# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Braunstein, Pierre' _publ_contact_author_email braunst@chimie.u-strasbg.fr _publ_section_title ; Electrophilic activation and the formation of an unusual Tl+/Cr3+ tetranuclear ion-complex adduct ; _publ_author_name P.Braunstein # Attachment '- C0CC00818D_ccdc_771851_771852_cif.txt' data_compound1 #TrackingRef '- C0CC00818D_ccdc_771851_771852_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 771851' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C18 H17 Cl3 Cr N2 P' _chemical_formula_sum 'C18 H17 Cl3 Cr N2 P' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour blue _diffrn_ambient_temperature 173(2) _chemical_formula_weight 450.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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' _cell_length_a 14.2128(5) _cell_length_b 13.4012(5) _cell_length_c 21.8650(7) _cell_angle_alpha 90.00 _cell_angle_beta 113.705(2) _cell_angle_gamma 90.00 _cell_volume 3813.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8304 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.48 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 1.108 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15041 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.1002 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8300 _reflns_number_gt 4637 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+0.0000P] 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_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8300 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1178 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cr1 Cr 0.51697(4) 0.68273(4) 0.84060(3) 0.02081(16) Uani 1 1 d . . . P1 P 0.59372(7) 0.73384(7) 0.95281(4) 0.0217(2) Uani 1 1 d . . . N1 N 0.5551(2) 0.5400(2) 0.88496(13) 0.0225(7) Uani 1 1 d . . . N2 N 0.6760(2) 0.6876(2) 0.85777(14) 0.0258(8) Uani 1 1 d . . . Cl1 Cl 0.46324(7) 0.63045(7) 0.72972(4) 0.0295(2) Uani 1 1 d . . . Cl2 Cl 0.50282(7) 0.85021(7) 0.81243(4) 0.0280(2) Uani 1 1 d . . . Cl3 Cl 0.35951(7) 0.66267(7) 0.84679(4) 0.0271(2) Uani 1 1 d . . . C1 C 0.6324(3) 0.6156(3) 0.99764(17) 0.0286(10) Uani 1 1 d . . . H1A H 0.7067 0.6140 1.0206 0.034 Uiso 1 1 calc R . . H1B H 0.6039 0.6116 1.0311 0.034 Uiso 1 1 calc R . . C2 C 0.5974(3) 0.5265(3) 0.95225(17) 0.0237(9) Uani 1 1 d . . . C3 C 0.6104(3) 0.4310(3) 0.97873(18) 0.0287(9) Uani 1 1 d . . . H3 H 0.6354 0.4225 1.0248 0.034 Uiso 1 1 calc R . . C4 C 0.5868(3) 0.3491(3) 0.93794(19) 0.0340(10) Uani 1 1 d . . . H4 H 0.5980 0.2852 0.9561 0.041 Uiso 1 1 calc R . . C5 C 0.5464(3) 0.3623(3) 0.8698(2) 0.0343(10) Uani 1 1 d . . . H5 H 0.5301 0.3078 0.8410 0.041 Uiso 1 1 calc R . . C6 C 0.5304(3) 0.4592(3) 0.84492(19) 0.0308(10) Uani 1 1 d . . . H6 H 0.5014 0.4686 0.7989 0.037 Uiso 1 1 calc R . . C7 C 0.7094(3) 0.7942(3) 0.95480(17) 0.0288(10) Uani 1 1 d . . . H7A H 0.6948 0.8632 0.9408 0.035 Uiso 1 1 calc R . . H7B H 0.7622 0.7931 0.9999 0.035 Uiso 1 1 calc R . . C8 C 0.7459(3) 0.7400(3) 0.90882(17) 0.0281(10) Uani 1 1 d . . . C9 C 0.8487(3) 0.7431(4) 0.9186(2) 0.0440(12) Uani 1 1 d . . . H9 H 0.8953 0.7808 0.9533 0.053 Uiso 1 1 calc R . . C10 C 0.8815(3) 0.6896(4) 0.8766(2) 0.0502(13) Uani 1 1 d . . . H10 H 0.9501 0.6912 0.8825 0.060 Uiso 1 1 calc R . . C11 C 0.8107(3) 0.6338(4) 0.8256(2) 0.0482(13) Uani 1 1 d . . . H11 H 0.8308 0.5961 0.7972 0.058 Uiso 1 1 calc