# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name F.Schaper _publ_contact_author_name F.Schaper _publ_contact_author_email Frank.Schaper@umontreal.ca data_todd252 _database_code_depnum_ccdc_archive 'CCDC 886541' #TrackingRef '- todd252.cif' _vrf_PLAT154_todd252 ; RESPONSE Coincidence, reported su's are correct. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H56 Cu2 N4 O2' _chemical_formula_sum 'C44 H56 Cu2 N4 O2' _chemical_formula_weight 800.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3589(4) _cell_length_b 12.1538(4) _cell_length_c 15.8856(5) _cell_angle_alpha 76.9762(16) _cell_angle_beta 80.6313(16) _cell_angle_gamma 71.9949(16) _cell_volume 2021.73(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _cell_measurement_reflns_used 8374 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 39.30 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 1.606 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details 'Twinabs (Sheldrick, 2008)' _exptl_special_details ; Twinned crystals. Four independent domains found by CELLNOW. Twinabs yielded the following twin fractions 0.4541 0.4470 0.0607 0.0381. Alternative integration with 2, 3 or 5 twin domains yielded higher Rint values. Reported Rint as reported by Twinabs "Rint is based on agreement between observed single and composite intensities and those calculated from refined unique intensities and twin fractions." for the HKLF 4 file produced. ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Helios multi-layers optics' _diffrn_measurement_device_type 'Bruker SMART 6000 / Nonius FR591' _diffrn_detector_area_resol_mean 5.5 _diffrn_reflns_number 82878 _diffrn_reflns_av_R_equivalents 0.0859 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 73.00 _reflns_number_total 7954 _reflns_number_gt 5908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker CELLNOW' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0993P)^2^+0.1931P] 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 7954 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1694 _refine_ls_wR_factor_gt 0.1590 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 0.53639(4) 0.07421(4) 0.54869(3) 0.03616(15) Uani 1 1 d . . . Cu31 Cu -0.04210(4) 0.62306(4) 0.94896(3) 0.03445(15) Uani 1 1 d . . . O1 O 0.6139(2) -0.0462(2) 0.47529(14) 0.0384(5) Uani 1 1 d . . . O31 O 0.1119(2) 0.4984(2) 0.97281(14) 0.0370(5) Uani 1 1 d . . . N1 N 0.6599(3) 0.1581(3) 0.51423(17) 0.0396(6) Uani 1 1 d . . . N2 N 0.4832(3) 0.1240(2) 0.66069(17) 0.0375(6) Uani 1 1 d . . . N31 N -0.1653(2) 0.7572(2) 0.98517(16) 0.0357(6) Uani 1 1 d . . . N32 N 0.0017(3) 0.7083(2) 0.83475(16) 0.0366(6) Uani 1 1 d . . . C1 C 0.5035(4) 0.2089(3) 0.7828(2) 0.0492(9) Uani 1 1 d . . . H23A H 0.4350 0.2793 0.7763 0.074 Uiso 1 1 calc R . . H23B H 0.5699 0.2238 0.8048 0.074 Uiso 1 1 calc R . . H23C H 0.4769 0.1472 0.8228 0.074 Uiso 1 1 calc R . . C2 C 0.5488(3) 0.1721(3) 0.6956(2) 0.0387(7) Uani 1 1 d . . . C3 C 0.6598(3) 0.1952(3) 0.6548(2) 0.0420(8) Uani 1 1 d . . . H21 H 0.7080 0.2111 0.6900 0.050 Uiso 1 1 calc R . . C4 C 0.7071(3) 0.1975(3) 0.5680(2) 0.0384(7) Uani 1 1 d . . . C5 C 0.8146(4) 0.2499(4) 0.5356(3) 0.0548(10) Uani 1 1 d . . . H50A H 0.8829 0.1932 0.5110 0.082 Uiso 1 1 calc R . . H50B H 0.8402 0.2706 0.5832 0.082 Uiso 1 1 calc R . . H50C H 0.7889 0.3190 0.4921 0.082 Uiso 1 1 calc R . . C6 C 0.6872(3) 0.1893(3) 0.4202(2) 0.0438(8) Uani 1 1 d . . . H1A H 0.6953 0.1221 0.3941 0.053 Uiso 1 1 calc R . . H1B H 0.7661 0.2080 0.4077 0.053 Uiso 1 1 calc R . . C7 C 0.5875(3) 0.2927(3) 0.3802(2) 0.0418(8) Uani 1 1 d . . . C8 C 0.5094(4) 0.3761(4) 0.4276(2) 0.0559(10) Uani 1 1 d . . . H9 