# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_publication_text _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 #TrackingRef '- 2I_pub_new.cif' _audit_update_record ; 2012-05-18 # Formatted by publCIF ; _publ_contact_author_name 'Radoslaw Starosta' _publ_contact_author_address ;Faculty of Chemistry University of Wroclaw ul. F. Joliot-Curie 14 50-383 Wroclaw Poland ; _publ_contact_author_email radoslaw.starosta@chem.uni.wroc.pl loop_ _publ_author_name _publ_author_address R.Starosta ;Faculty of Chemistry, University of Wroclaw ul. F. Joliot-Curie 14 50-383 Wroclaw Poland ; B.Maciej ;Faculty of Chemistry University of Wroclaw ul. F. Joliot-Curie 14 50-383 Wroclaw Poland ; U.K.Komarnicka ;Faculty of Chemistry University of Wroclaw ul. F. Joliot-Curie 14 50-383 Wroclaw Poland ; P.Malgorzata ;Faculty of Chemistry University of Wroclaw ul. F. Joliot-Curie 14 50-383 Wroclaw Poland ; data_3sn _database_code_depnum_ccdc_archive 'CCDC 842342' #TrackingRef '- 2I_pub_new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; iodo-(2,9-dimetyl-1,10-phenanthroline-N,N')-(tris(thiomorpholinomethyl) phosphine-P)-copper(i) hydrate ; _chemical_name_common ; iodo-(2,9-dimetyl-1,10-phenanthroline-N,N')- (tris(thiomorpholinomethyl) phosphine-P)-copper(i) hydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C29 H42 Cu I N5 P S3, 0.20(H2 O)' _chemical_formula_sum 'C29 H42.40 Cu I N5 O0.20 P S3' _chemical_formula_weight 781.87 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' I I -0.4742 1.8119 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.2770(10) _cell_length_b 15.6610(10) _cell_length_c 19.109(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.660(10) _cell_angle_gamma 90.00 _cell_volume 3352.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5668 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 36.94 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 1.835 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7963 _exptl_absorpt_correction_T_max 0.8377 _exptl_absorpt_process_details 'Oxford Diffraction, CrysAlis 1.171.30' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65786 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 36.94 _reflns_number_total 15626 _reflns_number_gt 11159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, date)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, date)' _computing_data_reduction 'CrysAlis RED ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1999)' _computing_publication_material SHELXL-97 _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^)+(0.0400P)^2^+0.0000P] 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 15626 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _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 I1 I 0.525590(8) 0.266922(6) 0.176627(5) 0.02280(3) Uani 1 1 d . . . Cu1 Cu 0.407478(14) 0.407665(10) 0.202951(8) 0.01524(3) Uani 1 1 d . . . P1 P 0.38060(3) 0.43056(2) 0.314250(17) 0.01388(6) Uani 1 1 d . . . N41 N 0.26080(10) 0.40480(7) 0.12360(6) 0.01485(19) Uani 1 1 d . . . N42 N 0.45833(10) 0.50396(7) 0.13537(6) 0.0155(2) Uani 1 1 d . . . N11 N 0.58285(10) 0.38257(7) 0.40444(6) 0.0182(2) Uani 1 1 d . . . C51 C 0.27465(11) 0.45923(8) 0.06940(6) 0.0149(2) Uani 1 1 d . . . C48 C 0.50029(13) 0.62093(9) 0.03006(8) 0.0210(3) Uani 1 1 d . . . H48 H 0.5164 0.6600 -0.0057 0.025 Uiso 1 1 calc R . . C44 C 0.19114(12) 0.46575(9) 0.00881(7) 0.0180(2) Uani 1 1 d . . . C11 C 0.50338(12) 0.45490(9) 0.38552(7) 0.0196(2) Uani 1 1 d . . . H11A H 0.5512 0.5029 0.3701 0.024 Uiso 1 1 calc R . . H11B H 0.4679 0.4737 0.4280 0.024 Uiso 1 1 calc R . . C53 C 0.14641(13) 0.30125(9) 0.18201(7) 0.0226(3) Uani 1 1 d . . . H53A H 0.2202 0.2695 0.1962 0.034 Uiso 1 1 calc R . . H53B H 0.0809 0.2610 0.1693 0.034 Uiso 1 1 calc R . . H53C H 0.1274 0.3371 0.2212 0.034 Uiso 1 1 calc R . . C47 C 0.39581(12) 0.57106(8) 0.02173(7) 0.0177(2) Uani 1 1 d . . . C43 C 0.08971(12) 0.41260(9) 0.00554(7) 0.0206(3) Uani 1 1 d . . . H43 H 0.0315 0.4140 -0.0346 0.025 Uiso 1 1 calc R . . C52 C 0.37936(11) 0.51258(8) 0.07595(7) 0.0152(2) Uani 1 1 d . . . C12 C 0.63822(13) 0.38948(9) 0.47740(7) 0.0221(3) Uani 1 1 d . . . H12A H 0.5757 0.4017 0.5084 0.027 Uiso 1 1 calc R . . H12B H 0.6951 0.4379 0.4813 0.027 Uiso 1 1 calc R . . C41 C 0.16276(11) 0.35659(8) 0.11979(7) 0.0172(2) Uani 1 1 d . . . N31 N 0.18080(10) 0.53528(7) 0.28304(5) 0.01518(19) Uani 1 1 d . . . N21 N 0.26385(10) 0.36400(7) 0.42249(6) 0.0165(2) Uani 1 1 d . . . C33 C 0.10915(12) 0.58807(9) 0.16301(7) 0.0196(2) Uani 1 1 d . . . H33A H 0.0854 0.5293 0.1482 0.024 Uiso 1 1 calc R . . H33B H 0.1364 0.6176 0.1219 0.024 Uiso 1 1 calc R . . C32 C 0.21193(12) 0.58387(9) 0.22206(7) 0.0178(2) Uani 1 1 d . . . H32A H 0.2817 0.5569 0.2040 0.021 Uiso 1 1 calc R . . H32B H 0.2349 0.6426 0.2372 0.021 Uiso 1 1 calc R . . C36 C 0.08695(12) 0.57932(9) 0.31627(7) 0.0195(3) Uani 1 1 d . . . H36A H 0.1125 0.6386 0.3279 0.023 Uiso 1 1 calc R . . H36B H 0.0748 0.5500 0.3608 0.023 Uiso 1 1 calc R . . C42 C 0.07570(12) 0.35898(9) 0.06059(7) 0.0205(3) Uani 1 1 d . . . H42 H 0.0072 0.3234 0.0589 0.025 Uiso 1 1 calc R . . C31 C 0.28817(11) 0.52336(8) 0.33365(7) 0.0159(2) Uani 1 1 d . . . H31A H 0.2634 0.5162 0.3814 0.019 Uiso 1 1 calc R . . H31B H 0.3376 0.5756 0.3341 0.019 Uiso 1 1 calc R . . C22 C 0.13338(12) 0.37166(9) 0.40940(7) 0.0191(2) Uani 1 1 d . . . H22A H 0.0972 0.3140 0.4071 0.023 Uiso 1 1 calc R . . H22B H 0.1112 0.4000 0.3634 0.023 Uiso 1 1 calc R . . C21 C 0.31446(12) 0.33927(8) 0.35857(7) 0.0182(2) Uani 1 1 d . . . H21A H 0.2510 0.3130 0.3253 0.022 Uiso 1 1 calc R . . H21B H 0.3770 0.2956 0.3707 0.022 Uiso 1 1 calc R . . C49 C 0.57860(13) 0.61283(9) 0.09002(8) 0.0211(3) Uani 1 1 d . . . H49 H 0.6488 0.6468 0.0962 0.025 Uiso 1 1 calc R . . C45 C 0.21107(13) 0.52562(9) -0.04551(7) 0.0215(3) Uani 1 1 d . . . H45 H 0.1547 0.5299 -0.0864 0.026 Uiso 1 1 calc R . . C46 C 0.30906(13) 0.57603(9) -0.03919(7) 0.0207(3) Uani 1 1 d . . . H46 H 0.3206 0.6153 -0.0757 0.025 Uiso 1 1 calc R . . C50 C 0.55514(12) 0.55378(9) 0.14288(7) 0.0188(2) Uani 1 1 d . . . C54 C 0.63932(13) 0.54471(11) 0.20848(8) 0.0274(3) Uani 1 1 d . . . H54A H 0.6033 0.5692 0.2482 0.041 Uiso 1 1 calc R . . H54B H 0.7138 0.5749 0.2029 0.041 Uiso 1 1 