Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _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_section_title ; Targeting Large Phosph(III)azane Macrocyles [{P(mu-NR)}2(LL)]n (n ? 2); Emerging Host-Guest Behaviour ; loop_ _publ_author_name D.S.Wright 'Fay Dodds' 'Felipe Garcia' 'Richard A. Kowenicki' M.McPartlin ; S.P.Parsons ; 'Alexander Steiner' # Attachment '2a.cif' data_dw0537 _database_code_depnum_ccdc_archive 'CCDC 608772' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H112 N6 O8 P6' _chemical_formula_weight 1459.57 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 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 13.205(3) _cell_length_b 33.184(7) _cell_length_c 18.385(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.98(3) _cell_angle_gamma 90.00 _cell_volume 7850(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 126738 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3128 _exptl_absorpt_coefficient_mu 0.194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.906 _exptl_absorpt_correction_T_max 0.971 _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_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 49553 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 21.05 _reflns_number_total 8441 _reflns_number_gt 6874 _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^)+(0.0954P)^2^+22.4642P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8441 _refine_ls_number_parameters 886 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.1975 _refine_ls_wR_factor_gt 0.1876 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.008 _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 0.60575(12) 0.77713(4) 0.85019(9) 0.0495(4) Uani 1 1 d . . . P2 P 0.48144(12) 0.73520(4) 0.89278(8) 0.0464(4) Uani 1 1 d . . . P3 P 0.24518(13) 0.49284(5) 0.88937(9) 0.0527(5) Uani 1 1 d . . . P4 P 0.17666(12) 0.49580(4) 0.74777(9) 0.0483(4) Uani 1 1 d . . . P5 P 0.35862(13) 0.56451(5) 0.40047(9) 0.0557(5) Uani 1 1 d . . . P6 P 0.41473(12) 0.63660(5) 0.44949(8) 0.0491(4) Uani 1 1 d . . . N1 N 0.6224(3) 0.74188(13) 0.9162(2) 0.0437(11) Uani 1 1 d . . . N2 N 0.4682(4) 0.76163(13) 0.8167(3) 0.0487(12) Uani 1 1 d . . . N3 N 0.2824(4) 0.47439(13) 0.8234(3) 0.0554(14) Uani 1 1 d . . . N4 N 0.1561(3) 0.52125(13) 0.8150(2) 0.0454(12) Uani 1 1 d . . . N5 N 0.4780(3) 0.59058(13) 0.4560(2) 0.0464(12) Uani 1 1 d . . . N6 N 0.2962(4) 0.60814(15) 0.4091(2) 0.0567(13) Uani 1 1 d . . . O1 O 0.6562(3) 0.75702(11) 0.7959(2) 0.0550(10) Uiso 1 1 d . . . O2 O 0.4572(3) 0.68796(10) 0.8615(2) 0.0500(10) Uani 1 1 d . . . O3 O 0.3467(3) 0.52337(12) 0.9433(2) 0.0580(11) Uani 1 1 d . . . O4 O 0.2412(3) 0.53055(10) 0.7205(2) 0.0493(10) Uani 1 1 d . . . O5 O 0.3447(3) 0.53054(12) 0.4555(2) 0.0624(12) Uani 1 1 d . . . O6 O 0.4288(3) 0.64330(11) 0.53515(19) 0.0515(10) Uani 1 1 d . . . C20 C 0.3974(4) 0.66172(16) 0.8854(3) 0.0434(14) Uani 1 1 d . . . C21 C 0.3110(5) 0.67387(17) 0.8997(3) 0.0499(15) Uani 1 1 d . . . H21 H 0.2900 0.7007 0.8945 0.060 Uiso 1 1 calc R . . C22 C 0.2540(5) 0.64530(19) 0.9225(3) 0.0547(16) Uani 1 1 d . . . H22 H 0.1926 0.6529 0.9354 0.066 Uiso 1 1 calc R . . C23 C 0.2807(5) 0.60598(19) 0.9279(3) 0.0516(15) Uani 1 1 d . . . H23 H 0.2360 0.5877 0.9428 0.062 Uiso 1 1 calc R . . C24 C 0.3700(4) 0.59214(17) 0.9126(3) 0.0426(14) Uani 1 1 d . . . C25 C 0.4305(4) 0.62069(16) 0.8919(3) 0.0408(14) Uani 1 1 d . . . C26 C 0.5223(4) 0.60744(18) 0.8789(3) 0.0494(15) Uani 1 1 d . . . H26 H 0.5657 0.6259 0.8631 0.059 Uiso 1 1 calc R . . C27 C 0.5538(5) 0.56794(18) 0.8881(3) 0.0540(16) Uani 1 1 d . . . H27 H 0.6180 0.5606 0.8793 0.065 Uiso 1 1 calc R . . C28 C 0.4936(5) 0.53950(18) 0.9097(3) 0.0502(15) Uani 1 1 d . . . H28 H 0.5153 0.5129 0.9173 0.060 Uiso 1 1 calc R . . C29 C 0.4034(5) 0.55136(17) 0.9194(3) 0.0458(14) Uani 1 1 d . . . C40 C 0.2119(4) 0.53350(15) 0.6448(3) 0.0435(14) Uani 1 1 d . . . C41 C 0.1039(4) 0.53668(16) 0.5914(3) 0.0493(15) Uani 1 1 d . . . H41 H 0.0477 0.5374 0.6141 0.059 Uiso 1 1 calc R . . C42 C 0.0801(5) 0.53851(17) 0.5159(3) 0.0532(15) Uani 1 1 d . . . H42 H 0.0141 0.5408 0.4851 0.064 Uiso 1 1 calc R . . C43 C 0.1653(4) 0.53649(17) 0.4958(3) 0.0503(15) Uani 1 1 d . . . H43 H 0.1619 0.5359 0.4447 0.060 Uiso 1 1 calc R . . C44 C 0.2791(4) 0.53484(15) 0.5502(3) 0.0423(14) Uani 1 1 d . . . C45 C 0.3061(4) 0.53350(14) 0.6270(3) 0.0399(13) Uani 1 1 d . . . C46 C 0.4200(5) 0.53216(16) 0.6819(3) 0.0491(15) Uani 1 1 d . . . H46 H 0.4236 0.5318 0.7330 0.059 Uiso 1 1 calc R . . C47 C 0.5041(5) 0.53158(17) 0.6610(4) 0.0547(16) Uani 1 1 d . . . H47 H 0.5705 0.5311 0.6918 0.066 Uiso 1 1 calc R . . C48 C 0.4805(5) 0.53182(18) 0.5857(4) 0.0586(17) Uani 1 1 d . . . H48 H 0.5368 0.5309 0.5630 0.070 Uiso 1 1 calc R . . C49 C 0.3717(5) 0.53348(16) 0.5320(3) 0.0501(16) Uani 1 1 d . . . C60 C 0.4540(4) 0.68115(16) 0.5684(3) 0.0412(14) Uani 1 1 d . . . C61 C 0.4067(5) 0.71556(17) 0.5302(3) 0.0494(15) Uani 1 1 d . . . H61 H 0.3601 0.7141 0.4842 0.059 Uiso 1 1 calc R . . C62 C 0.4358(5) 0.75275(18) 0.5676(3) 0.0544(17) Uani 1 1 d . . . H62 H 0.4084 0.7766 0.5448 0.065 Uiso 1 1 calc R . . C63 C 0.5084(5) 0.75454(17) 0.6416(3) 0.0516(16) Uani 1 1 d . . . H63 H 0.5257 0.7798 0.6629 0.062 Uiso 1 1 calc R . . C64 C 0.5544(4) 0.71929(16) 0.6832(3) 0.0411(14) Uani 1 1 d . . . C65 C 0.5282(4) 0.68137(16) 0.6455(3) 0.0404(14) Uani 1 1 d . . . C66 C 0.5755(4) 0.64586(17) 0.6873(3) 0.0472(15) Uani 1 1 d . . . H66 H 0.5606 0.6207 0.6652 0.057 Uiso 1 1 calc R . . C67 C 0.6448(5) 0.64773(18) 0.7617(3) 0.0525(16) Uani 1 1 d . . . H67 H 0.6722 0.6240 0.7850 0.063 Uiso 1 1 calc R . . C68 C 0.6708(5) 0.68478(18) 0.7987(3) 0.0519(15) Uani 1 1 d . . . H68 H 0.7148 0.6862 0.8459 0.062 Uiso 1 1 calc R . . C69 C 0.6268(4) 0.71938(17) 0.7605(3) 0.0452(14) Uani 1 1 d . . . C1 C 0.7166(4) 0.73783(17) 0.9914(3) 0.0506(15) Uani 1 1 d . . . H1 H 0.7817 0.7392 0.9743 0.061 Uiso 1 1 calc R . . C101 C 0.7206(5) 0.77074(19) 1.0443(3) 0.0650(18) Uani 1 1 d . . . H10A H 0.6544 0.7725 1.0587 0.078 Uiso 1 1 calc R . . H10B H 0.7312 0.7959 1.0202 0.078 Uiso 1 1 calc R . . C102 C 0.8180(6) 0.7647(2) 1.1230(4) 0.082(2) Uani 1 1 d . . . H10C H 0.8851 0.7690 1.1111 0.098 Uiso 1 1 calc R . . H10D H 0.8099 0.7842 1.1607 0.098 Uiso 1 1 calc R . . C103 C 0.8121(6) 0.7231(2) 1.1517(4) 0.081(2) Uani 1 1 d . . . H10E H 0.8711 0.7191 1.1932 0.097 Uiso 1 1 calc R . . H10F H 0.7498 0.7211 1.1712 0.097 Uiso 1 1 calc R . . C104 C 0.8107(6) 0.6908(2) 1.0994(4) 0.0729(19) Uani 1 1 d . . . H10G H 0.8020 0.6654 1.1232 0.087 Uiso 1 1 calc R . . H10H H 0.8765 0.6901 1.0843 0.087 Uiso 1 1 calc R . . C105 C 0.7124(5) 0.69691(18) 1.0227(3) 0.0621(17) Uani 1 1 d . . . H10I H 0.7184 0.6769 0.9854 0.075 Uiso 1 1 calc R . . H10J H 0.6461 0.6930 1.0362 0.075 Uiso 1 1 calc R . . C2 C 0.3655(5) 0.77651(19) 0.7530(4) 0.0627(17) Uani 1 1 d . . . H2 H 0.3769 0.7655 0.7060 0.075 Uiso 1 1 calc R . . C201 C 0.2588(6) 0.7637(3) 0.7549(6) 0.128(4) Uani 1 1 d . . . H20A H 0.2451 0.7734 0.8015 0.153 Uiso 1 1 calc R . . H20B H 0.2592 0.7345 0.7575 0.153 Uiso 1 1 calc R . . C202 C 0.1545(6) 0.7772(3) 0.6854(6) 0.123(4) Uani 1 1 d . . . H20C H 0.1566 0.7625 0.6401 0.147 Uiso 1 1 calc R . . H20D H 0.0906 0.7701 0.7000 0.147 Uiso 1 1 calc R . . C203 C 0.1560(6) 0.8203(3) 0.6712(5) 0.100(3) Uani 1 1 d . . . H20E H 0.1126 0.8261 0.6223 0.120 Uiso 1 1 calc R . . H20F H 0.1277 0.8347 0.7081 0.120 Uiso 1 1 calc R . . C204 C 0.2607(6) 0.8342(3) 0.6742(6) 0.120(4) Uani 1 1 d . . . H20G H 0.2584 0.8634 0.6751 0.144 Uiso 1 1 calc R . . H20H H 0.2769 0.8267 0.6271 0.144 Uiso 1 1 calc R . . C205 C 0.3653(6) 0.82013(19) 0.7426(4) 0.077(2) Uani 1 1 d . . . H20I H 0.4290 0.8283 0.7289 0.092 Uiso 1 1 calc R . . H20J H 0.3622 0.8334 0.7890 0.092 Uiso 1 1 calc R . . C3 C 0.3342(5) 0.43490(17) 0.8217(4) 0.0607(17) Uani 1 1 d . . . H3 H 0.2901 0.4175 0.7845 0.073 Uiso 1 1 calc R . . C301 C 0.3683(6) 0.41231(19) 0.8921(4) 0.079(2) Uani 1 1 d . . . H30A H 0.3067 0.4064 0.9107 0.094 Uiso 1 1 calc R . . H30B H 0.4109 0.4304 0.9279 0.094 Uiso 1 1 calc R . . C302 C 0.4289(6) 0.37281(18) 0.8935(4) 0.071(2) Uani 1 1 d . . . H30C H 0.4421 0.3615 0.9434 0.085 Uiso 1 1 calc R . . H30D H 0.3869 0.3537 0.8598 0.085 Uiso 1 1 calc R . . C303 C 0.5245(6) 0.3784(2) 0.8725(4) 0.084(2) Uani 1 1 d . . . H30E H 0.5566 0.3529 0.8649 0.101 Uiso 1 1 calc R . . H30F H 0.5727 0.3943 0.9089 0.101 Uiso 1 1 calc R . . C304 C 0.4881(6) 0.4006(2) 0.8011(4) 0.076(2) Uani 1 1 d . . . H30G H 0.4421 0.3828 0.7669 0.091 Uiso 1 1 calc R . . H30H H 0.5482 0.4054 0.7801 0.091 Uiso 1 1 calc R . . C305 C 0.4317(5) 0.44091(17) 0.8014(3) 0.0574(17) Uani 1 1 d . . . H30I H 0.4745 0.4591 0.8366 0.069 Uiso 1 1 calc R . . H30J H 0.4199 0.4530 0.7522 0.069 Uiso 1 1 calc R . . C4 C 0.0495(4) 0.53861(16) 0.8072(3) 0.0474(15) Uani 1 1 d . . . H4 H 0.0448 0.5466 0.8577 0.057 Uiso 1 1 calc R . . C401 C -0.0473(4) 0.50796(17) 0.7776(4) 0.0564(17) Uani 1 1 d . . . H40A H -0.0414 0.4973 0.7295 0.068 Uiso 1 1 calc R . . H40B H -0.0407 0.4854 0.8119 0.068 Uiso 1 1 calc R . . C402 C -0.1585(5) 0.5264(2) 0.7687(4) 0.0675(19) Uani 1 1 d . . . H40C H -0.2084 0.5052 0.7503 0.081 Uiso 1 1 calc R . . H40D H -0.1669 0.5335 0.8182 0.081 Uiso 1 1 calc R . . C403 C -0.1888(5) 0.5630(2) 0.7189(4) 0.0672(19) Uani 1 1 d . . . H40E H -0.2544 0.5742 0.7247 0.081 Uiso 1 1 calc R . . H40F H -0.1941 0.5562 0.6668 0.081 Uiso 1 1 calc R . . C404 C -0.0939(5) 0.59383(18) 0.7490(4) 0.0628(18) Uani 1 1 d . . . H40G H -0.1009 0.6164 0.7148 0.075 Uiso 1 1 calc R . . H40H H -0.1005 0.6042 0.7970 0.075 Uiso 1 1 calc R . . C405 C 0.0173(5) 0.57589(16) 0.7580(3) 0.0505(15) Uani 1 1 d . . . H40I H 0.0263 0.5693 0.7084 0.061 Uiso 1 1 calc R . . H40J H 0.0664 0.5972 0.7771 0.061 Uiso 1 1 calc R . . C5 C 0.5950(4) 0.58342(17) 0.4676(3) 0.0478(15) Uani 1 1 d . . . H5 H 0.6090 0.5552 0.4821 0.057 Uiso 1 1 calc R . . C501 C 0.6062(5) 0.5877(2) 0.3957(3) 0.0661(19) Uani 1 1 d U . . H50A H 0.5849 0.6142 0.3758 0.079 Uiso 1 1 calc R . . H50B H 0.5682 0.5672 0.3629 0.079 Uiso 1 1 calc R . . C502 C 0.7284(5) 0.5816(2) 0.4092(4) 0.072(2) Uani 1 1 d . . . H50C H 0.7433 0.5540 0.4256 0.086 Uiso 1 1 calc R . . H50D H 0.7466 0.5841 0.3611 0.086 Uiso 1 1 calc R . . C503 C 0.8065(5) 0.61046(19) 0.4672(4) 0.0630(18) Uani 1 1 d . . . H50E H 0.8775 0.6044 0.4648 0.076 Uiso 1 1 calc R . . H50F H 0.7927 0.6383 0.4523 0.076 Uiso 1 1 calc R . . C504 C 0.7967(5) 0.6060(3) 0.5381(4) 0.079(2) Uani 1 1 d . . . H50G H 0.8343 0.6267 0.5706 0.095 Uiso 1 1 calc R . . H50H H 0.8197 0.5796 0.5578 0.095 Uiso 1 1 calc R . . C505 C 0.6747(5) 0.6112(2) 0.5263(3) 0.0658(18) Uani 1 1 d . . . H50I H 0.6587 0.6390 0.5121 0.079 Uiso 1 1 calc R . . H50J H 0.6582 0.6074 0.5747 0.079 Uiso 1 1 calc R . . C6 C 0.1806(5) 0.6249(2) 0.3633(3) 0.0607(17) Uani 1 1 d . . . H6 H 0.1942 0.6485 0.3348 0.073 Uiso 1 1 calc R . . C601 C 0.1068(5) 0.5959(2) 0.3049(3) 0.0634(17) Uani 1 1 d . . . H60A H 0.0966 0.5715 0.3314 0.076 Uiso 1 1 calc R . . H60B H 0.1447 0.5883 0.2676 0.076 Uiso 1 1 calc R . . C602 C -0.0126(5) 0.6122(2) 0.2588(4) 0.0672(18) Uani 1 1 d . . . H60C H -0.0054 0.6336 0.2245 0.081 Uiso 1 1 calc R . . H60D H -0.0509 0.5903 0.2304 0.081 Uiso 1 1 calc R . . C603 C -0.0643(6) 0.6260(2) 0.3101(4) 0.082(2) Uani 1 1 d . . . H60E H -0.0845 0.6034 0.3373 0.099 Uiso 1 1 calc R . . H60F H -0.1268 0.6400 0.2850 0.099 Uiso 1 1 calc R . . C604 C 0.0088(5) 0.6557(2) 0.3665(4) 0.078(2) Uani 1 1 d . . . H60G H -0.0286 0.6640 0.4038 0.093 Uiso 1 1 calc R . . H60H H 0.0195 0.6796 0.3389 0.093 Uiso 1 1 calc R . . C605 C 0.1281(5) 0.63846(19) 0.4122(3) 0.0588(17) Uani 1 1 d . . . H60I H 0.1667 0.6601 0.4415 0.071 Uiso 1 1 calc R . . H60J H 0.1196 0.6169 0.4461 0.071 Uiso 1 1 calc R . . O1T O 0.1341(5) 0.74423(17) 0.8977(4) 0.1038(18) Uani 1 1 d . . . C1T C 0.0478(7) 0.7268(3) 0.8340(5) 