#Copyright The Royal Society of Chemistry, 1998 data_/tintin3/people/sam/cap/cap _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C58 H53 B4 Cu2 F8 N18 O2' _chemical_formula_weight 1356.50 _chemical_melting_point ? _chemical_compound_source ? 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.535(2) _cell_length_b 14.600(3) _cell_length_c 19.608(5) _cell_angle_alpha 71.96(2) _cell_angle_beta 85.08(2) _cell_angle_gamma 63.362(12) _cell_volume 3287.0(12) _cell_formula_units_Z 2 _cell_measurement_temperature 292(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour green _exptl_crystal_size_max 0.9 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.8 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method ? _exptl_crystal_F_000 1386 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type 'Empirical, SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 292(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33212 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14683 _reflns_number_observed 8002 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14677 _refine_ls_number_parameters 870 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_obs 0.0504 _refine_ls_wR_factor_all 0.1674 _refine_ls_wR_factor_obs 0.1322 _refine_ls_goodness_of_fit_all 0.919 _refine_ls_goodness_of_fit_obs 1.093 _refine_ls_restrained_S_all 1.003 _refine_ls_restrained_S_obs 1.093 _refine_ls_shift/esd_max -1.430 _refine_ls_shift/esd_mean 0.025 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.22458(3) -0.11467(3) 0.30670(2) 0.05185(13) Uani 1 d . . Cu2 Cu -0.16055(3) -0.09488(3) 0.23294(2) 0.05161(13) Uani 1 d . . B1 B -0.0512(4) -0.1106(3) 0.4229(2) 0.0667(11) Uani 1 d . . H1A H -0.0244(4) -0.0948(3) 0.4600(2) 0.080 Uiso 1 calc R . H1B H -0.1116(4) -0.1279(3) 0.4414(2) 0.080 Uiso 1 calc R . N11 N 0.3599(2) -0.0917(2) 0.23693(15) 0.0645(8) Uani 1 d . . C12 C 0.4256(3) -0.1814(3) 0.2200(2) 0.0644(9) Uani 1 d . . C13 C 0.4998(3) -0.1801(4) 0.1662(3) 0.0966(14) Uani 1 d . . H13A H 0.5447(3) -0.2426(4) 0.1543(3) 0.116 Uiso 1 calc R . C14 C 0.5059(4) -0.0863(5) 0.1310(3) 0.106(2) Uani 1 d . . H14A H 0.5546(4) -0.0844(5) 0.0947(3) 0.127 Uiso 1 calc R . C15 C 0.4403(4) 0.0045(4) 0.1491(3) 0.0968(15) Uani 1 d . . H15A H 0.4439(4) 0.0688(4) 0.1260(3) 0.116 Uiso 1 calc R . C16 C 0.3683(4) -0.0014(4) 0.2027(2) 0.0842(12) Uani 1 d . . H16A H 0.3237(4) 0.0603(4) 0.2154(2) 0.101 Uiso 1 calc R . N21 N 0.3199(2) -0.2599(2) 0.29846(13) 0.0532(6) Uani 1 d . . C22 C 0.4113(3) -0.2783(3) 0.2606(2) 0.0635(9) Uani 1 d . . C23 C 0.4858(3) -0.3809(3) 0.2621(2) 0.0807(12) Uani 1 d . . H23A H 0.5480(3) -0.3929(3) 0.2353(2) 0.097 Uiso 1 calc R . C24 C 0.4666(4) -0.4661(3) 0.3041(3) 0.0898(13) Uani 1 d . . H24A H 0.5169(4) -0.5361(3) 0.3062(3) 0.108 Uiso 1 calc R . C25 C 0.3749(3) -0.4485(3) 0.3425(2) 0.0729(10) Uani 1 d . . H25A H 0.3619(3) -0.5058(3) 0.3709(2) 0.087 Uiso 1 calc R . C26 C 0.3008(3) -0.3430(3) 0.3385(2) 0.0565(8) Uani 1 d . . N31 N 0.0429(2) -0.2095(2) 0.40668(13) 0.0552(7) Uani 1 d . . N32 N 0.1329(2) -0.2120(2) 0.36993(13) 0.0525(6) Uani 1 d . . C33 C 0.1989(3) -0.3150(3) 0.3763(2) 0.0540(8) Uani 1 d . . C34 C 0.1524(3) -0.3813(3) 0.4182(2) 0.0632(9) Uani 1 d . . H34A H 0.1817(3) -0.4558(3) 0.4311(2) 0.076 Uiso 1 calc R . C35 C 0.0548(3) -0.3108(3) 0.4355(2) 0.0630(9) Uani 1 d . . H35A H 0.0035(3) -0.3297(3) 0.4632(2) 0.076 Uiso 1 calc R . N41 N -0.0961(2) -0.0088(2) 0.35624(14) 0.0564(7) Uani 1 d . . N42 N -0.1314(2) -0.0031(2) 0.29189(14) 0.0532(6) Uani 1 d . . C43 C -0.1781(3) 0.1023(2) 0.2532(2) 0.0547(8) Uani 1 d . . C44 C -0.1731(3) 0.1642(3) 0.2934(2) 0.0646(9) Uani 1 d . . H44A H -0.1997(3) 0.2386(3) 0.2797(2) 0.078 Uiso 1 calc R . C45 C -0.1203(3) 0.0912(3) 0.3571(2) 0.0658(10) Uani 1 d . . H45A H -0.1035(3) 0.1076(3) 0.3954(2) 0.079 Uiso 1 calc R . N51 N -0.2090(2) 0.0472(2) 0.15997(13) 0.0524(6) Uani 1 d . . C52 C -0.2410(3) 0.0609(3) 0.0925(2) 0.0588(9) Uani 1 d . . C53 C -0.2818(3) 0.1625(3) 0.0427(2) 0.0765(11) Uani 1 d . . H53A H -0.3013(3) 0.1726(3) -0.0044(2) 0.092 Uiso 1 calc R . C54 C -0.2934(4) 0.2483(3) 0.0635(2) 0.0855(12) Uani 1 d . . H54A H -0.3234(4) 0.3171(3) 0.0307(2) 0.103 Uiso 1 calc R . C55 C -0.2615(3) 0.2336(3) 0.1313(2) 0.0748(11) Uani 1 d . . H55A H -0.2687(3) 0.2917(3) 0.1451(2) 0.090 Uiso 1 calc R . C56 C -0.2179(3) 0.1309(3) 0.1799(2) 0.0564(8) Uani 1 d . . N61 N -0.2044(2) -0.1228(2) 0.13936(14) 0.0560(7) Uani 1 d . . C62 C -0.2298(3) -0.0377(3) 0.0797(2) 0.0552(8) Uani 1 d . . C63 C -0.2436(3) -0.0443(3) 0.0127(2) 0.0698(10) Uani 1 d . . H63A H -0.2604(3) 0.0151(3) -0.0279(2) 0.084 Uiso 1 calc R . C64 C -0.2324(3) -0.1390(4) 0.0067(2) 0.0794(11) Uani 1 d . . H64A H -0.2411(3) -0.1448(4) -0.0381(2) 0.095 Uiso 1 calc R . C65 C -0.2080(3) -0.2262(3) 0.0675(2) 0.0768(11) Uani 1 d . . H65A H -0.2005(3) -0.2914(3) 0.0648(2) 0.092 Uiso 1 calc R . C66 C -0.1951(3) -0.2137(3) 0.1324(2) 0.0695(10) Uani 1 d . . H66A H -0.1791(3) -0.2722(3) 0.1735(2) 0.083 Uiso 1 calc R . B2 B 0.1261(4) -0.1276(4) 0.1262(2) 0.0668(11) Uani 1 d . . H2A H 0.2046(4) -0.1526(4) 0.1192(2) 0.080 Uiso 1 calc R . H2B H 0.0889(4) -0.1105(4) 0.0806(2) 0.080 Uiso 1 calc R . N71 N 0.3076(2) -0.1455(2) 0.40621(14) 0.0572(7) Uani 1 d . . C72 C 0.2666(3) -0.0585(3) 0.4300(2) 0.0566(8) Uani 1 d . . C73 C 0.3040(3) -0.0637(3) 0.4958(2) 0.0717(10) Uani 1 d . . H73A H 0.2738(3) -0.0043(3) 0.5126(2) 0.086 Uiso 1 calc R . C74 C 0.3876(4) -0.1602(4) 0.5351(2) 0.0842(12) Uani 1 d . . H74A H 0.4145(4) -0.1661(4) 0.5791(2) 0.101 Uiso 1 calc R . C75 C 0.4308(4) -0.2466(4) 0.5102(2) 0.0802(11) Uani 1 d . . H75A H 0.4884(4) -0.3111(4) 0.5359(2) 0.096 Uiso 1 calc R . C76 C 0.3872(3) -0.2361(3) 0.4457(2) 0.0704(10) Uani 1 d . . H76A H 0.4152(3) -0.2958(3) 0.4292(2) 0.084 Uiso 1 calc R . N81 N 0.1570(2) 0.0274(2) 0.31990(14) 0.0516(6) Uani 1 d . . C82 C 0.1841(3) 0.0412(3) 0.3795(2) 0.0559(8) Uani 1 d . . C83 C 0.1423(3) 0.1436(3) 0.3870(2) 0.0693(10) Uani 1 d . . H83A H 0.1607(3) 0.1533(3) 0.4279(2) 0.083 Uiso 1 calc R . C84 C 0.0734(3) 0.2295(3) 0.3326(2) 0.0745(11) Uani 1 d . . H84A H 0.0438(3) 0.2983(3) 0.3371(2) 0.089 Uiso 1 calc R . C85 C 0.0470(3) 0.2158(3) 0.2711(2) 0.0687(10) Uani 1 d . . H85A H 0.0011(3) 0.2748(3) 0.2340(2) 0.082 Uiso 1 calc R . C86 C 0.0900(3) 0.1129(3) 0.2657(2) 0.0562(8) Uani 1 d . . N91 N 0.0831(2) -0.0255(2) 0.14866(13) 0.0542(7) Uani 1 d . . N92 N 0.1140(2) -0.0200(2) 0.21085(13) 0.0516(6) Uani 1 d . . C93 C 0.0711(3) 0.0843(3) 0.2055(2) 0.0538(8) Uani 1 d . . C94 C 0.0130(3) 0.1483(3) 0.1388(2) 0.0642(9) Uani 1 d . . H94A H -0.0233(3) 0.2230(3) 0.1213(2) 0.077 Uiso 1 calc R . C95 C 0.0217(3) 0.0763(3) 0.1057(2) 0.0626(9) Uani 1 d . . H95A H -0.0097(3) 0.0940(3) 0.0603(2) 0.075 Uiso 1 calc R . N101 N 0.1074(2) -0.2197(2) 0.18257(14) 0.0556(7) Uani 1 d . . N102 N 0.0157(2) -0.2096(2) 0.21886(13) 0.0512(6) Uani 1 d . . C103 C 0.0315(3) -0.3098(3) 0.2551(2) 0.0543(8) Uani 1 d . . C104 C 0.1330(3) -0.3843(3) 0.2418(2) 0.0682(10) Uani 1 d . . H10A H 0.1635(3) -0.4588(3) 0.2604(2) 0.082 Uiso 1 calc R . C105 C 0.1785(3) -0.3252(3) 0.1960(2) 0.0694(10) Uani 1 d . . H10B H 0.2472(3) -0.3526(3) 0.1769(2) 0.083 Uiso 1 calc R . N111 N -0.1428(2) -0.2324(2) 0.30318(13) 0.0539(7) Uani 1 d . . C112 C -0.2244(3) -0.2360(3) 0.3471(2) 0.0630(9) Uani 1 d . . C113 C -0.2172(4) -0.3329(4) 0.3922(2) 0.0871(13) Uani 1 d . . H11A H -0.2730(4) -0.3348(4) 0.4230(2) 0.104 Uiso 1 calc R . C114 C -0.1263(5) -0.4266(4) 0.3909(2) 0.0968(15) Uani 1 d . . H11B H -0.1210(5) -0.4924(4) 0.4205(2) 0.116 Uiso 1 calc R . C115 C -0.0430(4) -0.4232(3) 0.3459(2) 0.0768(11) Uani 1 d . . H11C H 0.0184(4) -0.4863(3) 0.3446(2) 0.092 Uiso 1 calc R . C116 C -0.0525(3) -0.3243(3) 0.3028(2) 0.0582(8) Uani 1 d . . N121 N -0.3271(3) -0.0509(2) 0.2834(2) 0.0658(8) Uani 1 d . . C122 C -0.3200(3) -0.1302(3) 0.3421(2) 0.0626(9) Uani 1 d . . C123 C -0.3955(4) -0.1141(4) 0.3937(2) 0.0858(13) Uani 1 d . . H12A H -0.3887(4) -0.1707(4) 0.4345(2) 0.103 Uiso 1 calc R . C124 C -0.4817(4) -0.0131(4) 0.3844(3) 0.0943(14) Uani 1 d . . H12B H -0.5329(4) -0.0003(4) 0.4193(3) 0.113 Uiso 1 calc R . C125 C -0.4912(3) 0.0680(4) 0.3235(3) 0.0853(12) Uani 1 d . . H12C H -0.5495(3) 0.1365(4) 0.3155(3) 0.102 Uiso 1 calc R . C126 C -0.4127(3) 0.0457(3) 0.2749(2) 0.0774(11) Uani 1 d . . H12D H -0.4191(3) 0.1009(3) 0.2333(2) 0.093 Uiso 1 calc R . B3 B -0.2138(6) 0.4794(6) 0.1954(4) 0.108(2) Uani 1 d . . F31 F -0.1425(4) 0.4581(4) 0.2492(3) 0.229(2) Uani 1 d . . F32 F -0.2803(4) 0.4353(3) 0.2242(3) 0.195(2) Uani 1 d . . F33 F -0.1569(3) 0.4285(3) 0.1493(2) 0.182(2) Uani 1 d . . F34 F -0.2763(3) 0.5860(2) 0.1673(2) 0.1479(13) Uani 1 d . . C1 C 0.2337(5) -0.3521(5) 0.5830(3) 0.124(2) Uani 1 d . . H1A H 0.1871(22) -0.3030(15) 0.5405(7) 0.186 Uiso 1 calc R . H1B H 0.2699(5) -0.3183(19) 0.5989(22) 0.186 Uiso 1 calc R . H1C H 0.1894(23) -0.3719(7) 0.6201(16) 0.186 Uiso 1 calc R . C2 C 0.3157(5) -0.4470(6) 0.5672(3) 0.107(2) Uani 1 d . . N2 N 0.3805(5) -0.5210(5) 0.5538(3) 0.141(2) Uani 1 d . . C3 C 0.4449(13) -0.6311(11) 0.2013(8) 0.335(10) Uani 1 d . . H3A H 0.5213(24) -0.6736(69) 0.2184(58) 0.503 Uiso 1 calc R . H3B H 0.4199(129) -0.6732(71) 0.1849(26) 0.503 Uiso 1 calc R . H3C H 0.4013(111) -0.6090(11) 0.2397(38) 0.503 Uiso 1 calc R . C4 C 0.4314(9) -0.5223(16) 0.1334(9) 0.241(7) Uani 1 d . . N4 N 0.4338(35) -0.4780(28) 0.0927(16) 0.905(45) Uani 1 d . . C5 C -0.3892(12) -0.4090(12) 0.0269(8) 0.307(7) Uani 1 d . . H5A H -0.3182(58) -0.4459(12) 0.0097(65) 0.460 Uiso 1 calc R . H5B H -0.4415(65) -0.4279(20) 0.0121(67) 0.460 Uiso 1 calc R . H5C H -0.3833(121) -0.4293(21) 0.0784(8) 0.460 Uiso 1 calc R . O5 O -0.4368(8) -0.2625(12) -0.0105(5) 0.368(7) Uani 1 d . . H5 H -0.4626(157) -0.2341(24) 0.0212(26) 0.553 Uiso 1 calc R . B4 B 0.7203(6) -0.3047(4) 0.6005(4) 0.103(2) Uani 1 d . . F43 F 0.6923(3) -0.3518(2) 0.5590(2) 0.1460(12) Uani 1 d . . F44 F 0.6694(2) -0.1964(2) 0.5711(2) 0.1065(8) Uani 1 d . . F41A F 0.6222(8) -0.3205(6) 0.6457(4) 0.137(4) Uani 0.482(10) d P 1 F42A F 0.7963(10) -0.3539(7) 0.6457(10) 0.179(9) Uani 0.482(10) d P 1 F41B F 0.7299(11) -0.3283(9) 0.6681(4) 0.170(6) Uani 0.518(10) d P 2 F42B F 0.8340(5) -0.3333(6) 0.5717(5) 0.115(3) Uani 0.518(10) d P 2 C6 C -0.1933(22) 0.6959(17) -0.1201(15) 0.230(11) Uani 0.50 d P . C7 C -0.1373(15) 0.5597(23) -0.0929(11) 0.289(17) Uani 0.50 d P . C8 C -0.1440(23) 0.6073(26) -0.1549(11) 0.256(13) Uani 0.50 d P . C9 C -0.0820(14) 0.4016(26) -0.0481(13) 0.341(18) Uani 0.50 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0522(2) 0.0528(2) 0.0480(2) -0.0155(2) 0.0037(2) -0.0213(2) Cu2 0.0561(2) 0.0508(2) 0.0480(2) -0.0156(2) 0.0084(2) -0.0244(2) B1 0.076(3) 0.072(3) 0.050(2) -0.019(2) 0.014(2) -0.032(2) N11 0.059(2) 0.067(2) 0.064(2) -0.017(2) 0.0084(15) -0.028(2) C12 0.045(2) 0.077(3) 0.062(2) -0.019(2) 0.006(2) -0.022(2) C13 0.069(3) 0.092(3) 0.105(3) -0.025(3) 0.032(3) -0.024(2) C14 0.068(3) 0.108(4) 0.119(4) -0.014(3) 0.030(3) -0.036(3) C15 0.078(3) 0.104(4) 0.104(3) -0.005(3) 0.006(3) -0.054(3) C16 0.078(3) 0.083(3) 0.087(3) -0.019(2) 0.007(2) -0.036(2) N21 0.050(2) 0.057(2) 0.0484(14) -0.0177(13) 0.0021(12) -0.0184(13) C22 0.051(2) 0.067(2) 0.063(2) -0.023(2) 0.002(2) -0.015(2) C23 0.059(2) 0.074(3) 0.086(3) -0.029(2) 0.010(2) -0.007(2) C24 0.070(3) 0.061(3) 0.112(3) -0.029(3) -0.004(3) -0.003(2) C25 0.064(2) 0.056(2) 0.081(3) -0.015(2) -0.006(2) -0.014(2) C26 0.058(2) 0.052(2) 0.052(2) -0.014(2) -0.008(2) -0.017(2) N31 0.063(2) 0.056(2) 0.0437(14) -0.0087(12) 0.0026(13) -0.0287(14) N32 0.057(2) 0.050(2) 0.0480(14) -0.0098(12) 0.0024(13) -0.0245(14) C33 0.061(2) 0.050(2) 0.047(2) -0.0097(15) -0.005(2) -0.023(2) C34 0.072(2) 0.055(2) 0.059(2) -0.008(2) -0.002(2) -0.030(2) C35 0.077(3) 0.065(2) 0.051(2) -0.006(2) 0.005(2) -0.044(2) N41 0.059(2) 0.054(2) 0.055(2) -0.0213(13) 0.0147(13) -0.0235(14) N42 0.060(2) 0.050(2) 0.053(2) -0.0213(13) 0.0152(13) -0.0261(13) C43 0.061(2) 0.043(2) 0.060(2) -0.016(2) 0.014(2) -0.024(2) C44 0.074(2) 0.044(2) 0.074(2) -0.021(2) 0.014(2) -0.024(2) C45 0.075(2) 0.064(2) 0.074(2) -0.040(2) 0.023(2) -0.036(2) N51 0.051(2) 0.052(2) 0.0482(15) -0.0126(12) 0.0106(12) -0.0215(13) C52 0.058(2) 0.062(2) 0.050(2) -0.011(2) 0.011(2) -0.026(2) C53 0.084(3) 0.068(3) 0.055(2) -0.005(2) -0.001(2) -0.023(2) C54 0.094(3) 0.053(2) 0.082(3) -0.001(2) 0.000(2) -0.022(2) C55 0.083(3) 0.054(2) 0.077(3) -0.014(2) 0.008(2) -0.026(2) C56 0.057(2) 0.049(2) 0.060(2) -0.016(2) 0.014(2) -0.023(2) N61 0.056(2) 0.055(2) 0.051(2) -0.0142(13) 0.0048(13) -0.0213(14) C62 