# Copyright The Royal Society of Chemistry, 1998 # 8/04768E data_CuQ2.H2O_Compound_No.1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 Cu N4 O5' _chemical_formula_weight 624.22 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' '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' 'Cu' 'Cu' 0.3201 1.2651 '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 9.169(2) _cell_length_b 13.410(3) _cell_length_c 14.350(3) _cell_angle_alpha 65.93(3) _cell_angle_beta 73.23(3) _cell_angle_gamma 78.72(3) _cell_volume 1536.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 16 _cell_measurement_theta_max 18 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 658 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 STADI-4 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 2h _diffrn_standards_decay_% 0.02 _diffrn_reflns_number 3744 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0164 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 22.00 _reflns_number_total 3744 _reflns_number_gt 3209 _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 w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+1.8697P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3744 _refine_ls_number_parameters 412 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1392 _refine_ls_wR_factor_gt 0.1315 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.007 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.85838(6) 0.19522(4) 0.72900(4) 0.0590(3) Uani 1 d . . . O1 O 0.7825(3) 0.1125(2) 0.8746(2) 0.0580(8) Uani 1 d . . . O2 O 1.0023(4) 0.0752(3) 0.7089(3) 0.0929(13) Uani 1 d . . . O3 O 0.6919(3) 0.3065(2) 0.7472(2) 0.0638(8) Uani 1 d . . . O4 O 0.9090(3) 0.2696(2) 0.5789(2) 0.0636(8) Uani 1 d . . . O5 O 1.0296(5) 0.2751(3) 0.7546(3) 0.0910(13) Uani 1 d D . . H5A H 1.069(7) 0.328(4) 0.718(4) 0.109 Uiso 1 d D . . H5B H 1.070(7) 0.246(5) 0.799(4) 0.109 Uiso 1 d D . . N1 N 0.7863(4) -0.0449(2) 1.0236(2) 0.0483(8) Uani 1 d . . . N2 N 0.8721(4) -0.1463(2) 1.0534(3) 0.0534(9) Uani 1 d . . . N3 N 0.9045(4) 0.4280(3) 0.4306(3) 0.0545(9) Uani 1 d . . . N4 N 0.8243(4) 0.5320(3) 0.4025(3) 0.0606(10) Uani 1 d . . . C1 C 0.8402(4) 0.0157(3) 0.9206(3) 0.0476(10) Uani 1 d . . . C2 C 0.9620(5) -0.0500(3) 0.8814(3) 0.0539(11) Uani 1 d . . . C3 C 0.9741(5) -0.1488(3) 0.9705(4) 0.0558(11) Uani 1 d . . . C4 C 1.0855(6) -0.2494(4) 0.9795(4) 0.0824(16) Uani 1 d . . . H4A H 1.1881 -0.2285 0.9566 0.124 Uiso 1 calc R . . H4B H 1.0711 -0.2840 0.9363 0.124 Uiso 1 calc R . . H4C H 1.0681 -0.2997 1.0512 0.124 Uiso 1 calc R . . C5 C 1.0380(6) -0.0169(4) 0.7758(4) 0.0832(16) Uani 1 d . . . C6 C 1.1736(10) -0.0884(5) 0.7390(5) 0.156(4) Uani 1 d . . . H6A H 1.2613 -0.0748 0.7556 0.188 Uiso 1 calc R A 1 H6B H 1.1533 -0.1639 0.7828 0.188 Uiso 1 calc R A 1 C71 C 1.2214(5) -0.0824(3) 0.6321(4) 0.0611(12) Uani 0.12(2) d PD B 1 C81 C 1.364(10) -0.165(9) 0.639(10) 0.09(3) Uiso 0.12(2) d PD B 1 H81A H 1.4279 -0.1488 0.6728 0.139 Uiso 0.12(2) calc PR B 1 H81B H 1.4203 -0.1594 0.5695 0.139 Uiso 0.12(2) calc PR B 1 H81C H 1.3336 -0.2378 0.6788 0.139 Uiso 0.12(2) calc PR B 1 C91 C 1.306(10) 0.022(6) 0.589(7) 0.11(3) Uiso 0.12(2) d PD B 1 H91A H 1.2435 0.0748 0.6162 0.166 Uiso 0.12(2) calc PR B 1 H91B H 1.3266 0.0518 0.5140 0.166 Uiso 0.12(2) calc PR B 1 H91C H 1.4007 0.0034 0.6110 0.166 Uiso 0.12(2) calc