0.104(3) Uani 1 1 d . . . H1T1 H 0.0297 0.7474 0.7958 0.125 Uiso 1 1 calc R . . H1T2 H 0.0773 0.7044 0.8120 0.125 Uiso 1 1 calc R . . C2T C -0.0412(9) 0.7139(5) 0.8511(8) 0.176(6) Uani 1 1 d . . . H2T1 H -0.0507 0.6850 0.8455 0.211 Uiso 1 1 calc R . . H2T2 H -0.1021 0.7280 0.8233 0.211 Uiso 1 1 calc R . . C3T C -0.0123(11) 0.7262(5) 0.9272(9) 0.182(6) Uani 1 1 d . . . H3T1 H -0.0230 0.7036 0.9580 0.219 Uiso 1 1 calc R . . H3T2 H -0.0593 0.7475 0.9348 0.219 Uiso 1 1 calc R . . C4T C 0.1050(9) 0.7421(3) 0.9571(6) 0.120(4) Uani 1 1 d U . . H4T1 H 0.1066 0.7683 0.9809 0.144 Uiso 1 1 calc R . . H4T2 H 0.1465 0.7232 0.9915 0.144 Uiso 1 1 calc R . . O1S O 0.0922(7) 0.6560(4) 0.6494(7) 0.220(5) Uani 1 1 d . . . C1S C 0.1980(11) 0.6417(4) 0.7028(6) 0.137(4) Uani 1 1 d D . . H1S1 H 0.2072 0.6560 0.7499 0.165 Uiso 1 1 calc R . . H1S2 H 0.1929 0.6132 0.7131 0.165 Uiso 1 1 calc R . . C2S C 0.2751(11) 0.6473(4) 0.6769(10) 0.166(5) Uani 1 1 d U . . H2S1 H 0.3243 0.6656 0.7073 0.199 Uiso 1 1 calc R . . H2S2 H 0.3097 0.6223 0.6699 0.199 Uiso 1 1 calc R . . C3S C 0.2245(14) 0.6650(6) 0.6077(8) 0.201(7) Uani 1 1 d DU . . H3S1 H 0.2404 0.6483 0.5684 0.242 Uiso 1 1 calc R . . H3S2 H 0.2574 0.6909 0.6046 0.242 Uiso 1 1 calc R . . C4S C 0.1125(14) 0.6719(5) 0.5892(7) 0.191(7) Uani 1 1 d . . . H4S1 H 0.0951 0.7003 0.5844 0.229 Uiso 1 1 calc R . . H4S2 H 0.0781 0.6576 0.5444 0.229 Uiso 1 1 calc R . . C1P C 0.8782(12) 0.6074(5) 0.9720(9) 0.204(7) Uani 1 1 d . . . H1P1 H 0.8145 0.6068 0.9888 0.306 Uiso 1 1 calc R . . H1P2 H 0.8670 0.5958 0.9230 0.306 Uiso 1 1 calc R . . H1P3 H 0.9011 0.6348 0.9703 0.306 Uiso 1 1 calc R . . C2P C 0.9509(15) 0.5862(5) 1.0191(10) 0.216(8) Uani 1 1 d . B . H2P1 H 0.9129 0.5614 1.0217 0.260 Uiso 1 1 calc R . . H2P2 H 0.9499 0.5999 1.0656 0.260 Uiso 1 1 calc R . . C3P C 1.0553(10) 0.5710(4) 1.0361(9) 0.165(5) Uani 1 1 d . . . H3P1 H 1.0509 0.5534 0.9934 0.198 Uiso 0.60 1 calc PR A 1 H3P2 H 1.0907 0.5948 1.0234 0.198 Uiso 0.60 1 calc PR A 1 H3P3 H 1.0847 0.5841 0.9983 0.198 Uiso 0.40 1 calc PR A 2 H3P4 H 1.0854 0.5852 1.0820 0.198 Uiso 0.40 1 calc PR A 2 C4P C 1.1475(19) 0.5508(7) 1.0905(13) 0.154(8) Uiso 0.60 1 d P B 1 H4P1 H 1.1731 0.5725 1.1250 0.185 Uiso 0.60 1 calc PR B 1 H4P2 H 1.1123 0.5327 1.1181 0.185 Uiso 0.60 1 calc PR B 1 C4P' C 1.101(4) 0.5404(13) 1.044(3) 0.189(16) Uiso 0.40 1 d P B 2 H4P3 H 1.0922 0.5293 0.9946 0.227 Uiso 0.40 1 calc PR B 2 H4P4 H 1.0608 0.5231 1.0699 0.227 Uiso 0.40 1 calc PR B 2 C5P C 1.2369(10) 0.5299(4) 1.0898(7) 0.165(5) Uani 1 1 d . . . H5P1 H 1.2791 0.5284 1.1396 0.198 Uiso 0.60 1 calc PR B 1 H5P2 H 1.2747 0.5435 1.0581 0.198 Uiso 0.60 1 calc PR B 1 H5P3 H 1.2196 0.5032 1.0711 0.198 Uiso 0.60 1 calc PR B 1 H5P4 H 1.2404 0.5061 1.1198 0.198 Uiso 0.40 1 calc PR B 2 H5P5 H 1.2651 0.5523 1.1209 0.198 Uiso 0.40 1 calc PR B 2 H5P6 H 1.2763 0.5259 1.0524 0.198 Uiso 0.40 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0602(10) 0.0436(9) 0.0482(9) -0.0086(7) 0.0200(8) -0.0075(7) P2 0.0513(9) 0.0454(9) 0.0480(9) -0.0122(7) 0.0227(7) -0.0001(7) P3 0.0676(11) 0.0463(9) 0.0563(10) 0.0143(8) 0.0398(9) 0.0079(8) P4 0.0593(10) 0.0418(9) 0.0566(10) 0.0004(7) 0.0403(8) -0.0036(7) P5 0.0621(11) 0.0712(11) 0.0456(9) -0.0184(8) 0.0371(8) -0.0122(9) P6 0.0607(10) 0.0585(10) 0.0356(9) -0.0018(7) 0.0269(7) 0.0069(8) N1 0.052(3) 0.046(3) 0.039(3) -0.008(2) 0.024(2) -0.004(2) N2 0.056(3) 0.039(3) 0.054(3) -0.007(2) 0.019(2) 0.000(2) N3 0.079(4) 0.042(3) 0.065(3) 0.009(2) 0.058(3) 0.007(3) N4 0.056(3) 0.047(3) 0.046(3) 0.003(2) 0.039(2) 0.002(2) N5 0.058(3) 0.055(3) 0.038(3) -0.008(2) 0.037(2) -0.001(2) N6 0.063(3) 0.076(3) 0.040(3) -0.012(2) 0.031(2) 0.011(3) O2 0.068(3) 0.041(2) 0.055(2) -0.0107(18) 0.042(2) -0.001(2) O3 0.080(3) 0.059(3) 0.047(2) 0.020(2) 0.038(2) 0.014(2) O4 0.062(3) 0.047(2) 0.053(3) -0.0003(19) 0.042(2) -0.0099(19) O5 0.076(3) 0.059(3) 0.070(3) -0.033(2) 0.055(2) -0.014(2) O6 0.078(3) 0.052(2) 0.037(2) -0.0007(19) 0.040(2) 0.004(2) C20 0.053(4) 0.044(4) 0.040(3) -0.003(3) 0.025(3) -0.005(3) C21 0.057(4) 0.046(4) 0.056(4) -0.005(3) 0.035(3) 0.011(3) C22 0.058(4) 0.060(4) 0.060(4) -0.002(3) 0.043(3) 0.005(3) C23 0.057(4) 0.062(4) 0.047(4) 0.007(3) 0.034(3) 0.003(3) C24 0.044(3) 0.055(4) 0.035(3) 0.000(3) 0.021(3) 0.001(3) C25 0.043(3) 0.048(4) 0.036(3) -0.006(3) 0.020(3) 0.002(3) C26 0.048(4) 0.055(4) 0.054(4) -0.007(3) 0.031(3) -0.002(3) C27 0.048(4) 0.058(4) 0.066(4) -0.004(3) 0.033(3) 0.006(3) C28 0.051(4) 0.050(4) 0.055(4) 0.005(3) 0.022(3) 0.014(3) C29 0.055(4) 0.050(4) 0.038(3) 0.011(3) 0.021(3) 0.008(3) C40 0.063(4) 0.039(3) 0.041(4) -0.001(3) 0.037(3) -0.005(3) C41 0.051(4) 0.053(4) 0.057(4) 0.002(3) 0.039(3) -0.001(3) C42 0.054(4) 0.059(4) 0.052(4) 0.005(3) 0.024(3) -0.005(3) C43 0.053(4) 0.059(4) 0.051(4) -0.007(3) 0.038(3) -0.012(3) C44 0.054(4) 0.035(3) 0.050(4) -0.011(3) 0.039(3) -0.008(3) C45 0.045(3) 0.033(3) 0.053(4) -0.002(3) 0.033(3) -0.004(2) C46 0.060(4) 0.043(3) 0.057(4) 0.004(3) 0.038(3) -0.003(3) C47 0.044(4) 0.064(4) 0.068(5) 0.007(3) 0.036(3) 0.000(3) C48 0.060(4) 0.061(4) 0.072(5) -0.004(3) 0.051(4) 0.000(3) C49 0.067(4) 0.044(3) 0.055(4) -0.015(3) 0.047(4) -0.012(3) C60 0.054(4) 0.046(4) 0.035(3) -0.001(3) 0.034(3) 0.002(3) C61 0.064(4) 0.059(4) 0.035(3) 0.004(3) 0.032(3) 0.006(3) C62 0.083(5) 0.047(4) 0.046(4) 0.012(3) 0.043(4) 0.013(3) C63 0.076(4) 0.043(3) 0.049(4) -0.001(3) 0.043(3) -0.008(3) C64 0.051(3) 0.045(3) 0.040(3) -0.001(3) 0.037(3) -0.003(3) C65 0.045(3) 0.046(3) 0.042(3) 0.005(3) 0.035(3) 0.007(3) C66 0.064(4) 0.047(3) 0.044(4) 0.001(3) 0.039(3) 0.011(3) C67 0.070(4) 0.054(4) 0.043(4) 0.008(3) 0.034(3) 0.021(3) C68 0.062(4) 0.064(4) 0.036(3) 0.002(3) 0.025(3) 0.010(3) C69 0.050(3) 0.052(4) 0.042(3) -0.007(3) 0.030(3) -0.008(3) C1 0.053(4) 0.059(4) 0.047(3) -0.008(3) 0.026(3) 0.001(3) C101 0.086(5) 0.061(4) 0.053(4) -0.015(3) 0.026(4) -0.004(4) C102 0.097(6) 0.092(6) 0.055(4) -0.020(4) 0.014(4) -0.009(4) C103 0.079(5) 0.110(6) 0.052(4) 0.007(4) 0.012(4) -0.002(4) C104 0.084(5) 0.077(5) 0.061(4) 0.011(4) 0.025(4) 0.010(4) C105 0.084(5) 0.053(4) 0.058(4) 0.000(3) 0.034(4) 0.004(3) C2 0.067(4) 0.069(4) 0.055(4) -0.005(3) 0.020(3) 0.004(3) C201 0.061(5) 0.126(8) 0.189(10) 0.089(7) 0.014(6) -0.008(5) C202 0.065(5) 0.139(9) 0.154(9) 0.057(7) 0.006(5) -0.014(5) C203 0.086(6) 0.125(7) 0.097(6) 0.043(5) 0.039(5) 0.041(5) C204 0.073(6) 0.109(7) 0.168(9) 0.081(7) 0.007(6) -0.014(5) C205 0.079(5) 0.056(4) 0.096(6) 0.024(4) 0.019(4) -0.009(4) C3 0.083(5) 0.047(4) 0.064(4) -0.001(3) 0.043(4) 0.006(3) C301 0.126(6) 0.049(4) 0.086(5) 0.025(4) 0.074(5) 0.028(4) C302 0.114(6) 0.049(4) 0.069(5) 0.016(3) 0.060(4) 0.021(4) C303 0.117(6) 0.068(5) 0.086(5) 0.015(4) 0.060(5) 0.037(4) C304 0.102(5) 0.067(4) 0.078(5) 0.023(4) 0.060(4) 0.030(4) C305 0.087(5) 0.046(4) 0.057(4) 0.009(3) 0.052(4) 0.012(3) C4 0.062(4) 0.046(3) 0.050(3) 0.000(3) 0.045(3) 0.005(3) C401 0.064(4) 0.047(3) 0.075(4) 0.004(3) 0.052(3) -0.005(3) C402 0.056(4) 0.068(4) 0.094(5) 0.000(4) 0.049(4) 0.000(3) C403 0.061(4) 0.072(5) 0.079(5) -0.003(4) 0.038(4) 0.014(4) C404 0.084(5) 0.049(4) 0.070(4) 0.003(3) 0.047(4) 0.011(3) C405 0.071(4) 0.038(3) 0.056(4) 0.004(3) 0.043(3) 0.004(3) C5 0.059(4) 0.043(3) 0.055(4) 0.001(3) 0.040(3) 0.003(3) C501 0.068(4) 0.098(5) 0.046(4) -0.018(3) 0.042(3) -0.018(4) C502 0.076(5) 0.087(5) 0.072(5) -0.018(4) 0.061(4) -0.014(4) C503 0.061(4) 0.068(4) 0.077(5) 0.002(4) 0.052(4) -0.003(3) C504 0.062(5) 0.123(6) 0.060(5) -0.013(4) 0.027(4) -0.002(4) C505 0.063(4) 0.095(5) 0.050(4) -0.014(4) 0.034(3) -0.005(4) C6 0.063(4) 0.077(4) 0.051(4) -0.004(3) 0.030(3) -0.003(3) C601 0.072(4) 0.069(4) 0.056(4) -0.013(3) 0.029(3) -0.004(4) C602 0.073(5) 0.074(5) 0.053(4) -0.002(3) 0.011(4) -0.021(4) C603 0.073(5) 0.084(5) 0.100(6) -0.021(5) 0.039(5) -0.004(4) C604 0.072(5) 0.085(5) 0.087(5) -0.007(4) 0.041(4) 0.001(4) C605 0.064(4) 0.071(4) 0.052(4) -0.006(3) 0.034(3) -0.001(3) O1T 0.092(4) 0.102(4) 0.129(5) -0.017(4) 0.051(4) 0.008(3) C1T 0.088(6) 0.125(7) 0.101(7) 0.024(6) 0.025(6) 0.018(6) C2T 0.107(9) 0.285(18) 0.161(12) -0.031(12) 0.083(9) -0.058(10) C3T 0.162(13) 0.226(15) 0.208(16) -0.013(12) 0.143(12) -0.036(11) C4T 0.171(11) 0.111(7) 0.108(7) 0.003(6) 0.094(8) 0.022(7) O1S 0.128(7) 0.357(16) 0.193(10) 0.032(10) 0.073(7) -0.007(8) C1S 0.149(11) 0.172(11) 0.094(7) 0.017(7) 0.034(8) -0.054(9) C2S 0.158(10) 0.130(9) 0.241(14) -0.020(9) 0.112(11) 0.009(8) C3S 0.183(12) 0.342(16) 0.117(9) -0.017(10) 0.114(9) -0.077(12) C4S 0.225(17) 0.261(16) 0.101(9) 0.109(10) 0.068(10) 0.102(13) C1P 0.190(14) 0.203(16) 0.221(17) -0.007(13) 0.053(12) 0.087(13) C2P 0.232(19) 0.177(14) 0.26(2) 0.041(14) 0.098(16) 0.085(14) C3P 0.124(10) 0.140(11) 0.233(15) -0.009(10) 0.046(10) 0.033(8) C5P 0.167(11) 0.169(11) 0.205(13) 0.044(9) 0.138(10) 0.019(9) _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 O1 1.478(4) . ? P1 N1 1.664(5) . ? P1 N2 1.855(5) . ? P1 P2 2.413(2) . ? P2 N2 1.626(5) . ? P2 O2 1.676(4) . ? P2 N1 1.827(5) . ? P3 N3 1.535(5) . ? P3 O3 1.792(5) . ? P3 N4 1.850(5) . ? P3 P4 2.559(2) . ? P4 N4 1.570(4) . ? P4 O4 1.582(4) . ? P4 N3 1.875(6) . ? P5 O5 1.553(5) . ? P5 N6 1.691(5) . ? P5 N5 1.885(5) . ? P5 P6 2.605(2) . ? P6 O6 1.560(4) . ? P6 N5 1.732(5) . ? P6 N6 1.836(5) . ? N1 C1 1.645(7) . ? N2 C2 1.656(8) . ? N3 C3 1.482(7) . ? N4 C4 1.497(7) . ? N5 C5 1.530(7) . ? N6 C6 1.665(8) . ? O1 C69 1.421(6) . ? O2 C20 1.316(6) . ? O3 C29 1.328(7) . ? O4 C40 1.360(6) . ? O5 C49 1.375(7) . ? O6 C60 1.404(6) . ? C20 C21 1.292(7) . ? C20 C25 1.427(8) . ? C21 C22 1.335(8) . ? C22 C23 1.349(8) . ? C23 C24 1.353(7) . ? C24 C25 1.348(7) . ? C24 C29 1.420(8) . ? C25 C26 1.360(7) . ? C26 C27 1.374(8) . ? C27 C28 1.350(8) . ? C28 C29 1.304(7) . ? C40 C45 1.356(7) . ? C40 C41 1.542(8) . ? C41 C42 1.354(8) . ? C42 C43 1.263(7) . ? C43 C44 1.608(8) . ? C44 C49 1.339(7) . ? C44 C45 1.377(8) . ? C45 C46 1.614(8) . ? C46 C47 1.254(7) . ? C47 C48 1.350(8) . ? C48 C49 1.550(9) . ? C60 C61 1.411(8) . ? C60 C65 1.531(8) . ? C61 C62 1.423(8) . ? C62 C63 1.480(9) . ? C63 C64 1.454(8) . ? C64 C65 1.441(7) . ? C64 C69 1.524(8) . ? C65 C66 1.467(7) . ? C66 C67 1.467(8) . ? C67 C68 1.410(8) . ? C68 C69 1.402(8) . ? C1 C105 1.480(8) . ? C1 C101 1.456(8) . ? C101 C102 1.718(10) . ? C102 C103 1.486(10) . ? C103 C104 1.437(9) . ? C104 C105 1.700(9) . ? C2 C205 1.460(9) . ? C2 C201 1.480(10) . ? C201 C202 1.714(12) . ? C202 C203 1.456(12) . ? C203 C204 1.446(10) . ? C204 C205 1.710(10) . ? C3 C305 1.432(8) . ? C3 C301 1.477(9) . ? C301 C302 1.533(8) . ? C302 C303 1.413(10) . ? C303 C304 1.488(9) . ? C304 C305 1.532(8) . ? C4 C405 1.536(7) . ? C4 C401 1.629(8) . ? C401 C402 1.564(8) . ? C402 C403 1.519(9) . ? C403 C404 1.617(9) . ? C404 C405 1.558(8) . ? C5 C501 1.370(8) . ? C5 C505 1.616(8) . ? C501 C502 1.589(9) . ? C502 C503 1.621(9) . ? C503 C504 1.345(8) . ? C504 C505 1.585(9) . ? C6 C605 1.331(8) . ? C6 C601 1.601(9) . ? C601 C602 1.702(9) . ? C602 C603 1.361(9) . ? C603 C604 1.591(10) . ? C604 C605 1.709(9) . ? O1T C4T 1.237(9) . ? O1T C1T 1.551(10) . ? C1T C2T 1.352(12) . ? C2T C3T 1.424(16) . ? C3T C4T 1.611(16) . ? O1S C4S 1.306(13) . ? O1S C1S 1.589(14) . ? C1S C2S 1.233(14) . ? C2S C3S 1.424(18) . ? C3S C4S 1.459(18) . ? C1P C2P 1.339(18) . ? C2P C3P 1.435(18) . ? C3P C4P' 1.18(4) . ? C3P C4P 1.55(3) . ? C4P C5P 1.37(2) . ? C4P' C5P 1.83(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 P1 N1 99.8(2) . . ? O1 P1 N2 102.0(2) . . ? N1 P1 N2 90.3(2) . . ? O1 P1 P2 113.67(17) . . ? N1 P1 P2 49.15(16) . . ? N2 P1 P2 42.32(15) . . ? N2 P2 O2 103.6(2) . . ? N2 P2 N1 92.5(2) . . ? O2 P2 N1 107.5(2) . . ? N2 P2 P1 50.17(17) . . ? O2 P2 P1 121.31(14) . . ? N1 P2 P1 43.56(14) . . ? N3 P3 O3 109.3(2) . . ? N3 P3 N4 83.2(2) . . ? O3 P3 N4 113.2(2) . . ? N3 P3 P4 46.7(2) . . ? O3 P3 P4 126.25(14) . . ? N4 P3 P4 37.56(14) . . ? N4 P4 O4 93.4(2) . . ? N4 