Synthesis of New Tren-Based Tris-Macrocycles. Anion Cluster Assembling Inside the Cavity Generated by a Bowl-Shaped Receptor
Carla Bazzicalupi; Andrea Bencini; Emanuela Berni; Antonio Bianchi; Samuele Ciattini; Claudia Giorgi; Sauro Maoggi; Piero Paoletti; Barbara Valtancoli; Journal of Organic Chemistry 67 (2002) 9107–9110; doi:10.1021/jo020474b

data_4022215
_publ_contact_author_address
;
Department of Chemistry,
POlo Scientifico,
University of Florence
via della Lastruccia 3
I-50019 Sesto Fiorentino, Firenze, Italy
;
_publ_contact_author_email       andrea.bencini@unifi.it
_publ_contact_author_name        'Dr. Andrea Bencini'
_publ_section_title
;
 Synthesis of New Tren-Based Tris-Macrocycles.
 Anion Cluster Assembling Inside the Cavity Generated
 by a Bowl-Shaped Receptor
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9107
_journal_page_last               9110
_journal_paper_doi               10.1021/jo020474b
_journal_volume                  67
_journal_year                    2002
_chemical_formula_moiety
;
2(C30 H60 N13), Cl12 Na6 O48, 6(Cl O4), 2(Cl), Na
;
_chemical_formula_sum            'C60 H120 Cl20 N26 Na7 O72'
_chemical_formula_weight         3227.76
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   21.670(2)
_cell_length_b                   21.670(2)
_cell_length_c                   23.534(2)
_cell_measurement_reflns_used    112
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      3.5
_cell_volume                     9570.3(15)
_computing_cell_refinement       'CCD Smart'
_computing_data_collection       'CCD Smart'
_computing_data_reduction        'CCD Smart'
_computing_molecular_graphics    'ORETEP 3 (Farrugia, 2001)'
_computing_publication_material  'parst97 (Nardelli, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'CCD smart 1K'
_diffrn_radiation_monochromator  'Gobel mirrors'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9707
_diffrn_reflns_theta_full        57.95
_diffrn_reflns_theta_max         57.95
_diffrn_reflns_theta_min         4.18
_exptl_absorpt_coefficient_mu    5.161
_exptl_absorpt_correction_T_max  0.213
_exptl_absorpt_correction_T_min  0.112
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4965
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.000019(18)
_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   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         2603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0834
_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^)+(0.1314P)^2^+273.9363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2233
_refine_ls_wR_factor_ref         0.2342
_reflns_number_gt                2240
_reflns_number_total             2603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo020474b.cif
_cod_data_source_block           '[(Na(ClO4)6)(L1)2H13][Na6Cl2(ClO4)12]'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4022215