# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1783 data_tacnzrcl3 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Jul 4 10:40:25 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 7.517(1) _cell_length_b 10.144(1) _cell_length_c 22.790(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1738.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_meas ? _chemical_formula_weight 409.94 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H26 Cl3 N3 Zr ' _chemical_formula_moiety 'C12 H26 Cl3 N3 Zr ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 840.00 _exptl_absorpt_coefficient_mu 1.085 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'SMART CCD' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 7804 _reflns_number_total 2947 _reflns_number_observed 1735 _reflns_observed_criterion 'I>3.00 sigma' _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.59 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 48 0.003 0.002 'International Tables' H 0 104 0.000 0.000 'International Tables' N 0 12 0.006 0.003 'International Tables' Zr 0 4 -2.967 0.560 'International Tables' Cl 0 12 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Zr(1) 1.01657(8) 0.06806(6) 0.64383(3) 0.025 Uij ? ? Cl(1) 0.8711(2) 0.1709(2) 0.55757(8) 0.026 Uij ? ? Cl(2) 0.7822(2) 0.1351(2) 0.71219(8) 0.024 Uij ? ? Cl(3) 0.8963(2) -0.1509(2) 0.62634(8) 0.025 Uij ? ? N(1) 1.1929(6) 0.0552(5) 0.7094(2) 0.016 Uij ? ? N(2) 1.2897(7) -0.0226(5) 0.6031(3) 0.020 Uij ? ? N(3) 1.2086(6) 0.2672(5) 0.6379(3) 0.021 Uij ? ? C(1) 1.2270(9) 0.1821(7) 0.7400(3) 0.021 Uij ? ? C(2) 1.3050(9) 0.2798(7) 0.6957(3) 0.018 Uij ? ? C(3) 1.3329(9) 0.2240(7) 0.5903(3) 0.021 Uij ? ? C(4) 1.4200(8) 0.0897(7) 0.5981(3) 0.024 Uij ? ? C(5) 1.3457(8) -0.1111(6) 0.6528(4) 0.021 Uij ? ? C(6) 1.3391(9) -0.0372(7) 0.7107(3) 0.023 Uij ? ? C(7) 1.1302(9) 0.3990(6) 0.6190(3) 0.025 Uij ? ? C(8) 0.9780(9) 0.4392(7) 0.6591(3) 0.031 Uij ? ? C(9) 1.265(1) 0.5099(7) 0.6125(4) 0.040 Uij ? ? C(10) 1.2857(9) -0.1031(6) 0.5472(3) 0.021 Uij ? ? C(11) 1.226(1) -0.0230(7) 0.4951(3) 0.028 Uij ? ? C(12) 1.4571(10) -0.1737(7) 0.5321(4) 0.039 Uij ? ? H(1) 1.119 0.216 0.755 0.025 Uij ? ? H(2) 1.309 0.169 0.771 0.025 Uij ? ? H(3) 1.292 0.367 0.710 0.022 Uij ? ? H(4) 1.428 0.261 0.690 0.022 Uij ? ? H(5) 1.268 0.222 0.555 0.025 Uij ? ? H(6) 1.425 0.288 0.587 0.025 Uij ? ? H(7) 1.495 0.074 0.565 0.029 Uij ? ? H(8) 1.490 0.092 0.633 0.029 Uij ? ? H(9) 1.267 -0.185 0.655 0.025 Uij ? ? H(10) 1.464 -0.141 0.646 0.025 Uij ? ? H(11) 1.322 -0.098 0.742 0.028 Uij ? ? H(12) 1.448 0.009 0.716 0.028 Uij ? ? H(13) 1.080 0.386 0.581 0.029 Uij ? ? H(14) 0.886 0.376 0.657 0.037 Uij ? ? H(15) 0.934 0.523 0.647 0.037 Uij ? ? H(16) 1.020 0.445 0.698 0.037 Uij ? ? H(17) 1.215 0.578 0.589 0.048 Uij ? ? H(18) 1.294 0.543 0.650 0.048 Uij ? ? H(19) 1.369 0.477 0.594 0.048 Uij ? ? H(20) 1.199 -0.170 0.553 0.026 Uij ? ? H(21) 1.177 -0.080 0.466 0.034 Uij ? ? H(22) 1.137 0.038 0.507 0.034 Uij ? ? H(23) 1.324 0.023 0.479 0.034 Uij ? ? H(24) 1.548 -0.111 0.526 0.046 Uij ? ? H(25) 1.490 -0.230 0.564 0.046 Uij ? ? H(26) 1.440 -0.225 0.498 0.046 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zr(1) 0.0192(3) 0.0211(3) 0.0151(3) -0.0021(3) 0.0000(4) 0.0020(4) Cl(1) 0.033(1) 0.039(1) 0.022(1) -0.0015(9) -0.0083(9) 0.0076(9) Cl(2) 0.0264(10) 0.039(1) 0.023(1) 0.0020(9) 0.0053(9) -0.001(1) Cl(3) 0.0321(10) 0.029(1) 0.034(1) -0.0099(8) 0.0017(9) 0.0007(9) N(1) 0.021(3) 0.014(3) 0.025(4) 0.002(3) 0.000(3) 0.000(3) N(2) 0.030(3) 0.017(4) 0.023(4) -0.004(3) -0.002(3) -0.004(3) N(3) 0.028(3) 0.022(3) 0.012(3) -0.004(2) -0.006(3) -0.003(3) C(1) 0.027(4) 0.037(5) 0.027(5) -0.007(4) -0.010(4) 0.000(4) C(2) 0.036(5) 0.022(4) 0.020(5) -0.005(3) -0.002(4) -0.007(3) C(3) 