Rare earth benzene tetraanion-bridged amidinate complexes.
Jin, Peng-Bo; Luo, Qian-Cheng; Gransbury, Gemma K.; Winpenny, Richard E. P.; Mills, David P.; Zheng, Yan-Zhen; Chemical science 16 (2025) 1907–1924; doi:10.1039/d4sc05982d

data_1573555
_publ_section_title
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 Rare earth benzene tetraanion-bridged amidinate complexes.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              1907
_journal_page_last               1924
_journal_paper_doi               10.1039/d4sc05982d
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C58 H86 I N4 Y, C7 H8'
_chemical_formula_sum            'C65 H94 I N4 Y'
_chemical_formula_weight         1147.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-12-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
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2024-07-13 deposited with the CCDC.	2024-12-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.041(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.2282(11)
_cell_length_b                   10.9625(3)
_cell_length_c                   23.8393(9)
_cell_measurement_reflns_used    5749
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.6150
_cell_measurement_theta_min      3.7610
_cell_volume                     5923.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1428
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.843
_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    -90.00   0.00   1.00    3.11    --  -18.62 -37.00 -30.00   90
  2  \w    -80.00 -41.00   1.00    3.11    --  -18.62-178.00   0.00   39
  3  \w     49.00  87.00   1.00    3.11    --   20.34  57.00 -60.00   38
  4  \w     39.00  98.00   1.00    3.11    --   20.34 178.00 -90.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0123715000
_diffrn_orient_matrix_UB_12      -0.0435646000
_diffrn_orient_matrix_UB_13      0.0243352000
_diffrn_orient_matrix_UB_21      0.0136576000
_diffrn_orient_matrix_UB_22      -0.0298184000
_diffrn_orient_matrix_UB_23      -0.0166531000
_diffrn_orient_matrix_UB_31      0.0252797000
_diffrn_orient_matrix_UB_32      0.0374277000
_diffrn_orient_matrix_UB_33      0.0150661000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            12717
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.149
_diffrn_reflns_theta_min         3.405
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6732
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0412P)^2^+7.6212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5596
_reflns_number_total             6732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05982d2.cif
_cod_data_source_block           1Y
_cod_depositor_comments
'Adding full bibliography for 1573553--1573561.cif.'
_cod_original_cell_volume        5923.8(4)
_cod_database_code               1573555
_shelx_shelxl_version_number     2014/7
_diffrn_oxdiff_digest_frames
;
0111b855e93706c385d1061082ebeb423d00029f536
;
_diffrn_oxdiff_digest_hkl
;
010bd161fa7edc520260d8c8c2857bf5338763
;
_reflns_odcompleteness_completeness 99.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 C2-C3
 1.51 with sigma of 0.02
 C3-C4 = C3-C8 = C5-C6
 1.39 with sigma of 0.02
 C4-C5 = C6-C7 = C7-C8
 1.38 with sigma of 0.02
 C2-C4 = C2-C8
 2.52 with sigma of 0.04
 C3-C5
 2.42 with sigma of 0.04
 C3-C7
 2.41 with sigma of 0.04
 C4-C6
 2.39 with sigma of 0.04
 C5-C7 = C6-C8
 2.4 with sigma of 0.04
 C3-C4 \\sim C4-C5 \\sim C5-C6 \\sim C6-C7 \\sim C7-C8 \\sim C8-C3
 with sigma of 0.02
 C3-C7 \\sim C3-C5 \\sim C8-C6 \\sim C4-C8 \\sim C5-C7 \\sim C4-C6
 with sigma of 0.04
 C2-C8 \\sim C2-C4
 with sigma of 0.04
2. Restrained planarity
 C2, C3, C4, C5, C6, C7, C8
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C2, C3, C4, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C3(0.5) C4(0.5) H4(0.5) C5(0.5)
 H5(0.5) C6(0.5) H6(0.5) C7(0.5) H7(0.5) C8(0.5) H8(0.5)
6.a Ternary CH refined with riding coordinates:
 C009(H009), C00G(H00G), C00H(H00H), C00M(H00N)
6.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00C(H00C), C00D(H00D), C00J(H00J), C00K(H00K), C00Q(H00U),
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
6.c Idealised Me refined as rotating group:
 C00I(H00A,H00E,H00F), C00L(H00I,H00L,H00M), C00O(H00O,H00P,H00Q), C00P(H00R,
 H00S,H00T), C00R(H00V,H00W,H00X), C00S(H00Y,H,HA), C00T(H00Z,HB,HC), C00U(H00,
 HD,HE), C00V(H0AA,HF,HG), C00W(H1AA,HH,HI), C00X(H2AA,HJ,HK), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              94587
_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 1.408
_oxdiff_exptl_absorpt_empirical_full_min 0.747