# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Michael Hill' _publ_contact_author_email M.S.HILL@BATH.AC.UK _publ_section_title ; Calcium-Centred Phosphine Oxide Reactivity: Sequential P-C Metathesis, Reduction and P-P Dehydrocoupling ; _publ_author_name 'Michael Hill' # Attachment 'bigcif_compounds1_3.CIF' data_k09msh10-(Compound_1) _database_code_depnum_ccdc_archive 'CCDC 749969' #TrackingRef 'bigcif_compounds1_3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H80 Ca O2 P2 Si4' _chemical_formula_weight 1071.64 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' Si Si 0.0817 0.0704 '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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.5254(5) _cell_length_b 11.7454(2) _cell_length_c 23.6923(5) _cell_angle_alpha 90.00 _cell_angle_beta 122.870(1) _cell_angle_gamma 90.00 _cell_volume 6199.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 38901 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.003 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 0.270 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.569 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31751 _diffrn_reflns_av_R_equivalents 0.1448 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5430 _reflns_number_gt 4255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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^)+(0.0572P)^2^+4.9705P] 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 5430 _refine_ls_number_parameters 327 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.055 _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 C1 C -0.05660(10) 0.34821(17) 0.14459(11) 0.0241(5) Uani 1 1 d D . . H1 H -0.0326 0.2763 0.1593 0.029 Uiso 1 1 calc RD . . C2 C -0.07151(19) 0.2708(3) 0.00948(17) 0.0677(10) Uani 1 1 d . . . H2A H -0.0424 0.2091 0.0321 0.101 Uiso 1 1 calc R . . H2B H -0.0688 0.3005 -0.0274 0.101 Uiso 1 1 calc R . . H2C H -0.1121 0.2416 -0.0085 0.101 Uiso 1 1 calc R . . C3 C 0.02220(13) 0.4367(3) 0.09608(15) 0.0492(7) Uani 1 1 d . . . H3A H 0.0350 0.4998 0.1281 0.074 Uiso 1 1 calc R . . H3B H 0.0211 0.4622 0.0560 0.074 Uiso 1 1 calc R . . H3C H 0.0506 0.3734 0.1170 0.074 Uiso 1 1 calc R . . C4 C -0.10741(17) 0.5069(3) 0.02141(18) 0.0679(10) Uani 1 1 d . . . H4A H -0.1488 0.4831 0.0041 0.102 Uiso 1 1 calc R . . H4B H -0.1034 0.5260 -0.0162 0.102 Uiso 1 1 calc R . . H4C H -0.0976 0.5738 0.0503 0.102 Uiso 1 1 calc R . . C5 C -0.16869(13) 0.1829(2) 0.07279(19) 0.0577(9) Uani 1 1 d . . . H5A H -0.1783 0.2051 0.0281 0.087 Uiso 1 1 calc R . . H5B H -0.2059 0.1673 0.0709 0.087 Uiso 1 1 calc R . . H5C H -0.1437 0.1142 0.0875 0.087 Uiso 1 1 calc R . . C6 C -0.18377(11) 0.4193(2) 0.10481(15) 0.0419(6) Uani 1 1 d . . . H6A H -0.1656 0.4855 0.1343 0.063 Uiso 1 1 calc R . . H6B H -0.2181 0.3929 0.1062 0.063 Uiso 1 1 calc R . . H6C H -0.1973 0.4405 0.0586 0.063 Uiso 1 1 calc R . . C7 C -0.11313(13) 0.2509(3) 0.21677(16) 0.0582(9) Uani 1 1 d . . . H7A H -0.0857 0.1857 0.2328 0.087 Uiso 1 1 calc R . . H7B H -0.1513 0.2279 0.2106 0.087 Uiso 1 1 calc R . . H7C H -0.0953 0.3125 0.2499 0.087 Uiso 1 1 calc R . . C8 C 0.14633(10) 0.65976(18) 0.21935(11) 0.0245(5) Uani 1 1 d . . . C9 C 0.17068(11) 0.55010(19) 0.23466(12) 0.0309(5) Uani 1 1 d . . . H9 H 0.1572 0.4959 0.2534 0.037 Uiso 1 1 calc R . . C10 C 0.21443(12) 0.5206(2) 0.22242(14) 0.0400(6) Uani 1 1 d . . . H10 H 0.2309 0.4460 0.2329 0.048 Uiso 1 1 calc R . . C11 C 0.23404(12) 0.5983(2) 0.19533(14) 0.0423(7) Uani 1 1 d . . . H11 H 0.2645 0.5776 0.1876 0.051 Uiso 1 1 calc R . . C12 C 0.20979(12) 0.7069(2) 0.17907(14) 0.0404(6) Uani 1 1 d . . . H12 H 0.2231 0.7601 0.1597 0.048 Uiso 1 1 calc R . . C13 C 0.16615(11) 0.7373(2) 0.19113(13) 0.0329(5) Uani 1 1 d . . . H13 H 0.1495 0.8118 0.1801 0.039 Uiso 1 1 calc R . . C14 C 0.13653(10) 0.76865(17) 0.32213(11) 0.0243(5) Uani 1 1 d . . . C15 C 0.17834(11) 0.8531(2) 0.33492(13) 0.0347(6) Uani 1 1 d . . . H15 H 0.1839 0.8766 0.3003 0.042 Uiso 1 1 calc R . . C16 C 0.21160(12) 0.9026(2) 0.39748(14) 0.0427(6) Uani 1 1 d . . . H16 H 0.2401 0.9600 0.4058 0.051 Uiso 1 1 calc R . . C17 C 0.20389(12) 0.8697(2) 0.44802(14) 0.0387(6) Uani 1 1 d . . . H17 H 0.2271 0.9039 0.4912 0.046 Uiso 1 1 calc R . . C18 C 0.16211(12) 0.7865(2) 0.43569(13) 0.0382(6) Uani 1 1 d . . . H18 H 0.1564 0.7641 0.4703 0.046 Uiso 1 1 calc R . . C19 C 0.12875(11) 0.73615(19) 0.37310(12) 0.0328(5) Uani 1 1 d . . . H19 H 0.1003 0.6788 0.3650 0.039 Uiso 1 1 calc R . . C20 C 0.04362(10) 0.80313(17) 0.18164(12) 0.0259(5) Uani 1 1 d . . . C21 C 0.03260(10) 0.90619(19) 0.20198(13) 0.0336(5) Uani 1 1 d . . . H21 H 0.0537 0.9253 0.2483 0.040 Uiso 1 1 calc R . . C22 C -0.00964(12) 0.9814(2) 0.15375(15) 0.0427(7) Uani 1 1 d . . . H22 H -0.0174 1.0517 0.1675 0.051 Uiso 1 1 calc R . . C23 C -0.03997(12) 0.9545(2) 0.08689(15) 0.0432(7) Uani 1 1 d . . . H23 H -0.0688 1.0059 0.0545 0.052 Uiso 1 1 calc R . . C24 C -0.02869(12) 0.8523(2) 0.06633(14) 0.0434(6) Uani 1 1 d . . . H24 H -0.0495 0.8342 0.0199 0.052 Uiso 1 1 calc R . . C25 C 0.01286(11) 0.7766(2) 0.11353(13) 0.0347(6) Uani 1 1 d . . . H25 H 0.0204 0.7065 0.0994 0.042 Uiso 1 1 calc R . . C26 C 0.14211(16) 0.2042(3) 0.14074(19) 0.0700(10) Uani 1 1 d . . . H26 H 0.1348 0.2694 0.1590 0.084 Uiso 1 1 calc R . . C27 C 0.10823(16) 0.1102(5) 0.12732(19) 0.0858(14) Uani 1 1 d . . . H27 H 0.0773 0.1088 0.1361 0.103 Uiso 1 1 calc R . . C28 C 0.1194(2) 0.0151(3) 0.1003(2) 0.0898(16) Uani 1 1 d . . . H28 H 0.0959 -0.0519 0.0899 0.108 Uiso 1 1 calc R . . C29 C 0.16489(18) 0.0200(3) 0.08916(18) 0.0756(12) Uani 1 1 d . . . H29 H 0.1733 -0.0440 0.0711 0.091 Uiso 1 1 calc R . . C30 C 0.19762(14) 0.1155(3) 0.10379(15) 0.0560(8) Uani 1 1 d . . . H30 H 0.2295 0.1186 0.0965 0.067 Uiso 1 1 calc R . . C31 C 0.18539(14) 0.2068(3) 0.12878(17) 0.0556(8) Uani 1 1 d . . . H31 H 0.2083 0.2744 0.1380 0.067 Uiso 1 1 calc R . . Si1 Si -0.05479(3) 0.38802(5) 0.07130(3) 0.02985(18) Uani 1 1 d . . . Si2 Si -0.12672(3) 0.30190(5) 0.13410(3) 0.02866(18) Uani 1 1 d . . . O1 O 0.06161(7) 0.59691(12) 0.24532(8) 0.0278(4) Uani 1 1 d . . . P1 P 0.09385(2) 0.69897(4) 0.24181(3) 0.02244(16) Uani 1 1 d . . . Ca1 Ca 0.0000 0.46958(5) 0.2500 0.01951(16) Uani 1 2 d S . . 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 C1 0.0232(11) 0.0195(10) 0.0223(12) -0.0037(9) 0.0076(10) -0.0004(8) C2 0.104(3) 0.0623(19) 0.049(2) -0.0266(16) 0.049(2) -0.029(2) C3 0.0489(17) 0.0600(18) 0.0445(18) 0.0033(14) 0.0292(16) -0.0039(14) C4 0.071(2) 0.087(2) 0.056(2) 0.0371(19) 0.041(2) 0.0397(19) C5 0.0389(16) 0.0368(14) 0.082(2) -0.0229(15) 0.0228(17) -0.0153(12) C6 0.0305(14) 0.0407(14) 0.0496(17) -0.0067(12) 0.0185(14) 0.0018(11) C7 0.0361(16) 0.083(2) 0.053(2) 0.0211(17) 0.0222(16) -0.0079(15) C8 0.0223(11) 0.0244(11) 0.0245(12) -0.0040(9) 0.0112(10) -0.0041(9) C9 0.0317(13) 0.0249(11) 0.0322(14) -0.0004(10) 0.0148(12) 0.0015(9) C10 0.0399(15) 0.0325(13) 0.0446(17) -0.0067(11) 0.0210(14) 0.0059(11) C11 0.0356(14) 0.0504(16) 0.0483(17) -0.0137(13) 0.0275(14) -0.0017(12) C12 0.0427(15) 0.0443(15) 0.0455(17) 0.0000(12) 0.0313(15) -0.0039(12) C13 0.0329(13) 0.0307(12) 0.0361(15) 0.0047(10) 0.0193(13) 0.0013(10) C14 0.0236(11) 0.0215(10) 0.0259(12) -0.0001(9) 0.0121(11) 0.0025(9) C15 0.0390(14) 0.0318(12) 0.0338(15) -0.0050(11) 0.0201(13) -0.0110(11) C16 0.0441(16) 0.0365(14) 0.0440(17) -0.0103(12) 0.0217(14) -0.0152(12) C17 0.0422(15) 