PR B 1 C101 C 1.093(5) -0.140(3) 0.628(3) 0.038(14) Uiso 0.12(2) d PD B 1 H101 H 1.1203 -0.1528 0.5637 0.058 Uiso 0.12(2) calc PR B 1 H102 H 0.9986 -0.0935 0.6307 0.058 Uiso 0.12(2) calc PR B 1 H103 H 1.0800 -0.2083 0.6865 0.058 Uiso 0.12(2) calc PR B 1 C7 C 1.2214(5) -0.0824(3) 0.6321(4) 0.0611(12) Uani 0.88(2) d P B 2 C8 C 1.3277(17) -0.1722(9) 0.6108(11) 0.142(7) Uani 0.88(2) d P B 2 H8A H 1.3590 -0.1548 0.5365 0.213 Uiso 0.88(2) calc PR B 2 H8B H 1.2776 -0.2387 0.6442 0.213 Uiso 0.88(2) calc PR B 2 H8C H 1.4159 -0.1817 0.6379 0.213 Uiso 0.88(2) calc PR B 2 C9 C 1.2632(13) 0.0264(6) 0.5520(8) 0.113(4) Uani 0.88(2) d P B 2 H9A H 1.3482 0.0468 0.5647 0.169 Uiso 0.88(2) calc PR B 2 H9B H 1.1776 0.0798 0.5559 0.169 Uiso 0.88(2) calc PR B 2 H9C H 1.2911 0.0230 0.4835 0.169 Uiso 0.88(2) calc PR B 2 C10 C 1.0752(15) -0.090(2) 0.6081(18) 0.287(11) Uani 0.88(2) d P B 2 H10A H 1.0214 -0.0185 0.5857 0.431 Uiso 0.88(2) calc PR B 2 H10B H 1.0123 -0.1383 0.6700 0.431 Uiso 0.88(2) calc PR B 2 H10C H 1.0989 -0.1183 0.5532 0.431 Uiso 0.88(2) calc PR B 2 C11 C 0.6540(4) -0.0252(3) 1.0959(3) 0.0478(10) Uani 1 d . . . C12 C 0.5538(5) 0.0684(4) 1.0660(4) 0.0659(12) Uani 1 d . . . H12 H 0.5756 0.1208 0.9983 0.079 Uiso 1 calc R . . C13 C 0.4214(6) 0.0827(4) 1.1379(4) 0.0762(14) Uani 1 d . . . H13 H 0.3541 0.1449 1.1175 0.091 Uiso 1 calc R . . C14 C 0.3882(6) 0.0075(4) 1.2379(4) 0.0744(14) Uani 1 d . . . H14 H 0.3004 0.0187 1.2861 0.089 Uiso 1 calc R . . C15 C 0.4858(6) -0.0846(4) 1.2661(4) 0.0754(14) Uani 1 d . . . H15 H 0.4627 -0.1372 1.3336 0.090 Uiso 1 calc R . . C16 C 0.6171(5) -0.1008(4) 1.1967(3) 0.0642(12) Uani 1 d . . . H16 H 0.6824 -0.1639 1.2180 0.077 Uiso 1 calc R . . C17 C 0.8554(5) 0.3684(3) 0.5354(3) 0.0529(10) Uani 1 d . . . C18 C 0.7412(5) 0.4369(3) 0.5766(3) 0.0510(10) Uani 1 d . . . C19 C 0.7291(5) 0.5364(3) 0.4881(3) 0.0575(11) Uani 1 d . . . C20 C 0.6256(6) 0.6400(4) 0.4801(4) 0.0792(15) Uani 1 d . . . H20A H 0.6416 0.6702 0.5263 0.119 Uiso 1 calc R . . H20B H 0.5210 0.6239 0.4998 0.119 Uiso 1 calc R . . H20C H 0.6480 0.6922 0.4092 0.119 Uiso 1 calc R . . C21 C 0.6635(5) 0.4020(3) 0.6837(3) 0.0529(10) Uani 1 d . . . C22 C 0.5458(5) 0.4785(3) 0.7250(3) 0.0603(11) Uani 1 d . . . H22A H 0.4699 0.5040 0.6832 0.072 Uiso 1 calc R . . H22B H 0.5962 0.5419 0.7113 0.072 Uiso 1 calc R . . C23 C 0.4601(4) 0.4387(3) 0.8400(3) 0.0540(10) Uani 1 d . . . C24 C 0.3561(5) 0.5364(4) 0.8571(4) 0.0723(13) Uani 1 d . . . H24A H 0.3012 0.5151 0.9292 0.109 Uiso 1 calc R . . H24B H 0.2848 0.5606 0.8130 0.109 Uiso 1 calc R . . H24C H 0.4168 0.5950 0.8398 0.109 Uiso 1 calc R . . C25 C 0.3633(5) 0.3459(4) 0.8668(5) 0.0788(15) Uani 1 d . . . H25A H 0.3025 0.3280 0.9373 0.118 Uiso 1 calc R . . H25B H 0.4292 0.2825 0.8609 0.118 Uiso 1 calc R . . H25C H 0.2976 0.3687 0.8191 0.118 Uiso 1 calc R . . C26 C 0.5696(5) 0.3993(4) 0.9130(4) 0.0696(13) Uani 1 d . . . H26A H 0.5121 0.3856 0.9838 0.104 Uiso 1 calc R . . H26B H 0.6377 0.4545 0.8923 0.104 Uiso 1 calc R . . H26C H 0.6278 0.3329 0.9087 0.104 Uiso 1 calc R . . C27 C 1.0091(5) 0.3960(3) 0.3518(3) 0.0519(10) Uani 1 d . . . C28 C 1.1215(5) 0.3112(4) 0.3766(4) 0.0670(12) Uani 1 d . . . H28 H 1.1302 0.2746 0.4458 0.080 Uiso 1 calc R . . C29 C 1.2209(6) 0.2814(4) 0.2977(4) 0.0794(15) Uani 1 d . . . H29 H 1.2964 0.2240 0.3140 0.095 