Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_dw0110 _database_code_CSD 172095 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Bahall, Alan' 'Doyle, Emma L.' 'Kidd, Sara J.' 'McPartlin, M.' 'Tubb, Catherine' 'Woods, Anthony D.' 'Wright, Dominic' _publ_contact_author_name 'Dr Dominic Wright' _publ_contact_author_address ; Dr Dominic Wright Department of Chemistry Cambridge University Cambridge Cambridgeshire CB2 1EW UNITED KINGDOM ; _publ_contact_author_email 'DSW1000@CUS.CAM.AC.UK' _publ_section_title ; The Tetrameric Macroicycle [{P(mu-NtBu)2(mu-NH)]4. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H76 N12 P8' _chemical_formula_sum 'C32 H76 N12 P8' _chemical_formula_weight 876.81 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' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.3936(2) _cell_length_b 17.1372(4) _cell_length_c 21.7137(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4983.92(18) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 23934 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.315 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 1.021 _exptl_absorpt_correction_T_max 0.966 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (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 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'fine slice omega/phi scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25299 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8699 _reflns_number_gt 7805 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution ; SIR92: A.Altomare, G.Cascarano, C.Giacovazzo, A.Guagliardi, M.C.Burla, G.Ploidori, M.Camalli. J.Appl.Cryst. (1994) 27, 435-435 ; _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ; XP (Sheldrick, 1993) CAMERON (Watkin et al. 1996) ; _computing_publication_material ? _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^)+(0.0235P)^2^+2.2029P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(6) _refine_ls_number_reflns 8699 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.37725(5) 0.12633(4) 0.40650(3) 0.03041(16) Uani 1 1 d . . . P2 P 0.45780(5) 0.05432(4) 0.31271(3) 0.02995(16) Uani 1 1 d . . . P3 P 0.40943(5) 0.04539(4) 0.17460(3) 0.03031(16) Uani 1 1 d . . . P4 P 0.28784(5) 0.12074(4) 0.10168(3) 0.02929(16) Uani 1 1 d . . . P5 P 0.13355(5) 0.25025(4) 0.11671(3) 0.03306(17) Uani 1 1 d . . . P6 P 0.05568(5) 0.32301(4) 0.21093(4) 0.03463(18) Uani 1 1 d . . . P7 P 0.08198(5) 0.31355(4) 0.35028(4) 0.03458(17) Uani 1 1 d . . . P8 P 