#------------------------------------------------------------------------------
#$Date: 2015-07-05 11:57:37 +0300 (Sun, 05 Jul 2015) $
#$Revision: 140123 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/38/4123816.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_4123816
loop_
_publ_author_name
'Mizuno, Asato'
'Shuku, Yoshiaki'
'Suizu, Rie'
'Matsushita, Michio M.'
'Tsuchiizu, Masahisa'
'Reta Mañeru, Daniel'
'Illas, Francesc'
'Robert, Vincent'
'Awaga, Kunio'
_publ_section_title
;
 Discovery of the K4 Structure Formed by a Triangular π Radical Anion.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7612
_journal_page_last               7615
_journal_paper_doi               10.1021/jacs.5b04180
_journal_volume                  137
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C60 H42 N6 O12 Rb1.4'
_chemical_formula_sum            'C60 H42 N6 O12 Rb1.4'
_chemical_formula_weight         1158.68
_space_group_crystal_system      cubic
_space_group_IT_number           214
_space_group_name_Hall           'I 4bd 2c 3'
_space_group_name_H-M_alt        'I 41 3 2'
_symmetry_space_group_name_Hall  'I 4bd 2c 3'
_symmetry_space_group_name_H-M   'I 41 3 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   30.582(3)
_cell_length_b                   30.582(3)
_cell_length_c                   30.582(3)
_cell_measurement_reflns_used    14999
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.10
_cell_volume                     28602(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            115158
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.453
_diffrn_reflns_theta_min         3.124
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4734.40
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.26
_refine_ls_abs_structure_details
;
 Flack x determined using 1001 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.036(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     128
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1341
_refine_ls_R_factor_gt           0.1217
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3413
_refine_ls_wR_factor_ref         0.3552
_reflns_number_gt                3768
_reflns_number_total             5478
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ja5b04180_si_002.cif
_cod_data_source_block           RbNDI
_cod_depositor_comments          'Adding full bibliography for 4123816.cif.'
_cod_database_code               4123816
_platon_squeeze_void_probe_radius 1.20
loop_
_symmetry_equiv_pos_site_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 +Y,+Z,+X
3 +Z,+X,+Y
4 1/4-Y,3/4+X,1/4+Z
5 1/4-Z,3/4+Y,1/4+X
6 1/4-X,3/4+Z,1/4+Y
7 1/2-X,-Y,1/2+Z
8 -Z,1/2+X,1/2-Y
9 -X,1/2+Y,1/2-Z
10 1/2-Y,-Z,1/2+X
11 1/2-Z,-X,1/2+Y
12 1/4+Y,1/4-X,3/4+Z
13 1/4+Z,1/4-Y,3/4+X
14 1/4+X,1/4-Z,3/4+Y
15 -Y,1/2+Z,1/2-X
16 3/4-Z,3/4-Y,3/4-X
17 3/4-X,3/4-Z,3/4-Y
18 3/4-Y,3/4-X,3/4-Z
19 1/2+Y,1/2-Z,-X
20 3/4+Y,1/4+X,1/4-Z
21 3/4+Z,1/4+Y,1/4-X
22 3/4+X,1/4+Z,1/4-Y
23 1/2+X,1/2-Y,-Z
24 1/2+Z,1/2-X,-Y
25 1/2+X,1/2+Y,1/2+Z
26 1/2+Y,1/2+Z,1/2+X
27 1/2+Z,1/2+X,1/2+Y
28 3/4-Y,1/4+X,3/4+Z
29 3/4-Z,1/4+Y,3/4+X
30 3/4-X,1/4+Z,3/4+Y
31 -X,1/2-Y,+Z
32 1/2-Z,+X,-Y
33 1/2-X,+Y,-Z
34 -Y,1/2-Z,+X
35 -Z,1/2-X,+Y
36 3/4+Y,3/4-X,1/4+Z
37 3/4+Z,3/4-Y,1/4+X
38 3/4+X,3/4-Z,1/4+Y
39 1/2-Y,+Z,-X
40 1/4-Z,1/4-Y,1/4-X
41 1/4-X,1/4-Z,1/4-Y
42 1/4-Y,1/4-X,1/4-Z
43 +Y,-Z,1/2-X
44 1/4+Y,3/4+X,3/4-Z
45 1/4+Z,3/4+Y,3/4-X
46 1/4+X,3/4+Z,3/4-Y
47 +X,-Y,1/2-Z
48 +Z,-X,1/2-Y
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_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Rb1 Rb 0.58696(9) 0.54394(11) 0.15702(13) 0.1515(18) Uani 0.233(3) 48 d .
O1 O 0.51164(11) 0.53507(11) 0.20842(12) 0.1065(10) Uani 1 48 d .