Uiso 1 calc R . . C30 C 1.2093(6) 0.3356(4) 0.1956(4) 0.0843(16) Uani 1 d . . . H30 H 1.2768 0.3152 0.1427 0.101 Uiso 1 calc R . . C31 C 1.0974(6) 0.4200(4) 0.1719(4) 0.0804(15) Uani 1 d . . . H31 H 1.0889 0.4567 0.1027 0.096 Uiso 1 calc R . . C32 C 0.9992(5) 0.4505(4) 0.2486(4) 0.0666(12) Uani 1 d . . . H32 H 0.9246 0.5085 0.2316 0.080 Uiso 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 Cu 0.0698(4) 0.0337(3) 0.0547(4) -0.0081(3) -0.0143(3) 0.0175(2) O1 0.0710(19) 0.0330(15) 0.0550(17) -0.0101(13) -0.0152(14) 0.0149(13) O2 0.115(3) 0.047(2) 0.060(2) -0.0016(16) 0.0063(19) 0.0375(18) O3 0.073(2) 0.0390(17) 0.0576(18) -0.0081(14) -0.0133(15) 0.0176(14) O4 0.079(2) 0.0382(16) 0.0545(18) -0.0095(14) -0.0168(15) 0.0207(14) O5 0.093(3) 0.075(3) 0.083(3) 0.012(2) -0.043(2) -0.019(2) N1 0.053(2) 0.0321(18) 0.054(2) -0.0102(16) -0.0201(17) 0.0059(15) N2 0.056(2) 0.0322(18) 0.060(2) -0.0061(16) -0.0193(18) 0.0086(15) N3 0.066(2) 0.0384(19) 0.051(2) -0.0118(16) -0.0205(17) 0.0127(16) N4 0.071(2) 0.040(2) 0.057(2) -0.0081(17) -0.024(2) 0.0154(17) C1 0.055(2) 0.030(2) 0.054(3) -0.0109(19) -0.020(2) 0.0035(18) C2 0.053(2) 0.030(2) 0.064(3) -0.008(2) -0.014(2) 0.0079(18) C3 0.050(2) 0.036(2) 0.066(3) -0.009(2) -0.013(2) 0.0057(18) C4 0.075(3) 0.050(3) 0.076(3) 0.000(2) -0.008(3) 0.027(2) C5 0.088(4) 0.044(3) 0.071(3) -0.004(3) 0.003(3) 0.024(2) C6 0.204(8) 0.079(4) 0.086(5) -0.004(4) 0.011(5) 0.081(5) C71 0.055(3) 0.051(3) 0.067(3) -0.025(2) 0.004(2) -0.001(2) C7 0.055(3) 0.051(3) 0.067(3) -0.025(2) 0.004(2) -0.001(2) C8 0.160(11) 0.063(5) 0.114(10) -0.020(5) 0.046(8) 0.042(7) C9 0.114(7) 0.069(5) 0.084(6) -0.001(4) 0.028(6) 0.012(4) C10 0.127(10) 0.33(2) 0.57(4) -0.35(2) -0.095(15) 0.041(12) C11 0.051(2) 0.040(2) 0.055(3) -0.019(2) -0.018(2) 0.0026(18) C12 0.071(3) 0.045(3) 0.070(3) -0.017(2) -0.015(2) 0.007(2) C13 0.075(3) 0.054(3) 0.090(4) -0.030(3) -0.017(3) 0.020(2) C14 0.074(3) 0.074(3) 0.069(3) -0.033(3) -0.004(3) 0.005(3) C15 0.083(3) 0.069(3) 0.055(3) -0.017(2) -0.009(3) 0.011(3) C16 0.071(3) 0.057(3) 0.053(3) -0.016(2) -0.019(2) 0.016(2) C17 0.060(3) 0.035(2) 0.059(3) -0.013(2) -0.026(2) 0.009(2) C18 0.057(2) 0.036(2) 0.053(3) -0.0111(19) -0.020(2) 0.0098(18) C19 0.065(3) 0.039(2) 0.060(3) -0.012(2) -0.024(2) 0.013(2) C20 0.095(4) 0.046(3) 0.070(3) -0.008(2) -0.022(3) 0.028(2) C21 0.056(3) 0.035(2) 0.064(3) -0.014(2) -0.024(2) 0.0085(18) C22 0.067(3) 0.038(2) 0.065(3) -0.014(2) -0.020(2) 0.015(2) C23 0.047(2) 0.043(2) 0.067(3) -0.018(2) -0.016(2) 0.0054(18) C24 0.065(3) 0.060(3) 0.084(3) -0.031(3) -0.012(3) 0.015(2) C25 0.064(3) 0.054(3) 0.114(4) -0.027(3) -0.022(3) -0.001(2) C26 0.071(3) 0.067(3) 0.074(3) -0.027(3) -0.028(2) 0.005(2) C27 0.054(2) 0.042(2) 0.055(3) -0.014(2) -0.015(2) 0.0020(19) C28 0.070(3) 0.053(3) 0.066(3) -0.016(2) -0.015(2) 0.006(2) C29 0.074(3) 0.052(3) 0.087(4) -0.018(3) -0.002(3) 0.008(2) C30 0.093(4) 0.066(3) 0.080(4) -0.033(3) 0.012(3) -0.011(3) C31 0.099(4) 0.071(3) 0.057(3) -0.018(3) -0.012(3) 0.000(3) C32 0.073(3) 0.056(3) 0.060(3) -0.017(2) -0.018(2) 0.010(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 Cu O1 1.912(3) . ? Cu O4 1.924(3) . ? Cu O2 1.935(3) . ? Cu O3 1.955(3) . ? Cu O5 2.250(4) . ? O1 C1 1.278(4) . ? O2 C5 1.268(5) . ? O3 C21 1.262(5) . ? O4 C17 1.278(4) . ? N1 C1 1.358(5) . ? N1 N2 1.398(4) . ? N1 