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_7710647
_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_compound_source        'synthetical product'
_chemical_formula_moiety         '3(C6 H14 N4 O6 S2 W2), 4(K2 S4 W), 14(H2 O)'
_chemical_formula_sum            'C18 H70 K8 N12 O32 S22 W10'
_chemical_formula_weight         3823.48
_chemical_name_common
'tris[bis(mu2-sulfido)-bis(2,3-diaminopropionato-N,N',O)-dioxo-di-tungsten(V)]-tetrakis[potassium tetrasulfido-tungsten(VI)]-tetradecaaqua adduct'
_chemical_name_systematic
'tris[bis(mu2-sulfido)-bis(2,3-diaminopropionato-N,N',O)-dioxo-di-tungsten(V)]-tetrakis[potassium tetrasulfido-tungsten(VI)]-tetradecaaqua adduct'
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_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                120
_cell_formula_units_Z            6
_cell_length_a                   18.0697(7)
_cell_length_b                   18.0697(7)
_cell_length_c                   45.2783(18)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.55
_cell_measurement_theta_min      2.63
_cell_volume                     12803.3(9)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -73
_diffrn_reflns_number            48598
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        35.0
_diffrn_reflns_theta_max         35.0
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    14.416
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.349
_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    2.975
_exptl_crystal_description       plate
_exptl_crystal_F_000             10572
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.052
_refine_diff_density_min         -1.799
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         12558
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0128P)^2^+2.6029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11195
_reflns_number_total             12558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01470j2.cif
_cod_data_source_block           HV25B
_cod_original_cell_volume        12803.3(13)
_cod_database_code               7710647
_shelx_estimated_absorpt_t_min   0.098
_shelx_estimated_absorpt_t_max   0.300
_shelxl_version_number           2014/6
_shelx_res_checksum              38510
_shelx_hkl_checksum              44171