#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/46/7004681.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_7004681
loop_
_publ_author_name
'Laidlaw, William Michael'
'Denning, Robert Gordon'
'Murphy, Damien Martin'
'Green, Jennifer C.'
_publ_section_title
;
 Solvent dependence of the g-anisotropy in the ESR of cyanide-bridged
 mixed-valence complexes
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              6257
_journal_page_last               6264
_journal_paper_doi               10.1039/b810224d
_journal_year                    2008
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C6 H15 Cr N6 O5 Ru, 2(C F3 O3 S) '
_chemical_formula_sum            'C8 H15 Cr F6 N6 O11 Ru S2'
_chemical_formula_weight         702.43
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 112.0394(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1853(2)
_cell_length_b                   11.6464(2)
_cell_length_c                   16.6937(3)
_cell_measurement_reflns_used    20225
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     2376.18(7)
_computing_cell_refinement
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Nonius KappaCCD
;
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20225
_diffrn_reflns_theta_full        27.490
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         5.140
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' blue '
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_description       ' fragment '
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_thermal_history
;
The material was crystallised at ambient temperature. A suitable crystal
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis.
;
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1251
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4261
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.034379
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
0.292 0.106 0.0457
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0399
_refine_ls_wR_factor_gt          0.0279
_refine_ls_wR_factor_ref         0.0279
_reflns_limit_h_max              15
_reflns_limit_h_min              -17
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                4261
_reflns_number_total             5398
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b810224d.txt
_cod_data_source_block           CrRuTf2
_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      'P 1 21/n 1 '
_cod_original_formula_sum        ' C8 H15 Cr F6 N6 O11 Ru1 S2 '
_cod_database_code               7004681
