# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Housecroft, Catherine E' _publ_contact_author_name 'Housecroft, Catherine E' _publ_contact_author_email Catherine.Housecroft@unibas.ch _publ_section_title ; When five are six: the myth of five-coordinate copper(II) in supramolecular chemistry ; # Attachment '- JP100.CIF' data_jp100 _database_code_depnum_ccdc_archive 'CCDC 770973' #TrackingRef '- JP100.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H23 Cu N5, 2(F6 P), C2 H3 N' _chemical_formula_sum 'C29 H26 Cu F12 N6 P2' _chemical_formula_weight 812.04 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc 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 14.222(3) _cell_length_b 28.141(6) _cell_length_c 16.880(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.59(3) _cell_angle_gamma 90.00 _cell_volume 6593(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 0.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6265 _exptl_absorpt_correction_T_max 0.9039 _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 126453 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.05 _reflns_number_total 11581 _reflns_number_gt 10753 _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^)+(0.0561P)^2^+5.8899P] 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 11581 _refine_ls_number_parameters 903 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.129810(18) 0.356377(9) 0.437930(16) 0.01899(9) Uani 1 1 d . . . N1 N 0.04271(13) 0.30945(7) 0.36350(11) 0.0226(4) Uani 1 1 d . . . N2 N 0.21728(13) 0.30298(6) 0.44307(11) 0.0199(4) Uani 1 1 d . . . N3 N 0.24488(13) 0.38132(7) 0.52081(11) 0.0222(4) Uani 1 1 d . . . C1 C -0.04844(16) 0.31664(9) 0.32311(14) 0.0284(5) Uani 1 1 d . . . H1A H -0.0774 0.3467 0.3269 0.034 Uiso 1 1 calc R . . C2 C -0.10177(17) 0.28144(9) 0.27596(15) 0.0329(6) Uani 1 1 d . . . H2A H -0.1663 0.2873 0.2480 0.039 Uiso 1 1 calc R . . C3 C -0.05940(18) 0.23784(9) 0.27053(16) 0.0345(6) Uani 1 1 d . . . H3A H -0.0949 0.2131 0.2392 0.041 Uiso 1 1 calc R . . C4 C 0.03474(18) 0.23025(9) 0.31079(16) 0.0315(5) Uani 1 1 d . . . H4A H 0.0649 0.2004 0.3073 0.038 Uiso 1 1 calc R . . C5 C 0.08438(15) 0.26689(8) 0.35635(13) 0.0218(4) Uani 1 1 d . . . C6 C 0.18620(16) 0.26342(8) 0.40165(13) 0.0228(5) Uani 1 1 d . . . C7 C 0.24612(18) 0.22457(9) 0.40419(15) 0.0308(5) Uani 1 1 d . . . H7A H 0.2245 0.1965 0.3746 0.037 Uiso 1 1 calc R . . C8 C 0.33874(19) 0.22781(9) 0.45122(16) 0.0365(6) Uani 1 1 d . . . H8A H 0.3815 0.2017 0.4534 0.044 Uiso 1 1 calc R . . C9 C 0.37018(17) 0.26872(9) 0.49532(15) 0.0315(5) Uani 1 1 d . . . H9A H 0.4337 0.2710 0.5277 0.038 Uiso 1 1 calc R . . C10 C 0.30548(15) 0.30612(8) 0.49039(13) 0.0225(4) Uani 1 1 d . . . C11 C 0.32245(16) 0.35201(8) 0.53457(13) 0.0224(5) Uani 1 1 d . . . C12 C 0.40784(17) 0.36437(9) 0.58629(15) 0.0310(5) Uani 1 1 d . . . H12A H 0.4613 0.3433 0.5955 0.037 Uiso 1 1 calc R . . C13 C 0.41443(18) 0.40833(10) 0.62490(16) 0.0344(6) Uani 1 1 d . . . H13A H 0.4728 0.4177 0.6605 0.041 Uiso 1 1 calc R . . C14 C 0.33593(19) 0.43805(9) 0.61113(15) 0.0331(5) Uani 1 1 d . . . H14A H 0.3389 0.4681 0.6374 0.040 Uiso 1 1 calc R . . C15 C 0.25253(17) 0.42340(8) 0.55832(15) 0.0283(5) Uani 1 1 d . . . H15A H 0.1984 0.4441 0.5483 0.034 Uiso 1 1 calc R . . N4 N 0.02438(12) 0.39539(6) 0.47076(11) 0.0198(4) Uani 1 1 d . . . N5 N 0.11978(13) 0.41640(6) 0.35601(11) 0.0221(4) Uani 1 1 d . . . C16 C 0.02267(18) 0.33980(9) 0.58057(15) 0.0319(5) Uani 1 1 d . . . H16A H 0.0737 0.3257 0.5575 0.048 Uiso 1 1 calc R . . H16B H -0.0296 0.3167 0.5779 0.048 Uiso 1 1 calc R . . H16C H 0.0489 0.3485 0.6373 0.048 Uiso 1 1 calc R . . C17 C -0.01553(16) 0.38326(8) 0.53333(14) 0.0238(5) Uani 1 1 d . . . C18 C -0.08926(18) 0.41098(9) 0.55213(16) 0.0328(5) Uani 1 1 d . . . H18A H -0.1172 0.4026 0.5965 0.039 Uiso 1 1 calc R . . C19 C -0.12108(18) 0.45044(10) 0.50590(17) 0.0362(6) Uani 1 1 d . . . H19A H -0.1711 0.4695 0.5183 0.043 Uiso 1 1 calc R . . C20 C -0.08041(17) 0.46238(8) 0.44149(16) 0.0302(5) Uani 1 1 d . . . H20A H -0.1024 0.4894 0.4090 0.036 Uiso 1 1 calc R . . C21 C -0.00694(15) 0.43426(8) 0.42504(13) 0.0217(4) Uani 1 1 d . . . C22 C 0.04385(16) 0.44469(8) 0.35912(13) 0.0228(4) Uani 1 1 d . . . C23 C 0.01700(18) 0.48191(9) 0.30432(15) 0.0325(5) Uani 1 1 d . . . H23A H -0.0366 0.5015 0.3070 0.039 Uiso 1 1 calc R . . C24 C 0.0699(2) 0.48956(10) 0.24627(16) 0.0401(6) Uani 1 1 d . . . H24A H 0.0521 0.5142 0.2074 0.048 Uiso 1 1 calc R . . C25 C 0.14873(19) 0.46148(10) 0.24454(15) 0.0362(6) Uani 1 1 d . . . H25A H 0.1863 0.4670 0.2053 0.043 Uiso 1 1 calc R . . C26 C 0.17312(17) 0.42471(9) 0.30099(14) 0.0276(5) Uani 1 1 d . . . C27 C 0.26052(19) 0.39474(10) 0.30427(16) 0.0372(6) Uani 1 1 d . . . H27A H 0.2656 0.3713 0.3479 0.056 Uiso 1 1 calc R . . H27B H 0.3180 0.4150 0.3148 0.056 Uiso 1 1 calc R . . H27C H 0.2553 0.3783 0.2523 0.056 Uiso 1 1 calc R . . Cu2 Cu 0.367080(18) 0.639828(9) 0.070177(17) 0.02294(9) Uani 1 1 d . . . N6 N 0.45993(13) 0.68278(7) 0.14951(12) 0.0241(4) Uani 1 1 d . . . N7 N 0.29495(13) 0.69875(6) 0.05731(11) 0.0205(4) Uani 1 1 d . . . N8 N 0.24909(14) 0.61940(7) -0.01341(12) 0.0268(4) Uani 1 1 d . . . C28 C 0.54703(17) 0.67127(9) 0.19418(15) 0.0302(5) Uani 1 1 d . . . H28A H 0.5689 0.6394 0.1932 0.036 Uiso 1 1 calc R . . C29 C 0.60617(17) 0.70441(10) 0.24178(15) 0.0332(6) Uani 1 1 d . . . H29A H 0.6676 0.6954 0.2729 0.040 Uiso 1 1 calc R . . C30 C 0.57424(17) 0.75064(10) 0.24317(16) 0.0338(6) Uani 1 1 d . . . H30A H 0.6137 0.7739 0.2751 0.041 Uiso 1 1 calc R . . C31 C 0.48449(17) 0.76282(9) 0.19782(15) 0.0299(5) Uani 1 1 d . . . H31A H 0.4613 0.7945 0.1982 0.036 Uiso 1 1 calc R . . C32 C 0.42890(15) 0.72805(8) 0.15172(13) 0.0223(4) Uani 1 1 d . . . C33 C 0.33175(16) 0.73688(8) 0.10036(13) 0.0226(4) Uani 1 1 d . . . C34 C 0.28057(17) 0.77897(8) 0.09482(15) 0.0289(5) Uani 1 1 d . . . H34A H 0.3064 0.8060 0.1257 0.035 Uiso 1 1 calc R . . C35 C 0.19042(18) 0.78052(9) 0.04292(16) 0.0331(5) Uani 1 1 d . . . H35A H 0.1542 0.8092 0.0377 0.040 Uiso 1 1 calc R . . C36 C 0.15239(17) 0.74080(8) -0.00147(15) 0.0289(5) Uani 1 1 d . . . H36A H 0.0901 0.7416 -0.0363 0.035 Uiso 1 1 calc R . . C37 C 0.20803(15) 0.69975(8) 0.00644(13) 0.0218(4) Uani 1 1 d . . . C38 C 0.18320(15) 0.65431(8) -0.03661(13) 0.0222(4) Uani 1 1 d . . . C39 C 0.10156(17) 0.64706(9) -0.09648(15) 0.0283(5) Uani 1 1 d . . . H39A H 0.0566 0.6721 -0.1127 0.034 Uiso 1 1 calc R . . C40 C 0.08610(18) 0.60258(9) -0.13265(15) 0.0333(6) Uani 1 1 d . . . H40A H 0.0304 0.5968 -0.1741 0.040 Uiso 1 1 calc R . . C41 C 0.15218(18) 0.56683(9) -0.10789(16) 0.0329(5) Uani 1 1 d . . . H41A H 0.1424 0.5361 -0.1314 0.039 Uiso 1 1 calc R . . C42 C 0.23301(18) 0.57663(9) -0.04816(16) 0.0324(5) Uani 1 1 d . . . H42A H 0.2788 0.5521 -0.0312 0.039 Uiso 1 1 calc R . . N9 N 0.47498(13) 0.60858(7) 0.01872(12) 0.0254(4) Uani 1 1 d . . . N10 N 0.39159(14) 0.57643(7) 0.13398(12) 0.0271(4) Uani 1 1 d . . . C43 C 0.4594(2) 0.66931(11) -0.08499(17) 0.0465(7) Uani 1 1 d . . . H43A H 0.4066 0.6786 -0.0593 0.070 Uiso 1 1 calc R . . H43B H 0.4335 0.6622 -0.1424 0.070 Uiso 1 1 calc R . . H43C H 0.5058 0.6954 -0.0804 0.070 Uiso 1 1 calc R . . C44 C 0.50847(18) 0.62622(10) -0.04350(16) 0.0353(6) Uani 1 1 d . . . C45 C 0.5861(2) 0.60451(14) -0.0675(2) 0.0561(9) Uani 1 1 d . . . H45A H 0.6099 0.6170 -0.1116 0.067 Uiso 1 1 calc R . . C46 C 0.6277(2) 0.56502(15) -0.0269(2) 0.0627(11) Uani 1 1 d . . . H46A H 0.6805 0.5500 -0.0428 0.075 Uiso 1 1 calc R . . C47 C 0.5929(2) 0.54706(12) 0.0370(2) 0.0516(8) Uani 1 1 d . . . H47A H 0.6214 0.5198 0.0657 0.062 Uiso 1 1 calc R . . C48 C 0.51545(16) 0.56954(9) 0.05852(16) 0.0311(5) Uani 1 1 d . . . C49 C 0.47064(17) 0.55247(8) 0.12460(15) 0.0308(5) Uani 1 1 d . . . C50 C 0.5048(2) 0.51342(10) 0.1732(2) 0.0500(8) Uani 1 1 d . . . H50A H 0.5610 0.4970 0.1667 0.060 Uiso 1 1 calc R . . C51 C 0.4557(3) 0.49910(11) 0.2307(2) 0.0609(10) Uani 1 1 d . . . H51A H 0.4787 0.4730 0.2653 0.073 Uiso 1 1 calc R . . C52 C 0.3740(3) 0.52241(12) 0.23793(18) 0.0555(9) Uani 1 1 d . . . H52A H 0.3389 0.5120 0.2766 0.067 Uiso 1 1 calc R . . C53 C 0.3416(2) 0.56174(10) 0.18841(15) 0.0363(6) Uani 1 1 d . . . C54 C 0.2507(2) 0.58724(12) 0.19163(18) 0.0466(7) Uani 1 1 d . . . H54A H 0.2411 0.6135 0.1526 0.070 Uiso 1 1 calc R . . H54B H 0.2549 0.5998 0.2464 0.070 Uiso 1 1 calc R . . H54C H 0.1963 0.5652 0.1780 0.070 Uiso 1 1 calc R . . P1 P 0.16294(4) 0.29294(2) 0.12970(4) 0.03134(15) Uani 1 1 d . . . F10 F 0.11655(15) 0.30180(8) 0.03640(11) 0.0653(6) Uani 1 1 d . . . F11 F 0.26077(13) 0.31817(7) 0.12166(13) 0.0610(5) Uani 1 1 d . . . F12 F 0.20425(12) 0.24287(7) 0.10831(11) 0.0511(4) Uani 1 1 d . . . F13 F 0.12131(12) 0.34329(6) 0.15116(12) 0.0525(5) Uani 1 1 d . . . F14 F 0.06467(11) 0.26773(6) 0.13917(11) 0.0443(4) Uani 1 1 d . . . F15 F 0.20724(11) 0.28374(6) 0.22347(9) 0.0443(4) Uani 1 1 d . . . P2 P 0.32608(5) 0.69447(3) 0.35724(4) 0.03393(16) Uani 1 1 d . . . F20 F 0.22881(12) 0.66971(8) 0.36726(13) 0.0632(6) Uani 1 1 d . . . F21 F 0.42432(11) 0.71890(7) 0.34690(11) 0.0481(4) Uani 1 1 d . . . F22 F 0.37249(14) 0.68802(8) 0.45160(10) 0.0584(5) Uani 1 1 d . . . F23 F 0.28442(13) 0.74520(7) 0.37423(12) 0.0541(5) Uani 1 1 d . . . F24 F 0.28243(12) 0.70082(7) 0.26234(10) 0.0485(4) Uani 1 1 d . . . F25 F 0.36919(12) 0.64351(6) 0.34010(12) 0.0513(5) Uani 1 1 d . . . P3 P 0.29836(5) 0.90635(2) 0.22053(4) 0.03186(16) Uani 1 1 d . . . F30 F 0.39822(14) 0.88237(8) 0.21454(13) 0.0655(6) Uani 1 1 d . . . F31 F 0.32783(17) 0.95363(6) 0.18067(12) 0.0638(6) Uani 1 1 d . . . F32 F 0.26907(16) 0.85884(7) 0.25974(12) 0.0661(6) Uani 1 1 d . . . F33 F 0.19754(14) 0.92931(8) 0.22508(11) 0.0625(5) Uani 1 1 d . . . F34 F 0.25128(14) 0.88642(6) 0.13162(10) 0.0527(5) Uani 1 1 d . . . F35 F 0.34598(13) 0.92593(6) 0.30886(10) 0.0473(4) Uani 1 1 d . . . P4 P 0.18453(5) 0.08845(2) 0.28145(4) 0.03324(16) Uani 1 1 d . . . F40 F 0.28961(15) 0.06946(10) 0.28415(13) 0.0771(7) Uani 1 1 d . . . F41 F 0.07904(16) 0.10862(9) 0.27849(14) 0.0776(7) Uani 1 1 d . . . F42 F 0.20887(18) 0.13567(8) 0.23862(13) 0.0796(8) Uani 1 1 d . . . F43 F 0.22085(17) 0.11203(7) 0.36870(11) 0.0655(6) Uani 1 1 d . . . F44 F 0.15844(19) 0.04197(6) 0.32419(12) 0.0701(6) Uani 1 1 d . . . F45 F 0.14619(13) 0.06523(6) 0.19418(10) 0.0484(4) Uani 1 1 d . . . N100 N 0.3523(4) 0.49976(19) 0.4316(3) 0.1044(15) Uani 1 1 d . . . C100 C 0.3815(3) 0.53221(18) 0.4694(2) 0.0697(11) Uani 1 1 d . . . C101 C 0.4192(4) 0.57285(16) 0.5183(3) 0.0826(13) Uani 1 1 d . . . H10A H 0.3921 0.5737 0.5670 0.124 Uiso 1 1 calc R . . H10B H 0.4015 0.6020 0.4868 0.124 Uiso 1 1 calc R . . H10C H 0.4895 0.5705 0.5344 0.124 Uiso 1 1 calc R . . N200 N 0.1417(3) 0.01071(15) 0.5499(2) 0.0738(9) Uani 1 1 d . . . C200 C 0.1014(3) 0.04212(15) 0.5165(2) 0.0552(9) Uani 1 1 d . . . C201 C 0.0486(3) 0.08178(15) 0.4740(2) 0.0712(11) Uani 1 1 d . . . H20B H -0.0203 0.0777 0.4719 0.107 Uiso 1 1 calc R . . H20C H 0.0594 0.0832 0.4187 0.107 Uiso 1 1 calc R . . H20D H 0.0710 0.1114 0.5026 0.107 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 0.01693(14) 0.01319(14) 0.02404(15) -0.00264(9) -0.00165(11) 0.00252(9) N1 0.0211(9) 0.0182(9) 0.0263(9) -0.0024(7) 0.0008(7) 0.0003(7) N2 0.0205(9) 0.0168(9) 0.0213(9) -0.0005(7) 0.0022(7) 0.0022(7) N3 0.0208(9) 0.0169(9) 0.0267(10) -0.0019(7) 0.0004(7) 0.0021(7) C1 0.0226(11) 0.0268(12) 0.0323(12) -0.0042(10) -0.0016(9) 0.0018(9) C2 0.0215(11) 0.0379(14) 0.0361(13) -0.0088(11) -0.0007(10) -0.0045(10) C3 0.0300(13) 0.0333(14) 0.0388(14) -0.0139(11) 0.0042(11) -0.0091(10) C4 0.0314(13) 0.0231(12) 0.0394(14) -0.0096(10) 0.0064(11) -0.0020(10) C5 0.0209(10) 0.0210(11) 0.0235(11) -0.0015(8) 0.0046(9) -0.0013(8) C6 0.0272(11) 0.0173(11) 0.0233(11) -0.0019(8) 0.0043(9) 0.0016(9) C7 0.0356(13) 0.0219(12) 0.0325(13) -0.0055(10) 0.0019(10) 0.0061(10) C8 0.0385(14) 0.0279(13) 0.0399(14) -0.0059(11) 0.0013(11) 0.0179(11) C9 0.0248(12) 0.0327(13) 0.0327(13) -0.0030(10) -0.0032(10) 0.0103(10) C10 0.0211(10) 0.0220(11) 0.0232(11) -0.0015(9) 0.0020(9) 0.0035(9) C11 0.0200(11) 0.0225(11) 0.0236(11) -0.0015(9) 0.0023(9) 0.0019(8) C12 0.0222(12) 0.0326(13) 0.0341(13) -0.0066(10) -0.0031(10) 0.0043(10) C13 0.0271(12) 0.0371(14) 0.0338(13) -0.0091(11) -0.0049(10) -0.0063(10) C14 0.0380(14) 0.0233(12) 0.0354(13) -0.0085(10) 0.0020(11) -0.0051(10) C15 0.0269(12) 0.0204(11) 0.0347(13) -0.0062(9) 0.0006(10) 0.0027(9) N4 0.0187(9) 0.0155(9) 0.0227(9) -0.0034(7) -0.0009(7) 0.0011(7) N5 0.0234(9) 0.0178(9) 0.0228(9) -0.0019(7) 0.0001(7) -0.0026(7) C16 0.0324(13) 0.0325(14) 0.0297(12) 0.0065(10) 0.0041(10) -0.0028(10) C17 0.0219(11) 0.0224(11) 0.0259(11) -0.0046(9) 0.0023(9) -0.0049(9) C18 0.0289(12) 0.0352(14) 0.0358(13) -0.0088(11) 0.0101(10) -0.0042(10) C19 0.0253(12) 0.0336(14) 0.0501(16) -0.0133(12) 0.0087(11) 0.0059(10) C20 0.0247(12) 0.0193(11) 0.0427(14) -0.0039(10) -0.0011(10) 0.0058(9) C21 0.0192(10) 0.0149(10) 0.0270(11) -0.0048(8) -0.0040(8) -0.0007(8) C22 0.0223(11) 0.0160(10) 0.0259(11) -0.0010(8) -0.0037(9) -0.0001(8) C23 0.0340(13) 0.0219(12) 0.0357(13) 0.0058(10) -0.0053(10) -0.0005(10) C24 0.0446(15) 0.0348(15) 0.0341(14) 0.0153(11) -0.0064(11) -0.0089(12) C25 0.0359(14) 0.0416(15) 0.0285(12) 0.0061(11) 0.0015(10) -0.0146(12) C26 0.0283(12) 0.0296(13) 0.0236(11) -0.0039(9) 0.0026(9) -0.0095(10) C27 0.0332(13) 0.0446(16) 0.0357(14) -0.0017(12) 0.0119(11) -0.0015(12) Cu2 0.01957(15) 0.01537(15) 0.02930(16) -0.00367(10) -0.00471(11) 0.00345(10) N6 0.0206(9) 0.0209(10) 0.0278(10) -0.0037(8) -0.0013(7) 0.0005(7) N7 0.0201(9) 0.0171(9) 0.0228(9) -0.0011(7) 0.0017(7) 0.0017(7) N8 0.0241(10) 0.0203(10) 0.0322(10) -0.0037(8) -0.0019(8) 0.0034(8) C28 0.0230(11) 0.0273(13) 0.0364(13) -0.0031(10) -0.0022(10) 0.0036(9) C29 0.0216(11) 0.0403(15) 0.0340(13) -0.0057(11) -0.0017(10) 0.0000(10) C30 0.0253(12) 0.0349(14) 0.0389(14) -0.0113(11) 0.0022(10) -0.0077(10) C31 0.0259(12) 0.0256(12) 0.0372(13) -0.0075(10) 0.0047(10) -0.0023(9) C32 0.0208(11) 0.0207(11) 0.0256(11) -0.0025(9) 0.0054(9) -0.0004(8) C33 0.0238(11) 0.0203(11) 0.0230(11) -0.0008(8) 0.0034(9) -0.0008(9) C34 0.0321(12) 0.0194(11) 0.0339(13) -0.0047(9) 0.0041(10) 0.0035(9) C35 0.0334(13) 0.0242(12) 0.0394(14) -0.0017(10) 0.0026(11) 0.0120(10) C36 0.0252(11) 0.0257(12) 0.0325(13) -0.0014(10) -0.0012(10) 0.0077(9) C37 0.0190(10) 0.0221(11) 0.0232(11) -0.0002(9) 0.0022(8) 0.0024(8) C38 0.0205(11) 0.0211(11) 0.0241(11) -0.0013(9) 0.0031(9) 0.0018(9) C39 0.0212(11) 0.0302(13) 0.0303(12) -0.0035(10) -0.0010(9) 0.0037(9) C40 0.0279(12) 0.0374(14) 0.0301(12) -0.0072(11) -0.0031(10) -0.0028(10) C41 0.0341(13) 0.0257(13) 0.0361(13) -0.0096(10) 0.0014(10) -0.0042(10) C42 0.0320(13) 0.0204(12) 0.0400(14) -0.0084(10) -0.0027(11) 0.0033(10) N9 0.0216(9) 0.0241(10) 0.0289(10) -0.0082(8) 0.0018(8) -0.0014(8) N10 0.0303(10) 0.0187(9) 0.0274(10) -0.0003(8) -0.0045(8) -0.0038(8) C43 0.0576(18) 0.0485(18) 0.0321(14) 0.0012(12) 0.0068(13) -0.0240(14) C44 0.0315(13) 0.0397(15) 0.0344(13) -0.0151(11) 0.0061(11) -0.0158(11) C45 0.0379(16) 0.083(3) 0.0535(18) -0.0320(18) 0.0227(14) -0.0215(17) C46 0.0273(15) 0.085(3) 0.077(2) -0.041(2) 0.0128(15) 0.0057(16) C47 0.0322(14) 0.0513(19) 0.064(2) -0.0269(16) -0.0051(14) 0.0150(13) C48 0.0218(11) 0.0242(12) 0.0405(14) -0.0140(10) -0.0080(10) 0.0037(9) C49 0.0309(12) 0.0170(11) 0.0357(13) -0.0015(10) -0.0116(10) 0.0011(9) C50 0.0478(17) 0.0228(13) 0.063(2) 0.0039(13) -0.0229(15) 0.0048(12) C51 0.070(2) 0.0342(17) 0.058(2) 0.0239(15) -0.0314(17) -0.0175(16) C52 0.069(2) 0.0482(19) 0.0367(15) 0.0150(13) -0.0153(15) -0.0341(17) C53 0.0435(15) 0.0361(14) 0.0247(12) 0.0001(10) -0.0027(10) -0.0212(12) C54 0.0440(16) 0.0594(19) 0.0387(15) -0.0066(13) 0.0142(13) -0.0195(14) P1 0.0237(3) 0.0351(4) 0.0325(3) 0.0015(3) 0.0001(2) 0.0046(3) F10 0.0661(12) 0.0861(15) 0.0365(10) 0.0120(9) -0.0043(9) 0.0142(11) F11 0.0376(9) 0.0654(13) 0.0807(14) 0.0237(10) 0.0143(9) -0.0048(9) F12 0.0447(9) 0.0504(11) 0.0576(11) -0.0120(8) 0.0096(8) 0.0149(8) F13 0.0377(9) 0.0353(9) 0.0748(12) -0.0098(8) -0.0085(8) 0.0077(7) F14 0.0264(7) 0.0436(9) 0.0604(10) -0.0016(8) 0.0039(7) 0.0000(7) F15 0.0355(8) 0.0587(11) 0.0346(8) 0.0032(7) -0.0013(6) 0.0083(7) P2 0.0236(3) 0.0426(4) 0.0339(4) 0.0055(3) 0.0027(3) 0.0073(3) F20 0.0340(9) 0.0759(14) 0.0803(14) 0.0265(11) 0.0137(9) -0.0031(9) F21 0.0301(8) 0.0552(11) 0.0584(10) 0.0038(8) 0.0083(7) 0.0007(7) F22 0.0585(11) 0.0782(14) 0.0345(9) 0.0087(9) 0.0015(8) 0.0151(10) F23 0.0494(10) 0.0529(11) 0.0602(11) 0.0002(9) 0.0125(8) 0.0199(8) F24 0.0389(9) 0.0665(12) 0.0357(9) 0.0078(8) -0.0018(7) 0.0136(8) F25 0.0389(9) 0.0435(10) 0.0616(11) -0.0044(8) -0.0105(8) 0.0119(7) P3 0.0383(4) 0.0190(3) 0.0357(3) 0.0012(2) 0.0022(3) -0.0003(3) F30 0.0515(11) 0.0700(14) 