Synthesis and characterization of rare earth/lithium complexes stabilized by ethylenediamine-bridged bis(phenolate) ligands and their activity in catalyzing amidation reactions
Ismaeel, Nadia; Zhuo, Zhixing; Imran, Sajid; Yuan, Dan; Yao, Yingming; Dalton Transactions  (2022) –; doi:10.1039/D2DT02642B

data_7711037
_publ_section_title
;
 Synthesis and characterization of rare earth/lithium complexes stabilized
 by ethylenediamine-bridged bis(phenolate) ligands and their activity in
 catalyzing amidation reactions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02642B
_journal_year                    2022
_chemical_formula_moiety         '2(C40 H78 Li N4 O2 Si4 Yb), C7 H8'
_chemical_formula_sum            'C87 H164 Li2 N8 O4 Si8 Yb2'
_chemical_formula_weight         1970.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2018-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2021-12-14 deposited with the CCDC.	2022-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.109
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8829
_cell_length_b                   15.8417
_cell_length_c                   23.6738
_cell_measurement_reflns_used    9513
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.30
_cell_measurement_theta_min      2.58
_cell_volume                     5090.705
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      119.98
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            79324
_diffrn_reflns_theta_full        26.3711
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    1.967
_exptl_absorpt_correction_T_max  0.5067
_exptl_absorpt_correction_T_min  0.3848
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.2857
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2064.9867
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.8057
_refine_diff_density_min         -0.7923
_refine_diff_density_rms         0.2145
_refine_ls_d_res_high            0.8000
_refine_ls_d_res_low             11.5735
_refine_ls_goodness_of_fit_ref   1.2333
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    124
_refine_ls_number_parameters     507
_refine_ls_number_reflns         10400
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.2331
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.2055
_refine_ls_shift/su_mean         0.0029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+2.5059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                9199
_reflns_number_total             10400
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt02642b2.cif
_cod_data_source_block           mo_b171008c_0m
_cod_original_cell_volume        5090.70477
_cod_database_code               7711037
_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
 C42-C43
 1.5 with sigma of 0.02
 C42-C44 \\sim C42-C48
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C42) = Uanis(C43) = Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47) =
Uanis(C48)
4. Others
 Fixed Sof: C42(0.5) H42a(0.5) H42b(0.5) H42c(0.5) C43(0.5) C44(0.5) H44(0.5)
 C45(0.5) H45(0.5) C46(0.5) H46(0.5) C47(0.5) H47(0.5) C48(0.5) H48(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C17(H17a,H17b), C26(H26a,H26b)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C22(H22), C24(H24), C44(H44), C45(H45), C46(H46),
 C47(H47), C48(H48)
5.c Fitted hexagon refined as free rotating group:
 C43(C44,C45,C46,C47,C48)
5.d Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C8(H8a,H8b,H8c), C9(H9a,
 H9b,H9c), C10(H10a,H10b,H10c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c),
 C27(H27a,H27b,H27c), C28(H28a,H28b,H28c), C30(H30a,H30b,H30c), C31(H31a,H31b,
 H31c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C34(H34a,H34b,H34c), C35(H35a,
 H35b,H35c), C36(H36a,H36b,H36c), C37(H37a,H37b,H37c), C38(H38a,H38b,H38c),
 C39(H39a,H39b,H39c), C40(H40a,H40b,H40c), C41(H41a,H41b,H41c), C42(H42a,H42b,
 H42c)
;
_olex2_submission_special_instructions 'No special instructions were received'