P4 N3 81.5(2) . . ? O4 P4 N3 98.4(2) . . ? N4 P4 P3 45.91(17) . . ? O4 P4 P3 104.98(17) . . ? N3 P4 P3 36.56(14) . . ? O5 P5 N6 115.4(2) . . ? O5 P5 N5 100.8(2) . . ? N6 P5 N5 85.5(2) . . ? O5 P5 P6 120.49(16) . . ? N6 P5 P6 44.58(18) . . ? N5 P5 P6 41.65(14) . . ? O6 P6 N5 96.3(2) . . ? O6 P6 N6 112.3(2) . . ? N5 P6 N6 85.9(2) . . ? O6 P6 P5 116.12(16) . . ? N5 P6 P5 46.31(16) . . ? N6 P6 P5 40.27(15) . . ? C1 N1 P1 128.4(3) . . ? C1 N1 P2 136.6(3) . . ? P1 N1 P2 87.3(2) . . ? P2 N2 C2 133.0(4) . . ? P2 N2 P1 87.5(2) . . ? C2 N2 P1 137.5(4) . . ? C3 N3 P3 126.9(4) . . ? C3 N3 P4 126.1(4) . . ? P3 N3 P4 96.8(2) . . ? C4 N4 P4 117.2(4) . . ? C4 N4 P3 134.0(3) . . ? P4 N4 P3 96.5(2) . . ? C5 N5 P6 127.1(4) . . ? C5 N5 P5 134.4(3) . . ? P6 N5 P5 92.0(2) . . ? C6 N6 P5 130.5(4) . . ? C6 N6 P6 129.3(4) . . ? P5 N6 P6 95.1(2) . . ? C69 O1 P1 126.0(3) . . ? C20 O2 P2 126.0(3) . . ? C29 O3 P3 128.2(3) . . ? C40 O4 P4 109.1(3) . . ? C49 O5 P5 125.0(3) . . ? C60 O6 P6 122.0(3) . . ? C21 C20 O2 119.1(5) . . ? C21 C20 C25 123.3(5) . . ? O2 C20 C25 117.6(5) . . ? C20 C21 C22 115.4(5) . . ? C21 C22 C23 123.6(5) . . ? C22 C23 C24 122.6(5) . . ? C25 C24 C23 114.8(5) . . ? C25 C24 C29 120.2(5) . . ? C23 C24 C29 125.0(5) . . ? C24 C25 C26 115.5(5) . . ? C24 C25 C20 120.3(5) . . ? C26 C25 C20 124.2(5) . . ? C25 C26 C27 123.0(5) . . ? C28 C27 C26 121.4(5) . . ? C29 C28 C27 116.5(6) . . ? C28 C29 O3 115.7(5) . . ? C28 C29 C24 123.4(5) . . ? O3 C29 C24 120.6(5) . . ? O4 C40 C45 100.5(5) . . ? O4 C40 C41 131.8(4) . . ? C45 C40 C41 127.8(5) . . ? C42 C41 C40 128.7(5) . . ? C43 C42 C41 106.3(6) . . ? C42 C43 C44 126.1(5) . . ? C49 C44 C45 102.3(5) . . ? C49 C44 C43 128.7(5) . . ? C45 C44 C43 129.0(4) . . ? C40 C45 C44 102.0(5) . . ? C40 C45 C46 128.7(5) . . ? C44 C45 C46 129.3(4) . . ? C47 C46 C45 125.0(6) . . ? C46 C47 C48 107.4(6) . . ? C47 C48 C49 128.3(5) . . ? C44 C49 O5 102.5(5) . . ? C44 C49 C48 127.6(5) . . ? O5 C49 C48 129.7(5) . . ? O6 C60 C61 118.2(5) . . ? O6 C60 C65 116.6(4) . . ? C61 C60 C65 125.2(5) . . ? C60 C61 C62 114.9(5) . . ? C61 C62 C63 121.9(5) . . ? C64 C63 C62 124.0(5) . . ? C65 C64 C63 115.0(5) . . ? C65 C64 C69 118.9(5) . . ? C63 C64 C69 126.1(5) . . ? C64 C65 C66 114.9(5) . . ? C64 C65 C60 119.0(5) . . ? C66 C65 C60 126.1(5) . . ? C67 C66 C65 123.9(5) . . ? C68 C67 C66 121.4(5) . . ? C69 C68 C67 116.4(5) . . ? C68 C69 O1 116.8(5) . . ? C68 C69 C64 124.6(5) . . ? O1 C69 C64 118.5(5) . . ? C105 C1 C101 115.3(5) . . ? C105 C1 N1 108.3(5) . . ? C101 C1 N1 114.0(5) . . ? C1 C101 C102 112.5(5) . . ? C103 C102 C101 108.6(6) . . ? C104 C103 C102 116.7(6) . . ? C103 C104 C105 111.1(6) . . ? C1 C105 C104 110.0(5) . . ? C205 C2 C201 108.3(6) . . ? C205 C2 N2 111.4(5) . . ? C201 C2 N2 122.0(6) . . ? C2 C201 C202 121.1(7) . . ? C203 C202 C201 110.5(8) . . ? C204 C203 C202 110.9(7) . . ? C203 C204 C205 123.3(7) . . ? C2 C205 C204 110.1(6) . . ? C305 C3 N3 109.2(5) . . ? C305 C3 C301 100.7(6) . . ? N3 C3 C301 118.8(5) . . ? C3 C301 C302 120.2(5) . . ? C303 C302 C301 112.2(6) . . ? C302 C303 C304 100.1(6) . . ? C303 C304 C305 119.4(6) . . ? C3 C305 C304 110.2(5) . . ? N4 C4 C405 119.8(4) . . ? N4 C4 C401 116.2(4) . . ? C405 C4 C401 102.3(5) . . ? C402 C401 C4 116.0(5) . . ? C403 C402 C401 119.3(5) . . ? C402 C403 C404 102.8(5) . . ? C405 C404 C403 115.7(5) . . ? C4 C405 C404 120.0(4) . . ? C501 C5 N5 100.0(5) . . ? C501 C5 C505 113.0(5) . . ? N5 C5 C505 119.4(4) . . ? C5 C501 C502 99.3(5) . . ? C503 C502 C501 120.1(5) . . ? C504 C503 C502 112.8(5) . . ? C503 C504 C505 99.9(6) . . ? C504 C505 C5 121.3(5) . . ? C605 C6 C601 109.0(5) . . ? C605 C6 N6 109.2(5) . . ? C601 C6 N6 119.2(5) . . ? C6 C601 C602 119.9(5) . . ? C603 C602 C601 108.4(6) . . ? C602 C603 C604 109.5(6) . . ? C603 C604 C605 118.1(6) . . ? C6 C605 C604 110.0(5) . . ? C4T O1T C1T 108.9(8) . . ? C2T C1T O1T 118.1(9) . . ? C1T C2T C3T 94.7(10) . . ? C2T C3T C4T 117.0(9) . . ? O1T C4T C3T 100.5(9) . . ? C4S O1S C1S 109.0(10) . . ? C2S C1S O1S 113.8(11) . . ? C3S C2S C1S 98.4(12) . . ? C2S C3S C4S 121.3(9) . . ? O1S C4S C3S 97.5(9) . . ? C1P C2P C3P 147.0(17) . . ? C4P' C3P C4P 40(2) . . ? C4P' C3P C2P 140(3) . . ? C4P C3P C2P 150.7(16) . . ? C5P C4P C3P 140(2) . . ? C3P C4P' C5P 130(4) . . ? C4P C5P C4P' 32.0(16) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 21.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.697 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.064 # Attachment '4.cif' data_dw0519 _database_code_depnum_ccdc_archive 'CCDC 608773' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H66 Li0 N6 O6 P6' _chemical_formula_weight 936.83 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' Li Li -0.0003 0.0001 '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 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 17.410(4) _cell_length_b 15.925(3) _cell_length_c 37.093(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.04(3) _cell_angle_gamma 90.00 _cell_volume 10126(4) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 81560 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 23.26 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 0.260 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.722 _exptl_absorpt_correction_T_max 0.991 _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_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 25649 _diffrn_reflns_av_R_equivalents 0.1583 _diffrn_reflns_av_sigmaI/netI 0.1222 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 19.00 _reflns_number_total 7235 _reflns_number_gt 5514 _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^)+(0.0000P)^2^+540.9540P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7235 _refine_ls_number_parameters 901 _refine_ls_number_restraints 1032 _refine_ls_R_factor_all 0.1980 _refine_ls_R_factor_gt 0.1687 _refine_ls_wR_factor_ref 0.3729 _refine_ls_wR_factor_gt 0.3619 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.021 _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 0.54471(12) 0.77790(17) 0.01657(7) 0.0216(15) Uani 1 1 d DU . . P2 P 0.67448(12) 0.72723(17) 0.05483(7) 0.0223(15) Uani 1 1 d DU . . P3 P 0.81320(16) 0.52755(16) -0.12140(6) 0.0256(16) Uani 1 1 d DU . . P4 P 0.77538(16) 0.46202(17) -0.18572(6) 0.0258(15) Uani 1 1 d DU . . P5 P 0.33636(12) 0.59242(16) -0.19306(7) 0.0311(17) Uani 1 1 d DU . . P6 P 0.24308(13) 0.69496(16) -0.16844(8) 0.0337(17) Uani 1 1 d DU . . O1 O 0.5377(4) 0.7537(5) -0.02798(13) 0.034(4) Uani 1 1 d DU . . O2 O 0.7352(2) 0.6736(4) 0.0349(2) 0.031(4) Uani 1 1 d DU . . O3 O 0.7454(3) 0.5907(4) -0.10970(17) 0.024(4) Uani 1 1 d DU . . O4 O 0.6872(3) 0.4766(5) -0.20954(16) 0.033(4) Uani 1 1 d DU . . O5 O 0.4106(2) 0.5582(4) -0.1619(2) 0.030(4) Uani 1 1 d DU . . O6 O 0.2610(4) 0.7313(4) -0.12590(17) 0.036(4) Uani 1 1 d DU . . N1 N 0.6390(3) 0.8064(3) 0.0253(2) 0.018(4) Uani 1 1 d DU . . N2 N 0.5816(3) 0.6877(4) 0.0386(2) 0.023(4) Uani 1 1 d DU . . N3 N 0.8068(4) 0.5560(4) -0.16682(15) 0.025(4) Uani 1 1 d DU . . N4 N 0.7641(5) 0.4434(4) -0.14129(15) 0.015(4) Uani 1 1 d DU . . N5 N 0.3297(3) 0.6967(3) -0.1847(2) 0.020(4) Uani 1 1 d DU . . N6 N 0.2624(3) 0.5886(3) -0.1681(2) 0.025(5) Uani 1 1 d DU . . C1 C 0.6714(10) 0.8936(12) 0.0267(5) 0.028(6) Uani 1 1 d DU . . C2 C 0.5410(9) 0.6287(11) 0.0583(4) 0.019(5) Uani 1 1 d DU . . C3 C 0.8536(11) 0.6199(13) -0.1812(5) 0.038(6) Uani 1 1 d DU . . C4 C 0.7516(11) 0.3636(13) -0.1254(5) 0.042(6) Uani 1 1 d DU . . C5 C 0.3578(10) 0.7648(12) -0.2068(5) 0.031(6) Uani 1 1 d DU . . C6 C 0.2068(11) 0.5231(13) -0.1680(5) 0.033(6) Uani 1 1 d DU . . C11 C 0.6582(16) 0.9401(17) 0.0619(6) 0.084(10) Uani 1 1 d DU . . H11A H 0.6833 0.9096 0.0830 0.127 Uiso 1 1 calc R . . H11B H 0.6033 0.9438 0.0622 0.127 Uiso 1 1 calc R . . H11C H 0.6799 0.9955 0.0621 0.127 Uiso 1 1 calc R . . C12 C 0.7572(14) 0.890(2) 0.0250(9) 0.108(12) Uani 1 1 d DU . . H12A H 0.7848 0.8641 0.0468 0.162 Uiso 1 1 calc R . . H12B H 0.7766 0.9458 0.0229 0.162 Uiso 1 1 calc R . . H12C H 0.7648 0.8575 0.0040 0.162 Uiso 1 1 calc R . . C13 C 0.6282(15) 0.9426(16) -0.0065(6) 0.078(9) Uani 1 1 d DU . . H13A H 0.6399 0.9182 -0.0286 0.117 Uiso 1 1 calc R . . H13B H 0.6448 1.0002 -0.0049 0.117 Uiso 1 1 calc R . . H13C H 0.5730 0.9399 -0.0068 0.117 Uiso 1 1 calc R . . C14 C 0.4683(6) 0.7475(8) -0.0514(3) 0.016(3) Uani 1 1 d GDU . . C15 C 0.4203(7) 0.8173(7) -0.0591(3) 0.034(4) Uani 1 1 d GDU . . H15 H 0.4346 0.8683 -0.0476 0.041 Uiso 1 1 calc R . . C16 C 0.3508(7) 0.8109(7) -0.0839(3) 0.031(4) Uani 1 1 d GDU . . H16 H 0.3187 0.8576 -0.0890 0.037 Uiso 1 1 calc R . . C17 C 0.3293(6) 0.7348(9) -0.1011(3) 0.025(4) Uani 1 1 d GDU . . C18 C 0.3774(7) 0.6650(7) -0.0934(3) 0.030(4) Uani 1 1 d GDU . . H18 H 0.3630 0.6140 -0.1049 0.036 Uiso 1 1 calc R . . C19 C 0.4468(7) 0.6714(7) -0.0686(3) 0.022(4) Uani 1 1 d GDU . . H19 H 0.4789 0.6247 -0.0634 0.027 Uiso 1 1 calc R . . C21 C 0.4639(12) 0.6042(15) 0.0340(6) 0.052(7) Uani 1 1 d DU . . H21A H 0.4330 0.6536 0.0276 0.078 Uiso 1 1 calc R . . H21B H 0.4360 0.5661 0.0471 0.078 Uiso 1 1 calc R . . H21C H 0.4744 0.5775 0.0122 0.078 Uiso 1 1 calc R . . C22 C 0.5926(12) 0.5523(12) 0.0669(5) 0.039(6) Uani 1 1 d DU . . H22A H 0.6028 0.5280 0.0446 0.059 Uiso 1 1 calc R . . H22B H 0.5667 0.5118 0.0798 0.059 Uiso 1 1 calc R . . H22C H 0.6409 0.5686 0.0819 0.059 Uiso 1 1 calc R . . C23 C 0.5241(14) 0.6691(14) 0.0950(5) 0.051(7) Uani 1 1 d DU . . H23A H 0.4923 0.7182 0.0894 0.076 Uiso 1 1 calc R . . H23B H 0.5725 0.6844 0.1102 0.076 Uiso 1 1 calc R . . H23C H 0.4973 0.6291 0.1077 0.076 Uiso 1 1 calc R . . C31 C 0.9273(13) 0.5801(15) -0.1900(6) 0.052(7) Uani 1 1 d DU . . H31A H 0.9137 0.5362 -0.2076 0.079 Uiso 1 1 calc R . . H31B H 0.9572 0.5571 -0.1680 0.079 Uiso 1 1 calc R . . H31C H 0.9576 0.6219 -0.1998 0.079 Uiso 1 1 calc R . . C32 C 0.8761(14) 0.6924(15) -0.1556(6) 0.064(8) Uani 1 1 d DU . . H32A H 0.8299 0.7188 -0.1502 0.096 Uiso 1 1 calc R . . H32B H 0.9055 0.7324 -0.1670 0.096 Uiso 1 1 calc R . . H32C H 0.9073 0.6723 -0.1334 0.096 Uiso 1 1 calc R . . C33 C 0.8036(13) 0.6532(15) -0.2155(6) 0.058(8) Uani 1 1 d DU . . H33A H 0.7585 0.6806 -0.2093 0.087 Uiso 1 1 calc R . . H33B H 0.7873 0.6075 -0.2320 0.087 Uiso 1 1 calc R . . H33C H 0.8331 0.6926 -0.2272 0.087 Uiso 1 1 calc R . . C34 C 0.7426(7) 0.6100(8) -0.0732(2) 0.021(4) Uani 1 1 d GDU . . C35 C 0.8036(6) 0.6531(8) -0.0519(3) 0.026(4) Uani 1 1 d GDU . . H35 H 0.8480 0.6665 -0.0614 0.031 Uiso 1 1 calc R . . C36 C 0.7983(6) 0.6762(8) -0.0163(3) 0.032(4) Uani 1 1 d GDU . . H36 H 0.8391 0.7050 -0.0020 0.038 Uiso 1 1 calc R . . C37 C 0.7319(7) 0.6562(8) -0.0020(2) 0.024(4) Uani 1 1 d GDU . . C38 C 0.6709(6) 0.6131(9) -0.0233(3) 0.031(4) Uani 1 1 d GDU . . H38 H 0.6264 0.5997 -0.0137 0.038 Uiso 1 1 calc R . . C39 C 0.6762(6) 0.5900(8) -0.0589(3) 0.026(4) Uani 1 1 d GDU . . H39 H 0.6354 0.5612 -0.0732 0.031 Uiso 1 1 calc R . . C41 C 0.7014(13) 0.3761(15) -0.0955(6) 0.059(8) Uani 1 1 d DU . . H41A H 0.6511 0.3973 -0.1064 0.088 Uiso 1 1 calc R . . H41B H 0.7265 0.4154 -0.0776 0.088 Uiso 1 1 calc R . . H41C H 0.6952 0.3233 -0.0839 0.088 Uiso 1 1 calc R . . C42 C 0.7071(12) 0.3036(13) -0.1533(6) 0.045(7) Uani 1 1 d DU . . H42A H 0.7381 0.2908 -0.1716 0.068 Uiso 1 1 calc R . . H42B H 0.6590 0.3293 -0.1647 0.068 Uiso 1 1 calc R . . H42C H 0.6961 0.2528 -0.1413 0.068 Uiso 1 1 calc R . . C43 C 0.8280(11) 0.3228(14) -0.1082(6) 0.046(7) Uani 1 1 d DU . . H43A H 0.8566 0.3070 -0.1270 0.069 Uiso 1 1 calc R . . H43B H 0.8174 0.2737 -0.0948 0.069 Uiso 1 1 calc R . . H43C H 0.8582 0.3618 -0.0918 0.069 Uiso 1 1 calc R . . C51 C 0.3006(12) 0.7801(16) -0.2423(5) 0.050(7) Uani 1 1 d DU . . H51A H 0.2968 0.7305 -0.2572 0.075 Uiso 1 1 calc R . . H51B H 0.3189 0.8260 -0.2553 0.075 Uiso 1 1 calc R . . H51C H 0.2502 0.7937 -0.2367 0.075 Uiso 1 1 calc R . . C52 C 0.3623(12) 0.8444(13) -0.1827(6) 