0.0729(13) -0.0044(11) 0.0093(10) 0.0232(10) F31 0.1039(16) 0.0304(9) 0.0594(12) 0.0082(8) 0.0230(11) -0.0132(10) F32 0.0764(14) 0.0459(11) 0.0610(12) 0.0212(9) -0.0178(10) -0.0302(10) F33 0.0517(11) 0.0915(16) 0.0416(10) 0.0010(10) 0.0045(8) 0.0279(10) F34 0.0768(12) 0.0319(9) 0.0402(9) -0.0065(7) -0.0073(8) 0.0118(8) F35 0.0542(10) 0.0396(9) 0.0422(9) -0.0060(7) -0.0022(8) -0.0086(8) P4 0.0428(4) 0.0206(3) 0.0332(3) -0.0019(3) 0.0013(3) -0.0052(3) F40 0.0518(12) 0.121(2) 0.0531(12) -0.0003(12) -0.0010(9) 0.0220(12) F41 0.0671(13) 0.0964(18) 0.0690(14) -0.0016(12) 0.0145(11) 0.0336(13) F42 0.1026(17) 0.0538(13) 0.0657(13) 0.0226(10) -0.0183(12) -0.0439(12) F43 0.1030(16) 0.0388(10) 0.0439(10) -0.0149(8) -0.0071(10) -0.0046(10) F44 0.1275(19) 0.0303(10) 0.0540(11) 0.0043(8) 0.0231(12) -0.0216(11) F45 0.0563(10) 0.0491(10) 0.0372(9) -0.0116(7) 0.0049(7) -0.0176(8) N100 0.135(4) 0.111(4) 0.069(3) -0.001(2) 0.027(3) -0.024(3) C100 0.077(3) 0.087(3) 0.053(2) 0.024(2) 0.031(2) 0.011(2) C101 0.114(4) 0.072(3) 0.075(3) 0.010(2) 0.050(3) 0.005(3) N200 0.082(2) 0.086(3) 0.0543(19) -0.0161(18) 0.0151(17) -0.001(2) C200 0.058(2) 0.069(2) 0.0425(18) -0.0249(17) 0.0210(16) -0.0184(18) C201 0.091(3) 0.069(3) 0.063(2) -0.0129(19) 0.038(2) -0.007(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 Cu1 N2 1.9407(18) . ? Cu1 N4 2.0305(18) . ? Cu1 N3 2.0323(19) . ? Cu1 N1 2.0441(19) . ? Cu1 N5 2.1679(19) . ? N1 C1 1.342(3) . ? N1 C5 1.353(3) . ? N2 C10 1.335(3) . ? N2 C6 1.337(3) . ? N3 C15 1.336(3) . ? N3 C11 1.356(3) . ? C1 C2 1.388(3) . ? C1 H1A 0.9500 . ? C2 C3 1.379(4) . ? C2 H2A 0.9500 . ? C3 C4 1.380(4) . ? C3 H3A 0.9500 . ? C4 C5 1.384(3) . ? C4 H4A 0.9500 . ? C5 C6 1.486(3) . ? C6 C7 1.381(3) . ? C7 C8 1.385(4) . ? C7 H7A 0.9500 . ? C8 C9 1.391(4) . ? C8 H8A 0.9500 . ? C9 C10 1.389(3) . ? C9 H9A 0.9500 . ? C10 C11 1.484(3) . ? C11 C12 1.377(3) . ? C12 C13 1.392(4) . ? C12 H12A 0.9500 . ? C13 C14 1.374(4) . ? C13 H13A 0.9500 . ? C14 C15 1.382(3) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? N4 C17 1.347(3) . ? N4 C21 1.357(3) . ? N5 C26 1.342(3) . ? N5 C22 1.352(3) . ? C16 C17 1.496(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.398(3) . ? C18 C19 1.376(4) . ? C18 H18A 0.9500 . ? C19 C20 1.380(4) . ? C19 H19A 0.9500 . ? C20 C21 1.386(3) . ? C20 H20A 0.9500 . ? C21 C22 1.482(3) . ? C22 C23 1.395(3) . ? C23 C24 1.376(4) . ? C23 H23A 0.9500 . ? C24 C25 1.377(4) . ? C24 H24A 0.9500 . ? C25 C26 1.398(4) . ? C25 H25A 0.9500 . ? C26 C27 1.493(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? Cu2 N7 1.9369(18) . ? Cu2 N8 2.026(2) . ? Cu2 N6 2.0560(19) . ? Cu2 N10 2.074(2) . ? Cu2 N9 2.113(2) . ? N6 C28 1.342(3) . ? N6 C32 1.351(3) . ? N7 C33 1.337(3) . ? N7 C37 1.343(3) . ? N8 C42 1.337(3) . ? N8 C38 1.355(3) . ? C28 C29 1.389(3) . ? C28 H28A 0.9500 . ? C29 C30 1.380(4) . ? C29 H29A 0.9500 . ? C30 C31 1.381(4) . ? C30 H30A 0.9500 . ? C31 C32 1.386(3) . ? C31 H31A 0.9500 . ? C32 C33 1.483(3) . ? C33 C34 1.383(3) . ? C34 C35 1.387(4) . ? C34 H34A 0.9500 . ? C35 C36 1.388(4) . ? C35 H35A 0.9500 . ? C36 C37 1.390(3) . ? C36 H36A 0.9500 . ? C37 C38 1.475(3) . ? C38 C39 1.378(3) . ? C39 C40 1.389(3) . ? C39 H39A 0.9500 . ? C40 C41 1.378(4) . ? C40 H40A 0.9500 . ? C41 C42 1.382(3) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? N9 C44 1.340(3) . ? N9 C48 1.350(3) . ? N10 C53 1.343(3) . ? N10 C49 1.350(3) . ? C43 C44 1.495(4) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.397(4) . ? C45 C46 1.370(6) . ? C45 H45A 0.9500 . ? C46 C47 1.376(5) . ? C46 H46A 0.9500 . ? C47 C48 1.386(4) . ? C47 H47A 0.9500 . ? C48 C49 1.480(4) . ? C49 C50 1.394(4) . ? C50 C51 1.373(5) . ? C50 H50A 0.9500 . ? C51 C52 1.363(5) . ? C51 H51A 0.9500 . ? C52 C53 1.403(4) . ? C52 H52A 0.9500 . ? C53 C54 1.491(4) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? P1 F10 1.5889(19) . ? P1 F15 1.5921(17) . ? P1 F11 1.5940(18) . ? P1 F12 1.5978(18) . ? P1 F14 1.6061(17) . ? P1 F13 1.6073(18) . ? P2 F20 1.5907(18) . ? P2 F23 1.5953(19) . ? P2 F22 1.5960(18) . ? P2 F24 1.5968(17) . ? P2 F21 1.6004(17) . ? P2 F25 1.6105(18) . ? P3 F32 1.5874(18) . ? P3 F31 1.5877(18) . ? P3 F33 1.5897(19) . ? P3 F35 1.5954(17) . ? P3 F30 1.5955(19) . ? P3 F34 1.6053(18) . ? P4 F44 1.5766(18) . ? P4 F40 1.578(2) . ? P4 F42 1.5865(19) . ? P4 F41 1.595(2) . ? P4 F45 1.5950(17) . ? P4 F43 1.5952(18) . ? N100 C100 1.140(6) . ? C100 C101 1.444(7) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? N200 C200 1.134(5) . ? C200 C201 1.445(6) . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C201 H20D 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 N4 155.61(8) . . ? N2 Cu1 N3 79.90(8) . . ? N4 Cu1 N3 99.04(7) . . ? N2 Cu1 N1 79.86(8) . . ? N4 Cu1 N1 97.61(7) . . ? N3 Cu1 N1 159.30(7) . . ? N2 Cu1 N5 125.75(8) . . ? N4 Cu1 N5 78.64(7) . . ? N3 Cu1 N5 95.80(7) . . ? N1 Cu1 N5 99.47(7) . . ? C1 N1 C5 118.77(19) . . ? C1 N1 Cu1 127.15(16) . . ? C5 N1 Cu1 114.08(14) . . ? C10 N2 C6 121.89(19) . . ? C10 N2 Cu1 119.00(15) . . ? C6 N2 Cu1 119.05(15) . . ? C15 N3 C11 118.61(19) . . ? C15 N3 Cu1 127.05(15) . . ? C11 N3 Cu1 114.24(15) . . ? N1 C1 C2 122.0(2) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C3 C2 C1 118.7(2) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C2 C3 C4 119.7(2) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C5 118.8(2) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? N1 C5 C4 121.9(2) . . ? N1 C5 C6 114.13(19) . . ? C4 C5 C6 124.0(2) . . ? N2 C6 C7 120.8(2) . . ? N2 C6 C5 112.85(19) . . ? C7 C6 C5 126.4(2) . . ? C6 C7 C8 118.0(2) . . ? C6 C7 H7A 121.0 . . ? C8 C7 H7A 121.0 . . ? C7 C8 C9 121.1(2) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? C10 C9 C8 117.6(2) . . ? C10 C9 H9A 121.2 . . ? C8 C9 H9A 121.2 . . ? N2 C10 C9 120.6(2) . . ? N2 C10 C11 112.76(19) . . ? C9 C10 C11 126.6(2) . . ? N3 C11 C12 121.8(2) . . ? N3 C11 C10 113.96(19) . . ? C12 C11 C10 124.2(2) . . ? C11 C12 C13 118.8(2) . . ? C11 C12 H12A 120.6 . . ? C13 C12 H12A 120.6 . . ? C14 C13 C12 119.5(2) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C13 C14 C15 118.6(2) . . ? C13 C14 H14A 120.7 . . ? C15 C14 H14A 120.7 . . ? N3 C15 C14 122.7(2) . . ? N3 C15 H15A 118.7 . . ? C14 C15 H15A 118.7 . . ? C17 N4 C21 120.53(19) . . ? C17 N4 Cu1 122.64(15) . . ? C21 N4 Cu1 116.81(15) . . ? C26 N5 C22 120.1(2) . . ? C26 N5 Cu1 127.51(16) . . ? C22 N5 Cu1 112.09(15) . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N4 C17 C18 120.1(2) . . ? N4 C17 C16 117.3(2) . . ? C18 C17 C16 122.6(2) . . ? C19 C18 C17 119.5(2) . . ? C19 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? C18 C19 C20 120.1(2) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C19 C20 C21 118.9(2) . . ? C19 C20 H20A 120.6 . . ? C21 C20 H20A 120.6 . . ? N4 C21 C20 121.0(2) . . ? N4 C21 C22 115.69(19) . . ? C20 C21 C22 123.3(2) . . ? N5 C22 C23 121.5(2) . . ? N5 C22 C21 115.90(19) . . ? C23 C22 C21 122.6(2) . . ? C24 C23 C22 118.5(2) . . ? C24 C23 H23A 120.8 . . ? C22 C23 H23A 120.8 . . ? C23 C24 C25 120.0(2) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C26 119.5(2) . . ? C24 C25 H25A 120.3 . . ? C26 C25 H25A 120.3 . . ? N5 C26 C25 120.5(2) . . ? N5 C26 C27 117.9(2) . . ? C25 C26 C27 121.6(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N7 Cu2 N8 80.03(8) . . ? N7 Cu2 N6 79.57(8) . . ? N8 Cu2 N6 159.60(8) . . ? N7 Cu2 N10 145.05(8) . . ? N8 Cu2 N10 97.90(8) . . ? N6 Cu2 N10 98.98(8) . . ? N7 Cu2 N9 136.43(8) . . ? N8 Cu2 N9 99.27(8) . . ? N6 Cu2 N9 95.25(7) . . ? N10 Cu2 N9 78.49(8) . . ? C28 N6 C32 118.6(2) . . ? C28 N6 Cu2 127.39(16) . . ? C32 N6 Cu2 113.88(15) . . ? C33 N7 C37 121.83(19) . . ? C33 N7 Cu2 119.42(15) . . ? C37 N7 Cu2 118.74(15) . . ? C42 N8 C38 119.0(2) . . ? C42 N8 Cu2 126.70(16) . . ? C38 N8 Cu2 114.27(15) . . ? N6 C28 C29 122.1(2) . . ? N6 C28 H28A 119.0 . . ? C29 C28 H28A 119.0 . . ? C30 C29 C28 118.9(2) . . ? C30 C29 H29A 120.6 . . ? C28 C29 H29A 120.6 . . ? C29 C30 C31 119.5(2) . . ? C29 C30 H30A 120.2 . . ? C31 C30 H30A 120.2 . . ? C30 C31 C32 118.8(2) . . ? C30 C31 H31A 120.6 . . ? C32 C31 H31A 120.6 . . ? N6 C32 C31 122.1(2) . . ? N6 C32 C33 114.21(19) . . ? C31 C32 C33 123.7(2) . . ? N7 C33 C34 120.9(2) . . ? N7 C33 C32 112.80(19) . . ? C34 C33 C32 126.3(2) . . ? C33 C34 C35 118.0(2) . . ? C33 C34 H34A 121.0 . . ? C35 C34 H34A 121.0 . . ? C34 C35 C36 120.9(2) . . ? C34 C35 H35A 119.6 . . ? C36 C35 H35A 119.6 . . ? C35 C36 C37 118.1(2) . . ? C35 C36 H36A 121.0 . . ? C37 C36 H36A 121.0 . . ? N7 C37 C36 120.3(2) . . ? N7 C37 C38 112.64(19) . . ? C36 C37 C38 127.1(2) . . ? N8 C38 C39 121.6(2) . . ? N8 C38 C37 114.20(19) . . ? C39 C38 C37 124.2(2) . . ? C38 C39 C40 118.9(2) . . ? C38 C39 H39A 120.6 . . ? C40 C39 H39A 120.6 . . ? C41 C40 C39 119.5(2) . . ? C41 C40 H40A 120.2 . . ? C39 C40 H40A 120.2 . . ? C40 C41 C42 118.7(2) . . ? C40 C41 H41A 120.7 . . ? C42 C41 H41A 120.7 . . ? N8 C42 C41 122.4(2) . . ? N8 C42 H42A 118.8 . . ? C41 C42 H42A 118.8 . . ? C44 N9 C48 120.4(2) . . ? C44 N9 Cu2 125.62(18) . . ? C48 N9 Cu2 113.79(16) . . ? C53 N10 C49 120.3(2) . . ? C53 N10 Cu2 124.46(18) . . ? C49 N10 Cu2 114.76(16) . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N9 C44 C45 120.3(3) . . ? N9 C44 C43 117.3(2) . . ? C45 C44 C43 122.5(3) . . ? C46 C45 C44 119.4(3) . . ? C46 C45 H45A 120.3 . . ? C44 C45 H45A 120.3 . . ? C45 C46 C47 120.0(3) . . ? C45 C46 H46A 120.0 . . ? C47 C46 H46A 120.0 . . ? C46 C47 C48 118.7(3) . . ? C46 C47 H47A 120.7 . . ? C48 C47 H47A 120.7 . . ? N9 C48 C47 121.2(3) . . ? N9 C48 C49 115.6(2) . . ? C47 C48 C49 123.2(3) . . ? N10 C49 C50 121.1(3) . . ? N10 C49 C48 115.7(2) . . ? C50 C49 C48 123.2(3) . . ? C51 C50 C49 118.8(3) . . ? C51 C50 H50A 120.6 . . ? C49 C50 H50A 120.6 . . ? C52 C51 C50 119.8(3) . . ? C52 C51 H51A 120.1 . . ? C50 C51 H51A 120.1 . . ? C51 C52 C53 120.1(3) . . ? C51 C52 H52A 119.9 . . ? C53 C52 H52A 119.9 . . ? N10 C53 C52 119.8(3) . . ? N10 C53 C54 118.0(2) . . ? C52 C53 C54 122.2(3) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? F10 P1 F15 178.78(11) . . ? F10 P1 F11 91.57(12) . . ? F15 P1 F11 89.62(10) . . ? F10 P1 F12 90.47(11) . . ? F15 P1 F12 89.77(10) . . ? F11 P1 F12 90.16(11) . . ? F10 P1 F14 89.18(11) . . ? F15 P1 F14 89.63(10) . . ? F11 P1 F14 179.16(12) . . ? F12 P1 F14 90.22(10) . . ? F10 P1 F13 89.50(11) . . ? F15 P1 F13 90.26(10) . . ? F11 P1 F13 89.87(11) . . ? F12 P1 F13 179.95(14) . . ? F14 P1 F13 89.75(10) . . ? F20 P2 F23 90.41(11) . . ? F20 P2 F22 91.38(12) . . ? F23 P2 F22 90.65(11) . . ? F20 P2 F24 89.93(11) . . ? F23 P2 F24 90.10(10) . . ? F22 P2 F24 178.48(10) . . ? F20 P2 F21 179.44(12) . . ? F23 P2 F21 90.14(10) . . ? F22 P2 F21 88.67(11) . . ? F24 P2 F21 90.02(10) . . ? F20 P2 F25 90.17(11) . . ? F23 P2 F25 179.42(11) . . ? F22 P2 F25 89.27(11) . . ? F24 P2 F25 89.96(10) . . ? F21 P2 F25 89.28(10) . . ? F32 P3 F31 179.51(13) . . ? F32 P3 F33 90.04(13) . . ? F31 P3 F33 90.23(13) . . ? F32 P3 F35 89.87(10) . . ? F31 P3 F35 90.52(10) . . ? F33 P3 F35 91.04(11) . . ? F32 P3 F30 89.33(13) . . ? F31 P3 F30 90.38(13) . . ? F33 P3 F30 178.64(13) . . ? F35 P3 F30 90.17(11) . . ? F32 P3 F34 90.10(11) . . ? F31 P3 F34 89.51(11) . . ? F33 P3 F34 89.45(11) . . ? F35 P3 F34 179.51(12) . . ? F30 P3 F34 89.35(11) . . ? F44 P4 F40 91.24(15) . . ? F44 P4 F42 178.89(15) . . ? F40 P4 F42 89.86(15) . . ? F44 P4 F41 89.77(14) . . ? F40 P4 F41 178.93(15) . . ? F42 P4 F41 89.13(15) . . ? F44 P4 F45 90.90(10) . . ? F40 P4 F45 91.08(11) . . ? F42 P4 F45 89.25(11) . . ? F41 P4 F45 89.26(12) . . ? F44 P4 F43 89.06(11) . . ? F40 P4 F43 90.01(12) . . ? F42 P4 F43 90.77(12) . . ? F41 P4 F43 89.65(13) . . ? F45 P4 F43 178.91(12) . . ? N100 C100 C101 179.1(5) . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? N200 C200 C201 179.1(4) . . ? C200 C201 H20B 109.5 . . ? C200 C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C200 C201 H20D 109.5 . . ? H20B C201 H20D 109.5 . . ? H20C C201 H20D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.507 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.062 # start Validation Reply Form _vrf_PLAT113_jp100 ; PROBLEM: ADDSYM Suggests Possible Pseudo/New Space-group. P21/c RESPONSE: Molecules are not equivalent ; # end Validation Reply Form # Attachment '- JP102.CIF' data_jp102 _database_code_depnum_ccdc_archive 'CCDC 770974' #TrackingRef '- JP102.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H19 Cu N5, 2(F6 P)' _chemical_formula_sum 'C25 H19 Cu F12 N5 P2' _chemical_formula_weight 742.93 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc 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 17.011(3) _cell_length_b 10.486(2) _cell_length_c 16.317(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.79(3) _cell_angle_gamma 90.00 _cell_volume 2786.3(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 blue _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 1.007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5833 _exptl_absorpt_correction_T_max 0.8636 _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 41272 _diffrn_reflns_av_R_equivalents 0.1369 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4846 _reflns_number_gt 4732 _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^)+(0.0554P)^2^+1.8849P] 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 4846 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 0.268956(15) 0.75774(2) 0.317436(17) 0.02400(12) Uani 1 1 d . . . N1 N 0.24598(11) 0.89489(19) 0.39606(12) 0.0272(4) Uani 1 1 d . . . N2 N 0.32268(10) 0.90067(18) 0.28280(11) 0.0242(4) Uani 1 1 d . . . N3 N 0.32645(11) 0.66507(19) 0.24123(12) 0.0279(4) Uani 1 1 d . . . C1 C 0.20192(14) 0.8833(2) 0.45245(16) 0.0333(5) Uani 1 1 d . . . H1A H 0.1800 0.8022 0.4599 0.040 Uiso 1 1 calc R . . C2 C 0.18771(15) 0.9851(3) 0.49958(17) 0.0379(6) Uani 1 1 d . . . H2A H 0.1574 0.9738 0.5397 0.045 Uiso 1 1 calc R . . C3 C 0.21784(15) 1.1037(3) 0.48806(16) 0.0360(5) Uani 1 1 d . . . H3A H 0.2087 1.1748 0.5202 0.043 Uiso 1 1 calc R . . C4 C 0.26192(14) 1.1177(2) 0.42859(15) 0.0317(5) Uani 1 1 d . . . H4A H 0.2827 1.1986 0.4189 0.038 Uiso 1 1 calc R . . C5 C 0.27481(12) 1.0114(2) 0.38411(14) 0.0266(5) Uani 1 1 d . . . C6 C 0.32103(13) 1.0137(2) 0.31926(14) 0.0265(5) Uani 1 1 d . . . C7 C 0.35998(14) 1.1184(2) 0.29626(15) 0.0320(5) Uani 1 1 d . . . H7A H 0.3591 1.1994 0.3220 0.038 Uiso 1 1 calc R . . C8 C 0.40040(15) 1.1001(3) 0.23395(16) 0.0352(5) Uani 1 1 d . . . H8A H 0.4268 1.1703 0.2163 0.042 Uiso 1 1 calc R . . C9 C 0.40261(14) 0.9815(2) 0.19746(15) 0.0317(5) Uani 1 1 d . . . H9A H 0.4301 0.9695 0.1550 0.038 Uiso 1 1 calc R . . C10 C 0.36369(13) 0.8809(2) 0.22447(14) 0.0276(5) Uani 1 1 d . . . C11 C 0.36407(14) 0.7456(2) 0.19943(16) 0.0285(5) Uani 1 1 d . . . C12 C 0.40188(15) 0.7005(3) 0.14037(16) 0.0354(5) Uani 1 1 d . . . H12A H 0.4273 0.7582 0.1109 0.042 Uiso 1 1 calc R . . C13 C 0.40223(16) 0.5703(3) 0.12464(17) 0.0408(6) Uani 1 1 d . . . H13A H 0.4281 0.5377 0.0846 0.049 Uiso 1 1 calc R . . C14 C 0.36440(16) 0.4891(3) 0.16804(17) 0.0399(6) Uani 1 1 d . . . H14A H 0.3643 0.3996 0.1588 0.048 Uiso 1 1 calc R . . C15 C 0.32655(15) 0.5402(2) 0.22537(16) 0.0341(5) Uani 1 1 d . . . H15A H 0.2997 0.4843 0.2544 0.041 Uiso 1 1 calc R . . N4 N 0.22381(11) 0.60997(18) 0.36471(12) 0.0260(4) Uani 1 1 d . . . N5 N 0.14818(12) 0.74201(17) 0.22395(13) 0.0277(4) Uani 1 1 d . . . C16 C 0.26214(14) 0.5554(2) 0.43989(15) 0.0323(5) Uani 1 1 d . . . H16A H 0.3180 0.5766 0.4668 0.039 Uiso 1 1 calc R . . C17 C 0.22360(15) 0.4698(3) 0.47964(16) 0.0357(5) Uani 1 1 d . . . H17A H 0.2520 0.4329 0.5332 0.043 Uiso 1 1 calc R . . C18 C 0.14248(16) 0.4390(3) 0.43949(17) 0.0387(6) Uani 1 1 d . . . H18A H 0.1139 0.3822 0.4661 0.046 Uiso 1 1 calc R . . C19 C 0.10318(14) 0.4912(3) 0.36030(16) 0.0345(5) Uani 1 1 d . . . H19A H 0.0479 0.4692 0.3317 0.041 Uiso 1 1 calc R . . C20 C 0.14524(13) 0.5759(2) 0.32322(14) 0.0260(4) Uani 1 1 d . . . C21 C 0.10888(13) 0.6378(2) 0.23863(15) 0.0274(5) Uani 1 1 d . . . C22 C 0.04082(14) 0.5891(3) 0.17741(17) 0.0370(6) Uani 1 1 d . . . H22A H 0.0135 0.5150 0.1887 0.044 Uiso 1 1 calc R . . C23 C 0.01381(16) 0.6517(3) 0.09933(18) 0.0455(7) Uani 1 1 d . . . H23A H -0.0321 0.6197 0.0560 0.055 Uiso 1 1 calc R . . C24 C 0.05337(17) 0.7602(3) 0.08449(18) 0.0407(6) Uani 1 1 d . . . H24A H 0.0351 0.8045 0.0316 0.049 Uiso 1 1 calc R . . C25 C 0.12059(15) 0.8025(3) 0.14916(16) 0.0359(5) Uani 1 1 d . . . H25A H 0.1481 0.8776 0.1399 0.043 Uiso 1 1 calc R . . P2 P -0.11504(4) 0.71019(7) 0.32655(4) 0.03719(18) Uani 1 1 d . . . F20 F -0.17663(14) 0.7964(2) 0.25735(14) 0.0699(6) Uani 1 1 d . . . F21 F -0.05450(11) 0.6197(2) 0.39689(11) 0.0620(5) Uani 1 1 d . . . F22 F -0.10381(13) 0.8189(2) 0.39712(14) 0.0705(6) Uani 1 1 d . . . F23 F -0.19079(11) 0.6544(2) 0.35482(12) 0.0650(6) Uani 