# Copyright The Royal Society of Chemistry, 1998. #================================================================ data_global #================================================================ _audit_creation_date 20-12-96 _audit_creation_method from_MolEN_master_file_using_cif_in _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author ; Ulli Englert Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; _publ_contact_author_email 'ullrich.englert@ac.rwth-aachen.de' _publ_contact_author_fax '(0241) 8888288' _publ_contact_author_phone '(0241) 804666' _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_letter ; ?edit? ; # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Englert, Ulli' #<--'Last name, first name' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; Backgrounds were obtained from analysis of the scan profile (Blessing, Coppens _& Becker, 1974) ; _publ_section_references ; Blessing, R.H., Coppens, P. & Becker, P. (1974). J. Appl. Cryst., 7, 488-492. Enraf-Nonius, CAD4 Operations Manual, Delft, 1977. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands. International Tables for X-Ray Crystallography, T. Hahn E Vol. A, D. Reidel Publ. Comp., Dordrecht, (1983) Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ?none? ?none? ; data_DJ1 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description 'almost isometric parallelepiped' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _chemical_name_common ; [ZrCl4.2(Pri-HNacac)] ; _chemical_formula_sum 'C16 H30 Cl4 N2 O2 Zr1' _chemical_formula_weight 515.46 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P-1' _cell_length_a 8.636(4) _cell_length_b 9.090(6) _cell_length_c 9.117(6) _cell_angle_alpha 119.58(5) _cell_angle_beta 91.07(5) _cell_angle_gamma 107.25(5) _cell_volume 583(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11 _cell_measurement_theta_max 23 _cell_formula_units_z 1.00 _exptl_crystal_density_diffrn 1.47 _exptl_crystal_density_meas none _diffrn_radiation_type Mo-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.938 _cell_measurement_temperature 293 _exptl_crystal_F_000 264 # 6. DATA COLLECTION _diffrn_ambient_temperature 293 _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/\q _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.972 _exptl_absorpt_correction_T_max 0.999 _diffrn_reflns_number 5755 _reflns_number_total 5112 _reflns_number_observed 4010 _reflns_observed_criterion >1.0\s(I) _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 35.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 3 _diffrn_standards_interval_time 166 _diffrn_standards_decay_% -20.6 # 7. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_obs 0.054 _refine_ls_wR_factor_obs 0.058 _refine_ls_hydrogen_treatment by_more_than_one_method _refine_ls_number_reflns 4010 _refine_ls_number_parameters 133 _refine_ls_number_restraints 45 _refine_ls_goodness_of_fit_obs 1.657 _refine_ls_weighting_scheme '4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)' _refine_ls_shift/esd_max 0.004 _refine_diff_density_max 1.6319 _refine_diff_density_min 0.0000 _refine_ls_extinction_method none _atom_type_scat_source International_Tables_for_Xray_Crystallography # 8. COMPUTING DATA _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_structure_solution