Alkoxy-, acyloxy-, and bromomethylation of resorcinarenes.
Nummelin, Sami; Falabu, Deszö; Shivanyuk, Alexander; Rissanen, Kari; Organic letters 6 (2004) 2869–2872; doi:10.1021/ol049179z

data_1507070
_publ_section_title
;
 Alkoxy-, acyloxy-, and bromomethylation of resorcinarenes.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              2869
_journal_page_last               2872
_journal_paper_doi               10.1021/ol049179z
_journal_volume                  6
_journal_year                    2004
_chemical_formula_sum            'C52 H72 O12'
_chemical_formula_weight         889.10
_chemical_name_common            resorcinarene
_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                79.5820(10)
_cell_angle_beta                 85.4510(10)
_cell_angle_gamma                85.5450(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2747(2)
_cell_length_b                   12.9814(2)
_cell_length_c                   16.4661(4)
_cell_measurement_temperature    173(2)
_cell_volume                     2357.87(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Kappa CCD'
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14863
_diffrn_reflns_theta_full        25.61
_diffrn_reflns_theta_max         25.61
_diffrn_reflns_theta_min         3.84
_exptl_absorpt_coefficient_mu    0.088
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         8222
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0682P)^2^+1.8146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1433
_reflns_number_gt                6925
_reflns_number_total             8222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol049179zsi20040505_071334.cif
_cod_data_source_block           als027
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1507070