Trivalent Rare-Earth Metal Cyclic (Alkyl)(Amino)Carbene Complexes
Xiao, Yuyuan; Liu, Ziyu; Liang, Jiefeng; Yang, Kexin; Huang, Wenliang; Dalton Transactions  (2022) –; doi:10.1039/D2DT02759C

data_7711329
_publ_section_title
;
 Trivalent Rare-Earth Metal Cyclic (Alkyl)(Amino)Carbene Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02759C
_journal_year                    2022
_chemical_formula_moiety         'C34 H68 Lu N Si3'
_chemical_formula_sum            'C34 H68 Lu N Si3'
_chemical_formula_weight         750.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-06-16
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2022-07-01 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.549(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4110(2)
_cell_length_b                   19.6904(4)
_cell_length_c                   21.3623(5)
_cell_measurement_reflns_used    16242
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      29.3920
_cell_measurement_theta_min      2.3360
_cell_volume                     4341.25(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.22a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.22a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.22a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -23.00  16.00   0.50    0.87    --   15.80  19.00 -90.00   78
  2  \w     25.00  56.00   0.50    0.87    --   15.80  19.00 -90.00   62
  3  \w    -26.00  92.00   0.50    0.87    --   15.80  82.00 150.00  236
  4  \w      3.00  30.00   0.50    0.87    --   15.80  57.00-120.00   54
  5  \w    -19.00  97.00   0.50    0.87    --   15.80  57.00  30.00  232
  6  \w    -74.00 -49.00   0.50    0.87    --   15.80  19.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0265069000
_diffrn_orient_matrix_UB_12      -0.0181385000
_diffrn_orient_matrix_UB_13      0.0273669000
_diffrn_orient_matrix_UB_21      0.0071857000
_diffrn_orient_matrix_UB_22      0.0308422000
_diffrn_orient_matrix_UB_23      0.0172482000
_diffrn_orient_matrix_UB_31      -0.0629870000
_diffrn_orient_matrix_UB_32      -0.0041151000
_diffrn_orient_matrix_UB_33      0.0087126000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33192
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.448
_diffrn_reflns_theta_min         2.228
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.376
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.22a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.504
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.152
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         10941
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.8613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9080
_reflns_number_total             10941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02759c2.cif
_cod_data_source_block           lzy0614_sq
_cod_database_code               7711329
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Si Lu'
_shelx_estimated_absorpt_t_max   0.714
_shelx_estimated_absorpt_t_min   0.381
_olex2_refinement_description
;
1. Restrained distances
 Si3-C34 \\sim Si3-C34A
 with sigma of 0.02
 Si2-C30A \\sim Si2-C30
 with sigma of 0.02
 C9-C10A \\sim C9-C10
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C34)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) = Uanis(C34A)
3. Others
 Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(C30)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(2)
 Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(2)
 Sof(H9BC)=Sof(H9BD)=Sof(C10)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(3)
 Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20)
4.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C31(H31A,H31B), C3(H3A,H3B), C27(H27A,H27B), C7(H7A,H7B),
 C9(H9AA,H9AB), C9(H9BC,H9BD)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C13(H13), C14(H14)
4.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C18(H18A,H18B,H18C), C21(H21A,H21B,
 H21C), C8(H8A,H8B,H8C), C5(H5A,H5B,H5C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C6(H6A,H6B,H6C), C33(H33A,H33B,H33C), C24(H24A,H24B,H24C), C10A(H10A,
 H10B,H10C), C29(H29A,H29B,H29C), C30A(H30A,H30B,H30C), C32(H32A,H32B,H32C),
 C34(H34A,H34B,H34C), C28(H28A,H28B,H28C), C34A(H34D,H34E,H34F), C30(H30D,H30E,
 H30F), C10(H10D,H10E,H10F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25443
_shelx_hkl_checksum              32107
_shelx_fab_checksum              48320
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.795
_oxdiff_exptl_absorpt_empirical_full_min 0.714