#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/01/2100158.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2100158 loop_ _publ_author_name 'Stash, Adam I.' 'Tanaka, Kiyoaki' 'Shiozawa, Kazunari' 'Makino, Hitoshi' 'Tsirelson, Vladimir G.' _publ_section_title ; Atomic interactions in ethylenebis(1-indenyl)zirconium dichloride as derived by experimental electron density analysis ; _journal_coeditor_code BS5015 _journal_issue 4 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 418 _journal_page_last 428 _journal_volume 61 _journal_year 2005 _chemical_formula_moiety 'C20 H16 Cl2 Zr' _chemical_formula_sum 'C20 H16 Cl2 Zr' _chemical_formula_weight 418.45 _chemical_name_systematic ; Ethylenebis(1-indenyl)zirconium dichloride ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 121.850(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.3870(5) _cell_length_b 10.5120(5) _cell_length_c 11.9270(5) _cell_measurement_reflns_used 40 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 35.0 _cell_measurement_theta_min 30.0 _cell_volume 1638.7(2) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.770 _diffrn_measured_fraction_theta_max 0.770 _diffrn_measurement_device_type 'MacScience four-circle' _diffrn_measurement_method \w/2\q? _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 10224 _diffrn_reflns_theta_full 49.97 _diffrn_reflns_theta_max 49.97 _diffrn_reflns_theta_min 2.49 _diffrn_standards_decay_% 1.5 _diffrn_standards_interval_count 30 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.992 _exptl_absorpt_correction_T_max 0.863 _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_type sphere _exptl_absorpt_process_details ; Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_description sphere _exptl_crystal_F_000 840 _exptl_crystal_size_rad 0.09 _refine_diff_density_max 1.368 _refine_diff_density_min -1.442 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 137 _refine_ls_number_reflns 6602 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.016 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0298 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+1.3284P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.0721 _reflns_number_gt 6151 _reflns_number_total 6602 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file bs5015.cif _[local]_cod_data_source_block zrsh _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2100158 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Zr 0.0000 0.271052(11) 0.2500 0.01012(2) Uani d S 1 . . Zr Cl -0.136622(17) 0.42390(2) 0.18359(2) 0.01786(4) Uani d . 1 . . Cl C1 -0.00110(7) 0.07448(8) 0.13263(9) 0.01541(12) Uani d . 1 . . C C2 -0.09921(7) 0.13235(10) 0.05610(9) 0.01863(14) Uani d . 1 . . C C3 -0.09025(8) 0.24789(10) 0.00163(9) 0.01878(15) Uani d . 1 . . C C3A 0.01377(7) 0.26199(9) 0.04028(8) 0.01545(12) Uani d . 1 . . C C4 0.06545(10) 0.35219(10) 0.00658(10) 0.02057(16) Uani d . 1 . . C C5 0.16749(10) 0.33535(11) 0.05609(12) 0.02325(18) Uani d . 1 . . C C6 0.22272(9) 0.23071(12) 0.13963(12) 0.02224(16) Uani d . 1 . . C C7 0.17584(8) 0.14142(10) 0.17323(10) 0.01779(13) Uani d . 1 . . C C7A 0.06909(7) 0.15477(8) 0.12271(8) 0.01380(11) Uani d . 1 . . C C8 0.02332(10) -0.04865(9) 0.20705(11) 0.02108(16) Uani d . 1 . . C H2 -0.1615(16) 0.102(2) 0.040(2) 0.029(5) Uiso d . 1 . . H H3 -0.1394(15) 0.301(2) -0.047(2) 0.025(5) Uiso d . 1 . . H H4 0.0289(15) 0.4190(19) -0.0500(19) 0.020(4) Uiso d . 1 . . H H5 0.2021(18) 0.390(2) 0.038(2) 0.039(6) Uiso d . 1 . . H H6 0.2965(17) 0.222(2) 0.169(2) 0.027(5) Uiso d . 1 . . H H7 0.2130(16) 0.070(2) 0.222(2) 0.028(5) Uiso d . 1 . . H H81 0.1003(15) -0.0621(19) 0.2686(19) 0.022(4) Uiso d . 