#------------------------------------------------------------------------------
#$Date: 2025-08-21 22:04:39 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301851 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/21/7052122.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_7052122
loop_
_publ_author_name
'Mezei, Gellert'
'Kampf, Jeff W.'
'Pecoraro, Vincent L.'
_publ_section_title
;
 Temperature-, molar ratio- and counterion-effects on the crystal
 growth of bipyridinium-bis(alkylcarboxylic acid)?crown ether
 pseudorotaxanes
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              439
_journal_paper_doi               10.1039/b615273b
_journal_volume                  31
_journal_year                    2007
_chemical_formula_moiety
;
C36 H44 O10, C18 H22 N2 O4, 2(F6 P), 4(C2 H3 N)
;
_chemical_formula_sum            'C62 H78 F12 N6 O14 P2'
_chemical_formula_weight         1421.24
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.769(6)
_cell_angle_beta                 110.295(6)
_cell_angle_gamma                109.052(6)
_cell_formula_units_Z            1
_cell_length_a                   11.7067(11)
_cell_length_b                   12.1212(11)
_cell_length_c                   13.9127(13)
_cell_measurement_reflns_used    5755
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      2.43
_cell_volume                     1706.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-1K'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32530
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  0.9871
_exptl_absorpt_correction_T_min  0.9651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Blessing, R. Acta Cryst. (1995) A51 33-38.
Sheldrick, G. SADABS (Version 2.10) Bruker/Siemens area
detector absorption and other corrections, University of
Gottingen, Germany 2003.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0508
_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)+(0.0478P)²+0.9117P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                4452
_reflns_number_total             6965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b615273b.txt
_cod_data_source_block           Pseudorotaxane_Ic(gm13)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7052122
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
P1 P 0.66958(7) 0.36237(7) 0.50495(5) 0.0376(2) Uani 1 1 d . . .
F1 F 0.63352(18) 0.23907(15) 0.42939(12) 0.0566(5) Uani 1 1 d . . .
F2 F 0.58623(19) 0.29328(16) 0.56627(14) 0.0620(5) Uani 1 1 d . . .
F3 F 0.75417(19) 0.43093(17) 0.44418(14) 0.0691(6) Uani 1 1 d . . .
F4 F 0.54413(19) 0.3777(2) 0.42525(14) 0.0726(6) Uani 1 1 d . . .
F5 F 0.79390(19) 0.3428(2) 0.58429(14) 0.0841(7) Uani 1 1 d . . .
F6 F 0.7080(2) 0.48639(16) 0.58092(14) 0.0733(6) Uani 1 1 d . . .
N1 N 0.91499(18) 0.39799(17) 0.20391(15) 0.0258(5) Uani 1 1 d . . .
N2 N 0.1964(3) 0.8647(2) 0.19287(19) 0.0482(6) Uani 1 1 d . . .
N3 N 0.6969(3) 0.8936(3) 0.3914(2) 0.0753(9) Uani 1 1 d . . .
O1 O 0.9677(2) 0.12287(19) 0.55509(14) 0.0456(5) Uani 1 1 d . . .
H1 H 0.990(3) 0.053(3) 0.573(3) 0.085(12) Uiso 1 1 d . . .
O2 O 0.99805(19) 0.07772(17) 0.40746(14) 0.0419(5) Uani 1 1 d . . .
O3 O 0.74001(15) 0.03117(13) 0.08103(12) 0.0260(4) Uani 1 1 d . . .
O4 O 0.61198(15) 0.11707(13) 0.18989(12) 0.0265(4) Uani 1 1 d . . .
O5 O 0.55644(16) 0.29899(14) 0.09535(12) 0.0281(4) Uani 1 1 d . . .
O6 O 0.76819(15) 0.67616(13) -0.11783(12) 0.0250(4) Uani 1 1 d . . .
O7 O 0.97554(15) 0.86374(14) -0.13689(13) 0.0281(4) Uani 1 1 d . . .
C1 C 0.9673(3) 0.1390(2) 0.4613(2) 0.0365(6) Uani 1 1 d . . .
C2 C 0.9229(3) 0.2361(3) 0.4276(2) 0.0399(7) Uani 1 1 d . . .
H2A H 0.9581 0.3022 0.4896 0.048 Uiso 1 1 calc R . .
