# CIF-file generated for KUNB 4320-133 # Compound 1 #=================================================================== data_global #=================================================================== # 0. AUDIT DETAILS _audit_creation_date 5-Nov-03 _audit_creation_method 'PLATON option' _audit_update_record ; 5-Nov-03 Updated by the Author E.H. Textwriting by E.H. Checkcif OK 8-Dez-04 Updated by the Author E.H. 4-Mar-05 Updated by the Author E.H. ; #=================================================================== # 1. SUBMISSION DETAILS #=================================================================== # Name and address of author for X-ray correspondence _publ_contact_author ; Dr. Eberhardt Herdtweck, Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; _publ_contact_author_email 'eberhardt.herdtweck@ch.tum.de' _publ_contact_author_fax ' +49(0)89 289 13473' _publ_contact_author_phone '+49(0)89 289 13143' _publ_requested_journal 'Organometallics' # Publication choise FI FM FO CI CM CO _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission: March 2005 ; #=================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE 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 ; Cycloheptatrienyl-Cyclopentadienlyl-Zirconium Sandwich Complexes: Structure and Bonding ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Tamm, M.' ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; 'Kunst, A.' ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; 'Bannenberg, T.' ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; 'Herdtweck, E.' ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; 'Schmid, R.' ; Lehrstuhl f\"ur Anorganische Chemie II, Ruhr-Universit\"at Bochum, Organometallics & Materials Chemistry, Universit\"atsstrasse 150 D-44780 Bochum, Germany. ; #===================================================================== # 4. TEXT #===================================================================== _publ_section_synopsis ; ; _publ_section_abstract ; ... ; # Insert blank lines between paragraphs _publ_section_comment ; ; _publ_section_experimental ; ; # Insert blank lines between references _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436. Nonius (2001a). Data Collection Software for Nonius Kappa-CCD devices. Nonius BV, Delft, The Netherlands. Nonius (2001b). DENZO Processing Software for Nonius Kappa-CCD devices, Nonius BV, Delft, The Netherlands. Sheldrick, G. M. (1998). SHELXL97, University of G\"ottingen, G\"ottingen, Germany. Spek, A. L. (2001). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; _publ_section_table_legends ; ; #=================================================================== data_KUNB-4320-133 #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C12 H12 Zr' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H12 Zr' _chemical_formula_weight 247.