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_7134858
_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         'C54 H50 N2'
_chemical_formula_sum            'C54 H50 N2'
_chemical_formula_weight         726.96
_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             2025-07-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-07-22 deposited with the CCDC.	2025-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                74.666(3)
_cell_angle_beta                 84.430(3)
_cell_angle_gamma                85.549(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2880(4)
_cell_length_b                   11.9759(4)
_cell_length_c                   15.6694(5)
_cell_measurement_reflns_used    15030
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.6680
_cell_measurement_theta_min      2.9200
_cell_volume                     2030.22(12)
_computing_cell_refinement       'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.957
_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    -18.00   8.00   0.50    0.05    --  -48.32  19.00-150.00   52
  2  \w    -23.00  20.00   0.50    0.05    --  -48.32  19.00-120.00   86
  3  \w    -65.00  16.00   0.50    0.05    --  -48.32  76.00-104.00  162
  4  \w     29.00 116.00   0.50    0.05    --   48.32  76.00-104.00  174
  5  \w    110.00 175.00   0.50    0.16    --  103.74  38.00-180.00  130
  6  \w     91.00 175.00   0.50    0.16    --  103.74  57.00-150.00  168
  7  \w     92.00 174.00   0.50    0.16    --  103.74  76.00-104.00  164
  8  \w     82.00 164.00   0.50    0.16    --  103.74 125.00-150.00  164
  9  \w    133.00 170.00   0.50    0.16    --  103.74 125.00  90.00   74
 10  \w     83.00 118.00   0.50    0.16    --  103.74 125.00  90.00   70
 11  \w     35.00 105.00   0.50    0.16    --  103.74 -99.00 120.00  140
 12  \w     36.00 106.00   0.50    0.16    --  103.74-125.00  30.00  140
 13  \w     66.00  92.00   0.50    0.05    --   48.32-125.00  30.00   52
 14  \w     45.00 111.00   0.50    0.16    --  103.74-125.00 -90.00  132
 15  \w     35.00  99.00   0.50    0.16    --  103.74 -99.00  30.00  128
 16  \w     71.00 106.00   0.50    0.16    --  103.74 -99.00  60.00   70
 17  \w     32.00  67.00   0.50    0.16    --  103.74 -57.00 120.00   70
 18  \w     47.00  79.00   0.50    0.16    --  103.74 -76.00 128.00   64
 19  \w     18.00  54.00   0.50    0.05    --   48.32 -76.00 128.00   72
 20  \w   -110.00 -36.00   0.50    0.05    --  -48.32 -76.00 128.00  148
 21  \w   -174.00-143.00   0.50    0.16    -- -103.74 -76.00 128.00   62
 22  \w   -174.00-122.00   0.50    0.16    -- -103.74 -38.00  30.00  104
 23  \w   -168.00-142.00   0.50    0.16    -- -103.74 -19.00-180.00   52
 24  \w   -161.00-135.00   0.50    0.16    -- -103.74 -57.00-180.00   52
 25  \w    -81.00 -56.00   0.50    0.16    -- -103.74  77.00 -90.00   50
 26  \w    -91.00 -48.00   0.50    0.16    -- -103.74  76.00-104.00   86
 27  \w    -62.00 -34.00   0.50    0.16    -- -103.74  57.00 -60.00   56
 28  \w    -60.00 -33.00   0.50    0.16    -- -103.74  57.00   0.00   54
 29  \w    -61.00 -33.00   0.50    0.16    -- -103.74  57.00  60.00   56
 30  \w    -61.00 -36.00   0.50    0.16    -- -103.74  57.00  90.00   50
 31  \w   -106.00 -38.00   0.50    0.16    -- -103.74 125.00 150.00  136
 32  \w    -91.00 -15.00   0.50    0.05    --  -48.32 125.00  30.00  152
 33  \w   -128.00-102.00   0.50    0.16    -- -103.74 150.00  -9.45   52
 34  \w    -86.00 -42.00   0.50    0.16    -- -103.74 150.00  -9.45   88
 35  \w   -106.00 -74.00   0.50    0.16    -- -103.74 125.00 -90.00   64
 36  \w   -123.00 -34.00   0.50    0.16    -- -103.74 140.00-120.05  178
 37  \w    -63.00 -37.00   0.50    0.16    -- -103.74 125.00 -90.00   52
 38  \w   -111.00 -78.00   0.50    0.16    -- -103.74 125.00-150.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0610969000
_diffrn_orient_matrix_UB_12      -0.0812694000
_diffrn_orient_matrix_UB_13      0.0829470000
_diffrn_orient_matrix_UB_21      0.1187545000
_diffrn_orient_matrix_UB_22      -0.0713005000
_diffrn_orient_matrix_UB_23      0.0178843000
_diffrn_orient_matrix_UB_31      0.0319836000
_diffrn_orient_matrix_UB_32      0.0784585000
_diffrn_orient_matrix_UB_33      0.0570891000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26564
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.983
_diffrn_reflns_theta_min         2.934
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.143a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         8234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.9805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7079
_reflns_number_total             8234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03678j2.cif
_cod_data_source_block           3_auto
_cod_depositor_comments
'Adding full bibliography for 7134851--7134861.cif.'
_cod_database_code               7134858
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.861
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C35(H35A,H35B), C37(H37A,H37B)
1.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29),
  C30(H30), C32(H32), C33(H33), C40(H40), C41(H41), C43(H43), C44(H44),
 C46(H46), C47(H47), C48(H48), C51(H51), C52(H52), C53(H53), C54(H54)
1.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              29871
_shelx_hkl_checksum              40450
_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 1.857
_oxdiff_exptl_absorpt_empirical_full_min 0.476