Stable Germenolates and Germenes with Exocyclic Structures
Haas, Michael; Leypold, Mario; Schnalzer, Dominik; Torvisco, Ana; Stueger, Harald; Organometallics 34 (2015) 5291–; doi:10.1021/acs.organomet.5b00750

data_4087948
_publ_section_title
;
 Stable Germenolates and Germenes with Exocyclic Structures
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5291
_journal_paper_doi               10.1021/acs.organomet.5b00750
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C34 H73 Ge2 K O7 Si6, C7 H8'
_chemical_formula_sum            'C41 H81 Ge2 K O7 Si6'
_chemical_formula_weight         1038.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-01-28 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 92.703(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0779(12)
_cell_length_b                   23.527(3)
_cell_length_c                   23.354(3)
_cell_measurement_reflns_used    9287
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.33
_cell_volume                     5531.1(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1674
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            112336
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.332
_exptl_absorpt_coefficient_mu    1.332
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       plate
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.552
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         9717
_refine_ls_number_restraints     702
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0646
_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^)+(0.1093P)^2^+2.5635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6698
_reflns_number_total             9717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00750_si_001.cif
_cod_data_source_block           AT378_a_a_a
_cod_original_cell_volume        5531.1(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4087948
_publcif_datablock.id            {5e3711f3-6f6e-4074-9a7b-91fe1193cf93}
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.878
_shelx_estimated_absorpt_t_max   0.961
_shelx_res_checksum              40199
_shelx_hkl_checksum              96984