# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_12_wa3590_pl413
_database_code_depnum_ccdc_archive 'CCDC 2385628'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT601_12_wa3590_pl413     
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .         39 Ang**3
RESPONSE: No any significant residual density left. This is just an 
effect of crystal packing.
;
_vrf_PLAT910_12_wa3590_pl413     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         10 Note  
RESPONSE: These reflections are hidden by the beamstop.
;
_vrf_PLAT911_12_wa3590_pl413     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          4 Report
RESPONSE: These reflections belong to the Lorentz area of the detector.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H28 Al4'
_chemical_formula_sum            'C28 H28 Al4'
_chemical_formula_weight         472.42

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7750(3)
_cell_length_b                   16.6702(6)
_cell_length_c                   25.7105(8)
_cell_angle_alpha                107.247(3)
_cell_angle_beta                 93.692(3)
_cell_angle_gamma                98.988(3)
_cell_volume                     3924.7(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    14911
_cell_measurement_theta_min      2.6840
_cell_measurement_theta_max      27.7910

_exptl_crystal_description       'elongated prism'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_F_000             1488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.192
_shelx_estimated_absorpt_T_min   0.924
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_T_min  0.76499
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            53408
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.372
_diffrn_reflns_theta_max         26.733
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             16650
_reflns_number_gt                13432
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  'IUCr PublCIF online service'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0531P)²+0.4904P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16650
_refine_ls_number_parameters     877
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1139
_refine_ls_wR_factor_gt          0.1052
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Al1 Al 0.52633(5) 0.00720(3) 0.18884(2) 0.02377(11) Uani 1 1 d . . . . .
Al2 Al 0.53539(5) 0.13791(3) 0.14832(2) 0.02201(11) Uani 1 1 d . . . . .
Al3 Al 0.21589(5) 0.09895(3) 0.20776(2) 0.02437(12) Uani 1 1 d . . . . .
Al4 Al 0.20418(5) -0.01109(3) 0.10789(2) 0.02372(11) Uani 1 1 d . . . . .
C1 C 0.6929(2) -0.03182(14) 0.21117(10) 0.0416(5) Uani 1 1 d . . . . .
H1A H 0.703997 -0.019340 0.251086 0.062 Uiso 1 1 calc R U . . .
H1B H 0.775098 -0.002104 0.200117 0.062 Uiso 1 1 calc R U . . .
H1C H 0.682906 -0.093536 0.193473 0.062 Uiso 1 1 calc R U . . .
C2 C 0.71319(18) 0.19948(12) 0.13677(8) 0.0324(4) Uani 1 1 d . . . . .
H2A H 0.731311 0.175349 0.098741 0.049 Uiso 1 1 calc R U . . .
H2B H 0.788666 0.193773 0.161670 0.049 Uiso 1 1 calc R U . . .
H2C H 0.708383 0.260053 0.144123 0.049 Uiso 1 1 calc R U . . .
C3 C 0.0509(2) 0.13512(14) 0.23942(9) 0.0424(5) Uani 1 1 d . . . . .
H3A H 0.044977 0.122814 0.274274 0.064 Uiso 1 1 calc R U . . .
H3B H -0.032717 0.104080 0.214029 0.064 Uiso 1 1 calc R U . . .
H3C H 0.057490 0.196638 0.245855 0.064 Uiso 1 1 calc R U . . .
C4 C 0.0280(2) -0.07022(14) 0.06275(9) 0.0404(5) Uani 1 1 d . . . . .
H4A H 0.020429 -0.052167 0.029870 0.061 Uiso 1 1 calc R U . . .
H4B H -0.049841 -0.056088 0.083800 0.061 Uiso 1 1 calc R U . . .
H4C H 0.024968 -0.132060 0.051939 0.061 Uiso 1 1 calc R U . . .
C13 C 0.4033(2) 0.19519(11) 0.30686(7) 0.0303(4) Uani 1 1 d . . . . .
H13 H 0.317758 0.202016 0.321692 0.036 Uiso 1 1 calc R U . . .
C14 C 0.5272(2) 0.23090(13) 0.34066(8) 0.0374(5) Uani 1 1 d . . . . .
H14 H 0.525363 0.261140 0.378199 0.045 Uiso 1 1 calc R U . . .
C15 C 0.6540(2) 0.22311(13) 0.32044(8) 0.0374(5) Uani 1 1 d . . . . .
H15 H 0.738958 0.248694 0.343641 0.045 Uiso 1 1 calc R U . . .
C16 C 0.65509(19) 0.17741(12) 0.26581(7) 0.0314(4) Uani 1 1 d . . . . .
H16 H 0.742006 0.171815 0.251907 0.038 Uiso 1 1 calc R U . . .
C17 C 0.40006(18) 0.14929(10) 0.25146(7) 0.0242(3) Uani 1 1 d . . . . .
C18 C 0.53064(18) 0.13904(11) 0.23036(7) 0.0250(4) Uani 1 1 d . . . . .
C21 C 0.51536(18) 0.00461(11) 0.10602(7) 0.0247(3) Uani 1 1 d . . . . .
C22 C 0.37980(18) -0.03667(11) 0.07806(7) 0.0237(3) Uani 1 1 d . . . . .
C23 C 0.3711(2) -0.09746(11) 0.02657(7) 0.0293(4) Uani 1 1 d . . . . .
H23 H 0.281747 -0.125646 0.007612 0.035 Uiso 1 1 calc R U . . .
C24 C 0.4891(2) -0.11798(12) 0.00222(7) 0.0325(4) Uani 1 1 d . . . . .
H24 H 0.479410 -0.160204 -0.032663 0.039 Uiso 1 1 calc R U . . .
C25 C 0.6209(2) -0.07730(12) 0.02846(7) 0.0303(4) Uani 1 1 d . . . . .
H25 H 0.701586 -0.090474 0.011498 0.036 Uiso 1 1 calc R U . . .
C26 C 0.63332(19) -0.01714(11) 0.07978(8) 0.0283(4) Uani 1 1 d . . . . .
H26 H 0.723762 0.010351 0.097902 0.034 Uiso 1 1 calc R U . . .
C31 C 0.34302(18) -0.05471(11) 0.19813(7) 0.0242(3) Uani 1 1 d . . . . .
C32 C 0.21122(18) -0.03433(11) 0.18488(7) 0.0265(4) Uani 1 1 d . . . . .
C33 C 0.08922(19) -0.08460(12) 0.19316(8) 0.0302(4) Uani 1 1 d . . . . .
H33 H 0.001092 -0.071423 0.184576 0.036 Uiso 1 1 calc R U . . .
C34 C 0.0942(2) -0.15248(12) 0.21341(8) 0.0336(4) Uani 1 1 d . . . . .
H34 H 0.010628 -0.185651 0.218334 0.040 Uiso 1 1 calc R U . . .
C35 C 0.2219(2) -0.17126(12) 0.22630(9) 0.0372(5) Uani 1 1 d . . . . .
H35 H 0.226489 -0.217285 0.240628 0.045 Uiso 1 1 calc R U . . .
C36 C 0.3446(2) -0.12331(12) 0.21852(8) 0.0324(4) Uani 1 1 d . . . . .
H36 H 0.431482 -0.137762 0.227330 0.039 Uiso 1 1 calc R U . . .
C41 C 0.35644(17) 0.17013(10) 0.12764(7) 0.0229(3) Uani 1 1 d . . . . .
C42 C 0.22342(18) 0.12235(11) 0.13065(7) 0.0263(4) Uani 1 1 d . . . . .
C43 C 0.10132(19) 0.14849(12) 0.11439(8) 0.0321(4) Uani 1 1 d . . . . .
H43 H 0.013107 0.116791 0.116216 0.038 Uiso 1 1 calc R U . . .
C44 C 0.1058(2) 0.21853(13) 0.09592(9) 0.0380(5) Uani 1 1 d . . . . .
H44 H 0.022233 0.234732 0.085106 0.046 Uiso 1 1 calc R U . . .
C45 C 0.2342(2) 0.26458(13) 0.09349(9) 0.0410(5) Uani 1 1 d . . . . .
H45 H 0.238819 0.312820 0.080756 0.049 Uiso 1 1 calc R U . . .
C46 C 0.3570(2) 0.24130(11) 0.10943(8) 0.0298(4) Uani 1 1 d . . . . .
H46 H 0.443814 0.274763 0.107888 0.036 Uiso 1 1 calc R U . . .
Al5 Al 0.43774(5) 0.50281(3) 0.89261(2) 0.02361(11) Uani 1 1 d . . . . .
Al6 Al 0.38157(5) 0.38071(3) 0.79594(2) 0.02381(11) Uani 1 1 d . . . . .
Al7 Al 0.14129(5) 0.52787(3) 0.81034(2) 0.02329(11) Uani 1 1 d . . . . .
Al8 Al 0.07078(5) 0.41361(3) 0.86194(2) 0.02330(11) Uani 1 1 d . . . . .
C5 C 0.61740(19) 0.53310(13) 0.93866(8) 0.0362(4) Uani 1 1 d . . . . .
H5A H 0.636855 0.594623 0.958060 0.054 Uiso 1 1 calc R U . . .
H5B H 0.691345 0.518221 0.915572 0.054 Uiso 1 1 calc R U . . .
H5C H 0.613822 0.501584 0.965381 0.054 Uiso 1 1 calc R U . . .
C6 C 0.5215(2) 0.31831(14) 0.76145(9) 0.0396(5) Uani 1 1 d . . . . .
H6A H 0.488837 0.256892 0.753965 0.059 Uiso 1 1 calc R U . . .
H6B H 0.609037 0.336489 0.786075 0.059 Uiso 1 1 calc R U . . .
H6C H 0.537010 0.330160 0.726956 0.059 Uiso 1 1 calc R U . . .
C7 C 0.0019(2) 0.58557(13) 0.78617(9) 0.0361(4) Uani 1 1 d . . . . .
H7A H -0.086603 0.570179 0.799805 0.054 Uiso 1 1 calc R U . . .
H7B H -0.011540 0.567881 0.746007 0.054 Uiso 1 1 calc R U . . .
H7C H 0.034024 0.647560 0.800584 0.054 Uiso 1 1 calc R U . . .
C8 C -0.12059(19) 0.38697(13) 0.87783(8) 0.0344(4) Uani 1 1 d . . . . .
H8A H -0.152904 0.324936 0.864769 0.052 Uiso 1 1 calc R U . . .
H8B H -0.180931 0.414261 0.859223 0.052 Uiso 1 1 calc R U . . .
H8C H -0.124008 0.408349 0.917493 0.052 Uiso 1 1 calc R U . . .
C51 C 0.44663(17) 0.51486(11) 0.81271(7) 0.0253(4) Uani 1 1 d . . . . .
C52 C 0.33759(17) 0.55235(10) 0.79481(7) 0.0231(3) Uani 1 1 d . . . . .
C53 C 0.37019(18) 0.60642(11) 0.76323(7) 0.0271(4) Uani 1 1 d . . . . .
H53 H 0.299002 0.632070 0.751395 0.032 Uiso 1 1 calc R U . . .
C54 C 0.5035(2) 0.62394(12) 0.74852(8) 0.0327(4) Uani 1 1 d . . . . .
H54 H 0.522001 0.660559 0.726673 0.039 Uiso 1 1 calc R U . . .
C55 C 0.60889(19) 0.58806(12) 0.76570(8) 0.0335(4) Uani 1 1 d . . . . .
H55 H 0.700115 0.600046 0.755854 0.040 Uiso 1 1 calc R U . . .
C56 C 0.58102(18) 0.53454(12) 0.79732(8) 0.0290(4) Uani 1 1 d . . . . .
H56 H 0.654334 0.510313 0.809051 0.035 Uiso 1 1 calc R U . . .
C61 C 0.35698(18) 0.37037(11) 0.87518(7) 0.0249(3) Uani 1 1 d . . . . .
C62 C 0.21331(17) 0.35320(10) 0.88360(7) 0.0230(3) Uani 1 1 d . . . . .
C63 C 0.17203(19) 0.28876(12) 0.90693(8) 0.0308(4) Uani 1 1 d . . . . .
H63 H 0.077483 0.276932 0.913369 0.037 Uiso 1 1 calc R U . . .
C64 C 0.2652(2) 0.24147(13) 0.92099(9) 0.0376(5) Uani 1 1 d . . . . .
H64 H 0.233528 0.198162 0.936793 0.045 Uiso 1 1 calc R U . . .
C65 C 0.4037(2) 0.25693(12) 0.91218(8) 0.0329(4) Uani 1 1 d . . . . .
H65 H 0.466986 0.223965 0.921282 0.039 Uiso 1 1 calc R U . . .
C66 C 0.44868(18) 0.32111(11) 0.88992(7) 0.0281(4) Uani 1 1 d . . . . .
H66 H 0.544038 0.332355 0.884383 0.034 Uiso 1 1 calc R U . . .
C71 C 0.28828(18) 0.56503(11) 0.92244(7) 0.0249(3) Uani 1 1 d . . . . .
C72 C 0.14928(18) 0.54661(11) 0.89575(7) 0.0261(4) Uani 1 1 d . . . . .
C73 C 0.0504(2) 0.59331(12) 0.92193(8) 0.0315(4) Uani 1 1 d . . . . .
H73 H -0.042476 0.581121 0.904478 0.038 Uiso 1 1 calc R U . . .
C74 C 0.0850(2) 0.65619(13) 0.97219(8) 0.0369(4) Uani 1 1 d . . . . .
H74 H 0.016668 0.686411 0.989119 0.044 Uiso 1 1 calc R U . . .
C75 C 0.2205(2) 0.67456(13) 0.99754(8) 0.0383(5) Uani 1 1 d . . . . .
H75 H 0.245392 0.718009 1.031907 0.046 Uiso 1 1 calc R U . . .
C76 C 0.3202(2) 0.62983(12) 0.97302(8) 0.0324(4) Uani 1 1 d . . . . .
H76 H 0.412692 0.643566 0.991058 0.039 Uiso 1 1 calc R U . . .
C81 C 0.18993(18) 0.34998(11) 0.75718(7) 0.0251(4) Uani 1 1 d . . . . .
C82 C 0.07917(18) 0.39352(11) 0.77626(7) 0.0252(4) Uani 1 1 d . . . . .
C83 C -0.05326(19) 0.36615(12) 0.74452(8) 0.0310(4) Uani 1 1 d . . . . .
H83 H -0.127148 0.395473 0.756251 0.037 Uiso 1 1 calc R U . . .
C84 C -0.0772(2) 0.29756(13) 0.69676(8) 0.0384(5) Uani 1 1 d . . . . .
H84 H -0.166667 0.279992 0.676032 0.046 Uiso 1 1 calc R U . . .
C85 C 0.0299(2) 0.25486(13) 0.67946(8) 0.0412(5) Uani 1 1 d . . . . .
H85 H 0.013228 0.206976 0.647154 0.049 Uiso 1 1 calc R U . . .
C86 C 0.1614(2) 0.28116(12) 0.70876(8) 0.0347(4) Uani 1 1 d . . . . .
H86 H 0.234098 0.251677 0.695618 0.042 Uiso 1 1 calc R U . . .
Al9 Al 0.46662(6) 0.19185(4) 0.48263(2) 0.03087(13) Uani 1 1 d . . . . .
Al10 Al 0.45419(5) 0.32085(3) 0.57159(2) 0.02731(12) Uani 1 1 d . . . . .
Al11 Al 0.12416(6) 0.17414(4) 0.52703(2) 0.02968(13) Uani 1 1 d . . . . .
Al12 Al 0.16143(6) 0.28207(4) 0.46785(2) 0.02909(12) Uani 1 1 d . . . . .
C9 C 0.6422(2) 0.15775(16) 0.46173(10) 0.0478(5) Uani 1 1 d . . . . .
H9A H 0.642657 0.099981 0.463705 0.072 Uiso 1 1 calc R U . . .
H9B H 0.719854 0.197719 0.486801 0.072 Uiso 1 1 calc R U . . .
H9C H 0.652237 0.158401 0.424171 0.072 Uiso 1 1 calc R U . . .
C10 C 0.6221(2) 0.38482(14) 0.62106(8) 0.0398(5) Uani 1 1 d . . . . .
H10A H 0.699888 0.354541 0.611858 0.060 Uiso 1 1 calc R U . . .
H10B H 0.605440 0.390043 0.658998 0.060 Uiso 1 1 calc R U . . .
H10C H 0.645212 0.441904 0.617087 0.060 Uiso 1 1 calc R U . . .
C11 C -0.0584(2) 0.11267(14) 0.53442(9) 0.0415(5) Uani 1 1 d . . . . .
H11A H -0.045708 0.076802 0.557781 0.062 Uiso 1 1 calc R U . . .
H11B H -0.103907 0.076615 0.498116 0.062 Uiso 1 1 calc R U . . .
H11C H -0.116761 0.153928 0.551040 0.062 Uiso 1 1 calc R U . . .
C12 C 0.0061(2) 0.30933(17) 0.42856(10) 0.0498(6) Uani 1 1 d . . . . .
H12A H -0.082062 0.277862 0.434302 0.075 Uiso 1 1 calc R U . . .
H12B H 0.015987 0.292944 0.389292 0.075 Uiso 1 1 calc R U . . .
H12C H 0.006443 0.370842 0.442378 0.075 Uiso 1 1 calc R U . . .
C91 C 0.4306(2) 0.18814(12) 0.56217(8) 0.0328(4) Uani 1 1 d . . . . .
C92 C 0.2904(2) 0.15219(12) 0.56590(7) 0.0308(4) Uani 1 1 d . . . . .
C93 C 0.2700(2) 0.09924(13) 0.59908(8) 0.0397(5) Uani 1 1 d . . . . .
H93 H 0.177714 0.073438 0.601379 0.048 Uiso 1 1 calc R U . . .
C94 C 0.3813(3) 0.08334(15) 0.62885(9) 0.0489(6) Uani 1 1 d . . . . .
H94 H 0.363811 0.048187 0.651670 0.059 Uiso 1 1 calc R U . . .
C95 C 0.5166(3) 0.11826(14) 0.62539(9) 0.0466(5) Uani 1 1 d . . . . .
H95 H 0.592355 0.107192 0.645595 0.056 Uiso 1 1 calc R U . . .
C96 C 0.5406(2) 0.16941(13) 0.59231(8) 0.0390(5) Uani 1 1 d . . . . .
H96 H 0.634024 0.192781 0.589686 0.047 Uiso 1 1 calc R U . . .
C101 C 0.47560(19) 0.32404(12) 0.49062(7) 0.0283(4) Uani 1 1 d . . . . .
C102 C 0.35373(19) 0.33756(11) 0.46320(7) 0.0280(4) Uani 1 1 d . . . . .
C103 C 0.3711(2) 0.39368(12) 0.43189(8) 0.0336(4) Uani 1 1 d . . . . .
H103 H 0.291214 0.403455 0.413317 0.040 Uiso 1 1 calc R U . . .
C104 C 0.5031(2) 0.43555(13) 0.42736(9) 0.0401(5) Uani 1 1 d . . . . .
H104 H 0.511778 0.472807 0.405579 0.048 Uiso 1 1 calc R U . . .
C105 C 0.6207(2) 0.42327(13) 0.45420(8) 0.0375(5) Uani 1 1 d . . . . .
H105 H 0.710262 0.452442 0.451462 0.045 Uiso 1 1 calc R U . . .
C106 C 0.6070(2) 0.36788(12) 0.48524(8) 0.0332(4) Uani 1 1 d . . . . .
H106 H 0.688466 0.359140 0.503436 0.040 Uiso 1 1 calc R U . . .
C111 C 0.2933(2) 0.13000(12) 0.43376(8) 0.0317(4) Uani 1 1 d . . . . .
C112 C 0.1576(2) 0.14849(12) 0.44331(8) 0.0329(4) Uani 1 1 d . . . . .
C113 C 0.0419(2) 0.10033(13) 0.40488(8) 0.0382(5) Uani 1 1 d . . . . .
H113 H -0.048583 0.112487 0.410990 0.046 Uiso 1 1 calc R U . . .
C114 C 0.0579(3) 0.03587(14) 0.35855(9) 0.0451(5) Uani 1 1 d . . . . .
H114 H -0.021000 0.003755 0.333341 0.054 Uiso 1 1 calc R U . . .
C115 C 0.1890(3) 0.01862(14) 0.34927(9) 0.0477(6) Uani 1 1 d . . . . .
H115 H 0.200351 -0.025210 0.317315 0.057 Uiso 1 1 calc R U . . .
C116 C 0.3044(2) 0.06460(13) 0.38612(8) 0.0408(5) Uani 1 1 d . . . . .
H116 H 0.393764 0.051392 0.378865 0.049 Uiso 1 1 calc R U . . .
C121 C 0.27092(18) 0.35373(12) 0.58713(7) 0.0278(4) Uani 1 1 d . . . . .
C122 C 0.14332(19) 0.31008(12) 0.55298(7) 0.0298(4) Uani 1 1 d . . . . .
C123 C 0.0203(2) 0.34275(13) 0.56619(8) 0.0357(4) Uani 1 1 d . . . . .
H123 H -0.065554 0.313957 0.544395 0.043 Uiso 1 1 calc R U . . .
C124 C 0.0213(2) 0.41543(14) 0.60992(9) 0.0421(5) Uani 1 1 d . . . . .
H124 H -0.062275 0.436895 0.617250 0.050 Uiso 1 1 calc R U . . .
C125 C 0.1448(2) 0.45642(13) 0.64275(9) 0.0404(5) Uani 1 1 d . . . . .
H125 H 0.146165 0.506092 0.672943 0.048 Uiso 1 1 calc R U . . .
C126 C 0.2670(2) 0.42526(12) 0.63179(8) 0.0328(4) Uani 1 1 d . . . . .
H126 H 0.350549 0.453445 0.655379 0.039 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C1 1.958(2) . ?
Al1 C31 1.9891(17) . ?
Al1 C21 2.1123(18) . ?
Al1 C18 2.1320(18) . ?
Al1 Al2 2.6718(7) . ?
Al2 C2 1.9627(17) . ?
Al2 C41 1.9936(18) . ?
Al2 C18 2.1074(18) . ?
Al2 C21 2.1361(18) . ?
Al3 C3 1.952(2) . ?
Al3 C17 1.9789(18) . ?
Al3 C32 2.1152(18) . ?
Al3 C42 2.1346(18) . ?
Al3 Al4 2.6598(7) . ?
Al4 C4 1.9543(19) . ?
Al4 C22 1.9803(18) . ?
Al4 C42 2.0999(18) . ?
Al4 C32 2.1255(18) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C13 C14 1.382(3) . ?
C13 C17 1.398(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.384(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(3) . ?
C15 H15 0.9500 . ?
C16 C18 1.410(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.434(2) . ?
C21 C26 1.415(2) . ?
C21 C22 1.430(2) . ?
C22 C23 1.396(2) . ?
C23 C24 1.389(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.385(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C36 1.394(2) . ?
C31 C32 1.428(2) . ?
C32 C33 1.413(2) . ?
C33 C34 1.385(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.378(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.394(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C46 1.398(2) . ?
C41 C42 1.434(2) . ?
C42 C43 1.413(3) . ?
C43 C44 1.381(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.381(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.391(3) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
Al5 C5 1.960(2) . ?
Al5 C71 1.9861(18) . ?
Al5 C61 2.1265(17) . ?
Al5 C51 2.1285(18) . ?
Al5 Al6 2.6640(7) . ?
Al6 C6 1.947(2) . ?
Al6 C81 1.9803(19) . ?
Al6 C61 2.1204(18) . ?
Al6 C51 2.1307(18) . ?
Al7 C7 1.955(2) . ?
Al7 C52 1.9896(17) . ?
Al7 C72 2.1187(18) . ?
Al7 C82 2.1203(18) . ?
Al7 Al8 2.6588(7) . ?
Al8 C8 1.9519(18) . ?
Al8 C62 1.9840(19) . ?
Al8 C72 2.1213(18) . ?
Al8 C82 2.1368(18) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C51 C56 1.414(2) . ?
C51 C52 1.433(2) . ?
C52 C53 1.397(2) . ?
C53 C54 1.392(3) . ?
C53 H53 0.9500 . ?
C54 C55 1.380(3) . ?
C54 H54 0.9500 . ?
C55 C56 1.384(3) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C61 C66 1.411(2) . ?
C61 C62 1.432(2) . ?
C62 C63 1.398(2) . ?
C63 C64 1.390(3) . ?
C63 H63 0.9500 . ?
C64 C65 1.384(3) . ?
C64 H64 0.9500 . ?
C65 C66 1.384(3) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C71 C76 1.402(2) . ?
C71 C72 1.427(2) . ?
C72 C73 1.415(2) . ?
C73 C74 1.383(3) . ?
C73 H73 0.9500 . ?
C74 C75 1.384(3) . ?
C74 H74 0.9500 . ?
C75 C76 1.390(3) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
C81 C86 1.397(3) . ?
C81 C82 1.429(2) . ?
C82 C83 1.417(2) . ?
C83 C84 1.384(3) . ?
C83 H83 0.9500 . ?
C84 C85 1.380(3) . ?
C84 H84 0.9500 . ?
C85 C86 1.384(3) . ?
C85 H85 0.9500 . ?
C86 H86 0.9500 . ?
Al9 C9 1.949(2) . ?
Al9 C111 1.981(2) . ?
Al9 C91 2.114(2) . ?
Al9 C101 2.139(2) . ?
Al9 Al10 2.6592(8) . ?
Al10 C10 1.957(2) . ?
Al10 C121 1.9846(19) . ?
Al10 C101 2.1209(18) . ?
Al10 C91 2.126(2) . ?
Al11 C11 1.964(2) . ?
Al11 C92 1.992(2) . ?
Al11 C112 2.1241(19) . ?
Al11 C122 2.138(2) . ?
Al11 Al12 2.6786(8) . ?
Al12 C12 1.955(2) . ?
Al12 C102 1.9886(19) . ?
Al12 C112 2.120(2) . ?
Al12 C122 2.1235(19) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C91 C96 1.413(3) . ?
C91 C92 1.429(3) . ?
C92 C93 1.400(3) . ?
C93 C94 1.394(3) . ?
C93 H93 0.9500 . ?
C94 C95 1.379(3) . ?
C94 H94 0.9500 . ?
C95 C96 1.378(3) . ?
C95 H95 0.9500 . ?
C96 H96 0.9500 . ?
C101 C106 1.412(2) . ?
C101 C102 1.427(3) . ?
C102 C103 1.402(3) . ?
C103 C104 1.397(3) . ?
C103 H103 0.9500 . ?
C104 C105 1.376(3) . ?
C104 H104 0.9500 . ?
C105 C106 1.386(3) . ?
C105 H105 0.9500 . ?
C106 H106 0.9500 . ?
C111 C116 1.401(3) . ?
C111 C112 1.428(3) . ?
C112 C113 1.415(3) . ?
C113 C114 1.384(3) . ?
C113 H113 0.9500 . ?
C114 C115 1.376(3) . ?
C114 H114 0.9500 . ?
C115 C116 1.386(3) . ?
C115 H115 0.9500 . ?
C116 H116 0.9500 . ?
C121 C126 1.396(3) . ?
C121 C122 1.433(3) . ?
C122 C123 1.416(3) . ?
C123 C124 1.385(3) . ?
C123 H123 0.9500 . ?
C124 C125 1.381(3) . ?
C124 H124 0.9500 . ?
C125 C126 1.388(3) . ?
C125 H125 0.9500 . ?
C126 H126 0.9500 . ?

