# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1804 data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Mark Thornton-Pett' _publ_contact_author_address ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_contact_author_phone '+44 (0)113 2336423' _publ_contact_author_fax '+44 (0)113 2336565' _publ_contact_author_email marktp@chem.leeds.ac.uk _publ_requested_journal 'J Chem. Soc., Dalton Trans.' _publ_contact_letter ; The following 4 sets of data is included in the paper below (m/s which 9/09125D) we have just submitted to you. ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and reactivity of sterically hindered iminopyrrolato complexes of zirconium, iron, cobalt and nickel ; loop_ _publ_author_name _publ_author_address 'David M. Dawson' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Dennis A. Walker' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Mark Thornton-Pett' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Manfred Bochmann' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; #================================================================= data_MB41 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H76 Fe N6' _chemical_formula_weight 937.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.64980(10) _cell_length_b 21.2477(2) _cell_length_c 24.3318(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.2920(5) _cell_angle_gamma 90.00 _cell_volume 5461.36(10) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.318 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8320 _exptl_absorpt_correction_T_max 0.8779 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree phi range. ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20488 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10540 _reflns_number_gt 8977 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KCCD (Nonius, 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.0552P)^2^+1.9324P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10540 _refine_ls_number_parameters 641 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.011 _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 N1 N 0.71522(12) 0.26494(6) 0.21251(6) 0.0410(3) Uani 1 1 d . . . C11 C 0.63568(15) 0.21771(8) 0.18275(7) 0.0431(4) Uani 1 1 d . . . C12 C 0.62900(17) 0.15812(8) 0.20681(7) 0.0498(4) Uani 1 1 d . . . C121 C 0.7014(2) 0.14242(9) 0.26307(8) 0.0603(5) Uani 1 1 d . . . H121 H 0.7308 0.1829 0.2813 0.072 Uiso 1 1 calc R . . C122 C 0.8179(3) 0.10361(13) 0.25585(12) 0.1012(10) Uani 1 1 d . . . H12A H 0.7919 0.0637 0.2377 0.152 Uiso 1 1 calc R . . H12B H 0.8658 0.0952 0.2922 0.152 Uiso 1 1 calc R . . H12C H 0.8714 0.1269 0.2329 0.152 Uiso 1 1 calc R . . C123 C 0.6181(3) 0.10935(15) 0.30062(11) 0.1063(11) Uani 1 1 d . . . H12D H 0.5403 0.1337 0.3018 0.159 Uiso 1 1 calc R . . H12E H 0.6638 0.1059 0.3381 0.159 Uiso 1 1 calc R . . H12F H 0.5965 0.0672 0.2861 0.159 Uiso 1 1 calc R . . C13 C 0.55359(19) 0.11270(9) 0.17760(8) 0.0600(5) Uani 1 1 d . . . H13 H 0.5487 0.0718 0.1930 0.072 Uiso 1 1 calc R . . C14 C 0.4859(2) 0.12567(10) 0.12678(8) 0.0624(5) Uani 1 1 d . . . H14 H 0.4350 0.0940 0.1075 0.075 Uiso 1 1 calc R . . C15 C 0.49234(18) 0.18463(10) 0.10416(8) 0.0578(5) Uani 1 1 d . . . H15 H 0.4450 0.1933 0.0692 0.069 Uiso 1 1 calc R . . C16 C 0.56679(16) 0.23225(8) 0.13121(7) 0.0487(4) Uani 1 1 d . . . C161 C 0.56807(19) 0.29671(10) 0.10429(8) 0.0592(5) Uani 1 1 d . . . H161 H 0.6365 0.3221 0.1258 0.071 Uiso 1 1 calc R . . C162 C 0.5975(2) 0.29262(13) 0.04458(9) 0.0752(6) Uani 1 1 d . . . H16A H 0.6759 0.2688 0.0435 0.113 Uiso 1 1 calc R . . H16B H 0.6077 0.3351 0.0302 0.113 Uiso 1 1 calc R . . H16C H 0.5277 0.2713 0.0217 0.113 Uiso 1 1 calc R . . C163 C 0.4420(2) 0.33109(11) 0.10680(10) 0.0720(6) Uani 1 1 d . . . H16D H 0.3728 0.3065 0.0869 0.108 Uiso 1 1 calc R . . H16E H 0.4452 0.3726 0.0895 0.108 Uiso 1 1 calc R . . H16F H 0.4277 0.3361 0.1456 0.108 Uiso 1 1 calc R . . C1 C 0.65926(15) 0.31228(8) 0.23298(7) 0.0444(4) Uani 1 1 d . . . H1 H 0.5694 0.3142 0.2281 0.053 Uiso 1 1 calc R . . C2 C 0.72909(15) 0.36102(8) 0.26231(7) 0.0444(4) Uani 1 1 d . . . C21 C 0.69057(16) 0.41497(9) 0.28849(8) 0.0549(4) Uani 1 1 d . . . H21 H 0.6061 0.4288 0.2895 0.066 Uiso 1 1 calc R . . N2 N 0.85876(12) 0.35654(6) 0.26918(6) 0.0417(3) Uani 1 1 d . . . C3 C 0.90186(15) 0.40735(7) 0.30007(7) 0.0442(4) Uani 1 1 d . . . C31 C 0.79985(17) 0.44422(9) 0.31269(8) 0.0541(4) Uani 1 1 d . . . H31 H 0.8049 0.4820 0.3338 0.065 Uiso 1 1 calc R . . C4 C 1.03566(16) 0.41681(8) 0.31695(7) 0.0465(4) Uani 1 1 d . . . H4 H 1.0942 0.3861 0.3076 0.056 Uiso 1 1 calc R . . N4 N 1.07654(13) 0.46540(7) 0.34413(7) 0.0520(4) Uani 1 1 d . . . C41 C 1.20934(16) 0.47087(8) 0.36126(8) 0.0522(4) Uani 1 1 d . . . C42 C 1.29126(18) 0.49031(9) 0.32391(9) 0.0589(5) Uani 1 1 d . . . C421 C 1.2454(2) 0.50604(13) 0.26400(11) 0.0781(6) Uani 1 1 d . . . H421 H 1.1508 0.5039 0.2594 0.094 Uiso 1 1 calc R . . C422 C 1.2916(3) 0.4561(2) 0.22553(13) 0.1202(12) Uani 1 1 d . . . H42A H 1.2580 0.4656 0.1870 0.180 Uiso 1 1 calc R . . H42B H 1.2619 0.4145 0.2355 0.180 Uiso 1 1 calc R . . H42C H 1.3843 0.4563 0.2295 0.180 Uiso 1 1 calc R . . C423 C 1.2814(4) 0.57260(19) 0.24875(18) 0.1372(15) Uani 1 1 d . . . H42D H 1.2510 0.6026 0.2746 0.206 Uiso 1 1 calc R . . H42E H 1.2428 0.5822 0.2110 0.206 Uiso 1 1 calc R . . H42F H 1.3737 0.5758 0.2508 0.206 Uiso 1 1 calc R . . C43 C 1.42013(19) 0.49418(10) 0.34370(11) 0.0688(6) Uani 1 1 d . . . H43 H 1.4780 0.5072 0.3193 0.083 Uiso 1 1 calc R . . C44 C 1.4649(2) 0.47975(12) 0.39741(12) 0.0792(7) Uani 1 1 d . . . H44 H 1.5533 0.4807 0.4094 0.095 Uiso 1 1 calc R . . C45 C 1.3817(2) 0.46380(12) 0.43424(11) 0.0779(7) Uani 1 1 d . . . H45 H 1.4135 0.4551 0.4717 0.093 Uiso 1 1 calc R . . C46 C 1.25218(19) 0.46031(10) 0.41740(9) 0.0628(5) Uani 1 1 d . . . C461 C 1.1596(2) 0.44311(13) 0.45769(10) 0.0774(6) Uani 1 1 d . . . H461 H 1.0733 0.4555 0.4399 0.093 Uiso 1 1 calc R . . C462 C 1.1586(3) 0.37166(15) 0.46559(14) 0.1118(11) Uani 1 1 d . . . H46A H 1.1342 0.3512 0.4297 0.168 Uiso 1 1 calc R . . H46B H 1.0977 0.3606 0.4910 0.168 Uiso 1 1 calc R . . H46C H 1.2433 0.3574 0.4811 0.168 Uiso 1 1 calc R . . C463 C 1.1840(3) 0.47837(17) 0.51246(12) 0.1063(10) Uani 1 1 d . . . H46D H 1.2666 0.4661 0.5319 0.159 Uiso 1 1 calc R . . H46E H 1.1177 0.4679 0.5354 0.159 Uiso 1 1 calc R . . H46F H 1.1832 0.5238 0.5053 0.159 Uiso 1 1 calc R . . N5 N 1.02013(13) 0.29022(7) 0.16458(6) 0.0504(3) Uani 1 1 d . . . C51 C 0.98546(16) 0.29984(9) 0.10610(8) 0.0504(4) Uani 1 1 d . . . C52 C 0.95946(16) 0.36097(9) 0.08558(8) 0.0505(4) Uani 1 1 d . . . C521 C 0.96655(18) 0.41757(9) 0.12370(9) 0.0585(5) Uani 1 1 d . . . H521 H 1.0164 0.4051 0.1596 0.070 Uiso 1 1 calc R . . C522 C 1.0331(3) 0.47391(13) 0.10102(13) 0.0987(9) Uani 1 1 d . . . H52A H 1.1166 0.4609 0.0923 0.148 Uiso 1 1 calc R . . H52B H 1.0431 0.5074 0.1289 0.148 Uiso 1 1 calc R . . H52C H 0.9823 0.4895 0.0674 0.148 Uiso 1 1 calc R . . C523 C 0.8350(2) 0.43629(12) 0.13554(12) 0.0786(7) Uani 1 1 d . . . H52D H 0.7842 0.4493 0.1010 0.118 Uiso 1 1 calc R . . H52E H 0.8415 0.4713 0.1619 0.118 Uiso 1 1 calc R . . H52F H 0.7945 0.4003 0.1514 0.118 Uiso 1 1 calc R . . C53 C 0.92371(17) 0.36748(10) 0.02895(8) 0.0590(5) Uani 1 1 d . . . H53 H 0.9061 0.4083 0.0139 0.071 Uiso 1 1 calc R . . C54 C 0.91325(18) 0.31617(12) -0.00593(9) 0.0654(5) Uani 1 1 d . . . H54 H 0.8884 0.3217 -0.0445 0.079 Uiso 1 1 calc R . . C55 C 0.9388(2) 0.25686(11) 0.01529(10) 0.0671(5) Uani 1 1 d . . . H55 H 0.9312 0.2218 -0.0091 0.081 Uiso 1 1 calc