# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author 'Dr. Simon M. Humphrey' _publ_contact_author_email smh@cm.utexas.edu loop_ _publ_author_name 'Ana J. Nunez' 'Lindse N. Shear' 'Naween Dahal' 'Ilich A. Ibarra' 'Ji Woong Yoon' 'Young Kyu Hwang' ; J.-S.Chang ; 'Simon M. Humphrey' data_sh0804 _database_code_depnum_ccdc_archive 'CCDC 827201' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H37 Ca3 N2 O15 P2' _chemical_formula_sum 'C48 H37 Ca3 N2 O15 P2' _chemical_formula_weight 1063.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 '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 orthorhombic _symmetry_space_group_name_H-M Pcca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 23.476(5) _cell_length_b 9.5054(19) _cell_length_c 27.629(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6165(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 63081 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.03 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2196 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.541 _exptl_absorpt_correction_T_max 0.996 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 19685 _diffrn_reflns_av_R_equivalents 0.1269 _diffrn_reflns_av_sigmaI/netI 0.0972 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 23.99 _reflns_number_total 4327 _reflns_number_gt 2862 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.1372P)^2^+2.4325P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4327 _refine_ls_number_parameters 321 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1178 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2360 _refine_ls_wR_factor_gt 0.2172 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.20144(5) 0.34928(14) 0.12792(4) 0.0371(4) Uani 1 1 d . . . Ca2 Ca 0.2500 0.0000 0.10670(5) 0.0329(5) Uani 1 2 d S . . P1 P 0.58372(7) 0.3116(2) 0.16110(5) 0.0453(5) Uani 1 1 d . . . O1 O 0.29779(17) 0.2140(5) 0.12372(15) 0.0526(13) Uani 1 1 d . . . O2 O 0.29905(16) 0.4181(5) 0.16123(13) 0.0405(11) Uani 1 1 d . . . O3 O 0.6836(2) -0.0309(6) -0.03907(15) 0.0586(14) Uani 1 1 d . . . O4 O 0.69751(18) 0.1888(5) -0.06219(14) 0.0497(12) Uani 1 1 d . . . O5 O 0.69655(19) -0.1123(5) 0.33417(14) 0.0585(14) Uani 1 1 d . . . O6 O 0.6360(2) -0.2635(6) 0.30495(18) 0.0756(16) Uani 1 1 d . . . O7 O 0.2500 0.5000 0.06696(17) 0.0437(15) Uani 1 2 d S . . C1 C 0.5063(2) 0.2991(7) 