The Reactivity of Phosphagermaallene Tip(t-Bu)Ge=C=PMes* with Doubly and Triply Bonded Nitrogen Compounds
Dumitru Ghereg; Heinz Gornitzka; Jean Escudié; Sonia Ladeira; Inorganic Chemistry 49 (2010) 10497–10505; doi:10.1021/ic1014913

data_4317039
_publ_section_title
;
 The Reactivity of Phosphagermaallene Tip(t-Bu)Ge=C=PMes* with Doubly and
 Triply Bonded Nitrogen Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10497
_journal_page_last               10505
_journal_paper_doi               10.1021/ic1014913
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C40 H64 Ge N P'
_chemical_formula_sum            'C40 H64 Ge N P'
_chemical_formula_weight         662.50
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90
_cell_angle_beta                 113.189(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.710(16)
_cell_length_b                   9.831(8)
_cell_length_c                   19.999(15)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      31.86
_cell_measurement_theta_min      2.21
_cell_measurement_wavelength     0.71073
_cell_volume                     3924(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            101060
_diffrn_reflns_theta_full        36.83
_diffrn_reflns_theta_max         36.83
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         19550
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.9811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                13205
_reflns_number_total             19550
_reflns_threshold_expression     >2/sigma(I)
_cod_data_source_file            ic1014913_si_001_3.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4317039