Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _audit_creation_date 01-08-11 _audit_creation_method CRYSTALS _publ_contact_letter ; Chem Comm manuscript no: B109251K These are the *revised* CIF format data (3 compound3) for the paper "Comparison of the relative importance of Ti-Cl...H-N hydrogen bonds and supramolecular interactions between perfluorophenyl rings in the complexes [Ti(NR)Cl2(NHMe2)2] (R = i-Pr, C6H5 or C6F5)" N. Adams, A. R. Cowley, S. R. Dubberley, A. J. Sealey, M. E. G. Skinner and P. Mountford ; _publ_contact_author ; Dr P. Mountford Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; _publ_contact_author_phone '+44 1865 272679 _contact_author_fax '+44 1865 272690' _publ_contact_author_email Philip.Mountford@chem.ox.ac.uk data_COMPOUND1 # Local code MEGS34 _chemical_name_systematic ; [Ti(N-i-Pr)Cl2(NHMe2)2] ; _publ_section_exptl_refinement ; Systematic absences were consistent with either Cc or C2/c. Comparison of the molecular structures obtained in Cc and C2/c, along with the more successful structure solution and refinement in the latter, favoured the non-centrosymmetric alternative. H atoms were placed in calculated positions. The C(1), carbon atom of the i-Pr group is positionally disordered across the crystallographic 2-fold axis at 0,y,1/4. All H atoms were refined in a riding model. Loose similarity restraints were applied to the i-Pr group C(1)-C(2) and C(1)-C(2B) distances. ; _cell_length_a 16.913(1) _cell_angle_alpha 90 _cell_length_b 9.101(1) _cell_angle_beta 128.78(5) _cell_length_c 12.044(1) _cell_angle_gamma 90 _cell_volume 1445.1(1) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C7 H21 Cl2 N3 Ti1 ' _chemical_formula_moiety ' C7 H21 Cl2 N3 Ti1 ' _chemical_compound_source ; TiCl2(NMe2)2 + i-PrNH2 ; _chemical_formula_weight 266.07 _cell_measurement_reflns_used 4793 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 175 _cell_formula_units_Z 4 _exptl_crystal_description 'rod ' _exptl_crystal_colour 'yellow ' _exptl_crystal_size_min 0.35 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.40 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.22 _exptl_crystal_F_000 560.06 _exptl_absorpt_coefficient_mu 0.93 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.689 _exptl_absorpt_correction_T_max 0.722 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-nonius DIP2000' _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_ambient_temperature 175 _reflns_number_total 1374 _diffrn_reflns_av_R_equivalents 0.01 _reflns_number_gt 1078 _diffrn_reflns_number 4793 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.40 _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -21 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _reflns_threshold_expression >3.00\s(I) _refine_ls_hydrogen_treatment constr _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc' _refine_ls_number_restraints 2 _refine_ls_abs_structure_flack ? _refine_ls_extinction_coef 'none required' _refine_diff_density_min -0.28 _refine_diff_density_max 0.28 _refine_ls_number_reflns 1078 _refine_ls_number_parameters 67 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0333 _refine_ls_goodness_of_fit_ref 1.0524 _refine_ls_shift/su_max 0.006 _refine_ls_structure_factor_coef F _refine_ls_extinction_method 'None' _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_data_collection ; DIP2000 software Xpress (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ti1 1.0000 0.48069(5) 0.2500 0.0300 1.0000 Uani Cl1 0.89576(4) 0.38105(7) 0.01857(5) 0.0530 1.0000 Uani N1 1.00000(1) 0.6645(3) 0.25000(1) 0.0560 1.0000 Uani N2 0.87263(12) 0.44813(18) 0.25425(18) 0.0400 1.0000 Uani C1 1.0277(3) 0.8207(4) 0.2870(5) 0.0641 0.5000 Uani C2 0.9673(4) 0.8902(3) 0.3178(6) 0.1176 1.0000 Uani C3 0.77790(16) 0.5250(3) 0.1410(3) 0.0577 1.0000 Uani C4 0.85044(19) 0.2951(3) 0.2640(3) 0.0611 1.0000 Uani H1 0.89677 0.4901 0.33476 0.0511 1.0000 Uiso H11 1.0980 0.8324 0.3786 0.0693 0.5000 Uiso H21 0.9877 0.9957 0.3423 0.1806 0.5000 Uiso H22 0.9787 0.8395 0.4004 0.1806 0.5000 Uiso H23 0.8939 0.8841 0.2329 0.1806 0.5000 Uiso H211 0.9485 0.9960 0.2925 0.1806 0.5000 Uiso H212 1.0352 0.8828 0.4141 0.1806 0.5000 Uiso H213 0.9154 0.8395 0.3189 0.1806 0.5000 Uiso H31 0.72483 0.5040 0.1515 0.0721 1.0000 Uiso H32 0.79067 0.6332 0.1490 0.0721 1.0000 Uiso H33 0.75402 0.4898 0.0458 0.0721 1.0000 Uiso H41 0.79190 0.2920 0.2653 0.0813 1.0000 Uiso H42 0.91135 0.2501 0.3535 0.0813 1.0000 Uiso H43 0.83295 0.2389 0.1799 0.0813 1.0000 Uiso 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 0.0281(2) 0.0299(2) 0.0268(3) 0.0000 0.01472(19) 0.0000 Cl1 0.0426(3) 0.0851(5) 0.0279(3) -0.0110(2) 0.0204(2) -0.0181(2) N1 0.0590(16) 0.0314(13) 0.087(2) 0.0000 0.0500(16) 0.0000 N2 0.0343(8) 0.049(1) 0.0343(9) -0.0039(7) 0.0204(7) -0.0015(7) C1 0.057(3) 0.035(2) 0.067(4) -0.0081(18) 0.022(3) -0.0011(17) C2 0.220(5) 0.0452(17) 0.150(4) -0.0035(18) 0.147(4) 0.015(2) C3 0.036(1) 0.0781(16) 0.0519(15) 0.0033(11) 0.024(1) 0.011(1) C4 0.0558(13) 0.0627(15) 0.0681(17) 0.0022(12) 0.0404(12) -0.0135(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . Cl1 . 2.3544(5) yes Ti1 . Cl1 5_755 2.3544(5) yes Ti1 . N1 . 1.672(2) yes Ti1 . N2 . 2.2067(17) yes Ti1 . N2 5_755 2.2067(17) yes N1 . C1 . 1.476(5) yes N1 . C1 5_755 1.476(5) yes N2 . C3 . 1.476(3) yes N2 . C4 . 1.466(3) yes N2 . H1 . 0.870 no Cl1 . H1 6_564 2.51 no C1 . C2 . 1.433(4) yes C1 . C2 5_755 1.461(4) yes C1 . H11 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no C2 . H211 . 1.000 no C2 . H212 . 1.000 no C2 . H213 . 1.000 no C3 . H31 . 1.000 no C3 . H32 . 1.000 no C3 . H33 . 1.000 no C4 . H41 . 1.000 no C4 . H42 . 1.000 no C4 . H43 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ti1 . Cl1 5_755 134.69(4) yes Cl1 . Ti1 . N1 . 112.655(19) yes Cl1 5_755 Ti1 . N1 . 112.655(19) yes Cl1 . Ti1 . N2 . 87.58(5) yes Cl1 5_755 Ti1 . N2 . 86.49(5) yes N1 . Ti1 . N2 . 97.72(5) yes Cl1 . Ti1 . N2 5_755 86.49(5) yes Cl1 5_755 Ti1 . N2 5_755 87.58(5) yes N1 . Ti1 . N2 5_755 97.72(5) yes N2 . Ti1 . N2 5_755 164.56(9) yes Ti1 . N1 . C1 . 164.46(17) yes Ti1 . N2 . C3 . 115.17(14) yes Ti1 . N2 . C4 . 