0.15542(18) 0.0393(16) Uani 1 1 d . . . C2 C 0.4749(2) 0.3873(7) 0.18388(19) 0.0399(16) Uani 1 1 d . . . H2A H 0.4939 0.4479 0.2060 0.048 Uiso 1 1 calc R . . C3 C 0.4153(2) 0.3899(7) 0.18111(19) 0.0396(15) Uani 1 1 d . . . H3A H 0.3943 0.4537 0.2006 0.048 Uiso 1 1 calc R . . C4 C 0.3873(2) 0.2996(6) 0.14992(17) 0.0312(14) Uani 1 1 d . . . C5 C 0.4187(3) 0.2097(8) 0.1222(2) 0.0507(18) Uani 1 1 d . . . H5A H 0.3996 0.1453 0.1015 0.061 Uiso 1 1 calc R . . C6 C 0.4767(3) 0.2098(8) 0.1234(2) 0.0523(19) Uani 1 1 d . . . H6A H 0.4974 0.1492 0.1024 0.063 Uiso 1 1 calc R . . C7 C 0.3244(2) 0.3108(7) 0.14510(19) 0.0344(15) Uani 1 1 d . . . C8 C 0.6100(2) 0.2386(8) 0.10331(19) 0.0420(17) Uani 1 1 d . . . C9 C 0.6301(3) 0.3354(7) 0.0699(2) 0.0451(17) Uani 1 1 d . . . H9A H 0.6296 0.4329 0.0775 0.054 Uiso 1 1 calc R . . C10 C 0.6509(3) 0.2917(7) 0.0257(2) 0.0502(18) Uani 1 1 d . . . H10A H 0.6635 0.3594 0.0028 0.060 Uiso 1 1 calc R . . C11 C 0.6536(2) 0.1480(7) 0.01429(18) 0.0371(15) Uani 1 1 d . . . C12 C 0.6330(3) 0.0510(8) 0.0478(2) 0.0500(18) Uani 1 1 d . . . H12A H 0.6331 -0.0466 0.0405 0.060 Uiso 1 1 calc R . . C13 C 0.6121(3) 0.0985(8) 0.0919(2) 0.055(2) Uani 1 1 d . . . H13A H 0.5988 0.0317 0.1149 0.066 Uiso 1 1 calc R . . C14 C 0.6795(3) 0.0994(8) -0.0313(2) 0.0418(16) Uani 1 1 d . . . C15 C 0.6008(2) 0.1709(7) 0.20466(18) 0.0421(17) Uani 1 1 d . . . C16 C 0.6534(3) 0.1815(7) 0.2278(2) 0.0464(17) Uani 1 1 d . . . H16A H 0.6776 0.2590 0.2208 0.056 Uiso 1 1 calc R . . C17 C 0.6708(3) 0.0813(7) 0.26065(19) 0.0424(16) Uani 1 1 d . . . H17A H 0.7068 0.0906 0.2761 0.051 Uiso 1 1 calc R . . C18 C 0.6367(2) -0.0318(7) 0.27132(18) 0.0350(15) Uani 1 1 d . . . C19 C 0.5839(3) -0.0451(8) 0.2493(2) 0.058(2) Uani 1 1 d . . . H19A H 0.5602 -0.1234 0.2562 0.070 Uiso 1 1 calc R . . C20 C 0.5659(3) 0.0607(8) 0.2160(2) 0.057(2) Uani 1 1 d . . . H20A H 0.5292 0.0545 0.2016 0.068 Uiso 1 1 calc R . . C21 C 0.6574(3) -0.1424(9) 0.30541(19) 0.0469(18) Uani 1 1 d . . . N100 N 0.0257(4) 0.3258(15) 0.0749(6) 0.193(7) Uani 1 1 d D . . C101 C 0.0348(10) 0.186(2) 0.0880(13) 0.39(2) Uani 1 1 d D . . H10B H 0.0756 0.1699 0.0931 0.585 Uiso 1 1 calc R . . H10C H 0.0212 0.1238 0.0621 0.585 Uiso 1 1 calc R . . H10D H 0.0141 0.1651 0.1179 0.585 Uiso 1 1 calc R . . C102 C -0.0286(9) 0.360(3) 0.0599(14) 0.45(2) Uani 1 1 d D . . H10E H -0.0282 0.4524 0.0443 0.673 Uiso 