#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:22:13 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178896 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/25/4112599.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_4112599
loop_
_publ_author_name
'Anne Petitjean'
'Richard G. Khoury'
'Nathalie Kyritsakas'
'Jean-Marie Lehn'
_publ_section_title
;
 Dynamic Devices. Shape Switching and Substrate Binding in Ion-Controlled
 Nanomechanical Molecular Tweezers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6637
_journal_page_last               6647
_journal_paper_doi               10.1021/ja031915r
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C51 H35 F6 N7 O8 S2 Zn'
_chemical_formula_sum            'C51 H35 F6 N7 O8 S2 Zn'
_chemical_formula_weight         1117.38
_chemical_name_systematic        ' ?'
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2654(2)
_cell_length_b                   18.7260(3)
_cell_length_c                   19.6692(4)
_cell_measurement_reflns_used    14000
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      1.4
_cell_volume                     4885.98(15)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
  14000 reflections were collected using program Collect
 ("Collect" Data collection software, Nonius B.V., 1998)
 The conditions were as follow : crystal to detector distance =  36. mm.
 Scan angle =  2.0 deg 1 scans of   90 sec per frame.
 Data collection was divided into  2 set(s)
 with the following starting angles and number of frames :

 Set 1 Theta =    8.80 Omega =    0.00 Kappa =    0.00  122 frames
 Set 2 Theta =   -8.80 Kappa =  165.00 Phi   =    0.00   26 frames
 Friedel pairs were averaged. Internal R = 0.07
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'π scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14000
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.52
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.251
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4005
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.095
_refine_ls_R_factor_gt           0.033
_refine_ls_shift/esd_mean        0.003
_refine_ls_shift/su_max          0.014
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.516
_refine_ls_wR_factor_ref         0.056
_reflns_number_gt                4005
_reflns_number_total             7817
_reflns_threshold_expression     >3.0σ(I)
_cod_data_source_file            ja031915rsi20031223_051017.cif
_cod_data_source_block           st1175
_cod_original_cell_volume        4886.0(1)
_cod_database_code               4112599
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2-y,+z
-x,1/2+y,1/2-z
1/2+x,-y,1/2-z
-x,-y,-z
1/2+x,1/2+y,-z
+x,1/2-y,1/2+z
1/2-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
ZN Zn 0.7500 0.2500 0.46547(2) 0.0224(2) Uani 1 2 d S
N1 N 0.8535(1) 0.1656(1) 0.4867(1) 0.036(1) Uani 1 1 d .
C1 C 0.8877(2) 0.1263(1) 0.5244(1) 0.033(1) Uani 1 1 d .
C2 C 0.9298(2) 0.0770(2) 0.5742(1) 0.048(1) Uani 1 1 d .
N2 N 0.7500 0.2500 0.3535(1) 0.023(1) Uani 1 2 d S
C3 C 0.6895(2) 0.2050(1) 0.3195(1) 0.023(1) Uani 1 1 d .
C4 C 0.6879(2) 0.2038(1) 0.2488(1) 0.026(1) Uani 1 1 d .
C5 C 0.7500 0.2500 0.2134(1) 0.027(1) Uani 1 2 d S
C6 C 0.6269(1) 0.1600(1) 0.3642(1) 0.023(1) Uani 1 1 d .
C7 C 0.5640(2) 0.1059(1) 0.3411(1) 0.032(1) Uani 1 1 d .
C8 C 0.5071(2) 0.0685(1) 0.3878(1) 0.037(1) Uani 1 1 d .
C9 C 0.5124(2) 0.0858(1) 0.4559(1) 0.030(1) Uani 1 1 d .
C10 C 0.5765(2) 0.1398(1) 0.4755(1) 0.024(1) Uani 1 1 d .
N3 N 0.6337(1) 0.17574(9) 0.43073(8) 0.0221(8) Uani 1 1 d .
C11 C 0.5931(2) 0.1638(1) 0.5476(1) 0.024(1) Uani 1 1 d .
O1 O 0.6674(1) 0.20052(8) 0.56161(8) 0.0294(8) Uani 1 1 d .
N4 N 0.5241(1) 0.1426(1) 0.59276(9) 0.0264(9) Uani 1 1 d .
C12 C 0.5281(2) 0.1553(1) 0.6647(1) 0.026(1) Uani 1 1 d .
