# 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 'Shaowu Du' _publ_contact_author_address ; Fuzhou Fujian China 350002 ; _publ_contact_author_email swdu@fjirsm.ac.cn loop_ _publ_author_name 'Jian-Di Lin' 'Shu-Ting Wu' 'Zhi-Hua Li' 'Shaowu Du' # Attachment '- CIFs.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 759707' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H22 Ca Cd N2 O10' _chemical_formula_sum 'C22 H22 Ca Cd N2 O10' _chemical_formula_weight 626.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 19.131(5) _cell_length_b 19.226(5) _cell_length_c 7.1899(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2644.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6589 _cell_measurement_theta_min 3.0034 _cell_measurement_theta_max 27.4797 _exptl_crystal_description strip-shaped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.074 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7570 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _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 Monochromator' _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14302 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 23.99 _reflns_number_total 4133 _reflns_number_gt 3926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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. Some bonds were restrained to more standard values by dfix command, they are as follows: dfix N1 C19 1.3 dfix N1 C19' 1.4 dfix c18 c19' 2.2 ; _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^)+(0.0314P)^2^+0.9631P] 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 0.00(3) _refine_ls_number_reflns 4133 _refine_ls_number_parameters 335 _refine_ls_number_restraints 514 _refine_ls_R_factor_all 0.0281 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.067 _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 Cd1 Cd 0.245582(12) 0.300700(10) 0.66330(7) 0.02864(8) Uani 1 1 d . . . Ca1 Ca 0.23236(4) 0.35977(3) 1.13047(10) 0.02794(18) Uani 1 1 d . . . O1 O 0.67840(13) 0.22268(13) 0.9370(4) 0.0401(6) Uani 1 1 d . . . O2 O 0.62309(12) 0.23452(14) 0.6718(5) 0.0492(7) Uani 1 1 d . . . O3 O 0.37560(14) 0.30775(17) 0.6642(6) 0.0665(9) Uani 1 1 d . . . O4 O 0.31998(13) 0.32547(14) 0.9244(4) 0.0437(7) Uani 1 1 d . . . O5 O 0.25726(13) 0.26842(13) 1.3334(4) 0.0358(7) Uani 1 1 d . . . O6 O 0.26508(17) 0.19069(14) 1.5548(4) 0.0459(8) Uani 1 1 d . . . O7 O 0.27879(16) -0.09056(13) 1.1016(4) 0.0494(8) Uani 1 1 d . . . O8 O 0.28972(19) -0.06121(14) 1.3990(5) 0.0572(8) Uani 1 1 d . . . O9 O 0.31471(18) 0.43586(17) 1.2451(5) 0.0684(10) Uani 1 1 d . A . O10 O 0.12290(15) 0.38948(16) 1.2446(5) 0.0566(8) Uani 1 1 d . . . N1 N 0.3797(3) 0.5148(3) 1.3911(8) 0.0909(16) Uani 0.50 1 d PD A 1 C19 C 0.4200(9) 0.5257(13) 1.559(2) 0.147(5) Uani 0.73(4) 1 d PDU A 1 H19A H 0.4190 0.4842 1.6336 0.220 Uiso 0.73(4) 1 calc PR A 1 H19B H 0.4002 0.5635 1.6288 0.220 Uiso 0.73(4) 1 calc PR A 1 H19C H 0.4674 0.5366 1.5272 0.220 Uiso 0.73(4) 1 calc PR A 1 N1' N 0.3797(3) 0.5148(3) 1.3911(8) 0.0909(16) Uani 0.50 1 d P A 2 C19' C 0.402(3) 0.5574(18) 1.538(3) 0.118(6) Uani 0.27(4) 1 d PDU A 2 H19D H 0.4100 0.5294 1.6463 0.178 Uiso 0.27(4) 1 calc PR A 2 H19E H 0.3660 0.5911 1.5650 0.178 Uiso 0.27(4) 1 calc PR A 2 H19F H 0.4440 0.5810 1.5035 0.178 Uiso 0.27(4) 1 calc PR A 2 N2 N 0.0132(2) 0.3940(2) 1.3519(7) 0.0677(11) Uani 1 1 d . . . C1 C 0.6245(2) 0.23859(19) 0.8460(6) 0.0355(9) Uani 1 1 d U . . C2 C 0.3757(2) 0.31281(19) 0.8353(6) 0.0378(8) Uani 1 1 d U . . C3 C 0.56203(19) 0.26421(18) 0.9488(5) 0.0343(8) Uani 1 1 d U . . C4 C 0.56326(19) 0.27361(19) 1.1401(7) 0.0422(8) Uani 1 1 d U . . H4 H 0.6042 0.2651 1.2061 0.051 Uiso 1 1 calc R . . C5 C 0.5042(2) 0.2955(2) 1.2331(6) 0.0484(10) Uani 1 1 d U . . H5 H 0.5054 0.3014 1.3614 0.058 Uiso 1 1 calc R . . C6 C 0.4436(2) 0.30842(18) 1.1359(7) 0.0434(9) Uani 1 1 d U . . H6 H 0.4037 0.3226 1.1995 0.052 Uiso 1 1 calc R . . C7 C 0.4413(2) 0.30052(17) 0.9441(6) 0.0345(8) Uani 1 1 d U . . C8 C 0.50105(19) 0.27877(19) 0.8523(6) 0.0342(8) Uani 1 1 d U . . H8 H 0.5002 0.2738 0.7236 0.041 Uiso 1 1 calc R . . C9 C 0.2669(2) 0.20635(19) 1.3869(6) 0.0320(8) Uani 1 1 d U . . C10 C 0.2863(2) -0.0470(2) 1.2317(6) 0.0411(9) Uani 1 1 d U . . C11 C 0.2812(2) 0.15049(19) 1.2488(6) 0.0327(9) Uani 1 1 d U . . C12 C 0.2961(2) 0.1655(2) 1.0651(6) 0.0383(9) Uani 1 1 d U . . H12 H 0.2971 0.2117 1.0272 0.046 Uiso 1 1 calc R . . C13 C 0.3096(2) 0.11411(19) 0.9358(6) 0.0408(8) Uani 1 1 d U . . H13 H 0.3209 0.1257 0.8139 0.049 Uiso 1 1 calc R . . C14 C 0.3061(2) 0.04527(19) 0.9900(6) 0.0389(9) Uani 1 1 d U . . H14 H 0.3139 0.0102 0.9032 0.047 Uiso 1 1 calc R . . C15 C 0.29099(17) 0.02788(15) 1.1747(6) 0.0327(7) Uani 1 1 d U . . C16 C 0.2797(2) 0.08034(19) 1.3025(5) 0.0337(8) Uani 1 1 d U . . H16 H 0.2709 0.0690 1.4260 0.040 Uiso 1 1 calc R . . C17 C 0.3501(3) 0.4537(3) 1.3756(8) 0.0704(13) Uani 1 1 d U . . H17 H 0.3569 0.4219 1.4714 0.084 Uiso 1 1 calc R A 1 C18 C 0.3692(4) 0.5665(4) 1.2468(13) 0.134(3) Uani 1 1 d DU . . H18A H 0.3411 0.5471 1.1492 0.201 Uiso 1 1 calc R A 1 H18B H 0.4137 0.5803 1.1972 0.201 Uiso 1 1 calc R A 1 H18C H 0.3460 0.6063 1.2984 0.201 Uiso 1 1 calc R A 1 C20 C 0.0802(2) 0.3837(2) 1.3686(7) 0.0542(11) Uani 1 1 d U . . H20 H 0.0968 0.3708 1.4853 0.065 Uiso 1 1 calc R . . C21 C -0.0351(3) 0.3810(4) 1.5087(11) 0.119(3) Uani 1 1 d U . . H21A H -0.0087 0.3720 1.6195 0.178 Uiso 1 1 calc R . . H21B H -0.0639 0.3415 1.4808 0.178 Uiso 1 1 calc R . . H21C H -0.0642 0.4211 1.5274 0.178 Uiso 1 1 calc R . . C22 C -0.0170(3) 0.4094(4) 1.1738(12) 0.128(3) Uani 1 1 d U . . H22A H 0.0196 0.4179 1.0853 0.192 Uiso 1 1 calc R . . H22B H -0.0460 0.4500 1.1838 0.192 Uiso 1 1 calc R . . H22C H -0.0448 0.3707 1.1331 0.192 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 Cd1 0.03286(14) 0.02379(12) 0.02926(14) -0.00029(16) -0.00027(15) 0.00126(9) Ca1 0.0290(3) 0.0217(3) 0.0332(5) 0.0045(3) -0.0008(4) 0.0008(2) O1 0.0283(15) 0.0401(14) 0.0519(18) 0.0019(14) -0.0057(13) 0.0081(12) O2 0.0353(13) 0.0664(17) 0.0460(17) -0.005(2) 0.0002(18) 0.0124(12) O3 0.0402(15) 0.111(3) 