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
C1 Al1 C31 116.95(9) . . ?
C1 Al1 C21 111.93(9) . . ?
C31 Al1 C21 106.51(7) . . ?
C1 Al1 C18 112.30(8) . . ?
C31 Al1 C18 106.06(7) . . ?
C21 Al1 C18 101.80(7) . . ?
C1 Al1 Al2 123.42(7) . . ?
C31 Al1 Al2 119.62(6) . . ?
C21 Al1 Al2 51.43(5) . . ?
C18 Al1 Al2 50.52(5) . . ?
C2 Al2 C41 120.08(8) . . ?
C2 Al2 C18 112.20(8) . . ?
C41 Al2 C18 105.44(7) . . ?
C2 Al2 C21 109.65(7) . . ?
C41 Al2 C21 105.95(7) . . ?
C18 Al2 C21 101.83(7) . . ?
C2 Al2 Al1 121.26(7) . . ?
C41 Al2 Al1 118.63(5) . . ?
C18 Al2 Al1 51.34(5) . . ?
C21 Al2 Al1 50.64(5) . . ?
C3 Al3 C17 118.16(9) . . ?
C3 Al3 C32 114.59(8) . . ?
C17 Al3 C32 104.09(7) . . ?
C3 Al3 C42 108.98(9) . . ?
C17 Al3 C42 107.91(7) . . ?
C32 Al3 C42 101.71(7) . . ?
C3 Al3 Al4 122.93(7) . . ?
C17 Al3 Al4 118.90(5) . . ?
C32 Al3 Al4 51.33(5) . . ?
C42 Al3 Al4 50.51(5) . . ?
C4 Al4 C22 118.13(9) . . ?
C4 Al4 C42 112.23(9) . . ?
C22 Al4 C42 105.83(7) . . ?
C4 Al4 C32 110.55(8) . . ?
C22 Al4 C32 106.27(7) . . ?
C42 Al4 C32 102.52(7) . . ?
C4 Al4 Al3 122.58(7) . . ?
C22 Al4 Al3 119.28(5) . . ?
C42 Al4 Al3 51.67(5) . . ?
C32 Al4 Al3 50.98(5) . . ?
Al1 C1 H1A 109.5 . . ?
Al1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Al1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Al2 C2 H2A 109.5 . . ?
Al2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Al2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Al3 C3 H3A 109.5 . . ?
Al3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Al3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Al4 C4 H4A 109.5 . . ?
Al4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Al4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C14 C13 C17 121.95(17) . . ?
C14 C13 H13 119.0 . . ?
C17 C13 H13 119.0 . . ?
C13 C14 C15 120.74(17) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C14 C15 C16 119.02(18) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
C15 C16 C18 121.74(18) . . ?
C15 C16 H16 119.1 . . ?
C18 C16 H16 119.1 . . ?
C13 C17 C18 117.82(16) . . ?
C13 C17 Al3 118.09(13) . . ?
C18 C17 Al3 124.05(12) . . ?
C16 C18 C17 118.70(16) . . ?
C16 C18 Al2 116.19(12) . . ?
C17 C18 Al2 115.00(13) . . ?
C16 C18 Al1 111.99(13) . . ?
C17 C18 Al1 109.43(11) . . ?
Al2 C18 Al1 78.13(6) . . ?
C26 C21 C22 118.44(15) . . ?
C26 C21 Al1 114.65(13) . . ?
C22 C21 Al1 110.37(11) . . ?
C26 C21 Al2 113.68(12) . . ?
C22 C21 Al2 115.02(12) . . ?
Al1 C21 Al2 77.93(6) . . ?
C23 C22 C21 118.07(15) . . ?
C23 C22 Al4 118.33(13) . . ?
C21 C22 Al4 123.60(12) . . ?
C24 C23 C22 122.01(17) . . ?
C24 C23 H23 119.0 . . ?
C22 C23 H23 119.0 . . ?
C25 C24 C23 120.43(16) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 119.07(16) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
C25 C26 C21 121.97(17) . . ?
C25 C26 H26 119.0 . . ?
C21 C26 H26 119.0 . . ?
C36 C31 C32 118.25(15) . . ?
C36 C31 Al1 117.08(13) . . ?
C32 C31 Al1 124.66(13) . . ?
C33 C32 C31 118.37(16) . . ?
C33 C32 Al3 116.23(13) . . ?
C31 C32 Al3 112.48(12) . . ?
C33 C32 Al4 114.98(13) . . ?
C31 C32 Al4 110.22(12) . . ?
Al3 C32 Al4 77.69(6) . . ?
C34 C33 C32 122.02(18) . . ?
C34 C33 H33 119.0 . . ?
C32 C33 H33 119.0 . . ?
C35 C34 C33 119.08(17) . . ?
C35 C34 H34 120.5 . . ?
C33 C34 H34 120.5 . . ?
C34 C35 C36 120.57(18) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C31 C36 C35 121.70(18) . . ?
C31 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
C46 C41 C42 117.43(16) . . ?
C46 C41 Al2 120.38(13) . . ?
C42 C41 Al2 122.19(13) . . ?
C43 C42 C41 118.76(16) . . ?
C43 C42 Al4 112.86(13) . . ?
C41 C42 Al4 116.86(12) . . ?
C43 C42 Al3 112.07(13) . . ?
C41 C42 Al3 111.36(12) . . ?
Al4 C42 Al3 77.82(6) . . ?
C44 C43 C42 122.22(17) . . ?
C44 C43 H43 118.9 . . ?
C42 C43 H43 118.9 . . ?
C45 C44 C43 118.71(19) . . ?
C45 C44 H44 120.6 . . ?
C43 C44 H44 120.6 . . ?
C44 C45 C46 120.89(18) . . ?
C44 C45 H45 119.6 . . ?
C46 C45 H45 119.6 . . ?
C45 C46 C41 121.98(17) . . ?
C45 C46 H46 119.0 . . ?
C41 C46 H46 119.0 . . ?
C5 Al5 C71 116.84(9) . . ?
C5 Al5 C61 109.78(8) . . ?
C71 Al5 C61 106.78(7) . . ?
C5 Al5 C51 115.22(8) . . ?
C71 Al5 C51 104.72(7) . . ?
C61 Al5 C51 102.20(7) . . ?
C5 Al5 Al6 124.05(7) . . ?
C71 Al5 Al6 119.06(6) . . ?
C61 Al5 Al6 51.05(5) . . ?
C51 Al5 Al6 51.32(5) . . ?
C6 Al6 C81 117.85(9) . . ?
C6 Al6 C61 112.32(8) . . ?
C81 Al6 C61 104.80(7) . . ?
C6 Al6 C51 111.10(8) . . ?
C81 Al6 C51 107.12(7) . . ?
C61 Al6 C51 102.33(7) . . ?
C6 Al6 Al5 122.69(7) . . ?
C81 Al6 Al5 119.46(6) . . ?
C61 Al6 Al5 51.25(5) . . ?
C51 Al6 Al5 51.25(5) . . ?
C7 Al7 C52 119.99(8) . . ?
C7 Al7 C72 111.06(8) . . ?
C52 Al7 C72 106.48(7) . . ?
C7 Al7 C82 110.20(8) . . ?
C52 Al7 C82 104.91(7) . . ?
C72 Al7 C82 102.66(7) . . ?
C7 Al7 Al8 120.77(6) . . ?
C52 Al7 Al8 119.22(6) . . ?
C72 Al7 Al8 51.21(5) . . ?
C82 Al7 Al8 51.63(5) . . ?
C8 Al8 C62 119.44(8) . . ?
C8 Al8 C72 110.25(8) . . ?
C62 Al8 C72 107.33(7) . . ?
C8 Al8 C82 111.29(8) . . ?
C62 Al8 C82 105.00(7) . . ?
C72 Al8 C82 102.02(7) . . ?
C8 Al8 Al7 120.79(7) . . ?
C62 Al8 Al7 119.77(5) . . ?
C72 Al8 Al7 51.12(5) . . ?
C82 Al8 Al7 51.07(5) . . ?
Al5 C5 H5A 109.5 . . ?
Al5 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Al5 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Al6 C6 H6A 109.5 . . ?
Al6 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Al6 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Al7 C7 H7A 109.5 . . ?
Al7 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Al7 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Al8 C8 H8A 109.5 . . ?
Al8 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Al8 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C56 C51 C52 118.18(16) . . ?
C56 C51 Al5 116.57(13) . . ?
C52 C51 Al5 114.66(12) . . ?
C56 C51 Al6 111.57(12) . . ?
C52 C51 Al6 111.23(12) . . ?
Al5 C51 Al6 77.43(6) . . ?
C53 C52 C51 118.12(15) . . ?
C53 C52 Al7 118.51(13) . . ?
C51 C52 Al7 123.33(12) . . ?
C54 C53 C52 122.16(17) . . ?
C54 C53 H53 118.9 . . ?
C52 C53 H53 118.9 . . ?
C55 C54 C53 119.92(17) . . ?
C55 C54 H54 120.0 . . ?
C53 C54 H54 120.0 . . ?
C54 C55 C56 119.68(17) . . ?
C54 C55 H55 120.2 . . ?
C56 C55 H55 120.2 . . ?
C55 C56 C51 121.93(17) . . ?
C55 C56 H56 119.0 . . ?
C51 C56 H56 119.0 . . ?
C66 C61 C62 118.85(15) . . ?
C66 C61 Al6 111.46(12) . . ?
C62 C61 Al6 112.26(12) . . ?
C66 C61 Al5 116.25(12) . . ?
C62 C61 Al5 113.16(12) . . ?
Al6 C61 Al5 77.70(6) . . ?
C63 C62 C61 117.67(16) . . ?
C63 C62 Al8 118.91(13) . . ?
C61 C62 Al8 123.39(12) . . ?
C64 C63 C62 121.97(17) . . ?
C64 C63 H63 119.0 . . ?
C62 C63 H63 119.0 . . ?
C65 C64 C63 120.60(17) . . ?
C65 C64 H64 119.7 . . ?
C63 C64 H64 119.7 . . ?
C66 C65 C64 118.98(18) . . ?
C66 C65 H65 120.5 . . ?
C64 C65 H65 120.5 . . ?
C65 C66 C61 121.92(17) . . ?
C65 C66 H66 119.0 . . ?
C61 C66 H66 119.0 . . ?
C76 C71 C72 117.99(16) . . ?
C76 C71 Al5 118.27(14) . . ?
C72 C71 Al5 123.74(12) . . ?
C73 C72 C71 118.63(16) . . ?
C73 C72 Al7 114.60(13) . . ?
C71 C72 Al7 112.97(12) . . ?
C73 C72 Al8 113.33(13) . . ?
C71 C72 Al8 112.78(12) . . ?
Al7 C72 Al8 77.67(6) . . ?
C74 C73 C72 121.89(18) . . ?
C74 C73 H73 119.1 . . ?
C72 C73 H73 119.1 . . ?
C73 C74 C75 119.22(18) . . ?
C73 C74 H74 120.4 . . ?
C75 C74 H74 120.4 . . ?
C74 C75 C76 120.42(18) . . ?
C74 C75 H75 119.8 . . ?
C76 C75 H75 119.8 . . ?
C75 C76 C71 121.85(18) . . ?
C75 C76 H76 119.1 . . ?
C71 C76 H76 119.1 . . ?
C86 C81 C82 118.30(17) . . ?
C86 C81 Al6 117.95(14) . . ?
C82 C81 Al6 123.74(12) . . ?
C83 C82 C81 118.48(16) . . ?
C83 C82 Al7 114.82(13) . . ?
C81 C82 Al7 114.06(11) . . ?
C83 C82 Al8 113.84(12) . . ?
C81 C82 Al8 111.35(12) . . ?
Al7 C82 Al8 77.30(6) . . ?
C84 C83 C82 121.35(19) . . ?
C84 C83 H83 119.3 . . ?
C82 C83 H83 119.3 . . ?
C85 C84 C83 119.55(18) . . ?
C85 C84 H84 120.2 . . ?
C83 C84 H84 120.2 . . ?
C84 C85 C86 120.60(18) . . ?
C84 C85 H85 119.7 . . ?
C86 C85 H85 119.7 . . ?
C85 C86 C81 121.68(19) . . ?
C85 C86 H86 119.2 . . ?
C81 C86 H86 119.2 . . ?
C9 Al9 C111 118.05(10) . . ?
C9 Al9 C91 112.64(9) . . ?
C111 Al9 C91 106.44(8) . . ?
C9 Al9 C101 110.05(9) . . ?
C111 Al9 C101 106.00(8) . . ?
C91 Al9 C101 102.31(7) . . ?
C9 Al9 Al10 122.39(8) . . ?
C111 Al9 Al10 119.52(6) . . ?
C91 Al9 Al10 51.37(5) . . ?
C101 Al9 Al10 51.07(5) . . ?
C10 Al10 C121 119.61(9) . . ?
C10 Al10 C101 110.52(8) . . ?
C121 Al10 C101 105.06(8) . . ?
C10 Al10 C91 110.91(9) . . ?
C121 Al10 C91 106.75(8) . . ?
C101 Al10 C91 102.51(8) . . ?
C10 Al10 Al9 121.32(7) . . ?
C121 Al10 Al9 119.05(6) . . ?
C101 Al10 Al9 51.68(5) . . ?
C91 Al10 Al9 50.96(5) . . ?
C11 Al11 C92 116.70(9) . . ?
C11 Al11 C112 111.10(9) . . ?
C92 Al11 C112 107.03(8) . . ?
C11 Al11 C122 114.15(9) . . ?
C92 Al11 C122 105.02(8) . . ?
C112 Al11 C122 101.49(8) . . ?
C11 Al11 Al12 124.31(7) . . ?
C92 Al11 Al12 118.99(6) . . ?
C112 Al11 Al12 50.81(6) . . ?
C122 Al11 Al12 50.82(5) . . ?
C12 Al12 C102 117.97(9) . . ?
C12 Al12 C112 111.05(10) . . ?
C102 Al12 C112 106.89(8) . . ?
C12 Al12 C122 112.06(9) . . ?
C102 Al12 C122 105.44(7) . . ?
C112 Al12 C122 102.08(8) . . ?
C12 Al12 Al11 122.59(8) . . ?
C102 Al12 Al11 119.44(6) . . ?
C112 Al12 Al11 50.93(5) . . ?
C122 Al12 Al11 51.29(5) . . ?
Al9 C9 H9A 109.5 . . ?
Al9 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Al9 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Al10 C10 H10A 109.5 . . ?
Al10 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Al10 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Al11 C11 H11A 109.5 . . ?
Al11 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Al11 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Al12 C12 H12A 109.5 . . ?
Al12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Al12 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C96 C91 C92 118.73(18) . . ?
C96 C91 Al9 115.75(14) . . ?
C92 C91 Al9 113.77(13) . . ?
C96 C91 Al10 112.09(14) . . ?
C92 C91 Al10 111.71(14) . . ?
Al9 C91 Al10 77.67(7) . . ?
C93 C92 C91 117.71(19) . . ?
C93 C92 Al11 118.76(15) . . ?
C91 C92 Al11 123.53(14) . . ?
C94 C93 C92 121.8(2) . . ?
C94 C93 H93 119.1 . . ?
C92 C93 H93 119.1 . . ?
C95 C94 C93 120.5(2) . . ?
C95 C94 H94 119.8 . . ?
C93 C94 H94 119.8 . . ?
C96 C95 C94 119.2(2) . . ?
C96 C95 H95 120.4 . . ?
C94 C95 H95 120.4 . . ?
C95 C96 C91 122.0(2) . . ?
C95 C96 H96 119.0 . . ?
C91 C96 H96 119.0 . . ?
C106 C101 C102 118.70(17) . . ?
C106 C101 Al10 113.39(13) . . ?
C102 C101 Al10 114.04(12) . . ?
C106 C101 Al9 114.91(14) . . ?
C102 C101 Al9 111.54(12) . . ?
Al10 C101 Al9 77.25(7) . . ?
C103 C102 C101 118.00(16) . . ?
C103 C102 Al12 118.58(14) . . ?
C101 C102 Al12 123.42(13) . . ?
C104 C103 C102 121.58(19) . . ?
C104 C103 H103 119.2 . . ?
C102 C103 H103 119.2 . . ?
C105 C104 C103 120.55(19) . . ?
C105 C104 H104 119.7 . . ?
C103 C104 H104 119.7 . . ?
C104 C105 C106 119.23(18) . . ?
C104 C105 H105 120.4 . . ?
C106 C105 H105 120.4 . . ?
C105 C106 C101 121.94(19) . . ?
C105 C106 H106 119.0 . . ?
C101 C106 H106 119.0 . . ?
C116 C111 C112 117.59(18) . . ?
C116 C111 Al9 117.99(16) . . ?
C112 C111 Al9 124.41(14) . . ?
C113 C112 C111 119.04(18) . . ?
C113 C112 Al12 113.67(15) . . ?
C111 C112 Al12 110.98(13) . . ?
C113 C112 Al11 115.47(14) . . ?
C111 C112 Al11 112.46(13) . . ?
Al12 C112 Al11 78.26(7) . . ?
C114 C113 C112 121.3(2) . . ?
C114 C113 H113 119.4 . . ?
C112 C113 H113 119.4 . . ?
C115 C114 C113 119.5(2) . . ?
C115 C114 H114 120.2 . . ?
C113 C114 H114 120.2 . . ?
C114 C115 C116 120.6(2) . . ?
C114 C115 H115 119.7 . . ?
C116 C115 H115 119.7 . . ?
C115 C116 C111 121.9(2) . . ?
C115 C116 H116 119.0 . . ?
C111 C116 H116 119.0 . . ?
C126 C121 C122 118.42(17) . . ?
C126 C121 Al10 118.52(14) . . ?
C122 C121 Al10 122.98(13) . . ?
C123 C122 C121 117.90(17) . . ?
C123 C122 Al12 111.17(14) . . ?
C121 C122 Al12 113.44(12) . . ?
C123 C122 Al11 116.63(13) . . ?
C121 C122 Al11 113.22(14) . . ?
Al12 C122 Al11 77.89(7) . . ?
C124 C123 C122 122.00(19) . . ?
C124 C123 H123 119.0 . . ?
C122 C123 H123 119.0 . . ?
C125 C124 C123 119.46(19) . . ?
C125 C124 H124 120.3 . . ?
C123 C124 H124 120.3 . . ?
C124 C125 C126 120.19(19) . . ?
C124 C125 H125 119.9 . . ?
C126 C125 H125 119.9 . . ?
C125 C126 C121 121.98(18) . . ?
C125 C126 H126 119.0 . . ?
C121 C126 H126 119.0 . . ?

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
C17 C13 C14 C15 0.7(3) . . . . ?
C13 C14 C15 C16 -1.2(3) . . . . ?
C14 C15 C16 C18 0.2(3) . . . . ?
C14 C13 C17 C18 0.8(3) . . . . ?
C14 C13 C17 Al3 178.59(15) . . . . ?
C15 C16 C18 C17 1.2(3) . . . . ?
C15 C16 C18 Al2 144.95(16) . . . . ?
C15 C16 C18 Al1 -127.83(17) . . . . ?
C13 C17 C18 C16 -1.7(3) . . . . ?
Al3 C17 C18 C16 -179.36(13) . . . . ?
C13 C17 C18 Al2 -145.86(13) . . . . ?
Al3 C17 C18 Al2 36.51(18) . . . . ?
C13 C17 C18 Al1 128.51(14) . . . . ?
Al3 C17 C18 Al1 -49.13(17) . . . . ?
C26 C21 C22 C23 1.0(3) . . . . ?
Al1 C21 C22 C23 -133.96(14) . . . . ?
Al2 C21 C22 C23 140.21(14) . . . . ?
C26 C21 C22 Al4 -178.03(13) . . . . ?
Al1 C21 C22 Al4 46.97(17) . . . . ?
Al2 C21 C22 Al4 -38.86(18) . . . . ?
C21 C22 C23 C24 -0.4(3) . . . . ?
Al4 C22 C23 C24 178.75(14) . . . . ?
C22 C23 C24 C25 -0.8(3) . . . . ?
C23 C24 C25 C26 1.3(3) . . . . ?
C24 C25 C26 C21 -0.6(3) . . . . ?
C22 C21 C26 C25 -0.6(3) . . . . ?
Al1 C21 C26 C25 132.59(16) . . . . ?
Al2 C21 C26 C25 -140.27(15) . . . . ?
C36 C31 C32 C33 0.1(3) . . . . ?
Al1 C31 C32 C33 179.37(13) . . . . ?
C36 C31 C32 Al3 140.18(14) . . . . ?
Al1 C31 C32 Al3 -40.54(18) . . . . ?
C36 C31 C32 Al4 -135.18(14) . . . . ?
Al1 C31 C32 Al4 44.10(18) . . . . ?
C31 C32 C33 C34 -0.2(3) . . . . ?
Al3 C32 C33 C34 -138.84(16) . . . . ?
Al4 C32 C33 C34 133.03(16) . . . . ?
C32 C33 C34 C35 0.5(3) . . . . ?
C33 C34 C35 C36 -0.7(3) . . . . ?
C32 C31 C36 C35 -0.3(3) . . . . ?
Al1 C31 C36 C35 -179.65(15) . . . . ?
C34 C35 C36 C31 0.7(3) . . . . ?
C46 C41 C42 C43 1.0(3) . . . . ?
Al2 C41 C42 C43 -178.95(14) . . . . ?
C46 C41 C42 Al4 141.80(14) . . . . ?
Al2 C41 C42 Al4 -38.19(18) . . . . ?
C46 C41 C42 Al3 -131.40(14) . . . . ?
Al2 C41 C42 Al3 48.61(16) . . . . ?
C41 C42 C43 C44 -0.2(3) . . . . ?
Al4 C42 C43 C44 -142.48(17) . . . . ?
Al3 C42 C43 C44 131.89(18) . . . . ?
C42 C43 C44 C45 -0.2(3) . . . . ?
C43 C44 C45 C46 -0.2(3) . . . . ?
C44 C45 C46 C41 1.1(3) . . . . ?
C42 C41 C46 C45 -1.5(3) . . . . ?
Al2 C41 C46 C45 178.54(16) . . . . ?
C56 C51 C52 C53 -0.1(2) . . . . ?
Al5 C51 C52 C53 143.45(13) . . . . ?
Al6 C51 C52 C53 -131.06(14) . . . . ?
C56 C51 C52 Al7 177.54(13) . . . . ?
Al5 C51 C52 Al7 -38.91(18) . . . . ?
Al6 C51 C52 Al7 46.59(17) . . . . ?
C51 C52 C53 C54 0.6(3) . . . . ?
Al7 C52 C53 C54 -177.20(14) . . . . ?
C52 C53 C54 C55 -0.6(3) . . . . ?
C53 C54 C55 C56 0.2(3) . . . . ?
C54 C55 C56 C51 0.2(3) . . . . ?
C52 C51 C56 C55 -0.3(3) . . . . ?
Al5 C51 C56 C55 -143.14(16) . . . . ?
Al6 C51 C56 C55 130.52(17) . . . . ?
C66 C61 C62 C63 0.9(2) . . . . ?
Al6 C61 C62 C63 133.53(14) . . . . ?
Al5 C61 C62 C63 -140.79(14) . . . . ?
C66 C61 C62 Al8 -177.25(13) . . . . ?
Al6 C61 C62 Al8 -44.65(17) . . . . ?
Al5 C61 C62 Al8 41.04(17) . . . . ?
C61 C62 C63 C64 -0.9(3) . . . . ?
Al8 C62 C63 C64 177.33(16) . . . . ?
C62 C63 C64 C65 0.0(3) . . . . ?
C63 C64 C65 C66 1.0(3) . . . . ?
C64 C65 C66 C61 -1.0(3) . . . . ?
C62 C61 C66 C65 0.0(3) . . . . ?
Al6 C61 C66 C65 -132.94(16) . . . . ?
Al5 C61 C66 C65 140.58(15) . . . . ?
C76 C71 C72 C73 -1.1(3) . . . . ?
Al5 C71 C72 C73 177.82(13) . . . . ?
C76 C71 C72 Al7 137.16(14) . . . . ?
Al5 C71 C72 Al7 -43.90(18) . . . . ?
C76 C71 C72 Al8 -137.06(14) . . . . ?
Al5 C71 C72 Al8 41.88(17) . . . . ?
C71 C72 C73 C74 0.4(3) . . . . ?
Al7 C72 C73 C74 -137.26(17) . . . . ?
Al8 C72 C73 C74 136.09(17) . . . . ?
C72 C73 C74 C75 0.5(3) . . . . ?
C73 C74 C75 C76 -0.6(3) . . . . ?
C74 C75 C76 C71 -0.2(3) . . . . ?
C72 C71 C76 C75 1.1(3) . . . . ?
Al5 C71 C76 C75 -177.94(15) . . . . ?
C86 C81 C82 C83 -1.5(2) . . . . ?
Al6 C81 C82 C83 179.28(13) . . . . ?
C86 C81 C82 Al7 -141.41(14) . . . . ?
Al6 C81 C82 Al7 39.35(17) . . . . ?
C86 C81 C82 Al8 133.41(15) . . . . ?
Al6 C81 C82 Al8 -45.83(16) . . . . ?
C81 C82 C83 C84 1.6(3) . . . . ?
Al7 C82 C83 C84 141.23(16) . . . . ?
Al8 C82 C83 C84 -132.24(16) . . . . ?
C82 C83 C84 C85 -0.2(3) . . . . ?
C83 C84 C85 C86 -1.4(3) . . . . ?
C84 C85 C86 C81 1.5(3) . . . . ?
C82 C81 C86 C85 0.0(3) . . . . ?
Al6 C81 C86 C85 179.26(15) . . . . ?
C96 C91 C92 C93 -0.7(3) . . . . ?
Al9 C91 C92 C93 140.87(15) . . . . ?
Al10 C91 C92 C93 -133.48(16) . . . . ?
C96 C91 C92 Al11 178.89(14) . . . . ?
Al9 C91 C92 Al11 -39.58(19) . . . . ?
Al10 C91 C92 Al11 46.07(18) . . . . ?
C91 C92 C93 C94 1.7(3) . . . . ?
Al11 C92 C93 C94 -177.90(17) . . . . ?
C92 C93 C94 C95 -1.5(3) . . . . ?
C93 C94 C95 C96 0.2(3) . . . . ?
C94 C95 C96 C91 0.8(3) . . . . ?
C92 C91 C96 C95 -0.5(3) . . . . ?
Al9 C91 C96 C95 -141.33(18) . . . . ?
Al10 C91 C96 C95 132.11(19) . . . . ?
C106 C101 C102 C103 0.3(3) . . . . ?
Al10 C101 C102 C103 138.06(14) . . . . ?
Al9 C101 C102 C103 -136.74(14) . . . . ?
C106 C101 C102 Al12 -178.93(13) . . . . ?
Al10 C101 C102 Al12 -41.22(18) . . . . ?
Al9 C101 C102 Al12 43.98(17) . . . . ?
C101 C102 C103 C104 0.0(3) . . . . ?
Al12 C102 C103 C104 179.28(15) . . . . ?
C102 C103 C104 C105 -0.6(3) . . . . ?
C103 C104 C105 C106 0.9(3) . . . . ?
C104 C105 C106 C101 -0.6(3) . . . . ?
C102 C101 C106 C105 0.0(3) . . . . ?
Al10 C101 C106 C105 -138.02(16) . . . . ?
Al9 C101 C106 C105 135.66(17) . . . . ?
C116 C111 C112 C113 0.3(3) . . . . ?
Al9 C111 C112 C113 179.19(15) . . . . ?
C116 C111 C112 Al12 -134.53(16) . . . . ?
Al9 C111 C112 Al12 44.38(19) . . . . ?
C116 C111 C112 Al11 139.90(16) . . . . ?
Al9 C111 C112 Al11 -41.2(2) . . . . ?
C111 C112 C113 C114 0.2(3) . . . . ?
Al12 C112 C113 C114 133.85(18) . . . . ?
Al11 C112 C113 C114 -138.29(18) . . . . ?
C112 C113 C114 C115 -0.6(3) . . . . ?
C113 C114 C115 C116 0.6(3) . . . . ?
C114 C115 C116 C111 -0.2(3) . . . . ?
C112 C111 C116 C115 -0.3(3) . . . . ?
Al9 C111 C116 C115 -179.26(17) . . . . ?
C126 C121 C122 C123 0.7(3) . . . . ?
Al10 C121 C122 C123 -175.97(14) . . . . ?
C126 C121 C122 Al12 133.17(15) . . . . ?
Al10 C121 C122 Al12 -43.53(19) . . . . ?
C126 C121 C122 Al11 -140.43(15) . . . . ?
Al10 C121 C122 Al11 42.87(18) . . . . ?
C121 C122 C123 C124 1.2(3) . . . . ?
Al12 C122 C123 C124 -132.25(19) . . . . ?
Al11 C122 C123 C124 141.05(18) . . . . ?
C122 C123 C124 C125 -1.8(3) . . . . ?
C123 C124 C125 C126 0.4(3) . . . . ?
C124 C125 C126 C121 1.6(3) . . . . ?
C122 C121 C126 C125 -2.1(3) . . . . ?
Al10 C121 C126 C125 174.73(15) . . . . ?

_refine_diff_density_max         0.453
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.064


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_alpha-2AlBr32_wa3234_av
_database_code_depnum_ccdc_archive 'CCDC 2385633'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT910_alpha-2AlBr32_wa3234_av 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note  
RESPONSE: These reflections are hidden by the beamstop.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 Al4 Br8'
_chemical_formula_sum            'C12 H8 Al4 Br8'
_chemical_formula_weight         899.38

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5249(4)
_cell_length_b                   10.0840(6)
_cell_length_c                   15.0220(7)
_cell_angle_alpha                80.500(4)
_cell_angle_beta                 80.878(4)
_cell_angle_gamma                65.121(5)
_cell_volume                     1149.72(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6698
_cell_measurement_theta_min      3.8070
_cell_measurement_theta_max      25.9110

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.598
_exptl_crystal_F_000             824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    14.101
_shelx_estimated_absorpt_T_min   0.121
_shelx_estimated_absorpt_T_max   0.140
_exptl_absorpt_correction_T_min  0.03151
_exptl_absorpt_correction_T_max  0.05141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            16804
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_av_R_equivalents  0.1061
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.471
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4533
_reflns_number_gt                4003
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  'IUCr PublCIF online service'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0834P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.0051(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4533
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0590
_refine_ls_wR_factor_ref         0.1552
_refine_ls_wR_factor_gt          0.1503
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Al1 Al -0.0119(3) 0.9013(2) 0.41838(14) 0.0189(4) Uani 1 1 d . . . . .
Al2 Al 0.2406(3) 0.7246(2) 0.56790(15) 0.0195(4) Uani 1 1 d . . . . .
Br1 Br -0.01485(11) 0.74151(8) 0.33155(5) 0.0290(2) Uani 1 1 d . . . . .
Br2 Br -0.08325(10) 1.12704(7) 0.31062(5) 0.0242(2) Uani 1 1 d . . . . .
Br3 Br 0.52171(10) 0.61483(8) 0.59844(6) 0.0295(2) Uani 1 1 d . . . . .
Br4 Br 0.10572(10) 0.57410(8) 0.56885(5) 0.0278(2) Uani 1 1 d . . . . .
C1 C 0.2239(9) 0.8747(7) 0.4560(5) 0.0181(14) Uani 1 1 d . . . . .
C2 C 0.1971(9) 1.0142(7) 0.4841(5) 0.0180(14) Uani 1 1 d . . . . .
C3 C 0.3025(9) 1.0842(8) 0.4386(5) 0.0240(15) Uani 1 1 d . . . . .
H3 H 0.288499 1.174922 0.456444 0.029 Uiso 1 1 calc R U . . .
C4 C 0.4263(11) 1.0252(9) 0.3685(6) 0.0317(18) Uani 1 1 d . . . . .
H4 H 0.494761 1.076622 0.339094 0.038 Uiso 1 1 calc R U . . .
C5 C 0.4532(10) 0.8928(9) 0.3401(6) 0.0287(17) Uani 1 1 d . . . . .
H5 H 0.538367 0.854375 0.291267 0.034 Uiso 1 1 calc R U . . .
C6 C 0.3547(9) 0.8173(8) 0.3835(5) 0.0190(14) Uani 1 1 d . . . . .
H6 H 0.374337 0.725559 0.364850 0.023 Uiso 1 1 calc R U . . .
Al1A Al 0.6219(3) 0.5176(2) 0.07274(15) 0.0185(4) Uani 1 1 d . . . . .
Al2A Al 0.6770(3) 0.1823(2) 0.00855(15) 0.0194(5) Uani 1 1 d . . . . .
Br1A Br 0.72779(10) 0.57893(9) 0.18062(6) 0.0320(2) Uani 1 1 d . . . . .
Br2A Br 0.86745(9) 0.30274(8) 0.01532(6) 0.0250(2) Uani 1 1 d . . . . .
Br3A Br 0.72393(11) 0.11389(10) -0.13241(6) 0.0337(2) Uani 1 1 d . . . . .
Br4A Br 0.74120(11) -0.00974(9) 0.11865(6) 0.0371(3) Uani 1 1 d . . . . .
C1A C 0.5605(9) 0.6613(7) -0.0441(5) 0.0213(15) Uani 1 1 d . . . . .
C2A C 0.5501(8) 0.5700(7) -0.1048(5) 0.0192(14) Uani 1 1 d . . . . .
C3A C 0.6658(10) 0.5445(9) -0.1834(5) 0.0262(16) Uani 1 1 d . . . . .
H3A H 0.661613 0.483317 -0.223961 0.031 Uiso 1 1 calc R U . . .
C4A C 0.7872(11) 0.6068(10) -0.2037(6) 0.0353(19) Uani 1 1 d . . . . .
H4A H 0.862858 0.588994 -0.258229 0.042 Uiso 1 1 calc R U . . .
C5A C 0.7986(10) 0.6929(10) -0.1462(6) 0.0322(18) Uani 1 1 d . . . . .
H5A H 0.883013 0.733519 -0.160715 0.039 Uiso 1 1 calc R U . . .
C6A C 0.6879(9) 0.7221(8) -0.0665(5) 0.0244(16) Uani 1 1 d . . . . .
H6A H 0.696919 0.782404 -0.026998 0.029 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C2 1.978(7) 2_576 ?
Al1 C1 2.071(7) . ?
Al1 Br1 2.245(2) . ?
Al1 Br2 2.470(2) . ?
Al2 C1 2.048(7) . ?
Al2 Br4 2.254(2) . ?
Al2 Br3 2.265(2) . ?
Al2 Br2 2.409(2) 2_576 ?
C1 C6 1.430(9) . ?
C1 C2 1.450(9) . ?
C2 C3 1.397(9) . ?
C3 C4 1.379(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.383(10) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
Al1A C2A 1.972(7) 2_665 ?
Al1A C1A 2.066(8) . ?
Al1A Br1A 2.256(2) . ?
Al1A Br2A 2.460(2) . ?
Al2A C1A 2.030(7) 2_665 ?
Al2A Br3A 2.258(2) . ?
Al2A Br4A 2.263(2) . ?
Al2A Br2A 2.424(2) . ?
C1A C6A 1.429(9) . ?
C1A C2A 1.435(10) . ?
C2A C3A 1.396(10) . ?
C3A C4A 1.394(11) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.361(12) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.391(11) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?

