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_4327995
_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         'C64 H78 Ge2 N4'
_chemical_formula_sum            'C64 H78 Ge2 N4'
_chemical_formula_weight         1048.48
_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                 120.555(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8962(6)
_cell_length_b                   20.0041(9)
_cell_length_c                   23.8699(10)
_cell_measurement_reflns_used    4371
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      21.33
_cell_measurement_theta_min      2.51
_cell_volume                     5714.0(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1258
_diffrn_reflns_av_sigmaI/netI    0.0750
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            79103
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.9373
_exptl_absorpt_correction_T_min  0.8444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         11671
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0671P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1309
_reflns_number_gt                8059
_reflns_number_total             11671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202138t_si_002_4.cif
_cod_data_source_block           scw394
_cod_original_cell_volume        5714.0(4)
_cod_database_code               4327995