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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/4/31/22/4312262.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_4312262
loop_
_publ_author_name
'Panagiotis Angaridis'
'F. Albert Cotton'
'Carlos A. Murillo'
'Dino Villagrán'
'Xiaoping Wang'
_publ_contact_author_address
;  Laboratory for Molecular Structure and Bonding
   Dept. of Chemistry
   Texas A&M University, PO Box  30012
   College Station, TX 77842-3012, USA
;
_publ_contact_author_email       cotton@tamu.edu
_publ_contact_author_fax         '(979) 845 9351'
_publ_contact_author_name        'F. A. Cotton'
_publ_contact_author_phone       '(979) 845 4432'
_publ_section_title
;
 Paramagnetic Precursors for Supramolecular Assemblies: Selective
 Syntheses, Crystal Structures, and Electrochemical and Magnetic
 Properties of Ru2(O2CMe)4-n(formamidinate)nCl Complexes,n= 1-4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8290
_journal_page_last               8300
_journal_paper_doi               10.1021/ic049108w
_journal_volume                  43
_journal_year                    2004
_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)
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                   13.1343(6)
_cell_length_b                   13.1343(6)
_cell_length_c                   16.5787(16)
_cell_measurement_reflns_used    5675
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.51
_cell_volume                     2860.0(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      213(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17577
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.8257
_exptl_absorpt_correction_T_min  0.7805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallepiped
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0292P)²+2.2904P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                2938
_reflns_number_total             3290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049108wsi20040707_033913_6.cif
_cod_data_source_block           cmpd5
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'C60.50 H61 Cl2 N8 O8 Ru2'
_cod_database_code               4312262
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 0.573327(15) 0.01830(7) Uani 1 4 d S . .
Ru1 Ru 0.2500 0.2500 0.717850(14) 0.01877(8) Uani 1 4 d S . .
Cl Cl 0.2500 0.2500 0.86491(5) 0.02532(17) Uani 1 4 d S . .
N2 N 0.09643(10) 0.27712(11) 0.57392(8) 0.0213(3) Uani 1 1 d . . .
N1 N 0.09944(11) 0.29712(11) 0.71304(8) 0.0223(3) Uani 1 1 d . . .
O20 O -0.13172(13) 0.33465(12) 0.29184(9) 0.0433(4) Uani 1 1 d . . .
C10 C 0.05205(13) 0.30059(13) 0.64330(10) 0.0236(3) Uani 1 1 d . . .
H10A H -0.0166 0.3207 0.6426 0.028 Uiso 1 1 calc R . .
C21 C 0.03628(13) 0.28888(13) 0.50226(10) 0.0233(3) Uani 1 1 d . . .
C22 C -0.03271(15) 0.36919(15) 0.49328(12) 0.0330(4) Uani 1 1 d . . .
H22A H -0.0422 0.4155 0.5359 0.040 Uiso 1 1 calc R . .
C23 C -0.08696(16) 0.38133(16) 0.42273(12) 0.0378(5) Uani 1 1 d . . .
H23A H -0.1328 0.4359 0.4178 0.045 Uiso 1 1 calc R . .
C24 C -0.07466(15) 0.31405(15) 0.35907(11) 0.0318(4) Uani 1 1 d . . .
C25 C -0.00671(16) 0.23433(15) 0.36673(11) 0.0329(4) Uani 1 1 d . . .
H25A H 0.0023 0.1882 0.3240 0.039 Uiso 1 1 calc R . .
C26 C 0.04833(14) 0.22251(14) 0.43778(11) 0.0293(4) Uani 1 1 d . . .
H26A H 0.0948 0.1683 0.4422 0.035 Uiso 1 1 calc R . .
O10 O -0.12668(13) 0.46962(13) 0.96467(9) 0.0478(4) Uani 1 1 d . . .
C27 C -0.1188(2) 0.26858(19) 0.22466(13) 0.0484(6) Uani 1 1 d . . .
H27A H -0.1627 0.2905 0.1809 0.073 Uiso 1 1 calc R . .
H27B H -0.1364 0.1996 0.2402 0.073 Uiso 1 1 calc R . .
H27C H -0.0484 0.2706 0.2070 0.073 Uiso 1 1 calc R . .
C11 C 0.04197(13) 0.34129(14) 0.77854(10) 0.0254(4) Uani 1 1 d . . .
C12 C 0.00148(15) 0.28240(15) 0.84048(11) 0.0305(4) Uani 1 1 d . . .
H12A H 0.0126 0.2117 0.8412 0.037 Uiso 1 1 calc R . .
C13 C -0.05502(15) 0.32751(16) 0.90100(11) 0.0340(4) Uani 1 1 d . . .
H13A H -0.0830 0.2871 0.9422 0.041 Uiso 1 1 calc R . .
C14 C -0.07082(15) 0.43218(16) 0.90154(12) 0.0341(4) Uani 1 1 d . . .
C15 C -0.03064(16) 0.49149(16) 0.84036(12) 0.0359(4) Uani 1 1 d . . .
H15A H -0.0407 0.5624 0.8403 0.043 Uiso 1 1 calc R . .
C16 C 0.02492(15) 0.44512(15) 0.77870(11) 0.0319(4) Uani 1 1 d . . .
H16A H 0.0512 0.4852 0.7366 0.038 Uiso 1 1 calc R . .
