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_7715887
_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
'B8.5 Mg0.5 O15.5, B8.5 Mg0.5 O15, [C11.75H49.5N5O1.5]'
_chemical_formula_sum            'B17 Mg O30.5'
_chemical_formula_weight         696.0567
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2024-02-26
_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                 91.091(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.5105(10)
_cell_length_b                   19.9572(8)
_cell_length_c                   21.3269(11)
_cell_measurement_reflns_used    10048
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      25.2720
_cell_measurement_theta_min      2.1470
_cell_volume                     8302.7(7)
_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(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -29.00  10.00   0.50   50.00    --   11.38 -96.00 -18.00   78
  2  \w     -7.00  20.00   0.50   50.00    --  -11.70  96.00  90.00   54
  3  \w    -16.00  44.00   0.50   50.00    --   11.38 -99.00-120.00  120
  4  \w    -80.00  -8.00   0.50   50.00    --  -11.70 -38.00 -60.00  144
  5  \w    -24.00  16.00   0.50   50.00    --  -11.70 -99.00   0.00   80
  6  \w    -20.00  14.00   0.50   50.00    --  -11.70 -99.00  30.00   68
  7  \w    -13.00  16.00   0.50   50.00    --  -11.70 -99.00-150.00   58
  8  \w    -20.00  16.00   0.50   50.00    --  -11.70 -99.00-180.00   72
;
_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      0.0237908000
_diffrn_orient_matrix_UB_12      -0.0268552000
_diffrn_orient_matrix_UB_13      -0.0000074000
_diffrn_orient_matrix_UB_21      -0.0237401000
_diffrn_orient_matrix_UB_22      -0.0197735000
_diffrn_orient_matrix_UB_23      -0.0175152000
_diffrn_orient_matrix_UB_31      0.0138715000
_diffrn_orient_matrix_UB_32      0.0122671000
_diffrn_orient_matrix_UB_33      -0.0282893000
_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  0.1342
_diffrn_reflns_av_unetI/netI     0.1477
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            72918
_diffrn_reflns_point_group_measured_fraction_full 0.837
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.734
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50206
_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    1.114
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   1
_exptl_transmission_factor_min   0.476
_refine_diff_density_max         0.018
_refine_diff_density_min         -0.023
_refine_diff_density_rms         0.002
_refine_ls_abs_structure_details
;
 Flack x determined using 3236 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.6(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         25415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1687
_refine_ls_R_factor_gt           0.0988
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1709P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2447
_refine_ls_wR_factor_ref         0.2969
_reflns_Friedel_coverage         0.694
_reflns_Friedel_fraction_full    0.688
_reflns_Friedel_fraction_max     0.685
_reflns_number_gt                12696
_reflns_number_total             25415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04048h2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7715886--7715891.cif.'
_cod_original_cell_volume        8302.6(7)
_cod_original_formula_sum        'B17 Mg O30.50'
_cod_database_code               7715887
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C11.75H49.5B17MgN5O32
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uiso(O71) = Uiso(O33) = Uiso(B12) = Uiso(O25)
Uanis(B8) = Uanis(O26) = Uanis(O70) = Uanis(O49)
Uanis(O1) = Uanis(O29) = Uanis(O8) = Uanis(O63) = Uanis(B7) = Uanis(O39) =
Uanis(B11) = Uanis(O76) = Uanis(O35)
Uanis(O3) = Uanis(O34) = Uanis(O67) = Uanis(O38) = Uanis(B46) = Uanis(O7) =
Uanis(B17) = Uanis(O54) = Uanis(O90)
Uiso(O24) = Uiso(O71) = Uiso(O6) = Uiso(O33) = Uiso(O25) = Uiso(B12)
Uanis(B43) = Uanis(O18) = Uanis(O41) = Uanis(O98) = Uanis(O17) = Uanis(B25) =
Uanis(O48)
Uanis(B52) = Uanis(B1) = Uanis(B6) = Uanis(O50)