0.0326(13) 0.0337(15) -0.0088(11) 0.0157(13) -0.0040(11) C18 0.0468(16) 0.0389(14) 0.0289(14) -0.0013(11) 0.0205(13) -0.0027(12) C19 0.0353(13) 0.0286(12) 0.0319(14) -0.0019(10) 0.0166(12) -0.0063(10) C20 0.0212(11) 0.0247(11) 0.0294(13) 0.0044(9) 0.0121(11) 0.0005(9) C21 0.0297(13) 0.0307(12) 0.0340(14) 0.0017(10) 0.0131(12) 0.0028(10) C22 0.0370(15) 0.0327(13) 0.0533(19) 0.0085(12) 0.0212(15) 0.0090(11) C23 0.0312(14) 0.0407(15) 0.0456(18) 0.0183(13) 0.0129(14) 0.0082(11) C24 0.0359(14) 0.0500(16) 0.0298(15) 0.0075(12) 0.0085(13) 0.0027(12) C25 0.0337(13) 0.0347(13) 0.0297(14) 0.0026(11) 0.0133(12) 0.0021(11) C26 0.052(2) 0.088(3) 0.058(2) -0.0222(19) 0.0222(19) 0.0155(19) C27 0.0390(19) 0.170(5) 0.048(2) 0.028(3) 0.0238(18) -0.005(3) C28 0.065(3) 0.062(2) 0.065(3) 0.038(2) -0.015(2) -0.030(2) C29 0.065(2) 0.057(2) 0.045(2) -0.0125(16) -0.0093(19) 0.0318(19) C30 0.0397(17) 0.094(3) 0.0314(17) -0.0008(16) 0.0174(15) 0.0104(17) C31 0.0499(18) 0.0489(17) 0.056(2) 0.0022(15) 0.0212(17) -0.0064(14) Si1 0.0340(4) 0.0289(3) 0.0231(4) -0.0032(3) 0.0132(3) 0.0000(3) Si2 0.0226(3) 0.0249(3) 0.0296(4) -0.0020(3) 0.0084(3) -0.0037(2) O1 0.0285(8) 0.0241(8) 0.0300(9) -0.0001(7) 0.0154(8) -0.0053(6) P1 0.0221(3) 0.0197(3) 0.0240(3) 0.0016(2) 0.0116(3) -0.0010(2) Ca1 0.0187(3) 0.0168(3) 0.0192(3) 0.000 0.0079(3) 0.000 _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 C1 Si2 1.821(2) . ? C1 Si1 1.824(2) . ? C1 Ca1 2.540(2) . ? C1 H1 1.0000 . ? C2 Si1 1.880(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 Si1 1.882(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 Si1 1.872(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 Si2 1.884(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si2 1.879(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 Si2 1.886(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.391(3) . ? C8 C9 1.398(3) . ? C8 P1 1.799(2) . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 C11 1.371(4) . ? C10 H10 0.9500 . ? C11 C12 1.386(4) . ? C11 H11 0.9500 . ? C12 C13 1.382(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.385(3) . ? C14 C15 1.393(3) . ? C14 P1 1.798(2) . ? C15 C16 1.376(4) . ? C15 H15 0.9500 . ? C16 C17 1.375(4) . ? C16 H16 0.9500 . ? C17 C18 1.385(4) . ? C17 H17 0.9500 . ? C18 C19 1.381(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.391(3) . ? C20 C25 1.392(3) . ? C20 P1 1.801(2) . ? C21 C22 1.397(3) . ? C21 H21 0.9500 . ? C22 C23 1.369(4) . ? C22 H22 0.9500 . ? C23 C24 1.388(4) . ? C23 H23 0.9500 . ? C24 C25 1.384(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.324(5) . ? C26 C27 1.348(6) . ? C26 H26 0.9500 . ? C27 C28 1.398(6) . ? C27 H27 0.9500 . ? C28 C29 1.369(6) . ? C28 H28 0.9500 . ? C29 C30 1.343(5) . ? C29 H29 0.9500 . ? C30 C31 1.347(4) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? O1 P1 1.5010(15) . ? O1 Ca1 2.2618(14) . ? Ca1 O1 2.2618(14) 2 ? Ca1 C1 2.540(2) 2 ? Ca1 Si2 3.5635(7) 2 ? 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 Si2 C1 Si1 119.96(12) . . ? Si2 C1 Ca1 108.46(9) . . ? Si1 C1 Ca1 119.02(10) . . ? Si2 C1 H1 101.9 . . ? Si1 C1 H1 101.9 . . ? Ca1 C1 H1 101.9 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 119.1(2) . . ? C13 C8 P1 121.96(17) . . ? C9 C8 P1 118.80(17) . . ? C10 C9 C8 119.9(2) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.4(2) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.4(2) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 119.7(2) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C8 120.5(2) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? C19 C14 C15 119.0(2) . . ? C19 C14 P1 119.42(17) . . ? C15 C14 P1 121.58(18) . . ? C16 C15 C14 120.3(2) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 120.5(2) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 119.7(2) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 120.1(2) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C14 120.4(2) . . ? C18 C19 H19 119.8 . . ? C14 C19 H19 119.8 . . ? C21 C20 C25 119.7(2) . . ? C21 C20 P1 121.41(18) . . ? C25 C20 P1 118.83(17) . . ? C20 C21 C22 119.5(2) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 120.5(2) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 120.2(2) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C20 120.1(2) . . ? C24 C25 H25 119.9 . . ? C20 C25 H25 119.9 . . ? C31 C26 C27 120.9(3) . . ? C31 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C28 118.9(3) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C29 C28 C27 118.8(3) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C30 C29 C28 120.0(3) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.1(3) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C26 C31 C30 121.3(3) . . ? C26 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C1 Si1 C4 113.37(12) . . ? C1 Si1 C2 115.91(12) . . ? C4 Si1 C2 105.95(18) . . ? C1 Si1 C3 111.45(12) . . ? C4 Si1 C3 106.34(15) . . ? C2 Si1 C3 102.88(15) . . ? C1 Si2 C6 112.92(11) . . ? C1 Si2 C5 117.34(12) . . ? C6 Si2 C5 103.84(13) . . ? C1 Si2 C7 110.35(12) . . ? C6 Si2 C7 106.16(14) . . ? C5 Si2 C7 105.35(16) . . ? P1 O1 Ca1 168.35(10) . . ? O1 P1 C14 110.81(10) . . ? O1 P1 C8 111.57(9) . . ? C14 P1 C8 106.61(10) . . ? O1 P1 C20 112.79(9) . . ? C14 P1 C20 107.39(10) . . ? C8 P1 C20 107.38(10) . . ? O1 Ca1 O1 97.22(8) 2 . ? O1 Ca1 C1 111.22(6) 2 . ? O1 Ca1 C1 112.34(6) . . ? O1 Ca1 C1 112.34(6) 2 2 ? O1 Ca1 C1 111.22(6) . 2 ? C1 Ca1 C1 111.73(10) . 2 ? O1 Ca1 Si2 137.06(4) 2 2 ? O1 Ca1 Si2 89.93(4) . 2 ? C1 Ca1 Si2 104.74(5) . 2 ? C1 Ca1 Si2 28.99(5) 2 2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 C8 C9 C10 0.8(4) . . . . ? P1 C8 C9 C10 -175.24(19) . . . . ? C8 C9 C10 C11 0.0(4) . . . . ? C9 C10 C11 C12 -0.8(4) . . . . ? C10 C11 C12 C13 0.9(4) . . . . ? C11 C12 C13 C8 -0.1(4) . . . . ? C9 C8 C13 C12 -0.7(4) . . . . ? P1 C8 C13 C12 175.17(19) . . . . ? C19 C14 C15 C16 0.5(4) . . . . ? P1 C14 C15 C16 -178.1(2) . . . . ? C14 C15 C16 C17 -0.2(4) . . . . ? C15 C16 C17 C18 -0.3(4) . . . . ? C16 C17 C18 C19 0.6(4) . . . . ? C17 C18 C19 C14 -0.3(4) . . . . ? C15 C14 C19 C18 -0.2(3) . . . . ? P1 C14 C19 C18 178.41(19) . . . . ? C25 C20 C21 C22 0.6(3) . . . . ? P1 C20 C21 C22 -175.84(18) . . . . ? C20 C21 C22 C23 -0.2(4) . . . . ? C21 C22 C23 C24 -0.4(4) . . . . ? C22 C23 C24 C25 0.7(4) . . . . ? C23 C24 C25 C20 -0.3(4) . . . . ? C21 C20 C25 C24 -0.3(3) . . . . ? P1 C20 C25 C24 176.19(19) . . . . ? C31 C26 C27 C28 -0.1(6) . . . . ? C26 C27 C28 C29 0.7(5) . . . . ? C27 C28 C29 C30 -0.3(5) . . . . ? C28 C29 C30 C31 -0.7(5) . . . . ? C27 C26 C31 C30 -1.0(5) . . . . ? C29 C30 C31 C26 1.4(5) . . . . ? Si2 C1 Si1 C4 58.3(2) . . . . ? Ca1 C1 Si1 C4 -79.23(18) . . . . ? Si2 C1 Si1 C2 -64.6(2) . . . . ? Ca1 C1 Si1 C2 157.90(16) . . . . ? Si2 C1 Si1 C3 178.25(13) . . . . ? Ca1 C1 Si1 C3 40.71(16) . . . . ? Si1 C1 Si2 C6 -67.74(16) . . . . ? Ca1 C1 Si2 C6 73.78(14) . . . . ? Si1 C1 Si2 C5 52.99(19) . . . . ? Ca1 C1 Si2 C5 -165.49(13) . . . . ? Si1 C1 Si2 C7 173.63(15) . . . . ? Ca1 C1 Si2 C7 -44.85(15) . . . . ? Ca1 O1 P1 C14 77.1(5) . . . . ? Ca1 O1 P1 C8 -164.3(5) . . . . ? Ca1 O1 P1 C20 -43.4(5) . . . . ? C19 C14 P1 O1 -9.9(2) . . . . ? C15 C14 P1 O1 168.70(18) . . . . ? C19 C14 P1 C8 -131.44(19) . . . . ? C15 C14 P1 C8 47.1(2) . . . . ? C19 C14 P1 C20 113.73(19) . . . . ? C15 C14 P1 C20 -67.7(2) . . . . ? C13 C8 P1 O1 157.80(18) . . . . ? C9 C8 P1 O1 -26.3(2) . . . . ? C13 C8 P1 C14 -81.1(2) . . . . ? C9 C8 P1 C14 94.8(2) . . . . ? C13 C8 P1 C20 33.7(2) . . . . ? C9 C8 P1 C20 -150.36(18) . . . . ? C21 C20 P1 O1 107.82(19) . . . . ? C25 C20 P1 O1 -68.6(2) . . . . ? C21 C20 P1 C14 -14.5(2) . . . . ? C25 C20 P1 C14 168.99(18) . . . . ? C21 C20 P1 C8 -128.86(18) . . . . ? C25 C20 P1 C8 54.7(2) . . . . ? P1 O1 Ca1 O1 -3.9(5) . . . 