Synthesis and crystal structure of [Li(NH3)4]4[Sn9]·NH3 and [Li(NH3)4]4[Pb9]·NH3 †
Korber, Nikolaus; Fleischmann, Andrea; Journal of the Chemical Society, Dalton Transactions  (2001) 383–; doi:10.1039/b008123j

data_7010327
_publ_contact_author
;
Prof. Dr. Nikolaus Korber
Institut f. Anorganische Chemie, Universit\"at Regensburg
93040 Regensburg
Germany
;
_publ_section_title
;
 Synthesis and crystal structure of [Li(NH3)4]4[Sn9]&#x00B7;NH3 and
 [Li(NH3)4]4[Pb9]&#x00B7;NH3&#x200A;&#x2020;
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              383
_journal_paper_doi               10.1039/b008123j
_journal_year                    2001
_chemical_formula_moiety         '4 (H12 Li N4 +), (Pb9 4-), (H3 N)'
_chemical_formula_sum            'H51 Li4 N17 Pb9'
_chemical_formula_weight         2182.05
_chemical_name_systematic
; 
Tetrakis(tetraamminelithium)nonaplumbide-ammonia(1/1) 
;
_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                 99.046(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6109(8)
_cell_length_b                   17.8636(9)
_cell_length_c                   21.4144(16)
_cell_measurement_reflns_used    499
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      23.19
_cell_measurement_theta_min      11.91
_cell_volume                     4008.6(5)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1998)'
_computing_data_reduction        IPDS
_computing_publication_material  'CIFTAB in SHELXL97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       Phi
_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  0.0759
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19948
_diffrn_reflns_theta_full        25.79
_diffrn_reflns_theta_max         25.79
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    37.667
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.288
_refine_diff_density_min         -1.771
_refine_diff_density_rms         0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         7491
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0278P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0753
_reflns_number_gt                4807
_reflns_number_total             7491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008123j.txt
_cod_data_source_block           '[Li(NH~3~)~4~]~4~Pb~9~(NH~3~)'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7010327