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_4067237
_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         'C60 H64 Br2 Mg2 O6,  0.6(C4 H10 O2)'
_chemical_formula_sum            'C62.4 H70 Br2 Mg2 O7.2'
_chemical_formula_weight         1143.60
_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                87.816(3)
_cell_angle_beta                 79.614(3)
_cell_angle_gamma                76.216(3)
_cell_formula_units_Z            1
_cell_length_a                   7.5104(3)
_cell_length_b                   10.7441(5)
_cell_length_c                   19.2715(9)
_cell_measurement_reflns_used    10104
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.85
_cell_volume                     1485.52(12)
_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      183(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0835
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10104
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             596.0
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.288
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0919P)^2^+0.8244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1753
_reflns_number_gt                4446
_reflns_number_total             6602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1009632_si_001.cif
_cod_data_source_block           FO3703
_cod_original_cell_volume        1485.52(11)
_cod_original_formula_sum        'C62.40 H70 Br2 Mg2 O7.20'
_cod_database_code               4067237