#------------------------------------------------------------------------------ #$Date: 2016-03-21 04:06:01 +0000 (Mon, 21 Mar 2016) $ #$Revision: 178490 $ #$URL: svn://www.crystallography.net/cod/cif/4/06/01/4060126.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_4060126 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 'C52 H48 Cl2 N4 P2 Ti' _chemical_formula_weight 909.68 _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 'Patterson and Fourier' _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.319(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.605(1) _cell_length_b 21.317(2) _cell_length_c 20.485(2) _cell_measurement_reflns_used 26 _cell_measurement_temperature 160(2) _cell_measurement_theta_max 15.85 _cell_measurement_theta_min 10.57 _cell_volume 4630.9(8) _diffrn_ambient_temperature 160(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'Siemens 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 0.0157 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 8606 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.14 _diffrn_standards_decay_% +/-2% _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.410 _exptl_absorpt_correction_T_max 0.8334 _exptl_absorpt_correction_T_min 0.8137 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'Face-indexed analytical' _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'Needle prism fragment' _exptl_crystal_F_000 1896 _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.52 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 2.415 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 550 _refine_ls_number_reflns 8138 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 2.415 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0333 _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^)+(0.0010P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.0681 _reflns_number_gt 6782 _reflns_number_total 8138 _reflns_threshold_expression >2sigma(I) _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. '_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 P2(1)/c _cod_database_code 4060126 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 Ti1 Ti 0.35947(3) 0.659553(15) 0.222783(16) 0.02630(9) Uani 1 1 d . . . Cl1 Cl 0.48542(5) 0.71367(2) 0.14648(2) 0.03771(13) Uani 1 1 d . . . Cl2 Cl 0.31701(5) 0.75428(2) 0.27892(2) 0.03777(13) Uani 1 1 d . . . P1 P 0.45739(5) 0.59057(2) 0.32503(2) 0.02365(11) Uani 1 1 d . . . P2 P 0.19026(5) 0.60140(2) 0.14069(2) 0.02970(12) Uani 1 1 d . . . N1 N 0.52145(14) 0.62642(7) 0.26370(7) 0.0250(4) Uani 1 1 d . . . N2 N 0.31489(15) 0.60914(7) 0.30502(7) 