none _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ORTEP_(Johnson,_1976) _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Zr 0.0000 0.0000 0.0000 0.03389(7) Ueq ? Cl1 -0.18446(8) -0.17462(8) 0.10678(8) 0.0518(2) Ueq . Cl2 0.22816(8) 0.11362(8) 0.23778(8) 0.0540(2) Ueq . O 0.0590(2) -0.2247(2) -0.1534(2) 0.0439(5) Ueq . N -0.1745(2) -0.5649(2) -0.2863(3) 0.0432(6) Ueq . C1 0.1589(3) -0.3102(3) -0.2260(3) 0.0392(6) Ueq . C2 0.1086(3) -0.4942(3) -0.3177(3) 0.0436(6) Ueq . C3 -0.0508(3) -0.6171(3) -0.3439(3) 0.0402(6) Ueq . C4 -0.0751(4) -0.8137(3) -0.4386(4) 0.0568(8) Ueq . C5 0.3339(3) -0.1980(4) -0.2021(4) 0.0604(9) Ueq . C6 -0.3414(3) -0.6787(3) -0.2972(4) 0.0524(8) Ueq . C7 -0.3456(5) -0.6960(4) -0.1404(4) 0.075(1) Ueq . C8 -0.4645(4) -0.5946(4) -0.3123(4) 0.069(1) Ueq . H -0.146(4) -0.451(4) -0.234(4) 0.037(9) Uiso . H2 0.1967 -0.5394 -0.3660 0.025(8) Uiso calc H4a 0.0124 -0.8297 -0.5057 0.05(1) Uiso calc H4b -0.1755 -0.9090 -0.5219 0.09(2) Uiso calc H4c -0.0778 -0.8331 -0.3419 0.08(2) Uiso calc H5a 0.3648 -0.0996 -0.0811 0.10(2) Uiso calc H5b 0.3449 -0.1537 -0.2814 0.09(2) Uiso calc H5c 0.4051 -0.2708 -0.2337 0.07(1) Uiso calc H6 -0.3647 -0.8017 -0.3950 0.027(8) Uiso calc H7a -0.2565 -0.7400 -0.1336 0.031(9) Uiso calc H7b -0.4561 -0.7622 -0.1359 0.06(1) Uiso calc H7c -0.3150 -0.5727 -0.0410 0.05(1) Uiso calc H8a -0.5713 -0.6802 -0.3231 0.04(1) Uiso calc H8b -0.4642 -0.5805 -0.4121 0.04(1) Uiso calc H8c -0.4351 -0.4722 -0.2117 0.06(1) Uiso calc 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 0.0314(1) 0.02677(8) 0.0370(1) 0.01010(7) 0.01083(9) 0.01201(7) Cl1 0.0517(3) 0.0426(2) 0.0534(2) 0.0089(2) 0.0213(2) 0.0233(2) Cl2 0.0416(3) 0.0561(2) 0.0548(3) 0.0127(2) 0.0029(2) 0.0251(2) O 0.0396(6) 0.0338(5) 0.0510(7) 0.0175(4) 0.0171(6) 0.0142(5) N 0.0419(8) 0.0314(6) 0.0507(8) 0.0138(6) 0.0128(7) 0.0170(5) C1 0.0357(8) 0.0423(7) 0.0405(8) 0.0194(6) 0.0114(7) 0.0189(6) C2 0.0431(9) 0.0432(7) 0.0469(9) 0.0255(6) 0.0149(8) 0.0193(6) C3 0.051(1) 0.0352(6) 0.0354(8) 0.0211(6) 0.0088(8) 0.0156(5) C4 0.073(1) 0.0358(8) 0.056(1) 0.0285(7) 0.017(1) 0.0142(8) C5 0.037(1) 0.062(1) 0.076(1) 0.0171(9) 0.018(1) 0.032(1) C6 0.043(1) 0.0359(8) 0.063(1) 0.0081(8) 0.012(1) 0.0183(8) C7 0.073(2) 0.078(1) 0.106(1) 0.030(1) 0.035(1) 0.0677(8) C8 0.045(1) 0.074(1) 0.081(2) 0.018(1) 0.004(1) 0.038(1) # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O C1 1.303(2) ? N C3 1.310(3) ? N C6 1.472(3) ? N H 0.84(3) ? C1 C2 1.363(3) ? C1 C5 1.492(3) ? C2 C3 1.418(3) ? C2 H2 0.980(2) ? C3 C4 1.494(3) ? C4 H4a 0.980(3) ? C4 H4b 0.980(3) ? C4 H4c 0.980(3) ? C5 H5a 0.980(3) ? C5 H5b 0.980(3) ? C5 H5c 0.980(2) ? C6 C7 1.513(4) ? C6 C8 1.521(4) ? C6 H6 0.980(2) ? C7 H7a 0.980(3) ? C7 H7b 0.980(3) ? C7 H7c 0.980(4) ? C8 H8a 0.980(3) ? C8 H8b 0.980(3) ? C8 H8c 0.980(3) ? Zr Cl1 2.468(1) ? Zr Cl2 2.464(1) ? Zr O 2.052(1) ? Zr O 2.052(1) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C3 N C6 127.6(2) ? C3 N H 111(2) ? C6 N H 121(2) ? O C1 C2 122.2(2) ? O C1 C5 117.1(2) ? C2 C1 C5 120.7(2) ? C1 C2 C3 126.8(2) ? C1 C2 H2 113.1(2) ? C3 C2 H2 120.1(2) ? N C3 C2 122.9(2) ? N C3 C4 119.5(2) ? C2 C3 C4 117.6(2) ? C3 C4 H4a 107.0(2) ? C3 C4 H4b 123.8(2) ? C3 C4 H4c 99.5(2) ? H4a C4 H4b 103.4(2) ? H4a C4 H4c 