1 1 d . . . F24 F -0.12488(13) 0.59833(18) 0.25891(11) 0.0612(5) Uani 1 1 d . . . F25 F -0.03927(13) 0.76553(19) 0.29959(15) 0.0630(6) Uani 1 1 d . . . P1 P 0.51149(4) 0.72954(6) 0.45616(4) 0.02807(17) Uani 1 1 d . . . F10 F 0.60377(10) 0.6951(2) 0.45813(11) 0.0532(5) Uani 1 1 d . . . F11 F 0.47910(12) 0.60322(16) 0.40331(12) 0.0562(5) Uani 1 1 d . . . F12 F 0.41821(10) 0.76487(16) 0.45280(11) 0.0437(4) Uani 1 1 d . . . F13 F 0.52338(13) 0.65809(18) 0.54467(11) 0.0594(5) Uani 1 1 d . . . F14 F 0.54193(10) 0.85832(15) 0.50713(10) 0.0433(4) Uani 1 1 d . . . F15 F 0.49998(9) 0.80338(16) 0.36771(9) 0.0404(4) 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 0.02233(18) 0.02672(19) 0.02719(19) 0.00045(10) 0.01387(13) -0.00308(9) N1 0.0230(9) 0.0314(10) 0.0309(10) 0.0008(8) 0.0138(8) -0.0004(8) N2 0.0190(8) 0.0318(10) 0.0245(9) 0.0032(7) 0.0105(7) -0.0011(7) N3 0.0251(9) 0.0321(10) 0.0298(10) -0.0002(8) 0.0134(8) -0.0011(8) C1 0.0307(12) 0.0375(13) 0.0388(13) 0.0012(10) 0.0214(10) -0.0011(10) C2 0.0345(12) 0.0471(15) 0.0401(13) -0.0010(11) 0.0236(11) 0.0058(11) C3 0.0344(12) 0.0398(14) 0.0369(13) -0.0056(10) 0.0150(10) 0.0086(11) C4 0.0309(12) 0.0303(12) 0.0345(12) -0.0003(9) 0.0105(9) 0.0011(9) C5 0.0190(9) 0.0334(12) 0.0280(11) 0.0009(9) 0.0080(8) 0.0003(9) C6 0.0210(10) 0.0316(12) 0.0270(10) 0.0031(9) 0.0072(8) -0.0017(9) C7 0.0320(12) 0.0310(12) 0.0328(12) 0.0036(9) 0.0090(9) -0.0041(10) C8 0.0304(12) 0.0424(14) 0.0343(12) 0.0101(10) 0.0119(10) -0.0096(10) C9 0.0269(11) 0.0424(14) 0.0291(11) 0.0063(10) 0.0134(9) -0.0031(10) C10 0.0211(10) 0.0388(13) 0.0242(10) 0.0032(9) 0.0089(8) -0.0004(9) C11 0.0216(11) 0.0378(13) 0.0265(12) 0.0009(9) 0.0079(9) -0.0008(8) C12 0.0317(12) 0.0485(15) 0.0311(12) 0.0002(11) 0.0174(10) 0.0004(11) C13 0.0372(13) 0.0522(16) 0.0380(13) -0.0066(12) 0.0187(11) 0.0063(12) C14 0.0409(13) 0.0396(14) 0.0415(13) -0.0071(11) 0.0157(11) 0.0058(11) C15 0.0350(12) 0.0329(13) 0.0387(13) -0.0025(10) 0.0171(10) 0.0007(10) N4 0.0228(9) 0.0300(10) 0.0285(9) 0.0009(8) 0.0129(7) -0.0013(7) N5 0.0246(10) 0.0296(10) 0.0301(10) 0.0019(7) 0.0100(8) 0.0007(7) C16 0.0278(11) 0.0371(13) 0.0330(12) 0.0048(10) 0.0103(9) -0.0011(10) C17 0.0373(13) 0.0370(13) 0.0350(12) 0.0085(10) 0.0140(10) 0.0006(10) C18 0.0365(13) 0.0392(14) 0.0477(14) 0.0078(11) 0.0237(11) -0.0056(11) C19 0.0259(11) 0.0371(13) 0.0437(14) 0.0022(10) 0.0153(10) -0.0067(10) C20 0.0214(10) 0.0276(11) 0.0330(11) -0.0034(9) 0.0140(9) 0.0001(8) C21 0.0218(10) 0.0299(11) 0.0336(12) -0.0019(9) 0.0131(9) 0.0033(9) C22 0.0254(11) 0.0417(14) 0.0426(14) -0.0018(11) 0.0081(10) -0.0031(10) C23 0.0291(12) 0.0576(18) 0.0435(15) -0.0030(13) 0.0003(11) 0.0019(12) C24 0.0358(14) 0.0530(17) 0.0320(14) 0.0062(11) 0.0077(11) 0.0125(11) C25 0.0328(12) 0.0389(14) 0.0373(13) 0.0067(11) 0.0120(10) 0.0055(11) P2 0.0375(4) 0.0485(4) 0.0301(3) -0.0054(3) 0.0169(3) -0.0077(3) F20 0.0728(13) 0.0765(14) 0.0668(13) 0.0272(11) 0.0303(11) 0.0164(11) F21 0.0541(10) 0.0800(14) 0.0449(10) -0.0011(9) 0.0031(8) 0.0035(10) F22 0.0674(12) 0.0828(15) 0.0736(13) -0.0410(12) 0.0399(11) -0.0090(11) F23 0.0456(10) 0.0984(16) 0.0562(11) 0.0179(11) 0.0226(8) -0.0172(10) F24 0.0797(13) 0.0581(11) 0.0419(9) -0.0164(8) 0.0115(9) -0.0134(10) F25 0.0627(12) 0.0613(12) 0.0860(15) -0.0183(10) 0.0550(11) -0.0166(9) P1 0.0294(3) 0.0313(3) 0.0277(3) 0.0005(2) 0.0149(3) 0.0029(2) F10 0.0348(8) 0.0800(13) 0.0457(9) -0.0083(9) 0.0128(7) 0.0219(8) F11 0.0706(12) 0.0411(9) 0.0665(11) -0.0156(8) 0.0349(9) -0.0111(8) F12 0.0307(8) 0.0639(11) 0.0435(9) -0.0031(7) 0.0216(7) 0.0005(7) F13 0.0887(13) 0.0527(10) 0.0471(10) 0.0207(8) 0.0361(9) 0.0247(10) F14 0.0453(8) 0.0420(9) 0.0424(8) -0.0107(7) 0.0121(7) -0.0006(7) F15 0.0368(8) 0.0569(10) 0.0310(7) 0.0081(7) 0.0152(6) 0.0000(7) _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 1.9233(18) . ? Cu1 N4 1.9819(19) . ? Cu1 N3 2.0369(19) . ? Cu1 N1 2.039(2) . ? Cu1 N5 2.183(2) . ? N1 C1 1.350(3) . ? N1 C5 1.352(3) . ? N2 C6 1.330(3) . ? N2 C10 1.349(3) . ? N3 C15 1.334(3) . ? N3 C11 1.356(3) . ? C1 C2 1.377(4) . ? C1 H1A 0.9500 . ? C2 C3 1.378(4) . ? C2 H2A 0.9500 . ? C3 C4 1.395(4) . ? C3 H3A 0.9500 . ? C4 C5 1.381(3) . ? C4 H4A 0.9500 . ? C5 C6 1.490(3) . ? C6 C7 1.389(3) . ? C7 C8 1.395(4) . ? C7 H7A 0.9500 . ? C8 C9 1.384(4) . ? C8 H8A 0.9500 . ? C9 C10 1.384(3) . ? C9 H9A 0.9500 . ? C10 C11 1.477(3) . ? C11 C12 1.387(3) . ? C12 C13 1.390(4) . ? C12 H12A 0.9500 . ? C13 C14 1.380(4) . ? C13 H13A 0.9500 . ? C14 C15 1.388(4) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? N4 C16 1.340(3) . ? N4 C20 1.360(3) . ? N5 C25 1.335(3) . ? N5 C21 1.338(3) . ? C16 C17 1.379(3) . ? C16 H16A 0.9500 . ? C17 C18 1.384(4) . ? C17 H17A 0.9500 . ? C18 C19 1.385(4) . ? C18 H18A 0.9500 . ? C19 C20 1.385(3) . ? C19 H19A 0.9500 . ? C20 C21 1.488(3) . ? C21 C22 1.390(3) . ? C22 C23 1.388(4) . ? C22 H22A 0.9500 . ? C23 C24 1.378(4) . ? C23 H23A 0.9500 . ? C24 C25 1.386(4) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? P2 F20 1.583(2) . ? P2 F24 1.5858(18) . ? P2 F25 1.5873(19) . ? P2 F22 1.5921(19) . ? P2 F23 1.5996(18) . ? P2 F21 1.611(2) . ? P1 F13 1.5872(17) . ? P1 F11 1.5897(18) . ? P1 F14 1.5919(16) . ? P1 F15 1.5993(15) . ? P1 F10 1.6021(16) . ? P1 F12 1.6148(16) . ? 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 N4 173.73(7) . . ? N2 Cu1 N3 80.77(8) . . ? N4 Cu1 N3 99.96(8) . . ? N2 Cu1 N1 80.16(8) . . ? N4 Cu1 N1 98.06(8) . . ? N3 Cu1 N1 159.02(8) . . ? N2 Cu1 N5 106.55(7) . . ? N4 Cu1 N5 79.66(8) . . ? N3 Cu1 N5 93.35(8) . . ? N1 Cu1 N5 100.38(7) . . ? C1 N1 C5 118.4(2) . . ? C1 N1 Cu1 127.64(16) . . ? C5 N1 Cu1 113.79(14) . . ? C6 N2 C10 122.34(19) . . ? C6 N2 Cu1 119.31(14) . . ? C10 N2 Cu1 118.29(16) . . ? C15 N3 C11 119.1(2) . . ? C15 N3 Cu1 127.89(16) . . ? C11 N3 Cu1 112.93(16) . . ? N1 C1 C2 122.2(2) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C1 C2 C3 119.4(2) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C2 C3 C4 119.1(2) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C3 118.6(2) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? N1 C5 C4 122.3(2) . . ? N1 C5 C6 113.9(2) . . ? C4 C5 C6 123.8(2) . . ? N2 C6 C7 120.7(2) . . ? N2 C6 C5 112.80(19) . . ? C7 C6 C5 126.5(2) . . ? C6 C7 C8 117.6(2) . . ? C6 C7 H7A 121.2 . . ? C8 C7 H7A 121.2 . . ? C9 C8 C7 121.1(2) . . ? C9 C8 H8A 119.4 . . ? C7 C8 H8A 119.4 . . ? C10 C9 C8 118.3(2) . . ? C10 C9 H9A 120.9 . . ? C8 C9 H9A 120.9 . . ? N2 C10 C9 120.0(2) . . ? N2 C10 C11 112.8(2) . . ? C9 C10 C11 127.2(2) . . ? N3 C11 C12 121.2(2) . . ? N3 C11 C10 114.7(2) . . ? C12 C11 C10 124.0(2) . . ? C11 C12 C13 119.4(2) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C14 C13 C12 119.0(2) . . ? C14 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? C13 C14 C15 118.9(3) . . ? C13 C14 H14A 120.6 . . ? C15 C14 H14A 120.6 . . ? N3 C15 C14 122.5(2) . . ? N3 C15 H15A 118.8 . . ? C14 C15 H15A 118.8 . . ? C16 N4 C20 119.5(2) . . ? C16 N4 Cu1 123.31(16) . . ? C20 N4 Cu1 116.55(15) . . ? C25 N5 C21 119.3(2) . . ? C25 N5 Cu1 127.91(17) . . ? C21 N5 Cu1 110.77(15) . . ? N4 C16 C17 122.5(2) . . ? N4 C16 H16A 118.8 . . ? C17 C16 H16A 118.8 . . ? C16 C17 C18 118.3(2) . . ? C16 C17 H17A 120.9 . . ? C18 C17 H17A 120.9 . . ? C17 C18 C19 119.7(2) . . ? C17 C18 H18A 120.1 . . ? C19 C18 H18A 120.1 . . ? C20 C19 C18 119.4(2) . . ? C20 C19 H19A 120.3 . . ? C18 C19 H19A 120.3 . . ? N4 C20 C19 120.6(2) . . ? N4 C20 C21 115.64(19) . . ? C19 C20 C21 123.8(2) . . ? N5 C21 C22 121.8(2) . . ? N5 C21 C20 115.3(2) . . ? C22 C21 C20 122.9(2) . . ? C23 C22 C21 118.2(2) . . ? C23 C22 H22A 120.9 . . ? C21 C22 H22A 120.9 . . ? C24 C23 C22 120.2(2) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C23 C24 C25 117.9(3) . . ? C23 C24 H24A 121.0 . . ? C25 C24 H24A 121.0 . . ? N5 C25 C24 122.6(3) . . ? N5 C25 H25A 118.7 . . ? C24 C25 H25A 118.7 . . ? F20 P2 F24 90.63(12) . . ? F20 P2 F25 90.95(13) . . ? F24 P2 F25 90.49(11) . . ? F20 P2 F22 91.33(14) . . ? F24 P2 F22 177.95(13) . . ? F25 P2 F22 90.07(11) . . ? F20 P2 F23 89.56(12) . . ? F24 P2 F23 89.91(12) . . ? F25 P2 F23 179.36(12) . . ? F22 P2 F23 89.52(12) . . ? F20 P2 F21 178.38(12) . . ? F24 P2 F21 88.72(11) . . ? F25 P2 F21 90.55(12) . . ? F22 P2 F21 89.30(12) . . ? F23 P2 F21 88.95(11) . . ? F13 P1 F11 91.91(11) . . ? F13 P1 F14 89.33(10) . . ? F11 P1 F14 178.35(11) . . ? F13 P1 F15 179.18(11) . . ? F11 P1 F15 88.91(10) . . ? F14 P1 F15 89.85(9) . . ? F13 P1 F10 90.50(11) . . ? F11 P1 F10 90.40(10) . . ? F14 P1 F10 90.67(10) . . ? F15 P1 F10 89.48(9) . . ? F13 P1 F12 90.28(10) . . ? F11 P1 F12 89.41(10) . . ? F14 P1 F12 89.51(9) . . ? F15 P1 F12 89.74(9) . . ? F10 P1 F12 179.20(10) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.498 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.068 # Attachment '- JP110.CIF' data_jp110 _database_code_depnum_ccdc_archive 'CCDC 770975' #TrackingRef '- JP110.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H23 Cu N5, 2(F6 P)' _chemical_formula_sum 'C29 H23 Cu F12 N5 P2' _chemical_formula_weight 795.01 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 Orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall -P2n2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.406(3) _cell_length_b 20.617(4) _cell_length_c 8.9854(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3039.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 113145 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0129 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3470 _reflns_number_gt 3394 _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^)+(0.0396P)^2^+2.9162P] 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 3470 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.012 _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 0.5000 0.804344(17) 0.2500 0.03368(13) Uani 1 2 d S . . N1 N 0.39945(12) 0.82231(9) 0.1218(2) 0.0367(4) Uani 1 1 d . . . N2 N 0.5000 0.89800(12) 0.2500 0.0322(5) Uani 1 2 d S . . N3 N 0.46293(11) 0.72645(9) 0.3834(2) 0.0329(4) Uani 1 1 d . . . C1 C 0.35247(16) 0.77867(13) 0.0535(3) 0.0480(6) Uani 1 1 d . . . H1A H 0.3612 0.7344 0.0732 0.058 Uiso 1 1 calc R . . C2 C 0.29135(17) 0.79600(15) -0.0454(3) 0.0514(7) Uani 1 1 d . . . H2A H 0.2598 0.7640 -0.0926 0.062 Uiso 1 1 calc R . . C3 C 0.27753(16) 0.86023(15) -0.0735(3) 0.0485(6) Uani 1 1 d . . . H3A H 0.2366 0.8732 -0.1404 0.058 Uiso 1 1 calc R . . C4 C 0.32478(16) 0.90546(13) -0.0015(3) 0.0429(5) Uani 1 1 d . . . H4A H 0.3159 0.9499 -0.0176 0.052 Uiso 1 1 calc R . . C5 C 0.38559(14) 0.88526(11) 0.0949(2) 0.0332(5) Uani 1 1 d . . . C6 C 0.44179(15) 0.92896(11) 0.1735(3) 0.0351(5) Uani 1 1 d . . . C7 C 0.43986(18) 0.99606(12) 0.1729(3) 0.0492(6) Uani 1 1 d . . . H7A H 0.3989 1.0188 0.1216 0.059 Uiso 1 1 calc R . . C8 C 0.5000 1.02839(17) 0.2500 0.0573(11) Uani 1 2 d S . . H8A H 0.5000 1.0740 0.2500 0.069 Uiso 1 2 calc SR . . C9 C 0.48020(13) 0.66819(11) 0.3206(3) 0.0357(5) Uani 1 1 d . . . C10 C 0.46052(16) 0.60936(13) 0.3904(4) 0.0526(7) Uani 1 1 d . . . C11 C 0.42406(19) 0.61353(18) 0.5316(4) 0.0676(10) Uani 1 1 d . . . H11A H 0.4090 0.5754 0.5819 0.081 Uiso 1 1 calc R . . C12 C 0.41052(18) 0.67124(19) 0.5953(4) 0.0641(9) Uani 1 1 d . . . H12A H 0.3880 0.6734 0.6913 0.077 Uiso 1 1 calc R . . C13 C 0.43005(15) 0.72852(15) 0.5184(3) 0.0461(6) Uani 1 1 d . . . C15 C 0.4150(2) 0.79330(18) 0.5852(3) 0.0657(9) Uani 1 1 d . . . H15A H 0.3842 0.8198 0.5159 0.099 Uiso 1 1 calc R . . H15B H 0.4668 0.8142 0.6064 0.099 Uiso 1 1 calc R . . H15C H 0.3844 0.7883 0.6768 0.099 Uiso 1 1 calc R . . C14 C 0.4808(2) 0.55092(13) 0.3146(5) 0.0719(12) Uani 1 1 d . . . H14A H 0.4664 0.5110 0.3579 0.086 Uiso 1 1 calc R . . P1 P 0.28009(4) 0.59039(3) 0.94474(8) 0.04445(18) Uani 1 1 d . . . F10 F 0.2674(4) 0.6375(3) 1.0810(5) 0.0862(15) Uani 0.731(16) 1 d P A 1 F11 F 0.3716(4) 0.6161(4) 0.9330(8) 0.0877(19) Uani 0.731(16) 1 d P A 1 F12 F 0.1852(3) 0.5728(2) 0.9493(8) 0.0779(14) Uani 0.731(16) 1 d P A 1 F15 F 0.30594(17) 0.53054(12) 1.0411(3) 0.1020(9) Uani 1 1 d . A 1 F14 F 0.25399(13) 0.65029(9) 0.8437(2) 0.0711(5) Uani 1 1 d . A 1 F13 F 0.2904(5) 0.5511(4) 0.8009(7) 0.114(3) Uani 0.731(16) 1 d P A 1 F10' F 0.2000(13) 0.5798(10) 1.040(4) 0.133(10) Uani 0.269(16) 1 d P A 2 F11' F 0.3168(19) 0.6295(7) 1.0865(16) 0.105(7) Uani 0.269(16) 1 d P A 2 F12' F 0.251(2) 0.5425(8) 0.821(3) 0.157(12) Uani 0.269(16) 1 d P A 2 F13' F 0.3709(11) 0.5898(9) 0.885(2) 0.086(6) Uani 0.269(16) 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 0.0344(2) 0.02200(19) 0.0446(2) 0.000 -0.00504(16) 0.000 N1 0.0349(9) 0.0304(9) 0.0448(11) -0.0017(8) -0.0031(8) 0.0010(7) N2 0.0417(14) 0.0241(11) 0.0307(13) 0.000 0.0018(11) 0.000 N3 0.0293(9) 0.0345(9) 0.0350(9) 0.0074(8) 0.0022(7) -0.0008(7) C1 0.0389(13) 0.0386(12) 0.0665(18) -0.0063(12) -0.0087(12) -0.0013(10) C2 0.0386(13) 0.0594(16) 0.0562(16) -0.0118(14) -0.0048(12) -0.0035(12) C3 0.0394(13) 0.0664(17) 0.0398(13) 0.0004(12) -0.0047(11) 0.0062(12) C4 0.0452(13) 0.0448(13) 0.0388(12) 0.0060(11) -0.0010(11) 0.0093(11) C5 0.0373(11) 0.0328(10) 0.0295(10) 0.0007(8) 0.0030(9) 0.0050(9) C6 0.0441(12) 0.0291(10) 0.0319(11) 0.0021(9) 0.0004(10) 0.0033(9) C7 0.0686(17) 0.0291(11) 0.0499(15) 0.0035(11) -0.0088(13) 0.0076(12) C8 0.087(3) 0.0218(15) 0.063(3) 0.000 -0.010(2) 0.000 C9 0.0288(10) 0.0285(10) 0.0496(13) 0.0068(10) -0.0107(9) -0.0023(8) C10 0.0397(13) 0.0385(13) 0.080(2) 0.0232(14) -0.0202(14) -0.0082(10) C11 0.0477(16) 0.070(2) 0.085(2) 0.050(2) -0.0118(16) -0.0138(15) C12 0.0414(14) 0.096(3) 0.0547(17) 0.0418(18) 0.0070(13) -0.0016(15) C13 0.0324(11) 0.0679(17) 0.0379(13) 0.0157(12) 0.0049(10) 0.0027(11) C15 0.068(2) 0.091(2) 0.0380(14) -0.0079(15) 0.0142(14) 0.0210(18) C14 0.064(2) 0.0272(11) 0.124(3) 0.0145(15) -0.040(2) -0.0069(12) P1 0.0489(4) 0.0434(4) 0.0410(4) 0.0025(3) 0.0037(3) -0.0049(3) F10 0.110(4) 0.104(3) 0.0441(18) -0.0206(17) 0.009(2) -0.017(3) F11 0.047(2) 0.121(5) 0.095(4) 0.025(3) -0.012(2) -0.015(3) F12 0.0570(17) 0.077(2) 0.100(3) 0.028(2) 0.004(2) -0.0282(17) F15 0.115(2) 0.0791(15) 0.111(2) 0.0472(14) -0.0253(16) -0.0070(14) F14 0.0746(12) 0.0587(11) 0.0801(13) 0.0238(10) -0.0073(11) -0.0039(9) F13 0.134(5) 0.120(5) 0.088(3) -0.062(3) -0.004(3) 0.037(4) F10' 0.092(10) 0.116(11) 0.19(2) 0.099(13) 0.090(12) 0.042(8) F11' 0.183(19) 0.060(6) 0.074(6) 0.002(5) -0.026(10) -0.063(9) F12' 0.29(3) 0.052(6) 0.130(15) -0.008(7) -0.146(18) -0.003(12) F13' 0.076(8) 0.084(9) 0.096(11) 0.046(7) 0.044(8) 0.031(7) _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 1.931(3) . ? Cu1 N1 2.046(2) 3_655 ? Cu1 N1 2.046(2) . ? Cu1 N3 2.0944(18) 3_655 ? Cu1 N3 2.0944(18) . ? N1 C1 1.334(3) . ? N1 C5 1.340(3) . ? N2 C6 1.339(3) 3_655 ? N2 C6 1.339(3) . ? N3 C13 1.328(3) . ? N3 C9 1.357(3) . ? C1 C2 1.387(4) . ? C1 H1A 0.9400 . ? C2 C3 1.367(4) . ? C2 H2A 0.9400 . ? C3 C4 1.374(4) . ? C3 H3A 0.9400 . ? C4 C5 1.385(3) . ? C4 H4A 0.9400 . ? C5 C6 1.470(3) . ? C6 C7 1.384(3) . ? C7 C8 1.378(3) . ? C7 H7A 0.9400 . ? C8 C7 1.378(3) 3_655 ? C8 H8A 0.9400 . ? C9 C10 1.403(3) . ? C9 C9 1.425(5) 3_655 ? C10 C11 1.406(5) . ? C10 C14 1.423(5) . ? C11 C12 1.339(5) . ? C11 H11A 0.9400 . ? C12 C13 1.405(4) . ? C12 H12A 0.9400 . ? C13 C15 1.485(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C14 C14 1.321(8) 3_655 ? C14 H14A 0.9400 . ? P1 F13 1.535(5) . ? P1 F12' 1.561(16) . ? P1 F15 1.566(2) . ? P1 F10 1.576(4) . ? P1 F10' 1.582(11) . ? P1 F13' 1.583(15) . ? P1 F14 1.5916(19) . ? P1 F11 1.596(5) . ? P1 F12 1.599(4) . ? P1 F11' 1.624(12) . ? 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 79.57(5) . 3_655 ? N2 Cu1 N1 79.57(5) . . ? N1 Cu1 N1 159.14(11) 3_655 . ? N2 Cu1 N3 140.07(5) . 3_655 ? N1 Cu1 N3 103.12(8) 3_655 3_655 ? N1 Cu1 N3 92.90(8) . 3_655 ? N2 Cu1 N3 140.07(5) . . ? N1 Cu1 N3 92.90(8) 3_655 . ? N1 Cu1 N3 103.12(8) . . ? N3 Cu1 N3 79.86(11) 3_655 . ? C1 N1 C5 118.2(2) . . ? C1 N1 Cu1 127.07(17) . . ? C5 N1 Cu1 114.46(15) . . ? C6 N2 C6 123.0(3) 3_655 . ? C6 N2 Cu1 118.48(14) 3_655 . ? C6 N2 Cu1 118.48(14) . . ? C13 N3 C9 119.6(2) . . ? C13 N3 Cu1 128.03(18) . . ? C9 N3 Cu1 112.31(15) . . ? N1 C1 C2 122.6(3) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 119.2(3) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 118.5(3) . . ? C2 C3 H3A 120.8 . . ? C4 C3 H3A 120.8 . . ? C3 C4 C5 119.8(2) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? N1 C5 C4 121.8(2) . . ? N1 C5 C6 113.6(2) . . ? C4 C5 C6 124.6(2) . . ? N2 C6 C7 119.7(2) . . ? N2 C6 C5 113.7(2) . . ? C7 C6 C5 126.6(2) . . ? C8 C7 C6 117.7(3) . . ? C8 C7 H7A 121.1 . . ? C6 C7 H7A 121.1 . . ? C7 C8 C7 122.1(3) . 3_655 ? C7 C8 H8A 118.9 . . ? C7 C8 H8A 118.9 3_655 . ? N3 C9 C10 122.1(3) . . ? N3 C9 C9 117.76(13) . 3_655 ? C10 C9 C9 120.19(18) . 