#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:02:54 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180220 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/06/7110697.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7110697
loop_
_publ_author_name
'Jaunky, Wojciech'
'Hosseini, Mir Wais'
'Planeix, Jean Marc'
'Cian, André De'
'Kyritsakas, Nathalie'
'Fischer, Jean'
_publ_section_title
;
 Molecular braids: quintuple helical hydrogen bonded molecular
 network†
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2313
_journal_paper_doi               10.1039/a906728k
_journal_year                    1999
_chemical_formula_moiety         'C68 H68 Cl12 N8 O4'
_chemical_formula_sum            'C68 H68 Cl12 N8 O4'
_chemical_formula_weight         1486.79
_chemical_name_systematic        ' ?'
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3435(6)
_cell_length_b                   17.3435(6)
_cell_length_c                   24.104(1)
_cell_measurement_reflns_used    14248
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      1.4
_cell_volume                     7250.4(5)
_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
;
  14248 reflections were collected using program Collect
 ("Collect" Data collection software, Nonius B.V., 1998)
 The conditions were as follow : crystal to detector distance =  39. mm.
 Scan angle =  2.0 deg 1 scans of  150 sec per frame.
 Data collection was divided into  1 sets
 with the following starting angles and number of frames :

 Set 1 Theta =    9.59 Omega =  180.00 Kappa =    0.00   64 frames
 Friedel pairs were not averaged. Internal R = 0.06
;
_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
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14248
_diffrn_reflns_theta_max         31.99
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.36
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.483
_refine_ls_goodness_of_fit_ref   1.414
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2474
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.183
_refine_ls_R_factor_gt           0.067
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo²/(σ²(Fo²)+0.0004 Fo⁴)+1.0'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.140
_refine_ls_wR_factor_ref         0.079
_reflns_number_gt                2474
_reflns_number_total             5968
_reflns_threshold_expression     >3.0σ(I)
_cod_data_source_file            906728ksup1.cif
_cod_data_source_block           st410
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^)+0.0004
Fo^4^)+1.0' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0004 Fo^4^)+1.0'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7250.4(9)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7110697
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,-y,1/2+z
3/4-y,1/4+x,1/4+z
3/4+y,3/4-x,3/4+z
-x,-y,-z
1/2+x,+y,1/2-z
3/4+y,1/4-x,1/4-z
3/4-y,3/4+x,3/4-z
1/2+x,1/2+y,1/2+z
-x,1/2-y,+z
1/4-y,3/4+x,3/4+z
1/4+y,1/4-x,1/4+z
1/2-x,1/2-y,1/2-z
+x,1/2+y,-z
1/4+y,3/4-x,3/4-z
1/4-y,1/4+x,1/4-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
C1 0.9439(2) 0.0940(2) 0.0947(2) 0.023(2) Uani ? ? C
C2 0.8874(2) 0.1384(2) 0.1205(2) 0.023(2) Uani ? ? C
