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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/4/11/16/4111632.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_4111632
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            'C30.25 H30.5 Cl N4 O4 Ru'
_chemical_formula_weight         650.61
_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            4
_cell_length_a                   13.1651(4)
_cell_length_b                   13.1651(4)
_cell_length_c                   16.6065(11)
_cell_measurement_reflns_used    8809
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.46
_cell_volume                     2878.2(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      220(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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0161
_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       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17594
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.9539
_exptl_absorpt_correction_T_min  0.9049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.501
_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         2.276
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0422
_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          0.1083
_refine_ls_wR_factor_ref         0.1171
_reflns_number_gt                2802
_reflns_number_total             3314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050828rsi20050208_053738_5.cif
_cod_data_source_block           2at220k
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'C30.25 H30.50 Cl N4 O4 Ru'
_cod_database_code               4111632
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 0.57374(2) 0.02396(13) Uani 1 4 d S . .
Ru1 Ru 0.2500 0.2500 0.71837(2) 0.02417(13) Uani 1 4 d S . .
Cl1 Cl 0.2500 0.2500 0.86496(7) 0.0269(3) Uani 0.961(3) 4 d SP A 1
Cl1A Cl 0.2500 0.2500 0.4257(17) 0.0269(3) Uani 0.039(3) 4 d SP A 2
N2 N 0.09654(16) 0.27656(17) 0.57437(11) 0.0261(4) Uani 1 1 d . A .
N1 N 0.09954(17) 0.29607(17) 0.71378(12) 0.0275(4) Uani 1 1 d . . .
O20 O -0.13095(19) 0.33416(18) 0.29293(13) 0.0493(6) Uani 1 1 d . . .
C10 C 0.0519(2) 0.2994(2) 0.64404(14) 0.0275(5) Uani 1 1 d . A .
H10A H -0.0168 0.3189 0.6434 0.033 Uiso 1 1 calc R . .
C21 C 0.03690(19) 0.28827(19) 0.50296(16) 0.0283(5) Uani 1 1 d . . .
C22 C -0.0319(2) 0.3688(2) 0.49369(18) 0.0379(6) Uani 1 1 d . A .
H22A H -0.0410 0.4154 0.5360 0.046 Uiso 1 1 calc R . .
C23 C -0.0863(2) 0.3807(2) 0.42372(18) 0.0427(7) Uani 1 1 d . . .
H23A H -0.1319 0.4352 0.4188 0.051 Uiso 1 1 calc R A .
C24 C -0.0748(2) 0.3132(2) 0.36003(16) 0.0368(6) Uani 1 1 d . A .
C25 C -0.0075(2) 0.2331(2) 0.36793(17) 0.0394(6) Uani 1 1 d . . .
H25A H 0.0008 0.1866 0.3255 0.047 Uiso 1 1 calc R A .
C26 C 0.0479(2) 0.2214(2) 0.43905(16) 0.0338(6) Uani 1 1 d . A .
H26A H 0.0937 0.1670 0.4437 0.041 Uiso 1 1 calc R . .
O10 O -0.12615(19) 0.46887(19) 0.96473(14) 0.0551(6) Uani 1 1 d . A .
C27 C -0.1188(3) 0.2679(3) 0.22574(19) 0.0536(9) Uani 1 1 d . . .
H27A H -0.1628 0.2900 0.1822 0.080 Uiso 1 1 calc R . .
H27B H -0.1368 0.1992 0.2414 0.080 Uiso 1 1 calc R . .
H27C H -0.0487 0.2695 0.2079 0.080 Uiso 1 1 calc R . .
C11 C 0.0424(2) 0.3409(2) 0.77877(15) 0.0314(6) Uani 1 1 d . A .
C12 C 0.0016(2) 0.2823(2) 0.84072(17) 0.0369(6) Uani 1 1 d . . .
H12A H 0.0130 0.2118 0.8416 0.044 Uiso 1 1 calc R A .
C13 C -0.0554(2) 0.3270(2) 0.90065(17) 0.0401(6) Uani 1 1 d . A .
H13A H -0.0844 0.2866 0.9412 0.048 Uiso 1 1 calc R . .
C14 C -0.0703(2) 0.4314(2) 0.90144(18) 0.0407(6) Uani 1 1 d . . .
C15 C -0.0298(2) 0.4906(2) 0.84068(19) 0.0425(7) Uani 1 1 d . A .
H15A H -0.0397 0.5613 0.8408 0.051 Uiso 1 1 calc R . .
C16 C 0.0259(2) 0.4444(2) 0.77912(17) 0.0374(6) Uani 1 1 d . . .
H16A H 0.0525 0.4845 0.7373 0.045 Uiso 1 1 calc R A .
C17 C -0.1412(3) 0.5751(3) 0.9683(2) 0.0569(9) Uani 1 1 d . . .
H17A H -0.1816 0.5917 1.0154 0.085 Uiso 1 1 calc R A .
H17B H -0.1765 0.5975 0.9202 0.085 Uiso 1 1 calc R . .
H17C H -0.0760 0.6090 0.9718 0.085 Uiso 1 1 calc R . .
C1S C 0.7500 0.7500 0.7150(13) 0.099(7) Uani 0.50 4 d SP . .