1 1 calc R . . H10F H -0.0541 0.3623 0.0880 0.673 Uiso 1 1 calc R . . H10G H -0.0421 0.2890 0.0369 0.673 Uiso 1 1 calc R . . C100 C 0.0693(5) 0.4190(13) 0.0770(4) 0.122(4) Uani 1 1 d D . . H10X H 0.0618 0.5087 0.0632 0.10(7) Uiso 0.50 1 calc PR . . O100 O 0.1149(2) 0.4042(7) 0.09344(18) 0.0837(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0348(7) 0.0358(10) 0.0407(7) -0.0032(5) 0.0003(5) 0.0001(6) Ca2 0.0342(9) 0.0350(12) 0.0293(8) 0.000 0.000 0.0025(9) P1 0.0357(9) 0.0607(14) 0.0395(8) -0.0006(8) 0.0023(6) 0.0132(9) O1 0.037(3) 0.055(4) 0.066(3) -0.015(2) 0.0021(19) -0.003(2) O2 0.035(2) 0.038(3) 0.048(2) -0.001(2) 0.0046(17) 0.006(2) O3 0.082(4) 0.040(4) 0.054(3) 0.000(2) 0.031(2) -0.002(3) O4 0.064(3) 0.048(3) 0.037(2) 0.004(2) 0.0126(19) 0.008(2) O5 0.070(3) 0.056(4) 0.049(2) 0.006(2) -0.030(2) -0.018(3) O6 0.081(4) 0.051(4) 0.096(4) 0.014(3) -0.044(3) -0.023(3) O7 0.050(4) 0.048(4) 0.034(3) 0.000 0.000 -0.001(3) C1 0.037(3) 0.046(5) 0.035(3) -0.006(3) -0.010(2) 0.011(3) C2 0.028(3) 0.055(5) 0.037(3) -0.009(3) -0.006(2) 0.002(3) C3 0.045(4) 0.034(4) 0.040(3) 0.003(3) 0.002(3) 0.005(3) C4 0.031(3) 0.028(4) 0.035(3) 0.000(3) -0.003(2) -0.008(3) C5 0.041(4) 0.057(5) 0.054(4) -0.022(3) -0.005(3) 0.006(4) C6 0.039(4) 0.067(6) 0.051(4) -0.018(3) 0.002(3) 0.014(4) C7 0.036(3) 0.034(5) 0.033(3) -0.003(3) -0.002(2) 0.001(3) C8 0.030(3) 0.053(6) 0.042(3) 0.002(3) 0.002(2) 0.016(3) C9 0.062(4) 0.027(4) 0.047(3) 0.006(3) 0.006(3) 0.010(4) C10 0.075(5) 0.031(5) 0.044(3) 0.010(3) 0.008(3) 0.000(4) C11 0.040(4) 0.037(5) 0.034(3) 0.006(3) 0.001(2) 0.008(3) C12 0.062(4) 0.038(5) 0.050(4) 0.000(3) 0.024(3) 0.012(4) C13 0.069(5) 0.054(6) 0.043(3) 0.010(3) 0.020(3) 0.004(4) C14 0.045(4) 0.045(5) 0.036(3) 0.004(3) 0.004(3) 0.003(4) C15 0.033(3) 0.063(5) 0.031(3) 0.004(3) 0.004(2) 0.017(4) C16 0.044(4) 0.054(5) 0.041(3) 0.002(3) 0.002(3) -0.004(4) C17 0.036(3) 0.051(5) 0.040(3) 0.009(3) -0.014(3) -0.003(4) C18 0.038(3) 0.033(4) 0.034(3) 0.003(3) 0.000(2) -0.002(3) C19 0.040(4) 0.075(6) 0.060(4) 0.013(4) -0.006(3) -0.022(4) C20 0.034(4) 0.068(6) 0.068(4) 0.022(4) -0.011(3) -0.010(4) C21 0.039(4) 0.070(6) 0.032(3) -0.010(3) 0.000(3) 0.003(4) N100 0.058(6) 0.195(14) 0.326(17) -0.102(13) -0.072(8) -0.012(8) C101 0.23(3) 0.24(3) 0.70(6) 0.24(4) 0.04(3) -0.09(2) C102 0.20(3) 0.37(4) 0.77(7) -0.07(4) -0.27(3) 0.04(3) C100 0.113(10) 0.091(10) 