Anion Binding with Two Polyammonium Macrocycles of Different Dimensionality
Thomas Clifford; Andrew Danby; José M. Llinares; Susan Mason; Nathaniel W. Alcock; Douglas Powell; Juan A. Aguilar; Enrique García-España; Kristin Bowman-James; Inorganic Chemistry 40 (2001) 4710–4720; doi:10.1021/ic010135l

data_4320175
_publ_contact_author
;
    Prof. Kristin Bowman-James
    Department of Chemistry
    University of Kansas
    2010 Malott Hall
    1251 Wescoe Hall Dr.
    Lawrence, KS  66045-7582  USA
;
_publ_contact_author_email       kbowmanjames@ku.edu
_publ_contact_author_fax         1(785)8645396
_publ_contact_author_phone       1(785)8644673
_publ_section_title
;
 Anion Binding with Two Polyammonium Macrocycles of Different
 Dimensionality
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4710
_journal_page_last               4720
_journal_paper_doi               10.1021/ic010135l
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '(C36 H60 N8)6+ 6(C7 H7 O3 S)- 8(H2 O)'
_chemical_formula_sum            'C78 H118 N8 O26 S6'
_chemical_formula_weight         1776.16
_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                79.04(2)
_cell_angle_beta                 82.05(2)
_cell_angle_gamma                83.39(2)
_cell_formula_units_Z            2
_cell_length_a                   13.726(2)
_cell_length_b                   14.990(3)
_cell_length_c                   22.818(4)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.47
_cell_measurement_theta_min      17.01
_cell_volume                     4545.9(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       '\q-2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.1308
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14130
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         60.07
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        4.62
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.033
_exptl_absorpt_correction_T_max  0.8226
_exptl_absorpt_correction_T_min  0.6866
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.00052(10)
_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   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1068
_refine_ls_number_reflns         13530
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1807
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1980
_refine_ls_wR_factor_ref         0.2388
_reflns_number_gt                6773
_reflns_number_total             13530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010135l_1.cif
_cod_data_source_block           compound_5
_cod_database_code               4320175