calc R . . H54C H 0.6563 0.4841 0.2175 0.041 Uiso 1 1 calc R . . S34 S -0.01949(3) 0.64384(3) 0.189658(19) 0.02451(7) Uani 1 1 d . . . S24 S 0.11328(4) 0.37115(3) 0.551948(19) 0.02642(8) Uani 1 1 d . . . S14 S 0.82491(4) 0.28339(3) 0.45167(2) 0.02984(8) Uani 1 1 d . . . C26 C 0.30037(12) 0.30960(9) 0.48380(7) 0.0189(2) Uani 1 1 d . . . H26A H 0.3873 0.2986 0.4870 0.023 Uiso 1 1 calc R . . H26B H 0.2585 0.2540 0.4780 0.023 Uiso 1 1 calc R . . C35 C -0.03005(13) 0.58082(10) 0.26801(8) 0.0232(3) Uani 1 1 d . . . H35A H -0.0935 0.6047 0.2940 0.028 Uiso 1 1 calc R . . H35B H -0.0529 0.5216 0.2541 0.028 Uiso 1 1 calc R . . C25 C 0.27122(14) 0.35215(10) 0.55097(7) 0.0236(3) Uani 1 1 d . . . H25A H 0.3142 0.4073 0.5566 0.028 Uiso 1 1 calc R . . H25B H 0.3004 0.3156 0.5916 0.028 Uiso 1 1 calc R . . C23 C 0.08456(13) 0.42281(9) 0.46710(7) 0.0205(3) Uani 1 1 d . . . H23A H -0.0026 0.4303 0.4552 0.025 Uiso 1 1 calc R . . H23B H 0.1217 0.4802 0.4698 0.025 Uiso 1 1 calc R . . C13 C 0.70386(14) 0.30832(10) 0.50223(8) 0.0255(3) Uani 1 1 d . . . H13A H 0.6466 0.2601 0.4987 0.031 Uiso 1 1 calc R . . H13B H 0.7359 0.3148 0.5524 0.031 Uiso 1 1 calc R . . C16 C 0.67152(13) 0.37356(10) 0.35481(8) 0.0254(3) Uani 1 1 d . . . H16A H 0.7286 0.4217 0.3611 0.030 Uiso 1 1 calc R . . H16B H 0.6310 0.3760 0.3060 0.030 Uiso 1 1 calc R . . C15 C 0.73910(15) 0.28998(11) 0.36566(9) 0.0305(3) Uani 1 1 d . . . H15A H 0.7936 0.2841 0.3289 0.037 Uiso 1 1 calc R . . H15B H 0.6816 0.2420 0.3602 0.037 Uiso 1 1 calc R . . O1W O 0.8442(4) 0.3336(4) 0.1966(3) 0.0282(12) Uani 0.20 1 d P . . 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 I1 0.02409(5) 0.02021(4) 0.02370(5) -0.00217(3) 0.00105(3) 0.00530(3) Cu1 0.01503(7) 0.01763(7) 0.01301(7) -0.00017(5) 0.00142(5) -0.00016(5) P1 0.01377(14) 0.01516(14) 0.01248(14) -0.00061(11) 0.00047(11) 0.00096(11) N41 0.0152(5) 0.0151(5) 0.0142(5) -0.0015(4) 0.0012(4) 0.0002(4) N42 0.0148(5) 0.0161(5) 0.0158(5) -0.0012(4) 0.0027(4) -0.0003(4) N11 0.0176(5) 0.0206(5) 0.0154(5) -0.0026(4) -0.0031(4) 0.0042(4) C51 0.0143(5) 0.0168(5) 0.0138(5) -0.0020(4) 0.0018(4) 0.0021(4) C48 0.0249(7) 0.0156(6) 0.0239(7) 0.0026(5) 0.0092(5) 0.0006(5) C44 0.0186(6) 0.0209(6) 0.0144(6) -0.0016(5) 0.0010(4) 0.0040(5) C11 0.0181(6) 0.0195(6) 0.0198(6) -0.0028(5) -0.0034(5) 0.0042(5) C53 0.0213(7) 0.0244(7) 0.0219(7) 0.0011(5) 0.0015(5) -0.0073(5) C47 0.0218(6) 0.0150(6) 0.0172(6) 0.0006(4) 0.0062(5) 0.0035(4) C43 0.0186(6) 0.0240(7) 0.0181(6) -0.0040(5) -0.0032(5) 0.0024(5) C52 0.0156(6) 0.0149(5) 0.0156(6) -0.0006(4) 0.0038(4) 0.0015(4) C12 0.0272(7) 0.0219(6) 0.0155(6) -0.0019(5) -0.0051(5) 0.0038(5) C41 0.0159(6) 0.0177(6) 0.0179(6) -0.0032(5) 0.0019(4) -0.0002(4) N31 0.0159(5) 0.0172(5) 0.0124(5) 0.0011(4) 0.0012(4) 0.0029(4) N21 0.0174(5) 0.0192(5) 0.0133(5) 0.0012(4) 0.0027(4) 0.0024(4) C33 0.0199(6) 0.0237(6) 0.0150(6) 0.0004(5) 0.0013(5) 0.0040(5) C32 0.0185(6) 0.0198(6) 0.0147(6) 0.0016(5) 0.0007(4) 0.0015(5) C36 0.0197(6) 0.0237(6) 0.0150(6) 0.0005(5) 0.0020(5) 0.0068(5) C42 0.0173(6) 0.0218(6) 0.0214(6) -0.0043(5) -0.0011(5) -0.0033(5) C31 0.0172(6) 0.0165(6) 0.0136(5) -0.0006(4) 0.0000(4) 0.0021(4) C22 0.0169(6) 0.0222(6) 0.0178(6) -0.0009(5) 0.0008(5) 0.0018(5) C21 0.0220(6) 0.0163(6) 0.0167(6) 0.0002(5) 0.0045(5) 0.0016(5) C49 0.0213(6) 0.0170(6) 0.0260(7) 0.0000(5) 0.0073(5) -0.0028(5) C45 0.0255(7) 0.0228(6) 0.0159(6) 0.0007(5) 0.0006(5) 0.0060(5) C46 0.0271(7) 0.0199(6) 0.0156(6) 0.0033(5) 0.0045(5) 0.0039(5) C50 0.0173(6) 0.0180(6) 0.0212(6) -0.0010(5) 0.0034(5) -0.0013(5) C54 0.0225(7) 0.0321(8) 0.0266(7) 0.0037(6) -0.0015(6) -0.0095(6) S34 0.02490(17) 0.02949(18) 0.01846(16) 0.00244(13) -0.00047(13) 0.01181(14) S24 0.0337(2) 0.02743(18) 0.02012(16) 0.00474(14) 0.01163(14) 0.00733(15) S14 0.02014(17) 0.0310(2) 0.0363(2) 0.00388(16) -0.00549(15) 0.00614(14) C26 0.0211(6) 0.0184(6) 0.0169(6) 0.0033(5) 0.0015(5) 0.0037(5) C35 0.0191(6) 0.0296(7) 0.0208(7) 0.0016(5) 0.0023(5) 0.0065(5) C25 0.0293(7) 0.0251(7) 0.0158(6) 0.0030(5) -0.0002(5) 0.0028(5) C23 0.0206(6) 0.0218(6) 0.0194(6) 0.0026(5) 0.0039(5) 0.0044(5) C13 0.0284(7) 0.0236(7) 0.0226(7) 0.0034(5) -0.0045(6) 0.0025(6) C16 0.0225(7) 0.0328(8) 0.0207(7) 0.0027(6) 0.0022(5) 0.0070(6) C15 0.0258(8) 0.0366(8) 0.0285(8) -0.0022(6) 0.0011(6) 0.0136(6) O1W 0.011(2) 0.041(3) 0.032(3) 0.017(2) 0.0037(19) -0.003(2) _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 I1 Cu1 2.6535(2) . ? Cu1 N42 2.1078(11) . ? Cu1 N41 2.1108(11) . ? Cu1 P1 2.2121(4) . ? P1 C31 1.8508(13) . ? P1 C21 1.8612(14) . ? P1 C11 1.8654(14) . ? N41 C41 1.3338(16) . ? N41 C51 1.3642(16) . ? N42 C50 1.3360(17) . ? N42 C52 1.3660(17) . ? N11 C16 1.4626(19) . ? N11 C11 1.4634(17) . ? N11 C12 1.4641(17) . ? C51 C44 1.4089(18) . ? C51 C52 1.4401(18) . ? C48 C49 1.369(2) . ? C48 C47 1.407(2) . ? C48 H48 0.9500 . ? C44 C43 1.410(2) . ? C44 C45 1.4357(19) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C53 C41 1.5000(19) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C47 C52 1.4111(18) . ? C47 C46 1.433(2) . ? C43 C42 1.369(2) . ? C43 H43 0.9500 . ? C12 C13 1.519(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C41 C42 1.4097(19) . ? N31 C36 1.4679(17) . ? N31 C32 1.4680(16) . ? N31 C31 1.4713(16) . ? N21 C21 1.4592(17) . ? N21 C26 1.4683(16) . ? N21 C22 1.4685(17) . ? C33 C32 1.5225(18) . ? C33 S34 1.8161(14) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C36 C35 1.5197(19) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C42 H42 0.9500 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C22 C23 1.5169(19) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C49 C50 1.4168(19) . ? C49 H49 0.9500 . ? C45 C46 1.352(2) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C50 C54 1.489(2) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? S34 C35 1.8087(15) . ? S24 C23 1.8074(14) . ? S24 C25 1.8081(16) . ? S14 C13 1.8041(17) . ? S14 C15 1.8110(17) . ? C26 C25 1.5157(19) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C16 C15 1.517(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 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 N42 Cu1 N41 79.70(4) . . ? N42 Cu1 P1 123.40(3) . . ? N41 Cu1 P1 120.71(3) . . ? N42 Cu1 I1 107.45(3) . . ? N41 Cu1 I1 102.41(3) . . ? P1 Cu1 I1 