# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Dautel, O. J.' ;"Architecture Mol\'eculaire et Mat\'eriaux Nanostructur\'es Instituts Charles Gerhardt Montpellier UMR CNRS 5253, Ecole Nationale Sup\'erieure de Chimie de Montpellier 8 rue de l'Ecole Normale 34396 Montpellier Cedex 05 France" ; 'Moreau, J. J. E.' ;"Architecture Mol\'eculaire et Mat\'eriaux Nanostructur\'es Instituts Charles Gerhardt Montpellier UMR CNRS 5253, Ecole Nationale Sup\'erieure de Chimie de Montpellier 8 rue de l'Ecole Normale 34396 Montpellier Cedex 05 France" ; 'Reynes, M.' ;"Architecture Mol\'eculaire et Mat\'eriaux Nanostructur\'es Instituts Charles Gerhardt Montpellier UMR CNRS 5253, Ecole Nationale Sup\'erieure de Chimie de Montpellier 8 rue de l'Ecole Normale 34396 Montpellier Cedex 05 France" ; 'Virieux, D.' ;"Architecture Mol\'eculaire et Mat\'eriaux Nanostructur\'es Instituts Charles Gerhardt Montpellier UMR CNRS 5253, Ecole Nationale Sup\'erieure de Chimie de Montpellier 8 rue de l'Ecole Normale 34396 Montpellier Cedex 05 France" ; 'Flot, D. M. M. P.' ;European Synchrotron Radiation Facility 6 rue Jules Horowitz BP 220 38043 Grenoble cedex 9 France ; _publ_contact_author_address ;"Architecture Mol\'eculaire et Mat\'eriaux Nanostructur\'es Instituts Charles Gerhardt Montpellier UMR CNRS 5253 Ecole Nationale Sup\'erieure de Chimie de Montpellier 8 rue de l'Ecole Normale 34396 Montpellier Cedex 05 France" ; _publ_contact_author_email olivier.dautel@enscm.fr _publ_contact_author_fax '04 67 14 72 12' _publ_contact_author_phone '04 67 14 72 17' _publ_contact_author_name ; Dautel, O. J. ; data_mrm26a _database_code_depnum_ccdc_archive 'CCDC 812014' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H35 Cl6 N3 O6 P3' _chemical_formula_weight 1271.58 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.769(2) _cell_length_b 15.024(2) _cell_length_c 21.216(2) _cell_angle_alpha 94.818(3) _cell_angle_beta 99.983(5) _cell_angle_gamma 98.226(6) _cell_volume 2707.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21428 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 30.77 _exptl_crystal_description needle _exptl_crystal_colour none _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1294 _exptl_absorpt_coefficient_mu 0.468 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.87260 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'ESRF synchrotron' _diffrn_source_type 'ID23-2 gemini-microfocus' _diffrn_radiation_monochromator Si111 _diffrn_measurement_device_type 'ESRF-EMBL MD2M diffractometer' _diffrn_measurement_method oscillation _diffrn_detector_area_resol_mean ? _diffrn_detector_type 'marMOSAIC 225' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30257 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 30.77 _reflns_number_total 7949 _reflns_number_gt 6770 _reflns_threshold_expression >2sigma(I) _computing_data_collection mxCuBE _computing_cell_refinement 'XDS (Kabsch, 2010)' _computing_data_reduction 'XDS (Kabsch, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer, WinGX' _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^)+(0.1163P)^2^+5.3925P] 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 7949 _refine_ls_number_parameters 791 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1965 _refine_ls_wR_factor_gt 0.1895 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 P1 P 0.78469(13) 0.29338(6) 0.33811(5) 0.0250(3) Uani 1 1 d . . . P2 P 0.96391(13) 0.18179(6) 0.28311(5) 0.0255(3) Uani 1 1 d . . . P3 P 0.83890(13) 0.31247(6) 0.21451(4) 0.0257(3) Uani 1 1 d . . . O1 O 0.6145(3) 0.25961(17) 0.35453(12) 0.0280(6) Uani 1 1 d . . . O2 O 0.8488(3) 0.36658(18) 0.40079(13) 0.0289(6) Uani 1 1 d . . . O3 O 1.1483(3) 0.17975(17) 0.30932(13) 0.0296(6) Uani 1 1 d . . . O4 O 0.9104(3) 0.07454(17) 0.26288(14) 0.0295(6) Uani 1 1 d . . . O5 O 0.9332(3) 0.40109(18) 0.19053(12) 0.0287(6) Uani 1 1 d . . . O6 O 0.7013(4) 0.28613(18) 0.15084(13) 0.0335(7) Uani 1 1 d . . . N1 N 0.8852(4) 0.2135(2) 0.34086(15) 0.0300(8) Uani 1 1 d . . . N2 N 0.9427(4) 0.2346(2) 0.22156(15) 0.0292(8) Uani 1 1 d . . . N3 N 0.7682(4) 0.3431(2) 0.27498(16) 0.0293(8) Uani 1 1 d . . . C1 C 0.5994(5) 0.3069(2) 0.41240(17) 0.0226(8) Uani 1 1 d . . . C2 C 0.4689(5) 0.2992(2) 0.43900(17) 0.0244(8) Uani 1 1 d . . . H2 H 0.3765 0.2587 0.4191 0.029 Uiso 1 1 calc R . . C3 C 0.4750(5) 0.3539(2) 0.49790(17) 0.0235(8) Uani 1 1 d . . . C4 C 0.3371(5) 0.3498(3) 0.52813(18) 0.0274(9) Uani 1 1 d . . . C5 C 0.1951(5) 0.2920(3) 0.5005(2) 0.0336(10) Uani 1 1 d . . . H5 H 0.1900 0.2550 0.4614 0.040 Uiso 1 1 calc R . . C6 C 0.0638(6) 0.2876(3) 0.5284(2) 0.0403(11) Uani 1 1 d . . . H6 H -0.0302 0.2484 0.5086 0.048 Uiso 1 1 calc R . . C7 C 0.0710(6) 0.3420(3) 0.5866(2) 0.0423(12) Uani 1 1 d . . . H7 H -0.0178 0.3386 0.6069 0.051 Uiso 1 1 calc R . . C8 C 0.2061(6) 0.3998(3) 0.6140(2) 0.0379(11) Uani 1 1 d . . . H8 H 0.2083 0.4368 0.6528 0.045 Uiso 1 1 calc R . . C9 C 0.3429(5) 0.4062(3) 0.58637(18) 0.0294(9) Uani 1 1 d . . . C10 C 0.4859(5) 0.4679(3) 0.61511(18) 0.0303(10) Uani 1 1 d . . . C11 C 0.4950(6) 0.5281(3) 0.67175(19) 0.0377(11) Uani 1 1 d . . . H11 H 0.4059 0.5273 0.6917 0.045 Uiso 1 1 calc R . . C12 C 0.6306(7) 0.5874(3) 0.69835(19) 0.0406(12) Uani 1 1 d . . . H12 H 0.6330 0.6280 0.7355 0.049 Uiso 1 1 calc R . . C13 C 0.7627(6) 0.5880(3) 0.6712(2) 0.0392(12) Uani 1 1 d . . . H13 H 0.8566 0.6278 0.6902 0.047 Uiso 1 1 calc R . . C14 C 0.7584(6) 0.5305(3) 0.61616(18) 0.0322(10) Uani 1 1 d . . . H14 H 0.8500 0.5312 0.5979 0.039 Uiso 1 1 calc R . . C15 C 0.6211(5) 0.4714(2) 0.58686(17) 0.0262(9) Uani 1 1 d . . . C16 C 0.6147(5) 0.4139(2) 0.52651(17) 0.0243(9) Uani 1 1 d . . . C17 C 0.7468(5) 0.4204(2) 