#------------------------------------------------------------------------------ #$Date: 2016-03-21 04:06:01 +0000 (Mon, 21 Mar 2016) $ #$Revision: 178490 $ #$URL: svn://www.crystallography.net/cod/cif/4/06/01/4060133.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_4060133 loop_ _publ_author_name 'Rainer Vollmerhaus' 'Robert Tomaszewski' 'Pengcheng Shao' 'Nicholas J. Taylor' 'Kevin J. Wiacek' 'Stewart P. Lewis' 'Abdulaziz Al-Humydi' 'Scott Collins' _journal_name_full Organometallics _journal_paper_doi 10.1021/om0492350 _journal_year 2005 _chemical_formula_sum 'C33 H27 F10 N4 P Zr' _chemical_formula_weight 791.78 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary 'Patterson and Fourier' _atom_sites_solution_secondary difmap _cell_angle_alpha 97.448(4) _cell_angle_beta 102.867(7) _cell_angle_gamma 90.501(8) _cell_formula_units_Z 2 _cell_length_a 9.9455(14) _cell_length_b 12.7251(15) _cell_length_c 12.9468(14) _cell_measurement_reflns_used 25 _cell_measurement_temperature 160(2) _cell_measurement_theta_max 15.78 _cell_measurement_theta_min 10.58 _cell_volume 1582.7(3) _diffrn_ambient_temperature 160(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method Omega _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 6592 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.10 _diffrn_standards_decay_% +/-2% _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.489 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'Face-indexed analytical' _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 796 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _refine_ls_extinction_coef 0.00100(12) _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 1.545 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 447 _refine_ls_number_reflns 6214 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.545 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0248 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.0515 _reflns_number_gt 5274 _reflns_number_total 6214 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'Integration' changed to 'integration' 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_original_sg_symbol_H-M P-1 _cod_database_code 4060133 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Zr1 Zr 0.629925(19) 0.454751(14) 0.291775(14) 0.01803(6) Uani 1 1 d . . . P1 P 0.63752(5) 0.22771(4) 0.20484(4) 0.01765(10) Uani 1 1 d . . . F1 F 0.48691(11) 0.42135(8) 0.36771(8) 0.0269(3) Uani 1 1 d . . . F2 F 0.68756(11) 0.47919(8) 0.15862(8) 0.0251(2) Uani 1 1 d . . . N1 N 0.73987(15) 0.30288(11) 0.30390(11) 0.0196(3) Uani 