s-Block metal complexes of superbulky (<sup><i>t</i></sup>Bu<sub>3</sub>Si)<sub>2</sub>N<sup>-</sup>: a new weakly coordinating anion?
Knüpfer, Christian; Klerner, Lukas; Mai, Jonathan; Langer, Jens; Harder, Sjoerd; Chemical science 15 (2024) 4386–4395; doi:10.1039/d3sc06896j

data_1571052
_publ_section_title
;
 s-Block metal complexes of superbulky
 (<sup><i>t</i></sup>Bu<sub>3</sub>Si)<sub>2</sub>N<sup>-</sup>: a new
 weakly coordinating anion?
;
_journal_issue                   12
_journal_name_full               'Chemical science'
_journal_page_first              4386
_journal_page_last               4395
_journal_paper_doi               10.1039/d3sc06896j
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C24 H54 Li N Si2'
_chemical_formula_sum            'C24 H54 Li N Si2'
_chemical_formula_weight         419.80
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-22 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                86.9319(12)
_cell_angle_beta                 72.3912(13)
_cell_angle_gamma                76.3044(13)
_cell_formula_units_Z            4
_cell_length_a                   11.12464(16)
_cell_length_b                   14.7718(2)
_cell_length_c                   17.2761(3)
_cell_measurement_reflns_used    23186
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.2290
_cell_measurement_theta_min      3.0280
_cell_volume                     2628.53(7)
_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  (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 1.000
_diffrn_measured_fraction_theta_max 0.989
_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      3.00  28.00   1.00    1.00    --   38.00  85.00 115.05   25
  2  \w   -113.00 -48.00   1.00    1.00    --  -41.33 -57.00-150.00   65
  3  \w    -65.00  33.00   1.00    1.00    --  -41.33  38.00   0.00   98
  4  \w    -65.00 -18.00   1.00    1.00    --  -41.33 -38.00 -90.00   47
  5  \w   -115.00 -22.00   1.00    1.00    --  -41.33 -38.00  30.00   93
  6  \w    -47.00 -13.00   1.00    1.00    --  -41.33 -57.00-150.00   34
  7  \w     28.00  95.00   1.00    1.00    --   41.33-125.00-120.00   67
  8  \w     27.00  91.00   1.00    1.00    --   41.33-125.00 120.00   64
  9  \w     10.00  35.00   1.00    1.00    --   42.00  73.00   4.07   25
 10  \w     13.00  38.00   1.00    1.00    --   46.00  79.00  -4.81   25
 11  \w     16.00  41.00   1.00    1.00    --   50.00  82.00 -82.37   25
 12  \w     16.00  41.00   1.00    1.00    --   50.00  81.00 152.56   25
 13  \w     16.00  41.00   1.00    1.00    --   50.00  81.00  62.29   25
 14  \w     16.00  41.00   1.00    1.00    --   50.00  81.00-165.64   25
 15  \w     25.00  55.00   1.00    1.00    --   54.00  67.00 -69.71   30
 16  \w     86.00 126.00   1.00    1.00    --   54.00  67.00 -69.71   40
 17  \w    102.00 133.00   1.00    1.00    --   62.00  67.00 -32.54   31
 18  \w     32.00  57.00   1.00    1.00    --   62.00  71.00-124.64   25
 19  \w     34.00  60.00   1.00    1.00    --   62.00  67.00 -32.54   26
 20  \w     92.00 129.00   1.00    1.00    --   62.00  71.00-124.64   37
 21  \w    101.00 128.00   1.00    1.00    --   66.00  71.00   1.73   27
 22  \w     35.00  63.00   1.00    1.00    --   66.00  71.00   1.73   28
 23  \w     35.00  62.00   1.00    1.00    --   66.00  69.00 172.91   27
 24  \w     37.00  64.00   1.00    1.00    --   66.00  69.00 107.76   27
