#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:36:34 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179022 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/20/4122086.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_4122086
loop_
_publ_author_name
'Chiarella, Gina M.'
'Cotton, F. Albert'
'Murillo, Carlos A.'
'Ventura, Karen'
'Villagrán, Dino'
'Wang, Xiaoping'
_publ_section_title
;
 Manipulating magnetism: ru2(5+) paddlewheels devoid of axial
 interactions.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9580
_journal_page_last               9589
_journal_paper_doi               10.1021/ja5020647
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C60 H60 N8 O8 Ru2, B F4 '
_chemical_formula_sum            'C60 H60 B F4 N8 O8 Ru2'
_chemical_formula_weight         1310.11
_chemical_name_common            Ru2(m-DAniF)4BF4
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           126
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2bc'
_symmetry_space_group_name_H-M   'P 4/n n c :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                   13.7952(18)
_cell_length_b                   13.7952(18)
_cell_length_c                   15.095(3)
_cell_measurement_reflns_used    7138
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.69
_cell_volume                     2872.7(8)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SMART (Bruker, 2001)'
_computing_molecular_graphics    'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16571
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.9423
_exptl_absorpt_correction_T_min  0.8892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1338
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.052
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.397
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1662
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.393
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0719
_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)+(0.0238P)²+20.2572P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1697
_reflns_number_gt                1442
_reflns_number_total             1662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5020647_si_001.cif
_cod_data_source_block           Ru2(mdanif)4BF4-213K
_cod_depositor_comments
'Adding full bibliography for 4122084--4122090.cif.'
_cod_original_sg_symbol_H-M      'P 4/nnc'
_cod_database_code               4122086
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+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'
'-y, -x, 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
Ru1 Ru 0.2500 0.2500 0.67090(6) 0.0286(3) Uani 1 4 d S
C1 C 0.3866(4) 0.1134(4) 0.7500 0.0362(18) Uani 1 2 d S
H1A H 0.4343 0.0657 0.7500 0.043 Uiso 1 2 calc SR
N1 N 0.3649(3) 0.1576(3) 0.6752(3) 0.0331(11) Uani 1 1 d .
C12 C 0.3965(4) 0.1203(4) 0.5192(4) 0.0342(13) Uani 1 1 d .
H12A H 0.3308 0.1086 0.5108 0.041 Uiso 1 1 calc R
C16 C 0.5285(5) 0.1676(5) 0.6145(5) 0.0409(15) Uani 1 1 d .
H16A H 0.5513 0.1865 0.6699 0.049 Uiso 1 1 calc R
C14 C 0.5589(5) 0.1311(5) 0.4618(5) 0.0418(16) Uani 1 1 d .
H14A H 0.6023 0.1247 0.4150 0.050 Uiso 1 1 calc R
C15 C 0.5916(5) 0.1597(5) 0.5432(5) 0.0471(17) Uani 1 1 d .
H15A H 0.6569 0.1740 0.5509 0.057 Uiso 1 1 calc R
C11 C 0.4308(4) 0.1468(4) 0.6021(4) 0.0315(12) Uani 1 1 d .
C13 C 0.4604(5) 0.1115(5) 0.4487(4) 0.0376(14) Uani 1 1 d .
O1 O 0.4362(4) 0.0847(4) 0.3651(3) 0.0497(12) Uani 1 1 d .
C17 C 0.3370(6) 0.0602(7) 0.3490(5) 0.056(2) Uani 1 1 d .
H17A H 0.3292 0.0412 0.2883 0.084 Uiso 1 1 calc R
H17B H 0.2967 0.1154 0.3610 0.084 Uiso 1 1 calc R
H17C H 0.3184 0.0075 0.3870 0.084 Uiso 1 1 calc R
B1 B 0.7500 0.2500 0.7500 0.055(8) Uani 0.50 4 d SPDU
F1 F 0.8024(16) 0.211(4) 0.690(3) 0.144(14) Uani 0.25 1 d PDU
F2 F 0.8042(16) 0.184(3) 0.715(3) 0.144(14) Uani 0.25 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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
N1 Ru1 N1 176.4(3) 4 3
N1 Ru1 N1 89.942(10) 4 2
N1 Ru1 N1 89.942(10) 3 2
N1 Ru1 N1 89.942(10) 4 .
N1 Ru1 N1 89.942(10) 3 .
N1 Ru1 N1 176.4(3) 2 .
N1 Ru1 Ru1 88.18(15) 4 5_556
N1 Ru1 Ru1 88.18(15) 3 5_556
N1 Ru1 Ru1 88.18(15) 2 5_556
N1 Ru1 Ru1 88.18(15) . 5_556
N1 C1 N1 121.6(7) . 8_556
N1 C1 H1A 119.2 . .
N1 C1 H1A 119.2 8_556 .
C1 N1 C11 117.8(5) . .
C1 N1 Ru1 119.6(4) . .
C11 N1 Ru1 122.2(4) . .
C11 C12 C13 119.9(6) . .
C11 C12 H12A 120.0 . .
C13 C12 H12A 120.0 . .
C15 C16 C11 119.1(7) . .
C15 C16 H16A 120.4 . .
C11 C16 H16A 120.4 . .
