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_1571048
_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         '1(C24 H54 N Si2), C37 H58.489 Mg N2 O2'
_chemical_formula_sum            'C61 H112.49 Mg N3 O2 Si2'
_chemical_formula_weight         1000.51
_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             2023-12-14
_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                 106.935(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7968(4)
_cell_length_b                   16.8461(3)
_cell_length_c                   23.1147(5)
_cell_measurement_reflns_used    19170
_cell_measurement_temperature    99.97(11)
_cell_measurement_theta_max      72.4270
_cell_measurement_theta_min      3.8950
_cell_volume                     6256.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_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_temperature      99.97(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_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    -61.00  30.00   1.00    5.00    --  -41.15  57.00-180.00   91
  2  \w    -61.00 -14.00   1.00    5.00    --  -41.15 -57.00-150.00   47
  3  \w   -114.00 -13.00   1.00    5.00    --  -41.15 -19.00   0.00  101
  4  \w     97.00 173.00   1.00   20.00    --  104.66 125.00  60.00   76
  5  \w    115.00 164.00   1.00   20.00    --  104.66 125.00  30.00   49
  6  \w    144.00 178.00   1.00   20.00    --  104.66  77.00-150.00   34
  7  \w     95.00 164.00   1.00   20.00    --  104.66  45.00-120.00   69
  8  \w    111.00 172.00   1.00   20.00    --  104.66  77.00-180.00   61
  9  \w    133.00 160.00   1.00   20.00    --  104.66 125.00 -30.00   27
 10  \w     76.00 178.00   1.00   20.00    --  104.66  30.00 150.00  102
 11  \w     81.00 127.00   1.00   20.00    --  104.66 -45.00  90.00   46
 12  \w    -87.00 -11.00   1.00    5.00    --  -41.15 125.00 -60.00   76
 13  \w   -108.00 -81.00   1.00    5.00    --  -41.15 -38.00  30.00   27
 14  \w    -42.00 -17.00   1.00    5.00    --  -41.15 -38.00  30.00   25
 15  \w     58.00 109.00   1.00    5.00    --   41.15  38.00 -60.00   51
 16  \w    116.00 163.00   1.00   20.00    --  104.66 125.00 120.00   47
 17  \w     53.00 123.00   1.00   20.00    --  104.66 -61.00  60.00   70
 18  \w     62.00 113.00   1.00   20.00    --  104.66-125.00  90.00   51
 19  \w     82.00 113.00   1.00   20.00    --  104.66-125.00   0.00   31
 20  \w     44.00  78.00   1.00   20.00    --  104.66-125.00   0.00   34
 21  \w    124.00 154.00   1.00   20.00    --  104.66 125.00   0.00   30
 22  \w     87.00 113.00   1.00   20.00    --  104.66-125.00-180.00   26
 23  \w     81.00 107.00   1.00   20.00    --  104.66 -97.00 -33.76   26
 24  \w     80.00 124.00   1.00   20.00    --  104.66  45.00  60.00   44
 25  \w     67.00 108.00   1.00   20.00    --  104.66-105.00-137.00   41
;
_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      0.0954166000
_diffrn_orient_matrix_UB_12      -0.0088696000
_diffrn_orient_matrix_UB_13      0.0195950000
_diffrn_orient_matrix_UB_21      -0.0063234000
_diffrn_orient_matrix_UB_22      -0.0550928000
_diffrn_orient_matrix_UB_23      -0.0543833000
_diffrn_orient_matrix_UB_31      0.0068703000
_diffrn_orient_matrix_UB_32      0.0724425000
_diffrn_orient_matrix_UB_33      -0.0389022000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16924
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.626
_diffrn_reflns_theta_min         3.802
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
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    1.062
_exptl_crystal_description       block
_exptl_crystal_F_000             2222
_exptl_crystal_size_max          0.418
_exptl_crystal_size_mid          0.399
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         16924
_refine_ls_number_restraints     924
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+5.0916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14220
_reflns_number_total             16924
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9700\% 
around [0.93 0.00 -0.37] (reciprocal) or [1.00 0.00 0.00] (direct)
;
_cod_data_source_file            d3sc06896j2.cif
_cod_data_source_block           hasj231120b_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 1571041--1571052.cif.'