R . . C12 C 0.7095(3) 0.6353(3) 0.81791(19) 0.0349(10) Uani 1 1 d . . . H12 H 0.6618 0.5983 0.7833 0.042 Uiso 1 1 calc R . . C13 C 0.5444(3) 0.8124(3) 0.99983(16) 0.0230(9) Uani 1 1 d . . . C14 C 0.4495(3) 0.8557(3) 0.97036(18) 0.0263(9) Uani 1 1 d . . . H14 H 0.4103 0.8454 0.9251 0.032 Uiso 1 1 calc R . . C15 C 0.4109(3) 0.9148(3) 1.00720(19) 0.0327(10) Uani 1 1 d . . . H15 H 0.3461 0.9436 0.9868 0.039 Uiso 1 1 calc R . . C16 C 0.4693(3) 0.9304(3) 1.07429(19) 0.0367(11) Uani 1 1 d . . . H16 H 0.4438 0.9693 1.0994 0.044 Uiso 1 1 calc R . . C17 C 0.5659(3) 0.8878(3) 1.10403(18) 0.0357(11) Uani 1 1 d . . . H17 H 0.6053 0.8986 1.1492 0.043 Uiso 1 1 calc R . . C18 C 0.6041(3) 0.8299(3) 1.06747(17) 0.0303(10) Uani 1 1 d . . . H18 H 0.6695 0.8025 1.0877 0.036 Uiso 1 1 calc R . . Cr1B Cr 0.00781(4) 0.68409(5) 0.64936(3) 0.02526(17) Uani 1 1 d . . . P1B P 0.14321(8) 0.71630(8) 0.61506(5) 0.0273(3) Uani 1 1 d . . . N1B N 0.0976(2) 0.7819(2) 0.72852(14) 0.0268(8) Uani 1 1 d . . . N2B N 0.1173(2) 0.5686(2) 0.69743(14) 0.0264(8) Uani 1 1 d . . . Cl1B Cl -0.10777(8) 0.64715(8) 0.69672(5) 0.0400(3) Uani 1 1 d . . . Cl2B Cl -0.06589(7) 0.57463(8) 0.56027(5) 0.0351(3) Uani 1 1 d . . . Cl3B Cl -0.08383(7) 0.82319(7) 0.59412(4) 0.0322(3) Uani 1 1 d . . . C1B C 0.2365(3) 0.7788(3) 0.68855(18) 0.0332(10) Uani 1 1 d . . . H1B1 H 0.2905 0.7321 0.7135 0.040 Uiso 1 1 calc R . . H1B2 H 0.2677 0.8335 0.6743 0.040 Uiso 1 1 calc R . . C2B C 0.1884(3) 0.8186(3) 0.73324(18) 0.0296(10) Uani 1 1 d . . . C3B C 0.2411(3) 0.8903(3) 0.7819(2) 0.0397(11) Uani 1 1 d . . . H3B H 0.3039 0.9150 0.7847 0.048 Uiso 1 1 calc R . . C4B C 0.2003(3) 0.9236(3) 0.8247(2) 0.0417(12) Uani 1 1 d . . . H4B H 0.2347 0.9715 0.8567 0.050 Uiso 1 1 calc R . . C5B C 0.1073(3) 0.8860(3) 0.82050(19) 0.0404(12) Uani 1 1 d . . . H5B H 0.0784 0.9070 0.8496 0.049 Uiso 1 1 calc R . . C6B C 0.0590(3) 0.8161(3) 0.77157(18) 0.0343(10) Uani 1 1 d . . . H6B H -0.0040 0.7912 0.7681 0.041 Uiso 1 1 calc R . . C7B C 0.1935(3) 0.5919(3) 0.61536(18) 0.0328(10) Uani 1 1 d . . . H7B1 H 0.1529 0.5576 0.5740 0.039 Uiso 1 1 calc R . . H7B2 H 0.2641 0.5954 0.6198 0.039 Uiso 1 1 calc R . . C8B C 0.1876(3) 0.5376(3) 0.67375(18) 0.0282(9) Uani 1 1 d . . . C9B C 0.2533(3) 0.4578(3) 0.70302(19) 0.0344(10) Uani 1 1 d . . . H9B H 0.3014 0.4376 0.6866 0.041 Uiso 1 1 calc R . . C10B C 0.2460(3) 0.4088(3) 0.7572(2) 0.0401(12) Uani 1 1 d . . . H10B H 0.2884 0.3546 0.7767 0.048 Uiso 1 1 calc R . . C11B C 0.1764(3) 0.4404(3) 0.7814(2) 0.0360(11) Uani 1 1 d . . . H11B H 0.1713 0.4087 0.8178 0.043 Uiso 1 1 calc R . . C12B C 0.1136(3) 0.5204(3) 0.75094(18) 0.0324(10) Uani 1 1 d . . . H12B H 0.0667 0.5422 0.7679 0.039 Uiso 1 1 calc R . . C13B C 0.1414(3) 0.7858(3) 0.54390(19) 0.0297(10) Uani 1 1 d . . . C14B C 0.1615(3) 0.7444(3) 0.49203(19) 0.0393(11) Uani 1 1 d . . . H14B H 0.1733 0.6762 0.4913 0.047 Uiso 1 1 calc R . . C15B C 0.1636(3) 0.8053(4) 0.44146(19) 0.0444(12) Uani 1 1 d . . . H15B H 0.1798 0.7780 0.4078 0.053 Uiso 1 1 calc R . . C16B C 0.1423(3) 0.9054(4) 0.4402(2) 0.0460(13) Uani 1 1 d . . . H16B H 0.1428 0.9451 0.4055 0.055 Uiso 1 1 calc R . . C17B C 0.1199(3) 0.9469(4) 0.4907(2) 0.0453(12) Uani 1 1 d . . . H17B H 0.1052 1.0146 0.4899 0.054 Uiso 1 1 calc R . . C18B C 0.1195(3) 0.8876(3) 0.5422(2) 0.0387(11) Uani 1 1 d . . . H18B H 0.1045 0.9157 0.5761 0.046 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 