# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Scott Browning' _publ_contact_author_address ; Department of Chemistry University of Toronto 80 St. George Street Toronto, Ontario M5S 3H6 CANADA ; _publ_contact_author_email sbrownin@chem.utoronto.ca _publ_section_title ; Tris(3-methylindolyl)phosphine as an anion receptor ; loop_ _publ_author_name 'Joanne O Yu' 'C Scott Browning' 'David H Farrar' data_k06149_(Complex_2) _database_code_depnum_ccdc_archive 'CCDC 662466' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C27 H24 N3 P),2(C8 H20 N),3(C H4 O),2(F)' _chemical_formula_sum 'C73 H100 F2 N8 O3 P2' _chemical_formula_weight 1237.55 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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 2(1) 2(1) 2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.3758(1) _cell_length_b 24.2008(2) _cell_length_c 24.9237(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6861.58(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 153384 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 0.121 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.591 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 46395 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.55 _reflns_number_total 15463 _reflns_number_gt 12728 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXTL V6.12 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL V6.12' _computing_molecular_graphics 'SHELXTL V6.12' _computing_publication_material 'SHELXTL V6.12' _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^)+(0.0719P)^2^+1.2805P] 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 SHELXL _refine_ls_extinction_coef 0.0014(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(7) _refine_ls_number_reflns 15463 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1389 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 P1A P 0.61771(6) 0.89858(3) 0.10102(3) 0.03109(14) Uani 1 1 d . . . N1A N 0.57465(19) 0.94414(8) -0.00347(8) 0.0333(4) Uani 1 1 d . . . H1A H 0.5024 0.9314 -0.0057 0.040 Uiso 1 1 calc R . . N11A N 0.38190(18) 0.94169(8) 0.10158(9) 0.0347(5) Uani 1 1 d . . . H11A H 0.3593 0.9244 0.0723 0.042 Uiso 1 1 calc R . . N21A N 0.47183(17) 0.82445(8) 0.04017(8) 0.0309(4) Uani 1 1 d . . . H21A H 0.4275 0.8505 0.0261 0.037 Uiso 1 1 calc R . . N31A N 0.46319(16) 1.11696(8) 0.03506(8) 0.0283(4) Uani 1 1 d . . . F1A F 0.34888(13) 0.90639(6) -0.00076(7) 0.0435(4) Uani 1 1 d . . . C2A C 0.6505(2) 0.93566(9) 0.03954(10) 0.0305(5) Uani 1 1 d . . . C3A C 0.7562(2) 0.96197(10) 0.02852(11) 0.0346(6) Uani 1 1 d . . . C3S C 0.2855(5) 0.9304(2) -0.1289(2) 0.0982(16) Uani 1 1 d . . . H3S1 H 0.2290 0.9525 -0.1084 0.147 Uiso 1 1 calc R . . H3S2 H 0.2515 0.9207 -0.1637 0.147 Uiso 1 1 calc R . . H3S3 H 0.3577 0.9517 -0.1343 0.147 Uiso 1 1 calc R . . C4A C 0.7438(2) 0.98777(11) -0.02285(11) 0.0376(6) Uani 1 1 d . . . C5A C 0.8170(3) 1.02107(12) -0.05456(13) 0.0510(8) Uani 1 1 d . . . H5AA H 0.8937 1.0305 -0.0426 0.061 Uiso 1 1 calc R . . C6A C 0.7763(3) 1.03987(13) -0.10332(14) 0.0577(9) Uani 1 1 d . . . H6AA H 0.8258 1.0623 -0.1250 0.069 Uiso 1 1 calc R . . C7A C 0.6634(3) 1.02653(13) -0.12159(12) 0.0540(8) Uani 1 1 d . . . H7AA H 0.6374 1.0403 -0.1552 0.065 Uiso 1 1 calc R . . C8A C 0.5895(3) 0.99385(11) -0.09165(11) 0.0465(7) Uani 1 1 d . . . H8AA H 0.5136 0.9842 -0.1045 0.056 Uiso 1 1 calc R . . C9A C 0.6296(2) 0.97528(10) -0.04175(11) 0.0363(6) Uani 1 1 d . . . C10A C 0.8624(2) 0.96521(12) 0.06436(12) 0.0422(6) Uani 1 1 d . . . H10A H 0.8559 0.9375 0.0928 0.063 Uiso 1 1 calc R . . H10B H 0.8671 1.0021 0.0804 0.063 Uiso 1 1 calc R . . H10C H 0.9334 0.9582 0.0432 0.063 Uiso 1 1 calc R . . C12A C 0.4913(2) 0.93616(10) 0.12606(11) 0.0331(5) Uani 1 1 d . . . C13A C 0.4943(2) 0.96908(10) 0.17125(11) 0.0346(5) Uani 1 1 d . . . C14A C 0.3825(2) 0.99650(10) 0.17490(11) 0.0358(5) Uani 1 1 d . . . C15A C 0.3363(3) 1.03660(12) 0.20952(12) 0.0454(7) Uani 1 1 d . . . H15A H 0.3805 1.0496 0.2393 0.054 Uiso 1 1 calc R . . C16A C 0.2245(3) 1.05684(12) 0.19931(13) 0.0496(8) Uani 1 1 d . . . H16A H 0.1916 1.0838 0.2226 0.059 Uiso 1 1 calc R . . C17A C 0.1591(3) 1.03817(12) 0.15521(13) 0.0470(7) Uani 1 1 d . . . H17A H 0.0831 1.0532 0.1490 0.056 Uiso 1 1 calc R . . C18A C 0.2019(3) 0.99876(11) 0.12068(12) 0.0417(6) Uani 1 1 d . . . H18A H 0.1563 0.9858 0.0913 0.050 Uiso 1 1 calc R . . C19A C 0.3150(2) 0.97837(10) 0.13035(11) 0.0337(5) Uani 1 1 d . . . C20A C 0.5948(3) 0.97835(13) 0.20909(13) 0.0492(7) Uani 1 1 d . . . H20A H 0.6592 0.9531 0.2001 0.074 Uiso 1 1 calc R . . H20B H 0.5687 0.9714 0.2460 0.074 Uiso 1 1 calc R . . H20C H 0.6222 1.0166 0.2059 0.074 Uiso 1 1 calc R . . C22A C 0.5627(2) 0.83258(10) 0.07752(10) 0.0291(5) Uani 1 1 d . . . C23A C 0.6097(2) 0.78228(9) 0.09119(9) 0.0289(5) Uani 1 1 d . . . C24A C 0.5482(2) 0.74097(10) 0.06034(9) 0.0297(5) Uani 1 1 d . . . C25A C 0.5571(2) 0.68358(10) 0.05603(10) 0.0361(6) Uani 1 1 d . . . H25A H 0.6136 0.6638 0.0765 0.043 Uiso 1 1 calc R . . C26A C 0.4819(3) 0.65613(11) 0.02135(11) 0.0400(6) Uani 1 1 d . . . H26A H 0.4863 0.6170 0.0184 0.048 Uiso 1 1 calc R . . C27A C 0.3995(2) 0.68515(11) -0.00934(10) 0.0376(6) Uani 1 1 d . . . H27A H 0.3498 0.6652 -0.0331 0.045 Uiso 1 1 calc R . . C28A C 0.3881(2) 0.74138(11) -0.00632(10) 0.0342(5) Uani 1 1 d . . . H28A H 0.3319 0.7607 -0.0273 0.041 Uiso 1 1 calc R . . C29A C 0.4640(2) 0.76937(10) 0.02951(10) 0.0295(5) Uani 1 1 d . . . C30A C 0.7044(2) 0.77065(11) 0.13133(11) 0.0365(6) Uani 1 1 d . . . H30A H 0.7541 0.8035 0.1355 0.055 Uiso 1 1 calc R . . H30B H 0.7525 0.7396 0.1188 0.055 Uiso 1 1 calc R . . H30C H 0.6687 0.7613 0.1659 0.055 Uiso 1 1 calc R . . C32A C 0.5268(2) 1.07260(10) 0.06749(11) 0.0317(5) Uani 1 1 d . . . H32A H 0.4798 1.0644 0.1000 0.038 Uiso 1 1 calc R . . H32B H 0.5302 1.0384 0.0458 0.038 Uiso 1 1 calc R . . C33A C 0.6511(2) 1.08754(11) 0.08479(12) 0.0390(6) Uani 1 1 d . . . H33A H 0.6865 1.0562 0.1037 0.059 Uiso 1 1 calc R . . H33B H 0.6486 1.1196 0.1087 0.059 Uiso 1 1 calc R . . H33C H 0.6984 1.0964 0.0531 0.059 Uiso 1 1 calc R . . C34A C 0.5253(2) 1.12341(10) -0.01881(10) 0.0328(5) Uani 1 1 d . . . H34A H 0.6034 1.1402 -0.0125 0.039 Uiso 1 1 calc R . . H34B H 0.5385 1.0862 -0.0342 0.039 Uiso 1 1 calc R . . C35A C 0.4606(2) 1.15800(12) -0.05975(11) 0.0397(6) Uani 1 1 d . . . H35A H 0.5048 1.1582 -0.0935 0.060 Uiso 1 1 calc R . . H35B H 0.4528 1.1959 -0.0464 0.060 Uiso 1 1 calc R . . H35C H 0.3824 1.1423 -0.0659 0.060 Uiso 1 1 calc R . . C36A C 0.3362(2) 1.09882(11) 0.02753(12) 0.0366(6) Uani 1 1 d . . . H36A H 0.3011 1.0925 0.0634 0.044 Uiso 1 1 calc R . . H36B H 0.2922 1.1294 0.0105 0.044 Uiso 1 1 calc R . . C37A C 0.3190(3) 1.04743(11) -0.00571(12) 0.0433(7) Uani 1 1 d . . . H37A H 0.2349 1.0392 -0.0085 0.065 Uiso 1 1 calc R . . H37B H 0.3595 1.0163 0.0114 0.065 Uiso 1 1 calc R . . H37C H 0.3516 1.0533 -0.0417 0.065 Uiso 1 1 calc R . . C38A C 0.4651(2) 1.17175(10) 0.06453(10) 0.0334(5) Uani 1 1 d . . . H38A H 0.4185 1.1988 0.0437 0.040 Uiso 1 1 calc R . . H38B H 0.5472 1.1853 0.0656 0.040 Uiso 1 1 calc R . . C39A C 0.4178(3) 1.17034(12) 0.12146(11) 0.0415(6) Uani 1 1 d . . . H39A H 0.4274 1.2068 0.1380 0.062 Uiso 1 1 calc R . . H39B H 0.4613 1.1428 0.1424 0.062 Uiso 1 1 calc R . . H39C H 0.3343 1.1605 0.1208 0.062 Uiso 1 1 calc R . . O3S O 0.3112(3) 0.88289(14) -0.10097(12) 0.0975(10) Uani 1 1 d . . . H3S H 0.3306 0.8910 -0.0694 0.146 Uiso 1 1 calc R . . P1B P 0.92626(5) 1.18119(3) 0.16103(2) 0.02782(14) Uani 1 1 d . . . N1B N 0.87848(19) 1.29435(8) 0.18776(8) 0.0320(4) Uani 1 1 d . . . H1B H 0.8063 1.2940 0.1751 0.038 Uiso 1 1 calc R . . N11B N 0.69178(17) 1.18866(8) 0.20495(8) 0.0294(4) Uani 1 1 d . . . H11B H 0.6709 1.2178 0.1861 0.035 Uiso 1 1 calc R . . N21B N 0.77846(17) 1.22719(8) 0.07906(8) 0.0275(4) Uani 1 1 d . . . H21B H 0.7353 1.2469 0.1012 0.033 Uiso 1 1 calc R . . N31B N 0.15743(18) 0.74941(9) 0.13158(8) 0.0310(4) Uani 1 1 d . . . F1B F 0.65351(13) 1.28784(6) 0.15058(6) 0.0378(3) Uani 1 1 d . . . C2B C 0.9569(2) 1.25041(10) 0.18559(10) 0.0292(5) Uani 1 1 d . . . C3B C 1.0615(2) 1.26625(10) 0.20929(10) 0.0323(5) Uani 1 1 d . . . C4B C 1.0462(2) 1.32230(11) 0.22701(10) 0.0341(5) Uani 1 1 d . . . C5B C 1.1169(3) 1.36000(12) 0.25589(11) 0.0437(6) Uani 1 1 d . . . H5BA H 1.1946 1.3502 0.2662 0.052 Uiso 1 1 calc R . . C6B C 1.0720(3) 1.41100(13) 0.26889(13) 0.0526(8) Uani 1 1 d . . . H6BA H 1.1193 1.4366 0.2881 0.063 Uiso 1 1 calc R . . C7B C 0.9565(3) 1.42587(12) 0.25400(13) 0.0527(8) Uani 1 1 d . . . H7BA H 0.9272 1.4612 0.2638 0.063 Uiso 1 1 calc R . . C8B C 0.8858(3) 1.39033(11) 0.22572(11) 0.0423(6) Uani 1 1 d . . . H8BA H 0.8086 1.4008 0.2154 0.051 Uiso 1 1 calc R . . C9B C 0.9307(2) 1.33834(10) 0.21264(10) 0.0337(5) Uani 1 1 d . . . C10B C 1.1720(2) 1.23289(12) 0.21651(11) 0.0387(6) Uani 1 1 d . . . H10D H 1.1631 1.1971 0.1986 0.058 Uiso 1 1 calc R . . H10E H 1.1864 1.2270 0.2549 0.058 Uiso 1 1 calc R . . H10F H 1.2386 1.2528 0.2007 0.058 Uiso 1 1 calc R . . C12B C 0.7992(2) 1.16081(10) 0.20067(9) 0.0291(5) Uani 1 1 d . . . C13B C 0.7984(2) 1.11668(10) 0.23551(10) 0.0309(5) Uani 1 1 d . . . C14B C 0.6886(2) 1.11814(10) 0.26349(10) 0.0325(5) Uani 1 1 d . . . C15B C 0.6406(2) 1.08603(11) 0.30573(10) 0.0377(6) Uani 1 1 d . . . H15B H 0.6824 1.0555 0.3202 0.045 Uiso 1 1 calc R . . C16B C 0.5310(3) 1.10046(12) 0.32516(11) 0.0442(7) Uani 1 1 d . . . H16B H 0.4976 1.0796 0.3536 0.053 Uiso 1 1 calc R . . C17B C 0.4681(3) 1.14497(12) 0.30394(11) 0.0425(6) Uani 1 1 d . . . H17B H 0.3930 1.1535 0.3184 0.051 Uiso 1 1 calc R . . C18B C 0.5117(2) 1.17710(11) 0.26246(10) 0.0363(6) Uani 1 1 d . . . H18B H 0.4679 1.2069 0.2478 0.044 Uiso 1 1 calc R . . C19B C 0.6245(2) 1.16324(10) 0.24310(9) 0.0309(5) Uani 1 1 d . . . C20B C 0.8925(3) 1.07398(11) 0.24413(12) 0.0422(6) Uani 1 1 d . . . H20D H 0.9684 1.0887 0.2323 0.063 Uiso 1 1 calc R . . H20E H 0.8737 1.0407 0.2234 0.063 Uiso 1 1 calc R . . H20F H 0.8969 1.0646 0.2823 0.063 Uiso 1 1 calc R . . C22B C 0.8711(2) 1.19224(9) 0.09385(9) 0.0260(5) Uani 1 1 d . . . C23B C 0.9154(2) 1.16741(9) 0.04860(9) 0.0265(5) Uani 1 1 d . . . C24B C 0.8503(2) 1.18819(9) 0.00377(9) 0.0271(5) Uani 1 1 d . . . C25B C 0.8536(2) 1.17853(10) -0.05182(10) 0.0321(5) Uani 1 1 d . . . H25B H 0.9089 1.1534 -0.0667 0.039 Uiso 1 1 calc R . . C26B C 0.7752(2) 1.20610(11) -0.08442(10) 0.0367(6) Uani 1 1 d . . . H26B H 0.7767 1.1997 -0.1220 0.044 Uiso 1 1 calc R . . C27B C 0.6932(2) 1.24356(11) -0.06298(11) 0.0359(6) Uani 1 1 d . . . H27B H 0.6404 1.2620 -0.0865 0.043 Uiso 1 1 calc R . . C28B C 0.6875(2) 1.25427(10) -0.00877(10) 0.0316(5) Uani 1 1 d . . . H28B H 0.6326 1.2800 0.0055 0.038 Uiso 1 1 calc R . . C29B C 0.7661(2) 1.22556(9) 0.02445(9) 0.0275(5) Uani 1 1 d . . . C30B C 1.0110(2) 1.12474(10) 0.04525(10) 0.0319(5) Uani 1 1 d . . . H30D H 1.0659 1.1298 0.0751 0.048 Uiso 1 1 calc R . . H30E H 1.0532 1.1288 0.0112 0.048 Uiso 1 1 calc R . . H30F H 0.9762 1.0877 0.0472 0.048 Uiso 1 1 calc R . . C32B C 0.0282(2) 0.73563(12) 0.14079(11) 0.0401(6) Uani 1 1 d . . . H32C H -0.0102 0.7680 0.1576 0.048 Uiso 1 1 calc R . . H32D H -0.0095 0.7297 0.1055 0.048 Uiso 1 1 calc R . . C33B C 0.0050(2) 0.68610(14) 0.17512(11) 0.0464(7) Uani 1 1 d . . . H33D H -0.0799 0.6796 0.1773 0.070 Uiso 1 1 calc R . . H33E H 0.0363 0.6926 0.2112 0.070 Uiso 1 1 calc R . . H33F H 0.0435 0.6537 0.1594 0.070 Uiso 1 1 calc R . . C34B C 0.2229(2) 0.69875(11) 0.11099(10) 0.0348(6) Uani 1 1 d . . . H34C H 0.3025 0.7103 0.0997 0.042 Uiso 1 1 calc R . . H34D H 0.2322 0.6724 0.1411 0.042 Uiso 1 1 calc R . . C35B C 0.1654(2) 0.66892(12) 0.06491(11) 0.0412(6) Uani 1 1 d . . . H35D H 0.2125 0.6365 0.0553 0.062 Uiso 1 1 calc R . . H35E H 0.1600 0.6938 0.0340 0.062 Uiso 1 1 calc R . . H35F H 0.0864 0.6571 0.0755 0.062 Uiso 1 1 calc R . . C36B C 0.2106(2) 0.76723(12) 0.18479(10) 0.0400(6) Uani 1 1 d . . . H36C H 0.1594 0.7958 0.2010 0.048 Uiso 1 1 calc R . . H36D H 0.2114 0.7351 0.2093 0.048 Uiso 1 1 calc R . . C37B C 0.3344(3) 0.79006(14) 0.18078(12) 0.0483(7) Uani 1 1 d . . . H37D H 0.3653 0.7968 0.2169 0.072 Uiso 1 1 calc R . . H37E H 0.3331 0.8248 0.1606 0.072 Uiso 1 1 calc R . . H37F H 0.3847 0.7633 0.1622 0.072 Uiso 1 1 calc R . . C38B C 0.1652(2) 0.79503(11) 0.09014(11) 0.0379(6) Uani 1 1 d . . . H38C H 0.2489 0.8005 0.0808 0.045 Uiso 1 1 calc R . . H38D H 0.1242 0.7825 0.0573 0.045 Uiso 1 1 calc R . . C39B C 0.1141(3) 0.85021(12) 0.10667(14) 0.0513(7) Uani 1 1 d . . . H39D H 0.1235 0.8767 0.0773 0.077 Uiso 1 1 calc R . . H39E H 0.1555 0.8638 0.1385 0.077 Uiso 1 1 calc R . . H39F H 0.0304 0.8458 0.1149 0.077 Uiso 1 1 calc R . . C2S C 0.6222(4) 1.42437(18) 0.11753(19) 0.0846(13) Uani 1 1 d . . . H2S1 H 0.6917 1.4322 0.1395 0.127 Uiso 1 1 calc R . . H2S2 H 0.5542 1.4183 0.1410 0.127 Uiso 1 1 calc R . . H2S3 H 0.6066 1.4558 0.0937 0.127 Uiso 1 1 calc R . . C1S C 0.4471(3) 1.35177(16) 0.22746(17) 0.0696(10) Uani 1 1 d . . . H1S1 H 0.4240 1.3475 0.2651 0.104 Uiso 1 1 calc R . . H1S2 H 0.3889 1.3746 0.2088 0.104 Uiso 1 1 calc R . . H1S3 H 0.5243 1.3696 0.2256 0.104 Uiso 1 1 calc R . . O2S O 0.6420(3) 1.37737(11) 0.08701(11) 0.0782(8) Uani 1 1 d . . . H2S H 0.6449 1.3496 0.1072 0.117 Uiso 1 1 calc R . . O1S O 0.4528(2) 1.30015(11) 0.20324(11) 0.0707(7) Uani 1 1 d . . . H1S H 0.5169 1.2971 0.1867 0.106 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 P1A 0.0282(3) 0.0289(3) 0.0361(3) -0.0040(3) -0.0028(3) 0.0000(2) N1A 0.0298(10) 0.0337(11) 0.0363(11) -0.0022(9) -0.0018(9) 0.0014(8) N11A 0.0305(11) 0.0353(11) 0.0382(11) -0.0051(9) -0.0007(9) 0.0018(8) N21A 0.0268(10) 0.0309(10) 0.0350(11) -0.0002(9) -0.0042(8) 0.0009(8) N31A 0.0226(9) 0.0267(10) 0.0357(11) 0.0017(8) 0.0002(8) 0.0004(7) F1A 0.0357(8) 0.0437(8) 0.0511(9) -0.0056(7) -0.0145(7) 0.0054(6) C2A 0.0341(13) 0.0233(11) 0.0339(12) -0.0053(10) -0.0005(10) 0.0022(9) C3A 0.0299(13) 0.0294(12) 0.0444(15) -0.0062(11) 0.0014(11) -0.0028(9) C3S 0.091(3) 0.101(3) 0.102(4) 0.011(3) -0.051(3) -0.023(3) C4A 0.0423(15) 0.0301(13) 0.0404(14) -0.0065(11) 0.0036(11) -0.0035(10) C5A 0.0549(19) 0.0471(17) 0.0508(18) -0.0063(14) 0.0115(14) -0.0140(14) C6A 0.083(2) 0.0469(17) 0.0437(17) -0.0005(15) 0.0152(17) -0.0134(16) C7A 0.081(2) 0.0448(17) 0.0365(15) -0.0038(13) 0.0016(15) 0.0007(15) C8A 0.0629(19) 0.0383(14) 0.0383(15) -0.0061(12) -0.0025(13) 0.0046(13) C9A 0.0433(15) 0.0288(12) 0.0370(13) -0.0071(11) 0.0022(11) -0.0001(10) C10A 0.0324(14) 0.0428(15) 0.0516(16) -0.0071(13) -0.0002(12) -0.0041(11) C12A 0.0297(13) 0.0304(12) 0.0392(14) -0.0011(11) 0.0009(10) -0.0003(9) C13A 0.0350(13) 0.0329(13) 0.0361(13) -0.0043(11) 0.0009(10) -0.0016(10) C14A 0.0393(14) 0.0307(12) 0.0373(14) -0.0010(11) 0.0060(11) 0.0005(11) C15A 0.0493(17) 0.0428(15) 0.0440(16) -0.0097(13) 0.0078(13) 0.0010(12) C16A 0.0545(19) 0.0404(15) 0.0539(18) -0.0027(14) 0.0184(15) 0.0113(13) C17A 0.0419(16) 0.0442(16) 0.0549(18) 0.0108(14) 0.0140(13) 0.0118(12) C18A 0.0388(15) 0.0403(15) 0.0459(16) 0.0080(12) 0.0030(12) 0.0031(12) C19A 0.0337(13) 0.0303(12) 0.0372(13) 0.0028(11) 0.0043(10) 0.0004(10) C20A 0.0433(17) 0.0539(17) 0.0505(17) -0.0159(15) -0.0070(13) 0.0004(13) C22A 0.0241(11) 0.0321(12) 0.0312(12) -0.0016(10) 0.0006(9) -0.0011(9) C23A 0.0289(12) 0.0296(12) 0.0283(12) 0.0005(10) 0.0031(9) -0.0004(9) C24A 0.0296(12) 0.0338(12) 0.0257(11) 0.0003(10) 0.0055(9) -0.0018(9) C25A 0.0459(15) 0.0305(12) 0.0318(13) 0.0031(11) 0.0045(11) -0.0016(11) C26A 0.0540(17) 0.0309(13) 0.0350(14) -0.0047(11) 0.0104(12) -0.0065(11) C27A 0.0394(14) 0.0436(15) 0.0299(12) -0.0086(11) 0.0060(10) -0.0106(11) C28A 0.0298(12) 