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_1571047
_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 H48 I O6 Sr, C24 H54 N Si2, 2(C4 H8 O)'
_chemical_formula_sum            'C56 H118 I N O8 Si2 Sr'
_chemical_formula_weight         1204.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 106.4553(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1783(2)
_cell_length_b                   12.98186(13)
_cell_length_c                   25.3950(3)
_cell_measurement_reflns_used    15537
_cell_measurement_temperature    100.0(6)
_cell_measurement_theta_max      72.5720
_cell_measurement_theta_min      3.8280
_cell_volume                     6379.80(12)
_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 0.997
_diffrn_measured_fraction_theta_max 0.968
_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   -116.00 -19.00   1.00    1.00    --  -41.44 -38.00   0.00   97
  2  \w     19.00  70.00   1.00    1.00    --   41.44 -99.00  30.00   51
  3  \w     27.00  89.00   1.00    1.00    --   41.44-125.00-180.00   62
  4  \w     43.00 128.00   1.00    4.00    --  104.37 -30.00-150.00   85
  5  \w     97.00 178.00   1.00    4.00    --  104.37 125.00 -60.00   81
  6  \w     76.00 158.00   1.00    4.00    --  104.37  30.00 120.00   82
  7  \w     49.00 132.00   1.00    4.00    --  104.37 -77.00-150.00   83
  8  \w     56.00 133.00   1.00    4.00    --  104.37 -30.00 120.00   77
;
_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      -0.0732471000
_diffrn_orient_matrix_UB_12      -0.0354842000
_diffrn_orient_matrix_UB_13      -0.0318559000
_diffrn_orient_matrix_UB_21      0.0272728000
_diffrn_orient_matrix_UB_22      -0.1102866000
_diffrn_orient_matrix_UB_23      -0.0026119000
_diffrn_orient_matrix_UB_31      -0.0152621000
_diffrn_orient_matrix_UB_32      -0.0262922000
_diffrn_orient_matrix_UB_33      0.0545020000
_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  0.0278
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23607
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.724
_diffrn_reflns_theta_min         3.295
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.697
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.214
_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    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.234
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         12282
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+1.1536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11652
_reflns_number_total             12282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06896j2.cif
_cod_data_source_block           hasj211029b
_cod_depositor_comments
'Adding full bibliography for 1571041--1571052.cif.'
_cod_original_cell_volume        6379.80(13)
_cod_database_code               1571047
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C56H118INO8Si2Sr
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O7-C49 \\sim O7A-C49 \\sim O7A-C52A \\sim O7-C52 \\sim O6-C24A \\sim O6-C24
\\sim O8-C56A \\sim O8-C56 ~
 O8-C53
 with sigma of 0.02
 C23A-C24A \\sim C23-C24 \\sim C56A-C55A \\sim C55-C56 \\sim C53-C54A \\sim
C53-C54 \\sim C10A-C9A ~
 C10-C9 \\sim C51-C52A \\sim C51-C52
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O6 \\sim C22 \\sim C23 \\sim C24 \\sim C23A \\sim C24A: within 4A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 4A
C49 \\sim C51 \\sim O7 \\sim C52 \\sim O7A \\sim C52A: within 4A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 4A
4. Rigid body (RIGU) restrains
 O3, C9A, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H22c)=Sof(H22d)=Sof(C23A)=Sof(H23c)=Sof(H23d)=Sof(C24A)=Sof(H24c)=
 Sof(H24d)=1-FVAR(1)
 Sof(H22a)=Sof(H22b)=Sof(C23)=Sof(H23a)=Sof(H23b)=Sof(C24)=Sof(H24a)=Sof(H24b)=
 FVAR(1)
 Sof(H53c)=Sof(H53d)=Sof(C54A)=Sof(H54c)=Sof(H54d)=Sof(C55A)=Sof(H55c)=
 Sof(H55d)=Sof(C56A)=Sof(H56c)=Sof(H56d)=1-FVAR(2)
 Sof(H53a)=Sof(H53b)=Sof(C54)=Sof(H54a)=Sof(H54b)=Sof(C55)=Sof(H55a)=Sof(H55b)=
 Sof(C56)=Sof(H56a)=Sof(H56b)=FVAR(2)
 Sof(H11c)=Sof(H11d)=Sof(C9A)=Sof(H9Aa)=Sof(H9Ab)=Sof(C10A)=Sof(H10c)=
 Sof(H10d)=1-FVAR(3)
 Sof(H11a)=Sof(H11b)=Sof(C9)=Sof(H9a)=Sof(H9b)=Sof(C10)=Sof(H10a)=Sof(H10b)=
 FVAR(3)
 Sof(H49c)=Sof(H49d)=Sof(H51c)=Sof(H51d)=Sof(O7A)=Sof(C52A)=Sof(H52c)=
 Sof(H52d)=1-FVAR(4)
 Sof(H49a)=Sof(H49b)=Sof(H51a)=Sof(H51b)=Sof(O7)=Sof(C52)=Sof(H52a)=Sof(H52b)=
 FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b),
 C7(H7a,H7b), C8(H8a,H8b), C11(H11a,H11b), C11(H11c,H11d), C12(H12a,H12b),
 C13(H13a,H13b), C14(H14a,H14b), C15(H15a,H15b), C16(H16a,H16b), C17(H17a,H17b),
  C18(H18a,H18b), C19(H19a,H19b), C20(H20a,H20b), C21(H21a,H21b), C22(H22a,
 H22b), C22(H22c,H22d), C9(H9a,H9b), C10(H10a,H10b), C23(H23a,H23b), C24(H24a,
 H24b), C9A(H9Aa,H9Ab), C10A(H10c,H10d), C23A(H23c,H23d), C24A(H24c,H24d),
 C53(H53c,H53d), C53(H53a,H53b), C54(H54a,H54b), C55(H55a,H55b), C56(H56a,H56b),
  C54A(H54c,H54d), C55A(H55c,H55d), C56A(H56c,H56d), C49(H49a,H49b), C49(H49c,
 H49d), C50(H50a,H50b), C51(H51a,H51b), C51(H51c,H51d), C52(H52a,H52b),
 C52A(H52c,H52d)
6.b Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C27(H27a,H27b,H27c), C28(H28a,H28b,H28c), C30(H30a,H30b,
 H30c), C31(H31a,H31b,H31c), C32(H32a,H32b,H32c), C34(H34a,H34b,H34c), C35(H35a,
 H35b,H35c), C36(H36a,H36b,H36c), C38(H38a,H38b,H38c), C39(H39a,H39b,H39c),
 C40(H40a,H40b,H40c), C42(H42a,H42b,H42c), C43(H43a,H43b,H43c), C44(H44a,H44b,
 H44c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c)
;
_shelx_res_checksum              57950
_shelx_hkl_checksum              31028
_olex2_date_sample_data_collection 2021-10-29
_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 1.399
_oxdiff_exptl_absorpt_empirical_full_min 0.779