121.1(3) ? H4b C4 H4c 103.5(2) ? C1 C5 H5a 105.5(2) ? C1 C5 H5b 111.2(2) ? C1 C5 H5c 111.0(2) ? H5a C5 H5b 112.5(3) ? H5a C5 H5c 113.3(3) ? H5b C5 H5c 103.4(2) ? N C6 C7 109.8(2) ? N C6 C8 108.7(2) ? N C6 H6 108.6(2) ? C7 C6 C8 111.5(2) ? C7 C6 H6 105.2(2) ? C8 C6 H6 113.0(2) ? C6 C7 H7a 106.5(3) ? C6 C7 H7b 113.4(3) ? C6 C7 H7c 106.0(2) ? H7a C7 H7b 117.3(3) ? H7a C7 H7c 107.1(3) ? H7b C7 H7c 105.9(3) ? C6 C8 H8a 103.3(2) ? C6 C8 H8b 113.5(3) ? C6 C8 H8c 109.5(2) ? H8a C8 H8b 110.5(3) ? H8a C8 H8c 114.9(3) ? H8b C8 H8c 105.4(3) ? Cl1 Zr Cl1 180.00 ? Cl1 Zr Cl2 90.20(2) ? Cl1 Zr Cl2 89.80(2) ? Cl1 Zr O 87.98(4) ? Cl1 Zr O 92.02(4) ? Cl1 Zr Cl2 89.80(2) ? Cl1 Zr Cl2 90.20(2) ? Cl1 Zr O 92.02(4) ? Cl1 Zr O 87.98(4) ? Cl2 Zr Cl2 180.00 ? Cl2 Zr O 91.93(4) ? Cl2 Zr O 88.07(4) ? Cl2 Zr O 88.07(4) ? Cl2 Zr O 91.93(4) ? O Zr O 180.00 ? #=END data_kcticl _audit_creation_date 96-12-01 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural ? #ActaC _chemical_formula_sum ? #ActaC _chemical_formula_weight ? #ActaC _chemical_melting_point ? #ActaC _computing_data_collection ? #ActaC _computing_cell_refinement ? #ActaC _computing_data_reduction xtal_DIFDAT_ABSORB_SORTRF_ADDREF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 8.834(4) #ActaC _cell_length_b 8.974(4) #ActaC _cell_length_c 9.028(4) #ActaC _cell_angle_alpha 120.18(3) #ActaC _cell_angle_beta 90.10(3) #ActaC _cell_angle_gamma 107.62(3) #ActaC _cell_volume 579.3(5) #ActaC _cell_formula_units_Z ? #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used ? #ActaC _cell_measurement_theta_min ? #ActaC _cell_measurement_theta_max ? #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting triclinic #ActaC _symmetry_space_group_name_H-M p_-1 #ActaC _symmetry_space_group_name_Hall -p_1 #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,-y,-z _exptl_crystal_description ? #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour ? #ActaC _exptl_crystal_size_max ? #ActaC _exptl_crystal_size_mid ? #ActaC _exptl_crystal_size_min ? #ActaC _exptl_crystal_density_diffrn 2.707 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 492 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu ? #ActaC _exptl_absorpt_correction_type ? #ActaC _exptl_absorpt_correction_T_min ? #ActaC _exptl_absorpt_correction_T_max ? #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength ? #ActaC _diffrn_radiation_type xray_tube #ActaC _diffrn_radiation_source ? #ActaC _diffrn_radiation_monochromator ? #ActaC _diffrn_radiation_detector ? #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method ? #ActaC _diffrn_standards_number ? #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time ? #ActaC _diffrn_standards_decay_% ? #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 3489 #ActaC _diffrn_reflns_av_R_equivalents .043 #ActaC _diffrn_reflns_av_sigmaI/netI 0 #ActaC _diffrn_reflns_limit_h_min -12 #ActaC _diffrn_reflns_limit_h_max 11 #ActaC _diffrn_reflns_limit_k_min -6 #ActaC _diffrn_reflns_limit_k_max 12 #ActaC _diffrn_reflns_limit_l_min -12 #ActaC _diffrn_reflns_limit_l_max 12 #ActaC _diffrn_reflns_theta_min 2.52 #ActaC _diffrn_reflns_theta_max 29.99 #ActaC _diffrn_reflns_reduction_process perpendicular_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 32 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 4 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 60 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Cl ? 