#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:36:34 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179022 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/20/4122084.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_4122084
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_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    6361
_cell_measurement_temperature    33(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.51
_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      33(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14111
_diffrn_reflns_theta_full        26.29
_diffrn_reflns_theta_max         26.29
_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         2.262
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1417
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      2.027
_refine_ls_R_factor_all          0.1359
_refine_ls_R_factor_gt           0.1222
_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)+(0.0250P)²+20.5628P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2291
_reflns_number_gt                1222
_reflns_number_total             1417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5020647_si_001.cif
_cod_data_source_block           Ru2(mdanif)4BF4-33K
_cod_depositor_comments
'Adding full bibliography for 4122084--4122090.cif.'
_cod_original_sg_symbol_H-M      P4/nnc
_cod_database_code               4122084
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 0.67087(13) 0.0400(6) Uani 1 4 d S
C1 C 0.3879(6) 0.1121(6) 0.7500 0.033(3) Uani 1 2 d SU
H1A H 0.4366 0.0634 0.7500 0.039 Uiso 1 2 calc SR
N1 N 0.3657(5) 0.1551(5) 0.6753(5) 0.0324(17) Uani 1 1 d U
C12 C 0.3972(6) 0.1197(6) 0.5192(6) 0.031(2) Uani 1 1 d U
H12A H 0.3298 0.1082 0.5114 0.037 Uiso 1 1 calc R
C16 C 0.5315(6) 0.1656(6) 0.6142(8) 0.040(3) Uani 1 1 d .
H16A H 0.5544 0.1844 0.6710 0.048 Uiso 1 1 calc R
C14 C 0.5620(6) 0.1308(6) 0.4612(8) 0.039(2) Uani 1 1 d U
H14A H 0.6064 0.1246 0.4134 0.047 Uiso 1 1 calc R
C15 C 0.5955(7) 0.1585(7) 0.5431(8) 0.038(2) Uani 1 1 d U
H15A H 0.6622 0.1728 0.5513 0.046 Uiso 1 1 calc R
C11 C 0.4322(7) 0.1447(6) 0.6011(7) 0.032(2) Uani 1 1 d U
C13 C 0.4611(6) 0.1110(6) 0.4464(8) 0.039(3) Uani 1 1 d U
O1 O 0.4365(5) 0.0853(5) 0.3641(5) 0.0414(17) Uani 1 1 d U
C17 C 0.3364(6) 0.0624(8) 0.3489(9) 0.052(3) Uani 1 1 d .
H17A H 0.3276 0.0428 0.2870 0.078 Uiso 1 1 calc R
H17B H 0.2965 0.1196 0.3612 0.078 Uiso 1 1 calc R
H17C H 0.3168 0.0092 0.3879 0.078 Uiso 1 1 calc R
B1 B 0.7500 0.2500 0.7500 0.069(15) Uani 0.50 4 d SPDU
F1 F 0.7979(14) 0.2232(12) 0.6776(11) 0.059(5) Uani 0.25 1 d PDU
F2 F 0.8180(14) 0.1715(11) 0.7260(11) 0.059(5) Uani 0.25 1 d PDU
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 176.3(5) 3 4
N1 Ru1 N1 89.940(17) 3 .
N1 Ru1 N1 89.940(16) 4 .
N1 Ru1 N1 89.940(16) 3 2
N1 Ru1 N1 89.940(17) 4 2
N1 Ru1 N1 176.3(5) . 2
N1 Ru1 Ru1 88.2(2) 3 5_556
N1 Ru1 Ru1 88.2(2) 4 5_556
N1 Ru1 Ru1 88.2(2) . 5_556
N1 Ru1 Ru1 88.2(2) 2 5_556
N1 C1 N1 122.0(11) . 8_556
N1 C1 H1A 119.0 . .
N1 C1 H1A 119.0 8_556 .
C1 N1 C11 118.1(8) . .
C1 N1 Ru1 119.7(7) . .
C11 N1 Ru1 121.7(6) . .
C11 C12 C13 120.1(9) . .
C11 C12 H12A 119.9 . .
C13 C12 H12A 119.9 . .
C15 C16 C11 119.4(11) . .
C15 C16 H16A 120.3 . .
C11 C16 H16A 120.3 . .
C15 C14 C13 121.2(10) . .
C15 C14 H14A 119.4 . .
C13 C14 H14A 119.4 . .
C14 C15 C16 120.0(9) . .
C14 C15 H15A 120.0 . .
C16 C15 H15A 120.0 . .
C12 C11 C16 121.3(9) . .
C12 C11 N1 119.8(8) . .
C16 C11 N1 118.9(9) . .
O1 C13 C12 125.9(8) . .
O1 C13 C14 116.2(9) . .
C12 C13 C14 117.9(11) . .
C13 O1 C17 116.9(9) . .
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 147.7(15) 6_556 2_655
F1 B1 F1 120.4(13) 6_556 .
F1 B1 F1 69.5(13) 2_655 .
