A dual-functional tetrakis-imidazolium macrocycle for supramolecular assembly
Serpell, Christopher J.; Cookson, James; Thompson, Amber L.; Beer, Paul D.; Chemical Science 2 (2011) 494–; doi:10.1039/c0sc00511h

data_1515505
_publ_section_title
;
 A dual-functional tetrakis-imidazolium macrocycle for supramolecular
 assembly
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              494
_journal_paper_doi               10.1039/c0sc00511h
_journal_volume                  2
_journal_year                    2011
_chemical_formula_moiety         'C40 H36 N8, 2(C3 H6 O), 4(F6 P)'
_chemical_formula_sum            'C46 H48 F24 N8 O2 P4'
_chemical_formula_weight         1324.80
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-01-09
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 114.5895(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.7695(4)
_cell_length_b                   11.2232(2)
_cell_length_c                   24.0588(5)
_cell_measurement_reflns_used    6846
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5836.11(19)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.067
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            39540
_diffrn_reflns_theta_full        26.921
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         5.104
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_dark_red
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
It was found after refinement of the main residue, counter anions
and two equivalents of acetone that there was some residual electron
density to be accounted for. However, it was not possible to create
a sensible solvent disorder system to take this into account, and
therefore Platon Squeeze was applied in order to include this information
in the refinement.
;
_refine_diff_density_max         1.21
_refine_diff_density_min         -1.10
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9391
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6634
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.005040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.11P)^2^ +25.20P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2254
_refine_ls_wR_factor_gt          0.1963
_refine_ls_wR_factor_ref         0.2254
_reflns_limit_h_max              28
_reflns_limit_h_min              -30
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                4167
_reflns_number_total             6634
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.54
_oxford_diffrn_Wilson_scale      48.75
_oxford_refine_ls_r_factor_ref   0.1201
_oxford_refine_ls_scale          0.16878(18)
_oxford_reflns_number_all        6634
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 006CJS08
_cod_data_source_file            c0sc00511h.txt
_cod_data_source_block           1.AcetoneI
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               1515505