0 8 .132 .159 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 4 .004 .003 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Ti ? 0 2 .248 .446 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Ti .00000 .00000 .00000 .0375(2) Uani ? ? Cl1 -.17450(6) -.16934(7) .10532(7) .0506(2) Uani ? ? Cl2 .21931(6) .10741(7) .22355(7) .0531(2) Uani ? ? O .05369(16) -.21352(17) -.14977(18) .0441(5) Uani ? ? N -.1780(2) -.5613(2) -.2870(2) .0434(7) Uani ? ? C1 .1559(2) -.2986(3) -.2208(3) .0391(7) Uani ? ? C2 .1068(2) -.4852(3) -.3125(3) .0449(8) Uani ? ? C3 -.0532(2) -.6130(3) -.3411(2) .0402(7) Uani ? ? C4 -.0738(4) -.8121(3) -.4351(4) .0575(11) Uani ? ? C5 .3312(3) -.1821(4) -.1954(4) .0589(10) Uani ? ? C6 -.3468(3) -.6781(3) -.2991(3) .0526(9) Uani ? ? C7 -.3535(4) -.6962(5) -.1414(5) .0755(15) Uani ? ? C8 -.4687(3) -.5964(5) -.3172(5) .0702(13) Uani ? ? H -.162(3) -.457(4) -.234(3) .064(8) Uiso ? ? H2 .187(3) -.532(3) -.352(3) .062(7) Uiso ? ? H4a -.169(5) -.881(5) -.520(5) .125(14) Uiso ? ? H4b -.005(5) -.830(5) -.498(5) .117(14) Uiso ? ? H4c -.085(4) -.859(5) -.366(5) .114(13) Uiso ? ? H5a .393(4) -.247(4) -.245(4) .082(9) Uiso ? ? H5b .346(4) -.118(4) -.257(4) .105(12) Uiso ? ? H5c .365(4) -.102(5) -.085(5) .094(11) Uiso ? ? H6 -.368(3) -.798(3) -.404(3) .057(7) Uiso ? ? H7a -.295(4) -.770(5) -.152(5) .118(13) Uiso ? ? H7b -.338(5) -.591(6) -.030(6) .143(17) Uiso ? ? H7c -.461(4) -.769(4) -.152(4) .091(10) Uiso ? ? H8a -.454(5) -.499(5) -.226(5) .121(15) Uiso ? ? H8b -.478(4) -.608(4) -.432(4) .085(10) Uiso ? ? H8c -.590(4) -.677(4) -.327(4) .106(11) Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Ti .0325(2) .0273(2) .0425(3) .00766(18) .0094(2) .0129(2) Cl1 .0498(3) .0382(3) .0527(3) .0070(2) .0171(2) .0210(2) Cl2 .0417(3) .0511(3) .0558(3) .0109(2) .0014(2) .0239(3) O .0373(7) .0308(6) .0523(8) .0119(5) .0128(6) .0138(6) N .0417(9) .0285(8) .0502(10) .0106(7) .0102(8) .0150(8) C1 .0341(9) .0395(10) .0414(10) .0151(8) .0075(8) .0186(8) C2 .0396(10) .0415(10) .0521(12) .0220(9) .0126(9) .0195(9) C3 .0486(11) .0319(9) .0364(10) .0171(8) .0062(8) .0138(8) C4 .0696(17) .0344(11) .0597(15) .0248(11) .0146(14) .0153(11) C5 .0351(11) .0541(14) .0739(19) .0122(10) .0147(12) .0265(14) C6 .0435(11) .0335(10) .0611(14) .0046(9) .0109(10) .0164(10) C7 .073(2) .071(2) .103(3) .0272(17) .0358(18) .060(2) C8 .0447(14) .072(2) .085(2) .0143(13) .0033(14) .0382(19) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls:_F____sigma_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment ? #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 2383(314) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 2624 #ActaC _refine_ls_number_parameters 176 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .046 #ActaC _refine_ls_R_factor_obs .037 #ActaC _refine_ls_wR_factor_all .046 #ActaC _refine_ls_wR_factor_obs .044 #ActaC _refine_ls_goodness_of_fit_all 1.93 #ActaC _refine_ls_goodness_of_fit_obs 2.1 #ActaC _refine_ls_shift/esd_max .074 #ActaC _refine_ls_shift/esd_mean .005 #ActaC _refine_diff_density_min -.324 #ActaC _refine_diff_density_max .28 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Ti Cl1 2.3726(9) . . ? Ti Cl2 2.3781(10) . . ? Ti O 1.9163(15) . . ? Ti Cl1 2.3726(9) . 