0.048(2) 0.065(2) 0.048(2) -0.015(2) 0.0077(15) -0.024(2) C63 0.075(3) 0.082(3) 0.050(2) -0.015(2) 0.004(2) -0.037(2) C64 0.090(3) 0.101(3) 0.059(2) -0.034(2) 0.005(2) -0.046(3) C65 0.085(3) 0.078(3) 0.076(3) -0.032(2) 0.004(2) -0.038(2) C66 0.073(3) 0.065(2) 0.062(2) -0.014(2) 0.001(2) -0.026(2) B2 0.077(3) 0.079(3) 0.050(2) -0.025(2) 0.013(2) -0.038(2) N71 0.058(2) 0.062(2) 0.054(2) -0.0199(14) 0.0040(13) -0.0274(15) C72 0.057(2) 0.074(2) 0.051(2) -0.020(2) 0.010(2) -0.040(2) C73 0.079(3) 0.094(3) 0.058(2) -0.031(2) 0.009(2) -0.048(2) C74 0.088(3) 0.120(4) 0.056(2) -0.020(2) -0.008(2) -0.058(3) C75 0.080(3) 0.086(3) 0.073(3) -0.015(2) -0.013(2) -0.038(2) C76 0.069(2) 0.066(2) 0.074(2) -0.013(2) -0.005(2) -0.031(2) N81 0.051(2) 0.057(2) 0.0521(15) -0.0211(13) 0.0092(12) -0.0263(13) C82 0.056(2) 0.065(2) 0.057(2) -0.024(2) 0.014(2) -0.035(2) C83 0.075(3) 0.075(3) 0.076(2) -0.037(2) 0.013(2) -0.041(2) C84 0.083(3) 0.057(2) 0.093(3) -0.035(2) 0.014(2) -0.033(2) C85 0.067(2) 0.053(2) 0.081(3) -0.017(2) 0.003(2) -0.024(2) C86 0.054(2) 0.052(2) 0.060(2) -0.014(2) 0.007(2) -0.024(2) N91 0.058(2) 0.060(2) 0.0457(14) -0.0137(13) 0.0070(13) -0.0292(14) N92 0.053(2) 0.051(2) 0.0469(14) -0.0121(12) 0.0064(12) -0.0222(13) C93 0.055(2) 0.049(2) 0.054(2) -0.0113(15) 0.006(2) -0.024(2) C94 0.065(2) 0.052(2) 0.063(2) -0.003(2) -0.003(2) -0.023(2) C95 0.064(2) 0.070(2) 0.048(2) -0.005(2) -0.002(2) -0.032(2) N101 0.059(2) 0.058(2) 0.0498(15) -0.0214(13) 0.0078(13) -0.0235(14) N102 0.054(2) 0.049(2) 0.0477(14) -0.0168(12) 0.0049(12) -0.0203(13) C103 0.061(2) 0.046(2) 0.052(2) -0.0153(15) -0.004(2) -0.019(2) C104 0.073(2) 0.044(2) 0.077(2) -0.020(2) -0.003(2) -0.015(2) C105 0.064(2) 0.062(2) 0.074(2) -0.030(2) 0.008(2) -0.016(2) N111 0.065(2) 0.057(2) 0.0470(14) -0.0149(12) 0.0044(13) -0.0340(15) C112 0.074(2) 0.071(2) 0.056(2) -0.016(2) 0.012(2) -0.046(2) C113 0.102(3) 0.083(3) 0.081(3) -0.009(2) 0.024(2) -0.060(3) C114 0.127(4) 0.073(3) 0.093(3) 0.005(2) 0.004(3) -0.066(3) C115 0.094(3) 0.052(2) 0.079(3) -0.008(2) -0.003(2) -0.035(2) C116 0.071(2) 0.050(2) 0.054(2) -0.010(2) -0.005(2) -0.030(2) N121 0.078(2) 0.067(2) 0.063(2) -0.023(2) 0.022(2) -0.042(2) C122 0.068(2) 0.077(2) 0.058(2) -0.023(2) 0.017(2) -0.046(2) C123 0.090(3) 0.104(3) 0.071(3) -0.021(2) 0.032(2) -0.059(3) C124 0.079(3) 0.117(4) 0.097(3) -0.042(3) 0.041(3) -0.052(3) C125 0.072(3) 0.087(3) 0.108(3) -0.043(3) 0.027(3) -0.041(2) C126 0.082(3) 0.074(3) 0.080(3) -0.030(2) 0.025(2) -0.037(2) B3 0.087(4) 0.090(5) 0.103(4) -0.019(4) 0.010(4) -0.012(4) F31 0.203(5) 0.187(4) 0.252(5) -0.118(4) -0.069(4) 0.001(4) F32 0.204(4) 0.095(2) 0.253(5) -0.033(3) 0.070(4) -0.061(3) F33 0.154(3) 0.161(3) 0.138(3) -0.059(3) 0.016(2) 0.016(3) F34 0.129(2) 0.062(2) 0.200(3) -0.009(2) 0.027(2) -0.021(2) C1 0.129(5) 0.145(5) 0.123(4) -0.065(4) 0.022(4) -0.069(4) C2 0.107(5) 0.129(5) 0.096(4) -0.023(4) -0.012(3) -0.066(4) N2 0.114(4) 0.137(5) 0.166(5) -0.043(4) -0.023(4) -0.045(4) C3 0.430(23) 0.244(14) 0.295(16) -0.125(12) 0.154(16) -0.114(14) C4 0.160(8) 0.371(20) 0.274(15) -0.254(16) 0.088(9) -0.099(11) N4 1.074(81) 0.662(46) 0.427(31) 0.011(31) -0.240(40) 0.016(48) C5 0.351(19) 0.333(18) 0.218(12) -0.015(12) -0.038(12) -0.172(16) O5 0.224(8) 0.711(23) 0.243(8) -0.104(11) 0.043(6) -0.302(13) B4 0.122(6) 0.056(3) 0.127(5) -0.007(3) -0.048(5) -0.039(3) F43 0.171(3) 0.103(2) 0.178(3) -0.044(2) -0.007(3) -0.069(2) F44 0.099(2) 0.0602(15) 0.141(2) -0.0221(14) -0.004(2) -0.0223(13) F41A 0.150(8) 0.110(5) 0.150(6) -0.019(4) 0.022(6) -0.071(5) F42A 0.128(9) 0.069(4) 0.296(23) 0.003(8) -0.120(12) -0.023(6) F41B 0.171(12) 0.172(9) 0.076(5) 0.017(5) 0.005(6) -0.034(8) F42B 0.075(4) 0.096(4) 0.167(7) -0.063(5) 0.009(4) -0.017(3) C6 0.303(26) 0.194(18) 0.271(23) -0.102(18) 0.189(21) -0.185(20) C7 0.145(14) 0.331(33) 0.167(17) 0.012(19) 0.076(13) 0.015(17) C8 0.331(31) 0.395(37) 0.176(17) -0.029(19) 0.068(18) -0.322(32) C9 0.101(12) 0.489(42) 0.297(26) -0.225(29) -0.042(14) 0.060(18) _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 N81 1.949(3) . ? Cu1 N21 1.977(3) . ? Cu1 N71 2.157(3) . ? Cu1 N92 2.169(3) . ? Cu1 N11 2.275(3) . ? Cu1 N32 2.307(3) . ? Cu2 N51 1.970(3) . ? Cu2 N111 1.975(3) . ? Cu2 N61 2.179(3) . ? Cu2 N42 2.191(3) . ? Cu2 N102 2.273(3) . ? Cu2 N121 2.278(3) . ? B1 N31 1.541(5) . ? B1 N41 1.552(5) . ? N11 C16 1.332(5) . ? N11 C12 1.338(4) . ? C12 C13 1.394(5) . ? C12 C22 1.482(5) . ? C13 C14 1.366(6) . ? C14 C15 1.362(7) . ? C15 C16 1.379(6) . ? N21 C26 1.346(4) . ? N21 C22 1.350(4) . ? C22 C23 1.373(5) . ? C23 C24 1.383(6) . ? C24 C25 1.359(6) . ? C25 C26 1.392(5) . ? C26 C33 1.459(5) . ? N31 C35 1.348(4) . ? N31 N32 1.353(3) . ? N32 C33 1.331(4) . ? C33 C34 1.405(4) . ? C34 C35 1.357(5) . ? N41 C45 1.351(4) . ? N41 N42 1.352(4) . ? N42 C43 1.352(4) . ? C43 C44 1.397(5) . ? C43 C56 1.446(5) . ? C44 C45 1.361(5) . ? N51 C56 1.348(4) . ? N51 C52 1.354(4) . ? C52 C53 1.386(5) . ? C52 C62 1.477(5) . ? C53 C54 1.375(6) . ? C54 C55 1.356(6) . ? C55 C56 1.386(5) . ? N61 C66 1.326(4) . ? N61 C62 1.348(4) . ? C62 C63 1.380(5) . ? C63 C64 1.362(5) . ? C64 C65 1.379(5) . ? C65 C66 1.375(5) . ? B2 N91 1.530(5) . ? B2 N101 1.559(5) . ? N71 C76 1.320(4) . ? N71 C72 1.352(4) . ? C72 C73 1.393(5) . ? C72 C82 1.479(5) . ? C73 C74 1.381(6) . ? C74 C75 1.358(6) . ? C75 C76 1.377(5) . ? N81 C82 1.352(4) . ? N81 C86 1.355(4) . ? C82 C83 1.392(5) . ? C83 C84 1.369(5) . ? C84 C85 1.382(5) . ? C85 C86 1.383(5) . ? C86 C93 1.446(5) . ? N91 C95 1.358(4) . ? N91 N92 1.359(3) . ? N92 C93 1.336(4) . ? C93 C94 1.401(4) . ? C94 C95 1.355(5) . ? N101 N102 1.348(3) . ? N101 C105 1.353(4) . ? N102 C103 1.340(4) . ? C103 C104 1.383(5) . ? C103 C116 1.457(5) . ? C104 C105 1.353(5) . ? N111 C112 1.351(4) . ? N111 C116 1.352(4) . ? C112 C113 1.382(5) . ? C112 C122 1.485(5) . ? C113 C114 1.376(6) . ? C114 C115 1.380(6) . ? C115 C116 1.383(4) . ? N121 C122 1.329(4) . ? N121 C126 1.335(5) . ? C122 C123 1.372(5) . ? C123 C124 1.377(6) . ? C124 C125 1.363(6) . ? C125 C126 1.361(5) . ? B3 F33 1.320(7) . ? B3 F32 1.323(8) . ? B3 F34 1.346(7) . ? B3 F31 1.358(8) . ? C1 C2 1.441(8) . ? C2 N2 1.137(7) . ? C3 C4 1.67(2) . ? C4 N4 0.87(4) . ? C5 O5 1.844(14) . ? B4 F42A 1.208(10) . ? B4 F41B 1.265(11) . ? B4 F44 1.355(6) . ? B4 F43 