116.403(12) . . ? C31 P1 C21 104.32(6) . . ? C31 P1 C11 94.64(6) . . ? C21 P1 C11 97.32(6) . . ? C31 P1 Cu1 117.58(4) . . ? C21 P1 Cu1 114.82(4) . . ? C11 P1 Cu1 124.21(5) . . ? C41 N41 C51 118.64(11) . . ? C41 N41 Cu1 128.82(9) . . ? C51 N41 Cu1 112.51(8) . . ? C50 N42 C52 118.52(11) . . ? C50 N42 Cu1 128.98(9) . . ? C52 N42 Cu1 112.49(8) . . ? C16 N11 C11 111.08(11) . . ? C16 N11 C12 112.11(11) . . ? C11 N11 C12 111.06(10) . . ? N41 C51 C44 123.00(12) . . ? N41 C51 C52 117.49(11) . . ? C44 C51 C52 119.51(12) . . ? C49 C48 C47 119.58(13) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C51 C44 C43 117.07(12) . . ? C51 C44 C45 119.72(13) . . ? C43 C44 C45 123.20(12) . . ? N11 C11 P1 113.81(9) . . ? N11 C11 H11A 108.8 . . ? P1 C11 H11A 108.8 . . ? N11 C11 H11B 108.8 . . ? P1 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C41 C53 H53A 109.5 . . ? C41 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C41 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C48 C47 C52 117.18(12) . . ? C48 C47 C46 123.06(12) . . ? C52 C47 C46 119.75(13) . . ? C42 C43 C44 119.55(12) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? N42 C52 C47 123.09(12) . . ? N42 C52 C51 117.63(11) . . ? C47 C52 C51 119.28(12) . . ? N11 C12 C13 111.97(12) . . ? N11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? N11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? N41 C41 C42 121.63(12) . . ? N41 C41 C53 117.46(11) . . ? C42 C41 C53 120.89(12) . . ? C36 N31 C32 110.52(10) . . ? C36 N31 C31 110.79(10) . . ? C32 N31 C31 109.46(10) . . ? C21 N21 C26 114.40(10) . . ? C21 N21 C22 111.13(11) . . ? C26 N21 C22 111.47(11) . . ? C32 C33 S34 112.16(9) . . ? C32 C33 H33A 109.2 . . ? S34 C33 H33A 109.2 . . ? C32 C33 H33B 109.2 . . ? S34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? N31 C32 C33 112.29(11) . . ? N31 C32 H32A 109.1 . . ? C33 C32 H32A 109.1 . . ? N31 C32 H32B 109.1 . . ? C33 C32 H32B 109.1 . . ? H32A C32 H32B 107.9 . . ? N31 C36 C35 111.32(11) . . ? N31 C36 H36A 109.4 . . ? C35 C36 H36A 109.4 . . ? N31 C36 H36B 109.4 . . ? C35 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C43 C42 C41 120.07(13) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? N31 C31 P1 114.05(9) . . ? N31 C31 H31A 108.7 . . ? P1 C31 H31A 108.7 . . ? N31 C31 H31B 108.7 . . ? P1 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? N21 C22 C23 111.12(11) . . ? N21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? N21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? N21 C21 P1 113.16(9) . . ? N21 C21 H21A 108.9 . . ? P1 C21 H21A 108.9 . . ? N21 C21 H21B 108.9 . . ? P1 C21 H21B 108.9 . . ? H21A C21 H21B 107.8 . . ? C48 C49 C50 120.10(13) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C46 C45 C44 120.77(13) . . ? C46 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? C45 C46 C47 120.97(13) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? N42 C50 C49 121.49(12) . . ? N42 C50 C54 117.91(12) . . ? C49 C50 C54 120.60(12) . . ? C50 C54 H54A 109.5 . . ? C50 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C50 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C35 S34 C33 95.80(6) . . ? C23 S24 C25 97.97(7) . . ? C13 S14 C15 96.65(7) . . ? N21 C26 C25 110.63(11) . . ? N21 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? N21 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C36 C35 S34 112.02(10) . . ? C36 C35 H35A 109.2 . . ? S34 C35 H35A 109.2 . . ? C36 C35 H35B 109.2 . . ? S34 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C26 C25 S24 113.07(10) . . ? C26 C25 H25A 109.0 . . ? S24 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? S24 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C22 C23 S24 111.92(9) . . ? C22 C23 H23A 109.2 . . ? S24 C23 H23A 109.2 . . ? C22 C23 H23B 109.2 . . ? S24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C12 C13 S14 112.67(11) . . ? C12 C13 H13A 109.1 . . ? S14 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? S14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? N11 C16 C15 111.41(13) . . ? N11 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? N11 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C16 C15 S14 112.36(11) . . ? C16 C15 H15A 109.1 . . ? S14 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? S14 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.563 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.100 data_publication_text _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 #TrackingRef '3nr_pub.cif' _audit_update_record ; 2011-01-23 # Formatted by publCIF ; _publ_contact_author_name 'Radoslaw Starosta' _publ_contact_author_address ;Faculty of Chemistry University of Wroclaw ul. F. Joliot-Curie 14 50-383 Wroclaw Poland ; _publ_contact_author_email radoslaw.starosta@chem.uni.wroc.pl loop_ _publ_author_name _publ_author_address R.Starosta ;Faculty of Chemistry, University of Wroclaw ul. F. Joliot-Curie 14 50-383 Wroclaw Poland ; B.Maciej ;Faculty of Chemistry University of Wroclaw ul. F. Joliot-Curie 14 50-383 Wroclaw Poland ; U.K.Komarnicka ;Faculty of Chemistry University of Wroclaw ul. F. Joliot-Curie 14 50-383 Wroclaw Poland ; P.Malgorzata ;Faculty of Chemistry University of Wroclaw ul. F. Joliot-Curie 14 50-383 Wroclaw Poland ; data_3nr _database_code_depnum_ccdc_archive 'CCDC 842341' #TrackingRef '3nr_pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Isothiocyanato-(2,9-dimetyl-1,10-phenanthroline-N,N') -(tris(morpholinomethyl)phosphine-P)-copper(i) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H42 Cu N6 O3 P S' _chemical_formula_sum 'C30 H42 Cu N6 O3 P S' _chemical_formula_weight 661.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.067(1) _cell_length_b 13.205(1) _cell_length_c 16.127(2) _cell_angle_alpha 86.10(2) _cell_angle_beta 76.29(1) _cell_angle_gamma 77.52(1) _cell_volume 1629.