#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:00:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179435 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/32/4333228.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_4333228
loop_
_publ_author_name
'Cantorias, Melchor V.'
'Howell, Robertha C.'
'Todaro, Louis'
'Cyr, John E.'
'Berndorff, Dietmar'
'Rogers, Robin D.'
'Francesconi, Lynn C.'
_publ_section_title
;
 MO tripeptide diastereomers (M=99/99mTc, Re): models to identify the
 structure of 99mTc peptide targeted radiopharmaceuticals.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7326
_journal_page_last               7340
_journal_paper_doi               10.1021/ic070077p
_journal_volume                  46
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_sum            'C18 H30 N5 O6 Re S'
_chemical_formula_weight         630.73
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 106.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6480(19)
_cell_length_b                   10.186(2)
_cell_length_c                   12.272(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1157.2(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'ω 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  0.0914
_diffrn_reflns_av_sigmaI/netI    0.0839
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10247
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    5.384
_exptl_absorpt_correction_T_max  0.9000
_exptl_absorpt_correction_T_min  0.3463
_exptl_absorpt_correction_type   integration
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.304
_refine_diff_density_min         -2.787
_refine_diff_density_rms         0.219
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 2054 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.006(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4820
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0466P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                4345
_reflns_number_total             4820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070077psup4.cif
_cod_data_source_block           x1463l
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

 Adding full bibliography for 4333225--4333231.cif.
;
_cod_original_cell_volume        1157.2(4)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4333228
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
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
Re Re 0.43657(2) 0.40992(4) 0.368861(19) 0.00932(9) Uani 1 1 d .
S S 0.2864(2) 0.56306(19) 0.41249(17) 0.0131(4) Uani 1 1 d .
O1 O 0.4350(6) 0.2722(6) 0.4446(5) 0.0159(12) Uani 1 1 d .
O3 O 0.7689(6) 0.4323(7) 0.2213(4) 0.0169(16) Uani 1 1 d .
O6 O 0.2294(6) 0.3467(6) 0.0316(5) 0.0171(12) Uani 1 1 d .
O9 O 0.2240(6) 0.6734(6) 0.1272(5) 0.0162(12) Uani 1 1 d .
N1 N 0.6065(7) 0.5173(6) 0.4385(5) 0.0107(13) Uani 1 1 d U
H1A H 0.6050 0.5774 0.4897 0.013 Uiso 1 1 calc R
N4 N 0.5530(6) 0.3906(7) 0.2568(5) 0.0090(17) Uani 1 1 d .
N7 N 0.2842(5) 0.4133(13) 0.2163(4) 0.0118(11) Uani 1 1 d U
N9 N -0.0100(8) 0.6161(7) 0.0561(6) 0.0154(15) Uani 1 1 d .
H9A H -0.0304 0.6879 0.0147 0.018 Uiso 1 1 calc R
H9B H -0.0782 0.5581 0.0544 0.018 Uiso 1 1 calc R
N15 N 0.5050(8) -0.2615(7) 0.2661(6) 0.0141(16) Uani 1 1 d .
H15A H 0.4141 -0.2876 0.2280 0.017 Uiso 1 1 calc R
H15B H 0.5363 -0.3081 0.3318 0.017 Uiso 1 1 calc R
H15C H 0.5653 -0.2758 0.2222 0.017 Uiso 1 1 calc R
C2 C 0.7368(9) 0.4936(8) 0.4019(7) 0.0129(17) Uani 1 1 d .
H2A H 0.7865 0.5792 0.3991 0.015 Uiso 1 1 calc R
C3 C 0.6883(8) 0.4358(7) 0.2832(6) 0.0095(19) Uani 1 1 d .
C5 C 0.4797(8) 0.3424(8) 0.1425(7) 0.0117(16) Uani 1 1 d .
H5A H 0.5125 0.3965 0.0864 0.014 Uiso 1 1 calc R
C6 C 0.3178(9) 0.3671(7) 0.1237(6) 0.0124(16) Uani 1 1 d .