1.382(7) . ? B4 F42B 1.510(10) . ? B4 F41A 1.598(11) . ? C6 C8 1.51(3) . ? C6 C7 1.70(3) . ? C7 C8 1.19(2) . ? C7 C9 1.99(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 N81 Cu1 N21 169.08(11) . . ? N81 Cu1 N71 78.15(11) . . ? N21 Cu1 N71 94.02(11) . . ? N81 Cu1 N92 78.95(11) . . ? N21 Cu1 N92 108.48(10) . . ? N71 Cu1 N92 157.06(11) . . ? N81 Cu1 N11 96.11(11) . . ? N21 Cu1 N11 76.76(11) . . ? N71 Cu1 N11 94.60(10) . . ? N92 Cu1 N11 86.49(10) . . ? N81 Cu1 N32 109.55(10) . . ? N21 Cu1 N32 77.60(10) . . ? N71 Cu1 N32 89.10(10) . . ? N92 Cu1 N32 99.82(9) . . ? N11 Cu1 N32 154.28(11) . . ? N51 Cu2 N111 168.44(11) . . ? N51 Cu2 N61 77.67(11) . . ? N111 Cu2 N61 96.70(11) . . ? N51 Cu2 N42 78.31(11) . . ? N111 Cu2 N42 107.40(10) . . ? N61 Cu2 N42 155.84(10) . . ? N51 Cu2 N102 111.56(10) . . ? N111 Cu2 N102 77.64(11) . . ? N61 Cu2 N102 85.27(10) . . ? N42 Cu2 N102 101.25(10) . . ? N51 Cu2 N121 94.07(11) . . ? N111 Cu2 N121 76.57(11) . . ? N61 Cu2 N121 97.94(11) . . ? N42 Cu2 N121 86.28(10) . . ? N102 Cu2 N121 154.21(10) . . ? N31 B1 N41 113.4(3) . . ? C16 N11 C12 118.9(3) . . ? C16 N11 Cu1 129.4(3) . . ? C12 N11 Cu1 110.5(2) . . ? N11 C12 C13 120.7(4) . . ? N11 C12 C22 115.6(3) . . ? C13 C12 C22 123.7(4) . . ? C14 C13 C12 119.4(4) . . ? C15 C14 C13 119.7(4) . . ? C14 C15 C16 118.4(4) . . ? N11 C16 C15 122.9(4) . . ? C26 N21 C22 119.8(3) . . ? C26 N21 Cu1 119.1(2) . . ? C22 N21 Cu1 120.6(2) . . ? N21 C22 C23 121.1(4) . . ? N21 C22 C12 115.3(3) . . ? C23 C22 C12 123.6(3) . . ? C22 C23 C24 118.8(4) . . ? C25 C24 C23 120.6(4) . . ? C24 C25 C26 118.5(4) . . ? N21 C26 C25 121.1(3) . . ? N21 C26 C33 115.8(3) . . ? C25 C26 C33 123.1(3) . . ? C35 N31 N32 109.1(3) . . ? C35 N31 B1 124.0(3) . . ? N32 N31 B1 126.4(3) . . ? C33 N32 N31 106.4(2) . . ? C33 N32 Cu1 107.0(2) . . ? N31 N32 Cu1 146.4(2) . . ? N32 C33 C34 111.0(3) . . ? N32 C33 C26 119.2(3) . . ? C34 C33 C26 129.7(3) . . ? C35 C34 C33 103.5(3) . . ? N31 C35 C34 110.0(3) . . ? C45 N41 N42 109.2(3) . . ? C45 N41 B1 124.4(3) . . ? N42 N41 B1 125.8(3) . . ? C43 N42 N41 106.4(3) . . ? C43 N42 Cu2 109.2(2) . . ? N41 N42 Cu2 143.8(2) . . ? N42 C43 C44 110.3(3) . . ? N42 C43 C56 117.9(3) . . ? C44 C43 C56 131.7(3) . . ? C45 C44 C43 104.3(3) . . ? N41 C45 C44 109.8(3) . . ? C56 N51 C52 121.2(3) . . ? C56 N51 Cu2 119.0(2) . . ? C52 N51 Cu2 119.7(2) . . ? N51 C52 C53 119.4(3) . . ? N51 C52 C62 114.8(3) . . ? C53 C52 C62 125.8(3) . . ? C54 C53 C52 119.4(4) . . ? C55 C54 C53 120.6(4) . . ? C54 C55 C56 119.2(4) . . ? N51 C56 C55 120.2(3) . . ? N51 C56 C43 114.2(3) . . ? C55 C56 C43 125.6(3) . . ? C66 N61 C62 117.9(3) . . ? C66 N61 Cu2 128.7(2) . . ? C62 N61 Cu2 112.7(2) . . ? N61 C62 C63 121.8(3) . . ? N61 C62 C52 114.4(3) . . ? C63 C62 C52 123.9(3) . . ? C64 C63 C62 119.2(4) . . ? C63 C64 C65 119.6(4) . . ? C66 C65 C64 117.9(4) . . ? N61 C66 C65 123.6(4) . . ? N91 B2 N101 112.9(3) . . ? C76 N71 C72 118.6(3) . . ? C76 N71 Cu1 128.7(3) . . ? C72 N71 Cu1 112.6(2) . . ? N71 C72 C73 121.6(3) . . ? N71 C72 C82 114.6(3) . . ? C73 C72 C82 123.8(3) . . ? C74 C73 C72 117.7(4) . . ? C75 C74 C73 120.6(4) . . ? C74 C75 C76 118.3(4) . . ? N71 C76 C75 123.2(4) . . ? C82 N81 C86 120.8(3) . . ? C82 N81 Cu1 120.2(2) . . ? C86 N81 Cu1 118.7(2) . . ? N81 C82 C83 120.5(3) . . ? N81 C82 C72 114.0(3) . . ? C83 C82 C72 125.2(3) . . ? C84 C83 C82 118.4(4) . . ? C83 C84 C85 121.1(4) . . ? C84 C85 C86 118.7(4) . . ? N81 C86 C85 120.4(3) . . ? N81 C86 C93 113.7(3) . . ? C85 C86 C93 125.9(3) . . ? C95 N91 N92 108.4(3) . . ? C95 N91 B2 125.6(3) . . ? N92 N91 B2 125.3(3) . . ? C93 N92 N91 106.8(3) . . ? C93 N92 Cu1 109.5(2) . . ? N91 N92 Cu1 142.9(2) . . ? N92 C93 C94 110.7(3) . . ? N92 C93 C86 118.2(3) . . ? C94 C93 C86 131.1(3) . . ? C95 C94 C93 104.0(3) . . ? C94 C95 N91 110.1(3) . . ? N102 N101 C105 109.5(3) . . ? N102 N101 B2 126.6(3) . . ? C105 N101 B2 123.4(3) . . ? C103 N102 N101 106.1(3) . . ? C103 N102 Cu2 107.9(2) . . ? N101 N102 Cu2 145.4(2) . . ? N102 C103 C104 110.6(3) . . ? N102 C103 C116 118.6(3) . . ? C104 C103 C116 130.8(3) . . ? C105 C104 C103 105.1(3) . . ? C104 C105 N101 108.7(3) . . ? C112 N111 C116 120.2(3) . . ? C112 N111 Cu2 120.2(2) . . ? C116 N111 Cu2 119.3(2) . . ? N111 C112 C113 120.8(4) . . ? N111 C112 C122 115.3(3) . . ? C113 C112 C122 123.9(3) . . ? C114 C113 C112 119.0(4) . . ? C113 C114 C115 120.2(4) . . ? C114 C115 C116 118.8(4) . . ? N111 C116 C115 120.9(3) . . ? N111 C116 C103 115.1(3) . . ? C115 C116 C103 124.0(3) . . ? C122 N121 C126 117.9(3) . . ? C122 N121 Cu2 110.0(2) . . ? C126 N121 Cu2 129.3(2) . . ? N121 C122 C123 121.9(4) . . ? N121 C122 C112 114.9(3) . . ? C123 C122 C112 123.2(3) . . ? C122 C123 C124 119.1(4) . . ? C125 C124 C123 119.3(4) . . ? C126 C125 C124 118.1(4) . . ? N121 C126 C125 123.7(4) . . ? F33 B3 F32 106.3(7) . . ? F33 B3 F34 115.8(6) . . ? F32 B3 F34 108.0(5) . . ? F33 B3 F31 108.5(5) . . ? F32 B3 F31 107.0(6) . . ? F34 B3 F31 110.8(7) . . ? N2 C2 C1 179.0(7) . . ? N4 C4 C3 165.5(28) . . ? F42A B4 F44 125.2(6) . . ? F41B B4 F44 109.5(8) . . ? F42A B4 F43 123.5(7) . . ? F41B B4 F43 129.9(8) . . ? F44 B4 F43 109.5(5) . . ? F41B B4 F42B 108.5(8) . . ? F44 B4 F42B 101.8(6) . . ? F43 B4 F42B 93.0(6) . . ? F42A B4 F41A 101.2(10) . . ? F44 B4 F41A 99.1(6) . . ? F43 B4 F41A 81.6(5) . . ? C8 C6 C7 43.0(10) . . ? C8 C7 C6 60.1(19) . . ? C8 C7 C9 127.5(30) . . ? C6 C7 C9 172.0(16) . . ? C7 C8 C6 76.9(21) . . ? _refine_diff_density_max 0.627 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.080 #=END data_/tintin3/people/sam/gim/gim _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C31 H32 B Gd N11 O7.50' _chemical_formula_weight 846.74 _chemical_melting_point ? _chemical_compound_source ? 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0077(12) _cell_length_b 13.0213(13) _cell_length_c 14.719(3) _cell_angle_alpha 70.236(12) _cell_angle_beta 71.349(7) _cell_angle_gamma 79.566(8) _cell_volume 1704.