Modified synthesis and supramolecular polymerization of rim-to-rim connected bisresorcinarenes.
Yamada, Hitomi; Ikeda, Toshiaki; Mizuta, Tsutomu; Haino, Takeharu; Organic letters 14 (2012) 4510–4513; doi:10.1021/ol301996q

data_1508618
_publ_section_title
;
 Modified synthesis and supramolecular polymerization of rim-to-rim
 connected bisresorcinarenes.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4510
_journal_page_last               4513
_journal_paper_doi               10.1021/ol301996q
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C87.75 H113.75 N5.25 O23.75'
_chemical_formula_weight         1622.09
_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                75.126(3)
_cell_angle_beta                 86.009(3)
_cell_angle_gamma                66.856(2)
_cell_formula_units_Z            4
_cell_length_a                   17.196(3)
_cell_length_b                   20.217(4)
_cell_length_c                   27.804(5)
_cell_measurement_reflns_used    3651
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      2.26
_cell_volume                     8585(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.1285
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            44131
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         1.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.9955
_exptl_absorpt_correction_T_min  0.9829
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Sheldrick 1996 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3468
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.225
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.094
_refine_ls_d_res_low             15.80
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2057
_refine_ls_number_reflns         29151
_refine_ls_number_restraints     477
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1910
_refine_ls_R_factor_gt           0.1268
_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^)+(0.0755P)^2^+46.4638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2652
_refine_ls_wR_factor_ref         0.3036
_reflns_number_gt                26507
_reflns_number_total             36198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol301996q_si_003.cif
_cod_data_source_block           111108ikeda7
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C175.50 H227.50 N10.50 O47.50'
_cod_database_code               1508618
_refine_ls_d_res_max             0.84