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_7702856
_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            'C88 H144 Ga2 K2 N4 O18'
_chemical_formula_weight         1763.72
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.70(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.844(4)
_cell_length_b                   26.080(5)
_cell_length_c                   17.719(4)
_cell_measurement_temperature    150(2)
_cell_volume                     9317(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0964
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            137685
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.9303
_exptl_absorpt_correction_T_min  0.8101
_exptl_absorpt_correction_type   'Sortav (Blessing 1995)'
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         21191
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+18.0496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1565
_reflns_number_gt                14543
_reflns_number_total             21191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206605j.txt
_cod_data_source_block           compound13
_cod_original_cell_volume        9317(3)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7702856