0.161(10) -0.042(8) -0.057(8) 0.034(8) O100 0.051(3) 0.116(5) 0.084(3) -0.036(3) -0.021(3) 0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 O100 2.304(5) . ? Ca1 O4 2.373(4) 6 ? Ca1 O2 2.395(5) 2_565 ? Ca1 O5 2.487(5) 4_455 ? Ca1 O7 2.488(3) . ? Ca1 O6 2.542(5) 4_455 ? Ca1 O2 2.555(4) . ? Ca1 O1 2.604(4) . ? Ca1 C21 2.886(7) 4_455 ? Ca1 C7 2.948(6) . ? Ca1 Ca2 3.5589(15) . ? Ca1 Ca1 3.662(3) 2_565 ? Ca2 O5 2.320(4) 3_655 ? Ca2 O5 2.320(4) 4_455 ? Ca2 O1 2.370(5) . ? Ca2 O1 2.370(5) 2 ? Ca2 O3 2.450(4) 6 ? Ca2 O3 2.450(4) 5_655 ? Ca2 O4 2.501(4) 5_655 ? Ca2 O4 2.501(4) 6 ? Ca2 C14 2.823(6) 5_655 ? Ca2 C14 2.823(6) 6 ? Ca2 Ca1 3.5589(15) 2 ? P1 C1 1.829(6) . ? P1 C15 1.843(6) . ? P1 C8 1.847(6) . ? O1 C7 1.260(7) . ? O2 C7 1.262(7) . ? O2 Ca1 2.395(5) 2_565 ? O3 C14 1.260(8) . ? O3 Ca2 2.450(4) 5_655 ? O4 C14 1.277(7) . ? O4 Ca1 2.373(4) 6_655 ? O4 Ca2 2.501(4) 5_655 ? O5 C21 1.248(7) . ? O5 Ca2 2.320(4) 3_655 ? O5 Ca1 2.487(5) 4 ? O6 C21 1.255(8) . ? O6 Ca1 2.542(5) 4 ? O7 Ca1 2.488(3) 2_565 ? C1 C2 1.364(8) . ? C1 C6 1.409(9) . ? C2 C3 1.401(8) . ? C2 H2A 0.9500 . ? C3 C4 1.383(8) . ? C3 H3A 0.9500 . ? C4 C5 1.365(8) . ? C4 C7 1.486(8) . ? C5 C6 1.362(9) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C8 C13 1.369(10) . ? C8 C9 1.386(9) . ? C9 C10 1.378(8) . ? C9 H9A 0.9500 . ? C10 C11 1.404(9) . ? C10 H10A 0.9500 . ? C11 C12 1.393(8) . ? C11 C14 1.473(8) . ? C12 C13 1.390(8) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 Ca2 2.823(6) 5_655 ? C15 C20 1.366(9) . ? C15 C16 1.395(8) . ? C16 C17 1.377(8) . ? C16 H16A 0.9500 . ? C17 C18 1.372(8) . ? C17 H17A 0.9500 . ? C18 C19 1.387(8) . ? C18 C21 1.493(9) . ? C19 C20 1.426(9) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 Ca1 2.886(7) 4 ? N100 C100 1.353(14) . ? N100 C102 1.380(16) . ? N100 C101 1.396(17) . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C101 H10D 0.9800 . ? C102 H10E 0.9800 . ? C102 H10F 0.9800 . ? C102 H10G 0.9800 . ? C100 O100 1.172(11) . ? C100 H10X 0.9500 . ? 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 O100 Ca1 O4 78.18(17) . 6 ? O100 Ca1 O2 86.87(18) . 2_565 ? O4 Ca1 O2 152.52(15) 6 2_565 ? O100 Ca1 O5 109.8(2) . 4_455 ? O4 Ca1 O5 74.84(15) 6 4_455 ? O2 Ca1 O5 132.39(14) 2_565 4_455 ? O100 Ca1 O7 89.64(17) . . ? O4 Ca1 O7 82.52(13) 6 . ? O2 Ca1 O7 74.37(12) 2_565 . ? O5 Ca1 O7 145.89(10) 4_455 . ? O100 Ca1 O6 80.9(2) . 