Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name D.S.Wright 'Fay Dodds' 'Felipe Garcia' 'Richard A. Kowenicki' 'Mary McPartlin' 'Lucia Riera' 'Alexander Steiner' _publ_contact_author_name 'D. S. Wright' _publ_contact_author_address ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UNITED KINGDOM ; _publ_contact_author_email DSW1000@CAM.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; The Folded Phosph(III)azane Macrocycle [{P(mu-NtBu)}2{1,4-(NH)2C6H4}]4 ; data_dw0512 _database_code_depnum_ccdc_archive 'CCDC 279778' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H96 N16 P8, 1.5(C5 H12)' _chemical_formula_sum 'C63.50 H114 N16 P8' _chemical_formula_weight 1349.47 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' 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 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 36.887(7) _cell_length_b 22.223(4) _cell_length_c 25.007(5) _cell_angle_alpha 90.00 _cell_angle_beta 129.86(3) _cell_angle_gamma 90.00 _cell_volume 15734(5) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 43429 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5816 _exptl_absorpt_coefficient_mu 0.223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.921 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 63538 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13817 _reflns_number_gt 10065 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+37.6143P] 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 13817 _refine_ls_number_parameters 832 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1335 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.223 _refine_ls_shift/su_mean 0.002 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 0.37358(3) 0.37090(4) 0.86503(5) 0.0435(2) Uani 1 1 d . A . N1 N 0.38379(9) 0.34995(11) 0.80969(14) 0.0393(6) Uani 1 1 d . A . C1 C 0.39935(13) 0.38980(16) 0.7807(2) 0.0511(9) Uani 1 1 d . . . C11 C 0.4494(2) 0.4118(3) 0.8395(3) 0.0831(17) Uiso 0.800(4) 1 d P A 1 H11A H 0.4706 0.3771 0.8632 0.125 Uiso 0.800(4) 1 calc PR A 1 H11B H 0.4496 0.4352 0.8729 0.125 Uiso 0.800(4) 1 calc PR A 1 H11C H 0.4603 0.4372 0.8202 0.125 Uiso 0.800(4) 1 calc PR A 1 C12 C 0.4015(2) 0.3537(3) 0.7309(3) 0.0754(16) Uiso 0.800(4) 1 d P A 1 H12A H 0.4135 0.3793 0.7134 0.113 Uiso 0.800(4) 1 calc PR A 1 H12B H 0.3698 0.3394 0.6917 0.113 Uiso 0.800(4) 1 calc PR A 1 H12C H 0.4226 0.3192 0.7556 0.113 Uiso 0.800(4) 1 calc PR A 1 C13 C 0.3652(2) 0.4410(3) 0.7431(4) 0.0862(18) Uiso 0.800(4) 1 d P A 1 H13A H 0.3647 0.4641 0.7760 0.129 Uiso 0.800(4) 1 calc PR A 1 H13B H 0.3335 0.4251 0.7059 0.129 Uiso 0.800(4) 1 calc PR A 1 H13C H 0.3750 0.4671 0.7228 0.129 Uiso 0.800(4) 1 calc PR A 1 C11' C 0.4008(9) 0.4555(11) 0.8027(14) 0.0831(17) Uiso 0.200(4) 1 d P A 2 H11D H 0.4279 0.4606 0.8522 0.125 Uiso 0.200(4) 1 calc PR A 2 H11E H 0.3716 0.4645 0.7945 0.125 Uiso 0.200(4) 1 calc PR A 2 H11F H 0.4039 0.4831 0.7751 0.125 Uiso 0.200(4) 1 calc PR A 2 C12' C 0.4390(8) 0.3702(11) 0.7883(13) 0.0754(16) Uiso 0.200(4) 1 d P A 2 H12D H 0.4666 0.3677 0.8380 0.113 Uiso 0.200(4) 1 calc PR A 2 H12E H 0.4454 0.3989 0.7655 0.113 Uiso 0.200(4) 1 calc PR A 2 H12F H 0.4325 0.3304 0.7669 0.113 Uiso 0.200(4) 1 calc PR A 2 C13' C 0.3546(9) 0.3979(12) 0.7015(13) 0.0862(18) Uiso 0.200(4) 1 d P A 2 H13D H 0.3567 0.4365 0.6846 0.129 Uiso 0.200(4) 1 calc PR A 2 H13E H 0.3260 0.3971 0.6965 0.129 Uiso 0.200(4) 1 calc PR A 2 H13F H 0.3534 0.3651 0.6742 0.129 Uiso 0.200(4) 1 calc PR A 2 P2 P 0.39662(3) 0.27540(4) 0.83248(4) 0.0369(2) Uani 1 1 d . . . N2 N 0.37704(9) 0.29395(12) 0.87717(13) 0.0417(6) Uani 1 1 d . A . C2 C 0.39219(12) 0.26451(19) 0.94185(18) 0.0554(10) Uani 1 1 d . . . C21 C 0.35710(17) 0.2833(2) 0.9519(2) 0.0822(14) Uani 1 1 d . A . H21A H 0.3597 0.3267 0.9606 0.123 Uiso 1 1 calc R . . H21B H 0.3642 0.2617 0.9918 0.123 Uiso 1 1 calc R . . H21C H 0.3250 0.2735 0.9099 0.123 Uiso 1 1 calc R . . C22 C 0.44232(14) 0.2836(2) 1.00435(19) 0.0760(13) Uani 1 1 d . A . H22A H 0.4641 0.2728 0.9960 0.114 Uiso 1 1 calc R . . H22B H 0.4518 0.2631 1.0463 0.114 Uiso 1 1 calc R . . H22C H 0.4432 0.3273 1.0108 0.114 Uiso 1 1 calc R . . C23 C 0.39041(15) 0.19640(19) 0.9321(2) 0.0688(12) Uani 1 1 d . A . H23A H 0.3587 0.1846 0.8905 0.103 Uiso 1 1 calc R . . H23B H 0.3980 0.1762 0.9730 0.103 Uiso 1 1 calc R . . H23C H 0.4134 0.1847 0.9265 0.103 Uiso 1 1 calc R . . N9 N 0.35189(9) 0.23690(13) 0.76214(14) 0.0403(7) Uani 1 1 d . A . H9N H 0.3583(12) 0.2117(16) 0.7482(17) 0.041(11) Uiso 1 1 d . . . C14 C 0.30318(10) 0.25411(13) 0.71400(15) 0.0347(7) Uani 1 1 d . . . C15 C 0.28291(11) 0.27456(16) 0.64816(17) 0.0476(8) Uani 1 1 d . A . H15 H 0.3014 0.2758 0.6339 0.057 Uiso 1 1 calc R . . C16 C 0.23650(11) 0.29324(18) 0.60243(18) 0.0515(9) Uani 1 1 d . . . H16 H 0.2234 0.3066 0.5572 0.062 Uiso 1 1 calc R A . C17 C 0.20844(10) 0.29277(14) 0.62188(15) 0.0368(7) Uani 1 1 d . A . C18 C 0.27522(10) 0.25088(14) 0.73228(16) 0.0385(7) Uani 1 1 d . A . H18 H 0.2881 0.2351 0.7766 0.046 Uiso 1 1 calc R . . C19 C 0.22848(10) 0.27020(14) 0.68736(16) 0.0384(7) Uani 1 1 d . . . H19 H 0.2101 0.2679 0.7016 0.046 Uiso 1 1 calc R A . N10 N 0.16170(9) 0.31341(14) 0.57793(14) 0.0448(7) Uani 1 1 d . . . H10N H 0.1471(13) 0.3049(16) 0.5928(18) 0.049(11) Uiso 1 1 d . . . P3 P 0.13244(3) 0.34587(4) 0.49853(4) 0.0426(2) Uani 1 1 d . A . N3 N 0.09016(9) 0.38864(12) 0.49062(13) 0.0412(7) Uani 1 1 d . . . C3 C 0.09325(12) 0.45521(16) 0.49845(18) 0.0505(9) Uani 1 1 d . A . C31 C 0.09383(17) 0.48484(19) 0.4441(2) 0.0718(12) Uani 1 1 d . . . H31A H 0.1211 0.4703 0.4496 0.108 Uiso 1 1 calc R A . H31B H 0.0960 0.5286 0.4504 0.108 Uiso 1 1 calc R . . H31C H 0.0647 0.4747 0.3974 0.108 Uiso 1 1 calc R . . C32 C 0.13875(14) 0.46922(19) 0.5720(2) 0.0690(12) Uani 1 1 d . . . H32A H 0.1384 0.4481 0.6061 0.103 Uiso 1 1 calc R A . H32B H 0.1409 0.5127 0.5803 0.103 Uiso 1 1 calc R . . H32C H 0.1660 0.4559 0.5767 0.103 Uiso 1 1 calc R . . C33 C 0.05109(14) 0.47749(18) 0.4905(2) 0.0627(11) Uani 1 1 d . . . H33A H 0.0219 0.4660 0.4445 0.094 Uiso 1 1 calc R A . H33B H 0.0526 0.5214 0.4951 0.094 Uiso 1 1 calc R . . H33C H 0.0516 0.4594 0.5267 0.094 Uiso 1 1 calc R . . P4 P 0.04124(3) 0.34899(4) 0.42346(4) 0.0421(2) Uani 1 1 d . A . N4 N 0.08427(9) 0.30069(13) 0.44140(13) 0.0429(7) Uani 1 1 d . . . C4 C 0.08040(13) 0.25940(17) 0.39148(18) 0.0531(9) Uani 1 1 d . A . C41 C 0.07978(17) 0.2949(2) 0.3382(2) 0.0759(13) Uani 1 1 d . . . H41A H 0.0526 0.3221 0.3122 0.114 Uiso 1 1 calc R A . H41B H 0.0774 0.2668 0.3058 0.114 Uiso 1 1 calc R . . H41C H 0.1090 0.3183 0.3626 0.114 Uiso 1 1 calc R . . C42 C 0.12292(16) 0.2171(2) 0.4331(2) 0.0787(13) Uani 1 1 d . . . H42A H 0.1521 0.2407 0.4574 0.118 Uiso 1 1 calc R A . H42B H 0.1208 0.1886 0.4014 0.118 Uiso 1 1 calc R . . H42C H 0.1231 0.1951 0.4673 0.118 Uiso 1 1 calc R . . C43 C 0.03467(14) 0.22371(19) 0.3535(2) 0.0674(12) Uani 1 1 d . . . H43A H 0.0350 0.2010 0.3874 0.101 Uiso 1 1 calc R A . H43B H 0.0318 0.1958 0.3206 0.101 Uiso 1 1 calc R . . H43C H 0.0078 0.2514 0.3280 0.101 Uiso 1 1 calc R . . N11 N 0.02091(10) 0.31971(14) 0.46219(15) 0.0475(8) Uani 1 1 d . . . H11N H -0.0031(14) 0.3028(17) 0.438(2) 0.056(12) Uiso 1 1 d . . . C24 C 0.05158(11) 0.29256(16) 0.53026(17) 0.0430(8) Uani 1 1 d . A . C25 C 0.06994(12) 0.32667(16) 0.58865(18) 0.0476(9) Uani 1 1 d . . . H25 H 0.0603 0.3674 0.5833 0.057 Uiso 1 1 calc R A . C26 C 0.10217(12) 0.30287(16) 0.65515(18) 0.0470(8) Uani 1 1 d . A . H26 H 0.1141 0.3274 0.6945 0.056 Uiso 1 1 calc R . . C27 C 0.11714(11) 0.24374(15) 0.66489(16) 0.0396(8) Uani 1 1 d . . . C28 C 0.09903(12) 0.20922(16) 0.60640(17) 0.0486(9) Uani 1 1 d . A . H28 H 0.1091 0.1687 0.6119 0.058 Uiso 1 1 calc R . . C29 C 0.06643(12) 0.23311(16) 0.53990(17) 0.0489(9) Uani 1 1 d . . . H29 H 0.0541 0.2085 0.5005 0.059 Uiso 1 1 calc R A . N12 N 0.15049(10) 0.21952(14) 0.73230(15) 0.0439(7) Uani 1 1 d . A . H12N H 0.1588(12) 0.2431(15) 0.7623(17) 0.038(10) Uiso 1 1 d . . . P5 P 0.14699(3) 0.14751(4) 0.75242(4) 0.0394(2) Uani 1 1 d . . . N5 N 0.12895(9) 0.15470(12) 0.80047(14) 0.0436(7) Uani 1 1 d . A . C5 C 0.07982(12) 0.14991(17) 0.7734(2) 0.0543(10) Uani 1 1 d . . . C51 C 0.06185(17) 0.0860(2) 0.7500(3) 0.0975(18) Uani 1 1 d . A . H51A H 0.0635 0.0743 0.7138 0.146 Uiso 1 1 calc R . . H51B H 0.0290 0.0837 0.7312 0.146 Uiso 1 1 calc R . . H51C H 0.0814 0.0586 0.7898 0.146 Uiso 1 1 calc R . . C52 C 0.04995(16) 0.1936(3) 0.7130(3) 0.114(2) Uani 1 1 d . A . H52A H 0.0611 0.2347 0.7297 0.171 Uiso 1 1 calc R . . H52B H 0.0169 0.1903 0.6929 0.171 Uiso 1 1 calc R . . H52C H 0.0526 0.1839 0.6773 0.171 Uiso 1 1 calc R . . C53 C 0.07902(17) 0.1666(3) 0.8310(3) 0.0970(17) Uani 1 1 d . A . H53A H 0.1003 0.1400 0.8710 0.146 Uiso 1 1 calc R . . H53B H 0.0468 0.1623 0.8145 0.146 Uiso 1 1 calc R . . H53C H 0.0894 0.2084 0.8451 0.146 Uiso 1 1 calc R . . P6 P 0.18005(3) 0.13128(4) 0.87957(4) 0.0373(2) Uani 1 1 d . A . N6 N 0.20044(9) 0.13840(11) 0.83415(12) 0.0336(6) Uani 1 1 d . A . C6 C 0.24134(11) 0.10498(14) 0.85007(16) 