#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:57:47 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180116 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/14/7101494.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_7101494
loop_
_publ_author_name
'Richard S. Herrick'
'Tim J. Brunker'
'Caroline Maus'
'Kerianne Crandall'
'Anil Cetin'
'Christopher J. Ziegler'
_publ_section_title
;
Aqueous preparation and physiological stability studies of
Re(CO)3(tripodal) compounds
;
_journal_issue                   41
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b608683g
_journal_year                    2006
_chemical_formula_sum            'C13 H9 N6 O6 Re S'
_chemical_formula_weight         563.52
_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                 96.909(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8316(17)
_cell_length_b                   8.9876(17)
_cell_length_c                   20.941(4)
_cell_measurement_reflns_used    2808
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.41
_cell_volume                     1650.1(5)
_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 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14220
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    7.539
_exptl_absorpt_correction_T_max  0.5194
_exptl_absorpt_correction_T_min  0.3015
_exptl_absorpt_correction_type   'Empirical SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.114
_refine_diff_density_min         -2.187
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0150P)²+8.2948P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                3348
_reflns_number_total             3962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b608683g.txt
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7101494
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
C1 C 1.0961(7) 1.1360(7) 0.0717(3) 0.0119(12) Uani 1 1 d .
H1 H 1.0685 1.2382 0.0699 0.014 Uiso 1 1 calc R
C2 C 1.2068(7) 1.0714(7) 0.0378(3) 0.0138(13) Uani 1 1 d .
H2 H 1.2673 1.1208 0.0098 0.017 Uiso 1 1 calc R
C3 C 1.2104(7) 0.9238(7) 0.0529(3) 0.0141(13) Uani 1 1 d .
H3 H 1.2737 0.8501 0.0373 0.017 Uiso 1 1 calc R
C4 C 1.0641(7) 0.8532(7) 0.2874(3) 0.0158(13) Uani 1 1 d .
H4 H 1.0429 0.9156 0.3219 0.019 Uiso 1 1 calc R
C5 C 1.1327(7) 0.7128(7) 0.2946(3) 0.0154(13) Uani 1 1 d .
H5 H 1.1655 0.6630 0.3339 0.018 Uiso 1 1 calc R
C6 C 1.1427(7) 0.6629(7) 0.2348(3) 0.0139(13) Uani 1 1 d .
H6 H 1.1835 0.5697 0.2240 0.017 Uiso 1 1 calc R
C7 C 0.6518(7) 0.7991(7) 0.1109(3) 0.0145(13) Uani 1 1 d .
H7 H 0.5609 0.8464 0.1203 0.017 Uiso 1 1 calc R
C8 C 0.6557(7) 0.6681(7) 0.0768(3) 0.0134(13) Uani 1 1 d .
H8 H 0.5705 0.6108 0.0590 0.016 Uiso 1 1 calc R
C9 C 0.8054(7) 0.6374(7) 0.0736(3) 0.0141(13) Uani 1 1 d .
H9 H 0.8451 0.5536 0.0535 0.017 Uiso 1 1 calc R
C10 C 1.0532(6) 0.7629(7) 0.1227(3) 0.0101(12) Uani 1 1 d .
C11 C 0.9798(6) 1.2198(7) 0.2234(3) 0.0122(12) Uani 1 1 d .
C12 C 0.7427(7) 1.1845(7) 0.1284(3) 0.0178(14) Uani 1 1 d .
C13 C 0.7518(7) 1.0474(7) 0.2456(3) 0.0163(13) Uani 1 1 d .
N1 N 1.0352(6) 1.0334(5) 0.1069(2) 0.0134(11) Uani 1 1 d .
N2 N 1.1056(6) 0.9024(5) 0.0948(2) 0.0114(10) Uani 1 1 d .
N3 N 1.0327(5) 0.8865(5) 0.2255(2) 0.0108(10) Uani 1 1 d .
N4 N 1.0850(5) 0.7679(5) 0.1928(2) 0.0099(10) Uani 1 1 d .
N5 N 0.7923(5) 0.8510(6) 0.1290(2) 0.0107(10) Uani 1 1 d .
N6 N 0.8879(5) 0.7497(5) 0.1050(2) 0.0092(10) Uani 1 1 d .
