Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name L.Thompson 'Tareque S. M. Abedin' 'Loiuse N. Dawe' _publ_contact_author_name L.Thompson _publ_contact_author_address ; Department of Chemistry Memorial University of St John's Newfoundland A1B 3X7 CANADA ; _publ_contact_author_email LTHOMP@MUN.CA _publ_section_title ; ; # Attachment 'LND985A.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 664563' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C163.40 H120 Cu8.50 F25.80 N54 O19.20 P3.60 S1.40' _chemical_formula_weight 4333.79 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' Cu Cu 0.3201 1.2651 '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' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n' _symmetry_space_group_name_Hall '-P 4bc' _symmetry_Int_Tables_number 86 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/2' '-x+1/2, -y+1/2, z' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'y, -x-1/2, -z-1/2' 'x-1/2, y-1/2, -z' '-y-1/2, x, -z-1/2' _cell_length_a 20.580(3) _cell_length_b 20.580(3) _cell_length_c 22.970(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9729(3) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 36294 _cell_measurement_theta_min 2.1686 _cell_measurement_theta_max 31.0074 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4374.2 _exptl_absorpt_coefficient_mu 1.053 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.7165 _exptl_absorpt_correction_T_max 0.8284 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 75221 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9535 _reflns_number_gt 8635 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.2000P)^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 9535 _refine_ls_number_parameters 722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.1174 _refine_ls_wR_factor_ref 0.3717 _refine_ls_wR_factor_gt 0.3616 _refine_ls_goodness_of_fit_ref 1.683 _refine_ls_restrained_S_all 1.683 _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 0.48522(3) 0.65591(3) 0.21141(3) 0.0430(3) Uani 1 1 d . . . Cu2 Cu 0.66170(3) 0.57305(3) 0.23245(3) 0.0439(3) Uani 1 1 d . . . Cu3 Cu 0.7500 0.7500 0.2500 0.0641(8) Uani 0.50 4 d SP . . S1 S 0.8186(2) 0.3631(3) 0.05182(17) 0.0627(12) Uani 0.35 1 d P . . P1 P 0.10890(14) 0.34120(11) 0.06802(11) 0.0597(7) Uani 0.65 1 d P . . P2 P 0.5000 0.5000 0.0000 0.0607(12) Uani 0.50 2 d SP . . F1 F 0.7069(9) 0.3189(7) 0.0244(14) 0.204(15) Uani 0.35 1 d P . . F2 F 0.7121(13) 0.4063(9) -0.0106(7) 0.178(13) Uani 0.35 1 d P . . F3 F 0.7041(6) 0.4102(6) 0.0706(5) 0.077(3) Uani 0.35 1 d P . . F4 F 0.0863(5) 0.3726(4) 0.0077(3) 0.114(3) Uani 0.65 1 d P . . F5 F 0.1307(3) 0.3082(4) 0.1283(3) 0.0839(19) Uani 