C11 1.411(5) . ? N2 C3 1.292(5) . ? N3 C17 1.368(5) . ? N3 N4 1.400(4) . ? N3 C27 1.412(5) . ? N4 C19 1.302(5) . ? C1 C2 1.414(5) . ? C2 C5 1.394(6) . ? C2 C3 1.430(6) . ? C3 C4 1.508(6) . ? C5 C6 1.520(7) . ? C6 C71 1.441(8) . ? C71 C81 1.54(4) . ? C71 C101 1.56(4) . ? C71 C91 1.54(4) . ? C11 C16 1.374(6) . ? C11 C12 1.392(6) . ? C12 C13 1.387(7) . ? C13 C14 1.363(7) . ? C14 C15 1.363(6) . ? C15 C16 1.369(6) . ? C17 C18 1.414(6) . ? C18 C21 1.415(6) . ? C18 C19 1.431(6) . ? C19 C20 1.504(6) . ? C21 C22 1.503(6) . ? C22 C23 1.524(6) . ? C23 C24 1.524(6) . ? C23 C26 1.528(6) . ? C23 C25 1.526(6) . ? C27 C32 1.379(6) . ? C27 C28 1.381(6) . ? C28 C29 1.380(7) . ? C29 C30 1.370(7) . ? C30 C31 1.373(7) . ? C31 C32 1.357(7) . ? 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 Cu O4 170.79(13) . . ? O1 Cu O2 92.93(12) . . ? O4 Cu O2 87.27(12) . . ? O1 Cu O3 86.00(12) . . ? O4 Cu O3 92.53(12) . . ? O2 Cu O3 172.06(16) . . ? O1 Cu O5 95.06(14) . . ? O4 Cu O5 94.10(14) . . ? O2 Cu O5 94.41(18) . . ? O3 Cu O5 93.52(15) . . ? C1 O1 Cu 122.0(3) . . ? C5 O2 Cu 129.9(3) . . ? C21 O3 Cu 129.7(3) . . ? C17 O4 Cu 121.0(3) . . ? C1 N1 N2 110.6(3) . . ? C1 N1 C11 130.2(3) . . ? N2 N1 C11 118.8(3) . . ? C3 N2 N1 106.7(3) . . ? C17 N3 N4 110.8(3) . . ? C17 N3 C27 129.7(3) . . ? N4 N3 C27 119.3(3) . . ? C19 N4 N3 106.3(3) . . ? O1 C1 N1 122.8(4) . . ? O1 C1 C2 130.6(4) . . ? N1 C1 C2 106.6(3) . . ? C5 C2 C1 122.5(4) . . ? C5 C2 C3 133.0(4) . . ? C1 C2 C3 104.4(4) . . ? N2 C3 C2 111.7(3) . . ? N2 C3 C4 118.6(4) . . ? C2 C3 C4 129.7(4) . . ? O2 C5 C2 121.6(4) . . ? O2 C5 C6 118.1(4) . . ? C2 C5 C6 120.2(4) . . ? C71 C6 C5 122.6(5) . . ? C6 C71 C81 100(5) . . ? C6 C71 C101 100.9(15) . . ? C81 C71 C101 107(4) . . ? C6 C71 C91 96(4) . . ? C81 C71 C91 97(6) . . ? C101 C71 C91 148(4) . . ? C16 C11 C12 118.3(4) . . ? C16 C11 N1 120.5(3) . . ? C12 C11 N1 121.1(4) . . ? C13 C12 C11 119.6(4) . . ? C14 C13 C12 121.2(4) . . ? C15 C14 C13 118.9(5) . . ? C14 C15 C16 121.1(5) . . ? C15 C16 C11 121.0(4) . . ? O4 C17 N3 122.3(4) . . ? O4 C17 C18 131.3(4) . . ? N3 C17 C18 106.4(3) . . ? C21 C18 C17 122.3(3) . . ? C21 C18 C19 133.1(4) . . ? C17 C18 C19 104.6(4) . . ? N4 C19 C18 111.9(4) . . ? N4 C19 C20 117.6(4) . . ? C18 C19 C20 130.4(4) . . ? O3 C21 C18 121.0(4) . . ? O3 C21 C22 118.3(4) . . ? C18 C21 C22 120.6(3) . . ? C21 C22 C23 120.0(3) . . ? C22 C23 C24 106.8(3) . . ? C22 C23 C26 111.5(4) . . ? C24 C23 C26 108.7(4) . . ? C22 C23 C25 111.4(4) . . ? C24 C23 C25 109.4(4) . . ? C26 C23 C25 108.8(4) . . ? C32 C27 C28 119.7(4) . . ? C32 C27 N3 119.6(4) . . ? C28 C27 N3 120.8(4) . . ? C29 C28 C27 119.2(5) . . ? C30 C29 C28 120.6(5) . . ? C29 C30 C31 119.5(5) . . ? C32 C31 C30 120.5(5) . . ? C31 C32 C27 120.4(4) . . ? _refine_diff_density_max 0.563 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.051 #=END data_CaQ2.2EtOH_Compound_No.9 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H50 Ca N4 O6' _chemical_formula_weight 674.88 _chemical_melting_point ? _chemical_compound_source ? 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 9.652(2) _cell_length_b 11.476(2) _cell_length_c 16.828(3) _cell_angle_alpha 97.51(3) _cell_angle_beta 100.22(3) _cell_angle_gamma 90.10(3) _cell_volume 1818.