# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Franco Benetollo' _publ_contact_author_address ; ICIS - C.N.R. Corso Stati Uniti 4 35127 Padova Italy ; _publ_contact_author_email benetollo@icis.cnr.it _publ_contact_author_phone '++39 049 8295930' _publ_contact_author_fax '++39 049 8705951' _publ_contact_letter ; Please consider this CIF submission as revised version numbers: 755292-755294 before publication in the Dalton Transactions. ; _publ_section_title ; Synthesis and characterization of calcium \b-dichetonate complexes. X-ray crystal and molecular structures of: [(Ca(tmhd)~2~)~2~(18-crown-6)], [Ca(dpp)~2~(thf)~2~] and [Ca(dpp)~2~(triglyme)]. ; loop_ _publ_author_name 'Naida El Habra ' 'Franco Benetollo' 'Maurizio Casarin' 'Marco Bolzan' 'Andrea Sartori' 'Gilberto Rossetto' #The chemical, crystallographic and experimental data data_new-crown1 _database_code_depnum_ccdc_archive 'CCDC 755292' #TrackingRef 'EL_HABRA_C001854F.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(Ca(tmhd)~2~)~2~(18-crown-6)]' _chemical_formula_sum 'C56 H100 Ca2 O14' _chemical_formula_weight 1077.52 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.558(2) _cell_length_b 10.574(2) _cell_length_c 15.776(3) _cell_angle_alpha 72.84(3) _cell_angle_beta 80.19(3) _cell_angle_gamma 72.33(3) _cell_volume 1597.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 0.234 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6855 _exptl_absorpt_correction_T_max 0.9099 _exptl_absorpt_process_details 'A. T. C. North, et al. Acta Crystallogr., A24 (1968) 351' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' Philips PW1100 ' _diffrn_measurement_method \Q/2\Q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7307 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 26.98 _reflns_number_total 6931 _reflns_number_gt 6301 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al. 1999)' _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. Restraints of the distance c25-c261 due to the disordered of the (terminal) methyl of the ligand 2,2,6,6-tetramethyl-3,5-heptanedione. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+0.8482P] 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 6931 _refine_ls_number_parameters 369 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.178 _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 Ca Ca 0.48384(4) -0.67583(3) -0.35034(2) 0.03676(11) Uani 1 1 d . . . O1 O 0.38060(13) -0.41670(13) -0.42294(9) 0.0462(3) Uani 1 1 d . . . O2 O 0.25370(14) -0.61605(15) -0.40333(10) 0.0523(3) Uani 1 1 d . . . O3 O 0.46555(14) -0.77693(15) -0.47820(9) 0.0500(3) Uani 1 1 d . . . O4 O 0.68793(14) -0.83403(14) -0.37020(10) 0.0498(3) Uani 1 1 d . . . O5 O 0.65009(13) -0.59170(13) -0.32052(9) 0.0467(3) Uani 1 1 d . . . O6 O 0.41801(17) -0.85988(14) -0.25916(10) 0.0570(4) Uani 1 1 d . . . O7 O 0.36710(16) -0.59864(14) -0.23073(9) 0.0526(4) Uani 1 1 d . . . C1 C 0.2398(2) -0.3829(2) -0.42842(16) 0.0571(5) Uani 1 1 d . . . H1A H 0.2092 -0.2913 -0.4669 0.068 Uiso 1 1 calc R . . H1B H 0.1928 -0.3848 -0.3698 0.068 Uiso 1 1 calc R . . C2 C 0.2127(2) -0.4856(2) -0.46503(15) 0.0585(5) Uani 1 1 d . . . H2A H 0.1183 -0.4632 -0.4722 0.070 Uiso 1 1 calc R . . H2B H 0.2622 -0.4865 -0.5227 0.070 Uiso 1 1 calc R . . C3 C 0.2376(3) -0.7286(3) -0.42917(18) 0.0668(6) Uani 1 1 d . . . H3A H 0.1487 -0.7052 -0.4479 0.080 Uiso 1 1 calc R . . H3B H 0.2469 -0.8084 -0.3784 0.080 Uiso 1 1 calc R . . C4 C 0.3383(3) -0.7628(3) -0.50331(18) 0.0685(7) Uani 1 1 d . . . H4A H 0.3353 -0.8478 -0.5136 0.082 Uiso 1 1 calc R . . H4B H 0.3199 -0.6902 -0.5577 0.082 Uiso 1 1 calc R . . C5 C 0.5709(2) -0.8046(2) -0.54548(13) 0.0509(5) Uani 1 1 d . . . H5A H 0.5537 -0.8665 -0.5741 0.061 Uiso 1 1 calc R . . H5B H 0.6541 -0.8501 -0.5181 0.061 Uiso 1 1 calc R . . C6 C 0.5849(2) -0.6752(2) -0.61481(13) 0.0517(5) Uani 1 1 d . . . H6A H 0.6534 -0.6992 -0.6612 0.062 Uiso 1 1 calc R . . H6B H 0.5014 -0.6291 -0.6418 0.062 Uiso 1 1 calc R . . C7 C 0.78699(19) -0.8738(2) -0.32635(13) 0.0452(4) Uani 1 1 d . . . C8 C 0.8232(2) -0.7928(2) -0.28401(17) 0.0635(6) Uani 1 1 d . . . H8 H 0.9001 -0.8324 -0.2541 0.078(8) Uiso 1 1 calc R . . C9 C 0.75498(19) -0.6586(2) -0.28253(12) 0.0422(4) Uani 1 1 d . . . C10 C 0.8123(2) -0.5838(2) -0.23377(14) 0.0492(5) Uani 1 1 d . . . C11 C 0.9338(4) -0.5477(5) -0.2908(3) 0.1209(16) Uani 1 1 d . . . H11A H 0.9630 -0.4886 -0.2669 0.145 Uiso 1 1 calc R . . H11B H 0.9111 -0.5014 -0.3506 0.145 Uiso 1 1 calc R . . H11C H 1.0043 -0.6303 -0.2909 0.145 Uiso 1 1 calc R . . C12 C 0.7124(3) -0.4497(3) -0.2237(2) 0.0773(8) Uani 1 1 d . . . H12A H 0.6317 -0.4683 -0.1912 0.093 Uiso 1 1 calc R . . H12B H 0.6930 -0.3896 -0.2815 0.093 Uiso 1 1 calc R . . H12C