 25  \w     40.00  65.00   1.00    1.00    --   70.00  71.00 119.46   25
 26  \w    119.00 145.00   1.00    1.00    --   74.00  70.00 165.96   26
 27  \w     44.00  69.00   1.00    1.00    --   74.00  70.00  70.65   25
 28  \w     43.00  70.00   1.00    1.00    --   74.00  70.00 165.96   27
 29  \w    122.00 150.00   1.00    2.00    --   78.00  65.00 -66.64   28
 30  \w     49.00  74.00   1.00    2.00    --   78.00  65.00 -66.64   25
 31  \w     50.00  76.00   1.00    2.00    --   78.00  67.00 -99.87   26
 32  \w     48.00  73.00   1.00    2.00    --   78.00  70.00  45.86   25
 33  \w     55.00  82.00   1.00    2.00    --   82.00  71.00 -67.67   27
 34  \w     52.00  78.00   1.00    2.00    --   82.00  71.00-179.81   26
 35  \w     51.00  77.00   1.00    2.00    --   82.00  69.00  19.05   26
 36  \w     52.00  79.00   1.00    2.00    --   82.00  69.00-141.90   27
 37  \w     57.00  82.00   1.00    2.00    --   86.00  65.00  95.41   25
 38  \w    132.00 163.00   1.00    2.00    --   90.00  71.00 113.53   31
 39  \w     59.00  85.00   1.00    2.00    --   90.00  71.00 113.53   26
 40  \w     59.00  85.00   1.00    2.00    --   90.00  69.00 -41.04   26
 41  \w     63.00  89.00   1.00    2.00    --   90.00  67.00  73.52   26
 42  \w    111.00 139.00   1.00    2.00    --   90.00  71.00  44.38   28
 43  \w     59.00  85.00   1.00    2.00    --   90.00  71.00  44.38   26
 44  \w     61.00  86.00   1.00    2.00    --   90.00  66.00  -7.37   25
 45  \w     66.00  93.00   1.00    2.00    --   94.00  66.00 176.29   27
 46  \w     69.00  94.00   1.00    2.00    --   98.00  66.00-141.38   25
 47  \w     73.00 106.00   1.00    2.00    --  102.00  63.00-126.33   33
 48  \w    123.00 164.00   1.00    2.00    --  110.00  62.00 -83.23   41
 49  \w     81.00 116.00   1.00    2.00    --  110.00  62.00 -83.23   35
 50  \w    115.00 154.00   1.00    2.00    --  112.00  64.00  37.54   39
 51  \w     83.00 110.00   1.00    2.00    --  112.00  61.00 120.00   27
 52  \w     83.00 113.00   1.00    2.00    --  112.00  64.00  37.54   30
 53  \w    132.00 173.00   1.00    2.00    --  112.00  61.00 150.00   41
 54  \w     85.00 125.00   1.00    2.00    --  112.00  61.00 150.00   40
 55  \w     98.00 134.00   1.00    2.00    --  112.00 178.00 -60.00   36
 56  \w     84.00 176.00   1.00    2.00    --  112.00  61.00  60.00   92
 57  \w     83.00 178.00   1.00    2.00    --  112.00  61.00-150.00   95
 58  \w    136.00 178.00   1.00    2.00    --  112.00  54.00 -97.66   42
 59  \w    116.00 141.00   1.00    2.00    --  112.00 -61.00  60.00   25
 60  \w     84.00 114.00   1.00    2.00    --  112.00  54.00 -97.66   30
 61  \w    127.00 177.00   1.00    2.00    --  112.00  61.00 120.00   50
 62  \w     80.00 106.00   1.00    2.00    --  112.00 -61.00  60.00   26
 63  \w    109.00 138.00   1.00    2.00    --  112.00 -61.00 -90.00   29
 64  \w     46.00  85.00   1.00    2.00    --  112.00 -61.00 -90.00   39
 65  \w     84.00 174.00   1.00    2.00    --  112.00  61.00  90.00   90
 66  \w     51.00 109.00   1.00    2.00    --  112.00-111.00 120.00   58
 67  \w     92.00 132.00   1.00    2.00    --  112.00 -77.00 120.00   40
 68  \w     41.00 103.00   1.00    2.00    --  112.00-111.00 -90.00   62
 69  \w     52.00 101.00   1.00    2.00    --  112.00-111.00  90.00   49
 70  \w     43.00 109.00   1.00    2.00    --  112.00-111.00-180.00   66
 71  \w     86.00 178.00   1.00    2.00    --  112.00  61.00   0.00   92