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zr Zr -2.9673 0.5597 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,1/2-z -x,1/2+y,-z -x,-y,-z 1/2+x,y,1/2-z 1/2-x,1/2+y,1/2+z x,1/2-y,z _cell_length_a 11.1033(2) _cell_length_b 10.5715(2) _cell_length_c 8.2212(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 964.99(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(1) _cell_measurement_reflns_used 1059 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 25.39 _exptl_crystal_description 'fragment' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method none _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 1.084 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.723 _exptl_absorpt_correction_T_max 0.918 _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 40 s per film repetition 1 dx 40 566 films measured in 9 data sets set 1: phi-scan with delta_phi = 2.0 set 2 to 9 omega-scans with delta_omega = 2.0 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Straight forward after integration with the program NPROCESS, source: Nonius (2001b). Hydrogen atoms could be located in the difference Fourier maps and were allowed to refine freely. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 133(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 23575 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.0146 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.39 _reflns_number_total 935 _reflns_number_gt 897 # number of observed reflections (> n sig(I)) _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0099P)^2^+0.6089P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 935 _refine_ls_number_parameters 90 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0155 _refine_ls_R_factor_gt 0.0143 _refine_ls_wR_factor_ref 0.0338 _refine_ls_wR_factor_gt 0.0334 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.276 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.044 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Zr Zr Uani 0.13759(2) 0.25000 0.94639(2) 1.000 0.0164(1) . . C1 C Uani 0.3468(2) 0.25000 0.9525(3) 1.000 0.0297(8) . . C2 C Uani 0.30899(14) 0.12893(17) 0.8967(2) 1.000 0.0272(5) . . C3 C Uani 0.22363(14) 0.09904(15) 0.77399(19) 1.000 0.0237(5) . . C4 C Uani 0.15492(13) 0.18264(15) 0.67607(18) 1.000 0.0229(4) . . C5 C Uani 0.0870(2) 0.25000 1.2419(3) 1.000 0.0248(7) . . C6 C Uani 0.03087(14) 0.14208(15) 1.17553(18) 1.000 0.0232(5) . . C7 C Uani -0.05931(13) 0.18341(15) 1.06761(18) 1.000 0.0215(4) . . H11 H Uiso 0.397(2) 0.25000 1.042(3) 1.000 0.038(7) . . H21 H Uiso 0.3353(16) 0.0631(19) 0.955(2) 1.000 0.035(5) . . H31 H Uiso 0.2050(15) 0.0138(17) 0.761(2) 1.000 0.029(4) . . H41 H Uiso 0.0951(15) 0.1426(17) 0.611(2) 1.000 0.031(4) . . H51 H Uiso 0.149(2) 0.25000 1.309(3) 1.000 0.037(8) . . H61 H Uiso 0.0523(15) 0.0590(16) 1.1969(19) 1.000 0.028(5) . . H71 H Uiso -0.1078(15) 0.1347(18) 1.007(2) 1.000 0.028(5) . . 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 Zr 0.0152(1) 0.0203(1) 0.0137(1) 0.0000 0.0039(1) 0.0000 C1 0.0158(11) 0.0544(17) 0.0190(12) 0.0000 -0.0018(9) 0.0000 C2 0.0246(8) 0.0326(9) 0.0245(8) 0.0101(7) 0.0071(7) 0.0127(7) C3 0.0286(8) 0.0180(8) 0.0246(8) -0.0018(7) 0.0110(7) 0.0007(6) C4 0.0231(8) 0.0296(8) 0.0161(7) -0.0055(7) 0.0014(6) -0.0048(7) C5 0.0193(11) 0.0433(14) 0.0117(10) 0.0000 0.0024(9) 0.0000 C6 0.0254(8) 0.0226(8) 0.0216(8) 0.0070(7) 0.0101(6) 0.0029(6) C7 0.0168(7) 0.0260(8) 0.0216(8) -0.0034(7) 0.0049(6) -0.0060(6) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 C1 2.323(2) . . yes Zr C2 2.3295(16) . . yes Zr C3 2.3384(16) . . yes Zr C4 2.3416(15) . . yes Zr C5 2.494(2) . . yes Zr C6 2.5009(15) . . yes Zr C7 2.5037(15) . . yes C1 C2 1.423(2) . . no C2 C3 1.420(2) . . no C3 C4 1.418(2) . . no C4 C4 1.424(2) . 