H 0.7495 -0.4066 -0.1919 0.093 Uiso 1 1 calc R . . C13 C 0.8484(5) -0.6726(3) -0.1424(2) 0.1204(16) Uani 1 1 d . . . H13A H 0.9207 -0.7516 -0.1481 0.145 Uiso 1 1 calc R . . H13B H 0.7725 -0.7021 -0.1097 0.145 Uiso 1 1 calc R . . H13C H 0.8751 -0.6208 -0.1112 0.145 Uiso 1 1 calc R . . C14 C 0.8750(2) -1.0224(2) -0.31853(18) 0.0620(6) Uani 1 1 d . . . C15 C 1.0182(3) -1.0207(4) -0.3547(3) 0.1206(15) Uani 1 1 d . . . H15A H 1.0530 -0.9797 -0.3202 0.145 Uiso 1 1 calc R . . H15B H 1.0196 -0.9683 -0.4158 0.145 Uiso 1 1 calc R . . H15C H 1.0721 -1.1132 -0.3507 0.145 Uiso 1 1 calc R . . C16 C 0.8231(3) -1.0911(3) -0.3719(2) 0.0913(10) Uani 1 1 d . . . H16A H 0.8779 -1.1836 -0.3663 0.110 Uiso 1 1 calc R . . H16B H 0.8257 -1.0408 -0.4335 0.110 Uiso 1 1 calc R . . H16C H 0.7329 -1.0925 -0.3499 0.110 Uiso 1 1 calc R . . C17 C 0.8721(5) -1.1022(3) -0.2211(2) 0.1166(14) Uani 1 1 d . . . H17A H 0.7818 -1.1022 -0.1983 0.140 Uiso 1 1 calc R . . H17B H 0.9070 -1.0597 -0.1877 0.140 Uiso 1 1 calc R . . H17C H 0.9255 -1.1951 -0.2158 0.140 Uiso 1 1 calc R . . C18 C 0.3599(2) -0.88543(19) -0.18243(14) 0.0478(4) Uani 1 1 d . A . C19 C 0.3095(2) -0.7913(2) -0.13086(14) 0.0537(5) Uani 1 1 d . . . H19 H 0.2686 -0.8218 -0.0746 0.064 Uiso 1 1 calc R . . C20 C 0.31561(19) -0.65437(19) -0.15688(12) 0.0425(4) Uani 1 1 d . . . C21 C 0.2579(2) -0.5611(2) -0.09255(13) 0.0453(4) Uani 1 1 d . . . C22 C 0.1589(3) -0.4320(3) -0.14030(17) 0.0673(6) Uani 1 1 d . . . H22A H 0.0855 -0.4563 -0.1537 0.081 Uiso 1 1 calc R . . H22B H 0.2024 -0.3881 -0.1946 0.081 Uiso 1 1 calc R . . H22C H 0.1264 -0.3701 -0.1027 0.081 Uiso 1 1 calc R . . C23 C 0.3728(3) -0.5202(3) -0.07153(19) 0.0723(7) Uani 1 1 d . . . H23A H 0.3392 -0.4584 -0.0339 0.087 Uiso 1 1 calc R . . H23B H 0.4156 -0.4756 -0.1259 0.087 Uiso 1 1 calc R . . H23C H 0.4361 -0.6008 -0.0415 0.087 Uiso 1 1 calc R . . C24 C 0.1876(3) -0.6283(3) -0.00574(16) 0.0703(7) Uani 1 1 d . . . H24A H 0.1515 -0.5635 0.0296 0.084 Uiso 1 1 calc R . . H24B H 0.2505 -0.7069 0.0266 0.084 Uiso 1 1 calc R . . H24C H 0.1167 -0.6569 -0.0189 0.084 Uiso 1 1 calc R . . C25 C 0.3455(3) -1.0335(2) -0.14426(17) 0.0627(6) Uani 1 1 d D . . C27 C 0.1987(6) -1.0306(6) -0.1079(6) 0.118(2) Uani 0.70 1 d P A 1 H27A H 0.1403 -0.9724 -0.1527 0.142 Uiso 0.70 1 calc PR A 1 H27B H 0.1766 -0.9957 -0.0560 0.142 Uiso 0.70 1 calc PR A 1 H27C H 0.1884 -1.1221 -0.0924 0.142 Uiso 0.70 1 calc PR A 1 C26 C 0.4296(11) -1.1060(6) -0.0711(8) 0.176(5) Uani 0.70 1 d P A 1 H26A H 0.4141 -1.1947 -0.0442 0.211 Uiso 0.70 1 calc PR A 1 H26B H 0.4086 -1.0540 -0.0276 0.211 Uiso 0.70 1 calc PR A 1 H26C H 0.5217 -1.1172 -0.0935 0.211 Uiso 0.70 1 calc PR A 1 C28 C 0.3738(10) -1.1070(6) -0.2184(4) 0.123(3) Uani 0.70 1 d P A 1 H28A H 0.3594 -1.1967 -0.1944 0.148 Uiso 0.70 1 calc PR A 1 H28B H 0.4647 -1.1157 -0.2431 0.148 Uiso 0.70 1 calc PR A 1 H28C H 0.3151 -1.0547 -0.2642 0.148 Uiso 0.70 1 calc PR A 1 C261 C 0.4831(11) -1.1291(9) -0.1613(12) 0.111(5) Uani 0.30 1 d PD A 2 H26D H 0.4786 -1.2227 -0.1415 0.133 Uiso 0.30 1 calc PR A 2 H26E H 0.5463 -1.1170 -0.1292 0.133 Uiso 0.30 1 calc PR A 2 H26F H 0.5109 -1.1074 -0.2238 0.133 Uiso 0.30 1 calc PR A 2 C271 C 0.308(3) -1.0726(14) -0.0466(9) 0.131(7) Uani 0.30 1 d P A 2 H27D H 0.2220 -1.0141 -0.0330 0.157 Uiso 0.30 1 calc PR A 2 H27E H 0.3731 -1.0623 -0.0154 0.157 Uiso 0.30 1 calc PR A 2 H27F H 0.3041 -1.1665 -0.0284 0.157 Uiso 0.30 1 calc PR A 2 C281 C 0.2544(18) -1.0485(13) -0.1961(13) 0.116(5) Uani 0.30 1 d P A 2 H28D H 0.2442 -1.1402 -0.1754 0.139 Uiso 0.30 1 calc PR A 2 H28E H 0.2887 -1.0317 -0.2576 0.139 Uiso 0.30 1 calc PR A 2 H28F H 0.1693 -0.9837 -0.1899 0.139 Uiso 0.30 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.0423(2) 0.03326(18) 0.03553(18) -0.00904(13) -0.00695(14) -0.00926(14) O1 0.0481(7) 0.0391(7) 0.0496(7) -0.0118(6) -0.0093(6) -0.0060(6) O2 0.0511(8) 0.0574(8) 0.0487(8) -0.0081(6) -0.0098(6) -0.0179(7) O3 0.0576(8) 0.0555(8) 0.0436(7) -0.0152(6) -0.0126(6) -0.0182(7) O4 0.0494(8) 0.0469(7) 0.0570(8) -0.0221(6) -0.0205(6) -0.0015(6) O5 0.0493(7) 0.0408(7) 0.0542(8) -0.0149(6) -0.0174(6) -0.0085(6) O6 0.0863(11) 0.0383(7) 0.0467(8) -0.0120(6) 0.0054(7) -0.0223(7) O7 0.0746(10) 0.0391(7) 0.0426(7) -0.0133(6) 0.0091(7) -0.0185(7) C1 0.0449(11) 0.0519(12) 0.0604(13) -0.0061(10) -0.0046(9) -0.0012(9) C2 0.0474(11) 0.0714(15) 0.0508(12) -0.0009(10) -0.0130(9) -0.0173(10) C3 0.0618(14) 0.0753(16) 0.0752(16) -0.0149(13) -0.0149(12) -0.0354(12) C4 0.0708(15) 0.0785(17) 0.0738(16) -0.0318(13) -0.0226(13) -0.0249(13) C5 0.0712(13) 0.0369(9) 0.0432(10) -0.0145(8) -0.0122(9) -0.0045(9) C6 0.0704(13) 0.0426(10) 0.0400(10) -0.0132(8) -0.0110(9) -0.0066(9) C7 0.0462(10) 0.0412(10) 0.0484(10) -0.0135(8) -0.0123(8) -0.0057(8) C8 