H2B H 0.8256 0.2053 0.4007 0.048 Uiso 1 1 calc R . .
C3 C 0.9654(3) 0.2853(2) 0.3433(2) 0.0341(6) Uani 1 1 d . . .
H3A H 1.0594 0.3395 0.3752 0.041 Uiso 1 1 calc R . .
H3B H 0.9549 0.2187 0.2904 0.041 Uiso 1 1 calc R . .
C4 C 0.8821(2) 0.3529(2) 0.2909(2) 0.0314(6) Uani 1 1 d . . .
H4A H 0.7880 0.2994 0.2628 0.038 Uiso 1 1 calc R . .
H4B H 0.8961 0.4212 0.3437 0.038 Uiso 1 1 calc R . .
C5 C 0.8816(2) 0.3187(2) 0.11521(19) 0.0284(6) Uani 1 1 d . . .
H5A H 0.8350 0.2360 0.1085 0.034 Uiso 1 1 calc R . .
C6 C 0.9146(2) 0.3565(2) 0.03464(19) 0.0288(6) Uani 1 1 d . . .
H6A H 0.8917 0.2998 -0.0270 0.035 Uiso 1 1 calc R . .
C7 C 0.9818(2) 0.4785(2) 0.04291(17) 0.0241(5) Uani 1 1 d . . .
C8 C 1.0118(2) 0.5576(2) 0.13515(19) 0.0313(6) Uani 1 1 d . . .
H8A H 1.0560 0.6410 0.1433 0.038 Uiso 1 1 calc R . .
C9 C 0.9781(2) 0.5159(2) 0.2137(2) 0.0314(6) Uani 1 1 d . . .
H9A H 0.9994 0.5708 0.2760 0.038 Uiso 1 1 calc R . .
C10 C 0.8157(2) -0.0174(2) 0.04201(19) 0.0292(6) Uani 1 1 d . . .
H10A H 0.8199 0.0135 -0.0208 0.035 Uiso 1 1 calc R . .
H10B H 0.7692 -0.1055 0.0194 0.035 Uiso 1 1 calc R . .
C11 C 0.7021(2) -0.0260(2) 0.15742(19) 0.0295(6) Uani 1 1 d . . .
H11A H 0.7746 0.0087 0.2279 0.035 Uiso 1 1 calc R . .
H11B H 0.6832 -0.1127 0.1397 0.035 Uiso 1 1 calc R . .
C12 C 0.5809(2) -0.0075(2) 0.15765(19) 0.0270(5) Uani 1 1 d . . .
H12A H 0.5098 -0.0392 0.0863 0.032 Uiso 1 1 calc R . .
H12B H 0.5496 -0.0511 0.2064 0.032 Uiso 1 1 calc R . .
C13 C 0.4971(2) 0.1414(2) 0.17895(19) 0.0272(5) Uani 1 1 d . . .
H13A H 0.4677 0.1167 0.2353 0.033 Uiso 1 1 calc R . .
H13B H 0.4249 0.0955 0.1103 0.033 Uiso 1 1 calc R . .
C14 C 0.5293(2) 0.2733(2) 0.18596(18) 0.0264(5) Uani 1 1 d . . .
H14A H 0.4539 0.2937 0.1858 0.032 Uiso 1 1 calc R . .
H14B H 0.6070 0.3202 0.2513 0.032 Uiso 1 1 calc R . .
C15 C 0.6151(2) 0.4161(2) 0.09226(17) 0.0228(5) Uani 1 1 d . . .
C16 C 0.6539(2) 0.5134(2) 0.17104(18) 0.0273(6) Uani 1 1 d . . .
H16A H 0.6380 0.5030 0.2328 0.033 Uiso 1 1 calc R . .
C17 C 0.7176(2) 0.6289(2) 0.15899(19) 0.0289(6) Uani 1 1 d . . .
H17A H 0.7463 0.6961 0.2140 0.035 Uiso 1 1 calc R . .
C18 C 0.7391(2) 0.6464(2) 0.06982(18) 0.0254(5) Uani 1 1 d . . .
H18A H 0.7826 0.7251 0.0638 0.031 Uiso 1 1 calc R . .
