#------------------------------------------------------------------------------
#$Date: 2016-12-29 13:12:14 +0200 (Thu, 29 Dec 2016) $
#$Revision: 189495 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/17/7051706.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_7051706
loop_
_publ_author_name
'Fonari, Marina S.'
'Ganin, Eduard V.'
'Chumakov, Yurii M.'
'Botoshansky, Mark M.'
'Suwinska, Kinga'
'Basok, Stepan S.'
'Simonov, Yurii A.'
_publ_section_title
;
 Conformational mobility of
 7,16-bis(4-methoxybenzyl)-1,4,10,13-tetraoxa-7,16-diazacyclooctadecane
 in molecular and proton-transfer complexes: X-ray and DFT studies
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1646
_journal_paper_doi               10.1039/b902953b
_journal_volume                  33
_journal_year                    2009
_chemical_formula_moiety         'C28 H44 N2 O6, 2(Ta F6), 2(H2 O)'
_chemical_formula_sum            'C28 H48 F12 N2 O8 Ta2'
_chemical_formula_weight         1130.58
_chemical_name_common
;
7,16-bis(4-methoxybenzyl)-1,4,10,13-tetraoxa-7,16-
diazoniacyclooctadecane dihexafluorotantalate dihydrate
;
_chemical_name_systematic
;
7,16-bis(4-methoxybenzyl)-1,4,10,13-tetraoxa-7,16-
diazoniacyclooctadecane dihexafluorotantalate dihydrate
;
_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                105.873(9)
_cell_angle_beta                 101.336(9)
_cell_angle_gamma                106.175(6)
_cell_formula_units_Z            1
_cell_length_a                   6.8062(11)
_cell_length_b                   11.3381(18)
_cell_length_c                   14.098(2)
_cell_measurement_temperature    293(2)
_cell_volume                     960.2(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker CCD diffractometer'
_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  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5444
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    5.797
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.290
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            light-brown
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.751
_refine_diff_density_min         -1.973
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3640
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1169P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1874
_reflns_number_gt                2021
_reflns_number_total             3640
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b902953b.txt
_cod_data_source_block           ych1
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2016-12-29
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051706
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
_atom_site_attached_hydrogens
Ta1 Ta 0.0000 0.0000 0.5000 0.0885(3) Uani 1 2 d S . . 0
Ta2 Ta 0.0000 0.0000 0.0000 0.0870(3) Uani 1 2 d S . . 0
F1 F -0.0128(18) 0.1673(9) 0.5253(7) 0.147(4) Uani 1 1 d . . . 0
F2 F -0.1518(18) -0.0507(10) 0.3609(7) 0.165(4) Uani 1 1 d . . . 0
F3 F 0.2584(15) 0.0583(9) 0.4727(9) 0.167(4) Uani 1 1 d . . . 0
F4 F 0.0768(17) -0.0901(10) -0.1091(7) 0.163(3) Uani 1 1 d . . . 0
F5 F 0.2820(12) 0.0527(7) 0.0858(7) 0.120(2) Uani 1 1 d . . . 0
F6 F 0.0765(15) 0.1525(9) -0.0300(9) 0.156(4) Uani 1 1 d . . . 0