0.048(7) Uani 1 1 d DU . . H52A H 0.3973 0.8347 -0.1601 0.072 Uiso 1 1 calc R . . H52B H 0.3113 0.8575 -0.1777 0.072 Uiso 1 1 calc R . . H52C H 0.3810 0.8906 -0.1954 0.072 Uiso 1 1 calc R . . C53 C 0.4376(11) 0.7473(15) -0.2119(6) 0.055(8) Uani 1 1 d DU . . H53A H 0.4705 0.7409 -0.1884 0.083 Uiso 1 1 calc R . . H53B H 0.4563 0.7930 -0.2249 0.083 Uiso 1 1 calc R . . H53C H 0.4384 0.6964 -0.2257 0.083 Uiso 1 1 calc R . . C54 C 0.4791(6) 0.5355(8) -0.1730(3) 0.017(3) Uani 1 1 d GDU . . C55 C 0.5447(7) 0.5850(7) -0.1619(3) 0.038(4) Uani 1 1 d GDU . . H55 H 0.5419 0.6311 -0.1467 0.045 Uiso 1 1 calc R . . C56 C 0.6145(6) 0.5657(7) -0.1733(3) 0.029(4) Uani 1 1 d GDU . . H56 H 0.6584 0.5989 -0.1659 0.035 Uiso 1 1 calc R . . C57 C 0.6186(6) 0.4969(8) -0.1960(3) 0.016(4) Uani 1 1 d GDU . . C58 C 0.5531(7) 0.4474(7) -0.2071(3) 0.032(4) Uani 1 1 d GDU . . H58 H 0.5558 0.4013 -0.2222 0.038 Uiso 1 1 calc R . . C59 C 0.4833(6) 0.4667(7) -0.1956(3) 0.036(4) Uani 1 1 d GDU . . H59 H 0.4394 0.4336 -0.2031 0.043 Uiso 1 1 calc R . . C61 C 0.1403(13) 0.5327(17) -0.2027(5) 0.068(9) Uani 1 1 d DU . . H61A H 0.1155 0.5864 -0.2020 0.102 Uiso 1 1 calc R . . H61B H 0.1023 0.4890 -0.2026 0.102 Uiso 1 1 calc R . . H61C H 0.1626 0.5286 -0.2245 0.102 Uiso 1 1 calc R . . C62 C 0.2469(12) 0.4383(13) -0.1695(6) 0.056(8) Uani 1 1 d DU . . H62A H 0.2888 0.4333 -0.1490 0.083 Uiso 1 1 calc R . . H62B H 0.2672 0.4341 -0.1918 0.083 Uiso 1 1 calc R . . H62C H 0.2098 0.3941 -0.1685 0.083 Uiso 1 1 calc R . . C63 C 0.1693(13) 0.5282(16) -0.1334(6) 0.062(8) Uani 1 1 d DU . . H63A H 0.1454 0.5822 -0.1322 0.093 Uiso 1 1 calc R . . H63B H 0.2088 0.5204 -0.1121 0.093 Uiso 1 1 calc R . . H63C H 0.1305 0.4851 -0.1342 0.093 Uiso 1 1 calc R . . P1X P 0.9723(2) 0.2784(3) 0.00954(11) 0.0226(15) Uani 1 1 d DU . . P2X P 0.8695(2) 0.2343(3) 0.04820(11) 0.0284(16) Uani 1 1 d DU . . P3X P 0.5871(3) 0.0222(3) -0.12148(9) 0.0252(15) Uani 1 1 d DU . . P4X P 0.5674(3) -0.0448(3) -0.18585(10) 0.0273(16) Uani 1 1 d DU . . P5X P 0.9988(2) 0.0861(3) -0.20186(12) 0.0286(16) Uani 1 1 d DU . . P6X P 1.1261(2) 0.1652(3) -0.17642(13) 0.0324(17) Uani 1 1 d DU . . O1X O 0.9448(5) 0.2539(6) -0.03491(15) 0.025(4) Uani 1 1 d DU . . O2X O 0.7917(4) 0.1837(6) 0.0285(2) 0.045(4) Uani 1 1 d DU . . O3X O 0.6621(5) 0.0883(5) -0.1131(2) 0.028(4) Uani 1 1 d DU . . O4X O 0.6316(5) -0.0278(6) -0.21292(18) 0.028(4) Uani 1 1 d DU . . O5X O 0.9402(4) 0.0690(6) -0.1715(2) 0.029(4) Uani 1 1 d DU . . O6X O 1.1434(5) 0.2042(6) -0.1343(2) 0.034(4) Uani 1 1 d DU . . N1X N 0.8858(4) 0.3116(4) 0.0183(2) 0.026(4) Uani 1 1 d DU . . N2X N 0.9483(4) 0.1901(5) 0.0319(2) 0.020(4) Uani 1 1 d DU . . N3X N 0.5507(5) 0.0488(5) -0.16642(18) 0.028(5) Uani 1 1 d DU . . N4X N 0.6198(5) -0.0609(5) -0.14266(18) 0.026(4) Uani 1 1 d DU . . N5X N 1.0303(4) 0.1865(4) -0.1944(3) 0.021(4) Uani 1 1 d DU . . N6X N 1.0876(4) 0.0655(4) -0.1754(3) 0.019(4) Uani 1 1 d DU . . C1X C 0.8636(12) 0.3992(14) 0.0226(5) 0.050(7) Uani 1 1 d DU . . C2X C 0.9989(10) 0.1274(12) 0.0507(5) 0.030(6) Uani 1 1 d DU . . C3X C 0.4863(10) 0.1104(11) -0.1772(5) 0.021(5) Uani 1 1 d DU . . C4X C 0.6482(10) -0.1414(11) -0.1262(5) 0.023(5) Uani 1 1 d DU . . C5X C 0.9938(10) 0.2643(12) -0.2129(5) 0.027(6) Uani 1 1 d DU . . C6X C 1.1304(12) -0.0134(14) -0.1734(5) 0.050(7) Uani 1 1 d DU . . C11X C 0.9141(13) 0.4407(14) 0.0565(5) 0.052(7) Uani 1 1 d DU . . H11D H 0.9044 0.4134 0.0784 0.077 Uiso 1 1 calc R . . H11E H 0.9009 0.4991 0.0573 0.077 Uiso 1 1 calc R . . H11F H 0.9683 0.4352 0.0549 0.077 Uiso 1 1 calc R . . C12X C 0.7781(14) 0.4044(17) 0.0250(8) 0.079(9) Uani 1 1 d DU . . H12D H 0.7477 0.3805 0.0034 0.118 Uiso 1 1 calc R . . H12E H 0.7636 0.4621 0.0271 0.118 Uiso 1 1 calc R . . H12F H 0.7686 0.3739 0.0462 0.118 Uiso 1 1 calc R . . C13X C 0.8790(15) 0.4481(15) -0.0113(6) 0.064(8) Uani 1 1 d DU . . H13D H 0.8465 0.4261 -0.0328 0.096 Uiso 1 1 calc R . . H13E H 0.9328 0.4423 -0.0135 0.096 Uiso 1 1 calc R . . H13F H 0.8671 0.5064 -0.0086 0.096 Uiso 1 1 calc R . . C14X C 0.9953(6) 0.2422(8) -0.0591(3) 0.016(3) Uani 1 1 d GDU . . C15X C 1.0479(8) 0.3036(7) -0.0659(3) 0.034(4) Uani 1 1 d GDU . . H15X H 1.0503 0.3546 -0.0535 0.041 Uiso 1 1 calc R . . C16X C 1.0968(7) 0.2886(8) -0.0910(4) 0.031(4) Uani 1 1 d GDU . . H16X H 1.1320 0.3297 -0.0955 0.037 Uiso 1 1 calc R . . C17X C 1.0932(7) 0.2124(9) -0.1095(3) 0.025(4) Uani 1 1 d GDU . . C18X C 1.0407(8) 0.1511(7) -0.1028(3) 0.030(4) Uani 1 1 d GDU . . H18X H 1.0383 0.1000 -0.1151 0.036 Uiso 1 1 calc R . . C19X C 0.9917(7) 0.1660(7) -0.0776(3) 0.022(4) Uani 1 1 d GDU . . H19X H 0.9566 0.1249 -0.0731 0.027 Uiso 1 1 calc R . . C21X C 1.0579(12) 0.1017(13) 0.0268(6) 0.045(7) Uani 1 1 d DU . . H21D H 1.0887 0.1496 0.0226 0.068 Uiso 1 1 calc R . . H21E H 1.0308 0.0808 0.0038 0.068 Uiso 1 1 calc R . . H21F H 1.0914 0.0586 0.0389 0.068 Uiso 1 1 calc R . . C22X C 0.9522(12) 0.0522(12) 0.0593(6) 0.045(7) Uani 1 1 d DU . . H22D H 0.9170 0.0689 0.0753 0.068 Uiso 1 1 calc R . . H22E H 0.9870 0.0098 0.0711 0.068 Uiso 1 1 calc R . . H22F H 0.9229 0.0301 0.0370 0.068 Uiso 1 1 calc R . . C23X C 1.0427(12) 0.1641(13) 0.0885(5) 0.045(7) Uani 1 1 d DU . . H23D H 1.0739 0.2113 0.0839 0.068 Uiso 1 1 calc R . . H23E H 1.0756 0.1215 0.1014 0.068 Uiso 1 1 calc R . . H23F H 1.0050 0.1817 0.1030 0.068 Uiso 1 1 calc R . . C31X C 0.4203(15) 0.102(2) -0.1552(8) 0.103(12) Uani 1 1 d DU . . H31D H 0.4411 0.1068 -0.1295 0.155 Uiso 1 1 calc R . . H31E H 0.3955 0.0484 -0.1600 0.155 Uiso 1 1 calc R . . H31F H 0.3827 0.1458 -0.1622 0.155 Uiso 1 1 calc R . . C32X C 0.5152(13) 0.1992(14) -0.1733(7) 0.072(9) Uani 1 1 d DU . . H32D H 0.5563 0.2067 -0.1872 0.107 Uiso 1 1 calc R . . H32E H 0.5347 0.2109 -0.1479 0.107 Uiso 1 1 calc R . . H32F H 0.4731 0.2369 -0.1822 0.107 Uiso 1 1 calc R . . C33X C 0.4535(17) 0.0935(19) -0.2166(6) 0.092(10) Uani 1 1 d DU . . H33D H 0.4934 0.1017 -0.2311 0.138 Uiso 1 1 calc R . . H33E H 0.4110 0.1313 -0.2246 0.138 Uiso 1 1 calc R . . H33F H 0.4351 0.0366 -0.2192 0.138 Uiso 1 1 calc R . . C34X C 0.6947(7) 0.1105(8) -0.0772(2) 0.021(4) Uani 1 1 d GDU . . C35X C 0.6502(6) 0.1521(8) -0.0551(3) 0.026(4) Uani 1 1 d GDU . . H35X H 0.5975 0.1620 -0.0635 0.031 Uiso 1 1 calc R . . C36X C 0.6845(7) 0.1788(8) -0.0203(3) 0.032(4) Uani 1 1 d GDU . . H36X H 0.6548 0.2067 -0.0055 0.038 Uiso 1 1 calc R . . C37X C 0.7633(7) 0.1640(8) -0.0077(3) 0.024(4) Uani 1 1 d GDU . . C38X C 0.8078(6) 0.1224(9) -0.0298(3) 0.031(4) Uani 1 1 d GDU . . H38X H 0.8605 0.1125 -0.0213 0.038 Uiso 1 1 calc R . . C39X C 0.7734(7) 0.0957(8) -0.0646(3) 0.026(4) Uani 1 1 d GDU . . H39X H 0.8032 0.0679 -0.0794 0.031 Uiso 1 1 calc R . . C41X C 0.7244(11) -0.1252(15) -0.0995(6) 0.048(7) Uani 1 1 d DU . . H41D H 0.7142 -0.0897 -0.0800 0.072 Uiso 1 1 calc R . . H41E H 0.7612 -0.0982 -0.1122 0.072 Uiso 1 1 calc R . . H41F H 0.7456 -0.1777 -0.0896 0.072 Uiso 1 1 calc R . . C42X C 0.6683(12) -0.2002(13) -0.1556(5) 0.038(6) Uani 1 1 d DU . . H42D H 0.7105 -0.1768 -0.1659 0.057 Uiso 1 1 calc R . . H42E H 0.6235 -0.2068 -0.1745 0.057 Uiso 1 1 calc R . . H42F H 0.6835 -0.2539 -0.1449 0.057 Uiso 1 1 calc R . . C43X C 0.5898(11) -0.1818(14) -0.1059(6) 0.044(7) Uani 1 1 d DU . . H43D H 0.5816 -0.1460 -0.0861 0.066 Uiso 1 1 calc R . . H43E H 0.6094 -0.2351 -0.0963 0.066 Uiso 1 1 calc R . . H43F H 0.5413 -0.1898 -0.1223 0.066 Uiso 1 1 calc R . . C51X C 1.0457(14) 0.2977(16) -0.2385(6) 0.075(9) Uani 1 1 d DU . . H51D H 1.0990 0.2974 -0.2263 0.113 Uiso 1 1 calc R . . H51E H 1.0305 0.3541 -0.2457 0.113 Uiso 1 1 calc R . . H51F H 1.0405 0.2627 -0.2599 0.113 Uiso 1 1 calc R . . C52X C 0.9943(16) 0.3283(17) -0.1814(7) 0.087(10) Uani 1 1 d DU . . H52D H 1.0469 0.3368 -0.1690 0.130 Uiso 1 1 calc R . . H52E H 0.9634 0.3069 -0.1644 0.130 Uiso 1 1 calc R . . H52F H 0.9729 0.3807 -0.1913 0.130 Uiso 1 1 calc R . . C53X C 0.9122(13) 0.2512(19) -0.2290(9) 0.109(12) Uani 1 1 d DU . . H53D H 0.9082 0.2062 -0.2465 0.164 Uiso 1 1 calc R . . H53E H 0.8913 0.3016 -0.2410 0.164 Uiso 1 1 calc R . . H53F H 0.8832 0.2369 -0.2101 0.164 Uiso 1 1 calc R . . C54X C 0.8627(6) 0.0450(8) -0.1827(3) 0.017(3) Uani 1 1 d GDU . . C55X C 0.8041(7) 0.0990(7) -0.1761(3) 0.038(4) Uani 1 1 d GDU . . H55X H 0.8169 0.1504 -0.1647 0.045 Uiso 1 1 calc R . . C56X C 0.7263(6) 0.0763(8) -0.1864(3) 0.029(4) Uani 1 1 d GDU . . H56X H 0.6870 0.1124 -0.1820 0.035 Uiso 1 1 calc R . . C57X C 0.7072(6) -0.0006(8) -0.2034(3) 0.016(4) Uani 1 1 d GDU . . C58X C 0.7658(7) -0.0546(7) -0.2101(3) 0.032(4) Uani 1 1 d GDU . . H58X H 0.7530 -0.1060 -0.2215 0.038 Uiso 1 1 calc R . . C59X C 0.8436(6) -0.0318(7) -0.1997(3) 0.036(4) Uani 1 1 d GDU . . H59X H 0.8829 -0.0680 -0.2042 0.043 Uiso 1 1 calc R . . C61X C 1.1995(12) -0.0078(16) -0.1402(6) 0.059(8) Uani 1 1 d DU . . H61D H 1.2327 0.0386 -0.1438 0.088 Uiso 1 1 calc R . . H61E H 1.2291 -0.0589 -0.1385 0.088 Uiso 1 1 calc R . . H61F H 1.1791 0.0005 -0.1180 0.088 Uiso 1 1 calc R . . C62X C 1.1597(14) -0.0282(16) -0.2091(5) 0.059(8) Uani 1 1 d DU . . H62D H 1.1938 0.0168 -0.2132 0.089 Uiso 1 1 calc R . . H62E H 1.1162 -0.0304 -0.2289 0.089 Uiso 1 1 calc R . . H62F H 1.1876 -0.0805 -0.2078 0.089 Uiso 1 1 calc R . . C63X C 1.0754(13) -0.0847(15) -0.1664(6) 0.060(8) Uani 1 1 d DU . . H63D H 1.0317 -0.0869 -0.1862 0.090 Uiso 1 1 calc R . . H63E H 1.0573 -0.0746 -0.1438 0.090 Uiso 1 1 calc R . . H63F H 1.1029 -0.1372 -0.1650 0.090 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 0.030(3) 0.020(4) 0.016(3) 0.004(3) 0.006(3) -0.002(3) P2 0.026(3) 0.025(4) 0.017(3) -0.005(3) 0.007(3) -0.003(3) P3 0.021(3) 0.033(4) 0.023(3) -0.004(3) 0.006(3) -0.003(3) P4 0.032(4) 0.025(4) 0.020(3) -0.004(3) 0.004(3) 0.001(3) P5 0.028(4) 0.037(4) 0.025(3) 0.001(3) -0.005(3) -0.004(3) P6 0.031(4) 0.040(4) 0.028(4) -0.001(3) -0.001(3) 0.004(3) O1 0.036(8) 0.003(8) 0.057(10) -0.007(7) -0.011(8) 0.000(6) O2 0.032(8) 0.050(10) 0.011(8) -0.007(7) 0.000(6) -0.007(7) O3 0.021(8) 0.031(9) 0.021(8) 0.002(7) 0.007(6) 0.008(7) O4 0.033(9) 0.035(9) 0.032(8) -0.008(7) 0.004(7) 0.017(7) O5 0.040(9) 0.027(9) 0.020(8) 0.013(6) -0.002(7) 0.002(7) O6 0.018(8) 0.062(11) 0.025(8) -0.002(7) -0.007(7) 0.011(7) N1 0.024(7) 0.019(7) 0.014(7) 0.001(6) 0.012(6) -0.010(6) N2 0.006(9) 0.034(11) 0.030(10) 0.005(8) 0.003(8) 0.001(8) N3 0.036(10) 0.030(11) 0.015(9) 0.003(8) 0.021(8) 0.010(9) N4 0.015(9) 0.018(10) 0.011(9) -0.001(7) 0.003(7) -0.011(8) N5 0.010(7) 0.024(8) 0.025(7) 0.010(6) -0.002(6) 0.000(6) N6 0.015(9) 0.023(11) 0.034(10) -0.006(8) -0.001(8) 0.003(8) C1 0.033(9) 0.029(9) 0.024(8) -0.006(7) 0.009(7) 0.000(7) C2 0.020(8) 0.015(8) 0.020(8) 0.001(7) 0.002(7) 0.003(7) C3 0.037(8) 0.042(8) 0.038(8) 0.001(6) 0.014(6) -0.003(6) C4 0.042(9) 0.042(10) 0.042(9) -0.004(8) 0.005(7) -0.004(8) C5 0.035(9) 0.029(9) 0.031(9) 0.002(7) 0.008(7) -0.001(7) C6 0.034(9) 0.036(9) 0.030(8) -0.001(7) 0.008(7) 0.003(7) C11 0.10(2) 0.075(19) 0.077(18) -0.029(16) 0.020(16) -0.031(17) C12 0.09(2) 0.08(2) 0.15(2) -0.007(19) 0.019(19) -0.034(17) C13 0.13(2) 0.053(17) 0.046(16) 0.022(13) -0.009(15) -0.039(16) C14 0.023(6) 0.020(6) 0.007(5) 0.000(5) 0.006(5) 0.007(5) C15 0.030(9) 0.037(10) 0.031(9) -0.020(8) -0.006(8) -0.003(8) C16 0.026(9) 0.037(10) 0.031(9) 0.012(8) 0.009(8) -0.007(8) C17 0.041(9) 0.025(10) 0.011(8) 0.009(7) 0.011(7) -0.008(8) C18 0.036(9) 0.030(10) 0.023(8) 0.003(7) -0.001(7) -0.004(8) C19 0.027(9) 0.019(9) 0.019(8) 0.001(7) -0.002(7) 0.003(7) C21 0.064(16) 0.049(16) 0.044(14) 0.018(12) 0.012(13) -0.007(13) C22 0.062(15) 0.033(15) 0.029(13) -0.003(11) 0.026(11) -0.012(12) C23 0.087(17) 0.039(15) 0.037(14) -0.002(11) 0.043(13) -0.019(13) C31 0.080(17) 0.049(16) 0.031(13) -0.003(12) 0.019(12) 0.003(14) C32 0.048(15) 0.075(19) 0.065(16) -0.031(14) 0.001(13) -0.016(14) C33 0.076(17) 0.051(16) 0.047(15) 0.040(13) 0.013(13) -0.006(14) C34 0.020(9) 0.034(10) 0.008(8) 0.001(7) -0.005(7) 0.005(7) C35 