O2 O 0.43639(11) 0.62194(11) 0.30172(11) 0.1044(10) Uani 1 48 d .
N1 N 0.47389(11) 0.58140(11) 0.25192(12) 0.0880(10) Uani 1 48 d .
C1 C 0.5755(3) 0.5985(3) 0.3244(3) 0.176(4) Uani 1 48 d .
C2 C 0.52739(19) 0.5843(2) 0.31488(19) 0.126(2) Uani 1 48 d .
C3 C 0.51665(15) 0.59951(16) 0.26778(17) 0.1019(14) Uani 1 48 d .
C4 C 0.47713(14) 0.54746(13) 0.22046(14) 0.0811(11) Uani 1 48 d .
C5 C 0.43558(13) 0.59613(16) 0.27133(13) 0.0866(11) Uani 1 48 d .
C6 C 0.43529(13) 0.53115(13) 0.20352(14) 0.0855(11) Uani 1 48 d .
C7 C 0.39409(14) 0.57898(13) 0.25225(13) 0.0840(11) Uani 1 48 d .
C8 C 0.43529(13) 0.49726(14) 0.17131(13) 0.0843(11) Uani 1 48 d .
C9 C 0.39485(12) 0.54767(13) 0.22036(12) 0.0778(10) Uani 1 48 d .
C10 C 0.35371(15) 0.59356(13) 0.26826(14) 0.0917(12) Uani 1 48 d .
H1A H 0.59539 0.58793 0.30118 0.2113 Uiso 1 48 calc R
H1B H 0.5855 0.58668 0.35287 0.2113 Uiso 1 48 calc R
H2A H 0.52445 0.55217 0.31728 0.1518 Uiso 1 48 calc R
H2B H 0.50717 0.59813 0.33605 0.1518 Uiso 1 48 calc R
H3 H 0.54022 0.58846 0.248 0.1223 Uiso 1 48 calc R
H8 H 0.46203 0.48576 0.16046 0.1012 Uiso 1 48 calc R
H10 H 0.35354 0.61476 0.29097 0.1100 Uiso 1 48 calc R
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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Rb Rb -0.9393 2.9676
;
International Tables for Crystallography
(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_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Rb1 O2 67.09(12) yes . 13_564
Rb1 O1 C4 151.5(3) yes . .
Rb1 O2 C5 147.4(3) yes 13_564 .
C3 N1 C4 115.4(3) yes . .
C3 N1 C5 118.5(4) yes . .
C4 N1 C5 125.9(4) yes . .
C1 C1 C2 105.2(6) yes 13_564 .
C1 C2 C3 106.9(5) yes . .
N1 C3 C2 112.0(4) yes . .
N1 C3 C3 112.4(4) yes . 13_564
C2 C3 C3 108.4(4) yes . 13_564
O1 C4 N1 120.6(4) yes . .
O1 C4 C6 124.1(4) yes . .
N1 C4 C6 115.3(4) yes . .
O2 C5 N1 121.2(4) yes . .
O2 C5 C7 122.9(4) yes . .
N1 C5 C7 115.9(4) yes . .
C4 C6 C8 119.3(4) yes . .
C4 C6 C9 120.4(4) yes . .
C8 C6 C9 120.2(4) yes . .
C5 C7 C9 120.7(4) yes . .
C5 C7 C10 120.1(4) yes . .
C9 C7 C10 119.2(4) yes . .
C6 C8 C10 118.9(4) yes . 17_555
C6 C9 C7 121.2(4) yes . .
C6 C9 C9 117.0(3) yes . 17_555
C7 C9 C9 121.7(4) yes . 17_555
C7 C10 C8 122.9(4) yes . 17_555
C1 C1 H1A 110.707 no 13_564 .
C1 C1 H1B 110.689 no 13_564 .
C2 C1 H1A 110.718 no . .
C2 C1 H1B 110.710 no . .
H1A C1 H1B 108.799 no . .
C1 C2 H2A 110.333 no . .
C1 C2 H2B 110.356 no . .
C3 C2 H2A 110.339 no . .
C3 C2 H2B 110.355 no . .
H2A C2 H2B 108.571 no . .
N1 C3 H3 107.935 no . .
C2 C3 H3 107.964 no . .
C3 C3 H3 107.965 no 13_564 .
C6 C8 H8 120.594 no . .
C10 C8 H8 120.546 no 17_555 .
C7 C10 H10 118.514 no . .
C8 C10 H10 118.544 no 17_555 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_2
Rb1 O1 2.802(5) yes .
Rb1 O2 2.930(5) yes 13_564
O1 C4 1.180(5) yes .
O2 C5 1.220(6) yes .
N1 C3 1.501(6) yes .
N1 C4 1.419(5) yes .
N1 C5 1.388(5) yes .
