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_1573554
_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         '0.17(C58 H86 Cl Dy N4)'
_chemical_formula_sum            'C10.09 H14.96 Cl0.17 Dy0.17 N0.7'
_chemical_formula_weight         180.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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
;
2024-07-13 deposited with the CCDC.	2024-12-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.235(6)
_cell_angle_gamma                90
_cell_formula_units_Z            23
_cell_length_a                   23.9612(13)
_cell_length_b                   10.5893(4)
_cell_length_c                   22.5423(13)
_cell_measurement_reflns_used    5061
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.8150
_cell_measurement_theta_min      3.6210
_cell_volume                     5294.4(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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.858
_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  87.00   1.00    4.28    --   20.18  57.00-120.00   55
  2  \w     15.00  89.00   1.00    4.28    --   20.18  57.00 -60.00   74
  3  \w     18.00  85.00   1.00    4.28    --   20.18  57.00-180.00   67
  4  \w     24.00  63.00   1.00    4.28    --   20.18 -99.00   0.00   39
;
_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      0.0299867000
_diffrn_orient_matrix_UB_12      -0.0044813000
_diffrn_orient_matrix_UB_13      0.0013466000
_diffrn_orient_matrix_UB_21      0.0109128000
_diffrn_orient_matrix_UB_22      -0.0009301000
_diffrn_orient_matrix_UB_23      0.0339949000
_diffrn_orient_matrix_UB_31      -0.0021237000
_diffrn_orient_matrix_UB_32      -0.0667802000
_diffrn_orient_matrix_UB_33      -0.0005300000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0910
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11961
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.164
_diffrn_reflns_theta_min         3.361
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.502
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39583
_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            colorless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       block
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.085
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         6138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0511P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5280
_reflns_number_total             6138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05982d2.cif
_cod_data_source_block           arepw2045
_cod_depositor_comments
'Adding full bibliography for 1573553--1573561.cif.'
_cod_original_formula_sum        'C10.09 H14.96 Cl0.17 Dy0.17 N0.70'
_cod_database_code               1573554
_shelx_shelxl_version_number     2014/7
_diffrn_oxdiff_digest_frames
;
0176bb3acccc1dc72077f965210714024000028b912
;
_diffrn_oxdiff_digest_hkl
;
01a466f1666b994e0c4f8d4378a403ee277996
;
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C007(H007), C00A(H00A), C00I(H00I), C00L(H00L)
1.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00F(H00F), C00G(H00G), C00N(H00P), C00O(H00Q), C00S(H00Z)
1.c Idealised Me refined as rotating group:
 C00H(H00B,H00C,H00E), C00J(H00H,H00J,H00K), C00M(H00M,H00N,H00O), C00P(H00R,
 H00S,H00T), C00Q(H00U,H00V,H00W), C00R(H00X,H00Y,H), C00T(H00,HA,HB),
 C00U(H0AA,HC,HD), C00V(H1AA,HE,HF), C00W(H2AA,HG,HH), C00X(H3AA,HI,HJ)
;
_shelx_res_checksum              7312
_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 2.408
_oxdiff_exptl_absorpt_empirical_full_min 0.363