# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Catherine E. Housecroft' _publ_contact_author_email Catherine.Housecroft@unibas.ch loop_ _publ_author_name 'Ruben D. Costa' 'Daniel Tordera' 'Enrique Orti' 'Henk J. Bolink' 'Jonas Schonle' 'Stefan Graber' ; C.E.Housecroft ; 'Edwin C. Constable' 'Jennifer A. Zampese' data_again _database_code_depnum_ccdc_archive 'CCDC 802645' #TrackingRef 'JS25.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H36 Cu N2 O P2, F6 P, C H Cl3' _chemical_formula_sum 'C47 H37 Cl3 Cu F6 N2 O P3' _chemical_formula_weight 1022.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 9.7047(19) _cell_length_b 29.019(6) _cell_length_c 16.265(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.76(3) _cell_angle_gamma 90.00 _cell_volume 4484.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.837 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7044 _exptl_absorpt_correction_T_max 0.9209 _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 73671 _diffrn_reflns_av_R_equivalents 0.1013 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.50 _reflns_number_total 11274 _reflns_number_gt 10623 _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^)+(0.0453P)^2^+3.1889P] 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 11274 _refine_ls_number_parameters 660 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.1094 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.154 _refine_ls_shift/su_max 0.004 _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 0.54767(2) 0.884379(8) 0.804020(13) 0.02344(7) Uani 1 1 d . . . P1 P 0.46781(5) 0.870526(17) 0.66723(3) 0.02442(10) Uani 1 1 d . . . P2 P 0.78397(5) 0.883239(16) 0.84596(3) 0.02361(10) Uani 1 1 d . . . O1 O 0.69491(14) 0.80752(5) 0.72059(8) 0.0266(3) Uani 1 1 d . . . N1 N 0.45168(17) 0.93375(5) 0.86270(10) 0.0270(3) Uani 1 1 d . . . N2 N 0.46305(17) 0.84369(6) 0.88616(10) 0.0266(3) Uani 1 1 d . . . C1 C 0.6091(2) 0.85921(7) 0.61140(12) 0.0272(4) Uani 1 1 d . . . C2 C 0.7180(2) 0.83033(6) 0.64978(11) 0.0255(3) Uani 1 1 d . . . C3 C 0.8376(2) 0.82404(7) 0.61708(13) 0.0322(4) Uani 1 1 d . . . H3A H 0.9123 0.8050 0.6451 0.039 Uiso 1 1 calc R . . C4 C 0.8463(3) 0.84603(9) 0.54271(15) 0.0407(5) Uani 1 1 d . . . H4A H 0.9283 0.8423 0.5199 0.049 Uiso 1 1 calc R . . C5 C 0.7374(3) 0.87323(9) 0.50126(15) 0.0450(5) Uani 1 1 d . . . H5A H 0.7434 0.8873 0.4494 0.054 Uiso 1 1 calc R . . C6 C 0.6189(3) 0.87998(8) 0.53553(14) 0.0371(5) Uani 1 1 d . . . H6A H 0.5442 0.8989 0.5071 0.044 Uiso 1 1 calc R . . C7 C 0.80982(19) 0.79469(6) 0.78242(12) 0.0264(3) Uani 1 1 d . . . C8 C 0.86347(19) 0.82594(6) 0.84615(12) 0.0267(3) Uani 1 1 d . . . C9 C 0.9721(2) 0.81077(8) 0.91043(14) 0.0342(4) Uani 1 1 d . . . H9A H 1.0118 0.8313 0.9544 0.041 Uiso 1 1 calc R . . C10 C 1.0229(2) 0.76604(8) 0.91079(15) 0.0382(5) Uani 1 1 d . . . H10A H 1.0966 0.7562 0.9551 0.046 Uiso 1 1 calc R . . C11 C 0.9670(2) 0.73581(7) 0.84746(15) 0.0375(5) Uani 1 1 d . . . H11A H 1.0019 0.7052 0.8483 0.045 Uiso 1 1 calc R . . C12 C 0.8599(2) 0.75010(7) 0.78258(14) 0.0335(4) Uani 1 1 d . . . H12A H 0.8211 0.7294 0.7386 0.040 Uiso 1 1 calc R . . C13 C 0.3674(2) 0.91580(7) 0.60457(12) 0.0299(4) Uani 1 1 d . . . C14 C 0.2385(3) 0.90839(9) 0.55120(15) 0.0443(5) Uani 1 1 d . . . H14A H 0.1989 0.8783 0.5452 0.053 Uiso 1 1 calc R . . C15 C 0.1673(3) 0.94504(11) 0.50648(19) 0.0583(7) Uani 1 1 d . . . H15A H 0.0788 0.9398 0.4701 0.070 Uiso 1 1 calc R . . C16 C 0.2228(3) 0.98851(10) 0.51415(17) 0.0553(7) Uani 1 1 d . . . H16A H 0.1736 1.0132 0.4828 0.066 Uiso 1 1 calc R . . C17 C 0.3500(3) 0.99628(9) 0.56738(17) 0.0515(6) Uani 1 1 d . . . H17A H 0.3891 1.0264 0.5729 0.062 Uiso 1 1 calc R . . C18 C 0.4212(3) 0.96012(8) 0.61288(15) 0.0408(5) Uani 1 1 d . . . H18A H 0.5082 0.9658 0.6504 0.049 Uiso 1 1 calc R . . C19 C 0.3586(2) 0.81911(7) 0.64700(12) 0.0289(4) Uani 1 1 d . . . C20 C 0.3682(2) 0.78799(8) 0.58339(14) 0.0379(4) Uani 1 1 d . . . H20A H 0.4300 0.7942 0.5464 0.046 Uiso 1 1 calc R . . C21 C 0.2881(3) 0.74800(9) 0.57355(19) 0.0506(6) Uani 1 1 d . . . H21A H 0.2939 0.7273 0.5292 0.061 Uiso 1 1 calc R . . C22 C 0.2005(3) 0.73829(9) 0.62795(19) 0.0516(6) Uani 1 1 d . . . H22A H 0.1479 0.7104 0.6221 0.062 Uiso 1 1 calc R . . C23 C 0.1889(2) 0.76908(10) 0.69111(17) 0.0464(6) Uani 1 1 d . . . H23A H 0.1273 0.7626 0.7281 0.056 Uiso 1 1 calc R . . C24 C 0.2672(2) 0.80938(8) 0.70045(14) 0.0367(4) Uani 1 1 d . . . H24A H 0.2584 0.8305 0.7437 0.044 Uiso 1 1 calc R . . C25 C 0.8839(2) 0.91901(7) 0.78735(11) 0.0276(4) Uani 1 1 d . . . C26 C 0.8256(2) 0.96078(8) 0.75665(14) 0.0358(4) Uani 1 1 d . . . H26A H 0.7342 0.9690 0.7643 0.043 Uiso 1 1 calc R . . C27 C 0.8992(3) 0.99074(9) 0.71493(15) 0.0460(6) Uani 1 1 d . . . H27A H 0.8584 1.0193 0.6940 0.055 Uiso 1 1 calc R . . C28 C 1.0319(3) 0.97894(10) 0.70399(16) 0.0521(7) Uani 1 1 d . . . H28A H 1.0827 0.9994 0.6755 0.063 Uiso 1 1 calc R . . C29 C 1.0910(3) 0.93760(10) 0.73425(17) 0.0491(6) Uani 1 1 d . . . H29A H 1.1825 0.9297 0.7265 0.059 Uiso 1 1 calc R . . C30 C 1.0182(2) 0.90749(8) 0.77586(15) 0.0381(5) Uani 1 1 d . . . H30A H 1.0597 0.8790 0.7966 0.046 Uiso 1 1 calc R . . C31 C 0.84911(19) 0.90093(6) 0.95459(12) 0.0264(3) Uani 1 1 d . . . C32 C 0.7823(2) 0.88248(7) 1.01547(12) 0.0291(4) Uani 1 1 d . . . H32A H 0.7036 0.8626 0.9990 0.035 Uiso 1 1 calc R . . C33 C 0.8295(2) 0.89282(7) 1.09965(13) 0.0335(4) Uani 1 1 d . . . H33A H 0.7843 0.8797 1.1407 0.040 Uiso 1 1 calc R . . C34 C 0.9424(2) 0.92227(8) 1.12375(13) 0.0365(4) Uani 1 1 d . . . H34A H 0.9748 0.9294 1.1815 0.044 Uiso 1 1 calc R . . C35 C 1.0084(2) 0.94134(8) 1.06408(14) 0.0376(5) Uani 1 1 d . . . H35A H 1.0857 0.9617 1.0809 0.045 Uiso 1 1 calc R . . C36 C 0.9620(2) 0.93082(7) 0.97941(13) 0.0329(4) Uani 1 1 d . . . H36A H 1.0075 0.9440 0.9386 0.040 Uiso 1 1 calc R . . C37 C 0.4427(2) 0.97875(7) 0.84511(15) 0.0361(4) Uani 1 1 d . . . H37A H 0.4846 0.9899 0.8011 0.043 Uiso 1 1 calc R . . C38 C 0.3755(3) 1.00977(8) 0.88781(18) 0.0450(5) Uani 1 1 d . . . H38A H 0.3695 1.0414 0.8727 0.054 Uiso 1 1 calc R . . C39 C 0.3173(3) 0.99388(9) 0.95261(17) 0.0459(6) Uani 1 1 d . . . H39A H 0.2714 1.0145 0.9836 0.055 Uiso 1 1 calc R . . C40 C 0.3265(2) 0.94763(8) 0.97219(14) 0.0383(5) Uani 1 1 d . . . H40A H 0.2876 0.9361 1.0172 0.046 Uiso 1 1 calc R . . C41 C 0.39312(19) 0.91806(7) 0.92559(12) 0.0269(3) Uani 1 1 d . . . C42 C 0.40248(19) 0.86778(7) 0.94009(12) 0.0271(4) Uani 1 1 d . . . C43 C 0.3529(2) 0.84610(9) 1.00486(14) 0.0396(5) Uani 1 1 d . . . H43A H 0.3113 0.8636 1.0428 0.047 Uiso 1 1 calc R . . C44 C 0.3651(3) 0.79915(10) 1.01306(17) 0.0488(6) Uani 1 1 d . . . H44A H 0.3331 0.7838 1.0573 0.059 Uiso 1 1 calc R . . C45 C 0.4240(3) 0.77435(9) 0.95666(17) 0.0461(6) Uani 1 1 d . . . H45A H 0.4310 0.7417 0.9604 0.055 Uiso 1 1 calc R . . C46 C 0.4727(2) 0.79800(7) 0.89446(14) 0.0355(4) Uani 1 1 d . . . H46A H 0.5147 0.7810 0.8561 0.043 Uiso 1 1 calc R . . C100 C 1.0747(14) 0.8409(3) 1.3108(8) 0.037(2) Uani 0.471(14) 1 d P A 3 H10B H 1.1475 0.8611 1.2939 0.045 Uiso 0.471(14) 1 calc PR A 3 Cl1 Cl 1.1458(9) 0.8142(3) 1.3978(4) 0.0676(16) Uani 0.471(14) 1 d P A 3 Cl2 Cl 1.01975(18) 0.79918(8) 1.23032(11) 0.0409(10) Uani 0.471(14) 1 d PDU A 3 Cl3 Cl 0.9253(7) 0.8775(2) 1.3270(4) 0.0655(10) Uani 0.471(14) 1 d P A 3 C10' C 1.0531(17) 0.8433(6) 1.3067(8) 0.072(5) Uani 0.529(14) 1 d P A 4 H10C H 1.1088 0.8676 1.2847 0.087 Uiso 0.529(14) 1 calc PR A 4 Cl1' Cl 1.1571(6) 0.8169(2) 1.4026(3) 0.0528(11) Uani 0.529(14) 1 d P A 4 Cl2' Cl 1.0066(8) 0.8020(2) 1.2361(4) 0.152(3) Uani 0.529(14) 1 d PDU A 4 Cl3' Cl 0.9052(9) 0.8644(4) 1.3237(4) 0.123(3) Uani 0.529(14) 1 d P A 4 P10 P 0.42666(10) 0.89955(2) 1.24719(4) 0.0554(2) Uani 1 1 d . . . F10 F 0.3320(5) 0.85729(12) 1.2136(2) 0.0618(12) Uani 0.612(7) 1 d P B 1 F11 F 0.5233(6) 0.8876(3) 1.1855(6) 0.141(3) Uani 0.612(7) 1 d P B 1 F12 F 0.5221(11) 0.9415(2) 1.2811(3) 0.138(4) Uani 0.612(7) 1 d P B 1 F13 F 0.3409(6) 0.93081(18) 1.1779(4) 0.0947(19) Uani 0.612(7) 1 d P B 1 F14 F 0.5087(12) 0.8725(2) 1.3232(6) 0.190(5) Uani 0.612(7) 1 d P B 1 F15 F 0.3150(11) 0.9131(2) 1.3027(5) 0.180(4) Uani 0.612(7) 1 d P B 1 F10' F 0.2805(15) 0.8832(8) 1.2123(10) 0.217(9) Uani 0.388(7) 1 d PU B 2 F11' F 0.4312(18) 0.9160(4) 1.1573(4) 0.146(7) Uani 0.388(7) 1 d P B 2 F12' F 0.5792(9) 0.9115(6) 1.2743(7) 0.133(4) Uani 0.388(7) 1 d P B 2 F13' F 0.3944(14) 0.9480(3) 1.2735(9) 0.141(5) Uani 0.388(7) 1 d P B 2 F14' F 0.481(2) 0.8507(3) 1.2241(7) 0.186(8) Uani 0.388(7) 1 d P B 2 F15' F 0.4134(9) 0.8809(3) 1.3333(4) 0.076(2) Uani 0.388(7) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02417(12) 0.02454(12) 0.02319(12) -0.00128(7) 0.00856(8) 0.00265(8) P1 0.0239(2) 0.0285(2) 0.0220(2) -0.00064(16) 0.00723(16) 0.00269(17) P2 0.0229(2) 0.0238(2) 0.0248(2) -0.00258(16) 0.00658(17) 0.00201(15) O1 0.0267(6) 0.0284(6) 0.0265(6) -0.0001(5) 0.0096(5) 0.0013(5) N1 0.0274(7) 0.0251(7) 0.0308(8) -0.0020(6) 0.0116(6) 0.0029(6) N2 0.0278(7) 0.0261(7) 0.0260(7) 0.0011(6) 0.0053(6) -0.0009(6) C1 0.0280(9) 0.0301(9) 0.0255(8) -0.0020(7) 0.0105(7) 0.0006(7) C2 0.0291(9) 0.0254(8) 0.0242(8) -0.0045(6) 0.0107(7) -0.0006(6) C3 0.0314(9) 0.0347(10) 0.0338(10) -0.0043(8) 0.0143(8) 0.0038(8) C4 0.0424(12) 0.0475(12) 0.0397(11) -0.0019(9) 0.0262(10) 0.0030(10) C5 0.0540(14) 0.0516(13) 0.0370(11) 0.0088(10) 0.0275(11) 0.0090(11) C6 0.0411(11) 0.0447(12) 0.0290(10) 0.0061(8) 0.0156(9) 0.0092(9) C7 0.0261(8) 0.0259(8) 0.0298(9) 0.0009(7) 0.0115(7) 0.0028(6) C8 0.0250(8) 0.0259(8) 0.0305(9) -0.0005(7) 0.0083(7) 0.0035(6) C9 0.0295(9) 0.0357(10) 0.0363(10) -0.0012(8) 0.0043(8) 0.0068(8) C10 0.0327(10) 0.0389(11) 0.0430(11) 0.0079(9) 0.0076(9) 0.0110(8) C11 0.0383(11) 0.0273(9) 0.0495(12) 0.0071(8) 0.0152(9) 0.0099(8) C12 0.0376(10) 0.0250(9) 0.0408(11) -0.0019(8) 0.0147(9) 0.0032(7) C13 0.0328(9) 0.0343(10) 0.0240(8) 0.0007(7) 0.0088(7) 0.0076(7) C14 0.0424(12) 0.0451(13) 0.0403(11) -0.0008(10) -0.0036(9) 0.0082(10) C15 0.0540(16) 0.0608(17) 0.0508(15) 0.0030(13) -0.0113(12) 0.0180(13) C16 0.0714(18) 0.0509(15) 0.0394(12) 0.0078(11) 0.0018(12) 0.0263(13) C17 0.0729(18) 0.0377(12) 