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
C2 Al1 C1 109.0(3) 2_576 . ?
C2 Al1 Br1 123.3(2) 2_576 . ?
C1 Al1 Br1 118.6(2) . . ?
C2 Al1 Br2 97.2(2) 2_576 . ?
C1 Al1 Br2 101.73(19) . . ?
Br1 Al1 Br2 101.23(9) . . ?
C1 Al2 Br4 116.6(2) . . ?
C1 Al2 Br3 107.9(2) . . ?
Br4 Al2 Br3 116.26(9) . . ?
C1 Al2 Br2 104.1(2) . 2_576 ?
Br4 Al2 Br2 104.49(8) . 2_576 ?
Br3 Al2 Br2 106.23(9) . 2_576 ?
Al2 Br2 Al1 90.51(7) 2_576 . ?
C6 C1 C2 118.6(6) . . ?
C6 C1 Al2 113.3(5) . . ?
C2 C1 Al2 109.4(5) . . ?
C6 C1 Al1 108.0(5) . . ?
C2 C1 Al1 106.3(5) . . ?
Al2 C1 Al1 99.2(3) . . ?
C3 C2 C1 117.6(6) . . ?
C3 C2 Al1 123.1(5) . 2_576 ?
C1 C2 Al1 119.3(5) . 2_576 ?
C4 C3 C2 121.8(7) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 121.6(7) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C6 C5 C4 119.2(7) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C1 121.2(6) . . ?
C5 C6 H6 119.4 . . ?
C1 C6 H6 119.4 . . ?
C2A Al1A C1A 108.9(3) 2_665 . ?
C2A Al1A Br1A 121.2(2) 2_665 . ?
C1A Al1A Br1A 117.9(2) . . ?
C2A Al1A Br2A 98.3(2) 2_665 . ?
C1A Al1A Br2A 102.0(2) . . ?
Br1A Al1A Br2A 104.40(8) . . ?
C1A Al2A Br3A 116.9(2) 2_665 . ?
C1A Al2A Br4A 108.9(2) 2_665 . ?
Br3A Al2A Br4A 113.32(9) . . ?
C1A Al2A Br2A 102.1(2) 2_665 . ?
Br3A Al2A Br2A 107.49(9) . . ?
Br4A Al2A Br2A 107.01(9) . . ?
Al2A Br2A Al1A 91.24(7) . . ?
C6A C1A C2A 118.8(7) . . ?
C6A C1A Al2A 111.2(5) . 2_665 ?
C2A C1A Al2A 111.5(5) . 2_665 ?
C6A C1A Al1A 107.9(5) . . ?
C2A C1A Al1A 101.9(5) . . ?
Al2A C1A Al1A 104.0(3) 2_665 . ?
C3A C2A C1A 118.2(6) . . ?
C3A C2A Al1A 122.8(6) . 2_665 ?
C1A C2A Al1A 119.0(5) . 2_665 ?
C4A C3A C2A 121.5(7) . . ?
C4A C3A H3A 119.3 . . ?
C2A C3A H3A 119.3 . . ?
C5A C4A C3A 120.7(8) . . ?
C5A C4A H4A 119.7 . . ?
C3A C4A H4A 119.7 . . ?
C4A C5A C6A 120.7(7) . . ?
C4A C5A H5A 119.6 . . ?
C6A C5A H5A 119.6 . . ?
C5A C6A C1A 120.0(7) . . ?
C5A C6A H6A 120.0 . . ?
C1A C6A H6A 120.0 . . ?

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
C6 C1 C2 C3 -0.4(10) . . . . ?
Al2 C1 C2 C3 131.6(6) . . . . ?
Al1 C1 C2 C3 -122.1(6) . . . . ?
C6 C1 C2 Al1 178.1(5) . . . 2_576 ?
Al2 C1 C2 Al1 -49.9(6) . . . 2_576 ?
Al1 C1 C2 Al1 56.4(6) . . . 2_576 ?
C1 C2 C3 C4 0.9(11) . . . . ?
Al1 C2 C3 C4 -177.5(6) 2_576 . . . ?
C2 C3 C4 C5 -0.4(13) . . . . ?
C3 C4 C5 C6 -0.6(13) . . . . ?
C4 C5 C6 C1 1.1(12) . . . . ?
C2 C1 C6 C5 -0.6(10) . . . . ?
Al2 C1 C6 C5 -130.9(7) . . . . ?
Al1 C1 C6 C5 120.3(7) . . . . ?
C6A C1A C2A C3A 0.0(10) . . . . ?
Al2A C1A C2A C3A 131.4(6) 2_665 . . . ?
Al1A C1A C2A C3A -118.2(6) . . . . ?
C6A C1A C2A Al1A 178.6(5) . . . 2_665 ?
Al2A C1A C2A Al1A -50.1(6) 2_665 . . 2_665 ?
Al1A C1A C2A Al1A 60.4(5) . . . 2_665 ?
C1A C2A C3A C4A -0.8(11) . . . . ?
Al1A C2A C3A C4A -179.3(6) 2_665 . . . ?
C2A C3A C4A C5A 1.1(13) . . . . ?
C3A C4A C5A C6A -0.8(13) . . . . ?
C4A C5A C6A C1A 0.1(12) . . . . ?
C2A C1A C6A C5A 0.3(11) . . . . ?
Al2A C1A C6A C5A -131.2(7) 2_665 . . . ?
Al1A C1A C6A C5A 115.4(7) . . . . ?

_refine_diff_density_max         1.644
_refine_diff_density_min         -1.575
_refine_diff_density_rms         0.279


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_K1mu-pz_wa3541
_database_code_depnum_ccdc_archive 'CCDC 2385630'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_RINTA01_K1mu-pz_wa3541      
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The crystal scattered weakly, showing also pseudo-merohedry 
twinning. The resulting diffraction data of rather limited quality did
not allow us to refine some fine features as disorder of THF ligands.
;
_vrf_PLAT084_K1mu-pz_wa3541      
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.39 Report
RESPONSE: The crystal scattered weakly, showing also pseudo-merohedry 
twinning. The resulting diffraction data of rather limited quality did
not allow us to refine some fine features as disorder of THF ligands.
;
_vrf_PLAT220_K1mu-pz_wa3541      
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        6.2 Ratio 
RESPONSE: The crystal scattered weakly, showing also pseudo-merohedry 
twinning. The resulting diffraction data of rather limited quality did
not allow us to refine some fine features as disorder of THF ligands.
;
_vrf_PLAT234_K1mu-pz_wa3541      
;
PROBLEM: Large Hirshfeld Difference O3       --C34T     .       0.26 Ang.  
RESPONSE: The crystal scattered weakly, showing also pseudo-merohedry 
twinning. The resulting diffraction data of rather limited quality did
not allow us to refine some fine features as disorder of THF ligands.
;
_vrf_PLAT241_K1mu-pz_wa3541      
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       C33T Check 
RESPONSE: The crystal scattered weakly, showing also pseudo-merohedry 
twinning. The resulting diffraction data of rather limited quality did
not allow us to refine some fine features as disorder of THF ligands.
;
_vrf_PLAT242_K1mu-pz_wa3541      
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         O3 Check 
RESPONSE: The crystal scattered weakly, showing also pseudo-merohedry 
twinning. The resulting diffraction data of rather limited quality did
not allow us to refine some fine features as disorder of THF ligands.
;
_vrf_PLAT340_K1mu-pz_wa3541      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02811 Ang.  
RESPONSE: The crystal scattered weakly, showing also pseudo-merohedry 
twinning. The resulting diffraction data of rather limited quality did
not allow us to refine some fine features as disorder of THF ligands.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H42 Al4 K N4 O, C8 H16 K O2'
_chemical_formula_sum            'C23 H29 Al2 K N2 O1.50'
_chemical_formula_weight         450.54

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9074(12)
_cell_length_b                   12.1287(12)
_cell_length_c                   20.097(2)
_cell_angle_alpha                90.030(9)
_cell_angle_beta                 91.767(9)
_cell_angle_gamma                109.036(9)
_cell_volume                     2512.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2581
_cell_measurement_theta_min      3.1980
_cell_measurement_theta_max      26.7700

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_F_000             952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.299
_shelx_estimated_absorpt_T_min   0.929
_shelx_estimated_absorpt_T_max   0.957
_exptl_absorpt_correction_T_min  0.17122
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5461 346 24301 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.4539 291 24301 nmt -0.9998 -0.0005 -0.0002 -0.0014 -1.0001 0.0001 0.1174
0.0332 1.0044
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by -179.9387° 
around [-0.00 -0.00 1.00] (reciprocal) or [0.06 0.02 1.00] (direct)
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            9521
_diffrn_reflns_av_unetI/netI     0.1372
_diffrn_reflns_av_R_equivalents  0.2042
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.389
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             9521
_reflns_number_gt                4260
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Refined as a 2-component twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1985P)²+3.2515P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9521
_refine_ls_number_parameters     537
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.1567
_refine_ls_R_factor_gt           0.1057
_refine_ls_wR_factor_ref         0.3937
_refine_ls_wR_factor_gt          0.3841
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
K1 K 0.5146(7) 0.7549(5) 0.17665(14) 0.0967(13) Uani 1 1 d . . . . .
K2 K 1.0121(4) 1.2534(4) 0.31511(13) 0.0637(8) Uani 1 1 d . . . . .
Al1 Al 0.1878(4) 0.6382(4) 0.2876(2) 0.0432(11) Uani 1 1 d . . . . .
Al2 Al 0.1440(5) 0.4986(4) 0.1492(2) 0.0461(11) Uani 1 1 d . . . . .
N1 N 0.1882(11) 0.7246(10) 0.2030(6) 0.041(3) Uani 1 1 d . U . . .
N2 N 0.1711(12) 0.6653(11) 0.1444(6) 0.048(3) Uani 1 1 d . . . . .
C1 C 0.2098(16) 0.7433(14) 0.3644(8) 0.057(4) Uani 1 1 d . . . . .
H1A H 0.168217 0.802017 0.354228 0.086 Uiso 1 1 calc R U . . .
H1B H 0.302565 0.782119 0.374189 0.086 Uiso 1 1 calc R U . . .
H1C H 0.169760 0.698306 0.403094 0.086 Uiso 1 1 calc R U . . .
C2 C 0.1206(19) 0.4302(18) 0.0583(10) 0.080(6) Uani 1 1 d . . . . .
H2A H 0.031373 0.377243 0.051798 0.120 Uiso 1 1 calc R U . . .
H2B H 0.181234 0.386723 0.052666 0.120 Uiso 1 1 calc R U . . .
H2C H 0.137520 0.492662 0.025484 0.120 Uiso 1 1 calc R U . . .
C11 C 0.3265(15) 0.5692(13) 0.2648(8) 0.048(4) Uani 1 1 d . . . . .
C12 C 0.3060(14) 0.5093(13) 0.1998(8) 0.046(4) Uani 1 1 d . . . . .
C13 C 0.4027(14) 0.4666(15) 0.1803(11) 0.069(5) Uani 1 1 d . . . . .
H13 H 0.393731 0.426301 0.138940 0.082 Uiso 1 1 calc R U . . .
C14 C 0.5191(14) 0.4828(14) 0.2230(11) 0.062(5) Uani 1 1 d . . . . .
H14 H 0.583164 0.450855 0.209388 0.074 Uiso 1 1 calc R U . . .
C15 C 0.5365(16) 0.5412(15) 0.2802(10) 0.065(5) Uani 1 1 d . . . . .
H15 H 0.613980 0.554142 0.306437 0.077 Uiso 1 1 calc R U . . .
C16 C 0.4399(13) 0.5830(12) 0.3011(9) 0.051(4) Uani 1 1 d . . . . .
H16 H 0.452551 0.623309 0.342626 0.061 Uiso 1 1 calc R U . . .
C21 C -0.0002(13) 0.4494(13) 0.2148(8) 0.043(4) Uani 1 1 d . . . . .
C22 C 0.0205(14) 0.5091(12) 0.2742(7) 0.040(3) Uani 1 1 d . . . . .
C23 C -0.0822(13) 0.4839(11) 0.3181(9) 0.047(4) Uani 1 1 d . . . . .
H23 H -0.069795 0.527629 0.358426 0.057 Uiso 1 1 calc R U . . .
C24 C -0.1992(15) 0.3996(14) 0.3057(8) 0.053(4) Uani 1 1 d . . . . .
H24 H -0.266555 0.385983 0.336692 0.063 Uiso 1 1 calc R U . . .
C25 C -0.2191(15) 0.3325(16) 0.2461(10) 0.062(5) Uani 1 1 d . . . . .
H25 H -0.298256 0.270953 0.237580 0.075 Uiso 1 1 calc R U . . .
C26 C -0.1218(16) 0.3579(13) 0.2007(10) 0.055(5) Uani 1 1 d . . . . .
H26 H -0.134646 0.315076 0.160058 0.066 Uiso 1 1 calc R U . . .
C31 C 0.1914(15) 0.8402(13) 0.1915(8) 0.048(4) Uani 1 1 d . . . . .
H31 H 0.199918 0.899208 0.224113 0.057 Uiso 1 1 calc R U . . .
C32 C 0.1796(15) 0.8505(14) 0.1224(10) 0.053(4) Uani 1 1 d . . . . .
H32 H 0.179233 0.918109 0.098651 0.064 Uiso 1 1 calc R U . . .
C33 C 0.1686(17) 0.7426(15) 0.0959(9) 0.057(5) Uani 1 1 d . . . . .
H33 H 0.160396 0.724611 0.049611 0.069 Uiso 1 1 calc R U . . .
Al3 Al 0.8519(4) 0.8732(4) 0.2869(2) 0.0451(11) Uani 1 1 d . . . . .
Al4 Al 0.8806(4) 1.0129(4) 0.1512(3) 0.0491(12) Uani 1 1 d . . . . .
N4 N 0.8543(11) 0.8436(11) 0.1455(7) 0.044(3) Uani 1 1 d . . . . .
N43 N 0.8445(12) 0.7833(10) 0.2072(6) 0.046(3) Uani 1 1 d . . . . .
C3 C 0.8372(16) 0.7658(14) 0.3633(9) 0.062(4) Uani 1 1 d . . . . .
H3A H 0.761098 0.763087 0.388782 0.094 Uiso 1 1 calc R U . . .
H3B H 0.915453 0.793952 0.392113 0.094 Uiso 1 1 calc R U . . .
H3C H 0.827683 0.687371 0.346618 0.094 Uiso 1 1 calc R U . . .
C4 C 0.8929(19) 1.0757(17) 0.0594(8) 0.070(5) Uani 1 1 d . . . . .
H4A H 0.955698 1.050596 0.034946 0.105 Uiso 1 1 calc R U . . .
H4B H 0.921351 1.161139 0.061457 0.105 Uiso 1 1 calc R U . . .
H4C H 0.807650 1.046441 0.036463 0.105 Uiso 1 1 calc R U . . .
C41 C 0.7064(13) 0.9363(13) 0.2638(8) 0.046(4) Uani 1 1 d . . . . .
C42 C 0.7224(14) 1.0002(13) 0.2030(8) 0.050(4) Uani 1 1 d . . . . .
C43 C 0.6235(14) 1.0450(12) 0.1820(7) 0.044(4) Uani 1 1 d . . . . .
H43 H 0.630971 1.084585 0.140817 0.053 Uiso 1 1 calc R U . . .
C44 C 0.5167(16) 1.0328(15) 0.2195(10) 0.061(5) Uani 1 1 d . . . . .
H44 H 0.452117 1.064980 0.204835 0.073 Uiso 1 1 calc R U . . .
C45 C 0.5046(13) 0.9739(13) 0.2782(10) 0.058(5) Uani 1 1 d . . . . .
H45 H 0.431165 0.966413 0.304335 0.070 Uiso 1 1 calc R U . . .
C46 C 0.5971(15) 0.9242(14) 0.3010(9) 0.060(4) Uani 1 1 d . . . . .
H46 H 0.585435 0.882556 0.341625 0.072 Uiso 1 1 calc R U . . .
C51 C 1.0233(14) 1.0023(15) 0.2737(9) 0.053(4) Uani 1 1 d . . . . .
C52 C 1.0358(14) 1.0642(12) 0.2102(9) 0.045(4) Uani 1 1 d . . . . .
C53 C 1.1541(16) 1.1507(15) 0.2042(11) 0.065(5) Uani 1 1 d . . . . .
H53 H 1.168454 1.193229 0.163918 0.078 Uiso 1 1 calc R U . . .
C54 C 1.2544(16) 1.1806(15) 0.2527(10) 0.061(5) Uani 1 1 d . . . . .
H54 H 1.333256 1.240541 0.243682 0.073 Uiso 1 1 calc R U . . .
C55 C 1.2418(13) 1.1254(12) 0.3129(10) 0.060(5) Uani 1 1 d . . . . .
H55 H 1.310262 1.147877 0.345705 0.072 Uiso 1 1 calc R U . . .
C56 C 1.1265(14) 1.0356(13) 0.3253(8) 0.051(4) Uani 1 1 d . . . . .
H56 H 1.115397 0.996579 0.366823 0.061 Uiso 1 1 calc R U . . .
C61 C 0.8335(13) 0.6763(12) 0.1886(8) 0.042(4) Uani 1 1 d . . . . .
H61 H 0.825972 0.614950 0.219209 0.051 Uiso 1 1 calc R U . . .
C62 C 0.8341(16) 0.6617(14) 0.1216(8) 0.051(4) Uani 1 1 d . . . . .
H62 H 0.825536 0.592014 0.097462 0.061 Uiso 1 1 calc R U . . .
C63 C 0.8498(17) 0.7704(16) 0.0968(8) 0.061(5) Uani 1 1 d . . . . .
H63 H 0.856490 0.789886 0.050953 0.073 Uiso 1 1 calc R U . . .
O1 O 1.1568(13) 1.3437(15) 0.4231(7) 0.096(5) Uani 1 1 d . . . . .
C11T C 1.295(2) 1.375(2) 0.4400(14) 0.108(8) Uani 1 1 d . . . . .
H11A H 1.347239 1.388561 0.399521 0.129 Uiso 1 1 calc R U . . .
H11B H 1.313722 1.312990 0.466598 0.129 Uiso 1 1 calc R U . . .
C12T C 1.321(3) 1.486(3) 0.4806(15) 0.138(11) Uani 1 1 d . . . . .
H12A H 1.382087 1.487041 0.518444 0.165 Uiso 1 1 calc R U . . .
H12B H 1.361957 1.554565 0.452514 0.165 Uiso 1 1 calc R U . . .
C13T C 1.206(3) 1.491(2) 0.5039(15) 0.137(11) Uani 1 1 d . . . . .
H13A H 1.196551 1.567982 0.493413 0.165 Uiso 1 1 calc R U . . .
H13B H 1.204232 1.481577 0.552815 0.165 Uiso 1 1 calc R U . . .
C14T C 1.101(2) 1.396(2) 0.4708(13) 0.110(8) Uani 1 1 d . . . . .
H14A H 1.055047 1.338187 0.503976 0.132 Uiso 1 1 calc R U . . .
H14B H 1.036802 1.428044 0.448907 0.132 Uiso 1 1 calc R U . . .
O2 O 0.8537(13) 1.1590(14) 0.4185(8) 0.099(5) Uani 1 1 d . . . . .
C21T C 0.896(2) 1.086(2) 0.4650(15) 0.119(9) Uani 1 1 d . . . . .
H21A H 0.959536 1.054951 0.444396 0.143 Uiso 1 1 calc R U . . .
H21B H 0.937238 1.131272 0.505577 0.143 Uiso 1 1 calc R U . . .
C22T C 0.780(3) 0.993(3) 0.4810(14) 0.123(9) Uani 1 1 d . . . . .
H22A H 0.786420 0.964142 0.526583 0.148 Uiso 1 1 calc R U . . .
H22B H 0.761660 0.927511 0.448785 0.148 Uiso 1 1 calc R U . . .
C23T C 0.679(2) 1.055(2) 0.4752(12) 0.114(9) Uani 1 1 d . . . . .
H23A H 0.594928 0.999991 0.458193 0.137 Uiso 1 1 calc R U . . .
H23B H 0.665225 1.084285 0.519447 0.137 Uiso 1 1 calc R U . . .
C24T C 0.725(2) 1.153(2) 0.4291(13) 0.099(7) Uani 1 1 d . . . . .
H24A H 0.672864 1.137642 0.386898 0.119 Uiso 1 1 calc R U . . .
H24B H 0.721693 1.226457 0.449292 0.119 Uiso 1 1 calc R U . . .
O3 O 0.502(2) 0.7554(17) 0.0469(5) 0.104(4) Uani 1 1 d D . . . .
C31T C 0.534(4) 0.843(2) -0.0027(15) 0.169(12) Uani 1 1 d D U . . .
H31A H 0.617629 0.904577 0.008424 0.203 Uiso 1 1 calc R U . . .
H31B H 0.465253 0.878975 -0.008890 0.203 Uiso 1 1 calc R U . . .
C32T C 0.544(3) 0.774(3) -0.0633(13) 0.170(11) Uani 1 1 d D U . . .
H32A H 0.530894 0.812179 -0.105103 0.205 Uiso 1 1 calc R U . . .
H32B H 0.628000 0.758793 -0.063951 0.205 Uiso 1 1 calc R U . . .
C33T C 0.433(4) 0.664(4) -0.051(2) 0.25(2) Uani 1 1 d D U . . .
H33A H 0.348349 0.677740 -0.048361 0.297 Uiso 1 1 calc R U . . .
H33B H 0.426394 0.600851 -0.083648 0.297 Uiso 1 1 calc R U . . .
C34T C 0.490(4) 0.648(3) 0.0152(18) 0.202(17) Uani 1 1 d D U . . .
H34A H 0.431437 0.580667 0.039164 0.243 Uiso 1 1 calc R U . . .
H34B H 0.575559 0.636393 0.010929 0.243 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
K1 O3 2.607(10) . ?
K1 C41 3.009(15) . ?
K1 C11 3.104(16) . ?
K1 C42 3.130(16) . ?
K1 C12 3.147(16) . ?
K1 C46 3.151(18) . ?
K1 C16 3.208(16) . ?
K1 C13 3.308(17) . ?
K1 C43 3.327(15) . ?
K1 C45 3.381(18) . ?
K1 C15 3.389(19) . ?
K1 C14 3.445(17) . ?
K2 O1 2.656(15) . ?
K2 O2 2.747(16) . ?
K2 C21 3.150(15) 1_665 ?
K2 C26 3.166(16) 1_665 ?
K2 C22 3.181(14) 1_665 ?
K2 C52 3.193(15) . ?
K2 C51 3.198(16) . ?
K2 C53 3.223(18) . ?
K2 C25 3.250(16) 1_665 ?
K2 C56 3.274(14) . ?
K2 C23 3.279(14) 1_665 ?
K2 C54 3.327(18) . ?
Al1 C1 1.959(15) . ?
Al1 C22 1.991(16) . ?
Al1 N1 1.997(12) . ?
Al1 C11 2.016(16) . ?
Al2 N2 1.947(14) . ?
Al2 C12 1.978(16) . ?
Al2 C2 1.980(19) . ?
Al2 C21 2.022(16) . ?
N1 N2 1.356(17) . ?
N1 C31 1.410(17) . ?
N2 C33 1.36(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C11 C16 1.378(19) . ?
C11 C12 1.47(2) . ?
C12 C13 1.38(2) . ?
C13 C14 1.47(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.33(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.39(2) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.37(2) . ?
C21 C26 1.44(2) . ?
C22 C23 1.401(19) . ?
C23 C24 1.37(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.42(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.38(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C32 1.40(2) . ?
C31 H31 0.9500 . ?
C32 C33 1.38(2) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
Al3 N43 1.922(14) . ?
Al3 C3 1.991(17) . ?
Al3 C41 2.017(15) . ?
Al3 C51 2.034(18) . ?
Al4 C52 1.962(17) . ?
Al4 N4 1.982(13) . ?
Al4 C4 1.989(17) . ?
Al4 C42 2.006(16) . ?
N4 C63 1.31(2) . ?
N4 N43 1.428(17) . ?
N43 C61 1.316(18) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C41 C46 1.39(2) . ?
C41 C42 1.43(2) . ?
C42 C43 1.41(2) . ?
C43 C44 1.37(2) . ?
C43 H43 0.9500 . ?
C44 C45 1.37(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.40(2) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C56 1.46(2) . ?
C51 C52 1.47(2) . ?
C52 C53 1.38(2) . ?
C53 C54 1.40(3) . ?
C53 H53 0.9500 . ?
C54 C55 1.37(2) . ?
C54 H54 0.9500 . ?
C55 C56 1.40(2) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C61 C62 1.36(2) . ?
C61 H61 0.9500 . ?
C62 C63 1.37(2) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
O1 C14T 1.41(3) . ?
O1 C11T 1.46(2) . ?
C11T C12T 1.52(3) . ?
C11T H11A 0.9900 . ?
C11T H11B 0.9900 . ?
C12T C13T 1.38(3) . ?
C12T H12A 0.9900 . ?
C12T H12B 0.9900 . ?
C13T C14T 1.48(3) . ?
C13T H13A 0.9900 . ?
C13T H13B 0.9900 . ?
C14T H14A 0.9900 . ?
C14T H14B 0.9900 . ?
O2 C24T 1.40(2) . ?
O2 C21T 1.45(3) . ?
C21T C22T 1.44(3) . ?
C21T H21A 0.9900 . ?
C21T H21B 0.9900 . ?
C22T C23T 1.53(3) . ?
C22T H22A 0.9900 . ?
C22T H22B 0.9900 . ?
C23T C24T 1.47(4) . ?
C23T H23A 0.9900 . ?
C23T H23B 0.9900 . ?
C24T H24A 0.9900 . ?
C24T H24B 0.9900 . ?
O3 C34T 1.42(2) . ?
O3 C31T 1.42(2) . ?
C31T C32T 1.506(10) . ?
C31T H31A 0.9900 . ?
C31T H31B 0.9900 . ?
C32T C33T 1.504(10) . ?
C32T H32A 0.9900 . ?
C32T H32B 0.9900 . ?
C33T C34T 1.500(10) . ?
C33T H33A 0.9900 . ?
C33T H33B 0.9900 . ?
C34T H34A 0.9900 . ?
C34T H34B 0.9900 . ?

