#------------------------------------------------------------------------------ #$Date: 2015-01-07 16:25:02 +0000 (Wed, 07 Jan 2015) $ #$Revision: 129439 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/10/4301057.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_4301057 loop_ _publ_author_name 'Nico Adams' 'Helen R. Bigmore' 'Timothy L. Blundell' 'Catherine L. Boyd' 'Stuart R. Dubberley' 'Andrew J. Sealey' 'Andrew R. Cowley' 'Michael E. G. Skinner' 'Philip Mountford' _publ_contact_author ; Dr P. Mountford Chemistry Reaearch Laboratory Mansfield Road Oxford OX1 3TA UK ; _publ_contact_author_email Philip.Mountford@chem.ox.ac.uk _publ_contact_author_fax '+44 1865 285141' _publ_contact_author_phone '+44 1865 285140' _publ_section_title ; New Titanium Imido Synthons: Syntheses and Supramolecular Structures ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 2882 _journal_page_last 2894 _journal_volume 44 _journal_year 2005 _chemical_compound_source ; ? ; _chemical_formula_moiety ' C10 H14 Cl2 F5 N3 Ti1 ' _chemical_formula_sum 'C10 H14 Cl2 F5 N3 Ti' _chemical_formula_weight 390.04 _chemical_melting_point ? _chemical_name_systematic ; Ti(NC6F5)Cl2(NHMe2)2 ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _cell_angle_alpha 90 _cell_angle_beta 109.69(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.696(3) _cell_length_b 15.569(1) _cell_length_c 6.7371(9) _cell_measurement_reflns_used 24 _cell_measurement_temperature 200 _cell_measurement_theta_max 32 _cell_measurement_theta_min 22 _cell_volume 1550.1(4) _diffrn_ambient_temperature 200 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_method \w/2\q _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_reflns_av_R_equivalents 0.08 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 3439 _diffrn_reflns_theta_max 74.27 _diffrn_reflns_theta_min 4.12 _diffrn_standards_decay_% 32.61 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 8.334 _exptl_absorpt_correction_T_max 0.04 _exptl_absorpt_correction_T_min 0.02 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; Azimutal absorption correction (North et al, 1968) ; _exptl_crystal_colour 'orange ' _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_meas ? _exptl_crystal_description 'fragment ' _exptl_crystal_F_000 789.960 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _refine_diff_density_max 0.75 _refine_diff_density_min -0.60 _refine_ls_extinction_coef 67.5(57) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _refine_ls_goodness_of_fit_ref 1.0778 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 99 _refine_ls_number_reflns 1536 _refine_ls_R_factor_gt 0.0615 _refine_ls_shift/su_max 0.002145 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 14.1 -1.25 9.02 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0648 _reflns_limit_h_max 18 _reflns_limit_h_min -19 _reflns_limit_k_max 19 _reflns_limit_k_min 0 _reflns_limit_l_max 8 _reflns_limit_l_min 0 _reflns_number_gt 1536 _reflns_number_total 1581 _reflns_threshold_expression >3.00\s(I) _[local]_cod_data_source_file ic050011zsi20050104_034133_4.cif _[local]_cod_data_source_block COMPOUND_9 _[local]_cod_cif_authors_sg_H-M 'C 1 2/c 1 ' _[local]_cod_chemical_formula_sum_orig ' C10 H14 Cl2 F5 N3 Ti1 ' _cod_depositor_comments ; The following automatic conversions were performed: _chemical_melting_point value 'not measured' changed to '?' - value is undefined or not given. Automatic conversion script Id: cif_fix_values 1391 2010-09-07 12:51:13Z saulius 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_original_cell_volume 1550.1(3) _cod_database_code 4301057 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_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_ _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 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 . 180 yes Ti1 . N2 . C5 . 112.70(19) yes Ti1 . N2 . C6 . 115.81(19) yes C5 . N2 . C6 . 109.6(2) yes 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 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 _journal_paper_doi 10.1021/ic050011z