0.0484(19) -0.012(2) -0.014(2) 0.0219(15) O4 0.0289(14) 0.0441(15) 0.0582(19) 0.0046(15) 0.0054(14) 0.0025(12) O5 0.0581(18) 0.0219(13) 0.0276(15) -0.0001(11) -0.0027(12) 0.0067(11) O6 0.081(2) 0.0292(15) 0.0277(18) 0.0046(12) 0.0052(15) 0.0111(14) O7 0.0614(19) 0.0274(14) 0.059(2) 0.0029(14) 0.0082(15) -0.0055(13) O8 0.084(2) 0.0355(15) 0.0517(19) 0.0151(14) 0.0006(19) -0.0086(16) O9 0.070(2) 0.068(2) 0.067(2) -0.0245(18) -0.0016(19) -0.0244(17) O10 0.0446(17) 0.067(2) 0.058(2) -0.0068(16) 0.0056(16) 0.0071(15) N1 0.081(3) 0.075(3) 0.117(4) -0.024(3) -0.019(3) -0.024(3) C19 0.145(9) 0.131(10) 0.165(9) -0.051(8) -0.068(7) -0.017(8) N1' 0.081(3) 0.075(3) 0.117(4) -0.024(3) -0.019(3) -0.024(3) C19' 0.126(12) 0.086(11) 0.144(11) -0.044(11) -0.023(11) -0.027(11) N2 0.043(2) 0.087(3) 0.073(3) 0.003(2) 0.000(2) 0.011(2) C1 0.032(2) 0.0311(17) 0.043(2) 0.0010(16) -0.0005(17) 0.0005(15) C2 0.0352(19) 0.0354(17) 0.043(2) 0.0028(16) 0.0034(16) 0.0027(15) C3 0.0307(18) 0.0357(18) 0.0364(19) -0.0004(16) -0.0022(16) 0.0041(15) C4 0.0386(18) 0.0493(18) 0.039(2) -0.003(2) -0.0085(19) 0.0081(15) C5 0.048(2) 0.059(2) 0.0380(19) -0.0031(16) -0.0009(17) 0.0110(17) C6 0.0403(17) 0.0503(17) 0.040(2) 0.0014(18) 0.0043(18) 0.0092(14) C7 0.0312(17) 0.0332(17) 0.0391(18) 0.0020(15) -0.0012(16) 0.0029(14) C8 0.0324(18) 0.0367(17) 0.0336(18) 0.0009(16) 0.0006(15) 0.0035(15) C9 0.0358(18) 0.0286(17) 0.0315(19) 0.0011(14) -0.0015(16) 0.0015(14) C10 0.043(2) 0.0290(18) 0.052(2) 0.0039(18) 0.0033(18) -0.0033(17) C11 0.0398(19) 0.0266(17) 0.0316(18) 0.0059(15) -0.0001(16) 0.0035(15) C12 0.050(2) 0.0300(17) 0.0349(18) 0.0035(15) 0.0000(17) 0.0057(17) C13 0.057(2) 0.0330(16) 0.0325(17) 0.0063(16) 0.0042(17) 0.0049(16) C14 0.055(2) 0.0279(17) 0.0341(19) -0.0023(15) 0.0028(18) 0.0010(17) C15 0.0355(16) 0.0250(14) 0.0374(18) 0.0049(18) -0.0006(19) 0.0001(13) C16 0.042(2) 0.0273(17) 0.0318(19) 0.0065(16) 0.0020(17) -0.0019(16) C17 0.066(3) 0.063(3) 0.081(3) -0.005(3) 0.000(3) -0.013(2) C18 0.128(5) 0.099(5) 0.175(6) 0.017(5) -0.020(5) -0.026(4) C20 0.045(3) 0.061(3) 0.057(3) 0.007(2) -0.003(2) 0.009(2) C21 0.072(4) 0.154(6) 0.129(6) 0.015(5) 0.044(4) 0.008(4) C22 0.075(4) 0.184(7) 0.125(6) 0.037(6) -0.017(5) 0.023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O7 2.187(3) 4_554 ? Cd1 O6 2.285(3) 1_554 ? Cd1 O1 2.393(3) 3_455 ? Cd1 O4 2.403(3) . ? Cd1 O2 2.440(2) 3_455 ? Cd1 O5 2.462(3) 1_554 ? Cd1 O3 2.491(3) . ? Cd1 C9 2.722(4) 1_554 ? Cd1 Ca1 3.5547(12) . ? Ca1 O8 2.293(3) 4_554 ? Ca1 O9 2.302(3) . ? Ca1 O10 2.321(3) . ? Ca1 O5 2.332(3) . ? Ca1 O4 2.333(3) . ? Ca1 O1 2.348(3) 3_455 ? O1 C1 1.260(4) . ? O1 Ca1 2.348(3) 3 ? O1 Cd1 2.393(3) 3 ? O2 C1 1.255(5) . ? O2 Cd1 2.440(2) 3 ? O3 C2 1.234(6) . ? O4 C2 1.268(5) . ? O5 C9 1.267(4) . ? O5 Cd1 2.462(3) 1_556 ? O6 C9 1.244(5) . ? O6 Cd1 2.285(3) 1_556 ? O7 C10 1.264(5) . ? O7 Cd1 2.187(3) 4_545 ? O8 C10 1.235(5) . ? O8 Ca1 2.293(3) 4_545 ? O9 C17 1.207(6) . ? O10 C20 1.214(5) . ? N1 C17 1.309(6) . ? N1 C19 1.450(12) . ? N1 C18 1.450(9) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C19' H19D 0.9600 . ? C19' H19E 0.9600 . ? C19' H19F 0.9600 . ? N2 C20 1.304(6) . ? N2 C22 1.436(9) . ? N2 C21 1.478(8) . ? C1 C3 1.488(5) . ? C2 C7 1.498(5) . ? C3 C8 1.386(5) . ? C3 C4 1.388(6) . ? C4 C5 1.378(6) . ? C4 H4 0.9300 . ? C5 C6 1.378(6) . ? C5 H5 0.9300 . ? C6 C7 1.388(6) . ? C6 H6 0.9300 . ? C7 C8 1.384(5) . ? C8 H8 0.9300 . ? C9 C11 1.488(6) . ? C9 Cd1 2.722(4) 1_556 ? C10 C15 1.499(5) . ? C11 C12 1.382(5) . ? C11 C16 1.403(5) . ? C12 C13 1.381(5) . ? C12 H12 0.9300 . ? C13 C14 1.381(5) . ? C13 H13 0.9300 . ? C14 C15 1.399(6) . ? C14 H14 0.9300 . ? C15 C16 1.382(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C20 H20 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 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 O7 Cd1 O6 148.23(12) 4_554 1_554 ? O7 Cd1 O1 103.40(11) 4_554 3_455 ? O6 Cd1 O1 101.23(10) 1_554 3_455 ? O7 Cd1 O4 95.46(10) 4_554 . ? O6 Cd1 O4 110.70(10) 1_554 . ? O1 Cd1 O4 73.33(10) 3_455 . ? O7 Cd1 O2 93.76(10) 4_554 3_455 ? O6 Cd1 O2 84.75(11) 1_554 3_455 ? O1 Cd1 O2 53.94(11) 3_455 3_455 ? O4 Cd1 O2 127.17(11) . 3_455 ? O7 Cd1 O5 93.73(10) 4_554 1_554 ? O6 Cd1 O5 54.75(9) 1_554 1_554 ? O1 Cd1 O5 142.53(9) 3_455 1_554 ? O4 Cd1 O5 138.47(9) . 1_554 ? O2 Cd1 O5 92.38(11) 3_455 1_554 ? O7 Cd1 O3 99.29(11) 4_554 . ? O6 Cd1 O3 83.58(11) 1_554 . ? O1 Cd1 O3 122.98(13) 3_455 . ? O4 Cd1 O3 52.83(12) . . ? O2 Cd1 O3 166.90(10) 3_455 . ? O5 Cd1 O3 85.73(12) 1_554 . ? O7 Cd1 C9 121.40(12) 4_554 1_554 ? O6 Cd1 C9 27.02(11) 1_554 1_554 ? O1 Cd1 C9 123.77(10) 3_455 1_554 ? O4 Cd1 C9 127.85(10) . 1_554 ? O2 Cd1 C9 88.71(11) 3_455 1_554 ? O5 Cd1 C9 27.73(10) 1_554 1_554 ? O3 Cd1 C9 83.59(12) . 1_554 ? O7 Cd1 Ca1 82.59(9) 4_554 . ? O6 Cd1 Ca1 129.05(7) 1_554 . ? O1 Cd1 Ca1 40.95(6) 3_455 . ? O4 Cd1 Ca1 40.61(7) . . ? O2 Cd1 Ca1 89.80(9) 3_455 . ? O5 Cd1 Ca1 175.84(6) 1_554 . ? O3 Cd1 Ca1 92.94(10) . . ? C9 Cd1 Ca1 156.01(8) 1_554 . ? O8 Ca1 O9 88.00(13) 4_554 . ? O8 Ca1 O10 85.84(12) 4_554 . ? O9 Ca1 O10 109.54(12) . . ? O8 Ca1 O5 172.16(11) 4_554 . ? O9 Ca1 O5 96.59(12) . . ? O10 Ca1 O5 98.54(11) . . ? O8 Ca1 O4 81.86(11) 4_554 . ? O9 Ca1 O4 85.14(11) . . ? O10 Ca1 O4 160.53(12) . . ? O5 Ca1 O4 92.16(10) . . ? O8 Ca1 O1 86.34(11) 4_554 3_455 ? O9 Ca1 O1 160.36(12) . 3_455 ? O10 Ca1 O1 88.79(11) . 3_455 ? O5 Ca1 O1 87.25(10) . 3_455 ? O4 Ca1 O1 75.45(11) . 3_455 ? O8 Ca1 Cd1 62.54(9) 4_554 . ? O9 Ca1 Cd1 119.51(9) . . ? O10 Ca1 Cd1 118.49(8) . . ? O5 Ca1 Cd1 109.63(7) . . ? O4 Ca1 Cd1 42.12(7) . . ? O1 Ca1 Cd1 41.91(7) 3_455 . ? C1 O1 Ca1 146.3(2) . 3 ? C1 O1 Cd1 93.4(2) . 3 ? Ca1 O1 Cd1 97.14(9) 3 3 ? C1 O2 Cd1 91.3(2) . 3 ? C2 O3 Cd1 90.5(3) . . ? C2 O4 Ca1 168.5(3) . . ? C2 O4 Cd1 93.8(3) . . ? Ca1 O4 Cd1 97.27(9) . . ? C9 O5 Ca1 158.2(3) . . ? C9 O5 Cd1 87.6(2) . 1_556 ? Ca1 O5 Cd1 113.22(10) . 1_556 ? C9 O6 Cd1 96.4(2) . 1_556 ? C10 O7 Cd1 120.5(3) . 4_545 ? C10 O8 Ca1 147.5(3) . 