0.49560(17) 0.0250(8) Uani 1 1 d . . . H17 H 0.8408 0.4607 0.5138 0.030 Uiso 1 1 calc R . . C18 C 0.7346(5) 0.3670(2) 0.43901(17) 0.0243(8) Uani 1 1 d . . . C19 C 1.1758(5) 0.0903(2) 0.30374(18) 0.0258(9) Uani 1 1 d . . . C20 C 1.3163(5) 0.0628(3) 0.32035(17) 0.0259(9) Uani 1 1 d . . . H20 H 1.4084 0.1051 0.3378 0.031 Uiso 1 1 calc R . . C21 C 1.3214(5) -0.0322(3) 0.31067(17) 0.0250(9) Uani 1 1 d . . . C22 C 1.4719(5) -0.0652(3) 0.32602(17) 0.0271(9) Uani 1 1 d . . . C23 C 1.6123(5) -0.0055(3) 0.34978(19) 0.0324(10) Uani 1 1 d . . . H23 H 1.6104 0.0577 0.3546 0.039 Uiso 1 1 calc R . . C24 C 1.7533(5) -0.0363(3) 0.3664(2) 0.0367(10) Uani 1 1 d . . . H24 H 1.8470 0.0052 0.3828 0.044 Uiso 1 1 calc R . . C25 C 1.7568(6) -0.1286(3) 0.3588(2) 0.0420(11) Uani 1 1 d . . . H25 H 1.8531 -0.1503 0.3709 0.050 Uiso 1 1 calc R . . C26 C 1.6241(6) -0.1880(3) 0.3342(2) 0.0392(11) Uani 1 1 d . . . H26 H 1.6297 -0.2508 0.3286 0.047 Uiso 1 1 calc R . . C27 C 1.4762(5) -0.1587(3) 0.31654(19) 0.0308(9) Uani 1 1 d . . . C28 C 1.3322(5) -0.2225(3) 0.29035(19) 0.0318(10) Uani 1 1 d . . . C29 C 1.3334(6) -0.3163(3) 0.2778(2) 0.0415(11) Uani 1 1 d . . . H29 H 1.4305 -0.3382 0.2856 0.050 Uiso 1 1 calc R . . C30 C 1.1969(7) -0.3771(3) 0.2543(2) 0.0466(13) Uani 1 1 d . . . H30 H 1.2012 -0.4397 0.2458 0.056 Uiso 1 1 calc R . . C31 C 1.0553(6) -0.3464(3) 0.2435(2) 0.0395(11) Uani 1 1 d . . . H31 H 0.9612 -0.3881 0.2284 0.047 Uiso 1 1 calc R . . C32 C 1.0495(6) -0.2554(3) 0.2545(2) 0.0345(10) Uani 1 1 d . . . H32 H 0.9508 -0.2352 0.2468 0.041 Uiso 1 1 calc R . . C33 C 1.1877(5) -0.1909(3) 0.27708(18) 0.0281(9) Uani 1 1 d . . . C34 C 1.1814(5) -0.0936(2) 0.28618(17) 0.0246(8) Uani 1 1 d . . . C35 C 1.0384(5) -0.0610(3) 0.26969(18) 0.0255(8) Uani 1 1 d . . . H35 H 0.9437 -0.1015 0.2530 0.031 Uiso 1 1 calc R . . C36 C 1.0392(5) 0.0295(3) 0.27829(18) 0.0252(8) Uani 1 1 d . . . C37 C 0.8520(5) 0.4156(3) 0.13041(18) 0.0296(9) Uani 1 1 d . . . C38 C 0.8921(5) 0.4851(3) 0.09598(19) 0.0294(9) Uani 1 1 d . . . H38 H 0.9819 0.5298 0.1119 0.035 Uiso 1 1 calc R . . C39 C 0.7947(5) 0.4886(3) 0.03521(19) 0.0312(10) Uani 1 1 d . . . C40 C 0.8298(6) 0.5627(3) -0.0032(2) 0.0349(10) Uani 1 1 d . . . C41 C 0.9510(6) 0.6360(3) 0.0205(2) 0.0404(11) Uani 1 1 d . . . H41 H 1.0108 0.6377 0.0625 0.049 Uiso 1 1 calc R . . C42 C 0.9852(7) 0.7061(3) -0.0162(2) 0.0462(12) Uani 1 1 d . . . H42 H 1.0689 0.7543 0.0004 0.055 Uiso 1 1 calc R . . C43 C 0.8969(7) 0.7052(3) -0.0769(2) 0.0515(14) Uani 1 1 d . . . H43 H 0.9204 0.7529 -0.1021 0.062 Uiso 1 1 calc R . . C44 C 0.7759(7) 0.6361(3) -0.1011(2) 0.0466(13) Uani 1 1 d . . . H44 H 0.7157 0.6373 -0.1427 0.056 Uiso 1 1 calc R . . C45 C 0.7381(6) 0.5625(3) -0.0654(2) 0.0391(11) Uani 1 1 d . . . C46 C 0.6094(6) 0.4896(3) -0.0909(2) 0.0387(11) Uani 1 1 d . . . C47 C 0.5181(7) 0.4840(4) -0.1536(2) 0.0468(13) Uani 1 1 d . . . H47 H 0.5452 0.5287 -0.1807 0.056 Uiso 1 1 calc R . . C48 C 0.3946(7) 0.4182(4) -0.1765(2) 0.0530(14) Uani 1 1 d . . . H48 H 0.3385 0.4164 -0.2192 0.064 Uiso 1 1 calc R . . C49 C 0.3489(6) 0.3528(4) -0.1375(2) 0.0487(13) Uani 1 1 d . . . H49 H 0.2586 0.3082 -0.1526 0.058 Uiso 1 1 calc R . . C50 C 0.4370(6) 0.3538(3) -0.0765(2) 0.0421(11) Uani 1 1 d . . . H50 H 0.4080 0.3079 -0.0506 0.051 Uiso 1 1 calc R . . C51 C 0.5679(6) 0.4206(3) -0.0519(2) 0.0350(10) Uani 1 1 d . . . C52 C 0.6635(5) 0.4206(3) 0.01206(19) 0.0324(10) Uani 1 1 d . . . C53 C 0.6258(5) 0.3504(3) 0.0507(2) 0.0319(9) Uani 1 1 d . . . H53 H 0.5364 0.3050 0.0365 0.038 Uiso 1 1 calc R . . C54 C 0.7208(5) 0.3503(3) 0.10792(19) 0.0293(9) Uani 1 1 d . . . Cl3 Cl -0.6498(2) 0.11104(13) -0.16222(8) 0.0792(5) Uani 1 1 d . A . C55 C -0.5020(7) -0.0317(4) -0.1758(2) 0.0519(13) Uani 1 1 d . A . H55 H -0.6032 -0.0660 -0.1916 0.08(2) Uiso 1 1 calc R . . C56 C -0.3705(6) -0.0725(4) -0.1700(2) 0.0496(13) Uani 1 1 d . . . H56 H -0.3813 -0.1356 -0.1824 0.060 Uiso 0.219(3) 1 calc PR A 2 C57 C -0.2243(7) -0.0240(4) -0.1468(2) 0.0504(13) Uani 1 1 d . A . H57 H -0.1353 -0.0539 -0.1427 0.060 Uiso 0.781(3) 1 calc PR A 1 C58 C -0.2053(7) 0.0675(4) -0.1295(2) 0.0530(14) Uani 1 1 d . . . H58 H -0.1034 0.1009 -0.1135 0.064 Uiso 0.781(3) 1 calc PR A 1 C59 C -0.3364(7) 0.1115(4) -0.1353(2) 0.0563(14) Uani 1 1 d . A . H59 H -0.3253 0.1750 -0.1239 0.068 Uiso 0.219(3) 1 calc PR A 2 C60 C -0.4838(7) 0.0597(4) -0.1582(2) 0.0535(14) Uani 1 1 d . . . Cl1 Cl -0.3922(2) -0.18851(10) -0.19508(8) 0.0496(5) Uani 0.781(3) 1 d P A 1 Cl2 Cl -0.3110(3) 0.22384(12) -0.11424(9) 0.0614(6) Uani 0.781(3) 1 d P A 1 Cl4 Cl -0.0231(10) 0.1305(5) -0.1116(3) 0.072(2) Uani 0.219(3) 1 d P A 2 Cl5 Cl -0.0555(9) -0.0577(5) -0.1286(3) 0.063(2) Uani 0.219(3) 1 d P A 2 Cl6 Cl 0.2811(2) 0.14318(10) 0.00835(8) 0.0526(6) Uani 0.840(5) 1 d P A . Cl7 Cl 0.1441(3) -0.05600(15) -0.04467(12) 0.0670(9) Uani 0.660(5) 1 d P . . C61 C 0.3401(7) -0.0258(3) -0.0208(2) 0.0478(12) Uani 1 1 d . . . C62 C 0.5632(7) 0.0888(3) 0.0245(2) 0.0480(13) Uani 1 1 d . . . H62 H 0.6056 0.1496 0.0413 0.058 Uiso 1 1 calc R . . C63 C 0.4046(7) 0.0639(3) 0.0037(2) 0.0444(12) Uani 1 1 d . . . Cl8 Cl 0.2983(3) 0.82353(15) 0.44962(10) 0.0592(8) Uani 0.630(5) 1 d P . . Cl9 Cl 0.1421(2) 0.98976(18) 0.45788(8) 0.0805(8) Uani 0.870(5) 1 d P . . C64 C 0.5673(7) 0.9224(5) 0.4968(2) 0.0560(15) Uani 1 1 d . . . H64 H 0.6133 0.8690 0.4945 0.067 Uiso 1 1 calc R . . C65 C 0.3411(6) 0.9966(5) 0.4807(2) 0.0556(15) Uani 1 1 d . . . C66 C 0.4063(7) 0.9176(5) 0.4773(2) 0.0587(16) 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 P1 0.0336(6) 0.0233(5) 0.0220(5) 0.0065(4) 0.0083(4) 0.0118(4) P2 0.0317(6) 0.0212(5) 0.0272(5) 0.0063(4) 0.0072(4) 0.0125(4) P3 0.0362(6) 0.0229(5) 0.0210(5) 0.0080(4) 0.0064(4) 