0.0631(13) 0.0530(12) 0.0820(16) -0.0271(11) -0.0410(12) 0.0018(10) C9 0.0449(10) 0.0460(10) 0.0404(9) -0.0126(8) -0.0092(7) -0.0149(8) C10 0.0525(11) 0.0567(12) 0.0484(11) -0.0210(9) -0.0115(9) -0.0180(9) C11 0.097(2) 0.190(4) 0.139(3) -0.104(3) 0.037(2) -0.096(3) C12 0.0871(19) 0.0703(16) 0.093(2) -0.0429(15) -0.0236(15) -0.0185(14) C13 0.218(5) 0.076(2) 0.079(2) -0.0189(16) -0.082(3) -0.021(2) C14 0.0612(13) 0.0444(11) 0.0818(16) -0.0236(11) -0.0281(12) 0.0024(10) C15 0.0642(18) 0.110(3) 0.204(5) -0.097(3) -0.006(2) 0.0040(18) C16 0.104(2) 0.0516(14) 0.130(3) -0.0416(16) -0.051(2) 0.0026(14) C17 0.167(4) 0.0586(18) 0.104(3) 0.0010(17) -0.056(3) 0.002(2) C18 0.0585(12) 0.0359(9) 0.0473(10) -0.0037(8) -0.0089(9) -0.0147(8) C19 0.0713(14) 0.0438(10) 0.0431(10) -0.0080(8) 0.0050(9) -0.0200(10) C20 0.0463(10) 0.0419(10) 0.0387(9) -0.0113(7) -0.0023(7) -0.0110(8) C21 0.0497(10) 0.0464(10) 0.0403(9) -0.0153(8) -0.0012(8) -0.0110(8) C22 0.0711(15) 0.0601(14) 0.0605(14) -0.0216(11) -0.0058(11) 0.0027(12) C23 0.0664(15) 0.0894(19) 0.0783(17) -0.0438(15) -0.0054(13) -0.0247(14) C24 0.0885(18) 0.0715(16) 0.0504(13) -0.0238(12) 0.0159(12) -0.0250(14) C25 0.0867(17) 0.0377(10) 0.0635(14) -0.0039(9) -0.0063(12) -0.0254(11) C27 0.111(4) 0.079(3) 0.173(7) -0.035(4) 0.022(4) -0.055(3) C26 0.227(9) 0.067(4) 0.232(11) 0.066(6) -0.169(9) -0.057(6) C28 0.217(8) 0.059(3) 0.108(4) -0.034(3) 0.026(5) -0.067(4) C261 0.114(9) 0.037(5) 0.129(11) 0.019(6) 0.011(9) 0.003(5) C271 0.24(2) 0.057(7) 0.088(8) 0.014(6) 0.021(12) -0.075(12) C281 0.139(12) 0.064(7) 0.162(15) -0.002(8) -0.051(11) -0.058(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca O6 2.2734(16) . ? Ca O7 2.2917(15) . ? Ca O4 2.3304(16) . ? Ca O5 2.3601(14) . ? Ca O2 2.5398(16) . ? Ca O1 2.6016(16) . ? Ca O3 2.6038(15) . ? O1 C1 1.431(2) . ? O1 C6 1.436(2) 2_644 ? O2 C2 1.424(3) . ? O2 C3 1.429(3) . ? O3 C4 1.418(3) . ? O3 C5 1.426(3) . ? O4 C7 1.248(2) . ? O5 C9 1.260(2) . ? O6 C18 1.253(2) . ? O7 C20 1.254(2) . ? C1 C2 1.487(3) . ? C3 C4 1.490(4) . ? C5 C6 1.508(3) . ? C6 O1 1.436(2) 2_644 ? C7 C8 1.396(3) . ? C7 C14 1.544(3) . ? C8 C9 1.388(3) . ? C9 C10 1.546(2) . ? C10 C13 1.509(4) . ? C10 C11 1.518(4) . ? C10 C12 1.522(3) . ? C14 C16 1.517(3) . ? C14 C17 1.520(4) . ? C14 C15 1.525(4) . ? C18 C19 1.395(3) . ? C18 C25 1.547(3) . ? C19 C20 1.402(3) . ? C20 C21 1.545(3) . ? C21 C23 1.520(3) . ? C21 C22 1.523(3) . ? C21 C24 1.526(3) . ? C25 C281 1.434(13) . ? C25 C26 1.456(6) . ? C25 C271 1.490(13) . ? C25 C261 1.529(7) . ? C25 C28 1.528(6) . ? C25 C27 1.553(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ca O7 75.83(6) . . ? O6 Ca O4 85.43(6) . . ? O7 Ca O4 133.87(6) . . ? O6 Ca O5 124.22(6) . . ? O7 Ca O5 83.35(6) . . ? O4 Ca O5 73.07(5) . . ? O6 Ca O2 81.94(6) . . ? O7 Ca O2 83.69(6) . . ? O4 Ca O2 135.30(5) . . ? O5 Ca O2 146.39(5) . . ? O6 Ca O1 139.06(6) . . ? O7 Ca O1 77.77(6) . . ? O4 Ca O1 134.88(6) . . ? O5 Ca O1 82.51(5) . . ? O2 Ca O1 64.47(5) . . ? O6 Ca O3 84.68(5) . . ? O7 Ca O3 143.69(6) . . ? O4 Ca O3 73.07(5) . . ? O5 Ca O3 132.57(5) . . ? O2 Ca O3 63.20(5) . . ? O1 Ca O3 99.11(5) . . ? C1 O1 C6 111.78(16) . 2_644 ? C1 O1 Ca 113.09(12) . . ? C6 O1 Ca 114.28(11) 2_644 . ? C2 O2 C3 114.75(18) . . ? C2 O2 Ca 115.91(12) . . ? C3 O2 Ca 110.24(13) . . ? C4 O3 C5 113.10(17) . . ? C4 O3 Ca 119.85(13) . . ? C5 O3 Ca 123.63(12) . . ? C7 O4 Ca 129.00(13) . . ? C9 O5 Ca 128.38(12) . . ? C18 O6 Ca 134.88(13) . . ? C20 O7 Ca 134.26(12) . . ? O1 C1 C2 108.16(18) . . ? O2 C2 C1 107.10(17) . . ? O2 C3 C4 111.38(19) . . ? O3 C4 C3 107.51(19) . . ? O3 C5 C6 112.02(16) . . ? O1 C6 C5 111.70(16) 2_644 . ? O4 C7 C8 124.28(18) . . ? O4 C7 C14 117.72(17) . . ? C8 C7 C14 118.00(18) . . ? C9 C8 C7 125.94(19) . . ? O5 C9 C8 124.07(17) . . ? O5 C9 C10 117.30(17) . . ? C8 C9 C10 118.60(17) . . ? C13 C10 C11 110.9(3) . . ? C13 C10 C12 108.5(2) . . ? C11 C10 C12 107.3(3) . . ? C13 C10 C9 111.1(2) . . ? C11 C10 C9 107.78(19) . . ? C12 C10 C9 111.20(18) . . ? C16 C14 C17 109.7(3) . . ? C16 C14 C15 108.7(3) . . ? C17 C14 C15 109.6(3) . . ? C16 C14 C7 110.07(19) . . ? C17 C14 C7 109.0(2) . . ? C15 C14 C7 109.8(2) . . ? O6 C18 C19 124.76(18) . . ? O6 C18 C25 115.93(19) . . ? C19 C18 C25 119.32(19) . . ? C18 C19 C20 125.40(19) . . ? O7 C20 C19 124.53(18) . . ? O7 C20 C21 115.23(16) . . ? C19 C20 C21 120.23(17) . . ? C23 C21 C22 108.6(2) . . ? C23 C21 C24 109.3(2) . . ? C22 C21 C24 108.8(2) . . ? C23 C21 C20 107.54(17) . . ? C22 C21 C20 108.35(17) . . ? C24 C21 C20 114.17(17) . . ? C281 C25 C26 143.4(6) . . ? C281 C25 C271 113.2(11) . . ? C26 C25 C271 50.2(8) . . ? C281 C25 C261 108.5(11) . . ? C26 C25 C261 60.2(7) . . ? C271 C25 C261 106.9(10) . . ? C281 C25 C28 50.4(8) . . ? C26 C25 C28 113.4(6) . . ? C271 C25 C28 134.5(6) . . ? C261 C25 C28 59.0(8) . . ? C281 C25 C18 106.7(5) . . ? C26 C25 C18 109.9(3) . . ? C271 C25 C18 115.1(5) . . ? C261 C25 C18 106.1(5) . . ? C28 C25 C18 110.4(3) . . ? C281 C25 C27 58.3(8) . . ? C26 C25 C27 108.2(6) . . ? C271 C25 C27 59.4(9) . . ? C261 C25 C27 143.5(5) . . ? C28 C25 C27 104.5(5) . . ? C18 C25 C27 110.3(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.98 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.259 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.045 #=== END data_ca-thf _database_code_depnum_ccdc_archive 'CCDC 755293' #TrackingRef 'EL_HABRA_C001854F.