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_7226107
_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
'2(C22 H24 N3 O5 U 1+), C22 H20 N3 O, 2(N O3 1-), 4(H2 O)'
_chemical_formula_sum            'C66 H76 N11 O21 U2'
_chemical_formula_weight         1835.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-07-23
_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                105.45(3)
_cell_angle_beta                 113.33(3)
_cell_angle_gamma                90.57(3)
_cell_formula_units_Z            2
_cell_length_a                   15.416(3)
_cell_length_b                   15.959(3)
_cell_length_c                   16.435(3)
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.925
_cell_measurement_theta_min      1.335
_cell_volume                     3548.1(16)
_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 0.931
_diffrn_measured_fraction_theta_max 0.916
_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  0.0746
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60448
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.925
_diffrn_reflns_theta_min         1.335
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    4.639
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       prism
_exptl_crystal_F_000             1802
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.728
_refine_diff_density_min         -2.045
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       0.0060(2)
_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   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         15564
_refine_ls_number_restraints     947
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0596P)^2^+11.1362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11059
_reflns_number_total             15564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra12872f2.cif
_cod_data_source_block           complex3
_cod_original_cell_volume        3548.2(15)
_cod_database_code               7226107
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 N2N-O1N2
 1.26 with sigma of 0.02
 N2N-O2N2
 1.26 with sigma of 0.02
 N2N-O3N2
 1.26 with sigma of 0.02
 O1N3-N3N = O2N3-N3N = O3N3-N3N
 1.27 with sigma of 0.02
 C62A-C61A \\sim C62B-C61B \\sim C63-C62A \\sim C63-C62B
 with sigma of 0.02
3. Restrained planarity
 O1N2, O2N2, O3N2, N2N
 with sigma of 0.1
 O3N3, N3N, O1N3, O2N3
 with sigma of 0.1
4. 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
5. Others
 Fixed Sof: C61A(0.5) H61A(0.5) H61B(0.5) C61B(0.5) H61C(0.5) H61D(0.5)
 C62A(0.5) H62A(0.5) H62B(0.5) C62B(0.5) H62C(0.5) H62D(0.5) H63A(0.5)
 H63B(0.5) O1N2(0.5) O2N2(0.5) O3N2(0.5) N2N(0.5) O7W(0.5) O9W(0.5) O8W(0.5)
 O10W(0.3) O3N3(0.5) N3N(0.5) O1N3(0.5) O12W(0.2) O2N3(0.5)
6.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O6W(H6WA,H6WB)
6.b Free rotating group:
 O5W(H5WA,H5WB)
6.c Rotating group:
 O3W(H3WA,H3WB), O4W(H4WA,H4WB)
6.d Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
 H18B), C19(H19A,H19B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C58(H58A,H58B), C59(H59A,H59B),
  C60(H60A,H60B), C61A(H61A,H61B), C61B(H61C,H61D), C62A(H62A,H62B), C62B(H62C,
 H62D), C63(H63A,H63B)
6.e Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C23(H23),
 C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C32(H32), C34(H34), C45(H45),
  C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C54(H54), C56(H56)
6.f Idealised tetrahedral OH refined as rotating group:
 O7(H7A)
;
_shelx_res_checksum              85841
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'