3_655 ? C9 C10 C11 116.7(3) . . ? C9 C10 C14 117.7(3) . . ? C11 C10 C14 125.7(3) . . ? C12 C11 C10 120.7(3) . . ? C12 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C11 C12 C13 120.0(3) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? N3 C13 C12 121.0(3) . . ? N3 C13 C15 117.7(2) . . ? C12 C13 C15 121.3(3) . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C14 C10 122.13(19) 3_655 . ? C14 C14 H14A 118.9 3_655 . ? C10 C14 H14A 118.9 . . ? F13 P1 F15 91.1(3) . . ? F12' P1 F15 88.8(6) . . ? F13 P1 F10 173.6(4) . . ? F12' P1 F10 154.3(14) . . ? F15 P1 F10 95.3(2) . . ? F13 P1 F10' 118.2(13) . . ? F12' P1 F10' 92.3(12) . . ? F15 P1 F10' 79.5(6) . . ? F10 P1 F10' 63.7(13) . . ? F13 P1 F13' 66.9(8) . . ? F12' P1 F13' 92.6(12) . . ? F15 P1 F13' 85.7(5) . . ? F10 P1 F13' 113.0(8) . . ? F10' P1 F13' 164.3(9) . . ? F13 P1 F14 87.7(3) . . ? F12' P1 F14 90.1(6) . . ? F15 P1 F14 178.78(15) . . ? F10 P1 F14 86.0(2) . . ? F10' P1 F14 101.0(6) . . ? F13' P1 F14 93.8(5) . . ? F13 P1 F11 90.9(3) . . ? F12' P1 F11 116.9(14) . . ? F15 P1 F11 92.5(3) . . ? F10 P1 F11 88.3(3) . . ? F10' P1 F11 149.7(14) . . ? F14 P1 F11 87.6(3) . . ? F13 P1 F12 90.5(3) . . ? F12' P1 F12 64.8(14) . . ? F15 P1 F12 94.1(2) . . ? F10 P1 F12 89.5(3) . . ? F13' P1 F12 157.4(8) . . ? F14 P1 F12 85.9(2) . . ? F11 P1 F12 173.2(4) . . ? F13 P1 F11' 151.9(10) . . ? F12' P1 F11' 170.5(9) . . ? F15 P1 F11' 81.8(6) . . ? F10' P1 F11' 87.4(11) . . ? F13' P1 F11' 85.4(8) . . ? F14 P1 F11' 99.3(6) . . ? F11 P1 F11' 62.5(8) . . ? F12 P1 F11' 117.0(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.413 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.055 # Attachment '- JP130.CIF' data_JP130 _database_code_depnum_ccdc_archive 'CCDC 770976' #TrackingRef '- JP130.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C31 H23 Cu N5), 4(F6 P), 2(C H3 N O2), H2 O' _chemical_formula_sum 'C64 H54 Cu2 F24 N12 O5 P4' _chemical_formula_weight 1778.18 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' _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 8.3566(17) _cell_length_b 29.699(6) _cell_length_c 14.607(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.78(3) _cell_angle_gamma 90.00 _cell_volume 3612.6(13) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4611 _cell_measurement_theta_min 5.45 _cell_measurement_theta_max 49.08 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1788 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6682 _exptl_absorpt_correction_T_max 0.9765 _exptl_absorpt_process_details '(Blessing, 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 41695 _diffrn_reflns_av_R_equivalents 0.1356 _diffrn_reflns_av_sigmaI/netI 0.0696 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.50 _reflns_number_total 9078 _reflns_number_gt 7507 _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^)+(0.0584P)^2^+2.5234P] 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 9078 _refine_ls_number_parameters 608 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1536 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.022 _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 0.34909(4) 0.157731(11) 0.786476(19) 0.03725(11) Uani 1 1 d . . . N1 N 0.4543(3) 0.21567(8) 0.75105(15) 0.0414(5) Uani 1 1 d . . . N2 N 0.4242(2) 0.17994(8) 0.90688(13) 0.0363(4) Uani 1 1 d . . . N3 N 0.2592(3) 0.10931(8) 0.86525(15) 0.0426(5) Uani 1 1 d . . . C1 C 0.4629(4) 0.23182(12) 0.6656(2) 0.0540(7) Uani 1 1 d . . . H1A H 0.4204 0.2145 0.6155 0.065 Uiso 1 1 calc R . . C2 C 0.5314(5) 0.27274(13) 0.6490(2) 0.0634(9) Uani 1 1 d . . . H2A H 0.5347 0.2833 0.5885 0.076 Uiso 1 1 calc R . . C3 C 0.5950(5) 0.29798(13) 0.7219(3) 0.0621(9) Uani 1 1 d . . . H3A H 0.6426 0.3261 0.7122 0.074 Uiso 1 1 calc R . . C4 C 0.5878(4) 0.28145(12) 0.8100(2) 0.0539(7) Uani 1 1 d . . . H4A H 0.6302 0.2983 0.8607 0.065 Uiso 1 1 calc R . . C5 C 0.5188(3) 0.24049(10) 0.82288(18) 0.0404(5) Uani 1 1 d . . . C6 C 0.5054(3) 0.21871(10) 0.91273(17) 0.0388(5) Uani 1 1 d . . . C7 C 0.5677(4) 0.23419(12) 0.9980(2) 0.0510(7) Uani 1 1 d . . . H7A H 0.6279 0.2609 1.0033 0.061 Uiso 1 1 calc R . . C8 C 0.5391(4) 0.20930(13) 1.0752(2) 0.0567(8) Uani 1 1 d . . . H8A H 0.5796 0.2194 1.1336 0.068 Uiso 1 1 calc R . . C9 C 0.4514(4) 0.16966(13) 1.06721(18) 0.0521(7) Uani 1 1 d . . . H9A H 0.4304 0.1529 1.1195 0.062 Uiso 1 1 calc R . . C10 C 0.3954(3) 0.15536(10) 0.97969(17) 0.0400(5) Uani 1 1 d . . . C11 C 0.3035(3) 0.11395(10) 0.95638(17) 0.0412(5) Uani 1 1 d . . . C12 C 0.2665(4) 0.08156(12) 1.0185(2) 0.0535(7) Uani 1 1 d . . . H12A H 0.2991 0.0850 1.0812 0.064 Uiso 1 1 calc R . . C13 C 0.1810(5) 0.04398(13) 0.9879(2) 0.0625(9) Uani 1 1 d . . . H13A H 0.1541 0.0217 1.0296 0.075 Uiso 1 1 calc R . . C14 C 0.1358(5) 0.03959(12) 0.8958(2) 0.0602(8) Uani 1 1 d . . . H14A H 0.0773 0.0143 0.8735 0.072 Uiso 1 1 calc R . . C15 C 0.1778(4) 0.07301(11) 0.8367(2) 0.0519(7) Uani 1 1 d . . . H15A H 0.1473 0.0699 0.7736 0.062 Uiso 1 1 calc R . . N4 N 0.1900(3) 0.15261(8) 0.67385(14) 0.0400(5) Uani 1 1 d . . . N5 N 0.4728(3) 0.11291(8) 0.70066(14) 0.0399(5) Uani 1 1 d . . . C16 C 0.0454(3) 0.17234(11) 0.66740(19) 0.0465(6) Uani 1 1 d . . . H16A H 0.0157 0.1898 0.7169 0.056 Uiso 1 1 calc R . . C17 C -0.0613(4) 0.16796(13) 0.5908(2) 0.0564(8) Uani 1 1 d . . . H17A H -0.1626 0.1819 0.5881 0.068 Uiso 1 1 calc R . . C18 C -0.0158(5) 0.14268(17) 0.5185(2) 0.0752(12) Uani 1 1 d . . . H18A H -0.0857 0.1393 0.4652 0.090 Uiso 1 1 calc R . . C19 C 0.1321(5) 0.12235(16) 0.5245(2) 0.0731(12) Uani 1 1 d . . . H19A H 0.1640 0.1049 0.4755 0.088 Uiso 1 1 calc R . . C20 C 0.2344(4) 0.12771(11) 0.60390(18) 0.0465(6) Uani 1 1 d . . . C21 C 0.3938(4) 0.10548(10) 0.61789(18) 0.0456(6) Uani 1 1 d . . . C22 C 0.4586(5) 0.07840(14) 0.5525(2) 0.0633(9) Uani 1 1 d . . . H22A H 0.4039 0.0742 0.4943 0.076 Uiso 1 1 calc R . . C23 C 0.6047(5) 0.05795(15) 0.5748(2) 0.0727(11) Uani 1 1 d . . . H23A H 0.6507 0.0396 0.5317 0.087 Uiso 1 1 calc R . . C24 C 0.6831(5) 0.06446(13) 0.6603(2) 0.0611(9) Uani 1 1 d . . . H24A H 0.7819 0.0503 0.6766 0.073 Uiso 1 1 calc R . . C25 C 0.6137(3) 0.09237(10) 0.72206(18) 0.0428(6) Uani 1 1 d . . . C26 C 0.6906(3) 0.10109(10) 0.81625(18) 0.0418(6) Uani 1 1 d . . . C27 C 0.6739(4) 0.07018(12) 0.8861(2) 0.0555(7) Uani 1 1 d . . . H27A H 0.6169 0.0432 0.8740 0.067 Uiso 1 1 calc R . . C28 C 0.7418(6) 0.07936(15) 0.9739(2) 0.0715(11) Uani 1 1 d . . . H28A H 0.7297 0.0587 1.0215 0.086 Uiso 1 1 calc R . . C29 C 0.8267(5) 0.11837(15) 0.9920(2) 0.0691(11) Uani 1 1 d . . . H29A H 0.8733 0.1240 1.0517 0.083 Uiso 1 1 calc R . . C30 C 0.8437(4) 0.14910(15) 0.9233(3) 0.0657(9) Uani 1 1 d . . . H30A H 0.9018 0.1758 0.9357 0.079 Uiso 1 1 calc R . . C31 C 0.7742(4) 0.14030(13) 0.8353(2) 0.0556(7) Uani 1 1 d . . . H31A H 0.7846 0.1614 0.7883 0.067 Uiso 1 1 calc R . . P1 P 0.11292(10) 0.05907(3) 0.26930(5) 0.0534(2) Uani 1 1 d . . . F10 F 0.2325(4) 0.09803(9) 0.2418(2) 0.0958(8) Uani 1 1 d . . . F11 F -0.0007(4) 0.01877(13) 0.29370(19) 0.1007(9) Uani 1 1 d . . . F12 F 0.2086(3) 0.02512(8) 0.21033(14) 0.0722(6) Uani 1 1 d . . . F13 F 0.0187(3) 0.09358(12) 0.32726(17) 0.1047(11) Uani 1 1 d . . . F14 F 0.2302(3) 0.04710(10) 0.35769(15) 0.0843(8) Uani 1 1 d . . . F15 F -0.0029(3) 0.07073(10) 0.18145(15) 0.0837(8) Uani 1 1 d . . . P2 P 0.05754(11) 0.28628(4) 0.88052(6) 0.0604(2) Uani 1 1 d . . . F20 F -0.0536(13) 0.2509(3) 0.8164(7) 0.159(4) Uani 0.604(12) 1 d P A 1 F21 F 0.1442(14) 0.3207(5) 0.9342(10) 0.199(6) Uani 0.604(12) 1 d PU A 1 F22 F 0.1787(10) 0.2818(7) 0.8046(5) 0.195(7) Uani 0.604(12) 1 d P A 1 F23 F 0.1827(16) 0.2672(6) 0.9605(9) 0.107(5) Uani 0.396(12) 1 d P A 2 F24 F -0.0376(17) 0.3090(7) 0.8022(7) 0.117(7) Uani 0.396(12) 1 d P A 2 F25 F -0.0855(17) 0.2662(5) 0.9309(11) 0.111(6) Uani 0.396(12) 1 d P A 2 F20' F 0.084(3) 0.2453(5) 0.8273(10) 0.153(7) Uani 0.396(12) 1 d P A 2 F21' F 0.059(3) 0.3291(5) 0.9481(12) 0.174(8) Uani 0.396(12) 1 d P A 2 F22' F 0.2149(12) 0.3085(4) 0.8458(10) 0.105(4) Uani 0.396(12) 1 d P A 2 F23' F 0.1457(12) 0.2463(5) 0.9315(11) 0.165(6) Uani 0.604(12) 1 d P A 1 F24' F -0.0500(12) 0.3220(3) 0.8275(8) 0.120(4) Uani 0.604(12) 1 d P A 1 F25' F -0.0778(12) 0.2824(5) 0.9439(5) 0.124(5) Uani 0.604(12) 1 d P A 1 N100 N 0.6079(17) 0.0362(4) 0.2564(15) 0.090(5) Uani 0.67(3) 1 d P B 3 C100 C 0.624(2) 0.0810(7) 0.2980(13) 0.095(4) Uani 0.67(3) 1 d P B 3 H10A H 0.6919 0.0792 0.3549 0.143 Uiso 0.67(3) 1 calc PR B 3 H10B H 0.5183 0.0920 0.3107 0.143 Uiso 0.67(3) 1 calc PR B 3 H10C H 0.6708 0.1014 0.2561 0.143 Uiso 0.67(3) 1 calc PR B 3 O100 O 0.582(2) 0.0310(7) 0.1739(13) 0.151(8) Uani 0.67(3) 1 d P B 3 O101 O 0.6140(19) 0.0070(7) 0.3066(18) 0.207(10) Uani 0.67(3) 1 d PD B 3 C10' C 0.624(4) 0.0729(17) 0.290(4) 0.16(2) Uani 0.33(3) 1 d P B 4 H10D H 0.7101 0.0914 0.2700 0.246 Uiso 0.33(3) 1 calc PR B 4 H10E H 0.6517 0.0620 0.3514 0.246 Uiso 0.33(3) 1 calc PR B 4 H10F H 0.5260 0.0906 0.2886 0.246 Uiso 0.33(3) 1 calc PR B 4 N10' N 0.600(4) 0.038(2) 0.233(3) 0.124(18) Uani 0.33(3) 1 d P B 4 O10' O 0.578(4) 0.054(2) 0.1596(16) 0.21(2) Uani 0.33(3) 1 d P B 4 O11' O 0.623(3) -0.0005(12) 0.262(4) 0.140(13) Uani 0.33(3) 1 d P B 4 O201 O 0.8427(17) -0.0112(9) 0.4575(15) 0.152(18) Uani 0.15 1 d PD C 2 O200 O 0.983(4) -0.0207(9) 0.4726(17) 0.253(14) Uani 0.35 1 d PU . 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 0.04074(18) 0.04470(19) 0.02530(15) -0.00255(11) -0.00319(11) -0.00469(13) N1 0.0433(12) 0.0459(12) 0.0340(10) 0.0003(9) -0.0036(8) -0.0060(10) N2 0.0309(10) 0.0483(12) 0.0289(9) -0.0041(8) -0.0020(7) 0.0005(8) N3 0.0440(12) 0.0485(13) 0.0346(10) 0.0009(9) -0.0003(9) -0.0048(10) C1 0.0621(19) 0.0617(19) 0.0365(13) 0.0035(12) -0.0050(12) -0.0095(15) C2 0.073(2) 0.066(2) 0.0494(17) 0.0148(15) -0.0037(15) -0.0162(18) C3 0.061(2) 0.060(2) 0.065(2) 0.0105(16) 0.0018(15) -0.0183(16) C4 0.0467(16) 0.0591(19) 0.0548(17) -0.0045(14) -0.0018(13) -0.0142(14) C5 0.0327(12) 0.0487(15) 0.0388(12) -0.0034(10) -0.0031(9) -0.0013(10) C6 0.0324(11) 0.0505(14) 0.0330(11) -0.0061(10) -0.0016(9) -0.0013(10) C7 0.0483(15) 0.0614(19) 0.0416(14) -0.0138(13) -0.0060(11) -0.0070(13) C8 0.0587(18) 0.077(2) 0.0325(13) -0.0122(13) -0.0067(12) -0.0048(16) C9 0.0538(17) 0.073(2) 0.0283(12) -0.0038(12) -0.0014(11) -0.0023(15) C10 0.0356(12) 0.0536(15) 0.0302(11) -0.0017(10) -0.0014(9) 0.0025(11) C11 0.0388(13) 0.0531(15) 0.0316(11) 0.0000(10) 0.0019(9) 0.0013(11) C12 0.0582(18) 0.0618(19) 0.0407(14) 0.0083(13) 0.0048(12) -0.0023(15) C13 0.069(2) 0.063(2) 0.0565(18) 0.0112(15) 0.0119(16) -0.0113(17) C14 0.067(2) 0.0549(19) 0.0584(18) -0.0021(15) 0.0063(15) -0.0170(16) C15 0.0616(18) 0.0515(17) 0.0422(14) -0.0042(12) 0.0012(13) -0.0113(14) N4 0.0385(11) 0.0489(13) 0.0308(10) -0.0007(8) -0.0070(8) -0.0033(9) N5 0.0430(11) 0.0463(12) 0.0293(9) -0.0032(8) -0.0030(8) 0.0026(9) C16 0.0419(14) 0.0582(17) 0.0382(13) -0.0001(12) -0.0043(11) 0.0002(12) C17 0.0436(16) 0.071(2) 0.0518(17) 0.0009(14) -0.0133(13) 0.0040(14) C18 0.068(2) 0.104(3) 0.0480(18) -0.0171(19) -0.0304(16) 0.015(2) C19 0.070(2) 0.101(3) 0.0440(16) -0.0274(18) -0.0248(16) 0.020(2) C20 0.0504(15) 0.0551(16) 0.0317(12) -0.0071(11) -0.0098(10) 0.0005(13) C21 0.0548(16) 0.0492(16) 0.0315(12) -0.0055(10) -0.0048(11) 0.0039(12) C22 0.076(2) 0.073(2) 0.0398(15) -0.0166(14) -0.0069(14) 0.0180(18) C23 0.085(3) 0.082(3) 0.0494(18) -0.0210(17) 0.0000(17) 0.031(2) C24 0.063(2) 0.067(2) 0.0523(17) -0.0100(15) -0.0004(14) 0.0249(17) C25 0.0455(14) 0.0456(14) 0.0365(12) 0.0012(10) -0.0009(10) 0.0043(11) C26 0.0371(13) 0.0487(15) 0.0389(12) -0.0014(11) -0.0014(10) 0.0094(11) C27 0.067(2) 0.0511(17) 0.0467(16) 0.0048(13) -0.0028(14) 0.0071(15) C28 0.095(3) 0.071(2) 0.0452(17) 0.0090(16) -0.0092(17) 0.024(2) C29 0.069(2) 0.083(3) 0.0501(17) -0.0128(17) -0.0208(16) 0.025(2) C30 0.0498(18) 0.080(3) 0.065(2) -0.0156(18) -0.0123(15) -0.0020(17) C31 0.0479(16) 0.065(2) 0.0530(17) 0.0009(14) -0.0021(13) -0.0041(14) P1 0.0487(4) 0.0686(5) 0.0407(4) -0.0144(3) -0.0098(3) 0.0105(4) F10 0.0865(18) 0.0679(16) 0.131(2) -0.0054(15) -0.0021(17) -0.0057(14) F11 0.0871(18) 0.136(3) 0.0790(16) 0.0113(16) 0.0053(14) -0.0301(18) F12 0.0891(16) 0.0745(14) 0.0534(11) -0.0075(10) 0.0085(10) 0.0226(12) F13 0.0922(18) 0.153(3) 0.0650(13) -0.0495(16) -0.0156(12) 0.0599(19) F14 0.0844(16) 0.1068(19) 0.0555(11) -0.0243(12) -0.0307(11) 0.0317(14) F15 0.0837(16) 0.110(2) 0.0525(11) -0.0093(12) -0.0241(11) 0.0283(14) P2 0.0479(5) 0.0778(6) 0.0552(5) 0.0042(4) 0.0040(4) 0.0054(4) F20 0.119(7) 0.148(7) 0.204(9) -0.113(6) -0.019(6) 0.013(5) F21 0.125(7) 0.206(11) 0.246(12) -0.076(8) -0.108(8) -0.044(7) F22 0.068(5) 0.43(2) 0.087(5) 0.033(8) 0.026(4) 0.060(8) F23 0.074(6) 0.155(13) 0.085(5) 0.027(6) -0.026(4) -0.001(6) F24 0.055(4) 0.25(2) 0.045(4) 0.041(6) -0.006(3) 0.014(8) F25 0.046(4) 0.123(8) 0.160(13) 0.084(9) -0.011(6) -0.020(5) F20' 0.198(17) 0.133(9) 0.135(10) -0.094(8) 0.056(11) -0.036(11) F21' 0.230(19) 0.114(9) 0.185(13) -0.055(8) 0.057(13) 0.055(11) F22' 0.068(5) 0.130(8) 0.120(9) 0.030(7) 0.018(6) -0.028(5) F23' 0.083(6) 0.177(11) 0.237(15) 0.103(10) 0.024(6) 0.068(7) F24' 0.073(4) 0.085(4) 0.196(10) 0.069(5) -0.023(6) -0.012(3) F25' 0.062(4) 0.269(14) 0.043(2) 0.013(5) 0.010(2) 0.017(6) N100 0.060(5) 0.078(7) 0.136(15) -0.010(6) 0.028(6) -0.010(4) C100 0.082(8) 0.092(8) 0.111(8) -0.014(8) -0.003(6) 0.009(6) O100 0.109(9) 0.205(15) 0.143(14) -0.082(13) 0.041(9) -0.051(10) O101 0.135(9) 0.132(12) 0.37(3) 0.124(15) 0.105(13) 0.032(8) C10' 0.045(12) 0.15(3) 0.29(5) -0.15(3) -0.026(16) 0.016(12) N10' 0.041(9) 0.26(6) 0.070(15) 0.016(17) 0.013(7) 0.028(15) O10' 0.107(16) 0.46(6) 0.060(10) 0.06(2) 0.010(8) 0.08(3) O11' 0.068(11) 0.105(16) 0.25(4) -0.04(2) 0.040(16) 0.005(9) O201 0.21(4) 0.12(2) 0.14(3) 0.08(2) 0.13(3) 0.07(3) O200 0.29(2) 0.28(2) 0.204(19) 0.114(18) 0.089(16) -0.128(19) _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 1.933(2) . ? Cu1 N1 2.020(2) . ? Cu1 N3 2.025(2) . ? Cu1 N4 2.033(2) . ? Cu1 N5 2.151(2) . ? N1 C1 1.344(4) . ? N1 C5 1.356(3) . ? N2 C10 1.328(3) . ? N2 C6 1.335(4) . ? N3 C15 1.324(4) . ? N3 C11 1.359(3) . ? C1 C2 1.374(5) . ? C1 H1A 0.9400 . ? C2 C3 1.374(5) . ? C2 H2A 0.9400 . ? C3 C4 1.382(5) . ? C3 H3A 0.9400 . ? C4 C5 1.366(4) . ? C4 H4A 0.9400 . ? C5 C6 1.476(4) . ? C6 C7 1.388(3) . ? C7 C8 1.385(5) . ? C7 H7A 0.9400 . ? C8 C9 1.386(5) . ? C8 H8A 0.9400 . ? C9 C10 1.391(4) . ? C9 H9A 0.9400 . ? C10 C11 1.475(4) . ? C11 C12 1.375(4) . ? C12 C13 1.379(5) . ? C12 H12A 0.9400 . ? C13 C14 1.373(5) . ? C13 H13A 0.9400 . ? C14 C15 1.380(5) . ? C14 H14A 0.9400 . ? C15 H15A 0.9400 . ? N4 C20 1.338(4) . ? N4 C16 1.339(4) . ? N5 C25 1.340(4) . ? N5 C21 1.346(3) . ? C16 C17 1.378(4) . ? C16 H16A 0.9400 . ? C17 C18 1.375(5) . ? C17 H17A 0.9400 . ? C18 C19 1.371(6) . ? C18 H18A 0.9400 . ? C19 C20 1.391(4) . ? C19 H19A 0.9400 . ? C20 C21 1.486(4) . ? C21 C22 1.392(4) . ? C22 C23 1.378(5) . ? C22 H22A 0.9400 . ? C23 C24 1.373(5) . ? C23 H23A 0.9400 . ? C24 C25 1.387(4) . ? C24 H24A 0.9400 . ? C25 C26 1.492(4) . ? C26 C31 1.375(5) . ? C26 C27 1.389(4) . ? C27 C28 1.385(5) . ? C27 H27A 0.9400 . ? C28 C29 1.372(6) . ? C28 H28A 0.9400 . ? C29 C30 1.372(6) . ? C29 H29A 0.9400 . ? C30 C31 1.390(5) . ? C30 H30A 0.9400 . ? C31 H31A 0.9400 . ? P1 F15 1.580(2) . ? P1 F13 1.581(2) . ? P1 F12 1.585(2) . ? P1 F11 1.587(3) . ? P1 F14 1.594(2) . ? P1 F10 1.601(3) . ? P2 F21 1.445(8) . ? P2 F20' 1.471(9) . ? P2 F24 1.498(11) . ? P2 F25' 1.524(8) . ? P2 F23' 1.555(9) . ? P2 F24' 1.556(9) . ? P2 F22 1.568(7) . ? P2 F25 1.573(13) . ? P2 F22' 1.592(8) . ? P2 F23 1.606(11) . ? P2 F21' 1.608(13) . ? P2 F20 1.643(7) . ? N100 O101 1.13(2) . ? N100 O100 1.22(2) . ? N100 C100 1.46(2) . ? C100 H10A 0.9700 . ? C100 H10B 0.9700 . ? C100 H10C 0.9700 . ? C10' N10' 1.32(7) . ? C10' H10D 0.9700 . ? C10' H10E 0.9700 . ? C10' H10F 0.9700 . ? N10' O10' 1.18(5) . ? N10' O11' 1.23(6) . ? O200 O200 1.48(5) 3_756 ? 