0.0107(4) O1 0.0354(17) 0.0273(14) 0.0225(13) 0.0000(11) 0.0066(12) 0.0091(11) O2 0.0313(17) 0.0286(14) 0.0286(14) 0.0024(11) 0.0091(12) 0.0070(11) O3 0.0361(17) 0.0175(13) 0.0363(15) 0.0040(11) 0.0058(13) 0.0089(11) O4 0.0266(16) 0.0228(14) 0.0418(16) 0.0079(11) 0.0047(13) 0.0123(11) O5 0.0400(18) 0.0291(14) 0.0187(13) 0.0068(11) 0.0048(12) 0.0093(12) O6 0.0467(19) 0.0259(14) 0.0294(15) 0.0109(11) 0.0073(13) 0.0060(12) N1 0.041(2) 0.0298(18) 0.0263(17) 0.0134(14) 0.0110(15) 0.0178(15) N2 0.038(2) 0.0296(17) 0.0252(17) 0.0057(13) 0.0115(15) 0.0134(15) N3 0.039(2) 0.0260(17) 0.0285(17) 0.0083(13) 0.0099(15) 0.0175(14) C1 0.032(2) 0.0218(18) 0.0164(17) 0.0058(14) 0.0044(16) 0.0099(15) C2 0.031(2) 0.0225(18) 0.0213(18) 0.0075(14) 0.0034(16) 0.0087(15) C3 0.031(2) 0.0247(19) 0.0199(18) 0.0100(14) 0.0071(16) 0.0153(16) C4 0.038(3) 0.028(2) 0.0242(19) 0.0159(15) 0.0092(17) 0.0194(17) C5 0.038(3) 0.038(2) 0.030(2) 0.0128(17) 0.0084(19) 0.0154(19) C6 0.031(3) 0.053(3) 0.044(3) 0.023(2) 0.013(2) 0.014(2) C7 0.042(3) 0.060(3) 0.038(2) 0.025(2) 0.020(2) 0.027(2) C8 0.054(3) 0.046(3) 0.027(2) 0.0188(19) 0.016(2) 0.031(2) C9 0.042(3) 0.034(2) 0.0236(19) 0.0182(16) 0.0133(18) 0.0258(18) C10 0.051(3) 0.027(2) 0.0192(18) 0.0127(15) 0.0059(18) 0.0246(18) C11 0.069(3) 0.032(2) 0.022(2) 0.0125(17) 0.013(2) 0.033(2) C12 0.076(4) 0.032(2) 0.0175(19) 0.0053(16) 0.002(2) 0.028(2) C13 0.061(3) 0.029(2) 0.025(2) 0.0036(17) -0.006(2) 0.015(2) C14 0.047(3) 0.028(2) 0.0215(19) 0.0064(16) -0.0022(18) 0.0135(18) C15 0.042(3) 0.0239(19) 0.0172(18) 0.0105(14) 0.0045(17) 0.0175(17) C16 0.037(2) 0.0221(18) 0.0178(17) 0.0083(14) 0.0036(16) 0.0145(16) C17 0.033(2) 0.0214(18) 0.0215(18) 0.0075(14) 0.0013(16) 0.0086(15) C18 0.029(2) 0.027(2) 0.0223(18) 0.0089(15) 0.0095(16) 0.0126(16) C19 0.034(2) 0.0214(19) 0.0246(19) 0.0049(15) 0.0069(17) 0.0117(16) C20 0.030(2) 0.027(2) 0.0215(18) 0.0070(15) 0.0018(16) 0.0062(16) C21 0.033(2) 0.028(2) 0.0200(18) 0.0127(15) 0.0086(16) 0.0152(17) C22 0.031(2) 0.038(2) 0.0178(18) 0.0147(16) 0.0075(16) 0.0154(18) C23 0.037(3) 0.038(2) 0.027(2) 0.0157(17) 0.0083(18) 0.0110(19) C24 0.031(3) 0.055(3) 0.031(2) 0.023(2) 0.0078(19) 0.017(2) C25 0.035(3) 0.061(3) 0.040(2) 0.028(2) 0.010(2) 0.024(2) C26 0.047(3) 0.042(3) 0.040(2) 0.024(2) 0.014(2) 0.026(2) C27 0.037(3) 0.037(2) 0.026(2) 0.0191(17) 0.0106(18) 0.0192(19) C28 0.044(3) 0.031(2) 0.027(2) 0.0138(16) 0.0093(19) 0.0193(18) C29 0.049(3) 0.032(2) 0.050(3) 0.015(2) 0.008(2) 0.022(2) C30 0.071(4) 0.024(2) 0.049(3) 0.0112(19) 0.011(3) 0.022(2) C31 0.051(3) 0.026(2) 0.043(3) 0.0037(18) 0.010(2) 0.0083(19) C32 0.042(3) 0.030(2) 0.033(2) 0.0077(17) 0.0032(19) 0.0128(18) C33 0.037(3) 0.027(2) 0.0242(19) 0.0085(15) 0.0078(17) 0.0120(17) C34 0.034(2) 0.0234(19) 0.0203(18) 0.0088(14) 0.0081(16) 0.0098(16) C35 0.029(2) 0.0245(19) 0.0262(19) 0.0067(15) 0.0073(17) 0.0095(16) C36 0.024(2) 0.029(2) 0.0246(19) 0.0058(15) 0.0057(16) 0.0108(16) C37 0.042(3) 0.029(2) 0.0222(19) 0.0073(16) 0.0072(18) 0.0131(18) C38 0.041(3) 0.0245(19) 0.028(2) 0.0069(16) 0.0129(18) 0.0117(17) C39 0.045(3) 0.027(2) 0.029(2) 0.0078(16) 0.0158(19) 0.0197(19) C40 0.049(3) 0.034(2) 0.033(2) 0.0114(18) 0.022(2) 0.024(2) C41 0.061(3) 0.034(2) 0.034(2) 0.0111(19) 0.018(2) 0.018(2) C42 0.067(4) 0.033(2) 0.049(3) 0.015(2) 0.028(3) 0.017(2) C43 0.078(4) 0.045(3) 0.047(3) 0.024(2) 0.031(3) 0.027(3) C44 0.066(4) 0.053(3) 0.034(2) 0.023(2) 0.020(2) 0.031(3) C45 0.054(3) 0.047(3) 0.031(2) 0.0172(19) 0.023(2) 0.032(2) C46 0.047(3) 0.050(3) 0.029(2) 0.0125(19) 0.014(2) 0.029(2) C47 0.056(3) 0.067(3) 0.029(2) 0.019(2) 0.015(2) 0.031(3) C48 0.052(3) 0.082(4) 0.030(2) 0.015(2) 0.004(2) 0.030(3) C49 0.045(3) 0.060(3) 0.041(3) 0.003(2) -0.003(2) 0.023(2) C50 0.049(3) 0.043(3) 0.038(2) 0.009(2) 0.003(2) 0.022(2) C51 0.042(3) 0.042(2) 0.028(2) 0.0058(18) 0.0097(19) 0.026(2) C52 0.042(3) 0.033(2) 0.030(2) 0.0087(17) 0.0111(19) 0.0223(19) C53 0.037(3) 0.029(2) 0.032(2) 0.0065(17) 0.0065(19) 0.0121(17) C54 0.040(3) 0.025(2) 0.027(2) 0.0080(16) 0.0101(18) 0.0126(17) Cl3 0.0823(12) 0.0957(12) 0.0622(9) 0.0083(8) 0.0010(8) 0.0388(9) C55 0.051(4) 0.073(4) 0.035(3) 0.013(2) 0.009(2) 0.015(3) C56 0.048(3) 0.070(3) 0.036(2) 0.016(2) 0.013(2) 0.015(3) C57 0.053(3) 0.069(4) 0.034(2) 0.018(2) 0.009(2) 0.019(3) C58 0.043(3) 0.084(4) 0.036(3) 0.009(2) 0.010(2) 0.018(3) C59 0.064(4) 0.077(4) 0.031(2) 0.008(2) 0.011(2) 0.015(3) C60 0.058(4) 0.083(4) 0.026(2) 0.014(2) 0.010(2) 0.025(3) Cl1 0.0626(11) 0.0434(9) 0.0485(9) 0.0193(7) 0.0213(8) 0.0064(7) Cl2 0.0759(14) 0.0546(10) 0.0578(11) -0.0023(8) 0.0164(9) 0.0243(9) Cl4 0.093(6) 0.073(5) 0.046(4) -0.009(3) 0.002(3) 0.027(4) Cl5 0.073(5) 0.088(5) 0.041(3) 0.027(3) 0.017(3) 0.039(4) Cl6 0.0662(12) 0.0414(8) 0.0622(10) 0.0163(7) 0.0261(8) 0.0257(7) Cl7 0.0576(15) 0.0596(14) 0.0775(16) 0.0196(11) -0.0036(11) 0.0015(10) C61 0.057(3) 0.042(3) 0.048(3) 0.015(2) 0.012(2) 0.013(2) C62 0.064(4) 0.033(2) 0.048(3) 0.007(2) 0.012(3) 0.011(2) C63 0.061(4) 0.041(3) 0.039(2) 0.013(2) 0.017(2) 0.020(2) Cl8 0.0704(17) 0.0607(14) 0.0437(12) 0.0170(9) 0.0139(10) -0.0087(11) Cl9 0.0406(11) 0.170(2) 0.0386(9) 0.0302(10) 0.0060(7) 0.0328(11) C64 0.061(4) 0.090(4) 0.026(2) 0.028(3) 0.012(2) 0.028(3) C65 0.039(3) 0.107(5) 0.024(2) 0.024(3) 0.005(2) 0.015(3) C66 0.058(4) 0.096(4) 0.024(2) 0.021(3) 0.011(2) 0.008(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 P1 N3 1.583(3) . ? P1 N1 1.587(3) . ? P1 O1 1.612(3) . ? P1 O2 1.616(3) . ? P2 N1 1.579(4) . ? P2 N2 1.582(3) . ? P2 O4 1.612(3) . ? P2 O3 1.622(3) . ? P3 N3 1.581(3) . ? P3 N2 1.583(3) . ? P3 O6 1.627(3) . ? P3 O5 1.631(3) . ? O1 C1 1.403(5) . ? O2 C18 1.393(5) . ? O3 C19 1.398(4) . ? O4 C36 1.403(5) . ? O5 