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_4327993
_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         'C21 H24 Cl Ge N O2'
_chemical_formula_sum            'C21 H24 Cl Ge N O2'
_chemical_formula_weight         430.45
_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                 112.2490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.9469(3)
_cell_length_b                   15.6737(3)
_cell_length_c                   18.6069(4)
_cell_measurement_reflns_used    8751
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.26
_cell_volume                     4034.55(14)
_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 0.998
_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  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            57560
_diffrn_reflns_theta_full        29.94
_diffrn_reflns_theta_max         29.94
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    1.665
_exptl_absorpt_correction_T_max  0.9364
_exptl_absorpt_correction_T_min  0.8252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.552
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         11670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0627P)^2^+1.1769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1305
_reflns_number_gt                7809
_reflns_number_total             11670
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202138t_si_002_2.cif
_cod_data_source_block           scw285s
_cod_database_code               4327993