Carbene-Stabilized Beryllium Borohydride
Robert J. Gilliard; Mariham Y. Abraham; Yuzhong Wang; Pingrong Wei; Yaoming Xie; Brandon Quillian; Henry F. Schaefer; Paul v. R. Schleyer; Gregory H. Robinson; Journal of the American Chemical Society 134 (2012) 9953–9955; doi:10.1021/ja304514f

data_4118111
_publ_section_title
;
 Carbene-Stabilized Beryllium Borohydride
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9953
_journal_page_last               9955
_journal_paper_doi               10.1021/ja304514f
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C54 H77 B N4'
_chemical_formula_weight         793.01
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.1000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4807(7)
_cell_length_b                   23.1679(12)
_cell_length_c                   17.7375(10)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.961
_cell_measurement_theta_min      2.297
_cell_volume                     5127.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER SMART APEX II'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57706
_diffrn_reflns_theta_full        25.60
_diffrn_reflns_theta_max         25.60
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.059
_exptl_absorpt_correction_T_max  0.9918
_exptl_absorpt_correction_T_min  0.9797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.027
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0066(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         9641
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+0.9169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                7051
_reflns_number_total             9641
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja304514f_si_004.cif
_cod_data_source_block           j1
_cod_database_code               4118111