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
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_occupancy
_atom_site_adp_type
Ru1 Ru 0.513523(14) 0.228263(16) 0.683924(12) 0.0126 1.0000 Uani
N1 N 0.35167(16) 0.23260(17) 0.65785(13) 0.0166 1.0000 Uani
C1 C 0.26659(19) 0.2369(2) 0.66331(15) 0.0170 1.0000 Uani
Cr1 Cr 0.12533(3) 0.24261(3) 0.68403(2) 0.0158 1.0000 Uani
N2 N 0.51367(19) 0.40922(18) 0.67487(15) 0.0183 1.0000 Uani
N3 N 0.49402(18) 0.2212(2) 0.55323(13) 0.0167 1.0000 Uani
N4 N 0.51119(19) 0.04710(19) 0.69006(16) 0.0200 1.0000 Uani
N5 N 0.5338(2) 0.2358(2) 0.81598(14) 0.0205 1.0000 Uani
N6 N 0.68459(16) 0.22497(19) 0.72017(14) 0.0158 1.0000 Uani
C2 C 0.1279(2) 0.0811(2) 0.69906(16) 0.0222 1.0000 Uani
O1 O 0.12498(19) -0.01593(18) 0.70894(15) 0.0371 1.0000 Uani
C3 C 0.0491(2) 0.2222(2) 0.56247(17) 0.0209 1.0000 Uani
O2 O 0.00696(17) 0.2089(2) 0.49003(13) 0.0348 1.0000 Uani
C4 C 0.1139(2) 0.4046(2) 0.67094(17) 0.0216 1.0000 Uani
O3 O 0.10161(18) 0.50220(17) 0.66521(15) 0.0352 1.0000 Uani
C5 C 0.2165(2) 0.2638(2) 0.80218(18) 0.0265 1.0000 Uani
O4 O 0.2740(2) 0.2775(2) 0.87191(14) 0.0464 1.0000 Uani
C6 C -0.0017(2) 0.2483(2) 0.70941(18) 0.0260 1.0000 Uani
O5 O -0.07733(19) 0.2539(2) 0.72731(18) 0.0476 1.0000 Uani
O6 O 0.68060(16) 0.38209(17) 0.58122(13) 0.0310 1.0000 Uani
O7 O 0.79802(16) 0.54361(18) 0.64703(12) 0.0312 1.0000 Uani
O8 O 0.62560(16) 0.57339(17) 0.52649(14) 0.0320 1.0000 Uani
S1 S 0.71428(5) 0.49707(5) 0.57120(4) 0.0180 1.0000 Uani
C7 C 0.7853(2) 0.4813(3) 0.49707(17) 0.0282 1.0000 Uani
F1 F 0.83580(19) 0.57910(19) 0.49331(14) 0.0536 1.0000 Uani
F2 F 0.71674(16) 0.4563(2) 0.41782(11) 0.0468 1.0000 Uani
F3 F 0.86031(15) 0.39933(18) 0.52252(12) 0.0431 1.0000 Uani
O9 O 0.61126(15) -0.01266(17) 0.56157(13) 0.0303 1.0000 Uani
O10 O 0.77993(17) -0.00312(18) 0.68691(12) 0.0312 1.0000 Uani
O11 O 0.74437(15) -0.16677(16) 0.58953(13) 0.0262 1.0000 Uani
S2 S 0.72434(5) -0.04690(5) 0.60048(4) 0.0191 1.0000 Uani
C8 C 0.7881(3) 0.0293(3) 0.5365(2) 0.0332 1.0000 Uani
F4 F 0.89383(18) 0.0055(2) 0.56428(18) 0.0636 1.0000 Uani
F5 F 0.7421(2) -0.00071(18) 0.45362(12) 0.0557 1.0000 Uani
F6 F 0.7773(2) 0.14157(16) 0.54251(13) 0.0511 1.0000 Uani
H1 H 0.461(4) 0.435(4) 0.686(3) 0.059(13) 1.0000 Uiso
H2 H 0.578(3) 0.446(3) 0.713(2) 0.032(9) 1.0000 Uiso
H3 H 0.507(3) 0.431(4) 0.622(3) 0.058(12) 1.0000 Uiso
H4 H 0.428(3) 0.242(3) 0.520(3) 0.045(11) 1.0000 Uiso
H5 H 0.542(3) 0.266(3) 0.548(2) 0.037(10) 1.0000 Uiso
H6 H 0.500(3) 0.154(3) 0.534(2) 0.034(9) 1.0000 Uiso
H7 H 0.445(3) 0.023(3) 0.688(2) 0.050(11) 1.0000 Uiso
