#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:26:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179141 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/02/4310232.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_4310232
loop_
_publ_author_name
'Tobias K. Heinrich'
'Werner Kraus'
'Hans-Jürgen Pietzsch'
'Sepp Seifert'
'Christoph Smuda'
'Hartmut Spies'
_publ_contact_author
;
      Hans-Jürgen Pietzsch
      Forschungszentrum Rossendorf,
      Institut für Bioanorganische und Radiopharmazeutische Chemie, 
      Postfach 510119, 
    D-01314 Dresden
     Germany
;
_publ_contact_author_email       h.j.pietzsch@fz-rossendorf.de
_publ_contact_author_fax         '+49 351 260 3232'
_publ_section_title
;
Novel Rhenium Chelate System Derived from Dimercaptosuccinic Acid for the
Selective Labeling of Biomolecules
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9930
_journal_page_last               9937
_journal_paper_doi               10.1021/ic051148s
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C31 H60 N5 O6 Re S4'
_chemical_formula_weight         913.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.539(11)
_cell_angle_beta                 97.841(11)
_cell_angle_gamma                108.967(10)
_cell_formula_units_Z            2
_cell_length_a                   10.576(6)
_cell_length_b                   12.616(7)
_cell_length_c                   16.991(9)
_cell_measurement_reflns_used    941
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      22.915
_cell_measurement_theta_min      2.491
_cell_volume                     2078(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL-NT (Sheldrick, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       omega-scan
_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  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0847
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10496
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.92
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.167
_exptl_absorpt_correction_T_max  0.504
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.705
_refine_diff_density_min         -1.437
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7245
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.852
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0363P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                5245
_reflns_number_total             7245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051148ssi20050711_095159_1.cif
_cod_data_source_block           5g-a
_cod_database_code               4310232
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Re Re 0.69352(3) 0.86301(2) 0.717655(15) 0.04298(9) Uani 1 1 d . . .
S1 S 0.66241(14) 1.00987(12) 0.65920(9) 0.0471(4) Uani 1 1 d . . .
S2 S 0.91587(15) 0.98621(14) 0.76467(10) 0.0541(4) Uani 1 1 d . . .
S3 S 0.73452(15) 0.80998(13) 0.84115(9) 0.0519(4) Uani 1 1 d . . .
S4 S 0.47215(14) 0.82343(12) 0.73714(9) 0.0468(4) Uani 1 1 d . . .
O1 O 0.6932(4) 0.7603(3) 0.6429(2) 0.0604(11) Uani 1 1 d . . .
O2 O 1.0637(5) 1.2682(4) 0.8335(3) 0.0851(15) Uani 1 1 d . . .
O3 O 0.5439(4) 0.9213(3) 0.9354(2) 0.0522(10) Uani 1 1 d . . .
O4 O 0.8991(4) 1.2918(4) 0.6556(2) 0.0599(11) Uani 1 1 d . . .
O5 O 0.2904(4) 0.7173(3) 0.8803(2) 0.0597(11) Uani 1 1 d . . .
N1 N 0.8357(6) 1.2186(4) 0.8088(3) 0.0651(15) Uani 1 1 d . . .
H1B H 0.7607 1.1745 0.7768 0.078 Uiso 1 1 calc R . .
N2 N 0.7585(6) 1.1020(5) 1.0305(3) 0.0532(13) Uani 1 1 d D . .
H2C H 0.739(5) 1.148(3) 1.069(2) 0.039(16) Uiso 1 1 d D . .
H2D H 0.673(2) 1.056(4) 1.007(3) 0.07(2) Uiso 1 1 d D . .
N3 N 0.5990(5) 0.8098(4) 1.0154(3) 0.0515(12) Uani 1 1 d . . .
H3A H 0.6108 0.7458 1.0174 0.062 Uiso 1 1 calc R . .
N4 N 0.7671(5) 1.1843(4) 0.5374(3) 0.0484(12) Uani 1 1 d . . .
N5 N 0.2142(5) 0.5861(4) 0.7641(3) 0.0450(12) Uani 1 1 d . . .
C1 C 0.8359(5) 1.0897(5) 0.6442(3) 0.0411(13) Uani 1 1 d . . .
H1C H 0.8586 1.0400 0.6027 0.049 Uiso 1 1 calc R . .
C2 C 0.9411(5) 1.1162(5) 0.7217(3) 0.0431(14) Uani 1 1 d . . .
H2B H 1.0306 1.1361 0.7062 0.052 Uiso 1 1 calc R . .
C3 C 0.9520(7) 1.2097(5) 0.7917(4) 0.0557(16) Uani 1 1 d . . .
C4 C 0.8272(9) 1.2974(6) 0.8776(4) 0.091(3) Uani 1 1 d . . .