0.0378(7) Uani 1 1 d . . . C61 C 0.25429(13) 0.13530(16) 0.80930(19) 0.0501(9) Uani 1 1 d . A . H61A H 0.2278 0.1318 0.7592 0.075 Uiso 1 1 calc R . . H61B H 0.2822 0.1156 0.8204 0.075 Uiso 1 1 calc R . . H61C H 0.2612 0.1779 0.8222 0.075 Uiso 1 1 calc R . . C62 C 0.28254(12) 0.10973(16) 0.92790(17) 0.0487(9) Uani 1 1 d . A . H62A H 0.2908 0.1522 0.9408 0.073 Uiso 1 1 calc R . . H62B H 0.3098 0.0880 0.9392 0.073 Uiso 1 1 calc R . . H62C H 0.2735 0.0921 0.9538 0.073 Uiso 1 1 calc R . . C63 C 0.22891(13) 0.03911(15) 0.82921(19) 0.0513(9) Uani 1 1 d . A . H63A H 0.2201 0.0205 0.8550 0.077 Uiso 1 1 calc R . . H63B H 0.2563 0.0181 0.8401 0.077 Uiso 1 1 calc R . . H63C H 0.2024 0.0363 0.7791 0.077 Uiso 1 1 calc R . . N13 N 0.20095(11) 0.19171(12) 0.93111(15) 0.0409(7) Uani 1 1 d . . . H13N H 0.2098(12) 0.1852(15) 0.9687(19) 0.045(11) Uiso 1 1 d . . . C34 C 0.20049(11) 0.25334(13) 0.91331(15) 0.0358(7) Uani 1 1 d . A . C35 C 0.17199(12) 0.29547(14) 0.91068(17) 0.0408(8) Uani 1 1 d . . . H35 H 0.1521 0.2834 0.9205 0.049 Uiso 1 1 calc R A . C36 C 0.17169(12) 0.35484(14) 0.89411(18) 0.0439(8) Uani 1 1 d . A . H36 H 0.1520 0.3830 0.8933 0.053 Uiso 1 1 calc R . . C37 C 0.20007(11) 0.37390(13) 0.87850(15) 0.0341(7) Uani 1 1 d . . . C38 C 0.22863(11) 0.33170(13) 0.88074(16) 0.0368(7) Uani 1 1 d . A . H38 H 0.2483 0.3436 0.8704 0.044 Uiso 1 1 calc R . . C39 C 0.22894(11) 0.27216(13) 0.89791(16) 0.0373(7) Uani 1 1 d . . . H39 H 0.2488 0.2439 0.8992 0.045 Uiso 1 1 calc R A . N14 N 0.20085(11) 0.43396(12) 0.86254(17) 0.0474(8) Uani 1 1 d . A . H14N H 0.2163(12) 0.4380(15) 0.8523(17) 0.036(10) Uiso 1 1 d . . . P7 P 0.17336(3) 0.49383(4) 0.86403(4) 0.0374(2) Uani 1 1 d . . . N7 N 0.15052(8) 0.53185(11) 0.78830(13) 0.0355(6) Uani 1 1 d . A . C7 C 0.09985(11) 0.53187(15) 0.72521(17) 0.0423(8) Uani 1 1 d . . . C71 C 0.06951(13) 0.5568(2) 0.7421(2) 0.0687(12) Uani 1 1 d . A . H71A H 0.0746 0.5327 0.7792 0.103 Uiso 1 1 calc R . . H71B H 0.0361 0.5549 0.7003 0.103 Uiso 1 1 calc R . . H71C H 0.0783 0.5987 0.7574 0.103 Uiso 1 1 calc R . . C72 C 0.09374(13) 0.56993(17) 0.66935(18) 0.0542(10) Uani 1 1 d . A . H72A H 0.1029 0.6116 0.6857 0.081 Uiso 1 1 calc R . . H72B H 0.0606 0.5689 0.6267 0.081 Uiso 1 1 calc R . . H72C H 0.1137 0.5539 0.6596 0.081 Uiso 1 1 calc R . . C73 C 0.08608(13) 0.46681(17) 0.7006(2) 0.0619(11) Uani 1 1 d . A . H73A H 0.1060 0.4510 0.6905 0.093 Uiso 1 1 calc R . . H73B H 0.0529 0.4652 0.6582 0.093 Uiso 1 1 calc R . . H73C H 0.0906 0.4424 0.7371 0.093 Uiso 1 1 calc R . . P8 P 0.18632(3) 0.59434(3) 0.82513(4) 0.03381(19) Uani 1 1 d . A . N8 N 0.21400(9) 0.55049(11) 0.89818(13) 0.0393(6) Uani 1 1 d . A . C8 C 0.25071(12) 0.56673(16) 0.97228(17) 0.0446(8) Uani 1 1 d . . . C81 C 0.28974(18) 0.5201(3) 1.0061(2) 0.131(3) Uani 1 1 d . A . H81A H 0.3037 0.5207 0.9834 0.197 Uiso 1 1 calc R . . H81B H 0.2766 0.4802 1.0009 0.197 Uiso 1 1 calc R . . H81C H 0.3141 0.5295 1.0557 0.197 Uiso 1 1 calc R . . C82 C 0.2682(3) 0.6282(3) 0.9781(2) 0.157(4) Uani 1 1 d . A . H82A H 0.2822 0.6297 0.9556 0.235 Uiso 1 1 calc R . . H82B H 0.2920 0.6390 1.0273 0.235 Uiso 1 1 calc R . . H82C H 0.2418 0.6567 0.9551 0.235 Uiso 1 1 calc R . . C83 C 0.23138(17) 0.5627(2) 1.0102(2) 0.0869(15) Uani 1 1 d . A . H83A H 0.2568 0.5707 1.0599 0.130 Uiso 1 1 calc R . . H83B H 0.2186 0.5223 1.0043 0.130 Uiso 1 1 calc R . . H83C H 0.2062 0.5925 0.9910 0.130 Uiso 1 1 calc R . . N15 N 0.21911(10) 0.59043(13) 0.79988(15) 0.0382(7) Uani 1 1 d . . . H15N H 0.2289(13) 0.6196(17) 0.8004(19) 0.050(12) Uiso 1 1 d . . . C44 C 0.24427(11) 0.53899(13) 0.80378(16) 0.0347(7) Uani 1 1 d . A . C45 C 0.29295(12) 0.53534(15) 0.85108(18) 0.0469(8) Uani 1 1 d . . . H45 H 0.3105 0.5680 0.8819 0.056 Uiso 1 1 calc R A . C46 C 0.31682(11) 0.48547(16) 0.85478(18) 0.0502(9) Uani 1 1 d . A . H46 H 0.3504 0.4846 0.8875 0.060 Uiso 1 1 calc R . . C47 C 0.29203(11) 0.43623(14) 0.81080(16) 0.0372(7) Uani 1 1 d . . . C48 C 0.24323(10) 0.44008(14) 0.76293(16) 0.0368(7) Uani 1 1 d . A . H48 H 0.2255 0.4074 0.7321 0.044 Uiso 1 1 calc R . . C49 C 0.21987(11) 0.49069(14) 0.75926(16) 0.0374(7) Uani 1 1 d . . . H49 H 0.1864 0.4923 0.7255 0.045 Uiso 1 1 calc R A . N16 N 0.31492(10) 0.38476(14) 0.81288(16) 0.0489(8) Uani 1 1 d . A . H16N H 0.2977(11) 0.3629(14) 0.7826(17) 0.033(9) Uiso 1 1 d . . . C1P C 0.0465(4) -0.0596(4) 1.0351(5) 0.241(6) Uani 1 1 d . . . H1P1 H 0.0268 -0.0241 1.0227 0.362 Uiso 1 1 calc R . . H1P2 H 0.0729 -0.0597 1.0854 0.362 Uiso 1 1 calc R . . H1P3 H 0.0276 -0.0960 