Reaction of a diarylgermylene with a phosphaalkyne: formation of a germadiphosphacyclobutene with an exocyclic CGe double bond
Meiners, Frank; Saak, Wolfgang; Weidenbruch, Manfred; Chemical Communications  (2001) 215–; doi:10.1039/b008472g

data_7111172
_publ_section_title
;
 Reaction of a diarylgermylene with a phosphaalkyne: formation of a
 germadiphosphacyclobutene with an exocyclic C&#xE006;Ge double bond
;
_journal_issue                   2
_journal_name_full               'Chemical Communications'
_journal_page_first              215
_journal_paper_doi               10.1039/b008472g
_journal_year                    2001
_chemical_formula_sum            'C68 H108 Ge2 P2'
_chemical_formula_weight         1132.66
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.207(5)
_cell_angle_beta                 80.276(5)
_cell_angle_gamma                87.046(6)
_cell_formula_units_Z            2
_cell_length_a                   12.1315(6)
_cell_length_b                   15.3937(8)
_cell_length_c                   17.6016(7)
_cell_measurement_temperature    193(2)
_cell_volume                     3232.9(3)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'XRED (Stoe, 1997)'
_computing_molecular_graphics    'Oretp-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Stoe IPDS'
_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  0.0782
_diffrn_reflns_av_sigmaI/netI    0.1023
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39739
_diffrn_reflns_theta_full        25.92
_diffrn_reflns_theta_max         25.92
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  0.8625
_exptl_absorpt_correction_T_min  0.7368
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         11735
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1064
_reflns_number_gt                6979
_reflns_number_total             11735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008472gsup1.cif
_cod_data_source_block           gemep
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111172