2 ? Ti Cl2 2.3781(10) . 2 ? Ti O 1.9163(15) . 2 ? O C1 1.318(3) . . ? N C3 1.323(3) . . ? N C6 1.508(3) . . ? N H .77(3) . . ? C1 C2 1.357(3) . . ? C1 C5 1.523(3) . . ? C2 C3 1.449(3) . . ? C2 H2 .91(3) . . ? C3 C4 1.491(3) . . ? C4 H4a .94(4) . . ? C4 H4b .83(4) . . ? C4 H4c .91(5) . . ? C5 H5a .88(4) . . ? C5 H5b .97(5) . . ? C5 H5c .86(3) . . ? C6 C7 1.511(6) . . ? C6 C8 1.525(5) . . ? C6 H6 .97(2) . . ? C7 H7a .92(5) . . ? C7 H7b .94(4) . . ? C7 H7c .95(3) . . ? C8 H8a .81(3) . . ? C8 H8b .99(4) . . ? C8 H8c 1.07(4) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Ti C1 3.150(2) . . ? Ti C1 3.150(2) . 2 ? Cl1 Cl2 3.3913(15) . . ? Cl1 Cl2 3.3270(17) . 2 ? Cl1 O 3.082(2) . 2 ? Cl1 O 3.0177(19) . . ? Cl2 O 3.0768(16) . . ? Cl2 O 3.031(2) . 2 ? O N 2.775(2) . . ? O C2 2.327(3) . . ? O C3 2.906(3) . . ? O C5 2.442(3) . . ? O H 2.19(2) . . ? N C1 2.997(3) . . ? N C2 2.443(3) . . ? N C4 2.435(4) . . ? N C7 2.463(6) . . ? N C8 2.489(4) . . ? N H6 2.01(2) . . ? C1 C3 2.512(3) . . ? C1 H2 1.93(3) . . ? C1 H5a 2.04(3) . . ? C1 H5b 2.11(4) . . ? C1 H5c 1.97(3) . . ? C2 C4 2.504(3) . . ? C2 C5 2.506(3) . . ? C3 C6 2.553(3) . . ? C3 H 1.81(3) . . ? C3 H2 2.04(3) . . ? C3 H4a 2.01(3) . . ? C3 H4b 1.93(4) . . ? C3 H4c 2.03(5) . . ? C6 H 1.95(3) . . ? C6 H7a 1.99(6) . . ? C6 H7b 2.14(5) . . ? C6 H7c 2.01(4) . . ? C6 H8a 1.94(5) . . ? C6 H8b 2.09(4) . . ? C6 H8c 2.17(4) . . ? C7 C8 2.517(8) . . ? C7 H6 2.06(3) . . ? C8 H6 2.05(3) . . ? H4a H4b 1.36(6) . . ? H4a H4c 1.47(7) . . ? H4b H4c 1.49(7) . . ? H5a H5b 1.40(7) . . ? H5a H5c 1.47(4) . . ? H5b H5c 1.49(6) . . ? H7a H7b 1.59(6) . . ? H7a H7c 1.47(6) . . ? H7b H7c 1.46(4) . . ? H8a H8b 1.58(5) . . ? H8a H8c 1.48(4) . . ? H8b H8c 1.58(6) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC Cl1 Ti Cl2 91.10(4) . . . ? Cl1 Ti O 88.77(6) . . . ? Cl1 Ti Cl1 180.0(3) . . 2 ? Cl1 Ti Cl2 88.90(4) . . 2 ? Cl1 Ti O 91.23(6) . . 2 ? Cl2 Ti O 90.87(6) . . . ? Cl2 Ti Cl1 88.90(4) . . 2 ? Cl2 Ti Cl2 180.0(6) . . 2 ? Cl2 Ti O 89.13(6) . . 2 ? O Ti Cl1 91.23(6) . . 2 ? O Ti Cl2 89.13(6) . . 2 ? O Ti O 180.0000 . . 2 ? Cl1 Ti Cl2 91.10(4) 2 . 2 ? Cl1 Ti O 88.77(6) 2 . 2 ? Cl2 Ti O 90.87(6) 2 . 2 ? Ti O C1 153.36(10) . . . ? C3 N C6 128.7(2) . . . ? C3 N H 117(2) . . . ? C6 N H 114(2) . . . ? O C1 C2 120.86(17) . . . ? O C1 C5 118.32(19) . . . ? C2 C1 C5 120.8(2) . . . ? C1 C2 C3 127.0(2) . . . ? C1 C2 H2 114.6(15) . . . ? C3 C2 H2 118.2(15) . . . ? N C3 C2 123.5(2) . . . ? N C3 C4 119.7(2) . . . ? C2 C3 C4 116.8(2) . . . ? C3 C4 H4a 110(3) . . . ? C3 C4 H4b 109(3) . . . ? C3 C4 H4c 114(2) . . . ? H4a C4 H4b 100(4) . . . ? H4a C4 H4c 105(4) . . . ? H4b C4 H4c 117(5) . . . ? C1 C5 H5a 113.7(19) . . . ? C1 C5 H5b 114(2) . . . ? C1 C5 H5c 108(2) . . . ? H5a C5 H5b 98(4) . . . ? H5a C5 H5c 115(3) . . . ? H5b C5 H5c 109(4) . . . ? N C6 C7 109.4(2) . . . ? N C6 C8 110.3(3) . . . ? N C6 H6 106.1(15) . . . ? C7 C6 C8 112.0(3) . . . ? C7 C6 H6 110(2) . . . ? C8 C6 H6 108.8(19) . . . ? C6 C7 H7a 107(3) . . . ? C6 C7 H7b 119(4) . . . ? C6 C7 H7c 108(3) . . . ? H7a C7 H7b 117(4) . . . ? H7a C7 H7c 103(4) . . . ? H7b C7 H7c 101(3) . . . ? C6 C8 H8a 108(4) . . . ? C6 C8 H8b 