_cod_database_code               1571048
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C61H112.5MgN3O2Si2
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.561(1)
 0.439(1)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C37-C36 = C35-C34
 1.52 with sigma of 0.01
 C26A-C24A \\sim C26-C24 \\sim C25-C24 \\sim C25A-C24A \\sim C13A-C12A \\sim
C13-C12 \\sim C14A-C12A ~
 C14-C12 \\sim C29-C27 \\sim C27A-C29A \\sim C27A-C28A \\sim C28-C27
 with sigma of 0.02
 C24A-C19 \\sim C24-C19 \\sim C12-C7 \\sim C12A-C7 \\sim C27A-C23 \\sim C27-C23
 with sigma of 0.02
 C26A-C25A \\sim C26-C25 \\sim C28A-C29A \\sim C28-C29
 with sigma of 0.02
 C26A-C19 \\sim C19-C25A \\sim C26-C19 \\sim C19-C25 \\sim C28-C23 \\sim
C23-C28A \\sim C29A-C23 \\sim C23-
 C29
 with sigma of 0.02
 Si1A-C46A \\sim Si1-C42 \\sim Si1A-C42A \\sim Si1-C38 \\sim Si1A-C38A \\sim
Si1-C46
 with sigma of 0.02
 C36A-C34A \\sim C33-C30
 with sigma of 0.02
 C36A-C35A \\sim C37A-C34A \\sim C31A-C33 \\sim C33-C31
 with sigma of 0.02
 O2-C34 \\sim O2-C36
 with sigma of 0.02
 O1-C30 \\sim O1-C33 \\sim O2-C34A \\sim O2-C36A
 with sigma of 0.02
 C32-C31 \\sim C32-C31A \\sim C35A-C37A
 with sigma of 0.02
 C30-C32 \\sim C31A-C33 \\sim C33-C31 \\sim C34A-C37A \\sim C36A-C35A
 with sigma of 0.02
 Si2A-N3A \\sim Si2-N3 \\sim Si1-N3 \\sim Si1A-N3A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C19 \\sim C24 \\sim C25 \\sim C26 \\sim C24A \\sim C25A \\sim C26A: within 3A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3A
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
C7 \\sim C12 \\sim C13 \\sim C14 \\sim C12A \\sim C13A \\sim C14A: within 4A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 4A
C27 \\sim C28 \\sim C29 \\sim C27A \\sim C28A \\sim C29A: within 4A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 4A
C30 \\sim C32 \\sim C33 \\sim C31 \\sim C31A: within 3A with sigma of 0.03 and
sigma for terminal atoms of 0.06 within 3A
Si1A \\sim Si2A \\sim N3A \\sim Si1 \\sim Si2 \\sim N3: within 3A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 3A
5. Rigid body (RIGU) restrains
 C19, C24, C25, C26, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O2, C34, C35, C36, C37, C34A, C35A, C36A, C37A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30, C32, C33, C31, C31A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Si1A, Si2A, N3A, Si1, Si2, N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Si1A)=Sof(Si2A)=Sof(N3A)=Sof(C38A)=Sof(C39A)=Sof(H39a)=Sof(H39b)=
