An Intramolecularly Base-Stabilized Diphosphagermylene and Two Unusual Germanium(II) Ate Complexes: A Structural, NMR, and DFT Study
Izod, Keith; McFarlane, William; Allen, Ben; Clegg, William; Harrington, Ross W.; Organometallics 24 (2005) 2157–2167; doi:10.1021/om0501125

data_1100899
_publ_section_title
;
 An Intramolecularly Base-Stabilized Diphosphagermylene and Two Unusual
 Germanium(II) Ate Complexes: A Structural, NMR, and DFT Study
;
_journal_coden_ASTM              ORGND7
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2157
_journal_page_last               2167
_journal_paper_doi               10.1021/om0501125
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C32 H62 Ge N2 P2 Si4, 0.5 C7 H14'
_chemical_formula_sum            'C35.5 H69 Ge N2 P2 Si4'
_chemical_formula_weight         770.82
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                78.569(1)
_cell_angle_beta                 89.576(1)
_cell_angle_gamma                75.536(1)
_cell_formula_units_Z            2
_cell_length_a                   11.4596(5)
_cell_length_b                   12.0029(5)
_cell_length_c                   16.3524(7)
_cell_measurement_reflns_used    13588
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9
_cell_measurement_theta_min      2.16
_cell_volume                     2132.65(16)
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15612
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         9401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0417P)^2^+0.8715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                8637
_reflns_number_total             9401
_reflns_threshold_expression     I>2\s(I)
_cod_database_code               1100899