0.0426(13) 0.0090(10) 0.0087(12) 0.0093(12) C18 0.0470(12) 0.0367(11) 0.0366(11) 0.0056(9) 0.0037(9) 0.0021(9) C19 0.0242(8) 0.0336(9) 0.0283(9) 0.0016(7) 0.0041(7) 0.0014(7) C20 0.0387(11) 0.0372(11) 0.0381(11) -0.0058(9) 0.0083(9) -0.0033(9) C21 0.0522(14) 0.0397(13) 0.0572(15) -0.0108(11) 0.0050(12) -0.0080(11) C22 0.0387(12) 0.0435(13) 0.0668(17) 0.0070(12) -0.0028(11) -0.0110(10) C23 0.0282(10) 0.0582(15) 0.0518(13) 0.0146(11) 0.0056(9) -0.0076(10) C24 0.0263(9) 0.0486(12) 0.0354(10) 0.0021(9) 0.0072(8) -0.0018(8) C25 0.0285(9) 0.0307(9) 0.0246(8) -0.0045(7) 0.0079(7) -0.0029(7) C26 0.0372(10) 0.0355(10) 0.0343(10) 0.0026(8) 0.0067(8) -0.0028(8) C27 0.0584(15) 0.0403(12) 0.0381(11) 0.0064(9) 0.0069(10) -0.0108(11) C28 0.0643(16) 0.0575(15) 0.0402(12) -0.0035(11) 0.0240(12) -0.0255(13) C29 0.0452(13) 0.0603(16) 0.0494(13) -0.0113(12) 0.0276(11) -0.0126(11) C30 0.0349(10) 0.0427(11) 0.0411(11) -0.0065(9) 0.0182(9) -0.0017(9) C31 0.0262(8) 0.0265(8) 0.0269(8) -0.0030(7) 0.0057(7) 0.0034(7) C32 0.0303(9) 0.0284(9) 0.0284(9) 0.0008(7) 0.0058(7) 0.0019(7) C33 0.0402(11) 0.0339(10) 0.0271(9) 0.0021(7) 0.0087(8) 0.0048(8) C34 0.0438(11) 0.0380(11) 0.0260(9) -0.0048(8) 0.0028(8) 0.0029(9) C35 0.0364(11) 0.0404(11) 0.0351(10) -0.0100(8) 0.0053(8) -0.0061(9) C36 0.0335(10) 0.0351(10) 0.0312(9) -0.0067(8) 0.0092(8) -0.0039(8) C37 0.0394(11) 0.0265(9) 0.0465(12) -0.0002(8) 0.0184(9) 0.0039(8) C38 0.0480(13) 0.0289(10) 0.0624(15) -0.0057(10) 0.0212(11) 0.0082(9) C39 0.0444(12) 0.0440(13) 0.0534(14) -0.0139(11) 0.0194(11) 0.0119(10) C40 0.0347(10) 0.0477(12) 0.0367(10) -0.0071(9) 0.0169(9) 0.0063(9) C41 0.0229(8) 0.0333(9) 0.0256(8) -0.0035(7) 0.0077(6) 0.0013(7) C42 0.0227(8) 0.0336(9) 0.0254(8) 0.0010(7) 0.0060(6) -0.0007(7) C43 0.0360(11) 0.0532(13) 0.0322(10) 0.0078(9) 0.0132(8) -0.0020(9) C44 0.0453(13) 0.0559(15) 0.0467(13) 0.0225(11) 0.0133(11) -0.0051(11) C45 0.0458(13) 0.0358(11) 0.0548(14) 0.0173(10) 0.0058(11) -0.0044(9) C46 0.0382(11) 0.0278(9) 0.0392(11) 0.0034(8) 0.0048(9) -0.0004(8) C100 0.031(3) 0.035(3) 0.049(5) -0.007(3) 0.013(3) 0.000(3) Cl1 0.082(3) 0.053(2) 0.074(3) 0.001(2) 0.030(2) 0.005(2) Cl2 0.0378(13) 0.0476(10) 0.0318(12) -0.0053(6) -0.0058(5) -0.0058(5) Cl3 0.0693(16) 0.090(2) 0.0442(13) 0.0136(12) 0.0284(11) 0.0215(18) C10' 0.073(8) 0.113(9) 0.036(4) 0.028(5) 0.020(4) 0.032(5) Cl1' 0.0531(14) 0.066(2) 0.0335(13) -0.0023(12) -0.0062(12) 0.0070(13) Cl2' 0.187(4) 0.104(3) 0.141(3) -0.005(2) -0.027(3) -0.007(2) Cl3' 0.137(5) 0.190(6) 0.058(2) 0.047(3) 0.057(3) 0.112(4) P10 0.0821(5) 0.0383(3) 0.0403(3) 0.0106(3) -0.0008(3) -0.0175(3) F10 0.086(3) 0.0453(17) 0.0601(18) -0.0113(13) 0.0293(19) -0.0311(16) F11 0.075(3) 0.142(6) 0.228(9) -0.059(6) 0.085(4) -0.035(3) F12 0.244(9) 0.080(3) 0.059(2) 0.013(2) -0.041(4) -0.102(5) F13 0.095(3) 0.080(3) 0.099(4) 0.042(3) -0.001(3) 0.011(2) F14 0.229(9) 0.103(5) 0.170(7) 0.090(5) -0.117(7) -0.066(5) F15 0.316(11) 0.097(4) 0.191(7) -0.048(5) 0.198(8) -0.037(6) F10' 0.105(9) 0.33(2) 0.195(12) 0.059(14) -0.024(8) -0.119(12) F11' 0.253(15) 0.138(9) 0.030(3) 0.023(4) -0.011(5) -0.143(10) F12' 0.071(4) 0.203(13) 0.127(8) -0.009(9) 0.025(4) -0.007(7) F13' 0.172(10) 0.069(5) 0.208(13) 0.043(6) 0.099(9) 0.059(6) F14' 0.40(2) 0.052(4) 0.148(9) 0.003(4) 0.157(12) 0.015(8) F15' 0.117(6) 0.082(5) 0.035(3) -0.007(3) 0.027(3) -0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.0480(16) . ? Cu1 N2 2.0738(16) . ? Cu1 P1 2.2382(8) . ? Cu1 P2 2.2555(8) . ? P1 C13 1.819(2) . ? P1 C19 1.821(2) . ? P1 C1 1.8219(19) . ? P2 C25 1.818(2) . ? P2 C31 1.825(2) . ? P2 C8 1.8327(19) . ? O1 C2 1.386(2) . ? O1 C7 1.391(2) . ? N1 C37 1.336(3) . ? N1 C41 1.347(2) . ? N2 C46 1.334(3) . ? N2 C42 1.347(2) . ? C1 C2 1.393(3) . ? C1 C6 1.394(3) . ? C2 C3 1.384(3) . ? C3 C4 1.385(3) . ? C3 H3A 0.9500 . ? C4 C5 1.380(4) . ? C4 H4A 0.9500 . ? C5 C6 1.390(3) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.382(3) . ? C7 C8 1.396(3) . ? C8 C9 1.396(3) . ? C9 C10 1.388(3) . ? C9 H9A 0.9500 . ? C10 C11 1.377(3) . ? C10 H10A 0.9500 . ? C11 C12 1.385(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.384(3) . ? C13 C14 1.387(3) . ? C14 C15 1.390(4) . ? C14 H14A 0.9500 . ? C15 C16 1.367(5) . ? C15 H15A 0.9500 . ? C16 C17 1.375(4) . ? C16 H16A 0.9500 . ? C17 C18 1.385(3) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.391(3) . ? C19 C24 1.392(3) . ? C20 C21 1.387(3) . ? C20 H20A 0.9500 . ? C21 C22 1.376(4) . ? C21 H21A 0.9500 . ? C22 C23 1.383(4) . ? C22 H22A 0.9500 . ? C23 C24 1.386(3) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.387(3) . ? C25 C30 1.394(3) . ? C26 C27 1.388(3) . ? C26 H26A 0.9500 . ? C27 C28 1.378(4) . ? C27 H27A 0.9500 . ? C28 C29 1.377(4) . ? C28 H28A 0.9500 . ? C29 C30 1.384(3) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.391(3) . ? C31 C32 1.396(3) . ? C32 C33 1.385(3) . ? C32 H32A 0.9500 . ? C33 C34 1.382(3) . ? C33 H33A 0.9500 . ? C34 C35 1.383(3) . ? C34 H34A 0.9500 . ? C35 C36 1.393(3) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.380(3) . ? C37 H37A 0.9500 . ? C38 C39 1.373(4) . ? C38 H38A 0.9500 . ? C39 C40 1.378(4) . ? C39 H39A 0.9500 . ? C40 C41 1.389(3) . ? C40 H40A 0.9500 . ? C41 C42 1.478(3) . ? C42 C43 1.394(3) . ? C43 C44 1.372(4) . ? C43 H43A 0.9500 . ? C44 C45 1.379(4) . ? C44 H44A 0.9500 . ? C45 C46 1.383(3) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C100 Cl1 1.637(16) . ? C100 Cl2 1.783(10) . ? C100 Cl3 1.858(15) . ? C100 H10B 1.0000 . ? C10' Cl3' 1.635(17) . ? C10' Cl2' 1.658(16) . ? C10' Cl1' 1.843(16) . ? C10' H10C 1.0000 . ? P10 F10' 1.494(11) . ? P10 F12' 1.497(9) . ? P10 F13' 1.521(9) . ? P10 F15' 1.532(6) . ? P10 F14 1.542(5) . ? P10 F11 1.546(6) . ? P10 F11' 1.547(6) . ? P10 F13 1.551(4) . ? P10 F12 1.560(4) . ? P10 F10 1.562(3) . ? P10 F14' 1.585(9) . ? P10 F15 1.595(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N2 79.66(7) . . ? N1 Cu1 P1 119.39(5) . . ? N2 Cu1 P1 115.84(5) . . ? N1 Cu1 P2 113.60(5) . . ? N2 Cu1 P2 107.97(5) . . ? P1 Cu1 P2 115.00(3) . . ? C13 P1 C19 105.37(10) . . ? C13 P1 C1 102.86(9) . . ? C19 P1 C1 103.39(9) . . ? C13 P1 Cu1 117.68(7) . . ? C19 P1 Cu1 113.43(7) . . ? C1 P1 Cu1 112.62(7) . . ? C25 P2 C31 103.33(9) . . ? C25 P2 C8 104.44(9) . . ? C31 P2 C8 101.01(9) . . ? C25 P2 Cu1 116.84(7) . . ? C31 P2 Cu1 114.76(7) . . ? C8 P2 Cu1 114.55(6) . . ? C2 O1 C7 119.14(14) . . ? C37 N1 C41 118.29(17) . . ? C37 N1 Cu1 126.88(14) . . ? C41 N1 Cu1 114.83(13) . . ? C46 N2 C42 118.74(18) . . ? C46 N2 Cu1 127.03(15) . . ? C42 N2 Cu1 114.01(13) . . ? C2 C1 C6 118.31(18) . . ? C2 C1 P1 117.67(14) . . ? C6 C1 P1 123.88(16) . . ? C3 C2 O1 123.16(18) . . ? C3 C2 C1 121.75(18) . . ? O1 C2 C1 115.05(16) . . ? C2 C3 C4 118.7(2) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C5 C4 C3 120.9(2) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 119.9(2) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C5 C6 C1 120.4(2) . . ? C5 C6 H6A 119.8 . . ? C1 C6 H6A 119.8 . . ? C12 C7 O1 118.78(18) . . ? C12 C7 C8 121.96(19) . . ? O1 C7 C8 119.05(16) . . ? C7 C8 C9 117.49(18) . . ? C7 C8 P2 119.68(14) . . ? C9 C8 P2 122.73(15) . . ? C10 C9 C8 120.7(2) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C11 C10 C9 120.5(2) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 119.93(19) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C7 C12 C11 119.4(2) . . ? C7 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C18 C13 C14 118.6(2) . . ? C18 C13 P1 117.91(16) . . ? C14 C13 P1 123.41(18) . . ? C13 C14 C15 119.9(3) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C16 C15 C14 120.9(3) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C15 C16 C17 119.7(2) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C16 C17 C18 119.9(3) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C13 C18 C17 121.0(2) . . ? C13 C18 H18A 119.5 . . ? C17 C18 H18A 119.5 . . ? C20 C19 C24 118.7(2) . . ? C20 C19 P1 122.82(16) . . ? C24 C19 P1 118.35(16) . . ? C21 C20 C19 120.6(2) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C22 C21 C20 120.1(3) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C21 C22 C23 120.0(2) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C24 120.1(2) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C19 120.5(2) . . ? C23 C24 H24A 119.8 . . ? C19 C24 H24A 119.8 . . ? C26 C25 C30 119.0(2) . . ? C26 C25 P2 117.73(15) . . ? C30 C25 P2 123.14(17) . . ? C25 C26 C27 120.7(2) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C28 C27 C26 119.7(2) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? C29 C28 C27 120.2(2) . . ? C29 C28 H28A 119.9 . . ? C27 C28 H28A 119.9 . . ? C28 C29 C30 120.5(2) . . ? C28 C29 H29A 119.7 . . ? C30 C29 H29A 119.7 . . ? C29 C30 C25 119.9(2) . . ? C29 C30 H30A 120.1 . . ? C25 C30 H30A 120.1 . . ? C36 C31 C32 119.06(18) . . ? C36 C31 P2 123.58(15) . . ? C32 C31 P2 117.35(15) . . ? C33 C32 C31 120.65(19) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C34 C33 C32 119.9(2) . . ? C34 C33 H33A 120.1 . . ? C32 C33 H33A 120.1 . . ? C33 C34 C35 120.17(19) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C34 C35 C36 120.2(2) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C31 C36 C35 120.0(2) . . ? C31 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? N1 C37 C38 123.2(2) . . ? N1 C37 H37A 118.4 . . ? C38 C37 H37A 118.4 . . ? C39 C38 C37 118.6(2) . . ? C39 C38 H38A 120.7 . . ? C37 C38 H38A 120.7 . . ? C38 C39 C40 119.2(2) . . ? C38 C39 H39A 120.4 . . ? C40 C39 H39A 120.4 . . ? C39 C40 C41 119.4(2) . . ? C39 C40 H40A 120.3 . . ? C41 C40 H40A 120.3 . . ? N1 C41 C40 121.41(19) . . ? N1 C41 C42 115.68(16) . . ? C40 C41 C42 122.90(18) . . ? N2 C42 C43 121.43(19) . . ? N2 C42 C41 115.42(16) . . ? C43 C42 C41 123.15(19) . . ? C44 C43 C42 119.1(2) . . ? C44 C43 H43A 120.5 . . ? C42 C43 H43A 120.5 . . ? C43 C44 C45 119.5(2) . . ? C43 C44 H44A 120.2 . . ? C45 C44 H44A 120.2 . . ? C44 C45 C46 118.5(2) . . ? C44 C45 H45A 120.7 . . ? C46 C45 H45A 120.7 . . ? N2 C46 C45 122.7(2) . . ? N2 C46 H46A 118.7 . . ? C45 C46 H46A 118.7 . . ? Cl1 C100 Cl2 109.0(7) . . ? Cl1 C100 Cl3 110.6(8) . . ? Cl2 C100 Cl3 111.5(7) . . ? Cl1 C100 H10B 108.6 . . ? Cl2 