#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/71/2007111.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_2007111 loop_ _publ_author_name 'Craig, Fiona J.' 'Kennedy, Alan R.' 'Mulvey, Robert E.' _publ_section_title ; Chloro(dibenzylamine-N)dimethylaluminium(III) ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 335 _journal_page_last 337 _journal_paper_doi 10.1107/S010827019701679X _journal_volume 54 _journal_year 1998 _chemical_formula_iupac '[Al Cl (C1 H3)2 (C14 H15 N1)]' _chemical_formula_moiety 'C16 H21 Al Cl N' _chemical_formula_sum 'C16 H21 Al Cl N' _chemical_formula_weight 289.78 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 93.12(2) _cell_angle_beta 112.80(2) _cell_angle_gamma 108.05(2) _cell_formula_units_Z 2 _cell_length_a 9.720(2) _cell_length_b 9.735(2) _cell_length_c 10.111(2) _cell_measurement_reflns_used 24 _cell_measurement_temperature 295 _cell_measurement_theta_max 21.3 _cell_measurement_theta_min 18.5 _cell_volume 821.8(4) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1985) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1993)' _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _computing_structure_solution 'SIR (Burla et al., 1989)' _diffrn_ambient_temperature 295 _diffrn_measurement_device 'Rigaku AFC7S' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 4008 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% none _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.273 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_meas ? _exptl_crystal_description block _exptl_crystal_F_000 308 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _refine_diff_density_max 0.23 _refine_diff_density_min -0.22 _refine_ls_extinction_coef 6.5E-6(6) _refine_ls_extinction_method 'Zachariasen (1968) type 2, Gaussian isotropic' _refine_ls_goodness_of_fit_obs 1.614 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 257 _refine_ls_number_reflns 2514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.077 _refine_ls_R_factor_obs .036 _refine_ls_shift/esd_max 0.002 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/\s^2^(F)' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.048 _refine_ls_wR_factor_obs .043 _reflns_number_observed 2514 _reflns_number_total 3787 _reflns_observed_criterion I>1.5\s(I) _[local]_cod_data_source_file mu1362.cif _[local]_cod_data_source_block 1 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'none' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 1/\s^2^(F)' 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^(F)'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 821.8(3) _cod_database_code 2007111 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' 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 Cl1 .0479(3) .0605(4) .0478(3) .0174(3) .0123(2) -.0033(2) Al1 .0381(3) .0429(3) .0423(3) .0167(3) .0166(2) .0103(3) N1 .0363(8) .0398(9) .0383(8) .0142(7) .0143(7) .0030(7) C1 .068(2) .055(2) .065(2) .0240(10) .039(2) .0280(10) C2 .0430(10) .0590(10) .0550(10) .0240(10) .0190(10) .0070(10) C3 .0380(10) .0500(10) .0510(10) .0117(10) .0127(9) -.0060(10) C4 .0372(10) .0450(10) .0385(10) .0115(9) .0057(8) -.0047(9) C5 .0570(10) .0500(10) .0600(10) .0180(10) .0130(10) -.0030(10) C6 .066(2) .069(2) .093(2) .030(2) .011(2) -.027(2) C7 .055(2) .109(3) .085(2) .016(2) .0210(10) -.049(2) C8 .069(2) .103(2) .053(2) .004(2) .0290(10) -.017(2) C9 .0610(10) .059(2) .0460(10) .0130(10) .0150(10) -.0010(10) C10 .0500(10) .0620(10) .0430(10) .0320(10) .0174(10) .0060(10) C11 .0410(10) .0460(10) .0410(10) .0201(9) .0143(8) .0017(8) C12 .0420(10) .065(2) .077(2) .0180(10) .0240(10) .0240(10) C13 .069(2) .078(2) .078(2) .0350(10) .0310(10) .038(2) C14 .0560(10) .080(2) .0590(10) .0400(10) .0140(10) .0140(10) C15 .0390(10) .070(2) .0630(10) .0220(10) .0200(10) .0010(10) C16 .0490(10) .0530(10) .0530(10) .0220(10) .0260(10) .0090(10) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Cl1 1.01751(6) .43879(6) 1.20802(6) .0560(3) Uani ? ? Al1 .89156(7) .23232(7) 1.04290(6) .0408(3) Uani ? ? N1 .7224(2) .2831(2) .8836(2) .0388(6) Uani ? ? C1 .7677(4) .0771(4) 1.1143(4) .0580(10) Uani ? ? C2 1.0431(3) .2048(3) .9724(3) .0516(9) Uani ? ? C3 .6023(2) .1523(3) .7644(3) .0505(9) Uani ? ? C4 .6753(2) .0873(2) .6830(2) .0452(8) Uani ? ? C5 .6823(3) -.0515(3) .6919(3) .0611(10) Uani ? ? C6 .7466(4) -.1113(4) .6149(4) .0830(10) Uani ? ? C7 .8054(3) -.0333(5) .5288(4) .0930(10) Uani ? ? C8 .7988(3) .1044(4) .5170(3) .0830(10) Uani ? ? C9 .7331(3) .1642(3) .5936(2) .0610(10) Uani ? ? C10 .6399(3) .3596(3) .9438(2) .0500(9) Uani ? ? C11 .5111(2) .3991(2) .8304(2) .0429(8) Uani ? ? C12 .5449(3) .4964(3) .7433(3) .0621(10) Uani ? ? C13 .4256(3) .5324(3) .6405(3) .0720(10) Uani ? ? C14 .2707(3) .4738(3) .6254(3) .0640(10) Uani ? ? C15 .2357(3) .3774(3) .7112(3) .0580(10) Uani ? ? C16 .3546(3) .3399(2) .8128(2) .0496(9) Uani ? ? H1 .727(4) .112(3) 1.145(3) .080(10) Uiso ? ? H2 .827(4) .061(3) 1.183(4) .090(10) Uiso ? ? H3 .720(4) .011(3) 1.054(4) .090(10) Uiso ? ? H4 1.122(4) .205(3) 1.043(3) .084(9) Uiso ? ? H5 1.070(4) .284(4) .922(3) .110(10) Uiso ? ? H6 1.001(4) .120(4) .900(3) .102(10) Uiso ? ? H7 .770(2) .345(2) .847(2) .040(6) Uiso ? ? H8 .554(3) .086(3) .809(3) .064(7) Uiso ? ? H9 .522(3) .186(3) .695(3) .069(7) Uiso ? ? H10 .648(3) -.101(3) .749(3) .068(8) Uiso ? ? H11 .755(3) -.204(4) .629(3) .096(10) Uiso ? ? H12 .853(4) -.068(4) .478(4) .130(10) Uiso ? ? H13 .834(4) .160(3) .453(3) .100(10) Uiso ? ? H14 .726(3) .254(3) .588(2) .056(7) Uiso ? ? H15 .723(3) .450(3) 1.009(2) .053(6) Uiso ? ? H16 .599(3) .295(2) .998(2) .053(6) Uiso ? ? H17 .645(3) .532(3) .751(3) .068(7) Uiso ? ? H18 .447(4) .602(3) .580(3) .102(10) Uiso ? ? H19 .197(3) .497(3) .558(3) .086(9) Uiso ? ? H20 .132(3) .335(3) .706(3) .077(8) Uiso ? ? H21 .333(3) .276(3) .872(3) .065(7) Uiso ? ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.003 0.002 'International Tables' H 0.000 0.000 'International Tables' Al 0.064 0.051 'International Tables' Cl 0.148 0.159 'International Tables' N 0.006 0.003 'International Tables' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 4 4 4 1 2 4 1 0 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl1 Al1 N1 101.84(5) yes Cl1 Al1 C1 110.00(10) yes Cl1 Al1 C2 107.00(8) yes N1 Al1 C1 103.90(10) yes N1 Al1 C2 109.43(9) yes C1 Al1 C2 122.80(10) yes Al1 N1 C3 113.00(10) yes Al1 N1 C10 112.10(10) yes C3 N1 C10 110.7(2) yes N1 C3 C4 112.9(2) yes C3 C4 C5 121.4(2) no C3 C4 C9 120.3(2) no C5 C4 C9 118.3(2) no C4 C5 C6 121.0(3) no C5 C6 C7 120.1(3) no C6 C7 C8 120.1(3) no C7 C8 C9 119.9(3) no C4 C9 C8 120.7(3) no N1 C10 C11 114.8(2) yes C10 C11 C12 121.6(2) no C10 C11 C16 120.3(2) no C12 C11 C16 118.1(2) no C11 C12 C13 120.9(2) no C12 C13 C14 120.3(2) no C13 C14 C15 119.3(2) no C14 C15 C16 120.4(2) no C11 C16 C15 120.9(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 Al1 ? ? 2.2027(8) yes Al1 N1 ? ? 2.020(2) yes Al1 C1 ? ? 1.979(3) yes Al1 C2 ? ? 1.946(2) yes N1 C3 ? ? 1.502(3) yes N1 C10 ? ? 1.505(3) yes C3 C4 ? ? 1.502(3) yes C4 C5 ? ? 1.380(3) no C4 C9 ? ? 1.378(3) no C5 C6 ? ? 1.375(4) no C6 C7 ? ? 1.360(5) no C7 C8 ? ? 1.371(5) no C8 C9 ? ? 1.382(4) no C10 C11 ? ? 1.505(3) no C11 C12 ? ? 1.380(3) no C11 C16 ? ? 1.384(3) no C12 C13 ? ? 1.380(3) no C13 C14 ? ? 1.377(4) no C14 C15 ? ? 1.367(4) no C15 C16 ? ? 1.380(3) no N1 H7 ? ? .83(2) no C1 H1 ? ? .73(3) no C1 H2 ? ? .77(3) no C1 H3 ? ? .74(3) no C2 H4 ? ? .82(3) no C2 H5 ? ? .97(3) no C2 H6 ? ? .93(3) no C3 H8 ? ? .92(2) no C3 H9 ? ? .98(2) no C5 H10 ? ? .87(2) no C6 H11 ? ? .95(3) no C7 H12 ? ? .92(4) no C8 H13 ? ? .96(3) no C9 H14 ? ? .90(2) no C10 H15 ? ? .97(2) no C10 H16 ? ? .95(2) no C12 H17 ? ? .90(2) no C13 H18 ? ? .97(3) no C14 H19 ? ? .88(3) no C15 H20 ? ? .94(3) no C16 H21 ? ? .91(2) no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag Cl1 Al1 N1 C3 -171.60(10) yes Cl1 Al1 N1 C10 -45.7(2) yes Al1 N1 C3 C4 -63.1(2) yes Al1 N1 C10 C11 -179.4(2) yes C3 N1 C10 C11 -52.2(3) yes C4 C3 N1 C10 170.2(2) yes