0.20335(5) 0.23977(4) 0.42454(3) 0.03418(18) Uani 1 1 d . . . N1 N 0.36248(16) 0.03988(12) 0.36549(9) 0.0299(5) Uani 1 1 d . . . N2 N 0.46837(14) 0.14023(13) 0.35227(10) 0.0303(5) Uani 1 1 d . . . N3 N 0.28964(15) 0.03915(12) 0.14716(10) 0.0305(5) Uani 1 1 d . . . N4 N 0.40795(14) 0.13041(13) 0.13089(9) 0.0283(5) Uani 1 1 d . . . N5 N 0.03513(14) 0.23898(13) 0.16793(10) 0.0326(5) Uani 1 1 d . . . N6 N 0.15293(15) 0.33218(13) 0.16002(11) 0.0351(5) Uani 1 1 d . . . N7 N 0.08962(15) 0.22728(13) 0.38990(10) 0.0323(5) Uani 1 1 d . . . N8 N 0.19827(16) 0.32716(13) 0.38400(11) 0.0365(6) Uani 1 1 d . . . N9 N 0.39463(16) 0.07975(13) 0.24754(10) 0.0333(5) Uani 1 1 d . . . N10 N 0.22076(15) 0.18609(13) 0.14333(10) 0.0308(5) Uani 1 1 d . . . N11 N 0.11052(16) 0.28952(13) 0.27623(10) 0.0359(6) Uani 1 1 d . . . N12 N 0.28172(15) 0.18356(13) 0.38103(10) 0.0313(5) Uani 1 1 d . . . C1 C 0.3476(2) -0.03644(15) 0.39718(13) 0.0341(6) Uani 1 1 d . . . C2 C 0.53631(19) 0.20735(16) 0.34285(13) 0.0366(7) Uani 1 1 d . . . C3 C 0.2108(2) -0.01980(15) 0.15869(13) 0.0341(6) Uani 1 1 d . . . C4 C 0.49336(19) 0.15337(17) 0.09069(13) 0.0355(7) Uani 1 1 d . . . C5 C -0.06709(19) 0.21674(18) 0.14631(13) 0.0396(7) Uani 1 1 d . . . C6 C 0.2340(2) 0.39076(17) 0.15729(15) 0.0430(8) Uani 1 1 d . . . C7 C 0.02199(19) 0.15945(17) 0.39002(13) 0.0378(7) Uani 1 1 d . . . C8 C 0.2268(2) 0.40386(18) 0.41142(16) 0.0482(8) Uani 1 1 d . . . C11 C 0.3425(2) -0.10055(16) 0.34842(14) 0.0446(8) Uani 1 1 d . . . H11A H 0.2856 -0.0909 0.3211 0.067 Uiso 1 1 calc R . . H11B H 0.3344 -0.1513 0.3686 0.067 Uiso 1 1 calc R . . H11C H 0.4044 -0.1006 0.3243 0.067 Uiso 1 1 calc R . . C12 C 0.2490(2) -0.03211(18) 0.43203(14) 0.0421(7) Uani 1 1 d . . . H12A H 0.2515 0.0110 0.4616 0.063 Uiso 1 1 calc R . . H12B H 0.2378 -0.0813 0.4540 0.063 Uiso 1 1 calc R . . H12C H 0.1944 -0.0233 0.4028 0.063 Uiso 1 1 calc R . . C13 C 0.4334(2) -0.05298(19) 0.44203(15) 0.0503(8) Uani 1 1 d . . . H13A H 0.4959 -0.0586 0.4190 0.075 Uiso 1 1 calc R . . H13B H 0.4196 -0.1013 0.4646 0.075 Uiso 1 1 calc R . . H13C H 0.4395 -0.0096 0.4712 0.075 Uiso 1 1 calc R . . C21 C 0.5516(2) 0.2463(2) 0.40488(15) 0.0543(8) Uani 1 1 d . . . H21A H 0.4874 0.2655 0.4203 0.082 Uiso 1 1 calc R . . H21B H 0.5980 0.2901 0.4003 0.082 Uiso 1 1 calc R . . H21C H 0.5792 0.2083 0.4340 0.082 Uiso 1 1 calc R . . C22 C 0.6348(2) 0.1775(2) 0.31778(17) 0.0584(9) Uani 1 1 d . . . H22A H 0.6648 0.1414 0.3475 0.088 Uiso 1 1 calc R . . H22B H 0.6801 0.2215 0.3108 0.088 Uiso 