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_4504525
_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            'C144 H262 N8 Nd2 O123 S16'
_chemical_formula_weight         4875.06
_chemical_name_common
'[(Nd(H2O)9)2][((1,7-diaza-12-crown-4 + 2H+)?p-sulfonatocalix[4]arene)4 + 2H+]?33H2O'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.4550(3)
_cell_angle_beta                 83.0468(3)
_cell_angle_gamma                80.6640(10)
_cell_formula_units_Z            2
_cell_length_a                   19.92300(10)
_cell_length_b                   21.0935(2)
_cell_length_c                   24.7992(2)
_cell_measurement_temperature    150(2)
_cell_volume                     10198.60(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
;
 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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1605
_diffrn_reflns_av_sigmaI/netI    0.1076
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            194935
_diffrn_reflns_theta_full        27.32
_diffrn_reflns_theta_max         27.32
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  0.8720
_exptl_absorpt_correction_T_min  0.7660
_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_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5084
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.891
_refine_diff_density_min         -4.440
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.344
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2677
_refine_ls_number_reflns         45488
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.345
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.003
_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          0.2209
_refine_ls_wR_factor_ref         0.2460
_reflns_number_gt                29303
_reflns_number_total             45488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050261qsi20050922_023019.cif
_cod_data_source_block           diaza12c4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        10198.61(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4504525