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 80.04(9) . . ? N2 Cu1 N3 80.39(10) . . ? N1 Cu1 N3 160.19(9) . . ? N2 Cu1 N4 154.50(10) . . ? N1 Cu1 N4 97.23(9) . . ? N3 Cu1 N4 99.10(9) . . ? N2 Cu1 N5 127.29(9) . . ? N1 Cu1 N5 97.89(10) . . ? N3 Cu1 N5 96.35(10) . . ? N4 Cu1 N5 78.20(9) . . ? C1 N1 C5 118.4(3) . . ? C1 N1 Cu1 126.8(2) . . ? C5 N1 Cu1 114.72(18) . . ? C10 N2 C6 123.2(2) . . ? C10 N2 Cu1 118.30(19) . . ? C6 N2 Cu1 118.49(17) . . ? C15 N3 C11 118.8(3) . . ? C15 N3 Cu1 127.20(19) . . ? C11 N3 Cu1 113.63(19) . . ? N1 C1 C2 122.3(3) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C1 C2 C3 119.0(3) . . ? C1 C2 H2A 120.5 . . ? C3 C2 H2A 120.5 . . ? C2 C3 C4 118.9(3) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? N1 C5 C4 121.5(3) . . ? N1 C5 C6 113.3(2) . . ? C4 C5 C6 125.3(3) . . ? N2 C6 C7 119.6(3) . . ? N2 C6 C5 113.4(2) . . ? C7 C6 C5 127.0(3) . . ? C8 C7 C6 118.4(3) . . ? C8 C7 H7A 120.8 . . ? C6 C7 H7A 120.8 . . ? C7 C8 C9 120.7(3) . . ? C7 C8 H8A 119.6 . . ? C9 C8 H8A 119.6 . . ? C8 C9 C10 118.1(3) . . ? C8 C9 H9A 120.9 . . ? C10 C9 H9A 120.9 . . ? N2 C10 C9 119.9(3) . . ? N2 C10 C11 113.5(2) . . ? C9 C10 C11 126.6(3) . . ? N3 C11 C12 121.1(3) . . ? N3 C11 C10 113.9(2) . . ? C12 C11 C10 124.9(3) . . ? C11 C12 C13 119.4(3) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C14 C13 C12 119.2(3) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C13 C14 C15 118.8(3) . . ? C13 C14 H14A 120.6 . . ? C15 C14 H14A 120.6 . . ? N3 C15 C14 122.6(3) . . ? N3 C15 H15A 118.7 . . ? C14 C15 H15A 118.7 . . ? C20 N4 C16 119.6(2) . . ? C20 N4 Cu1 117.07(19) . . ? C16 N4 Cu1 123.34(19) . . ? C25 N5 C21 119.4(2) . . ? C25 N5 Cu1 126.96(17) . . ? C21 N5 Cu1 113.67(19) . . ? N4 C16 C17 122.4(3) . . ? N4 C16 H16A 118.8 . . ? C17 C16 H16A 118.8 . . ? C18 C17 C16 118.2(3) . . ? C18 C17 H17A 120.9 . . ? C16 C17 H17A 120.9 . . ? C19 C18 C17 119.8(3) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C18 C19 C20 119.4(3) . . ? C18 C19 H19A 120.3 . . ? C20 C19 H19A 120.3 . . ? N4 C20 C19 120.6(3) . . ? N4 C20 C21 116.3(2) . . ? C19 C20 C21 123.1(3) . . ? N5 C21 C22 121.4(3) . . ? N5 C21 C20 114.7(2) . . ? C22 C21 C20 123.9(3) . . ? C23 C22 C21 118.7(3) . . ? C23 C22 H22A 120.7 . . ? C21 C22 H22A 120.7 . . ? C24 C23 C22 119.9(3) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 118.8(3) . . ? C23 C24 H24A 120.6 . . ? C25 C24 H24A 120.6 . . ? N5 C25 C24 121.8(3) . . ? N5 C25 C26 116.0(2) . . ? C24 C25 C26 122.2(3) . . ? C31 C26 C27 119.4(3) . . ? C31 C26 C25 120.4(3) . . ? C27 C26 C25 120.1(3) . . ? C28 C27 C26 119.4(3) . . ? C28 C27 H27A 120.3 . . ? C26 C27 H27A 120.3 . . ? C29 C28 C27 120.7(4) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C30 C29 C28 120.3(3) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C29 C30 C31 119.3(4) . . ? C29 C30 H30A 120.3 . . ? C31 C30 H30A 120.3 . . ? C26 C31 C30 120.9(3) . . ? C26 C31 H31A 119.6 . . ? C30 C31 H31A 119.6 . . ? F15 P1 F13 89.66(14) . . ? F15 P1 F12 90.04(13) . . ? F13 P1 F12 179.1(2) . . ? F15 P1 F11 90.58(16) . . ? F13 P1 F11 92.0(2) . . ? F12 P1 F11 88.90(17) . . ? F15 P1 F14 179.72(16) . . ? F13 P1 F14 90.62(13) . . ? F12 P1 F14 89.68(13) . . ? F11 P1 F14 89.38(16) . . ? F15 P1 F10 89.48(16) . . ? F13 P1 F10 90.84(19) . . ? F12 P1 F10 88.28(15) . . ? F11 P1 F10 177.18(18) . . ? F14 P1 F10 90.55(17) . . ? F21 P2 F20' 141.2(9) . . ? F21 P2 F24 107.9(9) . . ? F20' P2 F24 93.6(10) . . ? F21 P2 F25' 95.0(7) . . ? F20' P2 F25' 114.3(8) . . ? F24 P2 F25' 97.1(6) . . ? F21 P2 F23' 94.8(7) . . ? F20' P2 F23' 62.2(8) . . ? F24 P2 F23' 155.5(9) . . ? F25' P2 F23' 89.8(6) . . ? F21 P2 F24' 91.8(6) . . ? F20' P2 F24' 114.1(8) . . ? F25' P2 F24' 85.8(7) . . ? F23' P2 F24' 172.4(6) . . ? F21 P2 F22 96.8(8) . . ? F20' P2 F22 54.6(7) . . ? F24 P2 F22 80.3(6) . . ? F25' P2 F22 168.1(8) . . ? F23' P2 F22 88.1(7) . . ? F24' P2 F22 94.9(7) . . ? F21 P2 F25 112.3(9) . . ? F20' P2 F25 95.1(9) . . ? F24 P2 F25 98.8(8) . . ? F23' P2 F25 80.4(7) . . ? F24' P2 F25 93.5(7) . . ? F22 P2 F25 149.3(10) . . ? F21 P2 F22' 59.4(7) . . ? F20' P2 F22' 90.4(7) . . ? F24 P2 F22' 88.3(7) . . ? F25' P2 F22' 154.1(7) . . ? F23' P2 F22' 95.7(6) . . ? F24' P2 F22' 91.0(5) . . ? F25 P2 F22' 170.7(8) . . ? F21 P2 F23 65.7(7) . . ? F20' P2 F23 88.4(9) . . ? F24 P2 F23 170.8(8) . . ? F25' P2 F23 90.2(7) . . ? F24' P2 F23 156.7(7) . . ? F22 P2 F23 93.7(7) . . ? F25 P2 F23 90.0(8) . . ? F22' P2 F23 82.7(8) . . ? F20' P2 F21' 169.8(10) . . ? F24 P2 F21' 95.1(9) . . ? F25' P2 F21' 69.7(8) . . ? F23' P2 F21' 109.4(9) . . ? F24' P2 F21' 74.9(8) . . ? F22 P2 F21' 122.0(10) . . ? F25 P2 F21' 88.8(9) . . ? F22' P2 F21' 84.6(8) . . ? F23 P2 F21' 82.1(9) . . ? F21 P2 F20 174.5(6) . . ? F24 P2 F20 67.3(8) . . ? F25' P2 F20 83.4(5) . . ? F23' P2 F20 90.4(7) . . ? F24' P2 F20 82.9(5) . . ? F22 P2 F20 84.9(6) . . ? F25 P2 F20 66.9(7) . . ? F22' P2 F20 121.8(6) . . ? F23 P2 F20 119.4(7) . . ? F21' P2 F20 146.0(8) . . ? O101 N100 O100 122.5(17) . . ? O101 N100 C100 115(2) . . ? O100 N100 C100 122.0(19) . . ? O10' N10' O11' 134(7) . . ? O10' N10' C10' 105(6) . . ? O11' N10' C10' 120(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.638 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.067 # Attachment '- JP131.CIF' data_JP131 _database_code_depnum_ccdc_archive 'CCDC 770977' #TrackingRef '- JP131.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C26 H21 Cu N5), C4 H10 O, 8(F6 P), 3(H2 O)' _chemical_formula_sum 'C108 H100 Cu4 F48 N20 O4 P8' _chemical_formula_weight 3156.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 P2(1)/c _symmetry_space_group_name_Hall -P2ybc 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 19.703(4) _cell_length_b 11.221(2) _cell_length_c 15.989(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.56(3) _cell_angle_gamma 90.00 _cell_volume 3287.4(13) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2924 _cell_measurement_theta_min 5.57 _cell_measurement_theta_max 43.60 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1572 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6981 _exptl_absorpt_correction_T_max 0.9746 _exptl_absorpt_process_details '(Blessing, 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 45192 _diffrn_reflns_av_R_equivalents 0.1008 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6427 _reflns_number_gt 5858 _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^)+(0.0953P)^2^+2.9649P] 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 0.019(2) _refine_ls_number_reflns 6427 _refine_ls_number_parameters 498 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1707 _refine_ls_wR_factor_gt 0.1657 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.002 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 0.29326(2) 0.77600(3) 0.52048(2) 0.04114(16) Uani 1 1 d . . . N1 N 0.34648(15) 0.8651(3) 0.63596(18) 0.0455(6) Uani 1 1 d . . . N2 N 0.34290(15) 0.6444(2) 0.59528(18) 0.0420(6) Uani 1 1 d . . . N3 N 0.27225(16) 0.6434(3) 0.42629(18) 0.0462(6) Uani 1 1 d . . . C1 C 0.3476(2) 0.9825(3) 0.6492(3) 0.0560(9) Uani 1 1 d . . . H1A H 0.3239 1.0327 0.6000 0.067 Uiso 1 1 calc R . . C2 C 0.3828(2) 1.0328(4) 0.7336(3) 0.0643(11) Uani 1 1 d . . . H2A H 0.3830 1.1158 0.7415 0.077 Uiso 1 1 calc R . . C3 C 0.4169(2) 0.9595(4) 0.8047(3) 0.0633(10) Uani 1 1 d . . . H3A H 0.4403 0.9917 0.8624 0.076 Uiso 1 1 calc R . . C4 C 0.4171(2) 0.8382(4) 0.7917(2) 0.0565(9) Uani 1 1 d . . . H4A H 0.4409 0.7870 0.8401 0.068 Uiso 1 1 calc R . . C5 C 0.38173(19) 0.7931(3) 0.7064(2) 0.0447(7) Uani 1 1 d . . . C6 C 0.38038(18) 0.6652(3) 0.6823(2) 0.0447(7) Uani 1 1 d . . . C7 C 0.4148(2) 0.5724(4) 0.7395(2) 0.0526(8) Uani 1 1 d . . . H7A H 0.4408 0.5859 0.8011 0.063 Uiso 1 1 calc R . . C8 C 0.4097(2) 0.4592(3) 0.7030(3) 0.0561(9) Uani 1 1 d . . . H8A H 0.4318 0.3946 0.7406 0.067 Uiso 1 1 calc R . . C9 C 0.3728(2) 0.4399(3) 0.6122(3) 0.0534(8) Uani 1 1 d . . . H9A H 0.3707 0.3636 0.5872 0.064 Uiso 1 1 calc R . . C10 C 0.33905(18) 0.5361(3) 0.5593(2) 0.0445(7) Uani 1 1 d . . . C11 C 0.29771(19) 0.5349(3) 0.4617(2) 0.0456(7) Uani 1 1 d . . . C12 C 0.2852(2) 0.4346(4) 0.4089(3) 0.0581(9) Uani 1 1 d . . . H12A H 0.3030 0.3602 0.4347 0.070 Uiso 1 1 calc R . . C13 C 0.2463(3) 0.4442(4) 0.3180(3) 0.0673(11) Uani 1 1 d . . . H13A H 0.2377 0.3766 0.2808 0.081 Uiso 1 1 calc R . . C14 C 0.2202(3) 0.5540(4) 0.2822(3) 0.0659(11) Uani 1 1 d . . . H14A H 0.1934 0.5623 0.2203 0.079 Uiso 1 1 calc R . . C15 C 0.2340(2) 0.6514(4) 0.3382(2) 0.0579(9) Uani 1 1 d . . . H15A H 0.2158 0.7262 0.3136 0.069 Uiso 1 1 calc R . . N4 N 0.25878(16) 0.9120(3) 0.43630(18) 0.0452(6) Uani 1 1 d . . . N5 N 0.17878(17) 0.7982(3) 0.5154(2) 0.0473(6) Uani 1 1 d . . . C16 C 0.3024(2) 0.9655(3) 0.3981(3) 0.0543(9) Uani 1 1 d . . . H16A H 0.3522 0.9456 0.4187 0.065 Uiso 1 1 calc R . . C17 C 0.2755(2) 1.0476(4) 0.3303(3) 0.0588(9) Uani 1 1 d . . . H17A H 0.3061 1.0839 0.3046 0.071 Uiso 1 1 calc R . . C18 C 0.2030(2) 1.0751(4) 0.3012(3) 0.0630(10) Uani 1 1 d . . . H18A H 0.1834 1.1299 0.2540 0.076 Uiso 1 1 calc R . . C19 C 0.1586(2) 1.0245(4) 0.3396(3) 0.0605(10) Uani 1 1 d . . . H19A H 0.1088 1.0447 0.3197 0.073 Uiso 1 1 calc R . . C20 C 0.18842(19) 0.9417(3) 0.4091(2) 0.0452(7) Uani 1 1 d . . . C21 C 0.14454(19) 0.8846(3) 0.4547(2) 0.0483(8) Uani 1 1 d . . . C22 C 0.0726(2) 0.9177(4) 0.4389(3) 0.0679(11) Uani 1 1 d . . . H22A H 0.0498 0.9786 0.3978 0.081 Uiso 1 1 calc R . . C23 C 0.0356(3) 0.8591(5) 0.4849(4) 0.0797(14) Uani 1 1 d . . . H23A H -0.0134 0.8783 0.4734 0.096 Uiso 1 1 calc R . . C24 C 0.0692(3) 0.7738(4) 0.5467(4) 0.0725(12) Uani 1 1 d . . . H24A H 0.0442 0.7356 0.5792 0.087 Uiso 1 1 calc R . . C25 C 0.1425(2) 0.7435(4) 0.5613(3) 0.0582(9) Uani 1 1 d . . . C26 C 0.1821(3) 0.6493(5) 0.6259(3) 0.0767(13) Uani 1 1 d . . . H26A H 0.1929 0.5835 0.5934 0.115 Uiso 1 1 calc R . . H26B H 0.1519 0.6211 0.6580 0.115 Uiso 1 1 calc R . . H26C H 0.2272 0.6816 0.6684 0.115 Uiso 1 1 calc R . . P1 P 0.18326(6) 0.26026(10) 0.06407(7) 0.0583(3) Uani 1 1 d . . . F10 F 0.12745(19) 0.2236(4) 0.1096(3) 0.1221(16) Uani 1 1 d . . . F11 F 0.18829(19) 0.1276(3) 0.0351(3) 0.0997(10) Uani 1 1 d . . . F12 F 0.1810(2) 0.3959(3) 0.0935(2) 0.1073(12) Uani 1 1 d . . . F13 F 0.25014(18) 0.2372(3) 0.1562(2) 0.0890(9) Uani 1 1 d . . . F14 F 0.23931(17) 0.2983(3) 0.0185(2) 0.0833(8) Uani 1 1 d . . . F15 F 0.11616(17) 0.2857(3) -0.02615(18) 0.0821(8) Uani 1 1 d . . . P2 P 0.52173(6) 0.77568(8) 0.54827(6) 0.0493(2) Uani 1 1 d . . . F20 F 0.5179(2) 0.6441(2) 0.5134(2) 0.0948(10) Uani 1 1 d . . . F21 F 0.5400(2) 0.8177(3) 0.4654(2) 0.1050(11) Uani 1 1 d . . . F22 F 0.60523(17) 0.7545(3) 0.6085(2) 0.0992(10) Uani 1 1 d . . . F23 F 0.43740(18) 0.7918(4) 0.4897(2) 0.1085(12) Uani 1 1 d . . . F24 F 0.5303(2) 0.9080(3) 0.5828(2) 0.1070(13) Uani 1 1 d . . . F25 F 0.50318(18) 0.7316(3) 0.63161(19) 0.0854(9) Uani 1 1 d . . . O100 O -0.0334(10) 1.059(2) 0.2153(17) 0.125(7) Uani 0.25 1 d PD A 1 C101 C 0.0180(13) 1.2696(18) 0.2590(13) 0.079(7) Uani 0.25 1 d PD A 1 H10X H 0.0659 1.2357 0.2909 0.119 Uiso 0.25 1 calc PR A 1 H10Y H 0.0073 1.3287 0.2968 0.119 Uiso 0.25 1 calc PR A 1 H10Z H 0.0172 1.3070 0.2040 0.119 Uiso 0.25 1 calc PR A 1 C102 C -0.0380(15) 1.174(2) 0.237(2) 0.091(8) Uani 0.25 1 d PDU A 1 H10A H -0.0535 1.1707 0.2884 0.109 Uiso 0.25 1 calc PR A 1 H10B H -0.0797 1.2054 0.1868 0.109 Uiso 0.25 1 calc PR A 1 C103 C -0.0544(12) 0.964(2) 0.1603(17) 0.102(9) Uani 0.25 1 d P A 1 H10C H -0.0163 0.9429 0.1372 0.122 Uiso 0.25 1 calc PR A 1 H10D H -0.0992 0.9829 0.1091 0.122 Uiso 0.25 1 calc PR A 1 C104 C -0.0692(11) 0.8503(18) 0.2205(12) 0.071(5) Uani 0.25 1 d P A 1 H10E H -0.0734 0.8811 0.2751 0.107 Uiso 0.25 1 calc PR A 1 H10F H -0.0287 0.7948 0.2360 0.107 Uiso 0.25 1 calc PR A 1 H10G H -0.1140 0.8096 0.1850 0.107 Uiso 0.25 1 calc PR A 1 O200 O -0.0103(12) 1.0359(16) 0.1064(14) 0.129(8) Uani 0.25 1 d P B 2 O300 O 0.0051(14) 1.350(3) 0.2867(14) 0.118(9) Uani 0.20 1 d P C 2 O400 O -0.044(2) 1.252(4) 0.2570(17) 0.105(10) Uani 0.15 1 d PU D 3 O500 O -0.0293(19) 1.146(5) 0.188(3) 0.134(16) Uani 0.15 1 d P E 4 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 0.0499(3) 0.0388(2) 0.0314(2) 0.00234(14) 0.01102(17) 0.00329(15) N1 0.0500(15) 0.0467(15) 0.0360(13) -0.0017(11) 0.0112(11) -0.0002(12) N2 0.0473(14) 0.0425(14) 0.0365(13) 0.0025(11) 0.0159(11) 0.0022(11) N3 0.0564(16) 0.0436(15) 0.0365(14) -0.0014(11) 0.0145(12) 0.0033(12) C1 0.064(2) 0.0458(19) 0.051(2) -0.0067(16) 0.0135(17) 0.0014(16) C2 0.071(3) 0.056(2) 0.058(2) -0.0156(19) 0.014(2) -0.0027(19) C3 0.061(2) 0.075(3) 0.047(2) -0.0181(19) 0.0120(17) -0.005(2) C4 0.055(2) 0.068(2) 0.0392(17) -0.0004(17) 0.0086(15) 0.0017(18) C5 0.0455(17) 0.0519(19) 0.0352(16) 0.0004(13) 0.0132(13) 0.0007(14) C6 0.0453(16) 0.0518(19) 0.0365(15) 0.0053(14) 0.0145(13) 0.0002(14) C7 0.0532(19) 0.060(2) 0.0427(18) 0.0145(16) 0.0155(15) 0.0048(16) C8 0.060(2) 0.051(2) 0.057(2) 0.0197(17) 0.0208(17) 0.0101(16) C9 0.064(2) 0.0424(18) 0.059(2) 0.0083(16) 0.0281(18) 0.0062(16) C10 0.0491(17) 0.0421(17) 0.0445(17) 0.0042(13) 0.0198(14) 0.0021(14) C11 0.0550(18) 0.0428(17) 0.0420(17) -0.0011(13) 0.0213(14) -0.0006(14) C12 0.080(3) 0.0448(19) 0.056(2) -0.0037(16) 0.0327(19) 0.0039(18) C13 0.095(3) 0.057(2) 0.053(2) -0.0202(19) 0.032(2) -0.007(2) C14 0.084(3) 0.072(3) 0.0382(18) -0.0107(18) 0.0183(18) -0.003(2) C15 0.074(2) 0.056(2) 0.0395(18) -0.0015(16) 0.0159(17) 0.0053(18) N4 0.0522(15) 0.0430(15) 0.0365(13) -0.0003(11) 0.0118(12) 0.0008(12) N5 0.0543(16) 0.0472(15) 0.0432(15) -0.0070(12) 0.0214(13) -0.0075(12) C16 0.061(2) 0.053(2) 0.0502(19) 0.0090(16) 0.0214(17) -0.0020(16) C17 0.074(3) 0.054(2) 0.051(2) 0.0080(17) 0.0258(19) -0.0048(18) C18 0.075(3) 0.056(2) 0.054(2) 0.0153(18) 0.0184(19) 0.0067(19) C19 0.060(2) 0.064(2) 0.052(2) 0.0098(18) 0.0139(17) 0.0073(18) C20 0.0511(18) 0.0431(17) 0.0380(16) -0.0045(13) 0.0123(14) -0.0006(14) C21 0.0476(17) 0.0455(18) 0.0483(18) -0.0059(14) 0.0136(14) 0.0004(14) C22 0.055(2) 0.065(3) 0.083(3) 0.005(2) 0.025(2) 0.0052(19) C23 0.063(3) 0.078(3) 0.110(4) 0.000(3) 0.046(3) -0.001(2) C24 0.071(3) 0.070(3) 0.091(3) -0.002(2) 0.047(3) -0.008(2) C25 0.070(2) 0.059(2) 0.056(2) -0.0045(18) 0.035(2) -0.0079(18) C26 0.092(3) 0.079(3) 0.075(3) 0.016(2) 0.049(3) -0.003(3) P1 0.0663(6) 0.0638(6) 0.0469(5) 0.0080(4) 0.0232(5) 0.0127(5) F10 0.084(2) 0.201(4) 0.099(2) 0.072(3) 0.055(2) 0.040(2) F11 0.104(2) 0.0600(17) 0.133(3) -0.0044(17) 0.040(2) -0.0005(15) F12 0.139(3) 0.086(2) 0.081(2) -0.0165(16) 0.0214(19) 0.042(2) F13 0.0831(19) 0.114(2) 0.0605(16) 0.0174(15) 0.0155(14) 0.0265(16) F14 0.092(2) 0.092(2) 0.0783(19) 0.0047(15) 0.0452(16) -0.0081(16) F15 0.0824(18) 0.102(2) 0.0528(14) 0.0101(13) 0.0142(13) 0.0108(15) P2 0.0587(5) 0.0459(5) 0.0380(5) -0.0002(3) 0.0116(4) 0.0028(4) F20 0.147(3) 0.0477(14) 0.0701(17) -0.0104(12) 0.0170(18) 0.0049(15) F21 0.166(3) 0.095(2) 0.0710(18) 0.0013(17) 0.063(2) -0.029(2) F22 0.0589(16) 0.124(3) 0.098(2) 0.0002(19) 0.0082(16) 0.0031(16) F23 0.0721(19) 0.149(3) 0.079(2) 0.003(2) -0.0026(16) 0.0314(19) F24 0.186(4) 0.0514(15) 0.0627(16) -0.0090(12) 0.0210(19) 0.0128(18) F25 0.091(2) 0.111(2) 0.0612(16) 0.0113(15) 0.0364(15) -0.0065(16) O100 0.089(12) 0.16(2) 0.138(18) 0.042(18) 0.053(12) 0.016(13) C101 0.11(2) 0.069(13) 0.033(8) 0.016(8) 0.003(10) 0.034(14) C102 0.095(15) 0.099(18) 0.075(15) -0.008(14) 0.026(12) 0.006(14) C103 0.068(12) 0.12(2) 0.102(17) -0.079(17) 0.013(11) -0.007(12) C104 0.076(11) 0.078(12) 0.052(9) -0.027(9) 0.014(8) 0.010(9) O200 0.147(16) 0.076(11) 0.118(14) 0.051(10) -0.006(12) -0.004(10) O300 0.123(18) 0.14(2) 0.063(12) 0.073(15) 0.005(12) -0.021(17) O400 0.12(2) 0.13(2) 0.040(12) 0.004(14) 0.000(13) -0.029(19) O500 0.11(2) 0.18(4) 0.11(3) 0.11(3) 0.04(2) 0.08(3) _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 1.926(3) . ? Cu1 N4 1.982(3) . ? Cu1 N1 2.021(3) . ? Cu1 N3 2.048(3) . ? Cu1 N5 2.241(3) . ? N1 C1 1.333(5) . ? N1 C5 1.351(4) . ? N2 C6 1.334(4) . ? N2 C10 1.335(4) . ? N3 C15 1.334(5) . ? N3 C11 1.358(5) . ? C1 C2 1.390(5) . ? C1 H1A 0.9400 . ? C2 C3 1.363(6) . ? C2 H2A 0.9400 . ? C3 C4 1.377(6) . ? C3 H3A 0.9400 . ? C4 C5 1.379(5) . ? C4 H4A 0.9400 . ? C5 C6 1.484(5) . ? C6 C7 1.387(5) . ? C7 C8 1.386(6) . ? C7 H7A 0.9400 . ? C8 C9 1.380(6) . ? C8 H8A 0.9400 . ? C9 C10 1.383(5) . ? C9 H9A 0.9400 . ? C10 C11 1.471(5) . ? C11 C12 1.373(5) . ? C12 C13 1.376(6) . ? C12 H12A 0.9400 . ? C13 C14 1.376(7) . ? C13 H13A 0.9400 . ? C14 C15 1.376(6) . ? C14 H14A 0.9400 . ? C15 H15A 0.9400 . ? N4 C20 1.334(5) . ? N4 C16 1.363(5) . ? N5 C25 1.346(5) . ? N5 C21 1.363(5) . ? C16 C17 1.372(5) . ? C16 H16A 0.9400 . ? C17 C18 1.365(6) . ? C17 H17A 0.9400 . ? C18 C19 1.364(6) . ? C18 H18A 0.9400 . ? C19 C20 1.401(5) . ? C19 H19A 0.9400 . ? C20 C21 1.467(5) . ? C21 C22 1.396(5) . ? C22 C23 1.378(7) . ? C22 H22A 0.9400 . ? C23 C24 1.359(8) . ? C23 H23A 0.9400 . ? C24 C25 1.418(7) . ? C24 H24A 0.9400 . ? C25 C26 1.483(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? P1 F11 1.572(3) . ? P1 F10 1.580(3) . ? P1 F15 1.584(3) . ? P1 F14 1.589(3) . ? P1 F13 1.596(3) . ? P1 F12 1.599(3) . ? P2 F21 1.569(3) . ? P2 F20 1.570(3) . ? P2 F24 1.572(3) . ? P2 F25 1.585(3) . ? P2 F22 1.589(3) . ? P2 F23 1.589(3) . ? O100 C103 1.34(3) . ? O100 C102 1.345(18) . ? C101 C102 1.489(19) . ? C101 H10X 0.9700 . ? C101 H10Y 0.9700 . ? C101 H10Z 0.9700 . ? C102 H10A 0.9800 . ? C102 H10B 0.9800 . ? C103 C104 1.69(4) . ? C103 H10C 0.9800 . ? C103 H10D 0.9800 . ? C104 H10E 0.9700 . ? C104 H10F 0.9700 . ? C104 H10G 0.9700 . ? 