#------------------------------------------------------------------------------ #$Date: 2008-06-25 12:31:45 +0300 (Wed, 25 Jun 2008) $ #$Revision: 403 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7101691.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_7101691 loop_ _publ_author_name 'Garc\'ia, Felipe' 'Hopkins, Alexander D' 'Kowenicki, Richard A' 'McPartlin, Mary' 'Silvia, Jared S' 'Rawson, Jeremy M' 'Rogers, Michael C' 'Wright, Dominic S' _publ_section_title ; Pyridyl 'ring-flipping' in the dimers [Me2E(2-py)]2 (E=B, Al, Ga; 2-py=2-pyridyl). ; _journal_issue 6 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 586 _journal_page_last 588 _journal_year 2007 _chemical_formula_moiety 'C14 H20 Al2 N2' _chemical_formula_sum 'C14 H20 Al2 N2' _chemical_formula_weight 270.28 _chemical_name_systematic ; ? ; _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 _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 112.26(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 14.027(3) _cell_length_b 16.564(3) _cell_length_c 14.656(3) _cell_measurement_reflns_used 11466 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.00 _cell_volume 3151.5(11) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _diffrn_ambient_temperature 180(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 12895 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 3.82 _exptl_absorpt_coefficient_mu 0.170 _exptl_absorpt_correction_T_max 0.994 _exptl_absorpt_correction_T_min 0.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rods _exptl_crystal_F_000 1152 _exptl_crystal_size_max 0.81 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.329 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.049 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 165 _refine_ls_number_reflns 3605 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.030 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0492 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+3.0330P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1208 _refine_ls_wR_factor_ref 0.1404 _reflns_number_gt 2441 _reflns_number_total 3605 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b613748b.txt _[local]_cod_data_source_block dw0451 _[local]_cod_cif_authors_sg_H-M C2/c 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.04043(5) 0.15710(4) 0.07423(5) 0.03324(19) Uani 1 1 d . . . Al2 Al 0.03265(5) 0.34477(4) -0.04015(5) 0.03499(19) Uani 1 1 d . . . N1 N 0.08135(15) 0.17070(12) -0.04094(15) 0.0355(5) Uani 0.50 1 d P A 1 C1 C 0.08519(14) 0.24509(12) -0.08155(14) 0.0353(5) Uani 0.50 1 d P A 1 N1' N 0.08519(14) 0.24509(12) -0.08155(14) 0.0353(5) Uani 0.50 1 d P A 2 C1' C 0.08135(15) 0.17070(12) -0.04094(15) 0.0355(5) Uani 0.50 1 d P A 2 C2 C 0.11816(19) 0.24941(17) -0.15859(19) 0.0485(6) Uani 1 1 d . . . H2 H 0.1222 0.3008 -0.1856 0.058 Uiso 1 1 calc R A 1 C3 C 0.1455(2) 0.1823(2) -0.1979(2) 0.0570(7) Uani 1 1 d . A . H3 H 0.1682 0.1872 -0.2511 0.068 Uiso 1 1 calc R . . C4 C 0.13950(19) 0.10867(19) -0.1593(2) 0.0572(8) Uani 1 1 d . . . H4 H 0.1566 0.0611 -0.1861 0.069 Uiso 1 1 calc R A . C5 C 0.10825(18) 0.10400(16) -0.0809(2) 0.0477(6) Uani 1 1 d . A . H5 H 0.1053 0.0525 -0.0536 0.057 Uiso 1 1 calc R B 1 N2 N 0.08130(14) 0.33406(11) 0.10521(14) 0.0320(4) Uani 0.50 1 d P A 1 C6 C 0.08527(14) 0.26027(12) 0.14967(14) 0.0324(4) Uani 0.50 1 d P A 1 N2' N 0.08527(14) 0.26027(12) 0.14967(14) 0.0324(4) Uani 0.50 1 d P A 2 C6' C 0.08130(14) 0.33406(11) 0.10521(14) 0.0320(4) Uani 0.50 1 d P A 2 C7 C 0.11835(17) 0.25762(15) 0.25116(17) 0.0411(5) Uani 1 1 d . . . H7 H 0.1225 0.2068 0.2825 0.049 Uiso 1 1 calc R A 1 C8 C 0.14558(18) 0.32601(19) 0.30859(19) 0.0509(7) Uani 1 1 d . A . H8 H 0.1669 0.3225 0.3782 0.061 Uiso 1 1 calc R . . C9 C 0.14153(18) 0.39902(18) 