8_555 no C5 C6 1.410(2) . . no C6 C7 1.407(2) . . no C7 C7 1.408(2) . 8_555 no C1 H11 0.92(2) . . no C2 H21 0.894(19) . . no C3 H31 0.931(18) . . no C4 H41 0.952(17) . . no C5 H51 0.88(2) . . no C6 H61 0.927(17) . . no C7 H71 0.896(17) . . no 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 C1 Zr C2 35.61(5) . . . yes C1 Zr C3 66.71(6) . . . yes C1 Zr C4 86.47(7) . . . yes C1 Zr C5 101.78(8) . . . yes C1 Zr C6 117.22(6) . . . yes C1 Zr C7 149.82(6) . . . yes C1 Zr C2 35.61(5) . . 8_555 yes C1 Zr C3 66.71(6) . . 8_555 yes C1 Zr C4 86.47(7) . . 8_555 yes C1 Zr C6 117.22(6) . . 8_555 yes C1 Zr C7 149.82(6) . . 8_555 yes C2 Zr C3 35.41(6) . . . yes C2 Zr C4 66.38(5) . . . yes C2 Zr C5 110.79(6) . . . yes C2 Zr C6 105.58(6) . . . yes C2 Zr C7 128.95(6) . . . yes C2 Zr C2 66.65(6) . . 8_555 yes C2 Zr C3 86.27(6) . . 8_555 yes C2 Zr C4 86.19(6) . . 8_555 yes C2 Zr C6 140.34(5) . . 8_555 yes C2 Zr C7 159.66(6) . . 8_555 yes C3 Zr C4 35.28(5) . . . yes C3 Zr C5 133.04(4) . . . yes C3 Zr C6 109.80(5) . . . yes C3 Zr C7 113.96(5) . . . yes C2 Zr C3 86.27(6) 8_555 . . yes C3 Zr C3 86.07(5) . . 8_555 yes C3 Zr C4 66.34(5) . . 8_555 yes C3 Zr C6 164.04(5) . . 8_555 yes C3 Zr C7 142.17(5) . . 8_555 yes C4 Zr C5 160.60(4) . . . yes C4 Zr C6 127.96(5) . . . yes C4 Zr C7 111.35(5) . . . yes C2 Zr C4 86.19(6) 8_555 . . yes C3 Zr C4 66.34(5) 8_555 . . yes C4 Zr C4 35.41(5) . . 8_555 yes C4 Zr C6 153.20(5) . . 8_555 yes C4 Zr C7 122.35(5) . . 8_555 yes C5 Zr C6 32.79(4) . . . yes C5 Zr C7 54.23(6) . . . yes C2 Zr C5 110.79(6) 8_555 . . yes C3 Zr C5 133.04(4) 8_555 . . yes C4 Zr C5 160.60(4) 8_555 . . yes C5 Zr C6 32.79(4) . . 8_555 yes C5 Zr C7 54.23(6) . . 8_555 yes C6 Zr C7 32.67(5) . . . yes C2 Zr C6 140.34(5) 8_555 . . yes C3 Zr C6 164.04(5) 8_555 . . yes C4 Zr C6 153.20(5) 8_555 . . yes C6 Zr C6 54.28(5) . . 8_555 yes C6 Zr C7 54.17(5) . . 8_555 yes C2 Zr C7 159.66(6) 8_555 . . yes C3 Zr C7 142.17(5) 8_555 . . yes C4 Zr C7 122.35(5) 8_555 . . yes C6 Zr C7 54.17(5) 8_555 . . yes C7 Zr C7 32.66(5) . . 8_555 yes C2 Zr C3 35.41(6) 8_555 . 8_555 yes C2 Zr C4 66.38(5) 8_555 . 8_555 yes C2 Zr C6 105.58(6) 8_555 . 8_555 yes C2 Zr C7 128.95(6) 8_555 . 8_555 yes C3 Zr C4 35.28(5) 8_555 . 8_555 yes C3 Zr C6 109.80(5) 8_555 . 8_555 yes C3 Zr C7 113.96(5) 8_555 . 8_555 yes C4 Zr C6 127.96(5) 8_555 . 8_555 yes C4 Zr C7 111.35(5) 8_555 . 8_555 yes C6 Zr C7 32.67(5) 8_555 . 8_555 yes Zr C1 C2 72.43(11) . . . yes Zr C1 C2 72.43(11) . . 8_555 yes C2 C1 C2 128.17(19) . . 8_555 no Zr C2 C1 71.96(11) . . . yes Zr C2 C3 72.63(9) . . . yes C1 C2 C3 128.77(16) . . . no Zr C3 C2 71.95(9) . . . yes Zr C3 C4 72.48(9) . . . yes C2 C3 C4 128.59(15) . . . no Zr C4 C3 72.24(9) . . . yes Zr C4 C4 72.30(9) . . 8_555 yes C3 C4 C4 128.55(14) . . 8_555 no Zr C5 C6 73.89(11) . . . yes Zr C5 C6 73.89(11) . . 8_555 yes C6 C5 C6 108.04(18) . . 8_555 no Zr C6 C5 73.32(11) . . . yes Zr C6 C7 73.78(9) . . . yes C5 C6 C7 107.89(14) . . . no Zr C7 C6 73.56(9) . . . yes Zr C7 C7 73.67(8) . . 8_555 yes C6 C7 C7 108.09(13) . . 