Thermal fluctuation-induced selective CO2 uptake of seemingly nonporous N,C-protected dipeptide crystals as elucidated by in situ X-ray crystallographic analysis
Yamanaka, Kazuaki; Oketani, Ryusei; Mori, Yuya; Sato, Takashi; Tsuzuki, Seiji; Takahashi, Hiroki; Tsue, Hirohito; CrystEngComm 26 (2024) 2314–2321; doi:10.1039/D3CE01018J

data_7248341
_publ_section_title
;
 Thermal fluctuation-induced selective CO2 uptake of seemingly nonporous
 N,C-protected dipeptide crystals as elucidated by in situ X-ray
 crystallographic analysis
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2314
_journal_page_last               2321
_journal_paper_doi               10.1039/D3CE01018J
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C14 H26 N2 O5 S, 0.254(C O2)'
_chemical_formula_sum            'C14.25 H26 N2 O5.51 S'
_chemical_formula_weight         345.61
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_symmetry_Int_Tables_number      170
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-02-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-22 deposited with the CCDC.	2024-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   11.239(4)
_cell_length_b                   11.239(4)
_cell_length_c                   27.0392(10)
_cell_measurement_reflns_used    5390
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2957.9(15)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      188.15
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.9970
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.9967
_diffrn_reflns_Laue_measured_fraction_max 0.9970
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9839
_diffrn_reflns_point_group_measured_fraction_full 0.9150
_diffrn_reflns_point_group_measured_fraction_max 0.9031
_diffrn_reflns_theta_full        25.2425
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.63
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.189
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       needle
_exptl_crystal_F_000             1118.444
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.3331
_refine_diff_density_min         -0.1966
_refine_diff_density_rms         0.0494
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.05(11)
_refine_ls_d_res_high            0.7702
_refine_ls_d_res_low             5.6195
_refine_ls_goodness_of_fit_ref   0.8487
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    66
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4090
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.8476
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.0722
_refine_ls_shift/su_mean         0.0019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1201P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1886
_reflns_Friedel_coverage         0.805
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              34
_reflns_limit_l_min              -26
_reflns_number_gt                2329
_reflns_number_total             4090
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3ce01018j4.cif
_cod_data_source_block           cmpd_1_CO2_188K
_cod_depositor_comments
'Adding full bibliography for 7248340--7248345.cif.'
_cod_original_sg_symbol_Hall     ' P 65'
_cod_database_code               7248341
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O6-C15
 1.2 with sigma of 0.02
 O7-C15
 1.2 with sigma of 0.02
 O7-O6
 2.4 with sigma of 0.02
3. Restrained angles
 O6-C15-O7
 fixed at 180 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C2B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
5. Others
 Sof(C1B)=Sof(C9B)=Sof(O1B)=Sof(O2B)=Sof(C3B)=Sof(C2B)=Sof(O6)=Sof(O7)=Sof(C15)=
 Sof(H9Ba)=Sof(H9Bb)=Sof(H9Bc)=Sof(H3Ba)=Sof(H3Bb)=Sof(H3Bc)=Sof(H16)=
 Sof(H1nb)=1-FVAR(1)
 Sof(C2A)=Sof(C3A)=Sof(C1A)=Sof(O2A)=Sof(O1A)=Sof(C9A)=Sof(H2A)=Sof(H3Aa)=Sof(H3Ab)=
 Sof(H3Ac)=Sof(H9Aa)=Sof(H9Ab)=Sof(H9Ac)=Sof(H1na)=FVAR(1)
 Sof(C10B)=Sof(O4B)=Sof(O5B)=Sof(C13B)=Sof(C14B)=Sof(C11B)=Sof(C12B)=Sof(H13Ba)=
 Sof(H13Bb)=Sof(H13Bc)=Sof(H12Ba)=Sof(H12Bb)=Sof(H12Bc)=Sof(H2nb)=Sof(H14Ba)=Sof(H14Bb)=
 Sof(H14Bc)=1-FVAR(2)
 Sof(C10A)=Sof(C11A)=Sof(C12A)=Sof(C13A)=Sof(C14A)=Sof(O4A)=Sof(O5A)=Sof(H12Aa)=
 Sof(H12Ab)=Sof(H12Ac)=Sof(H13Aa)=Sof(H13Ab)=Sof(H13Ac)=Sof(H14Aa)=Sof(H14Ab)=
 Sof(H14Ac)=Sof(H2na)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C2A(H2A), C5(H5), C2B(H16)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C7(H7a,H7b)
6.c Aromatic/amide H refined with riding coordinates:
 N1(H1na), N1(H1nb), N2(H2na), N2(H2nb)
6.d Idealised Me refined as rotating group:
 C3A(H3Aa,H3Ab,H3Ac), C8(H8a,H8b,H8c), C9B(H9Ba,H9Bb,H9Bc), C12A(H12Aa,H12Ab,H12Ac),
 C13A(H13Aa,H13Ab,H13Ac), C14A(H14Aa,H14Ab,H14Ac), C3B(H3Ba,H3Bb,H3Bc), C9A(H9Aa,H9Ab,
 H9Ac), C13B(H13Ba,H13Bb,H13Bc), C12B(H12Ba,H12Bb,H12Bc), C14B(H14Ba,H14Bb,H14Bc)
;
_olex2_submission_special_instructions 'No special instructions were received'