Acyclic Germylones: Congeners of Allenes with a Central Germanium Atom
Yan Li; Kartik Chandra Mondal; Herbert W. Roesky; Hongping Zhu; Peter Stollberg; Regine Herbst-Irmer; Dietmar Stalke; Diego M. Andrada; Journal of the American Chemical Society 135 (2013) 12422–12428; doi:10.1021/ja406112u

data_4120342
_publ_contact_author_address
;Institute of Inorganic Chemistry
Georg-August-University
Tammannstrasse 4
37077 Goettingen
Germany
;
_publ_contact_author_email       hroesky@gwdg.de
_publ_contact_author_fax         +495513933373
_publ_contact_author_name        'Herbert W. Roesky'
_publ_contact_author_phone       +495513933001
_publ_section_title
;
 Acyclic Germylones: Congeners of Allenes with a Central Germanium Atom
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12422
_journal_page_last               12428
_journal_paper_doi               10.1021/ja406112u
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         '2(C40 H62 Ge N2), C6 H14'
_chemical_formula_sum            'C43 H69 Ge N2'
_chemical_formula_weight         686.59
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                112.30(3)
_cell_angle_beta                 98.13(2)
_cell_angle_gamma                91.48(2)
_cell_formula_units_Z            4
_cell_length_a                   9.161(2)
_cell_length_b                   19.325(3)
_cell_length_c                   24.760(3)
_cell_measurement_reflns_used    9557
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.613
_cell_measurement_theta_min      2.287
_cell_volume                     3999.7(15)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Smart APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 1.000
_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       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            156015
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.752
_diffrn_reflns_theta_min         1.143
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.7792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            brown_green
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       plate
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         17001
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+2.2979P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14479
_reflns_number_total             17001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja406112u_si_006.cif
_cod_data_source_block           p-1_a
_cod_original_cell_volume        3999.7(14)
_cod_database_code               4120342
_shelxl_version_number           2013-2
_shelx_res_checksum              47104