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_7039905
_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         '2(C30 H36 N2 O7 U), C H Cl3'
_chemical_formula_sum            'C61 H73 Cl3 N4 O14 U2'
_chemical_formula_weight         1668.64
_chemical_name_common            UO2(Salophen)OMe
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-01
_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                 91.856(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4679(4)
_cell_length_b                   10.7796(5)
_cell_length_c                   30.4674(14)
_cell_measurement_reflns_used    4599
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.454
_cell_measurement_theta_min      2.903
_cell_volume                     3107.9(2)
_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 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.97
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9028
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.499
_diffrn_reflns_theta_min         2.902
_diffrn_source
'Microfocus sealed X-ray tub fitted with HELIOS multilayer optics'
_diffrn_source_target            Cu
_exptl_absorpt_coefficient_mu    17.208
_exptl_absorpt_correction_T_max  0.467166
_exptl_absorpt_correction_T_min  0.210861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1239 before and 0.0517 after correction.
 The Ratio of minimum to maximum transmission is 0.45.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1283 before and 0.0599 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 38731 reflections, Rint = 0.0803
 (19723 with I > 3sig(I), Rint = 0.0669)
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       needle
_exptl_crystal_F_000             1628
_exptl_crystal_recrystallization_method
'Crystallized from CDCl3 in an NMR tube via slow evaporation.'
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.029
_refine_diff_density_max         2.128
_refine_diff_density_min         -4.506
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       0.000066(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         9028
_refine_ls_number_restraints     411
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0063P)^2^+64.1379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8111
_reflns_number_total             9028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02089e2.cif
_cod_data_source_block           kh140_a
_cod_depositor_comments
'Adding full bibliography for 7039904--7039905.cif.'
_cod_database_code               7039905
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5812(12) 0.4188(12)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, H31 of C31, All O(H,H) groups
 At 1.2 times of:
  H3 of C3, H14 of C14, H16 of C16, H15 of C15, H21 of C21, H23 of C23, H5 of
  C5, H17 of C17, H19 of C19, H12 of C12
3. Restrained distances
 H5A-H5B
 1.518 with sigma of 0.02
 O5-H5A
 0.96 with sigma of 0.02
 O5-H5B
 0.96 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C31(0.5) H31(0.5) Cl4(0.5) Cl5(0.5) Cl6(0.5)
7.a Free rotating group:
 C31(H31,Cl4,Cl5,Cl6)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C12(H12), C14(H14), C16(H16), C15(H15),
 C21(H21), C23(H23)
7.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_shelx_res_checksum              21425
_olex2_date_sample_completion    2015-02-18
_olex2_date_sample_data_collection 2015-02-18
_olex2_date_sample_submission    2015-02-18
_olex2_exptl_crystal_mounting_method
'MiTeGen dual-thickness MicroMounts using parabar oil'
_olex2_submission_original_sample_id KH_1_40
_olex2_submission_special_instructions 'No special instructions were received'