data_global data_squeeze #TrackingRef '18496_web_deposit_cif_file_0_PatriciaHorcajada_1363104284.Ca2(azbz-TC)(DMF)(H2O).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ca2(azbz-TC)(DMF)(H2O) _chemical_melting_point ? _chemical_formula_moiety C19H15Ca2N3O10 _chemical_formula_sum 'C19 H15 Ca2 N3 O10' _chemical_formula_weight 525.50 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1119(5) _cell_length_b 11.0499(8) _cell_length_c 12.7808(8) _cell_angle_alpha 101.472(6) _cell_angle_beta 102.024(4) _cell_angle_gamma 108.351(5) _cell_volume 1270.77(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6587 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.04 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 0.502 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9609 _exptl_absorpt_correction_T_max 0.9900 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.709622 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Beamline BM1A, SNBL, ESRF, Grenoble, France' _diffrn_radiation_monochromator 'Si (111)' _diffrn_measurement_device_type 'MAR345 Image plate' _diffrn_measurement_method \f-scan _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8751 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4101 _reflns_number_gt 3764 _reflns_threshold_expression >2\s(I) _computing_data_collection 'MAR345 control software (MAR, 2002)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis (Oxford Diffraction, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0992P)^2^+4.6908P] 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 4101 _refine_ls_number_parameters 301 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1976 _refine_ls_wR_factor_gt 0.1949 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.069 _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 0.33118(8) 0.25761(7) 0.86540(6) 0.0184(3) Uani 1 1 d . . . Ca2 Ca 0.19995(8) 0.10208(8) 0.56701(7) 0.0243(3) Uani 1 1 d . . . N1 N -0.0663(4) 0.4828(5) 0.9778(4) 0.0483(13) Uani 1 1 d . . . C1 C -0.1220(5) 0.3842(5) 0.8714(4) 0.0377(12) Uani 1 1 d . . . C2 C -0.0355(4) 0.3348(4) 0.8175(3) 0.0249(9) Uani 1 1 d . . . H2 H 0.0646 0.3663 0.8500 0.030 Uiso 1 1 calc R . . C3 C -0.0998(4) 0.2380(4) 0.7145(3) 0.0207(8) Uani 1 1 d . . . C4 C -0.2513(4) 0.1903(4) 0.6653(3) 0.0277(10) Uani 1 1 d . . . H4 H -0.2942 0.1249 0.5971 0.033 Uiso 1 1 calc R . . C5 C -0.3368(5) 0.2413(5) 0.7188(4) 0.0387(12) Uani 1 1 d . . . C6 