0.027(4) 0.024(4) 0.019(5) -0.005(3) 0.005(4) 0.002(3) C(4) 0.023(4) 0.030(5) 0.024(4) -0.005(3) 0.005(3) -0.002(4) C(5) 0.027(4) 0.025(4) 0.033(5) 0.008(3) -0.004(4) 0.006(4) C(6) 0.028(4) 0.037(5) 0.020(5) -0.004(3) 0.000(4) 0.008(4) C(7) 0.036(4) 0.016(4) 0.022(4) 0.003(3) -0.002(3) 0.008(3) C(8) 0.046(4) 0.026(3) 0.030(4) 0.012(4) -0.002(4) 0.000(3) C(9) 0.059(5) 0.017(4) 0.054(6) -0.008(4) 0.004(5) 0.003(4) C(10) 0.032(4) 0.022(4) 0.032(5) -0.001(3) 0.001(4) -0.005(3) C(11) 0.044(5) 0.035(5) 0.027(5) -0.008(4) 0.007(4) -0.013(4) C(12) 0.042(5) 0.037(5) 0.053(6) 0.003(4) 0.007(4) -0.019(4) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1735 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_obs 0.0311 _refine_ls_wR_factor_all 0.0397 _refine_ls_wR_factor_obs 0.0316 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 0.760 _refine_ls_shift/esd_max 0.0310 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.52 _refine_diff_density_max 0.66 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr(1) Cl(1) 2.480(2) ? ? yes Zr(1) Cl(2) 2.449(2) ? ? yes Zr(1) Cl(3) 2.431(2) ? ? yes Zr(1) N(1) 2.003(5) ? ? yes Zr(1) N(2) 2.434(5) ? ? yes Zr(1) N(3) 2.487(5) ? ? yes N(1) C(1) 1.486(9) ? ? yes N(1) C(6) 1.444(8) ? ? yes N(2) C(4) 1.506(7) ? ? yes N(2) C(5) 1.505(9) ? ? yes N(2) C(10) 1.513(9) ? ? yes N(3) C(2) 1.508(9) ? ? yes N(3) C(3) 1.498(9) ? ? yes N(3) C(7) 1.523(7) ? ? yes C(1) C(2) 1.532(10) ? ? yes C(3) C(4) 1.522(9) ? ? yes C(5) C(6) 1.52(1) ? ? yes C(7) C(8) 1.520(9) ? ? yes C(7) C(9) 1.521(9) ? ? yes C(10) C(11) 1.51(1) ? ? yes C(10) C(12) 1.514(9) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Zr(1) Cl(2) 94.02(7) ? ? ? yes Cl(1) Zr(1) Cl(3) 95.19(6) ? ? ? yes Cl(1) Zr(1) N(1) 155.7(2) ? ? ? yes Cl(1) Zr(1) N(2) 103.2(1) ? ? ? yes Cl(1) Zr(1) N(3) 82.6(1) ? ? ? yes Cl(2) Zr(1) Cl(3) 95.20(6) ? ? ? yes Cl(2) Zr(1) N(1) 91.1(2) ? ? ? yes Cl(2) Zr(1) N(2) 162.7(1) ? ? ? yes Cl(2) Zr(1) N(3) 103.1(1) ? ? ? yes Cl(3) Zr(1) N(1) 108.0(2) ? ? ? yes Cl(3) Zr(1) N(2) 84.6(1) ? ? ? yes Cl(3) Zr(1) N(3) 161.7(1) ? ? ? yes N(1) Zr(1) N(2) 72.7(2) ? ? ? yes N(1) Zr(1) N(3) 73.1(2) ? ? ? yes N(2) Zr(1) N(3) 78.3(2) ? ? ? yes Zr(1) N(1) C(1) 114.0(4) ? ? ? yes Zr(1) N(1) C(6) 124.1(5) ? ? ? yes C(1) N(1) C(6) 114.9(5) ? ? ? yes Zr(1) N(2) C(4) 106.9(4) ? ? ? yes Zr(1) N(2) C(5) 100.0(4) ? ? ? yes Zr(1) N(2) C(10) 120.6(4) ? ? ? yes C(4) N(2) C(5) 109.0(5) ? ? ? yes C(4) N(2) C(10) 111.0(5) ? ? ? yes C(5) N(2) C(10) 108.5(5) ? ? ? yes Zr(1) N(3) C(2) 107.5(4) ? ? ? yes Zr(1) N(3) C(3) 99.4(4) ? ? ? yes Zr(1) N(3) C(7) 120.3(4) ? ? ? yes C(2) N(3) C(3) 110.9(5) ? ? ? yes C(2) N(3) C(7) 111.0(5) ? ? ? yes C(3) N(3) C(7) 107.1(5) ? ? ? yes N(1) C(1) C(2) 108.5(6) ? ? ? yes N(3) C(2) C(1) 109.7(5) ? ? ? yes N(3) C(3) C(4) 116.4(6) ? ? ? yes N(2) C(4) C(3) 113.9(5) ? ? ? yes N(2) C(5) C(6) 110.5(5) ? ? ? yes N(1) C(6) C(5) 109.1(6) ? ? ? yes N(3) C(7) C(8) 110.9(5) ? ? ? yes N(3) C(7) C(9) 114.8(6) ? ? ? yes C(8) C(7) C(9) 111.2(6) ? ? ? yes N(2) C(10) C(11) 112.2(5) ? ? ? yes N(2) C(10) C(12) 115.4(6) ? ? ? yes C(11) C(10) C(12) 109.4(6) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' Chemical Communications' _publ_contact_author ; John Arnold Dept of Chemistry, UC Berkeley, Berkeley, CA 94720-1460 ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 510 643 5181 ' _publ_contact_author_fax ' 510 643 5482 ' _publ_contact_author_email ' arnold@socrates.berkeley.edu ' loop_ _publ_author_name _publ_author_address ' Garth R. Giesbrecht ' ; Dept of Chemistry, UC Berkeley, Berkeley, CA 94720-1460 ; _publ_section_title ; Zirconium tacn Complexes ; _publ_section_abstract ; Zirconium tacn Complexes ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END