C8 C 0.1397(8) 0.4733(8) 0.1957(7) 0.0123(16) Uani 1 1 d .
H8A H 0.0650 0.4074 0.1573 0.015 Uiso 1 1 calc R
C9 C 0.1229(10) 0.5955(9) 0.1209(7) 0.0167(18) Uani 1 1 d .
C10 C 0.1174(9) 0.5085(8) 0.3109(6) 0.0128(16) Uani 1 1 d .
H10A H 0.0799 0.4309 0.3420 0.015 Uiso 1 1 calc R
H10B H 0.0444 0.5793 0.3004 0.015 Uiso 1 1 calc R
C11 C 0.5127(9) 0.1992(8) 0.1251(6) 0.0129(16) Uani 1 1 d .
H11A H 0.4522 0.1704 0.0496 0.015 Uiso 1 1 calc R
H11B H 0.6150 0.1915 0.1254 0.015 Uiso 1 1 calc R
C12 C 0.4859(11) 0.1088(9) 0.2145(7) 0.017(2) Uani 1 1 d .
H12A H 0.3854 0.1211 0.2178 0.020 Uiso 1 1 calc R
H12B H 0.5512 0.1339 0.2893 0.020 Uiso 1 1 calc R
C13 C 0.5094(9) -0.0374(8) 0.1931(7) 0.0154(17) Uani 1 1 d .
H13A H 0.4337 -0.0676 0.1252 0.018 Uiso 1 1 calc R
H13B H 0.6044 -0.0491 0.1784 0.018 Uiso 1 1 calc R
C14 C 0.5039(10) -0.1175(7) 0.2934(7) 0.023(2) Uani 1 1 d .
H14A H 0.4151 -0.0961 0.3150 0.028 Uiso 1 1 calc R
H14B H 0.5882 -0.0964 0.3585 0.028 Uiso 1 1 calc R
C20 C 0.8429(7) 0.3994(13) 0.4798(6) 0.0136(17) Uani 1 1 d .
H20A H 0.7896 0.3201 0.4915 0.016 Uiso 1 1 calc R
H20B H 0.9154 0.3716 0.4413 0.016 Uiso 1 1 calc R
C21 C 0.9208(8) 0.4565(7) 0.5944(7) 0.0138(16) Uani 1 1 d .
C22 C 1.0140(10) 0.5624(10) 0.6020(8) 0.024(2) Uani 1 1 d .
H22A H 1.0259 0.5998 0.5343 0.029 Uiso 1 1 calc R
C23 C 1.0896(11) 0.6147(10) 0.7054(7) 0.026(2) Uani 1 1 d .
H23A H 1.1529 0.6870 0.7087 0.032 Uiso 1 1 calc R
C24 C 1.0721(10) 0.5609(9) 0.8036(8) 0.025(2) Uani 1 1 d .
H24A H 1.1241 0.5959 0.8753 0.029 Uiso 1 1 calc R
C25 C 0.9790(9) 0.4559(8) 0.7984(7) 0.0201(19) Uani 1 1 d .
H25A H 0.9679 0.4161 0.8655 0.024 Uiso 1 1 calc R
C26 C 0.9042(7) 0.4120(15) 0.6937(5) 0.0190(14) Uani 1 1 d .
H26A H 0.8348 0.3447 0.6901 0.023 Uiso 1 1 calc R
O11 O 0.7256(7) 0.7104(6) 0.1630(5) 0.0217(14) Uani 1 1 d .
H11C H 0.7421 0.6294 0.1692 0.026 Uiso 1 1 d .
H11D H 0.7426 0.7365 0.1037 0.026 Uiso 1 1 d .
O12 O 0.1907(7) 0.8879(7) -0.0152(5) 0.0239(19) Uani 1 1 d .
H12C H 0.2090 0.8840 -0.0779 0.029 Uiso 1 1 d .
