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_4336701
_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            'C33 H33 O4 P2 Re'
_chemical_formula_weight         741.73
_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                90.0000(10)
_cell_angle_beta                 104.730(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.7703(4)
_cell_length_b                   9.1874(1)
_cell_length_c                   16.2740(3)
_cell_measurement_reflns_used    20867
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.94
_cell_measurement_theta_min      7.30
_cell_volume                     3148.03(9)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20253
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         7.30
_exptl_absorpt_coefficient_mu    8.788
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.341
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            light-green
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.856
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00067(4)
_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   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+2.7469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0565
_reflns_number_gt                2520
_reflns_number_total             2570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401503b_si_002_4.cif
_cod_data_source_block           compound7
_cod_database_code               4336701