0.0418(14) 0.0311(13) -0.0053(11) 0.0022(10) -0.0056(10) C29A 0.0246(11) 0.0349(12) 0.0290(12) -0.0017(10) 0.0056(9) -0.0036(9) C30A 0.0310(13) 0.0415(14) 0.0370(14) 0.0022(12) -0.0038(11) 0.0031(10) C32A 0.0307(13) 0.0260(11) 0.0385(14) 0.0038(10) -0.0029(10) 0.0024(9) C33A 0.0317(13) 0.0362(14) 0.0491(16) 0.0000(12) -0.0098(11) 0.0023(10) C34A 0.0296(12) 0.0348(13) 0.0339(13) -0.0016(11) 0.0026(10) -0.0006(10) C35A 0.0360(14) 0.0440(15) 0.0390(14) 0.0072(12) -0.0042(11) -0.0024(11) C36A 0.0236(12) 0.0366(13) 0.0496(15) 0.0059(12) -0.0035(10) -0.0011(10) C37A 0.0378(15) 0.0403(15) 0.0519(17) 0.0035(13) -0.0094(12) -0.0057(11) C38A 0.0306(13) 0.0299(12) 0.0396(14) -0.0009(11) -0.0002(10) 0.0025(9) C39A 0.0475(16) 0.0398(15) 0.0371(14) -0.0020(12) 0.0021(11) 0.0056(12) O3S 0.141(3) 0.095(2) 0.0566(16) -0.0162(17) 0.0195(18) -0.015(2) P1B 0.0258(3) 0.0322(3) 0.0255(3) 0.0004(3) -0.0002(2) -0.0002(2) N1B 0.0304(11) 0.0346(11) 0.0309(11) -0.0014(9) -0.0028(8) -0.0003(9) N11B 0.0288(10) 0.0335(11) 0.0258(10) 0.0030(8) 0.0009(8) 0.0019(8) N21B 0.0249(10) 0.0306(10) 0.0270(10) -0.0006(8) 0.0013(7) 0.0025(8) N31B 0.0283(10) 0.0416(12) 0.0230(10) -0.0027(9) -0.0029(8) 0.0045(8) F1B 0.0316(7) 0.0432(8) 0.0386(8) -0.0005(7) 0.0019(6) 0.0077(6) C2B 0.0301(12) 0.0311(12) 0.0265(12) 0.0028(10) -0.0008(9) -0.0008(9) C3B 0.0308(13) 0.0377(13) 0.0283(12) 0.0038(10) -0.0007(10) -0.0058(10) C4B 0.0347(13) 0.0405(14) 0.0273(12) 0.0059(11) -0.0008(9) -0.0080(11) C5B 0.0448(16) 0.0457(15) 0.0406(15) 0.0029(13) -0.0074(12) -0.0137(13) C6B 0.063(2) 0.0448(17) 0.0501(17) -0.0078(14) -0.0058(15) -0.0182(15) C7B 0.072(2) 0.0368(15) 0.0499(18) -0.0074(14) 0.0046(16) -0.0071(14) C8B 0.0483(16) 0.0379(14) 0.0407(14) -0.0019(12) -0.0004(12) 0.0011(12) C9B 0.0366(13) 0.0368(13) 0.0278(12) 0.0017(11) 0.0022(10) -0.0066(11) C10B 0.0312(13) 0.0496(16) 0.0353(14) 0.0045(12) -0.0036(10) -0.0032(11) C12B 0.0290(12) 0.0317(12) 0.0267(11) -0.0027(10) 0.0003(9) -0.0022(9) C13B 0.0338(13) 0.0296(12) 0.0293(12) -0.0031(10) -0.0009(10) -0.0015(10) C14B 0.0353(13) 0.0312(12) 0.0312(12) -0.0018(10) 0.0012(10) -0.0033(10) C15B 0.0462(16) 0.0362(14) 0.0306(13) 0.0023(11) 0.0030(11) -0.0065(11) C16B 0.0534(17) 0.0452(15) 0.0340(14) 0.0005(12) 0.0109(12) -0.0115(13) C17B 0.0394(15) 0.0498(16) 0.0383(15) -0.0062(13) 0.0121(12) -0.0046(12) C18B 0.0359(14) 0.0395(14) 0.0336(13) -0.0048(11) 0.0040(10) -0.0007(11) C19B 0.0337(13) 0.0337(12) 0.0253(11) -0.0020(10) 0.0006(9) -0.0040(10) C20B 0.0435(16) 0.0392(14) 0.0440(15) 0.0067(12) 0.0019(12) 0.0075(12) C22B 0.0246(11) 0.0272(11) 0.0263(11) 0.0010(9) -0.0027(9) -0.0009(8) C23B 0.0243(11) 0.0277(11) 0.0275(11) -0.0001(9) 0.0005(9) -0.0023(9) C24B 0.0250(11) 0.0259(11) 0.0305(12) 0.0016(10) 0.0016(9) -0.0046(8) C25B 0.0347(13) 0.0327(12) 0.0289(12) -0.0014(10) 0.0022(9) -0.0024(10) C26B 0.0457(15) 0.0381(14) 0.0263(12) 0.0018(11) -0.0038(10) -0.0052(11) C27B 0.0341(14) 0.0378(13) 0.0357(14) 0.0080(11) -0.0075(10) -0.0037(11) C28B 0.0258(12) 0.0302(12) 0.0388(14) 0.0031(11) -0.0017(10) -0.0001(9) C29B 0.0278(12) 0.0270(12) 0.0277(12) 0.0012(9) 0.0010(9) -0.0041(9) C30B 0.0304(12) 0.0309(12) 0.0345(13) -0.0001(10) 0.0015(10) 0.0038(9) C32B 0.0256(13) 0.0587(17) 0.0361(14) -0.0053(13) -0.0007(10) 0.0033(11) C33B 0.0330(14) 0.072(2) 0.0345(14) -0.0017(14) 0.0039(11) -0.0033(13) C34B 0.0334(13) 0.0400(14) 0.0310(13) 0.0035(11) 0.0022(10) 0.0057(10) C35B 0.0423(15) 0.0415(15) 0.0397(14) -0.0107(12) 0.0071(11) -0.0030(11) C36B 0.0402(15) 0.0531(16) 0.0268(13) -0.0028(12) -0.0052(11) 0.0022(12) C37B 0.0437(16) 0.0592(18) 0.0419(16) 0.0022(14) -0.0122(12) -0.0087(14) C38B 0.0388(14) 0.0422(14) 0.0327(13) 0.0008(11) -0.0048(11) 0.0030(11) C39B 0.0580(19) 0.0410(15) 0.0550(18) -0.0048(14) -0.0193(15) 0.0059(13) C2S 0.084(3) 0.072(3) 0.099(3) 0.023(2) 0.013(3) 0.010(2) C1S 0.053(2) 0.074(2) 0.082(3) -0.001(2) 0.0102(19) 0.0153(18) O2S 0.104(2) 0.0668(16) 0.0642(16) 0.0166(14) -0.0095(15) -0.0106(15) O1S 0.0455(14) 0.0775(17) 0.0891(19) -0.0084(15) 0.0132(13) -0.0042(12) _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 P1A C12A 1.812(3) . ? P1A C22A 1.813(2) . ? P1A C2A 1.814(3) . ? N1A C9A 1.367(3) . ? N1A C2A 1.391(3) . ? N11A C19A 1.371(3) . ? N11A C12A 1.392(3) . ? N21A C29A 1.362(3) . ? N21A C22A 1.404(3) . ? N31A C38A 1.516(3) . ? N31A C36A 1.522(3) . ? N31A C34A 1.525(3) . ? N31A C32A 1.526(3) . ? C2A C3A 1.388(4) . ? C3A C4A 1.431(4) . ? C3A C10A 1.505(4) . ? C3S O3S 1.374(6) . ? C4A C5A 1.403(4) . ? C4A C9A 1.415(4) . ? C5A C6A 1.378(5) . ? C6A C7A 1.401(5) . ? C7A C8A 1.374(5) . ? C8A C9A 1.399(4) . ? C12A C13A 1.380(4) . ? C13A C14A 1.438(4) . ? C13A C20A 1.499(4) . ? C14A C15A 1.401(4) . ? C14A C19A 1.419(4) . ? C15A C16A 1.387(4) . ? C16A C17A 1.402(5) . ? C17A C18A 1.374(4) . ? C18A C19A 1.400(4) . ? C22A C23A 1.373(3) . ? C23A C24A 1.442(3) . ? C23A C30A 1.497(3) . ? C24A C25A 1.397(4) . ? C24A C29A 1.407(3) . ? C25A C26A 1.386(4) . ? C26A C27A 1.399(4) . ? C27A C28A 1.369(4) . ? C28A C29A 1.415(3) . ? C32A C33A 1.522(3) . ? C34A C35A 1.511(4) . ? C36A C37A 1.507(4) . ? C38A C39A 1.518(4) . ? P1B C22B 1.808(2) . ? P1B C2B 1.817(2) . ? P1B C12B 1.819(2) . ? N1B C9B 1.368(3) . ? N1B