# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email Catherine.Housecroft@unibas.ch _publ_contact_author_name 'Catherine E. Housecroft' _publ_author_name C.Housecroft data_esc59 _database_code_depnum_ccdc_archive 'CCDC 796687' #TrackingRef 'Cu(PS)(POP).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H45 Cu O P3 S, F6 P' _chemical_formula_sum 'C55 H45 Cu F6 O P4 S' _chemical_formula_weight 1055.41 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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn 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 11.476(2) _cell_length_b 26.337(5) _cell_length_c 16.155(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.18(3) _cell_angle_gamma 90.00 _cell_volume 4879.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12675 _cell_measurement_theta_min 3.73 _cell_measurement_theta_max 54.88 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 0.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8474 _exptl_absorpt_correction_T_max 0.8752 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70500 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9533 _reflns_number_gt 9284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0035P)^2^+12.8373P] 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 9533 _refine_ls_number_parameters 679 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.225 _refine_ls_restrained_S_all 1.226 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 0.77904(4) 0.088216(15) 0.73729(2) 0.02616(11) Uani 1 1 d . . . S1 S 0.97753(8) 0.08783(4) 0.68468(6) 0.0317(2) Uani 1 1 d . . . P1 P 0.73470(8) 0.10579(3) 0.60238(5) 0.02339(18) Uani 1 1 d . . . P2 P 0.77481(8) 0.14833(3) 0.83765(5) 0.02479(18) Uani 1 1 d . . . P3 P 0.74760(7) 0.00837(3) 0.78586(5) 0.02346(18) Uani 1 1 d . . . C1 C 1.1033(4) 0.1047(2) 0.7483(3) 0.0492(11) Uani 1 1 d . . . H1A H 1.1731 0.1030 0.7153 0.074 Uiso 1 1 calc R . . H1B H 1.1115 0.0810 0.7949 0.074 Uiso 1 1 calc R . . H1C H 1.0940 0.1393 0.7694 0.074 Uiso 1 1 calc R . . C2 C 0.9649(3) 0.13806(13) 0.6120(2) 0.0293(7) Uani 1 1 d . . . C3 C 0.8565(3) 0.14456(13) 0.5701(2) 0.0283(7) Uani 1 1 d . . . C4 C 0.8455(4) 0.18175(16) 0.5096(2) 0.0385(9) Uani 1 1 d . . . H4A H 0.7728 0.1862 0.4803 0.046 Uiso 1 1 calc R . . C5 C 0.9387(4) 0.21255(18) 0.4911(3) 0.0501(11) Uani 1 1 d . . . H5A H 0.9303 0.2375 0.4489 0.060 Uiso 1 1 calc R . . C6 C 1.0435(4) 0.20678(17) 0.5342(3) 0.0480(11) Uani 1 1 d . . . H6A H 1.1065 0.2288 0.5228 0.058 Uiso 1 1 calc R . . C7 C 1.0585(3) 0.16927(15) 0.5940(3) 0.0379(9) Uani 1 1 d . . . H7A H 1.1319 0.1650 0.6224 0.046 Uiso 1 1 calc R . . C8 C 0.6030(3) 0.13829(13) 0.5664(2) 0.0290(7) Uani 1 1 d . . . C9 C 0.5417(5) 0.1654(2) 0.6234(3) 0.0582(13) Uani 1 1 d . . . H9A H 0.5703 0.1675 0.6793 0.070 Uiso 1 1 calc R . . C10 C 0.4384(5) 0.1896(2) 0.5996(4) 0.0795(19) Uani 1 1 d . . . H10A H 0.3964 0.2081 0.6392 0.095 Uiso 1 1 calc R . . C11 C 0.3973(4) 0.1869(2) 0.5199(4) 0.0627(15) Uani 1 1 d . . . H11A H 0.3258 0.2030 0.5040 0.075 Uiso 1 1 calc R . . C12 C 0.4583(4) 0.16112(17) 0.4628(3) 0.0498(11) Uani 1 1 d . . . H12A H 0.4300 0.1602 0.4068 0.060 Uiso 1 1 calc R . . C13 C 0.5609(4) 0.13635(15) 0.4852(3) 0.0391(9) Uani 1 1 d . . . H13A H 0.6023 0.1181 0.4450 0.047 Uiso 1 1 calc R . . C14 C 0.7401(3) 0.04972(13) 0.5369(2) 0.0251(7) Uani 1 1 d . . . C15 C 0.6505(3) 0.01426(14) 0.5398(2) 0.0341(8) Uani 1 1 d . . . H15A H 0.5837 0.0214 0.5708 0.041 Uiso 1 1 calc R . . C16 C 0.6584(4) -0.03155(16) 0.4977(3) 0.0452(10) Uani 1 1 d . . . H16A H 0.5967 -0.0555 0.4993 0.054 Uiso 1 1 calc R . . C17 C 0.7561(4) -0.04212(17) 0.4533(3) 0.0501(11) Uani 1 1 d . . . H17A H 0.7625 -0.0738 0.4257 0.060 Uiso 1 1 calc R . . C18 C 0.8431(4) -0.00726(18) 0.4491(3) 0.0495(11) Uani 1 1 d . . . H18A H 0.9092 -0.0144 0.4174 0.059 Uiso 1 1 calc R . . C19 C 0.8359(3) 0.03856(16) 0.4907(2) 0.0378(9) Uani 1 1 d . . . H19A H 0.8974 0.0626 0.4875 0.045 Uiso 1 1 calc R . . C20 C 0.9097(3) 0.14948(14) 0.9019(2) 0.0303(7) Uani 1 1 d . . . O1 O 0.9188(2) 0.05791(9) 0.89517(15) 0.0299(5) Uani 1 1 d . . . C21 C 0.9658(3) 0.10411(15) 0.9234(2) 0.0321(8) Uani 1 1 d . . . C22 C 1.0710(4) 0.10322(17) 0.9678(2) 0.0419(9) Uani 1 1 d . . . H22A H 1.1086 0.0719 0.9808 0.050 Uiso 1 1 calc R . . C23 C 1.1208(4) 0.1488(2) 0.9929(3) 0.0538(12) Uani 1 1 d . . . H23A H 1.1928 0.1487 1.0239 0.065 Uiso 1 1 calc R . . C24 C 1.0679(5) 0.1938(2) 0.9739(3) 0.0584(13) Uani 1 1 d . . . H24A H 1.1029 0.2247 0.9918 0.070 Uiso 1 1 calc R . . C25 C 0.9630(4) 0.19443(17) 0.9283(3) 0.0475(11) Uani 1 1 d . . . H25A H 0.9270 0.2260 0.9149 0.057 Uiso 1 1 calc R . . C26 C 0.7496(3) 0.00694(13) 0.8987(2) 0.0280(7) Uani 1 1 d . . . C27 C 0.8326(3) 0.03586(14) 0.9416(2) 0.0292(7) Uani 1 1 d . . . C28 C 0.8304(4) 0.04204(16) 1.0268(2) 0.0377(9) Uani 1 1 d . . . H28A H 0.8881 0.0621 1.0551 0.045 Uiso 1 1 calc R . . C29 C 0.7439(4) 0.01888(17) 1.0700(2) 0.0433(10) Uani 1 1 d . . . H29A H 0.7423 0.0228 1.1284 0.052 Uiso 1 1 calc R . . C30 C 0.6598(4) -0.00988(17) 1.0291(2) 0.0419(9) Uani 1 1 d . . . H30A H 0.5999 -0.0255 1.0592 0.050 Uiso 1 1 calc R . . C31 C 0.6625(3) -0.01610(15) 0.9439(2) 0.0360(8) Uani 1 1 d . . . H31A H 0.6045 -0.0362 0.9160 0.043 Uiso 1 1 calc R . . C32 C 0.7621(3) 0.21256(13) 0.7968(2) 0.0306(8) Uani 1 1 d . . . C33 C 0.6626(4) 0.24183(16) 0.8080(4) 0.0585(14) Uani 1 1 d . . . H33A H 0.6054 0.2307 0.8449 0.070 Uiso 1 1 calc R . . C34 C 0.6474(5) 0.28718(19) 0.7651(4) 0.0745(18) Uani 1 1 d . . . H34A H 0.5790 0.3068 0.7721 0.089 Uiso 1 1 calc R . . C35 C 0.7305(5) 0.30395(17) 0.7126(4) 0.0621(14) Uani 1 1 d . . . H35A H 0.7185 0.3344 0.6820 0.074 Uiso 1 1 calc R . . C36 C 0.8310(5) 0.27646(17) 0.7047(3) 0.0547(12) Uani 1 1 d . . . H36A H 0.8913 0.2890 0.6715 0.066 Uiso 1 1 calc R . . C37 C 0.8443(4) 0.23044(15) 0.7450(3) 0.0405(9) Uani 1 1 d . . . H37A H 0.9122 0.2107 0.7366 0.049 Uiso 1 1 calc R . . C38 C 0.6591(3) 0.14465(13) 0.9116(2) 0.0318(8) Uani 1 1 d . . . C39 C 0.5476(4) 0.13357(17) 0.8813(3) 0.0461(10) Uani 1 1 d . . . H39A H 0.5347 0.1260 0.8242 0.055 Uiso 1 1 calc R . . C40 C 0.4542(4) 0.13346(19) 0.9337(3) 0.0543(12) Uani 1 1 d . . . H40A H 0.3775 0.1274 0.9119 0.065 Uiso 1 1 calc R . . C41 C 0.4727(4) 0.14200(18) 1.0167(3) 0.0517(12) Uani 1 1 d . . . H41A H 0.4092 0.1410 1.0527 0.062 Uiso 1 1 calc R . . C42 C 0.5838(4) 0.15204(18) 1.0478(3) 0.0523(12) Uani 1 1 d . . . H42A H 0.5964 0.1578 1.1054 0.063 Uiso 1 1 calc R . . C43 C 0.6780(4) 0.15383(16) 0.9957(2) 0.0403(9) Uani 1 1 d . . . H43A H 0.7542 0.1612 1.0175 0.048 Uiso 1 1 calc R . . C44 C 0.8555(3) -0.03821(12) 0.7552(2) 0.0276(7) Uani 1 1 d . . . C45 C 0.9408(4) -0.05759(18) 0.8072(3) 0.0531(12) Uani 1 1 d . . . H45A H 0.9425 -0.0487 0.8642 0.064 Uiso 1 1 calc R . . C46 C 1.0257(4) -0.0903(2) 0.7778(3) 0.0644(15) Uani 1 1 d . . . H46A H 1.0851 -0.1029 0.8149 0.077 Uiso 1 1 calc R . . C47 C 1.0243(4) -0.10430(16) 0.6971(3) 0.0455(10) Uani 1 1 d . . . H47A H 1.0821 -0.1267 0.6777 0.055 Uiso 1 1 calc R . . C48 C 0.9393(4) -0.08595(16) 0.6440(3) 0.0447(10) Uani 1 1 d . . . H48A H 0.9367 -0.0960 0.5875 0.054 Uiso 1 1 calc R . . C49 C 0.8566(4) -0.05262(16) 0.6726(2) 0.0416(10) Uani 1 1 d . . . H49A H 0.7992 -0.0393 0.6347 0.050 Uiso 1 1 calc R . . C50 C 0.6080(3) -0.02067(14) 0.7578(2) 0.0288(7) Uani 1 1 d . . . C51 C 0.5910(4) -0.07280(15) 0.7529(2) 0.0367(8) Uani 1 1 d . . . H51A H 0.6551 -0.0952 0.7622 0.044 Uiso 1 1 calc R . . C52 C 0.4805(4) -0.09242(18) 0.7345(3) 0.0463(10) Uani 1 1 d . . . H52A H 0.4691 -0.1281 0.7321 0.056 Uiso 1 1 calc R . . C53 C 0.3880(4) -0.0604(2) 0.7198(3) 0.0485(11) Uani 1 1 d . . . H53A H 0.3128 -0.0740 0.7070 0.058 Uiso 1 1 calc R . . C54 C 0.4034(4) -0.00886(19) 0.7234(3) 0.0456(10) Uani 1 1 d . . . H54A H 0.3389 0.0131 0.7131 0.055 Uiso 1 1 calc R . . C55 C 0.5133(3) 0.01142(16) 0.7420(2) 0.0370(8) Uani 1 1 d . . . H55A H 0.5238 0.0472 0.7439 0.044 Uiso 1 1 calc R . . P10 P 0.2369(8) 0.2690(4) 0.7679(8) 0.054(2) Uani 0.53(3) 1 d PU A 1 F10 F 0.2361(8) 0.3240(4) 0.8065(12) 0.087(4) Uani 0.53(3) 1 d P A 1 F11 F 0.3647(15) 0.2656(8) 0.7884(12) 0.075(4) Uani 0.53(3) 1 d P A 1 F12 F 0.1075(17) 0.2663(10) 0.7524(16) 0.136(8) Uani 0.53(3) 1 d PU A 1 F13 F 0.2743(13) 0.2877(9) 0.6825(10) 0.110(6) Uani 0.53(3) 1 d P A 1 F14 F 0.2452(17) 0.2125(6) 0.7422(11) 0.113(6) Uani 0.53(3) 1 d P A 1 F15 F 0.2202(14) 0.2484(5) 0.8598(8) 0.103(4) Uani 0.53(3) 1 d P A 1 P10' P 0.2357(10) 0.2728(4) 0.7572(10) 0.060(3) Uani 0.47(3) 1 d PU A 2 F10' F 0.2389(8) 0.3329(4) 0.742(2) 0.114(8) Uani 0.47(3) 1 d P A 2 F11' F 0.3786(18) 0.2723(8) 0.7764(16) 0.091(7) Uani 0.47(3) 1 d P A 2 F12' F 0.0951(15) 0.2800(6) 0.7322(11) 0.062(3) Uani 0.47(3) 1 d P A 2 F13' F 0.2450(12) 0.2658(6) 0.6586(8) 0.076(3) Uani 0.47(3) 1 d P A 2 F14' F 0.223(2) 0.2140(6) 0.7615(12) 0.119(8) Uani 0.47(3) 1 d P A 2 F15' F 0.2046(13) 0.2797(13) 0.8485(11) 0.141(9) Uani 0.47(3) 1 d PU A 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 Cu1 0.0356(2) 0.0213(2) 0.0216(2) -0.00062(16) 0.00181(16) 0.00136(17) S1 0.0316(5) 0.0330(5) 0.0307(4) 0.0012(4) 0.0052(4) 0.0049(4) P1 0.0259(4) 0.0234(4) 0.0209(4) 0.0001(3) 0.0015(3) -0.0021(3) P2 0.0274(4) 0.0227(4) 0.0245(4) -0.0042(3) 0.0037(3) -0.0011(3) P3 0.0248(4) 0.0222(4) 0.0233(4) 0.0020(3) -0.0006(3) -0.0003(3) C1 0.032(2) 0.075(3) 0.040(2) 0.006(2) -0.0010(17) 0.002(2) C2 0.0332(19) 0.0270(17) 0.0279(17) 0.0001(14) 0.0043(14) -0.0009(14) C3 0.0300(18) 0.0294(17) 0.0257(17) 0.0001(14) 0.0033(14) -0.0058(14) C4 0.038(2) 0.045(2) 0.032(2) 0.0099(17) -0.0015(16) -0.0078(18) C5 0.051(3) 0.048(3) 0.052(3) 0.025(2) 0.002(2) -0.010(2) C6 0.044(2) 0.043(2) 0.058(3) 0.011(2) 0.007(2) -0.017(2) C7 0.033(2) 0.040(2) 0.041(2) 0.0015(17) 0.0012(16) -0.0066(17) C8 0.0290(18) 0.0243(17) 0.0339(18) 0.0044(14) 0.0060(15) 0.0015(14) C9 0.065(3) 0.065(3) 0.046(3) -0.001(2) 0.016(2) 0.025(3) C10 0.071(4) 0.090(4) 0.080(4) 0.010(3) 0.032(3) 0.050(3) C11 0.035(2) 0.057(3) 0.097(4) 0.028(3) 0.010(3) 0.015(2) C12 0.038(2) 0.045(2) 0.066(3) 0.013(2) -0.011(2) 0.0032(19) C13 0.038(2) 0.039(2) 0.040(2) 0.0003(17) -0.0049(17) 0.0085(17) C14 0.0264(17) 0.0254(16) 0.0234(16) -0.0007(13) -0.0023(13) 0.0041(13) C15 0.0317(19) 0.0340(19) 0.036(2) -0.0031(16) -0.0035(15) -0.0010(16) C16 0.051(3) 0.033(2) 0.051(2) -0.0081(18) -0.014(2) -0.0057(19) C17 0.063(3) 0.042(2) 0.045(2) -0.0203(19) -0.014(2) 0.015(2) C18 0.046(2) 0.058(3) 0.045(2) -0.021(2) 0.0009(19) 0.015(2) C19 0.034(2) 0.047(2) 0.033(2) -0.0102(17) 0.0051(16) 0.0020(17) C20 0.0314(18) 0.0308(18) 0.0286(18) -0.0053(14) 0.0021(14) -0.0049(15) O1 0.0319(13) 0.0308(13) 0.0272(12) 0.0001(10) 0.0018(10) -0.0023(10) C21 0.0321(19) 0.038(2) 0.0264(17) -0.0028(15) 0.0002(14) -0.0058(16) C22 0.036(2) 0.052(2) 0.037(2) -0.0015(18) -0.0066(17) -0.0007(19) C23 0.042(2) 0.067(3) 0.051(3) -0.007(2) -0.015(2) -0.013(2) C24 0.060(3) 0.053(3) 0.061(3) -0.013(2) -0.016(2) -0.019(2) C25 0.053(3) 0.039(2) 0.050(3) -0.0094(19) -0.009(2) -0.003(2) C26 0.0319(18) 0.0274(17) 0.0246(16) 0.0024(14) 0.0000(14) -0.0007(14) C27 0.0310(18) 0.0312(18) 0.0255(17) 0.0048(14) 0.0014(14) 0.0012(15) C28 0.046(2) 0.042(2) 0.0250(18) 0.0006(16) -0.0036(16) -0.0041(18) C29 0.054(3) 0.052(2) 0.0244(18) 0.0030(17) 0.0067(17) -0.003(2) C30 0.044(2) 0.049(2) 0.033(2) 0.0090(18) 0.0090(17) -0.0066(19) C31 0.038(2) 0.038(2) 0.0318(19) 0.0064(16) 0.0026(16) -0.0065(17) C32 0.0319(19) 0.0222(16) 0.0375(19) -0.0057(14) 0.0011(15) -0.0037(14) C33 0.050(3) 0.031(2) 0.096(4) -0.001(2) 0.029(3) 0.0064(19) C34 0.055(3) 0.035(2) 0.134(6) 0.008(3) 0.013(3) 0.014(2) C35 0.060(3) 0.027(2) 0.097(4) 0.014(2) -0.019(3) -0.008(2) C36 0.059(3) 0.039(2) 0.066(3) 0.015(2) 0.003(2) -0.010(2) C37 0.038(2) 0.032(2) 0.052(2) 0.0029(18) 0.0068(18) -0.0022(17) C38 0.0356(19) 0.0262(17) 0.0345(19) -0.0062(15) 0.0114(15) -0.0055(15) C39 0.041(2) 0.054(3) 0.044(2) -0.016(2) 0.0107(19) -0.013(2) C40 0.039(2) 0.062(3) 0.063(3) -0.018(2) 0.016(2) -0.017(2) C41 0.051(3) 0.052(3) 0.054(3) -0.009(2) 0.030(2) -0.009(2) C42 0.068(3) 0.056(3) 0.034(2) -0.004(2) 0.020(2) 0.007(2) C43 0.043(2) 0.043(2) 0.036(2) -0.0060(17) 0.0072(17) 0.0034(18) C44 0.0268(17) 0.0209(16) 0.0349(18) 0.0022(14) -0.0009(14) -0.0009(13) C45 0.061(3) 0.052(3) 0.044(2) -0.018(2) -0.021(2) 0.027(2) C46 0.054(3) 0.065(3) 0.072(3) -0.024(3) -0.030(3) 0.032(3) C47 0.035(2) 0.036(2) 0.066(3) -0.010(2) 0.005(2) 0.0034(17) C48 0.051(3) 0.042(2) 0.041(2) 0.0033(18) 0.0119(19) 0.017(2) C49 0.047(2) 0.046(2) 0.032(2) 0.0059(17) 0.0050(17) 0.0176(19) C50 0.0303(18) 0.0315(18) 0.0246(17) 0.0014(14) -0.0007(14) -0.0045(14) C51 0.038(2) 0.033(2) 0.039(2) 0.0010(16) -0.0022(16) -0.0053(16) C52 0.049(3) 0.047(2) 0.043(2) -0.0052(19) 0.0028(19) -0.021(2) C53 0.034(2) 0.077(3) 0.035(2) -0.007(2) 0.0014(17) -0.018(2) C54 0.029(2) 0.069(3) 0.038(2) 0.000(2) -0.0033(17) 0.005(2) C55 0.0323(19) 0.041(2) 0.037(2) -0.0007(17) -0.0035(16) 0.0011(17) P10 0.025(3) 0.082(5) 0.054(3) -0.016(2) 0.0072(17) -0.019(2) F10 0.062(5) 0.066(5) 0.136(11) -0.023(6) 0.013(6) 0.004(4) F11 0.031(6) 0.093(9) 0.101(7) 0.012(6) -0.015(6) -0.008(5) F12 0.027(4) 0.205(19) 0.173(16) -0.054(13) -0.021(7) -0.008(10) F13 0.090(7) 0.178(16) 0.062(7) 0.050(8) 0.008(6) 0.015(8) F14 0.112(8) 0.090(9) 0.139(11) -0.075(9) 0.022(8) -0.049(6) F15 0.127(9) 0.105(8) 0.082(6) -0.001(6) 0.050(6) -0.040(7) P10' 0.042(4) 0.044(3) 0.094(8) -0.038(4) 0.018(4) -0.013(2) F10' 0.052(5) 0.041(4) 0.25(2) -0.030(8) 0.007(8) -0.003(3) F11' 0.031(5) 0.058(6) 0.186(17) -0.041(9) 0.028(6) -0.020(4) F12' 0.029(6) 0.072(6) 0.084(6) -0.009(5) 0.004(5) -0.006(4) F13' 0.057(6) 0.102(8) 0.069(6) -0.008(5) -0.005(4) 0.033(5) F14' 0.183(19) 0.067(9) 0.104(10) 0.042(8) -0.056(11) -0.041(9) F15' 0.102(8) 0.24(2) 0.077(9) -0.101(13) 0.002(7) -0.016(13) _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 P1 2.2667(10) . ? Cu1 P2 2.2681(10) . ? Cu1 P3 2.2782(10) . ? Cu1 S1 2.4614(11) . ? S1 C2 1.772(4) . ? S1 C1 1.796(4) . ? P1 C8 1.813(4) . ? P1 C14 1.819(3) . ? P1 C3 1.823(3) . ? P2 C32 1.820(4) . ? P2 C38 1.823(4) . ? P2 C20 1.831(4) . ? P3 C50 1.817(4) . ? P3 C26 1.822(3) . ? P3 C44 1.824(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.392(5) . ? C2 C3 1.404(5) . ? C3 C4 1.386(5) . ? C4 C5 1.384(6) . ? C4 H4A 0.9500 . ? C5 C6 1.374(6) . ? C5 H5A 0.9500 . ? C6 C7 1.389(6) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.379(6) . ? C8 C13 1.381(5) . ? C9 C10 1.386(7) . ? C9 H9A 0.9500 . ? C10 C11 1.356(8) . ? C10 H10A 0.9500 . ? C11 C12 1.360(7) . ? C11 H11A 0.9500 . ? C12 C13 1.383(6) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C19 1.383(5) . ? C14 C15 1.392(5) . ? C15 C16 1.390(5) . ? C15 H15A 0.9500 . ? C16 C17 1.382(7) . ? C16 H16A 0.9500 . ? C17 C18 1.360(7) . ? C17 H17A 0.9500 . ? C18 C19 1.386(6) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C25 1.392(5) . ? C20 C21 1.395(5) . ? O1 C27 1.391(4) . ? O1 C21 1.400(4) . ? C21 C22 1.381(5) . ? C22 C23 1.385(6) . ? C22 H22A 0.9500 . ? C23 C24 1.359(7) . ? C23 H23A 0.9500 . ? C24 C25 1.388(7) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C27 1.385(5) . ? C26 C31 1.400(5) . ? C27 C28 1.387(5) . ? C28 C29 1.377(6) . ? C28 H28A 0.9500 . ? C29 C30 1.376(6) . ? C29 H29A 0.9500 . ? C30 C31 1.387(5) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 C37 1.368(5) . ? C32 C33 1.395(6) . ? C33 C34 1.389(7) . ? C33 H33A 0.9500 . ? C34 C35 1.373(8) . ? C34 H34A 0.9500 . ? C35 C36 1.372(7) . ? C35 H35A 0.9500 . ? C36 C37 1.382(6) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? C38 C39 1.384(6) . ? C38 C43 1.388(5) . ? C39 C40 1.391(6) . ? C39 H39A 0.9500 . ? C40 C41 1.367(7) . ? C40 H40A 0.9500 . ? C41 C42 1.378(7) . ? C41 H41A 0.9500 . ? C42 C43 1.396(6) . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? C44 C45 1.363(5) . ? C44 C49 1.389(5) . ? C45 C46 1.397(6) . ? C45 H45A 0.9500 . ? C46 C47 1.355(7) . ? C46 H46A 0.9500 . ? C47 C48 1.363(6) . ? C47 H47A 0.9500 . ? C48 C49 1.384(5) . