Redox-active inverse crowns - pockets for heavier chalcogenides.
Maurer, Johannes; Klerner, Lukas; Langer, Jens; Harder, Sjoerd; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13950–13957; doi:10.1039/d5dt01896j

data_7719350
_publ_section_title
;
 Redox-active inverse crowns - pockets for heavier chalcogenides.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13950
_journal_page_last               13957
_journal_paper_doi               10.1039/d5dt01896j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C61 H123 Mg N7 Na4 O S Si6'
_chemical_formula_sum            'C61 H123 Mg N7 Na4 O S Si6'
_chemical_formula_weight         1287.53
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-26 deposited with the CCDC.	2025-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                87.022(2)
_cell_angle_beta                 81.394(2)
_cell_angle_gamma                72.168(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5264(4)
_cell_length_b                   15.7132(3)
_cell_length_c                   21.5530(5)
_cell_measurement_reflns_used    25129
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      72.5860
_cell_measurement_theta_min      4.2290
_cell_volume                     3992.91(18)
_computing_cell_refinement       'CrysAlisPro 1.171.43.106a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.105a 64-bit (release 11-01-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.106a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_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    -74.00  35.00   1.00    1.00    --  -41.40  77.00-180.00  109
  2  \w   -116.00 -17.00   1.00    1.00    --  -41.40 -38.00 -90.00   99
  3  \w    -66.00  33.00   1.00    1.00    --  -41.40  38.00  90.00   99
  4  \w      7.00  33.00   1.00    1.00    --   41.40  84.00 -10.26   26
  5  \w      7.00  34.00   1.00    1.00    --   41.40  83.00 -65.00   27
  6  \w      9.00  36.00   1.00    1.00    --   41.40  75.00 103.78   27
  7  \w      7.00  34.00   1.00    1.00    --   41.40  83.00-103.49   27
  8  \w     33.00 113.00   1.00    2.50    --  104.66-125.00  90.00   80
  9  \w     32.00 131.00   1.00    2.50    --  104.66 -45.00 -60.00   99
 10  \w     22.00 106.00   1.00    2.50    --  104.66 -94.00  90.00   84
 11  \w    103.00 178.00   1.00    2.50    --  104.66  77.00  90.00   75
 12  \w    103.00 178.00   1.00    2.50    --  104.66  77.00-120.00   75
 13  \w     33.00 113.00   1.00    2.50    --  104.66-125.00 -90.00   80
 14  \w     97.00 176.00   1.00    2.50    --  104.66 125.00-120.00   79
 15  \w    103.00 178.00   1.00    2.50    --  104.66  77.00-180.00   75
 16  \w    103.00 178.00   1.00    2.50    --  104.66  77.00-150.00   75
 17  \w     29.00 137.00   1.00    2.50    --  104.66 -77.00 150.00  108
 18  \w     22.00 106.00   1.00    2.50    --  104.66 -94.00-180.00   84
 19  \w     32.00 131.00   1.00    2.50    --  104.66 -45.00 150.00   99
 20  \w     52.00 178.00   1.00    2.50    --  104.66  15.00-180.00  126
 21  \w     33.00 113.00   1.00    2.50    --  104.66-125.00  30.00   80
 22  \w     26.00 107.00   1.00    2.50    --  104.66-101.00 -46.93   81
 23  \w   -114.00 -67.00   1.00    1.00    --  -41.40 -57.00  60.00   47
 24  \w      8.00  42.00   1.00    1.00    --   41.40  79.00 165.75   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1221171000
_diffrn_orient_matrix_UB_12      -0.0040044000
_diffrn_orient_matrix_UB_13      0.0035259000
_diffrn_orient_matrix_UB_21      -0.0455012000
_diffrn_orient_matrix_UB_22      0.1020155000
_diffrn_orient_matrix_UB_23      0.0091933000
_diffrn_orient_matrix_UB_31      0.0066757000
_diffrn_orient_matrix_UB_32      0.0135751000
_diffrn_orient_matrix_UB_33      -0.0716197000
_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  0.0310
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            45297
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.721
_diffrn_reflns_theta_min         3.599
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.805
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.106a (Rigaku Oxford Diffraction, 2024)
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_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.299
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         15588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+1.4568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14079
_reflns_number_total             15588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01896j2.cif
_cod_data_source_block           hasj240319a
_cod_depositor_comments
'Adding full bibliography for 7719350--7719354.cif.'
_cod_database_code               7719350
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C61H123MgN7Na4OSSi6
_shelx_estimated_absorpt_t_max   0.749
_shelx_estimated_absorpt_t_min   0.613
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C18(H18), C23(H23), C34(H34), C39(H39)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19a,H19b), C21(H21a,H21b), C24(H24a,H24b), C26(H26a,H26b), C35(H35a,
 H35b), C37(H37a,H37b), C40(H40a,H40b), C42(H42a,H42b)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C14(H14), C15(H15), C16(H16), C30(H30), C31(H31), C32(H32)
2.d Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C9(H9a,H9b,H9c), C10(H10a,
 H10b,H10c), C11(H11a,H11b,H11c), C20(H20a,H20b,H20c), C22(H22a,H22b,H22c),
 C25(H25a,H25b,H25c), C27(H27a,H27b,H27c), C36(H36a,H36b,H36c), C38(H38a,H38b,
 H38c), C41(H41a,H41b,H41c), C43(H43a,H43b,H43c), C44(H44a,H44b,H44c), C45(H45a,
 H45b,H45c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c),
 C49(H49a,H49b,H49c), C50(H50a,H50b,H50c), C51(H51a,H51b,H51c), C52(H52a,H52b,
 H52c), C53(H53a,H53b,H53c), C54(H54a,H54b,H54c), C55(H55a,H55b,H55c), C56(H56a,
 H56b,H56c), C57(H57a,H57b,H57c), C58(H58a,H58b,H58c), C59(H59a,H59b,H59c),
 C60(H60a,H60b,H60c), C61(H61a,H61b,H61c)
;
_shelx_res_checksum              16216
_shelx_hkl_checksum              35559
_olex2_date_sample_data_collection 2024-03-19
_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 1.587
_oxdiff_exptl_absorpt_empirical_full_min 0.748