#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:22:36 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180075 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/21/7052177.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_7052177
loop_
_publ_author_name
'Jones, Cameron'
'Rose, Richard P.'
_publ_section_title
;
 Synthesis and characterisation of tetramethylpiperidinyloxide (TEMPO)
 complexes of group 13 metal hydrides
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1484
_journal_paper_doi               10.1039/b702641b
_journal_volume                  31
_journal_year                    2007
_chemical_formula_sum            'C16 H33 Al N2 O'
_chemical_formula_weight         296.42
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 92.69(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.3500(13)
_cell_length_b                   10.747(2)
_cell_length_c                   13.239(3)
_cell_measurement_temperature    150(2)
_cell_volume                     902.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0913
_diffrn_reflns_av_sigmaI/netI    0.0797
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6069
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0679
_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)+(0.0680P)²+0.5442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1679
_reflns_number_gt                1127
_reflns_number_total             1674
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702641b.txt
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               7052177
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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 0.0110(2) 0.2500 0.61435(9) 0.0336(4) Uani 1 2 d S . .
O1 O 0.2313(4) 0.2500 0.69939(17) 0.0306(7) Uani 1 2 d S . .
N1 N 0.1836(5) 0.2500 0.4916(2) 0.0235(8) Uani 1 2 d S . .
N2 N 0.1768(5) 0.2500 0.8050(2) 0.0295(8) Uani 1 2 d S . .
C1 C 0.0485(7) 0.2500 0.3966(3) 0.0462(13) Uani 1 2 d S . .
H1A H -0.0433 0.3245 0.3954 0.055 Uiso 0.50 1 calc PR . .
H1B H -0.0433 0.1755 0.3954 0.055 Uiso 0.50 1 calc PR . .
C2 C 0.1789(7) 0.2500 0.3029(3) 0.0357(11) Uani 1 2 d S . .
H2A H 0.1449 0.1754 0.2615 0.043 Uiso 0.50 1 calc PR . .
H2B H 0.1449 0.3246 0.2615 0.043 Uiso 0.50 1 calc PR . .
C3 C 0.4122(7) 0.2500 0.3348(3) 0.0315(10) Uani 1 2 d S . .
H3 H 0.5005 0.2500 0.2742 0.038 Uiso 1 2 calc SR . .
C4 C 0.3206(5) 0.1378(3) 0.4915(2) 0.0365(8) Uani 1 1 d . . .
H4A H 0.2313 0.0623 0.4918 0.044 Uiso 1 1 calc R . .
H4B H 0.4130 0.1371 0.5538 0.044 Uiso 1 1 calc R . .
C5 C 0.4570(5) 0.1345(3) 0.3992(2) 0.0360(8) Uani 1 1 d . . .
H5A H 0.6080 0.1322 0.4215 0.043 Uiso 1 1 calc R . .
H5B H 0.4247 0.0587 0.3589 0.043 Uiso 1 1 calc R . .
C6 C 0.2608(5) 0.1312(3) 0.8500(2) 0.0360(8) Uani 1 1 d . . .
C7 C 0.2164(6) 0.1355(4) 0.9628(2) 0.0557(10) Uani 1 1 d . . .
H7A H 0.0621 0.1334 0.9703 0.067 Uiso 1 1 calc R . .
H7B H 0.2774 0.0605 0.9962 0.067 Uiso 1 1 calc R . .
C8 C 0.3061(10) 0.2500 1.0155(3) 0.0654(17) Uani 1 2 d S . .
H8A H 0.4617 0.2500 1.0133 0.078 Uiso 1 2 calc SR . .
H8B H 0.2685 0.2500 1.0873 0.078 Uiso 1 2 calc SR . .
C9 C 0.1287(6) 0.0264(3) 0.8017(3) 0.0536(10) Uani 1 1 d . . .
H9A H -0.0214 0.0455 0.8069 0.080 Uiso 1 1 calc R . .
H9B H 0.1616 -0.0519 0.8370 0.080 Uiso 1 1 calc R . .
H9C H 0.1609 0.0184 0.7304 0.080 Uiso 1 1 calc R . .
C10 C 0.4929(5) 0.1041(3) 0.8343(2) 0.0464(9) Uani 1 1 d . . .
H10A H 0.5258 0.1256 0.7649 0.070 Uiso 1 1 calc R . .
H10B H 0.5210 0.0156 0.8462 0.070 Uiso 1 1 calc R . .
H10C H 0.5808 0.1539 0.8818 0.070 Uiso 1 1 calc R . .
H1 H -0.121(5) 0.125(3) 0.603(2) 0.052(9) Uiso 1 1 d . . .
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'
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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Al1 N1 94.04(13) . . ?
O1 Al1 H1 117.7(10) . . ?
N1 Al1 H1 103.2(11) . . ?
N2 O1 Al1 113.4(2) . . ?
C4 N1 C4 108.4(3) . 4_565 ?
C4 N1 C1 108.3(2) . . ?
C4 N1 C1 108.3(2) 4_565 . ?
C4 N1 Al1 110.06(17) . . ?
C4 N1 Al1 110.06(17) 4_565 . ?
C1 N1 Al1 111.7(2) . . ?
O1 N2 C6 106.64(19) . 4_565 ?
O1 N2 C6 106.64(19) . . ?
C6 N2 C6 117.1(3) 4_565 . ?
N1 C1 C2 112.0(3) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C3 C2 C1 109.5(3) . . ?
C3 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
C3 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
C2 C3 C5 108.0(2) . . ?
C2 C3 C5 108.0(2) . 4_565 ?
C5 C3 C5 109.0(3) . 4_565 ?
C2 C3 H3 110.6 . . ?
C5 C3 H3 110.6 . . ?
C5 C3 H3 110.6 4_565 . ?
N1 C4 C5 111.9(2) . . ?
N1 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
N1 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C3 C5 C4 109.2(3) . . ?
C3 C5 H5A 109.8 . . ?
C4 C5 H5A 109.8 . . ?
C3 C5 H5B 109.8 . . ?
C4 C5 H5B 109.8 . . ?
H5A C5 H5B 108.3 . . ?
N2 C6 C10 115.9(3) . . ?
N2 C6 C9 106.5(2) . . ?
C10 C6 C9 108.5(3) . . ?
N2 C6 C7 106.5(3) . . ?
C10 C6 C7 111.2(3) . . ?
C9 C6 C7 107.9(3) . . ?
C8 C7 C6 113.1(3) . . ?
C8 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C7 C8 C7 108.8(4) . 4_565 ?
C7 C8 H8A 109.9 . . ?
C7 C8 H8A 109.9 4_565 . ?
C7 C8 H8B 109.9 . . ?
C7 C8 H8B 109.9 4_565 . ?
H8A C8 H8B 108.3 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10A 109.5 . . ?
C6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
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 O1 1.754(3) . ?
Al1 N1 2.003(3) . ?
Al1 H1 1.59(3) . ?
O1 N2 1.456(4) . ?
N1 C4 1.487(3) . ?
N1 C4 1.487(3) 4_565 ?
N1 C1 1.488(4) . ?
N2 C6 1.497(3) 4_565 ?
N2 C6 1.497(3) . ?
C1 C2 1.524(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.521(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C5 1.525(4) . ?
C3 C5 1.525(4) 4_565 ?
C3 H3 1.0000 . ?
C4 C5 1.531(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C10 1.526(4) . ?
C6 C9 1.527(4) . ?
C6 C7 1.533(4) . ?
C7 C8 1.513(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C7 1.513(4) 4_565 ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