O1 O 0.6328(14) 0.2845(8) 0.8962(6) 0.091(2) Uani 1 1 d . . . 0
O2 O 1.2286(16) 0.5316(9) 0.9010(6) 0.107(3) Uani 1 1 d . . . 0
O3 O 0.2431(14) 0.6530(8) 0.6180(7) 0.102(2) Uani 1 1 d . . . 0
N1 N 0.8471(16) 0.3453(9) 0.7544(7) 0.085(2) Uani 1 1 d D . . 0
H1N1 H 0.85(2) 0.422(6) 0.792(8) 0.127 Uiso 1 1 d D . . 0
C1 C 1.045(2) 0.3124(13) 0.7845(10) 0.110(4) Uani 1 1 d . . . 0
H1A H 1.0496 0.2460 0.7255 0.132 Uiso 1 1 calc R . . 0
H1B H 1.0358 0.2758 0.8389 0.132 Uiso 1 1 calc R . . 0
C2 C 1.250(2) 0.4307(15) 0.8217(10) 0.100(4) Uani 1 1 d . . . 0
H2A H 1.3712 0.4080 0.8483 0.120 Uiso 1 1 calc R . . 0
H2B H 1.2723 0.4603 0.7650 0.120 Uiso 1 1 calc R . . 0
C3 C 1.410(3) 0.6512(15) 0.9374(12) 0.133(6) Uani 1 1 d . . . 0
H3A H 1.4315 0.6794 0.8800 0.160 Uiso 1 1 calc R . . 0
H3B H 1.5376 0.6372 0.9685 0.160 Uiso 1 1 calc R . . 0
C4 C 0.649(2) 0.2300(11) 0.7276(8) 0.098(3) Uani 1 1 d . . . 0
H4A H 0.6488 0.1605 0.6691 0.118 Uiso 1 1 calc R . . 0
H4B H 0.5266 0.2542 0.7058 0.118 Uiso 1 1 calc R . . 0
C5 C 0.621(3) 0.1765(12) 0.8123(10) 0.102(4) Uani 1 1 d . . . 0
H5A H 0.4842 0.1063 0.7908 0.122 Uiso 1 1 calc R . . 0
H5B H 0.7342 0.1431 0.8315 0.122 Uiso 1 1 calc R . . 0
C6 C 0.630(3) 0.2492(13) 0.9871(10) 0.126(5) Uani 1 1 d . . . 0
H6A H 0.7656 0.2421 1.0159 0.152 Uiso 1 1 calc R . . 0
H6B H 0.5178 0.1650 0.9689 0.152 Uiso 1 1 calc R . . 0
C7 C 0.842(2) 0.4039(12) 0.6668(9) 0.094(3) Uani 1 1 d . . . 0
H7A H 0.9826 0.4673 0.6801 0.113 Uiso 1 1 calc R . . 0
H7B H 0.8114 0.3343 0.6020 0.113 Uiso 1 1 calc R . . 0
C8 C 0.6795(19) 0.4694(12) 0.6558(8) 0.076(3) Uani 1 1 d . . . 0
C9 C 0.4770(19) 0.4044(10) 0.5880(8) 0.077(3) Uani 1 1 d . . . 0
H9A H 0.4343 0.3159 0.5495 0.092 Uiso 1 1 calc R . . 0
C10 C 0.3390(18) 0.4702(10) 0.5774(8) 0.077(3) Uani 1 1 d . . . 0
H10A H 0.2031 0.4263 0.5304 0.092 Uiso 1 1 calc R . . 0
C11 C 0.3967(18) 0.5984(10) 0.6343(8) 0.077(3) Uani 1 1 d . . . 0
C12 C 0.6009(19) 0.6643(10) 0.7021(8) 0.083(3) Uani 1 1 d . . . 0
H12A H 0.6439 0.7526 0.7414 0.100 Uiso 1 1 calc R . . 0
C13 C 0.738(2) 0.5974(12) 0.7105(9) 0.084(3) Uani 1 1 d . . . 0
H13A H 0.8766 0.6416 0.7554 0.101 Uiso 1 1 calc R . . 0
C14 C 0.300(3) 0.7884(14) 0.6775(13) 0.134(6) Uani 1 1 d . . . 0
H14A H 0.1892 0.8193 0.6534 0.202 Uiso 1 1 calc R . . 0
H14B H 0.4321 0.8382 0.6702 0.202 Uiso 1 1 calc R . . 0
H14C H 0.3177 0.7984 0.7489 0.202 Uiso 1 1 calc R . . 0
O1W O 0.836(5) 0.549(3) 0.924(2) 0.047(10) Uiso 0.167(16) 1 d P . . 2
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'
Ta Ta -0.7052 6.5227 '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
F3 Ta1 F3 180.000(1) 2_556 . ?
F3 Ta1 F1 90.9(4) 2_556 . ?
F3 Ta1 F1 89.1(4) . . ?
F3 Ta1 F1 89.1(4) 2_556 2_556 ?
F3 Ta1 F1 90.9(4) . 2_556 ?
F1 Ta1 F1 180.000(2) . 2_556 ?
F3 Ta1 F2 91.3(5) 2_556 2_556 ?
F3 Ta1 F2 88.7(5) . 2_556 ?
F1 Ta1 F2 89.1(4) . 2_556 ?
F1 Ta1 F2 90.9(4) 2_556 2_556 ?
F3 Ta1 F2 88.7(5) 2_556 . ?
F3 Ta1 F2 91.3(5) . . ?
F1 Ta1 F2 90.9(4) . . ?
F1 Ta1 F2 89.1(4) 2_556 . ?
F2 Ta1 F2 180.000(2) 2_556 . ?
F6 Ta2 F6 180.0(9) 2 . ?
F6 Ta2 F4 92.3(5) 2 2 ?
F6 Ta2 F4 87.7(5) . 2 ?
F6 Ta2 F4 87.7(5) 2 . ?
F6 Ta2 F4 92.3(5) . . ?
F4 Ta2 F4 180.0(6) 2 . ?
F6 Ta2 F5 90.7(4) 2 . ?
F6 Ta2 F5 89.3(4) . . ?
F4 Ta2 F5 90.6(4) 2 . ?
