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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/4/11/16/4111628.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_4111628
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                   13.0725(6)
_cell_length_b                   13.0725(6)
_cell_length_c                   16.5571(14)
_cell_measurement_reflns_used    9509
_cell_measurement_temperature    27(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.46
_cell_volume                     2829.4(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      27(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0181
_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            16495
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  0.9519
_exptl_absorpt_correction_T_min  0.9045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.527
_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         2.417
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0419
_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         0.1108
_reflns_number_gt                2903
_reflns_number_total             3209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050828rsi20050208_053738_1.cif
_cod_data_source_block           2at27k
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'C60.50 H61 Cl2 N8 O8 Ru2'
_cod_database_code               4111628
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 0.57040(2) 0.01215(12) Uani 1 4 d S . .
Ru1 Ru 0.2500 0.2500 0.718196(19) 0.01201(12) Uani 1 4 d S . .
Cl1 Cl 0.2500 0.2500 0.86626(6) 0.0107(3) Uani 0.968(3) 4 d SP A 1
Cl1A Cl 0.2500 0.2500 0.4175(19) 0.0107(3) Uani 0.032(3) 4 d SP . 2
N2 N 0.09643(15) 0.27812(15) 0.57253(10) 0.0127(4) Uani 1 1 d . A .
N1 N 0.09966(15) 0.29710(15) 0.71284(10) 0.0135(4) Uani 1 1 d . . .
O20 O -0.13424(14) 0.33452(13) 0.29005(10) 0.0202(4) Uani 1 1 d . . .
C10 C 0.05157(18) 0.30128(17) 0.64261(12) 0.0134(4) Uani 1 1 d . A .
H10A H -0.0182 0.3217 0.6420 0.016 Uiso 1 1 calc R . .
C21 C 0.03537(17) 0.28918(17) 0.50097(14) 0.0156(4) Uani 1 1 d . . .
C22 C -0.03399(18) 0.37023(18) 0.49216(14) 0.0181(5) Uani 1 1 d . A .
H22A H -0.0432 0.4173 0.5353 0.022 Uiso 1 1 calc R . .
C23 C -0.08921(18) 0.38255(19) 0.42149(14) 0.0190(5) Uani 1 1 d . . .
H23A H -0.1355 0.4382 0.4164 0.023 Uiso 1 1 calc R A .
C24 C -0.07726(19) 0.31369(19) 0.35766(13) 0.0174(5) Uani 1 1 d . A .
C25 C -0.00912(19) 0.23282(19) 0.36514(14) 0.0188(5) Uani 1 1 d . . .
H25A H -0.0005 0.1856 0.3220 0.023 Uiso 1 1 calc R A .
C26 C 0.04703(18) 0.22122(18) 0.43689(13) 0.0174(5) Uani 1 1 d . A .
H26A H 0.0938 0.1660 0.4418 0.021 Uiso 1 1 calc R . .
O10 O -0.12599(14) 0.46999(14) 0.96647(11) 0.0252(4) Uani 1 1 d . A .
C27 C -0.1206(2) 0.2677(2) 0.22247(14) 0.0213(5) Uani 1 1 d . . .
H27A H -0.1650 0.2897 0.1781 0.032 Uiso 1 1 calc R . .
H27B H -0.1383 0.1976 0.2382 0.032 Uiso 1 1 calc R . .
H27C H -0.0490 0.2700 0.2048 0.032 Uiso 1 1 calc R . .
C11 C 0.04177(17) 0.34173(19) 0.77820(13) 0.0161(5) Uani 1 1 d . A .
C12 C 0.00182(18) 0.28174(18) 0.84073(14) 0.0180(5) Uani 1 1 d . . .
H12A H 0.0137 0.2100 0.8414 0.022 Uiso 1 1 calc R A .
C13 C -0.05491(17) 0.32688(18) 0.90166(14) 0.0183(5) Uani 1 1 d . A .
H13A H -0.0835 0.2856 0.9432 0.022 Uiso 1 1 calc R . .
C14 C -0.07057(18) 0.43257(19) 0.90269(15) 0.0208(5) Uani 1 1 d . . .
C15 C -0.03065(19) 0.49291(19) 0.84082(15) 0.0223(5) Uani 1 1 d . A .
H15A H -0.0410 0.5648 0.8409 0.027 Uiso 1 1 calc R . .
C16 C 0.02481(19) 0.44629(19) 0.77848(14) 0.0196(5) Uani 1 1 d . . .
H16A H 0.0512 0.4870 0.7358 0.024 Uiso 1 1 calc R A .
C17 C -0.1415(2) 0.5780(2) 0.96936(16) 0.0261(5) Uani 1 1 d . . .
H17A H -0.1825 0.5954 1.0170 0.039 Uiso 1 1 calc R A .
H17B H -0.1776 0.6002 0.9205 0.039 Uiso 1 1 calc R . .
H17C H -0.0752 0.6127 0.9725 0.039 Uiso 1 1 calc R . .
C1S C 0.7500 0.7500 0.7110(6) 0.026(2) Uani 0.50 4 d SP . .
Cl1S Cl 0.83304(15) 0.67622(15) 0.77087(11) 0.0118(4) 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 89.984(2) 4 2
N2 Ru2 N2 89.981(2) 4 .
N2 Ru2 N2 178.01(10) 2 .
