#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:08:31 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180289 $
#$URL: svn://www.crystallography.net/cod/cif/7/15/03/7150397.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_7150397
loop_
_publ_author_name
'Loeb, Stephen J.'
'Tiburcio, Jorge'
'Vella, Sarah J.'
'Wisner, James A.'
_publ_section_title
;
 A versatile template for the formation of [2]pseudorotaxanes.
 1,2-Bis(pyridinium)ethane axles and 24-crown-8 ether wheels.
;
_journal_issue                   4
_journal_name_full               'Organic & biomolecular chemistry'
_journal_page_first              667
_journal_page_last               680
_journal_paper_doi               10.1039/b514528g
_journal_volume                  4
_journal_year                    2006
_chemical_formula_sum            'C30 H50 B2 F8 N2 O10'
_chemical_formula_weight         772.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 96.5840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4924(6)
_cell_length_b                   16.5364(10)
_cell_length_c                   10.7738(6)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.5
_cell_volume                     1857.00(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_molecular_graphics    'Bruker SHELXTL XP'
_computing_publication_material  'Bruker SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'hemisphere 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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14875
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.871299
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       yellow
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.8(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         6537
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1379P)²+1.4729P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2265
_refine_ls_wR_factor_ref         0.2357
_reflns_number_gt                5684
_reflns_number_total             6537
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b514528g.txt
_cod_data_source_block
'[2]pseudorotaxane_[(1,2-bis(3-methoxypyridinium)ethane)-24C8][BF4]2'
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7150397
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
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
O1 O 0.8322(3) 0.0569(2) 1.1068(3) 0.0519(8) Uani 1 1 d . . .
O2 O 0.6974(3) 0.4793(2) 0.4043(3) 0.0499(8) Uani 1 1 d . . .
O3 O 1.0880(3) 0.2229(2) 0.8867(4) 0.0595(9) Uani 1 1 d . A .
O4 O 1.0822(4) 0.2047(2) 0.6248(4) 0.0650(10) Uani 1 1 d . . .
O5 O 0.8496(5) 0.2151(4) 0.4370(4) 0.0880(16) Uani 1 1 d . . .
O6 O 0.5812(4) 0.2646(3) 0.4482(4) 0.0732(11) Uani 1 1 d . . .
O7 O 0.4439(3) 0.3155(2) 0.6411(4) 0.0555(9) Uani 1 1 d . . .
O8 O 0.4401(4) 0.3399(3) 0.8963(4) 0.0682(11) Uani 1 1 d . . .
O9 O 0.6811(4) 0.3529(3) 1.0697(3) 0.0807(14) Uani 1 1 d . . .
O10 O 0.9560(3) 0.3254(3) 1.0491(3) 0.0618(10) Uani 1 1 d . . .
N1 N 0.7175(3) 0.1857(2) 0.8478(3) 0.0369(8) Uani 1 1 d . . .
N2 N 0.8232(3) 0.36330(19) 0.6741(3) 0.0358(8) Uani 1 1 d . . .
C1 C 0.9620(5) 0.0415(4) 1.0799(6) 0.0697(16) Uani 1 1 d . . .
H1A H 1.0058 0.0092 1.1455 0.104 Uiso 1 1 calc R . .
H1B H 1.0064 0.0919 1.0746 0.104 Uiso 1 1 calc R . .
H1C H 0.9599 0.0132 1.0019 0.104 Uiso 1 1 calc R . .
C2 C 0.7574(4) 0.1026(3) 1.0226(4) 0.0385(9) Uani 1 1 d . . .
C3 C 0.6279(4) 0.1084(3) 1.0404(4) 0.0410(10) Uani 1 1 d . . .
H3A H 0.5976 0.0824 1.1078 0.049 Uiso 1 1 calc R . .
C4 C 0.5465(5) 0.1518(3) 0.9593(5) 0.0485(11) Uani 1 1 d . . .
H4A H 0.4601 0.1558 0.9702 0.058 Uiso 1 1 calc R . .
C5 C 0.5938(4) 0.1903(3) 0.8600(5) 0.0467(10) Uani 1 1 d . . .
H5A H 0.5389 0.2192 0.8023 0.056 Uiso 1 1 calc R . .
C6 C 0.8003(4) 0.1443(2) 0.9266(4) 0.0342(8) Uani 1 1 d . . .
H6A H 0.8870 0.1439 0.9161 0.041 Uiso 1 1 calc R . .
C7 C 0.7656(4) 0.2306(3) 0.7420(4) 0.0388(9) Uani 1 1 d . . .
H7A H 0.7059 0.2246 0.6669 0.047 Uiso 1 1 calc R . .
H7B H 0.8481 0.2091 0.7257 0.047 Uiso 1 1 calc R . .