2 ? P1 O1 Ca1 C1 112.7(5) . . . . ? P1 O1 Ca1 C1 -121.3(5) . . . 2 ? P1 O1 Ca1 Si2 -141.4(5) . . . 2 ? Si2 C1 Ca1 O1 -45.28(11) . . . 2 ? Si1 C1 Ca1 O1 96.65(11) . . . 2 ? Si2 C1 Ca1 O1 -153.06(8) . . . . ? Si1 C1 Ca1 O1 -11.12(13) . . . . ? Si2 C1 Ca1 C1 81.14(9) . . . 2 ? Si1 C1 Ca1 C1 -136.93(13) . . . 2 ? Si2 C1 Ca1 Si2 110.82(9) . . . 2 ? Si1 C1 Ca1 Si2 -107.25(10) . . . 2 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.380 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.098 #===end data_k09msh8-(Compound-3) _database_code_depnum_ccdc_archive 'CCDC 749970' #TrackingRef 'bigcif_compounds1_3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H110 Ca2 N4 O2 P2' _chemical_formula_weight 1409.91 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4254(2) _cell_length_b 15.0443(3) _cell_length_c 19.9224(4) _cell_angle_alpha 86.844(1) _cell_angle_beta 82.166(1) _cell_angle_gamma 85.912(1) _cell_volume 3971.96(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 98737 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 26.373 _exptl_crystal_description colorless _exptl_crystal_colour block _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 0.233 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.857 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68872 _diffrn_reflns_av_R_equivalents 0.0898 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 26.40 _reflns_number_total 16164 _reflns_number_gt 10610 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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. The asymmetric unit consists of 2 independent dimer halves in this structure, in addition to one molecule of toluene. The latter was split evenly over two voids in the structure, both proximate to inversion centres, and was hopelessly disordered. Ultimately, treatment with SQUEEZE was employed and the results are presented herein. ; _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^)+(0.0873P)^2^+1.0304P] 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 16164 _refine_ls_number_parameters 891 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1744 _refine_ls_wR_factor_gt 0.1555 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 1.05336(4) 0.46008(4) 0.07376(3) 0.02426(14) Uani 1 1 d . . . Ca2 Ca 0.46255(4) 0.08923(4) 0.55613(3) 0.02699(15) Uani 1 1 d . . . P1 P 1.17409(6) 0.39649(5) -0.05315(4) 0.02706(18) Uani 1 1 d . . . P2 P 0.66786(7) 0.00092(6) 0.57333(5) 0.0406(2) Uani 1 1 d . . . O1 O 1.05753(14) 0.42925(13) -0.04274(10) 0.0271(4) Uani 1 1 d . . . O2 O 0.60657(14) 0.00354(13) 0.50994(10) 0.0300(5) Uani 1 1 d . . . N1 N 1.00485(17) 0.33912(16) 0.14814(12) 0.0268(5) Uani 1 1 d . . . N2 N 1.14544(17) 0.49112(16) 0.16301(12) 0.0274(5) Uani 1 1 d . . . N3 N 0.36993(17) 0.13399(16) 0.66116(12) 0.0265(5) Uani 1 1 d . . . N4 N 0.47200(17) 0.24523(15) 0.54068(12) 0.0254(5) Uani 1 1 d . . . C1 C 0.9327(3) 0.2795(2) 0.26136(16) 0.0396(8) Uani 1 1 d . . . H1A H 0.8663 0.2795 0.2461 0.059 Uiso 1 1 calc R . . H1B H 0.9247 0.2983 0.3082 0.059 Uiso 1 1 calc R . . H1C H 0.9655 0.2192 0.2591 0.059 Uiso 1 1 calc R . . C2 C 0.9970(2) 0.34364(19) 0.21578(15) 0.0284(6) Uani 1 1 d . . . C3 C 1.0477(2) 0.4021(2) 0.25004(15) 0.0290(6) Uani 1 1 d . . . H3 H 1.0268 0.4024 0.2975 0.035 Uiso 1 1 calc R . . C5 C 1.1857(2) 0.4842(2) 0.28102(16) 0.0353(7) Uani 1 1 d . . . H5A H 1.2357 0.4351 0.2884 0.053 Uiso 1 1 calc R . . H5B H 1.1408 0.4941 0.3234 0.053 Uiso 1 1 calc R . . H5C H 1.2203 0.5385 0.2664 0.053 Uiso 1 1 calc R . . C6 C 0.9736(2) 0.25941(19) 0.12252(14) 0.0272(6) Uani 1 1 d . . . C7 C 0.8838(2) 0.26028(19) 0.09297(15) 0.0293(6) Uani 1 1 d . . . C8 C 0.8617(2) 0.1838(2) 0.06282(16) 0.0343(7) Uani 1 1 d . . . H8 H 0.8015 0.1842 0.0426 0.041 Uiso 1 1 calc R . . C9 C 0.9253(3) 0.1080(2) 0.06186(17) 0.0383(8) Uani 1 1 d . . . H9 H 0.9096 0.0568 0.0405 0.046 Uiso 1 1 calc R . . C10 C 1.0123(3) 0.1065(2) 0.09205(17) 0.0375(7) Uani 1 1 d . . . H10 H 1.0556 0.0537 0.0916 0.045 Uiso 1 1 calc R . . C11 C 1.0375(2) 0.1807(2) 0.12309(15) 0.0321(7) Uani 1 1 d . . . C12 C 0.8099(2) 0.3405(2) 0.09370(17) 0.0353(7) Uani 1 1 d . . . H12 H 0.8390 0.3894 0.1153 0.042 Uiso 1 1 calc R . . C13 C 0.7093(3) 0.3215(3) 0.1357(2) 0.0607(11) Uani 1 1 d . . . H13A H 0.6793 0.2733 0.1158 0.091 Uiso 1 1 calc R . . H13B H 0.6637 0.3754 0.1359 0.091 Uiso 1 1 calc R . . H13C H 0.7201 0.3035 0.1823 0.091 Uiso 1 1 calc R . . C14 C 0.7939(3) 0.3738(2) 0.02149(19) 0.0473(9) Uani 1 1 d . . . H14A H 0.8593 0.3823 -0.0057 0.071 Uiso 1 1 calc R . . H14B H 0.7533 0.4306 0.0232 0.071 Uiso 1 1 calc R . . H14C H 0.7588 0.3296 0.0008 0.071 Uiso 1 1 calc R . . C15 C 1.1363(2) 0.1767(2) 0.15327(17) 0.0373(7) Uani 1 1 d . . . H15 H 1.1331 0.2281 0.1834 0.045 Uiso 1 1 calc R . . C16 C 1.1527(4) 0.0917(3) 0.1965(3) 0.0716(13) Uani 1 1 d . . . H16A H 1.0987 0.0890 0.2348 0.107 Uiso 1 1 calc R . . H16B H 1.2178 0.0916 0.2136 0.107 Uiso 1 1 calc R . . H16C H 1.1522 0.0398 0.1689 0.107 Uiso 1 1 calc R . . C17 C 1.2222(3) 0.1888(3) 0.0977(2) 0.0601(11) Uani 1 1 d . . . H17A H 1.2272 0.1394 0.0670 0.090 Uiso 1 1 calc R . . H17B H 1.2852 0.1895 0.1174 0.090 Uiso 1 1 calc R . . H17C H 1.2106 0.2453 0.0722 0.090 Uiso 1 1 calc R . . C18 C 1.2322(2) 0.5435(2) 0.14679(14) 0.0294(7) Uani 1 1 d . . . C19 C 1.2215(2) 0.6373(2) 0.15122(16) 0.0347(7) Uani 1 1 d . . . C20 C 1.3079(3) 0.6842(2) 0.13655(18) 0.0449(9) Uani 1 1 d . . . H20 H 1.3026 0.7471 0.1401 0.054 Uiso 1 1 calc R . . C21 C 1.4015(3) 0.6418(3) 0.1169(2) 0.0491(9) Uani 1 1 d . . . H21 H 1.4598 0.6751 0.1088 0.059 Uiso 1 1 calc R . . C22 C 1.4095(2) 0.5521(3) 0.10929(18) 0.0450(9) Uani 1 1 d . . . H22 H 1.4734 0.5239 0.0937 0.054 Uiso 1 1 calc R . . C23 C 1.3259(2) 0.5005(2) 0.12393(15) 0.0333(7) Uani 1 1 d . . . C24 C 1.1186(2) 0.6868(2) 0.16758(18) 0.0408(8) Uani 1 1 d . . . H24 H 1.0710 0.6578 0.1425 0.049 Uiso 1 1 calc R . . C25 C 1.0752(3) 0.6824(3) 0.2415(2) 0.0589(10) Uani 1 1 d . . . H25A H 1.0625 0.6205 0.2560 0.088 Uiso 1 1 calc R . . H25B H 1.0119 0.7194 0.2479 0.088 Uiso 1 1 calc R . . H25C H 1.1231 0.7045 0.2685 0.088 Uiso 1 1 calc R . . C26 C 1.1189(3) 0.7854(2) 0.1419(2) 0.0531(10) Uani 1 1 d . . . H26A H 1.0501 0.8130 0.1490 0.080 Uiso 1 1 calc R . . H26B H 1.1445 0.7889 0.0934 0.080 Uiso 1 1 calc R . . H26C H 1.1623 0.8171 0.1669 0.080 Uiso 1 1 calc R . . C27 C 1.3408(2) 0.4007(2) 0.11502(17) 0.0384(8) Uani 1 1 d . . . H27 H 1.2726 0.3780 0.1145 0.046 Uiso 1 1 calc R . . C28 C 1.4045(3) 0.3773(3) 0.04778(18) 0.0479(9) Uani 1 1 d . . . H28A H 1.3804 0.4149 0.0108 0.072 Uiso 1 1 calc R . . H28B H 1.3987 0.3144 0.0395 0.072 Uiso 1 1 calc R . . H28C H 1.4751 0.3877 0.0501 0.072 Uiso 1 1 calc R . . C29 C 1.3861(3) 0.3518(3) 0.1736(2) 0.0639(11) Uani 1 1 d . . . H29A H 1.4492 0.3777 0.1793 0.096 Uiso 1 1 calc R . . H29B H 1.3996 0.2886 0.1640 0.096 Uiso 1 1 calc R . . H29C H 1.3386 0.3576 0.2154 0.096 Uiso 1 1 calc R . . C30 C 1.2241(2) 0.43415(19) -0.13941(15) 0.0289(6) Uani 1 1 d . . . C31 C 1.3270(2) 0.4401(2) -0.15560(17) 