#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:43:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179761 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/57/7005779.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_7005779
loop_
_publ_author_name
'Maria, Leonor'
'Cunha, Susana'
'Videira, Margarida'
'Gano, Lurdes'
'Paulo, António'
'Santos, Isabel C.'
'Santos, Isabel'
_publ_section_title
;
 Rhenium and technetium tricarbonyl complexes anchored by
 pyrazole-based tripods: novel lead structures for the design of
 myocardial imaging agents.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3010
_journal_page_last               3019
_journal_paper_doi               10.1039/b705226j
_journal_year                    2007
_chemical_formula_moiety         'C11 H11 N5 O3 Re, C H4 O, Br'
_chemical_formula_sum            'C12 H15 Br N5 O4 Re'
_chemical_formula_weight         559.40
_chemical_name_common            (Re(CO)3(NH2CH2CH(pz)2))Br
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000(10)
_cell_angle_beta                 110.3190(10)
_cell_angle_gamma                90.0000(10)
_cell_formula_units_Z            4
_cell_length_a                   12.5900(2)
_cell_length_b                   10.0842(2)
_cell_length_c                   14.5569(2)
_cell_measurement_temperature    130(2)
_cell_volume                     1733.14(5)
_computing_cell_refinement       'Bruker SMART, (Bruker, 2004)'
_computing_data_collection       'Bruker SMART, (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT, (Bruker, 2004)'
_computing_molecular_graphics    ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker-AXS APEX- CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15143
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    9.342
_exptl_absorpt_correction_T_max  0.2566
_exptl_absorpt_correction_T_min  0.1178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.635
_refine_diff_density_min         -2.585
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0444P)²+0.1234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0938
_reflns_number_gt                2995
_reflns_number_total             3529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b705226j.txt
_cod_data_source_block           rebr
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7005779
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.38348(4) -0.06112(5) 0.29736(4) 0.02394(14) Uani 1 1 d . . .
Re1 Re 0.719327(14) 0.001742(14) 0.256272(13) 0.01102(10) Uani 1 1 d . . .
C1 C 0.5909(4) -0.0674(5) 0.1518(4) 0.0187(10) Uani 1 1 d . . .
C2 C 0.8182(4) -0.1230(5) 0.2257(3) 0.0174(10) Uani 1 1 d . . .
C3 C 0.7446(4) 0.1200(5) 0.1619(4) 0.0180(10) Uani 1 1 d . . .
O1 O 0.5135(3) -0.1048(4) 0.0886(3) 0.0293(9) Uani 1 1 d . . .
O2 O 0.8762(3) -0.2000(4) 0.2089(3) 0.0309(9) Uani 1 1 d . . .
O3 O 0.7633(3) 0.1846(4) 0.1038(3) 0.0279(8) Uani 1 1 d . . .
N1 N 0.6973(3) -0.1261(4) 0.3689(3) 0.0121(7) Uani 1 1 d . . .
N2 N 0.7055(3) -0.0773(4) 0.4582(3) 0.0168(9) Uani 1 1 d . . .
N3 N 0.8499(3) 0.0918(4) 0.3801(3) 0.0142(8) Uani 1 1 d . . .
N4 N 0.8386(3) 0.0960(4) 0.4708(3) 0.0143(8) Uani 1 1 d . . .
N5 N 0.6079(3) 0.1306(4) 0.3088(3) 0.0151(8) Uani 1 1 d . . .
H5A H 0.6044 0.2122 0.2797 0.018 Uiso 1 1 calc R . .
H5B H 0.5362 0.0951 0.2852 0.018 Uiso 1 1 calc R . .
C4 C 0.6772(4) -0.2555(4) 0.3722(4) 0.0170(9) Uani 1 1 d . . .
H4 H 0.6693 -0.3164 0.3204 0.020 Uiso 1 1 calc R . .
C5 C 0.6695(4) -0.2888(5) 0.4631(4) 0.0267(12) Uani 1 1 d . . .
H5 H 0.6547 -0.3738 0.4840 0.032 Uiso 1 1 calc R . .
C6 C 0.6879(4) -0.1726(5) 0.5157(4) 0.0250(11) Uani 1 1 d . . .
H6 H 0.6880 -0.1618 0.5805 0.030 Uiso 1 1 calc R . .
C7 C 0.7291(4) 0.0629(5) 0.4796(4) 0.0148(10) Uani 1 1 d . . .
H7 H 0.7358 0.0778 0.5493 0.018 Uiso 1 1 calc R . .
C8 C 0.6361(4) 0.1538(5) 0.4161(3) 0.0159(9) Uani 1 1 d . . .
