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_7711033
_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 O2 Si4 Y'
_chemical_formula_sum            'C40 H78 Li N4 O2 Si4 Y'
_chemical_formula_weight         855.27
_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     dual
_audit_creation_date             2021-10-09
_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                 102.163(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.910(3)
_cell_length_b                   15.955(3)
_cell_length_c                   23.692(4)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.79
_cell_measurement_theta_min      2.28
_cell_volume                     5140.0(17)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.981
_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  0.0844
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27207
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.420
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_type   multi-scan
_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    1.105
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   25.681
_exptl_transmission_factor_min   2.420
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         9570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0517P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5939
_reflns_number_total             9570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02642b2.cif
_cod_data_source_block           b190506e_0m_a
_cod_original_cell_volume        5140.1(16)
_cod_database_code               7711033
_shelx_shelxl_version_number     2018/3
_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.a Secondary CH2 refined with riding coordinates:
 C00G(H00A,H00B), C00I(H00F,H00G), C00J(H00H,H00I), C00O(H00J,H00L)
2.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00M(H00M), C00N(H00N), C00T(H00U)
2.c Idealised Me refined as rotating group:
 C00H(H00C,H00D,H00E), C00R(H00O,H00P,H00Q), C00S(H00R,H00S,H00T), C00V(H00V,
 H00W,H00X), C00X(H00Y,H,HA), C00Z(H00Z,HB,HC), C010(H01A,H01B,H01C), C011(H01D,
 H01E,H01F), C012(H01G,H01H,H01I), C013(H01J,H01K,H01L), C014(H01M,H01N,H01O),
 C015(H01P,H01Q,H01R), C016(H01S,H01T,H01U), C017(H01V,H01W,H01X), C018(H01Y,HD,
 HE), C019(H01Z,HF,HG), C01A(H01,HH,HI), C01B(H1,HJ,HK), C01C(H2,HL,HM),
 C01D(H3,HN,HO), C01E(H4,HP,HQ), C01F(H5,HR,HS)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51451
_shelx_fab_checksum              91822
_olex2_submission_special_instructions 'No special instructions were received'