#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/19/4111900.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_4111900
loop_
_publ_author_name
'Wei-Zhong Chen'
'F. Albert Cotton'
'Naresh S. Dalal'
'Carlos A. Murillo'
'Chris M. Ramsey'
'Tong Ren'
'Xiaoping Wang'
_publ_section_title
;
 Proof of Large Positive Zero-Field Splitting in a Ru25+ Paddlewheel
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12691
_journal_page_last               12696
_journal_paper_doi               10.1021/ja053615a
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C52 H28 N8 Cl17 Ru2, 0.5(H2O), C6 H14 '
_chemical_formula_sum            'C58 H43 Cl17 N8 O0.5 Ru2'
_chemical_formula_weight         1664.79
_chemical_name_systematic
; 
Tetrakis(N,N'-di(3,5-diclorophenyl)formamidinato) chloro 
diruthenium(II,III) 0.5water hexanes solvate

;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :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            4
_cell_length_a                   15.5980(11)
_cell_length_b                   15.5980(11)
_cell_length_c                   27.063(4)
_cell_measurement_reflns_used    5887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.386
_cell_volume                     6584.4(12)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31871
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_T_max  0.7874
_exptl_absorpt_correction_T_min  0.6729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       plate
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.632
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2928
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0941P)²+34.6070P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1876
_refine_ls_wR_factor_ref         0.1959
_reflns_number_gt                2458
_reflns_number_total             2928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja053615asi20050602_113034_2.cif
_cod_data_source_block           100k
_cod_original_cell_volume        6584.5(11)
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_original_formula_sum        'C58 H43 Cl17 N8 O0.50 Ru2'
_cod_database_code               4111900
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+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'y, x, 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_assembly
_atom_site_disorder_group
Ru1 Ru 0.2500 0.2500 0.65769(3) 0.0269(3) Uani 1 4 d S . .
Ru2 Ru 0.2500 0.2500 0.74501(3) 0.0278(3) Uani 1 4 d S . .
Cl1 Cl 0.2500 0.2500 0.83300(10) 0.0333(6) Uani 1 4 d S . .
O1 O 0.2500 0.2500 0.5604(10) 0.061(6) Uani 0.50 4 d SPDU . .
H1 H 0.282(15) 0.284(15) 0.5389(12) 0.079 Uiso 0.25 1 d PD . .
Cl4 Cl 0.22765(15) -0.04430(15) 0.90095(7) 0.0696(6) Uani 1 1 d . . .
Cl5 Cl -0.08609(12) 0.04369(13) 0.83766(7) 0.0615(5) Uani 1 1 d . . .
N1 N 0.1911(3) 0.1323(3) 0.65693(16) 0.0321(10) Uani 1 1 d D . .
N2 N 0.1853(3) 0.1318(3) 0.74246(17) 0.0328(10) Uani 1 1 d . . .
C1 C 0.1693(4) 0.0958(3) 0.6997(2) 0.0328(12) Uani 1 1 d . A .
H1A H 0.1412 0.0417 0.6992 0.039 Uiso 1 1 calc R . .
C2 C 0.1824(8) 0.0798(5) 0.6143(2) 0.0317(13) Uani 0.684(14) 1 d PGD A 1
C3 C 0.1390(7) 0.1115(4) 0.5734(3) 0.039(3) Uani 0.684(14) 1 d PGD A 1
H3 H 0.1123 0.1662 0.5748 0.047 Uiso 0.684(14) 1 calc PR A 1
C4 C 0.1348(7) 0.0633(5) 0.5303(2) 0.051(4) Uani 0.684(14) 1 d PGD A 1
C5 C 0.1739(7) -0.0167(5) 0.5281(2) 0.056(2) Uani 0.684(14) 1 d PGD A 1
H5 H 0.1710 -0.0497 0.4987 0.067 Uiso 0.684(14) 1 calc PR A 1
C6 C 0.2173(5) -0.0484(4) 0.5691(3) 0.0420(16) Uani 0.684(14) 1 d PGD A 1
C7 C 0.2215(8) -0.0002(6) 0.6122(3) 0.033(3) Uani 0.684(14) 1 d PGD A 1
H7 H 0.2512 -0.0219 0.6402 0.039 Uiso 0.684(14) 1 calc PR A 1
Cl2 Cl 0.0840(7) 0.1027(5) 0.4798(2) 0.101(3) Uani 0.684(14) 1 d PDU A 1
Cl3 Cl 0.2656(7) -0.1472(5) 0.5662(4) 0.0571(17) Uani 0.684(14) 1 d PD A 1
C2B C 0.185(2) 0.0847(12) 0.6124(5) 0.0317(13) Uani 0.316(14) 1 d PD A 2
C3B C 0.161(2) 0.1255(11) 0.5689(5) 0.039(3) Uani 0.316(14) 1 d PD A 2
H3B H 0.1418 0.1834 0.5697 0.047 Uiso 0.316(14) 1 calc PR A 2
C4B C 0.164(2) 0.0815(10) 0.5243(4) 0.051(4) Uani 0.316(14) 1 d PD A 2
C5B C 0.178(2) -0.0067(9) 0.5237(5) 0.056(2) Uani 0.316(14) 1 d PD A 2
H5B H 0.1674 -0.0393 0.4947 0.067 Uiso 0.316(14) 1 calc PR A 2
C6B C 0.2065(14) -0.0457(9) 0.5668(5) 0.0420(16) Uani 0.316(14) 1 d PD A 2
C7B C 0.202(3) -0.0029(13) 0.6117(5) 0.033(3) Uani 0.316(14) 1 d PD A 2
H7B H 0.2108 -0.0331 0.6418 0.039 Uiso 0.316(14) 1 calc PR A 2
Cl2B Cl 0.1282(14) 0.1304(9) 0.4723(5) 0.101(3) Uani 0.316(14) 1 d PD A 2
Cl3B Cl 0.2479(18) -0.1476(12) 0.5644(9) 0.0571(17) Uani 0.316(14) 1 d PD A 2
C8 C 0.1484(4) 0.0883(4) 0.7843(2) 0.0351(12) Uani 1 1 d . A .
