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_4131270
_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
'C72 H80.72 N12 O2, H2.92 O14 P4, 2(C4 H12 N), 2(C3.89 H11.67 N)'
_chemical_formula_sum            'C98 H134 N18 O28 P4'
_chemical_formula_weight         2127.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.226(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.0606(6)
_cell_length_b                   18.5209(7)
_cell_length_c                   20.3176(10)
_cell_measurement_reflns_used    7565
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.2260
_cell_measurement_theta_min      3.2200
_cell_volume                     5633.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -69.00  28.00   1.00   12.50    --  -42.42  57.00 150.00   97
  2  \w   -115.00 -20.00   1.00   12.50    --  -42.42 -38.00 -30.00   95
  3  \w     11.00 116.00   1.00   12.50    --   42.42  77.00 -90.00  105
  4  \w     87.00 178.00   1.00   37.50    --  111.00  45.00 -60.00   91
  5  \w     36.00 135.00   1.00   37.50    --  111.00 -30.00  60.00   99
  6  \w     87.00 178.00   1.00   37.50    --  111.00  45.00 -90.00   91
  7  \w     83.00 178.00   1.00   37.50    --  111.00  61.00-180.00   95
  8  \w     41.00 139.00   1.00   37.50    --  111.00 -61.00  30.00   98
  9  \w     94.00 178.00   1.00   37.50    --  111.00 125.00-150.00   84
 10  \w     94.00 178.00   1.00   37.50    --  111.00 125.00 120.00   84
 11  \w   -121.00  -6.00   1.00   12.50    --  -42.42 -19.00  60.00  115
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1000626000
_diffrn_orient_matrix_UB_12      0.0190594000
_diffrn_orient_matrix_UB_13      0.0046240000
_diffrn_orient_matrix_UB_21      0.0187155000
_diffrn_orient_matrix_UB_22      -0.0716124000
_diffrn_orient_matrix_UB_23      -0.0345775000
_diffrn_orient_matrix_UB_31      -0.0153982000
_diffrn_orient_matrix_UB_32      0.0378199000
_diffrn_orient_matrix_UB_33      -0.0677711000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34773
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.372
_diffrn_reflns_theta_min         3.237
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             2295
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.020
_refine_diff_density_min         -1.626
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.379
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         11546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.379
_refine_ls_R_factor_all          0.1753
_refine_ls_R_factor_gt           0.1393
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3719
_refine_ls_wR_factor_ref         0.4136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6937
_reflns_number_total             11546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02329_si_006.cif
_cod_data_source_block           hq-cisbiscp-pyrophosphate
_cod_database_code               4131270
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C100H150N18O8P4
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Others
 Sof(O7)=1-FVAR(1)
 Sof(O8)=Sof(H8B)=FVAR(1)
 Sof(C38)=1-FVAR(2)
 Sof(H33)=Sof(C34)=FVAR(2)
 Sof(N8)=Sof(H8A)=1-FVAR(3)
 Sof(N7)=FVAR(3)
 Sof(C39)=1-FVAR(4)
 Sof(C35)=FVAR(4)
 Sof(C40)=Sof(H40)=1-FVAR(5)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H37A)=Sof(H37B)=FVAR(5)
 Sof(O10)=1-FVAR(6)
 Sof(O9)=FVAR(6)
 Sof(C52)=1-FVAR(7)
 Sof(C53)=FVAR(7)
 Sof(O15)=1-FVAR(8)
 Sof(O16)=FVAR(8)
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(9)
3.a Riding coordinates:
 N7(H7)
3.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C36(H36A,H36B), C37(H37A,H37B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3A), N3(H3), C4(H4A), N4(H4), N5(H5), C8(H8), N8(H8A), C9(H9),
 C13(H13), C14(H14), C18(H18), C19(H19), C31(H31), C32(H32), C33(H33), C40(H40)
3.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
3.e Idealised tetrahedral OH refined as rotating group:
 O5(H5A), O8(H8B)
;
_shelx_res_checksum              23202
_shelx_hkl_checksum              21995
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.631
_oxdiff_exptl_absorpt_empirical_full_min 0.703