#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:44:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179260 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/80/4318037.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_4318037
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_moiety         '[C16H24N6O10Re2S2].2H2O'
_chemical_formula_sum            'C16 H28 N6 O12 Re2 S2'
_chemical_formula_weight         932.96
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.243(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7978(17)
_cell_length_b                   10.526(2)
_cell_length_c                   13.427(3)
_cell_measurement_reflns_used    9715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.01
_cell_measurement_theta_min      2.66
_cell_volume                     1238.2(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21042
_diffrn_reflns_theta_full        33.00
_diffrn_reflns_theta_max         33.00
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    10.010
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.739347
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.502
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.245
_refine_diff_density_min         -3.213
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         4446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.285
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0500P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                3883
_reflns_number_total             4446
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011325z_3.cif
_cod_data_source_block           '[ReO(MECG2H2)]2(compound#12)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318037
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.23414(2) 0.239477(19) 1.066811(15) 0.01242(8) Uani 1 1 d . . .
S1 S 0.41319(16) 0.13331(13) 1.16819(10) 0.0153(3) Uani 1 1 d . . .
C1 C 0.3412(7) -0.0274(6) 1.1448(4) 0.0202(12) Uani 1 1 d . . .
H1A H 0.4223 -0.0898 1.1651 0.024 Uiso 1 1 calc R . .
H1B H 0.2541 -0.0434 1.1848 0.024 Uiso 1 1 calc R . .
C2 C 0.2902(7) -0.0432(5) 1.0344(4) 0.0183(11) Uani 1 1 d . . .
H2A H 0.3800 -0.0581 0.9967 0.022 Uiso 1 1 calc R . .
H2B H 0.2215 -0.1176 1.0246 0.022 Uiso 1 1 calc R . .
C3 C 0.1406(6) 0.0677(5) 0.9039(4) 0.0149(10) Uani 1 1 d . . .
C4 C 0.0721(7) 0.1897(6) 0.8636(4) 0.0197(12) Uani 1 1 d . . .
H4A H 0.0990 0.2012 0.7942 0.024 Uiso 1 1 calc R . .
H4B H -0.0405 0.1833 0.8613 0.024 Uiso 1 1 calc R . .
C5 C 0.2234(6) 0.3888(5) 0.8706(4) 0.0154(10) Uani 1 1 d . . .
H5A H 0.2136 0.4775 0.8937 0.018 Uiso 1 1 calc R . .
H5B H 0.1940 0.3860 0.7977 0.018 Uiso 1 1 calc R . .
C6 C 0.3844(6) 0.3440(5) 0.8927(4) 0.0106(9) Uani 1 1 d . . .
C7 C 0.6492(6) 0.3637(5) 0.8613(4) 0.0150(10) Uani 1 1 d . . .
H11A H 0.6929 0.3264 0.8025 0.018 Uiso 1 1 calc R . .
H11B H 0.6618 0.3007 0.9162 0.018 Uiso 1 1 calc R . .
C8 C 0.7395(7) 0.4822(6) 0.8933(4) 0.0164(10) Uani 1 1 d . . .
N1 N 0.2090(5) 0.0733(4) 0.9969(3) 0.0138(9) Uani 1 1 d . . .
N2 N 0.1228(6) 0.3046(5) 0.9234(4) 0.0162(9) Uani 1 1 d . . .
H2 H 0.0363 0.3506 0.9360 0.019 Uiso 1 1 calc R . .
N3 N 0.4897(5) 0.3851(5) 0.8364(3) 0.0143(9) Uani 1 1 d . . .
H3 H 0.4606 0.4273 0.7814 0.017 Uiso 1 1 calc R . .
O1 O 0.0818(5) 0.2541(4) 1.1323(4) 0.0196(9) Uani 1 1 d . . .
O2 O 0.1299(5) -0.0285(4) 0.8517(3) 0.0237(9) Uani 1 1 d . . .
O3 O 0.4159(5) 0.2734(4) 0.9673(3) 0.0163(8) Uani 1 1 d . . .
O4 O 0.6650(4) 0.5852(4) 0.8836(3) 0.0143(7) Uani 1 1 d . . .