data_tacn_zirconium_tribenzyl #------------------------------------------------------------------------------ _audit_creation_date 'Tue Jul 4 11:19:35 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 39.6517(3) _cell_length_b 39.6517(3) _cell_length_c 9.74690(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 13271.5(2) _cell_formula_units_Z 18 _cell_measurement_temperature 173 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3 ' _symmetry_Int_Tables_number 148 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '2/3+x,1/3+y,1/3+z' '1/3+x,2/3+y,2/3+z' ' -y, +x-y, +z' '2/3-y,1/3+x-y,1/3+z' '1/3-y,2/3+x-y,2/3+z' ' -x+y, -x, +z' '2/3-x+y,1/3-x,1/3+z' '1/3-x+y,2/3-x,2/3+z' ' -x, -y, -z' '2/3-x,1/3-y,1/3-z' '1/3-x,2/3-y,2/3-z' ' +y, -x+y, -z' '2/3+y,1/3-x+y,1/3-z' '1/3+y,2/3-x+y,2/3-z' ' +x-y, +x, -z' '2/3+x-y,1/3+x,1/3-z' '1/3+x-y,2/3+x,2/3-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_meas ? _chemical_formula_weight 576.97 _chemical_formula_analytical ? _chemical_formula_sum 'C33 H47 N3 Zr ' _chemical_formula_moiety 'C33 H47 N3 Zr ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 5508.00 _exptl_absorpt_coefficient_mu 0.398 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'SMART CCD' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 20082 _reflns_number_total 5097 _reflns_number_observed 3539 _reflns_observed_criterion 'I>3.00 sigma' _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.67 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 594 0.003 0.002 'International Tables' H 0 846 0.000 0.000 'International Tables' N 0 54 0.006 0.003 'International Tables' Zr 0 18 -2.967 0.560 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Zr(1) 0.812497(6) 0.004209(6) 1.12621(2) 0.025 Uij ? ? N(1) 0.76096(6) -0.02636(6) 1.0172(2) 0.023 Uij ? ? N(2) 0.82568(5) 0.01841(5) 0.8650(2) 0.018 Uij ? ? N(3) 0.79096(5) 0.05164(5) 1.0643(2) 0.018 Uij ? ? C(1) 0.88059(7) 0.04230(7) 1.1387(2) 0.022 Uij ? ? C(2) 0.90141(7) 0.02298(7) 1.1967(3) 0.022 Uij ? ? C(3) 0.92393(7) 0.01256(8) 1.1159(3) 0.028 Uij ? ? C(4) 0.94125(7) -0.00718(8) 1.1712(3) 0.032 Uij ? ? C(5) 0.93687(8) -0.01750(8) 1.3076(3) 0.034 Uij ? ? C(6) 0.91514(8) -0.00706(9) 1.3898(3) 0.036 Uij ? ? C(7) 0.89818(8) 0.01302(8) 1.3343(3) 0.031 Uij ? ? C(8) 0.80885(7) -0.05497(7) 1.1743(3) 0.024 Uij ? ? C(9) 0.77859(8) -0.07887(7) 1.2768(3) 0.025 Uij ? ? C(10) 0.78784(8) -0.08068(8) 1.4137(3) 0.033 Uij ? ? C(11) 0.7595(1) -0.10209(9) 1.5097(3) 0.046 Uij ? ? C(12) 0.7208(1) -0.12219(9) 1.4736(4) 0.048 Uij ? ? C(13) 0.71060(8) -0.12047(8) 1.3395(3) 0.042 Uij ? ? C(14) 0.73896(8) -0.09902(7) 1.2416(3) 0.031 Uij ? ? C(15) 0.80653(7) 0.01864(7) 1.3506(2) 0.021 Uij ? ? C(16) 0.77359(7) 0.01602(7) 1.4327(2) 0.020 Uij ? ? C(17) 0.73899(7) -0.01910(7) 1.4487(3) 0.024 Uij ? ? C(18) 0.70819(7) -0.02170(8) 1.5239(3) 0.030 Uij ? ? C(19) 0.71055(8) 0.01089(8) 1.5849(3) 0.032 Uij ? ? C(20) 0.74455(8) 0.04604(7) 1.5708(3) 0.027 Uij ? ? C(21) 0.77561(7) 0.04870(7) 1.4970(2) 0.024 Uij ? ? C(22) 0.76342(7) -0.04335(7) 0.8872(3) 0.027 Uij ? ? C(23) 0.78996(7) -0.01106(7) 0.7887(3) 0.024 Uij ? ? C(24) 0.83059(7) 0.05799(7) 0.8519(2) 0.020 Uij ? ? C(25) 0.79770(7) 0.06179(7) 0.9156(3) 0.022 Uij ? ? C(26) 0.74842(7) 0.02526(8) 1.0930(3) 0.026 Uij ? ? C(27) 0.73268(7) -0.01307(8) 1.0155(3) 0.028 Uij ? ? C(28) 0.86145(7) 0.01883(7) 0.8099(2) 0.022 Uij ? ? C(29) 0.85992(8) -0.01946(7) 0.8402(3) 0.029 Uij ? ? C(30) 0.86947(8) 0.02849(8) 0.6584(3) 0.032 Uij ? ? C(31) 0.80652(8) 0.08728(7) 1.1547(3) 0.026 Uij ? ? C(32) 0.84916(8) 0.11503(7) 1.1270(3) 0.027 Uij ? ? C(33) 0.78350(8) 0.10862(8) 1.1478(3) 0.038 Uij ? ? H(1) 0.887 0.064 1.194 0.027 Uij ? ? H(2) 0.890 0.051 1.048 0.027 Uij ? ? H(3) 0.927 0.019 1.021 0.034 Uij ? ? H(4) 0.956 -0.014 1.112 0.038 Uij ? ? H(5) 0.949 -0.031 1.342 0.041 Uij ? ? H(6) 0.912 -0.014 1.485 0.043 Uij ? ? H(7) 0.884 0.020 1.393 0.037 Uij ? ? H(8) 0.833 -0.050 1.209 0.028 Uij ? ? H(9) 0.803 -0.069 1.092 0.028 Uij ? ? H(10) 0.814 -0.067 1.442 0.040 Uij ? ? H(11) 0.767 -0.103 1.602 0.055 Uij ? ? H(12) 0.701 -0.137 1.540 0.058 Uij ? ? H(13) 0.684 -0.134 1.314 0.050 Uij ? ? H(14) 0.731 -0.098 1.150 0.037 Uij ? ? H(15) 0.814 0.003 1.401 0.026 Uij ? ? H(16) 0.826 0.045 1.359 0.026 Uij ? ? H(17) 0.736 -0.042 1.407 0.029 Uij ? ? H(18) 0.685 -0.046 1.534 0.036 Uij ? ? H(19) 0.689 0.009 1.635 0.038 Uij ? ? H(20) 0.747 0.069 1.612 0.033 Uij ? ? H(21) 0.799 0.073 1.490 0.029 Uij ? ? H(22) 0.774 -0.060 0.903 0.032 Uij ? ? H(23) 0.738 -0.058 0.848 0.032 Uij ? ? H(24) 0.797 -0.022 0.716 0.029 Uij ? ? H(25) 0.777 0.001 0.753 0.029 Uij ? ? H(26) 0.832 0.064 0.757 0.024 Uij ? ? H(27) 0.854 0.076 0.896 0.024 Uij ? ? H(28) 0.774 0.045 0.867 0.027 Uij ? ? H(29) 0.804 0.088 0.905 0.027 Uij ? ? H(30) 0.735 0.038 1.065 0.032 Uij ? ? H(31) 0.745 0.020 1.189 0.032 Uij ? ? H(32) 0.709 -0.032 1.058 0.034 Uij ? ? H(33) 0.727 -0.009 0.923 0.034 Uij ? ? H(34) 0.883 0.039 0.859 0.027 Uij ? ? H(35) 0.858 -0.024 0.937 0.035 Uij ? ? H(36) 0.838 -0.040 0.797 0.035 Uij ? ? H(37) 0.883 -0.019 0.806 0.035 Uij ? ? H(38) 0.895 0.033 0.636 0.038 Uij ? ? H(39) 0.850 0.008 0.605 0.038 Uij ? ? H(40) 0.869 0.051 0.639 0.038 Uij ? ? H(41) 0.805 0.079 1.247 0.031 Uij ? ? H(42) 0.863 0.101 1.128 0.032 Uij ? ? H(43) 0.852 0.127 1.040 0.032 Uij ? ? H(44) 0.859 0.135 1.196 0.032 Uij ? ? H(45) 0.783 0.116 1.056 0.046 Uij ? ? H(46) 0.795 0.131 1.205 0.046 Uij ? ? H(47) 0.758 0.092 1.178 0.046 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zr(1) 0.0200(1) 0.0177(1) 0.0206(1) 0.0092(1) 0.0010(1) 0.0018(1) N(1) 0.020(1) 0.022(1) 0.031(1) 0.0065(10) -0.0009(9) 0.0032(9) N(2) 0.020(1) 0.018(1) 0.022(1) 0.0077(9) -0.0011(9) 0.0005(9) N(3) 0.022(1) 0.023(1) 0.024(1) 0.0123(9) 0.0022(9) 0.0043(9) C(1) 0.025(1) 0.035(2) 0.017(1) 0.012(1) -0.002(1) -0.004(1) C(2) 0.017(1) 0.029(1) 0.024(1) 0.007(1) -0.001(1) -0.003(1) C(3) 0.022(1) 0.040(2) 0.024(1) 0.010(1) 0.001(1) -0.006(1) C(4) 0.026(2) 0.041(2) 0.042(2) 0.017(1) 0.000(1) -0.013(1) C(5) 0.030(2) 0.035(2) 0.053(2) 0.018(1) -0.007(1) 0.000(1) C(6) 0.036(2) 0.056(2) 0.027(2) 0.023(2) -0.002(1) 0.008(1) C(7) 0.031(2) 0.052(2) 0.024(1) 0.023(1) 0.002(1) -0.002(1) C(8) 0.030(1) 0.023(1) 0.032(2) 0.014(1) 0.001(1) 0.001(1) C(9) 0.039(2) 0.016(1) 0.031(2) 0.016(1) 0.007(1) 0.004(1) C(10) 0.052(2) 0.029(2) 0.038(2) 0.024(1) 0.004(1) 0.005(1) C(11) 0.082(3) 0.037(2) 0.035(2) 0.033(2) 0.015(2) 0.012(1) C(12) 0.075(3) 0.031(2) 0.054(2) 0.024(2) 0.036(2) 0.019(2) C(13) 0.041(2) 0.020(2) 0.070(2) 0.010(1) 0.017(2) 0.004(2) C(14) 0.041(2) 0.018(1) 0.038(2) 0.012(1) 0.007(1) 0.001(1) C(15) 0.026(1) 0.019(1) 0.026(1) 0.012(1) 0.000(1) 0.003(1) C(16) 0.031(1) 0.025(1) 0.015(1) 0.017(1) -0.002(1) 0.002(1) C(17) 0.033(2) 0.024(1) 0.024(1) 0.013(1) 0.000(1) -0.002(1) C(18) 0.028(2) 0.034(2) 0.029(2) 0.009(1) 0.003(1) 0.001(1) C(19) 0.033(2) 0.050(2) 0.026(2) 0.024(1) 0.005(1) 0.000(1) C(20) 0.043(2) 0.034(2) 0.026(2) 0.025(1) 0.001(1) -0.004(1) C(21) 0.031(1) 0.025(1) 0.023(1) 0.013(1) 0.001(1) 0.001(1) C(22) 0.025(1) 0.026(1) 0.030(2) 0.006(1) -0.007(1) -0.003(1) C(23) 0.026(1) 0.025(1) 0.025(1) 0.010(1) -0.007(1) -0.005(1) C(24) 0.026(1) 0.023(1) 0.019(1) 0.011(1) 0.001(1) 0.003(1) C(25) 0.026(1) 0.023(1) 0.027(1) 0.012(1) -0.001(1) 0.005(1) C(26) 0.025(1) 0.038(2) 0.032(2) 0.020(1) 0.006(1) 0.011(1) C(27) 0.019(1) 0.035(2) 0.037(2) 0.008(1) 0.002(1) 0.010(1) C(28) 0.024(1) 0.025(1) 0.024(1) 0.011(1) 0.001(1) -0.002(1) C(29) 0.033(2) 0.033(2) 0.034(2) 0.018(1) 