C100 H10B 108.6 . . ? Cl3 C100 H10B 108.6 . . ? Cl3' C10' Cl2' 105.3(10) . . ? Cl3' C10' Cl1' 111.2(8) . . ? Cl2' C10' Cl1' 108.1(9) . . ? Cl3' C10' H10C 110.7 . . ? Cl2' C10' H10C 110.7 . . ? Cl1' C10' H10C 110.7 . . ? F10' P10 F12' 172.3(10) . . ? F10' P10 F13' 99.6(11) . . ? F12' P10 F13' 87.2(7) . . ? F10' P10 F15' 89.1(7) . . ? F12' P10 F15' 94.3(5) . . ? F13' P10 F15' 90.5(5) . . ? F10' P10 F14 116.0(7) . . ? F12' P10 F14 64.1(6) . . ? F13' P10 F14 110.3(7) . . ? F10' P10 F11 109.7(9) . . ? F12' P10 F11 63.2(5) . . ? F13' P10 F11 125.2(5) . . ? F15' P10 F11 133.6(5) . . ? F14 P10 F11 97.1(7) . . ? F10' P10 F11' 86.9(7) . . ? F12' P10 F11' 89.4(7) . . ? F13' P10 F11' 91.6(7) . . ? F15' P10 F11' 175.8(4) . . ? F14 P10 F11' 143.7(9) . . ? F11 P10 F11' 47.0(6) . . ? F10' P10 F13 65.3(7) . . ? F12' P10 F13 115.6(6) . . ? F13' P10 F13 63.4(5) . . ? F15' P10 F13 137.6(4) . . ? F14 P10 F13 173.6(5) . . ? F11 P10 F13 88.1(4) . . ? F10' P10 F12 146.3(10) . . ? F13' P10 F12 47.3(5) . . ? F15' P10 F12 96.1(3) . . ? F14 P10 F12 86.6(3) . . ? F11 P10 F12 90.5(5) . . ? F11' P10 F12 87.9(3) . . ? F13 P10 F12 89.6(3) . . ? F12' P10 F10 139.5(6) . . ? F13' P10 F10 133.1(6) . . ? F15' P10 F10 83.6(3) . . ? F14 P10 F10 93.0(3) . . ? F11 P10 F10 89.3(3) . . ? F11' P10 F10 92.3(3) . . ? F13 P10 F10 90.9(3) . . ? F12 P10 F10 179.5(4) . . ? F10' P10 F14' 87.8(10) . . ? F12' P10 F14' 85.4(9) . . ? F13' P10 F14' 172.6(10) . . ? F15' P10 F14' 89.7(4) . . ? F14 P10 F14' 66.0(6) . . ? F11 P10 F14' 51.0(5) . . ? F11' P10 F14' 88.7(7) . . ? F13 P10 F14' 120.5(6) . . ? F12 P10 F14' 125.4(9) . . ? F10 P10 F14' 54.2(7) . . ? F10' P10 F15 65.9(8) . . ? F12' P10 F15 121.4(6) . . ? F13' P10 F15 53.9(4) . . ? F15' P10 F15 51.4(4) . . ? F14 P10 F15 88.3(6) . . ? F11 P10 F15 174.2(6) . . ? F11' P10 F15 127.8(9) . . ? F13 P10 F15 86.6(5) . . ? F12 P10 F15 91.8(5) . . ? F10 P10 F15 88.4(3) . . ? F14' P10 F15 130.7(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.421 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.061 # Attachment 'JS32.CIF' data_js32 _database_code_depnum_ccdc_archive 'CCDC 802646' #TrackingRef 'JS32.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H32 Cu N2 P2, F6 P' _chemical_formula_sum 'C40 H32 Cu F6 N2 P3' _chemical_formula_weight 811.14 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 16.487(3) _cell_length_b 11.005(2) _cell_length_c 20.886(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.93(3) _cell_angle_gamma 90.00 _cell_volume 3661.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8579 _exptl_absorpt_correction_T_max 0.8579 _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 50120 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 28.00 _reflns_number_total 8820 _reflns_number_gt 7919 _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^)+(0.0344P)^2^+2.8482P] 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 8820 _refine_ls_number_parameters 506 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.265811(14) 0.20756(2) 0.127761(10) 0.02241(6) Uani 1 1 d . . . P1 P 0.15121(3) 0.29310(5) 0.06363(2) 0.02380(10) Uani 1 1 d . . . P2 P 0.34939(3) 0.33874(4) 0.09659(2) 0.02203(10) Uani 1 1 d . . . C1 C 0.19071(11) 0.42203(16) 0.02557(8) 0.0220(3) Uani 1 1 d . . . C2 C 0.27731(11) 0.44323(16) 0.04093(8) 0.0231(3) Uani 1 1 d . . . C3 C 0.30779(13) 0.54090(18) 0.01185(10) 0.0317(4) Uani 1 1 d . . . H3A H 0.3666 0.5548 0.0218 0.038 Uiso 1 1 calc R . . C4 C 0.25376(14) 0.61799(19) -0.03128(10) 0.0349(4) Uani 1 1 d . . . H4A H 0.2754 0.6844 -0.0508 0.042 Uiso 1 1 calc R . . C5 C 0.16812(14) 0.59806(18) -0.04583(9) 0.0321(4) Uani 1 1 d . . . H5A H 0.1308 0.6518 -0.0748 0.038 Uiso 1 1 calc R . . C6 C 0.13688(12) 0.50054(18) -0.01849(9) 0.0275(4) Uani 1 1 d . . . H6A H 0.0781 0.4863 -0.0296 0.033 Uiso 1 1 calc R . . C7 C 0.08845(11) 0.3613(2) 0.11428(9) 0.0314(4) Uani 1 1 d . . . C8 C 0.04348(14) 0.2826(3) 0.14478(12) 0.0470(6) Uani 1 1 d . . . H8A H 0.0410 0.1983 0.1349 0.056 Uiso 1 1 calc R . . C9 C 0.00195(15) 0.3293(4) 0.19023(12) 0.0656(10) Uani 1 1 d . . . H9A H -0.0287 0.2762 0.2112 0.079 Uiso 1 1 calc R . . C10 C 0.00527(18) 0.4510(4) 0.20463(13) 0.0708(11) Uani 1 1 d . . . H10A H -0.0231 0.4820 0.2354 0.085 Uiso 1 1 calc R . . C11 C 0.04910(18) 0.5271(3) 0.17496(13) 0.0627(9) Uani 1 1 d . . . H11A H 0.0510 0.6114 0.1850 0.075 Uiso 1 1 calc R . . C12 C 0.09144(15) 0.4834(3) 0.12997(11) 0.0424(5) Uani 1 1 d . . . H12A H 0.1225 0.5377 0.1100 0.051 Uiso 1 1 calc R . . C13 C 0.07593(12) 0.21827(18) -0.00428(9) 0.0279(4) Uani 1 1 d . . . C14 C 0.10542(14) 0.1276(2) -0.03864(13) 0.0445(6) Uani 1 1 d . . . H14A H 0.1634 0.1076 -0.0270 0.053 Uiso 1 1 calc R . . C15 C 0.05071(18) 0.0661(3) -0.08988(15) 0.0602(8) Uani 1 1 d . . . H15A H 0.0714 0.0050 -0.1137 0.072 Uiso 1 1 calc R . . C16 C -0.03375(17) 0.0937(3) -0.10632(14) 0.0555(7) Uani 1 1 d . . . H16A H -0.0713 0.0517 -0.1415 0.067 Uiso 1 1 calc R . . C17 C -0.06337(15) 0.1814(3) -0.07192(14) 0.0530(7) Uani 1 1 d . . . H17A H -0.1217 0.1993 -0.0829 0.064 Uiso 1 1 calc R . . C18 C -0.00895(14) 0.2442(2) -0.02123(12) 0.0413(5) Uani 1 1 d . . . H18A H -0.0301 0.3055 0.0021 0.050 Uiso 1 1 calc R . . C19 C 0.42263(11) 0.43910(17) 0.15248(9) 0.0268(4) Uani 1 1 d . . . C20 C 0.48782(13) 0.5010(2) 0.13571(11) 0.0366(5) Uani 1 1 d . . . H20A H 0.4983 0.4883 0.0936 0.044 Uiso 1 1 calc R . . C21 C 0.53763(14) 0.5810(2) 0.18036(13) 0.0466(6) Uani 1 1 d . . . H21A H 0.5816 0.6238 0.1684 0.056 Uiso 1 1 calc R . . C22 C 0.52353(15) 0.5988(2) 0.24189(13) 0.0486(6) Uani 1 1 d . . . H22A H 0.5578 0.6536 0.2723 0.058 Uiso 1 1 calc R . . C23 C 0.45981(15) 0.5373(2) 0.25924(12) 0.0462(6) Uani 1 1 d . . . H23A H 0.4502 0.5496 0.3017 0.055 Uiso 1 1 calc R . . C24 C 0.40941(13) 0.4571(2) 0.21488(10) 0.0346(4) Uani 1 1 d . . . H24A H 0.3657 0.4144 0.2273 0.042 Uiso 1 1 calc R . . C25 C 0.40683(12) 0.27373(17) 0.04156(9) 0.0270(4) Uani 1 1 d . . . C26 C 0.36557(14) 0.2523(2) -0.02446(10) 0.0357(4) Uani 1 1 d . . . H26A H 0.3099 0.2812 -0.0415 0.043 Uiso 1 1 calc R . . C27 C 0.40449(16) 0.1897(2) -0.06547(12) 0.0461(6) Uani 1 1 d . . . H27A H 0.3755 0.1759 -0.1105 0.055 Uiso 1 1 calc R . . C28 C 0.48510(17) 0.1473(3) -0.04143(14) 0.0517(6) Uani 1 1 d . . . H28A H 0.5116 0.1034 -0.0696 0.062 Uiso 1 1 calc R . . C29 C 0.52722(16) 0.1685(3) 0.02347(14) 0.0527(7) Uani 1 1 d . . . H29A H 0.5833 0.1405 0.0398 0.063 Uiso 1 1 calc R . . C30 C 0.48856(14) 0.2305(2) 0.06529(11) 0.0393(5) Uani 1 1 d . . . H30A H 0.5178 0.2435 0.1103 0.047 Uiso 1 1 calc R . . N1 N 0.24898(10) 0.17477(14) 0.21890(7) 0.0240(3) Uani 1 1 d . . . N2 N 0.28752(10) 0.02743(15) 0.13127(8) 0.0277(3) Uani 1 1 d . . . C31 C 0.22444(13) 0.25374(19) 0.25829(9) 0.0291(4) Uani 1 1 d . . . H31A H 0.2232 0.3376 0.2473 0.035 Uiso 1 1 calc R . . C32 C 0.20066(15) 0.2195(2) 0.31463(10) 0.0388(5) Uani 1 1 d . . . H32A H 0.1832 0.2781 0.3417 0.047 Uiso 1 1 calc R . . C33 C 0.20312(18) 0.0979(3) 0.33003(12) 0.0480(6) Uani 1 1 d . . . H33A H 0.1871 0.0713 0.3683 0.058 Uiso 1 1 calc R . . C34 C 0.22888(16) 0.0143(2) 0.28997(11) 0.0419(5) Uani 1 1 d . . . H34A H 0.2309 -0.0698 0.3004 0.050 Uiso 1 1 calc R . . C35 C 0.25186(12) 0.05542(18) 0.23415(9) 0.0275(4) Uani 1 1 d . . . C36 C 0.27890(12) -0.02573(17) 0.18729(10) 0.0291(4) Uani 1 1 d . . . C37 C 0.29547(16) -0.1485(2) 0.19942(13) 0.0441(5) Uani 1 1 d . . . H37A H 0.2902 -0.1844 0.2395 0.053 Uiso 1 1 calc R . . C38 C 0.31965(19) -0.2175(2) 0.15251(16) 0.0542(7) Uani 1 1 d . . . H38A H 0.3307 -0.3018 0.1597 0.065 Uiso 1 1 calc R . . C39 C 0.32763(17) -0.1635(2) 0.09528(14) 0.0485(6) Uani 1 1 d . . . H39A H 0.3440 -0.2098 0.0623 0.058 Uiso 1 1 calc R . . C40 C 0.31138(14) -0.0408(2) 0.08647(12) 0.0379(5) Uani 1 1 d . . . H40A H 0.3174 -0.0034 0.0470 0.045 Uiso 1 1 calc R . . P10 P 0.24476(4) -0.39310(5) 0.33419(3) 0.03982(14) Uani 1 1 d . . . F10 F 0.31328(12) -0.28892(16) 0.34602(8) 0.0667(5) Uani 1 1 d . A . F11 F 0.17540(14) -0.49571(19) 0.32071(10) 0.0794(6) Uani 1 1 d . A . F12 F 0.1769(2) -0.2958(4) 0.3275(2) 0.0994(15) Uani 0.851(5) 1 d P A 1 F13 F 0.23822(16) -0.3895(2) 0.25616(9) 0.0710(8) Uani 0.851(5) 1 d P A 1 F14 F 0.31665(19) -0.4926(2) 0.33919(16) 0.0814(9) Uani 0.851(5) 1 d P A 1 F15 F 0.2572(2) -0.4022(3) 0.41188(12) 0.0612(7) Uani 0.851(5) 1 d PU A 1 F12' F 0.1761(12) -0.2937(17) 0.2927(13) 0.101(8) Uani 0.149(5) 1 d PU A 2 F13' F 0.2700(13) -0.4643(16) 0.2999(10) 0.103(6) Uani 0.149(5) 1 d PU A 2 F14' F 0.2654(17) -0.462(2) 0.3981(14) 0.131(10) Uani 0.149(5) 1 d PU A 2 F15' F 0.1895(19) -0.346(2) 0.3861(14) 0.128(9) Uani 0.149(5) 1 d PU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02289(11) 0.02154(11) 0.02188(11) 0.00434(8) 0.00411(8) 0.00236(8) P1 0.0181(2) 0.0288(2) 0.0233(2) 0.00369(18) 0.00331(16) 0.00260(17) P2 0.0184(2) 0.0236(2) 0.0219(2) 0.00416(17) 0.00125(16) 0.00127(16) C1 0.0228(8) 0.0236(8) 0.0185(7) 0.0003(6) 0.0033(6) 0.0041(7) C2 0.0242(8) 0.0221(8) 0.0210(8) 0.0018(6) 0.0021(6) 0.0033(7) C3 0.0296(9) 0.0276(9) 0.0339(10) 0.0058(8) 0.0007(8) -0.0028(8) C4 0.0448(12) 0.0244(9) 0.0308(10) 0.0072(8) 0.0011(9) -0.0016(8) C5 0.0407(11) 0.0272(9) 0.0241(9) 0.0036(7) 0.0008(8) 0.0117(8) C6 0.0260(9) 0.0321(10) 0.0220(8) 0.0002(7) 0.0017(7) 0.0091(7) C7 0.0185(8) 0.0529(13) 0.0217(8) 0.0024(8) 0.0033(7) 0.0064(8) C8 0.0262(10) 0.0784(19) 0.0363(11) 0.0128(12) 0.0075(9) 0.0002(11) C9 0.0252(11) 0.141(3) 0.0318(12) 0.0175(16) 0.0092(9) 0.0031(15) C10 0.0420(14) 0.140(4) 0.0315(12) -0.0127(17) 0.0118(11) 0.0206(18) C11 0.0548(16) 0.094(2) 0.0384(13) -0.0230(14) 0.0109(12) 0.0199(16) C12 0.0373(11) 0.0602(15) 0.0287(10) -0.0083(10) 0.0067(8) 0.0100(11) C13 0.0230(8) 0.0309(10) 0.0285(9) 0.0010(7) 0.0044(7) -0.0016(7) C14 0.0276(10) 0.0539(14) 0.0522(13) -0.0169(11) 0.0104(9) -0.0012(10) C15 0.0457(14) 0.0701(19) 0.0642(17) -0.0366(15) 0.0133(13) -0.0054(13) C16 0.0424(13) 0.0633(17) 0.0540(15) -0.0231(13) 0.0000(11) -0.0116(12) C17 0.0282(11) 0.0600(16) 0.0613(16) -0.0164(13) -0.0061(11) 0.0016(11) C18 0.0260(10) 0.0433(12) 0.0485(12) -0.0107(10) -0.0014(9) 0.0052(9) C19 0.0214(8) 0.0268(9) 0.0288(9) 