0.65 1 d P . . F6 F 0.1044(4) 0.4114(3) 0.0987(3) 0.096(3) Uani 0.65 1 d P . . F7 F 0.0341(3) 0.3334(3) 0.0885(3) 0.0780(18) Uani 0.65 1 d P . . F8 F 0.1036(4) 0.2718(3) 0.0378(3) 0.086(2) Uani 0.65 1 d P . . F9 F 0.1818(4) 0.3471(5) 0.0498(3) 0.133(4) Uani 0.65 1 d P . . F10 F 0.5246(4) 0.5097(4) 0.0656(3) 0.073(2) Uani 0.50 1 d P . . F11 F 0.4322(5) 0.5315(5) 0.0160(3) 0.082(2) Uani 0.50 1 d P . . F12 F 0.4765(5) 0.4282(4) 0.0133(4) 0.087(3) Uani 0.50 1 d P . . O1 O 0.57425(17) 0.61953(17) 0.18929(15) 0.0442(8) Uani 1 1 d . . . O2 O 0.76758(19) 0.53355(19) 0.22896(15) 0.0475(9) Uani 1 1 d . . . O3 O 0.70004(18) 0.65606(18) 0.26930(15) 0.0460(9) Uani 1 1 d . . . O4 O 0.8459(6) 0.4304(6) 0.0522(5) 0.060(3) Uani 0.35 1 d P . . O5 O 0.8475(6) 0.3232(5) 0.0078(4) 0.046(2) Uani 0.35 1 d P . . O6 O 0.8170(6) 0.3465(8) 0.1110(4) 0.074(4) Uani 0.35 1 d P . . O7 O 0.9293(14) 0.5041(10) 0.0263(10) 0.109(10) Uani 0.25 1 d P . . O8 O 0.1276(5) 0.5544(7) 0.0606(5) 0.103(4) Uani 0.50 1 d P . . N1 N 0.4087(2) 0.7204(2) 0.2048(2) 0.0457(10) Uani 1 1 d . . . N2 N 0.4532(3) 0.7403(3) 0.0527(2) 0.0783(18) Uani 1 1 d . . . H7 H 0.4854 0.7271 0.0305 0.094 Uiso 1 1 calc R . . H8 H 0.4231 0.7661 0.0384 0.094 Uiso 1 1 calc R . . N3 N 0.4932(2) 0.6824(2) 0.1326(2) 0.0451(10) Uani 1 1 d . . . N4 N 0.5447(2) 0.6627(2) 0.1001(2) 0.0498(11) Uani 1 1 d . . . N5 N 0.6876(2) 0.5803(2) 0.14889(19) 0.0430(9) Uani 1 1 d . . . N6 N 0.8403(2) 0.5003(2) 0.1610(2) 0.0498(11) Uani 1 1 d . . . N7 N 0.8766(2) 0.4757(2) 0.20711(19) 0.0455(10) Uani 1 1 d . . . N8 N 0.9546(3) 0.4451(3) 0.1393(2) 0.0715(16) Uani 1 1 d . . . H12 H 0.9320 0.4621 0.1106 0.086 Uiso 1 1 calc R . . H13 H 0.9921 0.4261 0.1321 0.086 Uiso 1 1 calc R . . N9 N 0.9458(2) 0.4356(2) 0.2962(2) 0.0512(11) Uani 1 1 d . . . N10 N 0.6136(2) 0.4850(2) 0.2288(2) 0.0484(11) Uani 1 1 d . . . N11 N 0.6041(3) 0.4924(3) 0.3866(2) 0.0779(18) Uani 1 1 d . . . H26 H 0.6173 0.5196 0.4137 0.093 Uiso 1 1 calc R . . H27 H 0.5840 0.4563 0.3964 0.093 Uiso 1 1 calc R . . N12 N 0.6442(2) 0.5585(2) 0.3122(2) 0.0513(11) Uani 1 1 d . . . N13 N 0.6665(2) 0.6017(2) 0.35304(19) 0.0524(11) Uani 1 1 d . . . N14 N 0.7500 0.7500 0.3331(3) 0.0523(15) Uani 1 2 d S . . C1 C 0.3721(3) 0.7452(3) 0.2473(3) 0.0560(13) Uani 1 1 d . . . H1 H 0.3787 0.7298 0.2859 0.067 Uiso 1 1 calc R . . C2 C 0.3246(3) 0.7926(3) 0.2383(3) 0.0511(13) Uani 1 1 d . . . C3 C 0.2893(3) 0.8186(3) 0.2849(3) 0.0628(16) Uani 1 1 d . . . H2 H 0.2979 0.8047 0.3236 0.075 Uiso 1 1 calc R . . C4 C 0.2418(3) 0.8647(3) 0.2741(4) 0.0690(19) Uani 1 1 d . . . H3 H 0.2177 0.8823 0.3056 0.083 Uiso 1 1 calc R . . C5 C 0.2291(3) 0.8851(4) 0.2185(4) 0.0703(18) Uani 1 1 d . . . H4 H 0.1963 0.9168 