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_1571042
_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_formula_moiety         'C20 H40 K O8, C24 H54 N Si2'
_chemical_formula_sum            'C44 H94 K N O8 Si2'
_chemical_formula_weight         860.48
_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             2022-07-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-12-22 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                80.1846(15)
_cell_angle_beta                 78.8889(16)
_cell_angle_gamma                83.5830(15)
_cell_formula_units_Z            3
_cell_length_a                   10.7820(2)
_cell_length_b                   15.4196(3)
_cell_length_c                   23.6530(4)
_cell_measurement_reflns_used    13364
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      72.2800
_cell_measurement_theta_min      2.8850
_cell_volume                     3789.53(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_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 0.973
_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   -113.00 -12.00   1.00    1.00    --  -40.61 -57.00 120.00  101
  2  \w    -69.00  33.00   1.00    1.00    --  -40.61  57.00 -90.00  102
  3  \w    -65.00  34.00   1.00    1.00    --  -40.61  38.00  60.00   99
  4  \w     27.00  97.00   1.00    1.00    --   40.61-125.00  60.00   70
  5  \w     76.00 178.00   1.00    2.03    --  104.57  30.00  60.00  102
  6  \w     28.00 109.00   1.00    2.03    --  104.57-111.00-180.00   81
  7  \w     76.00 178.00   1.00    2.03    --  104.57  30.00 -30.00  102
  8  \w     28.00 133.00   1.00    2.03    --  104.57 -30.00   0.00  105
  9  \w     22.00 106.00   1.00    2.03    --  104.57 -94.00-120.00   84
 10  \w     32.00 134.00   1.00    2.03    --  104.57 -61.00-120.00  102
 11  \w    104.00 178.00   1.00    2.03    --  104.57 111.00 -30.00   74
 12  \w     38.00  65.00   1.00    2.03    --  104.57-126.00  41.00   27
 13  \w     84.00 113.00   1.00    2.03    --  104.57-126.00  41.00   29
 14  \w     50.00  77.00   1.00    2.03    --  104.57 -45.00 120.00   27
 15  \w     89.00 130.00   1.00    2.03    --  104.57 -45.00 120.00   41
 16  \w     48.00 135.00   1.00    2.03    --  104.57 -77.00   0.00   87
;
_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      0.0097221000
_diffrn_orient_matrix_UB_12      0.1006161000
_diffrn_orient_matrix_UB_13      -0.0119803000
_diffrn_orient_matrix_UB_21      0.0140418000
_diffrn_orient_matrix_UB_22      -0.0013616000
_diffrn_orient_matrix_UB_23      -0.0659115000
_diffrn_orient_matrix_UB_31      -0.1450978000
_diffrn_orient_matrix_UB_32      0.0149700000
_diffrn_orient_matrix_UB_33      0.0048125000
_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  0.0352
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28075
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.266
_diffrn_reflns_theta_min         2.918
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.739
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
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    1.131
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.439
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         14567
_refine_ls_number_restraints     739
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0676P)^2^+0.5872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12634
_reflns_number_total             14567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06896j2.cif
_cod_data_source_block           hasj210730a
_cod_depositor_comments
'Adding full bibliography for 1571041--1571052.cif.'
