# Electronic Supplementary Material (ESI) for Chemical Communications # 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_Ca-BTC-DMA _database_code_depnum_ccdc_archive 'CCDC 885042' #TrackingRef 'Ca-BTC-DMA.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ca-BTC-DMA _chemical_melting_point ? _chemical_formula_moiety 'C26 H28 Ca3 N2 O16' _chemical_formula_sum 'C26 H28 Ca3 N2 O16' _chemical_formula_weight 744.74 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' Ca Ca 0.2262 0.3064 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 16.552(7) _cell_length_b 10.961(5) _cell_length_c 18.691(11) _cell_angle_alpha 90.00 _cell_angle_beta 111.514(7) _cell_angle_gamma 90.00 _cell_volume 3155(3) _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 Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 0.602 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17703 _diffrn_reflns_av_R_equivalents 0.1230 _diffrn_reflns_av_sigmaI/netI 0.0991 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.82 _reflns_number_total 3737 _reflns_number_gt 3207 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^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 3696 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1613 _refine_ls_goodness_of_fit_ref 1.597 _refine_ls_restrained_S_all 1.597 _refine_ls_shift/su_max 0.027 _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 Ca1 Ca 0.0000 0.45626(8) -0.2500 0.0120(2) Uani 1 2 d S . . Ca2 Ca 0.14554(4) 0.59582(6) -0.04872(4) 0.0145(2) Uani 1 1 d . . . O2 O 0.00100(15) 0.6054(2) -0.16148(13) 0.0185(5) Uani 1 1 d . . . O3 O 0.00891(15) 0.6999(2) -0.05503(13) 0.0201(5) Uani 1 1 d . . . O4 O -0.35523(14) 0.9791(2) -0.17152(13) 0.0172(5) Uani 1 1 d . . . O5 O -0.23893(16) 0.9775(2) -0.06533(13) 0.0255(6) Uani 1 1 d . . . O6 O -0.29960(18) 0.8958(2) -0.41576(15) 0.0296(6) Uani 1 1 d . . . O7 O 0.0819(2) 0.4122(2) -0.02966(16) 0.0364(7) Uani 1 1 d . . . H7 H 0.0576 0.3931 -0.0065 0.055 Uiso 1 1 d R . . H7A H 0.0563 0.3788 -0.0727 0.055 Uiso 1 1 d R . . O8 O -0.00366(18) 0.2952(2) -0.17025(15) 0.0296(6) Uani 1 1 d . . . O9 O -0.19381(17) 0.7658(2) -0.40978(14) 0.0262(6) Uani 1 1 d . . . N1 N 0.0587(2) 0.1169(3) -0.1218(2) 0.0352(8) Uani 1 1 d . . . C1 C -0.1354(2) 0.7575(3) -0.25027(18) 0.0152(7) Uani 1 1 d . . . H1 H -0.1047 0.7151 -0.2752 0.018 Uiso 1 1 calc R . . C2 C -0.1086(2) 0.7524(3) -0.17077(18) 0.0152(7) Uani 1 1 d . . . C3 C -0.22814(19) 0.8825(3) -0.17587(18) 0.0132(7) Uani 1 1 d . . . C4 C -0.0283(2) 0.6807(3) -0.12630(19) 0.0159(7) Uani 1 1 d . . . C5 C -0.15404(19) 0.8159(3) -0.13337(17) 0.0126(6) Uani 1 1 d . . . H5 H -0.1352 0.8140 -0.0800 0.015 Uiso 1 1 calc R . . C6 C -0.2767(2) 0.9503(3) -0.13462(19) 0.0153(7) Uani 1 1 d . . . C7 C -0.2359(2) 0.8290(3) -0.37936(19) 0.0184(7) Uani 1 1 d . . . C8 C -0.2548(2) 0.8872(3) -0.25525(19) 0.0155(7) Uani 1 1 d . . . H8 H -0.3041 0.9315 -0.2836 0.019 Uiso 1 1 calc R . . C9 C -0.2081(2) 0.8259(3) -0.29293(18) 0.0155(7) Uani 1 1 d . . . C10 C -0.0092(3) 0.1869(3) -0.1494(2) 0.0321(9) Uani 1 1 d . . . C11 C -0.0954(3) 0.1391(5) -0.1533(5) 0.086(3) Uani 1 1 d . . . H11A H -0.0958 0.1320 -0.1023 0.129 Uiso 1 1 calc R . . H11B H -0.1052 0.0603 -0.1775 0.129 Uiso 1 1 calc R . . H11C H -0.1404 0.1941 -0.1828 0.129 Uiso 1 1 calc R . . C12 C 0.1431(3) 0.1602(4) -0.1173(4) 0.0579(15) Uani 1 1 d . . . H12A H 0.1360 0.2174 -0.1581 0.087 Uiso 1 1 calc R . . H12B H 0.1775 0.0924 -0.1223 0.087 Uiso 1 1 calc R . . H12C H 0.1719 0.1995 -0.0686 0.087 Uiso 1 1 calc R . . C13 C 0.0552(3) -0.0082(4) -0.0936(3) 0.0494(14) Uani 1 1 d . . . H13A H 0.0038 -0.0174 -0.0817 0.074 Uiso 1 1 calc R . . H13B H 0.1055 -0.0226 -0.0481 0.074 Uiso 1 1 calc R . . H13C H 0.0540 -0.0659 -0.1326 0.074 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 0.0097(4) 0.0112(4) 0.0157(5) 0.000 0.0054(3) 0.000 Ca2 0.0133(3) 0.0177(4) 0.0144(3) 0.0013(3) 0.0074(3) 0.0042(2) O2 0.0186(12) 0.0227(13) 0.0166(12) -0.0010(10) 0.0091(10) 0.0086(10) O3 0.0183(12) 0.0251(13) 0.0168(12) -0.0016(10) 0.0065(10) 0.0088(10) O4 0.0089(11) 0.0223(12) 0.0218(12) -0.0018(10) 0.0071(9) 0.0033(9) O5 0.0200(13) 0.0377(15) 0.0180(13) -0.0064(11) 0.0058(10) 0.0118(11) O6 0.0302(15) 0.0377(16) 0.0187(13) 0.0043(11) 0.0062(11) 0.0099(12) O7 0.057(2) 0.0306(15) 0.0263(15) -0.0004(12) 0.0213(14) -0.0153(14) O8 0.0372(16) 0.0167(13) 0.0358(15) 0.0086(11) 0.0143(13) -0.0014(11) O9 0.0375(15) 0.0280(14) 0.0172(12) -0.0049(10) 0.0148(11) 0.0025(11) N1 0.0312(19) 0.0218(17) 0.050(2) 0.0039(15) 0.0122(17) -0.0022(14) C1 0.0168(16) 0.0155(16) 0.0177(16) 0.0009(13) 0.0114(13) 0.0043(12) C2 0.0130(16) 0.0161(16) 0.0185(16) -0.0010(13) 0.0080(13) 0.0014(12) C3 0.0072(14) 0.0166(16) 0.0176(16) 0.0005(12) 0.0065(12) -0.0001(11) C4 0.0154(16) 0.0169(16) 0.0190(16) 0.0015(13) 0.0105(13) 0.0024(13) C5 0.0100(15) 0.0173(16) 0.0122(15) 0.0006(12) 0.0060(12) 0.0009(12) C6 0.0140(16) 0.0143(16) 0.0206(17) 0.0016(13) 0.0100(13) 0.0032(12) C7 0.0225(18) 0.0163(16) 0.0166(16) -0.0007(13) 0.0075(14) -0.0035(13) C8 0.0122(16) 0.0141(16) 0.0203(17) 0.0002(13) 0.0060(13) 0.0015(11) C9 0.0148(16) 0.0158(16) 0.0166(16) 0.0010(13) 0.0066(13) -0.0002(12) C10 0.035(2) 0.0212(19) 0.038(2) 0.0042(17) 0.0102(18) -0.0015(16) C11 0.033(3) 0.037(3) 0.186(8) 0.045(4) 0.038(4) 0.004(2) C12 0.032(3) 0.038(3) 0.107(5) 0.017(3) 0.028(3) 0.003(2) C13 0.038(3) 0.022(2) 0.076(4) 0.016(2) 0.006(2) 0.0034(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 O4 2.319(2) 4_444 ? Ca1 O4 2.319(2) 3_545 ? Ca1 O2 2.321(2) 2_554 ? Ca1 O2 2.321(2) . ? Ca1 O8 2.325(3) . ? Ca1 O8 2.325(3) 2_554 ? Ca1 Ca2 3.9559(18) 2_554 ? Ca1 Ca2 3.9559(18) . ? Ca2 O9 2.273(3) 2_554 ? Ca2 O6 2.314(3) 8_566 ? Ca2 O7 2.358(3) . ? Ca2 O5 2.423(3) 3_545 ? Ca2 O3 2.497(2) . ? Ca2 O2 2.545(3) . ? Ca2 O4 2.624(3) 3_545 ? Ca2 C4 2.862(3) . ? Ca2 C6 2.880(3) 3_545 ? Ca2 C7 3.161(4) 8_566 ? Ca2 H7A 2.7486 . ? O2 C4 1.258(4) . ? O3 C4 1.263(4) . ? O4 C6 1.267(4) . ? O4 Ca1 2.319(2) 3_455 ? O4 Ca2 2.624(3) 3_455 ? O5 C6 1.250(4) . ? O5 Ca2 2.423(3) 3_455 ? O6 C7 1.259(4) . ? O6 Ca2 2.314(3) 8_465 ? O7 H7 0.7227 . ? O7 H7A 0.8436 . ? O8 C10 1.263(4) . ? O9 C7 1.257(4) . ? O9 Ca2 2.273(3) 2_554 ? N1 C10 1.301(5) . ? N1 C12 1.450(5) . ? N1 C13 1.478(5) . ? C1 C2 1.387(5) . ? C1 C9 1.393(4) . ? C1 H1 0.9300 . ? C2 C5 1.387(4) . ? C2 C4 1.504(4) . ? C3 C8 1.385(5) . ? C3 C5 1.398(4) . ? C3 C6 1.499(4) . ? C5 H5 0.9300 . ? C6 Ca2 2.880(3) 3_455 ? C7 C9 1.509(5) . ? C7 Ca2 3.161(4) 8_465 ? C8 C9 1.394(5) . ? C8 H8 0.9300 . ? C10 C11 1.496(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 Ca1 O4 167.62(12) 4_444 3_545 ? O4 Ca1 O2 74.79(8) 4_444 2_554 ? O4 Ca1 O2 96.35(9) 3_545 2_554 ? O4 Ca1 O2 96.35(9) 4_444 . ? O4 Ca1 O2 74.79(8) 3_545 . ? O2 Ca1 O2 90.50(13) 2_554 . ? O4 Ca1 O8 102.92(9) 4_444 . ? O4 Ca1 O8 86.57(9) 3_545 . ? O2 Ca1 O8 175.03(9) 2_554 . ? O2 Ca1 O8 94.16(10) . . ? O4 Ca1 O8 86.57(9) 4_444 2_554 ? O4 Ca1 O8 102.92(9) 3_545 2_554 ? O2 Ca1 O8 94.16(10) 2_554 2_554 ? O2 Ca1 O8 175.03(9) . 2_554 ? O8 Ca1 O8 81.24(14) . 2_554 ? O4 Ca1 Ca2 39.57(6) 4_444 2_554 ? O4 Ca1 Ca2 133.43(6) 3_545 2_554 ? O2 Ca1 Ca2 37.56(6) 2_554 2_554 ? O2 Ca1 Ca2 104.37(7) . 2_554 ? O8 Ca1 Ca2 138.87(7) . 2_554 ? O8 Ca1 Ca2 80.43(7) 2_554 2_554 ? O4 Ca1 Ca2 133.43(6) 4_444 . ? O4 Ca1 Ca2 39.57(6) 3_545 . ? O2 Ca1 Ca2 104.37(7) 2_554 . ? O2 Ca1 Ca2 37.56(6) . . ? O8 Ca1 Ca2 80.44(7) . . ? O8 Ca1 Ca2 138.87(7) 2_554 . ? Ca2 Ca1 Ca2 134.50(4) 2_554 . ? O9 Ca2 O6 106.59(9) 2_554 8_566 ? O9 Ca2 O7 169.57(9) 2_554 . ? O6 Ca2 O7 83.84(10) 8_566 . ? O9 Ca2 O5 90.13(10) 2_554 3_545 ? O6 Ca2 O5 98.13(9) 8_566 3_545 ? O7 Ca2 O5 88.83(10) . 3_545 ? O9 Ca2 O3 92.02(9) 2_554 . ? O6 Ca2 O3 91.41(9) 8_566 . ? O7 Ca2 O3 87.13(10) . . ? O5 Ca2 O3 169.18(8) 3_545 . ? O9 Ca2 O2 91.44(9) 2_554 . ? O6 Ca2 O2 140.11(9) 8_566 . ? O7 Ca2 O2 79.86(9) . . ? O5 Ca2 O2 117.53(8) 3_545 . ? O3 Ca2 O2 51.83(8) . . ? O9 Ca2 O4 89.47(9) 2_554 3_545 ? O6 Ca2 O4 146.40(9) 8_566 3_545 ? O7 Ca2 O4 81.76(9) . 