4_545 ? C17 O9 Ca1 147.4(4) . . ? C20 O10 Ca1 147.6(3) . . ? C17 N1 C19 115.5(11) . . ? C17 N1 C18 119.7(6) . . ? C19 N1 C18 124.8(11) . . ? N1 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? H19D C19' H19E 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? C20 N2 C22 120.6(5) . . ? C20 N2 C21 121.3(5) . . ? C22 N2 C21 117.6(5) . . ? O2 C1 O1 121.4(4) . . ? O2 C1 C3 119.9(3) . . ? O1 C1 C3 118.7(3) . . ? O3 C2 O4 121.1(4) . . ? O3 C2 C7 120.7(4) . . ? O4 C2 C7 118.1(4) . . ? C8 C3 C4 119.0(4) . . ? C8 C3 C1 119.6(3) . . ? C4 C3 C1 121.4(3) . . ? C5 C4 C3 120.4(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 120.0(4) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.6(4) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 118.8(4) . . ? C8 C7 C2 119.3(4) . . ? C6 C7 C2 121.8(4) . . ? C7 C8 C3 121.1(4) . . ? C7 C8 H8 119.4 . . ? C3 C8 H8 119.4 . . ? O6 C9 O5 121.2(4) . . ? O6 C9 C11 118.5(3) . . ? O5 C9 C11 120.3(4) . . ? O6 C9 Cd1 56.5(2) . 1_556 ? O5 C9 Cd1 64.7(2) . 1_556 ? C11 C9 Cd1 174.8(3) . 1_556 ? O8 C10 O7 125.4(4) . . ? O8 C10 C15 118.4(4) . . ? O7 C10 C15 116.2(4) . . ? C12 C11 C16 117.9(4) . . ? C12 C11 C9 121.7(4) . . ? C16 C11 C9 120.4(4) . . ? C11 C12 C13 122.2(4) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C14 C13 C12 119.1(4) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 120.4(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 119.3(3) . . ? C16 C15 C10 120.6(4) . . ? C14 C15 C10 120.1(4) . . ? C15 C16 C11 121.0(3) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? O9 C17 N1 124.3(6) . . ? O9 C17 H17 117.9 . . ? N1 C17 H17 117.9 . . ? N1 C18 H18A 109.5 . . ? N1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O10 C20 N2 125.5(5) . . ? O10 C20 H20 117.3 . . ? N2 C20 H20 117.3 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.385 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.049 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 759708' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H36 Cd N6 O18 Sr2' _chemical_formula_weight 1032.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 17.4938(4) _cell_length_b 17.4938(4) _cell_length_c 13.2142(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4044.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11364 _cell_measurement_theta_min 3.0229 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 3.227 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6229 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _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 Monochromator' _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23212 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 23.98 _reflns_number_total 3120 _reflns_number_gt 3010 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0650P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(9) _refine_ls_number_reflns 3120 _refine_ls_number_parameters 249 _refine_ls_number_restraints 336 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.185 _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 Cd1 Cd 0.33480(2) 0.33480(2) 0.0000 0.03207(18) Uani 1 2 d S . . Sr1 Sr 0.36070(3) 0.88821(3) -0.19668(4) 0.03183(17) Uani 1 1 d . . . O1 O 0.3549(3) 0.4483(2) 0.0921(3) 0.0534(12) Uani 1 1 d . . . O2 O 0.2751(2) 0.4527(2) -0.0358(3) 0.0361(9) Uani 1 1 d . . . O3 O 0.2464(2) 0.8053(2) -0.1183(3) 0.0380(9) Uani 1 1 d . . . O4 O 0.1802(3) 0.7027(2) -0.1585(3) 0.0450(10) Uani 1 1 d . . . O5 O 0.3811(3) 1.0070(3) -0.3085(4) 0.0536(12) Uani 1 1 d . . . O6 O 0.4202(4) 0.7566(3) -0.1708(5) 0.0786(18) Uani 1 1 d . . . O7 O 0.3953(3) 0.8912(2) 0.0024(4) 0.0543(11) Uani 1 1 d . . . O8 O 0.3725(2) 1.0027(2) -0.0595(3) 0.0417(10) Uani 1 1 d . . . O9 O 0.4233(3) 0.9920(3) 0.0883(3) 0.0557(13) Uani 1 1 d . . . N1 N 0.4126(4) 1.1293(4) -0.3416(5) 0.0587(16) Uani 1 1 d . . . N2 N 0.5094(6) 0.6669(6) -0.1655(7) 0.127(4) Uani 1 1 d . . . N3 N 0.3975(3) 0.9621(3) 0.0118(4) 0.0378(11) Uani 1 1 d . . . C1 C 0.3134(4) 0.4846(3) 0.0336(4) 0.0393(12) Uani 1 1 d U . . C2 C 0.2292(4) 0.7363(3) -0.1057(4) 0.0376(12) Uani 1 1 d U . . C3 C 0.3105(4) 0.5710(3) 0.0414(4) 0.0384(12) Uani 1 1 d U . . C4 C 0.3517(4) 0.6083(4) 0.1166(5) 0.0478(13) Uani 1 1 d U . . H4 H 0.3793 0.5802 0.1639 0.057 Uiso 1 1 calc R . . C5 C 0.3515(4) 0.6860(4) 0.1209(5) 0.0522(14) Uani 1 1 d U . . H5 H 0.3777 0.7109 0.1726 0.063 Uiso 1 1 calc R . . C6 C 0.3121(4) 0.7289(4) 0.0481(5) 0.0441(13) Uani 1 1 d U . . H6 H 0.3138 0.7820 0.0496 0.053 Uiso 1 1 calc R . . C7 C 0.2703(4) 0.6911(3) -0.0265(4) 0.0356(12) Uani 1 1 d U . . C8 C 0.2698(3) 0.6124(3) -0.0289(4) 0.0350(11) Uani 1 1 d U . . H8 H 0.2417 0.5870 -0.0783 0.042 Uiso 1 1 calc R . . C9 C 0.4085(4) 1.0685(4) -0.2841(5) 0.0495(16) Uani 1 1 d U . . H9 H 0.4281 1.0725 -0.2189 0.059 Uiso 1 1 calc R . . C10 C 0.4442(6) 1.2003(5) -0.3054(8) 0.083(2) Uani 1 1 d U . . H10A H 0.4628 1.1935 -0.2376 0.124 Uiso 1 1 calc R . . H10B H 0.4053 1.2390 -0.3058 0.124 Uiso 1 1 calc R . . H10C H 0.4855 1.2157 -0.3486 0.124 Uiso 1 1 calc R . . C11 C 0.3848(7) 1.1274(6) -0.4431(7) 0.094(3) Uani 1 1 d U . . H11A H 0.3660 1.0771 -0.4582 0.142 Uiso 1 1 calc R . . H11B H 0.4255 1.1400 -0.4889 0.142 Uiso 1 1 calc R . . H11C H 0.3441 1.1638 -0.4505 0.142 Uiso 1 1 calc R . . C12 C 0.4678(6) 0.7152(6) -0.2053(8) 0.0818(18) Uani 1 1 d U . . H12 H 0.4748 0.7203 -0.2747 0.098 Uiso 1 1 calc R . . C13 C 0.5795(8) 0.6428(9) -0.1979(10) 0.124(3) Uani 1 1 d U . . H13A H 0.5831 0.6492 -0.2699 0.186 Uiso 1 1 calc R . . H13B H 0.5861 0.5899 -0.1812 0.186 Uiso 1 1 calc R . . H13C H 0.6186 0.6725 -0.1655 0.186 Uiso 1 1 calc R . . C14 C 0.5087(8) 0.6554(9) -0.0552(10) 0.128(3) Uani 1 1 d U . . H14A H 0.4605 0.6722 -0.0283 0.191 Uiso 1 1 calc R . . H14B H 0.5493 0.6844 -0.0249 0.191 Uiso 1 1 calc R . . H14C H 0.5156 0.6021 -0.0403 0.191 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 Cd1 0.0254(2) 0.0254(2) 0.0455(3) 0.00147(17) -0.00147(17) 0.0017(2) Sr1 0.0273(3) 0.0283(3) 0.0399(3) -0.0024(2) -0.0021(2) -0.0016(2) O1 0.070(3) 0.031(2) 0.060(3) 0.001(2) -0.032(2) 0.008(2) O2 0.039(2) 0.0209(19) 0.048(2) -0.0059(16) -0.0092(18) 0.0022(17) O3 0.037(2) 0.028(2) 0.049(2) 0.0074(17) -0.0048(18) -0.0034(18) O4 0.051(3) 0.036(2) 0.048(2) 0.0047(19) -0.018(2) -0.004(2) O5 