1 1 calc R . . H22C H 0.6232 0.1502 0.2788 0.088 Uiso 1 1 calc R . . C23 C 0.4890(2) 0.26433(19) 0.29760(15) 0.0527(8) Uani 1 1 d . . . H23A H 0.4704 0.2365 0.2599 0.079 Uiso 1 1 calc R . . H23B H 0.5370 0.3056 0.2876 0.079 Uiso 1 1 calc R . . H23C H 0.4293 0.2875 0.3162 0.079 Uiso 1 1 calc R . . C31 C 0.1455(2) -0.0253(2) 0.10213(15) 0.0533(9) Uani 1 1 d . . . H31A H 0.1162 0.0259 0.0934 0.080 Uiso 1 1 calc R . . H31B H 0.0920 -0.0632 0.1094 0.080 Uiso 1 1 calc R . . H31C H 0.1858 -0.0422 0.0669 0.080 Uiso 1 1 calc R . . C32 C 0.2595(2) -0.09730(17) 0.17213(17) 0.0532(9) Uani 1 1 d . . . H32A H 0.2997 -0.1134 0.1366 0.080 Uiso 1 1 calc R . . H32B H 0.2080 -0.1366 0.1802 0.080 Uiso 1 1 calc R . . H32C H 0.3027 -0.0923 0.2084 0.080 Uiso 1 1 calc R . . C33 C 0.1489(2) 0.00593(19) 0.21417(15) 0.0512(8) Uani 1 1 d . . . H33A H 0.1922 0.0099 0.2504 0.077 Uiso 1 1 calc R . . H33B H 0.0962 -0.0325 0.2220 0.077 Uiso 1 1 calc R . . H33C H 0.1186 0.0569 0.2057 0.077 Uiso 1 1 calc R . . C41 C 0.5873(2) 0.1569(2) 0.13061(15) 0.0529(9) Uani 1 1 d . . . H41A H 0.5996 0.1056 0.1491 0.079 Uiso 1 1 calc R . . H41B H 0.5781 0.1957 0.1633 0.079 Uiso 1 1 calc R . . H41C H 0.6446 0.1717 0.1051 0.079 Uiso 1 1 calc R . . C42 C 0.5074(2) 0.09479(19) 0.03813(14) 0.0504(8) Uani 1 1 d . . . H42A H 0.5219 0.0431 0.0553 0.076 Uiso 1 1 calc R . . H42B H 0.5631 0.1115 0.0120 0.076 Uiso 1 1 calc R . . H42C H 0.4462 0.0923 0.0135 0.076 Uiso 1 1 calc R . . C43 C 0.4714(2) 0.23420(18) 0.06470(14) 0.0441(7) Uani 1 1 d . . . H43A H 0.5268 0.2507 0.0382 0.066 Uiso 1 1 calc R . . H43B H 0.4637 0.2714 0.0986 0.066 Uiso 1 1 calc R . . H43C H 0.4096 0.2325 0.0405 0.066 Uiso 1 1 calc R . . C51 C -0.1121(2) 0.2816(2) 0.10727(15) 0.0554(9) Uani 1 1 d . . . H51A H -0.1191 0.3289 0.1322 0.083 Uiso 1 1 calc R . . H51B H -0.1780 0.2653 0.0923 0.083 Uiso 1 1 calc R . . H51C H -0.0684 0.2923 0.0721 0.083 Uiso 1 1 calc R . . C52 C -0.0593(2) 0.1423(2) 0.10892(17) 0.0576(9) Uani 1 1 d . . . H52A H -0.0152 0.1510 0.0736 0.086 Uiso 1 1 calc R . . H52B H -0.1258 0.1273 0.0943 0.086 Uiso 1 1 calc R . . H52C H -0.0320 0.1006 0.1347 0.086 Uiso 1 1 calc R . . C53 C -0.1321(2) 0.2036(2) 0.20322(15) 0.0615(10) Uani 1 1 d . . . H53A H -0.1040 0.1610 0.2279 0.092 Uiso 1 1 calc R . . H53B H -0.2000 0.1898 0.1903 0.092 Uiso 1 1 calc R . . H53C H -0.1340 0.2514 0.2279 0.092 Uiso 1 1 calc R . . C61 C 0.1931(3) 0.46818(18) 0.1812(2) 0.0714(12) Uani 1 1 d . . . H61A H 0.1385 0.4857 0.1545 0.107 Uiso 1 1 calc R . . H61B