# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Cudppbbpz2ph2 _database_code_depnum_ccdc_archive 'CCDC 898693' #TrackingRef 'Complex1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H40 B Cu N4 P2, C H2 Cl2' _chemical_formula_sum 'C49 H42 B Cl2 Cu N4 P2' _chemical_formula_weight 894.06 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' B B 0.0013 0.0007 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 9.6512(8) _cell_length_b 22.813(2) _cell_length_c 19.5335(17) _cell_angle_alpha 90 _cell_angle_beta 93.960(2) _cell_angle_gamma 90 _cell_volume 4290.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 13014 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 32.8 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.841 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku AFC-8 with Saturn CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 115869 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 31.00 _reflns_number_total 13634 _reflns_number_gt 11982 _reflns_threshold_expression I>2\s(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution SIR2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.079P)^2^+6.4455P] 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 13634 _refine_ls_number_parameters 574 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1721 _refine_ls_wR_factor_gt 0.1658 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.11170(3) 0.425827(12) 0.762734(14) 0.01578(8) Uani 1 1 d . . . P1 P 0.04150(6) 0.50991(2) 0.71033(3) 0.01555(11) Uani 1 1 d . . . P2 P 0.32873(6) 0.43900(3) 0.72926(3) 0.01682(12) Uani 1 1 d . . . N1 N 0.0954(2) 0.42454(8) 0.86482(10) 0.0170(4) Uani 1 1 d . . . N2 N 0.0746(2) 0.37407(8) 0.89977(10) 0.0172(3) Uani 1 1 d . . . N3 N -0.0061(2) 0.35344(9) 0.74639(10) 0.0173(3) Uani 1 1 d . . . N4 N -0.0288(2) 0.31419(8) 0.79742(10) 0.0159(3) Uani 1 1 d . . . C1 C -0.0737(2) 0.51133(10) 0.63193(12) 0.0182(4) Uani 1 1 d . . . C2 C -0.0595(3) 0.46531(11) 0.58554(12) 0.0228(5) Uani 1 1 d . . . H2 H 0.0073 0.4355 0.5960 0.027 Uiso 1 1 calc R . . C3 C -0.1417(3) 0.46272(12) 0.52454(13) 0.0278(5) Uani 1 1 d . . . H3 H -0.1311 0.4312 0.4936 0.033 Uiso 1 1 calc R . . C4 C -0.2390(3) 0.50599(14) 0.50873(14) 0.0308(6) Uani 1 1 d . . . H4 H -0.2965 0.5039 0.4673 0.037 Uiso 1 1 calc R . . C5 C -0.2522(3) 0.55244(15) 0.55367(14) 0.0321(6) Uani 1 1 d . . . H5 H -0.3177 0.5826 0.5424 0.039 Uiso 1 1 calc R . . C6 C -0.1704(3) 0.55516(12) 0.61505(14) 0.0261(5) Uani 1 1 d . . . H6 H -0.1805 0.5871 0.6456 0.031 Uiso 1 1 calc R . . C7 C -0.0304(2) 0.56623(10) 0.76431(12) 0.0184(4) Uani 1 1 d . . . C8 C -0.1616(3) 0.55458(12) 0.78745(14) 0.0263(5) Uani 1 1 d . . . H8 H -0.2097 0.5200 0.7728 0.032 Uiso 1 1 calc R . . C9 C -0.2224(3) 0.59320(13) 0.83175(16) 0.0325(6) Uani 1 1 d . . . H9 H -0.3123 0.5853 0.8465 0.039 Uiso 1 1 calc R . . C10 C -0.1515(4) 0.64303(13) 0.85427(14) 0.0333(6) Uani 1 1 d . . . H10 H -0.1928 0.6693 0.8846 0.040 Uiso 1 1 calc R . . C11 C -0.0213(4) 0.65467(12) 0.83290(15) 0.0335(6) Uani 1 1 d . . . H11 H 0.0274 0.6888 0.8488 0.040 Uiso 1 1 calc R . . C12 C 0.0392(3) 0.61634(12) 0.78781(14) 0.0267(5) Uani 1 1 d . . . H12 H 0.1289 0.6247 0.7731 0.032 Uiso 1 1 calc R . . C13 C 0.2004(2) 0.54313(10) 0.68125(11) 0.0169(4) Uani 1 1 d . . . C14 C 0.1971(3) 0.59766(10) 0.64838(12) 0.0199(4) Uani 1 1 d . . . H14 H 0.1106 0.6165 0.6376 0.024 Uiso 1 1 calc R . . C15 C 0.3190(3) 0.62449(11) 0.63135(13) 0.0232(5) Uani 1 1 d . . . H15 H 0.3159 0.6612 0.6083 0.028 Uiso 1 1 calc R . . C16 C 0.4461(3) 0.59740(11) 0.64824(14) 0.0238(5) Uani 1 1 d . . . H16 H 0.5300 0.6164 0.6383 0.029 Uiso 1 1 calc R . . C17 C 0.4504(3) 0.54288(11) 0.67947(13) 0.0221(4) Uani 1 1 d . . . H17 H 0.5375 0.5246 0.6906 0.027 Uiso 1 1 calc R . . C18 C 0.3280(2) 0.51435(9) 0.69477(12) 0.0168(4) Uani 1 1 d . . . C19 C 0.4812(2) 0.44039(10) 0.78988(13) 0.0196(4) Uani 1 1 d . . . C20 C 0.4683(3) 0.46927(13) 0.85226(15) 0.0294(5) Uani 1 1 d . . . H20 H 0.3833 0.4881 0.8607 0.035 Uiso 1 1 calc R . . C21 C 0.5778(3) 0.47074(14) 0.90179(16) 0.0337(6) Uani 1 1 d . . . H21 H 0.5678 0.4906 0.9439 0.040 Uiso 1 1 calc R . . C22 C 0.7025(3) 0.44321(12) 0.89021(15) 0.0286(5) Uani 1 1 d . . . H22 H 0.7776 0.4441 0.9243 0.034 Uiso 1 1 calc R . . C23 C 0.7163(3) 0.41450(12) 0.82877(15) 0.0270(5) Uani 1 1 d . . . H23 H 0.8015 0.3957 0.8206 0.032 Uiso 1 1 calc R . . C24 C 0.6063(3) 0.41284(11) 0.77870(14) 0.0238(5) Uani 1 1 d . . . H24 H 0.6168 0.3928 0.7367 0.029 Uiso 1 1 calc R . . C25 C 0.3808(2) 0.39375(10) 0.65785(13) 0.0206(4) Uani 1 1 d . . . C26 C 0.4784(3) 0.40956(11) 0.61135(14) 0.0241(5) Uani 1 1 d . . . H26 H 0.5229 0.4467 0.6156 0.029 Uiso 1 1 calc R . . C27 C 0.5112(3) 0.37175(12) 0.55908(14) 0.0272(5) Uani 1 1 d . . . H27 H 0.5784 0.3829 0.5283 0.033 Uiso 1 1 calc R . . C28 C 0.4464(3) 0.31810(14) 0.55185(18) 0.0377(7) Uani 1 1 d . . . H28 H 0.4680 0.2924 0.5158 0.045 Uiso 1 1 calc R . . C29 C 0.3500(4) 0.30182(15) 0.5973(2) 0.0517(10) Uani 1 1 d . . . H29 H 0.3057 0.2647 0.5925 0.062 Uiso 1 1 calc R . . C30 C 0.3170(3) 0.33937(13) 0.65005(19) 0.0372(7) Uani 1 1 d . . . H30 H 0.2504 0.3277 0.6809 0.045 Uiso 1 1 calc R . . C31 C 0.1123(3) 0.46717(11) 0.91205(13) 0.0232(5) Uani 1 1 d . . . H31 H 0.1267 0.5073 0.9019 0.028 Uiso 1 1 calc R . . C32 C 0.1059(3) 0.44453(12) 0.97791(13) 0.0263(5) Uani 1 1 d . . . H32 H 0.1158 0.4651 1.0202 0.032 Uiso 1 1 calc R . . C33 C 0.0818(3) 0.38527(11) 0.96774(12) 0.0232(5) Uani 1 1 d . . . H33 H 0.0719 0.3571 1.0029 0.028 Uiso 1 1 calc R . . C34 C -0.0987(3) 0.34090(12) 0.69453(13) 0.0246(5) Uani 1 1 d . . . H34 H -0.1077 0.3619 0.6525 0.029 Uiso 1 1 calc R . . C35 C -0.1806(3) 0.29303(12) 0.71010(14) 0.0267(5) Uani 1 1 d . . . H35 H -0.2532 0.2753 0.6820 0.032 Uiso 1 1 calc R . . C36 C -0.1324(2) 0.27732(10) 0.77560(13) 0.0209(4) Uani 1 1 d . . . H36 H -0.1665 0.2457 0.8013 0.025 Uiso 1 1 calc R . . C37 C -0.0052(2) 0.26878(10) 0.91944(12) 0.0193(4) Uani 1 1 d . . . C38 C -0.1403(3) 0.28082(11) 0.93872(13) 0.0233(5) Uani 1 1 d . . . H38 H -0.1893 0.3132 0.9183 0.028 Uiso 1 1 calc R . . C39 C -0.2040(3) 0.24697(12) 0.98642(14) 0.0273(5) Uani 1 1 d . . . H39 H -0.2953 0.2563 0.9982 0.033 Uiso 1 1 calc R . . C40 C -0.1345(3) 0.19962(13) 1.01696(14) 0.0320(6) Uani 1 1 d . . . H40 H -0.1779 0.1761 1.0495 0.038 Uiso 1 1 calc R . . C41 C -0.0012(3) 0.18686(14) 0.99967(16) 0.0353(6) Uani 1 1 d . . . H41 H 0.0476 0.1548 1.0210 0.042 Uiso 1 1 calc R . . C42 C 0.0620(3) 0.22069(12) 0.95110(14) 0.0270(5) Uani 1 1 d . . . H42 H 0.1529 0.2108 0.9393 0.032 Uiso 1 1 calc R . . C43 C 0.2196(2) 0.29001(10) 0.84680(12) 0.0190(4) Uani 1 1 d . . . C44 C 0.2336(3) 0.24326(12) 0.80129(15) 0.0287(5) Uani 1 1 d . . . H44 H 0.1523 0.2248 0.7813 0.034 Uiso 1 1 calc R . . C45 C 0.3622(3) 0.22307(15) 0.78457(17) 0.0361(7) Uani 1 1 d . . . H45 H 0.3684 0.1913 0.7535 0.043 Uiso 1 1 calc R . . C46 C 0.4820(3) 0.24950(14) 0.81335(17) 0.0336(6) Uani 1 1 d . . . H46 H 0.5706 0.2365 0.8012 0.040 Uiso 1 1 calc R . . C47 C 0.4720(3) 0.29472(13) 0.85964(17) 0.0322(6) Uani 1 1 d . . . H47 H 0.5537 0.3120 0.8807 0.039 Uiso 1 1 calc R . . C48 C 0.3414(3) 0.31504(11) 0.87551(15) 0.0262(5) Uani 1 1 d . . . H48 H 0.3357 0.3468 0.9067 0.031 Uiso 1 1 calc R . . B1 B 0.0673(3) 0.31118(11) 0.86576(13) 0.0171(4) Uani 1 1 d . . . Cl1 Cl 0.40372(11) 0.64538(9) 0.82214(6) 0.0868(5) Uani 1 1 d . . . Cl2 Cl 0.49854(16) 0.64120(7) 0.96526(6) 0.0808(4) Uani 1 1 d . . . C49 C 0.3613(7) 0.6365(5) 0.9042(3) 0.135(4) Uani 1 1 d . . . H49A H 0.3169 0.5976 0.9083 0.162 Uiso 1 1 calc R . . H49B H 0.2918 0.6666 0.9144 0.162 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01450(14) 0.01459(13) 0.01844(14) 0.00095(9) 0.00243(10) -0.00006(9) P1 0.0142(2) 0.0144(2) 0.0181(3) 0.00076(19) 0.00129(19) 0.00115(19) P2 0.0134(2) 0.0158(2) 0.0215(3) 0.0008(2) 0.0027(2) 0.00098(19) N1 0.0182(9) 0.0148(8) 0.0183(8) -0.0008(6) 0.0031(7) 0.0002(6) N2 0.0169(9) 0.0175(8) 0.0171(8) 0.0002(7) 0.0008(7) 0.0003(7) N3 0.0187(9) 0.0175(8) 0.0158(8) 