#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:41:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178911 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/40/4114095.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_4114095
loop_
_publ_author_name
'Panagiotis Angaridis'
'John F. Berry'
'F. Albert Cotton'
'Carlos A. Murillo'
'Xiaoping Wang'
_publ_contact_author_address
;  Laboratory for Molecular Structure and Bonding
   Dept. of Chemistry
   Texas A&M University, P.O. 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
;
 Molecular Squares with Paramagnetic Diruthenium Corners: Synthetic and
 Crystallographic Challenges
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10327
_journal_page_last               10334
_journal_paper_doi               10.1021/ja036095x
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety
'(C128H128N16O36Cl4Ru8) (C2H3N) (C6H14)2 (H2O)12'
_chemical_formula_sum            'C142 H183 Cl4 N17 O48 Ru8'
_chemical_formula_weight         3846.41
_chemical_name_common
'{cis-(DAniF)2Ru2Cl(oxalate)(H2O)}4 (CH3CN) 2(C6H14) 12H2O'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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                   19.9157(14)
_cell_length_b                   19.9157(14)
_cell_length_c                   25.760(4)
_cell_measurement_reflns_used    8338
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      2.42
_cell_volume                     10217.3(19)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        'SAINT and SADABS'
_computing_molecular_graphics    'SHELXTL V6.10 (Bruker, 2000)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       'w/ 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  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19332
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  0.8566
_exptl_absorpt_correction_T_min  0.7424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V1.03'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             3916
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3426
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0820
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0820P)²+267.8000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1973
_refine_ls_wR_factor_ref         0.2443
_reflns_number_gt                2353
_reflns_number_total             3426
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036095xsi20030512_050600_3.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        10217.1(18)
_cod_database_code               4114095
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
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
Ru1 Ru 0.03654(5) 0.76049(5) 0.45473(3) 0.0369(4) Uani 1 1 d . . .
Cl1 Cl 0.0352(4) 0.7696(3) 0.3602(2) 0.0350(15) Uani 0.50 1 d P . .
O3 O 0.0243(12) 0.7972(10) 0.6435(7) 0.0350(15) Uani 0.50 1 d P . .
O1 O 0.0968(4) 0.8462(4) 0.4563(3) 0.035(2) Uani 1 1 d . . .
O2 O -0.0471(4) 0.8238(4) 0.4563(3) 0.0312(19) Uani 1 1 d . . .
C1 C 0.1149(10) 0.8683(10) 0.5000 0.050(5) Uani 1 2 d S . .
C2 C -0.0704(9) 0.8396(8) 0.5000 0.038(4) Uani 1 2 d S . .
C10 C 0.1488(10) 0.6851(9) 0.5000 0.042(5) Uani 1 2 d S . .
N1 N 0.1214(6) 0.7034(5) 0.4555(4) 0.042(3) Uani 1 1 d . . .
C11 C 0.1556(9) 0.6852(9) 0.4086(6) 0.068(5) Uani 1 1 d . . .
C12 C 0.1617(13) 0.6208(11) 0.3918(8) 0.136(10) Uani 1 1 d D . .
H12A H 0.1427 0.5863 0.4119 0.163 Uiso 1 1 calc R . .
C13 C 0.1946(16) 0.6040(12) 0.3466(11) 0.156(13) Uani 1 1 d D . .
H13A H 0.1930 0.5601 0.3335 0.188 Uiso 1 1 calc R . .
C14 C 0.2291(10) 0.6526(12) 0.3219(7) 0.112(8) Uani 1 1 d D A .
C15 C 0.2232(16) 0.7182(13) 0.3360(10) 0.167(14) Uani 1 1 d D . .
H15A H 0.2438 0.7520 0.3162 0.200 Uiso 1 1 calc R . .
C16 C 0.1868(13) 0.7347(11) 0.3798(9) 0.132(10) Uani 1 1 d D . .
H16A H 0.1832 0.7798 0.3900 0.158 Uiso 1 1 calc R . .
O10 O 0.2643(10) 0.6405(11) 0.2747(6) 0.170(9) Uani 1 1 d D . .