0.001(1) -0.002(1) C(30) 0.037(2) 0.037(2) 0.030(2) 0.018(1) 0.008(1) -0.001(1) C(31) 0.040(2) 0.026(1) 0.025(1) 0.021(1) 0.004(1) 0.005(1) C(32) 0.045(2) 0.026(1) 0.032(2) 0.022(1) -0.004(1) -0.005(1) C(33) 0.050(2) 0.035(2) 0.056(2) 0.029(2) 0.014(2) 0.006(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3539 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_obs 0.0236 _refine_ls_wR_factor_all 0.0315 _refine_ls_wR_factor_obs 0.0280 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.008 _refine_ls_shift/esd_max 0.0030 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.34 _refine_diff_density_max 0.37 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr(1) N(1) 2.073(2) ? ? yes Zr(1) N(2) 2.604(2) ? ? yes Zr(1) N(3) 2.497(2) ? ? yes Zr(1) C(1) 2.347(2) ? ? yes Zr(1) C(8) 2.326(2) ? ? yes Zr(1) C(15) 2.303(2) ? ? yes N(1) C(22) 1.462(3) ? ? yes N(1) C(27) 1.458(3) ? ? yes N(2) C(23) 1.506(3) ? ? yes N(2) C(24) 1.487(3) ? ? yes N(2) C(28) 1.509(3) ? ? yes N(3) C(25) 1.492(3) ? ? yes N(3) C(26) 1.501(3) ? ? yes N(3) C(31) 1.511(3) ? ? yes C(1) C(2) 1.490(3) ? ? yes C(2) C(3) 1.399(3) ? ? yes C(2) C(7) 1.386(3) ? ? yes C(3) C(4) 1.383(4) ? ? yes C(4) C(5) 1.376(4) ? ? yes C(5) C(6) 1.383(4) ? ? yes C(6) C(7) 1.384(4) ? ? yes C(8) C(9) 1.483(3) ? ? yes C(9) C(10) 1.396(4) ? ? yes C(9) C(14) 1.403(4) ? ? yes C(10) C(11) 1.381(4) ? ? yes C(11) C(12) 1.374(4) ? ? yes C(12) C(13) 1.380(4) ? ? yes C(13) C(14) 1.393(4) ? ? yes C(15) C(16) 1.490(3) ? ? yes C(16) C(17) 1.391(3) ? ? yes C(16) C(21) 1.405(3) ? ? yes C(17) C(18) 1.383(3) ? ? yes C(18) C(19) 1.382(4) ? ? yes C(19) C(20) 1.378(4) ? ? yes C(20) C(21) 1.384(3) ? ? yes C(22) C(23) 1.523(3) ? ? yes C(24) C(25) 1.518(3) ? ? yes C(26) C(27) 1.524(4) ? ? yes C(28) C(29) 1.518(3) ? ? yes C(28) C(30) 1.519(3) ? ? yes C(31) C(32) 1.511(4) ? ? yes C(31) C(33) 1.525(3) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Zr(1) N(2) 70.00(7) ? ? ? yes N(1) Zr(1) N(3) 73.03(7) ? ? ? yes N(1) Zr(1) C(1) 152.07(8) ? ? ? yes N(1) Zr(1) C(8) 88.13(8) ? ? ? yes N(1) Zr(1) C(15) 116.00(8) ? ? ? yes N(2) Zr(1) N(3) 73.02(6) ? ? ? yes N(2) Zr(1) C(1) 82.50(7) ? ? ? yes N(2) Zr(1) C(8) 108.64(7) ? ? ? yes N(2) Zr(1) C(15) 155.45(7) ? ? ? yes N(3) Zr(1) C(1) 104.15(8) ? ? ? yes N(3) Zr(1) C(8) 159.47(7) ? ? ? yes N(3) Zr(1) C(15) 85.77(7) ? ? ? yes C(1) Zr(1) C(8) 96.32(9) ? ? ? yes C(1) Zr(1) C(15) 91.08(8) ? ? ? yes C(8) Zr(1) C(15) 95.57(8) ? ? ? yes Zr(1) N(1) C(22) 116.1(1) ? ? ? yes Zr(1) N(1) C(27) 120.4(2) ? ? ? yes C(22) N(1) C(27) 113.4(2) ? ? ? yes Zr(1) N(2) C(23) 107.8(1) ? ? ? yes Zr(1) N(2) C(24) 102.6(1) ? ? ? yes Zr(1) N(2) C(28) 115.9(1) ? ? ? yes C(23) N(2) C(24) 110.6(2) ? ? ? yes C(23) N(2) C(28) 110.3(2) ? ? ? yes C(24) N(2) C(28) 109.4(2) ? ? ? yes Zr(1) N(3) C(25) 110.8(1) ? ? ? yes Zr(1) N(3) C(26) 96.8(1) ? ? ? yes Zr(1) N(3) C(31) 115.5(1) ? ? ? yes C(25) N(3) C(26) 110.9(2) ? ? ? yes C(25) N(3) C(31) 112.3(2) ? ? ? yes C(26) N(3) C(31) 109.5(2) ? ? ? yes Zr(1) C(1) C(2) 116.3(2) ? ? ? yes C(1) C(2) C(3) 122.5(2) ? ? ? yes C(1) C(2) C(7) 121.2(2) ? ? ? yes C(3) C(2) C(7) 116.2(2) ? ? ? yes C(2) C(3) C(4) 121.3(2) ? ? ? yes C(3) C(4) C(5) 121.3(2) ? ? ? yes C(4) C(5) C(6) 118.4(2) ? ? ? yes C(5) C(6) C(7) 120.0(3) ? ? ? yes C(2) C(7) C(6) 122.7(2) ? ? ? yes Zr(1) C(8) C(9) 113.7(2) ? ? ? yes C(8) C(9) C(10) 121.9(2) ? ? ? yes C(8) C(9) C(14) 121.2(2) ? ? ? yes C(10) C(9) C(14) 116.9(2) ? ? ? yes C(9) C(10) C(11) 121.7(3) ? ? ? yes C(10) C(11) C(12) 120.8(3) ? ? ? yes C(11) C(12) C(13) 119.0(3) ? ? ? yes C(12) C(13) C(14) 120.8(3) ? ? ? yes C(9) C(14) C(13) 120.8(3) ? ? ? yes Zr(1) C(15) C(16) 133.4(2) ? ? ? yes C(15) C(16) C(17) 121.4(2) ? ? ? yes C(15) C(16) C(21) 122.1(2) ? ? ? yes C(17) C(16) C(21) 