Synthesis and Characterization of fac-[M(CO)3(P)(OO)] and cis-trans-[M(CO)2(P)2(OO)] Complexes (M = Re,99mTc) with Acetylacetone and Curcumin as OO Donor Bidentate Ligands
Charalampos Triantis; Theodoros Tsotakos; Charalampos Tsoukalas; Marina Sagnou; Catherine Raptopoulou; Aris Terzis; Vassilis Psycharis; Maria Pelecanou; Ioannis Pirmettis; Minas Papadopoulos; Inorganic Chemistry 52 (2013) 12995–13003; doi:10.1021/ic401503b

data_4336702
_publ_section_title
;
 Synthesis and Characterization of fac-[M(CO)3(P)(OO)] and
 cis-trans-[M(CO)2(P)2(OO)] Complexes (M = Re,99mTc) with Acetylacetone
 and Curcumin as OO Donor Bidentate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12995
_journal_page_last               13003
_journal_paper_doi               10.1021/ic401503b
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C76 H74 O10 P2 Re'
_chemical_formula_weight         1395.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 112.1270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.7881(4)
_cell_length_b                   9.14860(10)
_cell_length_c                   30.0583(6)
_cell_measurement_reflns_used    22476
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      71.95
_cell_measurement_theta_min      6.55
_cell_volume                     6823.96(19)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q 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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            24043
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         64.99
_diffrn_reflns_theta_min         6.55
_exptl_absorpt_coefficient_mu    4.389
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2860
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.427
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         5619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+24.3789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                5468
_reflns_number_total             5619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401503b_si_002_5.cif
_cod_data_source_block           compound8
_cod_database_code               4336702