C8 C 0.7788(4) 0.3184(3) 0.7776(4) 0.0401(9) Uani 1 1 d . . .
H8A H 0.6967 0.3395 0.7958 0.048 Uiso 1 1 calc R . .
H8B H 0.8398 0.3243 0.8518 0.048 Uiso 1 1 calc R . .
C9 C 0.9505(4) 0.3654(3) 0.6627(4) 0.0428(10) Uani 1 1 d . . .
H9A H 1.0087 0.3408 0.7226 0.051 Uiso 1 1 calc R . .
C10 C 0.9920(4) 0.4031(3) 0.5650(5) 0.0463(11) Uani 1 1 d . . .
H10A H 1.0792 0.4031 0.5562 0.056 Uiso 1 1 calc R . .
C11 C 0.9071(4) 0.4422(3) 0.4766(4) 0.0422(10) Uani 1 1 d . . .
H11A H 0.9369 0.4691 0.4098 0.051 Uiso 1 1 calc R . .
C12 C 0.7783(4) 0.4405(2) 0.4890(4) 0.0370(9) Uani 1 1 d . . .
C13 C 0.7371(4) 0.3996(3) 0.5909(4) 0.0364(9) Uani 1 1 d . . .
H13A H 0.6503 0.3976 0.6009 0.044 Uiso 1 1 calc R . .
C14 C 0.5641(5) 0.4843(4) 0.4211(5) 0.0607(14) Uani 1 1 d . . .
H14A H 0.5191 0.5136 0.3527 0.091 Uiso 1 1 calc R . .
H14B H 0.5548 0.5118 0.4980 0.091 Uiso 1 1 calc R . .
H14C H 0.5292 0.4307 0.4240 0.091 Uiso 1 1 calc R . .
C15 C 1.0714(6) 0.2855(4) 1.0870(6) 0.0757(17) Uani 1 1 d . . .
H15A H 1.0527 0.2337 1.1230 0.091 Uiso 1 1 calc R . .
H15B H 1.1205 0.3172 1.1515 0.091 Uiso 1 1 calc R . .
C16 C 1.1502(5) 0.2722(4) 0.9825(5) 0.0624(14) Uani 1 1 d . . .
H16A H 1.1699 0.3241 0.9473 0.075 Uiso 1 1 calc R . .
H16B H 1.2307 0.2470 1.0150 0.075 Uiso 1 1 calc R . .
C17 C 1.1789(5) 0.1783(4) 0.8280(6) 0.0651(15) Uani 1 1 d . . .
H17A H 1.2140 0.1356 0.8835 0.078 Uiso 1 1 calc R A .
H17B H 1.2488 0.2137 0.8116 0.078 Uiso 1 1 calc R . .
C18 C 1.1202(6) 0.1425(4) 0.7092(7) 0.0761(19) Uani 1 1 d . A .
H18A H 1.1817 0.1076 0.6748 0.091 Uiso 1 1 calc R . .
H18B H 1.0464 0.1100 0.7240 0.091 Uiso 1 1 calc R . .
C21 C 0.7358(8) 0.1752(5) 0.3764(6) 0.088(2) Uani 1 1 d . . .
H21A H 0.7558 0.1480 0.3012 0.105 Uiso 1 1 calc R . .
H21B H 0.7060 0.1350 0.4320 0.105 Uiso 1 1 calc R . .
C22 C 0.6368(7) 0.2349(5) 0.3449(5) 0.083(2) Uani 1 1 d . . .
H22A H 0.6733 0.2799 0.3032 0.099 Uiso 1 1 calc R A .
H22B H 0.5701 0.2112 0.2864 0.099 Uiso 1 1 calc R . .
C23 C 0.4762(7) 0.2221(5) 0.4875(7) 0.083(2) Uani 1 1 d . . .
H23A H 0.5077 0.1838 0.5521 0.100 Uiso 1 1 calc R A .
H23B H 0.4341 0.1916 0.4175 0.100 Uiso 1 1 calc R . .
C24 C 0.3851(5) 0.2739(5) 0.5346(5) 0.0691(16) Uani 1 1 d . . .
H24A H 0.3529 0.3125 0.4708 0.083 Uiso 1 1 calc R . .
H24B H 0.3133 0.2423 0.5570 0.083 Uiso 1 1 calc R . .
C25 C 0.3535(5) 0.3689(4) 0.6920(7) 0.0740(19) Uani 1 1 d . . .
H25A H 0.3296 0.4124 0.6337 0.089 Uiso 1 1 calc R . .
H25B H 0.2765 0.3391 0.7051 0.089 Uiso 1 1 calc R . .
C26 C 0.4119(6) 0.4019(4) 0.8098(8) 0.079(2) Uani 1 1 d . . .
H26A H 0.4900 0.4305 0.7968 0.094 Uiso 1 1 calc R . .
