#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2009108.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2009108 loop_ _publ_author_name 'Gelbrich, T.' 'D\"umichen, U.' 'Sieler, J.' _publ_section_title ; Bis-adduct of trimethylamine with aluminium trichloride ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1797 _journal_page_last 1798 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '[Al Cl3 (C3 H9 N)2]' _chemical_formula_sum 'C6 H18 Al Cl3 N2' _chemical_formula_weight 251.55 _chemical_name_systematic ; bis(trimetylamine) aluminiumtrichloride ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.645(8) _cell_length_b 9.994(2) _cell_length_c 12.918(6) _cell_measurement_reflns_used 80 _cell_measurement_temperature 203(2) _cell_measurement_theta_max 19.3 _cell_measurement_theta_min 10.3 _cell_volume 1245.2(12) _computing_cell_refinement DIF4 _computing_data_collection 'DIF4 (Stoe & Cie, 1990a)' _computing_data_reduction 'REDU4 (Stoe & Cie, 1990b)' _computing_molecular_graphics 'SHELXTL (Siemens, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 203(2) _diffrn_measured_fraction_theta_full 0.917 _diffrn_measured_fraction_theta_max 0.917 _diffrn_measurement_device 'Stoe Stadi-4' _diffrn_measurement_method \w-\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 3832 _diffrn_reflns_theta_full 30.05 _diffrn_reflns_theta_max 30.05 _diffrn_reflns_theta_min 2.58 _diffrn_standards_decay_% 1.5 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_description platelet _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _refine_diff_density_max 0.220 _refine_diff_density_min -0.208 _refine_ls_extinction_coef 0.0179(15) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 103 _refine_ls_number_reflns 1916 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.026 _refine_ls_R_factor_gt 0.020 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.1290P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_ref 0.059 _reflns_number_gt 1666 _reflns_number_total 1916 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file cf1327.cif _[local]_cod_data_source_block s171 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (4 times). '_geom_bond_publ_flag' value 'No' changed to 'no' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (17 times). '_geom_angle_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (7 times). '_geom_angle_publ_flag' value 'No' changed to 'no' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (33 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2009108 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-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_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Al1 0.20521(4) 0.2500 0.02323(3) 0.02302(10) Uani d S 1 Al N1 0.03169(11) 0.2500 0.12869(8) 0.0270(2) Uani d S 1 N N2 0.37630(13) 0.2500 -0.08541(8) 0.0332(2) Uani d S 1 N Cl1 0.06061(4) 0.2500 -0.10522(2) 0.03899(10) Uani d S 1 Cl Cl2 0.27989(2) 0.43618(2) 0.089765(17) 0.03131(8) Uani d . 1 Cl C2 -0.05751(11) 0.12952(11) 0.11420(9) 0.0395(2) Uani d . 