Cr1 0.0245(3) 0.0206(3) 0.0164(3) 0.0005(2) 0.0073(3) 0.0007(3) P1 0.0225(5) 0.0237(6) 0.0177(5) -0.0003(4) 0.0068(4) -0.0006(4) N1 0.0254(17) 0.0204(18) 0.0215(15) 0.0021(13) 0.0094(14) 0.0060(14) N2 0.0264(17) 0.032(2) 0.0198(16) 0.0035(14) 0.0104(14) 0.0070(15) Cl1 0.0362(5) 0.0311(6) 0.0188(4) -0.0023(4) 0.0085(4) 0.0009(5) Cl2 0.0340(5) 0.0230(5) 0.0259(5) 0.0033(4) 0.0111(4) -0.0005(4) Cl3 0.0249(5) 0.0301(6) 0.0254(5) 0.0007(4) 0.0092(4) -0.0008(4) C1 0.030(2) 0.032(2) 0.0205(19) 0.0021(17) 0.0073(17) 0.0039(19) C2 0.0193(19) 0.028(2) 0.025(2) 0.0009(17) 0.0102(16) 0.0037(18) C3 0.029(2) 0.031(2) 0.028(2) 0.0084(18) 0.0135(18) 0.0032(19) C4 0.034(2) 0.029(2) 0.042(2) 0.011(2) 0.018(2) 0.002(2) C5 0.040(2) 0.025(2) 0.039(2) -0.0015(19) 0.017(2) -0.002(2) C6 0.037(2) 0.024(2) 0.031(2) -0.0032(18) 0.0132(19) 0.001(2) C7 0.027(2) 0.033(2) 0.0247(19) -0.0032(17) 0.0084(17) -0.0032(19) C8 0.027(2) 0.035(3) 0.023(2) 0.0075(18) 0.0104(18) 0.0051(19) C9 0.030(2) 0.064(3) 0.037(2) 0.003(2) 0.012(2) -0.002(2) C10 0.032(2) 0.085(4) 0.039(2) -0.001(3) 0.019(2) 0.004(3) C11 0.041(3) 0.073(4) 0.039(3) 0.004(3) 0.024(2) 0.015(3) C12 0.035(2) 0.040(3) 0.030(2) -0.002(2) 0.0129(19) -0.001(2) C13 0.031(2) 0.021(2) 0.0209(18) 0.0022(16) 0.0145(17) -0.0040(18) C14 0.039(2) 0.021(2) 0.0233(19) 0.0013(16) 0.0170(18) 0.0009(19) C15 0.044(2) 0.023(2) 0.039(2) 0.0045(18) 0.025(2) 0.003(2) C16 0.063(3) 0.023(2) 0.042(2) -0.0049(19) 0.040(2) -0.006(2) C17 0.049(3) 0.039(3) 0.021(2) -0.0063(19) 0.016(2) -0.009(2) C18 0.036(2) 0.033(3) 0.025(2) -0.0027(18) 0.0146(19) -0.001(2) Cr1B 0.0265(3) 0.0253(4) 0.0235(3) 0.0018(3) 0.0094(3) 0.0015(3) P1B 0.0266(5) 0.0297(6) 0.0256(5) 0.0031(4) 0.0104(4) 0.0016(5) N1B 0.0262(18) 0.030(2) 0.0218(16) 0.0007(14) 0.0076(14) 0.0041(16) N2B 0.0266(18) 0.0260(19) 0.0221(16) 0.0019(14) 0.0052(14) -0.0006(15) Cl1B 0.0422(6) 0.0393(7) 0.0491(6) 0.0011(5) 0.0294(5) -0.0032(5) Cl2B 0.0349(6) 0.0341(6) 0.0293(5) -0.0043(4) 0.0057(4) 0.0010(5) Cl3B 0.0328(5) 0.0303(6) 0.0300(5) 0.0048(4) 0.0089(4) 0.0071(5) C1B 0.023(2) 0.039(3) 0.033(2) 0.0040(19) 0.0064(18) 0.0004(19) C2B 0.028(2) 0.027(2) 0.031(2) 0.0048(18) 0.0082(18) 0.0084(19) C3B 0.034(2) 0.028(3) 0.045(3) -0.002(2) 0.003(2) 0.002(2) C4B 0.044(3) 0.034(3) 0.033(2) -0.007(2) 0.000(2) 0.013(2) C5B 0.048(3) 0.037(3) 0.030(2) -0.002(2) 0.010(2) 0.014(2) C6B 0.034(2) 0.039(3) 0.032(2) 0.001(2) 0.0141(19) 0.009(2) C7B 0.036(2) 0.032(3) 0.033(2) 0.0008(19) 0.0169(19) 0.000(2) C8B 0.024(2) 0.026(2) 0.032(2) -0.0024(18) 0.0086(18) -0.0035(18) C9B 0.030(2) 0.028(2) 0.041(2) -0.001(2) 0.0100(19) 0.004(2) C10B 0.034(2) 0.028(3) 0.048(3) 0.012(2) 0.006(2) 0.002(2) C11B 0.037(2) 0.032(3) 0.036(2) 0.0076(19) 0.011(2) -0.006(2) C12B 0.032(2) 0.034(3) 0.030(2) -0.0011(19) 0.0113(19) -0.003(2) C13B 0.026(2) 0.030(2) 0.033(2) 0.0035(19) 0.0108(18) -0.0021(19) C14B 0.040(3) 0.042(3) 0.035(2) -0.003(2) 0.015(2) -0.006(2) C15B 0.047(3) 0.063(4) 0.025(2) -0.006(2) 0.016(2) -0.013(3) C16B 0.037(3) 0.062(4) 0.033(2) 0.012(2) 0.008(2) -0.009(3) C17B 0.038(3) 0.043(3) 0.054(3) 0.018(2) 0.017(2) 0.009(2) C18B 0.039(3) 0.043(3) 0.039(2) 0.009(2) 0.020(2) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N1 2.114(3) . ? Cr1 N2 2.138(3) . ? Cr1 Cl3 2.3116(11) . ? Cr1 Cl2 2.3147(11) . ? Cr1 Cl1 2.3372(10) . ? Cr1 P1 2.3510(10) . ? P1 C13 1.799(4) . ? P1 C7 1.817(4) . ? P1 C1 1.827(4) . ? N1 