115.60(14) yes C3 . N2 . C4 . 109.89(18) yes Ti1 . N2 . H1 . 100.56 no C3 . N2 . H1 . 107.5 no C4 . N2 . H1 . 107.0 no N1 . C1 . C2 . 111.2(3) yes N1 . C1 . C2 5_755 109.6(3) yes C2 . C1 . C2 5_755 117.9(4) yes N1 . C1 . H11 . 111.62) no C2 . C1 . H11 . 102.5 no C2 5_755 C1 . H11 . 103.5 no C1 . C2 . H21 . 109.3 no C1 . C2 . H22 . 109.2 no H21 . C2 . H22 . 109.476 no C1 . C2 . H23 . 109.9 no H21 . C2 . H23 . 109.476 no H22 . C2 . H23 . 109.475 no C1 5_755 C2 . H211 . 109.5 no C1 5_755 C2 . H212 . 109.0 no C1 5_755 C2 . H213 . 109.8 no H211 . C2 . H212 . 109.476 no H211 . C2 . H213 . 109.475 no H212 . C2 . H213 . 109.476 no N2 . C3 . H31 . 109.46 no N2 . C3 . H32 . 109.51 no H31 . C3 . H32 . 109.476 no N2 . C3 . H33 . 109.42 no H31 . C3 . H33 . 109.475 no H32 . C3 . H33 . 109.476 no N2 . C4 . H41 . 109.50 no N2 . C4 . H42 . 109.47 no H41 . C4 . H42 . 109.476 no N2 . C4 . H43 . 109.43 no H41 . C4 . H43 . 109.476 no H42 . C4 . H43 . 109.476 no Cl1 6_565 H1 . N2 . 158 no #===end data_COMPOUND2 # Local code ARC30 _chemical_name_systematic ; [Ti(NPh)Cl2(NHMe2)2] ; _chemical_melting_point 'not measured' _cell_length_a 16.260(1) _cell_angle_alpha 90 _cell_length_b 10.303(1) _cell_angle_beta 131.01(1) _cell_length_c 11.935(1) _cell_angle_gamma 90 _cell_volume 1508.8(1) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C10 H19 Cl2 N3 Ti1 ' _chemical_formula_moiety ' C10 H19 Cl2 N3 Ti1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 300.08 _cell_measurement_reflns_used 7655 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' orange-red ' _exptl_crystal_size_min 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 626.076 _exptl_absorpt_coefficient_mu 0.902 # Sheldrick geometric definitions 0.76 0.76 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.76 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 7655 _reflns_number_total 1706 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_gt 1583 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min -21 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _refine_diff_density_min -0.35 _refine_diff_density_max 0.29 _reflns_threshold_expression >3.00\s(I) _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1583 _refine_ls_abs_structure_flack ? _refine_ls_number_parameters 75 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0307 _refine_ls_goodness_of_fit_ref 1.0410 _refine_ls_shift/su_max 0.001517 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_extinction_method 'None' _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 3.14 -.797 2.16 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ti1 0.5000 -0.01106(2) 0.2500 0.0179 1.0000 Uani Cl1 0.39464(3) -0.10632(3) 0.01451(3) 0.0328 1.0000 Uani N1 0.35899(8) -0.03095(11) 0.23667(11) 0.0276 1.0000 Uani N2 0.5000 0.15417(13) 0.2500 0.0246 1.0000 Uani C1 0.26453(11) 0.0503(2) 0.11935(17) 0.0477 1.0000 Uani C2 0.32435(15) -0.16373(17) 0.2351(2) 0.0519 1.0000 Uani C3 0.5000 0.28809(15) 0.2500 0.0212 1.0000 Uani C4 0.5327(1) 0.35754(11) 0.18373(13) 0.0263 1.0000 Uani C5 0.53292(11) 