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_4300802
_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         'C72 H102 N2 Sn2, C6 H14'
_chemical_formula_sum            'C78 H116 N2 Sn2'
_chemical_formula_weight         1319.11
_chemical_name_common            '[Ar*SnNH~2~]~2~.hexane'
_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                92.9780(10)
_cell_angle_beta                 93.2220(10)
_cell_angle_gamma                94.6840(10)
_cell_formula_units_Z            1
_cell_length_a                   9.7531(4)
_cell_length_b                   13.2513(5)
_cell_length_c                   13.7548(5)
_cell_measurement_reflns_used    5879
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.2
_cell_measurement_theta_min      2.5
_cell_volume                     1766.09(12)
_computing_cell_refinement       'SAINT 6.45A (Bruker, 2003)'
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13124
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0226
_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^)+(0.0295P)^2^+0.7458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0587
_reflns_number_gt                5841
_reflns_number_total             6269
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic048362lsi20041118_070318.cif
_cod_data_source_block           mas94
_cod_database_code               4300802