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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/4/11/16/4111633.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_4111633
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                   13.2460(5)
_cell_length_b                   13.2460(5)
_cell_length_c                   16.6843(13)
_cell_measurement_reflns_used    7826
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.44
_cell_volume                     2927.4(3)
_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      299(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       17
_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            17705
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.9064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.476
_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         1.861
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0411
_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)+(0.0585P)²+2.7262P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                2751
_reflns_number_total             3359
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050828rsi20050208_053738_6.cif
_cod_data_source_block           2at299k
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'C60.50 H61 Cl2 N8 O8 Ru2'
_cod_database_code               4111633
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 0.57507(2) 0.03025(13) Uani 1 4 d S . .
Ru1 Ru 0.2500 0.2500 0.71873(2) 0.03080(13) Uani 1 4 d S . .
Cl1 Cl 0.2500 0.2500 0.86475(7) 0.0364(3) Uani 0.962(3) 4 d SP A 1
Cl1A Cl 0.2500 0.2500 0.4287(18) 0.0364(3) Uani 0.038(3) 4 d SP A 2
N2 N 0.09694(16) 0.27618(17) 0.57534(12) 0.0335(4) Uani 1 1 d . A .
N1 N 0.09988(17) 0.29577(18) 0.71427(12) 0.0354(5) Uani 1 1 d . . .
O20 O -0.1292(2) 0.3339(2) 0.29468(14) 0.0667(7) Uani 1 1 d . . .
C10 C 0.0527(2) 0.2989(2) 0.64476(14) 0.0353(6) Uani 1 1 d . A .
H10A H -0.0149 0.3178 0.6441 0.042 Uiso 1 1 calc R . .
C21 C 0.03750(19) 0.2878(2) 0.50406(16) 0.0355(5) Uani 1 1 d . . .
C22 C -0.0307(2) 0.3680(2) 0.49470(19) 0.0491(7) Uani 1 1 d . A .
H22A H -0.0395 0.4140 0.5363 0.059 Uiso 1 1 calc R . .
C23 C -0.0847(3) 0.3796(3) 0.42501(18) 0.0555(8) Uani 1 1 d . . .
H23A H -0.1298 0.4330 0.4203 0.067 Uiso 1 1 calc R A .
C24 C -0.0731(2) 0.3129(2) 0.36144(17) 0.0473(7) Uani 1 1 d . A .
C25 C -0.0064(3) 0.2336(2) 0.36955(18) 0.0505(7) Uani 1 1 d . . .
H25A H 0.0021 0.1879 0.3278 0.061 Uiso 1 1 calc R A .
C26 C 0.0485(2) 0.2217(2) 0.44046(17) 0.0435(6) Uani 1 1 d . A .
H26A H 0.0936 0.1681 0.4450 0.052 Uiso 1 1 calc R . .
O10 O -0.1264(2) 0.4680(2) 0.96348(14) 0.0716(7) Uani 1 1 d . A .
C27 C -0.1177(4) 0.2682(3) 0.2276(2) 0.0736(11) Uani 1 1 d . . .
H27A H -0.1611 0.2902 0.1849 0.110 Uiso 1 1 calc R . .
H27B H -0.1355 0.2007 0.2429 0.110 Uiso 1 1 calc R . .
H27C H -0.0488 0.2696 0.2097 0.110 Uiso 1 1 calc R . .
C11 C 0.0428(2) 0.3406(2) 0.77901(15) 0.0395(6) Uani 1 1 d . A .
C12 C 0.0018(2) 0.2823(2) 0.84047(17) 0.0466(7) Uani 1 1 d . . .
H12A H 0.0128 0.2130 0.8415 0.056 Uiso 1 1 calc R A .
C13 C -0.0554(2) 0.3273(3) 0.89998(18) 0.0523(7) Uani 1 1 d . A .
H13A H -0.0842 0.2876 0.9399 0.063 Uiso 1 1 calc R . .
C14 C -0.0703(2) 0.4308(3) 0.90079(19) 0.0515(7) Uani 1 1 d . . .
C15 C -0.0292(3) 0.4893(3) 0.84056(19) 0.0538(8) Uani 1 1 d . A .
H15A H -0.0386 0.5589 0.8406 0.065 Uiso 1 1 calc R . .
C16 C 0.0266(2) 0.4433(2) 0.77944(18) 0.0477(7) Uani 1 1 d . . .
H16A H 0.0531 0.4827 0.7384 0.057 Uiso 1 1 calc R A .
C17 C -0.1412(3) 0.5735(3) 0.9673(2) 0.0753(11) Uani 1 1 d . . .
H17A H -0.1810 0.5896 1.0137 0.113 Uiso 1 1 calc R A .
H17B H -0.1758 0.5957 0.9199 0.113 Uiso 1 1 calc R . .
H17C H -0.0770 0.6067 0.9709 0.113 Uiso 1 1 calc R . .
C1S C 0.7500 0.7500 0.7178(14) 0.129(10) Uani 0.50 4 d SP . .
