The introduction of a base component to porous organic salts and their CO2 storage capability
Ami, Takahiro; Oka, Kouki; Tsuchiya, Keiho; Kosaka, Wataru; Miyasaka, Hitoshi; Tohnai, Norimitsu; CrystEngComm 25 (2023) 2321–2325; doi:10.1039/D3CE00086A

data_7246492
_publ_section_title
;
 The introduction of a base component to porous organic salts and their
 CO2 storage capability
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2321
_journal_page_last               2325
_journal_paper_doi               10.1039/D3CE00086A
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety
'C53 H36 O12 S4, C13 H12 N7, 3(C17 H16 N3), 2[C4H9N1O1], 1[C7H5N1], 2[C4H9N1O1], 1[C7H5N1], 2[C4H9N1O1], 1[C7H5N1], 0.167[]'
_chemical_formula_sum            'C162 H165 N25 O18 S4'
_chemical_formula_weight         2878.42
_chemical_name_systematic        DPPMA/MTBPS
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-02-28
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.02.27 svn.rf166f9f3 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2023-03-02 deposited with the CCDC.	2023-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   21.9765(4)
_cell_length_b                   21.9765(4)
_cell_length_c                   114.166(2)
_cell_measurement_reflns_used    17860
_cell_measurement_temperature    213.0
_cell_measurement_theta_max      52.9560
_cell_measurement_theta_min      3.8770
_cell_volume                     47751.2(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      213.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -88.00   2.06   0.38   50.00    --    0.00 -37.00 -60.00  237
  2  \w    -14.00  12.22   0.38   50.00    --    0.00  37.00  30.00   69
  3  \w     77.00 180.74   0.38  150.00    --   95.80  45.00 -60.00  273
  4  \w     76.00 142.12   0.38  150.00    --   95.80  30.00  90.00  174
  5  \w    114.00 156.56   0.38  150.00    --   95.80  30.00-180.00  112
  6  \w     75.00 184.06   0.38  150.00    --   95.80  45.00 -90.00  287
  7  \w     78.00 103.08   0.38  150.00    --   95.80  79.00 166.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       134
_diffrn_reflns_limit_l_min       -127
_diffrn_reflns_number            49413
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        64.989
_diffrn_reflns_theta_max         64.989
_diffrn_reflns_theta_min         2.791
_exptl_absorpt_coefficient_mu    1.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       prism
_exptl_crystal_F_000             18240
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.251
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         9040
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.263
_refine_ls_R_factor_all          0.1275
_refine_ls_R_factor_gt           0.1015
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.005
_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          0.3298
_refine_ls_wR_factor_ref         0.3624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5166
_reflns_number_total             9040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00086a2.cif
_cod_data_source_block           exp_1377_sq_sq_sq
_cod_depositor_comments          'Adding full bibliography for 7246492.cif.'
_cod_original_cell_volume        47751(2)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7246492
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.469
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
2. Restrained distances
 C27-C1
 1.54 with sigma of 0.02
 C1-C0
 1.54 with sigma of 0.02
 C28-C0
 1.54 with sigma of 0.02
 C30-C32B
 1.54 with sigma of 0.02
 C32B-C31B
 1.54 with sigma of 0.02
 C31B-C29
 1.54 with sigma of 0.02
 C28-C1
 2.408 with sigma of 0.04
 C30-C31B
 2.408 with sigma of 0.04
 C32B-C29
 2.408 with sigma of 0.04
 C0-C27
 2.408 with sigma of 0.04
3. Restrained planarity
 C27, C1, C0, C28
 with sigma of 0.1
 C29, C32B, C30, C31B
 with sigma of 0.1
4. Rigid bond restraints
 N3, C010
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C00V, C00T
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C30, C32B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O003, S001
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N7, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C30 \\sim C32B \\sim C31B \\sim C29 \\sim C28 \\sim C1 \\sim C27 \\sim C0:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C33 \\sim N6 \\sim C35 \\sim N7: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
C38 \\sim C017 \\sim C37 \\sim C39 \\sim C36 \\sim C016: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
6. Others
 Sof(C1)=Sof(H1)=Sof(C0)=Sof(H0)=Sof(C31B)=Sof(H31B)=Sof(C32B)=Sof(H32B)=1-
 FVAR(1)
 Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=FVAR(1)
 Fixed Sof: H2A(0.33333) H2B(0.33333) H2C(0.33333)
7.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C22(H22), C00L(H00L), C00M(H00M), C010(H010), C015(H015),
 C00W(H00W), C00O(H00O), C00Q(H00Q), C00R(H00R), C00S(H00S), C39(H39), C36(H36),
  C017(H017), C38(H38), C016(H016), C011(H011), C00V(H00V), C019(H019),
 C01A(H01A), C018(H018), C1(H1), C0(H0), C31B(H31B), C32B(H32B), C35(H35),
 C012(H012), C33(H33), C31A(H31A), C32A(H32A), C2(H2), C3(H3)
7.b Fitted hexagon refined as free rotating group:
 C00N(C010,N3,C015,N4,C00W), C39(C36,C37,C017,C38,C016), C011(C00V,C00T,C019,
 C01A,C018), N7(C35,C00Z,C012,N6,C33)
7.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N5(H5A,H5B,H5C)
;
_shelx_res_checksum              96253
_shelx_hkl_checksum              5929
_shelx_fab_checksum              90257
_platon_squeeze_special_details
'6(C4 H9 N1 O1) and 3(C7 H5 N1) have been masked.'
_platon_squeeze_void_probe_radius 1.20
_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
;