0.024(8) 0.013(9) 0.042(10) 0.013(7) 0.007(8) 0.010(7) C36 0.048(10) 0.044(10) 0.003(8) 0.005(7) 0.006(7) -0.003(8) C37 0.024(8) 0.036(10) 0.014(8) -0.006(7) 0.009(7) -0.002(8) C38 0.018(8) 0.037(10) 0.042(10) -0.004(8) 0.013(8) -0.002(8) C39 0.022(8) 0.041(10) 0.016(8) -0.008(7) 0.006(7) 0.002(7) C41 0.054(15) 0.045(16) 0.087(18) 0.024(14) 0.043(14) -0.017(13) C42 0.049(14) 0.023(14) 0.061(15) -0.006(12) 0.003(12) -0.009(11) C43 0.061(15) 0.040(15) 0.041(14) -0.005(12) 0.018(12) 0.012(13) C51 0.043(14) 0.080(18) 0.025(13) 0.000(12) -0.002(11) 0.008(13) C52 0.034(13) 0.049(16) 0.063(15) 0.011(13) 0.012(12) -0.013(12) C53 0.045(15) 0.043(16) 0.071(16) 0.031(13) -0.010(13) 0.006(12) C54 0.023(6) 0.019(6) 0.012(5) 0.003(5) 0.006(5) 0.002(5) C55 0.050(10) 0.039(10) 0.022(8) 0.001(7) 0.001(8) -0.004(9) C56 0.028(6) 0.023(6) 0.037(6) -0.007(5) 0.005(5) 0.005(5) C57 0.016(8) 0.021(9) 0.010(7) -0.010(7) 0.000(6) 0.004(7) C58 0.029(9) 0.024(9) 0.039(9) 0.000(7) -0.002(8) -0.011(8) C59 0.042(6) 0.029(6) 0.038(6) -0.007(5) 0.010(5) 0.001(5) C61 0.073(17) 0.090(19) 0.043(15) -0.004(14) 0.013(13) -0.039(15) C62 0.036(14) 0.057(17) 0.070(16) 0.023(13) 0.000(12) -0.021(13) C63 0.066(16) 0.060(17) 0.071(17) -0.007(14) 0.046(14) -0.032(14) P1X 0.036(4) 0.019(4) 0.011(3) 0.001(3) 0.001(3) -0.002(3) P2X 0.026(3) 0.034(4) 0.025(3) -0.003(3) 0.006(3) 0.002(3) P3X 0.030(3) 0.024(4) 0.023(3) 0.006(3) 0.008(3) -0.001(3) P4X 0.032(4) 0.017(4) 0.032(4) -0.003(3) 0.006(3) -0.004(3) P5X 0.027(3) 0.032(4) 0.028(3) 0.000(3) 0.009(3) -0.003(3) P6X 0.018(3) 0.051(4) 0.030(4) 0.003(3) 0.010(3) -0.004(3) O1X 0.027(8) 0.022(9) 0.023(8) -0.009(6) -0.005(6) 0.012(6) O2X 0.036(9) 0.074(12) 0.024(9) -0.007(8) -0.001(7) 0.001(8) O3X 0.034(8) 0.036(9) 0.013(7) 0.014(7) -0.002(6) -0.027(7) O4X 0.033(9) 0.031(9) 0.019(8) 0.007(7) 0.004(7) -0.009(7) O5X 0.033(7) 0.033(7) 0.024(6) -0.014(5) 0.012(5) -0.004(6) O6X 0.028(8) 0.043(10) 0.032(9) 0.003(7) 0.011(7) 0.001(7) N1X 0.032(7) 0.018(8) 0.029(7) 0.001(6) 0.007(6) 0.014(6) N2X 0.019(7) 0.019(7) 0.023(7) 0.005(6) 0.004(6) 0.002(6) N3X 0.027(7) 0.028(8) 0.027(7) 0.003(6) -0.001(6) 0.008(6) N4X 0.029(7) 0.023(8) 0.025(7) 0.008(6) 0.001(6) 0.002(6) N5X 0.019(7) 0.020(8) 0.025(7) 0.001(6) 0.002(6) 0.000(6) N6X 0.025(7) 0.015(7) 0.016(7) 0.003(6) 0.004(6) 0.006(6) C1X 0.053(10) 0.047(10) 0.049(9) -0.001(8) 0.008(7) 0.002(8) C2X 0.031(9) 0.025(9) 0.033(9) 0.004(7) 0.004(7) 0.002(7) C3X 0.019(8) 0.022(9) 0.024(8) -0.008(7) 0.006(7) 0.002(7) C4X 0.025(7) 0.021(7) 0.023(7) 0.006(6) 0.008(6) -0.001(6) C5X 0.027(8) 0.022(9) 0.032(8) 0.003(7) 0.003(7) 0.004(7) C6X 0.053(8) 0.050(8) 0.046(8) -0.004(6) 0.009(6) 0.003(6) C11X 0.079(17) 0.038(15) 0.046(14) -0.001(12) 0.033(13) 0.022(13) C12X 0.089(19) 0.048(17) 0.10(2) 0.025(15) 0.018(16) 0.024(15) C13X 0.101(19) 0.034(16) 0.073(17) 0.032(13) 0.061(15) 0.029(14) C14X 0.023(6) 0.020(6) 0.007(5) 0.000(5) 0.006(5) 0.007(5) C15X 0.030(9) 0.037(10) 0.031(9) -0.020(8) -0.006(8) -0.003(8) C16X 0.026(9) 0.037(10) 0.031(9) 0.012(8) 0.009(8) -0.007(8) C17X 0.041(9) 0.025(10) 0.011(8) 0.009(7) 0.011(7) -0.008(8) C18X 0.036(9) 0.030(10) 0.023(8) 0.003(7) -0.001(7) -0.004(8) C19X 0.027(9) 0.019(9) 0.019(8) 0.001(7) -0.002(7) 0.003(7) C21X 0.057(15) 0.026(14) 0.055(14) 0.028(12) 0.017(12) 0.014(12) C22X 0.049(14) 0.018(14) 0.065(15) -0.008(12) 0.001(12) -0.008(12) C23X 0.052(14) 0.034(14) 0.038(14) 0.004(11) -0.022(12) 0.006(12) C31X 0.071(19) 0.12(2) 0.13(2) 0.010(19) 0.035(18) -0.005(18) C32X 0.042(15) 0.070(19) 0.089(19) 0.003(15) -0.028(14) 0.008(14) C33X 0.095(12) 0.085(12) 0.092(12) -0.002(8) 0.007(8) 0.007(8) C34X 0.020(9) 0.034(10) 0.008(8) 0.001(7) -0.005(7) 0.005(7) C35X 0.024(8) 0.013(9) 0.042(10) 0.013(7) 0.007(8) 0.010(7) C36X 0.048(10) 0.044(10) 0.003(8) 0.005(7) 0.006(7) -0.003(8) C37X 0.024(8) 0.036(10) 0.014(8) -0.006(7) 0.009(7) -0.002(8) C38X 0.018(8) 0.037(10) 0.042(10) -0.004(8) 0.013(8) -0.002(8) C39X 0.022(8) 0.041(10) 0.016(8) -0.008(7) 0.006(7) 0.002(7) C41X 0.035(13) 0.051(16) 0.048(15) -0.001(12) -0.019(12) 0.004(12) C42X 0.037(13) 0.032(14) 0.051(14) 0.003(11) 0.023(11) 0.011(11) C43X 0.019(12) 0.057(16) 0.058(15) 0.002(13) 0.014(11) -0.025(12) C51X 0.11(2) 0.064(18) 0.063(16) 0.049(14) 0.047(15) 0.028(16) C52X 0.10(2) 0.069(19) 0.10(2) 0.009(16) 0.031(17) 0.039(16) C53X 0.08(2) 0.09(2) 0.15(2) 0.041(19) -0.023(18) 0.007(17) C54X 0.023(6) 0.019(6) 0.012(5) 0.003(5) 0.006(5) 0.002(5) C55X 0.050(10) 0.039(10) 0.022(8) 0.001(7) 0.001(8) -0.004(9) C56X 0.028(6) 0.023(6) 0.037(6) -0.007(5) 0.005(5) 0.005(5) C57X 0.016(8) 0.021(9) 0.010(7) -0.010(7) 0.000(6) 0.004(7) C58X 0.029(9) 0.024(9) 0.039(9) 0.000(7) -0.002(8) -0.011(8) C59X 0.042(6) 0.029(6) 0.038(6) -0.007(5) 0.010(5) 0.001(5) C61X 0.039(14) 0.082(19) 0.063(16) 0.013(14) 0.028(13) 0.039(13) C62X 0.077(17) 0.064(17) 0.038(14) 0.000(13) 0.011(13) 0.039(14) C63X 0.069(16) 0.062(17) 0.045(15) 0.024(13) 0.002(13) -0.002(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 N1 1.680(5) . ? P1 O1 1.681(5) . ? P1 N2 1.720(7) . ? P1 P2 2.579(3) . ? P2 O2 1.634(7) . ? P2 N1 1.714(7) . ? P2 N2 1.741(6) . ? P3 O3 1.665(6) . ? P3 N4 1.688(7) . ? P3 N3 1.729(6) . ? P3 P4 2.582(3) . ? P4 O4 1.649(5) . ? P4 N3 1.702(6) . ? P4 N4 1.719(6) . ? P5 O5 1.668(6) . ? P5 N5 1.697(5) . ? P5 N6 1.713(8) . ? P5 P6 2.580(3) . ? P6 O6 1.658(7) . ? P6 N5 1.719(6) . ? P6 N6 1.726(6) . ? O1 C14 1.364(10) . ? O2 C37 1.385(12) . ? O3 C34 1.398(10) . ? O4 C57 1.411(11) . ? O5 C54 1.375(11) . ? O6 C17 1.373(10) . ? N1 C1 1.50(2) . ? N2 C2 1.450(19) . ? N3 C3 1.46(2) . ? N4 C4 1.43(2) . ? N5 C5 1.49(2) . ? N6 C6 1.42(2) . ? C1 C12 1.51(2) . ? C1 C11 1.55(2) . ? C1 C13 1.54(2) . ? C2 C22 1.51(2) . ? C2 C21 1.53(2) . ? C2 C23 1.58(2) . ? C3 C31 1.52(2) . ? C3 C32 1.50(2) . ? C3 C33 1.51(2) . ? C4 C42 1.52(2) . ? C4 C43 1.52(2) . ? C4 C41 1.54(2) . ? C5 C53 1.46(2) . ? C5 C52 1.54(2) . ? C5 C51 1.53(2) . ? C6 C62 1.52(2) . ? C6 C63 1.54(2) . ? C6 C61 1.58(2) . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C54 C55 1.3900 . ? C54 C59 1.3900 . ? C55 C56 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C58 C59 1.3900 . ? P1X N1X 1.680(5) . ? P1X O1X 1.681(5) . ? P1X N2X 1.719(7) . ? P1X P2X 2.579(3) . ? P2X O2X 1.634(7) . ? P2X N1X 1.714(7) . ? P2X N2X 1.741(6) . ? P3X O3X 1.665(6) . ? P3X N4X 1.688(7) . ? P3X N3X 1.729(6) . ? P3X P4X 2.582(3) . ? P4X O4X 1.649(5) . ? P4X N3X 1.702(6) . ? P4X N4X 1.719(6) . ? P5X O5X 1.668(6) . ? P5X N5X 1.697(6) . ? P5X N6X 1.713(8) . ? P5X P6X 2.580(3) . ? P6X O6X 1.658(7) . ? P6X N5X 1.719(7) . ? P6X N6X 1.726(6) . ? O1X C14X 1.375(12) . ? O2X C37X 1.384(12) . ? O3X C34X 1.399(11) . ? O4X C57X 1.372(12) . ? O5X C54X 1.393(11) . ? O6X C17X 1.382(12) . ? N1X C1X 1.46(2) . ? N2X C2X 1.43(2) . ? N3X C3X 1.492(19) . ? N4X C4X 1.467(19) . ? N5X C5X 1.50(2) . ? N6X C6X 1.46(2) . ? C1X C12X 1.51(3) . ? C1X C13X 1.54(2) . ? C1X C11X 1.55(2) . ? C2X C22X 1.51(2) . ? C2X C21X 1.53(2) . ? C2X C23X 1.58(2) . ? C3X C33X 1.50(2) . ? C3X C32X 1.50(2) . ? C3X C31X 1.53(2) . ? C4X C43X 1.51(2) . ? C4X C41X 1.53(2) . ? C4X C42X 1.52(2) . ? C5X C53X 1.46(2) . ? C5X C51X 1.52(2) . ? C5X C52X 1.55(2) . ? C6X C62X 1.52(2) . ? C6X C61X 1.57(2) . ? C6X C63X 1.54(2) . ? C14X C15X 1.3900 . ? C14X C19X 1.3900 . ? C15X C16X 1.3900 . ? C16X C17X 1.3900 . ? C17X C18X 1.3900 . ? C18X C19X 1.3900 . ? C34X C35X 1.3900 . ? C34X C39X 1.3900 . ? C35X C36X 1.3900 . ? C36X C37X 1.3900 . ? C37X C38X 1.3900 . ? C38X C39X 1.3900 . ? C54X C55X 1.3900 . ? C54X C59X 1.3900 . ? C55X C56X 1.3900 . ? C56X C57X 1.3900 . ? C57X C58X 1.3900 . ? C58X C59X 1.3900 . ? 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 N1 P1 O1 98.7(4) . . ? N1 P1 N2 82.1(3) . . ? O1 P1 N2 103.4(4) . . ? N1 P1 P2 41.0(2) . . ? O1 P1 P2 112.1(2) . . ? N2 P1 P2 42.1(2) . . ? O2 P2 N1 106.5(4) . . ? O2 P2 N2 106.8(3) . . ? N1 P2 N2 80.5(3) . . ? O2 P2 P1 119.2(3) . . ? N1 P2 P1 40.05(18) . . ? N2 P2 P1 41.5(2) . . ? O3 P3 N4 105.3(4) . . ? O3 P3 N3 99.6(3) . . ? N4 P3 N3 80.8(3) . . ? O3 P3 P4 114.0(2) . . ? N4 P3 P4 41.2(2) . . ? N3 P3 P4 40.8(2) . . ? O4 P4 N3 107.4(4) . . ? O4 P4 N4 106.6(4) . . ? N3 P4 N4 80.7(3) . . ? O4 P4 P3 120.1(3) . . ? N3 P4 P3 41.6(2) . . ? N4 P4 P3 40.3(2) . . ? O5 P5 N5 105.2(3) . . ? O5 P5 N6 100.3(3) . . ? N5 P5 N6 81.6(3) . . ? O5 P5 P6 114.9(3) . . ? N5 P5 P6 41.3(2) . . ? N6 P5 P6 41.6(2) . . ? O6 P6 N5 107.2(3) . . ? O6 P6 N6 109.4(4) . . ? N5 P6 N6 80.6(3) . . ? O6 P6 P5 122.1(2) . . ? N5 P6 P5 40.65(18) . . ? N6 P6 P5 41.2(2) . . ? C14 O1 P1 123.2(7) . . ? C37 O2 P2 129.3(7) . . ? C34 O3 P3 122.1(6) . . ? C57 O4 P4 127.4(6) . . ? C54 O5 P5 119.1(7) . . ? C17 O6 P6 130.6(7) . . ? C1 N1 P1 127.4(7) . . ? C1 N1 P2 124.6(8) . . ? P1 N1 P2 98.9(3) . . ? C2 N2 P1 127.3(7) . . ? C2 N2 P2 124.3(8) . . ? P1 N2 P2 96.4(3) . . ? C3 N3 P4 128.4(8) . . ? C3 N3 P3 126.4(8) . . ? P4 N3 P3 97.6(3) . . ? C4 N4 P3 128.7(8) . . ? C4 N4 P4 126.7(9) . . ? P3 N4 P4 98.5(4) . . ? C5 N5 P5 124.8(9) . . ? C5 N5 P6 126.6(8) . . ? P5 N5 P6 98.1(3) . . ? C6 N6 P5 127.1(9) . . ? C6 N6 P6 126.0(8) . . ? P5 N6 P6 97.2(3) . . ? C12 C1 N1 109.4(16) . . ? C12 C1 C11 110.4(18) . . ? N1 C1 C11 111.3(16) . . ? C12 C1 C13 109.5(18) . . ? N1 C1 C13 108.2(14) . . ? C11 C1 C13 108.0(17) . . ? N2 C2 C22 107.8(13) . . ? N2 C2 C21 108.8(13) . . ? C22 C2 C21 110.3(15) . . ? N2 C2 C23 110.6(14) . . ? C22 C2 C23 109.7(14) . . ? C21 C2 C23 109.6(15) . . ? N3 C3 C31 109.4(16) . . ? N3 C3 C32 113.8(16) . . ? C31 C3 C32 108.6(16) . . ? N3 C3 C33 106.1(15) . . ? C31 C3 C33 110.7(16) . . ? C32 C3 C33 108.2(17) . . ? N4 C4 C42 111.9(15) . . ? N4 C4 C43 111.7(15) . . ? C42 C4 C43 108.8(16) . . ? N4 C4 C41 109.1(15) . . ? C42 C4 C41 106.6(16) . . ? C43 C4 C41 108.6(16) . . ? C53 C5 N5 110.0(15) . . ? C53 C5 C52 106.1(16) . . ? N5 C5 C52 105.6(14) . . ? C53 C5 C51 114.2(16) . . ? N5 C5 C51 111.4(15) . . ? C52 C5 C51 109.1(16) . . ? N6 C6 C62 109.5(14) . . ? N6 C6 C63 110.6(15) . . ? C62 C6 C63 109.8(17) . . ? N6 C6 C61 109.1(15) . . ? C62 C6 C61 109.4(16) . . ? C63 C6 C61 108.4(16) . . ? O1 C14 C15 120.5(8) . . ? O1 C14 C19 119.5(8) . . ? C15 C14 C19 120.0 . