#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:17:09 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180070 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/16/7051649.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_7051649
loop_
_publ_author_name
'Ulrich, Sébastien'
'Buhler, Eric'
'Lehn, Jean-Marie'
_publ_section_title
;
 Reversible constitutional switching between macrocycles and polymers
 induced by shape change in a dynamic covalent system
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              271
_journal_paper_doi               10.1039/b817261g
_journal_volume                  33
_journal_year                    2009
_chemical_formula_sum            'C16 H12 F6 N4 O8 Pb S2'
_chemical_formula_weight         773.61
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 110.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5365(19)
_cell_length_b                   12.446(3)
_cell_length_c                   10.605(2)
_cell_measurement_reflns_used    10711
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1178.9(5)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       'phi&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  0.0718
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12942
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    7.431
_exptl_absorpt_correction_T_max  0.1640
_exptl_absorpt_correction_T_min  0.0754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   wingx
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.179
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.042
_refine_diff_density_min         -2.450
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0429
_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)+(0.0713P)²+0.4477P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                2281
_reflns_number_total             2709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b817261g.txt
_cod_data_source_block           su25
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        1178.9(4)
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               7051649
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
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
C1 C -0.0719(10) 0.7604(6) 0.1651(8) 0.0616(18) Uani 1 1 d . . .
C2 C -0.0435(8) 0.3793(6) 0.3653(7) 0.0472(15) Uani 1 1 d . . .
H2 H -0.0398 0.4555 0.3615 0.057 Uiso 1 1 calc R . .
C3 C -0.1432(8) 0.3327(6) 0.4165(6) 0.0497(15) Uani 1 1 d . . .
H3 H -0.2081 0.3754 0.4464 0.060 Uiso 1 1 calc R . .
C4 C -0.1459(7) 0.2222(6) 0.4232(6) 0.0472(14) Uani 1 1 d . . .
C5 C -0.2500(10) 0.1664(9) 0.4806(9) 0.072(2) Uani 1 1 d . . .
H5 H -0.3139 0.2095 0.5111 0.087 Uiso 1 1 calc R . .
C6 C -0.0518(7) 0.1616(6) 0.3779(6) 0.0460(14) Uani 1 1 d . A .
H6 H -0.0534 0.0854 0.3815 0.055 Uiso 1 1 calc R . .
C7 C 0.0450(6) 0.2143(5) 0.3270(6) 0.0410(13) Uani 1 1 d . . .
F1 F 0.0554(8) 0.8109(5) 0.1843(8) 0.120(3) Uani 1 1 d . . .
F2 F -0.0892(6) 0.7599(4) 0.2822(5) 0.0820(15) Uani 1 1 d . . .
F3 F -0.1873(8) 0.8158(5) 0.0833(6) 0.108(2) Uani 1 1 d . . .
N1 N 0.0482(6) 0.3221(4) 0.3206(5) 0.0409(11) Uani 1 1 d . A .
N2 N 0.2500 0.2078(6) 0.2500 0.0405(15) Uani 1 2 d S . .
C8 C 0.1452(7) 0.1561(5) 0.2795(7) 0.0530(16) Uani 0.50 1 d P A 1
H8 H 0.1364 0.0804 0.2692 0.079 Uiso 0.50 1 calc PR A 1
N3 N 0.1452(7) 0.1561(5) 0.2795(7) 0.0530(16) Uani 0.50 1 d P A 2
C9 C 0.1149(17) 0.0382(10) 0.2359(17) 0.053(3) Uani 0.50 1 d P A 2
H9A H 0.0874 0.0330 0.1380 0.080 Uiso 0.50 1 calc PR A 2
H9B H 0.0328 0.0107 0.2621 0.080 Uiso 0.50 1 calc PR A 2
H9C H 0.2053 -0.0045 0.2799 0.080 Uiso 0.50 1 calc PR A 2
O1 O 0.0519(8) 0.5789(4) 0.2071(7) 0.0746(19) Uani 1 1 d . . .
O2 O -0.2091(9) 0.5813(4) 0.0824(9) 0.083(2) Uani 1 1 d . . .
O3 O -0.0425(8) 0.6460(5) -0.0230(6) 0.0822(19) Uani 1 1 d . . .
O4 O -0.2570(11) 0.0711(6) 0.4900(10) 0.099(3) Uani 1 1 d . . .
Pb1 Pb 0.2500 0.41390(2) 0.2500 0.04113(14) Uani 1 2 d S . .
S1 S -0.0642(2) 0.62605(13) 0.10101(16) 0.0471(4) Uani 1 1 d . A .