8_555 no Zr C1 H11 128.4(14) . . . no C2 C1 H11 115.79(13) . . . no C2 C1 H11 115.79(13) 8_555 . . no Zr C2 H21 126.9(11) . . . no C1 C2 H21 115.5(12) . . . no C3 C2 H21 115.2(12) . . . no Zr C3 H31 129.8(10) . . . no C2 C3 H31 116.4(10) . . . no C4 C3 H31 114.8(10) . . . no Zr C4 H41 127.7(10) . . . no C3 C4 H41 114.7(11) . . . no C4 C4 H41 116.4(11) 8_555 . . no Zr C5 H51 115.7(15) . . . no C6 C5 H51 125.94(11) . . . no C6 C5 H51 125.94(11) 8_555 . . no Zr C6 H61 117.0(10) . . . no C5 C6 H61 125.5(10) . . . no C7 C6 H61 126.6(10) . . . no Zr C7 H71 117.7(11) . . . no C6 C7 H71 126.8(12) . . . no C7 C7 H71 125.1(12) 8_555 . . no ### End # CIF-file generated for KUNA 4319-133 # Compound 2a #=================================================================== data_global #=================================================================== # 0. AUDIT DETAILS _audit_creation_date 6-Nov-03 _audit_creation_method 'PLATON
option' _audit_update_record ; 6-Nov-03 Updated by the Author E.H. Textwriting by E.H. Checkcif OK 8-Dez-04 Updated by the Author E.H. 4-Mar-05 Updated by the Author E.H. ; #=================================================================== # 1. SUBMISSION DETAILS #=================================================================== # Name and address of author for X-ray correspondence _publ_contact_author ; Dr. Eberhardt Herdtweck, Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; _publ_contact_author_email 'eberhardt.herdtweck@ch.tum.de' _publ_contact_author_fax ' +49(0)89 289 13473' _publ_contact_author_phone '+49(0)89 289 13143' _publ_requested_journal 'Organometallics' # Publication choise FI FM FO CI CM CO _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission: March 2005 ; #=================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE 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 ; Cycloheptatrienyl-Cyclopentadienlyl-Zirconium Sandwich Complexes: Structure and Bonding ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Tamm, M.' ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; 'Kunst, A.' ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; 'Bannenberg, T.' ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; 'Herdtweck, E.' ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; 'Schmid, R.' ; Lehrstuhl f\"ur Anorganische Chemie II, Ruhr-Universit\"at Bochum, Organometallics & Materials Chemistry, Universit\"atsstrasse 150 D-44780 Bochum, Germany. ; #===================================================================== # 4. TEXT #===================================================================== _publ_section_synopsis ; ; _publ_section_abstract ; ... ; # Insert blank lines between paragraphs _publ_section_comment ; ; _publ_section_experimental ; ; # Insert blank lines between references _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436. Nonius (2001a). Data Collection Software for Nonius Kappa-CCD devices. Nonius BV, Delft, The Netherlands. Nonius (2001b). DENZO Processing Software for Nonius Kappa-CCD devices, Nonius BV, Delft, The Netherlands. Sheldrick, G. M. (1998). SHELXL97, University of G\"ottingen, G\"ottingen, Germany. Spek, A. L. (2001). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; _publ_section_table_legends ; ; #=================================================================== data_KUNA-4319-133 #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C17 H21 N Zr' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H21 N Zr' _chemical_formula_weight 330.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zr Zr -2.9673 0.5597 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall '-P 2c 2b' _symmetry_space_group_name_H-M 'P b c m' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,1/2+z x,1/2-y,-z -x,1/2+y,1/2-z -x,-y,-z x,y,1/2-z -x,1/2+y,z x,1/2-y,1/2+z _cell_length_a 8.3304(1) _cell_length_b 18.5959(2) _cell_length_c 10.1241(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1568.34(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(1) _cell_measurement_reflns_used 1694 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.37 _exptl_crystal_description 'fragment' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method none _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.688 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.870 _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 15 s per film repetition 1 dx 40 1076 films measured in 9 data sets set 1: phi-scan with delta_phi = 1.0 set 2 to 9 omega-scans with delta_omega = 1.0 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Straight forward after integration with the program NPROCESS, source: Nonius (2001b). Hydrogen atoms could not be located in the difference Fourier maps and were calculated in ideal positions (riding model). ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 133(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 35406 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.0112 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.37 _reflns_number_total 1532 _reflns_number_gt 1456 # number of observed reflections (> n sig(I)) _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0207P)^2^+2.0911P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1532 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.524 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.058 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Zr Zr Uani 0.84401(3) 0.09908(1) 0.25000 1.000 0.0184(1) . . N N Uani 0.5941(3) 0.25197(13) 0.25000 1.000 0.0286(7) . . C1 C Uani 0.5712(4) 0.05300(19) 0.25000 1.000 0.084(3) . . C2 C Uani 0.6406(5) 0.04179(15) 0.1237(4) 1.000 0.0747(15) . . C3 C Uani 0.7867(5) 0.00976(16) 0.0957(3) 1.000 0.0664(12) . . C4 C Uani 0.8898(3) -0.02228(12) 0.1835(4) 1.000 0.0613(12) . . C5 C Uani 1.1455(4) 0.1057(2) 0.25000 1.000 0.081(2) . . C6 C Uani 1.0957(3) 0.14389(14) 0.1375(4) 1.000 0.0616(10) . . C7 C Uani 1.0154(3) 0.20510(11) 0.1810(2) 1.000 0.0362(7) . . C8 C Uani 0.6697(3) 0.20021(15) 0.25000 1.000 0.0279(9) . . C9 C Uani 0.5134(4) 0.32200(14) 0.25000 1.000 0.0260(8) . . C10 C Uani 0.6461(4) 0.37850(16) 0.25000 1.000 0.0391(10) . . C11 C Uani 0.4114(3) 0.32638(12) 0.1259(2) 1.000 0.0383(7) . . H11 H Uiso 0.46400 0.07030 0.25000 1.000 0.1000 calc R H21 H Uiso 0.58000 0.05810 0.05010 1.000 0.0900 calc R H31 H Uiso 0.81920 0.01000 0.00580 1.000 0.0800 calc R H41 H Uiso 0.97480 -0.04870 0.14410 1.000 0.0740 calc R H51 H Uiso 1.20300 0.06160 0.25000 1.000 0.0980 calc R H61 H Uiso 1.11350 0.13040 0.04820 1.000 0.0740 calc R