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_4321914
_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)0.5'
_chemical_formula_sum            'C109 H218 Ge18 K6 N13 O36'
_chemical_formula_weight         3828.18
_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                87.485(9)
_cell_angle_beta                 79.168(9)
_cell_angle_gamma                85.415(8)
_cell_formula_units_Z            2
_cell_length_a                   14.3970(10)
_cell_length_b                   19.765(2)
_cell_length_c                   28.898(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    213(2)
_cell_volume                     8047.3(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_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  0.0894
_diffrn_reflns_av_sigmaI/netI    0.1063
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_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            43103
_diffrn_reflns_theta_full        24.02
_diffrn_reflns_theta_max         24.02
_diffrn_reflns_theta_min         3.91
_exptl_absorpt_coefficient_mu    3.528
_exptl_absorpt_correction_type   'STOE DECAY 0'
_exptl_crystal_colour            deep_brown
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3882
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.100
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1619
_refine_ls_number_reflns         23330
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1274
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.280
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+35.4135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.2053
_reflns_number_gt                14150
_reflns_number_total             23330
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic981157j_1.cif
_cod_data_source_block           ge9-brown
_cod_database_code               4321914