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_4327997
_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         'C100 H134.45 Ge4 K4 N4 O12'
_chemical_formula_sum            'C100 H134.45 Ge4 K4 N4 O12'
_chemical_formula_weight         2031.33
_chemical_name_systematic
; 
 ? 
;
_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                 95.867(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8408(6)
_cell_length_b                   26.3835(8)
_cell_length_c                   25.1989(9)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      20.41
_cell_measurement_theta_min      2.12
_cell_volume                     10476.4(6)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1045
_diffrn_reflns_av_sigmaI/netI    0.1317
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            129898
_diffrn_reflns_theta_full        25.44
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    1.352
_exptl_absorpt_correction_T_max  0.9479
_exptl_absorpt_correction_T_min  0.6137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       needle
_exptl_crystal_F_000             4250
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1333
_refine_ls_number_reflns         19228
_refine_ls_number_restraints     630
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1615
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1015P)^2^+3.0160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1975
_reflns_number_gt                9782
_reflns_number_total             19228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202138t_si_002_6.cif
_cod_data_source_block           scw421s
_cod_database_code               4327997