8) 0.1247(4) 0.037(3) Uani 1 1 d . . . H4A H -0.0993 -0.0327 0.1252 0.045 Uiso 1 1 calc R . . H4B H 0.0122 -0.1339 0.1351 0.045 Uiso 1 1 calc R . . C5 C 0.0152(10) -0.0070(8) 0.2386(4) 0.027(2) Uani 1 1 d . . . H5A H 0.0388 -0.0834 0.2546 0.032 Uiso 1 1 calc R . . H5B H -0.0904 -0.0016 0.2343 0.032 Uiso 1 1 calc R . . C6 C 0.0655(9) 0.0755(10) 0.2891(4) 0.036(3) Uani 1 1 d . . . H6A H 0.0194 0.0589 0.3332 0.043 Uiso 1 1 calc R . . H6B H 0.0338 0.1510 0.2748 0.043 Uiso 1 1 calc R . . C7 C 0.2933(10) 0.2248(7) 0.2924(3) 0.027(2) Uani 1 1 d . . . H7A H 0.2433 0.2645 0.3296 0.032 Uiso 1 1 calc R . . H7B H 0.3976 0.2372 0.2985 0.032 Uiso 1 1 calc R . . C8 C 0.2481(9) 0.2769(8) 0.2257(4) 0.032(3) Uani 1 1 d . . . H8A H 0.1422 0.2750 0.2214 0.038 Uiso 1 1 calc R . . H8B H 0.2796 0.3559 0.2239 0.038 Uiso 1 1 calc R . . C9 C 0.2788(8) 0.2629(8) 0.1067(3) 0.021(2) Uani 1 1 d . . . H9A H 0.2571 0.3437 0.1111 0.025 Uiso 1 1 calc R . . H9B H 0.1945 0.2250 0.0866 0.025 Uiso 1 1 calc R . . C10 C 0.4081(8) 0.2459(8) 0.0634(3) 0.020(2) Uani 1 1 d . . . H10A H 0.3876 0.2694 0.0163 0.024 Uiso 1 1 calc R . . H10B H 0.4893 0.2911 0.0807 0.024 Uiso 1 1 calc R . . C11 C 0.5530(9) 0.0997(9) 0.0161(3) 0.031(3) Uani 1 1 d . . . H11A H 0.6214 0.1627 0.0114 0.037 Uiso 1 1 calc R . . H11B H 0.5070 0.0876 -0.0286 0.037 Uiso 1 1 calc R . . C12 C 0.6316(10) -0.0013(10) 0.0354(4) 0.041(3) Uani 1 1 d . . . H12A H 0.7001 0.0189 0.0718 0.050 Uiso 1 1 calc R . . H12B H 0.6889 -0.0261 -0.0041 0.050 Uiso 1 1 calc R . . I1 I 0.81968(6) 0.25061(5) 0.13905(2) 0.02471(14) Uani 1 1 d . . . I2 I 0.33594(7) 0.59081(5) 0.12621(2) 0.02409(15) Uani 1 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 Ca1 0.0197(9) 0.0129(11) 0.0131(6) 0.0002(6) -0.0014(7) 0.0015(10) S1 0.0547(18) 0.038(2) 0.0161(10) 0.0039(11) 0.0078(11) 0.0180(17) S2 0.0175(11) 0.0317(17) 0.0164(9) -0.0027(11) 0.0006(8) 0.0026(14) O1 0.034(4) 0.028(5) 0.023(3) -0.004(3) -0.008(2) 0.001(4) O2 0.019(3) 0.033(5) 0.019(3) -0.003(3) -0.007(2) -0.005(3) O3 0.033(4) 0.014(4) 0.023(2) 0.003(2) 0.008(3) 0.009(4) O4 0.022(3) 0.021(4) 0.020(3) -0.002(3) 0.005(2) 0.002(3) O5 0.042(4) 0.022(4) 0.018(3) 0.003(3) 0.009(3) -0.003(4) O6 0.017(3) 0.030(4) 0.015(2) -0.003(3) -0.001(2) 0.003(3) C1 0.094(11) 0.030(8) 0.020(5) -0.014(5) 0.016(5) -0.011(8) C2 0.051(7) 0.048(8) 0.014(4) 0.003(4) -0.011(4) -0.007(7) C3 0.045(7) 0.032(8) 0.034(5) -0.002(5) -0.023(5) -0.001(7) C4 0.013(4) 0.051(8) 0.047(5) -0.009(6) -0.001(4) 0.006(5) C5 0.018(5) 0.028(7) 0.035(5) 0.013(5) 0.003(4) -0.004(5) C6 0.019(5) 0.045(8) 0.045(5) 0.009(6) 0.008(4) 0.007(6) C7 0.033(6) 0.015(6) 0.033(4) -0.012(4) -0.006(4) 0.005(5) C8 0.032(5) 0.024(7) 0.040(5) -0.002(5) 0.005(4) 0.009(6) C9 0.027(5) 0.010(5) 0.025(4) 0.007(4) 0.001(3) -0.004(5) C10 0.028(5) 0.018(6) 0.015(3) -0.001(4) -0.005(3) -0.008(6) C11 0.026(5) 0.052(8) 0.016(4) -0.003(5) 0.002(3) -0.010(6) C12 0.025(6) 0.082(10) 0.017(4) 0.001(5) 0.007(4) 0.000(7) I1 0.0230(3) 0.0316(4) 0.0196(2) -0.0037(3) 0.0037(2) -0.0032(4) I2 0.0315(3) 0.0231(3) 0.0176(2) -0.0019(2) -0.0037(3) -0.0055(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 Ca1 O5 2.318(6) . ? Ca1 O6 2.370(5) . ? Ca1 O3 2.424(6) . ? Ca1 O4 2.461(5) . ? Ca1 O2 2.487(6) . ? Ca1 O1 2.505(5) . ? Ca1 S1 2.971(3) . ? Ca1 S2 3.020(2) . ? S1 C12 1.802(10) . ? S1 C1 1.823(9) . ? S2 C7 1.800(9) . ? S2 C6 1.805(9) . ? O1 C3 1.414(10) . ? O1 C2 1.443(9) . ? O2 C4 1.422(9) . ? O2 C5 1.426(8) . ? O3 C8 1.421(9) . ? O3 C9 1.436(7) . ? O4 C10 1.437(10) . ? O4 C11 1.446(9) . ? O5 H1 0.83(2) . ? O5 H2 0.843(19) . ? C1 C2 1.521(13) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.476(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.478(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.517(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.491(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.462(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? # I1 I1 0.0000(19) 1 ? # What on earth is this doing here? 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 O5 Ca1 O6 90.8(2) . . ? O5 Ca1 O3 145.76(18) . . ? O6 Ca1 O3 84.5(2) . . ? O5 Ca1 O4 147.0(2) . . ? O6 Ca1 O4 81.20(18) . . ? O3 Ca1 O4 65.68(18) . . ? O5 Ca1 O2 83.5(2) . . ? O6 Ca1 O2 148.96(17) . . ? O3 Ca1 O2 83.4(2) . . ? O4 Ca1 O2 118.79(19) . . ? O5 Ca1 O1 90.5(2) . . ? O6 Ca1 O1 144.02(19) . . ? O3 Ca1 O1 112.8(2) . . ? O4 Ca1 O1 78.28(19) . . ? O2 Ca1 O1 66.78(18) . . ? O5 Ca1 S1 79.51(16) . . ? O6 Ca1 S1 79.17(14) . . ? O3 Ca1 S1 132.15(15) . . ? O4 Ca1 S1 67.52(15) . . ? O2 Ca1 S1 129.07(16) . . ? O1 Ca1 S1 65.77(15) . . ? O5 Ca1 S2 78.02(15) . . ? O6 Ca1 S2 81.12(12) . . ? O3 Ca1 S2 67.75(12) . . ? O4 Ca1 S2 131.33(16) . . ? O2 Ca1 S2 67.85(12) . . ? O1 Ca1 S2 134.13(16) . . ? S1 Ca1 S2 149.71(8) . . ? C12 S1 C1 104.4(4) . . ? C12 S1 Ca1 95.3(3) . . ? C1 S1 Ca1 102.6(4) . . ? C7 S2 C6 100.5(5) . . ? C7 S2 Ca1 96.1(2) . . ? C6 S2 Ca1 98.3(3) . . ? C3 O1 C2 114.0(6) . . ? C3 O1 Ca1 112.0(5) . . ? C2 O1 Ca1 123.1(5) . . ? C4 O2 C5 108.9(7) . . ? C4 O2 Ca1 114.7(4) . . ? C5 O2 Ca1 122.2(5) . . ? C8 O3 C9 112.2(6) . . ? C8 O3 Ca1 130.1(5) . . ? C9 O3 Ca1 108.3(4) . . ? C10 O4 C11 112.5(7) . . ? C10 O4 Ca1 117.7(4) . . ? C11 O4 Ca1 129.1(6) . . ? Ca1 O5 H1 117(6) . . ? Ca1 O5 H2 125(5) . . ? H1 O5 H2 103(7) . . ? C2 C1 S1 114.0(6) . . ? C2 C1 H1A 108.7 . . ? S1 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? S1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? O1 C2 C1 108.4(6) . . ? O1 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? O1 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? O1 C3 C4 109.2(7) . . ? O1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? O1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? O2 C4 C3 108.3(8) . . ? O2 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? O2 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? O2 C5 C6 111.8(7) . . ? O2 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? O2 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? C5 C6 S2 114.0(7) . . ? C5 C6 H6A 108.7 . . ? S2 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? S2 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C8 C7 S2 115.4(6) . . ? C8 C7 H7A 108.4 . . ? S2 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? S2 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? O3 C8 C7 108.8(7) . . ? O3 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? O3 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? O3 C9 C10 106.7(6) . . ? O3 C9 H9A 110.4 . . ? C10 C9 H9A 110.4 . . ? O3 C9 H9B 110.4 . . ? C10 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? O4 C10 C9 107.9(7) . . ? O4 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? O4 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? O4 