C13 C 0.5898(2) 0.1114(1) 0.7048(1) 0.027(1) Uani 1 1 d .
C14 C 0.6607(2) 0.0620(1) 0.6777(1) 0.032(1) Uani 1 1 d .
C15 C 0.7162(2) 0.0191(1) 0.7192(1) 0.037(1) Uani 1 1 d .
C16 C 0.7047(2) 0.0219(1) 0.7906(1) 0.042(1) Uani 1 1 d .
C17 C 0.6395(2) 0.0695(1) 0.8189(1) 0.037(1) Uani 1 1 d .
C18 C 0.5809(2) 0.1170(1) 0.7778(1) 0.030(1) Uani 1 1 d .
C19 C 0.5162(2) 0.1670(1) 0.8059(1) 0.033(1) Uani 1 1 d .
C20 C 0.4595(2) 0.2136(1) 0.7658(1) 0.032(1) Uani 1 1 d .
C21 C 0.3966(2) 0.2677(1) 0.7937(1) 0.047(1) Uani 1 1 d .
C22 C 0.3454(2) 0.3138(2) 0.7533(2) 0.054(2) Uani 1 1 d .
C23 C 0.3514(2) 0.3083(1) 0.6824(2) 0.052(2) Uani 1 1 d .
C24 C 0.4080(2) 0.2565(1) 0.6527(1) 0.040(1) Uani 1 1 d .
C25 C 0.4652(2) 0.2077(1) 0.6925(1) 0.030(1) Uani 1 1 d .
S S 0.25259(4) 0.05509(3) 0.51927(3) 0.0297(3) Uani 1 1 d .
O2 O 0.2982(1) 0.00642(9) 0.47230(9) 0.042(1) Uani 1 1 d .
O3 O 0.3219(1) 0.0866(1) 0.56713(9) 0.044(1) Uani 1 1 d .
O4 O 0.1592(1) 0.0323(1) 0.54792(9) 0.044(1) Uani 1 1 d .
C26 C 0.2150(3) 0.1299(2) 0.4655(1) 0.054(2) Uani 1 1 d .
F1 F 0.1649(2) 0.17849(9) 0.4993(1) 0.090(1) Uani 1 1 d .
F2 F 0.2939(2) 0.1613(1) 0.4374(1) 0.092(1) Uani 1 1 d .
F3 F 0.1548(2) 0.1070(1) 0.4155(1) 0.097(1) Uani 1 1 d .
H1 H 0.9736 0.0444 0.5520 0.0629 Uiso 1 1 d .
H2 H 0.9664 0.1031 0.6074 0.0629 Uiso 1 1 d .
H3 H 0.8767 0.0514 0.5956 0.0629 Uiso 1 1 d .
H4 H 0.6448 0.1717 0.2252 0.0358 Uiso 1 1 d .
H5 H 0.7500 0.2500 0.1651 0.0387 Uiso 1 2 d S
H6 H 0.5603 0.0948 0.2940 0.0430 Uiso 1 1 d .
H7 H 0.4644 0.0309 0.3731 0.0481 Uiso 1 1 d .
H8 H 0.4727 0.0610 0.4885 0.0391 Uiso 1 1 d .
H9 H 0.6694 0.0588 0.6299 0.0418 Uiso 1 1 d .
H10 H 0.7634 -0.0132 0.6999 0.0491 Uiso 1 1 d .
H11 H 0.7424 -0.0094 0.8188 0.0560 Uiso 1 1 d .
H12 H 0.6327 0.0712 0.8669 0.0511 Uiso 1 1 d .
H13 H 0.5101 0.1696 0.8540 0.0459 Uiso 1 1 d .
H14 H 0.3904 0.2716 0.8417 0.0611 Uiso 1 1 d .
H15 H 0.3051 0.3501 0.7732 0.0707 Uiso 1 1 d .
H16 H 0.3154 0.3412 0.6548 0.0681 Uiso 1 1 d .
H17 H 0.4095 0.2529 0.6045 0.0517 Uiso 1 1 d .
H18 H 0.4676 0.1169 0.5759 0.0361 Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1
H 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1
F 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1
N 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1
O 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1
S 0.110 0.124 International_Tables_Vol_IV_Table_2.3.1
Zn 0.222 1.431 International_Tables_Vol_IV_Table_2.3.1
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
N1 ZN N1 157.4(1) . 2_655
N1 ZN N3 92.55(7) . .
