The reactivity of diazabutadienes toward low oxidation state Group 13 iodides and the synthesis of a new gallium(i) carbene analogue
Baker, Robert J.; Farley, Robert D.; Jones, Cameron; Kloth, Marc; Murphy, Damien M.; Journal of the Chemical Society, Dalton Transactions  (2002) 3844–; doi:10.1039/b206605j

data_7702857
_publ_section_title
;
 The reactivity of diazabutadienes toward low oxidation state Group 13
 iodides and the synthesis of a new gallium(i) carbene analogue
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3844
_journal_paper_doi               10.1039/b206605j
_journal_year                    2002
_chemical_formula_sum            'C64 H104 Ga2 K2 N8'
_chemical_formula_weight         1203.20
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                82.22(3)
_cell_angle_beta                 62.52(3)
_cell_angle_gamma                66.93(3)
_cell_formula_units_Z            1
_cell_length_a                   12.615(3)
_cell_length_b                   12.650(3)
_cell_length_c                   12.727(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1655.2(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0895
_diffrn_reflns_av_sigmaI/netI    0.0785
_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       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18217
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    0.982
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   'Sortav (Blessing)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         '1.628 (near Ga1)'
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5715
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+3.7586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                4578
_reflns_number_total             5715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206605j.txt
_cod_data_source_block           compound12
_cod_original_cell_volume        1655.1(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702857