Structure and Properties of fac-[Re(I)(CO)3(NTA)](2-) (NTA(3-) = Trianion of Nitrilotriacetic Acid) and fac-[Re(I)(CO)3(L)](n-) Analogues Useful for Assessing the Excellent Renal Clearance of the fac-[(99m)Tc(I)(CO)3(NTA)](2-) Diagnostic Renal Agent.
Klenc, Jeffrey; Lipowska, Malgorzata; Abhayawardhana, Pramuditha L.; Taylor, Andrew T.; Marzilli, Luigi G.; Inorganic chemistry 54 (2015) 6281–6290; doi:10.1021/acs.inorgchem.5b00584

data_4343336
_publ_section_title
;
 Structure and Properties of fac-[Re(I)(CO)3(NTA)](2-) (NTA(3-) = Trianion
 of Nitrilotriacetic Acid) and fac-[Re(I)(CO)3(L)](n-) Analogues Useful
 for Assessing the Excellent Renal Clearance of the
 fac-[(99m)Tc(I)(CO)3(NTA)](2-) Diagnostic Renal Agent.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6281
_journal_page_last               6290
_journal_paper_doi               10.1021/acs.inorgchem.5b00584
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C10 H9 N O9 Re, 2(H2 O), C8 H20 N'
_chemical_formula_sum            'C18 H33 N2 O11 Re'
_chemical_formula_weight         639.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 92.8469(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4535(5)
_cell_length_b                   10.0859(5)
_cell_length_c                   12.7840(7)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      67.95
_cell_measurement_theta_min      3.46
_cell_volume                     1217.41(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.1-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type
'Bruker D8 diffractometer with APEX2 detector'
_diffrn_measurement_method       '\f and \w scans with a narrow frame width'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_laue_measured_fraction_full 0.971
_diffrn_reflns_laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_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            14416
_diffrn_reflns_point_group_measured_fraction_full 0.864
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.141
_diffrn_reflns_theta_min         5.688
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    10.273
_exptl_absorpt_correction_T_max  0.4214
_exptl_absorpt_correction_T_min  0.3061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_description       prism
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1531 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.046(5)
_refine_ls_extinction_coef       0.00591(18)
_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   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         3823
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+0.3283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0404
_refine_ls_wR_factor_ref         0.0404
_reflns_Friedel_coverage         0.673
_reflns_friedel_fraction_full    0.743
_reflns_friedel_fraction_max     0.737
_reflns_number_gt                3820
_reflns_number_total             3823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00584_si_005.cif
_cod_data_source_block           ndap
_cod_depositor_comments
'Adding full bibliography for 4343336--4343339.cif.'
_cod_database_code               4343336
_shelxl_version_number           2014/6