C -0.2721(5) 0.3389(6) 0.8221(4) 0.0459(15) Uani 1 1 d . . . H6 H -0.3291 0.3735 0.8578 0.055 Uiso 1 1 calc R . . C7 C -0.0043(4) 0.1839(4) 0.6600(3) 0.0167(8) Uani 1 1 d . . . O1 O 0.1300(3) 0.2286(3) 0.7103(2) 0.0185(6) Uani 1 1 d . . . O2 O -0.0574(3) 0.0979(3) 0.5663(2) 0.0239(6) Uani 1 1 d . . . C8 C -0.4994(5) 0.1926(5) 0.6672(4) 0.0430(14) Uani 1 1 d . . . O3 O -0.5705(3) 0.2488(3) 0.7155(2) 0.0298(7) Uani 1 1 d . . . O4 O -0.5592(4) 0.0995(5) 0.5783(4) 0.0753(17) Uani 1 1 d . . . N11 N 0.0446(4) 0.4845(3) 0.5312(3) 0.0302(9) Uani 1 1 d . . . C11 C 0.2388(5) 0.8130(4) 0.7514(4) 0.0331(11) Uani 1 1 d . . . C12 C 0.1493(5) 0.7212(4) 0.6502(4) 0.0325(11) Uani 1 1 d . . . H12 H 0.1004 0.7482 0.5949 0.039 Uiso 1 1 calc R . . C13 C 0.1338(5) 0.5886(4) 0.6325(3) 0.0263(9) Uani 1 1 d . . . C14 C 0.2095(4) 0.5473(4) 0.7139(3) 0.0224(9) Uani 1 1 d . . . H14 H 0.2013 0.4590 0.7001 0.027 Uiso 1 1 calc R . . C15 C 0.2972(4) 0.6392(4) 0.8160(3) 0.0219(9) Uani 1 1 d . . . C16 C 0.3128(5) 0.7723(4) 0.8342(3) 0.0295(10) Uani 1 1 d . . . H16 H 0.3726 0.8342 0.9017 0.035 Uiso 1 1 calc R . . C17 C 0.3791(4) 0.5953(4) 0.9054(3) 0.0218(8) Uani 1 1 d . . . O11 O 0.3558(3) 0.4733(3) 0.8861(2) 0.0292(7) Uani 1 1 d . . . O12 O 0.4628(4) 0.6836(3) 0.9915(3) 0.0373(9) Uani 1 1 d . . . C18 C 0.2565(6) 0.9577(4) 0.7717(4) 0.0449(14) Uani 1 1 d . . . O13 O 0.3337(7) 1.0386(3) 0.8613(4) 0.091(2) Uani 1 1 d . . . O14 O 0.1840(5) 0.9886(3) 0.6980(3) 0.0544(11) Uani 1 1 d . . . O21A O 0.2361(7) 0.2385(6) 0.4648(5) 0.0451(14) Uiso 0.60 1 d PD . . C21A C 0.2731(12) 0.3269(11) 0.4197(10) 0.065(3) Uiso 0.60 1 d PD . . H21A H 0.2192 0.3810 0.4142 0.078 Uiso 0.60 1 calc PR . . N21A N 0.3871(12) 0.3497(11) 0.3778(9) 0.080(3) Uiso 0.60 1 d PD . . C22A C 0.4873(17) 0.2781(16) 0.3920(14) 0.096(4) Uiso 0.60 1 d PD . . C23A C 0.418(2) 0.4495(19) 0.3153(16) 0.119(6) Uiso 0.60 1 d PD . . O21B O 0.2036(17) 0.3128(16) 0.5053(13) 0.089(4) Uiso 0.40 1 d P . . O31B O 0.2060(9) 0.2634(9) 1.0027(7) 0.0333(17) Uiso 0.40 1 d PD . . C31B C 0.266(2) 0.346(2) 1.0924(14) 0.092(6) Uiso 0.40 1 d PD . . H31B H 0.3616 0.4025 1.1055 0.111 Uiso 0.40 1 calc PR . . N31B N 0.2012(17) 0.3635(16) 1.1774(13) 0.075(4) Uiso 0.40 1 d PD . . C32B C 0.045(2) 0.292(3) 1.147(3) 0.154(13) Uiso 0.40 1 d PD . . C33B C 0.282(4) 0.448(4) 1.291(2) 0.164(14) Uiso 0.40 1 d PD . . O31A O 0.1615(12) 0.1881(12) 0.9598(10) 0.097(3) Uiso 0.60 1 d P . . 