Isolation of Free Phenylide-like Carbanions with N-Heterocyclic Carbene Frameworks
Kelly E. Krahulic; Heikki M. Tuononen; Masood Parvez; Roland Roesler; Journal of the American Chemical Society 131 (2009) 5858–5865; doi:10.1021/ja9001234

data_4104243
_publ_section_title
;
 Isolation of Free Phenylide-like Carbanions with N-Heterocyclic Carbene
 Frameworks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5858
_journal_page_last               5865
_journal_paper_doi               10.1021/ja9001234
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C59 H87 B2 K N2 O8'
_chemical_formula_sum            'C59 H87 B2 K N2 O8'
_chemical_formula_weight         1013.03
_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                74.015(10)
_cell_angle_beta                 78.738(10)
_cell_angle_gamma                68.096(11)
_cell_formula_units_Z            2
_cell_length_a                   11.411(2)
_cell_length_b                   13.544(2)
_cell_length_c                   21.362(4)
_cell_measurement_reflns_used    10586
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      3.66
_cell_volume                     2928.8(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        DENZO-SMN
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'KappaCCD (Nonius, FR540C)'
_diffrn_measurement_method       'phi\omega scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'Enraf Nonius FR590D, fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19568
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         3.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.9719
_exptl_absorpt_correction_T_min  0.9665
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         10586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.091
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.9700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                7646
_reflns_number_total             10586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9001234_si_004.cif
_cod_data_source_block           4b
_cod_database_code               4104243