C1 C1 1.622(11) yes 13_564
C1 C2 1.562(11) yes .
C2 C3 1.549(8) yes .
C3 C3 1.560(7) yes 13_564
C4 C6 1.468(6) yes .
C5 C7 1.492(6) yes .
C6 C8 1.430(6) yes .
C6 C9 1.432(5) yes .
C7 C9 1.367(6) yes .
C7 C10 1.401(6) yes .
C8 C10 1.362(6) yes 17_555
C9 C9 1.443(5) yes 17_555
C1 H1A 0.990 no .
C1 H1B 0.990 no .
C2 H2A 0.990 no .
C2 H2B 0.990 no .
C3 H3 1.000 no .
C8 H8 0.950 no .
C10 H10 0.950 no .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_2
O1 C3 2.684(6) no .
O1 C5 3.550(5) no .
O1 C8 2.842(5) no .
O2 N1 3.423(5) no 13_564
O2 C2 3.038(7) no .
O2 C3 2.752(6) no .
O2 C3 2.847(6) no 13_564
O2 C4 3.594(5) no .
O2 C4 3.516(5) no 13_564
O2 C10 2.862(6) no .
N1 N1 2.929(5) no 13_564
N1 C5 3.337(6) no 13_564
N1 C9 2.800(5) no .
C1 C3 2.961(10) no 13_564
C2 C2 2.970(9) no 13_564
C2 C4 3.460(7) no .
C2 C5 3.129(7) no .
C3 C5 3.017(7) no 13_564
C4 C7 2.885(6) no .
C5 C6 2.872(6) no .
C6 C7 2.815(6) no 17_555
C8 C9 2.808(5) no 17_555
C9 C10 2.809(6) no 17_555
O1 O1 3.327(5) no 47_565
O1 C4 3.495(5) no 47_565
N1 C8 3.563(5) no 47_565
C4 O1 3.495(5) no 47_565
C4 C4 3.419(6) no 47_565
C4 C6 3.581(6) no 47_565
C5 C8 3.352(6) no 47_565
C5 C10 3.463(6) no 30_554
C6 C4 3.581(6) no 47_565
C6 C6 3.422(6) no 47_565
C6 C9 3.572(6) no 47_565
C7 C7 3.518(6) no 30_554
C7 C8 3.534(6) no 47_565
C7 C10 3.354(6) no 30_554
C8 N1 3.563(5) no 47_565
C8 C5 3.352(6) no 47_565
C8 C7 3.534(6) no 47_565
C9 C6 3.572(6) no 47_565
C9 C9 3.557(5) no 30_554
C9 C9 3.433(6) no 47_565
C10 C5 3.463(6) no 30_554
C10 C7 3.354(6) no 30_554
C10 C10 3.507(6) no 30_554
Rb1 H3 3.4115 no .
Rb1 H10 3.5283 no 13_564
O1 H2A 3.3927 no .
O1 H3 2.2125 no .
O1 H8 2.5937 no .
O2 H2A 3.4687 no .
O2 H2B 2.5135 no .
O2 H3 2.2672 no 13_564
O2 H10 2.5644 no .
N1 H2A 2.6805 no .
N1 H2B 2.8138 no .
N1 H3 2.8146 no 13_564
C1 H2A 3.4099 no 13_564
C1 H2B 2.6455 no 13_564
C1 H3 2.5928 no .
C1 H3 3.2296 no 13_564
C2 H1A 2.6559 no 13_564
C2 H1B 3.4004 no 13_564
C2 H2B 3.2559 no 13_564
C2 H3 2.6369 no 13_564
C3 H1A 2.6396 no .
C3 H1A 3.2263 no 13_564
C3 H1B 3.3703 no .
C3 H2A 3.3882 no 13_564
C3 H2B 2.6784 no 13_564
C4 H2A 3.2988 no .
C4 H3 2.4503 no .
C4 H8 2.6722 no .
C5 H2A 3.3420 no .
C5 H2B 2.9520 no .
C5 H3 3.2871 no .
C5 H3 2.8247 no 13_564
C5 H10 2.6420 no .
C6 H10 3.2611 no 17_555
C7 H8 3.2819 no 17_555
C9 H8 3.3409 no .
C9 H10 3.2355 no .
H1A H1A 2.9659 no 13_564
H1A H1B 2.5435 no 13_564
H1A H2A 2.4789 no .
H1A H2A 3.5642 no 13_564
H1A H2B 2.9178 no .
H1A H2B 2.3910 no 13_564
H1A H3 2.3435 no .
H1B H1B 2.4613 no 13_564
H1B H2A 2.4051 no .
H1B H2B 2.4750 no .
H1B H2B 3.5412 no 13_564
H1B H3 3.4937 no .