0.2119 0.084 Uiso 1 1 calc R . . C6 C 0.2645(3) 0.8595(3) 0.1704(3) 0.0633(16) Uani 1 1 d . . . H5 H 0.2552 0.8738 0.1319 0.076 Uiso 1 1 calc R . . C7 C 0.3131(3) 0.8131(3) 0.1802(3) 0.0571(14) Uani 1 1 d . . . C8 C 0.3525(3) 0.7863(3) 0.1362(3) 0.0646(16) Uani 1 1 d . . . H6 H 0.3455 0.7984 0.0968 0.078 Uiso 1 1 calc R . . C9 C 0.3996(3) 0.7441(3) 0.1493(2) 0.0512(13) Uani 1 1 d . . . C10 C 0.4499(3) 0.7210(3) 0.1083(3) 0.0564(14) Uani 1 1 d . . . C11 C 0.5845(3) 0.6305(2) 0.1348(2) 0.0412(10) Uani 1 1 d . . . C12 C 0.6467(2) 0.6061(2) 0.1104(2) 0.0425(11) Uani 1 1 d . . . C13 C 0.6608(3) 0.6076(3) 0.0502(2) 0.0542(14) Uani 1 1 d . . . H9 H 0.6306 0.6253 0.0233 0.065 Uiso 1 1 calc R . . C14 C 0.7182(3) 0.5833(3) 0.0319(3) 0.0600(15) Uani 1 1 d . . . H10 H 0.7290 0.5840 -0.0083 0.072 Uiso 1 1 calc R . . C15 C 0.7615(3) 0.5573(3) 0.0725(2) 0.0537(13) Uani 1 1 d . . . H11 H 0.8022 0.5407 0.0600 0.064 Uiso 1 1 calc R . . C16 C 0.7452(2) 0.5557(3) 0.1298(2) 0.0449(11) Uani 1 1 d . . . C17 C 0.7857(2) 0.5288(2) 0.1771(2) 0.0415(11) Uani 1 1 d . . . C18 C 0.9323(3) 0.4480(3) 0.1932(2) 0.0484(12) Uani 1 1 d . . . C19 C 0.9706(2) 0.4219(3) 0.2427(2) 0.0443(11) Uani 1 1 d . . . C20 C 1.0268(3) 0.3882(3) 0.2344(2) 0.0482(12) Uani 1 1 d . . . H14 H 1.0421 0.3801 0.1961 0.058 Uiso 1 1 calc R . . C21 C 1.0621(3) 0.3654(3) 0.2831(2) 0.0484(12) Uani 1 1 d . . . C22 C 1.1209(3) 0.3300(3) 0.2781(3) 0.0635(16) Uani 1 1 d . . . H15 H 1.1380 0.3187 0.2410 0.076 Uiso 1 1 calc R . . C23 C 1.1527(4) 0.3124(4) 0.3288(3) 0.075(2) Uani 1 1 d . . . H16 H 1.1923 0.2888 0.3263 0.090 Uiso 1 1 calc R . . C24 C 1.1283(4) 0.3282(4) 0.3829(4) 0.081(2) Uani 1 1 d . . . H17 H 1.1509 0.3136 0.4165 0.097 Uiso 1 1 calc R . . C25 C 1.0736(4) 0.3638(4) 0.3900(3) 0.082(2) Uani 1 1 d . . . H18 H 1.0588 0.3757 0.4276 0.098 Uiso 1 1 calc R . . C26 C 1.0386(3) 0.3829(3) 0.3386(3) 0.0574(14) Uani 1 1 d . . . C27 C 0.9788(3) 0.4169(3) 0.3416(3) 0.0590(15) Uani 1 1 d . . . H19 H 0.9617 0.4266 0.3790 0.071 Uiso 1 1 calc R . . C28 C 0.5951(3) 0.4527(3) 0.1827(3) 0.0566(14) Uani 1 1 d . . . H20 H 0.6100 0.4676 0.1460 0.068 Uiso 1 1 calc R . . C29 C 0.5543(3) 0.3968(3) 0.1834(3) 0.0631(17) Uani 1 1 d . . . C30 C 0.5375(4) 0.3649(3) 0.1333(4) 0.081(2) Uani 1 1 d . . . H21 H 0.5547 0.3777 0.0967 0.097 Uiso 1 1 calc R . . C31 C 0.4935(4) 0.3121(4) 0.1378(4) 0.078(2) Uani 1 1 d . . . H22 H 0.4781 0.2910 0.1037 0.094 Uiso 1 1 calc R . . C32 C 0.4736(4) 0.2921(3) 0.1914(5) 0.086(3) Uani 1 1 d . . . H23 H 0.4464 0.2549 0.1938 0.103 Uiso 1 1 calc R . . C33 C 0.4906(3) 0.3225(3) 0.2415(4) 0.075(2) Uani 1 1 d . . . H24 H 0.4744 0.3076 0.2779 0.090 Uiso 1 1 calc R . . C34 C 0.5330(3) 0.3768(3) 0.2389(3) 