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 0.0200(4) 0.0133(4) 0.0156(4) -0.0001(3) -0.0065(3) 0.0079(3) Ca2 0.0102(4) 0.0222(4) 0.0267(5) -0.0115(3) -0.0041(3) 0.0055(3) N1 0.0128(15) 0.069(3) 0.033(2) -0.036(2) -0.0061(15) 0.0142(17) C1 0.0137(19) 0.053(3) 0.023(2) -0.026(2) -0.0041(18) 0.0103(19) C2 0.0104(17) 0.033(2) 0.0187(19) -0.0113(17) -0.0034(15) 0.0077(16) C3 0.0112(17) 0.0262(19) 0.0170(18) -0.0071(16) -0.0004(15) 0.0077(15) C4 0.0108(18) 0.036(2) 0.020(2) -0.0148(17) -0.0031(16) 0.0064(17) C5 0.012(2) 0.056(3) 0.028(2) -0.022(2) -0.0047(18) 0.013(2) C6 0.014(2) 0.065(3) 0.033(3) -0.032(2) -0.002(2) 0.015(2) C7 0.0112(17) 0.0160(17) 0.0168(18) -0.0023(14) -0.0012(14) 0.0050(14) O1 0.0092(12) 0.0210(13) 0.0166(13) -0.0060(10) -0.0025(10) 0.0051(10) O2 0.0127(12) 0.0290(15) 0.0170(13) -0.0138(11) -0.0048(11) 0.0091(11) C8 0.013(2) 0.056(3) 0.034(3) -0.028(2) -0.0055(19) 0.012(2) O3 0.0102(13) 0.0369(17) 0.0275(15) -0.0154(13) -0.0009(12) 0.0085(12) O4 0.0166(17) 0.107(4) 0.053(2) -0.060(2) -0.0151(17) 0.025(2) N11 0.0351(19) 0.0187(17) 0.0219(18) 0.0010(14) -0.0146(15) 0.0078(15) C11 0.041(3) 0.016(2) 0.029(2) 0.0003(17) -0.012(2) 0.0109(18) C12 0.037(2) 0.020(2) 0.027(2) 0.0040(17) -0.0155(19) 0.0100(18) C13 0.030(2) 0.0153(18) 0.0183(19) -0.0027(15) -0.0124(17) 0.0060(16) C14 0.025(2) 0.0118(17) 0.021(2) 0.0009(15) -0.0069(16) 0.0053(15) C15 0.0237(19) 0.0122(17) 0.0199(19) -0.0001(15) -0.0079(16) 0.0055(15) C16 0.037(2) 0.0141(18) 0.022(2) -0.0014(16) -0.0127(18) 0.0070(17) C17 0.0215(19) 0.0159(18) 0.0186(19) 0.0000(15) -0.0074(16) 0.0063(15) O11 0.0366(16) 0.0123(13) 0.0249(15) -0.0012(11) -0.0147(13) 0.0100(12) O12 0.0457(19) 0.0158(14) 0.0258(16) -0.0036(12) -0.0251(15) 0.0077(13) C18 0.062(3) 0.018(2) 0.040(3) 0.001(2) -0.015(3) 0.019(2) O13 0.159(5) 0.0139(17) 0.051(2) -0.0100(17) -0.044(3) 0.029(2) O14 0.068(3) 0.0279(18) 0.056(2) 0.0153(17) -0.015(2) 0.0226(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O11 2.272(3) . ? Ca1 O12 2.280(3) 2_667 ? Ca1 O31A 2.322(11) . ? Ca1 O3 2.334(3) 1_655 ? Ca1 O31B 2.370(8) . ? Ca1 O1 2.414(2) . ? Ca1 O13 2.418(4) 1_545 ? Ca1 O14 2.998(4) 1_545 ? Ca1 C18 3.075(4) 1_545 ? Ca1 C31B 3.146(17) . ? Ca1 Ca2 3.6204(11) . ? Ca2 O21A 2.179(6) . ? Ca2 O14 2.285(4) 1_545 ? Ca2 O2 2.310(3) 2_556 ? Ca2 O4 2.419(3) 1_655 ? Ca2 O1 2.440(3) . ? Ca2 O3 2.488(3) 1_655 ? Ca2 O2 2.586(3) . ? Ca2 O21B 2.595(15) . ? Ca2 C8 2.799(4) 