H 0.5172 0.3675 0.4863 0.067 Uiso 1 1 calc R . . C9 C 0.4202(5) 0.4716(4) 0.3878(3) 0.0693(13) Uani 1 1 d . . . H8 H 0.3698 0.5271 0.4200 0.083 Uiso 1 1 calc R . . C10 C 0.4050(5) 0.4855(4) 0.3017(3) 0.0680(13) Uani 1 1 d . . . H7 H 0.3450 0.5499 0.2756 0.082 Uiso 1 1 calc R . . C11 C 0.4800(4) 0.4027(4) 0.2542(3) 0.0594(11) Uani 1 1 d . . . H6 H 0.4707 0.4109 0.1958 0.071 Uiso 1 1 calc R . . C12 C 0.5688(4) 0.3080(4) 0.2937(2) 0.0481(9) Uani 1 1 d . . . H5 H 0.6179 0.2523 0.2613 0.058 Uiso 1 1 calc R . . C13 C 0.3638(3) 0.1099(3) 0.7065(2) 0.0439(8) Uani 1 1 d . . . H60A H 0.3108 0.1115 0.6639 0.053 Uiso 1 1 calc R . . H60B H 0.3236 0.1769 0.7347 0.053 Uiso 1 1 calc R . . C14 C 0.3726(3) -0.0028(3) 0.7749(2) 0.0419(8) Uani 1 1 d . . . C15 C 0.4839(4) -0.0762(3) 0.8046(2) 0.0469(8) Uani 1 1 d . . . H24 H 0.5582 -0.0597 0.7803 0.056 Uiso 1 1 calc R . . C16 C 0.4860(4) -0.1747(4) 0.8705(2) 0.0549(10) Uani 1 1 d . . . H25 H 0.5610 -0.2226 0.8905 0.066 Uiso 1 1 calc R . . C17 C 0.3762(5) -0.2002(4) 0.9057(2) 0.0614(12) Uani 1 1 d . . . H26 H 0.3770 -0.2647 0.9503 0.074 Uiso 1 1 calc R . . C18 C 0.2658(4) -0.1310(4) 0.8751(3) 0.0573(11) Uani 1 1 d . . . H27 H 0.1923 -0.1500 0.8979 0.069 Uiso 1 1 calc R . . C19 C 0.2632(4) -0.0318(3) 0.8097(2) 0.0479(9) Uani 1 1 d . . . H28 H 0.1879 0.0150 0.7894 0.057 Uiso 1 1 calc R . . C20 C 0.7133(3) -0.1465(3) 0.5058(3) 0.0458(8) Uani 1 1 d . . . H12 H 0.7109 -0.2127 0.4811 0.055 Uiso 1 1 calc R . . C21 C 0.6965(4) -0.1808(4) 0.6043(3) 0.0643(12) Uani 1 1 d . . . H11A H 0.7070 -0.1205 0.6299 0.096 Uiso 1 1 calc R . . H11B H 0.7574 -0.2539 0.6227 0.096 Uiso 1 1 calc R . . H11C H 0.6146 -0.1898 0.6223 0.096 Uiso 1 1 calc R . . C22 C 0.8380(4) -0.1224(4) 0.4749(3) 0.0670(12) Uani 1 1 d . . . H13A H 0.8468 -0.1026 0.4126 0.100 Uiso 1 1 calc R . . H13B H 0.9036 -0.1914 0.4938 0.100 Uiso 1 1 calc R . . H13C H 0.8425 -0.0581 0.4987 0.100 Uiso 1 1 calc R . . C31 C -0.3215(3) 0.9502(3) 0.9685(2) 0.0465(8) Uani 1 1 d . . . H30A H -0.3906 0.9197 0.9932 0.070 Uiso 1 1 calc R . . H30B H -0.3471 1.0155 0.9220 0.070 Uiso 1 1 calc R . . H30C H -0.2932 0.9760 1.0123 0.070 Uiso 1 1 calc R . . C32 C -0.2166(3) 0.8545(3) 0.9334(2) 0.0364(7) Uani 1 1 d . . . C33 C -0.1773(3) 0.8772(3) 0.8442(2) 0.0381(7) Uani 1 1 d . . . H32 H -0.2285 0.9413 0.8105 0.046 Uiso 1 1 calc R . . C34 C -0.0680(3) 0.8127(3) 0.8007(2) 0.0382(7) Uani 1 1 d . . . C35 C -0.0305(4) 0.8746(3) 0.7105(2) 0.0493(9) Uani 1 1 d . . . H34A H 0.0433 0.8967 0.7115 0.074 Uiso 1 1 calc R . . H34B H -0.0966 0.9437 0.6928 0.074 Uiso 1 1 calc R . . H34C H -0.0145 0.8223 0.6701 0.074 Uiso 1 1 calc R . . C36 C 0.1199(3) 0.6549(3) 0.7866(2) 0.0416(8) Uani 1 1 d . . . H35A H 0.1764 0.6037 0.8282 0.050 Uiso 1 1 calc R . . H35B H 0.1563 0.7172 0.7560 0.050 Uiso 1 1 calc R . . C37 C 0.1113(4) 0.5839(3) 0.7210(2) 0.0423(8) Uani 1 1 d . . . C38 C 0.0005(4) 0.5858(3) 0.6954(2) 0.0504(9) Uani 1 1 d . . . H37 H -0.0742 0.6296 0.7202 0.061 Uiso 1 1 calc R . . C39 C -0.0007(5) 0.5225(4) 0.6325(3) 0.0636(12) Uani 1 1 d . . . H38 H -0.0758 0.5248 0.6151 0.076 Uiso 1 1 calc R . . C40 C 0.1107(5) 0.4559(4) 0.5960(2) 0.0652(13) Uani 1 1 d . . . H39 H 0.1104 0.4145 0.5535 0.078 Uiso 1 1 calc R . . C41 C 0.2199(5) 0.4515(4) 0.6227(3) 0.0649(13) Uani 1 1 d . . . H40 H 0.2941 0.4058 0.5988 0.078 Uiso 1 1 calc R . . C42 C 0.2227(4) 0.5143(3) 0.6851(2) 0.0496(9) Uani 1 1 d . . . H10 H 0.2982 0.5101 0.7030 0.059 Uiso 1 1 calc R . . C43 C -0.1861(3) 0.7476(3) 1.07972(19) 0.0383(7) Uani 1 1 d . . . H41A H -0.1895 0.6685 1.1065 0.046 Uiso 1 1 calc R . . H41B H -0.2655 0.8019 1.0949 0.046 Uiso 1 1 calc R . . C44 C -0.0845(3) 0.7745(3) 