Solvent-mediated subcomponent self-assembly of covalent metallacycles for hierarchical porous materials synthesis.
Li, Zhi-Wei; Huang, Anlian; Wang, Zhenguo; Gao, Rui; Lan, Bang; Chen, Guosheng; Ouyang, Gangfeng; Chemical communications (Cambridge, England) 61 (2025) 4836–4839; doi:10.1039/d5cc00688k

data_7134289
_publ_section_title
;
 Solvent-mediated subcomponent self-assembly of covalent metallacycles for
 hierarchical porous materials synthesis.
;
_journal_issue                   25
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4836
_journal_page_last               4839
_journal_paper_doi               10.1039/d5cc00688k
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C144 H124 Mn4 N28 O16'
_chemical_formula_sum            'C144 H124 Mn4 N28 O16'
_chemical_formula_weight         2722.46
_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             2023-12-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-01-07 deposited with the CCDC.	2025-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                88.264(8)
_cell_angle_beta                 88.730(8)
_cell_angle_gamma                78.204(9)
_cell_formula_units_Z            1
_cell_length_a                   9.1397(10)
_cell_length_b                   19.8181(19)
_cell_length_c                   26.775(3)
_cell_measurement_reflns_used    2206
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      72.1010
_cell_measurement_theta_min      2.8200
_cell_volume                     4744.6(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      150.15
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -74.00  24.00   1.00    9.00    --  -41.39  77.00-120.00   98
  2  \w    -66.00  26.00   1.00    9.00    --  -41.39  38.00 150.00   92
  3  \w   -116.00 -18.00   1.00    9.00    --  -41.39 -38.00 -30.00   98
  4  \w     32.00 110.00   1.00   30.00    --  105.29-125.00 120.00   78
  5  \w    137.00 174.00   1.00   30.00    --  105.29  77.00-180.00   37
  6  \w    104.00 178.00   1.00   30.00    --  105.29  77.00 120.00   74
  7  \w    107.00 142.00   1.00   30.00    --  105.29  77.00 -90.00   35
  8  \w    101.00 166.00   1.00   30.00    --  105.29 125.00 150.00   65
  9  \w     38.00 131.00   1.00   30.00    --  105.29 -61.00-180.00   93
 10  \w     33.00 119.00   1.00   30.00    --  105.29 -45.00  60.00   86
 11  \w     26.00 152.00   1.00   30.00    --  105.29 -15.00 120.00  126
 12  \w     28.00 108.00   1.00   30.00    --  105.29-106.00  -8.57   80
 13  \w     62.00 108.00   1.00   30.00    --  105.29-105.00 168.35   46
 14  \w     47.00  73.00   1.00   20.00    --   41.39-125.00-180.00   26
 15  \w     40.00  84.00   1.00   20.00    --   41.39-125.00  30.00   44
 16  \w     57.00  83.00   1.00   72.50    --  105.29 -61.00  60.00   26
 17  \w    109.00 134.00   1.00   72.50    --  105.29 -61.00  60.00   25
 18  \w     84.00 110.00   1.00   72.50    --  105.29  45.00  30.00   26
 19  \w    103.00 144.00   1.00   72.50    --  105.29  77.00 -90.00   41
 20  \w     77.00 103.00   1.00   72.50    --  105.29 -94.00-120.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1436
_diffrn_reflns_av_unetI/netI     0.2254
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            32312
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        65.088
_diffrn_reflns_theta_max         65.088
_diffrn_reflns_theta_min         2.849
_exptl_absorpt_coefficient_mu    2.553
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.953
_exptl_crystal_description       block
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     833
_refine_ls_number_reflns         16129
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.1742
_refine_ls_R_factor_gt           0.0897
_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^)+(0.0719P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2212
_refine_ls_wR_factor_ref         0.2821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5898
_reflns_number_total             16129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00688k2.cif
_cod_data_source_block           a22121302a0071
_cod_depositor_comments          'Adding full bibliography for 7134289.cif.'
_cod_database_code               7134289
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C52) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60)
\\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(N6) \\sim Ueq,
Uanis(C57) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C61) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
2. Others
 Fixed Sof: H51C(0.5) H51D(0.5) H51A(0.5) H51B(0.5) C52(0.5) H52A(0.5)
 H52B(0.5) H52C(0.5) C73(0.5) H73A(0.5) H73B(0.5) H73C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C51(H51C,H51D), C51(H51A,H51B)
3.b Aromatic/amide H refined with riding coordinates:
 C57(H57), C56(H56), C55(H55), C54(H54), C53(H53), C24(H24), C40(H40),
 C67(H67), C63(H63), C64(H64), C65(H65), C66(H66), C23(H23), C38(H38), C4(H4),
 C12(H12), C14(H14), C71(H71), C48(H48), C45(H45), C29(H29), C30(H30), C31(H31),
  C32(H32), C72(H72), C7(H7), C46(H46), C21(H21), C68(H68), C20(H20), C69(H69),
 C3(H3), C6(H6), C49(H49), C60(H60), C61(H61), C62(H62), C58(H58), C59(H59),
 C70(H70)
3.c Fitted hexagon refined as free rotating group:
 N7(C57,C56,C55,C54,C53), C67(N13,C63,C64,C65,C66), C29(C28,C30,C31,C33,C32),
 C60(C61,C62,N6,C58,C59)
3.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C17(H17A,H17B,H17C), C10(H10A,H10B,H10C), C27(H27A,H27B,
 H27C), C36(H36A,H36B,H36C), C52(H52A,H52B,H52C), C73(H73A,H73B,H73C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              62185
_shelx_hkl_checksum              59274
_shelx_fab_checksum              26485
_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
;