H2A H3 2.4399 no .
H2A H3 3.5393 no 13_564
H2B H3 2.8914 no .
H2B H3 2.4091 no 13_564
H3 H3 2.8860 no 13_564
H8 H10 2.2987 no 17_555
Rb1 H2A 3.5932 no 47_565
O1 H2A 2.8088 no 47_565
O2 H8 3.5778 no 47_565
O2 H10 3.3674 no 30_554
N1 H8 3.3956 no 47_565
C2 H8 3.0261 no 47_565
C4 H2A 3.5651 no 47_565
C5 H8 3.3582 no 47_565
C5 H10 3.5272 no 30_554
C8 H2A 3.1372 no 47_565
H2A Rb1 3.5932 no 47_565
H2A O1 2.8088 no 47_565
H2A C4 3.5651 no 47_565
H2A C8 3.1372 no 47_565
H2A H8 2.3352 no 47_565
H2B H8 2.9153 no 47_565
H8 O2 3.5778 no 47_565
H8 N1 3.3956 no 47_565
H8 C2 3.0261 no 47_565
H8 C5 3.3582 no 47_565
H8 H2A 2.3352 no 47_565
H8 H2B 2.9153 no 47_565
H10 O2 3.3674 no 30_554
H10 C5 3.5272 no 30_554
H10 H10 3.4508 no 30_554
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_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O1 Rb1 O2 C5 -63.1(4) no . 13_564 13_564
O2 Rb1 O1 C4 34.0(5) no 13_564 . .
Rb1 O1 C4 N1 -78.7(8) no . . .
Rb1 O1 C4 C6 98.6(7) no . . .
Rb1 O2 C5 N1 124.9(5) no 13_564 . .
Rb1 O2 C5 C7 -54.1(7) no 13_564 . .
C3 N1 C4 O1 0.2(6) no . . .
C3 N1 C4 C6 -177.4(3) no . . .
C4 N1 C3 C2 -106.4(4) no . . .
C4 N1 C3 C3 131.3(3) no . . 13_564
C3 N1 C5 O2 -2.8(6) no . . .
C3 N1 C5 C7 176.3(3) no . . .
C5 N1 C3 C2 68.4(5) no . . .
C5 N1 C3 C3 -54.0(5) no . . 13_564
C4 N1 C5 O2 171.4(4) no . . .
C4 N1 C5 C7 -9.5(6) no . . .
C5 N1 C4 O1 -174.1(4) no . . .
C5 N1 C4 C6 8.4(6) no . . .
C1 C1 C2 C3 67.0(7) no 13_564 . .
C2 C1 C1 C2 -68.3(7) no . 13_564 13_564
C1 C2 C3 N1 170.6(4) no . . .
C1 C2 C3 C3 -64.8(5) no . . 13_564
N1 C3 C3 N1 -48.0(5) no . 13_564 13_564
N1 C3 C3 C2 -172.3(3) no . 13_564 13_564
C2 C3 C3 N1 -172.3(4) no . 13_564 13_564
C2 C3 C3 C2 63.3(4) no . 13_564 13_564
O1 C4 C6 C8 1.9(6) no . . .
O1 C4 C6 C9 179.3(4) no . . .
N1 C4 C6 C8 179.3(3) no . . .
N1 C4 C6 C9 -3.3(5) no . . .
O2 C5 C7 C9 -175.1(4) no . . .
O2 C5 C7 C10 2.1(6) no . . .
N1 C5 C7 C9 5.8(6) no . . .
N1 C5 C7 C10 -177.0(3) no . . .
C4 C6 C8 C10 178.7(3) no . . 17_555
C4 C6 C9 C7 0.3(6) no . . .
C4 C6 C9 C9 -179.4(3) no . . 17_555
C8 C6 C9 C7 177.7(3) no . . .
C8 C6 C9 C9 -2.0(5) no . . 17_555
C9 C6 C8 C10 1.3(6) no . . 17_555
C5 C7 C9 C6 -1.6(6) no . . .
C5 C7 C9 C9 178.1(3) no . . 17_555
C5 C7 C10 C8 -178.9(3) no . . 17_555
C9 C7 C10 C8 -1.6(6) no . . 17_555
C10 C7 C9 C6 -178.9(3) no . . .
C10 C7 C9 C9 0.8(6) no . . 17_555
C6 C8 C10 C7 0.6(6) no . 17_555 17_555
C6 C9 C9 C6 -179.4(3) no . 17_555 17_555
C6 C9 C9 C7 0.9(5) no . 17_555 17_555
C7 C9 C9 C6 0.9(5) no . 17_555 17_555
C7 C9 C9 C7 -178.8(3) no . 17_555 17_555
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.038 0.031 0.037 17787 1388 ' '
