#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:48:26 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179207 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/39/4313976.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_4313976
loop_
_publ_author_name
'Marcus Schiefer'
'N. Dastagiri Reddy'
'Hans-Jürgen Ahn'
'Andreas Stasch'
'Herbert W. Roesky'
'A. Christine Schlicker'
'Hans-Georg Schmidt'
'Mathias Noltemeyer'
'Denis Vidovic'
_publ_section_title
;
 Neutral and Ionic Aluminum, Gallium, and Indium Compounds Carrying Two or
 Three Terminal Ethynyl Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4970
_journal_page_last               4976
_journal_paper_doi               10.1021/ic0342806
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C27 H24 Al N'
_chemical_formula_weight         389.45
_chemical_name_systematic
;
compound 10
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.16(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.905(4)
_cell_length_b                   11.914(3)
_cell_length_c                   13.999(5)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     2313.0(12)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.774
_diffrn_measured_fraction_theta_max 0.774
_diffrn_measurement_device_type  'STOE AED2'
_diffrn_measurement_method       'profile fit'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2181
_diffrn_reflns_theta_full        20.35
_diffrn_reflns_theta_max         20.35
_diffrn_reflns_theta_min         3.60
_diffrn_standards_interval_time  '90 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.9520
_exptl_absorpt_correction_T_min  0.9072
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             824
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         1751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0890
_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)+(0.1700P)²+2.1700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2373
_refine_ls_wR_factor_ref         0.2802
_reflns_number_gt                1221
_reflns_number_total             1751
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            ic0342806_10.cif
_cod_data_source_block           roe955x
_cod_original_cell_volume        2313.1(12)
_cod_database_code               4313976
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.2084(2) 0.24091(17) 0.53955(16) 0.0503(11) Uani 1 1 d . . .
N1 N 0.1015(7) 0.2627(5) 0.6180(5) 0.064(3) Uani 1 1 d . . .
C1 C 0.1642(7) 0.3131(7) 0.4224(7) 0.066(3) Uani 1 1 d . . .
C2 C 0.2225(7) 0.0811(7) 0.5339(6) 0.064(3) Uani 1 1 d . . .
C3 C 0.3157(8) 0.3189(7) 0.6046(6) 0.064(3) Uani 1 1 d . . .
C11 C 0.1321(7) 0.3663(7) 0.3528(6) 0.054(3) Uani 1 1 d . . .
C12 C 0.0954(7) 0.4319(6) 0.2740(5) 0.049(3) Uani 1 1 d . . .
C13 C 0.0128(9) 0.4044(8) 0.2174(7) 0.072(3) Uani 1 1 d . . .
H13A H -0.0212 0.3379 0.2313 0.087 Uiso 1 1 calc R . .
C14 C -0.0209(9) 0.4689(10) 0.1433(7) 0.085(3) Uani 1 1 d . . .
H14A H -0.0775 0.4476 0.1057 0.102 Uiso 1 1 calc R . .
C15 C 0.0269(11) 0.5654(10) 0.1224(7) 0.085(4) Uani 1 1 d . . .
H15A H 0.0028 0.6120 0.0710 0.102 Uiso 1 1 calc R . .
C16 C 0.1079(10) 0.5939(8) 0.1748(7) 0.079(4) Uani 1 1 d . . .
H16A H 0.1419 0.6594 0.1581 0.094 Uiso 1 1 calc R . .
C17 C 0.1434(7) 0.5302(7) 0.2527(6) 0.060(3) Uani 1 1 d . . .
H17A H 0.1992 0.5533 0.2907 0.073 Uiso 1 1 calc R . .
C21 C 0.2316(6) -0.0188(7) 0.5294(5) 0.055(3) Uani 1 1 d . . .
C22 C 0.2424(6) -0.1397(6) 0.5216(6) 0.051(3) Uani 1 1 d . . .
C23 C 0.2924(7) -0.1840(7) 0.4521(7) 0.069(3) Uani 1 1 d . . .
H23A H 0.3226 -0.1365 0.4087 0.083 Uiso 1 1 calc R . .
C24 C 0.2994(8) -0.3006(9) 0.4442(8) 0.089(4) Uani 1 1 d . . .
H24A H 0.3348 -0.3320 0.3952 0.107 Uiso 1 1 calc R . .
C25 C 0.2575(9) -0.3683(8) 0.5041(10) 0.091(4) Uani 1 1 d . . .
H25A H 0.2635 -0.4474 0.4982 0.109 Uiso 1 1 calc R . .
C26 C 0.2072(9) -0.3250(9) 0.5721(9) 0.093(4) Uani 1 1 d . . .
H26A H 0.1761 -0.3735 0.6140 0.112 Uiso 1 1 calc R . .
C27 C 0.1995(8) -0.2106(8) 0.5826(7) 0.080(3) Uani 1 1 d . . .
H27A H 0.1643 -0.1807 0.6324 0.096 Uiso 1 1 calc R . .
C31 C 0.3834(8) 0.3746(8) 0.6395(6) 0.060(3) Uani 1 1 d . . .
C32 C 0.4654(7) 0.4398(6) 0.6745(6) 0.049(3) Uani 1 1 d . . .
C33 C 0.5162(9) 0.4178(7) 0.7567(6) 0.067(3) Uani 1 1 d . . .
H33A H 0.4976 0.3579 0.7962 0.080 Uiso 1 1 calc R . .
