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_4320178
_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 H54 N8) 12.64(H2 O)'
_chemical_formula_sum            'C36 H79.27 N8 O12.64'
_chemical_formula_weight         826.50
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.325(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6236(9)
_cell_length_b                   18.5875(15)
_cell_length_c                   23.978(2)
_cell_measurement_reflns_used    7176
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      2.0
_cell_volume                     4658.2(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART/P4'
_diffrn_measurement_method       '\f scan frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            14205
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9895
_exptl_absorpt_correction_T_min  0.9571
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1809
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         7714
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0587
_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          0.1534
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                5663
_reflns_number_total             7714
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010135l_4.cif
_cod_data_source_block           compound_3
_cod_database_code               4320178