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 N4 168.85(12) . . ? N2 Cu1 N1 80.63(12) . . ? N4 Cu1 N1 99.96(12) . . ? N2 Cu1 N3 79.56(12) . . ? N4 Cu1 N3 97.68(12) . . ? N1 Cu1 N3 158.09(12) . . ? N2 Cu1 N5 112.48(12) . . ? N4 Cu1 N5 78.51(12) . . ? N1 Cu1 N5 98.94(11) . . ? N3 Cu1 N5 97.21(12) . . ? C1 N1 C5 119.0(3) . . ? C1 N1 Cu1 127.3(3) . . ? C5 N1 Cu1 113.6(2) . . ? C6 N2 C10 122.1(3) . . ? C6 N2 Cu1 118.3(2) . . ? C10 N2 Cu1 119.7(2) . . ? C15 N3 C11 118.6(3) . . ? C15 N3 Cu1 127.6(3) . . ? C11 N3 Cu1 113.6(2) . . ? N1 C1 C2 121.9(4) . . ? N1 C1 H1A 119.1 . . ? C2 C1 H1A 119.1 . . ? C3 C2 C1 118.8(4) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C2 C3 C4 119.9(4) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C5 118.9(4) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? N1 C5 C4 121.5(3) . . ? N1 C5 C6 114.0(3) . . ? C4 C5 C6 124.4(3) . . ? N2 C6 C7 120.4(3) . . ? N2 C6 C5 112.9(3) . . ? C7 C6 C5 126.7(3) . . ? C8 C7 C6 117.9(3) . . ? C8 C7 H7A 121.1 . . ? C6 C7 H7A 121.1 . . ? C9 C8 C7 121.0(3) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C8 C9 C10 118.1(4) . . ? C8 C9 H9A 121.0 . . ? C10 C9 H9A 121.0 . . ? N2 C10 C9 120.6(3) . . ? N2 C10 C11 112.8(3) . . ? C9 C10 C11 126.6(3) . . ? N3 C11 C12 121.5(3) . . ? N3 C11 C10 114.2(3) . . ? C12 C11 C10 124.3(3) . . ? C11 C12 C13 119.4(4) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C12 C13 C14 119.1(4) . . ? C12 C13 H13A 120.4 . . ? C14 C13 H13A 120.4 . . ? C15 C14 C13 119.1(4) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? N3 C15 C14 122.2(4) . . ? N3 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? C20 N4 C16 119.7(3) . . ? C20 N4 Cu1 118.0(2) . . ? C16 N4 Cu1 121.9(2) . . ? C25 N5 C21 119.3(3) . . ? C25 N5 Cu1 131.2(3) . . ? C21 N5 Cu1 109.5(2) . . ? N4 C16 C17 121.6(4) . . ? N4 C16 H16A 119.2 . . ? C17 C16 H16A 119.2 . . ? C18 C17 C16 118.3(4) . . ? C18 C17 H17A 120.8 . . ? C16 C17 H17A 120.8 . . ? C19 C18 C17 121.1(4) . . ? C19 C18 H18A 119.5 . . ? C17 C18 H18A 119.5 . . ? C18 C19 C20 118.7(4) . . ? C18 C19 H19A 120.6 . . ? C20 C19 H19A 120.6 . . ? N4 C20 C19 120.5(3) . . ? N4 C20 C21 117.4(3) . . ? C19 C20 C21 122.1(3) . . ? N5 C21 C22 121.5(4) . . ? N5 C21 C20 115.9(3) . . ? C22 C21 C20 122.6(4) . . ? C23 C22 C21 118.5(4) . . ? C23 C22 H22A 120.8 . . ? C21 C22 H22A 120.8 . . ? C24 C23 C22 120.9(4) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 C25 118.8(4) . . ? C23 C24 H24A 120.6 . . ? C25 C24 H24A 120.6 . . ? N5 C25 C24 120.9(4) . . ? N5 C25 C26 117.1(4) . . ? C24 C25 C26 121.9(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? F11 P1 F10 91.1(2) . . ? F11 P1 F15 91.39(19) . . ? F10 P1 F15 88.71(19) . . ? F11 P1 F14 89.40(19) . . ? F10 P1 F14 179.5(2) . . ? F15 P1 F14 91.27(17) . . ? F11 P1 F13 89.9(2) . . ? F10 P1 F13 90.60(19) . . ? F15 P1 F13 178.55(19) . . ? F14 P1 F13 89.41(18) . . ? F11 P1 F12 177.9(2) . . ? F10 P1 F12 90.7(2) . . ? F15 P1 F12 89.56(18) . . ? F14 P1 F12 88.8(2) . . ? F13 P1 F12 89.17(19) . . ? F21 P2 F20 88.74(19) . . ? F21 P2 F24 89.1(2) . . ? F20 P2 F24 176.5(2) . . ? F21 P2 F25 179.3(2) . . ? F20 P2 F25 90.57(19) . . ? F24 P2 F25 91.57(19) . . ? F21 P2 F22 92.8(2) . . ? F20 P2 F22 88.7(2) . . ? F24 P2 F22 88.5(2) . . ? F25 P2 F22 87.22(19) . . ? F21 P2 F23 89.1(2) . . ? F20 P2 F23 89.7(2) . . ? F24 P2 F23 93.1(2) . . ? F25 P2 F23 90.9(2) . . ? F22 P2 F23 177.6(2) . . ? C103 O100 C102 153(3) . . ? C102 C101 H10X 109.5 . . ? C102 C101 H10Y 109.5 . . ? H10X C101 H10Y 109.5 . . ? C102 C101 H10Z 109.5 . . ? H10X C101 H10Z 109.5 . . ? H10Y C101 H10Z 109.5 . . ? O100 C102 C101 130(2) . . ? O100 C102 H10A 104.8 . . ? C101 C102 H10A 104.8 . . ? O100 C102 H10B 104.8 . . ? C101 C102 H10B 104.8 . . ? H10A C102 H10B 105.8 . . ? O100 C103 C104 107(2) . . ? O100 C103 H10C 110.2 . . ? C104 C103 H10C 110.2 . . ? O100 C103 H10D 110.2 . . ? C104 C103 H10D 110.2 . . ? H10C C103 H10D 108.5 . . ? C103 C104 H10E 109.5 . . ? C103 C104 H10F 109.5 . . ? H10E C104 H10F 109.5 . . ? C103 C104 H10G 109.5 . . ? H10E C104 H10G 109.5 . . ? H10F C104 H10G 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.775 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.082 # Attachment '- JP133.CIF' data_jp133 _database_code_depnum_ccdc_archive 'CCDC 770978' #TrackingRef '- JP133.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H27 Cu N5, 2(F6 P)' _chemical_formula_sum 'C37 H27 Cu F12 N5 P2' _chemical_formula_weight 895.12 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 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 11.257(2) _cell_length_b 13.441(3) _cell_length_c 24.554(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.57(3) _cell_angle_gamma 90.00 _cell_volume 3639.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1804 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6944 _exptl_absorpt_correction_T_max 0.9922 _exptl_absorpt_process_details '(Blessing, 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 48482 _diffrn_reflns_av_R_equivalents 0.1345 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 26.50 _reflns_number_total 7516 _reflns_number_gt 6825 _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^)+(0.0438P)^2^+3.0928P] 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 7516 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1249 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 0.50823(3) 0.76493(2) 0.598119(13) 0.03239(10) Uani 1 1 d . . . N1 N 0.36686(19) 0.85545(16) 0.60790(9) 0.0361(4) Uani 1 1 d . . . N2 N 0.3781(2) 0.66890(16) 0.58840(9) 0.0371(5) Uani 1 1 d . . . N3 N 0.5977(2) 0.64251(15) 0.57908(10) 0.0390(5) Uani 1 1 d . . . C1 C 0.3727(3) 0.9522(2) 0.62093(12) 0.0429(6) Uani 1 1 d . . . H1A H 0.4457 0.9866 0.6216 0.052 Uiso 1 1 calc R . . C2 C 0.2752(3) 1.0032(2) 0.63336(14) 0.0493(7) Uani 1 1 d . . . H2A H 0.2819 1.0711 0.6428 0.059 Uiso 1 1 calc R . . C3 C 0.1680(3) 0.9531(3) 0.63169(14) 0.0563(8) Uani 1 1 d . . . H3A H 0.1003 0.9865 0.6399 0.068 Uiso 1 1 calc R . . C4 C 0.1603(3) 0.8533(3) 0.61791(14) 0.0522(7) Uani 1 1 d . . . H4A H 0.0874 0.8182 0.6163 0.063 Uiso 1 1 calc R . . C5 C 0.2615(2) 0.8059(2) 0.60659(11) 0.0392(5) Uani 1 1 d . . . C6 C 0.2677(2) 0.6987(2) 0.59402(12) 0.0418(6) Uani 1 1 d . . . C7 C 0.1738(3) 0.6308(3) 0.58919(15) 0.0559(8) Uani 1 1 d . . . H7A H 0.0960 0.6509 0.5931 0.067 Uiso 1 1 calc R . . C8 C 0.1974(3) 0.5326(3) 0.57852(16) 0.0641(9) Uani 1 1 d . . . H8A H 0.1349 0.4852 0.5752 0.077 Uiso 1 1 calc R . . C9 C 0.3114(3) 0.5033(2) 0.57268(15) 0.0581(8) Uani 1 1 d . . . H9A H 0.3272 0.4365 0.5653 0.070 Uiso 1 1 calc R . . C10 C 0.4023(3) 0.5740(2) 0.57780(12) 0.0435(6) Uani 1 1 d . . . C11 C 0.5299(3) 0.55843(19) 0.57407(11) 0.0418(6) Uani 1 1 d . . . C12 C 0.5800(3) 0.4665(2) 0.56675(14) 0.0553(8) Uani 1 1 d . . . H12A H 0.5317 0.4089 0.5627 0.066 Uiso 1 1 calc R . . C13 C 0.7016(3) 0.4604(2) 0.56540(15) 0.0602(8) Uani 1 1 d . . . H13A H 0.7373 0.3984 0.5610 0.072 Uiso 1 1 calc R . . C14 C 0.7702(3) 0.5457(2) 0.57051(15) 0.0564(8) Uani 1 1 d . . . H14A H 0.8530 0.5430 0.5692 0.068 Uiso 1 1 calc R . . C15 C 0.7157(3) 0.6355(2) 0.57754(13) 0.0467(6) Uani 1 1 d . . . H15A H 0.7630 0.6937 0.5814 0.056 Uiso 1 1 calc R . . N4 N 0.62928(18) 0.86747(14) 0.58424(9) 0.0333(4) Uani 1 1 d . . . N5 N 0.5970(2) 0.80005(16) 0.68343(9) 0.0377(5) Uani 1 1 d . . . C16 C 0.6578(2) 0.88362(18) 0.53414(12) 0.0368(5) Uani 1 1 d . . . C17 C 0.7591(3) 0.9398(2) 0.52951(14) 0.0478(7) Uani 1 1 d . . . H17A H 0.7794 0.9495 0.4946 0.057 Uiso 1 1 calc R . . C18 C 0.8295(3) 0.9812(2) 0.57665(16) 0.0557(8) Uani 1 1 d . . . H18A H 0.8983 1.0190 0.5740 0.067 Uiso 1 1 calc R . . C19 C 0.7985(3) 0.9668(2) 0.62722(15) 0.0524(7) Uani 1 1 d . . . H19A H 0.8445 0.9961 0.6594 0.063 Uiso 1 1 calc R . . C20 C 0.6983(2) 0.90849(18) 0.63033(12) 0.0395(6) Uani 1 1 d . . . C21 C 0.6615(3) 0.8846(2) 0.68351(12) 0.0432(6) Uani 1 1 d . . . C22 C 0.6863(3) 0.9471(3) 0.72909(15) 0.0614(8) Uani 1 1 d . . . H22A H 0.7304 1.0062 0.7280 0.074 Uiso 1 1 calc R . . C23 C 0.6453(5) 0.9209(3) 0.77589(16) 0.0781(12) Uani 1 1 d . . . H23A H 0.6603 0.9624 0.8073 0.094 Uiso 1 1 calc R . . C24 C 0.5821(4) 0.8338(3) 0.77680(15) 0.0708(10) Uani 1 1 d . . . H24A H 0.5546 0.8148 0.8090 0.085 Uiso 1 1 calc R . . C25 C 0.5593(3) 0.7741(2) 0.72979(12) 0.0480(7) Uani 1 1 d . . . C26 C 0.4934(3) 0.6783(2) 0.72851(12) 0.0479(7) Uani 1 1 d . . . C27 C 0.3802(3) 0.6720(3) 0.74299(16) 0.0668(10) Uani 1 1 d . . . H27A H 0.3437 0.7294 0.7541 0.080 Uiso 1 1 calc R . . C28 C 0.3216(4) 0.5816(4) 0.74099(19) 0.0829(13) Uani 1 1 d . . . H28A H 0.2443 0.5782 0.7498 0.100 Uiso 1 1 calc R . . C29 C 0.3745(4) 0.4968(3) 0.72631(19) 0.0775(12) Uani 1 1 d . . . H29A H 0.3341 0.4355 0.7258 0.093 Uiso 1 1 calc R . . C30 C 0.4876(4) 0.5012(3) 0.71225(16) 0.0635(9) Uani 1 1 d . . . H30A H 0.5248 0.4430 0.7026 0.076 Uiso 1 1 calc R . . C31 C 0.5452(3) 0.5921(2) 0.71257(13) 0.0508(7) Uani 1 1 d . . . H31A H 0.6206 0.5957 0.7018 0.061 Uiso 1 1 calc R . . C32 C 0.5765(2) 0.84321(18) 0.48422(11) 0.0365(5) Uani 1 1 d . . . C33 C 0.6256(3) 0.8019(2) 0.44145(13) 0.0449(6) Uani 1 1 d . . . H33A H 0.7101 0.7953 0.4458 0.054 Uiso 1 1 calc R . . C34 C 0.5506(3) 0.7705(2) 0.39270(14) 0.0533(7) Uani 1 1 d . . . H34A H 0.5846 0.7437 0.3640 0.064 Uiso 1 1 calc R . . C35 C 0.4267(3) 0.7784(2) 0.38606(14) 0.0549(7) Uani 1 1 d . . . H35A H 0.3763 0.7575 0.3528 0.066 Uiso 1 1 calc R . . C36 C 0.3764(3) 0.8171(2) 0.42840(13) 0.0488(7) Uani 1 1 d . . . H36A H 0.2917 0.8211 0.4242 0.059 Uiso 1 1 calc R . . C37 C 0.4508(2) 0.8501(2) 0.47719(12) 0.0417(6) Uani 1 1 d . . . H37A H 0.4161 0.8772 0.5057 0.050 Uiso 1 1 calc R . . P1 P 0.46391(8) 0.80115(7) 0.21654(4) 0.0535(2) Uani 1 1 d . . . F10 F 0.4202(3) 0.71959(19) 0.25405(14) 0.1046(10) Uani 1 1 d . . . F11 F 0.5951(2) 0.7540(2) 0.22656(16) 0.1133(12) Uani 1 1 d . . . F12 F 0.5047(2) 0.8839(2) 0.17832(12) 0.0947(8) Uani 1 1 d . . . F13 F 0.4236(2) 0.7312(2) 0.16371(13) 0.0990(10) Uani 1 1 d . . . F14 F 0.5031(2) 0.87204(17) 0.26837(9) 0.0793(7) Uani 1 1 d . . . F15 F 0.33115(18) 0.84783(17) 0.20434(11) 0.0741(6) Uani 1 1 d . . . P2 P 0.99284(7) 0.74783(6) 0.44077(4) 0.0524(2) Uani 1 1 d . . . F20 F 0.9326(3) 0.7106(3) 0.48886(16) 0.1275(13) Uani 1 1 d . A 1 F21 F 1.0407(3) 0.6426(2) 0.4308(3) 0.185(2) Uani 1 1 d . A 1 F22 F 1.1150(2) 0.7748(2) 0.48206(12) 0.1003(9) Uani 1 1 d . A 1 F23 F 0.9425(2) 0.85488(16) 0.44731(14) 0.0918(8) Uani 1 1 d . A 1 F24 F 0.8708(2) 0.7219(3) 0.39955(16) 0.1176(11) Uani 1 1 d . A 1 F25 F 1.0526(2) 0.7906(2) 0.39181(11) 0.0974(9) Uani 1 1 d . 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 0.02974(16) 0.03042(16) 0.03688(18) 0.00177(11) 0.00638(12) -0.00151(11) N1 0.0323(10) 0.0396(11) 0.0375(11) 0.0055(8) 0.0095(9) 0.0007(8) N2 0.0373(11) 0.0375(11) 0.0355(11) 0.0052(8) 0.0051(9) -0.0061(9) N3 0.0417(12) 0.0336(10) 0.0404(12) 0.0002(9) 0.0054(9) 0.0016(9) C1 0.0375(13) 0.0437(14) 0.0486(16) 0.0055(11) 0.0114(11) 0.0040(11) C2 0.0475(16) 0.0489(16) 0.0538(17) 0.0051(13) 0.0157(13) 0.0124(12) C3 0.0413(15) 0.073(2) 0.0573(19) 0.0036(16) 0.0164(14) 0.0148(14) C4 0.0325(14) 0.070(2) 0.0557(18) 0.0067(15) 0.0123(12) -0.0007(13) C5 0.0315(12) 0.0518(15) 0.0342(13) 0.0074(11) 0.0062(10) -0.0020(10) C6 0.0367(13) 0.0506(15) 0.0372(14) 0.0080(11) 0.0053(10) -0.0086(11) C7 0.0417(16) 0.0651(19) 0.060(2) 0.0075(15) 0.0080(14) -0.0172(14) C8 0.057(2) 0.0597(19) 0.072(2) 0.0073(17) 0.0055(16) -0.0294(16) C9 0.067(2) 0.0417(15) 0.062(2) 0.0015(13) 0.0042(16) -0.0185(14) C10 0.0501(16) 0.0382(13) 0.0391(14) 0.0032(11) 0.0018(12) -0.0086(11) C11 0.0495(15) 0.0349(13) 0.0383(14) 0.0011(10) 0.0027(11) -0.0003(11) C12 0.072(2) 0.0363(14) 0.0546(18) -0.0032(13) 0.0053(15) 0.0015(13) C13 0.073(2) 0.0448(16) 0.060(2) -0.0052(14) 0.0055(16) 0.0191(15) C14 0.0526(18) 0.0562(18) 0.0582(19) -0.0068(14) 0.0062(14) 0.0169(14) C15 0.0426(15) 0.0452(14) 0.0508(17) -0.0028(12) 0.0060(12) 0.0056(12) N4 0.0285(10) 0.0301(9) 0.0410(12) 0.0013(8) 0.0062(8) 0.0016(7) N5 0.0378(11) 0.0403(11) 0.0327(11) 0.0011(9) 0.0016(9) 0.0065(9) C16 0.0301(12) 0.0331(12) 0.0482(15) 0.0078(10) 0.0104(10) 0.0036(9) C17 0.0360(14) 0.0431(14) 0.0663(19) 0.0134(13) 0.0152(13) -0.0001(11) C18 0.0345(14) 0.0463(16) 0.084(2) 0.0113(15) 0.0055(14) -0.0095(12) C19 0.0394(15) 0.0435(15) 0.068(2) -0.0006(14) -0.0042(13) -0.0071(12) C20 0.0353(13) 0.0329(12) 0.0465(15) -0.0003(10) -0.0007(11) 0.0013(10) C21 0.0422(14) 0.0389(13) 0.0442(15) -0.0042(11) -0.0019(11) 0.0046(11) C22 0.072(2) 0.0533(18) 0.0525(19) -0.0132(14) -0.0017(16) -0.0015(15) C23 0.116(4) 0.068(2) 0.045(2) -0.0163(17) 0.004(2) 0.009(2) C24 0.104(3) 0.072(2) 0.0371(17) -0.0006(15) 0.0164(18) 0.014(2) C25 0.0534(17) 0.0536(16) 0.0357(14) 0.0074(12) 0.0053(12) 0.0156(13) C26 0.0506(16) 0.0594(17) 0.0328(14) 0.0149(12) 0.0060(12) 0.0091(13) C27 0.063(2) 0.083(2) 0.059(2) 0.0251(18) 0.0233(17) 0.0166(18) C28 0.057(2) 0.116(4) 0.081(3) 0.043(3) 0.025(2) 0.001(2) C29 0.070(2) 0.080(3) 0.081(3) 0.034(2) 0.011(2) -0.013(2) C30 0.070(2) 0.059(2) 0.061(2) 0.0178(16) 0.0112(17) 0.0003(16) C31 0.0483(16) 0.0574(17) 0.0460(16) 0.0152(13) 0.0074(13) 0.0055(13) C32 0.0342(12) 0.0346(12) 0.0420(14) 0.0093(10) 0.0113(10) 0.0025(9) C33 0.0432(14) 0.0424(14) 0.0533(17) 0.0075(12) 0.0199(13) 0.0037(11) C34 0.065(2) 0.0474(15) 0.0511(18) -0.0006(13) 0.0214(15) 0.0016(14) C35 0.064(2) 0.0495(17) 0.0482(18) 0.0030(13) 0.0035(15) -0.0034(14) C36 0.0380(14) 0.0552(17) 0.0515(17) 0.0072(13) 0.0052(12) 0.0020(12) C37 0.0364(13) 0.0468(15) 0.0432(15) 0.0069(11) 0.0110(11) 0.0067(11) P1 0.0442(4) 0.0584(5) 0.0570(5) -0.0093(4) 0.0083(4) -0.0039(3) F10 0.138(3) 0.0653(15) 0.111(2) 0.0141(14) 0.027(2) -0.0186(15) F11 0.0552(15) 0.110(2) 0.160(3) -0.0364(19) -0.0149(17) 0.0196(13) F12 0.0851(17) 0.126(2) 0.0801(17) 0.0158(15) 0.0325(14) -0.0243(15) F13 0.0605(14) 0.125(2) 0.109(2) -0.0692(18) 0.0104(14) 0.0000(13) F14 0.0975(18) 0.0732(14) 0.0594(13) -0.0137(10) -0.0030(12) -0.0084(12) F15 0.0472(11) 0.0801(14) 0.0957(17) -0.0187(12) 0.0161(11) 0.0014(10) P2 0.0372(4) 0.0469(4) 0.0748(6) -0.0042(4) 0.0158(4) 0.0004(3) F20 0.094(2) 0.157(3) 0.143(3) 0.080(2) 0.050(2) -0.008(2) F21 0.088(2) 0.0571(16) 0.424(8) -0.041(3) 0.085(3) 0.0101(14) F22 0.0596(14) 0.155(2) 0.0766(17) 0.0283(16) -0.0094(12) -0.0237(15) F23 0.0874(17) 0.0572(13) 0.140(3) -0.0031(14) 0.0452(17) 0.0090(11) F24 0.0519(14) 0.156(3) 0.138(3) -0.055(2) 0.0046(16) -0.0285(16) F25 0.0822(18) 0.151(2) 0.0652(15) -0.0287(16) 0.0308(13) -0.0339(17) _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 1.931(2) . ? Cu1 N4 2.015(2) . ? Cu1 N3 2.032(2) . ? Cu1 N1 2.055(2) . ? Cu1 N5 2.184(2) . ? N1 C1 1.338(4) . ? N1 C5 1.355(3) . ? N2 C6 1.339(4) . ? N2 C10 1.340(4) . ? N3 C15 1.340(4) . ? N3 C11 1.355(3) . ? C1 C2 1.380(4) . ? C1 H1A 0.9400 . ? C2 C3 1.376(5) . ? C2 H2A 0.9400 . ? C3 C4 1.382(5) . ? C3 H3A 0.9400 . ? C4 C5 1.381(4) . ? C4 H4A 0.9400 . ? C5 C6 1.479(4) . ? C6 C7 1.383(4) . ? C7 C8 1.381(5) . ? C7 H7A 0.9400 . ? C8 C9 1.378(5) . ? C8 H8A 0.9400 . ? C9 C10 1.384(4) . ? C9 H9A 0.9400 . ? C10 C11 1.473(4) . ? C11 C12 1.385(4) . ? C12 C13 1.378(5) . ? C12 H12A 0.9400 . ? C13 C14 1.374(5) . ? C13 H13A 0.9400 . ? C14 C15 1.380(4) . ? C14 H14A 0.9400 . ? C15 H15A 0.9400 . ? N4 C16 1.350(3) . ? N4 C20 1.355(3) . ? N5 C25 1.338(4) . ? N5 C21 1.348(4) . ? C16 C17 1.391(4) . ? C16 C32 1.479(4) . ? C17 C18 1.382(5) . ? C17 H17A 0.9400 . ? C18 C19 1.369(5) . ? C18 H18A 0.9400 . ? C19 C20 1.389(4) . ? C19 H19A 0.9400 . ? C20 C21 1.482(4) . ? C21 C22 1.382(4) . ? C22 C23 1.368(6) . ? C22 H22A 0.9400 . ? C23 C24 1.372(6) . ? C23 H23A 0.9400 . ? C24 C25 1.387(5) . ? C24 H24A 0.9400 . ? C25 C26 1.483(5) . ? C26 C31 1.387(4) . ? C26 C27 1.393(5) . ? C27 C28 1.378(6) . ? C27 H27A 0.9400 . ? C28 C29 1.367(6) . ? C28 H28A 0.9400 . ? C29 C30 1.386(6) . ? C29 H29A 0.9400 . ? C30 C31 1.383(5) . ? C30 H30A 0.9400 . ? C31 H31A 0.9400 . ? C32 C37 1.394(4) . ? C32 C33 1.396(4) . ? C33 C34 1.385(5) . ? C33 H33A 0.9400 . ? C34 C35 1.376(5) . ? C34 H34A 0.9400 . ? C35 C36 1.381(5) . ? C35 H35A 0.9400 . ? C36 C37 1.389(4) . ? C36 H36A 0.9400 . ? C37 H37A 0.9400 . ? P1 F10 1.573(3) . ? P1 F14 1.580(2) . ? P1 F11 1.581(3) . ? P1 F12 1.581(3) . ? P1 F13 1.593(2) . ? P1 F15 1.593(2) . ? P2 F21 1.550(3) . ? P2 F20 1.558(3) . ? P2 F23 1.567(2) . ? P2 F24 1.573(3) . ? P2 F22 1.579(3) . ? P2 F25 1.598(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 N2 Cu1 N4 163.43(9) . . ? N2 Cu1 N3 80.16(9) . . ? N4 Cu1 N3 97.57(9) . . ? N2 Cu1 N1 79.87(9) . . ? N4 Cu1 N1 100.41(8) . . ? N3 Cu1 N1 159.62(9) . . ? N2 Cu1 N5 116.92(9) . . ? N4 Cu1 N5 79.60(9) . . ? N3 Cu1 N5 104.07(9) . . ? N1 Cu1 N5 88.63(9) . . ? C1 N1 C5 119.0(2) . . ? C1 N1 Cu1 126.95(18) . . ? C5 N1 Cu1 113.65(17) . . ? C6 N2 C10 122.2(2) . . ? C6 N2 Cu1 118.97(18) . . ? C10 N2 Cu1 118.77(19) . . ? C15 N3 C11 118.8(2) . . ? C15 N3 Cu1 127.11(19) . . ? C11 N3 Cu1 113.57(18) . . ? N1 C1 C2 122.2(3) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C3 C2 C1 118.8(3) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C2 C3 C4 119.6(3) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 118.9(3) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? N1 C5 C4 121.5(3) . . ? N1 C5 C6 113.9(2) . . ? C4 C5 C6 124.5(3) . . ? N2 C6 C7 120.2(3) . . ? N2 C6 C5 113.4(2) . . ? C7 C6 C5 126.4(3) . . ? C8 C7 C6 118.3(3) . . ? C8 C7 H7A 120.8 . . ? C6 C7 H7A 120.8 . . ? C9 C8 C7 120.8(3) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C8 C9 C10 118.8(3) . . ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 120.6 . . ? N2 C10 C9 119.8(3) . . ? N2 C10 C11 112.7(2) . . ? C9 C10 C11 127.5(3) . . ? N3 C11 C12 121.3(3) . . ? N3 C11 C10 114.5(2) . . ? C12 C11 C10 124.3(3) . . ? C13 C12 C11 119.2(3) . . ? C13 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? C14 C13 C12 119.4(3) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? C13 C14 C15 119.1(3) . . ? C13 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? N3 C15 C14 122.2(3) . . ? N3 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? C16 N4 C20 119.6(2) . . ? C16 N4 Cu1 123.84(18) . . ? C20 N4 Cu1 115.54(18) . . ? C25 N5 C21 118.7(3) . . ? C25 N5 Cu1 126.7(2) . . ? C21 N5 Cu1 109.04(17) . . ? N4 C16 C17 120.7(3) . . ? N4 C16 C32 118.4(2) . . ? C17 C16 C32 120.9(3) . . ? C18 C17 C16 119.5(3) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C19 C18 C17 119.7(3) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? C18 C19 C20 119.1(3) . . ? C18 C19 H19A 120.4 . . ? C20 C19 H19A 120.4 . . ? N4 C20 C19 121.3(3) . . ? N4 C20 C21 115.6(2) . . ? C19 C20 C21 123.0(3) . . ? N5 C21 C22 122.3(3) . . ? N5 C21 C20 115.3(2) . . ? C22 C21 C20 122.4(3) . . ? C23 C22 C21 118.5(3) . . ? C23 C22 H22A 120.8 . . ? C21 C22 H22A 120.8 . . ? C22 C23 C24 119.8(3) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? C23 C24 C25 119.4(3) . . ? C23 C24 H24A 120.3 . . ? C25 C24 H24A 120.3 . . ? N5 C25 C24 121.3(3) . . ? N5 C25 C26 116.8(3) . . ? C24 C25 C26 121.9(3) . . ? C31 C26 C27 118.7(3) . . ? C31 C26 C25 119.6(3) . . ? C27 C26 C25 121.8(3) . . ? C28 C27 C26 120.0(4) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C29 C28 C27 120.9(4) . . ? C29 C28 H28A 119.5 . . ? C27 C28 H28A 119.5 . . ? C28 C29 C30 120.1(4) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 119.3(4) . . ? C31 C30 H30A 120.4 . . ? C29 C30 H30A 120.4 . . ? C30 C31 C26 121.1(3) . . ? C30 C31 H31A 119.5 . . ? C26 C31 H31A 119.5 . . ? C37 C32 C33 118.6(3) . . ? C37 C32 C16 121.5(2) . . ? C33 C32 C16 119.8(2) . . ? C34 C33 C32 120.4(3) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C35 C34 C33 120.4(3) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C36 119.9(3) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C37 120.1(3) . . ? C35 C36 H36A 119.9 . . ? C37 C36 H36A 119.9 . . ? C36 C37 C32 120.5(3) . . ? C36 C37 H37A 119.8 . . ? C32 C37 H37A 119.8 . . ? F10 P1 F14 91.06(16) . . ? F10 P1 F11 91.3(2) . . ? F14 P1 F11 90.85(16) . . ? F10 P1 F12 178.66(18) . . ? F14 P1 F12 89.22(15) . . ? F11 P1 F12 90.05(18) . . ? F10 P1 F13 89.64(18) . . ? F14 P1 F13 179.08(17) . . ? F11 P1 F13 89.72(16) . . ? F12 P1 F13 90.07(18) . . ? F10 P1 F15 89.56(16) . . ? F14 P1 F15 90.81(13) . . ? F11 P1 F15 178.13(17) . . ? F12 P1 F15 89.13(15) . . ? F13 P1 F15 88.61(14) . . ? F21 P2 F20 92.5(2) . . ? F21 P2 F23 176.9(3) . . ? F20 P2 F23 89.78(18) . . ? F21 P2 F24 89.0(2) . . ? F20 P2 F24 87.7(2) . . ? F23 P2 F24 88.97(18) . . ? F21 P2 F22 91.4(2) . . ? F20 P2 F22 92.44(19) . . ? F23 P2 F22 90.57(18) . . ? F24 P2 F22 179.5(2) . . ? F21 P2 F25 89.9(2) . . ? F20 P2 F25 177.62(19) . . ? F23 P2 F25 87.84(16) . . ? F24 P2 F25 92.34(18) . . ? F22 P2 F25 87.50(15) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.696 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.063 # Attachment '- jp108.cif' data_jp108 _database_code_depnum_ccdc_archive 'CCDC 770979' #TrackingRef '- jp108.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C54 H44 Cu2 N10 S2), C4 H10 O, 8(F6 P), 1.5(C2 H3 N), 3(H2 O)' _chemical_formula_sum 'C115 H108.5 Cu4 F48 N21.5 O4 P8 S4' _chemical_formula_weight 3397.98 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' 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 11.866(2) _cell_length_b 14.572(3) _cell_length_c 22.212(4) _cell_angle_alpha 86.03(3) _cell_angle_beta 76.02(3) _cell_angle_gamma 88.28(3) _cell_volume 3717.7(13) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5096 _cell_measurement_theta_min 5.45 _cell_measurement_theta_max 45.07 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1677 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6612 _exptl_absorpt_correction_T_max 0.9601 _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 87691 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.05 _reflns_number_total 13087 _reflns_number_gt 11985 _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^)+(0.0794P)^2^+10.1085P] 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 13087 _refine_ls_number_parameters 976 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1779 _refine_ls_wR_factor_gt 0.1722 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.037 _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 0.31729(4) 0.24620(3) 0.11980(2) 0.03440(15) Uani 1 1 d . . . N1 N 0.3944(3) 0.3294(2) 0.04388(17) 0.0355(8) Uani 1 1 d . . . N2 N 0.1898(3) 0.3319(2) 0.11479(16) 0.0317(7) Uani 1 1 d . . . N3 N 0.1977(3) 0.2053(3) 0.1993(2) 0.0498(10) Uani 1 1 d . . . C1 C 0.5032(4) 0.3205(3) 0.0084(2) 0.0444(11) Uani 1 1 d . . . H1A H 0.5543 0.2761 0.0212 0.053 Uiso 1 1 calc R . . C2 C 0.5430(4) 0.3741(4) -0.0462(2) 0.0484(12) Uani 1 1 d . . . H2A H 0.6198 0.3660 -0.0705 0.058 Uiso 1 1 calc R . . C3 C 0.4695(4) 0.4394(4) -0.0647(2) 0.0481(11) Uani 1 1 d . . . H3A H 0.4949 0.4763 -0.1023 0.058 Uiso 1 1 calc R . . C4 C 0.3577(4) 0.4506(3) -0.0276(2) 0.0393(10) Uani 1 1 d . . . H4A H 0.3063 0.4960 -0.0391 0.047 Uiso 1 1 calc R . . C5 C 0.3226(3) 0.3946(3) 0.02609(19) 0.0330(9) Uani 1 1 d . . . C6 C 0.2058(3) 0.3990(3) 0.06919(18) 0.0292(8) Uani 1 1 d . . . C7 C 0.1191(3) 0.4639(3) 0.06569(19) 0.0309(8) Uani 1 1 d . . . H7A H 0.1301 0.5111 0.0332 0.037 Uiso 1 1 calc R . . C8 C 0.0156(3) 0.4576(3) 0.11135(19) 0.0305(8) Uani 1 1 d . . . C9 C 0.0006(3) 0.3886(3) 0.1588(2) 0.0326(9) Uani 1 1 d . . . H9A H -0.0698 0.3838 0.1901 0.039 Uiso 1 1 calc R . . C10 C 0.0919(3) 0.3267(3) 0.1590(2) 0.0338(9) Uani 1 1 d . . . C11 C 0.0941(4) 0.2508(3) 0.2067(3) 0.0491(12) Uani 1 1 d . . . C12 C -0.0002(5) 0.2267(5) 0.2550(4) 0.085(2) Uani 1 1 d . . . H12A H -0.0722 0.2590 0.2594 0.102 Uiso 1 1 calc R . . C13 C 0.0126(7) 0.1544(6) 0.2969(5) 0.125(4) Uani 1 1 d U . . H13A H -0.0510 0.1361 0.3302 0.150 Uiso 1 1 calc R . . C14 C 0.1194(7) 0.1087(6) 0.2898(5) 0.124(4) Uani 1 1 d U . . H14A H 0.1303 0.0602 0.3188 0.148 Uiso 1 1 calc R . . C15 C 0.2086(6) 0.1350(5) 0.2401(4) 0.083(2) Uani 1 1 d . . . H15A H 0.2805 0.1023 0.2344 0.099 Uiso 1 1 calc R . . S1 S -0.09112(9) 0.54345(8) 0.10306(5) 0.0359(2) Uani 1 1 d . . . S2 S -0.23885(9) 0.50205(8) 0.16595(5) 0.0356(2) Uani 1 1 d . . . Cu2 Cu -0.28994(4) 0.73605(4) 0.40645(3) 0.04081(16) Uani 1 1 d . . . N4 N -0.1146(3) 0.7394(3) 0.3740(2) 0.0543(11) Uani 1 1 d . . . N5 N -0.2716(3) 0.6695(2) 0.33211(16) 0.0300(7) Uani 1 1 d . . . N6 N -0.4576(3) 0.7013(3) 0.41281(17) 0.0387(8) Uani 1 1 d . . . C16 C -0.0392(5) 0.7842(5) 0.3982(3) 0.076(2) Uani 1 1 d . . . H16A H -0.0665 0.8082 0.4379 0.091 Uiso 1 1 calc R . . C17 C 0.0760(5) 0.7965(5) 0.3675(3) 0.078(2) Uani 1 1 d . . . H17A H 0.1264 0.8290 0.3856 0.094 Uiso 1 1 calc R . . C18 C 0.1163(4) 0.7610(4) 0.3105(3) 0.0684(18) Uani 1 1 d . . . H18A H 0.1950 0.7690 0.2884 0.082 Uiso 1 1 calc R . . C19 C 0.0405(4) 0.7131(4) 0.2853(3) 0.0535(13) Uani 1 1 d . . . H19A H 0.0672 0.6869 0.2463 0.064 Uiso 1 1 calc R . . C20 C -0.0741(4) 0.7041(3) 0.3179(2) 0.0406(10) Uani 1 1 d . . . C21 C -0.1648(3) 0.6578(3) 0.29557(19) 0.0320(8) Uani 1 1 d . . . C22 C -0.1478(3) 0.6067(3) 0.2440(2) 0.0333(9) Uani 1 1 d . . . H22A H -0.0721 0.5972 0.2186 0.040 Uiso 1 1 calc R . . C23 C -0.2448(3) 0.5692(3) 0.23011(18) 0.0297(8) Uani 1 1 d . . . C24 C -0.3556(3) 0.5821(3) 0.26836(18) 0.0291(8) Uani 1 1 d . . . H24A H -0.4219 0.5568 0.2592 0.035 Uiso 1 1 calc R . . C25 C -0.3661(3) 0.6326(3) 0.31975(18) 0.0274(8) Uani 1 1 d . . . C26 C -0.4743(3) 0.6533(3) 0.36599(18) 0.0286(8) Uani 1 1 d . . . C27 C -0.5837(3) 0.6263(3) 0.3628(2) 0.0330(9) Uani 1 1 d . . . H27A H -0.5931 0.5923 0.3294 0.040 Uiso 1 1 calc R . . C28 C -0.6794(4) 0.6498(3) 0.4093(2) 0.0364(9) Uani 1 1 d . . . H28A H -0.7553 0.6332 0.4076 0.044 Uiso 1 1 calc R . . C29 C -0.6630(4) 0.6971(3) 0.4576(2) 0.0443(11) Uani 1 1 d . . . H29A H -0.7269 0.7129 0.4903 0.053 Uiso 1 1 calc R . . C30 C -0.5502(4) 0.7218(4) 0.4576(2) 0.0510(13) Uani 1 1 d . . . H30A H -0.5388 0.7546 0.4911 0.061 Uiso 1 1 calc R . . N7 N 0.3206(3) 0.1159(3) 0.0752(2) 0.0472(10) Uani 1 1 d . . . N8 N 0.4577(3) 0.1837(2) 0.14120(17) 0.0363(8) Uani 1 1 d . . . C31 C 0.1576(6) 0.1548(5) 0.0283(4) 0.091(3) Uani 1 1 d . . . H31A H 0.1024 0.1691 0.0671 0.136 Uiso 1 1 calc R . . H31B H 0.1161 0.1281 0.0007 0.136 Uiso 1 1 calc R . . H31C H 0.1959 0.2113 0.0080 0.136 Uiso 1 1 calc R . . C32 C 0.2468(5) 0.0874(4) 0.0422(3) 0.0625(15) Uani 1 1 d . . . C33 C 0.2524(6) -0.0032(5) 0.0239(4) 0.087(2) Uani 1 1 d . . . H33A H 0.2021 -0.0227 0.0000 0.105 Uiso 1 1 calc R . . C34 C 0.3311(10) -0.0623(6) 0.0411(6) 0.134(4) Uani 1 1 d . . . H34A H 0.3337 -0.1245 0.0305 0.160 Uiso 1 1 calc R . . C35 C 0.4081(8) -0.0334(5) 0.0741(5) 0.109(3) Uani 1 1 d . . . H35A H 0.4640 -0.0748 0.0854 0.131 Uiso 1 1 calc R . . C36 C 0.4011(5) 0.0577(3) 0.0901(3) 0.0537(13) Uani 1 1 d . . . C37 C 0.4811(4) 0.0951(3) 0.1245(2) 0.0433(10) Uani 1 1 d . . . C38 C 0.5728(5) 0.0453(4) 0.1394(3) 0.0545(13) Uani 1 1 d . . . H38A H 0.5887 -0.0157 0.1268 0.065 Uiso 1 1 calc R . . C39 C 0.6401(5) 0.0844(4) 0.1722(3) 0.0595(14) Uani 1 1 d . . . H39A H 0.7021 0.0501 0.1835 0.071 Uiso 1 1 calc R . . C40 C 0.6183(4) 0.1730(4) 0.1888(2) 0.0519(12) Uani 1 1 d . . . H40A H 0.6655 0.2010 0.2111 0.062 Uiso 1 1 calc R . . C41 C 0.5255(4) 0.2219(3) 0.1725(2) 0.0394(10) Uani 1 1 d . . . C42 C 0.5010(5) 0.3207(4) 0.1873(3) 0.0571(13) Uani 1 1 d . . . H42A H 0.5402 0.3609 0.1517 0.086 Uiso 1 1 calc R . . H42B H 0.5298 0.3329 0.2237 0.086 Uiso 1 1 calc R . . H42C H 0.4171 0.3327 0.1961 0.086 Uiso 1 1 calc R . . N9 N -0.3043(3) 0.8790(3) 0.4208(2) 0.0471(10) Uani 1 1 d . . . N10 N -0.3022(3) 0.7332(3) 0.49914(17) 0.0391(8) Uani 1 1 d . . . C43 C -0.2651(8) 0.9226(7) 0.3099(4) 0.113(3) Uani 1 1 d U . . H43A H -0.2760 0.9760 0.2825 0.169 Uiso 1 1 calc R . . H43B H -0.3152 0.8727 0.3052 0.169 Uiso 1 1 calc R . . H43C H -0.1837 0.9020 0.2988 0.169 Uiso 1 1 calc R . . C44 C -0.2954(5) 0.9481(4) 0.3745(4) 0.082(2) Uani 1 1 d . . . C45 C -0.3098(8) 1.0369(6) 0.3870(7) 0.120(4) Uani 1 1 d . . . H45A H -0.2998 1.0839 0.3544 0.144 Uiso 1 1 calc R . . C46 C -0.3386(9) 1.0575(5) 0.4462(7) 0.121(4) Uani 1 1 d U . . H46A H -0.3576 1.1196 0.4552 0.146 Uiso 1 1 calc R . . C47 C -0.3424(8) 0.9889(7) 0.4986(6) 0.126(4) Uani 1 1 d . . . H47A H -0.3557 1.0047 0.5406 0.151 Uiso 1 1 calc R . . C48 C -0.3244(4) 0.8965(4) 0.4805(3) 0.0601(16) Uani 1 1 d . . . C49 C -0.3217(4) 0.8149(5) 0.5249(2) 0.0572(15) Uani 1 1 d . . . C50 C -0.3366(7) 0.8205(9) 0.5885(4) 0.114(4) Uani 1 1 d . . . H50A H -0.3515 0.8784 0.6062 0.137 Uiso 1 1 calc R . . C51 C -0.3298(9) 0.7433(12) 0.6251(4) 0.132(5) Uani 1 1 d U . . H51A H -0.3382 0.7472 0.6684 0.159 Uiso 1 1 calc R . . C52 C -0.3114(7) 0.6612(9) 0.6003(4) 0.113(4) Uani 1 1 d . . . H52A H -0.3078 0.6069 0.6261 0.136 Uiso 1 1 calc R . . C53 C -0.2971(5) 0.6556(5) 0.5351(3) 0.0708(19) Uani 1 1 d . . . C54 C -0.2766(8) 0.5684(5) 0.5027(5) 0.109(3) Uani 1 1 d U . . H54A H -0.3491 0.5494 0.4937 0.163 Uiso 1 1 calc R . . H54B H -0.2500 0.5203 0.5293 0.163 Uiso 1 1 calc R . . H54C H -0.2173 0.5780 0.4636 0.163 Uiso 1 1 calc R . . P1 P 0.84116(11) 0.26940(8) 0.02979(6) 0.0418(3) Uani 1 1 d . . . F10 F 0.7720(4) 0.3533(3) 0.0652(2) 0.0896(13) Uani 1 1 d . . . F11 F 0.8093(4) 0.3103(3) -0.03251(18) 0.0840(11) Uani 1 1 d . . . F12 F 0.8713(3) 0.2306(3) 0.09264(16) 0.0698(9) Uani 1 1 d . . . F13 F 0.9575(3) 0.3271(3) 0.01318(18) 0.0800(11) Uani 1 1 d . . . F14 F 0.9074(3) 0.1851(3) -0.0050(2) 0.0795(11) Uani 1 1 d . . . F15 F 0.7237(3) 0.2124(2) 0.04601(16) 0.0617(8) Uani 1 1 d . . . P2 P 0.68938(12) 0.33419(9) 0.35117(6) 0.0462(3) Uani 1 1 d . . . F20 F 0.6751(5) 0.4172(3) 0.3935(2) 0.1042(15) Uani 1 1 d . . . F21 F 0.5906(3) 0.2779(3) 0.39812(19) 0.0903(13) Uani 1 1 d . . . F22 F 0.7131(4) 0.2490(3) 0.30746(19) 0.0857(11) Uani 1 1 d . . . F23 F 0.5978(3) 0.3807(3) 0.31617(18) 0.0780(11) Uani 1 1 d . . . F24 F 0.7819(3) 0.2874(3) 0.38595(17) 0.0704(9) Uani 1 1 d . . . F25 F 0.7931(3) 0.3869(3) 0.30297(18) 0.0775(10) Uani 1 1 d . . . P3 P 0.39361(12) 0.92879(9) 0.30876(7) 0.0495(3) Uani 1 1 d . . . F30 F 0.3604(4) 0.8243(2) 0.3202(2) 0.0844(12) Uani 1 1 d . . . F31 F 0.4240(4) 1.0351(3) 0.2982(2) 0.1010(15) Uani 1 1 d . . . F32 F 0.4565(3) 0.9195(4) 0.36492(18) 0.0929(13) Uani 1 1 d . . . F33 F 0.5116(3) 0.9040(3) 0.26146(19) 0.0826(11) Uani 1 1 d . . . F34 F 0.3289(4) 0.9385(3) 0.25322(19) 0.0818(11) Uani 1 1 d . . . F35 F 0.2744(3) 0.9561(3) 0.35648(19) 0.0815(11) Uani 1 1 d . . . P4 P 0.26108(10) 0.51633(9) 0.23235(6) 0.0401(3) Uani 1 1 d . . . F40 F 0.2792(3) 0.6217(2) 0.20870(18) 0.0708(9) Uani 1 1 d . . . F41 F 0.2417(3) 0.4104(2) 0.25605(16) 0.0648(8) Uani 1 1 d . . . F42 F 0.3940(2) 0.5085(2) 0.23733(16) 0.0638(9) Uani 1 1 d . . . F43 F 0.1286(2) 0.5238(2) 0.22716(17) 0.0631(9) Uani 1 1 d . . . F44 F 0.2228(3) 0.5460(3) 0.30211(14) 0.0633(9) Uani 1 1 d . . . F45 F 0.3009(3) 0.4861(2) 0.16238(13) 0.0563(8) Uani 1 1 d . . . N100 N 0.0353(11) 0.6235(12) 0.4984(8) 0.171(6) Uani 0.75 1 d PU A 1 C100 C 0.0212(9) 0.5992(11) 0.5533(8) 0.127(6) Uani 0.75 1 d P A 1 C101 C 0.0068(8) 0.5563(8) 0.6128(5) 0.091(3) Uani 0.75 1 d P A 1 H10A H -0.0222 0.4939 0.6132 0.136 Uiso 0.75 1 calc PR A 1 H10B H -0.0492 0.5917 0.6427 0.136 Uiso 0.75 1 calc PR A 1 H10C H 0.0815 0.5531 0.6243 0.136 Uiso 0.75 1 calc PR A 1 O300 O 0.7997(15) -0.1192(9) 0.1365(6) 0.149(6) Uani 0.50 1 d PDU B 1 C301 C 0.911(2) -0.1009(16) 0.1429(10) 0.136(8) Uani 0.50 1 d PDU B 1 H30B H 0.9650 -0.1327 0.1093 0.163 Uiso 0.50 1 calc PR B 1 H30C H 0.9173 -0.1344 0.1823 0.163 Uiso 0.50 1 calc PR B 1 C302 C 0.9631(19) -0.009(2) 0.1433(13) 0.173(10) Uani 0.50 1 d PU B 1 H30D H 0.9813 0.0199 0.1011 0.259 Uiso 0.50 1 calc PR B 1 H30E H 1.0344 -0.0173 0.1581 0.259 Uiso 0.50 1 calc PR B 1 H30F H 0.9078 0.0293 0.1711 0.259 Uiso 0.50 1 calc PR B 1 C303 C 0.7270(18) -0.2079(8) 0.1446(8) 0.093(6) Uani 0.50 1 d PD B 1 H30G H 0.7794 -0.2533 0.1202 0.112 Uiso 0.50 1 calc PR B 1 H30H H 0.7175 -0.2296 0.1887 0.112 Uiso 0.50 1 calc PR B 1 C304 C 0.623(2) -0.2207(11) 0.1328(11) 0.127(7) Uani 0.50 1 d PU B 1 H30I H 0.5633 -0.1881 0.1623 0.191 Uiso 0.50 1 calc PR B 1 H30J H 0.6065 -0.2866 0.1372 0.191 Uiso 0.50 1 calc PR B 1 H30K H 0.6246 -0.1968 0.0903 0.191 Uiso 0.50 1 calc PR B 1 O400 O 0.503(3) -0.2545(19) 0.1792(15) 0.129(10) Uani 0.25 1 d P C 2 O100 O 0.0000 1.0000 0.5000 0.135(10) Uani 0.50 2 d SP D 1 O101 O 0.000(3) 0.9224(12) 0.5147(12) 0.198(12) Uani 0.50 1 d P E 2 O401 O 0.839(3) -0.190(2) 0.1407(14) 0.124(9) Uiso 0.25 1 d P F 2 O500 O -0.023(4) 0.451(3) 0.572(2) 0.212(18) Uiso 0.25 1 d P G 3 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 0.0274(3) 0.0327(3) 0.0415(3) -0.0052(2) -0.0047(2) 0.00404(19) N1 0.0282(17) 0.0396(19) 0.0378(19) -0.0068(15) -0.0053(15) 0.0024(14) N2 0.0271(17) 0.0307(17) 0.0371(19) -0.0103(14) -0.0051(14) 0.0014(13) N3 0.037(2) 0.042(2) 0.061(3) 0.0109(19) 0.0015(19) 0.0076(17) C1 0.028(2) 0.054(3) 0.049(3) -0.006(2) -0.0047(19) 0.0070(19) C2 0.029(2) 0.066(3) 0.044(3) -0.001(2) 0.0015(19) 0.005(2) C3 0.039(2) 0.063(3) 0.038(3) 0.001(2) -0.001(2) -0.001(2) C4 0.033(2) 0.050(3) 0.035(2) -0.0026(19) -0.0081(18) 0.0026(19) C5 0.029(2) 0.041(2) 0.031(2) -0.0095(17) -0.0087(16) 0.0012(17) C6 0.0255(19) 0.032(2) 0.032(2) -0.0092(16) -0.0083(16) 0.0002(15) C7 0.031(2) 0.034(2) 0.029(2) -0.0095(16) -0.0080(16) 0.0003(16) C8 0.0273(19) 0.034(2) 0.033(2) -0.0159(16) -0.0102(16) 0.0035(15) C9 0.028(2) 0.033(2) 0.035(2) -0.0094(17) -0.0037(16) -0.0022(16) C10 0.027(2) 0.032(2) 0.041(2) -0.0078(17) -0.0049(17) -0.0014(16) C11 0.034(2) 0.045(3) 0.058(3) 0.008(2) 0.005(2) 0.0066(19) C12 0.050(3) 0.076(4) 0.100(5) 0.041(4) 0.022(3) 0.021(3) C13 0.071(5) 0.122(7) 