0.0615(16) Uani 1 1 d . . . C35 C 0.5525(3) 0.4111(3) 0.2886(3) 0.0603(15) Uani 1 1 d . . . H25 H 0.5388 0.3975 0.3261 0.072 Uiso 1 1 calc R . . C36 C 0.5912(3) 0.4639(3) 0.2824(3) 0.0533(13) Uani 1 1 d . . . C37 C 0.6146(3) 0.5060(3) 0.3307(2) 0.0553(14) Uani 1 1 d . . . C38 C 0.6945(3) 0.6498(3) 0.3240(2) 0.0495(13) Uani 1 1 d . . . C39 C 0.7224(3) 0.6998(3) 0.3618(2) 0.0496(12) Uani 1 1 d . . . C40 C 0.7224(3) 0.6986(3) 0.4212(3) 0.0604(15) Uani 1 1 d . . . H28 H 0.7038 0.6630 0.4415 0.073 Uiso 1 1 calc R . . C41 C 0.7500 0.7500 0.4515(3) 0.064(2) Uani 1 2 d S . . H29 H 0.7500 0.7500 0.4929 0.077 Uiso 1 2 calc SR . . C42 C 0.7289(10) 0.3782(11) 0.0315(19) 0.115(12) Uani 0.35 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 Cu1 0.0417(4) 0.0449(4) 0.0423(5) 0.0017(2) 0.0009(2) 0.0014(2) Cu2 0.0508(5) 0.0432(4) 0.0377(5) 0.0017(2) 0.0012(2) -0.0011(3) Cu3 0.0650(12) 0.0650(12) 0.0624(18) 0.000 0.000 0.000 S1 0.070(3) 0.081(3) 0.037(2) -0.0100(18) 0.0005(17) 0.020(2) P1 0.0844(18) 0.0453(12) 0.0493(13) 0.0047(9) 0.0384(12) 0.0032(11) P2 0.078(3) 0.064(3) 0.040(2) 0.0075(18) -0.009(2) -0.023(2) F1 0.132(14) 0.060(8) 0.42(4) -0.054(15) -0.17(2) 0.009(9) F2 0.32(3) 0.128(13) 0.091(10) -0.061(10) -0.139(16) 0.133(17) F3 0.065(7) 0.078(7) 0.089(8) -0.033(6) 0.008(6) 0.007(6) F4 0.221(10) 0.075(4) 0.046(3) 0.014(3) 0.011(4) 0.021(5) F5 0.083(4) 0.108(5) 0.060(4) 0.017(3) 0.015(3) 0.014(4) F6 0.169(7) 0.058(3) 0.062(4) -0.014(3) 0.035(4) -0.040(4) F7 0.060(3) 0.087(4) 0.086(4) -0.016(3) 0.023(3) 0.025(3) F8 0.129(6) 0.042(3) 0.087(4) -0.010(3) 0.058(4) -0.010(3) F9 0.102(5) 0.211(10) 0.086(5) -0.053(6) 0.074(5) -0.081(6) F10 0.083(5) 0.093(6) 0.043(3) 0.006(4) -0.016(3) -0.028(4) F11 0.086(6) 0.108(7) 0.051(4) 0.009(4) 0.002(4) 0.003(5) F12 0.126(7) 0.052(4) 0.084(6) 0.016(4) -0.063(5) -0.021(4) O1 0.046(2) 0.047(2) 0.0399(18) 0.0030(14) 0.0024(15) 0.0026(15) O2 0.048(2) 0.052(2) 0.043(2) 0.0017(15) -0.0009(15) 0.0098(16) O3 0.049(2) 0.050(2) 0.039(2) -0.0001(15) 0.0013(15) -0.0005(16) O4 0.055(7) 0.070(8) 0.054(7) 0.004(5) 0.007(5) 0.025(6) O5 0.082(7) 0.038(5) 0.017(4) -0.011(3) 0.012(4) 0.009(5) O6 0.048(6) 0.149(13) 0.024(5) -0.003(6) 0.006(4) 0.000(7) O7 0.16(2) 0.077(13) 0.090(15) 0.036(11) -0.102(16) -0.016(14) O8 0.061(6) 0.162(12) 0.084(7) -0.075(8) 0.010(5) 0.024(7) N1 0.039(2) 0.047(2) 0.052(3) -0.0008(19) -0.0028(18) 0.0026(18) N2 0.090(4) 0.090(4) 0.055(3) 0.010(3) -0.002(3) 0.038(3) N3 0.042(2) 0.049(2) 0.045(2) 0.0040(19) 0.0013(17) 0.0056(18) N4 0.043(2) 0.060(3) 0.046(2) 0.006(2) -0.0019(18) 0.002(2) N5 0.047(2) 0.037(2) 0.045(2) -0.0003(16) 0.0002(18) -0.0044(17) N6 0.048(3) 0.052(3) 0.049(3) -0.007(2) 0.0003(19) 0.005(2) N7 