1 1 d . . . N2 N 0.52353(15) 0.31540(11) 0.17910(11) 0.0196(3) Uani 1 1 d . . . N3 N 0.41169(16) 0.51564(11) 0.17819(12) 0.0201(3) Uani 1 1 d . . . N4 N 0.99249(17) 0.20772(13) 0.27724(13) 0.0282(4) Uani 1 1 d . . . C1 C 0.8238(2) 0.51789(16) 0.45117(16) 0.0330(5) Uani 1 1 d . . . H1 H 0.8738 0.4652 0.4842 0.040 Uiso 1 1 calc R . . C2 C 0.8536(2) 0.56608(16) 0.36729(16) 0.0317(5) Uani 1 1 d . . . H2 H 0.9275 0.5514 0.3353 0.038 Uiso 1 1 calc R . . C3 C 0.7550(2) 0.63885(16) 0.34023(18) 0.0398(6) Uani 1 1 d . . . H3 H 0.7511 0.6821 0.2871 0.048 Uiso 1 1 calc R . . C4 C 0.6624(2) 0.63663(18) 0.4059(2) 0.0470(7) Uani 1 1 d . . . H4 H 0.5847 0.6773 0.4033 0.056 Uiso 1 1 calc R . . C5 C 0.7054(2) 0.5630(2) 0.47669(17) 0.0438(6) Uani 1 1 d . . . H5 H 0.6635 0.5471 0.5305 0.053 Uiso 1 1 calc R . . C6 C 0.71504(19) 0.18421(14) 0.09389(14) 0.0200(4) Uani 1 1 d . . . C7 C 0.8014(2) 0.25665(15) 0.06608(15) 0.0243(4) Uani 1 1 d . . . H7 H 0.8201 0.3234 0.1061 0.029 Uiso 1 1 calc R . . C8 C 0.8597(2) 0.23022(16) -0.02048(16) 0.0307(5) Uani 1 1 d . . . H8 H 0.9180 0.2790 -0.0382 0.037 Uiso 1 1 calc R . . C9 C 0.8319(2) 0.13133(17) -0.08111(17) 0.0377(5) Uani 1 1 d . . . H9 H 0.8720 0.1134 -0.1391 0.045 Uiso 1 1 calc R . . C10 C 0.7450(2) 0.06004(17) -0.05511(18) 0.0417(6) Uani 1 1 d . . . H10 H 0.7255 -0.0062 -0.0961 0.050 Uiso 1 1 calc R . . C11 C 0.6860(2) 0.08583(16) 0.03174(17) 0.0334(5) Uani 1 1 d . . . H11 H 0.6268 0.0371 0.0485 0.040 Uiso 1 1 calc R . . C12 C 0.57879(19) 0.11402(14) 0.25445(14) 0.0213(4) Uani 1 1 d . . . C13 C 0.4665(2) 0.12581(16) 0.30203(16) 0.0302(5) Uani 1 1 d . . . H13 H 0.4186 0.1883 0.3009 0.036 Uiso 1 1 calc R . . C14 C 0.4262(2) 0.04413(18) 0.35111(18) 0.0406(6) Uani 1 1 d . . . H14 H 0.3511 0.0520 0.3829 0.049 Uiso 1 1 calc R . . C15 C 0.4964(2) -0.04825(18) 0.35298(19) 0.0417(6) Uani 1 1 d . . . H15 H 0.4673 -0.1033 0.3845 0.050 Uiso 1 1 calc R . . C16 C 0.6090(2) -0.05983(17) 0.30878(19) 0.0426(6) Uani 1 1 d . . . H16 H 0.6577 -0.1218 0.3121 0.051 Uiso 1 1 calc R . . C17 C 0.6505(2) 0.02114(15) 0.25882(18) 0.0338(5) Uani 1 1 d . . . H17 H 0.7267 0.0130 0.2282 0.041 Uiso 1 1 calc R . . C18 C 0.8263(2) 0.25489(14) 0.38658(14) 0.0223(4) Uani 1 1 d . . . C19 C 0.9505(2) 0.20719(15) 0.37446(15) 0.0254(4) Uani 1 1 d . . . C20 C 1.0255(2) 0.16015(16) 0.45921(16) 0.0319(5) Uani 1 1 d . . . C21 C 0.9814(2) 0.15596(17) 0.55210(16) 0.0354(5) Uani 1 1 d . . . C22 C 0.8617(2) 0.20289(17) 0.56433(16) 0.0324(5) Uani 1 1 d . . . C23 C 0.7865(2) 0.25158(16) 0.48205(15) 0.0277(4) Uani 1 1 d . . . C24 C 0.41076(18) 0.32723(13) 