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 228 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Cube _exptl_crystal_colour Clear/white _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method ? _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 2.011 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.589354 _exptl_absorpt_correction_T_max 0.694165 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD Area Detector' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17644 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7705 _reflns_number_observed 6657 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXTL (Sheldrick, 1995)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1995)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1995)' _computing_publication_material 'SHELXTL (Sheldrick, 1995)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7705 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_obs 0.0245 _refine_ls_wR_factor_all 0.0620 _refine_ls_wR_factor_obs 0.0563 _refine_ls_goodness_of_fit_all 1.015 _refine_ls_goodness_of_fit_obs 0.997 _refine_ls_restrained_S_all 1.015 _refine_ls_restrained_S_obs 0.997 _refine_ls_shift/esd_max 0.096 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Gd1 Gd 0.211121(13) 0.306480(11) 0.278429(11) 0.01858(5) Uani 1 d . . B1 B 0.2854(4) -0.0090(3) 0.2830(3) 0.0358(9) Uani 1 d . . H1A H 0.3008(4) -0.0895(3) 0.3100(3) 0.043 Uiso 1 calc R . H1B H 0.2965(4) 0.0097(3) 0.2101(3) 0.043 Uiso 1 calc R . N11 N 0.2475(2) 0.5062(2) 0.1469(2) 0.0228(5) Uani 1 d . . C12 C 0.3758(3) 0.5468(2) 0.1118(2) 0.0207(6) Uani 1 d . . C13 C 0.3951(3) 0.6542(2) 0.0516(2) 0.0276(7) Uani 1 d . . H13A H 0.4867(3) 0.6803(2) 0.0262(2) 0.033 Uiso 1 calc R . C14 C 0.2802(3) 0.7228(3) 0.0290(2) 0.0317(7) Uani 1 d . . H14A H 0.2913(3) 0.7969(3) -0.0110(2) 0.038 Uiso 1 calc R . C15 C 0.1491(3) 0.6821(3) 0.0654(2) 0.0312(7) Uani 1 d . . H15A H 0.0681(3) 0.7276(3) 0.0512(2) 0.037 Uiso 1 calc R . C16 C 0.1380(3) 0.5745(2) 0.1226(2) 0.0260(7) Uani 1 d . . H16A H 0.0476(3) 0.5468(2) 0.1464(2) 0.031 Uiso 1 calc R . N21 N 0.4650(2) 0.3652(2) 0.1900(2) 0.0221(5) Uani 1 d . . C22 C 0.4950(3) 0.4692(2) 0.1407(2) 0.0225(6) Uani 1 d . . C23 C 0.6296(3) 0.5036(3) 0.1176(2) 0.0298(7) Uani 1 d . . H23A H 0.6475(3) 0.5783(3) 0.0842(2) 0.036 Uiso 1 calc R . C24 C 0.7362(3) 0.4265(3) 0.1443(2) 0.0326(7) Uani 1 d . . H24A H 0.8284(3) 0.4480(3) 0.1299(2) 0.039 Uiso 1 calc R . C25 C 0.7082(3) 0.3187(3) 0.1917(2) 0.0294(7) Uani 1 d . . H25A H 0.7810(3) 0.2648(3) 0.2092(2) 0.035 Uiso 1 calc R . C26 C 0.5709(3) 0.2896(3) 0.2138(2) 0.0247(6) Uani 1 d . . N31 N 0.3973(3) 0.0463(2) 0.2995(2) 0.0293(6) Uani 1 d . . N32 N 0.4026(2) 0.1567(2) 0.2646(2) 0.0262(5) Uani 1 d . . C33 C 0.5330(3) 0.1766(3) 0.2581(2) 0.0265(7) Uani 1 d . . C34 C 0.6124(3) 0.0785(3) 0.2902(3) 0.0368(8) Uani 1 d . . H34A H 0.7073(3) 0.0691(3) 0.2936(3) 0.044 Uiso 1 calc R . C35 C 0.5223(3) -0.0014(3) 0.3159(3) 0.0365(8) Uani 1 d . . H35A H 0.5446(3) -0.0779(3) 0.3411(3) 0.044 Uiso 1 calc R . N41 N 0.1330(3) 0.0300(2) 0.3365(2) 0.0275(6) Uani 1 d . . N42 N 0.0864(2) 0.1367(2) 0.3298(2) 0.0233(5) Uani 1 d . . C43 C -0.0535(3) 0.1361(2) 0.3781(2) 0.0242(6) Uani 1 d . . C44 C -0.0971(3) 0.0305(3) 0.4136(2) 0.0307(7) Uani 1 d . . H44A H -0.1898(3) 0.0081(3) 0.4487(2) 0.037 Uiso 1 calc R . C45 C 0.0241(3) -0.0338(3) 0.3864(2) 0.0331(7) Uani 1 d . . H45A H 0.0303(3) -0.1111(3) 0.4004(2) 0.040 Uiso 1 calc R . N51 N -0.0558(2) 0.3211(2) 0.3728(2) 0.0209(5) Uani 1 d . . C52 C -0.1233(3) 0.4147(2) 0.3896(2) 0.0241(6) Uani 1 d . . C53 C -0.2699(3) 0.4283(3) 0.4256(3) 0.0360(8) Uani 1 d . . H53A H -0.3157(3) 0.4960(3) 0.4348(3) 0.043 Uiso 1 calc R . C54 C -0.3476(3) 0.3406(3) 0.4477(3) 0.0402(9) Uani 1 d . . H54A H -0.4478(3) 0.3477(3) 0.4725(3) 0.048 Uiso 1 calc R . C55 C -0.2795(3) 0.2440(3) 0.4336(2) 0.0321(7) Uani 1 d . . H55A H -0.3315(3) 0.1827(3) 0.4504(2) 0.039 Uiso 1 calc R . C56 C -0.1329(3) 0.2364(2) 0.3944(2) 0.0229(6) Uani 1 d . . N61 N 0.1091(2) 0.4692(2) 0.3567(2) 0.0240(5) Uani 1 d . . C62 C -0.0311(3) 0.5008(2) 0.3741(2) 0.0247(6) Uani 1 d . . C63 C -0.0850(3) 0.6040(3) 0.3793(2) 0.0346(8) Uani 1 d . . H63A H -0.1836(3) 0.6242(3) 0.3895(2) 0.042 Uiso 1 calc R . C64 C 0.0050(4) 0.6786(3) 0.3695(3) 0.0418(9) Uani 1 d . . H64A H -0.0305(4) 0.7508(3) 0.3715(3) 0.050 Uiso 1 calc R . C65 C 0.1467(3) 0.6462(3) 0.3569(2) 0.0360(8) Uani 1 d . . H65A H 0.2104(3) 0.6945(3) 0.3528(2) 0.043 Uiso 1 calc R . C66 C 0.1945(3) 0.5413(3) 0.3504(2) 0.0288(7) Uani 1 d . . H66A H 0.2926(3) 0.5195(3) 0.3410(2) 0.035 Uiso 1 calc R . N1 N 0.1417(3) 0.3224(2) 0.0948(2) 0.0279(6) Uani 1 d . . O1 O 0.0504(2) 0.3465(2) 0.1690(2) 0.0269(5) Uani 1 d . . O2 O 0.1124(2) 0.3343(2) 0.0170(2) 0.0490(7) Uani 1 d . . O3 O 0.2637(2) 0.2868(2) 0.1056(2) 0.0290(5) Uani 1 d . . N4 N 0.2899(2) 0.2442(2) 0.4696(2) 0.0237(5) Uani 1 d . . O4 O 0.1886(2) 0.2066(2) 0.4590(2) 0.0276(5) Uani 1 d . . O5 O 0.3203(2) 0.2129(2) 0.5496(2) 0.0370(5) Uani 1 d . . O6 O 0.3562(2) 0.3151(2) 0.3938(2) 0.0288(5) Uani 1 d . . C5 C 0.2610(5) 0.2427(5) -0.1887(4) 0.093(2) Uani 1 d . . H5A H 0.2462(19) 0.3222(6) -0.2178(29) 0.140 Uiso 1 calc R . H5B H 0.1869(6) 0.2183(31) -0.1255(6) 0.140 Uiso 1 calc R . H5C H 0.2571(16) 0.2061(27) -0.2359(25) 0.140 Uiso 1 calc R . C6 C 0.4145(5) 0.1242(4) -0.0850(4) 0.0796(15) Uani 1 d . . H6A H 0.4011(36) 0.0568(5) -0.0954(12) 0.119 Uiso 1 calc R . H6B H 0.3442(25) 0.1335(14) -0.0237(5) 0.119 Uiso 1 calc R . H6C H 0.5098(14) 0.1197(17) -0.0781(16) 0.119 Uiso 1 calc R . N7 N 0.3974(3) 0.2159(3) -0.1693(3) 0.0561(9) Uani 1 d . . C8 C 0.5046(5) 0.2726(4) -0.2316(4) 0.0611(12) Uani 1 d . . H8A H 0.5934(5) 0.2520(4) -0.2172(4) 0.073 Uiso 1 calc R . O9 O 0.4991(4) 0.3501(3) -0.3069(3) 0.0837(10) Uani 1 d . . C1 C 0.0020(6) 1.0600(6) 0.1258(5) 0.102(2) Uani 1 d . . O O 0.0481(17) 0.9589(10) 0.0152(8) 0.138(5) Uani 0.50 d P . C2 C 0.0152(20) 1.0194(14) 0.0445(16) 0.121(7) Uani 0.50 d P . C2' C 0.0445(14) 0.9639(10) 0.1171(12) 0.102(5) Uani 0.50 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01443(7) 0.01852(8) 0.02196(8) -0.00427(5) -0.00515(5) -0.00270(5) B1 0.038(2) 0.026(2) 0.047(2) -0.016(2) -0.014(2) 0.003(2) N11 0.0186(11) 0.0248(13) 0.0234(13) -0.0046(11) -0.0059(10) -0.0033(9) C12 0.0178(13) 0.026(2) 0.0178(14) -0.0068(12) -0.0024(11) -0.0039(11) C13 0.0241(15) 0.029(2) 0.028(2) -0.0046(14) -0.0053(12) -0.0092(12) C14 0.036(2) 0.023(2) 0.033(2) -0.0011(14) -0.0101(14) -0.0066(13) C15 0.028(2) 0.028(2) 0.036(2) -0.0046(15) -0.0145(14) 0.0015(13) C16 0.0193(14) 0.028(2) 0.029(2) -0.0055(13) -0.0078(12) -0.0014(12) N21 