3_545 ? O5 Ca2 O4 51.51(7) 3_545 3_545 ? O3 Ca2 O4 117.89(7) . 3_545 ? O2 Ca2 O4 66.06(8) . 3_545 ? O9 Ca2 C4 88.55(10) 2_554 . ? O6 Ca2 C4 117.20(10) 8_566 . ? O7 Ca2 C4 86.11(10) . . ? O5 Ca2 C4 143.45(9) 3_545 . ? O3 Ca2 C4 26.15(8) . . ? O2 Ca2 C4 26.09(8) . . ? O4 Ca2 C4 91.95(8) 3_545 . ? O9 Ca2 C6 88.80(10) 2_554 3_545 ? O6 Ca2 C6 122.76(10) 8_566 3_545 ? O7 Ca2 C6 85.81(10) . 3_545 ? O5 Ca2 C6 25.45(9) 3_545 3_545 ? O3 Ca2 C6 143.98(9) . 3_545 ? O2 Ca2 C6 92.15(9) . 3_545 ? O4 Ca2 C6 26.10(8) 3_545 3_545 ? C4 Ca2 C6 118.00(10) . 3_545 ? O9 Ca2 C7 87.78(9) 2_554 8_566 ? O6 Ca2 C7 19.81(9) 8_566 8_566 ? O7 Ca2 C7 102.63(10) . 8_566 ? O5 Ca2 C7 92.21(9) 3_545 8_566 ? O3 Ca2 C7 98.46(9) . 8_566 ? O2 Ca2 C7 150.25(8) . 8_566 ? O4 Ca2 C7 143.62(8) 3_545 8_566 ? C4 Ca2 C7 124.21(9) . 8_566 ? C6 Ca2 C7 117.55(10) 3_545 8_566 ? O9 Ca2 Ca1 99.21(7) 2_554 . ? O6 Ca2 Ca1 154.03(7) 8_566 . ? O7 Ca2 Ca1 70.35(7) . . ? O5 Ca2 Ca1 84.55(6) 3_545 . ? O3 Ca2 Ca1 84.64(6) . . ? O2 Ca2 Ca1 33.77(5) . . ? O4 Ca2 Ca1 34.27(5) 3_545 . ? C4 Ca2 Ca1 59.69(7) . . ? C6 Ca2 Ca1 59.76(7) 3_545 . ? C7 Ca2 Ca1 172.28(6) 8_566 . ? O9 Ca2 H7A 152.7 2_554 . ? O6 Ca2 H7A 100.7 8_566 . ? O7 Ca2 H7A 16.9 . . ? O5 Ca2 H7A 85.3 3_545 . ? O3 Ca2 H7A 88.0 . . ? O2 Ca2 H7A 67.3 . . ? O4 Ca2 H7A 66.7 3_545 . ? C4 Ca2 H7A 79.5 . . ? C6 Ca2 H7A 75.7 3_545 . ? C7 Ca2 H7A 119.2 8_566 . ? Ca1 Ca2 H7A 53.6 . . ? C4 O2 Ca1 158.6(2) . . ? C4 O2 Ca2 91.13(19) . . ? Ca1 O2 Ca2 108.67(9) . . ? C4 O3 Ca2 93.27(19) . . ? C6 O4 Ca1 158.8(2) . 3_455 ? C6 O4 Ca2 88.30(19) . 3_455 ? Ca1 O4 Ca2 106.16(8) 3_455 3_455 ? C6 O5 Ca2 98.15(19) . 3_455 ? C7 O6 Ca2 121.6(2) . 8_465 ? Ca2 O7 H7 135.8 . . ? Ca2 O7 H7A 108.8 . . ? H7 O7 H7A 104.5 . . ? C10 O8 Ca1 158.9(3) . . ? C7 O9 Ca2 158.3(2) . 2_554 ? C10 N1 C12 120.2(3) . . ? C10 N1 C13 123.2(4) . . ? C12 N1 C13 116.5(3) . . ? C2 C1 C9 120.3(3) . . ? C2 C1 H1 119.8 . . ? C9 C1 H1 119.8 . . ? C1 C2 C5 120.0(3) . . ? C1 C2 C4 118.9(3) . . ? C5 C2 C4 121.0(3) . . ? C8 C3 C5 119.7(3) . . ? C8 C3 C6 120.8(3) . . ? C5 C3 C6 119.4(3) . . ? O2 C4 O3 121.8(3) . . ? O2 C4 C2 119.0(3) . . ? O3 C4 C2 119.1(3) . . ? O2 C4 Ca2 62.79(17) . . ? O3 C4 Ca2 60.58(16) . . ? C2 C4 Ca2 165.9(2) . . ? C2 C5 C3 120.1(3) . . ? C2 C5 H5 120.0 . . ? C3 C5 H5 120.0 . . ? O5 C6 O4 121.9(3) . . ? O5 C6 C3 119.5(3) . . ? O4 C6 C3 118.7(3) . . ? O5 C6 Ca2 56.40(17) . 3_455 ? O4 C6 Ca2 65.60(17) . 3_455 ? C3 C6 Ca2 174.1(2) . 3_455 ? O9 C7 O6 124.7(3) . . ? O9 C7 C9 118.0(3) . . ? O6 C7 C9 117.3(3) . . ? O9 C7 Ca2 86.2(2) . 8_465 ? O6 C7 Ca2 38.54(16) . 8_465 ? C9 C7 Ca2 155.7(2) . 8_465 ? C3 C8 C9 120.4(3) . . ? C3 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C1 C9 C8 119.5(3) . . ? C1 C9 C7 119.0(3) . . ? C8 C9 C7 121.4(3) . . ? O8 C10 N1 121.8(4) . . ? O8 C10 C11 119.3(4) . . ? N1 C10 C11 118.8(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 H13A 109.5 . . ? N1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? 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 O4 Ca1 Ca2 O9 -89.74(11) 4_444 . . 2_554 ? O4 Ca1 Ca2 O9 75.24(12) 3_545 . . 2_554 ? O2 Ca1 Ca2 O9 -7.23(10) 2_554 . . 2_554 ? O2 Ca1 Ca2 O9 -78.65(13) . . . 2_554 ? O8 Ca1 Ca2 O9 171.48(10) . . . 2_554 ? O8 Ca1 Ca2 O9 106.81(13) 2_554 . . 2_554 ? Ca2 Ca1 Ca2 O9 -33.65(7) 2_554 . . 2_554 ? O4 Ca1 Ca2 O6 83.62(19) 4_444 . . 8_566 ? O4 Ca1 Ca2 O6 -111.40(19) 3_545 . . 8_566 ? O2 Ca1 Ca2 O6 166.12(18) 2_554 . . 8_566 ? O2 Ca1 Ca2 O6 94.7(2) . . . 8_566 ? O8 Ca1 Ca2 O6 -15.16(18) . . . 8_566 ? O8 Ca1 Ca2 O6 -79.8(2) 2_554 . . 8_566 ? Ca2 Ca1 Ca2 O6 139.70(17) 2_554 . . 8_566 ? O4 Ca1 Ca2 O7 90.31(12) 4_444 . . . ? O4 Ca1 Ca2 O7 -104.71(12) 3_545 . . . ? O2 Ca1 Ca2 O7 172.82(10) 2_554 . . . ? O2 Ca1 Ca2 O7 101.40(13) . . . . ? O8 Ca1 Ca2 O7 -8.47(11) . . . . ? O8 Ca1 Ca2 O7 -73.14(14) 2_554 . . . ? Ca2 Ca1 Ca2 O7 146.40(8) 2_554 . . . ? O4 Ca1 Ca2 O5 -178.99(10) 4_444 . . 3_545 ? O4 Ca1 Ca2 O5 -14.01(11) 3_545 . . 3_545 ? O2 Ca1 Ca2 O5 -96.48(9) 2_554 . . 3_545 ? O2 Ca1 Ca2 O5 -167.90(12) . . . 3_545 ? O8 Ca1 Ca2 O5 82.23(10) . . . 3_545 ? O8 Ca1 Ca2 O5 17.56(13) 2_554 . . 3_545 ? Ca2 Ca1 Ca2 O5 -122.90(7) 2_554 . . 3_545 ? O4 Ca1 Ca2 O3 1.45(10) 4_444 . . . ? O4 Ca1 Ca2 O3 166.43(11) 3_545 . . . ? O2 Ca1 Ca2 O3 83.96(9) 2_554 . . . ? O2 Ca1 Ca2 O3 12.53(11) . . . . ? O8 Ca1 Ca2 O3 -97.33(9) . . . . ? O8 Ca1 Ca2 O3 -162.01(12) 2_554 . . . ? Ca2 Ca1 Ca2 O3 57.54(6) 2_554 . . . ? O4 Ca1 Ca2 O2 -11.09(12) 4_444 . . . ? O4 Ca1 Ca2 O2 153.89(14) 3_545 . . . ? O2 Ca1 Ca2 O2 71.42(16) 2_554 . . . ? O8 Ca1 Ca2 O2 -109.87(13) . . . . ? O8 Ca1 Ca2 O2 -174.54(14) 2_554 . . . ? Ca2 Ca1 Ca2 O2 45.00(10) 2_554 . . . ? O4 Ca1 Ca2 O4 -164.98(14) 4_444 . . 3_545 ? O2 Ca1 Ca2 O4 -82.47(11) 2_554 . . 3_545 ? O2 Ca1 Ca2 O4 -153.89(14) . . . 3_545 ? O8 Ca1 Ca2 O4 96.24(12) . . . 3_545 ? O8 Ca1 Ca2 O4 31.56(14) 2_554 . . 3_545 ? Ca2 Ca1 Ca2 O4 -108.89(9) 2_554 . . 3_545 ? O4 Ca1 Ca2 C4 -6.89(11) 4_444 . . . ? O4 Ca1 Ca2 C4 158.09(12) 3_545 . . . ? O2 Ca1 Ca2 C4 75.62(10) 2_554 . . . ? O2 Ca1 Ca2 C4 4.20(13) . . . . ? O8 Ca1 Ca2 C4 -105.67(11) . . . . ? O8 Ca1 Ca2 C4 -170.35(13) 2_554 . . . ? Ca2 Ca1 Ca2 C4 49.20(8) 2_554 . . . ? O4 Ca1 Ca2 C6 -172.89(11) 4_444 . . 3_545 ? O4 Ca1 Ca2 C6 -7.91(12) 3_545 . . 3_545 ? O2 Ca1 Ca2 C6 -90.38(10) 2_554 . . 3_545 ? O2 Ca1 Ca2 C6 -161.80(13) . . . 3_545 ? O8 Ca1 Ca2 C6 88.33(11) . . . 3_545 ? O8 Ca1 Ca2 C6 23.65(13) 2_554 . . 3_545 ? Ca2 Ca1 Ca2 C6 -116.80(8) 2_554 . . 3_545 ? O4 Ca1 Ca2 C7 115.5(5) 4_444 . . 8_566 ? O4 Ca1 Ca2 C7 -79.5(5) 3_545 . . 8_566 ? O2 Ca1 Ca2 C7 -162.0(5) 2_554 . . 8_566 ? O2 Ca1 Ca2 C7 126.6(5) . . . 8_566 ? O8 Ca1 Ca2 C7 16.7(5) . . . 8_566 ? O8 Ca1 Ca2 C7 -48.0(5) 2_554 . . 8_566 ? Ca2 Ca1 Ca2 C7 171.6(5) 2_554 . . 8_566 ? O4 Ca1 O2 C4 15.1(6) 4_444 . . . ? O4 Ca1 O2 C4 -173.7(6) 3_545 . . . ? O2 Ca1 O2 C4 89.9(6) 2_554 . . . ? O8 Ca1 O2 C4 -88.4(6) . . . . ? O8 Ca1 O2 C4 -110.6(11) 2_554 . . . ? Ca2 Ca1 O2 C4 54.6(6) 2_554 . . . ? Ca2 Ca1 O2 C4 -156.8(7) . . . . ? O4 Ca1 O2 Ca2 171.92(9) 4_444 . . . ? O4 Ca1 O2 Ca2 -16.89(9) 3_545 . . . ? O2 Ca1 O2 Ca2 -113.33(12) 2_554 . . . ? O8 Ca1 O2 Ca2 68.41(11) . . . . ? O8 Ca1 O2 Ca2 46.2(11) 2_554 . . . ? Ca2 Ca1 O2 Ca2 -148.62(7) 2_554 . . . ? O9 Ca2 O2 C4 -83.8(2) 2_554 . . . ? O6 Ca2 O2 C4 34.6(2) 8_566 . . . ? O7 Ca2 O2 C4 102.0(2) . . . . ? O5 Ca2 O2 C4 -174.65(19) 3_545 . . . ? O3 Ca2 O2 C4 7.69(18) . . . . ? O4 Ca2 O2 C4 -172.5(2) 3_545 . . . ? C6 Ca2 O2 C4 -172.6(2) 3_545 . . . ? C7 Ca2 O2 C4 4.3(3) 8_566 . . . ? Ca1 Ca2 O2 C4 171.7(2) . . . . ? O9 Ca2 O2 Ca1 104.51(11) 2_554 . . . ? O6 Ca2 O2 Ca1 -137.11(12) 8_566 . . . ? O7 Ca2 O2 Ca1 -69.69(11) . . . . ? O5 Ca2 O2 Ca1 13.61(13) 3_545 . . . ? O3 Ca2 O2 Ca1 -164.05(14) . . . . ? O4 Ca2 O2 Ca1 15.73(8) 3_545 . . . ? C4 Ca2 O2 Ca1 -171.7(2) . . . . ? C6 Ca2 O2 Ca1 15.66(11) 3_545 . . . ? C7 Ca2 O2 Ca1 -167.44(13) 8_566 . . . ? O9 Ca2 O3 C4 82.6(2) 2_554 . . . ? O6 Ca2 O3 C4 -170.8(2) 8_566 . . . ? O7 Ca2 O3 C4 -87.0(2) . . . . ? O5 Ca2 O3 C4 -18.8(6) 3_545 . . . ? O2 Ca2 O3 C4 -7.67(18) . . . . ? O4 Ca2 O3 C4 -7.9(2) 3_545 . . . ? C6 Ca2 O3 C4 -8.2(3) 3_545 . . . ? C7 Ca2 O3 C4 170.63(19) 8_566 . . . ? Ca1 Ca2 O3 C4 -16.50(18) . . . . ? O4 Ca1 O8 C10 75.6(8) 4_444 . . . ? O4 Ca1 O8 C10 -112.4(8) 3_545 . . . ? O2 Ca1 O8 C10 13.7(16) 2_554 . . . ? O2 Ca1 O8 C10 173.1(8) . . . . ? O8 Ca1 O8 C10 -8.8(7) 2_554 . . . ? Ca2 Ca1 O8 C10 55.6(8) 2_554 . . . ? Ca2 Ca1 O8 C10 -151.8(8) . . . . ? C9 C1 C2 C5 -0.2(5) . . . . ? C9 C1 C2 C4 -178.2(3) . . . . ? Ca1 O2 C4 O3 143.9(5) . . . . ? Ca2 O2 C4 O3 -14.2(3) . . . . ? Ca1 O2 C4 C2 -37.8(8) . . . . ? Ca2 O2 C4 C2 164.1(3) . . . . ? Ca1 O2 C4 Ca2 158.1(6) . . . . ? Ca2 O3 C4 O2 14.5(3) . . . . ? Ca2 O3 C4 C2 -163.8(3) . . . . ? C1 C2 C4 O2 -16.1(5) . . . . ? C5 C2 C4 O2 165.8(3) . . . . ? C1 C2 C4 O3 162.2(3) . . . . ? C5 C2 C4 O3 -15.8(5) . . . . ? C1 C2 C4 Ca2 77.5(10) . . . . ? C5 C2 C4 Ca2 -100.5(9) . . . . ? O9 Ca2 C4 O2 96.2(2) 2_554 . . . ? O6 Ca2 C4 O2 -155.81(18) 8_566 . . . ? O7 Ca2 C4 O2 -74.8(2) . . . . ? O5 Ca2 C4 O2 8.0(3) 3_545 . . . ? O3 Ca2 C4 O2 -166.2(3) . . . . ? O4 Ca2 C4 O2 6.82(19) 3_545 . . . ? C6 Ca2 C4 O2 8.4(2) 3_545 . . . ? C7 Ca2 C4 O2 -177.43(17) 8_566 . . . ? Ca1 Ca2 C4 O2 -5.31(16) . . . . ? O9 Ca2 C4 O3 -97.6(2) 2_554 . . . ? O6 Ca2 C4 O3 10.4(2) 8_566 . . . ? O7 Ca2 C4 O3 91.4(2) . . . . ? O5 Ca2 C4 O3 174.17(18) 3_545 . . . ? O2 Ca2 C4 O3 166.2(3) . . . . ? O4 Ca2 C4 O3 173.02(19) 3_545 . . . ? C6 Ca2 C4 O3 174.57(18) 3_545 . . . ? C7 Ca2 C4 O3 -11.2(2) 8_566 . . . ? Ca1 Ca2 C4 O3 160.9(2) . . . . ? O9 Ca2 C4 C2 -4.9(9) 2_554 . . . ? O6 Ca2 C4 C2 103.0(9) 8_566 . . . ? O7 Ca2 C4 C2 -176.0(9) . . . . ? O5 Ca2 C4 C2 -93.2(9) 3_545 . . . ? O3 Ca2 C4 C2 92.6(9) . . . . ? O2 Ca2 C4 C2 -101.2(10) . . . . ? O4 Ca2 C4 C2 -94.4(9) 3_545 . . . ? C6 Ca2 C4 C2 -92.8(9) 3_545 . . . ? C7 Ca2 C4 C2 81.4(9) 8_566 . . . ? Ca1 Ca2 C4 C2 -106.5(9) . . . . ? C1 C2 C5 C3 1.6(5) . . . . ? C4 C2 C5 C3 179.6(3) . . . . ? C8 C3 C5 C2 -1.5(5) . . . . ? C6 C3 C5 C2 179.8(3) . . . . ? Ca2 O5 C6 O4 -4.4(4) 3_455 . . . ? Ca2 O5 C6 C3 175.1(2) 3_455 . . . ? Ca1 O4 C6 O5 -130.0(5) 3_455 . . . ? Ca2 O4 C6 O5 4.0(3) 3_455 . . . ? Ca1 O4 C6 C3 50.5(7) 3_455 . . . ? Ca2 O4 C6 C3 -175.5(3) 3_455 . . . ? Ca1 O4 C6 Ca2 -134.0(6) 3_455 . . 3_455 ? C8 C3 C6 O5 -157.4(3) . . . . ? C5 C3 C6 O5 21.3(5) . . . . ? C8 C3 C6 O4 22.1(5) . . . . ? C5 C3 C6 O4 -159.2(3) . . . . ? C8 C3 C6 Ca2 -113(2) . . . 3_455 ? C5 C3 C6 Ca2 65(2) . . . 3_455 ? Ca2 O9 C7 O6 -107.8(6) 2_554 . . . ? Ca2 O9 C7 C9 72.8(7) 2_554 . . . ? Ca2 O9 C7 Ca2 -105.7(6) 2_554 . . 8_465 ? Ca2 O6 C7 O9 3.4(5) 8_465 . . . ? Ca2 O6 C7 C9 -177.2(2) 8_465 . . . ? C5 C3 C8 C9 0.0(5) . . . . ? C6 C3 C8 C9 178.7(3) . . . . ? C2 C1 C9 C8 -1.3(5) . . . . ? C2 C1 C9 C7 -179.7(3) . . . . ? C3 C8 C9 C1 1.4(5) . . . . ? C3 C8 C9 C7 179.7(3) . . . . ? O9 C7 C9 C1 2.5(5) . . . . ? O6 C7 C9 C1 -177.1(3) . . . . ? Ca2 C7 C9 C1 178.6(4) 8_465 . . . ? O9 C7 C9 C8 -175.8(3) . . . . ? O6 C7 C9 C8 4.6(5) . . . . ? Ca2 C7 C9 C8 0.3(7) 8_465 . . . ? Ca1 O8 C10 N1 87.8(8) . . . . ? Ca1 O8 C10 C11 -94.7(9) . . . . ? C12 N1 C10 O8 -2.7(7) . . . . ? C13 N1 C10 O8 177.2(4) . . . . ? C12 N1 C10 C11 179.8(5) . . . . ? C13 N1 C10 C11 -0.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.98 _diffrn_reflns_theta_full 27.82 _diffrn_measured_fraction_theta_full 0.98 _refine_diff_density_max 0.768 _refine_diff_density_min -0.787 _refine_diff_density_rms 0.110 data_Ca-BTC-DMF-313K _database_code_depnum_ccdc_archive 'CCDC 885043' #TrackingRef 'Ca-BTC-DMF-313K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ca-BTC-DMF-313K _chemical_melting_point ? _chemical_formula_moiety 'C28 H9 Ca3 N3 O14.98, C' _chemical_formula_sum 'C29 H9 Ca3 N3 O14.98' _chemical_formula_weight 759.34 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' N N 0.0061 0.0033 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 16.2817(3) _cell_length_b 13.5141(3) _cell_length_c 15.7591(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.2540(18) _cell_angle_gamma 90.00 _cell_volume 3461.92(12) _cell_formula_units_Z 4 _cell_measurement_temperature 313(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1535.2 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.848 _exptl_absorpt_correction_T_max 0.906 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _exptl_special_details ; ? ; _diffrn_ambient_temperature 313(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8481 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 28.08 _reflns_number_total 8481 _reflns_number_gt 5946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1102P)^2^+6.7123P] 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 -0.02(5) _refine_ls_number_reflns 6352 _refine_ls_number_parameters 384 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1728 _refine_ls_wR_factor_gt 0.1671 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.83952(5) 0.49366(6) 0.69240(5) 0.01855(19) Uani 1 1 d . . . Ca2 Ca 0.88322(5) 0.29920(7) 0.52193(5) 0.0232(2) Uani 1 1 d . . . Ca3 Ca 0.91303(6) 0.57405(7) 0.91462(5) 0.0251(2) Uani 1 1 d . . . O1 O 0.94520(19) 0.5793(3) 0.76402(19) 0.0246(6) Uani 1 1 d . . . O2 O 0.9419(2) 0.3683(3) 0.6612(2) 0.0322(8) Uani 1 1 d . . . O3 O 0.8530(3) 0.4263(3) 0.8383(3) 0.0446(10) Uani 1 1 d . . . C4 C 0.9908(3) 0.6546(4) 0.7702(3) 0.0243(9) Uani 1 1 d . . . O5 O 0.9924(3) 0.7119(3) 0.8324(2) 0.0411(10) Uani 1 1 d . . . O6 O 1.0246(2) 0.2749(2) 0.59081(18) 0.0248(7) Uani 1 1 d . . . O7 O 0.8283(2) 0.4835(4) 1.0163(2) 0.0452(11) Uani 1 1 d . . . O8 O 0.8492(3) 0.5727(4) 0.5633(2) 0.0445(10) Uani 1 1 d . . . C9 C 1.0080(3) 0.3216(3) 0.6565(3) 0.0213(9) Uani 1 1 d . . . C10 C 1.1835(3) 0.3243(4) 0.8685(3) 0.0298(11) Uani 1 1 d . . . H10 H 1.2230 0.3267 0.9135 0.036 Uiso 1 1 calc R . . O11 O 1.0492(3) 0.5205(4) 0.9322(3) 0.0565(14) Uani 1 1 d . . . C12 C 1.0679(3) 0.3182(4) 0.7319(3) 0.0255(10) Uani 1 1 d . . . C13 C 1.1298(3) 0.2492(4) 0.7388(3) 0.0248(9) Uani 1 1 d . . . H13 H 1.1325 0.2009 0.6970 0.030 Uiso 1 1 calc R . . O14 O 0.7666(2) 0.6278(3) 0.7447(3) 0.0440(10) Uani 1 1 d . . . N15 N 0.8033(10) 0.2799(9) 0.8759(8) 0.138(3) Uani 1 1 d . . . C16 C 1.0999(3) 0.7543(4) 0.7048(3) 0.0274(10) Uani 1 1 d . . . H16 H 1.0963 0.7996 0.7488 0.033 Uiso 1 1 calc R . . C17 C 1.0559(3) 0.6034(4) 0.6356(3) 0.0262(9) Uani 1 1 d . . . H17 H 1.0234 0.5468 0.6339 0.031 Uiso 1 1 calc R . . C18 C 0.8856(3) 0.4704(4) 1.0700(3) 0.0290(10) Uani 1 1 d . . . C19 C 0.7155(3) 0.3530(4) 0.6507(3) 0.0304(10) Uani 1 1 d . . . C20 C 1.1601(3) 0.7014(4) 0.5768(3) 0.0271(10) Uani 1 1 d . . . H20 H 1.1966 0.7120 0.5344 0.033 Uiso 1 1 calc R . . O21 O 0.7751(2) 0.3547(3) 0.6031(3) 0.0419(10) Uani 1 1 d . . . C22 C 1.0494(3) 0.6720(4) 0.7009(3) 0.0245(9) Uani 1 1 d . . . C23 C 0.8785(3) 0.5439(4) 0.4951(3) 0.0364(13) Uani 1 1 d . . . C24 C 1.0628(3) 0.3910(4) 0.7948(3) 0.0286(10) Uani 1 1 d . . . H24 H 1.0206 0.4374 0.7909 0.034 Uiso 1 1 calc R . . C25 C 1.1111(3) 0.6198(4) 0.5732(3) 0.0276(10) Uani 1 1 d . . . C26 C 1.1883(3) 0.2495(4) 0.8061(3) 0.0271(10) Uani 1 1 d . . . O27 O 0.7980(2) 0.6672(3) 0.8792(2) 0.0407(10) Uani 1 1 d . . . C28 C 1.1564(3) 0.7694(4) 0.6428(3) 0.0278(10) Uani 1 1 d . . . O29 O 0.7048(3) 0.4204(3) 0.7023(3) 0.0553(13) Uani 1 1 d . . . C30 C 1.1210(3) 0.3938(4) 0.8636(3) 0.0275(10) Uani 1 1 d . . . C31 C 0.7558(3) 0.6744(4) 0.8110(3) 0.0301(10) Uani 1 1 d . . . O32 O 0.8968(4) 0.4584(4) 0.4795(4) 0.0723(19) Uani 1 1 d . . . C38 C 0.8013(9) 0.3710(11) 0.8646(7) 0.105(2) Uani 1 1 d . . . H38 H 0.7526 0.4015 0.8784 0.125 Uiso 1 1 calc R . . O4 O 1.0000 0.7127(6) 1.0000 0.132(6) Uani 1 2 d S . . O9 O 0.8724(5) 0.1368(6) 0.5690(5) 0.094(2) Uiso 1 1 d . . . O10 O 0.7751(6) 0.3090(8) 0.4208(6) 0.051(4) Uiso 0.482(19) 1 d P . . C1 C 0.7311(16) 0.220(2) 0.9098(17) 0.203(4) Uiso 1 1 d . . . N1 N 0.6933(9) 0.3898(11) 0.3196(11) 0.153(5) Uani 1 1 d . . . C2 C 0.7131(8) 0.3079(11) 0.3694(7) 0.105(2) Uani 1 1 d . . . H2 H 0.6804 0.2515 0.3647 0.125 Uiso 1 1 calc R . . C3 C 0.7545(17) 0.484(2) 0.3207(17) 0.203(4) Uiso 1 1 d . . . C7 C 0.6139(15) 0.385(2) 0.2601(16) 0.203(4) Uiso 1 1 d . . . C11 C 0.8808(18) 0.224(2) 0.8605(18) 0.203(4) Uiso 1 1 d . . . N2 N 0.9564(10) -0.0083(9) 0.5540(8) 0.138(3) Uani 1 1 d . . . C5 C 0.8810(8) 0.0507(11) 0.5271(7) 0.105(2) Uani 1 1 d . . . H5 H 0.8431 0.0293 0.4847 0.125 Uiso 1 1 calc R . . C6 C 1.0247(16) 0.033(2) 0.6176(17) 0.203(4) Uiso 1 1 d . . . C8 C 0.9603(14) -0.115(2) 0.5161(18) 0.203(4) Uiso 1 1 d . . . C1A C 0.7833(7) 0.2049(9) 0.4248(7) 0.086(3) Uiso 1 1 d . . . C2A C 0.8972(18) 0.002(3) 0.654(2) 0.233(12) 