#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:01:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179737 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/33/7003325.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_7003325
loop_
_publ_author_name
'Pérez, Julio'
'Riera, Lucía'
'Ion, Laura'
'Riera, Víctor'
'Anderson, Kirsty M.'
'Steed, Jonathan W.'
'Miguel, Daniel'
_publ_section_title
;
 Second-sphere interaction of anions with a weakly binding metal
 complex host: probing the effect of counteranions
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              878
_journal_page_last               886
_journal_paper_doi               10.1039/b715599A
_journal_year                    2008
_chemical_formula_moiety         'C15 H18 N6 O3 Re, C F3 O3 S'
_chemical_formula_sum            'C16 H18 F3 N6 O6 Re S'
_chemical_formula_weight         665.62
_chemical_name_systematic
;
?
;
_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                95.450(2)
_cell_angle_beta                 98.829(2)
_cell_angle_gamma                90.805(2)
_cell_formula_units_Z            2
_cell_length_a                   7.0294(8)
_cell_length_b                   12.1099(14)
_cell_length_c                   13.4786(16)
_cell_measurement_temperature    120(2)
_cell_volume                     1128.2(2)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    X-Seed
_computing_publication_material  X-Seed
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SMART 1k'
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15709
_diffrn_reflns_theta_full        29.17
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    5.548
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.560656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABs
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         6034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0234
_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)+(0.0201P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0484
_reflns_number_gt                5375
_reflns_number_total             6034
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715599A.txt
_cod_data_source_block           Compound_1_(li418)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P-1
_cod_database_code               7003325
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 0.437711(16) 0.230999(9) 0.135342(8) 0.01230(4) Uani 1 1 d . . .
S1 S 0.30873(11) 0.27794(6) 0.62559(6) 0.01924(15) Uani 1 1 d . . .
F1 F 0.6531(3) 0.2513(2) 0.72314(18) 0.0471(6) Uani 1 1 d . . .
F2 F 0.4349(4) 0.2726(3) 0.81818(16) 0.0584(7) Uani 1 1 d . . .
F3 F 0.4513(4) 0.1176(2) 0.7281(2) 0.0580(7) Uani 1 1 d . . .
O1 O 0.7010(3) 0.0528(2) 0.05859(18) 0.0308(6) Uani 1 1 d . . .
O2 O 0.6634(3) 0.3928(2) 0.03247(18) 0.0298(5) Uani 1 1 d . . .
O3 O 0.1509(3) 0.17847(18) -0.05930(17) 0.0272(5) Uani 1 1 d . . .
O4 O 0.3844(4) 0.2317(2) 0.53795(18) 0.0384(6) Uani 1 1 d . . .
O5 O 0.3310(4) 0.39573(19) 0.6453(2) 0.0340(6) Uani 1 1 d . . .
O6 O 0.1236(3) 0.2333(2) 0.63735(18) 0.0326(6) Uani 1 1 d . . .
N1 N 0.2477(3) 0.3599(2) 0.18733(18) 0.0147(5) Uani 1 1 d . . .
N2 N 0.0721(4) 0.5088(2) 0.18010(19) 0.0184(5) Uani 1 1 d . . .
N3 N 0.2856(3) 0.1162(2) 0.21591(18) 0.0159(5) Uani 1 1 d . . .
N4 N 0.2033(3) 0.0185(2) 0.33301(18) 0.0157(5) Uani 1 1 d . . .
N5 N 0.6176(3) 0.2656(2) 0.28239(18) 0.0154(5) Uani 1 1 d . . .
N6 N 0.7395(4) 0.3406(2) 0.43378(18) 0.0186(5) Uani 1 1 d . . .
C1 C 0.6011(4) 0.1185(3) 0.0894(2) 0.0204(6) Uani 1 1 d . . .
C2 C 0.5771(4) 0.3324(3) 0.0715(2) 0.0183(6) Uani 1 1 d . . .
