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_7715891
_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
'B8.5 Mg0.5 O15, B8.5 Mg0.5 O15.5, 1[C11H41.5N4.5O]'
_chemical_formula_sum            'C11 H41.5 B17 Mg N4.5 O31.5'
_chemical_formula_weight         941.281
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_Int_Tables_number      4
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-05
_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                 94.5979(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.33587(19)
_cell_length_b                   19.9667(3)
_cell_length_c                   14.4962(2)
_cell_measurement_reflns_used    28247
_cell_measurement_temperature    266(30)
_cell_measurement_theta_max      79.3390
_cell_measurement_theta_min      3.0160
_cell_volume                     4136.04(10)
_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      N~2~
_diffrn_ambient_temperature      266(30)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9987
_diffrn_measured_fraction_theta_max 0.9826
_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    -71.00  24.00   0.50    2.00    --  -46.59  79.00  90.00  190
  2  \w     25.00  59.00   0.50    2.00    --   46.59 -79.00 -33.00   68
  3  \w    -72.00 -46.00   0.50    8.00    --  -91.75  79.00  90.00   52
  4  \w   -144.00 -98.00   0.50    8.00    --  -91.75 -79.00 -33.00   92
  5  \w    101.00 161.00   0.50    8.00    --  113.25  79.00  90.00  120
  6  \w    109.00 135.00   0.50    8.00    --  113.25 -79.00 -33.00   52
  7  \w   -115.00 -73.00   0.50    2.00    --  -46.59-125.00  90.00   84
  8  \w   -117.00 -73.00   0.50    2.00    --  -46.59-125.00 -60.00   88
  9  \w   -118.00 -31.00   0.50    2.00    --  -46.59 -57.00 -30.00  174
 10  \w   -102.00 -73.00   0.50    2.00    --  -46.59-125.00  60.00   58
 11  \w    -51.00 -26.00   0.50    8.00    --  -91.75  45.00 -90.00   50
 12  \w    -69.00 -29.00   0.50    8.00    --  -91.75  61.00 -30.00   80
 13  \w     42.00  70.00   0.50    8.00    --  113.25 -61.00  30.00   56
 14  \w     41.00  66.00   0.50    8.00    --  113.25 -61.00-150.00   50
 15  \w    143.00 178.00   0.50    8.00    --  113.25  15.00  30.00   70
 16  \w    141.00 173.00   0.50    8.00    --  113.25  15.00-180.00   64
 17  \w     46.00  71.00   0.50    8.00    --  113.25 -61.00 -30.00   50
 18  \w     58.00 105.00   0.50    8.00    --  113.25 -77.00 150.00   94
 19  \w    153.00 178.00   0.50    8.00    --  113.25  77.00-180.00   50
 20  \w     41.00  67.00   0.50    8.00    --  113.25 -61.00 -90.00   52
 21  \w     98.00 133.00   0.50    8.00    --  113.25  15.00-180.00   70
 22  \w     43.00  69.00   0.50    8.00    --  113.25 -61.00-120.00   52
 23  \w     53.00  91.00   0.50    8.00    --  113.25 -77.00   0.00   76
 24  \w     65.00  91.00   0.50    8.00    --  113.25-125.00  60.00   52
 25  \w     48.00 101.00   0.50    8.00    --  113.25 -77.00 -60.00  106
 26  \w     62.00  91.00   0.50    8.00    --  113.25 -95.00-150.00   58
 27  \w     50.00 107.00   0.50    8.00    --  113.25-125.00 120.00  114
 28  \w     96.00 128.00   0.50    8.00    --  113.25  15.00 -60.00   64
 29  \w    140.00 178.00   0.50    8.00    --  113.25  15.00 -60.00   76
 30  \w     41.00  71.00   0.50    8.00    --  113.25 -61.00  60.00   60
 31  \w     96.00 155.00   0.50    8.00    --  113.25  15.00  60.00  118
 32  \w    119.00 145.00   0.50    8.00    --  113.25  77.00-180.00   52
 33  \w     41.00  66.00   0.50    8.00    --  113.25 -61.00  90.00   50
 34  \w    109.00 157.00   0.50    8.00    --  113.25  45.00 150.00   96
 35  \w    122.00 159.00   0.50    8.00    --  113.25  45.00  60.00   74
 36  \w     43.00  74.00   0.50    8.00    --  113.25 -95.00   0.00   62
 37  \w     43.00 104.00   0.50    8.00    --  113.25 -77.00-120.00  122
 38  \w     78.00 105.00   0.50    8.00    --  113.25 -95.00   0.00   54
 39  \w     45.00  98.00   0.50    8.00    --  113.25 -77.00 120.00  106
 40  \w     42.00  71.00   0.50    8.00    --  113.25 -77.00  30.00   58
 41  \w     41.00  68.00   0.50    8.00    --  113.25 -61.00   0.00   54
 42  \w     91.00 116.00   0.50    8.00    --  113.25  77.00-150.00   50
 43  \w    143.00 170.00   0.50    8.00    --  113.25  77.00-150.00   54
 44  \w     42.00  67.00   0.50    8.00    --  113.25 -61.00-180.00   50
 45  \w     58.00  83.00   0.50    8.00    --  113.25-125.00 -60.00   50
 46  \w     98.00 133.00   0.50    8.00    --  113.25  15.00  30.00   70
;
_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      0.0134339000
_diffrn_orient_matrix_UB_12      -0.0578288000
_diffrn_orient_matrix_UB_13      0.0701604000
_diffrn_orient_matrix_UB_21      0.0741476000
_diffrn_orient_matrix_UB_22      -0.0314032000
_diffrn_orient_matrix_UB_23      -0.0580681000
_diffrn_orient_matrix_UB_31      0.0770734000
_diffrn_orient_matrix_UB_32      0.0402581000
_diffrn_orient_matrix_UB_33      0.0554932000
_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  0.0567
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.9987
_diffrn_reflns_Laue_measured_fraction_max 0.9826
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43527
_diffrn_reflns_point_group_measured_fraction_full 0.9158
_diffrn_reflns_point_group_measured_fraction_max 0.8737
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         79.90
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.324
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.483
_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    1.512
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2396.293
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.3478
_refine_diff_density_min         -0.4077
_refine_diff_density_rms         0.0830
_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   0.53(2)
_refine_ls_d_res_high            0.7831
_refine_ls_d_res_low             14.4496
_refine_ls_goodness_of_fit_ref   1.0168
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     874
_refine_ls_number_reflns         15771
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0168
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1229P)^2^+0.6903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.758
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              25
_reflns_limit_k_min              -25
_reflns_limit_l_max              18
_reflns_limit_l_min              -18
_reflns_number_gt                14747
_reflns_number_total             15771
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt04048h2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7715886--7715891.cif.'
_cod_original_cell_volume        4136.05(10)
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_original_formula_sum        'C11 H41.5 B17 Mg1 N4.5 O31.5'
_cod_database_code               7715891
_chemical_oxdiff_formula         C11H41.5B17MgN4.5O31.5
_olex2_refinement_description
;
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 581 electrons were 
found in a volume of 2008\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C11H41N4O1.5] per formula unit 
which account for 572 electrons 
per unit cell.
;
_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 2.874
_oxdiff_exptl_absorpt_empirical_full_min 0.350