1.1150(2) 0.0388(7) Uani 1 1 d . . . C49 C -0.0098(4) 0.8409(4) 1.0652(2) 0.0494(9) Uani 1 1 d . . . H43 H -0.0175 0.8658 1.0061 0.059 Uiso 1 1 calc R . . C48 C 0.0757(4) 0.8711(4) 1.1012(3) 0.0609(11) Uani 1 1 d . . . H44 H 0.1220 0.9189 1.0668 0.073 Uiso 1 1 calc R . . C47 C 0.0930(4) 0.8307(4) 1.1881(3) 0.0646(12) Uani 1 1 d . . . H45 H 0.1497 0.8518 1.2128 0.078 Uiso 1 1 calc R . . C46 C 0.0246(4) 0.7589(4) 1.2373(3) 0.0573(10) Uani 1 1 d . . . H46 H 0.0375 0.7290 1.2953 0.069 Uiso 1 1 calc R . . C45 C -0.0626(4) 0.7304(3) 1.2020(2) 0.0456(8) Uani 1 1 d . . . H47 H -0.1075 0.6814 1.2364 0.055 Uiso 1 1 calc R . . C50 C 0.2166(3) 0.5262(3) 0.9928(2) 0.0426(8) Uani 1 1 d . . . H53 H 0.2113 0.6082 0.9655 0.051 Uiso 1 1 calc R . . C51 C 0.3366(3) 0.4489(4) 0.9566(3) 0.0549(10) Uani 1 1 d . . . H56A H 0.3422 0.3679 0.9810 0.082 Uiso 1 1 calc R . . H56B H 0.4055 0.4685 0.9712 0.082 Uiso 1 1 calc R . . H56C H 0.3386 0.4611 0.8946 0.082 Uiso 1 1 calc R . . C52 C 0.2139(4) 0.5149(4) 1.0908(3) 0.0639(12) Uani 1 1 d . . . H52A H 0.1330 0.5569 1.1136 0.096 Uiso 1 1 calc R . . H52B H 0.2753 0.5474 1.1025 0.096 Uiso 1 1 calc R . . H52C H 0.2318 0.4333 1.1179 0.096 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 0.0324(3) 0.0419(3) 0.0351(3) -0.0114(2) 0.0009(2) -0.0110(2) Cu31 0.0354(3) 0.0347(3) 0.0302(2) -0.00612(19) 0.00038(19) -0.0075(2) O1 0.0314(11) 0.0425(12) 0.0426(12) -0.0160(10) -0.0034(10) -0.0069(10) O31 0.0356(12) 0.0365(12) 0.0364(11) -0.0033(9) 0.0010(10) -0.0116(10) N1 0.0382(15) 0.0459(16) 0.0348(14) -0.0111(12) 0.0045(12) -0.0137(12) N2 0.0362(14) 0.0430(15) 0.0303(13) -0.0065(12) 0.0022(11) -0.0102(12) N31 0.0365(14) 0.0392(14) 0.0306(13) -0.0101(11) 0.0036(11) -0.0106(12) N32 0.0371(14) 0.0395(15) 0.0302(13) -0.0086(11) 0.0005(11) -0.0072(12) C1 0.058(2) 0.053(2) 0.0382(18) -0.0148(16) 0.0022(17) -0.0173(18) C2 0.0450(19) 0.0378(17) 0.0333(16) -0.0089(14) -0.0056(15) -0.0093(14) C3 0.0459(19) 0.0440(19) 0.0389(17) -0.0094(15) -0.0063(15) -0.0146(15) C4 0.0347(16) 0.0371(17) 0.0422(17) -0.0063(14) -0.0018(14) -0.0101(13) C5 0.045(2) 0.073(3) 0.054(2) -0.017(2) 0.0010(18) -0.027(2) C6 0.0443(19) 0.052(2) 0.0369(17) -0.0140(16) 0.0071(15) -0.0179(16) C7 0.049(2) 0.048(2) 0.0342(16) -0.0124(15) 0.0061(15) -0.0232(16) C8 0.074(3) 0.053(2) 0.0382(19) -0.0182(17) -0.0073(19) -0.006(2) C9 0.081(3) 0.058(3) 0.057(2) -0.019(2) -0.001(2) 0.000(2) C10 0.086(3) 0.049(2) 0.060(3) -0.006(2) -0.022(3) -0.003(2) C11 0.076(3) 0.057(2) 0.044(2) -0.0062(18) -0.008(2) -0.018(2) C12 0.055(2) 0.053(2) 0.0373(18) -0.0140(16) 0.0034(17) -0.0178(18) C13 0.0395(18) 0.054(2) 0.0354(17) -0.0101(15) 0.0032(15) -0.0113(16) C14 0.048(2) 0.0454(19) 0.0343(16) -0.0140(15) 0.0038(15) -0.0164(16) C15 0.046(2) 0.054(2) 0.0440(19) -0.0132(17) -0.0012(16) -0.0182(17) C16 0.068(3) 0.055(2) 0.043(2) -0.0097(18) -0.0096(19) -0.017(2) C17 0.097(4) 0.054(2) 0.0380(19) -0.0070(17) 0.003(2) -0.034(2) C18 0.073(3) 0.059(2) 0.048(2) -0.0204(19) 0.020(2) -0.035(2) C19 0.049(2) 0.053(2) 0.0430(19) -0.0185(17) 0.0063(16) -0.0151(17) C20 0.0330(17) 0.047(2) 0.057(2) -0.0161(17) -0.0085(16) -0.0045(15) C21 0.060(3) 0.067(3) 0.058(3) 0.000(2) -0.018(2) -0.009(2) C22 0.037(2) 0.080(3) 0.084(3) -0.023(3) -0.004(2) -0.011(2) C31 0.045(2) 0.0418(19) 0.048(2) -0.0128(16) -0.0014(17) -0.0041(16) C32 0.0360(16) 0.0376(17) 0.0369(16) -0.0099(14) -0.0028(14) -0.0108(14) C33 0.0383(17) 0.0383(17) 0.0369(16) -0.0062(14) -0.0082(14) -0.0079(14) C34 0.0431(18) 0.0401(18) 0.0325(16) -0.0062(14) -0.0062(14) -0.0124(15) C35 0.059(2) 0.048(2) 0.0334(17) -0.0024(15) 0.0017(17) -0.0115(18) C36 0.0405(18) 0.049(2) 0.0311(16) -0.0083(15) 