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? O6 C17 C16 118.3(9) . . ? O6 C17 C18 121.6(9) . . ? C16 C17 C18 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C14 120.0 . . ? C35 C34 C39 120.0 . . ? C35 C34 O3 120.5(8) . . ? C39 C34 O3 119.4(8) . . ? C36 C35 C34 120.0 . . ? C35 C36 C37 120.0 . . ? O2 C37 C38 123.8(8) . . ? O2 C37 C36 115.9(8) . . ? C38 C37 C36 120.0 . . ? C39 C38 C37 120.0 . . ? C38 C39 C34 120.0 . . ? O5 C54 C55 118.2(8) . . ? O5 C54 C59 121.8(8) . . ? C55 C54 C59 120.0 . . ? C56 C55 C54 120.0 . . ? C57 C56 C55 120.0 . . ? C56 C57 C58 120.0 . . ? C56 C57 O4 122.2(8) . . ? C58 C57 O4 117.8(8) . . ? C59 C58 C57 120.0 . . ? C58 C59 C54 120.0 . . ? N1X P1X O1X 98.7(4) . . ? N1X P1X N2X 82.1(3) . . ? O1X P1X N2X 103.4(4) . . ? N1X P1X P2X 41.0(2) . . ? O1X P1X P2X 112.1(3) . . ? N2X P1X P2X 42.1(2) . . ? O2X P2X N1X 106.5(4) . . ? O2X P2X N2X 106.7(3) . . ? N1X P2X N2X 80.5(3) . . ? O2X P2X P1X 119.2(3) . . ? N1X P2X P1X 40.05(18) . . ? N2X P2X P1X 41.5(2) . . ? O3X P3X N4X 105.4(4) . . ? O3X P3X N3X 99.7(3) . . ? N4X P3X N3X 80.8(3) . . ? O3X P3X P4X 114.0(2) . . ? N4X P3X P4X 41.2(2) . . ? N3X P3X P4X 40.8(2) . . ? O4X P4X N3X 107.4(4) . . ? O4X P4X N4X 106.7(4) . . ? N3X P4X N4X 80.7(3) . . ? O4X P4X P3X 120.1(3) . . ? N3X P4X P3X 41.6(2) . . ? N4X P4X P3X 40.3(2) . . ? O5X P5X N5X 105.2(3) . . ? O5X P5X N6X 100.4(4) . . ? N5X P5X N6X 81.6(3) . . ? O5X P5X P6X 114.9(3) . . ? N5X P5X P6X 41.3(2) . . ? N6X P5X P6X 41.6(2) . . ? O6X P6X N5X 107.3(4) . . ? O6X P6X N6X 109.4(4) . . ? N5X P6X N6X 80.6(3) . . ? O6X P6X P5X 122.1(3) . . ? N5X P6X P5X 40.64(18) . . ? N6X P6X P5X 41.2(2) . . ? C14X O1X P1X 124.5(7) . . ? C37X O2X P2X 132.3(7) . . ? C34X O3X P3X 120.8(7) . . ? C57X O4X P4X 128.1(7) . . ? C54X O5X P5X 121.2(7) . . ? C17X O6X P6X 129.1(7) . . ? C1X N1X P1X 125.7(9) . . ? C1X N1X P2X 122.5(9) . . ? P1X N1X P2X 98.9(3) . . ? C2X N2X P1X 128.7(9) . . ? C2X N2X P2X 124.5(9) . . ? P1X N2X P2X 96.3(3) . . ? C3X N3X P4X 129.6(8) . . ? C3X N3X P3X 123.5(8) . . ? P4X N3X P3X 97.6(3) . . ? C4X N4X P3X 127.4(8) . . ? C4X N4X P4X 127.2(8) . . ? P3X N4X P4X 98.6(4) . . ? C5X N5X P5X 127.2(8) . . ? C5X N5X P6X 130.1(8) . . ? P5X N5X P6X 98.1(3) . . ? C6X N6X P5X 126.6(9) . . ? C6X N6X P6X 126.8(9) . . ? P5X N6X P6X 97.2(3) . . ? N1X C1X C12X 109.9(17) . . ? N1X C1X C13X 107.9(16) . . ? C12X C1X C13X 109.5(18) . . ? N1X C1X C11X 111.8(16) . . ? C12X C1X C11X 110.7(18) . . ? C13X C1X C11X 107.0(17) . . ? N2X C2X C22X 110.4(14) . . ? N2X C2X C21X 108.8(14) . . ? C22X C2X C21X 110.6(16) . . ? N2X C2X C23X 109.6(14) . . ? C22X C2X C23X 107.4(15) . . ? C21X C2X C23X 110.1(15) . . ? C33X C3X N3X 106.6(16) . . ? C33X C3X C32X 109.2(17) . . ? N3X C3X C32X 111.7(14) . . ? C33X C3X C31X 108.2(18) . . ? N3X C3X C31X 113.6(17) . . ? C32X C3X C31X 107.5(18) . . ? N4X C4X C43X 111.8(14) . . ? N4X C4X C41X 108.3(14) . . ? C43X C4X C41X 109.3(15) . . ? N4X C4X C42X 110.0(14) . . ? C43X C4X C42X 110.7(16) . . ? C41X C4X C42X 106.6(15) . . ? C53X C5X C51X 116.0(18) . . ? C53X C5X N5X 111.9(17) . . ? C51X C5X N5X 108.9(15) . . ? C53X C5X C52X 106.3(18) . . ? C51X C5X C52X 108.5(17) . . ? N5X C5X C52X 104.5(15) . . ? N6X C6X C62X 109.7(16) . . ? N6X C6X C61X 107.8(16) . . ? C62X C6X C61X 111.5(17) . . ? N6X C6X C63X 108.6(16) . . ? C62X C6X C63X 110.3(18) . . ? C61X C6X C63X 109.0(17) . . ? O1X C14X C15X 122.6(9) . . ? O1X C14X C19X 117.4(9) . . ? C15X C14X C19X 120.0 . . ? C16X C15X C14X 120.0 . . ? C15X C16X C17X 120.0 . . ? O6X C17X C18X 124.4(10) . . ? O6X C17X C16X 115.6(10) . . ? C18X C17X C16X 120.0 . . ? C17X C18X C19X 120.0 . . ? C18X C19X C14X 120.0 . . ? C35X C34X C39X 120.0 . . ? C35X C34X O3X 120.5(9) . . ? C39X C34X O3X 119.3(9) . . ? C34X C35X C36X 120.0 . . ? C35X C36X C37X 120.0 . . ? O2X C37X C38X 122.7(9) . . ? O2X C37X C36X 116.9(9) . . ? C38X C37X C36X 120.0 . . ? C37X C38X C39X 120.0 . . ? C38X C39X C34X 120.0 . . ? C55X C54X C59X 120.0 . . ? C55X C54X O5X 118.7(9) . . ? C59X C54X O5X 121.3(9) . . ? C54X C55X C56X 120.0 . . ? C57X C56X C55X 120.0 . . ? O4X C57X C58X 117.4(9) . . ? O4X C57X C56X 122.6(9) . . ? C58X C57X C56X 120.0 . . ? C57X C58X C59X 120.0 . . ? C58X C59X C54X 120.0 . . ? _diffrn_measured_fraction_theta_max 0.888 _diffrn_reflns_theta_full 19.00 _diffrn_measured_fraction_theta_full 0.888 _refine_diff_density_max 0.981 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.143 # Attachment '6.cif' data_dw0517#(6.2toluene) _database_code_depnum_ccdc_archive 'CCDC 608774' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H56 N8 O2, 2(C7 H8)' _chemical_formula_sum 'C54 H72 N8 O2 P4' _chemical_formula_weight 989.08 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.832(4) _cell_length_b 13.419(3) _cell_length_c 23.479(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.05(3) _cell_angle_gamma 90.00 _cell_volume 5615(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 23498 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.49 _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 0.180 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.867 _exptl_absorpt_correction_T_max 0.997 _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 22915 _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_sigmaI/netI 0.1052 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 24.00 _reflns_number_total 8650 _reflns_number_gt 5368 _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^)+(0.0811P)^2^+0.7060P] 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 8650 _refine_ls_number_parameters 580 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1645 _refine_ls_wR_factor_gt 0.1465 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _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 0.86229(5) 0.78621(7) 0.17548(4) 0.0296(3) Uani 1 1 d . . . N1 N 0.91110(15) 0.8457(2) 0.12354(11) 0.0311(7) Uani 1 1 d . . . C1 C 0.9948(2) 0.8495(3) 0.11879(15) 0.0373(9) Uani 1 1 d . . . C11 C 1.0267(2) 0.7462(3) 0.1083(2) 0.0624(13) Uani 1 1 d . . . H11A H 1.0171 0.7032 0.1409 0.094 Uiso 1 1 calc R . . H11B H 1.0809 0.7512 0.1034 0.094 Uiso 1 1 calc R . . H11C H 1.0027 0.7178 0.0738 0.094 Uiso 1 1 calc R . . C12 C 1.0114(2) 0.9199(3) 0.07006(18) 0.0545(12) Uani 1 1 d . . . H12A H 0.9911 0.8918 0.0342 0.082 Uiso 1 1 calc R . . H12B H 1.0657 0.9285 0.0678 0.082 Uiso 1 1 calc R . . H12C H 0.9879 0.9846 0.0768 0.082 Uiso 1 1 calc R . . C13 C 1.0282(2) 0.8920(3) 0.17447(16) 0.0470(11) Uani 1 1 d . . . H13A H 1.0072 0.9583 0.1810 0.071 Uiso 1 1 calc R . . H13B H 1.0828 0.8970 0.1720 0.071 Uiso 1 1 calc R . . H13C H 1.0160 0.8479 0.2061 0.071 Uiso 1 1 calc R . . P2 P 0.84937(5) 0.82422(7) 0.06728(4) 0.0325(3) Uani 1 1 d . . . N2 N 0.79276(15) 0.7945(2) 0.12263(12) 0.0329(7) Uani 1 1 d . . . C2 C 0.7230(2) 0.7350(3) 0.11713(16) 0.0373(9) Uani 1 1 d . . . C21 C 0.6789(2) 0.7492(3) 0.17045(18) 0.0535(11) Uani 1 1 d . . . H21A H 0.7087 0.7258 0.2037 0.080 Uiso 1 1 calc R . . H21B H 0.6321 0.7110 0.1671 0.080 Uiso 1 1 calc R . . H21C H 0.6672 0.8201 0.1751 0.080 Uiso 1 1 calc R . . C22 C 0.7416(2) 0.6244(3) 0.1099(2) 0.0575(12) Uani 1 1 d . . . H22A H 0.7703 0.6154 0.0754 0.086 Uiso 1 1 calc R . . H22B H 0.6950 0.5859 0.1065 0.086 Uiso 1 1 calc R . . H22C H 0.7716 0.6012 0.1431 0.086 Uiso 1 1 calc R . . C23 C 0.6782(2) 0.7728(3) 0.06457(18) 0.0583(12) Uani 1 1 d . . . H23A H 0.6693 0.8445 0.0683 0.087 Uiso 1 1 calc R . . H23B H 0.6299 0.7378 0.0615 0.087 Uiso 1 1 calc R . . H23C H 0.7065 0.7601 0.0303 0.087 Uiso 1 1 calc R . . N5 N 0.82026(18) 0.9385(2) 0.04654(13) 0.0366(8) Uani 1 1 d . . . H5N H 0.8084(18) 0.980(2) 0.0714(14) 0.024(10) Uiso 1 1 d . . . C51 C 0.80686(19) 0.9722(3) -0.00946(14) 0.0316(9) Uani 1 1 d . . . C52 C 0.8132(2) 0.9084(3) -0.05583(15) 0.0377(9) Uani 1 1 d . . . H52 H 0.8283 0.8412 -0.0497 0.045 Uiso 1 1 calc R . . C53 C 0.7979(2) 0.9421(3) -0.11077(14) 0.0355(9) Uani 1 1 d . . . H53 H 0.8016 0.8976 -0.1420 0.043 Uiso 1 1 calc R . . C54 C 0.77746(19) 1.0391(3) -0.12026(13) 0.0294(8) Uani 1 1 d . . . C55 C 0.7731(2) 1.1040(3) -0.07527(14) 0.0335(9) Uani 1 1 d . . . H55 H 0.7600 1.1718 -0.0818 0.040 Uiso 1 1 calc R . . C56 C 0.78794(19) 1.0699(3) -0.02012(14) 0.0316(9) Uani 1 1 d . . . H56 H 0.7850 1.1150 0.0109 0.038 Uiso 1 1 calc R . . O1 O 0.76420(14) 1.06545(17) -0.17750(9) 0.0378(6) Uani 1 1 d . . . C61 C 0.7349(2) 1.1603(3) -0.18935(14) 0.0323(9) Uani 1 1 d . . . C62 C 0.7782(2) 1.2252(3) -0.21998(14) 0.0325(9) Uani 1 1 d . . . H62 H 0.8264 1.2056 -0.2318 0.039 Uiso 1 1 calc R . . C63 C 0.75075(19) 1.3185(3) -0.23321(14) 0.0333(9) Uani 1 1 d . . . H63 H 0.7803 1.3629 -0.2545 0.040 Uiso 1 1 calc R . . C64 C 0.68063(19) 1.3489(3) -0.21600(13) 0.0274(8) Uani 1 1 d . . . C65 C 0.6370(2) 1.2815(3) -0.18763(14) 0.0327(9) Uani 1 1 d . . . H65 H 0.5879 1.2999 -0.1773 0.039 Uiso 1 1 calc R . . C66 C 0.6642(2) 1.1865(3) -0.17394(14) 0.0331(9) Uani 1 1 d . . . H66 H 0.6340 1.1406 -0.1542 0.040 Uiso 1 1 calc R . . N6 N 0.65460(17) 1.4480(2) -0.22570(13) 0.0334(8) Uani 1 1 d . . . H6N H 0.6721(18) 1.475(3) -0.2529(15) 0.027(10) Uiso 1 1 d . . . P3 P 0.65171(5) 1.53711(7) -0.17436(4) 0.0299(3) Uani 1 1 d . . . N3 N 0.72083(15) 1.5089(2) -0.12335(12) 0.0312(7) Uani 1 1 d . . . C3 C 0.7978(2) 1.5512(3) -0.11865(16) 0.0384(9) Uani 1 1 d . . . C31 C 0.7925(3) 1.6607(4) -0.1055(4) 0.139(3) Uani 1 1 d . . . H31A H 0.7590 1.6930 -0.1339 0.208 Uiso 1 1 calc R . . H31B H 0.8425 1.6908 -0.1065 0.208 Uiso 1 1 calc R . . H31C H 0.7725 1.6696 -0.0675 0.208 Uiso 1 1 calc R . . C32 C 0.8358(3) 1.5399(5) -0.1741(2) 0.0824(18) Uani 1 1 d . . . H32A H 0.8412 1.4689 -0.1829 0.124 Uiso 1 1 calc R . . H32B H 0.8855 1.5711 -0.1713 0.124 Uiso 1 1 calc R . . H32C H 0.8055 1.5722 -0.2045 0.124 Uiso 1 1 calc R . . C33 C 0.8408(3) 1.4974(6) -0.0734(3) 0.117(3) Uani 1 1 d . . . H33A H 0.8162 1.5059 -0.0370 0.176 Uiso 1 1 calc R . . H33B H 0.8919 1.5242 -0.0701 0.176 Uiso 1 1 calc R . . H33C H 0.8428 1.4264 -0.0829 0.176 Uiso 1 1 calc R . . P4 P 0.66329(5) 1.48662(7) -0.06807(4) 0.0306(3) Uani 1 1 d . . . N4 N 0.59712(15) 1.4856(2) -0.12317(11) 0.0297(7) Uani 1 1 d . . . C4 C 0.5161(2) 1.5091(3) -0.11581(16) 0.0393(10) Uani 1 1 d . . . C41 C 0.5064(2) 1.6152(3) -0.09447(19) 0.0583(12) Uani 1 1 d . . . H41A H 0.5354 1.6240 -0.0586 0.087 Uiso 1 1 calc R . . H41B H 0.4532 1.6279 -0.0882 0.087 Uiso 1 1 calc R . . H41C H 0.5244 1.6621 -0.1229 0.087 Uiso 1 1 calc R . . C42 C 0.4743(2) 1.4946(4) -0.17343(18) 0.0586(13) Uani 1 1 d . . . H42A H 0.4926 1.5432 -0.2008 0.088 Uiso 1 1 calc R . . H42B H 0.4204 1.5044 -0.1688 0.088 Uiso 1 1 calc R . . H42C H 0.4833 1.4270 -0.1874 0.088 Uiso 1 1 calc R . . C43 C 0.4872(2) 1.4333(3) -0.07308(17) 0.0491(11) Uani 1 1 d . . . H43A H 0.4920 1.3659 -0.0886 0.074 Uiso 1 1 calc R . . H43B H 0.4344 1.4471 -0.0660 0.074 Uiso 1 1 calc R . . H43C H 0.5168 1.4384 -0.0372 0.074 Uiso 1 1 calc R . . N7 N 0.67449(18) 1.3640(2) -0.05119(13) 0.0333(8) Uani 1 1 d . . . H7N H 0.666(2) 1.326(3) -0.0765(17) 0.047(13) Uiso 1 1 d . . . C71 C 0.67812(19) 1.3279(3) 0.00519(14) 0.0295(8) Uani 1 1 d . . . C72 C 0.7148(2) 1.3818(3) 0.04804(15) 0.0380(9) Uani 1 1 d . . . H72 H 0.7381 1.4433 0.0392 0.046 Uiso 1 1 calc R . . C73 C 0.7182(2) 1.3474(3) 0.10351(15) 0.0421(10) Uani 1 1 d . . . H73 H 0.7433 1.3852 0.1326 0.050 Uiso 1 1 calc R . . C74 C 0.6853(2) 1.2590(3) 0.11625(14) 0.0346(9) Uani 1 1 d . . . C75 C 0.6489(2) 1.2033(3) 0.07495(15) 0.0367(9) Uani 1 1 d . . . H75 H 0.6264 1.1415 0.0842 0.044 Uiso 1 1 calc R . . C76 C 0.6454(2) 1.2385(3) 0.01950(14) 0.0341(9) Uani 1 1 d . . . H76 H 0.6200 1.2004 -0.0093 0.041 Uiso 1 1 calc R . . O2 O 0.68598(15) 1.22781(18) 0.17372(10) 0.0422(7) Uani 1 1 d . . . C81 C 0.7269(2) 1.1405(2) 0.18631(14) 0.0302(8) Uani 1 1 d . . . C82 C 0.6977(2) 1.0744(3) 0.22397(14) 0.0354(9) Uani 1 1 d . . . H82 H 0.6514 1.0883 0.2411 0.042 Uiso 1 1 calc R . . C83 C 0.7362(2) 0.9870(3) 0.23695(14) 0.0308(8) Uani 1 1 d . . . H83 H 0.7151 0.9402 0.2621 0.037 Uiso 1 1 calc R . . C84 C 0.80514(19) 0.9667(2) 0.21381(14) 0.0284(8) Uani 1 1 d . . . C85 C 0.8352(2) 1.0376(3) 0.17817(15) 0.0342(9) Uani 1 1 d . . . H85 H 0.8834 1.0265 0.1633 0.041 Uiso 1 1 calc R . . C86 C 0.7967(2) 1.1244(3) 0.16363(15) 0.0355(9) Uani 1 1 d . . . H86 H 0.8177 1.1718 0.1387 0.043 Uiso 1 1 calc R . . N8 N 0.84314(16) 0.8750(2) 0.22428(13) 0.0308(7) Uani 1 1 d . . . H8N H 0.836(2) 0.852(3) 0.2555(18) 0.056(14) Uiso 1 1 d . . . C1T C 0.9716(3) 0.2961(4) 0.1464(3) 0.098(3) Uiso 0.639(5) 1 d PG A 1 C2T C 0.9497(3) 0.3816(5) 0.17480(19) 0.115(5) Uiso 0.639(5) 1 d PG A 1 H2T H 0.9517 0.3833 0.2153 0.138 Uiso 0.639(5) 1 calc PR A 1 C3T C 0.9249(3) 0.4644(4) 0.1440(3) 0.093(2) Uiso 0.639(5) 1 d PG A 1 H3T H 0.9099 0.5228 0.1635 0.111 Uiso 0.639(5) 1 calc PR A 1 C4T C 0.9220(3) 0.4619(4) 0.0848(2) 0.086(3) Uiso 0.639(5) 1 d PG A 1 H4T H 0.9050 0.5185 0.0638 0.103 Uiso 0.639(5) 1 calc PR A 1 C5T C 0.9439(4) 0.3764(5) 0.05636(19) 0.104(3) Uiso 0.639(5) 1 d PG A 1 H5T H 0.9419 0.3747 0.0159 0.124 Uiso 0.639(5) 1 calc PR A 1 C6T C 0.9687(4) 0.2935(4) 0.0871(3) 0.111(5) Uiso 0.639(5) 1 d PG A 1 H6T H 0.9837 0.2351 0.0677 0.133 Uiso 0.639(5) 1 calc PR A 1 C7T C 0.9995(5) 0.2284(6) 0.1870(4) 0.244(10) Uiso 0.639(5) 1 d PG A 1 H7T1 H 1.0508 0.2473 0.1989 0.365 Uiso 0.639(5) 1 calc PR A 1 H7T2 H 0.9998 0.1614 0.1704 0.365 Uiso 0.639(5) 1 calc PR A 1 H7T3 H 0.9676 0.2290 0.2201 0.365 Uiso 0.639(5) 1 calc PR A 1 C1T' C 0.9489(2) 0.3668(5) 0.1133(3) 0.098(3) Uiso 0.361(5) 1 d PG A 2 C2T' C 0.9796(2) 0.2819(6) 0.0895(3) 0.115(5) Uiso 