Aluminum and Gallium Hydrazides as Active Lewis Pairs: Cooperative C‒H Bond Activation with H‒C≡C‒Ph and Pentafluorobenzene
Uhl, Werner; Willeke, Matthias; Hengesbach, Frank; Hepp, Alexander; Layh, Marcus; Organometallics 35 (2016) 3701–; doi:10.1021/acs.organomet.6b00658

data_4089033
_publ_section_title
;
 Aluminum and Gallium Hydrazides as Active Lewis Pairs: Cooperative C--H
 Bond Activation with H--C\\tb C--Ph and Pentafluorobenzene
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              3701
_journal_paper_doi               10.1021/acs.organomet.6b00658
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C21 H39 Al N2 O'
_chemical_formula_weight         362.52
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.5768(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4956(3)
_cell_length_b                   24.8278(12)
_cell_length_c                   12.7550(6)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.065
_cell_measurement_theta_min      2.293
_cell_volume                     2050.46(17)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32110
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.102
_diffrn_reflns_theta_min         2.937
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.6017
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         6004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0521P)^2^+0.8314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5004
_reflns_number_total             6004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00658_si_001.cif
_cod_data_source_block           sad_(compound_3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089033
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              79951
_shelx_hkl_checksum              2786