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ca(dpp)~2~(thf)~2~]' _chemical_formula_sum 'C38 H38 Ca O6' _chemical_formula_weight 630.76 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.939(2) _cell_length_b 15.574(3) _cell_length_c 10.861(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.10(3) _cell_angle_gamma 90.00 _cell_volume 1630.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.239 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.5138 _exptl_absorpt_correction_T_max 0.8466 _exptl_absorpt_process_details 'A. T. C. North, et al. Acta Crystallogr., A24 (1968) 351' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' Philips PW1100 ' _diffrn_measurement_method \Q/2\Q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3733 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3546 _reflns_number_gt 2002 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al. 1999)' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^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 3546 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _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 Ca Ca 0.0000 0.0000 0.0000 0.0479(2) Uani 1 2 d S . . O2 O 0.07346(17) -0.13967(10) 0.02867(16) 0.0571(4) Uani 1 1 d . . . O1 O -0.17659(16) -0.06515(10) 0.06057(16) 0.0583(4) Uani 1 1 d . . . O3 O -0.11899(19) -0.02205(12) -0.21499(17) 0.0737(5) Uani 1 1 d . . . C1 C -0.1806(2) -0.13419(15) 0.1208(2) 0.0493(6) Uani 1 1 d . . . C2 C -0.0807(3) -0.19802(15) 0.1394(2) 0.0518(6) Uani 1 1 d . . . H2 H -0.0958 -0.2459 0.1855 0.062 Uiso 1 1 calc R . . C3 C 0.0408(2) -0.19810(14) 0.0961(2) 0.0466(5) Uani 1 1 d . . . C4 C 0.1395(2) -0.27130(13) 0.1297(2) 0.0444(5) Uani 1 1 d . . . C5 C 0.1482(2) -0.32220(15) 0.2355(2) 0.0543(6) Uani 1 1 d . . . H5 H 0.0867 -0.3133 0.2866 0.065 Uiso 1 1 calc R . . C6 C 0.2467(3) -0.38580(17) 0.2663(2) 0.0666(7) Uani 1 1 d . . . H6 H 0.2509 -0.4195 0.3378 0.080 Uiso 1 1 calc R . . C7 C 0.3376(3) -0.39991(18) 0.1934(3) 0.0704(8) Uani 1 1 d . . . H7 H 0.4045 -0.4427 0.2153 0.084 Uiso 1 1 calc R . . C8 C 0.3304(3) -0.35048(17) 0.0871(3) 0.0661(7) Uani 1 1 d . . . H8 H 0.3914 -0.3603 0.0360 0.079 Uiso 1 1 calc R . . C9 C 0.2328(2) -0.28658(15) 0.0565(2) 0.0550(6) Uani 1 1 d . . . H9 H 0.2294 -0.2529 -0.0149 0.066 Uiso 1 1 calc R . . C10 C -0.3058(3) -0.14590(15) 0.1729(2) 0.0525(6) Uani 1 1 d . . . C11 C -0.4284(3) -0.10932(18) 0.1095(3) 0.0659(7) Uani 1 1 d . . . H11 H -0.4325 -0.0779 0.0358 0.079 Uiso 1 1 calc R . . C12 C -0.5462(3) -0.1189(2) 0.1546(3) 0.0841(9) Uani 1 1 d . . . H12 H -0.6295 -0.0944 0.1109 0.101 Uiso 1 1 calc R . . C13 C -0.5403(4) -0.1648(2) 0.2638(4) 0.0916(11) Uani 1 1 d . . . H13 H -0.6195 -0.1716 0.2940 0.110 Uiso 1 1 calc R . . C14 C -0.4191(3) -0.1999(2) 0.3273(3) 0.0825(9) Uani 1 1 d . . . H14 H -0.4151 -0.2304 0.4017 0.099 Uiso 1 1 calc R . . C15 C -0.3012(3) -0.19123(18) 0.2830(3) 0.0665(7) Uani 1 1 d . . . H15 H -0.2184 -0.2160 0.3274 0.080 Uiso 1 1 calc R . . C16 C -0.0876(3) 0.0120(2) -0.3265(3) 0.0828(9) Uani 1 1 d . . . H16A H 0.0119 0.0124 -0.3181 0.099 Uiso 1 1 calc R . . H16B H -0.1222 0.0702 -0.3419 0.099 Uiso 1 1 calc R . . C17 C -0.1578(4) -0.0457(2) -0.4320(3) 0.0898(10) Uani 1 1 d . . . H17A H -0.1002 -0.0947 -0.4397 0.108 Uiso 1 1 calc R . . H17B H -0.1822 -0.0153 -0.5124 0.108 Uiso 1 1 calc R . . C18 C -0.2849(4) -0.0726(2) -0.3900(3) 0.1027(11) Uani 1 1 d . . . H18A H -0.3606 -0.0327 -0.4209 0.123 Uiso 1 1 calc R . . H18B H -0.3144 -0.1296 -0.4210 0.123 Uiso 1 1 calc R . . C19 C -0.2415(3) -0.0715(2) -0.2493(3) 0.0953(11) Uani 1 1 d . . . H19A H -0.3136 -0.0462 -0.2146 0.114 Uiso 1 1 calc R . . H19B H -0.2242 -0.1295 -0.2166 0.114 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 Ca 0.0489(4) 0.0440(4) 0.0536(4) 0.0100(3) 0.0175(3) -0.0013(3) O2 0.0635(10) 0.0465(9) 0.0714(11) 0.0151(8) 0.0357(9) 0.0065(8) O1 0.0538(10) 0.0515(10) 0.0764(12) 0.0110(9) 0.0288(9) -0.0012(8) O3 0.0774(12) 0.0788(13) 0.0587(11) 0.0036(10) 0.0046(9) -0.0145(10) C1 0.0516(14) 0.0456(13) 0.0542(14) -0.0054(11) 0.0199(11) -0.0106(11) C2 