O5 O 0.8727(5) 0.4691(4) 0.9269(3) 0.0241(10) Uani 1 1 d . . .
O1W O 0.2599(8) 0.6951(6) 0.8633(5) 0.0543(18) Uani 1 1 d . . .
H1W H 0.1596 0.7030 0.8652 0.081 Uiso 1 1 d R . .
H2W H 0.2832 0.7809 0.8446 0.081 Uiso 1 1 d R . .
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'
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 Re1 N1 105.6(2) . . ?
O1 Re1 O4 94.97(18) . 3_667 ?
N1 Re1 O4 159.40(18) . 3_667 ?
O1 Re1 N2 96.8(2) . . ?
N1 Re1 N2 80.69(19) . . ?
O4 Re1 N2 98.28(17) 3_667 . ?
O1 Re1 O3 164.21(18) . . ?
N1 Re1 O3 84.94(17) . . ?
O4 Re1 O3 75.19(15) 3_667 . ?
N2 Re1 O3 72.99(17) . . ?
O1 Re1 S1 105.91(16) . . ?
N1 Re1 S1 83.79(14) . . ?
O4 Re1 S1 89.58(11) 3_667 . ?
N2 Re1 S1 155.29(14) . . ?
O3 Re1 S1 86.62(11) . . ?
C1 S1 Re1 98.1(2) . . ?
C2 C1 S1 109.7(4) . . ?
C2 C1 H1A 109.7 . . ?
S1 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
S1 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N1 C2 C1 109.3(5) . . ?
N1 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N1 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
O2 C3 N1 124.9(5) . . ?
O2 C3 C4 119.5(5) . . ?
N1 C3 C4 115.5(5) . . ?
N2 C4 C3 114.1(5) . . ?
N2 C4 H4A 108.7 . . ?
C3 C4 H4A 108.7 . . ?
N2 C4 H4B 108.7 . . ?
C3 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
N2 C5 C6 108.3(4) . . ?
N2 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
N2 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
O3 C6 N3 122.2(5) . . ?
O3 C6 C5 118.7(5) . . ?
N3 C6 C5 119.0(5) . . ?
N3 C7 C8 114.4(5) . . ?
N3 C7 H11A 108.7 . . ?
C8 C7 H11A 108.7 . . ?
N3 C7 H11B 108.7 . . ?
C8 C7 H11B 108.7 . . ?
H11A C7 H11B 107.6 . . ?
O5 C8 O4 127.1(6) . . ?
O5 C8 C7 118.0(5) . . ?
O4 C8 C7 114.9(5) . . ?
C3 N1 C2 116.3(5) . . ?
C3 N1 Re1 120.1(4) . . ?
C2 N1 Re1 122.5(4) . . ?
C5 N2 C4 113.0(5) . . ?
C5 N2 Re1 111.7(3) . . ?
C4 N2 Re1 107.8(4) . . ?
C5 N2 H2 108.1 . . ?
C4 N2 H2 108.1 . . ?
Re1 N2 H2 108.1 . . ?
C6 N3 C7 122.7(5) . . ?
C6 N3 H3 118.7 . . ?
C7 N3 H3 118.7 . . ?
C6 O3 Re1 117.3(4) . . ?
C8 O4 Re1 120.8(4) . 3_667 ?
H1W O1W H2W 98.9 . . ?
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
Re1 O1 1.676(5) . ?
Re1 N1 1.988(5) . ?
Re1 O4 2.128(4) 3_667 ?
Re1 N2 2.190(5) . ?
Re1 O3 2.205(4) . ?
Re1 S1 2.2784(14) . ?
S1 C1 1.824(6) . ?
C1 C2 1.517(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N1 1.484(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O2 1.230(7) . ?
C3 N1 1.337(7) . ?
C3 C4 1.498(8) . ?
C4 N2 1.496(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.478(7) . ?
C5 C6 1.497(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O3 1.259(6) . ?
C6 N3 1.321(6) . ?
C7 N3 1.430(7) . ?
C7 C8 1.520(8) . ?