1.0222 0.362 Uiso 1 1 calc R . . C2P C 0.0687(4) -0.0576(6) 0.9902(7) 0.221(5) Uiso 1 1 d . . . H2P1 H 0.1034 -0.0629 1.0213 0.265 Uiso 1 1 calc R . . H2P2 H 0.0528 -0.0866 0.9511 0.265 Uiso 1 1 calc R . . C3P C 0.0549(4) 0.0006(5) 0.9684(6) 0.201(4) Uiso 1 1 d . . . H3P1 H 0.0684 0.0290 1.0076 0.241 Uiso 1 1 calc R . . H3P2 H 0.0201 0.0051 0.9341 0.241 Uiso 1 1 calc R . . C4P C 0.0797(5) 0.0062(6) 0.9328(7) 0.258(6) Uiso 1 1 d . . . H4P1 H 0.0707 0.0462 0.9100 0.310 Uiso 1 1 calc R . . H4P2 H 0.1142 0.0076 0.9716 0.310 Uiso 1 1 calc R . . C5P C 0.0724(5) -0.0341(6) 0.8857(7) 0.271(6) Uiso 1 1 d . . . H5P1 H 0.0825 -0.0741 0.9069 0.407 Uiso 1 1 calc R . . H5P2 H 0.0908 -0.0220 0.8716 0.407 Uiso 1 1 calc R . . H5P3 H 0.0388 -0.0350 0.8447 0.407 Uiso 1 1 calc R . . C1T C 0.0169(7) 0.3556(7) 0.8599(9) 0.130(5) Uani 0.50 1 d P . . H1T1 H -0.0131 0.3349 0.8382 0.195 Uiso 0.50 1 calc PR . . H1T2 H 0.0223 0.3857 0.8930 0.195 Uiso 0.50 1 calc PR . . H1T3 H 0.0427 0.3262 0.8846 0.195 Uiso 0.50 1 calc PR . . C2T C 0.0155(9) 0.3805(10) 0.8151(13) 0.190(9) Uiso 0.50 1 d P . . H2T1 H 0.0477 0.3960 0.8387 0.228 Uiso 0.50 1 calc PR . . H2T2 H -0.0051 0.4161 0.8002 0.228 Uiso 0.50 1 calc PR . . C3T C 0.0000 0.3508(12) 0.7500 0.312(13) Uiso 1 2 d S . . H3T1 H 0.0234 0.3582 0.7434 0.375 Uiso 0.50 1 calc PR . . H3T2 H -0.0027 0.3068 0.7529 0.375 Uiso 0.50 1 calc PR . . C4T C -0.0363(9) 0.3707(12) 0.7038(13) 0.212(10) Uiso 0.50 1 d P . . H4T1 H -0.0345 0.4151 0.7038 0.255 Uiso 0.50 1 calc PR . . H4T2 H -0.0605 0.3594 0.7076 0.255 Uiso 0.50 1 calc PR . . C5T C -0.0490(6) 0.3450(6) 0.6371(8) 0.115(5) Uani 0.50 1 d P . . H5T1 H -0.0283 0.3626 0.6294 0.173 Uiso 0.50 1 calc PR . . H5T2 H -0.0820 0.3547 0.5976 0.173 Uiso 0.50 1 calc PR . . H5T3 H -0.0450 0.3012 0.6414 0.173 Uiso 0.50 1 calc PR . . 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 0.0307(4) 0.0477(5) 0.0425(5) -0.0118(4) 0.0191(4) 0.0033(4) N1 0.0358(14) 0.0359(15) 0.0477(16) -0.0052(12) 0.0274(13) 0.0022(11) C1 0.047(2) 0.045(2) 0.066(2) -0.0064(18) 0.0381(19) -0.0071(16) P2 0.0257(4) 0.0382(5) 0.0366(4) -0.0035(4) 0.0153(4) 0.0044(3) N2 0.0327(14) 0.0511(17) 0.0340(14) -0.0017(12) 0.0181(12) 0.0072(12) C2 0.042(2) 0.079(3) 0.0388(19) 0.0046(19) 0.0226(17) 0.0054(18) C21 0.081(3) 0.119(4) 0.072(3) 0.010(3) 0.061(3) 0.012(3) C22 0.052(2) 0.102(4) 0.036(2) 0.004(2) 0.0109(19) 0.004(2) C23 0.063(3) 0.070(3) 0.055(2) 0.017(2) 0.030(2) 0.003(2) N9 0.0311(14) 0.0364(16) 0.0407(16) -0.0054(13) 0.0171(13) 0.0044(12) C14 0.0279(15) 0.0286(16) 0.0339(16) -0.0044(13) 0.0135(14) -0.0018(12) C15 0.0338(17) 0.065(2) 0.0427(19) 0.0017(17) 0.0239(16) 0.0019(16) C16 0.0329(18) 0.080(3) 0.0345(18) 0.0130(18) 0.0182(15) 0.0047(17) C17 0.0250(15) 0.0399(18) 0.0318(16) 0.0037(14) 0.0119(13) -0.0016(13) C18 0.0309(16) 0.0403(18) 0.0331(16) 0.0077(14) 0.0153(14) -0.0001(13) C19 0.0282(15) 0.0471(19) 0.0356(17) 0.0028(14) 0.0184(14) -0.0042(13) N10 0.0235(13) 0.068(2) 0.0333(15) 0.0160(14) 0.0135(12) 0.0029(13) P3 0.0268(4) 0.0550(6) 0.0332(4) 0.0108(4) 0.0134(4) -0.0009(4) N3 0.0283(13) 0.0456(16) 0.0342(14) 0.0091(12) 0.0130(12) -0.0009(11) C3 0.045(2) 0.046(2) 0.046(2) 0.0072(16) 0.0225(17) -0.0017(16) C31 0.086(3) 0.055(2) 0.074(3) 0.021(2) 0.050(3) 0.002(2) C32 0.051(2) 0.059(3) 0.058(2) -0.007(2) 0.017(2) -0.0134(19) C33 0.054(2) 0.056(2) 0.062(2) 0.005(2) 0.031(2) 0.0062(19) P4 0.0266(4) 0.0522(5) 0.0308(4) 0.0105(4) 0.0108(4) -0.0002(4) N4 0.0323(14) 0.0554(18) 0.0286(14) 0.0057(12) 0.0138(12) -0.0001(12) C4 0.050(2) 0.059(2) 0.0391(19) 0.0026(17) 0.0232(17) -0.0001(18) C41 0.087(3) 0.089(3) 0.055(2) -0.005(2) 0.047(2) -0.012(3) C42 0.068(3) 0.081(3) 0.065(3) -0.006(2) 0.032(2) 0.016(2) C43 0.068(3) 0.065(3) 0.048(2) -0.008(2) 0.027(2) -0.013(2) N11 0.0229(14) 0.062(2) 0.0369(16) 0.0118(14) 0.0095(13) -0.0037(13) C24 0.0274(16) 0.055(2) 0.0392(18) 0.0120(16) 0.0178(15) -0.0005(15) C25 0.0445(19) 0.047(2) 0.049(2) 0.0117(17) 0.0288(18) 0.0084(16) C26 0.050(2) 0.048(2) 0.0403(19) 0.0063(16) 0.0276(17) 0.0050(16) C27 0.0337(16) 0.045(2) 0.0345(17) 0.0073(15) 0.0195(15) -0.0013(14) C28 0.052(2) 0.044(2) 0.0406(19) 0.0078(16) 0.0258(17) 0.0040(16) C29 0.0442(19) 0.055(2) 0.0356(18) 0.0021(16) 0.0204(16) -0.0049(16) N12 0.0462(17) 0.0426(17) 0.0317(15) 0.0063(14) 0.0198(14) 0.0014(13) P5 0.0387(5) 0.0398(5) 0.0348(4) 0.0032(4) 0.0213(4) -0.0001(4) N5 0.0364(15) 0.0475(17) 0.0472(16) 0.0044(13) 0.0269(13) -0.0004(12) C5 0.041(2) 0.054(2) 0.075(3) -0.001(2) 0.040(2) -0.0038(16) C51 