_cod_original_cell_volume        3789.54(12)
_cod_database_code               1571042
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C44H94KNO8Si2
_shelx_estimated_absorpt_t_max   0.661
_shelx_estimated_absorpt_t_min   0.516
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 Si1-C35 \\sim Si1-C35A \\sim Si1-C39A \\sim Si1-C39 \\sim Si1-C31A \\sim
Si1-C31
 with sigma of 0.02
 C38-C35 \\sim C38A-C35A \\sim C36A-C35A \\sim C36-C35 \\sim C37A-C35A \\sim
C37-C35 \\sim C34-C31 ~
 C34-C31A \\sim C32A-C31A \\sim C33A-C31A \\sim C32-C31 \\sim C33-C31 \\sim
C42A-C39A \\sim C42-C39 ~
 C40-C39 \\sim C40A-C39A \\sim C41-C39 \\sim C41A-C39A
 with sigma of 0.02
 K2-O12 \\sim K2-O12A
 with sigma of 0.02
 C28A-C29A \\sim C29-C28 \\sim C8-C9 \\sim C8A-C9A \\sim C25A-C24A \\sim C25-C24
 with sigma of 0.02
 C28-C27 \\sim C27A-C28A \\sim C29A-C30A \\sim C30-C29 \\sim C24-C23 \\sim
C24A-C23 \\sim C26-C25A ~
 C26-C25 \\sim C8A-C7 \\sim C8-C7 \\sim C10-C9A \\sim C10-C9
 with sigma of 0.02
 O12A-C27A \\sim O12-C27 \\sim O12A-C30A \\sim O12-C30
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O11 \\sim C23 \\sim C26 \\sim C24 \\sim C25 \\sim C24A \\sim C25A: within 3A
with sigma of 0.03 and sigma for terminal atoms of 0.06 within 3A
O12 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim O12A \\sim C27A \\sim C28A
\\sim C29A \\sim C30A: within 4A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 4A
4. Rigid body (RIGU) restrains
 C39, C42, C39A, C42A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11, C23, C26, C24, C25, C24A, C25A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O12A, C27A, C28A, C29A, C30A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C31)=Sof(C32)=Sof(H32D)=Sof(H32E)=Sof(H32F)=
 Sof(C33)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C35A)=Sof(C36A)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38A)=Sof(H38D)=
 Sof(H38E)=Sof(H38F)=Sof(C39A)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=
 Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42A)=Sof(H42D)=Sof(H42E)=
 Sof(H42F)=1-FVAR(1)
 Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C31A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=
 Sof(H32C)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C35)=Sof(C36)=Sof(H36A)=
 Sof(H36B)=Sof(H36C)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=
 Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41)=
 Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(1)
 Sof(H23C)=Sof(H23D)=Sof(H26C)=Sof(H26D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=
 Sof(C25A)=Sof(H25C)=Sof(H25D)=1-FVAR(2)
 Sof(H23A)=Sof(H23B)=Sof(H26A)=Sof(H26B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=FVAR(2)
 Sof(O12A)=Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=1-FVAR(3)
 Sof(O12)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=
 Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=FVAR(3)
 Sof(H7BC)=Sof(H7BD)=Sof(H10C)=Sof(H10D)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=1-FVAR(4)
 Sof(H7AA)=Sof(H7AB)=Sof(H10A)=Sof(H10B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7AA,H7AB), C7(H7BC,H7BD), C10(H10A,H10B), C10(H10C,H10D), C8(H8A,H8B),
 C9(H9A,H9B), C8A(H8AA,H8AB), C9A(H9AA,H9AB), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
  C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C23(H23A,H23B), C23(H23C,H23D), C26(H26A,H26B), C26(H26C,H26D),
 C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
  C30(H30A,H30B), C24A(H24C,H24D), C25A(H25C,H25D), C27A(H27C,H27D), C28A(H28C,
 H28D), C29A(H29C,H29D), C30A(H30C,H30D)
6.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C34(H34D,H34E,H34F), C32A(H32A,H32B,H32C), C33A(H33A,
 H33B,H33C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C32(H32D,H32E,
 H32F), C33(H33D,H33E,H33F), C36A(H36D,H36E,H36F), C37A(H37D,H37E,H37F),
 C38A(H38D,H38E,H38F), C40A(H40D,H40E,H40F), C41A(H41D,H41E,H41F), C42A(H42D,
 H42E,H42F), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C),
 C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C)
;
_shelx_res_checksum              39205
_shelx_hkl_checksum              63331
_olex2_date_sample_data_collection 2021-07-30
_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 1.294
_oxdiff_exptl_absorpt_empirical_full_min 0.761