0.0170(11) 0.0256(14) 0.0221(13) -0.0057(11) -0.0049(9) -0.0015(9) C22 0.0171(13) 0.029(2) 0.0193(14) -0.0071(13) -0.0013(11) -0.0055(11) C23 0.0202(14) 0.035(2) 0.031(2) -0.0074(14) -0.0041(12) -0.0066(12) C24 0.0168(14) 0.047(2) 0.035(2) -0.012(2) -0.0056(13) -0.0077(13) C25 0.0157(14) 0.041(2) 0.031(2) -0.0105(15) -0.0074(12) 0.0022(12) C26 0.0188(14) 0.033(2) 0.0217(15) -0.0075(13) -0.0071(11) -0.0002(12) N31 0.0282(13) 0.0222(14) 0.037(2) -0.0089(12) -0.0117(11) 0.0039(10) N32 0.0228(12) 0.0232(14) 0.0314(14) -0.0079(11) -0.0081(10) 0.0011(10) C33 0.0192(14) 0.031(2) 0.027(2) -0.0091(14) -0.0064(12) 0.0030(12) C34 0.025(2) 0.040(2) 0.046(2) -0.014(2) -0.0164(15) 0.0084(14) C35 0.037(2) 0.026(2) 0.046(2) -0.008(2) -0.020(2) 0.0094(14) N41 0.0330(14) 0.0190(13) 0.0334(15) -0.0069(11) -0.0132(11) -0.0039(10) N42 0.0244(12) 0.0186(13) 0.0283(13) -0.0066(11) -0.0084(10) -0.0039(9) C43 0.0250(15) 0.026(2) 0.025(2) -0.0061(13) -0.0087(12) -0.0081(12) C44 0.031(2) 0.030(2) 0.034(2) -0.0050(14) -0.0108(13) -0.0146(13) C45 0.044(2) 0.023(2) 0.039(2) -0.0065(15) -0.018(2) -0.0136(14) N51 0.0191(11) 0.0238(13) 0.0207(12) -0.0065(10) -0.0057(9) -0.0043(9) C52 0.0196(14) 0.028(2) 0.023(2) -0.0081(13) -0.0035(11) -0.0031(12) C53 0.021(2) 0.043(2) 0.046(2) -0.022(2) -0.0044(14) -0.0015(14) C54 0.018(2) 0.058(2) 0.051(2) -0.030(2) -0.0017(14) -0.0073(15) C55 0.024(2) 0.041(2) 0.034(2) -0.014(2) -0.0034(13) -0.0128(14) C56 0.0225(14) 0.028(2) 0.0191(14) -0.0054(12) -0.0055(11) -0.0080(12) N61 0.0219(12) 0.0242(13) 0.0251(13) -0.0052(11) -0.0056(10) -0.0059(10) C62 0.0255(15) 0.025(2) 0.0217(15) -0.0079(13) -0.0023(12) -0.0031(12) C63 0.030(2) 0.031(2) 0.039(2) -0.015(2) 0.0004(14) -0.0018(13) C64 0.046(2) 0.029(2) 0.047(2) -0.021(2) 0.001(2) -0.004(2) C65 0.042(2) 0.033(2) 0.035(2) -0.016(2) 0.0006(15) -0.0175(15) C66 0.029(2) 0.031(2) 0.027(2) -0.0079(14) -0.0037(13) -0.0114(13) N1 0.0265(13) 0.034(2) 0.0255(14) -0.0045(12) -0.0093(11) -0.0124(11) O1 0.0173(10) 0.0337(12) 0.0282(12) -0.0069(10) -0.0056(8) -0.0042(8) O2 0.0443(14) 0.080(2) 0.0301(13) -0.0133(13) -0.0161(11) -0.0202(13) O3 0.0208(10) 0.0363(13) 0.0290(12) -0.0107(10) -0.0057(9) -0.0008(9) N4 0.0206(12) 0.0239(14) 0.0266(14) -0.0085(11) -0.0076(10) 0.0016(10) O4 0.0277(11) 0.0269(12) 0.0292(12) -0.0053(9) -0.0088(9) -0.0089(9) O5 0.0397(13) 0.0454(15) 0.0280(12) -0.0078(11) -0.0190(10) 0.0028(10) O6 0.0230(10) 0.0329(12) 0.0279(12) -0.0028(10) -0.0067(9) -0.0089(9) C5 0.046(3) 0.165(6) 0.073(4) -0.044(4) -0.014(2) -0.004(3) C6 0.068(3) 0.090(4) 0.069(3) -0.023(3) -0.007(3) -0.002(3) N7 0.038(2) 0.076(3) 0.050(2) -0.025(2) -0.002(2) -0.002(2) C8 0.053(3) 0.077(3) 0.056(3) -0.036(3) -0.005(2) -0.001(2) O9 0.093(3) 0.077(2) 0.065(2) -0.019(2) -0.003(2) -0.009(2) C1 0.093(4) 0.139(6) 0.079(4) -0.041(4) -0.031(3) 0.006(4) O 0.269(16) 0.065(7) 0.107(7) -0.044(6) -0.102(8) 0.048(7) C2 0.159(14) 0.047(8) 0.219(22) -0.045(14) -0.134(16) 0.000(9) C2' 0.124(10) 0.055(7) 0.165(14) -0.039(9) -0.096(11) 0.012(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 N32 2.487(2) . ? Gd1 O4 2.488(2) . ? Gd1 O1 2.498(2) . ? Gd1 N42 2.506(2) . ? Gd1 O3 2.519(2) . ? Gd1 N21 2.579(2) . ? Gd1 N51 2.593(2) . ? Gd1 O6 2.602(2) . ? Gd1 N61 2.641(2) . ? Gd1 N11 2.671(2) . ? Gd1 N1 2.932(3) . ? Gd1 N4 2.973(2) . ? B1 N31 1.554(4) . ? B1 N41 1.558(4) . ? N11 C16 1.342(3) . ? N11 C12 1.353(3) . ? C12 C13 1.390(4) . ? C12 C22 1.491(4) . ? C13 C14 1.379(4) . ? C14 C15 1.378(4) . ? C15 C16 1.372(4) . ? N21 C22 1.340(4) . ? N21 C26 1.357(3) . ? C22 C23 1.397(4) . ? C23 C24 1.383(4) . ? C24 C25 1.375(4) . ? C25 C26 1.399(4) . ? C26 C33 1.458(4) . ? N31 C35 1.349(4) . ? N31 N32 1.357(3) . ? N32 C33 1.344(3) . ? C33 C34 1.397(4) . ? C34 C35 1.376(5) . ? N41 C45 1.350(4) . ? N41 N42 1.364(3) . ? N42 C43 1.352(3) . ? C43 C44 1.392(4) . ? C43 C56 1.453(4) . ? C44 C45 1.371(4) . ? N51 C52 1.342(4) . ? N51 C56 1.352(3) . ? C52 C53 1.391(4) . ? C52 C62 1.492(4) . ? C53 C54 1.387(5) . ? C54 C55 1.365(5) . ? C55 C56 1.393(4) . ? N61 C66 1.342(4) . ? N61 C62 1.355(3) . ? C62 C63 1.373(4) . ? C63 C64 1.383(5) . ? C64 C65 1.375(5) . ? C65 C66 1.387(4) . ? N1 O2 1.225(3) . ? N1 O3 1.266(3) . ? N1 O1 1.271(3) . ? N4 O5 1.228(3) . ? N4 O6 1.260(3) . ? N4 O4 1.274(3) . ? C5 N7 1.441(5) . ? C6 N7 1.433(6) . ? N7 C8 1.318(5) . ? C8 O9 1.229(5) . ? C1 C2' 1.282(13) . ? C1 C2 1.42(2) . ? O C2 0.980(15) . ? O C2 1.174(14) 2_575 ? O O 1.36(2) 2_575 ? O C2' 1.51(2) . ? C2 O 1.174(14) 2_575 ? C2 C2' 1.16(2) . ? C2 C2 1.68(3) 2_575 ? 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 N32 Gd1 O4 79.10(7) . . ? N32 Gd1 O1 117.59(7) . . ? O4 Gd1 O1 133.94(6) . . ? N32 Gd1 N42 74.76(8) . . ? O4 Gd1 N42 70.16(7) . . ? O1 Gd1 N42 73.73(7) . . ? N32 Gd1 O3 72.78(7) . . ? O4 Gd1 O3 145.09(7) . . ? O1 Gd1 O3 50.90(6) . . ? N42 Gd1 O3 82.65(7) . . ? N32 Gd1 N21 63.58(8) . . ? O4 Gd1 N21 109.52(7) . . ? O1 Gd1 N21 116.35(7) . . ? N42 Gd1 N21 137.09(8) . . ? O3 Gd1 N21 75.93(7) . . ? N32 Gd1 N51 136.37(8) . . ? O4 Gd1 N51 73.25(7) . . ? O1 Gd1 N51 65.82(7) . . ? N42 Gd1 N51 64.46(7) . . ? O3 Gd1 N51 114.65(7) . . ? N21 Gd1 N51 158.39(8) . . ? N32 Gd1 O6 76.04(7) . . ? O4 Gd1 O6 50.02(6) . . ? O1 Gd1 O6 165.47(7) . . ? N42 Gd1 O6 116.88(7) . . ? O3 Gd1 O6 136.80(6) . . ? N21 Gd1 O6 63.62(7) . . ? N51 Gd1 O6 108.54(7) . . ? N32 Gd1 N61 144.74(8) . . ? O4 Gd1 N61 80.03(7) . . ? O1 Gd1 N61 97.31(7) . . ? N42 Gd1 N61 123.30(7) . . ? O3 Gd1 N61 134.44(7) . . ? N21 Gd1 N61 97.72(7) . . ? N51 Gd1 N61 61.17(7) . . ? O6 Gd1 N61 68.76(7) . . ? N32 Gd1 N11 119.99(7) . . ? O4 Gd1 N11 141.00(7) . . ? O1 Gd1 N11 70.58(7) . . ? N42 Gd1 N11 144.19(7) . . ? O3 Gd1 N11 72.78(7) . . ? N21 Gd1 N11 61.28(7) . . ? N51 Gd1 N11 102.51(7) . . ? O6 Gd1 N11 98.77(7) . . ? N61 Gd1 N11 65.19(7) . . ? N32 Gd1 N1 95.59(8) . . ? O4 Gd1 N1 147.61(7) . . ? O1 Gd1 N1 25.49(6) . . ? N42 Gd1 N1 77.60(7) . . ? O3 Gd1 N1 25.43(6) . . ? N21 Gd1 N1 95.97(7) . . ? N51 Gd1 N1 90.45(7) . . ? O6 Gd1 N1 159.59(6) . . ? N61 Gd1 N1 116.85(7) . . ? N11 Gd1 N1 68.97(7) . . ? N32 Gd1 N4 75.67(7) . . ? O4 Gd1 N4 25.02(6) . . ? O1 Gd1 N4 156.83(6) . . ? N42 Gd1 N4 93.36(7) . . ? O3 Gd1 N4 148.13(6) . . ? N21 Gd1 N4 86.28(7) . . ? N51 Gd1 N4 91.37(7) . . ? O6 Gd1 N4 25.01(6) . . ? N61 Gd1 N4 