Tritopic (Cascade) and Ditopic Complexes of Halides with an Azacryptand
Md. Alamgir Hossain; Paula Morehouse; Douglas Powell; Kristin Bowman-James; Inorganic Chemistry 44 (2005) 2143–2149; doi:10.1021/ic048937e

data_4309022
_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
;
Tritopic (Cascade) and Ditopic Complexes of Halides with an Azacryptand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2143
_journal_page_last               2149
_journal_paper_doi               10.1021/ic048937e
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety
'C36 H60 N8 6+, 2(H2 P O4) 1-, 4 Cl 1-, 7.5(H2 O), 0.25(C2 H6 O)'
_chemical_formula_sum            'C36.5 H80.5 Cl4 N8 O15.75 P2'
_chemical_formula_weight         1087.33
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 90.456(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   30.9882(17)
_cell_length_b                   20.6547(11)
_cell_length_c                   32.8991(18)
_cell_measurement_reflns_used    5514
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.20
_cell_volume                     21056(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            59671
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.71
_diffrn_standards_number         325
_exptl_absorpt_coefficient_mu    0.355
_exptl_absorpt_correction_T_max  0.9790
_exptl_absorpt_correction_T_min  0.9134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             9272
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.437
_refine_diff_density_min         -1.373
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1305
_refine_ls_number_reflns         18493
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.1067
_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^)+(0.1300P)^2^+252.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2839
_refine_ls_wR_factor_ref         0.3049
_reflns_number_gt                13177
_reflns_number_total             18493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048937esi20040803_053427_5.cif
_cod_data_source_block           compound_2A_
_cod_original_formula_sum        'C36.50 H80.50 Cl4 N8 O15.75 P2'
_cod_database_code               4309022