0.056(3) 0.046(3) 0.060(3) 0.004(2) 0.006(2) -0.007(2) O6 0.085(4) 0.047(3) 0.103(4) 0.014(3) 0.024(3) 0.027(3) O7 0.074(3) 0.032(3) 0.056(3) 0.001(2) -0.003(2) -0.011(2) O8 0.045(2) 0.038(2) 0.042(2) 0.0011(19) -0.006(2) 0.0047(19) O9 0.087(4) 0.037(3) 0.043(2) -0.005(2) -0.026(2) 0.001(2) N1 0.060(4) 0.055(4) 0.061(4) 0.009(3) 0.005(3) -0.004(3) N2 0.146(8) 0.107(7) 0.128(7) 0.060(6) 0.074(7) 0.094(7) N3 0.041(3) 0.029(3) 0.044(3) -0.001(2) 0.001(2) -0.002(2) C1 0.045(3) 0.030(3) 0.044(3) 0.002(2) -0.002(2) 0.002(2) C2 0.044(3) 0.030(3) 0.039(2) 0.002(2) -0.002(2) -0.002(2) C3 0.046(3) 0.029(2) 0.041(2) -0.002(2) -0.004(2) -0.010(2) C4 0.061(3) 0.040(3) 0.043(3) 0.006(2) -0.014(2) -0.002(3) C5 0.067(3) 0.043(3) 0.046(3) -0.003(2) -0.014(3) -0.013(3) C6 0.058(3) 0.033(3) 0.041(2) -0.004(2) -0.007(2) -0.007(2) C7 0.042(3) 0.028(2) 0.037(2) 0.002(2) -0.001(2) -0.005(2) C8 0.041(3) 0.027(2) 0.037(2) 0.002(2) -0.002(2) -0.005(2) C9 0.050(4) 0.043(4) 0.056(4) 0.013(3) 0.004(3) 0.002(3) C10 0.088(6) 0.062(5) 0.098(6) 0.013(5) -0.004(5) -0.021(5) C11 0.139(8) 0.077(6) 0.067(5) 0.017(5) -0.006(5) -0.008(6) C12 0.094(4) 0.073(3) 0.079(3) 0.001(3) -0.005(3) 0.010(3) C13 0.123(7) 0.123(7) 0.126(6) 0.005(6) 0.008(6) -0.005(6) C14 0.133(6) 0.127(6) 0.123(6) 0.003(6) 0.006(6) 0.002(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 Cd1 O3 2.305(4) 5_544 ? Cd1 O3 2.305(4) 4_455 ? Cd1 O1 2.355(4) . ? Cd1 O1 2.355(4) 7 ? Cd1 O2 2.359(4) . ? Cd1 O2 2.359(4) 7 ? Cd1 O4 2.621(4) 5_544 ? Cd1 O4 2.621(4) 4_455 ? Cd1 C1 2.683(6) . ? Cd1 C1 2.683(6) 7 ? Cd1 Sr1 3.6148(6) 5_544 ? Cd1 Sr1 3.6148(6) 4_455 ? Sr1 O4 2.515(4) 8_664 ? Sr1 O6 2.550(5) . ? Sr1 O5 2.574(5) . ? Sr1 O2 2.640(4) 5_554 ? Sr1 O3 2.679(4) . ? Sr1 O9 2.688(5) 3_654 ? Sr1 O7 2.700(5) . ? Sr1 O8 2.709(4) . ? Sr1 O8 2.830(4) 3_654 ? Sr1 N3 3.111(5) . ? Sr1 N3 3.152(5) 3_654 ? Sr1 Cd1 3.6148(6) 3_554 ? O1 C1 1.235(7) . ? O2 C1 1.266(7) . ? O2 Sr1 2.640(4) 5_544 ? O3 C2 1.254(7) . ? O3 Cd1 2.305(4) 3_554 ? O4 C2 1.253(7) . ? O4 Sr1 2.515(4) 8_664 ? O4 Cd1 2.621(4) 3_554 ? O5 C9 1.221(8) . ? O6 C12 1.194(11) . ? O7 N3 1.247(7) . ? O8 N3 1.258(6) . ? O8 Sr1 2.830(4) 4_465 ? O9 N3 1.224(7) . ? O9 Sr1 2.688(5) 4_465 ? N1 C9 1.310(9) . ? N1 C11 1.427(11) . ? N1 C10 1.441(10) . ? N2 C12 1.233(12) . ? N2 C13 1.365(15) . ? N2 C14 1.472(16) . ? N3 Sr1 3.152(5) 4_465 ? C1 C3 1.516(8) . ? C2 C7 1.495(8) . ? C3 C8 1.377(8) . ? C3 C4 1.390(8) . ? C4 C5 1.361(9) . ? C4 H4 0.9300 . ? C5 C6 1.401(9) . ? C5 H5 0.9300 . ? C6 C7 1.395(8) . ? C6 H6 0.9300 . ? C7 C8 1.378(8) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 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 O3 Cd1 O3 107.1(2) 5_544 4_455 ? O3 Cd1 O1 132.14(14) 5_544 . ? O3 Cd1 O1 99.35(16) 4_455 . ? O3 Cd1 O1 99.35(16) 5_544 7 ? O3 Cd1 O1 132.14(14) 4_455 7 ? O1 Cd1 O1 90.9(3) . 7 ? O3 Cd1 O2 76.80(13) 5_544 . ? O3 Cd1 O2 126.23(14) 4_455 . ? O1 Cd1 O2 55.44(13) . . ? O1 Cd1 O2 97.99(15) 7 . ? O3 Cd1 O2 126.23(14) 5_544 7 ? O3 Cd1 O2 76.80(13) 4_455 7 ? O1 Cd1 O2 97.99(15) . 7 ? O1 Cd1 O2 55.44(13) 7 7 ? O2 Cd1 O2 144.46(19) . 7 ? O3 Cd1 O4 52.60(13) 5_544 5_544 ? O3 Cd1 O4 77.45(14) 4_455 5_544 ? O1 Cd1 O4 175.21(13) . 5_544 ? O1 Cd1 O4 88.70(17) 7 5_544 ? O2 Cd1 O4 129.33(13) . 5_544 ? O2 Cd1 O4 77.88(14) 7 5_544 ? O3 Cd1 O4 77.45(14) 5_544 4_455 ? O3 Cd1 O4 52.60(13) 4_455 4_455 ? O1 Cd1 O4 88.70(17) . 4_455 ? O1 Cd1 O4 175.21(13) 7 4_455 ? O2 Cd1 O4 77.88(14) . 4_455 ? O2 Cd1 O4 129.33(13) 7 4_455 ? O4 Cd1 O4 92.1(2) 5_544 4_455 ? O3 Cd1 C1 104.95(16) 5_544 . ? O3 Cd1 C1 116.43(17) 4_455 . ? O1 Cd1 C1 27.39(16) . . ? O1 Cd1 C1 93.30(19) 7 . ? O2 Cd1 C1 28.15(16) . . ? O2 Cd1 C1 121.36(17) 7 . ? O4 Cd1 C1 157.39(16) 5_544 . ? O4 Cd1 C1 84.17(16) 4_455 . ? O3 Cd1 C1 116.43(17) 5_544 7 ? O3 Cd1 C1 104.95(16) 4_455 7 ? O1 Cd1 C1 93.30(19) . 7 ? O1 Cd1 C1 27.39(16) 7 7 ? O2 Cd1 C1 121.36(17) . 7 ? O2 Cd1 C1 28.15(16) 7 7 ? O4 Cd1 C1 84.17(16) 5_544 7 ? O4 Cd1 C1 157.39(16) 4_455 7 ? C1 Cd1 C1 107.4(3) . 7 ? O3 Cd1 Sr1 47.77(10) 5_544 5_544 ? O3 Cd1 Sr1 95.42(10) 4_455 5_544 ? O1 Cd1 Sr1 91.36(11) . 5_544 ? O1 Cd1 Sr1 131.18(10) 7 5_544 ? O2 Cd1 Sr1 46.87(10) . 5_544 ? O2 Cd1 Sr1 168.66(10) 7 5_544 ? O4 Cd1 Sr1 92.48(10) 5_544 5_544 ? O4 Cd1 Sr1 44.08(9) 4_455 5_544 ? C1 Cd1 Sr1 69.40(13) . 5_544 ? C1 Cd1 Sr1 158.04(13) 7 5_544 ? O3 Cd1 Sr1 95.42(10) 5_544 4_455 ? O3 Cd1 Sr1 47.77(10) 4_455 4_455 ? O1 Cd1 Sr1 131.18(10) . 4_455 ? O1 Cd1 Sr1 91.36(11) 7 4_455 ? O2 Cd1 Sr1 168.66(10) . 4_455 ? O2 Cd1 Sr1 46.87(10) 7 4_455 ? O4 Cd1 Sr1 44.08(9) 5_544 4_455 ? O4 Cd1 Sr1 92.48(10) 4_455 4_455 ? C1 Cd1 Sr1 158.04(13) . 4_455 ? C1 Cd1 Sr1 69.40(13) 7 4_455 ? Sr1 Cd1 Sr1 121.81(2) 5_544 4_455 ? O4 Sr1 O6 81.51(19) 8_664 . ? O4 Sr1 O5 90.49(16) 8_664 . ? O6 Sr1 O5 138.52(17) . . ? O4 Sr1 O2 74.90(13) 8_664 5_554 ? O6 Sr1 O2 139.86(17) . 5_554 ? O5 Sr1 O2 74.34(14) . 5_554 ? O4 Sr1 O3 72.98(13) 8_664 . ? O6 Sr1 O3 76.32(17) . . ? O5 Sr1 O3 139.69(14) . . ? O2 Sr1 O3 66.00(12) 5_554 . ? O4 Sr1 O9 131.48(13) 8_664 3_654 ? O6 Sr1 O9 78.0(2) . 3_654 ? O5 Sr1 O9 77.37(17) . 3_654 ? O2 Sr1 O9 141.26(14) 5_554 3_654 ? O3 Sr1 O9 140.58(14) . 3_654 ? O4 Sr1 O7 148.16(15) 8_664 . ? O6 Sr1 O7 78.18(19) . . ? O5 Sr1 O7 120.83(14) . . ? O2 Sr1 O7 106.19(14) 5_554 . ? O3 Sr1 O7 78.53(14) . . ? O9 Sr1 O7 67.24(14) 3_654 . ? O4 Sr1 O8 153.43(13) 8_664 . ? O6 Sr1 O8 123.15(18) . . ? O5 Sr1 O8 77.12(14) . . ? O2 Sr1 O8 79.12(12) 5_554 . ? O3 Sr1 O8 101.42(13) . . ? O9 Sr1 O8 69.11(13) 3_654 . ? O7 Sr1 O8 46.89(13) . . ? O4 Sr1 O8 85.74(13) 8_664 3_654 ? O6 Sr1 O8 68.80(16) . 3_654 ? O5 Sr1 O8 70.07(13) . 3_654 ? O2 Sr1 O8 139.08(12) 5_554 3_654 ? O3 Sr1 O8 141.39(13) . 3_654 ? O9 Sr1 O8 45.85(12) 3_654 3_654 ? O7 Sr1 O8 109.00(14) . 3_654 ? O8 Sr1 O8 111.12(15) . 3_654 ? O4 Sr1 N3 164.35(14) 8_664 . ? O6 Sr1 N3 99.90(18) . . ? O5 Sr1 N3 98.30(14) . . ? O2 Sr1 N3 94.95(12) 5_554 . ? O3 Sr1 N3 92.12(13) . . ? O9 Sr1 N3 63.54(13) 3_654 . ? O7 Sr1 N3 23.45(13) . . ? O8 Sr1 N3 23.71(12) . . ? O8 Sr1 N3 109.39(12) 3_654 . ? O4 Sr1 N3 109.04(13) 8_664 3_654 ? O6 Sr1 N3 70.67(17) . 