New strategies towards advanced CT contrast agents. Development of neutral and monoanionic sulfur-bridged W(V) dimeric complexes
Varbanov, Hristo Plamenov; Glasnov, Toma N.; Belaj, Ferdinand; Herbert, Simon; Brumby, Thomas; Moesch-Zanetti, Nadia Carmen; Dalton Transactions  (2022) –; doi:10.1039/D2DT01470J

data_7710646
_publ_section_title
;
 New strategies towards advanced CT contrast agents. Development of
 neutral and monoanionic sulfur-bridged W(V) dimeric complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01470J
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         '6(C12 H16 N6 O6 S2 W2), 17(H2 O)'
_chemical_formula_sum            'C72 H130 N36 O53 S12 W12'
_chemical_formula_weight         4939.03
_chemical_name_common
'bis(mu2-sulfido)-bis(L-histidinato-O,N,N')-dioxo-di-tungsten(V) hydrate (6:17)'
_chemical_name_systematic
'bis(mu2-sulfido)-bis(S-2-amino-3-(1H-imidazol-4-yl)propanoato-O,N,N')-dioxo-di-tungsten(V) hydrate (6:17)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'
_audit_update_record
;
2022-03-19 deposited with the CCDC.	2022-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0553(5)
_cell_length_b                   31.7945(16)
_cell_length_c                   39.5192(19)
_cell_measurement_reflns_used    9173
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.48
_cell_measurement_theta_min      2.40
_cell_volume                     12634.4(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0820
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            49623
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    11.173
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.597
_exptl_crystal_description       plate
_exptl_crystal_F_000             9272
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.213
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.231
_refine_ls_abs_structure_details
;
 Flack x determined using 7154 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1531
_refine_ls_number_reflns         21953
_refine_ls_number_restraints     380
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0008P)^2^+2.6043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0636
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                18585
_reflns_number_total             21953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01470j2.cif
_cod_data_source_block           HV22
_cod_database_code               7710646
_shelx_estimated_absorpt_t_min   0.347
_shelx_estimated_absorpt_t_max   0.730
_shelxl_version_number           2014/6
_shelx_res_checksum              99828
_shelx_hkl_checksum              6040