#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/32/7003246.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_7003246
loop_
_publ_author_name
'Singh, Ashutosh S.'
'Bharadwaj, Parimal K.'
_publ_section_title
;
 Binding of HgCl2 by tripodal ligands controlled by AgPF6: receptors
 for the PF6− anion
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              738
_journal_page_last               741
_journal_paper_doi               10.1039/b714654j
_journal_year                    2008
_chemical_formula_moiety         '2(C27 H25 N4 O3), F8 P, F6 P'
_chemical_formula_sum            'C54 H50 F14 N8 O6 P2'
_chemical_formula_weight         1234.96
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.3330(17)
_cell_length_b                   13.3330(17)
_cell_length_c                   26.773(4)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      +28.0
_cell_measurement_theta_min      2.11
_cell_volume                     4121.8(10)
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 ( Bruker, 2003)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       phi-omega
_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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            6983
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_T_max  0.9745
_exptl_absorpt_correction_T_min  0.9586
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1902
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.0006(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0701P)²+15.5923P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1548
_reflns_number_gt                1344
_reflns_number_total             1564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b714654j.txt
_cod_data_source_block           Compound6.CIF
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C54 H50 F14 N8 O6 P2 '
_cod_database_code               7003246
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.6667 0.3333 0.8333 0.0141(5) Uani 1 6 d S . .
P2 P 0.0000 0.0000 0.0000 0.0487(7) Uani 1 6 d S . .
F1 F 0.55617(14) 0.25736(15) 0.86784(6) 0.0260(5) Uani 1 1 d . . .
F2 F 0.0000 0.0000 -0.05923(15) 0.0677(13) Uani 1 3 d S . .
F3 F -0.049(5) 0.080(4) 0.0012(3) 0.245(7) Uani 1 1 d . . .
O1 O 0.06667(17) 0.17328(17) 0.74760(7) 0.0200(5) Uani 1 1 d . . .
N1 N 0.0000 0.0000 0.68028(14) 0.0154(9) Uani 1 3 d S . .
H1N H 0.0000 0.0000 0.7138 0.020 Uiso 1 3 d S . .
N2 N -0.0235(2) 0.4288(2) 0.94441(10) 0.0272(7) Uani 1 1 d . . .
C1 C 0.0776(2) 0.1237(2) 0.66464(10) 0.0176(7) Uani 1 1 d . . .
H1A H 0.0624 0.1334 0.6293 0.021 Uiso 1 1 calc R . .
H1B H 0.1596 0.1438 0.6676 0.021 Uiso 1 1 calc R . .
C2 C 0.0561(3) 0.2035(3) 0.69725(10) 0.0192(7) Uani 1 1 d . . .
H2B H 0.1139 0.2855 0.6904 0.023 Uiso 1 1 calc R . .
H2A H -0.0223 0.1918 0.6912 0.023 Uiso 1 1 calc R . .
C3 C 0.0398(2) 0.2249(2) 0.78550(10) 0.0170(6) Uani 1 1 d . . .
C4 C 0.0124(2) 0.3117(3) 0.77835(11) 0.0206(7) Uani 1 1 d . . .
H4 H 0.0079 0.3365 0.7456 0.025 Uiso 1 1 calc R . .
C5 C -0.0082(2) 0.3616(3) 0.81957(11) 0.0207(7) Uani 1 1 d . . .
H5 H -0.0266 0.4212 0.8152 0.025 Uiso 1 1 calc R . .
C6 C -0.0020(2) 0.3244(2) 0.86733(10) 0.0192(7) Uani 1 1 d . . .
C7 C 0.0230(2) 0.2354(2) 0.87419(11) 0.0193(7) Uani 1 1 d . . .
H7 H 0.0259 0.2092 0.9069 0.023 Uiso 1 1 calc R . .
C8 C 0.0434(2) 0.1859(2) 0.83325(10) 0.0183(7) Uani 1 1 d . . .
H8 H 0.0599 0.1249 0.8376 0.022 Uiso 1 1 calc R . .
C9 C -0.0156(2) 0.3817(3) 0.91012(12) 0.0207(7) Uani 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'
P P 0.1023 0.0942 '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'
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'
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
F1 P1 F1 180.00(11) 17_556 2_655 ?
F1 P1 F1 90.04(9) 17_556 . ?
F1 P1 F1 89.96(9) 2_655 . ?
F1 P1 F1 90.04(9) 17_556 3_665 ?
F1 P1 F1 89.96(9) 2_655 3_665 ?
F1 P1 F1 89.96(9) . 3_665 ?
F1 P1 F1 89.96(9) 17_556 16_656 ?
F1 P1 F1 90.04(9) 2_655 16_656 ?
F1 P1 F1 180.00(10) . 16_656 ?
F1 P1 F1 90.04(9) 3_665 16_656 ?
F1 P1 F1 89.96(9) 17_556 18_546 ?
F1 P1 F1 90.04(9) 2_655 18_546 ?
F1 P1 F1 90.04(9) . 18_546 ?
F1 P1 F1 180.00(9) 3_665 18_546 ?
F1 P1 F1 89.96(9) 16_656 18_546 ?
F3 P2 F3 119.95(3) 3 2 ?
F3 P2 F3 60.05(3) 3 11 ?
F3 P2 F3 180.0(5) 2 11 ?
F3 P2 F3 119.95(3) 3 . ?
F3 P2 F3 119.95(3) 2 . ?
F3 P2 F3 60.05(3) 11 . ?
F3 P2 F3 60.05(3) 3 10 ?
F3 P2 F3 60.05(3) 2 10 ?
F3 P2 F3 119.95(3) 11 10 ?
F3 P2 F3 180.0(13) . 10 ?
