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_4089030
_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            'C37 H62 Ga2 N4'
_chemical_formula_weight         702.34
_space_group_crystal_system      tetragonal
_space_group_IT_number           117
_space_group_name_Hall           'P -4 -2ab'
_space_group_name_H-M_alt        'P -4 b 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2929(17)
_cell_length_b                   19.2929(17)
_cell_length_c                   10.2158(9)
_cell_measurement_reflns_used    6768
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.755
_cell_measurement_theta_min      2.361
_cell_volume                     3802.5(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20112
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.122
_diffrn_reflns_theta_min         2.904
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.446
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.798
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 1900 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.107(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         5113
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0584P)^2^+3.4670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1279
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4681
_reflns_number_total             5113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00658_si_001.cif
_cod_data_source_block           sad_(compound_1c(cis))
_cod_original_cell_volume        3802.5(7)
_cod_database_code               4089030
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.696
_shelx_estimated_absorpt_t_max   0.812
_shelx_res_checksum              26601
_shelx_hkl_checksum              68977