H8 H 0.528(3) 0.018(3) 0.649(3) 0.045(11) 1.0000 Uiso
H9 H 0.560(3) 0.026(3) 0.737(2) 0.026(8) 1.0000 Uiso
H10 H 0.499(5) 0.288(6) 0.822(4) 0.10(2) 1.0000 Uiso
H11 H 0.514(4) 0.179(5) 0.834(3) 0.075(16) 1.0000 Uiso
H12 H 0.599(5) 0.253(4) 0.848(3) 0.074(16) 1.0000 Uiso
H13 H 0.715(3) 0.241(3) 0.775(3) 0.047(11) 1.0000 Uiso
H14 H 0.707(3) 0.272(3) 0.689(2) 0.030(9) 1.0000 Uiso
H15 H 0.709(3) 0.155(4) 0.714(2) 0.041(10) 1.0000 Uiso
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 International_Tables_Vol_IV_Table_2.2B
'Cr ' 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399
1.1832 International_Tables_Vol_IV_Table_2.2B
'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'Ru ' -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676
94.2928 5.3787 International_Tables_Vol_IV_Table_2.2B
'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Ru1 . N2 . 89.36(8) yes
N1 . Ru1 . N3 . 94.00(8) yes
N2 . Ru1 . N3 . 88.16(9) yes
N1 . Ru1 . N4 . 90.11(9) yes
N2 . Ru1 . N4 . 178.74(9) yes
N3 . Ru1 . N4 . 90.73(9) yes
N1 . Ru1 . N5 . 86.18(9) yes
N2 . Ru1 . N5 . 91.72(10) yes
N3 . Ru1 . N5 . 179.78(9) yes
N4 . Ru1 . N5 . 89.39(10) yes
N1 . Ru1 . N6 . 176.10(8) yes
N2 . Ru1 . N6 . 90.52(9) yes
N3 . Ru1 . N6 . 89.90(8) yes
N4 . Ru1 . N6 . 90.08(9) yes
N5 . Ru1 . N6 . 89.93(9) yes
Ru1 . N1 . C1 . 164.23(19) yes
N1 . C1 . Cr1 . 175.0(2) yes
C1 . Cr1 . C2 . 91.04(10) yes
C1 . Cr1 . C3 . 88.01(10) yes
C2 . Cr1 . C3 . 89.62(11) yes
C1 . Cr1 . C4 . 92.93(10) yes
C2 . Cr1 . C4 . 176.02(11) yes
C3 . Cr1 . C4 . 90.80(11) yes
C1 . Cr1 . C5 . 85.24(11) yes
C2 . Cr1 . C5 . 91.07(12) yes
C3 . Cr1 . C5 . 173.23(11) yes
C4 . Cr1 . C5 . 88.97(12) yes
C1 . Cr1 . C6 . 177.05(11) yes
C2 . Cr1 . C6 . 88.77(11) yes
C3 . Cr1 . C6 . 94.93(11) yes
C4 . Cr1 . C6 . 87.25(11) yes
C5 . Cr1 . C6 . 91.82(12) yes
Ru1 . N2 . H1 . 109(3) no
Ru1 . N2 . H2 . 115(2) no
H1 . N2 . H2 . 107(3) no
Ru1 . N2 . H3 . 111(3) no
H1 . N2 . H3 . 109(4) no
H2 . N2 . H3 . 105(3) no
Ru1 . N3 . H4 . 111(3) no
Ru1 . N3 . H5 . 106(2) no
H4 . N3 . H5 . 111(3) no
Ru1 . N3 . H6 . 115(2) no
H4 . N3 . H6 . 103(3) no
H5 . N3 . H6 . 110(3) no
Ru1 . N4 . H7 . 110(3) no
Ru1 . N4 . H8 . 110(3) no
H7 . N4 . H8 . 112(3) no
Ru1 . N4 . H9 . 108(2) no
H7 . N4 . H9 . 109(3) no
H8 . N4 . H9 . 107(3) no
Ru1 . N5 . H10 . 108(4) no
Ru1 . N5 . H11 . 115(3) no
H10 . N5 . H11 . 107(5) no
Ru1 . N5 . H12 . 112(3) no
H10 . N5 . H12 . 104(5) no
H11 . N5 . H12 . 110(5) no
Ru1 . N6 . H13 . 109(3) no
Ru1 . N6 . H14 . 112(2) no
H13 . N6 . H14 . 111(3) no
Ru1 . N6 . H15 . 112(2) no
H13 . N6 . H15 . 106(3) no
H14 . N6 . H15 . 107(3) no