H8B H 0.5671 0.1404 0.4328 0.019 Uiso 1 1 calc R . .
H8A H 0.6604 0.2471 0.4313 0.019 Uiso 1 1 calc R . .
C9 C 0.9313(4) 0.1499(5) 0.5384(4) 0.0198(10) Uani 1 1 d . . .
H9 H 0.9431 0.1647 0.6057 0.024 Uiso 1 1 calc R . .
C10 C 1.0055(4) 0.1793(6) 0.4903(4) 0.0218(12) Uani 1 1 d . . .
H10 H 1.0788 0.2171 0.5182 0.026 Uiso 1 1 calc R . .
C11 C 0.9515(4) 0.1423(5) 0.3921(4) 0.0188(10) Uani 1 1 d . . .
H11 H 0.9828 0.1520 0.3417 0.023 Uiso 1 1 calc R . .
O4 O 0.1113(4) -0.0494(7) 0.2574(4) 0.0561(14) Uani 1 1 d . . .
H4A H 0.1818 -0.0516 0.2713 0.084 Uiso 1 1 calc R . .
C12 C 0.0595(7) 0.0101(6) 0.1632(6) 0.0431(18) Uani 1 1 d . . .
H12A H 0.0244 0.0944 0.1703 0.065 Uiso 1 1 calc R . .
H12B H 0.0015 -0.0496 0.1211 0.065 Uiso 1 1 calc R . .
H12C H 0.1172 0.0264 0.1334 0.065 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
C1 Re1 C3 87.8(2) . . ?
C1 Re1 C2 90.8(2) . . ?
C3 Re1 C2 87.7(2) . . ?
C1 Re1 N3 173.24(16) . . ?
C3 Re1 N3 93.91(17) . . ?
C2 Re1 N3 95.79(17) . . ?
C1 Re1 N1 95.09(17) . . ?
C3 Re1 N1 177.02(16) . . ?
C2 Re1 N1 92.78(17) . . ?
N3 Re1 N1 83.11(14) . . ?
C1 Re1 N5 91.51(17) . . ?
C3 Re1 N5 99.37(17) . . ?
C2 Re1 N5 172.64(16) . . ?
N3 Re1 N5 81.77(13) . . ?
N1 Re1 N5 80.05(14) . . ?
O1 C1 Re1 177.9(4) . . ?
O2 C2 Re1 178.1(4) . . ?
O3 C3 Re1 175.8(4) . . ?
C4 N1 N2 105.8(4) . . ?
C4 N1 Re1 133.0(3) . . ?
N2 N1 Re1 121.2(3) . . ?
C6 N2 N1 111.3(4) . . ?
C6 N2 C7 128.9(4) . . ?
N1 N2 C7 119.9(4) . . ?
C11 N3 N4 106.0(4) . . ?
C11 N3 Re1 133.2(3) . . ?
N4 N3 Re1 120.6(3) . . ?
C9 N4 N3 111.1(4) . . ?
C9 N4 C7 128.9(4) . . ?
N3 N4 C7 119.3(4) . . ?
C8 N5 Re1 120.0(3) . . ?
N1 C4 C5 110.2(4) . . ?
C6 C5 C4 105.6(4) . . ?
N2 C6 C5 107.2(4) . . ?
N2 C7 N4 109.3(3) . . ?
N2 C7 C8 113.5(4) . . ?
N4 C7 C8 111.0(4) . . ?
N5 C8 C7 113.2(4) . . ?
N4 C9 C10 106.4(4) . . ?
C9 C10 C11 106.7(4) . . ?
N3 C11 C10 109.8(4) . . ?
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 C1 1.925(5) . ?
Re1 C3 1.927(5) . ?
Re1 C2 1.927(5) . ?
Re1 N3 2.172(4) . ?
Re1 N1 2.177(4) . ?
Re1 N5 2.233(4) . ?
C1 O1 1.147(6) . ?
C2 O2 1.149(6) . ?
C3 O3 1.156(6) . ?
N1 C4 1.334(6) . ?
N1 N2 1.360(5) . ?
N2 C6 1.342(6) . ?
N2 C7 1.455(7) . ?
N3 C11 1.331(6) . ?
N3 N4 1.377(5) . ?
N4 C9 1.352(6) . ?
N4 C7 1.467(6) . ?
N5 C8 1.495(6) . ?
C4 C5 1.401(7) . ?
C5 C6 1.375(7) . ?
C7 C8 1.521(6) . ?
C9 C10 1.379(7) . ?
C10 C11 1.404(7) . ?
O4 C12 1.431(9) . ?