0.0608(15) 0.0408(13) 0.0614(15) 0.0065(12) 0.0294(12) -0.0049(12) C3 0.0565(14) 0.0392(13) 0.0467(13) -0.0025(10) 0.0176(11) -0.0063(10) C4 0.0507(13) 0.0385(12) 0.0442(13) -0.0033(10) 0.0117(11) -0.0063(10) C5 0.0587(14) 0.0539(14) 0.0501(14) 0.0047(12) 0.0128(12) -0.0064(12) C6 0.0731(18) 0.0640(17) 0.0595(17) 0.0203(14) 0.0099(14) -0.0008(14) C7 0.0709(18) 0.0576(16) 0.0764(19) 0.0089(15) 0.0059(16) 0.0136(14) C8 0.0717(17) 0.0651(17) 0.0649(17) 0.0014(14) 0.0233(14) 0.0161(14) C9 0.0683(15) 0.0502(14) 0.0494(14) 0.0050(11) 0.0201(12) 0.0076(12) C10 0.0561(15) 0.0469(13) 0.0613(15) -0.0135(12) 0.0275(13) -0.0140(12) C11 0.0589(16) 0.0676(18) 0.0771(18) -0.0103(15) 0.0280(14) -0.0097(14) C12 0.0539(17) 0.104(2) 0.099(2) -0.035(2) 0.0276(17) -0.0147(16) C13 0.074(2) 0.119(3) 0.100(3) -0.050(2) 0.056(2) -0.043(2) C14 0.095(2) 0.094(2) 0.074(2) -0.0223(17) 0.0496(19) -0.037(2) C15 0.0733(17) 0.0675(17) 0.0674(17) -0.0083(14) 0.0340(14) -0.0163(14) C16 0.095(2) 0.085(2) 0.0602(18) 0.0135(16) 0.0029(16) -0.0087(18) C17 0.099(2) 0.098(2) 0.064(2) -0.0004(18) 0.0028(18) 0.016(2) C18 0.086(2) 0.116(3) 0.094(3) -0.019(2) -0.003(2) -0.008(2) C19 0.085(2) 0.102(3) 0.099(3) -0.036(2) 0.024(2) -0.0242(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca O1 2.2595(15) 3 ? Ca O1 2.2595(15) . ? Ca O2 2.2915(16) . ? Ca O2 2.2915(16) 3 ? Ca O3 2.3714(19) 3 ? Ca O3 2.3714(19) . ? Ca C1 3.234(2) . ? Ca C1 3.234(2) 3 ? O2 C3 1.259(2) . ? O1 C1 1.264(3) . ? O3 C19 1.412(3) . ? O3 C16 1.425(3) . ? C1 C2 1.384(3) . ? C1 C10 1.498(3) . ? C2 C3 1.399(3) . ? C2 H2 0.91(2) . ? C3 C4 1.490(3) . ? C4 C9 1.381(3) . ? C4 C5 1.381(3) . ? C5 C6 1.375(3) . ? C5 H5 0.9300 . ? C6 C7 1.357(4) . ? C6 H6 0.9300 . ? C7 C8 1.375(4) . ? C7 H7 0.9300 . ? C8 C9 1.373(3) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.370(4) . ? C10 C15 1.380(3) . ? C11 C12 1.383(3) . ? C11 H11 0.9300 . ? C12 C13 1.374(5) . ? C12 H12 0.9300 . ? C13 C14 1.349(4) . ? C13 H13 0.9300 . ? C14 C15 1.377(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.490(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.503(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.484(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? 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 Ca O1 180 3 . ? O1 Ca O2 102.79(6) 3 . ? O1 Ca O2 77.21(6) . . ? O1 Ca O2 77.21(6) 3 3 ? O1 Ca O2 102.79(6) . 3 ? O2 Ca O2 180 3 . ? O1 Ca O3 89.15(7) 3 3 ? O1 Ca O3 90.85(7) . 3 ? O2 Ca O3 86.43(6) . 3 ? O2 Ca O3 93.57(6) 3 3 ? O1 Ca O3 90.85(7) 3 . ? O1 Ca O3 89.15(7) . . ? O2 Ca O3 93.57(6) . . ? O2 Ca O3 86.43(6) 3 . ? O3 Ca O3 180 3 . ? O1 Ca C1 162.86(6) 3 . ? O1 Ca C1 17.14(6) . . ? O2 Ca C1 61.40(6) . . ? O2 Ca C1 118.60(6) 3 . ? O3 Ca C1 83.52(6) 3 . ? O3 Ca C1 96.48(6) . . ? O1 Ca C1 17.14(6) 3 3 ? O1 Ca C1 162.86(6) . 3 ? O2 Ca C1 118.60(6) . 3 ? O2 Ca C1 61.40(6) 3 3 ? O3 Ca C1 96.48(6) 3 3 ? O3 Ca C1 83.52(6) . 3 ? C1 Ca C1 180.00(6) . 3 ? C3 O2 Ca 130.27(14) . . ? C1 O1 Ca 131.07(15) . . ? C19 O3 C16 109.4(2) . . ? C19 O3 Ca 121.98(18) . . ? C16 O3 Ca 128.55(16) . . ? O1 C1 C2 125.1(2) . . ? O1 C1 C10 115.6(2) . . ? C2 C1 C10 119.3(2) . . ? O1 C1 Ca 31.79(10) . . ? C2 C1 Ca 94.26(14) . . ? C10 C1 Ca 145.68(16) . . ? C1 C2 C3 126.8(2) . . ? C1 C2 H2 118.9(13) . . ? C3 C2 H2 114.3(14) . . ? O2 C3 C2 124.1(2) . . ? O2 C3 C4 116.61(19) . . ? C2 C3 C4 119.3(2) . . ? C9 C4 C5 117.7(2) . . ? C9 C4 C3 119.01(19) . . ? C5 C4 C3 123.2(2) . . ? C6 C5 C4 120.8(2) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C7 C6 C5 120.7(2) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 119.5(3) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 119.9(2) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C4 121.3(2) . . ? C8 C9 H9 119.3 . . ? C4 C9 H9 119.3 . . ? C11 C10 C15 119.1(2) . . ? C11 C10 C1 118.6(2) . . ? C15 C10 C1 122.3(2) . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 120.0(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 119.8(3) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 120.8(3) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C10 120.1(3) . . ? C14 C15 H15 119.9 . . ? C10 C15 H15 119.9 . . ? O3 C16 C17 105.7(2) . . ? O3 C16 H16A 110.6 . . ? C17 C16 H16A 110.6 . . ? O3 C16 H16B 110.6 . . ? C17 C16 H16B 110.6 . . ? H16A C16 H16B 108.7 . . ? C16 C17 C18 101.9(3) . . ? C16 C17 H17A 111.4 . . ? C18 C17 H17A 111.4 . . ? C16 C17 H17B 111.4 . . ? C18 C17 H17B 111.4 . . ? H17A C17 H17B 109.3 . . ? C19 C18 C17 104.8(3) . . ? C19 C18 H18A 110.8 . . ? C17 C18 H18A 110.8 . . ? C19 C18 H18B 110.8 . . ? C17 C18 H18B 110.8 . . ? H18A C18 H18B 108.9 . . ? O3 C19 C18 107.0(3) . . ? O3 C19 H19A 110.3 . . ? C18 C19 H19A 110.3 . . ? O3 C19 H19B 110.3 . . ? C18 C19 H19B 110.3 . . ? H19A C19 H19B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.155 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.043 #=== END data_ca-triglyme _database_code_depnum_ccdc_archive 'CCDC 755294' #TrackingRef 'EL_HABRA_C001854F.