#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:21:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180258 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/44/7114462.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_7114462
loop_
_publ_author_name
'Dalgarno, Scott J.'
'Raston, Colin L.'
_publ_section_title
;
 Capture of di-protonated [2.2.2]cryptand in the cavity of two
 p-sulfonated calixarenes as part of 2-D bi-layer lanthanide coordination
 polymers
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              2216
_journal_paper_doi               10.1039/b207922b
_journal_year                    2002
_chemical_formula_sum            'C9.25 H10.75 N0.25 Nd0.25 O6.38 S'
_chemical_formula_weight         295.55
_chemical_name_common
(2H[2.2.2]cryptand)2+(p-sulfonatocalix[4]arene)4-2(M(H2O)4)3+2
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           126
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2bc'
_symmetry_space_group_name_H-M   'P 4/n n c :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   11.9026(17)
_cell_length_b                   11.9026(17)
_cell_length_c                   32.876(7)
_cell_measurement_temperature    150(2)
_cell_volume                     4657.6(14)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
ORTEP3 for Windows (Farrugia, 1997) 
XSeed (Barbour, 2001)
;
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets 
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_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  0.1563
_diffrn_reflns_av_sigmaI/netI    0.1008
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            17329
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    1.385
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program 
SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.530
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.1219
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.091
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1767
_refine_ls_wR_factor_ref         0.2046
_reflns_number_gt                1674
_reflns_number_total             2701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207922b.txt
_cod_data_source_block           sjd128
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        4657.6(13)
_cod_original_sg_symbol_H-M      P4/nnc
_cod_database_code               7114462
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y, -z+1/2'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y, z-1/2'
'-y, -x, z-1/2'
'y-1/2, x-1/2, 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_group
O8 O -0.287(4) 0.184(4) 0.6976(13) 0.040(11) Uiso 0.13 1 d P .
C11 C -0.343(6) 0.009(6) 0.7418(19) 0.189(6) Uani 0.38 1 d P .
C10 C -0.281(8) 0.027(6) 0.7325(16) 0.189(6) Uani 0.38 1 d P 2
C9 C -0.323(3) -0.047(2) 0.6662(6) 0.189(6) Uani 0.75 1 d P 2
H9A H -0.2889 0.0241 0.6570 0.226 Uiso 0.75 1 calc PR 2
H9B H -0.4055 -0.0440 0.6620 0.226 Uiso 0.75 1 calc PR 2
C8 C -0.276(4) -0.138(3) 0.6470(6) 0.189(6) Uani 0.75 1 d P 2
H8A H -0.2036 -0.1080 0.6373 0.226 Uiso 0.75 1 calc PR 2
H8B H -0.3231 -0.1452 0.6222 0.226 Uiso 0.75 1 calc PR 2
C7 C 0.0379(5) -0.1568(5) 0.52520(19) 0.0201(14) Uani 1 1 d . .
H7A H 0.0263 -0.1609 0.4954 0.024 Uiso 1 1 calc R .
H7B H 0.1160 -0.1313 0.5300 0.024 Uiso 1 1 calc R .
O7 O -0.2952(18) -0.0712(16) 0.7088(5) 0.189(6) Uani 0.75 1 d P .
C6 C -0.0429(5) -0.0695(5) 0.54290(19) 0.0173(14) Uani 1 1 d . .
O6 O -0.0540(10) 0.2500 0.7500 0.085(3) Uiso 1 2 d S .
C5 C -0.0107(5) 0.0008(5) 0.5749(2) 0.0180(13) Uani 1 1 d . .
H5 H 0.0618 -0.0078 0.5865 0.022 Uiso 1 1 calc R .
O5 O 0.1068(4) 0.3431(4) 0.70065(14) 0.0341(13) Uani 1 1 d . .
C4 C -0.0814(5) 0.0819(5) 0.58986(19) 0.0199(14) Uani 1 1 d . .
O4 O 0.0829(4) 0.1923(4) 0.62144(14) 0.0290(12) Uani 1 1 d . .
C3 C -0.1905(5) 0.0913(5) 0.57462(19) 0.0195(14) Uani 1 1 d . .
H3 H -0.2406 0.1446 0.5862 0.023 Uiso 1 1 calc R .
O3 O -0.0557(4) 0.1132(4) 0.66681(15) 0.0343(13) Uani 1 1 d . .
C2 C -0.2262(5) 0.0242(5) 0.5430(2) 0.0179(15) Uani 1 1 d . .
O2 O -0.1030(4) 0.2746(4) 0.62489(16) 0.0366(13) Uani 1 1 d . .
C1 C -0.1503(5) -0.0526(5) 0.52657(19) 0.0179(14) Uani 1 1 d . .
N1 N -0.2500 -0.2500 0.6557(9) 0.189(6) Uani 1 4 d S .
H1A H -0.2500 -0.2500 0.6877 0.226 Uiso 1 4 calc SR 2
O1 O -0.1822(4) -0.1108(4) 0.49199(12) 0.0229(11) Uani 1 1 d . .
H1 H -0.1300 -0.1541 0.4849 0.027 Uiso 1 1 calc R .
S1 S -0.03777(15) 0.17311(14) 0.62876(5) 0.0256(4) Uani 1 1 d . .
Nd1 Nd 0.2500 0.2500 0.65813(2) 0.0216(3) Uani 1 4 d S .
