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_7715889
_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[C19H68N9]'
_chemical_formula_sum            'C19 H68 B17 Mg N9 O28'
_chemical_formula_weight         1079.113
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_symmetry_Int_Tables_number      113
_atom_sites_solution_primary     dual
_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            2
_cell_length_a                   16.1163(6)
_cell_length_b                   16.1163(6)
_cell_length_c                   10.0685(6)
_cell_measurement_reflns_used    3637
_cell_measurement_temperature    296.3(9)
_cell_measurement_theta_max      24.1650
_cell_measurement_theta_min      1.7860
_cell_volume                     2615.1(2)
_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    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.3(9)
_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 1.0000
_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     21.00  46.00   0.50   80.00    --   11.38-142.00 166.00   50
  2  \w    -60.00 -35.00   0.50   80.00    --  -11.70 128.00  51.00   50
  3  \w    -17.00  36.00   0.50   80.00    --   11.38 -99.00-150.00  106
  4  \w    -60.00  33.00   0.50   80.00    --   11.38 -77.00-120.00  186
  5  \w      2.00  82.00   0.50   80.00    --   11.38  38.00   0.00  160
  6  \w    -20.00  14.00   0.50   80.00    --  -11.70 -99.00-150.00   68
  7  \w    -50.00  -9.00   0.50   80.00    --  -11.70 -38.00  30.00   82
  8  \w    -20.00  21.00   0.50   80.00    --  -11.70 -99.00-180.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0426594000
_diffrn_orient_matrix_UB_12      -0.0102831000
_diffrn_orient_matrix_UB_13      0.0055586000
_diffrn_orient_matrix_UB_21      0.0106054000
_diffrn_orient_matrix_UB_22      0.0425140000
_diffrn_orient_matrix_UB_23      -0.0063557000
_diffrn_orient_matrix_UB_31      -0.0024293000
_diffrn_orient_matrix_UB_32      0.0047110000
_diffrn_orient_matrix_UB_33      0.0699475000
_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  0.1326
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 1.0000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25772
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.9996
_diffrn_reflns_theta_full        24.4210
_diffrn_reflns_theta_max         24.42
_diffrn_reflns_theta_min         1.79
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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_density_diffrn    1.370
_exptl_crystal_description       prizm
_exptl_crystal_F_000             1133.045
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.2196
_refine_diff_density_min         -0.2171
_refine_diff_density_rms         0.0326
_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   0.2(4)
_refine_ls_d_res_high            0.8595
_refine_ls_d_res_low             11.3960
_refine_ls_goodness_of_fit_ref   0.9012
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9012
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0466P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.999
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              11
_reflns_limit_l_min              -11
_reflns_number_gt                1783
_reflns_number_total             2278
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt04048h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7715886--7715891.cif.'
_cod_original_sg_symbol_Hall     ' P -4 2ab'
_cod_original_formula_sum        'C19 H68 B17 Mg1 N9 O28'
_cod_database_code               7715889
_chemical_oxdiff_formula         C19H68B17MgN9O28
_olex2_refinement_description
;
;
_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.45
_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 2.280
_oxdiff_exptl_absorpt_empirical_full_min 0.583