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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/16/4111630.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_4111630
loop_
_publ_author_name
'Panagiotis Angaridis'
'F. Albert Cotton'
'Carlos A. Murillo'
'Dino Villagrán'
'Xiaoping Wang'
_publ_section_title
;
 Structural and Magnetic Evidence Concerning Spin Crossover in
 Formamidinate Compounds with Ru25+ Cores
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5008
_journal_page_last               5009
_journal_paper_doi               10.1021/ja050828r
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C60.5 H61 Cl2 N8 O8 Ru2'
_chemical_formula_weight         1301.21
_chemical_name_systematic
; 
tetrakis-[bis-(p-anisyl)-fromamidinato]-chloro-diruthenium(II,III)
0.5 dichloromethane solvate 
;
_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                   13.0913(4)
_cell_length_b                   13.0913(4)
_cell_length_c                   16.5568(11)
_cell_measurement_reflns_used    8595
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.46
_cell_volume                     2837.5(2)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16934
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.9520
_exptl_absorpt_correction_T_min  0.9048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       plate
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.431
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0430
_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)+(0.0685P)²+3.7262P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                2712
_reflns_number_total             3224
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050828rsi20050208_053738_3.cif
_cod_data_source_block           2at100k
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'C60.50 H61 Cl2 N8 O8 Ru2'
_cod_database_code               4111630
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
Ru2 Ru 0.2500 0.2500 0.57143(2) 0.01615(13) Uani 1 4 d S . .
Ru1 Ru 0.2500 0.2500 0.71813(2) 0.01602(13) Uani 1 4 d S . .
Cl1 Cl 0.2500 0.2500 0.86573(7) 0.0155(3) Uani 0.966(3) 4 d SP A 1
Cl1A Cl 0.2500 0.2500 0.4205(19) 0.0155(3) Uani 0.034(3) 4 d SP . 2
N2 N 0.09644(15) 0.27758(16) 0.57302(11) 0.0166(4) Uani 1 1 d . A .
N1 N 0.09957(16) 0.29675(17) 0.71306(11) 0.0175(4) Uani 1 1 d . . .
O20 O -0.13330(16) 0.33447(16) 0.29092(11) 0.0293(5) Uani 1 1 d . . .
C10 C 0.05140(19) 0.30088(19) 0.64295(13) 0.0174(5) Uani 1 1 d . A .
H10A H -0.0182 0.3213 0.6423 0.021 Uiso 1 1 calc R . .
C21 C 0.03585(19) 0.28893(19) 0.50139(15) 0.0192(5) Uani 1 1 d . . .
C22 C -0.0332(2) 0.3700(2) 0.49252(16) 0.0244(5) Uani 1 1 d . A .
H22A H -0.0421 0.4174 0.5355 0.029 Uiso 1 1 calc R . .
C23 C -0.0884(2) 0.3819(2) 0.42209(16) 0.0262(6) Uani 1 1 d . . .
H23A H -0.1349 0.4373 0.4171 0.031 Uiso 1 1 calc R A .
C24 C -0.0766(2) 0.3136(2) 0.35840(15) 0.0233(5) Uani 1 1 d . A .
C25 C -0.0088(2) 0.2328(2) 0.36592(16) 0.0254(6) Uani 1 1 d . . .
H25A H -0.0005 0.1855 0.3229 0.030 Uiso 1 1 calc R A .
C26 C 0.0472(2) 0.2214(2) 0.43732(15) 0.0226(5) Uani 1 1 d . A .
H26A H 0.0940 0.1663 0.4421 0.027 Uiso 1 1 calc R . .
O10 O -0.12588(16) 0.46970(16) 0.96608(12) 0.0347(5) Uani 1 1 d . A .
C27 C -0.1201(2) 0.2676(2) 0.22349(16) 0.0309(6) Uani 1 1 d . . .
H27A H -0.1645 0.2896 0.1791 0.046 Uiso 1 1 calc R . .
H27B H -0.1380 0.1978 0.2393 0.046 Uiso 1 1 calc R . .
H27C H -0.0487 0.2696 0.2057 0.046 Uiso 1 1 calc R . .
C11 C 0.04198(19) 0.3414(2) 0.77849(14) 0.0206(5) Uani 1 1 d . A .
C12 C 0.0018(2) 0.2820(2) 0.84079(15) 0.0236(5) Uani 1 1 d . . .
H12A H 0.0136 0.2104 0.8416 0.028 Uiso 1 1 calc R A .
C13 C -0.0551(2) 0.3270(2) 0.90132(16) 0.0250(5) Uani 1 1 d . A .
H13A H -0.0839 0.2858 0.9427 0.030 Uiso 1 1 calc R . .
C14 C -0.0705(2) 0.4322(2) 0.90231(17) 0.0277(6) Uani 1 1 d . . .
C15 C -0.0303(2) 0.4922(2) 0.84079(17) 0.0286(6) Uani 1 1 d . A .
H15A H -0.0403 0.5641 0.8410 0.034 Uiso 1 1 calc R . .
C16 C 0.0250(2) 0.4458(2) 0.77861(15) 0.0248(6) Uani 1 1 d . . .
H16A H 0.0513 0.4864 0.7359 0.030 Uiso 1 1 calc R A .
C17 C -0.1413(2) 0.5772(2) 0.96909(18) 0.0357(7) Uani 1 1 d . . .
H17A H -0.1822 0.5944 1.0167 0.054 Uiso 1 1 calc R A .
H17B H -0.1773 0.5994 0.9203 0.054 Uiso 1 1 calc R . .
H17C H -0.0751 0.6118 0.9723 0.054 Uiso 1 1 calc R . .
C1S C 0.7500 0.7500 0.7125(9) 0.050(4) Uani 0.50 4 d SP . .