C17 C -0.1412(2) 0.57683(19) 0.96790(14) 0.0502(6) Uani 1 1 d . . .
H17A H -0.1817 0.5939 1.0149 0.075 Uiso 1 1 calc R . .
H17B H -0.1764 0.5992 0.9196 0.075 Uiso 1 1 calc R . .
H17C H -0.0756 0.6104 0.9714 0.075 Uiso 1 1 calc R . .
C1SA C 0.7500 0.7500 0.7145(9) 0.085(4) Uiso 0.50 4 d SP . .
Cl1A Cl 0.8323(3) 0.6789(3) 0.7711(2) 0.0820(9) Uiso 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
_geom_angle_publ_flag
N2 Ru2 N2 90.001(1) 4 2 ?
N2 Ru2 N2 179.45(7) 4 3 ?
N2 Ru2 N2 90.0 2 3 ?
N2 Ru2 N2 90.0 4 . ?
N2 Ru2 N2 179.45(7) 2 . ?
N2 Ru2 N2 89.998(1) 3 . ?
N2 Ru2 Ru1 89.72(4) 4 . ?
N2 Ru2 Ru1 89.72(4) 2 . ?
N2 Ru2 Ru1 89.72(4) 3 . ?
N2 Ru2 Ru1 89.72(4) . . ?
N1 Ru1 N1 89.917(3) 4 2 ?
N1 Ru1 N1 89.916(3) 4 . ?
N1 Ru1 N1 175.59(7) 2 . ?
N1 Ru1 N1 175.59(7) 4 3 ?
N1 Ru1 N1 89.915(3) 2 3 ?
N1 Ru1 N1 89.913(3) . 3 ?
N1 Ru1 Ru2 87.79(4) 4 . ?
N1 Ru1 Ru2 87.79(4) 2 . ?
N1 Ru1 Ru2 87.79(4) . . ?
N1 Ru1 Ru2 87.79(4) 3 . ?
N1 Ru1 Cl 92.21(4) 4 . ?
N1 Ru1 Cl 92.21(4) 2 . ?
N1 Ru1 Cl 92.21(4) . . ?
N1 Ru1 Cl 92.21(4) 3 . ?
Ru2 Ru1 Cl 180.0 . . ?
C10 N2 C21 116.81(14) . . ?
C10 N2 Ru2 118.53(11) . . ?
C21 N2 Ru2 123.84(11) . . ?
C10 N1 C11 113.59(14) . . ?
C10 N1 Ru1 119.73(11) . . ?
C11 N1 Ru1 126.11(11) . . ?
C24 O20 C27 116.83(17) . . ?
N1 C10 N2 123.17(16) . . ?
C26 C21 C22 117.74(16) . . ?
C26 C21 N2 120.47(15) . . ?
C22 C21 N2 121.74(16) . . ?
C23 C22 C21 120.82(18) . . ?
C22 C23 C24 120.80(18) . . ?
O20 C24 C25 125.28(18) . . ?
O20 C24 C23 115.46(18) . . ?
C25 C24 C23 119.25(17) . . ?
C24 C25 C26 119.87(17) . . ?
C21 C26 C25 121.52(17) . . ?
C14 O10 C17 117.15(18) . . ?
C16 C11 C12 119.03(17) . . ?
C16 C11 N1 118.86(16) . . ?
C12 C11 N1 122.10(17) . . ?
C13 C12 C11 120.19(18) . . ?
C12 C13 C14 120.59(18) . . ?
O10 C14 C15 124.22(19) . . ?
O10 C14 C13 116.10(18) . . ?
C15 C14 C13 119.68(18) . . ?
C14 C15 C16 119.38(19) . . ?
C11 C16 C15 121.11(18) . . ?
Cl1A C1SA Cl1A 113.4(9) . 2_665 ?
Cl1A C1SA Cl1A 113.4(9) 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
_geom_bond_publ_flag
Ru2 N2 2.0482(14) 4 ?
Ru2 N2 2.0482(14) 2 ?
Ru2 N2 2.0482(14) 3 ?
Ru2 N2 2.0482(14) . ?
Ru2 Ru1 2.3960(4) . ?
Ru1 N1 2.0736(15) 4 ?
Ru1 N1 2.0736(15) 2 ?
Ru1 N1 2.0736(15) . ?
Ru1 N1 2.0736(15) 3 ?
Ru1 Cl 2.4380(8) . ?
N2 C10 1.326(2) . ?
N2 C21 1.435(2) . ?
N1 C10 1.314(2) . ?
N1 C11 1.444(2) . ?
O20 C24 1.370(2) . ?
O20 C27 1.422(3) . ?
C21 C26 1.389(2) . ?
C21 C22 1.399(3) . ?
C22 C23 1.379(3) . ?
C23 C24 1.386(3) . ?
C24 C25 1.382(3) . ?
C25 C26 1.391(3) . ?
O10 C14 1.369(2) . ?
O10 C17 1.422(3) . ?
C11 C16 1.382(3) . ?
C11 C12 1.391(3) . ?
C12 C13 1.382(3) . ?
C13 C14 1.390(3) . ?
C14 C15 1.383(3) . ?
C15 C16 1.396(3) . ?
C1SA Cl1A 1.709(9) 3_655 ?
C1SA Cl1A 1.709(9) . ?
