#------------------------------------------------------------------------------
#$Date: 2018-10-29 09:33:49 +0200 (Mon, 29 Oct 2018) $
#$Revision: 211691 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/93/7229332.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_7229332
loop_
_publ_author_name
'Kim, Yoseph'
'Lee, Kang Mun'
'Kim, So Han'
'Moon, Jung Hee'
'Kim, Youngjo'
_publ_section_title
;
 Dimeric alumatranes as catalysts for trimethylsilylcyanation reaction
;
_journal_issue                   76
_journal_name_full               'RSC Adv.'
_journal_page_first              48151
_journal_paper_doi               10.1039/C7RA09851K
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         C34H56Al2N2O6
_chemical_formula_sum            'C34 H56 Al2 N2 O6'
_chemical_formula_weight         642.76
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-02-07 deposited with the CCDC.
2017-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.997(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6533(6)
_cell_length_b                   14.1939(6)
_cell_length_c                   18.8530(8)
_cell_measurement_reflns_used    13281
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.12
_cell_measurement_theta_min      1.72
_cell_volume                     3608.6(3)
_computing_cell_refinement       'Bruker APEX II'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker APEX II'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            79871
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.119
_diffrn_reflns_theta_min         1.720
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         13281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0964P)²+0.6417P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8046
_reflns_number_total             13281
_reflns_threshold_expression     'I > 2σ(I)'
_cod_depositor_comments
;

2018-10-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C68 H112 Al4 N4 O12'
_cod_original_formula_weight         1285.53
_cod_original_formula_moiety         C68H112Al4N4O12
_cod_original_formula_units_Z            2
_cod_data_source_file            c7ra09851k2.cif
_cod_data_source_block           Al-tea-Me2-2
_cod_database_code               7229332
_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.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Al Al 0.07640(3) 0.92880(3) 0.00775(2) 0.02308(10) Uani 1 1 d . .
N N 0.16897(9) 0.90954(9) -0.07052(6) 0.0268(2) Uani 1 1 d . .
O1 O -0.02185(8) 0.97738(7) 0.05487(5) 0.0242(2) Uani 1 1 d . .
C1 C -0.07674(12) 0.94177(10) 0.10833(7) 0.0293(3) Uani 1 1 d . .
C2 C -0.13375(12) 1.02756(11) 0.13193(7) 0.0306(3) Uani 1 1 d . .
H33A H -0.1901 1.0056 0.1529 0.037 Uiso 1 1 calc R U
H33B H -0.0906 1.0627 0.1684 0.037 Uiso 1 1 calc R U
C3 C -0.14469(15) 0.86234(13) 0.07516(10) 0.0443(4) Uani 1 1 d . .
H32A H -0.1828 0.8837 0.0310 0.066 Uiso 1 1 calc R U
H32B H -0.1886 0.8444 0.1079 0.066 Uiso 1 1 calc R U
H32C H -0.1053 0.8091 0.0658 0.066 Uiso 1 1 calc R U
C4 C -0.00492(15) 0.90597(14) 0.17248(8) 0.0443(4) Uani 1 1 d . .
H34A H 0.0283 0.8508 0.1589 0.066 Uiso 1 1 calc R U
H34B H -0.0408 0.8905 0.2108 0.066 Uiso 1 1 calc R U
H34C H 0.0431 0.9540 0.1883 0.066 Uiso 1 1 calc R U
O2 O 0.18518(8) 0.95015(8) 0.06913(5) 0.0344(3) Uani 1 1 d . .
C21 C 0.27223(13) 0.91476(13) 0.04763(9) 0.0392(4) Uani 1 1 d . .
H11A H 0.2771 0.8475 0.0567 0.047 Uiso 1 1 calc R U
H11B H 0.3297 0.9449 0.0752 0.047 Uiso 1 1 calc R U
C22 C 0.27051(12) 0.93366(12) -0.03255(9) 0.0355(3) Uani 1 1 d . .
H12A H 0.2851 0.9994 -0.0403 0.043 Uiso 1 1 calc R U
H12B H 0.3199 0.8952 -0.0507 0.043 Uiso 1 1 calc R U
O3 O 0.03969(8) 0.81122(7) -0.00769(5) 0.0306(2) Uani 1 1 d . .
C31 C 0.06041(11) 0.76730(10) -0.07088(7) 0.0293(3) Uani 1 1 d . .
C32 C 0.15965(12) 0.80721(11) -0.08792(8) 0.0313(3) Uani 1 1 d . .
H22A H 0.2144 0.7733 -0.0602 0.038 Uiso 1 1 calc R U
H22B H 0.1631 0.7979 -0.1384 0.038 Uiso 1 1 calc R U
C33 C 0.07328(14) 0.66147(12) -0.05788(9) 0.0394(4) Uani 1 1 d . .
