Synthesis and Structural Characterization of a Series of Dimeric Metal(II) Imido Complexes {M(μ-NAr#)}2 [M = Ge, Sn, Pb; Ar#= C6H3-2,6-(C6H2-2,4,6-Me3)2] and the Related Monomeric Primary Amido Derivatives M{N(H)Ar#}2 (M = Ge, Sn, Pb): Spectroscopic Manifestations of Secondary Metal-Ligand Interactions
William A. Merrill; Robert J. Wright; Corneliu S. Stanciu; Marilyn M. Olmstead; James C. Fettinger; Philip P. Power; Inorganic Chemistry 49 (2010) 7097–7105; doi:10.1021/ic100831c

data_4316142
_publ_section_title
;
 Synthesis and Structural Characterization of a Series of Dimeric
 Metal(II) Imido Complexes {M(\m-NAr#)}2 [M = Ge, Sn, Pb; Ar#=
 C6H3-2,6-(C6H2-2,4,6-Me3)2] and the Related Monomeric Primary Amido
 Derivatives M{N(H)Ar#}2 (M = Ge, Sn, Pb): Spectroscopic Manifestations of
 Secondary Metal-Ligand Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7097
_journal_page_last               7105
_journal_paper_doi               10.1021/ic100831c
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C48 H52 Ge N2'
_chemical_formula_sum            'C48 H52 Ge N2'
_chemical_formula_weight         729.51
_chemical_name_common            'Compound 4'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 123.311(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0482(8)
_cell_length_b                   15.1138(6)
_cell_length_c                   16.7892(7)
_cell_measurement_reflns_used    5006
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.2
_cell_measurement_theta_min      2.5
_cell_volume                     4039.3(3)
_computing_cell_refinement       'Apex2 (Bruker, 2004)'
_computing_data_collection       'Apex2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXLTL 6.1 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART Apex II'
_diffrn_measurement_method       \w
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22455
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_T_max  0.8837
_exptl_absorpt_correction_T_min  0.7634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         5889
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+2.5696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                4927
_reflns_number_total             5889
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100831c_si_001_4.cif
_cod_data_source_block           jf1308
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4316142