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_4071611
_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            'C45 H79 Ge N2 P Si2'
_chemical_formula_weight         807.84
_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                 93.2330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5933(4)
_cell_length_b                   22.8578(9)
_cell_length_c                   18.3221(7)
_cell_measurement_temperature    173(2)
_cell_volume                     4847.6(3)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29934
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.7551
_exptl_absorpt_correction_T_min  0.6638
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         8532
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0666P)^2^+1.4402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1259
_reflns_number_gt                6718
_reflns_number_total             8532
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800269f-file001.cif
_cod_data_source_block           COMPOUND(4)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4071611