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_7711323
_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 N Sc Si3'
_chemical_formula_sum            'C34 H68 N Sc Si3'
_chemical_formula_weight         620.12
_chemical_name_systematic        EtCAACScSi3
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-30
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-01 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.1966(12)
_cell_length_b                   16.7104(10)
_cell_length_c                   23.0440(14)
_cell_measurement_reflns_used    5836
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.4150
_cell_measurement_theta_min      2.9690
_cell_volume                     8162.3(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.855
_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    -32.00  -1.00   0.50   49.28    --   -1.70 -82.00-150.00   62
  2  \w      6.00  31.00   0.50   49.28    --   -1.70 -82.00-150.00   50
  3  \w    -32.00  32.00   0.50   49.28    --    1.90 -82.00 -30.00  128
;
_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      -0.0326267000
_diffrn_orient_matrix_UB_12      0.0085334000
_diffrn_orient_matrix_UB_13      -0.0028845000
_diffrn_orient_matrix_UB_21      0.0071600000
_diffrn_orient_matrix_UB_22      0.0410112000
_diffrn_orient_matrix_UB_23      -0.0045560000
_diffrn_orient_matrix_UB_31      0.0020616000
_diffrn_orient_matrix_UB_32      -0.0069488000
_diffrn_orient_matrix_UB_33      -0.0302968000
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37290
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.240
_diffrn_reflns_theta_min         2.593
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.288
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.009
_exptl_crystal_description       plate
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.299
_exptl_crystal_size_min          0.111
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         10401
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0681
_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^)+(0.0696P)^2^+7.8296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7147
_reflns_number_total             10401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02759c2.cif
_cod_data_source_block           exp_5650
_cod_database_code               7711323
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Sc Si'
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.844
_olex2_refinement_description
;
1. Restrained distances
 C39-Si4
 1.82 with sigma of 0.1
 C39-C39_$1
 2.2 with sigma of 0.01
 C39_$1-C39
 2.3 with sigma of 0.01
2. Rigid bond restraints
 Si3, C28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C36: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.001 within
2A
Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C25) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C35) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C36) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(Si1)=1-FVAR(1)
 Sof(Si4)=FVAR(1)
 Sof(C23)=Sof(H23A)=Sof(H23B)=1-FVAR(2)
 Sof(C37)=Sof(H37A)=Sof(H37B)=FVAR(2)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=1-FVAR(3)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(3)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=1-FVAR(4)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(4)
 Fixed Sof: C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C40(0.5) H40A(0.5)
 H40B(0.5) H40C(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C25(0.5) H25A(0.5)
 H25B(0.5) H25C(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C39(0.5) H39A(0.5)
 H39B(0.5) H39C(0.5)
5.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C27(H27A,H27B), C3(H3A,H3B), C7(H7A,H7B), C31(H31A,H31B),
 C37(H37A,H37B), C23(H23A,H23B)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C14(H14)
5.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C34(H34A,H34B,H34C), C22(H22A,H22B,
 H22C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C21(H21A,H21B,H21C), C32(H32A,
 H32B,H32C), C8(H8A,H8B,H8C), C33(H33A,H33B,H33C), C28(H28A,H28B,H28C), C6(H6A,
 H6B,H6C), C29(H29A,H29B,H29C), C38(H38A,H38B,H38C), C30(H30A,H30B,H30C),
 C40(H40A,H40B,H40C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C24(H24A,H24B,
 H24C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              21006
_shelx_hkl_checksum              75594
_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 1.986
_oxdiff_exptl_absorpt_empirical_full_min 0.398