0.0004(6) 0.0019(7) -0.0031(7) N4 0.0155(8) 0.0136(8) 0.0185(8) 0.0008(6) 0.0010(7) -0.0003(6) C1 0.0156(9) 0.0208(10) 0.0181(10) 0.0010(8) 0.0009(8) -0.0016(8) C2 0.0296(12) 0.0194(10) 0.0197(10) 0.0017(8) 0.0035(9) -0.0020(9) C3 0.0389(15) 0.0262(12) 0.0186(11) -0.0005(9) 0.0036(10) -0.0079(11) C4 0.0246(12) 0.0461(16) 0.0212(11) 0.0040(11) -0.0025(10) -0.0059(11) C5 0.0227(12) 0.0484(17) 0.0245(12) 0.0022(11) -0.0038(10) 0.0113(12) C6 0.0236(12) 0.0308(13) 0.0234(11) -0.0021(9) -0.0013(9) 0.0081(10) C7 0.0207(10) 0.0177(9) 0.0169(9) 0.0023(7) 0.0017(8) 0.0045(8) C8 0.0267(12) 0.0216(11) 0.0315(13) 0.0017(9) 0.0088(10) 0.0035(9) C9 0.0328(14) 0.0328(14) 0.0338(14) 0.0026(11) 0.0145(11) 0.0120(11) C10 0.0508(18) 0.0272(13) 0.0228(12) 0.0015(10) 0.0097(12) 0.0143(12) C11 0.0517(18) 0.0232(12) 0.0257(12) -0.0074(10) 0.0039(12) -0.0010(12) C12 0.0323(13) 0.0243(11) 0.0237(11) -0.0055(9) 0.0034(10) -0.0025(10) C13 0.0171(10) 0.0160(9) 0.0176(9) -0.0004(7) 0.0022(8) -0.0008(7) C14 0.0230(11) 0.0172(10) 0.0196(10) 0.0017(8) 0.0019(8) -0.0004(8) C15 0.0276(12) 0.0196(10) 0.0228(11) 0.0020(8) 0.0035(9) -0.0029(9) C16 0.0221(11) 0.0202(11) 0.0296(12) 0.0012(9) 0.0063(9) -0.0044(9) C17 0.0177(10) 0.0201(10) 0.0290(12) -0.0005(9) 0.0051(9) -0.0021(8) C18 0.0161(10) 0.0146(9) 0.0200(10) -0.0007(7) 0.0035(8) 0.0001(7) C19 0.0147(10) 0.0184(10) 0.0254(11) 0.0016(8) 0.0000(8) -0.0002(8) C20 0.0198(11) 0.0371(14) 0.0312(13) -0.0065(11) 0.0006(10) 0.0038(10) C21 0.0284(14) 0.0401(15) 0.0322(14) -0.0098(12) -0.0016(11) 0.0015(12) C22 0.0214(12) 0.0276(12) 0.0357(14) 0.0027(10) -0.0059(10) -0.0010(10) C23 0.0163(11) 0.0257(12) 0.0386(14) 0.0030(10) -0.0015(10) 0.0043(9) C24 0.0188(11) 0.0224(11) 0.0301(12) 0.0015(9) 0.0027(9) 0.0045(9) C25 0.0173(10) 0.0193(10) 0.0256(11) -0.0010(8) 0.0033(8) 0.0031(8) C26 0.0230(11) 0.0222(11) 0.0278(12) 0.0012(9) 0.0057(9) 0.0013(9) C27 0.0238(12) 0.0304(13) 0.0282(12) -0.0017(10) 0.0070(10) 0.0065(10) C28 0.0356(15) 0.0319(14) 0.0470(18) -0.0158(13) 0.0128(13) 0.0041(12) C29 0.053(2) 0.0292(15) 0.077(3) -0.0241(16) 0.032(2) -0.0139(14) C30 0.0350(15) 0.0255(13) 0.0538(19) -0.0118(12) 0.0237(14) -0.0070(11) C31 0.0236(11) 0.0194(10) 0.0269(11) -0.0043(9) 0.0031(9) -0.0009(9) C32 0.0284(13) 0.0291(12) 0.0213(11) -0.0078(9) 0.0007(9) 0.0008(10) C33 0.0260(12) 0.0257(11) 0.0178(10) -0.0004(8) 0.0004(9) -0.0002(9) C34 0.0293(13) 0.0259(12) 0.0179(10) 0.0023(9) -0.0030(9) -0.0068(10) C35 0.0285(13) 0.0269(12) 0.0237(11) -0.0008(9) -0.0056(10) -0.0086(10) C36 0.0194(10) 0.0197(10) 0.0234(11) 0.0010(8) -0.0001(8) -0.0058(8) C37 0.0209(10) 0.0181(10) 0.0185(10) 0.0021(8) -0.0012(8) -0.0012(8) C38 0.0221(11) 0.0223(11) 0.0259(11) 0.0047(9) 0.0046(9) 0.0006(9) C39 0.0276(13) 0.0299(12) 0.0250(12) 0.0028(10) 0.0056(10) -0.0055(10) C40 0.0379(15) 0.0344(14) 0.0234(12) 0.0093(10) 0.0010(11) -0.0115(12) C41 0.0356(15) 0.0334(14) 0.0360(15) 0.0187(12) -0.0033(12) -0.0025(12) C42 0.0252(12) 0.0256(12) 0.0296(12) 0.0088(10) -0.0026(10) 0.0005(9) C43 0.0175(10) 0.0172(9) 0.0222(10) 0.0039(8) -0.0003(8) 0.0003(8) C44 0.0208(12) 0.0296(13) 0.0355(14) -0.0077(11) 0.0012(10) 0.0048(10) C45 0.0270(14) 0.0385(16) 0.0433(17) -0.0072(13) 0.0056(12) 0.0119(12) C46 0.0197(12) 0.0350(14) 0.0468(17) 0.0101(12) 0.0079(11) 0.0096(10) C47 0.0157(11) 0.0280(13) 0.0520(18) 0.0087(12) -0.0035(11) -0.0007(9) C48 0.0201(11) 0.0215(11) 0.0365(14) 0.0015(10) -0.0026(10) -0.0003(9) B1 0.0168(11) 0.0166(10) 0.0178(10) 0.0007(8) -0.0001(8) 0.0006(8) Cl1 0.0310(5) 0.1808(16) 0.0488(6) 0.0370(8) 0.0042(4) 0.0025(7) Cl2 0.0902(9) 0.1057(11) 0.0445(6) -0.0073(6) -0.0088(6) 0.0288(8) C49 0.070(4) 0.255(11) 0.078(4) -0.078(6) -0.012(3) 0.032(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.011(2) . ? Cu1 N3 2.0180(19) . ? Cu1 P1 2.2562(6) . ? Cu1 P2 2.2571(7) . ? P1 C7 1.829(2) . ? P1 C1 1.830(2) . ? P1 C13 1.835(2) . ? P2 C19 1.824(2) . ? P2 C25 1.833(2) . ? P2 C18 1.846(2) . ? N1 C31 1.343(3) . ? N1 N2 1.361(3) . ? N2 C33 1.349(3) . ? N2 B1 1.581(3) . ? N3 C34 1.335(3) . ? N3 N4 1.369(3) . ? N4 C36 1.353(3) . ? N4 B1 1.574(3) . ? C1 C6 1.391(3) . ? C1 C2 1.400(3) . ? C2 C3 1.386(4) . ? C2 H2 0.9500 . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 C5 1.387(4) . ? C4 H4 0.9500 . ? C5 C6 1.391(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.388(3) . ? C7 C8 1.399(4) . ? C8 C9 1.393(4) . ? C8 H8 0.9500 . ? C9 C10 1.383(5) . ? C9 H9 0.9500 . ? C10 C11 1.377(5) . ? C10 H10 0.9500 . ? C11 C12 1.397(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.399(3) . ? C13 C18 1.404(3) . ? C14 C15 1.387(3) . ? C14 H14 0.9500 . ? C15 C16 1.392(4) . ? C15 H15 0.9500 . ? C16 C17 1.385(3) . ? C16 H16 0.9500 . ? C17 C18 1.399(3) . ? C17 H17 0.9500 . ? C19 C24 1.392(3) . ? C19 C20 1.398(4) . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C21 C22 1.389(4) . ? C21 H21 0.9500 . ? C22 C23 1.382(4) . ? C22 H22 0.9500 . ? C23 C24 1.393(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.389(4) . ? C25 C26 1.400(3) . ? C26 C27 1.390(4) . ? C26 H26 0.9500 . ? C27 C28 1.377(4) . ? C27 H27 0.9500 . ? C28 C29 1.381(5) . ? C28 H28 0.9500 . ? C29 C30 1.394(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.392(4) . ? C31 H31 0.9500 . ? C32 C33 1.384(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.394(4) . ? C34 H34 0.9500 . ? C35 C36 1.378(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.397(3) . ? C37 C38 1.409(3) . ? C37 B1 1.620(3) . ? C38 C39 1.386(3) . ? C38 H38 0.9500 . ? C39 C40 1.385(4) . ? C39 H39 0.9500 . ? C40 C41 1.383(5) . ? C40 H40 0.9500 . ? C41 C42 1.396(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.390(3) . ? C43 C44 1.401(4) . ? C43 B1 1.614(3) . ? C44 C45 1.383(4) . ? C44 H44 0.9500 . ? C45 C46 1.389(5) . ? C45 H45 0.9500 . ? C46 C47 1.380(5) . ? C46 H46 0.9500 . ? C47 C48 1.398(4) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? Cl1 C49 1.695(8) . ? Cl2 C49 1.723(6) . ? C49 H49A 0.9900 . ? C49 H49B 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 N1 Cu1 N3 93.62(8) . . ? N1 Cu1 P1 114.88(6) . . ? N3 Cu1 P1 118.40(6) . . ? N1 Cu1 P2 115.26(6) . . ? N3 Cu1 P2 125.97(6) . . ? P1 Cu1 P2 90.63(2) . . ? C7 P1 C1 103.72(11) . . ? C7 P1 C13 104.29(11) . . ? C1 P1 C13 101.90(10) . . ? C7 P1 Cu1 116.72(8) . . ? C1 P1 Cu1 122.74(8) . . ? C13 P1 Cu1 105.09(7) . . ? C19 P2 C25 104.62(11) . . ? C19 P2 C18 101.74(11) . . ? C25 P2 C18 103.95(11) . . ? C19 P2 Cu1 122.51(8) . . ? C25 P2 Cu1 117.01(8) . . ? C18 P2 Cu1 104.44(7) . . ? C31 N1 N2 106.46(19) . . ? C31 N1 Cu1 131.04(17) . . ? N2 N1 Cu1 122.29(14) . . ? C33 N2 N1 109.53(19) . . ? C33 N2 B1 125.7(2) . . ? N1 N2 B1 124.13(18) . . ? C34 N3 N4 106.27(19) . . ? C34 N3 Cu1 129.49(17) . . ? N4 N3 Cu1 122.47(14) . . ? C36 N4 N3 109.21(18) . . ? C36 N4 B1 128.30(19) . . ? N3 N4 B1 122.13(18) . . ? C6 C1 C2 118.6(2) . . ? C6 C1 P1 124.73(19) . . ? C2 C1 P1 116.60(18) . . ? C3 C2 C1 120.8(2) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.6(2) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 120.2(3) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C12 C7 C8 118.6(2) . . ? C12 C7 P1 125.1(2) . . ? C8 C7 P1 116.16(19) . . ? C9 C8 C7 120.7(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.3(3) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.0(3) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 120.7(3) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C18 119.6(2) . . ? C14 C13 P1 121.07(17) . . ? C18 C13 P1 119.30(17) . . ? C15 C14 C13 120.6(2) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.7(2) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 120.2(2) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.8(2) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C13 119.0(2) . . ? C17 C18 P2 121.93(18) . . ? C13 C18 P2 119.03(16) . . ? C24 C19 C20 118.7(2) . . ? C24 C19 P2 124.1(2) . . ? C20 C19 P2 117.21(18) . