#------------------------------------------------------------------------------ #$Date: 2012-08-17 08:48:30 +0100 (Fri, 17 Aug 2012) $ #$Revision: 64510 $ #$URL: svn://www.crystallography.net/cod/cif/4/06/02/4060211.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4060211 loop_ _publ_author_name 'Eugene Y.-X. Chen' 'Richard E. Campbell' 'David D. Devore' 'D. Patrick Green' 'Bernie Link' 'Jorge Soto' 'David R. Wilson' 'Khalil A. Abboud' _publ_section_title ; Divalentansa-Zirconocenes: Stereoselective Synthesis and High Activity for Propylene Polymerization ; _journal_name_full 'Journal of the American Chemical Society' _journal_volume 126 _journal_page_first 42 _journal_page_last 43 _journal_year 2004 _chemical_formula_sum 'C28 H44 Cl2 P2 Zr' _chemical_formula_weight 604.69 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 94.356(1) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.1306(5) _cell_length_b 13.2410(7) _cell_length_c 24.7714(14) _cell_measurement_reflns_used 94 _cell_measurement_temperature 446(2) _cell_measurement_theta_max 28.0 _cell_measurement_theta_min 2.0 _cell_volume 2986.2(3) _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0866 _diffrn_reflns_av_sigmaI/netI 0.1118 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 19880 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 1.75 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.669 _exptl_absorpt_correction_T_max 0.9504 _exptl_absorpt_correction_T_min 0.8466 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'based on measured indexed crystal faces, SHELXTL (Bruker 1998)' _exptl_crystal_colour Purple _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plates _exptl_crystal_F_000 1264 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.30 _refine_ls_extinction_coef 0.00020(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.808 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 318 _refine_ls_number_reflns 6843 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 0.809 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0337 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0145P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.0664 _reflns_number_gt 3975 _reflns_number_total 6843 _reflns_threshold_expression I>2\s(I) _[local]_cod_cif_authors_sg_H-M 'P 21/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 ; _cod_database_code 4060211 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.24494(3) 0.861847(19) 0.386412(10) 0.02627(8) Uani 1 1 d . . . Cl1 Cl 0.43892(7) 0.73757(5) 0.37536(3) 0.03681(17) Uani 1 1 d . A . Cl2 Cl 0.04811(7) 0.88467(5) 0.31423(3) 0.04060(18) Uani 1 1 d . A . P1 P 0.07120(8) 0.68837(6) 0.39361(3) 0.03810(19) Uani 1 1 d . A . P2 P 0.41467(8) 0.96597(5) 0.31382(3) 0.03187(17) Uani 1 1 d . A . C1 C 0.2884(4) 0.8510(2) 0.48456(11) 0.0532(8) Uani 1 1 d D A . H1A H 0.3580 0.9048 0.4957 0.064 Uiso 0.498(4) 1 calc PR A 1 H1B H 0.2061 0.8844 0.5005 0.064 Uiso 0.502(4) 1 d PR A 2 C2 C 0.1627(5) 0.8910(4) 0.4786(2) 0.0359(15) Uani 0.498(4) 1 d PD A 1 H2 H 0.0811 0.8486 0.4886 0.043 Uiso 0.498(4) 1 calc PR A 1 C3 C 0.1230(5) 0.9747(3) 0.44571(19) 0.0342(15) Uani 0.498(4) 1 d PD A 1 H3 H 0.0177 0.9858 0.4371 0.041 Uiso 0.498(4) 1 calc PR A 1 C2' C 0.3748(5) 0.9195(3) 