Conformation Isomerism of Nonagermanide Ions. Crystal Structures of Brown and Red [K-([2.2.2]crypt)]6Ge9Ge9.(ethylenediamine)x (x= 0.5, 1.5)
Thomas F. Fässler; Uwe Schütz; Inorganic Chemistry 38 (1999) 1866–1870; doi:10.1021/ic981157j

data_4321915
_publ_section_title
;
 Conformation Isomerism of Nonagermanide Ions. Crystal Structures of Brown
 and Red [K-([2.2.2]crypt)]6Ge9Ge9.(ethylenediamine)x (x= 0.5, 1.5)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1866
_journal_page_last               1870
_journal_paper_doi               10.1021/ic981157j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         'Ge9 Ge9 [K-(2.2.2-crtpt)]6 (en)1.5'
_chemical_formula_sum            'C108 H216 Ge18 K6 N12 O36'
_chemical_formula_weight         3800.15
_chemical_name_systematic
; 
 ? 
;
_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                87.430(10)
_cell_angle_beta                 80.850(10)
_cell_angle_gamma                85.920(10)
_cell_formula_units_Z            2
_cell_length_a                   14.5030(10)
_cell_length_b                   19.924(2)
_cell_length_c                   28.935(3)
_cell_measurement_temperature    233(2)
_cell_volume                     8228.9(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'STOE IPDSB0 (image plate detector)'
_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  0.0829
_diffrn_reflns_av_sigmaI/netI    0.0960
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            48186
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    3.449
_exptl_absorpt_correction_type   'STOE DECAY 3'
_exptl_crystal_colour            deep_red
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3852
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.499
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1635
_refine_ls_number_reflns         24458
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0884
_refine_ls_shift/su_max          0.653
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1263P)^2^+49.3805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2334
_refine_ls_wR_factor_ref         0.2691
_reflns_number_gt                15072
_reflns_number_total             24458
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic981157j_2.cif
_cod_data_source_block           ge9-red
_cod_database_code               4321915