111(2) . . . ? C6 C8 H8c 112(3) . . . ? H8a C8 H8b 123(5) . . . ? H8a C8 H8c 103(3) . . . ? H8b C8 H8c 100(3) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min -6 _reflns_limit_k_max 12 _reflns_limit_l_min -12 _reflns_limit_l_max 12 _reflns_number_total 3297 #ActaC _reflns_number_observed 2624 #ActaC _reflns_observed_criterion refl_observed_if_F____>_.000_sigma(F___) _reflns_d_resolution_high .711 _reflns_d_resolution_low 8.071 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? .408791 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_observed_status _refln_scale_group_code -12 3 -1 2.883 2.698 .229 o 1 -12 3 0 .866 .994 .471 < 1 -12 3 1 4.153 4.127 .215 o 1 -12 4 -1 1.257 1.183 .465 < 1 -12 4 0 1.394 1.190 .197 < 1 -12 4 1 1.882 1.909 .269 o 1 -12 5 -1 1.721 1.625 .269 o 1 -12 5 0 2.143 2.282 .188 o 1 -11 -1 2 4.889 5.321 .204 o 1 -11 -1 3 2.085 2.709 .252 o 1 -11 -1 4 .786 .571 .425 < 1 -11 0 1 5.543 5.432 .205 o 1 -11 0 2 8.657 8.999 .218 o 1 -11 0 3 3.788 4.002 .211 o 1 -11 0 4 2.378 2.558 .263 o 1 -11 0 5 2.407 2.148 .238 o 1 -11 1 -1 3.602 4.045 .244 o 1 -11 1 0 3.251 2.943 .228 o 1 -11 1 1 10.124 10.413 .216 o 1 -11 1 2 7.226 7.484 .213 o 1 -11 1 3 .493 .680 .399 < 1 -11 1 4 .456 1.491 .349 < 1 -11 1 5 3.041 3.005 .241 o 1 -11 2 -3 1.309 1.646 .444 < 1 -11 2 -2 1.286 1.484 .401 < 1 -11 2 -1 .408 .159 .292 < 1 -11 2 0 3.811 3.812 .146 o 1 -11 2 1 3.345 3.232 .212 o 1 -11 2 2 2.041 1.979 .228 o 1 -11 2 3 3.289 3.120 .212 o 1 -11 2 4 3.330 3.222 .193 o 1 -11 2 5 4.952 5.005 .204 o 1 -11 3 -4 3.785 4.083 .225 o 1 -11 3 -3 4.018 3.647 .215 o 1 -11 3 -2 2.716 2.597 .211 o 1 -11 3 -1 1.157 1.651 .448 < 1 -11 3 0 .694 1.626 .435 < 1 -11 3 1 2.599 2.686 .231 o 1 -11 3 2 1.482 2.002 .388 < 1 -11 3 3 1.955 1.827 .257 o 1 -11 3 4 4.514 4.787 .213 o 1 -11 4 -4 5.718 5.542 .211 o 1 -11 4 -3 3.332 3.268 .215 o 1 -11 4 -2 .670 .474 .376 < 1 -11 4 -1 4.764 5.301 .201 o 1 -11 4 0 6.435 6.452 .159 o 1 -11 4 1 .558 .884 .336 < 1 -11 4 2 3.259 2.955 .213 o 1 -11 4 3 2.288 2.483 .225 o 1 -11 4 4 3.452 3.029 .224 o 1 -11 5 -5 4.509 4.497 .220 o 1 -11 5 -4 1.528 .681 .211 o 1 -11 5 -3 1.605 .486 .205 o 1 -11 5 -2 3.611 3.442 .214 o 1 -11 5 -1 4.514 4.739 .201 o 1 -11 5 0 3.556 3.439 .143 o 1 -11 5 1 3.877 3.699 .210 o 1 -11 5 2 1.181 1.562 .453 < 1 -11 5 3 .405 .804 .320 < 1 -11 6 -5 1.714 1.969 .472 < 1 -11 6 -4 .390 .192 .273 < 1 -11 6 -3 .767 1.525 .433 < 1 -11 6 -2 .911 .931 .420 < 1 -11 6 -1 6.391 5.618 .193 o 1 -11 6 0 4.849 4.568 .151 o 1 -11 6 1 .448 .649 .349 < 1 -11 6 2 5.985 5.742 .210 o 1 -11 7 -5 2.400 1.953 .264 o 1 -11 7 -4 .771 .850 .414 < 1 -11 7 -3 .755 .692 .399 < 1 -11 7 -2 1.949 2.369 .287 o 1 -11 7 -1 .348 1.128 .312 < 1 -11 7 0 3.960 3.513 .154 o 1 -11 7 1 3.962 3.878 .227 o 1 -11 8 -4 .416 .599 .307 < 1 -11 8 -3 .686 .896 .408 < 1 -11 8 -2 3.341 3.190 .238 o 1 -11 8 -1 3.437 2.743 .236 o 1 -10 -3 6 5.541 5.343 .209 o 1 -10 -2 4 4.924 5.348 .213 o 1 -10 -2 5 1.023 .848 .391 < 1 -10 -2 6 6.856 6.912 .226 o 1 -10 -1 2 3.582 3.925 .209 o 1 -10 -1 3 .502 .664 .375 < 1 -10 -1 4 3.273 3.510 .210 o 1 -10 -1 5 1.253 1.182 .345 < 1 -10 -1 6 1.067 .726 .433 < 1 -10 -1 7 .414 .208 .282 < 1 -10 0 1 4.897 5.426 .198 o 1 -10 0 2 10.251 10.377 .208 o 1 -10 0 3 5.644 6.101 .203 o 1 -10 0 4 3.820 4.322 .195 o 1 -10 0 5 3.138 3.665 .219 o 1 -10 0 6 1.377 1.289 .380 < 1 -10 0 7 2.101 2.362 .258 o 1 -10 1 -1 4.572 4.422 .188 o 1 -10 1 0 5.028 5.137 .211 o 1 -10 1 1 6.472 5.996 .192 o 1 -10 1 2 3.537 3.218 .195 o 1 -10 1 3 2.273 2.548 .247 o 1 -10 1 4 6.461 6.795 .198 o 1 -10 1 5 7.006 7.345 .202 o 1 -10 1 6 2.065 2.281 .243 o 1 -10 2 -3 1.447 .408 .205 o 1 -10 2 -2 .652 .371 .376 < 1 -10 2 -1 3.241 3.464 .191 o 1 -10 2 0 6.978 7.381 .274 o 1 -10 2 1 1.692 1.576 .258 o 1 -10 2 2 3.222 3.333 .200 o 1 -10 2 3 1.897 1.729 .229 o 1 -10 2 4 5.253 5.219 .196 o 1 -10 2 5 5.008 4.684 .202 o 1 -10 2 6 4.774 4.316 .227 o 1 -10 3 -5 2.679 2.904 .250 o 1 -10 3 -4 3.403 3.293 .228 o 1 -10 3 -3 .965 .668 .378 < 1 -10 3 -2 4.506 4.848 .190 o 1 -10 3 -1 9.652 9.891 .201 o 1 -10 3 0 5.402 5.242 .196 o 1 -10 3 1 .489 .264 .310 < 1 -10 3 2 3.154 2.783 .195 o 1 -10 3 3 .649 .764 .366 < 1 -10 3 4 3.347 3.062 .206 o 1 -10 3 5 5.337 5.167 .205 o 1 -10 3 6 2.007 1.831 .282 o 1 -10 4 -6 2.193 2.321 .262 o 1 -10 4 -5 3.353 2.466 .204 o 1 -10 4 -4 .932 .980 .447 < 1 -10 4 -3 .985 1.238 .373 < 1 -10 4 -2 5.851 6.047 .194 o 1 -10 4 -1 9.993 9.703 .202 o 1 -10 4 0 6.768 6.627 .207 o 1 -10 4 1 .845 .684 .388 < 1 -10 4 2 .839 1.137 .424 < 1 -10 4 3 3.429 3.965 .209 o 1 -10 4 4 .873 1.539 .460 < 1 -10 4 5 1.201 .582 .384 < 1 -10 5 -6 3.169 2.769 .222 o 1 -10 5 -5 2.717 3.063 .234 o 1 -10 5 -4 1.636 .798 .192 o 1 -10 5 -3 3.094 2.911 .185 o 1 -10 5 -2 2.880 2.973 .213 o 1 -10 5 -1 8.955 8.633 .196 o 1 -10 5 0 3.282 2.955 .139 o 1 -10 5 1 2.464 2.818 .229 o 1 -10 5 2 4.790 5.440 .208 o 1 -10 5 3 4.855 5.268 .214 o 1 -10 5 4 5.174 4.723 .220 o 1 -10 6 -7 3.407 3.778 .242 o 1 -10 6 -6 7.947 7.704 .206 o 1 -10 6 -5 .923 .744 .413 < 1 -10 6 -4 4.584 4.380 .196 o 1 -10 6 -3 2.856 3.045 .194 o 1 -10 6 -2 4.747 4.153 .195 o 1 -10 6 -1 .265 .009 .247 < 1 -10 6 0 .423 .009 .278 < 1 -10 6 1 1.282 2.004 .434 < 1 -10 6 2 8.659 8.767 .206 o 1 -10 6 3 6.739 6.876 .217 o 1 -10 7 -7 4.700 4.623 .235 o 1 -10 7 -6 .536 .473 .377 < 1 -10 7 -5 .666 .898 .390 < 1 -10 7 -4 2.277 2.094 .229 o 1 -10 7 -3 3.235 3.164 .219 o 1 -10 7 -2 6.051 5.636 .185 o 1 -10 7 -1 .683 .650 .371 < 1 -10 7 0 2.267 2.327 .180 o 1 -10 7 1 2.056 2.156 .235 o 1 -10 7 2 5.706 5.746 .212 o 1 -10 8 -6 1.147 .785 .438 < 1 -10 8 -5 1.627 2.040 .424 < 1 -10 8 -4 4.882 4.701 .201 o 1 -10 8 -3 7.433 7.240 .213 o 1 -10 8 -2 3.051 2.477 .225 o 1 -10 8 -1 1.050 .798 .382 < 1 -10 8 0 2.010 2.296 .235 o 1 -10 8 1 2.783 2.561 .230 o 1 -10 9 -6 .740 .652 .414 < 1 -10 9 -5 1.995 1.883 .257 o 1 -10 9 -4 3.530 3.621 .255 o 1 -10 9 -3 3.628 3.242 .225 o 1 -10 9 -2 3.094 2.981 .227 o 1 -10 9 -1 2.890 2.779 .238 o 1 -9 -3 6 1.766 1.485 .280 o 1 -9 -3 7 6.488 6.219 .202 o 1 -9 -3 8 4.666 4.883 .241 o 1 -9 -2 4 3.460 2.773 .181 o 1 -9 -2 5 4.216 4.079 .196 o 1 -9 -2 6 2.532 2.674 .222 o 1 -9 -2 7 .964 .836 .463 < 1 -9 -2 8 .503 .124 .360 < 1 -9 -1 2 1.662 1.772 .258 o 1 -9 -1 3 3.798 4.108 .191 o 1 -9 -1 4 7.703 7.924 .199 o 1 -9 -1 5 7.814 8.186 .193 o 1 -9 -1 6 2.199 1.928 .211 o 1 -9 -1 7 4.156 4.010 .218 o 1 -9 -1 8 .652 .781 .388 < 1 -9 0 1 2.935 2.630 .179 o 1 -9 0 2 .414 .351 .266 < 1 -9 0 3 7.600 7.698 .189 o 1 -9 0 4 14.542 14.837 .229 o 1 -9 0 5 6.392 6.288 .194 o 1 -9 0 6 2.112 1.988 .205 o 1 -9 0 