C34 C 0.5973(8) 0.4833(9) 0.7848(7) 0.077(3) Uani 1 1 d . . .
H34A H 0.6346 0.4668 0.8427 0.092 Uiso 1 1 calc R . .
C35 C 0.6223(8) 0.5700(8) 0.7293(8) 0.070(3) Uani 1 1 d . . .
H35A H 0.6764 0.6155 0.7486 0.084 Uiso 1 1 calc R . .
C36 C 0.5689(10) 0.5918(8) 0.6449(8) 0.075(3) Uani 1 1 d . . .
H36A H 0.5873 0.6513 0.6049 0.090 Uiso 1 1 calc R . .
C37 C 0.4897(7) 0.5287(7) 0.6182(6) 0.059(3) Uani 1 1 d . . .
H37A H 0.4515 0.5460 0.5611 0.071 Uiso 1 1 calc R . .
C41 C 0.0126(10) 0.2103(11) 0.5714(9) 0.113(4) Uani 1 1 d . . .
H41A H -0.0394 0.2143 0.6148 0.170 Uiso 1 1 calc R . .
H41B H 0.0256 0.1316 0.5565 0.170 Uiso 1 1 calc R . .
H41C H -0.0067 0.2506 0.5120 0.170 Uiso 1 1 calc R . .
C42 C 0.0849(9) 0.3866(8) 0.6292(9) 0.120(5) Uani 1 1 d . . .
H42A H 0.0312 0.3986 0.6697 0.180 Uiso 1 1 calc R . .
H42B H 0.0693 0.4202 0.5661 0.180 Uiso 1 1 calc R . .
H42C H 0.1433 0.4216 0.6591 0.180 Uiso 1 1 calc R . .
C43 C 0.1220(9) 0.2136(9) 0.7129(7) 0.096(4) Uani 1 1 d . . .
H43A H 0.0679 0.2283 0.7523 0.144 Uiso 1 1 calc R . .
H43B H 0.1808 0.2473 0.7433 0.144 Uiso 1 1 calc R . .
H43C H 0.1310 0.1324 0.7068 0.144 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Al1 C2 116.0(4) . . ?
C1 Al1 N1 102.4(4) . . ?
C2 Al1 N1 104.0(3) . . ?
C1 Al1 C3 112.2(4) . . ?
C2 Al1 C3 114.8(4) . . ?
N1 Al1 C3 105.5(4) . . ?
C43 N1 C41 109.4(8) . . ?
C43 N1 C42 108.6(8) . . ?
C41 N1 C42 109.1(9) . . ?
C43 N1 Al1 110.9(7) . . ?
C41 N1 Al1 110.0(6) . . ?
C42 N1 Al1 108.8(5) . . ?
C11 C1 Al1 174.1(8) . . ?
C21 C2 Al1 179.3(8) . . ?
C31 C3 Al1 174.6(7) . . ?
C1 C11 C12 177.8(8) . . ?
C13 C12 C17 117.8(8) . . ?
C13 C12 C11 123.4(8) . . ?
C17 C12 C11 118.7(9) . . ?
C14 C13 C12 122.2(10) . . ?
C13 C14 C15 119.8(11) . . ?
C16 C15 C14 119.7(10) . . ?
C15 C16 C17 121.8(10) . . ?
C12 C17 C16 118.7(10) . . ?
C2 C21 C22 178.7(9) . . ?
C23 C22 C27 118.8(8) . . ?
C23 C22 C21 120.3(7) . . ?
C27 C22 C21 120.9(8) . . ?
C22 C23 C24 119.3(9) . . ?
C25 C24 C23 121.2(10) . . ?
C26 C25 C24 119.7(9) . . ?
C25 C26 C27 120.8(10) . . ?
C22 C27 C26 120.3(9) . . ?
C3 C31 C32 176.3(8) . . ?
C33 C32 C37 120.6(10) . . ?
C33 C32 C31 123.1(9) . . ?
C37 C32 C31 116.3(9) . . ?
C32 C33 C34 119.9(9) . . ?
C35 C34 C33 119.8(9) . . ?
C34 C35 C36 119.5(11) . . ?
C37 C36 C35 120.5(9) . . ?
C36 C37 C32 119.6(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 C1 1.913(11) . ?
Al1 C2 1.917(9) . ?
Al1 N1 1.929(8) . ?
Al1 C3 1.930(13) . ?
N1 C43 1.460(12) . ?
N1 C41 1.492(13) . ?
N1 C42 1.504(11) . ?
C1 C11 1.220(12) . ?
C2 C21 1.198(11) . ?
C3 C31 1.223(13) . ?
C11 C12 1.417(13) . ?
C12 C13 1.386(12) . ?
C12 C17 1.390(11) . ?
C13 C14 1.347(13) . ?
C14 C15 1.371(14) . ?
C15 C16 1.342(14) . ?
C16 C17 1.390(13) . ?
C21 C22 1.454(12) . ?
C22 C23 1.345(11) . ?
C22 C27 1.368(12) . ?
C23 C24 1.398(13) . ?
C24 C25 1.328(14) . ?
C25 C26 1.326(14) . ?
C26 C27 1.376(13) . ?
C31 C32 1.436(14) . ?
C32 C33 1.331(12) . ?
C32 C37 1.377(11) . ?
C33 C34 1.405(13) . ?
C34 C35 1.353(13) . ?
C35 C36 1.374(14) . ?
C36 C37 1.363(13) . ?
