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_7711034
_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         'C40 H78 Li N4 Nd O2 Si4, C4 H5'
_chemical_formula_sum            'C44 H83 Li N4 Nd O2 Si4'
_chemical_formula_weight         963.68
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-10-15
_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                90
_cell_angle_beta                 102.626(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9562(7)
_cell_length_b                   15.9734(8)
_cell_length_c                   23.9218(12)
_cell_measurement_reflns_used    9817
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.28
_cell_volume                     5203.9(5)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0606
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            70042
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.530
_diffrn_reflns_theta_min         2.401
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0987 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.8564.
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    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         11980
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0320P)^2^+3.4606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8914
_reflns_number_total             11980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02642b2.cif
_cod_data_source_block           b190507d_0m_a_sx
_cod_database_code               7711034
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.729
_shelx_estimated_absorpt_t_min   0.603
_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
 C00T-Li1
 3 with sigma of 0.02
 C00T-Li1 = Li1-C00M
 3.3 with sigma of 0.02
 C00L-Li1
 3.3 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C00L(H00A,H00B), C00M(H00C,H00D), C00P(H00J,H00K), C00T(H00P,H00Q)
3.b Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00I(H00I), C00N(H00N), C00S(H00S), C01H(H5), C01J(H6)
3.c Idealised Me refined as rotating group:
 C00O(H00E,H00F,H00H), C00Q(H00L,H00M,H00O), C00U(H00R,H00T,H00U), C00V(H00V,
 H00W,H00X), C00W(H00Y,H,HA), C00X(H00Z,HB,HC), C00Z(H00,HD,HE), 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,HF,HG), C01A(H01Z,HH,HI), C01B(H01,HJ,HK), C01C(H1,HL,
 HM), C01D(H2,HN,HO), C01E(H3,HP,HQ), C01F(H4,HR,HS), C01K(H7,HT,HU)
;
_shelx_res_checksum              94088
_olex2_submission_special_instructions 'No special instructions were received'