7 .440 .292 .314 < 1 -9 0 8 .530 .642 .328 < 1 -9 1 -1 6.427 6.705 .186 o 1 -9 1 0 2.378 2.462 .143 o 1 -9 1 1 3.914 4.056 .192 o 1 -9 1 2 .485 .768 .314 < 1 -9 1 3 3.338 3.457 .200 o 1 -9 1 4 9.357 9.508 .194 o 1 -9 1 5 8.681 8.636 .204 o 1 -9 1 6 2.474 2.280 .231 o 1 -9 1 7 2.001 1.928 .284 o 1 -9 1 8 4.328 4.267 .239 o 1 -9 2 -3 .589 .162 .353 < 1 -9 2 -2 8.726 8.938 .189 o 1 -9 2 -1 12.256 12.016 .206 o 1 -9 2 0 9.816 9.962 .134 o 1 -9 2 1 3.665 3.641 .181 o 1 -9 2 2 4.813 5.081 .183 o 1 -9 2 3 3.483 3.673 .173 o 1 -9 2 4 3.314 3.533 .207 o 1 -9 2 5 1.093 .648 .366 < 1 -9 2 6 3.910 3.559 .201 o 1 -9 2 7 6.217 6.074 .236 o 1 -9 3 -5 .588 .454 .333 < 1 -9 3 -4 3.362 3.131 .187 o 1 -9 3 -3 1.829 2.121 .240 o 1 -9 3 -2 12.445 12.370 .207 o 1 -9 3 -1 16.676 16.644 .237 o 1 -9 3 0 4.234 4.490 .167 o 1 -9 3 1 .320 .105 .277 < 1 -9 3 2 4.548 4.980 .175 o 1 -9 3 3 4.897 4.999 .181 o 1 -9 3 4 .773 1.326 .401 < 1 -9 3 5 1.419 2.145 .448 < 1 -9 3 6 .481 .199 .305 < 1 -9 3 7 6.203 5.911 .236 o 1 -9 4 -7 3.563 3.552 .222 o 1 -9 4 -6 5.407 5.490 .207 o 1 -9 4 -5 3.894 3.819 .206 o 1 -9 4 -4 5.132 5.288 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2.286 1.965 .253 o 1 5 5 -9 2.463 2.393 .250 o 1 5 5 -8 1.035 1.201 .429 < 1 5 5 -7 4.036 4.285 .176 o 1 5 5 -6 .722 .953 .369 < 1 5 5 -5 3.743 3.743 .177 o 1 5 5 -4 10.648 10.573 .194 o 1 5 5 -3 22.212 21.519 .281 o 1 5 5 -2 11.834 11.409 .203 o 1 5 5 -1 4.287 3.964 .165 o 1 5 5 0 .737 .266 .378 < 1 5 5 1 4.636 4.731 .200 o 1 5 5 2 3.868 3.932 .225 o 1 5 5 3 1.318 1.470 .409 < 1 5 5 4 1.116 1.314 .472 < 1 5 6 -11 2.882 2.859 .271 o 1 5 6 -10 1.235 1.387 .417 < 1 5 6 -9 3.932 4.310 .195 o 1 5 6 -8 6.818 7.139 .193 o 1 5 6 -7 2.674 2.331 .216 o 1 5 6 -6 3.901 3.986 .196 o 1 5 6 -5 4.268 3.800 .199 o 1 5 6 -4 1.607 1.130 .228 o 1 5 6 -3 9.923 9.668 .206 o 1 5 6 -2 6.372 6.397 .196 o 1 5 6 -1 7.251 6.927 .202 o 1 5 6 0 10.904 10.641 .170 o 1 5 6 1 6.845 7.078 .219 o 1 5 6 2 1.171 1.464 .471 < 1 5 7 -10 3.592 3.541 .219 o 1 5 7 -9 6.549 7.126 .207 o 1 5 7 -8 7.371 7.980 .200 o 1 5 7 -7 4.180 4.065 .191 o 1 5 7 -6 2.093 2.382 .269 o 1 5 7 -5 1.465 1.074 .201 o 1 5 7 -4 .483 .555 .298 < 1 5 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14.813 14.024 .212 o 1 6 3 -1 6.334 7.110 .163 o 1 6 3 0 4.378 4.220 .125 o 1 6 3 1 2.206 2.024 .192 o 1 6 3 2 3.344 3.087 .185 o 1 6 3 3 2.040 2.033 .229 o 1 6 3 4 2.746 2.739 .216 o 1 6 3 5 5.665 5.933 .228 o 1 6 4 -7 2.248 2.677 .209 o 1 6 4 -6 4.126 4.249 .179 o 1 6 4 -5 2.586 3.307 .178 o 1 6 4 -4 16.957 16.837 .235 o 1 6 4 -3 18.158 17.304 .245 o 1 6 4 -2 9.844 9.584 .188 o 1 6 4 -1 2.030 1.792 .194 o 1 6 4 0 1.756 1.516 .172 o 1 6 4 1 4.714 4.564 .188 o 1 6 4 2 1.833 1.680 .222 o 1 6 4 3 .560 .006 .327 < 1 6 4 4 .475 .468 .314 < 1 6 5 -9 4.267 4.376 .202 o 1 6 5 -8 2.597 2.585 .233 o 1 6 5 -7 2.512 2.653 .224 o 1 6 5 -6 3.658 3.346 .191 o 1 6 5 -5 .456 .278 .310 < 1 6 5 -4 8.165 7.641 .183 o 1 6 5 -3 9.950 9.539 .196 o 1 6 5 -2 4.081 3.693 .179 o 1 6 5 -1 2.925 2.961 .216 o 1 6 5 0 8.299 8.483 .143 o 1 6 5 1 11.893 11.780 .229 o 1 6 5 2 1.303 1.714 .426 < 1 6 5 3 3.234 3.250 .220 o 1 6 6 -10 3.216 3.056 .225 o 1 6 6 -9 6.450 7.058 .227 o 1 6 6 -8 8.969 8.862 .224 o 1 6 6 -7 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