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 Ca1 0.0207(4) 0.0180(4) 0.0172(3) -0.0009(3) 0.0035(3) -0.0001(3) Ca2 0.0219(4) 0.0298(5) 0.0183(4) 0.0000(4) 0.0033(3) 0.0008(4) Ca3 0.0237(4) 0.0336(5) 0.0181(4) 0.0051(4) 0.0026(3) 0.0094(4) O1 0.0213(14) 0.0284(16) 0.0243(14) 0.0010(14) 0.0048(12) -0.0038(14) O2 0.0290(17) 0.038(2) 0.0288(16) -0.0076(15) -0.0039(13) 0.0175(17) O3 0.056(3) 0.039(2) 0.040(2) 0.0101(19) 0.0165(19) -0.007(2) C4 0.024(2) 0.030(2) 0.0200(19) -0.0003(18) 0.0050(17) -0.0003(19) O5 0.050(2) 0.043(2) 0.0317(18) -0.0190(17) 0.0178(17) -0.0119(19) O6 0.0287(16) 0.0302(17) 0.0157(13) -0.0026(13) 0.0012(11) 0.0029(14) O7 0.0357(19) 0.063(3) 0.0358(19) 0.025(2) -0.0088(15) -0.013(2) O8 0.056(2) 0.050(2) 0.0301(17) 0.0186(19) 0.0194(17) 0.007(2) C9 0.023(2) 0.022(2) 0.0189(17) 0.0003(16) 0.0015(16) 0.0028(17) C10 0.027(2) 0.037(3) 0.024(2) -0.004(2) -0.0066(17) 0.015(2) O11 0.051(2) 0.071(3) 0.046(2) -0.038(2) -0.0195(19) 0.038(2) C12 0.025(2) 0.035(3) 0.0158(17) -0.0040(18) -0.0004(16) 0.005(2) C13 0.029(2) 0.025(2) 0.0201(19) -0.0043(18) -0.0006(17) 0.003(2) O14 0.037(2) 0.045(2) 0.050(2) -0.021(2) -0.0054(17) 0.0180(19) N15 0.190(9) 0.101(6) 0.125(6) 0.008(5) 0.032(6) -0.074(6) C16 0.028(2) 0.029(2) 0.026(2) -0.009(2) 0.0112(18) -0.007(2) C17 0.025(2) 0.023(2) 0.032(2) -0.0038(19) 0.0049(18) -0.0067(19) C18 0.031(2) 0.035(3) 0.0203(19) 0.0031(19) -0.0013(18) -0.012(2) C19 0.025(2) 0.032(3) 0.035(2) -0.010(2) 0.0064(19) -0.008(2) C20 0.028(2) 0.029(2) 0.025(2) -0.0054(19) 0.0121(18) -0.007(2) O21 0.0344(19) 0.043(2) 0.051(2) -0.0162(19) 0.0244(17) -0.0170(18) C22 0.023(2) 0.027(2) 0.024(2) -0.0039(18) 0.0033(17) -0.0068(19) C23 0.037(3) 0.037(3) 0.037(3) 0.021(2) 0.013(2) 0.010(2) C24 0.025(2) 0.038(3) 0.022(2) -0.005(2) -0.0060(17) 0.016(2) C25 0.025(2) 0.030(2) 0.028(2) -0.011(2) 0.0075(18) -0.007(2) C26 0.027(2) 0.029(2) 0.025(2) -0.0013(19) 0.0019(17) 0.010(2) O27 0.038(2) 0.053(3) 0.0316(18) 0.0057(18) -0.0010(15) 0.024(2) C28 0.030(2) 0.025(2) 0.029(2) -0.0077(19) 0.0081(18) -0.011(2) O29 0.049(2) 0.043(2) 0.078(3) -0.040(2) 0.035(2) -0.024(2) C30 0.028(2) 0.033(2) 0.0209(19) -0.0071(19) -0.0037(17) 0.010(2) C31 0.028(2) 0.029(2) 0.034(2) -0.003(2) 0.0022(19) 0.012(2) O32 0.105(4) 0.036(2) 0.082(4) 0.035(2) 0.056(3) 0.035(3) C38 0.116(5) 0.112(6) 0.083(4) 0.002(4) -0.011(4) -0.010(5) O4 0.319(19) 0.040(4) 0.035(4) 0.000 -0.004(7) 0.000 N1 0.147(11) 0.117(9) 0.188(13) -0.008(10) -0.042(10) 0.033(9) C2 0.116(5) 0.112(6) 0.083(4) 0.002(4) -0.011(4) -0.010(5) N2 0.190(9) 0.101(6) 0.125(6) 0.008(5) 0.032(6) -0.074(6) C5 0.116(5) 0.112(6) 0.083(4) 0.002(4) -0.011(4) -0.010(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 Ca1 O8 2.311(4) . ? Ca1 O1 2.314(3) . ? Ca1 O14 2.342(4) . ? Ca1 O29 2.419(4) . ? Ca1 O2 2.446(3) . ? Ca1 O3 2.471(4) . ? Ca1 O21 2.538(4) . ? Ca2 O32 2.268(5) . ? Ca2 O10 2.310(10) . ? Ca2 O9 2.327(8) . ? Ca2 O21 2.357(4) . ? Ca2 O6 2.412(3) 2_756 ? Ca2 O6 2.510(3) . ? Ca2 O2 2.523(4) . ? Ca2 Ca2 3.9033(17) 2_756 ? Ca3 O27 2.299(4) . ? Ca3 O11 2.334(4) . ? Ca3 O1 2.460(3) . ? Ca3 O7 2.495(4) . ? Ca3 O3 2.501(5) . ? Ca3 O11 2.562(4) 2_757 ? Ca3 O5 2.648(4) . ? Ca3 O4 2.666(6) . ? Ca3 Ca3 3.7943(18) 2_757 ? O1 C4 1.259(6) . ? O2 C9 1.253(6) . ? O3 C38 1.216(14) . ? C4 O5 1.248(6) . ? C4 C22 1.509(6) . ? O6 C9 1.255(5) . ? O6 Ca2 2.412(3) 2_756 ? O7 C18 1.237(6) . ? O8 C23 1.261(7) . ? C9 C12 1.495(6) . ? C10 C30 1.384(7) . ? C10 C26 1.414(7) . ? O11 C18 1.260(6) 2_757 ? O11 Ca3 2.562(4) 2_757 ? C12 C13 1.372(7) . ? C12 C24 1.402(7) . ? C13 C26 1.385(6) . ? O14 C31 1.242(6) . ? N15 C38 1.244(17) . ? N15 C11 1.50(3) . ? N15 C1 1.55(3) . ? C16 C22 1.383(7) . ? C16 C28 1.394(6) . ? C17 C25 1.387(6) . ? C17 C22 1.393(7) . ? C18 O11 1.260(6) 2_757 ? C18 C30 1.480(6) 2_757 ? C19 O29 1.239(6) . ? C19 O21 1.260(6) . ? C19 C28 1.485(7) 3_445 ? C20 C25 1.361(7) . ? C20 C28 1.392(7) . ? C23 O32 1.222(8) . ? C23 C25 1.502(6) 2_756 ? C24 C30 1.399(6) . ? C25 C23 1.502(6) 2_756 ? C26 C31 1.495(7) 3_545 ? O27 C31 1.246(6) . ? C28 C19 1.485(7) 3 ? C30 C18 1.480(6) 2_757 ? C31 C26 1.495(7) 3_455 ? O4 Ca3 2.666(6) 2_757 ? O9 C5 1.349(15) . ? O10 C2 1.259(15) . ? N1 C2 1.385(19) . ? N1 C7 1.56(3) . ? N1 C3 1.61(3) . ? N2 C5 1.504(19) . ? N2 C8 1.56(3) . ? N2 C6 1.56(3) . ? C8 C8 1.42(4) 2_756 ? 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 O8 Ca1 O1 96.44(15) . . ? O8 Ca1 O14 90.77(17) . . ? O1 Ca1 O14 79.55(13) . . ? O8 Ca1 O29 110.69(19) . . ? O1 Ca1 O29 145.60(14) . . ? O14 Ca1 O29 79.34(15) . . ? O8 Ca1 O2 93.54(14) . . ? O1 Ca1 O2 87.03(12) . . ? O14 Ca1 O2 166.29(13) . . ? O29 Ca1 O2 111.09(15) . . ? O8 Ca1 O3 169.26(17) . . ? O1 Ca1 O3 72.92(14) . . ? O14 Ca1 O3 88.72(16) . . ? O29 Ca1 O3 79.76(18) . . ? O2 Ca1 O3 84.62(14) . . ? O8 Ca1 O21 84.28(16) . . ? O1 Ca1 O21 155.97(13) . . ? O14 Ca1 O21 124.48(14) . . ? O29 Ca1 O21 52.04(12) . . ? O2 Ca1 O21 68.97(13) . . ? O3 Ca1 O21 104.80(15) . . ? O32 Ca2 O10 80.0(3) . . ? O32 Ca2 O9 178.2(3) . . ? O10 Ca2 O9 101.9(3) . . ? O32 Ca2 O21 86.95(16) . . ? O10 Ca2 O21 78.0(3) . . ? O9 Ca2 O21 93.1(2) . . ? O32 Ca2 O6 80.58(15) . 2_756 ? O10 Ca2 O6 88.9(2) . 2_756 ? O9 Ca2 O6 99.7(2) . 2_756 ? O21 Ca2 O6 163.37(15) . 2_756 ? O32 Ca2 O6 98.6(2) . . ? O10 Ca2 O6 161.8(2) . . ? O9 Ca2 O6 79.8(2) . . ? O21 Ca2 O6 120.13(13) . . ? O6 Ca2 O6 72.97(11) 2_756 . ? O32 Ca2 O2 82.4(2) . . ? O10 Ca2 O2 144.6(3) . . ? O9 Ca2 O2 95.9(2) . . ? O21 Ca2 O2 70.60(14) . . ? O6 Ca2 O2 118.06(12) 2_756 . ? O6 Ca2 O2 51.63(10) . . ? O32 Ca2 Ca2 80.51(15) . 2_756 ? O10 Ca2 Ca2 126.1(2) . 2_756 ? O9 Ca2 Ca2 98.56(19) . 2_756 ? O21 Ca2 Ca2 149.49(11) . 2_756 ? O6 Ca2 Ca2 38.42(8) 2_756 2_756 ? O6 Ca2 Ca2 36.67(7) . 2_756 ? O2 Ca2 Ca2 80.18(8) . 2_756 ? O27 Ca3 O11 162.6(2) . . ? O27 Ca3 O1 88.02(13) . . ? O11 Ca3 O1 82.56(14) . . ? O27 Ca3 O7 87.23(15) . . ? O11 Ca3 O7 109.15(18) . . ? O1 Ca3 O7 142.17(14) . . ? O27 Ca3 O3 91.70(16) . . ? O11 Ca3 O3 98.75(16) . . ? O1 Ca3 O3 70.01(12) . . ? O7 Ca3 O3 72.65(15) . . ? O27 Ca3 O11 122.13(17) . 2_757 ? O11 Ca3 O11 68.0(2) . 2_757 ? O1 Ca3 O11 149.82(16) . 2_757 ? O7 Ca3 O11 50.78(13) . 2_757 ? O3 Ca3 O11 107.09(15) . 2_757 ? O27 Ca3 O5 84.81(15) . . ? O11 Ca3 O5 77.86(18) . . ? O1 Ca3 O5 51.01(11) . . ? O7 Ca3 O5 164.36(15) . . ? O3 Ca3 O5 120.97(12) . . ? O11 Ca3 O5 124.24(13) 2_757 . ? O27 Ca3 O4 98.02(17) . . ? O11 Ca3 O4 71.60(16) . . ? O1 Ca3 O4 109.29(10) . . ? O7 Ca3 O4 108.54(12) . . ? O3 Ca3 O4 170.23(16) . . ? O11 Ca3 O4 68.34(16) 2_757 . ? O5 Ca3 O4 59.52(11) . . ? O27 Ca3 Ca3 137.47(11) . 2_757 ? O11 Ca3 Ca3 41.42(10) . 2_757 ? O1 Ca3 Ca3 119.53(8) . 2_757 ? O7 Ca3 Ca3 87.84(9) . 2_757 ? O3 Ca3 Ca3 126.64(11) . 2_757 ? O11 Ca3 Ca3 37.07(9) 2_757 2_757 ? O5 Ca3 Ca3 88.96(10) . 2_757 ? O4 Ca3 Ca3 44.64(13) . 2_757 ? C4 O1 Ca1 149.3(3) . . ? C4 O1 Ca3 96.0(3) . . ? Ca1 O1 Ca3 105.24(12) . . ? C9 O2 Ca1 163.3(3) . . ? C9 O2 Ca2 92.6(3) . . ? Ca1 O2 Ca2 101.67(12) . . ? C38 O3 Ca1 121.1(6) . . ? C38 O3 Ca3 125.9(7) . . ? Ca1 O3 Ca3 99.49(15) . . ? O5 C4 O1 123.3(4) . . ? O5 C4 C22 119.0(4) . . ? O1 C4 C22 117.6(4) . . ? C4 O5 Ca3 87.6(3) . . ? C9 O6 Ca2 135.4(3) . 2_756 ? C9 O6 Ca2 93.2(3) . . ? Ca2 O6 Ca2 104.91(11) 2_756 . ? C18 O7 Ca3 94.9(3) . . ? C23 O8 Ca1 131.0(4) . . ? O2 C9 O6 121.9(4) . . ? O2 C9 C12 119.5(4) . . ? O6 C9 C12 118.6(4) . . ? C30 C10 C26 121.0(4) . . ? C18 O11 Ca3 163.5(4) 2_757 . ? C18 O11 Ca3 91.2(3) 2_757 2_757 ? Ca3 O11 Ca3 101.51(15) . 2_757 ? C13 C12 C24 119.6(4) . . ? C13 C12 C9 121.7(4) . . ? C24 C12 C9 118.6(4) . . ? C12 C13 C26 121.8(4) . . ? C31 O14 Ca1 142.0(4) . . ? C38 N15 C11 119.4(17) . . ? C38 N15 C1 123.5(19) . . ? C11 N15 C1 117.0(17) . . ? C22 C16 C28 120.1(4) . . ? C25 C17 C22 119.9(4) . . ? O7 C18 O11 120.6(5) . 2_757 ? O7 C18 C30 120.0(4) . 2_757 ? O11 C18 C30 119.4(4) 2_757 2_757 ? O29 C19 O21 121.2(5) . . ? O29 C19 C28 120.0(4) . 