0.072(3) 0.086(4) 0.145(5) -0.034(3) 0.074(3) -0.037(3) C52 0.049(3) 0.137(5) 0.143(5) 0.069(4) 0.056(3) 0.033(3) C53 0.069(3) 0.128(4) 0.130(5) -0.029(4) 0.080(3) -0.018(3) P6 0.0484(5) 0.0305(4) 0.0418(5) 0.0044(4) 0.0330(4) 0.0007(4) N6 0.0372(14) 0.0346(14) 0.0312(13) 0.0054(11) 0.0229(12) 0.0051(11) C6 0.0388(17) 0.0367(17) 0.0367(17) 0.0010(14) 0.0237(15) 0.0040(14) C61 0.050(2) 0.057(2) 0.054(2) -0.0016(18) 0.0384(19) 0.0023(17) C62 0.0428(19) 0.049(2) 0.0443(19) 0.0026(16) 0.0233(17) 0.0103(16) C63 0.058(2) 0.0359(19) 0.057(2) -0.0024(17) 0.0355(19) 0.0033(16) N13 0.0635(19) 0.0313(15) 0.0366(16) 0.0050(12) 0.0361(15) 0.0003(13) C34 0.0453(18) 0.0291(16) 0.0319(16) 0.0028(13) 0.0242(15) 0.0002(14) C35 0.051(2) 0.0383(18) 0.049(2) 0.0008(15) 0.0393(17) -0.0001(15) C36 0.051(2) 0.0356(18) 0.057(2) 0.0085(16) 0.0405(18) 0.0089(15) C37 0.0387(17) 0.0287(16) 0.0332(16) 0.0050(13) 0.0222(14) 0.0043(13) C38 0.0392(17) 0.0356(17) 0.0395(17) 0.0039(14) 0.0271(15) 0.0035(14) C39 0.0439(18) 0.0292(16) 0.0403(17) 0.0046(14) 0.0277(15) 0.0080(14) N14 0.0554(19) 0.0343(16) 0.072(2) 0.0173(14) 0.0500(18) 0.0107(13) P7 0.0392(5) 0.0314(4) 0.0438(5) 0.0061(4) 0.0276(4) 0.0044(3) N7 0.0329(13) 0.0290(13) 0.0388(14) 0.0039(11) 0.0204(12) 0.0038(11) C7 0.0302(16) 0.0437(19) 0.0409(18) -0.0008(15) 0.0171(15) 0.0033(14) C71 0.038(2) 0.094(3) 0.061(2) 0.008(2) 0.0257(19) 0.022(2) C72 0.043(2) 0.055(2) 0.0402(19) 0.0052(17) 0.0158(17) 0.0051(17) C73 0.050(2) 0.052(2) 0.059(2) -0.0085(19) 0.0230(19) -0.0125(18) P8 0.0356(4) 0.0266(4) 0.0377(4) 0.0040(3) 0.0228(4) 0.0055(3) N8 0.0418(15) 0.0348(14) 0.0333(14) 0.0020(11) 0.0203(12) -0.0020(12) C8 0.0417(19) 0.054(2) 0.0345(17) 0.0007(15) 0.0228(15) 0.0005(16) C81 0.068(3) 0.203(7) 0.052(3) -0.011(4) 0.006(3) 0.066(4) C82 0.197(7) 0.133(5) 0.042(3) -0.021(3) 0.032(4) -0.123(5) C83 0.086(3) 0.121(4) 0.063(3) -0.033(3) 0.051(3) -0.025(3) N15 0.0432(16) 0.0279(15) 0.0475(17) 0.0028(13) 0.0309(14) 0.0022(13) C44 0.0393(17) 0.0334(17) 0.0392(17) 0.0047(14) 0.0287(15) 0.0039(13) C45 0.0404(19) 0.0439(19) 0.052(2) -0.0135(16) 0.0275(17) -0.0019(15) C46 0.0280(16) 0.056(2) 0.054(2) -0.0179(18) 0.0208(16) 0.0010(15) C47 0.0365(17) 0.0395(18) 0.0395(17) -0.0008(14) 0.0262(15) 0.0047(14) C48 0.0335(16) 0.0375(18) 0.0365(17) -0.0060(14) 0.0211(14) -0.0024(13) C49 0.0309(16) 0.0397(18) 0.0351(17) 0.0058(14) 0.0182(14) 0.0055(13) N16 0.0310(15) 0.0496(18) 0.0499(18) -0.0188(15) 0.0184(14) 0.0013(13) C1P 0.246(12) 0.149(8) 0.173(9) 0.033(7) 0.063(9) 0.080(8) C1T 0.164(16) 0.080(9) 0.145(13) 0.013(9) 0.099(13) 0.007(10) C5T 0.126(12) 0.085(9) 0.136(12) -0.020(8) 0.085(11) -0.021(8) _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 N16 1.691(3) . ? P1 N1 1.715(3) . ? P1 N2 1.727(3) . ? P1 P2 2.6030(12) . ? N1 C1 1.475(4) . ? N1 P2 1.717(3) . ? C1 C12' 1.42(2) . ? C1 C13 1.499(7) . ? C1 C12 1.525(7) . ? C1 C11 1.527(7) . ? C1 C11' 1.55(2) . ? C1 C13' 1.58(2) . ? P2 N9 1.682(3) . ? P2 N2 1.725(3) . ? N2 C2 1.483(4) . ? C2 C21 1.527(5) . ? C2 C23 1.528(6) . ? C2 C22 1.529(5) . ? N9 C14 1.432(4) . ? C14 C18 1.372(4) . ? C14 C15 1.378(5) . ? C15 C16 1.379(5) . ? C16 C17 1.397(5) . ? C17 C19 1.388(4) . ? C17 N10 1.401(4) . ? C18 C19 1.391(4) . ? N10 P3 1.697(3) . ? P3 N4 1.718(3) . ? P3 N3 1.726(3) . ? P3 P4 2.5980(16) . ? N3 C3 1.487(4) . ? N3 P4 1.723(3) . ? C3 C33 1.518(5) . ? C3 C31 1.522(5) . ? C3 C32 1.530(5) . ? P4 N11 1.690(3) . ? P4 N4 1.720(3) . ? N4 C4 1.481(5) . ? C4 C43 1.524(5) . ? C4 C42 1.527(5) . ? C4 C41 1.536(5) . ? N11 C24 1.440(4) . ? C24 C25 1.377(5) . ? C24 C29 1.391(5) . ? C25 C26 1.387(5) . ? C26 C27 1.385(5) . ? C27 C28 1.386(5) . ? C27 N12 1.409(4) . ? C28 C29 1.389(5) . ? N12 P5 1.707(3) . ? P5 N5 1.714(3) . ? P5 N6 1.715(3) . ? P5 P6 2.5994(14) . ? N5 C5 1.477(4) . ? N5 P6 1.720(3) . ? C5 C53 1.507(6) . ? C5 C51 1.518(6) . ? C5 C52 1.518(6) . ? P6 N13 1.669(3) . ? P6 N6 1.725(3) . ? N6 C6 1.489(4) . ? C6 C63 1.523(4) . ? C6 C62 1.522(4) . ? C6 C61 1.532(5) . ? N13 C34 1.437(4) . ? C34 C35 1.378(4) . ? C34 C39 1.393(4) . ? C35 C36 1.381(4) . ? C36 C37 1.397(4) . ? C37 C38 1.384(4) . ? C37 N14 1.399(4) . ? C38 C39 1.389(4) . ? N14 P7 1.688(3) . ? P7 N8 1.709(3) . ? P7 N7 1.722(3) . ? P7 P8 2.6000(12) . ? N7 C7 1.484(4) . ? N7 P8 1.721(3) . ? C7 C72 1.521(5) . ? C7 C73 1.525(5) . ? C7 C71 1.530(5) . ? P8 N15 1.688(3) . ? P8 N8 1.714(3) . ? N8 C8 1.477(4) . ? C8 C82 1.477(6) . ? C8 C83 1.511(5) . ? C8 C81 1.516(6) . ? N15 C44 1.436(4) . ? C44 C45 1.381(4) . ? C44 C49 1.385(4) . ? C45 C46 1.381(5) . ? C46 C47 1.398(4) . ? C47 C48 1.385(4) . ? C47 N16 1.403(4) . ? C48 C49 1.384(4) . ? C1P C2P 1.764(15) . ? C2P C3P 1.368(12) . ? C3P C4P 1.640(14) . ? C4P C5P 1.362(15) . ? C1T C2T 1.22(2) . ? C2T C3T 1.49(2) . ? C3T C4T 1.16(2) . ? C4T C5T 1.52(3) . ? 