73.40(7) . . ? N11 Gd1 N4 121.16(7) . . ? N1 Gd1 N4 168.93(7) . . ? N31 B1 N41 110.6(3) . . ? C16 N11 C12 117.4(2) . . ? C16 N11 Gd1 121.8(2) . . ? C12 N11 Gd1 120.3(2) . . ? N11 C12 C13 121.8(2) . . ? N11 C12 C22 116.2(2) . . ? C13 C12 C22 122.1(2) . . ? C14 C13 C12 119.5(3) . . ? C13 C14 C15 118.9(3) . . ? C16 C15 C14 118.6(3) . . ? N11 C16 C15 123.8(3) . . ? C22 N21 C26 118.7(2) . . ? C22 N21 Gd1 123.6(2) . . ? C26 N21 Gd1 116.2(2) . . ? N21 C22 C23 122.4(3) . . ? N21 C22 C12 115.9(2) . . ? C23 C22 C12 121.7(3) . . ? C24 C23 C22 118.6(3) . . ? C25 C24 C23 119.7(3) . . ? C24 C25 C26 119.0(3) . . ? N21 C26 C25 121.6(3) . . ? N21 C26 C33 115.3(2) . . ? C25 C26 C33 123.0(3) . . ? C35 N31 N32 109.4(2) . . ? C35 N31 B1 126.3(3) . . ? N32 N31 B1 120.8(2) . . ? C33 N32 N31 106.7(2) . . ? C33 N32 Gd1 117.5(2) . . ? N31 N32 Gd1 130.6(2) . . ? N32 C33 C34 110.3(3) . . ? N32 C33 C26 117.9(2) . . ? C34 C33 C26 131.7(3) . . ? C35 C34 C33 104.5(3) . . ? N31 C35 C34 109.1(3) . . ? C45 N41 N42 109.9(2) . . ? C45 N41 B1 125.5(3) . . ? N42 N41 B1 124.3(2) . . ? C43 N42 N41 105.4(2) . . ? C43 N42 Gd1 120.3(2) . . ? N41 N42 Gd1 133.1(2) . . ? N42 C43 C44 111.1(3) . . ? N42 C43 C56 119.5(3) . . ? C44 C43 C56 129.2(3) . . ? C45 C44 C43 104.4(3) . . ? N41 C45 C44 109.1(3) . . ? C52 N51 C56 118.6(2) . . ? C52 N51 Gd1 122.0(2) . . ? C56 N51 Gd1 118.8(2) . . ? N51 C52 C53 122.2(3) . . ? N51 C52 C62 115.9(2) . . ? C53 C52 C62 121.8(3) . . ? C54 C53 C52 118.5(3) . . ? C55 C54 C53 119.7(3) . . ? C54 C55 C56 119.1(3) . . ? N51 C56 C55 121.8(3) . . ? N51 C56 C43 116.1(2) . . ? C55 C56 C43 122.1(3) . . ? C66 N61 C62 117.2(3) . . ? C66 N61 Gd1 120.7(2) . . ? C62 N61 Gd1 118.8(2) . . ? N61 C62 C63 122.3(3) . . ? N61 C62 C52 115.4(3) . . ? C63 C62 C52 122.3(3) . . ? C62 C63 C64 119.7(3) . . ? C65 C64 C63 118.8(3) . . ? C64 C65 C66 118.6(3) . . ? N61 C66 C65 123.3(3) . . ? O2 N1 O3 122.2(3) . . ? O2 N1 O1 121.3(2) . . ? O3 N1 O1 116.5(2) . . ? O2 N1 Gd1 177.0(2) . . ? O3 N1 Gd1 58.71(13) . . ? O1 N1 Gd1 57.80(13) . . ? N1 O1 Gd1 96.72(15) . . ? N1 O3 Gd1 95.9(2) . . ? O5 N4 O6 122.2(2) . . ? O5 N4 O4 121.4(2) . . ? O6 N4 O4 116.4(2) . . ? O5 N4 Gd1 176.5(2) . . ? O6 N4 Gd1 60.77(13) . . ? O4 N4 Gd1 55.67(13) . . ? N4 O4 Gd1 99.30(15) . . ? N4 O6 Gd1 94.21(15) . . ? C8 N7 C6 121.6(4) . . ? C8 N7 C5 119.5(4) . . ? C6 N7 C5 118.8(4) . . ? O9 C8 N7 125.4(5) . . ? C2' C1 C2 50.5(10) . . ? C2 O C2 102.3(17) . 2_575 ? C2 O O 57.5(11) . 2_575 ? C2 O O 44.7(9) 2_575 2_575 ? C2 O C2' 50.3(15) . . ? C2 O C2' 145.2(16) 2_575 . ? O O C2' 104.4(13) 2_575 . ? O C2 O 77.7(17) . 2_575 ? O C2 C2' 89.4(19) . . ? O C2 C2' 152.7(18) 2_575 . ? O C2 C1 147.5(22) . . ? O C2 C1 132.8(19) 2_575 . ? C2' C2 C1 58.4(11) . . ? O C2 C2 43.0(11) . 2_575 ? O C2 C2 34.7(8) 2_575 2_575 ? C2' C2 C2 127.9(20) . 2_575 ? C1 C2 C2 164.9(21) . 2_575 ? C2 C2' C1 71.1(12) . . ? C2 C2' O 40.4(10) . . ? C1 C2' O 111.4(12) . . ? _refine_diff_density_max 0.808 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.104 #=END data_/tintin3/people/sam/oil/oil _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H20 B N8 Tl' _chemical_formula_weight 659.68 _chemical_melting_point ? _chemical_compound_source ? 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tl' 'Tl' -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.608(4) _cell_length_b 17.775(4) _cell_length_c 15.910(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.533(5) _cell_angle_gamma 90.00 _cell_volume 4696.4(20) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method ? _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 6.912 _exptl_absorpt_correction_type 'empirical - SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18437 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5356 _reflns_number_observed 4052 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5356 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_obs 0.0253 _refine_ls_wR_factor_all 0.0521 _refine_ls_wR_factor_obs 0.0480 _refine_ls_goodness_of_fit_all 0.958 _refine_ls_goodness_of_fit_obs 1.024 _refine_ls_restrained_S_all 0.958 _refine_ls_restrained_S_obs 1.024 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Tl1 Tl 0.112071(8) 0.197160(7) 0.290958(9) 0.03241(5) Uani 1 d . . N11 N -0.0539(2) 0.3776(2) 0.5068(2) 0.0391(8) Uani 1 d . . C12 C 0.0000(2) 0.3773(2) 0.4438(2) 0.0294(8) Uani 1 d . . C13 C -0.0229(2) 0.3711(2) 0.3614(2) 0.0320(8) Uani 1 d . . H13A H 0.0169(2) 0.3711(2) 0.3188(2) 0.038 Uiso 1 calc R . C14 C -0.1029(2) 0.3646(2) 0.3396(2) 0.0406(10) Uani 1 d . . H14A H -0.1193(2) 0.3612(2) 0.2823(2) 0.049 Uiso 1 calc R . C15 C -0.1585(2) 0.3634(2) 0.4034(3) 0.0413(10) Uani 1 d . . H15A H -0.2143(2) 0.3582(2) 0.3912(3) 0.050 Uiso 1 calc R . C16 C -0.1318(3) 0.3699(2) 0.4844(3) 0.0455(10) Uani 1 d . . H16A H -0.1707(3) 0.3688(2) 0.5278(3) 0.055 Uiso 1 calc R . N21 N 0.1397(2) 0.34502(14) 0.4226(2) 0.0251(6) Uani 1 d . . C22 C 0.0858(2) 0.3830(2) 0.4698(2) 0.0278(8) Uani 1 d . . C23 C 0.1077(2) 0.4247(2) 0.5408(2) 0.0349(9) Uani 1 d . . H23A H 0.0682(2) 0.4505(2) 0.5725(2) 0.042 Uiso 1 calc R . C24 C 0.1872(3) 0.4275(2) 0.5636(2) 0.0408(10) Uani 1 d . . H24A H 0.2037(3) 0.4566(2) 0.6108(2) 0.049 Uiso 1 calc R . C25 C 0.2434(2) 0.3880(2) 0.5181(2) 0.0358(9) Uani 1 d . . H25A H 0.2986(2) 0.3887(2) 0.5342(2) 0.043 Uiso 1 calc R . C26 C 0.2178(2) 0.3467(2) 0.4475(2) 0.0273(8) Uani 1 d . . N31 N 0.3247(2) 0.24262(15) 0.2922(2) 0.0299(7) Uani 1 d . . N32 N 0.2561(2) 0.27539(15) 0.3217(2) 0.0281(7) Uani 1 d . . C33 C 0.2762(2) 0.3049(2) 0.3971(2) 0.0272(7) Uani 1 d . . C34 C 0.3574(2) 0.2905(2) 0.4166(2) 0.0338(9) Uani 1 d . . H34A H 0.3864(2) 0.3047(2) 0.4658(2) 0.041 Uiso 1 calc R . C35 C 0.3854(2) 0.2512(2) 0.3487(2) 0.0348(9) Uani 1 d . . H35A H 0.4388(2) 0.2330(2) 0.3423(2) 0.042 Uiso 1 calc R . B B 0.3267(3) 0.2042(2) 0.2057(3) 0.0353(10) Uani 1 d . . H0A H 0.3822(3) 0.2055(2) 0.1835(3) 0.042 Uiso 1 calc R . H0B H 0.2911(3) 0.2316(2) 0.1659(3) 0.042 Uiso 1 calc R . N41 N -0.0025(2) 0.1309(2) 0.4169(2) 0.0343(7) Uani 1 d . . C42 C -0.0271(2) 0.0598(2) 0.4022(2) 0.0254(8) Uani 1 d . . C43 C -0.1042(2) 0.0353(2) 0.4233(2) 0.0346(9) Uani 1 d . . H43A H -0.1199(2) -0.0153(2) 0.4132(2) 0.041 Uiso 1 calc R . C44 C -0.1572(2) 0.0850(2) 0.4589(3) 0.0449(10) Uani 