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_7711324
_publ_section_title
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 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         'C32 H64 N Sc Si3'
_chemical_formula_sum            'C32 H64 N Sc Si3'
_chemical_formula_weight         592.07
_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            16
_cell_length_a                   21.2782(4)
_cell_length_b                   17.1989(3)
_cell_length_c                   41.7376(10)
_cell_measurement_reflns_used    27902
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.4130
_cell_measurement_theta_min      2.5910
_cell_volume                     15274.4(5)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.875
_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    -30.00  -3.78   0.38    5.00    --  -21.28  28.00 -49.00   69
  2  \w    -23.00 101.26   0.38    5.00    --   19.72  77.00  90.00  327
  3  \w     47.00  83.86   0.38    5.00    --   19.72 178.00 -60.00   97
  4  \w    -62.00 -10.70   0.38    5.00    --   19.72 -28.00 148.00  135
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0155725000
_diffrn_orient_matrix_UB_12      0.0351213000
_diffrn_orient_matrix_UB_13      0.0040006000
_diffrn_orient_matrix_UB_21      -0.0269523000
_diffrn_orient_matrix_UB_22      -0.0214487000
_diffrn_orient_matrix_UB_23      0.0047050000
_diffrn_orient_matrix_UB_31      0.0119293000
_diffrn_orient_matrix_UB_32      -0.0025331000
_diffrn_orient_matrix_UB_33      0.0158377000
_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  0.0316
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            73359
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.420
_diffrn_reflns_theta_min         2.303
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.22a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.030
_exptl_crystal_description       block
_exptl_crystal_F_000             5216
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.169
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         20247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+6.9799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16006
_reflns_number_total             20247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02759c2.cif
_cod_data_source_block           20090012xiao
_cod_database_code               7711324
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Si Sc Cl'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Si2) = Uanis(C25)
Uanis(Si4) = Uanis(C55)
2.a Ternary CH refined with riding coordinates:
 C15(H15), C47(H47), C18(H18), C50(H50)
2.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C57(H57A,H57B), C61(H61A,H61B), C35(H35A,H35B), C21(H21A,
 H21B), C3(H3A,H3B), C25(H25A,H25B), C53(H53A,H53B)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C12(H12), C45(H45), C43(H43), C44(H44)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C63(H63A,H63B,H63C), C37(H37A,H37B,H37C), C26(H26A,H26B,
 H26C), C5(H5A,H5B,H5C), C22(H22A,H22B,H22C), C31(H31A,H31B,H31C), C16(H16A,
 H16B,H16C), C62(H62A,H62B,H62C), C40(H40A,H40B,H40C), C59(H59A,H59B,H59C),
 C20(H20A,H20B,H20C), C7(H7A,H7B,H7C), C58(H58A,H58B,H58C), C48(H48A,H48B,H48C),
  C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C32(H32A,H32B,H32C), C23(H23A,H23B,H23C),
 C17(H17A,H17B,H17C), C60(H60A,H60B,H60C), C52(H52A,H52B,H52C), C19(H19A,H19B,
 H19C), C38(H38A,H38B,H38C), C64(H64A,H64B,H64C), C28(H28A,H28B,H28C), C51(H51A,
 H51B,H51C), C39(H39A,H39B,H39C), C49(H49A,H49B,H49C), C30(H30A,H30B,H30C),
 C56(H56A,H56B,H56C), C27(H27A,H27B,H27C), C55(H55A,H55B,H55C), C54(H54A,H54B,
 H54C)
;
_shelx_res_checksum              30196
_shelx_hkl_checksum              55242
_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 1.208
_oxdiff_exptl_absorpt_empirical_full_min 0.831