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_7719353
_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 Si6 Te'
_chemical_formula_sum            'C61 H123 Mg N5 Na4 Si6 Te'
_chemical_formula_weight         1339.05
_chemical_properties_physical    Moisture-sensitive
_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_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                 97.130(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6902(3)
_cell_length_b                   28.8769(6)
_cell_length_c                   23.3975(5)
_cell_measurement_reflns_used    25673
_cell_measurement_temperature    99.96(13)
_cell_measurement_theta_max      28.9000
_cell_measurement_theta_min      2.3070
_cell_volume                     7837.4(3)
_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      99.96(13)
_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 0.904
_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    -63.00  48.00   1.00   20.00    --   15.31 -57.00-120.00  111
  2  \w    -64.00  47.00   1.00   20.00    --   15.31 -38.00 120.00  111
  3  \w     37.00 106.00   1.00   20.00    --   15.31-178.00  90.00   69
  4  \w    -42.00  22.00   1.00   20.00    --  -14.06 -77.00  60.00   64
  5  \w    -42.00 -17.00   1.00   20.00    --  -14.06 -77.00 -30.00   25
  6  \w    -17.00  93.00   1.00   20.00    --   15.31  57.00-120.00  110
;
_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      -0.0213015000
_diffrn_orient_matrix_UB_12      0.0050393000
_diffrn_orient_matrix_UB_13      -0.0290527000
_diffrn_orient_matrix_UB_21      -0.0572522000
_diffrn_orient_matrix_UB_22      -0.0007782000
_diffrn_orient_matrix_UB_23      0.0070453000
_diffrn_orient_matrix_UB_31      0.0026077000
_diffrn_orient_matrix_UB_32      0.0240240000
_diffrn_orient_matrix_UB_33      0.0063370000
_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  0.0510
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            89700
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.516
_diffrn_reflns_theta_min         1.891
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.320
_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    1.135
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.594
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.156
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         19778
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0275P)^2^+4.1879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15949
_reflns_number_total             19778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01896j2.cif
_cod_data_source_block           hasj231208b
_cod_depositor_comments
'Adding full bibliography for 7719350--7719354.cif.'
_cod_database_code               7719353
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C61H123MgN5Na4Si6Te
_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. Restrained distances
 Si6-N5 \\sim Si6A-N5
 with sigma of 0.02
 Si6-C61 \\sim Si6A-C61A \\sim Si6A-C59A \\sim Si6-C59 \\sim Si6A-C60A \\sim
Si6-C60
 with sigma of 0.02
 C42-C39 \\sim C42A-C39
 with sigma of 0.02
 C43A-C42A \\sim C43-C42
 with sigma of 0.02
 C43A-C39 \\sim C39-C43
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si6 \\sim C59 \\sim C60 \\sim C61 \\sim Si6A \\sim C59A \\sim C60A \\sim C61A:
within 4A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 4A
C42 \\sim C43 \\sim C42A \\sim C43A: within 4A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 4A
4. Rigid body (RIGU) restrains
 C39, C42, C43, C42A, C43A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Si6A)=Sof(C59A)=Sof(H59D)=Sof(H59E)=Sof(H59F)=Sof(C60A)=Sof(H60D)=
 Sof(H60E)=Sof(H60F)=Sof(C61A)=Sof(H61D)=Sof(H61E)=Sof(H61F)=1-FVAR(1)
 Sof(Si6)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C60)=Sof(H60A)=Sof(H60B)=
 Sof(H60C)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=FVAR(1)
 Sof(H39A)=Sof(C42A)=Sof(H42C)=Sof(H42D)=Sof(C43A)=Sof(H43D)=Sof(H43E)=
 Sof(H43F)=1-FVAR(2)
 Sof(H39)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=
 FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C18(H18), C23(H23), C34(H34), C39(H39), C39(H39A)
6.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), C42A(H42C,H42D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C14(H14), C15(H15), C16(H16), C30(H30), C31(H31), C32(H32)
6.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), 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), C43(H43A,H43B,H43C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C43A(H43D,H43E,H43F), C59A(H59D,H59E,
 H59F), C60A(H60D,H60E,H60F), C61A(H61D,H61E,H61F)
;
_shelx_res_checksum              9620
_shelx_hkl_checksum              97023
_olex2_date_sample_data_collection 2023-12-08
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.214
_oxdiff_exptl_absorpt_empirical_full_min 0.815