O1 O 1.3149(5) 0.6341(5) 0.1145(2) 0.0157(9) Uani 1 1 d .
O2 O 1.1200(5) 0.6222(4) 0.02169(19) 0.0137(9) Uani 1 1 d .
O3 O 1.0941(5) 0.4747(4) 0.1176(2) 0.0146(9) Uani 1 1 d .
O4 O 1.0375(5) 1.3156(5) 0.2529(2) 0.0195(10) Uani 1 1 d .
O5 O 0.6584(6) 1.2612(6) 0.0980(2) 0.0311(12) Uani 1 1 d .
O6 O 0.6780(5) 1.0466(5) 0.2874(2) 0.0215(10) Uani 1 1 d .
Re1 Re 0.88032(3) 1.05183(3) 0.178051(11) 0.01101(8) Uani 1 1 d .
S1 S 1.15820(17) 0.60196(16) 0.08997(7) 0.0115(3) 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'
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
N1 C1 C2 110.3(5)
C3 C2 C1 106.5(5)
N2 C3 C2 106.8(5)
N3 C4 C5 110.2(6)
C6 C5 C4 106.0(6)
C5 C6 N4 108.2(6)
N5 C7 C8 111.4(5)
C9 C8 C7 106.5(6)
C8 C9 N6 107.0(5)
N4 C10 N6 108.8(4)
N4 C10 N2 109.8(5)
N6 C10 N2 108.5(5)
N4 C10 S1 110.1(4)
N6 C10 S1 111.3(4)
N2 C10 S1 108.4(4)
O4 C11 Re1 176.6(5)
O5 C12 Re1 178.4(6)
O6 C13 Re1 178.0(5)
C1 N1 N2 105.7(5)
C1 N1 Re1 131.6(4)
N2 N1 Re1 122.4(4)
C3 N2 N1 110.8(5)
C3 N2 C10 129.9(5)
N1 N2 C10 119.0(5)
C4 N3 N4 105.6(5)
C4 N3 Re1 130.4(4)
N4 N3 Re1 122.1(4)
C6 N4 N3 109.9(5)
C6 N4 C10 130.2(5)
N3 N4 C10 119.2(5)
C7 N5 N6 104.7(5)
C7 N5 Re1 133.7(4)
N6 N5 Re1 121.4(3)
C9 N6 N5 110.4(5)
C9 N6 C10 129.6(5)
N5 N6 C10 119.3(4)
C12 Re1 C13 91.1(3)
C12 Re1 C11 90.1(3)
C13 Re1 C11 85.9(3)
C12 Re1 N1 95.0(2)
C13 Re1 N1 173.5(2)
C11 Re1 N1 96.4(2)
C12 Re1 N3 174.0(2)
C13 Re1 N3 92.2(2)
C11 Re1 N3 95.2(2)
N1 Re1 N3 81.53(19)
C12 Re1 N5 95.3(2)
C13 Re1 N5 97.0(2)
C11 Re1 N5 173.8(2)
N1 Re1 N5 80.21(18)
N3 Re1 N5 79.27(18)
O3 S1 O2 116.5(3)
O3 S1 O1 115.1(3)
O2 S1 O1 115.3(3)
O3 S1 C10 103.3(3)
O2 S1 C10 101.3(2)
O1 S1 C10 102.0(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.333(7)
C1 C2 1.401(8)
C2 C3 1.364(8)
C3 N2 1.363(8)
C4 N3 1.328(8)
C4 C5 1.400(9)
C5 C6 1.343(8)
C6 N4 1.348(8)
C7 N5 1.337(8)
C7 C8 1.379(9)
C8 C9 1.361(8)
C9 N6 1.366(7)
C10 N4 1.462(7)
C10 N6 1.467(7)
C10 N2 1.480(7)
C10 S1 1.890(6)
C11 O4 1.143(7)
C11 Re1 1.937(6)
C12 O5 1.149(8)
C12 Re1 1.918(7)
C13 O6 1.152(8)
C13 Re1 1.918(7)
N1 N2 1.370(7)
N1 Re1 2.147(5)
N3 N4 1.376(7)
N3 Re1 2.165(5)
N5 N6 1.378(6)
N5 Re1 2.174(5)
O1 S1 1.446(4)
O2 S1 1.441(4)
O3 S1 1.430(4)