1_655 ? Ca2 C7 2.875(4) . ? Ca2 Ca2 3.7693(15) 2_556 ? N1 N1 1.241(7) 2_567 ? N1 C1 1.436(5) . ? C1 C2 1.392(6) . ? C1 C6 1.396(6) . ? C2 C3 1.394(5) . ? C3 C4 1.407(5) . ? C3 C7 1.502(6) . ? C4 C5 1.390(7) . ? C5 C6 1.401(6) . ? C5 C8 1.510(6) . ? C7 O2 1.258(5) . ? C7 O1 1.260(4) . ? O2 Ca2 2.310(3) 2_556 ? C8 O4 1.254(6) . ? C8 O3 1.263(6) . ? C8 Ca2 2.799(4) 1_455 ? O3 Ca1 2.334(3) 1_455 ? O3 Ca2 2.488(3) 1_455 ? O4 Ca2 2.419(3) 1_455 ? N11 N11 1.252(7) 2_566 ? N11 C13 1.443(5) . ? C11 C12 1.390(6) . ? C11 C16 1.398(6) . ? C11 C18 1.515(6) . ? C12 C13 1.390(6) . ? C13 C14 1.397(5) . ? C14 C15 1.394(5) . ? C15 C16 1.395(5) . ? C15 C17 1.518(5) . ? C17 O12 1.243(5) . ? C17 O11 1.256(5) . ? O12 Ca1 2.280(3) 2_667 ? C18 O13 1.225(6) . ? C18 O14 1.241(6) . ? C18 Ca1 3.075(4) 1_565 ? O13 Ca1 2.418(3) 1_565 ? O14 Ca2 2.285(4) 1_565 ? O14 Ca1 2.998(4) 1_565 ? O21A O21B 1.059(16) . ? O21A C21A 1.229(11) . ? C21A N21A 1.344(13) . ? N21A C22A 1.473(14) . ? N21A C23A 1.480(15) . ? O31B O31A 0.822(12) . ? O31B C31B 1.210(16) . ? C31B N31B 1.391(16) . ? N31B C32B 1.448(18) . ? N31B C33B 1.456(18) . ? 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 O11 Ca1 O12 91.93(10) . 2_667 ? O11 Ca1 O31A 101.9(3) . . ? O12 Ca1 O31A 98.2(3) 2_667 . ? O11 Ca1 O3 92.96(12) . 1_655 ? O12 Ca1 O3 99.74(12) 2_667 1_655 ? O31A Ca1 O3 156.2(3) . 1_655 ? O11 Ca1 O31B 85.8(2) . . ? O12 Ca1 O31B 86.8(2) 2_667 . ? O31A Ca1 O31B 20.1(3) . . ? O3 Ca1 O31B 173.4(2) 1_655 . ? O11 Ca1 O1 80.26(9) . . ? O12 Ca1 O1 171.23(11) 2_667 . ? O31A Ca1 O1 87.4(3) . . ? O3 Ca1 O1 76.85(10) 1_655 . ? O31B Ca1 O1 96.6(2) . . ? O11 Ca1 O13 172.84(13) . 1_545 ? O12 Ca1 O13 80.93(13) 2_667 1_545 ? O31A Ca1 O13 79.8(3) . 1_545 ? O3 Ca1 O13 87.78(18) 1_655 1_545 ? O31B Ca1 O13 94.2(3) . 1_545 ? O1 Ca1 O13 106.82(12) . 1_545 ? O11 Ca1 O14 141.22(9) . 1_545 ? O12 Ca1 O14 124.15(10) 2_667 1_545 ? O31A Ca1 O14 87.7(3) . 1_545 ? O3 Ca1 O14 69.34(12) 1_655 1_545 ? O31B Ca1 O14 107.8(2) . 1_545 ? O1 Ca1 O14 62.54(9) . 1_545 ? O13 Ca1 O14 45.38(11) 1_545 1_545 ? O11 Ca1 C18 164.51(12) . 1_545 ? O12 Ca1 C18 101.68(12) 2_667 1_545 ? O31A Ca1 C18 83.6(3) . 1_545 ? O3 Ca1 C18 77.60(14) 1_655 1_545 ? O31B Ca1 C18 102.1(2) . 1_545 ? O1 Ca1 C18 85.59(11) . 