R . . C56 C 0.97534(19) 0.24701(10) 0.07121(9) 0.0598(5) Uani 1 1 d . A . C561 C 1.0036(3) 0.18044(11) 0.09296(14) 0.0850(7) Uani 1 1 d . . . H56A H 0.9692 0.1593 0.0575 0.102 Uiso 0.534(16) 1 calc PR A 1 H56B H 1.0159 0.1925 0.1330 0.102 Uiso 0.466(16) 1 d PR A 2 C62A C 0.9129(9) 0.1551(3) 0.1234(5) 0.076(2) Uani 0.534(16) 1 d P A 1 H62A H 0.9143 0.1091 0.1209 0.114 Uiso 0.534(16) 1 calc PR A 1 H62B H 0.8289 0.1707 0.1085 0.114 Uiso 0.534(16) 1 calc PR A 1 H62C H 0.9321 0.1678 0.1623 0.114 Uiso 0.534(16) 1 calc PR A 1 C63A C 1.1261(7) 0.1602(4) 0.0915(5) 0.081(2) Uani 0.534(16) 1 d P A 1 H63A H 1.1825 0.1813 0.1208 0.121 Uiso 0.534(16) 1 calc PR A 1 H63B H 1.1524 0.1703 0.0554 0.121 Uiso 0.534(16) 1 calc PR A 1 H63C H 1.1305 0.1146 0.0974 0.121 Uiso 0.534(16) 1 calc PR A 1 C62B C 0.8887(8) 0.1405(5) 0.0953(6) 0.084(3) Uani 0.466(16) 1 d P A 2 H62D H 0.8527 0.1288 0.0576 0.126 Uiso 0.466(16) 1 calc PR A 2 H62E H 0.8257 0.1642 0.1129 0.126 Uiso 0.466(16) 1 calc PR A 2 H62F H 0.9122 0.1024 0.1168 0.126 Uiso 0.466(16) 1 calc PR A 2 C63B C 1.0992(13) 0.1432(5) 0.0639(7) 0.101(4) Uani 0.466(16) 1 d P A 2 H63D H 1.1760 0.1684 0.0631 0.152 Uiso 0.466(16) 1 calc PR A 2 H63E H 1.0621 0.1334 0.0260 0.152 Uiso 0.466(16) 1 calc PR A 2 H63F H 1.1207 0.1040 0.0842 0.152 Uiso 0.466(16) 1 calc PR A 2 C5 C 1.13913(18) 0.28557(11) 0.18316(9) 0.0636(5) Uani 1 1 d . . . H5 H 1.2014 0.2934 0.1593 0.076 Uiso 1 1 calc R . . C6 C 1.17641(18) 0.26881(11) 0.23927(9) 0.0645(6) Uani 1 1 d . . . C61 C 1.2934(2) 0.26524(17) 0.27189(12) 0.1047(11) Uani 1 1 d . . . H61 H 1.3737 0.2738 0.2605 0.126 Uiso 1 1 calc R . . N6 N 1.08244(12) 0.25245(7) 0.27015(6) 0.0464(3) Uani 1 1 d . . . C7 C 1.13963(16) 0.23893(10) 0.32183(8) 0.0543(4) Uani 1 1 d . . . C71 C 1.27000(19) 0.24696(15) 0.32377(11) 0.0903(9) Uani 1 1 d . . . H71 H 1.3314 0.2409 0.3552 0.108 Uiso 1 1 calc R . . C8 C 1.06969(16) 0.21627(8) 0.36483(7) 0.0478(4) Uani 1 1 d . . . H8 H 1.1125 0.2107 0.4012 0.057 Uiso 1 1 calc R . . N8 N 0.95266(12) 0.20357(7) 0.35548(6) 0.0432(3) Uani 1 1 d . . . C81 C 0.89157(14) 0.17541(8) 0.39795(6) 0.0435(4) Uani 1 1 d . . . C82 C 0.92364(16) 0.11429(9) 0.41736(7) 0.0478(4) Uani 1 1 d . . . C821 C 1.02695(17) 0.07492(9) 0.39616(8) 0.0519(4) Uani 1 1 d . . . H821 H 1.0497 0.0954 0.3618 0.062 Uiso 1 1 calc R . . C822 C 0.9831(2) 0.00770(10) 0.38125(11) 0.0740(6) Uani 1 1 d . . . H82A H 0.9636 -0.0140 0.4147 0.111 Uiso 1 1 calc R . . H82B H 1.0504 -0.0149 0.3656 0.111 Uiso 1 1 calc R . . H82C H 0.9071 0.0091 0.3539 0.111 Uiso 1 1 calc R . . C823 C 1.14663(19) 0.07264(11) 0.43843(9) 0.0662(5) Uani 1 1 d . . . H82D H 1.1788 0.1154 0.4457 0.099 Uiso 1 1 calc R . . H82E H 1.2113 0.0472 0.4236 0.099 Uiso 1 1 calc R . . H82F H 1.1263 0.0538 0.4730 0.099 Uiso 1 1 calc R . . C83 C 0.85496(18) 0.08873(10) 0.45719(8) 0.0587(5) Uani 1 1 d . . . H83 H 0.8752 0.0477 0.4710 0.070 Uiso 1 1 calc R . . C84 C 0.75852(19) 0.12155(11) 0.47697(9) 0.0659(5) Uani 1 1 d . . . H84 H 0.7138 0.1034 0.5044 0.079 Uiso 1 1 calc R . . C85 C 0.72718(18) 0.18083(11) 0.45681(8) 0.0615(5) Uani 1 1 d . . . H85 H 0.6608 0.2032 0.4707 0.074 Uiso 1 1 calc R . . C86 C 0.79063(16) 0.20865(9) 0.41648(7) 0.0500(4) Uani 1 1 d . . . C861 C 0.75385(18) 0.27375(9) 0.39431(8) 0.0558(4) Uani 1 1 d . . . H861 H 0.7912 0.2790 0.3589 0.067 Uiso 1 1 calc R . . C862 C 0.6108(2) 0.28153(13) 0.38070(12) 0.0860(8) Uani 1 1 d . . . H86A H 0.5768 0.2474 0.3561 0.129 Uiso 1 1 calc R . . H86B H 0.5921 0.3221 0.3623 0.129 Uiso 1 1 calc R . . H86C H 0.5716 0.2801 0.4150 0.129 Uiso 1 1 calc R . . C863 C 0.8104(3) 0.32418(13) 0.43360(12) 0.1021(9) Uani 1 1 d . . . H86D H 0.7769 0.3200 0.4691 0.153 Uiso 1 1 calc R . . H86E H 0.7883 0.3657 0.4177 0.153 Uiso 1 1 calc R . . H86F H 0.9027 0.3196 0.4394 0.153 Uiso 1 1 calc R . . Fe1 Fe 0.91150(2) 0.276461(11) 0.231547(10) 0.04172(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0333(7) 0.0432(7) 0.0466(7) -0.0002(6) 0.0051(5) -0.0050(5) C11 0.0351(8) 0.0474(9) 0.0465(9) -0.0030(7) 0.0044(6) -0.0061(6) C12 0.0480(9) 0.0463(9) 0.0527(10) 0.0000(7) -0.0024(7) -0.0055(7) C121 0.0691(12) 0.0485(10) 0.0580(11) 0.0024(8) -0.0130(9) -0.0096(9) C122 0.104(2) 0.0888(18) 0.0959(19) -0.0253(15) -0.0449(16) 0.0357(15) C123 0.134(3) 0.110(2) 0.0661(15) 0.0278(14) -0.0208(15) -0.0580(19) C13 0.0649(12) 0.0469(10) 0.0643(12) 0.0000(8) -0.0071(9) -0.0106(8) C14 0.0637(12) 0.0572(11) 0.0617(12) -0.0053(9) -0.0094(9) -0.0161(9) C15 0.0537(11) 0.0658(12) 0.0508(10) 0.0008(9) -0.0054(8) -0.0132(9) C16 0.0410(9) 0.0557(10) 0.0491(9) 0.0024(7) 0.0038(7) -0.0083(7) C161 0.0565(11) 0.0645(12) 0.0540(11) 0.0109(9) -0.0025(8) -0.0181(9) C162 0.0654(13) 0.0970(17) 0.0646(13) 0.0234(12) 0.0129(10) -0.0090(12) C163 0.0835(15) 0.0618(13) 0.0699(13) 0.0074(10) 0.0063(11) 0.0052(11) C1 0.0316(8) 0.0502(9) 0.0510(9) 0.0007(7) 0.0039(7) -0.0027(6) C2 0.0328(8) 0.0459(9) 0.0537(10) -0.0017(7) 0.0027(7) 0.0005(6) C21 0.0378(9) 0.0544(10) 0.0710(12) -0.0100(9) 0.0015(8) 0.0079(7) N2 0.0326(6) 0.0417(7) 0.0503(8) -0.0006(6) 0.0038(5) -0.0020(5) C3 0.0407(8) 0.0404(8) 0.0500(9) 0.0003(7) 0.0003(7) -0.0020(6) C31 0.0486(10) 0.0458(9) 0.0657(11) -0.0100(8) -0.0005(8) 0.0049(7) C4 0.0399(8) 0.0421(9) 0.0562(10) -0.0014(7) 0.0012(7) -0.0017(7) N4 0.0413(8) 0.0447(8) 0.0672(9) -0.0046(7) -0.0033(7) -0.0013(6) C41 0.0411(9) 0.0400(9) 0.0730(12) -0.0120(8) -0.0028(8) -0.0022(7) C42 0.0461(10) 0.0502(10) 0.0793(13) -0.0140(9) 0.0042(9) -0.0026(8) C421 0.0570(13) 0.0937(17) 0.0836(16) 0.0062(13) 0.0089(11) -0.0087(11) C422 0.094(2) 0.181(4) 0.087(2) -0.032(2) 0.0165(16) -0.007(2) C423 0.119(3) 0.130(3) 0.157(3) 0.061(3) -0.002(2) -0.034(2) C43 0.0458(10) 0.0620(12) 0.0980(17) -0.0227(11) 0.0072(11) -0.0075(9) C44 0.0422(11) 0.0779(15) 0.112(2) -0.0230(14) -0.0109(12) -0.0055(10) C45 0.0567(13) 0.0807(15) 0.0892(16) -0.0083(12) -0.0182(12) -0.0093(11) C46 0.0509(11) 0.0560(11) 0.0773(13) -0.0081(10) -0.0080(9) -0.0065(8) C461 0.0638(13) 0.0916(17) 0.0726(14) 0.0011(12) -0.0071(11) -0.0108(12) C462 0.118(3) 0.099(2) 0.115(2) 0.0097(18) -0.0002(19) -0.0362(19) C463 0.098(2) 0.137(3) 0.0825(18) -0.0193(18) 0.0051(15) -0.0127(19) N5 0.0391(8) 0.0585(9) 0.0556(9) 0.0113(7) 0.0133(6) 0.0011(6) C51 0.0366(8) 0.0614(11) 0.0559(10) 0.0081(8) 0.0166(7) -0.0001(7) C52 0.0374(8) 0.0593(10) 0.0558(10) 0.0074(8) 0.0100(7) 0.0003(7) C521 0.0527(11) 0.0575(11) 0.0652(12) 0.0065(9) 0.0065(9) -0.0007(8) C522 0.104(2) 0.0830(17) 0.114(2) -0.0067(15) 0.0321(17) -0.0399(16) C523 0.0659(14) 0.0694(14) 0.1035(18) -0.0161(13) 0.0218(12) 0.0014(11) C53 0.0436(10) 0.0735(13) 0.0606(11) 0.0137(10) 0.0096(8) 0.0029(9) C54 0.0463(10) 0.0990(17) 0.0525(11) -0.0016(11) 0.0122(8) 0.0011(10) C55 0.0542(12) 0.0774(14) 0.0737(14) -0.0126(11) 0.0238(10) -0.0035(10) C56 0.0512(11) 0.0618(11) 0.0709(13) 0.0002(10) 0.0249(9) -0.0003(9) C561 0.0812(16) 0.0614(13) 0.121(2) 0.0061(13) 0.0436(15) 0.0071(12) C62A 0.073(4) 0.056(3) 0.105(5) 0.007(3) 0.036(4) -0.002(3) C63A 0.061(3) 0.070(4) 0.115(6) 0.009(3) 0.025(4) 0.017(3) C62B 0.066(4) 0.068(5) 0.119(7) 0.014(5) 0.015(4) -0.008(3) C63B 0.105(7) 0.071(5) 0.143(9) 0.008(5) 0.076(7) 0.020(5) C5 0.0374(9) 0.0875(15) 0.0685(12) 0.0222(11) 0.0167(8) -0.0013(9) C6 0.0359(9) 0.0912(15) 0.0679(12) 0.0257(11) 0.0129(8) -0.0028(9) C61 0.0294(10) 0.184(3) 0.1008(19) 0.068(2) 0.0067(11) -0.0130(13) N6 0.0330(7) 0.0523(8) 0.0554(8) 0.0072(6) 0.0113(6) -0.0016(6) C7 0.0347(9) 0.0696(12) 0.0579(11) 0.0145(9) 0.0033(7) -0.0037(8) C71 0.0322(10) 0.155(2) 0.0818(16) 0.0472(17) -0.0011(10) -0.0128(12) C8 0.0374(9) 