Synthesis and comparison of iso-structural f-block metal complexes (Ce, U, Np, Pu) featuring <i>η</i><sup>6</sup>-arene interactions.
Murillo, Jesse; Goodwin, Conrad A. P.; Stevens, Lauren; Fortier, Skye; Gaunt, Andrew J.; Scott, Brian L.; Chemical science 14 (2023) 7438–7446; doi:10.1039/d3sc02194g

data_1569302
_publ_section_title
;
 Synthesis and comparison of iso-structural f-block metal complexes (Ce,
 U, Np, Pu) featuring <i>&#x3b7;</i><sup>6</sup>-arene interactions.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              7438
_journal_page_last               7446
_journal_paper_doi               10.1039/d3sc02194g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C50 H65.73 Cl2 K N2 O2 U'
_chemical_formula_sum            'C50 H65.73 Cl2 K N2 O2 U'
_chemical_formula_weight         1074.80
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.263(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3428(16)
_cell_length_b                   16.9863(19)
_cell_length_c                   25.645(3)
_cell_measurement_reflns_used    9442
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.84
_cell_volume                     5810.9(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_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  0.0336
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34546
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.652
_diffrn_reflns_theta_min         1.941
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.989
_exptl_absorpt_correction_T_max  0.746072
_exptl_absorpt_correction_T_min  0.605955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 266824 reflections, Rint = 0.0591
 (103563 with I > 3sig(I), Rint = 0.0384)
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       block
_exptl_crystal_F_000             2163
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.350
_refine_diff_density_min         -2.759
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         17753
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0001P)^2^+22.0423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14382
_reflns_number_total             17753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02194g2.cif
_cod_data_source_block           2_U
_cod_depositor_comments
'Adding full bibliography for 1569298--1569306.cif.'
_cod_original_cell_volume        5811.0(11)
_cod_database_code               1569302
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.467
_shelx_estimated_absorpt_t_min   0.381
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O010-C01M \\sim O010-C7
 with sigma of 0.02
 C7-C13 \\sim C01M-C01K
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C13 \\sim C01K: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C7 \\sim C01M: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
4. Others
 Sof(C3AA)=Sof(H3AB)=Sof(H3AC)=Sof(H3AD)=1-FVAR(1)
 Sof(C01I)=Sof(H0AA)=Sof(HE)=Sof(HF)=FVAR(1)
 Sof(C4AA)=Sof(H4AB)=Sof(H4AC)=Sof(H4AD)=1-FVAR(2)
 Sof(H00Q)=Sof(C01J)=Sof(H1AA)=Sof(HG)=Sof(HH)=FVAR(2)
 Sof(C01M)=Sof(H4AA)=Sof(HL)=1-FVAR(3)
 Sof(C7)=Sof(H7A)=Sof(H7B)=FVAR(3)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=1-FVAR(4)
 Sof(C01K)=Sof(H2AA)=Sof(HI)=Sof(HJ)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C00U(H00U), C00X(H00X), C01E(H01W)
5.b Secondary CH2 refined with riding coordinates:
 C016(H01D,H01E), C01D(H01U,H01V), C01L(H3AA,HK), C01M(H4AA,HL), C7(H7A,H7B)
5.c Aromatic/amide H refined with riding coordinates:
 C008(H008), C009(H009), C00D(H00D), C00G(H00G), C00N(H00N), C00O(H00O),
 C00P(H00P), C00R(H00R), C00T(H00T), C00V(H00V), C00W(H00W), C00Y(H00Y),
 C00Z(H00Z), C011(H011), C013(H013), C014(H014), C015(H015), C018(H018)
5.d Idealised Me refined as rotating group:
 C012(H01A,H01B,H01C), C017(H01F,H01G,H01H), C019(H01I,H01J,H01K), C01A(H01L,
 H01M,H01N), C01B(H01O,H01P,H01Q), C01C(H01R,H01S,H01T), C01F(H01X,H01Y,H),
 C01G(H01Z,HA,HB), C01H(H01,HC,HD), C01I(H0AA,HE,HF), C01J(H1AA,HG,HH),
 C01K(H2AA,HI,HJ), C4AA(H4AB,H4AC,H4AD), C3AA(H3AB,H3AC,H3AD), C13(H13A,H13B,
 H13C)
;
_shelx_res_checksum              85496
_shelx_fab_checksum              33190
_olex2_submission_special_instructions 'No special instructions were received'