Synthesis of rare-earth metal complexes with a morpholine-functionalized β-diketiminato ligand and their catalytic activities towards C-O and C-N bond formation.
Zhu, Xiancui; He, Jinqiang; Yang, Yuanqing; Zhou, Shuangliu; Wei, Yun; Wang, Shaowu; Dalton transactions (Cambridge, England : 2003) 51 (2022) 13227–13235; doi:10.1039/d2dt02053j

data_7711414
_publ_section_title
;
 Synthesis of rare-earth metal complexes with a morpholine-functionalized
 \b-diketiminato ligand and their catalytic activities towards C-O and C-N
 bond formation.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13227
_journal_page_last               13235
_journal_paper_doi               10.1039/d2dt02053j
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C31 H52 Cl3 Li N3 O3 Y'
_chemical_formula_sum            'C31 H52 Cl3 Li N3 O3 Y'
_chemical_formula_weight         717.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2c79nl
_audit_creation_date             2021-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-25 deposited with the CCDC.	2022-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                103.679(2)
_cell_angle_beta                 94.344(2)
_cell_angle_gamma                116.617(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0084(8)
_cell_length_b                   11.5337(8)
_cell_length_c                   17.1823(11)
_cell_measurement_reflns_used    9294
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.552
_cell_measurement_theta_min      3.139
_cell_volume                     1853.2(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.9880
_diffrn_measured_fraction_theta_max 0.9880
_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  0.0604
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            75295
_diffrn_reflns_theta_full        27.5917
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.839
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.3763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1263 before and 0.0587 after correction. The Ratio of minimum to maximum transmission is 0.5048. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.2848
_exptl_crystal_description       block
_exptl_crystal_F_000             747.1264
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.7432
_refine_diff_density_min         -0.9134
_refine_diff_density_rms         0.1074
_refine_ls_d_res_high            0.7672
_refine_ls_d_res_low             6.9878
_refine_ls_goodness_of_fit_ref   1.0916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    91
_refine_ls_number_parameters     431
_refine_ls_number_reflns         8492
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.0860
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.0012
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+2.3444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                6883
_reflns_number_total             8492
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt02053j2.cif
_cod_data_source_block           1Y
_cod_database_code               7711414
_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
 C24-O2 = O2-C27
 1.43 with sigma of 0.02
 C24a-O2a = O2a-C27a
 1.43 with sigma of 0.02
 C24-C25 = C25-C26
 1.54 with sigma of 0.02
 C25-C26 = C26-C27
 1.54 with sigma of 0.02
 C24a-C25a = C25a-C26a
 1.54 with sigma of 0.02
 C25a-C26a = C26a-C27a
 1.54 with sigma of 0.02
 C24-C27
 2.336 with sigma of 0.04
 C24a-C27a
 2.336 with sigma of 0.04
 C24-C26
 2.515 with sigma of 0.04
 C25-C27
 2.515 with sigma of 0.04
 C24a-C26a
 2.515 with sigma of 0.04
 C25a-C27a
 2.515 with sigma of 0.04
 O2-C25 \\sim O2a-C25a
 with sigma of 0.02
 O2-C26 \\sim O2a-C26a
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim C27 \\sim C24 \\sim C25 \\sim C26 \\sim C27a \\sim C26a \\sim C25a
\\sim C24a \\sim O2a: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
4. Rigid body (RIGU) restrains
 O2, C27, C24, C25, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C27a, C26a, C25a, C24a, O2a
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C27a)=Sof(C26a)=Sof(C25a)=Sof(C24a)=Sof(O2a)=Sof(H27d)=Sof(H27c)=
 Sof(H26d)=Sof(H26c)=Sof(H25d)=Sof(H25c)=Sof(H24c)=Sof(H24d)=1-FVAR(1)
 Sof(C27)=Sof(C26)=Sof(C25)=Sof(C24)=Sof(O2)=Sof(H27b)=Sof(H27a)=Sof(H24a)=
 Sof(H24b)=Sof(H25a)=Sof(H25b)=Sof(H26b)=Sof(H26a)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C10(H10), C3(H3)
6.b Secondary CH2 refined with riding coordinates:
 C18(H18a,H18b), C20(H20a,H20b), C23(H23a,H23b), C19(H19a,H19b), C22(H22a,
 H22b), C29(H29a,H29b), C28(H28a,H28b), C31(H31a,H31b), C21(H21a,H21b),
 C27(H27b,H27a), C30(H30a,H30b), C24(H24a,H24b), C25(H25a,H25b), C26(H26b,H26a),
  C27a(H27d,H27c), C26a(H26d,H26c), C25a(H25d,H25c), C24a(H24c,H24d)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C5(H5), C15(H15)
6.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C13(H13a,H13b,H13c), C17(H17a,H17b,H17c), C12(H12a,H12b,
 H12c), C11(H11a,H11b,H11c), C2(H2a,H2b,H2c)
;
_olex2_submission_special_instructions 'No special instructions were received'