C6 1.347(5) . ? N1 C2 1.359(4) . ? N2 C12 1.345(5) . ? N2 C8 1.354(4) . ? C1 C2 1.504(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.386(5) . ? C3 C4 1.368(5) . ? C3 H3 0.9300 . ? C4 C5 1.376(5) . ? C4 H4 0.9300 . ? C5 C6 1.391(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.493(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.389(5) . ? C9 C10 1.387(6) . ? C9 H9 0.9300 . ? C10 C11 1.383(6) . ? C10 H10 0.9300 . ? C11 C12 1.380(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.369(5) . ? C13 C18 1.398(5) . ? C14 C15 1.390(5) . ? C14 H14 0.9300 . ? C15 C16 1.380(5) . ? C15 H15 0.9300 . ? C16 C17 1.384(6) . ? C16 H16 0.9300 . ? C17 C18 1.373(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? Cr1B N1B 2.137(3) . ? Cr1B N2B 2.147(3) . ? Cr1B Cl3B 2.3163(11) . ? Cr1B Cl1B 2.3202(12) . ? Cr1B Cl2B 2.3244(11) . ? Cr1B P1B 2.3690(12) . ? P1B C13B 1.805(4) . ? P1B C7B 1.812(4) . ? P1B C1B 1.825(4) . ? N1B C2B 1.345(5) . ? N1B C6B 1.347(5) . ? N2B C12B 1.356(5) . ? N2B C8B 1.361(5) . ? C1B C2B 1.498(6) . ? C1B H1B1 0.9700 . ? C1B H1B2 0.9700 . ? C2B C3B 1.405(5) . ? C3B C4B 1.361(6) . ? C3B H3B 0.9300 . ? C4B C5B 1.382(6) . ? C4B H4B 0.9300 . ? C5B C6B 1.379(5) . ? C5B H5B 0.9300 . ? C6B H6B 0.9300 . ? C7B C8B 1.501(5) . ? C7B H7B1 0.9700 . ? C7B H7B2 0.9700 . ? C8B C9B 1.395(5) . ? C9B C10B 1.394(6) . ? C9B H9B 0.9300 . ? C10B C11B 1.364(6) . ? C10B H10B 0.9300 . ? C11B C12B 1.383(5) . ? C11B H11B 0.9300 . ? C12B H12B 0.9300 . ? C13B C14B 1.391(5) . ? C13B C18B 1.396(6) . ? C14B C15B 1.385(6) . ? C14B H14B 0.9300 . ? C15B C16B 1.373(6) . ? C15B H15B 0.9300 . ? C16B C17B 1.381(6) . ? C16B H16B 0.9300 . ? C17B C18B 1.380(6) . ? C17B H17B 0.9300 . ? C18B H18B 0.9300 . ? 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_3 _geom_angle_publ_flag N1 Cr1 N2 83.64(12) . . ? N1 Cr1 Cl3 86.78(9) . . ? N2 Cr1 Cl3 166.74(8) . . ? N1 Cr1 Cl2 167.98(8) . . ? N2 Cr1 Cl2 89.40(9) . . ? Cl3 Cr1 Cl2 98.38(4) . . ? N1 Cr1 Cl1 96.97(8) . . ? N2 Cr1 Cl1 94.18(8) . . ? Cl3 Cr1 Cl1 96.06(4) . . ? Cl2 Cr1 Cl1 93.30(4) . . ? N1 Cr1 P1 81.89(8) . . ? N2 Cr1 P1 78.09(8) . . ? Cl3 Cr1 P1 91.53(4) . . ? Cl2 Cr1 P1 87.10(4) . . ? Cl1 Cr1 P1 172.26(5) . . ? C13 P1 C7 106.38(18) . . ? C13 P1 C1 107.65(17) . . ? C7 P1 C1 107.41(18) . . ? C13 P1 Cr1 130.03(12) . . ? C7 P1 Cr1 100.98(12) . . ? C1 P1 Cr1 102.74(12) . . ? C6 N1 C2 118.9(3) . . ? C6 N1 Cr1 118.5(2) . . ? C2 N1 Cr1 122.5(2) . . ? C12 N2 C8 118.1(3) . . ? C12 N2 Cr1 119.6(3) . . ? C8 N2 Cr1 122.3(3) . . ? C2 C1 P1 112.7(2) . . ? C2 C1 H1A 109.0 . . ? P1 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? P1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N1 C2 C3 120.1(3) . . ? N1 C2 C1 119.6(3) . . ? C3 C2 C1 120.3(3) . . ? C4 C3 C2 120.8(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 118.3(4) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? N1 C6 C5 122.5(3) . . ? N1 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? C8 C7 P1 108.9(3) . . ? C8 C7 H7A 109.9 . . ? P1 C7 H7A 109.9 . . ? C8 C7 H7B 109.9 . . ? P1 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? N2 C8 C9 121.4(4) . . ? N2 C8 C7 117.9(3) . . ? C9 C8 C7 120.7(4) . . ? C10 C9 C8 119.7(4) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 119.0(4) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C12 C11 C10 118.4(4) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? N2 C12 C11 