F3 P2 F3 180(4) 3 12 ?
F3 P2 F3 60.05(3) 2 12 ?
F3 P2 F3 119.95(3) 11 12 ?
F3 P2 F3 60.05(3) . 12 ?
F3 P2 F3 119.95(3) 10 12 ?
F3 P2 F2 91.3(3) 3 . ?
F3 P2 F2 91.3(3) 2 . ?
F3 P2 F2 88.7(3) 11 . ?
F3 P2 F2 91.3(3) . . ?
F3 P2 F2 88.7(3) 10 . ?
F3 P2 F2 88.7(3) 12 . ?
F3 P2 F2 88.7(3) 3 10 ?
F3 P2 F2 88.7(3) 2 10 ?
F3 P2 F2 91.3(3) 11 10 ?
F3 P2 F2 88.7(3) . 10 ?
F3 P2 F2 91.3(3) 10 10 ?
F3 P2 F2 91.3(3) 12 10 ?
F2 P2 F2 180.0 . 10 ?
P2 F3 F3 59.976(14) . 11 ?
P2 F3 F3 59.976(14) . 12 ?
F3 F3 F3 119.81(11) 11 12 ?
C3 O1 C2 117.9(2) . . ?
C1 N1 C1 112.56(15) 2 . ?
C1 N1 C1 112.56(15) 2 3 ?
C1 N1 C1 112.56(15) . 3 ?
C1 N1 H1N 106.2 2 . ?
C1 N1 H1N 106.2 . . ?
C1 N1 H1N 106.2 3 . ?
N1 C1 C2 110.1(2) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.2 . . ?
O1 C2 C1 105.4(2) . . ?
O1 C2 H2B 110.7 . . ?
C1 C2 H2B 110.7 . . ?
O1 C2 H2A 110.7 . . ?
C1 C2 H2A 110.7 . . ?
H2B C2 H2A 108.8 . . ?
O1 C3 C8 115.3(2) . . ?
O1 C3 C4 124.0(3) . . ?
C8 C3 C4 120.7(3) . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 120.1(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C7 120.4(3) . . ?
C5 C6 C9 119.9(3) . . ?
C7 C6 C9 119.6(3) . . ?
C8 C7 C6 119.5(3) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 C3 120.1(3) . . ?
C7 C8 H8 119.9 . . ?
C3 C8 H8 119.9 . . ?
N2 C9 C6 178.3(3) . . ?
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 F1 1.5993(16) 17_556 ?
P1 F1 1.5993(16) 2_655 ?
P1 F1 1.5993(17) . ?
P1 F1 1.5993(16) 3_665 ?
P1 F1 1.5993(17) 16_656 ?
P1 F1 1.5994(16) 18_546 ?
P2 F3 1.504(7) 3 ?
P2 F3 1.504(7) 2 ?
P2 F3 1.504(7) 11 ?
P2 F3 1.504(7) . ?
P2 F3 1.504(7) 10 ?
P2 F3 1.504(7) 12 ?
P2 F2 1.586(4) . ?
P2 F2 1.586(4) 10 ?
F3 F3 1.506(7) 11 ?
F3 F3 1.506(7) 12 ?
O1 C3 1.370(3) . ?
O1 C2 1.434(3) . ?
N1 C1 1.503(3) 2 ?
N1 C1 1.503(3) . ?
N1 C1 1.503(3) 3 ?
N1 H1N 0.8975 . ?
N2 C9 1.146(4) . ?
C1 C2 1.511(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2B 0.9900 . ?
C2 H2A 0.9900 . ?
C3 C8 1.390(4) . ?
C3 C4 1.390(4) . ?
C4 C5 1.385(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.397(4) . ?
C6 C9 1.438(4) . ?
C7 C8 1.375(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F3 P2 F3 F3 4.4(12) 3 . . 11 ?
F3 P2 F3 F3 180.0 2 . . 11 ?
F3 P2 F3 F3 101(19) 10 . . 11 ?
F3 P2 F3 F3 -175.6(12) 12 . . 11 ?
F2 P2 F3 F3 -87.8(6) . . . 11 ?
F2 P2 F3 F3 92.2(6) 10 . . 11 ?
F3 P2 F3 F3 180.0 3 . . 12 ?
F3 P2 F3 F3 -4.4(12) 2 . . 12 ?
F3 P2 F3 F3 175.6(12) 11 . . 12 ?
F3 P2 F3 F3 -84(19) 10 . . 12 ?
F2 P2 F3 F3 87.8(6) . . . 12 ?
F2 P2 F3 F3 -92.2(6) 10 . . 12 ?
C1 N1 C1 C2 74.0(4) 2 . . . ?
C1 N1 C1 C2 -157.5(2) 3 . . . ?
C3 O1 C2 C1 -173.7(2) . . . . ?
N1 C1 C2 O1 52.6(3) . . . . ?
C2 O1 C3 C8 175.4(2) . . . . ?
C2 O1 C3 C4 -5.6(4) . . . . ?
O1 C3 C4 C5 -177.1(3) . . . . ?
C8 C3 C4 C5 1.8(4) . . . . ?
C3 C4 C5 C6 -0.3(4) . . . . ?
C4 C5 C6 C7 -1.1(4) . . . . ?
C4 C5 C6 C9 175.7(3) . . . . ?
C5 C6 C7 C8 1.1(4) . . . . ?
C9 C6 C7 C8 -175.8(3) . . . . ?
C6 C7 C8 C3 0.5(4) . . . . ?
O1 C3 C8 C7 177.1(2) . . . . ?
C4 C3 C8 C7 -1.9(4) . . . . ?
C5 C6 C9 N2 -103(11) . . . . ?
C7 C6 C9 N2 74(11) . . . . ?