 72  \w     83.00 120.00   1.00    2.00    --  112.00  61.00 -60.00   37
 73  \w     61.00 109.00   1.00    2.00    --  112.00-111.00   0.00   48
 74  \w    133.00 166.00   1.00    2.00    --  112.00  45.00-180.00   33
 75  \w     98.00 124.00   1.00    2.00    --  112.00  45.00-180.00   26
 76  \w     80.00 106.00   1.00    2.00    --  112.00-111.00  30.00   26
 77  \w     85.00 175.00   1.00    2.00    --  112.00  71.00 -55.67   90
 78  \w     50.00  75.00   1.00    2.00    --  112.00-111.00  30.00   25
 79  \w    129.00 154.00   1.00    2.00    --  112.00  56.00  -9.68   25
 80  \w    131.00 178.00   1.00    2.00    --  112.00  61.00 -30.00   47
 81  \w     83.00 108.00   1.00    2.00    --  112.00  61.00  30.00   25
 82  \w    126.00 151.00   1.00    2.00    --  112.00  61.00  30.00   25
 83  \w     85.00 118.00   1.00    2.00    --  112.00  56.00  -9.68   33
 84  \w     37.00  80.00   1.00    2.00    --  112.00 -77.00 120.00   43
 85  \w     85.00 112.00   1.00    2.00    --  112.00  61.00 -30.00   27
 86  \w     40.00 109.00   1.00    2.00    --  112.00-111.00 -60.00   69
 87  \w    140.00 177.00   1.00    2.00    --  112.00  61.00-180.00   37
 88  \w    129.00 154.00   1.00    2.00    --  112.00  57.00 138.90   25
 89  \w     83.00 122.00   1.00    2.00    --  112.00  61.00-180.00   39
 90  \w    120.00 170.00   1.00    2.00    --  112.00  61.00-120.00   50
 91  \w     84.00 122.00   1.00    2.00    --  112.00  57.00 138.90   38
 92  \w     84.00 110.00   1.00    2.00    --  112.00  61.00-120.00   26
 93  \w      8.00  33.00   1.00    1.00    --   41.33  80.00 -66.68   25
 94  \w     56.00  82.00   1.00    2.00    --   86.00  67.00  29.75   26
 95  \w     57.00  84.00   1.00    2.00    --   86.00  68.00 141.86   27
 96  \w     81.00 120.00   1.00    2.00    --  110.00  62.00  19.58   39
 97  \w     79.00 106.00   1.00    2.00    --  110.00  70.00-116.37   27
 98  \w      8.00  42.00   1.00    1.00    --   41.33  80.00 -66.68   34
 99  \w     16.00  42.00   1.00    1.00    --   50.00  82.00-133.02   26
;
_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      0.0419249000
_diffrn_orient_matrix_UB_12      0.0921169000
_diffrn_orient_matrix_UB_13      0.0004913000
_diffrn_orient_matrix_UB_21      0.0352958000
_diffrn_orient_matrix_UB_22      -0.0282424000
_diffrn_orient_matrix_UB_23      0.0789343000
_diffrn_orient_matrix_UB_31      0.1389375000
_diffrn_orient_matrix_UB_32      -0.0473687000
_diffrn_orient_matrix_UB_33      -0.0502529000
_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  0.0268
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60832
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.270
_diffrn_reflns_theta_min         2.684
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
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    1.061
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.474(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1388
_refine_ls_number_reflns         20603
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0659P)^2^+0.3978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.928
_reflns_Friedel_fraction_max     0.884
_reflns_number_gt                18576
_reflns_number_total             20603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06896j2.cif
_cod_data_source_block           hasj230309b
_cod_depositor_comments
'Adding full bibliography for 1571041--1571052.cif.'