0.0378(7) Uani 1 1 d . . . H31 H 1.3692 0.4280 -0.1211 0.045 Uiso 1 1 calc R . . C32 C 1.3702(3) 0.4633(2) -0.22109(19) 0.0474(9) Uani 1 1 d . . . H32 H 1.4413 0.4644 -0.2317 0.057 Uiso 1 1 calc R . . C33 C 1.3083(3) 0.4847(2) -0.27072(18) 0.0480(9) Uani 1 1 d . . . H33 H 1.3368 0.5018 -0.3154 0.058 Uiso 1 1 calc R . . C34 C 1.2057(3) 0.4811(2) -0.25536(17) 0.0416(8) Uani 1 1 d . . . H34 H 1.1635 0.4965 -0.2894 0.050 Uiso 1 1 calc R . . C35 C 1.1630(2) 0.4549(2) -0.19010(15) 0.0330(7) Uani 1 1 d . . . H35 H 1.0921 0.4512 -0.1802 0.040 Uiso 1 1 calc R . . C36 C 1.1827(2) 0.27734(19) -0.06835(15) 0.0290(6) Uani 1 1 d . . . C37 C 1.2788(2) 0.2337(2) -0.08168(16) 0.0360(7) Uani 1 1 d . . . H37 H 1.3368 0.2670 -0.0842 0.043 Uiso 1 1 calc R . . C38 C 1.2901(3) 0.1439(2) -0.09103(16) 0.0390(8) Uani 1 1 d . . . H38 H 1.3557 0.1155 -0.1004 0.047 Uiso 1 1 calc R . . C39 C 1.2063(3) 0.0943(2) -0.08693(17) 0.0412(8) Uani 1 1 d . . . H39 H 1.2142 0.0321 -0.0937 0.049 Uiso 1 1 calc R . . C40 C 1.1115(3) 0.1358(2) -0.07305(17) 0.0400(8) Uani 1 1 d . . . H40 H 1.0539 0.1019 -0.0703 0.048 Uiso 1 1 calc R . . C41 C 1.0995(2) 0.2276(2) -0.06292(16) 0.0347(7) Uani 1 1 d . . . H41 H 1.0339 0.2555 -0.0523 0.042 Uiso 1 1 calc R . . C42 C 0.2444(2) 0.2301(2) 0.73204(16) 0.0370(7) Uani 1 1 d . . . H42A H 0.2508 0.1812 0.7661 0.055 Uiso 1 1 calc R A . H42B H 0.1749 0.2367 0.7217 0.055 Uiso 1 1 calc R . . H42C H 0.2617 0.2857 0.7498 0.055 Uiso 1 1 calc R . . C43 C 0.3153(2) 0.20960(19) 0.66789(15) 0.0279(6) Uani 1 1 d . A . C44 C 0.3184(2) 0.2802(2) 0.61767(16) 0.0305(7) Uani 1 1 d . . . H44 H 0.2610 0.3212 0.6218 0.037 Uiso 1 1 calc R A . C45 C 0.3917(2) 0.2994(2) 0.56307(15) 0.0300(7) Uani 1 1 d . A . C46 C 0.3773(3) 0.3918(2) 0.52791(18) 0.0390(8) Uani 1 1 d . . . H46A H 0.4309 0.4290 0.5364 0.059 Uiso 1 1 calc R A . H46B H 0.3117 0.4200 0.5459 0.059 Uiso 1 1 calc R . . H46C H 0.3800 0.3856 0.4790 0.059 Uiso 1 1 calc R . . C47 C 0.3684(2) 0.06756(19) 0.71648(14) 0.0286(6) Uani 1 1 d . A . C48 C 0.2868(2) 0.0128(2) 0.73278(15) 0.0344(7) Uani 1 1 d . . . C49 C 0.2947(3) -0.0560(2) 0.78159(17) 0.0424(8) Uani 1 1 d . A . H49 H 0.2408 -0.0941 0.7927 0.051 Uiso 1 1 calc R . . C50 C 0.3786(3) -0.0703(2) 0.81404(18) 0.0481(9) Uani 1 1 d . . . H50 H 0.3824 -0.1181 0.8470 0.058 Uiso 1 1 calc R A . C51 C 0.4577(3) -0.0154(2) 0.79904(17) 0.0419(8) Uani 1 1 d . A . H51 H 0.5153 -0.0256 0.8220 0.050 Uiso 1 1 calc R . . C52 C 0.4541(2) 0.0552(2) 0.75046(15) 0.0325(7) Uani 1 1 d . . . C53 C 0.1915(2) 0.0267(2) 0.69877(17) 0.0407(8) Uani 1 1 d . A . H53 H 0.1956 0.0837 0.6705 0.049 Uiso 1 1 calc R . . C54 C 0.0955(3) 0.0355(3) 0.7514(2) 0.0627(11) Uani 1 1 d . . . H54A H 0.0368 0.0516 0.7279 0.094 Uiso 1 1 calc R A . H54B H 0.1028 0.0819 0.7827 0.094 Uiso 1 1 calc R . . H54C H 0.0863 -0.0216 0.7770 0.094 Uiso 1 1 calc R . . C55 C 0.1829(3) -0.0473(3) 0.6525(2) 0.0643(11) Uani 1 1 d . . . H55A H 0.2414 -0.0496 0.6172 0.096 Uiso 1 1 calc R A . H55B H 0.1212 -0.0362 0.6313 0.096 Uiso 1 1 calc R . . H55C H 0.1805 -0.1042 0.6788 0.096 Uiso 1 1 calc R . . C56 C 0.5369(2) 0.1206(2) 0.73791(16) 0.0336(7) Uani 1 1 d . A . H56 H 0.5464 0.1374 0.6883 0.040 Uiso 1 1 calc R . . C57 C 0.5046(3) 0.2057(2) 0.77542(19) 0.0445(8) Uani 1 1 d . . . H57A H 0.4398 0.2303 0.7629 0.067 Uiso 1 1 calc R A . H57B H 0.5555 0.2495 0.7631 0.067 Uiso 1 1 calc R . . H57C H 0.4978 0.1921 0.8244 0.067 Uiso 1 1 calc R . . C58 C 0.6380(3) 0.0827(3) 0.75623(19) 0.0499(9) Uani 1 1 d . . . H58A H 0.6325 0.0697 0.8053 0.075 Uiso 1 1 calc R A . H58B H 0.6888 0.1262 0.7428 0.075 Uiso 1 1 calc R . . H58C H 0.6579 0.0276 0.7324 0.075 Uiso 1 1 calc R . . C59 C 0.5539(2) 0.28689(19) 0.50010(15) 0.0295(6) Uani 1 1 d . A . C60 C 0.6214(2) 0.3317(2) 0.53299(16) 0.0330(7) Uani 1 1 d . . . C61 C 0.7021(3) 0.3708(2) 0.49303(17) 0.0410(8) Uani 1 1 d . A . H61 H 0.7467 0.4026 0.5144 0.049 Uiso 1 1 calc R . . C62 C 0.7188(3) 0.3647(2) 0.42419(18) 0.0468(9) Uani 1 1 d . . . H62 H 0.7748 0.3911 0.3984 0.056 Uiso 1 1 calc R A . C63 C 0.6531(3) 0.3194(2) 0.39236(17) 0.0429(8) Uani 1 1 d . A . H63 H 0.6654 0.3142 0.3446 0.052 Uiso 1 1 calc R . . C64 C 0.5699(2) 0.2817(2) 0.42899(16) 0.0340(7) Uani 1 1 d . . . C65 C 0.6108(3) 0.3382(2) 0.60954(16) 0.0404(8) Uani 1 1 d . A . H65 H 0.5506 0.3058 0.6299 0.049 Uiso 1 1 calc R . . C66 C 0.5942(3) 0.4353(3) 0.6305(2) 0.0547(10) Uani 1 1 d . . . H66A H 0.6531 0.4680 0.6120 0.082 Uiso 1 1 calc R A . H66B H 0.5845 0.4367 0.6801 0.082 Uiso 1 1 calc R . . H66C H 0.5343 0.4632 0.6127 0.082 Uiso 1 1 calc R . . C67 C 0.7021(3) 0.2940(3) 0.63777(19) 0.0506(9) Uani 1 1 d . . . H67A H 0.7126 0.2322 0.6240 0.076 Uiso 1 1 calc R A . H67B H 0.6911 0.2948 0.6874 0.076 Uiso 1 1 calc R . . H67C H 0.7616 0.3265 0.6202 0.076 Uiso 1 1 calc R . . C68 C 0.4978(3) 0.2359(2) 0.39189(16) 0.0380(7) Uani 1 1 d . A . H68 H 0.4360 0.2249 0.4245 0.046 Uiso 1 1 calc R . . C69 C 0.5445(3) 0.1455(2) 0.36721(19) 0.0485(9) Uani 1 1 d . . . H69A H 0.6031 0.1549 0.3331 0.073 Uiso 1 1 calc R A . H69B H 0.4945 0.1150 0.3471 0.073 Uiso 1 1 calc R . . H69C H 0.5656 0.1090 0.4057 0.073 Uiso 1 1 calc R . . C70 C 0.4658(3) 0.2937(3) 0.3316(2) 0.0591(11) Uani 1 1 d . . . H70A H 0.4349 0.3511 0.3475 0.089 Uiso 1 1 calc R A . H70B H 0.4169 0.2630 0.3105 0.089 Uiso 1 1 calc R . . H70C H 0.5250 0.3039 0.2982 0.089 Uiso 1 1 calc R . . C71 C 0.7270(2) -0.1120(2) 0.57800(17) 0.0371(7) Uani 1 1 d . A . C72 C 0.7465(3) -0.1507(3) 0.64048(19) 0.0528(10) Uani 1 1 d . . . H72 H 0.7271 -0.1184 0.6803 0.063 Uiso 1 1 calc R A . C73 C 0.7938(3) -0.2354(3) 0.6457(2) 0.0628(11) Uani 1 1 d . A . H73 H 0.8084 -0.2597 0.6885 0.075 Uiso 1 1 calc R . . C74 C 0.8194(3) -0.2840(3) 0.5887(2) 0.0544(10) Uani 1 1 d . . . H74 H 0.8505 -0.3425 0.5921 0.065 Uiso 1 1 calc R A . C75 C 0.7999(2) -0.2475(2) 0.5266(2) 0.0444(8) Uani 1 1 d . A . H75 H 0.8168 -0.2814 0.4873 0.053 Uiso 1 1 calc R . . C76 C 0.7558(2) -0.1619(2) 0.52073(17) 0.0363(7) Uani 1 1 d . . . H76 H 0.7450 -0.1368 0.4773 0.044 Uiso 1 1 calc R A . C77 C 0.7716(4) 0.0624(6) 0.5591(4) 0.037(3) Uani 0.50 1 d PG A 1 C78 C 0.8454(4) 0.0523(4) 0.6020(3) 0.0516(19) Uani 0.50 1 d PG A 1 H78 H 0.8379 0.0116 0.6403 0.062 Uiso 0.50 1 calc PR A 1 C85 C 1.1242(2) 0.46037(19) 0.22635(15) 0.0279(6) Uani 1 1 d . . . C79 C 0.9302(4) 0.1016(4) 0.5890(4) 0.069(3) Uani 0.50 1 d PG A 1 H79 H 0.9806 0.0947 0.6184 0.083 Uiso 0.50 1 calc PR A 1 C80 C 0.9412(4) 0.1611(4) 0.5330(4) 0.062(2) Uani 0.50 1 d PG A 1 H80 H 0.9991 0.1949 0.5241 0.074 Uiso 0.50 1 calc PR A 1 C81 C 0.8674(7) 0.1713(7) 0.4900(4) 0.062(6) Uani 0.50 1 d PG A 1 H81 H 0.8749 0.2120 0.4518 0.074 Uiso 0.50 1 calc PR A 1 C82 C 0.7826(6) 0.1220(9) 0.5031(5) 0.059(8) Uani 0.50 1 d PG A 1 H82 H 0.7322 0.1289 0.4737 0.070 Uiso 0.50 1 calc PR A 1 C77A C 0.7914(7) 0.0577(7) 0.5326(6) 0.034(2) Uani 0.50 1 d P A 2 C78A C 0.8877(6) 0.0268(6) 0.5470(6) 0.070(3) Uani 0.50 1 d P A 2 H78A H 0.8951 -0.0248 0.5761 0.083 Uiso 0.50 1 calc PR A 2 C79A C 0.9722(6) 0.0708(6) 0.5192(6) 0.080(3) Uani 0.50 1 d P A 2 H79A H 1.0373 0.0477 0.5275 0.096 Uiso 0.50 1 calc PR A 2 C80A C 0.9620(6) 0.1463(6) 0.4803(6) 0.058(2) Uani 0.50 1 d P A 2 H80A H 1.0207 0.1745 0.4603 0.069 Uiso 0.50 1 calc PR A 2 C81A C 0.8705(8) 0.1829(10) 0.4690(10) 0.050(3) Uani 0.50 1 d P A 2 H81A H 0.8638 0.2375 0.4432 0.061 Uiso 0.50 1 calc PR A 2 C82A C 0.7828(8) 0.1358(12) 0.4976(6) 