#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:51:55 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178827 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/81/4108130.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_4108130
loop_
_publ_author_name
'Caixia Yin'
'Gin-Chen Huang'
'Ching-Kuo Kuo'
'Ming-Dung Fu'
'Hao-Cheng Lu'
'Jhih-Hong Ke'
'Kai-Neng Shih'
'Yi-Lin Huang'
'Gene-Hsiang Lee'
'Chen-Yu Yeh'
'Chun-hsien Chen'
'Shie-Ming Peng'
_publ_section_title
;
 Extended Metal-Atom Chains with an Inert Second Row Transition Metal:
 [Ru5(μ5-tpda)4X2] (tpda2-= tripyridyldiamido dianion, X = Cl and NCS)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10090
_journal_page_last               10092
_journal_paper_doi               10.1021/ja8016818
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C62 H44 N22 Ru5 S2'
_chemical_formula_weight         1666.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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                   10.5330(7)
_cell_length_b                   10.5330(7)
_cell_length_c                   26.1558(17)
_cell_measurement_reflns_used    1462
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.19
_cell_measurement_theta_min      2.73
_cell_volume                     2901.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11354
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_T_max  0.7856
_exptl_absorpt_correction_T_min  0.7377
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.644
_refine_diff_density_min         -3.830
_refine_diff_density_rms         0.275
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1716P)²+30.0507P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2539
_refine_ls_wR_factor_ref         0.2791
_reflns_number_gt                1251
_reflns_number_total             1726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8016818-file002.cif
_cod_data_source_block           ic12707
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4108130
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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_group
Ru1 Ru 0.0000 0.0000 0.17390(5) 0.0424(5) Uani 1 4 d S .
Ru2 Ru 0.0000 0.0000 0.08635(4) 0.0333(5) Uani 1 4 d S .
Ru3 Ru 0.0000 0.0000 0.0000 0.0488(6) Uani 1 8 d S .
S1 S 0.0000 0.0000 0.36225(18) 0.0606(14) Uani 1 4 d S .
N3 N 0.0845(8) -0.1666(7) 0.0000 0.0267(16) Uani 1 2 d S .
N4 N 0.0000 0.0000 0.2558(5) 0.039(3) Uani 1 4 d S .
C8 C 0.2053(15) -0.3994(12) 0.0000 0.057(4) Uani 1 2 d S .
H8 H 0.2080 -0.4905 0.0000 0.068 Uiso 1 2 d SR .
C9 C 0.0000 0.0000 0.3004(8) 0.043(4) Uani 1 4 d S .
N1 N 0.1725(13) -0.0948(14) 0.1700(5) 0.030(3) Uiso 0.50 1 d P 1
N2 N 0.1375(11) -0.1347(11) 0.0843(4) 0.027(2) Uiso 0.50 1 d P 1