C11 C12 112.1(7) . . ? O4 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? O4 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 C12 S1 116.6(7) . . ? C11 C12 H12A 108.1 . . ? S1 C12 H12A 108.1 . . ? C11 C12 H12B 108.1 . . ? S1 C12 H12B 108.1 . . ? H12A C12 H12B 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 S1 C1 C2 -79.3(8) . . . . ? Ca1 S1 C1 C2 19.6(7) . . . . ? C3 O1 C2 C1 -156.3(8) . . . . ? Ca1 O1 C2 C1 62.5(9) . . . . ? S1 C1 C2 O1 -48.1(9) . . . . ? C2 O1 C3 C4 165.1(8) . . . . ? Ca1 O1 C3 C4 -49.4(10) . . . . ? C5 O2 C4 C3 177.0(8) . . . . ? Ca1 O2 C4 C3 -42.0(9) . . . . ? O1 C3 C4 O2 60.8(11) . . . . ? C4 O2 C5 C6 -166.8(8) . . . . ? Ca1 O2 C5 C6 55.8(9) . . . . ? O2 C5 C6 S2 -57.5(10) . . . . ? C7 S2 C6 C5 129.9(7) . . . . ? Ca1 S2 C6 C5 32.1(7) . . . . ? C6 S2 C7 C8 -58.9(7) . . . . ? Ca1 S2 C7 C8 40.7(6) . . . . ? C9 O3 C8 C7 -177.5(7) . . . . ? Ca1 O3 C8 C7 40.6(10) . . . . ? S2 C7 C8 O3 -54.3(9) . . . . ? C8 O3 C9 C10 145.2(7) . . . . ? Ca1 O3 C9 C10 -64.6(7) . . . . ? C11 O4 C10 C9 170.2(6) . . . . ? Ca1 O4 C10 C9 -18.3(7) . . . . ? O3 C9 C10 O4 53.5(8) . . . . ? C10 O4 C11 C12 155.9(7) . . . . ? Ca1 O4 C11 C12 -14.4(10) . . . . ? O4 C11 C12 S1 45.9(9) . . . . ? C1 S1 C12 C11 57.4(7) . . . . ? Ca1 S1 C12 C11 -47.1(6) . . . . ? 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 O5 H1 I2 0.83(2) 2.72(6) 3.432(6) 144(8) 1_545 O5 H2 I1 0.843(19) 2.66(3) 3.479(5) 163(7) 4_645 loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O6 I1 3.548(6) . . ? O6 I2 3.490(4) . 4_645 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.880 _refine_diff_density_min -0.812 _refine_diff_density_rms 0.183 data_12paf072ka _database_code_depnum_ccdc_archive 'CCDC 891795' #TrackingRef '- CaSr_all11_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-05-10 _audit_author_name 'Webster, M.' _chemical_name_systematic ; 1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane ; # C12H24O4Se2 = [18]aneO4Se2 # 1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane (iLab defaults) # 1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane (iLab selected options) _chemical_name_common 1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 O4 Se2' _chemical_formula_sum 'C12 H24 O4 Se2' _chemical_formula_weight 390.23 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' 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 6.933(4) _cell_length_b 13.419(7) _cell_length_c 8.573(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.489(7) _cell_angle_gamma 90.00 _cell_volume 778.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5186 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392 _exptl_absorpt_coefficient_mu 4.752 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.637 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ; Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, HF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ SuperBright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7115 _diffrn_reflns_av_R_equivalents 0.1176 _diffrn_reflns_av_sigmaI/netI 0.1786 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1775 _reflns_number_gt 1020 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1775 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 0.652 _refine_ls_restrained_S_all 0.652 _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 Se1 Se 0.89182(6) 0.65394(2) 0.41737(5) 0.01958(12) Uani 1 1 d . . . O1 O 0.4290(3) 0.46156(15) 0.2393(3) 0.0143(6) Uani 1 1 d . . . O2 O 0.1907(3) 0.35587(16) -0.0208(3) 0.0143(6) Uani 1 1 d . . . C1 C 0.7411(5) 0.5372(2) 0.3255(4) 0.0132(8) Uani 1 1 d . . . H1A H 0.7761 0.5207 0.2225 0.016 Uiso 1 1 calc R . . H1B H 0.7784 0.4797 0.3982 0.016 Uiso 1 1 calc R . . C2 C 0.5210(5) 0.5532(2) 0.2979(4) 0.0161(9) Uani 1 1 d . . . H2A H 0.4836 0.5721 0.3990 0.019 Uiso 1 1 calc R . . H2B H 0.4793 0.6071 0.2189 0.019 Uiso 1 1 calc R . . C3 C 0.2218(5) 0.4701(2) 0.1951(4) 0.0150(8) Uani 1 1 d . . . H3A H 0.1852 0.5239 0.1150 0.018 Uiso 1 1 calc R . . H3B H 0.1683 0.4873 0.2898 0.018 Uiso 1 1 calc R . . C4 C 0.1365(5) 0.3730(2) 0.1262(4) 0.0152(9) Uani 1 1 d . . . H4A H 0.1862 0.3182 0.2014 0.018 Uiso 1 1 calc R . . H4B H -0.0092 0.3749 0.1098 0.018 Uiso 1 1 calc R . . C5 C 0.1007(5) 0.2688(2) -0.1000(4) 0.0189(9) Uani 1 1 d . . . H5A H -0.0443 0.2781 -0.1304 0.023 Uiso 1 1 calc R . . H5B H 0.1284 0.2109 -0.0270 0.023 Uiso 1 1 calc R . . C6 C 0.1801(5) 0.2496(2) -0.2462(4) 0.0173(9) Uani 1 1 d . . . H6A H 0.1338 0.1831 -0.2885 0.021 Uiso 1 1 calc R . . H6B H 0.3260 0.2468 -0.2142 0.021 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 Se1 0.0223(2) 0.01791(16) 0.0164(2) -0.0008(2) -0.00041(15) -0.0020(2) O1 0.0103(14) 0.0125(11) 0.0208(15) -0.0003(11) 0.0048(11) -0.0011(10) O2 0.0167(14) 0.0166(12) 0.0106(14) -0.0044(11) 0.0050(10) -0.0073(11) C1 0.017(2) 0.0088(15) 0.014(2) 0.0018(15) 0.0029(16) -0.0006(15) C2 0.019(2) 0.0141(16) 0.016(2) 0.0018(15) 0.0065(17) 0.0018(16) C3 0.014(2) 0.0196(17) 0.012(2) 0.0005(16) 0.0036(16) 0.0027(16) C4 0.012(2) 0.0235(19) 0.010(2) 0.0025(15) 0.0015(17) 0.0010(15) C5 0.022(2) 0.0143(17) 0.018(2) 0.0013(16) -0.0009(18) -0.0044(16) C6 0.020(2) 0.0116(16) 0.020(2) -0.0015(17) 0.0040(17) -0.0046(16) _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 Se1 C6 1.940(3) 3_665 ? Se1 C1 1.952(3) . ? O1 C3 1.409(4) . ? O1 C2 1.425(4) . ? O2 C4 1.410(4) . ? O2 C5 1.425(4) . ? C1 C2 1.508(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.499(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.497(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 Se1 1.940(3) 3_665 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? 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 C6 Se1 C1 101.70(14) 3_665 . ? C3 O1 C2 112.1(2) . . ? C4 O2 C5 112.7(2) . . ? C2 C1 Se1 112.6(2) . . ? C2 C1 H1A 109.1 . . ? Se1 C1 H1A 109.1 . . ? C2 C1 H1B 109.1 . . ? Se1 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? O1 C2 C1 107.0(3) . . ? O1 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O1 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.6 . . ? O1 C3 C4 109.1(3) . . ? O1 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? O1 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? O2 C4 C3 109.6(3) . . ? O2 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? O2 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? O2 C5 C6 109.7(3) . . ? O2 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? O2 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? C5 C6 Se1 115.9(2) . 3_665 ? C5 C6 H6A 108.3 . . ? Se1 C6 H6A 108.3 3_665 . ? C5 C6 H6B 108.3 . . ? Se1 C6 H6B 108.3 3_665 . ? H6A C6 H6B 107.