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_7711325
_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         'C40 H62 I3 N2 Y, C7 H8'
_chemical_formula_sum            'C47 H70 I3 N2 Y'
_chemical_formula_weight         1132.66
_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     heavy
_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            4
_cell_length_a                   18.3616(4)
_cell_length_b                   13.3428(3)
_cell_length_c                   19.9386(5)
_cell_measurement_reflns_used    36166
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      30.5760
_cell_measurement_theta_min      2.5220
_cell_volume                     4884.9(2)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(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 0.921
_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    -47.00 -21.00   0.50    0.29    --   17.58 -37.00 150.00   52
  2  \w     69.00  98.00   0.50    0.29    --   17.58 178.00 120.00   58
  3  \w    -12.00  75.00   0.50    0.29    --   17.58  57.00-120.00  174
  4  \w    -10.00  16.00   0.50    0.29    --   17.58 -37.00 150.00   52
  5  \w    -12.00  79.00   0.50    0.29    --   17.58  57.00   0.00  182
  6  \w     71.00  97.00   0.50    0.29    --   17.58 178.00-180.00   52
  7  \w    -21.00  49.00   0.50    0.29    --  -18.20  19.00 120.00  140
  8  \w    -16.00  28.00   0.50    0.29    --  -18.20 -99.00  90.00   88
  9  \w   -108.00  54.00   0.50    0.29    --  -18.20   0.00 -30.00  324
;
_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      0.0010665000
_diffrn_orient_matrix_UB_12      -0.0479521000
_diffrn_orient_matrix_UB_13      0.0153019000
_diffrn_orient_matrix_UB_21      0.0086878000
_diffrn_orient_matrix_UB_22      -0.0219688000
_diffrn_orient_matrix_UB_23      -0.0314015000
_diffrn_orient_matrix_UB_31      0.0376308000
_diffrn_orient_matrix_UB_32      0.0064501000
_diffrn_orient_matrix_UB_33      0.0067980000
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            61388
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.764
_diffrn_reflns_theta_min         2.442
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.121
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61807
_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    1.540
_exptl_crystal_description       plate
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.302
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.028(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         13316
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0249P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0602
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.821
_reflns_number_gt                11385
_reflns_number_total             13316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02759c2.cif
_cod_data_source_block           exp_536
_cod_database_code               7711325
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.335
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.02792
 -0.02792
2. Restrained distances
 C41-C42
 1.51 with sigma of 0.02
 C42-C47 = C42-C43 = C46-C45
 1.39 with sigma of 0.02
 C47-C46 = C45-C44 = C44-C43
 1.38 with sigma of 0.02
 C42-C46
 2.42 with sigma of 0.04
 C47-C45
 2.39 with sigma of 0.04
 C42-C44
 2.41 with sigma of 0.04
 C46-C44 = C45-C43
 2.4 with sigma of 0.04
 C41-C47 = C41-C43
 2.52 with sigma of 0.04
 C42-C47 \\sim C47-C46 \\sim C46-C45 \\sim C45-C44 \\sim C44-C43 \\sim C43-C42
 with sigma of 0.02
 C42-C44 \\sim C42-C46 \\sim C43-C45 \\sim C47-C43 \\sim C46-C44 \\sim C47-C45
 with sigma of 0.04
 C41-C43 \\sim C41-C47
 with sigma of 0.04
3. Restrained planarity
 C41, C42, C47, C46, C45, C44, C43
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C41 \\sim C42 \\sim C47 \\sim C46 \\sim C45 \\sim C44 \\sim C43: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C41, C42, C47, C46, C45, C44, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Ternary CH refined with riding coordinates:
 C18(H18), C15(H15), C38(H38), C35(H35)
6.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C3(H3A,H3B)
6.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C32(H32), C12(H12), C31(H31), C33(H33), C13(H13), C47(H47),
 C46(H46), C45(H45), C44(H44), C43(H43)
6.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C20(H20A,H20B,H20C), C36(H36A,H36B,H36C), C28(H28A,H28B,
 H28C), C39(H39A,H39B,H39C), C26(H26A,H26B,H26C), C17(H17A,H17B,H17C), C19(H19A,
 H19B,H19C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C40(H40A,H40B,H40C), C37(H37A,
 H37B,H37C), C27(H27A,H27B,H27C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C16(H16A,
 H16B,H16C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              43784
_shelx_hkl_checksum              79875
_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 1.522
_oxdiff_exptl_absorpt_empirical_full_min 0.788