H24A H 0.1239 0.6508 -0.0173 0.059 Uiso 1 1 calc R U
H24B H 0.0922 0.6322 -0.0996 0.059 Uiso 1 1 calc R U
H24C H 0.0119 0.6349 -0.0486 0.059 Uiso 1 1 calc R U
C34 C -0.02624(13) 0.78427(14) -0.13135(9) 0.0429(4) Uani 1 1 d . .
H23A H -0.0848 0.7546 -0.1195 0.064 Uiso 1 1 calc R U
H23B H -0.0108 0.7581 -0.1752 0.064 Uiso 1 1 calc R U
H23C H -0.0375 0.8508 -0.1373 0.064 Uiso 1 1 calc R U
Al2 Al 0.57554(3) 0.57158(3) 1.01378(2) 0.02133(10) Uani 1 1 d . .
N2 N 0.67997(9) 0.59305(9) 0.94419(6) 0.0268(2) Uani 1 1 d . .
O4 O 0.67692(8) 0.55035(8) 1.08182(5) 0.0328(2) Uani 1 1 d . .
C41 C 0.76765(12) 0.58636(13) 1.06761(9) 0.0382(4) Uani 1 1 d . .
H41A H 0.8219 0.5556 1.0984 0.046 Uiso 1 1 calc R U
H41B H 0.7712 0.6533 1.0779 0.046 Uiso 1 1 calc R U
C42 C 0.77737(12) 0.56966(12) 0.98867(9) 0.0360(3) Uani 1 1 d . .
H42A H 0.8292 0.6094 0.9751 0.043 Uiso 1 1 calc R U
H42B H 0.7944 0.5044 0.9814 0.043 Uiso 1 1 calc R U
O5 O 0.53920(8) 0.68888(7) 0.99692(5) 0.0276(2) Uani 1 1 d . .
C51 C 0.56742(11) 0.73305(10) 0.93589(7) 0.0288(3) Uani 1 1 d . .
C52 C 0.67124(12) 0.69545(11) 0.92725(8) 0.0319(3) Uani 1 1 d . .
H52A H 0.6826 0.7058 0.8783 0.038 Uiso 1 1 calc R U
H52B H 0.7215 0.7298 0.9591 0.038 Uiso 1 1 calc R U
C53 C 0.48835(14) 0.71284(13) 0.87074(9) 0.0427(4) Uani 1 1 d . .
H53A H 0.4795 0.6460 0.8652 0.064 Uiso 1 1 calc R U
H53B H 0.5091 0.7385 0.8284 0.064 Uiso 1 1 calc R U
H53C H 0.4268 0.7413 0.8777 0.064 Uiso 1 1 calc R U
C54 C 0.57571(14) 0.83920(12) 0.94827(9) 0.0400(4) Uani 1 1 d . .
H54A H 0.5122 0.8640 0.9546 0.060 Uiso 1 1 calc R U
H54B H 0.5971 0.8687 0.9075 0.060 Uiso 1 1 calc R U
H54C H 0.6230 0.8517 0.9905 0.060 Uiso 1 1 calc R U
O6 O 0.47068(7) 0.52092(7) 1.05278(5) 0.02273(19) Uani 1 1 d . .
C61 C 0.40730(11) 0.55544(10) 1.10112(7) 0.0273(3) Uani 1 1 d . .
C62 C 0.65446(12) 0.53055(11) 0.88099(7) 0.0299(3) Uani 1 1 d . .
H62A H 0.7149 0.5087 0.8654 0.036 Uiso 1 1 calc R U
H62B H 0.6169 0.5659 0.8419 0.036 Uiso 1 1 calc R U
C63 C 0.34394(13) 0.63529(12) 1.06372(9) 0.0371(3) Uani 1 1 d . .
H63A H 0.3856 0.6880 1.0572 0.056 Uiso 1 1 calc R U
H63B H 0.2954 0.6540 1.0927 0.056 Uiso 1 1 calc R U
H63C H 0.3110 0.6140 1.0178 0.056 Uiso 1 1 calc R U
C64 C 0.47022(14) 0.59029(13) 1.16973(8) 0.0412(4) Uani 1 1 d . .
H64A H 0.5175 0.5426 1.1879 0.062 Uiso 1 1 calc R U
H64B H 0.4283 0.6037 1.2049 0.062 Uiso 1 1 calc R U
H64C H 0.5047 0.6465 1.1598 0.062 Uiso 1 1 calc R U
C101 C 0.85538(14) 0.47491(13) 0.27718(8) 0.0388(4) Uani 1 1 d . .
C102 C 0.78247(14) 0.42192(13) 0.23377(8) 0.0408(4) Uani 1 1 d . .
H102 H 0.7417 0.4508 0.1959 0.049 Uiso 1 1 calc R U
C103 C 0.77094(14) 0.32743(14) 0.24695(9) 0.0442(4) Uani 1 1 d . .