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Se1 C1 C2 -65.3(3) 3_665 . . . ? C3 O1 C2 C1 -174.5(3) . . . . ? Se1 C1 C2 O1 -176.9(2) . . . . ? C2 O1 C3 C4 176.8(3) . . . . ? C5 O2 C4 C3 -175.0(3) . . . . ? O1 C3 C4 O2 -67.8(3) . . . . ? C4 O2 C5 C6 -174.3(3) . . . . ? O2 C5 C6 Se1 -67.8(3) . . . 3_665 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.577 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.108 data_12paf086ra _database_code_depnum_ccdc_archive 'CCDC 891796' #TrackingRef '- CaSr_all11_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-05-21 _audit_author_name 'Farina Paolo A.' _chemical_name_systematic ; diiodo(1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane)calcium(II) ; # C12H24O4Se2 = [18]aneO4Se2 # 1,4,10,13-tetraoxo-7,16-diselena-cyclooctadecane # 1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane (iLab defaults) # 1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane (iLab selected options) _chemical_name_common ;diiodo(1,4,10,13-tetraoxa-7,16- diselenacyclooctadecane)calcium(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Ca I2 O4 Se2' _chemical_formula_sum 'C12 H24 Ca I2 O4 Se2' _chemical_formula_weight 684.11 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.808(3) _cell_length_b 11.798(3) _cell_length_c 15.203(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.040(7) _cell_angle_gamma 90.00 _cell_volume 1935.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3551 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description chip _exptl_crystal_colour colourless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 7.284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.464 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4452 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.0842 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2202 _reflns_number_gt 1626 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+67.3800P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2202 _refine_ls_number_parameters 96 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.5000 0.1232(2) 0.2500 0.0135(5) Uani 1 2 d S . . I1 I 0.50026(5) 0.29696(5) 0.09065(4) 0.01795(17) Uani 1 1 d . . . Se1 Se 0.22526(8) 0.18836(8) 0.27349(6) 0.0185(2) Uani 1 1 d . . . O1 O 0.5903(5) -0.0082(5) 0.1480(4) 0.0143(13) Uani 1 1 d . . . O2 O 0.3397(6) 0.0123(5) 0.1498(4) 0.0151(13) Uani 1 1 d . . . C1 C 0.5133(8) -0.1051(8) 0.1255(6) 0.0160(19) Uani 1 1 d . . . H1A H 0.5005 -0.1510 0.1788 0.019 Uiso 1 1 calc R . . H1B H 0.5538 -0.1534 0.0822 0.019 Uiso 1 1 calc R . . C2 C 0.3923(8) -0.0631(8) 0.0874(6) 0.016(2) Uani 1 1 d . . . H2A H 0.4045 -0.0225 0.0315 0.020 Uiso 1 1 calc R . . H2B H 0.3356 -0.1277 0.0747 0.020 Uiso 1 1 calc R . . C3 C 0.2304(8) 0.0668(8) 0.1098(6) 0.018(2) Uani 1 1 d . . . H3A H 0.1887 0.0148 0.0666 0.022 Uiso 1 1 calc R . . H3B H 0.2550 0.1358 0.0780 0.022 Uiso 1 1 calc R . . C4 C 0.1432(8) 0.0980(8) 0.1787(6) 0.017(2) Uani 1 1 d . . . H4A H 0.1091 0.0280 0.2040 0.021 Uiso 1 1 calc R . . H4B H 0.0733 0.1419 0.1513 0.021 Uiso 1 1 calc R . . C5 C 0.2128(9) 0.0773(8) 0.3687(6) 0.019(2) Uani 1 1 d . . . H5A H 0.2464 0.1117 0.4244 0.022 Uiso 1 1 calc R . . H5B H 0.1242 0.0602 0.3758 0.022 Uiso 1 1 calc R . . C6 C 0.2795(8) -0.0306(8) 0.3540(6) 0.0150(19) Uani 1 1 d . . . H6A H 0.2639 -0.0847 0.4019 0.018 Uiso 1 1 calc R . . H6B H 0.2489 -0.0649 0.2975 0.018 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 0.0110(12) 0.0135(13) 0.0161(13) 0.000 0.0017(10) 0.000 I1 0.0164(3) 0.0169(3) 0.0206(3) 0.0021(3) 0.0017(2) 0.0015(2) Se1 0.0141(5) 0.0175(5) 0.0239(5) -0.0012(4) 0.0008(4) 0.0011(4) O1 0.007(3) 0.016(3) 0.020(3) -0.003(3) 0.004(2) -0.003(2) O2 0.013(3) 0.017(3) 0.015(3) -0.004(3) 0.001(2) 0.003(3) C1 0.011(4) 0.017(5) 0.021(5) -0.003(4) 0.007(3) -0.001(4) C2 0.012(4) 0.020(5) 0.017(5) -0.003(4) 0.001(4) -0.007(4) C3 0.018(5) 0.022(5) 0.015(5) 0.002(4) 0.002(4) 0.006(4) C4 0.010(4) 0.019(5) 0.022(5) 0.004(4) -0.006(4) 0.000(4) C5 0.018(5) 0.019(5) 0.018(5) 0.001(4) 0.000(4) 0.001(4) C6 0.006(4) 0.020(5) 0.020(5) 0.003(4) 0.003(3) -0.002(3) _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 O1 2.434(6) . ? Ca1 O1 2.434(6) 2_655 ? Ca1 O2 2.599(6) . ? Ca1 O2 2.599(6) 2_655 ? Ca1 Se1 3.1061(14) 2_655 ? Ca1 Se1 3.1061(14) . ? Ca1 I1 3.1737(19) 2_655 ? Ca1 I1 3.1737(19) . ? Se1 C5 1.963(9) . ? Se1 C4 1.966(9) . ? O1 C6 1.434(9) 2_655 ? O1 C1 1.444(10) . ? O2 C2 1.439(10) . ? O2 C3 1.450(10) . ? C1 C2 1.487(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.492(13) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.485(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O1 1.434(9) 2_655 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? 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 O1 Ca1 O1 100.8(3) . 2_655 ? O1 Ca1 O2 65.3(2) . . ? O1 Ca1 O2 77.0(2) 2_655 . ? O1 Ca1 O2 77.0(2) . 2_655 ? O1 Ca1 O2 65.3(2) 2_655 2_655 ? O2 Ca1 O2 119.5(3) . 2_655 ? O1 Ca1 Se1 70.51(14) . 2_655 ? O1 Ca1 Se1 130.46(15) 2_655 2_655 ? O2 Ca1 Se1 131.97(14) . 2_655 ? O2 Ca1 Se1 65.20(13) 2_655 2_655 ? O1 Ca1 Se1 130.46(15) . . ? O1 Ca1 Se1 70.51(14) 2_655 . ? O2 Ca1 Se1 65.20(13) . . ? O2 Ca1 Se1 131.97(14) 2_655 . ? Se1 Ca1 Se1 151.35(10) 2_655 . ? O1 Ca1 I1 156.16(14) . 2_655 ? O1 Ca1 I1 84.75(15) 2_655 2_655 ? O2 Ca1 I1 138.18(13) . 2_655 ? O2 Ca1 I1 84.57(14) 2_655 2_655 ? Se1 Ca1 I1 88.14(5) 2_655 2_655 ? Se1 Ca1 I1 73.31(4) . 2_655 ? O1 Ca1 I1 84.75(15) . . ? O1 Ca1 I1 156.16(14) 2_655 . ? O2 Ca1 I1 84.57(14) . . ? O2 Ca1 I1 138.18(13) 2_655 . ? Se1 Ca1 I1 73.31(4) 2_655 . ? Se1 Ca1 I1 88.14(5) . . ? I1 Ca1 I1 99.53(8) 2_655 . ? C5 Se1 C4 97.6(4) . . ? C5 Se1 Ca1 91.3(3) . . ? C4 Se1 Ca1 100.3(3) . . ? C6 O1 C1 113.8(6) 2_655 . ? C6 O1 Ca1 123.9(5) 2_655 . ? C1 O1 Ca1 114.2(5) . . ? C2 O2 C3 109.8(6) . . ? C2 O2 Ca1 115.0(5) . . ? C3 O2 Ca1 121.7(5) . . ? O1 C1 C2 108.2(7) . . ? O1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? O1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? O2 C2 C1 108.6(7) . . ? O2 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? O2 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? O2 C3 C4 110.2(7) . . ? O2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? O2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C3 C4 Se1 111.8(6) . . ? C3 C4 H4A 109.3 . . ? Se1 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? Se1 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C6 C5 Se1 114.1(7) . . ? C6 C5 H5A 108.7 . . ? Se1 C5 H5A 108.7 . . ? C6 C5 H5B 108.7 . . ? Se1 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? O1 C6 C5 109.3(7) 2_655 . ? O1 C6 H6A 109.8 2_655 . ? C5 C6 H6A 109.8 . . ? O1 C6 H6B 109.8 2_655 . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 O1 C1 C2 -152.5(7) 2_655 . . . ? Ca1 O1 C1 C2 57.5(8) . . . . ? C3 O2 C2 C1 172.1(7) . . . . ? Ca1 O2 C2 C1 30.4(8) . . . . ? O1 C1 C2 O2 -56.1(9) . . . . ? C2 O2 C3 C4 152.7(7) . . . . ? Ca1 O2 C3 C4 -68.6(9) . . . . ? O2 C3 C4 Se1 53.3(9) . . . . ? C5 Se1 C4 C3 -114.0(7) . . . . ? Ca1 Se1 C4 C3 -21.3(7) . . . . ? C4 Se1 C5 C6 61.9(7) . . . . ? Ca1 Se1 C5 C6 -38.6(7) . . . . ? Se1 C5 C6 O1 63.9(9) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.275 _refine_diff_density_min -1.465 _refine_diff_density_rms 0.291 data_12paf088ra _database_code_depnum_ccdc_archive 'CCDC 891797' #TrackingRef '- CaSr_all11_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-05-22 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trisaqua(1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane)strontium(II) iodide ; # C12H24O4Se2 = [18]aneO4Se2 # 1,4,10,13-tetraoxo-7,16-diselena-cyclooctadecane # 1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane (iLab defaults) # 1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane (iLab selected options) _chemical_name_common ;trisaqua(1,4,10,13-tetraoxa-7,16- diselenacyclooctadecane)strontium(ii) iodide ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H30 O7 Se2 Sr 2+, 2(I 1-)' _chemical_formula_sum 'C12 H30 I2 O7 Se2 Sr' _chemical_formula_structural '((C12 H24 O4 Se2) (H2 O)3 Sr) I2' _chemical_formula_weight 785.70 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' Se Se -0.0929 2.2259 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' 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 10.2300(18) _cell_length_b 14.005(2) _cell_length_c 16.244(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.305(6) _cell_angle_gamma 90.00 _cell_volume 2326.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14213 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.6 _exptl_crystal_description chip _exptl_crystal_colour colourless _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 8.125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.464 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19785 _diffrn_reflns_av_R_equivalents 0.1480 _diffrn_reflns_av_sigmaI/netI 0.1503 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5295 _reflns_number_gt 3089 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0951P)^2^+32.8566P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5295 _refine_ls_number_parameters 217 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1527 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.2391 _refine_ls_wR_factor_gt 0.2043 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.039 _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 Sr1 Sr 0.16439(13) 0.37637(11) 0.23691(9) 0.0216(3) Uani 1 1 d . . . I1 I 0.66186(10) 0.71443(8) 0.08332(7) 0.0307(3) Uani 1 1 d . . . I2 I 0.85127(10) 0.19437(8) 0.05451(7) 0.0301(3) Uani 1 1 d . . . Se1 Se 0.43569(18) 0.26819(14) 0.25237(13) 0.0413(5) Uani 1 1 d U . . Se2 Se -0.14512(17) 0.41598(14) 0.21681(12) 0.0359(5) Uani 1 1 d U . . O1 O 0.3605(9) 0.4439(7) 0.1424(6) 0.022(2) Uani 1 1 d U . . O2 O 0.1057(11) 0.5086(8) 0.1257(7) 0.032(3) Uani 1 1 d U . . O3 O 0.0724(10) 0.5220(8) 0.3340(7) 0.028(2) Uani 1 1 d U . . O4 O 0.3371(10) 0.4574(7) 0.3406(6) 0.023(2) Uani 1 1 d U . . O5 O 0.1610(11) 0.2878(8) 0.0980(7) 0.033(3) Uani 1 1 d . . . O6 O 0.0332(11) 0.2102(9) 0.2401(7) 0.035(3) Uani 1 1 d . . . O7 O 0.1456(11) 0.3086(8) 0.3829(6) 0.030(3) Uani 1 1 d . . . C1 C 0.5010(16) 0.3055(14) 0.1487(12) 0.038(3) Uani 1 1 d U . . H1A H 0.5945 0.2876 0.1476 0.046 Uiso 1 1 calc R . . H1B H 0.4550 0.2674 0.1057 0.046 Uiso 1 1 calc R . . C2 C 0.4897(15) 0.4103(13) 0.1244(11) 0.033(3) Uani 1 1 d U . . H2A H 0.5558 0.4484 0.1555 0.040 Uiso 1 1 calc R . . H2B H 0.5060 0.4177 0.0649 0.040 Uiso 1 1 calc R . . C3 C 0.3307(14) 0.5259(10) 0.0930(10) 0.023(3) Uani 1 1 d U . . H3A H 0.3145 0.5067 0.0350 0.028 Uiso 1 1 calc R . . H3B H 0.4048 0.5714 0.0949 0.028 Uiso 1 1 calc R . . C4 C 0.2103(15) 0.5718(12) 0.1272(11) 0.031(4) Uani 1 1 d U . . H4A H 0.2287 0.5924 0.1846 0.037 Uiso 1 1 calc R . . H4B H 0.1873 0.6291 0.0942 0.037 Uiso 1 1 calc R . . C5 C -0.0176(15) 0.5540(12) 0.1091(11) 0.031(3) Uani 1 1 d U . . H5A H -0.0173 0.5835 0.0538 0.037 Uiso 1 1 calc R . . H5B H -0.0314 0.6052 0.1500 0.037 Uiso 1 1 calc R . . C6 C -0.1255(16) 0.4837(12) 0.1131(12) 0.033(3) Uani 1 1 d U . . H6A H -0.1129 0.4358 0.0692 0.040 Uiso 1 1 calc R . . H6B H -0.2085 0.5175 0.1002 0.040 Uiso 1 1 calc R . . C7 C -0.1553(15) 0.5250(14) 0.2925(12) 0.037(4) Uani 1 1 d U . . H7A H -0.1419 0.5845 0.2610 0.045 Uiso 1 1 calc R . . H7B H -0.2444 0.5274 0.3151 0.045 Uiso 1 1 calc R . . C8 C -0.0600(16) 0.5221(13) 0.3614(12) 0.036(4) Uani 1 1 d U . . H8A H -0.0734 0.5782 0.3973 0.043 Uiso 1 1 calc R . . H8B H -0.0751 0.4640 0.3945 0.043 Uiso 1 1 calc R . . C9 C 0.1564(15) 0.5381(12) 0.4030(10) 0.026(3) Uani 1 1 d U . . H9A H 0.1496 0.4844 0.4424 0.032 Uiso 1 1 calc R . . H9B H 0.1309 0.5975 0.4314 0.032 Uiso 1 1 calc R . . C10 C 0.2945(16) 0.5463(12) 0.3742(11) 0.030(3) Uani 1 1 d U . . H10A H 0.2995 0.5969 0.3318 0.036 Uiso 1 1 calc R . . H10B H 0.3528 0.5646 0.4211 0.036 Uiso 1 1 calc R . . C11 C 0.4742(15) 0.4548(13) 0.3309(11) 0.032(3) Uani 1 1 d U . . H11A H 0.5180 0.4887 0.3773 0.039 Uiso 1 1 calc R . . H11B H 0.4969 0.4878 0.2792 0.039 Uiso 1 1 calc R . . C12 C 0.5210(15) 0.3549(14) 0.3282(11) 0.036(3) Uani 1 1 d U . . H12A H 0.5138 0.3278 0.3842 0.044 Uiso 1 1 calc R . . H12B H 0.6151 0.3562 0.3153 0.044 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 Sr1 0.0164(7) 0.0282(8) 0.0204(8) 0.0014(6) 0.0042(6) -0.0004(6) I1 0.0219(5) 0.0417(7) 0.0288(6) -0.0029(5) 0.0087(4) 0.0018(5) I2 0.0218(5) 0.0415(7) 0.0270(6) 0.0018(5) 0.0011(4) -0.0046(5) Se1 0.0296(10) 0.0419(11) 0.0526(13) 0.0076(9) 0.0081(9) 0.0026(8) Se2 0.0228(9) 0.0423(11) 0.0431(11) -0.0011(8) 0.0081(8) -0.0010(8) O1 0.015(5) 0.029(5) 0.024(6) 0.002(4) 0.008(4) 0.003(4) O2 0.023(4) 0.031(6) 0.042(7) 0.005(5) 0.017(5) 0.001(4) O3 0.022(4) 0.037(6) 0.026(6) 0.007(5) 0.004(4) 0.005(5) O4 0.019(4) 0.027(5) 0.024(6) -0.001(4) 0.005(4) -0.004(4) O5 0.030(6) 0.036(7) 0.033(7) -0.012(5) 0.005(5) -0.010(5) O6 0.026(6) 0.046(7) 0.034(7) 0.006(6) 0.007(5) 0.007(6) O7 0.041(7) 0.037(7) 0.013(5) -0.003(5) -0.002(5) -0.010(6) C1 0.016(7) 0.059(8) 0.040(6) 0.001(7) 0.007(6) 0.022(7) C2 0.016(6) 0.056(8) 0.029(9) -0.002(6) 0.016(6) 0.006(6) C3 0.019(5) 0.019(7) 0.032(9) -0.005(5) -0.003(6) -0.010(5) C4 0.018(5) 0.034(8) 0.040(10) 0.005(8) -0.002(6) 0.002(4) C5 0.023(5) 0.036(9) 0.032(9) 0.003(6) -0.011(7) -0.007(5) C6 0.027(6) 0.029(8) 0.044(6) -0.008(5) 0.012(8) -0.004(6) C7 0.015(5) 0.051(10) 0.047(7) -0.008(7) 0.017(6) 0.009(8) C8 0.024(5) 0.038(10) 0.045(9) -0.007(7) 0.014(5) 0.004(7) C9 0.030(5) 0.029(8) 0.021(7) -0.005(7) 0.008(5) -0.003(6) C10 0.026(5) 0.030(7) 0.035(10) -0.007(7) 0.005(6) -0.006(6) C11 0.016(5) 0.056(7) 0.025(9) 0.001(6) 0.014(6) -0.007(6) C12 0.009(6) 0.064(8) 0.037(8) 0.007(7) 0.008(6) 0.003(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 Sr1 O7 2.565(11) . ? Sr1 O5 2.575(11) . ? Sr1 O2 2.648(12) . ? Sr1 O4 2.666(10) . ? Sr1 O6 2.688(12) . ? Sr1 O1 2.723(10) . ? Sr1 O3 2.756(11) . ? Sr1 Se1 3.167(2) . ? Sr1 Se2 3.224(2) . ? Se1 C1 1.899(19) . ? Se1 C12 1.925(19) . ? Se2 C6 1.948(19) . ? Se2 C7 1.965(18) . ? O1 C3 1.430(18) . ? O1 C2 1.440(17) . ? O2 C4 1.388(19) . ? O2 C5 1.432(18) . ? O3 C9 1.415(18) . ? O3 C8 1.435(18) . ? O4 C11 1.416(17) . ? O4 C10 1.432(19) . ? C1 C2 1.52(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.51(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.48(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.47(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.50(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.48(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? 