C1 C 0.232(3) -0.105(2) 0.2098(10) 0.038(7) Uiso 0.50 1 d P 1
H1 H 0.1913 -0.0831 0.2410 0.045 Uiso 0.50 1 calc PR 1
C2 C 0.359(2) -0.149(2) 0.2110(9) 0.033(5) Uiso 0.50 1 d P 1
H2 H 0.4042 -0.1533 0.2423 0.039 Uiso 0.50 1 calc PR 1
C3 C 0.4153(18) -0.1848(19) 0.1653(7) 0.042(4) Uiso 0.50 1 d P 1
H3 H 0.5017 -0.2105 0.1645 0.050 Uiso 0.50 1 calc PR 1
C4 C 0.3442(16) -0.1827(16) 0.1214(7) 0.041(3) Uiso 0.50 1 d P 1
H4 H 0.3797 -0.2080 0.0896 0.049 Uiso 0.50 1 calc PR 1
C5 C 0.2163(14) -0.1420(14) 0.1247(5) 0.031(3) Uiso 0.50 1 d P 1
C6 C 0.1430(15) -0.2110(14) 0.0429(5) 0.028(3) Uiso 0.50 1 d P 1
C7 C 0.2044(19) -0.3298(17) 0.0422(6) 0.042(4) Uiso 0.50 1 d P 1
H7 H 0.2454 -0.3602 0.0722 0.050 Uiso 0.50 1 calc PR 1
N1' N 0.1794(13) -0.0529(15) 0.1673(5) 0.034(4) Uiso 0.50 1 d P 2
N2' N 0.0202(11) -0.1824(11) 0.0838(4) 0.030(2) Uiso 0.50 1 d P 2
C1' C 0.255(3) -0.108(3) 0.2069(11) 0.042(8) Uiso 0.50 1 d P 2
H1' H 0.2188 -0.1125 0.2401 0.050 Uiso 0.50 1 calc PR 2
C2' C 0.375(3) -0.153(3) 0.2014(13) 0.061(10) Uiso 0.50 1 d P 2
H2' H 0.4167 -0.1952 0.2289 0.073 Uiso 0.50 1 calc PR 2
C3' C 0.4300(18) -0.139(2) 0.1595(8) 0.045(4) Uiso 0.50 1 d P 2
H3' H 0.5127 -0.1740 0.1553 0.053 Uiso 0.50 1 calc PR 2
C4' C 0.3751(16) -0.0758(16) 0.1189(7) 0.044(4) Uiso 0.50 1 d P 2
H4' H 0.4216 -0.0614 0.0884 0.053 Uiso 0.50 1 calc PR 2
C5' C 0.2464(13) -0.0317(13) 0.1238(5) 0.031(3) Uiso 0.50 1 d P 2
C6' C 0.0845(15) -0.2342(14) 0.0439(5) 0.027(3) Uiso 0.50 1 d P 2
C7' C 0.1499(17) -0.3488(16) 0.0475(6) 0.035(3) Uiso 0.50 1 d P 2
H7' H 0.1583 -0.3923 0.0791 0.042 Uiso 0.50 1 calc PR 2
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'
S S 0.1246 0.1234 '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'
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
N1' Ru1 N1' 89.57(7) 3 2
N1' Ru1 N1' 89.57(7) 3 .
N1' Ru1 N1' 170.0(8) 2 .
N1' Ru1 N1' 170.0(8) 3 4
N1' Ru1 N1' 89.57(7) 2 4
N1' Ru1 N1' 89.57(7) . 4
N1' Ru1 N1 12.5(5) 3 3
N1' Ru1 N1 102.1(5) 2 3
N1' Ru1 N1 77.4(5) . 3
N1' Ru1 N1 165.4(5) 4 3
N1' Ru1 N1 77.4(5) 3 2
N1' Ru1 N1 12.5(5) 2 2
N1' Ru1 N1 165.4(5) . 2
N1' Ru1 N1 102.1(5) 4 2
N1 Ru1 N1 89.86(4) 3 2
N1' Ru1 N1 102.1(5) 3 .
N1' Ru1 N1 165.4(5) 2 .
N1' Ru1 N1 12.5(5) . .
N1' Ru1 N1 77.4(5) 4 .
N1 Ru1 N1 89.86(4) 3 .
N1 Ru1 N1 174.3(8) 2 .
N1' Ru1 N1 165.4(5) 3 4
N1' Ru1 N1 77.4(5) 2 4
N1' Ru1 N1 102.1(5) . 4
N1' Ru1 N1 12.5(5) 4 4
N1 Ru1 N1 174.3(8) 3 4
N1 Ru1 N1 89.86(4) 2 4
N1 Ru1 N1 89.86(4) . 4
N1' Ru1 N4 95.0(4) 3 .
N1' Ru1 N4 95.0(4) 2 .
N1' Ru1 N4 95.0(4) . .
N1' Ru1 N4 95.0(4) 4 .
N1 Ru1 N4 92.8(4) 3 .
N1 Ru1 N4 92.8(4) 2 .
N1 Ru1 N4 92.8(4) . .
N1 Ru1 N4 92.8(4) 4 .
N1' Ru1 Ru2 85.0(4) 3 .
N1' Ru1 Ru2 85.0(4) 2 .
N1' Ru1 Ru2 85.0(4) . .
N1' Ru1 Ru2 85.0(4) 4 .
