#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:41:58 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179073 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/35/4303562.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_4303562
loop_
_publ_author_name
'Haiyang He'
'Jennifer E. Morley'
'Brendan Twamley'
'Ryan H. Groeneman'
'Dejan-Krešimir Bučǎr'
'Leonard R. MacGillivray'
'Paul D. Benny'
_publ_contact_author             'Benny, Paul'
_publ_contact_author_address
;Department of Chemistry
Washington State University
Pullman, WA 99164-4630 
USA
;
_publ_contact_author_email       bennyp@wsu.edu
_publ_contact_author_phone       '509 335-3858'
_publ_section_title
;
Investigation of the Coordination Interactions of
S-(Pyridin-2-ylmethyl)-l-Cysteine Ligands with M(CO)3+ (M = Re, 99mTc)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10625
_journal_page_last               10634
_journal_paper_doi               10.1021/ic901159r
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C11 H8 N O5 Re S'
_chemical_formula_sum            'C11 H8 N O5 Re S'
_chemical_formula_weight         452.44
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2008-10-29T16:45:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                101.925(5)
_cell_angle_beta                 106.904(5)
_cell_angle_gamma                101.832(5)
_cell_formula_units_Z            2
_cell_length_a                   7.2461(8)
_cell_length_b                   9.3299(10)
_cell_length_c                   10.3539(11)
_cell_measurement_reflns_used    2994
_cell_measurement_temperature    190(1)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.00
_cell_volume                     628.45(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo, Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL v6.1 (Sheldrick, 1997)'
_diffrn_ambient_temperature      190(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.014
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4297
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3.07
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'Kappa CCD'
_exptl_absorpt_coefficient_mu    9.848
_exptl_absorpt_correction_T_max  0.669
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.314
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0373P)²+0.3561P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0549
_reflns_number_gt                2128
_reflns_number_total             2207
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901159r_si_002_1.cif
_cod_data_source_block           9
_cod_database_code               4303562
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
C3 C 0.0004(6) 0.0017(5) 0.2961(4) 0.0278(9) Uani 1 1 d . . .
O3 O -0.0069(6) -0.1237(4) 0.2858(4) 0.0451(9) Uani 1 1 d . . .
O5 O 0.2508(5) 0.3876(3) 0.0449(3) 0.0333(7) Uani 1 1 d . . .
C11 C 0.1890(5) 0.3793(4) 0.1420(4) 0.0205(8) Uani 1 1 d . . .
C10 C 0.1241(6) 0.5127(4) 0.2086(4) 0.0253(9) Uani 1 1 d . . .
H10A H 0.052 0.5505 0.1345 0.03 Uiso 1 1 calc R . .
H10B H 0.2436 0.5944 0.2693 0.03 Uiso 1 1 calc R . .
Re1 Re -0.003477(19) 0.212524(14) 0.314175(13) 0.01970(9) Uani 1 1 d . . .
S1 S -0.03351(15) 0.46895(11) 0.31069(11) 0.0212(2) Uani 1 1 d . . .
O4 O 0.1891(4) 0.2681(3) 0.1988(3) 0.0235(6) Uani 1 1 d . . .
C2 C -0.1898(7) 0.1850(5) 0.4103(5) 0.0276(10) Uani 1 1 d . . .
N1 N -0.2242(5) 0.1616(4) 0.1012(4) 0.0190(7) Uani 1 1 d . . .
C1 C 0.2134(7) 0.2746(5) 0.4906(5) 0.0281(10) Uani 1 1 d . . .
C9 C -0.2838(6) 0.4077(4) 0.1780(4) 0.0240(8) Uani 1 1 d . . .
H9A H -0.3831 0.3854 0.2222 0.029 Uiso 1 1 calc R . .
H9B H -0.306 0.4901 0.1371 0.029 Uiso 1 1 calc R . .
O2 O -0.3047(5) 0.1749(4) 0.4681(3) 0.0413(8) Uani 1 1 d . . .
C6 C -0.4455(6) 0.1232(4) -0.1791(4) 0.0249(8) Uani 1 1 d . . .
H6 H -0.5188 0.1109 -0.2727 0.03 Uiso 1 1 calc R . .
C8 C -0.3116(5) 0.2686(4) 0.0633(4) 0.0194(8) Uani 1 1 d . . .
