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_7715888
_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_formula_moiety         'B17 Mg O30, [C9H41N4.5O1.5]'
_chemical_formula_sum            'C9 H41 B17 Mg N4.5 O31.5'
_chemical_formula_weight         924.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2024-02-27
_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                 90.418(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.6909(10)
_cell_length_b                   15.9750(8)
_cell_length_c                   22.8241(10)
_cell_measurement_reflns_used    10909
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      18.8170
_cell_measurement_theta_min      2.1860
_cell_volume                     7179.4(6)
_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  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.2739
_diffrn_measured_fraction_theta_max 0.945
_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      7.00  34.00   0.50   59.00    --   11.38-110.00 107.00   54
  2  \w    -50.00 -25.00   0.50   59.00    --  -11.70 110.00-157.00   50
  3  \w    -60.00  25.00   0.50   59.00    --   11.38 -57.00  60.00  170
  4  \w    -52.00  15.00   0.50   59.00    --   11.38 -57.00 -60.00  134
  5  \w    -59.00  24.00   0.50   59.00    --   11.38 -57.00 120.00  166
  6  \w    -58.00  24.00   0.50   59.00    --   11.38 -57.00  30.00  164
  7  \w      6.00  71.00   0.50   59.00    --   11.38  38.00-120.00  130
  8  \w    -24.00  12.00   0.50   59.00    --  -11.70 -99.00  90.00   72
  9  \w     -5.00  20.00   0.50   59.00    --  -11.70 -99.00-180.00   50
 10  \w    -24.00  16.00   0.50   59.00    --  -11.70 -99.00 -60.00   80
 11  \w    -24.00  11.00   0.50   59.00    --  -11.70 -99.00 -90.00   70
 12  \w    -24.00  18.00   0.50   59.00    --  -11.70 -99.00 120.00   84
;
_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      -0.0038538000
_diffrn_orient_matrix_UB_12      0.0198960000
_diffrn_orient_matrix_UB_13      0.0275645000
_diffrn_orient_matrix_UB_21      -0.0234519000
_diffrn_orient_matrix_UB_22      0.0285251000
_diffrn_orient_matrix_UB_23      -0.0126771000
_diffrn_orient_matrix_UB_31      -0.0270579000
_diffrn_orient_matrix_UB_32      -0.0276056000
_diffrn_orient_matrix_UB_33      0.0067621000
_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  0.1211
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            56873
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        18.860
_diffrn_reflns_theta_max         18.860
_diffrn_reflns_theta_min         1.784
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_description       prizm
_exptl_crystal_F_000             3804
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     861
_refine_ls_number_reflns         5346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0995
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2541
_refine_ls_wR_factor_ref         0.2635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4651
_reflns_number_total             5346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04048h2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7715886--7715891.cif.'
_cod_original_formula_sum        'C9 H41 B17 Mg N4.50 O31.50'
_cod_database_code               7715888
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C9H41B17MgN4.5O31.5
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.983
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(B7) = Uanis(B8)
;
_smtbx_masks_void_probe_radius   0.755
_smtbx_masks_void_truncation_radius 1.45
_shelx_res_checksum              64385
_shelx_fab_checksum              34941
_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 8.783
_oxdiff_exptl_absorpt_empirical_full_min 0.495