#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:40:26 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179930 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/25/7022531.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_7022531
loop_
_publ_author_name
'Humphries, Terry D.'
'Munroe, Keelie T.'
'Decken, Andreas'
'McGrady, G. Sean'
_publ_section_title
;
 Lewis base complexes of AlH3: structural determination of monomeric and
 polymeric adducts by X-ray crystallography and DFT calculations.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6953
_journal_page_last               6964
_journal_paper_doi               10.1039/c3dt00046j
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C4 H11 Al O2'
_chemical_formula_sum            'C4 H11 Al O2'
_chemical_formula_weight         118.11
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.450(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.318(3)
_cell_length_b                   8.570(4)
_cell_length_c                   6.811(4)
_cell_measurement_reflns_used    1644
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      3.57
_cell_volume                     333.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker AXS SMART1000/P4'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2161
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.57
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.9595
_exptl_absorpt_correction_T_min  0.8852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             128
_exptl_crystal_recrystallization_method ether
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0387
_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)+(0.0523P)²+0.0957P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                647
_reflns_number_total             737
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3dt00046j.txt
_cod_data_source_block           sg081264
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7022531
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Al1 Al 0.0000 0.0000 0.0000 0.0266(3) Uani 1 2 d S
O1 O 0.3067(2) -0.01437(13) 0.2937(2) 0.0303(3) Uani 1 1 d .
C2 C 0.7193(3) 0.0351(2) 0.5075(3) 0.0346(4) Uani 1 1 d .
C1 C 0.4940(3) 0.0949(2) 0.3302(3) 0.0354(4) Uani 1 1 d .
H1A H 0.514(3) 0.103(2) 0.197(3) 0.043(5) Uiso 1 1 d .
H1B H 0.444(4) 0.193(3) 0.366(3) 0.044(5) Uiso 1 1 d .
H2A H 0.758(4) -0.064(3) 0.462(4) 0.050(6) Uiso 1 1 d .
H2B H 0.839(4) 0.107(3) 0.539(3) 0.044(6) Uiso 1 1 d .
H1 H -0.145(7) -0.070(5) 0.094(7) 0.049(12) Uiso 0.50 1 d P
H2 H 0.032(8) 0.174(7) -0.004(7) 0.065(15) Uiso 0.50 1 d P
H3 H -0.125(8) 0.101(5) 0.098(8) 0.057(13) Uiso 0.50 1 d P
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 0.0213(4) 0.0300(4) 0.0226(4) -0.0004(2) 0.0039(3) 0.0005(2)
O1 0.0211(6) 0.0426(7) 0.0202(6) 0.0016(4) 0.0023(4) -0.0053(4)
C2 0.0211(7) 0.0519(10) 0.0264(8) 0.0052(7) 0.0061(6) -0.0051(7)
C1 0.0249(8) 0.0475(11) 0.0267(7) 0.0083(6) 0.0045(6) -0.0069(7)
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'
O O 0.0106 0.0060 '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
O1 Al1 O1 180.0 3
O1 Al1 H1 86.8(16) 3
O1 Al1 H1 93.2(16) .
O1 Al1 H2 90.0(16) 3
O1 Al1 H2 90.0(16) .
H1 Al1 H2 122(2) .
O1 Al1 H3 86.8(17) 3
O1 Al1 H3 93.2(17) .
H1 Al1 H3 60(2) .
H2 Al1 H3 63(2) .
C2 O1 C1 109.48(13) 3_656
C2 O1 Al1 117.95(10) 3_656
C1 O1 Al1 118.48(9) .
O1 C2 C1 110.16(14) 3_656
O1 C2 H2A 109.8(14) 3_656
C1 C2 H2A 108.8(14) .
O1 C2 H2B 105.8(13) 3_656
C1 C2 H2B 111.1(13) .
H2A C2 H2B 111.2(19) .
O1 C1 C2 109.86(14) .
O1 C1 H1A 108.2(12) .
C2 C1 H1A 108.3(12) .
O1 C1 H1B 106.0(12) .
C2 C1 H1B 113.0(12) .
H1A C1 H1B 111.5(17) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 O1 2.1071(14) 3
Al1 O1 2.1071(14) .
Al1 H1 1.45(4) .
Al1 H2 1.51(6) .
Al1 H3 1.50(5) .
O1 C2 1.444(2) 3_656
O1 C1 1.4440(19) .
C2 O1 1.444(2) 3_656
C2 C1 1.506(2) .
C2 H2A 0.97(2) .
C2 H2B 0.93(2) .
C1 H1A 0.97(2) .
C1 H1B 0.96(2) .
