#------------------------------------------------------------------------------
#$Date: 2023-10-06 03:31:37 +0300 (Fri, 06 Oct 2023) $
#$Revision: 286773 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/26/7062672.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_7062672
loop_
_publ_author_name
'Schumann, Erik'
'Böhme, Uwe'
'Brendler, Erica'
'Mertens, Florian'
_publ_section_title
;
 Syntheses and ligand exchange experiments of N,N-dialkylcarbamate bridged
 {Al3(μ3-O)}7+ complexes
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16981
_journal_page_last               16992
_journal_paper_doi               10.1039/D3NJ02389C
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C51 H93 Al3 N9 O13, 11(C H Cl3), Cl'
_chemical_formula_sum            'C62 H104 Al3 Cl34 N9 O13'
_chemical_formula_weight         2469.78
_chemical_melting_point          470
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-04-19 deposited with the CCDC.	2023-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.2329(3)
_cell_length_b                   15.2329(3)
_cell_length_c                   27.0649(5)
_cell_measurement_reflns_used    31630
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.68
_cell_volume                     5438.79(18)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      153
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      ' 343 frames, detector distance = 119 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            65373
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.271
_diffrn_reflns_theta_min         2.674
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.8573
_exptl_absorpt_correction_T_min  0.7510
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-RED; Stoe, 2009'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Refined as an inversion twin. 
 Flack test results are ambiguous with a Flack parameter 
 of 0.46(5). Therefore, the absolute structure parameter
 was removed from the CIF.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7788
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0223P)²+2.0308P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7178
_reflns_number_total             7788
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3nj02389c2.cif
_cod_data_source_block           ES0114h_k2
_cod_depositor_comments
'Adding full bibliography for 7062672--7062674.cif.'
_cod_original_cell_volume        5438.8(2)
_cod_database_code               7062672
_shelx_shelxl_version_number     2017/1
_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   0.681
_shelx_estimated_absorpt_t_max   0.738
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, 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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 1.000000 1.000000 0.33515(5) 0.0334(2) Uani 1 3 d S T P . .
Al1 Al 0.76331(5) 0.46608(5) 0.57587(3) 0.02100(14) Uani 1 1 d . . . . .
O1 O 0.82498(14) 0.45447(13) 0.63491(7) 0.0247(4) Uani 1 1 d . . . . .
O2 O 0.82069(13) 0.30831(13) 0.61644(7) 0.0249(4) Uani 1 1 d . . . . .
O3 O 0.71542(13) 0.49684(13) 0.51777(7) 0.0258(4) Uani 1 1 d . . . . .
O4 O 0.54829(13) 0.40608(13) 0.53487(7) 0.0243(4) Uani 1 1 d . . . . .
O5 O 0.666667 0.333333 0.57542(11) 0.0213(6) Uani 1 3 d S T P . .
N2 N 0.9040(2) 0.39705(19) 0.68407(9) 0.0343(6) Uani 1 1 d . . . . .
N3 N 0.60245(18) 0.48946(19) 0.46224(9) 0.0314(5) Uani 1 1 d . . . . .
C1 C 0.84678(19) 0.3854(2) 0.64395(10) 0.0235(5) Uani 1 1 d . . . . .
C2 C 0.6224(2) 0.46259(19) 0.50644(10) 0.0241(5) Uani 1 1 d . . . . .
N1 N 0.87570(16) 0.61992(16) 0.58205(12) 0.0328(5) Uani 1 1 d D . . . .
H1 H 0.869(3) 0.632(3) 0.6190(16) 0.049 Uiso 1 1 d . U . . .