H4A H 0.7775 1.3442 0.8587 0.109 Uiso 1 1 calc R . .
H4B H 0.9183 1.3478 0.9050 0.109 Uiso 1 1 calc R . .
C5 C 0.7550(8) 1.2317(6) 0.9370(4) 0.082(2) Uani 1 1 d . . .
H5A H 0.7391 1.2850 0.9784 0.099 Uiso 1 1 calc R . .
H5B H 0.6670 1.1769 0.9081 0.099 Uiso 1 1 calc R . .
C6 C 0.8336(8) 1.1713(6) 0.9757(4) 0.075(2) Uani 1 1 d . . .
H6A H 0.9196 1.2264 1.0072 0.089 Uiso 1 1 calc R . .
H6B H 0.8538 1.1209 0.9343 0.089 Uiso 1 1 calc R . .
C7 C 0.8322(6) 1.0319(6) 1.0642(4) 0.0640(18) Uani 1 1 d . . .
H7A H 0.9236 1.0814 1.0917 0.077 Uiso 1 1 calc R . .
H7B H 0.8402 0.9777 1.0200 0.077 Uiso 1 1 calc R . .
C8 C 0.7607(6) 0.9671(6) 1.1232(4) 0.0647(18) Uani 1 1 d . . .
H8A H 0.8134 0.9228 1.1427 0.078 Uiso 1 1 calc R . .
H8B H 0.7613 1.0225 1.1696 0.078 Uiso 1 1 calc R . .
C9 C 0.6164(6) 0.8877(5) 1.0909(3) 0.0579(16) Uani 1 1 d . . .
H9A H 0.5858 0.8435 1.1311 0.070 Uiso 1 1 calc R . .
H9B H 0.5589 0.9330 1.0827 0.070 Uiso 1 1 calc R . .
C10 C 0.5655(5) 0.8325(5) 0.9424(3) 0.0467(14) Uani 1 1 d . . .
C11 C 0.5685(6) 0.7467(5) 0.8711(3) 0.0448(14) Uani 1 1 d . . .
H11A H 0.5686 0.6774 0.8906 0.054 Uiso 1 1 calc R . .
C12 C 0.4549(6) 0.7112(4) 0.7978(3) 0.0423(14) Uani 1 1 d . . .
H12A H 0.4633 0.6456 0.7629 0.051 Uiso 1 1 calc R . .
C13 C 0.8367(6) 1.1970(6) 0.6119(4) 0.0472(15) Uani 1 1 d . . .
C14 C 0.7515(7) 1.2869(5) 0.5126(4) 0.0624(18) Uani 1 1 d . . .
H14A H 0.8395 1.3484 0.5272 0.075 Uiso 1 1 calc R . .
H14B H 0.7236 1.2707 0.4540 0.075 Uiso 1 1 calc R . .
C15 C 0.6526(11) 1.3264(8) 0.5490(6) 0.117(4) Uani 1 1 d . . .
H15A H 0.6993 1.3577 0.6057 0.141 Uiso 1 1 calc R . .
C16 C 0.5300(10) 1.2478(8) 0.5555(7) 0.151(5) Uani 1 1 d . . .
H16A H 0.5466 1.1869 0.5779 0.226 Uiso 1 1 calc R . .
H16B H 0.4722 1.2170 0.5028 0.226 Uiso 1 1 calc R . .
H16C H 0.4862 1.2850 0.5905 0.226 Uiso 1 1 calc R . .
C17 C 0.6387(11) 1.4307(8) 0.5198(6) 0.151(5) Uani 1 1 d . . .
H17A H 0.5769 1.4563 0.5470 0.226 Uiso 1 1 calc R . .
H17B H 0.6041 1.4111 0.4623 0.226 Uiso 1 1 calc R . .
H17C H 0.7264 1.4908 0.5316 0.226 Uiso 1 1 calc R . .
C18 C 0.7079(6) 1.0778(5) 0.4757(3) 0.0510(15) Uani 1 1 d . . .
H18A H 0.6142 1.0675 0.4535 0.061 Uiso 1 1 calc R . .
H18B H 0.7069 1.0139 0.5013 0.061 Uiso 1 1 calc R . .
C19 C 0.7867(7) 1.0767(6) 0.4058(4) 0.0620(18) Uani 1 1 d . . .
H19A H 0.7815 1.1386 0.3783 0.074 Uiso 1 1 calc R . .
C20 C 0.9322(8) 1.0958(8) 0.4343(5) 0.117(3) Uani 1 1 d . . .
H20A H 0.9768 1.0956 0.3888 0.175 Uiso 1 1 calc R . .
H20B H 0.9399 1.0360 0.4614 0.175 Uiso 1 1 calc R . .