4_455 ? O4 Ca1 O6 109.19(18) 6 4_455 ? O2 Ca1 O6 90.74(16) 2_565 4_455 ? O5 Ca1 O6 51.26(16) 4_455 4_455 ? O7 Ca1 O6 162.83(14) . 4_455 ? O100 Ca1 O2 151.9(2) . . ? O4 Ca1 O2 118.36(15) 6 . ? O2 Ca1 O2 68.25(17) 2_565 . ? O5 Ca1 O2 96.97(15) 4_455 . ? O7 Ca1 O2 71.67(11) . . ? O6 Ca1 O2 111.16(16) 4_455 . ? O100 Ca1 O1 149.25(17) . . ? O4 Ca1 O1 71.48(14) 6 . ? O2 Ca1 O1 118.49(14) 2_565 . ? O5 Ca1 O1 67.15(15) 4_455 . ? O7 Ca1 O1 81.73(11) . . ? O6 Ca1 O1 113.50(17) 4_455 . ? O2 Ca1 O1 50.46(14) . . ? O100 Ca1 C21 95.9(2) . 4_455 ? O4 Ca1 C21 92.10(17) 6 4_455 ? O2 Ca1 C21 112.46(17) 2_565 4_455 ? O5 Ca1 C21 25.51(17) 4_455 4_455 ? O7 Ca1 C21 171.38(16) . 4_455 ? O6 Ca1 C21 25.76(16) 4_455 4_455 ? O2 Ca1 C21 105.41(15) . 4_455 ? O1 Ca1 C21 90.18(18) . 4_455 ? O100 Ca1 C7 163.37(19) . . ? O4 Ca1 C7 94.68(16) 6 . ? O2 Ca1 C7 93.28(17) 2_565 . ? O5 Ca1 C7 82.24(17) 4_455 . ? O7 Ca1 C7 74.44(12) . . ? O6 Ca1 C7 115.73(17) 4_455 . ? O2 Ca1 C7 25.23(14) . . ? O1 Ca1 C7 25.26(15) . . ? C21 Ca1 C7 99.41(18) 4_455 . ? O100 Ca1 Ca2 115.21(15) . . ? O4 Ca1 Ca2 44.51(10) 6 . ? O2 Ca1 Ca2 157.83(10) 2_565 . ? O5 Ca1 Ca2 40.47(9) 4_455 . ? O7 Ca1 Ca2 106.20(6) . . ? O6 Ca1 Ca2 90.83(13) 4_455 . ? O2 Ca1 Ca2 90.62(11) . . ? O1 Ca1 Ca2 41.74(11) . . ? C21 Ca1 Ca2 65.44(15) 4_455 . ? C7 Ca1 Ca2 66.25(13) . . ? O100 Ca1 Ca1 111.82(18) . 2_565 ? O4 Ca1 Ca1 121.81(11) 6 2_565 ? O2 Ca1 Ca1 43.99(9) 2_565 2_565 ? O5 Ca1 Ca1 137.52(12) 4_455 2_565 ? O7 Ca1 Ca1 42.61(8) . 2_565 ? O6 Ca1 Ca1 128.84(14) 4_455 2_565 ? O2 Ca1 Ca1 40.64(10) . 2_565 ? O1 Ca1 Ca1 81.12(12) . 2_565 ? C21 Ca1 Ca1 139.13(11) 4_455 2_565 ? C7 Ca1 Ca1 59.16(13) . 2_565 ? Ca2 Ca1 Ca1 122.04(5) . 2_565 ? O5 Ca2 O5 90.5(2) 3_655 4_455 ? O5 Ca2 O1 89.95(17) 3_655 . ? O5 Ca2 O1 73.82(16) 4_455 . ? O5 Ca2 O1 73.82(16) 3_655 2 ? O5 Ca2 O1 89.95(17) 4_455 2 ? O1 Ca2 O1 157.1(2) . 2 ? O5 Ca2 O3 145.66(17) 3_655 6 ? O5 Ca2 O3 104.37(17) 4_455 6 ? O1 Ca2 O3 123.71(17) . 6 ? O1 Ca2 O3 75.38(16) 2 6 ? O5 Ca2 O3 104.37(17) 3_655 5_655 ? O5 Ca2 O3 145.66(17) 4_455 5_655 ? O1 Ca2 O3 75.38(16) . 5_655 ? O1 Ca2 O3 123.71(17) 2 5_655 ? O3 Ca2 O3 80.6(2) 6 5_655 ? O5 Ca2 O4 75.50(14) 3_655 5_655 ? O5 Ca2 O4 160.58(16) 4_455 5_655 ? O1 Ca2 O4 118.71(15) . 5_655 ? O1 Ca2 O4 73.43(15) 2 5_655 ? O3 Ca2 O4 81.51(16) 6 5_655 ? O3 Ca2 O4 52.96(16) 5_655 5_655 ? O5 Ca2 O4 160.58(16) 3_655 6 ? O5 Ca2 O4 75.50(14) 4_455 6 ? O1 Ca2 O4 73.43(15) . 