N1 Ru1 Ru2 87.2(4) 3 .
N1 Ru1 Ru2 87.2(4) 2 .
N1 Ru1 Ru2 87.2(4) . .
N1 Ru1 Ru2 87.2(4) 4 .
N4 Ru1 Ru2 180.0 . .
N2' Ru2 N2' 176.0(7) 2 .
N2' Ru2 N2' 89.93(2) 2 3
N2' Ru2 N2' 89.93(2) . 3
N2' Ru2 N2' 89.93(2) 2 4
N2' Ru2 N2' 89.93(2) . 4
N2' Ru2 N2' 176.0(7) 3 4
N2' Ru2 N2 50.7(5) 2 3
N2' Ru2 N2 129.2(5) . 3
N2' Ru2 N2 39.3(5) 3 3
N2' Ru2 N2 140.6(5) 4 3
N2' Ru2 N2 39.3(5) 2 2
N2' Ru2 N2 140.6(5) . 2
N2' Ru2 N2 129.2(5) 3 2
N2' Ru2 N2 50.7(5) 4 2
N2 Ru2 N2 89.961(16) 3 2
N2' Ru2 N2 129.2(5) 2 4
N2' Ru2 N2 50.7(5) . 4
N2' Ru2 N2 140.6(5) 3 4
N2' Ru2 N2 39.3(5) 4 4
N2 Ru2 N2 177.0(6) 3 4
N2 Ru2 N2 89.961(16) 2 4
N2' Ru2 N2 140.6(5) 2 .
N2' Ru2 N2 39.3(5) . .
N2' Ru2 N2 50.7(5) 3 .
N2' Ru2 N2 129.2(5) 4 .
N2 Ru2 N2 89.961(16) 3 .
N2 Ru2 N2 177.0(6) 2 .
N2 Ru2 N2 89.961(16) 4 .
N2' Ru2 Ru3 88.0(3) 2 .
N2' Ru2 Ru3 88.0(3) . .
N2' Ru2 Ru3 88.0(3) 3 .
N2' Ru2 Ru3 88.0(3) 4 .
N2 Ru2 Ru3 88.5(3) 3 .
N2 Ru2 Ru3 88.5(3) 2 .
N2 Ru2 Ru3 88.5(3) 4 .
N2 Ru2 Ru3 88.5(3) . .
N2' Ru2 Ru1 92.0(3) 2 .
N2' Ru2 Ru1 92.0(3) . .
N2' Ru2 Ru1 92.0(3) 3 .
N2' Ru2 Ru1 92.0(3) 4 .
N2 Ru2 Ru1 91.5(3) 3 .
N2 Ru2 Ru1 91.5(3) 2 .
N2 Ru2 Ru1 91.5(3) 4 .
N2 Ru2 Ru1 91.5(3) . .
Ru3 Ru2 Ru1 180.0 . .
N3 Ru3 N3 180.0 3 11
N3 Ru3 N3 90.0 3 9
N3 Ru3 N3 90.0 11 9
N3 Ru3 N3 90.0 3 .
N3 Ru3 N3 90.0 11 .
N3 Ru3 N3 180.0(4) 9 .
N3 Ru3 Ru2 90.0 3 9
N3 Ru3 Ru2 90.0 11 9
N3 Ru3 Ru2 90.0 9 9
N3 Ru3 Ru2 90.0 . 9
N3 Ru3 Ru2 90.0 3 .
N3 Ru3 Ru2 90.0 11 .
N3 Ru3 Ru2 90.0 9 .
N3 Ru3 Ru2 90.0 . .
Ru2 Ru3 Ru2 180.0 9 .
C6' N3 C6' 116.4(13) 10 .
C6' N3 C6 121.3(9) 10 .
C6' N3 C6 28.3(7) . .
C6' N3 C6 28.3(7) 10 10
C6' N3 C6 121.3(9) . 10
C6 N3 C6 110.8(13) . 10
C6' N3 Ru3 118.0(7) 10 .
C6' N3 Ru3 118.0(7) . .
C6 N3 Ru3 120.7(7) . .
C6 N3 Ru3 120.7(7) 10 .