N2 Ru2 N2 178.01(10) 4 3
N2 Ru2 N2 89.982(2) 2 3
N2 Ru2 N2 89.983(2) . 3
N2 Ru2 Ru1 89.01(5) 4 .
N2 Ru2 Ru1 89.01(5) 2 .
N2 Ru2 Ru1 89.01(5) . .
N2 Ru2 Ru1 89.01(5) 3 .
N2 Ru2 Cl1A 90.99(5) 4 .
N2 Ru2 Cl1A 90.99(5) 2 .
N2 Ru2 Cl1A 90.99(5) . .
N2 Ru2 Cl1A 90.99(5) 3 .
Ru1 Ru2 Cl1A 180.000(5) . .
N1 Ru1 N1 89.895(5) 4 2
N1 Ru1 N1 175.07(10) 4 3
N1 Ru1 N1 89.893(4) 2 3
N1 Ru1 N1 89.894(4) 4 .
N1 Ru1 N1 175.07(10) 2 .
N1 Ru1 N1 89.894(4) 3 .
N1 Ru1 Ru2 87.53(5) 4 .
N1 Ru1 Ru2 87.53(5) 2 .
N1 Ru1 Ru2 87.53(5) 3 .
N1 Ru1 Ru2 87.53(5) . .
N1 Ru1 Cl1 92.47(5) 4 .
N1 Ru1 Cl1 92.47(5) 2 .
N1 Ru1 Cl1 92.47(5) 3 .
N1 Ru1 Cl1 92.47(5) . .
Ru2 Ru1 Cl1 180.0 . .
C1S Cl1A Ru2 179.999(1) 5_666 .
C10 N2 C21 116.75(19) . .
C10 N2 Ru2 119.21(15) . .
C21 N2 Ru2 123.41(14) . .
C10 N1 C11 113.15(19) . .
C10 N1 Ru1 120.21(15) . .
C11 N1 Ru1 126.03(14) . .
C24 O20 C27 116.69(19) . .
N1 C10 N2 123.1(2) . .
C26 C21 C22 118.3(2) . .
C26 C21 N2 120.2(2) . .
C22 C21 N2 121.4(2) . .
C23 C22 C21 120.9(2) . .
C22 C23 C24 120.4(2) . .
O20 C24 C25 124.9(2) . .
O20 C24 C23 115.4(2) . .
C25 C24 C23 119.7(2) . .
C24 C25 C26 119.5(2) . .
C21 C26 C25 121.2(2) . .
C14 O10 C17 117.0(2) . .
C16 C11 C12 119.4(2) . .
C16 C11 N1 119.0(2) . .
C12 C11 N1 121.6(2) . .
C13 C12 C11 120.0(2) . .
C12 C13 C14 120.6(2) . .
O10 C14 C15 124.2(2) . .
O10 C14 C13 116.1(2) . .
C15 C14 C13 119.7(2) . .
C14 C15 C16 119.3(2) . .
C11 C16 C15 121.0(2) . .
Cl1S C1S Cl1S 71.5(3) 3_655 2_665
Cl1S C1S Cl1S 71.5(3) 3_655 .
Cl1S C1S Cl1S 111.4(5) 2_665 .
Cl1S C1S Cl1S 111.3(5) 3_655 4_565
Cl1S C1S Cl1S 71.5(3) 2_665 4_565
Cl1S C1S Cl1S 71.5(3) . 4_565
Cl1S C1S Cl1A 124.3(3) 3_655 5_666
Cl1S C1S Cl1A 124.3(3) 2_665 5_666
Cl1S C1S Cl1A 124.3(3) . 5_666
Cl1S C1S Cl1A 124.3(3) 4_565 5_666
C1S Cl1S Cl1S 54.27(13) . 3_655
C1S Cl1S Cl1S 54.27(13) . 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 2.0411(19) 4
Ru2 N2 2.0412(19) 2
Ru2 N2 2.0412(19) .
Ru2 N2 2.0412(19) 3
Ru2 Ru1 2.4471(5) .
Ru2 Cl1A 2.53(3) .
Ru1 N1 2.061(2) 4
Ru1 N1 2.061(2) 2
Ru1 N1 2.061(2) 3
Ru1 N1 2.061(2) .
Ru1 Cl1 2.4516(10) .
Cl1A C1S 2.13(3) 5_666
N2 C10 1.335(3) .
N2 C21 1.436(3) .
N1 C10 1.323(3) .
N1 C11 1.444(3) .
O20 C24 1.372(3) .
O20 C27 1.431(3) .
C21 C26 1.392(3) .
C21 C22 1.402(3) .
C22 C23 1.384(3) .
C23 C24 1.397(3) .
C24 C25 1.388(3) .
C25 C26 1.405(3) .
O10 C14 1.371(3) .
O10 C17 1.428(3) .
C11 C16 1.385(3) .
C11 C12 1.400(3) .
C12 C13 1.384(3) .
C13 C14 1.397(3) .
C14 C15 1.394(4) .
C15 C16 1.401(3) .
C1S Cl1S 1.758(6) 3_655
C1S Cl1S 1.758(6) 2_665
C1S Cl1S 1.758(6) .
C1S Cl1S 1.758(6) 4_565
C1S Cl1A 2.13(3) 5_666
Cl1S Cl1S 2.054(3) 3_655
Cl1S Cl1S 2.054(3) 4_565
