Picolyl-armed 1,3-alternate calix[4]areneazacrown ethers
Seung Kim, Jong; Shon, Ok Jae; Sim, Wonbo; Kyu Kim, Sun; Cho, Moon Hwan; Kim, Jin-Gyu; Suh, Il-Hwan; Kim, Dong Won; Journal of the Chemical Society, Perkin Transactions 1  (2001) 31–; doi:10.1039/b006801m

data_7216922
_publ_section_title
;
 Picolyl-armed 1,3-alternate calix[4]areneazacrown ethers
;
_journal_issue                   1
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              31
_journal_paper_doi               10.1039/b006801m
_journal_year                    2001
_chemical_formula_sum            'C49 H57 Cl K N O10'
_chemical_formula_weight         894.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 92.856(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4923(15)
_cell_length_b                   13.9235(11)
_cell_length_c                   19.913(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    288
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      11.49
_cell_volume                     4567.0(13)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        ' XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      288
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_sigmaI/netI    0.1200
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8234
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  0.9385
_exptl_absorpt_correction_T_min  0.8909
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   1
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.264
_exptl_crystal_size_min          0.264
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0007(6)
_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   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         7981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.2128
_refine_ls_R_factor_gt           0.0863
_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^)+(0.1205P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2096
_refine_ls_wR_factor_ref         0.2730
_reflns_number_gt                3298
_reflns_number_total             7981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006801m.txt
_cod_data_source_block           fuu
_cod_depositor_comments
;
 Removing the 'geom_hbond' loop since it contained incorrect values.
 An incorrectly marked comment had been previously erroneously interpreted
 as the values of this loop. The following comment was removed:

 _Least-squares planes (x,y,z in crystal coordinates) and deviations from them
 (* indicates atom used to define plane)
 
 1.2358 (0.0454) x + 3.4631 (0.0368) y + 19.1312 (0.0158) z = 15.3250 (0.0121)
 *    0.0185 (0.0044)  C2
 *    0.0101 (0.0048)  C3
 *   -0.0251 (0.0053)  C4
 *    0.0123 (0.0054)  C5
 *    0.0161 (0.0048)  C6
 *   -0.0319 (0.0046)  C7
 Rms deviation of fitted atoms =   0.0204
 
 15.0908 (0.0179) x - 5.4332 (0.0338) y + 1.1270 (0.0571) z = 6.7642 (0.0497)
 *   -0.0147 (0.0048)  C9
 *   -0.0086 (0.0051)  C10
 *    0.0229 (0.0054)  C11
 *   -0.0140 (0.0052)  C12
 *   -0.0097 (0.0047)  C13
 *    0.0241 (0.0047)  C14
 Rms deviation of fitted atoms =   0.0168
 
 - 4.1789 (0.0459) x - 1.7848 (0.0405) y + 19.3210 (0.0145) z = 17.6172 (0.0339)
 *   -0.0175 (0.0049)  C19
 *   -0.0070 (0.0059)  C20
 *    0.0188 (0.0060)  C21
 *   -0.0066 (0.0052)  C22
 *   -0.0182 (0.0046)  C23
 *    0.0304 (0.0046)  C24
 Rms deviation of fitted atoms =   0.0183
 
 - 8.8412 (0.0342) x + 11.6384 (0.0188) y - 1.8150 (0.0508) z = 0.8403 (0.0447)
 *   -0.0043 (0.0042)  C26
 *    0.0018 (0.0045)  C27
 *    0.0044 (0.0046)  C28
 *   -0.0080 (0.0044)  C29
 *    0.0053 (0.0042)  C30
 *    0.0008 (0.0042)  C31
 Rms deviation of fitted atoms =   0.0047
 
 14.1303 (0.0255) x - 7.1777 (0.0354) y - 1.1080 (0.0662) z = 2.6387 (0.0600)
 *   -0.0027 (0.0047)  C44
 *    0.0037 (0.0053)  C45
 *    0.0005 (0.0061)  C46
 *   -0.0059 (0.0065)  C47
 *    0.0068 (0.0060)  C48
 *   -0.0024 (0.0052)  C49
 Rms deviation of fitted atoms =   0.0043
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7216922