1 d . . H44A H -0.2098(2) 0.0691(2) 0.4737(3) 0.054 Uiso 1 calc R . C45 C -0.1334(2) 0.1580(2) 0.4727(3) 0.0419(10) Uani 1 d . . H45A H -0.1692(2) 0.1938(2) 0.4961(3) 0.050 Uiso 1 calc R . C46 C -0.0558(3) 0.1776(2) 0.4514(3) 0.0433(10) Uani 1 d . . H46A H -0.0391(3) 0.2279(2) 0.4620(3) 0.052 Uiso 1 calc R . N51 N 0.0953(2) 0.03950(15) 0.3241(2) 0.0241(6) Uani 1 d . . C52 C 0.0322(2) 0.0079(2) 0.3622(2) 0.0243(7) Uani 1 d . . C53 C 0.0206(2) -0.0695(2) 0.3648(2) 0.0307(8) Uani 1 d . . H53A H -0.0247(2) -0.0902(2) 0.3925(2) 0.037 Uiso 1 calc R . C54 C 0.0758(2) -0.1155(2) 0.3268(2) 0.0381(9) Uani 1 d . . H54A H 0.0690(2) -0.1686(2) 0.3279(2) 0.046 Uiso 1 calc R . C55 C 0.1413(2) -0.0840(2) 0.2867(2) 0.0296(8) Uani 1 d . . H55A H 0.1800(2) -0.1147(2) 0.2596(2) 0.036 Uiso 1 calc R . C56 C 0.1489(2) -0.0060(2) 0.2872(2) 0.0226(7) Uani 1 d . . N61 N 0.2981(2) 0.1213(2) 0.2138(2) 0.0296(7) Uani 1 d . . N62 N 0.2266(2) 0.10550(14) 0.2498(2) 0.0259(6) Uani 1 d . . C63 C 0.2188(2) 0.0299(2) 0.2481(2) 0.0243(7) Uani 1 d . . C64 C 0.2857(2) -0.0027(2) 0.2084(2) 0.0301(8) Uani 1 d . . H64A H 0.2951(2) -0.0544(2) 0.1975(2) 0.036 Uiso 1 calc R . C66 C 0.3344(2) 0.0570(2) 0.1893(2) 0.0324(8) Uani 1 d . . H66A H 0.3854(2) 0.0538(2) 0.1630(2) 0.039 Uiso 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 Tl1 0.02736(8) 0.02742(7) 0.04244(9) 0.00558(7) -0.00055(6) 0.00333(7) N11 0.038(2) 0.042(2) 0.037(2) -0.0044(15) 0.006(2) 0.000(2) C12 0.036(2) 0.020(2) 0.032(2) -0.0022(14) 0.001(2) 0.003(2) C13 0.030(2) 0.034(2) 0.032(2) 0.001(2) 0.001(2) 0.003(2) C14 0.044(3) 0.042(2) 0.036(2) -0.007(2) -0.009(2) 0.011(2) C15 0.034(2) 0.038(2) 0.052(3) -0.008(2) -0.004(2) 0.007(2) C16 0.040(3) 0.048(2) 0.049(3) -0.007(2) 0.006(2) 0.005(2) N21 0.030(2) 0.0205(14) 0.024(2) 0.0033(11) 0.0007(13) -0.0021(13) C22 0.035(2) 0.021(2) 0.027(2) 0.0049(14) 0.001(2) -0.002(2) C23 0.045(2) 0.031(2) 0.029(2) -0.006(2) -0.002(2) 0.005(2) C24 0.054(3) 0.034(2) 0.034(2) -0.006(2) -0.011(2) -0.002(2) C25 0.040(2) 0.033(2) 0.034(2) 0.002(2) -0.011(2) -0.006(2) C26 0.033(2) 0.022(2) 0.027(2) 0.0067(14) -0.001(2) -0.005(2) N31 0.025(2) 0.0218(15) 0.043(2) 0.0035(13) 0.0057(14) -0.0019(13) N32 0.029(2) 0.0233(14) 0.032(2) 0.0010(12) 0.0021(13) -0.0028(13) C33 0.027(2) 0.022(2) 0.033(2) 0.009(2) -0.0017(15) -0.006(2) C34 0.030(2) 0.032(2) 0.039(2) 0.006(2) -0.006(2) -0.008(2) C35 0.023(2) 0.028(2) 0.053(3) 0.008(2) 0.003(2) -0.007(2) B 0.032(2) 0.029(2) 0.045(3) 0.005(2) 0.011(2) -0.002(2) N41 0.035(2) 0.027(2) 0.041(2) 0.0071(13) 0.0095(15) 0.0072(14) C42 0.027(2) 0.026(2) 0.023(2) 0.0047(14) -0.0033(15) -0.001(2) C43 0.029(2) 0.039(2) 0.036(2) -0.002(2) 0.001(2) -0.003(2) C44 0.027(2) 0.057(3) 0.051(3) 0.000(2) 0.002(2) 0.001(2) C45 0.034(2) 0.042(2) 0.049(3) 0.006(2) 0.009(2) 0.013(2) C46 0.050(3) 0.028(2) 0.053(3) 0.005(2) 0.012(2) 0.007(2) N51 0.025(2) 0.0241(14) 0.0236(14) 0.0008(12) -0.0009(12) -0.0014(13) C52 0.026(2) 0.024(2) 0.023(2) 0.0005(14) -0.0040(15) -0.003(2) C53 0.032(2) 0.026(2) 0.035(2) 0.001(2) 0.004(2) -0.010(2) C54 0.052(3) 0.020(2) 0.043(2) -0.001(2) 0.003(2) -0.007(2) C55 0.031(2) 0.026(2) 0.032(2) -0.0067(15) 0.001(2) -0.001(2) C56 0.025(2) 0.021(2) 0.021(2) 0.0003(13) -0.0059(14) 0.0000(15) N61 0.024(2) 0.0257(15) 0.039(2) 0.0023(13) 0.0049(14) 0.0008(13) N62 0.022(2) 0.0217(14) 0.034(2) 0.0006(12) 0.0051(13) -0.0016(12) C63 0.026(2) 0.024(2) 0.022(2) -0.0031(14) -0.0031(14) 0.000(2) C64 0.036(2) 0.022(2) 0.033(2) -0.0032(15) 0.001(2) 0.004(2) C66 0.028(2) 0.033(2) 0.037(2) -0.004(2) 0.005(2) 0.005(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 Tl1 N62 2.593(3) . ? Tl1 N32 2.806(3) . ? N11 C16 1.345(5) . ? N11 C12 1.349(4) . ? C12 C13 1.365(5) . ? C12 C22 1.484(5) . ? C13 C14 1.375(5) . ? C14 C15 1.380(5) . ? C15 C16 1.363(5) . ? N21 C26 1.352(4) . ? N21 C22 1.355(4) . ? C22 C23 1.396(5) . ? C23 C24 1.367(5) . ? C24 C25 1.379(5) . ? C25 C26 1.404(5) . ? C26 C33 1.466(5) . ? N31 C35 1.353(4) . ? N31 N32 1.366(4) . ? N31 B 1.537(5) . ? N32 C33 1.348(4) . ? C33 C34 1.405(5) . ? C34 C35 1.371(5) . ? B N61 1.554(5) . ? N41 C46 1.335(5) . ? N41 C42 1.347(4) . ? C42 C43 1.398(5) . ? C42 C52 1.496(5) . ? C43 C44 1.373(5) . ? C44 C45 1.373(5) . ? C45 C46 1.380(5) . ? N51 C52 1.340(4) . ? N51 C56 1.343(4) . ? C52 C53 1.389(4) . ? C53 C54 1.372(5) . ? C54 C55 1.385(5) . ? C55 C56 1.391(4) . ? C56 C63 1.468(5) . ? N61 C66 1.350(4) . ? N61 N62 1.353(4) . ? N62 C63 1.351(4) . ? C63 C64 1.407(5) . ? C64 C66 1.370(5) . ? 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 N62 Tl1 N32 74.30(8) . . ? C16 N11 C12 116.4(3) . . ? N11 C12 C13 122.2(3) . . ? N11 C12 C22 115.7(3) . . ? C13 C12 C22 122.1(3) . . ? C12 C13 C14 120.6(4) . . ? C13 C14 C15 117.9(4) . . ? C16 C15 C14 118.7(4) . . ? N11 C16 C15 124.2(4) . . ? C26 N21 C22 117.6(3) . . ? N21 C22 C23 122.9(3) . . ? N21 C22 C12 116.8(3) . . ? C23 C22 C12 120.3(3) . . ? C24 C23 C22 118.6(4) . . ? C23 C24 C25 119.9(3) . . ? C24 C25 C26 119.0(4) . . ? N21 C26 C25 121.9(3) . . ? N21 C26 C33 117.7(3) . . ? C25 C26 C33 120.4(3) . . ? C35 N31 N32 110.0(3) . . ? C35 N31 B 128.5(3) . . ? N32 N31 B 121.5(3) . . ? C33 N32 N31 105.7(3) . . ? C33 N32 Tl1 123.4(2) . . ? N31 N32 Tl1 116.2(2) . . ? N32 C33 C34 110.8(3) . . ? N32 C33 C26 121.7(3) . . ? C34 C33 C26 127.6(3) . . ? C35 C34 C33 104.5(3) . . ? N31 C35 C34 108.9(3) . . ? N31 B N61 109.7(3) . . ? C46 N41 C42 117.0(3) . . ? N41 C42 C43 121.8(3) . . ? N41 C42 C52 117.0(3) . . ? C43 C42 C52 121.2(3) . . ? C44 C43 C42 119.4(4) . . ? C45 C44 C43 119.3(4) . . ? C44 C45 C46 117.9(4) . . ? N41 C46 C45 124.6(4) . . ? C52 N51 C56 118.0(3) . . ? N51 C52 C53 122.5(3) . . ? N51 C52 C42 117.0(3) . . ? C53 C52 C42 120.5(3) . . ? C54 C53 C52 118.9(3) . . ? C53 C54 C55 119.5(3) . . ? C54 C55 C56 118.2(3) . . ? N51 C56 C55 122.8(3) . . ? N51 C56 C63 117.0(3) . . ? C55 C56 C63 120.2(3) . . ? C66 N61 N62 110.0(3) . . ? C66 N61 B 129.9(3) . . ? N62 N61 B 120.1(3) . . ? C63 N62 N61 106.4(3) . . ? C63 N62 Tl1 124.0(2) . . ? N61 N62 Tl1 128.7(2) . . ? N62 C63 C64 110.0(3) . . ? N62 C63 C56 120.0(3) . . ? C64 C63 C56 130.0(3) . . ? C66 C64 C63 104.6(3) . . ? N61 C66 C64 109.0(3) . . ? _refine_diff_density_max 0.819 _refine_diff_density_min -1.138 _refine_diff_density_rms 0.096 #=END