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C50 C51 1.389(5) . ? C50 C55 1.392(5) . ? C51 C52 1.391(6) . ? C51 H51A 0.9500 . ? C52 C53 1.369(7) . ? C52 H52A 0.9500 . ? C53 C54 1.370(7) . ? C53 H53A 0.9500 . ? C54 C55 1.392(6) . ? C54 H54A 0.9500 . ? C55 H55A 0.9500 . ? P10 F11 1.494(18) . ? P10 F12 1.50(2) . ? P10 F13 1.542(16) . ? P10 F14 1.549(18) . ? P10 F10 1.578(13) . ? P10 F15 1.597(18) . ? P10' F15' 1.541(19) . ? P10' F14' 1.555(18) . ? P10' F10' 1.605(16) . ? P10' F13' 1.612(18) . ? P10' F11' 1.66(2) . ? P10' F12' 1.66(2) . ? 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 Cu1 P2 122.33(4) . . ? P1 Cu1 P3 119.14(4) . . ? P2 Cu1 P3 112.96(4) . . ? P1 Cu1 S1 81.12(4) . . ? P2 Cu1 S1 107.16(4) . . ? P3 Cu1 S1 106.01(4) . . ? C2 S1 C1 103.8(2) . . ? C2 S1 Cu1 99.94(12) . . ? C1 S1 Cu1 122.39(15) . . ? C8 P1 C14 104.09(16) . . ? C8 P1 C3 106.40(16) . . ? C14 P1 C3 104.15(16) . . ? C8 P1 Cu1 123.95(12) . . ? C14 P1 Cu1 112.47(11) . . ? C3 P1 Cu1 104.07(12) . . ? C32 P2 C38 103.72(17) . . ? C32 P2 C20 104.15(17) . . ? C38 P2 C20 104.51(17) . . ? C32 P2 Cu1 113.15(12) . . ? C38 P2 Cu1 117.88(12) . . ? C20 P2 Cu1 112.10(12) . . ? C50 P3 C26 102.59(16) . . ? C50 P3 C44 104.52(16) . . ? C26 P3 C44 105.92(16) . . ? C50 P3 Cu1 116.89(12) . . ? C26 P3 Cu1 111.56(12) . . ? C44 P3 Cu1 114.16(11) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 120.3(3) . . ? C7 C2 S1 122.4(3) . . ? C3 C2 S1 117.3(3) . . ? C4 C3 C2 118.7(3) . . ? C4 C3 P1 123.2(3) . . ? C2 C3 P1 118.0(3) . . ? C5 C4 C3 121.1(4) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C6 C5 C4 119.6(4) . . ? C6 C5 H5A 120.2 . . ? C4 C5 H5A 120.2 . . ? C5 C6 C7 120.9(4) . . ? C5 C6 H6A 119.5 . . ? C7 C6 H6A 119.5 . . ? C6 C7 C2 119.3(4) . . ? C6 C7 H7A 120.4 . . ? C2 C7 H7A 120.4 . . ? C9 C8 C13 119.0(4) . . ? C9 C8 P1 118.1(3) . . ? C13 C8 P1 123.0(3) . . ? C8 C9 C10 120.3(5) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 120.1(5) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C10 C11 C12 120.1(4) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C13 120.8(5) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C8 C13 C12 119.7(4) . . ? C8 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C19 C14 C15 118.7(3) . . ? C19 C14 P1 122.1(3) . . ? C15 C14 P1 118.9(3) . . ? C16 C15 C14 120.2(4) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C17 C16 C15 119.9(4) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C18 C17 C16 120.1(4) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C19 120.4(4) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C14 C19 C18 120.7(4) . . ? C14 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C25 C20 C21 117.3(4) . . ? C25 C20 P2 122.7(3) . . ? C21 C20 P2 119.9(3) . . ? C27 O1 C21 117.4(3) . . ? C22 C21 C20 122.0(4) . . ? C22 C21 O1 118.2(4) . . ? C20 C21 O1 119.7(3) . . ? C21 C22 C23 118.7(4) . . ? C21 C22 H22A 120.6 . . ? C23 C22 H22A 120.6 . . ? C24 C23 C22 120.9(4) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 C25 120.1(4) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C24 C25 C20 120.9(4) . . ? C24 C25 H25A 119.5 . . ? C20 C25 H25A 119.5 . . ? C27 C26 C31 117.9(3) . . ? C27 C26 P3 118.2(3) . . ? C31 C26 P3 123.3(3) . . ? C26 C27 C28 121.6(3) . . ? C26 C27 O1 116.6(3) . . ? C28 C27 O1 121.8(3) . . ? C29 C28 C27 119.4(4) . . ? C29 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? C30 C29 C28 120.5(4) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 119.9(4) . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C30 C31 C26 120.7(4) . . ? C30 C31 H31A 119.6 . . ? C26 C31 H31A 119.6 . . ? C37 C32 C33 118.4(4) . . ? C37 C32 P2 119.6(3) . . ? C33 C32 P2 121.4(3) . . ? C34 C33 C32 119.9(5) . . ? C34 C33 H33A 120.1 . . ? C32 C33 H33A 120.1 . . ? C35 C34 C33 120.5(5) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C36 C35 C34 119.6(4) . . ? C36 C35 H35A 120.2 . . ? C34 C35 H35A 120.2 . . ? C35 C36 C37 119.8(5) . . ? C35 C36 H36A 120.1 . . ? C37 C36 H36A 120.1 . . ? C32 C37 C36 121.6(4) . . ? C32 C37 H37A 119.2 . . ? C36 C37 H37A 119.2 . . ? C39 C38 C43 119.5(4) . . ? C39 C38 P2 117.7(3) . . ? C43 C38 P2 122.8(3) . . ? C38 C39 C40 120.5(4) . . ? C38 C39 H39A 119.8 . . ? C40 C39 H39A 119.8 . . ? C41 C40 C39 120.2(4) . . ? C41 C40 H40A 119.9 . . ? C39 C40 H40A 119.9 . . ? C40 C41 C42 119.7(4) . . ? C40 C41 H41A 120.2 . . ? C42 C41 H41A 120.2 . . ? C41 C42 C43 120.9(4) . . ? C41 C42 H42A 119.5 . . ? C43 C42 H42A 119.5 . . ? C38 C43 C42 119.2(4) . . ? C38 C43 H43A 120.4 . . ? C42 C43 H43A 120.4 . . ? C45 C44 C49 117.1(4) . . ? C45 C44 P3 124.3(3) . . ? C49 C44 P3 118.4(3) . . ? C44 C45 C46 121.1(4) . . ? C44 C45 H45A 119.5 . . ? C46 C45 H45A 119.5 . . ? C47 C46 C45 120.8(4) . . ? C47 C46 H46A 119.6 . . ? C45 C46 H46A 119.6 . . ? C46 C47 C48 119.4(4) . . ? C46 C47 H47A 120.3 . . ? C48 C47 H47A 120.3 . . ? C47 C48 C49 119.9(4) . . ? C47 C48 H48A 120.1 . . ? C49 C48 H48A 120.1 . . ? C48 C49 C44 121.7(4) . . ? C48 C49 H49A 119.2 . . ? C44 C49 H49A 119.2 . . ? C51 C50 C55 118.9(3) . . ? C51 C50 P3 123.4(3) . . ? C55 C50 P3 117.7(3) . . ? C50 C51 C52 120.3(4) . . ? C50 C51 H51A 119.9 . . ? C52 C51 H51A 119.9 . . ? C53 C52 C51 120.2(4) . . ? C53 C52 H52A 119.9 . . ? C51 C52 H52A 119.9 . . ? C52 C53 C54 120.3(4) . . ? C52 C53 H53A 119.8 . . ? C54 C53 H53A 119.8 . . ? C53 C54 C55 120.3(4) . . ? C53 C54 H54A 119.9 . . ? C55 C54 H54A 119.9 . . ? C50 C55 C54 120.0(4) . . ? C50 C55 H55A 120.0 . . ? C54 C55 H55A 120.0 . . ? F11 P10 F12 173.2(18) . . ? F11 P10 F13 85.0(11) . . ? F12 P10 F13 100.0(15) . . ? F11 P10 F14 86.1(12) . . ? F12 P10 F14 88.9(13) . . ? F13 P10 F14 92.5(11) . . ? F11 P10 F10 89.3(10) . . ? F12 P10 F10 95.1(11) . . ? F13 P10 F10 93.8(10) . . ? F14 P10 F10 171.9(13) . . ? F11 P10 F15 85.8(12) . . ? F12 P10 F15 89.2(12) . . ? F13 P10 F15 170.7(11) . . ? F14 P10 F15 86.3(10) . . ? F10 P10 F15 86.7(8) . . ? F15' P10' F14' 93.0(14) . . ? F15' P10' F10' 92.1(10) . . ? F14' P10' F10' 172.7(14) . . ? F15' P10' F13' 170.4(11) . . ? F14' P10' F13' 86.5(10) . . ? F10' P10' F13' 87.5(11) . . ? F15' P10' F11' 94.9(13) . . ? F14' P10' F11' 94.4(13) . . ? F10' P10' F11' 90.4(10) . . ? F13' P10' F11' 94.7(12) . . ? F15' P10' F12' 87.8(11) . . ? F14' P10' F12' 92.0(12) . . ? F10' P10' F12' 82.9(9) . . ? F13' P10' F12' 82.6(10) . . ? F11' P10' F12' 172.9(14) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.588 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.068 # Attachment 'Cu(PS)(bpy).CIF' data_esc57 _database_code_depnum_ccdc_archive 'CCDC 796688' #TrackingRef 'Cu(PS)(bpy).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H25 Cu N2 P S, F6 P' _chemical_formula_sum 'C29 H25 Cu F6 N2 P2 S' _chemical_formula_weight 673.07 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' S S 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn 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 10.4500(14) _cell_length_b 19.688(4) _cell_length_c 13.830(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.245(11) _cell_angle_gamma 90.00 _cell_volume 2845.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3003 _cell_measurement_theta_min 7.28 _cell_measurement_theta_max 69.56 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7174 _exptl_absorpt_correction_T_max 0.9605 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44421 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6200 _reflns_number_gt 5859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0340P)^2^+2.8874P] 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 6200 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.24636(2) 0.164409(12) 0.219288(16) 0.02189(7) Uani 1 1 d . . . P1 P 0.10294(4) 0.24279(2) 0.24539(3) 0.01715(10) Uani 1 1 d . . . S1 S 0.12785(5) 0.12879(2) 0.08264(4) 0.02828(12) Uani 1 1 d . . . C1 C 0.2365(3) 0.12683(16) -0.01907(18) 0.0531(8) Uani 1 1 d . . . H1A H 0.1885 0.1164 -0.0783 0.080 Uiso 1 1 calc R . . H1B H 0.3017 0.0919 -0.0082 0.080 Uiso 1 1 calc R . . H1C H 0.2779 0.1712 -0.0258 0.080 Uiso 1 1 calc R . . C2 C 0.04011(18) 0.20453(10) 0.05740(13) 0.0224(4) Uani 1 1 d . . . C3 C 0.02960(17) 0.25573(9) 0.12685(12) 0.0193(3) Uani 1 1 d . . . C4 C -0.03886(18) 0.31436(10) 0.10329(14) 0.0237(4) Uani 1 1 d . . . H4A H -0.0473 0.3495 0.1499 0.028 Uiso 1 1 calc R . . C5 C -0.09453(19) 0.32202(11) 0.01299(14) 0.0277(4) Uani 1 1 d . . . H5A H -0.1395 0.3626 -0.0025 0.033 Uiso 1 1 calc R . . C6 C -0.0847(2) 0.27068(12) -0.05461(14) 0.0306(4) Uani 1 1 d . . . H6A H -0.1232 0.2759 -0.1165 0.037 Uiso 1 1 calc R . . C7 C -0.0189(2) 0.21161(11) -0.03267(14) 0.0290(4) Uani 1 1 d . . . H7A H -0.0141 0.1760 -0.0788 0.035 Uiso 1 1 calc R . . C8 C -0.02989(18) 0.21483(9) 0.32021(13) 0.0202(3) Uani 1 1 d . . . C9 C -0.0011(2) 0.18489(10) 0.40905(14) 0.0260(4) Uani 1 1 d . . . H9A H 0.0856 0.1783 0.4276 0.031 Uiso 1 1 calc R . . C10 C -0.0985(2) 0.16479(11) 0.47032(16) 0.0344(5) Uani 1 1 d . . . H10A H -0.0784 0.1443 0.5307 0.041 Uiso 1 1 calc R . . C11 C -0.2252(2) 0.17448(11) 0.44358(17) 0.0377(5) Uani 1 1 d . . . H11A H -0.2918 0.1609 0.4859 0.045 Uiso 1 1 calc R . . C12 C -0.2546(2) 0.20380(12) 0.35588(17) 0.0358(5) Uani 1 1 d . . . H12A H -0.3415 0.2102 0.3377 0.043 Uiso 1 1 calc R . . C13 C -0.15748(19) 0.22401(11) 0.29399(15) 0.0275(4) Uani 1 1 d . . . H13A H -0.1782 0.2442 0.2335 0.033 Uiso 1 1 calc R . . C14 C 0.13454(18) 0.32756(9) 0.29256(12) 0.0195(3) Uani 1 1 d . . . C15 C 0.0426(2) 0.36437(10) 0.34264(14) 0.0259(4) Uani 1 1 d . . . H15A H -0.0408 0.3461 0.3507 0.031 Uiso 1 1 calc R . . C16 C 0.0722(2) 0.42747(11) 0.38073(16) 0.0327(4) Uani 1 1 d . . . H16A H 0.0090 0.4526 0.4146 0.039 Uiso 1 1 calc R . . C17 C 0.1935(2) 0.45392(11) 0.36949(16) 0.0344(5) Uani 1 1 d . . . H17A H 0.2138 0.4970 0.3965 0.041 Uiso 1 1 calc R . . C18 C 0.2850(2) 0.41846(11) 0.31951(17) 0.0344(5) Uani 1 1 d . . . H18A H 0.3680 0.4373 0.3111 0.041 Uiso 1 1 calc R . . C19 C 0.25612(19) 0.35510(11) 0.28125(15) 0.0276(4) Uani 1 1 d . . . H19A H 0.3197 0.3304 0.2472 0.033 Uiso 1 1 calc R . . N1 N 0.28913(15) 0.08162(8) 0.30151(11) 0.0203(3) Uani 1 1 d . . . N2 N 0.43694(16) 0.15716(9) 0.18939(12) 0.0268(3) Uani 1 1 d . . . C20 C 0.21155(19) 0.04785(10) 0.36076(14) 0.0243(4) Uani 1 1 d . . . H20A H 0.1238 0.0603 0.3626 0.029 Uiso 1 1 calc R . . C21 C 0.2531(2) -0.00458(10) 0.41968(15) 0.0289(4) Uani 1 1 d . . . H21A H 0.1956 -0.0275 0.4615 0.035 Uiso 1 1 calc R . . C22 C 0.3804(2) -0.02249(11) 0.41587(16) 0.0328(5) Uani 1 1 d . . . H22A H 0.4122 -0.0577 0.4563 0.039 Uiso 1 1 calc R . . C23 C 0.4619(2) 0.01066(10) 0.35342(15) 0.0295(4) Uani 1 1 d . . . H23A H 0.5495 -0.0019 0.3494 0.035 Uiso 1 1 calc R . . C24 C 0.41314(18) 0.06279(9) 0.29652(13) 0.0216(4) Uani 1 1 d . . . C25 C 0.49198(18) 0.10109(10) 0.22687(14) 0.0235(4) Uani 1 1 d . . . C26 C 0.6145(2) 0.08092(12) 0.19978(16) 0.0332(5) Uani 1 1 d . . . H26A H 0.6517 0.0410 0.2264 0.040 Uiso 1 1 calc R . . C27 C 0.6810(2) 0.11967(14) 0.13378(18) 0.0408(5) Uani 1 1 d . . . H27A H 0.7641 0.1062 0.1138 0.049 Uiso 1 1 calc R . . C28 C 0.6265(2) 0.17769(15) 0.09726(17) 0.0421(6) Uani 1 1 d . . . H28A H 0.6714 0.2055 0.0527 0.050 Uiso 1 1 calc R . . C29 C 0.5043(2) 0.19466(13) 0.12711(16) 0.0364(5) Uani 1 1 d . . . H29A H 0.4665 0.2349 0.1021 0.044 Uiso 1 1 calc R . . P10 P 0.14094(5) 0.07774(4) 0.69615(4) 0.03562(14) Uani 1 1 d . . . F10 F 0.11418(18) 0.02892(11) 0.78400(14) 0.0684(5) Uani 1 1 d . . . F11 F 0.16661(19) 0.12679(15) 0.60803(16) 0.0921(8) Uani 1 1 d . . . F12 F 0.27473(16) 0.09597(14) 0.74516(14) 0.0800(7) Uani 1 1 d . . . F13 F 0.0746(2) 0.13684(11) 0.75260(17) 0.0814(6) Uani 1 1 d . . . F14 F 0.2130(3) 0.01902(17) 0.64110(17) 0.1185(12) Uani 1 1 d . . . F15 F 0.00981(17) 0.05736(11) 0.64857(14) 0.0691(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02113(12) 0.02253(12) 0.02200(12) 0.00324(8) -0.00219(8) 0.00504(9) P1 0.0180(2) 0.0180(2) 0.0154(2) 0.00114(16) -0.00195(16) 0.00087(16) S1 0.0393(3) 0.0227(2) 0.0228(2) -0.00276(18) -0.00731(19) 0.0058(2) C1 0.0699(19) 0.0611(17) 0.0282(12) 0.0012(11) 0.0093(11) 0.0354(15) C2 0.0234(9) 0.0244(9) 0.0193(8) 0.0013(7) -0.0028(7) 0.0022(7) C3 0.0179(8) 0.0236(9) 0.0163(8) 0.0033(7) -0.0006(6) 0.0003(7) C4 0.0224(9) 0.0267(9) 0.0220(9) 0.0029(7) 0.0006(7) 0.0053(7) C5 0.0227(9) 0.0356(11) 0.0247(9) 0.0092(8) -0.0012(7) 0.0075(8) C6 0.0267(10) 0.0450(12) 0.0202(9) 0.0058(8) -0.0064(7) 0.0028(9) C7 0.0308(10) 0.0359(11) 0.0203(9) -0.0030(8) -0.0071(8) 0.0016(9) C8 0.0256(9) 0.0160(8) 0.0190(8) -0.0025(6) 0.0019(7) -0.0020(7) C9 0.0357(11) 0.0207(9) 0.0217(9) 0.0005(7) 0.0015(8) 0.0017(8) C10 0.0537(14) 0.0242(10) 0.0254(10) 0.0038(8) 0.0098(9) -0.0018(9) C11 0.0449(13) 0.0294(11) 0.0390(12) -0.0033(9) 0.0205(10) -0.0123(10) C12 0.0270(10) 0.0384(12) 0.0419(12) -0.0056(10) 0.0072(9) -0.0093(9) C13 0.0254(10) 0.0309(10) 0.0264(9) -0.0014(8) -0.0002(8) -0.0062(8) C14 0.0228(9) 0.0181(8) 0.0176(8) 0.0029(6) -0.0041(6) -0.0009(7) C15 0.0270(10) 0.0234(9) 0.0273(9) -0.0007(7) 0.0014(7) -0.0021(8) C16 0.0420(12) 0.0235(10) 0.0327(11) -0.0039(8) 0.0033(9) 0.0009(9) C17 0.0467(13) 0.0215(9) 0.0351(11) -0.0010(8) -0.0066(9) -0.0086(9) C18 0.0299(11) 0.0311(11) 0.0420(12) 0.0036(9) -0.0060(9) -0.0109(9) C19 0.0239(9) 0.0271(10) 0.0318(10) 0.0035(8) -0.0013(8) -0.0021(8) N1 0.0230(8) 0.0179(7) 0.0201(7) -0.0019(6) -0.0026(6) 0.0016(6) N2 0.0238(8) 0.0314(9) 0.0253(8) 0.0029(7) 0.0003(6) -0.0009(7) C20 0.0269(9) 0.0203(9) 0.0256(9) -0.0018(7) 0.0004(7) -0.0011(7) C21 0.0386(11) 0.0219(9) 0.0263(10) 0.0023(8) -0.0011(8) -0.0049(8) C22 0.0431(12) 0.0241(10) 0.0312(11) 0.0066(8) -0.0106(9) 0.0027(9) C23 0.0292(10) 0.0254(10) 0.0337(10) 0.0004(8) -0.0073(8) 0.0071(8) C24 0.0230(9) 0.0205(8) 0.0212(8) -0.0046(7) -0.0044(7) 0.0029(7) C25 0.0221(9) 0.0253(9) 0.0232(9) -0.0041(7) -0.0032(7) 0.0006(7) C26 0.0233(10) 0.0391(12) 0.0371(11) -0.0062(9) -0.0004(8) 0.0031(8) C27 0.0241(10) 0.0603(15) 0.0381(12) -0.0095(11) 0.0054(9) -0.0022(10) C28 0.0327(12) 0.0606(16) 0.0330(12) 0.0045(11) 0.0059(9) -0.0125(11) C29 0.0333(11) 0.0435(13) 0.0324(11) 0.0108(9) 0.0008(9) -0.0045(10) P10 0.0211(3) 0.0550(4) 0.0307(3) -0.0033(3) 0.0002(2) -0.0021(2) F10 0.0560(11) 0.0879(14) 0.0612(11) 0.0297(10) -0.0085(8) -0.0075(10) F11 0.0491(11) 0.156(2) 0.0716(13) 0.0544(14) 0.0022(9) -0.0260(13) F12 0.0343(9) 0.147(2) 0.0586(11) 0.0069(12) -0.0097(8) -0.0295(11) F13 0.0828(15) 0.0736(13) 0.0877(15) -0.0236(11) 0.0004(12) 0.0213(11) F14 0.114(2) 0.176(3) 0.0655(13) -0.0525(16) -0.0223(13) 0.088(2) F15 0.0464(9) 0.0919(14) 0.0689(11) 0.0191(10) -0.0295(8) -0.0254(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 Cu1 N1 2.0359(16) . ? Cu1 N2 2.0407(17) . ? Cu1 P1 2.1824(6) . ? Cu1 S1 2.3616(6) . ? P1 C8 1.8201(19) . ? P1 C14 1.8217(18) . ? P1 C3 1.8246(18) . ? S1 C2 1.7842(19) . ? S1 C1 1.812(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.395(3) . ? C2 C3 1.397(3) . ? C3 C4 1.396(3) . ? C4 C5 1.384(3) . ? C4 H4A 0.9500 . ? C5 C6 1.381(3) . ? C5 H5A 0.9500 . ? C6 C7 1.384(3) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C13 1.392(3) . ? C8 C9 1.394(3) . ? C9 C10 1.385(3) . ? C9 H9A 0.9500 . ? C10 C11 1.386(4) . ? C10 H10A 0.9500 . ? C11 C12 1.377(4) . ? C11 H11A 0.9500 . ? C12 C13 1.389(3) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.390(3) . ? C14 C19 1.391(3) . ? C15 C16 1.384(3) . ? C15 H15A 0.9500 . ? C16 C17 1.379(3) . ? C16 H16A 0.9500 . ? C17 C18 1.373(3) . ? C17 H17A 0.9500 . ? C18 C19 1.388(3) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? N1 C20 1.333(2) . ? N1 C24 1.350(2) . ? N2 C29 1.337(3) . ? N2 C25 1.348(3) . ? C20 C21 1.384(3) . ? C20 H20A 0.9500 . ? C21 C22 1.377(3) . ? C21 H21A 0.9500 . ? C22 C23 1.379(3) . ? C22 H22A 0.9500 . ? C23 C24 1.389(3) . ? C23 H23A 0.9500 . ? C24 C25 1.477(3) . ? C25 C26 1.393(3) . ? C26 C27 1.380(3) . ? C26 H26A 0.9500 . ? C27 C28 1.372(4) . ? C27 H27A 0.9500 . ? C28 C29 1.385(3) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? P10 F13 1.565(2) . ? P10 F15 1.5697(16) . ? P10 F10 1.5750(18) . ? P10 F14 1.577(2) . ? P10 F11 1.579(2) . ? P10 F12 1.5921(17) . ? 