C9 N4 Ru1 180.000(1) . .
C7 C8 C7 112.8(18) . 10
C7 C8 C7' 120.0(12) . 10
C7 C8 C7' 25.1(8) 10 10
C7 C8 C7' 25.1(8) . .
C7 C8 C7' 120.0(12) 10 .
C7' C8 C7' 115.0(15) 10 .
N4 C9 S1 180.000(1) . .
C1 N1 C5 122.4(18) . .
C1 N1 Ru1 116.7(16) . .
C5 N1 Ru1 120.9(10) . .
C5 N2 C6 124.7(12) . .
C5 N2 Ru2 117.3(9) . .
C6 N2 Ru2 117.9(9) . .
N1 C1 C2 122(2) . .
C3 C2 C1 118(2) . .
C4 C3 C2 118.8(18) . .
C3 C4 C5 118.3(16) . .
N2 C5 N1 116.9(13) . .
N2 C5 C4 123.8(13) . .
N1 C5 C4 119.0(13) . .
N2 C6 N3 115.9(12) . .
N2 C6 C7 124.0(13) . .
N3 C6 C7 120.1(12) . .
C8 C7 C6 120.4(15) . .
C5' N1' C1' 112.5(16) . .
C5' N1' Ru1 121.5(11) . .
C1' N1' Ru1 125.8(15) . .
C6' N2' C5' 126.3(13) . 4
C6' N2' Ru2 118.8(9) . .
C5' N2' Ru2 114.9(9) 4 .
C2' C1' N1' 126(3) . .
C3' C2' C1' 119(3) . .
C2' C3' C4' 123(2) . .
C3' C4' C5' 118.9(16) . .
N1' C5' N2' 117.0(13) . 3
N1' C5' C4' 120.7(14) . .
N2' C5' C4' 122.0(13) 3 .
N3 C6' N2' 116.1(12) . .
N3 C6' C7' 120.9(12) . .
N2' C6' C7' 123.0(13) . .
C6' C7' C8 117.0(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N1' 1.978(14) 3
Ru1 N1' 1.978(14) 2
Ru1 N1' 1.978(14) .
Ru1 N1' 1.978(14) 4
Ru1 N1 2.075(14) 3
Ru1 N1 2.075(14) 2
Ru1 N1 2.075(14) .
Ru1 N1 2.075(14) 4
Ru1 N4 2.143(13) .
Ru1 Ru2 2.2899(17) .
Ru2 N2' 1.934(12) 2
Ru2 N2' 1.934(12) .
Ru2 N2' 1.934(12) 3
Ru2 N2' 1.934(12) 4
Ru2 N2 2.028(11) 3
Ru2 N2 2.028(11) 2
Ru2 N2 2.028(11) 4
Ru2 N2 2.028(11) .
Ru2 Ru3 2.2585(12) .
Ru3 N3 1.967(7) 3
Ru3 N3 1.967(7) 11
Ru3 N3 1.967(7) 9
Ru3 N3 1.967(7) .
Ru3 Ru2 2.2585(12) 9
S1 C9 1.62(2) .
N3 C6' 1.352(13) 10
N3 C6' 1.352(13) .
N3 C6 1.364(14) .
N3 C6 1.364(14) 10
N4 C9 1.17(2) .
C8 C7 1.326(18) .
C8 C7 1.326(18) 10
C8 C7' 1.472(17) 10
C8 C7' 1.472(17) .
N1 C1 1.22(3) .
N1 C5 1.364(19) .
N2 C5 1.346(18) .
N2 C6 1.349(17) .
C1 C2 1.42(3) .
C2 C3 1.39(3) .
C3 C4 1.37(2) .
C4 C5 1.42(2) .
C6 C7 1.41(2) .
N1' C5' 1.36(2) .
N1' C1' 1.43(3) .
N2' C6' 1.358(17) .
N2' C5' 1.360(18) 4
C1' C2' 1.36(4) .
C2' C3' 1.25(4) .
C3' C4' 1.38(3) .
C4' C5' 1.44(2) .
C5' N2' 1.360(18) 3
C6' C7' 1.39(2) .