H 0.2465 0.5073 0.1811 0.107 Uiso 1 1 calc R . . H61C H 0.1682 0.4612 0.2232 0.107 Uiso 1 1 calc R . . C62 C 0.2656(2) 0.3992(2) 0.09004(17) 0.0621(11) Uani 1 1 d . . . H62A H 0.2878 0.3485 0.0743 0.093 Uiso 1 1 calc R . . H62B H 0.3204 0.4369 0.0871 0.093 Uiso 1 1 calc R . . H62C H 0.2088 0.4176 0.0656 0.093 Uiso 1 1 calc R . . C63 C 0.3219(2) 0.36458(19) 0.19632(15) 0.0476(8) Uani 1 1 d . . . H63A H 0.3004 0.3584 0.2392 0.071 Uiso 1 1 calc R . . H63B H 0.3750 0.4038 0.1942 0.071 Uiso 1 1 calc R . . H63C H 0.3472 0.3146 0.1808 0.071 Uiso 1 1 calc R . . C71 C -0.0855(2) 0.1892(2) 0.38470(17) 0.0546(9) Uani 1 1 d . . . H71A H -0.1011 0.2223 0.4203 0.082 Uiso 1 1 calc R . . H71B H -0.1315 0.1448 0.3837 0.082 Uiso 1 1 calc R . . H71C H -0.0927 0.2197 0.3468 0.082 Uiso 1 1 calc R . . C72 C 0.0355(2) 0.11555(19) 0.45023(14) 0.0495(8) Uani 1 1 d . . . H72A H 0.1048 0.0976 0.4537 0.074 Uiso 1 1 calc R . . H72B H -0.0095 0.0705 0.4511 0.074 Uiso 1 1 calc R . . H72C H 0.0199 0.1502 0.4848 0.074 Uiso 1 1 calc R . . C73 C 0.0475(2) 0.10604(17) 0.33595(14) 0.0479(8) Uani 1 1 d . . . H73A H 0.0397 0.1349 0.2973 0.072 Uiso 1 1 calc R . . H73B H 0.0024 0.0610 0.3360 0.072 Uiso 1 1 calc R . . H73C H 0.1166 0.0880 0.3399 0.072 Uiso 1 1 calc R . . C81 C 0.3332(3) 0.3950(2) 0.4363(2) 0.0770(13) Uani 1 1 d . . . H81A H 0.3778 0.3791 0.4029 0.115 Uiso 1 1 calc R . . H81B H 0.3340 0.3553 0.4688 0.115 Uiso 1 1 calc R . . H81C H 0.3558 0.4450 0.4533 0.115 Uiso 1 1 calc R . . C82 C 0.1558(3) 0.4276(2) 0.46314(18) 0.0721(11) Uani 1 1 d . . . H82A H 0.1732 0.4799 0.4778 0.108 Uiso 1 1 calc R . . H82B H 0.1614 0.3903 0.4972 0.108 Uiso 1 1 calc R . . H82C H 0.0870 0.4277 0.4476 0.108 Uiso 1 1 calc R . . C83 C 0.2251(3) 0.46462(18) 0.36099(18) 0.0624(10) Uani 1 1 d . . . H83A H 0.2702 0.4487 0.3277 0.094 Uiso 1 1 calc R . . H83B H 0.2470 0.5149 0.3777 0.094 Uiso 1 1 calc R . . H83C H 0.1571 0.4696 0.3448 0.094 Uiso 1 1 calc R . . H9 H 0.3484 0.1135 0.2496 0.054(10) Uiso 1 1 d . . . H10 H 0.2233 0.1847 0.1829 0.040(8) Uiso 1 1 d . . . H11 H 0.1604 0.2559 0.2731 0.034(8) Uiso 1 1 d . . . H12 H 0.2728 0.1820 0.3356 0.060(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0294(3) 0.0324(4) 0.0295(4) 0.0006(3) -0.0013(3) 0.0010(3) P2 0.0278(3) 0.0311(4) 0.0310(4) 0.0033(3) 0.0011(3) 0.0030(3) P3 0.0298(4) 0.0306(4) 0.0305(4) 0.0004(3) 0.0029(3) 0.0032(3) P4 0.0285(3) 0.0327(4) 0.0267(4) 0.0005(3) 0.0017(3) -0.0011(3) P5 0.0245(3) 0.0386(4) 0.0362(4) 0.0097(3) 0.0003(3) 0.0020(3) P6 