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_1573561
_publ_section_title
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 Rare earth benzene tetraanion-bridged amidinate complexes.
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_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         'C64 H92 Gd2 N4'
_chemical_formula_sum            'C64 H92 Gd2 N4'
_chemical_formula_weight         1231.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-09
_audit_creation_method
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Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
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_audit_update_record
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2024-11-13 deposited with the CCDC.	2024-12-24 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.1193(11)
_cell_length_b                   35.666(2)
_cell_length_c                   36.498(3)
_cell_measurement_reflns_used    9215
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.57
_cell_volume                     23587(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0795
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            294771
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.351
_diffrn_reflns_theta_min         2.026
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.271
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6672
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1554 before and 0.0630 after correction.
The Ratio of minimum to maximum transmission is 0.8953.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             10112
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.930
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1353
_refine_ls_number_reflns         21523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+31.6184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18209
_reflns_number_total             21523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05982d2.cif
_cod_data_source_block           2Gd
_cod_depositor_comments
'Adding full bibliography for 1573553--1573561.cif.'
_cod_database_code               1573561
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C01C(H01P), C01I(H01I), C01M(H01M), C01Q(H01Q), C01U(H01U), C021(H021),
 C023(H023), C027(H027), C02A(H02Z), C02I(H8), C02N(H12), C02Q(H02Q),
 C02T(H02T), C02X(H17), C03A(H24), C03N(H03)
1.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00W(H00W), C00Z(H00Z), C011(H011), C016(H016), C017(H017),
 C01B(H01O), C01E(H01E), C01H(H01H), C01L(H01W), C01N(H01N), C01R(H01R),
 C01T(H01T), C025(H025), C02H(H7), C02J(H9), C02K(H02K), C02L(H10), C02M(H11),
 C02W(H16), C031(H031), C03M(H03Z), C03P(H1), C03R(H2)
1.c Idealised Me refined as rotating group:
 C01P(H01A,H01B,H01C), C01W(H01D,H01F,H01G), C01X(H01J,H01K,H01L), C022(H02V,
 H02W,H02X), C029(H02Y,H,HA), C02B(H02,HB,HC), C02C(H02A,H02B,H02C), C02E(H02D,
 H02E,H02F), C02F(H02G,H02H,H02I), C02O(H13,HD,HE), C02P(H02J,H02L,H02M),
 C02R(H02N,H02O,H02P), C02S(H14,HF,HG), C02U(H02R,H02S,H02U), C02V(H15,HH,HI),
 C02Y(H18,HJ,HK), C02Z(H19,HL,HM), C030(H20,HN,HO), C032(H21,HP,HQ), C033(H22,
 HR,HS), C034(H03A,H03B,H03C), C035(H03D,H03E,H03F), C036(H23,HT,HU), C037(H03G,
 H03H,H03I), C038(H03J,H03K,H03L), C039(H03M,H03N,H03O), C03B(H25,HV,HW),
 C03C(H26,HX,HY), C03D(H27,HZ,H35), C03E(H03P,H03Q,H03R), C03F(H03S,H03T,H03U),
 C03G(H28,H36,H37), C03H(H29,H38,H39), C03I(H30,H40,H41), C03J(H03V,H03W,H03X),
 C03K(H03Y,H42,H43), C03L(H31,H44,H45), C03O(H32,H46,H47), C03Q(H33,H48,H49),
 C03S(H3,H50,H51), C03T(H34,H52,H53), C03U(H4,H54,H55), C03V(H5,H56,H57),
 C03W(H6,H58,H59)
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_shelx_res_checksum              52529
_olex2_submission_special_instructions 'No special instructions were received'