#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:36:34 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179022 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/20/4122087.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_4122087
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                   13.8927(5)
_cell_length_b                   13.8927(5)
_cell_length_c                   15.0744(11)
_cell_measurement_reflns_used    7151
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      2505
_cell_measurement_theta_min      2.7
_cell_volume                     2909.5(3)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13579
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.9162
_exptl_absorpt_correction_T_min  0.7971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1338
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.398
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.721
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1284
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.707
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0541
_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)+(0.0381P)²+4.9941P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1452
_reflns_number_gt                1127
_reflns_number_total             1284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5020647_si_001.cif
_cod_data_source_block           Ru2(mdanif)4BF4-298K
_cod_depositor_comments
'Adding full bibliography for 4122084--4122090.cif.'
_cod_original_sg_symbol_H-M      P4/nnc
_cod_database_code               4122087
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 0.67086(5) 0.0344(3) Uani 1 4 d S
C1 C 0.3860(4) 0.1140(4) 0.7500 0.0418(16) Uani 1 2 d S
H1A H 0.4333 0.0667 0.7500 0.050 Uiso 1 2 calc SR
N1 N 0.3640(3) 0.1583(3) 0.6749(3) 0.0394(10) Uani 1 1 d .
C12 C 0.3956(4) 0.1199(4) 0.5193(3) 0.0433(12) Uani 1 1 d .
H12A H 0.3305 0.1072 0.5109 0.052 Uiso 1 1 calc R
C16 C 0.5261(4) 0.1689(4) 0.6144(4) 0.0517(14) Uani 1 1 d .
H16A H 0.5487 0.1884 0.6696 0.062 Uiso 1 1 calc R
C14 C 0.5561(4) 0.1316(4) 0.4616(4) 0.0528(14) Uani 1 1 d .
H14A H 0.5988 0.1251 0.4144 0.063 Uiso 1 1 calc R
C15 C 0.5889(4) 0.1608(5) 0.5427(5) 0.0603(16) Uani 1 1 d .
H15A H 0.6537 0.1753 0.5501 0.072 Uiso 1 1 calc R
C11 C 0.4297(4) 0.1474(4) 0.6023(3) 0.0395(11) Uani 1 1 d .
C13 C 0.4593(4) 0.1118(4) 0.4497(4) 0.0479(13) Uani 1 1 d .
O1 O 0.4352(3) 0.0841(4) 0.3659(3) 0.0657(12) Uani 1 1 d .
C17 C 0.3378(5) 0.0592(6) 0.3495(4) 0.075(2) Uani 1 1 d .
H17A H 0.3306 0.0403 0.2887 0.113 Uiso 1 1 calc R
H17B H 0.2974 0.1138 0.3614 0.113 Uiso 1 1 calc R
H17C H 0.3196 0.0068 0.3875 0.113 Uiso 1 1 calc R
B1 B 0.7500 0.2500 0.7500 0.064(7) Uani 0.50 4 d SPDU
F1 F 0.8030(14) 0.2169(18) 0.6842(14) 0.141(11) Uani 0.25 1 d PDU
F2 F 0.8067(15) 0.1783(15) 0.7202(16) 0.141(11) 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 89.950(7) 3 2
N1 Ru1 N1 176.6(2) 3 4
N1 Ru1 N1 89.950(8) 2 4
N1 Ru1 N1 89.950(7) 3 .
N1 Ru1 N1 176.6(2) 2 .
N1 Ru1 N1 89.950(7) 4 .
N1 Ru1 Ru1 88.30(11) 3 5_556
N1 Ru1 Ru1 88.30(11) 2 5_556
N1 Ru1 Ru1 88.30(11) 4 5_556
N1 Ru1 Ru1 88.30(11) . 5_556
N1 C1 N1 121.2(6) . 8_556
N1 C1 H1A 119.4 . .
N1 C1 H1A 119.4 8_556 .
C1 N1 C11 117.2(4) . .
C1 N1 Ru1 119.7(4) . .
C11 N1 Ru1 122.7(3) . .
C13 C12 C11 119.3(5) . .
C13 C12 H12A 120.4 . .
C11 C12 H12A 120.4 . .
C11 C16 C15 119.1(6) . .
C11 C16 H16A 120.5 . .
C15 C16 H16A 120.5 . .
C15 C14 C13 119.9(5) . .
C15 C14 H14A 120.1 . .
C13 C14 H14A 120.1 . .
C14 C15 C16 120.6(5) . .
C14 C15 H15A 119.7 . .
C16 C15 H15A 119.7 . .
C16 C11 C12 120.5(5) . .
C16 C11 N1 119.6(5) . .
C12 C11 N1 119.9(4) . .
O1 C13 C12 124.9(5) . .
O1 C13 C14 114.5(5) . .
C12 C13 C14 120.6(5) . .
C13 O1 C17 117.6(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 139(3) 6_556 2_655
F1 B1 F1 112.0(14) 6_556 .
F1 B1 F1 82(2) 2_655 .
F1 B1 F1 82(2) 6_556 5_656
F1 B1 F1 112.0(14) 2_655 5_656
F1 B1 F1 139(3) . 5_656
F1 B1 F2 108.7(4) 2_655 6_556
F1 B1 F2 100.5(14) . 6_556
F1 B1 F2 109.5(4) 5_656 6_556
F1 B1 F2 109.5(4) 6_556 5_656
F1 B1 F2 100.5(14) 2_655 5_656
F1 B1 F2 108.7(4) . 5_656
F2 B1 F2 141(2) 6_556 5_656
F1 B1 F2 100.5(14) 6_556 .
