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_7063368
_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 Er2 N6 S2 Si4, 0.5(C6 H14)'
_chemical_formula_sum            'C59 H75 Er2 N6 S2 Si4'
_chemical_formula_weight         1379.25
_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     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                88.6080(10)
_cell_angle_beta                 84.5980(10)
_cell_angle_gamma                69.5020(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4821(13)
_cell_length_b                   15.7715(17)
_cell_length_c                   17.7444(19)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    293.15(10)
_cell_measurement_theta_max      28.322
_cell_measurement_theta_min      2.306
_cell_volume                     3257.3(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker SMART APEX II 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      293.15(10)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.894
_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  0.0255
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28879
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.762
_diffrn_reflns_theta_min         1.153
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.735
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.3886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1187 before and 0.0435 after correction.
The Ratio of minimum to maximum transmission is 0.5211.
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    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             1390
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.231
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         15124
_refine_ls_number_restraints     509
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+1.7266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11615
_reflns_number_total             15124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02131b2.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 7063367--7063371.cif.'
_cod_database_code               7063368
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.625
_shelx_estimated_absorpt_t_min   0.597
_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. Restrained planarity
 C30, C32, C33, C29, C31, N5
 with sigma of 0.01
 C30A, C32A, C33A, C29, C31A, N5
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C62 \\sim C61 \\sim C60 \\sim C59 \\sim C58 \\sim C57 \\sim C60A \\sim C62A
\\sim C61A \\sim C59A \\sim C58A \\sim C57A: 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
C29 \\sim N5 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C30A \\sim C31A
\\sim C32A \\sim C33A: 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
Uanis(C57A) \\sim Ueq, Uanis(C58A) \\sim Ueq, Uanis(C59A) \\sim Ueq,
Uanis(C60A) \\sim Ueq, Uanis(C61A) \\sim Ueq, Uanis(C62A) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq,
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Same fragment restrains
{C29, N5, C30A, C31A, C32A, C33A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C29, N5, C30, C31, C32, C33}
{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}
{C57A, C58A, C59A, C60A, C61A, C62A} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C57, C58, C59, C60, C61, C62}
6. Others
 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(1)
 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(1)
 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(2)
 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(2)
 Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=
 Sof(H33A)=1-FVAR(3)
 Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=FVAR(3)
 Sof(C57A)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58A)=Sof(H58A)=Sof(H58B)=
 Sof(C59A)=Sof(H59A)=Sof(H59B)=Sof(C60A)=Sof(H60A)=Sof(H60B)=Sof(C61A)=
 Sof(H61A)=Sof(H61B)=Sof(C62A)=Sof(H62A)=Sof(H62B)=Sof(H62C)=0.5*(1-FVAR(5))
 Sof(C57)=Sof(H57D)=Sof(H57E)=Sof(H57F)=Sof(C58)=Sof(H58C)=Sof(H58D)=Sof(C59)=
 Sof(H59C)=Sof(H59D)=Sof(C60)=Sof(H60C)=Sof(H60D)=Sof(C61)=Sof(H61C)=Sof(H61D)=
 Sof(C62)=Sof(H62D)=Sof(H62E)=Sof(H62F)=0.5*FVAR(5)
7.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C45(H45A,H45B), C49(H49A,H49B), C53(H53A,H53B), C58A(H58A,
 H58B), C59A(H59A,H59B), C60A(H60A,H60B), C61A(H61A,H61B), C58(H58C,H58D),
 C59(H59C,H59D), C60(H60C,H60D), C61(H61C,H61D)
7.b Me refined with riding coordinates:
 C57A(H57A,H57B,H57C), C62A(H62A,H62B,H62C), C57(H57D,H57E,H57F), C62(H62D,
 H62E,H62F)
7.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), C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A)
7.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C),
 C56(H56A,H56B,H56C), C50A(H50D,H50E,H50F), C51A(H51D,H51E,H51F), C52A(H52D,
 H52E,H52F), C54A(H54D,H54E,H54F), C55A(H55D,H55E,H55F), C56A(H56D,H56E,H56F)
;
_shelx_res_checksum              95095
_olex2_submission_special_instructions 'No special instructions were received'