0.0566(10) 0.0484(9) 0.0064(7) 0.0018(7) -0.0020(7) N8 0.0360(7) 0.0499(8) 0.0442(7) -0.0002(6) 0.0072(5) -0.0013(6) C81 0.0342(8) 0.0571(10) 0.0387(8) 0.0011(7) 0.0028(6) -0.0040(7) C82 0.0411(9) 0.0559(10) 0.0455(9) 0.0032(7) 0.0028(7) -0.0040(7) C821 0.0481(10) 0.0520(10) 0.0556(10) 0.0026(8) 0.0064(8) 0.0007(8) C822 0.0785(15) 0.0565(12) 0.0880(16) -0.0033(11) 0.0147(12) -0.0033(10) C823 0.0528(11) 0.0726(13) 0.0714(13) -0.0006(10) 0.0008(9) 0.0132(9) C83 0.0534(11) 0.0669(12) 0.0561(11) 0.0137(9) 0.0086(8) -0.0048(9) C84 0.0532(11) 0.0894(15) 0.0576(11) 0.0167(11) 0.0175(9) -0.0055(10) C85 0.0430(10) 0.0870(15) 0.0571(11) 0.0089(10) 0.0166(8) 0.0050(9) C86 0.0373(8) 0.0666(11) 0.0463(9) 0.0030(8) 0.0066(7) 0.0010(7) C861 0.0442(10) 0.0696(12) 0.0550(11) 0.0056(9) 0.0118(8) 0.0090(8) C862 0.0508(12) 0.108(2) 0.1015(19) 0.0345(15) 0.0188(12) 0.0225(12) C863 0.139(3) 0.0694(16) 0.0904(19) -0.0040(14) -0.0158(18) 0.0025(16) Fe1 0.03026(13) 0.04476(14) 0.05085(15) -0.00150(10) 0.00792(10) -0.00170(9) _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 N1 C1 1.300(2) . ? N1 C11 1.447(2) . ? N1 Fe1 2.0972(13) . ? C11 C12 1.401(2) . ? C11 C16 1.404(2) . ? C12 C13 1.392(2) . ? C12 C121 1.520(2) . ? C121 C122 1.518(3) . ? C121 C123 1.524(3) . ? C13 C14 1.378(3) . ? C14 C15 1.374(3) . ? C15 C16 1.398(2) . ? C16 C161 1.519(3) . ? C161 C162 1.527(3) . ? C161 C163 1.536(3) . ? C1 C2 1.414(2) . ? C2 N2 1.373(2) . ? C2 C21 1.398(2) . ? C21 C31 1.383(3) . ? N2 C3 1.361(2) . ? N2 Fe1 2.0444(13) . ? C3 C31 1.405(2) . ? C3 C4 1.446(2) . ? C4 N4 1.273(2) . ? N4 C41 1.427(2) . ? C41 C42 1.400(3) . ? C41 C46 1.402(3) . ? C42 C43 1.398(3) . ? C42 C421 1.515(3) . ? C421 C423 1.524(4) . ? C421 C422 1.536(4) . ? C43 C44 1.368(4) . ? C44 C45 1.380(4) . ? C45 C46 1.390(3) . ? C46 C461 1.520(3) . ? C461 C463 1.522(4) . ? C461 C462 1.530(4) . ? N5 C5 1.294(2) . ? N5 C51 1.439(2) . ? N5 Fe1 2.1347(14) . ? C51 C56 1.403(3) . ? C51 C52 1.406(3) . ? C52 C53 1.389(3) . ? C52 C521 1.515(3) . ? C521 C523 1.518(3) . ? C521 C522 1.529(3) . ? C53 C54 1.377(3) . ? C54 C55 1.376(3) . ? C55 C56 1.383(3) . ? C56 C561 1.527(3) . ? C561 C63A 1.378(8) . ? C561 C62A 1.398(7) . ? C561 C62B 1.496(9) . ? C561 C63B 1.530(9) . ? C5 C6 1.418(3) . ? C6 N6 1.370(2) . ? C6 C61 1.392(3) . ? C61 C71 1.373(3) . ? N6 C7 1.357(2) . ? N6 Fe1 2.0057(14) . ? C7 C71 1.394(3) . ? C7 C8 1.442(2) . ? C8 N8 1.267(2) . ? N8 C81 1.421(2) . ? C81 C86 1.407(2) . ? C81 C82 1.409(2) . ? C82 C83 1.396(2) . ? C82 C821 1.523(3) . ? C821 C822 1.532(3) . ? C821 C823 1.534(3) . ? C83 C84 1.378(3) . ? C84 C85 1.377(3) . ? C85 C86 1.392(3) . ? C86 C861 1.518(3) . ? C861 C863 1.510(3) . ? C861 C862 1.527(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C11 117.43(13) . . ? C1 N1 Fe1 108.52(10) . . ? C11 N1 Fe1 134.06(11) . . ? C12 C11 C16 121.57(15) . . ? C12 C11 N1 118.38(14) . . ? C16 C11 N1 120.04(15) . . ? C13 C12 C11 118.03(16) . . ? C13 C12 C121 120.11(16) . . ? C11 C12 C121 121.86(15) . . ? C122 C121 C12 110.10(19) . . ? C122 C121 C123 111.4(2) . . ? C12 C121 C123 111.93(17) . . ? C14 C13 C12 121.47(18) . . ? C15 C14 C13 119.65(17) . . ? C14 C15 C16 121.74(17) . . ? C15 C16 C11 117.52(16) . . ? C15 C16 C161 119.03(16) . . ? C11 C16 C161 123.44(15) . . ? C16 C161 C162 111.91(18) . . ? C16 C161 C163 110.84(16) . . ? C162 C161 C163 110.53(17) . . ? N1 C1 C2 121.50(14) . . ? N2 C2 C21 110.50(14) . . ? N2 C2 C1 117.84(14) . . ? C21 C2 C1 131.64(15) . . ? C31 C21 C2 106.42(15) . . ? C3 N2 C2 105.99(13) . . ? C3 N2 Fe1 144.56(11) . . ? C2 N2 Fe1 109.42(10) . . ? N2 C3 C31 110.31(14) . . ? N2 C3 C4 121.20(15) . . ? C31 C3 C4 128.46(15) . . ? C21 C31 C3 106.77(16) . . ? N4 C4 C3 121.35(16) . . ? C4 N4 C41 118.60(15) . . ? C42 C41 C46 121.81(17) . . ? C42 C41 N4 120.70(17) . . ? C46 C41 N4 117.34(18) . . ? C43 C42 C41 117.3(2) . . ? C43 C42 C421 120.1(2) . . ? C41 C42 C421 122.58(17) . . ? C42 C421 C423 112.2(2) . . ? C42 C421 C422 110.2(2) . . ? C423 C421 C422 112.5(3) . . ? C44 C43 C42 121.6(2) . . ? C43 C44 C45 120.1(2) . . ? C44 C45 C46 121.1(2) . . ? C45 C46 C41 117.8(2) . . ? C45 C46 C461 121.5(2) . . ? C41 C46 C461 120.61(17) . . ? C46 C461 C463 113.2(2) . . ? C46 C461 C462 109.6(2) . . ? C463 C461 C462 112.4(2) . . ? C5 N5 C51 118.25(15) . . ? C5 N5 Fe1 108.94(13) . . ? C51 N5 Fe1 132.73(11) . . ? C56 C51 C52 121.84(18) . . ? C56 C51 N5 118.37(17) . . ? C52 C51 N5 119.77(17) . . ? C53 C52 C51 117.44(18) . . ? C53 C52 C521 120.95(17) . . ? C51 C52 C521 121.59(17) . . ? C52 C521 C523 110.40(17) . . ? C52 C521 C522 112.95(19) . . ? C523 C521 C522 110.2(2) . . ? C54 C53 C52 121.5(2) . . ? C55 C54 C53 119.8(2) . . ? C54 C55 C56 121.7(2) . . ? C55 C56 C51 117.7(2) . . ? C55 C56 C561 120.0(2) . . ? C51 C56 C561 122.3(2) . . ? C63A C561 C62A 127.8(6) . . ? C63A C561 C62B 127.3(6) . . ? C62A C561 C62B 30.5(3) . . ? C63A C561 C56 115.2(4) . . ? C62A C561 C56 114.9(3) . . ? C62B C561 C56 114.3(4) . . ? C63A C561 C63B 30.7(5) . . ? C62A C561 C63B 126.2(6) . . ? C62B C561 C63B 108.7(10) . . ? C56 C561 C63B 115.6(5) . . ? N5 C5 C6 119.83(17) . . ? N6 C6 C61 109.67(18) . . ? N6 C6 C5 117.19(17) . . ? C61 C6 C5 133.14(19) . . ? C71 C61 C6 106.62(18) . . ? C7 N6 C6 106.79(14) . . ? C7 N6 Fe1 139.64(12) . . ? C6 N6 Fe1 111.18(12) . . ? N6 C7 C71 109.49(17) . . ? N6 C7 C8 122.06(15) . . ? C71 C7 C8 128.35(18) . . ? C61 C71 C7 107.43(19) . . ? N8 C8 C7 121.84(16) . . ? C8 N8 C81 119.31(14) . . ? C86 C81 C82 121.18(15) . . ? C86 C81 N8 117.41(15) . . ? C82 C81 N8 121.19(15) . . ? C83 C82 C81 117.71(17) . . ? C83 C82 C821 119.09(17) . . ? C81 C82 C821 123.19(15) . . ? C82 C821 C822 112.35(16) . . ? C82 C821 C823 111.38(16) . . ? C822 C821 C823 109.39(17) . . ? C84 C83 C82 121.68(19) . . ? C85 C84 C83 119.74(18) . . ? C84 C85 C86 121.47(19) . . ? C85 C86 C81 118.14(18) . . ? C85 C86 C861 120.74(17) . . ? C81 C86 C861 121.11(16) . . ? C863 C861 C86 110.95(18) . . ? C863 C861 C862 111.6(2) . . ? C86 C861 C862 112.41(17) . . ? N6 Fe1 N2 106.65(6) . . ? N6 Fe1 N1 153.35(6) . . ? N2 Fe1 N1 82.72(5) . . ? N6 Fe1 N5 81.06(6) . . ? N2 Fe1 N5 115.74(6) . . ? N1 Fe1 N5 117.96(6) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.197 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.035 #===END data_mb42 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H44 N3 O0.50' _chemical_formula_weight 478.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.07990(10) _cell_length_b 18.1845(5) _cell_length_c 27.3900(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.7080(14) _cell_angle_gamma 90.00 _cell_volume 3026.89(12) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9578 _exptl_absorpt_correction_T_max 0.9636 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree phi range. ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11599 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5903 _reflns_number_gt 4812 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KCCD (Nonius, 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.1000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.022(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5903 _refine_ls_number_parameters 362 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.2051 _refine_ls_wR_factor_gt 0.1940 _refine_ls_goodness_of_fit_ref 1.601 _refine_ls_restrained_S_all 1.603 _refine_ls_shift/su_max 0.060 _refine_ls_shift/su_mean 0.005 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 N1 N 0.64096(16) 0.71772(6) 0.05238(4) 0.0394(3) Uani 1 1 d . . . H1 H 0.4963 0.7197 0.0518 0.047 Uiso 1 1 calc R . . C2 C 0.7645(2) 0.70394(8) 0.01283(5) 0.0430(3) Uani 1 1 d . . . C3 C 0.9821(2) 0.70519(11) 0.02852(6) 0.0613(5) Uani 1 1 d . . . H3 H 1.1061 0.6972 0.0089 0.074 Uiso 1 1 calc R . . C4 C 0.9872(2) 0.72030(11) 0.07860(6) 0.0612(5) Uani 1 1 d . . . H4 H 1.1154 0.7245 0.0991 0.073 Uiso 1 1 calc R . . C5 C 0.7724(2) 0.72804(8) 0.09298(5) 0.0443(4) Uani 1 1 d . . . C6 C 0.6601(2) 0.69032(8) -0.03450(5) 0.0428(3) Uani 1 1 d . . . H6 H 0.7467 0.6811 -0.0621 0.051 Uiso 1 1 calc R . . N6 N 0.45228(17) 0.69079(6) -0.03872(4) 0.0429(3) Uani 1 1 d . . . C7 C 0.3392(2) 0.67626(8) -0.08398(5) 0.0453(4) Uani 1 1 d . . . C8 C 0.2406(2) 0.73553(10) -0.10912(6) 0.0564(4) Uani 1 1 d . . . C81 C 0.2753(3) 0.81327(11) -0.09141(7) 0.0701(5) Uani 1 1 d . . . H81 H 0.3326 0.8114 -0.0568 0.084 Uiso 1 1 calc R . . C82 C 0.4404(6) 0.85200(18) -0.12131(13) 0.1282(11) Uani 1 1 d . . . H82A H 0.5771 0.8234 -0.1212 0.192 Uiso 1 1 calc R . . H82B H 0.4700 0.9008 -0.1074 0.192 Uiso 1 1 calc R . . H82C H 0.3826 0.8572 -0.1549 0.192 Uiso 1 1 calc R . . C83 C 0.0551(5) 0.85770(18) -0.09287(14) 0.1311(11) Uani 1 1 d . . . H83A H 0.0835 0.9081 -0.0818 0.197 Uiso 1 1 calc R . . H83B H -0.0501 0.8342 -0.0714 0.197 Uiso 1 1 calc R . . H83C H -0.0060 0.8586 -0.1264 0.197 Uiso 1 1 calc R . . C9 C 0.1145(3) 0.72029(14) -0.15110(7) 0.0766(6) Uani 1 1 d . . . H9 H 0.0464 0.7597 -0.1686 0.092 Uiso 1 1 calc R . . C10 C 0.0863(3) 0.65034(15) -0.16768(7) 0.0839(7) Uani 1 1 d . . . H10 H 0.0017 0.6414 -0.1968 0.101 Uiso 1 1 calc R . . C11 C 0.1797(3) 0.59306(14) -0.14250(8) 0.0845(7) Uani 1 1 d . . . H11 H 0.1576 0.5445 -0.1544 0.101 Uiso 1 1 calc R . . C12 C 0.3074(3) 0.60378(10) -0.09954(7) 0.0638(5) Uani 1 1 d . A . C121 C 0.3963(4) 0.53959(11) -0.07001(10) 0.0907(8) Uani 1 1 d . . . H121 H 0.4492 0.5584 -0.0374 0.109 Uiso 0.69(2) 1 calc PR A 1 H21B H 0.5068 0.5615 -0.0465 0.136 Uiso 0.31(2) 1 d PR A 2 C122 C 0.5924(16) 0.5082(7) -0.0963(4) 0.158(4) Uani 0.69(2) 1 d P A 1 H12A H 0.5470 0.4946 -0.1297 0.237 Uiso 0.69(2) 1 calc PR A 1 H12B H 0.6472 0.4645 -0.0789 0.237 Uiso 0.69(2) 1 calc PR A 1 H12C H 0.7094 0.5452 -0.0972 0.237 Uiso 0.69(2) 1 calc PR A 1 C123 C 0.2206(18) 0.4829(5) -0.0620(6) 0.146(4) Uani 0.69(2) 1 d P A 1 H12D H 0.1702 0.4626 -0.0935 0.219 Uiso 0.69(2) 1 calc PR A 1 H12E H 0.0965 0.5058 -0.0458 0.219 Uiso 0.69(2) 1 calc PR A 1 H12F H 0.2809 0.4432 -0.0414 0.219 Uiso 0.69(2) 1 calc PR A 1 C12A C 0.220(4) 0.5078(17) -0.0365(8) 0.134(7) Uani 0.31(2) 1 d P A 2 H12G H 0.0924 0.4915 -0.0565 0.201 Uiso 0.31(2) 1 calc PR A 2 H12H H 0.1732 0.5459 -0.0137 0.201 Uiso 0.31(2) 1 calc PR A 2 H12I H 0.2810 0.4660 -0.0182 0.201 Uiso 0.31(2) 1 calc PR A 2 C12B C 0.519(4) 0.4745(11) -0.0942(9) 0.159(7) Uani 0.31(2) 1 d P A 2 H12J H 0.5808 0.4421 -0.0688 0.238 Uiso 0.31(2) 1 calc PR A 2 H12K H 0.6372 0.4938 -0.1140 0.238 Uiso 0.31(2) 1 calc PR A 2 H12L H 0.4147 0.4467 -0.1151 0.238 Uiso 0.31(2) 1 calc PR A 2 C13 C 0.6768(2) 0.74487(8) 0.13939(5) 0.0449(4) Uani 1 1 d . . . H13 H 0.7681 0.7526 0.1677 0.054 Uiso 1 1 calc R . . N13 N 0.46980(17) 0.74918(7) 0.14170(4) 0.0433(3) Uani 1 1 d . . . C14 C 0.3568(2) 0.76700(8) 0.18469(5) 0.0467(4) Uani 1 1 d . . . C15 C 0.2922(2) 0.83995(10) 0.19255(6) 0.0562(4) Uani 1 1 d . . . C151 C 0.3713(3) 0.90078(10) 0.15976(7) 0.0689(5) Uani 1 1 d . . . H151 H 0.4200 0.8775 0.1288 0.083 Uiso 1 1 calc R . . C152 C 0.1916(4) 0.95655(18) 0.14608(12) 0.1194(10) Uani 1 1 d . . . H15A H 0.0551 0.9305 0.1373 0.179 Uiso 1 1 calc R . . H15B H 0.2379 0.9860 0.1182 0.179 Uiso 1 1 calc R . . H15C H 0.1668 0.9890 0.1740 0.179 Uiso 1 1 calc R . . C153 C 0.5679(4) 0.93958(16) 0.18276(11) 0.1070(9) Uani 1 1 d . . . H15D H 0.5221 0.9670 0.2115 0.160 Uiso 1 1 calc R . . H15E H 0.6296 0.9737 0.1591 0.160 Uiso 1 1 calc R . . H15F H 0.6797 0.9032 0.1926 0.160 Uiso 1 1 calc R . . C16 C 0.1585(3) 0.85441(13) 0.23183(7) 0.0752(6) Uani 1 1 d . . . H16 H 0.1136 0.9036 0.2377 0.090 Uiso 1 1 calc R . . C17 C 0.0895(3) 0.79951(16) 0.26233(7) 0.0833(7) Uani 1 1 d . . . H17 H -0.0005 0.8106 0.2891 0.100 Uiso 1 1 calc R . . C18 C 0.1520(3) 0.72914(15) 0.25360(7) 0.0781(6) Uani 1 1 d . . . H18 H 0.1032 0.6915 0.2747 0.094 Uiso 1 1 calc R . . C19 C 0.2847(3) 0.70975(10) 0.21499(5) 0.0593(5) Uani 1 1 d . . . C191 C 0.3476(4) 0.63100(11) 0.20557(7) 0.0733(6) Uani 1 1 d . . . H191 H 0.4104 0.6288 0.1723 0.088 Uiso 1 1 calc R . . C192 C 0.5241(4) 0.60449(16) 0.24162(11) 0.1073(8) Uani 1 1 d . . . H19A H 0.6481 0.6389 0.2420 0.161 Uiso 1 1 calc R . . H19B H 0.5748 0.5556 0.2319 0.161 Uiso 1 1 calc R . . H19C H 0.4634 0.6018 0.2743 0.161 Uiso 1 1 calc R . . C193 C 0.1494(5) 0.57945(15) 0.20565(12) 0.1125(9) Uani 1 1 d . . . H19D H 0.1007 0.5732 0.2392 0.169 Uiso 1 1 calc R . . H19E H 0.1908 0.5316 0.1923 0.169 Uiso 1 1 calc R . . H19F H 0.0294 0.6005 0.1855 0.169 Uiso 1 1 calc R . . O1S O 0.5000 1.0000 0.0000 0.177(2) Uani 1 2 d SU . . C1S1 C 0.668(3) 0.9730(10) -0.0002(6) 0.140(5) Uani 0.343(16) 1 d PU B 1 H1S1 H 0.7759 1.0132 0.0058 0.169 Uiso 0.343(16) 1 calc PR B 1 H1S1 H 0.6884 0.9566 -0.0342 0.169 Uiso 0.343(16) 1 calc PR B 1 C1S2 C 0.583(3) 0.9394(9) 0.0212(5) 0.230(6) Uani 0.657(16) 1 d PU B 2 H1S2 H 0.5104 0.9404 0.0531 0.275 Uiso 0.657(16) 1 calc PR B 2 H1S2 H 0.5045 0.9003 0.0025 0.275 Uiso 0.657(16) 1 calc PR B 2 C2S C 0.7442(11) 0.9110(3) 0.0313(2) 0.199(2) Uani 1 1 d U . . H2SA H 0.9018 0.9028 0.0271 0.299 Uiso 0.343(16) 1 calc PR B 1 H2SB H 0.6627 0.8663 0.0221 0.299 Uiso 0.343(16) 1 calc PR B 1 H2SC H 0.7181 0.9228 0.0656 0.299 Uiso 0.343(16) 1 calc PR B 1 H2SD H 0.7283 0.8602 0.0427 0.299 Uiso 0.657(16) 1 d PR B 2 H2SE H 0.8156 0.9405 0.0572 0.299 Uiso 0.657(16) 1 d PR B 2 H2SF H 0.8343 0.9117 0.0022 0.299 Uiso 0.657(16) 1 d PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0304(5) 0.0485(6) 0.0391(6) -0.0025(5) -0.0012(4) -0.0015(4) C2 0.0362(6) 0.0512(8) 0.0416(7) -0.0059(6) 0.0017(5) -0.0021(5) C3 0.0331(7) 0.0985(13) 0.0524(9) -0.0157(8) 0.0026(6) -0.0002(7) C4 0.0346(7) 0.0969(13) 0.0516(9) -0.0140(8) -0.0068(6) -0.0017(7) C5 0.0365(6) 0.0537(8) 0.0425(8) -0.0036(6) -0.0054(5) -0.0039(5) C6 0.0394(7) 0.0491(8) 0.0400(7) -0.0062(6) 0.0037(5) -0.0008(5) N6 0.0391(6) 0.0509(7) 0.0385(6) -0.0061(5) -0.0003(4) -0.0002(4) C7 0.0382(6) 0.0605(9) 0.0371(7) -0.0060(6) 0.0017(5) -0.0009(5) C8 0.0532(8) 0.0750(11) 0.0411(8) 0.0069(7) 0.0022(6) 0.0009(7) C81 0.0914(13) 0.0635(11) 0.0555(10) 0.0123(8) 0.0014(9) 0.0084(9) C82 0.150(3) 0.101(2) 0.136(3) -0.0071(18) 0.045(2) -0.0468(18) C83 0.132(2) 0.102(2) 0.160(3) 0.007(2) 0.017(2) 0.0349(17) C9 0.0688(11) 0.1118(17) 0.0485(10) 0.0141(10) -0.0100(8) -0.0022(10) C10 0.0690(11) 0.129(2) 0.0529(11) -0.0107(11) -0.0165(9) -0.0147(11) C11 0.0802(12) 0.0980(16) 0.0745(13) -0.0306(12) -0.0128(10) -0.0226(11) C12 0.0570(9) 0.0682(11) 0.0656(11) -0.0180(8) -0.0091(7) -0.0055(7) C121 0.0968(14) 0.0534(11) 0.120(2) -0.0207(11) -0.0348(14) 0.0052(10) C122 0.126(5) 0.098(6) 0.246(8) -0.046(6) -0.036(5) 0.054(4) C123 0.163(6) 0.080(4) 0.191(10) 0.046(5) -0.046(7) -0.021(4) C12A 0.141(12) 0.142(16) 0.119(12) 0.036(10) -0.006(9) 0.030(11) C12B 0.177(14) 0.063(8) 0.237(17) -0.042(10) 0.035(13) 0.013(8) C13 0.0387(7) 0.0559(8) 0.0396(7) -0.0027(6) -0.0067(5) -0.0042(5) N13 0.0408(6) 0.0526(7) 0.0365(6) -0.0029(5) -0.0016(4) -0.0050(4) C14 0.0388(6) 0.0661(9) 0.0349(7) -0.0065(6) -0.0035(5) -0.0069(6) C15 0.0498(8) 0.0712(11) 0.0474(9) -0.0118(7) -0.0028(6) 0.0030(7) C151 0.0776(11) 0.0625(11) 0.0668(11) -0.0050(8) 0.0057(8) 0.0115(8) C152 0.0996(17) 0.112(2) 0.146(3) 0.0337(19) -0.0111(16) 0.0234(15) C153 0.0879(14) 