Dioxo-vanadium(V), oxo-rhenium(V) and dioxo-uranium(VI) complexes with a tridentate Schiff base ligand
Zhang, Yingjie; Fanna, Daniel; Shepherd, Nicholas D.; Karatchevtseva, Inna; Lu, Kim; Kong, Linggen; Price, Jason R.; RSC Adv.  (2016) –; doi:10.1039/C6RA12872F

data_7226108
_publ_section_title
;
 Dioxo-vanadium(V), oxo-rhenium(V) and dioxo-uranium(VI) complexes with a
 tridentate Schiff base ligand
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA12872F
_journal_year                    2016
_chemical_formula_moiety         'C24 H28 N3 O5 U, C H4 O, N O3'
_chemical_formula_sum            'C25 H32 N4 O9 U'
_chemical_formula_weight         770.57
_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
_audit_creation_date             2016-07-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-27 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.58(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.447(2)
_cell_length_b                   15.650(3)
_cell_length_c                   15.962(3)
_cell_measurement_reflns_used    10000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.902
_cell_measurement_theta_min      1.884
_cell_volume                     2677.0(10)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'ADSC Quantum Detector'
_diffrn_measurement_method       '\p  scans'
_diffrn_radiation_type
'silicon double crystal monochromated synchrotron'
_diffrn_radiation_wavelength     0.71074
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44068
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.901
_diffrn_reflns_theta_min         1.884
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    6.123
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_refine_diff_density_max         3.370
_refine_diff_density_min         -3.251
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6353
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0258P)^2^+26.6349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5689
_reflns_number_total             6353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra12872f2.cif
_cod_data_source_block           complex4
_cod_database_code               7226108
_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, All O(H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 C24-H5
 1.915356 with sigma of 0.02
 U1-H5
 3.059805 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C18) = Uanis(C19) = Uanis(C20)
Uanis(C23) = Uanis(C24)
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C20(H20A,H20B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5A), C6(H6), C7(H7), C10(H10), C12(H12)
4.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
4.d Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_shelx_res_checksum              89621
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'