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_4025605
_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
'C113 H182 N32 Cl4 Na6 O34, 2(Cl O4), 6(H2 O), 4(C H4 O)'
_chemical_formula_sum            'C117 H210 Cl6 N32 Na6 O52'
_chemical_formula_weight         3247.81
_chemical_name_systematic
; 
 ? 
;
_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                78.2280(10)
_cell_angle_beta                 69.1940(10)
_cell_angle_gamma                84.7170(10)
_cell_formula_units_Z            1
_cell_length_a                   14.4465(6)
_cell_length_b                   15.4789(6)
_cell_length_c                   19.1776(7)
_cell_measurement_reflns_used    9387
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.039
_cell_measurement_theta_min      2.194
_cell_volume                     3923.5(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            63682
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         13929
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0841P)^2^+3.1607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                11634
_reflns_number_total             13929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo1009596_si_008.cif
_cod_data_source_block           kri138m
_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               4025605