 Sof(H39c)=Sof(C40A)=Sof(H40a)=Sof(H40b)=Sof(H40c)=Sof(C41A)=Sof(H41a)=
 Sof(H41b)=Sof(H41c)=Sof(C42A)=Sof(C43A)=Sof(H43a)=Sof(H43b)=Sof(H43c)=
 Sof(C44A)=Sof(H44a)=Sof(H44b)=Sof(H44c)=Sof(C45A)=Sof(H45a)=Sof(H45b)=
 Sof(H45c)=Sof(C46A)=Sof(C47A)=Sof(H47a)=Sof(H47b)=Sof(H47c)=Sof(C48A)=
 Sof(H48a)=Sof(H48b)=Sof(H48c)=Sof(C49A)=Sof(H49a)=Sof(H49b)=Sof(H49c)=
 Sof(C50A)=Sof(C51A)=Sof(H51a)=Sof(H51b)=Sof(H51c)=Sof(C52A)=Sof(H52a)=
 Sof(H52b)=Sof(H52c)=Sof(C53A)=Sof(H53a)=Sof(H53b)=Sof(H53c)=Sof(C54A)=
 Sof(C55A)=Sof(H55a)=Sof(H55b)=Sof(H55c)=Sof(C56A)=Sof(H56a)=Sof(H56b)=
 Sof(H56c)=Sof(C57A)=Sof(H57a)=Sof(H57b)=Sof(H57c)=Sof(C58A)=Sof(C59A)=
 Sof(H59a)=Sof(H59b)=Sof(H59c)=Sof(C60A)=Sof(H60a)=Sof(H60b)=Sof(H60c)=
 Sof(C61A)=Sof(H61a)=Sof(H61b)=Sof(H61c)=Sof(H30c)=Sof(H30d)=Sof(H32c)=
 Sof(H32d)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13d)=Sof(H13e)=Sof(H13f)=
 Sof(C14A)=Sof(H14d)=Sof(H14e)=Sof(H14f)=Sof(C24A)=Sof(H24A)=Sof(C25A)=
 Sof(H25d)=Sof(H25e)=Sof(H25f)=Sof(C26A)=Sof(H26d)=Sof(H26e)=Sof(H26f)=
 Sof(C31A)=Sof(H31c)=Sof(H31d)=1-FVAR(1)
 Sof(Si1)=Sof(Si2)=Sof(N3)=Sof(C38)=Sof(C39)=Sof(H39d)=Sof(H39e)=Sof(H39f)=
 Sof(C40)=Sof(H40d)=Sof(H40e)=Sof(H40f)=Sof(C41)=Sof(H41d)=Sof(H41e)=Sof(H41f)=
 Sof(C42)=Sof(C43)=Sof(H43d)=Sof(H43e)=Sof(H43f)=Sof(C44)=Sof(H44d)=Sof(H44e)=
 Sof(H44f)=Sof(C45)=Sof(H45d)=Sof(H45e)=Sof(H45f)=Sof(C46)=Sof(C47)=Sof(H47d)=
 Sof(H47e)=Sof(H47f)=Sof(C48)=Sof(H48d)=Sof(H48e)=Sof(H48f)=Sof(C49)=Sof(H49d)=
 Sof(H49e)=Sof(H49f)=Sof(C50)=Sof(C51)=Sof(H51d)=Sof(H51e)=Sof(H51f)=Sof(C52)=
 Sof(H52d)=Sof(H52e)=Sof(H52f)=Sof(C53)=Sof(H53d)=Sof(H53e)=Sof(H53f)=Sof(C54)=
 Sof(C55)=Sof(H55d)=Sof(H55e)=Sof(H55f)=Sof(C56)=Sof(H56d)=Sof(H56e)=Sof(H56f)=
 Sof(C57)=Sof(H57d)=Sof(H57e)=Sof(H57f)=Sof(C58)=Sof(C59)=Sof(H59d)=Sof(H59e)=
 Sof(H59f)=Sof(C60)=Sof(H60d)=Sof(H60e)=Sof(H60f)=Sof(C61)=Sof(H61d)=Sof(H61e)=
 Sof(H61f)=Sof(H30a)=Sof(H30b)=Sof(H32a)=Sof(H32b)=Sof(C12)=Sof(H12)=Sof(C13)=
 Sof(H13a)=Sof(H13b)=Sof(H13c)=Sof(C14)=Sof(H14a)=Sof(H14b)=Sof(H14c)=Sof(C24)=
 Sof(H24)=Sof(C25)=Sof(H25a)=Sof(H25b)=Sof(H25c)=Sof(C26)=Sof(H26a)=Sof(H26b)=
 Sof(H26c)=Sof(C31)=Sof(H31a)=Sof(H31b)=FVAR(1)
 Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28d)=Sof(H28e)=Sof(H28f)=Sof(C29A)=
