Versatile 1,2- and 1,3-Dipole Behavior of the 1-Arsa-3-Germaallene Tip(t-Bu)Ge═C═AsMes*: Formation of a Heterocyclic Arsa(germa)carbene (AsGeHC)
Ghereg, Dumitru; Sotiropoulos, Jean-Marc; Escudié, Jean; Miqueu, Karinne; Matioszek, Dimitri; Ladeira, Sonia; Saffon-Merceron, Nathalie; Organometallics 31 (2012) 930–; doi:10.1021/om200968x

data_4067970
_publ_section_title
;
 Versatile 1,2- and 1,3-Dipole Behavior of the 1-Arsa-3-Germaallene
 Tip(t-Bu)Ge&#x2550;C&#x2550;AsMes*: Formation of a Heterocyclic
 Arsa(germa)carbene (AsGeHC)
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              930
_journal_paper_doi               10.1021/om200968x
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C51 H69 As Ge O, C4 H10 O'
_chemical_formula_sum            'C55 H79 As Ge O2'
_chemical_formula_weight         919.71
_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                77.202(4)
_cell_angle_beta                 85.813(4)
_cell_angle_gamma                82.062(4)
_cell_formula_units_Z            2
_cell_length_a                   10.1766(10)
_cell_length_b                   12.5486(12)
_cell_length_c                   20.381(2)
_cell_measurement_reflns_used    9489
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.46
_cell_measurement_wavelength     0.71073
_cell_volume                     2511.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33681
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         5.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_T_max  0.9744
_exptl_absorpt_correction_T_min  0.8594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         10088
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0334P)^2^+1.5176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                7739
_reflns_number_total             10088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200968x_si_002.cif
_cod_data_source_block           3
_cod_database_code               4067970