A Ditopic Azacryptate Proton Cage
Paula Morehouse; Md. Alamgir Hossain; José M. Llinares; Douglas Powell; Kristin Bowman-James; Inorganic Chemistry 42 (2003) 8131–8133; doi:10.1021/ic034972u

data_4312734
_publ_contact_author
; 
   Prof. Kristin Bowman-James
   Department of Chemistry 
   University of Kansas 
   Malott Hall, Room 2010
   1251 Wescoe Hall Dr. 
   Lawrence, KS  66045-7582  USA 
;
_publ_contact_author_email       kbowman-james@ku.edu
_publ_contact_author_fax         1(785)8645396
_publ_contact_author_phone       1(785)8644278
_publ_section_title
;
 A Ditopic Azacryptate Proton Cage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8131
_journal_page_last               8133
_journal_paper_doi               10.1021/ic034972u
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety
'(C78 H90 N8 O12 S6), (C2 H3 N)1.5, (C H Cl3)0.183'
_chemical_formula_sum            'C81.18 H94.68 Cl0.55 N9.5 O12 S6'
_chemical_formula_weight         1607.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   21.9335(6)
_cell_length_b                   21.9335(6)
_cell_length_c                   65.463(3)
_cell_measurement_reflns_used    7415
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.54
_cell_measurement_theta_min      2.23
_cell_volume                     27273.6(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w scan frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       80
_diffrn_reflns_limit_l_min       -80
_diffrn_reflns_number            58095
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        -0.11
_diffrn_standards_number         286
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.9605
_exptl_absorpt_correction_T_min  0.9478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, 1996'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             10196
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         11906
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2124
_reflns_number_gt                4885
_reflns_number_total             11906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034972usi20030815_122818_2.cif
_cod_data_source_block           compound_L_
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C81.18 H94.68 Cl0.55 N9.50 O12 S6'
_cod_database_code               4312734