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_7719351
_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         'C18 H54 N2 Na2 O2 P2 Si4'
_chemical_formula_sum            'C18 H54 N2 Na2 O2 P2 Si4'
_chemical_formula_weight         550.91
_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             2025-05-06
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-06 deposited with the CCDC.	2025-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                98.369(3)
_cell_angle_beta                 90.807(3)
_cell_angle_gamma                106.935(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4010(3)
_cell_length_b                   9.4361(3)
_cell_length_c                   20.4747(8)
_cell_measurement_reflns_used    13594
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.7380
_cell_measurement_theta_min      4.3600
_cell_volume                     1715.96(11)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_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 0.999
_diffrn_measured_fraction_theta_max 0.976
_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     -4.00  22.00   1.00    1.00    --   34.00  91.00 135.12   26
  2  \w    -54.00 -18.00   1.00    1.00    --  -41.15 -38.00  90.00   36
  3  \w    -74.00  31.00   1.00    1.00    --  -41.15  77.00 150.00  105
  4  \w    -65.00  33.00   1.00    1.00    --  -41.15  38.00  60.00   98
  5  \w   -114.00 -57.00   1.00    1.00    --  -41.15 -38.00  90.00   57
  6  \w    -82.00 -17.00   1.00    1.00    --  -41.15 -38.00-150.00   65
  7  \w   -113.00 -20.00   1.00    1.00    --  -41.15 -38.00   0.00   93
  8  \w     30.00  93.00   1.00    1.00    --   41.15-125.00 -30.00   63
  9  \w      4.00  29.00   1.00    1.00    --   41.15  89.00 -67.57   25
 10  \w     16.00  41.00   1.00    1.00    --   50.00  81.00  53.35   25
 11  \w     16.00  42.00   1.00    1.00    --   50.00  82.00-144.61   26
 12  \w     16.00  41.00   1.00    1.00    --   50.00  81.00 144.36   25
 13  \w     16.00  41.00   1.00    1.00    --   50.00  81.00 -82.90   25
 14  \w     16.00  41.00   1.00    1.00    --   50.00  81.00  -7.30   25
 15  \w     27.00  54.00   1.00    1.00    --   58.00  70.00 172.67   27
 16  \w     31.00  64.00   1.00    1.00    --   62.00  71.00 129.40   33
 17  \w    107.00 134.00   1.00    1.00    --   66.00  69.00  80.42   27
 18  \w    110.00 138.00   1.00    1.00    --   66.00  70.00  28.47   28
 19  \w     35.00  73.00   1.00    1.00    --   66.00  69.00  80.42   38
 20  \w     35.00  71.00   1.00    1.00    --   66.00  70.00  28.47   36
 21  \w     36.00  67.00   1.00    1.00    --   66.00  69.00-101.93   31
 22  \w     35.00  83.00   1.00    1.00    --   66.00  69.00-167.80   48
 23  \w     40.00  94.00   1.00    1.00    --   70.00  71.00 -74.90   54
 24  \w     40.00  65.00   1.00    1.00    --   70.00  69.00  -7.24   25
 25  \w     74.00 101.00   1.00    2.00    --  103.09  61.00   0.00   27
 26  \w     74.00 104.00   1.00    2.00    --  103.09 -94.00  60.00   30
 27  \w    111.00 136.00   1.00    2.00    --  103.09 -77.00 120.00   25
 28  \w     29.00  88.00   1.00    2.00    --  103.09 -77.00 120.00   59
 29  \w     77.00 104.00   1.00    2.00    --  103.09  61.00 150.00   27
 30  \w    113.00 175.00   1.00    2.00    --  103.09  61.00 150.00   62
 31  \w     20.00 105.00   1.00    2.00    --  103.09 -94.00 -90.00   85
 32  \w     35.00 112.00   1.00    2.00    --  103.09-125.00-120.00   77
 33  \w    115.00 174.00   1.00    2.00    --  103.09  61.00-120.00   59
 34  \w     46.00 131.00   1.00    2.00    --  103.09 -61.00 -30.00   85
 35  \w     74.00 101.00   1.00    2.00    --  103.09  61.00-120.00   27