 Sof(H29d)=Sof(H29e)=Sof(H29f)=Sof(C34A)=Sof(H34c)=Sof(H34d)=Sof(C35A)=
 Sof(H35d)=Sof(H35e)=Sof(C36A)=Sof(H36c)=Sof(H36d)=Sof(C37A)=Sof(H37d)=
 Sof(H37e)=1-FVAR(2)
 Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28a)=Sof(H28b)=Sof(H28c)=Sof(C29)=Sof(H29a)=
 Sof(H29b)=Sof(H29c)=Sof(C34)=Sof(H34a)=Sof(H34b)=Sof(C35)=Sof(H35a)=Sof(H35b)=
 Sof(H35c)=Sof(C36)=Sof(H36a)=Sof(H36b)=Sof(C37)=Sof(H37a)=Sof(H37b)=Sof(H37c)=
 FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C15(H15), C12(H12), C24(H24), C27(H27), C12A(H12A), C24A(H24A), C27A(H27A)
7.b Secondary CH2 refined with riding coordinates:
 C30(H30c,H30d), C30(H30a,H30b), C32(H32a,H32b), C32(H32c,H32d), C33(H33a,
 H33b), C31(H31a,H31b), C34(H34a,H34b), C36(H36a,H36b), C31A(H31c,H31d),
 C34A(H34c,H34d), C35A(H35d,H35e), C36A(H36c,H36d), C37A(H37d,H37e)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22)
7.d Idealised Me refined as rotating group:
 C39A(H39a,H39b,H39c), C40A(H40a,H40b,H40c), C41A(H41a,H41b,H41c), C43A(H43a,
 H43b,H43c), C44A(H44a,H44b,H44c), C45A(H45a,H45b,H45c), C47A(H47a,H47b,H47c),
 C48A(H48a,H48b,H48c), C49A(H49a,H49b,H49c), C51A(H51a,H51b,H51c), C52A(H52a,
 H52b,H52c), C53A(H53a,H53b,H53c), C55A(H55a,H55b,H55c), C56A(H56a,H56b,H56c),
 C57A(H57a,H57b,H57c), C59A(H59a,H59b,H59c), C60A(H60a,H60b,H60c), C61A(H61a,
 H61b,H61c), C39(H39d,H39e,H39f), C40(H40d,H40e,H40f), C41(H41d,H41e,H41f),
 C43(H43d,H43e,H43f), C44(H44d,H44e,H44f), C45(H45d,H45e,H45f), C47(H47d,H47e,
 H47f), C48(H48d,H48e,H48f), C49(H49d,H49e,H49f), C51(H51d,H51e,H51f), C52(H52d,
 H52e,H52f), C53(H53d,H53e,H53f), C55(H55d,H55e,H55f), C56(H56d,H56e,H56f),
 C57(H57d,H57e,H57f), C59(H59d,H59e,H59f), C60(H60d,H60e,H60f), C61(H61d,H61e,
 H61f), C1(H1a,H1b,H1c), C5(H5a,H5b,H5c), C16(H16a,H16b,H16c), C17(H17a,H17b,
 H17c), C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C25(H25a,H25b,H25c), C26(H26a,
 H26b,H26c), C28(H28a,H28b,H28c), C29(H29a,H29b,H29c), C35(H35a,H35b,H35c),
 C37(H37a,H37b,H37c), C13A(H13d,H13e,H13f), C14A(H14d,H14e,H14f), C25A(H25d,
 H25e,H25f), C26A(H26d,H26e,H26f), C28A(H28d,H28e,H28f), C29A(H29d,H29e,H29f)
;
_shelx_res_checksum              36308
_shelx_hkl_checksum              4528
_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 1.898
_oxdiff_exptl_absorpt_empirical_full_min 0.467
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2