C3A C 0.8627(7) 0.6999(6) 0.5587(5) 0.035(2) Uani 0.761(10) 1 d D . P A 1
H3A H 0.791233 0.682748 0.562499 0.042 Uiso 0.761(10) 1 calc R U P A 1
H3B H 0.876778 0.701432 0.522919 0.042 Uiso 0.761(10) 1 calc R U P A 1
C4A C 0.9308(4) 0.8045(4) 0.5801(3) 0.0433(14) Uani 0.761(10) 1 d D . P A 1
H4A H 0.907751 0.807226 0.613959 0.052 Uiso 0.761(10) 1 calc R U P A 1
H4B H 0.924678 0.855237 0.559812 0.052 Uiso 0.761(10) 1 calc R U P A 1
C5A C 1.0420(4) 0.8322(3) 0.5819(2) 0.0405(12) Uani 0.761(10) 1 d D . P A 1
H5A H 1.069247 0.842347 0.547869 0.049 Uiso 0.761(10) 1 calc R U P A 1
H5B H 1.081723 0.896559 0.600212 0.049 Uiso 0.761(10) 1 calc R U P A 1
C6A C 1.0532(7) 0.7491(7) 0.6070(5) 0.0387(18) Uani 0.761(10) 1 d D . P A 1
H6A H 1.037710 0.747416 0.642628 0.046 Uiso 0.761(10) 1 calc R U P A 1
H6B H 1.124088 0.764053 0.603777 0.046 Uiso 0.761(10) 1 calc R U P A 1
C7A C 0.9821(3) 0.6464(3) 0.5840(2) 0.0309(11) Uani 0.761(10) 1 d D . P A 1
H7A H 1.005476 0.645492 0.549978 0.037 Uiso 0.761(10) 1 calc R U P A 1
H7B H 0.987028 0.593556 0.603122 0.037 Uiso 0.761(10) 1 calc R U P A 1
C3B C 0.8429(19) 0.6925(15) 0.5648(15) 0.031(7) Uani 0.239(10) 1 d D U P A 2
H3C H 0.797204 0.695169 0.589974 0.037 Uiso 0.239(10) 1 calc R U P A 2
H3D H 0.803217 0.665520 0.533996 0.037 Uiso 0.239(10) 1 calc R U P A 2
C4B C 0.9291(13) 0.8010(12) 0.5549(7) 0.039(4) Uani 0.239(10) 1 d D . P A 2
H4C H 0.963663 0.802672 0.523620 0.047 Uiso 0.239(10) 1 calc R U P A 2
H4D H 0.900727 0.846612 0.551258 0.047 Uiso 0.239(10) 1 calc R U P A 2
C5B C 1.0046(16) 0.8378(12) 0.5965(7) 0.049(5) Uani 0.239(10) 1 d D . P A 2
H5C H 0.971600 0.839747 0.627690 0.059 Uiso 0.239(10) 1 calc R U P A 2
H5D H 1.060952 0.906945 0.589387 0.059 Uiso 0.239(10) 1 calc R U P A 2
C6B C 1.044(2) 0.7645(17) 0.6013(19) 0.052(10) Uani 0.239(10) 1 d D . P A 2
H6C H 1.094759 0.786774 0.628375 0.063 Uiso 0.239(10) 1 calc R U P A 2
H6D H 1.078722 0.764245 0.570223 0.063 Uiso 0.239(10) 1 calc R U P A 2
C7B C 0.9576(10) 0.6580(9) 0.6119(6) 0.032(4) Uani 0.239(10) 1 d D . P A 2
H7C H 0.985016 0.611270 0.610956 0.039 Uiso 0.239(10) 1 calc R U P A 2
H7D H 0.934215 0.657224 0.646161 0.039 Uiso 0.239(10) 1 calc R U P A 2
C8 C 0.9245(2) 0.4744(2) 0.72127(11) 0.0344(6) Uani 1 1 d . . . . .
H8A H 0.910050 0.525967 0.707410 0.041 Uiso 1 1 calc R U . . .
H8B H 0.996978 0.508652 0.730752 0.041 Uiso 1 1 calc R U . . .
C9 C 0.8591(3) 0.4262(3) 0.76644(13) 0.0447(8) Uani 1 1 d . . . . .
H9A H 0.786976 0.399414 0.757746 0.054 Uiso 1 1 calc R U . . .
H9B H 0.877394 0.478126 0.792504 0.054 Uiso 1 1 calc R U . . .
