Synthesis, Characterization, and Reactivity of an N-Heterocyclic Germanium(II) Hydride: Reversible Hydrogermylation of a Phosphaalkyne
Choong, Sam L.; Woodul, William D.; Schenk, Christian; Stasch, Andreas; Richards, Anne F.; Jones, Cameron; Organometallics 30 (2011) 5543–; doi:10.1021/om200823x

data_4065466
_publ_section_title
;
 Synthesis, Characterization, and Reactivity of an N-Heterocyclic
 Germanium(II) Hydride: Reversible Hydrogermylation of a Phosphaalkyne
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5543
_journal_paper_doi               10.1021/om200823x
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C23 H30 Ge N2'
_chemical_formula_weight         407.08
_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                 99.41(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1930(14)
_cell_length_b                   24.351(5)
_cell_length_c                   12.147(2)
_cell_measurement_temperature    150(2)
_cell_volume                     2099.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8572
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.468
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4627
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0462P)^2^+0.3385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                2944
_reflns_number_total             4627
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200823x_si_004.cif
_cod_data_source_block           compound6
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4065466