0.0255(4) Uani 1 1 d . . . N3 N 0.17862(15) 0.66093(7) 0.18981(7) 0.0303(4) Uani 1 1 d . . . N4 N 0.33701(15) 0.58832(7) 0.15550(7) 0.0265(4) Uani 1 1 d . . . C1 C 0.50377(18) 0.61795(8) 0.40458(9) 0.0244(4) Uani 1 1 d . . . C2 C 0.4919(2) 0.68208(9) 0.41721(10) 0.0338(5) Uani 1 1 d . . . H2 H 0.4717 0.7097 0.3836 0.041 Uiso 1 1 calc R . . C3 C 0.5105(2) 0.70427(9) 0.47989(10) 0.0391(5) Uani 1 1 d . . . H3 H 0.5012 0.7469 0.4884 0.047 Uiso 1 1 calc R . . C4 C 0.5426(2) 0.66394(9) 0.52997(10) 0.0366(5) Uani 1 1 d . . . H4 H 0.5545 0.6794 0.5720 0.044 Uiso 1 1 calc R . . C5 C 0.55707(19) 0.60085(9) 0.51766(9) 0.0340(5) Uani 1 1 d . . . H5 H 0.5806 0.5738 0.5512 0.041 Uiso 1 1 calc R . . C6 C 0.53654(18) 0.57766(9) 0.45533(9) 0.0284(4) Uani 1 1 d . . . H6 H 0.5447 0.5349 0.4474 0.034 Uiso 1 1 calc R . . C7 C 0.4902(2) 0.50750(8) 0.32251(9) 0.0291(5) Uani 1 1 d . . . C8 C 0.3943(2) 0.46588(9) 0.30664(9) 0.0376(5) Uani 1 1 d . . . H8 H 0.3126 0.4806 0.3001 0.045 Uiso 1 1 calc R . . C9 C 0.4198(3) 0.40279(10) 0.30051(11) 0.0562(7) Uani 1 1 d . . . H9 H 0.3548 0.3750 0.2908 0.067 Uiso 1 1 calc R . . C10 C 0.5399(3) 0.38085(11) 0.30853(11) 0.0616(8) Uani 1 1 d . . . H10 H 0.5566 0.3383 0.3032 0.074 Uiso 1 1 calc R . . C11 C 0.6368(3) 0.42141(11) 0.32447(11) 0.0563(7) Uani 1 1 d . . . H11 H 0.7209 0.4056 0.3301 0.068 Uiso 1 1 d R . . C12 C 0.6122(2) 0.48499(9) 0.33215(10) 0.0394(5) Uani 1 1 d . . . H12 H 0.6768 0.5124 0.3437 0.047 Uiso 1 1 calc R . . C13 C 0.65508(18) 0.62362(9) 0.24695(9) 0.0304(5) Uani 1 1 d . . . H13X H 0.6658 0.6381 0.2024 0.036 Uiso 1 1 calc R . . H13Y H 0.6832 0.5804 0.2491 0.036 Uiso 1 1 calc R . . C14 C 0.73598(18) 0.66286(9) 0.29176(9) 0.0319(5) Uani 1 1 d . . . C15 C 0.8264(2) 0.63624(11) 0.33166(10) 0.0402(5) Uani 1 1 d . . . H15 H 0.8403 0.5932 0.3301 0.048 Uiso 1 1 calc R . . C16 C 0.8973(2) 0.67317(14) 0.37433(11) 0.0551(7) Uani 1 1 d . . . H16 H 0.9573 0.6547 0.4014 0.066 Uiso 1 1 calc R . . C17 C 0.8784(2) 0.73653(14) 0.37629(12) 0.0590(7) Uani 1 1 d . . . H17 H 0.9257 0.7612 0.4047 0.071 Uiso 1 1 calc R . . C18 C 0.7895(3) 0.76391(12) 0.33630(12) 0.0581(7) Uani 1 1 d . . . H18 H 0.7773 0.8071 0.3375 0.070 Uiso 1 1 calc R . . C19 C 0.7178(2) 0.72725(10) 0.29412(11) 0.0448(6) Uani 1 1 d . . . H19 H 0.6575 0.7459 0.2674 0.054 Uiso 1 1 calc R . . C20 C 0.21017(19) 0.62224(9) 0.34956(10) 0.0363(5) Uani 1 1 d . . . H20X H 0.1357 0.6322 0.3239 0.044 Uiso 1 1 calc R . . H20Y H 0.2311 0.6590 0.3754 0.044 Uiso 1 1 calc R . . C21 C 0.17927(19) 0.56947(10) 0.39474(10) 0.0346(5) Uani 1 1 d . . . C22 C 0.2180(2) 0.56915(12) 0.45910(10) 0.0467(6) Uani 