H103 H 0.7222 0.2930 0.2180 0.053 Uiso 1 1 calc R U
C104 C 0.83165(15) 0.28317(14) 0.30327(10) 0.0468(4) Uani 1 1 d . .
H104 H 0.8238 0.2193 0.3120 0.056 Uiso 1 1 calc R U
C105 C 0.90341(16) 0.33459(15) 0.34604(10) 0.0494(5) Uani 1 1 d . .
H105 H 0.9443 0.3054 0.3838 0.059 Uiso 1 1 calc R U
C106 C 0.91486(15) 0.42905(14) 0.33316(10) 0.0453(4) Uani 1 1 d . .
H106 H 0.9635 0.4629 0.3626 0.054 Uiso 1 1 calc R U
C107 C 0.86511(19) 0.57884(15) 0.26564(12) 0.0602(6) Uani 1 1 d . .
H10A H 0.8579 0.6118 0.3090 0.090 Uiso 1 1 calc R U
H10B H 0.8145 0.5991 0.2275 0.090 Uiso 1 1 calc R U
H10C H 0.9292 0.5921 0.2531 0.090 Uiso 1 1 calc R U
C108 C 0.18976(14) 0.67698(13) 0.21356(8) 0.0384(4) Uani 1 1 d . .
C109 C 0.11832(14) 0.65214(14) 0.15570(9) 0.0421(4) Uani 1 1 d . .
H109 H 0.0994 0.6954 0.1191 0.051 Uiso 1 1 calc R U
C110 C 0.07517(15) 0.56383(16) 0.15195(12) 0.0522(5) Uani 1 1 d . .
H110 H 0.0275 0.5483 0.1129 0.063 Uiso 1 1 calc R U
C111 C 0.10226(18) 0.49850(17) 0.20577(12) 0.0589(6) Uani 1 1 d . .
H111 H 0.0732 0.4391 0.2029 0.071 Uiso 1 1 calc R U
C112 C 0.17250(18) 0.52177(15) 0.26370(11) 0.0549(5) Uani 1 1 d . .
H112 H 0.1905 0.4782 0.3002 0.066 Uiso 1 1 calc R U
C113 C 0.21666(15) 0.61014(15) 0.26774(9) 0.0455(4) Uani 1 1 d . .
H113 H 0.2646 0.6251 0.3068 0.055 Uiso 1 1 calc R U
C114 C 0.23906(17) 0.77190(14) 0.21760(10) 0.0534(5) Uani 1 1 d . .
H11C H 0.2139 0.8077 0.1755 0.080 Uiso 1 1 calc R U
H11D H 0.3094 0.7639 0.2204 0.080 Uiso 1 1 calc R U
H11E H 0.2254 0.8047 0.2595 0.080 Uiso 1 1 calc R U
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
O3 Al O2 117.56(6) . .
O3 Al O1 102.94(5) . .
O2 Al O1 102.72(5) . .
O3 Al O1 120.08(5) . 3_575
O2 Al O1 120.52(6) . 3_575
O1 Al O1 77.85(4) . 3_575
O3 Al N 86.99(5) . .
O2 Al N 86.90(5) . .
O1 Al N 160.53(5) . .
O1 Al N 82.68(5) 3_575 .
O3 Al Al 117.79(5) . 3_575
O2 Al Al 117.91(5) . 3_575
O1 Al Al 38.96(3) . 3_575
O1 Al Al 38.89(3) 3_575 3_575
N Al Al 121.57(4) . 3_575
C2 N C32 114.16(11) 3_575 .
C2 N C22 113.52(12) 3_575 .
C32 N C22 111.66(12) . .
C2 N Al 108.20(9) 3_575 .
C32 N Al 103.94(9) . .
C22 N Al 104.34(9) . .
C1 O1 Al 134.46(9) . .
C1 O1 Al 119.77(9) . 3_575
Al O1 Al 102.14(4) . 3_575
O1 C1 C4 109.45(13) . .
O1 C1 C3 108.76(12) . .
C4 C1 C3 110.69(15) . .
O1 C1 C2 105.39(11) . .
C4 C1 C2 108.97(12) . .
C3 C1 C2 113.40(14) . .
N C2 C1 111.47(10) 3_575 .
C21 O2 Al 114.40(9) . .
O2 C21 C22 109.78(13) . .
N C22 C21 107.58(13) . .
C31 O3 Al 118.06(9) . .
O3 C31 C33 109.39(12) . .
O3 C31 C34 109.03(13) . .
C33 C31 C34 109.32(13) . .
O3 C31 C32 108.11(11) . .
C33 C31 C32 108.10(13) . .
C34 C31 C32 112.83(13) . .
N C32 C31 111.01(12) . .
O5 Al2 O4 117.59(6) . .
O5 Al2 O6 103.07(5) . .
