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_4089036
_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            'C28 H27 F10 Ga N2'
_chemical_formula_weight         651.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                82.4720(13)
_cell_angle_beta                 72.5308(12)
_cell_angle_gamma                79.9641(12)
_cell_formula_units_Z            2
_cell_length_a                   10.1498(4)
_cell_length_b                   10.9810(5)
_cell_length_c                   12.7022(5)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.138
_cell_measurement_theta_min      2.309
_cell_volume                     1325.09(10)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.989
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21588
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.077
_diffrn_reflns_theta_min         2.125
_diffrn_source                   mircosource
_exptl_absorpt_coefficient_mu    1.131
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         7697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0464P)^2^+0.5219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6565
_reflns_number_total             7697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00658_si_001.cif
_cod_data_source_block           sad-1_(compound_7a)
_cod_database_code               4089036
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.742
_shelx_estimated_absorpt_t_max   0.886
_shelx_res_checksum              16440
_shelx_hkl_checksum              47475