C10 C 0.8734(3) 0.3400(3) 0.78610(13) 0.0518(9) Uani 1 1 d . . . . .
H10A H 0.942842 0.368457 0.799568 0.062 Uiso 1 1 calc R U . . .
H10B H 0.824881 0.305029 0.813336 0.062 Uiso 1 1 calc R U . . .
C11 C 0.8571(3) 0.2638(2) 0.74580(14) 0.0439(8) Uani 1 1 d . . . . .
H11A H 0.874052 0.213299 0.758658 0.053 Uiso 1 1 calc R U . . .
H11B H 0.784823 0.227499 0.735873 0.053 Uiso 1 1 calc R U . . .
C12 C 0.9225(2) 0.3166(2) 0.70134(12) 0.0359(7) Uani 1 1 d . . . . .
H12A H 0.994812 0.345977 0.710255 0.043 Uiso 1 1 calc R U . . .
H12B H 0.906915 0.266754 0.674497 0.043 Uiso 1 1 calc R U . . .
C13 C 0.4997(2) 0.4563(3) 0.44514(11) 0.0361(7) Uani 1 1 d . . . . .
H13A H 0.488425 0.514904 0.444414 0.043 Uiso 1 1 calc R U . . .
H13B H 0.450258 0.405533 0.468438 0.043 Uiso 1 1 calc R U . . .
C14 C 0.4826(2) 0.4100(3) 0.39381(13) 0.0460(8) Uani 1 1 d . . . . .
H14A H 0.415137 0.394625 0.381583 0.055 Uiso 1 1 calc R U . . .
H14B H 0.483592 0.345619 0.395555 0.055 Uiso 1 1 calc R U . . .
C15 C 0.5639(3) 0.4817(4) 0.35787(14) 0.0626(12) Uani 1 1 d . . . . .
H15A H 0.558006 0.543009 0.352995 0.075 Uiso 1 1 calc R U . . .
H15B H 0.554228 0.447948 0.325459 0.075 Uiso 1 1 calc R U . . .
C16 C 0.6685(3) 0.5119(4) 0.37818(13) 0.0556(10) Uani 1 1 d . . . . .
H16A H 0.676392 0.451328 0.380241 0.067 Uiso 1 1 calc R U . . .
H16B H 0.721214 0.561120 0.355514 0.067 Uiso 1 1 calc R U . . .
C17 C 0.6826(2) 0.5586(3) 0.42861(12) 0.0396(7) Uani 1 1 d . . . . .
H17A H 0.749413 0.574512 0.442015 0.048 Uiso 1 1 calc R U . . .
H17B H 0.681289 0.622783 0.426010 0.048 Uiso 1 1 calc R U . . .
C18 C 0.333333 0.666667 0.7134(4) 0.074(2) Uani 1 3 d S T P . .
H18 H 0.333332 0.666666 0.676452 0.088 Uiso 1 3 calc R U P . .
Cl2 Cl 0.45828(12) 0.74258(14) 0.73377(7) 0.1109(6) Uani 1 1 d . . . . .
C19 C 0.333333 0.666667 0.4279(3) 0.0587(17) Uani 1 3 d S T P . .
H19 H 0.333334 0.666668 0.464868 0.070 Uiso 1 3 calc R U P B 3
Cl3A Cl 0.2506(8) 0.5416(5) 0.4090(3) 0.084(3) Uani 0.72(8) 1 d . . P C 3
Cl3B Cl 0.273(6) 0.548(3) 0.4046(14) 0.128(8) Uani 0.28(8) 1 d . . P C 4
C20 C 0.5108(3) 0.6056(3) 0.56209(16) 0.0523(9) Uani 1 1 d . . . . .