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 Cu1 N2 81.09(7) . . ? N1 Cu1 P1 128.53(5) . . ? N2 Cu1 P1 138.98(5) . . ? N1 Cu1 S1 108.80(5) . . ? N2 Cu1 S1 109.02(5) . . ? P1 Cu1 S1 89.09(2) . . ? C8 P1 C14 102.19(8) . . ? C8 P1 C3 103.57(8) . . ? C14 P1 C3 105.58(8) . . ? C8 P1 Cu1 113.96(6) . . ? C14 P1 Cu1 125.70(6) . . ? C3 P1 Cu1 103.66(6) . . ? C2 S1 C1 100.90(11) . . ? C2 S1 Cu1 100.12(6) . . ? C1 S1 Cu1 107.43(11) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 120.41(18) . . ? C7 C2 S1 118.90(15) . . ? C3 C2 S1 120.69(14) . . ? C4 C3 C2 118.56(16) . . ? C4 C3 P1 122.55(14) . . ? C2 C3 P1 118.89(14) . . ? C5 C4 C3 120.92(18) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C6 C5 C4 119.93(19) . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C5 C6 C7 120.34(18) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C6 C7 C2 119.82(19) . . ? C6 C7 H7A 120.1 . . ? C2 C7 H7A 120.1 . . ? C13 C8 C9 119.16(18) . . ? C13 C8 P1 122.99(14) . . ? C9 C8 P1 117.81(15) . . ? C10 C9 C8 120.2(2) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C9 C10 C11 120.1(2) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C12 C11 C10 120.1(2) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C13 120.2(2) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C12 C13 C8 120.3(2) . . ? C12 C13 H13A 119.9 . . ? C8 C13 H13A 119.9 . . ? C15 C14 C19 119.09(18) . . ? C15 C14 P1 122.10(14) . . ? C19 C14 P1 118.76(15) . . ? C16 C15 C14 120.26(19) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C17 C16 C15 120.0(2) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C18 C17 C16 120.5(2) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C17 C18 C19 119.9(2) . . ? C17 C18 H18A 120.1 . . ? C19 C18 H18A 120.1 . . ? C18 C19 C14 120.3(2) . . ? C18 C19 H19A 119.8 . . ? C14 C19 H19A 119.8 . . ? C20 N1 C24 118.74(16) . . ? C20 N1 Cu1 127.60(13) . . ? C24 N1 Cu1 113.57(12) . . ? C29 N2 C25 118.37(19) . . ? C29 N2 Cu1 127.51(15) . . ? C25 N2 Cu1 113.25(13) . . ? N1 C20 C21 122.94(19) . . ? N1 C20 H20A 118.5 . . ? C21 C20 H20A 118.5 . . ? C22 C21 C20 117.99(19) . . ? C22 C21 H21A 121.0 . . ? C20 C21 H21A 121.0 . . ? C21 C22 C23 120.09(19) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C24 118.60(19) . . ? C22 C23 H23A 120.7 . . ? C24 C23 H23A 120.7 . . ? N1 C24 C23 121.59(18) . . ? N1 C24 C25 115.55(16) . . ? C23 C24 C25 122.85(18) . . ? N2 C25 C26 121.42(19) . . ? N2 C25 C24 115.51(17) . . ? C26 C25 C24 123.07(18) . . ? C27 C26 C25 119.1(2) . . ? C27 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? C28 C27 C26 119.6(2) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C27 C28 C29 118.2(2) . . ? C27 C28 H28A 120.9 . . ? C29 C28 H28A 120.9 . . ? N2 C29 C28 123.2(2) . . ? N2 C29 H29A 118.4 . . ? C28 C29 H29A 118.4 . . ? F13 P10 F15 90.66(13) . . ? F13 P10 F10 89.35(13) . . ? F15 P10 F10 90.56(10) . . ? F13 P10 F14 177.73(14) . . ? F15 P10 F14 91.61(14) . . ? F10 P10 F14 90.68(15) . . ? F13 P10 F11 90.41(15) . . ? F15 P10 F11 89.06(11) . . ? F10 P10 F11 179.55(12) . . ? F14 P10 F11 89.58(17) . . ? F13 P10 F12 90.57(13) . . ? F15 P10 F12 178.22(13) . . ? F10 P10 F12 88.15(11) . . ? F14 P10 F12 87.16(14) . . ? F11 P10 F12 92.23(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.604 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.057 # Attachment 'Cu(PS)(phen).CIF' data_esc58 _database_code_depnum_ccdc_archive 'CCDC 796689' #TrackingRef 'Cu(PS)(phen).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H25 Cu N2 P S, F6 P, C H2 Cl2' _chemical_formula_sum 'C32 H27 Cl2 Cu F6 N2 P2 S' _chemical_formula_weight 782.00 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' 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' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9997(16) _cell_length_b 11.507(2) _cell_length_c 16.728(4) _cell_angle_alpha 78.417(16) _cell_angle_beta 86.517(16) _cell_angle_gamma 78.320(15) _cell_volume 1661.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4042 _cell_measurement_theta_min 5.97 _cell_measurement_theta_max 65.52 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 1.038 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8856 _exptl_absorpt_correction_T_max 0.9597 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24092 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6500 _reflns_number_gt 5690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0267P)^2^+1.3463P] 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 6500 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 Cu1 Cu 0.83549(3) 0.90775(2) 0.338741(16) 0.02129(8) Uani 1 1 d . . . P1 P 0.89184(6) 0.95100(5) 0.20917(3) 0.01824(12) Uani 1 1 d . . . S1 S 0.69480(6) 0.76829(5) 0.31480(3) 0.02393(12) Uani 1 1 d . . . C1 C 0.7756(4) 0.6205(2) 0.37265(16) 0.0386(6) Uani 1 1 d . . . H1A H 0.7274 0.5593 0.3572 0.058 Uiso 1 1 calc R . . H1B H 0.7581 0.6201 0.4311 0.058 Uiso 1 1 calc R . . H1C H 0.8849 0.6021 0.3610 0.058 Uiso 1 1 calc R . . C2 C 0.7565(2) 0.75130(19) 0.21431(13) 0.0207(4) Uani 1 1 d . . . C3 C 0.8439(2) 0.82854(19) 0.16739(13) 0.0202(4) Uani 1 1 d . . . C4 C 0.8910(3) 0.8090(2) 0.08946(14) 0.0260(5) Uani 1 1 d . . . H4A H 0.9532 0.8589 0.0572 0.031 Uiso 1 1 calc R . . C5 C 0.8485(3) 0.7184(2) 0.05852(15) 0.0301(5) Uani 1 1 d . . . H5A H 0.8814 0.7065 0.0052 0.036 Uiso 1 1 calc R . . C6 C 0.7582(3) 0.6446(2) 0.10483(15) 0.0305(5) Uani 1 1 d . . . H6A H 0.7273 0.5835 0.0828 0.037 Uiso 1 1 calc R . . C7 C 0.7133(3) 0.6599(2) 0.18295(15) 0.0263(5) Uani 1 1 d . . . H7A H 0.6532 0.6084 0.2153 0.032 Uiso 1 1 calc R . . C8 C 1.0871(2) 0.95096(19) 0.17461(13) 0.0201(4) Uani 1 1 d . . . C9 C 1.1373(3) 1.0543(2) 0.13418(14) 0.0272(5) Uani 1 1 d . . . H9A H 1.0663 1.1273 0.1174 0.033 Uiso 1 1 calc R . . C10 C 1.2913(3) 1.0506(2) 0.11834(16) 0.0358(6) Uani 1 1 d . . . H10A H 1.3254 1.1215 0.0910 0.043 Uiso 1 1 calc R . . C11 C 1.3947(3) 0.9452(3) 0.14189(17) 0.0375(6) Uani 1 1 d . . . H11A H 1.4998 0.9431 0.1306 0.045 Uiso 1 1 calc R . . C12 C 1.3452(3) 0.8423(2) 0.18215(16) 0.0343(6) Uani 1 1 d . . . H12A H 1.4167 0.7695 0.1987 0.041 Uiso 1 1 calc R . . C13 C 1.1933(3) 0.8446(2) 0.19837(15) 0.0276(5) Uani 1 1 d . . . H13A H 1.1604 0.7733 0.2259 0.033 Uiso 1 1 calc R . . C14 C 0.7790(2) 1.08946(19) 0.15236(13) 0.0215(4) Uani 1 1 d . . . C15 C 0.7199(3) 1.1798(2) 0.19549(16) 0.0307(5) Uani 1 1 d . . . H15A H 0.7422 1.1684 0.2516 0.037 Uiso 1 1 calc R . . C16 C 0.6285(3) 1.2867(2) 0.15805(18) 0.0410(7) Uani 1 1 d . . . H16A H 0.5882 1.3477 0.1885 0.049 Uiso 1 1 calc R . . C17 C 0.5963(3) 1.3040(2) 0.07697(19) 0.0434(7) Uani 1 1 d . . . H17A H 0.5330 1.3768 0.0513 0.052 Uiso 1 1 calc R . . C18 C 0.6556(4) 1.2162(3) 0.03288(18) 0.0461(7) Uani 1 1 d . . . H18A H 0.6343 1.2289 -0.0235 0.055 Uiso 1 1 calc R . . C19 C 0.7462(3) 1.1090(2) 0.07000(15) 0.0344(6) Uani 1 1 d . . . H19A H 0.7862 1.0486 0.0390 0.041 Uiso 1 1 calc R . . N1 N 0.7244(2) 1.00865(16) 0.42006(11) 0.0199(4) Uani 1 1 d . . . N2 N 0.9672(2) 0.82631(16) 0.43658(11) 0.0211(4) Uani 1 1 d . . . C20 C 0.6052(3) 1.0987(2) 0.41192(15) 0.0250(5) Uani 1 1 d . . . H20A H 0.5602 1.1260 0.3599 0.030 Uiso 1 1 calc R . . C21 C 0.5424(3) 1.1553(2) 0.47575(16) 0.0295(5) Uani 1 1 d . . . H21A H 0.4575 1.2203 0.4671 0.035 Uiso 1 1 calc R . . C22 C 0.6053(3) 1.1158(2) 0.55111(16) 0.0302(5) Uani 1 1 d . . . H22A H 0.5655 1.1542 0.5952 0.036 Uiso 1 1 calc R . . C23 C 0.7287(3) 1.0184(2) 0.56312(14) 0.0242(5) Uani 1 1 d . . . C24 C 0.7857(2) 0.96860(19) 0.49519(13) 0.0195(4) Uani 1 1 d . . . C25 C 0.9142(2) 0.87000(19) 0.50445(13) 0.0194(4) Uani 1 1 d . . . C26 C 0.9791(3) 0.8230(2) 0.58125(14) 0.0246(5) Uani 1 1 d . . . C27 C 1.1051(3) 0.7277(2) 0.58626(15) 0.0307(5) Uani 1 1 d . . . H27A H 1.1520 0.6929 0.6372 0.037 Uiso 1 1 calc R . . C28 C 1.1596(3) 0.6856(2) 0.51789(16) 0.0313(5) Uani 1 1 d . . . H28A H 1.2459 0.6220 0.5203 0.038 Uiso 1 1 calc R . . C29 C 1.0874(3) 0.7369(2) 0.44408(15) 0.0271(5) Uani 1 1 d . . . H29A H 1.1263 0.7062 0.3968 0.033 Uiso 1 1 calc R . . C30 C 0.7973(3) 0.9680(2) 0.64091(14) 0.0314(5) Uani 1 1 d . . . H30A H 0.7582 1.0013 0.6872 0.038 Uiso 1 1 calc R . . C31 C 0.9155(3) 0.8746(2) 0.64945(14) 0.0316(5) Uani 1 1 d . . . H31A H 0.9576 0.8423 0.7018 0.038 Uiso 1 1 calc R . . P10 P 1.37314(7) 0.48077(6) 0.33798(4) 0.02795(14) Uani 1 1 d . . . F10 F 1.4002(2) 0.60769(14) 0.35245(11) 0.0460(4) Uani 1 1 d . . . F11 F 1.34572(19) 0.35405(13) 0.32286(10) 0.0398(4) Uani 1 1 d . . . F12 F 1.54927(19) 0.42476(16) 0.34941(12) 0.0506(4) Uani 1 1 d . . . F13 F 1.19656(17) 0.53727(15) 0.32445(11) 0.0438(4) Uani 1 1 d . . . F14 F 1.4030(2) 0.52168(15) 0.24251(10) 0.0450(4) Uani 1 1 d . . . F15 F 1.3422(2) 0.44032(16) 0.43257(10) 0.0541(5) Uani 1 1 d . . . C100 C 0.8749(5) 1.5458(4) -0.1648(2) 0.0677(11) Uani 1 1 d . . . H10B H 0.7913 1.5975 -0.1989 0.081 Uiso 1 1 calc R . . H10C H 0.9205 1.4781 -0.1923 0.081 Uiso 1 1 calc R . . Cl1 Cl 1.01347(11) 1.63152(7) -0.15734(5) 0.0568(2) Uani 1 1 d . . . Cl2 Cl 0.80063(10) 1.48773(9) -0.06966(6) 0.0630(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02391(15) 0.02451(14) 0.01404(13) -0.00416(10) 0.00142(10) -0.00151(10) P1 0.0203(3) 0.0187(3) 0.0148(3) -0.00301(19) 0.0017(2) -0.0024(2) S1 0.0239(3) 0.0268(3) 0.0211(3) -0.0050(2) 0.0067(2) -0.0067(2) C1 0.0553(18) 0.0303(13) 0.0283(13) 0.0038(10) -0.0034(12) -0.0127(12) C2 0.0197(11) 0.0195(10) 0.0205(11) -0.0041(8) 0.0000(8) 0.0017(8) C3 0.0206(11) 0.0197(10) 0.0184(10) -0.0040(8) -0.0015(8) 0.0009(8) C4 0.0319(13) 0.0241(11) 0.0196(11) -0.0033(9) 0.0016(9) -0.0018(9) C5 0.0412(14) 0.0268(12) 0.0211(11) -0.0088(9) -0.0012(10) 0.0006(10) C6 0.0363(14) 0.0247(12) 0.0324(13) -0.0122(10) -0.0062(10) -0.0019(10) C7 0.0259(12) 0.0226(11) 0.0301(13) -0.0055(9) -0.0008(9) -0.0033(9) C8 0.0202(11) 0.0238(11) 0.0156(10) -0.0041(8) 0.0007(8) -0.0031(8) C9 0.0273(12) 0.0260(12) 0.0262(12) -0.0005(9) -0.0014(9) -0.0045(9) C10 0.0309(14) 0.0394(14) 0.0352(14) 0.0050(11) -0.0002(11) -0.0147(11) C11 0.0199(12) 0.0515(16) 0.0385(15) -0.0030(12) -0.0010(10) -0.0062(11) C12 0.0259(13) 0.0371(14) 0.0346(14) -0.0033(11) -0.0030(10) 0.0037(10) C13 0.0270(12) 0.0261(11) 0.0267(12) -0.0015(9) 0.0012(9) -0.0026(9) C14 0.0203(11) 0.0199(10) 0.0218(11) -0.0013(8) 0.0019(8) -0.0014(8) C15 0.0345(14) 0.0257(12) 0.0280(12) -0.0041(10) 0.0065(10) -0.0001(10) C16 0.0442(16) 0.0272(13) 0.0443(16) -0.0070(11) 0.0112(13) 0.0061(11) C17 0.0395(16) 0.0304(14) 0.0481(17) 0.0068(12) -0.0022(13) 0.0075(12) C18 0.0593(19) 0.0387(15) 0.0327(15) 0.0022(12) -0.0149(13) 0.0036(14) C19 0.0449(16) 0.0288(13) 0.0256(13) -0.0037(10) -0.0059(11) 0.0016(11) N1 0.0196(9) 0.0196(9) 0.0196(9) -0.0038(7) 0.0021(7) -0.0021(7) N2 0.0211(9) 0.0212(9) 0.0195(9) -0.0039(7) 0.0014(7) -0.0008(7) C20 0.0220(11) 0.0229(11) 0.0272(12) -0.0008(9) 0.0028(9) -0.0024(9) C21 0.0231(12) 0.0243(11) 0.0386(14) -0.0064(10) 0.0084(10) -0.0010(9) C22 0.0297(13) 0.0291(12) 0.0337(13) -0.0135(10) 0.0133(10) -0.0068(10) C23 0.0256(12) 0.0264(11) 0.0234(11) -0.0088(9) 0.0057(9) -0.0091(9) C24 0.0213(11) 0.0197(10) 0.0186(10) -0.0038(8) 0.0020(8) -0.0070(8) C25 0.0212(11) 0.0194(10) 0.0179(10) -0.0026(8) -0.0005(8) -0.0058(8) C26 0.0269(12) 0.0263(11) 0.0211(11) -0.0020(9) -0.0019(9) -0.0087(9) C27 0.0364(14) 0.0279(12) 0.0254(12) 0.0028(9) -0.0092(10) -0.0059(10) C28 0.0277(13) 0.0243(12) 0.0377(14) -0.0003(10) -0.0037(10) 0.0000(10) C29 0.0261(12) 0.0252(11) 0.0281(12) -0.0057(9) 0.0005(9) 0.0000(9) C30 0.0402(15) 0.0392(14) 0.0193(12) -0.0117(10) 0.0055(10) -0.0137(11) C31 0.0416(15) 0.0369(13) 0.0174(11) -0.0038(10) -0.0041(10) -0.0106(11) P10 0.0286(3) 0.0257(3) 0.0284(3) -0.0060(2) 0.0004(2) -0.0021(2) F10 0.0483(10) 0.0318(8) 0.0619(11) -0.0169(8) -0.0051(8) -0.0078(7) F11 0.0475(10) 0.0291(8) 0.0446(9) -0.0099(7) -0.0026(7) -0.0082(7) F12 0.0309(9) 0.0480(10) 0.0715(12) -0.0173(9) -0.0123(8) 0.0044(7) F13 0.0284(8) 0.0479(9) 0.0560(10) -0.0206(8) -0.0005(7) 0.0010(7) F14 0.0543(10) 0.0427(9) 0.0331(9) -0.0021(7) 0.0086(7) -0.0060(8) F15 0.0808(14) 0.0516(10) 0.0273(9) -0.0066(7) 0.0048(8) -0.0092(9) C100 0.081(3) 0.089(3) 0.0424(19) -0.0149(18) -0.0155(18) -0.032(2) Cl1 0.0753(6) 0.0334(4) 0.0604(5) -0.0055(3) -0.0198(4) -0.0059(4) Cl2 0.0536(5) 0.0802(6) 0.0532(5) -0.0205(4) 0.0048(4) -0.0026(4) _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 N2 2.0326(19) . ? Cu1 N1 2.0487(18) . ? Cu1 P1 2.1768(8) . ? Cu1 S1 2.3412(7) . ? P1 C8 1.816(2) . ? P1 C14 1.824(2) . ? P1 C3 1.827(2) . ? S1 C2 1.774(2) . ? S1 C1 1.811(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.395(3) . ? C2 C3 1.397(3) . ? C3 C4 1.393(3) . ? C4 C5 1.380(3) . ? C4 H4A 0.9500 . ? C5 C6 1.386(4) . ? C5 H5A 0.9500 . ? C6 C7 1.379(3) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.390(3) . ? C8 C13 1.395(3) . ? C9 C10 1.389(4) . ? C9 H9A 0.9500 . ? C10 C11 1.374(4) . ? C10 H10A 0.9500 . ? C11 C12 1.383(4) . ? C11 H11A 0.9500 . ? C12 C13 1.373(4) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.384(3) . ? C14 C19 1.391(3) . ? C15 C16 1.388(4) . ? C15 H15A 0.9500 . ? C16 C17 1.371(4) . ? C16 H16A 0.9500 . ? C17 C18 1.373(4) . ? C17 H17A 0.9500 . ? C18 C19 1.385(4) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? N1 C20 1.324(3) . ? N1 C24 1.358(3) . ? N2 C29 1.326(3) . ? N2 C25 1.355(3) . ? C20 C21 1.394(3) . ? C20 H20A 0.9500 . ? C21 C22 1.367(4) . ? C21 H21A 0.9500 . ? C22 C23 1.400(3) . ? C22 H22A 0.9500 . ? C23 C24 1.398(3) . ? C23 C30 1.435(3) . ? C24 C25 1.438(3) . ? C25 C26 1.403(3) . ? C26 C27 1.403(3) . ? C26 C31 1.427(3) . ? C27 C28 1.357(4) . ? C27 H27A 0.9500 . ? C28 C29 1.395(3) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C31 1.342(4) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? P10 F15 1.5816(17) . ? P10 F12 1.5932(17) . ? P10 F14 1.5943(17) . ? P10 F10 1.5951(16) . ? P10 F11 1.5976(16) . ? P10 F13 1.6018(17) . ? C100 Cl2 1.746(4) . ? C100 Cl1 1.763(4) . ? C100 H10B 0.9900 . ? C100 H10C 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N1 82.47(7) . . ? N2 Cu1 P1 131.37(6) . . ? N1 Cu1 P1 133.24(5) . . ? N2 Cu1 S1 107.15(6) . . ? N1 Cu1 S1 111.10(6) . . ? P1 Cu1 S1 90.59(3) . . ? C8 P1 C14 106.12(10) . . ? C8 P1 C3 103.08(10) . . ? C14 P1 C3 105.28(10) . . ? C8 P1 Cu1 120.62(7) . . ? C14 P1 Cu1 115.59(8) . . ? C3 P1 Cu1 104.34(7) . . ? C2 S1 C1 101.05(12) . . ? C2 S1 Cu1 101.47(8) . . ? C1 S1 Cu1 108.62(10) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 120.9(2) . . ? C7 C2 S1 118.11(17) . . ? C3 C2 S1 120.97(17) . . ? C4 C3 C2 118.1(2) . . ? C4 C3 P1 122.27(18) . . ? C2 C3 P1 119.59(16) . . ? C5 C4 C3 120.9(2) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 120.4(2) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C7 C6 C5 119.9(2) . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C6 C7 C2 119.7(2) . . ? C6 C7 H7A 120.1 . . ? C2 C7 H7A 120.1 . . ? C9 C8 C13 119.1(2) . . ? C9 C8 P1 123.14(17) . . ? C13 C8 P1 117.39(17) . . ? C10 C9 C8 119.9(2) . . ? C10 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? C11 C10 C9 120.5(2) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 119.7(2) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? C13 C12 C11 120.4(2) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C12 C13 C8 120.4(2) . . ? C12 C13 H13A 119.8 . . ? C8 C13 H13A 119.8 . . ? C15 C14 C19 118.3(2) . . ? C15 C14 P1 116.95(18) . . ? C19 C14 P1 124.72(18) . . ? C14 C15 C16 121.0(2) . . ? C14 C15 H15A 119.5 . . ? C16 C15 H15A 119.5 . . ? C17 C16 C15 119.8(3) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C16 C17 C18 120.0(2) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C18 C19 120.5(3) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C18 C19 C14 120.4(2) . . ? C18 C19 H19A 119.8 . . ? C14 C19 H19A 119.8 . . ? C20 N1 C24 117.73(19) . . ? C20 N1 Cu1 131.54(16) . . ? C24 N1 Cu1 110.67(14) . . ? C29 N2 C25 117.6(2) . . ? C29 N2 Cu1 130.60(16) . . ? C25 N2 Cu1 111.72(14) . . ? N1 C20 C21 123.4(2) . . ? N1 C20 H20A 118.3 . . ? C21 C20 H20A 118.3 . . ? C22 C21 C20 118.8(2) . . ? C22 C21 H21A 120.6 . . ? C20 C21 H21A 120.6 . . ? C21 C22 C23 119.8(2) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C24 C23 C22 117.4(2) . . ? C24 C23 C30 119.3(2) . . ? C22 C23 C30 123.4(2) . . ? N1 C24 C23 122.9(2) . . ? N1 C24 C25 117.88(19) . . ? C23 C24 C25 119.2(2) . . ? N2 C25 C26 122.8(2) . . ? N2 C25 C24 117.07(19) . . ? C26 C25 C24 120.1(2) . . ? C27 C26 C25 117.5(2) . . ? C27 C26 C31 123.6(2) . . ? C25 C26 C31 118.9(2) . . ? C28 C27 C26 119.6(2) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C27 C28 C29 119.2(2) . . ? C27 C28 H28A 120.4 . . ? C29 C28 H28A 120.4 . . ? N2 C29 C28 123.3(2) . . ? N2 C29 H29A 118.3 . . ? C28 C29 H29A 118.3 . . ? C31 C30 C23 121.2(2) . . ? C31 C30 H30A 119.4 . . ? C23 C30 H30A 119.4 . . ? C30 C31 C26 121.2(2) . . ? C30 C31 H31A 119.4 . . ? C26 C31 H31A 119.4 . . ? F15 P10 F12 90.59(11) . . ? F15 P10 F14 179.55(11) . . ? F12 P10 F14 89.84(10) . . ? F15 P10 F10 90.21(10) . . ? F12 P10 F10 90.47(10) . . ? F14 P10 F10 89.92(10) . . ? F15 P10 F11 90.15(10) . . ? F12 P10 F11 89.68(9) . . ? F14 P10 F11 89.73(9) . . ? F10 P10 F11 179.61(10) . . ? F15 P10 F13 90.59(11) . . ? F12 P10 F13 178.79(11) . . ? F14 P10 F13 88.98(10) . . ? F10 P10 F13 89.82(9) . . ? F11 P10 F13 90.03(9) . . ? Cl2 C100 Cl1 112.59(19) . . ? Cl2 C100 H10B 109.1 . . ? Cl1 C100 H10B 109.1 . . ? Cl2 C100 H10C 109.1 . . ? Cl1 C100 H10C 109.1 . . ? H10B C100 H10C 107.8 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.792 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.055 # Attachment 'Cu(PS)2.CIF' data_esc69 _database_code_depnum_ccdc_archive 'CCDC 796690' #TrackingRef 'Cu(PS)2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H34 Cu P2 S2, F6 P' _chemical_formula_sum 'C38 H34 Cu F6 P3 S2' _chemical_formula_weight 825.25 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' 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' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.137(2) _cell_length_b 13.453(2) _cell_length_c 13.9427(19) _cell_angle_alpha 97.305(12) _cell_angle_beta 110.279(12) _cell_angle_gamma 114.695(11) _cell_volume 1838.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5063 _cell_measurement_theta_min 5.56 _cell_measurement_theta_max 70.24 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7156 _exptl_absorpt_correction_T_max 0.8070 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65210 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 31.00 _reflns_number_total 11608 _reflns_number_gt 11278 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0338P)^2^+0.8179P] 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 11608 _refine_ls_number_parameters 508 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.076 _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 0.587840(13) 0.186567(11) 0.248127(10) 0.01728(4) Uani 1 1 d . . . S1 S 0.37753(3) 0.03473(2) 0.12406(2) 0.02075(5) Uani 1 1 d . . . S2 S 0.65894(3) 0.31421(2) 0.15738(2) 0.02094(5) Uani 1 1 d . . . P1 P 0.65948(3) 0.06301(2) 0.28754(2) 0.01535(5) Uani 1 1 d . . . P2 P 0.61188(3) 0.32552(2) 0.37246(2) 0.01760(5) Uani 1 1 d . . . C1 C 0.24388(13) 0.03551(12) 0.15325(12) 0.0313(3) Uani 1 1 d . . . H1A H 0.1595 -0.0375 0.1092 0.047 Uiso 1 1 calc R . . H1B H 0.2315 0.0998 0.1366 0.047 Uiso 1 1 calc R . . H1C H 0.2681 0.0446 0.2298 0.047 Uiso 1 1 calc R . . C2 C 0.38281(11) -0.08567(9) 0.16164(9) 0.01970(18) Uani 1 1 d . . . C3 C 0.50371(10) -0.07513(9) 0.23417(8) 0.01777(17) Uani 1 1 d . . . C4 C 0.50006(12) -0.17226(10) 0.26224(10) 0.0240(2) Uani 1 1 d . . . H4A H 0.5806 -0.1659 0.3134 0.029 Uiso 1 1 calc R . . C5 C 0.38131(15) -0.27765(11) 0.21699(12) 0.0318(3) Uani 1 1 d . . . H5A H 0.3810 -0.3428 0.2366 0.038 Uiso 1 1 calc R . . C6 C 0.26338(14) -0.28762(11) 0.14327(13) 0.0345(3) Uani 1 1 d . . . H6A H 0.1821 -0.3600 0.1115 0.041 Uiso 1 1 calc R . . C7 C 0.26333(12) -0.19248(11) 0.11558(11) 0.0288(2) Uani 1 1 d . . . H7A H 0.1819 -0.1997 0.0651 0.035 Uiso 1 1 calc R . . C8 C 0.76211(11) 0.04280(10) 0.22699(9) 0.02011(19) Uani 1 1 d . . . C9 C 0.77179(15) -0.05674(12) 0.20970(13) 0.0334(3) Uani 1 1 d . . . H9A H 0.7239 -0.1188 0.2312 0.040 Uiso 1 1 calc R . . C10 C 0.85113(17) -0.06592(16) 0.16127(14) 0.0437(4) Uani 1 1 d . . . H10A H 0.8568 -0.1344 0.1492 0.052 Uiso 1 1 calc R . . C11 C 0.92148(15) 0.02390(18) 0.13077(12) 0.0429(4) Uani 1 1 d . . . H11A H 0.9758 0.0173 0.0978 0.051 Uiso 1 1 calc R . . C12 C 0.91362(14) 0.12341(17) 0.14770(12) 0.0395(3) Uani 1 1 d . . . H12A H 0.9625 0.1853 0.1266 0.047 Uiso 1 1 calc R . . C13 C 0.83393(12) 0.13299(12) 0.19580(11) 0.0281(2) Uani 1 1 d . . . H13A H 0.8285 0.2016 0.2074 0.034 Uiso 1 1 calc R . . C14 C 0.74344(11) 0.07862(9) 0.42894(9) 0.01961(18) Uani 1 1 d . . . C15 C 0.87476(13) 0.09815(13) 0.47861(11) 0.0323(3) Uani 1 1 d . . . H15A H 0.9206 0.0933 0.4367 0.039 Uiso 1 1 calc R . . C16 C 0.93911(16) 0.12495(16) 0.59036(13) 0.0458(4) Uani 1 1 d . . . H16A H 1.0288 0.1380 0.6243 0.055 Uiso 1 1 calc R . . C17 C 0.87370(18) 0.13268(15) 0.65214(11) 0.0455(4) Uani 1 1 d . . . H17A H 0.9189 0.1524 0.7283 0.055 Uiso 1 1 calc R . . C18 C 0.74232(18) 0.11162(13) 0.60297(11) 0.0380(3) Uani 1 1 d . . . H18A H 0.6966 0.1157 0.6453 0.046 Uiso 1 1 calc R . . C19 C 0.67721(14) 0.08463(11) 0.49216(10) 0.0272(2) Uani 1 1 d . . . H19A H 0.5868 0.0701 0.4587 0.033 Uiso 1 1 calc R . . C20 C 0.52805(18) 0.26729(13) 0.02230(10) 0.0375(3) Uani 1 1 d . . . H20A H 0.4437 0.2542 0.0252 0.056 Uiso 1 1 calc R . . H20B H 0.5140 0.1953 -0.0200 0.056 Uiso 1 1 calc R . . H20C H 0.5553 0.3268 -0.0117 0.056 Uiso 1 1 calc R . . C21 C 0.65591(12) 0.43540(9) 0.22186(9) 0.02049(19) Uani 1 1 d . . . C22 C 0.64359(11) 0.44548(9) 0.31826(9) 0.01962(18) Uani 1 1 d . . . C23 C 0.65499(15) 0.54786(10) 0.37002(10) 0.0276(2) Uani 1 1 d . . . H23A H 0.6503 0.5572 0.4369 0.033 Uiso 1 1 calc R . . C24 C 0.67307(18) 0.63565(11) 0.32457(12) 0.0362(3) Uani 1 1 d . . . H24A H 0.6799 0.7046 0.3600 0.043 Uiso 1 1 calc R . . C25 C 0.68123(19) 0.62309(12) 0.22760(12) 0.0386(3) Uani 1 1 d . . . H25A H 0.6909 0.6826 0.1956 0.046 Uiso 1 1 calc R . . C26 C 0.67537(16) 0.52455(11) 0.17708(11) 0.0306(3) Uani 1 1 d . . . H26A H 0.6846 0.5176 0.1120 0.037 Uiso 1 1 calc R . . C27 C 0.46278(11) 0.29505(9) 0.39259(9) 0.01972(18) Uani 1 1 d . . . C28 C 0.42790(13) 0.21938(10) 0.45080(10) 0.0241(2) Uani 1 1 d . . . H28A H 0.4904 0.1975 0.4902 0.029 Uiso 1 1 calc R . . C29 C 0.30255(14) 0.17627(11) 0.45116(10) 0.0282(2) Uani 1 1 d . . . H29A H 0.2789 0.1242 0.4900 0.034 Uiso 1 1 calc R . . C30 C 0.21174(14) 0.20897(12) 0.39491(11) 0.0312(3) Uani 1 1 d . . . H30A H 0.1255 0.1789 0.3946 0.037 Uiso 1 1 calc R . . C31 C 0.24681(14) 0.28553(12) 0.33911(11) 0.0312(3) Uani 1 1 d . . . H31A H 0.1851 0.3091 0.3018 0.037 Uiso 1 1 calc R . . C32 C 0.37125(13) 0.32805(11) 0.33727(10) 0.0251(2) Uani 1 1 d . . . H32A H 0.3941 0.3799 0.2981 0.030 Uiso 1 1 calc R . . C33 C 0.75153(12) 0.38416(9) 0.50602(9) 0.02080(19) Uani 1 1 d . . . C34 C 0.86540(13) 0.37631(11) 0.51532(10) 0.0272(2) Uani 1 1 d . . . H34A H 0.8681 0.3426 0.4526 0.033 Uiso 1 1 calc R . . C35 C 0.97487(14) 0.41735(13) 0.61538(12) 0.0359(3) Uani 1 1 d . . . H35A H 1.0522 0.4117 0.6211 0.043 Uiso 1 1 calc R . . C36 C 0.97119(15) 0.46671(14) 0.70707(12) 0.0388(3) Uani 1 1 d . . . H36A H 1.0457 0.4941 0.7758 0.047 Uiso 1 1 calc R . . C37 C 0.85939(16) 0.47609(13) 0.69858(11) 0.0366(3) Uani 1 1 d . . . H37A H 0.8578 0.5109 0.7614 0.044 Uiso 1 1 calc R . . C38 C 0.74917(14) 0.43486(12) 0.59848(10) 0.0287(2) Uani 1 1 d . . . H38A H 0.6723 0.4412 0.5931 0.034 Uiso 1 1 calc R . . P10 P 0.17458(4) 0.35070(3) 0.02969(3) 0.02669(7) Uani 1 1 d . . . F10 F 0.1619(3) 0.24220(16) 0.07122(18) 0.0510(5) Uani 0.785(6) 1 d P A 1 F11 F 0.2862(3) 0.3486(2) -0.0004(2) 0.0511(6) Uani 0.785(6) 1 d PU A 1 F12 F 0.0579(3) 0.3500(2) 0.0598(2) 0.0509(6) Uani 0.785(6) 1 d P A 1 F13 F 0.28126(18) 0.43425(16) 0.15040(18) 0.0484(5) Uani 0.785(6) 1 d P A 1 F14 F 0.1892(3) 0.4597(2) -0.0068(2) 0.0618(8) Uani 0.785(6) 1 d PU A 1 F15 F 0.0628(2) 0.2650(3) -0.08684(15) 0.0752(9) Uani 0.785(6) 1 d PU A 1 F10' F 0.0873(14) 0.2225(7) 0.0137(12) 0.081(4) Uani 0.215(6) 1 d P A 2 F11' F 0.2992(14) 0.3367(16) 0.0341(16) 0.150(7) Uani 0.215(6) 1 d PU A 2 F12' F 0.0546(13) 0.3661(15) 0.0270(15) 0.115(7) Uani 0.215(6) 1 d P A 2 F13' F 0.231(2) 0.3887(14) 0.1466(8) 0.119(5) Uani 0.215(6) 1 d P A 2 F14' F 0.2517(15) 0.4783(6) 0.0286(10) 0.098(4) Uani 0.215(6) 1 d PU A 2 F15' F 0.1206(16) 0.3091(8) -0.0950(7) 0.126(5) Uani 0.215(6) 1 d PU A 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 Cu1 0.02111(6) 0.01518(6) 0.01599(6) 0.00475(4) 0.00834(5) 0.00936(5) S1 0.01858(11) 0.02108(12) 0.01902(11) 0.00523(9) 0.00526(9) 0.00965(9) S2 0.02715(13) 0.02134(12) 0.01893(11) 0.00819(9) 0.01357(10) 0.01273(10) P1 0.01588(11) 0.01514(11) 0.01458(11) 0.00434(8) 0.00678(9) 0.00740(9) P2 0.02457(13) 0.01605(11) 0.01450(11) 0.00602(9) 0.01012(10) 0.01053(10) C1 0.0240(5) 0.0346(6) 0.0360(7) 0.0071(5) 0.0120(5) 0.0172(5) C2 0.0185(4) 0.0171(4) 0.0192(4) 0.0034(3) 0.0073(4) 0.0068(4) C3 0.0183(4) 0.0154(4) 0.0178(4) 0.0040(3) 0.0083(4) 0.0070(3) C4 0.0261(5) 0.0191(5) 0.0258(5) 0.0084(4) 0.0108(4) 0.0105(4) C5 0.0354(6) 0.0173(5) 0.0373(7) 0.0100(5) 0.0156(5) 0.0085(5) C6 0.0280(6) 0.0190(5) 0.0403(7) 0.0047(5) 0.0119(5) 0.0022(4) C7 0.0202(5) 0.0217(5) 0.0303(6) 0.0028(4) 0.0058(4) 0.0044(4) C8 0.0179(4) 0.0253(5) 0.0173(4) 0.0048(4) 0.0079(4) 0.0113(4) C9 0.0325(6) 0.0313(6) 0.0420(7) 0.0061(5) 0.0203(6) 0.0191(5) C10 0.0372(7) 0.0540(9) 0.0432(8) -0.0005(7) 0.0177(6) 0.0299(7) C11 0.0274(6) 0.0811(12) 0.0242(6) 0.0077(7) 0.0127(5) 0.0318(7) C12 0.0251(6) 0.0714(11) 0.0304(6) 0.0239(7) 0.0182(5) 0.0240(7) C13 0.0229(5) 0.0394(7) 0.0276(6) 0.0163(5) 0.0148(5) 0.0158(5) C14 0.0208(4) 0.0179(4) 0.0159(4) 0.0053(3) 0.0063(4) 0.0075(4) C15 0.0201(5) 0.0415(7) 0.0252(6) 0.0143(5) 0.0060(4) 0.0091(5) C16 0.0261(6) 0.0550(9) 0.0289(7) 0.0177(7) -0.0008(5) 0.0063(6) C17 0.0498(9) 0.0403(8) 0.0170(6) 0.0079(5) 0.0031(6) 0.0075(7) C18 0.0575(9) 0.0360(7) 0.0212(6) 0.0095(5) 0.0201(6) 0.0218(7) C19 0.0366(6) 0.0303(6) 0.0211(5) 0.0100(4) 0.0152(5) 0.0196(5) C20 0.0547(9) 0.0373(7) 0.0160(5) 0.0054(5) 0.0086(5) 0.0256(7) C21 0.0263(5) 0.0173(4) 0.0179(4) 0.0067(4) 0.0109(4) 0.0096(4) C22 0.0262(5) 0.0159(4) 0.0166(4) 0.0062(3) 0.0099(4) 0.0098(4) C23 0.0433(7) 0.0199(5) 0.0229(5) 0.0074(4) 0.0172(5) 0.0163(5) C24 0.0614(9) 0.0211(5) 0.0337(7) 0.0118(5) 0.0250(7) 0.0228(6) C25 0.0665(10) 0.0239(6) 0.0348(7) 0.0177(5) 0.0279(7) 0.0237(6) C26 0.0490(8) 0.0238(5) 0.0258(6) 0.0141(4) 0.0224(6) 0.0174(5) C27 0.0252(5) 0.0185(4) 0.0163(4) 0.0051(3) 0.0104(4) 0.0108(4) C28 0.0305(5) 0.0246(5) 0.0233(5) 0.0111(4) 0.0156(4) 0.0151(4) C29 0.0324(6) 0.0281(6) 0.0257(5) 0.0100(4) 0.0178(5) 0.0120(5) C30 0.0268(6) 0.0341(6) 0.0291(6) 0.0063(5) 0.0142(5) 0.0116(5) C31 0.0280(6) 0.0354(6) 0.0300(6) 0.0097(5) 0.0104(5) 0.0177(5) C32 0.0278(5) 0.0254(5) 0.0225(5) 0.0094(4) 0.0098(4) 0.0140(4) C33 0.0254(5) 0.0180(4) 0.0167(4) 0.0064(3) 0.0091(4) 0.0088(4) C34 0.0243(5) 0.0258(5) 0.0254(5) 0.0058(4) 0.0103(4) 0.0086(4) C35 0.0231(6) 0.0368(7) 0.0338(7) 0.0083(5) 0.0070(5) 0.0084(5) C36 0.0300(6) 0.0382(7) 0.0243(6) 0.0070(5) 0.0027(5) 0.0051(5) C37 0.0399(7) 0.0376(7) 0.0177(5) 0.0032(5) 0.0099(5) 0.0109(6) C38 0.0341(6) 0.0308(6) 0.0186(5) 0.0048(4) 0.0117(5) 0.0148(5) P10 0.03120(15) 0.02842(15) 0.02305(14) 0.00845(11) 0.01500(12) 0.01453(13) F10 0.0778(13) 0.0335(7) 0.0589(11) 0.0264(7) 0.0436(10) 0.0280(8) F11 0.0633(13) 0.0604(10) 0.0822(14) 0.0474(11) 0.0597(13) 0.0458(10) F12 0.0392(12) 0.0502(9) 0.0542(11) -0.0055(8) 0.0283(10) 0.0147(7) F13 0.0432(8) 0.0392(8) 0.0357(8) -0.0015(6) -0.0029(6) 0.0177(6) F14 0.114(2) 0.0755(17) 0.0671(15) 0.0550(14) 0.0643(14) 0.0783(17) F15 0.0688(13) 0.0969(18) 0.0315(8) -0.0265(10) -0.0066(8) 0.0537(13) F10' 0.125(9) 0.043(3) 0.131(10) 0.049(5) 0.111(9) 0.039(5) F11' 0.062(5) 0.174(13) 0.163(14) -0.061(9) 0.013(7) 0.078(8) F12' 0.031(4) 0.132(11) 0.130(13) -0.027(9) -0.004(6) 0.047(6) F13' 0.213(16) 0.127(11) 0.027(4) 0.035(6) 0.043(7) 0.100(11) F14' 0.162(9) 0.018(2) 0.089(7) -0.006(3) 0.097(6) -0.004(4) F15' 0.174(9) 0.057(4) 0.031(3) -0.016(3) 0.035(5) -0.024(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 Cu1 P1 2.2203(4) . ? Cu1 P2 2.2258(5) . ? Cu1 S1 2.3161(7) . ? Cu1 S2 2.3163(4) . ? S1 C2 1.7836(12) . ? S1 C1 1.8077(13) . ? S2 C21 1.7799(12) . ? S2 C20 1.8042(15) . ? P1 C8 1.8143(11) . ? P1 C14 1.8146(11) . ? P1 C3 1.8218(11) . ? P2 C27 1.8119(12) . ? P2 C33 1.8123(12) . ? P2 C22 1.8210(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.3990(15) . ? C2 C7 1.3996(16) . ? C3 C4 1.3988(15) . ? C4 C5 1.3857(17) . ? C4 H4A 0.9500 . ? C5 C6 1.381(2) . ? C5 H5A 0.9500 . ? C6 C7 1.3832(19) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.3907(17) . ? C8 C13 1.3907(17) . ? C9 C10 1.3883(19) . ? C9 H9A 0.9500 . ? C10 C11 1.375(3) . ? C10 H10A 0.9500 . ? C11 C12 1.378(3) . ? C11 H11A 0.9500 . ? C12 C13 1.3906(18) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.3884(17) . ? C14 C19 1.3988(16) . ? C15 C16 1.395(2) . ? C15 H15A 0.9500 . ? C16 C17 1.379(3) . ? C16 H16A 0.9500 . ? C17 C18 1.382(3) . ? C17 H17A 0.9500 . ? C18 C19 1.3838(18) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.3927(16) . ? C21 C22 1.3990(15) . ? C22 C23 1.3986(15) . ? C23 C24 1.3836(17) . ? C23 H23A 0.9500 . ? C24 C25 1.384(2) . ? C24 H24A 0.9500 . ? C25 C26 1.3812(19) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C32 1.3898(16) . ? C27 C28 1.4008(15) . ? C28 C29 1.3857(17) . ? C28 H28A 0.9500 . ? C29 C30 1.385(2) . ? C29 H29A 0.9500 . ? C30 C31 1.384(2) . ? C30 H30A 0.9500 . ? C31 C32 1.3848(18) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.3926(17) . ? C33 C38 1.3950(16) . ? C34 C35 1.3866(19) . ? C34 H34A 0.9500 . ? C35 C36 1.388(2) . ? C35 H35A 0.9500 . ? C36 C37 1.381(2) . ? C36 H36A 0.9500 . ? C37 C38 1.3907(19) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? P10 F13' 1.453(9) . ? P10 F10' 1.536(7) . ? P10 F12' 1.544(13) . ? P10 F15' 1.557(8) . ? P10 F11 1.560(2) . ? P10 F14 1.573(2) . ? P10 F14' 1.580(8) . ? P10 F15 1.5805(18) . ? P10 F11' 1.583(11) . ? P10 F13 1.602(2) . ? P10 F10 1.6058(17) . ? P10 F12 1.607(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Cu1 P2 123.391(16) . . ? P1 Cu1 S1 90.231(19) . . ? P2 Cu1 S1 122.229(19) . . ? P1 Cu1 S2 125.606(15) . . ? P2 Cu1 S2 90.922(17) . . ? S1 Cu1 S2 106.312(18) . . ? C2 S1 C1 101.39(6) . . ? C2 S1 Cu1 101.84(4) . . ? C1 S1 Cu1 111.54(5) . . ? C21 S2 C20 101.82(6) . . ? C21 S2 Cu1 101.90(4) . . ? C20 S2 Cu1 110.62(6) . . ? C8 P1 C14 106.01(5) . . ? C8 P1 C3 106.28(5) . . ? C14 P1 C3 103.76(5) . . ? C8 P1 Cu1 118.02(4) . . ? C14 P1 Cu1 117.58(4) . . ? C3 P1 Cu1 103.66(4) . . ? C27 P2 C33 106.07(5) . . ? C27 P2 C22 105.70(5) . . ? C33 P2 C22 105.15(5) . . ? C27 P2 Cu1 115.53(4) . . ? C33 P2 Cu1 118.98(4) . . ? C22 P2 Cu1 104.15(4) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 120.13(11) . . ? C3 C2 S1 121.22(8) . . ? C7 C2 S1 118.64(9) . . ? C4 C3 C2 118.27(10) . . ? C4 C3 P1 122.47(9) . . ? C2 C3 P1 119.26(8) . . ? C5 C4 C3 121.34(12) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C6 C5 C4 119.78(12) . . ? C6 C5 H5A 120.1 . . ? C4 C5 H5A 120.1 . . ? C5 C6 C7 120.17(12) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C6 C7 C2 120.26(12) . . ? C6 C7 H7A 119.9 . . ? C2 C7 H7A 119.9 . . ? C9 C8 C13 118.93(11) . . ? C9 C8 P1 123.99(10) . . ? C13 C8 P1 117.08(9) . . ? C10 C9 C8 120.34(15) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C11 C10 C9 120.09(15) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.40(13) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C13 119.80(15) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C12 C13 C8 120.44(14) . . ? C12 C13 H13A 119.8 . . ? C8 C13 H13A 119.8 . . ? C15 C14 C19 119.14(11) . . ? C15 C14 P1 123.07(9) . . ? C19 C14 P1 117.34(9) . . ? C14 C15 C16 119.73(14) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C17 C16 C15 120.64(15) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C16 C17 C18 119.86(13) . . ? C16 C17 H17A 120.1 . . ? C18 C17 H17A 120.1 . . ? C17 C18 C19 120.06(14) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C18 C19 C14 120.55(13) . . ? C18 C19 H19A 119.7 . . ? C14 C19 H19A 119.7 . . ? S2 C20 H20A 109.5 . . ? S2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? S2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 120.43(10) . . ? C26 C21 S2 117.74(9) . . ? C22 C21 S2 121.69(8) . . ? C23 C22 C21 118.69(10) . . ? C23 C22 P2 121.75(9) . . ? C21 C22 P2 119.56(8) . . ? C24 C23 C22 120.54(11) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C23 C24 C25 120.08(12) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C26 C25 C24 120.39(12) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C25 C26 C21 119.80(12) . . ? C25 C26 H26A 120.1 . . ? C21 C26 H26A 120.1 . . ? C32 C27 C28 119.14(11) . . ? C32 C27 P2 121.76(9) . . ? C28 C27 P2 118.16(9) . . ? C29 C28 C27 120.26(11) . . ? C29 C28 H28A 119.9 . . ? C27 C28 H28A 119.9 . . ? C30 C29 C28 120.05(12) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C31 C30 C29 119.90(12) . . ? C31 C30 H30A 120.1 . . ? C29 C30 H30A 120.1 . . ? C30 C31 C32 120.47(12) . . ? C30 C31 H31A 119.8 . . ? C32 C31 H31A 119.8 . . ? C31 C32 C27 120.17(11) . . ? C31 C32 H32A 119.9 . . ? C27 C32 H32A 119.9 . . ? C34 C33 C38 119.26(11) . . ? C34 C33 P2 117.46(9) . . ? C38 C33 P2 123.27(10) . . ? C35 C34 C33 120.51(12) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C34 C35 C36 119.85(14) . . ? C34 C35 H35A 120.1 . . ? C36 C35 H35A 120.1 . . ? C37 C36 C35 120.09(13) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 120.31(13) . . ? C36 C37 H37A 119.8 . . ? C38 C37 H37A 119.8 . . ? C37 C38 C33 119.96(13) . . ? C37 C38 H38A 120.0 . . ? C33 C38 H38A 120.0 . . ? F13' P10 F10' 95.9(7) . . ? F13' P10 F12' 87.6(9) . . ? F10' P10 F12' 87.4(7) . . ? F13' P10 F15' 177.1(9) . . ? F10' P10 F15' 84.2(5) . . ? F12' P10 F15' 95.3(8) . . ? F13' P10 F11 107.7(7) . . ? F10' P10 F11 101.3(3) . . ? F12' P10 F11 161.3(8) . . ? F15' P10 F11 69.5(7) . . ? F13' P10 F14 106.9(6) . . ? F10' P10 F14 148.9(6) . . ? F12' P10 F14 73.1(8) . . ? F15' P10 F14 74.1(4) . . ? F11 P10 F14 91.73(12) . . ? F13' P10 F14' 92.0(7) . . ? F10' P10 F14' 171.9(6) . . ? F12' P10 F14' 90.7(8) . . ? F15' P10 F14' 88.1(5) . . ? F11 P10 F14' 78.3(5) . . ? F13' P10 F15 153.2(7) . . ? F10' P10 F15 60.1(5) . . ? F12' P10 F15 80.3(6) . . ? F11 P10 F15 89.75(14) . . ? F14 P10 F15 92.27(14) . . ? F14' P10 F15 111.8(5) . . ? F13' P10 F11' 91.7(9) . . ? F10' P10 F11' 93.2(7) . . ? F12' P10 F11' 179.1(8) . . ? F15' P10 F11' 85.4(9) . . ? F14 P10 F11' 106.6(9) . . ? F14' P10 F11' 88.8(8) . . ? F15 P10 F11' 100.6(6) . . ? F10' P10 F13 117.5(6) . . ? F12' P10 F13 97.3(6) . . ? F15' P10 F13 155.2(4) . . ? F11 P10 F13 93.22(14) . . ? F14 P10 F13 89.35(12) . . ? F14' P10 F13 70.5(5) . . ? F15 P10 F13 176.57(14) . . ? F11' P10 F13 81.8(6) . . ? F13' P10 F10 71.1(6) . . ? F12' P10 F10 106.6(8) . . ? F15' P10 F10 107.9(4) . . ? F11 P10 F10 88.99(10) . . ? F14 P10 F10 178.00(12) . . ? F14' P10 F10 154.8(6) . . ? F15 P10 F10 89.60(13) . . ? F11' P10 F10 73.7(9) . . ? F13 P10 F10 88.75(10) . . ? F13' P10 F12 72.7(7) . . ? F10' P10 F12 77.5(3) . . ? F15' P10 F12 110.1(7) . . ? F11 P10 F12 178.83(14) . . ? F14 P10 F12 89.20(15) . . ? F14' P10 F12 102.8(5) . . ? F15 P10 F12 89.50(13) . . ? F11' P10 F12 160.7(9) . . ? F13 P10 F12 87.50(13) . . ? F10 P10 F12 90.11(14) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.426 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.052 # Attachment 'Cu(PhbpyMe)2.CIF' data_3t _database_code_depnum_ccdc_archive 'CCDC 796691' #TrackingRef 'Cu(PhbpyMe)2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H28 Cu N4, F6 P' _chemical_formula_sum 'C34 H28 Cu F6 N4 P' _chemical_formula_weight 701.12 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' 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5396(10) _cell_length_b 12.2287(10) _cell_length_c 13.3195(11) _cell_angle_alpha 104.793(7) _cell_angle_beta 102.457(7) _cell_angle_gamma 105.796(7) _cell_volume 1520.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15807 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 64.09 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.840 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8843 _exptl_absorpt_correction_T_max 0.9592 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44176 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.00 _reflns_number_total 7306 _reflns_number_gt 6713 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0349P)^2^+0.9994P] 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 7306 _refine_ls_number_parameters 471 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.003 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 0.27954(2) 0.750717(19) 0.235238(16) 0.02250(6) Uani 1 1 d . . . N1 N 0.21684(15) 0.76861(12) 0.08909(11) 0.0218(3) Uani 1 1 d . . . N2 N 0.08133(14) 0.62756(12) 0.18127(11) 0.0217(3) Uani 1 1 d . . . C1 C 0.4428(2) 0.90528(18) 0.10799(17) 0.0335(4) Uani 1 1 d . . . H1A H 0.4632 0.8910 0.1779 0.050 Uiso 1 1 calc R . . H1B H 0.4618 0.9916 0.1213 0.050 Uiso 1 1 calc R . . H1C H 0.5011 0.8781 0.0664 0.050 Uiso 1 1 calc R . . C2 C 0.29371(19) 0.83691(15) 0.04458(14) 0.0264(3) Uani 1 1 d . . . C3 C 0.2362(2) 0.84551(18) -0.05622(16) 0.0350(4) Uani 1 1 d . . . H3A H 0.2923 0.8929 -0.0875 0.042 Uiso 1 1 calc R . . C4 C 0.0973(2) 0.78479(19) -0.11023(16) 0.0372(4) Uani 1 1 d . . . H4A H 0.0566 0.7905 -0.1788 0.045 Uiso 1 1 calc R . . C5 C 0.0176(2) 0.71531(17) -0.06386(15) 0.0310(4) Uani 1 1 d . . . H5A H -0.0786 0.6733 -0.0997 0.037 Uiso 1 1 calc R . . C6 C 0.08037(17) 0.70811(15) 0.03549(13) 0.0229(3) Uani 1 1 d . . . C7 C 0.00316(17) 0.63588(15) 0.09114(13) 0.0225(3) Uani 1 1 d . . . C8 C -0.14040(18) 0.58176(17) 0.05487(15) 0.0303(4) Uani 1 1 d . . . H8A H -0.1939 0.5887 -0.0089 0.036 Uiso 1 1 calc R . . C9 C -0.20354(19) 0.51798(18) 0.11296(17) 0.0336(4) Uani 1 1 d . . . H9A H -0.3012 0.4791 0.0889 0.040 Uiso 1 1 calc R . . C10 C -0.12382(19) 0.51095(17) 0.20632(16) 0.0310(4) Uani 1 1 d . . . H10A H -0.1661 0.4686 0.2480 0.037 Uiso 1 1 calc R . . C11 C 0.01901(18) 0.56655(15) 0.23853(14) 0.0252(3) Uani 1 1 d . . . C12 C 0.11108(19) 0.56064(16) 0.33667(15) 0.0301(4) Uani 1 1 d . . . C13 C 0.0918(2) 0.6006(2) 0.43785(17) 0.0420(5) Uani 1 1 d . . . H13A H 0.0177 0.6292 0.4441 0.050 Uiso 1 1 calc R . . C14 C 0.1821(3) 0.5982(2) 0.5301(2) 0.0573(7) Uani 1 1 d . . . H14A H 0.1711 0.6278 0.5997 0.069 Uiso 1 1 calc R . . C15 C 0.2872(3) 0.5533(2) 0.5209(2) 0.0590(8) Uani 1 1 d . . . H15A H 0.3477 0.5513 0.5841 0.071 Uiso 1 1 calc R . . C16 C 0.3047(3) 0.5112(2) 0.4205(2) 0.0497(6) Uani 1 1 d . . . H16A H 0.3761 0.4788 0.4142 0.060 Uiso 1 1 calc R . . C17 C 0.2184(2) 0.51625(17) 0.32840(18) 0.0356(4) Uani 1 1 d . . . H17A H 0.2324 0.4894 0.2595 0.043 Uiso 1 1 calc R . . N3 N 0.45575(14) 0.74215(12) 0.32052(12) 0.0226(3) Uani 1 1 d . . . N4 N 0.29645(15) 0.86035(12) 0.38800(11) 0.0225(3) Uani 1 1 d . . . C18 C 0.4933(2) 0.62729(17) 0.15844(15) 0.0316(4) Uani 1 1 d . . . H18A H 0.5725 0.6534 0.1322 0.047 Uiso 1 1 calc R . . H18B H 0.4178 0.6506 0.1237 0.047 Uiso 1 1 calc R . . H18C H 0.4617 0.5395 0.1402 0.047 Uiso 1 1 calc R . . C19 C 0.53566(18) 0.68595(15) 0.27961(15) 0.0260(3) Uani 1 1 d . . . C20 C 0.65235(19) 0.67996(18) 0.34796(17) 0.0331(4) Uani 1 1 d . . . H20A H 0.7085 0.6403 0.3180 0.040 Uiso 1 1 calc R . . C21 C 0.6854(2) 0.73196(18) 0.45914(17) 0.0352(4) Uani 1 1 d . . . H21A H 0.7645 0.7285 0.5066 0.042 Uiso 1 1 calc R . . C22 C 0.60269(19) 0.78929(17) 0.50113(15) 0.0310(4) Uani 1 1 d . . . H22A H 0.6239 0.8255 0.5777 0.037 Uiso 1 1 calc R . . C23 C 0.48815(17) 0.79310(15) 0.42963(14) 0.0243(3) Uani 1 1 d . . . C24 C 0.39133(18) 0.84947(15) 0.46710(14) 0.0244(3) Uani 1 1 d . . . C25 C 0.3929(2) 0.88372(18) 0.57568(15) 0.0331(4) Uani 1 1 d . . . H25A H 0.4611 0.8760 0.6304 0.040 Uiso 1 1 calc R . . C26 C 0.2937(2) 0.9289(2) 0.60198(16) 0.0384(4) Uani 1 1 d . . . H26A H 0.2928 0.9529 0.6754 0.046 Uiso 1 1 calc R . . C27 C 0.1956(2) 0.93900(18) 0.52094(16) 0.0341(4) Uani 1 1 d . . . H27A H 0.1259 0.9690 0.5380 0.041 Uiso 1 1 calc R . . C28 C 0.19987(18) 0.90479(15) 0.41420(14) 0.0257(3) Uani 1 1 d . . . C29 C 0.09876(19) 0.91535(15) 0.32433(15) 0.0262(3) Uani 1 1 d . . . C30 C -0.0423(2) 0.87173(18) 0.31191(18) 0.0350(4) Uani 1 1 d . . . H30A H -0.0734 0.8374 0.3625 0.042 Uiso 1 1 calc R . . C31 C -0.1372(2) 0.8784(2) 0.2259(2) 0.0431(5) Uani 1 1 d . . . H31A H -0.2335 0.8471 0.2170 0.052 Uiso 1 1 calc R . . C32 C -0.0934(2) 0.9300(2) 0.15301(19) 0.0438(5) Uani 1 1 d . . . H32A H -0.1591 0.9339 0.0940 0.053 Uiso 1 1 calc R . . C33 C 0.0471(2) 0.97609(18) 0.16609(17) 0.0370(4) Uani 1 1 d . . . H33A H 0.0777 1.0133 0.1170 0.044 Uiso 1 1 calc R . . C34 C 0.1427(2) 0.96794(16) 0.25071(15) 0.0292(4) Uani 1 1 d . . . H34A H 0.2388 0.9983 0.2586 0.035 Uiso 1 1 calc R . . P1 P 0.42623(6) 0.26790(4) 0.16095(4) 0.03156(11) Uani 1 1 d . . . F10 F 0.5320(7) 0.4020(3) 0.2325(4) 0.0770(17) Uani 0.662(11) 1 d P A 1 F11 F 0.3392(9) 0.1370(6) 0.0885(7) 0.093(3) Uani 0.662(11) 1 d P A 1 F12 F 0.3988(8) 0.2408(8) 0.2623(5) 0.099(2) Uani 0.662(11) 1 d P A 1 F13 F 0.3080(6) 0.3132(5) 0.1356(4) 0.0845(15) Uani 0.662(11) 1 d P A 1 F14 F 0.4686(6) 0.2967(5) 0.0624(4) 0.0909(17) Uani 0.662(11) 1 d P A 1 F15 F 0.5587(5) 0.2259(4) 0.1911(4) 0.0885(16) Uani 0.662(11) 1 d P A 1 F10' F 0.4602(12) 0.3944(7) 0.2453(6) 0.061(2) Uani 0.338(11) 1 d P A 2 F11' F 0.3670(19) 0.1360(11) 0.0744(12) 0.081(4) Uani 0.338(11) 1 d P A 2 F12' F 0.4350(16) 0.2195(12) 0.2563(9) 0.102(6) Uani 0.338(11) 1 d P A 2 F13' F 0.2611(8) 0.2462(16) 0.1484(12) 0.138(5) Uani 0.338(11) 1 d P A 2 F14' F 0.393(2) 0.3151(8) 0.0597(7) 0.132(6) Uani 0.338(11) 1 d PU A 2 F15' F 0.5678(10) 0.2876(15) 0.1647(11) 0.137(6) Uani 0.338(11) 1 d P A 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 Cu1 0.01982(10) 0.02482(11) 0.01885(10) 0.00599(7) 0.00111(7) 0.00659(8) N1 0.0241(7) 0.0206(6) 0.0206(6) 0.0057(5) 0.0052(5) 0.0100(5) N2 0.0209(6) 0.0193(6) 0.0213(6) 0.0041(5) 0.0037(5) 0.0063(5) C1 0.0318(9) 0.0319(9) 0.0378(10) 0.0161(8) 0.0115(8) 0.0078(8) C2 0.0324(9) 0.0233(8) 0.0268(8) 0.0096(7) 0.0100(7) 0.0127(7) C3 0.0470(11) 0.0322(10) 0.0305(9) 0.0173(8) 0.0126(8) 0.0139(8) C4 0.0494(12) 0.0366(10) 0.0257(9) 0.0152(8) 0.0029(8) 0.0174(9) C5 0.0336(9) 0.0296(9) 0.0243(8) 0.0064(7) -0.0015(7) 0.0128(7) C6 0.0249(8) 0.0213(7) 0.0207(7) 0.0033(6) 0.0034(6) 0.0114(6) C7 0.0217(7) 0.0215(7) 0.0210(7) 0.0024(6) 0.0034(6) 0.0092(6) C8 0.0217(8) 0.0346(9) 0.0297(9) 0.0059(7) 0.0023(7) 0.0111(7) C9 0.0194(8) 0.0352(10) 0.0393(10) 0.0052(8) 0.0073(7) 0.0072(7) C10 0.0263(9) 0.0297(9) 0.0368(10) 0.0097(7) 0.0137(7) 0.0077(7) C11 0.0255(8) 0.0200(7) 0.0268(8) 0.0051(6) 0.0068(7) 0.0061(6) C12 0.0298(9) 0.0234(8) 0.0295(9) 0.0113(7) 0.0035(7) -0.0006(7) C13 0.0490(12) 0.0362(11) 0.0329(10) 0.0145(8) 0.0122(9) 0.0003(9) C14 0.0743(18) 0.0467(13) 0.0315(11) 0.0195(10) 0.0071(11) -0.0075(12) C15 0.0613(16) 0.0451(13) 0.0472(14) 0.0300(11) -0.0128(12) -0.0077(12) C16 0.0417(12) 0.0368(11) 0.0569(14) 0.0251(10) -0.0094(10) 0.0027(9) C17 0.0317(9) 0.0282(9) 0.0381(10) 0.0133(8) -0.0012(8) 0.0042(7) N3 0.0196(6) 0.0208(6) 0.0245(7) 0.0092(5) 0.0027(5) 0.0042(5) N4 0.0232(7) 0.0188(6) 0.0206(6) 0.0054(5) 0.0040(5) 0.0030(5) C18 0.0325(9) 0.0313(9) 0.0321(9) 0.0083(7) 0.0086(8) 0.0159(8) C19 0.0237(8) 0.0232(8) 0.0303(9) 0.0111(7) 0.0055(7) 0.0068(6) C20 0.0237(8) 0.0320(9) 0.0437(11) 0.0152(8) 0.0053(8) 0.0114(7) C21 0.0252(9) 0.0337(10) 0.0417(11) 0.0174(8) -0.0032(8) 0.0083(7) C22 0.0277(9) 0.0299(9) 0.0273(8) 0.0126(7) -0.0023(7) 0.0034(7) C23 0.0224(8) 0.0210(7) 0.0243(8) 0.0101(6) 0.0022(6) 0.0012(6) C24 0.0243(8) 0.0203(7) 0.0215(8) 0.0069(6) 0.0030(6) 0.0006(6) C25 0.0360(10) 0.0349(10) 0.0211(8) 0.0092(7) 0.0040(7) 0.0052(8) C26 0.0471(12) 0.0408(11) 0.0229(8) 0.0072(8) 0.0131(8) 0.0096(9) C27 0.0394(10) 0.0329(10) 0.0301(9) 0.0066(7) 0.0155(8) 0.0123(8) C28 0.0282(8) 0.0199(7) 0.0257(8) 0.0055(6) 0.0085(7) 0.0050(6) C29 0.0284(8) 0.0190(7) 0.0278(8) 0.0027(6) 0.0075(7) 0.0089(6) C30 0.0309(9) 0.0296(9) 0.0428(11) 0.0081(8) 0.0127(8) 0.0109(8) C31 0.0288(10) 0.0365(11) 0.0568(14) 0.0069(10) 0.0063(9) 0.0140(8) C32 0.0435(12) 0.0386(11) 0.0425(12) 0.0062(9) -0.0031(9) 0.0231(9) C33 0.0468(11) 0.0325(10) 0.0322(10) 0.0102(8) 0.0068(9) 0.0191(9) C34 0.0324(9) 0.0249(8) 0.0280(9) 0.0054(7) 0.0076(7) 0.0112(7) P1 0.0392(3) 0.0283(2) 0.0277(2) 0.01194(19) 0.0070(2) 0.0125(2) F10 0.098(3) 0.0360(14) 0.057(2) 0.0173(13) -0.022(2) -0.0034(19) F11 0.096(3) 0.035(3) 0.086(5) 0.014(3) -0.040(3) -0.012(2) F12 0.118(4) 0.146(5) 0.076(3) 0.082(3) 0.058(3) 0.045(3) F13 0.059(3) 0.107(3) 0.115(3) 0.055(3) 0.020(2) 0.060(2) F14 0.124(4) 0.105(3) 0.056(2) 0.042(2) 0.054(3) 0.025(3) F15 0.051(2) 0.080(3) 0.135(3) 0.035(2) 0.009(2) 0.039(2) F10' 0.095(6) 0.028(3) 0.043(3) -0.002(2) 0.013(4) 0.017(4) F11' 0.149(11) 0.042(5) 0.043(4) -0.002(3) -0.002(5) 0.060(7) F12' 0.145(11) 0.068(5) 0.048(5) 0.039(4) -0.033(6) -0.002(6) F13' 0.037(4) 0.156(11) 0.199(11) 0.022(9) 0.027(5) 0.040(5) F14' 0.245(15) 0.055(4) 0.045(4) 0.028(3) -0.033(7) 0.023(6) F15' 0.059(5) 0.149(11) 0.181(11) 0.025(9) 0.079(6) -0.004(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 Cu1 N3 2.0018(14) . ? Cu1 N1 2.0038(14) . ? Cu1 N2 2.0580(14) . ? Cu1 N4 2.0712(14) . ? N1 C2 1.341(2) . ? N1 C6 1.354(2) . ? N2 C11 1.345(2) . ? N2 C7 1.346(2) . ? C1 C2 1.494(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.392(3) . ? C3 C4 1.375(3) . ? C3 H3A 0.9500 . ? C4 C5 1.383(3) . ? C4 H4A 0.9500 . ? C5 C6 1.382(2) . ? C5 H5A 0.9500 . ? C6 C7 1.482(2) . ? C7 C8 1.392(2) . ? C8 C9 1.378(3) . ? C8 H8A 0.9500 . ? C9 C10 1.379(3) . ? C9 H9A 0.9500 . ? C10 C11 1.388(2) . ? C10 H10A 0.9500 . ? C11 C12 1.482(2) . ? C12 C13 1.390(3) . ? C12 C17 1.394(3) . ? C13 C14 1.395(3) . ? C13 H13A 0.9500 . ? C14 C15 1.378(4) . ? C14 H14A 0.9500 . ? C15 C16 1.377(4) . ? C15 H15A 0.9500 . ? C16 C17 1.387(3) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? N3 C19 1.342(2) . ? N3 C23 1.351(2) . ? N4 C28 1.346(2) . ? N4 C24 1.348(2) . ? C18 C19 1.497(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.395(2) . ? C20 C21 1.376(3) . ? C20 H20A 0.9500 . ? C21 C22 1.381(3) . ? C21 H21A 0.9500 . ? C22 C23 1.387(2) . ? C22 H22A 0.9500 . ? C23 C24 1.481(3) . ? C24 C25 1.394(2) . ? C25 C26 1.376(3) . ? C25 H25A 0.9500 . ? C26 C27 1.380(3) . ? C26 H26A 0.9500 . ? C27 C28 1.390(3) . ? C27 H27A 0.9500 . ? C28 C29 1.479(2) . ? C29 C30 1.392(3) . ? C29 C34 1.395(3) . ? C30 C31 1.385(3) . ? C30 H30A 0.9500 . ? C31 C32 1.379(4) . ? C31 H31A 0.9500 . ? C32 C33 1.387(3) . ? C32 H32A 0.9500 . ? C33 C34 1.385(3) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? P1 F15' 1.433(9) . ? P1 F13 1.505(3) . ? P1 F12' 1.528(11) . ? P1 F12 1.536(5) . ? P1 F11 1.538(6) . ? P1 F10' 1.556(6) . ? P1 F14 1.565(4) . ? P1 F11' 1.585(11) . ? P1 F14' 1.605(7) . ? P1 F10 1.609(3) . ? P1 F15 1.621(3) . ? P1 F13' 1.651(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N1 133.57(6) . . ? N3 Cu1 N2 129.48(6) . . ? N1 Cu1 N2 81.41(6) . . ? N3 Cu1 N4 81.17(6) . . ? N1 Cu1 N4 129.45(6) . . ? N2 Cu1 N4 104.20(6) . . ? C2 N1 C6 119.32(15) . . ? C2 N1 Cu1 126.75(12) . . ? C6 N1 Cu1 113.85(11) . . ? C11 N2 C7 119.17(15) . . ? C11 N2 Cu1 126.64(11) . . ? C7 N2 Cu1 112.04(11) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 121.19(17) . . ? N1 C2 C1 117.62(16) . . ? C3 C2 C1 121.17(17) . . ? C4 C3 C2 119.46(18) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 119.39(17) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C6 C5 C4 118.83(18) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? N1 C6 C5 121.79(17) . . ? N1 C6 C7 115.66(14) . . ? C5 C6 C7 122.55(16) . . ? N2 C7 C8 121.72(16) . . ? N2 C7 C6 115.35(14) . . ? C8 C7 C6 122.92(16) . . ? C9 C8 C7 118.88(17) . . ? C9 C8 H8A 120.6 . . ? C7 C8 H8A 120.6 . . ? C8 C9 C10 119.51(17) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? C9 C10 C11 119.10(18) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? N2 C11 C10 121.62(17) . . ? N2 C11 C12 116.40(15) . . ? C10 C11 C12 121.97(17) . . ? C13 C12 C17 119.59(19) . . ? C13 C12 C11 120.12(19) . . ? C17 C12 C11 120.29(17) . . ? C12 C13 C14 119.5(2) . . ? C12 C13 H13A 120.3 . . ? C14 C13 H13A 120.3 . . ? C15 C14 C13 120.4(2) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C16 C15 C14 120.2(2) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 C17 120.1(3) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C17 C12 120.2(2) . . ? C16 C17 H17A 119.9 . . ? C12 C17 H17A 119.9 . . ? C19 N3 C23 119.55(15) . . ? C19 N3 Cu1 126.17(12) . . ? C23 N3 Cu1 114.16(11) . . ? C28 N4 C24 119.23(15) . . ? C28 N4 Cu1 125.89(12) . . ? C24 N4 Cu1 111.30(11) . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 121.05(17) . . ? N3 C19 C18 117.72(15) . . ? C20 C19 C18 121.21(17) . . ? C21 C20 C19 119.41(18) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? C20 C21 C22 119.46(17) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C21 C22 C23 118.86(18) . . ? C21 C22 H22A 120.6 . . ? C23 C22 H22A 120.6 . . ? N3 C23 C22 121.68(17) . . ? N3 C23 C24 115.57(15) . . ? C22 C23 C24 122.73(16) . . ? N4 C24 C25 121.85(17) . . ? N4 C24 C23 115.37(15) . . ? C25 C24 C23 122.71(16) . . ? C26 C25 C24 118.69(18) . . ? C26 C25 H25A 120.7 . . ? C24 C25 H25A 120.7 . . ? C25 C26 C27 119.57(18) . . ? C25 C26 H26A 120.2 . . ? C27 C26 H26A 120.2 . . ? C26 C27 C28 119.35(18) . . ? C26 C27 H27A 120.3 . . ? C28 C27 H27A 120.3 . . ? N4 C28 C27 121.32(17) . . ? N4 C28 C29 116.97(15) . . ? C27 C28 C29 121.72(17) . . ? C30 C29 C34 119.17(18) . . ? C30 C29 C28 120.04(17) . . ? C34 C29 C28 120.78(16) . . ? C31 C30 C29 120.1(2) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C32 C31 C30 120.6(2) . . ? C32 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? C31 C32 C33 119.8(2) . . ? C31 C32 H32A 120.1 . . ? C33 C32 H32A 120.1 . . ? C34 C33 C32 120.1(2) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C33 C34 C29 120.31(19) . . ? C33 C34 H34A 119.8 . . ? C29 C34 H34A 119.8 . . ? F15' P1 F13 144.2(7) . . ? F15' P1 F12' 94.9(8) . . ? F13 P1 F12' 114.9(7) . . ? F15' P1 F12 111.4(7) . . ? F13 P1 F12 95.6(3) . . ? F15' P1 F11 108.3(6) . . ? F13 P1 F11 93.8(4) . . ? F12' P1 F11 85.8(6) . . ? F12 P1 F11 90.9(5) . . ? F15' P1 F10' 93.7(5) . . ? F13 P1 F10' 69.9(4) . . ? F12' P1 F10' 87.3(6) . . ? F12 P1 F10' 75.9(4) . . ? F11 P1 F10' 157.4(5) . . ? F15' P1 F14 63.3(6) . . ? F13 P1 F14 89.3(3) . . ? F12' P1 F14 155.7(7) . . ? F12 P1 F14 174.7(4) . . ? F11 P1 F14 91.0(4) . . ? F10' P1 F14 103.8(3) . . ? F15' P1 F11' 95.4(8) . . ? F13 P1 F11' 102.4(6) . . ? F12' P1 F11' 92.0(8) . . ? F12 P1 F11' 100.8(7) . . ? F10' P1 F11' 171.0(7) . . ? F14 P1 F11' 80.3(7) . . ? F15' P1 F14' 93.5(8) . . ? F13 P1 F14' 57.3(7) . . ? F12' P1 F14' 171.6(8) . . ? F12 P1 F14' 152.8(8) . . ? F11 P1 F14' 91.4(5) . . ? F10' P1 F14' 92.4(5) . . ? F11' P1 F14' 87.0(7) . . ? F15' P1 F10 65.2(5) . . ? F13 P1 F10 91.6(2) . . ? F12' P1 F10 95.4(4) . . ? F12 P1 F10 92.3(4) . . ? F11 P1 F10 173.4(4) . . ? F14 P1 F10 85.3(3) . . ? F11' P1 F10 159.7(7) . . ? F14' P1 F10 88.3(4) . . ? F13 P1 F15 177.2(2) . . ? F12' P1 F15 65.7(7) . . ? F12 P1 F15 84.8(3) . . ? F11 P1 F15 89.0(4) . . ? F10' P1 F15 107.6(4) . . ? F14 P1 F15 90.2(3) . . ? F11' P1 F15 80.3(6) . . ? F14' P1 F15 122.2(7) . . ? F10 P1 F15 85.6(2) . . ? F15' P1 F13' 176.1(7) . . ? F12' P1 F13' 88.8(8) . . ? F12 P1 F13' 72.5(7) . . ? F11 P1 F13' 70.9(6) . . ? F10' P1 F13' 87.5(5) . . ? F14 P1 F13' 112.8(6) . . ? F11' P1 F13' 83.5(8) . . ? F14' P1 F13' 82.7(7) . . ? F10 P1 F13' 115.5(4) . . ? F15 P1 F13' 149.1(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.508 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.050 # Attachment 'Cu(bpy)(dppe).CIF' data_esc08 _database_code_depnum_ccdc_archive 'CCDC 796692' #TrackingRef 'Cu(bpy)(dppe).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H32 Cu N2 P2), C4 H10 O, 2(F6 P), 1.5(C H2 Cl2)' _chemical_formula_sum 'C77.50 H77 Cl3 Cu2 F12 N4 O P6' _chemical_formula_weight 1727.70 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' Cu Cu 0.3201 1.2651 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.611(2) _cell_length_b 13.045(3) _cell_length_c 14.699(3) _cell_angle_alpha 115.99(3) _cell_angle_beta 97.55(3) _cell_angle_gamma 90.93(3) _cell_volume 1977.1(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 885 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7310 _exptl_absorpt_correction_T_max 0.8849 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53834 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 31.00 _reflns_number_total 12473 _reflns_number_gt 11793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0618P)^2^+1.0665P] 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 12473 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Cu1 Cu 0.879428(15) 0.648228(14) 0.238875(12) 0.02153(5) Uani 1 1 d . . . P1 P 1.04132(3) 0.71933(3) 0.35630(3) 0.02108(7) Uani 1 1 d . . . P2 P 0.76718(3) 0.75111(3) 0.35485(3) 0.02291(8) Uani 1 1 d . . . C1 C 1.10183(12) 0.63737(12) 0.42159(11) 0.0233(2) Uani 1 1 d . . . C2 C 1.07778(16) 0.51950(14) 0.37445(14) 0.0320(3) Uani 1 1 d . . . H2A H 1.0290 0.4836 0.3099 0.038 Uiso 1 1 calc R . . C3 C 1.1245(2) 0.45312(16) 0.42082(17) 0.0415(4) Uani 1 1 d . . . H3A H 1.1083 0.3723 0.3877 0.050 Uiso 1 1 calc R . . C4 C 1.19418(18) 0.50549(17) 0.51497(16) 0.0390(4) Uani 1 1 d . . . H4A H 1.2263 0.4606 0.5468 0.047 Uiso 1 1 calc R . . C5 C 1.21768(17) 0.62278(17) 0.56331(14) 0.0357(3) Uani 1 1 d . . . H5A H 1.2654 0.6583 0.6285 0.043 Uiso 1 1 calc R . . C6 C 1.17187(15) 0.68931(14) 0.51721(13) 0.0302(3) Uani 1 1 d . . . H6A H 1.1882 0.7701 0.5508 0.036 Uiso 1 1 calc R . . C7 C 1.16826(13) 0.77887(13) 0.32973(11) 0.0246(2) Uani 1 1 d . . . C8 C 1.27292(14) 0.72664(16) 0.32198(13) 0.0313(3) Uani 1 1 d . . . H8A H 1.2804 0.6620 0.3354 0.038 Uiso 1 1 calc R . . C9 C 1.36630(15) 0.7693(2) 0.29457(15) 0.0396(4) Uani 1 1 d . . . H9A H 1.4371 0.7329 0.2888 0.048 Uiso 1 1 calc R . . C10 C 1.35702(17) 0.86391(19) 0.27573(15) 0.0409(4) Uani 1 1 d . . . H10A H 1.4215 0.8932 0.2580 0.049 Uiso 1 1 calc R . . C11 C 1.25347(17) 0.91588(16) 0.28279(14) 0.0370(4) Uani 1 1 d . . . H11A H 1.2469 0.9809 0.2698 0.044 Uiso 1 1 calc R . . C12 C 1.15891(15) 0.87332(14) 0.30884(13) 0.0302(3) Uani 1 1 d . . . H12A H 1.0877 0.9087 0.3124 0.036 Uiso 1 1 calc R . . C13 C 0.98838(14) 0.84414(12) 0.45725(11) 0.0266(3) Uani 1 1 d . . . H13A H 1.0449 0.8722 0.5214 0.032 Uiso 1 1 calc R . . H13B H 0.9809 0.9066 0.4363 0.032 Uiso 1 1 calc R . . C14 C 0.86982(14) 0.81048(14) 0.47564(11) 0.0275(3) Uani 1 1 d . . . H14A H 0.8393 0.8785 0.5273 0.033 Uiso 1 1 calc R . . H14B H 0.8786 0.7528 0.5023 0.033 Uiso 1 1 calc R . . C15 C 0.70424(13) 0.87680(13) 0.35093(12) 0.0259(3) Uani 1 1 d . . . C16 C 0.65580(16) 0.95819(15) 0.43220(13) 0.0338(3) Uani 1 1 d . . . H16A H 0.6546 0.9490 0.4927 0.041 Uiso 1 1 calc R . . C17 C 0.60952(17) 1.05216(15) 0.42504(17) 0.0410(4) Uani 1 1 d . . . H17A H 0.5766 1.1069 0.4805 0.049 Uiso 1 1 calc R . . C18 C 0.61120(17) 1.06641(17) 0.33735(19) 0.0434(4) Uani 1 1 d . . . H18A H 0.5792 1.1308 0.3327 0.052 Uiso 1 1 calc R . . C19 C 0.65919(19) 0.9874(2) 0.2568(2) 0.0470(5) Uani 1 1 d . . . H19A H 0.6610 0.9974 0.1967 0.056 Uiso 1 1 calc R . . C20 C 0.70513(17) 0.89245(18) 0.26391(16) 0.0386(4) Uani 1 1 d . . . H20A H 0.7376 0.8377 0.2080 0.046 Uiso 1 1 calc R . . C21 C 0.64964(14) 0.67727(14) 0.37957(13) 0.0279(3) Uani 1 1 d . . . C22 C 0.61408(17) 0.71335(17) 0.47514(15) 0.0365(4) Uani 1 1 d . . . H22A H 0.6519 0.7799 0.5322 0.044 Uiso 1 1 calc R . . C23 C 0.52281(19) 0.65146(19) 0.48670(18) 0.0439(5) Uani 1 1 d . . . H23A H 0.4986 0.6764 0.5518 0.053 Uiso 1 1 calc R . . C24 C 0.46754(19) 0.5548(2) 0.4050(2) 0.0471(5) Uani 1 1 d . . . H24A H 0.4048 0.5138 0.4136 0.056 Uiso 1 1 calc R . . C25 C 0.50319(19) 0.5174(2) 0.3105(2) 0.0473(5) Uani 1 1 d . . . H25A H 0.4659 0.4500 0.2541 0.057 Uiso 1 1 calc R . . C26 C 0.59432(16) 0.57888(17) 0.29793(15) 0.0361(3) Uani 1 1 d . . . H26A H 0.6186 0.5530 0.2327 0.043 Uiso 1 1 calc R . . N1 N 0.88466(11) 0.65287(11) 0.10309(9) 0.0237(2) Uani 1 1 d . . . N2 N 0.83646(11) 0.47966(11) 0.14278(10) 0.0248(2) Uani 1 1 d . . . C27 C 0.91209(15) 0.74454(14) 0.08903(12) 0.0291(3) Uani 1 1 d . . . H27A H 0.9324 0.8160 0.1477 0.035 Uiso 1 1 calc R . . C28 C 0.91237(18) 0.74036(16) -0.00663(14) 0.0359(3) Uani 1 1 d . . . H28A H 0.9325 0.8071 -0.0137 0.043 Uiso 1 1 calc R . . C29 C 0.8825(2) 0.63651(18) -0.09123(14) 0.0419(4) Uani 1 1 d . . . H29A H 0.8803 0.6308 -0.1581 0.050 Uiso 1 1 calc R . . C30 C 0.85573(19) 0.54038(16) -0.07810(13) 0.0372(4) Uani 1 1 d . . . H30A H 0.8361 0.4680 -0.1358 0.045 Uiso 1 1 calc R . . C31 C 0.85788(13) 0.55103(13) 0.02054(11) 0.0252(3) Uani 1 1 d . . . C32 C 0.83163(14) 0.45380(13) 0.04278(11) 0.0264(3) Uani 1 1 d . . . C33 C 0.8060(2) 0.34228(15) -0.03340(14) 0.0395(4) Uani 1 1 d . . . H33A H 0.8036 0.3256 -0.1034 0.047 Uiso 1 1 calc R . . C34 C 0.7841(2) 0.25564(16) -0.00610(16) 0.0475(5) Uani 1 1 d . . . H34A H 0.7667 0.1788 -0.0572 0.057 Uiso 1 1 calc R . . C35 C 0.7879(2) 0.28207(16) 0.09630(16) 0.0412(4) Uani 1 1 d . . . H35A H 0.7728 0.2241 0.1168 0.049 Uiso 1 1 calc R . . C36 C 0.81419(16) 0.39467(14) 0.16783(13) 0.0318(3) Uani 1 1 d . . . H36A H 0.8167 0.4130 0.2382 0.038 Uiso 1 1 calc R . . P10 P 1.02131(5) 0.90848(4) 0.79213(4) 0.04004(12) Uani 1 1 d . . . F10 F 1.05624(16) 0.97404(13) 0.72821(12) 0.0587(4) Uani 1 1 d . . . F11 F 1.13114(15) 0.97049(17) 0.87631(13) 0.0688(4) Uani 1 1 d . . . F12 F 0.94569(13) 1.01152(11) 0.85201(11) 0.0494(3) Uani 1 1 d . . . F13 F 1.0959(2) 0.80707(15) 0.73238(15) 0.0870(7) Uani 1 1 d . . . F14 F 0.98228(18) 0.84244(15) 0.85280(14) 0.0687(5) Uani 1 1 d . . . F15 F 0.90865(19) 0.84903(14) 0.70670(12) 0.0731(5) Uani 1 1 d . . . C100 C 0.2907(3) 0.1144(3) 0.1163(3) 0.0539(7) Uani 0.75 1 d P . . H10B H 0.2187 0.0769 0.1215 0.065 Uiso 0.75 1 calc PR . . H10C H 0.2717 0.1390 0.0616 0.065 Uiso 0.75 1 calc PR . . Cl1 Cl 0.39461(10) 0.01713(12) 0.08335(15) 0.0977(5) Uani 0.75 1 d P . . Cl2 Cl 0.33755(14) 0.23530(12) 0.23316(13) 0.0998(4) Uani 0.75 1 d P . . O200 O 0.4942(3) 0.4667(4) 0.0234(2) 0.0954(11) Uani 0.50 1 d P . 1 C201 C 0.4942(3) 0.4667(4) 0.0234(2) 0.0954(11) Uani 0.50 1 d P . 2 H20B H 0.4374 0.4978 0.0717 0.114 Uiso 0.50 1 calc PR . 2 H20C H 0.5700 0.4678 0.0636 0.114 Uiso 0.50 1 calc PR . 2 C202 C 0.4554(5) 0.3517(5) -0.0482(4) 0.1089(15) Uani 0.50 1 d P A 1 H20H H 0.3793 0.3482 -0.0893 0.131 Uiso 0.50 1 calc PR A 1 H20I H 0.5128 0.3172 -0.0951 0.131 Uiso 0.50 1 calc PR A 1 C203 C 0.4554(5) 0.3517(5) -0.0482(4) 0.1089(15) Uani 0.50 1 d P B 2 H20D H 0.3759 0.3492 -0.0817 0.163 Uiso 0.50 1 calc PR B 2 H20E H 0.4562 0.3037 -0.0123 0.163 Uiso 0.50 1 calc PR B 2 H20F H 0.5073 0.3233 -0.1000 0.163 Uiso 0.50 1 calc PR B 2 C204 C 0.4454(7) 0.2969(8) 0.0120(6) 0.094(2) Uani 0.50 1 d P A 1 H20G H 0.4275 0.2147 -0.0316 0.140 Uiso 0.50 1 calc PR A 1 H20J H 0.3827 0.3273 0.0526 0.140 Uiso 0.50 1 calc PR A 1 H20K H 0.5191 0.3097 0.0580 0.140 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 Cu1 0.02487(9) 0.02160(9) 0.01628(8) 0.00668(6) 0.00352(6) 0.00076(6) P1 0.02170(15) 0.01982(15) 0.01971(15) 0.00716(12) 0.00243(12) 0.00190(11) P2 0.02283(16) 0.02625(17) 0.02000(15) 0.00998(13) 0.00513(12) 0.00533(12) C1 0.0246(6) 0.0232(6) 0.0235(6) 0.0110(5) 0.0055(5) 0.0035(5) C2 0.0371(8) 0.0234(6) 0.0325(8) 0.0101(6) 0.0042(6) 0.0044(6) C3 0.0522(11) 0.0268(7) 0.0494(11) 0.0197(8) 0.0097(9) 0.0091(7) C4 0.0439(9) 0.0417(9) 0.0458(10) 0.0301(8) 0.0146(8) 0.0162(8) C5 0.0386(8) 0.0426(9) 0.0310(8) 0.0213(7) 0.0033(6) 0.0078(7) C6 0.0336(7) 0.0294(7) 0.0268(7) 0.0132(6) -0.0010(6) 0.0012(6) C7 0.0239(6) 0.0262(6) 0.0222(6) 0.0104(5) 0.0007(5) -0.0016(5) C8 0.0251(6) 0.0413(8) 0.0301(7) 0.0188(7) 0.0024(5) 0.0026(6) C9 0.0232(7) 0.0597(12) 0.0386(9) 0.0250(9) 0.0031(6) 0.0000(7) C10 0.0341(8) 0.0547(11) 0.0332(8) 0.0206(8) 0.0013(7) -0.0149(8) C11 0.0437(9) 0.0356(8) 0.0311(8) 0.0162(7) 0.0007(7) -0.0108(7) C12 0.0330(7) 0.0284(7) 0.0288(7) 0.0133(6) 0.0016(6) -0.0022(6) C13 0.0290(7) 0.0215(6) 0.0222(6) 0.0040(5) 0.0008(5) 0.0045(5) C14 0.0291(7) 0.0326(7) 0.0178(6) 0.0081(5) 0.0047(5) 0.0080(5) C15 0.0229(6) 0.0270(6) 0.0282(7) 0.0126(5) 0.0042(5) 0.0031(5) C16 0.0352(8) 0.0305(7) 0.0284(7) 0.0070(6) 0.0018(6) 0.0082(6) C17 0.0377(9) 0.0266(7) 0.0446(10) 0.0052(7) -0.0020(7) 0.0068(6) C18 0.0347(8) 0.0311(8) 0.0675(14) 0.0259(9) 0.0036(8) 0.0033(7) C19 0.0448(10) 0.0547(12) 0.0654(14) 0.0448(11) 0.0201(10) 0.0155(9) C20 0.0398(9) 0.0476(10) 0.0430(9) 0.0295(8) 0.0190(8) 0.0165(8) C21 0.0270(6) 0.0314(7) 0.0321(7) 0.0185(6) 0.0103(6) 0.0089(5) C22 0.0417(9) 0.0380(8) 0.0384(9) 0.0208(7) 0.0201(7) 0.0132(7) C23 0.0466(10) 0.0493(11) 0.0553(12) 0.0345(10) 0.0296(9) 0.0180(9) C24 0.0389(9) 0.0502(11) 0.0707(15) 0.0401(11) 0.0214(10) 0.0081(8) C25 0.0396(10) 0.0475(11) 0.0572(13) 0.0254(10) 0.0090(9) -0.0057(8) C26 0.0330(8) 0.0382(8) 0.0385(9) 0.0177(7) 0.0075(7) 0.0002(7) N1 0.0276(6) 0.0245(5) 0.0192(5) 0.0094(4) 0.0053(4) 0.0024(4) N2 0.0285(6) 0.0223(5) 0.0213(5) 0.0081(4) 0.0028(4) -0.0003(4) C27 0.0364(8) 0.0276(7) 0.0253(7) 0.0126(6) 0.0078(6) 0.0020(6) C28 0.0469(9) 0.0382(8) 0.0314(8) 0.0217(7) 0.0121(7) 0.0064(7) C29 0.0632(12) 0.0431(10) 0.0246(7) 0.0183(7) 0.0117(8) 0.0087(9) C30 0.0553(11) 0.0343(8) 0.0195(6) 0.0092(6) 0.0068(7) 0.0059(7) C31 0.0299(7) 0.0252(6) 0.0191(6) 0.0084(5) 0.0039(5) 0.0037(5) C32 0.0306(7) 0.0240(6) 0.0211(6) 0.0073(5) 0.0018(5) 0.0022(5) C33 0.0593(12) 0.0260(7) 0.0245(7) 0.0048(6) 0.0014(7) -0.0006(7) C34 0.0726(14) 0.0240(7) 0.0357(9) 0.0069(7) -0.0004(9) -0.0051(8) C35 0.0541(11) 0.0275(8) 0.0411(9) 0.0163(7) 0.0017(8) -0.0034(7) C36 0.0370(8) 0.0292(7) 0.0305(7) 0.0153(6) 0.0030(6) -0.0019(6) P10 0.0646(3) 0.0309(2) 0.0307(2) 0.01668(18) 0.0157(2) 0.0102(2) F10 0.0827(10) 0.0561(8) 0.0591(8) 0.0406(7) 0.0273(8) 0.0135(7) F11 0.0553(9) 0.0911(13) 0.0583(9) 0.0329(9) 0.0037(7) 0.0129(8) F12 0.0550(7) 0.0409(6) 0.0490(7) 0.0150(6) 0.0143(6) 0.0111(5) F13 0.155(2) 0.0594(10) 0.0720(11) 0.0370(9) 0.0666(13) 0.0604(12) F14 0.0999(13) 0.0718(10) 0.0678(10) 0.0555(9) 0.0333(9) 0.0208(9) F15 0.1131(15) 0.0484(8) 0.0442(8) 0.0155(7) -0.0112(9) -0.0209(9) C100 0.0435(14) 0.0525(17) 0.067(2) 0.0303(16) -0.0002(14) -0.0048(12) Cl1 0.0495(5) 0.0786(7) 0.1536(14) 0.0414(8) 0.0139(7) 0.0110(5) Cl2 0.0998(9) 0.0715(7) 0.0978(10) 0.0163(7) -0.0044(8) -0.0194(7) O200 0.085(2) 0.129(3) 0.0517(15) 0.0210(16) 0.0142(14) 0.002(2) C201 0.085(2) 0.129(3) 0.0517(15) 0.0210(16) 0.0142(14) 0.002(2) C202 0.102(3) 0.130(4) 0.084(3) 