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
O3 K1 C41 125.6(6) . . ?
O3 K1 C11 124.7(5) . . ?
C41 K1 C11 109.6(3) . . ?
O3 K1 C42 99.6(5) . . ?
C41 K1 C42 26.9(4) . . ?
C11 K1 C42 134.8(4) . . ?
O3 K1 C12 98.6(5) . . ?
C41 K1 C12 135.4(4) . . ?
C11 K1 C12 27.2(4) . . ?
C42 K1 C12 161.8(3) . . ?
O3 K1 C46 141.8(6) . . ?
C41 K1 C46 26.0(4) . . ?
C11 K1 C46 89.4(4) . . ?
C42 K1 C46 45.7(4) . . ?
C12 K1 C46 116.6(4) . . ?
O3 K1 C16 141.8(6) . . ?
C41 K1 C16 90.1(4) . . ?
C11 K1 C16 25.2(4) . . ?
C42 K1 C16 117.0(4) . . ?
C12 K1 C16 45.5(4) . . ?
C46 K1 C16 76.3(3) . . ?
O3 K1 C13 92.0(6) . . ?
C41 K1 C13 133.0(5) . . ?
C11 K1 C13 44.3(5) . . ?
C42 K1 C13 154.5(5) . . ?
C12 K1 C13 24.6(4) . . ?
C46 K1 C13 126.2(5) . . ?
C16 K1 C13 50.1(5) . . ?
O3 K1 C43 91.1(5) . . ?
C41 K1 C43 44.9(4) . . ?
C11 K1 C43 132.7(4) . . ?
C42 K1 C43 25.0(4) . . ?
C12 K1 C43 153.6(5) . . ?
C46 K1 C43 50.7(4) . . ?
C16 K1 C43 126.7(4) . . ?
C13 K1 C43 176.8(4) . . ?
O3 K1 C45 125.9(6) . . ?
C41 K1 C45 43.9(4) . . ?
C11 K1 C45 91.7(4) . . ?
C42 K1 C45 50.5(4) . . ?
C12 K1 C45 116.2(4) . . ?
C46 K1 C45 24.4(4) . . ?
C16 K1 C45 88.2(5) . . ?
C13 K1 C45 135.6(5) . . ?
C43 K1 C45 41.3(4) . . ?
O3 K1 C15 129.0(6) . . ?
C41 K1 C15 90.6(4) . . ?
C11 K1 C15 43.7(4) . . ?
C42 K1 C15 115.3(4) . . ?
C12 K1 C15 51.8(4) . . ?
C46 K1 C15 86.7(5) . . ?
C16 K1 C15 24.0(4) . . ?
C13 K1 C15 42.6(5) . . ?
C43 K1 C15 134.9(4) . . ?
C45 K1 C15 105.0(3) . . ?
O3 K1 C14 106.8(6) . . ?
C41 K1 C14 109.0(5) . . ?
C11 K1 C14 50.0(4) . . ?
C42 K1 C14 129.7(5) . . ?
C12 K1 C14 43.9(4) . . ?
C46 K1 C14 108.8(5) . . ?
C16 K1 C14 40.9(5) . . ?
C13 K1 C14 25.0(4) . . ?
C43 K1 C14 153.6(4) . . ?
C45 K1 C14 127.1(5) . . ?
C15 K1 C14 22.3(4) . . ?
O1 K2 O2 76.2(4) . . ?
O1 K2 C21 111.4(5) . 1_665 ?
O2 K2 C21 129.4(4) . 1_665 ?
O1 K2 C26 133.8(5) . 1_665 ?
O2 K2 C26 114.2(5) . 1_665 ?
C21 K2 C26 26.4(4) 1_665 1_665 ?
O1 K2 C22 88.9(5) . 1_665 ?
O2 K2 C22 115.0(4) . 1_665 ?
C21 K2 C22 25.0(4) 1_665 1_665 ?
C26 K2 C22 45.2(4) 1_665 1_665 ?
O1 K2 C52 130.4(4) . . ?
O2 K2 C52 113.7(5) . . ?
C21 K2 C52 98.8(3) 1_665 . ?
C26 K2 C52 88.4(4) 1_665 . ?
C22 K2 C52 123.0(4) 1_665 . ?
O1 K2 C51 113.5(5) . . ?
O2 K2 C51 91.1(5) . . ?
C21 K2 C51 125.2(4) 1_665 . ?
C26 K2 C51 111.2(4) 1_665 . ?
C22 K2 C51 149.6(3) 1_665 . ?
C52 K2 C51 26.6(4) . . ?
O1 K2 C53 115.3(5) . . ?
O2 K2 C53 134.6(5) . . ?
C21 K2 C53 89.1(5) 1_665 . ?
C26 K2 C53 89.7(4) 1_665 . ?
C22 K2 C53 109.2(4) 1_665 . ?
C52 K2 C53 24.8(4) . . ?
C51 K2 C53 43.5(5) . . ?
O1 K2 C25 127.8(5) . 1_665 ?
O2 K2 C25 89.6(4) . 1_665 ?
C21 K2 C25 44.9(4) 1_665 1_665 ?
C26 K2 C25 24.8(4) 1_665 1_665 ?
C22 K2 C25 52.1(4) 1_665 1_665 ?
C52 K2 C25 101.4(5) . 1_665 ?
C51 K2 C25 116.7(5) . 1_665 ?
C53 K2 C25 110.3(5) . 1_665 ?
O1 K2 C56 87.7(5) . . ?
O2 K2 C56 88.7(4) . . ?
C21 K2 C56 139.7(4) 1_665 . ?
C26 K2 C56 134.9(4) 1_665 . ?
C22 K2 C56 154.5(4) 1_665 . ?
C52 K2 C56 46.6(4) . . ?
C51 K2 C56 26.1(4) . . ?
C53 K2 C56 50.7(5) . . ?
C25 K2 C56 142.7(5) 1_665 . ?
O1 K2 C23 86.3(5) . 1_665 ?
O2 K2 C23 90.3(4) . 1_665 ?
C21 K2 C23 43.3(4) 1_665 1_665 ?
C26 K2 C23 50.6(4) 1_665 1_665 ?
C22 K2 C23 25.0(3) 1_665 1_665 ?
C52 K2 C23 138.8(4) . 1_665 ?
C51 K2 C23 159.8(4) . 1_665 ?
C53 K2 C23 132.3(5) . 1_665 ?
C25 K2 C23 43.2(4) 1_665 1_665 ?
C56 K2 C23 174.0(4) . 1_665 ?
O1 K2 C54 90.8(5) . . ?
O2 K2 C54 130.3(5) . . ?
C21 K2 C54 100.2(4) 1_665 . ?
C26 K2 C54 109.3(5) 1_665 . ?
C22 K2 C54 112.4(4) 1_665 . ?
C52 K2 C54 44.4(4) . . ?
C51 K2 C54 50.4(4) . . ?
C53 K2 C54 24.6(5) . . ?
C25 K2 C54 132.5(4) 1_665 . ?
C56 K2 C54 42.4(4) . . ?
C23 K2 C54 137.3(4) 1_665 . ?
C1 Al1 C22 118.8(6) . . ?
C1 Al1 N1 110.3(6) . . ?
C22 Al1 N1 99.6(5) . . ?
C1 Al1 C11 121.1(7) . . ?
C22 Al1 C11 105.4(6) . . ?
N1 Al1 C11 97.6(6) . . ?
N2 Al2 C12 97.4(6) . . ?
N2 Al2 C2 109.9(8) . . ?
C12 Al2 C2 117.6(8) . . ?
N2 Al2 C21 100.6(6) . . ?
C12 Al2 C21 106.4(6) . . ?
C2 Al2 C21 121.1(7) . . ?
N2 N1 C31 109.9(12) . . ?
N2 N1 Al1 118.7(9) . . ?
C31 N1 Al1 131.1(11) . . ?
N1 N2 C33 106.5(12) . . ?
N1 N2 Al2 116.9(9) . . ?
C33 N2 Al2 136.4(12) . . ?
Al1 C1 H1A 109.5 . . ?
Al1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Al1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Al2 C2 H2A 109.5 . . ?
Al2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Al2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C16 C11 C12 119.3(14) . . ?
C16 C11 Al1 126.1(12) . . ?
C12 C11 Al1 114.3(11) . . ?
C16 C11 K1 81.6(9) . . ?
C12 C11 K1 78.0(8) . . ?
Al1 C11 K1 104.7(6) . . ?
C13 C12 C11 116.3(16) . . ?
C13 C12 Al2 126.9(14) . . ?
C11 C12 Al2 116.8(10) . . ?
C13 C12 K1 84.2(10) . . ?
C11 C12 K1 74.8(8) . . ?
Al2 C12 K1 109.5(6) . . ?
C12 C13 C14 120.6(19) . . ?
C12 C13 K1 71.2(10) . . ?
C14 C13 K1 82.7(9) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
K1 C13 H13 117.0 . . ?
C15 C14 C13 121.3(16) . . ?
C15 C14 K1 76.5(10) . . ?
C13 C14 K1 72.3(9) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
K1 C14 H14 123.3 . . ?
C14 C15 C16 118.9(16) . . ?
C14 C15 K1 81.2(11) . . ?
C16 C15 K1 70.6(9) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
K1 C15 H15 118.5 . . ?
C11 C16 C15 123.4(17) . . ?
C11 C16 K1 73.2(9) . . ?
C15 C16 K1 85.3(11) . . ?
C11 C16 H16 118.3 . . ?
C15 C16 H16 118.3 . . ?
K1 C16 H16 113.0 . . ?
C22 C21 C26 120.2(15) . . ?
C22 C21 Al2 116.9(10) . . ?
C26 C21 Al2 122.9(12) . . ?
C22 C21 K2 78.8(9) . 1_445 ?
C26 C21 K2 77.4(9) . 1_445 ?
Al2 C21 K2 115.8(6) . 1_445 ?
C21 C22 C23 118.0(14) . . ?
C21 C22 Al1 117.3(10) . . ?
C23 C22 Al1 124.3(11) . . ?
C21 C22 K2 76.3(8) . 1_445 ?
C23 C22 K2 81.4(8) . 1_445 ?
Al1 C22 K2 117.8(6) . 1_445 ?
C24 C23 C22 123.2(16) . . ?
C24 C23 K2 80.4(8) . 1_445 ?
C22 C23 K2 73.6(7) . 1_445 ?
C24 C23 H23 118.4 . . ?
C22 C23 H23 118.4 . . ?
K2 C23 H23 118.2 1_445 . ?
C23 C24 C25 119.2(15) . . ?
C23 C24 K2 75.8(8) . 1_445 ?
C25 C24 K2 74.2(8) . 1_445 ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
K2 C24 H24 120.8 1_445 . ?
C26 C25 C24 119.0(16) . . ?
C26 C25 K2 74.2(9) . 1_445 ?
C24 C25 K2 81.0(9) . 1_445 ?
C26 C25 H25 120.5 . . ?
C24 C25 H25 120.5 . . ?
K2 C25 H25 115.0 1_445 . ?
C25 C26 C21 120.2(17) . . ?
C25 C26 K2 81.0(10) . 1_445 ?
C21 C26 K2 76.2(9) . 1_445 ?
C25 C26 H26 119.9 . . ?
C21 C26 H26 119.9 . . ?
K2 C26 H26 113.3 1_445 . ?
C32 C31 N1 106.2(14) . . ?
C32 C31 H31 126.9 . . ?
N1 C31 H31 126.9 . . ?
C33 C32 C31 106.0(15) . . ?
C33 C32 H32 127.0 . . ?
C31 C32 H32 127.0 . . ?
N2 C33 C32 111.4(16) . . ?
N2 C33 H33 124.3 . . ?
C32 C33 H33 124.3 . . ?
N43 Al3 C3 107.1(6) . . ?
N43 Al3 C41 98.7(6) . . ?
C3 Al3 C41 120.1(7) . . ?
N43 Al3 C51 99.4(6) . . ?
C3 Al3 C51 119.0(7) . . ?
C41 Al3 C51 108.3(6) . . ?
C52 Al4 N4 100.2(5) . . ?
C52 Al4 C4 118.2(8) . . ?
N4 Al4 C4 108.5(8) . . ?
C52 Al4 C42 109.9(7) . . ?
N4 Al4 C42 96.8(6) . . ?
C4 Al4 C42 119.1(8) . . ?
C63 N4 N43 108.8(12) . . ?
C63 N4 Al4 134.6(12) . . ?
N43 N4 Al4 116.5(9) . . ?
C61 N43 N4 103.2(12) . . ?
C61 N43 Al3 140.0(11) . . ?
N4 N43 Al3 116.8(8) . . ?
Al3 C3 H3A 109.5 . . ?
Al3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Al3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Al4 C4 H4A 109.5 . . ?
Al4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Al4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C46 C41 C42 119.2(14) . . ?
C46 C41 Al3 126.6(13) . . ?
C42 C41 Al3 114.2(11) . . ?
C46 C41 K1 82.7(9) . . ?
C42 C41 K1 81.3(9) . . ?
Al3 C41 K1 106.4(6) . . ?
C43 C42 C41 118.1(14) . . ?
C43 C42 Al4 124.4(12) . . ?
C41 C42 Al4 117.4(11) . . ?
C43 C42 K1 85.3(9) . . ?
C41 C42 K1 71.9(8) . . ?
Al4 C42 K1 109.3(7) . . ?
C44 C43 C42 121.8(14) . . ?
C44 C43 K1 84.3(10) . . ?
C42 C43 K1 69.7(8) . . ?
C44 C43 H43 119.1 . . ?
C42 C43 H43 119.1 . . ?
K1 C43 H43 117.3 . . ?
C45 C44 C43 119.2(14) . . ?
C45 C44 K1 74.8(10) . . ?
C43 C44 K1 72.5(9) . . ?
C45 C44 H44 120.4 . . ?
C43 C44 H44 120.4 . . ?
K1 C44 H44 123.8 . . ?
C44 C45 C46 121.9(16) . . ?
C44 C45 K1 82.2(11) . . ?
C46 C45 K1 68.5(10) . . ?
C44 C45 H45 119.0 . . ?
C46 C45 H45 119.0 . . ?
K1 C45 H45 121.1 . . ?
C41 C46 C45 119.6(17) . . ?
C41 C46 K1 71.3(10) . . ?
C45 C46 K1 87.1(11) . . ?
C41 C46 H46 120.2 . . ?
C45 C46 H46 120.2 . . ?
K1 C46 H46 111.7 . . ?
C56 C51 C52 121.5(14) . . ?
C56 C51 Al3 122.3(13) . . ?
C52 C51 Al3 116.2(11) . . ?
C56 C51 K2 79.8(8) . . ?
C52 C51 K2 76.5(8) . . ?
Al3 C51 K2 112.4(6) . . ?
C53 C52 C51 113.5(16) . . ?
C53 C52 Al4 132.0(14) . . ?
C51 C52 Al4 114.5(11) . . ?
C53 C52 K2 78.8(10) . . ?
C51 C52 K2 76.9(9) . . ?
Al4 C52 K2 110.3(5) . . ?
C52 C53 C54 125.2(19) . . ?
C52 C53 K2 76.4(9) . . ?
C54 C53 K2 81.9(11) . . ?
C52 C53 H53 117.4 . . ?
C54 C53 H53 117.4 . . ?
K2 C53 H53 114.2 . . ?
C55 C54 C53 121.6(15) . . ?
C55 C54 K2 79.1(9) . . ?
C53 C54 K2 73.6(10) . . ?
C55 C54 H54 119.2 . . ?
C53 C54 H54 119.2 . . ?
K2 C54 H54 118.9 . . ?
C54 C55 C56 119.0(15) . . ?
C54 C55 K2 77.1(9) . . ?
C56 C55 K2 74.7(8) . . ?
C54 C55 H55 120.5 . . ?
C56 C55 H55 120.5 . . ?
K2 C55 H55 118.6 . . ?
C55 C56 C51 119.2(16) . . ?
C55 C56 K2 80.9(8) . . ?
C51 C56 K2 74.1(8) . . ?
C55 C56 H56 120.4 . . ?
C51 C56 H56 120.4 . . ?
K2 C56 H56 115.3 . . ?
N43 C61 C62 113.8(14) . . ?
N43 C61 H61 123.1 . . ?
C62 C61 H61 123.1 . . ?
C61 C62 C63 104.1(15) . . ?
C61 C62 H62 127.9 . . ?
C63 C62 H62 127.9 . . ?
N4 C63 C62 110.1(14) . . ?
N4 C63 H63 125.0 . . ?
C62 C63 H63 125.0 . . ?
C14T O1 C11T 108.0(16) . . ?
C14T O1 K2 116.9(12) . . ?
C11T O1 K2 133.7(13) . . ?
O1 C11T C12T 102.4(19) . . ?
O1 C11T H11A 111.3 . . ?
C12T C11T H11A 111.3 . . ?
O1 C11T H11B 111.3 . . ?
C12T C11T H11B 111.3 . . ?
H11A C11T H11B 109.2 . . ?
C13T C12T C11T 109(2) . . ?
C13T C12T H12A 109.9 . . ?
C11T C12T H12A 109.9 . . ?
C13T C12T H12B 109.9 . . ?
C11T C12T H12B 109.9 . . ?
H12A C12T H12B 108.3 . . ?
C12T C13T C14T 107(2) . . ?
C12T C13T H13A 110.3 . . ?
C14T C13T H13A 110.3 . . ?
C12T C13T H13B 110.3 . . ?
C14T C13T H13B 110.3 . . ?
H13A C13T H13B 108.5 . . ?
O1 C14T C13T 108(2) . . ?
O1 C14T K2 42.2(9) . . ?
C13T C14T K2 140.8(18) . . ?
O1 C14T H14A 110.2 . . ?
C13T C14T H14A 110.2 . . ?
K2 C14T H14A 105.2 . . ?
O1 C14T H14B 110.2 . . ?
C13T C14T H14B 110.2 . . ?
K2 C14T H14B 72.8 . . ?
H14A C14T H14B 108.5 . . ?
C24T O2 C21T 111.4(18) . . ?
C24T O2 K2 130.1(14) . . ?
C21T O2 K2 117.6(13) . . ?
C22T C21T O2 105(2) . . ?
C22T C21T H21A 110.7 . . ?
O2 C21T H21A 110.7 . . ?
C22T C21T H21B 110.7 . . ?
O2 C21T H21B 110.7 . . ?
H21A C21T H21B 108.8 . . ?
C21T C22T C23T 101(2) . . ?
C21T C22T H22A 111.5 . . ?
C23T C22T H22A 111.5 . . ?
C21T C22T H22B 111.5 . . ?
C23T C22T H22B 111.5 . . ?
H22A C22T H22B 109.4 . . ?
C24T C23T C22T 109(2) . . ?
C24T C23T H23A 110.0 . . ?
C22T C23T H23A 110.0 . . ?
C24T C23T H23B 110.0 . . ?
C22T C23T H23B 110.0 . . ?
H23A C23T H23B 108.4 . . ?
O2 C24T C23T 103(2) . . ?
O2 C24T H24A 111.1 . . ?
C23T C24T H24A 111.1 . . ?
O2 C24T H24B 111.1 . . ?
C23T C24T H24B 111.1 . . ?
H24A C24T H24B 109.0 . . ?
C34T O3 C31T 107(2) . . ?
C34T O3 K1 115.6(18) . . ?
C31T O3 K1 135.1(16) . . ?
O3 C31T C32T 101.7(18) . . ?
O3 C31T H31A 111.4 . . ?
C32T C31T H31A 111.4 . . ?
O3 C31T H31B 111.4 . . ?
C32T C31T H31B 111.4 . . ?
H31A C31T H31B 109.3 . . ?
C33T C32T C31T 99(3) . . ?
C33T C32T H32A 112.0 . . ?
C31T C32T H32A 112.0 . . ?
C33T C32T H32B 112.0 . . ?
C31T C32T H32B 112.0 . . ?
H32A C32T H32B 109.6 . . ?
C34T C33T C32T 92(3) . . ?
C34T C33T H33A 113.3 . . ?
C32T C33T H33A 113.3 . . ?
C34T C33T H33B 113.3 . . ?
C32T C33T H33B 113.3 . . ?
H33A C33T H33B 110.7 . . ?
O3 C34T C33T 101(3) . . ?
O3 C34T K1 42.7(13) . . ?
C33T C34T K1 139(3) . . ?
O3 C34T H34A 111.7 . . ?
C33T C34T H34A 111.7 . . ?
K1 C34T H34A 77.5 . . ?
O3 C34T H34B 111.7 . . ?
C33T C34T H34B 111.7 . . ?
K1 C34T H34B 101.5 . . ?
H34A C34T H34B 109.4 . . ?

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
C31 N1 N2 C33 2.3(15) . . . . ?
Al1 N1 N2 C33 176.9(10) . . . . ?
C31 N1 N2 Al2 -173.2(9) . . . . ?
Al1 N1 N2 Al2 1.3(13) . . . . ?
C16 C11 C12 C13 2(2) . . . . ?
Al1 C11 C12 C13 176.3(12) . . . . ?
K1 C11 C12 C13 75.4(13) . . . . ?
C16 C11 C12 Al2 -177.6(11) . . . . ?
Al1 C11 C12 Al2 -3.5(15) . . . . ?
K1 C11 C12 Al2 -104.4(9) . . . . ?
C16 C11 C12 K1 -73.2(13) . . . . ?
Al1 C11 C12 K1 100.9(9) . . . . ?
C11 C12 C13 C14 -1(2) . . . . ?
Al2 C12 C13 C14 179.1(11) . . . . ?
K1 C12 C13 C14 69.0(15) . . . . ?
C11 C12 C13 K1 -69.8(12) . . . . ?
Al2 C12 C13 K1 110.0(12) . . . . ?
C12 C13 C14 C15 -2(3) . . . . ?
K1 C13 C14 C15 61.2(16) . . . . ?
C12 C13 C14 K1 -63.0(14) . . . . ?
C13 C14 C15 C16 3(3) . . . . ?
K1 C14 C15 C16 62.0(15) . . . . ?
C13 C14 C15 K1 -59.2(15) . . . . ?
C12 C11 C16 C15 -1(2) . . . . ?
Al1 C11 C16 C15 -174.6(13) . . . . ?
K1 C11 C16 C15 -72.5(15) . . . . ?
C12 C11 C16 K1 71.2(12) . . . . ?
Al1 C11 C16 K1 -102.1(11) . . . . ?
C14 C15 C16 C11 -1(3) . . . . ?
K1 C15 C16 C11 66.4(14) . . . . ?
C14 C15 C16 K1 -67.7(16) . . . . ?
C26 C21 C22 C23 -4(2) . . . . ?
Al2 C21 C22 C23 174.3(10) . . . . ?
K2 C21 C22 C23 -72.3(11) 1_445 . . . ?
C26 C21 C22 Al1 -177.4(11) . . . . ?
Al2 C21 C22 Al1 1.1(15) . . . . ?
K2 C21 C22 Al1 114.5(8) 1_445 . . . ?
C26 C21 C22 K2 68.1(13) . . . 1_445 ?
Al2 C21 C22 K2 -113.3(8) . . . 1_445 ?
C21 C22 C23 C24 3(2) . . . . ?
Al1 C22 C23 C24 175.7(11) . . . . ?
K2 C22 C23 C24 -66.4(13) 1_445 . . . ?
C21 C22 C23 K2 69.4(11) . . . 1_445 ?
Al1 C22 C23 K2 -117.9(10) . . . 1_445 ?
C22 C23 C24 C25 1(2) . . . . ?
K2 C23 C24 C25 -62.4(13) 1_445 . . . ?
C22 C23 C24 K2 63.1(13) . . . 1_445 ?
C23 C24 C25 C26 -3(2) . . . . ?
K2 C24 C25 C26 -66.2(13) 1_445 . . . ?
C23 C24 C25 K2 63.2(13) . . . 1_445 ?
C24 C25 C26 C21 2(2) . . . . ?
K2 C25 C26 C21 -68.2(13) 1_445 . . . ?
C24 C25 C26 K2 69.9(13) . . . 1_445 ?
C22 C21 C26 C25 2(2) . . . . ?
Al2 C21 C26 C25 -176.5(11) . . . . ?
K2 C21 C26 C25 70.8(13) 1_445 . . . ?
C22 C21 C26 K2 -68.8(13) . . . 1_445 ?
Al2 C21 C26 K2 112.7(10) . . . 1_445 ?
N2 N1 C31 C32 -1.8(16) . . . . ?
Al1 N1 C31 C32 -175.5(10) . . . . ?
N1 C31 C32 C33 0.6(18) . . . . ?
N1 N2 C33 C32 -2.0(18) . . . . ?
Al2 N2 C33 C32 172.3(12) . . . . ?
C31 C32 C33 N2 1(2) . . . . ?
C63 N4 N43 C61 -0.6(15) . . . . ?
Al4 N4 N43 C61 -177.3(9) . . . . ?
C63 N4 N43 Al3 178.9(11) . . . . ?
Al4 N4 N43 Al3 2.2(12) . . . . ?
C46 C41 C42 C43 -2(2) . . . . ?
Al3 C41 C42 C43 178.3(12) . . . . ?
K1 C41 C42 C43 74.2(13) . . . . ?
C46 C41 C42 Al4 -179.3(12) . . . . ?
Al3 C41 C42 Al4 1.3(15) . . . . ?
K1 C41 C42 Al4 -102.8(9) . . . . ?
C46 C41 C42 K1 -76.5(13) . . . . ?
Al3 C41 C42 K1 104.1(9) . . . . ?
C41 C42 C43 C44 3(2) . . . . ?
Al4 C42 C43 C44 179.5(13) . . . . ?
K1 C42 C43 C44 69.3(15) . . . . ?
C41 C42 C43 K1 -66.5(12) . . . . ?
Al4 C42 C43 K1 110.2(12) . . . . ?
C42 C43 C44 C45 -1(3) . . . . ?
K1 C43 C44 C45 60.6(16) . . . . ?
C42 C43 C44 K1 -61.8(14) . . . . ?
C43 C44 C45 C46 -1(3) . . . . ?
K1 C44 C45 C46 58.6(14) . . . . ?
C43 C44 C45 K1 -59.4(16) . . . . ?
C42 C41 C46 C45 0(2) . . . . ?
Al3 C41 C46 C45 179.7(12) . . . . ?
K1 C41 C46 C45 -75.2(15) . . . . ?
C42 C41 C46 K1 75.7(13) . . . . ?
Al3 C41 C46 K1 -105.0(12) . . . . ?
C44 C45 C46 C41 1(2) . . . . ?
K1 C45 C46 C41 66.5(14) . . . . ?
C44 C45 C46 K1 -65.4(16) . . . . ?
C56 C51 C52 C53 2(2) . . . . ?
Al3 C51 C52 C53 -180.0(11) . . . . ?
K2 C51 C52 C53 71.4(12) . . . . ?
C56 C51 C52 Al4 -175.5(11) . . . . ?
Al3 C51 C52 Al4 2.0(14) . . . . ?
K2 C51 C52 Al4 -106.6(8) . . . . ?
C56 C51 C52 K2 -68.9(12) . . . . ?
Al3 C51 C52 K2 108.6(8) . . . . ?
C51 C52 C53 C54 -1(2) . . . . ?
Al4 C52 C53 C54 176.8(13) . . . . ?
K2 C52 C53 C54 69.5(17) . . . . ?
C51 C52 C53 K2 -70.3(12) . . . . ?
Al4 C52 C53 K2 107.3(13) . . . . ?
C52 C53 C54 C55 -1(3) . . . . ?
K2 C53 C54 C55 65.7(16) . . . . ?
C52 C53 C54 K2 -66.9(16) . . . . ?
C53 C54 C55 C56 1(2) . . . . ?
K2 C54 C55 C56 64.2(12) . . . . ?
C53 C54 C55 K2 -62.9(16) . . . . ?
C54 C55 C56 C51 0(2) . . . . ?
K2 C55 C56 C51 65.9(11) . . . . ?
C54 C55 C56 K2 -65.5(13) . . . . ?
C52 C51 C56 C55 -2(2) . . . . ?
Al3 C51 C56 C55 -179.9(10) . . . . ?
K2 C51 C56 C55 -69.7(12) . . . . ?
C52 C51 C56 K2 67.2(12) . . . . ?
Al3 C51 C56 K2 -110.2(10) . . . . ?
N4 N43 C61 C62 -0.6(17) . . . . ?
Al3 N43 C61 C62 -179.9(12) . . . . ?
N43 C61 C62 C63 1(2) . . . . ?
N43 N4 C63 C62 1.5(18) . . . . ?
Al4 N4 C63 C62 177.4(11) . . . . ?
C61 C62 C63 N4 -2(2) . . . . ?
C14T O1 C11T C12T -23(3) . . . . ?
K2 O1 C11T C12T 142.0(19) . . . . ?
O1 C11T C12T C13T 20(3) . . . . ?
C11T C12T C13T C14T -9(4) . . . . ?
C11T O1 C14T C13T 19(3) . . . . ?
K2 O1 C14T C13T -149.3(18) . . . . ?
C11T O1 C14T K2 168(2) . . . . ?
C12T C13T C14T O1 -6(3) . . . . ?
C12T C13T C14T K2 -39(4) . . . . ?
C24T O2 C21T C22T 29(3) . . . . ?
K2 O2 C21T C22T -141.8(17) . . . . ?
O2 C21T C22T C23T -31(3) . . . . ?
C21T C22T C23T C24T 26(3) . . . . ?
C21T O2 C24T C23T -11(2) . . . . ?
K2 O2 C24T C23T 157.6(15) . . . . ?
C22T C23T C24T O2 -9(2) . . . . ?
C34T O3 C31T C32T -2(4) . . . . ?
K1 O3 C31T C32T 161(2) . . . . ?
O3 C31T C32T C33T 39(3) . . . . ?
C31T C32T C33T C34T -57(3) . . . . ?
C31T O3 C34T C33T -35(4) . . . . ?
K1 O3 C34T C33T 158(2) . . . . ?
C31T O3 C34T K1 167(3) . . . . ?
C32T C33T C34T O3 57(3) . . . . ?
C32T C33T C34T K1 79(4) . . . . ?

_refine_diff_density_max         0.609
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.137


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1py2_wa3112_AV
_database_code_depnum_ccdc_archive 'CCDC 2385629'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H24 Al2 N2, C6 H6'
_chemical_formula_sum            'C30 H30 Al2 N2'
_chemical_formula_weight         472.52

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0697(3)
_cell_length_b                   9.2595(4)
_cell_length_c                   9.8024(4)
_cell_angle_alpha                112.117(4)
_cell_angle_beta                 105.052(3)
_cell_angle_gamma                102.588(3)
_cell_volume                     689.09(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    10834
_cell_measurement_theta_min      4.1750
_cell_measurement_theta_max      27.7840

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_F_000             250
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.260
_exptl_absorpt_coefficient_mu    0.125
_shelx_estimated_absorpt_T_min   0.965
_shelx_estimated_absorpt_T_max   0.968
_exptl_absorpt_correction_T_min  0.84751
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            15378
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.570
_diffrn_reflns_theta_max         27.872
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             3239
_reflns_number_gt                3123
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  'IUCr PublCIF online service'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0518P)²+0.2530P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3239
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.1059
_refine_ls_wR_factor_gt          0.1051
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Al1 Al 0.50122(4) 0.67728(4) 0.65884(4) 0.02165(12) Uani 1 1 d . . . . .
C1 C 0.44986(13) 0.45451(14) 0.65156(13) 0.0224(2) Uani 1 1 d . . . . .
C2 C 0.44452(13) 0.31262(14) 0.52147(14) 0.0231(2) Uani 1 1 d . . . . .
C3 C 0.39849(16) 0.15719(15) 0.52187(17) 0.0317(3) Uani 1 1 d . . . . .
H3 H 0.394687 0.061698 0.436023 0.038 Uiso 1 1 calc R U . . .
C4 C 0.35853(18) 0.13887(18) 0.64342(19) 0.0378(3) Uani 1 1 d . . . . .
H4 H 0.328440 0.032409 0.640241 0.045 Uiso 1 1 calc R U . . .
C5 C 0.36275(17) 0.27644(18) 0.76917(17) 0.0359(3) Uani 1 1 d . . . . .
H5 H 0.334689 0.264936 0.852359 0.043 Uiso 1 1 calc R U . . .
C6 C 0.40833(15) 0.43134(16) 0.77271(14) 0.0291(3) Uani 1 1 d . . . . .
H6 H 0.411659 0.525155 0.859940 0.035 Uiso 1 1 calc R U . . .
C7 C 0.63772(18) 0.87154(17) 0.86917(16) 0.0379(3) Uani 1 1 d . . . . .
H7A H 0.654872 0.974118 0.858071 0.057 Uiso 1 1 calc R U . . .
H7B H 0.582398 0.875748 0.943455 0.057 Uiso 1 1 calc R U . . .
H7C H 0.743357 0.860784 0.909958 0.057 Uiso 1 1 calc R U . . .
N1 N 0.28313(12) 0.70668(11) 0.61519(11) 0.0228(2) Uani 1 1 d . . . . .
C12 C 0.18493(16) 0.65884(18) 0.46529(15) 0.0343(3) Uani 1 1 d . . . . .
H12 H 0.220543 0.611499 0.381294 0.041 Uiso 1 1 calc R U . . .
C13 C 0.03462(18) 0.6760(2) 0.42909(19) 0.0438(3) Uani 1 1 d . . . . .
H13 H -0.032321 0.640121 0.321803 0.053 Uiso 1 1 calc R U . . .
C14 C -0.01740(18) 0.7452(2) 0.5493(2) 0.0432(3) Uani 1 1 d . . . . .
H14 H -0.119744 0.760259 0.526979 0.052 Uiso 1 1 calc R U . . .
C15 C 0.08036(18) 0.7924(2) 0.70200(19) 0.0419(3) Uani 1 1 d . . . . .
H15 H 0.046386 0.840367 0.787122 0.050 Uiso 1 1 calc R U . . .
C16 C 0.22854(17) 0.76995(17) 0.73172(15) 0.0329(3) Uani 1 1 d . . . . .
H16 H 0.294239 0.800111 0.837875 0.039 Uiso 1 1 calc R U . . .
C21 C 0.0409(3) 0.6639(3) 0.0362(3) 0.0754(6) Uani 1 1 d . . . . .
H21 H 0.069634 0.778401 0.061228 0.091 Uiso 1 1 calc R U . . .
C22 C 0.1605(2) 0.5999(4) 0.0723(2) 0.0737(7) Uani 1 1 d . . . . .
H22 H 0.271968 0.670488 0.122966 0.088 Uiso 1 1 calc R U . . .
C23 C 0.1202(3) 0.4381(4) 0.0362(2) 0.0710(6) Uani 1 1 d . . . . .
H23 H 0.203023 0.394079 0.060730 0.085 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C1 1.9824(12) . ?
Al1 C7 1.9825(13) . ?
Al1 C2 1.9826(12) 2_666 ?
Al1 N1 2.0131(10) . ?
C1 C6 1.4097(16) . ?
C1 C2 1.4259(15) . ?
C2 C3 1.4102(16) . ?
C3 C4 1.3890(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.3877(18) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N1 C12 1.3442(16) . ?
N1 C16 1.3451(15) . ?
C12 C13 1.3766(19) . ?
C12 H12 0.9500 . ?
C13 C14 1.369(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.366(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.3778(19) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C23 1.373(4) 2_565 ?
C21 C22 1.376(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.341(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?

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
C1 Al1 C7 116.82(6) . . ?
C1 Al1 C2 114.66(5) . 2_666 ?
C7 Al1 C2 114.91(6) . 2_666 ?
C1 Al1 N1 102.80(4) . . ?
C7 Al1 N1 102.50(5) . . ?
C2 Al1 N1 102.12(4) 2_666 . ?
C6 C1 C2 118.19(10) . . ?
C6 C1 Al1 119.96(9) . . ?
C2 C1 Al1 121.76(8) . . ?
C3 C2 C1 118.00(10) . . ?
C3 C2 Al1 118.50(9) . 2_666 ?
C1 C2 Al1 123.50(8) . 2_666 ?
C4 C3 C2 122.29(12) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C5 C4 C3 119.69(12) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 119.44(12) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C1 122.38(12) . . ?
C5 C6 H6 118.8 . . ?
C1 C6 H6 118.8 . . ?
Al1 C7 H7A 109.5 . . ?
Al1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Al1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C12 N1 C16 117.72(11) . . ?
C12 N1 Al1 120.10(8) . . ?
C16 N1 Al1 122.16(8) . . ?
N1 C12 C13 122.37(12) . . ?
N1 C12 H12 118.8 . . ?
C13 C12 H12 118.8 . . ?
C14 C13 C12 119.31(14) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C15 C14 C13 118.88(13) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C16 119.57(13) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
N1 C16 C15 122.09(12) . . ?
N1 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C23 C21 C22 119.8(2) 2_565 . ?
C23 C21 H21 120.1 2_565 . ?
C22 C21 H21 120.1 . . ?
C23 C22 C21 120.1(2) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C21 120.0(2) . 2_565 ?
C22 C23 H23 120.0 . . ?
C21 C23 H23 120.0 2_565 . ?

