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_7108486
_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
;
3(C12 H27 O6 N Cs), C12 H30 O6 N2 Cs,
Sn4 Bi4, 7(NH3)
;
_chemical_formula_sum            'C48 H132 Bi4 Cs4 N12 O24 Sn4'
_chemical_formula_weight         3103.98
_chemical_name_common
;
tetrakis((1,4,7,10,13,16-hexaoxacyclooctadecane)-cesium)
tetra-bismuth-tetra-tin ammoniate
;
_chemical_name_systematic
;
tetrakis((1,4,7,10,13,16-hexaoxacyclooctadecane)-cesium)
tetra-bismuth-tetra-tin ammoniate
;
_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
_audit_update_record
;
2012-02-13 # Formatted by publCIF
;
_cell_angle_alpha                72.4420(10)
_cell_angle_beta                 87.7930(10)
_cell_angle_gamma                62.5700(10)
_cell_formula_units_Z            2
_cell_length_a                   15.5211(2)
_cell_length_b                   16.7664(2)
_cell_length_c                   21.7756(2)
_cell_measurement_reflns_used    25671
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      2.70
_cell_volume                     4761.41(11)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_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  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            691240
_diffrn_reflns_theta_full        29.53
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    9.964
_exptl_absorpt_correction_T_max  0.354
_exptl_absorpt_correction_T_min  0.149
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.559
_refine_diff_density_min         -2.312
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         25670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0345P)^2^+39.2621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                20919
_reflns_number_total             25670
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35380f.txt
_cod_data_source_block           Sn4Bi4(4-)
_cod_original_cell_volume        4761.41(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7108486