#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:01:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179737 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/33/7003328.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_7003328
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, H O4 S, C H2 Cl2'
_chemical_formula_sum            'C16 H21 Cl2 N6 O7 Re S'
_chemical_formula_weight         698.55
_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                97.15(3)
_cell_angle_beta                 96.72(3)
_cell_angle_gamma                107.55(3)
_cell_formula_units_Z            2
_cell_length_a                   7.1111(14)
_cell_length_b                   10.866(2)
_cell_length_c                   16.743(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1207.5(5)
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_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      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0966
_diffrn_reflns_av_sigmaI/netI    0.1031
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6292
_diffrn_reflns_theta_full        68.87
_diffrn_reflns_theta_max         68.87
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    13.129
_exptl_absorpt_correction_T_max  1.467
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.837
_refine_diff_density_min         -2.946
_refine_diff_density_rms         0.363
_refine_ls_extinction_coef       0.0047(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0697
_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)+(0.1546P)²+3.7547P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1880
_refine_ls_wR_factor_ref         0.2310
_reflns_number_gt                3963
_reflns_number_total             4407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715599A.txt
_cod_data_source_block           Compound_6_(li387)
_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.

'_exptl_absorpt_correction_type' value 'multi scan' changed
to 'multi-scan' 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_cell_volume        1207.5(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003328
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 0.60555(5) 0.10177(4) 0.32705(2) 0.0307(3) Uani 1 1 d . . .
Cl91 Cl 0.4519(5) 0.6548(4) 0.4380(2) 0.0662(9) Uani 1 1 d . . .
Cl92 Cl 0.0428(6) 0.4977(3) 0.3672(2) 0.0626(9) Uani 1 1 d . . .
S2 S 0.4411(4) 0.3041(3) -0.00187(17) 0.0395(6) Uani 1 1 d . . .
O1 O 0.4944(13) 0.3534(8) 0.3427(5) 0.0475(19) Uani 1 1 d . . .
O2 O 0.3123(13) 0.0056(10) 0.4457(5) 0.051(2) Uani 1 1 d . . .
O3 O 0.9364(13) 0.2399(8) 0.4742(5) 0.049(2) Uani 1 1 d . . .
O11 O 0.4780(13) 0.3102(10) 0.0855(6) 0.054(2) Uani 1 1 d . . .
O12 O 0.2948(11) 0.3664(8) -0.0269(5) 0.0413(17) Uani 1 1 d . . .
O13 O 0.6397(8) 0.3863(4) -0.0277(2) 0.048(2) Uani 1 1 d G . .
O14 O 0.3951(7) 0.1752(5) -0.04902(19) 0.062(3) Uani 1 1 d G . .
N1 N 0.8143(4) 0.1720(3) 0.24303(18) 0.0344(19) Uani 1 1 d G . .
N2 N 0.9864(5) 0.3102(4) 0.1741(2) 0.039(2) Uani 1 1 d G . .
N3 N 0.3802(4) -0.0078(3) 0.22087(19) 0.0349(19) Uani 1 1 d G . .
N4 N 0.2165(5) -0.0841(3) 0.0966(2) 0.0319(18) Uani 1 1 d G . .
N5 N 0.6980(5) -0.0731(3) 0.3135(2) 0.038(2) Uani 1 1 d G . .
N6 N 0.7231(8) -0.2675(4) 0.2744(3) 0.0339(18) Uani 1 1 d G . .
C1 C 0.5322(6) 0.2549(3) 0.33584(19) 0.035(2) Uani 1 1 d G . .
C2 C 0.4171(6) 0.0396(4) 0.3996(2) 0.041(3) Uani 1 1 d G . .
C3 C 0.8125(6) 0.1892(4) 0.41774(17) 0.044(3) Uani 1 1 d G . .
C11 C 0.8195(4) 0.2704(3) 0.2044(2) 0.030(2) Uani 1 1 d G . .
H11 H 0.7156 0.3085 0.1989 0.036 Uiso 1 1 calc R . .
C12 C 0.9896(17) 0.1445(12) 0.2350(8) 0.046(3) Uani 1 1 d . . .
H12 H 1.0277 0.0771 0.2565 0.055 Uiso 1 1 calc R . .
C13 C 1.0998(17) 0.2298(12) 0.1911(7) 0.042(2) Uani 1 1 d . . .
H13 H 1.2255 0.2332 0.1757 0.051 Uiso 1 1 calc R . .
C14 C 1.048(2) 0.4227(12) 0.1303(8) 0.047(3) Uani 1 1 d . . .
H14A H 0.9303 0.4458 0.1100 0.071 Uiso 1 1 calc R . .
H14B H 1.1105 0.3987 0.0842 0.071 Uiso 1 1 calc R . .
H14C H 1.1439 0.4979 0.1676 0.071 Uiso 1 1 calc R . .
C21 C 0.3722(15) 0.0048(9) 0.1435(6) 0.030(2) Uani 1 1 d . . .
H21 H 0.4679 0.0706 0.1237 0.036 Uiso 1 1 calc R . .
C22 C 0.2167(15) -0.1111(11) 0.2227(6) 0.037(2) Uani 1 1 d . . .
H22 H 0.1807 -0.1440 0.2707 0.044 Uiso 1 1 calc R . .
C23 C 0.1105(14) -0.1613(11) 0.1454(7) 0.040(2) Uani 1 1 d . . .
H23 H -0.0093 -0.2334 0.1295 0.049 Uiso 1 1 calc R . .
C24 C 0.1681(18) -0.1054(12) 0.0059(7) 0.043(3) Uani 1 1 d . . .
H24A H 0.2305 -0.0237 -0.0137 0.064 Uiso 1 1 calc R . .
