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_7709569
_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         '2(C31 H58 Li2 N2 O Si3)'
_chemical_formula_sum            'C62 H116 Li4 N4 O2 Si6'
_chemical_formula_weight         1145.88
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             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                77.906(2)
_cell_angle_beta                 84.578(2)
_cell_angle_gamma                75.704(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0442(3)
_cell_length_b                   16.4938(4)
_cell_length_c                   22.9493(5)
_cell_measurement_reflns_used    22978
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.3090
_cell_measurement_theta_min      2.4380
_cell_volume                     3598.77(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    -50.00 -24.00   0.50    4.03    --  -12.90 -57.00 -30.00   52
  2  \w    -10.00 102.00   0.50    4.03    --   12.90  77.00  30.00  224
  3  \w     28.00  73.00   0.50    4.03    --   12.90  57.00  90.00   90
  4  \w    -13.00  80.00   0.50    4.03    --   12.90  57.00-180.00  186
  5  \w     -6.00 102.00   0.50    4.03    --   12.90  57.00   0.00  216
  6  \w    -26.00  76.00   0.50    4.03    --   12.90  77.00-150.00  204
  7  \w    -14.00  97.00   0.50    4.03    --   12.90  57.00 -60.00  222
  8  \w    -28.00  -3.00   0.50    4.03    --   12.90 -19.00  90.00   50
  9  \w    -64.00 -38.00   0.50    4.03    --   12.90 -19.00  90.00   52
;
_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      -0.0043155000
_diffrn_orient_matrix_UB_12      -0.0237001000
_diffrn_orient_matrix_UB_13      0.0294319000
_diffrn_orient_matrix_UB_21      0.0449674000
_diffrn_orient_matrix_UB_22      0.0214032000
_diffrn_orient_matrix_UB_23      0.0093267000
_diffrn_orient_matrix_UB_31      -0.0572790000
_diffrn_orient_matrix_UB_32      0.0320283000
_diffrn_orient_matrix_UB_33      0.0069232000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0247
_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       -9
_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            51412
_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         26.022
_diffrn_reflns_theta_min         2.192
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.057
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         14186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0857P)^2^+1.2534P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11168
_reflns_number_total             14186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00049k2.cif
_cod_data_source_block           exp_6157
_cod_database_code               7709569
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H Si N Li O'
_chemical_oxdiff_usercomment     'FHM201214, 58Fe42Cugua'
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.970
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. 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
2. Others
 Sof(H59C)=Sof(H59D)=Sof(H61C)=Sof(H61D)=Sof(C60A)=Sof(H60C)=Sof(H60D)=1-FVAR(1)
 Sof(H59A)=Sof(H59B)=Sof(H61A)=Sof(H61B)=Sof(C60)=Sof(H60A)=Sof(H60B)=FVAR(1)
 Sof(H29C)=Sof(H29D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=1-FVAR(2)
 Sof(H29A)=Sof(H29B)=Sof(C28)=Sof(H28A)=Sof(H28B)=FVAR(2)
 Sof(H25A)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27D)=
 Sof(H27E)=Sof(H27F)=1-FVAR(3)
 Sof(H25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=FVAR(3)
 Sof(Si1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=
 Sof(H2AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(4)
 Sof(Si1)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(4)
 Sof(Si4A)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33A)=Sof(H33D)=
 Sof(H33E)=Sof(H33F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(5)
 Sof(Si4)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=
 Sof(H33C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(5)
3.a Ternary CH refined with riding coordinates:
 C13(H13), C22(H22), C25(H25A), C25(H25), C44(H44), C53(H53), C56(H56)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C29(H29A,H29B), C29(H29C,H29D), C30(H30A,H30B), C31(H31A,
 H31B), C28(H28A,H28B), C28A(H28C,H28D), C41(H41A,H41B), C59(H59A,H59B),
 C59(H59C,H59D), C61(H61A,H61B), C61(H61C,H61D), C62(H62A,H62B), C60(H60A,H60B),
  C60A(H60C,H60D)
3.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20), C49(H49), C50(H50), C51(H51)
3.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,
 H2AC), C3A(H3AA,H3AB,H3AC), C26A(H26D,H26E,H26F), C27A(H27D,H27E,H27F),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C54(H54A,
 H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C32A(H32D,H32E,
 H32F), C33A(H33D,H33E,H33F), C34A(H34D,H34E,H34F)
;
_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 1.365
_oxdiff_exptl_absorpt_empirical_full_min 0.650