 36  \w     74.00 154.00   1.00    2.00    --  103.09  61.00 -90.00   80
 37  \w     74.00 101.00   1.00    2.00    --  103.09  61.00-180.00   27
 38  \w    116.00 172.00   1.00    2.00    --  103.09  61.00 120.00   56
 39  \w     75.00 175.00   1.00    2.00    --  103.09  61.00  60.00  100
 40  \w     74.00 104.00   1.00    2.00    --  103.09  61.00 120.00   30
 41  \w    114.00 142.00   1.00    2.00    --  103.09  61.00 -30.00   28
 42  \w     53.00 106.00   1.00    2.00    --  103.09 -94.00 -30.00   53
 43  \w     74.00 100.00   1.00    2.00    --  103.09  61.00 -30.00   26
 44  \w    126.00 170.00   1.00    2.00    --  103.09  61.00-180.00   44
 45  \w    109.00 153.00   1.00    2.00    --  103.09  61.00  90.00   44
 46  \w     24.00  52.00   1.00    2.00    --  103.09 -94.00 -30.00   28
 47  \w     74.00 101.00   1.00    2.00    --  103.09  61.00  90.00   27
 48  \w     74.00 166.00   1.00    2.00    --  103.09  61.00-150.00   92
 49  \w     74.00 175.00   1.00    2.00    --  103.09  61.00 -60.00  101
 50  \w    109.00 136.00   1.00    2.00    --  103.09  61.00  30.00   27
 51  \w     74.00 101.00   1.00    2.00    --  103.09  61.00  30.00   27
 52  \w    114.00 174.00   1.00    2.00    --  103.09  61.00   0.00   60
 53  \w      0.00  27.00   1.00    1.00    --   41.15  19.00  30.00   27
 54  \w     39.00  76.00   1.00    1.00    --   70.00  69.00 136.75   37
 55  \w     43.00  71.00   1.00    2.00    --   74.00  69.00  -0.10   28
;
_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      0.1455399000
_diffrn_orient_matrix_UB_12      0.1104945000
_diffrn_orient_matrix_UB_13      -0.0172383000
_diffrn_orient_matrix_UB_21      -0.0424131000
_diffrn_orient_matrix_UB_22      -0.0563046000
_diffrn_orient_matrix_UB_23      -0.0741910000
_diffrn_orient_matrix_UB_31      -0.0804247000
_diffrn_orient_matrix_UB_32      0.1203227000
_diffrn_orient_matrix_UB_33      -0.0017696000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8326
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.874
_diffrn_reflns_theta_min         4.373
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.859
_exptl_absorpt_correction_T_max  0.655
_exptl_absorpt_correction_T_min  0.544
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.219
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         8326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0194P)^2^+2.7669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7592
_reflns_number_total             8326
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9984\% 
around [-0.70 0.70 -0.15] (reciprocal) or [-0.71 0.71 0.00] (direct)
;
_cod_data_source_file            d5dt01896j2.cif
_cod_data_source_block           hasj250312a_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 7719350--7719354.cif.'
_cod_original_cell_volume        1715.95(11)
_cod_database_code               7719351
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C18H54N2Na2O2P2Si4
_shelx_estimated_absorpt_t_max   0.573
_shelx_estimated_absorpt_t_min   0.481
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4978(8)
 0.5022(8)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3.a Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C5(H5a,
 H5b,H5c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c),
 C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C13(H13a,H13b,
 H13c), C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C17(H17a,
 H17b,H17c), C18(H18a,H18b,H18c)
;
_shelx_res_checksum              85386
_shelx_hkl_checksum              19093
_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 2.075
_oxdiff_exptl_absorpt_empirical_full_min 0.703
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2