Re(CO)3 Complexes Synthesized via an Improved Preparation of Aqueous fac-[Re(CO)3(H2O)3]+ as an Aid in Assessing 99mTc Imaging Agents. Structural Characterization and Solution Behavior of Complexes with Thioether-Bearing Amino Acids as Tridentate Ligands
Haiyang He; Malgorzata Lipowska; Xiaolong Xu; Andrew T. Taylor; Maria Carlone; Luigi G. Marzilli; Inorganic Chemistry 44 (2005) 5437–5446; doi:10.1021/ic0501869

data_4309257
_publ_contact_author_address
;
Emory University
Department of Chemistry
X-ray Crystallography Laboratory
Atlanta GA 30322-2210
USA
;
_publ_contact_author_email       khardca@emory.edu
_publ_contact_author_fax         404-727-6586
_publ_contact_author_name        'Kenneth I. Hardcastle'
_publ_contact_author_phone       404-727-6140
_publ_section_title
;
Re(CO)3 Complexes Synthesized via an Improved Preparation of
Aqueous fac-[Re(CO)3(H2O)3]+ as an Aid in Assessing 99mTc Imaging Agents.
Structural Characterization and Solution Behavior of Complexes with
Thioether-Bearing Amino Acids as Tridentate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5437
_journal_page_last               5446
_journal_paper_doi               10.1021/ic0501869
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '[C8 H8 N O7 Re S]2, [H2 O]'
_chemical_formula_sum            'C16 H18 N2 O15 Re2 S2'
_chemical_formula_weight         914.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 100.343(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6341(12)
_cell_length_b                   8.0536(7)
_cell_length_c                   23.669(2)
_cell_measurement_reflns_used    4364
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.60
_cell_measurement_theta_min      3.80
_cell_volume                     2369.2(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.876
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0786
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            4776
_diffrn_reflns_theta_full        65.76
_diffrn_reflns_theta_max         65.76
_diffrn_reflns_theta_min         3.80
_exptl_absorpt_coefficient_mu    22.066
_exptl_absorpt_correction_T_max  0.4723
_exptl_absorpt_correction_T_min  0.1365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10, Sheldrick 2003'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.094
_refine_diff_density_min         -2.943
_refine_diff_density_rms         0.339
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2838
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                2718
_reflns_number_total             2838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0501869si20050418_102502_1.cif
_cod_data_source_block           5B
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2369.1(4)
_cod_database_code               4309257