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 120.2(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 119.5(3) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 120.5(2) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C19 C24 C23 120.3(2) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C30 C25 C26 118.2(2) . . ? C30 C25 P2 116.3(2) . . ? C26 C25 P2 125.49(19) . . ? C27 C26 C25 120.9(2) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C28 C27 C26 120.2(3) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 119.6(3) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C28 C29 C30 120.5(3) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C25 C30 C29 120.6(3) . . ? C25 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? N1 C31 C32 110.8(2) . . ? N1 C31 H31 124.6 . . ? C32 C31 H31 124.6 . . ? C33 C32 C31 104.3(2) . . ? C33 C32 H32 127.8 . . ? C31 C32 H32 127.8 . . ? N2 C33 C32 108.8(2) . . ? N2 C33 H33 125.6 . . ? C32 C33 H33 125.6 . . ? N3 C34 C35 111.3(2) . . ? N3 C34 H34 124.4 . . ? C35 C34 H34 124.4 . . ? C36 C35 C34 104.2(2) . . ? C36 C35 H35 127.9 . . ? C34 C35 H35 127.9 . . ? N4 C36 C35 109.0(2) . . ? N4 C36 H36 125.5 . . ? C35 C36 H36 125.5 . . ? C42 C37 C38 116.4(2) . . ? C42 C37 B1 123.2(2) . . ? C38 C37 B1 120.4(2) . . ? C39 C38 C37 122.2(2) . . ? C39 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? C40 C39 C38 120.0(3) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 119.3(2) . . ? C41 C40 H40 120.3 . . ? C39 C40 H40 120.3 . . ? C40 C41 C42 120.5(3) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 121.6(3) . . ? C41 C42 H42 119.2 . . ? C37 C42 H42 119.2 . . ? C48 C43 C44 116.9(2) . . ? C48 C43 B1 122.9(2) . . ? C44 C43 B1 120.2(2) . . ? C45 C44 C43 122.1(3) . . ? C45 C44 H44 119.0 . . ? C43 C44 H44 119.0 . . ? C44 C45 C46 119.7(3) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C47 C46 C45 119.7(3) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C46 C47 C48 119.9(3) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C43 C48 C47 121.6(3) . . ? C43 C48 H48 119.2 . . ? C47 C48 H48 119.2 . . ? N4 B1 N2 108.87(18) . . ? N4 B1 C43 108.12(18) . . ? N2 B1 C43 110.69(19) . . ? N4 B1 C37 108.62(18) . . ? N2 B1 C37 106.17(18) . . ? C43 B1 C37 114.25(19) . . ? Cl1 C49 Cl2 115.0(4) . . ? Cl1 C49 H49A 108.5 . . ? Cl2 C49 H49A 108.5 . . ? Cl1 C49 H49B 108.5 . . ? Cl2 C49 H49B 108.5 . . ? H49A C49 H49B 107.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 P1 C7 -3.00(11) . . . . ? N3 Cu1 P1 C7 106.25(11) . . . . ? P2 Cu1 P1 C7 -121.40(9) . . . . ? N1 Cu1 P1 C1 -132.76(11) . . . . ? N3 Cu1 P1 C1 -23.50(11) . . . . ? P2 Cu1 P1 C1 108.85(9) . . . . ? N1 Cu1 P1 C13 111.96(10) . . . . ? N3 Cu1 P1 C13 -138.79(10) . . . . ? P2 Cu1 P1 C13 -6.44(8) . . . . ? N1 Cu1 P2 C19 6.42(11) . . . . ? N3 Cu1 P2 C19 -108.96(12) . . . . ? P1 Cu1 P2 C19 124.48(9) . . . . ? N1 Cu1 P2 C25 137.77(11) . . . . ? N3 Cu1 P2 C25 22.39(12) . . . . ? P1 Cu1 P2 C25 -104.17(9) . . . . ? N1 Cu1 P2 C18 -107.99(10) . . . . ? N3 Cu1 P2 C18 136.63(10) . . . . ? P1 Cu1 P2 C18 10.07(8) . . . . ? N3 Cu1 N1 C31 -158.5(2) . . . . ? P1 Cu1 N1 C31 -34.8(2) . . . . ? P2 Cu1 N1 C31 68.6(2) . . . . ? N3 Cu1 N1 N2 27.55(18) . . . . ? P1 Cu1 N1 N2 151.24(15) . . . . ? P2 Cu1 N1 N2 -105.34(16) . . . . ? C31 N1 N2 C33 -1.4(3) . . . . ? Cu1 N1 N2 C33 173.85(16) . . . . ? C31 N1 N2 B1 -172.5(2) . . . . ? Cu1 N1 N2 B1 2.7(3) . . . . ? N1 Cu1 N3 C34 143.0(2) . . . . ? P1 Cu1 N3 C34 22.1(2) . . . . ? P2 Cu1 N3 C34 -92.0(2) . . . . ? N1 Cu1 N3 N4 -19.67(18) . . . . ? P1 Cu1 N3 N4 -140.56(15) . . . . ? P2 Cu1 N3 N4 105.37(16) . . . . ? C34 N3 N4 C36 1.5(3) . . . . ? Cu1 N3 N4 C36 167.62(16) . . . . ? C34 N3 N4 B1 175.2(2) . . . . ? Cu1 N3 N4 B1 -18.7(3) . . . . ? C7 P1 C1 C6 12.9(2) . . . . ? C13 P1 C1 C6 -95.2(2) . . . . ? Cu1 P1 C1 C6 147.9(2) . . . . ? C7 P1 C1 C2 -168.70(18) . . . . ? C13 P1 C1 C2 83.2(2) . . . . ? Cu1 P1 C1 C2 -33.7(2) . . . . ? C6 C1 C2 C3 -1.2(4) . . . . ? P1 C1 C2 C3 -179.7(2) . . . . ? C1 C2 C3 C4 0.1(4) . . . . ? C2 C3 C4 C5 1.1(4) . . . . ? C3 C4 C5 C6 -1.3(5) . . . . ? C4 C5 C6 C1 0.3(4) . . . . ? C2 C1 C6 C5 1.0(4) . . . . ? P1 C1 C6 C5 179.3(2) . . . . ? C1 P1 C7 C12 -118.4(2) . . . . ? C13 P1 C7 C12 -12.1(2) . . . . ? Cu1 P1 C7 C12 103.3(2) . . . . ? C1 P1 C7 C8 66.9(2) . . . . ? C13 P1 C7 C8 173.24(19) . . . . ? Cu1 P1 C7 C8 -71.4(2) . . . . ? C12 C7 C8 C9 1.6(4) . . . . ? P1 C7 C8 C9 176.6(2) . . . . ? C7 C8 C9 C10 -1.3(4) . . . . ? C8 C9 C10 C11 0.2(4) . . . . ? C9 C10 C11 C12 0.6(4) . . . . ? C8 C7 C12 C11 -0.8(4) . . . . ? P1 C7 C12 C11 -175.4(2) . . . . ? C10 C11 C12 C7 -0.3(4) . . . . ? C7 P1 C13 C14 -54.3(2) . . . . ? C1 P1 C13 C14 53.4(2) . . . . ? Cu1 P1 C13 C14 -177.57(17) . . . . ? C7 P1 C13 C18 123.14(19) . . . . ? C1 P1 C13 C18 -129.17(19) . . . . ? Cu1 P1 C13 C18 -0.18(19) . . . . ? C18 C13 C14 C15 -2.4(3) . . . . ? P1 C13 C14 C15 174.99(19) . . . . ? C13 C14 C15 C16 -1.2(4) . . . . ? C14 C15 C16 C17 2.5(4) . . . . ? C15 C16 C17 C18 -0.3(4) . . . . ? C16 C17 C18 C13 -3.3(4) . . . . ? C16 C17 C18 P2 174.5(2) . . . . ? C14 C13 C18 C17 4.6(3) . . . . ? P1 C13 C18 C17 -172.85(18) . . . . ? C14 C13 C18 P2 -173.23(17) . . . . ? P1 C13 C18 P2 9.3(3) . . . . ? C19 P2 C18 C17 40.5(2) . . . . ? C25 P2 C18 C17 -68.0(2) . . . . ? Cu1 P2 C18 C17 168.79(18) . . . . ? C19 P2 C18 C13 -141.80(19) . . . . ? C25 P2 C18 C13 109.71(19) . . . . ? Cu1 P2 C18 C13 -13.46(19) . . . . ? C25 P2 C19 C24 1.4(2) . . . . ? C18 P2 C19 C24 -106.5(2) . . . . ? Cu1 P2 C19 C24 137.71(19) . . . . ? C25 P2 C19 C20 -176.1(2) . . . . ? C18 P2 C19 C20 75.9(2) . . . . ? Cu1 P2 C19 C20 -39.8(2) . . . . ? C24 C19 C20 C21 0.3(4) . . . . ? P2 C19 C20 C21 178.0(2) . . . . ? C19 C20 C21 C22 -0.3(5) . . . . ? C20 C21 C22 C23 0.2(5) . . . . ? C21 C22 C23 C24 -0.2(4) . . . . ? C20 C19 C24 C23 -0.4(4) . . . . ? P2 C19 C24 C23 -177.9(2) . . . . ? C22 C23 C24 C19 0.3(4) . . . . ? C19 P2 C25 C30 110.7(2) . . . . ? C18 P2 C25 C30 -143.0(2) . . . . ? Cu1 P2 C25 C30 -28.4(3) . . . . ? C19 P2 C25 C26 -69.3(2) . . . . ? C18 P2 C25 C26 37.1(2) . . . . ? Cu1 P2 C25 C26 151.6(2) . . . . ? C30 C25 C26 C27 -0.4(4) . . . . ? P2 C25 C26 C27 179.6(2) . . . . ? C25 C26 C27 C28 0.7(4) . . . . ? C26 C27 C28 C29 -0.7(5) . . . . ? C27 C28 C29 C30 0.4(6) . . . . ? C26 C25 C30 C29 0.0(5) . . . . ? P2 C25 C30 C29 -179.9(3) . . . . ? C28 C29 C30 C25 -0.1(6) . . . . ? N2 N1 C31 C32 1.4(3) . . . . ? Cu1 N1 C31 C32 -173.26(18) . . . . ? N1 C31 C32 C33 -0.9(3) . . . . ? N1 N2 C33 C32 0.9(3) . . . . ? B1 N2 C33 C32 171.8(2) . . . . ? C31 C32 C33 N2 0.0(3) . . . . ? N4 N3 C34 C35 -1.2(3) . . . . ? Cu1 N3 C34 C35 -166.03(19) . . . . ? N3 C34 C35 C36 0.5(3) . . . . ? N3 N4 C36 C35 -1.2(3) . . . . ? B1 N4 C36 C35 -174.4(2) . . . . ? C34 C35 C36 N4 0.4(3) . . . . ? C42 C37 C38 C39 -0.1(4) . . . . ? B1 C37 C38 C39 -177.5(2) . . . . ? C37 C38 C39 C40 0.2(4) . . . . ? C38 C39 C40 C41 0.4(4) . . . . ? C39 C40 C41 C42 -1.1(5) . . . . ? C40 C41 C42 C37 1.2(5) . . . . ? C38 C37 C42 C41 -0.6(4) . . . . ? B1 C37 C42 C41 176.8(3) . . . . ? C48 C43 C44 C45 -0.9(4) . . . . ? B1 C43 C44 C45 -178.9(3) . . . . ? C43 C44 C45 C46 0.0(5) . . . . ? C44 C45 C46 C47 1.6(5) . . . . ? C45 C46 C47 C48 -2.2(5) . . . . ? C44 C43 C48 C47 0.2(4) . . . . ? B1 C43 C48 C47 178.1(2) . . . . ? C46 C47 C48 C43 1.4(4) . . . . ? C36 N4 B1 N2 -133.0(2) . . . . ? N3 N4 B1 N2 54.6(3) . . . . ? C36 N4 B1 C43 106.7(3) . . . . ? N3 N4 B1 C43 -65.7(3) . . . . ? C36 N4 B1 C37 -17.8(3) . . . . ? N3 N4 B1 C37 169.78(19) . . . . ? C33 N2 B1 N4 144.4(2) . . . . ? N1 N2 B1 N4 -45.9(3) . . . . ? C33 N2 B1 C43 -96.9(3) . . . . ? N1 N2 B1 C43 72.8(3) . . . . ? C33 N2 B1 C37 27.7(3) . . . . ? N1 N2 B1 C37 -162.7(2) . . . . ? C48 C43 B1 N4 137.5(2) . . . . ? C44 C43 B1 N4 -44.7(3) . . . . ? C48 C43 B1 N2 18.3(3) . . . . ? C44 C43 B1 N2 -163.8(2) . . . . ? C48 C43 B1 C37 -101.5(3) . . . . ? C44 C43 B1 C37 76.4(3) . . . . ? C42 C37 B1 N4 125.8(2) . . . . ? C38 C37 B1 N4 -57.0(3) . . . . ? C42 C37 B1 N2 -117.3(2) . . . . ? C38 C37 B1 N2 59.9(3) . . . . ? C42 C37 B1 C43 5.0(3) . . . . ? C38 C37 B1 C43 -177.