123.5(4) . . ? N2 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? C14 C13 C18 119.4(4) . . ? C14 C13 P1 121.0(3) . . ? C18 C13 P1 119.5(3) . . ? C13 C14 C15 120.8(3) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 119.6(4) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 119.7(4) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C18 C17 C16 120.6(4) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C13 119.8(4) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? N1B Cr1B N2B 88.09(11) . . ? N1B Cr1B Cl3B 87.48(9) . . ? N2B Cr1B Cl3B 168.72(10) . . ? N1B Cr1B Cl1B 93.95(10) . . ? N2B Cr1B Cl1B 97.57(9) . . ? Cl3B Cr1B Cl1B 93.09(4) . . ? N1B Cr1B Cl2B 170.77(10) . . ? N2B Cr1B Cl2B 87.07(8) . . ? Cl3B Cr1B Cl2B 95.82(4) . . ? Cl1B Cr1B Cl2B 94.47(4) . . ? N1B Cr1B P1B 81.25(9) . . ? N2B Cr1B P1B 76.41(9) . . ? Cl3B Cr1B P1B 92.65(4) . . ? Cl1B Cr1B P1B 172.35(4) . . ? Cl2B Cr1B P1B 89.97(4) . . ? C13B P1B C7B 110.28(19) . . ? C13B P1B C1B 105.98(19) . . ? C7B P1B C1B 105.86(19) . . ? C13B P1B Cr1B 129.44(13) . . ? C7B P1B Cr1B 101.56(14) . . ? C1B P1B Cr1B 101.55(14) . . ? C2B N1B C6B 118.1(3) . . ? C2B N1B Cr1B 121.9(3) . . ? C6B N1B Cr1B 119.8(3) . . ? C12B N2B C8B 118.2(3) . . ? C12B N2B Cr1B 119.5(3) . . ? C8B N2B Cr1B 122.1(2) . . ? C2B C1B P1B 112.1(3) . . ? C2B C1B H1B1 109.2 . . ? P1B C1B H1B1 109.2 . . ? C2B C1B H1B2 109.2 . . ? P1B C1B H1B2 109.2 . . ? H1B1 C1B H1B2 107.9 . . ? N1B C2B C3B 120.7(4) . . ? N1B C2B C1B 119.7(3) . . ? C3B C2B C1B 119.5(4) . . ? C4B C3B C2B 120.0(4) . . ? C4B C3B H3B 120.0 . . ? C2B C3B H3B 120.0 . . ? C3B C4B C5B 119.6(4) . . ? C3B C4B H4B 120.2 . . ? C5B C4B H4B 120.2 . . ? C6B C5B C4B 117.7(4) . . ? C6B C5B H5B 121.1 . . ? C4B C5B H5B 121.1 . . ? N1B C6B C5B 123.9(4) . . ? N1B C6B H6B 118.1 . . ? C5B C6B H6B 118.1 . . ? C8B C7B P1B 107.0(3) . . ? C8B C7B H7B1 110.3 . . ? P1B C7B H7B1 110.3 . . ? C8B C7B H7B2 110.3 . . ? P1B C7B H7B2 110.3 . . ? H7B1 C7B H7B2 108.6 . . ? N2B C8B C9B 121.2(4) . . ? N2B C8B C7B 118.4(3) . . ? C9B C8B C7B 120.4(4) . . ? C10B C9B C8B 119.1(4) . . ? C10B C9B H9B 120.5 . . ? C8B C9B H9B 120.5 . . ? C11B C10B C9B 119.8(4) . . ? C11B C10B H10B 120.1 . . ? C9B C10B H10B 120.1 . . ? C10B C11B C12B 118.9(4) . . ? C10B C11B H11B 120.6 . . ? C12B C11B H11B 120.6 . . ? N2B C12B C11B 122.8(4) . . ? N2B C12B H12B 118.6 . . ? C11B C12B H12B 118.6 . . ? C14B C13B C18B 119.0(4) . . ? C14B C13B P1B 124.1(3) . . ? C18B C13B P1B 117.0(3) . . ? C15B C14B C13B 119.5(4) . . ? C15B C14B H14B 120.2 . . ? C13B C14B H14B 120.2 . . ? C16B C15B C14B 121.0(4) . . ? C16B C15B H15B 119.5 . . ? C14B C15B H15B 119.5 . . ? C15B C16B C17B 119.9(4) . . ? C15B C16B H16B 120.1 . . ? C17B C16B H16B 120.1 . . ? C16B C17B C18B 119.8(5) . . ? C16B C17B H17B 120.1 . . ? C18B C17B H17B 120.1 . . ? C17B C18B C13B 120.7(4) . . ? C17B C18B H18B 119.7 . . ? C13B C18B H18B 119.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.655 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.107 data_compound2 #TrackingRef '- C0CC00818D_ccdc_771851_771852_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 771852' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C18 H17 Cl3 Cr N2 P, F6 P, Tl' _chemical_formula_sum 'C18 H17 Cl3 Cr F6 N2 P2 Tl' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour purple _diffrn_ambient_temperature 173(2) _chemical_formula_weight 800.