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_1571045
_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         'C25 H50 Li N Si2'
_chemical_formula_sum            'C25 H50 Li N Si2'
_chemical_formula_weight         427.78
_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             2023-12-15
_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                90
_cell_angle_beta                 102.8939(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.2445(4)
_cell_length_b                   8.91795(8)
_cell_length_c                   16.82946(17)
_cell_measurement_reflns_used    20474
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.5410
_cell_measurement_theta_min      4.8520
_cell_volume                     5448.87(10)
_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(2)
_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 0.988
_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    -70.00  32.00   1.00    1.50    --  -41.44  57.00  30.00  102
  2  \w   -114.00 -13.00   1.00    1.50    --  -41.44 -57.00-120.00  101
  3  \w    -66.00  33.00   1.00    1.50    --  -41.44  38.00-180.00   99
  4  \w     27.00  97.00   1.00    1.50    --   41.44-125.00 120.00   70
  5  \w     31.00 112.00   1.00    6.00    --  104.37-125.00  60.00   81
  6  \w     22.00 106.00   1.00    6.00    --  104.37 -94.00  90.00   84
  7  \w     22.00 106.00   1.00    6.00    --  104.37 -94.00-180.00   84
  8  \w     31.00 130.00   1.00    6.00    --  104.37 -45.00  90.00   99
  9  \w    103.00 178.00   1.00    6.00    --  104.37  77.00-180.00   75
 10  \w     31.00 112.00   1.00    6.00    --  104.37-125.00   0.00   81
 11  \w     32.00 133.00   1.00    6.00    --  104.37 -61.00-180.00  101
 12  \w     76.00 178.00   1.00    6.00    --  104.37  30.00 -30.00  102
 13  \w     75.00 177.00   1.00    6.00    --  104.37  61.00-120.00  102
 14  \w     97.00 178.00   1.00    6.00    --  104.37 125.00 120.00   81
 15  \w   -114.00 -13.00   1.00    1.50    --  -41.44 -57.00  60.00  101
 16  \w   -114.00 -13.00   1.00    1.50    --  -41.44 -57.00 -30.00  101
 17  \w    -66.00  33.00   1.00    1.50    --  -41.44  38.00 -60.00   99
 18  \w   -114.00 -13.00   1.00    1.50    --  -41.44 -57.00 150.00  101
 19  \w     75.00 143.00   1.00    6.00    --  104.37  61.00-180.00   68
 20  \w     52.00 178.00   1.00    6.00    --  104.37  15.00 120.00  126
;
_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      0.0145063000
_diffrn_orient_matrix_UB_12      -0.1389637000
_diffrn_orient_matrix_UB_13      0.0516936000
_diffrn_orient_matrix_UB_21      0.0322607000
_diffrn_orient_matrix_UB_22      -0.0116925000
_diffrn_orient_matrix_UB_23      -0.0432076000
_diffrn_orient_matrix_UB_31      0.0234452000
_diffrn_orient_matrix_UB_32      0.1019430000
_diffrn_orient_matrix_UB_33      0.0654143000
_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  0.0190
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29522
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.472
_diffrn_reflns_theta_min         4.872
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.618
_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    1.043
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.127
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0376P)^2^+4.9028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5164
_reflns_number_total             5330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06896j2.cif
_cod_data_source_block           hasj220322c
_cod_depositor_comments
'Adding full bibliography for 1571041--1571052.cif.'
_cod_original_cell_volume        5448.87(9)
_cod_database_code               1571045
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C25H50LiNSi2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
2.c Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C8(H8a,
 H8b,H8c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C14(H14a,
 H14b,H14c), C15(H15a,H15b,H15c), C17(H17a,H17b,H17c), C18(H18a,H18b,H18c),
 C25(H25a,H25b,H25c)
;
_shelx_res_checksum              55886
_shelx_hkl_checksum              95042
_olex2_date_sample_data_collection 2022-03-22
_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 1.514
_oxdiff_exptl_absorpt_empirical_full_min 0.826