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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/4/11/16/4111631.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_4111631
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                   13.1235(4)
_cell_length_b                   13.1235(4)
_cell_length_c                   16.5799(10)
_cell_measurement_reflns_used    8790
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.45
_cell_volume                     2855.5(2)
_computing_cell_refinement       SAINT
_computing_data_collection       SAMRT
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16762
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.9536
_exptl_absorpt_correction_T_min  0.9042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.513
_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         2.453
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0436
_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          0.1108
_refine_ls_wR_factor_ref         0.1174
_reflns_number_gt                2835
_reflns_number_total             3269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050828rsi20050208_053738_4.cif
_cod_data_source_block           2at150k
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'C60.50 H61 Cl2 N8 O8 Ru2'
_cod_database_code               4111631
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 0.57243(2) 0.01932(13) Uani 1 4 d S . .
Ru1 Ru 0.2500 0.2500 0.71819(2) 0.01930(13) Uani 1 4 d S . .
Cl1 Cl 0.2500 0.2500 0.86537(7) 0.0202(3) Uani 0.964(3) 4 d SP A 1
Cl1A Cl 0.2500 0.2500 0.4219(18) 0.0202(3) Uani 0.036(3) 4 d SP . 2
N2 N 0.09636(16) 0.27721(16) 0.57349(11) 0.0207(4) Uani 1 1 d . A .
N1 N 0.09931(16) 0.29635(17) 0.71337(11) 0.0217(4) Uani 1 1 d . . .
O20 O -0.13248(17) 0.33436(17) 0.29157(12) 0.0374(5) Uani 1 1 d . . .
C10 C 0.05156(19) 0.3002(2) 0.64339(13) 0.0216(5) Uani 1 1 d . A .
H10A H -0.0180 0.3202 0.6428 0.026 Uiso 1 1 calc R . .
C21 C 0.03624(18) 0.28879(18) 0.50194(15) 0.0229(5) Uani 1 1 d . . .
C22 C -0.0328(2) 0.3696(2) 0.49302(16) 0.0300(5) Uani 1 1 d . A .
H22A H -0.0418 0.4167 0.5359 0.036 Uiso 1 1 calc R . .
C23 C -0.0877(2) 0.3815(2) 0.42282(16) 0.0336(6) Uani 1 1 d . . .
H23A H -0.1341 0.4367 0.4179 0.040 Uiso 1 1 calc R A .
C24 C -0.0759(2) 0.3134(2) 0.35895(15) 0.0293(6) Uani 1 1 d . A .
C25 C -0.0083(2) 0.2330(2) 0.36655(16) 0.0312(6) Uani 1 1 d . . .
H25A H 0.0003 0.1860 0.3235 0.037 Uiso 1 1 calc R A .
C26 C 0.0475(2) 0.2213(2) 0.43795(15) 0.0271(5) Uani 1 1 d . A .
H26A H 0.0939 0.1661 0.4428 0.033 Uiso 1 1 calc R . .
O10 O -0.12608(18) 0.46948(17) 0.96558(13) 0.0432(5) Uani 1 1 d . A .
C27 C -0.1196(3) 0.2677(3) 0.22431(17) 0.0394(7) Uani 1 1 d . . .
H27A H -0.1640 0.2898 0.1801 0.059 Uiso 1 1 calc R . .
H27B H -0.1376 0.1981 0.2402 0.059 Uiso 1 1 calc R . .
H27C H -0.0484 0.2696 0.2065 0.059 Uiso 1 1 calc R . .
C11 C 0.0422(2) 0.3412(2) 0.77854(14) 0.0255(5) Uani 1 1 d . A .
C12 C 0.0016(2) 0.2818(2) 0.84087(16) 0.0292(5) Uani 1 1 d . . .
H12A H 0.0131 0.2104 0.8417 0.035 Uiso 1 1 calc R A .
C13 C -0.0552(2) 0.3270(2) 0.90115(16) 0.0308(6) Uani 1 1 d . A .
H13A H -0.0842 0.2861 0.9425 0.037 Uiso 1 1 calc R . .
C14 C -0.0705(2) 0.4320(2) 0.90203(17) 0.0331(6) Uani 1 1 d . . .
C15 C -0.0301(2) 0.4917(2) 0.84084(18) 0.0342(6) Uani 1 1 d . A .
H15A H -0.0401 0.5634 0.8410 0.041 Uiso 1 1 calc R . .
C16 C 0.0255(2) 0.4452(2) 0.77873(16) 0.0297(6) Uani 1 1 d . . .
H16A H 0.0521 0.4858 0.7362 0.036 Uiso 1 1 calc R A .
C17 C -0.1414(3) 0.5765(3) 0.96884(19) 0.0444(7) Uani 1 1 d . . .
H17A H -0.1823 0.5935 1.0164 0.067 Uiso 1 1 calc R A .
H17B H -0.1772 0.5989 0.9201 0.067 Uiso 1 1 calc R . .
H17C H -0.0753 0.6110 0.9722 0.067 Uiso 1 1 calc R . .
C1S C 0.7500 0.7500 0.7139(10) 0.071(5) Uani 0.50 4 d SP . .
Cl1S Cl 0.8330(3) 0.6778(2) 0.77037(18) 0.0423(7) 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 89.995(1) 4 .