0.044(2) 0.047(3) 0.045(2) -0.0006(18) 0.0017(17) 0.0060(19) N8 0.069(4) 0.096(4) 0.049(3) 0.001(3) 0.006(2) 0.028(3) N9 0.055(3) 0.045(3) 0.054(3) 0.006(2) 0.002(2) 0.004(2) N10 0.052(3) 0.043(2) 0.051(3) 0.0058(19) 0.0000(19) -0.0014(19) N11 0.099(5) 0.085(4) 0.050(3) 0.016(3) 0.007(3) -0.034(3) N12 0.055(3) 0.054(3) 0.045(3) 0.000(2) -0.001(2) 0.000(2) N13 0.059(3) 0.065(3) 0.033(2) 0.002(2) 0.0015(18) -0.008(2) N14 0.058(4) 0.060(4) 0.039(3) 0.000 0.000 -0.001(3) C1 0.040(3) 0.058(3) 0.069(4) 0.000(3) -0.003(3) -0.003(2) C2 0.041(3) 0.051(3) 0.061(3) -0.006(2) 0.000(2) -0.002(2) C3 0.046(3) 0.064(4) 0.078(4) -0.011(3) 0.005(3) -0.009(3) C4 0.051(4) 0.058(4) 0.098(5) -0.016(3) 0.010(3) -0.006(3) C5 0.051(4) 0.063(4) 0.097(5) 0.006(4) -0.001(3) 0.008(3) C6 0.053(3) 0.066(4) 0.071(4) 0.006(3) -0.004(3) 0.016(3) C7 0.048(3) 0.055(3) 0.068(4) 0.002(3) 0.001(3) 0.005(2) C8 0.058(4) 0.072(4) 0.065(4) 0.012(3) -0.012(3) 0.011(3) C9 0.051(3) 0.052(3) 0.051(3) 0.001(2) -0.002(2) 0.004(2) C10 0.056(3) 0.065(4) 0.048(3) 0.005(3) -0.005(2) 0.010(3) C11 0.046(3) 0.044(3) 0.034(2) 0.0010(19) -0.0008(19) -0.003(2) C12 0.043(3) 0.040(3) 0.044(3) 0.003(2) 0.001(2) -0.004(2) C13 0.050(3) 0.069(4) 0.044(3) 0.003(3) -0.001(2) 0.003(3) C14 0.056(3) 0.078(4) 0.046(3) 0.007(3) 0.006(3) 0.003(3) C15 0.049(3) 0.064(3) 0.048(3) -0.002(2) 0.003(2) -0.002(3) C16 0.042(3) 0.044(3) 0.049(3) -0.003(2) -0.003(2) -0.001(2) C17 0.047(3) 0.036(2) 0.041(3) -0.0003(19) 0.001(2) 0.000(2) C18 0.049(3) 0.052(3) 0.044(3) 0.004(2) 0.003(2) 0.013(2) C19 0.042(3) 0.043(3) 0.048(3) 0.004(2) 0.002(2) 0.000(2) C20 0.050(3) 0.050(3) 0.045(3) 0.001(2) 0.003(2) 0.004(2) C21 0.042(3) 0.046(3) 0.057(3) 0.003(2) 0.003(2) 0.004(2) C22 0.051(3) 0.066(4) 0.074(4) 0.004(3) 0.001(3) 0.006(3) C23 0.060(4) 0.075(4) 0.088(5) 0.028(4) 0.008(3) 0.021(3) C24 0.059(4) 0.101(6) 0.083(5) 0.023(4) -0.011(4) 0.023(4) C25 0.084(5) 0.106(6) 0.056(4) 0.018(4) -0.001(3) 0.020(4) C26 0.055(3) 0.057(3) 0.060(3) 0.010(3) 0.002(3) 0.004(3) C27 0.058(3) 0.069(4) 0.050(3) 0.000(3) -0.001(3) 0.010(3) C28 0.056(3) 0.052(3) 0.061(4) 0.007(3) -0.005(3) -0.004(3) C29 0.066(4) 0.041(3) 0.082(4) 0.003(3) -0.022(3) -0.001(3) C30 0.093(5) 0.059(4) 0.091(6) 0.007(4) -0.026(4) -0.016(4) C31 0.081(5) 0.059(4) 0.095(6) 0.001(4) -0.015(4) -0.010(4) C32 0.075(5) 0.044(4) 0.139(8) 0.011(4) -0.026(5) -0.011(3) C33 0.057(4) 0.052(4) 0.116(6) 0.011(4) -0.009(4) -0.012(3) C34 0.053(3) 0.045(3) 0.087(5) 0.009(3) -0.005(3) 0.000(3) C35 0.052(3) 0.056(4) 0.074(4) 0.016(3) 0.000(3) 0.004(3) C36 0.044(3) 0.053(3) 0.064(3) 0.013(3) -0.002(2) 0.001(2) C37 0.046(3) 0.077(4) 0.043(3) 0.012(3) 0.005(2) -0.007(3) C38 0.047(3) 0.056(3) 