Synthesis, characterization, properties and structures of rhenium-(ii), -(iii), and -(v) complexes containing amino acids conjugated with a 2-aminothiazole ligand
Lazzaro, Antonio; Vertuani, Gianni; Bergamini, Paola; Mantovani, Nicoletta; Marchi, Andrea; Marvelli, Lorenza; Rossi, Roberto; Bertolasi, Valerio; Ferretti, Valeria; Journal of the Chemical Society, Dalton Transactions  (2002) 2843–; doi:10.1039/b201609p

data_7011566
_publ_section_title
;
 Synthesis, characterization, properties and structures of
 rhenium-(ii), -(iii), and -(v) complexes containing amino acids
 conjugated with a 2-aminothiazole ligand
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2843
_journal_paper_doi               10.1039/b201609p
_journal_year                    2002
_chemical_formula_moiety         'C56 H56 N6 O9 P2 Re2 S2'
_chemical_formula_sum            'C56 H56 N6 O9 P2 Re2 S2'
_chemical_formula_weight         1455.53
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9495(4)
_cell_length_b                   17.8488(5)
_cell_length_c                   21.3756(3)
_cell_measurement_reflns_used    15529
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.36
_cell_volume                     5703.7(2)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa CCD server software (Nonius, 1997)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'ORTEP II (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92(Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15529
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    4.430
_exptl_absorpt_correction_T_max  0.661
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SORTAV (R. H. Blessing, Acta Crystallogr., 1995, A51, 33)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.183
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.402(14)
_refine_ls_extinction_coef       0.00106(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         8629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+11.6278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1103
_reflns_number_gt                7129
_reflns_number_total             8629
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b201609p.txt
_cod_data_source_block           (14)
_cod_original_cell_volume        5703.6(2)
_cod_database_code               7011566