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10372 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 36.97 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.906 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details 'Oxford Diffraction, CrysAlis 1.171.30' _exptl_special_details ? _diffrn_ambient_temperature 100(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 KM4-CCD _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32746 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.1273 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 36.97 _reflns_number_total 14138 _reflns_number_gt 7427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, date)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, date)' _computing_data_reduction 'CrysAlis RED ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1999)' _computing_publication_material SHELXL-97 _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^)+(0.0314P)^2^+0.0000P] 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 14138 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 0.822 _refine_ls_restrained_S_all 0.822 _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 0.84045(3) 0.858307(15) 0.782576(12) 0.01537(5) Uani 1 1 d . . . P1 P 0.88606(5) 0.74914(3) 0.67872(2) 0.01326(8) Uani 1 1 d . . . S1 S 1.01671(6) 1.18360(3) 0.73986(3) 0.02710(10) Uani 1 1 d . . . N21 N 1.11131(16) 0.83368(9) 0.54435(8) 0.0145(3) Uani 1 1 d . . . O24 O 1.35799(14) 0.95354(9) 0.45353(7) 0.0245(3) Uani 1 1 d . . . N31 N 0.78138(17) 0.57034(9) 0.76191(8) 0.0164(3) Uani 1 1 d . . . N1 N 0.91595(17) 0.99180(10) 0.77062(8) 0.0200(3) Uani 1 1 d . . . N11 N 0.74034(16) 0.68536(10) 0.55678(8) 0.0172(3) Uani 1 1 d . . . N41 N 0.59502(16) 0.89019(9) 0.86980(8) 0.0155(3) Uani 1 1 d . . . C1 C 0.9586(2) 1.07105(12) 0.75790(9) 0.0173(3) Uani 1 1 d . . . N42 N 0.91196(17) 0.79706(10) 0.89594(8) 0.0167(3) Uani 1 1 d . . . C21 C 1.07705(19) 0.73664(12) 0.58758(9) 0.0159(3) Uani 1 1 d . . . H21A H 1.1816 0.7014 0.6082 0.019 Uiso 1 1 calc R . . H21B H 1.0610 0.6911 0.5451 0.019 Uiso 1 1 calc R . . C22 C 1.2146(2) 0.88222(12) 0.58765(10) 0.0168(3) Uani 1 1 d . . . H22A H 1.3221 0.8317 0.5928 0.020 Uiso 1 1 calc R . . H22B H 1.1465 0.9020 0.6459 0.020 Uiso 1 1 calc R . . C23 C 1.2630(2) 0.97778(13) 0.53861(11) 0.0232(4) Uani 1 1 d . . . H23A H 1.1554 1.0302 0.5372 0.028 Uiso 1 1 calc R . . H23B H 1.3344 1.0081 0.5684 0.028 Uiso 1 1 calc R . . C31 C 0.9254(2) 0.60747(11) 0.70361(9) 0.0164(3) Uani 1 1 d . . . H31A H 0.9539 0.5698 0.6494 0.020 Uiso 1 1 calc R . . H31B H 1.0291 0.5891 0.7286 0.020 Uiso 1 1 calc R . . C32 C 0.7632(2) 0.59897(13) 0.84980(10) 0.0239(4) Uani 1 1 d . . . H32A H 0.7368 0.6755 0.8538 0.029 Uiso 1 1 calc R . . H32B H 0.8746 0.5720 0.8672 0.029 Uiso 1 1 calc R . . C11 C 0.7081(2) 0.76394(12) 0.62155(10) 0.0174(3) Uani 1 1 d . . . H11A H 0.5981 0.7599 0.6635 0.021 Uiso 1 1 calc R . . H11B H 0.6928 0.8335 0.5938 0.021 Uiso 1 1 calc R . . C26 C 1.2073(2) 0.81224(13) 0.45557(9) 0.0207(3) Uani 1 1 d . . . H26A H 1.1346 0.7843 0.4249 0.025 Uiso 1 1 calc R . . H26B H 1.3150 0.7591 0.4550 0.025 Uiso 1 1 calc R . . C33 C 0.6193(2) 0.55563(14) 0.90934(11) 0.0299(4) Uani 1 1 d . . . H33A H 0.6106 0.5753 0.9686 0.036 Uiso 1 1 calc R . . H33B H 0.5068 0.5863 0.8942 0.036 Uiso 1 1 calc R . . O14 O 0.68726(16) 0.56052(9) 0.43244(7) 0.0265(3) Uani 1 1 d . . . O34 O 0.65023(16) 0.44553(9) 0.90479(7) 0.0290(3) Uani 1 1 d . . . C54 C 1.2172(2) 0.73893(14) 0.82871(11) 0.0250(4) Uani 1 1 d . . . H54A H 1.2337 0.6713 0.8030 0.038 Uiso 1 1 calc R . . H54B H 1.3242 0.7444 0.8453 0.038 Uiso 1 1 calc R . . H54C H 1.1905 0.7942 0.7872 0.038 Uiso 1 1 calc R . . C41 C 0.4403(2) 0.93895(12) 0.85594(10) 0.0179(3) Uani 1 1 d . . . C44 C 0.4585(2) 0.86962(12) 1.02029(10) 0.0199(3) Uani 1 1 d . . . C12 C 0.7296(2) 0.72777(12) 0.47149(10) 0.0199(3) Uani 1 1 d . . . H12A H 0.8060 0.7786 0.4545 0.024 Uiso 1 1 calc R . . H12B H 0.6083 0.7638 0.4717 0.024 Uiso 1 1 calc R . . C25 C 1.2545(2) 0.90997(14) 0.41021(10) 0.0263(4) Uani 1 1 d . . . H25A H 1.3204 0.8935 0.3510 0.032 Uiso 1 1 calc R . . H25B H 1.1466 0.9615 0.4076 0.032 Uiso 1 1 calc R . . C51 C 0.6048(2) 0.85632(11) 0.95084(9) 0.0166(3) Uani 1 1 d . . . C53 C 0.4325(2) 0.97504(13) 0.76644(10) 0.0214(3) Uani 1 1 d . . . H53A H 0.5508 0.9743 0.7324 0.032 Uiso 1 1 calc R . . H53B H 0.3626 1.0458 0.7673 0.032 Uiso 1 1 calc R . . H53C H 0.3790 0.9287 0.7411 0.032 Uiso 1 1 calc R . . C52 C 0.7734(2) 0.80608(12) 0.96492(9) 0.0174(3) Uani 1 1 d . . . C15 C 0.6974(2) 0.52161(13) 0.51611(11) 0.0235(4) Uani 1 1 d . . . H15A H 0.8198 0.4889 0.5165 0.028 Uiso 1 1 calc R . . H15B H 0.6264 0.4678 0.5323 0.028 Uiso 1 1 calc R . . C13 C 0.7864(2) 0.63990(14) 0.40869(11) 0.0256(4) Uani 1 1 d . . . H13A H 0.7739 0.6681 0.3515 0.031 Uiso 1 1 calc R . . H13B H 0.9112 0.6090 0.4048 0.031 Uiso 1 1 calc R . . C36 C 0.8105(2) 0.45700(12) 0.75803(10) 0.0222(3) Uani 1 1 d . . . H36A H 0.9228 0.4253 0.7730 0.027 Uiso 1 1 calc R . . H36B H 0.8169 0.4367 0.6992 0.027 Uiso 1 1 calc R . . C16 C 0.6324(2) 0.60752(12) 0.58054(10) 0.0191(3) Uani 1 1 d . . . H16A H 0.5092 0.6396 0.5815 0.023 Uiso 1 1 calc R . . H16B H 0.6393 0.5789 0.6383 0.023 Uiso 1 1 calc R . . C43 C 0.2974(2) 0.92098(13) 1.00382(11) 0.0232(4) Uani 1 1 d . . . H43 H 0.1954 0.9319 1.0487 0.028 Uiso 1 1 calc R . . C50 C 1.0689(2) 0.74952(12) 0.90631(10) 0.0205(3) Uani 1 1 d . . . C35 C 0.6642(2) 0.41733(14) 0.81916(11) 0.0286(4) Uani 1 1 d . . . H35A H 0.5529 0.4464 0.8024 0.034 Uiso 1 1 calc R . . H35B H 0.6860 0.3408 0.8158 0.034 Uiso 1 1 calc R . . C49 C 1.0952(2) 0.70861(14) 0.98645(11) 0.0266(4) Uani 1 1 d . . . H49 H 1.2086 0.6750 0.9924 0.032 Uiso 1 1 calc R . . C42 C 0.2888(2) 0.95503(13) 0.92273(11) 0.0227(3) Uani 1 1 d . . . H42 H 0.1803 0.9897 0.9112 0.027 Uiso 1 1 calc R . . C47 C 0.7895(2) 0.76784(12) 1.04677(10) 0.0214(3) Uani 1 1 d . . . C45 C 0.4803(2) 0.83059(13) 1.10348(10) 0.0250(4) Uani 1 1 d . . . H45 H 0.3822 0.8395 1.1505 0.030 Uiso 1 1 calc R . . C46 C 0.6373(2) 0.78175(13) 1.11569(10) 0.0262(4) Uani 1 1 d . . . H46 H 0.6477 0.7559 1.1711 0.031 Uiso 1 1 calc R . . C48 C 0.9571(2) 0.71750(13) 1.05550(11) 0.0275(4) Uani 1 1 d . . . H48 H 0.9743 0.6897 1.1094 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01758(10) 0.01463(10) 0.01344(9) 0.00050(7) -0.00215(7) -0.00407(7) P1 0.01383(19) 0.01212(18) 0.01305(18) 0.00139(15) -0.00121(14) -0.00356(15) S1 0.0360(3) 0.0166(2) 0.0318(2) 0.00210(18) -0.0093(2) -0.01106(18) N21 0.0133(6) 0.0163(6) 0.0135(6) 0.0026(5) -0.0007(5) -0.0058(5) O24 0.0189(6) 0.0304(7) 0.0250(6) 0.0080(5) -0.0024(5) -0.0120(5) N31 0.0197(7) 0.0118(6) 0.0158(6) 0.0017(5) 