0.0244(3) 0.0340(4) 0.0455(4) 0.0049(3) 0.0009(3) 0.0038(3) P7 0.0283(4) 0.0315(4) 0.0439(4) -0.0073(3) 0.0002(3) 0.0034(3) P8 0.0310(4) 0.0345(4) 0.0371(4) -0.0094(3) -0.0013(3) 0.0014(3) N1 0.0343(12) 0.0273(12) 0.0280(12) 0.0048(10) 0.0044(10) 0.0016(10) N2 0.0251(11) 0.0322(13) 0.0334(12) -0.0009(10) -0.0018(10) -0.0030(10) N3 0.0329(12) 0.0278(12) 0.0307(12) 0.0002(10) 0.0015(10) -0.0023(10) N4 0.0235(10) 0.0330(12) 0.0284(11) 0.0024(10) 0.0035(9) -0.0012(9) N5 0.0223(10) 0.0379(13) 0.0376(13) 0.0028(11) 0.0011(10) -0.0021(10) N6 0.0266(11) 0.0299(13) 0.0490(15) 0.0071(11) 0.0007(11) 0.0021(10) N7 0.0252(11) 0.0354(13) 0.0363(13) -0.0053(10) 0.0015(10) 0.0011(10) N8 0.0323(12) 0.0257(13) 0.0514(15) -0.0089(11) -0.0081(11) 0.0004(10) N9 0.0312(12) 0.0360(13) 0.0327(12) 0.0004(10) -0.0004(10) 0.0075(11) N10 0.0291(11) 0.0349(13) 0.0283(13) 0.0050(10) 0.0018(10) 0.0055(10) N11 0.0315(12) 0.0394(14) 0.0368(13) -0.0016(11) 0.0004(11) 0.0128(11) N12 0.0305(12) 0.0316(13) 0.0317(12) -0.0027(10) -0.0024(10) 0.0054(10) C1 0.0387(15) 0.0280(15) 0.0356(15) 0.0081(12) 0.0025(13) 0.0035(12) C2 0.0289(14) 0.0372(16) 0.0437(17) 0.0023(13) -0.0017(13) -0.0085(12) C3 0.0367(15) 0.0284(15) 0.0373(15) -0.0002(12) 0.0036(13) -0.0068(12) C4 0.0271(13) 0.0435(17) 0.0360(16) 0.0002(13) 0.0092(12) -0.0016(12) C5 0.0244(13) 0.0556(19) 0.0388(16) 0.0028(14) -0.0053(13) -0.0061(13) C6 0.0315(15) 0.0309(16) 0.067(2) 0.0165(15) 0.0007(15) -0.0028(12) C7 0.0310(14) 0.0423(17) 0.0400(16) -0.0041(14) 0.0064(13) -0.0077(13) C8 0.0446(17) 0.0349(17) 0.065(2) -0.0159(16) -0.0084(17) -0.0041(14) C11 0.0570(19) 0.0295(16) 0.0472(19) 0.0008(14) 0.0104(16) -0.0017(14) C12 0.0419(16) 0.0398(18) 0.0446(18) 0.0070(14) 0.0077(14) -0.0011(14) C13 0.0536(19) 0.0458(19) 0.0515(19) 0.0130(16) -0.0039(15) 0.0126(16) C21 0.0515(18) 0.055(2) 0.057(2) -0.0067(17) -0.0060(16) -0.0198(16) C22 0.0389(17) 0.061(2) 0.076(2) -0.0022(19) 0.0077(18) -0.0126(16) C23 0.0551(19) 0.0434(19) 0.060(2) 0.0128(16) -0.0020(16) -0.0093(16) C31 0.0530(19) 0.054(2) 0.053(2) -0.0006(16) -0.0057(17) -0.0217(16) C32 0.062(2) 0.0280(17) 0.070(2) -0.0008(16) 0.0047(18) -0.0066(15) C33 0.0498(18) 0.050(2) 0.0536(19) 0.0040(16) 0.0139(16) -0.0072(16) C41 0.0304(15) 0.073(2) 0.056(2) 0.0074(17) 0.0067(15) -0.0031(16) C42 0.0504(19) 0.055(2) 0.0460(19) -0.0054(16) 0.0200(16) 0.0065(16) C43 0.0432(17) 0.0440(18) 0.0451(17) 0.0046(15) 0.0134(14) -0.0075(15) C51 0.0355(16) 0.079(3) 0.052(2) 0.0109(18) -0.0110(15) 0.0108(16) C52 