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  (2022) –; doi:10.1039/D2DT02053J

data_7710933
_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_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02053J
_journal_year                    2022
_chemical_formula_moiety         'C81 H120 Cl N9 O3 Si6 Y3, C16 H32 Li O4'
_chemical_formula_sum            'C97 H152 Cl Li N9 O7 Si6 Y3'
_chemical_formula_weight         2033.93
_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
_audit_block_doi                 10.5517/ccdc.csd.cc28p448
_audit_creation_date             2019-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-26 deposited with the CCDC.	2022-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                67.6430(10)
_cell_angle_beta                 83.979(2)
_cell_angle_gamma                61.6610(10)
_cell_formula_units_Z            2
_cell_length_a                   19.816(2)
_cell_length_b                   20.172(2)
_cell_length_c                   21.517(2)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      25.777
_cell_measurement_theta_min      2.270
_cell_volume                     6970.8(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_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  0.0984
_diffrn_reflns_av_unetI/netI     0.1646
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81971
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.816
_diffrn_reflns_theta_min         1.028
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1210 before and 0.0591 after correction. The Ratio of minimum to maximum transmission is 0.4873. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.969
_exptl_crystal_description       block
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1229
_refine_ls_number_reflns         31977
_refine_ls_number_restraints     922
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1939
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1099P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.2275
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13022
_reflns_number_total             31977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02053j2.cif
_cod_data_source_block           1e
_cod_database_code               7710933
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.774
_shelx_estimated_absorpt_t_min   0.747
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O7-C97 = O7-C94 = O7-C94A = O7-C96
 1.43 with sigma of 0.01
 C94-C95 = C96-C95 = C97-C96 = C96A-C97 = C96A-C95A = C95A-C94A
 1.54 with sigma of 0.01
 O5-C86A = O5-C86 = O5-C89
 1.43 with sigma of 0.01
 C89-C88 = C88A-C89 = C88-C87 = C87A-C88A = C86-C87
 1.54 with sigma of 0.01
 O4-C85 = O4-C85A = O4-C82A = O4-C82
 1.43 with sigma of 0.01
 C82-C83 = C83-C82A = C83-C84A = C84-C83 = C84-C85 = C85A-C84A
 1.54 with sigma of 0.01
 O7-C95 = O7-C95A = O7-C96 = O7-C96A
 2.35 with sigma of 0.01
 C94-C96 = C95-C97
 2.52 with sigma of 0.01
 C94A-C96A = C95A-C97
 2.52 with sigma of 0.01
 C89-C87A = C86A-C88A
 2.52 with sigma of 0.01
 C89-C87 = C86-C88
 2.52 with sigma of 0.01
 C82-C84 = C83-C85
 2.52 with sigma of 0.01
 C82A-C84A = C83-C85A
 2.52 with sigma of 0.01
 O4-Li1 \\sim O5-Li1 \\sim O6-Li1 \\sim O7-Li1
 with sigma of 0.02
 O7-C96A \\sim O7-C95 \\sim O7-C95A \\sim O7-C96
 with sigma of 0.02
3. Rigid bond restraints
 O5, O6, C89, C93
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
O4 \\sim O5 \\sim O6 \\sim O7 \\sim C82 \\sim C82A \\sim C83 \\sim C84 \\sim
C84A \\sim C85 \\sim C85A \\sim C86 \\sim C86A \\sim C87 \\sim C87A \\sim C88
\\sim C88A \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim
C94A \\sim C95 \\sim C95A \\sim C96 \\sim C96A \\sim C97: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Li1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O4 \\sim O5 \\sim O6 \\sim O7 \\sim C82 \\sim C82A \\sim C83 \\sim C84 \\sim
C84A \\sim C85 \\sim C85A \\sim C86 \\sim C86A \\sim C87 \\sim C87A \\sim C88
\\sim C88A \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim
C94A \\sim C95 \\sim C95A \\sim C96 \\sim C96A \\sim C97 \\sim Li1: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C16 \\sim C17 \\sim C18 \\sim C35 \\sim C34 \\sim C61 \\sim C62 \\sim C63 \\sim
C57 \\sim C56 \\sim C55 \\sim C54: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(C82A)=Sof(H82C)=Sof(H82D)=Sof(H83C)=Sof(H83D)=Sof(C84A)=Sof(H84C)=
 Sof(H84D)=Sof(C85A)=Sof(H85C)=Sof(H85D)=Sof(C86A)=Sof(H86C)=Sof(H86D)=
 Sof(C87A)=Sof(H87C)=Sof(H87D)=Sof(C88A)=Sof(H88C)=Sof(H88D)=Sof(H89C)=
 Sof(H89D)=Sof(C94A)=Sof(H94C)=Sof(H94D)=Sof(C95A)=Sof(H95C)=Sof(H95D)=
 Sof(C96A)=Sof(H96C)=Sof(H96D)=Sof(H97C)=Sof(H97D)=1-FVAR(1)
 Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H83A)=Sof(H83B)=Sof(C84)=Sof(H84A)=Sof(H84B)=
 Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(C87)=Sof(H87A)=
 Sof(H87B)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H89A)=Sof(H89B)=Sof(C94)=Sof(H94A)=
 Sof(H94B)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(H97A)=
 Sof(H97B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C37(H37), C40(H40), C58(H58), C61(H61)
6.b Secondary CH2 refined with riding coordinates:
 C82(H82A,H82B), C82A(H82C,H82D), C83(H83C,H83D), C83(H83A,H83B), C84(H84A,
 H84B), C84A(H84C,H84D), C85(H85A,H85B), C85A(H85C,H85D), C86(H86A,H86B),
 C86A(H86C,H86D), C87(H87A,H87B), C87A(H87C,H87D), C88(H88A,H88B), C88A(H88C,
 H88D), C89(H89A,H89B), C89(H89C,H89D), C90(H90A,H90B), C91(H91A,H91B),
 C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C94A(H94C,H94D), C95(H95A,
 H95B), C95A(H95C,H95D), C96(H96A,H96B), C96A(H96C,H96D), C97(H97A,H97B),
 C97(H97C,H97D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14),
 C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C33(H33), C34(H34), C35(H35),
  C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C54(H54), C55(H55), C56(H56)
6.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,
 H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C),
 C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,
 H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,
 H81B,H81C)
;
_shelx_res_checksum              8665
_shelx_hkl_checksum              60835
_shelx_fab_checksum              9515
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'