Ge52? Zintl anions: synthesis and crystal structures of [K([2.2.2]-crypt)]2Ge5?4NH3 and [Rb([2.2.2]-crypt)]2Ge5?4NH3
Suchentrunk, Christof; Korber, Nikolaus; New Journal of Chemistry 30 (2006) 1737–; doi:10.1039/b610547e

data_7052393
_publ_section_title
;
 Ge52? Zintl anions: synthesis and crystal structures of
 [K([2.2.2]-crypt)]2Ge5?4NH3 and [Rb([2.2.2]-crypt)]2Ge5?4NH3
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1737
_journal_paper_doi               10.1039/b610547e
_journal_volume                  30
_journal_year                    2006
_chemical_formula_moiety         'C36 H84 Ge5 N8 O12 Rb2'
_chemical_formula_sum            'C36 H84 Ge5 N8 O12 Rb2'
_chemical_formula_weight         1355.00
_chemical_name_common
;
Bis(rubidium-(4,7,13,1621,24-Hexaoxa-1,10-
diazabicyclo(8.8.8)hexacosane))-nonagermanid - ammonia(1/4)
;
_chemical_name_systematic
;
Bis[rubidium-(4,7,13,1621,24-Hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)]-
nonagermanid - ammonia(1/4)
;
_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                89.183(13)
_cell_angle_beta                 83.60(2)
_cell_angle_gamma                78.266(15)
_cell_formula_units_Z            2
_cell_length_a                   11.3169(15)
_cell_length_b                   12.3333(15)
_cell_length_c                   20.915(3)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      51.84
_cell_measurement_theta_min      3.88
_cell_volume                     2840.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_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  0.0749
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36788
_diffrn_reflns_theta_full        25.92
_diffrn_reflns_theta_max         25.92
_diffrn_reflns_theta_min         1.94
_diffrn_standards_interval_time  7
_diffrn_standards_number         10249
_exptl_absorpt_coefficient_mu    4.374
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.216
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(A.L.Spek, Platon 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         10249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                7057
_reflns_number_total             10249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b610547e.txt
_cod_data_source_block           Rb_crypt_Ge5
_cod_database_code               7052393