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_7052392
_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 K2'
_chemical_formula_sum            'C36 H84 Ge5 K2 N8 O12'
_chemical_formula_weight         1262.26
_chemical_name_common
;
Bis(potassium-(4,7,13,1621,24-Hexaoxa-1,10-
diazabicyclo(8.8.8)hexacosane))-nonagermanid - ammonia(1/4)
;
_chemical_name_systematic
;
Bis[potassium-(4,7,13,1621,24-Hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)]-
nonagermanid - ammonia(1/4)
;
_space_group_IT_number           1
_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                117.911(8)
_cell_angle_beta                 98.650(9)
_cell_angle_gamma                91.797(9)
_cell_formula_units_Z            1
_cell_length_a                   11.2887(9)
_cell_length_b                   11.8949(9)
_cell_length_c                   11.9433(9)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      51.86
_cell_measurement_theta_min      3.90
_cell_volume                     1391.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_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  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10669
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         1.95
_diffrn_standards_interval_time  6.0
_diffrn_standards_number         8934
_exptl_absorpt_coefficient_mu    2.876
_exptl_absorpt_correction_T_max  0.649
_exptl_absorpt_correction_T_min  0.178
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(A.L.Spek, Platon 2004'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.668(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8934
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0866P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                8001
_reflns_number_total             8934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b610547e.txt
_cod_data_source_block           K-Crypt_Ge5
_cod_original_cell_volume        1391.51(19)
_cod_database_code               7052392