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_7719352
_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 N5 Na4 Se Si6'
_chemical_formula_sum            'C61 H123 Mg N5 Na4 Se Si6'
_chemical_formula_weight         1290.41
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-06
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7181)
;
_audit_update_record
;
2025-03-06 deposited with the CCDC.	2025-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.2720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.16500(10)
_cell_length_b                   27.8494(2)
_cell_length_c                   22.5057(2)
_cell_measurement_reflns_used    24934
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.5160
_cell_measurement_theta_min      4.6670
_cell_volume                     7545.33(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_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_temperature      100.00(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 0.988
_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    -69.00  32.00   1.00    1.00    --  -41.15  57.00  60.00  101
  2  \w   -115.00 -17.00   1.00    1.00    --  -41.15 -38.00 120.00   98
  3  \w    -66.00  33.00   1.00    1.00    --  -41.15  38.00 -60.00   99
  4  \w     33.00 101.00   1.00    1.00    --   41.15-133.00-153.00   68
  5  \w     23.00 157.00   1.00    3.00    --  104.66 -15.00 120.00  134
  6  \w    103.00 178.00   1.00    3.00    --  104.66  77.00-150.00   75
  7  \w     97.00 176.00   1.00    3.00    --  104.66 125.00-120.00   79
  8  \w     33.00 113.00   1.00    3.00    --  104.66-125.00 -60.00   80
  9  \w     22.00 106.00   1.00    3.00    --  104.66 -94.00 -30.00   84
 10  \w     22.00 106.00   1.00    3.00    --  104.66 -94.00  60.00   84
 11  \w     79.00 178.00   1.00    3.00    --  104.66  45.00 -60.00   99
 12  \w     28.00 133.00   1.00    3.00    --  104.66 -30.00 -90.00  105
 13  \w     22.00 106.00   1.00    3.00    --  104.66 -94.00-180.00   84
 14  \w     32.00 134.00   1.00    3.00    --  104.66 -61.00 150.00  102
 15  \w   -114.00 -13.00   1.00    1.00    --  -41.15 -57.00 120.00  101
 16  \w   -114.00 -13.00   1.00    1.00    --  -41.15 -57.00-150.00  101
 17  \w   -114.00 -13.00   1.00    1.00    --  -41.15 -57.00 -60.00  101
 18  \w   -114.00 -13.00   1.00    1.00    --  -41.15 -57.00  30.00  101
 19  \w     76.00 177.00   1.00    3.00    --  104.66  61.00   0.00  101
 20  \w     76.00 151.00   1.00    3.00    --  104.66  61.00-150.00   75
;
_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      0.0632396000
_diffrn_orient_matrix_UB_12      0.0420376000
_diffrn_orient_matrix_UB_13      0.0338346000
_diffrn_orient_matrix_UB_21      -0.0159714000
_diffrn_orient_matrix_UB_22      -0.0232139000
_diffrn_orient_matrix_UB_23      0.0603439000
_diffrn_orient_matrix_UB_31      0.1100746000
_diffrn_orient_matrix_UB_32      -0.0274611000
_diffrn_orient_matrix_UB_33      0.0009365000
_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  0.0297
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42406
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.576
_diffrn_reflns_theta_min         3.744
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.169
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.426
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
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    1.136
_exptl_crystal_description       block
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+7.1292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7045
_reflns_number_total             7413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01896j2.cif
_cod_data_source_block           hasj231026a
_cod_depositor_comments
'Adding full bibliography for 7719350--7719354.cif.'
_cod_database_code               7719352
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C61H123MgN5Na4SeSi6
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.523
_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:
 C13(H13), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C16(H16A,H16B), C19(H19A,H19B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C10(H10), C11(H11)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C15(H15A,H15B,H15C),
 C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              20271
_shelx_hkl_checksum              56151
_olex2_date_sample_data_collection 2023-10-26
_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 1.285
_oxdiff_exptl_absorpt_empirical_full_min 0.879