0.030(4) Uani 0.50 1 d P A 2 H82A H 0.7177 0.1611 0.4914 0.036 Uiso 0.50 1 calc PR A 2 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 0.0269(3) 0.0240(3) 0.0227(3) 0.0000(2) -0.0067(2) -0.0021(2) Ca2 0.0314(3) 0.0224(3) 0.0269(3) -0.0047(2) -0.0008(2) -0.0022(2) P1 0.0279(4) 0.0266(4) 0.0267(4) -0.0025(3) -0.0042(3) 0.0003(3) P2 0.0475(5) 0.0330(5) 0.0459(5) -0.0097(4) -0.0234(4) 0.0055(4) O1 0.0272(10) 0.0273(11) 0.0263(11) -0.0017(8) -0.0029(8) -0.0005(8) O2 0.0305(10) 0.0263(11) 0.0345(12) -0.0026(9) -0.0091(9) 0.0003(8) N1 0.0276(12) 0.0262(13) 0.0273(13) 0.0004(10) -0.0043(10) -0.0058(10) N2 0.0269(12) 0.0296(13) 0.0261(13) -0.0014(10) -0.0047(10) -0.0025(10) N3 0.0285(12) 0.0258(13) 0.0243(13) -0.0002(10) -0.0006(10) -0.0026(10) N4 0.0285(12) 0.0228(12) 0.0247(13) -0.0015(10) -0.0028(10) -0.0014(10) C1 0.0461(19) 0.043(2) 0.0290(17) 0.0020(14) 0.0022(14) -0.0136(15) C2 0.0270(15) 0.0268(16) 0.0300(16) 0.0011(12) -0.0009(12) 0.0000(12) C3 0.0318(15) 0.0327(16) 0.0217(15) 0.0013(12) -0.0026(12) -0.0015(13) C5 0.0360(17) 0.0437(19) 0.0287(17) -0.0008(14) -0.0109(13) -0.0062(14) C6 0.0330(15) 0.0257(15) 0.0224(15) 0.0028(12) -0.0003(12) -0.0066(12) C7 0.0334(16) 0.0257(15) 0.0291(16) 0.0020(12) -0.0046(13) -0.0061(12) C8 0.0359(17) 0.0330(17) 0.0361(18) 0.0005(14) -0.0085(14) -0.0118(14) C9 0.051(2) 0.0268(17) 0.0380(18) -0.0026(14) -0.0055(15) -0.0103(15) C10 0.0491(19) 0.0255(16) 0.0370(18) 0.0022(14) -0.0057(15) 0.0008(14) C11 0.0382(17) 0.0301(17) 0.0272(16) 0.0047(13) -0.0033(13) -0.0040(13) C12 0.0347(17) 0.0286(17) 0.0454(19) -0.0057(14) -0.0121(14) -0.0056(13) C13 0.044(2) 0.051(2) 0.083(3) -0.005(2) 0.003(2) 0.0013(18) C14 0.054(2) 0.0360(19) 0.056(2) 0.0010(17) -0.0258(18) 0.0013(16) C15 0.0389(17) 0.0374(18) 0.0355(18) -0.0022(14) -0.0075(14) 0.0035(14) C16 0.078(3) 0.060(3) 0.083(3) 0.026(2) -0.045(3) -0.001(2) C17 0.038(2) 0.092(3) 0.053(2) -0.012(2) -0.0077(17) -0.008(2) C18 0.0290(15) 0.0388(18) 0.0231(15) -0.0018(13) -0.0095(12) -0.0078(13) C19 0.0318(16) 0.0410(19) 0.0333(17) 0.0003(14) -0.0104(13) -0.0061(14) C20 0.050(2) 0.041(2) 0.048(2) -0.0036(16) -0.0138(17) -0.0155(16) C21 0.0369(19) 0.056(2) 0.057(2) -0.0055(19) -0.0065(17) -0.0228(17) C22 0.0273(17) 0.062(2) 0.048(2) -0.0094(18) -0.0047(15) -0.0107(16) C23 0.0302(16) 0.0441(19) 0.0279(16) -0.0045(14) -0.0088(13) -0.0062(14) C24 0.0358(17) 0.0370(19) 0.053(2) -0.0046(16) -0.0159(16) -0.0038(14) C25 0.054(2) 0.058(3) 0.062(3) -0.006(2) -0.0042(19) 0.0117(19) C26 0.058(2) 0.039(2) 0.066(3) -0.0058(18) -0.022(2) 0.0014(17) C27 0.0287(16) 0.047(2) 0.0401(19) -0.0037(15) -0.0071(14) 0.0005(14) C28 0.0406(19) 0.061(2) 0.042(2) -0.0073(18) -0.0077(16) 0.0006(17) C29 0.079(3) 0.067(3) 0.042(2) 0.004(2) -0.010(2) 0.020(2) C30 0.0288(15) 0.0246(15) 0.0330(17) -0.0034(12) -0.0019(12) -0.0012(12) C31 0.0320(17) 0.0386(19) 0.0420(19) 0.0003(15) -0.0011(14) -0.0051(14) C32 0.0420(19) 0.049(2) 0.048(2) 0.0002(17) 0.0100(16) -0.0121(16) C33 0.063(2) 0.039(2) 0.0351(19) 0.0021(15) 0.0140(17) -0.0046(17) C34 0.058(2) 0.0348(18) 0.0300(18) 0.0000(14) -0.0050(15) 0.0079(16) C35 0.0341(16) 0.0326(17) 0.0318(17) -0.0025(13) -0.0041(13) 0.0017(13) C36 0.0349(16) 0.0259(15) 0.0251(15) 0.0014(12) -0.0025(12) 0.0012(13) C37 0.0335(16) 0.0343(18) 0.0385(18) -0.0038(14) 0.0016(14) -0.0001(14) C38 0.0431(19) 0.0349(18) 0.0344(18) 0.0018(14) 0.0049(14) 0.0078(15) C39 0.055(2) 0.0305(18) 0.0358(19) -0.0035(14) 0.0032(15) -0.0001(15) C40 0.048(2) 0.0293(17) 0.043(2) -0.0001(15) -0.0023(15) -0.0102(15) C41 0.0355(17) 0.0319(17) 0.0360(18) -0.0023(14) -0.0043(14) 0.0024(13) C42 0.0377(17) 0.0390(19) 0.0317(17) -0.0042(14) 0.0029(13) 0.0025(14) C43 0.0265(14) 0.0288(16) 0.0283(16) -0.0040(12) -0.0016(12) -0.0026(12) C44 0.0292(15) 0.0255(16) 0.0357(17) -0.0031(13) -0.0034(13) 0.0049(12) C45 0.0342(16) 0.0276(16) 0.0284(16) -0.0018(13) -0.0060(13) 0.0000(13) C46 0.0466(19) 0.0287(17) 0.0406(19) 0.0055(14) -0.0066(15) 0.0023(14) C47 0.0377(16) 0.0228(15) 0.0239(15) -0.0043(12) 0.0004(12) 0.0019(12) C48 0.0469(19) 0.0303(17) 0.0252(16) -0.0050(13) 0.0024(13) -0.0062(14) C49 0.057(2) 0.0326(18) 0.0350(19) -0.0010(14) 0.0064(16) -0.0142(16) C50 0.080(3) 0.0314(18) 0.0302(18) 0.0065(15) -0.0010(18) -0.0029(18) C51 0.055(2) 0.0362(19) 0.0346(18) 0.0005(15) -0.0123(16) 0.0029(16) C52 0.0433(18) 0.0270(16) 0.0264(16) -0.0073(13) -0.0002(13) -0.0001(13) C53 0.0426(19) 0.0409(19) 0.0376(19) -0.0013(15) 0.0030(15) -0.0122(15) C54 0.046(2) 0.089(3) 0.051(2) -0.007(2) 0.0047(18) -0.011(2) C55 0.061(3) 0.075(3) 0.062(3) -0.019(2) -0.016(2) -0.012(2) C56 0.0375(17) 0.0392(18) 0.0246(16) -0.0041(13) -0.0057(13) -0.0003(14) C57 0.0463(19) 0.040(2) 0.048(2) -0.0129(16) -0.0023(16) -0.0098(16) C58 0.048(2) 0.060(2) 0.044(2) -0.0042(18) -0.0163(17) 0.0043(18) C59 0.0340(16) 0.0232(15) 0.0297(16) 0.0029(12) -0.0006(12) -0.0003(12) C60 0.0389(17) 0.0271(16) 0.0319(17) -0.0004(13) 0.0003(13) -0.0054(13) C61 0.0436(19) 0.0404(19) 0.0389(19) 0.0014(15) -0.0007(15) -0.0140(15) C62 0.046(2) 0.048(2) 0.044(2) 0.0060(17) 0.0057(16) -0.0126(17) C63 0.052(2) 0.047(2) 0.0270(17) 0.0044(15) 0.0026(15) -0.0022(16) C64 0.0396(17) 0.0320(17) 0.0283(17) 0.0000(13) 0.0002(13) 0.0013(14) C65 0.0421(18) 0.049(2) 0.0321(18) -0.0083(15) 0.0003(14) -0.0181(16) C66 0.057(2) 0.060(3) 0.048(2) -0.0208(19) -0.0028(18) -0.0036(19) C67 0.058(2) 0.055(2) 0.040(2) -0.0012(17) -0.0116(17) -0.0057(18) C68 0.0452(19) 0.0435(19) 0.0250(16) 0.0003(14) -0.0065(14) 0.0004(15) C69 0.057(2) 0.047(2) 0.043(2) -0.0124(17) -0.0096(17) 0.0007(17) C70 0.073(3) 0.059(3) 0.049(2) 0.005(2) -0.027(2) -0.001(2) C71 0.0366(17) 0.0357(18) 0.0412(19) -0.0004(15) -0.0139(14) -0.0021(14) C72 0.071(3) 0.050(2) 0.038(2) 0.0008(17) -0.0154(18) 0.0105(19) C73 0.073(3) 0.057(3) 0.057(3) 0.014(2) -0.018(2) 0.014(2) C74 0.051(2) 0.038(2) 0.071(3) 0.007(2) -0.007(2) 0.0063(17) C75 0.0355(18) 0.042(2) 0.057(2) -0.0078(17) -0.0095(16) 0.0029(15) C76 0.0332(16) 0.0357(18) 0.0411(19) -0.0022(15) -0.0106(14) -0.0002(14) C77 0.031(5) 0.040(5) 0.039(6) -0.006(5) -0.004(4) -0.003(4) C78 0.045(4) 0.047(5) 0.065(5) 0.007(4) -0.018(4) -0.008(4) C85 0.0278(15) 0.0299(16) 0.0265(16) -0.0019(12) -0.0069(12) 0.0004(12) C79 0.052(5) 0.050(5) 0.114(8) 0.004(5) -0.038(5) -0.011(4) C80 0.027(4) 0.045(5) 0.116(9) -0.005(6) -0.015(5) -0.011(3) C81 0.066(10) 0.033(7) 0.084(11) -0.003(6) -0.003(6) 0.002(5) C82 0.045(11) 0.053(14) 0.082(15) -0.024(11) -0.016(9) 0.005(8) C77A 0.031(4) 0.028(5) 0.045(7) -0.006(5) -0.013(4) -0.001(4) C78A 0.041(4) 0.062(6) 0.111(8) 0.033(6) -0.038(5) -0.008(4) C79A 0.034(4) 0.065(6) 0.150(11) 0.015(6) -0.043(6) -0.009(4) C80A 0.042(5) 0.045(5) 0.087(7) -0.005(5) -0.008(4) -0.012(4) C81A 0.030(6) 0.036(6) 0.090(8) -0.005(5) -0.017(4) -0.010(4) C82A 0.025(8) 0.021(5) 0.046(8) -0.003(5) -0.008(5) -0.001(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 Ca1 O1 2.270(2) 2_765 ? Ca1 N1 2.354(2) . ? Ca1 N2 2.383(2) . ? Ca1 O1 2.384(2) . ? Ca1 P1 2.9772(10) . ? Ca1 Ca1 3.5563(11) 2_765 ? Ca2 O2 2.294(2) 2_656 ? Ca2 O2 2.353(2) . ? Ca2 N4 2.360(2) . ? Ca2 N3 2.388(2) . ? Ca2 P2 3.0274(10) . ? Ca2 Ca2 3.5895(12) 2_656 ? P1 O1 1.596(2) . ? P1 C36 1.827(3) . ? P1 C30 1.832(3) . ? P2 O2 1.596(2) . ? P2 C77 1.710(5) . ? P2 C71 1.826(3) . ? P2 C77A 1.975(10) . ? O1 Ca1 2.270(2) 2_765 ? O2 Ca2 2.294(2) 2_656 ? N1 C2 1.342(4) . ? N1 C6 1.440(4) . ? N2 C85 