0.0037(7) -0.0001(7) 0.0009(7) C20 0.0267(10) 0.0443(12) 0.0347(10) 0.0054(9) 0.0003(8) -0.0068(9) C21 0.0287(11) 0.0468(13) 0.0561(14) 0.0061(11) -0.0040(10) -0.0119(10) C22 0.0365(12) 0.0422(13) 0.0553(14) -0.0121(11) -0.0097(10) -0.0041(10) C23 0.0404(12) 0.0522(14) 0.0407(12) -0.0153(11) 0.0009(10) -0.0009(11) C24 0.0301(10) 0.0384(11) 0.0331(10) -0.0036(8) 0.0043(8) -0.0012(8) C25 0.0257(9) 0.0263(9) 0.0287(9) 0.0031(7) 0.0066(7) 0.0022(7) C26 0.0310(10) 0.0418(11) 0.0317(10) -0.0031(9) 0.0035(8) 0.0038(9) C27 0.0474(13) 0.0536(15) 0.0366(11) -0.0098(10) 0.0097(10) 0.0042(11) C28 0.0496(14) 0.0584(16) 0.0515(14) -0.0110(12) 0.0209(12) 0.0122(12) C29 0.0358(12) 0.0652(17) 0.0567(15) -0.0037(13) 0.0111(11) 0.0205(12) C30 0.0300(10) 0.0481(13) 0.0363(11) 0.0023(9) 0.0022(8) 0.0125(9) N1 0.0241(7) 0.0241(7) 0.0216(7) 0.0030(6) 0.0021(6) -0.0017(6) N2 0.0268(8) 0.0222(7) 0.0325(8) -0.0009(6) 0.0045(6) 0.0014(6) C31 0.0317(9) 0.0310(9) 0.0233(8) 0.0002(7) 0.0048(7) -0.0012(8) C32 0.0456(12) 0.0471(13) 0.0252(9) -0.0015(9) 0.0119(9) -0.0033(10) C33 0.0627(16) 0.0539(15) 0.0312(11) 0.0089(10) 0.0194(11) -0.0098(12) C34 0.0539(14) 0.0353(11) 0.0368(11) 0.0114(9) 0.0122(10) -0.0083(10) C35 0.0270(9) 0.0257(9) 0.0261(9) 0.0057(7) 0.0002(7) -0.0035(7) C36 0.0273(9) 0.0231(9) 0.0330(9) 0.0028(7) 0.0005(7) -0.0022(7) C37 0.0514(14) 0.0247(10) 0.0515(13) 0.0075(9) 0.0049(11) 0.0017(9) C38 0.0589(16) 0.0230(11) 0.0768(19) -0.0010(11) 0.0101(14) 0.0067(10) C39 0.0482(14) 0.0321(11) 0.0662(16) -0.0138(11) 0.0168(12) 0.0056(10) C40 0.0394(11) 0.0325(11) 0.0423(11) -0.0071(9) 0.0118(9) 0.0032(9) P10 0.0455(3) 0.0270(3) 0.0455(3) -0.0021(2) 0.0089(3) -0.0025(2) F10 0.0775(12) 0.0555(10) 0.0554(9) 0.0060(8) -0.0040(8) -0.0306(9) F11 0.1010(15) 0.0719(12) 0.0732(12) -0.0230(10) 0.0367(11) -0.0467(11) F12 0.077(2) 0.093(2) 0.113(3) -0.019(2) -0.0019(19) 0.0515(18) F13 0.0918(17) 0.0779(16) 0.0387(10) -0.0004(10) 0.0084(10) -0.0383(13) F14 0.0849(18) 0.0627(15) 0.101(2) 0.0070(14) 0.0316(16) 0.0316(13) F15 0.0830(18) 0.0631(16) 0.0414(11) -0.0121(11) 0.0232(11) -0.0239(15) F12' 0.055(8) 0.061(9) 0.170(17) 0.062(11) 0.001(10) -0.025(7) F13' 0.120(10) 0.081(8) 0.105(9) -0.062(7) 0.025(7) 0.030(7) F14' 0.119(14) 0.111(14) 0.130(15) 0.064(12) -0.027(11) -0.024(12) F15' 0.168(19) 0.110(14) 0.142(17) -0.080(13) 0.103(15) -0.089(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.0125(17) . ? Cu1 N1 2.0255(16) . ? Cu1 P2 2.2065(6) . ? Cu1 P1 2.2240(8) . ? P1 C7 1.821(2) . ? P1 C13 1.823(2) . ? P1 C1 1.8265(19) . ? P2 C25 1.814(2) . ? P2 C19 1.820(2) . ? P2 C2 1.8368(18) . ? C1 C6 1.400(2) . ? C1 C2 1.400(2) . ? C2 C3 1.391(3) . ? C3 C4 1.382(3) . ? C3 H3A 0.9500 . ? C4 C5 1.383(3) . ? C4 H4A 0.9500 . ? C5 C6 1.377(3) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.381(4) . ? C7 C8 1.396(3) . ? C8 C9 1.403(4) . ? C8 H8A 0.9500 . ? C9 C10 1.370(5) . ? C9 H9A 0.9500 . ? C10 C11 1.356(5) . ? C10 H10A 0.9500 . ? C11 C12 1.393(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.382(3) . ? C13 C14 1.388(3) . ? C14 C15 1.386(3) . ? C14 H14A 0.9500 . ? C15 C16 1.379(4) . ? C15 H15A 0.9500 . ? C16 C17 1.366(4) . ? C16 H16A 0.9500 . ? C17 C18 1.383(3) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C24 1.390(3) . ? C19 C20 1.391(3) . ? C20 C21 1.388(3) . ? C20 H20A 0.9500 . ? C21 C22 1.378(4) . ? C21 H21A 0.9500 . ? C22 C23 1.375(4) . ? C22 H22A 0.9500 . ? C23 C24 1.389(3) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.392(3) . ? C25 C30 1.394(3) . ? C26 C27 1.380(3) . ? C26 H26A 0.9500 . ? C27 C28 1.376(4) . ? C27 H27A 0.9500 . ? C28 C29 1.374(4) . ? C28 H28A 0.9500 . ? C29 C30 1.386(3) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? N1 C31 1.330(3) . ? N1 C35 1.349(2) . ? N2 C40 1.336(3) . ? N2 C36 1.348(3) . ? C31 C32 1.385(3) . ? C31 H31A 0.9500 . ? C32 C33 1.374(4) . ? C32 H32A 0.9500 . ? C33 C34 1.382(4) . ? C33 H33A 0.9500 . ? C34 C35 1.391(3) . ? C34 H34A 0.9500 . ? C35 C36 1.476(3) . ? C36 C37 1.389(3) . ? C37 C38 1.377(4) . ? C37 H37A 0.9500 . ? C38 C39 1.371(4) . ? C38 H38A 0.9500 . ? C39 C40 1.380(3) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? P10 F13' 1.206(12) . ? P10 F14' 1.49(2) . ? P10 F12 1.529(3) . ? P10 F11 1.5799(18) . ? P10 F10 1.5837(17) . ? P10 F15 1.585(2) . ? P10 F14 1.597(2) . ? P10 F13 1.606(2) . ? P10 F12' 1.650(19) . ? P10 F15' 1.669(18) . ? F11 F13' 1.76(2) . ? F14' F15' 1.76(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N1 81.74(7) . . ? N2 Cu1 P2 122.44(5) . . ? N1 Cu1 P2 129.87(5) . . ? N2 Cu1 P1 123.67(5) . . ? N1 Cu1 P1 109.91(5) . . ? P2 Cu1 P1 92.50(2) . . ? C7 P1 C13 105.26(9) . . ? C7 P1 C1 104.62(10) . . ? C13 P1 C1 105.07(8) . . ? C7 P1 Cu1 110.25(6) . . ? C13 P1 Cu1 125.44(7) . . ? C1 P1 Cu1 104.36(6) . . ? C25 P2 C19 106.10(9) . . ? C25 P2 C2 101.78(8) . . ? C19 P2 C2 103.89(9) . . ? C25 P2 Cu1 113.37(7) . . ? C19 P2 Cu1 124.69(7) . . ? C2 P2 Cu1 104.18(6) . . ? C6 C1 C2 118.95(17) . . ? C6 C1 P1 121.92(14) . . ? C2 C1 P1 119.12(13) . . ? C3 C2 C1 119.39(16) . . ? C3 C2 P2 120.84(14) . . ? C1 C2 P2 119.73(14) . . ? C4 C3 C2 120.95(19) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C3 C4 C5 119.72(19) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C6 C5 C4 120.17(18) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C5 C6 C1 120.81(18) . . ? C5 C6 H6A 119.6 . . ? C1 C6 H6A 119.6 . . ? C12 C7 C8 119.1(2) . . ? C12 C7 P1 123.22(17) . . ? C8 C7 P1 117.24(19) . . ? C7 C8 C9 119.4(3) . . ? C7 C8 H8A 120.3 . . ? C9 C8 H8A 120.3 . . ? C10 C9 C8 120.5(3) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.7 . . ? C11 C10 C9 119.9(3) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.9(3) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C7 C12 C11 120.2(3) . . ? C7 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C18 C13 C14 118.83(19) . . ? C18 C13 P1 123.22(16) . . ? C14 C13 P1 117.90(15) . . ? C15 C14 C13 120.4(2) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C16 C15 C14 119.9(2) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C17 C16 C15 120.0(2) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C18 120.4(2) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C13 C18 C17 120.5(2) . . ? C13 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C24 C19 C20 118.97(19) . . ? C24 C19 P2 116.71(15) . . ? C20 C19 P2 124.27(16) . . ? C21 C20 C19 120.2(2) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C22 C21 C20 120.3(2) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C23 C22 C21 120.0(2) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 120.2(2) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C23 C24 C19 120.3(2) . . ? C23 C24 H24A 119.9 . . ? C19 C24 H24A 119.9 . . ? C26 C25 C30 118.37(19) . . ? C26 C25 P2 119.54(15) . . ? C30 C25 P2 121.60(16) . . ? C27 C26 C25 120.9(2) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C28 C27 C26 120.2(2) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C29 C28 C27 119.8(2) . . ? C29 C28 H28A 120.1 . . ? C27 C28 H28A 120.1 . . ? C28 C29 C30 120.5(2) . . ? C28 C29 H29A 119.7 . . ? C30 C29 H29A 119.7 . . ? C29 C30 C25 120.2(2) . . ? C29 C30 H30A 119.9 . . ? C25 C30 H30A 119.9 . . ? C31 N1 C35 119.20(17) . . ? C31 N1 Cu1 127.04(13) . . ? C35 N1 Cu1 112.97(13) . . ? C40 N2 C36 118.68(18) . . ? C40 N2 Cu1 127.60(15) . . ? C36 N2 Cu1 113.67(13) . . ? N1 C31 C32 123.1(2) . . ? N1 C31 H31A 118.5 . . ? C32 C31 H31A 118.5 . . ? C33 C32 C31 117.8(2) . . ? C33 C32 H32A 121.1 . . ? C31 C32 H32A 121.1 . . ? C32 C33 C34 120.1(2) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C33 C34 C35 118.9(2) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? N1 C35 C34 120.9(2) . . ? N1 C35 C36 115.51(17) . . ? C34 C35 C36 123.58(19) . . ? N2 C36 C37 121.4(2) . . ? N2 C36 C35 115.48(17) . . ? C37 C36 C35 123.1(2) . . ? C38 C37 C36 119.1(2) . . ? C38 C37 H37A 120.5 . . ? C36 C37 H37A 120.5 . . ? C39 C38 C37 119.5(2) . . ? C39 C38 H38A 120.3 . . ? C37 C38 H38A 120.3 . . ? C38 C39 C40 118.8(2) . . ? C38 C39 H39A 120.6 . . ? C40 C39 H39A 120.6 . . ? N2 C40 C39 122.6(2) . . ? N2 C40 H40A 118.7 . . ? C39 C40 H40A 118.7 . . ? F13' P10 F14' 99.8(17) . . ? F13' P10 F12 139.2(11) . . ? F14' P10 F12 115.4(14) . . ? F13' P10 F11 77.0(10) . . ? F14' P10 F11 77.7(10) . . ? F12 P10 F11 90.3(2) . . ? F13' P10 F10 102.8(10) . . ? F14' P10 F10 103.7(10) . . ? F12 P10 F10 89.01(19) . . ? F11 P10 F10 178.64(12) . . ? F13' P10 F15 126.4(11) . . ? F12 P10 F15 92.1(2) . . ? F11 P10 F15 91.95(13) . . ? F10 P10 F15 89.26(12) . . ? F14' P10 F14 66.5(14) . . ? F12 P10 F14 178.0(2) . . ? F11 P10 F14 90.72(14) . . ? F10 P10 F14 89.91(14) . . ? F15 P10 F14 89.53(17) . . ? F13' P10 F13 49.9(11) . . ? F14' P10 F13 149.3(14) . . ? F12 P10 F13 91.9(2) . . ? F11 P10 F13 88.88(11) . . ? F10 P10 F13 89.96(10) . . ? F15 P10 F13 175.88(18) . . ? F14 P10 F13 86.42(15) . . ? F13' P10 F12' 114.5(15) . . ? F14' P10 F12' 140.4(16) . . ? F11 P10 F12' 90.7(5) . . ? F10 P10 F12' 88.1(5) . . ? F15 P10 F12' 118.0(10) . . ? F14 P10 F12' 152.4(10) . . ? F13 P10 F12' 66.0(10) . . ? F13' P10 F15' 156.7(12) . . ? F14' P10 F15' 67.2(16) . . ? F12 P10 F15' 48.1(13) . . ? F11 P10 F15' 81.2(5) . . ? F10 P10 F15' 99.2(5) . . ? F15 P10 F15' 45.8(13) . . ? F14 P10 F15' 133.7(13) . . ? F13 P10 F15' 138.3(13) . . ? F12' P10 F15' 73.7(15) . . ? P10 F13' F11 61.1(8) . . ? P10 F14' F15' 61.1(10) . . ? P10 F15' F14' 51.6(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.463 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.053 # Attachment 'JS58.CIF' data_js58 _database_code_depnum_ccdc_archive 'CCDC 802647' #TrackingRef 'JS58.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H36 Cu N2 O P2, F6 P, C H2 Cl2' _chemical_formula_sum 'C49 H38 Cl2 Cu F6 N2 O P3' _chemical_formula_weight 1012.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 13.4327(10) _cell_length_b 25.218(2) _cell_length_c 13.6483(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.808(5) _cell_angle_gamma 90.00 _cell_volume 4448.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18770 _cell_measurement_theta_min 5.52 _cell_measurement_theta_max 66.78 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 0.