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_7063367
_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 N6 S2 Si4 Y2, 0.5(C6 H14)'
_chemical_formula_sum            'C59 H75 N6 S2 Si4 Y2'
_chemical_formula_weight         1222.55
_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
_audit_creation_date             2024-06-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-07-08 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                88.681(2)
_cell_angle_beta                 84.851(2)
_cell_angle_gamma                69.397(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4938(14)
_cell_length_b                   15.7972(18)
_cell_length_c                   17.7519(19)
_cell_measurement_reflns_used    4325
_cell_measurement_temperature    296.15(10)
_cell_measurement_theta_max      17.797
_cell_measurement_theta_min      2.578
_cell_volume                     3266.2(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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1632
_diffrn_reflns_av_unetI/netI     0.0892
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            58200
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        20.956
_diffrn_reflns_theta_max         20.956
_diffrn_reflns_theta_min         2.216
_exptl_absorpt_coefficient_mu    1.944
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0860 before and 0.0722 after correction.
The Ratio of minimum to maximum transmission is 0.7571.
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    1.243
_exptl_crystal_description       block
_exptl_crystal_F_000             1274
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         6941
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0214P)^2^+4.8026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4376
_reflns_number_total             6941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02131b2.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 7063367--7063371.cif.'
_cod_database_code               7063367
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.786
_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
 C58-C57 = C59-C58 = C60-C59 = C61-C60 = C62-C61
 1.54 with sigma of 0.01
 C57-C59 = C58-C60 = C59-C61 = C60-C62
 2.515 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si1 \\sim C42 \\sim C43 \\sim C44 \\sim C42A \\sim C43A \\sim C44A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Si4 \\sim C54 \\sim C55 \\sim C56 \\sim C54A \\sim C55A \\sim C56A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C60 \\sim C57 \\sim C58 \\sim C59 \\sim C61 \\sim C62: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Si3 \\sim C50 \\sim C51 \\sim C52 \\sim C50A \\sim C51A \\sim C52A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Same fragment restrains
{Si1, C42A, C43A, C44A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{Si1, C42, C43, C44}
{Si3, C50A, C51A, C52A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{Si3, C50, C51, C52}
{Si4, C54A, C55A, C56A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{Si4, C54, C55, C56}
5. Others
 Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=Sof(C43A)=Sof(H43D)=Sof(H43E)=
 Sof(H43F)=Sof(C44A)=Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(1)
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(1)
 Sof(C50A)=Sof(H50D)=Sof(H50E)=Sof(H50F)=Sof(C51A)=Sof(H51D)=Sof(H51E)=
 Sof(H51F)=Sof(C52A)=Sof(H52D)=Sof(H52E)=Sof(H52F)=1-FVAR(2)
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(2)
 Sof(C54A)=Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(C55A)=Sof(H55D)=Sof(H55E)=
 Sof(H55F)=Sof(C56A)=Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(3)
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(3)
 Fixed Sof: C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C58(0.5) H58A(0.5)
 H58B(0.5) C59(0.5) H59A(0.5) H59B(0.5) C60(0.5) H60A(0.5) H60B(0.5) C61(0.5)
 H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C45(H45A,H45B), C49(H49A,H49B), C53(H53A,H53B), C58(H58A,
 H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B)
6.b Me refined with riding coordinates:
 C57(H57A,H57B,H57C)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27),
  C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39), C40(H40)
6.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C),
 C56(H56A,H56B,H56C), C42A(H42D,H42E,H42F), C43A(H43D,H43E,H43F), C44A(H44D,
 H44E,H44F), C50A(H50D,H50E,H50F), C51A(H51D,H51E,H51F), C52A(H52D,H52E,H52F),
 C54A(H54D,H54E,H54F), C55A(H55D,H55E,H55F), C56A(H56D,H56E,H56F), C62(H62A,
 H62B,H62C)
;
_shelx_res_checksum              86744
_olex2_submission_special_instructions 'No special instructions were received'