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 N16 P1 N1 105.15(15) . . ? N16 P1 N2 103.28(15) . . ? N1 P1 N2 80.99(13) . . ? N16 P1 P2 114.84(11) . . ? N1 P1 P2 40.70(9) . . ? N2 P1 P2 41.03(9) . . ? C1 N1 P1 126.2(2) . . ? C1 N1 P2 129.2(2) . . ? P1 N1 P2 98.65(15) . . ? C12' C1 N1 116.3(10) . . ? C12' C1 C13 134.3(10) . . ? N1 C1 C13 109.1(4) . . ? C12' C1 C12 50.2(10) . . ? N1 C1 C12 109.0(3) . . ? C13 C1 C12 110.5(4) . . ? C12' C1 C11 57.4(10) . . ? N1 C1 C11 109.2(4) . . ? C13 C1 C11 111.9(4) . . ? C12 C1 C11 106.9(4) . . ? C12' C1 C11' 116.3(14) . . ? N1 C1 C11' 109.1(10) . . ? C13 C1 C11' 48.0(9) . . ? C12 C1 C11' 141.0(10) . . ? C11 C1 C11' 67.1(10) . . ? C12' C1 C13' 111.3(14) . . ? N1 C1 C13' 105.2(10) . . ? C13 C1 C13' 49.0(10) . . ? C12 C1 C13' 66.1(10) . . ? C11 C1 C13' 145.0(10) . . ? C11' C1 C13' 96.2(14) . . ? N9 P2 N1 105.48(14) . . ? N9 P2 N2 105.17(15) . . ? N1 P2 N2 81.00(13) . . ? N9 P2 P1 116.34(11) . . ? N1 P2 P1 40.65(9) . . ? N2 P2 P1 41.09(10) . . ? C2 N2 P2 125.4(2) . . ? C2 N2 P1 124.2(2) . . ? P2 N2 P1 97.88(15) . . ? N2 C2 C21 107.1(3) . . ? N2 C2 C23 108.4(3) . . ? C21 C2 C23 110.1(4) . . ? N2 C2 C22 110.8(3) . . ? C21 C2 C22 110.7(4) . . ? C23 C2 C22 109.8(3) . . ? C14 N9 P2 127.2(2) . . ? C18 C14 C15 117.9(3) . . ? C18 C14 N9 120.8(3) . . ? C15 C14 N9 121.3(3) . . ? C14 C15 C16 121.6(3) . . ? C15 C16 C17 120.8(3) . . ? C19 C17 C16 117.4(3) . . ? C19 C17 N10 120.0(3) . . ? C16 C17 N10 122.6(3) . . ? C14 C18 C19 121.5(3) . . ? C17 C19 C18 120.8(3) . . ? C17 N10 P3 126.6(3) . . ? N10 P3 N4 105.53(14) . . ? N10 P3 N3 102.61(15) . . ? N4 P3 N3 81.35(13) . . ? N10 P3 P4 114.49(11) . . ? N4 P3 P4 40.96(10) . . ? N3 P3 P4 41.08(9) . . ? C3 N3 P4 125.5(2) . . ? C3 N3 P3 123.1(2) . . ? P4 N3 P3 97.75(15) . . ? N3 C3 C33 108.8(3) . . ? N3 C3 C31 110.9(3) . . ? C33 C3 C31 109.9(3) . . ? N3 C3 C32 107.1(3) . . ? C33 C3 C32 109.5(3) . . ? C31 C3 C32 110.7(3) . . ? N11 P4 N4 106.52(14) . . ? N11 P4 N3 102.15(15) . . ? N4 P4 N3 81.38(13) . . ? N11 P4 P3 114.85(10) . . ? N4 P4 P3 40.89(9) . . ? N3 P4 P3 41.17(10) . . ? C4 N4 P3 123.5(2) . . ? C4 N4 P4 126.3(2) . . ? P3 N4 P4 98.15(15) . . ? N4 C4 C43 108.6(3) . . ? N4 C4 C42 107.7(3) . . ? C43 C4 C42 110.3(3) . . ? N4 C4 C41 110.7(3) . . ? C43 C4 C41 109.3(3) . . ? C42 C4 C41 110.2(4) . . ? C24 N11 P4 122.6(2) . . ? C25 C24 C29 117.9(3) . . ? C25 C24 N11 120.2(3) . . ? C29 C24 N11 121.8(3) . . ? C24 C25 C26 121.5(3) . . ? C27 C26 C25 120.8(3) . . ? C26 C27 C28 118.1(3) . . ? C26 C27 N12 121.1(3) . . ? C28 C27 N12 120.8(3) . . ? C27 C28 C29 120.9(3) . . ? C28 C29 C24 120.9(3) . . ? C27 N12 P5 122.5(2) . . ? N12 P5 N5 104.82(15) . . ? N12 P5 N6 102.45(13) . . ? N5 P5 N6 80.90(13) . . ? N12 P5 P6 115.20(11) . . ? N5 P5 P6 40.88(9) . . ? N6 P5 P6 41.06(9) . . ? C5 N5 P5 125.8(2) . . ? C5 N5 P6 128.6(2) . . ? P5 N5 P6 98.41(14) . . ? N5 C5 C53 108.3(3) . . ? N5 C5 C51 110.4(3) . . ? C53 C5 C51 109.2(4) . . ? N5 C5 C52 107.7(3) . . ? C53 C5 C52 110.4(4) . . ? C51 C5 C52 110.8(4) . . ? N13 P6 N5 105.55(15) . . ? N13 P6 N6 104.73(14) . . ? N5 P6 N6 80.44(13) . . ? N13 P6 P5 117.09(11) . . ? N5 P6 P5 40.71(10) . . ? N6 P6 P5 40.76(9) . . ? C6 N6 P5 124.9(2) . . ? C6 N6 P6 124.96(19) . . ? P5 N6 P6 98.18(13) . . ? N6 C6 C63 110.9(3) . . ? N6 C6 C62 108.5(3) . . ? C63 C6 C62 109.8(3) . . ? N6 C6 C61 107.3(2) . . ? C63 C6 C61 110.4(3) . . ? C62 C6 C61 109.8(3) . . ? C34 N13 P6 128.3(2) . . ? C35 C34 C39 118.0(3) . . ? C35 C34 N13 121.3(3) . . ? C39 C34 N13 120.7(3) . . ? C34 C35 C36 121.5(3) . . ? C35 C36 C37 120.7(3) . . ? C38 C37 C36 118.1(3) . . ? C38 C37 N14 120.3(3) . . ? C36 C37 N14 121.7(3) . . ? C37 C38 C39 120.9(3) . . ? C38 C39 C34 120.9(3) . . ? C37 N14 P7 128.6(3) . . ? N14 P7 N8 104.18(15) . . ? N14 P7 N7 103.88(14) . . ? N8 P7 N7 80.92(13) . . ? N14 P7 P8 114.32(12) . . ? N8 P7 P8 40.65(9) . . ? N7 P7 P8 40.94(9) . . ? C7 N7 P8 125.5(2) . . ? C7 N7 P7 124.4(2) . . ? P8 N7 P7 98.09(13) . . ? N7 C7 C72 108.7(3) . . ? N7 C7 C73 107.2(3) . . ? C72 C7 C73 109.9(3) . . ? N7 C7 C71 110.6(3) . . ? C72 C7 C71 110.4(3) . . ? C73 C7 C71 110.0(3) . . ? N15 P8 N8 106.82(14) . . ? N15 P8 N7 104.26(14) . . ? N8 P8 N7 80.81(13) . . ? N15 P8 P7 116.32(11) . . ? N8 