Double Helix of Opposite Charges to Form Channels with Unique CO2 Selectivity and Dynamics
Sozzani, Piero; Xing, Guolong; Bassanetti, Irene; Bracco, Silvia; Negroni, Mattia; Bezuidenhout, Charl; Ben, Teng; Comotti, Angiolina; Chemical Science  (2019) –; doi:10.1039/C8SC04376K

data_1550096
_publ_section_title
;
 Double Helix of Opposite Charges to Form Channels with Unique CO2
 Selectivity and Dynamics
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04376K
_journal_year                    2019
_chemical_formula_moiety         'C25 H16 O12 S4, 8(H2 O), 2(C8 H12 N4)'
_chemical_formula_sum            'C41 H56 N8 O20 S4'
_chemical_formula_weight         1109.17
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-08-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-01 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.7276(5)
_cell_length_b                   25.7276(5)
_cell_length_c                   7.7202(3)
_cell_measurement_reflns_used    12827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.2830
_cell_measurement_theta_min      2.1970
_cell_volume                     5110.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f      0.00 360.00   0.30    0.50   0.00   0.00   0.00    --  1200
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0074110000
_diffrn_orient_matrix_UB_12      0.0262150000
_diffrn_orient_matrix_UB_13      -0.0001164000
_diffrn_orient_matrix_UB_21      -0.0201599000
_diffrn_orient_matrix_UB_22      0.0055886000
_diffrn_orient_matrix_UB_23      0.0576307000
_diffrn_orient_matrix_UB_31      0.0166955000
_diffrn_orient_matrix_UB_32      -0.0046794000
_diffrn_orient_matrix_UB_33      0.0700128000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            24962
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.939
_diffrn_reflns_theta_min         2.205
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       needle
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.733
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0860P)^2^+6.1650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2436
_reflns_number_total             2609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04376k2.cif
_cod_data_source_block           pos-1100k
_cod_depositor_comments
;

2022-09-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C164 H224 N32 O80 S16'
_cod_original_formula_weight         4436.70
_cod_original_formula_moiety         '4(C25 H16 O12 S4), 32(H2 O), 8(C8 H12 N4)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        5110.1(3)
_cod_database_code               1550096
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.832
_reflns_odcompleteness_completeness 90.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.59
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups, All N(H,H) groups
2.a Free rotating group:
 O005(O006)
2.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00A(H00A), C00B(H00B), C00D(H00D), C00F(H00H), C00I(H00I)
2.c X=CH2 refined with riding coordinates:
 N007(H00C,H00E), N008(H00F,H00G)
;
_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 1.728
_oxdiff_exptl_absorpt_empirical_full_min 0.700