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
C6 C1 C2 C3 -0.23(16) . . . . ?
Al1 C1 C2 C3 -176.68(9) . . . . ?
C6 C1 C2 Al1 179.93(8) . . . 2_666 ?
Al1 C1 C2 Al1 3.48(13) . . . 2_666 ?
C1 C2 C3 C4 0.15(19) . . . . ?
Al1 C2 C3 C4 179.99(10) 2_666 . . . ?
C2 C3 C4 C5 0.2(2) . . . . ?
C3 C4 C5 C6 -0.6(2) . . . . ?
C4 C5 C6 C1 0.5(2) . . . . ?
C2 C1 C6 C5 -0.08(18) . . . . ?
Al1 C1 C6 C5 176.44(10) . . . . ?
C16 N1 C12 C13 1.4(2) . . . . ?
Al1 N1 C12 C13 179.89(12) . . . . ?
N1 C12 C13 C14 0.5(2) . . . . ?
C12 C13 C14 C15 -1.3(2) . . . . ?
C13 C14 C15 C16 0.2(2) . . . . ?
C12 N1 C16 C15 -2.6(2) . . . . ?
Al1 N1 C16 C15 178.97(11) . . . . ?
C14 C15 C16 N1 1.8(2) . . . . ?
C23 C21 C22 C23 0.4(3) 2_565 . . . ?
C21 C22 C23 C21 -0.4(3) . . . 2_565 ?

_refine_diff_density_max         0.295
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.042


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_22_wa3285
_database_code_depnum_ccdc_archive 'CCDC 2385635'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H16 Al4 Br4'
_chemical_formula_sum            'C24 H16 Al4 Br4'
_chemical_formula_weight         731.93

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   10.1518(8)
_cell_length_b                   9.9203(6)
_cell_length_c                   12.7992(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.072(7)
_cell_angle_gamma                90
_cell_volume                     1269.14(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3313
_cell_measurement_theta_min      4.1440
_cell_measurement_theta_max      26.6300

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.915
_exptl_crystal_F_000             704
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    6.493
_shelx_estimated_absorpt_T_min   0.329
_shelx_estimated_absorpt_T_max   0.697
_exptl_absorpt_correction_T_min  0.30742
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            7388
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.484
_diffrn_reflns_theta_max         26.793
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             2682
_reflns_number_gt                2361
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  'IUCr PublCIF online service'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0338P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.0022(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2682
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.0901
_refine_ls_wR_factor_gt          0.0850
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Br1 Br 0.28237(4) 0.88956(4) 0.52493(3) 0.03238(15) Uani 1 1 d . . . . .
Br2 Br 0.52044(4) 0.35145(4) 0.16417(3) 0.03047(15) Uani 1 1 d . . . . .
Al1 Al 0.28750(9) 0.73442(9) 0.39417(8) 0.0177(2) Uani 1 1 d . . . . .
Al2 Al 0.37189(10) 0.49361(9) 0.21999(8) 0.0178(2) Uani 1 1 d . . . . .
C1 C 0.3974(3) 0.7857(3) 0.2872(2) 0.0177(6) Uani 1 1 d . . . . .
C2 C 0.4137(3) 0.6896(3) 0.2066(3) 0.0190(6) Uani 1 1 d . . . . .
C3 C 0.4948(3) 0.7252(3) 0.1312(3) 0.0243(7) Uani 1 1 d . . . . .
H3 H 0.505722 0.662473 0.077296 0.029 Uiso 1 1 calc R U . . .
C4 C 0.5584(4) 0.8485(4) 0.1341(3) 0.0309(8) Uani 1 1 d . . . . .
H4 H 0.613277 0.869592 0.083379 0.037 Uiso 1 1 calc R U . . .
C5 C 0.5413(4) 0.9413(4) 0.2117(3) 0.0317(8) Uani 1 1 d . . . . .
H5 H 0.584275 1.026493 0.213531 0.038 Uiso 1 1 calc R U . . .
C6 C 0.4624(4) 0.9112(3) 0.2863(3) 0.0257(7) Uani 1 1 d . . . . .
H6 H 0.451756 0.976673 0.338311 0.031 Uiso 1 1 calc R U . . .
C7 C 0.3160(3) 0.5462(3) 0.4446(2) 0.0176(6) Uani 1 1 d . . . . .
C8 C 0.3301(3) 0.4492(3) 0.3650(3) 0.0200(7) Uani 1 1 d . . . . .
C9 C 0.3446(3) 0.3106(3) 0.3949(3) 0.0238(7) Uani 1 1 d . . . . .
H9 H 0.354670 0.244713 0.343029 0.029 Uiso 1 1 calc R U . . .
C10 C 0.3442(3) 0.2713(3) 0.4979(3) 0.0263(7) Uani 1 1 d . . . . .
H10 H 0.355512 0.178933 0.516978 0.032 Uiso 1 1 calc R U . . .
C11 C 0.3273(4) 0.3667(4) 0.5743(3) 0.0264(8) Uani 1 1 d . . . . .
H11 H 0.324331 0.338728 0.644869 0.032 Uiso 1 1 calc R U . . .
C12 C 0.3148(3) 0.5021(3) 0.5481(3) 0.0228(7) Uani 1 1 d . . . . .
H12 H 0.305328 0.566122 0.601510 0.027 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Br1 Al1 2.2811(10) . ?
Br2 Al2 2.2695(10) . ?
Al1 C1 1.978(3) . ?
Al1 C7 1.980(3) . ?
Al1 C2 2.261(3) 2 ?
Al2 C2 2.004(3) . ?
Al2 C8 2.023(3) . ?
Al2 C8 2.191(3) 2 ?
Al2 Al2 2.7167(19) 2 ?
C1 C6 1.410(4) . ?
C1 C2 1.436(4) . ?
C2 C3 1.418(4) . ?
C3 C4 1.380(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.398(4) . ?
C7 C8 1.427(4) . ?
C8 C9 1.428(4) . ?
C9 C10 1.375(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.393(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.384(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?

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
C1 Al1 C7 113.59(13) . . ?
C1 Al1 C2 102.64(13) . 2 ?
C7 Al1 C2 93.81(13) . 2 ?
C1 Al1 Br1 114.97(10) . . ?
C7 Al1 Br1 114.69(10) . . ?
C2 Al1 Br1 114.63(9) 2 . ?
C2 Al2 C8 111.81(13) . . ?
C2 Al2 C8 110.27(13) . 2 ?
C8 Al2 C8 94.77(13) . 2 ?
C2 Al2 Br2 114.42(10) . . ?
C8 Al2 Br2 114.27(10) . . ?
C8 Al2 Br2 109.54(9) 2 . ?
C2 Al2 Al2 103.98(9) . 2 ?
C8 Al2 Al2 52.63(10) . 2 ?
C8 Al2 Al2 47.21(9) 2 2 ?
Br2 Al2 Al2 141.02(3) . 2 ?
C6 C1 C2 117.8(3) . . ?
C6 C1 Al1 123.7(2) . . ?
C2 C1 Al1 118.5(2) . . ?
C3 C2 C1 118.5(3) . . ?
C3 C2 Al2 117.2(2) . . ?
C1 C2 Al2 122.0(2) . . ?
C3 C2 Al1 97.9(2) . 2 ?
C1 C2 Al1 94.2(2) . 2 ?
Al2 C2 Al1 93.20(13) . 2 ?
C4 C3 C2 121.8(3) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 119.4(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 120.8(3) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C1 121.7(3) . . ?
C5 C6 H6 119.2 . . ?
C1 C6 H6 119.2 . . ?
C12 C7 C8 119.0(3) . . ?
C12 C7 Al1 125.4(2) . . ?
C8 C7 Al1 115.5(2) . . ?
C7 C8 C9 118.4(3) . . ?
C7 C8 Al2 124.9(2) . . ?
C9 C8 Al2 115.3(2) . . ?
C7 C8 Al2 91.0(2) . 2 ?
C9 C8 Al2 111.7(2) . 2 ?
Al2 C8 Al2 80.17(12) . 2 ?
C10 C9 C8 120.8(3) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 120.1(3) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C12 C11 C10 120.4(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C7 121.2(3) . . ?
C11 C12 H12 119.4 . . ?
C7 C12 H12 119.4 . . ?

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
C6 C1 C2 C3 0.5(5) . . . . ?
Al1 C1 C2 C3 -178.7(2) . . . . ?
C6 C1 C2 Al2 162.8(2) . . . . ?
Al1 C1 C2 Al2 -16.4(4) . . . . ?
C6 C1 C2 Al1 -100.8(3) . . . 2 ?
Al1 C1 C2 Al1 80.0(2) . . . 2 ?
C1 C2 C3 C4 0.4(5) . . . . ?
Al2 C2 C3 C4 -162.7(3) . . . . ?
Al1 C2 C3 C4 99.6(3) 2 . . . ?
C2 C3 C4 C5 -0.9(6) . . . . ?
C3 C4 C5 C6 0.5(6) . . . . ?
C4 C5 C6 C1 0.5(6) . . . . ?
C2 C1 C6 C5 -1.0(5) . . . . ?
Al1 C1 C6 C5 178.2(3) . . . . ?
C12 C7 C8 C9 -1.0(5) . . . . ?
Al1 C7 C8 C9 -177.1(2) . . . . ?
C12 C7 C8 Al2 -166.8(2) . . . . ?
Al1 C7 C8 Al2 17.1(4) . . . . ?
C12 C7 C8 Al2 114.5(3) . . . 2 ?
Al1 C7 C8 Al2 -61.6(2) . . . 2 ?
C7 C8 C9 C10 0.4(5) . . . . ?
Al2 C8 C9 C10 167.5(3) . . . . ?
Al2 C8 C9 C10 -103.3(3) 2 . . . ?
C8 C9 C10 C11 1.1(5) . . . . ?
C9 C10 C11 C12 -2.0(5) . . . . ?
C10 C11 C12 C7 1.4(5) . . . . ?
C8 C7 C12 C11 0.1(5) . . . . ?
Al1 C7 C12 C11 175.8(3) . . . . ?

_refine_diff_density_max         0.706
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.119


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2AlMeBr32_wa3327
_database_code_depnum_ccdc_archive 'CCDC 2385632'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT077_2AlMeBr32_wa3327    
;
PROBLEM: Unitcell Contains Non-integer Number of Atoms ..     Please Check 
RESPONSE: The crystal is a solid solution of various forms resulting in
the crystallographic disorder
;
_vrf_PLAT155_2AlMeBr32_wa3327    
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !  
RESPONSE: The unit cell setting corresponds to the fully brominated
analog, C12 H8 Al4 Br8, to make easier a comparison of the structures.
;
_vrf_PLAT910_2AlMeBr32_wa3327    
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).          8 Note  
RESPONSE: These reflections are hidden by the beamstop.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13.90 H13.69 Al4 Br6.10'
_chemical_formula_sum            'C13.90 H13.69 Al4 Br6.10'
_chemical_formula_weight         776.11

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.1909(9)
_cell_length_b                   8.1869(9)
_cell_length_c                   9.8777(10)
_cell_angle_alpha                109.179(10)
_cell_angle_beta                 102.057(9)
_cell_angle_gamma                104.104(10)
_cell_volume                     575.79(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2332
_cell_measurement_theta_min      4.5670
_cell_measurement_theta_max      29.4400

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.238
_exptl_crystal_F_000             363
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    10.783
_shelx_estimated_absorpt_T_min   0.277
_shelx_estimated_absorpt_T_max   0.564
_exptl_absorpt_correction_T_min  0.21920
_exptl_absorpt_correction_T_max  0.24079
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            5874
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.066
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             2804
_reflns_number_gt                2211
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0357P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2804
_refine_ls_number_parameters     114
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0472
_refine_ls_wR_factor_ref         0.1077
_refine_ls_wR_factor_gt          0.0986
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Al1 Al 0.3628(2) 0.3020(2) 0.33817(17) 0.0263(3) Uani 1 1 d . . . . .
Al2 Al 0.3234(2) 0.4237(2) 0.70093(17) 0.0280(3) Uani 1 1 d . . . . .
Br1 Br 0.2385(3) 0.0671(2) 0.12826(19) 0.0434(6) Uani 0.266(3) 1 d . . P A 1
C1B C 0.2385(3) 0.0671(2) 0.12826(19) 0.0434(6) Uani 0.734(3) 1 d . . P A 2
H1BA H 0.299026 0.082899 0.055328 0.065 Uiso 0.734(3) 1 calc R U P A 2
H1BB H 0.113718 0.053994 0.089210 0.065 Uiso 0.734(3) 1 calc R U P A 2
H1BC H 0.245973 -0.043308 0.144104 0.065 Uiso 0.734(3) 1 calc R U P A 2
Br2 Br 0.11959(7) 0.31851(7) 0.45110(6) 0.03209(17) Uani 1 1 d . . . . .
Br3 Br 0.24199(8) 0.19402(8) 0.78067(7) 0.0383(2) Uani 0.956(3) 1 d . . P B 1
C3B C 0.24199(8) 0.19402(8) 0.78067(7) 0.0383(2) Uani 0.044(3) 1 d . . P B 2
H3BA H 0.193309 0.075314 0.693756 0.057 Uiso 0.044(3) 1 calc R U P B 2
H3BB H 0.151749 0.211594 0.829967 0.057 Uiso 0.044(3) 1 calc R U P B 2
H3BC H 0.345871 0.196269 0.852608 0.057 Uiso 0.044(3) 1 calc R U P B 2
Br4 Br 0.29532(11) 0.68494(10) 0.84339(8) 0.0426(3) Uani 0.830(3) 1 d . . P B 3
C4B C 0.29532(11) 0.68494(10) 0.84339(8) 0.0426(3) Uani 0.170(3) 1 d . . P B 4
H4BA H 0.391509 0.743971 0.939848 0.064 Uiso 0.170(3) 1 calc R U P B 4
H4BB H 0.180888 0.657561 0.862141 0.064 Uiso 0.170(3) 1 calc R U P B 4
H4BC H 0.301237 0.767720 0.790594 0.064 Uiso 0.170(3) 1 calc R U P B 4
C1 C 0.5606(6) 0.4352(6) 0.6638(5) 0.0233(9) Uani 1 1 d . . . . .
C2 C 0.5378(6) 0.3108(6) 0.5153(5) 0.0218(9) Uani 1 1 d . . . . .
C3 C 0.6457(7) 0.2019(7) 0.4997(6) 0.0281(11) Uani 1 1 d . . . . .
H3 H 0.633713 0.119179 0.401682 0.034 Uiso 1 1 calc R U . . .
C4 C 0.7684(7) 0.2115(7) 0.6226(7) 0.0336(12) Uani 1 1 d . . . . .
H4 H 0.835554 0.131254 0.607712 0.040 Uiso 1 1 calc R U . . .
C5 C 0.7974(7) 0.3335(7) 0.7666(6) 0.0342(12) Uani 1 1 d . . . . .
H5 H 0.888023 0.342596 0.849263 0.041 Uiso 1 1 calc R U . . .
C6 C 0.6919(7) 0.4435(7) 0.7893(6) 0.0298(11) Uani 1 1 d . . . . .
H6 H 0.706996 0.524603 0.888824 0.036 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C2 1.985(5) . ?
Al1 C1 2.097(4) 2_666 ?
Al1 C1B 2.140(2) . ?
Al1 Br1 2.140(2) . ?
Al1 Br2 2.4883(14) . ?
Al2 C1 2.037(4) . ?
Al2 C4B 2.2372(16) . ?
Al2 Br4 2.2372(16) . ?
Al2 Br3 2.2766(14) . ?
Al2 C3B 2.2766(14) . ?
Al2 Br2 2.4084(17) . ?
C1B H1BA 0.9800 . ?
C1B H1BB 0.9800 . ?
C1B H1BC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C4B H4BA 0.9800 . ?
C4B H4BB 0.9800 . ?
C4B H4BC 0.9800 . ?
C1 C2 1.427(6) . ?
C1 C6 1.432(7) . ?
C2 C3 1.396(5) . ?
C3 C4 1.371(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.373(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?

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
C2 Al1 C1 106.8(2) . 2_666 ?
C2 Al1 C1B 124.20(14) . . ?
C1 Al1 C1B 119.18(15) 2_666 . ?
C2 Al1 Br1 124.20(14) . . ?
C1 Al1 Br1 119.18(15) 2_666 . ?
C2 Al1 Br2 97.18(12) . . ?
C1 Al1 Br2 99.92(12) 2_666 . ?
C1B Al1 Br2 103.85(8) . . ?
Br1 Al1 Br2 103.85(8) . . ?
C1 Al2 C4B 118.07(14) . . ?
C1 Al2 Br4 118.07(14) . . ?
C1 Al2 Br3 108.57(12) . . ?
C1 Al2 C3B 108.57(12) . . ?
C1 Al2 Br2 103.29(14) . . ?
C4B Al2 Br2 107.32(6) . . ?
Br4 Al2 Br2 107.32(6) . . ?
Br3 Al2 Br2 105.73(7) . . ?
C3B Al2 Br2 105.73(7) . . ?
Al1 C1B H1BA 109.5 . . ?
Al1 C1B H1BB 109.5 . . ?
H1BA C1B H1BB 109.5 . . ?
Al1 C1B H1BC 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
Al2 Br2 Al1 91.14(5) . . ?
Al2 C3B H3BA 109.5 . . ?
Al2 C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
Al2 C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
Al2 C4B H4BA 109.5 . . ?
Al2 C4B H4BB 109.5 . . ?
H4BA C4B H4BB 109.5 . . ?
Al2 C4B H4BC 109.5 . . ?
H4BA C4B H4BC 109.5 . . ?
H4BB C4B H4BC 109.5 . . ?
C2 C1 C6 119.1(4) . . ?
C2 C1 Al2 111.6(3) . . ?
C6 C1 Al2 112.9(3) . . ?
C2 C1 Al1 105.6(3) . 2_666 ?
C6 C1 Al1 105.7(4) . 2_666 ?
Al2 C1 Al1 99.58(17) . 2_666 ?
C3 C2 C1 117.9(4) . . ?
C3 C2 Al1 122.0(3) . . ?
C1 C2 Al1 120.1(3) . . ?
C4 C3 C2 121.5(4) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 122.1(4) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C4 C5 C6 118.8(5) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C5 C6 C1 120.5(5) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?

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
C6 C1 C2 C3 0.1(6) . . . . ?
Al2 C1 C2 C3 -134.2(3) . . . . ?
Al1 C1 C2 C3 118.6(4) 2_666 . . . ?
C6 C1 C2 Al1 -177.9(3) . . . . ?
Al2 C1 C2 Al1 47.8(4) . . . . ?
Al1 C1 C2 Al1 -59.4(4) 2_666 . . . ?
C1 C2 C3 C4 0.8(7) . . . . ?
Al1 C2 C3 C4 178.8(4) . . . . ?
C2 C3 C4 C5 -2.8(7) . . . . ?
C3 C4 C5 C6 3.7(7) . . . . ?
C4 C5 C6 C1 -2.7(7) . . . . ?
C2 C1 C6 C5 0.8(7) . . . . ?
Al2 C1 C6 C5 134.6(4) . . . . ?
Al1 C1 C6 C5 -117.5(4) 2_666 . . . ?

_refine_diff_density_max         0.917
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.181


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1pyzthf_wa3538_PL402
_database_code_depnum_ccdc_archive 'CCDC 2385631'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
 (Al2 C22 H22 N4)0.333 (Al2 C22 H26 N2 O1)0.667
;
_chemical_formula_sum            'C22 H24.67 Al2 N2.67 O0.67'
_chemical_formula_weight         391.10

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   9.87648(19)
_cell_length_b                   14.3894(3)
_cell_length_c                   15.3682(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.960(2)
_cell_angle_gamma                90
_cell_volume                     2110.06(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16726
_cell_measurement_theta_min      2.6880
_cell_measurement_theta_max      30.4350

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_F_000             827
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.152
_shelx_estimated_absorpt_T_min   0.953
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_T_min  0.62841
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            49565
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.561
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4841
_reflns_number_gt                4455
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  'IUCr PublCIF online service'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0525P)²+3.1079P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4841
_refine_ls_number_parameters     265
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.1581
_refine_ls_wR_factor_gt          0.1552
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Al1 Al 0.73855(7) 0.37868(4) 0.26466(5) 0.02436(17) Uani 1 1 d . . . . .
C1 C 0.7960(3) 0.39935(19) 0.15175(17) 0.0354(5) Uani 1 1 d . . . . .
H1A H 0.745522 0.453035 0.119788 0.053 Uiso 1 1 calc R U . . .
H1B H 0.773857 0.344050 0.113486 0.053 Uiso 1 1 calc R U . . .
H1C H 0.897098 0.411173 0.166164 0.053 Uiso 1 1 calc R U . . .
N1 N 0.8072(2) 0.49775(14) 0.33339(14) 0.0351(5) Uani 1 1 d . . . . .
N2 N 0.8081(3) 0.49745(16) 0.42124(16) 0.0455(6) Uani 1 1 d . . . . .
C2N C 0.8586(4) 0.5719(2) 0.4696(2) 0.0618(10) Uani 1 1 d . . . . .
H2N H 0.860320 0.571934 0.531687 0.074 Uiso 1 1 calc R U . . .
C3N C 0.9094(4) 0.6501(2) 0.4349(3) 0.0726(13) Uani 1 1 d . . . . .
H3N H 0.947077 0.701321 0.472378 0.087 Uiso 1 1 calc R U . . .
C4N C 0.9032(4) 0.6506(2) 0.3463(3) 0.0690(12) Uani 1 1 d . . . . .
H4N H 0.933464 0.702994 0.318685 0.083 Uiso 1 1 calc R U . . .
C5N C 0.8507(3) 0.57123(19) 0.2963(2) 0.0503(8) Uani 1 1 d . . . . .
H5N H 0.846180 0.569996 0.233812 0.060 Uiso 1 1 calc R U . . .
C11 C 0.7775(2) 0.22326(15) 0.39811(14) 0.0233(4) Uani 1 1 d . . . . .
C12 C 0.8409(2) 0.27742(15) 0.34176(15) 0.0252(4) Uani 1 1 d . . . . .
C13 C 0.9777(2) 0.25397(19) 0.33823(19) 0.0375(6) Uani 1 1 d . . . . .
H13 H 1.020005 0.288675 0.299682 0.045 Uiso 1 1 calc R U . . .
C14 C 1.0538(3) 0.18192(19) 0.3889(2) 0.0395(6) Uani 1 1 d . . . . .
H14 H 1.146076 0.168237 0.384835 0.047 Uiso 1 1 calc R U . . .
C15 C 0.9940(2) 0.13081(16) 0.44498(16) 0.0304(5) Uani 1 1 d . . . . .
H15 H 1.045416 0.082508 0.481012 0.036 Uiso 1 1 calc R U . . .
C16 C 0.8578(2) 0.15049(15) 0.44841(15) 0.0265(4) Uani 1 1 d . . . . .
H16 H 0.816711 0.113590 0.486073 0.032 Uiso 1 1 calc R U . . .
C21 C 0.4719(2) 0.32656(18) 0.31163(18) 0.0333(5) Uani 1 1 d . . . . .
C22 C 0.5342(2) 0.37803(15) 0.25311(15) 0.0253(4) Uani 1 1 d . . . . .
C23 C 0.4469(3) 0.43074(17) 0.18423(17) 0.0335(5) Uani 1 1 d . . . . .
H23 H 0.488132 0.464085 0.144253 0.040 Uiso 1 1 calc R U . . .
C24 C 0.3031(3) 0.4362(2) 0.1720(2) 0.0510(8) Uani 1 1 d . . . . .
H24 H 0.247194 0.472690 0.124654 0.061 Uiso 1 1 calc R U . . .
C25 C 0.2430(3) 0.3883(3) 0.2294(3) 0.0738(13) Uani 1 1 d . . . . .
H25 H 0.144669 0.391812 0.222301 0.089 Uiso 1 1 calc R U . . .
C26 C 0.3260(3) 0.3341(3) 0.2984(3) 0.0617(10) Uani 1 1 d . . . . .
H26 H 0.282536 0.301340 0.337517 0.074 Uiso 1 1 calc R U . . .
Al2 Al 0.58159(7) 0.24133(5) 0.40534(5) 0.02900(19) Uani 1 1 d . . . . .
C2 C 0.4832(3) 0.1266(2) 0.4243(2) 0.0426(6) Uani 1 1 d . . . . .
H2A H 0.452322 0.092856 0.367269 0.064 Uiso 1 1 calc R U . . .
H2B H 0.401569 0.142751 0.446417 0.064 Uiso 1 1 calc R U . . .
H2C H 0.546947 0.087322 0.468788 0.064 Uiso 1 1 calc R U . . .
N1A N 0.7236(14) 0.3501(9) 0.5651(9) 0.077(4) Uiso 0.3333 1 d . . P A 1
N2A N 0.6134(12) 0.2944(7) 0.5266(6) 0.0289(19) Uiso 0.3333 1 d . . P A 1
C3A C 0.7208(13) 0.4100(10) 0.6377(9) 0.064(3) Uiso 0.3333 1 d . . P A 1
H3AA H 0.792779 0.454496 0.658974 0.076 Uiso 0.3333 1 calc R U P A 1
C4A C 0.6177(15) 0.4023(10) 0.6737(10) 0.074(3) Uiso 0.3333 1 d . . P A 1
H4A H 0.618820 0.434594 0.727799 0.089 Uiso 0.3333 1 calc R U P A 1
C5A C 0.4965(16) 0.3425(10) 0.6302(9) 0.077(3) Uiso 0.3333 1 d . . P A 1
H5AA H 0.422175 0.335721 0.658484 0.092 Uiso 0.3333 1 calc R U P A 1
C6A C 0.4887(11) 0.2998(8) 0.5561(7) 0.047(2) Uiso 0.3333 1 d . . P A 1
H6A H 0.403436 0.272882 0.522339 0.057 Uiso 0.3333 1 calc R U P A 1
O1B O 0.5824(8) 0.3061(7) 0.5100(5) 0.0304(18) Uiso 0.3333 1 d . . P A 2
C1B C 0.6699(13) 0.2826(8) 0.5974(7) 0.064(3) Uiso 0.3333 1 d D . P A 2
H1BA H 0.767539 0.273568 0.593390 0.077 Uiso 0.3333 1 calc R U P A 2
H1BB H 0.637280 0.223445 0.617927 0.077 Uiso 0.3333 1 calc R U P A 2
C2B C 0.6662(13) 0.3573(7) 0.6638(7) 0.056(3) Uiso 0.3333 1 d D . P A 2
H2BA H 0.753618 0.394335 0.677726 0.068 Uiso 0.3333 1 calc R U P A 2
H2BB H 0.652103 0.331113 0.720433 0.068 Uiso 0.3333 1 calc R U P A 2
C3B C 0.5416(11) 0.4151(8) 0.6151(6) 0.059(3) Uiso 0.3333 1 d D . P A 2
H3BA H 0.458110 0.398622 0.636248 0.071 Uiso 0.3333 1 calc R U P A 2
H3BB H 0.561663 0.482017 0.626902 0.071 Uiso 0.3333 1 calc R U P A 2
C4B C 0.5159(10) 0.3952(7) 0.5174(6) 0.049(2) Uiso 0.3333 1 d D . P A 2
H4BA H 0.414032 0.391902 0.488671 0.058 Uiso 0.3333 1 calc R U P A 2
H4BB H 0.557025 0.444685 0.487392 0.058 Uiso 0.3333 1 calc R U P A 2
O1C O 0.6138(10) 0.3226(6) 0.5192(6) 0.0331(18) Uiso 0.3333 1 d . . P A 3
C1C C 0.7415(10) 0.3226(7) 0.5854(6) 0.040(2) Uiso 0.3333 1 d D . P A 3
H1CA H 0.816075 0.352682 0.563051 0.048 Uiso 0.3333 1 calc R U P A 3
H1CB H 0.770909 0.258431 0.604824 0.048 Uiso 0.3333 1 calc R U P A 3
C2C C 0.7108(14) 0.3768(12) 0.6605(9) 0.071(4) Uiso 0.3333 1 d D . P A 3
H2CA H 0.756135 0.438562 0.664629 0.085 Uiso 0.3333 1 calc R U P A 3
H2CB H 0.747905 0.343835 0.718259 0.085 Uiso 0.3333 1 calc R U P A 3
C3C C 0.5546(13) 0.3878(11) 0.6421(8) 0.068(3) Uiso 0.3333 1 d D . P A 3
H3CA H 0.519393 0.357779 0.689998 0.081 Uiso 0.3333 1 calc R U P A 3
H3CB H 0.528194 0.454312 0.638691 0.081 Uiso 0.3333 1 calc R U P A 3
C4C C 0.4967(11) 0.3407(9) 0.5533(7) 0.053(2) Uiso 0.3333 1 d D . P A 3
H4CA H 0.448879 0.282096 0.561378 0.063 Uiso 0.3333 1 calc R U P A 3
H4CB H 0.429011 0.381600 0.511834 0.063 Uiso 0.3333 1 calc R U P A 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C22 1.980(2) . ?
Al1 C12 1.982(2) . ?
Al1 C1 1.982(3) . ?
Al1 N1 2.035(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
N1 C5N 1.325(3) . ?
N1 N2 1.348(3) . ?
N2 C2N 1.326(4) . ?
C2N C3N 1.393(5) . ?
C2N H2N 0.9500 . ?
C3N C4N 1.347(6) . ?
C3N H3N 0.9500 . ?
C4N C5N 1.399(4) . ?
C4N H4N 0.9500 . ?
C5N H5N 0.9500 . ?
C11 C16 1.416(3) . ?
C11 C12 1.424(3) . ?
C11 Al2 1.984(2) . ?
C12 C13 1.408(3) . ?
C13 C14 1.394(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.406(3) . ?
C21 C22 1.422(3) . ?
C21 Al2 1.987(3) . ?
C22 C23 1.403(3) . ?
C23 C24 1.386(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.370(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.398(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
Al2 O1B 1.857(7) . ?
Al2 N2A 1.963(9) . ?
Al2 C2 1.975(3) . ?
Al2 O1C 2.060(7) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
N1A N2A 1.359(18) . ?
N1A C3A 1.415(16) . ?
N2A C6A 1.419(14) . ?
C3A C4A 1.283(18) . ?
C3A H3AA 0.9500 . ?
C4A C5A 1.48(2) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.279(17) . ?
C5A H5AA 0.9500 . ?
C6A H6A 0.9500 . ?
O1B C1B 1.438(13) . ?
O1B C4B 1.458(13) . ?
C1B C2B 1.490(8) . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
C2B C3B 1.514(8) . ?
C2B H2BA 0.9900 . ?
C2B H2BB 0.9900 . ?
C3B C4B 1.486(6) . ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C4B H4BA 0.9900 . ?
C4B H4BB 0.9900 . ?
O1C C1C 1.401(14) . ?
O1C C4C 1.411(13) . ?
C1C C2C 1.487(8) . ?
C1C H1CA 0.9900 . ?
C1C H1CB 0.9900 . ?
C2C C3C 1.504(8) . ?
C2C H2CA 0.9900 . ?
C2C H2CB 0.9900 . ?
C3C C4C 1.499(8) . ?
C3C H3CA 0.9900 . ?
C3C H3CB 0.9900 . ?
C4C H4CA 0.9900 . ?
C4C H4CB 0.9900 . ?