C37 1.399(5) . ? O6 C54 1.394(5) . ? C1 C2 1.356(6) . ? C1 C18 1.384(6) . ? C2 C3 1.425(5) . ? C2 H2 0.9500 . ? C3 C16 1.420(6) . ? C3 C4 1.459(6) . ? C4 C5 1.414(6) . ? C4 C9 1.428(6) . ? C5 C6 1.379(7) . ? C5 H5 0.9500 . ? C6 C7 1.409(7) . ? C6 H6 0.9500 . ? C7 C8 1.370(7) . ? C7 H7 0.9500 . ? C8 C9 1.418(6) . ? C8 H8 0.9500 . ? C9 C10 1.453(6) . ? C10 C15 1.415(6) . ? C10 C11 1.425(6) . ? C11 C12 1.381(7) . ? C11 H11 0.9500 . ? C12 C13 1.380(7) . ? C12 H12 0.9500 . ? C13 C14 1.384(6) . ? C13 H13 0.9500 . ? C14 C15 1.402(6) . ? C14 H14 0.9500 . ? C15 C16 1.471(5) . ? C16 C17 1.423(6) . ? C17 C18 1.366(5) . ? C17 H17 0.9500 . ? C19 C20 1.353(6) . ? C19 C36 1.394(6) . ? C20 C21 1.433(5) . ? C20 H20 0.9500 . ? C21 C34 1.415(6) . ? C21 C22 1.470(6) . ? C22 C23 1.403(6) . ? C22 C27 1.408(6) . ? C23 C24 1.381(6) . ? C23 H23 0.9500 . ? C24 C25 1.387(7) . ? C24 H24 0.9500 . ? C25 C26 1.356(7) . ? C25 H25 0.9500 . ? C26 C27 1.429(6) . ? C26 H26 0.9500 . ? C27 C28 1.464(6) . ? C28 C33 1.407(6) . ? C28 C29 1.413(6) . ? C29 C30 1.385(7) . ? C29 H29 0.9500 . ? C30 C31 1.375(7) . ? C30 H30 0.9500 . ? C31 C32 1.378(6) . ? C31 H31 0.9500 . ? C32 C33 1.422(6) . ? C32 H32 0.9500 . ? C33 C34 1.470(5) . ? C34 C35 1.409(6) . ? C35 C36 1.355(5) . ? C35 H35 0.9500 . ? C37 C38 1.365(6) . ? C37 C54 1.386(6) . ? C38 C39 1.427(6) . ? C38 H38 0.9500 . ? C39 C52 1.411(7) . ? C39 C40 1.463(6) . ? C40 C41 1.408(7) . ? C40 C45 1.421(6) . ? C41 C42 1.390(6) . ? C41 H41 0.9500 . ? C42 C43 1.380(8) . ? C42 H42 0.9500 . ? C43 C44 1.369(8) . ? C43 H43 0.9500 . ? C44 C45 1.424(6) . ? C44 H44 0.9500 . ? C45 C46 1.450(7) . ? C46 C47 1.418(6) . ? C46 C51 1.426(6) . ? C47 C48 1.348(8) . ? C47 H47 0.9500 . ? C48 C49 1.396(8) . ? C48 H48 0.9500 . ? C49 C50 1.384(6) . ? C49 H49 0.9500 . ? C50 C51 1.405(7) . ? C50 H50 0.9500 . ? C51 C52 1.466(6) . ? C52 C53 1.426(6) . ? C53 C54 1.349(6) . ? C53 H53 0.9500 . ? Cl3 C60 1.735(6) . ? C55 C60 1.372(8) . ? C55 C56 1.373(8) . ? C55 H55 0.9500 . ? C56 C57 1.367(8) . ? C56 Cl1 1.753(6) . ? C56 H56 0.9500 . ? C57 C58 1.372(8) . ? C57 Cl5 1.627(8) . ? C57 H57 0.9500 . ? C58 C59 1.398(8) . ? C58 Cl4 1.700(10) . ? C58 H58 0.9500 . ? C59 C60 1.395(8) . ? C59 Cl2 1.682(6) . ? C59 H59 0.9500 . ? Cl5 Cl7 2.265(7) . ? Cl6 C63 1.729(5) . ? Cl7 C61 1.689(6) . ? C61 C62 1.364(7) 2_655 ? C61 C63 1.403(7) . ? C62 C61 1.364(7) 2_655 ? C62 C63 1.371(8) . ? C62 H62 0.9500 . ? Cl8 C66 1.588(7) . ? Cl9 C65 1.714(6) . ? C64 C65 1.358(9) 2_676 ? C64 C66 1.390(8) . ? C64 H64 0.9500 . ? C65 C64 1.358(9) 2_676 ? C65 C66 1.391(9) . ? 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 N3 P1 N1 117.35(18) . . ? N3 P1 O1 110.60(17) . . ? N1 P1 O1 110.10(17) . . ? N3 P1 O2 109.97(16) . . ? N1 P1 O2 109.83(17) . . ? O1 P1 O2 97.13(14) . . ? N1 P2 N2 117.39(17) . . ? N1 P2 O4 109.87(17) . . ? N2 P2 O4 110.40(16) . . ? N1 P2 O3 109.58(17) . . ? N2 P2 O3 110.35(17) . . ? O4 P2 O3 97.42(14) . . ? N3 P3 N2 117.12(17) . . ? N3 P3 O6 110.61(18) . . ? N2 P3 O6 109.77(17) . . ? N3 P3 O5 109.26(16) . . ? N2 P3 O5 110.95(18) . . ? O6 P3 O5 97.34(14) . . ? C1 O1 P1 109.7(2) . . ? C18 O2 P1 109.6(2) . . ? C19 O3 P2 109.3(2) . . ? C36 O4 P2 109.8(2) . . ? C37 O5 P3 108.7(2) . . ? C54 O6 P3 109.2(3) . . ? P2 N1 P1 122.50(19) . . ? P2 N2 P3 122.7(2) . . ? P3 N3 P1 122.6(2) . . ? C2 C1 C18 122.8(4) . . ? C2 C1 O1 125.7(3) . . ? C18 C1 O1 111.4(4) . . ? C1 C2 C3 117.7(4) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C16 C3 C2 119.8(4) . . ? C16 C3 C4 119.9(3) . . ? C2 C3 C4 120.2(4) . . ? C5 C4 C9 118.5(4) . . ? C5 C4 C3 121.6(4) . . ? C9 C4 C3 120.0(4) . . ? C6 C5 C4 122.2(4) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 119.1(5) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C8 C7 C6 120.0(5) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 122.2(4) . . ? C7 C8 H8 118.9 . . ? C9 C8 H8 118.9 . . ? C8 C9 C4 117.9(4) . . ? C8 C9 C10 122.3(4) . . ? C4 C9 C10 119.8(4) . . ? C15 C10 C11 117.5(4) . . ? C15 C10 C9 120.8(4) . . ? C11 C10 C9 121.7(4) . . ? C12 C11 C10 121.4(5) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C13 C12 C11 120.2(4) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 120.0(5) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 121.2(5) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C10 119.6(4) . . ? C14 C15 C16 121.0(4) . . ? C10 C15 C16 119.4(4) . . ? C3 C16 C17 119.8(3) . . ? C3 C16 C15 120.1(4) . . ? C17 C16 C15 120.0(4) . . ? C18 C17 C16 118.1(4) . . ? C18 C17 H17 121.0 . . ? C16 C17 H17 121.0 . . ? C17 C18 C1 121.7(4) . . ? C17 C18 O2 126.2(4) . . ? C1 C18 O2 112.1(3) . . ? C20 C19 C36 122.1(4) . . ? C20 C19 O3 125.9(4) . . ? C36 C19 O3 112.1(3) . . ? C19 C20 C21 117.7(4) . . ? C19 C20 H20 121.1 . . ? C21 C20 H20 121.1 . . ? C34 C21 C20 119.7(4) . . ? C34 C21 C22 120.4(3) . . ? C20 C21 C22 119.9(4) . . ? C23 C22 C27 119.0(4) . . ? C23 C22 C21 121.4(4) . . ? C27 C22 C21 119.6(4) . . ? C24 C23 C22 121.7(4) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 119.3(4) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C26 C25 C24 120.6(4) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 121.7(4) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C22 C27 C26 117.7(4) . . ? C22 C27 C28 120.3(4) . . ? C26 C27 C28 122.0(4) . . ? C33 C28 C29 118.3(4) . . ? C33 C28 C27 119.9(4) . . ? C29 C28 C27 121.7(4) . . ? C30 C29 C28 121.9(4) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C31 C30 C29 119.7(4) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 120.1(5) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 121.6(4) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C28 C33 C32 118.3(4) . . ? C28 C33 C34 120.4(4) . . ? C32 C33 C34 