0.045(3) -0.002(2) 0.004(2) 0.003(2) C39 0.053(3) 0.053(3) 0.043(3) -0.002(2) 0.007(2) 0.002(2) C40 0.074(4) 0.061(4) 0.047(3) -0.002(3) 0.007(3) -0.009(3) C41 0.084(6) 0.070(6) 0.038(4) 0.000 0.000 -0.013(5) C42 0.039(10) 0.061(13) 0.25(4) 0.015(19) 0.025(16) 0.000(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 N3 1.898(5) . ? Cu1 N7 1.997(4) 6_576 ? Cu1 O1 2.043(4) . ? Cu1 N1 2.064(4) . ? Cu1 O2 2.312(4) 6_576 ? Cu1 N9 2.336(5) 6_576 ? Cu2 N12 1.891(5) . ? Cu2 N5 1.998(4) . ? Cu2 O3 2.063(4) . ? Cu2 N10 2.067(5) . ? Cu2 O1 2.266(4) . ? Cu2 O2 2.327(4) . ? Cu3 N14 1.908(6) . ? Cu3 N14 1.908(6) 6_576 ? Cu3 O3 2.234(4) 3_665 ? Cu3 O3 2.234(4) 6_576 ? Cu3 O3 2.234(4) 8_756 ? Cu3 O3 2.234(4) . ? S1 O6 1.402(12) . ? S1 O5 1.432(9) . ? S1 O4 1.494(15) . ? S1 C42 1.93(2) . ? P1 F9 1.562(7) . ? P1 F8 1.592(6) . ? P1 F4 1.597(7) . ? P1 F5 1.606(7) . ? P1 F6 1.610(6) . ? P1 F7 1.619(6) . ? P2 F11 1.581(9) 5_665 ? P2 F11 1.581(9) . ? P2 F12 1.585(8) . ? P2 F12 1.585(8) 5_665 ? P2 F10 1.602(7) . ? P2 F10 1.602(7) 5_665 ? F1 C42 1.31(3) . ? F2 C42 1.18(4) . ? F3 C42 1.23(3) . ? O1 C11 1.290(6) . ? O2 C17 1.252(6) . ? O2 Cu1 2.312(4) 8_756 ? O3 C38 1.269(6) . ? N1 C1 1.336(8) . ? N1 C9 1.378(7) . ? N2 C10 1.339(8) . ? N3 C10 1.317(7) . ? N3 N4 1.358(6) . ? N4 C11 1.320(7) . ? N5 C12 1.332(7) . ? N5 C16 1.361(7) . ? N6 C17 1.319(7) . ? N6 N7 1.391(7) . ? N7 C18 1.321(7) . ? N7 Cu1 1.997(4) 8_756 ? N8 C18 1.323(8) . ? N9 C27 1.303(8) . ? N9 C19 1.360(8) . ? N9 Cu1 2.336(5) 8_756 ? N10 C28 1.306(8) . ? N10 C36 1.383(7) . ? N11 C37 1.331(8) . ? N12 C37 1.311(8) . ? N12 N13 1.371(7) . ? N13 C38 1.325(7) . ? N14 C39 1.351(6) . ? N14 C39 1.351(6) 3_665 ? C1 C2 1.396(8) . ? C2 C3 1.400(9) . ? C2 C7 1.418(9) . ? C3 C4 1.384(10) . ? C4 C5 1.370(11) . ? C5 C6 1.424(10) . ? C6 C7 1.402(9) . ? C7 C8 1.408(9) . ? C8 C9 1.336(8) . ? C9 C10 1.478(8) . ? C11 C12 1.484(7) . ? C12 C13 1.413(8) . ? C13 C14 1.349(9) . ? C14 C15 1.396(9) . ? C15 C16 1.358(8) . ? C16 C17 1.478(7) . ? C18 C19 1.484(8) . ? C19 C20 1.360(8) . ? C20 C21 1.416(8) . ? C21 C26 1.409(8) . ? C21 C22 1.418(9) . ? C22 C23 1.384(10) . ? C23 C24 1.379(11) . ? C24 C25 1.353(11) . ? C25 C26 1.437(9) . ? C26 C27 1.418(9) . ? C28 C29 1.424(9) . ? C29 C30 1.370(10) . ? C29 C34 1.409(10) . ? C30 C31 1.416(11) . ? C31 C32 1.362(12) . ? C32 C33 1.356(12) . ? C33 C34 1.419(9) . ? C34 C35 1.401(10) . ? C35 C36 1.354(9) . ? C36 C37 1.488(9) . ? C38 C39 1.463(8) . ? C39 C40 1.365(8) . ? C40 C41 1.387(7) . ? C41 C40 1.387(7) 3_665 ? 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 N7 177.04(19) . 6_576 ? N3 Cu1 O1 77.90(16) . . ? N7 Cu1 O1 101.45(17) 6_576 . ? N3 Cu1 N1 79.13(18) . . ? N7 Cu1 N1 102.07(19) 6_576 . ? O1 Cu1 N1 154.29(17) . . ? N3 Cu1 O2 109.41(17) . 