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.759 _refine_diff_density_min -2.210 _refine_diff_density_rms 0.102 data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 898694' #TrackingRef 'Complex2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H32 B Cu F8 N4 P2 ' _chemical_formula_sum 'C48 H32 B Cu F8 N4 P2' _chemical_formula_weight 953.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4467(8) _cell_length_b 13.2352(11) _cell_length_c 13.7652(9) _cell_angle_alpha 89.778(4) _cell_angle_beta 70.725(4) _cell_angle_gamma 78.648(3) _cell_volume 2094.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90 _cell_measurement_reflns_used 8990 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 32.6 _exptl_crystal_description prism _exptl_crystal_colour colorless _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 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.675 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.818 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku AFC-8 with Saturn70 CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29243 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 30.08 _reflns_number_total 12050 _reflns_number_gt 10392 _reflns_threshold_expression I>2\s(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution SIR2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0458P)^2^+0.4324P] 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 12050 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.196162(12) 0.237160(10) 0.775378(10) 0.01107(4) Uani 1 1 d . . . P1 P 0.05107(3) 0.16335(2) 0.76289(2) 0.01072(6) Uani 1 1 d . . . P2 P 0.15058(3) 0.35280(2) 0.66734(2) 0.01025(6) Uani 1 1 d . . . F1 F -0.16670(8) 0.09733(7) 1.13549(6) 0.02538(18) Uani 1 1 d . . . F2 F -0.19767(10) -0.11467(8) 0.87891(8) 0.0416(3) Uani 1 1 d . . . F3 F 0.31130(7) -0.15936(6) 0.54154(7) 0.02729(18) Uani 1 1 d . . . F4 F 0.09346(9) 0.07377(7) 0.38550(6) 0.0327(2) Uani 1 1 d . . . F5 F 0.17516(8) 0.66824(6) 0.86381(6) 0.02534(18) Uani 1 1 d . . . F6 F 0.13772(9) 0.72186(6) 0.53794(7) 0.0298(2) Uani 1 1 d . . . F7 F 0.50465(7) 0.22610(7) 0.34783(6) 0.02838(19) Uani 1 1 d . . . F8 F 0.14418(8) 0.29522(7) 0.29614(6) 0.02795(19) Uani 1 1 d . . . N1 N 0.18349(8) 0.30284(7) 0.91007(7) 0.01213(18) Uani 1 1 d . . . N2 N 0.27812(8) 0.30070(7) 0.93948(7) 0.01143(18) Uani 1 1 d . . . N3 N 0.35489(9) 0.14723(7) 0.74641(8) 0.01289(18) Uani 1 1 d . . . N4 N 0.42265(8) 0.15861(7) 0.80455(7) 0.01159(18) Uani 1 1 d . . . C1 C -0.04446(10) 0.09430(9) 0.85766(9) 0.0128(2) Uani 1 1 d . . . C2 C -0.07201(11) 0.12362(9) 0.96186(9) 0.0142(2) Uani 1 1 d . . . H2 H -0.0438 0.1787 0.9823 0.017 Uiso 1 1 calc R . . C3 C -0.14132(11) 0.07022(10) 1.03405(9) 0.0170(2) Uani 1 1 d . . . C4 C -0.18494(11) -0.01048(10) 1.00999(10) 0.0206(3) Uani 1 1 d . . . H4 H -0.2321 -0.0460 1.0617 0.025 Uiso 1 1 calc R . . C5 C -0.15612(12) -0.03674(11) 0.90639(11) 0.0232(3) Uani 1 1 d . . . C6 C -0.08707(12) 0.01324(10) 0.82943(10) 0.0194(2) Uani 1 1 d . . . H6 H -0.0691 -0.0072 0.7588 0.023 Uiso 1 1 calc R . . C7 C 0.10115(10) 0.07802(9) 0.64513(9) 0.0129(2) Uani 1 1 d . . . C8 C 0.18295(11) -0.01320(9) 0.63936(9) 0.0147(2) Uani 1 1 d . . . H8 H 0.2049 -0.0336 0.6975 0.018 Uiso 1 1 calc R . . C9 C 0.23090(11) -0.07266(10) 0.54736(10) 0.0187(2) Uani 1 1 d . . . C10 C 0.20253(12) -0.04678(11) 0.46022(10) 0.0223(3) Uani 1 1 d . . . H10 H 0.2365 -0.0890 0.3977 0.027 Uiso 1 1 calc R . . C11 C 0.12258(13) 0.04331(11) 0.46908(9) 0.0215(3) Uani 1 1 d . . . C12 C 0.06961(11) 0.10660(10) 0.55912(9) 0.0168(2) Uani 1 1 d . . . H12 H 0.0135 0.1677 0.5621 0.020 Uiso 1 1 calc R . . C13 C -0.04929(10) 0.27134(9) 0.73513(9) 0.0128(2) Uani 1 1 d . . . C14 C -0.16633(11) 0.27031(10) 0.75280(10) 0.0182(2) Uani 1 1 d . . . H14 H -0.1966 0.2119 0.7805 0.022 Uiso 1 1 calc R . . C15 C -0.23874(11) 0.35436(11) 0.73011(10) 0.0206(3) Uani 1 1 d . . . H15 H -0.3176 0.3523 0.7405 0.025 Uiso 1 1 calc R . . C16 C -0.19610(11) 0.44104(10) 0.69242(10) 0.0196(2) Uani 1 1 d . . . H16 H -0.2463 0.4990 0.6787 0.023 Uiso 1 1 calc R . . C17 C -0.07990(11) 0.44337(9) 0.67458(9) 0.0164(2) Uani 1 1 d . . . H17 H -0.0512 0.5031 0.6489 0.020 Uiso 1 1 calc R . . C18 C -0.00495(10) 0.35830(9) 0.69417(8) 0.0118(2) Uani 1 1 d . . . C19 C 0.15903(10) 0.48860(8) 0.67444(9) 0.0125(2) Uani 1 1 d . . . C20 C 0.16680(10) 0.52704(9) 0.76568(9) 0.0143(2) Uani 1 1 d . . . H20 H 0.1723 0.4830 0.8192 0.017 Uiso 1 1 calc R . . C21 C 0.16620(11) 0.63119(9) 0.77592(10) 0.0172(2) Uani 1 1 d . . . C22 C 0.15602(12) 0.69935(9) 0.70187(10) 0.0206(3) Uani 1 1 d . . . H22 H 0.1536 0.7709 0.7117 0.025 Uiso 1 1 calc R . . C23 C 0.14955(12) 0.65767(9) 0.61255(10) 0.0190(2) Uani 1 1 d . . . C24 C 0.15268(11) 0.55421(9) 0.59585(10) 0.0165(2) Uani 1 1 d . . . H24 H 0.1506 0.5282 0.5324 0.020 Uiso 1 1 calc R . . C25 C 0.21460(10) 0.31743(8) 0.52865(9) 0.0121(2) Uani 1 1 d . . . C26 C 0.33538(11) 0.28401(9) 0.49009(9) 0.0151(2) Uani 1 1 d . . . H26 H 0.3804 0.2798 0.5344 0.018 Uiso 1 1 calc R . . C27 C 0.38768(11) 0.25714(9) 0.38558(10) 0.0184(2) Uani 1 1 d . . . C28 C 0.32671(12) 0.25940(10) 0.31786(10) 0.0206(3) Uani 1 1 d . . . H28 H 0.3647 0.2398 0.2465 0.025 Uiso 1 1 calc R . . C29 C 0.20747(12) 0.29173(9) 0.35951(9) 0.0179(2) Uani 1 1 d . . . C30 C 0.14939(11) 0.32143(9) 0.46290(9) 0.0153(2) Uani 1 1 d . . . H30 H 0.0672 0.3440 0.4885 0.018 Uiso 1 1 calc R . . C31 C 0.24334(11) 0.35054(10) 1.03373(9) 0.0188(2) Uani 1 1 d . . . H31 H 0.2929 0.3601 1.0711 0.023 Uiso 1 1 calc R . . C32 C 0.12438(11) 0.38530(11) 1.06683(10) 0.0216(3) Uani 1 1 d . . . H32 H 0.0762 0.4227 1.1300 0.026 Uiso 1 1 calc R . . C33 C 0.09054(11) 0.35332(9) 0.98708(9) 0.0162(2) Uani 1 1 d . . . H33 H 0.0127 0.3655 0.9872 0.019 Uiso 1 1 calc R . . C34 C 0.52116(11) 0.08474(9) 0.77232(10) 0.0160(2) Uani 1 1 d . . . H34 H 0.5829 0.0767 0.7997 0.019 Uiso 1 1 calc R . . C35 C 0.51768(11) 0.02286(9) 0.69333(10) 0.0195(2) Uani 1 1 d . . . H35 H 0.5745 -0.0353 0.6564 0.023 Uiso 1 1 calc R . . C36 C 0.41220(11) 0.06498(9) 0.68007(10) 0.0169(2) Uani 1 1 d . . . H36 H 0.3845 0.0390 0.6307 0.020 Uiso 1 1 calc R . . C37 C 0.48606(10) 0.24573(9) 0.94009(9) 0.0135(2) Uani 1 1 d . . . C38 C 0.48102(11) 0.16196(10) 1.00368(10) 0.0182(2) Uani 1 1 d . . . H38 H 0.4365 0.1131 0.9979 0.022 Uiso 1 1 calc R . . C39 C 0.53944(12) 0.14876(11) 1.07470(10) 0.0217(3) Uani 1 1 d . . . H39 H 0.5350 0.0911 1.1161 0.026 Uiso 1 1 calc R . . C40 C 0.60407(12) 0.21934(11) 1.08531(10) 0.0229(3) Uani 1 1 d . . . H40 H 0.6433 0.2108 1.1344 0.027 Uiso 1 1 calc R . . C41 C 0.61122(12) 0.30254(11) 1.02389(10) 0.0221(3) Uani 1 1 d . . . H41 H 0.6561 0.3509 1.0301 0.027 Uiso 1 1 calc R . . C42 C 0.55226(11) 0.31530(10) 0.95269(10) 0.0173(2) Uani 1 1 d . . . H42 H 0.5574 0.3731 0.9116 0.021 Uiso 1 1 calc R . . C43 C 0.44299(10) 0.34802(8) 0.78010(9) 0.0116(2) Uani 1 1 d . . . C44 C 0.41973(11) 0.45379(9) 0.80809(10) 0.0166(2) Uani 1 1 d . . . H44 H 0.3777 0.4773 0.8780 0.020 Uiso 1 1 calc R . . C45 C 0.45615(12) 0.52574(9) 0.73695(10) 0.0203(3) Uani 1 1 d . . . H45 H 0.4393 0.5968 0.7589 0.024 Uiso 1 1 calc R . . C46 C 0.51708(12) 0.49373(10) 0.63393(10) 0.0200(2) Uani 1 1 d . . . H46 H 0.5422 0.5425 0.5851 0.024 Uiso 1 1 calc R . . C47 C 0.54074(11) 0.38943(10) 0.60338(9) 0.0174(2) Uani 1 1 d . . . H47 H 0.5818 0.3666 0.5331 0.021 Uiso 1 1 calc R . . C48 C 0.50455(10) 0.31831(9) 0.67531(9) 0.0138(2) Uani 1 1 d . . . H48 H 0.5220 0.2473 0.6529 0.017 Uiso 1 1 calc R . . B1 B 0.40801(11) 0.26417(9) 0.86528(10) 0.0113(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01056(7) 0.01336(7) 0.01015(7) -0.00009(5) -0.00442(5) -0.00279(5) P1 0.01170(14) 0.01276(12) 0.00893(13) 0.00100(9) -0.00370(10) -0.00495(10) P2 0.01013(13) 0.01136(12) 0.00967(13) 0.00087(9) -0.00333(10) -0.00319(10) F1 0.0304(5) 0.0314(4) 0.0090(3) 0.0032(3) -0.0026(3) -0.0011(3) F2 0.0525(6) 0.0448(6) 0.0340(5) 0.0020(4) -0.0056(4) -0.0406(5) F3 0.0233(4) 0.0224(4) 0.0292(4) -0.0083(3) -0.0025(3) 0.0005(3) F4 0.0526(6) 0.0403(5) 0.0138(4) 0.0036(3) -0.0177(4) -0.0183(4) F5 