Alkali Metal Ions As Probes of Structure and Recognition Properties of Macrocyclic Pyridyl Urea Hosts
Kinkini Roy; Chun Wang; Mark D. Smith; Perry J. Pellechia; Linda S. Shimizu; Journal of Organic Chemistry 75 (2010) 5453–5460; doi:10.1021/jo1009596

data_4025600
_publ_section_title
;
 Alkali Metal Ions As Probes of Structure and Recognition Properties of
 Macrocyclic Pyridyl Urea Hosts
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5453
_journal_page_last               5460
_journal_paper_doi               10.1021/jo1009596
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         '2(C28 H40 N8 O2), 3(C6 H6), 2(H2 O)'
_chemical_formula_sum            'C74 H102 N16 O6'
_chemical_formula_weight         1311.72
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                90.9320(10)
_cell_angle_beta                 93.8400(10)
_cell_angle_gamma                103.5500(10)
_cell_formula_units_Z            2
_cell_length_a                   14.2251(7)
_cell_length_b                   15.9467(7)
_cell_length_c                   16.5472(8)
_cell_measurement_reflns_used    6419
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.276
_cell_measurement_theta_min      2.196
_cell_volume                     3639.0(3)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics    various
_computing_publication_material  'SHELXTL Version 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44552
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         11589
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0632
_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^)+(0.0759P)^2^+2.7137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1790
_reflns_number_gt                8791
_reflns_number_total             11589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo1009596_si_003.cif
_cod_data_source_block           cw06250s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4025600