121.3(4) . . ? C35 C34 C21 120.0(3) . . ? C35 C34 C33 120.7(4) . . ? C21 C34 C33 119.3(4) . . ? C36 C35 C34 118.4(4) . . ? C36 C35 H35 120.8 . . ? C34 C35 H35 120.8 . . ? C35 C36 C19 122.0(4) . . ? C35 C36 O4 126.7(4) . . ? C19 C36 O4 111.3(3) . . ? C38 C37 C54 121.7(4) . . ? C38 C37 O5 125.8(4) . . ? C54 C37 O5 112.5(3) . . ? C37 C38 C39 117.8(4) . . ? C37 C38 H38 121.1 . . ? C39 C38 H38 121.1 . . ? C52 C39 C38 120.0(4) . . ? C52 C39 C40 119.7(4) . . ? C38 C39 C40 120.3(4) . . ? C41 C40 C45 118.6(4) . . ? C41 C40 C39 121.6(4) . . ? C45 C40 C39 119.8(4) . . ? C42 C41 C40 121.6(4) . . ? C42 C41 H41 119.2 . . ? C40 C41 H41 119.2 . . ? C43 C42 C41 119.6(5) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C44 C43 C42 120.6(4) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 121.6(5) . . ? C43 C44 H44 119.2 . . ? C45 C44 H44 119.2 . . ? C40 C45 C44 118.0(5) . . ? C40 C45 C46 120.4(4) . . ? C44 C45 C46 121.7(4) . . ? C47 C46 C51 117.2(5) . . ? C47 C46 C45 122.8(4) . . ? C51 C46 C45 120.0(4) . . ? C48 C47 C46 122.9(5) . . ? C48 C47 H47 118.6 . . ? C46 C47 H47 118.6 . . ? C47 C48 C49 120.2(4) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C50 C49 C48 119.1(5) . . ? C50 C49 H49 120.5 . . ? C48 C49 H49 120.5 . . ? C49 C50 C51 121.9(5) . . ? C49 C50 H50 119.1 . . ? C51 C50 H50 119.1 . . ? C50 C51 C46 118.6(4) . . ? C50 C51 C52 122.0(4) . . ? C46 C51 C52 119.4(4) . . ? C39 C52 C53 119.6(4) . . ? C39 C52 C51 120.5(4) . . ? C53 C52 C51 119.8(4) . . ? C54 C53 C52 118.1(4) . . ? C54 C53 H53 120.9 . . ? C52 C53 H53 120.9 . . ? C53 C54 C37 122.6(4) . . ? C53 C54 O6 125.2(4) . . ? C37 C54 O6 112.2(3) . . ? C60 C55 C56 118.4(5) . . ? C60 C55 H55 120.8 . . ? C56 C55 H55 120.8 . . ? C57 C56 C55 121.4(6) . . ? C57 C56 Cl1 119.9(4) . . ? C55 C56 Cl1 118.7(4) . . ? C57 C56 H56 119.3 . . ? C55 C56 H56 119.3 . . ? Cl1 C56 H56 1.5 . . ? C56 C57 C58 120.5(5) . . ? C56 C57 Cl5 130.5(6) . . ? C58 C57 Cl5 108.8(5) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? Cl5 C57 H57 11.9 . . ? C57 C58 C59 119.8(5) . . ? C57 C58 Cl4 120.5(5) . . ? C59 C58 Cl4 119.1(5) . . ? C57 C58 H58 120.1 . . ? C59 C58 H58 120.1 . . ? Cl4 C58 H58 7.9 . . ? C60 C59 C58 118.1(6) . . ? C60 C59 Cl2 122.6(5) . . ? C58 C59 Cl2 119.2(5) . . ? C60 C59 H59 120.9 . . ? C58 C59 H59 120.9 . . ? Cl2 C59 H59 1.7 . . ? C55 C60 C59 121.8(6) . . ? C55 C60 Cl3 118.8(5) . . ? C59 C60 Cl3 119.4(5) . . ? C57 Cl5 Cl7 141.6(4) . . ? C61 Cl7 Cl5 142.8(3) . . ? C62 C61 C63 119.5(5) 2_655 . ? C62 C61 Cl7 120.2(4) 2_655 . ? C63 C61 Cl7 120.4(4) . . ? C61 C62 C63 119.6(5) 2_655 . ? C61 C62 H62 120.2 2_655 . ? C63 C62 H62 120.2 . . ? C62 C63 C61 120.9(5) . . ? C62 C63 Cl6 120.0(4) . . ? C61 C63 Cl6 119.1(4) . . ? C65 C64 C66 120.1(6) 2_676 . ? C65 C64 H64 120.0 2_676 . ? C66 C64 H64 120.0 . . ? C64 C65 C66 120.8(5) 2_676 . ? C64 C65 Cl9 120.3(5) 2_676 . ? C66 C65 Cl9 118.9(5) . . ? C64 C66 C65 119.2(6) . . ? C64 C66 Cl8 120.6(6) . . ? C65 C66 Cl8 120.2(5) . . ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 30.77 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 1.086 _refine_diff_density_min -1.303 _refine_diff_density_rms 0.086 # Attachment 'mrm26b.cif' data_MRM26b _database_code_depnum_ccdc_archive 'CCDC 812015' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H30 N3 O6 P3' _chemical_formula_weight 909.72 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.909(2) _cell_length_b 31.013(4) _cell_length_c 9.0740(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.120(7) _cell_angle_gamma 90.00 _cell_volume 4102.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 33.53 _exptl_crystal_description needle _exptl_crystal_colour none _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.005 _exptl_crystal_size_min 0.004 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.87260 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'ESRF synchrotron' _diffrn_source_type 'ID23-2 gemini-microfocus' _diffrn_radiation_monochromator Si111 _diffrn_measurement_device_type 'ESRF-EMBL MD2M diffractometer' _diffrn_measurement_method oscillation _diffrn_detector_area_resol_mean ? _diffrn_detector_type 'marMOSAIC 225' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35280 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 33.53 _reflns_number_total 7523 _reflns_number_gt 6340 _reflns_threshold_expression >2sigma(I) _computing_data_collection mxCuBE _computing_cell_refinement 'XDS (Kabsch, 2010)' _computing_data_reduction 'XDS (Kabsch, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer, WinGX' _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^)+(0.0577P)^2^+2.1495P] 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 7523 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1081 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 P1 P 0.47486(3) 0.164593(15) 0.07654(5) 0.01718(13) Uani 1 1 d . . . P3 P 0.43481(3) 0.248216(15) -0.02427(5) 0.01578(13) Uani 1 1 d . . . P2 P 0.59260(3) 0.208383(16) -0.06830(6) 0.01770(13) Uani 1 1 d . . . O6 O 0.35619(9) 0.26118(4) -0.16940(14) 0.0187(3) Uani 1 1 d . . . O4 O 0.70002(9) 0.21995(4) -0.01668(15) 0.0204(3) Uani 1 1 d . . . O7 O 0.41839(8) 0.28844(4) 0.08098(14) 0.0181(3) Uani 1 1 d . . . O5 O 0.59448(8) 0.19419(5) -0.23928(15) 0.0224(3) Uani 1 1 d . . . O1 O 0.41779(9) 0.12188(4) 0.00982(14) 0.0208(3) Uani 1 1 d . . . O2 O 0.49547(9) 0.15044(4) 0.25242(15) 0.0207(3) Uani 1 1 d . . . N2 N 0.56828(11) 0.16771(5) 0.02184(19) 0.0218(4) Uani 1 1 d . . . C27 C 0.99954(13) 0.18880(6) -0.3872(2) 0.0194(4) Uani 1 1 d . . . C36 C 0.68378(12) 0.19594(6) -0.2617(2) 0.0179(4) Uani 1 1 d . . . C4 C 0.30675(13) -0.00695(6) 0.2415(2) 0.0186(4) Uani 1 1 d . . . N3 N 0.53263(11) 0.25033(5) -0.06610(19) 