N2 Ru2 N2 89.997(1) 4 2
N2 Ru2 N2 179.02(10) . 2
N2 Ru2 N2 179.02(10) 4 3
N2 Ru2 N2 89.996(1) . 3
N2 Ru2 N2 89.995(1) 2 3
N2 Ru2 Ru1 89.51(5) 4 .
N2 Ru2 Ru1 89.51(5) . .
N2 Ru2 Ru1 89.51(5) 2 .
N2 Ru2 Ru1 89.51(5) 3 .
N2 Ru2 Cl1A 90.49(5) 4 .
N2 Ru2 Cl1A 90.49(5) . .
N2 Ru2 Cl1A 90.49(5) 2 .
N2 Ru2 Cl1A 90.49(5) 3 .
Ru1 Ru2 Cl1A 180.000(4) . .
N1 Ru1 N1 89.915(4) 4 2
N1 Ru1 N1 175.57(10) 4 3
N1 Ru1 N1 89.914(4) 2 3
N1 Ru1 N1 89.913(4) 4 .
N1 Ru1 N1 175.57(10) 2 .
N1 Ru1 N1 89.915(4) 3 .
N1 Ru1 Ru2 87.79(5) 4 .
N1 Ru1 Ru2 87.79(5) 2 .
N1 Ru1 Ru2 87.79(5) 3 .
N1 Ru1 Ru2 87.79(5) . .
N1 Ru1 Cl1 92.21(5) 4 .
N1 Ru1 Cl1 92.21(5) 2 .
N1 Ru1 Cl1 92.21(5) 3 .
N1 Ru1 Cl1 92.21(5) . .
Ru2 Ru1 Cl1 180.0 . .
C1S Cl1A Ru2 179.999(1) 5_666 .
C10 N2 C21 116.9(2) . .
C10 N2 Ru2 118.74(16) . .
C21 N2 Ru2 123.61(15) . .
C10 N1 C11 113.4(2) . .
C10 N1 Ru1 119.91(16) . .
C11 N1 Ru1 125.99(16) . .
C24 O20 C27 116.7(2) . .
N1 C10 N2 123.1(2) . .
C26 C21 C22 118.0(2) . .
C26 C21 N2 120.4(2) . .
C22 C21 N2 121.6(2) . .
C23 C22 C21 120.8(2) . .
C22 C23 C24 120.7(3) . .
O20 C24 C25 125.1(3) . .
O20 C24 C23 115.5(2) . .
C25 C24 C23 119.4(2) . .
C24 C25 C26 119.7(3) . .
C21 C26 C25 121.3(2) . .
C14 O10 C17 117.3(2) . .
C16 C11 C12 119.2(2) . .
C16 C11 N1 119.2(2) . .
C12 C11 N1 121.6(2) . .
C13 C12 C11 120.0(3) . .
C12 C13 C14 120.7(3) . .
O10 C14 C15 124.2(3) . .
O10 C14 C13 116.1(3) . .
C15 C14 C13 119.8(3) . .
C14 C15 C16 119.4(3) . .
C11 C16 C15 120.9(3) . .
Cl1S C1S Cl1S 114.1(10) 3_655 4_565
Cl1S C1S Cl1S 72.8(5) 3_655 .
Cl1S C1S Cl1S 72.8(5) 4_565 .
Cl1S C1S Cl1S 72.8(5) 3_655 2_665
Cl1S C1S Cl1S 72.8(5) 4_565 2_665
Cl1S C1S Cl1S 114.1(10) . 2_665
Cl1S C1S Cl1A 123.0(5) 3_655 5_666
Cl1S C1S Cl1A 123.0(5) 4_565 5_666
Cl1S C1S Cl1A 123.0(5) . 5_666
Cl1S C1S Cl1A 123.0(5) 2_665 5_666
C1S Cl1S Cl1S 53.6(2) . 3_655
C1S Cl1S Cl1S 53.6(2) . 4_565
Cl1S Cl1S Cl1S 89.999(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 2.048(2) 4
Ru2 N2 2.048(2) .
Ru2 N2 2.048(2) 2
Ru2 N2 2.048(2) 3
Ru2 Ru1 2.4168(5) .
Ru2 Cl1A 2.50(3) .
Ru1 N1 2.071(2) 4
Ru1 N1 2.071(2) 2
Ru1 N1 2.071(2) 3
Ru1 N1 2.071(2) .
Ru1 Cl1 2.4403(11) .
Cl1A C1S 2.25(3) 5_666
N2 C10 1.334(3) .
N2 C21 1.433(3) .
N1 C10 1.320(3) .
N1 C11 1.441(3) .
O20 C24 1.370(3) .
O20 C27 1.427(3) .
C21 C26 1.390(4) .
C21 C22 1.403(4) .
C22 C23 1.378(4) .
C23 C24 1.394(4) .
C24 C25 1.384(4) .
C25 C26 1.400(4) .
O10 C14 1.373(3) .
O10 C17 1.420(4) .
C11 C16 1.383(4) .
C11 C12 1.400(4) .
C12 C13 1.381(4) .
C13 C14 1.392(4) .
C14 C15 1.387(4) .
C15 C16 1.402(4) .
C1S Cl1S 1.721(10) 3_655
C1S Cl1S 1.721(10) 4_565
C1S Cl1S 1.721(10) .
C1S Cl1S 1.721(10) 2_665
C1S Cl1A 2.25(3) 5_666
Cl1S Cl1S 2.042(5) 3_655
Cl1S Cl1S 2.042(5) 4_565