C9 C 0.2000(4) 0.0509(4) 0.8196(2) 0.0417(14) Uani 1 1 d . . .
H9A H 0.2607 0.0551 0.8174 0.050 Uiso 1 1 calc R A .
C10 C 0.1615(5) 0.0071(4) 0.8583(2) 0.0465(15) Uani 1 1 d . A .
C11 C 0.0747(5) 0.0020(4) 0.8643(2) 0.0488(16) Uani 1 1 d . . .
H11A H 0.0501 -0.0281 0.8913 0.059 Uiso 1 1 calc R A .
C12 C 0.0250(4) 0.0422(4) 0.8300(3) 0.0451(15) Uani 1 1 d . A .
C13 C 0.0599(4) 0.0838(4) 0.7883(2) 0.0410(14) Uani 1 1 d . . .
H13A H 0.0239 0.1081 0.7637 0.049 Uiso 1 1 calc R A .
C1S C 0.151(3) 0.816(3) 0.7700(17) 0.105(7) Uiso 0.25 1 d PD B -1
H1SA H 0.1028 0.8518 0.7595 0.157 Uiso 0.25 1 calc PR B -1
H1SB H 0.1762 0.8393 0.8002 0.157 Uiso 0.25 1 calc PR B -1
H1SC H 0.1300 0.7574 0.7765 0.157 Uiso 0.25 1 calc PR B -1
C2S C 0.218(2) 0.8130(19) 0.7294(11) 0.105(7) Uiso 0.25 1 d PD B -1
H2S H 0.1904 0.8442 0.7013 0.126 Uiso 0.25 1 calc PR B -1
C3S C 0.236(3) 0.7243(18) 0.7085(14) 0.105(7) Uiso 0.25 1 d PD B -1
H3S1 H 0.1798 0.7058 0.6949 0.126 Uiso 0.25 1 calc PR B -1
H3S2 H 0.2726 0.7354 0.6794 0.126 Uiso 0.25 1 calc PR B -1
C4S C 0.273(3) 0.643(3) 0.7309(19) 0.105(7) Uiso 0.25 1 d PD B -1
H4S1 H 0.2334 0.6190 0.7560 0.126 Uiso 0.25 1 calc PR B -1
H4S2 H 0.2828 0.5993 0.7050 0.126 Uiso 0.25 1 calc PR B -1
C5S C 0.357(3) 0.669(2) 0.755(3) 0.105(7) Uiso 0.25 1 d PD B -1
H5S1 H 0.4048 0.6413 0.7374 0.157 Uiso 0.25 1 calc PR B -1
H5S2 H 0.3573 0.6519 0.7895 0.157 Uiso 0.25 1 calc PR B -1
H5S3 H 0.3639 0.7317 0.7525 0.157 Uiso 0.25 1 calc PR B -1
C6S C 0.298(2) 0.865(2) 0.7400(16) 0.105(7) Uiso 0.25 1 d PD B -1
H6S1 H 0.3188 0.8522 0.7734 0.157 Uiso 0.25 1 calc PR B -1
H6S2 H 0.2848 0.9264 0.7376 0.157 Uiso 0.25 1 calc PR B -1
H6S3 H 0.3428 0.8506 0.7159 0.157 Uiso 0.25 1 calc PR B -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'
Cl Cl 0.1484 0.1585 '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'
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
N1 Ru1 N1 89.997(3) 4 .
N1 Ru1 N1 178.9(2) 4 3
N1 Ru1 N1 89.995(3) . 3
N1 Ru1 N1 89.994(3) 4 2
N1 Ru1 N1 178.9(2) . 2
N1 Ru1 N1 89.992(3) 3 2
N1 Ru1 Ru2 90.57(12) 4 .
N1 Ru1 Ru2 90.57(12) . .
N1 Ru1 Ru2 90.57(12) 3 .
N1 Ru1 Ru2 90.57(12) 2 .
N1 Ru1 O1 89.43(12) 4 .
N1 Ru1 O1 89.43(12) . .
