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_7226106
_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(C44 H40 N6 O3 Re 1+), Cl6 Re 2-, 7(C3 H7 N O)'
_chemical_formula_sum            'C109 H127 Cl6 N19 O13 Re3'
_chemical_formula_weight         2682.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.838(3)
_cell_length_b                   20.449(4)
_cell_length_c                   31.770(6)
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.929
_cell_measurement_theta_min      1.282
_cell_volume                     10939(4)
_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 0.981
_diffrn_measured_fraction_theta_max 0.974
_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  0.1491
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            183663
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.929
_diffrn_reflns_theta_min         1.282
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    3.528
_exptl_absorpt_correction_T_max  0.4308
_exptl_absorpt_correction_T_min  0.3479
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       prism
_exptl_crystal_F_000             5380
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.445
_refine_diff_density_min         -1.951
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       0.00134(5)
_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   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         12773
_refine_ls_number_restraints     642
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+23.4019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9073
_reflns_number_total             12773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra12872f2.cif
_cod_data_source_block           complex2_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_database_code               7226106
_exptl_absorpt_special_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1056 before and 0.0657 after correction.
The Ratio of minimum to maximum transmission is 0.8076.
The \l/2 correction factor is 0.0015.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C15A-C14B \\sim C15B-C14A
 with sigma of 0.02
 C16-C15B \\sim C16-C15A
 with sigma of 0.02
 C14B-C13 \\sim C14A-C13
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C14B) = Uanis(C14A)
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: C14B(0.5) H14A(0.5) H14B(0.5) C15A(0.5) H15A(0.5) H15B(0.5)
 C15B(0.5) H15C(0.5) H15D(0.5) H16A(0.5) H16B(0.5) H16C(0.5) H16D(0.5)
 C14A(0.5) H14C(0.5) H14D(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C14B(H14A,H14B), C15A(H15A,H15B), C15B(H15C,H15D), C16(H16A,H16B), C16(H16C,
 H16D), 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),
  C14A(H14C,H14D)
6.b 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), C3W(H3W),
  C9W(H9W), C6W(H6W)
6.c Idealised Me refined as rotating group:
 C4W(H4WA,H4WB,H4WC), C1W(H1WA,H1WB,H1WC), C2W(H2WA,H2WB,H2WC), C7W(H7WA,H7WB,
 H7WC), C8W(H8WA,H8WB,H8WC), C5W(H5WA,H5WB,H5WC)
;
_shelx_res_checksum              33414
_shelx_fab_checksum              89237
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'