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 951 _cell_measurement_theta_min 5 _cell_measurement_theta_max 20 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method ? _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.221 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 IPDS _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10632 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 22.53 _reflns_number_total 4499 _reflns_number_observed 3330 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 229 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0542P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4270 _refine_ls_number_parameters 441 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_obs 0.0387 _refine_ls_wR_factor_all 0.1243 _refine_ls_wR_factor_obs 0.0890 _refine_ls_goodness_of_fit_all 0.926 _refine_ls_goodness_of_fit_obs 1.029 _refine_ls_restrained_S_all 1.219 _refine_ls_restrained_S_obs 1.029 _refine_ls_shift/esd_max 0.008 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ca Ca 0.74447(5) 0.47420(4) 0.74938(3) 0.0193(2) Uani 1 d . . O1 O 0.5529(2) 0.41262(13) 0.65140(11) 0.0238(4) Uani 1 d . . O2 O 0.6432(2) 0.64527(13) 0.71504(11) 0.0282(5) Uani 1 d . . O4 O 0.9295(2) 0.55505(12) 0.84579(10) 0.0208(4) Uani 1 d . . O3 O 0.8659(2) 0.31282(13) 0.79040(11) 0.0253(4) Uani 1 d . . O5 O 0.6227(2) 0.4803(2) 0.85863(13) 0.0267(5) Uani 1 d . . H5 H 0.6674(31) 0.4799(23) 0.9024(20) 0.034(7) Uiso 1 d . . O6 O 0.8764(2) 0.4925(2) 0.64549(13) 0.0294(5) Uani 1 d . . H6 H 0.8382(30) 0.5068(23) 0.5998(20) 0.034(7) Uiso 1 d . . N1 N 0.3555(2) 0.4222(2) 0.55161(13) 0.0204(5) Uani 1 d . . N2 N 0.2753(2) 0.5078(2) 0.51438(13) 0.0215(5) Uani 1 d . . N3 N 1.1280(2) 0.56694(15) 0.94695(13) 0.0172(5) Uani 1 d . . N4 N 1.2211(2) 0.4906(2) 0.98567(13) 0.0184(5) Uani 1 d . . C1 C 0.4658(2) 0.4725(2) 0.6095(2) 0.0184(6) Uani 1 d . . C2 C 0.4530(2) 0.5969(2) 0.6103(2) 0.0195(6) Uani 1 d . . C3 C 0.3331(3) 0.6097(2) 0.5495(2) 0.0220(6) Uani 1 d . . C4 C 0.2685(3) 0.7194(2) 0.5212(2) 0.0284(7) Uani 1 d . . H4A H 0.3405(5) 0.7670(7) 0.5051(10) 0.043 Uiso 1 calc R . H4B H 0.2303(16) 0.7646(8) 0.5656(4) 0.043 Uiso 1 calc R . H4C H 0.1925(12) 0.6981(2) 0.4745(7) 0.043 Uiso 1 calc R . C5 C 0.5451(3) 0.6799(2) 0.6660(2) 0.0211(6) Uani 1 d . . C6 C 0.5291(3) 0.8115(2) 0.6663(2) 0.0277(7) Uani 1 d . . H6A H 0.4273(3) 0.8274(2) 0.6543(2) 0.033 Uiso 1 calc R . H6B H 0.5713(3) 0.8347(2) 0.6210(2) 0.033 Uiso 1 calc R . C7 C 0.5944(3) 0.8918(2) 0.7449(2) 0.0271(7) Uani 1 d . . C8 C 0.5585(3) 1.0187(2) 0.7309(2) 0.0425(8) Uani 1 d . . H8A H 0.6018(18) 1.0395(6) 0.6860(8) 0.064 Uiso 1 calc R . H8B H 0.5946(19) 1.0723(3) 0.7806(4) 0.064 Uiso 1 calc R . H8C H 0.4560(3) 1.0253(5) 0.7171(12) 0.064 Uiso 1 calc R . C9 C 0.7543(3) 0.8859(2) 0.7622(2) 0.0491(9) Uani 1 d . . H9A H 0.7927(3) 0.9465(12) 0.8074(8) 0.074 Uiso 1 calc R . H9B H 0.7915(3) 0.8992(17) 0.7135(4) 0.074 Uiso 1 calc R . H9C H 0.7817(3) 0.8082(7) 0.7769(13) 0.074 Uiso 1 calc R . C10 C 0.5333(4) 0.8607(2) 0.8168(2) 0.0470(9) Uani 1 d . . H10A H 0.4304(4) 0.8650(16) 0.8047(5) 0.071 Uiso 1 calc R . H10B H 0.5703(16) 0.9164(11) 0.8653(3) 0.071 Uiso 1 calc R . H10C H 0.5597(18) 0.7808(7) 0.8268(8) 0.071 Uiso 1 calc R . C11 C 0.3114(3) 0.3022(2) 0.5320(2) 0.0213(6) Uani 1 d . . C12 C 0.4000(3) 0.2120(2) 0.5563(2) 0.0249(6) Uani 1 d . . H12 H 0.4921(3) 0.2301(2) 0.5864(2) 0.030 Uiso 1 calc