116.5(2) ? ? ? yes C(16) C(17) C(18) 121.7(2) ? ? ? yes C(17) C(18) C(19) 120.9(2) ? ? ? yes C(18) C(19) C(20) 118.5(2) ? ? ? yes C(19) C(20) C(21) 120.8(2) ? ? ? yes C(16) C(21) C(20) 121.6(2) ? ? ? yes N(1) C(22) C(23) 109.7(2) ? ? ? yes N(2) C(23) C(22) 109.1(2) ? ? ? yes N(2) C(24) C(25) 113.8(2) ? ? ? yes N(3) C(25) C(24) 114.6(2) ? ? ? yes N(3) C(26) C(27) 111.1(2) ? ? ? yes N(1) C(27) C(26) 110.4(2) ? ? ? yes N(2) C(28) C(29) 110.6(2) ? ? ? yes N(2) C(28) C(30) 115.2(2) ? ? ? yes C(29) C(28) C(30) 109.9(2) ? ? ? yes N(3) C(31) C(32) 111.2(2) ? ? ? yes N(3) C(31) C(33) 114.5(2) ? ? ? yes C(32) C(31) C(33) 110.5(2) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' Chemical Communications' _publ_contact_author ; John Arnold Dept of Chemistry, UC Berkeley, Berkeley, CA 94720-1460 ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 510 643 5181 ' _publ_contact_author_fax ' 510 643 5482 ' _publ_contact_author_email ' arnold@socrates.berkeley.edu ' loop_ _publ_author_name _publ_author_address ' Garth R. Giesbrecht ' ; Dept of Chemistry, UC Berkeley, Berkeley, CA 94720-1460 ; _publ_section_title ; Zirconium tacn Complexes ; _publ_section_abstract ; Zirconium tacn Complexes ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END data_zrbzbz #------------------------------------------------------------------------------ _audit_creation_date 'Tue Jul 4 11:45:16 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 8.8810(5) _cell_length_b 25.936(2) _cell_length_c 11.7707(7) _cell_angle_alpha 90 _cell_angle_beta 112.017(1) _cell_angle_gamma 90 _cell_volume 2513.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 164 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_meas ? _chemical_formula_weight 484.83 _chemical_formula_analytical ? _chemical_formula_sum 'C26 H39 N3 Zr ' _chemical_formula_moiety 'C26 H39 N3 Zr ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1024.00 _exptl_absorpt_coefficient_mu 0.454 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 164 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'SMART CCD' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 11204 _reflns_number_total 4314 _reflns_number_observed 2387 _reflns_observed_criterion 'I>3.00 sigma' _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.59 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 104 0.003 0.002 'International Tables' H 0 156 0.000 0.000 'International Tables' N 0 12 0.006 0.003 'International Tables' Zr 0 4 -2.967 0.560 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Zr(1) 0.51600(7) 0.39706(2) 0.63763(5) 0.032 Uij ? ? N(1) 0.5331(5) 0.4560(2) 0.7682(4) 0.020 Uij ? ? N(2) 0.7970(5) 0.4071(2) 0.7699(4) 0.023 Uij ? ? N(3) 0.6480(6) 0.3407(2) 0.5966(5) 0.031 Uij ? ? C(1) 0.3923(7) 0.4416(2) 0.4588(5) 0.032 Uij ? ? C(2) 0.2495(7) 0.4148(2) 0.3665(5) 0.022 Uij ? ? C(3) 0.1091(7) 0.4055(3) 0.3886(6) 0.037 Uij ? ? C(4) -0.0200(8) 0.3778(3) 0.3050(8) 0.047 Uij ? ? C(5) -0.0090(9) 0.3603(3) 0.1981(8) 0.050 Uij ? ? C(6) 0.1265(10) 0.3688(3) 0.1763(6) 0.046 Uij ? ? C(7) 0.2537(7) 0.3956(3) 0.2579(5) 0.034 Uij ? ? C(8) 0.3278(7) 0.3498(2) 0.6835(6) 0.031 Uij ? ? C(9) 0.4057(7) 0.3273(2) 0.8071(5) 0.023 Uij ? ? C(10) 0.4206(7) 0.3546(2) 0.9133(6) 0.032 Uij ? ? C(11) 0.4967(8) 0.3344(3) 1.0286(6) 0.039 Uij ? ? C(12) 0.5628(8) 0.2847(3) 1.0428(6) 0.037 Uij ? ? C(13) 0.5489(8) 0.2574(3) 0.9400(6) 0.041 Uij ? ? C(14) 0.4724(8) 0.2781(3) 0.8249(6) 0.035 Uij ? ? C(15) 0.4120(7) 0.4919(2) 0.7513(5) 0.028 Uij ? ? C(16) 0.4087(8) 0.5318(2) 0.8196(6) 0.033 Uij ? ? C(17) 0.6761(7) 0.4628(3) 0.8804(5) 0.029 Uij ? ? C(18) 0.7854(7) 0.4175(3) 0.8892(6) 0.031 Uij ? ? C(19) 0.8851(8) 0.3575(3) 0.7752(6) 0.037 Uij ? ? C(20) 0.8209(8) 0.3287(3) 0.6555(7) 0.044 