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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/4/11/16/4111629.cif $
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#
# 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_4111629
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                   13.0675(4)
_cell_length_b                   13.0675(4)
_cell_length_c                   16.5408(11)
_cell_measurement_reflns_used    8809
_cell_measurement_temperature    60(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.46
_cell_volume                     2824.5(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      60(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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14694
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.9531
_exptl_absorpt_correction_T_min  0.9032
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.530
_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         2.164
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0428
_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          0.1113
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                2290
_reflns_number_total             2501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050828rsi20050208_053738_2.cif
_cod_data_source_block           2at60k
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'C60.50 H61 Cl2 N8 O8 Ru2'
_cod_database_code               4111629
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 0.57068(2) 0.01523(17) Uani 1 4 d S . .
Ru1 Ru 0.2500 0.2500 0.71818(2) 0.01497(17) Uani 1 4 d S . .
Cl1 Cl 0.2500 0.2500 0.86611(7) 0.0135(3) Uani 0.967(3) 4 d SP A 1
Cl1A Cl 0.2500 0.2500 0.417(2) 0.0135(3) Uani 0.033(3) 4 d SP . 2
N2 N 0.09646(18) 0.27823(18) 0.57268(12) 0.0161(5) Uani 1 1 d . A .
N1 N 0.09953(18) 0.29719(18) 0.71291(12) 0.0164(5) Uani 1 1 d . . .
O20 O -0.13381(17) 0.33453(16) 0.29028(12) 0.0253(5) Uani 1 1 d . . .
C10 C 0.0517(2) 0.3010(2) 0.64273(14) 0.0159(6) Uani 1 1 d . A .
H10A H -0.0182 0.3209 0.6421 0.019 Uiso 1 1 calc R . .
C21 C 0.0357(2) 0.2891(2) 0.50095(17) 0.0181(6) Uani 1 1 d . . .
C22 C -0.0339(2) 0.3703(2) 0.49212(17) 0.0224(6) Uani 1 1 d . A .
H22A H -0.0430 0.4175 0.5352 0.027 Uiso 1 1 calc R . .
C23 C -0.0890(2) 0.3823(2) 0.42167(17) 0.0233(6) Uani 1 1 d . . .
H23A H -0.1354 0.4379 0.4165 0.028 Uiso 1 1 calc R A .
C24 C -0.0771(2) 0.3135(2) 0.35799(16) 0.0215(6) Uani 1 1 d . A .
C25 C -0.0090(2) 0.2327(2) 0.36538(17) 0.0228(6) Uani 1 1 d . . .
H25A H -0.0003 0.1855 0.3223 0.027 Uiso 1 1 calc R A .
C26 C 0.0469(2) 0.2214(2) 0.43689(16) 0.0210(6) Uani 1 1 d . A .
H26A H 0.0936 0.1660 0.4418 0.025 Uiso 1 1 calc R . .
O10 O -0.12593(17) 0.46997(16) 0.96636(12) 0.0306(5) Uani 1 1 d . A .
C27 C -0.1203(3) 0.2677(3) 0.22264(17) 0.0272(7) Uani 1 1 d . . .
H27A H -0.1648 0.2897 0.1782 0.041 Uiso 1 1 calc R . .
H27B H -0.1381 0.1976 0.2384 0.041 Uiso 1 1 calc R . .
H27C H -0.0488 0.2699 0.2049 0.041 Uiso 1 1 calc R . .
C11 C 0.0419(2) 0.3415(2) 0.77828(16) 0.0197(6) Uani 1 1 d . A .
C12 C 0.0018(2) 0.2821(2) 0.84081(17) 0.0219(6) Uani 1 1 d . . .
H12A H 0.0138 0.2104 0.8416 0.026 Uiso 1 1 calc R A .
C13 C -0.0552(2) 0.3269(2) 0.90155(17) 0.0223(6) Uani 1 1 d . A .
H13A H -0.0840 0.2856 0.9430 0.027 Uiso 1 1 calc R . .
C14 C -0.0707(2) 0.4324(2) 0.90241(18) 0.0254(6) Uani 1 1 d . . .
C15 C -0.0304(2) 0.4927(2) 0.84095(18) 0.0264(7) Uani 1 1 d . A .
H15A H -0.0402 0.5647 0.8413 0.032 Uiso 1 1 calc R . .
C16 C 0.0248(2) 0.4460(2) 0.77867(16) 0.0234(6) Uani 1 1 d . . .
H16A H 0.0510 0.4868 0.7359 0.028 Uiso 1 1 calc R A .
C17 C -0.1415(3) 0.5777(3) 0.96925(19) 0.0320(7) Uani 1 1 d . . .
H17A H -0.1824 0.5950 1.0169 0.048 Uiso 1 1 calc R A .
H17B H -0.1776 0.5998 0.9204 0.048 Uiso 1 1 calc R . .
H17C H -0.0751 0.6124 0.9724 0.048 Uiso 1 1 calc R . .
C1S C 0.7500 0.7500 0.7114(8) 0.041(4) Uani 0.50 4 d SP . .
Cl1S Cl 0.8328(2) 0.6765(2) 0.77085(15) 0.0191(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 89.986(2) 2 3
N2 Ru2 N2 178.15(12) 2 .
N2 Ru2 N2 89.984(2) 3 .