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9323(4) _cell_length_b 12.0205(5) _cell_length_c 12.8804(4) _cell_angle_alpha 72.356(2) _cell_angle_beta 71.627(2) _cell_angle_gamma 69.739(2) _cell_volume 1201.70(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8502 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.48 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 758 _exptl_absorpt_coefficient_mu 7.672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.720 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9090 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5504 _reflns_number_gt 4796 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+2.4071P] 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_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5504 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 Cr1 Cr 0.35775(11) 0.89124(8) 0.81129(7) 0.01741(19) Uani 1 1 d . . . Tl1 Tl -0.04110(3) 1.13700(2) 0.85450(2) 0.03227(11) Uani 1 1 d . . . P1 P 0.62128(17) 0.92090(14) 0.74242(12) 0.0190(3) Uani 1 1 d . . . P2 P 0.0113(2) 1.48683(16) 0.74275(15) 0.0286(3) Uani 1 1 d . . . N1 N 0.4790(6) 0.7510(4) 0.9281(4) 0.0193(9) Uani 1 1 d . . . N2 N 0.4571(6) 0.7739(4) 0.6971(4) 0.0205(10) Uani 1 1 d . . . Cl1 Cl 0.09956(17) 0.85024(14) 0.88259(12) 0.0254(3) Uani 1 1 d . . . Cl2 Cl 0.27078(19) 1.04824(14) 0.66824(12) 0.0276(3) Uani 1 1 d . . . Cl3 Cl 0.28699(18) 1.01711(14) 0.93559(12) 0.0258(3) Uani 1 1 d . . . F1 F 0.0517(6) 1.5710(5) 0.7987(5) 0.0548(13) Uani 1 1 d . . . F2 F 0.0465(7) 1.5749(6) 0.6236(4) 0.0634(15) Uani 1 1 d . . . F3 F -0.1767(5) 1.5652(5) 0.7656(4) 0.0485(11) Uani 1 1 d . . . F4 F -0.0279(8) 1.4007(6) 0.6889(5) 0.0677(16) Uani 1 1 d . . . F5 F -0.0249(6) 1.3980(5) 0.8622(4) 0.0536(12) Uani 1 1 d . . . F6 F 0.2005(5) 1.4115(5) 0.7197(5) 0.0548(13) Uani 1 1 d . . . C1 C 0.7189(7) 0.8320(6) 0.8570(5) 0.0250(12) Uani 1 1 d . . . H1A H 0.8313 0.7893 0.8266 0.030 Uiso 1 1 calc R . . H1B H 0.7219 0.8863 0.8983 0.030 Uiso 1 1 calc R . . C2 C 0.6311(7) 0.7418(6) 0.9354(5) 0.0241(12) Uani 1 1 d . . . C3 C 0.7055(8) 0.6538(6) 1.0154(6) 0.0316(14) Uani 1 1 d . . . H3 H 0.8118 0.6472 1.0166 0.038 Uiso 1 1 calc R . . C4 C 0.6209(9) 0.5759(6) 1.0935(6) 0.0350(15) Uani 1 1 d . . . H4 H 0.6677 0.5180 1.1496 0.042 Uiso 1 1 calc R . . C5 C 0.4647(9) 0.5853(6) 1.0869(6) 0.0318(14) Uani 1 1 d . . . H5 H 0.4053 0.5335 1.1383 0.038 Uiso 1 1 calc R . . C6 C 0.4000(8) 0.6711(6) 1.0045(5) 0.0253(12) Uani 1 1 d . . . H6 H 0.2961 0.6757 1.0001 0.030 Uiso 1 1 calc R . . C7 C 0.7084(7) 0.8427(6) 0.6283(5) 0.0258(13) Uani 1 1 d . . . H7A H 0.7182 0.9023 0.5580 0.031 Uiso 1 1 calc R . . H7B H 0.8180 0.7917 0.6338 0.031 Uiso 1 1 calc R . . C8 C 0.6079(7) 0.7650(5) 0.6269(5) 0.0205(11) Uani 1 1 d . . . C9 C 0.6708(8) 0.6888(6) 0.5500(5) 0.0272(13) Uani 1 1 d . . . H9 H 0.7754 0.6827 0.5033 0.033 Uiso 1 1 calc R . . C10 C 0.5747(9) 0.6238(6) 0.5454(5) 0.0293(13) Uani 1 1 d . . . H10 H 0.6139 0.5729 0.4952 0.035 Uiso 1 1 calc R . . C11 C 0.4203(9) 0.6338(6) 0.6152(5) 0.0291(14) Uani 1 1 d . . . H11 H 0.3533 0.5912 0.6118 0.035 Uiso 1 1 calc R . . C12 C 0.3666(8) 0.7087(6) 0.6905(5) 0.0238(12) Uani 1 1 d . . . H12 H 0.2631 0.7139 0.7386 0.029 Uiso 1 1 calc R . . C13 C 0.6755(7) 1.0634(6) 0.6932(5) 0.0239(12) Uani 1 1 d . . . C14 C 0.8368(8) 1.0635(6) 0.6349(6) 0.0326(14) Uani 1 1 d . . . H14 H 0.9147 0.9916 0.6206 0.039 Uiso 1 1 