Multiple Hydrogen Bond Stabilization of a Sandwich Complex of Sulfate between Two Macrocyclic Tetraamides
Md. Alamgir Hossain; José M. Llinares; Douglas Powell; Kristin Bowman-James; Inorganic Chemistry 40 (2001) 2936–2937; doi:10.1021/ic015508x

data_4319885
_publ_contact_author
; 
   Prof. Kristin Bowman-James
   Department of Chemistry 
   University of Kansas 
   2010 Malott Hall 
   1251 Wescoe Hall Drive
   Lawrence, KS  66045-7582  USA 
;
_publ_contact_author_email       @ukans.edu
_publ_contact_author_fax         1(785)8645396
_publ_contact_author_phone       1(785)8643669
_publ_section_title
;
 Multiple Hydrogen Bond Stabilization of a Sandwich Complex of Sulfate
 between Two Macrocyclic Tetraamides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2936
_journal_page_last               2937
_journal_paper_doi               10.1021/ic015508x
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety
'2(C16 H36 N)+ 2(C26 H34 N6 O4).(S O4)2- 2(H2 O) 0.5(C4 H10 O)'
_chemical_formula_sum            'C86 H149 N14 O14.5 S'
_chemical_formula_weight         1643.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.214(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.299(4)
_cell_length_b                   18.902(4)
_cell_length_c                   16.313(4)
_cell_measurement_reflns_used    1493
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      25.22
_cell_measurement_theta_min      2.48
_cell_volume                     5026(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART/P4 diffractometer'
_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  0.0966
_diffrn_reflns_av_sigmaI/netI    0.3358
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28931
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        0.55
_diffrn_standards_number         25
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9815
_exptl_absorpt_correction_T_min  0.9724
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1790
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.18(15)
_refine_ls_extinction_coef       0.00151(16)
_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   0.708
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         16001
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      0.709
_refine_ls_R_factor_all          0.2349
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1697
_reflns_number_gt                4278
_reflns_number_total             16001
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic015508x_s2.cif
_cod_data_source_block           bj400
_cod_original_formula_sum        'C86 H149 N14 O14.50 S'
_cod_database_code               4319885