Uij ? ? C(21) 0.8700(7) 0.4522(2) 0.7295(6) 0.028 Uij ? ? C(22) 1.0309(8) 0.4708(3) 0.8248(7) 0.049 Uij ? ? C(23) 0.8857(8) 0.4432(3) 0.6069(6) 0.037 Uij ? ? C(24) 0.5539(8) 0.3127(2) 0.4864(6) 0.036 Uij ? ? C(25) 0.6144(9) 0.3216(3) 0.3822(7) 0.048 Uij ? ? C(26) 0.542(1) 0.2547(3) 0.5079(9) 0.066 Uij ? ? H(1) 0.470 0.447 0.423 0.038 Uij ? ? H(2) 0.356 0.474 0.478 0.038 Uij ? ? H(3) 0.101 0.418 0.462 0.044 Uij ? ? H(4) -0.115 0.371 0.322 0.056 Uij ? ? H(5) -0.097 0.342 0.140 0.060 Uij ? ? H(6) 0.134 0.356 0.103 0.055 Uij ? ? H(7) 0.348 0.401 0.240 0.040 Uij ? ? H(8) 0.287 0.323 0.625 0.037 Uij ? ? H(9) 0.241 0.372 0.682 0.037 Uij ? ? H(10) 0.377 0.388 0.905 0.039 Uij ? ? H(11) 0.504 0.354 1.099 0.047 Uij ? ? H(12) 0.616 0.270 1.122 0.044 Uij ? ? H(13) 0.593 0.224 0.948 0.049 Uij ? ? H(14) 0.465 0.258 0.755 0.042 Uij ? ? H(15) 0.317 0.487 0.680 0.034 Uij ? ? H(16) 0.316 0.553 0.796 0.039 Uij ? ? H(17) 0.499 0.539 0.892 0.039 Uij ? ? H(18) 0.645 0.464 0.949 0.034 Uij ? ? H(19) 0.730 0.494 0.877 0.034 Uij ? ? H(20) 0.743 0.388 0.914 0.037 Uij ? ? H(21) 0.891 0.425 0.948 0.037 Uij ? ? H(22) 0.873 0.336 0.837 0.045 Uij ? ? H(23) 0.997 0.365 0.795 0.045 Uij ? ? H(24) 0.835 0.293 0.670 0.053 Uij ? ? H(25) 0.877 0.339 0.605 0.053 Uij ? ? H(26) 0.795 0.480 0.717 0.034 Uij ? ? H(27) 1.014 0.481 0.897 0.059 Uij ? ? H(28) 1.070 0.499 0.792 0.059 Uij ? ? H(29) 1.108 0.443 0.845 0.059 Uij ? ? H(30) 0.916 0.474 0.579 0.045 Uij ? ? H(31) 0.966 0.418 0.616 0.045 Uij ? ? H(32) 0.785 0.432 0.549 0.045 Uij ? ? H(33) 0.446 0.326 0.459 0.043 Uij ? ? H(34) 0.616 0.357 0.367 0.058 Uij ? ? H(35) 0.721 0.308 0.405 0.058 Uij ? ? H(36) 0.544 0.305 0.310 0.058 Uij ? ? H(37) 0.645 0.239 0.524 0.079 Uij ? ? H(38) 0.464 0.240 0.437 0.079 Uij ? ? H(39) 0.511 0.250 0.576 0.079 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zr(1) 0.0362(3) 0.0305(3) 0.0279(3) 0.0000(3) 0.0096(2) 0.0008(3) N(1) 0.020(2) 0.023(3) 0.021(3) -0.004(2) 0.005(2) -0.002(2) N(2) 0.028(3) 0.026(3) 0.017(2) 0.008(2) 0.003(2) 0.008(2) N(3) 0.050(3) 0.020(3) 0.025(3) 0.004(2) 0.021(3) -0.004(2) C(1) 0.038(4) 0.024(3) 0.020(3) -0.002(3) 0.006(3) -0.001(3) C(2) 0.024(3) 0.021(3) 0.018(3) 0.000(2) 0.003(3) 0.005(3) C(3) 0.031(4) 0.048(4) 0.027(3) 0.008(3) 0.010(3) 0.020(3) C(4) 0.026(4) 0.055(5) 0.071(6) 0.001(3) 0.015(4) 0.037(5) C(5) 0.045(5) 0.031(4) 0.052(5) -0.011(3) -0.019(4) 0.011(4) C(6) 0.055(5) 0.033(4) 0.032(4) -0.002(4) -0.007(4) -0.006(3) C(7) 0.029(3) 0.036(4) 0.027(3) 0.000(3) 0.006(3) 0.000(4) C(8) 0.030(3) 0.029(4) 0.029(4) -0.004(3) 0.008(3) 0.003(3) C(9) 0.017(3) 0.023(3) 0.028(4) -0.009(3) 0.006(3) 0.001(3) C(10) 0.035(4) 0.025(3) 0.039(4) 0.001(3) 0.019(3) 0.004(3) C(11) 0.038(4) 0.043(4) 0.035(4) -0.006(3) 0.016(3) -0.002(4) C(12) 0.032(4) 0.044(4) 0.031(4) 0.001(3) 0.003(3) 0.011(4) C(13) 0.049(4) 0.032(4) 0.038(4) 0.009(3) 0.008(3) -0.001(4) C(14) 0.044(4) 0.033(4) 0.026(4) -0.003(3) 0.007(3) -0.007(3) C(15) 0.026(3) 0.032(4) 0.025(3) -0.003(3) 0.011(3) -0.001(3) C(16) 0.035(4) 0.032(4) 0.042(4) -0.002(3) 0.023(3) -0.006(3) C(17) 0.039(4) 0.039(4) 0.012(3) -0.004(3) 0.010(3) -0.004(3) C(18) 0.030(4) 0.041(4) 0.021(3) -0.002(3) 0.004(3) 0.005(3) C(19) 0.046(4) 0.040(4) 0.033(4) 0.017(3) 0.011(3) 0.011(4) C(20) 0.047(4) 0.032(4) 0.052(5) 0.019(3) 0.018(4) 0.003(4) C(21) 0.026(3) 0.029(3) 0.037(4) 0.002(3) 0.009(3) 0.004(3) C(22) 0.025(4) 0.065(5) 0.060(5) -0.008(4) 0.008(3) 0.004(4) C(23) 0.042(4) 0.040(4) 0.043(4) 0.010(3) 0.029(3) 0.012(4) C(24) 0.050(4) 0.024(4) 0.041(4) -0.006(3) 0.024(3) -0.006(3) C(25) 0.065(5) 0.046(5) 0.043(4) 0.008(4) 0.030(4) -0.004(4) C(26) 0.117(7) 0.028(4) 0.072(6) -0.009(5) 0.048(5) -0.010(5) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2387 