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ca(dpp)~2~(triglyme)]^.^0.25CH~2~Cl~2~' _chemical_formula_sum 'C38.25 H40.50 Ca Cl0.50 O8' _chemical_formula_weight 686.01 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' 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.321(3) _cell_length_b 26.791(3) _cell_length_c 12.451(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.06(3) _cell_angle_gamma 90.00 _cell_volume 3835.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1450 _exptl_absorpt_coefficient_mu 0.246 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4268 _exptl_absorpt_correction_T_max 0.8083 _exptl_absorpt_process_details 'A. T. C. North, et al. Acta Crystallogr., A24 (1968) 351' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' Philips PW1100 ' _diffrn_measurement_method \Q/2\Q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7043 _diffrn_reflns_av_R_equivalents 0.0136 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6716 _reflns_number_gt 3286 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al. 1999' _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. Restraint of the distances C-Cl due to the disordered of the dichloromethane solvent about an inversion centre with occupancy factors of 0.25. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1786P)^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 6716 _refine_ls_number_parameters 438 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1423 _refine_ls_R_factor_gt 0.0889 _refine_ls_wR_factor_ref 0.2052 _refine_ls_wR_factor_gt 0.1946 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 Ca Ca 0.91436(9) 0.13334(4) 0.56620(10) 0.0582(4) Uani 1 1 d . . . O1 O 1.0963(3) 0.10004(15) 0.6798(3) 0.0709(11) Uani 1 1 d . . . O2 O 1.0250(3) 0.12436(16) 0.4465(3) 0.0708(11) Uani 1 1 d . . . O3 O 0.8857(3) 0.11193(16) 0.7418(3) 0.0724(11) Uani 1 1 d . . . O7 O 0.7685(4) 0.12184(18) 0.3562(4) 0.0851(13) Uani 1 1 d . . . O5 O 1.0254(5) 0.20992(19) 0.6544(6) 0.1155(19) Uani 1 1 d . . . O6 O 0.8727(6) 0.21143(19) 0.4361(5) 0.1084(17) Uani 1 1 d . . . O4 O 0.7443(4) 0.17348(17) 0.5666(4) 0.0815(13) Uani 1 1 d . . . O8 O 0.8316(4) 0.05012(16) 0.5178(4) 0.0839(13) Uani 1 1 d . . . C1 C 1.1953(5) 0.10293(19) 0.6742(5) 0.0553(14) Uani 1 1 d . . . C2 C 1.2196(5) 0.1160(2) 0.5762(5) 0.0613(15) Uani 1 1 d . . . H2 H 1.2970 0.1191 0.5833 0.074 Uiso 1 1 calc R . . C3 C 1.1330(5) 0.12485(19) 0.4672(5) 0.0576(14) Uani 1 1 d . . . C4 C 1.1708(5) 0.13275(19) 0.3657(5) 0.0587(14) Uani 1 1 d . . . C5 C 1.2730(5) 0.1556(2) 0.3744(6) 0.0747(17) Uani 1 1 d . . . H5 H 1.3229 0.1671 0.4454 0.090 Uiso 1 1 calc R . . C6 C 1.3024(7) 0.1617(3) 0.2782(7) 0.091(2) Uani 1 1 d . . . H6 H 1.3708 0.1781 0.2841 0.110 Uiso 1 1 calc R . . C7 C 1.2308(8) 0.1437(3) 0.1743(7) 0.100(3) Uani 1 1 d . . . H7 H 1.2515 0.1476 0.1099 0.120 Uiso 1 1 calc R . . C8 C 1.1290(7) 0.1200(3) 0.1638(6) 0.0840(19) Uani 1 1 d . . . H8 H 1.0805 0.1076 0.0930 0.101 Uiso 1 1 calc R . . C9 C 1.1004(6) 0.1150(2) 0.2590(5) 0.0739(17) Uani 1 1 d . . . H9 H 1.0312 0.0991 0.2522 0.089 Uiso 1 1 calc R . . C10 C 1.2949(5) 0.0888(2) 0.7827(5) 0.0616(15) Uani 1 1 d . . . C11 C 1.4074(5) 0.0803(3) 0.7853(6) 0.0835(19) Uani 1 1 d . . . H11 H 1.4237 0.0837 0.7183 0.100 Uiso 1 1 calc R . . C12 C 1.4959(6) 0.0667(3) 0.8880(7) 0.098(2) Uani 1 1 d . . . H12 H 1.5698 0.0602 0.8873 0.117 Uiso 1 1 calc R . . C13 C 1.4776(7) 0.0628(3) 0.9866(6) 0.088(2) Uani 1 1 d . . . H13 H 1.5387 0.0550 1.0543 0.106 Uiso 1 1 calc R . . C14 C 1.3662(8) 0.0705(3) 0.9874(6) 0.098(2) Uani 1 1 d . . . H14 H 1.3512 0.0665 1.0550 0.117 Uiso 1 1 calc R . . C15 C 1.2760(6) 0.0845(2) 0.8841(6) 0.0777(18) Uani 1 1 d . . . H15 H 1.2023 0.0910 0.8852 0.093 Uiso 1 1 calc R . . C16 C 0.8151(5) 0.1237(2) 0.7874(5) 0.0597(14) Uani 1 1 d . . . C17 C 0.7224(5) 0.1569(2) 0.7421(5) 0.0650(15) Uani 1 1 d . . . H17 H 0.6775 0.1642 0.7863 0.078 Uiso 1 1 calc R . . C18 C 0.6936(5) 0.1793(2) 0.6371(5) 0.0632(15) Uani 1 1 d . . . C19 C 0.5883(5) 0.2158(2) 0.5967(5) 0.0637(15) Uani 1 1 d . . . C20 C 0.5832(7) 0.2504(2) 0.5119(6) 0.0852(19) Uani 1 1 d . . . H20 H 0.6416 0.2508 0.4811 0.102 Uiso 1 1 calc R . . C21 C 0.4939(8) 0.2839(3) 0.4729(7) 0.111(3) Uani 1 1 d . . . H21 H 0.4904 0.3061 0.4144 0.133 Uiso 1 1 calc R . . C22 C 0.4114(8) 0.2845(3) 0.5197(8) 0.117(3) Uani 1 1 d . . . H22 H 0.3527 0.3084 0.4964 0.141 Uiso 1 1 calc R . . C23 C 0.4135(6) 0.2499(3) 0.6024(7) 0.101(3) Uani 1 1 d . . . H23 H 0.3539 0.2493 