#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:44:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179260 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/80/4318036.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4318036
loop_
_publ_author_name
'Malgorzata Lipowska'
'Lory Hansen'
'Xiaolong Xu'
'Patricia A. Marzilli'
'Andrew Taylor,'
'Luigi G. Marzilli'
_publ_section_title
;
 New N3S Donor Ligand Small Peptide Analogues of the
 N-Mercaptoacetyl-glycylglycylglycine Ligand in the Clinically Used Tc-99m
 Renal Imaging Agent: Evidence for Unusual Amide Oxygen Coordination by
 Two New Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3032
_journal_page_last               3041
_journal_paper_doi               10.1021/ic011325z
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C8 H15 Cl N3 O6 Re S'
_chemical_formula_weight         502.94
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.771(2)
_cell_length_b                   11.105(2)
_cell_length_c                   16.575(3)
_cell_measurement_temperature    193(2)
_cell_volume                     1403.0(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8761
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    9.028
_exptl_crystal_density_diffrn    2.381
_exptl_crystal_F_000             960
_refine_diff_density_max         1.571
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.00314(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.089
_refine_ls_goodness_of_fit_obs   1.110
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_obs          0.0179
_refine_ls_shift/esd_max         0.035
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0206P)²+0.9023P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0450
_refine_ls_wR_factor_obs         0.0445
_reflns_number_observed          3143
_reflns_number_total             3330
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011325z_2.cif
_cod_data_source_block           Compound11(ReClO(MAEG2H3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+0.9023P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+0.9023P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4318036
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re Re 0.160328(13) 0.131894(9) 0.385890(6) 0.01397(5) Uani 1 d . .
Cl Cl -0.04308(11) 0.28824(7) 0.33050(5) 0.0297(2) Uani 1 d . .
N1 N 0.3271(3) -0.0054(2) 0.38737(15) 0.0167(5) Uani 1 d . .
N2 N 0.3967(3) 0.2319(2) 0.36858(15) 0.0167(4) Uani 1 d . .
H2A H 0.4034(47) 0.2909(35) 0.4006(23) 0.023(9) Uiso 1 d . .
N3 N 0.3132(3) 0.1679(2) 0.15073(15) 0.0192(5) Uani 1 d . .
H3A H 0.3867(50) 0.2132(35) 0.1340(23) 0.026(9) Uiso 1 d . .
O1 O 0.1815(3) 0.1698(2) 0.48529(13) 0.0239(4) Uani 1 d . .
O2 O 0.3704(3) -0.2035(2) 0.36142(13) 0.0226(4) Uani 1 d . .
O3 O 0.1762(3) 0.1193(2) 0.25364(12) 0.0172(4) Uani 1 d . .
O4 O 0.4114(3) 0.1173(2) 0.00619(13) 0.0203(4) Uani 1 d . .
O5 O 0.1985(3) -0.0213(2) -0.0264(2) 0.0325(6) Uani 1 d . .
H5A H 0.2198(85) -0.0230(59) -0.0638(41) 0.084(23) Uiso 1 d . .
O6 O 0.2711(3) -0.0608(2) -0.17118(14) 0.0283(5) Uani 1 d . .
H6A H 0.1854(3) -0.0532(2) -0.20227(14) 0.034 Uiso 1 d R .
H6B H 0.2845(3) -0.1394(2) -0.16507(14) 0.034 Uiso 1 d R .
S S -0.05208(8) -0.01262(6) 0.36204(4) 0.01871(14) Uani 1 d . .
C1 C 0.0867(4) -0.1463(3) 0.3846(2) 0.0211(6) Uani 1 d . .
H1A H 0.0396(4) -0.2101(3) 0.3478(2) 0.025 Uiso 1 d R .
H1B H 0.0863(4) -0.1725(3) 0.4398(2) 0.025 Uiso 1 d R .
C2 C 0.2732(4) -0.1210(2) 0.3761(2) 0.0165(5) Uani 1 d . .
C3 C 0.5062(4) 0.0229(3) 0.3761(2) 0.0211(6) Uani 1 d . .
