Facile Access to a Stable Divalent Germanium Compound with a Terminal PH2Group and Related PR2Derivatives
Yao, Shenglai; Brym, Markus; Merz, Klaus; Driess, Matthias; Organometallics 27 (2008) 3601–; doi:10.1021/om800269f

data_4071613
_publ_section_title
;
 Facile Access to a Stable Divalent Germanium Compound with a Terminal
 PH2Group and Related PR2Derivatives
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3601
_journal_paper_doi               10.1021/om800269f
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C30 H41 F3 Ge N2 O3 S'
_chemical_formula_weight         639.30
_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                 92.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.087(2)
_cell_length_b                   13.013(3)
_cell_length_c                   24.046(5)
_cell_measurement_temperature    173(2)
_cell_volume                     3779.6(13)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       \w
_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  0.0889
_diffrn_reflns_av_sigmaI/netI    0.0959
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22709
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.6941
_exptl_absorpt_correction_T_min  0.6860
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.39
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6653
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0808P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1561
_reflns_number_gt                3813
_reflns_number_total             6653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800269f-file001.cif
_cod_data_source_block           COMPOUND(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4071613