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_1571041
_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)'
_chemical_formula_sum            'C24 H54 N Si2'
_chemical_formula_weight         412.86
_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             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                76.376(5)
_cell_angle_beta                 86.941(4)
_cell_angle_gamma                72.404(5)
_cell_formula_units_Z            2
_cell_length_a                   8.6659(5)
_cell_length_b                   11.1071(6)
_cell_length_c                   14.7913(8)
_cell_measurement_reflns_used    5658
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.4070
_cell_measurement_theta_min      4.2670
_cell_volume                     1318.66(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.969
_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    -69.00  33.00   1.00    1.00    --  -40.61  57.00 150.00  102
  2  \w    -73.00  36.00   1.00    1.00    --  -40.61  77.00 -90.00  109
  3  \w     12.00 114.00   1.00    1.00    --   40.61  57.00  30.00  102
  4  \w    104.00 178.00   1.00    1.00    --  104.57 111.00 -30.00   74
  5  \w    104.00 178.00   1.00    1.00    --  104.57 111.00 -90.00   74
  6  \w     28.00 109.00   1.00    1.00    --  104.57-111.00 -90.00   81
  7  \w     61.00 146.00   1.00    1.00    --  104.57 178.00 -90.00   85
  8  \w     28.00 137.00   1.00    1.00    --  104.57 -77.00-120.00  109
  9  \w     76.00 178.00   1.00    1.00    --  104.57  30.00  90.00  102
 10  \w     28.00 109.00   1.00    1.00    --  104.57-111.00  60.00   81
 11  \w     92.00 176.00   1.00    1.00    --  104.57  30.00  30.00   84
 12  \w     29.00 133.00   1.00    1.00    --  104.57 -30.00-150.00  104
 13  \w     33.00 133.00   1.00    1.00    --  104.57 -61.00   0.00  100
;
_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      0.0569800000
_diffrn_orient_matrix_UB_12      -0.1016873000
_diffrn_orient_matrix_UB_13      0.0917461000
_diffrn_orient_matrix_UB_21      0.1601497000
_diffrn_orient_matrix_UB_22      0.0341497000
_diffrn_orient_matrix_UB_23      -0.0037149000
_diffrn_orient_matrix_UB_31      -0.0768118000
_diffrn_orient_matrix_UB_32      0.1041852000
_diffrn_orient_matrix_UB_33      0.0553008000
_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  0.0213
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9950
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.225
_diffrn_reflns_theta_min         4.291
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.040
_exptl_crystal_description       block
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.167
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5068
_refine_ls_number_restraints     1546
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0475P)^2^+0.3211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4567
_reflns_number_total             5068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06896j2.cif
_cod_data_source_block           hasj200807a
_cod_depositor_comments
'Adding full bibliography for 1571041--1571052.cif.'
_cod_original_cell_volume        1318.67(13)
_cod_database_code               1571041
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C24H54NSi2
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.725
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 Si2A-C17A \\sim Si2-C17 \\sim Si2A-C21A \\sim Si2-C21 \\sim Si2-C13 \\sim
Si2A-C13A
 with sigma of 0.02
 Si2A-N2 \\sim Si2-N2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N2 \\sim Si2 \\sim C17 \\sim C21 \\sim C13 \\sim C23 \\sim C21A \\sim Si2A
\\sim C16 \\sim C15A \\sim C14 \\sim C13A \\sim C15 \\sim C20 \\sim C17A \\sim
C20A \\sim C18 \\sim C19A \\sim C18A \\sim C19 \\sim C24 \\sim C22 \\sim C24A
\\sim C22A \\sim C16A \\sim C23A: within 4A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 4A
4. Rigid body (RIGU) restrains
 Si2, C21, C17, C13, N2, C23, C24, C22, C18, C19, C20, C15, C16, C14, Si2A,
 C13A, C17A, C21A, C15A, C16A, C20A, C19A, C18A, C24A, C22A, C23A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Si2A, C22A, C21A, C24A, C23A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(H14d)=Sof(H14e)=Sof(H14f)=Sof(C15A)=Sof(H15d)=Sof(H15e)=Sof(H15f)=
 Sof(C13A)=Sof(C16A)=Sof(H16d)=Sof(H16e)=Sof(H16f)=Sof(C17A)=Sof(C20A)=
 Sof(H20d)=Sof(H20e)=Sof(H20f)=Sof(C19A)=Sof(H19d)=Sof(H19e)=Sof(H19f)=
 Sof(C24A)=Sof(H24d)=Sof(H24e)=Sof(H24f)=Sof(C21A)=Sof(C22A)=Sof(H22d)=
 Sof(H22e)=Sof(H22f)=Sof(C18A)=Sof(H18d)=Sof(H18e)=Sof(H18f)=Sof(Si2A)=
 Sof(C23A)=Sof(H23d)=Sof(H23e)=Sof(H23f)=1-FVAR(1)
 Sof(Si2)=Sof(H14a)=Sof(H14b)=Sof(H14c)=Sof(C21)=Sof(C17)=Sof(C13)=Sof(C23)=
 Sof(H23a)=Sof(H23b)=Sof(H23c)=Sof(C18)=Sof(H18a)=Sof(H18b)=Sof(H18c)=Sof(C15)=
 Sof(H15a)=Sof(H15b)=Sof(H15c)=Sof(C24)=Sof(H24a)=Sof(H24b)=Sof(H24c)=Sof(C19)=
 Sof(H19a)=Sof(H19b)=Sof(H19c)=Sof(C16)=Sof(H16a)=Sof(H16b)=Sof(H16c)=Sof(C20)=
 Sof(H20a)=Sof(H20b)=Sof(H20c)=Sof(C22)=Sof(H22a)=Sof(H22b)=Sof(H22c)=FVAR(1)
6.a Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C14(H14a,H14b,H14c), C14(H14d,H14e,H14f), C4(H4a,H4b,H4c),
 C10(H10a,H10b,H10c), C6(H6a,H6b,H6c), C8(H8a,H8b,H8c), C12(H12a,H12b,H12c),
 C7(H7a,H7b,H7c), C3(H3a,H3b,H3c), C11(H11a,H11b,H11c), C23(H23a,H23b,H23c),
 C18(H18a,H18b,H18c), C15(H15a,H15b,H15c), C24(H24a,H24b,H24c), C19(H19a,H19b,
 H19c), C16(H16a,H16b,H16c), C20(H20a,H20b,H20c), C22(H22a,H22b,H22c),
 C15A(H15d,H15e,H15f), C16A(H16d,H16e,H16f), C20A(H20d,H20e,H20f), C19A(H19d,
 H19e,H19f), C24A(H24d,H24e,H24f), C22A(H22d,H22e,H22f), C18A(H18d,H18e,H18f),
 C23A(H23d,H23e,H23f)
;
_shelx_res_checksum              79554
_shelx_hkl_checksum              14767
_olex2_date_sample_data_collection 2020-08-07
_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 1.188
_oxdiff_exptl_absorpt_empirical_full_min 0.873