Positional isomerism-directed formation of hydrogen-bonded organic frameworks with distinct single-crystal transformation pathways.
Yang, Wenyan; Li, Lele; Xue, Xinlei; Deng, Shengyong; Wei, Peifa; Chemical communications (Cambridge, England) 61 (2025) 13113–13116; doi:10.1039/d5cc03678j

data_7134854
_publ_section_title
;
 Positional isomerism-directed formation of hydrogen-bonded organic
 frameworks with distinct single-crystal transformation pathways.
;
_journal_issue                   70
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13113
_journal_page_last               13116
_journal_paper_doi               10.1039/d5cc03678j
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         '0.5(C4 H8 O2), 0.5(C54 H50 N2)'
_chemical_formula_sum            'C29 H29 N O'
_chemical_formula_weight         407.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-07-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-07-25 deposited with the CCDC.	2025-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                105.062(3)
_cell_angle_beta                 90.118(3)
_cell_angle_gamma                107.315(3)
_cell_formula_units_Z            4
_cell_length_a                   9.6914(4)
_cell_length_b                   15.3962(6)
_cell_length_c                   16.3741(6)
_cell_measurement_reflns_used    14151
_cell_measurement_temperature    120
_cell_measurement_theta_max      69.81
_cell_measurement_theta_min      3.13
_cell_volume                     2243.97(16)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
 1440 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0828
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18889
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        62.492
_diffrn_reflns_theta_max         62.492
_diffrn_reflns_theta_min         3.125
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         6973
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0608
_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^)+(0.1088P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4254
_reflns_number_total             6973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03678j2.cif
_cod_data_source_block           0318-2
_cod_depositor_comments
'Adding full bibliography for 7134851--7134861.cif.'
_cod_database_code               7134854
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C3A \\sim C4A \\sim O1: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
2. Same fragment restrains
{C3, C4} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C3A, C4A}
3. Others
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C30(H30A,H30B), C31(H31A,H31B), C56(H56A,H56B), C57(H57A,H57B),
 C3A(H3AA,H3AB)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C12(H12), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28), C34(H34),
  C35(H35), C37(H37), C38(H38), C40(H40), C42(H42), C43(H43), C44(H44),
 C45(H45), C47(H47), C48(H48), C50(H50), C51(H51), C53(H53), C54(H54)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C),
 C55(H55A,H55B,H55C), C58(H58A,H58B,H58C), C4A(H4AA,H4AB,H4AC)
;
_shelx_res_checksum              63723
_shelx_hkl_checksum              96915
_olex2_submission_special_instructions 'No special instructions were received'