N1 Ru1 O1 89.43(12) 3 .
N1 Ru1 O1 89.43(12) 2 .
Ru2 Ru1 O1 180.000(4) . .
N2 Ru2 N2 89.939(9) 4 .
N2 Ru2 N2 176.2(2) 4 3
N2 Ru2 N2 89.941(9) . 3
N2 Ru2 N2 89.937(9) 4 2
N2 Ru2 N2 176.2(2) . 2
N2 Ru2 N2 89.936(9) 3 2
N2 Ru2 Ru1 88.12(12) 4 .
N2 Ru2 Ru1 88.12(12) . .
N2 Ru2 Ru1 88.12(12) 3 .
N2 Ru2 Ru1 88.12(12) 2 .
N2 Ru2 Cl1 91.88(12) 4 .
N2 Ru2 Cl1 91.88(12) . .
N2 Ru2 Cl1 91.88(12) 3 .
N2 Ru2 Cl1 91.88(12) 2 .
Ru1 Ru2 Cl1 180.000(1) . .
C1 N1 C2B 119.8(11) . .
C1 N1 C2 115.7(6) . .
C1 N1 Ru1 119.2(4) . .
C2B N1 Ru1 120.4(12) . .
C2 N1 Ru1 124.5(6) . .
C1 N2 C8 114.6(5) . .
C1 N2 Ru2 119.8(4) . .
C8 N2 Ru2 125.4(4) . .
N2 C1 N1 122.3(5) . .
C3 C2 C7 120.0 . .
C3 C2 N1 119.3(6) . .
C7 C2 N1 120.6(6) . .
C4 C3 C2 120.0 . .
C3 C4 C5 120.0 . .
C3 C4 Cl2 120.1(4) . .
C5 C4 Cl2 119.9(4) . .
C6 C5 C4 120.0 . .
C7 C6 C5 120.0 . .
C7 C6 Cl3 120.2(4) . .
C5 C6 Cl3 119.8(4) . .
C6 C7 C2 120.0 . .
C3B C2B C7B 119.3(6) . .
C3B C2B N1 119.9(11) . .
C7B C2B N1 120.7(12) . .
C4B C3B C2B 120.0(6) . .
C3B C4B C5B 120.2(7) . .
C3B C4B Cl2B 119.1(7) . .
C5B C4B Cl2B 119.1(6) . .
C6B C5B C4B 118.3(7) . .
C7B C6B C5B 120.5(6) . .
C7B C6B Cl3B 119.8(5) . .
C5B C6B Cl3B 119.8(6) . .
C6B C7B C2B 119.5(6) . .
C9 C8 C13 120.5(6) . .
C9 C8 N2 120.7(5) . .
C13 C8 N2 118.8(5) . .
C8 C9 C10 118.6(6) . .
C11 C10 C9 123.2(6) . .
C11 C10 Cl4 118.7(5) . .
C9 C10 Cl4 118.1(5) . .
C12 C11 C10 117.1(6) . .
C11 C12 C13 122.5(6) . .
C11 C12 Cl5 119.3(5) . .
C13 C12 Cl5 118.2(5) . .
C8 C13 C12 118.0(6) . .
C6S C2S C1S 114.6(8) . .
C6S C2S C3S 114.1(8) . .
C1S C2S C3S 114.8(8) . .
C4S C3S C2S 133(3) . .
C5S C4S C3S 106(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N1 2.053(5) 4
Ru1 N1 2.053(5) .
Ru1 N1 2.053(5) 3
Ru1 N1 2.053(5) 2
Ru1 Ru2 2.3632(12) .
Ru1 O1 2.63(3) .
Ru2 N2 2.103(5) 4
Ru2 N2 2.103(5) .
Ru2 N2 2.103(5) 3
Ru2 N2 2.104(5) 2
Ru2 Cl1 2.381(3) .
Cl4 C10 1.743(7) .
Cl5 C12 1.745(7) .
N1 C1 1.335(7) .
N1 C2B 1.419(9) .
N1 C2 1.420(6) .
N2 C1 1.310(7) .
N2 C8 1.441(7) .
C2 C3 1.3900 .
C2 C7 1.3900 .
C3 C4 1.3900 .
C4 C5 1.3900 .
C4 Cl2 1.694(4) .
C5 C6 1.3900 .
C6 C7 1.3900 .
C6 Cl3 1.716(4) .
C2B C3B 1.391(5) .
C2B C7B 1.393(5) .
C3B C4B 1.389(5) .
C4B C5B 1.391(5) .
C4B Cl2B 1.693(6) .
C5B C6B 1.390(5) .
C6B C7B 1.389(5) .
C6B Cl3B 1.716(5) .
C8 C9 1.377(9) .
C8 C13 1.386(9) .
C9 C10 1.388(9) .
C10 C11 1.366(10) .
C11 C12 1.364(10) .
C12 C13 1.410(9) .
C1S C2S 1.520(5) .
C2S C6S 1.520(5) .
C2S C3S 1.521(5) .
C3S C4S 1.520(5) .
C4S C5S 1.520(5) .