P8 P7 40.50(9) . . ? N7 P8 P7 40.97(9) . . ? C8 N8 P7 127.8(2) . . ? C8 N8 P8 129.7(2) . . ? P7 N8 P8 98.84(14) . . ? N8 C8 C82 109.9(3) . . ? N8 C8 C83 110.5(3) . . ? C82 C8 C83 110.2(4) . . ? N8 C8 C81 108.2(3) . . ? C82 C8 C81 112.2(5) . . ? C83 C8 C81 105.8(4) . . ? C44 N15 P8 127.1(2) . . ? C45 C44 C49 117.5(3) . . ? C45 C44 N15 122.3(3) . . ? C49 C44 N15 120.3(3) . . ? C44 C45 C46 121.8(3) . . ? C45 C46 C47 120.5(3) . . ? C48 C47 C46 117.7(3) . . ? C48 C47 N16 120.0(3) . . ? C46 C47 N16 122.3(3) . . ? C49 C48 C47 121.1(3) . . ? C48 C49 C44 121.4(3) . . ? C47 N16 P1 128.3(2) . . ? C3P C2P C1P 94.1(9) . . ? C2P C3P C4P 95.4(10) . . ? C5P C4P C3P 123.4(13) . . ? C1T C2T C3T 124(2) . . ? C4T C3T C2T 108(2) . . ? C3T C4T C5T 107(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 N16 P1 N1 C1 94.9(3) . . . . ? N2 P1 N1 C1 -163.7(3) . . . . ? P2 P1 N1 C1 -154.5(3) . . . . ? N16 P1 N1 P2 -110.65(15) . . . . ? N2 P1 N1 P2 -9.23(13) . . . . ? P1 N1 C1 C12' 128.9(11) . . . . ? P2 N1 C1 C12' -17.8(12) . . . . ? P1 N1 C1 C13 -56.1(4) . . . . ? P2 N1 C1 C13 157.2(3) . . . . ? P1 N1 C1 C12 -176.9(3) . . . . ? P2 N1 C1 C12 36.4(4) . . . . ? P1 N1 C1 C11 66.5(4) . . . . ? P2 N1 C1 C11 -80.1(4) . . . . ? P1 N1 C1 C11' -5.1(11) . . . . ? P2 N1 C1 C11' -151.8(11) . . . . ? P1 N1 C1 C13' -107.4(11) . . . . ? P2 N1 C1 C13' 105.9(11) . . . . ? C1 N1 P2 N9 -94.0(3) . . . . ? P1 N1 P2 N9 112.60(15) . . . . ? C1 N1 P2 N2 162.6(3) . . . . ? P1 N1 P2 N2 9.24(13) . . . . ? C1 N1 P2 P1 153.4(3) . . . . ? N16 P1 P2 N9 1.33(19) . . . . ? N1 P1 P2 N9 -83.13(18) . . . . ? N2 P1 P2 N9 82.90(18) . . . . ? N16 P1 P2 N1 84.46(19) . . . . ? N2 P1 P2 N1 166.03(19) . . . . ? N16 P1 P2 N2 -81.58(19) . . . . ? N1 P1 P2 N2 -166.03(19) . . . . ? N9 P2 N2 C2 104.4(3) . . . . ? N1 P2 N2 C2 -151.9(3) . . . . ? P1 P2 N2 C2 -142.7(3) . . . . ? N9 P2 N2 P1 -112.87(14) . . . . ? N1 P2 N2 P1 -9.16(12) . . . . ? N16 P1 N2 C2 -103.9(3) . . . . ? N1 P1 N2 C2 152.5(3) . . . . ? P2 P1 N2 C2 143.3(3) . . . . ? N16 P1 N2 P2 112.73(15) . . . . ? N1 P1 N2 P2 9.17(12) . . . . ? P2 N2 C2 C21 -165.4(3) . . . . ? P1 N2 C2 C21 61.2(4) . . . . ? P2 N2 C2 C23 -46.7(4) . . . . ? P1 N2 C2 C23 179.8(2) . . . . ? P2 N2 C2 C22 73.8(4) . . . . ? P1 N2 C2 C22 -59.6(4) . . . . ? N1 P2 N9 C14 -35.1(3) . . . . ? N2 P2 N9 C14 49.6(3) . . . . ? P1 P2 N9 C14 7.1(3) . . . . ? P2 N9 C14 C18 -74.0(4) . . . . ? P2 N9 C14 C15 105.8(4) . . . . ? C18 C14 C15 C16 2.2(5) . . . . ? N9 C14 C15 C16 -177.6(3) . . . . ? C14 C15 C16 C17 0.8(6) . . . . ? C15 C16 C17 C19 -3.0(5) . . . . ? C15 C16 C17 N10 177.6(3) . . . . ? C15 C14 C18 C19 -3.0(5) . . . . ? N9 C14 C18 C19 176.8(3) . . . . ? C16 C17 C19 C18 2.2(5) . . . . ? N10 C17 C19 C18 -178.4(3) . . . . ? C14 C18 C19 C17 0.8(5) . . . . ? C19 C17 N10 P3 176.3(3) . . . . ? C16 C17 N10 P3 -4.3(5) . . . . ? C17 N10 P3 N4 121.0(3) . . . . ? C17 N10 P3 N3 -154.6(3) . . . . ? C17 N10 P3 P4 163.7(2) . . . . ? N10 P3 N3 C3 105.0(3) . . . . ? N4 P3 N3 C3 -150.9(3) . . . . ? P4 P3 N3 C3 -142.0(3) . . . . ? N10 P3 N3 P4 -112.95(15) . . . . ? N4 P3 N3 P4 -8.86(13) . . . . ? P4 N3 C3 C33 50.3(4) . . . . ? P3 N3 C3 C33 -178.2(2) . . . . ? P4 N3 C3 C31 -70.7(4) . . . . ? P3 N3 C3 C31 60.8(4) . . . . ? P4 N3 C3 C32 168.5(3) . . . . ? P3 N3 C3 C32 -60.1(4) . . . . ? C3 N3 P4 N11 -105.3(3) . . . . ? P3 N3 P4 N11 114.01(15) . . . . ? C3 N3 P4 N4 149.5(3) . . . . ? P3 N3 P4 N4 8.85(13) . . . . ? C3 N3 P4 P3 140.7(3) . . . . ? N10 P3 P4 N11 1.15(19) . . . . ? N4 P3 P4 N11 86.78(19) . . . . ? N3 P3 P4 N11 -79.79(19) . . . . ? N10 P3 P4 N4 -85.63(19) . . . . ? N3 P3 P4 N4 -166.57(19) . . . . ? N10 P3 P4 N3 80.94(18) . . . . ? N4 P3 P4 N3 166.57(19) . . . . ? N10 P3 N4 C4 -105.9(3) . . . . ? N3 P3 N4 C4 153.3(3) . . . . ? P4 P3 N4 C4 144.4(3) . . . . ? N10 P3 N4 P4 109.66(15) . . . . ? N3 P3 N4 P4 8.88(13) . . . . ? N11 P4 N4 C4 107.9(3) . . . . ? N3 P4 N4 C4 -151.9(3) . . . . ? P3 P4 N4 C4 -143.0(3) . . . . ? N11 P4 N4 P3 -109.10(16) . . . . ? N3 P4 N4 P3 -8.90(13) . . . . ? P3 N4 C4 C43 176.0(2) . . . . ? P4 N4 C4 C43 -49.7(4) . . . . ? P3 N4 C4 C42 56.5(4) . . . . ? P4 N4 C4 C42 -169.2(3) . . . . ? P3 N4 C4 C41 -64.0(4) . . . . ? P4 N4 C4 C41 70.3(4) . . . . ? N4 P4 N11 C24 40.2(3) . . . . ? N3 P4 N11 C24 -44.3(3) . . . . ? P3 P4 N11 C24 -2.8(3) . . . . ? P4 N11 C24 C25 92.2(4) . . . . ? P4 N11 C24 C29 -82.9(4) . . . . ? C29 C24 C25 C26 -0.1(5) . . . . ? N11 C24 C25 C26 -175.4(3) . . . . ? C24 C25 C26 C27 0.3(5) . . . . ? C25 C26 C27 C28 0.0(5) . . . . ? C25 