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_1571044
_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         'C24 H54 N Si2, C13 H31 Li N3 O'
_chemical_formula_sum            'C37 H85 Li N4 O Si2'
_chemical_formula_weight         665.20
_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             2023-12-18
_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                90
_cell_angle_beta                 96.5480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.03040(10)
_cell_length_b                   26.9733(3)
_cell_length_c                   17.9436(2)
_cell_measurement_reflns_used    10621
_cell_measurement_temperature    100.0(6)
_cell_measurement_theta_max      75.5760
_cell_measurement_theta_min      2.9520
_cell_volume                     4342.19(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.963
_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   -129.00  44.00   1.00    1.50    --  -41.69   0.00 120.00  173
  2  \w     32.00  77.00   1.00    1.50    --   41.69-125.00  90.00   45
  3  \w     41.00 139.00   1.00    6.00    --  111.00 -61.00 120.00   98
  4  \w    110.00 137.00   1.00    6.00    --  111.00 -77.00   0.00   27
  5  \w     82.00 172.00   1.00    6.00    --  111.00  61.00 -90.00   90
  6  \w     38.00 108.00   1.00    6.00    --  111.00-111.00  90.00   70
  7  \w     35.00  83.00   1.00    6.00    --  111.00 -77.00   0.00   48
  8  \w    115.00 175.00   1.00    6.00    --  111.00  77.00 150.00   60
;
_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      0.0123732000
_diffrn_orient_matrix_UB_12      -0.0309891000
_diffrn_orient_matrix_UB_13      -0.0712243000
_diffrn_orient_matrix_UB_21      0.1710851000
_diffrn_orient_matrix_UB_22      0.0037160000
_diffrn_orient_matrix_UB_23      0.0136200000
_diffrn_orient_matrix_UB_31      0.0051760000
_diffrn_orient_matrix_UB_32      -0.0478388000
_diffrn_orient_matrix_UB_33      0.0470943000
_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  0.0171
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15845
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.767
_diffrn_reflns_theta_min         2.971
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.018
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.239
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         8713
_refine_ls_number_restraints     1551
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0576P)^2^+1.5762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8141
_reflns_number_total             8713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06896j2.cif
_cod_data_source_block           hasj211125a
_cod_depositor_comments
'Adding full bibliography for 1571041--1571052.cif.'
_cod_original_cell_volume        4342.18(8)
_cod_database_code               1571044
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C37H85LiN4OSi2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C25 \\sim N2-C26A \\sim N2-C26 \\sim N3A-C29A \\sim N4-C33 \\sim N4-C32
\\sim N4A-C32A \\sim N4A-C33A
 \\sim N3-C29
 with sigma of 0.02
 C33A-C32A \\sim C32-C33
 with sigma of 0.02
 N3A-C30A \\sim N4-C31 \\sim N3-C30 \\sim N4A-C31A \\sim N3-C28 \\sim N2-C27
\\sim N2-C27A \\sim N3A-C28A
 with sigma of 0.02
 C31-C30 \\sim C30A-C31A \\sim C27A-C28A \\sim C28-C27
 with sigma of 0.02
 C34-C35 \\sim C35A-C34A \\sim C37A-C36A \\sim C36-C37
 with sigma of 0.02
 O1-C34A \\sim O1-C34 \\sim O1-C37A \\sim O1-C37
 with sigma of 0.02
 C35-C36 \\sim C36A-C35A
 with sigma of 0.02
 C34A-C36A \\sim C35A-C37A \\sim C34-C36 \\sim C35-C37
 with sigma of 0.02
 N3-Li1 \\sim N4A-Li1A \\sim N2-Li1A \\sim N2-Li1 \\sim N4-Li1 \\sim N3A-Li1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N2 \\sim N3 \\sim N4 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim
C31 \\sim C32 \\sim C33 \\sim Li1 \\sim Li1 \\sim N3A \\sim N4A \\sim C26A
\\sim C27A \\sim C28A \\sim C29A \\sim C30A \\sim C31A \\sim C32A \\sim C33A
\\sim Li1A: within 4A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 4A
O1 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C34A \\sim C35A \\sim C36A
\\sim C37A: within 4A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 4A
4. Rigid body (RIGU) restrains
 O1, C34, C35, C36, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C34A, C35A, C36A, C37A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N3A)=Sof(N4A)=Sof(C26A)=Sof(H26d)=Sof(H26e)=Sof(H26f)=Sof(C27A)=Sof(H27c)=
 Sof(H27d)=Sof(C28A)=Sof(H28c)=Sof(H28d)=Sof(C29A)=Sof(H29d)=Sof(H29e)=
 Sof(H29f)=Sof(C30A)=Sof(H30c)=Sof(H30d)=Sof(C31A)=Sof(H31c)=Sof(H31d)=
 Sof(C32A)=Sof(H32d)=Sof(H32e)=Sof(H32f)=Sof(C33A)=Sof(H33d)=Sof(H33e)=
 Sof(H33f)=Sof(Li1A)=1-FVAR(1)
 Sof(N3)=Sof(N4)=Sof(C26)=Sof(H26a)=Sof(H26b)=Sof(H26c)=Sof(C27)=Sof(H27a)=
 Sof(H27b)=Sof(C28)=Sof(H28a)=Sof(H28b)=Sof(C29)=Sof(H29a)=Sof(H29b)=Sof(H29c)=
 Sof(C30)=Sof(H30a)=Sof(H30b)=Sof(C31)=Sof(H31a)=Sof(H31b)=Sof(C32)=Sof(H32a)=
 Sof(H32b)=Sof(H32c)=Sof(C33)=Sof(H33a)=Sof(H33b)=Sof(H33c)=Sof(Li1)=FVAR(1)
 Sof(C34A)=Sof(H34c)=Sof(H34d)=Sof(C35A)=Sof(H35c)=Sof(H35d)=Sof(C36A)=
 Sof(H36c)=Sof(H36d)=Sof(C37A)=Sof(H37c)=Sof(H37d)=1-FVAR(2)
 Sof(C34)=Sof(H34a)=Sof(H34b)=Sof(C35)=Sof(H35a)=Sof(H35b)=Sof(C36)=Sof(H36a)=
 Sof(H36b)=Sof(C37)=Sof(H37a)=Sof(H37b)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C27(H27a,H27b), C28(H28a,H28b), C30(H30a,H30b), C31(H31a,H31b), C34(H34a,
 H34b), C35(H35a,H35b), C36(H36a,H36b), C37(H37a,H37b), C27A(H27c,H27d),
 C28A(H28c,H28d), C30A(H30c,H30d), C31A(H31c,H31d), C34A(H34c,H34d), C35A(H35c,
 H35d), C36A(H36c,H36d), C37A(H37c,H37d)
6.b Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C6(H6a,H6b,H6c), C7(H7a,
 H7b,H7c), C8(H8a,H8b,H8c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C12(H12a,
 H12b,H12c), C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c),
 C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C22(H22a,H22b,
 H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C25(H25a,H25b,H25c), C26(H26a,
 H26b,H26c), C29(H29a,H29b,H29c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c),
 C26A(H26d,H26e,H26f), C29A(H29d,H29e,H29f), C32A(H32d,H32e,H32f), C33A(H33d,
 H33e,H33f)
;
_shelx_res_checksum              47856
_shelx_hkl_checksum              40348
_olex2_date_sample_data_collection 2021-11-25
_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 1.219
_oxdiff_exptl_absorpt_empirical_full_min 0.883