C3 C 0.2603(4) 0.1982(2) 0.0131(2) 0.0169(6) Uani 1 1 d . . .
C11 C 0.2156(4) 0.4537(2) 0.1441(2) 0.0194(6) Uani 1 1 d . . .
H11 H 0.2848 0.4784 0.0947 0.023 Uiso 1 1 calc R . .
C12 C 0.1188(4) 0.3566(3) 0.2539(2) 0.0218(6) Uani 1 1 d . . .
H12 H 0.1078 0.2993 0.2963 0.026 Uiso 1 1 calc R . .
C13 C 0.0091(4) 0.4483(3) 0.2497(2) 0.0215(6) Uani 1 1 d . . .
H13 H -0.0914 0.4665 0.2876 0.026 Uiso 1 1 calc R . .
C14 C -0.0093(5) 0.6115(3) 0.1463(3) 0.0275(7) Uani 1 1 d . . .
H14A H 0.0673 0.6399 0.0988 0.041 Uiso 1 1 calc R . .
H14B H -0.0076 0.6666 0.2046 0.041 Uiso 1 1 calc R . .
H14C H -0.1423 0.5968 0.1127 0.041 Uiso 1 1 calc R . .
C21 C 0.3135(4) 0.1028(2) 0.3131(2) 0.0168(6) Uani 1 1 d . . .
H21 H 0.4004 0.1470 0.3626 0.020 Uiso 1 1 calc R . .
C22 C 0.1507(4) 0.0347(2) 0.1711(2) 0.0191(6) Uani 1 1 d . . .
H22 H 0.1015 0.0232 0.1012 0.023 Uiso 1 1 calc R . .
C23 C 0.1001(4) -0.0258(2) 0.2430(2) 0.0187(6) Uani 1 1 d . . .
H23 H 0.0107 -0.0869 0.2330 0.022 Uiso 1 1 calc R . .
C24 C 0.2111(5) -0.0254(3) 0.4307(2) 0.0242(7) Uani 1 1 d . . .
H24A H 0.3096 -0.0818 0.4375 0.036 Uiso 1 1 calc R . .
H24B H 0.0854 -0.0588 0.4354 0.036 Uiso 1 1 calc R . .
H24C H 0.2434 0.0350 0.4847 0.036 Uiso 1 1 calc R . .
C31 C 0.6105(4) 0.3505(2) 0.3512(2) 0.0168(6) Uani 1 1 d . . .
H31 H 0.5253 0.4103 0.3431 0.020 Uiso 1 1 calc R . .
C32 C 0.7588(4) 0.1973(2) 0.3242(2) 0.0188(6) Uani 1 1 d . . .
H32 H 0.7966 0.1295 0.2924 0.023 Uiso 1 1 calc R . .
C33 C 0.8344(4) 0.2437(3) 0.4184(2) 0.0202(6) Uani 1 1 d . . .
H33 H 0.9330 0.2147 0.4643 0.024 Uiso 1 1 calc R . .
C34 C 0.7674(5) 0.4171(3) 0.5262(2) 0.0274(7) Uani 1 1 d . . .
H34A H 0.7555 0.4936 0.5086 0.041 Uiso 1 1 calc R . .
H34B H 0.8958 0.4078 0.5641 0.041 Uiso 1 1 calc R . .
H34C H 0.6695 0.4008 0.5677 0.041 Uiso 1 1 calc R . .
C41 C 0.4697(5) 0.2269(3) 0.7293(3) 0.0311(8) 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'
Re Re -1.0185 7.2310 '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'
F F 0.0171 0.0103 '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
C2 Re1 C3 90.34(12) . . ?
C2 Re1 C1 87.01(13) . . ?
C3 Re1 C1 89.26(12) . . ?
C2 Re1 N5 94.24(11) . . ?
C3 Re1 N5 174.61(10) . . ?
C1 Re1 N5 93.80(11) . . ?
C2 Re1 N1 93.14(11) . . ?
