Actinide arene-metalates: 2. A neutral uranium bis(anthracenide) sandwich complex and elucidation of its electronic structure
Murillo, Jesse; Bhowmick, Rina; Harriman, Katie L. M.; Gomez-Torres, Alejandra; Wright, Joshua; Miró, Pere; Metta-Magaña, Alejandro; Murugesu, Muralee; Vlaisavljevich, Bess; Fortier, Skye; Chemical Communications  (2022) –; doi:10.1039/D2CC03238D

data_7130400
_publ_section_title
;
 Actinide arene-metalates: 2. A neutral uranium bis(anthracenide) sandwich
 complex and elucidation of its electronic structure
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03238D
_journal_year                    2022
_chemical_formula_moiety         'C40 H57 N6 O2 P2 U, C4 H8 O'
_chemical_formula_sum            'C44 H65 N6 O3 P2 U'
_chemical_formula_weight         1025.99
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-11 deposited with the CCDC.	2022-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                89.209(2)
_cell_angle_beta                 73.340(2)
_cell_angle_gamma                67.677(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1073(17)
_cell_length_b                   12.4112(19)
_cell_length_c                   17.777(3)
_cell_measurement_reflns_used    7740
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.88
_cell_measurement_theta_min      2.23
_cell_volume                     2159.3(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20892
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.140
_diffrn_reflns_theta_min         1.203
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.879
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0789 before and 0.0436 after correction. The Ratio of minimum to maximum transmission is 0.7334. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             1034
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.370
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0326P)^2^+1.9268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7400
_reflns_number_total             8466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03238d2.cif
_cod_data_source_block           1_THF
_cod_database_code               7130400
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.698
_shelx_estimated_absorpt_t_min   0.594
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N006(H006), C002(H002), C009(H009), C015(H015), C016(H016), C023(H023),
 C024(H024)
2.b Secondary CH2 refined with riding coordinates:
 C042(H04D,H04E), C043(H04F,H04G), C044(H04H,H04I), C045(H04J,H04K)
2.c Aromatic/amide H refined with riding coordinates:
 C008(H008), C010(H010), C011(H011), C013(H013), C017(H017), C018(H018),
 C021(H021), C026(H026), C028(H028), C030(H030), C033(H033), C036(H036),
 C037(H037), C040(H040)
2.d Idealised Me refined as rotating group:
 C012(H01A,H01B,H01C), C014(H01D,H01E,H01F), C025(H02A,H02B,H02C), C027(H02D,
 H02E,H02F), C029(H02G,H02H,H02I), C031(H03A,H03B,H03C), C032(H03D,H03E,H03F),
 C034(H03G,H03H,H03I), C035(H03J,H03K,H03L), C038(H03M,H03N,H03O), C039(H03P,
 H03Q,H03R), C041(H04A,H04B,H04C)
;
_shelx_res_checksum              7508
_olex2_submission_special_instructions 'No special instructions were received'