H24B H 0.0229 -0.1327 -0.0108 0.064 Uiso 1 1 calc R . .
H24C H 0.2193 -0.1737 -0.0175 0.064 Uiso 1 1 calc R . .
C31 C 0.6452(16) -0.1727(10) 0.2546(6) 0.032(2) Uani 1 1 d . . .
H31 H 0.5630 -0.1788 0.2043 0.039 Uiso 1 1 calc R . .
C32 C 0.8204(15) -0.1054(10) 0.3751(7) 0.035(2) Uani 1 1 d . . .
H32 H 0.8819 -0.0516 0.4264 0.042 Uiso 1 1 calc R . .
C33 C 0.8363(17) -0.2229(11) 0.3501(7) 0.041(2) Uani 1 1 d . . .
H33 H 0.9115 -0.2667 0.3793 0.049 Uiso 1 1 calc R . .
C34 C 0.686(2) -0.3947(12) 0.2241(8) 0.048(3) Uani 1 1 d . . .
H34A H 0.8132 -0.4051 0.2134 0.072 Uiso 1 1 calc R . .
H34B H 0.6015 -0.4001 0.1722 0.072 Uiso 1 1 calc R . .
H34C H 0.6175 -0.4642 0.2527 0.072 Uiso 1 1 calc R . .
C90 C 0.2498(18) 0.5197(12) 0.4429(8) 0.047(3) Uani 1 1 d . . .
H90A H 0.2095 0.5304 0.4973 0.057 Uiso 1 1 calc R . .
H90B H 0.2912 0.4403 0.4367 0.057 Uiso 1 1 calc R . .
H1S H 0.6794 0.4503 -0.0128 0.057 Uiso 1 1 d G . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 '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 87.06(12) . . ?
C1 Re1 C2 87.20(13) . . ?
C3 Re1 C2 91.11(12) . . ?
C1 Re1 N5 177.82(17) . . ?
C3 Re1 N5 93.02(13) . . ?
C2 Re1 N5 94.97(13) . . ?
C1 Re1 N3 96.70(13) . . ?
C3 Re1 N3 175.98(18) . . ?
C2 Re1 N3 90.49(13) . . ?
N5 Re1 N3 83.17(11) . . ?
C1 Re1 N1 92.36(12) . . ?
C3 Re1 N1 89.87(13) . . ?
C2 Re1 N1 178.90(16) . . ?
N5 Re1 N1 85.47(11) . . ?
N3 Re1 N1 88.56(10) . . ?
O14 S2 O11 114.8(4) . . ?
O14 S2 O12 111.5(4) . . ?
O11 S2 O12 112.5(5) . . ?
O14 S2 O13 104.4(3) . . ?
O11 S2 O13 107.7(4) . . ?
O12 S2 O13 105.0(4) . . ?
C11 N1 C12 105.9(6) . . ?
C11 N1 Re1 125.16(8) . . ?
C12 N1 Re1 127.4(6) . . ?
C11 N2 C13 108.5(5) . . ?
C11 N2 C14 126.7(6) . . ?
C13 N2 C14 124.7(8) . . ?
C21 N3 C22 104.8(6) . . ?
C21 N3 Re1 130.2(5) . . ?
C22 N3 Re1 125.0(5) . . ?
C21 N4 C23 108.0(7) . . ?
C21 N4 C24 127.1(7) . . ?
C23 N4 C24 124.8(7) . . ?
C31 N5 C32 105.1(7) . . ?
C31 N5 Re1 130.2(5) . . ?
C32 N5 Re1 124.5(5) . . ?
C31 N6 C33 107.6(7) . . ?
C31 N6 C34 125.6(7) . . ?
C33 N6 C34 126.7(7) . . ?
O1 C1 Re1 177.3(6) . . ?
O2 C2 Re1 176.8(5) . . ?
O3 C3 Re1 178.1(6) . . ?
N1 C11 N2 111.7 . . ?
C13 C12 N1 109.3(10) . . ?
C12 C13 N2 104.5(9) . . ?
N3 C21 N4 112.4(8) . . ?
N3 C22 C23 110.5(9) . . ?
N4 C23 C22 104.4(8) . . ?
N5 C31 N6 111.2(8) . . ?
C33 C32 N5 109.7(9) . . ?
C32 C33 N6 106.4(9) . . ?
Cl91 C90 Cl92 112.7(7) . . ?
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 1.882(3) . ?
Re1 C3 1.910(3) . ?
Re1 C2 1.941(3) . ?
Re1 N5 2.185(3) . ?
Re1 N3 2.191(3) . ?
Re1 N1 2.199(3) . ?
Cl91 C90 1.735(12) . ?
Cl92 C90 1.762(12) . ?
S2 O14 1.442(5) . ?
S2 O11 1.445(9) . ?
S2 O12 1.453(8) . ?
S2 O13 1.568(5) . ?
O1 C1 1.175(9) . ?
O2 C2 1.152(8) . ?
O3 C3 1.165(8) . ?
N1 C11 1.3109 . ?
N1 C12 1.384(11) . ?
N2 C11 1.3185 . ?
N2 C13 1.388(13) . ?
N2 C14 1.484(12) . ?
N3 C21 1.316(10) . ?
N3 C22 1.357(10) . ?
N4 C21 1.318(10) . ?
N4 C23 1.369(12) . ?
N4 C24 1.490(11) . ?
N5 C31 1.299(11) . ?
N5 C32 1.417(10) . ?
N6 C31 1.365(10) . ?
N6 C33 1.365(12) . ?
N6 C34 1.459(13) . ?
C12 C13 1.372(17) . ?
C22 C23 1.375(15) . ?
C32 C33 1.335(16) . ?