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 O7 Sr1 O5 129.2(4) . . ? O7 Sr1 O2 150.4(4) . . ? O5 Sr1 O2 75.0(4) . . ? O7 Sr1 O4 68.7(3) . . ? O5 Sr1 O4 139.0(3) . . ? O2 Sr1 O4 105.7(3) . . ? O7 Sr1 O6 67.3(4) . . ? O5 Sr1 O6 66.6(4) . . ? O2 Sr1 O6 120.9(4) . . ? O4 Sr1 O6 132.9(3) . . ? O7 Sr1 O1 136.2(3) . . ? O5 Sr1 O1 70.7(3) . . ? O2 Sr1 O1 62.0(3) . . ? O4 Sr1 O1 73.9(3) . . ? O6 Sr1 O1 133.4(3) . . ? O7 Sr1 O3 73.2(3) . . ? O5 Sr1 O3 149.3(3) . . ? O2 Sr1 O3 78.3(3) . . ? O4 Sr1 O3 63.5(3) . . ? O6 Sr1 O3 116.9(3) . . ? O1 Sr1 O3 109.3(3) . . ? O7 Sr1 Se1 80.4(3) . . ? O5 Sr1 Se1 80.4(3) . . ? O2 Sr1 Se1 125.0(2) . . ? O4 Sr1 Se1 65.6(2) . . ? O6 Sr1 Se1 91.2(2) . . ? O1 Sr1 Se1 63.6(2) . . ? O3 Sr1 Se1 128.2(2) . . ? O7 Sr1 Se2 93.6(3) . . ? O5 Sr1 Se2 90.0(3) . . ? O2 Sr1 Se2 66.6(2) . . ? O4 Sr1 Se2 128.7(2) . . ? O6 Sr1 Se2 70.2(2) . . ? O1 Sr1 Se2 128.1(2) . . ? O3 Sr1 Se2 65.4(2) . . ? Se1 Sr1 Se2 161.32(7) . . ? C1 Se1 C12 103.3(8) . . ? C1 Se1 Sr1 97.1(5) . . ? C12 Se1 Sr1 97.6(5) . . ? C6 Se2 C7 99.8(8) . . ? C6 Se2 Sr1 92.9(5) . . ? C7 Se2 Sr1 97.8(5) . . ? C3 O1 C2 109.4(12) . . ? C3 O1 Sr1 116.5(8) . . ? C2 O1 Sr1 133.9(9) . . ? C4 O2 C5 113.4(12) . . ? C4 O2 Sr1 105.7(9) . . ? C5 O2 Sr1 128.6(9) . . ? C9 O3 C8 108.4(12) . . ? C9 O3 Sr1 111.2(9) . . ? C8 O3 Sr1 121.0(9) . . ? C11 O4 C10 112.1(12) . . ? C11 O4 Sr1 124.2(9) . . ? C10 O4 Sr1 114.1(8) . . ? C2 C1 Se1 117.9(12) . . ? C2 C1 H1A 107.8 . . ? Se1 C1 H1A 107.8 . . ? C2 C1 H1B 107.8 . . ? Se1 C1 H1B 107.8 . . ? H1A C1 H1B 107.2 . . ? O1 C2 C1 109.0(13) . . ? O1 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O1 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O1 C3 C4 107.5(13) . . ? O1 C3 H3A 110.2 . . ? C4 C3 H3A 110.2 . . ? O1 C3 H3B 110.2 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? O2 C4 C3 111.0(13) . . ? O2 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? O2 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? O2 C5 C6 110.6(14) . . ? O2 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? O2 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C5 C6 Se2 116.9(12) . . ? C5 C6 H6A 108.1 . . ? Se2 C6 H6A 108.1 . . ? C5 C6 H6B 108.1 . . ? Se2 C6 H6B 108.1 . . ? H6A C6 H6B 107.3 . . ? C8 C7 Se2 114.3(12) . . ? C8 C7 H7A 108.7 . . ? Se2 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? Se2 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? O3 C8 C7 112.3(15) . . ? O3 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? O3 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? O3 C9 C10 108.9(13) . . ? O3 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? O3 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? O4 C10 C9 110.4(13) . . ? O4 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? O4 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? O4 C11 C12 110.4(14) . . ? O4 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? O4 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C11 C12 Se1 118.2(12) . . ? C11 C12 H12A 107.8 . . ? Se1 C12 H12A 107.8 . . ? C11 C12 H12B 107.8 . . ? Se1 C12 H12B 107.8 . . ? H12A C12 H12B 107.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 Se1 C1 C2 -52.8(14) . . . . ? Sr1 Se1 C1 C2 46.8(13) . . . . ? C3 O1 C2 C1 -157.6(13) . . . . ? Sr1 O1 C2 C1 16(2) . . . . ? Se1 C1 C2 O1 -45.4(18) . . . . ? C2 O1 C3 C4 -167.1(13) . . . . ? Sr1 O1 C3 C4 17.9(14) . . . . ? C5 O2 C4 C3 -145.0(14) . . . . ? Sr1 O2 C4 C3 69.3(14) . . . . ? O1 C3 C4 O2 -59.3(17) . . . . ? C4 O2 C5 C6 -176.8(14) . . . . ? Sr1 O2 C5 C6 -40.6(19) . . . . ? O2 C5 C6 Se2 59.1(17) . . . . ? C7 Se2 C6 C5 54.0(14) . . . . ? Sr1 Se2 C6 C5 -44.5(13) . . . . ? C6 Se2 C7 C8 -125.6(14) . . . . ? Sr1 Se2 C7 C8 -31.2(14) . . . . ? C9 O3 C8 C7 168.6(14) . . . . ? Sr1 O3 C8 C7 -61.3(17) . . . . ? Se2 C7 C8 O3 60.5(18) . . . . ? C8 O3 C9 C10 -175.3(13) . . . . ? Sr1 O3 C9 C10 49.4(14) . . . . ? C11 O4 C10 C9 -166.0(13) . . . . ? Sr1 O4 C10 C9 46.1(15) . . . . ? O3 C9 C10 O4 -65.4(17) . . . . ? C10 O4 C11 C12 157.7(14) . . . . ? Sr1 O4 C11 C12 -58.3(16) . . . . ? O4 C11 C12 Se1 51.5(17) . . . . ? C1 Se1 C12 C11 74.9(14) . . . . ? # Sr1 Se1 C12 C11 -24.3(13) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O5 I1 3.493(12) . 3_665 ? O5 I2 3.485(11) . 1_455 ? O6 I1 3.531(12) . 2_545 ? O6 I2 3.514(12) . 1_455 ? O7 I1 3.466(12) . 2_545 ? O7 I2 3.455(10) . 4_566 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.969 _refine_diff_density_min -2.138 _refine_diff_density_rms 0.336 data_12paf091ra _database_code_depnum_ccdc_archive 'CCDC 891798' #TrackingRef '- CaSr_all11_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-06-12 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trisaqua(1,4,7-trioxa-10,13-dithiacyclopentadecane)strontium iodide ; # C10H20O3S2 = [15]aneO3S2 # 1,4,7-trioxa-10,13-dithiacyclopentadecane (iLab defaults) # 1,4,7-trioxa-10,13-dithiacyclopentadecane (iLab selected options) # 1,4,7-trioxa-10,13-dithiacyclopentadecane (Chemspider) _chemical_name_common ;trisaqua(1,4,7-trioxa-10,13-dithiacyclopentadecane)strontium iodide ; _chemical_melting_point ? _chemical_formula_moiety 'C10 H26 O6 S2 Sr 2+, 2(I 1-)' _chemical_formula_sum 'C10 H26 I2 O6 S2 Sr' _chemical_formula_structural '((C10 H20 O5) (H2 O)3 Sr) (I)2' _chemical_formula_weight 647.85 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.506(4) _cell_length_b 17.630(7) _cell_length_c 12.782(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.101(7) _cell_angle_gamma 90.00 _cell_volume 2140.7(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7808 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 5.