Trisyl-based multidentate ligands: synthesis and their transition-metal complexes
Yin, Zhu-Bao; Wei, Junnian; Xi, Zhenfeng; Dalton Transactions  (2022) –; doi:10.1039/D2DT00049K

data_7709577
_publ_section_title
;
 Trisyl-based multidentate ligands: synthesis and their transition-metal
 complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00049K
_journal_year                    2022
_chemical_formula_moiety         'C20 H52 Li S Si6, C12 H32 Li N4'
_chemical_formula_sum            'C32 H84 Li2 N4 S Si6'
_chemical_formula_weight         739.51
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2021-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-02 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.695(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4284(2)
_cell_length_b                   17.4514(4)
_cell_length_c                   29.3718(6)
_cell_measurement_reflns_used    27888
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      28.5220
_cell_measurement_theta_min      2.3030
_cell_volume                     4827.45(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -94.00  -4.00   0.50    2.00    --   -5.80 -37.00-120.00  180
  2  \w    -31.00  -5.00   0.50    2.00    --   -5.80 -57.00-120.00   52
  3  \w     20.00  46.00   0.50    2.00    --   -5.80  66.00  95.34   52
  4  \w    -37.00  14.00   0.50    2.00    --   -5.80 -57.00  30.00  102
  5  \w    -95.00   1.00   0.50    2.00    --   -5.80 -57.00 150.00  192
  6  \w    -18.00   8.00   0.50    2.00    --   -5.80  37.00 120.00   52
  7  \w    -83.00  35.00   0.50    2.00    --    6.10 -37.00-180.00  236
  8  \w    -77.00   1.00   0.50    2.00    --    6.10 -19.00-120.00  156
  9  \w     38.00  63.00   0.50    2.00    --    6.10  57.00 120.00   50
 10  \w    -28.00  74.00   0.50    2.00    --    6.10  77.00   0.00  204
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0175327000
_diffrn_orient_matrix_UB_12      0.0353241000
_diffrn_orient_matrix_UB_13      0.0107877000
_diffrn_orient_matrix_UB_21      -0.0598128000
_diffrn_orient_matrix_UB_22      0.0174119000
_diffrn_orient_matrix_UB_23      -0.0113008000
_diffrn_orient_matrix_UB_31      -0.0422821000
_diffrn_orient_matrix_UB_32      -0.0099959000
_diffrn_orient_matrix_UB_33      0.0184572000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            99372
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.302
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         11070
_refine_ls_number_restraints     482
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+1.6742P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9497
_reflns_number_total             11070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00049k2.cif
_cod_data_source_block           exp_6212
_cod_database_code               7709577
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H S N Si Li'
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.976
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C23A-C24A = C24-C23
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N3 \\sim N4 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim
Li2 \\sim N1 \\sim C22 \\sim C23 \\sim C24 \\sim N2A \\sim C21A \\sim C23A
\\sim C24A \\sim C25A \\sim C26A: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(Li2) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C21A) \\sim Ueq,
Uanis(C26A) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C24A)
\\sim Ueq, Uanis(C23A) \\sim Ueq: with sigma of 0.1 and sigma for terminal
atoms of 0.2
4. Others
 Sof(S1A)=Sof(Si4A)=Sof(Si6A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C10A)=
 Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C18A)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(Li1A)=1-FVAR(1)
 Sof(S1)=Sof(Si4)=Sof(Si6)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 Sof(H20C)=Sof(Li1)=FVAR(1)
 Sof(N1A)=Sof(N2A)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22A)=Sof(H22D)=
 Sof(H22E)=Sof(H22F)=Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24C)=
 Sof(H24D)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=1-FVAR(2)
 Sof(N1)=Sof(N2)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C10A(H10C,H10D), C11A(H11C,H11D), C29(H29A,
 H29B), C30(H30A,H30B), C23(H23A,H23B), C24(H24A,H24B), C23A(H23C,H23D),
 C24A(H24C,H24D)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C1(H1A,H1B,H1C), C12(H12A,H12B,H12C), C13(H13A,
 H13B,H13C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C1A(H1AA,H1AB,H1AC), C12A(H12D,H12E,H12F), C13A(H13D,H13E,H13F), C18A(H18D,
 H18E,H18F), C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F), C27(H27A,H27B,H27C),
 C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C21A(H21D,H21E,H21F), C22A(H22D,H22E,H22F), C25A(H25D,H25E,H25F), C26A(H26D,
 H26E,H26F)
;
_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 1.181
_oxdiff_exptl_absorpt_empirical_full_min 0.796