Cl1S Cl 0.8332(5) 0.6815(4) 0.7700(3) 0.0989(15) 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 90.001(1) 4 2
N2 Ru2 N2 179.75(11) 4 3
N2 Ru2 N2 90.0 2 3
N2 Ru2 N2 90.0 4 .
N2 Ru2 N2 179.75(11) 2 .
N2 Ru2 N2 89.999(1) 3 .
N2 Ru2 Ru1 89.88(5) 4 .
N2 Ru2 Ru1 89.88(5) 2 .
N2 Ru2 Ru1 89.88(5) 3 .
N2 Ru2 Ru1 89.88(5) . .
N2 Ru2 Cl1A 90.12(5) 4 .
N2 Ru2 Cl1A 90.12(5) 2 .
N2 Ru2 Cl1A 90.12(5) 3 .
N2 Ru2 Cl1A 90.12(5) . .
Ru1 Ru2 Cl1A 180.000(5) . .
N1 Ru1 N1 89.928(4) 4 2
N1 Ru1 N1 89.927(4) 4 .
N1 Ru1 N1 175.89(11) 2 .
N1 Ru1 N1 175.89(11) 4 3
N1 Ru1 N1 89.926(4) 2 3
N1 Ru1 N1 89.925(4) . 3
N1 Ru1 Ru2 87.95(5) 4 .
N1 Ru1 Ru2 87.95(5) 2 .
N1 Ru1 Ru2 87.95(5) . .
N1 Ru1 Ru2 87.95(5) 3 .
N1 Ru1 Cl1 92.05(5) 4 .
N1 Ru1 Cl1 92.05(5) 2 .
N1 Ru1 Cl1 92.05(5) . .
N1 Ru1 Cl1 92.05(5) 3 .
Ru2 Ru1 Cl1 180.0 . .
C10 N2 C21 117.0(2) . .
C10 N2 Ru2 118.28(16) . .
C21 N2 Ru2 123.88(16) . .
C10 N1 C11 113.4(2) . .
C10 N1 Ru1 119.61(17) . .
C11 N1 Ru1 126.34(16) . .
C24 O20 C27 117.2(3) . .
N1 C10 N2 123.3(2) . .
C26 C21 C22 117.5(2) . .
C26 C21 N2 120.6(2) . .
C22 C21 N2 121.8(2) . .
C23 C22 C21 120.9(3) . .
C22 C23 C24 121.2(3) . .
O20 C24 C25 125.7(3) . .
O20 C24 C23 115.6(3) . .
C25 C24 C23 118.7(3) . .
C24 C25 C26 120.1(3) . .
C21 C26 C25 121.5(3) . .
C14 O10 C17 117.6(3) . .
C16 C11 C12 118.8(3) . .
C16 C11 N1 119.4(3) . .
C12 C11 N1 121.8(3) . .
C13 C12 C11 120.2(3) . .
C12 C13 C14 120.7(3) . .
O10 C14 C15 124.5(3) . .
O10 C14 C13 116.0(3) . .
C15 C14 C13 119.5(3) . .
C14 C15 C16 119.6(3) . .
C11 C16 C15 121.1(3) . .
Cl1S C1S Cl1S 74.2(6) 3_655 .
Cl1S C1S Cl1S 74.2(6) 3_655 2_665
Cl1S C1S Cl1S 117.2(14) . 2_665
Cl1S C1S Cl1S 117.2(14) 3_655 4_565
Cl1S C1S Cl1S 74.2(6) . 4_565
Cl1S C1S Cl1S 74.2(6) 2_665 4_565
C1S Cl1S Cl1S 52.9(3) . 3_655
C1S Cl1S Cl1S 52.9(3) . 4_565
Cl1S Cl1S Cl1S 90.000(2) 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 2.057(2) 4
Ru2 N2 2.057(2) 2
Ru2 N2 2.057(2) 3
Ru2 N2 2.057(2) .
Ru2 Ru1 2.3968(5) .
Ru2 Cl1A 2.44(3) .
Ru1 N1 2.080(2) 4
Ru1 N1 2.080(2) 2
Ru1 N1 2.080(2) .
Ru1 N1 2.080(2) 3
Ru1 Cl1 2.4361(13) .
N2 C10 1.333(3) .
N2 C21 1.435(3) .
N1 C10 1.318(3) .
N1 C11 1.446(3) .
O20 C24 1.368(3) .
O20 C27 1.426(4) .
C21 C26 1.384(4) .
C21 C22 1.403(4) .
C22 C23 1.374(4) .
C23 C24 1.389(4) .
C24 C25 1.379(4) .
C25 C26 1.398(4) .
O10 C14 1.374(4) .
O10 C17 1.413(5) .
C11 C16 1.377(4) .
C11 C12 1.394(4) .
C12 C13 1.383(4) .
C13 C14 1.386(5) .
C14 C15 1.380(5) .
C15 C16 1.399(4) .
C1S Cl1S 1.672(13) 3_655
C1S Cl1S 1.672(13) .
C1S Cl1S 1.672(13) 2_665
C1S Cl1S 1.672(13) 4_565
Cl1S Cl1S 2.018(8) 3_655
Cl1S Cl1S 2.018(8) 4_565