6 ? O1 Ca2 O4 118.71(15) 2 6 ? O3 Ca2 O4 52.96(16) 6 6 ? O3 Ca2 O4 81.51(16) 5_655 6 ? O4 Ca2 O4 121.08(19) 5_655 6 ? O5 Ca2 C14 92.81(17) 3_655 5_655 ? O5 Ca2 C14 172.1(2) 4_455 5_655 ? O1 Ca2 C14 98.99(18) . 5_655 ? O1 Ca2 C14 97.85(19) 2 5_655 ? O3 Ca2 C14 76.68(17) 6 5_655 ? O3 Ca2 C14 26.46(16) 5_655 5_655 ? O4 Ca2 C14 26.89(17) 5_655 5_655 ? O4 Ca2 C14 99.55(17) 6 5_655 ? O5 Ca2 C14 172.1(2) 3_655 6 ? O5 Ca2 C14 92.81(17) 4_455 6 ? O1 Ca2 C14 97.85(19) . 6 ? O1 Ca2 C14 98.99(18) 2 6 ? O3 Ca2 C14 26.46(16) 6 6 ? O3 Ca2 C14 76.68(17) 5_655 6 ? O4 Ca2 C14 99.55(17) 5_655 6 ? O4 Ca2 C14 26.89(17) 6 6 ? C14 Ca2 C14 84.9(2) 5_655 6 ? O5 Ca2 Ca1 119.11(12) 3_655 . ? O5 Ca2 Ca1 44.08(12) 4_455 . ? O1 Ca2 Ca1 47.02(10) . . ? O1 Ca2 Ca1 128.05(11) 2 . ? O3 Ca2 Ca1 91.93(13) 6 . ? O3 Ca2 Ca1 102.57(13) 5_655 . ? O4 Ca2 Ca1 155.30(11) 5_655 . ? O4 Ca2 Ca1 41.71(10) 6 . ? C14 Ca2 Ca1 128.41(16) 5_655 . ? C14 Ca2 Ca1 67.78(15) 6 . ? O5 Ca2 Ca1 44.08(12) 3_655 2 ? O5 Ca2 Ca1 119.11(12) 4_455 2 ? O1 Ca2 Ca1 128.05(11) . 2 ? O1 Ca2 Ca1 47.02(10) 2 2 ? O3 Ca2 Ca1 102.57(13) 6 2 ? O3 Ca2 Ca1 91.93(13) 5_655 2 ? O4 Ca2 Ca1 41.71(10) 5_655 2 ? O4 Ca2 Ca1 155.30(11) 6 2 ? C14 Ca2 Ca1 67.78(15) 5_655 2 ? C14 Ca2 Ca1 128.41(16) 6 2 ? Ca1 Ca2 Ca1 161.04(6) . 2 ? C1 P1 C15 103.0(3) . . ? C1 P1 C8 103.5(3) . . ? C15 P1 C8 102.7(3) . . ? C7 O1 Ca2 162.7(4) . . ? C7 O1 Ca1 92.8(4) . . ? Ca2 O1 Ca1 91.23(14) . . ? C7 O2 Ca1 127.8(3) . 2_565 ? C7 O2 Ca1 95.1(3) . . ? Ca1 O2 Ca1 95.37(14) 2_565 . ? C14 O3 Ca2 93.5(3) . 5_655 ? C14 O4 Ca1 162.3(4) . 6_655 ? C14 O4 Ca2 90.8(4) . 5_655 ? Ca1 O4 Ca2 93.77(13) 6_655 5_655 ? C21 O5 Ca2 162.2(5) . 3_655 ? C21 O5 Ca1 95.4(4) . 4 ? Ca2 O5 Ca1 95.46(14) 3_655 4 ? C21 O6 Ca1 92.6(4) . 4 ? Ca1 O7 Ca1 94.78(17) 2_565 . ? C2 C1 C6 117.8(5) . . ? C2 C1 P1 116.5(4) . . ? C6 C1 P1 125.6(5) . . ? C1 C2 C3 121.2(5) . . ? C1 C2 H2A 119.4 . . ? C3 C2 H2A 119.4 . . ? C4 C3 C2 119.9(6) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C5 C4 C3 118.8(5) . . ? C5 C4 C7 122.1(5) . . ? C3 C4 C7 119.0(5) . . ? C6 C5 C4 121.8(6) . . ? C6 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C5 C6 C1 120.5(6) . . ? C5 C6 H6A 119.7 . . ? C1 C6 H6A 119.7 . . ? O1 C7 O2 121.5(5) . . ? O1 C7 C4 118.8(6) . . ? O2 C7 C4 119.7(5) . . ? O1 C7 Ca1 61.9(3) . . ? O2 C7 Ca1 59.7(3) . . ? C4 C7 Ca1 174.9(4) . . ? C13 