H20C H 0.9745 1.1685 0.4714 0.175 Uiso 1 1 calc R . .
C21 C 0.7145(8) 0.9636(7) 0.3452(4) 0.096(3) Uani 1 1 d . . .
H21A H 0.7621 0.9610 0.3011 0.144 Uiso 1 1 calc R . .
H21B H 0.6226 0.9571 0.3246 0.144 Uiso 1 1 calc R . .
H21C H 0.7134 0.9013 0.3717 0.144 Uiso 1 1 calc R . .
C22 C 0.3124(6) 0.6706(5) 0.8167(4) 0.0461(14) Uani 1 1 d . . .
C23 C 0.2296(6) 0.5241(5) 0.6873(3) 0.0534(16) Uani 1 1 d . . .
H23A H 0.3106 0.5711 0.6713 0.064 Uiso 1 1 calc R . .
H23B H 0.1519 0.5136 0.6454 0.064 Uiso 1 1 calc R . .
C24 C 0.2406(7) 0.4076(5) 0.6913(4) 0.067(2) Uani 1 1 d . . .
H24A H 0.1644 0.3653 0.7146 0.080 Uiso 1 1 calc R . .
C25 C 0.3707(8) 0.4139(6) 0.7445(5) 0.101(3) Uani 1 1 d . . .
H25A H 0.3790 0.4558 0.7981 0.151 Uiso 1 1 calc R . .
H25B H 0.4474 0.4522 0.7220 0.151 Uiso 1 1 calc R . .
H25C H 0.3685 0.3379 0.7472 0.151 Uiso 1 1 calc R . .
C26 C 0.2225(8) 0.3416(6) 0.6057(5) 0.100(3) Uani 1 1 d . . .
H26A H 0.1396 0.3398 0.5734 0.151 Uiso 1 1 calc R . .
H26B H 0.2179 0.2648 0.6074 0.151 Uiso 1 1 calc R . .
H26C H 0.2984 0.3786 0.5822 0.151 Uiso 1 1 calc R . .
C27 C 0.0764(6) 0.5474(5) 0.7821(4) 0.0539(16) Uani 1 1 d . . .
H27A H 0.0835 0.5662 0.8404 0.065 Uiso 1 1 calc R . .
H27B H 0.0369 0.4647 0.7651 0.065 Uiso 1 1 calc R . .
C28 C -0.0191(8) 0.5987(7) 0.7417(6) 0.102(3) Uani 1 1 d . . .
H28A H -0.0401 0.5546 0.6860 0.123 Uiso 1 1 calc R . .
C29 C 0.0172(11) 0.7010(11) 0.7284(10) 0.226(8) Uani 1 1 d . . .
H29A H -0.0589 0.7113 0.6969 0.339 Uiso 1 1 calc R . .
H29B H 0.0905 0.7130 0.6992 0.339 Uiso 1 1 calc R . .
H29C H 0.0470 0.7551 0.7792 0.339 Uiso 1 1 calc R . .
C30 C -0.1581(7) 0.5518(6) 0.7655(5) 0.104(3) Uani 1 1 d . . .
H30A H -0.2210 0.5803 0.7372 0.156 Uiso 1 1 calc R . .
H30B H -0.1487 0.5761 0.8230 0.156 Uiso 1 1 calc R . .
H30C H -0.1920 0.4697 0.7513 0.156 Uiso 1 1 calc R . .
C31 C 1.2935(15) 1.4688(10) 0.9907(8) 0.151(5) Uani 1 1 d D . .
O6 O 1.2827(7) 1.3618(6) 0.9559(4) 0.126(2) Uani 1 1 d D . .
H6F H 1.211(9) 1.316(9) 0.911(5) 0.25(6) Uiso 1 1 d D . .
H31B H 1.253(9) 1.523(7) 0.957(6) 0.24(6) Uiso 1 1 d D . .
H31A H 1.199(5) 1.424(8) 1.010(5) 0.16(5) Uiso 1 1 d D . .
H31C H 1.342(12) 1.534(7) 1.047(3) 0.35(9) Uiso 1 1 d 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'
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 S2 107.96(15) . . ?
O1 Re S4 107.88(15) . . ?
S2 Re S4 144.11(6) . . ?
O1 Re S1 107.61(15) . . ?
S2 Re S1 85.43(6) . . ?
S4 Re S1 85.66(5) . . ?
O1 Re S3 108.98(15) . . ?
S2 Re S3 81.17(6) . . ?
S4 Re S3 85.58(5) . . ?
S1 Re S3 143.33(6) . . ?
C1 S1 Re 103.04(17) . . ?
C2 S2 Re 108.92(18) . . ?
C11 S3 Re 108.19(18) . . ?