3_654 ? O5 Sr1 N3 73.86(14) . 3_654 ? O2 Sr1 N3 147.97(12) 5_554 3_654 ? O3 Sr1 N3 146.03(13) . 3_654 ? O9 Sr1 N3 22.44(13) 3_654 3_654 ? O7 Sr1 N3 87.01(15) . 3_654 ? O8 Sr1 N3 90.21(13) . 3_654 ? O8 Sr1 N3 23.50(12) 3_654 3_654 ? N3 Sr1 N3 85.93(15) . 3_654 ? O4 Sr1 Cd1 46.46(10) 8_664 3_554 ? O6 Sr1 Cd1 100.29(15) . 3_554 ? O5 Sr1 Cd1 103.18(11) . 3_554 ? O2 Sr1 Cd1 40.69(8) 5_554 3_554 ? O3 Sr1 Cd1 39.57(8) . 3_554 ? O9 Sr1 Cd1 177.72(10) 3_654 3_554 ? O7 Sr1 Cd1 114.03(11) . 3_554 ? O8 Sr1 Cd1 113.16(9) . 3_554 ? O8 Sr1 Cd1 132.16(8) 3_654 3_554 ? N3 Sr1 Cd1 118.42(9) . 3_554 ? N3 Sr1 Cd1 155.49(10) 3_654 3_554 ? C1 O1 Cd1 91.3(4) . . ? C1 O2 Cd1 90.3(3) . . ? C1 O2 Sr1 136.7(4) . 5_544 ? Cd1 O2 Sr1 92.44(13) . 5_544 ? C2 O3 Cd1 99.7(3) . 3_554 ? C2 O3 Sr1 138.7(4) . . ? Cd1 O3 Sr1 92.66(13) 3_554 . ? C2 O4 Sr1 163.2(4) . 8_664 ? C2 O4 Cd1 85.0(3) . 3_554 ? Sr1 O4 Cd1 89.46(13) 8_664 3_554 ? C9 O5 Sr1 127.9(4) . . ? C12 O6 Sr1 141.3(6) . . ? N3 O7 Sr1 97.1(3) . . ? N3 O8 Sr1 96.3(3) . . ? N3 O8 Sr1 92.8(3) . 4_465 ? Sr1 O8 Sr1 169.75(17) . 4_465 ? N3 O9 Sr1 100.6(3) . 4_465 ? C9 N1 C11 120.5(7) . . ? C9 N1 C10 121.9(7) . . ? C11 N1 C10 117.6(7) . . ? C12 N2 C13 127.4(11) . . ? C12 N2 C14 120.7(10) . . ? C13 N2 C14 106.1(11) . . ? O9 N3 O7 121.3(5) . . ? O9 N3 O8 120.3(5) . . ? O7 N3 O8 118.4(5) . . ? O9 N3 Sr1 170.1(4) . . ? O7 N3 Sr1 59.5(3) . . ? O8 N3 Sr1 60.0(3) . . ? O9 N3 Sr1 57.0(3) . 4_465 ? O7 N3 Sr1 173.6(4) . 4_465 ? O8 N3 Sr1 63.7(3) . 4_465 ? Sr1 N3 Sr1 123.51(16) . 4_465 ? O1 C1 O2 122.5(6) . . ? O1 C1 C3 119.3(6) . . ? O2 C1 C3 118.1(5) . . ? O1 C1 Cd1 61.3(3) . . ? O2 C1 Cd1 61.5(3) . . ? C3 C1 Cd1 171.7(4) . . ? O4 C2 O3 122.7(5) . . ? O4 C2 C7 118.1(5) . . ? O3 C2 C7 119.1(5) . . ? C8 C3 C4 120.2(5) . . ? C8 C3 C1 119.7(5) . . ? C4 C3 C1 120.0(5) . . ? C5 C4 C3 119.9(6) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.5(6) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 119.3(6) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C8 C7 C6 119.5(6) . . ? C8 C7 C2 120.6(5) . . ? C6 C7 C2 119.8(5) . . ? C3 C8 C7 120.5(5) . . ? C3 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? O5 C9 N1 125.8(7) . . ? O5 C9 H9 117.1 . . ? N1 C9 H9 117.1 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O6 C12 N2 131.7(10) . . ? O6 C12 H12 114.2 . . ? N2 C12 H12 114.2 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 23.98 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.557 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.085 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 759709' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H12 Ca Cd O12, 2(C2 H7 N)' _chemical_formula_sum 'C16 H12 Ca Cd O12' _chemical_formula_weight 548.74 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' 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-4c2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x, -y, z+1/2' '-x, y, z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1' '-x+1/2, y+1/2, z+1' 'y+1/2, x+1/2, -z+1' '-y+1/2, -x+1/2, -z+1' _cell_length_a 19.6226(4) _cell_length_b 19.6226(4) _cell_length_c 14.2086(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5471.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7799 _cell_measurement_theta_min 3.2214 _cell_measurement_theta_max 27.4680 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7346 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _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 Monochromator' _diffrn_measurement_device_type CCD_Profile_fitting _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20086 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0164 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3119 _reflns_number_gt 3035 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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. There are solvent accessible voids in the structure. This problem, as most of the MOFs with voids usually have, can not be solved after several refinements. ; _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^)+(0.0623P)^2^+11.2160P] 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 0.01(4) _refine_ls_number_reflns 3119 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Cd1 Cd -0.267766(10) 0.232234(10) 0.0000 0.02265(11) Uani 1 2 d S . . Ca1 Ca -0.79746(3) 0.20254(3) -0.2500 0.0248(2) Uani 1 2 d S . . O1 O -0.34116(13) 0.22991(14) -0.1262(2) 0.0298(6) Uani 1 1 d . . . O2 O -0.39717(13) 0.22086(16) 0.0063(3) 0.0392(6) Uani 1 1 d . . . O3 O -0.65550(15) 0.26864(17) -0.0359(2) 0.0403(8) Uani 1 1 d . . . O4 O -0.70288(14) 0.22128(19) -0.1603(2) 0.0430(8) Uani 1 1 d . . . O5 O -0.5046(2) 0.1753(2) -0.3797(2) 0.0600(10) Uani 1 1 d . . . H5 H -0.5362 0.1906 -0.4110 0.090 Uiso 1 1 calc R . . O6W O -0.8857(2) 0.1743(3) -0.3516(5) 0.0976(18) Uani 1 1 d . . . H6WB H -0.9212 0.1521 -0.3363 0.117 Uiso 1 1 d R . . H6WA H -0.8770 0.1894 -0.4063 0.146 Uiso 1 1 d R . . C1 C -0.39670(19) 0.2224(2) -0.0818(2) 0.0276(7) Uani 1 1 d . . . C2 C -0.65189(19) 0.2385(2) -0.1149(3) 0.0306(8) Uani 1 1 d . . . C3 C -0.46075(18) 0.2167(2) -0.1379(3) 0.0294(7) Uani 1 1 d . . . C4 C -0.4554(2) 0.1974(2) -0.2326(3) 0.0350(9) Uani 1 1 d . . . H4 H -0.4129 0.1877 -0.2583 0.042 Uiso 1 1 calc R . . C5 C -0.5133(2) 0.1927(2) -0.2878(3) 0.0368(9) Uani 1 1 d . . . C6 C -0.57678(19) 0.2060(2) -0.2493(3) 0.0349(8) Uani 1 1 d . . . H6 H -0.6157 0.2019 -0.2862 0.042 Uiso 1 1 calc R . . C7 C -0.58237(19) 0.2256(2) -0.1551(3) 0.0301(8) Uani 1 1 d . . . C8 C -0.5241(2) 0.2303(2) -0.0992(3) 0.0323(8) Uani 1 1 d . . . H8 H -0.5278 0.2425 -0.0361 0.039 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 Cd1 0.02537(13) 0.02537(13) 0.01720(16) 0.00298(11) -0.00298(11) -0.00418(10) Ca1 0.0287(3) 0.0287(3) 0.0169(4) -0.0019(3) 0.0019(3) -0.0002(4) O1 0.0174(11) 0.0496(18) 0.0224(12) 0.0060(9) -0.0018(10) -0.0056(10) O2 0.0251(11) 0.0749(18) 0.0176(13) 0.0003(16) -0.0034(13) -0.0048(11) O3 0.0236(14) 0.062(2) 0.0350(14) -0.0093(13) 0.0110(12) 0.0024(12) O4 0.0189(13) 0.074(2) 0.0360(14) -0.0016(14) -0.0016(11) 0.0011(14) O5 0.0374(16) 0.122(3) 