R . C13 C 0.3528(3) 0.0963(2) 0.5362(2) 0.0278(7) Uani 1 d . . H13 H 0.4133(3) 0.0357(2) 0.5533(2) 0.033 Uiso 1 calc R . C14 C 0.2209(3) 0.0669(2) 0.4923(2) 0.0333(7) Uani 1 d . . H14 H 0.1900(3) -0.0131(2) 0.4785(2) 0.040 Uiso 1 calc R . C15 C 0.1340(3) 0.1563(2) 0.4685(2) 0.0376(8) Uani 1 d . . H15 H 0.0425(3) 0.1375(2) 0.4379(2) 0.045 Uiso 1 calc R . C16 C 0.1778(3) 0.2721(2) 0.4885(2) 0.0314(7) Uani 1 d . . H16 H 0.1157(3) 0.3321(2) 0.4723(2) 0.038 Uiso 1 calc R . C17 C 1.0250(2) 0.5058(2) 0.8891(2) 0.0155(6) Uani 1 d . . C18 C 1.0573(2) 0.3834(2) 0.8902(2) 0.0172(6) Uani 1 d . . C19 C 1.1787(2) 0.3833(2) 0.9518(2) 0.0192(6) Uani 1 d . . C20 C 1.2602(3) 0.2840(2) 0.9850(2) 0.0276(7) Uani 1 d . . H20A H 1.3051(14) 0.2411(9) 0.9426(3) 0.041 Uiso 1 calc R . H20B H 1.1961(4) 0.2306(8) 1.0028(9) 0.041 Uiso 1 calc R . H20C H 1.3325(12) 0.3153(2) 1.0315(6) 0.041 Uiso 1 calc R . C21 C 0.9773(2) 0.2920(2) 0.8356(2) 0.0185(6) Uani 1 d . . C22 C 1.0257(3) 0.1664(2) 0.8260(2) 0.0226(6) Uani 1 d . . H22A H 0.9443(3) 0.1129(2) 0.8241(2) 0.027 Uiso 1 calc R . H22B H 1.0964(3) 0.1548(2) 0.8744(2) 0.027 Uiso 1 calc R . C23 C 1.0906(3) 0.1323(2) 0.7486(2) 0.0255(6) Uani 1 d . . C24 C 1.2193(3) 0.2097(2) 0.7496(2) 0.0363(7) Uani 1 d . . H24A H 1.2925(8) 0.1972(12) 0.7958(6) 0.055 Uiso 1 calc R . H24B H 1.1930(5) 0.2924(2) 0.7547(12) 0.055 Uiso 1 calc R . H24C H 1.2553(12) 0.1894(11) 0.6987(5) 0.055 Uiso 1 calc R . C25 C 1.1353(3) 0.0037(2) 0.7484(2) 0.0391(8) Uani 1 d . . H25A H 1.2056(16) -0.0031(4) 0.7972(6) 0.059 Uiso 1 calc R . H25B H 1.1760(19) -0.0213(6) 0.6997(6) 0.059 Uiso 1 calc R . H25C H 1.0528(5) -0.0464(3) 0.7481(12) 0.059 Uiso 1 calc R . C26 C 0.9847(3) 0.1421(2) 0.6712(2) 0.0419(8) Uani 1 d . . H26A H 0.8995(8) 0.0955(13) 0.6713(5) 0.063 Uiso 1 calc R . H26B H 1.0260(7) 0.1124(15) 0.6236(2) 0.063 Uiso 1 calc R . H26C H 0.9603(15) 0.2246(3) 0.6690(6) 0.063 Uiso 1 calc R . C27 C 1.1598(3) 0.6895(2) 0.9613(2) 0.0199(6) Uani 1 d . . C28 C 1.0625(3) 0.7703(2) 0.9334(2) 0.0274(7) Uani 1 d . . H28 H 0.9715(3) 0.7442(2) 0.9050(2) 0.033 Uiso 1 calc R . C29 C 1.0983(3) 0.8890(2) 0.9473(2) 0.0371(8) Uani 1 d . . H29 H 1.0311(3) 0.9438(2) 0.9278(2) 0.045 Uiso 1 calc R . C30 C 1.2281(3) 0.9293(2) 0.9883(2) 0.0435(8) Uani 1 d . . H30 H 1.2511(3) 1.0110(2) 0.9977(2) 0.052 Uiso 1 calc R . C31 C 1.3246(3) 0.8493(2) 1.0156(2) 0.0481(9) Uani 1 d . . H31 H 1.4152(3) 0.8762(2) 1.0441(2) 0.058 Uiso 1 calc R . C32 C 1.2918(3) 0.7300(2) 1.0023(2) 0.0358(8) Uani 1 d . . H32 H 1.3601(3) 0.6759(2) 1.0213(2) 0.043 Uiso 1 calc R . C33 C 0.4810(3) 0.4578(3) 0.8673(2) 0.0383(8) Uani 1 d . . H33A H 0.4718(3) 0.4790(3) 0.9251(2) 0.046 Uiso 1 calc R . H33B H 0.4580(3) 0.3728(3) 0.8520(2) 0.046 Uiso 1 calc R . C34 C 0.3807(3) 0.5253(2) 0.8160(2) 0.0341(7) Uani 1 d . . H34A H 0.2843(3) 0.5051(11) 0.8213(8) 0.051 Uiso 1 calc R . H34B H 0.3916(12) 0.5063(11) 0.7590(2) 0.051 Uiso 1 calc R . H34C H 0.3992(11) 0.6096(2) 0.8335(7) 0.051 Uiso 1 calc R . C35 C 1.0240(3) 0.5153(2) 0.6493(2) 0.0379(8) Uani 1 d . . H35A H 1.0449(3) 0.5038(2) 0.5934(2) 0.045 Uiso 1 calc R . H35B H 1.0785(3) 0.4576(2) 0.6802(2) 0.045 Uiso 1 calc R . C36 C 1.0710(3) 0.6364(2) 0.6886(2) 0.0415(8) Uani 1 d . . H36A H 1.1724(5) 0.6463(6) 0.6904(12) 0.062 Uiso 1 calc R . H36B H 1.0511(20) 0.6484(7) 0.7442(5) 0.062 Uiso 1 