0.47068(18) 0.0299(14) Uani 0.502(4) 1 d PD A 2 H2' H 0.4799 0.9037 0.4753 0.036 Uiso 0.502(4) 1 calc PR A 2 C3' C 0.3369(5) 1.0092(3) 0.44253(18) 0.0297(14) Uani 0.502(4) 1 d PD A 2 H3' H 0.4185 1.0472 0.4289 0.036 Uiso 0.502(4) 1 calc PR A 2 C4 C 0.2100(4) 1.0302(2) 0.42137(11) 0.0493(8) Uani 1 1 d D A . H4A H 0.2943 1.0470 0.4466 0.059 Uiso 0.498(4) 1 calc PR A 1 H4B H 0.1418 1.0246 0.4499 0.059 Uiso 0.502(4) 1 d PR A 2 C5 C 0.3296(4) 0.7611(2) 0.51824(11) 0.0478(8) Uani 1 1 d . . . C6 C 0.2434(4) 0.7275(2) 0.55894(11) 0.0564(9) Uani 1 1 d . A . H6A H 0.1599 0.7638 0.5661 0.068 Uiso 1 1 calc R . . C7 C 0.2790(4) 0.6421(3) 0.58864(13) 0.0709(10) Uani 1 1 d . . . H7A H 0.2189 0.6215 0.6152 0.085 Uiso 1 1 calc R A . C8 C 0.4013(5) 0.5869(3) 0.57972(14) 0.0745(11) Uani 1 1 d . A . H8A H 0.4241 0.5288 0.5997 0.089 Uiso 1 1 calc R . . C9 C 0.4903(4) 0.6190(2) 0.54060(13) 0.0649(10) Uani 1 1 d . . . H9A H 0.5740 0.5823 0.5341 0.078 Uiso 1 1 calc R A . C10 C 0.4562(4) 0.7057(2) 0.51083(12) 0.0535(9) Uani 1 1 d . A . H10A H 0.5191 0.7273 0.4854 0.064 Uiso 1 1 calc R . . C11 C 0.1678(3) 1.1213(2) 0.38907(11) 0.0420(7) Uani 1 1 d . . . C12 C 0.0335(3) 1.1297(2) 0.35868(12) 0.0493(8) Uani 1 1 d . A . H12A H -0.0352 1.0782 0.3605 0.059 Uiso 1 1 calc R . . C13 C -0.0010(4) 1.2122(3) 0.32589(13) 0.0575(9) Uani 1 1 d . . . H13A H -0.0909 1.2150 0.3056 0.069 Uiso 1 1 calc R A . C14 C 0.0979(4) 1.2903(2) 0.32322(13) 0.0594(9) Uani 1 1 d . A . H14A H 0.0755 1.3455 0.3009 0.071 Uiso 1 1 calc R . . C15 C 0.2282(4) 1.2862(2) 0.35344(13) 0.0537(9) Uani 1 1 d . . . H15A H 0.2945 1.3393 0.3521 0.064 Uiso 1 1 calc R A . C16 C 0.2637(4) 1.2032(2) 0.38645(12) 0.0480(8) Uani 1 1 d . A . H16A H 0.3530 1.2022 0.4072 0.058 Uiso 1 1 calc R . . C17 C -0.1192(3) 0.7092(3) 0.41046(14) 0.0671(10) Uani 1 1 d . . . H17A H -0.1710 0.7442 0.3804 0.081 Uiso 1 1 calc R A . H17B H -0.1657 0.6439 0.4136 0.081 Uiso 1 1 calc R . . C18 C -0.1394(4) 0.7669(3) 0.46027(16) 0.0998(15) Uani 1 1 d . A . H18A H -0.2424 0.7736 0.4648 0.150 Uiso 1 1 calc R . . H18B H -0.0964 0.8327 0.4576 0.150 Uiso 1 1 calc R . . H18C H -0.0926 0.7319 0.4908 0.150 Uiso 1 1 calc R . . C19 C 0.1471(3) 0.5875(2) 0.43763(11) 0.0499(8) Uani 1 1 d . . . H19A H 0.2478 0.5759 0.4293 0.060 Uiso 1 1 calc R A . H19B H 0.1498 0.6112 0.4748 0.060 Uiso 1 1 calc R . . C20 C 0.0669(4) 0.4870(2) 0.43437(13) 0.0626(10) Uani 1 1 d . A . H20A H 0.1161 0.4401 0.4591 0.094 Uiso 1 1 calc R . . H20B H 0.0662 0.4610 0.3982 0.094 Uiso 1 1 calc R . . H20C H -0.0322 0.4965 0.4438 0.094 Uiso 1 1 calc R . . C21 C 0.0319(3) 0.6246(2) 0.32825(12) 0.0478(8) Uani 1 1 d . . . H21A H -0.0369 0.5702 0.3332 0.057 Uiso 1 1 calc R A . H21B H -0.0164 0.6725 0.3031 0.057 Uiso 1 1 calc R . . C22 C 0.1639(3) 0.5812(2) 0.30249(12) 0.0524(8) Uani 1 1 d . A . H22A H 0.1320 0.5495 0.2687 0.079 Uiso 1 1 calc R . . H22B H 0.2113 0.5320 0.3263 0.079 Uiso 1 1 calc R . . H22C H 0.2317 0.6344 0.2961 0.079 Uiso 1 1 calc R . . C23 C 0.3094(3) 1.0535(2) 0.26790(11) 0.0401(7) Uani 1 1 d . . . H23A H 0.2212 1.0190 0.2535 0.048 Uiso 1 1 calc R A . H23B H 0.2785 1.1101 0.2892 0.048 Uiso 1 1 calc R . . C24 C 0.3872(3) 1.0953(2) 0.22051(11) 0.0532(9) Uani 1 1 d . A . H24A H 0.3222 1.1399 0.1996 0.080 Uiso 1 1 calc R . . H24B H 0.4153 1.0406 0.1981 0.080 Uiso 1 1 calc R . . H24C H 0.4733 1.1318 0.2339 0.080 Uiso 1 1 calc R . . C25 C 0.5689(3) 1.0425(2) 0.34283(12) 0.0447(8) Uani 1 1 d . . . H25A H 0.6256 1.0664 0.3138 0.054 Uiso 1 1 calc R A . H25B H 0.5307 1.1010 0.3606 0.054 Uiso 1 1 calc R . . C26 C 0.6706(3) 0.9833(2) 0.38383(13) 0.0625(9) Uani 1 1 d . A . H26A H 0.7493 1.0263 0.3977 0.094 Uiso 1 1 calc R . . H26B H 0.7103 0.9260 0.3663 0.094 Uiso 1 1 calc R . . H26C H 0.6156 0.9608 0.4131 0.094 Uiso 1 1 calc R . . C27 C 0.5037(3) 0.8831(2) 0.26717(11) 0.0430(8) Uani 1 1 d . . . H27A H 0.5627 0.9237 0.2445 0.052 Uiso 1 1 calc R A . H27B H 0.5693 0.8374 0.2879 0.052 Uiso 1 1 calc R . . C28 C 0.3953(4) 0.8217(2) 0.23139(12) 0.0562(9) Uani 1 1 d . A . H28A H 0.4477 0.7797 0.2078 0.084 Uiso 1 1 calc R . . H28B H 0.3314 0.8665 0.2101 0.084 Uiso 1 1 calc R . . H28C H 0.3381 0.7801 0.2535 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.03161(14) 0.02408(14) 0.02342(13) -0.00212(12) 0.00399(10) -0.00461(13) Cl1 0.0432(4) 0.0325(4) 0.0351(4) 0.0011(3) 0.0052(3) 0.0059(3) Cl2 0.0416(4) 0.0393(5) 0.0395(4) 0.0050(3) -0.0064(3) -0.0050(3) P1 0.0443(5) 0.0324(4) 0.0382(4) -0.0036(4) 0.0067(4) -0.0119(4) P2 0.0389(4) 0.0283(4) 0.0290(4) 0.0001(3) 0.0060(3) -0.0054(3) C1 0.102(3) 0.036(2) 0.0210(15) -0.0081(14) 0.0006(17) -0.004(2) C2 0.035(3) 0.046(4) 0.027(3) -0.007(3) 0.006(3) -0.002(3) C3 0.038(3) 0.035(4) 0.030(3) -0.012(3) 0.005(3) -0.002(3) C2' 0.043(3) 0.031(3) 0.015(3) -0.003(2) 0.002(2) -0.002(3) C3' 0.036(3) 0.033(3) 0.021(3) -0.010(2) 0.006(2) 0.000(3) C4 0.087(3) 0.0332(19) 0.0267(16) -0.0087(14) -0.0014(17) 0.0058(18) C5 0.082(2) 0.0373(19) 0.0230(16) -0.0029(14) -0.0066(15) -0.0085(17) C6 0.086(2) 0.057(2) 0.0257(17) 0.0013(16) -0.0051(16) -0.0111(19) C7 0.100(3) 0.070(3) 0.039(2) 0.009(2) -0.014(2) -0.030(2) C8 0.112(3) 0.061(3) 0.046(2) 0.025(2) -0.027(2) -0.028(2) C9 0.093(3) 0.047(2) 0.051(2) 0.0019(18) -0.0276(19) 0.0015(19) C10 0.079(2) 0.045(2) 0.0348(19) 0.0038(16) -0.0092(17) -0.0089(18) C11 0.0631(19) 0.0306(19) 0.0320(16) -0.0099(13) 0.0019(14) 0.0092(15) C12 0.0577(19) 0.0407(19) 0.0488(19) -0.0107(16) -0.0012(16) 0.0077(16) C13 0.067(2) 0.051(2) 0.051(2) -0.0173(18) -0.0162(17) 0.0214(19) C14 0.098(3) 0.032(2) 0.046(2) -0.0066(16) -0.006(2) 0.0172(19) C15 0.079(2) 0.0287(19) 0.051(2) -0.0068(15) -0.0088(19) 0.0032(16) C16 0.068(2) 0.0320(18) 0.0421(18) -0.0086(15) -0.0082(16) 0.0081(16) C17 0.064(2) 0.068(3) 0.072(3) -0.014(2) 0.020(2) -0.0206(19) C18 0.101(3) 0.101(4) 0.102(4) -0.012(3) 0.043(3) 0.003(3) C19 0.077(2) 0.0403(19) 0.0323(17) 0.0064(14) -0.0004(16) -0.0210(16) C20 0.093(3) 0.042(2) 0.054(2) 0.0002(17) 0.016(2) -0.0172(18) C21 0.0559(18) 0.0360(18) 0.0491(19) 0.0005(15) -0.0109(15) -0.0130(15) C22 0.078(2) 0.0383(19) 0.0418(19) -0.0065(15) 0.0100(17) -0.0112(17) C23 0.0494(17) 0.0348(18) 0.0363(16) 0.0051(13) 0.0036(14) -0.0047(14) C24 0.071(2) 0.045(2) 0.044(2) 0.0123(16) 0.0045(17) -0.0098(16) C25 0.0427(17) 0.0402(18) 0.052(2) -0.0098(15) 0.0074(15) -0.0088(14) C26 0.049(2) 0.060(2) 0.075(3) -0.0150(19) -0.0143(18) -0.0019(17) C27 0.0609(18) 0.0310(18) 0.0396(17) -0.0001(13) 0.0198(16) -0.0014(14) C28 0.090(2) 0.0406(19) 0.0384(19) -0.0049(15) 0.0083(17) -0.0070(17)