0.0210(14) -0.0128(17) -0.0062(12) 0.019(2) O6W 0.055(2) 0.125(4) 0.113(4) -0.038(4) -0.022(3) -0.026(3) C1 0.0223(17) 0.0411(19) 0.0194(17) 0.0015(14) -0.0013(13) -0.0021(14) C2 0.0188(16) 0.046(2) 0.0274(18) 0.0039(14) 0.0016(14) 0.0029(13) C3 0.0221(16) 0.047(2) 0.0187(16) 0.0019(15) -0.0019(13) -0.0037(15) C4 0.0223(16) 0.064(3) 0.0191(17) 0.0032(16) 0.0051(12) 0.0017(17) C5 0.0286(19) 0.064(3) 0.0178(15) -0.0036(17) -0.0010(14) 0.0067(18) C6 0.0239(16) 0.060(2) 0.0212(16) 0.0011(18) -0.0040(16) 0.0009(16) C7 0.0188(16) 0.047(2) 0.0241(17) 0.0010(14) 0.0007(13) 0.0010(14) C8 0.0247(18) 0.053(2) 0.0189(17) 0.0004(15) -0.0012(14) 0.0002(15) _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 Cd1 O3 2.261(3) 4_565 ? Cd1 O3 2.261(3) 13_554 ? Cd1 O1 2.301(3) . ? Cd1 O1 2.301(3) 15_454 ? Cd1 O2 2.551(3) . ? Cd1 O2 2.551(3) 15_454 ? Cd1 Ca1 3.8204(4) 4_565 ? Cd1 Ca1 3.8204(4) 11_444 ? Ca1 O4 2.282(3) . ? Ca1 O4 2.282(3) 7_464 ? Ca1 O6W 2.321(5) . ? Ca1 O6W 2.321(5) 7_464 ? Ca1 O1 2.363(3) 13_454 ? Ca1 O1 2.363(3) 12_454 ? Ca1 Cd1 3.8204(4) 3_455 ? Ca1 Cd1 3.8204(4) 12_454 ? Ca1 H6WA 2.7266 . ? O1 C1 1.268(4) . ? O1 Ca1 2.363(3) 11_444 ? O2 C1 1.252(5) . ? O3 C2 1.271(5) . ? O3 Cd1 2.261(3) 3_455 ? O4 C2 1.237(5) . ? O5 C5 1.362(5) . ? O5 H5 0.8200 . ? O6W H6WB 0.8500 . ? O6W H6WA 0.8500 . ? C1 C3 1.493(5) . ? C2 C7 1.501(5) . ? C3 C8 1.385(5) . ? C3 C4 1.402(5) . ? C4 C5 1.384(6) . ? C4 H4 0.9300 . ? C5 C6 1.385(5) . ? C6 C7 1.396(6) . ? C6 H6 0.9300 . ? C7 C8 1.396(5) . ? C8 H8 0.9300 . ? 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 O3 Cd1 O3 93.76(17) 4_565 13_554 ? O3 Cd1 O1 100.97(11) 4_565 . ? O3 Cd1 O1 115.72(11) 13_554 . ? O3 Cd1 O1 115.72(11) 4_565 15_454 ? O3 Cd1 O1 100.97(11) 13_554 15_454 ? O1 Cd1 O1 125.66(13) . 15_454 ? O3 Cd1 O2 94.00(11) 4_565 . ? O3 Cd1 O2 167.72(12) 13_554 . ? O1 Cd1 O2 53.30(11) . . ? O1 Cd1 O2 84.16(11) 15_454 . ? O3 Cd1 O2 167.72(12) 4_565 15_454 ? O3 Cd1 O2 94.00(11) 13_554 15_454 ? O1 Cd1 O2 84.16(11) . 15_454 ? O1 Cd1 O2 53.30(11) 15_454 15_454 ? O2 Cd1 O2 80.03(14) . 15_454 ? O3 Cd1 Ca1 86.65(8) 4_565 4_565 ? O3 Cd1 Ca1 83.23(9) 13_554 4_565 ? O1 Cd1 Ca1 158.68(7) . 4_565 ? O1 Cd1 Ca1 35.54(7) 15_454 4_565 ? O2 Cd1 Ca1 106.72(9) . 4_565 ? O2 Cd1 Ca1 84.84(9) 15_454 4_565 ? O3 Cd1 Ca1 83.23(9) 4_565 11_444 ? O3 Cd1 Ca1 86.65(8) 13_554 11_444 ? O1 Cd1 Ca1 35.54(7) . 11_444 ? O1 Cd1 Ca1 158.68(7) 15_454 11_444 ? O2 Cd1 Ca1 84.84(9) . 11_444 ? O2 Cd1 Ca1 106.72(9) 15_454 11_444 ? Ca1 Cd1 Ca1 165.171(8) 4_565 11_444 ? O4 Ca1 O4 92.88(18) . 7_464 ? O4 Ca1 O6W 173.08(17) . . ? O4 Ca1 O6W 88.11(18) 7_464 . ? O4 Ca1 O6W 88.11(18) . 7_464 ? O4 Ca1 O6W 173.08(17) 7_464 7_464 ? O6W Ca1 O6W 91.7(3) . 7_464 ? O4 Ca1 O1 77.81(10) . 13_454 ? O4 Ca1 O1 91.04(11) 7_464 13_454 ? O6W Ca1 O1 109.03(16) . 13_454 ? O6W Ca1 O1 82.47(17) 7_464 13_454 ? O4 Ca1 O1 91.04(11) . 12_454 ? O4 Ca1 O1 77.81(10) 7_464 12_454 ? O6W Ca1 O1 82.47(17) . 12_454 ? O6W Ca1 O1 109.03(16) 7_464 12_454 ? O1 Ca1 O1 163.90(14) 13_454 12_454 ? O4 Ca1 Cd1 45.76(8) . 3_455 ? O4 Ca1 Cd1 102.86(8) 7_464 3_455 ? O6W Ca1 Cd1 140.53(15) . 3_455 ? O6W Ca1 Cd1 73.03(16) 7_464 3_455 ? O1 Ca1 Cd1 34.47(6) 13_454 3_455 ? O1 Ca1 Cd1 136.71(8) 12_454 3_455 ? O4 Ca1 Cd1 102.86(8) . 12_454 ? O4 Ca1 Cd1 45.76(8) 7_464 12_454 ? O6W Ca1 Cd1 73.03(16) . 12_454 ? O6W Ca1 Cd1 140.53(15) 7_464 12_454 ? O1 Ca1 Cd1 136.71(8) 13_454 12_454 ? O1 Ca1 Cd1 34.47(6) 12_454 12_454 ? Cd1 Ca1 Cd1 139.67(3) 3_455 12_454 ? O4 Ca1 H6WA 159.4 . . ? O4 Ca1 H6WA 73.4 7_464 . ? O6W Ca1 H6WA 17.1 . . ? O6W Ca1 H6WA 107.4 7_464 . ? O1 Ca1 H6WA 116.8 13_454 . ? O1 Ca1 H6WA 71.4 12_454 . ? Cd1 Ca1 H6WA 151.2 3_455 . ? Cd1 Ca1 H6WA 56.5 12_454 . ? C1 O1 Cd1 98.8(2) . . ? C1 O1 Ca1 138.4(2) . 11_444 ? Cd1 O1 Ca1 109.99(10) . 11_444 ? C1 O2 Cd1 87.5(2) . . ? C2 O3 Cd1 104.5(3) . 3_455 ? C2 O4 Ca1 173.2(3) . . ? C5 O5 H5 109.5 . . ? Ca1 O6W H6WB 125.1 . . ? Ca1 O6W H6WA 109.6 . . ? H6WB O6W H6WA 125.3 . . ? O2 C1 O1 120.4(3) . . ? O2 C1 C3 121.7(3) . . ? O1 C1 C3 117.8(3) . . ? O4 C2 O3 122.8(4) . . ? O4 C2 C7 119.4(4) . . ? O3 C2 C7 117.8(4) . . ? C8 C3 C4 120.1(3) . . ? C8 C3 C1 121.9(3) . . ? C4 C3 C1 118.0(3) . . ? C5 C4 C3 120.0(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? O5 C5 C4 117.2(4) . . ? O5 C5 C6 122.6(4) . . ? C4 C5 C6 120.2(4) . . ? C5 C6 C7 120.0(3) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 120.0(4) . . ? C8 C7 C2 121.1(4) . . ? C6 C7 C2 118.9(3) . . ? C3 C8 C7 119.7(4) . . ? C3 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.464 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.108 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 759710' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H48 Ca Cd2 O16, 2(C2 H8 N)' _chemical_formula_sum 'C52 H64 Ca Cd2 N2 O16' _chemical_formula_weight 1237.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' _cell_length_a 19.8227(6) _cell_length_b 19.8227(6) _cell_length_c 9.9593(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3913.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9394 _cell_measurement_theta_min 3.0733 _cell_measurement_theta_max 27.4758 _exptl_crystal_description needle-shaped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.051 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7351 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _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 Monochromator' _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22309 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 23.99 _reflns_number_total 3204 _reflns_number_gt 2952 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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. There are solvent accessible voids in the structure. This problem, as most of the MOFs with voids usually have, can not be solved after several refinements. Some bonds and angles were restrained to more standard values by dfix command, they are as follows: dfix c10 c11 1.5 dfix c10 c12 1.5 dfix c10 c12' 1.35 dfix c10 c11' 1.6 dfix c17 c18 1.5 dfix c17 c19 1.5 dfix c12 c12' 1.6 dfix c11 c11' 1.5 dfix c8 c12 2.4 