Very Strong Binding for a Neutral Calix[4]pyrrole Receptor Displaying Positive Allosteric Binding.
Duedal, Troels; Nielsen, Kent A.; Olsen, Gunnar; Rasmussen, Charlotte B. G.; Kongsted, Jacob; Levillain, Eric; Breton, Tony; Miyazaki, Eigo; Takimiya, Kazuo; Bähring, Steffen; Jeppesen, Jan O.; The Journal of organic chemistry 82 (2017) 2123–2128; doi:10.1021/acs.joc.6b02944

data_4032173
_publ_section_title
;
 Very Strong Binding for a Neutral Calix[4]pyrrole Receptor Displaying
 Positive Allosteric Binding.
;
_journal_issue                   4
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2123
_journal_page_last               2128
_journal_paper_doi               10.1021/acs.joc.6b02944
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C96 H92 N4 O12 S24'
_chemical_formula_sum            'C96 H92 N4 O12 S24'
_chemical_formula_weight         2263.17
_chemical_name_common            49A
_chemical_name_systematic
; 
 22-1 complex
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 108.637(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   44.129(12)
_cell_length_b                   14.749(4)
_cell_length_c                   16.465(4)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.77
_cell_measurement_theta_min      2.61
_cell_volume                     10154(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27407
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.977
_diffrn_reflns_theta_min         1.464
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       block
_exptl_crystal_F_000             4704
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         12116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0114P)^2^+77.9779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.1900
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8679
_reflns_number_total             12116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b02944_si_001.cif
_cod_data_source_block           49A
_cod_depositor_comments          'Adding full bibliography for 4032173.cif.'
_cod_original_cell_volume        10155(5)
_cod_database_code               4032173
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.895
_shelx_res_checksum              56823
_shelx_hkl_checksum              39805