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_7249556
_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 Co24 N24 O126 S24'
_chemical_formula_sum            'C432 H360 Co24 N24 O126 S24'
_chemical_formula_weight         10087.18
_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             2022-10-06
_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                   33.0404(10)
_cell_length_b                   33.0404(10)
_cell_length_c                   54.083(2)
_cell_measurement_reflns_used    10630
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      55.3560
_cell_measurement_theta_min      2.6730
_cell_volume                     59041(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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 10.3895
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.709
_diffrn_measured_fraction_theta_max 0.985
_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    -87.00 -37.00   0.50   22.00    --    0.00 178.00  60.00  100
  2  \w    -87.00 -37.00   0.50   22.00    --    0.00 178.00-120.00  100
  3  \w     97.00 143.00   0.50   87.00    --   69.97 125.00 120.00   92
  4  \w     -6.00 103.00   0.50   87.00    --   69.97 -77.00  60.00  218
  5  \w     51.00 134.00   0.50   87.00    --   69.97  37.00-150.00  166
  6  \w     37.00 135.00   0.50   87.00    --   69.97  19.00   0.00  196
;
_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      0.0094903000
_diffrn_orient_matrix_UB_12      0.0446376000
_diffrn_orient_matrix_UB_13      0.0058619000
_diffrn_orient_matrix_UB_21      0.0303204000
_diffrn_orient_matrix_UB_22      0.0012167000
_diffrn_orient_matrix_UB_23      -0.0216929000
_diffrn_orient_matrix_UB_31      -0.0342202000
_diffrn_orient_matrix_UB_32      0.0134136000
_diffrn_orient_matrix_UB_33      -0.0174398000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0918
_diffrn_reflns_av_unetI/netI     0.0866
_diffrn_reflns_Laue_measured_fraction_full 0.709
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            72847
_diffrn_reflns_point_group_measured_fraction_full 0.709
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         55.943
_diffrn_reflns_theta_min         1.891
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.233
_exptl_absorpt_correction_T_max  0.580
_exptl_absorpt_correction_T_min  0.080
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    0.567
_exptl_crystal_description       block
_exptl_crystal_F_000             10320
_exptl_crystal_recrystallization_method 'In situ crystallisation.'
_exptl_crystal_size_max          0.502
_exptl_crystal_size_mid          0.409
_exptl_crystal_size_min          0.312
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         19170
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1510
_refine_ls_R_factor_gt           0.0858
_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^)+(0.1774P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2686
_refine_ls_wR_factor_ref         0.3117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9172
_reflns_number_total             19170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00964a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7249556--7249557.cif.'
_cod_original_cell_volume        59041(4)
_cod_database_code               7249556
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     54.18
_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
 H8B-H9B
 -2.2 with sigma of 0.02
 H9C-H5
 -2.1 with sigma of 0.02
 H23-H30A
 -2.1 with sigma of 0.01
 C28-C27 = C30-C27
 1.5 with sigma of 0.02
 H28C-H23
 -2.4 with sigma of 0.01
 C10-C7 = C9-C7
 1.5 with sigma of 0.02
 C9-C7
 1.5 with sigma of 0.02
 C52-C49
 1.5 with sigma of 0.001
 C17-C14
 1.5 with sigma of 0.02
 C18-C17 = C17-C19 = C17-C20
 1.5 with sigma of 0.02
 C18-C17
 1.5 with sigma of 0.001
 H19C-H18A
 -2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C24 \\sim C27 \\sim C28 \\sim C29 \\sim C30: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C4, C7, C8, C9, C10
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C14, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.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)
5.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              97521
_shelx_hkl_checksum              57423
_shelx_fab_checksum              26049
_ins_header
;
TITL NAFC73-1_numabs2 in I4/m 
REM I4/m (#87 in standard setting)
CELL 1.54184  33.040376  33.040376  54.083126  90.0000  90.0000  90.0000
ZERR    4.00   0.000997   0.000997   0.002411   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 Co
UNIT 1728.00 1440.00 96.00 480.00 96.00 96.00
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 1.386
_oxdiff_exptl_absorpt_empirical_full_min 0.735