Magnesium cations as templates for the self-assembly of supramolecular luminescent {Mg@[B<sub>18</sub>φ<sub>34-35</sub>]}-clusters.
Volkov, Sergey; Yukhno, Valentina; Banaru, Alexander; Deyneko, Dina; Aksenov, Sergey; Charkin, Dmitri; Povolotskiy, Alexey; Savchenko, Yevgeny; Antonov, Andrey; Krzhizhanovskaya, Maria; Ugolkov, Valery; Firsova, Vera; Vaitieva, Yulia; Boldyrev, Kirill; Bubnova, Rimma; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8112–8117; doi:10.1039/d3dt04048h

data_7715890
_publ_section_title
;
 Magnesium cations as templates for the self-assembly of supramolecular
 luminescent {Mg@[B<sub>18</sub>&#x3c6;<sub>34-35</sub>]}-clusters.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8112
_journal_page_last               8117
_journal_paper_doi               10.1039/d3dt04048h
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'B17 Mg O28, 1[C24N9H82O2]'
_chemical_formula_sum            'C24 H82 B17 Mg N9 O30'
_chemical_formula_weight         1185.279
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_symmetry_Int_Tables_number      122
_atom_sites_solution_primary     direct
_audit_creation_date             2024-03-03
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-15 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4695(3)
_cell_length_b                   22.4695(3)
_cell_length_c                   10.1408(5)
_cell_measurement_reflns_used    6092
_cell_measurement_temperature    298.5(3)
_cell_measurement_theta_max      75.7820
_cell_measurement_theta_min      3.9070
_cell_volume                     5119.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.5(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9961
_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    -76.00 -50.00   0.50   27.19    --  -48.51 136.00  80.00   52
  2  \w   -118.00 -93.00   0.50   27.19    --  -48.51-134.00-165.00   50
  3  \w    -92.00 -55.00   0.50   27.19    --  -48.51 134.00 -98.00   74
  4  \w   -119.00 -67.00   0.50   27.19    --  -48.51-136.00  15.00  104
  5  \w     45.00  70.00   0.50   27.19    --   48.51-136.00  15.00   50
  6  \w     50.00  92.00   0.50   27.19    --   48.51-134.00-165.00   84
  7  \w   -139.00-114.00   0.50   27.19    --  -90.00-134.00-165.00   50
  8  \w   -137.00-112.00   0.50   27.19    --  -90.00-136.00  15.00   50
  9  \w    121.00 147.00   0.50   27.19    --  111.50 136.00  80.00   52
 10  \w     64.00 115.00   0.50   27.19    --  111.50-134.00-165.00  102
 11  \w     80.00 105.00   0.50   27.19    --  111.50-136.00  15.00   50
 12  \w    116.00 142.00   0.50   27.19    --  111.50 134.00 -98.00   52
 13  \w   -117.00 -87.00   0.50   27.19    --  -48.51-125.00-180.00   60
 14  \w    -25.00  22.00   0.50   27.19    --  -48.51  19.00 -60.00   94
 15  \w   -118.00 -73.00   0.50   27.19    --  -48.51-125.00-120.00   90
 16  \w     -5.00  25.00   0.50   27.19    --   48.51 -19.00   0.00   60
 17  \w    112.00 177.00   0.50   27.19    --  111.50  15.00 -30.00  130
 18  \w     52.00  78.00   0.50   27.19    --  111.50 -77.00 -30.00   52
 19  \w     40.00  69.00   0.50   27.19    --  111.50 -61.00-180.00   58
 20  \w     40.00  65.00   0.50   27.19    --  111.50 -61.00   0.00   50
 21  \w     41.00  69.00   0.50   27.19    --  111.50 -61.00-120.00   56
 22  \w    102.00 175.00   0.50   27.19    --  111.50  15.00-150.00  146
 23  \w     58.00  84.00   0.50   27.19    --  111.50 -77.00-150.00   52
 24  \w     49.00  92.00   0.50   27.19    --  111.50 -77.00 -60.00   86
 25  \w     40.00  68.00   0.50   27.19    --  111.50 -61.00 -90.00   56
 26  \w    123.00 171.00   0.50   27.19    --  111.50  45.00-120.00   96
 27  \w    123.00 148.00   0.50   27.19    --  111.50  45.00  30.00   50
 28  \w     63.00  89.00   0.50   27.19    --  111.50 -95.00  90.00   52
 29  \w     74.00 100.00   0.50   27.19    --  111.50 -95.00-180.00   52
 30  \w     40.00  70.00   0.50   27.19    --  111.50 -61.00  90.00   60
 31  \w     40.00 104.00   0.50   27.19    --  111.50 -77.00-120.00  128
 32  \w     42.00  68.00   0.50   27.19    --  111.50 -77.00 120.00   52
 33  \w     73.00 104.00   0.50   27.19    --  111.50 -77.00 120.00   62
 34  \w    101.00 143.00   0.50   27.19    --  111.50  45.00  60.00   84
 35  \w     43.00  82.00   0.50   27.19    --  111.50 -77.00   0.00   78
 36  \w    113.00 138.00   0.50   27.19    --  111.50  45.00  90.00   50
 37  \w    143.00 178.00   0.50   27.19    --  111.50  45.00  90.00   70
 38  \w     59.00  84.00   0.50   27.19    --  111.50-125.00 -60.00   50
 39  \w     46.00  71.00   0.50   27.19    --  111.50 -61.00 150.00   50
 40  \w    150.00 176.00   0.50   27.19    --  111.50  45.00   0.00   52
 41  \w     48.00 105.00   0.50   27.19    --  111.50 -77.00  60.00  114
 42  \w     43.00  89.00   0.50   27.19    --  111.50-125.00 -90.00   92
 43  \w    104.00 144.00   0.50   27.19    --  111.50  45.00   0.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0316110000
_diffrn_orient_matrix_UB_12      -0.0465639000
_diffrn_orient_matrix_UB_13      0.0867771000
_diffrn_orient_matrix_UB_21      -0.0299481000
_diffrn_orient_matrix_UB_22      -0.0503509000
_diffrn_orient_matrix_UB_23      -0.0790218000
_diffrn_orient_matrix_UB_31      0.0529430000
_diffrn_orient_matrix_UB_32      -0.0006276000
_diffrn_orient_matrix_UB_33      -0.0964227000
_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  0.0829
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9961
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25273
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9918
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         79.84
_diffrn_reflns_theta_min         3.93
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_T_max  0.60364
_exptl_absorpt_correction_T_min  0.57064
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       sphere
_exptl_crystal_F_000             2514.689
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         0.1443
_refine_diff_density_min         -0.1184
_refine_diff_density_rms         0.0255
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.54(3)
_refine_ls_d_res_high            0.7832
_refine_ls_d_res_low             11.2348
_refine_ls_goodness_of_fit_ref   0.9844
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     105
_refine_ls_number_reflns         2775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9844
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.0592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0862
_reflns_Friedel_coverage         0.986
_reflns_limit_h_max              28
_reflns_limit_h_min              -28
_reflns_limit_k_max              20
_reflns_limit_k_min              -19
_reflns_limit_l_max              12
_reflns_limit_l_min              -12
_reflns_number_gt                2159
_reflns_number_total             2775
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt04048h2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7715886--7715891.cif.'
_cod_original_sg_symbol_Hall     ' I -4 2bw'
_cod_original_formula_sum        'C24 H82 B17 Mg1 N9 O30'
_cod_database_code               7715890
_chemical_oxdiff_formula         C24H82B17MgN9O30
_olex2_refinement_description
;
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 2.954
_oxdiff_exptl_absorpt_empirical_full_min 0.418