Subvalent Group 13 Molecules by Carbene-induced Hydrogen Abstraction
Werner, Luis; Hock, Andreas; Luz, Christian; Riethmann, Melanie; Radius, Udo; Dalton Transactions  (2023) –; doi:10.1039/D3DT00765K

data_7712757
_publ_section_title
;
 Subvalent Group 13 Molecules by Carbene-induced Hydrogen Abstraction
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00765K
_journal_year                    2023
_chemical_formula_moiety         'C30 H48 Al N'
_chemical_formula_sum            'C30 H48 Al N'
_chemical_formula_weight         449.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-03-13 deposited with the CCDC.	2023-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.2150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1032(2)
_cell_length_b                   16.9744(3)
_cell_length_c                   14.8699(2)
_cell_measurement_reflns_used    11153
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.9950
_cell_measurement_theta_min      4.8220
_cell_volume                     2758.11(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13947
_diffrn_reflns_point_group_measured_fraction_full 0.760
_diffrn_reflns_point_group_measured_fraction_max 0.760
_diffrn_reflns_theta_full        70.075
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         4.813
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 1298 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         3989
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.6430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.518
_reflns_Friedel_fraction_full    0.520
_reflns_Friedel_fraction_max     0.520
_reflns_number_gt                3909
_reflns_number_total             3989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00765k2.cif
_cod_data_source_block           compound_15
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7712757
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              15939
_shelx_hkl_checksum              10012