0.0005(5) -0.0045(5) N1 0.0226(7) 0.0185(7) 0.0173(7) 0.0002(5) -0.0012(5) -0.0049(6) N11 0.0181(7) 0.0165(6) 0.0182(6) -0.0012(5) -0.0049(5) -0.0051(5) N41 0.0183(7) 0.0131(6) 0.0156(6) -0.0002(5) -0.0023(5) -0.0055(5) C1 0.0163(8) 0.0188(8) 0.0142(7) -0.0022(6) -0.0022(6) 0.0009(6) N42 0.0189(7) 0.0158(6) 0.0158(6) 0.0003(5) -0.0036(5) -0.0049(5) C21 0.0147(7) 0.0148(7) 0.0170(7) 0.0002(6) -0.0010(6) -0.0033(6) C22 0.0147(7) 0.0173(7) 0.0186(7) -0.0001(6) -0.0027(6) -0.0047(6) C23 0.0174(8) 0.0207(8) 0.0302(9) 0.0016(7) -0.0013(7) -0.0065(7) C31 0.0173(8) 0.0147(7) 0.0157(7) 0.0021(6) -0.0009(6) -0.0039(6) C32 0.0336(10) 0.0210(8) 0.0162(8) 0.0002(7) -0.0004(7) -0.0099(7) C11 0.0158(8) 0.0168(7) 0.0195(8) -0.0012(6) -0.0046(6) -0.0021(6) C26 0.0191(8) 0.0308(9) 0.0141(7) 0.0009(7) -0.0022(6) -0.0112(7) C33 0.0361(11) 0.0254(9) 0.0218(9) 0.0039(7) 0.0055(7) -0.0072(8) O14 0.0315(7) 0.0287(7) 0.0235(6) -0.0042(5) -0.0054(5) -0.0150(5) O34 0.0326(7) 0.0212(6) 0.0267(6) 0.0097(5) 0.0027(5) -0.0050(5) C54 0.0207(9) 0.0294(9) 0.0248(9) 0.0010(7) -0.0068(7) -0.0033(7) C41 0.0178(8) 0.0156(7) 0.0203(8) -0.0019(6) -0.0033(6) -0.0042(6) C44 0.0242(9) 0.0159(7) 0.0183(8) -0.0021(6) 0.0018(6) -0.0077(6) C12 0.0211(8) 0.0200(8) 0.0187(8) 0.0000(6) -0.0035(6) -0.0059(7) C25 0.0227(9) 0.0384(10) 0.0201(8) 0.0116(8) -0.0050(7) -0.0151(8) C51 0.0225(8) 0.0123(7) 0.0151(7) -0.0017(6) -0.0017(6) -0.0062(6) C53 0.0182(8) 0.0214(8) 0.0235(8) 0.0002(7) -0.0060(7) -0.0004(7) C52 0.0245(8) 0.0143(7) 0.0140(7) -0.0002(6) -0.0040(6) -0.0060(6) C15 0.0235(9) 0.0206(8) 0.0280(9) -0.0017(7) -0.0067(7) -0.0069(7) C13 0.0261(9) 0.0289(9) 0.0218(8) -0.0027(7) 0.0010(7) -0.0117(7) C36 0.0267(9) 0.0146(8) 0.0230(8) 0.0015(6) 0.0003(7) -0.0062(7) C16 0.0183(8) 0.0178(8) 0.0218(8) 0.0019(6) -0.0050(6) -0.0057(6) C43 0.0199(8) 0.0221(8) 0.0240(8) -0.0071(7) 0.0058(7) -0.0066(7) C50 0.0227(9) 0.0190(8) 0.0207(8) -0.0004(6) -0.0068(7) -0.0040(7) C35 0.0310(10) 0.0192(8) 0.0320(10) 0.0019(7) 0.0037(8) -0.0103(7) C49 0.0292(10) 0.0270(9) 0.0249(9) 0.0013(7) -0.0137(7) -0.0007(7) C42 0.0166(8) 0.0211(8) 0.0283(9) -0.0044(7) -0.0014(7) -0.0023(6) C47 0.0327(10) 0.0169(8) 0.0154(7) -0.0003(6) -0.0059(7) -0.0064(7) C45 0.0349(10) 0.0207(8) 0.0164(8) -0.0031(7) 0.0053(7) -0.0109(7) C46 0.0421(11) 0.0223(9) 0.0126(7) 0.0015(7) -0.0012(7) -0.0096(8) C48 0.0398(11) 0.0256(9) 0.0182(8) 0.0047(7) -0.0127(8) -0.0042(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.9692(14) . ? Cu1 N42 2.1039(13) . ? Cu1 N41 2.1156(13) . ? Cu1 P1 2.1968(5) . ? P1 C21 1.8469(15) . ? P1 C11 1.8522(15) . ? P1 C31 1.8609(15) . ? S1 C1 1.6405(17) . ? N21 C21 1.4644(18) . ? N21 C22 1.4699(19) . ? N21 C26 1.4713(19) . ? O24 C23 1.424(2) . ? O24 C25 1.433(2) . ? N31 C32 1.457(2) . ? N31 C31 1.4632(19) . ? N31 C36 1.4673(19) . ? N1 C1 1.1611(19) . ? N11 C16 1.4615(19) . ? N11 C11 1.4620(19) . ? N11 C12 1.464(2) . ? N41 C41 1.337(2) . ? N41 C51 1.3669(19) . ? N42 C50 1.329(2) . ? N42 C52 1.368(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.517(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.511(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C26 C25 1.516(2) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C33 O34 1.425(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? O14 C15 1.425(2) . ? O14 C13 1.431(2) . ? O34 C35 1.427(2) . ? C54 C50 1.503(2) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C41 C42 1.412(2) . ? C41 C53 1.500(2) . ? C44 C43 1.406(2) . ? C44 C51 1.410(2) . ? C44 C45 1.441(2) . ? C12 C13 1.514(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C51 C52 1.441(2) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C52 C47 1.406(2) . ? C15 C16 1.512(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C36 C35 1.511(2) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C43 C42 1.366(2) . ? C43 H43 0.9500 . ? C50 C49 1.412(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C49 C48 1.367(3) . ? C49 H49 0.9500 . ? C42 H42 0.9500 . ? C47 C48 1.407(2) . ? C47 C46 1.435(2) . ? C45 C46 1.344(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C48 H48 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 N1 Cu1 N42 101.78(5) . . ? N1 Cu1 N41 103.56(5) . . ? N42 Cu1 N41 79.69(5) . . ? N1 Cu1 P1 125.05(4) . . ? N42 Cu1 P1 116.81(4) . . ? N41 Cu1 P1 119.92(4) . . ? C21 P1 C11 100.42(7) . . ? C21 P1 C31 93.46(7) . . ? C11 P1 C31 101.41(7) . . ? C21 P1 Cu1 122.78(5) . . ? C11 P1 Cu1 115.55(5) . . ? C31 P1 Cu1 118.91(5) . . ? C21 N21 C22 111.03(12) . . ? C21 N21 C26 109.35(12) . . ? C22 N21 C26 109.17(11) . . ? C23 O24 C25 109.42(12) . . ? C32 N31 C31 111.80(12) . . ? C32 N31 C36 108.74(12) . . ? C31 N31 C36 109.86(12) . . ? C1 N1 Cu1 175.27(12) . . ? C16 N11 C11 113.81(12) . . ? C16 N11 C12 109.84(12) . . ? C11 N11 C12 114.21(12) . . ? C41 N41 C51 118.55(13) . . ? C41 N41 Cu1 129.07(10) . . ? C51 N41 Cu1 112.37(10) . . ? N1 C1 S1 179.41(15) . . ? C50 N42 C52 118.80(14) . . ? C50 N42 Cu1 128.17(11) . . ? C52 N42 Cu1 112.98(10) . . ? N21 C21 P1 115.98(10) . . ? N21 C21 H21A 108.3 . . ? P1 C21 H21A 108.3 . . ? N21 C21 H21B 108.3 . . ? P1 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? N21 C22 C23 110.94(13) . . ? N21 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? N21 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.0 . . ? O24 C23 C22 111.49(13) . . ? O24 C23 H23A 109.3 . . ? C22 C23 H23A 109.3 . . ? O24 C23 H23B 109.3 . . ? C22 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? N31 C31 P1 115.89(10) . . ? N31 C31 H31A 108.3 . . ? P1 C31 H31A 108.3 . . ? N31 C31 H31B 108.3 . . ? P1 C31 H31B 108.3 . . ? H31A C31 H31B 107.4 . . ? N31 C32 C33 110.86(14) . . ? N31 C32 H32A 109.5 . . ? C33 C32 H32A 109.5 . . ? N31 C32 H32B 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? N11 C11 P1 113.27(10) . . ? N11 C11 H11A 108.9 . . ? P1 C11 H11A 108.9 . . ? N11 C11 H11B 108.9 . . ? P1 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N21 C26 C25 110.88(14) . . ? N21 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? N21 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? O34 C33 C32 111.54(14) . . ? O34 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? O34 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C15 O14 C13 