H20A H 0.522045 0.546353 0.563097 0.063 Uiso 0.59(4) 1 calc R U P D 5
H20B H 0.530544 0.552117 0.562210 0.063 Uiso 0.41(4) 1 calc R U P D 6
Cl4A Cl 0.5121(8) 0.6486(8) 0.6246(4) 0.0713(16) Uani 0.59(4) 1 d . . P D 5
Cl5A Cl 0.3886(5) 0.5657(5) 0.5384(3) 0.0585(14) Uani 0.59(4) 1 d . . P D 5
Cl6A Cl 0.6061(7) 0.7026(5) 0.5236(3) 0.0499(14) Uani 0.59(4) 1 d . . P D 5
Cl4B Cl 0.5258(17) 0.6497(10) 0.6188(8) 0.086(4) Uani 0.41(4) 1 d . . P D 6
Cl5B Cl 0.3878(9) 0.5502(17) 0.5376(4) 0.079(2) Uani 0.41(4) 1 d . . P D 6
Cl6B Cl 0.5942(13) 0.6999(9) 0.5259(5) 0.080(4) Uani 0.41(4) 1 d . . P D 6
C21 C 0.1077(2) 0.2053(2) 0.40806(13) 0.0385(7) Uani 1 1 d . . . . .
H21 H 0.104892 0.146790 0.389881 0.046 Uiso 1 1 calc R U . . .
Cl7 Cl 0.22612(7) 0.27283(9) 0.43746(4) 0.0645(3) Uani 1 1 d . . . . .
Cl8 Cl 0.00999(7) 0.15813(7) 0.45202(4) 0.0558(2) Uani 1 1 d . . . . .
Cl9 Cl 0.09266(8) 0.28364(7) 0.36528(4) 0.0537(2) Uani 1 1 d . . . . .
C22 C 0.9136(3) 0.1264(3) 0.26818(13) 0.0423(7) Uani 1 1 d . . . . .
H22 H 0.965997 0.118840 0.286905 0.051 Uiso 1 1 calc R U . . .
Cl10 Cl 0.80661(7) 0.08742(7) 0.30658(4) 0.0555(2) Uani 1 1 d . . . . .
Cl11 Cl 0.96460(8) 0.25541(7) 0.25238(4) 0.0637(3) Uani 1 1 d . . . . .
Cl12 Cl 0.88056(8) 0.05007(9) 0.21515(4) 0.0607(2) 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
30 7 0 0.1200
3 30 -5 0.1297
9 2 30 0.1680
15 -13 2 0.2277
17 -13 -30 0.2347
10 3 -30 0.1931
-1 5 10 0.2031
-10 -3 0 0.1222
-6 -30 -1 0.1302
-2 -1 -6 0.1588
-10 7 -30 0.2070
-5 4 0 0.2318
-8 6 15 0.2562
-7 -14 30 0.1658
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
O5 Al1 O3 94.14(10) . . ?
O5 Al1 O1 93.74(10) . . ?
O3 Al1 O1 172.11(9) . . ?
O5 Al1 O2 96.92(8) . 2_655 ?
O3 Al1 O2 91.39(9) . 2_655 ?
O1 Al1 O2 87.22(8) . 2_655 ?
O5 Al1 O4 96.10(8) . 3_665 ?
O3 Al1 O4 87.22(9) . 3_665 ?
O1 Al1 O4 92.39(8) . 3_665 ?
O2 Al1 O4 166.97(8) 2_655 3_665 ?
O5 Al1 N1 175.83(14) . . ?
O3 Al1 N1 89.43(10) . . ?
O1 Al1 N1 82.68(10) . . ?
O2 Al1 N1 80.82(9) 2_655 . ?
O4 Al1 N1 86.21(9) 3_665 . ?
C1 O1 Al1 125.53(17) . . ?
C1 O2 Al1 129.18(16) . 3_665 ?
C2 O3 Al1 125.82(17) . . ?
C2 O4 Al1 127.69(16) . 2_655 ?
Al1 O5 Al1 119.997(3) 2_655 . ?
Al1 O5 Al1 119.995(3) 2_655 3_665 ?
Al1 O5 Al1 119.995(3) . 3_665 ?
C1 N2 C8 121.7(2) . . ?
C1 N2 C12 122.0(2) . . ?
C8 N2 C12 113.7(2) . . ?
