#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:34:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179507 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/04/4340416.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_4340416
loop_
_publ_author_name
'Karagiorgou, O.'
'Patsis, G.'
'Pelecanou, M.'
'Raptopoulou, C. P.'
'Terzis, A.'
'Siatra-Papastaikoudi, T'
'Alberto, R.'
'Pirmettis, I.'
'Papadopoulos, M.'
_publ_section_title
;
 (S)-(2-(2'-Pyridyl)ethyl)cysteamine and
 (S)-(2-(2'-pyridyl)ethyl)-d,l-homocysteine as ligands for the
 "fac-[M(CO)(3)](+)" (M = Re, (99m)Tc) core.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4118
_journal_page_last               4120
_journal_paper_doi               10.1021/ic050254r
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C12 H14 Br N2 O3 Re S'
_chemical_formula_weight         532.42
_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                 112.747(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.981(3)
_cell_length_b                   14.230(3)
_cell_length_c                   12.264(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.0
_cell_measurement_theta_min      5.5
_cell_volume                     1606.4(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       θ/2θ
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2965
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.188
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parall
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0647P)²+5.8883P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                2527
_reflns_number_total             2829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050254rsi20050218_092742.cif
_cod_data_source_block           rera1
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4340416
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
Re Re 0.37435(3) 0.08515(2) 0.16244(3) 0.03594(15) Uani 1 1 d .
S1 S 0.3175(2) 0.24911(14) 0.19627(19) 0.0480(5) Uani 1 1 d .
N1 N 0.5957(7) 0.1317(4) 0.1837(5) 0.0394(14) Uani 1 1 d .
N2 N 0.4722(8) 0.0896(5) 0.3572(6) 0.0435(16) Uani 1 1 d .
H2A H 0.4090 0.0641 0.3848 0.14(4) Uiso 1 1 calc R
H2B H 0.5522 0.0533 0.3821 0.14(4) Uiso 1 1 calc R
C11 C 0.2939(10) 0.0954(6) -0.0068(9) 0.050(2) Uani 1 1 d .
C12 C 0.1874(9) 0.0443(6) 0.1522(8) 0.0464(18) Uani 1 1 d .
C13 C 0.4151(10) -0.0449(7) 0.1459(8) 0.051(2) Uani 1 1 d .
C1 C 0.7075(9) 0.0746(6) 0.2463(8) 0.0432(18) Uani 1 1 d .
C2 C 0.8506(10) 0.0962(7) 0.2736(9) 0.054(2) Uani 1 1 d .
C3 C 0.8817(10) 0.1795(7) 0.2317(11) 0.064(3) Uani 1 1 d .
C4 C 0.7730(11) 0.2387(7) 0.1713(10) 0.061(2) Uani 1 1 d .
C5 C 0.6281(9) 0.2149(6) 0.1470(7) 0.0463(18) Uani 1 1 d .
C6 C 0.5082(10) 0.2826(6) 0.0819(9) 0.058(2) Uani 1 1 d .
H6A H 0.4329 0.2496 0.0184 0.10(3) Uiso 1 1 calc R
H6B H 0.5464 0.3314 0.0467 0.10(3) Uiso 1 1 calc R
C7 C 0.4423(11) 0.3276(6) 0.1613(10) 0.064(3) Uani 1 1 d .
C8 C 0.3886(12) 0.2504(7) 0.3577(9) 0.059(2) Uani 1 1 d .
C9 C 0.5131(12) 0.1845(7) 0.4104(9) 0.057(2) Uani 1 1 d .
O11 O 0.2441(9) 0.1028(6) -0.1080(6) 0.071(2) Uani 1 1 d .
O12 O 0.0741(7) 0.0174(6) 0.1440(7) 0.073(2) Uani 1 1 d .
O13 O 0.4336(10) -0.1237(5) 0.1363(9) 0.086(2) Uani 1 1 d .
H1 H 0.676(8) 0.010(5) 0.271(6) 0.026(17) Uiso 1 1 d .
H2 H 0.921(9) 0.046(6) 0.313(7) 0.034(19) Uiso 1 1 d .
H3 H 0.989(13) 0.182(8) 0.265(10) 0.08(3) Uiso 1 1 d .
H4 H 0.790(12) 0.305(8) 0.145(10) 0.08(3) Uiso 1 1 d .
H7A H 0.383(9) 0.379(6) 0.122(8) 0.04(2) Uiso 1 1 d .
H7B H 0.515(11) 0.337(6) 0.255(9) 0.06(3) Uiso 1 1 d .
H8A H 0.405(14) 0.322(9) 0.385(12) 0.10(4) Uiso 1 1 d .
H8B H 0.292(13) 0.223(8) 0.379(10) 0.08(3) Uiso 1 1 d .
H9A H 0.539(7) 0.178(5) 0.493(7) 0.023(16) Uiso 1 1 d .
H9B H 0.570(11) 0.201(7) 0.391(9) 0.05(3) Uiso 1 1 d .
Br Br 0.75917(10) -0.04679(7) 0.51730(8) 0.0530(2) Uani 1 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'
Br Br -0.2901 2.4595 '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
C12 Re C11 87.8(4)
C12 Re C13 86.7(4)
C11 Re C13 88.6(4)
C12 Re N2 95.3(3)
C11 Re N2 173.8(3)
C13 Re N2 96.8(3)
C12 Re N1 177.2(3)
C11 Re N1 94.9(3)
C13 Re N1 93.3(3)
N2 Re N1 82.0(3)
C12 Re S1 90.9(3)
C11 Re S1 94.7(3)
C13 Re S1 175.8(3)
N2 Re S1 79.94(18)
N1 Re S1 88.93(18)
C8 S1 C7 103.4(5)
C8 S1 Re 100.0(3)
C7 S1 Re 108.3(3)
C5 N1 C1 117.7(7)
C5 N1 Re 125.3(5)
C1 N1 Re 116.8(5)
C9 N2 Re 115.7(5)
O11 C11 Re 178.7(9)
O12 C12 Re 178.1(8)
O13 C13 Re 176.9(8)
N1 C1 C2 123.8(8)
C1 C2 C3 117.8(9)
C4 C3 C2 119.7(9)
C3 C4 C5 120.7(9)
N1 C5 C4 120.2(8)
N1 C5 C6 119.7(7)
C4 C5 C6 120.1(8)
C5 C6 C7 112.6(8)
C6 C7 S1 113.3(6)
C9 C8 S1 111.9(7)
N2 C9 C8 109.9(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re C12 1.912(9)
Re C11 1.919(11)
Re C13 1.922(10)
Re N2 2.204(7)
Re N1 2.223(6)
Re S1 2.474(2)
S1 C8 1.826(10)
S1 C7 1.842(11)
N1 C5 1.350(10)
N1 C1 1.354(10)
N2 C9 1.487(12)
C11 O11 1.150(13)
C12 O12 1.161(11)
C13 O13 1.150(13)
C1 C2 1.370(13)
C2 C3 1.374(14)
C3 C4 1.348(15)
C4 C5 1.400(12)
C5 C6 1.503(12)
C6 C7 1.513(16)
C8 C9 1.490(14)