0.035(3) 0.027(3) 0.022(3) C203 0.102(3) 0.130(4) 0.084(3) 0.035(3) 0.027(3) 0.022(3) C204 0.086(5) 0.123(7) 0.056(4) 0.028(4) 0.004(4) -0.008(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 Cu1 N1 2.0320(13) . ? Cu1 N2 2.0337(15) . ? Cu1 P2 2.2451(10) . ? Cu1 P1 2.2496(11) . ? P1 C1 1.8177(15) . ? P1 C7 1.8189(16) . ? P1 C13 1.8397(17) . ? P2 C21 1.8214(17) . ? P2 C15 1.8265(16) . ? P2 C14 1.8388(17) . ? C1 C2 1.387(2) . ? C1 C6 1.394(2) . ? C2 C3 1.394(2) . ? C2 H2A 0.9500 . ? C3 C4 1.377(3) . ? C3 H3A 0.9500 . ? C4 C5 1.379(3) . ? C4 H4A 0.9500 . ? C5 C6 1.390(2) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.396(2) . ? C7 C12 1.397(2) . ? C8 C9 1.392(2) . ? C8 H8A 0.9500 . ? C9 C10 1.382(3) . ? C9 H9A 0.9500 . ? C10 C11 1.383(3) . ? C10 H10A 0.9500 . ? C11 C12 1.392(2) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.531(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.382(2) . ? C15 C16 1.398(2) . ? C16 C17 1.386(3) . ? C16 H16A 0.9500 . ? C17 C18 1.383(3) . ? C17 H17A 0.9500 . ? C18 C19 1.378(3) . ? C18 H18A 0.9500 . ? C19 C20 1.396(3) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C26 1.386(3) . ? C21 C22 1.394(2) . ? C22 C23 1.394(3) . ? C22 H22A 0.9500 . ? C23 C24 1.374(4) . ? C23 H23A 0.9500 . ? C24 C25 1.379(3) . ? C24 H24A 0.9500 . ? C25 C26 1.397(3) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? N1 C27 1.3400(19) . ? N1 C31 1.345(2) . ? N2 C36 1.344(2) . ? N2 C32 1.3493(19) . ? C27 C28 1.384(2) . ? C27 H27A 0.9500 . ? C28 C29 1.377(3) . ? C28 H28A 0.9500 . ? C29 C30 1.386(3) . ? C29 H29A 0.9500 . ? C30 C31 1.391(2) . ? C30 H30A 0.9500 . ? C31 C32 1.478(2) . ? C32 C33 1.389(2) . ? C33 C34 1.385(3) . ? C33 H33A 0.9500 . ? C34 C35 1.383(3) . ? C34 H34A 0.9500 . ? C35 C36 1.380(3) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? P10 F11 1.577(2) . ? P10 F13 1.5783(17) . ? P10 F14 1.5841(15) . ? P10 F12 1.5989(15) . ? P10 F15 1.604(2) . ? P10 F10 1.6036(14) . ? C100 Cl1 1.722(4) . ? C100 Cl2 1.757(4) . ? C100 H10B 0.9900 . ? C100 H10C 0.9900 . ? O200 O200 1.338(8) 2_665 ? O200 C202 1.425(7) . ? C202 C204 1.374(10) . ? C202 H20H 0.9900 . ? C202 H20I 0.9900 . ? C204 H20G 0.9800 . ? C204 H20J 0.9800 . ? C204 H20K 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 N1 Cu1 N2 80.91(6) . . ? N1 Cu1 P2 125.16(4) . . ? N2 Cu1 P2 121.72(5) . . ? N1 Cu1 P1 116.40(4) . . ? N2 Cu1 P1 125.27(5) . . ? P2 Cu1 P1 91.33(3) . . ? C1 P1 C7 104.23(7) . . ? C1 P1 C13 104.31(7) . . ? C7 P1 C13 103.79(8) . . ? C1 P1 Cu1 119.76(5) . . ? C7 P1 Cu1 120.95(5) . . ? C13 P1 Cu1 101.34(6) . . ? C21 P2 C15 104.60(7) . . ? C21 P2 C14 103.89(8) . . ? C15 P2 C14 103.83(8) . . ? C21 P2 Cu1 119.10(6) . . ? C15 P2 Cu1 120.28(6) . . ? C14 P2 Cu1 102.84(6) . . ? C2 C1 C6 119.12(15) . . ? C2 C1 P1 118.85(12) . . ? C6 C1 P1 122.02(12) . . ? C1 C2 C3 120.73(17) . . ? C1 C2 H2A 119.6 . . ? C3 C2 H2A 119.6 . . ? C4 C3 C2 119.52(17) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C3 C4 C5 120.37(16) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C4 C5 C6 120.35(17) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 119.89(16) . . ? C5 C6 H6A 120.1 . . ? C1 C6 H6A 120.1 . . ? C8 C7 C12 118.97(15) . . ? C8 C7 P1 121.16(12) . . ? C12 C7 P1 119.68(12) . . ? C9 C8 C7 120.06(16) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C10 C9 C8 120.61(18) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C9 C10 C11 119.70(16) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C10 C11 C12 120.31(17) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C7 120.33(17) . . ? C11 C12 H12A 119.8 . . ? C7 C12 H12A 119.8 . . ? C14 C13 P1 109.66(11) . . ? C14 C13 H13A 109.7 . . ? P1 C13 H13A 109.7 . . ? C14 C13 H13B 109.7 . . ? P1 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C13 C14 P2 109.64(10) . . ? C13 C14 H14A 109.7 . . ? P2 C14 H14A 109.7 . . ? C13 C14 H14B 109.7 . . ? P2 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C20 C15 C16 118.54(15) . . ? C20 C15 P2 118.50(13) . . ? C16 C15 P2 122.96(13) . . ? C17 C16 C15 120.45(18) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C18 C17 C16 120.20(19) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C19 C18 C17 120.11(17) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C18 C19 C20 119.60(19) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? C15 C20 C19 121.10(18) . . ? C15 C20 H20A 119.5 . . ? C19 C20 H20A 119.4 . . ? C26 C21 C22 119.01(16) . . ? C26 C21 P2 117.15(13) . . ? C22 C21 P2 123.84(15) . . ? C23 C22 C21 119.8(2) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C24 C23 C22 120.78(19) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 C25 119.91(19) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C26 119.8(2) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C21 C26 C25 120.68(19) . . ? C21 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C27 N1 C31 118.73(13) . . ? C27 N1 Cu1 127.02(11) . . ? C31 N1 Cu1 114.25(10) . . ? C36 N2 C32 118.40(14) . . ? C36 N2 Cu1 127.76(11) . . ? C32 N2 Cu1 113.84(10) . . ? N1 C27 C28 123.28(16) . . ? N1 C27 H27A 118.4 . . ? C28 C27 H27A 118.4 . . ? C29 C28 C27 117.95(17) . . ? C29 C28 H28A 121.0 . . ? C27 C28 H28A 121.0 . . ? C28 C29 C30 119.55(16) . . ? C28 C29 H29A 120.2 . . ? C30 C29 H29A 120.2 . . ? C29 C30 C31 119.26(17) . . ? C29 C30 H30A 120.4 . . ? C31 C30 H30A 120.4 . . ? N1 C31 C30 121.19(15) . . ? N1 C31 C32 115.34(13) . . ? C30 C31 C32 123.47(15) . . ? N2 C32 C33 121.60(15) . . ? N2 C32 C31 115.65(13) . . ? C33 C32 C31 122.74(14) . . ? C34 C33 C32 119.20(17) . . ? C34 C33 H33A 120.4 . . ? C32 C33 H33A 120.4 . . ? C35 C34 C33 119.33(17) . . ? C35 C34 H34A 120.3 . . ? C33 C34 H34A 120.3 . . ? C36 C35 C34 118.31(17) . . ? C36 C35 H35A 120.8 . . ? C34 C35 H35A 120.8 . . ? N2 C36 C35 123.16(16) . . ? N2 C36 H36A 118.4 . . ? C35 C36 H36A 118.4 . . ? F11 P10 F13 90.02(13) . . ? F11 P10 F14 91.66(11) . . ? F13 P10 F14 90.06(10) . . ? F11 P10 F12 90.12(9) . . ? F13 P10 F12 179.57(9) . . ? F14 P10 F12 90.34(9) . . ? F11 P10 F15 178.29(10) . . ? F13 P10 F15 91.28(13) . . ? F14 P10 F15 89.45(10) . . ? F12 P10 F15 88.58(10) . . ? F11 P10 F10 90.35(10) . . ? F13 P10 F10 90.44(9) . . ? F14 P10 F10 177.93(11) . . ? F12 P10 F10 89.15(8) . . ? F15 P10 F10 88.53(10) . . ? Cl1 C100 Cl2 112.2(2) . . ? Cl1 C100 H10B 109.2 . . ? Cl2 C100 H10B 109.2 . . ? Cl1 C100 H10C 109.2 . . ? Cl2 C100 H10C 109.2 . . ? H10B C100 H10C 107.9 . . ? O200 O200 C202 111.6(4) 2_665 . ? C204 C202 O200 104.0(5) . . ? C204 C202 H20H 111.0 . . ? O200 C202 H20H 111.0 . . ? C204 C202 H20I 111.0 . . ? O200 C202 H20I 111.0 . . ? H20H C202 H20I 109.0 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.105 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.068 # Attachment 'Cu(phen)(dppe).CIF' data_3tCu(phen)(dppe) _database_code_depnum_ccdc_archive 'CCDC 796693' #TrackingRef 'Cu(phen)(dppe).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C38 H32 Cu N2 P2), C4 H10 O, 2(F6 P), C H2 Cl2' _chemical_formula_sum 'C81 H76 Cl2 Cu2 F12 N4 O P6' _chemical_formula_weight 1733.28 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5635(17) _cell_length_b 13.0399(17) _cell_length_c 15.119(2) _cell_angle_alpha 112.413(10) _cell_angle_beta 98.097(11) _cell_angle_gamma 91.294(11) _cell_volume 2079.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9507 _cell_measurement_theta_min 5.61 _cell_measurement_theta_max 62.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9072 _exptl_absorpt_correction_T_max 0.9774 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41833 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7716 _reflns_number_gt 6781 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0632P)^2^+2.6222P] 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 7716 _refine_ls_number_parameters 507 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.019 _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 0.37582(3) 0.16884(3) 0.25566(2) 0.02000(12) Uani 1 1 d . . . P1 P 0.53682(7) 0.23297(6) 0.36905(5) 0.01930(17) Uani 1 1 d . . . P2 P 0.26052(7) 0.26005(7) 0.36247(6) 0.02223(18) Uani 1 1 d . . . C1 C 0.4809(3) 0.3472(3) 0.4644(2) 0.0255(7) Uani 1 1 d . . . H1A H 0.5365 0.3698 0.5259 0.031 Uiso 1 1 calc R . . H1B H 0.4742 0.4123 0.4460 0.031 Uiso 1 1 calc R . . C2 C 0.3608(3) 0.3101(3) 0.4786(2) 0.0279(7) Uani 1 1 d . . . H2A H 0.3289 0.3733 0.5269 0.034 Uiso 1 1 calc R . . H2B H 0.3687 0.2498 0.5032 0.034 Uiso 1 1 calc R . . C3 C 0.6631(3) 0.2995(3) 0.3459(2) 0.0226(6) Uani 1 1 d . . . C4 C 0.7721(3) 0.2560(3) 0.3456(2) 0.0283(7) Uani 1 1 d . . . H4A H 0.7841 0.1948 0.3644 0.034 Uiso 1 1 calc R . . C5 C 0.8631(3) 0.3020(4) 0.3180(3) 0.0385(8) Uani 1 1 d . . . H5A H 0.9373 0.2723 0.3180 0.046 Uiso 1 1 calc R . . C6 C 0.8463(3) 0.3907(4) 0.2906(3) 0.0406(9) Uani 1 1 d . . . H6A H 0.9088 0.4215 0.2713 0.049 Uiso 1 1 calc R . . C7 C 0.7391(4) 0.4348(3) 0.2910(3) 0.0371(8) Uani 1 1 d . . . H7A H 0.7279 0.4964 0.2727 0.044 Uiso 1 1 calc R . . C8 C 0.6475(3) 0.3892(3) 0.3182(2) 0.0297(7) Uani 1 1 d . . . H8A H 0.5735 0.4194 0.3178 0.036 Uiso 1 1 calc R . . C9 C 0.5988(3) 0.1449(3) 0.4289(2) 0.0224(6) Uani 1 1 d . . . C10 C 0.5784(3) 0.0297(3) 0.3812(3) 0.0298(7) Uani 1 1 d . . . H10A H 0.5316 -0.0010 0.3188 0.036 Uiso 1 1 calc R . . C11 C 0.6256(4) -0.0406(3) 0.4235(3) 0.0391(9) Uani 1 1 d . . . H11A H 0.6113 -0.1190 0.3904 0.047 Uiso 1 1 calc R . . C12 C 0.6934(3) 0.0042(3) 0.5143(3) 0.0367(8) Uani 1 1 d . . . H12A H 0.7263 -0.0435 0.5437 0.044 Uiso 1 1 calc R . . C13 C 0.7136(3) 0.1182(3) 0.5626(3) 0.0328(8) Uani 1 1 d . . . H13A H 0.7598 0.1485 0.6253 0.039 Uiso 1 1 calc R . . C14 C 0.6672(3) 0.1886(3) 0.5204(2) 0.0276(7) Uani 1 1 d . . . H14A H 0.6820 0.2669 0.5539 0.033 Uiso 1 1 calc R . . C15 C 0.1399(3) 0.1836(3) 0.3825(3) 0.0307(7) Uani 1 1 d . . . C16 C 0.0832(3) 0.0933(3) 0.3038(3) 0.0414(9) Uani 1 1 d . . . H16A H 0.1072 0.0743 0.2424 0.050 Uiso 1 1 calc R . . C17 C -0.0089(4) 0.0300(4) 0.3138(4) 0.0559(12) Uani 1 1 d . . . H17A H -0.0473 -0.0320 0.2592 0.067 Uiso 1 1 calc R . . C18 C -0.0444(4) 0.0569(4) 0.4026(4) 0.0587(14) Uani 1 1 d . . . H18A H -0.1073 0.0139 0.4095 0.070 Uiso 1 1 calc R . . C19 C 0.0109(4) 0.1451(4) 0.4799(4) 0.0508(12) Uani 1 1 d . . . H19A H -0.0137 0.1634 0.5411 0.061 Uiso 1 1 calc R . . C20 C 0.1033(4) 0.2098(4) 0.4715(3) 0.0404(9) Uani 1 1 d . . . H20A H 0.1409 0.2715 0.5266 0.049 Uiso 1 1 calc R . . C21 C 0.1995(3) 0.3852(3) 0.3555(2) 0.0248(6) Uani 1 1 d . . . C22 C 0.1984(3) 0.4015(3) 0.2702(3) 0.0377(8) Uani 1 1 d . . . H22A H 0.2284 0.3477 0.2179 0.045 Uiso 1 1 calc R . . C23 C 0.1544(4) 0.4950(4) 0.2598(4) 0.0482(11) Uani 1 1 d . . . H23A H 0.1541 0.5052 0.2008 0.058 Uiso 1 1 calc R . . C24 C 0.1111(3) 0.5732(3) 0.3357(4) 0.0444(10) Uani 1 1 d . . . H24A H 0.0813 0.6377 0.3292 0.053 Uiso 1 1 calc R . . C25 C 0.1110(4) 0.5579(3) 0.4205(3) 0.0455(10) Uani 1 1 d . . . H25A H 0.0805 0.6118 0.4724 0.055 Uiso 1 1 calc R . . C26 C 0.1549(3) 0.4648(3) 0.4309(3) 0.0366(8) Uani 1 1 d . . . H26A H 0.1547 0.4551 0.4900 0.044 Uiso 1 1 calc R . . N1 N 0.3847(2) 0.1842(2) 0.12726(18) 0.0206(5) Uani 1 1 d . . . N2 N 0.3333(2) 0.0055(2) 0.16688(19) 0.0235(5) Uani 1 1 d . . . C27 C 0.4136(3) 0.2725(3) 0.1090(2) 0.0253(6) Uani 1 1 d . . . H27A H 0.4293 0.3428 0.1616 0.030 Uiso 1 1 calc R . . C28 C 0.4220(3) 0.2667(3) 0.0158(3) 0.0313(7) Uani 1 1 d . . . H28A H 0.4437 0.3317 0.0058 0.038 Uiso 1 1 calc R . . C29 C 0.3987(3) 0.1666(3) -0.0604(2) 0.0306(7) Uani 1 1 d . . . H29A H 0.4032 0.1613 -0.1242 0.037 Uiso 1 1 calc R . . C30 C 0.3682(3) 0.0714(3) -0.0443(2) 0.0249(6) Uani 1 1 d . . . C31 C 0.3631(3) 0.0843(3) 0.0517(2) 0.0206(6) Uani 1 1 d . . . C32 C 0.3342(3) -0.0110(3) 0.0724(2) 0.0212(6) Uani 1 1 d . . . C33 C 0.3097(3) -0.1158(3) -0.0031(2) 0.0265(7) Uani 1 1 d . . . C34 C 0.2818(3) -0.2067(3) 0.0208(3) 0.0348(8) Uani 1 1 d . . . H34A H 0.2644 -0.2793 -0.0285 0.042 Uiso 1 1 calc R . . C35 C 0.2800(3) -0.1895(3) 0.1157(3) 0.0364(8) Uani 1 1 d . . . H35A H 0.2606 -0.2497 0.1330 0.044 Uiso 1 1 calc R . . C36 C 0.3070(3) -0.0826(3) 0.1863(3) 0.0310(7) Uani 1 1 d . . . H36A H 0.3067 -0.0720 0.2520 0.037 Uiso 1 1 calc R . . C37 C 0.3434(3) -0.0374(3) -0.1194(2) 0.0337(8) Uani 1 1 d . . . H37A H 0.3463 -0.0469 -0.1846 0.040 Uiso 1 1 calc R . . C38 C 0.3159(3) -0.1267(3) -0.0997(2) 0.0329(8) Uani 1 1 d . . . H38A H 0.3004 -0.1980 -0.1511 0.039 Uiso 1 1 calc R . . P10 P 0.52778(10) 0.38477(8) 0.78363(7) 0.0397(2) Uani 1 1 d . . . F10 F 0.6043(4) 0.2897(3) 0.7290(2) 0.0954(14) Uani 1 1 d . . . F11 F 0.6385(3) 0.4421(3) 0.8627(2) 0.0748(9) Uani 1 1 d . . . F12 F 0.4153(3) 0.3316(2) 0.7028(2) 0.0806(10) Uani 1 1 d . . . F13 F 0.4902(3) 0.3172(3) 0.8433(2) 0.0781(10) Uani 1 1 d . . . F14 F 0.4534(2) 0.4840(2) 0.83931(19) 0.0534(6) Uani 1 1 d . . . F15 F 0.5631(3) 0.4542(2) 0.7222(2) 0.0638(8) Uani 1 1 d . . . C100 C -0.2037(10) 0.6181(12) 0.1214(12) 0.087(4) Uani 0.50 1 d PU . . H10B H -0.2190 0.6408 0.0656 0.104 Uiso 0.50 1 calc PR . . H10C H -0.2804 0.5938 0.1321 0.104 Uiso 0.50 1 calc PR . . Cl1 Cl -0.1492(5) 0.7267(4) 0.2160(6) 0.159(3) Uani 0.50 1 d P . . Cl2 Cl -0.1199(3) 0.5028(4) 0.0887(4) 0.1145(14) Uani 0.50 1 d P . . O200 O -0.0083(5) -0.0364(6) 0.0217(4) 0.0894(17) Uani 0.50 1 d P . 1 C200 C -0.0404(7) -0.1476(8) -0.0515(6) 0.100(2) Uani 0.50 1 d P A 1 H20B H -0.1116 -0.1497 -0.0972 0.120 Uiso 0.50 1 calc PR A 1 H20C H 0.0242 -0.1762 -0.0884 0.120 Uiso 0.50 1 calc PR A 1 C201 C -0.0613(11) -0.2083(12) 0.0051(10) 0.081(3) Uani 0.50 1 d P A 1 H20D H 0.0127 -0.2127 0.0435 0.121 Uiso 0.50 1 calc PR A 1 H20E H -0.0951 -0.2836 -0.0374 0.121 Uiso 0.50 1 calc PR A 1 H20F H -0.1162 -0.1709 0.0486 0.121 Uiso 0.50 1 calc PR A 1 C20' C -0.0083(5) -0.0364(6) 0.0217(4) 0.0894(17) Uani 0.50 1 d P . 2 H20G H -0.0711 -0.0129 0.0617 0.107 Uiso 0.50 1 calc PR . 2 H20H H 0.0646 -0.0362 0.0648 0.107 Uiso 0.50 1 calc PR . 