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_7709568
_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         'C68 H136 Cl2 Mn4 N8 Si12, 2(C6 H14)'
_chemical_formula_sum            'C80 H164 Cl2 Mn4 N8 Si12'
_chemical_formula_weight         1865.92
_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_block_doi                 10.5517/ccdc.csd.cc2b5c63
_audit_creation_date             2022-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-04 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                107.997(5)
_cell_angle_beta                 105.323(5)
_cell_angle_gamma                101.251(5)
_cell_formula_units_Z            1
_cell_length_a                   10.4374(6)
_cell_length_b                   15.6526(8)
_cell_length_c                   18.7151(10)
_cell_measurement_reflns_used    11385
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.0220
_cell_measurement_theta_min      2.8180
_cell_volume                     2673.9(3)
_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      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    -89.00  -5.00   0.50    7.00    --   -1.70 -37.00 -30.00  168
  2  \w     45.00  87.00   0.50    7.00    --   -1.70  37.00-150.00   84
  3  \w     10.00  48.00   0.50    7.00    --   -1.70  77.00 -90.00   76
  4  \w     -9.00  17.00   0.50    7.00    --   -1.70  37.00-150.00   52
  5  \w     -9.00  17.00   0.50    7.00    --    1.90 -57.00  90.00   52
  6  \w     45.00  91.00   0.50    7.00    --    1.90  19.00 -30.00   92
  7  \w    -88.00 -39.00   0.50    7.00    --    1.90 -57.00  90.00   98
  8  \w    -52.00  16.00   0.50    7.00    --    1.90 -57.00-120.00  136
  9  \w    -12.00  22.00   0.50    7.00    --    1.90  57.00-120.00   68
 10  \w    -87.00   0.50   0.50    7.00    --    1.90 -57.00 120.00  175
;
_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      -0.0342524000
_diffrn_orient_matrix_UB_12      -0.0403363000
_diffrn_orient_matrix_UB_13      -0.0360680000
_diffrn_orient_matrix_UB_21      0.0005330000
_diffrn_orient_matrix_UB_22      -0.0292536000
_diffrn_orient_matrix_UB_23      0.0223659000
_diffrn_orient_matrix_UB_31      -0.0654883000
_diffrn_orient_matrix_UB_32      0.0038419000
_diffrn_orient_matrix_UB_33      0.0023572000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51851
_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         2.312
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63121
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       block
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.596
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         12256
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0719
_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^)+(0.1063P)^2^+4.5886P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1917
_refine_ls_wR_factor_ref         0.2100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9144
_reflns_number_total             12256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00049k2.cif
_cod_data_source_block           exp_6681
_cod_database_code               7709568
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H N Mn Cl Si'
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.935
_reflns_odcompleteness_completeness 99.78
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C39-C40 = C39-C38 = C38A-C39A = C38A-C37A = C38-C37 = C36A-C37A = C37-C36 =
 C35-C36
 1.54 with sigma of 0.01
 C36A-C35 = C40-C39A
 1.54 with sigma of 0.001
 C35-C37A
 2.5 with sigma of 0.02
 C36A-C38A
 2.5 with sigma of 0.02
 C37A-C39A
 2.5 with sigma of 0.02
 C38A-C40
 2.5 with sigma of 0.02
 C36-C38
 2.5 with sigma of 0.02
 C38-C40
 2.5 with sigma of 0.02
 C37-C39
 2.5 with sigma of 0.02
 C37-C35
 2.5 with sigma of 0.02
3. Rigid bond restraints
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C35, C40, C36A, C37A, C38A, C39A, C36, C37, C38, C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl1A: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C40) \\sim Ueq, Uanis(C39A) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38A)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C37A) \\sim Ueq,
Uanis(C36A) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37A) \\sim Ueq, Uanis(C39A) \\sim Ueq, Uanis(C36A) \\sim Ueq,
Uanis(C38A) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C40) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5. Others
 Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C36)=
 Sof(H36C)=Sof(H36D)=Sof(C37)=Sof(H37C)=Sof(H37D)=Sof(C38)=Sof(H38C)=Sof(H38D)=
 Sof(C39)=Sof(H39C)=Sof(H39D)=1-FVAR(1)
 Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C36A)=
 Sof(H36A)=Sof(H36B)=Sof(C37A)=Sof(H37B)=Sof(H37A)=Sof(C38A)=Sof(H38A)=
 Sof(H38B)=Sof(C39A)=Sof(H39A)=Sof(H39B)=FVAR(1)
 Sof(Cl1A)=1-FVAR(2)
 Sof(Cl1)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12B,H12A), C23(H23A,H23B), C25(H25A,H25B), C36A(H36A,
 H36B), C37A(H37B,H37A), C38A(H38A,H38B), C39A(H39A,H39B), C36(H36C,H36D),
 C37(H37C,H37D), C38(H38C,H38D), C39(H39C,H39D)
6.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21)
6.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(H7B,H7A,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,
 H11C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C35(H35D,H35E,
 H35F), C40(H40A,H40B,H40C), C40(H40D,H40E,H40F)
;
_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 1.469
_oxdiff_exptl_absorpt_empirical_full_min 0.775