C2B 1.389(3) . ? N11B C19B 1.367(3) . ? N11B C12B 1.400(3) . ? N21B C29B 1.369(3) . ? N21B C22B 1.401(3) . ? N31B C38B 1.514(3) . ? N31B C36B 1.520(3) . ? N31B C34B 1.523(3) . ? N31B C32B 1.525(3) . ? C2B C3B 1.382(3) . ? C3B C4B 1.437(4) . ? C3B C10B 1.505(4) . ? C4B C5B 1.414(4) . ? C4B C9B 1.416(4) . ? C5B C6B 1.375(4) . ? C6B C7B 1.412(5) . ? C7B C8B 1.373(4) . ? C8B C9B 1.396(4) . ? C12B C13B 1.376(4) . ? C13B C14B 1.431(4) . ? C13B C20B 1.503(4) . ? C14B C19B 1.407(4) . ? C14B C15B 1.418(4) . ? C15B C16B 1.382(4) . ? C16B C17B 1.397(4) . ? C17B C18B 1.385(4) . ? C18B C19B 1.412(4) . ? C22B C23B 1.374(3) . ? C23B C24B 1.432(3) . ? C23B C30B 1.502(3) . ? C24B C25B 1.406(3) . ? C24B C29B 1.414(3) . ? C25B C26B 1.378(4) . ? C26B C27B 1.407(4) . ? C27B C28B 1.377(4) . ? C28B C29B 1.403(3) . ? C32B C33B 1.496(4) . ? C34B C35B 1.506(4) . ? C36B C37B 1.515(4) . ? C38B C39B 1.513(4) . ? C2S O2S 1.387(5) . ? C1S O1S 1.389(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 C12A P1A C22A 106.22(11) . . ? C12A P1A C2A 101.86(11) . . ? C22A P1A C2A 103.51(11) . . ? C9A N1A C2A 109.6(2) . . ? C19A N11A C12A 109.2(2) . . ? C29A N21A C22A 108.3(2) . . ? C38A N31A C36A 109.00(18) . . ? C38A N31A C34A 109.29(18) . . ? C36A N31A C34A 111.2(2) . . ? C38A N31A C32A 110.60(19) . . ? C36A N31A C32A 108.23(18) . . ? C34A N31A C32A 108.56(18) . . ? C3A C2A N1A 108.5(2) . . ? C3A C2A P1A 124.9(2) . . ? N1A C2A P1A 126.63(18) . . ? C2A C3A C4A 106.9(2) . . ? C2A C3A C10A 127.0(3) . . ? C4A C3A C10A 126.0(2) . . ? C5A C4A C9A 118.7(3) . . ? C5A C4A C3A 134.1(3) . . ? C9A C4A C3A 107.2(2) . . ? C6A C5A C4A 119.2(3) . . ? C5A C6A C7A 121.2(3) . . ? C8A C7A C6A 121.1(3) . . ? C7A C8A C9A 118.0(3) . . ? N1A C9A C8A 130.5(3) . . ? N1A C9A C4A 107.8(2) . . ? C8A C9A C4A 121.8(3) . . ? C13A C12A N11A 108.9(2) . . ? C13A C12A P1A 123.4(2) . . ? N11A C12A P1A 127.34(19) . . ? C12A C13A C14A 107.2(2) . . ? C12A C13A C20A 128.2(2) . . ? C14A C13A C20A 124.5(2) . . ? C15A C14A C19A 119.6(3) . . ? C15A C14A C13A 133.7(3) . . ? C19A C14A C13A 106.6(2) . . ? C16A C15A C14A 118.4(3) . . ? C15A C16A C17A 121.1(3) . . ? C18A C17A C16A 121.8(3) . . ? C17A C18A C19A 117.6(3) . . ? N11A C19A C18A 130.4(3) . . ? N11A C19A C14A 108.0(2) . . ? C18A C19A C14A 121.5(2) . . ? C23A C22A N21A 109.1(2) . . ? C23A C22A P1A 124.51(18) . . ? N21A C22A P1A 126.28(18) . . ? C22A C23A C24A 107.1(2) . . ? C22A C23A C30A 127.8(2) . . ? C24A C23A C30A 125.1(2) . . ? C25A C24A C29A 119.6(2) . . ? C25A C24A C23A 134.0(2) . . ? C29A C24A C23A 106.4(2) . . ? C26A C25A C24A 118.7(2) . . ? C25A C26A C27A 120.9(2) . . ? C28A C27A C26A 122.1(2) . . ? C27A C28A C29A 117.0(2) . . ? N21A C29A C24A 109.1(2) . . ? N21A C29A C28A 129.2(2) . . ? C24A C29A C28A 121.7(2) . . ? C33A C32A N31A 115.1(2) . . ? C35A C34A N31A 115.2(2) . . ? C37A C36A N31A 115.4(2) . . ? N31A C38A C39A 115.4(2) . . ? C22B P1B C2B 104.01(10) . . ? C22B P1B C12B 105.51(11) . . ? C2B P1B C12B 102.68(11) . . ? C9B N1B C2B 109.6(2) . . ? C19B N11B C12B 109.0(2) . . ? C29B N21B C22B 108.77(19) . . ? C38B N31B C36B 111.4(2) . . ? C38B N31B C34B 109.19(19) . . ? C36B N31B C34B 109.13(19) . . ? C38B N31B C32B 108.5(2) . . ? C36B N31B C32B 108.3(2) . . ? C34B N31B C32B 110.2(2) . . ? C3B C2B N1B 108.9(2) . . ? C3B C2B P1B 124.38(19) . . ? N1B C2B P1B 126.56(18) . . ? C2B C3B C4B 106.8(2) . . ? C2B C3B C10B 128.4(2) . . ? C4B C3B C10B 124.8(2) . . ? C5B C4B C9B 118.7(2) . . ? C5B C4B C3B 134.2(3) . . ? C9B C4B C3B 107.1(2) . . ? C6B C5B C4B 119.2(3) . . ? C5B C6B C7B 120.8(3) . . ? C8B C7B C6B 121.4(3) . . ? C7B C8B C9B 118.0(3) . . ? N1B C9B C8B 130.4(3) . . ? N1B C9B C4B 107.7(2) . . ? C8B C9B C4B 121.8(2) . . ? C13B C12B N11B 108.7(2) . . ? C13B C12B P1B 123.92(19) . . ? N11B C12B P1B 127.20(18) . . ? C12B C13B C14B 107.1(2) . . ? C12B C13B C20B 128.3(2) . . ? C14B C13B C20B 124.7(2) . . ? C19B C14B C15B 119.6(2) . . ? C19B C14B C13B 107.2(2) . . ? C15B C14B C13B 133.2(2) . . ? C16B C15B C14B 118.0(3) . . ? C15B C16B C17B 121.6(3) . . ? C18B C17B C16B 122.2(3) . . ? C17B C18B C19B 116.6(3) . . ? N11B C19B C14B 108.1(2) . . ? N11B C19B C18B 129.8(2) . . ? C14B C19B C18B 122.1(2) . . ? C23B C22B N21B 108.9(2) . . ? C23B C22B P1B 124.63(17) . . ? N21B C22B P1B 126.46(17) . . ? C22B C23B C24B 107.3(2) . . ? C22B C23B C30B 127.7(2) . . ? C24B C23B C30B 125.0(2) . . ? C25B C24B C29B 118.9(2) . . ? C25B C24B C23B 134.2(2) . . ? C29B C24B C23B 106.9(2) . . ? C26B C25B C24B 118.9(2) . . ? C25B C26B C27B 121.1(2) . . ? C28B C27B C26B 121.7(2) . . ? C27B C28B C29B 117.1(2) . . ? N21B C29B C28B 129.7(2) . . ? N21B C29B C24B 108.1(2) . . ? C28B C29B C24B 122.2(2) . . ? C33B C32B N31B 115.5(2) . . ? C35B C34B N31B 115.5(2) . . ? C37B C36B N31B 114.5(2) . . ? C39B C38B N31B 115.8(2) . . ? 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 N1A H1A F1A 0.88 1.85 2.727(3) 172.5 . N11A H11A F1A 0.88 1.88 2.716(3) 159.1 . N21A H21A F1A 0.88 1.75 2.632(3) 175.1 . O3S H3S F1A 0.84 1.76 2.597(3) 171.4 . N1B H1B F1B 0.88 1.85 2.726(3) 175.7 . N11B H11B F1B 0.88 1.92 2.790(2) 168.6 . N21B H21B F1B 0.88 1.83 2.711(2) 176.2 . O1S H1S F1B 0.84 1.81 2.650(3) 177.9 . O2S H2S F1B 0.84 1.85 2.688(3) 178.7 . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.572 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.056 # start Validation Reply Form _vrf_PLAT061_k06149 ; PROBLEM: The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 RESPONSE: Since the multi-scan correction uses redundant data it corrects for more than just absorption: slight crystal alignment, poor crystal quality and maybe even sometimes partial twinning. When there are many kappa data sets within one collection, the transmission factors appear larger than they should and this is sometimes to do with inter-set scaling. You would expect this Alert to appear more for low absorbers (organics) where the absorption is minimal but the multi-scan absorption correction has been used. ; #===END data_k0775_(Compound_3) _database_code_depnum_ccdc_archive 'CCDC 662467' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H32 Cu N5 P, B F4' _chemical_formula_sum 'C39 H32 B Cu F4 N5 P' _chemical_formula_weight 752.02 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1112(4) _cell_length_b 12.1741(4) _cell_length_c 13.4482(6) _cell_angle_alpha 68.866(2) _cell_angle_beta 70.427(2) _cell_angle_gamma 72.803(2) _cell_volume 1707.76(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 7821 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.5 _exptl_crystal_description cubes _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 0.746 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.564 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18062 _diffrn_reflns_av_R_equivalents 0.1151 _diffrn_reflns_av_sigmaI/netI 0.2168 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7758 _reflns_number_gt 4903 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXTL V6.12 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL V6.12' _computing_molecular_graphics 'SHELXTL V6.12' _computing_publication_material 'SHELXTL V6.12' _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^)+(0.0722P)^2^+0.0164P] 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 7758 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1176 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1299 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Cu1 Cu 0.44898(3) 0.79639(3) 0.38141(3) 0.03069(15) Uani 1 1 d . . . P1 P 0.34667(7) 0.97700(7) 0.32920(7) 0.02314(19) Uani 1 1 d . . . N1 N 0.4288(2) 1.1794(2) 0.1708(2) 0.0263(6) Uani 1 1 d . . . H1 H 0.3633 1.2048 0.1475 0.032 Uiso 1 1 calc R . . N11 N 0.1806(2) 1.1145(2) 0.2070(2) 0.0250(6) Uani 1 1 d . . . H11 H 0.1550 1.1676 0.2441 0.030 Uiso 1 1 calc R . . N21 N 0.2389(2) 1.1686(2) 0.4202(2) 0.0260(6) Uani 1 1 d . . . H21 H 0.2838 1.2159 0.3662 0.031 Uiso 1 1 calc R . . N31 N 0.4894(2) 0.6726(2) 0.5187(2) 0.0266(6) Uani 1 1 d . . . N34 N 0.5950(2) 0.6900(2) 0.3048(2) 0.0298(6) Uani 1 1 d . . . B1 B 0.1538(3) 1.4165(3) 0.1935(3) 0.0339(9) Uani 1 1 d . . . F1 F 0.2294(2) 1.4111(2) 0.25543(19) 0.0551(6) Uani 1 1 d . . . F2 F 0.09284(19) 1.53054(17) 0.1602(2) 0.0642(7) Uani 1 1 d . . . F3 F 0.07415(15) 1.33876(16) 0.25870(16) 0.0358(5) Uani 1 1 d . . . F4 F 0.22591(16) 1.37444(17) 0.10432(16) 0.0403(5) Uani 1 1 d . . . C2 C 0.4519(3) 1.0761(3) 0.2559(3) 0.0239(7) Uani 1 1 d . . . C3 C 0.5627(3) 1.0656(3) 0.2695(3) 0.0275(7) Uani 1 1 d . . . C4 C 0.6101(3) 1.1662(3) 0.1895(3) 0.0292(7) Uani 1 1 d . . . C5 C 0.7190(3) 1.2047(3) 0.1600(3) 0.0353(8) Uani 1 1 d . . . H5A H 0.7787 1.1603 0.1986 0.042 Uiso 1 1 calc R . . C6 C 0.7371(3) 1.3071(3) 0.0750(3) 0.0437(10) Uani 1 1 d . . . H6A H 0.8092 1.3346 0.0561 0.052 Uiso 1 1 calc R . . C7 C 0.6514(3) 1.3720(3) 0.0154(3) 0.0437(9) Uani 1 1 d . . . H7A H 0.6679 1.4412 -0.0446 0.052 Uiso 1 1 calc R . . C8 C 0.5443(3) 1.3386(3) 0.0409(3) 0.0338(8) Uani 1 1 d . . . H8A H 0.4861 1.3834 0.0007 0.041 Uiso 1 1 calc R . . C9 C 0.5250(3) 1.2354(3) 0.1292(3) 0.0285(7) Uani 1 1 d . . . C10 C 0.6248(3) 0.9681(3) 0.3501(3) 0.0414(9) Uani 1 1 d . . . H10A H 0.5695 0.9157 0.4020 0.062 Uiso 1 1 calc R . . H10B H 0.6511 1.0039 0.3907 0.062 Uiso 1 1 calc R . . H10C H 0.6943 0.9208 0.3104 0.062 Uiso 1 1 calc R . . C12 C 0.2635(2) 1.0077(3) 0.2302(3) 0.0233(7) Uani 1 1 d . . . C13 C 0.2799(3) 0.9468(3) 0.1573(3) 0.0281(7) Uani 1 1 d . . . C14 C 0.2061(3) 1.0202(3) 0.0837(3) 0.0280(7) Uani 1 1 d . . . C15 C 0.1864(3) 1.0054(3) -0.0079(3) 0.0381(8) Uani 1 1 d . . . H15A H 0.2259 0.9354 -0.0309 0.046 Uiso 1 1 calc R . . C16 C 0.1095(3) 1.0935(3) -0.0629(3) 0.0427(9) Uani 1 1 d . . . H16A H 0.0969 1.0853 -0.1257 0.051 Uiso 1 1 calc R . . C17 C 0.0491(3) 1.1956(3) -0.0279(3) 0.0390(9) Uani 1 1 d . . . H17A H -0.0044 1.2552 -0.0674 0.047 Uiso 1 1 calc R . . C18 C 0.0646(3) 1.2126(3) 0.0620(3) 0.0343(8) Uani 1 1 d . . . H18A H 0.0222 1.2818 0.0855 0.041 Uiso 1 1 calc R . . C19 C 0.1452(3) 1.1237(3) 0.1174(3) 0.0243(7) Uani 1 1 d . . . C20 C 0.3588(3) 0.8282(3) 0.1489(3) 0.0465(10) Uani 1 1 d . . . H20A H 0.3823 0.7844 0.2180 0.070 Uiso 1 1 calc R . . H20B H 0.4304 0.8415 0.0880 0.070 Uiso 1 1 calc R . . H20C H 0.3154 0.7812 0.1351 0.070 Uiso 1 1 calc R . . C22 C 0.2437(3) 1.0497(3) 0.4303(3) 0.0235(7) Uani 1 1 d . . . C23 C 0.1604(2) 1.0041(3) 0.5249(3) 0.0238(7) Uani 1 1 d . . . C24 C 0.1029(2) 1.0983(3) 0.5757(3) 0.0238(7) Uani 1 1 d . . . C25 C 0.0143(3) 1.1066(3) 0.6732(3) 0.0291(7) Uani 1 1 d . . . H25A H -0.0214 1.0397 0.7201 0.035 Uiso 1 1 calc R . . C26 C -0.0201(3) 1.2122(3) 0.6999(3) 0.0342(8) Uani 1 1 d . . . H26A H -0.0794 1.2176 0.7663 0.041 Uiso 1 1 calc R . . C27 C 0.0303(3) 1.3134(3) 0.6309(3) 0.0335(8) Uani 1 1 d . . . H27A H 0.0042 1.3856 0.6515 0.040 Uiso 1 1 calc R . . C28 C 0.1173(3) 1.3091(3) 0.5336(3) 0.0314(7) Uani 1 1 d . . . H28A H 0.1511 1.3771 0.4866 0.038 Uiso 1 1 calc R . . C29 C 0.1533(3) 1.2006(3) 0.5075(3) 0.0258(7) Uani 1 1 d . . . C30 C 0.1342(3) 0.8800(3) 0.5668(3) 0.0318(8) Uani 1 1 d . . . H30A H 0.1977 0.8281 0.5268 0.048 Uiso 1 1 calc R . . H30B H 0.0574 0.8834 0.5553 0.048 Uiso 1 1 calc R . . H30C H 0.1304 0.8473 0.6457 0.048 Uiso 1 1 calc R . . C32 C 0.5911(3) 0.5904(2) 0.4951(3) 0.0246(7) Uani 1 1 d . . . C33 C 0.6471(3) 0.5992(3) 0.3800(3) 0.0251(7) Uani 1 1 d . . . C35 C 0.6469(3) 0.6974(3) 0.1986(3) 0.0383(8) Uani 1 1 d . . . H35A H 0.6128 0.7611 0.1447 0.046 Uiso 1 1 calc R . . C36 C 0.7488(3) 0.6163(3) 0.1626(3) 0.0435(9) Uani 1 1 d . . . H36A H 0.7806 0.6233 0.0862 0.052 Uiso 1 1 calc R . . C37 C 0.8019(3) 0.5274(3) 0.2380(3) 0.0383(9) Uani 1 1 d . . . H37A H 0.8723 0.4728 0.2146 0.046 Uiso 1 1 calc R . . C38 C 0.7520(3) 0.5167(3) 0.3509(3) 0.0303(7) Uani 1 1 d . . . C39 C 0.8029(3) 0.4270(3) 0.4362(3) 0.0363(8) Uani 1 1 d . . . H39A H 0.8746 0.3720 0.4165 0.044 Uiso 1 1 calc R . . C40 C 0.7511(3) 0.4192(3) 0.5439(3) 0.0345(8) Uani 1 1 d . . . H40A H 0.7867 0.3590 0.5987 0.041 Uiso 1 1 calc R . . C41 C 0.6423(3) 0.5014(3) 0.5765(3) 0.0293(7) Uani 1 1 d . . . C42 C 0.5858(3) 0.5002(3) 0.6865(3) 0.0328(8) Uani 1 1 d . . . H42A H 0.6186 0.4426 0.7442 0.039 Uiso 1 1 calc R . . C43 C 0.4842(3) 0.5813(3) 0.7102(3) 0.0334(8) Uani 1 1 d . . . H43A H 0.4450 0.5806 0.7845 0.040 Uiso 1 1 calc R . . C44 C 0.4375(3) 0.6662(3) 0.6241(3) 0.0317(8) Uani 1 1 d . . . H44A H 0.3655 0.7217 0.6419 0.038 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 Cu1 0.0322(2) 0.0241(2) 0.0326(3) -0.00608(18) -0.01376(18) 0.00258(16) P1 0.0251(4) 0.0207(4) 0.0231(4) -0.0056(3) -0.0097(3) -0.0007(3) N1 0.0228(13) 0.0276(13) 0.0269(15) -0.0058(12) -0.0070(11) -0.0049(11) N11 0.0280(13) 0.0224(13) 0.0263(15) -0.0090(11) -0.0107(11) -0.0005(10) N21 0.0280(13) 0.0221(13) 0.0235(15) -0.0046(11) -0.0027(11) -0.0057(11) N31 0.0260(13) 0.0231(13) 0.0306(16) -0.0096(12) -0.0085(11) -0.0009(11) N34 0.0296(14) 0.0288(14) 0.0294(16) -0.0073(12) -0.0081(12) -0.0045(11) B1 0.035(2) 0.0261(19) 0.034(2) -0.0079(17) -0.0040(17) -0.0029(16) F1 0.0691(15) 0.0623(15) 0.0434(14) -0.0080(12) -0.0156(12) -0.0346(12) F2 0.0508(13) 0.0270(11) 0.0772(19) 0.0031(11) 0.0009(12) 0.0035(10) F3 0.0301(10) 0.0298(10) 0.0385(12) -0.0091(9) 0.0015(8) -0.0061(8) F4 0.0387(10) 0.0417(11) 0.0358(12) -0.0142(9) 0.0004(9) -0.0090(9) C2 0.0250(15) 0.0224(15) 0.0232(17) -0.0072(13) -0.0062(12) -0.0023(12) C3 0.0234(15) 0.0311(17) 0.0314(19) -0.0152(15) -0.0080(13) -0.0014(13) C4 0.0248(15) 0.0315(17) 0.0338(19) -0.0189(15) -0.0035(13) -0.0019(13) C5 0.0247(16) 0.041(2) 0.048(2) -0.0264(18) -0.0049(15) -0.0061(14) C6 0.0281(18) 0.050(2) 0.058(3) -0.029(2) 0.0071(17) -0.0179(17) C7 0.046(2) 0.042(2) 0.038(2) -0.0152(18) 0.0104(17) -0.0214(18) C8 0.0378(18) 0.0340(18) 0.030(2) -0.0113(15) -0.0032(15) -0.0108(15) C9 0.0267(15) 0.0324(17) 0.0274(18) -0.0142(15) -0.0026(13) -0.0052(13) C10 0.0383(19) 0.040(2) 0.055(3) -0.0143(18) -0.0274(18) -0.0018(16) C12 0.0234(15) 0.0196(14) 0.0250(17) -0.0036(13) -0.0083(13) -0.0027(12) C13 0.0276(16) 0.0274(16) 0.0286(18) -0.0107(14) -0.0085(13) 0.0000(13) C14 0.0272(16) 0.0291(16) 0.0259(18) -0.0074(14) -0.0065(13) -0.0042(13) C15 0.041(2) 0.047(2) 0.034(2) -0.0225(17) -0.0123(16) -0.0035(16) C16 0.042(2) 0.063(3) 0.031(2) -0.0182(19) -0.0167(16) -0.0083(18) C17 0.0395(19) 0.046(2) 0.032(2) -0.0020(17) -0.0201(16) -0.0072(16) C18 0.0352(17) 0.0277(17) 0.037(2) -0.0037(15) -0.0154(15) -0.0028(14) C19 0.0246(14) 0.0287(16) 0.0201(17) -0.0044(13) -0.0073(12) -0.0075(12) C20 0.053(2) 0.041(2) 0.056(3) -0.0281(19) -0.032(2) 0.0150(17) C22 0.0287(15) 0.0216(15) 0.0210(17) -0.0049(13) -0.0104(13) -0.0031(12) C23 0.0240(15) 0.0259(15) 0.0230(17) -0.0041(13) -0.0103(13) -0.0060(12) C24 0.0218(14) 0.0284(16) 0.0235(17) -0.0063(13) -0.0095(12) -0.0055(12) C25 0.0240(15) 0.0371(18) 0.0250(18) -0.0052(15) -0.0074(13) -0.0078(13) C26 0.0306(17) 0.044(2) 0.030(2) -0.0180(16) -0.0075(14) -0.0015(15) C27 0.0318(17) 0.0358(18) 0.038(2) -0.0203(16) -0.0103(15) -0.0009(14) C28 0.0361(18) 0.0271(17) 0.035(2) -0.0095(15) -0.0101(15) -0.0099(14) C29 0.0260(15) 0.0253(16) 0.0257(18) -0.0079(13) -0.0065(13) -0.0039(12) C30 0.0301(17) 0.0291(17) 0.035(2) -0.0077(15) -0.0084(14) -0.0066(14) C32 0.0259(15) 0.0168(14) 0.0332(19) -0.0058(13) -0.0133(13) -0.0024(12) C33 0.0271(16) 0.0210(15) 0.0305(18) -0.0088(13) -0.0070(13) -0.0083(12) C35 0.0347(18) 0.043(2) 0.029(2) -0.0058(16) -0.0053(15) -0.0064(16) C36 0.0339(19) 0.056(2) 0.037(2) -0.0173(19) 0.0038(16) -0.0127(17) C37 0.0268(17) 0.041(2) 0.046(2) -0.0189(18) -0.0007(16) -0.0074(15) C38 0.0235(15) 