#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/94/4309421.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_4309421
loop_
_publ_author_name
'Niklaus Marti'
'Bernhard Spingler'
'Frank Breher'
'Roger Schibli'
_publ_contact_author_address
;
Department of Chemistry and Applied Biosciences
ETH Hoenggerberg
Wolgang-Pauli Str.
CH-8093 Zuerich
Switzerland
;
_publ_contact_author_email       roger.schibli@pharma.ethz.ch
_publ_contact_author_fax         '(+41) 44 633 13 67'
_publ_contact_author_name        'Prof. Dr. Roger Schibli'
_publ_section_title
;
Comparative Studies of Substitution Reactions of Rhenium(I)
Dicarbonyl-Nitrosyl and Tricarbonyl Complexes in Aqueous Media
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6082
_journal_page_last               6091
_journal_paper_doi               10.1021/ic050442h
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C13 H10 Br N3 O3 Re, C3 H6 O, Br, O'
_chemical_formula_sum            'C16 H16 Br2 N3 O5 Re'
_chemical_formula_weight         676.34
_chemical_name_common            Re(DPYM)nitrosyl
_chemical_name_systematic
; 
Bromo-dicarbonyl-nitrosyl-bromide-di(2-pyridyl)methane-rhenium
;
_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                108.679(9)
_cell_angle_beta                 111.992(9)
_cell_angle_gamma                95.426(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8236(8)
_cell_length_b                   10.0949(8)
_cell_length_c                   12.5346(10)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    183(2)
_cell_volume                     1058.82(19)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'X-RED (Stoe, 1999)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '/f oscillation 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  0.1116
_diffrn_reflns_av_sigmaI/netI    0.0653
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19274
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.77
_diffrn_standards_interval_time  4
_exptl_absorpt_coefficient_mu    9.542
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.1425
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.410
_refine_diff_density_min         -1.802
_refine_diff_density_rms         0.326
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4872
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0730
_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)+(0.1253P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1736
_reflns_number_gt                4421
_reflns_number_total             4872
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050442h__4.cif
_cod_data_source_block           6
_cod_original_cell_volume        1058.82(15)
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4309421
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
Re1 Re 0.07402(3) 0.40505(3) 0.23866(2) 0.03083(15) Uani 1 1 d . . .
C2 C 0.1753(10) 0.2767(8) 0.0286(7) 0.0401(16) Uani 1 1 d . . .
H3 H 0.0788 0.2162 -0.0089 0.048 Uiso 1 1 calc R . .
C3 C 0.2681(11) 0.2530(9) -0.0327(8) 0.0434(18) Uani 1 1 d . . .
H2 H 0.2349 0.1772 -0.1096 0.052 Uiso 1 1 calc R . .
C4 C 0.4095(11) 0.3434(9) 0.0221(8) 0.0448(18) Uani 1 1 d . . .
H4 H 0.4743 0.3293 -0.0166 0.054 Uiso 1 1 calc R . .
C5 C 0.4545(10) 0.4558(9) 0.1355(9) 0.0433(18) Uani 1 1 d . . .
H5 H 0.5500 0.5180 0.1729 0.052 Uiso 1 1 calc R . .
C6 C 0.3583(9) 0.4774(8) 0.1947(7) 0.0354(15) Uani 1 1 d . . .
C7 C 0.4031(9) 0.5978(8) 0.3158(7) 0.0349(14) Uani 1 1 d . . .
H7A H 0.5021 0.6560 0.3399 0.042 Uiso 1 1 calc R . .
H7B H 0.4123 0.5581 0.3784 0.042 Uiso 1 1 calc R . .
C8 C 0.2949(9) 0.6941(8) 0.3157(7) 0.0342(14) Uani 1 1 d . . .
C9 C 0.3457(10) 0.8410(8) 0.3490(8) 0.0408(17) Uani 1 1 d . . .
H9 H 0.4457 0.8803 0.3689 0.049 Uiso 1 1 calc R . .
C10 C 0.2446(10) 0.9286(8) 0.3520(8) 0.0425(18) Uani 1 1 d . . .
H10 H 0.2771 1.0274 0.3754 0.051 Uiso 1 1 calc R . .
C11 C 0.0971(10) 0.8682(8) 0.3204(8) 0.0393(16) Uani 1 1 d . . .