C19 C 0.6967(2) 0.5474(2) -0.01369(17) 0.0218(5) Uani 1 1 d . . .
C20 C 0.7119(2) 0.5598(2) -0.11066(17) 0.0221(5) Uani 1 1 d . . .
C21 C 0.6721(2) 0.4611(2) -0.18860(18) 0.0264(5) Uani 1 1 d . . .
H21A H 0.6831 0.4709 -0.2523 0.032 Uiso 1 1 calc R . .
C22 C 0.6150(2) 0.3457(2) -0.17373(18) 0.0267(5) Uani 1 1 d . . .
H22A H 0.5890 0.2779 -0.2274 0.032 Uiso 1 1 calc R . .
C23 C 0.5962(2) 0.3292(2) -0.08349(17) 0.0248(5) Uani 1 1 d . . .
H23A H 0.5571 0.2506 -0.0751 0.030 Uiso 1 1 calc R . .
C24 C 0.6351(2) 0.4294(2) -0.00227(17) 0.0209(5) Uani 1 1 d . . .
C25 C 0.7774(2) 0.6929(2) -0.21654(17) 0.0258(5) Uani 1 1 d . . .
H25A H 0.6884 0.6601 -0.2740 0.031 Uiso 1 1 calc R . .
H25B H 0.8304 0.6505 -0.2323 0.031 Uiso 1 1 calc R . .
C26 C 0.8414(2) 0.8241(2) -0.20813(18) 0.0268(5) Uani 1 1 d . . .
H26A H 0.8361 0.8397 -0.2780 0.032 Uiso 1 1 calc R . .
H26B H 0.7959 0.8678 -0.1821 0.032 Uiso 1 1 calc R . .
C27 C 1.0458(2) 0.9892(2) -0.11976(19) 0.0272(5) Uani 1 1 d . . .
H27A H 1.0036 1.0346 -0.0913 0.033 Uiso 1 1 calc R . .
H27B H 1.0466 1.0111 -0.1866 0.033 Uiso 1 1 calc R . .
C28 C 0.2597(3) 0.9052(2) 0.2792(2) 0.0399(7) Uani 1 1 d . . .
C29 C 0.3407(4) 0.9577(3) 0.3899(2) 0.0756(12) Uani 1 1 d . . .
H29A H 0.3784 1.0450 0.4007 0.113 Uiso 1 1 calc R . .
H29B H 0.4118 0.9277 0.4131 0.113 Uiso 1 1 calc R . .
H29C H 0.2865 0.9357 0.4307 0.113 Uiso 1 1 calc R . .
C30 C 0.6869(3) 0.8018(3) 0.4110(2) 0.0484(8) Uani 1 1 d . . .
C31 C 0.6728(3) 0.6845(3) 0.4344(2) 0.0539(8) Uani 1 1 d . . .
H31A H 0.5896 0.6243 0.3828 0.081 Uiso 1 1 calc R . .
H31B H 0.6731 0.6855 0.5050 0.081 Uiso 1 1 calc R . .
H31C H 0.7463 0.6645 0.4312 0.081 Uiso 1 1 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 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'
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'
P P 0.1023 0.0942 '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
F4 P1 F1 90.07(11) . . ?
F4 P1 F6 90.58(12) . . ?
F1 P1 F6 179.13(11) . . ?
F4 P1 F2 90.96(11) . . ?
F1 P1 F2 90.51(10) . . ?
F6 P1 F2 90.06(10) . . ?
F4 P1 F3 89.64(11) . . ?
F1 P1 F3 89.29(10) . . ?
F6 P1 F3 90.13(10) . . ?
F2 P1 F3 179.37(12) . . ?
F4 P1 F5 178.36(13) . . ?
F1 P1 F5 88.52(11) . . ?
F6 P1 F5 90.83(12) . . ?
F2 P1 F5 88.22(11) . . ?
F3 P1 F5 91.18(12) . . ?
C9 N1 C5 120.5(2) . . ?
C9 N1 C4 120.6(2) . . ?
C5 N1 C4 118.9(2) . . ?
C10 O3 C11 114.05(17) . . ?
C12 O4 C13 111.67(17) . . ?
C15 O5 C14 118.87(17) . . ?
C20 O6 C25 116.38(17) . . ?