0.0390(17) 0.059(2) 0.075(2) -0.0066(19) -0.0071(17) -0.0103(16) C53 0.0297(16) 0.104(3) 0.051(2) 0.006(2) -0.0001(15) -0.0207(18) C61 0.052(2) 0.0301(19) 0.132(4) 0.013(2) 0.000(2) -0.0006(15) C62 0.0392(18) 0.072(3) 0.076(3) 0.039(2) -0.0003(18) -0.0106(17) C63 0.0328(15) 0.0436(19) 0.066(2) 0.0025(16) -0.0042(15) -0.0045(14) C71 0.0296(15) 0.062(2) 0.073(2) -0.0017(19) 0.0031(16) -0.0058(15) C72 0.0441(18) 0.052(2) 0.0519(19) 0.0030(16) 0.0131(16) 0.0004(15) C73 0.0483(18) 0.0402(18) 0.0551(19) -0.0120(15) 0.0063(16) -0.0143(15) C81 0.058(2) 0.049(2) 0.124(4) -0.026(2) -0.032(2) -0.0106(18) C82 0.085(3) 0.056(2) 0.075(3) -0.036(2) 0.006(2) -0.006(2) C83 0.070(2) 0.0298(18) 0.087(3) -0.0118(18) 0.000(2) -0.0069(16) _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 N12 1.704(2) . ? P1 N2 1.713(2) . ? P1 N1 1.740(2) . ? P1 P2 2.6143(10) . ? P2 N9 1.705(2) . ? P2 N2 1.710(2) . ? P2 N1 1.733(2) . ? P3 N9 1.701(2) . ? P3 N3 1.715(2) . ? P3 N4 1.739(2) . ? P3 P4 2.6127(10) . ? P4 N10 1.697(2) . ? P4 N3 1.712(2) . ? P4 N4 1.737(2) . ? P5 N10 1.705(2) . ? P5 N6 1.710(2) . ? P5 N5 1.736(2) . ? P5 P6 2.6132(11) . ? P6 N11 1.697(2) . ? P6 N6 1.716(2) . ? P6 N5 1.738(2) . ? P7 N11 1.703(2) . ? P7 N7 1.714(2) . ? P7 N8 1.737(2) . ? P7 P8 2.6156(10) . ? P8 N12 1.709(2) . ? P8 N7 1.712(2) . ? P8 N8 1.739(2) . ? N1 C1 1.491(3) . ? N2 C2 1.481(3) . ? N3 C3 1.483(3) . ? N4 C4 1.492(3) . ? N5 C5 1.497(3) . ? N6 C6 1.480(3) . ? N7 C7 1.474(3) . ? N8 C8 1.493(4) . ? N9 H9 0.848(2) . ? N10 H10 0.860(2) . ? N11 H11 0.885(2) . ? N12 H12 0.994(2) . ? C1 C12 1.524(4) . ? C1 C11 1.527(4) . ? C1 C13 1.532(4) . ? C2 C22 1.516(4) . ? C2 C21 1.517(4) . ? C2 C23 1.523(4) . ? C3 C32 1.509(4) . ? C3 C31 1.511(4) . ? C3 C33 1.527(4) . ? C4 C43 1.524(4) . ? C4 C41 1.530(4) . ? C4 C42 1.531(4) . ? C5 C52 1.515(4) . ? C5 C51 1.522(4) . ? C5 C53 1.528(4) . ? C6 C63 1.519(4) . ? C6 C61 1.526(5) . ? C6 C62 1.527(5) . ? C7 C72 1.519(4) . ? C7 C73 1.527(4) . ? C7 C71 1.532(4) . ? C8 C83 1.511(5) . ? C8 C82 1.527(5) . ? C8 C81 1.531(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? 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 N12 P1 N2 103.40(11) . . ? N12 P1 N1 103.80(11) . . ? N2 P1 N1 81.23(10) . . ? N12 P1 P2 109.19(8) . . ? N2 P1 P2 40.18(7) . . ? N1 P1 P2 41.08(7) . . ? N9 P2 N2 103.76(11) . . ? N9 P2 N1 102.69(11) . . ? N2 P2 N1 81.48(10) . . ? N9 P2 P1 108.73(8) . . ? N2 P2 P1 40.24(7) . . ? N1 P2 P1 41.27(7) . . ? N9 P3 N3 103.65(11) . . ? N9 P3 N4 102.52(11) . . ? N3 P3 