H3B H 0.5132(4) 0.0152(3) 0.3191(2) 0.025 Uiso 1 d R .
H3C H 0.5888(4) -0.0318(3) 0.4075(2) 0.025 Uiso 1 d R .
C4 C 0.5465(4) 0.1517(3) 0.4044(2) 0.0207(6) Uani 1 d . .
H4A H 0.5652(4) 0.1549(3) 0.4633(2) 0.025 Uiso 1 d R .
H4B H 0.6516(4) 0.1788(3) 0.3877(2) 0.025 Uiso 1 d R .
C5 C 0.3953(4) 0.2707(3) 0.2834(2) 0.0191(5) Uani 1 d . .
H5B H 0.5135(4) 0.2744(3) 0.2734(2) 0.023 Uiso 1 d R .
H5C H 0.3441(4) 0.3494(3) 0.2741(2) 0.023 Uiso 1 d R .
C6 C 0.2889(3) 0.1804(2) 0.2261(2) 0.0158(5) Uani 1 d . .
C7 C 0.2108(4) 0.0804(3) 0.0962(2) 0.0253(6) Uani 1 d . .
H7A H 0.0921(4) 0.1085(3) 0.0804(2) 0.030 Uiso 1 d R .
H7B H 0.2091(4) 0.0054(3) 0.1247(2) 0.030 Uiso 1 d R .
C8 C 0.2867(4) 0.0614(3) 0.0208(2) 0.0193(5) Uani 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Re N1 103.90(11) . . ?
O1 Re N2 94.37(10) . . ?
N1 Re N2 80.32(9) . . ?
O1 Re O3 166.02(9) . . ?
N1 Re O3 78.68(9) . . ?
N2 Re O3 72.36(8) . . ?
O1 Re S 106.04(8) . . ?
N1 Re S 84.89(7) . . ?
N2 Re S 157.19(6) . . ?
O3 Re S 87.82(6) . . ?
O1 Re Cl 97.18(8) . . ?
N1 Re Cl 158.67(7) . . ?
N2 Re Cl 95.09(7) . . ?
O3 Re Cl 80.09(6) . . ?
S Re Cl 92.41(3) . . ?
C2 N1 C3 117.4(2) . . ?
C2 N1 Re 122.7(2) . . ?
C3 N1 Re 117.5(2) . . ?
C5 N2 C4 114.5(2) . . ?
C5 N2 Re 114.8(2) . . ?
C4 N2 Re 104.6(2) . . ?
C6 N3 C7 120.1(2) . . ?
C6 O3 Re 119.9(2) . . ?
C1 S Re 99.06(10) . . ?
C2 C1 S 111.6(2) . . ?
O2 C2 N1 122.9(3) . . ?
O2 C2 C1 120.9(3) . . ?
N1 C2 C1 116.2(2) . . ?
N1 C3 C4 107.7(2) . . ?
N2 C4 C3 109.9(2) . . ?
N2 C5 C6 108.0(2) . . ?
O3 C6 N3 121.9(3) . . ?
O3 C6 C5 117.6(2) . . ?
N3 C6 C5 120.5(2) . . ?
N3 C7 C8 110.9(2) . . ?
O4 C8 O5 125.8(3) . . ?
O4 C8 C7 123.6(3) . . ?
O5 C8 C7 110.6(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re O1 1.677(2) . ?
Re N1 1.999(2) . ?
Re N2 2.213(2) . ?
Re O3 2.224(2) . ?
Re S 2.2808(8) . ?
Re Cl 2.4064(9) . ?
N1 C2 1.352(4) . ?
N1 C3 1.474(3) . ?
N2 C5 1.473(4) . ?
N2 C4 1.494(4) . ?
N3 C6 1.307(4) . ?
N3 C7 1.455(4) . ?
O2 C2 1.241(3) . ?
O3 C6 1.261(3) . ?
O4 C8 1.214(4) . ?
O5 C8 1.309(4) . ?
S C1 1.830(3) . ?
C1 C2 1.510(4) . ?
C3 C4 1.519(4) . ?
C5 C6 1.512(4) . ?
C7 C8 1.498(4) . ?
