Macrocycles with Switchable exo/endo Metal Binding Sites
Lei-lei Tian; Chun Wang; Sandipan Dawn; Mark D. Smith; Jeanette A. Krause; Linda S. Shimizu; Journal of the American Chemical Society 131 (2009) 17620–17629; doi:10.1021/ja906474z

data_4105426
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of South Carolina
Columbia, South Carolina 29208
USA
;
_publ_contact_author_email       shimizul@mail.chem.sc.edu
_publ_contact_author_fax         '1 803 777 9521'
_publ_contact_author_name        'Professor Linda S. Shimizu'
_publ_contact_author_phone       '1 803 777 2066'
_publ_section_title
;
 Macrocycles with Switchable exo/endo Metal Binding Sites
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17620
_journal_page_last               17629
_journal_paper_doi               10.1021/ja906474z
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C38 H46 N10 O2, 3.7(C H2 Cl2), 0.3(C H4 O)'
_chemical_formula_sum            'C42 H54.6 Cl7.4 N10 O2.3'
_chemical_formula_weight         998.69
_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                 101.5610(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8857(5)
_cell_length_b                   15.0339(7)
_cell_length_c                   13.5999(6)
_cell_measurement_reflns_used    8150
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.363
_cell_measurement_theta_min      2.482
_cell_volume                     2380.84(18)
_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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35275
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2.05 (Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       plate
_exptl_crystal_F_000             1042
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4202
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0587P)^2^+1.7647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1218
_reflns_number_gt                3700
_reflns_number_total             4202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906474z_si_001_3.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C42 H54.60 Cl7.40 N10 O2.30'
_cod_database_code               4105426