Alkali Metal-Stabilized 1,3,5-Triphenylbenzene Monoanions: Synthesis and Characterization of the Lithium, Sodium, and Potassium Complexes†
Krieck, Sven; Görls, Helmar; Westerhausen, Matthias; Organometallics 29 (2010) 6790–; doi:10.1021/om1009632

data_4067239
_publ_section_title
;
 Alkali Metal-Stabilized 1,3,5-Triphenylbenzene Monoanions: Synthesis and
 Characterization of the Lithium, Sodium, and Potassium Complexes&#x2020;
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6790
_journal_paper_doi               10.1021/om1009632
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C16 H32 K O4, C24 H18 '
_chemical_formula_sum            'C40 H50 K O4'
_chemical_formula_weight         633.90
_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                 93.107(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7269(3)
_cell_length_b                   16.5121(7)
_cell_length_c                   19.7339(6)
_cell_measurement_reflns_used    24570
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.12
_cell_volume                     3490.2(2)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + 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  0.0747
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24570
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         7984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+1.4772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1733
_reflns_number_gt                4770
_reflns_number_total             7984
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1009632_si_001.cif
_cod_data_source_block           FO4018
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4067239