1.321(4) . ? N2 C18 1.443(4) . ? N3 C43 1.312(4) . ? N3 C47 1.445(4) . ? N4 C45 1.345(4) . ? N4 C59 1.434(4) . ? C1 C2 1.521(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.407(4) . ? C3 C85 1.413(4) . ? C3 H3 0.9500 . ? C5 C85 1.526(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.410(4) . ? C6 C11 1.413(4) . ? C7 C8 1.395(4) . ? C7 C12 1.506(4) . ? C8 C9 1.375(5) . ? C8 H8 0.9500 . ? C9 C10 1.383(5) . ? C9 H9 0.9500 . ? C10 C11 1.389(4) . ? C10 H10 0.9500 . ? C11 C15 1.526(4) . ? C12 C13 1.526(5) . ? C12 C14 1.535(5) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.500(5) . ? C15 C16 1.521(5) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.404(4) . ? C18 C19 1.414(4) . ? C19 C20 1.389(5) . ? C19 C24 1.526(5) . ? C20 C21 1.385(5) . ? C20 H20 0.9500 . ? C21 C22 1.362(5) . ? C21 H21 0.9500 . ? C22 C23 1.399(4) . ? C22 H22 0.9500 . ? C23 C27 1.517(5) . ? C24 C25 1.507(5) . ? C24 C26 1.542(5) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.520(5) . ? C27 C28 1.532(5) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.384(4) . ? C30 C35 1.395(4) . ? C31 C32 1.390(5) . ? C31 H31 0.9500 . ? C32 C33 1.387(5) . ? C32 H32 0.9500 . ? C33 C34 1.374(5) . ? C33 H33 0.9500 . ? C34 C35 1.395(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C41 1.378(4) . ? C36 C37 1.404(4) . ? C37 C38 1.369(5) . ? C37 H37 0.9500 . ? C38 C39 1.384(5) . ? C38 H38 0.9500 . ? C39 C40 1.376(5) . ? C39 H39 0.9500 . ? C40 C41 1.401(4) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.518(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.417(4) . ? C44 C45 1.397(4) . ? C44 H44 0.9500 . ? C45 C46 1.534(4) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C52 1.409(4) . ? C47 C48 1.410(4) . ? C48 C49 1.389(5) . ? C48 C53 1.524(5) . ? C49 C50 1.372(5) . ? C49 H49 0.9500 . ? C50 C51 1.383(5) . ? C50 H50 0.9500 . ? C51 C52 1.399(4) . ? C51 H51 0.9500 . ? C52 C56 1.524(4) . ? C53 C55 1.505(5) . ? C53 C54 1.549(5) . ? C53 H53 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C58 1.517(5) . ? C56 C57 1.524(5) . ? C56 H56 1.0000 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C64 1.409(4) . ? C59 C60 1.415(4) . ? C60 C61 1.399(4) . ? C60 C65 1.520(4) . ? C61 C62 1.366(5) . ? C61 H61 0.9500 . ? C62 C63 1.389(5) . ? C62 H62 0.9500 . ? C63 C64 1.387(5) . ? C63 H63 0.9500 . ? C64 C68 1.517(4) . ? C65 C67 1.513(5) . ? C65 C66 1.535(5) . ? C65 H65 1.0000 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.534(5) . ? C68 C70 1.535(5) . ? C68 H68 1.0000 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.395(5) . ? C71 C76 1.395(5) . ? C72 C73 1.387(5) . ? C72 H72 0.9500 . ? C73 C74 1.376(6) . ? C73 H73 0.9500 . ? C74 C75 1.376(5) . ? C74 H74 0.9500 . ? C75 C76 1.385(5) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 C78 1.3900 . ? C77 C82 1.3900 . ? C78 C79 1.3900 . ? C78 H78 0.9500 . ? C79 C80 1.3900 . ? C79 H79 0.9500 . ? C80 C81 1.3900 . ? C80 H80 0.9500 . ? C81 C82 1.3900 . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C77A C82A 1.339(15) . ? C77A C78A 1.403(11) . ? C78A C79A 1.390(12) . ? C78A H78A 0.9500 . ? C79A C80A 1.348(12) . ? C79A H79A 0.9500 . ? C80A C81A 1.353(14) . ? C80A H80A 0.9500 . ? C81A C82A 1.450(15) . ? C81A H81A 0.9500 . ? C82A H82A 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 O1 Ca1 N1 122.97(8) 2_765 . ? O1 Ca1 N2 116.13(8) 2_765 . ? N1 Ca1 N2 82.32(8) . . ? O1 Ca1 O1 80.39(7) 2_765 . ? N1 Ca1 O1 113.14(8) . . ? N2 Ca1 O1 147.56(8) . . ? O1 Ca1 P1 106.96(5) 2_765 . ? N1 Ca1 P1 110.90(6) . . ? N2 Ca1 P1 116.45(6) . . ? O1 Ca1 P1 32.29(5) . . ? O1 Ca1 Ca1 41.38(5) 2_765 2_765 ? N1 Ca1 Ca1 127.65(6) . 2_765 ? N2 Ca1 Ca1 147.88(6) . 2_765 ? O1 Ca1 Ca1 39.01(5) . 2_765 ? P1 Ca1 Ca1 67.63(2) . 2_765 ? O2 Ca2 O2 78.86(7) 2_656 . ? O2 Ca2 N4 127.37(8) 2_656 . ? O2 Ca2 N4 115.37(8) . . ? O2 Ca2 N3 119.67(8) 2_656 . ? O2 Ca2 N3 142.61(8) . . ? N4 Ca2 N3 80.57(8) . . ? O2 Ca2 P2 105.10(5) 2_656 . ? O2 Ca2 P2 31.44(5) . . ? N4 Ca2 P2 110.20(6) . . ? N3 Ca2 P2 112.50(6) . . ? O2 Ca2 Ca2 40.03(5) 2_656 2_656 ? O2 Ca2 Ca2 38.83(5) . 2_656 ? N4 Ca2 Ca2 131.97(6) . 2_656 ? N3 Ca2 Ca2 146.85(6) . 2_656 ? P2 Ca2 Ca2 66.87(2) . 2_656 ? O1 P1 C36 107.66(12) . . ? O1 P1 C30 106.33(12) . . ? C36 P1 C30 96.75(13) . . ? O1 P1 Ca1 52.95(7) . . ? C36 P1 Ca1 118.69(10) . . ? C30 P1 Ca1 142.22(10) . . ? O2 P2 C77 113.2(3) . . ? O2 P2 C71 105.20(13) . . ? C77 P2 C71 100.9(3) . . ? O2 P2 C77A 101.1(3) . . ? C77 P2 C77A 15.6(4) . . ? C71 P2 C77A 95.5(3) . . ? O2 P2 Ca2 50.28(8) . . ? C77 P2 Ca2 119.6(3) . . ? C71 P2 Ca2 137.87(10) . . ? C77A P2 Ca2 120.3(3) . . ? P1 O1 Ca1 142.53(11) . 2_765 ? P1 O1 Ca1 94.76(9) . . ? Ca1 O1 Ca1 99.61(7) 2_765 . ? P2 O2 Ca2 141.18(12) . 2_656 ? P2 O2 Ca2 98.28(10) . . ? Ca2 O2 Ca2 101.14(7) 2_656 . ? C2 N1 C6 117.1(2) . . ? C2 N1 Ca1 122.15(18) . . ? C6 N1 Ca1 120.57(17) . . ? C85 N2 C18 117.6(2) . . ? C85 N2 Ca1 123.90(19) . . ? C18 N2 Ca1 118.44(17) . . ? C43 N3 C47 120.9(2) . . ? C43 N3 Ca2 123.43(19) . . ? C47 N3 Ca2 115.37(17) . . ? C45 N4 C59 116.3(2) . . ? C45 N4 Ca2 119.49(18) . . ? C59 N4 Ca2 123.62(18) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 125.2(3) . . ? N1 C2 C1 119.7(3) . . ? C3 C2 C1 115.1(3) . . ? C2 C3 C85 131.4(3) . . ? C2 C3 H3 114.3 . . ? C85 C3 H3 114.3 . . ? C85 C5 H5A 109.5 . . ? C85 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C85 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 119.7(3) . . ? C7 C6 N1 121.1(3) . . ? C11 C6 N1 119.1(3) . . ? C8 C7 C6 119.0(3) . . ? C8 C7 C12 118.6(3) . . ? C6 C7 C12 122.3(3) . . ? C9 C8 C7 121.2(3) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.8(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 121.3(3) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 119.0(3) . . ? C10 C11 C15 119.2(3) . . ? C6 C11 C15 121.7(3) . . ? C7 C12 C13 111.7(3) . . ? C7 C12 C14 111.3(3) . . ? C13 C12 C14 110.3(3) . . ? C7 C12 H12 107.8 . . ? C13 C12 H12 107.8 . . ? C14 C12 H12 107.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 111.7(3) . . ? C17 C15 C11 109.6(3) . . ? C16 C15 C11 112.6(3) . . ? C17 C15 H15 107.5 . . ? C16 C15 H15 107.5 . . ? C11 C15 H15 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.8(3) . . ? C23 C18 N2 119.1(3) . . ? C19 C18 N2 120.1(3) . . ? C20 C19 C18 117.7(3) . . ? C20 C19 C24 120.4(3) . . ? C18 C19 C24 121.9(3) . . ? C21 C20 C19 121.9(3) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C22 C21 C20 119.6(3) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 121.6(3) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C18 118.3(3) . . ? C22 C23 C27 118.7(3) . . ? C18 C23 C27 123.0(3) . . ? C25 C24 C19 114.8(3) . . ? C25 C24 C26 108.9(3) . . ? C19 C24 C26 112.2(3) . . ? C25 C24 H24 106.8 . . ? C19 C24 H24 106.8 . . ? C26 C24 H24 106.