Variable ion selectivity in [N.3.3](1,3,5)crownophanes: the "breathing" process.
Xu, Jianwei; Lai, Yee-Hing; Wang, Weiling; Organic letters 5 (2003) 2781–2784; doi:10.1021/ol034424k

data_1507304
_publ_section_title
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 Variable ion selectivity in [N.3.3](1,3,5)crownophanes: the
 &quot;breathing&quot; process.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              2781
_journal_page_last               2784
_journal_paper_doi               10.1021/ol034424k
_journal_volume                  5
_journal_year                    2003
_chemical_formula_sum            'C30 H42 O5 S2'
_chemical_formula_weight         546.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           monoclinic
_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                96.557(1)
_cell_angle_beta                 99.129(1)
_cell_angle_gamma                105.923(1)
_cell_formula_units_Z            2
_cell_length_a                   10.1162(1)
_cell_length_b                   11.0901(1)
_cell_length_c                   13.6419(1)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.41
_cell_measurement_theta_min      2.26
_cell_volume                     1432.93(2)
_computing_cell_refinement       'Bruker AXS, SAINT'
_computing_data_collection       'Bruker AXS, SMART'
_computing_data_reduction        'Bruker AXS, SAINT'
_computing_molecular_graphics    'Bruker AXS, SHELXTL'
_computing_publication_material  'Bruker AXS, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.861
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_method       '\w 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  0.0153
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12928
_diffrn_reflns_theta_full        29.41
_diffrn_reflns_theta_max         29.41
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  0.9423
_exptl_absorpt_correction_T_min  0.7502
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular hexagonal blocks'
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.022(3)
_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   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         6807
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0757P)^2^+0.2516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                5509
_reflns_number_total             6807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol034424ksi20030311_021837.cif
_cod_data_source_block           lai15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1507304