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_4067973
_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_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C52 H71 As Ge O2'
_chemical_formula_sum            'C52 H71 As Ge O2'
_chemical_formula_weight         875.62
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 99.647(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9250(6)
_cell_length_b                   23.8454(15)
_cell_length_c                   22.0595(13)
_cell_measurement_reflns_used    7481
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.18
_cell_measurement_theta_min      2.54
_cell_measurement_wavelength     0.71073
_cell_volume                     5146.9(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.1122
_diffrn_reflns_av_unetI/netI     0.1656
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38494
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         5.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_T_max  0.9511
_exptl_absorpt_correction_T_min  0.9130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.13
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.475
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.089(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1101
_refine_ls_number_reflns         19545
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.0966
_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^)+(0.0633P)^2^+26.8454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2415
_refine_ls_wR_factor_ref         0.2627
_reflns_number_gt                14884
_reflns_number_total             19545
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200968x_si_002.cif
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4067973