1 C C1 0.07751(16) 0.2500 0.23854(10) 0.0359(3) Uani d S 1 C C3 0.51353(16) 0.2500 -0.03267(14) 0.0427(3) Uani d S 1 C C4 0.37242(15) 0.37039(11) -0.15361(9) 0.0452(3) Uani d . 1 C H1A 0.0018(19) 0.2500 0.2829(15) 0.047(5) Uiso d S 1 H H1B 0.1354(12) 0.1708(12) 0.2510(10) 0.043(3) Uiso d . 1 H H2A -0.0086(14) 0.0495(15) 0.1242(12) 0.052(4) Uiso d . 1 H H2B -0.0974(14) 0.1310(15) 0.0480(12) 0.054(4) Uiso d . 1 H H2C -0.1351(13) 0.1327(15) 0.1621(11) 0.050(4) Uiso d . 1 H H3A 0.588(2) 0.2500 -0.0793(15) 0.044(5) Uiso d S 1 H H3B 0.5215(13) 0.1713(15) 0.0078(10) 0.049(4) Uiso d . 1 H H4A 0.3764(13) 0.4498(14) -0.1115(10) 0.045(4) Uiso d . 1 H H4B 0.4437(14) 0.3691(15) -0.1986(11) 0.051(4) Uiso d . 1 H H4C 0.2881(12) 0.3661(14) -0.1920(10) 0.040(3) Uiso d . 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Al1 0.02999(18) 0.01889(16) 0.02019(16) 0.000 -0.00153(12) 0.000 N1 0.0277(5) 0.0251(5) 0.0283(5) 0.000 0.0009(4) 0.000 N2 0.0475(6) 0.0241(5) 0.0279(5) 0.000 0.0111(4) 0.000 Cl1 0.0512(2) 0.03894(18) 0.02679(15) 0.000 -0.01406(13) 0.000 Cl2 0.03670(13) 0.02444(12) 0.03279(12) -0.00575(8) 0.00339(8) -0.00659(7) C2 0.0350(5) 0.0355(5) 0.0481(6) -0.0101(4) 0.0048(4) -0.0018(4) C1 0.0402(7) 0.0431(7) 0.0242(6) 0.000 0.0052(5) 0.000 C3 0.0368(7) 0.0403(8) 0.0510(8) 0.000 0.0145(7) 0.000 C4 0.0685(7) 0.0335(5) 0.0335(5) -0.0011(5) 0.0184(5) 0.0076(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Al1 N2 . . 178.76(5) yes N1 Al1 Cl1 . . 89.10(6) yes N2 Al1 Cl1 . . 89.67(7) yes N1 Al1 Cl2 . . 90.42(3) yes N2 Al1 Cl2 . . 90.21(3) yes Cl1 Al1 Cl2 . . 121.075(16) yes N1 Al1 Cl2 . 7_565 90.42(3) no N2 Al1 Cl2 . 7_565 90.21(3) no Cl1 Al1 Cl2 . 7_565 121.075(16) no Cl2 Al1 Cl2 . 7_565 117.85(3) yes C1 N1 C2 . . 106.94(7) no C1 N1 C2 . 7_565 106.94(7) no C2 N1 C2 . 7_565 107.66(12) no C1 N1 Al1 . . 111.84(9) no C2 N1 Al1 . . 111.60(7) no C2 N1 Al1 7_565 . 111.60(7) no C3 N2 C4 . 7_565 107.01(9) no C3 N2 C4 . . 107.01(9) no C4 N2 C4 7_565 . 107.53(12) no C3 N2 Al1 . . 112.39(10) no C4 N2 Al1 7_565 . 111.32(7) no C4 N2 Al1 . . 111.32(7) no N1 C2 H2A . . 112.4(8) no N1 C2 H2B . . 109.8(9) no H2A C2 H2B . . 110.2(13) no N1 C2 H2C . . 109.8(8) no H2A C2 H2C . . 109.1(12) no H2B C2 H2C . . 105.3(11) no N1 C1 H1A . . 110.8(12) no N1 C1 H1B . . 109.0(8) no H1A C1 H1B . . 110.2(9) no N2 C3 H3A . . 112.8(12) no N2 C3 H3B . . 108.9(8) no H3A C3 H3B . . 107.0(10) no N2 C4 H4A . . 109.2(8) no N2 C4 H4B . . 110.5(9) no H4A C4 H4B . . 110.2(11) no N2 C4 H4C . . 107.0(8) no H4A C4 H4C . . 111.4(11) no H4B C4 H4C . . 108.4(11) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Al1 N1 . 2.1580(16) yes Al1 N2 . 2.1662(16) yes Al1 Cl1 . 2.1676(10) yes Al1 Cl2 . 2.1725(5) yes Al1 Cl2 7_565 2.1725(5) no N1 C1 . 1.4862(18) no N1 C2 . 1.4916(13) no N1 C2 7_565 1.4916(12) no N2 C3 . 1.489(2) no N2 C4 7_565 1.4917(12) no N2 C4 . 1.4917(12) no C2 H2A . 0.937(15) no C2 H2B . 0.938(15) no C2 H2C . 0.972(13) no C1 H1A . 0.929(19) no C1 H1B . 0.982(12) no C3 H3A . 0.94(2) no C3 H3B . 0.948(14) no C4 H4A . 0.963(14) no C4 H4B . 0.900(14) no C4 H4C . 0.954(12) no