0.0365(5) 0.0225(4) 0.0198(4) -0.0052(3) -0.0104(3) -0.0108(3) F6 0.0486(6) 0.0179(4) 0.0327(5) 0.0128(3) -0.0233(4) -0.0128(4) F7 0.0154(4) 0.0361(5) 0.0233(4) -0.0045(3) 0.0036(3) 0.0009(3) F8 0.0354(5) 0.0352(5) 0.0155(4) -0.0021(3) -0.0160(3) 0.0004(4) N1 0.0091(4) 0.0160(4) 0.0117(4) 0.0001(3) -0.0039(3) -0.0031(3) N2 0.0106(4) 0.0154(4) 0.0093(4) 0.0008(3) -0.0044(3) -0.0032(3) N3 0.0120(5) 0.0139(4) 0.0131(5) -0.0008(3) -0.0038(4) -0.0042(3) N4 0.0108(4) 0.0117(4) 0.0122(4) 0.0018(3) -0.0039(3) -0.0019(3) C1 0.0126(5) 0.0150(5) 0.0112(5) 0.0023(4) -0.0035(4) -0.0045(4) C2 0.0155(6) 0.0141(5) 0.0124(5) 0.0012(4) -0.0054(4) -0.0007(4) C3 0.0158(6) 0.0207(6) 0.0100(5) 0.0026(4) -0.0020(4) 0.0023(4) C4 0.0154(6) 0.0233(6) 0.0195(6) 0.0080(5) -0.0008(5) -0.0048(5) C5 0.0235(7) 0.0242(6) 0.0234(7) 0.0024(5) -0.0039(5) -0.0154(5) C6 0.0217(6) 0.0246(6) 0.0138(6) 0.0003(4) -0.0031(5) -0.0138(5) C7 0.0151(5) 0.0155(5) 0.0092(5) 0.0003(4) -0.0025(4) -0.0085(4) C8 0.0154(5) 0.0167(5) 0.0123(5) 0.0003(4) -0.0028(4) -0.0071(4) C9 0.0171(6) 0.0176(5) 0.0186(6) -0.0034(4) -0.0003(5) -0.0065(4) C10 0.0251(7) 0.0278(6) 0.0126(6) -0.0051(5) 0.0003(5) -0.0135(5) C11 0.0309(7) 0.0291(6) 0.0101(5) 0.0029(5) -0.0077(5) -0.0175(6) C12 0.0214(6) 0.0193(5) 0.0131(5) 0.0019(4) -0.0074(5) -0.0096(5) C13 0.0123(5) 0.0170(5) 0.0102(5) 0.0005(4) -0.0043(4) -0.0045(4) C14 0.0141(6) 0.0241(6) 0.0188(6) 0.0055(4) -0.0062(5) -0.0082(5) C15 0.0119(6) 0.0322(7) 0.0192(6) 0.0058(5) -0.0064(5) -0.0065(5) C16 0.0141(6) 0.0239(6) 0.0203(6) 0.0043(5) -0.0073(5) -0.0006(5) C17 0.0143(6) 0.0184(5) 0.0159(6) 0.0028(4) -0.0048(4) -0.0027(4) C18 0.0102(5) 0.0160(5) 0.0093(5) 0.0000(4) -0.0029(4) -0.0030(4) C19 0.0109(5) 0.0124(5) 0.0140(5) 0.0004(4) -0.0035(4) -0.0035(4) C20 0.0139(5) 0.0149(5) 0.0137(5) 0.0002(4) -0.0037(4) -0.0036(4) C21 0.0178(6) 0.0177(5) 0.0161(6) -0.0036(4) -0.0045(4) -0.0059(4) C22 0.0234(6) 0.0135(5) 0.0252(7) -0.0001(4) -0.0072(5) -0.0061(5) C23 0.0230(6) 0.0157(5) 0.0212(6) 0.0065(4) -0.0096(5) -0.0070(5) C24 0.0185(6) 0.0162(5) 0.0168(6) 0.0024(4) -0.0073(5) -0.0057(4) C25 0.0138(5) 0.0107(5) 0.0113(5) 0.0017(4) -0.0029(4) -0.0037(4) C26 0.0149(6) 0.0147(5) 0.0151(5) -0.0002(4) -0.0037(4) -0.0042(4) C27 0.0159(6) 0.0164(5) 0.0171(6) -0.0005(4) 0.0011(5) -0.0016(4) C28 0.0272(7) 0.0175(5) 0.0121(5) -0.0004(4) -0.0022(5) -0.0012(5) C29 0.0257(7) 0.0166(5) 0.0131(5) 0.0015(4) -0.0101(5) -0.0023(5) C30 0.0167(6) 0.0157(5) 0.0133(5) 0.0013(4) -0.0056(4) -0.0020(4) C31 0.0161(6) 0.0283(6) 0.0120(5) -0.0047(4) -0.0055(4) -0.0034(5) C32 0.0159(6) 0.0319(7) 0.0132(6) -0.0076(5) -0.0021(5) -0.0009(5) C33 0.0110(5) 0.0219(6) 0.0138(5) -0.0022(4) -0.0029(4) -0.0015(4) C34 0.0119(5) 0.0146(5) 0.0194(6) 0.0028(4) -0.0038(4) -0.0005(4) C35 0.0158(6) 0.0134(5) 0.0245(6) -0.0026(4) -0.0014(5) -0.0010(4) C36 0.0149(6) 0.0151(5) 0.0187(6) -0.0040(4) -0.0018(4) -0.0049(4) C37 0.0097(5) 0.0189(5) 0.0116(5) 0.0012(4) -0.0032(4) -0.0025(4) C38 0.0151(6) 0.0222(6) 0.0167(6) 0.0045(4) -0.0055(5) -0.0026(4) C39 0.0192(6) 0.0280(6) 0.0145(6) 0.0042(5) -0.0056(5) 0.0025(5) C40 0.0162(6) 0.0355(7) 0.0144(6) -0.0054(5) -0.0083(5) 0.0063(5) C41 0.0166(6) 0.0316(7) 0.0191(6) -0.0057(5) -0.0081(5) -0.0034(5) C42 0.0154(6) 0.0224(6) 0.0151(6) 0.0004(4) -0.0057(4) -0.0051(4) C43 0.0096(5) 0.0138(5) 0.0132(5) 0.0019(4) -0.0055(4) -0.0034(4) C44 0.0181(6) 0.0152(5) 0.0160(6) 0.0001(4) -0.0049(4) -0.0039(4) C45 0.0255(7) 0.0135(5) 0.0241(6) 0.0035(4) -0.0097(5) -0.0061(5) C46 0.0237(6) 0.0205(6) 0.0202(6) 0.0093(5) -0.0095(5) -0.0110(5) C47 0.0184(6) 0.0229(6) 0.0133(5) 0.0045(4) -0.0057(4) -0.0092(5) C48 0.0141(5) 0.0151(5) 0.0135(5) 0.0014(4) -0.0053(4) -0.0051(4) B1 0.0100(5) 0.0125(5) 0.0113(5) 0.0007(4) -0.0034(4) -0.0029(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 1.9959(10) . ? Cu1 N3 2.0091(10) . ? Cu1 P2 2.2524(4) . ? Cu1 P1 2.2685(3) . ? P1 C1 1.8290(12) . ? P1 C13 1.8323(12) . ? P1 C7 1.8335(11) . ? P2 C19 1.8258(11) . ? P2 C25 1.8315(11) . ? P2 C18 1.8335(12) . ? F1 C3 1.3588(14) . ? F2 C5 1.3477(15) . ? F3 C9 1.3491(15) . ? F4 C11 1.3534(16) . ? F5 C21 1.3535(14) . ? F6 C23 1.3571(15) . ? F7 C27 1.3510(15) . ? F8 C29 1.3501(15) . ? N1 C33 1.3417(15) . ? N1 N2 1.3615(14) . ? N2 C31 1.3524(14) . ? N2 B1 1.5801(16) . ? N3 C36 1.3415(14) . ? N3 N4 1.3679(14) . ? N4 C34 1.3522(15) . ? N4 B1 1.5786(15) . ? C1 C6 1.3951(16) . ? C1 C2 1.3974(16) . ? C2 C3 1.3784(17) . ? C3 C4 1.3766(19) . ? C4 C5 1.3786(19) . ? C5 C6 1.3842(18) . ? C7 C12 1.3942(17) . ? C7 C8 1.4014(17) . ? C8 C9 1.3796(16) . ? C9 C10 1.382(2) . ? C10 C11 1.372(2) . ? C11 C12 1.3869(17) . ? C13 C14 1.3983(17) . ? C13 C18 1.4096(16) . ? C14 C15 1.3912(18) . ? C15 C16 1.3858(19) . ? C16 C17 1.3914(18) . ? C17 C18 1.4004(16) . ? C19 C20 1.3965(16) . ? C19 C24 1.3974(17) . ? C20 C21 1.3845(16) . ? C21 C22 1.3790(19) . ? C22 C23 1.3823(18) . ? C23 C24 1.3802(17) . ? C25 C30 1.3959(17) . ? C25 C26 1.3967(16) . ? C26 C27 1.3835(17) . ? C27 C28 1.380(2) . ? C28 C29 1.3801(19) . ? C29 C30 1.3841(17) . ? C31 C32 1.3782(18) . ? C32 C33 1.3930(17) . ? C34 C35 1.3809(18) . ? C35 C36 1.3918(19) . ? C37 C42 1.3968(17) . ? C37 C38 1.4082(17) . ? C37 B1 1.6214(17) . ? C38 C39 1.3902(18) . ? C39 C40 1.384(2) . ? C40 C41 1.385(2) . ? C41 C42 1.3972(18) . ? C43 C44 1.4010(16) . ? C43 C48 1.4065(16) . ? C43 B1 1.6246(17) . ? C44 C45 1.3932(17) . ? C45 C46 1.3906(19) . ? C46 C47 1.3898(18) . ? C47 C48 1.3909(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N3 97.03(4) . . ? N1 Cu1 P2 112.85(3) . . ? N3 Cu1 P2 123.72(3) . . ? N1 Cu1 P1 120.03(3) . . ? N3 Cu1 P1 118.37(3) . . ? P2 Cu1 P1 86.932(13) . . ? C1 P1 C13 103.96(5) . . ? C1 P1 C7 103.22(5) . . ? C13 P1 C7 102.69(5) . . ? C1 P1 Cu1 129.78(4) . . ? C13 P1 Cu1 103.31(4) . . ? C7 P1 Cu1 110.78(4) . . ? C19 P2 C25 102.54(5) . . ? C19 P2 C18 103.24(5) . . ? C25 P2 C18 103.36(5) . . ? C19 P2 Cu1 123.96(4) . . ? C25 P2 Cu1 117.75(4) . . ? C18 P2 Cu1 103.33(4) . . ? C33 N1 N2 106.95(9) . . ? C33 N1 Cu1 130.95(8) . . ? N2 N1 Cu1 122.09(7) . . ? C31 N2 N1 109.00(9) . . ? C31 N2 B1 126.12(10) . . ? N1 N2 B1 123.96(9) . . ? C36 N3 N4 106.54(10) . . ? C36 N3 Cu1 131.76(9) . . ? N4 N3 Cu1 121.50(7) . . ? C34 N4 N3 109.02(9) . . ? C34 N4 B1 125.14(10) . . ? N3 N4 B1 121.92(9) . . ? C6 C1 C2 119.96(11) . . ? C6 C1 P1 122.49(9) . . ? C2 C1 P1 117.52(9) . . ? C3 C2 C1 118.03(11) . . ? F1 C3 C4 117.65(11) . . ? F1 C3 C2 118.23(12) . . ? C4 C3 C2 124.11(11) . . ? C3 C4 C5 116.05(12) . . ? F2 C5 C4 118.26(12) . . ? F2 C5 C6 118.54(12) . . ? C4 C5 C6 123.20(12) . . ? C5 C6 C1 118.65(11) . . ? C12 C7 C8 119.95(11) . . ? C12 C7 P1 121.88(9) . . ? C8 C7 P1 117.82(9) . . ? C9 C8 C7 118.54(11) . . ? F3 C9 C8 118.35(12) . . ? F3 C9 C10 118.33(11) . . ? C8 C9 C10 123.31(12) . . ? C11 C10 C9 116.24(11) . . ? F4 C11 C10 118.84(11) . . ? F4 C11 C12 117.31(13) . . ? C10 C11 C12 123.85(12) . . ? C11 C12 C7 118.09(12) . . ? C14 C13 C18 119.54(11) . . ? C14 C13 P1 122.74(9) . . ? C18 C13 P1 117.72(9) . . ? C15 C14 C13 120.39(12) . . ? C16 C15 C14 120.16(12) . . ? C15 C16 C17 120.14(12) . . ? C16 C17 C18 120.46(12) . . ? C17 C18 C13 119.26(11) . . ? C17 C18 P2 123.21(9) . . ? C13 C18 P2 117.53(9) . . ? C20 C19 C24 120.18(10) . . ? C20 C19 P2 116.75(9) . . ? C24 C19 P2 123.00(9) . . ? C21 C20 C19 118.13(11) . . ? F5 C21 C22 118.24(11) . . ? F5 C21 C20 118.15(11) . . ? C22 C21 C20 123.61(11) . . ? C21 C22 C23 116.20(11) . . ? F6 C23 C24 118.16(12) . . ? F6 C23 C22 118.45(11) . . ? C24 C23 C22 123.38(12) . . ? C23 C24 C19 118.44(11) . . ? C30 C25 C26 120.25(11) . . ? C30 C25 P2 123.58(9) . . ? C26 C25 P2 116.16(9) . . ? C27 C26 C25 118.19(12) . . ? F7 C27 C28 118.15(11) . . ? F7 C27 C26 118.32(12) . . ? C28 C27 C26 123.53(12) . . ? C27 C28 C29 116.30(11) . . ? F8 C29 C28 118.39(11) . . ? F8 C29 C30 118.25(12) . . ? C28 C29 C30 123.36(12) . . ? C29 C30 C25 118.35(11) . . ? N2 C31 C32 109.05(11) . . ? C31 C32 C33 104.62(10) . . ? N1 C33 C32 110.38(11) . . ? N4 C34 C35 109.15(11) . . ? C34 