Effect of the triphenylphosphonium cation on the biological properties of new rhenium and technetium-99m fac-[M(CO)3(NSN)]±-type complexes: Synthesis, structural characterization, in vitro and in vivo studies
Kyriazopoulos, Achilleas; Alexiou, Aikaterini-Lamprini; Miliotou, Androulla; Papadopoulou, Lefkothea; Hatzidimitriou, Antonios; Papagiannopoulou, Dionysia; Inorganica Chimica Acta 511 (2020) 119807–; doi:10.1016/j.ica.2020.119807

data_1564169
_publ_section_title
;
 Effect of the triphenylphosphonium cation on the biological properties of
 new rhenium and technetium-99m fac-[M(CO)3(NSN)]+--type complexes:
 Synthesis, structural characterization, in vitro and in vivo studies
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119807
_journal_paper_doi               10.1016/j.ica.2020.119807
_journal_volume                  511
_journal_year                    2020
_chemical_absolute_configuration .
_chemical_formula_moiety         'C13 H13 N3 O3 Re S, N O3, 0.5(C3 H8 O)'
_chemical_formula_sum            'C14.5 H17 N4 O6.5 Re S'
_chemical_formula_weight         569.58
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                70.130(3)
_cell_angle_beta                 84.944(3)
_cell_angle_gamma                78.415(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4875(5)
_cell_length_b                   10.6929(6)
_cell_length_c                   12.8734(8)
_cell_measurement_reflns_used    217
_cell_measurement_temperature    295
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     1076.15(11)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            69598
_diffrn_reflns_theta_full        31.039
_diffrn_reflns_theta_max         35.677
_diffrn_reflns_theta_min         2.060
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.780
_exptl_absorpt_correction_T_max  0.51
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.115
_refine_diff_density_max         2.60
_refine_diff_density_min         -0.86
_refine_ls_goodness_of_fit_ref   0.9999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         6989
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.0003798
_refine_ls_shift/su_mean         0.0000171
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 2.05 2.65 0.996 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0818
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0760
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                6989
_reflns_number_total             9583
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            ICA-2020-511-119807.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the built-in table derived from the CIF
Core dictionary named 'cif_core.dic' version 2.4.5 last updated on
2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C14.50 H17 N4 O6.50 Re1 S1'
_cod_database_code               1564169