#------------------------------------------------------------------------------
#$Date: 2018-02-01 09:42:29 +0200 (Thu, 01 Feb 2018) $
#$Revision: 206009 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/23/2242363.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_2242363
loop_
_publ_author_name
'Brieger, Lukas'
'Hermann, Andreas'
'Unkelbach, Christian'
'Strohmann, Carsten'
_publ_section_title
;
 Crystal structure and quantum-chemical calculations of a
 trimethylaluminium--THF adduct
;
_journal_coeditor_code           LH5865
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              267
_journal_page_last               270
_journal_paper_doi               10.1107/S2056989018001275
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Al (C H3)3 (C4 H8 O)]'
_chemical_formula_moiety         'C7 H17 Al O'
_chemical_formula_sum            'C7 H17 Al O'
_chemical_formula_weight         144.18
_chemical_name_systematic
;
Trimethyl(tetrahydrofuran-κO)aluminium(III)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.845(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7034(6)
_cell_length_b                   9.1228(7)
_cell_length_c                   13.6833(11)
_cell_measurement_reflns_used    8661
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.3846
_cell_measurement_theta_min      2.2281
_cell_volume                     950.18(13)
_computing_cell_refinement
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_data_collection
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_data_reduction
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2004 (Burla et al.,  2007)
;
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 16.0560
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16552
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         2.676
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.76728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.008
_exptl_crystal_description       block
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.325
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         2071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0539
_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/[σ²(Fo²)+(0.1010P)²+0.0468P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1518
_reflns_number_gt                1664
_reflns_number_total             2071
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            lh5865sup1.cif
_cod_data_source_block           I
_cod_database_code               2242363
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.943
_shelx_estimated_absorpt_t_max   0.971
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_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_occupancy
O O1 0.23608(15) 0.37473(13) 0.62125(9) 0.0358(3) Uani d 1
C C1 0.4234(2) 0.3761(2) 0.61379(15) 0.0403(4) Uani d 1
H H1A 0.4953 0.3839 0.6801 0.048 Uiso calc 1
H H1B 0.4521 0.4592 0.5726 0.048 Uiso calc 1
C C2 0.4549(3) 0.2322(2) 0.56601(16) 0.0500(5) Uani d 1
H H2A 0.5778 0.1990 0.5853 0.060 Uiso calc 1
H H2B 0.4284 0.2389 0.4930 0.060 Uiso calc 1
C C3 0.3280(3) 0.1316(2) 0.60652(16) 0.0507(5) Uani d 1
H H3A 0.3019 0.0440 0.5642 0.061 Uiso calc 1
H H3B 0.3748 0.1000 0.6747 0.061 Uiso calc 1
C C4 0.1680(3) 0.2259(2) 0.60476(16) 0.0445(5) Uani d 1
H H4B 0.0906 0.2184 0.5401 0.053 Uiso calc 1
H H4A 0.1006 0.1966 0.6576 0.053 Uiso calc 1
C C5 0.2460(3) 0.7005(2) 0.65333(15) 0.0439(5) Uani d 1
H H5A 0.3731 0.6915 0.6742 0.066 Uiso calc 1
H H5B 0.2022 0.7858 0.6856 0.066 Uiso calc 1
H H5C 0.2212 0.7130 0.5814 0.066 Uiso calc 1
C C6 0.1905(3) 0.4582(2) 0.83000(15) 0.0461(5) Uani d 1
H H6A 0.1225 0.3705 0.8410 0.069 Uiso calc 1
H H6B 0.1635 0.5367 0.8742 0.069 Uiso calc 1
H H6C 0.3162 0.4354 0.8438 0.069 Uiso calc 1
C C7 -0.1208(3) 0.5008(2) 0.63514(15) 0.0436(5) Uani d 1
H H7A -0.1357 0.5156 0.5634 0.065 Uiso calc 1
H H7B -0.1902 0.5737 0.6648 0.065 Uiso calc 1
H H7C -0.1608 0.4021 0.6493 0.065 Uiso calc 1
Al Al1 0.12856(7) 0.52245(6) 0.69114(4) 0.0335(2) Uani d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Al Al 0.0650 0.0510 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 '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_publ_flag
O1 C1 C2 104.49(15) ?
C1 C2 C3 102.38(16) ?
C4 C3 C2 102.87(16) ?
O1 C4 C3 104.82(15) ?
O1 Al1 C5 101.44(7) ?
O1 Al1 C6 102.27(8) ?
O1 Al1 C7 101.92(8) ?
C5 Al1 C6 116.43(9) y
C5 Al1 C7 116.24(9) y
C6 Al1 C7 114.97(9) y
C1 O1 Al1 122.45(10) y
C4 O1 Al1 124.00(11) y
C4 O1 C1 109.40(13) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1 1.462(2) ?
O1 C4 1.460(2) ?
O1 Al1 1.9131(13) y
C1 C2 1.503(3) ?
C2 C3 1.508(3) ?
C3 C4 1.500(3) ?
C5 Al1 1.9671(19) y
C6 Al1 1.976(2) y
C7 Al1 1.965(2) y

_cod_database_fobs_code 2242363
