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_1571051
_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         'C45 H78 Cs N Si2'
_chemical_formula_sum            'C45 H78 Cs N Si2'
_chemical_formula_weight         822.17
_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                 113.967(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2860(4)
_cell_length_b                   14.13261(17)
_cell_length_c                   17.3397(3)
_cell_measurement_reflns_used    39712
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.1880
_cell_measurement_theta_min      2.5060
_cell_volume                     4542.57(15)
_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      100.01(10)
_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 0.917
_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    -15.00  30.00   1.00   12.00    --  -14.29 -99.00  90.00   45
  2  \w    -79.00 -33.00   1.00   12.00    --  -14.29 133.00 176.00   46
  3  \w   -105.00 -58.00   1.00   12.00    --  -14.29 178.00 -60.00   47
  4  \w    -77.00 107.00   1.00   12.00    --   15.15   0.00 -90.00  184
  5  \w   -107.00 -61.00   1.00   12.00    --  -14.29-178.00  90.00   46
  6  \w    -15.00  30.00   1.00   12.00    --  -14.29 -99.00-150.00   45
  7  \w    -42.00  22.00   1.00   12.00    --  -14.29 -77.00  30.00   64
  8  \w    -50.00  21.00   1.00   12.00    --  -14.29  77.00 120.00   71
  9  \w    -50.00  10.00   1.00   12.00    --  -14.29  77.00 -90.00   60
 10  \w    -43.00 100.00   1.00   12.00    --   15.15  19.00  60.00  143
;
_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      0.0300782000
_diffrn_orient_matrix_UB_12      0.0162402000
_diffrn_orient_matrix_UB_13      0.0358266000
_diffrn_orient_matrix_UB_21      -0.0236456000
_diffrn_orient_matrix_UB_22      0.0188384000
_diffrn_orient_matrix_UB_23      0.0170336000
_diffrn_orient_matrix_UB_31      0.0010052000
_diffrn_orient_matrix_UB_32      -0.0435960000
_diffrn_orient_matrix_UB_33      0.0207114000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            79133
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.528
_diffrn_reflns_theta_min         2.197
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.333
_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    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.552
_exptl_crystal_size_mid          0.365
_exptl_crystal_size_min          0.334
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.063
_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     463
_refine_ls_number_reflns         11623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0234P)^2^+2.4761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10143
_reflns_number_total             11623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06896j2.cif
_cod_data_source_block           hasj201211b
_cod_depositor_comments
'Adding full bibliography for 1571041--1571052.cif.'
_cod_database_code               1571051
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C45 H78 Cs1 N1 Si2'
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.637
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34),
 C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44)
2.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), C31(H31a,H31b,H31c), C38(H38a,
 H38b,H38c), C45(H45a,H45b,H45c)
;
_shelx_res_checksum              92418
_shelx_hkl_checksum              80322
_olex2_date_sample_data_collection 2020-12-11
_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 1.145
_oxdiff_exptl_absorpt_empirical_full_min 0.850