C2 N3 C13 122.9(2) . . ?
C2 N3 C17 122.5(2) . . ?
C13 N3 C17 114.6(2) . . ?
O2 C1 O1 123.9(2) . . ?
O2 C1 N2 118.3(2) . . ?
O1 C1 N2 117.7(2) . . ?
O3 C2 O4 123.8(2) . . ?
O3 C2 N3 117.5(2) . . ?
O4 C2 N3 118.7(2) . . ?
C7A N1 C3A 112.1(5) . . ?
C7B N1 C3B 116.6(12) . . ?
C7B N1 Al1 126.0(5) . . ?
C7A N1 Al1 118.79(19) . . ?
C3A N1 Al1 121.1(4) . . ?
C3B N1 Al1 114.3(9) . . ?
C7B N1 H1 60(2) . . ?
C7A N1 H1 97(2) . . ?
C3A N1 H1 101(2) . . ?
C3B N1 H1 94(3) . . ?
Al1 N1 H1 100(2) . . ?
N1 C3A C4A 113.7(6) . . ?
N1 C3A H3A 108.8 . . ?
C4A C3A H3A 108.8 . . ?
N1 C3A H3B 108.8 . . ?
C4A C3A H3B 108.8 . . ?
H3A C3A H3B 107.7 . . ?
C3A C4A C5A 112.6(6) . . ?
C3A C4A H4A 109.1 . . ?
C5A C4A H4A 109.1 . . ?
C3A C4A H4B 109.1 . . ?
C5A C4A H4B 109.1 . . ?
H4A C4A H4B 107.8 . . ?
C6A C5A C4A 110.8(6) . . ?
C6A C5A H5A 109.5 . . ?
C4A C5A H5A 109.5 . . ?
C6A C5A H5B 109.5 . . ?
C4A C5A H5B 109.5 . . ?
H5A C5A H5B 108.1 . . ?
C5A C6A C7A 110.8(7) . . ?
C5A C6A H6A 109.5 . . ?
C7A C6A H6A 109.5 . . ?
C5A C6A H6B 109.5 . . ?
C7A C6A H6B 109.5 . . ?
H6A C6A H6B 108.1 . . ?
N1 C7A C6A 114.7(5) . . ?
N1 C7A H7A 108.6 . . ?
C6A C7A H7A 108.6 . . ?
N1 C7A H7B 108.6 . . ?
C6A C7A H7B 108.6 . . ?
H7A C7A H7B 107.6 . . ?
N1 C3B C4B 115.3(16) . . ?
N1 C3B H3C 108.4 . . ?
C4B C3B H3C 108.4 . . ?
N1 C3B H3D 108.4 . . ?
C4B C3B H3D 108.4 . . ?
H3C C3B H3D 107.5 . . ?
C5B C4B C3B 110.7(18) . . ?
C5B C4B H4C 109.5 . . ?
C3B C4B H4C 109.5 . . ?
C5B C4B H4D 109.5 . . ?
C3B C4B H4D 109.5 . . ?
H4C C4B H4D 108.1 . . ?
C4B C5B C6B 108(2) . . ?
C4B C5B H5C 110.2 . . ?
C6B C5B H5C 110.2 . . ?
C4B C5B H5D 110.2 . . ?
C6B C5B H5D 110.2 . . ?
H5C C5B H5D 108.5 . . ?
C5B C6B C7B 110.1(19) . . ?
C5B C6B H6C 109.6 . . ?
C7B C6B H6C 109.6 . . ?
C5B C6B H6D 109.6 . . ?
C7B C6B H6D 109.6 . . ?
H6C C6B H6D 108.1 . . ?
N1 C7B C6B 117.9(17) . . ?
N1 C7B H1 47(2) . . ?
C6B C7B H1 127(2) . . ?
N1 C7B H7C 107.8 . . ?
C6B C7B H7C 107.8 . . ?
H1 C7B H7C 124.8 . . ?
N1 C7B H7D 107.8 . . ?
C6B C7B H7D 107.8 . . ?
H1 C7B H7D 61.1 . . ?