C17 C 0.288(8) 0.573(3) 0.267(3) 0.21(4) Uani 0.49(9) 1 d PD A 1
H17A H 0.3122 0.5704 0.2343 0.313 Uiso 0.49(9) 1 calc PR A 1
H17B H 0.2498 0.5426 0.2657 0.313 Uiso 0.49(9) 1 calc PR A 1
H17C H 0.3173 0.5602 0.2951 0.313 Uiso 0.49(9) 1 calc PR A 1
C17B C 0.242(6) 0.581(4) 0.247(3) 0.21(4) Uani 0.51(9) 1 d PD A 2
H17D H 0.2684 0.5759 0.2160 0.313 Uiso 0.51(9) 1 calc PR A 2
H17E H 0.1950 0.5862 0.2384 0.313 Uiso 0.51(9) 1 calc PR A 2
H17F H 0.2479 0.5423 0.2694 0.313 Uiso 0.51(9) 1 calc PR A 2
N2 N -0.0273(5) 0.6805(4) 0.4551(3) 0.032(2) Uani 1 1 d . B .
C20 C -0.0476(9) 0.6548(8) 0.5000 0.036(4) Uani 1 2 d S . .
C21 C -0.0532(8) 0.6507(7) 0.4096(5) 0.054(4) Uani 1 1 d . . .
C22A C -0.0431(13) 0.5836(11) 0.4002(8) 0.067(6) Uani 0.619(11) 1 d PD B 1
H22A H -0.0148 0.5591 0.4223 0.080 Uiso 0.619(11) 1 calc PR B 1
C23A C -0.0735(15) 0.5513(11) 0.3593(10) 0.088(8) Uani 0.619(11) 1 d PD B 1
H23A H -0.0694 0.5046 0.3553 0.105 Uiso 0.619(11) 1 calc PR B 1
C24A C -0.1092(10) 0.5882(9) 0.3251(7) 0.090(6) Uani 0.619(11) 1 d PD B 1
C25A C -0.1240(16) 0.6538(12) 0.3349(11) 0.089(9) Uani 0.619(11) 1 d PD B 1
H25A H -0.1552 0.6769 0.3142 0.106 Uiso 0.619(11) 1 calc PR B 1
C26A C -0.0925(14) 0.6859(10) 0.3757(9) 0.068(7) Uani 0.619(11) 1 d PD B 1
H26A H -0.0981 0.7324 0.3802 0.082 Uiso 0.619(11) 1 calc PR B 1
O20A O -0.1456(13) 0.558(2) 0.2840(12) 0.131(6) Uani 0.619(11) 1 d PD B 1
C27A C -0.107(2) 0.532(3) 0.2410(13) 0.21(3) Uani 0.619(11) 1 d PD B 1
H27A H -0.1020 0.4842 0.2442 0.322 Uiso 0.619(11) 1 calc PR B 1
H27B H -0.0627 0.5532 0.2411 0.322 Uiso 0.619(11) 1 calc PR B 1
H27C H -0.1295 0.5430 0.2087 0.322 Uiso 0.619(11) 1 calc PR B 1
C22B C -0.0146(14) 0.6194(19) 0.3731(13) 0.067(6) Uani 0.381(11) 1 d PD B 2
H22B H 0.0323 0.6200 0.3768 0.080 Uiso 0.381(11) 1 calc PR B 2
C23B C -0.0421(13) 0.587(2) 0.3312(14) 0.088(8) Uani 0.381(11) 1 d PD B 2
H23B H -0.0146 0.5643 0.3073 0.105 Uiso 0.381(11) 1 calc PR B 2
C24B C -0.1092(10) 0.5882(9) 0.3251(7) 0.090(6) Uani 0.381(11) 1 d PD B 2
C25B C -0.1502(14) 0.618(2) 0.3603(14) 0.089(9) Uani 0.381(11) 1 d PD B 2
H25B H -0.1970 0.6175 0.3561 0.106 Uiso 0.381(11) 1 calc PR B 2
C26B C -0.1215(18) 0.6506(19) 0.4022(11) 0.068(7) Uani 0.381(11) 1 d PD B 2
H26B H -0.1492 0.6729 0.4263 0.082 Uiso 0.381(11) 1 calc PR B 2
O20B O -0.141(2) 0.555(3) 0.2826(19) 0.131(6) Uani 0.381(11) 1 d PD B 2
C27B C -0.190(3) 0.593(4) 0.254(2) 0.21(3) Uani 0.381(11) 1 d PD B 2
H27D H -0.2128 0.5634 0.2298 0.322 Uiso 0.381(11) 1 calc PR B 2
H27E H -0.1686 0.6291 0.2355 0.322 Uiso 0.381(11) 1 calc PR B 2
H27F H -0.2230 0.6113 0.2783 0.322 Uiso 0.381(11) 1 calc PR B 2
N1S N 0.0000 1.0000 0.4773(15) 0.040(11) Uani 0.50 4 d SPD . .
