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_7062673
_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         'C42 H74 Al3 N9 O13, 5(C6 H6), Cl'
_chemical_formula_sum            'C72 H104 Al3 Cl N9 O13'
_chemical_formula_weight         1420.03
_chemical_melting_point          496
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-07-14 deposited with the CCDC.	2023-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.685(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.0203(9)
_cell_length_b                   22.6402(6)
_cell_length_c                   27.6410(11)
_cell_measurement_reflns_used    58503
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.28
_cell_measurement_theta_min      2.74
_cell_volume                     15074.6(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      ' 203 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  0.0481
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            63158
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.279
_diffrn_reflns_theta_min         2.805
_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    0.152
_exptl_absorpt_correction_T_max  0.9816
_exptl_absorpt_correction_T_min  0.9478
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-RED; Stoe, 2009'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       Prism
_exptl_crystal_F_000             6072
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         16731
_refine_ls_number_restraints     1015
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+29.1802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12445
_reflns_number_total             16731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02389c2.cif
_cod_data_source_block           es0113p_n9
_cod_depositor_comments
'Adding full bibliography for 7062672--7062674.cif.'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7062673
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.935
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              30953