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_4089035
_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            'C39 H39 Ga N2'
_chemical_formula_weight         605.44
_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                 91.1009(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6237(2)
_cell_length_b                   16.6509(3)
_cell_length_c                   16.7153(4)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.010
_cell_measurement_theta_min      3.217
_cell_volume                     3234.57(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56476
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.042
_diffrn_reflns_theta_min         2.727
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.6826
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         9459
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0351P)^2^+1.5242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8358
_reflns_number_total             9459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00658_si_001.cif
_cod_data_source_block           sad_(compound_6b)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089035
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.778
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              85953
_shelx_hkl_checksum              85510