C26 C27 N12 178.9(3) . . . . ? C26 C27 C28 C29 -0.6(5) . . . . ? N12 C27 C28 C29 -179.5(3) . . . . ? C27 C28 C29 C24 0.9(5) . . . . ? C25 C24 C29 C28 -0.5(5) . . . . ? N11 C24 C29 C28 174.7(3) . . . . ? C26 C27 N12 P5 141.7(3) . . . . ? C28 C27 N12 P5 -39.5(4) . . . . ? C27 N12 P5 N5 -106.5(3) . . . . ? C27 N12 P5 N6 169.7(3) . . . . ? C27 N12 P5 P6 -148.8(2) . . . . ? N12 P5 N5 C5 96.2(3) . . . . ? N6 P5 N5 C5 -163.2(3) . . . . ? P6 P5 N5 C5 -152.2(3) . . . . ? N12 P5 N5 P6 -111.54(15) . . . . ? N6 P5 N5 P6 -10.96(13) . . . . ? P5 N5 C5 C53 -173.1(3) . . . . ? P6 N5 C5 C53 43.0(5) . . . . ? P5 N5 C5 C51 67.4(4) . . . . ? P6 N5 C5 C51 -76.5(4) . . . . ? P5 N5 C5 C52 -53.8(5) . . . . ? P6 N5 C5 C52 162.4(4) . . . . ? C5 N5 P6 N13 -95.2(3) . . . . ? P5 N5 P6 N13 113.67(15) . . . . ? C5 N5 P6 N6 162.0(3) . . . . ? P5 N5 P6 N6 10.91(13) . . . . ? C5 N5 P6 P5 151.1(4) . . . . ? N12 P5 P6 N13 1.23(18) . . . . ? N5 P5 P6 N13 -82.37(19) . . . . ? N6 P5 P6 N13 81.02(18) . . . . ? N12 P5 P6 N5 83.60(19) . . . . ? N6 P5 P6 N5 163.39(19) . . . . ? N12 P5 P6 N6 -79.79(17) . . . . ? N5 P5 P6 N6 -163.39(19) . . . . ? N12 P5 N6 C6 -102.1(3) . . . . ? N5 P5 N6 C6 154.6(3) . . . . ? P6 P5 N6 C6 143.7(3) . . . . ? N12 P5 N6 P6 114.22(15) . . . . ? N5 P5 N6 P6 10.92(13) . . . . ? N13 P6 N6 C6 101.8(3) . . . . ? N5 P6 N6 C6 -154.5(3) . . . . ? P5 P6 N6 C6 -143.6(3) . . . . ? N13 P6 N6 P5 -114.60(15) . . . . ? N5 P6 N6 P5 -10.90(13) . . . . ? P5 N6 C6 C63 -61.8(3) . . . . ? P6 N6 C6 C63 72.5(3) . . . . ? P5 N6 C6 C62 177.5(2) . . . . ? P6 N6 C6 C62 -48.2(3) . . . . ? P5 N6 C6 C61 58.9(3) . . . . ? P6 N6 C6 C61 -166.8(2) . . . . ? N5 P6 N13 C34 -37.8(3) . . . . ? N6 P6 N13 C34 46.2(3) . . . . ? P5 P6 N13 C34 4.4(3) . . . . ? P6 N13 C34 C35 109.8(3) . . . . ? P6 N13 C34 C39 -70.0(4) . . . . ? C39 C34 C35 C36 -0.7(5) . . . . ? N13 C34 C35 C36 179.5(3) . . . . ? C34 C35 C36 C37 0.9(5) . . . . ? C35 C36 C37 C38 -0.5(5) . . . . ? C35 C36 C37 N14 -179.1(3) . . . . ? C36 C37 C38 C39 0.1(5) . . . . ? N14 C37 C38 C39 178.7(3) . . . . ? C37 C38 C39 C34 0.0(5) . . . . ? C35 C34 C39 C38 0.3(5) . . . . ? N13 C34 C39 C38 -179.9(3) . . . . ? C38 C37 N14 P7 -173.8(3) . . . . ? C36 C37 N14 P7 4.7(5) . . . . ? C37 N14 P7 N8 139.9(3) . . . . ? C37 N14 P7 N7 -136.2(3) . . . . ? C37 N14 P7 P8 -178.2(3) . . . . ? N14 P7 N7 C7 104.9(3) . . . . ? N8 P7 N7 C7 -152.6(3) . . . . ? P8 P7 N7 C7 -143.8(3) . . . . ? N14 P7 N7 P8 -111.26(15) . . . . ? N8 P7 N7 P8 -8.78(13) . . . . ? P8 N7 C7 C72 46.4(4) . . . . ? P7 N7 C7 C72 -179.5(2) . . . . ? P8 N7 C7 C73 165.2(3) . . . . ? P7 N7 C7 C73 -60.7(4) . . . . ? P8 N7 C7 C71 -74.9(4) . . . . ? P7 N7 C7 C71 59.2(4) . . . . ? C7 N7 P8 N15 -102.9(3) . . . . ? P7 N7 P8 N15 113.90(14) . . . . ? C7 N7 P8 N8 152.0(3) . . . . ? P7 N7 P8 N8 8.75(13) . . . . ? C7 N7 P8 P7 143.2(3) . . . . ? N14 P7 P8 N15 1.81(18) . . . . ? N8 P7 P8 N15 85.28(18) . . . . ? N7 P7 P8 N15 -81.34(18) . . . . ? N14 P7 P8 N8 -83.47(19) . . . . ? N7 P7 P8 N8 -166.6(2) . . . . ? N14 P7 P8 N7 83.15(19) . . . . ? N8 P7 P8 N7 166.6(2) . . . . ? N14 P7 N8 C8 -89.2(3) . . . . ? N7 P7 N8 C8 168.6(3) . . . . ? P8 P7 N8 C8 159.8(4) . . . . ? N14 P7 N8 P8 110.97(16) . . . . ? N7 P7 N8 P8 8.83(13) . . . . ? N15 P8 N8 C8 89.7(3) . . . . ? N7 P8 N8 C8 -168.1(3) . . . . ? P7 P8 N8 C8 -159.2(4) . . . . ? N15 P8 N8 P7 -111.07(15) . . . . ? N7 P8 N8 P7 -8.84(13) . . . . ? P7 N8 C8 C82 -162.6(4) . . . . ? P8 N8 C8 C82 -9.0(6) . . . . ? P7 N8 C8 C83 -40.8(4) . . . . ? P8 N8 C8 C83 112.9(4) . . . . ? P7 N8 C8 C81 74.6(5) . . . . ? P8 N8 C8 C81 -131.8(4) . . . . ? N8 P8 N15 C44 36.1(3) . . . . ? N7 P8 N15 C44 -48.4(3) . . . . ? P7 P8 N15 C44 -6.4(3) . . . . ? P8 N15 C44 C45 -108.2(4) . . . . ? P8 N15 C44 C49 71.8(4) . . . . ? C49 C44 C45 C46 -0.5(5) . . . . ? N15 C44 C45 C46 179.5(3) . . . . ? C44 C45 C46 C47 -0.9(6) . . . . ? C45 C46 C47 C48 1.4(5) . . . . ? C45 C46 C47 N16 180.0(3) . . . . ? C46 C47 C48 C49 -0.6(5) . . . . ? N16 C47 C48 C49 -179.2(3) . . . . ? C47 C48 C49 C44 -0.8(5) . . . . ? C45 C44 C49 C48 1.4(5) . . . . ? N15 C44 C49 C48 -178.7(3) . . . . ? C48 C47 N16 P1 178.4(3) . . . . ? C46 C47 N16 P1 -0.1(5) . . . . ? N1 P1 N16 C47 -128.1(3) . . . . ? N2 P1 N16 C47 147.8(3) . . . . ? P2 P1 N16 C47 -170.4(3) . . . . ? C1P C2P C3P C4P 174.7(8) . . . . ? C2P C3P C4P C5P 52.0(17) . . . . ? C1T C2T C3T C4T 109(4) . . . . ? C2T C3T C4T C5T 174(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.674 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.054