C35 C36 104.40(11) . . ? N3 C36 C35 110.88(11) . . ? C42 C37 C38 116.41(11) . . ? C42 C37 B1 122.90(11) . . ? C38 C37 B1 120.42(11) . . ? C39 C38 C37 121.82(13) . . ? C40 C39 C38 120.23(13) . . ? C39 C40 C41 119.54(12) . . ? C40 C41 C42 119.90(13) . . ? C37 C42 C41 122.09(12) . . ? C44 C43 C48 116.12(10) . . ? C44 C43 B1 121.68(10) . . ? C48 C43 B1 122.09(10) . . ? C45 C44 C43 122.28(11) . . ? C46 C45 C44 120.12(11) . . ? C47 C46 C45 119.07(11) . . ? C46 C47 C48 120.22(11) . . ? C47 C48 C43 122.18(11) . . ? N4 B1 N2 110.21(9) . . ? N4 B1 C37 108.92(9) . . ? N2 B1 C37 105.57(9) . . ? N4 B1 C43 107.21(9) . . ? N2 B1 C43 110.57(9) . . ? C37 B1 C43 114.36(9) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.426 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.057 data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 898695' #TrackingRef 'Complex3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H32 B Cu F24 N4 P2' _chemical_formula_sum 'C56 H32 B Cu F24 N4 P2' _chemical_formula_weight 1353.15 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 12.6861(16) _cell_length_b 20.390(3) _cell_length_c 44.345(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11471(2) _cell_formula_units_Z 8 _cell_measurement_temperature 90 _cell_measurement_reflns_used 22643 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 31.40 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5408 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku AFC-8 with Saturn70 CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75702 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -62 _diffrn_reflns_limit_l_max 62 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 30.05 _reflns_number_total 16699 _reflns_number_gt 14202 _reflns_threshold_expression I>2\s(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution SIR2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0643P)^2^+13.5585P] 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 16699 _refine_ls_number_parameters 820 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1642 _refine_ls_wR_factor_gt 0.1561 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _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 0.03298(2) 0.156332(15) 0.605518(6) 0.01825(8) Uani 1 1 d . . . P1 P 0.19591(5) 0.19845(3) 0.602915(13) 0.01841(12) Uani 1 1 d . . . P2 P 0.07099(5) 0.12222(3) 0.652023(13) 0.01941(13) Uani 1 1 d . . . F1 F 0.15929(15) 0.09891(10) 0.49134(5) 0.0581(6) Uani 1 1 d . . . F2 F 0.28365(17) 0.04078(9) 0.50798(4) 0.0480(5) Uani 1 1 d . . . F3 F 0.3115(2) 0.10258(13) 0.47087(4) 0.0725(8) Uani 1 1 d . . . F4 F 0.54813(16) 0.30279(13) 0.54531(6) 0.0738(9) Uani 1 1 d . . . F5 F 0.43094(17) 0.35646(10) 0.52343(6) 0.0588(6) Uani 1 1 d . . . F6 F 0.5175(3) 0.28954(14) 0.49804(7) 0.1010(12) Uani 1 1 d . . . F7 F 0.0483(2) 0.47340(16) 0.59908(9) 0.1080(13) Uani 1 1 d . . . F8 F 0.2019(2) 0.50800(10) 0.59824(5) 0.0587(6) Uani 1 1 d . . . F9 F 0.1545(4) 0.44362(12) 0.56440(5) 0.1403(19) Uani 1 1 d . . . F10 F 0.3458(2) 0.33163(12) 0.70093(5) 0.0635(6) Uani 1 1 d . . . F11 F 0.1845(2) 0.33950(15) 0.71025(5) 0.0800(9) Uani 1 1 d . . . F12 F 0.2764(2) 0.42565(10) 0.70010(4) 0.0546(6) Uani 1 1 d . . . F13 F -0.10295(17) -0.12485(12) 0.61427(6) 0.0680(7) Uani 1 1 d . . . F14 F 0.0021(2) -0.18368(10) 0.64070(6) 0.0707(7) Uani 1 1 d . . . F15 F 0.06308(17) -0.11779(10) 0.60816(5) 0.0500(5) Uani 1 1 d . . . F16 F -0.0784(10) -0.1047(4) 0.7423(2) 0.107(5) Uani 0.60 1 d P . . F17 F -0.1860(6) -0.0308(5) 0.73658(18) 0.079(3) Uani 0.60 1 d P . . F18 F -0.0376(9) -0.0073(5) 0.75403(12) 0.107(4) Uani 0.60 1 d P . . F19 F -0.22592(18) 0.30099(13) 0.67642(5) 0.0628(6) Uani 1 1 d . . . F20 F -0.1828(3) 0.35188(16) 0.71634(6) 0.1023(12) Uani 1 1 d . . . F21 F -0.0992(2) 0.36850(12) 0.67527(8) 0.0862(9) Uani 1 1 d . . . F22 F 0.0705(3) 0.15155(14) 0.77703(5) 0.0863(10) Uani 1 1 d . . . F23 F 0.19904(19) 0.21088(17) 0.76542(5) 0.0834(9) Uani 1 1 d . . . F24 F 0.0630(2) 0.25400(14) 0.78456(5) 0.0819(9) Uani 1 1 d . . . F25 F -0.1306(16) -0.1001(8) 0.7358(3) 0.129(8) Uani 0.40 1 d P . . F26 F -0.1409(17) -0.0015(9) 0.7438(3) 0.124(7) Uani 0.40 1 d P . . F27 F -0.0054(8) -0.0541(11) 0.7513(2) 0.109(4) Uani 0.40 1 d P . . N1 N -0.08098(16) 0.22044(10) 0.59607(4) 0.0205(4) Uani 1 1 d . . . N2 N -0.16879(16) 0.20185(11) 0.58074(4) 0.0223(4) Uani 1 1 d . . . N3 N -0.00915(16) 0.08580(10) 0.57718(4) 0.0201(4) Uani 1 1 d . . . N4 N -0.10576(16) 0.08748(10) 0.56376(4) 0.0207(4) Uani 1 1 d . . . C1 C 0.27206(19) 0.20056(12) 0.56801(5) 0.0207(4) Uani 1 1 d . . . C2 C 0.24324(19) 0.15415(12) 0.54639(5) 0.0214(5) Uani 1 1 d . . . H2 H 0.1898 0.1230 0.5509 0.026 Uiso 1 1 calc R . . C3 C 0.29162(19) 0.15283(12) 0.51831(5) 0.0214(5) Uani 1 1 d . . . C4 C 0.3664(2) 0.19933(13) 0.51085(6) 0.0246(5) Uani 1 1 d . . . H4 H 0.3979 0.1995 0.4914 0.030 Uiso 1 1 calc R . . C5 C 0.3947(2) 0.24598(12) 0.53233(6) 0.0242(5) Uani 1 1 d . . . C6 C 0.3499(2) 0.24639(12) 0.56076(6) 0.0235(5) Uani 1 1 d . . . H6 H 0.3719 0.2777 0.5753 0.028 Uiso 1 1 calc R . . C7 C 0.20799(18) 0.28162(12) 0.61787(5) 0.0207(4) Uani 1 1 d . . . C8 C 0.1794(2) 0.33494(13) 0.59987(6) 0.0245(5) Uani 1 1 d . . . H8 H 0.1610 0.3281 0.5793 0.029 Uiso 1 1 calc R . . C9 C 0.1776(2) 0.39776(13) 0.61184(6) 0.0285(5) Uani 1 1 d . . . C10 C 0.2031(2) 0.40884(14) 0.64208(6) 0.0307(6) Uani 1 1 d . . . H10 H 0.2013 0.4519 0.6503 0.037 Uiso 1 1 calc R . . C11 C 0.2308(2) 0.35593(14) 0.65982(6) 0.0282(5) Uani 1 1 d . . . C12 C 0.2344(2) 0.29251(13) 0.64796(5) 0.0243(5) Uani 1 1 d . . . H12 H 0.2548 0.2568 0.6604 0.029 Uiso 1 1 calc R . . C13 C 0.27189(19) 0.15038(12) 0.63013(5) 0.0209(5) Uani 1 1 d . . . C14 C 0.3820(2) 0.14672(13) 0.62929(6) 0.0267(5) Uani 1 1 d . . . H14 H 0.4199 0.1694 0.6140 0.032 Uiso 1 1 calc R . . C15 C 0.4361(2) 0.11005(15) 0.65071(7) 0.0335(6) Uani 1 1 d . . . H15 H 0.5108 0.1077 0.6501 0.040 Uiso 1 1 calc R . . C16 C 0.3807(2) 0.07686(14) 0.67302(6) 0.0314(6) Uani 1 1 d . . . H16 H 0.4179 0.0520 0.6877 0.038 Uiso 1 1 calc R . . C17 C 0.2715(2) 0.07982(13) 0.67398(6) 0.0261(5) Uani 1 1 d . . . H17 H 0.2344 0.0567 0.6892 0.031 Uiso 1 1 calc R . . C18 C 0.21576(19) 0.11654(12) 0.65266(5) 0.0213(5) Uani 1 1 d . . . C19 C 0.02822(19) 0.04180(13) 0.66559(5) 0.0229(5) Uani 1 1 d . . . C20 C 0.0279(2) -0.00892(13) 0.64439(6) 0.0253(5) Uani 1 1 d . . . H20 H 0.0525 -0.0010 0.6245 0.030 Uiso 1 1 calc R . . C21 C -0.0081(2) -0.07085(14) 0.65233(6) 0.0282(5) Uani 1 1 d . . . C22 C -0.0452(2) -0.08324(15) 0.68111(7) 0.0331(6) Uani 1 1 d . . . H22 H -0.0700 -0.1257 0.6864 0.040 Uiso 1 1 calc R . . C23 C -0.0456(2) -0.03282(15) 0.70212(6) 0.0323(6) Uani 1 1 d . . . C24 C -0.0100(2) 0.02949(14) 0.69445(6) 0.0275(5) Uani 1 1 d . . . H24 H -0.0117 0.0637 0.7090 0.033 Uiso 1 1 calc R . . C25 C 0.0388(2) 0.17824(13) 0.68316(5) 0.0225(5) Uani 1 1 d . . . C26 C -0.0369(2) 0.22556(14) 0.67727(6) 0.0270(5) Uani 1 1 d . . . H26 H -0.0681 0.2281 0.6578 0.032 Uiso 1 1 calc R . . C27 C -0.0673(2) 0.26941(14) 0.69980(6) 0.0302(6) Uani 1 1 d . . . C28 C -0.0254(2) 0.26513(15) 0.72866(6) 0.0322(6) Uani 1 1 d . . . H28 H -0.0479 0.2941 0.7441 0.039 Uiso 1 1 calc R . . C29 C 0.0500(2) 0.21777(15) 0.73433(6) 0.0301(6) Uani 1 1 d . . . C30 C 0.0841(2) 0.17527(14) 0.71185(5) 0.0270(5) Uani 1 1 d . . . H30 H 0.1381 0.1443 0.7160 0.032 Uiso 1 1 calc R . . C31 C 0.2608(2) 0.09965(13) 0.49689(5) 0.0252(5) Uani 1 1 d . . . C32 C 0.4745(2) 0.29806(14) 0.52449(7) 0.0307(6) Uani 1 1 d . . . C33 C 0.1460(3) 0.45480(15) 0.59250(8) 0.0417(7) Uani 1 1 d . . . C34 C 0.2560(3) 0.36436(16) 0.69268(7) 0.0405(7) Uani 1 1 d . . . C35 C -0.0127(2) -0.12377(15) 0.62891(8) 0.0376(7) Uani 1 1 d . . . C36 C -0.0836(3) -0.0449(2) 0.73357(8) 0.0476(9) Uani 1 1 d . . . C37 C -0.1438(3) 0.32262(19) 0.69203(8) 0.0497(9) Uani 1 1 d . . . C38 C 0.0958(3) 0.20978(18) 0.76547(7) 0.0439(8) Uani 1 1 d . . . C39 C -0.2290(2) 0.25528(14) 0.57565(7) 0.0317(6) Uani 1 1 d . . . H39 H -0.2951 0.2553 0.5656 0.038 Uiso 1 1 calc