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_7711415
_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 Yb'
_chemical_formula_sum            'C31 H52 Cl3 Li N3 O3 Yb'
_chemical_formula_weight         801.08
_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     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2c79pm
_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                103.943(5)
_cell_angle_beta                 94.042(6)
_cell_angle_gamma                116.603(5)
_cell_formula_units_Z            2
_cell_length_a                   10.9753(17)
_cell_length_b                   11.5275(16)
_cell_length_c                   17.147(3)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    300
_cell_measurement_theta_max      27.457
_cell_measurement_theta_min      2.929
_cell_volume                     1842.4(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       '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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300.0
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.935
_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  0.0381
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23047
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.138
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.788
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0982 before and 0.0485 after correction. The Ratio of minimum to maximum transmission is 0.4922. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             814
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.351
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7900
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0239P)^2^+3.7886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6572
_reflns_number_total             7900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02053j2.cif
_cod_data_source_block           1Yb
_cod_original_cell_volume        1842.3(5)
_cod_database_code               7711415
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.606
_shelx_estimated_absorpt_t_min   0.579
_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
 C27A-C26A = C26A-C25A
 1.54 with sigma of 0.02
 C26A-C25A = C25A-C24A
 1.54 with sigma of 0.02
 C27A-O2 = O2-C24A
 1.43 with sigma of 0.02
 C24-O2 = O2-C27
 1.43 with sigma of 0.02
 C24-C25 = C25-C26
 1.54 with sigma of 0.02
 C27-C26 = C26-C25
 1.54 with sigma of 0.02
 C27A-C25A
 2.515 with sigma of 0.04
 C26A-C24A
 2.515 with sigma of 0.04
 C27A-C24A
 2.336 with sigma of 0.04
 C24-C27
 2.336 with sigma of 0.04
 C24-C26
 2.515 with sigma of 0.04
 C27-C25
 2.515 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O2 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C27A \\sim C26A \\sim C25A
\\sim C24A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O2, C24, C25, C26, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O2, C27A, C26A, C25A, C24A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C25A)=
 Sof(H25C)=Sof(H25D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=
 Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10)
6.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
  C27A(H27C,H27D), C26A(H26C,H26D), C25A(H25C,H25D), C24A(H24C,H24D)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C15(H15)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              11511
_olex2_submission_special_instructions 'No special instructions were received'