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_7709570
_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 Mn2 N4 Si6'
_chemical_formula_sum            'C38 H94 Cl2 Mn2 N4 Si6'
_chemical_formula_weight         956.49
_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                101.770(4)
_cell_angle_beta                 92.549(4)
_cell_angle_gamma                99.528(3)
_cell_formula_units_Z            1
_cell_length_a                   9.1109(4)
_cell_length_b                   12.3473(5)
_cell_length_c                   12.7686(6)
_cell_measurement_reflns_used    9613
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.1830
_cell_measurement_theta_min      2.6990
_cell_volume                     1382.24(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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      180.00(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    -90.00 -65.00   0.50    2.88    --   -1.70 -37.00   0.00   50
  2  \w    -88.00 -17.00   0.50    2.88    --   -1.70 -57.00-150.00  142
  3  \w      3.00  62.00   0.50    2.88    --    1.90  57.00 150.00  118
  4  \w    -19.00  45.00   0.50    2.88    --    1.90  57.00 -30.00  128
  5  \w    -87.00 -17.00   0.50    2.88    --    1.90 -82.00 -60.00  140
  6  \w     -2.00  34.00   0.50    2.88    --    1.90 -82.00 -60.00   72
  7  \w    -27.00   4.00   0.50    2.88    --    1.90 -37.00 -90.00   62
  8  \w     -7.00  25.00   0.50    2.88    --    1.90 -19.00   0.00   64
  9  \w    -21.00  71.00   0.50    2.88    --    1.90  57.00  60.00  184
;
_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      0.0504558000
_diffrn_orient_matrix_UB_12      0.0485772000
_diffrn_orient_matrix_UB_13      -0.0051884000
_diffrn_orient_matrix_UB_21      0.0378362000
_diffrn_orient_matrix_UB_22      0.0012866000
_diffrn_orient_matrix_UB_23      0.0501234000
_diffrn_orient_matrix_UB_31      0.0479116000
_diffrn_orient_matrix_UB_32      -0.0345724000
_diffrn_orient_matrix_UB_33      -0.0264919000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0244
_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       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25253
_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         27.482
_diffrn_reflns_theta_min         2.591
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
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    1.149
_exptl_crystal_description       block
_exptl_crystal_F_000             518
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.397
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         6323
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+1.2197P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1504
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5262
_reflns_number_total             6323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00049k2.cif
_cod_data_source_block           exp_6945
_cod_database_code               7709570
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H N Si Mn Cl'
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.932
_reflns_odcompleteness_completeness 99.86
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C19A-C17A = C19-C17 = C18A-C17A = C18-C17
 1.54 with sigma of 0.02
 N1A-C10A \\sim N1-C10
 with sigma of 0.01
 N2-C17 \\sim N2-C17A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C17 \\sim C18 \\sim C19 \\sim C17A \\sim C18A \\sim C19A: within 3A with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(N1)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C17A)=Sof(H17A)=
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=1-FVAR(1)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(N1A)=Sof(C11A)=Sof(H11D)=
 Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=
 Sof(H13D)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C17A(H17A)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C10A(H10C,H10D), C12A(H12C,
 H12D), C13A(H13C,H13D)
5.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 0.776