1 1 d . . . H22 H 0.2611 0.6035 0.4762 0.056 Uiso 1 1 calc R . . C23 C 0.1925(2) 0.51725(14) 0.49878(13) 0.0627(8) Uani 1 1 d . . . H23 H 0.2183 0.5174 0.5423 0.075 Uiso 1 1 calc R . . C24 C 0.1303(3) 0.46665(14) 0.47408(15) 0.0746(9) Uani 1 1 d . . . H24 H 0.1157 0.4319 0.5004 0.090 Uiso 1 1 calc R . . C25 C 0.0889(3) 0.46660(13) 0.41015(15) 0.0705(9) Uani 1 1 d . . . H25 H 0.0453 0.4323 0.3935 0.085 Uiso 1 1 calc R . . C26 C 0.1126(2) 0.51775(11) 0.37139(12) 0.0523(6) Uani 1 1 d . . . H26 H 0.0834 0.5179 0.3285 0.063 Uiso 1 1 calc R . . C27 C 0.1578(2) 0.61937(9) 0.05640(9) 0.0336(5) Uani 1 1 d . . . C28 C 0.0690(2) 0.58748(10) 0.01844(10) 0.0425(5) Uani 1 1 d . . . H28 H 0.0201 0.5560 0.0370 0.051 Uiso 1 1 calc R . . C29 C 0.0533(2) 0.60263(11) -0.04687(11) 0.0507(6) Uani 1 1 d . . . H29 H -0.0064 0.5816 -0.0721 0.061 Uiso 1 1 calc R . . C30 C 0.1265(2) 0.64894(11) -0.07447(11) 0.0526(7) Uani 1 1 d . . . H30 H 0.1165 0.6587 -0.1184 0.063 Uiso 1 1 calc R . . C31 C 0.2145(2) 0.68102(11) -0.03724(10) 0.0517(7) Uani 1 1 d . . . H31 H 0.2636 0.7123 -0.0560 0.062 Uiso 1 1 calc R . . C32 C 0.2292(2) 0.66627(10) 0.02827(10) 0.0437(6) Uani 1 1 d . . . H32 H 0.2875 0.6881 0.0535 0.052 Uiso 1 1 calc R . . C33 C 0.0880(2) 0.53721(10) 0.16499(10) 0.0356(5) Uani 1 1 d . . . C34 C -0.0427(2) 0.54294(11) 0.16470(11) 0.0500(6) Uani 1 1 d . . . H34 H -0.0805 0.5790 0.1482 0.060 Uiso 1 1 calc R . . C35 C -0.1170(2) 0.49423(13) 0.18927(13) 0.0623(8) Uani 1 1 d . . . H35 H -0.2044 0.4979 0.1890 0.075 Uiso 1 1 calc R . . C36 C -0.0612(3) 0.44099(13) 0.21379(12) 0.0603(8) Uani 1 1 d . . . H36 H -0.1111 0.4091 0.2306 0.072 Uiso 1 1 calc R . . C37 C 0.0677(3) 0.43445(11) 0.21372(10) 0.0492(6) Uani 1 1 d . . . H37 H 0.1049 0.3981 0.2299 0.059 Uiso 1 1 calc R . . C38 C 0.1423(2) 0.48275(9) 0.18913(9) 0.0380(5) Uani 1 1 d . . . H38 H 0.2295 0.4784 0.1889 0.046 Uiso 1 1 calc R . . C39 C 0.06101(19) 0.69283(9) 0.20774(9) 0.0336(5) Uani 1 1 d . . . H39X H 0.0780 0.7213 0.2437 0.040 Uiso 1 1 calc R . . H39Y H 0.0009 0.6618 0.2228 0.040 Uiso 1 1 calc R . . C40 C 0.0029(2) 0.72928(9) 0.15209(9) 0.0335(5) Uani 1 1 d . . . C41 C -0.1201(2) 0.71875(11) 0.13396(11) 0.0488(6) Uani 1 1 d . . . H41 H -0.1666 0.6890 0.1567 0.059 Uiso 1 1 calc R . . C42 C -0.1770(3) 0.75043(13) 0.08358(13) 0.0673(8) Uani 1 1 d . . . H42 H -0.2610 0.7429 0.0730 0.081 Uiso 1 1 calc R . . C43 C -0.1096(3) 0.79234(14) 0.04988(13) 0.0729(9) Uani 1 1 d . . . H43 H -0.1477 0.8134 0.0153 0.088 Uiso 1 1 calc R . . C44 C 0.0140(3) 0.80520(13) 0.06486(15) 0.0837(11) Uani 1 1 d . . . H44 H 0.0591 0.8346 0.0409 0.100 Uiso 1 1 