3_445 ? O21 C19 C28 118.8(4) . 3_445 ? C25 C20 C28 121.1(4) . . ? C19 O21 Ca2 160.3(4) . . ? C19 O21 Ca1 89.5(3) . . ? Ca2 O21 Ca1 103.78(14) . . ? C16 C22 C17 119.8(4) . . ? C16 C22 C4 119.5(4) . . ? C17 C22 C4 120.6(4) . . ? O32 C23 O8 124.8(5) . . ? O32 C23 C25 117.5(5) . 2_756 ? O8 C23 C25 117.6(5) . 2_756 ? C30 C24 C12 120.1(4) . . ? C20 C25 C17 120.1(4) . . ? C20 C25 C23 119.6(4) . 2_756 ? C17 C25 C23 120.2(4) . 2_756 ? C13 C26 C10 118.2(4) . . ? C13 C26 C31 120.6(4) . 3_545 ? C10 C26 C31 121.2(4) . 3_545 ? C31 O27 Ca3 130.8(3) . . ? C20 C28 C16 119.1(4) . . ? C20 C28 C19 120.6(4) . 3 ? C16 C28 C19 120.2(4) . 3 ? C19 O29 Ca1 95.6(3) . . ? C10 C30 C24 119.2(4) . . ? C10 C30 C18 121.3(4) . 2_757 ? C24 C30 C18 119.5(4) . 2_757 ? O14 C31 O27 126.1(5) . . ? O14 C31 C26 116.1(4) . 3_455 ? O27 C31 C26 117.7(4) . 3_455 ? C23 O32 Ca2 144.0(4) . . ? O3 C38 N15 130.1(16) . . ? Ca3 O4 Ca3 90.7(3) 2_757 . ? C5 O9 Ca2 130.2(7) . . ? C2 O10 Ca2 174.6(10) . . ? C2 N1 C7 117.8(17) . . ? C2 N1 C3 119.9(15) . . ? C7 N1 C3 122.2(17) . . ? O10 C2 N1 120.5(14) . . ? C5 N2 C8 115.6(15) . . ? C5 N2 C6 122.2(14) . . ? C8 N2 C6 122.2(19) . . ? O9 C5 N2 115.2(10) . . ? C8 C8 N2 101.3(13) 2_756 . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 28.08 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.979 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.107 data_Ca-BTC-DMSO _database_code_depnum_ccdc_archive 'CCDC 885044' #TrackingRef 'Ca-BTC-DMSO.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ca-BTC-DMSO _chemical_melting_point ? _chemical_formula_moiety 'C22 H22 Ca3 O16 S2, 2(C H3 O S)' _chemical_formula_sum 'C24 H28 Ca3 O18 S4' _chemical_formula_weight 852.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 15.547(3) _cell_length_b 13.6128(19) _cell_length_c 18.981(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.88(2) _cell_angle_gamma 90.00 _cell_volume 3931.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760.0 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.861 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10360 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 29.07 _reflns_number_total 5252 _reflns_number_gt 3542 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1243P)^2^+19.7714P] 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 4502 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0976 _refine_ls_R_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.2522 _refine_ls_wR_factor_gt 0.2320 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.003 _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 0.69807(8) 0.2500 0.0186(3) Uani 1 2 d S . . S1 S 0.32437(8) 0.71107(12) 0.08782(7) 0.0450(4) Uani 1 1 d . . . O2 O 0.4282(2) 0.5788(2) 0.30302(16) 0.0318(7) Uani 1 1 d . . . O3 O 0.0660(2) 0.9811(3) 0.45426(17) 0.0368(8) Uani 1 1 d . . . O4 O 0.4152(2) 0.6802(3) 0.12915(17) 0.0360(8) Uani 1 1 d . . . O5 O 0.4089(2) 0.7677(3) 0.3921(2) 0.0440(9) Uani 1 1 d . . . O6 O 0.1569(3) 0.8653(3) 0.5050(2) 0.0508(11) Uani 1 1 d . . . O7 O 0.3637(2) 0.4763(3) 0.36559(17) 0.0394(8) Uani 1 1 d . . . O9 O 0.4049(3) 0.8125(3) 0.2782(2) 0.0458(10) Uani 1 1 d . . . C10 C 0.3777(3) 0.5067(3) 0.3065(2) 0.0279(9) Uani 1 1 d . . . C11 C 0.2468(3) 0.9108(4) 0.2687(3) 0.0349(11) Uani 1 1 d . . . H11 H 0.2726 0.9085 0.2286 0.042 Uiso 1 1 calc R . . C12 C 0.3747(3) 0.8111(4) 0.3354(3) 0.0355(11) Uani 1 1 d . . . C13 C 0.1707(3) 0.9192(4) 0.3887(3) 0.0379(12) Uani 1 1 d . . . C14 C 0.2895(3) 0.8665(4) 0.3319(3) 0.0364(11) Uani 1 1 d . . . C15 C 0.3331(3) 0.4586(3) 0.2368(2) 0.0326(10) Uani 1 1 d . . . C16 C 0.2509(4) 0.8691(4) 0.3924(3) 0.0405(13) Uani 1 1 d . . . H16 H 0.2781 0.8380 0.4348 0.049 Uiso 1 1 calc R . . C17 C 0.2521(4) 0.6933(6) 0.1482(4) 0.0644(19) Uani 1 1 d . . . H17A H 0.2441 0.6243 0.1548 0.097 Uiso 1 1 calc R . . H17B H 0.1963 0.7232 0.1287 0.097 Uiso 1 1 calc R . . H17C H 0.2769 0.7230 0.1938 0.097 Uiso 1 1 calc R . . C19 C 0.1294(3) 0.9634(4) 0.3244(3) 0.0354(11) Uani 1 1 d . . . H19 H 0.0764 0.9963 0.3220 0.042 Uiso 1 1 calc R . . C20 C 0.1289(3) 0.9222(4) 0.4539(3) 0.0357(11) Uani 1 1 d . . . C22 C 0.3289(7) 0.8404(8) 0.0877(6) 0.106(2) Uani 1 1 d . . . H22A H 0.3571 0.8633 0.1347 0.158 Uiso 1 1 calc R . . H22B H 0.2704 0.8665 0.0755 0.158 Uiso 1 1 calc R . . H22C H 0.3618 0.8620 0.0530 0.158 Uiso 1 1 calc R . . Ca2 Ca 0.46456(5) 0.61221(6) 0.43405(4) 0.0221(3) Uani 1 1 d . . . O1 O 0.5632(3) 0.6858(3) 0.5366(2) 0.0447(9) Uani 1 1 d . . . H1A H 0.5399 0.7409 0.5524 0.067 Uiso 1 1 d R . . H1B H 0.5754 0.6439 0.5746 0.067 Uiso 1 1 d R . . S8 S 0.4668(3) 0.9192(5) 0.6097(4) 0.272(5) Uani 1 1 d . . . C8 C 0.3663(7) 0.8605(9) 0.6024(6) 0.106(2) Uani 1 1 d . . . H8A H 0.3198 0.9080 0.5912 0.158 Uiso 1 1 calc R . . H8B H 0.3640 0.8289 0.6472 0.158 Uiso 1 1 calc R . . H8C H 0.3595 0.8123 0.5648 0.158 Uiso 1 1 calc R . . O8 O 0.5321(6) 0.8460(8) 0.6111(6) 0.170(5) 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 0.0151(5) 0.0252(6) 0.0170(5) 0.000 0.0066(4) 0.000 S1 0.0261(6) 0.0758(10) 0.0289(6) -0.0044(6) -0.0039(5) 0.0052(6) O2 0.0424(18) 0.0358(17) 0.0206(14) -0.0055(13) 0.0139(13) -0.0190(14) O3 0.0425(19) 0.045(2) 0.0301(16) 0.0118(15) 0.0246(15) 0.0233(15) O4 0.0205(15) 0.062(2) 0.0243(16) -0.0050(15) 0.0015(12) 0.0024(14) O5 0.048(2) 0.045(2) 0.045(2) 0.0212(17) 0.0225(17) 0.0253(17) O6 0.055(2) 0.068(3) 0.040(2) 0.0312(19) 0.0344(18) 0.038(2) O7 0.049(2) 0.049(2) 0.0234(16) 0.0023(15) 0.0147(15) -0.0150(16) O9 0.052(2) 0.052(2) 0.044(2) 0.0153(17) 0.0354(18) 0.0279(18) C10 0.033(2) 0.032(2) 0.023(2) -0.0029(17) 0.0160(17) -0.0076(17) C11 0.045(3) 0.037(2) 0.031(2) 0.014(2) 0.027(2) 0.020(2) C12 0.041(3) 0.033(2) 0.039(3) 0.008(2) 0.023(2) 0.018(2) C13 0.047(3) 0.043(3) 0.033(2) 0.013(2) 0.029(2) 0.023(2) C14 0.042(3) 0.039(3) 0.037(2) 0.014(2) 0.029(2) 0.022(2) C15 0.041(3) 0.034(2) 0.028(2) -0.0123(19) 0.021(2) -0.019(2) C16 0.048(3) 0.047(3) 0.034(2) 0.019(2) 0.028(2) 0.026(2) C17 0.028(3) 0.087(5) 0.078(5) 0.009(4) 0.013(3) 0.014(3) C19 0.042(3) 0.039(3) 0.032(2) 0.012(2) 0.024(2) 0.023(2) C20 0.040(3) 0.043(3) 0.030(2) 0.011(2) 0.023(2) 0.017(2) C22 0.091(5) 0.109(6) 0.106(5) 0.007(5) -0.004(4) 0.009(4) Ca2 0.0235(4) 0.0282(5) 0.0160(4) 0.0034(3) 0.0076(3) 0.0074(3) O1 0.054(2) 0.044(2) 0.0342(19) -0.0017(16) 0.0057(17) -0.0030(17) S8 0.136(4) 0.250(6) 0.395(10) -0.249(7) -0.026(4) 0.044(4) C8 0.091(5) 0.109(6) 0.106(5) 0.007(5) -0.004(4) 0.009(4) O8 0.140(7) 0.156(8) 0.186(9) -0.094(7) -0.034(6) 0.075(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 O9 2.286(3) . ? Ca1 O9 2.286(3) 2_655 ? Ca1 O2 2.314(3) . ? Ca1 O2 2.314(3) 2_655 ? Ca1 O4 2.411(3) . ? Ca1 O4 2.411(3) 2_655 ? Ca1 C12 3.176(4) 2_655 ? Ca1 Ca2 3.8297(11) 2_655 ? S1 O4 1.526(3) . ? S1 C22 1.762(12) . ? S1 C17 1.779(7) . ? O2 C10 1.267(5) . ? O2 Ca2 2.477(3) . ? O3 C20 1.265(5) . ? O3 Ca2 2.360(3) 3_455 ? O3 Ca2 2.598(3) 7_566 ? O4 Ca2 2.591(3) 2_655 ? O5 C12 1.248(6) . ? O5 Ca2 2.361(3) . ? O6 C20 1.248(6) . ? O6 Ca2 2.429(3) 7_566 ? O7 C10 1.256(5) . ? O7 Ca2 2.594(4) . ? O9 C12 1.269(6) . ? C10 C15 1.511(6) . ? C11 C14 1.384(7) . ? C11 C15 1.387(6) 4 ? C12 C14 1.514(6) . ? C13 C19 1.393(7) . ? C13 C16 1.411(6) . ? C13 C20 1.512(6) . ? C14 C16 1.401(6) . ? C15 C11 1.387(6) 4_545 ? C15 C19 1.406(6) 4_545 ? C19 C15 1.406(6) 4 ? C20 Ca2 2.850(4) 7_566 ? Ca2 O3 2.360(3) 3_545 ? Ca2 O6 2.429(3) 7_566 ? Ca2 O1 2.432(4) . ? Ca2 O4 2.591(3) 2_655 ? Ca2 O3 2.598(3) 7_566 ? Ca2 C20 2.850(4) 7_566 ? Ca2 Ca2 3.9596(16) 5_666 ? S8 O8 1.418(8) . ? S8 C8 1.735(12) . ? 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 O9 Ca1 O9 94.0(2) . 2_655 ? O9 Ca1 O2 89.05(13) . . ? O9 Ca1 O2 166.63(14) 2_655 . ? O9 Ca1 O2 166.62(14) . 2_655 ? O9 Ca1 O2 89.05(13) 2_655 2_655 ? O2 Ca1 O2 90.91(17) . 2_655 ? O9 Ca1 O4 92.18(13) . . ? O9 Ca1 O4 95.72(14) 2_655 . ? O2 Ca1 O4 97.16(12) . . ? O2 Ca1 O4 74.55(12) 2_655 . ? O9 Ca1 O4 95.72(13) . 