The First Carbene Complex of a Diorganoberyllium: Synthesis and Structural Characterization of Ph2Be(i-Pr-carbene) and Ph2Be(n-Bu2O)
Gottfriedsen, Jochen; Blaurock, Steffen; Organometallics 25 (2006) 3784–; doi:10.1021/om0603114

data_4075475
_publ_section_title
;
 The First Carbene Complex of a Diorganoberyllium:&#x00A0; Synthesis and
 Structural Characterization of Ph2Be(i-Pr-carbene) and Ph2Be(n-Bu2O)
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3784
_journal_paper_doi               10.1021/om0603114
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C20 H28 Be O'
_chemical_formula_weight         293.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.118(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4993(9)
_cell_length_b                   10.5282(10)
_cell_length_c                   18.7174(18)
_cell_measurement_reflns_used    121
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      3.31
_cell_volume                     1823.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL PLUS'
_computing_publication_material  'Bruker SHELXTL PLUS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker CCD SMART'
_diffrn_measurement_method       'omega-, phi-scans'
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12185
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.9877
_exptl_absorpt_correction_T_min  0.9816
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0838P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1485
_reflns_number_gt                2757
_reflns_number_total             4258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0603114si20060509_120115.cif
_cod_data_source_block           c42
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4075475