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
Dalgarno, Scott J.; Raston, Colin L.; Chemical Communications  (2002) 2216–; doi:10.1039/b207922b

data_7114462
_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/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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