2_655 ? O9 Ca1 O4 92.18(13) 2_655 2_655 ? O2 Ca1 O4 74.56(12) . 2_655 ? O2 Ca1 O4 97.16(12) 2_655 2_655 ? O4 Ca1 O4 168.4(2) . 2_655 ? O9 Ca1 C12 106.46(14) . 2_655 ? O9 Ca1 C12 19.32(12) 2_655 2_655 ? O2 Ca1 C12 164.35(13) . 2_655 ? O2 Ca1 C12 73.53(12) 2_655 2_655 ? O4 Ca1 C12 80.58(13) . 2_655 ? O4 Ca1 C12 105.16(13) 2_655 2_655 ? O9 Ca1 Ca2 130.00(10) . 2_655 ? O9 Ca1 Ca2 76.89(9) 2_655 2_655 ? O2 Ca1 Ca2 110.82(8) . 2_655 ? O2 Ca1 Ca2 38.41(7) 2_655 2_655 ? O4 Ca1 Ca2 41.80(8) . 2_655 ? O4 Ca1 Ca2 133.14(9) 2_655 2_655 ? C12 Ca1 Ca2 57.58(9) 2_655 2_655 ? O4 S1 C22 104.0(4) . . ? O4 S1 C17 105.7(3) . . ? C22 S1 C17 99.6(5) . . ? C10 O2 Ca1 157.8(3) . . ? C10 O2 Ca2 96.0(2) . . ? Ca1 O2 Ca2 106.10(12) . . ? C20 O3 Ca2 165.8(3) . 3_455 ? C20 O3 Ca2 88.0(3) . 7_566 ? Ca2 O3 Ca2 105.91(11) 3_455 7_566 ? S1 O4 Ca1 136.7(2) . . ? S1 O4 Ca2 122.66(17) . 2_655 ? Ca1 O4 Ca2 99.86(11) . 2_655 ? C12 O5 Ca2 141.0(4) . . ? C20 O6 Ca2 96.3(3) . 7_566 ? C10 O7 Ca2 90.8(3) . . ? C12 O9 Ca1 124.1(3) . . ? O7 C10 O2 121.7(4) . . ? O7 C10 C15 120.4(4) . . ? O2 C10 C15 117.9(4) . . ? C14 C11 C15 122.1(4) . 4 ? O5 C12 O9 125.4(4) . . ? O5 C12 C14 119.2(4) . . ? O9 C12 C14 115.5(4) . . ? C19 C13 C16 119.7(4) . . ? C19 C13 C20 120.4(4) . . ? C16 C13 C20 119.8(4) . . ? C11 C14 C16 119.4(4) . . ? C11 C14 C12 120.9(4) . . ? C16 C14 C12 119.7(4) . . ? C11 C15 C19 118.6(4) 4_545 4_545 ? C11 C15 C10 120.8(4) 4_545 . ? C19 C15 C10 120.6(4) 4_545 . ? C14 C16 C13 119.6(4) . . ? C13 C19 C15 120.6(4) . 4 ? O6 C20 O3 122.5(4) . . ? O6 C20 C13 118.6(4) . . ? O3 C20 C13 118.9(4) . . ? O6 C20 Ca2 57.9(2) . 7_566 ? O3 C20 Ca2 65.6(2) . 7_566 ? C13 C20 Ca2 167.7(4) . 7_566 ? O3 Ca2 O5 156.71(13) 3_545 . ? O3 Ca2 O6 125.26(12) 3_545 7_566 ? O5 Ca2 O6 77.32(12) . 7_566 ? O3 Ca2 O1 83.75(14) 3_545 . ? O5 Ca2 O1 91.56(15) . . ? O6 Ca2 O1 89.49(15) 7_566 . ? O3 Ca2 O2 91.78(12) 3_545 . ? O5 Ca2 O2 80.46(13) . . ? O6 Ca2 O2 117.56(13) 7_566 . ? O1 Ca2 O2 148.76(12) . . ? O3 Ca2 O4 79.83(12) 3_545 2_655 ? O5 Ca2 O4 76.89(13) . 2_655 ? O6 Ca2 O4 151.80(14) 7_566 2_655 ? O1 Ca2 O4 80.02(12) . 2_655 ? O2 Ca2 O4 68.76(10) . 2_655 ? O3 Ca2 O7 81.77(14) 3_545 . ? O5 Ca2 O7 109.20(14) . . ? O6 Ca2 O7 83.10(15) 7_566 . ? O1 Ca2 O7 155.67(13) . . ? O2 Ca2 O7 51.44(10) . . ? O4 Ca2 O7 116.23(11) 2_655 . ? O3 Ca2 O3 74.10(11) 3_545 7_566 ? O5 Ca2 O3 126.68(11) . 7_566 ? O6 Ca2 O3 51.85(10) 7_566 7_566 ? O1 Ca2 O3 74.93(13) . 7_566 ? O2 Ca2 O3 133.43(12) . 7_566 ? O4 Ca2 O3 145.39(11) 2_655 7_566 ? O7 Ca2 O3 82.34(12) . 7_566 ? O3 Ca2 C20 100.41(12) 3_545 7_566 ? O5 Ca2 C20 101.02(13) . 7_566 ? O6 Ca2 C20 25.80(12) 7_566 7_566 ? O1 Ca2 C20 78.78(15) . 7_566 ? O2 Ca2 C20 132.31(14) . 7_566 ? O4 Ca2 C20 158.63(14) 2_655 7_566 ? O7 Ca2 C20 84.73(14) . 7_566 ? O3 Ca2 C20 26.34(11) 7_566 7_566 ? O3 Ca2 Ca2 39.13(7) 3_545 5_666 ? O5 Ca2 Ca2 159.94(10) . 5_666 ? O6 Ca2 Ca2 86.49(9) 7_566 5_666 ? O1 Ca2 Ca2 76.38(10) . 5_666 ? O2 Ca2 Ca2 118.01(9) . 5_666 ? O4 Ca2 Ca2 115.78(8) 2_655 5_666 ? O7 Ca2 Ca2 80.05(9) . 5_666 ? O3 Ca2 Ca2 34.97(7) 7_566 5_666 ? C20 Ca2 Ca2 61.29(10) 7_566 5_666 ? O8 S8 C8 107.9(7) . . ? _diffrn_measured_fraction_theta_max 0.857 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.929 _refine_diff_density_min -1.866 _refine_diff_density_rms 0.144 data_Ca-BTC-H2O-348 _database_code_depnum_ccdc_archive 'CCDC 885045' #TrackingRef 'Ca-BTC-H2O-348K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ca-BTC-H2O-348 _chemical_melting_point ? _chemical_formula_moiety 'C9 H6 Ca O7' _chemical_formula_sum 'C9 H6 Ca O7' _chemical_formula_weight 266.22 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 6.8656(11) _cell_length_b 9.1287(16) _cell_length_c 9.9209(14) _cell_angle_alpha 101.341(13) _cell_angle_beta 99.683(12) _cell_angle_gamma 111.950(16) _cell_volume 545.11(18) _cell_formula_units_Z 2 _cell_measurement_temperature 348(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 272.0 _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.836 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _exptl_special_details ; ? ; _diffrn_ambient_temperature 348(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4319 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 29.24 _reflns_number_total 2980 _reflns_number_gt 2100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.1163P] 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 2493 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.31318(6) 0.57803(5) 0.10836(4) 0.02219(15) Uani 1 1 d . . . O1 O 0.3236(3) 0.54708(19) 0.35115(16) 0.0318(4) Uani 1 1 d . . . O2 O 0.0216(2) 0.3973(2) -0.12080(15) 0.0293(4) Uani 1 1 d . . . O3 O 0.5818(3) 0.84635(19) 0.49765(16) 0.0306(4) Uani 1 1 d . . . H3 H 0.4919 0.7508 0.4603 0.046 Uiso 1 1 calc R . . O4 O 0.3578(2) 0.4590(2) -0.13354(16) 0.0326(4) Uani 1 1 d . . . O5 O 0.5618(3) 0.84825(19) 0.27104(16) 0.0351(4) Uani 1 1 d . . . O6 O 0.1111(3) 0.3271(2) 0.17544(16) 0.0358(4) Uani 1 1 d . . . C7 C 0.0833(3) 0.3175(3) 0.4098(2) 0.0216(4) Uani 1 1 d . . . C8 C 0.0732(3) 0.3147(3) -0.3488(2) 0.0206(4) Uani 1 1 d . . . C9 C -0.0874(3) 0.1622(3) 0.3607(2) 0.0231(5) Uani 1 1 d . . . H9 H -0.1413 0.1103 0.2633 0.028 Uiso 1 1 calc R . . C10 C 0.6425(3) 0.9153(3) 0.3984(2) 0.0234(5) Uani 1 1 d . . . C11 C -0.1001(3) 0.1605(3) -0.3991(2) 0.0229(5) Uani 1 1 d . . . H11 H -0.1638 0.1088 -0.3357 0.027 Uiso 1 1 calc R . . C12 C 0.1780(3) 0.4020(3) 0.3058(2) 0.0236(5) Uani 1 1 d . . . C13 C 0.1561(3) 0.3952(3) -0.1912(2) 0.0219(4) Uani 1 1 d . . . C14 C 0.1660(3) 0.3929(3) 0.5562(2) 0.0230(5) Uani 1 1 d . . . H14 H 0.2835 0.4958 0.5904 0.028 Uiso 1 1 calc R . . C15 C -0.1785(3) 0.0834(3) 0.4549(2) 0.0215(4) Uani 1 1 d . . . O16 O 0.3178(3) 0.7895(3) -0.0137(2) 0.0555(6) Uani 1 1 d . . . H16A H 0.1898 0.7611 -0.0698 0.083 Uiso 1 1 d R . . H16B H 0.3541 0.8832 0.0486 0.083 Uiso 1 1 d 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 0.0173(2) 0.0267(3) 0.0152(2) 0.00205(18) 0.00307(17) 0.00404(18) O1 0.0306(9) 0.0242(8) 0.0245(8) 0.0043(7) 0.0039(7) -0.0029(7) O2 0.0245(8) 0.0392(10) 0.0172(8) 0.0001(7) 0.0065(7) 0.0096(7) O3 0.0314(9) 0.0228(8) 0.0246(8) 0.0048(7) 0.0054(7) -0.0006(7) O4 0.0194(8) 0.0477(11) 0.0184(8) -0.0043(7) -0.0019(6) 0.0107(7) O5 0.0378(9) 0.0262(9) 0.0203(8) 0.0015(7) -0.0010(7) -0.0027(7) O6 0.0407(10) 0.0327(9) 0.0175(8) 0.0046(7) 0.0044(7) 0.0006(8) C7 0.0209(10) 0.0226(11) 0.0181(10) 0.0039(8) 0.0031(8) 0.0077(8) C8 0.0169(10) 0.0247(11) 0.0145(9) -0.0005(8) 0.0008(8) 0.0072(8) C9 0.0233(11) 0.0232(11) 0.0143(10) 0.0010(8) -0.0001(8) 0.0052(9) C10 0.0206(10) 0.0223(11) 0.0211(11) 0.0017(9) 0.0026(9) 0.0062(8) C11 0.0208(10) 0.0249(11) 0.0197(10) 0.0040(9) 0.0063(9) 0.0071(9) C12 0.0222(11) 0.0257(11) 0.0188(10) 0.0063(9) 0.0035(9) 0.0066(9) C13 0.0220(11) 0.0243(11) 0.0175(10) 0.0039(8) 0.0029(9) 0.0096(9) C14 0.0189(10) 0.0221(11) 0.0208(10) 0.0014(8) 0.0019(9) 0.0047(8) C15 0.0204(10) 0.0186(10) 0.0198(10) 0.0014(8) 0.0031(8) 0.0051(8) O16 0.0486(12) 0.0492(12) 0.0489(12) 0.0189(10) -0.0060(10) 0.0052(10) _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 2.3859(16) 2_665 ? Ca1 O2 2.4127(16) 2_565 ? Ca1 O5 2.4418(17) . ? Ca1 O16 2.466(2) . ? Ca1 O1 2.4722(16) . ? Ca1 O6 2.4795(18) . ? Ca1 O2 2.5343(16) . ? Ca1 O4 2.5506(16) . ? Ca1 C12 2.831(2) . ? Ca1 C13 2.900(2) . ? Ca1 Ca1 4.0311(12) 2_565 ? Ca1 Ca1 4.0762(10) 2_665 ? O1 C12 1.257(3) . ? O2 C13 1.252(3) . ? O2 Ca1 2.4127(16) 2_565 ? O3 C10 1.313(3) . ? O3 H3 0.8200 . ? O4 C13 1.258(2) . ? O4 Ca1 2.3859(16) 2_665 ? O5 C10 1.218(2) . ? O6 C12 1.253(2) . ? C7 C9 1.384(3) . ? C7 C14 1.394(3) . ? C7 C12 1.498(3) . ? C8 C11 1.385(3) . ? C8 C14 1.390(3) 1_554 ? C8 C13 1.498(3) . ? C9 C15 1.381(3) . ? C9 H9 0.9300 . ? C10 C15 1.483(3) 1_665 ? C11 C15 1.392(3) 1_554 ? C11 H11 0.9300 . ? C14 C8 1.390(3) 1_556 ? C14 H14 0.9300 . ? C15 C11 1.392(3) 1_556 ? C15 C10 1.483(3) 1_445 ? O16 H16A 0.8709 . ? O16 H16B 0.8703 . ? 