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_1571049
_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         '2(C12 H27 N0.5 Si), C16 H32 Li O8'
_chemical_formula_sum            'C40 H86 Li N O8 Si2'
_chemical_formula_weight         772.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-14
_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                 90.741(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.1279(3)
_cell_length_b                   26.8869(4)
_cell_length_c                   17.1171(3)
_cell_measurement_reflns_used    9404
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      71.7430
_cell_measurement_theta_min      3.2610
_cell_volume                     9262.6(3)
_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(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.966
_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   -115.00 -21.00   1.00    4.00    --  -40.61 -38.00 150.00   94
  2  \w      9.00  76.00   1.00    4.00    --   40.61 -99.00-180.00   67
  3  \w     27.00  80.00   1.00    4.00    --   40.61-125.00  90.00   53
  4  \w     88.00 178.00   1.00   16.00    --  104.57  45.00 120.00   90
  5  \w    103.00 178.00   1.00   16.00    --  104.57  77.00  30.00   75
  6  \w     38.00 121.00   1.00   16.00    --  104.57 -45.00 -30.00   83
  7  \w     78.00 175.00   1.00   16.00    --  104.57  61.00   0.00   97
  8  \w    111.00 178.00   1.00   16.00    --  104.57  77.00  60.00   67
;
_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      -0.0574824000
_diffrn_orient_matrix_UB_12      0.0282840000
_diffrn_orient_matrix_UB_13      0.0385916000
_diffrn_orient_matrix_UB_21      -0.0050393000
_diffrn_orient_matrix_UB_22      0.0346597000
_diffrn_orient_matrix_UB_23      -0.0715390000
_diffrn_orient_matrix_UB_31      -0.0502797000
_diffrn_orient_matrix_UB_32      -0.0357785000
_diffrn_orient_matrix_UB_33      -0.0387375000
_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  0.0253
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16992
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.337
_diffrn_reflns_theta_min         3.287
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.329
_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    1.107
_exptl_crystal_description       block
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.529
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.178
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         8855
_refine_ls_number_restraints     2200
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0780P)^2^+13.0434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7908
_reflns_number_total             8855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06896j2.cif
_cod_data_source_block           hasj211125b
_cod_depositor_comments
'Adding full bibliography for 1571041--1571052.cif.'
_cod_database_code               1571049
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C40H86LiNO8Si2
_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
 O7A-C36A \\sim O7-C36 \\sim O7A-C37A \\sim O7-C37 \\sim O8A-C38A \\sim O8-C38
\\sim O8A-C39A \\sim O8-C39
 \\sim O5A-C40A \\sim O5-C40 \\sim O5A-C33A \\sim O5-C33 \\sim O6A-C34A \\sim
O6A-C35A \\sim O6-C34 \\sim O6-
 C35 \\sim O1-C25 \\sim O1A-C25A \\sim O2-C26 \\sim O2A-C26A \\sim O2-C27 \\sim
O2A-C27A \\sim O3-C28 \\sim O3A-
 C28A \\sim O3A-C29A \\sim O3-C29 \\sim O4A-C30A \\sim O4-C30 \\sim O4A-C31A
\\sim O4-C31 \\sim O1A-C32A ~
 O1-C32
 with sigma of 0.02
 C27-C28 \\sim C27A-C28A \\sim C29-C30 \\sim C29A-C30A \\sim C31A-C32A \\sim
C31-C32 \\sim C25A-C26A ~
 C25-C26 \\sim C36A-C35A \\sim C36-C35 \\sim C34-C33 \\sim C34A-C33A \\sim
C40-C39 \\sim C40A-C39A ~
 C38-C37 \\sim C37A-C38A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1A \\sim O2A \\sim O3A \\sim O4A \\sim O5A \\sim O6A \\sim O7A \\sim O8A \\sim
C25A \\sim C26A \\sim C27A \\sim C28A \\sim C29A \\sim C30A \\sim C31A \\sim
C32A \\sim C33A \\sim C34A \\sim C35A \\sim C36A \\sim C37A \\sim C38A \\sim
C39A \\sim C40A \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7
\\sim O8 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31
\\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39
\\sim C40: within 3A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 3A
4. Others
 Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(O8A)=Sof(C33A)=Sof(H33a)=Sof(H33b)=Sof(C34A)=
 Sof(H34a)=Sof(H34b)=Sof(C35A)=Sof(H35a)=Sof(H35b)=Sof(C36A)=Sof(H36a)=
 Sof(H36b)=Sof(C37A)=Sof(H37a)=Sof(H37b)=Sof(C38A)=Sof(H38a)=Sof(H38b)=
 Sof(C39A)=Sof(H39a)=Sof(H39b)=Sof(C40A)=Sof(H40a)=Sof(H40b)=1-FVAR(1)
 Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=Sof(C33)=Sof(H33c)=Sof(H33d)=Sof(C34)=
 Sof(H34c)=Sof(H34d)=Sof(C35)=Sof(H35c)=Sof(H35d)=Sof(C36)=Sof(H36c)=Sof(H36d)=
 Sof(C37)=Sof(H37c)=Sof(H37d)=Sof(C38)=Sof(H38c)=Sof(H38d)=Sof(C39)=Sof(H39c)=
 Sof(H39d)=Sof(C40)=Sof(H40c)=Sof(H40d)=FVAR(1)
 Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(C25A)=Sof(H25a)=Sof(H25b)=Sof(C26A)=
 Sof(H26a)=Sof(H26b)=Sof(C27A)=Sof(H27a)=Sof(H27b)=Sof(C28A)=Sof(H28a)=
 Sof(H28b)=Sof(C29A)=Sof(H29a)=Sof(H29b)=Sof(C30A)=Sof(H30a)=Sof(H30b)=
 Sof(C31A)=Sof(H31a)=Sof(H31b)=Sof(C32A)=Sof(H32a)=Sof(H32b)=1-FVAR(2)
 Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(C25)=Sof(H25c)=Sof(H25d)=Sof(C26)=
 Sof(H26c)=Sof(H26d)=Sof(C27)=Sof(H27c)=Sof(H27d)=Sof(C28)=Sof(H28c)=Sof(H28d)=
 Sof(C29)=Sof(H29c)=Sof(H29d)=Sof(C30)=Sof(H30c)=Sof(H30d)=Sof(C31)=Sof(H31c)=
 Sof(H31d)=Sof(C32)=Sof(H32c)=Sof(H32d)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C25A(H25a,H25b), C26A(H26a,H26b), C27A(H27a,H27b), C28A(H28a,H28b), C29A(H29a,
 H29b), C30A(H30a,H30b), C31A(H31a,H31b), C32A(H32a,H32b), C33A(H33a,H33b),
 C34A(H34a,H34b), C35A(H35a,H35b), C36A(H36a,H36b), C37A(H37a,H37b), C38A(H38a,
 H38b), C39A(H39a,H39b), C40A(H40a,H40b), C25(H25c,H25d), C26(H26c,H26d),
 C27(H27c,H27d), C28(H28c,H28d), C29(H29c,H29d), C30(H30c,H30d), C31(H31c,H31d),
  C32(H32c,H32d), C33(H33c,H33d), C34(H34c,H34d), C35(H35c,H35d), C36(H36c,
 H36d), C37(H37c,H37d), C38(H38c,H38d), C39(H39c,H39d), C40(H40c,H40d)
5.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)
;
_shelx_res_checksum              65300
_shelx_hkl_checksum              58018
_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 1.280
_oxdiff_exptl_absorpt_empirical_full_min 0.748