Electrostatic and Allosteric Cooperativity in Ion-Pair Binding: A Quantitative and Coupled Experiment-Theory Study with Aryl-Triazole-Ether Macrocycles.
Qiao, Bo; Sengupta, Arkajyoti; Liu, Yun; McDonald, Kevin P.; Pink, Maren; Anderson, Joseph R.; Raghavachari, Krishnan; Flood, Amar H.; Journal of the American Chemical Society 137 (2015) 9746–9757; doi:10.1021/jacs.5b05839

data_4124192
_publ_section_title
;
 Electrostatic and Allosteric Cooperativity in Ion-Pair Binding: A
 Quantitative and Coupled Experiment-Theory Study with Aryl-Triazole-Ether
 Macrocycles.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9746
_journal_page_last               9757
_journal_paper_doi               10.1021/jacs.5b05839
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C40 H46 Cl N8 Na O11, 1.5 (C H Cl3)'
_chemical_formula_sum            'C41.5 H47.5 Cl5.5 N8 Na O11'
_chemical_formula_weight         1052.34
_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                71.201(4)
_cell_angle_beta                 74.532(4)
_cell_angle_gamma                70.716(4)
_cell_formula_units_Z            4
_cell_length_a                   15.2227(10)
_cell_length_b                   17.5544(12)
_cell_length_c                   20.4454(15)
_cell_measurement_reflns_used    4735
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.19
_cell_volume                     4802.7(6)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2013)'
_computing_publication_material  'SHELXTL (Bruker, 2013)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2010)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
'0.50 degree frames measured for 30 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi 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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            62658
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.9722
_exptl_absorpt_correction_T_min  0.9090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Twinabs, G. Sheldrick; 2013'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1233
_refine_ls_number_reflns         15220
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0587P)^2^+7.7070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1481
_reflns_number_gt                12477
_reflns_number_total             15220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b05839_si_003.cif
_cod_data_source_block           13096
_cod_depositor_comments
'Adding full bibliography for 4124192--4124194.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C41.50 H47.50 Cl5.50 N8 Na O11'
_cod_database_code               4124192