#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:48:26 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179207 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/39/4313988.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_4313988
loop_
_publ_author_name
'Youngjo Kim'
'John G. Verkade'
_publ_section_title
;
 The First Example of a Monomeric Alumatrane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4804
_journal_page_last               4806
_journal_paper_doi               10.1021/ic034444i
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C35 H43 Al N2 O3'
_chemical_formula_weight         566.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.250(2)
_cell_length_b                   14.250(2)
_cell_length_c                   26.738(4)
_cell_measurement_reflns_used    891
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.88
_cell_measurement_theta_min      2.25
_cell_volume                     4702.1(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7993
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0525
_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)+(0.0643P)²+7.3196P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1507
_reflns_number_gt                1448
_reflns_number_total             1782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034444isi20030612_030222.cif
_cod_data_source_block           ver69
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4313988
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.6667 0.3333 0.01106(4) 0.0591(4) Uani 1 3 d S . .
C1 C 0.7048(2) 0.2599(2) 0.10798(8) 0.0592(6) Uani 1 1 d . . .
H1A H 0.6562 0.1858 0.0951 0.071 Uiso 1 1 calc R . .
H1B H 0.6997 0.2570 0.1449 0.071 Uiso 1 1 calc R . .
C2 C 0.8190(2) 0.29422(18) 0.09316(8) 0.0581(6) Uani 1 1 d . . .
C3 C 0.8949(2) 0.3035(2) 0.12838(9) 0.0660(7) Uani 1 1 d . . .
H3A H 0.8742 0.2900 0.1626 0.079 Uiso 1 1 calc R . .
C4 C 0.9993(2) 0.3319(2) 0.11518(11) 0.0727(7) Uani 1 1 d . . .
C5 C 1.0811(3) 0.3433(3) 0.15427(13) 0.1012(11) Uani 1 1 d . . .
H5A H 1.0469 0.3268 0.1873 0.152 Uiso 1 1 calc R . .
H5B H 1.1424 0.4177 0.1540 0.152 Uiso 1 1 calc R . .
H5C H 1.1071 0.2928 0.1468 0.152 Uiso 1 1 calc R . .
C6 C 1.0260(2) 0.3495(2) 0.06484(12) 0.0737(7) Uani 1 1 d . . .
H6A H 1.0972 0.3679 0.0550 0.088 Uiso 1 1 calc R . .
C7 C 0.9536(2) 0.34159(19) 0.02840(10) 0.0651(7) Uani 1 1 d . . .
C8 C 0.9856(2) 0.3624(2) -0.02614(10) 0.0835(9) Uani 1 1 d . . .
H8A H 1.0608 0.3789 -0.0299 0.125 Uiso 1 1 calc R . .
H8B H 0.9791 0.4239 -0.0380 0.125 Uiso 1 1 calc R . .
H8C H 0.9378 0.2978 -0.0458 0.125 Uiso 1 1 calc R . .
C9 C 0.8487(2) 0.31517(19) 0.04292(8) 0.0596(6) Uani 1 1 d . . .
C10 C 0.7497(7) 0.4058(6) -0.08939(18) 0.206(5) Uani 0.67 1 d P . .
H10A H 0.7367 0.3945 -0.1255 0.310 Uiso 0.67 1 calc PR . .
H10B H 0.8135 0.4002 -0.0805 0.310 Uiso 0.67 1 calc PR . .
H10C H 0.7624 0.4779 -0.0804 0.310 Uiso 0.67 1 calc PR . .
C11 C -0.0465(3) 0.0634(3) 0.07155(13) 0.1003(10) Uani 1 1 d . . .
H11A H -0.0788 0.1077 0.0718 0.120 Uiso 1 1 calc R . .
C12 C 0.0633(3) 0.1092(3) 0.07134(14) 0.1002(10) Uani 1 1 d . . .
H12A H 0.1077 0.1859 0.0710 0.120 Uiso 1 1 calc R . .
