Hydroxy-substituted triarylcarbenium bromides. Synthesis, structure, derivatization and facile conversion to highly substituted xanthenes †
Dinger, Maarten B.; Scott, Michael J.; Journal of the Chemical Society, Perkin Transactions 1  (2000) 1741–; doi:10.1039/b001032o

data_7213277
_publ_section_title
;
 Hydroxy-substituted triarylcarbenium bromides. Synthesis, structure,
 derivatization and facile conversion to highly substituted
 xanthenes&#x200A;&#x2020;
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1741
_journal_paper_doi               10.1039/b001032o
_journal_year                    2000
_chemical_formula_sum            'C40 H58 O6'
_chemical_formula_weight         634.86
_space_group_IT_number           2
_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
_cell_angle_alpha                96.0340(10)
_cell_angle_beta                 94.0770(10)
_cell_angle_gamma                110.7520(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2038(6)
_cell_length_b                   13.5294(8)
_cell_length_c                   14.9405(9)
_cell_measurement_temperature    173(2)
_cell_volume                     1905.0(2)
_computing_cell_refinement       'Bruker AXS SMART  '
_computing_data_collection       ' Bruker AXS SMART '
_computing_data_reduction        ' Bruker AXS SMART  '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10563
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0054(18)
_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   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0789P)^2^+1.7326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1911
_reflns_number_gt                4830
_reflns_number_total             6651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001032osup1.cif
_cod_data_source_block           4a.2Me2CO
_cod_database_code               7213277