Cl1S Cl 0.8330(2) 0.6770(2) 0.77068(15) 0.0277(5) Uani 0.25 1 d P . .
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'
O O 0.0106 0.0060 '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'
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 Ru2 N2 89.990(2) . 4
N2 Ru2 N2 178.52(10) . 2
N2 Ru2 N2 89.990(2) 4 2
N2 Ru2 N2 89.992(2) . 3
N2 Ru2 N2 178.52(10) 4 3
N2 Ru2 N2 89.990(1) 2 3
N2 Ru2 Ru1 89.26(5) . .
N2 Ru2 Ru1 89.26(5) 4 .
N2 Ru2 Ru1 89.26(5) 2 .
N2 Ru2 Ru1 89.26(5) 3 .
N2 Ru2 Cl1A 90.74(5) . .
N2 Ru2 Cl1A 90.74(5) 4 .
N2 Ru2 Cl1A 90.74(5) 2 .
N2 Ru2 Cl1A 90.74(5) 3 .
Ru1 Ru2 Cl1A 180.000(5) . .
N1 Ru1 N1 89.907(4) 4 .
N1 Ru1 N1 175.34(10) 4 3
N1 Ru1 N1 89.905(5) . 3
N1 Ru1 N1 89.905(5) 4 2
N1 Ru1 N1 175.34(10) . 2
N1 Ru1 N1 89.904(4) 3 2
N1 Ru1 Ru2 87.67(5) 4 .
N1 Ru1 Ru2 87.67(5) . .
N1 Ru1 Ru2 87.67(5) 3 .
N1 Ru1 Ru2 87.67(5) 2 .
N1 Ru1 Cl1 92.33(5) 4 .
N1 Ru1 Cl1 92.33(5) . .
N1 Ru1 Cl1 92.33(5) 3 .
N1 Ru1 Cl1 92.33(5) 2 .
Ru2 Ru1 Cl1 180.0 . .
C1S Cl1A Ru2 180.0 5_666 .
C10 N2 C21 116.7(2) . .
C10 N2 Ru2 119.10(16) . .
C21 N2 Ru2 123.49(15) . .
C10 N1 C11 113.2(2) . .
C10 N1 Ru1 120.19(16) . .
C11 N1 Ru1 126.01(15) . .
C24 O20 C27 116.7(2) . .
N1 C10 N2 122.8(2) . .
C26 C21 C22 118.1(2) . .
C26 C21 N2 120.5(2) . .
C22 C21 N2 121.4(2) . .
C23 C22 C21 120.7(2) . .
C22 C23 C24 120.6(2) . .
O20 C24 C25 124.9(2) . .
O20 C24 C23 115.5(2) . .
C25 C24 C23 119.6(2) . .
C24 C25 C26 119.5(2) . .
C21 C26 C25 121.5(2) . .
C14 O10 C17 117.1(2) . .
C16 C11 C12 119.2(2) . .
C16 C11 N1 119.0(2) . .
C12 C11 N1 121.8(2) . .
C13 C12 C11 120.2(3) . .
C12 C13 C14 120.6(3) . .
O10 C14 C15 124.2(3) . .
O10 C14 C13 116.1(2) . .
C15 C14 C13 119.7(3) . .
C14 C15 C16 119.4(3) . .
C11 C16 C15 120.9(2) . .
Cl1S C1S Cl1S 112.8(8) 2_665 .
Cl1S C1S Cl1S 72.1(4) 2_665 3_655
Cl1S C1S Cl1S 72.1(4) . 3_655
Cl1S C1S Cl1S 72.1(4) 2_665 4_565
Cl1S C1S Cl1S 72.1(4) . 4_565
Cl1S C1S Cl1S 112.8(8) 3_655 4_565
Cl1S C1S Cl1A 123.6(4) 2_665 5_666
Cl1S C1S Cl1A 123.6(4) . 5_666
Cl1S C1S Cl1A 123.6(4) 3_655 5_666
Cl1S C1S Cl1A 123.6(4) 4_565 5_666
C1S Cl1S Cl1S 53.93(19) . 4_565
C1S Cl1S Cl1S 53.93(19) . 3_655
Cl1S Cl1S Cl1S 90.001(1) 4_565 3_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru2 N2 2.043(2) .
Ru2 N2 2.043(2) 4
Ru2 N2 2.043(2) 2
Ru2 N2 2.043(2) 3
Ru2 Ru1 2.4289(5) .
Ru2 Cl1A 2.50(3) .
Ru1 N1 2.064(2) 4
Ru1 N1 2.064(2) .
Ru1 N1 2.064(2) 3
Ru1 N1 2.064(2) 2
Ru1 Cl1 2.4438(11) .
Cl1A C1S 2.20(3) 5_666
N2 C10 1.335(3) .
N2 C21 1.434(3) .
N1 C10 1.322(3) .
N1 C11 1.444(3) .
O20 C24 1.369(3) .
O20 C27 1.429(3) .
C21 C26 1.389(4) .
C21 C22 1.402(4) .
C22 C23 1.381(4) .
C23 C24 1.391(4) .
C24 C25 1.387(4) .
C25 C26 1.399(4) .
O10 C14 1.371(3) .
O10 C17 1.423(4) .
C11 C16 1.385(4) .
C11 C12 1.395(4) .
C12 C13 1.380(4) .
C13 C14 1.392(4) .
C14 C15 1.390(4) .
C15 C16 1.397(4) .
C1S Cl1S 1.739(8) 2_665
C1S Cl1S 1.739(8) .
C1S Cl1S 1.739(8) 3_655
C1S Cl1S 1.739(8) 4_565
C1S Cl1A 2.20(3) 5_666
Cl1S Cl1S 2.047(4) 4_565
Cl1S Cl1S 2.047(4) 3_655