R . . C40 C -0.1800(2) 0.30962(15) 0.58735(7) 0.0339(6) Uani 1 1 d . . . H40 H -0.2040 0.3538 0.5870 0.041 Uiso 1 1 calc R . . C41 C -0.0874(2) 0.28548(13) 0.59981(6) 0.0259(5) Uani 1 1 d . . . H41 H -0.0357 0.3115 0.6096 0.031 Uiso 1 1 calc R . . C42 C -0.1103(2) 0.03967(13) 0.54282(6) 0.0276(5) Uani 1 1 d . . . H42 H -0.1696 0.0302 0.5305 0.033 Uiso 1 1 calc R . . C43 C -0.0157(2) 0.00669(14) 0.54213(6) 0.0281(5) Uani 1 1 d . . . H43 H 0.0038 -0.0289 0.5295 0.034 Uiso 1 1 calc R . . C44 C 0.04460(19) 0.03715(12) 0.56412(5) 0.0227(5) Uani 1 1 d . . . H44 H 0.1147 0.0251 0.5692 0.027 Uiso 1 1 calc R . . C45 C -0.22756(19) 0.09839(14) 0.61066(5) 0.0258(5) Uani 1 1 d . . . C46 C -0.2484(2) 0.13839(17) 0.63525(6) 0.0328(6) Uani 1 1 d . . . H46 H -0.2465 0.1847 0.6328 0.039 Uiso 1 1 calc R . . C47 C -0.2723(2) 0.1121(2) 0.66357(7) 0.0479(9) Uani 1 1 d . . . H47 H -0.2843 0.1405 0.6802 0.057 Uiso 1 1 calc R . . C48 C -0.2784(2) 0.0448(2) 0.66750(7) 0.0523(10) Uani 1 1 d . . . H48 H -0.2954 0.0268 0.6867 0.063 Uiso 1 1 calc R . . C49 C -0.2596(2) 0.00451(19) 0.64327(8) 0.0460(9) Uani 1 1 d . . . H49 H -0.2649 -0.0417 0.6456 0.055 Uiso 1 1 calc R . . C50 C -0.2329(2) 0.03066(16) 0.61537(7) 0.0341(6) Uani 1 1 d . . . H50 H -0.2179 0.0018 0.5991 0.041 Uiso 1 1 calc R . . C51 C -0.29566(19) 0.12159(13) 0.55292(5) 0.0241(5) Uani 1 1 d . . . C52 C -0.3859(2) 0.08392(14) 0.55773(6) 0.0287(5) Uani 1 1 d . . . H52 H -0.3996 0.0669 0.5773 0.034 Uiso 1 1 calc R . . C53 C -0.4565(2) 0.07072(15) 0.53433(7) 0.0346(6) Uani 1 1 d . . . H53 H -0.5170 0.0445 0.5381 0.042 Uiso 1 1 calc R . . C54 C -0.4392(2) 0.09532(16) 0.50586(7) 0.0365(7) Uani 1 1 d . . . H54 H -0.4862 0.0851 0.4899 0.044 Uiso 1 1 calc R . . C55 C -0.3523(2) 0.13526(17) 0.50077(6) 0.0363(7) Uani 1 1 d . . . H55 H -0.3409 0.1540 0.4814 0.044 Uiso 1 1 calc R . . C56 C -0.2822(2) 0.14771(15) 0.52407(6) 0.0305(6) Uani 1 1 d . . . H56 H -0.2230 0.1750 0.5203 0.037 Uiso 1 1 calc R . . B1 B -0.2013(2) 0.12772(14) 0.57745(6) 0.0209(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01803(14) 0.01843(16) 0.01829(13) -0.00266(10) -0.00339(9) 0.00018(11) P1 0.0189(3) 0.0167(3) 0.0196(3) -0.0029(2) -0.0022(2) -0.0009(2) P2 0.0218(3) 0.0185(3) 0.0179(3) -0.0010(2) -0.0026(2) -0.0002(2) F1 0.0366(10) 0.0507(13) 0.0871(16) -0.0397(11) -0.0327(10) 0.0153(9) F2 0.0716(14) 0.0234(9) 0.0491(11) -0.0127(8) -0.0265(10) 0.0094(9) F3 0.109(2) 0.0789(17) 0.0296(9) -0.0247(10) 0.0238(11) -0.0527(15) F4 0.0344(11) 0.0799(18) 0.107(2) 0.0561(15) -0.0341(12) -0.0318(11) F5 0.0455(11) 0.0248(10) 0.1061(19) 0.0191(11) -0.0183(12) -0.0111(9) F6 0.134(3) 0.0759(18) 0.0928(19) -0.0431(15) 0.0819(19) -0.0726(18) F7 0.0498(15) 0.081(2) 0.193(4) 0.071(2) -0.0085(18) 0.0166(14) F8 0.0868(17) 0.0262(10) 0.0632(13) 0.0063(9) 0.0026(12) -0.0085(11) F9 0.352(6) 0.0326(13) 0.0365(12) -0.0041(9) -0.052(2) 0.055(2) F10 0.0930(18) 0.0635(15) 0.0339(10) -0.0081(9) -0.0186(11) 0.0147(13) F11 0.0957(19) 0.111(2) 0.0327(10) -0.0177(12) 0.0190(11) -0.0622(17) F12 0.0916(17) 0.0311(10) 0.0409(10) -0.0109(8) -0.0164(10) -0.0110(11) F13 0.0366(11) 0.0738(16) 0.0934(18) -0.0484(14) -0.0234(11) 0.0034(11) F14 0.115(2) 0.0213(10) 0.0760(16) 0.0002(10) -0.0043(15) -0.0039(12) F15 0.0495(12) 0.0389(11) 0.0616(13) -0.0227(9) 0.0050(9) -0.0079(9) F16 0.178(10) 0.062(5) 0.081(6) 0.054(5) 0.062(6) 0.056(7) F17 0.060(3) 0.127(9) 0.049(3) 0.021(4) 0.022(2) 0.012(3) F18 0.165(10) 0.132(6) 0.026(2) -0.007(3) 0.015(4) -0.099(7) F19 0.0499(12) 0.0790(17) 0.0594(13) -0.0113(12) -0.0153(10) 0.0326(12) F20 0.128(3) 0.119(2) 0.0596(15) -0.0430(16) -0.0219(15) 0.095(2) F21 0.090(2) 0.0412(14) 0.127(3) 0.0265(15) -0.0133(18) 0.0230(14) F22 0.141(3) 0.0760(18) 0.0424(12) 0.0224(12) -0.0371(15) -0.0203(17) F23 0.0558(15) 0.156(3) 0.0384(11) -0.0123(14) -0.0215(10) 0.0050(16) F24 0.119(2) 0.095(2) 0.0314(10) -0.0305(11) -0.0230(12) 0.0420(17) F25 0.213(17) 0.129(14) 0.046(5) 0.006(6) 0.031(8) -0.135(14) F26 0.188(18) 0.112(11) 0.072(9) 0.055(8) 0.083(11) 0.080(11) F27 0.081(6) 0.214(14) 0.032(4) 0.035(7) -0.022(4) -0.034(10) N1 0.0188(9) 0.0202(10) 0.0224(9) -0.0019(7) -0.0025(7) 0.0006(8) N2 0.0199(9) 0.0246(11) 0.0224(9) -0.0015(8) -0.0037(7) 0.0033(8) N3 0.0195(9) 0.0198(10) 0.0208(9) -0.0028(7) -0.0032(7) -0.0016(8) N4 0.0200(9) 0.0219(10) 0.0201(9) -0.0018(7) -0.0035(7) -0.0025(8) C1 0.0211(11) 0.0195(12) 0.0214(10) -0.0026(8) 0.0002(8) 0.0016(9) C2 0.0221(11) 0.0199(12) 0.0223(10) -0.0012(9) -0.0016(8) -0.0026(9) C3 0.0231(11) 0.0188(12) 0.0223(10) -0.0020(8) -0.0017(8) 0.0006(9) C4 0.0261(12) 0.0222(13) 0.0255(11) 0.0010(9) 0.0032(9) 0.0028(10) C5 0.0234(12) 0.0187(12) 0.0306(12) 0.0012(9) 0.0022(9) -0.0013(10) C6 0.0236(11) 0.0187(12) 0.0281(11) -0.0029(9) -0.0002(9) -0.0010(9) C7 0.0198(11) 0.0171(12) 0.0253(11) -0.0028(8) -0.0002(8) -0.0018(9) C8 0.0257(12) 0.0199(12) 0.0278(11) -0.0024(9) -0.0018(9) 0.0003(10) C9 0.0308(13) 0.0196(13) 0.0350(13) -0.0003(10) 0.0024(10) 0.0016(10) C10 0.0371(15) 0.0202(13) 0.0350(13) -0.0083(10) 0.0087(11) -0.0033(11) C11 0.0351(14) 0.0235(13) 0.0261(12) -0.0073(10) 0.0046(10) -0.0086(11) C12 0.0281(12) 0.0215(12) 0.0234(11) -0.0036(9) 0.0022(9) -0.0043(10) C13 0.0214(11) 0.0163(11) 0.0249(10) -0.0049(8) -0.0033(8) 0.0010(9) C14 0.0221(12) 0.0240(13) 0.0341(13) -0.0021(10) -0.0054(10) -0.0013(10) C15 0.0237(12) 0.0336(16) 0.0432(15) -0.0041(12) -0.0100(11) 0.0031(11) C16 0.0321(14) 0.0253(14) 0.0369(14) -0.0016(11) -0.0151(11) 0.0038(11) C17 0.0308(13) 0.0202(13) 0.0272(11) -0.0010(9) -0.0075(10) 0.0026(10) C18 0.0238(11) 0.0181(12) 0.0219(10) -0.0039(8) -0.0055(8) 0.0005(9) C19 0.0227(11) 0.0227(13) 0.0233(11) 0.0016(9) -0.0034(8) -0.0022(9) C20 0.0248(12) 0.0240(13) 0.0272(11) 0.0001(9) -0.0024(9) -0.0021(10) C21 0.0249(12) 0.0226(13) 0.0370(13) -0.0005(10) -0.0053(10) -0.0023(10) C22 0.0296(14) 0.0263(15) 0.0433(15) 0.0088(12) -0.0037(11) -0.0051(11) C23 0.0324(14) 0.0349(16) 0.0295(13) 0.0097(11) -0.0006(10) -0.0063(12) C24 0.0294(13) 0.0278(14) 0.0255(11) 0.0026(10) -0.0017(10) -0.0028(11) C25 0.0260(12) 0.0217(13) 0.0199(10) -0.0015(9) -0.0006(8) -0.0009(10) C26 0.0289(13) 0.0299(14) 0.0221(11) -0.0017(10) -0.0027(9) 0.0018(11) C27 0.0322(14) 0.0298(15) 0.0285(12) -0.0057(10) 0.0006(10) 0.0082(11) C28 0.0373(15) 0.0312(15) 0.0280(12) -0.0078(11) 0.0026(10) 0.0006(12) C29 0.0381(15) 0.0322(15) 0.0199(11) -0.0034(10) -0.0015(10) -0.0016(12) C30 0.0333(13) 0.0258(14) 0.0217(11) -0.0016(9) -0.0050(9) 0.0010(11) C31 0.0294(13) 0.0239(13) 0.0225(10) -0.0028(9) -0.0019(9) 0.0000(10) C32 0.0297(13) 0.0240(14) 0.0386(14) -0.0007(11) 0.0032(11) -0.0050(11) C33 0.0523(19) 0.0222(15) 0.0506(18) 0.0024(12) -0.0062(15) 0.0045(14) C34 0.060(2) 0.0327(16) 0.0288(13) -0.0101(11) 0.0087(13) -0.0160(15) C35 0.0356(15) 0.0258(15) 0.0514(18) -0.0034(13) -0.0046(13) -0.0040(12) C36 0.056(2) 0.051(2) 0.0357(16) 0.0154(15) 0.0015(15) -0.0127(18) C37 0.058(2) 0.050(2) 0.0417(17) -0.0130(15) -0.0059(15) 0.0270(18) C38 0.058(2) 0.049(2) 0.0243(13) -0.0077(13) -0.0081(13) 0.0055(17) C39 0.0254(13) 0.0300(15) 0.0397(14) -0.0001(11) -0.0078(11) 0.0094(11) C40 0.0332(14) 0.0248(15) 0.0438(15) -0.0019(11) -0.0039(12) 0.0093(11) C41 0.0246(12) 0.0214(13) 0.0316(12) -0.0029(10) -0.0014(9) 0.0009(10) C42 0.0282(13) 0.0269(14) 0.0278(12) -0.0083(10) -0.0060(10) -0.0028(11) C43 0.0309(13) 0.0243(14) 0.0291(12) -0.0098(10) -0.0020(10) -0.0014(11) C44 0.0220(11) 0.0195(12) 0.0266(11) -0.0033(9) 0.0000(9) 0.0010(9) C45 0.0175(11) 0.0360(15) 0.0239(11) 0.0014(10) -0.0024(8) -0.0005(10) C46 0.0217(12) 0.0498(18) 0.0270(12) -0.0027(12) 0.0010(10) -0.0015(12) C47 0.0268(14) 0.091(3) 0.0262(13) -0.0021(16) 0.0063(11) -0.0004(16) C48 0.0267(15) 0.096(3) 0.0346(15) 0.0256(18) 0.0048(12) -0.0019(17) C49 0.0312(15) 0.058(2) 0.0484(18) 0.0268(16) 0.0014(13) 0.0009(15) C50 0.0274(13) 0.0421(18) 0.0329(13) 0.0109(12) 0.0010(11) 0.0003(12) C51 0.0188(11) 0.0292(14) 0.0245(11) -0.0037(9) -0.0037(8) 0.0014(10) C52 0.0223(12) 0.0333(15) 0.0305(12) 