0.0199(4) Uani 1 1 d . . . C15 C 0.40214(12) 0.02559(6) 0.5297(2) 0.0181(4) Uani 1 1 d . . . C53 C 0.31523(12) 0.35134(6) 0.0559(2) 0.0176(4) Uani 1 1 d . . . H53 H 0.3368 0.3605 0.1570 0.021 Uiso 1 1 calc R . . C3 C 0.35726(12) 0.03389(6) 0.2497(2) 0.0161(4) Uani 1 1 d . . . C33 C 0.83954(13) 0.17344(6) -0.5243(2) 0.0181(4) Uani 1 1 d . . . C22 C 0.96696(12) 0.20578(6) -0.2636(2) 0.0180(4) Uani 1 1 d . . . C5 C 0.26060(14) -0.02405(6) 0.1020(2) 0.0239(4) Uani 1 1 d . . . H5 H 0.2637 -0.0091 0.0119 0.029 Uiso 1 1 calc R . . C38 C 0.25372(12) 0.32283(6) -0.2452(2) 0.0188(4) Uani 1 1 d . . . H38 H 0.2339 0.3128 -0.3457 0.023 Uiso 1 1 calc R . . C9 C 0.30352(13) -0.02998(6) 0.3746(2) 0.0212(4) Uani 1 1 d . . . C16 C 0.40442(12) 0.04985(6) 0.3913(2) 0.0159(4) Uani 1 1 d . . . C23 C 1.02978(13) 0.22511(6) -0.1445(2) 0.0221(4) Uani 1 1 d . . . H23 H 1.0080 0.2372 -0.0623 0.027 Uiso 1 1 calc R . . C37 C 0.31620(12) 0.30026(6) -0.1436(2) 0.0161(4) Uani 1 1 d . . . C50 C 0.21950(13) 0.42398(7) 0.1620(3) 0.0279(5) Uani 1 1 d . . . H50 H 0.2569 0.4057 0.2338 0.033 Uiso 1 1 calc R . . C13 C 0.44626(14) 0.01779(7) 0.8020(2) 0.0265(5) Uani 1 1 d . . . H13 H 0.4781 0.0284 0.8969 0.032 Uiso 1 1 calc R . . C54 C 0.34921(12) 0.31500(6) 0.0025(2) 0.0163(4) Uani 1 1 d . . . C2 C 0.35918(12) 0.05737(6) 0.1161(2) 0.0169(4) Uani 1 1 d . . . H2 H 0.3279 0.0470 0.0206 0.020 Uiso 1 1 calc R . . C39 C 0.21892(12) 0.36181(6) -0.1969(2) 0.0180(4) Uani 1 1 d . . . C10 C 0.35199(13) -0.01355(6) 0.5209(2) 0.0197(4) Uani 1 1 d . . . C21 C 0.86837(12) 0.20296(6) -0.2623(2) 0.0165(4) Uani 1 1 d . . . C1 C 0.40694(12) 0.09509(6) 0.1283(2) 0.0165(4) Uani 1 1 d . . . C28 C 0.93543(13) 0.17242(6) -0.5202(2) 0.0202(4) Uani 1 1 d . . . C34 C 0.80601(12) 0.18732(6) -0.3916(2) 0.0164(4) Uani 1 1 d . . . C35 C 0.71133(12) 0.18407(6) -0.3901(2) 0.0179(4) Uani 1 1 d . . . H35 H 0.6684 0.1740 -0.4757 0.021 Uiso 1 1 calc R . . C20 C 0.83637(12) 0.21465(6) -0.1306(2) 0.0180(4) Uani 1 1 d . . . H20 H 0.8774 0.2248 -0.0429 0.022 Uiso 1 1 calc R . . C17 C 0.45348(12) 0.08941(6) 0.3983(2) 0.0169(4) Uani 1 1 d . . . H17 H 0.4861 0.1005 0.4919 0.020 Uiso 1 1 calc R . . C51 C 0.20409(12) 0.41324(6) 0.0083(2) 0.0223(4) Uani 1 1 d . . . C12 C 0.39727(14) -0.02070(7) 0.7937(2) 0.0274(5) Uani 1 1 d . . . H12 H 0.3956 -0.0364 0.8830 0.033 Uiso 1 1 calc R . . C14 C 0.44848(13) 0.04044(7) 0.6723(2) 0.0214(4) Uani 1 1 d . . . H14 H 0.4820 0.0667 0.6791 0.026 Uiso 1 1 calc R . . C18 C 0.45247(12) 0.11105(6) 0.2673(2) 0.0165(4) Uani 1 1 d . . . C32 C 0.77872(13) 0.16039(6) -0.6589(2) 0.0222(4) Uani 1 1 d . . . H32 H 0.7145 0.1616 -0.6641 0.027 Uiso 1 1 calc R . . C6 C 0.21111(15) -0.06191(7) 0.0927(3) 0.0297(5) Uani 1 1 d . . . H6 H 0.1801 -0.0726 -0.0025 0.036 Uiso 1 1 calc R . . C31 C 0.81042(14) 0.14606(7) -0.7824(2) 0.0266(5) Uani 1 1 d . . . H31 H 0.7683 0.1373 -0.8710 0.032 Uiso 1 1 calc R . . C26 C 1.09560(13) 0.18973(7) -0.3805(2) 0.0238(4) Uani 1 1 d . . . H26 H 1.1190 0.1772 -0.4603 0.029 Uiso 1 1 calc R . . N1 N 0.40778(10) 0.20459(5) 0.04482(18) 0.0195(4) Uani 1 1 d . . . C40 C 0.15443(12) 0.38836(6) -0.3048(2) 0.0218(4) Uani 1 1 d . . . C25 C 1.15541(13) 0.20823(7) -0.2621(2) 0.0272(5) Uani 1 1 d . . . H25 H 1.2193 0.2083 -0.2604 0.033 Uiso 1 1 calc R . . C19 C 0.74483(12) 0.21078(6) -0.1344(2) 0.0167(4) Uani 1 1 d . . . C44 C 0.05550(15) 0.45070(7) -0.3625(3) 0.0370(6) Uani 1 1 d . . . H44 H 0.0304 0.4764 -0.3312 0.044 Uiso 1 1 calc R . . C8 C 0.25205(16) -0.06870(7) 0.3613(3) 0.0308(5) Uani 1 1 d . . . H8 H 0.2486 -0.0844 0.4499 0.037 Uiso 1 1 calc R . . C11 C 0.35152(14) -0.03599(7) 0.6568(2) 0.0246(5) Uani 1 1 d . . . H11 H 0.3186 -0.0623 0.6528 0.030 Uiso 1 1 calc R . . C45 C 0.11891(13) 0.42670(6) -0.2554(3) 0.0258(5) Uani 1 1 d . . . C41 C 0.12745(15) 0.37651(7) -0.4574(2) 0.0294(5) Uani 1 1 d . . . H41 H 0.1524 0.3511 -0.4914 0.035 Uiso 1 1 calc R . . C24 C 1.12246(13) 0.22693(7) -0.1441(2) 0.0256(4) Uani 1 1 d . . . H24 H 1.1635 0.2409 -0.0640 0.031 Uiso 1 1 calc R . . C52 C 0.24645(12) 0.37503(6) -0.0446(2) 0.0182(4) Uani 1 1 d . . . C29 C 0.96548(14) 0.15743(7) -0.6486(2) 0.0282(5) Uani 1 1 d . . . H29 H 1.0294 0.1563 -0.6464 0.034 Uiso 1 1 calc R . . C30 C 0.90498(15) 0.14439(7) -0.7769(3) 0.0305(5) Uani 1 1 d . . . H30 H 0.9272 0.1343 -0.8614 0.037 Uiso 1 1 calc R . . C46 C 0.14457(13) 0.43953(6) -0.0974(3) 0.0264(5) Uani 1 1 d . . . C49 C 0.18146(14) 0.46042(7) 0.2108(3) 0.0351(6) Uani 1 1 d . . . H49 H 0.1916 0.4667 0.3155 0.042 Uiso 1 1 calc R . . C47 C 0.11004(14) 0.47768(7) -0.0435(3) 0.0350(6) Uani 1 1 d . . . H47 H 0.0733 0.4966 -0.1133 0.042 Uiso 1 1 calc R . . C42 C 0.06585(16) 0.40069(8) -0.5590(3) 0.0373(6) Uani 1 1 d . . . H42 H 0.0486 0.3920 -0.6614 0.045 Uiso 1 1 calc R . . C7 C 0.20706(16) -0.08418(7) 0.2240(3) 0.0350(5) Uani 1 1 d . . . H7 H 0.1730 -0.1102 0.2186 0.042 Uiso 1 1 calc R . . C48 C 0.12843(15) 0.48790(7) 0.1071(3) 0.0396(6) Uani 1 1 d . . . H48 H 0.1048 0.5138 0.1403 0.048 Uiso 1 1 calc R . . C43 C 0.02922(16) 0.43792(8) -0.5098(3) 0.0400(6) Uani 1 1 d . . . H43 H -0.0141 0.4545 -0.5785 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0188(2) 0.0139(2) 0.0205(3) 0.0011(2) 0.0078(2) -0.00044(19) P3 0.0133(2) 0.0144(2) 0.0214(3) 0.0010(2) 0.0077(2) 0.00055(18) P2 0.0137(2) 0.0179(3) 0.0235(3) 0.0011(2) 0.0085(2) 0.00123(19) O6 0.0203(6) 0.0156(6) 0.0219(7) -0.0022(6) 0.0081(6) 0.0025(5) O4 0.0170(6) 0.0239(7) 0.0224(7) -0.0027(6) 0.0094(6) 0.0012(6) O7 0.0138(6) 0.0197(7) 0.0211(7) 0.0021(6) 0.0045(5) 0.0018(5) O5 0.0116(6) 0.0309(8) 0.0256(7) -0.0012(6) 0.0059(5) -0.0001(6) O1 0.0284(7) 0.0185(7) 0.0166(7) 0.0032(6) 0.0072(6) -0.0032(6) O2 0.0234(7) 0.0151(7) 