1 . . H H82 0.0010(15) -0.118(2) 0.1477(19) 0.026(5) Uiso d . 1 . . H 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 0.00990(4) 0.01098(4) 0.00911(4) 0.000 0.00476(3) 0.000 Cl 0.01714(8) 0.02022(9) 0.01815(8) 0.00735(6) 0.01064(7) 0.00518(6) C1 0.0193(3) 0.0130(3) 0.0150(3) -0.0007(2) 0.0098(3) -0.0019(2) C2 0.0166(3) 0.0210(4) 0.0153(3) -0.0029(3) 0.0063(3) -0.0051(3) C3 0.0182(3) 0.0229(4) 0.0105(2) 0.0050(3) 0.0044(2) 0.0001(2) C3A 0.0210(3) 0.0149(3) 0.0115(2) 0.0032(2) 0.0093(2) 0.0012(2) C4 0.0350(5) 0.0151(3) 0.0189(3) 0.0030(3) 0.0192(4) 0.0025(3) C5 0.0342(5) 0.0204(4) 0.0270(4) -0.0036(4) 0.0243(4) -0.0019(3) C6 0.0233(4) 0.0247(4) 0.0262(4) -0.0007(3) 0.0182(3) -0.0026(4) C7 0.0192(3) 0.0184(3) 0.0185(3) 0.0044(3) 0.0118(3) 0.0008(3) C7A 0.0178(3) 0.0128(3) 0.0125(2) 0.0019(2) 0.0091(2) 0.0003(2) C8 0.0338(5) 0.0120(3) 0.0253(4) 0.0018(3) 0.0209(4) 0.0003(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zr Cl 2 2.4230(5) ? Zr Cl . 2.4230(5) ? Zr C2 . 2.4655(12) ? Zr C2 2 2.4655(12) ? Zr C1 . 2.4910(9) ? Zr C1 2 2.4910(9) ? Zr C3 . 2.5341(12) ? Zr C3 2 2.5341(12) ? Zr C7A 2 2.5754(9) ? Zr C7A . 2.5754(9) ? Zr C3A . 2.6210(9) ? Zr C3A 2 2.6210(9) ? C1 C2 . 1.4241(15) ? C1 C7A . 1.4240(13) ? C1 C8 . 1.5008(14) ? C2 C3 . 1.4180(16) ? C3 C3A . 1.4204(15) ? C3A C4 . 1.4250(14) ? C3A C7A . 1.4415(12) ? C4 C5 . 1.3664(18) ? C5 C6 . 1.4253(18) ? C6 C7 . 1.3664(15) ? C7 C7A . 1.4269(13) ? C8 C8 2 1.530(2) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle Cl Zr Cl 2 . 96.92(2) Cl Zr C2 2 . 134.40(3) Cl Zr C2 . . 94.85(4) Cl Zr C2 2 2 94.85(4) Cl Zr C2 . 2 134.40(3) C2 Zr C2 . 2 107.49(6) Cl Zr C1 2 . 118.76(3) Cl Zr C1 . . 128.24(3) C2 Zr C1 . . 33.39(3) C2 Zr C1 2 . 81.59(4) Cl Zr C1 2 2 128.24(3) Cl Zr C1 . 2 118.76(3) C2 Zr C1 . 2 81.59(4) C2 Zr C1 2 2 33.39(3) C1 Zr C1 . 2 67.90(4) Cl Zr C3 2 . 106.95(4) Cl Zr C3 . . 80.55(4) C2 Zr C3 . . 32.92(4) C2 Zr C3 2 . 136.54(4) C1 Zr C3 . . 54.99(3) C1 Zr C3 2 . 114.47(3) Cl Zr C3 2 2 80.55(4) Cl Zr C3 . 2 106.95(4) C2 Zr C3 . 2 136.54(4) C2 Zr C3 2 2 32.92(4) C1 Zr C3 . 2 114.47(3) C1 Zr C3 2 2 54.99(3) C3 Zr C3 . 2 168.97(5) Cl Zr C7A 2 2 132.75(3) Cl Zr C7A . 2 87.17(3) C2 Zr C7A . 2 91.63(3) C2 Zr C7A 2 2 53.86(3) C1 Zr C7A . 2 93.16(3) C1 Zr C7A 2 2 32.59(3) C3 Zr C7A . 2 120.10(4) C3 Zr C7A 2 2 53.65(3) Cl Zr C7A 2 . 87.17(3) Cl Zr C7A . . 132.75(3) C2 Zr C7A . . 53.86(3) C2 Zr C7A 2 . 91.63(3) C1 Zr C7A . . 32.59(3) C1 Zr C7A 2 . 93.16(3) C3 Zr C7A . . 53.65(3) C3 Zr C7A 2 . 120.10(4) C7A Zr C7A 2 . 123.33(4) Cl Zr C3A 2 . 80.97(3) Cl Zr C3A . . 101.84(3) C2 Zr C3A . . 53.50(3) C2 Zr C3A 2 . 123.49(3) C1 Zr C3A . . 54.09(3) C1 Zr C3A 2 . 121.75(3) C3 Zr C3A . . 31.93(3) C3 Zr C3A 2 . 147.32(3) C7A Zr C3A 2 . 144.26(3) C7A Zr C3A . . 32.20(3) Cl Zr C3A 2 2 101.84(3) Cl Zr C3A . 2 80.97(3) C2 Zr C3A . 2 123.49(3) C2 Zr C3A 2 2 53.50(3) C1 Zr C3A . 2 121.75(3) C1 Zr C3A 2 2 54.09(3) C3 Zr C3A . 2 147.32(3) C3 Zr C3A 2 2 31.93(3) C7A Zr C3A 2 2 32.20(3) C7A Zr C3A . 2 144.26(3) C3A Zr C3A . 2 175.83(4) C2 C1 C7A . . 106.71(8) C2 C1 C8 . . 126.68(9) C7A C1 C8 . . 126.60(9) C2 C1 Zr . . 72.32(6) C7A C1 Zr . . 76.97(5) C8 C1 Zr . . 117.24(6) C3 C2 C1 . . 109.46(9) C3 C2 Zr . . 76.20(6) C1 C2 Zr . . 74.29(6) C2 C3 C3A . . 107.82(8) C2 C3 Zr . . 70.88(5) C3A C3 Zr . . 77.41(6) C3 C3A C4 . . 132.75(9) C3 C3A C7A . . 107.37(8) C4 C3A C7A . . 119.74(9) C3 C3A Zr . . 70.66(6) C4 C3A Zr . . 125.68(6) C7A C3A Zr . . 72.16(5) C5 C4 C3A . . 118.48(9) C4 C5 C6 . . 121.83(10) C7 C6 C5 . . 121.52(10) C6 C7 C7A . . 118.48(9) C1 C7A C7 . . 131.38(8) C1 C7A C3A . . 108.62(8) C7 C7A C3A . . 119.92(8) C1 C7A Zr . . 70.44(5) C7 C7A Zr . . 122.61(6) C3A C7A Zr . . 75.64(5) C1 C8 C8 . 2 109.67(7)