Reversible Addition of Alkynes to Gallium Complex of Chelating Diamide Ligand
Igor L. Fedushkin; Alexander S. Nikipelov; Konstantin A. Lyssenko; Journal of the American Chemical Society 132 (2010) 7874–7875; doi:10.1021/ja103467a

data_4102541
_publ_section_title
;
 Reversible Addition of Alkynes to Gallium Complex of Chelating Diamide
 Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7874
_journal_page_last               7875
_journal_paper_doi               10.1021/ja103467a
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C84 H96 Ga2 N4 O4, 3(C6 H6)'
_chemical_formula_sum            'C102 H114 Ga2 N4 O4'
_chemical_formula_weight         1599.41
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.086(7)
_cell_angle_beta                 76.781(8)
_cell_angle_gamma                61.731(6)
_cell_formula_units_Z            2
_cell_length_a                   15.546(6)
_cell_length_b                   15.791(6)
_cell_length_c                   21.274(8)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     4310(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector''
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2619
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            29553
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         29554
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.2192
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.2026
_reflns_number_gt                12925
_reflns_number_total             19808
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja103467a_si_004.cif
_cod_data_source_block           ethyl-2-butynoate
_cod_database_code               4102541