0.49204(12) 0.18502(15) 0.0301 1.0000 Uani C6 0.5000 0.56024(16) 0.2500 0.0307 1.0000 Uani H1 0.3859 -0.0005 0.3228 0.0379 1.0000 Uiso H11 0.2903 0.1396 0.1230 0.0583 1.0000 Uiso H12 0.2277 0.0107 0.0199 0.0583 1.0000 Uiso H13 0.2118 0.0553 0.1360 0.0583 1.0000 Uiso H21 0.3895 -0.2163 0.3151 0.0801 1.0000 Uiso H22 0.2880 -0.2047 0.1364 0.0801 1.0000 Uiso H23 0.2721 -0.1602 0.2525 0.0801 1.0000 Uiso H41 0.5558 0.3098 0.1355 0.0365 1.0000 Uiso H51 0.5571 0.5406 0.1385 0.0422 1.0000 Uiso H61 0.5000 0.6573 0.2500 0.0398 1.0000 Uiso 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 0.02114(15) 0.01588(14) 0.01757(15) 0.0000 0.01303(12) 0.0000 Cl1 0.04109(19) 0.03839(19) 0.02424(16) -0.01102(11) 0.02377(15) -0.01633(12) N1 0.0264(5) 0.0331(5) 0.0278(5) -0.0079(4) 0.0197(4) -0.0067(4) N2 0.0235(6) 0.0211(6) 0.0282(7) 0.0000 0.0166(6) 0.0000 C1 0.0212(6) 0.0764(11) 0.0369(7) 0.0004(7) 0.0153(6) 0.0049(6) C2 0.064(1) 0.0451(9) 0.0757(12) -0.0209(8) 0.059(1) -0.0267(8) C3 0.0187(7) 0.0189(7) 0.0214(7) 0.0000 0.0112(6) 0.0000 C4 0.0305(6) 0.0242(5) 0.0295(6) -0.0017(4) 0.0220(5) -0.0008(4) C5 0.0380(7) 0.0238(6) 0.0357(6) 0.0020(4) 0.0274(6) -0.0028(4) C6 0.0379(9) 0.0175(7) 0.0365(9) 0.0000 0.0243(8) 0.0000 loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . Cl1 . 2.3406(3) yes Ti1 . Cl1 5_655 2.3406(3) yes Ti1 . N1 . 2.201(1) yes Ti1 . N1 5_655 2.201(1) yes Ti1 . N2 . 1.7024(14) yes N1 . C1 . 1.482(2) yes N1 . C2 . 1.4748(18) yes N1 . H1 . 0.870 no N2 . C3 . 1.380(2) yes C1 . H11 . 1.000 no C1 . H12 . 1.0000 no C1 . H13 . 1.0000 no C2 . H21 . 1.000 no C2 . H22 . 1.0000 no C2 . H23 . 1.0000 no C3 . C4 . 1.4040(14) yes C3 . C4 5_655 1.4040(14) yes C4 . C5 . 1.3858(17) yes C4 . H41 . 1.0000 no C5 . C6 . 1.3881(16) yes C5 . H51 . 1.0000 no C6 . H61 . 1.0000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ti1 . Cl1 5_655 130.42(2) yes Cl1 . Ti1 . N1 . 88.12(3) yes Cl1 5_655 Ti1 . N1 . 87.40(3) yes Cl1 . Ti1 . N1 5_655 87.40(3) yes Cl1 5_655 Ti1 . N1 5_655 88.12(3) yes N1 . Ti1 . N1 5_655 169.32(6) yes Cl1 . Ti1 . N2 . 114.79(1) yes Cl1 5_655 Ti1 . N2 . 114.79(1) yes N1 . Ti1 . N2 . 95.34(3) yes N1 5_655 Ti1 . N2 . 95.34(3) yes Ti1 . N1 . C1 . 113.60(9) yes Ti1 . N1 . C2 . 117.26(9) yes C1 . N1 . C2 . 111.17(13) yes Ti1 . N1 . H1 . 100.90 no C1 . N1 . H1 . 108.57 no C2 . N1 . H1 . 103.97 no Ti1 . N2 . C3 . 179.992 yes N1 . C1 . H11 . 109.47 no N1 . C1 . H12 . 109.47 no H11 . C1 . H12 . 109.48 no N1 . C1 . H13 . 109.47 no H11 . C1 . H13 . 109.48 no H12 . C1 . H13 . 109.48 no N1 . C2 . H21 . 109.47 no N1 . C2 . H22 . 109.47 no H21 . C2 . H22 . 109.48 no N1 . C2 . H23 . 109.47 no H21 . C2 . H23 . 109.48 no H22 . C2 . H23 . 109.48 no N2 . C3 . C4 . 120.64(7) yes N2 . C3 . C4 5_655 120.64(7) yes C4 . C3 . C4 5_655 118.71(14) yes C3 . C4 . C5 . 120.19(11) yes C3 . C4 . H41 . 119.90 no C5 . C4 . H41 . 119.90 no C4 . C5 . C6 . 120.86(12) yes C4 . C5 . H51 . 119.57 no C6 . C5 . H51 . 119.57 no C5 . C6 . C5 5_655 119.17(15) yes C5 . C6 . H61 . 120.42 no C5 5_655 C6 . H61 . 