C1S C 0.0000 1.0000 0.4325(14) 0.08(2) Uani 0.50 4 d SPD . .
C2S C 0.0000 1.0000 0.3733(14) 0.026(10) Uani 0.50 4 d SPD . .
H2S1 H 0.0360 1.0286 0.3607 0.039 Uiso 0.13 1 calc PR . .
H2S2 H -0.0427 1.0169 0.3607 0.039 Uiso 0.13 1 calc PR . .
H2S3 H 0.0068 0.9546 0.3607 0.039 Uiso 0.13 1 calc PR . .
O1S O 0.1019(19) 1.130(3) 0.3532(16) 0.113(9) Uani 0.49(3) 1 d P C 1
O1SA O 0.0698(18) 1.106(3) 0.3528(16) 0.113(9) Uani 0.51(3) 1 d P C 2
O2S O 0.5000 0.5000 0.2689(7) 0.069(6) Uani 1 4 d S . .
O3S O -0.204(3) 0.724(3) 0.5000 0.18(3) Uani 0.50 2 d SP . .
C3S C 0.170(4) 0.499(5) 0.5000 0.36(5) Uiso 1 2 d SD . .
H3S1 H 0.1940 0.5224 0.5272 0.435 Uiso 0.50 1 calc PR . .
H3S2 H 0.1899 0.5092 0.4666 0.435 Uiso 0.50 1 calc PR . .
H3S3 H 0.1719 0.4510 0.5062 0.435 Uiso 0.50 1 calc PR . .
C4S C 0.096(4) 0.522(4) 0.5000 0.26(3) Uiso 1 2 d SD . .
C5S C 0.030(3) 0.511(5) 0.529(2) 0.23(4) Uiso 0.50 1 d PD . .
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
N1 Ru1 N2 94.7(4) . . y
N1 Ru1 O1 88.8(4) . . y
N2 Ru1 O1 176.2(4) . . y
N1 Ru1 O2 176.4(4) . . y
N2 Ru1 O2 88.5(4) . . y
O1 Ru1 O2 88.0(3) . . y
N1 Ru1 Ru1 89.5(3) . 10_556 y
N2 Ru1 Ru1 89.7(2) . 10_556 y
O1 Ru1 Ru1 88.9(2) . 10_556 y
O2 Ru1 Ru1 88.86(19) . 10_556 y
N1 Ru1 Cl1 93.4(3) . . y
N2 Ru1 Cl1 93.2(3) . . y
O1 Ru1 Cl1 88.0(3) . . y
O2 Ru1 Cl1 88.1(2) . . y
Ru1 Ru1 Cl1 175.70(13) 10_556 . y
O3 Cl1 Ru1 103(2) 10_556 . ?
Cl1 O3 Ru1 64.0(18) 10_556 10_556 ?
C1 O1 Ru1 117.8(10) . . ?
C2 O2 Ru1 117.6(9) . . ?
O1 C1 O1 126(2) 10_556 . ?
O1 C1 C2 116.8(10) 10_556 3_665 ?
O1 C1 C2 116.8(10) . 3_665 ?
O2 C2 O2 127.0(16) 10_556 . ?
O2 C2 C1 116.5(8) 10_556 11_466 ?
O2 C2 C1 116.5(8) . 11_466 ?
N1 C10 N1 120.4(16) 10_556 . ?
C10 N1 C11 117.7(13) . . ?
C10 N1 Ru1 120.3(9) . . ?
C11 N1 Ru1 121.9(9) . . ?
C12 C11 C16 117.5(16) . . ?
C12 C11 N1 123.4(16) . . ?
C16 C11 N1 119.1(15) . . ?