O1 O 0.3448(5) 0.3140(4) 0.5976(3) 0.0412(8) Uani 1 1 d . . .
C5 C -0.3570(6) 0.0128(4) -0.1415(4) 0.0229(8) Uani 1 1 d . . .
H5 H -0.3696 -0.0747 -0.2095 0.027 Uiso 1 1 calc R . .
C7 C -0.4230(6) 0.2523(4) -0.0751(4) 0.0227(8) Uani 1 1 d . . .
H7 H -0.4824 0.3274 -0.0981 0.027 Uiso 1 1 calc R . .
C4 C -0.2504(5) 0.0345(4) -0.0023(4) 0.0197(8) Uani 1 1 d . . .
H4 H -0.1934 -0.041 0.0225 0.024 Uiso 1 1 calc 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 0 '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 0.006 '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 7.231 '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
O3 C3 Re1 176.6(4) . . ?
O5 C11 O4 123.7(4) . . ?
O5 C11 C10 118.7(3) . . ?
O4 C11 C10 117.5(3) . . ?
C11 C10 S1 115.1(3) . . ?
C11 C10 H10A 108.5 . . ?
S1 C10 H10A 108.5 . . ?
C11 C10 H10B 108.5 . . ?
S1 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
C2 Re1 C1 89.51(19) . . ?
C2 Re1 C3 89.19(18) . . ?
C1 Re1 C3 89.56(18) . . ?
C2 Re1 O4 172.10(14) . . ?
C1 Re1 O4 93.78(16) . . ?
C3 Re1 O4 98.00(14) . . ?
C2 Re1 N1 97.57(16) . . ?
C1 Re1 N1 171.96(15) . . ?
C3 Re1 N1 94.34(15) . . ?
O4 Re1 N1 78.73(12) . . ?
C2 Re1 S1 91.86(14) . . ?
C1 Re1 S1 96.52(13) . . ?
C3 Re1 S1 173.84(13) . . ?
O4 Re1 S1 80.65(8) . . ?
N1 Re1 S1 79.50(9) . . ?
C10 S1 C9 101.9(2) . . ?
C10 S1 Re1 99.01(13) . . ?
C9 S1 Re1 96.58(13) . . ?
C11 O4 Re1 122.9(2) . . ?
O2 C2 Re1 176.7(4) . . ?
C8 N1 C4 117.6(3) . . ?
C8 N1 Re1 120.2(3) . . ?
C4 N1 Re1 121.3(3) . . ?
O1 C1 Re1 179.2(4) . . ?
C8 C9 S1 111.9(3) . . ?
C8 C9 H9A 109.2 . . ?
S1 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
S1 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C5 C6 C7 119.0(4) . . ?
C5 C6 H6 120.5 . . ?
C7 C6 H6 120.5 . . ?
N1 C8 C7 122.1(3) . . ?
N1 C8 C9 117.3(3) . . ?
C7 C8 C9 120.5(3) . . ?
C4 C5 C6 119.0(4) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C8 C7 C6 119.4(3) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
N1 C4 C5 122.9(3) . . ?
N1 C4 H4 118.5 . . ?
C5 C4 H4 118.5 . . ?
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
C3 O3 1.141(5) . ?
C3 Re1 1.943(5) . ?
O5 C11 1.223(5) . ?
C11 O4 1.294(5) . ?
C11 C10 1.523(5) . ?
C10 S1 1.810(4) . ?
C10 H10A 0.97 . ?
C10 H10B 0.97 . ?
Re1 C2 1.904(5) . ?
Re1 C1 1.913(5) . ?
Re1 O4 2.138(3) . ?
Re1 N1 2.203(3) . ?
Re1 S1 2.4529(10) . ?
S1 C9 1.818(4) . ?
C2 O2 1.158(6) . ?
N1 C8 1.352(5) . ?
N1 C4 1.362(5) . ?
C1 O1 1.159(6) . ?
C9 C8 1.501(5) . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C6 C5 1.383(6) . ?
C6 C7 1.385(6) . ?
C6 H6 0.93 . ?
C8 C7 1.384(6) . ?
C5 C4 1.372(6) . ?
C5 H5 0.93 . ?
C7 H7 0.93 . ?
C4 H4 0.93 . ?
