Synthesis of low-oxidation-state germanium clusters comprising a functional anchor group - synthesis and characterization of [(Ge<sup>0</sup>)<sub>5</sub>(Ge-R)<sub>3</sub>(Ge-(CH<sub>2</sub>)<sub>n</sub>-CH[double bond, length as m-dash]CH<sub>2</sub>)] with R = Si(SiMe<sub>3</sub>)<sub>3</sub>.
Frischhut, Sabine; Fässler, Thomas F; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3223–3226; doi:10.1039/c8dt00321a

data_7045508
_publ_section_title
;
 Synthesis of low-oxidation-state germanium clusters comprising a
 functional anchor group - synthesis and characterization of
 [(Ge<sup>0</sup>)<sub>5</sub>(Ge-R)<sub>3</sub>(Ge-(CH<sub>2</sub>)<sub>n</sub>-CH[double
 bond, length as m-dash]CH<sub>2</sub>)] with R =
 Si(SiMe<sub>3</sub>)<sub>3</sub>.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3223
_journal_page_last               3226
_journal_paper_doi               10.1039/c8dt00321a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C32 H90 Ge9 Si12'
_chemical_formula_sum            'C32 H90 Ge9 Si12'
_chemical_formula_weight         1465.42
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-28 deposited with the CCDC.
2018-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0667(7)
_cell_length_b                   17.5351(8)
_cell_length_c                   23.8145(11)
_cell_measurement_reflns_used    9080
_cell_measurement_temperature    151(2)
_cell_measurement_theta_max      29.88
_cell_measurement_theta_min      2.43
_cell_volume                     6709.3(5)
_computing_cell_refinement       'SAINT (Bruker, 2012b)'
_computing_data_collection       'APEX II Control Software (Bruker, 2012a)'
_computing_data_reduction        'SAINT (Bruker, 2012b)'
_computing_molecular_graphics    'Diamond 3.2i (Brandenburg & Putz, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      151(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f- and \w-rotation'
_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  0.0419
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            286703
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         1.442
_exptl_absorpt_coefficient_mu    4.207
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
absorption correction with SADABS, Bruker AXS Inc., Madison, WI (2001). 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.508(5)
_refine_ls_extinction_coef       0.00014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         16198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0174
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+1.8894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0441
_reflns_number_gt                15370
_reflns_number_total             16198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00321a2.cif
_cod_data_source_block           PSF200
_cod_depositor_comments          'Adding full bibliography for 7045508.cif.'
_cod_database_code               7045508
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              85322