H11 H 0.0281 0.9251 0.3213 0.047 Uiso 1 1 calc R . .
C12 C 0.0524(10) 0.7212(8) 0.2869(7) 0.0380(15) Uani 1 1 d . . .
H12 H -0.0480 0.6804 0.2647 0.046 Uiso 1 1 calc R . .
C14 C -0.0724(9) 0.4387(9) 0.3181(8) 0.0387(17) Uani 1 1 d . . .
C16 C -0.0047(10) 0.1896(8) 0.1751(8) 0.0390(16) Uani 1 1 d . . .
C21 C 0.4310(14) 0.1248(10) 0.2337(10) 0.060(3) Uani 1 1 d D . .
N1 N 0.2204(8) 0.3847(6) 0.1409(6) 0.0321(12) Uani 1 1 d . . .
N13 N 0.1486(7) 0.6348(6) 0.2852(6) 0.0306(12) Uani 1 1 d . . .
N18 N 0.2113(9) 0.3996(7) 0.3780(7) 0.0424(16) Uani 1 1 d . . .
O15 O -0.1527(9) 0.4575(8) 0.3600(8) 0.0611(18) Uani 1 1 d . . .
O17 O -0.0459(9) 0.0722(7) 0.1406(7) 0.0578(17) Uani 1 1 d . . .
O19 O 0.2913(8) 0.3903(8) 0.4699(6) 0.0528(16) Uani 1 1 d . . .
O22 O 0.3186(16) 0.1479(17) 0.2284(16) 0.130(6) Uani 1 1 d . . .
O23 O -0.0233(10) 0.1893(8) 0.4280(8) 0.0626(18) Uani 1 1 d . . .
C23 C 0.574(2) 0.2074(17) 0.3463(19) 0.130(8) Uani 1 1 d D . .
H23A H 0.5692 0.1941 0.4173 0.156 Uiso 1 1 calc R . .
H23B H 0.5890 0.3080 0.3604 0.156 Uiso 1 1 calc R . .
H23C H 0.6576 0.1735 0.3341 0.156 Uiso 1 1 calc R . .
Br1 Br -0.26779(10) -0.14806(9) 0.34127(8) 0.0441(2) Uani 1 1 d . . .
Br2 Br -0.14504(10) 0.38826(9) 0.04130(8) 0.0435(2) Uani 1 1 d . . .
C22 C 0.446(3) 0.013(2) 0.1291(13) 0.146(11) Uani 1 1 d D . .
H22A H 0.4068 0.0341 0.0556 0.175 Uiso 1 1 calc R . .
H22B H 0.3906 -0.0804 0.1128 0.175 Uiso 1 1 calc R . .
H22C H 0.5511 0.0129 0.1521 0.175 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 0.0000 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N18 Re1 C16 88.9(3) . . ?
N18 Re1 C14 90.1(3) . . ?
C16 Re1 C14 90.7(3) . . ?
N18 Re1 N13 97.0(3) . . ?
C16 Re1 N13 173.5(3) . . ?
C14 Re1 N13 92.0(3) . . ?
N18 Re1 N1 95.6(3) . . ?
C16 Re1 N1 93.1(3) . . ?
C14 Re1 N1 173.2(3) . . ?
N13 Re1 N1 83.6(2) . . ?
N18 Re1 Br2 172.6(2) . . ?
C16 Re1 Br2 85.3(3) . . ?
C14 Re1 Br2 85.4(3) . . ?
N13 Re1 Br2 89.07(17) . . ?
N1 Re1 Br2 89.29(18) . . ?
N1 C2 C3 122.2(8) . . ?
C4 C3 C2 118.7(7) . . ?
C3 C4 C5 119.1(7) . . ?
C4 C5 C6 120.8(8) . . ?
N1 C6 C5 119.3(7) . . ?
N1 C6 C7 118.7(6) . . ?
C5 C6 C7 122.0(7) . . ?
C6 C7 C8 114.5(6) . . ?
N13 C8 C9 121.1(7) . . ?
N13 C8 C7 118.7(6) . . ?
C9 C8 C7 120.1(7) . . ?
C8 C9 C10 119.1(8) . . ?
C11 C10 C9 119.5(7) . . ?
C10 C11 C12 118.9(7) . . ?
N13 C12 C11 122.6(8) . . ?
O15 C14 Re1 179.2(9) . . ?
