Syntheses and ligand exchange experiments of N,N-dialkylcarbamate bridged {Al3(μ3-O)}7+ complexes
Schumann, Erik; Böhme, Uwe; Brendler, Erica; Mertens, Florian; New Journal of Chemistry 47 (2023) 16981–16992; doi:10.1039/D3NJ02389C

data_7062672
_publ_section_title
;
 Syntheses and ligand exchange experiments of N,N-dialkylcarbamate bridged
 {Al3(\m3-O)}7+ complexes
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16981
_journal_page_last               16992
_journal_paper_doi               10.1039/D3NJ02389C
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C51 H93 Al3 N9 O13, 11(C H Cl3), Cl'
_chemical_formula_sum            'C62 H104 Al3 Cl34 N9 O13'
_chemical_formula_weight         2469.78
_chemical_melting_point          470
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-04-19 deposited with the CCDC.	2023-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.2329(3)
_cell_length_b                   15.2329(3)
_cell_length_c                   27.0649(5)
_cell_measurement_reflns_used    31630
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.68
_cell_volume                     5438.79(18)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      153
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      ' 343 frames, detector distance = 119 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            65373
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.271
_diffrn_reflns_theta_min         2.674
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.8573
_exptl_absorpt_correction_T_min  0.7510
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-RED; Stoe, 2009'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Refined as an inversion twin. 
 Flack test results are ambiguous with a Flack parameter 
 of 0.46(5). Therefore, the absolute structure parameter
 was removed from the CIF.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7788
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+2.0308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7178
_reflns_number_total             7788
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02389c2.cif
_cod_data_source_block           ES0114h_k2
_cod_depositor_comments
'Adding full bibliography for 7062672--7062674.cif.'
_cod_original_cell_volume        5438.8(2)
_cod_database_code               7062672
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.681
_shelx_estimated_absorpt_t_max   0.738
_shelx_res_checksum              19447