Cl1S Cl 0.8331(3) 0.6795(3) 0.7701(2) 0.0650(10) 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 89.998(1) . 3
N2 Ru2 N2 179.41(11) . 2
N2 Ru2 N2 90.000(1) 3 2
N2 Ru2 N2 89.998(1) . 4
N2 Ru2 N2 179.41(11) 3 4
N2 Ru2 N2 89.998(1) 2 4
N2 Ru2 Ru1 89.71(5) . .
N2 Ru2 Ru1 89.71(5) 3 .
N2 Ru2 Ru1 89.71(5) 2 .
N2 Ru2 Ru1 89.71(5) 4 .
N2 Ru2 Cl1A 90.29(5) . .
N2 Ru2 Cl1A 90.29(5) 3 .
N2 Ru2 Cl1A 90.29(5) 2 .
N2 Ru2 Cl1A 90.29(5) 4 .
Ru1 Ru2 Cl1A 180.000(4) . .
N1 Ru1 N1 89.921(5) . 3
N1 Ru1 N1 175.79(11) . 2
N1 Ru1 N1 89.924(4) 3 2
N1 Ru1 N1 89.923(4) . 4
N1 Ru1 N1 175.78(11) 3 4
N1 Ru1 N1 89.922(4) 2 4
N1 Ru1 Ru2 87.89(5) . .
N1 Ru1 Ru2 87.89(5) 3 .
N1 Ru1 Ru2 87.89(5) 2 .
N1 Ru1 Ru2 87.89(5) 4 .
N1 Ru1 Cl1 92.11(5) . .
N1 Ru1 Cl1 92.11(5) 3 .
N1 Ru1 Cl1 92.11(5) 2 .
N1 Ru1 Cl1 92.11(5) 4 .
Ru2 Ru1 Cl1 180.0 . .
C10 N2 C21 117.0(2) . .
C10 N2 Ru2 118.54(16) . .
C21 N2 Ru2 123.71(16) . .
C10 N1 C11 113.3(2) . .
C10 N1 Ru1 119.81(17) . .
C11 N1 Ru1 126.19(16) . .
C24 O20 C27 117.0(3) . .
N1 C10 N2 123.1(2) . .
C26 C21 C22 117.6(2) . .
C26 C21 N2 120.6(2) . .
C22 C21 N2 121.8(2) . .
C23 C22 C21 121.0(3) . .
C22 C23 C24 121.0(3) . .
O20 C24 C25 125.3(3) . .
O20 C24 C23 115.6(3) . .
C25 C24 C23 119.0(3) . .
C24 C25 C26 119.9(3) . .
C21 C26 C25 121.5(3) . .
C14 O10 C17 117.5(3) . .
C16 C11 C12 118.9(2) . .
C16 C11 N1 119.3(2) . .
C12 C11 N1 121.8(3) . .
C13 C12 C11 120.4(3) . .
C12 C13 C14 120.4(3) . .
O10 C14 C15 124.2(3) . .
O10 C14 C13 116.0(3) . .
C15 C14 C13 119.8(3) . .
C14 C15 C16 119.4(3) . .
C11 C16 C15 121.0(3) . .
Cl1S C1S Cl1S 73.2(6) . 4_565
Cl1S C1S Cl1S 73.2(6) . 3_655
Cl1S C1S Cl1S 114.9(13) 4_565 3_655
Cl1S C1S Cl1S 114.9(13) . 2_665
Cl1S C1S Cl1S 73.2(6) 4_565 2_665
Cl1S C1S Cl1S 73.2(6) 3_655 2_665
C1S Cl1S Cl1S 53.4(3) . 4_565
C1S Cl1S Cl1S 53.4(3) . 3_655
Cl1S Cl1S Cl1S 90.000(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 2.050(2) .
Ru2 N2 2.050(2) 3
Ru2 N2 2.050(2) 2
Ru2 N2 2.050(2) 4
Ru2 Ru1 2.4019(5) .
Ru2 Cl1A 2.46(3) .
Ru1 N1 2.073(2) .
Ru1 N1 2.073(2) 3
Ru1 N1 2.073(2) 2
Ru1 N1 2.073(2) 4
Ru1 Cl1 2.4344(12) .
N2 C10 1.332(3) .
N2 C21 1.431(3) .
N1 C10 1.318(3) .
N1 C11 1.442(3) .
O20 C24 1.366(3) .
O20 C27 1.425(4) .
C21 C26 1.386(4) .
C21 C22 1.404(4) .
C22 C23 1.373(4) .
C23 C24 1.389(4) .
C24 C25 1.383(4) .
C25 C26 1.397(4) .
O10 C14 1.375(3) .
O10 C17 1.414(4) .
C11 C16 1.381(4) .
C11 C12 1.394(4) .
C12 C13 1.379(4) .
C13 C14 1.388(4) .
C14 C15 1.382(4) .
C15 C16 1.397(4) .
C1S Cl1S 1.702(12) .
C1S Cl1S 1.702(12) 4_565
C1S Cl1S 1.702(12) 3_655
C1S Cl1S 1.702(12) 2_665
Cl1S Cl1S 2.029(6) 4_565
Cl1S Cl1S 2.029(6) 3_655
