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_4317038
_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         'C49 H76 Ge N O P, (C4 H10 O)0.5'
_chemical_formula_sum            'C51 H81 Ge N O1.5 P'
_chemical_formula_weight         835.7704
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                97.9100(10)
_cell_angle_beta                 99.6360(10)
_cell_angle_gamma                105.7450(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9509(2)
_cell_length_b                   12.2987(2)
_cell_length_c                   19.9337(3)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.21
_cell_measurement_wavelength     0.71073
_cell_volume                     2499.67(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55247
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.11
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         9151
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+1.6385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                7786
_reflns_number_total             9151
_reflns_threshold_expression     >2/sigma(I)
_cod_data_source_file            ic1014913_si_001_2.cif
_cod_data_source_block           6
_cod_database_code               4317038