0.0009(10) -0.0046(9) -0.0016(11) C53 0.0227(13) 0.0349(17) 0.0462(16) -0.0064(13) -0.0103(11) -0.0022(11) C54 0.0299(14) 0.0428(18) 0.0368(14) -0.0141(13) -0.0141(11) 0.0084(13) C55 0.0341(15) 0.0509(19) 0.0239(12) -0.0040(12) -0.0080(10) 0.0073(13) C56 0.0245(12) 0.0421(17) 0.0249(12) 0.0003(11) -0.0024(9) -0.0021(11) B1 0.0178(11) 0.0241(14) 0.0209(11) -0.0007(10) -0.0009(9) -0.0024(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.983(2) . ? Cu1 N1 1.994(2) . ? Cu1 P2 2.2292(7) . ? Cu1 P1 2.2413(7) . ? P1 C1 1.825(2) . ? P1 C7 1.827(3) . ? P1 C13 1.829(2) . ? P2 C19 1.829(3) . ? P2 C25 1.838(3) . ? P2 C18 1.840(3) . ? F1 C31 1.312(3) . ? F2 C31 1.329(3) . ? F3 C31 1.322(3) . ? F4 C32 1.317(4) . ? F5 C32 1.313(4) . ? F6 C32 1.305(4) . ? F7 C33 1.329(5) . ? F8 C33 1.321(4) . ? F9 C33 1.272(4) . ? F10 C34 1.370(4) . ? F11 C34 1.299(4) . ? F12 C34 1.318(4) . ? F13 C35 1.316(4) . ? F14 C35 1.342(4) . ? F15 C35 1.337(4) . ? F16 F25 0.727(19) . ? F16 C36 1.280(7) . ? F16 F27 1.443(16) . ? F17 F26 0.89(2) . ? F17 C36 1.338(9) . ? F17 F25 1.58(2) . ? F18 F27 1.045(15) . ? F18 C36 1.323(7) . ? F18 F26 1.391(18) . ? F19 C37 1.326(4) . ? F20 C37 1.328(4) . ? F21 C37 1.322(5) . ? F22 C38 1.333(4) . ? F23 C38 1.310(4) . ? F24 C38 1.305(4) . ? F25 C36 1.277(11) . ? F26 C36 1.232(13) . ? F27 C36 1.279(10) . ? N1 C41 1.339(3) . ? N1 N2 1.359(3) . ? N2 C39 1.350(3) . ? N2 B1 1.574(4) . ? N3 C44 1.336(3) . ? N3 N4 1.363(3) . ? N4 C42 1.348(3) . ? N4 B1 1.585(3) . ? C1 C2 1.396(3) . ? C1 C6 1.397(3) . ? C2 C3 1.389(3) . ? C3 C4 1.381(4) . ? C3 C31 1.493(3) . ? C4 C5 1.393(4) . ? C5 C6 1.384(3) . ? C5 C32 1.507(4) . ? C7 C12 1.394(3) . ? C7 C8 1.397(4) . ? C8 C9 1.387(4) . ? C9 C10 1.398(4) . ? C9 C33 1.500(4) . ? C10 C11 1.381(4) . ? C11 C12 1.396(4) . ? C11 C34 1.502(4) . ? C13 C14 1.399(3) . ? C13 C18 1.408(3) . ? C14 C15 1.390(4) . ? C15 C16 1.389(4) . ? C16 C17 1.387(4) . ? C17 C18 1.398(3) . ? C19 C24 1.391(3) . ? C19 C20 1.398(4) . ? C20 C21 1.388(4) . ? C21 C22 1.384(4) . ? C21 C35 1.499(4) . ? C22 C23 1.388(4) . ? C23 C24 1.391(4) . ? C23 C36 1.496(4) . ? C25 C26 1.386(4) . ? C25 C30 1.397(3) . ? C26 C27 1.395(4) . ? C27 C28 1.389(4) . ? C27 C37 1.496(4) . ? C28 C29 1.382(4) . ? C29 C30 1.390(4) . ? C29 C38 1.507(4) . ? C39 C40 1.372(4) . ? C40 C41 1.388(4) . ? C42 C43 1.376(4) . ? C43 C44 1.386(3) . ? C45 C46 1.387(4) . ? C45 C50 1.398(4) . ? C45 B1 1.624(4) . ? C46 C47 1.398(4) . ? C47 C48 1.385(6) . ? C48 C49 1.374(6) . ? C49 C50 1.389(4) . ? C51 C52 1.395(4) . ? C51 C56 1.396(4) . ? C51 B1 1.622(4) . ? C52 C53 1.397(4) . ? C53 C54 1.376(5) . ? C54 C55 1.389(5) . ? C55 C56 1.387(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 N3 Cu1 N1 98.45(8) . . ? N3 Cu1 P2 114.72(6) . . ? N1 Cu1 P2 123.78(6) . . ? N3 Cu1 P1 119.59(6) . . ? N1 Cu1 P1 114.00(6) . . ? P2 Cu1 P1 88.15(2) . . ? C1 P1 C7 103.98(11) . . ? C1 P1 C13 107.04(11) . . ? C7 P1 C13 102.34(11) . . ? C1 P1 Cu1 122.74(8) . . ? C7 P1 Cu1 114.48(8) . . ? C13 P1 Cu1 104.28(8) . . ? C19 P2 C25 104.13(12) . . ? C19 P2 C18 103.57(11) . . ? C25 P2 C18 104.43(11) . . ? C19 P2 Cu1 121.33(8) . . ? C25 P2 Cu1 116.94(8) . . ? C18 P2 Cu1 104.46(8) . . ? F25 F16 C36 73.3(12) . . ? F25 F16 F27 127.0(16) . . ? C36 F16 F27 55.6(6) . . ? F26 F17 C36 63.5(11) . . ? F26 F17 F25 108.8(15) . . ? C36 F17 F25 51.1(6) . . ? F27 F18 C36 64.1(6) . . ? F27 F18 F26 114.1(11) . . ? C36 F18 F26 53.9(7) . . ? F16 F25 C36 73.7(12) . . ? F16 F25 F17 120.8(17) . . ? C36 F25 F17 54.6(7) . . ? F17 F26 C36 76.4(16) . . ? F17 F26 F18 131.9(19) . . ? C36 F26 F18 60.2(7) . . ? F18 F27 C36 68.6(9) . . ? F18 F27 F16 115.7(11) . . ? C36 F27 F16 55.7(5) . . ? C41 N1 N2 106.8(2) . . ? C41 N1 Cu1 131.87(17) . . ? N2 N1 Cu1 121.12(16) . . ? C39 N2 N1 108.8(2) . . ? C39 N2 B1 127.7(2) . . ? N1 N2 B1 121.95(19) . . ? C44 N3 N4 106.75(19) . . ? C44 N3 Cu1 132.52(17) . . ? N4 N3 Cu1 120.05(15) . . ? C42 N4 N3 108.8(2) . . ? C42 N4 B1 127.3(2) . . ? N3 N4 B1 122.26(18) . . ? C2 C1 C6 118.7(2) . . ? C2 C1 P1 115.34(18) . . ? C6 C1 P1 125.80(18) . . ? C3 C2 C1 120.9(2) . . ? C4 C3 C2 120.3(2) . . ? C4 C3 C31 121.7(2) . . ? C2 C3 C31 118.0(2) . . ? C3 C4 C5 118.8(2) . . ? C6 C5 C4 121.4(2) . . ? C6 C5 C32 118.8(2) . . ? C4 C5 C32 119.8(2) . . ? C5 C6 C1 119.8(2) . . ? C12 C7 C8 119.1(2) . . ? C12 C7 P1 121.03(19) . . ? C8 C7 P1 119.55(18) . . ? C9 C8 C7 120.3(2) . . ? C8 C9 C10 120.9(3) . . ? C8 C9 C33 120.1(3) . . ? C10 C9 C33 119.0(3) . . ? C11 C10 C9 118.6(2) . . ? C10 C11 C12 121.2(2) . . ? C10 C11 C34 121.2(3) . . ? C12 C11 C34 117.7(3) . . ? C7 C12 C11 120.0(2) . . ? C14 C13 C18 119.8(2) . . ? C14 C13 P1 122.5(2) . . ? C18 C13 P1 117.67(18) . . ? C15 C14 C13 120.2(3) . . ? C16 C15 C14 119.9(3) . . ? C17 C16 C15 120.4(3) . . ? C16 C17 C18 120.5(3) . . ? C17 C18 C13 119.1(2) . . ? C17 C18 P2 123.3(2) . . ? C13 C18 P2 117.59(18) . . ? C24 C19 C20 119.0(2) . . ? C24 C19 P2 124.6(2) . . ? C20 C19 P2 116.29(19) . . ? C21 C20 C19 120.2(2) . . ? C22 C21 C20 120.8(3) . . ? C22 C21 C35 119.6(3) . . ? C20 C21 C35 119.5(3) . . ? C21 C22 C23 119.0(3) . . ? C22 C23 C24 120.8(3) . . ? C22 C23 C36 120.3(3) . . ? C24 C23 C36 118.9(3) . . ? C23 C24 C19 120.2(3) . . ? C26 C25 C30 119.1(2) . . ? C26 C25 P2 116.41(18) . . ? C30 C25 P2 124.5(2) . . ? C25 C26 C27 120.2(2) . . ? C28 C27 C26 120.9(3) . . ? C28 C27 C37 120.4(3) . . ? C26 C27 C37 118.7(3) . . ? C29 C28 C27 118.5(2) . . ? C28 C29 C30 121.4(2) . . ? C28 C29 C38 120.6(3) . . ? C30 C29 C38 118.0(3) . . ? C29 C30 C25 119.9(3) . . ? F1 C31 F3 108.3(2) . . ? F1 C31 F2 105.8(2) . . ? F3 C31 F2 104.9(2) . . ? F1 C31 C3 112.6(2) . . ? F3 C31 C3 113.3(2) . . ? F2 C31 C3 111.3(2) . . ? F6 C32 F5 105.3(3) . . ? F6 C32 F4 110.1(3) . . ? F5 C32 F4 104.9(3) . . ? F6 C32 C5 113.2(2) . . ? F5 C32 C5 111.4(2) . . ? F4 C32 C5 111.5(2) . . ? F9 C33 F8 106.9(3) . . ? F9 C33 F7 110.2(4) . . ? F8 C33 F7 103.0(3) . . ? F9 C33 C9 113.5(3) . . ? F8 C33 C9 112.5(3) . . ? F7 C33 C9 110.2(3) . . ? F11 C34 F12 110.9(3) . . ? F11 C34 F10 103.3(3) . . ? F12 C34 F10 103.4(3) . . ? F11 C34 C11 112.8(3) . . ? F12 C34 C11 113.1(3) . . ? F10 C34 C11 112.4(3) . . ? F13 C35 F15 106.7(3) . . ? F13 C35 F14 107.4(3) . . ? F15 C35 F14 104.5(3) . . ? F13 C35 C21 112.8(3) . . ? F15 C35 C21 112.5(2) . . ? F14 C35 C21 112.3(3) . . ? F26 C36 F25 109.2(11) . . ? F26 C36 F27 109.6(10) . . ? F25 C36 F27 100.7(9) . . ? F26 C36 F16 127.1(8) . . ? F25 C36 F16 33.0(9) . . ? F27 C36 F16 68.7(8) . . ? F26 C36 F18 65.9(10) . . ? F25 C36 F18 131.5(6) . . ? F27 C36 F18 47.3(7) . . ? F16 C36 F18 108.8(6) . . ? F26 C36 F17 40.1(11) . . ? F25 C36 F17 74.2(10) . . ? F27 C36 F17 136.3(7) . . ? F16 C36 F17 103.0(6) . . ? F18 C36 F17 103.6(7) . . ? F26 C36 C23 114.5(6) . . ? F25 C36 C23 111.7(6) . . ? F27 C36 C23 110.3(6) . . ? F16 C36 C23 114.9(5) . . ? F18 C36 C23 113.7(4) . . ? F17 C36 C23 111.7(4) . . ? F21 C37 F19 106.2(3) . . ? F21 C37 F20 107.3(4) . . ? F19 C37 F20 106.3(3) . . ? F21 C37 C27 111.4(3) . . ? F19 C37 C27 112.9(3) . . ? F20 C37 C27 112.4(3) . . ? F24 C38 F23 107.9(3) . . ? F24 C38 F22 106.8(3) . . ? F23 C38 F22 104.9(3) . . ? F24 C38 C29 113.4(3) . . ? F23 C38 C29 112.5(3) . . ? F22 C38 C29 110.8(3) . . ? N2 C39 C40 109.4(2) . . ? C39 C40 C41 104.3(2) . . ? N1 C41 C40 110.7(2) . . ? N4 C42 C43 109.3(2) . . ? C42 C43 C44 104.3(2) . . ? N3 C44 C43 110.8(2) . . ? C46 C45 C50 117.0(3) . . ? C46 C45 B1 122.4(3) . . ? C50 C45 B1 120.6(2) . . ? C45 C46 C47 121.5(3) . . ? C48 C47 C46 120.3(3) . . ? C49 C48 C47 119.0(3) . . ? C48 C49 C50 120.6(4) . . ? C49 C50 C45 121.6(3) . . ? C52 C51 C56 116.8(2) . . ? C52 C51 B1 123.0(2) . . ? C56 C51 B1 119.7(2) . . ? C51 C52 C53 121.2(3) . . ? C54 C53 C52 120.6(3) . . ? C53 C54 C55 119.3(2) . . ? C56 C55 C54 119.7(3) . . ? C55 C56 C51 122.3(3) . . ? N2 B1 N4 109.40(19) . . ? N2 B1 C51 109.2(2) . . ? N4 B1 C51 105.53(19) . . ? N2 B1 C45 108.9(2) . . ? N4 B1 C45 108.3(2) . . ? C51 B1 C45 115.4(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.272 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.080