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_4504524
_publ_section_title
;
 Host&#x2212;Guest Complexes withp-Sulfonatocalix[4,5]arenes Charged Crown
 Ethers and Lanthanides:&#x2009; Factors Affecting Molecular Capsule
 Formation
;
_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            'C99 H187.5 Eu3 N3 O98.25 S12'
_chemical_formula_weight         3832.62
_chemical_name_common
'[(1,7-diaza-15-crown-5 + 2H+)1.5?[(H2O)3[Eu(H2O)7Eu(H2O)6(p-sulfonatocalix[4]arene)2](p-sulfonatocalix[4]arene) Eu(H2O)8]?20.75H2O'
_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                 99.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.9099(1)
_cell_length_b                   28.3481(2)
_cell_length_c                   17.4843(3)
_cell_measurement_temperature    150(2)
_cell_volume                     15116.4(13)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1523
_diffrn_reflns_av_sigmaI/netI    0.0904
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            156512
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_T_max  0.9016
_exptl_absorpt_correction_T_min  0.7623
_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    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             7878
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.938
_refine_diff_density_min         -2.595
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2001
_refine_ls_number_reflns         34476
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0922
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0983P)^2^+116.7786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2363
_refine_ls_wR_factor_ref         0.2618
_reflns_number_gt                23993
_reflns_number_total             34476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050261qsi20050922_023019.cif
_cod_data_source_block           diaza15c5
_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_cell_volume        15116.5(3)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C99 H187.50 Eu3 N3 O98.25 S12'
_cod_database_code               4504524