H7C C7B H7D 107.2 . . ?
N2 C8 C9 110.0(3) . . ?
N2 C8 H8A 109.7 . . ?
C9 C8 H8A 109.7 . . ?
N2 C8 H8B 109.7 . . ?
C9 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
C8 C9 C10 110.7(3) . . ?
C8 C9 H9A 109.5 . . ?
C10 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C11 C10 C9 111.5(3) . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C10 110.7(3) . . ?
C12 C11 H11A 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
N2 C12 C11 110.3(3) . . ?
N2 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
N2 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
N3 C13 C14 110.8(3) . . ?
N3 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C13 C14 C15 111.2(3) . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 109.8(3) . . ?
C14 C15 H15A 109.7 . . ?
C16 C15 H15A 109.7 . . ?
C14 C15 H15B 109.7 . . ?
C16 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C17 C16 C15 110.5(3) . . ?
C17 C16 H16A 109.6 . . ?
C15 C16 H16A 109.6 . . ?
C17 C16 H16B 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
N3 C17 C16 110.7(3) . . ?
N3 C17 H17A 109.5 . . ?
C16 C17 H17A 109.5 . . ?
N3 C17 H17B 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
Cl2 C18 Cl2 110.6(3) 2_665 3_565 ?
Cl2 C18 Cl2 110.6(3) 2_665 . ?
Cl2 C18 Cl2 110.6(3) 3_565 . ?
Cl2 C18 H18 108.4 2_665 . ?
Cl2 C18 H18 108.4 3_565 . ?
Cl2 C18 H18 108.4 . . ?
Cl3B C19 Cl3B 106.9(16) 3_565 2_665 ?
Cl3B C19 Cl3B 106.9(17) 3_565 . ?
Cl3B C19 Cl3B 106.9(16) 2_665 . ?
Cl3A C19 Cl3A 111.9(3) 3_565 2_665 ?
Cl3A C19 Cl3A 111.9(3) 3_565 . ?
Cl3A C19 Cl3A 111.9(3) 2_665 . ?
Cl3A C19 H19 107.0 3_565 . ?
Cl3A C19 H19 107.0 2_665 . ?
Cl3A C19 H19 107.0 . . ?
Cl4B C20 Cl6B 107.7(8) . . ?
Cl4B C20 Cl5B 116.5(11) . . ?
Cl6B C20 Cl5B 111.2(6) . . ?
Cl5A C20 Cl6A 110.6(4) . . ?
Cl5A C20 Cl4A 106.5(5) . . ?
Cl6A C20 Cl4A 112.7(5) . . ?
Cl5A C20 H20A 109.0 . . ?
Cl6A C20 H20A 109.0 . . ?
Cl4A C20 H20A 109.0 . . ?
Cl4B C20 H20B 107.0 . . ?
Cl6B C20 H20B 107.0 . . ?
Cl5B C20 H20B 107.0 . . ?
Cl8 C21 Cl7 110.18(19) . . ?
Cl8 C21 Cl9 110.64(18) . . ?
Cl7 C21 Cl9 110.18(18) . . ?
Cl8 C21 H21 108.6 . . ?
Cl7 C21 H21 108.6 . . ?
Cl9 C21 H21 108.6 . . ?
Cl12 C22 Cl10 110.34(19) . . ?
Cl12 C22 Cl11 111.10(19) . . ?
Cl10 C22 Cl11 109.6(2) . . ?
Cl12 C22 H22 108.6 . . ?
Cl10 C22 H22 108.6 . . ?
Cl11 C22 H22 108.6 . . ?
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 O5 1.8110(7) . ?
Al1 O3 1.8885(19) . ?
Al1 O1 1.906(2) . ?
Al1 O2 1.9138(19) 2_655 ?
Al1 O4 1.9146(19) 3_665 ?
Al1 N1 2.107(2) . ?
O1 C1 1.275(3) . ?
O2 C1 1.275(3) . ?
O3 C2 1.278(3) . ?
O4 C2 1.279(3) . ?
