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_7711416
_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         'C39 H65 N4 O Si Y'
_chemical_formula_sum            'C39 H65 N4 O Si Y'
_chemical_formula_weight         722.95
_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   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2c79vs
_audit_creation_date             2021-07-17
_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                86.101(2)
_cell_angle_beta                 84.965(2)
_cell_angle_gamma                69.8760(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1438(11)
_cell_length_b                   11.2147(12)
_cell_length_c                   21.504(2)
_cell_measurement_reflns_used    5343
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      22.02
_cell_measurement_theta_min      2.19
_cell_volume                     2511.6(4)
_computing_cell_refinement       '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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.982
_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  0.1144
_diffrn_reflns_av_unetI/netI     0.1374
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22403
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         1.903
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.211
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.956
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         11332
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1035P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1830
_refine_ls_wR_factor_ref         0.2091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6409
_reflns_number_total             11332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02053j2.cif
_cod_data_source_block           3Y
_cod_database_code               7711416
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.776
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H4-H37
 2 with sigma of 0.02
 H37-H4
 2.1 with sigma of 0.02
3. Rigid bond restraints
 Si1, C25
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Si1, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Si1, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C37, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C37, C39
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(Si1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Riding coordinates:
 N4(H4)
5.b Ternary CH refined with riding coordinates:
 C3(H3), C30(H30), C10(H10), C37(H37)
5.c Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C18(H18A,
 H18B), C19(H19A,H19B), C22(H22A,H22B)
5.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C33(H33), C7(H7), C5(H5), C34(H34), C35(H35), C6(H6)
5.e Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C13(H13A,H13B,H13C), C1(H1A,H1B,H1C), C17(H17A,H17B,H17C),
 C12(H12A,H12B,H12C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C11(H11A,H11B,
 H11C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C27(H27A,H27B,H27C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'