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_7226105
_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         'C22 H20 N3 O3 V, 0.67(H2 O)'
_chemical_formula_sum            'C22 H21.33 N3 O3.67 V'
_chemical_formula_weight         437.36
_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_method           SHELXL-2014/7
_audit_update_record
;
2016-07-27 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                100.25(3)
_cell_angle_beta                 98.44(3)
_cell_angle_gamma                106.11(3)
_cell_formula_units_Z            12
_cell_length_a                   15.390(3)
_cell_length_b                   17.480(4)
_cell_length_c                   22.770(5)
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.999
_cell_measurement_theta_min      0.929
_cell_volume                     5665(3)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0623
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22234
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         0.929
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    0.560
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       prism
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_refine_diff_density_max         2.995
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1616
_refine_ls_number_reflns         22234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0994P)^2^+9.4564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18937
_reflns_number_total             22234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra12872f2.cif
_cod_data_source_block           1
_cod_original_cell_volume        5665(2)
_cod_database_code               7226105
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              44615