#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:12:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179444 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/41/4334113.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_4334113
loop_
_publ_author_name
'German E. Pieslinger'
'Pablo Albores'
'Leonardo D. Slep'
'Benjamin J. Coe'
'Cliff J. Timpson'
'Luis M. Baraldo'
_publ_section_title
;
 Communication between Remote Moieties in Linear Ru-Ru-Ru Trimetallic
 Cyanide-Bridged Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2906
_journal_page_last               2917
_journal_paper_doi               10.1021/ic302173g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C66 H68 Cl2 F12 N14 O4 P2 Ru3'
_chemical_formula_weight         1785.39
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.2119(4)
_cell_length_b                   14.2119(4)
_cell_length_c                   18.9069(8)
_cell_measurement_reflns_used    2348
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7437
_cell_measurement_theta_min      3.5797
_cell_volume                     3818.8(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.1028
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8814
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       plate
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.690
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3962
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1614
_refine_ls_R_factor_gt           0.0906
_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)+(0.1832P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2816
_refine_ls_wR_factor_ref         0.3071
_reflns_number_gt                1893
_reflns_number_total             3962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302173g_si_002_3.cif
_cod_data_source_block           3
_cod_original_cell_volume        3818.8(4)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4334113
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -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
Ru1 Ru 0.2500 0.2500 0.03604(9) 0.0450(5) Uani 1 4 d S . .
Ru2 Ru 0.2500 0.2500 -0.23811(8) 0.0339(5) Uani 1 4 d S . .
Ru3 Ru 0.2500 0.2500 -0.51222(9) 0.0447(5) Uani 1 4 d S . .
Cl1 Cl 0.2500 0.2500 0.1622(3) 0.0563(15) Uani 1 4 d S . .
Cl3 Cl 0.2500 0.2500 -0.6387(3) 0.0564(15) Uani 1 4 d S . .
C1 C 0.2500 0.2500 -0.3436(14) 0.046(4) Uani 1 4 d S . .
C2 C 0.2500 0.2500 -0.1264(11) 0.042(5) Uani 1 4 d SU . .
N2 N 0.2500 0.2500 -0.0708(8) 0.048(5) Uani 1 4 d SU . .
N1 N 0.2500 0.2500 -0.4028(10) 0.046(4) Uani 1 4 d S . .
N5 N 0.2140(9) 0.1091(8) -0.5142(7) 0.081(4) Uani 1 1 d . . .
C4 C 0.3148(17) -0.0838(14) 0.0397(12) 0.116(7) Uani 1 1 d . . .
H4 H 0.3264 -0.1482 0.0402 0.139 Uiso 1 1 calc R A 1
C3 C 0.3323(15) 0.0736(15) -0.0114(10) 0.117(7) Uani 1 1 d . . .
H3 H 0.3559 0.1128 -0.0466 0.141 Uiso 1 1 calc R B 1
C5 C 0.2454(11) 0.0487(10) 0.0833(7) 0.071(4) Uani 1 1 d . . .
H5 H 0.2126 0.0757 0.1207 0.085 Uiso 1 1 calc R F .
C6 C 0.2549(13) -0.0459(11) 0.0863(9) 0.087(5) Uani 1 1 d . F .
H6 H 0.2218 -0.0823 0.1187 0.104 Uiso 1 1 calc R . .
N3 N 0.2757(10) 0.1069(8) 0.0358(6) 0.081(4) Uani 1 1 d . F .
P1 P 0.7500 0.2500 0.2624(4) 0.0910(19) Uani 1 2 d S . .
F1 F 0.7530(10) 0.3255(11) 0.3215(9) 0.203(7) Uani 1 1 d . . .
C17 C 0.1576(14) 0.0673(16) -0.4643(11) 0.109(6) Uani 1 1 d . E .
H17 H 0.1407 0.1037 -0.4255 0.131 Uiso 1 1 calc R C 1
F2 F 0.7532(10) 0.3265(9) 0.2017(7) 0.173(5) Uani 1 1 d . . .
F3 F 0.8580(8) 0.2488(14) 0.2635(6) 0.184(7) Uani 1 1 d . . .
C18 C 0.2495(11) 0.0488(10) -0.5622(7) 0.073(4) Uani 1 1 d . E .
