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_7719354
_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         'C98 H174 Mg2 N6 Na4 Se2 Si4, [+ solvents]'
_chemical_formula_sum            'C98 H174 Mg2 N6 Na4 Se2 Si4'
_chemical_formula_weight         1847.28
_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             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                83.441(2)
_cell_angle_beta                 79.270(2)
_cell_angle_gamma                76.307(2)
_cell_formula_units_Z            2
_cell_length_a                   16.8715(3)
_cell_length_b                   18.3957(4)
_cell_length_c                   21.5617(5)
_cell_measurement_reflns_used    43323
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      72.5680
_cell_measurement_theta_min      4.1770
_cell_volume                     6370.8(2)
_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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.980
_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    -70.00  32.00   1.00    1.75    --  -41.40  57.00  60.00  102
  2  \w    -74.00  35.00   1.00    1.75    --  -41.40  77.00-180.00  109
  3  \w   -114.00 -13.00   1.00    1.75    --  -41.40 -57.00 -90.00  101
  4  \w     97.00 176.00   1.00    7.00    --  104.66 125.00 -90.00   79
  5  \w     33.00 113.00   1.00    7.00    --  104.66-125.00 -90.00   80
  6  \w     28.00 133.00   1.00    7.00    --  104.66 -30.00 -30.00  105
  7  \w     33.00 113.00   1.00    7.00    --  104.66-125.00 120.00   80
  8  \w     28.00 133.00   1.00    7.00    --  104.66 -30.00-120.00  105
  9  \w     33.00 113.00   1.00    7.00    --  104.66-125.00-150.00   80
 10  \w     97.00 176.00   1.00    7.00    --  104.66 125.00-120.00   79
 11  \w     79.00 178.00   1.00    7.00    --  104.66  45.00 -30.00   99
 12  \w     76.00 178.00   1.00    7.00    --  104.66  30.00-120.00  102
 13  \w     32.00 131.00   1.00    7.00    --  104.66 -45.00 150.00   99
 14  \w     29.00 137.00   1.00    7.00    --  104.66 -77.00 -90.00  108
 15  \w   -114.00 -13.00   1.00    1.75    --  -41.40 -57.00 -30.00  101
 16  \w   -114.00 -13.00   1.00    1.75    --  -41.40 -57.00 150.00  101
 17  \w   -114.00 -13.00   1.00    1.75    --  -41.40 -57.00  60.00  101
 18  \w     76.00 177.00   1.00    7.00    --  104.66  61.00 150.00  101
 19  \w     76.00 177.00   1.00    7.00    --  104.66  61.00   0.00  101
 20  \w     76.00 177.00   1.00    7.00    --  104.66  61.00 -90.00  101
 21  \w     76.00 177.00   1.00    7.00    --  104.66  61.00 120.00  101
 22  \w     76.00 177.00   1.00    7.00    --  104.66  61.00-180.00  101
 23  \w     76.00 177.00   1.00    7.00    --  104.66  61.00  30.00  101
 24  \w     52.00 178.00   1.00    7.00    --  104.66  15.00 120.00  126
;
_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      0.0453657000
_diffrn_orient_matrix_UB_12      0.0525872000
_diffrn_orient_matrix_UB_13      -0.0466000000
_diffrn_orient_matrix_UB_21      0.0834832000
_diffrn_orient_matrix_UB_22      -0.0540047000
_diffrn_orient_matrix_UB_23      0.0067901000
_diffrn_orient_matrix_UB_31      -0.0072139000
_diffrn_orient_matrix_UB_32      -0.0422854000
_diffrn_orient_matrix_UB_33      -0.0556714000
_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  0.0314
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            96349
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.589
_diffrn_reflns_theta_min         3.515
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.589
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.558
_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    0.963
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.108
_refine_diff_density_max         1.608
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1133
_refine_ls_number_reflns         24788
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+3.0707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21956
_reflns_number_total             24788
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01896j2.cif
_cod_data_source_block           hasj231109a
_cod_depositor_comments
'Adding full bibliography for 7719350--7719354.cif.'
_cod_database_code               7719354
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C98H174Mg2N6Na4Se2Si4
_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
 C39A-C42A \\sim C42-C39 \\sim C39A-C40A \\sim C40-C39
 with sigma of 0.02
 C39A-C33 \\sim C39-C33
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C33, C39A, C40A, C42A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40c)=Sof(H40d)=Sof(C41A)=Sof(H41d)=
 Sof(H41e)=Sof(H41f)=Sof(C42A)=Sof(H42c)=Sof(H42d)=Sof(C43A)=Sof(H43d)=
 Sof(H43e)=Sof(H43f)=1-FVAR(1)
 Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40a)=Sof(H40b)=Sof(C41)=Sof(H41a)=Sof(H41b)=
 Sof(H41c)=Sof(C42)=Sof(H42a)=Sof(H42b)=Sof(C43)=Sof(H43a)=Sof(H43b)=Sof(H43c)=
 FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C18(H18), C23(H23), C34(H34), C73(H73), C78(H78), C89(H89), C94(H94),
 C39(H39), C39A(H39A)
5.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), C74(H74a,H74b), C76(H76a,H76b), C79(H79a,H79b),
 C81(H81a,H81b), C90(H90a,H90b), C92(H92a,H92b), C95(H95a,H95b), C97(H97a,H97b),
  C40(H40a,H40b), C42(H42a,H42b), C40A(H40c,H40d), C42A(H42c,H42d)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C14(H14), C15(H15), C16(H16), C30(H30), C31(H31), C32(H32), C57(H57),
 C69(H69), C70(H70), C71(H71), C85(H85), C86(H86), C87(H87)
5.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), 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), C60(H60a,H60b,H60c), C61(H61a,H61b,H61c), C62(H62a,
 H62b,H62c), C64(H64a,H64b,H64c), C65(H65a,H65b,H65c), C66(H66a,H66b,H66c),
 C75(H75a,H75b,H75c), C77(H77a,H77b,H77c), C80(H80a,H80b,H80c), C82(H82a,H82b,
 H82c), C91(H91a,H91b,H91c), C93(H93a,H93b,H93c), C96(H96a,H96b,H96c), C98(H98a,
 H98b,H98c), C41(H41a,H41b,H41c), C43(H43a,H43b,H43c), C41A(H41d,H41e,H41f),
 C43A(H43d,H43e,H43f)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              57476
_shelx_hkl_checksum              54399
_shelx_fab_checksum              14498
_olex2_date_sample_data_collection 2023-11-09
_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 1.228
_oxdiff_exptl_absorpt_empirical_full_min 0.723