0.6317 0.122 Uiso 1 1 calc R . . C24 C 0.5032(5) 0.2163(2) 0.6415(6) 0.0776(18) Uani 1 1 d . . . H24 H 0.5056 0.1938 0.6991 0.093 Uiso 1 1 calc R . . C25 C 0.8256(5) 0.0958(2) 0.8970(5) 0.0620(15) Uani 1 1 d . . . C26 C 0.8609(6) 0.0472(3) 0.9103(5) 0.0785(18) Uani 1 1 d . . . H26 H 0.8856 0.0328 0.8551 0.094 Uiso 1 1 calc R . . C27 C 0.8612(7) 0.0186(3) 1.0035(6) 0.090(2) Uani 1 1 d . . . H27 H 0.8783 -0.0153 1.0063 0.108 Uiso 1 1 calc R . . C28 C 0.8365(6) 0.0401(4) 1.0899(6) 0.097(2) Uani 1 1 d . . . H28 H 0.8432 0.0218 1.1554 0.116 Uiso 1 1 calc R . . C29 C 0.8011(6) 0.0899(3) 1.0812(6) 0.085(2) Uani 1 1 d . . . H29 H 0.7813 0.1047 1.1394 0.102 Uiso 1 1 calc R . . C30 C 0.7957(5) 0.1171(3) 0.9848(6) 0.0810(19) Uani 1 1 d . . . H30 H 0.7716 0.1502 0.9784 0.097 Uiso 1 1 calc R . . C31 C 1.1052(10) 0.2131(4) 0.7645(10) 0.155(4) Uani 1 1 d . . . H31A H 1.1820 0.2156 0.7621 0.186 Uiso 1 1 calc R . . H31B H 1.1002 0.1838 0.8069 0.186 Uiso 1 1 calc R . . H31C H 1.0892 0.2422 0.8015 0.186 Uiso 1 1 calc R . . C32 C 1.0057(11) 0.2554(4) 0.5953(13) 0.161(5) Uani 1 1 d . . . H32A H 1.0785 0.2736 0.6160 0.193 Uiso 1 1 calc R . . H32B H 0.9521 0.2753 0.6185 0.193 Uiso 1 1 calc R . . C33 C 0.9584(11) 0.2485(4) 0.4720(15) 0.181(6) Uani 1 1 d . . . H33A H 0.9253 0.2798 0.4360 0.218 Uiso 1 1 calc R . . H33B H 1.0211 0.2398 0.4457 0.218 Uiso 1 1 calc R . . C34 C 0.8214(9) 0.2024(3) 0.3161(8) 0.116(3) Uani 1 1 d . . . H34A H 0.8767 0.1867 0.2875 0.139 Uiso 1 1 calc R . . H34B H 0.7944 0.2333 0.2744 0.139 Uiso 1 1 calc R . . C35 C 0.7213(8) 0.1680(4) 0.3036(6) 0.119(3) Uani 1 1 d . . . H35A H 0.6717 0.1823 0.3410 0.143 Uiso 1 1 calc R . . H35B H 0.6753 0.1630 0.2229 0.143 Uiso 1 1 calc R . . C36 C 0.6874(7) 0.0862(4) 0.3539(7) 0.112(3) Uani 1 1 d . . . H36A H 0.6356 0.0803 0.2754 0.134 Uiso 1 1 calc R . . H36B H 0.6412 0.0975 0.3981 0.134 Uiso 1 1 calc R . . C37 C 0.7523(8) 0.0379(3) 0.4062(7) 0.103(3) Uani 1 1 d . . . H37A H 0.6978 0.0127 0.4111 0.124 Uiso 1 1 calc R . . H37B H 0.7937 0.0251 0.3589 0.124 Uiso 1 1 calc R . . C38 C 0.8856(8) 0.0076(3) 0.5842(8) 0.115(3) Uani 1 1 d . . . H38A H 0.8273 -0.0135 0.5948 0.138 Uiso 1 1 calc R . . H38B H 0.9389 0.0183 0.6579 0.138 Uiso 1 1 calc R . . H38C H 0.9271 -0.0106 0.5448 0.138 Uiso 1 1 calc R . . C39 C 0.4883(12) 0.0478(5) 0.4947(12) 0.037(3) Uiso 0.25 1 d PD . . Cl1 Cl 0.397(2) 0.0261(11) 0.3551(15) 0.184(10) Uiso 0.25 1 d PD . . Cl2 Cl 0.5841(19) 0.0170(9) 0.6163(16) 0.174(10) Uiso 0.25 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.0506(7) 0.0580(7) 0.0706(8) 0.0037(6) 0.0271(6) 0.0050(5) O1 0.055(2) 0.088(3) 0.077(3) 0.015(2) 0.031(2) 0.006(2) O2 0.047(2) 0.095(3) 0.074(3) 0.009(2) 0.026(2) 0.004(2) O3 0.061(2) 0.087(3) 0.075(3) 0.008(2) 0.032(2) 0.015(2) O7 0.070(3) 0.102(4) 0.079(3) 0.005(3) 0.021(2) 0.011(3) O5 0.098(4) 0.071(3) 0.155(5) -0.006(3) 0.019(4) -0.014(3) O6 0.147(5) 0.076(3) 0.110(4) 0.025(3) 0.056(4) 0.015(3) O4 0.072(3) 0.099(3) 0.084(3) 0.019(2) 0.041(2) 0.031(2) O8 0.103(3) 0.073(3) 0.081(3) -0.006(2) 0.041(3) -0.018(3) C1 0.050(3) 0.051(3) 0.066(4) -0.001(3) 0.023(3) 0.002(2) C2 0.052(3) 0.071(4) 0.067(4) 0.006(3) 0.030(3) 0.003(3) C3 0.061(4) 0.051(3) 0.066(4) -0.002(3) 0.029(3) 0.001(3) C4 0.066(4) 0.048(3) 0.066(4) 0.006(3) 0.029(3) 0.011(3) C5 0.069(4) 0.078(4) 0.085(4) 0.006(3) 0.036(3) -0.014(3) C6 0.094(5) 0.099(5) 0.095(6) 0.017(5) 0.051(5) -0.004(4) C7 0.141(8) 0.095(6) 0.090(6) 0.019(4) 0.074(6) 0.028(5) C8 0.105(6) 0.088(5) 0.071(4) 0.003(4) 0.045(4) 0.004(4) C9 0.079(4) 0.071(4) 0.071(4) 0.003(3) 0.025(4) 0.000(3) C10 0.064(4) 0.054(3) 0.063(4) 0.002(3) 0.020(3) -0.002(3) C11 0.061(4) 0.111(5) 0.074(4) 0.000(4) 0.020(3) 0.009(4) C12 0.073(5) 0.113(6) 0.089(6) 0.002(5) 0.006(4) 0.012(4) C13 0.079(5) 0.100(6) 0.074(5) 0.002(4) 0.015(4) 0.017(4) C14 0.131(7) 0.098(6) 0.056(4) 0.010(4) 0.023(4) 0.006(5) C15 0.078(4) 0.089(5) 0.074(4) 0.006(4) 0.036(4) 0.010(4) C16 0.052(3) 0.070(4) 0.064(4) -0.013(3) 0.029(3) -0.002(3) C17 0.064(4) 0.066(4) 0.071(4) -0.004(3) 0.031(3) 0.009(3) C18 0.054(3) 0.059(3) 0.077(4) -0.012(3) 0.024(3) -0.001(3) C19 0.052(3) 0.063(4) 0.072(4) -0.014(3) 0.017(3) 0.009(3) C20 0.098(5) 0.070(4) 0.086(5) 0.006(4) 0.031(4) 0.020(4) C21 0.126(7) 0.109(6) 0.106(6) 0.016(5) 0.050(6) 0.060(5) C22 0.124(7) 0.107(7) 0.100(6) -0.006(5) 0.014(6) 0.059(6) C23 0.075(5) 0.125(7) 0.098(5) -0.019(5) 0.024(4) 0.043(5) C24 0.073(4) 0.072(4) 0.088(5) -0.008(3) 0.029(4) 0.011(3) C25 0.049(3) 0.080(4) 0.058(3) -0.009(3) 0.020(3) 0.004(3) C26 0.082(4) 0.091(5) 0.069(4) -0.001(4) 0.035(4) 0.016(4) C27 0.101(5) 0.100(5) 0.079(5) 0.018(4) 0.045(4) 0.015(4) C28 0.072(4) 0.138(8) 0.079(5) 0.029(5) 0.026(4) 0.000(5) C29 0.071(4) 0.126(7) 0.062(4) -0.007(4) 