calc R . H36C H 1.0204(16) 0.6941(3) 0.6570(7) 0.062 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.0143(3) 0.0236(3) 0.0171(3) 0.0016(2) -0.0040(2) 0.0039(2) O1 0.0209(10) 0.0252(9) 0.0210(12) 0.0023(7) -0.0075(8) 0.0040(7) O2 0.0249(10) 0.0244(9) 0.0286(13) 0.0019(8) -0.0123(9) 0.0044(7) O4 0.0176(9) 0.0212(8) 0.0206(12) 0.0026(7) -0.0044(8) 0.0042(7) O3 0.0192(10) 0.0232(9) 0.0279(13) -0.0002(7) -0.0082(9) 0.0037(7) O5 0.0129(10) 0.0487(11) 0.0162(13) 0.0046(9) -0.0039(9) 0.0001(8) O6 0.0201(11) 0.0480(11) 0.0184(14) 0.0079(9) -0.0034(9) -0.0002(8) N1 0.0176(12) 0.0250(11) 0.0161(14) 0.0023(9) -0.0032(10) 0.0047(9) N2 0.0177(11) 0.0270(11) 0.0189(14) 0.0067(9) -0.0020(10) 0.0042(9) N3 0.0145(11) 0.0210(11) 0.0134(13) 0.0023(8) -0.0046(9) 0.0043(8) N4 0.0178(11) 0.0208(11) 0.0154(14) 0.0047(8) -0.0022(10) 0.0061(8) C1 0.0131(13) 0.0263(13) 0.014(2) 0.0036(11) -0.0016(12) 0.0033(10) C2 0.0145(13) 0.0270(13) 0.017(2) 0.0036(10) 0.0016(12) 0.0050(10) C3 0.0200(14) 0.0284(14) 0.019(2) 0.0050(11) 0.0060(12) 0.0051(11) C4 0.0245(15) 0.0340(14) 0.024(2) 0.0075(11) -0.0072(13) 0.0060(11) C5 0.0175(14) 0.0267(13) 0.019(2) 0.0035(11) 0.0012(13) 0.0034(11) C6 0.0260(15) 0.0253(13) 0.028(2) 0.0028(11) -0.0047(13) 0.0059(11) C7 0.0255(15) 0.0223(13) 0.030(2) 0.0014(11) -0.0042(13) 0.0005(11) C8 0.048(2) 0.0260(14) 0.044(2) -0.0012(13) -0.012(2) 0.0069(13) C9 0.031(2) 0.033(2) 0.075(3) 0.0106(15) -0.016(2) -0.0050(13) C10 0.068(2) 0.037(2) 0.034(2) -0.0038(13) 0.009(2) 0.0060(15) C11 0.0214(15) 0.0262(13) 0.016(2) 0.0010(11) 0.0030(12) -0.0011(11) C12 0.0209(14) 0.0292(14) 0.021(2) 0.0003(11) -0.0031(12) 0.0050(11) C13 0.031(2) 0.0252(14) 0.025(2) 0.0019(11) -0.0020(13) 0.0074(11) C14 0.041(2) 0.0246(13) 0.030(2) 0.0011(12) -0.0029(15) -0.0021(12) C15 0.029(2) 0.038(2) 0.037(2) 0.0022(13) -0.0161(14) -0.0075(13) C16 0.023(2) 0.0320(15) 0.034(2) 0.0043(12) -0.0083(13) 0.0030(11) C17 0.0117(13) 0.0220(12) 0.013(2) 0.0036(10) 0.0011(12) 0.0039(10) C18 0.0140(13) 0.0209(12) 0.016(2) 0.0038(10) 0.0002(12) 0.0026(10) C19 0.0174(14) 0.0219(13) 0.019(2) 0.0038(11) 0.0038(12) 0.0021(10) C20 0.027(2) 0.0249(13) 0.025(2) 0.0036(11) -0.0097(13) 0.0046(11) C21 0.0146(14) 0.0232(13) 0.018(2) 0.0045(10) 0.0016(12) 0.0016(10) C22 0.0195(14) 0.0201(12) 0.025(2) 0.0039(11) -0.0049(12) -0.0010(10) C23 0.0234(14) 0.0216(13) 0.029(2) -0.0016(11) -0.0002(13) 0.0021(10) C24 0.033(2) 0.0345(15) 0.042(2) -0.0011(13) 0.0127(15) -0.0033(12) C25 0.034(2) 0.0255(14) 0.055(2) -0.0060(13) 0.008(2) 0.0043(12) C26 0.044(2) 0.049(2) 0.027(2) -0.0073(13) 0.001(2) 0.0068(14) C27 0.0236(14) 0.0180(12) 0.017(2) -0.0002(10) 0.0015(12) 0.0005(10) C28 0.026(2) 0.0234(14) 0.028(2) 0.0008(11) -0.0045(13) 0.0052(11) C29 0.043(2) 0.0230(14) 0.040(2) 0.0038(12) -0.008(2) 0.0089(12) C30 0.055(2) 0.0181(13) 0.050(2) 0.0015(13) -0.009(2) -0.0024(13) C31 0.046(2) 0.027(2) 0.058(3) 0.0007(14) -0.023(2) -0.0093(14) C32 0.031(2) 0.0285(15) 0.040(2) 0.0029(12) -0.0135(14) 0.0047(12) C33 0.018(2) 0.060(2) 0.039(2) 0.0198(14) -0.0007(14) -0.0035(13) C34 0.0193(15) 0.051(2) 0.032(2) 0.0143(13) 0.0009(13) 0.0032(12) C35 0.021(2) 0.053(2) 0.042(2) 0.0116(14) 0.0073(15) 0.0083(13) C36 0.027(2) 0.062(2) 0.035(2) 0.0177(15) -0.0050(15) -0.0093(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca O2 2.290(2) . ? Ca O1 