Synthesis and electronic structure determination of uranium(vi) ligand radical complexes.
Herasymchuk, Khrystyna; Chiang, Linus; Hayes, Cassandra E.; Brown, Matthew L.; Ovens, Jeffrey S.; Patrick, Brian O.; Leznoff, Daniel B.; Storr, Tim; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12576–12586; doi:10.1039/c6dt02089e

data_7039904
_publ_section_title
;
 Synthesis and electronic structure determination of uranium(vi) ligand
 radical complexes.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12576
_journal_page_last               12586
_journal_paper_doi               10.1039/c6dt02089e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C36 H48 N2 O5 U, 0.5(C1 H4 O)'
_chemical_formula_sum            'C36.5 H50 N2 O5.5 U'
_chemical_formula_weight         842.81
_chemical_name_common            UO2(Salophen)tBu
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-20 deposited with the CCDC.
2016-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.9744(6)
_cell_length_b                   17.1766(7)
_cell_length_c                   34.6304(13)
_cell_measurement_reflns_used    9734
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      70.08
_cell_measurement_theta_min      3.83
_cell_volume                     7717.6(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics
'Olex2 (Dolomanov et al., 2009), ShelXle (H\"ubschle et al., 2011)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7065
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.236
_diffrn_reflns_theta_min         2.552
_diffrn_source
'Microfocus sealed X-ray tub fitted with HELIOS multilayer optics'
_diffrn_source_target            Cu
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.163
_exptl_absorpt_correction_T_max  0.753396
_exptl_absorpt_correction_T_min  0.256267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 2:
 wR2(int) was 0.1787 before and 0.1339 after correction.
 The Ratio of minimum to maximum transmission is 0.34.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 196361 reflections, Rint = 0.1060
 (79939 with I > 3sig(I), Rint = 0.0898)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       prism
_exptl_crystal_F_000             3352
_exptl_crystal_recrystallization_method
'Crystallized via slow evaporation from methanol'
_exptl_crystal_size_max          0.738
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.164
_refine_diff_density_max         4.815
_refine_diff_density_min         -2.866
_refine_diff_density_rms         0.226
_refine_ls_extinction_coef       0.000052(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7065
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1373P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1896
_refine_ls_wR_factor_ref         0.1937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5124
_reflns_number_total             7065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02089e2.cif
_cod_data_source_block           twin4_a
_cod_depositor_comments
'Adding full bibliography for 7039904--7039905.cif.'
_cod_original_formula_sum        'C36.50 H50 N2 O5.50 U'
_cod_database_code               7039904
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1 0
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Rigid body (RIGU) restrains
 C24, C35, C34, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C25, C26, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Rotating group:
 O5(H5A,H5B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C18(H18),
 C20(H20)
4.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              12386
_shelx_fab_checksum              70797
_olex2_exptl_crystal_mounting_method
'MiTeGen dual-thickness MicroMounts using parabar oil'
_olex2_submission_special_instructions 'No special instructions were received'