F4 Ta2 F5 89.4(4) . . ?
F6 Ta2 F5 89.3(4) 2 2 ?
F6 Ta2 F5 90.7(4) . 2 ?
F4 Ta2 F5 89.4(4) 2 2 ?
F4 Ta2 F5 90.6(4) . 2 ?
F5 Ta2 F5 180.0(6) . 2 ?
C5 O1 C6 110.7(9) . . ?
C2 O2 C3 112.3(11) . . ?
C11 O3 C14 116.5(11) . . ?
C4 N1 C1 111.1(9) . . ?
C4 N1 C7 110.8(9) . . ?
C1 N1 C7 113.9(9) . . ?
C4 N1 H1N1 117(8) . . ?
C1 N1 H1N1 117(9) . . ?
C7 N1 H1N1 84(8) . . ?
N1 C1 C2 112.7(10) . . ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
O2 C2 C1 107.8(11) . . ?
O2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
O2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.5 . . ?
O2 C3 C6 109.0(12) . 2_767 ?
O2 C3 H3A 109.9 . . ?
C6 C3 H3A 109.9 2_767 . ?
O2 C3 H3B 109.9 . . ?
C6 C3 H3B 109.9 2_767 . ?
H3A C3 H3B 108.3 . . ?
N1 C4 C5 115.7(11) . . ?
N1 C4 H4A 108.4 . . ?
C5 C4 H4A 108.4 . . ?
N1 C4 H4B 108.4 . . ?
C5 C4 H4B 108.4 . . ?
H4A C4 H4B 107.4 . . ?
O1 C5 C4 105.1(9) . . ?
O1 C5 H5A 110.7 . . ?
C4 C5 H5A 110.7 . . ?
O1 C5 H5B 110.7 . . ?
C4 C5 H5B 110.7 . . ?
H5A C5 H5B 108.8 . . ?
O1 C6 C3 109.1(11) . 2_767 ?
O1 C6 H6A 109.9 . . ?
C3 C6 H6A 109.9 2_767 . ?
O1 C6 H6B 109.9 . . ?
C3 C6 H6B 109.9 2_767 . ?
H6A C6 H6B 108.3 . . ?
C8 C7 N1 114.0(8) . . ?
C8 C7 H7A 108.8 . . ?
N1 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
N1 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C13 C8 C9 119.2(11) . . ?
C13 C8 C7 118.6(12) . . ?
C9 C8 C7 122.1(11) . . ?
C10 C9 C8 119.8(10) . . ?
C10 C9 H9A 120.1 . . ?
C8 C9 H9A 120.1 . . ?
C11 C10 C9 121.0(11) . . ?
C11 C10 H10A 119.5 . . ?
C9 C10 H10A 119.5 . . ?
C10 C11 O3 115.6(10) . . ?
C10 C11 C12 119.3(10) . . ?
O3 C11 C12 125.1(10) . . ?
C13 C12 C11 118.9(10) . . ?
C13 C12 H12A 120.6 . . ?
C11 C12 H12A 120.6 . . ?
C8 C13 C12 121.7(12) . . ?
C8 C13 H13A 119.1 . . ?
C12 C13 H13A 119.1 . . ?
O3 C14 H14A 109.5 . . ?
O3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
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
Ta1 F3 1.854(8) 2_556 ?
Ta1 F3 1.854(8) . ?
Ta1 F1 1.862(8) . ?
Ta1 F1 1.862(8) 2_556 ?
Ta1 F2 1.871(9) 2_556 ?
Ta1 F2 1.871(9) . ?
Ta2 F6 1.850(8) 2 ?
Ta2 F6 1.850(8) . ?
Ta2 F4 1.854(8) 2 ?
Ta2 F4 1.854(8) . ?
Ta2 F5 1.886(7) . ?
Ta2 F5 1.886(7) 2 ?
O1 C5 1.423(14) . ?
O1 C6 1.446(13) . ?
O2 C2 1.426(15) . ?
O2 C3 1.435(16) . ?
O3 C11 1.369(12) . ?
O3 C14 1.430(16) . ?
N1 C4 1.488(15) . ?
N1 C1 1.507(13) . ?
N1 C7 1.553(12) . ?
N1 H1N1 0.88(2) . ?
C1 C2 1.519(19) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C6 1.450(18) 2_767 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.500(16) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C3 1.450(18) 2_767 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.500(14) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C13 1.343(16) . ?
C8 C9 1.374(15) . ?
C9 C10 1.362(13) . ?
C9 H9A 0.9300 . ?
C10 C11 1.353(13) . ?
C10 H10A 0.9300 . ?
C11 C12 1.383(14) . ?
C12 C13 1.367(15) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
