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_7711036
_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 Nd O2 Si4, 0.5[C7H8]'
_chemical_formula_sum            'C44 H82 Li N4 Nd O2 Si4'
_chemical_formula_weight         962.67
_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             2021-04-21
_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                 95.962(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.118(2)
_cell_length_b                   24.770(5)
_cell_length_c                   18.258(3)
_cell_measurement_reflns_used    9520
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.08
_cell_measurement_theta_min      2.28
_cell_volume                     5450.7(17)
_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      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.1489
_diffrn_reflns_av_unetI/netI     0.0905
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            142296
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.521
_diffrn_reflns_theta_min         2.243
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1372 before and 0.0757 after correction.
The Ratio of minimum to maximum transmission is 0.7891.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       block
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.345
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         12480
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0837P)^2^+19.7297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1592
_refine_ls_wR_factor_ref         0.1833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8125
_reflns_number_total             12480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02642b2.cif
_cod_data_source_block           b210304a_0ma
_cod_original_cell_volume        5450.5(17)
_cod_database_code               7711036
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.739
_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
 C00V-Li1
 4 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C00L(H00L), C00M(H00M)
3.b Secondary CH2 refined with riding coordinates:
 C00D(H00A,H00B), C00I(H00C,H00D), C00J(H00F,H00G), C00P(H00H,H00I), C00Q(H00J,
 H00K), C00U(H00R,H00T), C00V(H00U,H00V), C00Z(H00,HC), C011(H01A,H01B),
 C014(H01I,H01J), C016(H01N,H01O), C01B(H01Z,HF), C01D(H1,HI), C01F(H3,HL)
3.c Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00N(H00N), C00S(H00S), C00W(H00W)
3.d Idealised Me refined as rotating group:
 C00R(H00O,H00P,H00Q), C00X(H00X,H00Y,H), C00Y(H00Z,HA,HB), C012(H01C,H01D,
 H01E), C013(H01F,H01G,H01H), C015(H01K,H01L,H01M), C017(H01P,H01Q,H01R),
 C018(H01S,H01T,H01U), C019(H01V,H01W,H01X), C01A(H01Y,HD,HE), C01C(H01,HG,HH),
 C01E(H2,HJ,HK), C01G(H4,HM,HN), C01H(H5,HO,HP), C01I(H6,HQ,HR), C01J(H7,HS,HT)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              83148
_olex2_submission_special_instructions 'No special instructions were received'