C11 C12 C13 122.8(19) . . ?
C14 C13 C12 117.9(18) . . ?
C13 C14 C15 121.3(16) . . ?
C13 C14 O10 122.2(18) . . ?
C15 C14 O10 115.7(19) . . ?
C14 C15 C16 119.4(19) . . ?
C15 C16 C11 120.4(19) . . ?
C14 O10 C17 116(2) . . ?
C14 O10 C17B 114(2) . . ?
C17 O10 C17B 43(5) . . ?
C20 N2 C21 116.8(11) . . ?
C20 N2 Ru1 119.7(8) . . ?
C21 N2 Ru1 123.5(8) . . ?
N2 C20 N2 121.2(15) 10_556 . ?
C22B C21 C26A 97(2) . . ?
C22B C21 C22A 49.6(19) . . ?
C26A C21 C22A 118.0(15) . . ?
C22B C21 C26B 117.5(16) . . ?
C26A C21 C26B 49.1(19) . . ?
C22A C21 C26B 97(2) . . ?
C22B C21 N2 124.0(15) . . ?
C26A C21 N2 121.6(14) . . ?
C22A C21 N2 120.2(14) . . ?
C26B C21 N2 118.4(15) . . ?
C21 C22A C23A 121.8(19) . . ?
C24A C23A C22A 118.5(18) . . ?
C23A C24A C25A 120.9(16) . . ?
C23A C24A O20A 121(2) . . ?
C25A C24A O20A 116(2) . . ?
C24A C25A C26A 119.2(19) . . ?
C21 C26A C25A 120.6(18) . . ?
C24A O20A C27A 117(2) . . ?
C21 C22B C23B 122(2) . . ?
C21 C26B C25B 121(2) . . ?
C1S N1S N1S 180.00(2) . 9_576 ?
N1S C1S C2S 180.00(2) . . ?
C5S C4S C3S 141(6) . . ?
C5S C4S C3S 141(6) 10_556 . ?
C4S C5S C5S 101(6) . 9_566 ?
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
Ru1 Ru1 2.3322(18) 10_556 y
Ru1 N1 2.036(11) . y
Ru1 N2 2.039(9) . y
Ru1 O1 2.087(8) . y
Ru1 O2 2.089(7) . y
Ru1 Cl1 2.443(6) . y
Cl1 O3 0.600(16) 10_556 ?
O3 Cl1 0.600(16) 10_556 ?
O3 Ru1 2.645(17) 10_556 y
O1 C1 1.263(12) . ?
O2 C2 1.257(10) . ?
C1 O1 1.263(12) 10_556 ?
C1 C2 1.52(3) 3_665 ?
C2 O2 1.257(10) 10_556 ?
C2 C1 1.52(3) 11_466 ?
C10 N1 1.322(13) 10_556 ?
C10 N1 1.322(13) . ?
N1 C11 1.433(18) . ?
C11 C12 1.36(2) . ?
C11 C16 1.38(3) . ?
C12 C13 1.38(2) . ?
C13 C14 1.35(2) . ?
C14 C15 1.36(2) . ?
C14 O10 1.424(16) . ?
C15 C16 1.38(2) . ?
O10 C17 1.440(19) . ?
O10 C17B 1.44(3) . ?
N2 C20 1.327(12) . ?
N2 C21 1.411(16) . ?
C20 N2 1.327(12) 10_556 ?
C21 C22B 1.36(4) . ?
C21 C26A 1.37(2) . ?
C21 C22A 1.37(2) . ?
C21 C26B 1.37(4) . ?
C22A C23A 1.37(2) . ?
C23A C24A 1.35(2) . ?
C24A C25A 1.36(2) . ?
C24A O20A 1.420(17) . ?
C25A C26A 1.38(2) . ?
O20A C27A 1.441(17) . ?
C22B C23B 1.37(2) . ?
C25B C26B 1.38(2) . ?
O20B C27B 1.439(19) . ?
N1S C1S 1.154(19) . ?
N1S N1S 1.17(8) 9_576 ?
C1S C2S 1.53(2) . ?
C3S C4S 1.53(2) . ?
C4S C5S 1.53(2) . ?
C4S C5S 1.53(2) 10_556 ?
C5S C5S 1.49(13) 10_556 ?