110.15(12) . . ? C33 O34 C35 109.24(12) . . ? C50 C54 H54A 109.5 . . ? C50 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C50 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N41 C41 C42 121.41(15) . . ? N41 C41 C53 117.63(14) . . ? C42 C41 C53 120.96(15) . . ? C43 C44 C51 117.34(15) . . ? C43 C44 C45 123.49(15) . . ? C51 C44 C45 119.17(16) . . ? N11 C12 C13 109.01(13) . . ? N11 C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? N11 C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? O24 C25 C26 111.06(13) . . ? O24 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? O24 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? N41 C51 C44 122.87(15) . . ? N41 C51 C52 117.75(14) . . ? C44 C51 C52 119.37(14) . . ? C41 C53 H53A 109.5 . . ? C41 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C41 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N42 C52 C47 122.90(15) . . ? N42 C52 C51 117.20(14) . . ? C47 C52 C51 119.90(14) . . ? O14 C15 C16 111.08(13) . . ? O14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? O14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? O14 C13 C12 112.66(13) . . ? O14 C13 H13A 109.1 . . ? C12 C13 H13A 109.1 . . ? O14 C13 H13B 109.1 . . ? C12 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? N31 C36 C35 110.45(13) . . ? N31 C36 H36A 109.6 . . ? C35 C36 H36A 109.6 . . ? N31 C36 H36B 109.6 . . ? C35 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? N11 C16 C15 108.85(13) . . ? N11 C16 H16A 109.9 . . ? C15 C16 H16A 109.9 . . ? N11 C16 H16B 109.9 . . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? C42 C43 C44 119.45(15) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? N42 C50 C49 121.57(15) . . ? N42 C50 C54 117.30(14) . . ? C49 C50 C54 121.11(15) . . ? O34 C35 C36 111.22(14) . . ? O34 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? O34 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C48 C49 C50 119.80(16) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C43 C42 C41 120.38(16) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C52 C47 C48 116.88(15) . . ? C52 C47 C46 119.11(16) . . ? C48 C47 C46 124.01(15) . . ? C46 C45 C44 121.08(15) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C45 C46 C47 121.34(16) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C49 C48 C47 120.05(16) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? _diffrn_measured_fraction_theta_max 0.854 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.537 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.078 # Attachment 'saz015_pub.cif' data_3SNR _database_code_depnum_ccdc_archive 'CCDC 842343' #TrackingRef 'saz015_pub.cif' _audit_update_record ; 2011-01-28 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; isothiocyanato-(2,9-dimetyl-1,10-phenanthroline-N,N')- (tris(thiomorpholinomethyl) phosphine-P)-copper(i) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H42 Cu N6 P S4' _chemical_formula_sum 'C30 H42 Cu N6 P S4' _chemical_formula_weight 709.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.313(1) _cell_length_b 13.258(5) _cell_length_c 14.436(2) _cell_angle_alpha 87.45(1) _cell_angle_beta 84.99(1) _cell_angle_gamma 71.36(2) _cell_volume 1682.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10153 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 36.99 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.976 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 0.925 _exptl_absorpt_process_details 'Oxford Diffraction, CrysAlis 1.171.30' _exptl_special_details ? _diffrn_ambient_temperature 100(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 KM4-CCD _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33363 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.1858 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 36.99 _reflns_number_total 17104 _reflns_number_gt 6157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, date)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, date)' _computing_data_reduction 'CrysAlis RED ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1999)' _computing_publication_material SHELXL-97 _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^)+(0.0631P)^2^+0.0000P] 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 14553 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1647 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1398 _refine_ls_wR_factor_gt 0.1170 _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_restrained_S_all 0.809 _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 0.67249(4) 0.64492(3) 0.70061(2) 0.01936(9) Uani 1 1 d . . . C1 C 0.5793(3) 0.4387(2) 0.7091(2) 0.0218(6) Uani 1 1 d . . . N1 N 0.6049(3) 0.51917(19) 0.70428(17) 0.0247(5) Uani 1 1 d . . . S1 S 0.54700(9) 0.32393(6) 0.71491(7) 0.0352(2) Uani 1 1 d . . . P1 P 0.63004(8) 0.75528(5) 0.81772(5) 0.01766(15) Uani 1 1 d . . . N11 N 0.4122(3) 0.68918(18) 0.92708(16) 0.0217(5) Uani 1 1 d . . . N21 N 0.7507(3) 0.78943(18) 0.97943(16) 0.0206(5) Uani 1 1 d . . . N31 N 0.7511(3) 0.91934(17) 0.76055(16) 0.0182(5) Uani 1 1 d . . . C11 C 0.4559(3) 0.7827(2) 0.8975(2) 0.0210(6) Uani 1 1 d . . . H11A H 0.4711 0.8175 0.9534 0.025 Uiso 1 1 calc R . . H11B H 0.3708 0.8338 0.8664 0.025 Uiso 1 1 calc R . . C12 C 0.3260(4) 0.7074(3) 1.0185(2) 0.0281(7) Uani 1 1 d . . . H12A H 0.2307 0.7673 1.0130 0.034 Uiso 1 1 calc R . . H12B H 0.3865 0.7280 1.0629 0.034 Uiso 1 1 calc R . . C13 C 0.2872(4) 0.6095(3) 1.0568(2) 0.0335(7) Uani 1 1 d . . . H13A H 0.2344 0.6251 1.1196 0.040 Uiso 1 1 calc R . . H13B H 0.3826 0.5500 1.0631 0.040 Uiso 1 1 calc R . . C15 C 0.2868(4) 0.5632(3) 0.8769(2) 0.0325(7) Uani 1 1 d . . . H15A H 0.3828 0.5037 0.8812 0.039 Uiso 1 1 calc R . . H15B H 0.2341 0.5487 0.8248 0.039 Uiso 1 1 calc R . . C16 C 0.3232(3) 0.6664(2) 0.8564(2) 0.0264(6) Uani 1 1 d . . . H16A H 0.3808 0.6617 0.7949 0.032 Uiso 1 1 calc R . . H16B H 0.2270 0.7260 0.8533 0.032 Uiso 1 1 calc R . . C21 C 0.7789(3) 0.7162(2) 0.90095(19) 0.0217(6) Uani 1 1 d . . . H21A H 0.7869 0.6440 0.9259 0.026 Uiso 1 1 calc R . . H21B H 0.8777 0.7126 0.8673 0.026 Uiso 1 1 calc R . . C22 C 0.8568(3) 0.8512(2) 0.9735(2) 0.0230(6) Uani 1 1 d . . . H22A H 0.8660 0.8787 0.9092 0.028 Uiso 1 1 calc R . . H22B H 0.9585 0.8044 0.9889 0.028 Uiso 1 