Cr1 . C2 . O1 . 176.7(2) yes
Cr1 . C3 . O2 . 177.7(2) yes
Cr1 . C4 . O3 . 175.4(2) yes
Cr1 . C5 . O4 . 177.6(3) yes
Cr1 . C6 . O5 . 177.7(3) yes
O6 . S1 . O7 . 114.63(13) yes
O6 . S1 . O8 . 114.19(12) yes
O7 . S1 . O8 . 115.54(13) yes
O6 . S1 . C7 . 104.17(13) yes
O7 . S1 . C7 . 102.45(13) yes
O8 . S1 . C7 . 103.64(13) yes
S1 . C7 . F1 . 109.8(2) yes
S1 . C7 . F2 . 111.6(2) yes
F1 . C7 . F2 . 107.8(2) yes
S1 . C7 . F3 . 111.57(19) yes
F1 . C7 . F3 . 107.8(2) yes
F2 . C7 . F3 . 108.1(2) yes
O9 . S2 . O10 . 113.83(12) yes
O9 . S2 . O11 . 114.68(12) yes
O10 . S2 . O11 . 114.78(12) yes
O9 . S2 . C8 . 103.20(14) yes
O10 . S2 . C8 . 103.95(13) yes
O11 . S2 . C8 . 104.51(13) yes
S2 . C8 . F4 . 110.5(2) yes
S2 . C8 . F5 . 110.6(2) yes
F4 . C8 . F5 . 108.5(3) yes
S2 . C8 . F6 . 110.6(2) yes
F4 . C8 . F6 . 108.1(3) yes
F5 . C8 . F6 . 108.5(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ru1 . N1 . 2.012(2) yes
Ru1 . N2 . 2.113(2) yes
Ru1 . N3 . 2.100(2) yes
Ru1 . N4 . 2.113(2) yes
Ru1 . N5 . 2.121(2) yes
Ru1 . N6 . 2.1050(19) yes
N1 . C1 . 1.160(3) yes
C1 . Cr1 . 2.019(2) yes
Cr1 . C2 . 1.896(3) yes
Cr1 . C3 . 1.911(3) yes
Cr1 . C4 . 1.899(3) yes
Cr1 . C5 . 1.902(3) yes
Cr1 . C6 . 1.877(3) yes
N2 . H1 . 0.84(5) no
N2 . H2 . 0.95(4) no
N2 . H3 . 0.89(5) no
N3 . H4 . 0.87(4) no
N3 . H5 . 0.85(4) no
N3 . H6 . 0.86(4) no
N4 . H7 . 0.91(4) no
N4 . H8 . 0.86(4) no
N4 . H9 . 0.84(4) no
N5 . H10 . 0.79(7) no
N5 . H11 . 0.81(6) no
N5 . H12 . 0.84(6) no
N6 . H13 . 0.87(4) no
N6 . H14 . 0.88(4) no
N6 . H15 . 0.89(4) no
C2 . O1 . 1.145(3) yes
C3 . O2 . 1.136(3) yes
C4 . O3 . 1.147(3) yes
C5 . O4 . 1.137(4) yes
C6 . O5 . 1.145(3) yes
O6 . S1 . 1.4402(19) yes
O7 . S1 . 1.4375(19) yes
O8 . S1 . 1.435(2) yes
S1 . C7 . 1.820(3) yes
C7 . F1 . 1.333(4) yes
C7 . F2 . 1.325(3) yes
C7 . F3 . 1.324(3) yes
O9 . S2 . 1.4413(18) yes
O10 . S2 . 1.4439(19) yes
O11 . S2 . 1.4451(19) yes
S2 . C8 . 1.819(3) yes
C8 . F4 . 1.323(4) yes
C8 . F5 . 1.333(3) yes
C8 . F6 . 1.323(3) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N2 H2 O10 3_656 0.95(4) 2.08(4) 3.010(3) 168(3) yes
N2 H3 O8 2_666 0.89(5) 2.44(4) 3.175(3) 140(3) yes
N3 H5 O6 . 0.85(4) 2.17(4) 2.987(3) 160(3) yes
N3 H6 O9 . 0.86(4) 2.37(4) 3.109(3) 144(3) yes
N3 H6 O9 2_656 0.86(4) 2.37(4) 3.082(3) 140(3) yes
N4 H8 O9 . 0.86(4) 2.17(4) 2.992(3) 161(4) yes
N4 H9 O7 3_646 0.84(4) 2.14(4) 2.931(3) 157(3) yes
N5 H12 O11 3_656 0.84(6) 2.15(6) 2.978(3) 167(5) yes
N6 H13 O11 3_656 0.87(4) 2.37(4) 3.213(3) 162(3) yes
N6 H14 O6 . 0.88(4) 2.13(4) 2.939(3) 153(3) yes
N6 H15 O10 . 0.89(4) 2.19(4) 3.077(3) 171(3) yes