0.0238(7) -0.0017(6) 0.0056(6) -0.0037(6) N2 0.0218(8) 0.0165(8) 0.0294(9) 0.0028(7) 0.0105(7) 0.0052(7) C27 0.0180(9) 0.0139(9) 0.0281(10) 0.0014(8) 0.0087(8) 0.0033(8) C36 0.0131(8) 0.0164(9) 0.0260(10) 0.0033(8) 0.0078(8) 0.0023(7) C4 0.0187(9) 0.0147(9) 0.0240(10) 0.0004(8) 0.0082(8) 0.0042(7) N3 0.0187(8) 0.0164(8) 0.0273(9) 0.0037(7) 0.0108(7) -0.0009(6) C15 0.0162(9) 0.0201(10) 0.0200(10) 0.0033(8) 0.0085(8) 0.0094(8) C53 0.0161(9) 0.0163(9) 0.0228(10) -0.0009(8) 0.0095(8) -0.0037(7) C3 0.0163(9) 0.0144(9) 0.0194(9) 0.0014(8) 0.0079(8) 0.0051(7) C33 0.0198(9) 0.0105(8) 0.0251(10) 0.0019(8) 0.0070(8) 0.0029(7) C22 0.0161(9) 0.0122(9) 0.0270(10) 0.0032(8) 0.0071(8) 0.0022(7) C5 0.0300(11) 0.0172(10) 0.0249(10) 0.0020(9) 0.0067(9) 0.0004(8) C38 0.0160(9) 0.0209(10) 0.0213(10) 0.0018(8) 0.0083(8) -0.0015(8) C9 0.0225(10) 0.0161(9) 0.0268(11) 0.0048(8) 0.0094(8) 0.0053(8) C16 0.0148(8) 0.0159(9) 0.0191(9) 0.0024(8) 0.0084(7) 0.0074(7) C23 0.0196(9) 0.0215(10) 0.0271(11) -0.0013(9) 0.0088(8) -0.0008(8) C37 0.0137(8) 0.0141(9) 0.0235(9) -0.0001(8) 0.0105(8) 0.0000(7) C50 0.0169(9) 0.0258(11) 0.0430(13) -0.0100(10) 0.0109(9) -0.0039(8) C13 0.0219(10) 0.0390(12) 0.0197(10) 0.0045(9) 0.0064(8) 0.0091(9) C54 0.0128(8) 0.0157(9) 0.0222(9) 0.0028(8) 0.0074(7) -0.0023(7) C2 0.0192(9) 0.0151(9) 0.0168(9) -0.0019(8) 0.0047(7) 0.0020(7) C39 0.0120(8) 0.0170(9) 0.0270(10) 0.0029(8) 0.0085(8) -0.0030(7) C10 0.0194(9) 0.0195(9) 0.0222(10) 0.0048(8) 0.0088(8) 0.0084(8) C21 0.0165(9) 0.0110(8) 0.0235(10) 0.0030(8) 0.0077(8) 0.0022(7) C1 0.0196(9) 0.0155(9) 0.0161(9) 0.0020(8) 0.0078(7) 0.0042(8) C28 0.0191(9) 0.0135(9) 0.0303(11) -0.0009(8) 0.0102(8) 0.0031(8) C34 0.0167(9) 0.0106(9) 0.0227(10) 0.0033(8) 0.0062(8) 0.0035(7) C35 0.0161(9) 0.0152(9) 0.0221(10) 0.0018(8) 0.0034(8) 0.0019(7) C20 0.0162(9) 0.0141(9) 0.0244(10) 0.0000(8) 0.0056(8) 0.0013(7) C17 0.0159(8) 0.0178(9) 0.0179(9) -0.0014(8) 0.0054(7) 0.0056(7) C51 0.0151(9) 0.0154(9) 0.0396(12) -0.0023(9) 0.0128(9) -0.0052(8) C12 0.0252(10) 0.0376(12) 0.0221(10) 0.0129(10) 0.0114(9) 0.0117(9) C14 0.0183(9) 0.0262(11) 0.0208(10) 0.0031(9) 0.0066(8) 0.0063(8) C18 0.0176(9) 0.0124(9) 0.0206(9) -0.0011(8) 0.0067(8) 0.0017(7) C32 0.0193(9) 0.0211(10) 0.0272(11) 0.0007(9) 0.0069(8) 0.0022(8) C6 0.0368(12) 0.0189(10) 0.0310(12) -0.0032(9) 0.0018(10) -0.0033(9) C31 0.0286(11) 0.0243(11) 0.0269(11) -0.0035(9) 0.0060(9) 0.0017(9) C26 0.0179(9) 0.0249(10) 0.0314(11) -0.0019(9) 0.0116(9) 0.0026(8) N1 0.0156(7) 0.0191(8) 0.0270(9) 0.0004(7) 0.0116(7) -0.0018(6) C40 0.0158(9) 0.0175(9) 0.0336(11) 0.0064(9) 0.0087(8) -0.0023(8) C25 0.0145(9) 0.0299(11) 0.0388(12) 0.0004(10) 0.0097(9) 0.0016(8) C19 0.0178(9) 0.0135(9) 0.0207(9) 0.0010(8) 0.0085(8) 0.0034(7) C44 0.0298(12) 0.0237(11) 0.0586(16) 0.0156(11) 0.0115(11) 0.0065(10) C8 0.0395(12) 0.0200(10) 0.0331(12) 0.0090(10) 0.0085(10) -0.0031(9) C11 0.0220(10) 0.0257(11) 0.0285(11) 0.0108(9) 0.0105(9) 0.0063(8) C45 0.0169(9) 0.0180(10) 0.0446(13) 0.0065(10) 0.0116(9) -0.0017(8) C41 0.0290(11) 0.0262(11) 0.0326(12) 0.0066(10) 0.0058(9) 0.0004(9) C24 0.0176(9) 0.0274(11) 0.0318(11) -0.0021(9) 0.0054(9) -0.0032(8) C52 0.0122(8) 0.0150(9) 0.0302(10) 0.0017(8) 0.0111(8) -0.0037(7) C29 0.0218(10) 0.0302(11) 0.0352(12) -0.0092(10) 0.0123(9) 0.0015(9) C30 0.0297(11) 0.0329(12) 0.0322(12) -0.0083(10) 0.0143(9) 0.0031(10) C46 0.0152(9) 0.0174(10) 0.0494(14) 0.0019(10) 0.0132(9) -0.0031(8) C49 0.0214(10) 0.0322(12) 0.0532(15) -0.0197(12) 0.0111(10) -0.0042(9) C47 0.0199(10) 0.0204(11) 0.0659(17) -0.0032(11) 0.0114(11) 0.0018(9) C42 0.0358(12) 0.0372(13) 0.0365(13) 0.0147(11) 0.0022(10) 0.0008(11) C7 0.0429(13) 0.0176(10) 0.0433(14) 0.0042(10) 0.0062(11) -0.0089(10) C48 0.0225(11) 0.0234(11) 0.0748(19) -0.0185(12) 0.0147(12) -0.0001(9) C43 0.0344(12) 0.0330(13) 0.0505(16) 0.0229(12) 0.0042(11) 0.0053(10) _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 P1 N2 1.5768(16) . ? P1 N1 1.5814(16) . ? P1 O2 1.6212(14) . ? P1 O1 1.6213(14) . ? P3 N1 1.5786(16) . ? P3 N3 1.5835(15) . ? P3 O6 1.6192(14) . ? P3 O7 1.6205(13) . ? P2 N3 1.5811(16) . ? P2 N2 1.5863(17) . ? P2 O4 1.6118(14) . ? P2 O5 1.6185(14) . ? O6 C37 1.392(2) . ? O4 C19 1.403(2) . ? O7 C54 1.393(2) . ? O5 C36 1.390(2) . ? O1 C1 1.395(2) . ? O2 C18 1.399(2) . ? C27 C22 1.414(3) . ? C27 C26 1.421(3) . ? C27 C28 1.465(3) . ? C36 C35 1.364(3) . ? C36 C19 1.390(3) . ? C4 C5 1.411(3) . ? C4 C9 1.413(3) . ? C4 C3 1.467(3) . ? C15 C14 1.410(3) . ? C15 C10 1.419(3) . ? C15 C16 1.470(3) . ? C53 C54 1.366(3) . ? C53 C52 1.425(3) . ? C53 H53 0.9500 . ? C3 C16 1.418(3) . ? C3 C2 1.419(3) . ? C33 C32 1.419(3) . ? C33 C28 1.423(3) . ? C33 C34 1.462(3) . ? C22 C23 1.407(3) . ? C22 C21 1.475(2) . ? C5 C6 1.380(3) . ? C5 H5 0.9500 . ? C38 C37 1.359(3) . ? C38 C39 1.421(3) . ? C38 H38 0.9500 . ? C9 C8 1.417(3) . ? C9 C10 1.463(3) . ? C16 C17 1.423(3) . ? C23 C24 1.382(3) . ? C23 H23 0.9500 . ? C37 C54 1.391(3) . ? C50 C49 1.379(3) . ? C50 C51 1.406(3) . ? C50 H50 0.9500 . ? C13 C14 1.377(3) . ? C13 C12 1.393(3) . ? C13 H13 0.9500 . ? C2 C1 1.362(3) . ? C2 H2 0.9500 . ? C39 C52 1.417(3) . ? C39 C40 1.472(3) . ? C10 C11 1.417(3) . ? C21 C34 1.420(3) . ? C21 C20 1.424(3) . ? C1 C18 1.391(3) . ? C28 C29 1.412(3) . ? C34 C35 1.418(2) . ? C35 H35 0.9500 . ? C20 C19 1.363(3) . ? C20 H20 0.9500 . ? C17 C18 1.362(3) . ? C17 H17 0.9500 . ? C51 C46 1.419(3) . ? C51 C52 1.470(3) . ? C12 C11 1.370(3) . ? C12 H12 0.9500 . ? C14 H14 0.9500 . ? C32 C31 1.378(3) . ? C32 H32 0.9500 . ? C6 C7 1.389(3) . ? C6 H6 0.9500 . ? C31 C30 1.401(3) . ? C31 H31 0.9500 . ? C26 C25 1.370(3) . ? C26 H26 0.9500 . ? C40 C41 1.407(3) . ? C40 C45 1.412(3) . ? C25 C24 1.394(3) . ? C25 H25 