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_7711327
_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         'C40 H62 I3 N2 Yb, C7 H8'
_chemical_formula_sum            'C47 H70 I3 N2 Yb'
_chemical_formula_weight         1216.79
_chemical_name_systematic        MeCAACYbI3
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-20
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3367(5)
_cell_length_b                   13.3310(6)
_cell_length_c                   19.8826(8)
_cell_measurement_reflns_used    11858
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.4770
_cell_measurement_theta_min      2.8540
_cell_volume                     4860.2(3)
_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      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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     54.00  81.00   0.50   17.00    --    1.90  57.00  60.00   54
  2  \w    -20.00  26.00   0.50   17.00    --    1.90  57.00   0.00   92
  3  \w     40.00  84.00   0.50   17.00    --    1.90  57.00   0.00   88
  4  \w    -87.00 -42.00   0.50   17.00    --    1.90 -37.00-120.00   90
  5  \w     -4.00  21.00   0.50   17.00    --    1.90 -37.00-120.00   50
  6  \w    -16.00  10.00   0.50   17.00    --    1.90 -37.00   0.00   52
  7  \w     10.00  35.00   0.50   17.00    --    1.90  57.00  60.00   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      -0.0251309000
_diffrn_orient_matrix_UB_12      0.0337433000
_diffrn_orient_matrix_UB_13      -0.0150498000
_diffrn_orient_matrix_UB_21      -0.0158289000
_diffrn_orient_matrix_UB_22      -0.0402913000
_diffrn_orient_matrix_UB_23      -0.0180720000
_diffrn_orient_matrix_UB_31      -0.0248161000
_diffrn_orient_matrix_UB_32      -0.0084723000
_diffrn_orient_matrix_UB_33      0.0267749000
_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  0.0691
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40645
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.787
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.861
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.373
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       block
_exptl_crystal_F_000             2380
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.364
_exptl_crystal_size_min          0.189
_refine_diff_density_max         1.525
_refine_diff_density_min         -1.508
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.023(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         11597
_refine_ls_number_restraints     248
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0830P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.922
_reflns_number_gt                9072
_reflns_number_total             11597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02759c2.cif
_cod_data_source_block           xiao
_cod_database_code               7711327
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Yb I'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.02326
 -0.02326
2. Restrained distances
 C47-C41
 1.51 with sigma of 0.02
 C41-C42 = C41-C46 = C43-C44
 1.39 with sigma of 0.02
 C42-C43 = C44-C45 = C45-C46
 1.38 with sigma of 0.02
 C30-C35
 1.516 with sigma of 0.01
 C31-C32
 1.35 with sigma of 0.01
 C29-C34
 1.4 with sigma of 0.01
 C2-C6
 1.53 with sigma of 0.01
 C35-C36
 1.53 with sigma of 0.01
 C32-C33
 1.4 with sigma of 0.01
 C38-C39
 1.51 with sigma of 0.01
 C38-C40
 1.55 with sigma of 0.01
 C4-C8
 1.52 with sigma of 0.01
 C4-C7
 1.51 with sigma of 0.01
 C22-C26
 1.53 with sigma of 0.01
 C22-C23
 1.55 with sigma of 0.01
 C22-C25
 1.55 with sigma of 0.01
 C15-C17
 1.54 with sigma of 0.01
 C15-C16
 1.54 with sigma of 0.01
 C11-C12
 1.37 with sigma of 0.01
 C24-C27
 1.53 with sigma of 0.01
 C24-C28
 1.5 with sigma of 0.01
 C23-C24
 1.52 with sigma of 0.01
 C41-C47
 1.49 with sigma of 0.01
 C41-C43
 2.42 with sigma of 0.04
 C42-C44
 2.39 with sigma of 0.04
 C41-C45
 2.41 with sigma of 0.04
 C43-C45 = C44-C46
 2.4 with sigma of 0.04
 C47-C42 = C47-C46
 2.52 with sigma of 0.04
 C41-C42 \\sim C42-C43 \\sim C43-C44 \\sim C44-C45 \\sim C45-C46 \\sim C46-C41
 with sigma of 0.02
 C41-C45 \\sim C41-C43 \\sim C46-C44 \\sim C42-C46 \\sim C43-C45 \\sim C42-C44
 with sigma of 0.04
 C47-C46 \\sim C47-C42
 with sigma of 0.04
3. Restrained planarity
 C47, C41, C42, C43, C44, C45, C46
 with sigma of 0.1
4. Rigid bond restraints
 C22, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C47 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C47) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C42) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 C47, C41, C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7.a Ternary CH refined with riding coordinates:
 C35(H35), C38(H38), C15(H15), C18(H18)
7.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C23(H23A,H23B)
7.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C33(H33), C13(H13), C12(H12), C11(H11), C42(H42),
 C43(H43), C44(H44), C45(H45), C46(H46)
7.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C),
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C8(H8A,H8B,H8C),
 C26(H26A,H26B,H26C), C37(H37A,H37B,H37C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C28(H28A,H28B,H28C), C25(H25A,H25B,H25C), C40(H40A,H40B,H40C), C27(H27A,
 H27B,H27C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              76023
_shelx_hkl_checksum              26547
_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 17.778
_oxdiff_exptl_absorpt_empirical_full_min 0.326