F1 B1 F1 69.5(13) 6_556 5_656
F1 B1 F1 120.4(13) 2_655 5_656
F1 B1 F1 147.7(15) . 5_656
F1 B1 F2 108.2(5) 2_655 6_556
F1 B1 F2 95.2(9) . 6_556
F1 B1 F2 108.5(5) 5_656 6_556
F1 B1 F2 108.5(5) 6_556 5_656
F1 B1 F2 95.2(9) 2_655 5_656
F1 B1 F2 108.2(5) . 5_656
F2 B1 F2 151.6(13) 6_556 5_656
F1 B1 F2 108.2(5) 6_556 2_655
F1 B1 F2 108.5(5) . 2_655
F1 B1 F2 95.2(9) 5_656 2_655
F2 B1 F2 85.7(11) 6_556 2_655
F2 B1 F2 101.2(10) 5_656 2_655
F1 B1 F2 95.2(9) 6_556 .
F1 B1 F2 108.5(5) 2_655 .
F1 B1 F2 108.2(5) 5_656 .
F2 B1 F2 101.2(10) 6_556 .
F2 B1 F2 85.7(11) 5_656 .
F2 B1 F2 151.6(13) 2_655 .
F2 F1 B1 75.6(11) . .
F2 F1 F1 124(2) . 2_655
B1 F1 F1 55.3(7) . 2_655
F1 F2 B1 60.6(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N1 2.065(7) 3
Ru1 N1 2.065(7) 4
Ru1 N1 2.065(7) .
Ru1 N1 2.065(7) 2
Ru1 Ru1 2.389(4) 5_556
C1 N1 1.311(10) .
C1 N1 1.311(10) 8_556
C1 H1A 0.9500 .
N1 C11 1.455(12) .
C12 C11 1.371(13) .
C12 C13 1.415(13) .
C12 H12A 0.9500 .
C16 C15 1.393(14) .
C16 C11 1.414(13) .
C16 H16A 0.9500 .
C14 C15 1.375(15) .
C14 C13 1.435(13) .
C14 H14A 0.9500 .
C15 H15A 0.9500 .
C13 O1 1.335(13) .
O1 C17 1.435(11) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
B1 F1 1.33(2) 6_556
B1 F1 1.33(2) 2_655
B1 F1 1.33(2) .
B1 F1 1.33(2) 5_656
B1 F2 1.48(2) 6_556
B1 F2 1.48(2) 5_656
B1 F2 1.48(2) 2_655
B1 F2 1.48(2) .
F1 F2 1.06(3) .
F1 F1 1.51(4) 2_655
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
_geom_torsion_site_symmetry_4
N1 C1 N1 C11 164.6(8) 8_556 .
N1 C1 N1 Ru1 -6.8(2) 8_556 .
N1 Ru1 N1 C1 101.6(5) 3 .
N1 Ru1 N1 C1 -74.7(6) 4 .
Ru1 Ru1 N1 C1 13.4(5) 5_556 .
N1 Ru1 N1 C11 -69.5(7) 3 .
N1 Ru1 N1 C11 114.2(6) 4 .
Ru1 Ru1 N1 C11 -157.6(6) 5_556 .
C13 C14 C15 C16 1.5(14) . .
C11 C16 C15 C14 -0.4(14) . .
C13 C12 C11 C16 2.3(13) . .
C13 C12 C11 N1 179.0(7) . .
C15 C16 C11 C12 -1.5(13) . .
C15 C16 C11 N1 -178.3(8) . .
C1 N1 C11 C12 131.8(8) . .
Ru1 N1 C11 C12 -57.0(10) . .
C1 N1 C11 C16 -51.4(10) . .
Ru1 N1 C11 C16 119.8(8) . .
C11 C12 C13 O1 178.6(8) . .
C11 C12 C13 C14 -1.1(12) . .
C15 C14 C13 O1 179.5(8) . .
C15 C14 C13 C12 -0.8(13) . .
C12 C13 O1 C17 -1.5(13) . .
C14 C13 O1 C17 178.2(8) . .
F1 B1 F1 F2 62.7(12) 6_556 .
F1 B1 F1 F2 -152(2) 2_655 .
F1 B1 F1 F2 -36.9(11) 5_656 .
F2 B1 F1 F2 100.8(18) 6_556 .
F2 B1 F1 F2 -62.9(19) 5_656 .
F2 B1 F1 F2 -171.9(7) 2_655 .
F1 B1 F1 F1 -145.7(14) 6_556 2_655
F1 B1 F1 F1 114.7(11) 5_656 2_655
F2 B1 F1 F1 -107.5(7) 6_556 2_655
F2 B1 F1 F1 88.8(13) 5_656 2_655
F2 B1 F1 F1 -20.3(17) 2_655 2_655
F2 B1 F1 F1 152(2) . 2_655
F1 F1 F2 B1 -28.1(14) 2_655 .
F1 B1 F2 F1 -129.7(16) 6_556 .
F1 B1 F2 F1 28(2) 2_655 .
F1 B1 F2 F1 160.2(12) 5_656 .
F2 B1 F2 F1 -85.8(16) 6_556 .
F2 B1 F2 F1 122.1(15) 5_656 .
F2 B1 F2 F1 16.2(12) 2_655 .