C15 C14 C13 120.2(6) . .
C15 C14 H14A 119.9 . .
C13 C14 H14A 119.9 . .
C14 C15 C16 120.9(6) . .
C14 C15 H15A 119.6 . .
C16 C15 H15A 119.6 . .
C12 C11 C16 120.4(6) . .
C12 C11 N1 120.3(5) . .
C16 C11 N1 119.2(6) . .
O1 C13 C12 125.5(6) . .
O1 C13 C14 115.0(6) . .
C12 C13 C14 119.4(6) . .
C13 O1 C17 117.2(5) . .
O1 C17 H17A 109.5 . .
O1 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
O1 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
F1 B1 F1 130(6) 6_556 2_655
F1 B1 F1 111.0(15) 6_556 .
F1 B1 F1 90(4) 2_655 .
F1 B1 F1 90(4) 6_556 5_656
F1 B1 F1 111.0(15) 2_655 5_656
F1 B1 F1 130(6) . 5_656
F1 B1 F2 108.6(4) 2_655 6_556
F1 B1 F2 105(2) . 6_556
F1 B1 F2 109.7(5) 5_656 6_556
F1 B1 F2 109.7(5) 6_556 5_656
F1 B1 F2 105(2) 2_655 5_656
F1 B1 F2 108.6(4) . 5_656
F2 B1 F2 131(5) 6_556 5_656
F1 B1 F2 105(2) 6_556 .
F1 B1 F2 109.7(5) 2_655 .
F1 B1 F2 108.6(4) 5_656 .
F2 B1 F2 109.2(15) 6_556 .
F2 B1 F2 91(4) 5_656 .
F1 B1 F2 108.6(4) 6_556 2_655
F1 B1 F2 109.7(5) . 2_655
F1 B1 F2 105(2) 5_656 2_655
F2 B1 F2 91(4) 6_556 2_655
F2 B1 F2 109.2(15) 5_656 2_655
F2 B1 F2 131(5) . 2_655
F2 F1 B1 80(4) . .
F1 F2 B1 77(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N1 2.035(5) 4
Ru1 N1 2.035(5) 3
Ru1 N1 2.035(5) 2
Ru1 N1 2.035(5) .
Ru1 Ru1 2.3879(19) 5_556
C1 N1 1.318(6) .
C1 N1 1.318(6) 8_556
C1 H1A 0.9300 .
N1 C11 1.438(7) .
C12 C11 1.387(8) .
C12 C13 1.387(8) .
C12 H12A 0.9300 .
C16 C15 1.389(9) .
C16 C11 1.390(8) .
C16 H16A 0.9300 .
C14 C15 1.366(10) .
C14 C13 1.400(9) .
C14 H14A 0.9300 .
C15 H15A 0.9300 .
C13 O1 1.357(8) .
O1 C17 1.431(9) .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
B1 F1 1.28(2) 6_556
B1 F1 1.28(2) 2_655
B1 F1 1.28(2) .
B1 F1 1.28(2) 5_656
B1 F2 1.29(2) 6_556
B1 F2 1.29(2) 5_656
B1 F2 1.29(2) .
B1 F2 1.29(2) 2_655
F1 F2 0.52(13) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
N1 C1 N1 C11 165.6(5) 8_556
N1 C1 N1 Ru1 -7.41(16) 8_556
N1 Ru1 N1 C1 -73.6(4) 4
N1 Ru1 N1 C1 102.7(3) 3
Ru1 Ru1 N1 C1 14.6(3) 5_556
N1 Ru1 N1 C11 113.7(4) 4
N1 Ru1 N1 C11 -69.9(5) 3
Ru1 Ru1 N1 C11 -158.1(4) 5_556
C13 C14 C15 C16 1.5(11) .
C11 C16 C15 C14 -0.6(10) .
C13 C12 C11 C16 2.1(9) .
C13 C12 C11 N1 179.0(5) .
C15 C16 C11 C12 -1.2(9) .
C15 C16 C11 N1 -178.2(6) .
C1 N1 C11 C12 130.3(5) .
Ru1 N1 C11 C12 -56.9(7) .
C1 N1 C11 C16 -52.7(7) .
Ru1 N1 C11 C16 120.1(5) .
C11 C12 C13 O1 178.9(6) .
C11 C12 C13 C14 -1.1(9) .
C15 C14 C13 O1 179.3(6) .
C15 C14 C13 C12 -0.7(10) .
C12 C13 O1 C17 -2.4(10) .
C14 C13 O1 C17 177.6(6) .
F1 B1 F1 F2 80(4) 6_556
F1 B1 F1 F2 -147(5) 2_655
F1 B1 F1 F2 -29(3) 5_656
F2 B1 F1 F2 103(5) 6_556
F2 B1 F1 F2 -41(5) 5_656
F2 B1 F1 F2 -160(3) 2_655
F1 B1 F2 F1 -108(5) 6_556
F1 B1 F2 F1 35(5) 2_655
F1 B1 F2 F1 157(4) 5_656
F2 B1 F2 F1 -84(4) 6_556
F2 B1 F2 F1 141(4) 5_656
F2 B1 F2 F1 25(3) 2_655
