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_4316143
_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 N2 Sn'
_chemical_formula_sum            'C48 H52 N2 Sn'
_chemical_formula_weight         775.61
_chemical_name_common            'Compound 5'
_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                73.768(2)
_cell_angle_beta                 87.967(2)
_cell_angle_gamma                88.886(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7754(9)
_cell_length_b                   11.7530(11)
_cell_length_c                   18.0055(17)
_cell_measurement_reflns_used    7978
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      2.4
_cell_volume                     1984.8(3)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL 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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART 1000'
_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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22162
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.332
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         11448
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0543P)^2^+0.7337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                9621
_reflns_number_total             11448
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic100831c_si_001_5.cif
_cod_data_source_block           jf1237
_cod_database_code               4316143