calc R . . C45 C 0.0715(3) 0.77267(11) 0.11768(13) 0.0636(8) Uani 1 1 d . . . H45 H 0.1550 0.7807 0.1289 0.076 Uiso 1 1 calc R . . C46 C 0.43173(19) 0.56422(9) 0.10949(9) 0.0330(5) Uani 1 1 d . . . H46X H 0.5148 0.5691 0.1289 0.040 Uiso 1 1 calc R . . H46Y H 0.4292 0.5896 0.0702 0.040 Uiso 1 1 calc R . . C47 C 0.4136(2) 0.49646(9) 0.09084(10) 0.0364(5) Uani 1 1 d . . . C48 C 0.4651(3) 0.44898(11) 0.12769(12) 0.0588(7) Uani 1 1 d . . . H48 H 0.5138 0.4584 0.1643 0.071 Uiso 1 1 calc R . . C49 C 0.4441(3) 0.38576(13) 0.10992(17) 0.0860(11) Uani 1 1 d . . . H49 H 0.4793 0.3534 0.1344 0.103 Uiso 1 1 calc R . . C50 C 0.3714(4) 0.37271(15) 0.05635(19) 0.0940(13) Uani 1 1 d . . . H50 H 0.3555 0.3311 0.0454 0.113 Uiso 1 1 calc R . . C51 C 0.3222(3) 0.41887(14) 0.01883(16) 0.0767(9) Uani 1 1 d . . . H51 H 0.2745 0.4091 -0.0180 0.092 Uiso 1 1 calc R . . C52 C 0.3434(2) 0.48059(11) 0.03568(12) 0.0508(6) Uani 1 1 d . . . H52 H 0.3101 0.5123 0.0096 0.061 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 Ti1 0.0347(2) 0.02063(17) 0.02347(18) 0.00078(14) -0.00412(15) 0.00062(16) Cl1 0.0527(3) 0.0297(3) 0.0307(3) 0.0089(2) -0.0025(2) -0.0072(2) Cl2 0.0551(3) 0.0227(2) 0.0355(3) -0.0028(2) -0.0050(2) 0.0025(2) P1 0.0306(3) 0.0193(2) 0.0210(2) -0.00007(19) -0.0005(2) 0.0012(2) P2 0.0335(3) 0.0303(3) 0.0253(3) -0.0046(2) -0.0031(2) 0.0016(2) N1 0.0296(9) 0.0231(8) 0.0223(8) 0.0014(7) -0.0002(7) -0.0014(7) N2 0.0299(9) 0.0245(8) 0.0220(8) 0.0007(7) -0.0001(7) 0.0009(7) N3 0.0329(10) 0.0307(9) 0.0271(9) -0.0044(7) -0.0055(7) 0.0068(8) N4 0.0316(9) 0.0248(8) 0.0232(8) -0.0026(7) -0.0005(7) 0.0017(7) C1 0.0254(11) 0.0248(10) 0.0230(10) -0.0012(8) -0.0007(8) -0.0011(8) C2 0.0461(13) 0.0242(10) 0.0309(11) 0.0012(8) -0.0058(10) -0.0005(10) C3 0.0547(15) 0.0245(11) 0.0380(12) -0.0072(9) -0.0021(11) -0.0055(10) C4 0.0464(13) 0.0368(12) 0.0265(11) -0.0080(9) -0.0042(10) -0.0084(10) C5 0.0421(13) 0.0360(12) 0.0237(10) 0.0029(9) -0.0047(9) -0.0027(10) C6 0.0323(12) 0.0250(10) 0.0281(10) -0.0002(8) 0.0009(9) 0.0010(9) C7 0.0456(13) 0.0218(10) 0.0199(10) 0.0022(8) 0.0043(9) 0.0050(9) C8 0.0592(15) 0.0257(11) 0.0280(11) -0.0016(9) -0.0010(10) -0.0043(10) C9 0.107(2) 0.0252(12) 0.0369(13) -0.0033(10) 0.0018(14) -0.0098(14) C10 0.121(3) 0.0238(12) 0.0403(14) 0.0021(11) 0.0280(16) 0.0162(15) C11 0.079(2) 0.0411(14) 0.0488(15) 0.0149(12) 0.0292(14) 0.0307(14) C12 0.0488(14) 0.0341(12) 0.0354(12) 0.0099(10) 0.0115(10) 0.0098(11) C13 0.0331(12) 0.0305(11) 0.0276(10) 0.0011(9) 0.0037(9) 0.0010(9) C14 0.0278(11) 0.0402(12) 0.0278(11) 0.0032(9) 0.0065(9) -0.0029(10) C15 0.0307(12) 0.0578(14) 0.0323(12) 