1 calc R . . C23 C 0.8022(4) 0.9439(2) 1.0402(2) 0.0267(6) Uani 1 1 d . . . H23A H 0.6992 0.9893 1.0257 0.032 Uiso 1 1 calc R . . H23B H 0.8710 0.9876 1.0312 0.032 Uiso 1 1 calc R . . C25 C 0.6835(3) 0.8127(2) 1.1469(2) 0.0255(6) Uani 1 1 d . . . H25A H 0.6769 0.7731 1.2061 0.031 Uiso 1 1 calc R . . H25B H 0.5791 0.8569 1.1340 0.031 Uiso 1 1 calc R . . C26 C 0.7482(3) 0.7341(2) 1.06956(19) 0.0229(6) Uani 1 1 d . . . H26A H 0.8528 0.6899 1.0818 0.027 Uiso 1 1 calc R . . H26B H 0.6857 0.6864 1.0678 0.027 Uiso 1 1 calc R . . C31 C 0.6117(3) 0.8979(2) 0.79563(19) 0.0188(5) Uani 1 1 d . . . H31A H 0.5344 0.9273 0.7502 0.023 Uiso 1 1 calc R . . H31B H 0.5732 0.9367 0.8544 0.023 Uiso 1 1 calc R . . C32 C 0.8000(3) 0.8779(2) 0.66713(19) 0.0211(6) Uani 1 1 d . . . H32A H 0.7228 0.9170 0.6242 0.025 Uiso 1 1 calc R . . H32B H 0.8059 0.8020 0.6675 0.025 Uiso 1 1 calc R . . C33 C 0.9528(3) 0.8875(2) 0.6310(2) 0.0254(6) Uani 1 1 d . . . H33A H 0.9830 0.8534 0.5696 0.030 Uiso 1 1 calc R . . H33B H 1.0301 0.8492 0.6741 0.030 Uiso 1 1 calc R . . C35 C 0.8746(3) 1.0607(2) 0.7378(2) 0.0256(6) Uani 1 1 d . . . H35A H 0.9523 1.0224 0.7807 0.031 Uiso 1 1 calc R . . H35B H 0.8545 1.1380 0.7450 0.031 Uiso 1 1 calc R . . C36 C 0.7294(3) 1.0342(2) 0.7644(2) 0.0213(6) Uani 1 1 d . . . H36A H 0.6910 1.0591 0.8283 0.026 Uiso 1 1 calc R . . H36B H 0.6515 1.0730 0.7218 0.026 Uiso 1 1 calc R . . S14 S 0.16843(9) 0.56881(6) 0.98393(6) 0.02931(18) Uani 1 1 d . . . S24 S 0.79643(9) 0.89923(6) 1.16028(5) 0.02728(17) Uani 1 1 d . . . S34 S 0.94828(9) 1.02484(6) 0.61971(6) 0.02959(18) Uani 1 1 d . . . N41 N 0.6404(3) 0.72179(18) 0.56991(16) 0.0188(5) Uani 1 1 d . . . N42 N 0.8973(3) 0.59220(17) 0.63802(15) 0.0183(5) Uani 1 1 d . . . C41 C 0.5122(3) 0.7891(2) 0.5403(2) 0.0236(6) Uani 1 1 d . . . C42 C 0.5137(3) 0.8537(2) 0.4597(2) 0.0267(6) Uani 1 1 d . . . H42 H 0.4214 0.9028 0.4410 0.032 Uiso 1 1 calc R . . C43 C 0.6472(4) 0.8458(2) 0.4088(2) 0.0271(6) Uani 1 1 d . . . H43 H 0.6483 0.8894 0.3549 0.032 Uiso 1 1 calc R . . C44 C 0.7837(3) 0.7723(2) 0.43685(19) 0.0210(6) Uani 1 1 d . . . C45 C 0.9291(3) 0.7566(2) 0.3870(2) 0.0243(6) Uani 1 1 d . . . H45 H 0.9355 0.7957 0.3308 0.029 Uiso 1 1 calc R . . C46 C 1.0570(3) 0.6874(2) 0.4184(2) 0.0251(6) Uani 1 1 d . . . H46 H 1.1516 0.6777 0.3835 0.030 Uiso 1 1 calc R . . C47 C 1.0521(3) 0.6285(2) 0.5035(2) 0.0216(6) Uani 1 1 d . . . C48 C 1.1814(3) 0.5568(2) 0.5411(2) 0.0257(6) Uani 1 1 d . . . H48 H 1.2788 0.5444 0.5090 0.031 Uiso 1 1 calc R . . C49 C 1.1670(3) 0.5050(2) 0.6237(2) 0.0249(6) Uani 1 1 d . . . H49 H 1.2543 0.4566 0.6489 0.030 Uiso 1 1 calc R . . C50 C 1.0224(3) 0.5235(2) 0.67143(19) 0.0217(6) Uani 1 1 d . . . C51 C 0.7741(3) 0.7131(2) 0.51937(18) 0.0172(5) Uani 1 1 d . . . C52 C 0.9109(3) 0.6418(2) 0.55465(18) 0.0181(5) Uani 1 1 d . . . C53 C 0.3652(3) 0.7951(3) 0.5952(2) 0.0344(8) Uani 1 1 d . . . H53A H 0.3525 0.7244 0.5990 0.052 Uiso 1 1 calc R . . H53B H 0.2804 0.8451 0.5645 0.052 Uiso 1 1 calc R . . H53C H 0.3667 0.8196 0.6581 0.052 Uiso 1 1 calc R . . C54 C 1.0013(3) 0.4682(2) 0.7618(2) 0.0254(6) Uani 1 1 d . . . H54A H 0.9882 0.5171 0.8131 0.038 Uiso 1 1 calc R . . H54B H 1.0908 0.4058 0.7697 0.038 Uiso 1 1 calc R . . H54C H 0.9110 0.4454 0.7617 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02374(19) 0.01596(17) 0.02069(18) 0.00105(13) -0.00070(14) -0.00996(14) C1 0.0195(14) 0.0193(14) 0.0257(15) 0.0008(11) 0.0002(11) -0.0056(11) N1 0.0299(14) 0.0217(12) 0.0260(13) -0.0020(10) 0.0020(10) -0.0141(11) S1 0.0301(4) 0.0159(4) 0.0623(6) 0.0006(4) -0.0003(4) -0.0119(3) P1 0.0204(4) 0.0145(3) 0.0197(4) 0.0011(3) -0.0001(3) -0.0083(3) N11 0.0245(12) 0.0200(12) 0.0235(12) 0.0022(9) 0.0017(10) -0.0122(10) N21 0.0234(12) 0.0171(11) 0.0222(12) -0.0011(9) -0.0024(10) -0.0073(9) N31 0.0226(12) 0.0130(10) 0.0212(12) 0.0021(9) -0.0011(9) -0.0090(9) C11 0.0218(14) 0.0192(13) 0.0242(15) 0.0006(11) 0.0006(11) -0.0104(11) C12 0.0306(17) 0.0323(17) 0.0246(16) -0.0016(13) 0.0020(13) -0.0154(14) C13 0.0335(18) 0.0385(19) 0.0316(18) 0.0101(14) -0.0006(14) -0.0176(15) C15 0.0334(18) 0.0306(17) 0.0379(19) -0.0079(14) 0.0067(14) -0.0180(14) C16 0.0255(15) 0.0283(16) 0.0291(16) -0.0023(12) 0.0030(12) -0.0147(13) C21 0.0239(14) 0.0164(13) 0.0246(15) 0.0007(11) -0.0019(11) -0.0061(11) C22 0.0277(15) 0.0217(14) 0.0212(14) 0.0034(11) -0.0008(12) -0.0110(12) C23 0.0364(17) 0.0205(14) 0.0265(16) 0.0002(12) -0.0019(13) -0.0139(13) C25 0.0279(16) 0.0264(15) 0.0256(15) 0.0004(12) 0.0018(12) -0.0144(13) C26 0.0282(16) 0.0194(14) 0.0219(14) 0.0016(11) 0.0021(12) -0.0099(12) C31 0.0206(14) 0.0146(12) 0.0225(14) 0.0022(10) -0.0013(11) -0.0079(11) C32 0.0258(15) 0.0157(13) 0.0238(15) 0.0010(11) -0.0020(11) -0.0099(11) C33 0.0310(16) 0.0184(14) 0.0282(16) -0.0026(12) 0.0066(12) -0.0120(12) C35 0.0311(16) 0.0182(14) 0.0305(16) -0.0009(12) -0.0002(13) -0.0126(12) C36 0.0246(15) 0.0150(13) 0.0254(15) 0.0009(11) -0.0019(11) -0.0080(11) S14 0.0251(4) 0.0226(4) 0.0423(5) 0.0047(3) 0.0015(3) -0.0122(3) S24 0.0340(4) 0.0300(4) 0.0224(4) -0.0023(3) -0.0022(3) -0.0162(3) S34 0.0388(5) 0.0210(4) 0.0330(4) -0.0011(3) 0.0088(3) -0.0180(3) N41 0.0208(12) 0.0175(11) 0.0193(12) -0.0007(9) -0.0033(9) -0.0073(9) N42 0.0228(12) 0.0136(11) 0.0197(12) 0.0026(9) -0.0016(9) -0.0079(9) C41 0.0240(15) 0.0215(14) 0.0254(15) 0.0011(11) -0.0059(12) -0.0065(12) C42 0.0269(16) 0.0232(15) 0.0276(16) 0.0060(12) -0.0108(12) -0.0032(12) C43 0.0420(18) 0.0202(14) 0.0208(15) 0.0053(11) -0.0081(13) -0.0118(13) C44 0.0289(15) 0.0171(13) 0.0187(14) 0.0001(11) -0.0024(11) -0.0094(12) C45 0.0331(17) 0.0203(14) 0.0229(15) 0.0001(11) 0.0026(12) -0.0147(13) C46 0.0285(16) 0.0229(15) 0.0264(16) -0.0038(12) 0.0073(12) -0.0139(13) C47 0.0231(14) 0.0157(13) 0.0270(15) -0.0041(11) 0.0014(12) -0.0079(11) C48 0.0197(14) 0.0242(15) 0.0329(17) -0.0075(12) 0.0019(12) -0.0069(12) C49 0.0240(15) 0.0188(14) 0.0310(16) -0.0025(12) -0.0087(12) -0.0036(12) C50 0.0276(15) 0.0168(13) 0.0228(15) -0.0007(11) -0.0061(12) -0.0089(12) C51 0.0208(14) 0.0136(12) 0.0180(13) -0.0016(10) -0.0019(10) -0.0064(10) C52 0.0241(14) 0.0153(12) 0.0175(13) -0.0023(10) 0.0005(11) -0.0101(11) C53 0.0223(16) 0.0370(18) 0.041(2) 0.0075(15) -0.0058(14) -0.0060(14) C54 0.0295(16) 0.0190(14) 0.0256(15) 