0.09893(14) 0.0180(4) Uani 1 1 d . . . C25 C 0.34958(18) 0.42691(14) 0.09679(14) 0.0189(4) Uani 1 1 d . . . C26 C 0.23217(19) 0.43733(14) 0.01840(15) 0.0218(4) Uani 1 1 d . . . C27 C 0.17569(19) 0.35514(15) -0.05983(15) 0.0241(4) Uani 1 1 d . . . C28 C 0.2342(2) 0.25822(15) -0.05827(15) 0.0253(4) Uani 1 1 d . . . C29 C 0.3483(2) 0.24520(14) 0.02016(15) 0.0226(4) Uani 1 1 d . . . F20 F 1.14664(13) 0.11646(11) 0.45285(10) 0.0510(4) Uani 1 1 d . . . F21 F 1.05698(15) 0.10858(11) 0.63219(10) 0.0517(4) Uani 1 1 d . . . F22 F 0.81665(15) 0.20050(11) 0.65479(10) 0.0500(4) Uani 1 1 d . . . F23 F 0.66759(12) 0.29462(10) 0.49661(9) 0.0395(3) Uani 1 1 d . . . F26 F 0.16665(11) 0.52940(8) 0.01564(9) 0.0291(3) Uani 1 1 d . . . F27 F 0.06432(11) 0.36984(9) -0.13668(9) 0.0329(3) Uani 1 1 d . . . F28 F 0.18036(13) 0.17598(9) -0.13316(9) 0.0384(3) Uani 1 1 d . . . F29 F 0.40277(12) 0.14819(8) 0.02181(9) 0.0335(3) Uani 1 1 d . . . C30 C 0.4492(2) 0.60697(14) 0.12621(16) 0.0288(5) Uani 1 1 d . . . H30X H 0.5134 0.5847 0.0831 0.043 Uiso 1 1 calc R . . H30Y H 0.4906 0.6640 0.1803 0.043 Uiso 1 1 calc R . . H30Z H 0.3675 0.6307 0.0819 0.043 Uiso 1 1 calc R . . C31 C 0.3114(2) 0.55098(16) 0.24513(16) 0.0307(5) Uani 1 1 d . . . H31X H 0.2323 0.5786 0.2014 0.046 Uiso 1 1 calc R . . H31Y H 0.3547 0.6052 0.3017 0.046 Uiso 1 1 calc R . . H31Z H 0.2829 0.4917 0.2752 0.046 Uiso 1 1 calc R . . C32 C 1.0764(3) 0.30028(19) 0.27279(19) 0.0467(6) Uani 1 1 d . . . H32X H 1.0321 0.3634 0.2947 0.070 Uiso 1 1 calc R . . H32Y H 1.0870 0.3008 0.2010 0.070 Uiso 1 1 calc R . . H32Z H 1.1655 0.2979 0.3198 0.070 Uiso 1 1 calc R . . C33 C 1.0392(2) 0.10832(18) 0.22857(17) 0.0414(6) Uani 1 1 d . . . H33X H 1.1350 0.1008 0.2600 0.062 Uiso 1 1 calc R . . H33Y H 1.0272 0.1093 0.1531 0.062 Uiso 1 1 calc R . . H33Z H 0.9859 0.0498 0.2408 0.062 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 Zr1 0.01865(10) 0.01797(9) 0.01704(9) -0.00087(7) 0.00488(7) 0.00283(7) P1 0.0192(2) 0.0166(2) 0.0178(2) 0.00174(19) 0.0058(2) 0.00272(19) F1 0.0257(6) 0.0347(6) 0.0230(6) 0.0047(5) 0.0103(5) 0.0044(5) F2 0.0300(6) 0.0243(6) 0.0233(6) 0.0033(5) 0.0108(5) 0.0027(5) N1 0.0198(8) 0.0203(8) 0.0176(8) 0.0011(6) 0.0030(7) 0.0040(6) N2 0.0216(8) 0.0166(7) 0.0189(8) 0.0007(6) 0.0018(7) 0.0027(6) N3 0.0222(8) 0.0180(8) 0.0200(8) 0.0008(6) 0.0056(7) 0.0028(6) N4 0.0258(9) 0.0342(10) 0.0246(9) 0.0007(7) 0.0071(7) 0.0088(8) C1 0.0316(12) 0.0331(12) 0.0273(11) 0.0003(9) -0.0057(9) -0.0053(10) C2 0.0265(11) 0.0337(12) 0.0327(12) -0.0071(9) 0.0089(9) -0.0082(9) C3 0.0489(15) 0.0226(11) 0.0396(13) -0.0021(10) -0.0038(12) -0.0074(10) C4 