C3 0.8451(2) 0.1937(2) 0.0911(2) 0.022(2) Uani ? ? C
C4 0.8553(2) 0.1988(2) 0.0342(2) 0.026(2) Uani ? ? C
C5 0.9081(2) 0.1519(2) 0.0073(2) 0.026(2) Uani ? ? C
C6 0.9531(2) 0.1011(2) 0.0377(2) 0.025(2) Uani ? ? C
O 0.8747(1) 0.1289(1) 0.1770(1) 0.026(1) Uani ? ? O
C7 0.8165(2) 0.0723(2) 0.1890(2) 0.034(2) Uani ? ? C
C8 0.8100(3) 0.0629(3) 0.2507(2) 0.043(2) Uani ? ? C
C9 0.7480(3) 0.0053(3) 0.2669(2) 0.050(3) Uani ? ? C
N1 0.9146(2) 0.1554(2) -0.0518(1) 0.028(2) Uani ? ? N
C10 0.9813(2) 0.1564(2) -0.0720(2) 0.030(2) Uani ? ? C
C11 0.9963(3) 0.1503(2) -0.1323(2) 0.030(2) Uani ? ? C
C12 1.0705(3) 0.1542(3) -0.1523(2) 0.041(2) Uani ? ? C
C13 1.0835(3) 0.1445(3) -0.2079(2) 0.054(3) Uani ? ? C
N2 1.0287(3) 0.1311(2) -0.2448(2) 0.052(2) Uani ? ? N
C14 0.9560(3) 0.1277(3) -0.2251(2) 0.049(3) Uani ? ? C
C15 0.9365(3) 0.1369(3) -0.1704(2) 0.040(2) Uani ? ? C
C16 0.9988(2) 0.0444(2) 0.1284(2) 0.025(2) Uani ? ? C
C17 0.6814(3) 0.2827(3) -0.1212(2) 0.050(3) Uani ? ? C
CL1 0.76019(7) 0.22518(8) -0.10201(6) 0.0558(7) Uani ? ? Cl
CL2 0.71095(9) 0.37471(9) -0.14170(8) 0.0722(9) Uani ? ? Cl
CL3 0.6257(1) 0.2407(1) -0.17205(8) 0.099(1) Uani ? ? Cl
H1 0.8258 0.2348 0.0134 0.0338 Uiso calc C4 H
H2 0.9907 0.0706 0.0192 0.0321 Uiso calc C6 H
H3 0.8304 0.0245 0.1727 0.0443 Uiso calc C7 H
H4 0.7684 0.0889 0.1744 0.0443 Uiso calc C7 H
H5 0.7978 0.1114 0.2667 0.0557 Uiso calc C8 H
H6 0.8581 0.0454 0.2648 0.0557 Uiso calc C8 H
H7 0.7459 0.0011 0.3062 0.0652 Uiso calc C9 H
H8 0.6995 0.0224 0.2533 0.0652 Uiso calc C9 H
H9 0.7598 -0.0436 0.2513 0.0652 Uiso calc C9 H
H10 1.0240 0.1613 -0.0476 0.0405 Uiso calc C10 H
H11 1.1123 0.1636 -0.1277 0.0540 Uiso calc C12 H
H12 1.1352 0.1475 -0.2207 0.0701 Uiso calc C13 H
H13 0.9156 0.1183 -0.2508 0.0672 Uiso calc C14 H
H14 0.8843 0.1342 -0.1587 0.0523 Uiso calc C15 H
H15 1.0258 0.0106 0.1043 0.0327 Uiso calc C16 H
H16 0.9703 0.0150 0.1546 0.0327 Uiso calc C16 H
H17 0.6502 0.2875 -0.0890 0.0658 Uiso calc C17 H
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
Cl 0.132 0.159 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
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_3
C2 C1 C6 118.2(3) .
C2 C1 C16 121.1(3) .
C6 C1 C16 120.4(3) .
C1 C2 C3 121.4(3) .
C1 C2 O 118.9(3) .
C3 C2 O 119.7(3) .
C2 C3 C4 118.6(3) .
C2 C3 C16 120.5(3) 7_565
C4 C3 C16 120.8(3) 7_565
C3 C4 C5 120.6(3) .
C4 C5 C6 119.9(4) .
C4 C5 N1 119.5(3) .
C6 C5 N1 120.6(3) .
C1 C6 C5 121.0(3) .
C2 O C7 113.0(3) .
O C7 C8 109.2(3) .
C7 C8 C9 112.3(4) .
C5 N1 C10 117.5(3) .
N1 C10 C11 122.9(4) .
C10 C11 C12 120.3(4) .
C10 C11 C15 121.7(4) .
C12 C11 C15 118.0(4) .
C11 C12 C13 119.4(4) .
C12 C13 N2 124.2(5) .
C13 N2 C14 116.2(4) .
N2 C14 C15 124.4(5) .
C11 C15 C14 117.8(4) .
CL1 C17 CL2 111.5(3) .
CL1 C17 CL3 112.6(3) .
CL2 C17 CL3 110.4(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.392(5) .
C1 C6 1.390(5) .
C1 C16 1.519(5) .
C2 C3 1.400(5) .
C2 O 1.389(5) .
C3 C4 1.385(5) .
C3 C16 1.519(5) 7_565
C4 C5 1.386(5) .
C5 C6 1.386(5) .
C5 N1 1.429(5) .
O C7 1.438(5) .
C7 C8 1.500(6) .
C8 C9 1.518(7) .
N1 C10 1.256(5) .
C10 C11 1.479(6) .
C11 C12 1.375(6) .
C11 C15 1.404(6) .
C12 C13 1.370(7) .
C13 N2 1.323(7) .
N2 C14 1.349(7) .
C14 C15 1.370(7) .
C17 CL1 1.753(5) .
C17 CL2 1.748(6) .
C17 CL3 1.723(5) .
