A Bis-calix[4]pyrrole Enzyme Mimic That Constrains Two Oxoanions in Close Proximity.
He, Qing; Kelliher, Michael; Bähring, Steffen; Lynch, Vincent M.; Sessler, Jonathan L.; Journal of the American Chemical Society 139 (2017) 7140–7143; doi:10.1021/jacs.7b02329

data_4131271
_publ_section_title
;
 A Bis-calix[4]pyrrole Enzyme Mimic That Constrains Two Oxoanions in Close
 Proximity.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7140
_journal_page_last               7143
_journal_paper_doi               10.1021/jacs.7b02329
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C31 H35 N7 O2, 2(C H4 O)'
_chemical_formula_sum            'C40 H0 Cl0.12 N6 O2'
_chemical_formula_weight         600.89
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.187(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.954(5)
_cell_length_b                   6.9664(9)
_cell_length_c                   24.402(3)
_cell_measurement_reflns_used    8806
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0047
_cell_measurement_theta_min      1.3877
_cell_volume                     6569.9(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1312
_diffrn_reflns_av_unetI/netI     0.1094
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34164
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.070
_exptl_absorpt_coefficient_mu    0.089
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       column
_exptl_crystal_F_000             2401
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.091
_refine_diff_density_max         1.747
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1803
_refine_ls_R_factor_gt           0.1138
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1531P)^2^+36.5003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2852
_refine_ls_wR_factor_ref         0.3306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3309
_reflns_number_total             5779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02329_si_003.cif
_cod_data_source_block           b
_cod_database_code               4131271
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C21(H21A,H21B), C27(H27A,H27B), C30(H30A,H30B)
2.b Aromatic/amide H refined with riding coordinates:
 N0AA(H0AA), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), C5(H5A), C8(H8), C10(H10),
  C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19),
 C25(H25), C29(H29), C31(H31), C32(H32), C33(H33)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2A)
;
_shelx_res_checksum              64164
_shelx_hkl_checksum              35141
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'