1_545 ? O13 Ca1 C18 21.86(13) 1_545 1_545 ? O14 Ca1 C18 23.54(11) 1_545 1_545 ? O11 Ca1 C31B 75.3(4) . . ? O12 Ca1 C31B 71.1(4) 2_667 . ? O31A Ca1 C31B 39.1(5) . . ? O3 Ca1 C31B 164.5(4) 1_655 . ? O31B Ca1 C31B 19.6(4) . . ? O1 Ca1 C31B 110.3(4) . . ? O13 Ca1 C31B 102.7(4) 1_545 . ? O14 Ca1 C31B 126.1(4) 1_545 . ? C18 Ca1 C31B 116.0(4) 1_545 . ? O11 Ca1 Ca2 105.06(8) . . ? O12 Ca1 Ca2 138.48(10) 2_667 . ? O31A Ca1 Ca2 114.3(3) . . ? O3 Ca1 Ca2 42.98(7) 1_655 . ? O31B Ca1 Ca2 131.2(2) . . ? O1 Ca1 Ca2 42.04(7) . . ? O13 Ca1 Ca2 80.27(10) 1_545 . ? O14 Ca1 Ca2 38.99(7) 1_545 . ? C18 Ca1 Ca2 59.70(10) 1_545 . ? C31B Ca1 Ca2 149.5(4) . . ? O21A Ca2 O14 170.8(2) . 1_545 ? O21A Ca2 O2 101.68(19) . 2_556 ? O14 Ca2 O2 87.54(12) 1_545 2_556 ? O21A Ca2 O4 88.8(2) . 1_655 ? O14 Ca2 O4 89.54(19) 1_545 1_655 ? O2 Ca2 O4 100.84(12) 2_556 1_655 ? O21A Ca2 O1 99.59(19) . . ? O14 Ca2 O1 74.21(13) 1_545 . ? O2 Ca2 O1 127.99(10) 2_556 . ? O4 Ca2 O1 126.56(11) 1_655 . ? O21A Ca2 O3 91.45(18) . 1_655 ? O14 Ca2 O3 80.32(13) 1_545 1_655 ? O2 Ca2 O3 151.15(10) 2_556 1_655 ? O4 Ca2 O3 53.37(11) 1_655 1_655 ? O1 Ca2 O3 73.60(9) . 1_655 ? O21A Ca2 O2 94.94(18) . . ? O14 Ca2 O2 86.56(13) 1_545 . ? O2 Ca2 O2 79.47(10) 2_556 . ? O4 Ca2 O2 176.08(16) 1_655 . ? O1 Ca2 O2 51.75(8) . . ? O3 Ca2 O2 125.30(9) 1_655 . ? O21A Ca2 O21B 23.6(4) . . ? O14 Ca2 O21B 149.8(4) 1_545 . ? O2 Ca2 O21B 115.2(3) 2_556 . ? O4 Ca2 O21B 104.3(4) 1_655 . ? O1 Ca2 O21B 76.0(4) . . ? O3 Ca2 O21B 86.6(3) 1_655 . ? O2 Ca2 O21B 79.0(4) . . ? O21A Ca2 C8 90.1(2) . 1_655 ? O14 Ca2 C8 84.44(17) 1_545 1_655 ? O2 Ca2 C8 126.45(12) 2_556 1_655 ? O4 Ca2 C8 26.56(13) 1_655 1_655 ? O1 Ca2 C8 100.23(12) . 1_655 ? O3 Ca2 C8 26.81(12) 1_655 1_655 ? O2 Ca2 C8 151.98(12) . 1_655 ? O21B Ca2 C8 96.0(4) . 1_655 ? O21A Ca2 C7 97.72(19) . . ? O14 Ca2 C7 79.70(14) 1_545 . ? O2 Ca2 C7 104.11(10) 2_556 . ? O4 Ca2 C7 152.27(11) 1_655 . ? O1 Ca2 C7 25.80(9) . . ? O3 Ca2 C7 99.35(10) 1_655 . ? O2 Ca2 C7 25.96(9) . . ? O21B Ca2 C7 75.7(4) . . ? C8 Ca2 C7 126.03(12) 1_655 . ? O21A Ca2 Ca1 115.21(17) . . ? O14 Ca2 Ca1 55.63(10) 1_545 . ? O2 Ca2 Ca1 142.45(8) 2_556 . ? O4 Ca2 Ca1 87.23(10) 1_655 . ? O1 Ca2 Ca1 41.50(6) . . ? O3 Ca2 Ca1 39.76(7) 1_655 . ? O2 Ca2 Ca1 90.19(6) . . ? O21B Ca2 Ca1 97.7(3) . . ? C8 Ca2 Ca1 62.94(11) 1_655 . ? C7 Ca2 Ca1 65.57(7) . . ? O21A Ca2 Ca2 100.55(16) . 2_556 ? O14 Ca2 Ca2 86.14(11) 1_545 2_556 ? O2 Ca2 Ca2 42.41(7) 2_556 2_556 ? O4 Ca2 Ca2 143.10(10) 1_655 2_556 ? O1 Ca2 Ca2 87.28(6) . 2_556 ? O3 Ca2 Ca2 158.94(8) 1_655 2_556 ? O2 Ca2 Ca2 37.05(6) . 2_556 ? O21B Ca2 Ca2 97.5(3) . 2_556 ? C8 Ca2 Ca2 165.86(13) 1_655 2_556 ? C7 Ca2 Ca2 62.13(7) . 