dfix c8 c11' 2.35 dfix c8 c12' 2.8 dfix c16 c19 2.3 dfix c18 c19 2.35 dfix c18 c16 2.55 dfix n1 c20 1.4 dfix n1 c21 1.45 ; _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^)+(0.1224P)^2^+11.5902P] 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 3204 _refine_ls_number_parameters 218 _refine_ls_number_restraints 190 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1851 _refine_ls_wR_factor_gt 0.1790 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.097 _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 Cd1 Cd 0.07081(3) -0.34248(3) 0.0000 0.0318(3) Uani 1 2 d S . . Ca1 Ca 0.0000 -0.5000 0.0000 0.0273(5) Uani 1 4 d S . . O1 O 0.3959(3) -0.0481(3) 0.0000 0.0588(18) Uani 1 2 d S . . O2 O 0.2869(3) -0.0329(3) 0.0000 0.0476(15) Uani 1 2 d S . . O3 O 0.1874(3) -0.3398(3) 0.0000 0.0548(16) Uani 1 2 d S . . O4 O 0.1387(3) -0.2419(3) 0.0000 0.0614(19) Uani 1 2 d S . . O5 O 0.0737(2) -0.4463(2) 0.1440(4) 0.0504(11) Uani 1 1 d . . . O6 O 0.0699(2) -0.3474(2) 0.2419(5) 0.0547(13) Uani 1 1 d . . . N1 N 0.329(2) -0.7647(17) 0.5000 0.29(3) Uani 1 2 d SD . . H1A H 0.3612 -0.7899 0.5393 0.348 Uiso 0.50 1 d PR . . H1B H 0.3265 -0.7246 0.5420 0.348 Uiso 0.50 1 d PR . . C1 C 0.3374(4) -0.0710(4) 0.0000 0.0400(18) Uani 1 2 d SU . . C2 C 0.1904(4) -0.2775(5) 0.0000 0.046(2) Uani 1 2 d SU . . C3 C 0.0752(3) -0.4102(3) 0.2489(6) 0.0425(13) Uani 1 1 d U . . C4 C 0.3291(4) -0.1459(4) 0.0000 0.0389(16) Uani 1 2 d SU . . C5 C 0.2641(4) -0.1746(4) 0.0000 0.0408(17) Uani 1 2 d SU . . H5 H 0.2258 -0.1474 0.0000 0.049 Uiso 1 2 calc SR . . C6 C 0.2586(4) -0.2442(4) 0.0000 0.0436(18) Uani 1 2 d SU . . C7 C 0.3170(4) -0.2835(4) 0.0000 0.049(2) Uani 1 2 d SU . . H7 H 0.3130 -0.3303 0.0000 0.058 Uiso 1 2 calc SR . . C8 C 0.3801(4) -0.2555(4) 0.0000 0.0550(19) Uani 1 2 d SDU . . C9 C 0.3856(4) -0.1864(4) 0.0000 0.0449(18) Uani 1 2 d SU . . H9 H 0.4281 -0.1666 0.0000 0.054 Uiso 1 2 calc SR . . C10 C 0.4454(5) -0.3009(5) 0.0000 0.071(2) Uani 0.50 2 d SPDU . 1 C10' C 0.4454(5) -0.3009(5) 0.0000 0.071(2) Uani 0.50 2 d SPU . 2 C11 C 0.4867(9) -0.2822(10) -0.1255(16) 0.101(5) Uani 0.50 1 d PDU . 1 H11A H 0.5269 -0.3091 -0.1285 0.151 Uiso 0.50 1 calc PR . 1 H11B H 0.4987 -0.2353 -0.1217 0.151 Uiso 0.50 1 calc PR . 1 H11C H 0.4602 -0.2905 -0.2045 0.151 Uiso 0.50 1 calc PR . 1 C12 C 0.4255(12) -0.3723(7) 0.0000 0.088(5) Uani 0.50 2 d SPDU . 1 H12A H 0.4651 -0.4002 0.0000 0.132 Uiso 0.50 2 calc SPR . 1 H12B H 0.3991 -0.3817 -0.0787 0.132 Uiso 0.25 1 calc PR . 1 H12C H 0.3991 -0.3817 0.0787 0.132 Uiso 0.25 1 calc PR . 1 C11' C 0.5048(8) -0.2558(12) 0.0000 0.093(5) Uani 0.50 2 d SPDU . 2 H11D H 0.5452 -0.2824 0.0000 0.140 Uiso 0.50 2 calc SPR . 2 H11E H 0.5038 -0.2279 0.0787 0.140 Uiso 0.25 1 calc PR . 2 H11F H 0.5038 -0.2279 -0.0787 0.140 Uiso 0.25 1 calc PR . 2 C12' C 0.4470(10) -0.3454(9) -0.1290(17) 0.108(5) Uani 0.50 1 d PDU . 2 H12D H 0.4868 -0.3730 -0.1284 0.162 Uiso 0.50 1 calc PR . 2 H12E H 0.4474 -0.3170 -0.2070 0.162 Uiso 0.50 1 calc PR . 2 H12F H 0.4077 -0.3738 -0.1311 0.162 Uiso 0.50 1 calc PR . 2 C13 C 0.0776(4) -0.4103(4) 0.5000 0.0411(18) Uani 1 2 d SU . . H13 H 0.0661 -0.3648 0.5000 0.049 Uiso 1 2 calc SR . . C14 C 0.0861(3) -0.4442(3) 0.3794(6) 0.0412(12) Uani 1 1 d U . . C15 C 0.1049(3) -0.5120(3) 0.3806(6) 0.0453(14) Uani 1 1 d U . . H15 H 0.1105 -0.5343 0.2992 0.054 Uiso 1 1 calc R . . C16 C 0.1155(5) -0.5477(4) 0.5000 0.051(2) Uani 1 2 d SDU . . C17 C 0.1426(6) -0.6187(6) 0.5000 0.068(3) Uani 1 2 d SDU . . C18 C 0.2180(7) -0.6180(10) 0.5000 0.155(7) Uani 1 2 d SDU . . H18A H 0.2345 -0.6635 0.5000 0.233 Uiso 1 2 calc SR . . H18B H 0.2339 -0.5950 0.5787 0.233 Uiso 0.50 1 calc PR . . H18C H 0.2339 -0.5950 0.4213 0.233 Uiso 0.50 1 calc PR . . C19 C 0.1193(9) -0.6559(5) 0.6169(13) 0.145(5) Uani 1 1 d DU . . H19A H 0.1372 -0.7009 0.6146 0.217 Uiso 1 1 calc R . . H19B H 0.0709 -0.6579 0.6164 0.217 Uiso 1 1 calc R . . H19C H 0.1343 -0.6336 0.6971 0.217 Uiso 1 1 calc R . . C20 C 0.342(2) -0.7573(13) 0.357(3) 0.196(19) Uani 0.50 1 d PD . . H20A H 0.3847 -0.7347 0.3444 0.294 Uiso 0.50 1 calc PR . . H20B H 0.3070 -0.7313 0.3164 0.294 Uiso 0.50 1 calc PR . . H20C H 0.3442 -0.8011 0.3159 0.294 Uiso 0.50 1 calc PR . . C21 C 0.264(2) -0.7981(16) 0.5000 0.22(2) Uani 1 2 d SD . . H21A H 0.2505 -0.8064 0.5909 0.336 Uiso 0.50 1 calc PR . . H21B H 0.2679 -0.8401 0.4528 0.336 Uiso 0.50 1 calc PR . . H21C H 0.2317 -0.7699 0.4564 0.336 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0290(4) 0.0300(4) 0.0364(4) 0.000 0.000 -0.00406(19) Ca1 0.0297(10) 0.0229(10) 0.0294(11) 0.000 0.000 0.0015(8) O1 0.036(3) 0.039(3) 0.101(6) 0.000 0.000 -0.013(3) O2 0.040(3) 0.033(3) 0.070(4) 0.000 0.000 -0.006(3) O3 0.045(3) 0.036(3) 0.084(5) 0.000 0.000 -0.012(3) O4 0.034(3) 0.043(3) 0.108(6) 0.000 0.000 -0.006(3) O5 0.057(3) 0.065(3) 0.029(2) -0.0071(19) -0.0060(18) -0.010(2) O6 0.075(3) 0.055(3) 0.035(3) 0.0043(19) -0.007(2) -0.006(2) N1 0.46(7) 0.20(3) 0.22(3) 0.000 0.000 0.25(4) C1 0.035(4) 0.038(4) 0.047(4) 0.000 0.000 -0.010(3) C2 0.038(4) 0.047(5) 0.053(5) 0.000 0.000 -0.009(4) C3 0.041(3) 0.054(4) 0.033(3) 0.003(3) 0.000(2) -0.010(2) C4 0.030(3) 0.034(3) 0.053(4) 0.000 0.000 -0.011(3) C5 0.029(3) 0.038(4) 0.055(4) 0.000 0.000 -0.003(3) C6 0.032(4) 0.035(4) 0.064(4) 0.000 0.000 -0.009(3) C7 0.036(4) 0.034(4) 0.077(5) 0.000 0.000 -0.004(3) C8 0.035(4) 0.041(4) 0.088(5) 0.000 0.000 0.003(3) C9 0.028(4) 0.039(4) 0.068(5) 0.000 0.000 -0.009(3) C10 0.038(4) 0.051(4) 0.124(6) 0.000 0.000 0.016(3) C10' 0.038(4) 0.051(4) 0.124(6) 0.000 0.000 0.016(3) C11 0.070(8) 0.076(8) 0.156(11) -0.003(8) 0.023(8) 0.026(7) C12 0.062(10) 0.052(9) 0.150(13) 0.000 0.000 0.023(8) C11' 0.045(9) 0.076(11) 0.159(13) 0.000 0.000 0.010(9) C12' 0.073(8) 0.089(9) 0.162(11) -0.016(9) 0.005(9) 0.028(8) C13 0.047(4) 0.039(4) 0.038(4) 0.000 0.000 -0.007(3) C14 0.043(3) 0.050(3) 0.030(3) -0.001(2) -0.002(2) -0.007(2) C15 0.053(3) 0.052(3) 0.031(3) -0.002(2) -0.002(2) -0.002(3) C16 0.058(5) 0.050(4) 0.045(4) 0.000 0.000 0.000(4) C17 0.086(6) 0.057(5) 0.061(5) 0.000 0.000 0.016(5) C18 0.139(13) 0.111(11) 0.216(18) 0.000 0.000 