H18 H 0.2914 0.0734 -0.5951 0.087 Uiso 1 1 calc R D 1
O1 O -0.0563(8) -0.0645(8) -0.2210(6) 0.099(3) Uani 1 1 d . E 1
N4 N 0.1464(6) 0.1452(6) -0.2365(4) 0.0417(19) Uani 1 1 d . E 1
C8 C 0.1506(14) 0.0663(14) -0.1926(9) 0.112(6) Uani 1 1 d . E 1
H8 H 0.2016 0.0607 -0.1620 0.134 Uiso 1 1 calc R E 1
C9 C 0.0686(12) 0.1455(12) -0.2811(10) 0.096(5) Uani 1 1 d . E 1
H9 H 0.0636 0.1958 -0.3123 0.115 Uiso 1 1 calc R E 1
C10 C 0.0016(12) 0.0824(12) -0.2838(11) 0.107(6) Uani 1 1 d . E 1
H10 H -0.0474 0.0858 -0.3162 0.128 Uiso 1 1 calc R E 1
C11 C 0.0096(10) 0.0052(9) -0.2314(8) 0.074(4) Uani 1 1 d . E 1
C12 C 0.0865(11) -0.0009(10) -0.1921(11) 0.104(6) Uani 1 1 d . E 1
H12 H 0.0954 -0.0535 -0.1636 0.124 Uiso 1 1 calc R E 1
C13 C -0.117(2) -0.070(2) -0.2740(11) 0.200(14) Uani 1 1 d . E 1
H13A H -0.1607 -0.1197 -0.2650 0.300 Uiso 1 1 calc R E 1
H13B H -0.0831 -0.0829 -0.3170 0.300 Uiso 1 1 calc R E 1
H13C H -0.1496 -0.0114 -0.2785 0.300 Uiso 1 1 calc R E 1
C16 C 0.1266(15) -0.0151(15) -0.4662(14) 0.116(7) Uani 1 1 d . E 1
H16 H 0.0826 -0.0347 -0.4330 0.139 Uiso 1 1 calc R E 1
C7 C 0.3596(15) -0.0265(18) -0.0095(17) 0.148(10) Uani 1 1 d . F 1
H7 H 0.4050 -0.0503 -0.0401 0.178 Uiso 1 1 calc R F 1
C14 C 0.229(2) -0.0485(13) -0.5673(11) 0.136(10) Uani 1 1 d . E 1
H14 H 0.2584 -0.0895 -0.5988 0.163 Uiso 1 1 calc R E 1
C15 C 0.1570(19) -0.076(2) -0.5165(15) 0.148(9) Uani 1 1 d . E 1
H15 H 0.1313 -0.1360 -0.5187 0.178 Uiso 1 1 calc R E 1
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
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
N2 Ru1 N3 89.9(3) . 4
N2 Ru1 N3 89.9(3) . 2
N3 Ru1 N3 90.000(2) 4 2
N2 Ru1 N3 89.9(3) . 3
N3 Ru1 N3 179.7(6) 4 3
N3 Ru1 N3 90.000(2) 2 3
N2 Ru1 N3 89.9(3) . .
N3 Ru1 N3 90.000(2) 4 .
N3 Ru1 N3 179.7(7) 2 .
N3 Ru1 N3 90.000(2) 3 .
N2 Ru1 Cl1 180.0 . .
N3 Ru1 Cl1 90.1(3) 4 .
N3 Ru1 Cl1 90.1(3) 2 .
N3 Ru1 Cl1 90.1(3) 3 .
N3 Ru1 Cl1 90.1(3) . .
C1 Ru2 N4 90.8(2) . .
C1 Ru2 N4 90.8(2) . 2
N4 Ru2 N4 178.4(5) . 2
C1 Ru2 N4 90.8(2) . 4
N4 Ru2 N4 89.988(7) . 4
N4 Ru2 N4 89.988(7) 2 4
C1 Ru2 N4 90.8(2) . 3
N4 Ru2 N4 89.988(7) . 3
N4 Ru2 N4 89.988(7) 2 3
N4 Ru2 N4 178.4(5) 4 3
C1 Ru2 C2 180.000(1) . .
N4 Ru2 C2 89.2(2) . .
N4 Ru2 C2 89.2(2) 2 .
N4 Ru2 C2 89.2(2) 4 .
N4 Ru2 C2 89.2(2) 3 .
N5 Ru3 N5 89.981(16) 4 .
N5 Ru3 N5 89.981(15) 4 2
N5 Ru3 N5 177.9(8) . 2
N5 Ru3 N5 177.9(8) 4 3
N5 Ru3 N5 89.981(15) . 3
N5 Ru3 N5 89.980(15) 2 3
N5 Ru3 N1 91.1(4) 4 .