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
C22 Al1 C12 113.62(9) . . ?
C22 Al1 C1 115.96(10) . . ?
C12 Al1 C1 114.61(11) . . ?
C22 Al1 N1 104.22(9) . . ?
C12 Al1 N1 104.98(9) . . ?
C1 Al1 N1 101.29(11) . . ?
Al1 C1 H1A 109.5 . . ?
Al1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Al1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C5N N1 N2 121.0(2) . . ?
C5N N1 Al1 123.4(2) . . ?
N2 N1 Al1 115.62(16) . . ?
C2N N2 N1 117.6(3) . . ?
N2 C2N C3N 124.0(3) . . ?
N2 C2N H2N 118.0 . . ?
C3N C2N H2N 118.0 . . ?
C4N C3N C2N 117.7(3) . . ?
C4N C3N H3N 121.2 . . ?
C2N C3N H3N 121.2 . . ?
C3N C4N C5N 117.7(3) . . ?
C3N C4N H4N 121.2 . . ?
C5N C4N H4N 121.2 . . ?
N1 C5N C4N 122.1(3) . . ?
N1 C5N H5N 119.0 . . ?
C4N C5N H5N 119.0 . . ?
C16 C11 C12 117.7(2) . . ?
C16 C11 Al2 118.87(16) . . ?
C12 C11 Al2 123.38(16) . . ?
C13 C12 C11 118.0(2) . . ?
C13 C12 Al1 119.97(17) . . ?
C11 C12 Al1 121.98(16) . . ?
C14 C13 C12 122.8(2) . . ?
C14 C13 H13 118.6 . . ?
C12 C13 H13 118.6 . . ?
C15 C14 C13 119.4(2) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 119.4(2) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C15 C16 C11 122.7(2) . . ?
C15 C16 H16 118.6 . . ?
C11 C16 H16 118.6 . . ?
C26 C21 C22 117.5(2) . . ?
C26 C21 Al2 120.0(2) . . ?
C22 C21 Al2 122.41(17) . . ?
C23 C22 C21 118.5(2) . . ?
C23 C22 Al1 118.59(17) . . ?
C21 C22 Al1 122.90(17) . . ?
C24 C23 C22 122.8(2) . . ?
C24 C23 H23 118.6 . . ?
C22 C23 H23 118.6 . . ?
C25 C24 C23 118.9(3) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C24 C25 C26 120.1(3) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C21 122.1(3) . . ?
C25 C26 H26 118.9 . . ?
C21 C26 H26 118.9 . . ?
O1B Al2 C2 100.6(3) . . ?
N2A Al2 C2 98.6(3) . . ?
O1B Al2 C11 109.2(2) . . ?
N2A Al2 C11 100.7(3) . . ?
C2 Al2 C11 115.02(11) . . ?
O1B Al2 C21 101.4(3) . . ?
N2A Al2 C21 111.8(3) . . ?
C2 Al2 C21 115.22(11) . . ?
C11 Al2 C21 113.44(10) . . ?
C2 Al2 O1C 108.8(2) . . ?
C11 Al2 O1C 100.5(3) . . ?
C21 Al2 O1C 101.6(3) . . ?
Al2 C2 H2A 109.5 . . ?
Al2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Al2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2A N1A C3A 121.7(11) . . ?
N1A N2A C6A 119.5(9) . . ?
N1A N2A Al2 123.8(8) . . ?
C6A N2A Al2 112.6(8) . . ?
C4A C3A N1A 117.8(14) . . ?
C4A C3A H3AA 121.1 . . ?
N1A C3A H3AA 121.1 . . ?
C3A C4A C5A 119.5(14) . . ?
C3A C4A H4A 120.2 . . ?
C5A C4A H4A 120.2 . . ?
C6A C5A C4A 122.4(13) . . ?
C6A C5A H5AA 118.8 . . ?
C4A C5A H5AA 118.8 . . ?
C5A C6A N2A 116.9(11) . . ?
C5A C6A H6A 121.6 . . ?
N2A C6A H6A 121.6 . . ?
C1B O1B C4B 108.0(7) . . ?
C1B O1B Al2 123.9(7) . . ?
C4B O1B Al2 127.4(7) . . ?
O1B C1B C2B 110.8(9) . . ?
O1B C1B H1BA 109.5 . . ?
C2B C1B H1BA 109.5 . . ?
O1B C1B H1BB 109.5 . . ?
C2B C1B H1BB 109.5 . . ?
H1BA C1B H1BB 108.1 . . ?
C1B C2B C3B 102.6(9) . . ?
C1B C2B H2BA 111.2 . . ?
C3B C2B H2BA 111.2 . . ?
C1B C2B H2BB 111.2 . . ?
C3B C2B H2BB 111.2 . . ?
H2BA C2B H2BB 109.2 . . ?
C4B C3B C2B 107.4(8) . . ?
C4B C3B H3BA 110.2 . . ?
C2B C3B H3BA 110.2 . . ?
C4B C3B H3BB 110.2 . . ?
C2B C3B H3BB 110.2 . . ?
H3BA C3B H3BB 108.5 . . ?
O1B C4B C3B 106.6(8) . . ?
O1B C4B H4BA 110.4 . . ?
C3B C4B H4BA 110.4 . . ?
O1B C4B H4BB 110.4 . . ?
C3B C4B H4BB 110.4 . . ?
H4BA C4B H4BB 108.6 . . ?
C1C O1C C4C 113.6(8) . . ?
C1C O1C Al2 122.0(6) . . ?
C4C O1C Al2 117.3(7) . . ?
O1C C1C C2C 103.8(8) . . ?
O1C C1C H1CA 111.0 . . ?
C2C C1C H1CA 111.0 . . ?
O1C C1C H1CB 111.0 . . ?
C2C C1C H1CB 111.0 . . ?
H1CA C1C H1CB 109.0 . . ?
C1C C2C C3C 108.3(10) . . ?
C1C C2C H2CA 110.0 . . ?
C3C C2C H2CA 110.0 . . ?
C1C C2C H2CB 110.0 . . ?
C3C C2C H2CB 110.0 . . ?
H2CA C2C H2CB 108.4 . . ?
C4C C3C C2C 104.7(9) . . ?
C4C C3C H3CA 110.8 . . ?
C2C C3C H3CA 110.8 . . ?
C4C C3C H3CB 110.8 . . ?
C2C C3C H3CB 110.8 . . ?
H3CA C3C H3CB 108.9 . . ?
O1C C4C C3C 105.4(9) . . ?
O1C C4C H4CA 110.7 . . ?
C3C C4C H4CA 110.7 . . ?
O1C C4C H4CB 110.7 . . ?
C3C C4C H4CB 110.7 . . ?
H4CA C4C H4CB 108.8 . . ?

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
C5N N1 N2 C2N -2.3(4) . . . . ?
Al1 N1 N2 C2N 176.7(2) . . . . ?
N1 N2 C2N C3N 0.5(5) . . . . ?
N2 C2N C3N C4N 1.7(6) . . . . ?
C2N C3N C4N C5N -2.1(6) . . . . ?
N2 N1 C5N C4N 1.9(5) . . . . ?
Al1 N1 C5N C4N -177.1(3) . . . . ?
C3N C4N C5N N1 0.5(6) . . . . ?
C16 C11 C12 C13 1.3(3) . . . . ?
Al2 C11 C12 C13 -176.01(18) . . . . ?
C16 C11 C12 Al1 177.95(15) . . . . ?
Al2 C11 C12 Al1 0.6(3) . . . . ?
C11 C12 C13 C14 -1.6(4) . . . . ?
Al1 C12 C13 C14 -178.3(2) . . . . ?
C12 C13 C14 C15 0.1(4) . . . . ?
C13 C14 C15 C16 1.5(4) . . . . ?
C14 C15 C16 C11 -1.8(4) . . . . ?
C12 C11 C16 C15 0.3(3) . . . . ?
Al2 C11 C16 C15 177.74(17) . . . . ?
C26 C21 C22 C23 -1.9(4) . . . . ?
Al2 C21 C22 C23 174.94(18) . . . . ?
C26 C21 C22 Al1 178.0(2) . . . . ?
Al2 C21 C22 Al1 -5.1(3) . . . . ?
C21 C22 C23 C24 1.4(4) . . . . ?
Al1 C22 C23 C24 -178.6(2) . . . . ?
C22 C23 C24 C25 -0.1(5) . . . . ?
C23 C24 C25 C26 -0.6(6) . . . . ?
C24 C25 C26 C21 0.0(7) . . . . ?
C22 C21 C26 C25 1.3(6) . . . . ?
Al2 C21 C26 C25 -175.6(3) . . . . ?
C3A N1A N2A C6A 3.6(18) . . . . ?
C3A N1A N2A Al2 159.4(10) . . . . ?
N2A N1A C3A C4A 8(2) . . . . ?
N1A C3A C4A C5A -9(2) . . . . ?
C3A C4A C5A C6A -2(2) . . . . ?
C4A C5A C6A N2A 13.8(19) . . . . ?
N1A N2A C6A C5A -14.4(17) . . . . ?
Al2 N2A C6A C5A -172.7(10) . . . . ?
C2 Al2 O1B C1B 73.1(9) . . . . ?
C11 Al2 O1B C1B -48.3(10) . . . . ?
C21 Al2 O1B C1B -168.2(9) . . . . ?
C2 Al2 O1B C4B -117.7(8) . . . . ?
C11 Al2 O1B C4B 120.9(8) . . . . ?
C21 Al2 O1B C4B 0.9(8) . . . . ?
C4B O1B C1B C2B -1.7(13) . . . . ?
Al2 O1B C1B C2B 169.3(8) . . . . ?
O1B C1B C2B C3B 14.0(14) . . . . ?
C1B C2B C3B C4B -20.9(13) . . . . ?
C1B O1B C4B C3B -11.9(11) . . . . ?
Al2 O1B C4B C3B 177.6(7) . . . . ?
C2B C3B C4B O1B 20.8(12) . . . . ?
C4C O1C C1C C2C -21.1(14) . . . . ?
Al2 O1C C1C C2C -170.7(9) . . . . ?
O1C C1C C2C C3C 13.0(16) . . . . ?
C1C C2C C3C C4C -1.5(18) . . . . ?
C1C O1C C4C C3C 20.5(14) . . . . ?
Al2 O1C C4C C3C 171.6(9) . . . . ?
C2C C3C C4C O1C -10.5(16) . . . . ?

_refine_diff_density_max         0.569
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.063


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2OEt22_wa3310
_database_code_depnum_ccdc_archive 'CCDC 2385640'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H28 Al2 Br2 O2'
_chemical_formula_weight         514.20

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.694(3)
_cell_length_b                   7.0404(6)
_cell_length_c                   19.080(4)
_cell_angle_alpha                90
_cell_angle_beta                 120.073(18)
_cell_angle_gamma                90
_cell_volume                     2289.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    2361
_cell_measurement_theta_min      4.3500
_cell_measurement_theta_max      26.3180

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_F_000             1040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    3.629
_shelx_estimated_absorpt_T_min   0.516
_shelx_estimated_absorpt_T_max   0.760
_exptl_absorpt_correction_T_min  0.25299
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            6600
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.140
_diffrn_reflns_theta_max         26.384
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             2323
_reflns_number_gt                1690
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0474P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2323
_refine_ls_number_parameters     121
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_ref         0.0984
_refine_ls_wR_factor_gt          0.0956
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Br1 Br 0.39530(3) 0.34972(7) 0.51762(3) 0.02059(16) Uani 1 1 d . . . . .
Al1 Al 0.45390(8) 0.47934(19) 0.64771(8) 0.0127(3) Uani 1 1 d . . . . .
O1 O 0.44213(18) 0.7424(4) 0.62513(18) 0.0164(7) Uani 1 1 d . . . . .
C1 C 0.5677(3) 0.4328(6) 0.7110(3) 0.0134(10) Uani 1 1 d . . . . .
C2 C 0.6050(3) 0.4278(6) 0.7967(3) 0.0152(10) Uani 1 1 d . . . . .
C3 C 0.6859(3) 0.3807(7) 0.8407(3) 0.0219(11) Uani 1 1 d . . . . .
H3 H 0.711434 0.372971 0.898051 0.026 Uiso 1 1 calc R U . . .
C4 C 0.7287(3) 0.3460(8) 0.8029(3) 0.0259(11) Uani 1 1 d . . . . .
H4 H 0.782890 0.315638 0.834312 0.031 Uiso 1 1 calc R U . . .
C5 C 0.6930(3) 0.3550(8) 0.7194(3) 0.0248(11) Uani 1 1 d . . . . .
H5 H 0.722450 0.332866 0.693119 0.030 Uiso 1 1 calc R U . . .
C6 C 0.6135(3) 0.3971(6) 0.6747(3) 0.0202(11) Uani 1 1 d . . . . .
H6 H 0.589067 0.401914 0.617327 0.024 Uiso 1 1 calc R U . . .
C7 C 0.4714(3) 0.8300(8) 0.5753(3) 0.0272(12) Uani 1 1 d . . . . .
H7A H 0.433345 0.926406 0.539136 0.033 Uiso 1 1 calc R U . . .
H7B H 0.476094 0.731489 0.540881 0.033 Uiso 1 1 calc R U . . .
C8 C 0.5494(3) 0.9219(8) 0.6264(3) 0.0301(13) Uani 1 1 d . . . . .
H8A H 0.566854 0.980286 0.591540 0.045 Uiso 1 1 calc R U . . .
H8B H 0.587630 0.825923 0.660991 0.045 Uiso 1 1 calc R U . . .
H8C H 0.544899 1.019733 0.660425 0.045 Uiso 1 1 calc R U . . .
C9 C 0.4024(3) 0.8747(7) 0.6522(3) 0.0250(12) Uani 1 1 d . . . . .
H9A H 0.427753 1.000922 0.662083 0.030 Uiso 1 1 calc R U . . .
H9B H 0.408176 0.828889 0.703978 0.030 Uiso 1 1 calc R U . . .
C10 C 0.3172(3) 0.8939(8) 0.5912(4) 0.0357(14) Uani 1 1 d . . . . .
H10A H 0.311254 0.945081 0.540662 0.054 Uiso 1 1 calc R U . . .
H10B H 0.292414 0.980330 0.612050 0.054 Uiso 1 1 calc R U . . .
H10C H 0.291978 0.769053 0.580888 0.054 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Br1 Al1 2.3355(14) . ?
Al1 O1 1.890(3) . ?
Al1 C2 1.958(5) 2_656 ?
Al1 C1 1.968(5) . ?
O1 C9 1.467(6) . ?
O1 C7 1.473(6) . ?
C1 C6 1.408(7) . ?
C1 C2 1.419(6) . ?
C2 C3 1.420(6) . ?
C3 C4 1.378(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.492(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.494(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

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 C2 105.48(18) . 2_656 ?
O1 Al1 C1 105.95(17) . . ?
C2 Al1 C1 115.99(19) 2_656 . ?
O1 Al1 Br1 101.65(11) . . ?
C2 Al1 Br1 113.08(15) 2_656 . ?
C1 Al1 Br1 113.02(15) . . ?
C9 O1 C7 114.4(4) . . ?
C9 O1 Al1 124.6(3) . . ?
C7 O1 Al1 121.0(3) . . ?
C6 C1 C2 118.3(4) . . ?
C6 C1 Al1 122.8(3) . . ?
C2 C1 Al1 118.9(3) . . ?
C1 C2 C3 117.8(4) . . ?
C1 C2 Al1 121.0(3) . 2_656 ?
C3 C2 Al1 121.2(3) . 2_656 ?
C4 C3 C2 122.2(4) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C4 C5 120.2(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 118.9(5) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C5 C6 C1 122.6(4) . . ?
C5 C6 H6 118.7 . . ?
C1 C6 H6 118.7 . . ?
O1 C7 C8 111.5(4) . . ?
O1 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
O1 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 C9 C10 111.9(4) . . ?
O1 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
O1 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

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
C2 Al1 O1 C9 5.0(4) 2_656 . . . ?
C1 Al1 O1 C9 -118.5(4) . . . . ?
Br1 Al1 O1 C9 123.2(3) . . . . ?
C2 Al1 O1 C7 -173.2(3) 2_656 . . . ?
C1 Al1 O1 C7 63.3(4) . . . . ?
Br1 Al1 O1 C7 -55.0(3) . . . . ?
C6 C1 C2 C3 -2.0(7) . . . . ?
Al1 C1 C2 C3 175.6(3) . . . . ?
C6 C1 C2 Al1 179.1(3) . . . 2_656 ?
Al1 C1 C2 Al1 -3.2(5) . . . 2_656 ?
C1 C2 C3 C4 1.9(7) . . . . ?
Al1 C2 C3 C4 -179.3(4) 2_656 . . . ?
C2 C3 C4 C5 -0.4(8) . . . . ?
C3 C4 C5 C6 -0.9(8) . . . . ?
C4 C5 C6 C1 0.6(8) . . . . ?
C2 C1 C6 C5 0.8(7) . . . . ?
Al1 C1 C6 C5 -176.7(4) . . . . ?
C9 O1 C7 C8 83.1(5) . . . . ?
Al1 O1 C7 C8 -98.6(4) . . . . ?
C7 O1 C9 C10 87.0(5) . . . . ?
Al1 O1 C9 C10 -91.2(5) . . . . ?

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
C7 H7A Br1 0.99 3.05 3.898(5) 144.4 1_565 yes
C7 H7B Br1 0.99 3.04 3.639(5) 120.1 . yes

_refine_diff_density_max         1.592
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.113


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2thf2_wa3381
_database_code_depnum_ccdc_archive 'CCDC 2385636'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT910_2thf2_wa3381        
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         11 Note  
RESPONSE: These reflections are hidden by the beamstop.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H24 Al2 Br2 O2'
_chemical_formula_sum            'C20 H24 Al2 Br2 O2'
_chemical_formula_weight         510.17

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   9.5845(4)
_cell_length_b                   13.7779(5)
_cell_length_c                   16.7652(6)
_cell_angle_alpha                90
_cell_angle_beta                 106.151(4)
_cell_angle_gamma                90
_cell_volume                     2126.54(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7114
_cell_measurement_theta_min      3.7540
_cell_measurement_theta_max      26.2760

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_F_000             1024
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.906
_shelx_estimated_absorpt_T_min   0.419
_shelx_estimated_absorpt_T_max   0.696
_exptl_absorpt_correction_T_min  0.53453
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            31664
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.694
_diffrn_reflns_theta_max         26.383
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4322
_reflns_number_gt                3674
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'IUCr PublCIF online service'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0116P)²+2.5684P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4322
_refine_ls_number_parameters     235
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0651
_refine_ls_wR_factor_gt          0.0619
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Al1 Al 0.35019(9) 0.95052(6) 0.52351(5) 0.01957(17) Uani 1 1 d . . . . .
Br1 Br 0.22849(4) 0.96817(2) 0.62574(2) 0.03705(9) Uani 1 1 d . . . . .
O1 O 0.2329(2) 0.85552(14) 0.45555(11) 0.0284(4) Uani 1 1 d . . . . .
C21 C 0.5437(3) 0.89206(18) 0.56601(15) 0.0202(5) Uani 1 1 d . . . . .
C22 C 0.5644(3) 0.8064(2) 0.61351(16) 0.0259(6) Uani 1 1 d . . . . .
H22 H 0.484660 0.780302 0.629719 0.031 Uiso 1 1 calc R U . . .
C23 C 0.6965(3) 0.7586(2) 0.63749(18) 0.0312(7) Uani 1 1 d . . . . .
H23 H 0.705859 0.699957 0.668273 0.037 Uiso 1 1 calc R U . . .
C24 C 0.8144(3) 0.7968(2) 0.61640(19) 0.0332(7) Uani 1 1 d . . . . .
H24 H 0.905320 0.764335 0.632450 0.040 Uiso 1 1 calc R U . . .
C25 C 0.8000(3) 0.8830(2) 0.57162(18) 0.0278(6) Uani 1 1 d . . . . .
H25 H 0.882661 0.909431 0.558744 0.033 Uiso 1 1 calc R U . . .
C26 C 0.6662(3) 0.93214(19) 0.54483(16) 0.0213(6) Uani 1 1 d . . . . .
C27 C 0.1446(3) 0.8685(2) 0.36880(17) 0.0307(7) Uani 1 1 d . . . . .
H27A H 0.206448 0.885275 0.332351 0.037 Uiso 1 1 calc R U . . .
H27B H 0.071136 0.920231 0.364663 0.037 Uiso 1 1 calc R U . . .
C28 C 0.0733(4) 0.7715(2) 0.3460(2) 0.0387(8) Uani 1 1 d . . . . .
H28A H 0.137073 0.726780 0.326019 0.046 Uiso 1 1 calc R U . . .
H28B H -0.020348 0.778125 0.302608 0.046 Uiso 1 1 calc R U . . .
C29 C 0.0505(4) 0.7363(2) 0.4271(2) 0.0389(8) Uani 1 1 d . . . . .
H29A H -0.032505 0.769728 0.439563 0.047 Uiso 1 1 calc R U . . .
H29B H 0.034199 0.665323 0.426283 0.047 Uiso 1 1 calc R U . . .
C30 C 0.1922(4) 0.7636(2) 0.4885(2) 0.0383(8) Uani 1 1 d . . . . .
H30A H 0.179746 0.772997 0.544696 0.046 Uiso 1 1 calc R U . . .
H30B H 0.266780 0.713016 0.491241 0.046 Uiso 1 1 calc R U . . .
Al2 Al 0.58776(9) 0.51988(6) 0.42448(5) 0.01924(17) Uani 1 1 d . . . . .
Br2 Br 0.67782(3) 0.41558(2) 0.34108(2) 0.03109(9) Uani 1 1 d . . . . .
O2 O 0.6282(2) 0.64038(13) 0.38313(11) 0.0248(4) Uani 1 1 d . . . . .
C11 C 0.6971(3) 0.51314(19) 0.54207(16) 0.0211(5) Uani 1 1 d . . . . .
C12 C 0.6244(3) 0.48926(19) 0.60296(16) 0.0209(5) Uani 1 1 d . . . . .
C13 C 0.7082(3) 0.4780(2) 0.68573(17) 0.0285(6) Uani 1 1 d . . . . .
H13 H 0.660675 0.460916 0.726494 0.034 Uiso 1 1 calc R U . . .
C14 C 0.8573(3) 0.4908(2) 0.71007(18) 0.0314(7) Uani 1 1 d . . . . .
H14 H 0.910915 0.481345 0.766380 0.038 Uiso 1 1 calc R U . . .
C15 C 0.9273(3) 0.5173(2) 0.6517(2) 0.0348(7) Uani 1 1 d . . . . .
H15 H 1.029128 0.528676 0.668080 0.042 Uiso 1 1 calc R U . . .
C16 C 0.8482(3) 0.5275(2) 0.56873(19) 0.0294(6) Uani 1 1 d . . . . .
H16 H 0.897822 0.544591 0.528991 0.035 Uiso 1 1 calc R U . . .
C17 C 0.5659(4) 0.7270(2) 0.41191(19) 0.0343(7) Uani 1 1 d . . . . .
H17A H 0.638414 0.759029 0.458219 0.041 Uiso 1 1 calc R U . . .
H17B H 0.479813 0.709659 0.430628 0.041 Uiso 1 1 calc R U . . .
C18 C 0.5241(3) 0.7917(2) 0.33716(19) 0.0352(7) Uani 1 1 d . . . . .
H18A H 0.524348 0.860882 0.353288 0.042 Uiso 1 1 calc R U . . .
H18B H 0.427142 0.774631 0.300456 0.042 Uiso 1 1 calc R U . . .
C19 C 0.6423(4) 0.7708(2) 0.2959(2) 0.0354(7) Uani 1 1 d . . . . .
H19A H 0.612179 0.790488 0.236762 0.042 Uiso 1 1 calc R U . . .
H19B H 0.733287 0.805082 0.324443 0.042 Uiso 1 1 calc R U . . .
C20 C 0.6615(3) 0.6625(2) 0.30431(18) 0.0306(7) Uani 1 1 d . . . . .
H20A H 0.593619 0.628443 0.257235 0.037 Uiso 1 1 calc R U . . .
H20B H 0.762243 0.643443 0.306832 0.037 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 1.887(2) . ?
Al1 C26 1.963(3) 3_676 ?
Al1 C21 1.965(3) . ?
Al1 Br1 2.3386(8) . ?
O1 C27 1.476(3) . ?
O1 C30 1.477(3) . ?
C21 C22 1.407(4) . ?
C21 C26 1.429(4) . ?
C22 C23 1.383(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.379(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.409(4) . ?
C25 H25 0.9500 . ?
C27 C28 1.501(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.516(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.506(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
Al2 O2 1.8806(19) . ?
Al2 C12 1.960(3) 3_666 ?
Al2 C11 1.961(3) . ?
Al2 Br2 2.3317(8) . ?
O2 C20 1.475(3) . ?
O2 C17 1.475(3) . ?
C11 C16 1.405(4) . ?
C11 C12 1.425(3) . ?
C12 C13 1.405(4) . ?
C13 C14 1.384(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.394(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.499(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.510(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.506(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?

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 C26 106.34(10) . 3_676 ?
O1 Al1 C21 106.14(10) . . ?
C26 Al1 C21 117.62(11) 3_676 . ?
O1 Al1 Br1 100.36(7) . . ?
C26 Al1 Br1 111.54(8) 3_676 . ?
C21 Al1 Br1 112.93(8) . . ?
C27 O1 C30 109.5(2) . . ?
C27 O1 Al1 126.34(16) . . ?
C30 O1 Al1 122.92(17) . . ?
C22 C21 C26 117.9(2) . . ?
C22 C21 Al1 121.3(2) . . ?
C26 C21 Al1 120.63(19) . . ?
C23 C22 C21 122.5(3) . . ?
C23 C22 H22 118.8 . . ?
C21 C22 H22 118.8 . . ?
C24 C23 C22 119.5(3) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 119.9(3) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C26 121.8(3) . . ?
C24 C25 H25 119.1 . . ?
C26 C25 H25 119.1 . . ?
C25 C26 C21 118.2(2) . . ?
C25 C26 Al1 120.0(2) . 3_676 ?
C21 C26 Al1 121.71(19) . 3_676 ?
O1 C27 C28 103.8(2) . . ?
O1 C27 H27A 111.0 . . ?
C28 C27 H27A 111.0 . . ?
O1 C27 H27B 111.0 . . ?
C28 C27 H27B 111.0 . . ?
H27A C27 H27B 109.0 . . ?
C27 C28 C29 103.0(2) . . ?
C27 C28 H28A 111.2 . . ?
C29 C28 H28A 111.2 . . ?
C27 C28 H28B 111.2 . . ?
C29 C28 H28B 111.2 . . ?
H28A C28 H28B 109.1 . . ?
C30 C29 C28 101.9(3) . . ?
C30 C29 H29A 111.4 . . ?
C28 C29 H29A 111.4 . . ?
C30 C29 H29B 111.4 . . ?
C28 C29 H29B 111.4 . . ?
H29A C29 H29B 109.3 . . ?
O1 C30 C29 103.9(2) . . ?
O1 C30 H30A 111.0 . . ?
C29 C30 H30A 111.0 . . ?
O1 C30 H30B 111.0 . . ?
C29 C30 H30B 111.0 . . ?
H30A C30 H30B 109.0 . . ?
O2 Al2 C12 106.08(10) . 3_666 ?
O2 Al2 C11 107.77(10) . . ?
C12 Al2 C11 117.54(11) 3_666 . ?
O2 Al2 Br2 100.04(6) . . ?
C12 Al2 Br2 110.64(8) 3_666 . ?
C11 Al2 Br2 112.98(8) . . ?
C20 O2 C17 109.5(2) . . ?
C20 O2 Al2 129.09(16) . . ?
C17 O2 Al2 116.76(16) . . ?
C16 C11 C12 118.1(2) . . ?
C16 C11 Al2 121.9(2) . . ?
C12 C11 Al2 120.01(19) . . ?
C13 C12 C11 118.3(2) . . ?
C13 C12 Al2 119.7(2) . 3_666 ?
C11 C12 Al2 121.91(19) . 3_666 ?
C14 C13 C12 122.4(3) . . ?
C14 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
C15 C14 C13 119.4(3) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 119.8(3) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C11 122.0(3) . . ?
C15 C16 H16 119.0 . . ?
C11 C16 H16 119.0 . . ?
O2 C17 C18 104.2(2) . . ?
O2 C17 H17A 110.9 . . ?
C18 C17 H17A 110.9 . . ?
O2 C17 H17B 110.9 . . ?
C18 C17 H17B 110.9 . . ?
H17A C17 H17B 108.9 . . ?
C17 C18 C19 102.1(2) . . ?
C17 C18 H18A 111.3 . . ?
C19 C18 H18A 111.3 . . ?
C17 C18 H18B 111.3 . . ?
C19 C18 H18B 111.3 . . ?
H18A C18 H18B 109.2 . . ?
C20 C19 C18 103.5(2) . . ?
C20 C19 H19A 111.1 . . ?
C18 C19 H19A 111.1 . . ?
C20 C19 H19B 111.1 . . ?
C18 C19 H19B 111.1 . . ?
H19A C19 H19B 109.0 . . ?
O2 C20 C19 103.7(2) . . ?
O2 C20 H20A 111.0 . . ?
C19 C20 H20A 111.0 . . ?
O2 C20 H20B 111.0 . . ?
C19 C20 H20B 111.0 . . ?
H20A C20 H20B 109.0 . . ?