0.0979(18) 0.135(2) 0.0190(16) -0.0074(14) -0.0187(13) C16 0.0594(10) 0.1075(16) 0.0589(11) -0.0263(11) 0.0020(8) 0.0122(9) C17 0.0613(10) 0.137(2) 0.0522(11) -0.0270(12) 0.0150(8) -0.0115(11) C18 0.0722(11) 0.1170(18) 0.0458(10) -0.0047(10) 0.0109(8) -0.0326(11) C19 0.0620(9) 0.0767(12) 0.0392(8) -0.0031(7) 0.0009(6) -0.0219(7) C191 0.0972(13) 0.0698(12) 0.0532(10) 0.0060(8) 0.0059(9) -0.0277(10) C192 0.1051(17) 0.0920(18) 0.123(2) 0.0006(15) -0.0190(16) -0.0029(13) C193 0.1175(18) 0.0895(17) 0.129(2) 0.0077(16) -0.0171(16) -0.0469(15) O1S 0.246(6) 0.102(3) 0.186(5) 0.036(3) 0.076(4) 0.016(3) C1S1 0.203(12) 0.113(10) 0.108(8) 0.020(6) 0.043(8) -0.008(7) C1S2 0.260(13) 0.240(12) 0.187(9) 0.087(10) -0.018(9) 0.031(10) C2S 0.313(8) 0.116(3) 0.171(5) 0.036(3) 0.037(5) 0.039(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.3599(17) . ? N1 C5 1.3628(16) . ? C2 C3 1.3793(19) . ? C2 C6 1.4477(18) . ? C3 C4 1.398(2) . ? C4 C5 1.382(2) . ? C5 C13 1.446(2) . ? C6 N6 1.2651(17) . ? N6 C7 1.4242(17) . ? C7 C12 1.397(2) . ? C7 C8 1.404(2) . ? C8 C9 1.391(2) . ? C8 C81 1.507(3) . ? C81 C82 1.491(3) . ? C81 C83 1.563(3) . ? C9 C10 1.360(3) . ? C10 C11 1.363(3) . ? C11 C12 1.404(2) . ? C12 C121 1.511(3) . ? C121 C123 1.505(9) . ? C121 C122 1.523(9) . ? C121 C12B 1.556(16) . ? C121 C12A 1.54(2) . ? C13 N13 1.2644(17) . ? N13 C14 1.4182(18) . ? C14 C19 1.409(2) . ? C14 C15 1.402(2) . ? C15 C16 1.393(2) . ? C15 C151 1.512(3) . ? C151 C153 1.509(3) . ? C151 C152 1.529(3) . ? C16 C17 1.375(3) . ? C17 C18 1.358(3) . ? C18 C19 1.395(3) . ? C19 C191 1.506(3) . ? C191 C192 1.515(3) . ? C191 C193 1.527(3) . ? O1S C1S1 1.135(16) . ? O1S C1S2 1.337(12) . ? C1S1 C2S 1.486(19) . ? C1S2 C2S 1.136(11) . ? 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 C2 N1 C5 110.55(10) . . ? N1 C2 C3 107.23(12) . . ? N1 C2 C6 120.46(11) . . ? C3 C2 C6 132.30(13) . . ? C2 C3 C4 107.56(13) . . ? C5 C4 C3 107.84(12) . . ? N1 C5 C4 106.82(12) . . ? N1 C5 C13 120.33(11) . . ? C4 C5 C13 132.84(12) . . ? N6 C6 C2 119.38(12) . . ? C6 N6 C7 122.20(11) . . ? C12 C7 C8 121.43(14) . . ? C12 C7 N6 119.97(14) . . ? C8 C7 N6 118.20(13) . . ? C9 C8 C7 118.00(17) . . ? C9 C8 C81 121.44(17) . . ? C7 C8 C81 120.55(14) . . ? C82 C81 C8 110.9(2) . . ? C82 C81 C83 109.4(2) . . ? C8 C81 C83 111.4(2) . . ? C10 C9 C8 121.56(19) . . ? C9 C10 C11 119.97(16) . . ? C10 C11 C12 122.0(2) . . ? C7 C12 C11 117.05(18) . . ? C7 C12 C121 121.44(14) . . ? C11 C12 C121 121.43(18) . . ? C123 C121 C12 111.3(3) . . ? C123 C121 C122 112.4(5) . . ? C12 C121 C122 108.0(5) . . ? C12 C121 C12B 121.8(10) . . ? C12 C121 C12A 111.3(7) . . ? C12B C121 C12A 108.6(11) . . ? N13 C13 C5 118.93(11) . . ? C13 N13 C14 124.27(11) . . ? C19 C14 C15 120.98(14) . . ? C19 C14 N13 119.15(14) . . ? C15 C14 N13 119.25(13) . . ? C16 C15 C14 118.05(17) . . ? C16 C15 C151 121.59(17) . . ? C14 C15 C151 120.34(14) . . ? C153 C151 C15 110.86(17) . . ? C153 C151 C152 110.1(2) . . ? C15 C151 C152 113.14(18) . . ? C17 C16 C15 121.8(2) . . ? C18 C17 C16 119.02(18) . . ? C17 C18 C19 122.89(19) . . ? C18 C19 C14 117.20(18) . . ? C18 C19 C191 121.72(17) . . ? C14 C19 C191 121.08(15) . . ? C19 C191 C192 111.67(17) . . ? C19 C191 C193 112.3(2) . . ? C192 C191 C193 110.3(2) . . ? C1S1 O1S C1S2 132.9(7) 3_675 . ? O1S C1S1 C2S 126.1(15) . . ? C2S C1S2 O1S 142.4(19) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.391 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.031 #===END data_MB48 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H54 N6 Zr' _chemical_formula_weight 686.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.7035(2) _cell_length_b 11.32660(10) _cell_length_c 22.2836(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.8130(6) _cell_angle_gamma 90.00 _cell_volume 3676.68(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.61 _exptl_crystal_size_min 0.49 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8228 _exptl_absorpt_correction_T_max 0.8539 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree phi range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13383 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7069 _reflns_number_gt 6675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.0480P)^2^+1.5040P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7069 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Zr1 Zr 0.321787(9) 0.343799(13) 0.159828(6) 0.02146(8) Uani 1 1 d . . . N1 N 0.33875(9) 0.47488(12) 0.08599(6) 0.0261(3) Uani 1 1 d . . . C2 C 0.41060(12) 0.51598(16) 0.06010(8) 0.0312(4) Uani 1 1 d . . . H2 H 0.4731 0.4970 0.0733 0.037 Uiso 1 1 calc R . . C3 C 0.38038(13) 0.59015(17) 0.01138(8) 0.0354(4) Uani 1 1 d . . . H3 H 0.4177 0.6298 -0.0138 0.042 Uiso 1 1 calc R . . C4 C 0.28520(13) 0.59493(15) 0.00687(8) 0.0330(4) Uani 1 1 d . . . H4 H 0.2447 0.6380 -0.0220 0.040 Uiso 1 1 calc R . . C5 C 0.26109(12) 0.52346(14) 0.05339(8) 0.0275(3) Uani 1 1 d . . . C6 C 0.17604(11) 0.48838(15) 0.06974(7) 0.0274(3) Uani 1 1 d . . . H6 H 0.1209 0.5203 0.0488 0.033 Uiso 1 1 calc R . . N7 N 0.17185(9) 0.41254(12) 0.11335(6) 0.0257(3) Uani 1 1 d . . . C71 C 0.07893(11) 0.38717(16) 0.12488(8) 0.0283(3) Uani 1 1 d . . . C72 C 0.04276(12) 0.44774(17) 0.17138(8) 0.0329(4) Uani 1 1 d . . . C73 C -0.04835(13) 0.4267(2) 0.17891(10) 0.0420(5) Uani 1 1 d . . . H73 H -0.0741 0.4670 0.2100 0.050 Uiso 1 1 calc R . . C74 C -0.10208(14) 0.34799(19) 0.14191(12) 0.0468(5) Uani 1 1 d . . . H74 H -0.1643 0.3354 0.1473 0.056 Uiso 1 1 calc R . . C75 C -0.06491(13) 0.28797(19) 0.09723(10) 0.0432(5) Uani 1 1 d . . . H75 H -0.1020 0.2336 0.0723 0.052 Uiso 1 1 calc R . . C76 C 0.02580(12) 0.30539(17) 0.08783(9) 0.0328(4) Uani 1 1 d . . . C77 C 0.09904(13) 0.5372(2) 0.21137(9) 0.0402(4) Uani 1 1 d . . . H77 H 0.1654 0.5202 0.2098 0.048 Uiso 1 1 calc R . . C78 C 0.0792(2) 0.6630(2) 0.18766(13) 0.0594(7) Uani 1 1 d . . . H78A H 0.0927 0.6686 0.1459 0.089 Uiso 1 1 calc R . . H78B H 0.1178 0.7190 0.2132 0.089 Uiso 1 1 calc R . . H78C H 0.0144 0.6818 0.1888 0.089 Uiso 1 1 calc R . . C79 C 0.08245(16) 0.5290(3) 0.27753(10) 0.0579(6) Uani 1 1 d . . . H79A H 0.0196 0.5542 0.2810 0.087 Uiso 1 1 calc R . . H79B H 0.1260 0.5802 0.3025 0.087 Uiso 1 1 calc R . . H79C H 0.0911 0.4472 0.2915 0.087 Uiso 1 1 calc R . . C80 C 0.06374(12) 0.23169(17) 0.03989(9) 0.0364(4) Uani 1 1 d . . . H80 H 0.1280 0.2585 0.0377 0.044 Uiso 1 1 calc R . . C81 C 0.00844(15) 0.2478(3) -0.02274(10) 0.0547(6) Uani 1 1 d . . . H81A H 0.0358 0.2002 -0.0524 0.082 Uiso 1 1 calc R . . H81B H 0.0091 0.3313 -0.0343 0.082 Uiso 1 1 calc R . . H81C H -0.0550 0.2224 -0.0217 0.082 Uiso 1 1 calc R . . C82 C 0.06713(17) 0.1016(2) 0.05720(12) 0.0520(5) Uani 1 1 d . . . H82A H 0.1082 0.0910 0.0953 0.078 Uiso 1 1 calc R . . H82B H 0.0901 0.0556 0.0252 0.078 Uiso 1 1 calc R . . H82C H 0.0053 0.0746 0.0623 0.078 Uiso 1 1 calc R . . N8 N 0.47434(10) 0.32508(13) 0.16565(6) 0.0270(3) Uani 1 1 d . . . C9 C 0.54711(12) 0.37905(18) 0.19846(8) 0.0325(4) Uani 1 1 d . . . H9 H 0.5426 0.4329 0.2306 0.039 Uiso 1 1 calc R . . C10 C 0.62919(13) 0.34531(17) 0.17887(9) 0.0349(4) Uani 1 1 d . . . H10 H 0.6891 0.3715 0.1947 0.042 Uiso 1 1 calc R . . C11 C 0.60635(12) 0.26536(17) 0.13148(8) 0.0320(4) Uani 1 1 d . . . H11 H 0.6475 0.2259 0.1088 0.038 Uiso 1 1 calc R . . C12 C 0.51088(11) 0.25510(15) 0.12409(7) 0.0261(3) Uani 1 1 d . . . C13 C 0.44938(11) 0.18995(15) 0.08172(7) 0.0267(3) Uani 1 1 d . . . H13 H 0.4737 0.1395 0.0538 0.032 Uiso 1 1 calc R . . N14 N 0.36114(9) 0.19738(12) 0.08013(6) 0.0248(3) Uani 1 1 d . . . C141 C 0.31032(11) 0.12060(15) 0.03546(7) 