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_7709572
_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         'C38 H94 Cl2 Fe2 N4 Si6'
_chemical_formula_sum            'C38 H94 Cl2 Fe2 N4 Si6'
_chemical_formula_weight         958.31
_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     iterative
_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                100.964(5)
_cell_angle_beta                 92.641(4)
_cell_angle_gamma                99.343(5)
_cell_formula_units_Z            1
_cell_length_a                   9.0648(5)
_cell_length_b                   12.2798(7)
_cell_length_c                   12.6473(7)
_cell_measurement_reflns_used    6177
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      29.2360
_cell_measurement_theta_min      2.7180
_cell_volume                     1359.48(14)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -42.00  49.00   0.50    4.00    --   -6.00  82.00  30.00  182
  2  \w    -30.00  81.00   0.50    4.00    --   -6.00  57.00 120.00  222
  3  \w    -82.00 -11.00   0.50    4.00    --    6.10 -37.00  30.00  142
  4  \w      8.00  83.00   0.50    4.00    --    6.10  37.00 -60.00  150
  5  \w    -21.00  80.00   0.50    4.00    --    6.10  77.00 -30.00  202
  6  \w     -5.00  62.00   0.50    4.00    --    6.10  82.00 150.00  134
;
_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      -0.0307658000
_diffrn_orient_matrix_UB_12      -0.0464500000
_diffrn_orient_matrix_UB_13      -0.0418420000
_diffrn_orient_matrix_UB_21      0.0312353000
_diffrn_orient_matrix_UB_22      -0.0366750000
_diffrn_orient_matrix_UB_23      0.0281736000
_diffrn_orient_matrix_UB_31      -0.0663790000
_diffrn_orient_matrix_UB_32      -0.0082226000
_diffrn_orient_matrix_UB_33      0.0271952000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23073
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.605
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86672
_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    1.171
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6225
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0386P)^2^+0.4508P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4710
_reflns_number_total             6225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00049k2.cif
_cod_data_source_block           exp_6987
_cod_original_cell_volume        1359.48(13)
_cod_database_code               7709572
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H N Si Fe Cl'
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.925
_reflns_odcompleteness_completeness 99.87
_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. Uiso/Uaniso restraints and constraints
N1A \\sim C11A \\sim C12A \\sim C13A: within 3A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C18 \\sim C19 \\sim C18A \\sim C19A: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C11A) \\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C13A)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N1) \\sim Ueq,
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18A) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C19)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H10A)=Sof(H10B)=Sof(N1)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=
 Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=1-FVAR(1)
 Sof(H10C)=Sof(H10D)=Sof(N1A)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=
 Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=FVAR(1)
 Sof(H17)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(H19C)=1-FVAR(2)
 Sof(H17A)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=
 Sof(H19E)=Sof(H19F)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C17(H17A)
4.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C10(H10C,H10D), C12(H12A,H12B), C13(H13A,H13B), C12A(H12C,
 H12D), C13A(H13C,H13D)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), 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), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C19(H19A,
 H19B,H19C), C11A(H11D,H11E,H11F), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F)
;
_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 1.332
_oxdiff_exptl_absorpt_empirical_full_min 0.847