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_7710928
_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 Nd3 O3 Si6, C16 H32 Li O4'
_chemical_formula_sum            'C97 H152 Cl Li N9 Nd3 O7 Si6'
_chemical_formula_weight         2199.92
_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.cc28p404
_audit_creation_date             2019-11-07
_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                68.2219(10)
_cell_angle_beta                 84.2175(10)
_cell_angle_gamma                61.4812(9)
_cell_formula_units_Z            2
_cell_length_a                   19.8695(14)
_cell_length_b                   20.1675(14)
_cell_length_c                   21.5072(15)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      21.296
_cell_measurement_theta_min      2.196
_cell_volume                     7001.2(9)
_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)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1055
_diffrn_reflns_av_unetI/netI     0.1441
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            69464
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.024
_exptl_absorpt_coefficient_mu    1.207
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1007 before and 0.0570 after correction. The Ratio of minimum to maximum transmission is 0.7055. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.044
_exptl_crystal_description       block
_exptl_crystal_F_000             2274
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1075
_refine_ls_number_reflns         24635
_refine_ls_number_restraints     627
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1627
_refine_ls_R_factor_gt           0.0705
_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^)+(0.0959P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.2029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11236
_reflns_number_total             24635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02053j2.cif
_cod_data_source_block           1a
_cod_database_code               7710928
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.869
_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
 O4-C81 = O4-C84 = O5-C85 = O5-C88 = O6-C89 = O6-C92
 1.43 with sigma of 0.01
 C81-C82 = C83-C82 = C84-C83 = C86-C85 = C87-C86 = C87-C88 = C90-C89 = C90-C91
 = C91-C92
 1.54 with sigma of 0.01
 O7-C96 = O7-C93
 1.43 with sigma of 0.01
 C95-C96 = C94-C95 = C94-C93
 1.54 with sigma of 0.01
 C61-C60 = C60-C62
 1.54 with sigma of 0.01
 C83-C81 = C82-C84 = C85-C87 = C86-C88 = C92-C90 = C89-C91
 2.52 with sigma of 0.01
 C96-C94 = C95-C93
 2.52 with sigma of 0.01
3. Rigid bond restraints
 C19, C21, C46, C47, C25, C26
 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 Li1: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
O4 \\sim O5 \\sim O6 \\sim O7 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85
\\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93
\\sim C94 \\sim C95 \\sim C96 \\sim Li1: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C4 \\sim C9AA \\sim C13 \\sim C14 \\sim C15 \\sim C24 \\sim C9AA \\sim C28
\\sim C33 \\sim C34 \\sim C35 \\sim C39 \\sim C40 \\sim C41 \\sim C55 \\sim C56
\\sim C60 \\sim C61 \\sim C62: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C36(H36), C39(H39), C57(H57), C60(H60)
5.b Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,
 H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B),
 C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B),
  C95(H95A,H95B), C96(H96A,H96B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C4(H4), C7(H7), C6(H6), C12(H12), C13(H13), C14(H14),
 C23(H23), C27(H27), C26(H26), C25(H25), C28(H28), C32(H32), C33(H33), C34(H34),
  C43(H43), C45(H45), C48(H48), C47(H47), C46(H46), C53(H53), C54(H54), C55(H55)
5.d Fitted hexagon refined as free rotating group:
 C5(C4,C3,C8,C7,C6), C10(C11,C12,C13,C14,C15), C27(C26,C25,C24,C9AA,C28),
 C30(C31,C32,C33,C34,C35), C45(C44,C49,C48,C47,C46), C51(C52,C53,C54,C55,C56)
5.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C),
 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)
;
_shelx_res_checksum              82138
_shelx_hkl_checksum              66890
_shelx_fab_checksum              80762
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'