H71 H Uiso 0.96860 0.24080 0.12610 1.000 0.0430 calc R H101 H Uiso 0.59810 0.42660 0.25000 1.000 0.0590 calc R H102 H Uiso 0.71270 0.37260 0.17100 0.500 0.0590 calc R H103 H Uiso 0.71270 0.37260 0.32900 0.500 0.0590 calc R H111 H Uiso 0.48000 0.32080 0.04800 1.000 0.0580 calc R H112 H Uiso 0.35740 0.37320 0.12250 1.000 0.0580 calc R H113 H Uiso 0.33080 0.28800 0.12720 1.000 0.0580 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 Zr 0.0180(2) 0.0139(2) 0.0235(2) 0.0000 0.0000 -0.0005(1) N 0.0257(12) 0.0179(11) 0.0423(15) 0.0000 0.0000 0.0033(11) C1 0.0115(16) 0.0155(17) 0.224(8) 0.0000 0.0000 -0.0026(13) C2 0.095(3) 0.0321(14) 0.097(3) 0.0295(16) -0.078(2) -0.0332(16) C3 0.120(3) 0.0484(17) 0.0309(14) -0.0151(13) 0.0199(18) -0.051(2) C4 0.0429(14) 0.0241(11) 0.117(3) -0.0298(14) 0.0352(16) -0.0078(10) C5 0.0171(18) 0.027(2) 0.200(7) 0.0000 0.0000 -0.0022(14) C6 0.0447(15) 0.0480(16) 0.092(2) -0.0281(16) 0.0425(17) -0.0249(13) C7 0.0363(12) 0.0283(11) 0.0440(12) 0.0047(10) 0.0066(11) -0.0137(9) C8 0.0252(15) 0.0190(14) 0.0395(17) 0.0000 0.0000 -0.0029(12) C9 0.0286(15) 0.0138(12) 0.0356(16) 0.0000 0.0000 0.0053(11) C10 0.0364(18) 0.0189(14) 0.062(2) 0.0000 0.0000 -0.0005(13) C11 0.0455(13) 0.0292(11) 0.0403(13) -0.0033(10) -0.0080(11) 0.0097(10) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== 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 C1 2.429(3) . . yes Zr C2 2.375(4) . . yes Zr C3 2.330(3) . . yes Zr C4 2.386(2) . . yes Zr C5 2.515(3) . . yes Zr C6 2.527(3) . . yes Zr C7 2.532(2) . . yes Zr C8 2.376(3) . . yes N C8 1.150(4) . . yes N C9 1.466(4) . . yes C1 C2 1.419(4) . . no C2 C3 1.384(6) . . no C3 C4 1.372(5) . . no C4 C4 1.347(6) . 6_555 no C5 C6 1.405(4) . . no C6 C7 1.392(4) . . no C7 C7 1.397(3) . 6_555 no C9 C10 1.525(4) . . no C9 C11 1.519(3) . . no C1 H11 0.9492 . . no C2 H21 0.9498 . . no C3 H31 0.9496 . . no C4 H41 0.9497 . . no C5 H51 0.9497 . . no C6 H61 0.9499 . . no C7 H71 0.9496 . . no C10 H101 0.9798 . . no C10 H102 0.9796 . . no C10 H103 0.9796 . . no C11 H111 0.9795 . . no C11 H112 0.9806 . . no C11 H113 0.9800 . . no 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 C1 Zr C2 34.33(10) . . . yes C1 Zr C3 63.68(11) . . . yes C1 Zr C4 79.39(10) . . . yes C1 Zr C5 162.14(12) . . . yes C1 Zr C6 153.20(9) . . . yes C1 Zr C7 143.34(9) . . . yes C1 Zr C8 72.99(10) . . . yes C1 Zr C2 34.33(10) . . 6_555 yes C1 Zr C3 63.68(11) . . 6_555 yes C1 Zr C4 79.39(10) . . 6_555 yes C1 Zr C6 153.20(9) . . 6_555 yes C1 Zr C7 143.34(9) . . 6_555 yes C2 Zr C3 34.21(13) . . . yes C2 Zr C4 62.47(11) . . . yes C2 Zr C5 137.27(11) . . . yes C2 Zr C6 119.81(13) . . . yes C2 Zr C7 127.08(10) . . . yes C2 Zr C8 85.36(10) . . . yes C2 Zr C2 65.14(14) . . 6_555 yes C2 Zr C3 83.97(12) . . 6_555 yes C2 Zr C4 80.89(11) . . 6_555 yes C2 Zr C6 169.22(11) . . 6_555 yes C2 Zr C7 154.15(9) . . 6_555 yes C3 Zr C4 33.81(12) . . . yes C3 Zr C5 103.86(12) . . . yes C3 Zr C6 95.91(12) . . . yes C3 Zr C7 119.05(10) . . . yes C3 Zr C8 116.05(10) . . . yes C2 Zr C3 83.97(12) 6_555 . . yes C3 Zr C3 84.22(11) . . 6_555 yes C3 Zr C4 63.10(12) . . 6_555 yes C3 Zr C6 135.01(12) . . 6_555 yes C3 Zr C7 148.82(10) . . 