Topological control in paddlewheel metal-organic cages <i>via</i> ligand length variation.
Tsoukatos, Steven; Maibam, Ashakiran; Babarao, Ravichandar; Bloch, Witold M.; Chemical communications (Cambridge, England) 60 (2024) 13183–13186; doi:10.1039/d4cc03769c

data_7133774
_publ_section_title
;
 Topological control in paddlewheel metal-organic cages <i>via</i> ligand
 length variation.
;
_journal_issue                   90
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13183
_journal_page_last               13186
_journal_paper_doi               10.1039/d4cc03769c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'C264 H212 Cu8 N4 O56, (C6 H13 N1 O1)16.5, (H2 O1)4'
_chemical_formula_sum            'C363 H434.5 Cu8 N20.5 O76.5'
_chemical_formula_weight         6817.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-09-23 deposited with the CCDC.	2024-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.1090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.7693(3)
_cell_length_b                   53.8990(8)
_cell_length_c                   31.4036(3)
_cell_measurement_reflns_used    69058
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.0090
_cell_measurement_theta_min      2.7660
_cell_volume                     48321.2(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_molecular_graphics    'shelXle (Huebschle, 2014)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_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  0.0695
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            257707
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        56.893
_diffrn_reflns_theta_max         56.893
_diffrn_reflns_theta_min         2.764
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.54a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.937
_exptl_crystal_description       plate
_exptl_crystal_F_000             14400
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3030
_refine_ls_number_reflns         63356
_refine_ls_number_restraints     3560
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.1471
_refine_ls_R_factor_gt           0.1050
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3386
_refine_ls_wR_factor_ref         0.3703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                34150
_reflns_number_total             63356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03769c2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7133774--7133778.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C363 H434.50 Cu8 N20.50 O76.50'
_cod_database_code               7133774
_shelx_shelxl_version_number     2019/3
_oxdiff_exptl_absorpt_empirical_full_min 0.729
_oxdiff_exptl_absorpt_empirical_full_max 1.638
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              94731
_shelx_hkl_checksum              866
_shelx_fab_checksum              28128