Regioselectively N-methylated azacalix[8]arene octamethyl ether prepared by catalytic aryl amination reaction using a temporal N-silylation protocol.
Ishibashi, Koichi; Tsue, Hirohito; Tokita, Satoshi; Matsui, Kazuhiro; Takahashi, Hiroki; Tamura, Rui; Organic letters 8 (2006) 5991–5994; doi:10.1021/ol062459p

data_1506311
_publ_section_title
;
 Regioselectively N-methylated azacalix[8]arene octamethyl ether prepared
 by catalytic aryl amination reaction using a temporal N-silylation
 protocol.
;
_journal_issue                   26
_journal_name_full               'Organic letters'
_journal_page_first              5991
_journal_page_last               5994
_journal_paper_doi               10.1021/ol062459p
_journal_volume                  8
_journal_year                    2006
_chemical_formula_moiety         'C105.50 H143 N8 O8.50 '
_chemical_formula_sum            'C105.5 H143 N8 O8.5'
_chemical_formula_weight         1659.34
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 102.267(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   24.468(2)
_cell_length_b                   24.214(3)
_cell_length_c                   19.3043(19)
_cell_measurement_reflns_used    26792
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     11176(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.789
_diffrn_measured_fraction_theta_max 0.789
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.135
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51919
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.986
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3600.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.89
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     578
_refine_ls_number_reflns         11618
_refine_ls_R_factor_gt           0.1226
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3856
_reflns_number_gt                5493
_reflns_number_total             10111
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol062459psi20061006_055645.cif
_cod_data_source_block           '_NMe4H4-ACA8-OMe'
_cod_original_cell_volume        11175.8(20)
_cod_original_formula_sum        'C105.50 H143 N8 O8.50 '
_cod_database_code               1506311