0.0345(13) 0.0360(13) 0.0556(16) -0.0278(12) -0.0023(12) 0.0070(11) C5 0.0402(14) 0.0646(16) 0.0214(11) -0.0207(11) 0.0117(10) -0.0207(12) C6 0.0217(10) 0.0198(9) 0.0193(9) 0.0013(7) 0.0067(8) 0.0030(8) C7 0.0268(11) 0.0195(9) 0.0280(10) 0.0044(8) 0.0083(9) 0.0046(8) C8 0.0343(12) 0.0287(11) 0.0365(12) 0.0098(9) 0.0204(10) 0.0065(9) C9 0.0481(14) 0.0411(13) 0.0294(12) -0.0003(10) 0.0229(11) 0.0075(11) C10 0.0545(15) 0.0327(12) 0.0389(13) -0.0132(10) 0.0234(12) -0.0062(11) C11 0.0403(13) 0.0260(11) 0.0356(12) -0.0050(9) 0.0179(10) -0.0072(10) C12 0.0215(10) 0.0233(10) 0.0193(9) 0.0045(8) 0.0038(8) 0.0007(8) C13 0.0259(11) 0.0363(12) 0.0327(11) 0.0127(9) 0.0108(9) 0.0083(9) C14 0.0323(12) 0.0562(15) 0.0426(14) 0.0231(12) 0.0187(11) 0.0048(11) C15 0.0408(14) 0.0432(13) 0.0479(14) 0.0273(11) 0.0124(12) -0.0012(11) C16 0.0446(14) 0.0287(12) 0.0612(16) 0.0217(11) 0.0168(12) 0.0082(11) C17 0.0324(12) 0.0271(11) 0.0492(14) 0.0138(10) 0.0193(11) 0.0086(9) C18 0.0240(10) 0.0201(9) 0.0206(10) 0.0000(8) 0.0018(8) 0.0021(8) C19 0.0244(10) 0.0255(10) 0.0233(10) -0.0013(8) 0.0016(8) 0.0023(8) C20 0.0278(11) 0.0352(12) 0.0291(11) 0.0009(9) 0.0005(9) 0.0133(9) C21 0.0405(13) 0.0368(12) 0.0244(11) 0.0083(9) -0.0048(10) 0.0093(10) C22 0.0368(13) 0.0383(12) 0.0224(11) 0.0067(9) 0.0059(9) 0.0037(10) C23 0.0261(11) 0.0326(11) 0.0239(10) 0.0029(9) 0.0049(9) 0.0062(9) C24 0.0179(9) 0.0194(9) 0.0180(9) 0.0045(7) 0.0056(8) -0.0009(7) C25 0.0189(9) 0.0202(9) 0.0197(9) 0.0042(7) 0.0079(8) 0.0003(8) C26 0.0191(10) 0.0225(10) 0.0265(10) 0.0091(8) 0.0076(8) 0.0034(8) C27 0.0179(10) 0.0332(11) 0.0209(10) 0.0087(8) 0.0007(8) -0.0019(8) C28 0.0254(11) 0.0268(10) 0.0216(10) -0.0003(8) 0.0030(8) -0.0078(8) C29 0.0258(10) 0.0172(9) 0.0250(10) 0.0038(8) 0.0057(8) 0.0020(8) F20 0.0389(8) 0.0729(10) 0.0390(8) 0.0092(7) 0.0020(6) 0.0334(7) F21 0.0578(9) 0.0620(9) 0.0334(7) 0.0206(7) -0.0025(7) 0.0240(7) F22 0.0557(9) 0.0732(10) 0.0273(7) 0.0214(7) 0.0136(6) 0.0141(8) F23 0.0355(7) 0.0608(8) 0.0274(6) 0.0116(6) 0.0141(6) 0.0192(6) F26 0.0247(6) 0.0273(6) 0.0361(7) 0.0101(5) 0.0049(5) 0.0088(5) F27 0.0217(6) 0.0439(7) 0.0300(6) 0.0113(5) -0.0040(5) -0.0010(5) F28 0.0382(7) 0.0342(7) 0.0327(7) -0.0068(5) -0.0065(6) -0.0062(6) F29 0.0379(7) 0.0180(6) 0.0376(7) -0.0018(5) -0.0033(6) 0.0023(5) C30 0.0294(11) 0.0197(10) 0.0355(12) 0.0077(9) 0.0013(9) 0.0001(9) C31 0.0279(11) 0.0357(12) 0.0281(11) -0.0001(9) 0.0078(9) 0.0128(9) C32 0.0488(15) 0.0524(15) 0.0401(14) -0.0015(11) 0.0175(12) -0.0059(12) C33 0.0395(13) 0.0498(14) 0.0326(12) -0.0041(11) 0.0079(11) 0.0220(11)