120.42 no #===end data_COMPOUND3 # Local code ARC17 _chemical_name_systematic ; [Ti(NC6F5)Cl2(NHMe2)2] ; _chemical_melting_point 'not measured' _cell_length_a 15.696(3) _cell_angle_alpha 90 _cell_length_b 15.569(1) _cell_angle_beta 109.69(2) _cell_length_c 6.7371(9) _cell_angle_gamma 90 _cell_volume 1550.1(3) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0170 0.0090 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.3480 0.7020 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0690 0.0530 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0290 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.1890 1.8070 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C10 H14 Cl2 F5 N3 Ti1 ' _chemical_formula_moiety ' C10 H14 Cl2 F5 N3 Ti1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 390.04 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 22 _cell_measurement_theta_max 32 _cell_measurement_temperature 200 _cell_formula_units_Z 4 _exptl_crystal_description 'fragment ' _exptl_crystal_colour 'orange ' _exptl_crystal_size_min 0.40 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_max 0.60 _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 789.960 _exptl_absorpt_coefficient_mu 8.334 _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; Azimutal absorption correction (North et al, 1968) ; _exptl_absorpt_correction_T_min 0.02 _exptl_absorpt_correction_T_max 0.04 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 2 _diffrn_standards_decay_% 32.61 _diffrn_ambient_temperature 200 _diffrn_reflns_number 3439 _reflns_number_total 1581 _diffrn_reflns_av_R_equivalents 0.08 _diffrn_measured_fraction_theta_max 1.000 _reflns_number_gt 1536 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 74.27 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _reflns_limit_h_min -19 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 8 _refine_diff_density_min -0.60 _refine_diff_density_max 0.75 _reflns_threshold_expression >3.00\s(I) _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_abs_structure_flack ? _refine_ls_extinction_coef 67.5(57) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _refine_ls_number_reflns 1536 _refine_ls_number_parameters 99 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.0648 _refine_ls_goodness_of_fit_ref 1.0778 _refine_ls_shift/su_max 0.002145 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 14.1 -1.25 9.02 ; _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ti1 0.0000 -0.20170(4) 0.7500 0.0251 1.0000 Uani Cl1 0.09906(5) -0.15376(5) 1.07447(11) 0.0363 1.0000 Uani F1 -0.15240(12) -0.40633(13) 0.5278(3) 0.0450 1.0000 Uani F2 -0.15230(16) -0.57823(14) 0.5305(4) 0.0550 1.0000 Uani F3 0.0000 -0.66544(17) 0.7500 0.0609 1.0000 Uani N1 0.0000 -0.3112(2) 0.7500 0.0298 1.0000 Uani N2 -0.10605(15) -0.17331(15) 0.8866(4) 0.0281 1.0000 Uani C1 0.0000 -0.3985(2) 0.7500 0.0247 1.0000 Uani C2 -0.07672(19) -0.44724(19) 0.6398(4) 0.0298 1.0000 Uani C3 -0.0770(2) -0.5353(2) 0.6405(5) 0.0355 1.0000 Uani C4 0.0000 -0.5796(3) 0.7500 0.0389 1.0000 Uani C5 -0.1248(2) -0.0802(2) 0.8901(6) 0.0432 