Synthesis and Characterization of Ge(II), Sn(II), and Pb(II) Monoamides with -NH2 Ligands
Stanciu, Corneliu; Hino, Shirley S.; Stender, Matthias; Richards, Anne F.; Olmstead, Marilyn M.; Power, Philip P.; Inorganic Chemistry 44 (2005) 2774–2780; doi:10.1021/ic048362l

data_4300801
_publ_section_title
;
 Synthesis and Characterization of Ge(II), Sn(II), and Pb(II)
 Monoamides with -NH2 Ligands
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2774
_journal_page_last               2780
_journal_paper_doi               10.1021/ic048362l
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C60 H78 Ge2 N2, 1.5(C7 H8)'
_chemical_formula_sum            'C70.5 H90 Ge2 N2'
_chemical_formula_weight         1110.63
_chemical_name_common            '[(Dipp*GeNH2)2].1.5toluene'
_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                 114.265(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   43.490(5)
_cell_length_b                   16.840(2)
_cell_length_c                   18.469(2)
_cell_measurement_reflns_used    985
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      2.5
_cell_volume                     12331(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.45A (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            58631
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4728
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         11141
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+27.5399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                7896
_reflns_number_total             11141
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic048362lsi20041118_070255.cif
_cod_data_source_block           ar118
_cod_original_cell_volume        12331(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C70.50 H90 Ge2 N2'
_cod_database_code               4300801