0.134(7) 0.081(6) 0.039(5) 0.030(4) C14 0.075(5) 0.113(6) 0.135(7) 0.083(6) 0.038(5) 0.038(4) C15 0.054(3) 0.069(4) 0.102(5) 0.037(4) 0.010(3) 0.020(3) S1 0.0314(5) 0.0434(6) 0.0318(5) -0.0089(4) -0.0053(4) 0.0105(4) S2 0.0274(5) 0.0459(6) 0.0353(5) -0.0186(4) -0.0071(4) 0.0038(4) Cu2 0.0292(3) 0.0591(4) 0.0359(3) -0.0233(3) -0.0049(2) -0.0078(2) N4 0.032(2) 0.080(3) 0.055(3) -0.033(2) -0.0109(18) -0.008(2) N5 0.0261(16) 0.0308(17) 0.0338(18) -0.0096(14) -0.0063(14) -0.0006(13) N6 0.0310(18) 0.053(2) 0.0319(19) -0.0175(16) -0.0015(15) -0.0081(16) C16 0.042(3) 0.118(6) 0.074(4) -0.052(4) -0.011(3) -0.017(3) C17 0.039(3) 0.111(5) 0.092(5) -0.053(4) -0.016(3) -0.014(3) C18 0.027(2) 0.083(4) 0.095(5) -0.041(4) -0.003(3) -0.009(2) C19 0.030(2) 0.064(3) 0.067(3) -0.032(3) -0.006(2) -0.003(2) C20 0.028(2) 0.050(3) 0.046(3) -0.018(2) -0.0093(18) -0.0007(18) C21 0.0263(19) 0.034(2) 0.036(2) -0.0097(17) -0.0053(16) 0.0021(16) C22 0.0255(19) 0.038(2) 0.037(2) -0.0112(17) -0.0058(16) 0.0035(16) C23 0.0296(19) 0.0305(19) 0.029(2) -0.0089(16) -0.0060(16) 0.0040(15) C24 0.0277(19) 0.0282(19) 0.033(2) -0.0081(15) -0.0086(16) -0.0009(15) C25 0.0255(18) 0.0267(18) 0.029(2) -0.0034(15) -0.0048(15) -0.0009(14) C26 0.0286(19) 0.0286(19) 0.0281(19) -0.0040(15) -0.0051(15) -0.0029(15) C27 0.029(2) 0.033(2) 0.036(2) -0.0062(17) -0.0050(17) -0.0033(16) C28 0.028(2) 0.039(2) 0.040(2) -0.0024(18) -0.0016(17) -0.0066(16) C29 0.033(2) 0.056(3) 0.039(2) -0.014(2) 0.0045(19) -0.005(2) C30 0.038(2) 0.072(3) 0.041(3) -0.028(2) 0.003(2) -0.010(2) N7 0.039(2) 0.043(2) 0.062(3) -0.0199(19) -0.0139(19) 0.0018(17) N8 0.0291(17) 0.0389(19) 0.040(2) -0.0040(15) -0.0054(15) 0.0023(14) C31 0.072(4) 0.094(5) 0.131(7) -0.051(5) -0.062(5) 0.018(4) C32 0.047(3) 0.063(3) 0.083(4) -0.028(3) -0.020(3) -0.001(2) C33 0.075(4) 0.076(4) 0.124(6) -0.055(4) -0.035(4) 0.000(4) C34 0.152(9) 0.060(5) 0.225(13) -0.075(6) -0.100(9) 0.021(5) C35 0.122(7) 0.050(4) 0.189(10) -0.050(5) -0.093(7) 0.028(4) C36 0.053(3) 0.038(2) 0.074(4) -0.017(2) -0.020(3) 0.005(2) C37 0.041(2) 0.034(2) 0.053(3) -0.005(2) -0.009(2) 0.0055(18) C38 0.054(3) 0.042(3) 0.067(3) -0.002(2) -0.015(3) 0.015(2) C39 0.047(3) 0.071(4) 0.060(3) 0.011(3) -0.017(3) 0.018(3) C40 0.044(3) 0.068(3) 0.046(3) 0.002(2) -0.017(2) 0.003(2) C41 0.035(2) 0.048(3) 0.035(2) -0.0055(19) -0.0079(18) 0.0014(19) C42 0.060(3) 0.055(3) 0.064(3) -0.021(3) -0.025(3) 0.004(2) N9 0.040(2) 0.0327(19) 0.074(3) 0.0042(19) -0.026(2) -0.0073(16) N10 0.0343(19) 0.050(2) 0.0342(19) 0.0014(16) -0.0113(15) -0.0083(16) C43 0.106(6) 0.133(7) 0.100(6) 0.072(6) -0.047(5) -0.029(5) C44 0.054(3) 0.050(3) 0.152(8) 0.033(4) -0.050(4) -0.019(3) C45 0.086(6) 0.050(4) 0.224(14) 0.021(6) -0.046(7) -0.004(4) C46 0.114(7) 0.035(4) 0.212(11) -0.021(6) -0.034(7) 0.023(4) C47 0.090(6) 0.097(7) 0.209(12) -0.102(8) -0.048(7) 0.016(5) C48 0.040(3) 0.045(3) 0.101(5) -0.039(3) -0.019(3) 0.003(2) C49 0.034(2) 0.096(4) 0.045(3) -0.037(3) -0.004(2) -0.012(3) C50 0.073(5) 0.210(11) 0.063(5) -0.070(6) -0.002(4) -0.038(6) C51 0.104(7) 0.249(13) 0.044(4) 0.000(7) -0.011(4) -0.069(8) C52 0.068(5) 0.192(10) 0.082(6) 0.081(7) -0.040(4) -0.057(6) C53 0.051(3) 0.095(5) 0.068(4) 0.039(3) -0.027(3) -0.024(3) C54 0.113(6) 0.053(4) 0.160(8) 0.041(5) -0.047(6) -0.004(4) P1 0.0415(6) 0.0375(6) 0.0484(7) -0.0105(5) -0.0126(5) 0.0000(5) F10 0.104(3) 0.060(2) 0.110(3) -0.042(2) -0.030(3) 0.030(2) F11 0.096(3) 0.098(3) 0.066(2) 0.013(2) -0.039(2) -0.016(2) F12 0.062(2) 0.088(2) 0.065(2) 0.0112(18) -0.0282(17) -0.0106(17) F13 0.079(2) 0.087(3) 0.076(2) -0.0010(19) -0.0179(19) -0.044(2) F14 0.0549(19) 0.078(2) 0.110(3) -0.053(2) -0.0162(19) 0.0153(17) F15 0.0434(16) 0.068(2) 0.075(2) -0.0049(16) -0.0168(15) -0.0077(14) P2 0.0516(7) 0.0500(7) 0.0357(6) 0.0038(5) -0.0091(5) -0.0066(6) F20 0.134(4) 0.092(3) 0.103(3) -0.052(3) -0.052(3) 0.037(3) F21 0.057(2) 0.116(3) 0.081(3) 0.042(2) 0.0022(19) -0.008(2) F22 0.111(3) 0.074(2) 0.075(3) -0.0203(19) -0.022(2) -0.008(2) F23 0.071(2) 0.089(3) 0.081(3) 0.029(2) -0.039(2) -0.0174(19) F24 0.064(2) 0.079(2) 0.068(2) 0.0138(18) -0.0224(17) 0.0026(17) F25 0.071(2) 0.076(2) 0.074(2) 0.0257(19) -0.0023(18) -0.0114(18) P3 0.0484(7) 0.0483(7) 0.0525(8) -0.0028(6) -0.0129(6) -0.0067(6) F30 0.087(3) 0.0478(19) 0.126(3) 0.019(2) -0.046(2) -0.0125(17) F31 0.131(4) 0.061(2) 0.099(3) -0.022(2) 0.005(3) -0.035(2) F32 0.063(2) 0.158(4) 0.064(2) -0.007(2) -0.0247(19) -0.015(2) F33 0.068(2) 0.098(3) 0.077(3) -0.025(2) -0.0040(19) 0.002(2) F34 0.111(3) 0.068(2) 0.081(3) -0.0083(19) -0.054(2) 0.016(2) F35 0.056(2) 0.096(3) 0.085(3) -0.009(2) -0.0008(18) 0.0029(19) P4 0.0318(6) 0.0516(7) 0.0394(6) -0.0183(5) -0.0089(5) -0.0047(5) F40 0.070(2) 0.0505(18) 0.087(3) -0.0146(17) -0.0048(18) -0.0074(15) F41 0.066(2) 0.0545(18) 0.069(2) -0.0061(15) -0.0066(16) -0.0056(15) F42 0.0349(15) 0.088(2) 0.077(2) -0.0442(18) -0.0193(14) 0.0031(14) F43 0.0383(15) 0.077(2) 0.084(2) -0.0351(18) -0.0252(15) 0.0024(14) F44 0.0517(17) 0.094(2) 0.0466(17) -0.0343(16) -0.0077(14) -0.0031(16) F45 0.0582(18) 0.074(2) 0.0392(15) -0.0232(14) -0.0105(13) -0.0044(15) N100 0.090(7) 0.208(13) 0.192(12) 0.084(11) -0.015(8) 0.001(8) C100 0.050(6) 0.171(13) 0.145(12) 0.072(11) -0.017(7) -0.028(7) C101 0.059(5) 0.125(9) 0.082(7) 0.010(6) -0.006(5) -0.034(5) O300 0.208(14) 0.107(9) 0.094(8) 0.016(7) 0.018(9) 0.097(10) C301 0.187(17) 0.128(14) 0.073(10) -0.013(10) 0.000(12) 0.046(14) C302 0.088(11) 0.189(17) 0.189(17) 0.045(14) 0.051(12) 0.018(12) C303 0.146(16) 0.022(5) 0.091(11) -0.004(6) 0.009(10) 0.005(7) C304 0.181(16) 0.039(7) 0.148(15) -0.025(8) -0.011(13) 0.021(10) O400 0.18(3) 0.092(17) 0.13(2) -0.029(16) -0.06(2) 0.006(18) O100 0.100(13) 0.27(3) 0.047(9) -0.025(17) -0.033(9) 0.02(2) O101 0.27(3) 0.124(14) 0.19(2) -0.087(16) -0.015(19) -0.026(17) _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 1.952(3) . ? Cu1 N8 2.016(4) . ? Cu1 N3 2.045(4) . ? Cu1 N1 2.047(4) . ? Cu1 N7 2.196(4) . ? N1 C1 1.348(6) . ? N1 C5 1.359(5) . ? N2 C10 1.327(5) . ? N2 C6 1.341(5) . ? N3 C15 1.345(7) . ? N3 C11 1.359(6) . ? C1 C2 1.384(7) . ? C1 H1A 0.9500 . ? C2 C3 1.379(7) . ? C2 H2A 0.9500 . ? C3 C4 1.394(6) . ? C3 H3A 0.9500 . ? C4 C5 1.381(6) . ? C4 H4A 0.9500 . ? C5 C6 1.485(5) . ? C6 C7 1.389(6) . ? C7 C8 1.392(6) . ? C7 H7A 0.9500 . ? C8 C9 1.388(6) . ? C8 S1 1.786(4) . ? C9 C10 1.389(6) . ? C9 H9A 0.9500 . ? C10 C11 1.482(7) . ? C11 C12 1.385(7) . ? C12 C13 1.386(9) . ? C12 H12A 0.9500 . ? C13 C14 1.393(10) . ? C13 H13A 0.9500 . ? C14 C15 1.373(9) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? S1 S2 2.0375(17) . ? S2 C23 1.771(4) . ? Cu2 N5 1.936(3) . ? Cu2 N10 2.026(4) . ? Cu2 N4 2.031(4) . ? Cu2 N6 2.037(4) . ? Cu2 N9 2.124(4) . ? N4 C20 1.354(6) . ? N4 C16 1.354(6) . ? N5 C21 1.342(5) . ? N5 C25 1.352(5) . ? N6 C30 1.334(6) . ? N6 C26 1.349(5) . ? C16 C17 1.383(8) . ? C16 H16A 0.9500 . ? C17 C18 1.372(9) . ? C17 H17A 0.9500 . ? C18 C19 1.395(7) . ? C18 H18A 0.9500 . ? C19 C20 1.382(7) . ? C19 H19A 0.9500 . ? C20 C21 1.486(6) . ? C21 C22 1.380(6) . ? C22 C23 1.396(6) . ? C22 H22A 0.9500 . ? C23 C24 1.397(5) . ? C24 C25 1.379(5) . ? C24 H24A 0.9500 . ? C25 C26 1.476(5) . ? C26 C27 1.387(6) . ? C27 C28 1.390(6) . ? C27 H27A 0.9500 . ? C28 C29 1.371(6) . ? C28 H28A 0.9500 . ? C29 C30 1.397(7) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? N7 C36 1.343(7) . ? N7 C32 1.361(7) . ? N8 C41 1.338(6) . ? N8 C37 1.370(6) . ? C31 C32 1.494(9) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.403(8) . ? C33 C34 1.356(12) . ? C33 H33A 0.9500 . ? C34 C35 1.392(11) . ? C34 H34A 0.9500 . ? C35 C36 1.394(8) . ? C35 H35A 0.9500 . ? C36 C37 1.491(7) . ? C37 C38 1.382(7) . ? C38 C39 1.365(8) . ? C38 H38A 0.9500 . ? C39 C40 1.367(8) . ? C39 H39A 0.9500 . ? C40 C41 1.401(7) . ? C40 H40A 0.9500 . ? C41 C42 1.502(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? N9 C48 1.330(8) . ? N9 C44 1.376(8) . ? N10 C49 1.346(7) . ? N10 C53 1.348(7) . ? C43 C44 1.465(13) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.340(12) . ? C45 C46 1.330(16) . ? C45 H45A 0.9500 . ? C46 C47 1.473(17) . ? C46 H46A 0.9500 . ? C47 C48 1.428(9) . ? C47 H47A 0.9500 . ? C48 C49 1.495(9) . ? C49 C50 1.388(9) . ? C50 C51 1.354(17) . ? C50 H50A 0.9500 . ? C51 C52 1.342(16) . ? C51 H51A 0.9500 . ? C52 C53 1.424(12) . ? C52 H52A 0.9500 . ? C53 C54 1.489(12) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? P1 F14 1.583(3) . ? P1 F12 1.586(4) . ? P1 F13 1.591(3) . ? P1 F11 1.593(4) . ? P1 F10 1.596(3) . ? P1 F15 1.597(3) . ? P2 F20 1.563(4) . ? P2 F21 1.575(4) . ? P2 F23 1.592(4) . ? P2 F25 1.599(4) . ? P2 F24 1.600(4) . ? P2 F22 1.606(4) . ? P3 F30 1.573(4) . ? P3 F33 1.583(4) . ? P3 F31 1.590(4) . ? P3 F32 1.597(4) . ? P3 F34 1.600(4) . ? P3 F35 1.607(4) . ? P4 F44 1.592(3) . ? P4 F40 1.592(4) . ? P4 F45 1.600(3) . ? P4 F41 1.601(3) . ? P4 F43 1.604(3) . ? P4 F42 1.608(3) . ? N100 C100 1.218(19) . ? C100 C101 1.397(16) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? O300 C301 1.398(17) . ? O300 C303 1.552(16) . ? C301 C302 1.49(3) . ? C301 H30B 0.9900 . ? C301 H30C 0.9900 . ? C302 H30D 0.9800 . ? C302 H30E 0.9800 . ? C302 H30F 0.9800 . ? C303 C304 1.34(3) . ? C303 H30G 0.9900 . ? C303 H30H 0.9900 . ? C304 H30I 0.9800 . ? C304 H30J 0.9800 . ? C304 H30K 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 N8 163.77(14) . . ? N2 Cu1 N3 79.46(15) . . ? N8 Cu1 N3 97.76(16) . . ? N2 Cu1 N1 79.43(14) . . ? N8 Cu1 N1 100.78(14) . . ? N3 Cu1 N1 158.01(15) . . ? N2 Cu1 N7 116.96(15) . . ? N8 Cu1 N7 79.15(15) . . ? N3 Cu1 N7 95.49(17) . . ? N1 Cu1 N7 99.51(16) . . ? C1 N1 C5 118.7(4) . . ? C1 N1 Cu1 126.7(3) . . ? C5 N1 Cu1 114.4(3) . . ? C10 N2 C6 121.2(3) . . ? C10 N2 Cu1 119.4(3) . . ? C6 N2 Cu1 119.2(3) . . ? C15 N3 C11 118.9(4) . . ? C15 N3 Cu1 126.9(4) . . ? C11 N3 Cu1 113.9(3) . . ? N1 C1 C2 122.1(4) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C3 C2 C1 119.2(4) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 119.2(5) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 119.0(4) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? N1 C5 C4 121.8(4) . . ? N1 C5 C6 114.0(4) . . ? C4 C5 C6 124.2(4) . . ? N2 C6 C7 121.0(4) . . ? N2 C6 C5 112.6(3) . . ? C7 C6 C5 126.4(4) . . ? C6 C7 C8 117.8(4) . . ? C6 C7 H7A 121.1 . . ? C8 C7 H7A 121.1 . . ? C9 C8 C7 120.6(4) . . ? C9 C8 S1 124.6(3) . . ? C7 C8 S1 114.8(3) . . ? C8 C9 C10 117.8(4) . . ? C8 C9 H9A 121.1 . . ? C10 C9 H9A 121.1 . . ? N2 C10 C9 121.5(4) . . ? N2 C10 C11 112.8(4) . . ? C9 C10 C11 125.7(4) . . ? N3 C11 C12 121.8(5) . . ? N3 C11 C10 114.2(4) . . ? C12 C11 C10 124.0(4) . . ? C11 C12 C13 118.6(6) . . ? C11 C12 H12A 120.7 . . ? C13 C12 H12A 120.7 . . ? C12 C13 C14 119.6(6) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.2 . . ? C15 C14 C13 118.8(6) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? N3 C15 C14 122.3(6) . . ? N3 C15 H15A 118.8 . . ? C14 C15 H15A 118.8 . . ? C8 S1 S2 105.02(15) . . ? C23 S2 S1 104.13(15) . . ? N5 Cu2 N10 148.77(15) . . ? N5 Cu2 N4 79.58(15) . . ? N10 Cu2 N4 100.09(16) . . ? N5 Cu2 N6 79.37(14) . . ? N10 Cu2 N6 96.43(15) . . ? N4 Cu2 N6 158.76(15) . . ? N5 Cu2 N9 131.77(16) . . ? N10 Cu2 N9 79.44(17) . . ? N4 Cu2 N9 93.55(17) . . ? N6 Cu2 N9 102.56(15) . . ? C20 N4 C16 118.0(4) . . ? C20 N4 Cu2 114.8(3) . . ? C16 N4 Cu2 126.4(4) . . ? C21 N5 C25 121.6(3) . . ? C21 N5 Cu2 119.2(3) . . ? C25 N5 Cu2 119.1(3) . . ? C30 N6 C26 118.1(4) . . ? C30 N6 Cu2 126.7(3) . . ? C26 N6 Cu2 115.2(3) . . ? N4 C16 C17 122.7(5) . . ? N4 C16 H16A 118.7 . . ? C17 C16 H16A 118.7 . . ? C18 C17 C16 118.9(5) . . ? C18 C17 H17A 120.5 . . ? C16 C17 H17A 120.5 . . ? C17 C18 C19 119.2(5) . . ? C17 C18 H18A 120.4 . . ? C19 C18 H18A 120.4 . . ? C20 C19 C18 119.1(5) . . ? C20 C19 H19A 120.4 . . ? C18 C19 H19A 120.4 . . ? N4 C20 C19 122.0(4) . . ? N4 C20 C21 113.3(4) . . ? C19 C20 C21 124.7(4) . . ? N5 C21 C22 120.8(4) . . ? N5 C21 C20 112.5(3) . . ? C22 C21 C20 126.7(4) . . ? C21 C22 C23 118.3(4) . . ? C21 C22 H22A 120.9 . . ? C23 C22 H22A 120.9 . . ? C22 C23 C24 120.4(4) . . ? C22 C23 S2 124.3(3) . . ? C24 C23 S2 115.3(3) . . ? C25 C24 C23 118.2(4) . . ? C25 C24 H24A 120.9 . . ? C23 C24 H24A 120.9 . . ? N5 C25 C24 120.6(3) . . ? N5 C25 C26 112.7(3) . . ? C24 C25 C26 126.6(3) . . ? N6 C26 C27 122.2(4) . . ? N6 C26 C25 113.6(3) . . ? C27 C26 C25 124.2(4) . . ? C26 C27 C28 118.9(4) . . ? C26 C27 H27A 120.5 . . ? C28 C27 H27A 120.5 . . ? C29 C28 C27 119.2(4) . . ? C29 C28 H28A 120.4 . . ? C27 C28 H28A 120.4 . . ? C28 C29 C30 118.5(4) . . ? C28 C29 H29A 120.7 . . ? C30 C29 H29A 120.7 . . ? N6 C30 C29 123.0(4) . . ? N6 C30 H30A 118.5 . . ? C29 C30 H30A 118.5 . . ? C36 N7 C32 120.3(4) . . ? C36 N7 Cu1 110.9(3) . . ? C32 N7 Cu1 128.4(4) . . ? C41 N8 C37 118.8(4) . . ? C41 N8 Cu1 124.2(3) . . ? C37 N8 Cu1 117.0(3) . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N7 C32 C33 120.7(6) . . ? N7 C32 C31 117.7(5) . . ? C33 C32 C31 121.5(6) . . ? C34 C33 C32 118.5(6) . . ? C34 C33 H33A 120.8 . . ? C32 C33 H33A 120.8 . . ? C33 C34 C35 121.2(6) . . ? C33 C34 H34A 119.4 . . ? C35 C34 H34A 119.4 . . ? C34 C35 C36 118.3(7) . . ? C34 C35 H35A 120.9 . . ? C36 C35 H35A 120.9 . . ? N7 C36 C35 121.0(5) . . ? N7 C36 C37 117.0(4) . . ? C35 C36 C37 122.0(5) . . ? N8 C37 C38 121.2(5) . . ? N8 C37 C36 115.2(4) . . ? C38 C37 C36 123.6(4) . . ? C39 C38 C37 119.6(5) . . ? C39 C38 H38A 120.2 . . ? C37 C38 H38A 120.2 . . ? C38 C39 C40 119.8(5) . . ? C38 C39 H39A 120.1 . . ? C40 C39 H39A 120.1 . . ? C39 C40 C41 119.2(5) . . ? C39 C40 H40A 120.4 . . ? C41 C40 H40A 120.4 . . ? N8 C41 C40 121.4(4) . . ? N8 C41 C42 117.3(4) . . ? C40 C41 C42 121.2(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 N9 C44 122.0(6) . . ? C48 N9 Cu2 113.0(3) . . ? C44 N9 Cu2 125.0(5) . . ? C49 N10 C53 120.1(5) . . ? C49 N10 Cu2 115.9(4) . . ? C53 N10 Cu2 124.0(4) . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 N9 122.0(10) . . ? C45 C44 C43 119.8(9) . . ? N9 C44 C43 118.2(6) . . ? C46 C45 C44 118.2(10) . . ? C46 C45 H45A 120.9 . . ? C44 C45 H45A 120.9 . . ? C45 C46 C47 123.4(7) . . ? C45 C46 H46A 118.3 . . ? C47 C46 H46A 118.3 . . ? C48 C47 C46 113.8(9) . . ? C48 C47 H47A 123.1 . . ? C46 C47 H47A 123.1 . . ? N9 C48 C47 120.2(8) . . ? N9 C48 C49 115.8(4) . . ? C47 C48 C49 123.9(8) . . ? N10 C49 C50 120.7(8) . . ? N10 C49 C48 115.5(4) . . ? C50 C49 C48 123.8(7) . . ? C51 C50 C49 119.9(10) . . ? C51 C50 H50A 120.1 . . ? C49 C50 H50A 120.1 . . ? C52 C51 C50 120.2(8) . . ? C52 C51 H51A 119.9 . . ? C50 C51 H51A 119.9 . . ? C51 C52 C53 119.8(9) . . ? C51 C52 H52A 120.1 . . ? C53 C52 H52A 120.1 . . ? N10 C53 C52 119.3(8) . . ? N10 C53 C54 116.3(6) . . ? C52 C53 C54 124.4(8) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? F14 P1 F12 90.5(2) . . ? F14 P1 F13 90.8(2) . . ? F12 P1 F13 89.6(2) . . ? F14 P1 F11 90.8(2) . . ? F12 P1 F11 178.7(2) . . ? F13 P1 F11 90.4(2) . . ? F14 P1 F10 178.8(2) . . ? F12 P1 F10 89.6(2) . . ? F13 P1 F10 90.3(2) . . ? F11 P1 F10 89.1(2) . . ? F14 P1 F15 89.52(19) . . ? F12 P1 F15 90.99(19) . . ? F13 P1 F15 179.3(2) . . ? F11 P1 F15 89.0(2) . . ? F10 P1 F15 89.3(2) . . ? F20 P2 F21 93.0(3) . . ? F20 P2 F23 90.1(2) . . ? F21 P2 F23 91.2(2) . . ? F20 P2 F25 89.1(3) . . ? F21 P2 F25 177.3(2) . . ? F23 P2 F25 90.6(2) . . ? F20 P2 F24 90.1(2) . . ? F21 P2 F24 89.1(2) . . ? F23 P2 F24 179.7(2) . . ? F25 P2 F24 89.2(2) . . ? F20 P2 F22 176.2(3) . . ? F21 P2 F22 89.4(3) . . ? F23 P2 F22 92.7(2) . . ? F25 P2 F22 88.4(2) . . ? F24 P2 F22 87.0(2) . . ? F30 P3 F33 90.9(2) . . ? F30 P3 F31 178.6(3) . . ? F33 P3 F31 90.5(2) . . ? F30 P3 F32 90.3(2) . . ? F33 P3 F32 90.4(2) . . ? F31 P3 F32 90.0(3) . . ? F30 P3 F34 89.8(2) . . ? F33 P3 F34 90.4(2) . . ? F31 P3 F34 90.0(3) . . ? F32 P3 F34 179.1(2) . . ? F30 P3 F35 90.3(2) . . ? F33 P3 F35 178.9(2) . . ? F31 P3 F35 88.3(2) . . ? F32 P3 F35 89.6(2) . . ? F34 P3 F35 89.5(2) . . ? F44 P4 F40 89.5(2) . . ? F44 P4 F45 179.3(2) . . ? F40 P4 F45 90.69(19) . . ? F44 P4 F41 90.5(2) . . ? F40 P4 F41 179.5(2) . . ? F45 P4 F41 89.29(18) . . ? F44 P4 F43 90.18(18) . . ? F40 P4 F43 90.1(2) . . ? F45 P4 F43 90.46(17) . . ? F41 P4 F43 89.38(19) . . ? F44 P4 F42 90.04(17) . . ? F40 P4 F42 90.0(2) . . ? F45 P4 F42 89.32(17) . . ? F41 P4 F42 90.5(2) . . ? F43 P4 F42 179.74(19) . . ? N100 C100 C101 170(2) . . ? C301 O300 C303 133.7(16) . . ? O300 C301 C302 128(2) . . ? O300 C301 H30B 105.4 . . ? C302 C301 H30B 105.4 . . ? O300 C301 H30C 105.4 . . ? C302 C301 H30C 105.4 . . ? H30B C301 H30C 106.0 . . ? C304 C303 O300 129.8(15) . . ? C304 C303 H30G 104.8 . . ? O300 C303 H30G 104.8 . . ? C304 C303 H30H 104.8 . . ? O300 C303 H30H 104.8 . . ? H30G C303 H30H 105.8 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.657 _refine_diff_density_min -1.351 _refine_diff_density_rms 0.091