#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/91/2009108.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, Thomas' 'D\"umichen, Ulf' 'Sieler, Joachim' _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_paper_doi 10.1107/S0108270199009658 _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_details 'w = 1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.1290P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _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). Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 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 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.1290P] where P = (Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.1290P] where P = (Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2009108 _cod_database_fobs_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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Al1 .20521(4) .2500 .02323(3) .02302(10) Uani d S 1 . . Al N1 .03169(11) .2500 .12869(8) .0270(2) Uani d S 1 . . N N2 .37630(13) .2500 -.08541(8) .0332(2) Uani d S 1 . . N Cl1 .06061(4) .2500 -.10522(2) .03899(10) Uani d S 1 . . Cl Cl2 .27989(2) .43618(2) .089765(17) .03131(8) Uani d . 1 . . Cl C2 -.05751(11) .12952(11) .11420(9) .0395(2) Uani d . 1 . . C C1 .07751(16) .2500 .23854(10) .0359(3) Uani d S 1 . . C C3 .51353(16) .2500 -.03267(14) .0427(3) Uani d S 1 . . C C4 .37242(15) .37039(11) -.15361(9) .0452(3) Uani d . 1 . . C H1A .0018(19) .2500 .2829(15) .047(5) Uiso d S 1 . . H H1B .1354(12) .1708(12) .2510(10) .043(3) Uiso d . 1 . . H H2A -.0086(14) .0495(15) .1242(12) .052(4) Uiso d . 1 . . H H2B -.0974(14) .1310(15) .0480(12) .054(4) Uiso d . 1 . . H H2C -.1351(13) .1327(15) .1621(11) .050(4) Uiso d . 1 . . H H3A .588(2) .2500 -.0793(15) .044(5) Uiso d S 1 . . H H3B .5215(13) .1713(15) .0078(10) .049(4) Uiso d . 1 . . H H4A .3764(13) .4498(14) -.1115(10) .045(4) Uiso d . 1 . . H H4B .4437(14) .3691(15) -.1986(11) .051(4) Uiso d . 1 . . H H4C .2881(12) .3661(14) -.1920(10) .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 .02999(18) .01889(16) .02019(16) .000 -.00153(12) .000 N1 .0277(5) .0251(5) .0283(5) .000 .0009(4) .000 N2 .0475(6) .0241(5) .0279(5) .000 .0111(4) .000 Cl1 .0512(2) .03894(18) .02679(15) .000 -.01406(13) .000 Cl2 .03670(13) .02444(12) .03279(12) -.00575(8) .00339(8) -.00659(7) C2 .0350(5) .0355(5) .0481(6) -.0101(4) .0048(4) -.0018(4) C1 .0402(7) .0431(7) .0242(6) .000 .0052(5) .000 C3 .0368(7) .0403(8) .0510(8) .000 .0145(7) .000 C4 .0685(7) .0335(5) .0335(5) -.0011(5) .0184(5) .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 . .937(15) no C2 H2B . .938(15) no C2 H2C . .972(13) no C1 H1A . .929(19) no C1 H1B . .982(12) no C3 H3A . .94(2) no C3 H3B . .948(14) no C4 H4A . .963(14) no C4 H4B . .900(14) no C4 H4C . .954(12) no