Rare-earth metal complexes bearing electrophilic and nucleophilic carbon centres and their unique reactivity patterns towards pyridine derivatives.
Wu, Weikang; Rajeshkumar, Thayalan; Zhu, Shan; Chai, Fuxiang; Hong, Dongjing; Huang, Zeming; Yuan, Qingbing; Maron, Laurent; Wang, Shaowu; Chemical science 15 (2024) 20315–20327; doi:10.1039/d4sc04197f

data_1573118
_publ_section_title
;
 Rare-earth metal complexes bearing electrophilic and nucleophilic carbon
 centres and their unique reactivity patterns towards pyridine
 derivatives.
;
_journal_issue                   48
_journal_name_full               'Chemical science'
_journal_page_first              20315
_journal_page_last               20327
_journal_paper_doi               10.1039/d4sc04197f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C62 H76 Er N8, 1[C7H8]'
_chemical_formula_sum            'C69 H84 Er N8'
_chemical_formula_weight         1192.70
_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     iterative
_audit_creation_date             2024-04-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-29 deposited with the CCDC.	2024-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                75.276(6)
_cell_angle_beta                 84.282(6)
_cell_angle_gamma                74.311(6)
_cell_formula_units_Z            2
_cell_length_a                   14.584(9)
_cell_length_b                   14.899(9)
_cell_length_c                   15.053(9)
_cell_measurement_reflns_used    2045
_cell_measurement_temperature    300
_cell_measurement_theta_max      24.05
_cell_measurement_theta_min      2.25
_cell_volume                     3044(3)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.4064
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11005
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.433
_diffrn_reflns_theta_min         1.399
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.426
_exptl_absorpt_correction_T_max  0.745163
_exptl_absorpt_correction_T_min  0.359662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0988 before and 0.0595 after correction.
 
For component 2:
 wR2(int) was 0.1002 before and 0.0615 after correction.
 The Ratio of minimum to maximum transmission is 0.50.

Final HKLF 4 output contains 27470 reflections, Rint = 0.1330
 (11701 with I > 3sig(I), Rint = 0.0802)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.186
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         11005
_refine_ls_number_restraints     493
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.2280
_refine_ls_R_factor_gt           0.1202
_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^)+(0.1325P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2386
_refine_ls_wR_factor_ref         0.2746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4864
_reflns_number_total             11005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04197f4.cif
_cod_data_source_block           13
_cod_depositor_comments
'Adding full bibliography for 1573095--1573138.cif.'
_cod_database_code               1573118
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.815
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C23-C26
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(C23) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
4.a Ternary CH refined with riding coordinates:
 C19(H19), C21(H21), C26(H26), C45(H45), C47(H47), C52(H52)
4.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C18(H18A,H18B), C20(H20A,H20B), C22(H22A,H22B),
  C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
 C41(H41A,H41B), C44(H44A,H44B), C46(H46A,H46B), C48(H48A,H48B), C49(H49A,H49B),
  C50(H50A,H50B), C51(H51A,H51B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C16(H16), C30(H30), C31(H31), C32(H32),
 C33(H33), C42(H42), C53(H53), C54(H54), C55(H55), C56(H56), C59(H59), C60(H60),
  C61(H61), C62(H62)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 102 electrons were 
found in a volume of 604\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C7H8] per Unit Cell 
which account for 100 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91569
_shelx_hkl_checksum              74452
_shelx_fab_checksum              37283
_olex2_submission_special_instructions 'No special instructions were received'