H26B H 0.3536 0.4401 0.8418 0.094 Uiso 1 1 calc R . .
C27 C 0.4619(7) 0.3665(7) 1.0256(8) 0.119(4) Uani 1 1 d . . .
H27A H 0.3932 0.4038 1.0381 0.142 Uiso 1 1 calc R . .
H27B H 0.4502 0.3195 1.0769 0.142 Uiso 1 1 calc R . .
C28 C 0.5682(8) 0.4008(9) 1.0723(7) 0.148(5) Uani 1 1 d . . .
H28A H 0.5605 0.4154 1.1583 0.178 Uiso 1 1 calc R . .
H28B H 0.5788 0.4505 1.0267 0.178 Uiso 1 1 calc R . .
C29 C 0.7903(8) 0.3993(5) 1.1180(6) 0.088(2) Uani 1 1 d . . .
H29A H 0.8113 0.4374 1.0550 0.105 Uiso 1 1 calc R . .
H29B H 0.7700 0.4299 1.1901 0.105 Uiso 1 1 calc R . .
C30 C 0.8968(6) 0.3495(5) 1.1530(5) 0.0786(19) Uani 1 1 d . . .
H30A H 0.9581 0.3784 1.2109 0.094 Uiso 1 1 calc R . .
H30B H 0.8692 0.3019 1.1955 0.094 Uiso 1 1 calc R . .
C19A C 1.0647(13) 0.1927(10) 0.4834(14) 0.036(3) Uani 0.40 1 d P A -1
H19A H 1.1447 0.2103 0.4551 0.043 Uiso 0.40 1 calc PR A -1
H19B H 1.0611 0.1346 0.4710 0.043 Uiso 0.40 1 calc PR A -1
C20A C 1.0055(19) 0.2121(8) 0.4304(12) 0.055(4) Uani 0.40 1 d P A -1
H20A H 1.0157 0.1848 0.3525 0.066 Uiso 0.40 1 calc PR A -1
H20B H 1.0303 0.2679 0.4187 0.066 Uiso 0.40 1 calc PR A -1
C19B C 1.0511(16) 0.1557(9) 0.5229(13) 0.083(4) Uani 0.60 1 d P A -2
H19C H 1.0750 0.1017 0.5523 0.100 Uiso 0.60 1 calc PR A -2
H19D H 1.1119 0.1701 0.4652 0.100 Uiso 0.60 1 calc PR A -2
C20B C 0.9383(8) 0.1457(6) 0.4500(9) 0.058(2) Uani 0.60 1 d P A -2
H20C H 0.8937 0.1006 0.4830 0.069 Uiso 0.60 1 calc PR A -2
H20D H 0.9573 0.1305 0.3671 0.069 Uiso 0.60 1 calc PR A -2
B1 B 0.2207(5) 0.4875(4) 0.2999(6) 0.0499(13) Uani 1 1 d . . .
F1 F 0.2143(5) 0.4307(4) 0.3870(6) 0.162(3) Uani 1 1 d . . .
F2 F 0.2810(6) 0.5581(3) 0.3418(5) 0.1235(18) Uani 1 1 d . . .
F3 F 0.2895(5) 0.4637(4) 0.2120(5) 0.1259(19) Uani 1 1 d . . .
F4 F 0.1008(4) 0.5076(3) 0.2518(5) 0.1042(15) Uani 1 1 d . . .
B2 B 0.6918(5) 0.5730(3) 0.7876(4) 0.0384(10) Uani 1 1 d . . .
F5 F 0.7710(5) 0.6001(4) 0.7081(5) 0.130(2) Uani 1 1 d . . .
F6 F 0.7394(5) 0.5010(3) 0.8336(5) 0.1054(15) Uani 1 1 d . . .
F7 F 0.5716(4) 0.5602(3) 0.7281(4) 0.0927(11) Uiso 1 1 d . . .
F8 F 0.6804(7) 0.6257(5) 0.8732(7) 0.156(2) Uiso 1 1 d . . .
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'
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
C2 O1 C1 116.7(4) . . ?
C12 O2 C14 119.6(4) . . ?
C16 O3 C17 110.4(4) . . ?
C19B O4 C18 96.2(8) . . ?
C19B O4 C19A 30.1(7) . . ?
C18 O4 C19A 123.0(8) . . ?
C20B O5 C21 99.6(6) . . ?
C20B O5 C20A 50.3(6) . . ?
C21 O5 C20A 137.5(6) . . ?
C22 O6 C23 118.3(5) . . ?
C24 O7 C25 111.1(4) . . ?
C26 O8 C27 114.6(6) . . ?
C29 O9 C28 109.1(7) . . ?
C15 O10 C30 110.5(5) . . ?
C5 N1 C6 122.8(4) . . ?