O17 C16 Re1 179.1(8) . . ?
O22 C21 C23 121.0(16) . . ?
O22 C21 C22 123.1(17) . . ?
C23 C21 C22 115.8(17) . . ?
C2 N1 C6 119.8(7) . . ?
C2 N1 Re1 120.0(5) . . ?
C6 N1 Re1 120.2(5) . . ?
C12 N13 C8 118.7(6) . . ?
C12 N13 Re1 121.0(5) . . ?
C8 N13 Re1 120.2(5) . . ?
O19 N18 Re1 174.4(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
Re1 N18 1.784(8) . ?
Re1 C16 2.018(7) . ?
Re1 C14 2.030(7) . ?
Re1 N13 2.179(6) . ?
Re1 N1 2.197(6) . ?
Re1 Br2 2.5407(10) . ?
C2 N1 1.351(9) . ?
C2 C3 1.388(11) . ?
C3 C4 1.371(13) . ?
C4 C5 1.380(13) . ?
C5 C6 1.397(11) . ?
C6 N1 1.356(10) . ?
C6 C7 1.480(10) . ?
C7 C8 1.506(11) . ?
C8 N13 1.360(9) . ?
C8 C9 1.389(10) . ?
C9 C10 1.394(12) . ?
C10 C11 1.370(12) . ?
C11 C12 1.382(10) . ?
C12 N13 1.346(10) . ?
C14 O15 1.100(10) . ?
C16 O17 1.098(9) . ?
C21 O22 1.132(15) . ?
C21 C23 1.486(15) . ?
C21 C22 1.500(14) . ?
N18 O19 1.166(10) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 C4 -0.8(13) . . . . ?
C2 C3 C4 C5 -0.7(13) . . . . ?
C3 C4 C5 C6 0.4(13) . . . . ?
C4 C5 C6 N1 1.3(13) . . . . ?
C4 C5 C6 C7 -179.4(8) . . . . ?
N1 C6 C7 C8 -56.0(10) . . . . ?
C5 C6 C7 C8 124.7(8) . . . . ?
C6 C7 C8 N13 58.8(9) . . . . ?
C6 C7 C8 C9 -122.6(8) . . . . ?
N13 C8 C9 C10 0.6(12) . . . . ?
C7 C8 C9 C10 -178.0(7) . . . . ?
C8 C9 C10 C11 -1.0(12) . . . . ?
C9 C10 C11 C12 0.5(12) . . . . ?
C10 C11 C12 N13 0.6(12) . . . . ?
C3 C2 N1 C6 2.5(12) . . . . ?
C3 C2 N1 Re1 -175.2(6) . . . . ?
C5 C6 N1 C2 -2.7(12) . . . . ?
C7 C6 N1 C2 178.0(7) . . . . ?
C5 C6 N1 Re1 175.0(6) . . . . ?
C7 C6 N1 Re1 -4.3(10) . . . . ?
N18 Re1 N1 C2 123.8(6) . . . . ?
C16 Re1 N1 C2 34.6(6) . . . . ?
N13 Re1 N1 C2 -139.8(6) . . . . ?
Br2 Re1 N1 C2 -50.6(6) . . . . ?
N18 Re1 N1 C6 -54.0(6) . . . . ?
C16 Re1 N1 C6 -143.2(6) . . . . ?
N13 Re1 N1 C6 42.5(6) . . . . ?
Br2 Re1 N1 C6 131.6(6) . . . . ?
C11 C12 N13 C8 -1.1(11) . . . . ?
C11 C12 N13 Re1 177.6(6) . . . . ?
C9 C8 N13 C12 0.4(11) . . . . ?
C7 C8 N13 C12 179.0(7) . . . . ?
C9 C8 N13 Re1 -178.2(6) . . . . ?
C7 C8 N13 Re1 0.4(9) . . . . ?
N18 Re1 N13 C12 -123.6(6) . . . . ?
C14 Re1 N13 C12 -33.2(6) . . . . ?
N1 Re1 N13 C12 141.5(6) . . . . ?
Br2 Re1 N13 C12 52.1(6) . . . . ?
N18 Re1 N13 C8 55.0(6) . . . . ?
C14 Re1 N13 C8 145.3(6) . . . . ?
N1 Re1 N13 C8 -39.9(6) . . . . ?
Br2 Re1 N13 C8 -129.3(5) . . . . ?
