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_7134856
_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, C H2 Cl2'
_chemical_formula_sum            'C55 H52 Cl2 N2'
_chemical_formula_weight         811.88
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2025-07-22 deposited with the CCDC.	2025-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                103.388(2)
_cell_angle_beta                 92.384(2)
_cell_angle_gamma                106.529(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7520(3)
_cell_length_b                   15.4169(5)
_cell_length_c                   15.7126(5)
_cell_measurement_reflns_used    14693
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      70.13
_cell_measurement_theta_min      23.74
_cell_volume                     2188.48(12)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19911
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.635
_diffrn_reflns_theta_min         3.669
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2909
_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            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         7845
_refine_ls_number_restraints     374
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0619
_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^)+(0.1092P)^2^+0.9683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.1843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5918
_reflns_number_total             7845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03678j2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7134851--7134861.cif.'
_cod_database_code               7134856
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.641
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2-C55
 1.78 with sigma of 0.02
 Cl3-C55
 1.77 with sigma of 0.02
 Cl2-C55 = Cl3-C55
 1.771 with sigma of 0.01
 Cl2-Cl3
 2.916 with sigma of 0.03
 Cl2-Cl3
 2.92 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C55 \\sim Cl2 \\sim Cl3: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim
C53 \\sim C54 \\sim C45A \\sim C46A \\sim C47A \\sim C48A \\sim C49A \\sim C50A
\\sim C51A \\sim C52A \\sim C53A \\sim C54A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C55, Cl2, Cl3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C45A, C46A, C47A, C48A, C49A, C50A, C51A, C52A, C53A, C54A} sigma for 1-2:
0.02, 1-3: 0.02
as in
{C45, C46, C47, C48, C49, C50, C51, C52, C53, C54}
6. Others
 Sof(H55C)=Sof(H55D)=Sof(Cl2A)=Sof(Cl3A)=1-FVAR(1)
 Sof(H55A)=Sof(H55B)=Sof(Cl2)=Sof(Cl3)=FVAR(1)
 Sof(C45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=
 Sof(H49A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=Sof(H51A)=Sof(C52A)=Sof(C53A)=
 Sof(H53A)=Sof(C54A)=Sof(H54A)=1-FVAR(2)
 Sof(C45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=
 Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(C53)=Sof(H53)=Sof(C54)=
 Sof(H54)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C35(H35A,H35B), C37(H37A,H37B), C55(H55A,H55B),
 C55(H55C,H55D)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C14(H14), C15(H15), C17(H17), C18(H18),
 C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30),
  C31(H31), C33(H33), C34(H34), C40(H40), C41(H41), C43(H43), C44(H44),
 C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C53(H53), C54(H54),
 C46A(H46A), C48A(H48A), C49A(H49A), C50A(H50A), C51A(H51A), C53A(H53A),
 C54A(H54A)
7.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C)
;
_shelx_res_checksum              20090
_shelx_hkl_checksum              70880
_olex2_submission_special_instructions 'No special instructions were received'