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 112.2(3) . . ? C23 C27 C28 112.7(3) . . ? C29 C27 C28 109.8(3) . . ? C23 C27 H27 107.3 . . ? C29 C27 H27 107.3 . . ? C28 C27 H27 107.3 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C35 118.5(3) . . ? C31 C30 P1 118.8(2) . . ? C35 C30 P1 122.7(2) . . ? C30 C31 C32 121.6(3) . . ? C30 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C33 C32 C31 119.2(3) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C34 C33 C32 120.1(3) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 120.4(3) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C30 C35 C34 120.2(3) . . ? C30 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C41 C36 C37 118.7(3) . . ? C41 C36 P1 122.9(2) . . ? C37 C36 P1 118.3(2) . . ? C38 C37 C36 121.0(3) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 120.2(3) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 119.7(3) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 120.4(3) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C36 C41 C40 120.0(3) . . ? C36 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C43 C42 H42A 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C43 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N3 C43 C44 123.9(3) . . ? N3 C43 C42 122.3(3) . . ? C44 C43 C42 113.7(3) . . ? C45 C44 C43 130.7(3) . . ? C45 C44 H44 114.6 . . ? C43 C44 H44 114.6 . . ? N4 C45 C44 125.8(3) . . ? N4 C45 C46 119.2(3) . . ? C44 C45 C46 115.0(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C52 C47 C48 121.1(3) . . ? C52 C47 N3 117.8(3) . . ? C48 C47 N3 121.0(3) . . ? C49 C48 C47 118.2(3) . . ? C49 C48 C53 119.6(3) . . ? C47 C48 C53 122.3(3) . . ? C50 C49 C48 121.5(3) . . ? C50 C49 H49 119.3 . . ? C48 C49 H49 119.3 . . ? C49 C50 C51 120.3(3) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C50 C51 C52 120.9(3) . . ? C50 C51 H51 119.6 . . ? C52 C51 H51 119.6 . . ? C51 C52 C47 118.1(3) . . ? C51 C52 C56 121.1(3) . . ? C47 C52 C56 120.7(3) . . ? C55 C53 C48 111.5(3) . . ? C55 C53 C54 109.8(3) . . ? C48 C53 C54 111.8(3) . . ? C55 C53 H53 107.9 . . ? C48 C53 H53 107.9 . . ? C54 C53 H53 107.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C58 C56 C52 114.0(3) . . ? C58 C56 C57 109.9(3) . . ? C52 C56 C57 110.5(3) . . ? C58 C56 H56 107.4 . . ? C52 C56 H56 107.4 . . ? C57 C56 H56 107.4 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C64 C59 C60 119.8(3) . . ? C64 C59 N4 121.5(3) . . ? C60 C59 N4 118.7(3) . . ? C61 C60 C59 118.2(3) . . ? C61 C60 C65 118.8(3) . . ? C59 C60 C65 123.0(3) . . ? C62 C61 C60 122.1(3) . . ? C62 C61 H61 119.0 . . ? C60 C61 H61 119.0 . . ? C61 C62 C63 119.3(3) . . ? C61 C62 H62 120.3 . . ? C63 C62 H62 120.3 . . ? C64 C63 C62 121.3(3) . . ? C64 C63 H63 119.4 . . ? C62 C63 H63 119.4 . . ? C63 C64 C59 119.2(3) . . ? C63 C64 C68 119.5(3) . . ? C59 C64 C68 121.3(3) . . ? C67 C65 C60 111.1(3) . . ? C67 C65 C66 109.9(3) . . ? C60 C65 C66 111.7(3) . . ? C67 C65 H65 108.0 . . ? C60 C65 H65 108.0 . . ? C66 C65 H65 108.0 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C64 C68 C69 111.0(3) . . ? C64 C68 C70 112.2(3) . . ? C69 C68 C70 109.5(3) . . ? C64 C68 H68 108.0 . . ? C69 C68 H68 108.0 . . ? C70 C68 H68 108.0 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 C76 117.6(3) . . ? C72 C71 P2 119.9(3) . . ? C76 C71 P2 122.5(2) . . ? C73 C72 C71 121.4(4) . . ? C73 C72 H72 119.3 . . ? C71 C72 H72 119.3 . . ? C74 C73 C72 119.9(4) . . ? C74 C73 H73 120.1 . . ? C72 C73 H73 120.1 . . ? C75 C74 C73 119.7(4) . . ? C75 C74 H74 120.2 . . ? C73 C74 H74 120.2 . . ? C74 C75 C76 120.7(4) . . ? C74 C75 H75 119.6 . . ? C76 C75 H75 119.6 . . ? C75 C76 C71 120.7(3) . . ? C75 C76 H76 119.7 . . ? C71 C76 H76 119.7 . . ? C78 C77 C82 120.0 . . ? C78 C77 P2 120.8(4) . . ? C82 C77 P2 119.2(4) . . ? C77 C78 C79 120.0 . . ? C77 C78 H78 120.0 . . ? C79 C78 H78 120.0 . . ? N2 C85 C3 125.3(3) . . ? N2 C85 C5 120.9(3) . . ? C3 C85 C5 113.8(3) . . ? C80 C79 C78 120.0 . . ? C80 C79 H79 120.0 . . ? C78 C79 H79 120.0 . . ? C81 C80 C79 120.0 . . ? C81 C80 H80 120.0 . . ? C79 C80 H80 120.0 . . ? C80 C81 C82 120.0 . . ? C80 C81 H81 120.0 . . ? C82 C81 H81 120.0 . . ? C81 C82 C77 120.0 . . ? C81 C82 H82 120.0 . . ? C77 C82 H82 120.0 . . ? C82A C77A C78A 117.7(9) . . ? C82A C77A P2 119.0(7) . . ? C78A C77A P2 122.6(8) . . ? C79A C78A C77A 120.7(8) . . ? C79A C78A H78A 119.7 . . ? C77A C78A H78A 119.7 . . ? C80A C79A C78A 120.1(7) . . ? C80A C79A H79A 120.0 . . ? C78A C79A H79A 120.0 . . ? C79A C80A C81A 121.7(10) . . ? C79A C80A H80A 119.1 . . ? C81A C80A H80A 119.1 . . ? C80A C81A C82A 117.7(13) . . ? C80A C81A H81A 121.2 . . ? C82A C81A H81A 121.2 . . ? C77A C82A C81A 121.7(11) . . ? C77A C82A H82A 119.2 . . ? C81A C82A H82A 119.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ca1 P1 O1 -35.96(13) 2_765 . . . ? N1 Ca1 P1 O1 100.55(11) . . . . ? N2 Ca1 P1 O1 -167.71(11) . . . . ? Ca1 Ca1 P1 O1 -22.81(9) 2_765 . . . ? O1 Ca1 P1 C36 -127.11(12) 2_765 . . . ? N1 Ca1 P1 C36 9.41(13) . . . . ? N2 Ca1 P1 C36 101.14(13) . . . . ? O1 Ca1 P1 C36 -91.15(14) . . . . ? Ca1 Ca1 P1 C36 -113.96(11) 2_765 . . . ? O1 Ca1 P1 C30 30.52(17) 2_765 . . . ? N1 Ca1 P1 C30 167.03(16) . . . . ? N2 Ca1 P1 C30 -101.23(17) . . . . ? O1 Ca1 P1 C30 66.48(18) . . . . ? Ca1 Ca1 P1 C30 43.67(15) 2_765 . . . ? O2 Ca2 P2 O2 34.42(14) 2_656 . . . ? N4 Ca2 P2 O2 -105.86(12) . . . . ? N3 Ca2 P2 O2 166.24(11) . . . . ? Ca2 Ca2 P2 O2 22.29(9) 2_656 . . . ? O2 Ca2 P2 C77 131.1(3) 2_656 . . . ? O2 Ca2 P2 C77 96.7(3) . . . . ? N4 Ca2 P2 C77 -9.2(3) . . . . ? N3 Ca2 P2 C77 -97.1(3) . . . . ? Ca2 Ca2 P2 C77 119.0(3) 2_656 . . . ? O2 Ca2 P2 C71 -31.35(18) 2_656 . . . ? O2 Ca2 P2 C71 -65.77(19) . . . . ? N4 Ca2 P2 C71 -171.63(18) . . . . ? N3 Ca2 P2 C71 100.47(18) . . . . ? Ca2 Ca2 P2 C71 -43.48(17) 2_656 . . . ? O2 Ca2 P2 C77A 113.1(3) 2_656 . . . ? O2 Ca2 P2 C77A 78.7(3) . . . . ? N4 Ca2 P2 C77A -27.2(3) . . . . ? N3 Ca2 P2 C77A -115.1(3) . . . . ? Ca2 Ca2 P2 C77A 101.0(3) 2_656 . . . ? C36 P1 O1 Ca1 -134.39(19) . . . 2_765 ? C30 P1 O1 Ca1 -31.6(2) . . . 2_765 ? Ca1 P1 O1 Ca1 112.6(2) . . . 2_765 ? C36 P1 O1 Ca1 113.02(11) . . . . ? C30 P1 O1 Ca1 -144.17(11) . . . . ? O1 Ca1 O1 P1 145.27(12) 2_765 . . . ? N1 Ca1 O1 P1 -92.87(10) . . . . ? N2 Ca1 O1 P1 20.80(19) . . . . ? Ca1 Ca1 O1 P1 145.27(12) 2_765 . . . ? O1 Ca1 O1 Ca1 0.0 2_765 . . 2_765 ? N1 Ca1 O1 Ca1 121.86(8) . . . 2_765 ? N2 Ca1 O1 Ca1 -124.47(13) . . . 2_765 ? P1 Ca1 O1 Ca1 -145.27(12) . . . 2_765 ? C77 P2 O2 Ca2 130.4(4) . . . 2_656 ? C71 P2 O2 Ca2 21.2(2) . . . 2_656 ? C77A P2 O2 Ca2 120.1(4) . . . 2_656 ? Ca2 P2 O2 Ca2 -119.5(2) . . . 2_656 ? C77 P2 O2 Ca2 -110.1(4) . . . . ? C71 P2 O2 Ca2 140.66(12) . . . . ? C77A P2 O2 Ca2 -120.4(3) . . . . ? O2 Ca2 O2 P2 -146.21(14) 2_656 . . . ? N4 Ca2 O2 P2 87.54(11) . . . . ? N3 Ca2 O2 P2 -21.22(17) . . . . ? Ca2 Ca2 O2 P2 -146.21(14) 2_656 . . . ? O2 Ca2 O2 Ca2 0.0 2_656 . . 2_656 ? N4 Ca2 O2 Ca2 -126.25(8) . . . 2_656 ? N3 Ca2 O2 Ca2 124.98(12) . . . 2_656 ? P2 Ca2 O2 Ca2 146.21(14) . . . 