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7985 _exptl_absorpt_correction_T_max 0.9256 _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 77797 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 29.00 _reflns_number_total 11763 _reflns_number_gt 10959 _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^)+(0.0325P)^2^+3.1949P] 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 11763 _refine_ls_number_parameters 614 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.003 _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 0.235952(13) 0.076656(7) 0.876950(12) 0.01601(5) Uani 1 1 d . . . P1 P 0.14708(3) 0.043652(14) 0.72934(3) 0.01473(7) Uani 1 1 d . . . P2 P 0.19578(3) 0.159218(14) 0.92339(3) 0.01624(7) Uani 1 1 d . . . O1 O 0.00268(8) 0.10219(4) 0.80644(8) 0.01799(19) Uani 1 1 d . . . C1 C 0.05309(10) 0.09049(6) 0.65619(10) 0.0172(2) Uani 1 1 d . . . C2 C -0.00870(10) 0.11772(6) 0.70649(11) 0.0175(2) Uani 1 1 d . . . C3 C -0.07949(12) 0.15550(6) 0.65724(12) 0.0250(3) Uani 1 1 d . . . H3A H -0.1195 0.1746 0.6930 0.030 Uiso 1 1 calc R . . C4 C -0.09093(13) 0.16500(7) 0.55478(13) 0.0291(3) Uani 1 1 d . . . H4A H -0.1399 0.1905 0.5200 0.035 Uiso 1 1 calc R . . C5 C -0.03238(13) 0.13801(7) 0.50249(12) 0.0271(3) Uani 1 1 d . . . H5A H -0.0416 0.1446 0.4321 0.033 Uiso 1 1 calc R . . C6 C 0.04022(12) 0.10109(6) 0.55343(11) 0.0217(3) Uani 1 1 d . . . H6A H 0.0815 0.0829 0.5177 0.026 Uiso 1 1 calc R . . C7 C 0.06493(11) 0.16877(6) 0.93471(11) 0.0182(3) Uani 1 1 d . . . C8 C -0.01691(11) 0.13984(6) 0.87345(11) 0.0183(3) Uani 1 1 d . . . C9 C -0.11743(11) 0.14565(6) 0.87981(13) 0.0241(3) Uani 1 1 d . . . H9A H -0.1716 0.1247 0.8386 0.029 Uiso 1 1 calc R . . C10 C -0.13780(12) 0.18239(7) 0.94716(13) 0.0271(3) Uani 1 1 d . . . H10A H -0.2066 0.1871 0.9515 0.033 Uiso 1 1 calc R . . C11 C -0.05833(13) 0.21226(7) 1.00827(13) 0.0265(3) Uani 1 1 d . . . H11A H -0.0729 0.2378 1.0537 0.032 Uiso 1 1 calc R . . C12 C 0.04207(12) 0.20500(6) 1.00330(12) 0.0234(3) Uani 1 1 d . . . H12A H 0.0964 0.2249 1.0470 0.028 Uiso 1 1 calc R . . C13 C 0.06688(11) -0.01337(6) 0.73892(10) 0.0172(2) Uani 1 1 d . . . C14 C -0.03034(12) -0.02175(7) 0.67110(11) 0.0229(3) Uani 1 1 d . . . H14A H -0.0578 0.0034 0.6189 0.027 Uiso 1 1 calc R . . C15 C -0.08705(13) -0.06672(7) 0.67966(13) 0.0299(3) Uani 1 1 d . . . H15A H -0.1532 -0.0722 0.6334 0.036 Uiso 1 1 calc R . . C16 C -0.04766(15) -0.10352(7) 0.75518(14) 0.0323(4) Uani 1 1 d . . . H16A H -0.0861 -0.1346 0.7599 0.039 Uiso 1 1 calc R . . C17 C 0.04761(15) -0.09521(7) 0.82388(14) 0.0308(3) Uani 1 1 d . . . H17A H 0.0741 -0.1202 0.8766 0.037 Uiso 1 1 calc R . . C18 C 0.10470(12) -0.05031(6) 0.81599(12) 0.0231(3) Uani 1 1 d . . . H18A H 0.1701 -0.0447 0.8635 0.028 Uiso 1 1 calc R . . C19 C 0.21620(10) 0.02177(6) 0.63888(10) 0.0173(2) Uani 1 1 d . . . C20 C 0.20287(12) -0.02815(6) 0.59342(12) 0.0232(3) Uani 1 1 d . . . H20A H 0.1535 -0.0520 0.6068 0.028 Uiso 1 1 calc R . . C21 C 0.26165(14) -0.04315(8) 0.52844(13) 0.0305(3) Uani 1 1 d . . . H21A H 0.2531 -0.0774 0.4983 0.037 Uiso 1 1 calc R . . C22 C 0.33237(13) -0.00829(8) 0.50771(13) 0.0314(4) Uani 1 1 d . . . H22A H 0.3723 -0.0186 0.4632 0.038 Uiso 1 1 calc R . . C23 C 0.34554(13) 0.04162(8) 0.55138(13) 0.0288(3) Uani 1 1 d . . . H23A H 0.3935 0.0657 0.5359 0.035 Uiso 1 1 calc R . . C24 C 0.28869(12) 0.05646(6) 0.61782(12) 0.0227(3) Uani 1 1 d . . . H24A H 0.2991 0.0904 0.6492 0.027 Uiso 1 1 calc R . . C25 C 0.27660(11) 0.17079(6) 1.05251(11) 0.0186(3) Uani 1 1 d . . . C26 C 0.25191(13) 0.14699(7) 1.13492(12) 0.0264(3) Uani 1 1 d . . . H26A H 0.1889 0.1279 1.1244 0.032 Uiso 1 1 calc R . . C27 C 0.31829(16) 0.15085(8) 1.23211(13) 0.0341(4) Uani 1 1 d . . . H27A H 0.3002 0.1348 1.2878 0.041 Uiso 1 1 calc R . . C28 C 0.41060(16) 0.17802(9) 1.24822(14) 0.0395(4) Uani 1 1 d . . . H28A H 0.4557 0.1810 1.3150 0.047 Uiso 1 1 calc R . . C29 C 0.43692(15) 0.20081(8) 1.16654(15) 0.0377(4) Uani 1 1 d . . . H29A H 0.5008 0.2192 1.1773 0.045 Uiso 1 1 calc R . . C30 C 0.37063(12) 0.19705(7) 1.06888(13) 0.0267(3) Uani 1 1 d . . . H30A H 0.3897 0.2125 1.0131 0.032 Uiso 1 1 calc R . . C31 C 0.22029(11) 0.21738(6) 0.85432(11) 0.0216(3) Uani 1 1 d . . . C32 C 0.18279(13) 0.26756(7) 0.86613(14) 0.0288(3) Uani 1 1 d . . . H32A H 0.1387 0.2723 0.9093 0.035 Uiso 1 1 calc R . . C33 C 0.20889(16) 0.31078(8) 0.81561(16) 0.0386(4) Uani 1 1 d . . . H33A H 0.1816 0.3448 0.8229 0.046 Uiso 1 1 calc R . . C34 C 0.27459(19) 0.30413(10) 0.75470(18) 0.0486(5) Uani 1 1 d . . . H34A H 0.2931 0.3337 0.7204 0.058 Uiso 1 1 calc R . . C35 C 0.3133(2) 0.25497(12) 0.7434(2) 0.0599(7) Uani 1 1 d . . . H35A H 0.3594 0.2507 0.7022 0.072 Uiso 1 1 calc R . . C36 C 0.28544(18) 0.21111(9) 0.79220(17) 0.0429(5) Uani 1 1 d . . . H36A H 0.3112 0.1769 0.7828 0.051 Uiso 1 1 calc R . . N1 N 0.22977(9) 0.03546(5) 1.00638(9) 0.0182(2) Uani 1 1 d . . . N2 N 0.39240(9) 0.07143(5) 0.94720(9) 0.0173(2) Uani 1 1 d . . . C37 C 0.14865(12) 0.01838(7) 1.03501(12) 0.0236(3) Uani 1 1 d . . . H37A H 0.0820 0.0216 0.9884 0.028 Uiso 1 1 calc R . . C38 C 0.15623(13) -0.00411(7) 1.13016(13) 0.0274(3) Uani 1 1 d . . . H38A H 0.0961 -0.0162 1.1472 0.033 Uiso 1 1 calc R . . C39 C 0.25160(14) -0.00853(7) 1.19857(12) 0.0278(3) Uani 1 1 d . . . H39A H 0.2584 -0.0242 1.2634 0.033 Uiso 1 1 calc R . . C40 C 0.33920(12) 0.01020(6) 1.17225(11) 0.0227(3) Uani 1 1 d . . . C41 C 0.32402(11) 0.03179(6) 1.07419(10) 0.0172(2) Uani 1 1 d . . . C42 C 0.41069(10) 0.05201(6) 1.04330(11) 0.0172(2) Uani 1 1 d . . . C43 C 0.50931(11) 0.05143(6) 1.11298(12) 0.0226(3) Uani 1 1 d . . . C44 C 0.59122(12) 0.07209(7) 1.07997(14) 0.0290(3) Uani 1 1 d . . . H44A H 0.6591 0.0730 1.1248 0.035 Uiso 1 1 calc R . . C45 C 0.57307(12) 0.09098(7) 0.98279(14) 0.0280(3) Uani 1 1 d . . . H45A H 0.6283 0.1047 0.9593 0.034 Uiso 1 1 calc R . . C46 C 0.47230(12) 0.08994(6) 0.91821(12) 0.0223(3) Uani 1 1 d . . . H46A H 0.4607 0.1031 0.8508 0.027 Uiso 1 1 calc R . . C47 C 0.44090(14) 0.00932(8) 1.24016(12) 0.0304(3) Uani 1 1 d . . . H47A H 0.4516 -0.0057 1.3060 0.036 Uiso 1 1 calc R . . C48 C 0.52180(13) 0.02941(8) 1.21243(13) 0.0307(4) Uani 1 1 d . . . H48A H 0.5885 0.0290 1.2596 0.037 Uiso 1 1 calc R . . P10 P 0.58539(4) 0.15614(2) 0.66897(4) 0.03316(10) Uani 1 1 d . . . F10 F 0.53071(16) 0.16586(7) 0.55249(11) 0.0684(5) Uani 1 1 d . A . F11 F 0.63835(11) 0.14698(7) 0.78794(11) 0.0598(4) Uani 1 1 d . A . F12 F 0.6834(3) 0.1728(4) 0.6438(5) 0.101(2) Uani 0.551(11) 1 d PU A 1 F13 F 0.5957(7) 0.09656(17) 0.6368(4) 0.0784(17) Uani 0.551(11) 1 d P A 1 F14 F 0.4753(4) 0.1401(3) 0.6857(5) 0.0653(16) Uani 0.551(11) 1 d P A 1 F15 F 0.5594(5) 0.21516(16) 0.6928(4) 0.0672(17) Uani 0.551(11) 1 d PU A 1 F12' F 0.6807(5) 0.1969(3) 0.6749(7) 0.079(2) Uani 0.449(11) 1 d PU A 2 F13' F 0.6662(10) 0.1109(3) 0.6560(4) 0.092(3) Uani 0.449(11) 1 d P A 2 F14' F 0.5049(10) 0.1177(6) 0.6818(8) 0.133(5) Uani 0.449(11) 1 d P A 2 F15' F 0.5290(7) 0.2053(4) 0.6944(6) 0.099(3) Uani 0.449(11) 1 d PU A 2 C100 C -0.3637(2) 0.27414(10) 0.9046(2) 0.0512(5) Uani 1 1 d . . . H10B H -0.4248 0.2955 0.8693 0.061 Uiso 1 1 calc R . . H10C H -0.3407 0.2541 0.8524 0.061 Uiso 1 1 calc R . . Cl1 Cl -0.26429(5) 0.31655(2) 0.96930(5) 0.05101(13) Uani 1 1 d . . . Cl2 Cl -0.39894(5) 0.22967(3) 0.98707(7) 0.06431(19) 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 0.01412(8) 0.01971(9) 0.01307(8) -0.00138(6) 0.00180(6) 0.00042(6) P1 0.01357(15) 0.01683(15) 0.01293(15) -0.00119(11) 0.00217(11) 0.00060(12) P2 0.01410(15) 0.01806(16) 0.01680(16) -0.00252(12) 0.00462(12) -0.00075(12) O1 0.0170(4) 0.0192(5) 0.0173(5) -0.0024(4) 0.0039(4) 0.0021(4) C1 0.0151(6) 0.0175(6) 0.0169(6) -0.0003(5) 0.0010(5) -0.0004(5) C2 0.0144(6) 0.0179(6) 0.0178(6) -0.0010(5) 0.0005(5) -0.0013(5) C3 0.0213(7) 0.0237(7) 0.0266(7) -0.0014(6) 0.0011(6) 0.0061(6) C4 0.0278(8) 0.0247(7) 0.0281(8) 0.0047(6) -0.0039(6) 0.0062(6) C5 0.0308(8) 0.0270(8) 0.0195(7) 0.0050(6) -0.0001(6) 0.0003(6) C6 0.0221(7) 0.0233(7) 0.0178(6) 0.0004(5) 0.0024(5) -0.0006(5) C7 0.0159(6) 0.0189(6) 0.0208(6) -0.0014(5) 0.0071(5) 0.0010(5) C8 0.0168(6) 0.0187(6) 0.0203(6) -0.0021(5) 0.0065(5) 0.0018(5) C9 0.0153(6) 0.0270(7) 0.0305(8) -0.0028(6) 0.0069(6) 0.0007(5) C10 0.0208(7) 0.0295(8) 0.0343(8) -0.0010(6) 0.0133(6) 0.0053(6) C11 0.0278(8) 0.0256(7) 0.0297(8) -0.0043(6) 0.0139(6) 0.0051(6) C12 0.0234(7) 0.0222(7) 0.0254(7) -0.0058(6) 0.0084(6) 0.0007(5) C13 0.0172(6) 0.0191(6) 0.0165(6) -0.0030(5) 0.0065(5) -0.0011(5) C14 0.0208(7) 0.0291(8) 0.0185(6) -0.0028(5) 0.0048(5) -0.0045(6) C15 0.0266(8) 0.0379(9) 0.0278(8) -0.0111(7) 0.0122(6) -0.0126(7) C16 0.0410(10) 0.0277(8) 0.0368(9) -0.0094(7) 0.0250(8) -0.0131(7) C17 0.0433(10) 0.0226(7) 0.0313(8) 0.0032(6) 0.0185(7) -0.0003(7) C18 0.0245(7) 0.0221(7) 0.0236(7) 0.0010(5) 0.0078(6) 0.0023(6) C19 0.0145(6) 0.0228(7) 0.0137(6) -0.0017(5) 0.0022(5) 0.0018(5) C20 0.0213(7) 0.0270(7) 0.0219(7) -0.0059(6) 0.0069(5) -0.0010(6) C21 0.0303(8) 0.0358(9) 0.0268(8) -0.0111(7) 0.0102(6) 0.0029(7) C22 0.0257(8) 0.0495(11) 0.0212(7) -0.0036(7) 0.0102(6) 0.0058(7) C23 0.0221(7) 0.0428(10) 0.0233(7) 0.0027(7) 0.0090(6) -0.0021(7) C24 0.0202(7) 0.0273(7) 0.0210(7) -0.0008(5) 0.0062(5) -0.0008(6) C25 0.0182(6) 0.0187(6) 0.0183(6) -0.0035(5) 0.0039(5) -0.0002(5) C26 0.0282(8) 0.0322(8) 0.0197(7) -0.0041(6) 0.0079(6) -0.0050(6) C27 0.0402(10) 0.0419(10) 0.0192(7) -0.0016(7) 0.0061(7) -0.0016(8) C28 0.0386(10) 0.0472(11) 0.0237(8) -0.0032(7) -0.0070(7) -0.0042(8) C29 0.0282(8) 0.0414(10) 0.0344(9) 0.0007(8) -0.0070(7) -0.0104(7) C30 0.0227(7) 0.0274(8) 0.0263(8) 0.0015(6) 0.0004(6) -0.0053(6) C31 0.0188(6) 0.0255(7) 0.0191(6) 0.0020(5) 0.0027(5) -0.0039(5) C32 0.0262(8) 0.0262(8) 0.0320(8) 0.0029(6) 0.0048(6) -0.0013(6) C33 0.0391(10) 0.0282(9) 0.0421(10) 0.0091(8) 0.0004(8) -0.0050(7) C34 0.0518(13) 0.0478(12) 0.0446(12) 0.0206(10) 0.0105(10) -0.0134(10) C35 0.0714(17) 0.0645(16) 0.0591(15) 0.0194(12) 0.0438(14) -0.0022(13) C36 0.0526(12) 0.0416(11) 0.0451(11) 0.0091(9) 0.0315(10) 0.0047(9) N1 0.0164(5) 0.0229(6) 0.0154(5) -0.0013(4) 