Host−Guest Complexes withp-Sulfonatocalix[4,5]arenes Charged Crown Ethers and Lanthanides: Factors Affecting Molecular Capsule Formation
Dalgarno, Scott J.; Atwood, Jerry L.; Raston, Colin L.; Crystal Growth & Design 6 (2006) 174–; doi:10.1021/cg050261q

data_4504526
_publ_section_title
;
 Host&#x2212;Guest Complexes withp-Sulfonatocalix[4,5]arenes Charged Crown
 Ethers and Lanthanides:&#x2009; Factors Affecting Molecular Capsule
 Formation
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_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              174
_journal_paper_doi               10.1021/cg050261q
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C45 H90.5 Eu N2 O43.75 S5'
_chemical_formula_weight         1671.95
_chemical_name_common
'[[(1,7-diaza-15-crown-5 + 2H)?p-sulfonatocalix[5]-arene][Eu(H2O)9]]2.11.75H2O'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.627(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3620(4)
_cell_length_b                   19.9020(6)
_cell_length_c                   30.3716(12)
_cell_measurement_temperature    150(2)
_cell_volume                     6821.9(4)
_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
;
 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 0.741
_diffrn_measured_fraction_theta_max 0.741
_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  0.0689
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            12949
_diffrn_reflns_theta_full        23.59
_diffrn_reflns_theta_max         23.59
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  0.9434
_exptl_absorpt_correction_T_min  0.8913
_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    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3470
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.250
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         7561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1059P)^2^+59.5498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2162
_reflns_number_gt                5829
_reflns_number_total             7561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050261qsi20050922_023019.cif
_cod_data_source_block           5diaza15c5
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C45 H90.50 Eu N2 O43.75 S5'
_cod_database_code               4504526