N4 81.49(10) . . ? N9 P3 P4 108.69(8) . . ? N3 P3 P4 40.28(7) . . ? N4 P3 P4 41.24(7) . . ? N10 P4 N3 103.83(11) . . ? N10 P4 N4 103.46(10) . . ? N3 P4 N4 81.62(10) . . ? N10 P4 P3 109.46(8) . . ? N3 P4 P3 40.36(7) . . ? N4 P4 P3 41.30(7) . . ? N10 P5 N6 103.83(11) . . ? N10 P5 N5 103.37(11) . . ? N6 P5 N5 81.61(11) . . ? N10 P5 P6 108.40(8) . . ? N6 P5 P6 40.36(7) . . ? N5 P5 P6 41.25(8) . . ? N11 P6 N6 103.93(11) . . ? N11 P6 N5 103.72(11) . . ? N6 P6 N5 81.37(11) . . ? N11 P6 P5 108.67(8) . . ? N6 P6 P5 40.20(8) . . ? N5 P6 P5 41.17(7) . . ? N11 P7 N7 104.60(11) . . ? N11 P7 N8 103.25(11) . . ? N7 P7 N8 81.41(11) . . ? N11 P7 P8 109.00(8) . . ? N7 P7 P8 40.21(7) . . ? N8 P7 P8 41.21(8) . . ? N12 P8 N7 103.48(10) . . ? N12 P8 N8 103.27(11) . . ? N7 P8 N8 81.40(11) . . ? N12 P8 P7 108.26(8) . . ? N7 P8 P7 40.24(8) . . ? N8 P8 P7 41.16(7) . . ? C1 N1 P2 121.90(17) . . ? C1 N1 P1 121.72(16) . . ? P2 N1 P1 97.65(11) . . ? C2 N2 P2 130.55(18) . . ? C2 N2 P1 129.87(18) . . ? P2 N2 P1 99.58(11) . . ? C3 N3 P4 130.07(17) . . ? C3 N3 P3 130.57(18) . . ? P4 N3 P3 99.36(11) . . ? C4 N4 P4 121.45(16) . . ? C4 N4 P3 122.11(17) . . ? P4 N4 P3 97.46(11) . . ? C5 N5 P5 121.46(18) . . ? C5 N5 P6 121.62(18) . . ? P5 N5 P6 97.58(11) . . ? C6 N6 P5 130.3(2) . . ? C6 N6 P6 130.2(2) . . ? P5 N6 P6 99.43(11) . . ? C7 N7 P8 130.14(18) . . ? C7 N7 P7 130.14(18) . . ? P8 N7 P7 99.55(11) . . ? C8 N8 P7 121.08(18) . . ? C8 N8 P8 123.1(2) . . ? P7 N8 P8 97.63(11) . . ? P3 N9 P2 128.77(14) . . ? P3 N9 H9 111.72(19) . . ? P2 N9 H9 119.51(19) . . ? P4 N10 P5 127.42(13) . . ? P4 N10 H10 119.54(18) . . ? P5 N10 H10 112.56(18) . . ? P6 N11 P7 127.58(13) . . ? P6 N11 H11 118.88(19) . . ? P7 N11 H11 113.53(19) . . ? P1 N12 P8 127.30(13) . . ? P1 N12 H12 113.37(16) . . ? P8 N12 H12 119.33(16) . . ? N1 C1 C12 107.6(2) . . ? N1 C1 C11 108.5(2) . . ? C12 C1 C11 109.9(2) . . ? N1 C1 C13 110.8(2) . . ? C12 C1 C13 110.0(2) . . ? C11 C1 C13 109.9(2) . . ? N2 C2 C22 108.8(2) . . ? N2 C2 C21 107.6(2) . . ? C22 C2 C21 110.5(3) . . ? N2 C2 C23 109.4(2) . . ? C22 C2 C23 110.3(3) . . ? C21 C2 C23 110.3(3) . . ? N3 C3 C32 108.9(2) . . ? N3 C3 C31 108.5(2) . . ? C32 C3 C31 110.7(3) . . ? N3 C3 C33 108.8(2) . . ? C32 C3 C33 109.7(3) . . ? C31 C3 C33 110.2(2) . . ? N4 C4 C43 107.9(2) . . ? N4 C4 C41 108.1(2) . . ? C43 C4 C41 109.4(2) . . ? N4 C4 C42 110.9(2) . . ? C43 C4 C42 110.1(2) . . ? C41 C4 C42 110.3(2) . . ? N5 C5 C52 108.6(2) . . ? N5 C5 C51 110.6(2) . . ? C52 C5 C51 110.1(3) . . ? N5 C5 C53 