C8 C9 118.7(5) . . ? C13 C8 P1 125.1(5) . . ? C9 C8 P1 116.1(5) . . ? C10 C9 C8 120.7(6) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C9 C10 C11 120.6(6) . . ? C9 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 . . ? C12 C11 C10 118.6(5) . . ? C12 C11 C14 120.3(6) . . ? C10 C11 C14 121.1(6) . . ? C13 C12 C11 119.4(7) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C8 C13 C12 122.0(6) . . ? C8 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? O3 C14 O4 121.0(5) . . ? O3 C14 C11 119.1(6) . . ? O4 C14 C11 120.0(6) . . ? O3 C14 Ca2 60.0(3) . 5_655 ? O4 C14 Ca2 62.3(3) . 5_655 ? C11 C14 Ca2 168.0(4) . 5_655 ? C20 C15 C16 118.8(6) . . ? C20 C15 P1 125.1(5) . . ? C16 C15 P1 116.1(5) . . ? C17 C16 C15 121.0(6) . . ? C17 C16 H16A 119.5 . . ? C15 C16 H16A 119.5 . . ? C18 C17 C16 120.7(6) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C17 C18 C19 119.9(6) . . ? C17 C18 C21 119.8(5) . . ? C19 C18 C21 120.2(6) . . ? C18 C19 C20 118.9(6) . . ? C18 C19 H19A 120.5 . . ? C20 C19 H19A 120.5 . . ? C15 C20 C19 120.7(6) . . ? C15 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? O5 C21 O6 120.7(6) . . ? O5 C21 C18 118.6(7) . . ? O6 C21 C18 120.6(5) . . ? O5 C21 Ca1 59.1(4) . 4 ? O6 C21 Ca1 61.7(4) . 4 ? C18 C21 Ca1 177.6(5) . 4 ? C100 N100 C102 123.9(14) . . ? C100 N100 C101 119.8(11) . . ? C102 N100 C101 116.3(12) . . ? N100 C101 H10B 109.5 . . ? N100 C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? N100 C101 H10D 109.5 . . ? H10B C101 H10D 109.5 . . ? H10C C101 H10D 109.5 . . ? N100 C102 H10E 109.5 . . ? N100 C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? N100 C102 H10G 109.5 . . ? H10E C102 H10G 109.5 . . ? H10F C102 H10G 109.5 . . ? O100 C100 N100 128.9(12) . . ? O100 C100 H10X 115.5 . . ? N100 C100 H10X 115.5 . . ? C100 O100 Ca1 173.4(9) . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 1.431 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.087 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.750 -0.029 0.130 397 171 ' ' 2 0.250 -0.026 0.370 399 171 ' ' 3 0.750 -0.030 0.630 397 172 ' ' 4 0.250 -0.026 0.870 399 172 ' ' 5 0.500 0.000 0.000 46 13 ' ' 6 1.000 0.000 0.000 46 14 ' ' 7 0.500 0.000 0.500 46 13 ' ' 8 0.000 0.000 0.500 46 14 ' ' 9 0.000 0.335 0.250 2 1 ' ' 10 0.500 0.335 0.750 2 1 ' ' 11 0.500 0.665 0.250 2 1 ' ' 12 0.000 0.665 0.750 2 1 ' ' _platon_squeeze_details ; ;