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'
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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
F2 C1 F1 105.7(7) . . ?
F2 C1 F3 105.7(7) . . ?
F1 C1 F3 111.1(7) . . ?
F2 C1 S1 112.7(6) . . ?
F1 C1 S1 110.0(6) . . ?
F3 C1 S1 111.5(6) . . ?
N1 C2 C3 122.9(6) . . ?
N1 C2 H2 118.6 . . ?
C3 C2 H2 118.6 . . ?
C4 C3 C2 118.0(6) . . ?
C4 C3 H3 121.0 . . ?
C2 C3 H3 121.0 . . ?
C3 C4 C6 120.0(6) . . ?
C3 C4 C5 120.6(7) . . ?
C6 C4 C5 119.4(7) . . ?
O4 C5 C4 123.8(8) . . ?
O4 C5 H5 118.1 . . ?
C4 C5 H5 118.1 . . ?
C4 C6 C7 118.7(6) . . ?
C4 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
N1 C7 C6 121.4(6) . . ?
N1 C7 C8 117.4(5) . . ?
C6 C7 C8 121.2(6) . . ?
C2 N1 C7 119.0(5) . . ?
C2 N1 Pb1 121.1(4) . . ?
C7 N1 Pb1 119.5(4) . . ?
C8 N2 N3 121.4(7) . 2 ?
C8 N2 C8 121.4(7) . 2 ?
N3 N2 C8 0.0(7) 2 2 ?
C8 N2 Pb1 119.3(4) . . ?
N3 N2 Pb1 119.3(4) 2 . ?
C8 N2 Pb1 119.3(4) 2 . ?
N2 C8 C7 119.7(5) . . ?
N2 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
S1 O1 Pb1 139.3(4) . . ?
S1 O3 Pb1 119.3(4) . 3_565 ?
N2 Pb1 N1 63.55(11) . . ?
N2 Pb1 N1 63.55(11) . 2 ?
N1 Pb1 N1 127.1(2) . 2 ?
N2 Pb1 O3 73.55(14) . 3_565 ?
N1 Pb1 O3 74.95(17) . 3_565 ?
N1 Pb1 O3 90.43(18) 2 3_565 ?
N2 Pb1 O3 73.55(14) . 4_666 ?
N1 Pb1 O3 90.43(18) . 4_666 ?
N1 Pb1 O3 74.95(17) 2 4_666 ?
O3 Pb1 O3 147.1(3) 3_565 4_666 ?
N2 Pb1 O1 139.07(15) . . ?
N1 Pb1 O1 80.6(2) . . ?
N1 Pb1 O1 146.7(2) 2 . ?
O3 Pb1 O1 78.8(2) 3_565 . ?
O3 Pb1 O1 128.50(19) 4_666 . ?
N2 Pb1 O1 139.07(15) . 2 ?
N1 Pb1 O1 146.7(2) . 2 ?
N1 Pb1 O1 80.6(2) 2 2 ?
O3 Pb1 O1 128.50(19) 3_565 2 ?
O3 Pb1 O1 78.8(2) 4_666 2 ?
O1 Pb1 O1 81.9(3) . 2 ?
O1 S1 O3 119.0(5) . . ?
O1 S1 O2 113.5(4) . . ?
O3 S1 O2 112.6(5) . . ?
O1 S1 C1 102.1(3) . . ?
O3 S1 C1 102.9(4) . . ?
O2 S1 C1 104.2(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
C1 F2 1.309(9) . ?
C1 F1 1.319(10) . ?
C1 F3 1.330(10) . ?
C1 S1 1.816(7) . ?
C2 N1 1.336(8) . ?
C2 C3 1.378(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(10) . ?
C3 H3 0.9500 . ?
C4 C6 1.381(9) . ?
C4 C5 1.503(10) . ?
C5 O4 1.195(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.387(8) . ?
C6 H6 0.9500 . ?
C7 N1 1.344(8) . ?
C7 C8 1.424(8) . ?
N1 Pb1 2.565(5) . ?
N2 C8 1.315(6) . ?
N2 N3 1.315(6) 2 ?
N2 C8 1.315(6) 2 ?
N2 Pb1 2.565(7) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
O1 S1 1.401(6) . ?
O1 Pb1 2.718(5) . ?
O2 S1 1.438(8) . ?
O3 S1 1.423(6) . ?
O3 Pb1 2.632(7) 3_565 ?
Pb1 N1 2.565(5) 2 ?
Pb1 O3 2.632(7) 3_565 ?
Pb1 O3 2.632(7) 4_666 ?
Pb1 O1 2.718(5) 2 ?
