Post-synthetic modification of amine-functionalized permanently porous coordination cages.
Hoq, Jahidul; Dworzak, Michael R.; Dissanayake, Duleeka; Skalla, Rebecca X.; Yamamoto, Nobuyuki; Yap, Glenn P. A.; Bloch, Eric D.; Chemical communications (Cambridge, England) 61 (2025) 1641–1644; doi:10.1039/d4cc04370g

data_7134033
_publ_section_title
;
 Post-synthetic modification of amine-functionalized permanently porous
 coordination cages.
;
_journal_issue                   8
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1641
_journal_page_last               1644
_journal_paper_doi               10.1039/d4cc04370g
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C32 H28 Cl2 Co N4 O8, 2(C2 H3 N)'
_chemical_formula_sum            'C36 H34 Cl2 Co N6 O8'
_chemical_formula_weight         808.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-06-03
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-19 deposited with the CCDC.	2024-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.0298(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3352(6)
_cell_length_b                   11.9100(3)
_cell_length_c                   16.3910(7)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.370
_cell_measurement_theta_min      2.510
_cell_volume                     3684.0(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'Photon III'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35180
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.022
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1007 before and 0.0833 after correction.
The Ratio of minimum to maximum transmission is 0.7792.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'orangish brown'
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_recrystallization_method
'Vapor diffusion: benzene into acetonitrile solution'
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0407P)^2^+4.1089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3330
_reflns_number_total             3624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04370g2.cif
_cod_data_source_block           24125
_cod_depositor_comments
'Adding full bibliography for 7134033--7134034.cif.'
_cod_database_code               7134033
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.914
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C3S(H3SA,H3SB,H3SC)
;
_shelx_res_checksum              44565
_shelx_hkl_checksum              33490
_olex2_date_sample_data_collection 2024-05-17
_olex2_date_sample_submission    2024-05-17
_olex2_exptl_crystal_mounting_method 'MiTeGen loop; paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'