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_7711035
_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         'C44 H82 Li N4 O2 Si4 Y'
_chemical_formula_sum            'C44 H82 Li N4 O2 Si4 Y'
_chemical_formula_weight         907.34
_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
_audit_creation_date             2021-03-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-12-14 deposited with the CCDC.	2022-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                88.666(2)
_cell_angle_beta                 87.092(2)
_cell_angle_gamma                71.124(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2861(8)
_cell_length_b                   12.8406(9)
_cell_length_c                   17.9613(11)
_cell_measurement_reflns_used    9694
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.25
_cell_volume                     2677.7(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_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      150.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.983
_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_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            97127
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.587
_diffrn_reflns_theta_min         2.251
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1265 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.7648.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_preparation       absorption
_exptl_crystal_recrystallization_method correction
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         12180
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.325
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+1.6567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10037
_reflns_number_total             12180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02642b2.cif
_cod_data_source_block           mo_b20190424_0m_a
_cod_database_code               7711035
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.793
_shelx_estimated_absorpt_t_min   0.712
_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
 C00D-Li1
 3 with sigma of 0.02
 C00J-Li1
 4.5 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C00Q(H00Q), C00T(H00T)
3.b Secondary CH2 refined with riding coordinates:
 C00D(H00A,H00B), C00J(H00C,H00D), C00L(H00E,H00F), C00O(H00J,H00L), C00X(H00Z,
 H), C00Y(H00,HA), C00Z(H1,HB), C01A(H01Z,HE), C01B(H01,HF), C01C(H2,HG),
 C01E(H4,HJ), C01F(H5,HK), C01H(H7,HN), C01J(H9,HQ)
3.c Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00P(H00P), C00R(H00R), C014(H014)
3.d Idealised Me refined as rotating group:
 C00M(H00G,H00H,H00I), C00U(H00M,H00N,H00O), C00V(H00S,H00U,H00V), C00W(H00W,
 H00X,H00Y), C010(H01A,H01B,H01C), C011(H01D,H01E,H01F), C012(H01G,H01H,H01I),
 C013(H01J,H01K,H01L), C015(H01M,H01N,H01O), C016(H01P,H01Q,H01R), C017(H01S,
 H01T,H01U), C018(H01V,H01W,H01X), C019(H01Y,HC,HD), C01D(H3,HH,HI), C01G(H6,HL,
 HM), C01I(H8,HO,HP)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82568
_shelx_fab_checksum              47060
_olex2_exptl_crystal_mounting_method 'multi screen'
_olex2_submission_special_instructions 'No special instructions were received'