Metal-Assisted In Situ Formation of a Tridentate Acetylacetone Ligand for Complexation of fac-Re(CO)3+ for Radiopharmaceutical Applications
Paul D. Benny; Glenn A. Fugate; Adam O. Barden; Jennifer E. Morley; Elsa Silva-Lopez; Brendan Twamley; Inorganic Chemistry 47 (2008) 2240–2242; doi:10.1021/ic701996e

data_4304498
_publ_contact_author_address
;University Research Office
University of Idaho
Moscow, 
ID 83844-3010
USA
;
_publ_contact_author_email       btwamley@uidaho.edu
_publ_contact_author_fax         '208 885 5752'
_publ_contact_author_name        'Brendan Twamley'
_publ_contact_author_phone       '208 885 2847'
_publ_section_title
;
Metal-Assisted In Situ Formation of a Tridentate Acetylacetone Ligand for
Complexation of fac-Re(CO)3+ for Radiopharmaceutical Applications
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2240
_journal_page_last               2242
_journal_paper_doi               10.1021/ic701996e
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C10.5 H11 Br Cl N2 O3 Re'
_chemical_formula_weight         514.77
_chemical_name_common            'C10 H10 Br N2 O3 Re, 0.5 CH2Cl2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 103.563(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.129(4)
_cell_length_b                   9.2109(16)
_cell_length_c                   12.832(2)
_cell_measurement_reflns_used    6851
_cell_measurement_temperature    89(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.36
_cell_volume                     2887.3(8)
_computing_cell_refinement       'Bruker SAINT+ v. 6.45a'
_computing_data_collection       'Bruker SMART v. 5.630'
_computing_data_reduction        'Bruker SAINT+ v. 6.45a'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 6.12'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 6.12'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 6.12'
_computing_structure_solution    'XS, Bruker SHELXTL v. 6.12'
_diffrn_ambient_temperature      89(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker/Siemens SMART APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21452
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.36
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.372
_exptl_absorpt_correction_T_max  0.359
_exptl_absorpt_correction_T_min  0.221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2001'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.480
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0193
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+6.6121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0490
_reflns_number_gt                2476
_reflns_number_total             2613
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic701996e-file001_1.cif
_cod_data_source_block           4
_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_formula_sum        'C10.50 H11 Br Cl N2 O3 Re'
_cod_database_code               4304498