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
C26 Al1 O1 C27 -1.2(2) 3_676 . . . ?
C21 Al1 O1 C27 -127.2(2) . . . . ?
Br1 Al1 O1 C27 115.1(2) . . . . ?
C26 Al1 O1 C30 -167.2(2) 3_676 . . . ?
C21 Al1 O1 C30 66.8(2) . . . . ?
Br1 Al1 O1 C30 -50.9(2) . . . . ?
C26 C21 C22 C23 -2.3(4) . . . . ?
Al1 C21 C22 C23 173.7(2) . . . . ?
C21 C22 C23 C24 1.7(4) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
C23 C24 C25 C26 -1.6(4) . . . . ?
C24 C25 C26 C21 1.0(4) . . . . ?
C24 C25 C26 Al1 -176.6(2) . . . 3_676 ?
C22 C21 C26 C25 0.9(4) . . . . ?
Al1 C21 C26 C25 -175.1(2) . . . . ?
C22 C21 C26 Al1 178.41(19) . . . 3_676 ?
Al1 C21 C26 Al1 2.4(3) . . . 3_676 ?
C30 O1 C27 C28 -11.7(3) . . . . ?
Al1 O1 C27 C28 -179.3(2) . . . . ?
O1 C27 C28 C29 33.4(3) . . . . ?
C27 C28 C29 C30 -42.5(3) . . . . ?
C27 O1 C30 C29 -14.9(3) . . . . ?
Al1 O1 C30 C29 153.2(2) . . . . ?
C28 C29 C30 O1 35.0(3) . . . . ?
C12 Al2 O2 C20 -97.5(2) 3_666 . . . ?
C11 Al2 O2 C20 135.8(2) . . . . ?
Br2 Al2 O2 C20 17.6(2) . . . . ?
C12 Al2 O2 C17 55.7(2) 3_666 . . . ?
C11 Al2 O2 C17 -71.0(2) . . . . ?
Br2 Al2 O2 C17 170.72(18) . . . . ?
C16 C11 C12 C13 -2.2(4) . . . . ?
Al2 C11 C12 C13 175.3(2) . . . . ?
C16 C11 C12 Al2 173.9(2) . . . 3_666 ?
Al2 C11 C12 Al2 -8.7(3) . . . 3_666 ?
C11 C12 C13 C14 1.1(4) . . . . ?
Al2 C12 C13 C14 -175.1(2) 3_666 . . . ?
C12 C13 C14 C15 1.2(4) . . . . ?
C13 C14 C15 C16 -2.3(4) . . . . ?
C14 C15 C16 C11 1.2(5) . . . . ?
C12 C11 C16 C15 1.1(4) . . . . ?
Al2 C11 C16 C15 -176.3(2) . . . . ?
C20 O2 C17 C18 15.5(3) . . . . ?
Al2 O2 C17 C18 -142.7(2) . . . . ?
O2 C17 C18 C19 -34.6(3) . . . . ?
C17 C18 C19 C20 41.3(3) . . . . ?
C17 O2 C20 C19 10.2(3) . . . . ?
Al2 O2 C20 C19 164.84(19) . . . . ?
C18 C19 C20 O2 -31.7(3) . . . . ?

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
C28 H28B Br2 0.99 3.11 3.920(3) 140.5 2 yes
C30 H30A Br1 0.99 2.99 3.593(3) 120.3 . yes

_refine_diff_density_max         0.499
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.072


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_beta-2AlBr32_wa3282
_database_code_depnum_ccdc_archive 'CCDC 2385634'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 Al4 Br8'
_chemical_formula_sum            'C12 H8 Al4 Br8'
_chemical_formula_weight         899.38

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.0710(5)
_cell_length_b                   8.2992(6)
_cell_length_c                   9.8658(7)
_cell_angle_alpha                108.901(7)
_cell_angle_beta                 101.510(6)
_cell_angle_gamma                103.983(6)
_cell_volume                     578.23(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3283
_cell_measurement_theta_min      4.5570
_cell_measurement_theta_max      27.0390

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.583
_exptl_crystal_F_000             412
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    14.018
_shelx_estimated_absorpt_T_min   0.244
_shelx_estimated_absorpt_T_max   0.604
_exptl_absorpt_correction_T_min  0.14492
_exptl_absorpt_correction_T_max  0.16647
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            6330
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.055
_diffrn_reflns_theta_max         27.124
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             2534
_reflns_number_gt                2281
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0415P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2534
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0867
_refine_ls_wR_factor_gt          0.0827
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Al1 Al 0.36452(16) 0.31116(14) 0.34448(13) 0.0216(2) Uani 1 1 d . . . . .
Al2 Al 0.32011(16) 0.41799(15) 0.70219(14) 0.0230(3) Uani 1 1 d . . . . .
Br1 Br 0.24121(7) 0.06908(6) 0.12741(5) 0.03751(14) Uani 1 1 d . . . . .
Br2 Br 0.11813(5) 0.32143(5) 0.45363(5) 0.02894(13) Uani 1 1 d . . . . .
Br3 Br 0.24190(6) 0.18838(6) 0.77853(6) 0.03517(14) Uani 1 1 d . . . . .
Br4 Br 0.28343(7) 0.67315(6) 0.84483(6) 0.03853(14) Uani 1 1 d . . . . .
C1 C 0.5623(5) 0.4386(5) 0.6664(4) 0.0221(8) Uani 1 1 d . . . . .
C2 C 0.5392(5) 0.3138(5) 0.5173(4) 0.0205(7) Uani 1 1 d . . . . .
C3 C 0.6429(6) 0.2009(5) 0.5009(5) 0.0263(8) Uani 1 1 d . . . . .
H3 H 0.629078 0.117827 0.403463 0.032 Uiso 1 1 calc R U . . .
C4 C 0.7660(6) 0.2078(5) 0.6245(5) 0.0295(9) Uani 1 1 d . . . . .
H4 H 0.832388 0.126740 0.610089 0.035 Uiso 1 1 calc R U . . .
C5 C 0.7947(6) 0.3293(6) 0.7682(5) 0.0311(9) Uani 1 1 d . . . . .
H5 H 0.882425 0.334357 0.850938 0.037 Uiso 1 1 calc R U . . .
C6 C 0.6940(6) 0.4435(5) 0.7898(5) 0.0247(8) Uani 1 1 d . . . . .
H6 H 0.712709 0.526666 0.888496 0.030 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C2 1.974(4) . ?
Al1 C1 2.062(3) 2_666 ?
Al1 Br1 2.2380(13) . ?
Al1 Br2 2.4492(11) . ?
Al2 C1 2.032(4) . ?
Al2 Br4 2.2563(12) . ?
Al2 Br3 2.2661(11) . ?
Al2 Br2 2.4111(14) . ?
C1 C6 1.430(6) . ?
C1 C2 1.443(5) . ?
C2 C3 1.393(5) . ?
C3 C4 1.386(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?

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
C2 Al1 C1 109.11(16) . 2_666 ?
C2 Al1 Br1 122.02(11) . . ?
C1 Al1 Br1 117.67(12) 2_666 . ?
C2 Al1 Br2 97.91(11) . . ?
C1 Al1 Br2 101.63(11) 2_666 . ?
Br1 Al1 Br2 103.93(5) . . ?
C1 Al2 Br4 117.37(12) . . ?
C1 Al2 Br3 108.98(10) . . ?
Br4 Al2 Br3 113.37(5) . . ?
C1 Al2 Br2 103.28(12) . . ?
Br4 Al2 Br2 106.31(5) . . ?
Br3 Al2 Br2 106.43(5) . . ?
Al2 Br2 Al1 90.91(4) . . ?
C6 C1 C2 118.3(3) . . ?
C6 C1 Al2 112.9(2) . . ?
C2 C1 Al2 109.9(3) . . ?
C6 C1 Al1 107.7(3) . 2_666 ?
C2 C1 Al1 104.4(2) . 2_666 ?
Al2 C1 Al1 101.97(16) . 2_666 ?
C3 C2 C1 118.5(4) . . ?
C3 C2 Al1 122.5(3) . . ?
C1 C2 Al1 119.0(3) . . ?
C4 C3 C2 121.0(4) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C5 C4 C3 121.8(4) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 119.1(4) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C1 121.2(4) . . ?
C5 C6 H6 119.4 . . ?
C1 C6 H6 119.4 . . ?

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
C6 C1 C2 C3 1.6(5) . . . . ?
Al2 C1 C2 C3 -130.1(3) . . . . ?
Al1 C1 C2 C3 121.2(3) 2_666 . . . ?
C6 C1 C2 Al1 -177.7(2) . . . . ?
Al2 C1 C2 Al1 50.6(3) . . . . ?
Al1 C1 C2 Al1 -58.1(3) 2_666 . . . ?
C1 C2 C3 C4 -0.1(5) . . . . ?
Al1 C2 C3 C4 179.2(3) . . . . ?
C2 C3 C4 C5 -1.7(6) . . . . ?
C3 C4 C5 C6 2.0(6) . . . . ?
C4 C5 C6 C1 -0.5(6) . . . . ?
C2 C1 C6 C5 -1.3(5) . . . . ?
Al2 C1 C6 C5 129.0(3) . . . . ?
Al1 C1 C6 C5 -119.2(3) 2_666 . . . ?

_refine_diff_density_max         0.790
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.152


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2py2_wa3239_av
_database_code_depnum_ccdc_archive 'CCDC 2385637'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H18 Al2 Br2 N2, C6 H6'
_chemical_formula_sum            'C28 H24 Al2 Br2 N2'
_chemical_formula_weight         602.27

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0374(7)
_cell_length_b                   9.3213(6)
_cell_length_c                   9.7274(9)
_cell_angle_alpha                110.307(7)
_cell_angle_beta                 104.486(8)
_cell_angle_gamma                104.444(6)
_cell_volume                     691.18(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3581
_cell_measurement_theta_min      3.8320
_cell_measurement_theta_max      25.8900

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             302
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.260
_exptl_absorpt_coefficient_mu    3.014
_shelx_estimated_absorpt_T_min   0.475
_shelx_estimated_absorpt_T_max   0.508
_exptl_absorpt_correction_T_min  0.65758
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            12141
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.592
_diffrn_reflns_theta_max         26.035
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2719
_reflns_number_gt                2310
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  'IUCr PublCIF online service'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0176P)²+0.3795P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2719
_refine_ls_number_parameters     181
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0678
_refine_ls_wR_factor_gt          0.0652
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_restrained_S_all      1.144
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Al1 Al 0.49265(9) 0.66661(9) 0.64586(9) 0.01699(18) Uani 1 1 d . . . . .
Br1 Br 0.66833(4) 0.88617(4) 0.88880(4) 0.03409(11) Uani 1 1 d . . . . .
C1 C 0.4457(3) 0.4524(3) 0.6529(3) 0.0171(5) Uani 1 1 d . . . . .
C2 C 0.4459(3) 0.3148(3) 0.5289(3) 0.0181(6) Uani 1 1 d . . . . .
C3 C 0.4032(3) 0.1625(3) 0.5356(4) 0.0260(6) Uani 1 1 d . . . . .
H3 H 0.402758 0.069569 0.453765 0.031 Uiso 1 1 calc R U . . .
C4 C 0.3617(4) 0.1434(4) 0.6572(4) 0.0307(7) Uani 1 1 d . . . . .
H4 H 0.333696 0.038637 0.658204 0.037 Uiso 1 1 calc R U . . .
C5 C 0.3608(3) 0.2763(4) 0.7775(4) 0.0296(7) Uani 1 1 d . . . . .
H5 H 0.332304 0.263451 0.861251 0.036 Uiso 1 1 calc R U . . .
C6 C 0.4020(3) 0.4288(3) 0.7749(3) 0.0231(6) Uani 1 1 d . . . . .
H6 H 0.400723 0.519795 0.857573 0.028 Uiso 1 1 calc R U . . .
N1 N 0.2838(3) 0.7065(2) 0.6155(3) 0.0180(5) Uani 1 1 d . . . . .
C12 C 0.1860(3) 0.6669(4) 0.4676(3) 0.0271(6) Uani 1 1 d . . . . .
H12 H 0.221349 0.623508 0.383384 0.033 Uiso 1 1 calc R U . . .
C13 C 0.0378(3) 0.6864(4) 0.4337(4) 0.0333(7) Uani 1 1 d . . . . .
H13 H -0.027782 0.657423 0.328091 0.040 Uiso 1 1 calc R U . . .
C14 C -0.0148(3) 0.7487(4) 0.5555(4) 0.0319(7) Uani 1 1 d . . . . .
H14 H -0.116315 0.764886 0.535291 0.038 Uiso 1 1 calc R U . . .
C15 C 0.0826(3) 0.7871(4) 0.7064(4) 0.0296(7) Uani 1 1 d . . . . .
H15 H 0.048273 0.828748 0.791834 0.035 Uiso 1 1 calc R U . . .
C16 C 0.2302(3) 0.7646(3) 0.7330(3) 0.0240(6) Uani 1 1 d . . . . .
H16 H 0.296346 0.790846 0.837585 0.029 Uiso 1 1 calc R U . . .
C21 C 0.127(3) 0.434(4) 0.036(3) 0.047(5) Uani 0.53 1 d D U P A 1
H21 H 0.210015 0.390988 0.060659 0.056 Uiso 0.53 1 calc R U P A 1
C22 C 0.158(2) 0.597(3) 0.068(2) 0.040(6) Uani 0.53 1 d D U P A 1
H22 H 0.269600 0.670781 0.116060 0.048 Uiso 0.53 1 calc R U P A 1
C23 C 0.038(4) 0.660(2) 0.036(4) 0.051(7) Uani 0.53 1 d D U P A 1
H23 H 0.071774 0.774977 0.065125 0.061 Uiso 0.53 1 calc R U P A 1
C21B C 0.018(4) 0.354(3) -0.010(5) 0.052(7) Uani 0.47 1 d D U P B 2
H21B H 0.036072 0.257614 -0.012032 0.062 Uiso 0.47 1 calc R U P B 2
C22B C 0.149(2) 0.500(4) 0.049(3) 0.035(5) Uani 0.47 1 d D U P B 2
H22B H 0.255797 0.497271 0.080176 0.042 Uiso 0.47 1 calc R U P B 2
C23B C 0.139(4) 0.649(3) 0.067(3) 0.042(6) Uani 0.47 1 d D U P B 2
H23B H 0.233582 0.747750 0.115835 0.050 Uiso 0.47 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C2 1.964(3) 2_666 ?
Al1 C1 1.964(3) . ?
Al1 N1 1.984(2) . ?
Al1 Br1 2.3322(9) . ?
C1 C6 1.408(4) . ?
C1 C2 1.424(4) . ?
C2 C3 1.404(4) . ?
C3 C4 1.381(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
N1 C16 1.347(3) . ?
N1 C12 1.348(3) . ?
C12 C13 1.371(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.376(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C23 1.373(10) 2_565 ?
C21 C22 1.382(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.376(9) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C21B C22B 1.375(10) . ?
C21B C23B 1.378(10) 2_565 ?
C21B H21B 0.9500 . ?
C22B C23B 1.364(11) . ?
C22B H22B 0.9500 . ?
C23B H23B 0.9500 . ?

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
C2 Al1 C1 117.40(11) 2_666 . ?
C2 Al1 N1 104.50(10) 2_666 . ?
C1 Al1 N1 106.03(10) . . ?
C2 Al1 Br1 112.07(8) 2_666 . ?
C1 Al1 Br1 112.84(8) . . ?
N1 Al1 Br1 102.23(7) . . ?
C6 C1 C2 118.6(2) . . ?
C6 C1 Al1 121.1(2) . . ?
C2 C1 Al1 120.21(19) . . ?
C3 C2 C1 117.9(2) . . ?
C3 C2 Al1 119.9(2) . 2_666 ?
C1 C2 Al1 122.24(19) . 2_666 ?
C4 C3 C2 122.2(3) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 119.4(3) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C1 121.8(3) . . ?
C5 C6 H6 119.1 . . ?
C1 C6 H6 119.1 . . ?
C16 N1 C12 117.8(2) . . ?
C16 N1 Al1 123.89(18) . . ?
C12 N1 Al1 118.29(18) . . ?
N1 C12 C13 122.8(3) . . ?
N1 C12 H12 118.6 . . ?
C13 C12 H12 118.6 . . ?
C12 C13 C14 118.9(3) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
C15 C14 C13 118.8(3) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C16 119.5(3) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
N1 C16 C15 122.1(3) . . ?
N1 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
C23 C21 C22 112.0(16) 2_565 . ?
C23 C21 H21 124.0 2_565 . ?
C22 C21 H21 124.0 . . ?
C23 C22 C21 124.3(16) . . ?
C23 C22 H22 117.8 . . ?
C21 C22 H22 117.8 . . ?
C21 C23 C22 123.7(18) 2_565 . ?
C21 C23 H23 118.2 2_565 . ?
C22 C23 H23 118.2 . . ?
C22B C21B H21B 120.6 . . ?
C23B C21B H21B 120.6 2_565 . ?
C23B C22B C21B 126.2(14) . . ?
C23B C22B H22B 116.9 . . ?
C21B C22B H22B 116.9 . . ?
C22B C23B H23B 122.5 . . ?
C21B C23B H23B 122.5 2_565 . ?

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
C6 C1 C2 C3 -0.4(4) . . . . ?
Al1 C1 C2 C3 -176.75(19) . . . . ?
C6 C1 C2 Al1 -179.19(19) . . . 2_666 ?
Al1 C1 C2 Al1 4.4(3) . . . 2_666 ?
C1 C2 C3 C4 0.0(4) . . . . ?
Al1 C2 C3 C4 178.9(2) 2_666 . . . ?
C2 C3 C4 C5 0.2(4) . . . . ?
C3 C4 C5 C6 0.0(4) . . . . ?
C4 C5 C6 C1 -0.3(4) . . . . ?
C2 C1 C6 C5 0.5(4) . . . . ?
Al1 C1 C6 C5 176.9(2) . . . . ?
C16 N1 C12 C13 1.4(4) . . . . ?
Al1 N1 C12 C13 178.6(2) . . . . ?
N1 C12 C13 C14 -0.2(5) . . . . ?
C12 C13 C14 C15 -0.9(5) . . . . ?
C13 C14 C15 C16 0.8(4) . . . . ?
C12 N1 C16 C15 -1.4(4) . . . . ?
Al1 N1 C16 C15 -178.5(2) . . . . ?
C14 C15 C16 N1 0.3(4) . . . . ?
C23 C21 C22 C23 1(5) 2_565 . . . ?
C21 C22 C23 C21 -2(5) . . . 2_565 ?
C23B C21B C22B C23B 5(6) 2_565 . . . ?
C21B C22B C23B C21B -4(6) . . . 2_565 ?

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
C16 H16 Br1 0.95 3.12 3.582(3) 112.0 . yes
C16 H16 Br1 0.95 3.13 3.672(3) 118.1 2_677 yes

_refine_diff_density_max         0.434
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.069


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nBu4N3_wa3283_av
_database_code_depnum_ccdc_archive 'CCDC 2385638'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H36 N, C6 H4 Al2 Br5'
_chemical_formula_sum            'C22 H40 Al2 Br5 N'
_chemical_formula_weight         772.06

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   9.4049(4)
_cell_length_b                   16.9807(6)
_cell_length_c                   10.3837(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.989(4)
_cell_angle_gamma                90
_cell_volume                     1568.06(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5380
_cell_measurement_theta_min      2.8350
_cell_measurement_theta_max      26.9770

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_F_000             760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    6.474
_shelx_estimated_absorpt_T_min   0.264
_shelx_estimated_absorpt_T_max   0.625
_exptl_absorpt_correction_T_min  0.14197
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            15380
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.290
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6903
_reflns_number_gt                5835
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.995

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'IUCr PublCIF online service'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0384P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2252 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6903
_refine_ls_number_parameters     275
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.0965
_refine_ls_wR_factor_gt          0.0901
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Br1 Br 0.12560(10) 0.39433(5) 0.82644(9) 0.0520(2) Uani 1 1 d . . . . .
Br2 Br 0.00827(9) 0.46784(7) 0.46751(8) 0.0579(3) Uani 1 1 d . . . . .
Br3 Br 0.50790(10) 0.71066(5) 0.95612(8) 0.0499(2) Uani 1 1 d . . . . .
Br4 Br 0.33463(14) 0.74478(6) 0.58179(9) 0.0655(3) Uani 1 1 d . . . . .
Br5 Br 0.14759(9) 0.60824(5) 0.76198(9) 0.0511(2) Uani 1 1 d . . . . .
Al1 Al 0.1849(2) 0.47759(13) 0.6790(2) 0.0340(4) Uani 1 1 d . . . . .
Al2 Al 0.3904(3) 0.65165(13) 0.7502(2) 0.0381(5) Uani 1 1 d . . . . .
C1 C 0.3953(7) 0.4828(5) 0.6869(7) 0.0354(15) Uani 1 1 d . . . . .
C2 C 0.4786(8) 0.5524(5) 0.7174(7) 0.0362(16) Uani 1 1 d . . . . .
C3 C 0.6310(8) 0.5519(6) 0.7265(8) 0.0441(18) Uani 1 1 d . . . . .
H3 H 0.687704 0.599248 0.747640 0.053 Uiso 1 1 calc R U . . .
C4 C 0.6995(9) 0.4831(6) 0.7048(8) 0.052(2) Uani 1 1 d . . . . .
H4 H 0.802442 0.483548 0.710842 0.062 Uiso 1 1 calc R U . . .
C5 C 0.6189(9) 0.4144(6) 0.6749(8) 0.050(2) Uani 1 1 d . . . . .
H5 H 0.666178 0.367304 0.660498 0.060 Uiso 1 1 calc R U . . .
C6 C 0.4679(8) 0.4137(5) 0.6655(7) 0.0412(17) Uani 1 1 d . . . . .
H6 H 0.412709 0.365836 0.644338 0.049 Uiso 1 1 calc R U . . .
N1 N 0.4378(6) 0.5151(3) 0.2391(5) 0.0307(12) Uani 1 1 d . . . . .
C11 C 0.4993(7) 0.4911(4) 0.1258(6) 0.0300(14) Uani 1 1 d . . . . .
H11A H 0.417313 0.465456 0.052649 0.036 Uiso 1 1 calc R U . . .
H11B H 0.527747 0.539503 0.086992 0.036 Uiso 1 1 calc R U . . .
C12 C 0.6314(8) 0.4370(5) 0.1659(8) 0.0413(17) Uani 1 1 d . . . . .
H12A H 0.605227 0.387300 0.202586 0.050 Uiso 1 1 calc R U . . .
H12B H 0.716386 0.461835 0.237314 0.050 Uiso 1 1 calc R U . . .
C13 C 0.6761(10) 0.4202(6) 0.0385(9) 0.055(2) Uani 1 1 d . . . . .
H13A H 0.591955 0.392706 -0.029696 0.066 Uiso 1 1 calc R U . . .
H13B H 0.692420 0.470809 -0.001759 0.066 Uiso 1 1 calc R U . . .
C14 C 0.8147(11) 0.3712(7) 0.0675(11) 0.067(3) Uani 1 1 d . . . . .
H14A H 0.824077 0.351955 -0.018395 0.100 Uiso 1 1 calc R U . . .
H14B H 0.808170 0.326240 0.124561 0.100 Uiso 1 1 calc R U . . .
H14C H 0.902874 0.403087 0.115312 0.100 Uiso 1 1 calc R U . . .
C21 C 0.3879(8) 0.4437(4) 0.3009(7) 0.0349(16) Uani 1 1 d . . . . .
H21A H 0.478623 0.413318 0.351657 0.042 Uiso 1 1 calc R U . . .
H21B H 0.340999 0.462483 0.367900 0.042 Uiso 1 1 calc R U . . .
C22 C 0.2794(8) 0.3885(5) 0.2040(7) 0.0374(16) Uani 1 1 d . . . . .
H22A H 0.326124 0.366559 0.138983 0.045 Uiso 1 1 calc R U . . .
H22B H 0.187865 0.417705 0.151309 0.045 Uiso 1 1 calc R U . . .
C23 C 0.2371(10) 0.3224(5) 0.2812(10) 0.051(2) Uani 1 1 d . . . . .
H23A H 0.177115 0.344134 0.335442 0.062 Uiso 1 1 calc R U . . .
H23B H 0.330065 0.299553 0.345477 0.062 Uiso 1 1 calc R U . . .
C24 C 0.1480(10) 0.2574(5) 0.1908(11) 0.057(2) Uani 1 1 d . . . . .
H24A H 0.209089 0.233057 0.140987 0.085 Uiso 1 1 calc R U . . .
H24B H 0.056394 0.279476 0.125791 0.085 Uiso 1 1 calc R U . . .
H24C H 0.120927 0.217509 0.246933 0.085 Uiso 1 1 calc R U . . .
C31 C 0.5592(8) 0.5549(4) 0.3555(7) 0.0343(15) Uani 1 1 d . . . . .
H31A H 0.513872 0.570854 0.425248 0.041 Uiso 1 1 calc R U . . .
H31B H 0.637967 0.515406 0.397990 0.041 Uiso 1 1 calc R U . . .
C32 C 0.6345(8) 0.6264(5) 0.3191(8) 0.0411(17) Uani 1 1 d . . . . .
H32A H 0.557788 0.666148 0.273252 0.049 Uiso 1 1 calc R U . . .
H32B H 0.688968 0.611035 0.255847 0.049 Uiso 1 1 calc R U . . .
C33 C 0.7439(9) 0.6608(5) 0.4484(9) 0.0474(19) Uani 1 1 d . . . . .
H33A H 0.686413 0.683356 0.504360 0.057 Uiso 1 1 calc R U . . .
H33B H 0.808043 0.618064 0.501692 0.057 Uiso 1 1 calc R U . . .
C34 C 0.8434(10) 0.7243(6) 0.4207(10) 0.059(2) Uani 1 1 d . . . . .
H34A H 0.780713 0.764262 0.360423 0.088 Uiso 1 1 calc R U . . .
H34B H 0.911171 0.700748 0.376937 0.088 Uiso 1 1 calc R U . . .
H34C H 0.902790 0.748860 0.506797 0.088 Uiso 1 1 calc R U . . .
C41 C 0.3067(8) 0.5697(5) 0.1723(8) 0.0394(17) Uani 1 1 d . . . . .
H41A H 0.341653 0.610725 0.121832 0.047 Uiso 1 1 calc R U . . .
H41B H 0.227668 0.538904 0.104669 0.047 Uiso 1 1 calc R U . . .
C42 C 0.2359(11) 0.6103(7) 0.2661(10) 0.067(3) Uani 1 1 d . . . . .
H42A H 0.310222 0.646006 0.328468 0.080 Uiso 1 1 calc R U . . .
H42B H 0.205729 0.570525 0.321872 0.080 Uiso 1 1 calc R U . . .
C43 C 0.0981(13) 0.6576(8) 0.1835(13) 0.084(4) Uani 1 1 d . . . . .
H43A H 0.067637 0.692884 0.245902 0.101 Uiso 1 1 calc R U . . .
H43B H 0.125898 0.691141 0.117418 0.101 Uiso 1 1 calc R U . . .
C44 C -0.0354(13) 0.6064(11) 0.1067(14) 0.107(5) Uani 1 1 d . . . . .
H44A H -0.007973 0.573351 0.041066 0.160 Uiso 1 1 calc R U . . .
H44B H -0.120633 0.640090 0.058175 0.160 Uiso 1 1 calc R U . . .
H44C H -0.063481 0.572866 0.171309 0.160 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Br1 Al1 2.282(2) . ?
Br2 Al1 2.288(2) . ?
Br3 Al2 2.294(2) . ?
Br4 Al2 2.288(2) . ?
Br5 Al2 2.440(2) . ?
Br5 Al1 2.446(2) . ?
Al1 C1 1.956(7) . ?
Al2 C2 1.957(8) . ?
C1 C2 1.396(11) . ?
C1 C6 1.411(10) . ?
C2 C3 1.405(10) . ?
C3 C4 1.388(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.370(14) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(11) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
N1 C21 1.515(9) . ?
N1 C41 1.518(9) . ?
N1 C31 1.525(8) . ?
N1 C11 1.525(8) . ?
C11 C12 1.491(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.540(10) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.492(12) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C21 C22 1.505(10) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.506(11) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.513(12) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C31 C32 1.514(10) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.518(11) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.515(11) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C41 C42 1.513(10) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.529(14) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.522(19) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

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
Al2 Br5 Al1 90.71(7) . . ?
C1 Al1 Br1 117.7(2) . . ?
C1 Al1 Br2 116.9(2) . . ?
Br1 Al1 Br2 109.83(9) . . ?
C1 Al1 Br5 101.7(2) . . ?
Br1 Al1 Br5 103.38(8) . . ?
Br2 Al1 Br5 105.13(9) . . ?
C2 Al2 Br4 117.8(2) . . ?
C2 Al2 Br3 115.8(2) . . ?
Br4 Al2 Br3 109.37(10) . . ?
C2 Al2 Br5 101.8(2) . . ?
Br4 Al2 Br5 105.17(10) . . ?
Br3 Al2 Br5 105.07(9) . . ?
C2 C1 C6 118.4(6) . . ?
C2 C1 Al1 122.2(5) . . ?
C6 C1 Al1 119.4(6) . . ?
C1 C2 C3 119.7(7) . . ?
C1 C2 Al2 122.0(5) . . ?
C3 C2 Al2 118.3(6) . . ?
C4 C3 C2 120.7(8) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 C3 120.2(7) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.0(8) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 121.1(8) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
C21 N1 C41 111.4(5) . . ?
C21 N1 C31 105.9(5) . . ?
C41 N1 C31 112.2(6) . . ?
C21 N1 C11 111.1(5) . . ?
C41 N1 C11 105.4(5) . . ?
C31 N1 C11 110.8(5) . . ?
C12 C11 N1 116.1(5) . . ?
C12 C11 H11A 108.3 . . ?
N1 C11 H11A 108.3 . . ?
C12 C11 H11B 108.3 . . ?
N1 C11 H11B 108.3 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 C13 108.1(7) . . ?
C11 C12 H12A 110.1 . . ?
C13 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
C13 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
C14 C13 C12 113.3(8) . . ?
C14 C13 H13A 108.9 . . ?
C12 C13 H13A 108.9 . . ?
C14 C13 H13B 108.9 . . ?
C12 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C22 C21 N1 116.8(6) . . ?
C22 C21 H21A 108.1 . . ?
N1 C21 H21A 108.1 . . ?
C22 C21 H21B 108.1 . . ?
N1 C21 H21B 108.1 . . ?
H21A C21 H21B 107.3 . . ?
C21 C22 C23 110.4(6) . . ?
C21 C22 H22A 109.6 . . ?
C23 C22 H22A 109.6 . . ?
C21 C22 H22B 109.6 . . ?
C23 C22 H22B 109.6 . . ?
H22A C22 H22B 108.1 . . ?
C22 C23 C24 113.7(7) . . ?
C22 C23 H23A 108.8 . . ?
C24 C23 H23A 108.8 . . ?
C22 C23 H23B 108.8 . . ?
C24 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C32 C31 N1 116.6(6) . . ?
C32 C31 H31A 108.1 . . ?
N1 C31 H31A 108.1 . . ?
C32 C31 H31B 108.1 . . ?
N1 C31 H31B 108.1 . . ?
H31A C31 H31B 107.3 . . ?
C31 C32 C33 109.0(6) . . ?
C31 C32 H32A 109.9 . . ?
C33 C32 H32A 109.9 . . ?
C31 C32 H32B 109.9 . . ?
C33 C32 H32B 109.9 . . ?
H32A C32 H32B 108.3 . . ?
C34 C33 C32 112.9(7) . . ?
C34 C33 H33A 109.0 . . ?
C32 C33 H33A 109.0 . . ?
C34 C33 H33B 109.0 . . ?
C32 C33 H33B 109.0 . . ?
H33A C33 H33B 107.8 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C42 C41 N1 116.5(6) . . ?
C42 C41 H41A 108.2 . . ?
N1 C41 H41A 108.2 . . ?
C42 C41 H41B 108.2 . . ?
N1 C41 H41B 108.2 . . ?
H41A C41 H41B 107.3 . . ?
C41 C42 C43 110.4(8) . . ?
C41 C42 H42A 109.6 . . ?
C43 C42 H42A 109.6 . . ?
C41 C42 H42B 109.6 . . ?
C43 C42 H42B 109.6 . . ?
H42A C42 H42B 108.1 . . ?
C44 C43 C42 113.4(11) . . ?
C44 C43 H43A 108.9 . . ?
C42 C43 H43A 108.9 . . ?
C44 C43 H43B 108.9 . . ?
C42 C43 H43B 108.9 . . ?
H43A C43 H43B 107.7 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

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
C12 H12B Br2 0.99 3.00 3.927(8) 156.6 1_655 yes
C42 H42A Br4 0.99 3.06 3.852(11) 137.4 . yes