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.741 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9930 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0946 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3986 _reflns_number_gt 2685 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+15.1124P] 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 constr _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 0.080(18) _chemical_absolute_configuration ad _refine_ls_number_reflns 3986 _refine_ls_number_parameters 190 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.002 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 Sr1 Sr 0.84555(14) 0.36958(7) 1.00678(11) 0.0438(3) Uani 1 1 d . . . I1 I 0.17226(12) 0.48565(5) 0.74739(9) 0.0645(4) Uani 1 1 d . . . I2 I 0.30099(14) 0.18726(6) 0.92880(10) 0.0712(4) Uani 1 1 d . . . S1 S 0.5839(6) 0.4638(3) 1.0515(6) 0.097(2) Uani 1 1 d D . . S2 S 0.7361(7) 0.4508(4) 0.8108(5) 0.0991(18) Uani 1 1 d D . . O1 O 0.7819(11) 0.2784(6) 0.8390(9) 0.068(4) Uani 1 1 d D . . O2 O 0.8711(17) 0.2215(6) 1.0358(10) 0.080(4) Uani 1 1 d D . . O3 O 0.6487(11) 0.2978(6) 1.1104(12) 0.078(4) Uani 1 1 d D . . O4 O 1.0908(13) 0.3518(6) 0.9421(12) 0.078(4) Uani 1 1 d . . . O5 O 0.9391(12) 0.3706(6) 1.1949(9) 0.063(3) Uani 1 1 d . . . O6 O 0.9422(14) 0.5036(6) 1.0231(10) 0.069(3) Uani 1 1 d . . . C1 C 0.522(4) 0.4894(19) 0.9216(17) 0.26(3) Uani 1 1 d D . . H1A H 0.4181 0.4915 0.9252 0.314 Uiso 1 1 calc R . . H1B H 0.5530 0.5425 0.9122 0.314 Uiso 1 1 calc R . . C2 C 0.5487(19) 0.451(2) 0.821(2) 0.176(16) Uani 1 1 d D . . H2A H 0.5037 0.4797 0.7615 0.211 Uiso 1 1 calc R . . H2B H 0.5113 0.3989 0.8202 0.211 Uiso 1 1 calc R . . C3 C 0.748(3) 0.3765(10) 0.7142(16) 0.127(10) Uani 1 1 d D . . H3A H 0.6910 0.3911 0.6509 0.152 Uiso 1 1 calc R . . H3B H 0.8468 0.3715 0.6941 0.152 Uiso 1 1 calc R . . C4 C 0.6968(16) 0.3005(9) 0.7525(16) 0.083(7) Uani 1 1 d D . . H4A H 0.5975 0.3045 0.7727 0.100 Uiso 1 1 calc R . . H4B H 0.7022 0.2623 0.6960 0.100 Uiso 1 1 calc R . . C5 C 0.752(2) 0.2009(9) 0.8676(19) 0.108(10) Uani 1 1 d D . . H5A H 0.6571 0.1977 0.8962 0.130 Uiso 1 1 calc R . . H5B H 0.7542 0.1682 0.8047 0.130 Uiso 1 1 calc R . . C6 C 0.859(3) 0.1735(11) 0.9475(17) 0.109(9) Uani 1 1 d D . . H6A H 0.8319 0.1220 0.9706 0.130 Uiso 1 1 calc R . . H6B H 0.9513 0.1697 0.9150 0.130 Uiso 1 1 calc R . . C7 C 0.817(2) 0.2040(10) 1.133(2) 0.141(14) Uani 1 1 d D . . H7A H 0.8672 0.2339 1.1882 0.169 Uiso 1 1 calc R . . H7B H 0.8331 0.1496 1.1483 0.169 Uiso 1 1 calc R . . C8 C 0.6621(17) 0.2202(7) 1.1368(18) 0.076(6) Uani 1 1 d D . . H8A H 0.6082 0.1882 1.0859 0.091 Uiso 1 1 calc R . . H8B H 0.6276 0.2105 1.2077 0.091 Uiso 1 1 calc R . . C9 C 0.538(2) 0.3375(11) 1.1476(16) 0.101(9) Uani 1 1 d D . . H9A H 0.5736 0.3720 1.2036 0.121 Uiso 1 1 calc R . . H9B H 0.4723 0.3013 1.1795 0.121 Uiso 1 1 calc R . . C10 C 0.455(2) 0.3850(12) 1.064(2) 0.24(3) Uani 1 1 d D . . H10A H 0.3636 0.4030 1.0898 0.286 Uiso 1 1 calc R . . H10B H 0.4392 0.3568 0.9977 0.286 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 Sr1 0.0485(9) 0.0374(6) 0.0456(8) -0.0049(6) 0.0022(7) -0.0035(6) I1 0.0613(7) 0.0437(5) 0.0862(9) -0.0042(6) -0.0280(6) 0.0129(5) I2 0.1097(11) 0.0511(5) 0.0523(6) -0.0090(5) -0.0036(6) 0.0233(6) S1 0.058(3) 0.068(3) 0.164(6) -0.038(4) 0.010(4) 0.004(2) S2 0.102(5) 0.111(4) 0.081(4) 0.007(3) -0.035(3) 0.013(4) O1 0.038(7) 0.076(7) 0.088(9) -0.051(7) -0.026(6) 0.017(5) O2 0.124(12) 0.046(6) 0.070(8) 0.003(6) 0.002(8) 0.028(7) O3 0.035(7) 0.067(7) 0.132(12) -0.026(7) 0.017(7) -0.005(5) O4 0.064(8) 0.062(7) 0.110(11) -0.021(7) 0.029(8) -0.008(6) O5 0.058(7) 0.068(7) 0.061(7) 0.013(5) -0.018(6) -0.028(5) O6 0.079(9) 0.041(5) 0.085(8) 0.017(5) -0.022(7) -0.005(5) C1 0.19(4) 0.25(4) 0.32(6) -0.20(4) -0.21(4) 0.17(3) C2 0.11(3) 0.26(4) 0.16(3) -0.08(3) -0.06(2) 0.05(3) C3 0.18(3) 0.105(18) 0.096(19) -0.017(15) -0.05(2) 0.039(17) C4 0.028(11) 0.077(11) 0.14(2) -0.039(13) -0.042(12) 0.019(8) C5 0.082(16) 0.073(13) 0.17(3) -0.076(16) 0.037(17) -0.031(12) C6 0.13(2) 0.062(12) 0.14(3) 0.003(14) 0.036(19) 0.024(12) C7 0.13(2) 0.030(9) 0.27(4) 0.017(14) 0.06(3) -0.012(10) C8 0.051(12) 0.042(8) 0.135(19) 0.012(10) 0.019(12) -0.001(7) C9 0.13(2) 0.095(13) 0.084(14) 0.043(12) 0.096(15) 0.077(14) C10 0.044(17) 0.16(3) 0.51(8) -0.18(4) -0.02(3) 0.003(16) _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 Sr1 O4 2.522(12) . ? Sr1 O5 2.533(11) . ? Sr1 O6 2.542(10) . ? Sr1 O2 2.646(11) . ? Sr1 O3 2.653(11) . ? Sr1 O1 2.730(10) . ? Sr1 S2 3.036(6) . ? Sr1 S1 3.062(5) . ? S1 C1 1.799(18) . ? S1 C10 1.865(17) . ? S2 C2 1.790(17) . ? S2 C3 1.806(16) . ? O1 C4 1.402(15) . ? O1 C5 1.445(15) . ? O2 C7 1.399(17) . ? O2 C6 1.413(16) . ? O3 C9 1.365(13) . ? O3 C8 1.414(14) . ? C1 C2 1.485(18) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.511(18) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.491(17) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.498(17) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.549(19) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? 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 O4 Sr1 O5 90.9(4) . . ? O4 Sr1 O6 78.9(4) . . ? O5 Sr1 O6 78.6(4) . . ? O4 Sr1 O2 80.9(4) . . ? O5 Sr1 O2 81.2(4) . . ? O6 Sr1 O2 151.0(4) . . ? O4 Sr1 O3 141.4(4) . . ? O5 Sr1 O3 76.0(4) . . ? O6 Sr1 O3 131.4(4) . . ? O2 Sr1 O3 61.5(4) . . ? O4 Sr1 O1 81.4(4) . . ? O5 Sr1 O1 144.1(4) . . ? O6 Sr1 O1 132.9(4) . . ? O2 Sr1 O1 63.0(4) . . ? O3 Sr1 O1 88.4(4) . . ? O4 Sr1 S2 94.7(4) . . ? O5 Sr1 S2 151.4(3) . . ? O6 Sr1 S2 75.0(3) . . ? O2 Sr1 S2 127.4(3) . . ? O3 Sr1 S2 114.2(3) . . ? O1 Sr1 S2 64.5(3) . . ? O4 Sr1 S1 153.6(3) . . ? O5 Sr1 S1 94.5(3) . . ? O6 Sr1 S1 76.9(3) . . ? O2 Sr1 S1 125.4(4) . . ? O3 Sr1 S1 64.7(3) . . ? O1 Sr1 S1 107.9(2) . . ? S2 Sr1 S1 69.0(2) . . ? C1 S1 C10 94.2(17) . . ? C1 S1 Sr1 101.8(9) . . ? C10 S1 Sr1 98.8(8) . . ? C2 S2 C3 97.9(14) . . ? C2 S2 Sr1 104.9(13) . . ? C3 S2 Sr1 101.2(8) . . ? C4 O1 C5 110.5(14) . . ? C4 O1 Sr1 124.1(9) . . ? C5 O1 Sr1 113.4(11) . . ? C7 O2 C6 123.7(18) . . ? C7 O2 Sr1 107.9(9) . . ? C6 O2 Sr1 118.3(11) . . ? C9 O3 C8 118.5(13) . . ? C9 O3 Sr1 119.8(10) . . ? C8 O3 Sr1 121.5(9) . . ? C2 C1 S1 129(2) . . ? C2 C1 H1A 105.1 . . ? S1 C1 H1A 105.1 . . ? C2 C1 H1B 105.1 . . ? S1 C1 H1B 105.1 . . ? H1A C1 H1B 105.9 . . ? C1 C2 S2 105(2) . . ? C1 C2 H2A 110.7 . . ? S2 C2 H2A 110.7 . . ? C1 C2 H2B 110.7 . . ? S2 C2 H2B 110.7 . . ? H2A C2 H2B 108.8 . . ? C4 C3 S2 113.2(15) . . ? C4 C3 H3A 108.9 . . ? S2 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? S2 C3 H3B 108.9 . . ? H3A C3 H3B 107.8 . . ? O1 C4 C3 108.6(14) . . ? O1 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? O1 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.3 . . ? C6 C5 O1 110.3(16) . . ? C6 C5 H5A 109.6 . . ? O1 C5 H5A 109.6 . . ? C6 C5 H5B 109.6 . . ? O1 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? O2 C6 C5 112.8(17) . . ? O2 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? O2 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 C8 112(2) . . ? O2 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? O2 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? O3 C8 C7 104.9(13) . . ? O3 C8 H8A 110.8 . . ? C7 C8 H8A 110.8 . . ? O3 C8 H8B 110.8 . . ? C7 C8 H8B 110.8 . . ? H8A C8 H8B 108.8 . . ? O3 C9 C10 114.7(17) . . ? O3 C9 H9A 108.6 . . ? C10 C9 H9A 108.6 . . ? O3 C9 H9B 108.6 . . ? C10 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C9 C10 S1 98.1(13) . . ? C9 C10 H10A 112.1 . . ? S1 C10 H10A 112.1 . . ? C9 C10 H10B 112.1 . . ? S1 C10 H10B 112.1 . . ? H10A C10 H10B 109.