0.0008(14) -0.0089(15) C37 0.057(2) 0.0368(18) 0.0257(14) -0.0031(13) 0.0041(15) -0.0083(15) C38 0.063(2) 0.047(2) 0.0341(17) -0.0060(15) -0.0069(17) -0.0051(18) C39 0.090(3) 0.054(2) 0.045(2) -0.0068(19) -0.021(2) -0.013(2) C40 0.110(4) 0.050(2) 0.0335(18) -0.0100(17) -0.002(2) -0.020(3) C41 0.092(4) 0.047(2) 0.045(2) -0.0139(18) 0.027(2) -0.018(2) C42 0.060(2) 0.044(2) 0.0408(18) -0.0091(16) 0.0122(17) -0.0172(18) C43 0.0433(18) 0.0403(18) 0.0299(15) -0.0090(13) 0.0037(14) -0.0120(14) C44 0.0432(18) 0.0388(17) 0.0319(15) -0.0088(13) -0.0024(14) -0.0074(14) C49 0.056(2) 0.063(2) 0.0336(17) 0.0049(17) -0.0083(17) -0.031(2) C48 0.070(3) 0.066(3) 0.055(2) 0.003(2) -0.012(2) -0.039(2) C47 0.072(3) 0.067(3) 0.067(3) -0.005(2) -0.030(2) -0.029(2) C46 0.071(3) 0.065(3) 0.041(2) -0.0044(19) -0.018(2) -0.024(2) C45 0.056(2) 0.048(2) 0.0334(17) -0.0064(15) 0.0004(16) -0.0191(17) C50 0.0434(19) 0.0433(19) 0.0427(18) -0.0077(15) -0.0064(16) -0.0138(15) C51 0.042(2) 0.065(3) 0.056(2) -0.008(2) -0.0025(18) -0.0157(19) C52 0.065(3) 0.076(3) 0.055(2) -0.021(2) -0.018(2) -0.015(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 N1 1.921(3) . ? Cu1 N2 1.951(3) . ? Cu1 O1 1.951(2) 2_656 ? Cu1 O1 1.979(2) . ? Cu1 Cu1 2.9877(9) 2_656 ? Cu31 N31 1.923(3) . ? Cu31 N32 1.946(3) . ? Cu31 O31 1.954(2) . ? Cu31 O31 1.982(2) 2_567 ? Cu31 Cu31 3.0071(9) 2_567 ? O1 C20 1.434(4) . ? O1 Cu1 1.951(2) 2_656 ? O31 C50 1.432(4) . ? O31 Cu31 1.982(2) 2_567 ? N1 C4 1.319(4) . ? N1 C6 1.463(4) . ? N2 C2 1.325(4) . ? N2 C13 1.471(4) . ? N31 C32 1.305(4) . ? N31 C43 1.466(4) . ? N32 C34 1.319(4) . ? N32 C36 1.470(4) . ? C1 C2 1.513(4) . ? C1 H23A 0.9600 . ? C1 H23B 0.9600 . ? C1 H23C 0.9600 . ? C2 C3 1.400(5) . ? C3 C4 1.392(5) . ? C3 H21 0.9300 . ? C4 C5 1.513(5) . ? C5 H50A 0.9600 . ? C5 H50B 0.9600 . ? C5 H50C 0.9600 . ? C6 C7 1.503(5) . ? C6 H1A 0.9700 . ? C6 H1B 0.9700 . ? C7 C12 1.386(5) . ? C7 C8 1.397(5) . ? C8 C9 1.388(6) . ? C8 H9 0.9300 . ? C9 C10 1.373(6) . ? C9 H8 0.9300 . ? C10 C11 1.382(6) . ? C10 H7 0.9300 . ? C11 C12 1.378(6) . ? C11 H6 0.9300 . ? C12 H5 0.9300 . ? C13 C14 1.531(5) . ? C13 H60A 0.9700 . ? C13 H60B 0.9700 . ? C14 C15 1.387(5) . ? C14 C19 1.390(5) . ? C15 C16 1.399(5) . ? C15 H24 0.9300 . ? C16 C17 1.378(6) . ? C16 H25 0.9300 . ? C17 C18 1.371(6) . ? C17 H26 0.9300 . ? C18 C19 1.398(5) . ? C18 H27 0.9300 . ? C19 H28 0.9300 . ? C20 C22 1.516(5) . ? C20 C21 1.522(5) . ? C20 H12 0.9800 . ? C21 H11A 0.9600 . ? C21 H11B 0.9600 . ? C21 H11C 0.9600 . ? C22 H13A 0.9600 . ? C22 H13B 0.9600 . ? C22 H13C 0.9600 . ? C31 C32 1.517(5) . ? C31 H30A 0.9600 . ? C31 H30B 0.9600 . ? C31 H30C 0.9600 . ? C32 C33 1.406(4) . ? C33 C34 1.414(5) . ? C33 H32 0.9300 . ? C34 C35 1.521(4) . ? C35 H34A 0.9600 . ? C35 H34B 0.9600 . ? C35 H34C 0.9600 . ? C36 C37 1.527(5) . ? C36 H35A 0.9700 . ? C36 H35B 0.9700 . ? C37 C38 1.376(5) . ? C37 C42 1.401(5) . ? C38 C39 1.396(5) . ? C38 H37 0.9300 . ? C39 C40 1.389(7) . ? C39 H38 0.9300 . ? C40 C41 1.357(7) . ? C40 H39 0.9300 . ? C41 C42 1.390(6) . ? C41 H40 0.9300 . ? C42 H10 0.9300 . ? C43 C44 1.509(5) . ? C43 H41A 0.9700 . ? C43 H41B 0.9700 . ? C44 C49 1.383(5) . ? C44 C45 1.398(4) . ? C49 C48 1.378(5) . ? C49 H43 0.9300 . ? C48 C47 1.381(6) . ? C48 H44 0.9300 . ? C47 C46 1.375(6) . ? C47 H45 0.9300 . ? C46 C45 1.377(5) . ? C46 H46 0.9300 . ? C45 H47 0.9300 . ? C50 C51 1.506(5) . ? C50 C52 1.528(5) . ? C50 H53 0.9800 . ? C51 H56A 0.9600 . ? C51 H56B 0.9600 . ? C51 H56C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? 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 95.19(12) . . ? N1 Cu1 O1 148.64(11) . 2_656 ? N2 Cu1 O1 101.42(10) . 