N1 ZN N3 94.46(7) . 2_655
N1 ZN N3 94.46(7) 2_655 .
N1 ZN N3 92.55(7) 2_655 2_655
N3 ZN N3 143.6(1) . 2_655
ZN N1 C1 149.5(2) . .
N1 C1 C2 178.4(3) . .
C3 N2 C3 120.1(3) . 2_655
N2 C3 C4 121.2(2) . .
N2 C3 C6 113.4(2) . .
C4 C3 C6 125.3(2) . .
C3 C4 C5 118.9(2) . .
C4 C5 C4 119.5(3) . 2_655
C3 C6 C7 124.1(2) . .
C3 C6 N3 114.7(2) . .
C7 C6 N3 121.2(2) . .
C6 C7 C8 118.8(2) . .
C7 C8 C9 120.0(2) . .
C8 C9 C10 118.4(2) . .
C9 C10 N3 122.2(2) . .
C9 C10 C11 125.0(2) . .
N3 C10 C11 112.7(2) . .
ZN N3 C6 119.4(1) . .
ZN N3 C10 120.8(1) . .
C6 N3 C10 119.4(2) . .
C10 C11 O1 119.6(2) . .
C10 C11 N4 115.9(2) . .
O1 C11 N4 124.4(2) . .
C11 N4 C12 125.4(2) . .
N4 C12 C13 118.6(2) . .
N4 C12 C25 118.6(2) . .
C13 C12 C25 122.6(2) . .
C12 C13 C14 123.8(2) . .
C12 C13 C18 118.0(2) . .
C14 C13 C18 118.2(2) . .
C13 C14 C15 121.1(2) . .
C14 C15 C16 121.0(3) . .
C15 C16 C17 119.9(3) . .
C16 C17 C18 121.4(2) . .
C13 C18 C17 118.2(2) . .
C13 C18 C19 119.7(2) . .
C17 C18 C19 122.1(2) . .
C18 C19 C20 122.0(2) . .
C19 C20 C21 122.8(2) . .
C19 C20 C25 119.2(2) . .
C21 C20 C25 118.0(3) . .
C20 C21 C22 121.4(3) . .
C21 C22 C23 120.6(3) . .
C22 C23 C24 120.9(3) . .
C23 C24 C25 121.1(3) . .
C12 C25 C20 118.3(2) . .
C12 C25 C24 123.6(2) . .
C20 C25 C24 118.1(2) . .
O2 S O3 114.3(1) . .
O2 S O4 115.6(1) . .
O2 S C26 103.3(1) . .
O3 S O4 114.7(1) . .
O3 S C26 103.8(2) . .
O4 S C26 102.8(1) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
ZN N1 2.134(2) .
ZN N1 2.134(2) 2_655
ZN N3 2.187(2) .
ZN N3 2.187(2) 2_655
N1 C1 1.139(3) .
C1 C2 1.457(4) .
N2 C3 1.342(2) .
N2 C3 1.342(2) 2_655
C3 C4 1.390(3) .
C3 C6 1.474(3) .
C4 C5 1.383(3) .
C4 C5 1.383(3) 2_655
C6 C7 1.389(3) .
C6 N3 1.344(3) .
C7 C8 1.380(4) .
C8 C9 1.381(3) .
C9 C10 1.377(3) .
C10 N3 1.342(3) .
C10 C11 1.503(3) .
C11 O1 1.232(3) .
C11 N4 1.337(3) .
N4 C12 1.435(3) .
C12 C13 1.402(3) .
C12 C25 1.400(3) .
C13 C14 1.423(3) .
C13 C18 1.445(3) .
C14 C15 1.360(4) .
C15 C16 1.413(4) .
C16 C17 1.360(4) .
C17 C18 1.431(4) .
C18 C19 1.386(4) .
C19 C20 1.397(4) .
C20 C21 1.422(4) .
C20 C25 1.448(3) .
C21 C22 1.356(4) .
C22 C23 1.399(5) .
C23 C24 1.359(4) .
C24 C25 1.423(4) .
S O2 1.432(2) .
S O3 1.442(2) .
S O4 1.426(2) .
S C26 1.826(3) .
C26 F1 1.308(3) .
C26 F2 1.321(4) .
C26 F3 1.338(4) .
F1 F2 2.123(3) .
F1 F3 2.127(4) .
F2 F3 2.151(4) .