F1 B1 F2 109.5(4) 2_655 .
F1 B1 F2 108.7(4) 5_656 .
F2 B1 F2 108.4(14) 6_556 .
F2 B1 F2 84.7(19) 5_656 .
F1 B1 F2 108.7(4) 6_556 2_655
F1 B1 F2 109.5(4) . 2_655
F1 B1 F2 100.5(14) 5_656 2_655
F2 B1 F2 84.7(19) 6_556 2_655
F2 B1 F2 108.4(14) 5_656 2_655
F2 B1 F2 141(2) . 2_655
F2 F1 B1 75.4(19) . .
F2 F1 F1 115(3) . 2_655
B1 F1 F1 48.8(10) . 2_655
F1 F2 B1 71.3(18) . .
F1 F2 F2 107(3) . 5_656
B1 F2 F2 47.7(9) . 5_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N1 2.033(4) 3
Ru1 N1 2.033(4) 2
Ru1 N1 2.033(4) 4
Ru1 N1 2.033(4) .
Ru1 Ru1 2.3859(14) 5_556
C1 N1 1.324(5) .
C1 N1 1.324(5) 8_556
C1 H1A 0.9300 .
N1 C11 1.433(6) .
C12 C13 1.377(7) .
C12 C11 1.392(7) .
C12 H12A 0.9300 .
C16 C11 1.384(7) .
C16 C15 1.394(8) .
C16 H16A 0.9300 .
C14 C15 1.366(9) .
C14 C13 1.386(8) .
C14 H14A 0.9300 .
C15 H15A 0.9300 .
C13 O1 1.362(7) .
O1 C17 1.418(8) .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
B1 F1 1.318(17) 6_556
B1 F1 1.318(17) 2_655
B1 F1 1.318(17) .
B1 F1 1.318(17) 5_656
B1 F2 1.347(18) 6_556
B1 F2 1.347(18) 5_656
B1 F2 1.347(18) .
B1 F2 1.347(18) 2_655
F1 F2 0.76(6) .
F1 F1 1.74(4) 2_655
F2 F2 1.81(4) 5_656
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 165.3(4) 8_556 .
N1 C1 N1 Ru1 -7.35(14) 8_556 .
N1 Ru1 N1 C1 102.8(3) 3 .
N1 Ru1 N1 C1 -73.8(3) 4 .
Ru1 Ru1 N1 C1 14.5(3) 5_556 .
N1 Ru1 N1 C11 -69.5(4) 3 .
N1 Ru1 N1 C11 113.9(3) 4 .
Ru1 Ru1 N1 C11 -157.8(4) 5_556 .
C13 C14 C15 C16 1.3(9) . .
C11 C16 C15 C14 -0.3(9) . .
C15 C16 C11 C12 -1.2(8) . .
C15 C16 C11 N1 -178.1(5) . .
C13 C12 C11 C16 1.7(8) . .
C13 C12 C11 N1 178.6(5) . .
C1 N1 C11 C16 -53.4(6) . .
Ru1 N1 C11 C16 119.1(5) . .
C1 N1 C11 C12 129.7(5) . .
Ru1 N1 C11 C12 -57.8(6) . .
C11 C12 C13 O1 178.9(5) . .
C11 C12 C13 C14 -0.7(8) . .
C15 C14 C13 O1 179.5(6) . .
C15 C14 C13 C12 -0.8(9) . .
C12 C13 O1 C17 -1.8(9) . .
C14 C13 O1 C17 177.8(6) . .
F1 B1 F1 F2 75(2) 6_556 .
F1 B1 F1 F2 -145(3) 2_655 .
F1 B1 F1 F2 -29.5(19) 5_656 .
F2 B1 F1 F2 108(3) 6_556 .
F2 B1 F1 F2 -46(3) 5_656 .
F2 B1 F1 F2 -164.4(16) 2_655 .
F1 B1 F1 F1 -140(2) 6_556 2_655
F1 B1 F1 F1 115.1(13) 5_656 2_655
F2 B1 F1 F1 -107.7(5) 6_556 2_655
F2 B1 F1 F1 99(2) 5_656 2_655
F2 B1 F1 F1 145(3) . 2_655
F2 B1 F1 F1 -20(2) 2_655 2_655
F1 F1 F2 B1 -28.8(16) 2_655 .
B1 F1 F2 F2 32.0(13) . 5_656
F1 F1 F2 F2 3(2) 2_655 5_656
F1 B1 F2 F1 -114(3) 6_556 .
F1 B1 F2 F1 37(3) 2_655 .
F1 B1 F2 F1 160.1(18) 5_656 .
F2 B1 F2 F1 -81(2) 6_556 .
F2 B1 F2 F1 137(3) 5_656 .
F2 B1 F2 F1 24(2) 2_655 .
F1 B1 F2 F2 108.9(5) 6_556 5_656
F1 B1 F2 F2 -99(2) 2_655 5_656
F1 B1 F2 F2 -137(3) . 5_656
F1 B1 F2 F2 23(2) 5_656 5_656
F2 B1 F2 F2 142(2) 6_556 5_656
F2 B1 F2 F2 -112.8(12) 2_655 5_656