_refine_diff_density_max         0.621
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.078


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1thf2_wa3621
_database_code_depnum_ccdc_archive 'CCDC 2385639'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H30 Al2 O2'
_chemical_formula_sum            'C22 H30 Al2 O2'
_chemical_formula_weight         380.42

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   9.9086(5)
_cell_length_b                   13.8047(6)
_cell_length_c                   16.1315(7)
_cell_angle_alpha                90
_cell_angle_beta                 95.104(4)
_cell_angle_gamma                90
_cell_volume                     2197.80(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3457
_cell_measurement_theta_min      2.5020
_cell_measurement_theta_max      26.2990

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.145
_shelx_estimated_absorpt_T_min   0.969
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_T_min  0.83074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            16944
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.516
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4161
_reflns_number_gt                3073
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  'IUCr PublCIF online service'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0757P)²+1.0510P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4161
_refine_ls_number_parameters     277
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1612
_refine_ls_wR_factor_gt          0.1451
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Al1 Al 0.58854(8) 0.47720(6) 0.41079(5) 0.0475(2) Uani 1 1 d . . . . .
O1 O 0.6005(2) 0.34234(13) 0.38188(11) 0.0565(5) Uani 1 1 d . . . . .
C1 C 0.6902(3) 0.5359(2) 0.32354(19) 0.0664(8) Uani 1 1 d . . . . .
H1A H 0.777612 0.502982 0.322167 0.100 Uiso 1 1 calc R U . . .
H1B H 0.705524 0.604767 0.335819 0.100 Uiso 1 1 calc R U . . .
H1C H 0.637948 0.529102 0.269359 0.100 Uiso 1 1 calc R U . . .
C11 C 0.3906(3) 0.50268(18) 0.40332(15) 0.0470(6) Uani 1 1 d . . . . .
C12 C 0.3145(3) 0.5028(2) 0.32523(17) 0.0555(7) Uani 1 1 d . . . . .
H12 H 0.359513 0.488879 0.277024 0.067 Uiso 1 1 calc R U . . .
C13 C 0.1776(3) 0.5223(2) 0.31579(18) 0.0590(7) Uani 1 1 d . . . . .
H13 H 0.129767 0.521278 0.262075 0.071 Uiso 1 1 calc R U . . .
C14 C 0.1107(3) 0.5431(2) 0.38485(19) 0.0586(7) Uani 1 1 d . . . . .
H14 H 0.016915 0.558570 0.379033 0.070 Uiso 1 1 calc R U . . .
C15 C 0.1816(3) 0.54144(19) 0.46314(17) 0.0528(7) Uani 1 1 d . . . . .
H15 H 0.133753 0.553671 0.510558 0.063 Uiso 1 1 calc R U . . .
C16 C 0.3210(3) 0.52233(17) 0.47481(15) 0.0454(6) Uani 1 1 d . . . . .
C11A C 0.5498(10) 0.3138(8) 0.2966(6) 0.052(2) Uiso 0.36 1 d . . P A 1
H11A H 0.617590 0.327281 0.256582 0.063 Uiso 0.36 1 calc R U P A 1
H11B H 0.464263 0.347661 0.278327 0.063 Uiso 0.36 1 calc R U P A 1
C12A C 0.5270(13) 0.2043(8) 0.3061(7) 0.071(3) Uiso 0.36 1 d . . P A 1
H12A H 0.429113 0.190557 0.307324 0.085 Uiso 0.36 1 calc R U P A 1
H12B H 0.560252 0.169098 0.258446 0.085 Uiso 0.36 1 calc R U P A 1
C13A C 0.5998(12) 0.1736(7) 0.3825(7) 0.062(2) Uiso 0.36 1 d . . P A 1
H13A H 0.691603 0.150532 0.372475 0.075 Uiso 0.36 1 calc R U P A 1
H13B H 0.550986 0.120614 0.408436 0.075 Uiso 0.36 1 calc R U P A 1
C14A C 0.6078(11) 0.2586(7) 0.4352(6) 0.055(3) Uiso 0.36 1 d . . P A 1
H14A H 0.531859 0.259093 0.471150 0.066 Uiso 0.36 1 calc R U P A 1
H14B H 0.694023 0.258704 0.471254 0.066 Uiso 0.36 1 calc R U P A 1
C11B C 0.6105(10) 0.3138(7) 0.2943(5) 0.055(2) Uiso 0.43 1 d . . P A 2
H11C H 0.702195 0.326741 0.276932 0.066 Uiso 0.43 1 calc R U P A 2
H11D H 0.542631 0.348238 0.256337 0.066 Uiso 0.43 1 calc R U P A 2
C12B C 0.5818(10) 0.2075(6) 0.2961(5) 0.054(2) Uiso 0.43 1 d . . P A 2
H12C H 0.663958 0.170741 0.284720 0.065 Uiso 0.43 1 calc R U P A 2
H12D H 0.508680 0.191128 0.252560 0.065 Uiso 0.43 1 calc R U P A 2
C13B C 0.5348(12) 0.1770(7) 0.3899(6) 0.070(2) Uiso 0.43 1 d . . P A 2
H13C H 0.437188 0.160643 0.386879 0.085 Uiso 0.43 1 calc R U P A 2
H13D H 0.588189 0.121394 0.413646 0.085 Uiso 0.43 1 calc R U P A 2
C14B C 0.5653(12) 0.2683(6) 0.4403(5) 0.048(2) Uiso 0.43 1 d . . P A 2
H14C H 0.484916 0.288470 0.468390 0.058 Uiso 0.43 1 calc R U P A 2
H14D H 0.641567 0.257223 0.483172 0.058 Uiso 0.43 1 calc R U P A 2
C11C C 0.5909(18) 0.2874(11) 0.3030(8) 0.034(3) Uiso 0.21 1 d . . P A 3
H11E H 0.665219 0.306087 0.269044 0.041 Uiso 0.21 1 calc R U P A 3
H11F H 0.503323 0.300635 0.270460 0.041 Uiso 0.21 1 calc R U P A 3
C12C C 0.602(2) 0.1821(13) 0.3261(16) 0.072(5) Uiso 0.21 1 d . . P A 3
H12E H 0.688847 0.164301 0.357071 0.086 Uiso 0.21 1 calc R U P A 3
H12F H 0.579387 0.137493 0.278759 0.086 Uiso 0.21 1 calc R U P A 3
C13C C 0.4845(19) 0.1968(13) 0.3820(12) 0.070(2) Uiso 0.21 1 d . . P A 3
H13E H 0.397921 0.204804 0.347060 0.085 Uiso 0.21 1 calc R U P A 3
H13F H 0.476578 0.139334 0.417987 0.085 Uiso 0.21 1 calc R U P A 3
C14C C 0.509(2) 0.2757(14) 0.4292(13) 0.076(6) Uiso 0.21 1 d . . P A 3
H14E H 0.555613 0.257505 0.483880 0.091 Uiso 0.21 1 calc R U P A 3
H14F H 0.423514 0.309021 0.438493 0.091 Uiso 0.21 1 calc R U P A 3
Al2 Al 1.12179(8) 0.09392(6) 0.51913(5) 0.0541(3) Uani 1 1 d . . . . .
C2 C 1.2693(3) 0.1494(3) 0.5946(2) 0.0781(10) Uani 1 1 d . . . . .
H2A H 1.350132 0.157744 0.564506 0.117 Uiso 1 1 calc R U . . .
H2B H 1.290064 0.105569 0.641831 0.117 Uiso 1 1 calc R U . . .
H2C H 1.240931 0.212391 0.615029 0.117 Uiso 1 1 calc R U . . .
C21 C 0.9372(3) 0.1018(2) 0.55649(17) 0.0525(7) Uani 1 1 d . . . . .
C22 C 0.8990(3) 0.1838(2) 0.59980(18) 0.0595(7) Uani 1 1 d . . . . .
H22 H 0.964262 0.233507 0.611297 0.071 Uiso 1 1 calc R U . . .
C23 C 0.7721(3) 0.1964(2) 0.6267(2) 0.0654(8) Uani 1 1 d . . . . .
H23 H 0.750726 0.253676 0.655440 0.078 Uiso 1 1 calc R U . . .
C24 C 0.6778(3) 0.1255(3) 0.6114(2) 0.0712(9) Uani 1 1 d . . . . .
H24 H 0.590323 0.132393 0.630497 0.085 Uiso 1 1 calc R U . . .
C25 C 0.7098(3) 0.0426(2) 0.5677(2) 0.0675(8) Uani 1 1 d . . . . .
H25 H 0.642173 -0.005687 0.556758 0.081 Uiso 1 1 calc R U . . .
C26 C 0.8384(3) 0.0277(2) 0.53903(18) 0.0548(7) Uani 1 1 d . . . . .
O2A O 1.109(2) 0.183(2) 0.4219(13) 0.047(4) Uani 0.43 1 d . U P B 1
C21A C 1.0786(9) 0.2879(6) 0.4325(5) 0.050(2) Uiso 0.43 1 d . . P B 1
H21A H 1.057438 0.301641 0.490205 0.060 Uiso 0.43 1 calc R U P B 1
H21B H 1.156500 0.328462 0.419655 0.060 Uiso 0.43 1 calc R U P B 1
C22B C 0.9783(10) 0.3038(8) 0.3822(5) 0.0724(17) Uiso 0.43 1 d . . P B 1
H22A H 0.959103 0.373756 0.374351 0.087 Uiso 0.43 1 calc R U P B 1
H22B H 0.895961 0.269379 0.396728 0.087 Uiso 0.43 1 calc R U P B 1
C23A C 1.0467(14) 0.2539(9) 0.3008(7) 0.084(4) Uiso 0.43 1 d . . P B 1
H23A H 0.978984 0.246124 0.252254 0.100 Uiso 0.43 1 calc R U P B 1
H23B H 1.124481 0.292068 0.284236 0.100 Uiso 0.43 1 calc R U P B 1
C24A C 1.0926(9) 0.1538(5) 0.3393(4) 0.0523(18) Uiso 0.43 1 d . . P B 1
H24A H 1.021893 0.103388 0.329444 0.063 Uiso 0.43 1 calc R U P B 1
H24B H 1.178530 0.130852 0.319086 0.063 Uiso 0.43 1 calc R U P B 1
O2B O 1.138(3) 0.179(2) 0.428(2) 0.054(5) Uani 0.36 1 d . U P B 2
C21B C 1.1205(14) 0.2813(8) 0.4368(8) 0.065(3) Uiso 0.36 1 d . . P B 2
H21C H 1.204582 0.316998 0.427751 0.079 Uiso 0.36 1 calc R U P B 2
H21D H 1.091348 0.298260 0.492099 0.079 Uiso 0.36 1 calc R U P B 2
C22A C 0.9838(12) 0.3053(9) 0.3519(7) 0.0724(17) Uiso 0.36 1 d . . P B 2
H22C H 0.892428 0.298434 0.371496 0.087 Uiso 0.36 1 calc R U P B 2
H22D H 0.992841 0.370310 0.327001 0.087 Uiso 0.36 1 calc R U P B 2
C23B C 1.0118(15) 0.2311(9) 0.2963(7) 0.058(3) Uiso 0.36 1 d . . P B 2
H23C H 1.091895 0.247505 0.266465 0.070 Uiso 0.36 1 calc R U P B 2
H23D H 0.933386 0.219967 0.254917 0.070 Uiso 0.36 1 calc R U P B 2
C24B C 1.0376(11) 0.1482(6) 0.3471(6) 0.059(2) Uiso 0.36 1 d . . P B 2
H24C H 1.080460 0.096965 0.315460 0.071 Uiso 0.36 1 calc R U P B 2
H24D H 0.951429 0.122498 0.364909 0.071 Uiso 0.36 1 calc R U P B 2
O2C O 1.0824(19) 0.2029(11) 0.4437(12) 0.042(4) Uani 0.21 1 d . U P B 3
C21C C 1.1930(17) 0.2551(12) 0.4090(10) 0.064(4) Uiso 0.21 1 d . . P B 3
H21E H 1.201710 0.321292 0.432447 0.077 Uiso 0.21 1 calc R U P B 3
H21F H 1.279927 0.220535 0.421729 0.077 Uiso 0.21 1 calc R U P B 3
C22C C 1.158(2) 0.2587(14) 0.3212(12) 0.085(5) Uiso 0.21 1 d . . P B 3
H22E H 1.193761 0.201404 0.293384 0.101 Uiso 0.21 1 calc R U P B 3
H22F H 1.194658 0.318062 0.296929 0.101 Uiso 0.21 1 calc R U P B 3
C23C C 0.9862(14) 0.2594(12) 0.3114(9) 0.039(3) Uiso 0.21 1 d . . P B 3
H23E H 0.949559 0.325999 0.313676 0.047 Uiso 0.21 1 calc R U P B 3
H23F H 0.949103 0.227592 0.259314 0.047 Uiso 0.21 1 calc R U P B 3
C24C C 0.9591(16) 0.2034(12) 0.3844(10) 0.069(4) Uiso 0.21 1 d . . P B 3
H24E H 0.934230 0.136189 0.367868 0.083 Uiso 0.21 1 calc R U P B 3
H24F H 0.882485 0.232408 0.411055 0.083 Uiso 0.21 1 calc R U P B 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 1.925(2) . ?
Al1 C1 1.976(3) . ?
Al1 C16 1.979(3) 3_666 ?
Al1 C11 1.986(3) . ?
O1 C14A 1.439(10) . ?
O1 C14B 1.454(9) . ?
O1 C11A 1.475(9) . ?
O1 C11C 1.477(13) . ?
O1 C11B 1.479(8) . ?
O1 C14C 1.539(19) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C11 C12 1.409(3) . ?
C11 C16 1.421(4) . ?
C12 C13 1.378(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.376(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.403(4) . ?
C15 H15 0.9500 . ?
C11A C12A 1.538(15) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C12A C13A 1.437(15) . ?
C12A H12A 0.9900 . ?
C12A H12B 0.9900 . ?
C13A C14A 1.448(14) . ?
C13A H13A 0.9900 . ?
C13A H13B 0.9900 . ?
C14A H14A 0.9900 . ?
C14A H14B 0.9900 . ?
C11B C12B 1.496(12) . ?
C11B H11C 0.9900 . ?
C11B H11D 0.9900 . ?
C12B C13B 1.675(13) . ?
C12B H12C 0.9900 . ?
C12B H12D 0.9900 . ?
C13B C14B 1.517(13) . ?
C13B H13C 0.9900 . ?
C13B H13D 0.9900 . ?
C14B H14C 0.9900 . ?
C14B H14D 0.9900 . ?
C11C C12C 1.50(2) . ?
C11C H11E 0.9900 . ?
C11C H11F 0.9900 . ?
C12C C13C 1.55(3) . ?
C12C H12E 0.9900 . ?
C12C H12F 0.9900 . ?
C13C C14C 1.34(3) . ?
C13C H13E 0.9900 . ?
C13C H13F 0.9900 . ?
C14C H14E 0.9900 . ?
C14C H14F 0.9900 . ?
Al2 O2B 1.89(3) . ?
Al2 O2C 1.952(19) . ?
Al2 C2 1.972(3) . ?
Al2 C21 1.979(3) . ?
Al2 C26 1.980(3) 3_756 ?
Al2 O2A 1.99(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C21 C22 1.400(4) . ?
C21 C26 1.427(4) . ?
C22 C23 1.377(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.360(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.396(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.409(4) . ?
C25 H25 0.9500 . ?
O2A C24A 1.39(2) . ?
O2A C21A 1.49(3) . ?
C21A C22B 1.246(12) . ?
C21A H21A 0.9900 . ?
C21A H21B 0.9900 . ?
C22B C23A 1.678(16) . ?
C22B H22A 0.9900 . ?
C22B H22B 0.9900 . ?
C23A C24A 1.567(14) . ?
C23A H23A 0.9900 . ?
C23A H23B 0.9900 . ?
C24A H24A 0.9900 . ?
C24A H24B 0.9900 . ?
O2B C21B 1.43(4) . ?
O2B C24B 1.63(3) . ?
C21B C22A 1.869(17) . ?
C21B H21C 0.9900 . ?
C21B H21D 0.9900 . ?
C22A C23B 1.406(16) . ?
C22A H22C 0.9900 . ?
C22A H22D 0.9900 . ?
C23B C24B 1.418(14) . ?
C23B H23C 0.9900 . ?
C23B H23D 0.9900 . ?
C24B H24C 0.9900 . ?
C24B H24D 0.9900 . ?
O2C C21C 1.46(2) . ?
O2C C24C 1.48(3) . ?
C21C C22C 1.43(2) . ?
C21C H21E 0.9900 . ?
C21C H21F 0.9900 . ?
C22C C23C 1.70(2) . ?
C22C H22E 0.9900 . ?
C22C H22F 0.9900 . ?
C23C C24C 1.45(2) . ?
C23C H23E 0.9900 . ?
C23C H23F 0.9900 . ?
C24C H24E 0.9900 . ?
C24C H24F 0.9900 . ?

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 C1 100.23(12) . . ?
O1 Al1 C16 101.33(9) . 3_666 ?
C1 Al1 C16 116.46(13) . 3_666 ?
O1 Al1 C11 103.80(10) . . ?
C1 Al1 C11 116.59(13) . . ?
C16 Al1 C11 114.77(11) 3_666 . ?
C14A O1 C11A 109.7(6) . . ?
C14B O1 C11B 118.2(5) . . ?
C11C O1 C14C 97.2(10) . . ?
C14A O1 Al1 129.3(4) . . ?
C14B O1 Al1 119.9(4) . . ?
C11A O1 Al1 117.4(4) . . ?
C11C O1 Al1 134.8(6) . . ?
C11B O1 Al1 120.0(4) . . ?
C14C O1 Al1 114.0(7) . . ?
Al1 C1 H1A 109.5 . . ?
Al1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Al1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C12 C11 C16 117.8(2) . . ?
C12 C11 Al1 120.1(2) . . ?
C16 C11 Al1 122.15(18) . . ?
C13 C12 C11 122.8(3) . . ?
C13 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
C14 C13 C12 119.4(3) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 119.4(3) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C14 C15 C16 122.5(3) . . ?
C14 C15 H15 118.8 . . ?
C16 C15 H15 118.8 . . ?
C15 C16 C11 118.0(2) . . ?
C15 C16 Al1 118.9(2) . 3_666 ?
C11 C16 Al1 123.06(19) . 3_666 ?
O1 C11A C12A 102.2(7) . . ?
O1 C11A H11A 111.3 . . ?
C12A C11A H11A 111.3 . . ?
O1 C11A H11B 111.3 . . ?
C12A C11A H11B 111.3 . . ?
H11A C11A H11B 109.2 . . ?
C13A C12A C11A 107.9(8) . . ?
C13A C12A H12A 110.1 . . ?
C11A C12A H12A 110.1 . . ?
C13A C12A H12B 110.1 . . ?
C11A C12A H12B 110.1 . . ?
H12A C12A H12B 108.4 . . ?
C12A C13A C14A 105.2(8) . . ?
C12A C13A H13A 110.7 . . ?
C14A C13A H13A 110.7 . . ?
C12A C13A H13B 110.7 . . ?
C14A C13A H13B 110.7 . . ?
H13A C13A H13B 108.8 . . ?
O1 C14A C13A 107.6(8) . . ?
O1 C14A H14A 110.2 . . ?
C13A C14A H14A 110.2 . . ?
O1 C14A H14B 110.2 . . ?
C13A C14A H14B 110.2 . . ?
H14A C14A H14B 108.5 . . ?
O1 C11B C12B 102.3(6) . . ?
O1 C11B H11C 111.3 . . ?
C12B C11B H11C 111.3 . . ?
O1 C11B H11D 111.3 . . ?
C12B C11B H11D 111.3 . . ?
H11C C11B H11D 109.2 . . ?
C11B C12B C13B 109.5(7) . . ?
C11B C12B H12C 109.8 . . ?
C13B C12B H12C 109.8 . . ?
C11B C12B H12D 109.8 . . ?
C13B C12B H12D 109.8 . . ?
H12C C12B H12D 108.2 . . ?
C14B C13B C12B 102.5(7) . . ?
C14B C13B H13C 111.3 . . ?
C12B C13B H13C 111.3 . . ?
C14B C13B H13D 111.3 . . ?
C12B C13B H13D 111.3 . . ?
H13C C13B H13D 109.2 . . ?
O1 C14B C13B 106.5(6) . . ?
O1 C14B H14C 110.4 . . ?
C13B C14B H14C 110.4 . . ?
O1 C14B H14D 110.4 . . ?
C13B C14B H14D 110.4 . . ?
H14C C14B H14D 108.6 . . ?
O1 C11C C12C 106.6(12) . . ?
O1 C11C H11E 110.4 . . ?
C12C C11C H11E 110.4 . . ?
O1 C11C H11F 110.4 . . ?
C12C C11C H11F 110.4 . . ?
H11E C11C H11F 108.6 . . ?
C11C C12C C13C 88.7(14) . . ?
C11C C12C H12E 113.9 . . ?
C13C C12C H12E 113.9 . . ?
C11C C12C H12F 113.9 . . ?
C13C C12C H12F 113.9 . . ?
H12E C12C H12F 111.1 . . ?
C14C C13C C12C 109.2(17) . . ?
C14C C13C H13E 109.8 . . ?
C12C C13C H13E 109.8 . . ?
C14C C13C H13F 109.8 . . ?
C12C C13C H13F 109.8 . . ?
H13E C13C H13F 108.3 . . ?
C13C C14C O1 106.9(15) . . ?
C13C C14C H14E 110.3 . . ?
O1 C14C H14E 110.3 . . ?
C13C C14C H14F 110.3 . . ?
O1 C14C H14F 110.3 . . ?
H14E C14C H14F 108.6 . . ?
O2B Al2 C2 97.4(8) . . ?
O2C Al2 C2 100.5(6) . . ?
O2B Al2 C21 110.2(8) . . ?
O2C Al2 C21 90.5(5) . . ?
C2 Al2 C21 116.41(14) . . ?
O2B Al2 C26 97.1(11) . 3_756 ?
O2C Al2 C26 113.3(4) . 3_756 ?
C2 Al2 C26 117.00(15) . 3_756 ?
C21 Al2 C26 114.80(12) . 3_756 ?
C2 Al2 O2A 103.8(7) . . ?
C21 Al2 O2A 102.1(8) . . ?
C26 Al2 O2A 98.8(8) 3_756 . ?
Al2 C2 H2A 109.5 . . ?
Al2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Al2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C22 C21 C26 117.8(3) . . ?
C22 C21 Al2 119.7(2) . . ?
C26 C21 Al2 122.5(2) . . ?
C23 C22 C21 123.7(3) . . ?
C23 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
C24 C23 C22 118.9(3) . . ?
C24 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
C23 C24 C25 119.9(3) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C24 C25 C26 122.6(3) . . ?
C24 C25 H25 118.7 . . ?
C26 C25 H25 118.7 . . ?
C25 C26 C21 117.1(3) . . ?
C25 C26 Al2 120.2(2) . 3_756 ?
C21 C26 Al2 122.7(2) . 3_756 ?
C24A O2A C21A 112.8(16) . . ?
C24A O2A Al2 124.7(17) . . ?
C21A O2A Al2 120.6(14) . . ?
C22B C21A O2A 104.6(11) . . ?
C22B C21A H21A 110.8 . . ?
O2A C21A H21A 110.8 . . ?
C22B C21A H21B 110.8 . . ?
O2A C21A H21B 110.8 . . ?
H21A C21A H21B 108.9 . . ?
C21A C22B C23A 94.8(8) . . ?
C21A C22B H22A 112.8 . . ?
C23A C22B H22A 112.8 . . ?
C21A C22B H22B 112.8 . . ?
C23A C22B H22B 112.8 . . ?
H22A C22B H22B 110.2 . . ?
C24A C23A C22B 100.1(8) . . ?
C24A C23A H23A 111.8 . . ?
C22B C23A H23A 111.8 . . ?
C24A C23A H23B 111.8 . . ?
C22B C23A H23B 111.8 . . ?
H23A C23A H23B 109.5 . . ?
O2A C24A C23A 97.4(13) . . ?
O2A C24A H24A 112.3 . . ?
C23A C24A H24A 112.3 . . ?
O2A C24A H24B 112.3 . . ?
C23A C24A H24B 112.3 . . ?
H24A C24A H24B 109.9 . . ?
C21B O2B C24B 105.3(18) . . ?
C21B O2B Al2 121(2) . . ?
C24B O2B Al2 112.0(17) . . ?
O2B C21B C22A 101.0(13) . . ?
O2B C21B H21C 111.6 . . ?
C22A C21B H21C 111.6 . . ?
O2B C21B H21D 111.6 . . ?
C22A C21B H21D 111.6 . . ?
H21C C21B H21D 109.4 . . ?
C23B C22A C21B 99.6(9) . . ?
C23B C22A H22C 111.9 . . ?
C21B C22A H22C 111.9 . . ?
C23B C22A H22D 111.9 . . ?
C21B C22A H22D 111.9 . . ?
H22C C22A H22D 109.6 . . ?
C22A C23B C24B 104.8(9) . . ?
C22A C23B H23C 110.8 . . ?
C24B C23B H23C 110.8 . . ?
C22A C23B H23D 110.8 . . ?
C24B C23B H23D 110.8 . . ?
H23C C23B H23D 108.9 . . ?
C23B C24B O2B 108.8(14) . . ?
C23B C24B H24C 109.9 . . ?
O2B C24B H24C 109.9 . . ?
C23B C24B H24D 109.9 . . ?
O2B C24B H24D 109.9 . . ?
H24C C24B H24D 108.3 . . ?
C21C O2C C24C 110.7(15) . . ?
C21C O2C Al2 120.2(14) . . ?
C24C O2C Al2 120.8(12) . . ?
C22C C21C O2C 105.9(15) . . ?
C22C C21C H21E 110.6 . . ?
O2C C21C H21E 110.6 . . ?
C22C C21C H21F 110.6 . . ?
O2C C21C H21F 110.6 . . ?
H21E C21C H21F 108.7 . . ?
C21C C22C C23C 104.1(13) . . ?
C21C C22C H22E 110.9 . . ?
C23C C22C H22E 110.9 . . ?
C21C C22C H22F 110.9 . . ?
C23C C22C H22F 110.9 . . ?
H22E C22C H22F 109.0 . . ?
C24C C23C C22C 100.3(11) . . ?
C24C C23C H23E 111.7 . . ?
C22C C23C H23E 111.7 . . ?
C24C C23C H23F 111.7 . . ?
C22C C23C H23F 111.7 . . ?
H23E C23C H23F 109.5 . . ?
C23C C24C O2C 108.9(13) . . ?
C23C C24C H24E 109.9 . . ?
O2C C24C H24E 109.9 . . ?
C23C C24C H24F 109.9 . . ?
O2C C24C H24F 109.9 . . ?
H24E C24C H24F 108.3 . . ?

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
C16 C11 C12 C13 0.9(4) . . . . ?
Al1 C11 C12 C13 -178.4(2) . . . . ?
C11 C12 C13 C14 0.4(4) . . . . ?
C12 C13 C14 C15 -1.9(4) . . . . ?
C13 C14 C15 C16 2.2(4) . . . . ?
C14 C15 C16 C11 -1.0(4) . . . . ?
C14 C15 C16 Al1 179.5(2) . . . 3_666 ?
C12 C11 C16 C15 -0.6(4) . . . . ?
Al1 C11 C16 C15 178.70(19) . . . . ?
C12 C11 C16 Al1 178.92(19) . . . 3_666 ?
Al1 C11 C16 Al1 -1.8(3) . . . 3_666 ?
C14A O1 C11A C12A 0.5(9) . . . . ?
Al1 O1 C11A C12A -160.2(6) . . . . ?
O1 C11A C12A C13A -16.9(12) . . . . ?
C11A C12A C13A C14A 26.7(14) . . . . ?
C11A O1 C14A C13A 15.9(10) . . . . ?
Al1 O1 C14A C13A 173.6(6) . . . . ?
C12A C13A C14A O1 -26.3(13) . . . . ?
C14B O1 C11B C12B -1.6(10) . . . . ?
Al1 O1 C11B C12B -166.1(5) . . . . ?
O1 C11B C12B C13B 7.0(10) . . . . ?
C11B C12B C13B C14B -9.9(12) . . . . ?
C11B O1 C14B C13B -4.9(11) . . . . ?
Al1 O1 C14B C13B 159.5(6) . . . . ?
C12B C13B C14B O1 8.3(11) . . . . ?
C14C O1 C11C C12C -42.1(15) . . . . ?
Al1 O1 C11C C12C -176.7(8) . . . . ?
O1 C11C C12C C13C 53.5(16) . . . . ?
C11C C12C C13C C14C -48(2) . . . . ?
C12C C13C C14C O1 26(2) . . . . ?
C11C O1 C14C C13C 8.9(18) . . . . ?
Al1 O1 C14C C13C 155.2(13) . . . . ?
C26 C21 C22 C23 0.4(4) . . . . ?
Al2 C21 C22 C23 178.7(2) . . . . ?
C21 C22 C23 C24 0.6(4) . . . . ?
C22 C23 C24 C25 -1.3(5) . . . . ?
C23 C24 C25 C26 1.0(5) . . . . ?
C24 C25 C26 C21 -0.1(4) . . . . ?
C24 C25 C26 Al2 177.8(2) . . . 3_756 ?
C22 C21 C26 C25 -0.6(4) . . . . ?
Al2 C21 C26 C25 -178.8(2) . . . . ?
C22 C21 C26 Al2 -178.43(19) . . . 3_756 ?
Al2 C21 C26 Al2 3.3(3) . . . 3_756 ?
C24A O2A C21A C22B 39.4(19) . . . . ?
Al2 O2A C21A C22B -125.7(13) . . . . ?
O2A C21A C22B C23A -50.8(12) . . . . ?
C21A C22B C23A C24A 51.2(9) . . . . ?
C21A O2A C24A C23A -0.7(18) . . . . ?
Al2 O2A C24A C23A 163.7(16) . . . . ?
C22B C23A C24A O2A -26.7(13) . . . . ?
C2 Al2 O2B C21B -60.3(17) . . . . ?
C21 Al2 O2B C21B 61.4(18) . . . . ?
C26 Al2 O2B C21B -178.9(16) 3_756 . . . ?
C2 Al2 O2B C24B 174.5(16) . . . . ?
C21 Al2 O2B C24B -64(2) . . . . ?
C26 Al2 O2B C24B 56.0(18) 3_756 . . . ?
C24B O2B C21B C22A 3.9(19) . . . . ?
Al2 O2B C21B C22A -124.3(14) . . . . ?
O2B C21B C22A C23B -29.2(17) . . . . ?
C21B C22A C23B C24B 43.5(12) . . . . ?
C22A C23B C24B O2B -45.4(17) . . . . ?
C21B O2B C24B C23B 23(2) . . . . ?
Al2 O2B C24B C23B 156.2(14) . . . . ?
C24C O2C C21C C22C -19.4(19) . . . . ?
Al2 O2C C21C C22C 129.1(14) . . . . ?
O2C C21C C22C C23C 29.9(17) . . . . ?
C21C C22C C23C C24C -30.8(17) . . . . ?
C22C C23C C24C O2C 19.0(17) . . . . ?
C21C O2C C24C C23C -2.3(19) . . . . ?
Al2 O2C C24C C23C -150.6(12) . . . . ?

_refine_diff_density_max         0.302
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.052


