Synthesis, crystal structure, and gas sorption studies of two neutral octahedral {MII24}-cages built from sulfonylcalix[4]arene tetranuclear clusters and triazine linkers
Khariushin, Ivan V.; Bulach, Véronique; Ward, Jas S.; Rissanen, Kari; Solovieva, Svetlana E.; Antipin, Igor S.; Ovsyannikov, Alexander S.; Ferlay, Sylvie; CrystEngComm 26 (2024) 6789–6795; doi:10.1039/D4CE00964A

data_7249557
_publ_section_title
;
 Synthesis, crystal structure, and gas sorption studies of two neutral
 octahedral {MII24}-cages built from sulfonylcalix[4]arene tetranuclear
 clusters and triazine linkers
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              6789
_journal_page_last               6795
_journal_paper_doi               10.1039/D4CE00964A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C432 H360 N24 Ni24 O126 S24'
_chemical_formula_sum            'C432 H360 N24 Ni24 O126 S24'
_chemical_formula_weight         10081.90
_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             2022-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-09-18 deposited with the CCDC.	2024-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   32.9311(3)
_cell_length_b                   32.9311(3)
_cell_length_c                   54.0192(6)
_cell_measurement_reflns_used    56005
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.5070
_cell_measurement_theta_min      1.9520
_cell_volume                     58581.5(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1947
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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    -75.00  34.00   0.50    8.00    --  -41.92  77.00 150.00  218
  2  \w   -114.00 -14.00   0.50    8.00    --  -41.92 -57.00  30.00  200
  3  \w    -21.00  75.00   0.50    8.00    --   41.92 -77.00 -90.00  192
  4  \w    104.00 178.00   0.50   50.00    --  106.04 111.00 120.00  148
  5  \w     30.00 109.00   0.50   50.00    --  106.04-111.00 -60.00  158
  6  \w     30.00 134.00   0.50   50.00    --  106.04 -30.00   0.00  208
  7  \w     80.00 178.00   0.50   50.00    --  106.04  45.00-180.00  196
  8  \w     24.00 106.00   0.50   50.00    --  106.04 -94.00-180.00  164
  9  \w    104.00 176.00   0.50   50.00    --  106.04 111.00  90.00  144
 10  \w     41.00 109.00   0.50   50.00    --  106.04-111.00  60.00  136
 11  \w     41.00  98.00   0.50   50.00    --  106.04 -94.00 120.00  114
 12  \w     30.00 134.00   0.50   50.00    --  106.04 -30.00 150.00  208
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0359804000
_diffrn_orient_matrix_UB_12      -0.0101247000
_diffrn_orient_matrix_UB_13      0.0171618000
_diffrn_orient_matrix_UB_21      -0.0299401000
_diffrn_orient_matrix_UB_22      0.0119677000
_diffrn_orient_matrix_UB_23      -0.0206759000
_diffrn_orient_matrix_UB_31      0.0000946000
_diffrn_orient_matrix_UB_32      -0.0440523000
_diffrn_orient_matrix_UB_33      -0.0095560000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            189192
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.524
_diffrn_reflns_theta_min         1.897
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.328
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.572
_exptl_crystal_description       block
_exptl_crystal_F_000             10368
_exptl_crystal_recrystallization_method 'Solvothermal synthesis.'
_exptl_crystal_size_max          0.351
_exptl_crystal_size_mid          0.281
_exptl_crystal_size_min          0.212
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         29635
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0895
_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^)+(0.1415P)^2^+242.7556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2632
_refine_ls_wR_factor_ref         0.2982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22239
_reflns_number_total             29635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00964a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7249556--7249557.cif.'
_cod_original_cell_volume        58581.7(12)
_cod_database_code               7249557
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_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. Restrained distances
 C8-C7
 1.52 with sigma of 0.01
 C9-C7
 1.52 with sigma of 0.01
 C30-C27
 1.52 with sigma of 0.01
 C18-C17
 1.48 with sigma of 0.01
 C20-C17
 1.52 with sigma of 0.01
 C28-C27
 1.52 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C11, C12, C13, C14, C15, C16, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C21, C22, C23, C24, C25, C26, C30, C28, C29, C27
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C15(H15), C23(H23), C25(H25), C38(H38), C39(H39),
 C41(H41), C42(H42), C47(H47), C48(H48), C50(H50), C51(H51), C56(H56), C57(H57),
  C59(H59), C60(H60)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              50018
_shelx_hkl_checksum              773
_shelx_fab_checksum              31624
_ins_header
;
TITL NAFC73-4_numabs2 in I4/m 
REM I4/m (#87 in standard setting)
CELL 1.54184  32.931146  32.931146  54.019244  90.0000  90.0000  90.0000
ZERR    4.00   0.000288   0.000288   0.000627   0.0000   0.0000   0.0000
LATT  2
SYMM -x,-y, z 
SYMM -y, x, z 
SYMM  y,-x, z 
SFAC C H N O S Ni
UNIT 1728.00 1440.00 96.00 480.00 96.00 96.00
REM  CrysAlisPro recorded range (K): Min=120.0; max=120.0; aver:120.0
TEMP -153
SIZE 0.21 0.28 0.35
TREF
HKLF 4
END
;
_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 1.335
_oxdiff_exptl_absorpt_empirical_full_min 0.825