2.291(2) . ? Ca O4 2.293(2) . ? Ca O3 2.310(2) . ? Ca O5 2.345(2) . ? Ca O6 2.368(2) . ? O1 C1 1.262(3) . ? O2 C5 1.244(3) . ? O4 C17 1.254(3) . ? O3 C21 1.245(3) . ? O5 C33 1.428(3) . ? O6 C35 1.436(3) . ? N1 C1 1.378(3) . ? N1 N2 1.396(3) . ? N1 C11 1.420(3) . ? N2 C3 1.315(3) . ? N3 C17 1.380(3) . ? N3 N4 1.394(3) . ? N3 C27 1.419(3) . ? N4 C19 1.320(3) . ? C1 C2 1.432(3) . ? C2 C3 1.425(4) . ? C2 C5 1.429(3) . ? C3 C4 1.500(4) . ? C5 C6 1.518(3) . ? C6 C7 1.543(4) . ? C7 C10 1.518(4) . ? C7 C9 1.522(4) . ? C7 C8 1.536(4) . ? C11 C16 1.384(4) . ? C11 C12 1.400(4) . ? C12 C13 1.381(3) . ? C13 C14 1.371(4) . ? C14 C15 1.381(4) . ? C15 C16 1.374(4) . ? C17 C18 1.441(3) . ? C18 C19 1.421(3) . ? C18 C21 1.426(3) . ? C19 C20 1.498(3) . ? C21 C22 1.513(3) . ? C22 C23 1.548(4) . ? C23 C24 1.523(4) . ? C23 C26 1.524(4) . ? C23 C25 1.538(3) . ? C27 C32 1.385(4) . ? C27 C28 1.386(4) . ? C28 C29 1.385(3) . ? C29 C30 1.367(4) . ? C30 C31 1.372(4) . ? C31 C32 1.384(4) . ? C33 C34 1.472(4) . ? C35 C36 1.492(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ca O1 75.97(6) . . ? O2 Ca O4 98.19(6) . . ? O1 Ca O4 174.15(6) . . ? O2 Ca O3 174.35(6) . . ? O1 Ca O3 109.52(6) . . ? O4 Ca O3 76.33(6) . . ? O2 Ca O5 90.42(7) . . ? O1 Ca O5 94.95(7) . . ? O4 Ca O5 85.00(7) . . ? O3 Ca O5 90.45(7) . . ? O2 Ca O6 85.07(7) . . ? O1 Ca O6 89.33(7) . . ? O4 Ca O6 90.15(7) . . ? O3 Ca O6 93.51(7) . . ? O5 Ca O6 172.86(6) . . ? C1 O1 Ca 129.47(14) . . ? C5 O2 Ca 140.20(15) . . ? C17 O4 Ca 129.78(14) . . ? C21 O3 Ca 138.34(14) . . ? C33 O5 Ca 135.7(2) . . ? C35 O6 Ca 131.2(2) . . ? C1 N1 N2 111.2(2) . . ? C1 N1 C11 129.0(2) . . ? N2 N1 C11 119.7(2) . . ? C3 N2 N1 106.2(2) . . ? C17 N3 N4 111.2(2) . . ? C17 N3 C27 128.8(2) . . ? N4 N3 C27 119.2(2) . . ? C19 N4 N3 106.4(2) . . ? O1 C1 N1 122.8(2) . . ? O1 C1 C2 131.3(2) . . ? N1 C1 C2 105.9(2) . . ? C3 C2 C5 132.7(2) . . ? C3 C2 C1 104.6(2) . . ? C5 C2 C1 122.6(2) . . ? N2 C3 C2 112.2(2) . . ? N2 C3 C4 118.2(2) . . ? C2 C3 C4 129.6(2) . . ? O2 C5 C2 120.2(2) . . ? O2 C5 C6 118.0(2) . . ? C2 C5 C6 121.8(2) . . ? C5 C6 C7 117.3(2) . . ? C10 C7 C9 110.5(3) . . ? C10 C7 C8 109.8(2) . . ? C9 C7 C8 107.0(2) . . ? C10 C7 C6 110.5(2) . . ? C9 C7 C6 111.9(2) . . ? C8 C7 C6 107.0(2) . . ? C16 C11 C12 118.4(2) . . ? C16 C11 N1 120.1(2) . . ? C12 C11 N1 121.5(2) . . ? C13 C12 C11 119.7(2) . . ? C14 C13 C12 121.7(2) . . ? C13 C14 C15 118.3(2) . . ? C16 C15 C14 121.1(3) . . ? C15 C16 C11 120.8(2) . . ? O4 C17 N3 123.1(2) . . ? O4 C17 C18 131.2(2) . . ? N3 C17 C18 105.7(2) . . ? C19 C18 C21 132.9(2) . . ? C19 C18 C17 104.6(2) . . ? C21 C18 C17 122.4(2) . . ? N4 C19 C18 112.2(2) . . ? N4 C19 C20 116.7(2) . . ? C18 C19 C20 131.1(2) . . ? O3 C21 C18 121.2(2) . . ? O3 C21 C22 116.2(2) . . ? C18 C21 C22 122.4(2) . . ? C21 C22 C23 113.7(2) . . ? C24 C23 C26 108.8(2) . . ? C24 C23 C25 109.2(2) . . ? C26 C23 C25 108.8(2) . . ? C24 C23 C22 111.1(2) . . ? C26 C23 C22 111.6(2) . . ? C25 C23 C22 107.2(2) . . ? C32 C27 C28 118.8(2) . . ? C32 C27 N3 119.8(2) . . ? C28 C27 N3 121.4(2) . . ? C29 C28 C27 119.8(2) . . ? C30 C29 C28 121.5(3) . . ? C29 C30 C31 118.7(2) . . ? C30 C31 C32 121.0(3) . . ? C31 C32 C27 120.2(2) . . ? O5 C33 C34 111.5(2) . . ? O6 C35 C36 113.2(2) . . ? _refine_diff_density_max 0.258 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.048