C3 Re1 N1 90.30(10) . . ?
C1 Re1 N1 179.54(11) . . ?
N5 Re1 N1 86.63(9) . . ?
C2 Re1 N3 177.31(11) . . ?
C3 Re1 N3 92.34(11) . . ?
C1 Re1 N3 93.24(11) . . ?
N5 Re1 N3 83.07(9) . . ?
N1 Re1 N3 86.63(9) . . ?
O5 S1 O4 114.72(16) . . ?
O5 S1 O6 114.87(15) . . ?
O4 S1 O6 115.27(15) . . ?
O5 S1 C41 103.53(17) . . ?
O4 S1 C41 103.11(16) . . ?
O6 S1 C41 102.93(15) . . ?
C11 N1 C12 105.8(2) . . ?
C11 N1 Re1 123.26(19) . . ?
C12 N1 Re1 130.1(2) . . ?
C11 N2 C13 107.8(2) . . ?
C11 N2 C14 126.0(3) . . ?
C13 N2 C14 126.1(3) . . ?
C21 N3 C22 105.7(2) . . ?
C21 N3 Re1 128.50(19) . . ?
C22 N3 Re1 125.59(19) . . ?
C21 N4 C23 107.3(2) . . ?
C21 N4 C24 125.7(3) . . ?
C23 N4 C24 126.6(2) . . ?
C31 N5 C32 106.1(2) . . ?
C31 N5 Re1 128.4(2) . . ?
C32 N5 Re1 125.44(19) . . ?
C31 N6 C33 108.0(2) . . ?
C31 N6 C34 126.0(3) . . ?
C33 N6 C34 126.0(3) . . ?
O1 C1 Re1 177.4(3) . . ?
O2 C2 Re1 179.1(3) . . ?
O3 C3 Re1 178.7(3) . . ?
N1 C11 N2 110.7(3) . . ?
C13 C12 N1 109.4(3) . . ?
C12 C13 N2 106.3(3) . . ?
N3 C21 N4 111.3(3) . . ?
C23 C22 N3 109.2(3) . . ?
C22 C23 N4 106.5(3) . . ?
N5 C31 N6 110.9(3) . . ?
C33 C32 N5 108.7(3) . . ?
C32 C33 N6 106.3(3) . . ?
F3 C41 F2 108.2(3) . . ?
F3 C41 F1 107.8(3) . . ?
F2 C41 F1 107.3(3) . . ?
F3 C41 S1 111.2(3) . . ?
F2 C41 S1 111.5(2) . . ?
F1 C41 S1 110.7(2) . . ?
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 C2 1.906(3) . ?
Re1 C3 1.912(3) . ?
Re1 C1 1.914(3) . ?
Re1 N5 2.182(2) . ?
Re1 N1 2.202(2) . ?
Re1 N3 2.204(2) . ?
S1 O5 1.428(2) . ?
S1 O4 1.438(2) . ?
S1 O6 1.439(2) . ?
S1 C41 1.821(4) . ?
F1 C41 1.335(4) . ?
F2 C41 1.330(4) . ?
F3 C41 1.326(4) . ?
O1 C1 1.158(4) . ?
O2 C2 1.157(4) . ?
O3 C3 1.150(4) . ?
N1 C11 1.332(4) . ?
N1 C12 1.372(4) . ?
N2 C11 1.344(4) . ?
N2 C13 1.364(4) . ?
N2 C14 1.458(4) . ?
N3 C21 1.320(4) . ?
N3 C22 1.386(4) . ?
N4 C21 1.344(4) . ?
N4 C23 1.372(4) . ?
N4 C24 1.460(4) . ?
N5 C31 1.324(4) . ?
N5 C32 1.388(4) . ?
N6 C31 1.339(4) . ?
N6 C33 1.373(4) . ?
N6 C34 1.466(4) . ?
C12 C13 1.362(4) . ?
C22 C23 1.355(4) . ?
C32 C33 1.364(4) . ?