calc R . . C15 C 0.8789(9) 1.1704(7) 0.5992(6) 0.0345(15) Uani 1 1 d . . . H15 H 0.9862 1.1704 0.5606 0.041 Uiso 1 1 calc R . . C16 C 0.7646(8) 1.2790(6) 0.6195(5) 0.0291(14) Uani 1 1 d . . . H16 H 0.7944 1.3512 0.5942 0.035 Uiso 1 1 calc R . . C17 C 0.6060(8) 1.2780(6) 0.6778(6) 0.0316(14) Uani 1 1 d . . . H17 H 0.5290 1.3501 0.6924 0.038 Uiso 1 1 calc R . . C18 C 0.5597(8) 1.1699(6) 0.7150(6) 0.0308(14) Uani 1 1 d . . . H18 H 0.4525 1.1698 0.7539 0.037 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 Cr1 0.0145(4) 0.0210(4) 0.0170(4) -0.0062(3) -0.0019(3) -0.0051(3) Tl1 0.02871(16) 0.03191(16) 0.02840(15) -0.00753(10) -0.00260(10) -0.00187(11) P1 0.0160(7) 0.0230(7) 0.0187(7) -0.0067(6) -0.0011(5) -0.0071(6) P2 0.0238(8) 0.0309(9) 0.0321(9) -0.0039(7) -0.0067(7) -0.0113(7) N1 0.017(2) 0.022(2) 0.017(2) -0.0049(18) -0.0021(18) -0.0051(19) N2 0.021(2) 0.023(2) 0.018(2) -0.0076(19) -0.0021(18) -0.0063(19) Cl1 0.0179(6) 0.0312(7) 0.0282(7) -0.0108(6) -0.0004(5) -0.0089(6) Cl2 0.0267(7) 0.0285(7) 0.0210(7) -0.0024(6) -0.0054(6) -0.0026(6) Cl3 0.0240(7) 0.0303(7) 0.0246(7) -0.0135(6) -0.0008(5) -0.0074(6) F1 0.045(3) 0.056(3) 0.078(4) -0.034(3) -0.014(3) -0.016(2) F2 0.052(3) 0.079(4) 0.044(3) 0.013(3) -0.001(2) -0.031(3) F3 0.029(2) 0.058(3) 0.048(3) -0.001(2) -0.0099(19) -0.007(2) F4 0.078(4) 0.076(4) 0.078(4) -0.030(3) -0.028(3) -0.036(3) F5 0.052(3) 0.054(3) 0.046(3) 0.014(2) -0.017(2) -0.020(2) F6 0.029(2) 0.057(3) 0.077(4) -0.031(3) -0.011(2) 0.003(2) C1 0.020(3) 0.036(3) 0.024(3) -0.007(3) -0.006(2) -0.012(2) C2 0.025(3) 0.030(3) 0.020(3) -0.008(2) -0.004(2) -0.008(2) C3 0.025(3) 0.035(4) 0.034(3) -0.007(3) -0.010(3) -0.005(3) C4 0.041(4) 0.030(3) 0.031(3) 0.004(3) -0.017(3) -0.008(3) C5 0.037(4) 0.030(3) 0.028(3) 0.000(3) -0.008(3) -0.014(3) C6 0.022(3) 0.026(3) 0.027(3) -0.010(2) 0.002(2) -0.008(2) C7 0.021(3) 0.034(3) 0.021(3) -0.012(3) 0.002(2) -0.008(3) C8 0.019(3) 0.021(3) 0.017(3) -0.004(2) -0.003(2) -0.003(2) C9 0.026(3) 0.030(3) 0.022(3) -0.006(2) -0.003(2) -0.005(3) C10 0.038(4) 0.027(3) 0.026(3) -0.015(3) -0.005(3) -0.007(3) C11 0.041(4) 0.029(3) 0.029(3) -0.010(3) -0.012(3) -0.017(3) C12 0.024(3) 0.029(3) 0.020(3) -0.006(2) -0.002(2) -0.013(2) C13 0.020(3) 0.029(3) 0.021(3) -0.001(2) 0.000(2) -0.013(2) C14 0.019(3) 0.032(3) 0.042(4) -0.011(3) 0.000(3) -0.007(3) C15 0.028(3) 0.043(4) 0.033(3) -0.006(3) 0.004(3) -0.023(3) C16 0.037(4) 0.025(3) 0.031(3) 0.004(3) -0.014(3) -0.019(3) C17 0.030(3) 0.024(3) 0.042(4) -0.009(3) -0.007(3) -0.008(3) C18 0.028(3) 0.032(3) 0.034(3) -0.011(3) 0.001(3) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N1 2.122(5) . ? Cr1 N2 2.124(5) . ? Cr1 Cl2 2.3106(17) . ? Cr1 Cl3 2.3280(16) . ? Cr1 P1 2.3512(16) . ? Cr1 Cl1 2.3628(16) . ? Tl1 Cl3 3.1381(15) . ? Tl1 Cl2 3.1519(15) . ? Tl1 Cl1 3.1816(15) . ? Tl1 F5 3.223(5) . ? Tl1 F4 3.258(6) . ? P1 C7 1.805(6) . ? P1 C1 1.814(6) . ? P1 C13 1.814(6) . ? P2 F2 1.586(5) . ? P2 F4 1.586(5) . ? P2 F1 1.591(5) . ? P2 F5 1.594(5) . ? P2 F6 1.597(5) . ? P2 F3 1.599(5) . ? N1 C2 1.356(8) . ? N1 C6 1.359(8) . ? N2 C12 1.341(8) . ? N2 C8 1.354(7) . ? C1 C2 1.496(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.380(9) . ? C3 C4 1.378(10) . ? C3 H3 0.9300 . ? C4 C5 1.388(10) . ? C4 H4 0.9300 . ? C5 C6 1.354(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.510(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.406(8) . ? C9 C10 1.369(9) . ? C9 H9 0.9300 . ? C10 C11 1.377(10) . ? C10 H10 0.9300 . ? C11 C12 1.384(9) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.381(9) . ? C13 C14 1.400(8) . ? C14 C15 1.368(10) . ? C14 H14 0.9300 . ? C15 C16 1.389(10) . ? C15 H15 0.9300 . ? C16 C17 1.380(10) . ? C16 H16 0.9300 . ? C17 C18 1.400(9) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? 