Reactivity of Digermylenes toward Potassium Graphite: Synthesis and Characterization of Germylidenide Anions
Siew-Peng Chia; Hui-Xian Yeong; Cheuk-Wai So; Inorganic Chemistry 51 (2012) 1002–1010; doi:10.1021/ic202138t

data_4327992
_publ_section_title
;
 Reactivity of Digermylenes toward Potassium Graphite: Synthesis and
 Characterization of Germylidenide Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1002
_journal_page_last               1010
_journal_paper_doi               10.1021/ic202138t
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C32 H39 Cl Ge N2'
_chemical_formula_sum            'C32 H39 Cl Ge N2'
_chemical_formula_weight         559.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 118.9330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0808(2)
_cell_length_b                   26.5379(5)
_cell_length_c                   14.0952(2)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.41
_cell_volume                     2972.78(10)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            73916
_diffrn_reflns_theta_full        30.77
_diffrn_reflns_theta_max         30.77
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.142
_exptl_absorpt_correction_T_max  0.9346
_exptl_absorpt_correction_T_min  0.8037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.651
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         9068
_refine_ls_number_restraints     380
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0854P)^2^+3.6307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1840
_reflns_number_gt                6251
_reflns_number_total             9068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202138t_si_002_1.cif
_cod_data_source_block           scw303s
_cod_database_code               4327992