Solid-State Self-Assembly of a Calix[4]pyrrole-Resorcinarene Hybrid into a Hexameric Cage
Guzmán Gil-Ramírez; Jordi Benet-Buchholz; Eduardo C. Escudero-Adán; Pablo Ballester; Journal of the American Chemical Society 129 (2007) 3820–3821; doi:10.1021/ja070037k

data_4109274
_publ_contact_author
;
    Dr. Benet-Buchholz, Jordi
    The Institute of Chemical Research of Catalonia (ICIQ)    
    X-ray Diffraction Unit
    Avgda. Pa\=isos Catalans 16
    E-43007 Tarragona, Spain
;
_publ_contact_author_email       jbenet@iciq.es
_publ_contact_author_fax         '+34 977 920 224'
_publ_contact_author_phone       '+34 977 920 204'
_publ_section_title
;
 Solid-State Self-Assembly of a Calix[4]pyrrole-Resorcinarene Hybrid into
 a Hexameric Cage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3820
_journal_page_last               3821
_journal_paper_doi               10.1021/ja070037k
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C56 H62 Cl N7 O8'
_chemical_formula_weight         996.58
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c 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            4
_cell_length_a                   16.0984(19)
_cell_length_b                   16.0984(19)
_cell_length_c                   20.223(5)
_cell_measurement_reflns_used    6255
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.54
_cell_measurement_theta_min      3.23
_cell_volume                     5241.0(16)
_computing_cell_refinement       'Bruker-Nonius Apex v1.0-22 2002'
_computing_data_collection       'Bruker-Nonius Apex v1.0-22 2002'
_computing_data_reduction        'SAINT+ Version 7.06A Bruker-Nonius, 2004'
_computing_molecular_graphics    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_publication_material  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_refinement  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_solution    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30087
_diffrn_reflns_theta_full        22.56
_diffrn_reflns_theta_max         22.56
_diffrn_reflns_theta_min         2.53
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           90
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.842474
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2.1 2003 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       Block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       0.028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         1698
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.1486
_refine_ls_R_factor_gt           0.1344
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1483P)^2^+30.9290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3453
_refine_ls_wR_factor_ref         0.3678
_reflns_number_gt                1556
_reflns_number_total             1698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070037ksi20070103_112425_2.cif
_cod_data_source_block           ggp4ncc
_cod_original_cell_volume        5240.9(17)
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4109274