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 Ca1 O2 170.11(6) 2_665 2_565 ? O4 Ca1 O5 81.52(6) 2_665 . ? O2 Ca1 O5 97.17(6) 2_565 . ? O4 Ca1 O16 112.22(7) 2_665 . ? O2 Ca1 O16 76.33(7) 2_565 . ? O5 Ca1 O16 71.46(6) . . ? O4 Ca1 O1 86.48(6) 2_665 . ? O2 Ca1 O1 83.74(6) 2_565 . ? O5 Ca1 O1 74.26(6) . . ? O16 Ca1 O1 137.41(7) . . ? O4 Ca1 O6 94.59(6) 2_665 . ? O2 Ca1 O6 78.26(6) 2_565 . ? O5 Ca1 O6 126.64(6) . . ? O16 Ca1 O6 150.61(6) . . ? O1 Ca1 O6 52.38(5) . . ? O4 Ca1 O2 114.57(5) 2_665 . ? O2 Ca1 O2 70.88(6) 2_565 . ? O5 Ca1 O2 151.43(6) . . ? O16 Ca1 O2 80.40(6) . . ? O1 Ca1 O2 127.65(6) . . ? O6 Ca1 O2 77.51(6) . . ? O4 Ca1 O4 68.71(6) 2_665 . ? O2 Ca1 O4 119.25(5) 2_565 . ? O5 Ca1 O4 124.26(6) . . ? O16 Ca1 O4 77.73(7) . . ? O1 Ca1 O4 144.04(6) . . ? O6 Ca1 O4 102.49(6) . . ? O2 Ca1 O4 51.13(5) . . ? O4 Ca1 C12 92.72(6) 2_665 . ? O2 Ca1 C12 77.84(6) 2_565 . ? O5 Ca1 C12 100.46(6) . . ? O16 Ca1 C12 151.60(7) . . ? O1 Ca1 C12 26.32(5) . . ? O6 Ca1 C12 26.23(5) . . ? O2 Ca1 C12 102.05(6) . . ? O4 Ca1 C12 126.03(6) . . ? O4 Ca1 C13 92.34(6) 2_665 . ? O2 Ca1 C13 94.61(6) 2_565 . ? O5 Ca1 C13 141.98(6) . . ? O16 Ca1 C13 76.51(7) . . ? O1 Ca1 C13 143.15(6) . . ? O6 Ca1 C13 91.12(6) . . ? O2 Ca1 C13 25.51(5) . . ? O4 Ca1 C13 25.69(5) . . ? C12 Ca1 C13 117.35(6) . . ? O4 Ca1 Ca1 148.32(4) 2_665 2_565 ? O2 Ca1 Ca1 36.44(4) 2_565 2_565 ? O5 Ca1 Ca1 128.81(5) . 2_565 ? O16 Ca1 Ca1 75.74(5) . 2_565 ? O1 Ca1 Ca1 108.59(4) . 2_565 ? O6 Ca1 Ca1 75.06(4) . 2_565 ? O2 Ca1 Ca1 34.44(4) . 2_565 ? O4 Ca1 Ca1 84.14(4) . 2_565 ? C12 Ca1 Ca1 90.30(5) . 2_565 ? C13 Ca1 Ca1 58.71(4) . 2_565 ? O4 Ca1 Ca1 35.66(4) 2_665 2_665 ? O2 Ca1 Ca1 151.93(4) 2_565 2_665 ? O5 Ca1 Ca1 105.42(5) . 2_665 ? O16 Ca1 Ca1 95.07(6) . 2_665 ? O1 Ca1 Ca1 118.07(5) . 2_665 ? O6 Ca1 Ca1 100.50(5) . 2_665 ? O2 Ca1 Ca1 81.41(4) . 2_665 ? O4 Ca1 Ca1 33.05(3) . 2_665 ? C12 Ca1 Ca1 113.31(5) . 2_665 ? C13 Ca1 Ca1 57.32(4) . 2_665 ? Ca1 Ca1 Ca1 115.74(2) 2_565 2_665 ? C12 O1 Ca1 92.99(12) . . ? C13 O2 Ca1 148.16(14) . 2_565 ? C13 O2 Ca1 93.79(12) . . ? Ca1 O2 Ca1 109.12(6) 2_565 . ? C10 O3 H3 109.5 . . ? C13 O4 Ca1 146.08(14) . 2_665 ? C13 O4 Ca1 92.85(13) . . ? Ca1 O4 Ca1 111.28(6) 2_665 . ? C10 O5 Ca1 139.82(15) . . ? C12 O6 Ca1 92.75(13) . . ? C9 C7 C14 119.2(2) . . ? C9 C7 C12 119.96(18) . . ? C14 C7 C12 120.83(19) . . ? C11 C8 C14 120.12(19) . 1_554 ? C11 C8 C13 118.83(19) . . ? C14 C8 C13 121.05(19) 1_554 . ? C15 C9 C7 120.76(19) . . ? C15 C9 H9 119.6 . . ? C7 C9 H9 119.6 . . ? O5 C10 O3 123.7(2) . . ? O5 C10 C15 122.4(2) . 1_665 ? O3 C10 C15 113.92(17) . 1_665 ? C8 C11 C15 119.6(2) . 1_554 ? C8 C11 H11 120.2 . . ? C15 C11 H11 120.2 1_554 . ? O6 C12 O1 121.1(2) . . ? O6 C12 C7 119.55(19) . . ? O1 C12 C7 119.32(18) . . ? O6 C12 Ca1 61.02(12) . . ? O1 C12 Ca1 60.69(11) . . ? C7 C12 Ca1 172.24(15) . . ? O2 C13 O4 121.92(19) . . ? O2 C13 C8 118.67(18) . . ? O4 C13 C8 119.41(19) . . ? O2 C13 Ca1 60.70(10) . . ? O4 C13 Ca1 61.47(11) . . ? C8 C13 Ca1 174.66(15) . . ? C8 C14 C7 120.2(2) 1_556 . ? C8 C14 H14 119.9 1_556 . ? C7 C14 H14 119.9 . . ? C9 C15 C11 120.06(19) . 1_556 ? C9 C15 C10 119.14(18) . 1_445 ? C11 C15 C10 120.79(19) 1_556 1_445 ? Ca1 O16 H16A 110.7 . . ? Ca1 O16 H16B 110.1 . . ? H16A O16 H16B 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 O4 Ca1 O1 C12 -103.38(14) 2_665 . . . ? O2 Ca1 O1 C12 75.16(14) 2_565 . . . ? O5 Ca1 O1 C12 174.44(14) . . . . ? O16 Ca1 O1 C12 137.08(14) . . . . ? O6 Ca1 O1 C12 -4.83(12) . . . . ? O2 Ca1 O1 C12 15.22(16) . . . . ? O4 Ca1 O1 C12 -58.15(17) . . . . ? C13 Ca1 O1 C12 -14.18(18) . . . . ? Ca1 Ca1 O1 C12 48.12(14) 2_565 . . . ? Ca1 Ca1 O1 C12 -86.19(13) 2_665 . . . ? O4 Ca1 O2 C13 -31.37(15) 2_665 . . . ? O2 Ca1 O2 C13 157.53(17) 2_565 . . . ? O5 Ca1 O2 C13 88.67(17) . . . . ? O16 Ca1 O2 C13 78.78(14) . . . . ? O1 Ca1 O2 C13 -136.88(13) . . . . ? O6 Ca1 O2 C13 -120.73(14) . . . . ? O4 Ca1 O2 C13 -3.15(12) . . . . ? C12 Ca1 O2 C13 -130.05(13) . . . . ? Ca1 Ca1 O2 C13 157.53(17) 2_565 . . . ? Ca1 Ca1 O2 C13 -17.90(12) 2_665 . . . ? O4 Ca1 O2 Ca1 171.10(6) 2_665 . . 2_565 ? O2 Ca1 O2 Ca1 0.0 2_565 . . 2_565 ? O5 Ca1 O2 Ca1 -68.86(14) . . . 2_565 ? O16 Ca1 O2 Ca1 -78.75(8) . . . 2_565 ? O1 Ca1 O2 Ca1 65.59(9) . . . 2_565 ? O6 Ca1 O2 Ca1 81.74(7) . . . 2_565 ? O4 Ca1 O2 Ca1 -160.68(10) . . . 2_565 ? C12 Ca1 O2 Ca1 72.42(8) . . . 2_565 ? C13 Ca1 O2 Ca1 -157.53(17) . . . 2_565 ? Ca1 Ca1 O2 Ca1 -175.43(6) 2_665 . . 2_565 ? O4 Ca1 O4 C13 155.64(18) 2_665 . . . ? O2 Ca1 O4 C13 -17.87(16) 2_565 . . . ? O5 Ca1 O4 C13 -141.54(13) . . . . ? O16 Ca1 O4 C13 -84.35(14) . . . . ? O1 Ca1 O4 C13 106.13(14) . . . . ? O6 Ca1 O4 C13 65.54(14) . . . . ? O2 Ca1 O4 C13 3.13(12) . . . . ? C12 Ca1 O4 C13 78.38(15) . . . . ? Ca1 Ca1 O4 C13 -7.71(13) 2_565 . . . ? Ca1 Ca1 O4 C13 155.64(18) 2_665 . . . ? O4 Ca1 O4 Ca1 0.0 2_665 . . 2_665 ? O2 Ca1 O4 Ca1 -173.51(6) 2_565 . . 2_665 ? O5 Ca1 O4 Ca1 62.82(10) . . . 2_665 ? O16 Ca1 O4 Ca1 120.00(8) . . . 2_665 ? O1 Ca1 O4 Ca1 -49.51(12) . . . 2_665 ? O6 Ca1 O4 Ca1 -90.10(8) . . . 2_665 ? O2 Ca1 O4 Ca1 -152.51(11) . . . 2_665 ? C12 Ca1 O4 Ca1 -77.27(9) . . . 2_665 ? C13 Ca1 O4 Ca1 -155.64(18) . . . 2_665 ? Ca1 Ca1 O4 Ca1 -163.36(7) 2_565 . . 2_665 ? O4 Ca1 O5 C10 -85.7(2) 2_665 . . . ? O2 Ca1 O5 C10 84.4(2) 2_565 . . . ? O16 Ca1 O5 C10 157.3(3) . . . . ? O1 Ca1 O5 C10 3.0(2) . . . . ? O6 Ca1 O5 C10 3.7(3) . . . . ? O2 Ca1 O5 C10 147.0(2) . . . . ? O4 Ca1 O5 C10 -142.7(2) . . . . ? C12 Ca1 O5 C10 5.5(3) . . . . ? C13 Ca1 O5 C10 -168.6(2) . . . . ? Ca1 Ca1 O5 C10 104.4(2) 2_565 . . . ? Ca1 Ca1 O5 C10 -112.5(2) 2_665 . . . ? O4 Ca1 O6 C12 86.82(14) 2_665 . . . ? O2 Ca1 O6 C12 -86.27(14) 2_565 . . . ? O5 Ca1 O6 C12 3.97(16) . . . . ? O16 Ca1 O6 C12 -116.88(17) . . . . ? O1 Ca1 O6 C12 4.85(12) . . . . ? O2 Ca1 O6 C12 -159.01(14) . . . . ? O4 Ca1 O6 C12 156.01(13) . . . . ? C13 Ca1 O6 C12 179.26(14) . . . . ? Ca1 Ca1 O6 C12 -123.62(14) 2_565 . . . ? Ca1 Ca1 O6 C12 122.32(13) 2_665 . . . ? C14 C7 C9 C15 1.3(3) . . . . ? C12 C7 C9 C15 -179.18(19) . . . . ? Ca1 O5 C10 O3 -9.9(4) . . . . ? Ca1 O5 C10 C15 169.51(16) . . . 1_665 ? C14 C8 C11 C15 1.0(3) 1_554 . . 1_554 ? C13 C8 C11 C15 -179.62(18) . . . 1_554 ? Ca1 O6 C12 O1 -8.8(2) . . . . ? Ca1 O6 C12 C7 171.13(17) . . . . ? Ca1 O1 C12 O6 8.9(2) . . . . ? Ca1 O1 C12 C7 -171.10(17) . . . . ? C9 C7 C12 O6 -4.4(3) . . . . ? C14 C7 C12 O6 175.1(2) . . . . ? C9 C7 C12 O1 175.5(2) . . . . ? C14 C7 C12 O1 -5.0(3) . . . . ? C9 C7 C12 Ca1 87.6(11) . . . . ? C14 C7 C12 Ca1 -92.9(11) . . . . ? O4 Ca1 C12 O6 -94.88(14) 2_665 . . . ? O2 Ca1 C12 O6 88.08(14) 2_565 . . . ? O5 Ca1 C12 O6 -176.76(13) . . . . ? O16 Ca1 C12 O6 113.03(17) . . . . ? O1 Ca1 C12 O6 -171.3(2) . . . . ? O2 Ca1 C12 O6 20.95(14) . . . . ? O4 Ca1 C12 O6 -29.39(15) . . . . ? C13 Ca1 C12 O6 -0.84(15) . . . . ? Ca1 Ca1 C12 O6 53.57(13) 2_565 . . . ? Ca1 Ca1 C12 O6 -64.79(14) 2_665 . . . ? O4 Ca1 C12 O1 76.43(14) 2_665 . . . ? O2 Ca1 C12 O1 -100.60(14) 2_565 . . . ? O5 Ca1 C12 O1 -5.44(14) . . . . ? O16 Ca1 C12 O1 -75.66(19) . . . . ? O6 Ca1 C12 O1 171.3(2) . . . . ? O2 Ca1 C12 O1 -167.73(13) . . . . ? O4 Ca1 C12 O1 141.92(12) . . . . ? C13 Ca1 C12 O1 170.48(12) . . . . ? Ca1 Ca1 C12 O1 -135.11(13) 2_565 . . . ? Ca1 Ca1 C12 O1 106.53(13) 2_665 . . . ? O4 Ca1 C12 C7 168.7(11) 2_665 . . . ? O2 Ca1 C12 C7 -8.3(11) 2_565 . . . ? O5 Ca1 C12 C7 86.8(11) . . . . ? O16 Ca1 C12 C7 16.6(11) . . . . ? O1 Ca1 C12 C7 92.3(11) . . . . ? O6 Ca1 C12 C7 -96.4(11) . . . . ? O2 Ca1 C12 C7 -75.4(11) . . . . ? O4 Ca1 C12 C7 -125.8(11) . . . . ? C13 Ca1 C12 C7 -97.2(11) . . . . ? Ca1 Ca1 C12 C7 -42.8(11) 2_565 . . . ? Ca1 Ca1 C12 C7 -161.2(11) 2_665 . . . ? Ca1 O2 C13 O4 142.7(2) 2_565 . . . ? Ca1 O2 C13 O4 5.9(2) . . . . ? Ca1 O2 C13 C8 -37.1(4) 2_565 . . . ? Ca1 O2 C13 C8 -173.94(17) . . . . ? Ca1 