2_656 ? N1 Cu1 O1 96.14(11) . . ? N2 Cu1 O1 152.70(11) . . ? O1 Cu1 O1 81.01(10) 2_656 . ? N1 Cu1 Cu1 128.94(8) . 2_656 ? N2 Cu1 Cu1 135.87(9) . 2_656 ? O1 Cu1 Cu1 40.85(6) 2_656 2_656 ? O1 Cu1 Cu1 40.16(6) . 2_656 ? N31 Cu31 N32 94.92(11) . . ? N31 Cu31 O31 146.79(11) . . ? N32 Cu31 O31 102.73(10) . . ? N31 Cu31 O31 96.57(10) . 2_567 ? N32 Cu31 O31 152.75(11) . 2_567 ? O31 Cu31 O31 80.34(10) . 2_567 ? N31 Cu31 Cu31 128.24(8) . 2_567 ? N32 Cu31 Cu31 136.81(8) . 2_567 ? O31 Cu31 Cu31 40.52(6) . 2_567 ? O31 Cu31 Cu31 39.83(6) 2_567 2_567 ? C20 O1 Cu1 117.9(2) . 2_656 ? C20 O1 Cu1 119.3(2) . . ? Cu1 O1 Cu1 98.99(10) 2_656 . ? C50 O31 Cu31 120.0(2) . . ? C50 O31 Cu31 121.53(19) . 2_567 ? Cu31 O31 Cu31 99.66(10) . 2_567 ? C4 N1 C6 121.1(3) . . ? C4 N1 Cu1 124.5(2) . . ? C6 N1 Cu1 114.0(2) . . ? C2 N2 C13 119.2(3) . . ? C2 N2 Cu1 122.6(2) . . ? C13 N2 Cu1 118.2(2) . . ? C32 N31 C43 121.1(3) . . ? C32 N31 Cu31 125.3(2) . . ? C43 N31 Cu31 113.1(2) . . ? C34 N32 C36 119.2(3) . . ? C34 N32 Cu31 122.8(2) . . ? C36 N32 Cu31 118.0(2) . . ? C2 C1 H23A 109.5 . . ? C2 C1 H23B 109.5 . . ? H23A C1 H23B 109.5 . . ? C2 C1 H23C 109.5 . . ? H23A C1 H23C 109.5 . . ? H23B C1 H23C 109.5 . . ? N2 C2 C3 123.4(3) . . ? N2 C2 C1 120.5(3) . . ? C3 C2 C1 116.1(3) . . ? C4 C3 C2 128.2(3) . . ? C4 C3 H21 115.9 . . ? C2 C3 H21 115.9 . . ? N1 C4 C3 122.3(3) . . ? N1 C4 C5 120.0(3) . . ? C3 C4 C5 117.7(3) . . ? C4 C5 H50A 109.5 . . ? C4 C5 H50B 109.5 . . ? H50A C5 H50B 109.5 . . ? C4 C5 H50C 109.5 . . ? H50A C5 H50C 109.5 . . ? H50B C5 H50C 109.5 . . ? N1 C6 C7 112.1(3) . . ? N1 C6 H1A 109.2 . . ? C7 C6 H1A 109.2 . . ? N1 C6 H1B 109.2 . . ? C7 C6 H1B 109.2 . . ? H1A C6 H1B 107.9 . . ? C12 C7 C8 117.2(4) . . ? C12 C7 C6 120.5(3) . . ? C8 C7 C6 122.3(3) . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H9 119.8 . . ? C7 C8 H9 119.8 . . ? C10 C9 C8 121.0(4) . . ? C10 C9 H8 119.5 . . ? C8 C9 H8 119.5 . . ? C9 C10 C11 119.2(4) . . ? C9 C10 H7 120.4 . . ? C11 C10 H7 120.4 . . ? C12 C11 C10 119.7(4) . . ? C12 C11 H6 120.2 . . ? C10 C11 H6 120.2 . . ? C11 C12 C7 122.3(4) . . ? C11 C12 H5 118.8 . . ? C7 C12 H5 118.8 . . ? N2 C13 C14 115.4(3) . . ? N2 C13 H60A 108.4 . . ? C14 C13 H60A 108.4 . . ? N2 C13 H60B 108.4 . . ? C14 C13 H60B 108.4 . . ? H60A C13 H60B 107.5 . . ? C15 C14 C19 118.5(4) . . ? C15 C14 C13 123.2(3) . . ? C19 C14 C13 118.2(3) . . ? C14 C15 C16 120.9(4) . . ? C14 C15 H24 119.5 . . ? C16 C15 H24 119.5 . . ? C17 C16 C15 119.6(4) . . ? C17 C16 H25 120.2 . . ? C15 C16 H25 120.2 . . ? C18 C17 C16 120.2(4) . . ? C18 C17 H26 119.9 . . ? C16 C17 H26 119.9 . . ? C17 C18 C19 120.3(4) . . ? C17 C18 H27 119.9 . . ? C19 C18 H27 119.9 . . ? C14 C19 C18 120.3(4) . . ? C14 C19 H28 119.8 . . ? C18 C19 H28 119.8 . . ? O1 C20 C22 110.5(3) . . ? O1 C20 C21 110.8(3) . . ? C22 C20 C21 111.2(3) . . ? O1 C20 H12 108.1 . . ? C22 C20 H12 108.1 . . ? C21 C20 H12 108.1 . . ? C20 C21 H11A 109.5 . . ? C20 C21 H11B 109.5 . . ? H11A C21 H11B 109.5 . . ? C20 C21 H11C 109.5 . . ? H11A C21 H11C 109.5 . . ? H11B C21 H11C 109.5 . . ? C20 C22 H13A 109.5 . . ? C20 C22 H13B 109.5 . . ? H13A C22 H13B 109.5 . . ? C20 C22 H13C 109.5 . . ? H13A C22 H13C 109.5 . . ? H13B C22 H13C 109.5 . . ? C32 C31 H30A 109.5 . . ? C32 C31 H30B 109.5 . . ? H30A C31 H30B 109.5 . . ? C32 C31 H30C 109.5 . . ? H30A C31 H30C 109.5 . . ? H30B C31 H30C 109.5 . . ? N31 C32 C33 122.7(3) . . ? N31 C32 C31 120.6(3) . . ? C33 C32 C31 116.8(3) . . ? C32 C33 C34 126.6(3) . . ? C32 C33 H32 116.7 . . ? C34 C33 H32 116.7 . . ? N32 C34 C33 124.1(3) . . ? N32 C34 C35 120.6(3) . . ? C33 C34 C35 115.2(3) . . ? C34 C35 H34A 109.5 . . ? C34 C35 H34B 109.5 . . ? H34A C35 H34B 109.5 . . ? C34 C35 H34C 109.5 . . ? H34A C35 H34C 109.5 . . ? H34B C35 H34C 109.5 . . ? N32 C36 C37 115.6(3) . . ? N32 C36 H35A 108.4 . . ? C37 C36 H35A 108.4 . . ? N32 C36 H35B 108.4 . . ? C37 C36 H35B 108.4 . . ? H35A C36 H35B 107.4 . . ? C38 C37 C42 119.0(3) . . ? C38 C37 C36 123.4(3) . . ? C42 C37 C36 117.6(3) . . ? C37 C38 C39 120.5(4) . . ? C37 C38 H37 119.7 . . ? C39 C38 H37 119.7 . . ? C40 C39 C38 119.9(5) . . ? C40 C39 H38 120.1 . . ? C38 C39 H38 120.1 . . ? C41 C40 C39 119.8(4) . . ? C41 C40 H39 120.1 . . ? C39 C40 H39 120.1 . . ? C40 C41 C42 121.1(4) . . ? C40 C41 H40 119.5 . . ? C42 C41 H40 119.5 . . ? C41 C42 C37 119.8(4) . . ? C41 C42 H10 120.1 . . ? C37 C42 H10 120.1 . . ? N31 C43 C44 111.8(3) . . ? N31 C43 H41A 109.2 . . ? C44 C43 H41A 109.2 . . ? N31 C43 H41B 109.2 . . ? C44 C43 H41B 109.2 . . ? H41A C43 H41B 107.9 . . ? C49 C44 C45 117.3(3) . . ? C49 C44 C43 123.3(3) . . ? C45 C44 C43 119.5(3) . . ? C48 C49 C44 121.6(3) . . ? C48 C49 H43 119.2 . . ? C44 C49 H43 119.2 . . ? C49 C48 C47 120.3(4) . . ? C49 C48 H44 119.8 . . ? C47 C48 H44 119.8 . . ? C46 C47 C48 118.7(4) . . ? C46 C47 H45 120.7 . . ? C48 C47 H45 120.7 . . ? C47 C46 C45 121.1(4) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C45 C44 120.8(4) . . ? C46 C45 H47 119.6 . . ? C44 C45 H47 119.6 . . ? O31 C50 C51 110.8(3) . . ? O31 C50 C52 110.5(3) . . ? C51 C50 C52 110.9(3) . . ? O31 C50 H53 108.2 . . ? C51 C50 H53 108.2 . . ? C52 C50 H53 108.2 . . ? C50 C51 H56A 109.5 . . ? C50 C51 H56B 109.5 . . ? H56A C51 H56B 109.5 . . ? C50 C51 H56C 109.5 . . ? H56A C51 H56C 109.5 . . ? H56B C51 H56C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? _iucr_refine_instructions_details ; TITL todd252 in P-1 CELL 1.54178 11.3589 12.1538 15.8856 76.9762 80.6313 71.9949 ZERR 2.00 0.0004 0.0004 0.0005 0.0016 0.0016 0.0016 LATT 1 SFAC C H N O Cu UNIT 88 112 8 4 4 L.S. 20 ACTA BOND FMAP 2 PLAN -5 SIZE 0.11 0.18 0.22 TEMP 23 WGHT 0.099300 0.193100 FVAR 0.50902 CU1 5 0.536390 0.074208 0.548691 11.00000 0.03241 0.04192 = 0.03505 -0.01140 0.00090 -0.01099 CU31 5 -0.042102 0.623065 0.948961 11.00000 0.03541 0.03474 = 0.03025 -0.00612 0.00038 -0.00754 O1 4 0.613923 -0.046199 0.475294 11.00000 0.03141 0.04255 = 0.04264 -0.01598 -0.00336 -0.00695 O31 4 0.111859 0.498395 0.972810 11.00000 0.03559 0.03655 = 0.03643 -0.00328 0.00098 -0.01160 N1 3 0.659907 0.158061 0.514232 11.00000 0.03818 0.04590 = 0.03483 -0.01115 0.00451 -0.01374 N2 3 0.483198 0.123980 0.660691 11.00000 0.03619 0.04297 = 0.03033 -0.00645 0.00219 -0.01016 N31 3 -0.165327 0.757235 0.985169 11.00000 0.03648 0.03924 = 0.03056 -0.01010 0.00362 -0.01058 N32 3 0.001667 0.708253 0.834754 11.00000 0.03708 0.03952 = 0.03020 -0.00856 0.00046 -0.00719 C1 1 0.503508 0.208946 0.782830 11.00000 0.05820 0.05280 = 0.03821 -0.01475 0.00224 -0.01730 AFIX 137 H23A 2 0.435019 0.279255 0.776251 11.00000 -1.50000 H23B 2 0.569922 0.223815 0.804775 11.00000 -1.50000 H23C 2 0.476855 0.147161 0.822788 11.00000 -1.50000 AFIX 0 C2 1 0.548776 0.172082 0.695650 11.00000 0.04496 0.03780 = 0.03326 -0.00893 -0.00558 -0.00925 C3 1 0.659763 0.195234 0.654785 11.00000 0.04589 0.04401 = 0.03894 -0.00942 -0.00625 -0.01462 AFIX 43 H21 2 0.707998 0.211108 0.690035 11.00000 -1.20000 AFIX 0 C4 1 0.707062 0.197500 0.568050 11.00000 0.03467 0.03713 = 0.04217 -0.00630 -0.00182 -0.01006 C5 1 0.814610 0.249852 0.535636 11.00000 0.04477 0.07332 = 0.05375 -0.01689 0.00096 -0.02682 AFIX 137 H50A 2 0.882916 0.193163 0.511033 11.00000 -1.50000 H50B 2 0.840233 0.270592 0.583187 11.00000 -1.50000 H50C 2 0.788902 0.319007 0.492126 11.00000 -1.50000 AFIX 0 C6 1 0.687213 0.189304 0.420159 11.00000 0.04434 0.05208 = 0.03691 -0.01400 0.00715 -0.01792 