0.0044(4) -0.0022(4) N2 0.0150(5) 0.0196(5) 0.0176(5) 0.0001(4) 0.0048(4) 0.0012(4) C37 0.0196(6) 0.0299(8) 0.0223(7) -0.0022(6) 0.0074(5) -0.0046(6) C38 0.0286(8) 0.0314(8) 0.0266(8) 0.0003(6) 0.0149(6) -0.0055(6) C39 0.0352(8) 0.0297(8) 0.0217(7) 0.0060(6) 0.0131(6) 0.0014(7) C40 0.0257(7) 0.0250(7) 0.0178(6) 0.0030(5) 0.0068(5) 0.0046(6) C41 0.0171(6) 0.0186(6) 0.0159(6) -0.0004(5) 0.0045(5) 0.0020(5) C42 0.0153(6) 0.0180(6) 0.0176(6) 0.0000(5) 0.0033(5) 0.0023(5) C43 0.0164(6) 0.0259(7) 0.0234(7) 0.0006(6) 0.0016(5) 0.0044(5) C44 0.0144(6) 0.0335(8) 0.0360(9) 0.0007(7) 0.0017(6) 0.0020(6) C45 0.0159(7) 0.0300(8) 0.0400(9) 0.0018(7) 0.0108(6) -0.0008(6) C46 0.0194(7) 0.0233(7) 0.0263(7) 0.0033(6) 0.0101(6) 0.0004(5) C47 0.0288(8) 0.0412(9) 0.0187(7) 0.0082(6) 0.0026(6) 0.0089(7) C48 0.0224(7) 0.0409(9) 0.0234(7) 0.0056(7) -0.0033(6) 0.0084(7) P10 0.0315(2) 0.0324(2) 0.0364(2) 0.00872(18) 0.01055(18) 0.00100(18) F10 0.1069(14) 0.0602(9) 0.0318(7) 0.0043(6) 0.0081(8) 0.0070(9) F11 0.0462(8) 0.0831(11) 0.0435(7) 0.0196(7) 0.0008(6) 0.0143(7) F12 0.0336(16) 0.182(7) 0.099(3) -0.005(4) 0.0409(19) -0.032(3) F13 0.122(5) 0.0404(19) 0.075(3) 0.0123(16) 0.032(3) 0.042(2) F14 0.0369(16) 0.107(4) 0.056(2) -0.008(2) 0.0209(15) -0.024(2) F15 0.120(4) 0.0300(15) 0.0378(17) -0.0049(11) -0.001(2) -0.006(2) F12' 0.065(3) 0.073(4) 0.092(4) 0.037(3) 0.008(3) -0.027(3) F13' 0.158(8) 0.072(4) 0.050(2) 0.009(2) 0.034(4) 0.075(5) F14' 0.123(8) 0.166(10) 0.083(5) 0.038(6) -0.019(5) -0.121(8) F15' 0.082(4) 0.141(7) 0.072(3) 0.011(4) 0.017(3) 0.093(4) C100 0.0542(13) 0.0400(11) 0.0556(14) 0.0073(10) 0.0085(11) 0.0096(10) Cl1 0.0579(3) 0.0383(3) 0.0606(3) 0.0027(2) 0.0226(3) 0.0007(2) Cl2 0.0572(4) 0.0444(3) 0.1038(6) 0.0097(3) 0.0431(4) 0.0035(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 2.0628(12) . ? Cu1 N1 2.0704(12) . ? Cu1 P1 2.2059(4) . ? Cu1 P2 2.2835(4) . ? P1 C1 1.8164(14) . ? P1 C19 1.8209(14) . ? P1 C13 1.8226(15) . ? P2 C31 1.8214(16) . ? P2 C7 1.8219(14) . ? P2 C25 1.8240(15) . ? O1 C2 1.3871(17) . ? O1 C8 1.3921(17) . ? C1 C6 1.391(2) . ? C1 C2 1.394(2) . ? C2 C3 1.384(2) . ? C3 C4 1.385(2) . ? C3 H3A 0.9500 . ? C4 C5 1.377(3) . ? C4 H4A 0.9500 . ? C5 C6 1.390(2) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.393(2) . ? C7 C12 1.401(2) . ? C8 C9 1.3841(19) . ? C9 C10 1.384(2) . ? C9 H9A 0.9500 . ? C10 C11 1.385(2) . ? C10 H10A 0.9500 . ? C11 C12 1.381(2) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.393(2) . ? C13 C14 1.396(2) . ? C14 C15 1.389(2) . ? C14 H14A 0.9500 . ? C15 C16 1.381(3) . ? C15 H15A 0.9500 . ? C16 C17 1.381(3) . ? C16 H16A 0.9500 . ? C17 C18 1.388(2) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.393(2) . ? C19 C24 1.396(2) . ? C20 C21 1.391(2) . ? C20 H20A 0.9500 . ? C21 C22 1.379(3) . ? C21 H21A 0.9500 . ? C22 C23 1.383(3) . ? C22 H22A 0.9500 . ? C23 C24 1.387(2) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C30 1.389(2) . ? C25 C26 1.392(2) . ? C26 C27 1.386(2) . ? C26 H26A 0.9500 . ? C27 C28 1.381(3) . ? C27 H27A 0.9500 . ? C28 C29 1.383(3) . ? C28 H28A 0.9500 . ? C29 C30 1.390(2) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.383(2) . ? C31 C32 1.387(2) . ? C32 C33 1.385(2) . ? C32 H32A 0.9500 . ? C33 C34 1.378(3) . ? C33 H33A 0.9500 . ? C34 C35 1.369(4) . ? C34 H34A 0.9500 . ? C35 C36 1.394(3) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? N1 C37 1.3257(19) . ? N1 C41 1.3526(18) . ? N2 C46 1.3258(18) . ? N2 C42 1.3583(18) . ? C37 C38 1.395(2) . ? C37 H37A 0.9500 . ? C38 C39 1.369(2) . ? C38 H38A 0.9500 . ? C39 C40 1.403(2) . ? C39 H39A 0.9500 . ? C40 C41 1.407(2) . ? C40 C47 1.427(2) . ? C41 C42 1.4355(19) . ? C42 C43 1.4048(19) . ? C43 C44 1.398(2) . ? C43 C48 1.433(2) . ? C44 C45 1.367(3) . ? C44 H44A 0.9500 . ? C45 C46 1.400(2) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 C48 1.344(3) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? P10 F14' 1.498(7) . ? P10 F12 1.507(4) . ? P10 F15' 1.541(6) . ? P10 F10 1.5782(15) . ? P10 F13 1.582(4) . ? P10 F15 1.583(5) . ? P10 F11 1.6020(14) . ? P10 F14 1.609(5) . ? P10 F13' 1.617(6) . ? P10 F12' 1.626(5) . ? C100 Cl2 1.743(3) . ? C100 Cl1 1.751(3) . ? C100 H10B 0.9900 . ? C100 H10C 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N1 81.02(5) . . ? N2 Cu1 P1 129.03(4) . . ? N1 Cu1 P1 116.90(4) . . ? N2 Cu1 P2 102.54(4) . . ? N1 Cu1 P2 98.81(4) . . ? P1 Cu1 P2 119.175(15) . . ? C1 P1 C19 103.34(6) . . ? C1 P1 C13 102.50(7) . . ? C19 P1 C13 103.30(6) . . ? C1 P1 Cu1 112.27(5) . . ? C19 P1 Cu1 118.98(5) . . ? C13 P1 Cu1 114.55(5) . . ? C31 P2 C7 104.60(7) . . ? C31 P2 C25 103.14(7) . . ? C7 P2 C25 103.35(7) . . ? C31 P2 Cu1 120.06(5) . . ? C7 P2 Cu1 116.77(5) . . ? C25 P2 Cu1 106.89(5) . . ? C2 O1 C8 117.63(11) . . ? C6 C1 C2 118.35(13) . . ? C6 C1 P1 123.77(11) . . ? C2 C1 P1 117.88(10) . . ? C3 C2 O1 123.30(13) . . ? C3 C2 C1 121.50(14) . . ? O1 C2 C1 115.12(12) . . ? C2 C3 C4 118.81(15) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 C3 121.04(15) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 119.58(15) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C5 C6 C1 120.69(15) . . ? C5 C6 H6A 119.7 . . ? C1 C6 H6A 119.7 . . ? C8 C7 C12 117.52(13) . . ? C8 C7 P2 120.13(10) . . ? C12 C7 P2 122.35(11) . . ? C9 C8 O1 118.40(13) . . ? C9 C8 C7 122.07(13) . . ? O1 C8 C7 119.48(12) . . ? C10 C9 C8 119.03(15) . . ? C10 C9 H9A 120.5 . . ? C8 C9 H9A 120.5 . . ? C9 C10 C11 120.32(14) . . ? C9 C10 H10A 119.8 . . ? C11 C10 H10A 119.8 . . ? C12 C11 C10 120.08(14) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C7 120.94(15) . . ? C11 C12 H12A 119.5 . . ? C7 C12 H12A 119.5 . . ? C18 C13 C14 118.83(14) . . ? C18 C13 P1 118.72(11) . . ? C14 C13 P1 122.44(11) . . ? C15 C14 C13 120.23(15) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C16 C15 C14 120.28(16) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 C17 120.05(16) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C17 C18 120.03(16) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C18 C13 120.56(15) . . ? C17 C18 H18A 119.7 . . ? C13 C18 H18A 119.7 . . ? C20 C19 C24 119.13(13) . . ? C20 C19 P1 123.26(11) . . ? C24 C19 P1 117.57(11) . . ? C21 C20 C19 120.22(15) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C22 C21 C20 119.99(16) . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 120.40(15) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C22 C23 C24 119.92(16) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C19 120.32(15) . . ? C23 C24 H24A 119.8 . . ? C19 C24 H24A 119.8 . . ? C30 C25 C26 118.80(14) . . ? C30 C25 P2 120.49(12) . . ? C26 C25 P2 120.10(11) . . ? C27 C26 C25 120.69(16) . . ? C27 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C28 C27 C26 120.20(17) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C27 C28 C29 119.57(17) . . ? C27 C28 H28A 120.2 . . ? C29 C28 H28A 120.2 . . ? C28 C29 C30 120.46(17) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C25 C30 C29 120.24(16) . . ? C25 C30 H30A 119.9 . . ? C29 C30 H30A 119.9 . . ? C36 C31 C32 119.07(16) . . ? C36 C31 P2 117.31(14) . . ? C32 C31 P2 123.48(12) . . ? C33 C32 C31 120.71(18) . . ? C33 C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? C34 C33 C32 119.7(2) . . ? C34 C33 H33A 120.2 . . ? C32 C33 H33A 120.2 . . ? C35 C34 C33 120.22(19) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C34 C35 C36 120.4(2) . . ? C34 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? C31 C36 C35 119.9(2) . . ? C31 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C37 N1 C41 117.87(13) . . ? C37 N1 Cu1 129.92(11) . . ? C41 N1 Cu1 111.75(9) . . ? C46 N2 C42 117.84(13) . . ? C46 N2 Cu1 130.08(10) . . ? C42 N2 Cu1 111.42(9) . . ? N1 C37 C38 123.30(15) . . ? N1 C37 H37A 118.4 . . ? C38 C37 H37A 118.4 . . ? C39 C38 C37 119.04(15) . . ? C39 C38 H38A 120.5 . . ? C37 C38 H38A 120.5 . . ? C38 C39 C40 119.50(14) . . ? C38 C39 H39A 120.2 . . ? C40 C39 H39A 120.2 . . ? C39 C40 C41 117.36(14) . . ? C39 C40 C47 123.36(14) . . ? C41 C40 C47 119.26(14) . . ? N1 C41 C40 122.91(13) . . ? N1 C41 C42 117.23(12) . . ? C40 C41 C42 119.86(13) . . ? N2 C42 C43 123.14(13) . . ? N2 C42 C41 117.64(12) . . ? C43 C42 C41 119.22(13) . . ? C44 C43 C42 117.24(14) . . ? C44 C43 C48 123.37(14) . . ? C42 C43 C48 119.39(14) . . ? C45 C44 C43 119.63(15) . . ? C45 C44 H44A 120.2 . . ? C43 C44 H44A 120.2 . . ? C44 C45 C46 119.38(15) . . ? C44 C45 H45A 120.3 . . ? C46 C45 H45A 120.3 . . ? N2 C46 C45 122.77(15) . . ? N2 C46 H46A 118.6 . . ? C45 C46 H46A 118.6 . . ? C48 C47 C40 121.06(15) . . ? C48 C47 H47A 119.5 . . ? C40 C47 H47A 119.5 . . ? C47 C48 C43 121.18(15) . . ? C47 C48 H48A 119.4 . . ? C43 C48 H48A 119.4 . . ? F14' P10 F12 155.5(6) . . ? F14' P10 F15' 94.5(6) . . ? F12 P10 F15' 109.9(4) . . ? F14' P10 F10 93.7(4) . . ? F12 P10 F10 85.6(2) . . ? F15' P10 F10 88.8(3) . . ? F14' P10 F13 62.5(6) . . ? F12 P10 F13 93.0(3) . . ? F15' P10 F13 155.8(4) . . ? F10 P10 F13 85.4(2) . . ? F14' P10 F15 112.2(7) . . ? F12 P10 F15 92.3(4) . . ? F10 P10 F15 89.6(2) . . ? F13 P10 F15 172.3(3) . . ? F14' P10 F11 85.6(4) . . ? F12 P10 F11 95.5(2) . . ? F15' P10 F11 89.9(3) . . ? F10 P10 F11 178.49(10) . . ? F13 P10 F11 95.5(2) . . ? F15 P10 F11 89.4(2) . . ? F12 P10 F14 174.9(4) . . ? F15' P10 F14 69.1(5) . . ? F10 P10 F14 89.3(3) . . ? F13 P10 F14 87.3(3) . . ? F15 P10 F14 86.8(3) . . ? F11 P10 F14 89.5(3) . . ? F14' P10 F13' 94.8(6) . . ? F12 P10 F13' 61.2(4) . . ? F15' P10 F13' 167.9(4) . . ? F10 P10 F13' 98.1(2) . . ? F15 P10 F13' 151.4(5) . . ? F11 P10 F13' 83.3(2) . . ? F14 P10 F13' 120.6(5) . . ? F14' P10 F12' 170.7(4) . . ? F15' P10 F12' 84.8(4) . . ? F10 P10 F12' 95.5(3) . . ? F13 P10 F12' 119.1(3) . . ? F15 P10 F12' 67.1(3) . . ? F11 P10 F12' 85.1(3) . . ? F14 P10 F12' 153.3(4) . . ? F13' P10 F12' 84.7(4) . . ? Cl2 C100 Cl1 111.79(14) . . ? Cl2 C100 H10B 109.3 . . ? Cl1 C100 H10B 109.3 . . ? Cl2 C100 H10C 109.3 . . ? Cl1 C100 H10C 109.3 . . ? H10B C100 H10C 107.9 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.437 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.053 # Attachment 'JS61.CIF' data_js61 _database_code_depnum_ccdc_archive 'CCDC 802648' #TrackingRef 'JS61.