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_1507072
_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            'C61.75 H66.5 Br4 Cl11.5 O16'
_chemical_formula_weight         1791.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.0215(2)
_cell_length_b                   24.0218(3)
_cell_length_c                   36.5073(4)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    173(2)
_cell_volume                     15804.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            27843
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    2.484
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7204
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.510(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1715
_refine_ls_number_reflns         27843
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0785
_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^)+(0.1231P)^2^+49.9093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2057
_refine_ls_wR_factor_ref         0.2279
_reflns_number_gt                20462
_reflns_number_total             27843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol049179zsi20040505_071334.cif
_cod_data_source_block           als039
_cod_original_sg_symbol_H-M      P212121
_cod_original_formula_sum        'C123.50 H133 Br8 Cl23 O32'
_cod_database_code               1507072