0.361(5) 1 d PG A 2 H2T' H 0.9818 0.2759 0.0493 0.138 Uiso 0.361(5) 1 calc PR A 2 C3T' C 1.00701(17) 0.2057(6) 0.1246(3) 0.093(2) Uiso 0.361(5) 1 d PG A 2 H3T' H 1.0280 0.1477 0.1083 0.111 Uiso 0.361(5) 1 calc PR A 2 C4T' C 1.00376(16) 0.2144(6) 0.1834(3) 0.086(3) Uiso 0.361(5) 1 d PG A 2 H4T' H 1.0225 0.1624 0.2074 0.103 Uiso 0.361(5) 1 calc PR A 2 C5T' C 0.9731(2) 0.2994(6) 0.2072(3) 0.104(3) Uiso 0.361(5) 1 d PG A 2 H5T' H 0.9708 0.3053 0.2474 0.124 Uiso 0.361(5) 1 calc PR A 2 C6T' C 0.9456(2) 0.3755(5) 0.1722(3) 0.111(5) Uiso 0.361(5) 1 d PG A 2 H6T' H 0.9246 0.4336 0.1885 0.133 Uiso 0.361(5) 1 calc PR A 2 C7T' C 0.9252(3) 0.4551(5) 0.0845(4) 0.244(10) Uiso 0.361(5) 1 d PG A 2 H7T4 H 0.9630 0.4746 0.0573 0.365 Uiso 0.361(5) 1 calc PR A 2 H7T5 H 0.9190 0.5087 0.1123 0.365 Uiso 0.361(5) 1 calc PR A 2 H7T6 H 0.8773 0.4428 0.0640 0.365 Uiso 0.361(5) 1 calc PR A 2 C1U C 0.45939(14) 0.0880(2) 0.16469(13) 0.0714(14) Uani 1 1 d G . . C2U C 0.40495(15) 0.1178(2) 0.12626(17) 0.104(2) Uani 1 1 d G . . H2U H 0.3725 0.1712 0.1355 0.125 Uiso 1 1 calc R . . C3U C 0.39641(18) 0.0710(3) 0.07369(15) 0.124(3) Uani 1 1 d G . . H3U H 0.3585 0.0926 0.0470 0.148 Uiso 1 1 calc R . . C4U C 0.4429(2) -0.0069(4) 0.06028(14) 0.121(3) Uani 1 1 d G . . H4U H 0.4370 -0.0381 0.0241 0.146 Uiso 1 1 calc R . . C5U C 0.49913(18) -0.0411(2) 0.09922(18) 0.119(3) Uani 1 1 d G . . H5U H 0.5310 -0.0951 0.0900 0.143 Uiso 1 1 calc R . . C6U C 0.50638(15) 0.0076(2) 0.15237(14) 0.0833(16) Uani 1 1 d G . . H6U H 0.5432 -0.0141 0.1799 0.100 Uiso 1 1 calc R . . C7U C 0.46951(18) 0.1406(4) 0.22210(16) 0.138(3) Uani 1 1 d G . . H7U1 H 0.5182 0.1746 0.2241 0.206 Uiso 1 1 calc R . . H7U2 H 0.4676 0.0914 0.2529 0.206 Uiso 1 1 calc R . . H7U3 H 0.4293 0.1896 0.2262 0.206 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 0.0333(5) 0.0287(5) 0.0267(5) 0.0044(4) 0.0002(4) 0.0004(4) N1 0.0329(16) 0.0348(18) 0.0257(16) 0.0074(13) 0.0018(13) -0.0008(14) C1 0.033(2) 0.042(2) 0.037(2) 0.0024(18) 0.0062(17) 0.0040(18) C11 0.045(3) 0.065(3) 0.078(3) -0.004(3) 0.011(2) 0.013(2) C12 0.040(2) 0.072(3) 0.052(3) 0.012(2) 0.011(2) -0.009(2) C13 0.032(2) 0.063(3) 0.045(2) 0.004(2) -0.0059(19) -0.003(2) P2 0.0388(6) 0.0324(6) 0.0263(5) 0.0027(4) -0.0002(4) -0.0004(4) N2 0.0359(17) 0.0330(17) 0.0294(17) 0.0048(14) -0.0038(14) -0.0039(14) C2 0.035(2) 0.037(2) 0.040(2) 0.0012(18) -0.0040(18) -0.0065(18) C21 0.042(2) 0.064(3) 0.055(3) 0.000(2) 0.004(2) -0.018(2) C22 0.054(3) 0.044(3) 0.073(3) -0.006(2) -0.005(2) -0.010(2) C23 0.051(3) 0.066(3) 0.057(3) 0.011(2) -0.017(2) -0.016(2) N5 0.054(2) 0.0337(19) 0.0220(17) 0.0010(15) 0.0011(15) 0.0069(16) C51 0.033(2) 0.037(2) 0.025(2) 0.0049(17) 0.0024(16) -0.0024(17) C52 0.056(3) 0.025(2) 0.032(2) 0.0007(17) -0.0042(19) 0.0034(18) C53 0.057(2) 0.028(2) 0.021(2) -0.0028(16) -0.0005(17) 0.0001(19) C54 0.038(2) 0.033(2) 0.0176(18) -0.0001(16) 0.0034(15) 0.0021(17) C55 0.042(2) 0.030(2) 0.028(2) 0.0027(17) 0.0008(17) 0.0070(17) C56 0.040(2) 0.033(2) 0.0223(19) -0.0039(16) 0.0037(16) 0.0056(17) O1 0.0608(17) 0.0319(14) 0.0209(13) 0.0009(11) 0.0037(12) 0.0139(13) C61 0.045(2) 0.033(2) 0.0187(18) -0.0057(16) -0.0005(17) 0.0076(18) C62 0.032(2) 0.040(2) 0.027(2) -0.0027(17) 0.0051(17) 0.0077(18) C63 0.037(2) 0.036(2) 0.027(2) 0.0027(17) 0.0069(17) 0.0015(18) C64 0.038(2) 0.030(2) 0.0149(17) 0.0013(15) -0.0008(15) 0.0014(17) C65 0.033(2) 0.042(2) 0.0224(19) 0.0010(17) -0.0022(16) 0.0048(18) C66 0.042(2) 0.029(2) 0.028(2) 0.0034(16) 0.0043(17) -0.0024(18) N6 0.0407(19) 0.0371(19) 0.0227(17) 0.0095(15) 0.0060(15) 0.0032(16) P3 0.0333(5) 0.0289(5) 0.0277(5) 0.0061(4) 0.0049(4) 0.0038(4) N3 0.0309(16) 0.0343(17) 0.0284(16) 0.0035(13) 0.0003(13) -0.0013(14) C3 0.032(2) 0.043(2) 0.040(2) -0.0027(19) -0.0019(17) -0.0015(18) C31 0.070(4) 0.072(4) 0.277(10) -0.089(5) 0.038(5) -0.032(3) C32 0.046(3) 0.144(5) 0.058(3) -0.004(3) 0.007(2) -0.043(3) C33 0.043(3) 0.190(7) 0.116(5) 0.084(5) -0.035(3) -0.035(4) P4 0.0390(6) 0.0286(5) 0.0241(5) 0.0015(4) 0.0020(4) 0.0013(4) N4 0.0293(16) 0.0346(17) 0.0253(16) 0.0037(13) 0.0033(13) 0.0043(13) C4 0.030(2) 0.048(2) 0.039(2) 0.0063(19) 0.0046(18) 0.0112(18) C41 0.054(3) 0.054(3) 0.068(3) 0.007(2) 0.018(2) 0.023(2) C42 0.031(2) 0.095(4) 0.050(3) 0.021(3) -0.004(2) 0.010(2) C43 0.038(2) 0.066(3) 0.044(2) 0.012(2) 0.0138(19) -0.006(2) N7 0.045(2) 0.0299(18) 0.0243(17) 0.0001(15) -0.0028(15) 0.0028(15) C71 0.033(2) 0.031(2) 0.025(2) 0.0031(16) 0.0019(16) 0.0032(17) C72 0.047(2) 0.035(2) 0.031(2) 0.0062(18) -0.0036(18) -0.0096(19) C73 0.060(3) 0.041(2) 0.026(2) -0.0034(18) -0.0048(19) -0.004(2) C74 0.044(2) 0.034(2) 0.026(2) 0.0005(17) 0.0035(18) 0.0121(19) C75 0.051(2) 0.026(2) 0.034(2) 0.0016(17) 0.0063(19) 0.0024(18) C76 0.044(2) 0.032(2) 0.026(2) 0.0004(17) 0.0000(17) -0.0036(18) O2 0.0665(18) 0.0371(15) 0.0233(14) 0.0036(11) 0.0051(13) 0.0196(14) C81 0.046(2) 0.027(2) 0.0181(18) -0.0052(16) -0.0035(17) 0.0090(18) C82 0.044(2) 0.038(2) 0.025(2) -0.0008(18) 0.0107(17) 0.0011(19) C83 0.043(2) 0.028(2) 0.0220(19) 0.0024(16) 0.0066(17) -0.0010(18) C84 0.037(2) 0.026(2) 0.0214(18) -0.0021(16) -0.0040(16) -0.0036(17) C85 0.032(2) 0.037(2) 0.033(2) 0.0006(18) 0.0043(17) -0.0025(18) C86 0.050(2) 0.029(2) 0.028(2) 0.0033(16) 0.0042(18) 0.0013(19) N8 0.0378(18) 0.0326(18) 0.0221(17) 0.0083(14) 0.0006(14) 0.0015(14) C1U 0.049(3) 0.086(4) 0.079(4) -0.001(3) 0.004(3) -0.012(3) C2U 0.056(4) 0.117(5) 0.137(6) 0.034(5) -0.014(4) -0.011(3) C3U 0.125(6) 0.163(8) 0.083(5) 0.035(5) -0.012(4) -0.062(6) C4U 0.120(6) 0.145(7) 0.101(5) -0.037(5) 0.042(5) -0.085(6) C5U 0.086(5) 0.106(5) 0.168(8) -0.037(5) 0.053(5) -0.037(4) C6U 0.060(3) 0.088(4) 0.102(5) -0.008(4) 0.003(3) -0.005(3) C7U 0.105(5) 0.197(8) 0.112(6) -0.069(6) 0.020(4) -0.023(5) _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 N8 1.696(3) . ? P1 N1 1.720(3) . ? P1 N2 1.726(3) . ? P1 P2 2.5934(14) . ? N1 C1 1.502(4) . ? N1 P2 1.713(3) . ? C1 C12 1.520(5) . ? C1 C11 1.522(5) . ? C1 C13 1.527(5) . ? P2 N5 1.686(3) . ? P2 N2 1.721(3) . ? N2 C2 1.479(4) . ? C2 C21 1.515(5) . ? C2 C23 1.533(5) . ? C2 C22 1.532(5) . ? N5 C51 1.403(4) . ? C51 C56 1.374(5) . ? C51 C52 1.393(5) . ? C52 C53 1.385(5) . ? C53 C54 1.368(5) . ? C54 C55 1.373(5) . ? C54 O1 1.401(4) . ? C55 C56 1.390(5) . ? O1 C61 1.400(4) . ? C61 C66 1.369(5) . ? C61 C62 1.383(5) . ? C62 C63 1.375(5) . ? C63 C64 1.389(5) . ? C64 C65 1.380(5) . ? C64 N6 1.424(4) . ? C65 C66 1.398(5) . ? N6 P3 1.700(3) . ? P3 N4 1.718(3) . ? P3 N3 1.730(3) . ? P3 P4 2.5871(13) . ? N3 C3 1.487(4) . ? N3 P4 1.709(3) . ? C3 C33 1.477(6) . ? C3 C32 1.497(6) . ? C3 C31 1.505(6) . ? P4 N7 1.702(3) . ? P4 N4 1.720(3) . ? N4 C4 1.495(4) . ? C4 C41 1.522(5) . ? C4 C43 1.530(5) . ? C4 C42 1.533(5) . ? N7 C71 1.409(4) . ? C71 C76 1.381(5) . ? C71 C72 1.384(5) . ? C72 C73 1.381(5) . ? C73 C74 1.361(5) . ? C74 C75 1.370(5) . ? C74 O2 1.413(4) . ? C75 C76 1.385(5) . ? O2 C81 1.406(4) . ? C81 C82 1.368(5) . ? C81 C86 1.388(5) . ? C82 C83 1.388(5) . ? C83 C84 1.388(5) . ? C84 C85 1.387(5) . ? C84 N8 1.423(4) . ? C85 C86 1.389(5) . ? C1T C2T 1.3900 . ? C1T C6T 1.3900 . ? C1T C7T 1.3958 . ? C2T C3T 1.3900 . ? C3T C4T 1.3900 . ? C4T C5T 1.3900 . ? C5T C6T 1.3900 . ? C1T' C2T' 1.3900 . ? C1T' C6T' 1.3900 . ? C1T' C7T' 1.4213 . ? C2T' C3T' 1.3900 . ? C3T' C4T' 1.3900 . ? C4T' C5T' 1.3900 . ? C5T' C6T' 1.3900 . ? C1U C2U 1.3617 . ? C1U C6U 1.4021 . ? C1U C7U 1.5266 . ? C2U C3U 1.3886 . ? C3U C4U 1.3776 . ? C4U C5U 1.4093 . ? C5U C6U 1.4108 . ? 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 N8 P1 N1 105.80(15) . . ? N8 P1 N2 106.49(15) . . ? N1 P1 N2 80.15(14) . . ? N8 P1 P2 120.71(11) . . ? N1 P1 P2 40.85(10) . . ? N2 P1 P2 41.12(10) . . ? C1 N1 P2 124.2(2) . . ? C1 N1 P1 126.7(2) . . ? P2 N1 P1 98.11(15) . . ? N1 C1 C12 107.3(3) . . ? N1 C1 C11 111.1(3) . . ? C12 C1 C11 111.1(3) . . ? N1 C1 C13 107.9(3) . . ? C12 C1 C13 109.4(3) . . ? C11 C1 C13 110.0(3) . . ? N5 P2 N1 104.62(15) . . ? N5 P2 N2 104.27(15) . . ? N1 P2 N2 80.49(13) . . ? N5 P2 P1 118.53(12) . . ? N1 P2 P1 41.04(9) . . ? N2 P2 P1 41.28(10) . . ? C2 N2 P2 125.0(2) . . ? C2 N2 P1 127.4(2) . . ? P2 N2 P1 97.60(15) . . ? N2 C2 C21 108.7(3) . . ? N2 C2 C23 107.8(3) . . ? C21 C2 C23 110.6(3) . . ? N2 C2 C22 110.3(3) . . ? C21 C2 C22 109.6(3) . . ? C23 C2 C22 109.9(3) . . ? C51 N5 P2 127.2(3) . . ? C56 C51 C52 118.0(3) . . ? C56 C51 N5 120.7(3) . . ? C52 C51 N5 121.3(3) . . ? C53 C52 C51 120.6(3) . . ? C54 C53 C52 120.3(3) . . ? C53 C54 C55 120.0(3) . . ? C53 C54 O1 115.5(3) . . ? C55 C54 O1 124.4(3) . . ? C54 C55 C56 119.6(3) . . ? C51 C56 C55 121.4(3) . . ? C61 O1 C54 118.0(2) . . ? C66 C61 C62 120.8(3) . . ? C66 C61 O1 121.4(3) . . ? C62 C61 O1 117.7(3) . . ? C63 C62 C61 119.4(3) . . ? C62 C63 C64 121.2(3) . . ? C65 C64 C63 118.4(3) . . ? C65 C64 N6 120.2(3) . . ? C63 C64 N6 121.3(3) . . ? C64 C65 C66 120.8(3) . . ? C61 C66 C65 119.2(3) . . ? C64 N6 P3 124.1(2) . . ? N6 P3 N4 104.21(16) . . ? N6 P3 N3 107.34(15) . . ? N4 P3 N3 80.51(13) . . ? N6 P3 P4 119.77(12) . . ? N4 P3 P4 41.22(10) . . ? N3 P3 P4 40.91(9) . . ? C3 N3 P4 126.0(2) . . ? C3 N3 P3 126.9(2) . . ? P4 N3 P3 97.58(14) . . ? C33 C3 N3 108.7(3) . . ? C33 C3 C32 109.8(4) . . ? N3 C3 C32 110.0(3) . . ? C33 C3 C31 111.4(5) . . ? N3 C3 C31 108.9(3) . . ? C32 C3 C31 108.2(5) . . ? N7 P4 N3 106.08(15) . . ? N7 P4 N4 103.85(15) . . ? N3 P4 N4 81.05(13) . . ? N7 P4 P3 118.84(12) . . ? N3 P4 P3 41.51(10) . . ? N4 P4 P3 41.17(9) . . ? C4 N4 P3 124.8(2) . . ? C4 N4 P4 123.5(2) . . ? P3 N4 P4 97.61(14) . . ? N4 C4 C41 110.9(3) . . ? N4 C4 C43 106.6(3) . . ? C41 C4 C43 111.2(3) . . ? N4 C4 C42 108.2(3) . . ? C41 C4 C42 110.6(3) . . ? C43 C4 C42 109.3(3) . . ? C71 N7 P4 123.5(3) . . ? C76 C71 C72 118.0(3) . . ? C76 C71 N7 121.4(3) . . ? C72 C71 N7 120.5(3) . . ? C71 C72 C73 121.0(3) . . ? C74 C73 C72 119.6(4) . . ? C73 C74 C75 121.2(3) . . ? C73 C74 O2 118.6(3) . . ? C75 C74 O2 120.1(3) . . ? C74 C75 C76 118.9(3) . . ? C71 C76 C75 121.4(3) . . ? C81 O2 C74 115.8(2) . . ? C82 C81 C86 120.9(3) . . ? C82 C81 O2 118.0(3) . . ? C86 C81 O2 121.0(3) . . ? C81 C82 C83 119.6(3) . . ? C84 C83 C82 121.2(3) . . ? C85 C84 C83 117.9(3) . . ? C85 C84 N8 120.4(3) . . ? C83 C84 N8 121.7(3) . . ? C84 C85 C86 121.7(3) . . ? C81 C86 C85 118.6(3) . . ? C84 N8 P1 126.7(2) . . ? C2T C1T C6T 120.0 . . ? C2T C1T C7T 107.9 . . ? C6T C1T C7T 131.8 . . ? C1T C2T C3T 120.0 . . ? C2T C3T C4T 120.0 . . ? C5T C4T C3T 120.0 . . ? C4T C5T C6T 120.0 . . ? C5T C6T C1T 120.0 . . ? C2T' C1T' C6T' 120.0 . . ? C2T' C1T' C7T' 127.3 . . ? C6T' C1T' C7T' 112.4 . . ? C3T' C2T' C1T' 120.0 . . ? C2T' C3T' C4T' 120.0 . . ? C5T' C4T' C3T' 120.0 . . ? C4T' C5T' C6T' 120.0 . . ? C5T' C6T' C1T' 120.0 . . ? C2U C1U C6U 120.4 . . ? C2U C1U C7U 120.5 . . ? C6U C1U C7U 119.0 . . ? C1U C2U C3U 120.6 . . ? C4U C3U C2U 119.9 . . ? C3U C4U C5U 121.3 . . ? C4U C5U C6U 117.6 . . ? C1U C6U C5U 120.2 . . ? 