0.0038(11) -0.0090(12) -0.0034(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.958(2) . ? Cu1 N41 2.102(2) . ? Cu1 N42 2.116(2) . ? Cu1 P1 2.2110(9) . ? C1 N1 1.163(4) . ? C1 S1 1.641(3) . ? P1 C21 1.847(3) . ? P1 C11 1.850(3) . ? P1 C31 1.859(3) . ? N11 C11 1.460(3) . ? N11 C16 1.468(4) . ? N11 C12 1.471(4) . ? N21 C22 1.466(4) . ? N21 C26 1.467(4) . ? N21 C21 1.476(4) . ? N31 C32 1.458(3) . ? N31 C31 1.460(3) . ? N31 C36 1.474(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.524(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 S14 1.805(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 C16 1.523(4) . ? C15 S14 1.808(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.522(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 S24 1.808(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C25 C26 1.510(4) . ? C25 S24 1.813(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.514(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 S34 1.808(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C35 C36 1.517(4) . ? C35 S34 1.806(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N41 C41 1.334(4) . ? N41 C51 1.361(3) . ? N42 C50 1.342(4) . ? N42 C52 1.361(3) . ? C41 C42 1.415(4) . ? C41 C53 1.503(4) . ? C42 C43 1.364(4) . ? C42 H42 0.9500 . ? C43 C44 1.412(4) . ? C43 H43 0.9500 . ? C44 C51 1.409(4) . ? C44 C45 1.435(4) . ? C45 C46 1.350(4) . ? C45 H45 0.9500 . ? C46 C47 1.431(4) . ? C46 H46 0.9500 . ? C47 C48 1.410(4) . ? C47 C52 1.414(4) . ? C48 C49 1.367(4) . ? C48 H48 0.9500 . ? C49 C50 1.411(4) . ? C49 H49 0.9500 . ? C50 C54 1.497(4) . ? C51 C52 1.441(4) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 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 N41 110.06(10) . . ? N1 Cu1 N42 104.68(9) . . ? N41 Cu1 N42 79.49(9) . . ? N1 Cu1 P1 123.68(7) . . ? N41 Cu1 P1 113.78(7) . . ? N42 Cu1 P1 116.41(7) . . ? N1 C1 S1 178.7(3) . . ? C1 N1 Cu1 173.1(2) . . ? C21 P1 C11 101.16(13) . . ? C21 P1 C31 101.46(13) . . ? C11 P1 C31 94.71(12) . . ? C21 P1 Cu1 113.70(9) . . ? C11 P1 Cu1 121.53(9) . . ? C31 P1 Cu1 120.46(9) . . ? C11 N11 C16 109.1(2) . . ? C11 N11 C12 110.0(2) . . ? C16 N11 C12 111.5(2) . . ? C22 N21 C26 112.1(2) . . ? C22 N21 C21 112.1(2) . . ? C26 N21 C21 112.0(2) . . ? C32 N31 C31 110.7(2) . . ? C32 N31 C36 112.2(2) . . ? C31 N31 C36 110.0(2) . . ? N11 C11 P1 114.93(19) . . ? N11 C11 H11A 108.5 . . ? P1 C11 H11A 108.5 . . ? N11 C11 H11B 108.5 . . ? P1 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N11 C12 C13 112.6(3) . . ? N11 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? N11 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C12 C13 S14 112.8(2) . . ? C12 C13 H13A 109.0 . . ? S14 C13 H13A 109.0 . . ? C12 C13 H13B 109.0 . . ? S14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C16 C15 S14 112.1(2) . . ? C16 C15 H15A 109.2 . . ? S14 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? S14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? N11 C16 C15 112.5(3) . . ? N11 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? N11 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N21 C21 P1 113.88(19) . . ? N21 C21 H21A 108.8 . . ? P1 C21 H21A 108.8 . . ? N21 C21 H21B 108.8 . . ? P1 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? N21 C22 C23 110.8(2) . . ? N21 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? N21 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C22 C23 S24 112.0(2) . . ? C22 C23 H23A 109.2 . . ? S24 C23 H23A 109.2 . . ? C22 C23 H23B 109.2 . . ? S24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C26 C25 S24 112.9(2) . . ? C26 C25 H25A 109.0 . . ? S24 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? S24 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? N21 C26 C25 110.9(2) . . ? N21 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? N21 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.0 . . ? N31 C31 P1 115.54(19) . . ? N31 C31 H31A 108.4 . . ? P1 C31 H31A 108.4 . . ? N31 C31 H31B 108.4 . . ? P1 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? N31 C32 C33 113.1(2) . . ? N31 C32 H32A 109.0 . . ? C33 C32 H32A 109.0 . . ? N31 C32 H32B 109.0 . . ? C33 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C32 C33 S34 111.9(2) . . ? C32 C33 H33A 109.2 . . ? S34 C33 H33A 109.2 . . ? C32 C33 H33B 109.2 . . ? S34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C36 C35 S34 112.5(2) . . ? C36 C35 H35A 109.1 . . ? S34 C35 H35A 109.1 . . ? C36 C35 H35B 109.1 . . ? S34 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? N31 C36 C35 112.7(2) . . ? N31 C36 H36A 109.1 . . ? C35 C36 H36A 109.1 . . ? N31 C36 H36B 109.1 . . ? C35 C36 H36B 109.1 . . ? H36A C36 H36B 107.8 . . ? C13 S14 C15 96.55(15) . . ? C23 S24 C25 96.61(14) . . ? C35 S34 C33 96.12(13) . . ? C41 N41 C51 118.8(2) . . ? C41 N41 Cu1 127.65(19) . . ? C51 N41 Cu1 112.47(18) . . ? C50 N42 C52 118.7(2) . . ? C50 N42 Cu1 129.03(18) . . ? C52 N42 Cu1 112.14(17) . . ? N41 C41 C42 121.3(3) . . ? N41 C41 C53 118.1(3) . . ? C42 C41 C53 120.6(3) . . ? C43 C42 C41 120.3(3) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 119.5(3) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C51 C44 C43 117.1(3) . . ? C51 C44 C45 119.3(3) . . ? C43 C44 C45 123.6(3) . . ? C46 C45 C44 121.2(3) . . ? C46 C45 H45 119.4 . . ? C44 C45 H45 119.4 . . ? C45 C46 C47 121.0(3) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C48 C47 C52 116.6(3) . . ? C48 C47 C46 123.9(3) . . ? C52 C47 C46 119.5(3) . . ? C49 C48 C47 120.1(3) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C48 C49 C50 120.0(3) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? N42 C50 C49 121.4(3) . . ? N42 C50 C54 116.9(2) . . ? C49 C50 C54 121.8(3) . . ? N41 C51 C44 123.0(2) . . ? N41 C51 C52 117.4(2) . . ? C44 C51 C52 119.6(2) . . ? N42 C52 C47 123.1(3) . . ? N42 C52 C51 117.5(2) . . ? C47 C52 C51 119.4(2) . . ? C41 C53 H53A 109.5 . . ? C41 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C41 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C50 C54 H54A 109.5 . . ? C50 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C50 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.851 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.339 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.122