O4 Al2 O6 102.28(5) . .
O5 Al2 O6 119.51(5) . 3_667
O4 Al2 O6 121.12(5) . 3_667
O6 Al2 O6 77.99(4) . 3_667
O5 Al2 N2 87.11(5) . .
O4 Al2 N2 86.96(5) . .
O6 Al2 N2 160.67(5) . .
O6 Al2 N2 82.70(5) 3_667 .
O5 Al2 Al2 117.55(4) . 3_667
O4 Al2 Al2 118.00(4) . 3_667
O6 Al2 Al2 39.04(3) . 3_667
O6 Al2 Al2 38.95(3) 3_667 3_667
N2 Al2 Al2 121.65(4) . 3_667
C62 N2 C52 114.26(11) . .
C62 N2 C42 113.24(12) . .
C52 N2 C42 111.81(12) . .
C62 N2 Al2 108.50(9) . .
C52 N2 Al2 103.64(9) . .
C42 N2 Al2 104.37(9) . .
C41 O4 Al2 114.55(9) . .
O4 C41 C42 109.98(13) . .
N2 C42 C41 107.81(13) . .
C51 O5 Al2 117.58(9) . .
O5 C51 C54 109.64(12) . .
O5 C51 C53 108.77(13) . .
C54 C51 C53 109.51(13) . .
O5 C51 C52 107.65(11) . .
C54 C51 C52 108.02(13) . .
C53 C51 C52 113.20(13) . .
N2 C52 C51 110.98(12) . .
C61 O6 Al2 134.27(9) . .
C61 O6 Al2 119.66(9) . 3_667
Al2 O6 Al2 102.01(4) . 3_667
O6 C61 C64 109.54(13) . .
O6 C61 C63 108.26(11) . .
C64 C61 C63 110.79(14) . .
O6 C61 C62 105.75(11) . 3_667
C64 C61 C62 108.99(12) . 3_667
C63 C61 C62 113.34(13) . 3_667
N2 C62 C61 111.32(11) . 3_667
C106 C101 C102 117.96(17) . .
C106 C101 C107 121.11(18) . .
C102 C101 C107 120.86(17) . .
C103 C102 C101 120.46(16) . .
C102 C103 C104 120.42(18) . .
C105 C104 C103 119.49(19) . .
C106 C105 C104 120.22(18) . .
C105 C106 C101 121.45(18) . .
C109 C108 C113 118.18(18) . .
C109 C108 C114 121.40(17) . .
C113 C108 C114 120.40(17) . .
C110 C109 C108 120.76(18) . .
C111 C110 C109 120.5(2) . .
C112 C111 C110 119.7(2) . .
C111 C112 C113 120.20(19) . .
C112 C113 C108 120.65(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al O3 1.7539(11) .
Al O2 1.7604(11) .
Al O1 1.8540(10) .
Al O1 1.8565(10) 3_575
Al N 2.1055(12) .
Al Al 2.8866(8) 3_575
N C2 1.4813(18) 3_575
N C32 1.4901(19) .
N C22 1.497(2) .
O1 C1 1.4384(16) .
O1 Al 1.8566(10) 3_575
C1 C4 1.520(2) .
C1 C3 1.530(2) .
C1 C2 1.548(2) .
C2 N 1.4814(18) 3_575
O2 C21 1.407(2) .
C21 C22 1.532(2) .
O3 C31 1.4118(17) .
C31 C33 1.528(2) .
C31 C34 1.528(2) .
C31 C32 1.548(2) .
Al2 O5 1.7522(11) .
Al2 O4 1.7598(11) .
Al2 O6 1.8539(10) .
Al2 O6 1.8571(10) 3_667
Al2 N2 2.1052(13) .
Al2 Al2 2.8842(8) 3_667
N2 C62 1.4827(18) .
N2 C52 1.4889(19) .
N2 C42 1.494(2) .
O4 C41 1.404(2) .
C41 C42 1.533(2) .
O5 C51 1.4156(17) .
C51 C54 1.526(2) .
C51 C53 1.530(2) .
C51 C52 1.547(2) .
O6 C61 1.4374(16) .
O6 Al2 1.8571(10) 3_667
C61 C64 1.519(2) .
C61 C63 1.530(2) .
C61 C62 1.550(2) 3_667
C62 C61 1.550(2) 3_667
C101 C106 1.389(3) .
C101 C102 1.404(3) .
C101 C107 1.500(3) .
C102 C103 1.378(3) .
C103 C104 1.391(3) .
C104 C105 1.377(3) .
C105 C106 1.376(3) .
C108 C109 1.390(2) .
C108 C113 1.400(2) .
C108 C114 1.503(3) .
C109 C110 1.382(3) .
C110 C111 1.382(3) .
C111 C112 1.376(3) .
C112 C113 1.389(3) .