AFIX 23 H1A 2 0.695265 0.122110 0.394080 11.00000 -1.20000 H1B 2 0.766072 0.207989 0.407662 11.00000 -1.20000 AFIX 0 C7 1 0.587510 0.292722 0.380187 11.00000 0.04887 0.04784 = 0.03419 -0.01243 0.00611 -0.02321 C8 1 0.509382 0.376083 0.427641 11.00000 0.07378 0.05262 = 0.03824 -0.01821 -0.00729 -0.00595 AFIX 43 H9 2 0.517235 0.367469 0.486312 11.00000 -1.20000 AFIX 0 C9 1 0.420172 0.471614 0.387828 11.00000 0.08110 0.05846 = 0.05675 -0.01934 -0.00132 -0.00001 AFIX 43 H8 2 0.369832 0.527107 0.420003 11.00000 -1.20000 AFIX 0 C10 1 0.405034 0.485522 0.301672 11.00000 0.08604 0.04904 = 0.06034 -0.00551 -0.02163 -0.00280 AFIX 43 H7 2 0.345018 0.549905 0.275579 11.00000 -1.20000 AFIX 0 C11 1 0.480044 0.402709 0.254177 11.00000 0.07600 0.05699 = 0.04392 -0.00619 -0.00843 -0.01793 AFIX 43 H6 2 0.470671 0.410887 0.195812 11.00000 -1.20000 AFIX 0 C12 1 0.568796 0.307955 0.293749 11.00000 0.05530 0.05343 = 0.03731 -0.01401 0.00339 -0.01783 AFIX 43 H5 2 0.617860 0.252272 0.261297 11.00000 -1.20000 AFIX 0 C13 1 0.363828 0.109868 0.706546 11.00000 0.03950 0.05398 = 0.03536 -0.01010 0.00322 -0.01131 AFIX 23 H60A 2 0.310814 0.111452 0.663933 11.00000 -1.20000 H60B 2 0.323630 0.176945 0.734703 11.00000 -1.20000 AFIX 0 C14 1 0.372593 -0.002791 0.774898 11.00000 0.04845 0.04541 = 0.03430 -0.01395 0.00377 -0.01638 C15 1 0.483906 -0.076174 0.804558 11.00000 0.04643 0.05376 = 0.04401 -0.01317 -0.00124 -0.01821 AFIX 43 H24 2 0.558191 -0.059676 0.780253 11.00000 -1.20000 AFIX 0 C16 1 0.485982 -0.174659 0.870526 11.00000 0.06784 0.05467 = 0.04349 -0.00968 -0.00956 -0.01664 AFIX 43 H25 2 0.561028 -0.222590 0.890545 11.00000 -1.20000 AFIX 0 C17 1 0.376198 -0.200231 0.905667 11.00000 0.09676 0.05377 = 0.03804 -0.00696 0.00314 -0.03374 AFIX 43 H26 2 0.376992 -0.264741 0.950314 11.00000 -1.20000 AFIX 0 C18 1 0.265815 -0.130953 0.875073 11.00000 0.07257 0.05879 = 0.04837 -0.02036 0.01957 -0.03526 AFIX 43 H27 2 0.192313 -0.149971 0.897895 11.00000 -1.20000 AFIX 0 C19 1 0.263218 -0.031813 0.809705 11.00000 0.04856 0.05331 = 0.04303 -0.01846 0.00625 -0.01512 AFIX 43 H28 2 0.187942 0.014955 0.789405 11.00000 -1.20000 AFIX 0 C20 1 0.713280 -0.146504 0.505791 11.00000 0.03302 0.04680 = 0.05735 -0.01606 -0.00853 -0.00445 AFIX 13 H12 2 0.710925 -0.212705 0.481127 11.00000 -1.20000 AFIX 0 C21 1 0.696501 -0.180835 0.604261 11.00000 0.05993 0.06741 = 0.05785 0.00020 -0.01797 -0.00930 AFIX 137 H11A 2 0.706968 -0.120488 0.629863 11.00000 -1.50000 H11B 2 0.757367 -0.253897 0.622719 11.00000 -1.50000 H11C 2 0.614580 -0.189781 0.622327 11.00000 -1.50000 AFIX 0 C22 1 0.837969 -0.122425 0.474908 11.00000 0.03655 0.07981 = 0.08360 -0.02267 -0.00425 -0.01065 AFIX 137 H13A 2 0.846818 -0.102559 0.412649 11.00000 -1.50000 H13B 2 0.903561 -0.191409 0.493838 11.00000 -1.50000 H13C 2 0.842498 -0.058058 0.498680 11.00000 -1.50000 AFIX 0 C31 1 -0.321536 0.950226 0.968456 11.00000 0.04515 0.04185 = 0.04779 -0.01281 -0.00143 -0.00408 AFIX 137 H30A 2 -0.390638 0.919725 0.993168 11.00000 -1.50000 H30B 2 -0.347134 1.015515 0.922026 11.00000 -1.50000 H30C 2 -0.293201 0.976025 1.012331 11.00000 -1.50000 AFIX 0 C32 1 -0.216646 0.854468 0.933437 11.00000 0.03602 0.03761 = 0.03694 -0.00991 -0.00282 -0.01079 C33 1 -0.177323 0.877249 0.844237 11.00000 0.03826 0.03829 = 0.03688 -0.00624 -0.00819 -0.00793 AFIX 43 H32 2 -0.228456 0.941292 0.810457 11.00000 -1.20000 AFIX 0 C34 1 -0.067955 0.812710 0.800651 11.00000 0.04313 0.04006 = 0.03251 -0.00616 -0.00625 -0.01241 C35 1 -0.030479 0.874571 0.710475 11.00000 0.05933 0.04784 = 0.03343 -0.00240 0.00171 -0.01150 AFIX 137 H34A 2 0.043332 0.896695 0.711548 11.00000 -1.50000 H34B 2 -0.096615 0.943745 