N2 C1 1.348(3) . ?
N2 C8 1.460(4) . ?
N2 C12 1.464(4) . ?
N3 C2 1.348(3) . ?
N3 C13 1.459(4) . ?
N3 C17 1.464(4) . ?
N1 C7B 1.350(11) . ?
N1 C7A 1.463(4) . ?
N1 C3A 1.471(7) . ?
N1 C3B 1.497(18) . ?
N1 H1 1.03(4) . ?
C3A C4A 1.515(10) . ?
C3A H3A 0.9900 . ?
C3A H3B 0.9900 . ?
C4A C5A 1.528(8) . ?
C4A H4A 0.9900 . ?
C4A H4B 0.9900 . ?
C5A C6A 1.519(10) . ?
C5A H5A 0.9900 . ?
C5A H5B 0.9900 . ?
C6A C7A 1.522(9) . ?
C6A H6A 0.9900 . ?
C6A H6B 0.9900 . ?
C7A H7A 0.9900 . ?
C7A H7B 0.9900 . ?
C3B C4B 1.54(2) . ?
C3B H3C 0.9900 . ?
C3B H3D 0.9900 . ?
C4B C5B 1.503(19) . ?
C4B H4C 0.9900 . ?
C4B H4D 0.9900 . ?
C5B C6B 1.52(2) . ?
C5B H5C 0.9900 . ?
C5B H5D 0.9900 . ?
C6B C7B 1.52(2) . ?
C6B H6C 0.9900 . ?
C6B H6D 0.9900 . ?
C7B H1 1.22(4) . ?
C7B H7C 0.9900 . ?
C7B H7D 0.9900 . ?
C8 C9 1.515(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.531(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.519(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.512(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.520(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.523(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.524(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.504(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 Cl2 1.750(4) 2_665 ?
C18 Cl2 1.750(4) 3_565 ?
C18 Cl2 1.750(4) . ?
C18 H18 1.0000 . ?
C19 Cl3B 1.69(3) 3_565 ?
C19 Cl3B 1.69(3) 2_665 ?
C19 Cl3B 1.69(3) . ?
C19 Cl3A 1.755(8) 3_565 ?
C19 Cl3A 1.755(8) 2_665 ?
C19 Cl3A 1.755(8) . ?
C19 H19 1.0000 . ?
C20 Cl4B 1.65(2) . ?
C20 Cl6B 1.677(15) . ?
C20 Cl5B 1.755(13) . ?
C20 Cl5A 1.765(8) . ?
C20 Cl6A 1.798(9) . ?
C20 Cl4A 1.812(12) . ?
C20 H20A 1.0000 . ?
C20 H20B 1.0000 . ?
C21 Cl8 1.755(3) . ?
C21 Cl7 1.757(3) . ?
C21 Cl9 1.758(4) . ?
C21 H21 1.0000 . ?
C22 Cl12 1.755(4) . ?
C22 Cl10 1.766(4) . ?
C22 Cl11 1.766(3) . ?
C22 H22 1.0000 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C3A^a H3A^a O2 0.99 2.69 3.154(10) 109.0 2_655 yes
C6A^a H6A^a Cl11 0.99 2.97 3.942(13) 167.2 4_765 yes
C7A^a H7B^a O1 0.99 2.47 3.029(4) 115.5 . yes
C3B^b H3D^b O3 0.99 2.27 2.91(3) 121.7 . yes
C4B^b H4D^b Cl8 0.99 2.85 3.339(18) 111.6 2_665 yes
C4B^b H4C^b Cl7 0.99 2.79 3.77(2) 170.8 3_665 yes
C14 H14A Cl7 0.99 2.95 3.587(4) 123.4 . yes
C20 H20A^e O4 1.00 2.48 3.442(4) 160.5 . yes
C21 H21 Cl1 1.00 2.48 3.352(3) 144.8 1_445 yes
C22 H22 Cl1 1.00 2.49 3.356(3) 145.0 1_545 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 Al1 O3 C2 40.4(2) . . . . ?