6_555 yes C4 Zr C5 83.49(10) . . . yes C4 Zr C6 92.98(9) . . . yes C4 Zr C7 124.64(9) . . . yes C4 Zr C8 147.83(9) . . . yes C2 Zr C4 80.89(11) 6_555 . . yes C3 Zr C4 63.10(12) 6_555 . . yes C4 Zr C4 32.78(13) . . 6_555 yes C4 Zr C6 107.84(9) . . 6_555 yes C4 Zr C7 136.39(8) . . 6_555 yes C5 Zr C6 32.36(9) . . . yes C5 Zr C7 53.04(10) . . . yes C5 Zr C8 124.87(11) . . . yes C2 Zr C5 137.27(11) 6_555 . . yes C3 Zr C5 103.86(12) 6_555 . . yes C4 Zr C5 83.49(10) 6_555 . . yes C5 Zr C6 32.36(9) . . 6_555 yes C5 Zr C7 53.04(10) . . 6_555 yes C6 Zr C7 31.93(8) . . . yes C6 Zr C8 104.25(8) . . . yes C2 Zr C6 169.22(11) 6_555 . . yes C3 Zr C6 135.01(12) 6_555 . . yes C4 Zr C6 107.84(9) 6_555 . . yes C6 Zr C6 53.57(12) . . 6_555 yes C6 Zr C7 53.13(9) . . 6_555 yes C7 Zr C8 74.24(8) . . . yes C2 Zr C7 154.15(9) 6_555 . . yes C3 Zr C7 148.82(10) 6_555 . . yes C4 Zr C7 136.39(8) 6_555 . . yes C6 Zr C7 53.13(9) 6_555 . . yes C7 Zr C7 32.03(7) . . 6_555 yes C2 Zr C8 85.36(10) 6_555 . . yes C3 Zr C8 116.05(10) 6_555 . . yes C4 Zr C8 147.83(9) 6_555 . . yes C6 Zr C8 104.25(8) 6_555 . . yes C7 Zr C8 74.24(8) 6_555 . . yes C2 Zr C3 34.21(13) 6_555 . 6_555 yes C2 Zr C4 62.47(11) 6_555 . 6_555 yes C2 Zr C6 119.81(13) 6_555 . 6_555 yes C2 Zr C7 127.08(10) 6_555 . 6_555 yes C3 Zr C4 33.81(12) 6_555 . 6_555 yes C3 Zr C6 95.91(12) 6_555 . 6_555 yes C3 Zr C7 119.05(10) 6_555 . 6_555 yes C4 Zr C6 92.98(9) 6_555 . 6_555 yes C4 Zr C7 124.64(9) 6_555 . 6_555 yes C6 Zr C7 31.93(8) 6_555 . 6_555 yes C8 N C9 174.1(3) . . . yes Zr C1 C2 70.8(2) . . . yes Zr C1 C2 70.8(2) . . 6_555 yes C2 C1 C2 128.7(3) . . 6_555 no Zr C2 C1 74.9(2) . . . yes Zr C2 C3 71.1(2) . . . yes C1 C2 C3 127.3(3) . . . no Zr C3 C2 74.7(2) . . . yes Zr C3 C4 75.34(18) . . . yes C2 C3 C4 127.2(3) . . . no Zr C4 C3 70.85(16) . . . yes Zr C4 C4 73.61(16) . . 6_555 yes C3 C4 C4 130.4(3) . . 6_555 no Zr C5 C6 74.32(17) . . . yes Zr C5 C6 74.32(17) . . 6_555 yes C6 C5 C6 108.3(3) . . 6_555 no Zr C6 C5 73.32(19) . . . yes Zr C6 C7 74.23(15) . . . yes C5 C6 C7 107.4(3) . . . no Zr C7 C6 73.83(14) . . . yes Zr C7 C7 73.99(13) . . 6_555 yes C6 C7 C7 108.4(2) . . 6_555 no Zr C8 N 175.5(2) . . . yes N C9 C10 106.2(3) . . . yes N C9 C11 107.71(15) . . . yes N C9 C11 107.71(15) . . 6_555 yes C10 C9 C11 111.63(15) . . . no C10 C9 C11 111.63(15) . . 6_555 no C11 C9 C11 111.6(2) . . 6_555 no Zr C1 H11 139.53 . . . no C2 C1 H11 115.67 . . . no C2 C1 H11 115.67 6_555 . . no Zr C2 H21 131.17 . . . no C1 C2 H21 116.33 . . . no C3 C2 H21 116.36 . . . no Zr C3 H31 125.52 . . . no C2 C3 H31 116.42 . . . no C4 C3 H31 116.39 . . . no Zr C4 H41 136.64 . . . no C3 C4 H41 114.79 . . . no C4 C4 H41 114.84 6_555 . . no Zr C5 H51 117.48 . . . no C6 C5 H51 125.83 . . . no C6 C5 H51 125.83 6_555 . . no Zr C6 H61 118.12 . . . no C5 C6 H61 126.30 . . . no C7 C6 H61 126.31 . . . no Zr C7 H71 118.31 . . . no C6 C7 H71 125.73 . . . no C7 C7 H71 125.83 6_555 . . no C9 C10 H101 109.46 . . . no C9 C10 H102 109.47 . . . no C9 C10 H103 109.47 . . . no H101 C10 H102 109.48 . . . no H101 C10 H103 109.48 . . . no H102 C10 H103 109.47 . . . no C9 C11 H111 109.51 . . . no C9 C11 H112 109.47 . . . no C9 C11 H113 109.46 . . . no H111 C11 H112 109.48 . . . no H111 C11 H113 109.48 . . . no H112 C11 H113 109.44 . . . no ### End of Crystallographic Information Files