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_4131272
_publ_section_title
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 A Bis-calix[4]pyrrole Enzyme Mimic That Constrains Two Oxoanions in Close
 Proximity.
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_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         'C74 H86 N14 O4, 6.06(C2 H3 N), 0.49(O)'
_chemical_formula_sum            'C86.12 H104.18 N20.06 O4.49'
_chemical_formula_weight         1492.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-03-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
????
;
_cell_angle_alpha                90
_cell_angle_beta                 92.361(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2141(5)
_cell_length_b                   13.2874(8)
_cell_length_c                   29.0597(13)
_cell_measurement_reflns_used    3800
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.7980
_cell_measurement_theta_min      1.6690
_cell_volume                     3940.6(4)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            29099
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.119
_diffrn_reflns_theta_max         25.119
_diffrn_reflns_theta_min         2.078
_exptl_absorpt_coefficient_mu    0.081
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             1657
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         6875
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1623
_refine_ls_R_factor_gt           0.0989
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1332P)^2^+3.7437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2376
_refine_ls_wR_factor_ref         0.2795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4013
_reflns_number_total             6875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02329_si_002.cif
_cod_data_source_block           host
_cod_database_code               4131272
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
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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
2. Restrained distances
 N1A-C1A = N1B-C1B = N1C-C1C
 1.14 with sigma of 0.01
 C1A-C2A = C1B-C2B = C1C-C2C
 1.46 with sigma of 0.01
 N1A-C2A = N1B-C2B = N1C-C2C
 2.6 with sigma of 0.01
 N1D-C1D = N1E-C1E
 1.14 with sigma of 0.01
 C1D-C2D = C1E-C2E
 1.46 with sigma of 0.01
 N1D-C2D = N1E-C2E
 2.6 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N1A \\sim C1A \\sim C2A \\sim N1B \\sim C1B \\sim C2B \\sim N1C \\sim C1C \\sim
C2C \\sim N1D \\sim C1D \\sim C2D \\sim N1E \\sim C1E \\sim C2E: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: N1A(0.29) C1A(0.29) C2A(0.29) H2AA(0.29) H2AB(0.29) H2AC(0.29)
 N1B(0.46) C1B(0.46) C2B(0.46) H2BA(0.46) H2BB(0.46) H2BC(0.46) N1C(0.28)
 C1C(0.28) C2C(0.28) H2CA(0.28) H2CB(0.28) H2CC(0.28) N1D(0.38) C1D(0.38)
 C2D(0.38) H2DA(0.38) H2DB(0.38) H2DC(0.38) N1E(0.62) C1E(0.62) C2E(0.62)
 H2EA(0.62) H2EB(0.62) H2EC(0.62)
5.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C18(H18),
 C32(H32), C33(H33), C34(H34), N1(H1), N2(H2A), N3(H3A), N4(H4), N5(H5), N7(H7A)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C39(H39A,H39B,H39C), C2A(H2AA,
 H2AB,H2AC), C2B(H2BA,H2BB,H2BC), C2C(H2CA,H2CB,H2CC), C2D(H2DA,H2DB,H2DC),
 C2E(H2EA,H2EB,H2EC)
;
_shelx_res_checksum              12173
_shelx_hkl_checksum              86672
_olex2_submission_special_instructions 'No special instructions were received'