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_obs 0.0431 _refine_ls_wR_factor_all 0.0639 _refine_ls_wR_factor_obs 0.0535 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.244 _refine_ls_shift/esd_max 0.0020 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.61 _refine_diff_density_max 0.63 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr(1) N(1) 2.132(5) ? ? yes Zr(1) N(2) 2.410(4) ? ? yes Zr(1) N(3) 2.043(5) ? ? yes Zr(1) C(1) 2.289(6) ? ? yes Zr(1) C(8) 2.295(6) ? ? yes N(1) C(15) 1.380(8) ? ? yes N(1) C(17) 1.460(7) ? ? yes N(2) C(18) 1.470(8) ? ? yes N(2) C(19) 1.495(8) ? ? yes N(2) C(21) 1.498(8) ? ? yes N(3) C(20) 1.462(8) ? ? yes N(3) C(24) 1.447(8) ? ? yes C(1) C(2) 1.495(8) ? ? yes C(2) C(3) 1.387(9) ? ? yes C(2) C(7) 1.386(8) ? ? yes C(3) C(4) 1.40(1) ? ? yes C(4) C(5) 1.38(1) ? ? yes C(5) C(6) 1.34(1) ? ? yes C(6) C(7) 1.366(9) ? ? yes C(8) C(9) 1.477(8) ? ? yes C(9) C(10) 1.399(9) ? ? yes C(9) C(14) 1.390(9) ? ? yes C(10) C(11) 1.374(9) ? ? yes C(11) C(12) 1.402(9) ? ? yes C(12) C(13) 1.367(10) ? ? yes C(13) C(14) 1.377(9) ? ? yes C(15) C(16) 1.317(9) ? ? yes C(17) C(18) 1.502(9) ? ? yes C(19) C(20) 1.51(1) ? ? yes C(21) C(22) 1.528(9) ? ? yes C(21) C(23) 1.519(9) ? ? yes C(24) C(25) 1.53(1) ? ? yes C(24) C(26) 1.534(10) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Zr(1) N(2) 71.3(2) ? ? ? yes N(1) Zr(1) N(3) 142.4(2) ? ? ? yes N(1) Zr(1) C(1) 100.4(2) ? ? ? yes N(1) Zr(1) C(8) 94.3(2) ? ? ? yes N(2) Zr(1) N(3) 71.5(2) ? ? ? yes N(2) Zr(1) C(1) 124.3(2) ? ? ? yes N(2) Zr(1) C(8) 125.1(2) ? ? ? yes N(3) Zr(1) C(1) 105.3(2) ? ? ? yes N(3) Zr(1) C(8) 101.9(2) ? ? ? yes C(1) Zr(1) C(8) 110.2(2) ? ? ? yes Zr(1) N(1) C(15) 122.6(4) ? ? ? yes Zr(1) N(1) C(17) 122.8(4) ? ? ? yes C(15) N(1) C(17) 114.5(5) ? ? ? yes Zr(1) N(2) C(18) 102.1(3) ? ? ? yes Zr(1) N(2) C(19) 109.4(4) ? ? ? yes Zr(1) N(2) C(21) 110.2(3) ? ? ? yes C(18) N(2) C(19) 110.0(5) ? ? ? yes C(18) N(2) C(21) 110.7(5) ? ? ? yes C(19) N(2) C(21) 113.8(5) ? ? ? yes Zr(1) N(3) C(20) 129.3(4) ? ? ? yes Zr(1) N(3) C(24) 112.4(4) ? ? ? yes C(20) N(3) C(24) 118.0(5) ? ? ? yes Zr(1) C(1) C(2) 114.7(4) ? ? ? yes C(1) C(2) C(3) 121.5(6) ? ? ? yes C(1) C(2) C(7) 121.9(5) ? ? ? yes C(3) C(2) C(7) 116.6(5) ? ? ? yes C(2) C(3) C(4) 121.0(6) ? ? ? yes C(3) C(4) C(5) 119.6(6) ? ? ? yes C(4) C(5) C(6) 119.8(6) ? ? ? yes C(5) C(6) C(7) 121.0(7) ? ? ? yes C(2) C(7) C(6) 122.0(6) ? ? ? yes Zr(1) C(8) C(9) 109.3(4) ? ? ? yes C(8) C(9) C(10) 122.1(5) ? ? ? yes C(8) C(9) C(14) 121.8(6) ? ? ? yes C(10) C(9) C(14) 116.1(6) ? ? ? yes C(9) C(10) C(11) 122.4(6) ? ? ? yes C(10) C(11) C(12) 119.9(6) ? ? ? yes C(11) C(12) C(13) 118.4(6) ? ? ? yes C(12) C(13) C(14) 121.2(6) ? ? ? yes C(9) C(14) C(13) 122.0(6) ? ? ? yes N(1) C(15) C(16) 129.6(6) ? ? ? yes N(1) C(17) C(18) 106.7(5) ? ? ? yes N(2) C(18) C(17) 110.7(5) ? ? ? yes N(2) C(19) C(20) 112.3(5) ? ? ? yes N(3) C(20) C(19) 107.5(5) ? ? ? yes N(2) C(21) C(22) 114.2(5) ? ? ? yes N(2) C(21) C(23) 112.8(5) ? ? ? yes C(22) C(21) C(23) 110.7(5) ? ? ? yes N(3) C(24) C(25) 112.6(6) ? ? ? yes N(3) C(24) C(26) 113.3(6) ? ? ? yes C(25) C(24) C(26) 110.1(6) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' Chemical Communications' _publ_contact_author ; John Arnold Dept of Chemistry, UC Berkeley, Berkeley, CA 94720-1460 ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 510 643 5181 ' _publ_contact_author_fax ' 510 643 5482 ' _publ_contact_author_email ' arnold@socrates.berkeley.edu ' loop_ _publ_author_name _publ_author_address ' Garth R. Giesbrecht ' ; Dept of Chemistry, UC Berkeley, Berkeley, CA 94720-1460 ; _publ_section_title ; Zirconium tacn Complexes ; _publ_section_abstract ; Zirconium tacn Complexes ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END