#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:00:26 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180118 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/16/7101691.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
'García, 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_paper_doi               10.1039/b613748b
_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 ω and φ 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/[σ²(Fo²)+(0.0590P)²+3.0330P] where P=(Fo²+2Fc²)/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)
_cod_data_source_file            b613748b.txt
_cod_data_source_block           dw0451
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7101691
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_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_
_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)
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)