0.2640(2) 0.0524(7) Uani 1 1 d . . . H9 H 0.1603 0.4471 0.3021 0.063 Uiso 1 1 calc R A . C10 C 0.10984(17) 0.40174(15) 0.1630(2) 0.0455(6) Uani 1 1 d . A . H10 H 0.1077 0.4525 0.1322 0.055 Uiso 1 1 calc R C 1 C11 C 0.1236(2) 0.06904(16) 0.1566(2) 0.0566(7) Uani 1 1 d . A . H11A H 0.1969 0.0817 0.1762 0.085 Uiso 1 1 calc R . . H11B H 0.1080 0.0185 0.1191 0.085 Uiso 1 1 calc R . . H11C H 0.1072 0.0631 0.2157 0.085 Uiso 1 1 calc R . . C12 C -0.10907(19) 0.14123(17) 0.0289(2) 0.0525(7) Uani 1 1 d . A . H12A H -0.1446 0.1874 -0.0114 0.079 Uiso 1 1 calc R . . H12B H -0.1288 0.1366 0.0861 0.079 Uiso 1 1 calc R . . H12C H -0.1284 0.0918 -0.0105 0.079 Uiso 1 1 calc R . . C21 C 0.1005(2) 0.43803(16) -0.0736(2) 0.0547(7) Uani 1 1 d . A . H21A H 0.1754 0.4318 -0.0421 0.082 Uiso 1 1 calc R . . H21B H 0.0796 0.4877 -0.0499 0.082 Uiso 1 1 calc R . . H21C H 0.0802 0.4410 -0.1452 0.082 Uiso 1 1 calc R . . C22 C -0.11803(19) 0.34732(17) -0.0971(2) 0.0511(6) Uani 1 1 d . A . H22A H -0.1451 0.2988 -0.0770 0.077 Uiso 1 1 calc R . . H22B H -0.1419 0.3490 -0.1691 0.077 Uiso 1 1 calc R . . H22C H -0.1425 0.3954 -0.0736 0.077 Uiso 1 1 calc R . . 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 Al1 0.0391(4) 0.0285(3) 0.0320(4) 0.0002(3) 0.0133(3) -0.0014(3) Al2 0.0382(4) 0.0320(4) 0.0356(4) 0.0061(3) 0.0149(3) 0.0047(3) N1 0.0344(10) 0.0374(11) 0.0347(11) -0.0045(9) 0.0130(8) 0.0008(8) C1 0.0336(10) 0.0413(12) 0.0314(10) 0.0024(9) 0.0128(8) 0.0054(8) N1' 0.0336(10) 0.0413(12) 0.0314(10) 0.0024(9) 0.0128(8) 0.0054(8) C1' 0.0344(10) 0.0374(11) 0.0347(11) -0.0045(9) 0.0130(8) 0.0008(8) C2 0.0469(14) 0.0647(17) 0.0395(13) 0.0092(12) 0.0227(11) 0.0071(12) C3 0.0446(14) 0.090(2) 0.0434(15) -0.0073(15) 0.0240(12) 0.0063(14) C4 0.0456(14) 0.070(2) 0.0611(18) -0.0301(16) 0.0257(13) 0.0006(13) C5 0.0484(14) 0.0396(14) 0.0572(16) -0.0098(12) 0.0223(12) 0.0016(10) N2 0.0304(10) 0.0302(10) 0.0343(10) -0.0025(8) 0.0110(8) 0.0028(7) C6 0.0309(9) 0.0369(11) 0.0303(10) -0.0018(8) 0.0125(8) -0.0015(8) N2' 0.0309(9) 0.0369(11) 0.0303(10) -0.0018(8) 0.0125(8) -0.0015(8) C6' 0.0304(10) 0.0302(10) 0.0343(10) -0.0025(8) 0.0110(8) 0.0028(7) C7 0.0365(12) 0.0536(15) 0.0320(12) 0.0018(11) 0.0115(9) -0.0021(10) C8 0.0366(13) 0.082(2) 0.0342(13) -0.0164(13) 0.0138(10) -0.0052(12) C9 0.0404(13) 0.0598(18) 0.0550(17) -0.0307(14) 0.0158(11) -0.0007(11) C10 0.0433(13) 0.0323(12) 0.0595(16) -0.0095(11) 0.0179(11) 0.0032(10) C11 0.0737(18) 0.0377(14) 0.0536(16) 0.0065(12) 0.0187(14) 0.0076(12) C12 0.0457(14) 0.0525(16) 0.0582(17) -0.0151(13) 0.0185(12) -0.0076(11) C21 0.0566(16) 0.0456(15) 0.0632(18) 0.0168(13) 0.0240(13) 0.0016(11) C22 0.0427(14) 0.0588(17) 0.0497(15) -0.0031(13) 0.0152(11) 0.0034(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Al1 C12 1.963(3) Al1 C11 1.970(3) Al1 N1 1.991(2) Al1 C6 2.003(2) Al2 C22 1.957(3) Al2 C21 1.971(3) Al2 N2 1.983(2) Al2 C1 1.994(2) N1 C5 1.369(3) N1 C1 1.378(3) C1 C2 1.375(3) C2 C3 1.372(4) C3 C4 1.360(4) C4 C5 1.379(4) N2 C10 1.371(3) N2 C6 1.376(3) C6 C7 1.381(3) C7 C8 1.376(3) C8 C9 1.365(4) C9 C10 1.376(4) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C12 Al1 C11 114.65(13) C12 Al1 N1 110.02(11) C11 Al1 N1 108.04(11) C12 Al1 C6 111.90(10) C11 Al1 C6 107.70(11) N1 Al1 C6 103.91(8) C22 Al2 C21 114.98(12) C22 Al2 N2 109.65(11) C21 Al2 N2 109.57(11) C22 Al2 C1 110.62(10) C21 Al2 C1 107.74(11) N2 Al2 C1 103.67(8) C5 N1 C1 118.3(2) C5 N1 Al1 119.10(17) C1 N1 Al1 122.57(15) C2 C1 N1 118.8(2) C2 C1 Al2 119.01(17) N1 C1 Al2 121.97(15) C1 C2 C3 122.5(3) C4 C3 C2 118.7(2) C3 C4 C5 119.1(2) N1 C5 C4 122.5(3) C10 N2 C6 118.9(2) C10 N2 Al2 119.47(17) C6 N2 Al2 121.59(14) N2 C6 C7 118.36(19) N2 C6 Al1 123.26(14) C7 C6 Al1 118.34(16) C6 C7 C8 122.3(2) C9 C8 C7 119.0(2) C8 C9 C10 118.8(2) N2 C10 C9 122.6(2)