6_576 ? N7 Cu1 O2 73.43(16) 6_576 6_576 ? O1 Cu1 O2 90.64(15) . 6_576 ? N1 Cu1 O2 86.21(16) . 6_576 ? N3 Cu1 N9 102.95(19) . 6_576 ? N7 Cu1 N9 74.16(18) 6_576 6_576 ? O1 Cu1 N9 92.57(16) . 6_576 ? N1 Cu1 N9 103.72(18) . 6_576 ? O2 Cu1 N9 147.43(15) 6_576 6_576 ? N12 Cu2 N5 173.5(2) . . ? N12 Cu2 O3 78.86(18) . . ? N5 Cu2 O3 103.32(15) . . ? N12 Cu2 N10 79.0(2) . . ? N5 Cu2 N10 98.89(18) . . ? O3 Cu2 N10 157.78(16) . . ? N12 Cu2 O1 109.82(17) . . ? N5 Cu2 O1 76.15(16) . . ? O3 Cu2 O1 97.68(14) . . ? N10 Cu2 O1 88.38(17) . . ? N12 Cu2 O2 99.02(17) . . ? N5 Cu2 O2 75.08(16) . . ? O3 Cu2 O2 86.86(15) . . ? N10 Cu2 O2 98.11(16) . . ? O1 Cu2 O2 151.15(12) . . ? N14 Cu3 N14 180.000(1) . 6_576 ? N14 Cu3 O3 78.56(9) . 3_665 ? N14 Cu3 O3 101.44(9) 6_576 3_665 ? N14 Cu3 O3 101.44(9) . 6_576 ? N14 Cu3 O3 78.56(9) 6_576 6_576 ? O3 Cu3 O3 92.26(3) 3_665 6_576 ? N14 Cu3 O3 101.44(9) . 8_756 ? N14 Cu3 O3 78.56(9) 6_576 8_756 ? O3 Cu3 O3 92.26(3) 3_665 8_756 ? O3 Cu3 O3 157.11(18) 6_576 8_756 ? N14 Cu3 O3 78.56(9) . . ? N14 Cu3 O3 101.44(9) 6_576 . ? O3 Cu3 O3 157.12(18) 3_665 . ? O3 Cu3 O3 92.25(4) 6_576 . ? O3 Cu3 O3 92.26(3) 8_756 . ? O6 S1 O5 123.6(8) . . ? O6 S1 O4 103.2(9) . . ? O5 S1 O4 112.4(7) . . ? O6 S1 C42 104.5(13) . . ? O5 S1 C42 108.6(13) . . ? O4 S1 C42 102.2(8) . . ? F9 P1 F8 91.1(4) . . ? F9 P1 F4 90.8(5) . . ? F8 P1 F4 87.9(4) . . ? F9 P1 F5 89.8(5) . . ? F8 P1 F5 90.9(4) . . ? F4 P1 F5 178.7(5) . . ? F9 P1 F6 95.9(5) . . ? F8 P1 F6 172.7(5) . . ? F4 P1 F6 90.0(4) . . ? F5 P1 F6 91.1(4) . . ? F9 P1 F7 178.2(5) . . ? F8 P1 F7 88.4(4) . . ? F4 P1 F7 90.9(5) . . ? F5 P1 F7 88.5(4) . . ? F6 P1 F7 84.6(4) . . ? F11 P2 F11 179.997(1) 5_665 . ? F11 P2 F12 86.1(5) 5_665 . ? F11 P2 F12 93.9(5) . . ? F11 P2 F12 93.9(5) 5_665 5_665 ? F11 P2 F12 86.1(5) . 5_665 ? F12 P2 F12 179.998(1) . 5_665 ? F11 P2 F10 89.5(4) 5_665 . ? F11 P2 F10 90.5(4) . . ? F12 P2 F10 91.8(4) . . ? F12 P2 F10 88.2(4) 5_665 . ? F11 P2 F10 90.5(4) 5_665 5_665 ? F11 P2 F10 89.5(4) . 5_665 ? F12 P2 F10 88.2(4) . 5_665 ? F12 P2 F10 91.8(4) 5_665 5_665 ? F10 P2 F10 179.997(1) . 5_665 ? C11 O1 Cu1 108.9(3) . . ? C11 O1 Cu2 111.6(3) . . ? Cu1 O1 Cu2 139.28(18) . . ? C17 O2 Cu1 109.1(3) . 8_756 ? C17 O2 Cu2 109.8(3) . . ? Cu1 O2 Cu2 140.14(17) 8_756 . ? C38 O3 Cu2 106.7(4) . . ? C38 O3 Cu3 109.0(4) . . ? Cu2 O3 Cu3 144.20(17) . . ? C1 N1 C9 117.6(5) . . ? C1 N1 Cu1 128.5(4) . . ? C9 N1 Cu1 113.6(4) . . ? C10 N3 N4 118.4(5) . . ? C10 N3 Cu1 121.2(4) . . ? N4 N3 Cu1 120.4(3) . . ? C11 N4 N3 107.7(4) . . ? C12 N5 C16 119.0(5) . . ? C12 N5 Cu2 119.9(4) . . ? C16 N5 Cu2 121.0(4) . . ? C17 N6 N7 113.9(5) . . ? C18 N7 N6 116.1(4) . . ? C18 N7 Cu1 124.0(4) . 