0.9500 . ? C44 C43 1.370(4) . ? C44 C45 1.416(3) . ? C44 H44 0.9500 . ? C8 C7 1.372(3) . ? C8 H8 0.9500 . ? C11 H11 0.9500 . ? C45 C46 1.460(3) . ? C41 C42 1.378(3) . ? C41 H41 0.9500 . ? C24 H24 0.9500 . ? C29 C30 1.375(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C46 C47 1.417(3) . ? C49 C48 1.387(4) . ? C49 H49 0.9500 . ? C47 C48 1.374(4) . ? C47 H47 0.9500 . ? C42 C43 1.390(4) . ? C42 H42 0.9500 . ? C7 H7 0.9500 . ? C48 H48 0.9500 . ? C43 H43 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 N2 P1 N1 117.48(8) . . ? N2 P1 O2 109.21(8) . . ? N1 P1 O2 111.93(8) . . ? N2 P1 O1 111.19(8) . . ? N1 P1 O1 108.10(8) . . ? O2 P1 O1 97.04(7) . . ? N1 P3 N3 117.09(8) . . ? N1 P3 O6 109.53(8) . . ? N3 P3 O6 109.92(8) . . ? N1 P3 O7 110.05(8) . . ? N3 P3 O7 111.72(8) . . ? O6 P3 O7 96.61(7) . . ? N3 P2 N2 117.18(8) . . ? N3 P2 O4 110.08(8) . . ? N2 P2 O4 110.35(8) . . ? N3 P2 O5 111.07(8) . . ? N2 P2 O5 109.26(8) . . ? O4 P2 O5 97.06(7) . . ? C37 O6 P3 109.99(11) . . ? C19 O4 P2 109.67(11) . . ? C54 O7 P3 109.94(11) . . ? C36 O5 P2 109.87(12) . . ? C1 O1 P1 109.60(11) . . ? C18 O2 P1 109.58(11) . . ? P1 N2 P2 121.57(10) . . ? C22 C27 C26 118.03(18) . . ? C22 C27 C28 120.63(16) . . ? C26 C27 C28 121.29(17) . . ? C35 C36 O5 125.74(17) . . ? C35 C36 C19 122.45(17) . . ? O5 C36 C19 111.80(16) . . ? C5 C4 C9 118.64(18) . . ? C5 C4 C3 121.23(17) . . ? C9 C4 C3 120.13(18) . . ? P2 N3 P3 121.38(10) . . ? C14 C15 C10 118.77(17) . . ? C14 C15 C16 121.48(18) . . ? C10 C15 C16 119.75(17) . . ? C54 C53 C52 117.96(18) . . ? C54 C53 H53 121.0 . . ? C52 C53 H53 121.0 . . ? C16 C3 C2 119.97(16) . . ? C16 C3 C4 119.93(16) . . ? C2 C3 C4 120.10(17) . . ? C32 C33 C28 118.21(17) . . ? C32 C33 C34 121.73(17) . . ? C28 C33 C34 120.06(17) . . ? C23 C22 C27 118.95(16) . . ? C23 C22 C21 121.50(17) . . ? C27 C22 C21 119.55(17) . . ? C6 C5 C4 121.90(19) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C37 C38 C39 118.13(18) . . ? C37 C38 H38 120.9 . . ? C39 C38 H38 120.9 . . ? C4 C9 C8 118.09(19) . . ? C4 C9 C10 120.05(17) . . ? C8 C9 C10 121.86(18) . . ? C3 C16 C17 119.58(16) . . ? C3 C16 C15 119.96(17) . . ? C17 C16 C15 120.46(17) . . ? C24 C23 C22 121.50(18) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C38 C37 C54 122.16(17) . . ? C38 C37 O6 126.23(17) . . ? C54 C37 O6 111.61(16) . . ? C49 C50 C51 121.4(2) . . ? C49 C50 H50 119.3 . . ? C51 C50 H50 119.3 . . ? C14 C13 C12 119.8(2) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C53 C54 C37 121.76(17) . . ? C53 C54 O7 126.60(17) . . ? C37 C54 O7 111.64(15) . . ? C1 C2 C3 118.37(17) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C52 C39 C38 119.83(17) . . ? C52 C39 C40 120.13(17) . . ? C38 C39 C40 120.04(18) . . ? C11 C10 C15 118.06(18) . . ? C11 C10 C9 121.77(18) . . ? C15 C10 C9 120.17(17) . . ? C34 C21 C20 120.23(16) . . ? C34 C21 C22 119.63(16) . . ? C20 C21 C22 120.11(17) . . ? C2 C1 C18 121.78(17) . . ? C2 C1 O1 126.31(17) . . ? C18 C1 O1 111.90(16) . . ? C29 C28 C33 118.52(18) . . ? C29 C28 C27 121.95(17) . . ? C33 C28 C27 119.45(17) . . ? C35 C34 C21 119.79(16) . . ? C35 C34 C33 120.01(17) . . ? C21 C34 C33 120.18(16) . . ? C36 C35 C34 117.89(18) . . ? C36 C35 H35 121.1 . . ? C34 C35 H35 121.1 . . ? C19 C20 C21 117.78(18) . . ? C19 C20 H20 121.1 . . ? C21 C20 H20 121.1 . . ? C18 C17 C16 118.33(17) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C50 C51 C46 118.88(18) . . ? C50 C51 C52 121.54(19) . . ? C46 C51 C52 119.57(19) . . ? C11 C12 C13 120.08(19) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C13 C14 C15 121.5(2) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C17 C18 C1 121.94(17) . . ? C17 C18 O2 126.36(17) . . ? C1 C18 O2 111.69(16) . . ? C31 C32 C33 121.73(18) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C5 C6 C7 119.3(2) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C32 C31 C30 119.8(2) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C25 C26 C27 121.73(18) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? P3 N1 P1 122.69(9) . . ? C41 C40 C45 118.92(19) . . ? C41 C40 C39 121.36(18) . . ? C45 C40 C39 119.72(19) . . ? C26 C25 C24 120.02(18) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C20 C19 C36 121.85(17) . . ? C20 C19 O4 126.65(17) . . ? C36 C19 O4 111.50(15) . . ? C43 C44 C45 122.0(2) . . ? C43 C44 H44 119.0 . . ? C45 C44 H44 119.0 . . ? C7 C8 C9 121.78(19) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C12 C11 C10 121.75(19) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C40 C45 C44 117.7(2) . . ? C40 C45 C46 120.20(19) . . ? C44 C45 C46 122.0(2) . . ? C42 C41 C40 121.9(2) . . ? C42 C41 H41 119.1 . . ? C40 C41 H41 119.1 . . ? C23 C24 C25 119.64(19) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C39 C52 C53 119.82(17) . . ? C39 C52 C51 119.68(17) . . ? C53 C52 C51 120.50(18) . . ? C30 C29 C28 121.98(18) . . ? C30 C29 H29 119.0 . . ? C28 C29 H29 119.0 . . ? C29 C30 C31 119.71(19) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C47 C46 C51 117.9(2) . . ? C47 C46 C45 121.8(2) . . ? C51 C46 C45 120.30(18) . . ? C50 C49 C48 120.0(2) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C48 C47 C46 121.7(2) . . ? C48 C47 H47 119.2 . . ? C46 C47 H47 119.2 . . ? C41 C42 C43 119.3(2) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C8 C7 C6 120.3(2) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C47 C48 C49 119.9(2) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C44 C43 C42 120.1(2) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? _diffrn_measured_fraction_theta_max 0.864 _diffrn_reflns_theta_full 33.53 _diffrn_measured_fraction_theta_full 0.864 _refine_diff_density_max 0.429 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.056