Azolium-Linked Cyclophanes: Effects of Structure, Solvent, and Counteranions on Solution Conformation Behavior
Murray V. Baker; David H. Brown; Charles H. Heath; Brian W. Skelton; Allan H. White; Charlotte C. Williams; Journal of Organic Chemistry 73 (2008) 9340–9352; doi:10.1021/jo801860d

data_4023905
_publ_contact_author_address
;
   Department of Chemistry
   University of Western Australia
   35 Stirling Highway
   Crawley
   Western Australia 6009
   Australia
;
_publ_contact_author_email       bws@crystal.uwa.edu.au
_publ_contact_author_fax         (+61)_08_6488_1118
_publ_contact_author_name        'Skelton, B. W.'
_publ_contact_author_phone       (+61)_08_6488_7107
_publ_section_title
;
 Azolium-Linked Cyclophanes: Effects of Structure, Solvent,
 and Counteranions on Solution Conformation Behavior
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9340
_journal_page_last               9352
_journal_paper_doi               10.1021/jo801860d
_journal_volume                  73
_journal_year                    2008
_chemical_formula_moiety         'C46 H58 N4 O4, 4(H2 O), 2(Br)'
_chemical_formula_sum            'C46 H66 Br2 N4 O8'
_chemical_formula_weight         962.86
_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'
_audit_creation_date             05-11-11
_audit_creation_method           Xtal3.6
_cell_angle_alpha                90.00000
_cell_angle_beta                 126.3340(10)
_cell_angle_gamma                90.00000
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_cell_length_a                   20.524(2)
_cell_length_b                   20.512(2)
_cell_length_c                   13.6070(10)
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_cell_measurement_theta_max      32.65
_cell_measurement_theta_min      2.72
_cell_volume                     4614.7(7)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
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_computing_structure_solution    xtal
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_diffrn_measured_fraction_theta_full 1
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_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
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_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31846
_diffrn_reflns_theta_full        33.2
_diffrn_reflns_theta_max         33.2
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.812
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          .55
_exptl_crystal_size_mid          .38
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_refine_diff_density_max         .634
_refine_diff_density_min         -.593
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
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_refine_ls_number_reflns         8619
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .046
_refine_ls_R_factor_gt           .034
_refine_ls_shift/su_max          .007
_refine_ls_shift/su_mean         .0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .063
_refine_ls_wR_factor_ref         .08
_reflns_d_resolution_high        .645
_reflns_d_resolution_low         12.839
_reflns_Friedel_coverage         0
_reflns_limit_h_max              31
_reflns_limit_h_min              0
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_reflns_limit_k_min              0
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_reflns_limit_l_min              -20
_reflns_number_gt                6926
_reflns_number_total             8619
_reflns_threshold_expression     'I >  2.00 sig(I)'
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_cod_database_code               4023905