Donor-free 9,10-dihydro-9,10-dialuminaanthracenes.
Lückert, Paula L; Gilmer, Jannik; Virovets, Alexander; Lerner, Hans-Wolfram; Wagner, Matthias; Chemical science 16 (2024) 147–155; doi:10.1039/d4sc06940d

data_1573180
_publ_section_title
;
 Donor-free 9,10-dihydro-9,10-dialuminaanthracenes.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              147
_journal_page_last               155
_journal_paper_doi               10.1039/d4sc06940d
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'C38 H42 Al4 K N4 O, C8 H16 K O2'
_chemical_formula_sum            'C23 H29 Al2 K N2 O1.5'
_chemical_formula_weight         450.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.030(9)
_cell_angle_beta                 91.767(9)
_cell_angle_gamma                109.036(9)
_cell_formula_units_Z            4
_cell_length_a                   10.9074(12)
_cell_length_b                   12.1287(12)
_cell_length_c                   20.097(2)
_cell_measurement_reflns_used    2581
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.7700
_cell_measurement_theta_min      3.1980
_cell_volume                     2511.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'image plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2042
_diffrn_reflns_av_unetI/netI     0.1372
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9521
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.389
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17122
_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.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         9521
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1567
_refine_ls_R_factor_gt           0.1057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1985P)^2^+3.2515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3841
_refine_ls_wR_factor_ref         0.3937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4260
_reflns_number_total             9521
_reflns_threshold_expression     'I > 2\s(I)'
_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)
;
_cod_data_source_file            d4sc06940d3.cif
_cod_data_source_block           K1mu-pz_wa3541
_cod_depositor_comments
'Adding full bibliography for 1573178--1573190.cif.'
_cod_original_cell_volume        2512.0(5)
_cod_original_formula_sum        'C23 H29 Al2 K N2 O1.50'
_cod_database_code               1573180
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.957
_oxdiff_twin_integration_method  simultaneous
_shelx_res_checksum              29966
_shelx_hkl_checksum              19986