1.0000 Uani C6 -0.1924(2) -0.2207(2) 0.7936(5) 0.0370 1.0000 Uani H21 -0.0822 -0.1922 1.0150 0.0373 1.0000 Uiso H51 -0.0666 -0.0483 0.9529 0.0590 1.0000 Uiso H52 -0.1645 -0.0698 0.9770 0.0590 1.0000 Uiso H53 -0.1562 -0.0595 0.7430 0.0590 1.0000 Uiso H61 -0.1796 -0.2835 0.7913 0.0494 1.0000 Uiso H62 -0.2320 -0.2104 0.8804 0.0494 1.0000 Uiso H63 -0.2237 -0.2000 0.6464 0.0494 1.0000 Uiso 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 0.0254(4) 0.0167(4) 0.0350(4) 0.0000 0.0124(3) 0.0000 Cl1 0.0333(4) 0.0369(4) 0.0383(4) -0.0062(3) 0.0116(3) -0.0026(3) F1 0.0300(9) 0.0466(11) 0.0517(11) -0.0016(9) 0.0047(8) 0.0016(8) F2 0.0592(13) 0.0474(12) 0.0644(13) -0.020(1) 0.0288(11) -0.033(1) F3 0.106(3) 0.0160(12) 0.078(2) 0.0000 0.054(2) 0.0000 N1 0.0296(17) 0.0230(16) 0.0384(18) 0.0000 0.0135(14) 0.0000 N2 0.0262(11) 0.0230(11) 0.0368(12) 0.0041(9) 0.0128(9) 0.0020(9) C1 0.0272(17) 0.0201(17) 0.0292(17) 0.0000 0.0125(14) 0.0000 C2 0.0287(14) 0.0285(14) 0.0345(14) -0.0012(11) 0.0136(11) -0.002(1) C3 0.0444(17) 0.0287(15) 0.0406(16) -0.0070(12) 0.0237(14) -0.0133(13) C4 0.066(3) 0.0182(18) 0.046(2) 0.0000 0.036(2) 0.0000 C5 0.0460(18) 0.0242(15) 0.066(2) -0.0071(14) 0.0277(16) 0.0041(13) C6 0.0289(14) 0.0321(15) 0.0530(18) 0.0026(14) 0.0178(13) -0.0021(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . Cl1 . 2.3373(7) yes Ti1 . Cl1 5_556 2.3373(7) yes Ti1 . N1 . 1.706(3) yes Ti1 . N2 . 2.201(2) yes Ti1 . N2 5_556 2.201(2) yes F1 . C2 . 1.335(3) yes F2 . C3 . 1.343(4) yes F3 . C4 . 1.336(5) yes N1 . C1 . 1.359(5) yes N2 . C5 . 1.482(4) yes N2 . C6 . 1.483(4) yes N2 . H21 . 0.870 no C1 . C2 . 1.405(3) yes C1 . C2 5_556 1.405(3) yes C2 . C3 . 1.370(4) yes C3 . C4 . 1.371(4) yes C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . H61 . 1.000 no C6 . H62 . 1.000 no C6 . H63 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ti1 . Cl1 5_556 142.75(5) yes Cl1 . Ti1 . N1 . 108.62(2) yes Cl1 5_556 Ti1 . N1 . 108.62(2) yes Cl1 . Ti1 . N2 . 84.45(7) yes Cl1 5_556 Ti1 . N2 . 88.19(6) yes N1 . Ti1 . N2 . 101.58(6) yes Cl1 . Ti1 . N2 5_556 88.19(6) yes Cl1 5_556 Ti1 . N2 5_556 84.45(7) yes N1 . Ti1 . N2 5_556 101.58(6) yes N2 . Ti1 . N2 5_556 156.83(13) yes Ti1 . N1 . C1 . 179.992 yes Ti1 . N2 . C5 . 112.70(19) yes Ti1 . N2 . C6 . 115.81(19) yes C5 . N2 . C6 . 109.6(2) yes Ti1 . N2 . H21 . 102.44 no C5 . N2 . H21 . 109.7 no C6 . N2 . H21 . 106.1 no N1 . C1 . C2 . 122.67(17) yes N1 . C1 . C2 5_556 122.67(17) yes C2 . C1 . C2 5_556 114.7(3) yes F1 . C2 . C1 . 118.8(3) yes F1 . C2 . C3 . 118.4(3) yes C1 . C2 . C3 . 122.7(3) yes F2 . C3 . C2 . 119.9(3) yes F2 . C3 . C4 . 119.9(3) yes C2 . C3 . C4 . 120.2(3) yes F3 . C4 . C3 . 120.24(19) yes F3 . C4 . C3 5_556 120.24(19) yes C3 . C4 . C3 5_556 119.5(4) yes N2 . C5 . H51 . 109.5 no N2 . C5 . H52 . 109.5 no H51 . C5 . H52 . 109.5 no N2 . C5 . H53 . 109.5 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N2 . C6 . H61 . 109.5 no N2 . C6 . H62 . 109.5 no H61 . C6 . H62 . 109.5 no N2 . C6 . H63 . 109.5 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no #===end