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_7063371
_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 Yb2, 0.5(C6 H14)'
_chemical_formula_sum            'C59 H75 N6 S2 Si4 Yb2'
_chemical_formula_weight         1390.81
_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                88.403(2)
_cell_angle_beta                 84.3420(10)
_cell_angle_gamma                69.7400(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4889(5)
_cell_length_b                   15.7434(7)
_cell_length_c                   17.6727(6)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    296.15(10)
_cell_measurement_theta_max      27.474
_cell_measurement_theta_min      2.688
_cell_volume                     3243.8(2)
_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 1.3 (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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15(10)
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_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  0.0491
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            84224
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.554
_diffrn_reflns_theta_min         2.572
_exptl_absorpt_coefficient_mu    3.043
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0957 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.7096.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             1398
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         3.088
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.100
_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     761
_refine_ls_number_reflns         14907
_refine_ls_number_restraints     364
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0296P)^2^+8.1396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10729
_reflns_number_total             14907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02131b2.cif
_cod_data_source_block           3c
_cod_depositor_comments
'Adding full bibliography for 7063367--7063371.cif.'
_cod_database_code               7063371
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.596
_shelx_estimated_absorpt_t_min   0.567
_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
 Si3-C49 \\sim Si3-C52 \\sim Si3-C50 \\sim Si3-C51 \\sim Si4-C56 \\sim Si4-C54
\\sim Si4-C55 \\sim Si4-C53
 with sigma of 0.02
 Si4-C53 \\sim Si4-C54A \\sim Si4-C56A \\sim Si4-C55A \\sim Si3-C50A \\sim
Si3-C51A \\sim Si3-C52A ~
 Si3-C49
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si3 \\sim C51 \\sim C52 \\sim C50 \\sim C51A \\sim C52A \\sim C50A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Si4 \\sim C56 \\sim C55 \\sim C54 \\sim C56A \\sim C55A \\sim C54A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C59 \\sim C58 \\sim C60 \\sim C57 \\sim C61 \\sim C62: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C56) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C50A) \\sim Ueq, Uanis(C52A) \\sim Ueq, Uanis(Si3) \\sim Ueq, Uanis(C51A)
\\sim Ueq, Uanis(C56A) \\sim Ueq, Uanis(C54A) \\sim Ueq, Uanis(Si4) \\sim Ueq,
Uanis(C55A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Si3) \\sim Ueq, Uanis(Si4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(C51A)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C52A)=Sof(H52D)=Sof(H52E)=
 Sof(H52F)=Sof(C50A)=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(1)
 Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(1)
 Sof(C56A)=Sof(H56D)=Sof(H56E)=Sof(H56F)=Sof(C55A)=Sof(H55D)=Sof(H55E)=
 Sof(H55F)=Sof(C54A)=Sof(H54D)=Sof(H54E)=Sof(H54F)=1-FVAR(2)
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(2)
 Fixed Sof: C59(0.5) H59A(0.5) H59B(0.5) C57(0.5) H57A(0.5) H57B(0.5)
 H57C(0.5) C58(0.5) H58A(0.5) H58B(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)
5.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C49(H49A,H49B), C41(H41A,H41B), C53(H53A,H53B), C59(H59A,
 H59B), C58(H58A,H58B), C60(H60A,H60B), C61(H61A,H61B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C19(H19), C39(H39), C33(H33), C4(H4), C30(H30), C13(H13), C31(H31),
 C38(H38), C18(H18), C7(H7), C27(H27), C16(H16), C5(H5), C24(H24), C11(H11),
 C6(H6), C36(H36), C37(H37), C12(H12), C17(H17), C32(H32), C26(H26), C25(H25)
5.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C43(H43A,H43B,
 H43C), C56(H56A,H56B,H56C), C44(H44A,H44B,H44C), C42(H42A,H42B,H42C), C51(H51A,
 H51B,H51C), C55(H55A,H55B,H55C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C),
 C50(H50A,H50B,H50C), C51A(H51D,H51E,H51F), C52A(H52D,H52E,H52F), C50A(H50D,
 H50E,H50F), C56A(H56D,H56E,H56F), C55A(H55D,H55E,H55F), C54A(H54D,H54E,H54F),
 C57(H57A,H57B,H57C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              66793
_olex2_submission_special_instructions 'No special instructions were received'