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_7134852
_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         'C H Cl3, C54 H50 N2'
_chemical_formula_sum            'C55 H51 Cl3 N2'
_chemical_formula_weight         846.32
_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
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Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
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2025-07-25 deposited with the CCDC.	2025-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                107.880(2)
_cell_angle_beta                 102.522(2)
_cell_angle_gamma                99.296(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0040(2)
_cell_length_b                   15.3041(2)
_cell_length_c                   16.1113(3)
_cell_measurement_reflns_used    15773
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.7530
_cell_measurement_theta_min      2.9900
_cell_volume                     2221.55(8)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31186
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.064
_diffrn_reflns_theta_min         3.005
_exptl_absorpt_coefficient_mu    2.165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         9070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0702P)^2^+1.1560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8046
_reflns_number_total             9070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03678j2.cif
_cod_data_source_block           1121-6ywy_auto
_cod_depositor_comments
'Adding full bibliography for 7134851--7134861.cif.'
_cod_original_cell_volume        2221.55(7)
_cod_database_code               7134852
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.563
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C1(H1)
1.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C53(H53A,H53B), C54(H54A,H54B)
1.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C24(H24), C25(H25), C31(H31),
  C32(H32), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C41(H41),
 C42(H42), C43(H43), C44(H44), C47(H47), C48(H48), C50(H50), C51(H51)
1.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C52(H52A,H52B,H52C), C55(H55A,H55B,
 H55C)
;
_shelx_res_checksum              84698
_shelx_hkl_checksum              75421
_olex2_submission_special_instructions 'No special instructions were received'