Difunctionalized indol-2-yl-ligated bimetallic rare-earth metal complexes: synthesis, characterization and high activity towards polymerization of 2-vinylpyridine
Zhao, Zhiwei; Tong, Yao; Liu, ChenCheng; Huang, Zeming; Wang, Shaowu; Wang, Fenhua; New Journal of Chemistry 48 (2024) 14690–14696; doi:10.1039/D4NJ02131B

data_7063370
_publ_section_title
;
 Difunctionalized indol-2-yl-ligated bimetallic rare-earth metal
 complexes: synthesis, characterization and high activity towards
 polymerization of 2-vinylpyridine
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14690
_journal_page_last               14696
_journal_paper_doi               10.1039/D4NJ02131B
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C48 H44 N6 S2 Si2 Yb, C7 H8'
_chemical_formula_sum            'C55 H52 N6 S2 Si2 Yb'
_chemical_formula_weight         1090.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-06-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-07-08 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.427(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0398(11)
_cell_length_b                   17.4864(11)
_cell_length_c                   20.0662(13)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    296.15(10)
_cell_measurement_theta_max      26.360
_cell_measurement_theta_min      2.329
_cell_volume                     5172.6(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15(10)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48390
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.540
_diffrn_reflns_theta_min         2.071
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.977
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0904 before and 0.0547 after correction.
The Ratio of minimum to maximum transmission is 0.7027.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear whiteish black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00049(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5897
_refine_ls_number_restraints     312
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0380P)^2^+2.0477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5201
_reflns_number_total             5897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02131b2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7063367--7063371.cif.'
_cod_database_code               7063370
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.797
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C31-C25 = C31A-C25A
 1.5 with sigma of 0.01
 C31A-C30A \\sim C31A-C26A
 with sigma of 0.02
 C31-C30 \\sim C31-C26
 with sigma of 0.02
3. Restrained planarity
 C26A, C25A, C27A, C31A, C30A, C28A, C29A
 with sigma of 0.01
 C25, C31, C26, C30, C27, C29, C28
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C26A \\sim C25A \\sim C27A \\sim C31A \\sim C30A \\sim C28A \\sim C29A \\sim
C25 \\sim C31 \\sim C26 \\sim C30 \\sim C27 \\sim C29 \\sim C28: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C25) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C28) \\sim Ueq,
Uanis(C26A) \\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C27A) \\sim Ueq,
Uanis(C31A) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C28A) \\sim Ueq,
Uanis(C29A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C25A)=Sof(C26A)=Sof(H26A)=
 Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=
 Sof(H30A)=0.5*(1-FVAR(2))
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C25)=Sof(C26)=Sof(H26)=Sof(C27)=
 Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=0.5*FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C21(H21)
6.b Me refined with riding coordinates:
 C31(H31A,H31B,H31C), C31A(H31D,H31E,H31F)
6.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C13(H13), C4(H4), C19(H19), C10(H10), C12(H12), C5(H5), C18(H18),
 C11(H11), C7(H7), C17(H17), C6(H6), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C30A(H30A)
6.d Fitted hexagon refined as free rotating group:
 C25(C26,C27,C28,C29,C30), C25A(C26A,C27A,C28A,C29A,C30A)
6.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              13635
_olex2_submission_special_instructions 'No special instructions were received'