N5 Ru3 N1 91.1(4) . .
N5 Ru3 N1 91.1(4) 2 .
N5 Ru3 N1 91.1(4) 3 .
N5 Ru3 Cl3 88.9(4) 4 .
N5 Ru3 Cl3 88.9(4) . .
N5 Ru3 Cl3 88.9(4) 2 .
N5 Ru3 Cl3 88.9(4) 3 .
N1 Ru3 Cl3 180.000(1) . .
N1 C1 Ru2 180.000(2) . .
N2 C2 Ru2 180.0 . .
C2 N2 Ru1 180.000(1) . .
C1 N1 Ru3 180.000(2) . .
C18 N5 C17 114.0(15) . .
C18 N5 Ru3 122.4(11) . .
C17 N5 Ru3 123.4(13) . .
C6 C4 C7 119.6(19) . .
N3 C3 C7 120(2) . .
N3 C5 C6 129.1(15) . .
C4 C6 C5 115.9(17) . .
C3 N3 C5 116.9(15) . .
C3 N3 Ru1 118.2(13) . .
C5 N3 Ru1 124.7(11) . .
F3 P1 F3 178.4(10) 2_655 .
F3 P1 F1 90.5(8) 2_655 .
F3 P1 F1 88.3(8) . .
F3 P1 F1 88.3(8) 2_655 2_655
F3 P1 F1 90.5(8) . 2_655
F1 P1 F1 87.7(15) . 2_655
F3 P1 F2 91.8(8) 2_655 .
F3 P1 F2 89.4(8) . .
F1 P1 F2 92.7(9) . .
F1 P1 F2 179.6(9) 2_655 .
F3 P1 F2 89.4(8) 2_655 2_655
F3 P1 F2 91.8(8) . 2_655
F1 P1 F2 179.6(9) . 2_655
F1 P1 F2 92.7(9) 2_655 2_655
F2 P1 F2 86.9(12) . 2_655
C16 C17 N5 126(2) . .
N5 C18 C14 126.3(18) . .
C13 O1 C11 112.1(18) . .
C9 N4 C8 113.4(13) . .
C9 N4 Ru2 123.3(9) . .
C8 N4 Ru2 123.3(10) . .
C12 C8 N4 123.7(17) . .
C10 C9 N4 126.9(17) . .
C9 C10 C11 115.1(16) . .
C12 C11 O1 115.7(14) . .
C12 C11 C10 119.2(13) . .
O1 C11 C10 125.1(13) . .
C8 C12 C11 121.2(16) . .
C17 C16 C15 120(2) . .
C4 C7 C3 117(2) . .
C18 C14 C15 111(2) . .
C16 C15 C14 121(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N2 2.020(16) .
Ru1 N3 2.066(12) 4
Ru1 N3 2.066(12) 2
Ru1 N3 2.066(12) 3
Ru1 N3 2.066(12) .
Ru1 Cl1 2.385(6) .
Ru2 C1 1.99(3) .
Ru2 N4 2.095(8) .
Ru2 N4 2.095(8) 2
Ru2 N4 2.095(8) 4
Ru2 N4 2.095(8) 3
Ru2 C2 2.11(2) .
Ru3 N5 2.068(12) 4
Ru3 N5 2.068(12) .
Ru3 N5 2.068(12) 2
Ru3 N5 2.068(12) 3
Ru3 N1 2.07(2) .
Ru3 Cl3 2.392(6) .
C1 N1 1.12(3) .
C2 N2 1.05(2) .
N5 C18 1.346(17) .
N5 C17 1.37(2) .
C4 C6 1.34(2) .
C4 C7 1.39(3) .
C3 N3 1.29(2) .
C3 C7 1.48(3) .
C5 N3 1.295(17) .
C5 C6 1.351(19) .
P1 F3 1.536(11) 2_655
P1 F3 1.536(11) .
P1 F1 1.550(13) .
P1 F1 1.550(13) 2_655
P1 F2 1.582(12) .
P1 F2 1.582(12) 2_655
C17 C16 1.25(2) .
C18 C14 1.41(2) .
O1 C13 1.32(3) .
O1 C11 1.378(14) .
N4 C9 1.390(19) .
N4 C8 1.397(19) .
C8 C12 1.32(2) .
C9 C10 1.31(2) .
C10 C11 1.48(2) .
C11 C12 1.32(2) .
C16 C15 1.36(3) .
C14 C15 1.46(3) .
