In situ Ge‒Ge bond formation under ambient conditions: synthesis, characterization and reactivity of organo-functionalized telluridogermanate complexes
Heimann, Samuel; Holynska, Malgorzata; Dehnen, Stefanie; Chemical Communications (Cambridge, United Kingdom) 47 (2011) 1881–1883; doi:10.1039/c0cc03727c

data_7105923
_publ_section_title
;
 In situ Ge--Ge bond formation under ambient conditions:
 synthesis, characterization and reactivity of organo-functionalized
 telluridogermanate complexes
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   6
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1881
_journal_page_last               1883
_journal_paper_doi               10.1039/c0cc03727c
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C20 H20 Ge4 O16 Te5, 2(C4 H8 O)'
_chemical_formula_sum            'C28 H36 Ge4 O18 Te5'
_chemical_formula_weight         1588.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.57(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.901(4)
_cell_length_b                   23.406(6)
_cell_length_c                   19.298(5)
_cell_measurement_reflns_used    14918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.24
_cell_measurement_theta_min      3.08
_cell_volume                     5375(3)
_computing_cell_refinement       'Stoe, X-Area ver. 1.54'
_computing_data_collection       'Stoe, X-Area ver. 1.54'
_computing_data_reduction        'Stoe, X-Area ver. 1.54'
_computing_molecular_graphics    'DIAMOND 3.1'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  IPDS2
_diffrn_measurement_method       /w
_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  0.2528
_diffrn_reflns_av_sigmaI/netI    0.3767
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32249
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.68
_exptl_absorpt_coefficient_mu    4.930
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.47
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.643
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8337
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.643
_refine_ls_R_factor_all          0.2188
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1418
_reflns_number_gt                2357
_reflns_number_total             8337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC03727C.TXT
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7105923