O2 Al1 O3 C2 -56.6(2) 2_655 . . . ?
O4 Al1 O3 C2 136.3(2) 3_665 . . . ?
N1 Al1 O3 C2 -137.4(2) . . . . ?
O3 Al1 O5 Al1 -57.32(19) . . . 2_655 ?
O1 Al1 O5 Al1 122.23(18) . . . 2_655 ?
O2 Al1 O5 Al1 34.6(2) 2_655 . . 2_655 ?
O4 Al1 O5 Al1 -144.97(17) 3_665 . . 2_655 ?
O3 Al1 O5 Al1 124.01(18) . . . 3_665 ?
O1 Al1 O5 Al1 -56.44(19) . . . 3_665 ?
O2 Al1 O5 Al1 -144.08(17) 2_655 . . 3_665 ?
O4 Al1 O5 Al1 36.4(2) 3_665 . . 3_665 ?
Al1 O2 C1 O1 -31.3(4) 3_665 . . . ?
Al1 O2 C1 N2 151.3(2) 3_665 . . . ?
Al1 O1 C1 O2 -7.4(4) . . . . ?
Al1 O1 C1 N2 170.03(19) . . . . ?
C8 N2 C1 O2 -170.8(3) . . . . ?
C12 N2 C1 O2 -10.4(4) . . . . ?
C8 N2 C1 O1 11.6(4) . . . . ?
C12 N2 C1 O1 172.0(3) . . . . ?
Al1 O3 C2 O4 4.0(4) . . . . ?
Al1 O3 C2 N3 -177.13(18) . . . . ?
Al1 O4 C2 O3 -40.3(4) 2_655 . . . ?
Al1 O4 C2 N3 140.9(2) 2_655 . . . ?
C13 N3 C2 O3 -179.4(3) . . . . ?
C17 N3 C2 O3 -2.6(4) . . . . ?
C13 N3 C2 O4 -0.5(4) . . . . ?
C17 N3 C2 O4 176.3(3) . . . . ?
C7A N1 C3A C4A -50.7(11) . . . . ?
Al1 N1 C3A C4A 160.8(6) . . . . ?
N1 C3A C4A C5A 51.3(12) . . . . ?
C3A C4A C5A C6A -51.4(11) . . . . ?
C4A C5A C6A C7A 51.5(11) . . . . ?
C3A N1 C7A C6A 52.4(9) . . . . ?
Al1 N1 C7A C6A -158.4(6) . . . . ?
C5A C6A C7A N1 -53.4(10) . . . . ?
C7B N1 C3B C4B 35(4) . . . . ?
Al1 N1 C3B C4B -163(2) . . . . ?
N1 C3B C4B C5B -46(4) . . . . ?
C3B C4B C5B C6B 58(3) . . . . ?
C4B C5B C6B C7B -60(4) . . . . ?
C3B N1 C7B C6B -38(3) . . . . ?
Al1 N1 C7B C6B 163.3(19) . . . . ?
C5B C6B C7B N1 51(4) . . . . ?
C1 N2 C8 C9 103.1(3) . . . . ?
C12 N2 C8 C9 -58.8(3) . . . . ?
N2 C8 C9 C10 54.6(4) . . . . ?
C8 C9 C10 C11 -53.1(4) . . . . ?
C9 C10 C11 C12 53.1(4) . . . . ?
C1 N2 C12 C11 -102.8(3) . . . . ?
C8 N2 C12 C11 59.0(3) . . . . ?
C10 C11 C12 N2 -54.8(3) . . . . ?
C2 N3 C13 C14 -128.6(3) . . . . ?
C17 N3 C13 C14 54.4(4) . . . . ?
N3 C13 C14 C15 -53.3(4) . . . . ?
C13 C14 C15 C16 55.0(5) . . . . ?
C14 C15 C16 C17 -56.5(5) . . . . ?
C2 N3 C17 C16 126.8(3) . . . . ?
C13 N3 C17 C16 -56.2(4) . . . . ?
C15 C16 C17 N3 56.2(4) . . . . ?