0.692836 11.00000 -1.50000 H34C 2 -0.014494 0.822327 0.670112 11.00000 -1.50000 AFIX 0 C36 1 0.119941 0.654908 0.786612 11.00000 0.04050 0.04923 = 0.03112 -0.00829 0.00084 -0.00890 AFIX 23 H35A 2 0.176443 0.603667 0.828158 11.00000 -1.20000 H35B 2 0.156256 0.717181 0.756048 11.00000 -1.20000 AFIX 0 C37 1 0.111290 0.583858 0.721038 11.00000 0.05674 0.03675 = 0.02573 -0.00307 0.00414 -0.00832 C38 1 0.000515 0.585770 0.695432 11.00000 0.06269 0.04719 = 0.03407 -0.00597 -0.00695 -0.00508 AFIX 43 H37 2 -0.074160 0.629589 0.720239 11.00000 -1.20000 AFIX 0 C39 1 -0.000654 0.522468 0.632526 11.00000 0.08995 0.05415 = 0.04530 -0.00684 -0.02067 -0.01319 AFIX 43 H38 2 -0.075817 0.524830 0.615076 11.00000 -1.20000 AFIX 0 C40 1 0.110690 0.455919 0.596026 11.00000 0.11001 0.04955 = 0.03347 -0.00997 -0.00196 -0.01993 AFIX 43 H39 2 0.110364 0.414535 0.553484 11.00000 -1.20000 AFIX 0 C41 1 0.219930 0.451525 0.622682 11.00000 0.09238 0.04685 = 0.04518 -0.01392 0.02650 -0.01830 AFIX 43 H40 2 0.294143 0.405780 0.598797 11.00000 -1.20000 AFIX 0 C42 1 0.222691 0.514301 0.685114 11.00000 0.05956 0.04447 = 0.04081 -0.00912 0.01223 -0.01722 AFIX 43 H10 2 0.298220 0.510135 0.702966 11.00000 -1.20000 AFIX 0 C43 1 -0.186053 0.747614 1.079723 11.00000 0.04331 0.04033 = 0.02995 -0.00903 0.00374 -0.01201 AFIX 23 H41A 2 -0.189530 0.668481 1.106467 11.00000 -1.20000 H41B 2 -0.265516 0.801924 1.094876 11.00000 -1.20000 AFIX 0 C44 1 -0.084530 0.774481 1.114993 11.00000 0.04319 0.03883 = 0.03193 -0.00885 -0.00243 -0.00736 C49 1 -0.009838 0.840878 1.065247 11.00000 0.05630 0.06284 = 0.03359 0.00493 -0.00830 -0.03134 AFIX 43 H43 2 -0.017510 0.865769 1.006074 11.00000 -1.20000 AFIX 0 C48 1 0.075677 0.871071 1.101191 11.00000 0.07037 0.06622 = 0.05472 0.00342 -0.01175 -0.03937 AFIX 43 H44 2 0.121977 0.918850 1.066765 11.00000 -1.20000 AFIX 0 C47 1 0.092967 0.830735 1.188073 11.00000 0.07156 0.06667 = 0.06714 -0.00534 -0.02972 -0.02950 AFIX 43 H45 2 0.149710 0.851768 1.212816 11.00000 -1.20000 AFIX 0 C46 1 0.024613 0.758864 1.237255 11.00000 0.07095 0.06547 = 0.04079 -0.00441 -0.01847 -0.02435 AFIX 43 H46 2 0.037530 0.728951 1.295336 11.00000 -1.20000 AFIX 0 C45 1 -0.062616 0.730436 1.201978 11.00000 0.05581 0.04837 = 0.03341 -0.00642 0.00045 -0.01906 AFIX 43 H47 2 -0.107489 0.681360 1.236413 11.00000 -1.20000 AFIX 0 C50 1 0.216624 0.526213 0.992796 11.00000 0.04340 0.04329 = 0.04269 -0.00774 -0.00643 -0.01383 AFIX 13 H53 2 0.211257 0.608176 0.965507 11.00000 -1.20000 AFIX 0 C51 1 0.336611 0.448917 0.956635 11.00000 0.04199 0.06458 = 0.05590 -0.00784 -0.00246 -0.01568 AFIX 137 H56A 2 0.342246 0.367873 0.981040 11.00000 -1.50000 H56B 2 0.405522 0.468511 0.971171 11.00000 -1.50000 H56C 2 0.338571 0.461081 0.894637 11.00000 -1.50000 AFIX 0 C52 1 0.213937 0.514915 1.090832 11.00000 0.06522 0.07610 = 0.05525 -0.02129 -0.01760 -0.01475 AFIX 137 H52A 2 0.133006 0.556921 1.113621 11.00000 -1.50000 H52B 2 0.275294 0.547411 1.102524 11.00000 -1.50000 H52C 2 0.231822 0.433317 1.117929 11.00000 -1.50000 HKLF 4 REM todd252 in P-1 REM R1 = 0.0595 for 5908 Fo > 4sig(Fo) and 0.0826 for all 7954 data REM 477 parameters refined using 0 restraints END WGHT 0.0993 0.1931 REM Highest difference peak 0.722, deepest hole -0.448, 1-sigma level 0.079 Q1 1 0.0425 0.9587 1.0507 11.00000 0.05 0.72 Q2 1 0.4554 0.3414 0.4519 11.00000 0.05 0.60 Q3 1 -0.0275 0.6749 0.8833 11.00000 0.05 0.51 Q4 1 0.0465 0.7837 1.0458 11.00000 0.05 0.49 Q5 1 0.4709 0.5011 0.4425 11.00000 0.05 0.46 ; _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 73.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.722 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.079