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C42 H32 Cu N2 P2), C4 H10 O, C H2 Cl2, 2(F6 P), H2 O' _chemical_formula_sum 'C89 H78 Cl2 Cu2 F12 N4 O2 P6' _chemical_formula_weight 1847.38 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4818(15) _cell_length_b 13.4450(15) _cell_length_c 15.0834(18) _cell_angle_alpha 86.429(9) _cell_angle_beta 67.721(9) _cell_angle_gamma 62.963(8) _cell_volume 2067.6(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.774 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8300 _exptl_absorpt_correction_T_max 0.8605 _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 53123 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 30.00 _reflns_number_total 11970 _reflns_number_gt 11147 _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^)+(0.0651P)^2^+1.4814P] 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 11970 _refine_ls_number_parameters 606 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 5.892 _refine_ls_shift/su_max 0.026 _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 0.79937(8) 0.81016(7) 0.62022(6) 0.0292(2) Uani 1 1 d . . . P1 P 0.71317(16) 0.99785(14) 0.61570(13) 0.0276(4) Uani 1 1 d . . . P2 P 0.68208(18) 0.85002(15) 0.78011(13) 0.0316(4) Uani 1 1 d . . . C1 C 0.5388(7) 0.9826(6) 0.7891(6) 0.0328(16) Uani 1 1 d . . . C2 C 0.5520(6) 1.0489(6) 0.7139(6) 0.0311(16) Uani 1 1 d . . . C3 C 0.4442(7) 1.1503(6) 0.7186(7) 0.0374(18) Uani 1 1 d . . . H3A H 0.4529 1.1959 0.6683 0.045 Uiso 1 1 calc R . . C4 C 0.3247(8) 1.1853(7) 0.7959(8) 0.045(2) Uani 1 1 d . . . H4A H 0.2519 1.2545 0.7984 0.054 Uiso 1 1 calc R . . C5 C 0.3112(8) 1.1194(7) 0.8696(7) 0.046(2) Uani 1 1 d . . . H5A H 0.2290 1.1429 0.9222 0.055 Uiso 1 1 calc R . . C6 C 0.4179(8) 1.0189(7) 0.8665(6) 0.042(2) Uani 1 1 d . . . H6A H 0.4085 0.9745 0.9176 0.050 Uiso 1 1 calc R . . C7 C 0.7841(6) 1.0729(6) 0.6506(5) 0.0289(14) Uani 1 1 d . . . C8 C 0.7099(7) 1.1820(6) 0.7002(6) 0.0348(17) Uani 1 1 d . . . H8A H 0.6181 1.2204 0.7172 0.042 Uiso 1 1 calc R . . C9 C 0.7700(8) 1.2345(7) 0.7249(6) 0.0397(18) Uani 1 1 d . . . H9A H 0.7192 1.3090 0.7583 0.048 Uiso 1 1 calc R . . C10 C 0.9029(8) 1.1792(7) 0.7011(6) 0.0419(18) Uani 1 1 d . . . H10A H 0.9437 1.2158 0.7177 0.050 Uiso 1 1 calc R . . C11 C 0.9773(7) 1.0706(8) 0.6530(7) 0.043(2) Uani 1 1 d . . . H11A H 1.0688 1.0322 0.6375 0.052 Uiso 1 1 calc R . . C12 C 0.9183(7) 1.0177(7) 0.6273(6) 0.0345(17) Uani 1 1 d . . . H12A H 0.9698 0.9433 0.5936 0.041 Uiso 1 1 calc R . . C13 C 0.6841(6) 1.0593(6) 0.5105(5) 0.0299(15) Uani 1 1 d . . . C14 C 0.6939(8) 1.1566(7) 0.4826(6) 0.0430(18) Uani 1 1 d . . . H14A H 0.7046 1.1992 0.5234 0.052 Uiso 1 1 calc R . . C15 C 0.6879(8) 1.1914(7) 0.3951(7) 0.050(2) Uani 1 1 d . . . H15A H 0.6951 1.2576 0.3764 0.060 Uiso 1 1 calc R . . C16 C 0.6717(7) 1.1307(8) 0.3354(6) 0.0435(19) Uani 1 1 d . . . H16A H 0.6683 1.1547 0.2755 0.052 Uiso 1 1 calc R . . C17 C 0.6605(7) 1.0349(7) 0.3630(6) 0.0423(18) Uani 1 1 d . . . H17A H 0.6485 0.9931 0.3223 0.051 Uiso 1 1 calc R . . C18 C 0.6667(7) 0.9994(6) 0.4501(6) 0.0363(16) Uani 1 1 d . . . H18A H 0.6589 0.9334 0.4686 0.044 Uiso 1 1 calc R . . C19 C 0.7690(7) 0.8887(6) 0.8332(5) 0.0345(17) Uani 1 1 d . . . C20 C 0.7212(8) 0.9966(7) 0.8768(6) 0.0388(19) Uani 1 1 d . . . H20A H 0.6355 1.0526 0.8856 0.047 Uiso 1 1 calc R . . C21 C 0.7979(9) 1.0232(8) 0.9078(7) 0.049(2) Uani 1 1 d . . . H21A H 0.7648 1.0976 0.9367 0.058 Uiso 1 1 calc R . . C22 C 0.9217(9) 0.9420(9) 0.8966(8) 0.055(2) Uani 1 1 d . . . H22A H 0.9739 0.9605 0.9178 0.065 Uiso 1 1 calc R . . C23 C 0.9699(9) 0.8340(10) 0.8545(8) 0.055(3) Uani 1 1 d . . . H23A H 1.0546 0.7777 0.8478 0.065 Uiso 1 1 calc R . . C24 C 0.8951(8) 0.8076(8) 0.8220(7) 0.044(2) Uani 1 1 d . . . H24A H 0.9296 0.7335 0.7918 0.053 Uiso 1 1 calc R . . C25 C 0.6127(7) 0.7735(6) 0.8678(5) 0.0345(18) Uani 1 1 d . . . C26 C 0.6273(9) 0.7582(7) 0.9555(6) 0.042(2) Uani 1 1 d . . . H26A H 0.6740 0.7886 0.9715 0.050 Uiso 1 1 calc R . . C27 C 0.5733(10) 0.6981(8) 1.0202(7) 0.051(2) Uani 1 1 d . . . H27A H 0.5838 0.6875 1.0798 0.061 Uiso 1 1 calc R . . C28 C 0.5050(10) 0.6545(8) 0.9975(7) 0.052(3) Uani 1 1 d . . . H28A H 0.4686 0.6136 1.0414 0.062 Uiso 1 1 calc R . . C29 C 0.4891(10) 0.6700(8) 0.9106(7) 0.052(2) Uani 1 1 d . . . H29A H 0.4410 0.6405 0.8954 0.062 Uiso 1 1 calc R . . C30 C 0.5439(8) 0.7288(7) 0.8459(6) 0.043(2) Uani 1 1 d . . . H30A H 0.5340 0.7383 0.7860 0.051 Uiso 1 1 calc R . . N1 N 0.9958(5) 0.7035(5) 0.5498(4) 0.0278(12) Uani 1 1 d . . . N2 N 0.7871(5) 0.7172(5) 0.5263(5) 0.0314(13) Uani 1 1 d . . . C31 C 1.0995(7) 0.6934(6) 0.5635(6) 0.0347(16) Uani 1 1 d . . . H31A H 1.0849 0.7381 0.6174 0.042 Uiso 1 1 calc R . . C32 C 1.2280(7) 0.6207(7) 0.5030(7) 0.043(2) Uani 1 1 d . . . H32A H 1.2989 0.6156 0.5161 0.052 Uiso 1 1 calc R . . C33 C 1.2510(8) 0.5572(7) 0.4249(7) 0.045(2) Uani 1 1 d . . . H33A H 1.3383 0.5085 0.3821 0.054 Uiso 1 1 calc R . . C34 C 1.1449(8) 0.5640(6) 0.4078(6) 0.0374(19) Uani 1 1 d . . . C35 C 1.0183(6) 0.6383(5) 0.4731(5) 0.0280(14) Uani 1 1 d . . . C36 C 0.9063(7) 0.6463(5) 0.4602(5) 0.0296(14) Uani 1 1 d . . . C37 C 0.9249(8) 0.5804(6) 0.3816(6) 0.0411(18) Uani 1 1 d . . . C38 C 0.8133(9) 0.5886(7) 0.3734(7) 0.052(2) Uani 1 1 d . . . H38A H 0.8214 0.5462 0.3209 0.062 Uiso 1 1 calc R . . C39 C 0.6929(8) 0.6579(7) 0.4414(8) 0.053(2) Uani 1 1 d . . . H39A H 0.6164 0.6631 0.4375 0.064 Uiso 1 1 calc R . . C40 C 0.6827(7) 0.7215(7) 0.5171(7) 0.0429(19) Uani 1 1 d . . . H40A H 0.5980 0.7697 0.5639 0.051 Uiso 1 1 calc R . . C41 C 1.0561(11) 0.5066(8) 0.3162(7) 0.053(3) Uani 1 1 d . . . H41A H 1.0693 0.4618 0.2630 0.064 Uiso 1 1 calc RD . . C42 C 1.1603(10) 0.4991(7) 0.3279(7) 0.051(3) Uani 1 1 d . . . H42A H 1.2457 0.4501 0.2827 0.061 Uiso 1 1 calc R . . P10 P 0.63251(17) 0.47962(16) 1.25051(14) 0.0326(4) Uani 1 1 d . . . F10 F 0.7469(5) 0.4112(5) 1.2876(5) 0.0639(16) Uani 1 1 d . A . F11 F 0.5187(6) 0.5471(6) 1.2141(5) 0.0674(18) Uani 1 1 d . A . F12 F 0.5691(6) 0.3984(6) 1.2876(6) 0.0542(19) Uani 0.786(9) 1 d P A 1 F13 F 0.6929(7) 0.5634(7) 1.2147(7) 0.067(2) Uani 0.786(9) 1 d P A 1 F14 F 0.5413(8) 0.5595(9) 1.3514(7) 0.072(3) Uani 0.786(9) 1 d P A 1 F15 F 0.7219(8) 0.4022(9) 1.1506(6) 0.067(3) Uani 0.786(9) 1 d P A 1 F12' F 0.659(3) 0.355(3) 1.220(3) 0.123(10) Uani 0.214(9) 1 d P A 2 F13' F 0.625(4) 0.590(3) 1.270(5) 0.142(16) Uani 0.214(9) 1 d P A 2 F14' F 0.558(4) 0.471(6) 1.356(3) 0.13(2) Uani 0.214(9) 1 d P A 2 F15' F 0.709(5) 0.475(5) 1.139(3) 0.13(2) Uani 0.214(9) 1 d P A 2 C100 C 1.102(2) 0.693(3) 1.087(2) 0.087(8) Uani 0.50 1 d P B 1 H10C H 1.0453 0.6561 1.1015 0.104 Uiso 0.50 1 calc PR B 1 H10B H 1.1378 0.6875 1.0158 0.104 Uiso 0.50 1 calc PR B 1 Cl1 Cl 1.2106(11) 0.6026(8) 1.0960(8) 0.112(3) Uani 0.50 1 d P B 1 Cl2 Cl 0.9934(9) 0.8159(13) 1.1090(9) 0.138(5) Uani 0.50 1 d P B 1 C200 C 1.057(2) 0.416(2) 1.0554(18) 0.076(8) Uani 0.50 1 d P C 2 H20B H 1.0416 0.4173 0.9962 0.113 Uiso 0.50 1 calc PR C 2 H20C H 1.0269 0.3671 1.0967 0.113 Uiso 0.50 1 calc PR C 2 H20D H 1.1508 0.3875 1.0386 0.113 Uiso 0.50 1 calc PR C 2 C201 C 0.9780(16) 0.5414(17) 1.1121(11) 0.041(4) Uani 0.50 1 d PU C 2 H20E H 0.9564 0.5439 1.1825 0.049 Uiso 0.50 1 calc PRD C 2 H20F H 0.8995 0.5908 1.0990 0.049 Uiso 0.50 1 calc PR C 2 O202 O 1.105(4) 0.562(4) 1.051(3) 0.184(19) Uani 0.50 1 d PU C 2 C203 C 1.060(2) 0.691(2) 1.095(2) 0.068(8) Uani 0.50 1 d PD C 2 H20G H 0.9774 0.7428 1.0885 0.081 Uiso 0.50 1 calc PR C 2 H20H H 1.0415 0.6926 1.1650 0.081 Uiso 0.50 1 calc PR C 2 C204 C 1.143(4) 0.732(4) 1.056(3) 0.122(17) Uani 0.50 1 d PD C 2 H20I H 1.1591 0.7580 1.1069 0.183 Uiso 0.50 1 calc PR C 2 H20J H 1.1065 0.7951 1.0224 0.183 Uiso 0.50 1 calc PR C 2 H20K H 1.2261 0.6728 1.0099 0.183 Uiso 0.50 1 calc PR C 2 O300 O 0.999(3) 0.573(3) 1.105(3) 0.058(9) Uiso 0.25 1 d P D 3 O301 O 1.006(3) 0.500(3) 1.102(3) 0.059(9) Uiso 0.25 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 0.0293(3) 0.0219(3) 0.0279(4) 0.0008(3) -0.0058(3) -0.0093(3) P1 0.0280(6) 0.0217(6) 0.0294(7) 0.0056(5) -0.0084(5) -0.0114(5) P2 0.0338(7) 0.0219(6) 0.0262(7) 0.0030(6) -0.0034(6) -0.0094(5) C1 0.032(3) 0.024(2) 0.033(3) 0.002(2) -0.005(2) -0.011(2) C2 0.029(2) 0.023(2) 0.036(3) 0.004(2) -0.007(2) -0.0120(19) C3 0.031(3) 0.025(3) 0.050(4) 0.008(3) -0.013(3) -0.011(2) C4 0.031(3) 0.029(3) 0.061(5) 0.002(3) -0.010(3) -0.009(2) C5 0.031(3) 0.035(3) 0.049(5) -0.002(3) 0.002(3) -0.011(3) C6 0.038(3) 0.031(3) 0.038(4) 0.002(3) -0.001(3) -0.013(3) C7 0.031(2) 0.027(2) 0.027(3) 0.007(2) -0.009(2) -0.0147(19) C8 0.035(3) 0.027(3) 0.039(3) 0.004(2) -0.012(2) -0.014(2) C9 0.049(3) 0.033(3) 0.039(3) 0.005(3) -0.015(3) -0.023(2) C10 0.049(3) 0.050(3) 0.037(3) 0.008(3) -0.015(3) -0.033(3) C11 0.033(3) 0.052(4) 0.043(4) 0.005(3) -0.012(3) -0.021(3) C12 0.030(2) 0.034(3) 0.032(3) 0.003(2) -0.007(2) -0.014(2) C13 0.029(2) 0.027(2) 0.035(3) 0.009(2) -0.013(2) -0.0143(19) C14 0.063(3) 0.037(3) 0.050(4) 0.020(3) -0.034(3) -0.032(2) C15 0.073(3) 0.050(3) 0.059(4) 0.034(3) -0.044(3) -0.044(3) C16 0.047(3) 0.054(4) 0.046(3) 0.021(3) -0.028(3) -0.030(3) C17 0.047(3) 0.046(3) 0.048(4) 0.012(3) -0.028(3) -0.026(3) C18 0.039(2) 0.033(3) 0.045(3) 0.011(2) -0.020(2) -0.021(2) C19 0.037(3) 0.028(3) 0.027(3) 0.005(2) -0.004(2) -0.013(2) C20 0.043(3) 0.030(3) 0.032(3) 0.002(3) -0.005(3) -0.015(3) C21 0.059(4) 0.043(4) 0.042(4) 0.002(3) -0.012(3) -0.028(3) C22 0.056(4) 0.064(5) 0.051(5) 0.008(4) -0.019(4) -0.036(3) C23 0.042(4) 0.055(5) 0.057(5) 0.006(4) -0.016(4) -0.016(4) C24 0.042(3) 0.035(3) 0.042(4) 0.003(3) -0.011(3) -0.011(3) C25 0.040(3) 0.023(2) 0.028(3) 0.002(2) -0.003(3) -0.012(2) C26 0.054(3) 0.036(3) 0.033(3) 0.010(3) -0.013(3) -0.023(3) C27 0.068(4) 0.045(4) 0.035(4) 0.013(3) -0.011(3) -0.031(3) C28 0.067(4) 0.040(3) 0.040(4) 0.008(3) -0.005(4) -0.032(3) C29 0.064(4) 0.048(4) 0.043(4) 0.000(3) -0.007(4) -0.036(3) C30 0.051(3) 0.037(3) 0.032(3) 0.000(3) -0.006(3) -0.022(3) N1 0.0279(19) 0.023(2) 0.029(2) 0.0057(18) -0.0091(18) -0.0113(16) N2 0.034(2) 0.023(2) 0.039(3) 0.0074(19) -0.017(2) -0.0131(17) C31 0.034(2) 0.031(3) 0.043(3) 0.011(2) -0.017(2) -0.017(2) C32 