2_556 ? Ca1 Ca2 Ca2 119.22(4) . 2_556 ? N1 N1 C1 114.5(5) 2_567 . ? C2 C1 C6 120.4(4) . . ? C2 C1 N1 123.9(4) . . ? C6 C1 N1 115.7(4) . . ? C1 C2 C3 119.7(3) . . ? C2 C3 C4 120.2(4) . . ? C2 C3 C7 118.4(3) . . ? C4 C3 C7 121.3(3) . . ? C5 C4 C3 119.8(4) . . ? C4 C5 C6 120.0(4) . . ? C4 C5 C8 120.8(4) . . ? C6 C5 C8 119.2(4) . . ? C1 C6 C5 119.9(4) . . ? O2 C7 O1 121.5(3) . . ? O2 C7 C3 120.6(3) . . ? O1 C7 C3 117.9(3) . . ? O2 C7 Ca2 64.1(2) . . ? O1 C7 Ca2 57.43(19) . . ? C3 C7 Ca2 174.9(3) . . ? C7 O1 Ca1 151.5(3) . . ? C7 O1 Ca2 96.8(2) . . ? Ca1 O1 Ca2 96.45(9) . . ? C7 O2 Ca2 158.8(3) . 2_556 ? C7 O2 Ca2 90.0(2) . . ? Ca2 O2 Ca2 100.53(10) 2_556 . ? O4 C8 O3 122.3(4) . . ? O4 C8 C5 119.5(4) . . ? O3 C8 C5 118.2(4) . . ? O4 C8 Ca2 59.6(2) . 1_455 ? O3 C8 Ca2 62.7(2) . 1_455 ? C5 C8 Ca2 178.8(4) . 1_455 ? C8 O3 Ca1 142.5(4) . 1_455 ? C8 O3 Ca2 90.5(2) . 1_455 ? Ca1 O3 Ca2 97.26(10) 1_455 1_455 ? C8 O4 Ca2 93.9(3) . 1_455 ? N11 N11 C13 114.0(4) 2_566 . ? C12 C11 C16 120.3(4) . . ? C12 C11 C18 119.8(4) . . ? C16 C11 C18 119.9(4) . . ? C11 C12 C13 119.3(4) . . ? C12 C13 C14 120.9(4) . . ? C12 C13 N11 124.4(3) . . ? C14 C13 N11 114.8(3) . . ? C15 C14 C13 119.7(3) . . ? C14 C15 C16 119.6(3) . . ? C14 C15 C17 120.1(3) . . ? C16 C15 C17 120.2(3) . . ? C15 C16 C11 120.2(4) . . ? O12 C17 O11 125.8(3) . . ? O12 C17 C15 116.8(3) . . ? O11 C17 C15 117.3(3) . . ? C17 O11 Ca1 174.8(2) . . ? C17 O12 Ca1 144.3(3) . 2_667 ? O13 C18 O14 122.0(4) . . ? O13 C18 C11 120.0(4) . . ? O14 C18 C11 117.8(4) . . ? O13 C18 Ca1 47.3(2) . 1_565 ? O14 C18 Ca1 74.8(3) . 1_565 ? C11 C18 Ca1 167.3(3) . 1_565 ? C18 O13 Ca1 110.8(3) . 1_565 ? C18 O14 Ca2 143.6(4) . 1_565 ? C18 O14 Ca1 81.7(3) . 1_565 ? Ca2 O14 Ca1 85.38(11) 1_565 1_565 ? O21B O21A C21A 76.7(11) . . ? O21B O21A Ca2 100.8(9) . . ? C21A O21A Ca2 171.0(7) . . ? O21A C21A N21A 123.7(11) . . ? C21A N21A C22A 122.2(11) . . ? C21A N21A C23A 120.9(12) . . ? C22A N21A C23A 117.0(13) . . ? O21A O21B Ca2 55.5(8) . . ? O31A O31B C31B 156.0(17) . . ? O31A O31B Ca1 76.6(11) . . ? C31B O31B Ca1 119.4(11) . . ? O31B C31B N31B 124.6(19) . . ? O31B C31B Ca1 41.0(8) . . ? N31B C31B Ca1 165.5(14) . . ? C31B N31B C32B 116(2) . . ? C31B N31B C33B 123(2) . . ? C32B N31B C33B 120.8(19) . . ? O31B O31A Ca1 83.3(11) . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 1.115 _refine_diff_density_min -0.828 _refine_diff_density_rms 0.105