0.029(3) -0.007(4) C30 0.066(4) 0.096(5) 0.077(5) -0.007(4) 0.021(3) -0.001(4) C31 0.163(10) 0.126(8) 0.151(9) -0.054(7) 0.025(8) -0.029(7) C32 0.156(10) 0.081(7) 0.219(13) 0.003(9) 0.034(10) -0.014(6) C33 0.157(11) 0.089(7) 0.277(17) 0.076(10) 0.052(11) -0.010(7) C34 0.146(8) 0.101(6) 0.116(8) 0.046(5) 0.063(6) 0.037(6) C35 0.118(7) 0.161(9) 0.073(5) 0.026(5) 0.028(5) 0.073(7) C36 0.079(5) 0.162(9) 0.088(5) -0.006(6) 0.023(4) -0.038(6) C37 0.112(6) 0.108(6) 0.113(6) -0.033(5) 0.067(5) -0.042(5) C38 0.149(8) 0.057(4) 0.177(9) 0.011(5) 0.103(7) 0.008(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 Ca O1 2.354(4) . ? Ca O4 2.357(4) . ? Ca O2 2.367(4) . ? Ca O3 2.406(4) . ? Ca O8 2.436(4) . ? Ca O5 2.492(5) . ? Ca O6 2.582(5) . ? Ca O7 2.605(5) . ? O1 C1 1.249(6) . ? O2 C3 1.260(6) . ? O3 C16 1.238(6) . ? O7 C36 1.375(8) . ? O7 C35 1.423(9) . ? O5 C31 1.373(10) . ? O5 C32 1.399(11) . ? O6 C33 1.400(12) . ? O6 C34 1.418(10) . ? O4 C18 1.256(7) . ? O8 C37 1.420(9) . ? O8 C38 1.424(8) . ? C1 C2 1.402(7) . ? C1 C10 1.511(8) . ? C2 C3 1.413(8) . ? C3 C4 1.511(8) . ? C4 C5 1.370(8) . ? C4 C9 1.384(8) . ? C5 C6 1.380(9) . ? C6 C7 1.365(10) . ? C7 C8 1.369(10) . ? C8 C9 1.360(9) . ? C10 C15 1.369(8) . ? C10 C11 1.393(8) . ? C11 C12 1.398(9) . ? C12 C13 1.329(10) . ? C13 C14 1.392(10) . ? C14 C15 1.415(10) . ? C16 C17 1.396(8) . ? C16 C25 1.521(8) . ? C17 C18 1.365(8) . ? C18 C19 1.557(8) . ? C19 C24 1.353(8) . ? C19 C20 1.389(8) . ? C20 C21 1.367(9) . ? C21 C22 1.342(11) . ? C22 C23 1.380(11) . ? C23 C24 1.370(9) . ? C25 C26 1.362(9) . ? C25 C30 1.394(8) . ? C26 C27 1.391(9) . ? C27 C28 1.347(10) . ? C28 C29 1.396(10) . ? C29 C30 1.385(9) . ? C32 C33 1.444(15) . ? C34 C35 1.501(12) . ? C36 C37 1.538(12) . ? C39 Cl2 1.757(10) . ? C39 Cl1 1.794(10) . ? C39 Cl2 2.20(3) 3_656 ? Cl1 Cl2 1.21(3) 3_656 ? Cl2 Cl1 1.21(3) 3_656 ? Cl2 C39 2.20(3) 3_656 ? 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 Ca O4 145.79(15) . . ? O1 Ca O2 72.55(13) . . ? O4 Ca O2 139.62(15) . . ? O1 Ca O3 77.46(14) . . ? O4 Ca O3 71.68(14) . . ? O2 Ca O3 148.67(15) . . ? O1 Ca O8 91.46(16) . . ? O4 Ca O8 97.15(17) . . ? O2 Ca O8 92.06(15) . . ? O3 Ca O8 79.71(15) . . ? O1 Ca O5 78.10(17) . . ? O4 Ca O5 88.34(18) . . ? O2 Ca O5 90.69(19) . . ? O3 Ca O5 91.86(19) . . ? O8 Ca O5 167.9(2) . . ? O1 Ca O6 128.00(18) . . ? O4 Ca O6 69.82(17) . . ? O2 Ca O6 73.56(17) . . ? O3 Ca O6 134.60(17) . . ? O8 Ca O6 128.0(2) . . ? O5 Ca O6 64.1(2) . . ? O1 Ca O7 136.27(15) . . ? O4 Ca O7 76.30(15) . . ? O2 Ca O7 72.62(14) . . ? O3 Ca O7 127.63(15) . . ? O8 Ca O7 64.33(16) . . ? O5 Ca O7 127.7(2) . . ? O6 Ca O7 63.65(19) . . ? C1 O1 Ca 133.0(4) . . ? C3 O2 Ca 132.4(4) . . ? C16 O3 Ca 135.4(4) . . ? C36 O7 C35 114.8(7) . . ? C36 O7 Ca 109.7(4) . . ? C35 O7 Ca 112.3(5) . . ? C31 O5 C32 113.4(8) . . ? C31 O5 Ca 125.1(6) . . ? C32 O5 Ca 121.4(6) . . ? C33 O6 C34 117.2(9) . . ? C33 O6 Ca 114.6(6) . . ? C34 O6 Ca 115.8(5) . . ? C18 O4 Ca 136.4(4) . . ? C37 O8 C38 113.5(6) . . ? C37 O8 Ca 122.2(4) . . ? C38 O8 Ca 121.4(5) . . ? O1 C1 C2 125.6(5) . . ? O1 C1 C10 115.6(5) . . ? C2 C1 C10 118.8(5) . . ? C1 C2 C3 123.7(5) . . ? O2 C3 C2 124.9(5) . . ? O2 C3 C4 116.7(5) . . ? C2 C3 C4 118.3(5) . . ? C5 C4 C9 118.0(6) . . ? C5 C4 C3 123.3(5) . . ? C9 C4 C3 118.7(5) . . ? C4 C5 C6 120.4(6) . . ? C7 C6 C5 119.9(7) . . ? C6 C7 C8 120.8(7) . . ? C9 C8 C7 118.5(7) . . ? C8 C9 C4 122.3(6) . . ? C15 C10 C11 117.5(6) . . ? C15 C10 C1 119.5(5) . . ? C11 C10 C1 122.9(5) . . ? C10 C11 C12 120.4(7) . . ? C13 C12 C11 122.0(7) . . ? C12 C13 C14 119.3(7) . . ? C13 C14 C15 119.1(7) . . ? C10 C15 C14 121.5(7) . . ? O3 C16 C17 125.8(6) . . ? O3 C16 C25 116.0(5) . . ? C17 C16 C25 118.0(5) . . ? C18 C17 C16 124.1(5) . . ? O4 C18 C17 126.2(5) . . ? O4 C18 C19 114.7(5) . . ? C17 C18 C19 119.1(5) . . ? C24 C19 C20 118.4(6) . . ? C24 C19 C18 123.5(6) . . ? C20 C19 C18 118.0(6) . . ? C21 C20 C19 121.3(7) . . ? C22 C21 C20 119.5(8) . . ? C21 C22 C23 120.1(7) . . ? C24 C23 C22 120.1(8) . . ? C19 C24 C23 120.4(7) . . ? C26 C25 C30 117.3(6) . . ? C26 C25 C16 119.9(5) . . ? C30 C25 C16 122.7(6) . . ? C25 C26 C27 122.2(6) . . ? C28 C27 C26 119.7(7) . . ? C27 C28 C29 120.1(7) . . ? C30 C29 C28 119.0(7) . . ? C29 C30 C25 121.4(7) . . ? O5 C32 C33 112.0(9) . . ? O6 C33 C32 113.6(11) . . ? O6 C34 C35 104.6(7) . . ? O7 C35 C34 107.5(6) . . ? O7 C36 C37 108.2(6) . . ? O8 C37 C36 106.9(6) . . ? Cl2 C39 Cl1 132.6(14) . . ? Cl2 C39 Cl2 99.5(12) . 3_656 ? Cl1 C39 Cl2 33.3(9) . 3_656 ? Cl2 Cl1 C39 92.1(18) 3_656 . ? Cl1 Cl2 C39 135(2) 3_656 . ? Cl1 Cl2 C39 54.6(13) 3_656 3_656 ? C39 Cl2 C39 80.5(11) . 3_656 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.018 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.080