Evidence for the first oxidative insertion of a transition metal into a digallane(4): synthesis, structural characterisation and EPR studies of [Cp2ZrIII{Ga[N(Ar)C(H)]2}2][Li(THF)4], Ar = C6H3Pri2-2,6
Baker, Robert J.; Jones, Cameron; Murphy, Damien M.; Chemical Communications  (2005) 1339–1341; doi:10.1039/b417720g

data_7111482
_publ_section_title
;
 Evidence for the first oxidative insertion of a transition metal into a
 digallane(4): synthesis, structural characterisation and EPR studies of
 [Cp2ZrIII{Ga[N(Ar)C(H)]2}2][Li(THF)4], Ar = C6H3Pri2-2,6
;
_journal_issue                   10
_journal_name_full               'Chemical Communications'
_journal_page_first              1339
_journal_page_last               1341
_journal_paper_doi               10.1039/b417720g
_journal_year                    2005
_chemical_formula_sum            'C85 H121 Ga2 Li N4 O4 Zr'
_chemical_formula_weight         1500.46
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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                 105.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.171(3)
_cell_length_b                   21.373(4)
_cell_length_c                   26.866(5)
_cell_measurement_temperature    150(2)
_cell_volume                     8409(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            55600
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00000(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         16371
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+13.3909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                12291
_reflns_number_total             16371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b417720gsup1.cif
_cod_data_source_block           compound_4
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7111482