2 C21' C -0.0404(7) -0.1476(8) -0.0515(6) 0.100(2) Uani 0.50 1 d P B 2 H21A H -0.1145 -0.1483 -0.0922 0.151 Uiso 0.50 1 calc PR B 2 H21B H -0.0496 -0.1998 -0.0199 0.151 Uiso 0.50 1 calc PR B 2 H21C H 0.0212 -0.1700 -0.0919 0.151 Uiso 0.50 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 Cu1 0.0240(2) 0.0196(2) 0.01470(19) 0.00498(14) 0.00294(14) 0.00024(14) P1 0.0217(4) 0.0165(4) 0.0176(4) 0.0047(3) 0.0018(3) 0.0019(3) P2 0.0228(4) 0.0259(4) 0.0201(4) 0.0103(3) 0.0058(3) 0.0059(3) C1 0.0318(17) 0.0183(15) 0.0207(15) 0.0021(12) 0.0009(13) 0.0052(12) C2 0.0293(17) 0.0357(18) 0.0193(15) 0.0101(13) 0.0060(13) 0.0105(14) C3 0.0244(15) 0.0214(15) 0.0186(14) 0.0056(12) -0.0005(12) -0.0016(12) C4 0.0267(16) 0.0329(18) 0.0254(16) 0.0127(14) 0.0000(13) 0.0022(13) C5 0.0250(17) 0.054(2) 0.036(2) 0.0190(18) 0.0018(15) -0.0003(16) C6 0.0319(19) 0.052(2) 0.0348(19) 0.0163(18) -0.0007(15) -0.0190(17) C7 0.046(2) 0.0317(19) 0.0336(19) 0.0167(15) -0.0025(16) -0.0116(16) C8 0.0326(18) 0.0254(16) 0.0282(17) 0.0095(14) -0.0010(14) -0.0036(13) C9 0.0236(15) 0.0224(15) 0.0236(15) 0.0108(12) 0.0061(12) 0.0029(12) C10 0.0339(18) 0.0200(16) 0.0351(18) 0.0107(14) 0.0037(14) 0.0028(13) C11 0.046(2) 0.0232(17) 0.052(2) 0.0179(17) 0.0107(18) 0.0054(15) C12 0.039(2) 0.037(2) 0.046(2) 0.0288(18) 0.0101(17) 0.0112(16) C13 0.0337(18) 0.040(2) 0.0305(17) 0.0204(16) 0.0047(14) 0.0060(15) C14 0.0306(17) 0.0279(17) 0.0248(16) 0.0119(13) 0.0017(13) 0.0008(13) C15 0.0285(17) 0.0323(18) 0.043(2) 0.0247(16) 0.0140(15) 0.0119(14) C16 0.034(2) 0.041(2) 0.054(2) 0.0223(19) 0.0133(18) 0.0026(16) C17 0.041(2) 0.042(2) 0.091(4) 0.031(2) 0.015(2) -0.0043(19) C18 0.041(2) 0.057(3) 0.108(4) 0.057(3) 0.034(3) 0.013(2) C19 0.048(2) 0.059(3) 0.076(3) 0.049(3) 0.038(2) 0.025(2) C20 0.042(2) 0.046(2) 0.051(2) 0.0322(19) 0.0247(18) 0.0209(18) C21 0.0201(15) 0.0255(16) 0.0283(16) 0.0109(13) 0.0013(12) -0.0002(12) C22 0.0352(19) 0.048(2) 0.046(2) 0.0301(19) 0.0188(17) 0.0146(17) C23 0.041(2) 0.058(3) 0.073(3) 0.052(3) 0.019(2) 0.0142(19) C24 0.0308(19) 0.0273(19) 0.076(3) 0.025(2) -0.0025(19) 0.0013(15) C25 0.039(2) 0.0288(19) 0.047(2) -0.0036(17) -0.0113(18) 0.0100(16) C26 0.038(2) 0.0339(19) 0.0273(17) 0.0036(15) -0.0046(15) 0.0089(15) N1 0.0235(13) 0.0190(12) 0.0180(12) 0.0060(10) 0.0028(10) 0.0001(10) N2 0.0249(13) 0.0235(13) 0.0213(13) 0.0088(11) 0.0013(10) -0.0011(10) C27 0.0303(17) 0.0222(15) 0.0246(16) 0.0104(13) 0.0048(13) 0.0012(12) C28 0.0391(19) 0.0304(18) 0.0308(18) 0.0180(15) 0.0088(15) 0.0014(15) C29 0.0392(19) 0.0350(19) 0.0203(15) 0.0126(14) 0.0080(14) 0.0021(15) C30 0.0273(16) 0.0284(17) 0.0183(15) 0.0077(13) 0.0045(12) 0.0030(13) C31 0.0207(14) 0.0220(15) 0.0170(14) 0.0055(12) 0.0026(11) 0.0031(11) C32 0.0189(14) 0.0217(15) 0.0217(15) 0.0073(12) 0.0022(11) 0.0015(11) C33 0.0251(16) 0.0229(16) 0.0261(16) 0.0044(13) 0.0020(13) 0.0007(12) C34 0.041(2) 0.0194(16) 0.0372(19) 0.0046(14) 0.0029(16) -0.0032(14) C35 0.043(2) 0.0239(17) 0.044(2) 0.0173(16) 0.0023(17) -0.0049(15) C36 0.0370(19) 0.0279(17) 0.0309(17) 0.0163(14) 0.0020(14) -0.0023(14) C37 0.042(2) 0.0369(19) 0.0170(15) 0.0039(14) 0.0059(14) 0.0021(15) C38 0.0388(19) 0.0282(18) 0.0218(16) -0.0008(13) 0.0046(14) 0.0000(14) P10 0.0623(7) 0.0306(5) 0.0323(5) 0.0157(4) 0.0159(5) 0.0095(5) F10 0.175(4) 0.074(2) 0.072(2) 0.0441(18) 0.073(2) 0.081(2) F11 0.0583(18) 0.099(2) 0.0669(19) 0.0348(18) 0.0004(15) 0.0101(16) F12 0.121(3) 0.0463(16) 0.0566(17) 0.0131(14) -0.0197(18) -0.0180(17) F13 0.114(3) 0.076(2) 0.081(2) 0.0618(19) 0.041(2) 0.0170(19) F14 0.0601(16) 0.0445(14) 0.0518(15) 0.0123(12) 0.0147(12) 0.0117(12) F15 0.085(2) 0.0616(17) 0.0707(18) 0.0471(15) 0.0303(16) 0.0195(15) C100 0.060(6) 0.109(9) 0.150(11) 0.106(9) 0.043(7) 0.021(6) Cl1 0.104(3) 0.089(3) 0.261(7) 0.062(4) -0.023(4) -0.001(2) Cl2 0.068(2) 0.094(3) 0.173(4) 0.053(3) -0.012(2) 0.0098(18) O200 0.073(3) 0.125(5) 0.061(3) 0.027(3) 0.007(3) 0.019(3) C200 0.076(4) 0.122(6) 0.102(6) 0.042(5) 0.011(4) 0.020(4) C201 0.059(7) 0.097(10) 0.091(9) 0.044(8) 0.003(6) 0.011(6) C20' 0.073(3) 0.125(5) 0.061(3) 0.027(3) 0.007(3) 0.019(3) C21' 0.076(4) 0.122(6) 0.102(6) 0.042(5) 0.011(4) 0.020(4) _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 N2 2.041(3) . ? Cu1 N1 2.042(2) . ? Cu1 P2 2.2390(9) . ? Cu1 P1 2.2453(9) . ? P1 C9 1.816(3) . ? P1 C3 1.824(3) . ? P1 C1 1.839(3) . ? P2 C15 1.822(3) . ? P2 C21 1.827(3) . ? P2 C2 1.836(3) . ? C1 C2 1.531(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.393(5) . ? C3 C8 1.393(5) . ? C4 C5 1.389(5) . ? C4 H4A 0.9500 . ? C5 C6 1.378(6) . ? C5 H5A 0.9500 . ? C6 C7 1.378(6) . ? C6 H6A 0.9500 . ? C7 C8 1.388(5) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 C14 1.390(5) . ? C9 C10 1.393(5) . ? C10 C11 1.385(5) . ? C10 H10A 0.9500 . ? C11 C12 1.380(6) . ? C11 H11A 0.9500 . ? C12 C13 1.380(6) . ? C12 H12A 0.9500 . ? C13 C14 1.382(5) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.381(6) . ? C15 C20 1.387(5) . ? C16 C17 1.392(6) . ? C16 H16A 0.9500 . ? C17 C18 1.377(8) . ? C17 H17A 0.9500 . ? C18 C19 1.352(8) . ? C18 H18A 0.9500 . ? C19 C20 1.395(6) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.382(5) . ? C21 C26 1.389(5) . ? C22 C23 1.387(5) . ? C22 H22A 0.9500 . ? C23 C24 1.377(7) . ? C23 H23A 0.9500 . ? C24 C25 1.370(6) . ? C24 H24A 0.9500 . ? C25 C26 1.382(5) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? N1 C27 1.328(4) . ? N1 C31 1.355(4) . ? N2 C36 1.330(4) . ? N2 C32 1.362(4) . ? C27 C28 1.400(5) . ? C27 H27A 0.9500 . ? C28 C29 1.362(5) . ? C28 H28A 0.9500 . ? C29 C30 1.399(5) . ? C29 H29A 0.9500 . ? C30 C31 1.406(4) . ? C30 C37 1.430(5) . ? C31 C32 1.436(4) . ? C32 C33 1.398(4) . ? C33 C34 1.407(5) . ? C33 C38 1.425(5) . ? C34 C35 1.368(5) . ? C34 H34A 0.9500 . ? C35 C36 1.390(5) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.350(5) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? P10 F11 1.572(3) . ? P10 F10 1.573(3) . ? P10 F13 1.574(3) . ? P10 F12 1.591(3) . ? P10 F14 1.596(3) . ? P10 F15 1.606(3) . ? C100 Cl1 1.615(17) . ? C100 Cl2 1.755(13) . ? C100 H10B 0.9900 . ? C100 H10C 0.9900 . ? O200 O200 1.367(12) 2 ? O200 C200 1.450(10) . ? C200 C201 1.409(15) . ? C200 H20B 0.9900 . ? C200 H20C 0.9900 . ? C201 H20D 0.9800 . ? C201 H20E 0.9800 . ? C201 H20F 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 N2 Cu1 N1 82.45(10) . . ? N2 Cu1 P2 120.45(8) . . ? N1 Cu1 P2 125.60(8) . . ? N2 Cu1 P1 124.69(8) . . ? N1 Cu1 P1 115.95(8) . . ? P2 Cu1 P1 91.57(3) . . ? C9 P1 C3 104.80(14) . . ? C9 P1 C1 104.87(15) . . ? C3 P1 C1 103.76(15) . . ? C9 P1 Cu1 119.55(11) . . ? C3 P1 Cu1 120.28(10) . . ? C1 P1 Cu1 101.28(11) . . ? C15 P2 C21 104.96(15) . . ? C15 P2 C2 103.87(16) . . ? C21 P2 C2 104.61(15) . . ? C15 P2 Cu1 119.70(12) . . ? C21 P2 Cu1 118.69(11) . . ? C2 P2 Cu1 102.95(11) . . ? C2 C1 P1 110.2(2) . . ? C2 C1 H1A 109.6 . . ? P1 C1 H1A 109.6 . . ? C2 C1 H1B 109.6 . . ? P1 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? C1 C2 P2 109.5(2) . . ? C1 C2 H2A 109.8 . . ? P2 C2 H2A 109.8 . . ? C1 C2 H2B 109.8 . . ? P2 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C8 119.0(3) . . ? C4 C3 P1 121.6(2) . . ? C8 C3 P1 119.1(2) . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C6 C5 C4 120.3(4) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C7 C6 C5 120.1(3) . . ? C7 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? C6 C7 C8 120.0(3) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C7 C8 C3 120.5(3) . . ? C7 C8 H8A 119.7 . . ? C3 C8 H8A 119.7 . . ? C14 C9 C10 118.8(3) . . ? C14 C9 P1 122.1(2) . . ? C10 C9 P1 119.0(2) . . ? C11 C10 C9 120.9(3) . . ? C11 C10 H10A 119.5 . . ? C9 C10 H10A 119.5 . . ? C12 C11 C10 119.4(3) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? C11 C12 C13 120.2(3) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C12 C13 C14 120.5(3) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C13 C14 C9 120.1(3) . . ? C13 C14 H14A 120.0 . . ? C9 C14 H14A 120.0 . . ? C16 C15 C20 118.7(4) . . ? C16 C15 P2 117.3(3) . . ? C20 C15 P2 124.0(3) . . ? C15 C16 C17 120.6(4) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C18 C17 C16 120.1(5) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C19 C18 C17 119.5(4) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? C18 C19 C20 121.3(4) . . ? C18 C19 H19A 119.3 . . ? C20 C19 H19A 119.3 . . ? C15 C20 C19 119.8(4) . . ? C15 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C22 C21 C26 118.4(3) . . ? C22 C21 P2 117.8(3) . . ? C26 C21 P2 123.8(3) . . ? C21 C22 C23 121.1(4) . . ? C21 C22 H22A 119.5 . . ? C23 C22 H22A 119.5 . . ? C24 C23 C22 119.5(4) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C25 C24 C23 120.1(3) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C25 C26 C21 120.5(4) . . ? C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? C27 N1 C31 117.9(3) . . ? C27 N1 Cu1 130.6(2) . . ? C31 N1 Cu1 111.4(2) . . ? C36 N2 C32 117.6(3) . . ? C36 N2 Cu1 131.2(2) . . ? C32 N2 Cu1 111.1(2) . . ? N1 C27 C28 123.1(3) . . ? N1 C27 H27A 118.5 . . ? C28 C27 H27A 118.5 . . ? C29 C28 C27 119.0(3) . . ? C29 C28 H28A 120.5 . . ? C27 C28 H28A 120.5 . . ? C28 C29 C30 119.8(3) . . ? C28 C29 H29A 120.1 . . ? C30 C29 H29A 120.1 . . ? C29 C30 C31 117.5(3) . . ? C29 C30 C37 123.8(3) . . ? C31 C30 C37 118.6(3) . . ? N1 C31 C30 122.7(3) . . ? N1 C31 C32 117.5(3) . . ? C30 C31 C32 119.8(3) . . ? N2 C32 C33 122.7(3) . . ? N2 C32 C31 117.5(3) . . ? C33 C32 C31 119.8(3) . . ? C32 C33 C34 117.8(3) . . ? C32 C33 C38 119.2(3) . . ? C34 C33 C38 123.0(3) . . ? C35 C34 C33 119.3(3) . . ? C35 C34 H34A 120.3 . . ? C33 C34 H34A 120.3 . . ? C34 C35 C36 119.1(3) . . ? C34 C35 H35A 120.4 . . ? C36 C35 H35A 120.4 . . ? N2 C36 C35 123.5(3) . . ? N2 C36 H36A 118.3 . . ? C35 C36 H36A 118.3 . . ? C38 C37 C30 121.4(3) . . ? C38 C37 H37A 119.3 . . ? C30 C37 H37A 119.3 . . ? C37 C38 C33 121.1(3) . . ? C37 C38 H38A 119.5 . . ? C33 C38 H38A 119.5 . . ? F11 P10 F10 89.1(2) . . ? F11 P10 F13 91.1(2) . . ? F10 P10 F13 91.06(18) . . ? F11 P10 F12 177.50(18) . . ? F10 P10 F12 92.3(2) . . ? F13 P10 F12 90.9(2) . . ? F11 P10 F14 89.70(17) . . ? F10 P10 F14 178.2(2) . . ? F13 P10 F14 90.30(17) . . ? F12 P10 F14 88.90(18) . . ? F11 P10 F15 89.86(18) . . ? F10 P10 F15 89.83(17) . . ? F13 P10 F15 178.69(19) . . ? F12 P10 F15 88.05(18) . . ? F14 P10 F15 88.84(15) . . ? Cl1 C100 Cl2 117.3(8) . . ? Cl1 C100 H10B 108.0 . . ? Cl2 C100 H10B 108.0 . . ? Cl1 C100 H10C 108.0 . . ? Cl2 C100 H10C 108.0 . . ? H10B C100 H10C 107.2 . . ? O200 O200 C200 109.9(7) 2 . ? C201 C200 O200 101.9(8) . . ? C201 C200 H20B 111.4 . . ? O200 C200 H20B 111.4 . . ? C201 C200 H20C 111.4 . . ? O200 C200 H20C 111.4 . . ? H20B C200 H20C 109.2 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.970 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.078 # Attachment 'PSSP.CIF' data_esc24 _database_code_depnum_ccdc_archive 'CCDC 796694' #TrackingRef 'PSSP.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H28 O2 P2 S2' _chemical_formula_sum 'C36 H28 O2 P2 S2' _chemical_formula_weight 618.66 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.763(3) _cell_length_b 5.9420(12) _cell_length_c 30.238(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.51(3) _cell_angle_gamma 90.00 _cell_volume 3006.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.317 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9540 _exptl_absorpt_correction_T_max 0.9540 _exptl_absorpt_process_details '(Blessing, 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24155 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 28.50 _reflns_number_total 3760 _reflns_number_gt 3464 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0387P)^2^+2.4058P] 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 3760 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 S1 S 0.01215(2) -0.02618(6) 0.217399(10) 0.02639(9) Uani 1 1 d . . . P1 P 0.035887(19) 0.17079(5) 0.121308(10) 0.02220(9) Uani 1 1 d . . . O1 O 0.03851(6) -0.07932(17) 0.12161(3) 0.0315(2) Uani 1 1 d . . . C1 C 0.07972(7) 0.2043(2) 0.21186(4) 0.0232(2) Uani 1 1 d . . . C2 C 0.08982(7) 0.2905(2) 0.16914(4) 0.0231(2) Uani 1 1 d . . . C3 C 0.14259(9) 0.4683(3) 0.16451(5) 0.0314(3) Uani 1 1 d . . . H3A H 0.1497 0.5281 0.1359 0.038 Uiso 1 1 calc R . . C4 C 0.18499(9) 0.5596(3) 0.20102(5) 0.0363(3) Uani 1 1 d . . . H4A H 0.2211 0.6804 0.1974 0.044 Uiso 1 1 calc R . . C5 C 0.17444(9) 0.4742(3) 0.24268(5) 0.0342(3) Uani 1 1 d . . . H5A H 0.2033 0.5370 0.2677 0.041 Uiso 1 1 calc R . . C6 C 0.12214(8) 0.2977(3) 0.24830(4) 0.0299(3) Uani 1 1 d . . . H6A H 0.1152 0.2402 0.2771 0.036 Uiso 1 1 calc R . . C7 C -0.06406(7) 0.2806(2) 0.12165(4) 0.0249(2) Uani 1 1 d . . . C8 C -0.08095(9) 0.4897(2) 0.13930(5) 0.0307(3) Uani 1 1 d . . . H8A H -0.0390 0.5828 0.1514 0.037 Uiso 1 1 calc R . . C9 C -0.16000(10) 0.5615(3) 0.13910(5) 0.0415(4) Uani 1 1 d . . . H9A H -0.1723 0.7038 0.1513 0.050 Uiso 1 1 calc R . . C10 C -0.22054(9) 0.4264(4) 0.12122(6) 0.0476(5) Uani 1 1 d . . . H10A H -0.2745 0.4750 0.1217 0.057 Uiso 1 1 calc R . . C11 C -0.20352(9) 0.2215(4) 0.10269(6) 0.0466(4) Uani 1 1 d . . . H11A H -0.2455 0.1314 0.0897 0.056 Uiso 1 1 calc R . . C12 C -0.12552(9) 0.1471(3) 0.10307(5) 0.0341(3) Uani 1 1 d . . . H12A H -0.1138 0.0049 0.0907 0.041 Uiso 1 1 calc R . . C13 C 0.07717(7) 0.2801(2) 0.07191(4) 0.0247(2) Uani 1 1 d . . . C14 C 0.06508(9) 0.4983(2) 0.05599(4) 0.0303(3) Uani 1 1 d . . . H14A H 0.0367 0.6044 0.0725 0.036 Uiso 1 1 calc R . . C15 C 0.09497(10) 0.5594(3) 0.01578(5) 0.0371(3) Uani 1 1 d . . . H15A H 0.0867 0.7080 0.0048 0.045 Uiso 1 1 calc R . . C16 C 0.13647(10) 0.4062(3) -0.00831(5) 0.0398(4) Uani 1 1 d . . . H16A H 0.1564 0.4494 -0.0358 0.048 Uiso 1 1 calc R . . C17 C 0.14911(9) 0.1906(3) 0.00748(5) 0.0388(3) Uani 1 1 d . . . H17A H 0.1781 0.0857 -0.0090 0.047 Uiso 1 1 calc R . . C18 C 0.11931(8) 0.1273(3) 0.04748(4) 0.0306(3) Uani 1 1 d . . . H18A H 0.1278 -0.0216 0.0582 0.037 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 S1 0.03603(18) 0.02498(16) 0.01880(15) -0.00173(11) 0.00697(11) -0.00225(12) P1 0.02693(16) 0.02327(16) 0.01665(14) -0.00108(11) 0.00322(11) -0.00088(11) O1 0.0465(6) 0.0241(5) 0.0245(5) -0.0008(4) 0.0077(4) 0.0007(4) C1 0.0234(5) 0.0262(6) 0.0203(5) -0.0002(4) 0.0037(4) 0.0030(5) C2 0.0230(5) 0.0273(6) 0.0192(5) -0.0005(4) 0.0028(4) 0.0006(5) C3 0.0324(7) 0.0398(8) 0.0221(6) 0.0028(5) 0.0020(5) -0.0088(6) C4 0.0342(7) 0.0450(8) 0.0293(7) 0.0008(6) -0.0005(5) -0.0141(6) C5 0.0335(7) 0.0444(8) 0.0241(6) -0.0024(6) -0.0038(5) -0.0068(6) C6 0.0310(6) 0.0390(7) 0.0195(5) 0.0008(5) 0.0007(5) -0.0013(6) C7 0.0264(6) 0.0297(6) 0.0189(5) 0.0035(5) 0.0036(4) -0.0032(5) C8 0.0333(7) 0.0312(7) 0.0282(6) 0.0036(5) 0.0069(5) 0.0030(5) C9 0.0432(8) 0.0477(9) 0.0351(8) 0.0152(7) 0.0149(6) 0.0164(7) C10 0.0276(7) 0.0805(13) 0.0354(8) 0.0245(8) 0.0082(6) 0.0115(8) C11 0.0285(7) 0.0761(13) 0.0352(8) 0.0134(8) 0.0007(6) -0.0130(8) C12 0.0329(7) 0.0431(8) 0.0263(6) 0.0043(6) 0.0011(5) -0.0107(6) C13 0.0259(6) 0.0309(6) 0.0173(5) -0.0009(5) 0.0022(4) -0.0021(5) C14 0.0388(7) 0.0301(7) 0.0223(6) -0.0005(5) 0.0041(5) -0.0021(6) C15 0.0499(9) 0.0361(8) 0.0256(7) 0.0041(6) 0.0039(6) -0.0091(6) C16 0.0441(8) 0.0527(9) 0.0237(6) 0.0008(6) 0.0105(6) -0.0121(7) C17 0.0387(8) 0.0517(9) 0.0274(7) -0.0055(6) 0.0126(6) 0.0001(7) C18 0.0325(7) 0.0355(7) 0.0244(6) -0.0020(5) 0.0056(5) 0.0019(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 S1 C1 1.7915(14) . ? S1 S1 2.0375(7) 2 ? P1 O1 1.4868(11) . ? P1 C7 1.7986(14) . ? P1 C2 1.8042(13) . ? P1 C13 1.8052(13) . ? C1 C6 1.3898(18) . ? C1 C2 1.4095(17) . ? C2 C3 1.3902(19) . ? C3 C4 1.387(2) . ? C3 H3A 0.9500 . ? C4 C5 1.380(2) . ? C4 H4A 0.9500 . ? C5 C6 1.384(2) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.3888(19) . ? C7 C12 1.3910(19) . ? C8 C9 1.392(2) . ? C8 H8A 0.9500 . ? C9 C10 1.378(3) . ? C9 H9A 0.9500 . ? C10 C11 1.377(3) . ? C10 H10A 0.9500 . ? C11 C12 1.380(2) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.3905(19) . ? C13 C14 1.3932(19) . ? C14 C15 1.3913(19) . ? C14 H14A 0.9500 . ? C15 C16 1.380(2) . ? C15 H15A 0.9500 . ? C16 C17 1.379(3) . ? C16 H16A 0.9500 . ? C17 C18 1.3886(19) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 S1 104.80(5) . 2 ? O1 P1 C7 112.94(6) . . ? O1 P1 C2 112.08(6) . . ? C7 P1 C2 105.89(6) . . ? O1 P1 C13 110.62(6) . . ? C7 P1 C13 106.18(6) . . ? C2 P1 C13 108.83(6) . . ? C6 C1 C2 119.80(12) . . ? C6 C1 S1 121.79(10) . . ? C2 C1 S1 118.40(10) . . ? C3 C2 C1 118.77(12) . . ? C3 C2 P1 120.63(10) . . ? C1 C2 P1 120.59(10) . . ? C4 C3 C2 121.04(13) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C5 C4 C3 119.66(14) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 120.57(13) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C5 C6 C1 120.16(12) . . ? C5 C6 H6A 119.9 . . ? C1 C6 H6A 119.9 . . ? C8 C7 C12 120.14(13) . . ? C8 C7 P1 122.60(10) . . ? C12 C7 P1 117.26(11) . . ? C7 C8 C9 119.28(15) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? C10 C9 C8 120.09(17) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C11 C10 C9 120.57(15) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 C12 119.98(16) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C7 119.92(16) . . ? C11 C12 H12A 120.0 . . ? C7 C12 H12A 120.0 . . ? C18 C13 C14 119.47(12) . . ? C18 C13 P1 115.94(11) . . ? C14 C13 P1 124.45(10) . . ? C15 C14 C13 119.50(14) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C16 C15 C14 120.59(15) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C17 C16 C15 120.13(14) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C16 C17 C18 119.83(14) . . ? C16 C17 H17A 120.1 . . ? C18 C17 H17A 120.1 . . ? C17 C18 C13 120.49(14) . . ? C17 C18 H18A 119.8 . . ? C13 C18 H18A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.339 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.044