Synthesis and characterization of Lewis base stabilized mono- and di-organo aluminum radicals
Kundu, Subrata; Sinhababu, Soumen; Dutta, Sayan; Mondal, Totan; Koley, Debasis; Dittrich, Birger; Schwederski, Brigitte; Kaim, Wolfgang; Stückl, A. Claudia; Roesky, Herbert W.; Chemical Communications 53 (2017) 10516–10519; doi:10.1039/C7CC06358J

data_1546907
_publ_section_title
;
 Synthesis and characterization of Lewis base stabilized mono- and
 di-organo aluminum radicals
;
_journal_issue                   76
_journal_name_full               'Chemical Communications'
_journal_page_first              10516
_journal_page_last               10519
_journal_paper_doi               10.1039/C7CC06358J
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C42 H67 Al Cl N2'
_chemical_formula_sum            'C42 H67 Al Cl N2'
_chemical_formula_weight         662.40
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-08-01 deposited with the CCDC.
2017-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.410(2)
_cell_length_b                   17.145(3)
_cell_length_c                   17.2175(5)
_cell_measurement_reflns_used    1302
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      1.4
_cell_volume                     3881.8(9)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'SHELXLE (Huebschle, 2011)'
_computing_publication_material  'enCIFer 1.5.1, CCDC, 2015'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Microdiffractometer at the SLS'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6358
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.930
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            63363
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        22.425
_diffrn_reflns_theta_max         23.408
_diffrn_reflns_theta_min         1.396
_diffrn_source                   'monochromated X-rays beamline X10SA@SLS'
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.7074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       needle
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.061
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0647P)^2^+1.6437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6995
_reflns_number_total             7291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06358j2.cif
_cod_data_source_block           skr197
_cod_original_cell_volume        3881.9(8)
_cod_database_code               1546907
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              80188