107.8(2) . . ? C52 C5 C53 110.4(3) . . ? C51 C5 C53 109.4(3) . . ? N6 C6 C63 110.2(2) . . ? N6 C6 C61 108.3(2) . . ? C63 C6 C61 110.2(3) . . ? N6 C6 C62 107.8(3) . . ? C63 C6 C62 110.3(3) . . ? C61 C6 C62 110.0(3) . . ? N7 C7 C72 108.6(2) . . ? N7 C7 C73 109.5(2) . . ? C72 C7 C73 109.8(2) . . ? N7 C7 C71 108.4(2) . . ? C72 C7 C71 110.0(2) . . ? C73 C7 C71 110.6(3) . . ? N8 C8 C83 108.3(3) . . ? N8 C8 C82 111.6(3) . . ? C83 C8 C82 109.9(3) . . ? N8 C8 C81 107.0(2) . . ? C83 C8 C81 109.8(3) . . ? C82 C8 C81 110.3(3) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 H12A 109.5 . . ? C1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C2 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C2 C23 H23A 109.5 . . ? C2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C3 C31 H31A 109.5 . . ? C3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C3 C32 H32A 109.5 . . ? C3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C3 C33 H33A 109.5 . . ? C3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C42 H42A 109.5 . . ? C4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C4 C43 H43A 109.5 . . ? C4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C5 C52 H52A 109.5 . . ? C5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C5 C53 H53A 109.5 . . ? C5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C6 C61 H61A 109.5 . . ? C6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C6 C62 H62A 109.5 . . ? C6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C6 C63 H63A 109.5 . . ? C6 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C6 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C7 C71 H71A 109.5 . . ? C7 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C7 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C7 C72 H72A 109.5 . . ? C7 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C7 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C7 C73 H73A 109.5 . . ? C7 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C7 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C8 C81 H81A 109.5 . . ? C8 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C8 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C8 C82 H82A 109.5 . . ? C8 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C8 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C8 C83 H83A 109.5 . . ? C8 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C8 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.277 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.040