#------------------------------------------------------------------------------ #$Date: 2018-10-05 13:19:55 +0100 (Fri, 05 Oct 2018) $ #$Revision: 211332 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/10/4301055.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_4301055 loop_ _publ_author_name 'Adams, Nico' 'Bigmore, Helen R.' 'Blundell, Timothy L.' 'Boyd, Catherine L.' 'Dubberley, Stuart R.' 'Sealey, Andrew J.' 'Cowley, Andrew R.' 'Skinner, Michael E. G.' 'Mountford, Philip' _publ_section_title ; New Titanium Imido Synthons: Syntheses and Supramolecular Structures ; _journal_coden_ASTM INOCAJ _journal_issue 8 _journal_name_full 'Inorganic Chemistry' _journal_page_first 2882 _journal_page_last 2894 _journal_paper_doi 10.1021/ic050011z _journal_volume 44 _journal_year 2005 _chemical_compound_source 'TiCl2(NMe2)2 + i-PrNH2' _chemical_formula_moiety ' C7 H21 Cl2 N3 Ti1 ' _chemical_formula_sum 'C7 H21 Cl2 N3 Ti' _chemical_formula_weight 266.07 _chemical_name_systematic Ti(N-i-Pr)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 128.78(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.913(1) _cell_length_b 9.101(1) _cell_length_c 12.044(1) _cell_measurement_reflns_used 4793 _cell_measurement_temperature 175 _cell_measurement_theta_max 27 _cell_measurement_theta_min 0 _cell_volume 1445.2(10) _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_data_collection ; DIP2000 software Xpress (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _diffrn_ambient_temperature 175 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type 'Enraf-nonius DIP2000' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.01 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4793 _diffrn_reflns_theta_max 26.40 _diffrn_reflns_theta_min 2.17 _diffrn_standards_decay_% 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_number 'not measured' _exptl_absorpt_coefficient_mu 0.93 _exptl_absorpt_correction_T_max 0.722 _exptl_absorpt_correction_T_min 0.689 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour 'yellow ' _exptl_crystal_density_diffrn 1.22 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description 'rod ' _exptl_crystal_F_000 560.06 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _refine_diff_density_max 0.28 _refine_diff_density_min -0.28 _refine_ls_extinction_coef 'none required' _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.0524 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 67 _refine_ls_number_reflns 1078 _refine_ls_number_restraints 2 _refine_ls_R_factor_gt 0.0264 _refine_ls_shift/su_max 0.006 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0333 _reflns_limit_h_max 16 _reflns_limit_h_min -21 _reflns_limit_k_max 11 _reflns_limit_k_min 0 _reflns_limit_l_max 14 _reflns_limit_l_min 0 _reflns_number_gt 1078 _reflns_number_total 1374 _reflns_threshold_expression >3.00\s(I) _cod_data_source_file ic050011zsi20050104_034133_2.cif _cod_data_source_block COMPOUND_2 _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. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_atom_sites_solution_primary' value 'direct methods' was changed to 'direct'. '_atom_sites_solution_hydrogens' value 'geometric' was changed to 'geom'. Automatic conversion script Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius ; _cod_original_cell_volume 1445.1 _cod_original_sg_symbol_H-M 'C 1 2/c 1 ' _cod_original_formula_sum ' C7 H21 Cl2 N3 Ti1 ' _cod_database_code 4301055 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 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_ _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 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 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 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