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_3 _geom_angle_publ_flag N1 Cr1 N2 88.65(19) . . ? N1 Cr1 Cl2 169.98(14) . . ? N2 Cr1 Cl2 88.71(14) . . ? N1 Cr1 Cl3 87.36(14) . . ? N2 Cr1 Cl3 171.94(14) . . ? Cl2 Cr1 Cl3 94.03(6) . . ? N1 Cr1 P1 80.74(14) . . ? N2 Cr1 P1 81.57(14) . . ? Cl2 Cr1 P1 89.32(6) . . ? Cl3 Cr1 P1 90.87(6) . . ? N1 Cr1 Cl1 96.86(14) . . ? N2 Cr1 Cl1 96.57(14) . . ? Cl2 Cr1 Cl1 93.04(6) . . ? Cl3 Cr1 Cl1 90.86(6) . . ? P1 Cr1 Cl1 176.97(7) . . ? Cl3 Tl1 Cl2 65.29(4) . . ? Cl3 Tl1 Cl1 63.85(4) . . ? Cl2 Tl1 Cl1 64.75(4) . . ? Cl3 Tl1 F5 88.84(9) . . ? Cl2 Tl1 F5 104.51(10) . . ? Cl1 Tl1 F5 152.67(9) . . ? Cl3 Tl1 F4 108.76(10) . . ? Cl2 Tl1 F4 81.59(12) . . ? Cl1 Tl1 F4 145.73(11) . . ? F5 Tl1 F4 40.27(12) . . ? C7 P1 C1 108.6(3) . . ? C7 P1 C13 107.0(3) . . ? C1 P1 C13 107.4(3) . . ? C7 P1 Cr1 102.5(2) . . ? C1 P1 Cr1 102.1(2) . . ? C13 P1 Cr1 128.1(2) . . ? F2 P2 F4 90.5(3) . . ? F2 P2 F1 90.5(3) . . ? F4 P2 F1 178.9(3) . . ? F2 P2 F5 179.6(3) . . ? F4 P2 F5 89.1(3) . . ? F1 P2 F5 89.9(3) . . ? F2 P2 F6 89.4(3) . . ? F4 P2 F6 90.0(3) . . ? F1 P2 F6 89.5(3) . . ? F5 P2 F6 90.8(3) . . ? F2 P2 F3 89.9(3) . . ? F4 P2 F3 91.3(3) . . ? F1 P2 F3 89.2(3) . . ? F5 P2 F3 89.9(3) . . ? F6 P2 F3 178.5(3) . . ? C2 N1 C6 117.2(5) . . ? C2 N1 Cr1 122.5(4) . . ? C6 N1 Cr1 120.1(4) . . ? C12 N2 C8 118.0(5) . . ? C12 N2 Cr1 119.6(4) . . ? C8 N2 Cr1 122.4(4) . . ? Cr1 Cl1 Tl1 84.20(5) . . ? Cr1 Cl2 Tl1 85.72(5) . . ? Cr1 Cl3 Tl1 85.76(5) . . ? P2 F4 Tl1 113.5(3) . . ? P2 F5 Tl1 114.8(3) . . ? C2 C1 P1 112.3(4) . . ? C2 C1 H1A 109.1 . . ? P1 C1 H1A 109.1 . . ? C2 C1 H1B 109.1 . . ? P1 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? N1 C2 C3 122.0(6) . . ? N1 C2 C1 119.1(5) . . ? C3 C2 C1 118.9(6) . . ? C4 C3 C2 119.5(6) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 118.8(6) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 119.0(6) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 N1 123.4(6) . . ? C5 C6 H6 118.3 . . ? N1 C6 H6 118.3 . . ? C8 C7 P1 113.3(4) . . ? C8 C7 H7A 108.9 . . ? P1 C7 H7A 108.9 . . ? C8 C7 H7B 108.9 . . ? P1 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N2 C8 C9 121.9(5) . . ? N2 C8 C7 119.0(5) . . ? C9 C8 C7 119.1(5) . . ? C10 C9 C8 118.5(6) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C9 C10 C11 120.0(6) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 118.7(6) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? N2 C12 C11 123.0(6) . . ? N2 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? C18 C13 C14 120.5(6) . . ? C18 C13 P1 120.3(5) . . ? C14 C13 P1 119.2(5) . . ? C15 C14 C13 119.4(6) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 121.3(6) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C17 C16 C15 119.0(6) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 C18 120.9(6) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C13 C18 C17 119.0(6) . . ? C13 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.040 _refine_diff_density_min -1.795 _refine_diff_density_rms 0.256