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'
Nd Nd -0.1943 3.0179 '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
C10 C11 O7 65(8) . .
C10 C11 C10 52(9) . 6_456
O7 C11 C10 96(4) . 6_456
C11 C10 C10 100(8) . 6_456
C11 C10 O7 83(10) . .
C10 C10 O7 122(4) 6_456 .
C11 C10 C11 123(8) . 6_456
C10 C10 C11 29(5) 6_456 6_456
O7 C10 C11 106(6) . 6_456
O7 C9 C8 101(2) . .
C9 C8 N1 138(3) . .
C9 C8 C8 117(4) . 2_455
N1 C8 C8 46.2(4) . 2_455
C9 C8 C8 140(4) . 4_545
N1 C8 C8 46.2(4) . 4_545
C8 C8 C8 90.000(7) 2_455 4_545
C2 C7 C6 114.1(5) 4_545 .
C9 O7 C10 113(3) . .
C9 O7 C11 118(3) . .
C10 O7 C11 32(5) . .
C5 C6 C1 117.0(6) . .
C5 C6 C7 121.3(6) . .
C1 C6 C7 121.7(6) . .
C4 C5 C6 121.5(6) . .
C5 C4 C3 119.9(6) . .
C5 C4 S1 121.0(5) . .
C3 C4 S1 119.1(5) . .
S1 O4 Nd1 139.6(3) . .
C2 C3 C4 120.7(6) . .
C3 C2 C1 118.2(6) . .
C3 C2 C7 120.7(6) . 2_455
C1 C2 C7 121.0(6) . 2_455
O1 C1 C2 118.0(6) . .
O1 C1 C6 119.5(6) . .
C2 C1 C6 122.5(6) . .
C8 N1 C8 87.6(7) 3_445 4_545
C8 N1 C8 156(4) 3_445 .
C8 N1 C8 87.6(7) 4_545 .
C8 N1 C8 87.6(7) 3_445 2_455
C8 N1 C8 156(4) 4_545 2_455
C8 N1 C8 87.6(7) . 2_455
O2 S1 O3 114.0(3) . .
O2 S1 O4 112.4(3) . .
O3 S1 O4 111.1(3) . .
O2 S1 C4 107.1(3) . .
O3 S1 C4 106.2(3) . .
O4 S1 C4 105.4(3) . .
O4 Nd1 O4 120.4(2) 3 .
O4 Nd1 O4 75.68(10) 3 2
O4 Nd1 O4 75.68(10) . 2
O4 Nd1 O4 75.68(10) 3 4
O4 Nd1 O4 75.68(10) . 4
O4 Nd1 O4 120.4(2) 2 4
O4 Nd1 O5 73.61(17) 3 4
O4 Nd1 O5 147.75(17) . 4
O4 Nd1 O5 136.14(17) 2 4
O4 Nd1 O5 80.93(17) 4 4
O4 Nd1 O5 80.93(16) 3 3
O4 Nd1 O5 136.14(17) . 3
O4 Nd1 O5 73.61(17) 2 3
O4 Nd1 O5 147.75(17) 4 3
O5 Nd1 O5 71.28(11) 4 3
O4 Nd1 O5 136.14(17) 3 .
O4 Nd1 O5 80.93(16) . .
O4 Nd1 O5 147.75(17) 2 .
O4 Nd1 O5 73.61(16) 4 .
O5 Nd1 O5 71.28(11) 4 .
O5 Nd1 O5 111.0(2) 3 .
O4 Nd1 O5 147.75(17) 3 2
O4 Nd1 O5 73.61(17) . 2
O4 Nd1 O5 80.93(17) 2 2
O4 Nd1 O5 136.14(17) 4 2
O5 Nd1 O5 111.0(2) 4 2
O5 Nd1 O5 71.28(11) 3 2
O5 Nd1 O5 71.28(11) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O8 O8 1.81(8) 3_455
C11 C10 0.83(11) .
C11 O7 1.55(7) .
C11 C10 1.71(7) 6_456
C10 C10 1.36(15) 6_456
C10 O7 1.42(8) .
C10 C11 1.71(7) 6_456
C9 O7 1.47(2) .
C9 C8 1.37(3) .
C8 N1 1.40(2) .
C8 C8 1.93(4) 2_455
C8 C8 1.93(4) 4_545
C7 C2 1.519(8) 4_545
C7 C6 1.532(9) .
C6 C5 1.397(9) .
C6 C1 1.400(9) .
C5 C4 1.372(9) .
O5 Nd1 2.467(5) .
C4 C3 1.396(8) .
C4 S1 1.756(7) .
O4 S1 1.474(5) .
O4 Nd1 2.425(4) .
C3 C2 1.379(9) .
O3 S1 1.456(5) .
C2 C1 1.394(9) .
C2 C7 1.519(8) 2_455
O2 S1 1.442(5) .
C1 O1 1.385(7) .
N1 C8 1.40(2) 3_445
N1 C8 1.40(2) 4_545
N1 C8 1.40(2) 2_455
Nd1 O4 2.425(5) 3
Nd1 O4 2.425(4) 2
Nd1 O4 2.425(4) 4
Nd1 O5 2.467(5) 4
Nd1 O5 2.467(5) 3
Nd1 O5 2.467(5) 2
