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_1515503
_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         'C80 H72 N16, 8(F6 P), 2(C H Cl3)'
_chemical_formula_sum            'C82 H74 Cl6 F48 N16 P8'
_chemical_formula_weight         2656.01
_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
_audit_creation_date             10-07-23
_audit_creation_method           CRYSTALS_ver_14.07
_cell_angle_alpha                94.45(3)
_cell_angle_beta                 97.31(4)
_cell_angle_gamma                95.24(4)
_cell_formula_units_Z            1
_cell_length_a                   10.061(10)
_cell_length_b                   10.107(9)
_cell_length_c                   30.25(3)
_cell_measurement_reflns_used    5682
_cell_measurement_temperature    100
_cell_measurement_theta_max      32
_cell_measurement_theta_min      2
_cell_volume                     3026(5)
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_collection       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--2002)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'Si(1 1 1) double-crystal monochromator'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            38030
_diffrn_reflns_theta_full        25.084
_diffrn_reflns_theta_max         33.006
_diffrn_reflns_theta_min         2.032
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.368
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 1997--2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1332.000
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.005
_platon_squeeze_details
;
Large volumes containing diffuse electron density were observed.
Attempts to model these volumes as solvent molecules failed,
and consequently SQUEEZE was used in order to consider these
volumes in the refinement.
;
_refine_diff_density_max         1.35
_refine_diff_density_min         -1.25
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0207
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         8500
_refine_ls_number_restraints     590
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.1042
_refine_ls_shift/su_max          0.0008348
_refine_ls_shift/su_mean         0.0000283
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
35.1 44.8 15.1
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2124
_refine_ls_wR_factor_gt          0.1993
_refine_ls_wR_factor_ref         0.2124
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              13
_reflns_limit_k_min              -9
_reflns_limit_l_max              44
_reflns_limit_l_min              -45
_reflns_number_gt                6911
_reflns_number_total             27918
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.51
_oxford_diffrn_Wilson_scale      14.14
_oxford_refine_ls_r_factor_ref   0.1182
_oxford_refine_ls_scale          0.5409(14)
_oxford_reflns_number_all        8500
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 035CJS10
_cod_data_source_file            c0sc00511h.txt
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               1515503