C7 H11A 0.9900 . ?
C7 H11B 0.9900 . ?
C8 O5 1.224(7) . ?
C8 O4 1.267(7) . ?
N2 H2 0.9300 . ?
N3 H3 0.8800 . ?
O4 Re1 2.128(4) 3_667 ?
O1W H1W 0.8890 . ?
O1W H2W 0.9645 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Re1 S1 C1 81.3(3) . . . . ?
N1 Re1 S1 C1 -23.2(2) . . . . ?
O4 Re1 S1 C1 176.3(2) 3_667 . . . ?
N2 Re1 S1 C1 -74.5(4) . . . . ?
O3 Re1 S1 C1 -108.5(2) . . . . ?
Re1 S1 C1 C2 41.0(4) . . . . ?
S1 C1 C2 N1 -41.0(6) . . . . ?
O2 C3 C4 N2 -166.6(5) . . . . ?
N1 C3 C4 N2 14.0(7) . . . . ?
N2 C5 C6 O3 -18.9(7) . . . . ?
N2 C5 C6 N3 164.5(5) . . . . ?
N3 C7 C8 O5 171.6(5) . . . . ?
N3 C7 C8 O4 -7.0(7) . . . . ?
O2 C3 N1 C2 6.3(8) . . . . ?
C4 C3 N1 C2 -174.4(5) . . . . ?
O2 C3 N1 Re1 174.2(5) . . . . ?
C4 C3 N1 Re1 -6.5(7) . . . . ?
C1 C2 N1 C3 -172.0(5) . . . . ?
C1 C2 N1 Re1 20.4(6) . . . . ?
O1 Re1 N1 C3 93.2(4) . . . . ?
O4 Re1 N1 C3 -90.1(6) 3_667 . . . ?
N2 Re1 N1 C3 -1.3(4) . . . . ?
O3 Re1 N1 C3 -74.8(4) . . . . ?
S1 Re1 N1 C3 -162.0(4) . . . . ?
O1 Re1 N1 C2 -99.7(4) . . . . ?
O4 Re1 N1 C2 77.1(7) 3_667 . . . ?
N2 Re1 N1 C2 165.8(4) . . . . ?
O3 Re1 N1 C2 92.3(4) . . . . ?
S1 Re1 N1 C2 5.1(4) . . . . ?
C6 C5 N2 C4 -87.4(5) . . . . ?
C6 C5 N2 Re1 34.4(5) . . . . ?
C3 C4 N2 C5 110.1(5) . . . . ?
C3 C4 N2 Re1 -13.8(6) . . . . ?
O1 Re1 N2 C5 138.9(4) . . . . ?
N1 Re1 N2 C5 -116.4(4) . . . . ?
O4 Re1 N2 C5 42.8(4) 3_667 . . . ?
O3 Re1 N2 C5 -28.8(3) . . . . ?
S1 Re1 N2 C5 -64.5(5) . . . . ?
O1 Re1 N2 C4 -96.4(4) . . . . ?
N1 Re1 N2 C4 8.3(4) . . . . ?
O4 Re1 N2 C4 167.5(4) 3_667 . . . ?
O3 Re1 N2 C4 95.8(4) . . . . ?
S1 Re1 N2 C4 60.1(5) . . . . ?
O3 C6 N3 C7 -6.6(8) . . . . ?
C5 C6 N3 C7 169.9(5) . . . . ?
C8 C7 N3 C6 -109.8(6) . . . . ?
N3 C6 O3 Re1 170.2(4) . . . . ?
C5 C6 O3 Re1 -6.2(6) . . . . ?
O1 Re1 O3 C6 -31.2(9) . . . . ?
N1 Re1 O3 C6 101.6(4) . . . . ?
O4 Re1 O3 C6 -83.9(4) 3_667 . . . ?
N2 Re1 O3 C6 19.8(4) . . . . ?
S1 Re1 O3 C6 -174.4(4) . . . . ?
O5 C8 O4 Re1 -2.6(8) . . . 3_667 ?
C7 C8 O4 Re1 175.9(3) . . . 3_667 ?
