Synthesis and characterization of pristine closo-[Ge10](2.).
Bentlohner, Manuel M.; Fischer, Christina; Fässler, Thomas F; Chemical communications (Cambridge, England) 52 (2016) 9841–9843; doi:10.1039/c6cc04143d

data_7124720
_publ_section_title
;
 Synthesis and characterization of pristine closo-[Ge10](2.).
;
_journal_issue                   63
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9841
_journal_page_last               9843
_journal_paper_doi               10.1039/c6cc04143d
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         '2(C18 H36 N2 O6 Rb), Ge10, 1.5(C2 H8 N2)'
_chemical_formula_sum            'C39 H84 Ge10 N7 O12 Rb2'
_chemical_formula_weight         1739.97
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Pyrophoric
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
;
2016-05-13 deposited with the CCDC.
2016-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                85.907(2)
_cell_angle_beta                 88.885(2)
_cell_angle_gamma                88.995(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8759(2)
_cell_length_b                   13.4395(3)
_cell_length_c                   21.2985(4)
_cell_measurement_reflns_used    14276
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      33.7021
_cell_measurement_theta_min      2.6202
_cell_volume                     3104.20(11)
_computing_cell_refinement
; 
 CrysAlis RED, Oxford Diffraction Ltd.,
 Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
 (compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
; 
 CrysAlis CCD, Oxford Diffraction Ltd.,
 Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
 (compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
; 
 CrysAlis RED, Oxford Diffraction Ltd.,
 Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
 (compiled Feb 27 2009,15:38:38)
;
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 16.0238
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Oxford Xcalibur 3'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_sigmaI/netI    0.1173
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            65291
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.380
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.69409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillar
_exptl_crystal_F_000             1714
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.118
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.855
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         11569
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                6528
_reflns_number_total             11569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc04143d2.cif
_cod_data_source_block           pmb152b
_cod_database_code               7124720
_solvent_exptl_crystal_recrystallization_method ethylenediamine/toluene