Metallo-hydrogen bonded organic frameworks with nitrogen tridentate ligands: exploring inclusion and dye adsorption properties
Li, Haitao; Qin, Guangshan; Guo, Zhenwei; Guo, Fang; CrystEngComm 27 (2025) 1773–1780; doi:10.1039/D4CE01215A

data_7249919
_publ_section_title
;
 Metallo-hydrogen bonded organic frameworks with nitrogen tridentate
 ligands: exploring inclusion and dye adsorption properties
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              1773
_journal_page_last               1780
_journal_paper_doi               10.1039/D4CE01215A
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety
'Cl4 Zn, Cl, C24 H42 N3 O3, 0.725(H2 O1), 0.334(O)'
_chemical_formula_sum            'C24 H44 Cl5 N3 O4 Zn'
_chemical_formula_weight         681.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-01-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-01-16 deposited with the CCDC.	2025-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.7130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9164(4)
_cell_length_b                   19.7454(8)
_cell_length_c                   15.8657(6)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      23.96
_cell_measurement_theta_min      2.20
_cell_volume                     3275.4(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44126
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.856
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6315
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0896 before and 0.0591 after correction.
The Ratio of minimum to maximum transmission is 0.8471.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5731
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0853P)^2^+3.1419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4046
_reflns_number_total             5731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01215a2.cif
_cod_data_source_block           240604_l1_0m_a
_cod_depositor_comments
'Adding full bibliography for 7249917--7249919.cif.'
_cod_database_code               7249919
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.870
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-H4A
 0.89 with sigma of 0.01
 H4B-O4
 0.89 with sigma of 0.01
 H4A-H4B
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 1*[Sof(O4)+Sof(H4A)+Sof(H4B)]+1*[Sof(O5)]+1*[Sof(O6)]=1 with esd of 0.01
 Sof(O4)=Sof(H4A)=Sof(H4B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 N2(H2), N1(H1), N3(H3)
5.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C18(H18A,H18B), C17(H17A,H17B), C16(H16A,H16B), C15(H15A,
 H15B), C10(H10A,H10B), C14(H14A,H14B), C13(H13A,H13B), C12(H12A,H12B),
 C11(H11A,H11B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
  C24(H24A,H24B)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              16810
_olex2_submission_special_instructions 'No special instructions were received'