_cod_original_cell_volume        2628.52(7)
_cod_database_code               1571052
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C24H54LiNSi2
_shelx_estimated_absorpt_t_max   0.820
_shelx_estimated_absorpt_t_min   0.703
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.526(18)
 0.474(18)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
3. Restrained distances
 C75A-C73A \\sim C74A-C73A \\sim C76A-C73A \\sim C81A-C82 \\sim C84A-C81A \\sim
C83A-C81A \\sim C77A-
 C79A \\sim C77A-C78A \\sim C77A-C80A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C79A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 Si7, C82, C73A, C74A, C75A, C76A, C77A, C78A, C79A, C80A, C81A, C83A, C84A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(H82d)=Sof(H82e)=Sof(H82f)=Sof(C73A)=Sof(C74A)=Sof(H74d)=Sof(H74e)=
 Sof(H74f)=Sof(C75A)=Sof(H75d)=Sof(H75e)=Sof(H75f)=Sof(C76A)=Sof(H76d)=
 Sof(H76e)=Sof(H76f)=Sof(C77A)=Sof(C78A)=Sof(H78d)=Sof(H78e)=Sof(H78f)=
 Sof(C79A)=Sof(H79d)=Sof(H79e)=Sof(H79f)=Sof(C80A)=Sof(H80d)=Sof(H80e)=
 Sof(H80f)=Sof(C81A)=Sof(C83A)=Sof(H83d)=Sof(H83e)=Sof(H83f)=Sof(C84A)=
 Sof(H84d)=Sof(H84e)=Sof(H84f)=1-FVAR(1)
 Sof(H82a)=Sof(H82b)=Sof(H82c)=Sof(C73)=Sof(C74)=Sof(H74a)=Sof(H74b)=Sof(H74c)=
 Sof(C75)=Sof(H75a)=Sof(H75b)=Sof(H75c)=Sof(C76)=Sof(H76a)=Sof(H76b)=Sof(H76c)=
 Sof(C77)=Sof(C78)=Sof(H78a)=Sof(H78b)=Sof(H78c)=Sof(C79)=Sof(H79a)=Sof(H79b)=
 Sof(H79c)=Sof(C80)=Sof(H80a)=Sof(H80b)=Sof(H80c)=Sof(C81)=Sof(C83)=Sof(H83a)=
 Sof(H83b)=Sof(H83c)=Sof(C84)=Sof(H84a)=Sof(H84b)=Sof(H84c)=FVAR(1)
7.a Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C27(H27a,H27b,H27c), C28(H28a,H28b,H28c), C30(H30a,H30b,
 H30c), C31(H31a,H31b,H31c), C32(H32a,H32b,H32c), C34(H34a,H34b,H34c), C35(H35a,
 H35b,H35c), C36(H36a,H36b,H36c), C38(H38a,H38b,H38c), C39(H39a,H39b,H39c),
 C40(H40a,H40b,H40c), C42(H42a,H42b,H42c), C43(H43a,H43b,H43c), C44(H44a,H44b,
 H44c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c), C50(H50a,
 H50b,H50c), C51(H51a,H51b,H51c), C52(H52a,H52b,H52c), C54(H54a,H54b,H54c),
 C55(H55a,H55b,H55c), C56(H56a,H56b,H56c), C58(H58a,H58b,H58c), C59(H59a,H59b,
 H59c), C60(H60a,H60b,H60c), C62(H62a,H62b,H62c), C63(H63a,H63b,H63c), C64(H64a,
 H64b,H64c), C66(H66a,H66b,H66c), C67(H67a,H67b,H67c), C68(H68a,H68b,H68c),
 C70(H70a,H70b,H70c), C71(H71a,H71b,H71c), C72(H72a,H72b,H72c), C82(H82a,H82b,
 H82c), C82(H82d,H82e,H82f), C86(H86a,H86b,H86c), C87(H87a,H87b,H87c), C88(H88a,
 H88b,H88c), C90(H90a,H90b,H90c), C91(H91a,H91b,H91c), C92(H92a,H92b,H92c),
 C94(H94a,H94b,H94c), C95(H95a,H95b,H95c), C96(H96a,H96b,H96c), C74(H74a,H74b,
 H74c), C75(H75a,H75b,H75c), C76(H76a,H76b,H76c), C78(H78a,H78b,H78c), C79(H79a,
 H79b,H79c), C80(H80a,H80b,H80c), C83(H83a,H83b,H83c), C84(H84a,H84b,H84c),
 C74A(H74d,H74e,H74f), C75A(H75d,H75e,H75f), C76A(H76d,H76e,H76f), C78A(H78d,
 H78e,H78f), C79A(H79d,H79e,H79f), C80A(H80d,H80e,H80f), C83A(H83d,H83e,H83f),
 C84A(H84d,H84e,H84f)
;
_shelx_res_checksum              95828
_shelx_hkl_checksum              85847
_olex2_date_sample_data_collection 2023-03-09
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.348
_oxdiff_exptl_absorpt_empirical_full_min 0.603