0.0263(3) Uani 1 1 d . . . C142 C 0.27979(12) 0.16394(15) -0.02287(8) 0.0281(4) Uani 1 1 d . . . C143 C 0.23723(12) 0.08468(17) -0.06589(8) 0.0339(4) Uani 1 1 d . . . H143 H 0.2150 0.1124 -0.1054 0.041 Uiso 1 1 calc R . . C144 C 0.22680(14) -0.03302(18) -0.05223(9) 0.0388(4) Uani 1 1 d . . . H144 H 0.1997 -0.0859 -0.0826 0.047 Uiso 1 1 calc R . . C145 C 0.25586(14) -0.07389(17) 0.00575(9) 0.0374(4) Uani 1 1 d . . . H145 H 0.2475 -0.1547 0.0150 0.045 Uiso 1 1 calc R . . C146 C 0.29723(12) 0.00175(16) 0.05087(8) 0.0311(4) Uani 1 1 d . . . C147 C 0.29916(13) 0.28964(16) -0.04156(8) 0.0317(4) Uani 1 1 d . . . H147 H 0.3092 0.3391 -0.0041 0.038 Uiso 1 1 calc R . . C148 C 0.38751(14) 0.2919(2) -0.07058(9) 0.0431(5) Uani 1 1 d . . . H14A H 0.4389 0.2647 -0.0411 0.065 Uiso 1 1 calc R . . H14B H 0.3995 0.3726 -0.0832 0.065 Uiso 1 1 calc R . . H14C H 0.3809 0.2397 -0.1060 0.065 Uiso 1 1 calc R . . C149 C 0.22102(16) 0.34529(18) -0.08469(10) 0.0427(5) Uani 1 1 d . . . H14D H 0.2121 0.3009 -0.1228 0.064 Uiso 1 1 calc R . . H14E H 0.2365 0.4274 -0.0928 0.064 Uiso 1 1 calc R . . H14F H 0.1644 0.3432 -0.0661 0.064 Uiso 1 1 calc R . . C150 C 0.32976(14) -0.04678(17) 0.11363(9) 0.0389(4) Uani 1 1 d . . . H150 H 0.3415 0.0218 0.1419 0.047 Uiso 1 1 calc R . . C151 C 0.25799(17) -0.1259(2) 0.13741(10) 0.0499(5) Uani 1 1 d . . . H15A H 0.1981 -0.0865 0.1313 0.075 Uiso 1 1 calc R . . H15B H 0.2761 -0.1407 0.1807 0.075 Uiso 1 1 calc R . . H15C H 0.2539 -0.2011 0.1154 0.075 Uiso 1 1 calc R . . C152 C 0.41982(16) -0.1145(2) 0.11473(11) 0.0538(6) Uani 1 1 d . . . H15D H 0.4105 -0.1817 0.0868 0.081 Uiso 1 1 calc R . . H15E H 0.4400 -0.1433 0.1559 0.081 Uiso 1 1 calc R . . H15F H 0.4668 -0.0620 0.1022 0.081 Uiso 1 1 calc R . . N15 N 0.34201(10) 0.46769(13) 0.22721(6) 0.0293(3) Uani 1 1 d . . . C16 C 0.38543(15) 0.58261(18) 0.22181(9) 0.0416(4) Uani 1 1 d . . . H16A H 0.3411 0.6454 0.2264 0.062 Uiso 1 1 calc R . . H16B H 0.4060 0.5891 0.1819 0.062 Uiso 1 1 calc R . . H16C H 0.4383 0.5904 0.2534 0.062 Uiso 1 1 calc R . . C17 C 0.32078(13) 0.45443(18) 0.28908(8) 0.0372(4) Uani 1 1 d . . . H17A H 0.3780 0.4495 0.3172 0.056 Uiso 1 1 calc R . . H17B H 0.2849 0.3822 0.2920 0.056 Uiso 1 1 calc R . . H17C H 0.2851 0.5227 0.2996 0.056 Uiso 1 1 calc R . . N18 N 0.25726(10) 0.21987(13) 0.20587(6) 0.0283(3) Uani 1 1 d . . . C19 C 0.17110(14) 0.17082(19) 0.21884(10) 0.0398(5) Uani 1 1 d . . . H19A H 0.1700 0.0857 0.2108 0.060 Uiso 1 1 calc R . . H19B H 0.1202 0.2089 0.1930 0.060 Uiso 1 1 calc R . . H19C H 0.1648 0.1846 0.2615 0.060 Uiso 1 1 calc R . . C20 C 0.33346(14) 0.16514(17) 0.24514(9) 0.0361(4) Uani 1 1 d . . . H20A H 0.3256 0.1780 0.2876 0.054 Uiso 1 1 calc R . . H20B H 0.3915 0.2006 0.2372 0.054 Uiso 1 1 calc R . . H20C H 0.3344 0.0802 0.2369 0.054 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 Zr1 0.01901(11) 0.02234(11) 0.02298(11) -0.00004(5) 0.00266(7) -0.00063(5) N1 0.0250(7) 0.0255(7) 0.0279(7) 0.0001(6) 0.0038(5) -0.0036(5) C2 0.0290(8) 0.0303(9) 0.0353(9) -0.0002(7) 0.0076(7) -0.0057(7) C3 0.0424(10) 0.0304(9) 0.0350(9) 0.0026(7) 0.0110(8) -0.0090(8) C4 0.0434(10) 0.0248(8) 0.0307(8) 0.0026(7) 0.0042(7) -0.0008(7) C5 0.0308(8) 0.0230(8) 0.0286(8) -0.0011(6) 0.0032(6) 0.0004(6) C6 0.0258(8) 0.0265(8) 0.0291(8) -0.0017(6) 0.0004(6) 0.0050(6) N7 0.0221(6) 0.0271(7) 0.0279(7) -0.0021(5) 0.0032(5) 0.0006(5) C71 0.0198(8) 0.0302(9) 0.0348(9) 0.0021(7) 0.0035(6) 0.0022(7) C72 0.0270(8) 0.0367(9) 0.0353(9) 0.0015(7) 0.0048(7) 0.0062(7) C73 0.0294(9) 0.0499(12) 0.0491(11) -0.0024(9) 0.0136(8) 0.0068(8) C74 0.0240(9) 0.0535(13) 0.0652(14) -0.0020(10) 0.0140(9) -0.0016(8) C75 0.0238(9) 0.0429(11) 0.0627(13) -0.0072(10) 0.0058(8) -0.0036(8) C76 0.0245(8) 0.0308(9) 0.0426(10) -0.0025(8) 0.0026(7) 0.0014(7) C77 0.0300(9) 0.0529(12) 0.0383(10) -0.0118(9) 0.0066(7) 0.0052(8) C78 0.0694(17) 0.0472(14) 0.0609(15) -0.0132(11) 0.0068(13) -0.0063(11) C79 0.0467(12) 0.0886(19) 0.0383(11) -0.0137(12) 0.0054(9) 0.0129(12) C80 0.0230(8) 0.0393(10) 0.0461(10) -0.0121(8) 0.0018(7) -0.0015(7) C81 0.0384(11) 0.0742(16) 0.0497(12) -0.0104(11) 0.0000(9) 0.0071(11) C82 0.0524(13) 0.0386(12) 0.0649(14) -0.0114(10) 0.0075(11) 0.0050(10) N8 0.0223(7) 0.0291(7) 0.0293(7) -0.0021(6) 0.0021(5) -0.0011(5) C9 0.0270(8) 0.0374(9) 0.0319(9) -0.0035(8) -0.0009(7) -0.0043(8) C10 0.0224(8) 0.0437(11) 0.0376(10) 0.0008(7) -0.0002(7) -0.0062(7) C11 0.0237(8) 0.0400(10) 0.0330(9) 0.0048(7) 0.0062(6) 0.0016(7) C12 0.0222(8) 0.0278(8) 0.0283(8) 0.0021(6) 0.0040(6) 0.0009(6) C13 0.0279(8) 0.0252(8) 0.0276(8) -0.0007(7) 0.0063(6) 0.0020(7) N14 0.0247(7) 0.0234(7) 0.0258(7) -0.0005(6) 0.0012(5) -0.0010(6) C141 0.0236(8) 0.0272(8) 0.0284(8) -0.0054(7) 0.0045(6) -0.0004(7) C142 0.0272(8) 0.0301(9) 0.0277(8) -0.0032(6) 0.0062(7) -0.0027(6) C143 0.0344(9) 0.0383(10) 0.0287(8) -0.0056(7) 0.0034(7) -0.0061(8) C144 0.0438(11) 0.0377(10) 0.0347(9) -0.0104(8) 0.0044(8) -0.0119(8) C145 0.0438(10) 0.0271(9) 0.0412(10) -0.0058(8) 0.0052(8) -0.0060(8) C146 0.0322(9) 0.0279(8) 0.0334(9) -0.0026(7) 0.0051(7) -0.0004(7) C147 0.0376(9) 0.0313(9) 0.0256(8) -0.0025(7) 0.0021(7) -0.0064(7) C148 0.0406(11) 0.0482(12) 0.0410(10) 0.0026(9) 0.0075(8) -0.0146(9) C149 0.0487(12) 0.0415(11) 0.0364(10) 0.0054(8) 0.0003(9) 0.0007(8) C150 0.0525(12) 0.0272(9) 0.0354(9) -0.0001(7) 0.0000(8) -0.0017(8) C151 0.0622(14) 0.0411(11) 0.0472(12) 0.0129(10) 0.0107(10) 0.0018(10) C152 0.0474(12) 0.0503(13) 0.0590(14) 0.0096(11) -0.0097(10) 0.0004(10) N15 0.0283(7) 0.0303(7) 0.0287(7) -0.0022(6) 0.0019(6) 0.0002(6) C16 0.0521(12) 0.0326(10) 0.0402(10) -0.0079(8) 0.0065(9) -0.0084(9) C17 0.0385(10) 0.0443(11) 0.0284(9) -0.0052(8) 0.0035(7) 0.0015(8) N18 0.0264(7) 0.0294(7) 0.0294(7) 0.0036(6) 0.0045(5) -0.0016(6) C19 0.0329(10) 0.0450(11) 0.0419(11) 0.0125(8) 0.0060(8) -0.0063(8) C20 0.0351(10) 0.0375(10) 0.0358(10) 0.0090(7) 0.0045(8) 0.0019(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 Zr1 N18 2.0465(14) . ? Zr1 N15 2.0472(15) . ? Zr1 N8 2.2392(14) . ? Zr1 N1 2.2551(14) . ? Zr1 N7 2.4327(13) . ? Zr1 N14 2.5532(14) . ? N1 C2 1.353(2) . ? N1 C5 1.382(2) . ? C2 C3 1.397(3) . ? C3 C4 1.390(3) . ? C4 C5 1.398(2) . ? C5 C6 1.407(2) . ? C6 N7 1.305(2) . ? N7 C71 1.453(2) . ? C71 C76 1.405(3) . ? C71 C72 1.406(2) . ? C72 C73 1.393(3) . ? C72 C77 1.518(3) . ? C73 C74 1.386(3) . ? C74 C75 1.378(3) . ? C75 C76 1.392(3) . ? C76 C80 1.520(3) . ? C77 C79 1.529(3) . ? C77 C78 1.534(3) . ? C80 C82 1.522(3) . ? C80 C81 1.528(3) . ? N8 C9 1.357(2) . ? N8 C12 1.382(2) . ? C9 C10 1.391(3) . ? C10 C11 1.397(3) . ? C11 C12 1.396(2) . ? C12 C13 1.422(2) . ? C13 N14 1.296(2) . ? N14 C141 1.450(2) . ? C141 C142 1.405(2) . ? C141 C146 1.409(2) . ? C142 C143 1.398(2) . ? C142 C147 1.521(2) . ? C143 C144 1.381(3) . ? C144 C145 1.384(3) . ? C145 C146 1.396(3) . ? C146 C150 1.518(3) . ? C147 C148 1.528(3) . ? C147 C149 1.530(3) . ? C150 C152 1.528(3) . ? C150 C151 1.533(3) . ? N15 C16 1.462(2) . ? N15 C17 1.462(2) . ? N18 C19 1.448(2) . ? N18 C20 1.462(2) . ? 