0.030(3) 0.034(3) 0.062(5) 0.018(3) -0.016(3) -0.016(2) C33 0.029(3) 0.031(3) 0.051(5) 0.011(3) 0.000(3) -0.009(3) C34 0.039(3) 0.024(3) 0.031(3) 0.006(2) -0.001(3) -0.011(2) C35 0.032(2) 0.020(2) 0.025(3) 0.0065(19) -0.006(2) -0.0119(19) C36 0.042(3) 0.021(2) 0.028(3) 0.0077(19) -0.015(2) -0.0156(19) C37 0.067(4) 0.029(3) 0.035(3) 0.009(2) -0.024(3) -0.026(3) C38 0.087(4) 0.038(3) 0.059(4) 0.017(3) -0.049(3) -0.037(3) C39 0.074(3) 0.040(3) 0.082(5) 0.027(3) -0.058(3) -0.036(3) C40 0.043(3) 0.031(3) 0.067(4) 0.015(3) -0.032(3) -0.020(2) C41 0.084(5) 0.035(3) 0.031(3) 0.000(3) -0.016(4) -0.026(4) C42 0.060(5) 0.033(3) 0.032(4) -0.003(3) 0.002(4) -0.016(3) P10 0.0347(6) 0.0307(7) 0.0348(8) 0.0084(6) -0.0162(6) -0.0158(6) F10 0.066(2) 0.052(3) 0.097(4) 0.024(3) -0.058(2) -0.026(2) F11 0.066(2) 0.058(3) 0.092(4) 0.020(3) -0.057(2) -0.020(2) F12 0.053(3) 0.048(3) 0.079(4) 0.031(3) -0.033(3) -0.035(2) F13 0.078(3) 0.064(3) 0.094(5) 0.044(3) -0.049(3) -0.054(2) F14 0.061(4) 0.086(5) 0.053(4) -0.027(4) -0.011(3) -0.027(4) F15 0.050(3) 0.083(5) 0.050(4) -0.023(4) -0.009(3) -0.022(4) F12' 0.169(15) 0.039(14) 0.24(3) 0.023(15) -0.179(15) -0.034(13) F13' 0.15(2) 0.030(13) 0.30(5) 0.00(2) -0.17(2) -0.019(15) F14' 0.046(16) 0.22(5) 0.047(15) 0.06(2) -0.013(13) -0.01(3) F15' 0.11(3) 0.11(3) 0.06(2) 0.03(2) 0.01(2) 0.00(3) C100 0.058(7) 0.153(17) 0.060(12) -0.036(12) -0.007(9) -0.064(10) Cl1 0.161(6) 0.097(5) 0.098(5) 0.013(4) -0.058(5) -0.071(4) Cl2 0.104(4) 0.186(11) 0.132(6) 0.005(7) -0.079(4) -0.047(6) C200 0.079(11) 0.065(12) 0.078(11) 0.037(9) -0.055(9) -0.013(10) C201 0.042(6) 0.052(8) 0.016(5) -0.004(5) -0.001(5) -0.020(6) O202 0.15(2) 0.14(2) 0.12(2) 0.00(2) 0.01(2) -0.01(2) C203 0.042(9) 0.077(14) 0.072(14) -0.021(11) -0.020(9) -0.017(10) C204 0.16(3) 0.12(3) 0.065(19) 0.007(19) -0.02(2) -0.07(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 2.037(7) . ? Cu1 N1 2.053(5) . ? Cu1 P2 2.240(2) . ? Cu1 P1 2.2574(19) . ? P1 C7 1.820(9) . ? P1 C2 1.823(7) . ? P1 C13 1.825(8) . ? P2 C19 1.820(10) . ? P2 C25 1.825(8) . ? P2 C1 1.828(7) . ? C1 C6 1.395(10) . ? C1 C2 1.405(11) . ? C2 C3 1.395(9) . ? C3 C4 1.385(11) . ? C3 H3A 0.9500 . ? C4 C5 1.385(14) . ? C4 H4A 0.9500 . ? C5 C6 1.387(11) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.391(10) . ? C7 C8 1.394(9) . ? C8 C9 1.388(13) . ? C8 H8A 0.9500 . ? C9 C10 1.376(11) . ? C9 H9A 0.9500 . ? C10 C11 1.381(12) . ? C10 H10A 0.9500 . ? C11 C12 1.388(14) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.388(12) . ? C13 C14 1.394(11) . ? C14 C15 1.389(13) . ? C14 H14A 0.9500 . ? C15 C16 1.378(15) . ? C15 H15A 0.9500 . ? C16 C17 1.381(14) . ? C16 H16A 0.9500 . ? C17 C18 1.388(13) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.388(11) . ? C19 C24 1.399(11) . ? C20 C21 1.390(16) . ? C20 H20A 0.9500 . ? C21 C22 1.378(14) . ? C21 H21A 0.9500 . ? C22 C23 1.381(16) . ? C22 H22A 0.9500 . ? C23 C24 1.381(17) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C30 1.385(14) . ? C25 C26 1.393(13) . ? C26 C27 1.398(13) . ? C26 H26A 0.9500 . ? C27 C28 1.374(18) . ? C27 H27A 0.9500 . ? C28 C29 1.387(16) . ? C28 H28A 0.9500 . ? C29 C30 1.391(14) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? N1 C31 1.333(11) . ? N1 C35 1.357(10) . ? N2 C40 1.338(11) . ? N2 C36 1.349(8) . ? C31 C32 1.392(10) . ? C31 H31A 0.9500 . ? C32 C33 1.359(15) . ? C32 H32A 0.9500 . ? C33 C34 1.405(15) . ? C33 H33A 0.9500 . ? C34 C35 1.405(9) . ? C34 C42 1.433(14) . ? C35 C36 1.440(11) . ? C36 C37 1.407(11) . ? C37 C38 1.399(15) . ? C37 C41 1.435(12) . ? C38 C39 1.363(12) . ? C38 H38A 0.9500 . ? C39 C40 1.401(14) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.336(18) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? P10 F13' 1.49(4) . ? P10 F14' 1.54(4) . ? P10 F15 1.570(8) . ? P10 F15' 1.57(4) . ? P10 F11 1.581(7) . ? P10 F12 1.583(8) . ? P10 F13 1.587(9) . ? P10 F14 1.595(8) . ? P10 F10 1.595(7) . ? P10 F12' 1.61(4) . ? C100 Cl1 1.40(3) . ? C100 Cl2 1.54(3) . ? C100 H10C 0.9900 . ? C100 H10B 0.9900 . ? C200 C201 1.60(3) . ? C200 H20B 0.9800 . ? C200 H20C 0.9800 . ? C200 H20D 0.9800 . ? C201 O202 1.64(5) . ? C201 H20E 0.9900 . ? C201 H20F 0.9900 . ? O202 C203 1.66(6) . ? C203 C204 1.32(5) . ? C203 H20G 0.9900 . ? C203 H20H 0.9900 . ? C204 H20I 0.9800 . ? C204 H20J 0.9800 . ? C204 H20K 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N1 82.0(2) . . ? N2 Cu1 P2 125.61(19) . . ? N1 Cu1 P2 127.33(19) . . ? N2 Cu1 P1 117.06(18) . . ? N1 Cu1 P1 122.08(18) . . ? P2 Cu1 P1 87.14(7) . . ? C7 P1 C2 102.9(3) . . ? C7 P1 C13 104.5(3) . . ? C2 P1 C13 105.8(3) . . ? C7 P1 Cu1 117.9(2) . . ? C2 P1 Cu1 101.6(2) . . ? C13 P1 Cu1 121.7(2) . . ? C19 P2 C25 104.9(4) . . ? C19 P2 C1 104.7(4) . . ? C25 P2 C1 103.4(3) . . ? C19 P2 Cu1 107.0(2) . . ? C25 P2 Cu1 132.2(3) . . ? C1 P2 Cu1 101.8(3) . . ? C6 C1 C2 119.4(7) . . ? C6 C1 P2 122.6(6) . . ? C2 C1 P2 118.1(5) . . ? C3 C2 C1 119.4(6) . . ? C3 C2 P1 123.4(6) . . ? C1 C2 P1 117.2(5) . . ? C4 C3 C2 120.6(8) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 120.1(7) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C6 120.0(7) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C1 120.6(8) . . ? C5 C6 H6A 119.7 . . ? C1 C6 H6A 119.7 . . ? C12 C7 C8 119.1(8) . . ? C12 C7 P1 118.0(6) . . ? C8 C7 P1 123.0(6) . . ? C9 C8 C7 120.1(7) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C10 C9 C8 120.3(7) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C9 C10 C11 120.1(9) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C10 C11 C12 120.0(7) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C7 120.4(7) . . ? C11 C12 H12A 119.8 . . ? C7 C12 H12A 119.8 . . ? C18 C13 C14 118.7(8) . . ? C18 C13 P1 118.3(6) . . ? C14 C13 P1 122.6(7) . . ? C15 C14 C13 120.1(9) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C16 C15 C14 120.6(9) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 119.7(9) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C16 C17 C18 120.1(9) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C18 C13 120.8(8) . . ? C17 C18 H18A 119.6 . . ? C13 C18 H18A 119.6 . . ? C20 C19 C24 118.5(9) . . ? C20 C19 P2 123.4(6) . . ? C24 C19 P2 117.8(7) . . ? C19 C20 C21 120.5(8) . . ? C19 C20 H20A 119.7 . . ? C21 C20 H20A 119.7 . . ? C22 C21 C20 120.1(9) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C21 C22 C23 120.0(11) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C24 120.1(9) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C19 120.7(9) . . ? C23 C24 H24A 119.7 . . ? C19 C24 H24A 119.7 . . ? C30 C25 C26 119.1(8) . . ? C30 C25 P2 118.7(7) . . ? C26 C25 P2 122.3(7) . . ? C25 C26 C27 120.3(10) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C28 C27 C26 119.9(10) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C27 C28 C29 120.3(9) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C28 C29 C30 119.7(11) . . ? C28 C29 H29A 120.1 . . ? C30 C29 H29A 120.1 . . ? C25 C30 C29 120.7(9) . . ? C25 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? C31 N1 C35 117.6(6) . . ? C31 N1 Cu1 131.5(5) . . ? C35 N1 Cu1 110.8(5) . . ? C40 N2 C36 117.5(7) . . ? C40 N2 Cu1 130.6(5) . . ? C36 N2 Cu1 111.8(5) . . ? N1 C31 C32 123.3(8) . . ? N1 C31 H31A 118.4 . . ? C32 C31 H31A 118.4 . . ? C33 C32 C31 119.3(9) . . ? C33 C32 H32A 120.4 . . ? C31 C32 H32A 120.4 . . ? C32 C33 C34 119.6(7) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? C33 C34 C35 117.6(8) . . ? C33 C34 C42 123.2(7) . . ? C35 C34 C42 119.2(9) . . ? N1 C35 C34 122.7(8) . . ? N1 C35 C36 117.6(5) . . ? C34 C35 C36 119.7(7) . . ? N2 C36 C37 123.3(8) . . ? N2 C36 C35 117.1(7) . . ? C37 C36 C35 119.6(6) . . ? C38 C37 C36 117.6(7) . . ? C38 C37 C41 123.7(9) . . ? C36 C37 C41 118.7(9) . . ? C39 C38 C37 119.3(9) . . ? C39 C38 H38A 120.4 . . ? C37 C38 H38A 120.4 . . ? C38 C39 C40 119.6(9) . . ? C38 C39 H39A 120.2 . . ? C40 C39 H39A 120.2 . . ? N2 C40 C39 122.7(7) . . ? N2 C40 H40A 118.7 . . ? C39 C40 H40A 118.7 . . ? C42 C41 C37 121.9(9) . . ? C42 C41 H41A 119.1 . . ? C37 C41 H41A 119.1 . . ? C41 C42 C34 120.9(8) . . ? C41 C42 H42A 119.5 . . ? C34 C42 H42A 119.5 . . ? F13' P10 F14' 97(4) . . ? F13' P10 F15 123(2) . . ? F14' P10 F15 139(3) . . ? F13' P10 F15' 90(4) . . ? F14' P10 F15' 173(4) . . ? F13' P10 F11 86(2) . . ? F14' P10 F11 102.9(15) . . ? F15 P10 F11 90.9(4) . . ? F15' P10 F11 77(2) . . ? F13' P10 F12 146(2) . . ? F14' P10 F12 53(3) . . ? F15 P10 F12 90.3(5) . . ? F15' P10 F12 120(3) . . ? F11 P10 F12 86.9(4) . . ? F14' P10 F13 126(3) . . ? F15 P10 F13 90.8(5) . . ? F15' P10 F13 61(3) . . ? F11 P10 F13 92.4(5) . . ? F12 P10 F13 178.7(4) . . ? F13' P10 F14 56(2) . . ? F15 P10 F14 179.4(6) . . ? F15' P10 F14 145(2) . . ? F11 P10 F14 88.7(5) . . ? F12 P10 F14 90.1(5) . . ? F13 P10 F14 88.8(5) . . ? F13' P10 F10 94(2) . . ? F14' P10 F10 76.9(15) . . ? F15 P10 F10 89.2(4) . . ? F15' P10 F10 103(2) . . ? F11 P10 F10 179.7(4) . . ? F12 P10 F10 92.8(4) . . ? F13 P10 F10 87.9(4) . . ? F14 P10 F10 91.2(5) . . ? F13' P10 F12' 173(2) . . ? F14' P10 F12' 89(3) . . ? F15 P10 F12' 50.9(17) . . ? F15' P10 F12' 84(3) . . ? F11 P10 F12' 97.3(14) . . ? F13 P10 F12' 140.4(16) . . ? F14 P10 F12' 129.6(18) . . ? F10 P10 F12' 82.6(14) . . ? Cl1 C100 Cl2 155(2) . . ? Cl1 C100 H10C 97.8 . . ? Cl2 C100 H10C 97.8 . . ? Cl1 C100 H10B 97.8 . . ? Cl2 C100 H10B 97.8 . . ? H10C C100 H10B 103.7 . . ? C201 C200 H20B 109.5 . . ? C201 C200 H20C 109.5 . . ? H20B C200 H20C 109.5 . . ? C201 C200 H20D 109.5 . . ? H20B C200 H20D 109.5 . . ? H20C C200 H20D 109.5 . . ? C200 C201 O202 90(2) . . ? C200 C201 H20E 113.7 . . ? O202 C201 H20E 113.7 . . ? C200 C201 H20F 113.7 . . ? O202 C201 H20F 113.7 . . ? H20E C201 H20F 111.0 . . ? C201 O202 C203 104(2) . . ? C204 C203 O202 117(3) . . ? C204 C203 H20G 107.9 . . ? O202 C203 H20G 107.9 . . ? C204 C203 H20H 107.9 . . ? O202 C203 H20H 107.9 . . ? H20G C203 H20H 107.2 . . ? C203 C204 H20I 109.5 . . ? C203 C204 H20J 109.5 . . ? H20I C204 H20J 109.5 . . ? C203 C204 H20K 109.5 . . ? H20I C204 H20K 109.5 . . ? H20J C204 H20K 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.663 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.067