H12D H 0.2068 0.8151 0.0161 0.029 Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Re Re -1.0185 7.2310 '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'
O O 0.0106 0.0060 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 Re N1 111.2(3)
O1 Re N4 112.8(3)
N1 Re N4 78.1(3)
O1 Re N7 114.0(4)
N1 Re N7 134.0(4)
N4 Re N7 76.7(2)
O1 Re S 109.5(2)
N1 Re S 91.41(19)
N4 Re S 137.4(2)
N7 Re S 82.1(3)
C10 S Re 97.7(3)
C2 N1 Re 117.3(5)
C3 N4 C5 121.5(6)
C3 N4 Re 119.7(5)
C5 N4 Re 118.3(5)
C6 N7 C8 116.0(6)
C6 N7 Re 119.1(6)
C8 N7 Re 124.6(5)
N1 C2 C3 107.3(6)
N1 C2 C20 113.1(6)
C3 C2 C20 109.1(7)
O3 C3 N4 125.8(6)
O3 C3 C2 121.7(7)
N4 C3 C2 112.5(6)
N4 C5 C11 113.1(6)
N4 C5 C6 106.5(6)
C11 C5 C6 112.4(7)
O6 C6 N7 124.4(7)
O6 C6 C5 121.6(7)
N7 C6 C5 114.0(6)
N7 C8 C9 112.0(7)
N7 C8 C10 108.1(6)
C9 C8 C10 110.2(6)
O9 C9 N9 123.2(8)
O9 C9 C8 122.3(7)
N9 C9 C8 114.3(8)
C8 C10 S 111.6(6)
C12 C11 C5 113.4(7)
C11 C12 C13 113.8(7)
C14 C13 C12 110.4(7)
C13 C14 N15 110.3(7)
C21 C20 C2 114.2(9)
C26 C21 C22 116.0(8)
C26 C21 C20 123.8(8)
C22 C21 C20 120.3(8)
C23 C22 C21 121.7(8)
C24 C23 C22 119.2(9)
C23 C24 C25 120.2(8)
C26 C25 C24 117.5(9)
C21 C26 C25 125.1(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re O1 1.686(5)
Re N1 1.956(7)
Re N4 2.015(6)
Re N7 2.029(5)
Re S 2.293(2)
S C10 1.838(8)
O3 C3 1.232(9)
O6 C6 1.227(9)
O9 C9 1.243(11)
N1 C2 1.469(10)
N4 C3 1.336(9)
N4 C5 1.467(9)
N7 C6 1.351(11)
N7 C8 1.478(11)
N9 C9 1.322(11)
N15 C14 1.504(10)
C2 C3 1.518(10)
C2 C20 1.526(13)
C5 C11 1.521(11)
C5 C6 1.534(11)
C8 C9 1.529(12)
C8 C10 1.531(11)
C11 C12 1.509(12)
C12 C13 1.540(12)
C13 C14 1.490(12)
C20 C21 1.512(11)
C21 C26 1.352(12)
C21 C22 1.391(12)
C22 C23 1.379(13)
C23 C24 1.378(13)
C24 C25 1.387(13)
C25 C26 1.360(11)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O1 0.88 2.22 3.046(8) 157.3 2_656
N9 H9A O6 0.88 2.45 3.142(9) 135.6 2
N9 H9B O12 0.88 2.03 2.864(10) 157.7 2_545
N15 H15A O9 0.91 1.94 2.845(9) 170.9 1_545
N15 H15B N1 0.91 2.20 3.057(9) 156.7 1_545
N15 H15C O11 0.91 1.89 2.781(10) 165.7 1_545
O11 H11C O3 0.84 2.10 2.923(9) 166.0 .
O11 H11D O6 0.83 2.08 2.898(8) 165.7 2_655
O12 H12C O3 0.84 1.90 2.704(8) 161.5 2_655
O12 H12D O9 0.83 1.96 2.758(8) 161.5 .