N2 Ru2 N2 89.986(2) 2 4
N2 Ru2 N2 178.15(12) 3 4
N2 Ru2 N2 89.984(2) . 4
N2 Ru2 Ru1 89.07(6) 2 .
N2 Ru2 Ru1 89.07(6) 3 .
N2 Ru2 Ru1 89.07(6) . .
N2 Ru2 Ru1 89.07(6) 4 .
N2 Ru2 Cl1A 90.93(6) 2 .
N2 Ru2 Cl1A 90.93(6) 3 .
N2 Ru2 Cl1A 90.93(6) . .
N2 Ru2 Cl1A 90.93(6) 4 .
Ru1 Ru2 Cl1A 180.000(6) . .
N1 Ru1 N1 89.899(5) 2 3
N1 Ru1 N1 89.899(5) 2 4
N1 Ru1 N1 175.15(11) 3 4
N1 Ru1 N1 175.15(11) 2 .
N1 Ru1 N1 89.895(5) 3 .
N1 Ru1 N1 89.898(5) 4 .
N1 Ru1 Ru2 87.58(6) 2 .
N1 Ru1 Ru2 87.58(6) 3 .
N1 Ru1 Ru2 87.58(6) 4 .
N1 Ru1 Ru2 87.58(6) . .
N1 Ru1 Cl1 92.42(6) 2 .
N1 Ru1 Cl1 92.42(6) 3 .
N1 Ru1 Cl1 92.42(6) 4 .
N1 Ru1 Cl1 92.42(6) . .
Ru2 Ru1 Cl1 180.0 . .
C1S Cl1A Ru2 179.999(1) 5_666 .
C10 N2 C21 117.0(2) . .
C10 N2 Ru2 119.10(18) . .
C21 N2 Ru2 123.27(17) . .
C10 N1 C11 113.5(2) . .
C10 N1 Ru1 119.99(18) . .
C11 N1 Ru1 125.98(17) . .
C24 O20 C27 116.8(2) . .
N1 C10 N2 123.3(3) . .
C26 C21 C22 118.0(3) . .
C26 C21 N2 120.7(2) . .
C22 C21 N2 121.2(2) . .
C23 C22 C21 120.7(3) . .
C22 C23 C24 120.5(3) . .
O20 C24 C25 124.9(3) . .
O20 C24 C23 115.4(3) . .
C25 C24 C23 119.7(3) . .
C24 C25 C26 119.4(3) . .
C21 C26 C25 121.6(3) . .
C14 O10 C17 117.1(2) . .
C16 C11 C12 119.0(3) . .
C16 C11 N1 119.0(3) . .
C12 C11 N1 122.0(3) . .
C13 C12 C11 120.4(3) . .
C12 C13 C14 120.4(3) . .
O10 C14 C15 124.1(3) . .
O10 C14 C13 116.0(3) . .
C15 C14 C13 119.9(3) . .
C14 C15 C16 119.2(3) . .
C11 C16 C15 121.1(3) . .
Cl1S C1S Cl1S 111.6(8) 3_655 4_565
Cl1S C1S Cl1S 71.6(4) 3_655 2_665
Cl1S C1S Cl1S 71.6(4) 4_565 2_665
Cl1S C1S Cl1S 71.6(4) 3_655 .
Cl1S C1S Cl1S 71.6(4) 4_565 .
Cl1S C1S Cl1S 111.6(8) 2_665 .
Cl1S C1S Cl1A 124.2(4) 3_655 5_666
Cl1S C1S Cl1A 124.2(4) 4_565 5_666
Cl1S C1S Cl1A 124.2(4) 2_665 5_666
Cl1S C1S Cl1A 124.2(4) . 5_666
C1S Cl1S Cl1S 54.21(19) . 3_655
C1S Cl1S Cl1S 54.21(19) . 4_565
Cl1S Cl1S Cl1S 89.997(1) 3_655 4_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru2 N2 2.040(2) 2
Ru2 N2 2.040(2) 3
Ru2 N2 2.040(2) .
Ru2 N2 2.040(2) 4
Ru2 Ru1 2.4397(6) .
Ru2 Cl1A 2.54(4) .
Ru1 N1 2.062(2) 2
Ru1 N1 2.063(2) 3
Ru1 N1 2.063(2) 4
Ru1 N1 2.063(2) .
Ru1 Cl1 2.4469(12) .
Cl1A C1S 2.12(4) 5_666
N2 C10 1.331(3) .
N2 C21 1.435(3) .
N1 C10 1.319(3) .
N1 C11 1.439(3) .
O20 C24 1.371(3) .
O20 C27 1.430(3) .
C21 C26 1.388(4) .
C21 C22 1.405(4) .
C22 C23 1.379(4) .
C23 C24 1.393(4) .
C24 C25 1.387(4) .
C25 C26 1.397(4) .
O10 C14 1.371(3) .
O10 C17 1.423(4) .
C11 C16 1.384(4) .
C11 C12 1.395(4) .
C12 C13 1.381(4) .
C13 C14 1.393(4) .
C14 C15 1.390(4) .
C15 C16 1.397(4) .
C1S Cl1S 1.749(8) 3_655
C1S Cl1S 1.749(8) 4_565
C1S Cl1S 1.749(8) 2_665
C1S Cl1S 1.749(8) .
C1S Cl1A 2.12(4) 5_666
Cl1S Cl1S 2.046(4) 3_655
Cl1S Cl1S 2.046(4) 4_565