0.0004(11) 0.0056(10) 0.0028(11) C16 0.0319(14) 0.096(2) 0.0371(13) -0.0027(14) 0.0005(11) -0.0044(14) C17 0.0451(16) 0.087(2) 0.0446(15) -0.0162(14) -0.0003(12) -0.0274(15) C18 0.0649(18) 0.0489(15) 0.0605(17) -0.0101(13) 0.0074(14) -0.0196(14) C19 0.0464(15) 0.0420(13) 0.0459(13) 0.0005(11) -0.0041(11) -0.0079(11) C20 0.0338(13) 0.0393(12) 0.0358(12) 0.0035(10) 0.0050(10) 0.0081(10) C21 0.0290(12) 0.0431(12) 0.0318(11) 0.0020(9) 0.0085(9) 0.0072(10) C22 0.0296(13) 0.0752(17) 0.0352(13) 0.0043(12) 0.0047(10) 0.0085(12) C23 0.0409(16) 0.100(2) 0.0471(16) 0.0332(16) 0.0117(12) 0.0207(16) C24 0.068(2) 0.075(2) 0.081(2) 0.0361(18) 0.0373(18) 0.0152(17) C25 0.074(2) 0.0578(17) 0.080(2) 0.0012(16) 0.0399(18) -0.0127(15) C26 0.0549(16) 0.0568(16) 0.0453(14) -0.0032(12) 0.0154(12) -0.0120(13) C27 0.0401(13) 0.0330(11) 0.0278(11) -0.0068(9) -0.0062(10) 0.0084(10) C28 0.0444(14) 0.0482(13) 0.0348(12) -0.0098(10) -0.0067(10) 0.0026(11) C29 0.0544(16) 0.0595(16) 0.0379(13) -0.0131(12) -0.0189(12) 0.0045(13) C30 0.0741(19) 0.0529(15) 0.0307(12) -0.0037(11) -0.0156(12) 0.0137(14) C31 0.0765(19) 0.0435(13) 0.0349(13) 0.0060(11) -0.0137(13) -0.0019(13) C32 0.0577(15) 0.0390(13) 0.0341(12) -0.0013(10) -0.0161(11) -0.0024(12) C33 0.0368(13) 0.0412(13) 0.0290(11) -0.0122(9) 0.0039(9) -0.0051(10) C34 0.0427(15) 0.0522(15) 0.0552(15) -0.0225(12) 0.0074(12) -0.0007(12) C35 0.0424(15) 0.0709(19) 0.0738(19) -0.0392(16) 0.0268(14) -0.0188(14) C36 0.074(2) 0.0564(17) 0.0511(16) -0.0244(13) 0.0293(14) -0.0284(15) C37 0.0679(18) 0.0471(14) 0.0326(12) -0.0079(10) 0.0083(12) -0.0168(13) C38 0.0463(14) 0.0422(13) 0.0256(11) -0.0054(9) 0.0026(10) -0.0087(11) C39 0.0382(13) 0.0348(11) 0.0276(11) -0.0030(9) -0.0010(9) 0.0078(10) C40 0.0387(13) 0.0312(11) 0.0308(11) 0.0011(9) 0.0072(10) 0.0092(10) C41 0.0455(15) 0.0501(14) 0.0509(14) 0.0055(12) -0.0076(12) 0.0118(12) C42 0.068(2) 0.0728(19) 0.0614(18) 0.0027(15) -0.0164(15) 0.0199(16) C43 0.088(2) 0.084(2) 0.0473(16) 0.0179(15) 0.0090(16) 0.0422(19) C44 0.094(3) 0.0624(19) 0.096(2) 0.0434(17) 0.052(2) 0.0338(18) C45 0.0521(17) 0.0461(15) 0.093(2) 0.0248(15) 0.0187(15) 0.0148(13) C46 0.0353(12) 0.0307(11) 0.0331(11) -0.0011(9) 0.0044(9) 0.0001(9) C47 0.0402(13) 0.0317(11) 0.0374(12) -0.0040(10) 0.0173(10) 0.0014(10) C48 0.077(2) 0.0462(15) 0.0535(15) 0.0069(12) 0.0230(14) 0.0180(14) C49 0.112(3) 0.0422(17) 0.104(3) 0.0169(17) 0.045(2) 0.0209(18) C50 0.118(3) 0.0467(19) 0.117(3) -0.029(2) 0.050(3) -0.007(2) C51 0.075(2) 0.068(2) 0.088(2) -0.0427(18) 0.0228(18) -0.0156(17) C52 0.0507(16) 0.0489(14) 0.0528(15) -0.0215(12) 0.0130(12) -0.0035(12)