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 N18 Zr1 N15 97.67(6) . . ? N18 Zr1 N8 115.79(6) . . ? N15 Zr1 N8 88.74(5) . . ? N18 Zr1 N1 157.25(5) . . ? N15 Zr1 N1 93.69(6) . . ? N8 Zr1 N1 83.99(5) . . ? N18 Zr1 N7 88.73(5) . . ? N15 Zr1 N7 97.23(5) . . ? N8 Zr1 N7 153.85(5) . . ? N1 Zr1 N7 70.27(5) . . ? N18 Zr1 N14 93.87(5) . . ? N15 Zr1 N14 158.65(5) . . ? N8 Zr1 N14 70.05(5) . . ? N1 Zr1 N14 82.08(5) . . ? N7 Zr1 N14 100.94(4) . . ? C2 N1 C5 106.03(14) . . ? C2 N1 Zr1 135.04(12) . . ? C5 N1 Zr1 118.71(11) . . ? N1 C2 C3 110.72(16) . . ? C4 C3 C2 106.88(15) . . ? C3 C4 C5 106.14(16) . . ? N1 C5 C4 110.22(15) . . ? N1 C5 C6 116.85(14) . . ? C4 C5 C6 132.80(16) . . ? N7 C6 C5 120.83(15) . . ? C6 N7 C71 113.74(13) . . ? C6 N7 Zr1 113.33(10) . . ? C71 N7 Zr1 132.92(10) . . ? C76 C71 C72 121.25(16) . . ? C76 C71 N7 119.18(15) . . ? C72 C71 N7 119.54(15) . . ? C73 C72 C71 118.14(17) . . ? C73 C72 C77 119.99(17) . . ? C71 C72 C77 121.83(16) . . ? C74 C73 C72 121.19(18) . . ? C75 C74 C73 119.79(18) . . ? C74 C75 C76 121.40(19) . . ? C75 C76 C71 118.20(17) . . ? C75 C76 C80 118.59(17) . . ? C71 C76 C80 123.16(15) . . ? C72 C77 C79 112.31(19) . . ? C72 C77 C78 110.78(17) . . ? C79 C77 C78 109.9(2) . . ? C76 C80 C82 110.85(18) . . ? C76 C80 C81 112.05(16) . . ? C82 C80 C81 110.02(18) . . ? C9 N8 C12 105.65(14) . . ? C9 N8 Zr1 134.34(12) . . ? C12 N8 Zr1 119.55(11) . . ? N8 C9 C10 111.18(16) . . ? C9 C10 C11 106.60(16) . . ? C12 C11 C10 106.11(16) . . ? N8 C12 C11 110.47(15) . . ? N8 C12 C13 118.21(14) . . ? C11 C12 C13 131.30(16) . . ? N14 C13 C12 121.90(15) . . ? C13 N14 C141 113.60(14) . . ? C13 N14 Zr1 110.11(11) . . ? C141 N14 Zr1 136.27(10) . . ? C142 C141 C146 121.49(16) . . ? C142 C141 N14 119.71(15) . . ? C146 C141 N14 118.71(15) . . ? C143 C142 C141 117.85(16) . . ? C143 C142 C147 119.76(16) . . ? C141 C142 C147 122.16(15) . . ? C144 C143 C142 121.45(17) . . ? C143 C144 C145 119.95(17) . . ? C144 C145 C146 121.07(18) . . ? C145 C146 C141 118.13(17) . . ? C145 C146 C150 119.55(17) . . ? C141 C146 C150 122.28(16) . . ? C142 C147 C148 109.45(16) . . ? C142 C147 C149 113.89(15) . . ? C148 C147 C149 109.66(16) . . ? C146 C150 C152 111.13(17) . . ? C146 C150 C151 112.62(17) . . ? C152 C150 C151 109.68(18) . . ? C16 N15 C17 108.71(15) . . ? C16 N15 Zr1 124.85(12) . . ? C17 N15 Zr1 126.36(12) . . ? C19 N18 C20 109.75(14) . . ? C19 N18 Zr1 147.26(12) . . ? C20 N18 Zr1 102.77(11) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.696 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.072 #===END data_MB49 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H56 N6 Zr' _chemical_formula_weight 664.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.54770(10) _cell_length_b 16.45630(10) _cell_length_c 18.05230(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.5360(4) _cell_angle_gamma 90.00 _cell_volume 3792.98(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.65 _exptl_crystal_size_min 0.55 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.320 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8189 _exptl_absorpt_correction_T_max 0.8436 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree phi range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14177 _diffrn_reflns_av_R_equivalents 0.0120 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7244 _reflns_number_gt 6919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.0269P)^2^+1.6216P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7244 _refine_ls_number_parameters 402 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0632 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.196564(8) 0.237621(7) 0.095357(6) 0.02141(5) Uani 1 1 d . . . N1 N 0.32148(8) 0.33745(6) 0.14679(6) 0.0239(2) Uani 1 1 d . . . C2 C 0.41155(10) 0.31487(8) 0.19793(7) 0.0255(2) Uani 1 1 d . . . H2 H 0.4655 0.3536 0.2195 0.031 Uiso 1 1 calc R . . C3 C 0.42746(10) 0.23203(7) 0.22070(8) 0.0257(3) Uani 1 1 d . . . N4 N 0.34693(8) 0.17837(6) 0.18537(6) 0.0241(2) Uani 1 1 d . . . C5 C 0.38295(9) 0.10362(7) 0.21535(7) 0.0235(2) Uani 1 1 d . . . C6 C 0.48527(10) 0.10916(8) 0.27006(7) 0.0280(3) Uani 1 1 d . . . H6 H 0.5265 0.0657 0.2991 0.034 Uiso 1 1 calc R . . C7 C 0.51396(10) 0.19042(8) 0.27328(8) 0.0297(3) Uani 1 1 d . . . H7 H 0.5788 0.2135 0.3046 0.036 Uiso 1 1 calc R . . C8 C 0.31979(9) 0.03102(7) 0.18741(7) 0.0243(2) Uani 1 1 d . . . H8 H 0.2516 0.0371 0.1499 0.029 Uiso 1 1 calc R . . N9 N 0.35217(8) -0.04059(6) 0.21118(6) 0.0253(2) Uani 1 1 d . . . C10 C 0.30832(9) 0.42130(7) 0.12082(7) 0.0229(2) Uani 1 1 d . . . C11 C 0.33001(9) 0.44201(8) 0.05209(7) 0.0256(2) Uani 1 1 d . . . C12 C 0.31410(10) 0.52271(8) 0.02637(8) 0.0294(3) Uani 1 1 d . . . H12 H 0.3289 0.5383 -0.0195 0.035 Uiso 1 1 calc R . . C13 C 0.27701(10) 0.58034(8) 0.06676(8) 0.0285(3) Uani 1 1 d . . . H13 H 0.2673 0.6349 0.0487 0.034 Uiso 1 1 calc R . . C14 C 0.25420(10) 0.55844(8) 0.13330(8) 0.0277(3) Uani 1 1 d . . . H14 H 0.2281 0.5982 0.1601 0.033 Uiso 1 1 calc R . . C15 C 0.26895(10) 0.47863(8) 0.16178(7) 0.0257(2) Uani 1 1 d . . . C16 C 0.36972(11) 0.37829(8) 0.00734(8) 0.0333(3) Uani 1 1 d . . . H16 H 0.3347 0.3257 0.0112 0.040 Uiso 1 1 calc R . . C17 C 0.34371(15) 0.39737(11) -0.08080(9) 0.0471(4) Uani 1 1 d . . . H17A H 0.3856 0.4438 -0.0869 0.071 Uiso 1 1 calc R . . H17B H 0.2691 0.4105 -0.1040 0.071 Uiso 1 1 calc R . . H17C H 0.3599 0.3499 -0.1075 0.071 Uiso 1 1 calc R . . C18 C 0.48803(13) 0.36521(11) 0.04510(11) 0.0495(4) Uani 1 1 d . . . H18A H 0.5245 0.4171 0.0472 0.074 Uiso 1 1 calc R . . H18B H 0.5119 0.3262 0.0137 0.074 Uiso 1 1 calc R . . H18C H 0.5033 0.3440 0.0985 0.074 Uiso 1 1 calc R . . C19 C 0.24820(13) 0.45566(9) 0.23697(8) 0.0381(3) Uani 1 1 d . . . H19 H 0.2288 0.3968 0.2333 0.046 Uiso 1 1 calc R . . C20 C 0.15831(14) 0.50383(11) 0.25029(10) 0.0492(4) Uani 1 1 d . . . H20A H 0.1796 0.5606 0.2619 0.074 Uiso 1 1 calc R . . H20B H 0.1417 0.4803 0.2946 0.074 Uiso 1 1 calc R . . H20C H 0.0963 0.5013 0.2028 0.074 Uiso 1 1 calc R . . C21 C 0.34891(16) 0.46624(13) 0.30793(9) 0.0580(5) Uani 1 1 d . . . H21A H 0.4062 0.4363 0.2986 0.087 Uiso 1 1 calc R . . H21B H 0.3377 0.4451 0.3553 0.087 Uiso 1 1 calc R . . H21C H 0.3670 0.5240 0.3151 0.087 Uiso 1 1 calc R . . C22 C 0.28519(9) -0.10714(7) 0.17507(7) 0.0241(2) Uani 1 1 d . . . C23 C 0.22667(10) -0.14606(8) 0.21657(8) 0.0273(3) Uani 1 1 d . . . C24 C 0.16071(11) -0.21027(8) 0.18006(8) 0.0331(3) Uani 1 1 d . . . H24 H 0.1201 -0.2364 0.2070 0.040 Uiso 1 1 calc R . . C25 C 0.15335(11) -0.23656(8) 0.10535(9) 0.0345(3) Uani 1 1 d . . . H25 H 0.1065 -0.2791 0.0808 0.041 Uiso 1 1 calc R . . C26 C 0.21489(11) -0.20021(8) 0.06682(8) 0.0321(3) Uani 1 1 d . . . H26 H 0.2114 -0.2196 0.0164 0.038 Uiso 1 1 calc R . . C27 C 0.28204(10) -0.13562(8) 0.10048(8) 0.0278(3) Uani 1 1 d . . . C28 C 0.23115(12) -0.11655(9) 0.29774(8) 0.0362(3) Uani 1 1 d . . . H28 H 0.2960 -0.0830 0.3197 0.043 Uiso 1 1 calc R . . C29 C 0.23826(17) -0.18752(12) 0.35469(10) 0.0574(5) Uani 1 1 d . . . H29A H 0.1717 -0.2172 0.3385 0.086 Uiso 1 1 calc R . . H29B H 0.2529 -0.1663 0.4080 0.086 Uiso 1 1 calc R . . H29C H 0.2947 -0.2243 0.3538 0.086 Uiso 1 1 calc R . . C30 C 0.13739(15) -0.06199(13) 0.29141(12) 0.0612(5) Uani 1 1 d . . . H30A H 0.1377 -0.0152 0.2579 0.092 Uiso 1 1 calc R . . H30B H 0.1420 -0.0429 0.3439 0.092 Uiso 1 1 calc R . . H30C H 0.0724 -0.0928 0.2684 0.092 Uiso 1 1 calc R . . C31 C 0.34992(12) -0.09977(9) 0.05600(9) 0.0369(3) Uani 1 1 d . . . H31 H 0.3863 -0.0504 0.0848 0.044 Uiso 1 1 calc R . . C32 C 0.43290(14) -0.16095(12) 0.05154(12) 0.0552(4) Uani 1 1 d . . . H32A H 0.4783 -0.1749 0.1048 0.083 Uiso 1 1 calc R . . H32B H 0.4751 -0.1370 0.0224 0.083 Uiso 1 1 calc R . . H32C H 0.3984 -0.2102 0.0246 0.083 Uiso 1 1 calc R . . C33 C 0.28296(19) -0.07464(16) -0.02755(13) 0.0747(6) Uani 1 1 d . . . H33A H 0.3275 -0.0484 -0.0536 0.112 Uiso 1 1 calc R . . H33B H 0.2286 -0.0365 -0.0250 0.112 Uiso 1 1 calc R . . H33C H 0.2500 -0.1229 -0.0574 0.112 Uiso 1 1 calc R . . N5 N 0.10339(9) 0.18930(8) 0.15264(7) 0.0345(3) Uani 1 1 d . . . C34 C 0.12922(15) 0.20271(14) 0.23668(10) 0.0563(5) Uani 1 1 d . . . H34A H 0.0740 0.2351 0.2462 0.084 Uiso 1 1 calc R . . H34B H 0.1960 0.2318 0.2570 0.084 Uiso 1 1 calc R . . H34C H 0.1351 0.1503 0.2635 0.084 Uiso 1 1 calc R . . C35 C 0.00508(14) 0.14597(14) 0.11939(12) 0.0609(5) Uani 1 1 d . . . H35A H 0.0105 0.0925 0.1444 0.091 Uiso 1 1 calc R . . H35B H -0.0102 0.1391 0.0627 0.091 Uiso 1 1 calc R . . H35C H -0.0514 0.1771 0.1286 0.091 Uiso 1 1 calc R . . N6 N 0.20554(9) 0.17367(7) 0.00107(7) 0.0350(3) Uani 1 1 d . . . C36 C 0.30661(14) 0.15842(11) -0.00899(11) 0.0482(4) Uani 1 1 d . . . H36A H 0.3163 0.0998 -0.0132 0.072 Uiso 1 1 calc R . . H36B H 0.3629 0.1799 0.0364 0.072 Uiso 1 1 calc R . . H36C H 0.3084 0.1853 -0.0570 0.072 Uiso 1 1 calc R . . C37 C 0.11758(15) 0.14498(13) -0.06606(10) 0.0592(5) Uani 1 1 d . . . H37A H 0.1197 0.1714 -0.1141 0.089 Uiso 1 1 calc R . . H37B H 0.0515 0.1584 -0.0578 0.089 Uiso 1 1 calc R . . H37C H 0.1227 0.0860 -0.0711 0.089 Uiso 1 1 calc R . . N7 N 0.09025(9) 0.32573(7) 0.03206(7) 0.0326(2) Uani 1 1 d . . . C38 C 0.02369(13) 0.37241(11) 0.06512(11) 0.0517(4) Uani 1 1 d . . . H38A H 0.0513 0.4278 0.0767 0.078 Uiso 1 1 calc R . . H38B H 0.0226 0.3465 0.1137 0.078 Uiso 1 1 calc R . . H38C H -0.0476 0.3745 0.0272 0.078 Uiso 1 1 calc R . . C39 C 0.09009(12) 0.36354(10) -0.04144(11) 0.0497(4) Uani 1 1 d . . . H39A H 0.0180 0.3673 -0.0778 0.075 Uiso 1 1 calc R . . H39B H 0.1318 0.3305 -0.0652 0.075 Uiso 1 1 calc R . . H39C H 0.1204 0.4181 -0.0305 0.075 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 Zr1 0.01984(7) 0.01974(8) 0.02279(7) -0.00053(4) 0.00465(5) -0.00054(4) N1 0.0253(5) 0.0194(5) 0.0264(5) -0.0004(4) 0.0078(4) -0.0012(4) C2 0.0250(6) 0.0230(6) 0.0273(6) -0.0031(5) 0.0073(5) -0.0028(5) C3 0.0240(6) 0.0238(6) 0.0271(6) -0.0036(5) 0.0056(5) -0.0037(5) N4 0.0226(5) 0.0204(5) 0.0270(5) -0.0009(4) 0.0052(4) -0.0005(4) C5 0.0247(6) 0.0209(6) 0.0249(6) -0.0009(5) 0.0083(5) 0.0006(5) C6 0.0265(6) 0.0235(6) 0.0292(6) 0.0004(5) 0.0032(5) 0.0020(5) C7 0.0246(6) 0.0259(6) 0.0322(6) -0.0028(5) 0.0011(5) -0.0010(5) C8 0.0224(6) 0.0233(6) 0.0254(6) -0.0007(5) 0.0058(5) 0.0001(5) N9 0.0255(5) 0.0217(5) 0.0268(5) 0.0001(4) 0.0064(4) -0.0012(4) C10 0.0210(5) 0.0206(6) 0.0250(6) -0.0006(5) 0.0047(4) -0.0029(4) C11 0.0243(6) 0.0241(6) 0.0290(6) -0.0017(5) 0.0099(5) -0.0031(5) C12 0.0329(7) 0.0285(6) 0.0285(6) 0.0031(5) 0.0125(5) -0.0042(5) C13 0.0302(6) 0.0217(6) 0.0311(6) 0.0040(5) 0.0068(5) 0.0000(5) C14 0.0298(6) 0.0227(6) 0.0302(6) -0.0016(5) 0.0096(5) 0.0016(5) C15 0.0274(6) 0.0241(6) 0.0248(6) -0.0008(5) 0.0079(5) -0.0021(5) C16 0.0402(7) 0.0277(7) 0.0389(7) -0.0041(6) 0.0225(6) -0.0040(6) C17 0.0649(10) 0.0457(9) 0.0401(8) -0.0089(7) 0.0301(8) -0.0049(8) C18 0.0433(9) 0.0532(10) 0.0621(10) -0.0019(8) 0.0310(8) 0.0080(7) C19 0.0603(9) 0.0272(7) 0.0351(7) 0.0004(6) 0.0271(7) -0.0002(6) C20 0.0592(10) 0.0520(10) 0.0493(9) -0.0064(8) 0.0354(8) -0.0047(8) C21 0.0786(13) 0.0707(12) 0.0246(7) 0.0052(7) 0.0171(8) 0.0275(10) C22 0.0219(5) 0.0184(5) 0.0285(6) 0.0009(5) 0.0038(5) 0.0021(4) C23 0.0256(6) 0.0248(6) 0.0306(6) -0.0004(5) 0.0080(5) 0.0003(5) C24 0.0311(7) 0.0289(7) 0.0410(7) -0.0018(6) 0.0143(6) -0.0060(5) C25 0.0330(7) 0.0250(7) 0.0424(8) -0.0059(5) 0.0085(6) -0.0065(5) C26 0.0388(7) 0.0252(6) 0.0303(6) -0.0046(5) 0.0091(6) -0.0002(5) C27 0.0311(6) 0.0210(6) 0.0306(6) 0.0009(5) 0.0093(5) 0.0008(5) C28 0.0401(7) 0.0372(7) 0.0339(7) -0.0056(6) 0.0158(6) -0.0106(6) C29 0.0800(13) 0.0562(11) 0.0368(8) -0.0013(8) 0.0207(8) -0.0278(10) C30 0.0570(11) 0.0706(13) 0.0629(11) -0.0224(10) 0.0292(9) 0.0041(9) C31 0.0490(8) 0.0311(7) 0.0357(7) -0.0030(6) 0.0208(6) -0.0080(6) C32 0.0523(10) 0.0586(11) 0.0661(11) -0.0002(9) 0.0349(9) -0.0005(8) C33 0.0793(14) 0.0835(15) 0.0602(12) 0.0373(11) 0.0219(11) -0.0037(12) N5 0.0273(5) 0.0420(7) 0.0334(6) 0.0082(5) 0.0093(5) -0.0007(5) C34 0.0530(10) 0.0790(13) 0.0404(9) 0.0049(9) 0.0203(8) 0.0006(9) C35 0.0367(8) 0.0822(14) 0.0600(11) 0.0096(10) 0.0114(8) -0.0174(9) N6 0.0361(6) 0.0365(6) 0.0305(6) -0.0064(5) 0.0085(5) 0.0048(5) C36 0.0515(9) 0.0474(9) 0.0528(9) -0.0111(8) 0.0270(8) 0.0046(7) C37 0.0543(10) 0.0687(12) 0.0409(9) -0.0203(8) -0.0022(8) 0.0098(9) N7 0.0249(5) 0.0259(5) 0.0398(6) 0.0018(5) 0.0014(5) 0.0002(4) C38 0.0422(9) 0.0418(9) 0.0563(10) -0.0137(8) -0.0032(7) 0.0160(7) C39 0.0333(7) 0.0450(9) 0.0605(10) 0.0249(8) 0.0019(7) -0.0058(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 Zr1 N6 2.0391(11) . ? Zr1 N5 2.0417(11) . ? Zr1 N7 2.0933(11) . ? Zr1 N1 2.3182(10) . ? Zr1 N4 2.3510(10) . ? N1 C2 1.3137(16) . ? N1 C10 1.4491(15) . ? C2 C3 1.4194(18) . ? C3 N4 1.3825(15) . ? C3 C7 1.4140(18) . ? N4 C5 1.3667(15) . ? C5 C6 1.4105(17) . ? C5 C8 1.4579(17) . ? C6 C7 1.3884(18) . ? C8 N9 1.2803(16) . ? N9 C22 1.4326(15) . ? C10 C15 1.4089(17) . ? C10 C11 1.4091(17) . ? C11 C12 1.3994(18) . ? C11 C16 1.5273(18) . ? C12 C13 1.3888(19) . ? C13 C14 1.3844(18) . ? C14 C15 1.4001(18) . ? C15 C19 1.5230(18) . ? C16 C18 1.533(2) . ? C16 C17 1.542(2) . ? C19 C21 1.538(2) . ? C19 C20 1.538(2) . ? C22 C27 1.4129(18) . ? C22 C23 1.4133(18) . ? C23 C24 1.3985(18) . ? C23 C28 1.5254(18) . ? C24 C25 1.388(2) . ? C25 C26 1.387(2) . ? C26 C27 1.3989(18) . ? C27 C31 1.5272(19) . ? C28 C30 1.528(2) . ? C28 C29 1.538(2) . ? C31 C32 1.531(2) . ? C31 C33 1.534(2) . ? N5 C35 1.452(2) . ? N5 C34 1.455(2) . ? N6 C36 1.4619(19) . ? N6 C37 1.465(2) . ? N7 C38 1.456(2) . ? N7 C39 1.465(2) . ? 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 N6 Zr1 N5 116.19(5) . . ? N6 Zr1 N7 97.13(5) . . ? N5 Zr1 N7 96.73(5) . . ? N6 Zr1 N1 117.44(4) . . ? N5 Zr1 N1 124.43(4) . . ? N7 Zr1 N1 90.27(4) . . ? N6 Zr1 N4 94.77(4) . . ? N5 Zr1 N4 91.60(4) . . ? N7 Zr1 N4 160.66(4) . . ? N1 Zr1 N4 70.69(4) . . ? C2 N1 C10 118.78(10) . . ? C2 N1 Zr1 117.59(8) . . ? C10 N1 Zr1 123.43(7) . . ? N1 C2 C3 119.38(11) . . ? N4 C3 C7 110.46(11) . . ? N4 C3 C2 117.38(11) . . ? C7 C3 C2 132.15(12) . . ? C5 N4 C3 105.66(10) . . ? C5 N4 Zr1 139.39(8) . . ? C3 N4 Zr1 114.94(8) . . ? N4 C5 C6 110.87(10) . . ? N4 C5 C8 120.67(10) . . ? C6 C5 C8 128.38(11) . . ? C7 C6 C5 106.71(11) . . ? C6 C7 C3 106.30(11) . . ? N9 C8 C5 122.86(11) . . ? C8 N9 C22 117.21(10) . . ? C15 C10 C11 121.81(11) . . ? C15 C10 N1 119.67(11) . . ? C11 C10 N1 118.42(11) . . ? C12 C11 C10 117.86(11) . . ? C12 C11 C16 121.22(11) . . ? C10 C11 C16 120.91(11) . . ? C13 C12 C11 121.09(12) . . ? C14 C13 C12 120.18(12) . . ? C13 C14 C15 121.13(12) . . ? C14 C15 C10 117.91(11) . . ? C14 C15 C19 120.92(11) . . ? C10 C15 C19 121.10(11) . . ? C11 C16 C18 111.23(12) . . ? C11 C16 C17 113.99(12) . . ? C18 C16 C17 109.36(13) . . ? C15 C19 C21 109.73(13) . . ? C15 C19 C20 113.78(12) . . ? C21 C19 C20 109.86(13) . . ? C27 C22 C23 120.76(11) . . ? C27 C22 N9 120.00(11) . . ? C23 C22 N9 119.17(11) . . ? C24 C23 C22 118.41(12) . . ? C24 C23 C28 120.47(12) . . ? C22 C23 C28 121.05(11) . . ? C25 C24 C23 121.36(13) . . ? C26 C25 C24 119.53(12) . . ? C25 C26 C27 121.50(13) . . ? C26 C27 C22 118.29(12) . . ? C26 C27 C31 118.93(12) . . ? C22 C27 C31 122.78(11) . . ? C23 C28 C30 110.49(13) . . ? C23 C28 C29 111.96(13) . . ? C30 C28 C29 111.16(15) . . ? C27 C31 C32 110.82(12) . . ? C27 C31 C33 111.04(14) . . ? C32 C31 C33 109.19(16) . . ? C35 N5 C34 111.90(13) . . ? C35 N5 Zr1 128.24(11) . . ? C34 N5 Zr1 119.68(10) . . ? C36 N6 C37 112.24(13) . . ? C36 N6 Zr1 120.81(10) . . ? C37 N6 Zr1 126.71(11) . . ? C38 N7 C39 109.49(13) . . ? C38 N7 Zr1 123.31(10) . . ? C39 N7 Zr1 125.53(10) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.250 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.036