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_1573560
_publ_section_title
;
 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 Gd I N4, C7 H8'
_chemical_formula_sum            'C65 H94 Gd I N4'
_chemical_formula_weight         1215.59
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-09
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-13 deposited with the CCDC.	2024-12-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.762(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.171(2)
_cell_length_b                   11.0443(10)
_cell_length_c                   23.940(3)
_cell_measurement_reflns_used    9215
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.353
_cell_measurement_theta_min      2.57
_cell_volume                     6006.9(11)
_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_temperature      150.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38569
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.353
_diffrn_reflns_theta_min         2.050
_exptl_absorpt_coefficient_mu    1.659
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5438
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0272P)^2^+1.4152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4969
_reflns_number_total             5438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05982d2.cif
_cod_data_source_block           1Gd
_cod_depositor_comments
'Adding full bibliography for 1573553--1573561.cif.'
_cod_original_cell_volume        6007.0(11)
_cod_database_code               1573560
_shelx_shelxl_version_number     2018/3
_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:
 C00B(H00B), C00D(H00D), C00F(H00F), C00M(H00M)
6.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00H(H00H), C00J(H00J), C00L(H00L), C00N(H00N), C00Q(H00U),
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
6.c Idealised Me refined as rotating group:
 C00G(H00A,H00C,H00E), C00K(H00G,H00I,H00K), C00O(H00O,H00P,H00Q), C00P(H00R,
 H00S,H00T), C00R(H00V,H00W,H00X), C00S(H00Y,H,HA), C00U(H00,HB,HC), C00V(H1,HD,
 HE), C00W(H2,HF,HG), C00X(H3,HH,HI), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              4691
_olex2_submission_special_instructions 'No special instructions were received'