Uanis(B10) = Uanis(O14) = Uanis(B30) = Uanis(O96) = Uanis(B3)
Uanis(O123) = Uanis(B13) = Uanis(B44) = Uanis(O72)
Uanis(O59) = Uanis(O28)
Uiso(O116) = Uiso(B57) = Uiso(O78) = Uiso(O115)
Uanis(O5) = Uanis(B18) = Uanis(O73) = Uanis(O32)
Uanis(B36) = Uanis(B24) = Uanis(O40)
Uanis(O122) = Uanis(B61) = Uanis(B64)
Uanis(O81) = Uanis(B2) = Uanis(O46) = Uanis(O9)
Uanis(B15) = Uanis(B66) = Uanis(O87) = Uanis(B35)
Uanis(B41) = Uanis(O108) = Uanis(B40) = Uanis(B56) = Uanis(B38) = Uanis(O117)
Uanis(B65) = Uanis(B51) = Uanis(O111) = Uanis(B37) = Uanis(O47)
Uanis(O36) = Uanis(B29) = Uanis(B42) = Uanis(O89)
Uiso(B22) = Uiso(O104)
Uanis(B58) = Uanis(O42) = Uanis(B48) = Uanis(O92)
Uanis(O37) = Uanis(B27) = Uanis(O61)
Uanis(B47) = Uanis(B34) = Uanis(O82)
Uanis(O68) = Uanis(B34) = Uanis(B21)
Uanis(B68) = Uanis(O66) = Uanis(B45) = Uanis(B54)
Uanis(O20) = Uanis(B55) = Uanis(O53)
Uanis(B59) = Uanis(B61) = Uanis(O122) = Uanis(O57) = Uanis(O119)
Uanis(B60) = Uanis(B39) = Uanis(O102)
Uanis(O101) = Uanis(O32) = Uanis(B39) = Uanis(O45)
Uanis(B14) = Uanis(O65)
Uanis(O110) = Uanis(O93)
Uanis(O10) = Uanis(B36) = Uanis(O86)
Uanis(B49) = Uanis(O113)
Uanis(B28) = Uanis(O11)
Uanis(B43) = Uanis(O2)
Uanis(O22) = Uanis(O55)
Uanis(O20) = Uanis(O21) = Uanis(B35)
Uanis(O74) = Uanis(B24) = Uanis(B16)
Uanis(O81) = Uanis(O9) = Uanis(O46) = Uanis(B67)
Uanis(O91) = Uanis(B59)
Uanis(O85) = Uanis(O107)
Uanis(O93) = Uanis(O62) = Uanis(O75) = Uanis(O110)
Uanis(O80) = Uanis(B65) = Uanis(O85)
Uanis(O44) = Uanis(B59) = Uanis(O91)
Uanis(B10) = Uanis(O99) = Uanis(O14) = Uanis(O27)
Uanis(O59) = Uanis(O100) = Uanis(B53)
Uanis(O37) = Uanis(B31) = Uanis(O31) = Uanis(O58)
Uanis(O64) = Uanis(B65) = Uanis(O80) = Uanis(O85) = Uanis(B51) = Uanis(O111) =
Uanis(O107)
Uanis(O112) = Uanis(B49) = Uanis(O113) = Uanis(O28)
Uanis(B63) = Uanis(O30) = Uanis(O52)
Uanis(O97) = Uanis(B2) = Uanis(O42)
Uanis(O65) = Uanis(B14) = Uanis(B60) = Uanis(O45) = Uanis(O73)
Uanis(B36) = Uanis(B24) = Uanis(O91) = Uanis(O57)
Uanis(B14) = Uanis(O69)
Uanis(B41) = Uanis(O4)
Uanis(O105) = Uanis(B68) = Uanis(B29)
Uanis(O4) = Uanis(B41)
Uanis(O50) = Uanis(O23) = Uanis(B6)
Uanis(O114) = Uanis(O103) = Uanis(O121) = Uanis(B38)
Uanis(O93) = Uanis(O53) = Uanis(B14) = Uanis(O69)
Uanis(O19) = Uanis(B1) = Uanis(O63)
Uanis(O110) = Uanis(B40)
Uanis(O118) = Uanis(B61)
Uanis(Mg3) = Uanis(O72)
Uanis(O60) = Uanis(B44)
Uanis(O93) = Uanis(B23) = Uanis(O69) = Uanis(O53)
Uanis(O15) = Uanis(B58) = Uanis(O81) = Uanis(O42)
Uiso(B26) = Uiso(O12)
Uanis(Mg4) = Uanis(O79)
Uanis(B13) = Uanis(O83)
Uanis(B1) = Uanis(O43)
Uanis(B25) = Uanis(O16)
2. Others
 Fixed X: O62(0.90308) O75(1.02762) O77(0.89009) O78(0.81145) O79(0.99239)
 O88(0.867371) O94(0.902829) O102(0.80867) O108(0.87906) O109(0.91509)
 O110(0.83573) O111(0.87123) B37(0.89047) B38(0.897221) B40(0.85065)
 B45(0.855901) B50(0.88713) O115(0.85562) O116(0.939468) B51(0.79897)
 B55(0.98127) O117(0.84482) B56(0.84081) B57(0.87416) O119(0.8845)
 O120(0.838921) B62(0.844609) B64(0.84631) O121(0.89509)
 Fixed Y: O62(0.64692) O75(0.625851) O77(1.34359) O78(1.42773) O79(0.667701)
 O88(1.242789) O94(1.24512) O102(0.922509) O108(0.68222) O109(0.935999)
 O110(0.73226) O111(0.71035) B37(0.702009) B38(0.78912) B40(0.67218)
 B45(0.88109) B50(1.27632) O115(1.35566) O116(1.42542) B51(0.67493)
 B55(0.64644) O117(0.83863) B56(0.761861) B57(1.39105) O119(1.2205)
 O120(1.259549) B62(1.28104) B64(1.20513) O121(0.84915)
 Fixed Z: O62(0.244629) O75(0.25287) O77(0.38785) O78(0.332029) O79(0.15553)
 O88(0.32923) O94(0.440639) O102(0.3505) O108(0.126081) O109(0.265301)
 O110(0.2005) O111(0.51018) B37(0.44521) B38(0.35161) B40(0.18769) B45(0.29772)
 B50(0.3848) O115(0.297009) O116(0.33998) B51(0.55237) B55(0.22285)
 O117(0.25167) B56(0.24574) B57(0.35279) O119(0.1525) O120(0.246129)
 B62(0.296889) B64(0.20174) O121(0.37713)
;
_smtbx_masks_void_probe_radius   0.84
_smtbx_masks_void_truncation_radius 1.42
_shelx_res_checksum              74031
_shelx_fab_checksum              348
_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 2.193
_oxdiff_exptl_absorpt_empirical_full_min 0.639