8_756 ? N6 N7 Cu1 119.9(3) . 8_756 ? C27 N9 C19 117.8(5) . . ? C27 N9 Cu1 130.9(4) . 8_756 ? C19 N9 Cu1 111.1(4) . 8_756 ? C28 N10 C36 117.6(5) . . ? C28 N10 Cu2 128.2(4) . . ? C36 N10 Cu2 113.5(4) . . ? C37 N12 N13 118.0(5) . . ? C37 N12 Cu2 122.2(4) . . ? N13 N12 Cu2 119.7(4) . . ? C38 N13 N12 106.6(4) . . ? C39 N14 C39 121.5(7) . 3_665 ? C39 N14 Cu3 119.2(3) . . ? C39 N14 Cu3 119.2(3) 3_665 . ? N1 C1 C2 123.6(6) . . ? C1 C2 C3 121.1(6) . . ? C1 C2 C7 117.7(6) . . ? C3 C2 C7 121.2(6) . . ? C4 C3 C2 119.4(7) . . ? C5 C4 C3 120.9(7) . . ? C4 C5 C6 120.8(6) . . ? C7 C6 C5 119.4(6) . . ? C6 C7 C8 124.2(6) . . ? C6 C7 C2 118.3(6) . . ? C8 C7 C2 117.5(5) . . ? C9 C8 C7 120.7(6) . . ? C8 C9 N1 122.5(6) . . ? C8 C9 C10 125.1(6) . . ? N1 C9 C10 112.2(5) . . ? N3 C10 N2 123.3(6) . . ? N3 C10 C9 113.5(5) . . ? N2 C10 C9 123.1(5) . . ? O1 C11 N4 124.9(5) . . ? O1 C11 C12 116.6(4) . . ? N4 C11 C12 118.5(4) . . ? N5 C12 C13 121.8(5) . . ? N5 C12 C11 115.5(4) . . ? C13 C12 C11 122.6(5) . . ? C14 C13 C12 118.5(5) . . ? C13 C14 C15 119.5(6) . . ? C16 C15 C14 119.9(6) . . ? C15 C16 N5 121.2(5) . . ? C15 C16 C17 125.7(5) . . ? N5 C16 C17 113.1(5) . . ? O2 C17 N6 123.7(5) . . ? O2 C17 C16 120.2(5) . . ? N6 C17 C16 116.1(5) . . ? N7 C18 N8 123.2(5) . . ? N7 C18 C19 115.7(5) . . ? N8 C18 C19 121.1(5) . . ? N9 C19 C20 123.5(5) . . ? N9 C19 C18 114.6(5) . . ? C20 C19 C18 121.9(5) . . ? C19 C20 C21 119.6(5) . . ? C26 C21 C20 117.0(5) . . ? C26 C21 C22 119.9(6) . . ? C20 C21 C22 123.0(5) . . ? C23 C22 C21 117.9(6) . . ? C24 C23 C22 121.7(6) . . ? C25 C24 C23 122.6(7) . . ? C24 C25 C26 117.8(7) . . ? C21 C26 C27 117.9(5) . . ? C21 C26 C25 120.0(6) . . ? C27 C26 C25 122.0(6) . . ? N9 C27 C26 123.9(6) . . ? N10 C28 C29 125.0(6) . . ? C30 C29 C34 122.7(7) . . ? C30 C29 C28 121.8(7) . . ? C34 C29 C28 115.5(6) . . ? C29 C30 C31 117.9(8) . . ? C32 C31 C30 119.3(8) . . ? C33 C32 C31 123.4(7) . . ? C32 C33 C34 119.0(8) . . ? C35 C34 C29 119.9(6) . . ? C35 C34 C33 122.6(7) . . ? C29 C34 C33 117.4(7) . . ? C36 C35 C34 119.2(6) . . ? C35 C36 N10 122.8(6) . . ? C35 C36 C37 125.4(6) . . ? N10 C36 C37 111.9(5) . . ? N12 C37 N11 124.0(6) . . ? N12 C37 C36 112.9(5) . . ? N11 C37 C36 123.0(6) . . ? O3 C38 N13 127.8(5) . . ? O3 C38 C39 118.7(5) . . ? N13 C38 C39 113.5(5) . . ? N14 C39 C40 120.1(6) . . ? N14 C39 C38 114.4(5) . . ? C40 C39 C38 125.5(5) . . ? C39 C40 C41 119.2(6) . . ? C40 C41 C40 119.8(8) 3_665 . ? F2 C42 F3 103(2) . . ? F2 C42 F1 105(3) . . ? F3 C42 F1 117(3) . . ? F2 C42 S1 124(2) . . ? F3 C42 S1 108(2) . . ? F1 C42 S1 102.1(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.790 _refine_diff_density_min -1.457 _refine_diff_density_rms 0.177