C5 N1 C7 118.0(4) . . ?
C6 N1 C7 119.2(4) . . ?
C13 N2 C9 121.6(4) . . ?
C13 N2 C8 119.3(3) . . ?
C9 N2 C8 119.1(3) . . ?
O1 C2 C6 124.9(4) . . ?
O1 C2 C3 116.3(4) . . ?
C6 C2 C3 118.8(4) . . ?
C4 C3 C2 119.9(4) . . ?
C3 C4 C5 119.1(4) . . ?
N1 C5 C4 119.6(4) . . ?
N1 C6 C2 119.7(4) . . ?
N1 C7 C8 108.3(3) . . ?
N2 C8 C7 108.9(3) . . ?
C10 C9 N2 119.7(4) . . ?
C9 C10 C11 121.0(4) . . ?
C12 C11 C10 119.1(4) . . ?
O2 C12 C11 118.6(4) . . ?
O2 C12 C13 122.6(4) . . ?
C11 C12 C13 118.8(4) . . ?
N2 C13 C12 119.8(4) . . ?
O10 C15 C16 112.8(5) . . ?
O3 C16 C15 112.8(5) . . ?
O3 C17 C18 111.2(4) . . ?
O4 C18 C17 109.0(5) . . ?
C22 C21 O5 109.1(6) . . ?
O6 C22 C21 113.9(5) . . ?
O6 C23 C24 112.8(6) . . ?
O7 C24 C23 109.6(5) . . ?
C26 C25 O7 109.4(4) . . ?
O8 C26 C25 110.1(5) . . ?
C28 C27 O8 122.4(7) . . ?
C27 C28 O9 115.3(10) . . ?
C30 C29 O9 111.3(7) . . ?
O10 C30 C29 111.4(5) . . ?
C20A C19A O4 127.7(15) . . ?
C19A C20A O5 129.1(15) . . ?
O4 C19B C20B 130.4(10) . . ?
C19B C20B O5 117.4(8) . . ?
F3 B1 F1 111.8(6) . . ?
F3 B1 F4 111.3(5) . . ?
F1 B1 F4 108.9(5) . . ?
F3 B1 F2 102.8(6) . . ?
F1 B1 F2 115.1(6) . . ?
F4 B1 F2 106.9(5) . . ?
F8 B2 F5 110.4(6) . . ?
F8 B2 F7 106.6(5) . . ?
F5 B2 F7 111.1(5) . . ?
F8 B2 F6 113.1(5) . . ?
F5 B2 F6 107.2(5) . . ?
F7 B2 F6 108.4(4) . . ?
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
O1 C2 1.359(5) . ?
O1 C1 1.447(7) . ?
O2 C12 1.337(5) . ?
O2 C14 1.433(6) . ?
O3 C16 1.415(7) . ?
O3 C17 1.411(6) . ?
O4 C19B 1.373(13) . ?
O4 C18 1.401(8) . ?
O4 C19A 1.526(14) . ?
O5 C20B 1.474(10) . ?
O5 C21 1.452(10) . ?
O5 C20A 1.646(19) . ?
O6 C22 1.403(8) . ?
O6 C23 1.412(8) . ?
O7 C24 1.417(7) . ?
O7 C25 1.448(7) . ?
O8 C26 1.395(9) . ?
O8 C27 1.454(8) . ?
O9 C29 1.427(9) . ?
O9 C28 1.428(9) . ?
O10 C15 1.397(7) . ?
O10 C30 1.400(7) . ?
N1 C5 1.321(6) . ?
N1 C6 1.332(5) . ?
N1 C7 1.496(5) . ?
N2 C13 1.339(5) . ?
N2 C9 1.355(6) . ?
N2 C8 1.460(5) . ?
C2 C6 1.362(6) . ?
C2 C3 1.397(6) . ?
C3 C4 1.356(7) . ?
C4 C5 1.384(7) . ?
C7 C8 1.504(6) . ?
C9 C10 1.339(7) . ?
C10 C11 1.388(7) . ?
C11 C12 1.374(6) . ?
C12 C13 1.400(6) . ?
C15 C16 1.489(9) . ?
C17 C18 1.480(9) . ?
C21 C22 1.445(11) . ?
C23 C24 1.419(10) . ?
C25 C26 1.451(10) . ?
C27 C28 1.300(13) . ?
C29 C30 1.405(10) . ?
C19A C20A 0.857(17) . ?
C19B C20B 1.353(16) . ?
B1 F3 1.314(7) . ?
B1 F1 1.335(7) . ?
B1 F4 1.346(7) . ?
B1 F2 1.378(8) . ?
B2 F8 1.283(9) . ?
B2 F5 1.337(7) . ?
B2 F7 1.364(7) . ?
B2 F6 1.363(7) . ?