0.033(11) C19 0.248(14) 0.066(6) 0.120(9) 0.016(6) 0.045(10) 0.036(8) C20 0.22(4) 0.065(15) 0.31(6) -0.01(2) 0.04(4) 0.077(19) C21 0.26(4) 0.099(18) 0.32(5) 0.000 0.000 0.09(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.312(6) . ? Cd1 O2 2.331(6) 7 ? Cd1 O4 2.404(6) . ? Cd1 O6 2.412(5) 6 ? Cd1 O6 2.412(5) . ? Cd1 O5 2.509(5) 6 ? Cd1 O5 2.509(5) . ? Cd1 O1 2.584(6) 7 ? Cd1 C2 2.698(8) . ? Cd1 Ca1 3.4235(5) . ? Ca1 O1 2.274(6) 3_545 ? Ca1 O1 2.274(6) 7 ? Ca1 O5 2.307(4) 5_545 ? Ca1 O5 2.307(4) . ? Ca1 O5 2.307(4) 2_545 ? Ca1 O5 2.307(4) 6 ? Ca1 Cd1 3.4235(5) 5_545 ? O1 C1 1.245(10) . ? O1 Ca1 2.274(6) 3 ? O1 Cd1 2.584(6) 3 ? O2 C1 1.253(10) . ? O2 Cd1 2.331(6) 3 ? O3 C2 1.236(11) . ? O4 C2 1.244(11) . ? O5 C3 1.266(7) . ? O6 C3 1.252(8) . ? N1 C21 1.44(2) . ? N1 C20 1.46(2) 6_556 ? N1 C20 1.46(2) . ? N1 H1A 0.8999 . ? N1 H1B 0.9000 . ? C1 C4 1.494(11) . ? C2 C6 1.504(11) . ? C3 C14 1.480(8) . ? C4 C9 1.379(12) . ? C4 C5 1.408(11) . ? C5 C6 1.385(12) . ? C5 H5 0.9300 . ? C6 C7 1.396(12) . ? C7 C8 1.368(12) . ? C7 H7 0.9300 . ? C8 C9 1.374(12) . ? C8 C10 1.577(12) . ? C9 H9 0.9300 . ? C10 C12 1.470(16) . ? C10 C11 1.539(15) 6 ? C10 C11 1.539(15) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C11' H11D 0.9600 . ? C11' H11E 0.9600 . ? C11' H11F 0.9600 . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? C13 C14 1.387(7) . ? C13 C14 1.387(7) 6_556 ? C13 H13 0.9300 . ? C14 C15 1.395(9) . ? C15 C16 1.400(8) . ? C15 H15 0.9300 . ? C16 C15 1.400(8) 6_556 ? C16 C17 1.506(14) . ? C17 C19 1.454(11) 6_556 ? C17 C19 1.454(11) . ? C17 C18 1.495(15) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 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 O3 Cd1 O2 150.5(2) . 7 ? O3 Cd1 O4 54.7(2) . . ? O2 Cd1 O4 95.8(2) 7 . ? O3 Cd1 O6 90.49(11) . 6 ? O2 Cd1 O6 90.71(11) 7 6 ? O4 Cd1 O6 92.17(11) . 6 ? O3 Cd1 O6 90.49(11) . . ? O2 Cd1 O6 90.71(11) 7 . ? O4 Cd1 O6 92.17(11) . . ? O6 Cd1 O6 175.3(2) 6 . ? O3 Cd1 O5 89.78(16) . 6 ? O2 Cd1 O5 114.05(16) 7 6 ? O4 Cd1 O5 131.85(14) . 6 ? O6 Cd1 O5 52.84(15) 6 6 ? O6 Cd1 O5 122.54(14) . 6 ? O3 Cd1 O5 89.78(16) . . ? O2 Cd1 O5 114.05(16) 7 . ? O4 Cd1 O5 131.85(14) . . ? O6 Cd1 O5 122.54(14) 6 . ? O6 Cd1 O5 52.84(15) . . ? O5 Cd1 O5 69.70(19) 6 . ? O3 Cd1 O1 157.15(19) . 7 ? O2 Cd1 O1 52.4(2) 7 7 ? O4 Cd1 O1 148.2(2) . 7 ? O6 Cd1 O1 88.65(11) 6 7 ? O6 Cd1 O1 88.65(11) . 7 ? O5 Cd1 O1 71.63(14) 6 7 ? O5 Cd1 O1 71.63(14) . 7 ? O3 Cd1 C2 27.2(2) . . ? O2 Cd1 C2 123.3(2) 7 . ? O4 Cd1 C2 27.5(2) . . ? O6 Cd1 C2 91.49(11) 6 . ? O6 Cd1 C2 91.49(11) . . ? O5 Cd1 C2 111.82(19) 6 . ? O5 Cd1 C2 111.82(19) . . ? O1 Cd1 C2 175.7(2) 7 . ? O3 Cd1 Ca1 115.54(15) . . ? O2 Cd1 Ca1 93.97(15) 7 . ? O4 Cd1 Ca1 170.19(15) . . ? O6 Cd1 Ca1 87.70(11) 6 . ? O6 Cd1 Ca1 87.70(11) . . ? O5 Cd1 Ca1 42.37(9) 6 . ? O5 Cd1 Ca1 42.37(9) . . ? O1 Cd1 Ca1 41.62(13) 7 . ? C2 Cd1 Ca1 142.7(2) . . ? O1 Ca1 O1 180.0 3_545 7 ? O1 Ca1 O5 81.19(17) 3_545 5_545 ? O1 Ca1 O5 98.81(17) 7 5_545 ? O1 Ca1 O5 98.81(17) 3_545 . ? O1 Ca1 O5 81.19(17) 7 . ? O5 Ca1 O5 180.0 5_545 . ? O1 Ca1 O5 81.19(17) 3_545 2_545 ? O1 Ca1 O5 98.81(17) 7 2_545 ? O5 Ca1 O5 76.8(2) 5_545 2_545 ? O5 Ca1 O5 103.2(2) . 2_545 ? O1 Ca1 O5 98.81(17) 3_545 6 ? O1 Ca1 O5 81.19(17) 7 6 ? O5 Ca1 O5 103.2(2) 5_545 6 ? O5 Ca1 O5 76.8(2) . 6 ? O5 Ca1 O5 180.0 2_545 6 ? O1 Ca1 Cd1 49.01(16) 3_545 5_545 ? O1 Ca1 Cd1 130.99(16) 7 5_545 ? O5 Ca1 Cd1 47.12(11) 5_545 5_545 ? O5 Ca1 Cd1 132.88(11) . 5_545 ? O5 Ca1 Cd1 47.12(11) 2_545 5_545 ? O5 Ca1 Cd1 132.88(11) 6 5_545 ? O1 Ca1 Cd1 130.99(16) 3_545 . ? O1 Ca1 Cd1 49.01(16) 7 . ? O5 Ca1 Cd1 132.88(11) 5_545 . ? O5 Ca1 Cd1 47.12(11) . . ? O5 Ca1 Cd1 132.88(11) 2_545 . ? O5 Ca1 Cd1 47.12(11) 6 . ? Cd1 Ca1 Cd1 180.0 5_545 . ? C1 O1 Ca1 176.5(6) . 3 ? C1 O1 Cd1 87.2(5) . 3 ? Ca1 O1 Cd1 89.37(19) 3 3 ? C1 O2 Cd1 98.9(5) . 3 ? C2 O3 Cd1 94.1(5) . . ? C2 O4 Cd1 89.5(5) . . ? C3 O5 Ca1 142.0(4) . . ? C3 O5 Cd1 90.5(4) . . ? Ca1 O5 Cd1 90.51(14) . . ? C3 O6 Cd1 95.4(4) . . ? C21 N1 C20 102(3) . 6_556 ? C21 N1 C20 102(3) . . ? C20 N1 C20 156(5) 6_556 . ? C21 N1 H1A 112.0 . . ? C20 N1 H1A 60.2 6_556 . ? C20 N1 H1A 110.7 . . ? C21 N1 H1B 110.8 . . ? C20 N1 H1B 57.8 6_556 . ? C20 N1 H1B 112.1 . . ? H1A N1 H1B 109.3 . . ? O1 C1 O2 121.6(8) . . ? O1 C1 C4 117.7(8) . . ? O2 C1 C4 120.7(7) . . ? O3 C2 O4 121.7(8) . . ? O3 C2 C6 118.7(8) . . ? O4 C2 C6 119.5(8) . . ? O3 C2 Cd1 58.7(5) . . ? O4 C2 Cd1 63.0(4) . . ? C6 C2 Cd1 177.5(6) . . ? O6 C3 O5 120.9(6) . . ? O6 C3 C14 120.9(6) . . ? O5 C3 C14 118.1(5) . . ? C9 C4 C5 120.5(7) . . ? C9 C4 C1 119.3(7) . . ? C5 C4 C1 120.2(7) . . ? C6 C5 C4 118.3(8) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C5 C6 C7 119.4(7) . . ? C5 C6 C2 120.5(8) . . ? C7 C6 C2 120.1(7) . . ? C8 C7 C6 122.1(8) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C7 C8 C9 118.5(8) . . ? C7 C8 C10 121.2(8) . . ? C9 C8 C10 120.3(8) . . ? C8 C9 C4 121.1(7) . . ? C8 C9 H9 119.5 . . ? C4 C9 H9 119.5 . . ? C12 C10 C11 112.0(9) . 6 ? C12 C10 C11 112.0(9) . . ? C11 C10 C11 108.6(15) 6 . ? C12 C10 C8 109.2(10) . . ? C11 C10 C8 107.4(8) 6 . ? C11 C10 C8 107.4(8) . . ? 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 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? H11D C11' H11E 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? H12D C12' H12E 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? C14 C13 C14 120.0(8) . 6_556 ? C14 C13 H13 120.0 . . ? C14 C13 H13 120.0 6_556 . ? C13 C14 C15 119.5(6) . . ? C13 C14 C3 121.5(6) . . ? C15 C14 C3 119.0(5) . . ? C14 C15 C16 122.3(6) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C15 C16 C15 116.4(8) . 6_556 ? C15 C16 C17 121.7(4) . . ? C15 C16 C17 121.7(4) 6_556 . ? C19 C17 C19 106.4(14) 6_556 . ? C19 C17 C18 108.8(9) 6_556 . ? C19 C17 C18 108.8(9) . . ? C19 C17 C16 111.2(7) 6_556 . ? C19 C17 C16 111.2(7) . . ? C18 C17 C16 110.3(11) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 H20A 109.5 . . ? N1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 H21A 109.5 . . ? N1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.358 _refine_diff_density_min -1.017 _refine_diff_density_rms 0.122 #===END