O2 C13 Ca1 136.8(3) 2_565 . . . ? Ca1 O4 C13 O2 130.7(2) 2_665 . . . ? Ca1 O4 C13 O2 -5.8(2) . . . . ? Ca1 O4 C13 C8 -49.5(4) 2_665 . . . ? Ca1 O4 C13 C8 173.98(17) . . . . ? Ca1 O4 C13 Ca1 136.5(3) 2_665 . . . ? C11 C8 C13 O2 -47.2(3) . . . . ? C14 C8 C13 O2 132.1(2) 1_554 . . . ? C11 C8 C13 O4 133.0(2) . . . . ? C14 C8 C13 O4 -47.7(3) 1_554 . . . ? C11 C8 C13 Ca1 -129.0(15) . . . . ? C14 C8 C13 Ca1 50.3(16) 1_554 . . . ? O4 Ca1 C13 O2 151.72(13) 2_665 . . . ? O2 Ca1 C13 O2 -21.24(16) 2_565 . . . ? O5 Ca1 C13 O2 -129.08(14) . . . . ? O16 Ca1 C13 O2 -95.98(14) . . . . ? O1 Ca1 C13 O2 64.47(16) . . . . ? O6 Ca1 C13 O2 57.07(13) . . . . ? O4 Ca1 C13 O2 174.3(2) . . . . ? C12 Ca1 C13 O2 57.44(14) . . . . ? Ca1 Ca1 C13 O2 -14.65(11) 2_565 . . . ? Ca1 Ca1 C13 O2 158.84(15) 2_665 . . . ? O4 Ca1 C13 O4 -22.62(16) 2_665 . . . ? O2 Ca1 C13 O4 164.42(14) 2_565 . . . ? O5 Ca1 C13 O4 56.58(17) . . . . ? O16 Ca1 C13 O4 89.68(14) . . . . ? O1 Ca1 C13 O4 -109.87(15) . . . . ? O6 Ca1 C13 O4 -117.26(14) . . . . ? O2 Ca1 C13 O4 -174.3(2) . . . . ? C12 Ca1 C13 O4 -116.89(14) . . . . ? Ca1 Ca1 C13 O4 171.01(15) 2_565 . . . ? Ca1 Ca1 C13 O4 -15.50(11) 2_665 . . . ? O4 Ca1 C13 C8 -123.5(16) 2_665 . . . ? O2 Ca1 C13 C8 63.5(16) 2_565 . . . ? O5 Ca1 C13 C8 -44.3(16) . . . . ? O16 Ca1 C13 C8 -11.2(16) . . . . ? O1 Ca1 C13 C8 149.2(15) . . . . ? O6 Ca1 C13 C8 141.8(16) . . . . ? O2 Ca1 C13 C8 84.8(16) . . . . ? O4 Ca1 C13 C8 -100.9(16) . . . . ? C12 Ca1 C13 C8 142.2(16) . . . . ? Ca1 Ca1 C13 C8 70.1(16) 2_565 . . . ? Ca1 Ca1 C13 C8 -116.4(16) 2_665 . . . ? C9 C7 C14 C8 -2.0(3) . . . 1_556 ? C12 C7 C14 C8 178.53(19) . . . 1_556 ? C7 C9 C15 C11 0.5(3) . . . 1_556 ? C7 C9 C15 C10 -178.49(19) . . . 1_445 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.24 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.342 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.068 data_Ca-BTC _database_code_depnum_ccdc_archive 'CCDC 885046' #TrackingRef 'Ca-BTC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ca-BTC _chemical_melting_point ? _chemical_formula_moiety 'C6 H2 Ca O4' _chemical_formula_sum 'C6 H2 Ca O4' _chemical_formula_weight 178.16 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' Ca Ca 0.2262 0.3064 '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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 8.9636(3) _cell_length_b 8.9636(3) _cell_length_c 19.2832(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1341.76(10) _cell_formula_units_Z 9 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 810 _exptl_absorpt_coefficient_mu 1.000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.861 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1049 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 28.92 _reflns_number_total 795 _reflns_number_gt 580 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+2.8251P] 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 795 _refine_ls_number_parameters 51 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 -0.3333 0.3333 0.00637(4) 0.0140(3) Uani 1 3 d S . . Ca2 Ca 0.3333 0.6667 0.1667 0.0135(3) Uani 1 6 d S . . O1 O -0.1176(2) 0.3314(2) 0.06511(11) 0.0215(5) Uani 1 1 d . . . O3 O 0.1637(2) 0.4653(2) 0.08464(9) 0.0168(4) Uani 1 1 d . . . C5 C 0.1588(3) 0.1508(3) 0.08937(13) 0.0138(5) Uani 1 1 d . . . H5 H 0.2651 0.2518 0.0898 0.017 Uiso 1 1 calc R . . C8 C 0.0079(3) 0.1596(3) 0.08906(13) 0.0134(5) Uani 1 1 d . . . C11 C 0.0162(3) 0.3300(3) 0.07955(13) 0.0141(5) 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 0.0087(3) 0.0087(3) 0.0248(5) 0.000 0.000 0.00434(15) Ca2 0.0092(4) 0.0092(4) 0.0221(6) 0.000 0.000 0.00458(19) O1 0.0131(9) 0.0152(9) 0.0384(11) -0.0005(8) -0.0055(8) 0.0087(8) O3 0.0108(9) 0.0071(9) 0.0290(10) -0.0009(7) -0.0029(7) 0.0019(7) C5 0.0103(12) 0.0103(11) 0.0194(12) -0.0010(9) -0.0006(9) 0.0041(10) C8 0.0131(12) 0.0093(11) 0.0178(12) 0.0000(9) -0.0009(9) 0.0056(10) C11 0.0113(12) 0.0116(12) 0.0197(12) 0.0010(9) 0.0010(9) 0.0058(10) _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 2.2489(18) . ? Ca1 O1 2.2489(18) 2_565 ? Ca1 O1 2.2489(18) 3_455 ? Ca1 O3 2.4300(19) 12 ? Ca1 O3 2.4300(19) 10_565 ? Ca1 O3 2.4300(19) 11_455 ? Ca1 Ca2 3.3367(9) 7_444 ? Ca2 O3 2.3081(17) . ? Ca2 O3 2.3081(17) 3_565 ? Ca2 O3 2.3081(17) 2_665 ? Ca2 O3 2.3081(17) 15 ? Ca2 O3 2.3082(17) 13_565 ? Ca2 O3 2.3082(17) 14_455 ? Ca2 Ca1 3.3366(9) 10_565 ? Ca2 Ca1 3.3367(9) 4 ? O1 C11 1.237(3) . ? O3 C11 1.275(3) . ? O3 Ca1 2.4300(19) 10_565 ? C5 C8 1.392(3) 3 ? C5 C8 1.394(3) . ? C5 H5 0.9300 . ? C8 C5 1.392(3) 2 ? C8 C11 1.503(3) . ? 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 96.86(7) . 2_565 ? O1 Ca1 O1 96.86(7) . 3_455 ? O1 Ca1 O1 96.86(7) 2_565 3_455 ? O1 Ca1 O3 89.35(6) . 12 ? O1 Ca1 O3 162.58(7) 2_565 12 ? O1 Ca1 O3 98.54(6) 3_455 12 ? O1 Ca1 O3 98.54(6) . 10_565 ? O1 Ca1 O3 89.35(6) 2_565 10_565 ? O1 Ca1 O3 162.58(7) 3_455 10_565 ? O3 Ca1 O3 73.60(7) 12 10_565 ? O1 Ca1 O3 162.58(7) . 11_455 ? O1 Ca1 O3 98.54(6) 2_565 11_455 ? O1 Ca1 O3 89.35(6) 3_455 11_455 ? O3 Ca1 O3 73.60(7) 12 11_455 ? O3 Ca1 O3 73.60(7) 10_565 11_455 ? O1 Ca1 Ca2 120.24(6) . 7_444 ? O1 Ca1 Ca2 120.25(6) 2_565 7_444 ? O1 Ca1 Ca2 120.25(6) 3_455 7_444 ? O3 Ca1 Ca2 43.77(4) 12 7_444 ? O3 Ca1 Ca2 43.77(4) 10_565 7_444 ? O3 Ca1 Ca2 43.77(4) 11_455 7_444 ? O3 Ca2 O3 78.20(7) . 3_565 ? O3 Ca2 O3 78.20(7) . 2_665 ? O3 Ca2 O3 78.20(7) 3_565 2_665 ? O3 Ca2 O3 101.80(7) . 15 ? O3 Ca2 O3 180.0 3_565 15 ? O3 Ca2 O3 101.80(7) 2_665 15 ? O3 Ca2 O3 180.00(9) . 13_565 ? O3 Ca2 O3 101.80(7) 3_565 13_565 ? O3 Ca2 O3 101.80(7) 2_665 13_565 ? O3 Ca2 O3 78.20(7) 15 13_565 ? O3 Ca2 O3 101.80(7) . 14_455 ? O3 Ca2 O3 101.80(7) 3_565 14_455 ? O3 Ca2 O3 180.0 2_665 14_455 ? O3 Ca2 O3 78.20(7) 15 14_455 ? O3 Ca2 O3 78.20(7) 13_565 14_455 ? O3 Ca2 Ca1 46.74(4) . 10_565 ? O3 Ca2 Ca1 46.74(4) 3_565 10_565 ? O3 Ca2 Ca1 46.74(4) 2_665 10_565 ? O3 Ca2 Ca1 133.26(4) 15 10_565 ? O3 Ca2 Ca1 133.26(4) 13_565 10_565 ? O3 Ca2 Ca1 133.26(4) 14_455 10_565 ? O3 Ca2 Ca1 133.26(4) . 4 ? O3 Ca2 Ca1 133.26(4) 3_565 4 ? O3 Ca2 Ca1 133.26(4) 2_665 4 ? O3 Ca2 Ca1 46.74(4) 15 4 ? O3 Ca2 Ca1 46.74(4) 13_565 4 ? O3 Ca2 Ca1 46.74(4) 14_455 4 ? Ca1 Ca2 Ca1 180.0 10_565 4 ? C11 O1 Ca1 162.77(19) . . ? C11 O3 Ca2 139.54(16) . . ? C11 O3 Ca1 128.10(16) . 10_565 ? Ca2 O3 Ca1 89.49(6) . 10_565 ? C8 C5 C8 120.6(2) 3 . ? C8 C5 H5 119.7 3 . ? C8 C5 H5 119.7 . . ? C5 C8 C5 119.4(2) 2 . ? C5 C8 C11 120.0(2) 2 . ? C5 C8 C11 120.1(2) . . ? O1 C11 O3 123.9(2) . . ? O1 C11 C8 118.8(2) . . ? O3 C11 C8 117.2(2) . . ? 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 O1 Ca1 O1 C11 -131.3(6) 2_565 . . . ? O1 Ca1 O1 C11 130.9(6) 3_455 . . . ? O3 Ca1 O1 C11 32.4(6) 12 . . . ? O3 Ca1 O1 C11 -40.9(6) 10_565 . . . ? O3 Ca1 O1 C11 20.7(7) 11_455 . . . ? Ca2 Ca1 O1 C11 -0.2(6) 7_444 . . . ? O3 Ca2 O3 C11 -120.0(3) 3_565 . . . ? O3 Ca2 O3 C11 159.7(3) 2_665 . . . ? O3 Ca2 O3 C11 60.0(3) 15 . . . ? O3 Ca2 O3 C11 26.4(15) 13_565 . . . ? O3 Ca2 O3 C11 -20.3(3) 14_455 . . . ? Ca1 Ca2 O3 C11 -160.1(3) 10_565 . . . ? Ca1 Ca2 O3 C11 19.8(3) 4 . . . ? O3 Ca2 O3 Ca1 40.11(2) 3_565 . . 10_565 ? O3 Ca2 O3 Ca1 -40.11(2) 2_665 . . 10_565 ? O3 Ca2 O3 Ca1 -139.89(2) 15 . . 10_565 ? O3 Ca2 O3 Ca1 -173.4(15) 13_565 . . 10_565 ? O3 Ca2 O3 Ca1 139.89(2) 14_455 . . 10_565 ? Ca1 Ca2 O3 Ca1 180.0 4 . . 10_565 ? C8 C5 C8 C5 0.9(5) 3 . . 2 ? C8 C5 C8 C11 -171.61(16) 3 . . . ? Ca1 O1 C11 O3 86.7(6) . . . . ? Ca1 O1 C11 C8 -90.7(6) . . . . ? Ca2 O3 C11 O1 88.4(3) . . . . ? Ca1 O3 C11 O1 -66.1(3) 10_565 . . . ? Ca2 O3 C11 C8 -94.2(3) . . . . ? Ca1 O3 C11 C8 111.4(2) 10_565 . . . ? C5 C8 C11 O1 -7.3(4) 2 . . . ? C5 C8 C11 O1 165.2(2) . . . . ? C5 C8 C11 O3 175.1(2) 2 . . . ? C5 C8 C11 O3 -12.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.857 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.410 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.095