Preferential axial protonation in a zwitterionic calix[4]arene.
Simaan, Samah; Biali, Silvio E.; Organic letters 7 (2005) 1817–1820; doi:10.1021/ol0504392

data_1506559
_publ_section_title
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 Preferential axial protonation in a zwitterionic calix[4]arene.
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_journal_issue                   9
_journal_name_full               'Organic letters'
_journal_page_first              1817
_journal_page_last               1820
_journal_paper_doi               10.1021/ol0504392
_journal_volume                  7
_journal_year                    2005
_chemical_formula_moiety         'C48 H66 N2 O4, 2(CH3 C N)'
_chemical_formula_sum            'C52 H72 N4 O4'
_chemical_formula_weight         817.14
_chemical_name_systematic
; 
 ? 
;
_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                 111.874(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.578(3)
_cell_length_b                   13.143(2)
_cell_length_c                   21.494(3)
_cell_measurement_reflns_used    6966
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.36
_cell_volume                     4870.4(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0667
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28069
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.9800
_exptl_absorpt_correction_T_min  0.9706
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         10059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+1.8271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1494
_reflns_number_gt                7971
_reflns_number_total             10059
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0504392si20050228_070926.cif
_cod_data_source_block           samach1m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4870.6(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1506559