C26 O7 C27 113.25(17) . . ?
O2 C1 O1 123.2(2) . . ?
O2 C1 C2 123.6(2) . . ?
O1 C1 C2 113.2(2) . . ?
C1 C2 C3 113.8(2) . . ?
C4 C3 C2 109.3(2) . . ?
N1 C4 C3 111.69(19) . . ?
N1 C5 C6 120.5(2) . . ?
C5 C6 C7 120.3(2) . . ?
C8 C7 C6 117.1(2) . . ?
C8 C7 C7 121.5(3) . 2_765 ?
C6 C7 C7 121.4(3) . 2_765 ?
C9 C8 C7 120.6(2) . . ?
N1 C9 C8 120.8(2) . . ?
O3 C10 C27 114.71(19) . 2_765 ?
O3 C11 C12 108.68(19) . . ?
O4 C12 C11 109.27(18) . . ?
O4 C13 C14 108.96(19) . . ?
O5 C14 C13 106.35(18) . . ?
O5 C15 C16 125.1(2) . . ?
O5 C15 C24 113.32(19) . . ?
C16 C15 C24 121.6(2) . . ?
C15 C16 C17 119.1(2) . . ?
C18 C17 C16 121.6(2) . . ?
C17 C18 C19 120.3(2) . . ?
C18 C19 C24 119.3(2) . . ?
C18 C19 C20 123.1(2) . . ?
C24 C19 C20 117.60(19) . . ?
C21 C20 O6 124.2(2) . . ?
C21 C20 C19 121.2(2) . . ?
O6 C20 C19 114.62(18) . . ?
C20 C21 C22 119.8(2) . . ?
C23 C22 C21 121.3(2) . . ?
C22 C23 C24 120.1(2) . . ?
C23 C24 C15 121.8(2) . . ?
C23 C24 C19 120.0(2) . . ?
C15 C24 C19 118.21(19) . . ?
O6 C25 C26 108.10(18) . . ?
O7 C26 C25 108.23(18) . . ?
O7 C27 C10 106.98(18) . 2_765 ?
N2 C28 C29 179.8(4) . . ?
N3 C30 C31 179.3(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
P1 F4 1.5825(19) . ?
P1 F1 1.5926(17) . ?
P1 F6 1.5949(18) . ?
P1 F2 1.5950(18) . ?
P1 F3 1.5958(18) . ?
P1 F5 1.596(2) . ?
N1 C9 1.348(3) . ?
N1 C5 1.350(3) . ?
N1 C4 1.485(3) . ?
N2 C28 1.131(3) . ?
N3 C30 1.146(4) . ?
O1 C1 1.335(3) . ?
O2 C1 1.229(3) . ?
O3 C10 1.431(3) . ?
O3 C11 1.434(3) . ?
O4 C12 1.424(3) . ?
O4 C13 1.430(3) . ?
O5 C15 1.372(3) . ?
O5 C14 1.437(3) . ?
O6 C20 1.377(3) . ?
O6 C25 1.440(3) . ?
O7 C26 1.424(3) . ?
O7 C27 1.426(3) . ?
C1 C2 1.481(4) . ?
C2 C3 1.520(3) . ?
C3 C4 1.510(3) . ?
C5 C6 1.373(3) . ?
C6 C7 1.403(3) . ?
C7 C8 1.397(3) . ?
C7 C7 1.480(5) 2_765 ?
C8 C9 1.366(3) . ?
C10 C27 1.509(3) 2_765 ?
C11 C12 1.508(3) . ?
C13 C14 1.505(3) . ?
C15 C16 1.374(3) . ?
C15 C24 1.426(3) . ?
C16 C17 1.410(3) . ?
C17 C18 1.369(3) . ?
C18 C19 1.420(3) . ?
C19 C24 1.426(3) . ?
C19 C20 1.434(3) . ?
C20 C21 1.376(3) . ?
C21 C22 1.407(3) . ?
C22 C23 1.367(3) . ?
C23 C24 1.419(3) . ?
C25 C26 1.496(3) . ?
C27 C10 1.509(3) 2_765 ?
C28 C29 1.451(4) . ?
C30 C31 1.455(5) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O2 0.99(4) 1.67(4) 2.654(3) 171(3) 2_756
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139175783
