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_7063369
_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         'C56 H68 Lu2 N6 S2 Si4, 2(C6.42 H6.261 Cl0.58)'
_chemical_formula_sum            'C68.84 H80.53 Cl1.16 Lu2 N6 S2 Si4'
_chemical_formula_weight         1559.48
_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             2024-06-11
_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                 100.885(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6276(18)
_cell_length_b                   19.470(2)
_cell_length_c                   25.369(2)
_cell_measurement_reflns_used    5149
_cell_measurement_temperature    296.15(10)
_cell_measurement_theta_max      24.643
_cell_measurement_theta_min      2.836
_cell_volume                     7095.1(13)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 0.977
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture 296K'
_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  0.0855
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24878
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         2.655
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.979
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0969 before and 0.0668 after correction.
The Ratio of minimum to maximum transmission is 0.7083.
The \l/2 correction factor is Not present.
;
_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    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             3141
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.394
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7838
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0405P)^2^+48.6791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1437
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4758
_reflns_number_total             7838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02131b2.cif
_cod_data_source_block           3d
_cod_depositor_comments
'Adding full bibliography for 7063367--7063371.cif.'
_cod_original_cell_volume        7095.3(14)
_cod_database_code               7063369
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.601
_shelx_estimated_absorpt_t_min   0.573
_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
 Cl1-C29
 1.73 with sigma of 0.01
 C35-C29
 1.5 with sigma of 0.01
 Cl1-C30 \\sim Cl1-C34
 with sigma of 0.02
3. Restrained planarity
 Cl1, C29, C30, C31, C32, C33, C34
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C29 \\sim Cl1 \\sim C30 \\sim C34 \\sim C31 \\sim C33 \\sim C32 \\sim C35:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Si1 \\sim C22 \\sim C23 \\sim C24 \\sim C22A \\sim C23A \\sim C24A \\sim Si2
\\sim C26 \\sim C27 \\sim C28 \\sim C26A \\sim C27A \\sim C28A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Same fragment restrains
{Si1, C22A, C23A, C24A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{Si1, C22, C23, C24}
{Si2, C26A, C27A, C28A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{Si2, C26, C27, C28}
6. Others
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
 Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=1-FVAR(3)
 Sof(Cl1)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C25(H25A,H25B)
7.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18), C19(H19), C20(H20), C32(H32), C31(H31), C30(H30), C34(H34),
  C33(H33)
7.c Fitted hexagon refined as free rotating group:
 C6(C5,C4,C3,C8,C7), C15(C16,C17,C18,C19,C20), C32(C31,C30,C29,C34,C33)
7.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C22A(H22D,H22E,H22F),
 C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F), C26A(H26D,H26E,H26F), C27A(H27D,
 H27E,H27F), C28A(H28D,H28E,H28F), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              85899
_olex2_submission_special_instructions 'No special instructions were received'