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 S1 C1 C2 -77(4) . . . . ? Sr1 S1 C1 C2 23(4) . . . . ? S1 C1 C2 S2 -58(5) . . . . ? C3 S2 C2 C1 161(3) . . . . ? Sr1 S2 C2 C1 57(3) . . . . ? C2 S2 C3 C4 -64(2) . . . . ? Sr1 S2 C3 C4 43.2(19) . . . . ? C5 O1 C4 C3 -170.6(16) . . . . ? Sr1 O1 C4 C3 49.3(18) . . . . ? S2 C3 C4 O1 -62(2) . . . . ? C4 O1 C5 C6 170.5(16) . . . . ? Sr1 O1 C5 C6 -44.9(19) . . . . ? C7 O2 C6 C5 105(2) . . . . ? Sr1 O2 C6 C5 -36(3) . . . . ? O1 C5 C6 O2 54(3) . . . . ? C6 O2 C7 C8 -81(2) . . . . ? Sr1 O2 C7 C8 63.9(18) . . . . ? C9 O3 C8 C7 -153(2) . . . . ? Sr1 O3 C8 C7 21(2) . . . . ? O2 C7 C8 O3 -57(2) . . . . ? C8 O3 C9 C10 -131.3(19) . . . . ? Sr1 O3 C9 C10 54(2) . . . . ? O3 C9 C10 S1 -75(2) . . . . ? C1 S1 C10 C9 156.0(16) . . . . ? Sr1 S1 C10 C9 53.4(15) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O4 I1 3.536(14) . 1_655 ? O4 I2 3.530(12) . 1_655 ? O5 I1 3.417(10) . 2_665 ? O5 I2 3.463(12) . 4 ? O6 I1 3.546(12) . 2_665 ? O6 I2 3.690(10) . 3 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.539 _refine_diff_density_min -1.116 _refine_diff_density_rms 0.167 data_12paf093r _database_code_depnum_ccdc_archive 'CCDC 891799' #TrackingRef '- CaSr_all11_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-06-14 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trisaqua(1,4,10,13-tetraoxa-7,16-dithiacyclooctadecane)strontium iodide hydrate ; # C12H24O4S2 = [18]aneO4S2 # 1,4,10,13-tetraoxo-7,16-dithia-cyclooctadecane # 1,4,10,13-tetraoxa-7,16-dithiacyclooctadecane (iLab defaults) # 1,4,10,13-tetraoxa-7,16-dithiacyclooctadecane (iLab selected options) _chemical_name_common ;trisaqua(1,4,10,13-tetraoxa-7,16- dithiacyclooctadecane)strontium iodide hydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H30 O7 S2 Sr 2+, 2(I 1-), (H2 O)' _chemical_formula_sum 'C12 H32 I2 O8 S2 Sr' _chemical_formula_structural '((C12 H24 O4 S2) (H2O)3 Sr) (I)2 (H2O)' _chemical_formula_weight 709.92 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' 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 10.452(4) _cell_length_b 18.580(7) _cell_length_c 13.866(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.182(6) _cell_angle_gamma 90.00 _cell_volume 2493.5(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16629 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 4.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.587 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23787 _diffrn_reflns_av_R_equivalents 0.1294 _diffrn_reflns_av_sigmaI/netI 0.1294 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5671 _reflns_number_gt 3431 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+8.8913P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5671 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1233 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1578 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Sr1 Sr 0.40102(10) 0.90719(5) 0.73140(7) 0.0182(2) Uani 1 1 d . . . I1 I 0.83788(8) 1.12098(4) 0.87865(5) 0.02672(19) Uani 1 1 d . . . I2 I 0.28252(8) 1.17467(4) 0.67625(6) 0.0313(2) Uani 1 1 d . . . S1 S 0.5782(3) 0.92842(14) 0.96548(19) 0.0253(6) Uani 1 1 d . . . S2 S 0.2191(3) 0.96310(16) 0.5105(2) 0.0359(7) Uani 1 1 d . . . O1 O 0.2988(8) 0.8469(4) 0.8638(5) 0.0251(16) Uani 1 1 d . . . O2 O 0.1471(7) 0.8465(4) 0.6495(5) 0.0268(16) Uani 1 1 d . . . O3 O 0.5121(8) 0.8964(3) 0.5811(5) 0.0248(16) Uani 1 1 d . . . O4 O 0.6697(7) 0.8728(3) 0.7933(5) 0.0218(15) Uani 1 1 d . . . O5 O 0.5177(8) 1.0307(4) 0.7345(5) 0.0286(17) Uani 1 1 d . . . O6 O 0.2357(8) 0.9977(4) 0.7599(5) 0.0283(17) Uani 1 1 d . . . O7 O 0.4127(8) 0.7699(4) 0.7042(5) 0.0283(17) Uani 1 1 d . . . O8 O 0.0736(8) 0.9786(4) 0.8763(6) 0.0361(19) Uani 1 1 d . . . C1 C 0.4770(11) 0.8782(5) 1.0258(7) 0.025(2) Uani 1 1 d . . . H1A H 0.5403 0.8591 1.0937 0.029 Uiso 1 1 calc R . . H1B H 0.4120 0.9117 1.0394 0.029 Uiso 1 1 calc R . . C2 C 0.3984(12) 0.8183(5) 0.9617(7) 0.027(2) Uani 1 1 d . . . H2A H 0.4620 0.7844 0.9473 0.032 Uiso 1 1 calc R . . H2B H 0.3491 0.7920 0.9994 0.032 Uiso 1 1 calc R . . C3 C 0.1866(12) 0.7980(6) 0.8164(9) 0.034(3) Uani 1 1 d . . . H3A H 0.1421 0.7864 0.8661 0.041 Uiso 1 1 calc R . . H3B H 0.2217 0.7527 0.7978 0.041 Uiso 1 1 calc R . . C4 C 0.0853(11) 0.8312(6) 0.7224(8) 0.027(2) Uani 1 1 d . . . H4A H 0.0063 0.7981 0.6906 0.033 Uiso 1 1 calc R . . H4B H 0.0500 0.8762 0.7413 0.033 Uiso 1 1 calc R . . C5 C 0.0407(14) 0.8695(9) 0.5543(10) 0.064(4) Uani 1 1 d . . . H5A H -0.0047 0.9133 0.5670 0.076 Uiso 1 1 calc R . . H5B H -0.0301 0.8314 0.5278 0.076 Uiso 1 1 calc R . . C6 C 0.1040(14) 0.8857(10) 0.4739(10) 0.070(5) Uani 1 1 d . . . H6A H 0.0292 0.8950 0.4055 0.084 Uiso 1 1 calc R . . H6B H 0.1563 0.8430 0.4663 0.084 Uiso 1 1 calc R . . C7 C 0.3250(11) 0.9436(6) 0.4346(8) 0.029(2) Uani 1 1 d . . . H7A H 0.2633 0.9329 0.3619 0.034 Uiso 1 1 calc R . . H7B H 0.3793 0.9870 0.4334 0.034 Uiso 1 1 calc R . . C8 C 0.4206(13) 0.8825(6) 0.4754(7) 0.033(3) Uani 1 1 d . . . H8A H 0.3671 0.8381 0.4728 0.039 Uiso 1 1 calc R . . H8B H 0.4753 0.8751 0.4315 0.039 Uiso 1 1 calc R . . C9 C 0.6339(11) 0.8494(5) 0.6153(8) 0.026(2) Uani 1 1 d . . . H9A H 0.6061 0.7993 0.6216 0.031 Uiso 1 1 calc R . . H9B H 0.6782 0.8504 0.5635 0.031 Uiso 1 1 calc R . . C10 C 0.7320(11) 0.8752(6) 0.7171(8) 0.031(3) Uani 1 1 d . . . H10A H 0.8157 0.8446 0.7402 0.037 Uiso 1 1 calc R . . H10B H 0.7601 0.9251 0.7101 0.037 Uiso 1 1 calc R . . C11 C 0.7740(11) 0.8807(6) 0.8977(7) 0.027(2) Uani 1 1 d . . . H11A H 0.8083 0.9309 0.9084 0.032 Uiso 1 1 calc R . . H11B H 0.8531 0.8485 0.9062 0.032 Uiso 1 1 calc R . . C12 C 0.7141(11) 0.8622(6) 0.9761(8) 0.028(2) Uani 1 1 d . . . H12A H 0.7869 0.8634 1.0469 0.034 Uiso 1 1 calc R . . H12B H 0.6744 0.8131 0.9630 0.034 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 Sr1 0.0180(5) 0.0198(5) 0.0183(5) -0.0008(4) 0.0086(4) 0.0005(4) I1 0.0233(4) 0.0284(4) 0.0287(4) 0.0019(3) 0.0101(3) 0.0031(3) I2 0.0278(4) 0.0237(4) 0.0329(4) 0.0035(3) 0.0008(3) -0.0030(3) S1 0.0302(15) 0.0244(13) 