0.0288(17) 0.041(2) -0.0130(15) -0.0095(14) -0.0040(13) C39 0.0274(17) 0.0242(17) 0.059(3) -0.0170(17) -0.0133(17) 0.0017(13) C40 0.0352(18) 0.0218(16) 0.047(2) -0.0061(16) -0.0203(17) -0.0005(14) C41 0.0331(17) 0.0186(15) 0.039(2) -0.0049(14) -0.0164(15) -0.0057(13) C42 0.046(2) 0.0244(16) 0.031(2) -0.0011(14) -0.0198(16) -0.0084(15) C43 0.0411(19) 0.0319(18) 0.0283(19) -0.0093(15) -0.0120(15) -0.0044(15) C44 0.0336(17) 0.0271(17) 0.035(2) -0.0108(15) -0.0098(15) -0.0037(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 Cu1 N31 2.021(3) . ? Cu1 N34 2.063(3) . ? Cu1 P1 2.1729(8) . ? P1 C12 1.801(3) . ? P1 C2 1.806(3) . ? P1 C22 1.808(3) . ? N1 C9 1.376(4) . ? N1 C2 1.392(4) . ? N11 C19 1.366(4) . ? N11 C12 1.394(3) . ? N21 C29 1.371(4) . ? N21 C22 1.389(4) . ? N31 C44 1.328(4) . ? N31 C32 1.363(4) . ? N34 C35 1.335(4) . ? N34 C33 1.360(4) . ? B1 F2 1.357(4) . ? B1 F4 1.393(4) . ? B1 F3 1.404(4) . ? B1 F1 1.404(5) . ? C2 C3 1.378(4) . ? C3 C4 1.427(5) . ? C3 C10 1.497(4) . ? C4 C9 1.408(4) . ? C4 C5 1.413(4) . ? C5 C6 1.369(5) . ? C6 C7 1.401(5) . ? C7 C8 1.369(5) . ? C8 C9 1.399(5) . ? C12 C13 1.363(4) . ? C13 C14 1.435(4) . ? C13 C20 1.496(4) . ? C14 C19 1.406(4) . ? C14 C15 1.409(5) . ? C15 C16 1.364(5) . ? C16 C17 1.399(5) . ? C17 C18 1.376(5) . ? C18 C19 1.400(4) . ? C22 C23 1.381(4) . ? C23 C24 1.428(4) . ? C23 C30 1.501(4) . ? C24 C25 1.404(4) . ? C24 C29 1.420(4) . ? C25 C26 1.367(5) . ? C26 C27 1.412(5) . ? C27 C28 1.385(5) . ? C28 C29 1.395(4) . ? C32 C41 1.400(4) . ? C32 C33 1.445(4) . ? C33 C38 1.404(4) . ? C35 C36 1.399(5) . ? C36 C37 1.359(5) . ? C37 C38 1.406(5) . ? C38 C39 1.435(5) . ? C39 C40 1.353(5) . ? C40 C41 1.441(4) . ? C41 C42 1.402(5) . ? C42 C43 1.355(4) . ? C43 C44 1.399(4) . ? 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 N31 Cu1 N34 82.24(10) . . ? N31 Cu1 P1 140.38(8) . . ? N34 Cu1 P1 135.01(8) . . ? C12 P1 C2 102.18(14) . . ? C12 P1 C22 103.65(13) . . ? C2 P1 C22 102.46(14) . . ? C12 P1 Cu1 118.25(10) . . ? C2 P1 Cu1 107.43(9) . . ? C22 P1 Cu1 120.36(10) . . ? C9 N1 C2 108.8(2) . . ? C19 N11 C12 109.3(2) . . ? C29 N21 C22 109.4(3) . . ? C44 N31 C32 117.6(3) . . ? C44 N31 Cu1 129.8(2) . . ? C32 N31 Cu1 112.3(2) . . ? C35 N34 C33 117.0(3) . . ? C35 N34 Cu1 132.0(2) . . ? C33 N34 Cu1 111.0(2) . . ? F2 B1 F4 111.7(3) . . ? F2 B1 F3 110.4(3) . . ? F4 B1 F3 108.4(3) . . ? F2 B1 F1 110.5(3) . . ? F4 B1 F1 107.0(3) . . ? F3 B1 F1 108.8(3) . . ? C3 C2 N1 109.2(3) . . ? C3 C2 P1 129.0(2) . . ? N1 C2 P1 121.7(2) . . ? C2 C3 C4 106.6(3) . . ? C2 C3 C10 127.8(3) . . ? C4 C3 C10 125.5(3) . . ? C9 C4 C5 118.1(3) . . ? C9 C4 C3 107.7(3) . . ? C5 C4 C3 134.2(3) . . ? C6 C5 C4 119.0(3) . . ? C5 C6 C7 121.3(3) . . ? C8 C7 C6 122.0(3) . . ? C7 C8 C9 116.6(3) . . ? N1 C9 C8 129.4(3) . . ? N1 C9 C4 107.6(3) . . ? C8 C9 C4 123.0(3) . . ? C13 C12 N11 109.3(3) . . ? C13 C12 P1 128.8(2) . . ? N11 C12 P1 121.3(2) . . ? C12 C13 C14 106.5(3) . . ? C12 C13 C20 129.4(3) . . ? C14 C13 C20 124.0(3) . . ? C19 C14 C15 119.6(3) . . ? C19 C14 C13 107.7(3) . . ? C15 C14 C13 132.7(3) . . ? C16 C15 C14 118.9(3) . . ? C15 C16 C17 120.8(3) . . ? C18 C17 C16 122.1(3) . . ? C17 C18 C19 117.4(3) . . ? N11 C19 C18 131.5(3) . . ? N11 C19 C14 107.2(3) . . ? C18 C19 C14 121.2(3) . . ? C23 C22 N21 109.1(3) . . ? C23 C22 P1 129.3(2) . . ? N21 C22 P1 121.6(2) . . ? C22 C23 C24 106.8(3) . . ? C22 C23 C30 127.0(3) . . ? C24 C23 C30 126.2(3) . . ? C25 C24 C29 118.6(3) . . ? C25 C24 C23 133.9(3) . . ? C29 C24 C23 107.5(3) . . ? C26 C25 C24 119.2(3) . . ? C25 C26 C27 121.5(3) . . ? C28 C27 C26 121.0(3) . . ? C27 C28 C29 117.3(3) . . ? N21 C29 C28 130.4(3) . . ? N21 C29 C24 107.3(3) . . ? C28 C29 C24 122.4(3) . . ? N31 C32 C41 122.9(3) . . ? N31 C32 C33 117.0(3) . . ? C41 C32 C33 120.1(3) . . ? N34 C33 C38 123.4(3) . . ? N34 C33 C32 117.2(3) . . ? C38 C33 C32 119.4(3) . . ? N34 C35 C36 123.4(3) . . ? C37 C36 C35 119.3(4) . . ? C36 C37 C38 119.5(3) . . ? C33 C38 C37 117.3(3) . . ? C33 C38 C39 119.3(3) . . ? C37 C38 C39 123.4(3) . . ? C40 C39 C38 121.4(3) . . ? C39 C40 C41 120.7(3) . . ? C32 C41 C42 117.3(3) . . ? C32 C41 C40 119.2(3) . . ? C42 C41 C40 123.5(3) . . ? C43 C42 C41 119.9(3) . . ? C42 C43 C44 119.4(3) . . ? N31 C44 C43 122.9(3) . . ? 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 N11 H11 F3 0.88 2.07 2.879(3) 151.8 . N1 H1 F4 0.88 2.26 2.994(3) 140.4 . N1 H1 N11 0.88 2.52 3.169(3) 130.9 . N21 H21 F1 0.88 2.34 2.983(3) 129.9 . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.575 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.086 # start Validation Reply Form _vrf_PLAT061_k0775 ; PROBLEM: The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 RESPONSE: Since the multi-scan correction uses redundant data it corrects for more than just absorption: slight crystal alignment, poor crystal quality and maybe even sometimes partial twinning. When there are many kappa data sets within one collection, the transmission factors appear larger than they should and this is sometimes to do with inter-set scaling. You would expect this Alert to appear more for low absorbers (organics) where the absorption is minimal but the multi-scan absorption correction has been used. ; #===END