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 N8 P1 N1 C1 96.5(3) . . . . ? N2 P1 N1 C1 -159.0(3) . . . . ? P2 P1 N1 C1 -144.5(4) . . . . ? N8 P1 N1 P2 -118.96(15) . . . . ? N2 P1 N1 P2 -14.47(14) . . . . ? P2 N1 C1 C12 50.2(4) . . . . ? P1 N1 C1 C12 -173.8(3) . . . . ? P2 N1 C1 C11 -71.4(4) . . . . ? P1 N1 C1 C11 64.6(4) . . . . ? P2 N1 C1 C13 168.0(3) . . . . ? P1 N1 C1 C13 -56.0(4) . . . . ? C1 N1 P2 N5 -97.3(3) . . . . ? P1 N1 P2 N5 116.89(16) . . . . ? C1 N1 P2 N2 160.3(3) . . . . ? P1 N1 P2 N2 14.50(14) . . . . ? C1 N1 P2 P1 145.8(3) . . . . ? N8 P1 P2 N5 -0.91(19) . . . . ? N1 P1 P2 N5 -79.2(2) . . . . ? N2 P1 P2 N5 78.8(2) . . . . ? N8 P1 P2 N1 78.30(19) . . . . ? N2 P1 P2 N1 158.0(2) . . . . ? N8 P1 P2 N2 -79.72(19) . . . . ? N1 P1 P2 N2 -158.0(2) . . . . ? N5 P2 N2 C2 95.4(3) . . . . ? N1 P2 N2 C2 -161.8(3) . . . . ? P1 P2 N2 C2 -147.4(3) . . . . ? N5 P2 N2 P1 -117.22(16) . . . . ? N1 P2 N2 P1 -14.43(14) . . . . ? N8 P1 N2 C2 -95.7(3) . . . . ? N1 P1 N2 C2 160.6(3) . . . . ? P2 P1 N2 C2 146.2(4) . . . . ? N8 P1 N2 P2 118.09(15) . . . . ? N1 P1 N2 P2 14.39(14) . . . . ? P2 N2 C2 C21 -164.4(3) . . . . ? P1 N2 C2 C21 57.9(4) . . . . ? P2 N2 C2 C23 -44.5(4) . . . . ? P1 N2 C2 C23 177.8(3) . . . . ? P2 N2 C2 C22 75.4(4) . . . . ? P1 N2 C2 C22 -62.3(4) . . . . ? N1 P2 N5 C51 141.0(3) . . . . ? N2 P2 N5 C51 -135.3(3) . . . . ? P1 P2 N5 C51 -177.2(3) . . . . ? P2 N5 C51 C56 -175.7(3) . . . . ? P2 N5 C51 C52 3.5(5) . . . . ? C56 C51 C52 C53 -2.6(5) . . . . ? N5 C51 C52 C53 178.3(3) . . . . ? C51 C52 C53 C54 1.1(6) . . . . ? C52 C53 C54 C55 0.9(5) . . . . ? C52 C53 C54 O1 179.2(3) . . . . ? C53 C54 C55 C56 -1.4(5) . . . . ? O1 C54 C55 C56 -179.5(3) . . . . ? C52 C51 C56 C55 2.1(5) . . . . ? N5 C51 C56 C55 -178.8(3) . . . . ? C54 C55 C56 C51 -0.1(5) . . . . ? C53 C54 O1 C61 172.8(3) . . . . ? C55 C54 O1 C61 -9.0(5) . . . . ? C54 O1 C61 C66 -65.9(4) . . . . ? C54 O1 C61 C62 117.5(3) . . . . ? C66 C61 C62 C63 2.4(5) . . . . ? O1 C61 C62 C63 179.0(3) . . . . ? C61 C62 C63 C64 0.5(5) . . . . ? C62 C63 C64 C65 -3.3(5) . . . . ? C62 C63 C64 N6 174.9(3) . . . . ? C63 C64 C65 C66 3.2(5) . . . . ? N6 C64 C65 C66 -175.0(3) . . . . ? C62 C61 C66 C65 -2.4(5) . . . . ? O1 C61 C66 C65 -178.9(3) . . . . ? C64 C65 C66 C61 -0.4(5) . . . . ? C65 C64 N6 P3 74.1(4) . . . . ? C63 C64 N6 P3 -104.1(3) . . . . ? C64 N6 P3 N4 -57.1(3) . . . . ? C64 N6 P3 N3 27.2(3) . . . . ? C64 N6 P3 P4 -15.6(3) . . . . ? N6 P3 N3 C3 96.9(3) . . . . ? N4 P3 N3 C3 -161.1(3) . . . . ? P4 P3 N3 C3 -147.4(4) . . . . ? N6 P3 N3 P4 -115.72(16) . . . . ? N4 P3 N3 P4 -13.68(14) . . . . ? P4 N3 C3 C33 48.2(5) . . . . ? P3 N3 C3 C33 -173.1(4) . . . . ? P4 N3 C3 C32 168.3(3) . . . . ? P3 N3 C3 C32 -53.0(5) . . . . ? P4 N3 C3 C31 -73.3(5) . . . . ? P3 N3 C3 C31 65.4(5) . . . . ? C3 N3 P4 N7 -96.6(3) . . . . ? P3 N3 P4 N7 115.58(16) . . . . ? C3 N3 P4 N4 161.5(3) . . . . ? P3 N3 P4 N4 13.65(14) . . . . ? C3 N3 P4 P3 147.8(4) . . . . ? N6 P3 P4 N7 0.54(19) . . . . ? N4 P3 P4 N7 77.6(2) . . . . ? N3 P3 P4 N7 -81.65(19) . . . . ? N6 P3 P4 N3 82.19(19) . . . . ? N4 P3 P4 N3 159.3(2) . . . . ? N6 P3 P4 N4 -77.07(19) . . . . ? N3 P3 P4 N4 -159.3(2) . . . . ? N6 P3 N4 C4 -100.4(3) . . . . ? N3 P3 N4 C4 154.0(3) . . . . ? P4 P3 N4 C4 140.4(3) . . . . ? N6 P3 N4 P4 119.22(15) . . . . ? N3 P3 N4 P4 13.60(14) . . . . ? N7 P4 N4 C4 100.7(3) . . . . ? N3 P4 N4 C4 -154.8(3) . . . . ? P3 P4 N4 C4 -141.1(3) . . . . ? N7 P4 N4 P3 -118.22(15) . . . . ? N3 P4 N4 P3 -13.74(14) . . . . ? P3 N4 C4 C41 -68.9(4) . . . . ? P4 N4 C4 C41 61.8(4) . . . . ? P3 N4 C4 C43 169.9(3) . . . . ? P4 N4 C4 C43 -59.4(4) . . . . ? P3 N4 C4 C42 52.5(4) . . . . ? P4 N4 C4 C42 -176.8(3) . . . . ? N3 P4 N7 C71 139.8(3) . . . . ? N4 P4 N7 C71 -135.7(3) . . . . ? P3 P4 N7 C71 -177.2(2) . . . . ? P4 N7 C71 C76 142.1(3) . . . . ? P4 N7 C71 C72 -37.8(5) . . . . ? C76 C71 C72 C73 -0.5(5) . . . . ? N7 C71 C72 C73 179.5(3) . . . . ? C71 C72 C73 C74 0.4(6) . . . . ? C72 C73 C74 C75 0.1(6) . . . . ? C72 C73 C74 O2 -176.7(3) . . . . ? C73 C74 C75 C76 -0.4(5) . . . . ? O2 C74 C75 C76 176.3(3) . . . . ? C72 C71 C76 C75 0.1(5) . . . . ? N7 C71 C76 C75 -179.8(3) . . . . ? C74 C75 C76 C71 0.4(5) . . . . ? C73 C74 O2 C81 -115.4(4) . . . . ? C75 C74 O2 C81 67.7(4) . . . . ? C74 O2 C81 C82 -140.7(3) . . . . ? C74 O2 C81 C86 42.8(4) . . . . ? C86 C81 C82 C83 -4.1(5) . . . . ? O2 C81 C82 C83 179.4(3) . . . . ? C81 C82 C83 C84 2.1(5) . . . . ? C82 C83 C84 C85 1.3(5) . . . . ? C82 C83 C84 N8 -176.4(3) . . . . ? C83 C84 C85 C86 -2.9(5) . . . . ? N8 C84 C85 C86 174.9(3) . . . . ? C82 C81 C86 C85 2.6(5) . . . . ? O2 C81 C86 C85 179.0(3) . . . . ? C84 C85 C86 C81 1.0(5) . . . . ? C85 C84 N8 P1 -62.5(4) . . . . ? C83 C84 N8 P1 115.2(3) . . . . ? N1 P1 N8 C84 55.5(3) . . . . ? N2 P1 N8 C84 -28.6(3) . . . . ? P2 P1 N8 C84 13.8(3) . . . . ? C6T C1T C2T C3T 0.0 . . . . ? C7T C1T C2T C3T 175.2 . . . . ? C1T C2T C3T C4T 0.0 . . . . ? C2T C3T C4T C5T 0.0 . . . . ? C3T C4T C5T C6T 0.0 . . . . ? C4T C5T C6T C1T 0.0 . . . . ? C2T C1T C6T C5T 0.0 . . . . ? C7T C1T C6T C5T -173.8 . . . . ? C6T' C1T' C2T' C3T' 0.0 . . . . ? C7T' C1T' C2T' C3T' 173.3 . . . . ? C1T' C2T' C3T' C4T' 0.0 . . . . ? C2T' C3T' C4T' C5T' 0.0 . . . . ? C3T' C4T' C5T' C6T' 0.0 . . . . ? C4T' C5T' C6T' C1T' 0.0 . . . . ? C2T' C1T' C6T' C5T' 0.0 . . . . ? C7T' C1T' C6T' C5T' -174.3 . . . . ? C6U C1U C2U C3U -1.7 . . . . ? C7U C1U C2U C3U 179.0 . . . . ? C1U C2U C3U C4U 0.5 . . . . ? C2U C3U C4U C5U 0.6 . . . . ? C3U C4U C5U C6U -0.4 . . . . ? C2U C1U C6U C5U 1.9 . . . . ? C7U C1U C6U C5U -178.8 . . . . ? C4U C5U C6U C1U -0.9 . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6N O1 0.81(3) 2.36(4) 3.159(4) 171(3) 2_654 N8 H8N O2 0.81(4) 2.40(4) 3.161(4) 158(4) 2_645 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.698 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.080 # Attachment '7.cif' # data_604 _database_code_depnum_ccdc_archive 'CCDC 608775' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 Cl2 N2 P2' _chemical_formula_weight 327.16 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' Cl Cl 0.1484 0.1585 '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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.707(3) _cell_length_b 5.4813(11) _cell_length_c 21.039(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.74(3) _cell_angle_gamma 90.00 _cell_volume 1580.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 10675 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.599 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.898 _exptl_absorpt_correction_T_max 0.971 _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_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 5658 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1545 _reflns_number_gt 1152 _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^)+(0.0544P)^2^+3.1127P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1545 _refine_ls_number_parameters 114 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.088 _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 0.17310(6) 0.05040(15) 0.21719(4) 0.0236(4) Uani 0.50 1 d PD . . P2 P 0.33049(5) 0.0000 0.28427(4) 0.0285(2) Uani 1 2 d SD . . Cl1 Cl 0.10616(8) -0.30260(19) 0.20090(6) 0.0506(4) Uani 0.50 1 d PD . . Cl2 Cl 0.35224(9) -0.38601(18) 0.30320(6) 0.0475(3) Uani 0.50 1 d PD . . N1 N 0.20945(15) 0.0000 0.29460(11) 0.0363(7) Uani 1 2 d SD . . N2 N 0.29280(15) 0.0000 0.20644(11) 0.0279(6) Uani 1 2 d SD . . C1 C 0.1525(2) -0.0383(10) 0.35235(15) 0.0240(14) Uani 0.50 1 d PD A -1 H1 H 0.1143 0.1108 0.3581 0.029 Uiso 0.50 1 calc PR A -1 C12 C 0.0802(3) -0.2447(8) 0.3488(2) 0.0326(10) Uiso 0.50 1 d PD A -1 H12A H 0.0363 -0.2213 0.3122 0.039 Uiso 0.50 1 calc PR A -1 H12B H 0.1147 -0.3973 0.3431 0.039 Uiso 0.50 1 calc PR A -1 C13 C 0.0208(3) -0.2588(9) 0.4091(2) 0.0391(11) Uiso 0.50 1 d PD A -1 H13A H -0.0213 -0.4010 0.4069 0.047 Uiso 0.50 1 calc PR A -1 H13B H -0.0202 -0.1152 0.4119 0.047 Uiso 0.50 1 calc PR A -1 C14 C 0.0873(3) -0.2749(9) 0.4683(2) 0.0349(10) Uiso 0.50 1 d PD A -1 H14A H 0.0479 -0.2702 0.5058 0.042 Uiso 0.50 1 calc PR A -1 H14B H 0.1219 -0.4293 0.4682 0.042 Uiso 0.50 1 calc PR A -1 C15 C 0.1602(3) -0.0687(7) 0.47128(18) 0.0336(11) Uiso 0.50 1 d PD A -1 H15A H 0.2039 -0.0905 0.5080 0.040 Uiso 0.50 1 calc PR A -1 H15B H 0.1261 0.0848 0.4762 0.040 Uiso 0.50 1 calc PR A -1 C16 C 0.2202(3) -0.0597(8) 0.41053(17) 0.0349(17) Uani 0.50 1 d PD A -1 H16A H 0.2641 0.0791 0.4124 0.042 Uiso 0.50 1 calc PR A -1 H16B H 0.2592 -0.2066 0.4075 0.042 Uiso 0.50 1 calc PR A -1 C2 C 0.3517(2) -0.0250(14) 0.14954(15) 0.0235(11) Uani 0.50 1 d PD A -1 H2 H 0.3974 0.1126 0.1501 0.028 Uiso 0.50 1 calc PR A -1 C22 C 0.4119(3) -0.2501(8) 0.1512(2) 0.0330(10) Uiso 0.50 1 d PD A -1 H22A H 0.4550 -0.2474 0.1887 0.040 Uiso 0.50 1 calc PR A -1 H22B H 0.3695 -0.3911 0.1543 0.040 Uiso 0.50 1 calc PR A -1 C23 C 0.4727(3) -0.2732(9) 0.0918(2) 0.0395(11) Uiso 0.50 1 d PD A -1 H23A H 0.5081 -0.4265 0.0931 0.047 Uiso 0.50 1 calc PR A -1 H23B H 0.5200 -0.1416 0.0910 0.047 Uiso 0.50 1 calc PR A -1 C24 C 0.4075(3) -0.2634(9) 0.0323(2) 0.0366(11) Uiso 0.50 1 d PD A -1 H24A H 0.4477 -0.2671 -0.0049 0.044 Uiso 0.50 1 calc PR A -1 H24B H 0.3656 -0.4059 0.0309 0.044 Uiso 0.50 1 calc PR A -1 C25 C 0.3469(3) -0.0414(9) 0.03061(17) 0.0345(10) Uiso 0.50 1 d PD A -1 H25A H 0.3026 -0.0508 -0.0061 0.041 Uiso 0.50 1 calc PR A -1 H25B H 0.3892 0.0980 0.0245 0.041 Uiso 0.50 1 calc PR A -1 C26 C 0.2859(2) 0.006(3) 0.09022(15) 0.0411(11) Uani 1 2 d SD A -1 H26A H 0.2321 -0.1087 0.0913 0.049 Uiso 0.50 1 calc PR A -1 H26B H 0.2593 0.1698 0.0888 0.049 Uiso 0.50 1 calc PR A -1 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 0.0257(4) 0.0188(11) 0.0260(5) 0.0015(4) -0.0023(3) 0.0035(4) P2 0.0257(4) 0.0351(5) 0.0245(4) 0.000 -0.0027(3) 0.000 Cl1 0.0472(6) 0.0497(8) 0.0543(8) -0.0012(7) -0.0075(5) -0.0233(6) Cl2 0.0597(7) 0.0357(6) 0.0467(7) 0.0045(6) -0.0025(5) 0.0189(6) N1 0.0229(12) 0.063(2) 0.0234(14) 0.000 0.0005(10) 0.000 N2 0.0216(12) 0.0377(15) 0.0243(13) 0.000 -0.0004(10) 0.000 C1 0.0289(16) 0.018(4) 0.0256(17) 0.0018(19) 0.0041(13) 0.0019(18) C16 0.034(2) 0.042(5) 0.029(2) 0.0003(19) -0.0005(15) -0.0117(18) C2 0.0243(15) 0.020(3) 0.0264(16) -0.001(3) 0.0024(12) -0.006(3) C26 0.0372(18) 0.056(3) 0.0295(18) 0.009(8) -0.0007(15) -0.023(6) _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 P1 0.5525(16) 6 ? P1 N1 1.711(2) . ? P1 Cl1 1.6885(14) 6 ? P1 N2 1.686(2) . ? P1 Cl1 2.1642(11) . ? P1 P2 2.5568(14) . ? P2 N2 1.702(2) . ? P2 N1 1.680(2) . ? P2 Cl2 2.1718(11) 6 ? P2 Cl2 2.1718(11) . ? P2 P1 2.5568(13) 6 ? Cl1 P1 1.6885(14) 6 ? Cl1 Cl1 2.164(2) 6_545 ? Cl2 Cl2 1.250(2) 6_545 ? N1 C1 1.479(4) . ? N1 P1 1.711(2) 6 ? N2 C2 1.471(4) . ? N2 P1 1.686(2) 6 ? C1 C16 1.518(5) . ? C1 C12 1.504(6) . ? C12 C13 1.531(6) . ? C13 C14 1.523(6) . ? C14 C15 1.509(6) . ? C15 C16 1.541(5) . ? C2 C26 1.527(5) . ? C2 C22 1.484(8) . ? C22 C23 1.529(6) . ? C23 C24 1.517(6) . ? C24 C25 1.474(6) . ? C25 C26 1.550(6) . ? 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 P1 P1 N1 80.71(3) 6 . ? P1 P1 Cl1 144.95(5) 6 6 ? N1 P1 Cl1 117.78(8) . 6 ? P1 P1 N2 80.57(3) 6 . ? N1 P1 N2 81.07(11) . . ? Cl1 P1 N2 129.20(7) 6 . ? P1 P1 Cl1 26.62(4) 6 . ? N1 P1 Cl1 96.67(6) . . ? Cl1 P1 Cl1 118.34(9) 6 . ? N2 P1 Cl1 104.00(6) . . ? P1 P1 P2 83.797(18) 6 . ? N1 P1 P2 40.60(8) . . ? Cl1 P1 P2 130.14(6) 6 . ? N2 P1 P2 41.24(8) . . ? Cl1 P1 P2 109.71(5) . . ? N2 P2 N1 81.51(11) . . ? N2 P2 Cl2 102.26(4) . 6 ? N1 P2 Cl2 96.14(4) . 6 ? N2 P2 Cl2 102.26(4) . . ? N1 P2 Cl2 96.14(4) . . ? Cl2 P2 Cl2 153.92(8) 6 . ? N2 P2 P1 40.76(7) . . ? N1 P2 P1 41.52(8) . . ? Cl2 P2 P1 96.01(4) 6 . ? Cl2 P2 P1 108.38(4) . . ? N2 P2 P1 40.76(7) . 6 ? N1 P2 P1 41.52(8) . 6 ? Cl2 P2 P1 108.38(4) 6 6 ? Cl2 P2 P1 96.01(4) . 6 ? P1 P2 P1 12.41(4) . 6 ? P1 Cl1 P1 8.43(3) 6 . ? P1 Cl1 Cl1 144.95(5) 6 6_545 ? P1 Cl1 Cl1 153.38(4) . 6_545 ? Cl2 Cl2 P2 166.96(4) 6_545 . ? C1 N1 P1 131.24(19) . . ? C1 N1 P1 127.83(19) . 6 ? P1 N1 P1 18.58(6) . 6 ? C1 N1 P2 130.9(2) . . ? P1 N1 P2 97.88(12) . . ? P1 N1 P2 97.88(12) 6 . ? C2 N2 P2 128.68(18) . . ? C2 N2 P1 133.26(19) . . ? P2 N2 P1 98.00(12) . . ? C2 N2 P1 130.9(2) . 6 ? P2 N2 P1 98.00(12) . 6 ? P1 N2 P1 18.86(6) . 6 ? N1 C1 C16 110.4(3) . . ? N1 C1 C12 115.4(3) . . ? C16 C1 C12 111.6(4) . . ? C13 C12 C1 111.3(4) . . ? C12 C13 C14 111.2(4) . . ? C15 C14 C13 111.7(4) . . ? C14 C15 C16 111.0(3) . . ? C1 C16 C15 110.0(3) . . ? N2 C2 C26 109.2(3) . . ? N2 C2 C22 112.1(4) . . ? C26 C2 C22 115.2(7) . . ? C23 C22 C2 111.5(4) . . ? C22 C23 C24 110.5(4) . . ? C25 C24 C23 111.6(4) . . ? C24 C25 C26 115.8(7) . . ? C25 C26 C2 108.9(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.532 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.086