0.0218(13) -0.0012(10) 0.0101(12) 0.0000(12) S2 0.0336(17) 0.0477(18) 0.0231(14) 0.0043(12) 0.0071(13) 0.0146(15) O1 0.031(4) 0.025(4) 0.019(4) -0.003(3) 0.010(3) -0.001(3) O2 0.018(4) 0.033(4) 0.024(4) -0.006(3) 0.002(3) -0.001(3) O3 0.029(4) 0.025(4) 0.024(4) -0.001(3) 0.014(3) -0.003(3) O4 0.020(4) 0.019(4) 0.026(4) 0.003(3) 0.009(3) -0.001(3) O5 0.033(5) 0.028(4) 0.027(4) -0.004(3) 0.014(4) -0.002(4) O6 0.028(4) 0.029(4) 0.032(4) -0.002(3) 0.015(4) 0.000(3) O7 0.024(4) 0.027(4) 0.034(4) -0.005(3) 0.011(4) -0.001(3) O8 0.037(5) 0.035(4) 0.048(5) 0.006(4) 0.029(4) 0.003(4) C1 0.028(6) 0.032(6) 0.014(5) 0.004(4) 0.009(5) -0.002(5) C2 0.037(7) 0.025(6) 0.022(5) 0.000(4) 0.015(5) -0.004(5) C3 0.025(6) 0.037(6) 0.041(7) 0.001(5) 0.014(6) -0.001(5) C4 0.018(5) 0.027(6) 0.033(6) -0.009(5) 0.005(5) -0.003(5) C5 0.030(7) 0.119(13) 0.036(7) 0.016(8) 0.005(6) -0.015(9) C6 0.034(8) 0.146(15) 0.030(7) -0.005(8) 0.011(6) -0.048(10) C7 0.027(6) 0.036(6) 0.024(5) 0.009(5) 0.011(5) 0.001(5) C8 0.041(7) 0.039(6) 0.018(5) 0.000(5) 0.013(5) 0.003(6) C9 0.034(7) 0.023(5) 0.029(6) 0.000(4) 0.021(5) -0.003(5) C10 0.021(6) 0.034(6) 0.043(7) 0.006(5) 0.018(5) -0.004(5) C11 0.019(6) 0.033(6) 0.021(5) -0.003(4) 0.000(5) 0.006(5) C12 0.021(6) 0.025(6) 0.036(6) 0.005(5) 0.009(5) 0.013(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 Sr1 O6 2.546(7) . ? Sr1 O5 2.592(7) . ? Sr1 O7 2.587(7) . ? Sr1 O4 2.685(7) . ? Sr1 O1 2.691(6) . ? Sr1 O2 2.707(7) . ? Sr1 O3 2.750(6) . ? Sr1 S1 3.095(3) . ? Sr1 S2 3.111(3) . ? S1 C1 1.831(9) . ? S1 C12 1.844(10) . ? S2 C6 1.820(14) . ? S2 C7 1.829(10) . ? O1 C3 1.432(13) . ? O1 C2 1.464(12) . ? O2 C4 1.419(12) . ? O2 C5 1.433(14) . ? O3 C8 1.439(12) . ? O3 C9 1.466(12) . ? O4 C10 1.436(11) . ? O4 C11 1.454(11) . ? C1 C2 1.467(14) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.468(15) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.526(16) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.477(15) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.476(15) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.485(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? 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 O6 Sr1 O5 75.8(2) . . ? O6 Sr1 O7 138.2(2) . . ? O5 Sr1 O7 145.8(2) . . ? O6 Sr1 O4 142.8(2) . . ? O5 Sr1 O4 77.1(2) . . ? O7 Sr1 O4 73.2(2) . . ? O6 Sr1 O1 72.6(2) . . ? O5 Sr1 O1 131.5(2) . . ? O7 Sr1 O1 75.0(2) . . ? O4 Sr1 O1 108.6(2) . . ? O6 Sr1 O2 74.0(2) . . ? O5 Sr1 O2 139.2(2) . . ? O7 Sr1 O2 67.7(2) . . ? O4 Sr1 O2 140.9(2) . . ? O1 Sr1 O2 62.2(2) . . ? O6 Sr1 O3 132.2(2) . . ? O5 Sr1 O3 75.31(19) . . ? O7 Sr1 O3 76.2(2) . . ? O4 Sr1 O3 62.3(2) . . ? O1 Sr1 O3 151.2(2) . . ? O2 Sr1 O3 106.2(2) . . ? O6 Sr1 S1 85.71(17) . . ? O5 Sr1 S1 77.19(16) . . ? O7 Sr1 S1 103.64(17) . . ? O4 Sr1 S1 63.64(14) . . ? O1 Sr1 S1 64.67(16) . . ? O2 Sr1 S1 126.63(15) . . ? O3 Sr1 S1 123.19(16) . . ? O6 Sr1 S2 74.59(16) . . ? O5 Sr1 S2 80.18(17) . . ? O7 Sr1 S2 103.34(17) . . ? O4 Sr1 S2 124.80(14) . . ? O1 Sr1 S2 123.91(17) . . ? O2 Sr1 S2 65.67(16) . . ? O3 Sr1 S2 63.52(16) . . ? S1 Sr1 S2 153.01(8) . . ? C1 S1 C12 100.6(5) . . ? C1 S1 Sr1 101.2(3) . . ? C12 S1 Sr1 97.8(4) . . ? C6 S2 C7 99.3(6) . . ? C6 S2 Sr1 96.0(5) . . ? C7 S2 Sr1 102.9(4) . . ? C3 O1 C2 111.5(7) . . ? C3 O1 Sr1 114.7(5) . . ? C2 O1 Sr1 117.3(5) . . ? C4 O2 C5 108.2(8) . . ? C4 O2 Sr1 115.0(6) . . ? C5 O2 Sr1 124.0(7) . . ? C8 O3 C9 112.6(7) . . ? C8 O3 Sr1 118.5(6) . . ? C9 O3 Sr1 111.2(5) . . ? C10 O4 C11 110.6(8) . . ? C10 O4 Sr1 117.9(6) . . ? C11 O4 Sr1 126.5(5) . . ? C2 C1 S1 113.5(6) . . ? C2 C1 H1A 108.9 . . ? S1 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? S1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? O1 C2 C1 109.0(8) . . ? O1 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O1 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O1 C3 C4 109.4(9) . . ? O1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? O1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? O2 C4 C3 110.3(8) . . ? O2 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? O2 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? O2 C5 C6 109.3(11) . . ? O2 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? O2 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? C5 C6 S2 112.0(10) . . ? C5 C6 H6A 109.2 . . ? S2 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? S2 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C8 C7 S2 113.7(7) . . ? C8 C7 H7A 108.8 . . ? S2 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? S2 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? O3 C8 C7 110.2(8) . . ? O3 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? O3 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 O3 108.7(8) . . ? C10 C9 H9A 109.9 . . ? O3 C9 H9A 109.9 . . ? C10 C9 H9B 109.9 . . ? O3 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? O4 C10 C9 110.5(8) . . ? O4 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? O4 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? O4 C11 C12 109.9(9) . . ? O4 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? O4 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C11 C12 S1 108.2(7) . . ? C11 C12 H12A 110.1 . . ? S1 C12 H12A 110.1 . . ? C11 C12 H12B 110.1 . . ? S1 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 S1 C1 C2 -71.0(9) . . . . ? Sr1 S1 C1 C2 29.2(8) . . . . ? C3 O1 C2 C1 -157.8(8) . . . . ? Sr1 O1 C2 C1 67.0(8) . . . . ? S1 C1 C2 O1 -61.9(10) . . . . ? C2 O1 C3 C4 176.2(8) . . . . ? Sr1 O1 C3 C4 -47.4(9) . . . . ? C5 O2 C4 C3 172.3(10) . . . . ? Sr1 O2 C4 C3 -44.3(9) . . . . ? O1 C3 C4 O2 60.9(10) . . . . ? C4 O2 C5 C6 -179.4(11) . . . . ? Sr1 O2 C5 C6 41.4(16) . . . . ? O2 C5 C6 S2 -66.7(16) . . . . ? C7 S2 C6 C5 157.4(11) . . . . ? Sr1 S2 C6 C5 53.3(12) . . . . ? C6 S2 C7 C8 -71.6(10) . . . . ? Sr1 S2 C7 C8 26.8(9) . . . . ? C9 O3 C8 C7 -162.8(8) . . . . ? Sr1 O3 C8 C7 65.0(9) . . . . ? S2 C7 C8 O3 -58.7(11) . . . . ? C8 O3 C9 C10 170.8(8) . . . . ? Sr1 O3 C9 C10 -53.5(8) . . . . ? C11 O4 C10 C9 165.9(8) . . . . ? Sr1 O4 C10 C9 -37.5(10) . . . . ? O3 C9 C10 O4 60.6(10) . . . . ? C10 O4 C11 C12 -167.5(8) . . . . ? Sr1 O4 C11 C12 38.4(10) . . . . ? O4 C11 C12 S1 -64.5(9) . . . . ? C1 S1 C12 C11 158.7(7) . . . . ? Sr1 S1 C12 C11 55.7(8) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O5 I1 3.600(8) . . ? O5 I2 3.514(7) . . ? O6 O8 2.768(9) . . ? O6 I2 3.582(7) . . ? O7 I1 3.684(7) . 2_646 ? O7 I2 3.470(7) . 2_646 ? O8 I1 3.623(7) . 1_455 ? O8 I1 3.668(7) . 3_677 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.283 _refine_diff_density_min -1.116 _refine_diff_density_rms 0.235 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE =============================================================