2_656 ? O1 Ca1 N1 C2 -85.9(2) 2_765 . . . ? N2 Ca1 N1 C2 30.4(2) . . . . ? O1 Ca1 N1 C2 -179.3(2) . . . . ? P1 Ca1 N1 C2 145.8(2) . . . . ? Ca1 Ca1 N1 C2 -136.88(19) 2_765 . . . ? O1 Ca1 N1 C6 88.6(2) 2_765 . . . ? N2 Ca1 N1 C6 -155.2(2) . . . . ? O1 Ca1 N1 C6 -4.9(2) . . . . ? P1 Ca1 N1 C6 -39.7(2) . . . . ? Ca1 Ca1 N1 C6 37.6(2) 2_765 . . . ? O1 Ca1 N2 C85 102.3(2) 2_765 . . . ? N1 Ca1 N2 C85 -20.8(2) . . . . ? O1 Ca1 N2 C85 -142.6(2) . . . . ? P1 Ca1 N2 C85 -130.4(2) . . . . ? Ca1 Ca1 N2 C85 140.02(19) 2_765 . . . ? O1 Ca1 N2 C18 -80.4(2) 2_765 . . . ? N1 Ca1 N2 C18 156.5(2) . . . . ? O1 Ca1 N2 C18 34.7(3) . . . . ? P1 Ca1 N2 C18 47.0(2) . . . . ? Ca1 Ca1 N2 C18 -42.7(3) 2_765 . . . ? O2 Ca2 N3 C43 -96.4(2) 2_656 . . . ? O2 Ca2 N3 C43 151.29(19) . . . . ? N4 Ca2 N3 C43 31.4(2) . . . . ? P2 Ca2 N3 C43 139.5(2) . . . . ? Ca2 Ca2 N3 C43 -138.75(19) 2_656 . . . ? O2 Ca2 N3 C47 77.0(2) 2_656 . . . ? O2 Ca2 N3 C47 -35.3(2) . . . . ? N4 Ca2 N3 C47 -155.2(2) . . . . ? P2 Ca2 N3 C47 -47.1(2) . . . . ? Ca2 Ca2 N3 C47 34.6(3) 2_656 . . . ? O2 Ca2 N4 C45 82.1(2) 2_656 . . . ? O2 Ca2 N4 C45 177.42(19) . . . . ? N3 Ca2 N4 C45 -38.2(2) . . . . ? P2 Ca2 N4 C45 -148.85(19) . . . . ? Ca2 Ca2 N4 C45 134.57(19) 2_656 . . . ? O2 Ca2 N4 C59 -88.8(2) 2_656 . . . ? O2 Ca2 N4 C59 6.5(2) . . . . ? N3 Ca2 N4 C59 150.9(2) . . . . ? P2 Ca2 N4 C59 40.3(2) . . . . ? Ca2 Ca2 N4 C59 -36.3(2) 2_656 . . . ? C6 N1 C2 C3 161.5(3) . . . . ? Ca1 N1 C2 C3 -23.9(4) . . . . ? C6 N1 C2 C1 -15.8(4) . . . . ? Ca1 N1 C2 C1 158.8(2) . . . . ? N1 C2 C3 C85 -8.2(5) . . . . ? C1 C2 C3 C85 169.2(3) . . . . ? C2 N1 C6 C7 107.8(3) . . . . ? Ca1 N1 C6 C7 -66.9(3) . . . . ? C2 N1 C6 C11 -76.4(3) . . . . ? Ca1 N1 C6 C11 108.9(3) . . . . ? C11 C6 C7 C8 -2.1(4) . . . . ? N1 C6 C7 C8 173.7(3) . . . . ? C11 C6 C7 C12 177.0(3) . . . . ? N1 C6 C7 C12 -7.3(4) . . . . ? C6 C7 C8 C9 0.4(5) . . . . ? C12 C7 C8 C9 -178.7(3) . . . . ? C7 C8 C9 C10 0.9(5) . . . . ? C8 C9 C10 C11 -0.5(5) . . . . ? C9 C10 C11 C6 -1.1(5) . . . . ? C9 C10 C11 C15 -177.7(3) . . . . ? C7 C6 C11 C10 2.4(4) . . . . ? N1 C6 C11 C10 -173.4(3) . . . . ? C7 C6 C11 C15 178.9(3) . . . . ? N1 C6 C11 C15 3.0(4) . . . . ? C8 C7 C12 C13 64.1(4) . . . . ? C6 C7 C12 C13 -114.9(3) . . . . ? C8 C7 C12 C14 -59.6(4) . . . . ? C6 C7 C12 C14 121.3(3) . . . . ? C10 C11 C15 C17 78.1(4) . . . . ? C6 C11 C15 C17 -98.3(4) . . . . ? C10 C11 C15 C16 -47.0(4) . . . . ? C6 C11 C15 C16 136.6(3) . . . . ? C85 N2 C18 C23 91.8(3) . . . . ? Ca1 N2 C18 C23 -85.7(3) . . . . ? C85 N2 C18 C19 -90.9(3) . . . . ? Ca1 N2 C18 C19 91.6(3) . . . . ? C23 C18 C19 C20 -4.2(4) . . . . ? N2 C18 C19 C20 178.5(3) . . . . ? C23 C18 C19 C24 172.4(3) . . . . ? N2 C18 C19 C24 -4.8(4) . . . . ? C18 C19 C20 C21 1.2(5) . . . . ? C24 C19 C20 C21 -175.4(3) . . . . ? C19 C20 C21 C22 2.4(6) . . . . ? C20 C21 C22 C23 -3.1(6) . . . . ? C21 C22 C23 C18 0.2(5) . . . . ? C21 C22 C23 C27 -179.3(3) . . . . ? C19 C18 C23 C22 3.5(4) . . . . ? N2 C18 C23 C22 -179.2(3) . . . . ? C19 C18 C23 C27 -177.0(3) . . . . ? N2 C18 C23 C27 0.3(4) . . . . ? C20 C19 C24 C25 -105.1(4) . . . . ? C18 C19 C24 C25 78.3(4) . . . . ? C20 C19 C24 C26 19.9(4) . . . . ? C18 C19 C24 C26 -156.6(3) . . . . ? C22 C23 C27 C29 78.4(4) . . . . ? C18 C23 C27 C29 -101.0(4) . . . . ? C22 C23 C27 C28 -46.1(4) . . . . ? C18 C23 C27 C28 134.5(3) . . . . ? O1 P1 C30 C31 160.2(2) . . . . ? C36 P1 C30 C31 -89.1(3) . . . . ? Ca1 P1 C30 C31 110.5(2) . . . . ? O1 P1 C30 C35 -21.6(3) . . . . ? C36 P1 C30 C35 89.1(3) . . . . ? Ca1 P1 C30 C35 -71.2(3) . . . . ? C35 C30 C31 C32 -2.1(5) . . . . ? P1 C30 C31 C32 176.3(3) . . . . ? C30 C31 C32 C33 2.8(5) . . . . ? C31 C32 C33 C34 -1.3(5) . . . . ? C32 C33 C34 C35 -0.8(5) . . . . ? C31 C30 C35 C34 -0.1(5) . . . . ? P1 C30 C35 C34 -178.4(2) . . . . ? C33 C34 C35 C30 1.5(5) . . . . ? O1 P1 C36 C41 -6.8(3) . . . . ? C30 P1 C36 C41 -116.3(3) . . . . ? Ca1 P1 C36 C41 50.1(3) . . . . ? O1 P1 C36 C37 177.6(2) . . . . ? C30 P1 C36 C37 68.0(3) . . . . ? Ca1 P1 C36 C37 -125.6(2) . . . . ? C41 C36 C37 C38 1.8(5) . . . . ? P1 C36 C37 C38 177.6(3) . . . . ? C36 C37 C38 C39 -0.5(5) . . . . ? C37 C38 C39 C40 -0.3(5) . . . . ? C38 C39 C40 C41 -0.2(5) . . . . ? C37 C36 C41 C40 -2.3(5) . . . . ? P1 C36 C41 C40 -177.9(2) . . . . ? C39 C40 C41 C36 1.5(5) . . . . ? C47 N3 C43 C44 175.4(3) . . . . ? Ca2 N3 C43 C44 -11.6(4) . . . . ? C47 N3 C43 C42 -2.9(4) . . . . ? Ca2 N3 C43 C42 170.1(2) . . . . ? N3 C43 C44 C45 -20.3(5) . . . . ? C42 C43 C44 C45 158.1(3) . . . . ? C59 N4 C45 C44 -160.1(3) . . . . ? Ca2 N4 C45 C44 28.3(4) . . . . ? C59 N4 C45 C46 18.7(4) . . . . ? Ca2 N4 C45 C46 -152.8(2) . . . . ? C43 C44 C45 N4 10.3(5) . . . . ? C43 C44 C45 C46 -168.6(3) . . . . ? C43 N3 C47 C52 -107.6(3) . . . . ? Ca2 N3 C47 C52 78.8(3) . . . . ? C43 N3 C47 C48 76.7(4) . . . . ? Ca2 N3 C47 C48 -96.9(3) . . . . ? C52 C47 C48 C49 -2.4(4) . . . . ? N3 C47 C48 C49 173.2(3) . . . . ? C52 C47 C48 C53 177.7(3) . . . . ? N3 C47 C48 C53 -6.8(4) . . . . ? C47 C48 C49 C50 0.8(5) . . . . ? C53 C48 C49 C50 -179.2(3) . . . . ? C48 C49 C50 C51 0.5(5) . . . . ? C49 C50 C51 C52 -0.4(5) . . . . ? C50 C51 C52 C47 -1.1(5) . . . . ? C50 C51 C52 C56 174.8(3) . . . . ? C48 C47 C52 C51 2.5(4) . . . . ? N3 C47 C52 C51 -173.2(3) . . . . ? C48 C47 C52 C56 -173.5(3) . . . . ? N3 C47 C52 C56 10.8(4) . . . . ? C49 C48 C53 C55 -69.7(4) . . . . ? C47 C48 C53 C55 110.3(4) . . . . ? C49 C48 C53 C54 53.7(4) . . . . ? C47 C48 C53 C54 -126.4(3) . . . . ? C51 C52 C56 C58 25.6(4) . . . . ? C47 C52 C56 C58 -158.6(3) . . . . ? C51 C52 C56 C57 -98.8(4) . . . . ? C47 C52 C56 C57 77.1(4) . . . . ? C45 N4 C59 C64 -102.5(3) . . . . ? Ca2 N4 C59 C64 68.7(3) . . . . ? C45 N4 C59 C60 79.4(3) . . . . ? Ca2 N4 C59 C60 -109.5(3) . . . . ? C64 C59 C60 C61 0.7(5) . . . . ? N4 C59 C60 C61 178.9(3) . . . . ? C64 C59 C60 C65 -178.4(3) . . . . ? N4 C59 C60 C65 -0.2(5) . . . . ? C59 C60 C61 C62 -1.9(5) . . . . ? C65 C60 C61 C62 177.3(3) . . . . ? C60 C61 C62 C63 1.0(6) . . . . ? C61 C62 C63 C64 1.1(6) . . . . ? C62 C63 C64 C59 -2.2(5) . . . . ? C62 C63 C64 C68 177.7(3) . . . . ? C60 C59 C64 C63 1.3(5) . . . . ? N4 C59 C64 C63 -176.8(3) . . . . ? C60 C59 C64 C68 -178.7(3) . . . . ? N4 C59 C64 C68 3.2(4) . . . . ? C61 C60 C65 C67 -60.5(4) . . . . ? C59 C60 C65 C67 118.6(3) . . . . ? C61 C60 C65 C66 62.6(4) . . . . ? C59 C60 C65 C66 -118.3(3) . . . . ? C63 C64 C68 C69 73.8(4) . . . . ? C59 C64 C68 C69 -106.3(3) . . . . ? C63 C64 C68 C70 -49.1(4) . . . . ? C59 C64 C68 C70 130.8(3) . . . . ? O2 P2 C71 C72 -150.9(3) . . . . ? C77 P2 C71 C72 91.2(4) . . . . ? C77A P2 C71 C72 106.0(4) . . . . ? Ca2 P2 C71 C72 -104.2(3) . . . . ? O2 P2 C71 C76 30.3(3) . . . . ? C77 P2 C71 C76 -87.6(4) . . . . ? C77A P2 C71 C76 -72.8(4) . . . . ? Ca2 P2 C71 C76 77.0(3) . . . . ? C76 C71 C72 C73 0.6(5) . . . . ? P2 C71 C72 C73 -178.2(3) . . . . ? C71 C72 C73 C74 -2.1(6) . . . . ? C72 C73 C74 C75 1.4(6) . . . . ? C73 C74 C75 C76 0.8(6) . . . . ? C74 C75 C76 C71 -2.3(5) . . . . ? C72 C71 C76 C75 1.5(5) . . . . ? P2 C71 C76 C75 -179.6(2) . . . . ? O2 P2 C77 C78 -165.7(5) . . . . ? C71 P2 C77 C78 -53.7(7) . . . . ? C77A P2 C77 C78 -125(3) . . . . ? Ca2 P2 C77 C78 138.1(5) . . . . ? O2 P2 C77 C82 13.2(5) . . . . ? C71 P2 C77 C82 125.1(4) . . . . ? C77A P2 C77 C82 54(2) . . . . ? Ca2 P2 C77 C82 -43.0(5) . . . . ? C82 C77 C78 C79 0.0 . . . . ? P2 C77 C78 C79 178.8(7) . . . . ? C18 N2 C85 C3 -174.4(3) . . . . ? Ca1 N2 C85 C3 3.0(4) . . . . ? C18 N2 C85 C5 3.5(4) . . . . ? Ca1 N2 C85 C5 -179.2(2) . . . . ? C2 C3 C85 N2 20.5(5) . . . . ? C2 C3 C85 C5 -157.6(3) . . . . ? C77 C78 C79 C80 0.0 . . . . ? C78 C79 C80 C81 0.0 . . . . ? C79 C80 C81 C82 0.0 . . . . ? C80 C81 C82 C77 0.0 . . . . ? C78 C77 C82 C81 0.0 . . . . ? P2 C77 C82 C81 -178.8(7) . . . . ? O2 P2 C77A C82A 50.6(10) . . . . ? C77 P2 C77A C82A -92(2) . . . . ? C71 P2 C77A C82A 157.3(9) . . . . ? Ca2 P2 C77A C82A 0.3(11) . . . . ? O2 P2 C77A C78A -139.3(8) . . . . ? C77 P2 C77A C78A 78(2) . . . . ? C71 P2 C77A C78A -32.6(9) . . . . ? Ca2 P2 C77A C78A 170.5(8) . . . . ? C82A C77A C78A C79A -7.3(17) . . . . ? P2 C77A C78A C79A -177.5(9) . . . . ? C77A C78A C79A C80A 3.0(18) . . . . ? C78A C79A C80A C81A 2(2) . . . . ? C79A C80A C81A C82A -3(2) . . . . ? C78A C77A C82A C81A 6.6(17) . . . . ? P2 C77A C82A C81A 177.2(8) . . . . ? C80A C81A C82A C77A -1.7(19) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.389 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.066