Porous supramolecular gels produced by reversible self-gelation of ruthenium-based metal-organic polyhedra.
Troyano, Javier; Tayier, Fuerkaiti; Phattharaphuti, Phitchayapha; Aoyama, Takuma; Urayama, Kenji; Furukawa, Shuhei; Chemical science 14 (2023) 9543–9552; doi:10.1039/d3sc02888g

data_1569672
_publ_section_title
;
 Porous supramolecular gels produced by reversible self-gelation of
 ruthenium-based metal-organic polyhedra.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              9543
_journal_page_last               9552
_journal_paper_doi               10.1039/d3sc02888g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C224 H72 N8 O144 Ru24'
_chemical_formula_sum            'C224 H96 N8 O144 Ru24'
_chemical_formula_weight         7628.76
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-16
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-05-16 deposited with the CCDC.	2023-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   30.9370(2)
_cell_length_b                   30.9370(2)
_cell_length_c                   31.2314(3)
_cell_measurement_reflns_used    137758
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.4600
_cell_measurement_theta_min      2.0270
_cell_volume                     29891.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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   -105.00  71.70   0.38   10.40    --  -16.40  45.00 150.00  465
  2  \w   -105.00  71.70   0.38   10.40    --  -16.40  45.00 179.39  465
  3  \w   -105.00 -79.92   0.38   10.40    --  -16.40  45.00  -9.35   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0135798005
_diffrn_orient_matrix_UB_12      -0.0077183995
_diffrn_orient_matrix_UB_13      0.0166461005
_diffrn_orient_matrix_UB_21      0.0145924989
_diffrn_orient_matrix_UB_22      -0.0082993011
_diffrn_orient_matrix_UB_23      -0.0154493011
_diffrn_orient_matrix_UB_31      0.0113895484
_diffrn_orient_matrix_UB_32      0.0198939484
_diffrn_orient_matrix_UB_33      -0.0000285516
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            123553
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.853
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    0.848
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             7408
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.167
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         15592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0830P)^2^+119.6297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12154
_reflns_number_total             15592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02888g3.cif
_cod_data_source_block           ohrumop
_cod_depositor_comments          'Adding full bibliography for 1569672.cif.'
_cod_original_cell_volume        29891.5(5)
_cod_database_code               1569672
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru O C '
_chemical_oxdiff_usercomment     -173C
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.884
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C20(H20), C2(H2), C12(H12), C6(H6), C22(H22), C18(H18), C14(H14),
 C10(H10)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38815
_shelx_fab_checksum              27689
_olex2_submission_original_sample_id OHRuMOP
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.412
_oxdiff_exptl_absorpt_empirical_full_min 0.574