C12 S4 Re 101.50(18) . . ?
C3 N1 C4 124.5(6) . . ?
C7 N2 C6 112.1(5) . . ?
C10 N3 C9 123.1(5) . . ?
C13 N4 C18 126.3(5) . . ?
C13 N4 C14 117.7(5) . . ?
C18 N4 C14 116.0(5) . . ?
C22 N5 C27 118.9(5) . . ?
C22 N5 C23 125.9(5) . . ?
C27 N5 C23 115.2(5) . . ?
C2 C1 C13 112.9(5) . . ?
C2 C1 S1 110.9(4) . . ?
C13 C1 S1 110.1(3) . . ?
C3 C2 C1 120.3(5) . . ?
C3 C2 S2 105.4(4) . . ?
C1 C2 S2 110.0(4) . . ?
O2 C3 N1 122.7(6) . . ?
O2 C3 C2 119.7(6) . . ?
N1 C3 C2 117.4(6) . . ?
N1 C4 C5 110.5(5) . . ?
C6 C5 C4 112.3(7) . . ?
C5 C6 N2 111.9(6) . . ?
N2 C7 C8 112.3(5) . . ?
C9 C8 C7 116.2(5) . . ?
N3 C9 C8 113.7(5) . . ?
O3 C10 N3 121.6(5) . . ?
O3 C10 C11 123.3(5) . . ?
N3 C10 C11 114.9(5) . . ?
C12 C11 C10 117.8(4) . . ?
C12 C11 S3 109.6(4) . . ?
C10 C11 S3 106.0(4) . . ?
C11 C12 C22 114.3(5) . . ?
C11 C12 S4 112.5(4) . . ?
C22 C12 S4 110.3(4) . . ?
O4 C13 N4 121.9(5) . . ?
O4 C13 C1 119.3(5) . . ?
N4 C13 C1 118.8(6) . . ?
C15 C14 N4 114.5(5) . . ?
C16 C15 C14 120.0(8) . . ?
C16 C15 C17 113.7(8) . . ?
C14 C15 C17 112.0(7) . . ?
N4 C18 C19 112.9(5) . . ?
C20 C19 C21 111.9(6) . . ?
C20 C19 C18 112.8(6) . . ?
C21 C19 C18 108.1(6) . . ?
O5 C22 N5 121.5(5) . . ?
O5 C22 C12 119.6(5) . . ?
N5 C22 C12 118.9(5) . . ?
N5 C23 C24 114.4(5) . . ?
C25 C24 C26 111.5(6) . . ?
C25 C24 C23 113.8(6) . . ?
C26 C24 C23 109.1(6) . . ?
N5 C27 C28 114.5(5) . . ?
C29 C28 C27 124.7(8) . . ?
C29 C28 C30 117.0(7) . . ?
C27 C28 C30 109.2(6) . . ?
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 1.673(4) . ?
Re S2 2.3079(19) . ?
Re S4 2.3110(19) . ?
Re S1 2.3197(17) . ?
Re S3 2.3227(18) . ?
S1 C1 1.857(5) . ?
S2 C2 1.849(5) . ?
S3 C11 1.852(6) . ?
S4 C12 1.848(5) . ?
O2 C3 1.222(7) . ?
O3 C10 1.233(6) . ?
O4 C13 1.228(7) . ?
O5 C22 1.240(6) . ?
N1 C3 1.336(7) . ?
N1 C4 1.451(7) . ?
N2 C7 1.482(7) . ?
N2 C6 1.500(8) . ?
N3 C10 1.341(7) . ?
N3 C9 1.445(7) . ?
N4 C13 1.334(7) . ?
N4 C18 1.466(7) . ?
N4 C14 1.470(7) . ?
N5 C22 1.326(7) . ?
N5 C27 1.470(6) . ?
N5 C23 1.477(6) . ?
C1 C2 1.519(7) . ?
C1 C13 1.533(7) . ?
C2 C3 1.510(8) . ?
C4 C5 1.529(8) . ?
C5 C6 1.455(9) . ?
C7 C8 1.515(8) . ?
C8 C9 1.499(8) . ?
C10 C11 1.511(7) . ?
C11 C12 1.507(7) . ?
C12 C22 1.522(7) . ?
C14 C15 1.465(9) . ?
C15 C16 1.383(11) . ?
C15 C17 1.516(10) . ?
C18 C19 1.543(7) . ?
C19 C20 1.477(9) . ?
C19 C21 1.523(9) . ?
C23 C24 1.522(8) . ?
C24 C25 1.512(9) . ?
C24 C26 1.519(9) . ?
C27 C28 1.509(9) . ?
C28 C29 1.285(10) . ?
C28 C30 1.531(9) . ?
C31 O6 1.352(12) . ?