N1 N 0.6667 0.3333 0.08897(10) 0.0526(8) Uani 1 3 d S . .
N2 N 0.6667 0.3333 -0.06554(14) 0.1117(17) Uani 1 3 d S . .
O1 O 0.77678(14) 0.30993(14) 0.00837(6) 0.0684(5) Uani 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 O1 119.834(9) . 3_665 ?
O1 Al1 O1 119.834(9) . 2_655 ?
O1 Al1 O1 119.834(9) 3_665 2_655 ?
O1 Al1 N2 87.66(6) . . ?
O1 Al1 N2 87.66(6) 3_665 . ?
O1 Al1 N2 87.66(6) 2_655 . ?
O1 Al1 N1 92.34(6) . . ?
O1 Al1 N1 92.34(6) 3_665 . ?
O1 Al1 N1 92.34(6) 2_655 . ?
N2 Al1 N1 180.0 . . ?
N1 C1 C2 113.46(18) . . ?
C3 C2 C9 119.6(2) . . ?
C3 C2 C1 121.2(2) . . ?
C9 C2 C1 119.2(2) . . ?
C4 C3 C2 122.0(2) . . ?
C3 C4 C6 117.3(2) . . ?
C3 C4 C5 121.0(3) . . ?
C6 C4 C5 121.6(3) . . ?
C7 C6 C4 122.9(3) . . ?
C6 C7 C9 118.6(2) . . ?
C6 C7 C8 121.6(2) . . ?
C9 C7 C8 119.8(2) . . ?
O1 C9 C2 120.4(2) . . ?
O1 C9 C7 120.1(2) . . ?
C2 C9 C7 119.5(2) . . ?
N2 C10 C10 41.25(18) . 3_665 ?
N2 C10 C10 41.25(18) . 2_655 ?
C10 C10 C10 60.0 3_665 2_655 ?
C12 C11 C12 119.4(4) 2 . ?
C11 C12 C11 120.6(4) 3 . ?
C1 N1 C1 108.99(13) . 2_655 ?
C1 N1 C1 108.99(13) . 3_665 ?
C1 N1 C1 108.99(13) 2_655 3_665 ?
C1 N1 Al1 109.95(13) . . ?
C1 N1 Al1 109.95(13) 2_655 . ?
C1 N1 Al1 109.95(13) 3_665 . ?
C10 N2 C10 97.5(4) 3_665 . ?
C10 N2 C10 97.5(4) 3_665 2_655 ?
C10 N2 C10 97.5(4) . 2_655 ?
C10 N2 Al1 119.7(3) 3_665 . ?
C10 N2 Al1 119.7(3) . . ?
C10 N2 Al1 119.7(3) 2_655 . ?
C9 O1 Al1 133.08(15) . . ?
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 1.7613(18) . ?
Al1 O1 1.7613(18) 3_665 ?
Al1 O1 1.7613(17) 2_655 ?
Al1 N2 2.048(4) . ?
Al1 N1 2.083(3) . ?
C1 N1 1.490(2) . ?
C1 C2 1.499(3) . ?
C2 C3 1.390(3) . ?
C2 C9 1.395(3) . ?
C3 C4 1.379(4) . ?
C4 C6 1.387(4) . ?
C4 C5 1.513(4) . ?
C6 C7 1.382(4) . ?
C7 C9 1.402(3) . ?
C7 C8 1.513(3) . ?
C9 O1 1.353(3) . ?
C10 N2 1.285(5) . ?
C10 C10 1.933(10) 3_665 ?
C10 C10 1.933(10) 2_655 ?
C11 C12 1.353(5) 2 ?
C11 C12 1.362(5) . ?
C12 C11 1.353(5) 3 ?
N1 C1 1.490(2) 2_655 ?
N1 C1 1.490(2) 3_665 ?
N2 C10 1.285(5) 3_665 ?
N2 C10 1.285(5) 2_655 ?
