Synthesis of Heteroatomic Zintl Anions in Liquid Ammonia - the New Highly Charged [Sn~4~Bi~4~]^ 4‒^ and Fully Ordered [Sn~2~Bi~2~] ^2‒^
Ute Friedrich; Maria Neumeier; Carina Koch; Nikolaus Korber; Chem.Commun. 48 (2012) 10544–; doi:10.1039/c2cc35380f

data_7108485
_publ_section_title
;
 Synthesis of Heteroatomic Zintl Anions in Liquid Ammonia - the New Highly
 Charged [Sn~4~Bi~4~]^ 4--^ and Fully Ordered [Sn~2~Bi~2~] ^2--^
;
_journal_name_full               Chem.Commun.
_journal_page_first              10544
_journal_paper_doi               10.1039/c2cc35380f
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C12 H27 K N O6, C12 H24 K O6, Sn2 Bi2, N H3'
_chemical_formula_sum            'C24 H54 Bi2 K2 N2 O12 Sn2'
_chemical_formula_weight         1296.23
_chemical_name_common
;
bis((1,4,7,10,13,16-hexaoxacyclooctadecane)-potassium) di-
bismuth-di-tin ammoniate
;
_chemical_name_systematic
;
bis((1,4,7,10,13,16-hexaoxacyclooctadecane)-potassium)
di-bismuth-di-tin ammoniate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-02-15 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4079(7)
_cell_length_b                   14.4988(10)
_cell_length_c                   27.679(2)
_cell_measurement_reflns_used    52350
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.51
_cell_measurement_theta_min      2.03
_cell_volume                     4176.8(5)
_computing_cell_refinement       'Stoe & Cie (2002)'
_computing_data_collection       'Stoe & Cie (2002)'
_computing_data_reduction        'Stoe & Cie (2002)'
_computing_molecular_graphics    'Diamond Version 2.1e (Brandenburg 2001)'
_computing_publication_material  'publCIF (version 1.9.9_c), Westrip'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'STOE IPDS I'
_diffrn_measurement_method       'rotation method'
_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  0.0958
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            52350
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    9.831
_exptl_absorpt_correction_T_max  0.34
_exptl_absorpt_correction_T_min  0.16
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
X-SHAPE and X-RED; Stoe & Cie, 1999
A numerical absorption correction based on crystal-shape optimization was
applied for all data
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         2.142
_refine_diff_density_min         -1.595
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.503(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0516P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                5897
_reflns_number_total             7458
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2cc35380f.txt
_cod_data_source_block           Sn2Bi2(2-)
_cod_database_code               7108485