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_4309021
_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+, 6Cl 1-, 5(H2 O) (C H3 O H)'
_chemical_formula_sum            'C37 H74 Cl6 N8 O6'
_chemical_formula_weight         939.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.164(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4706(6)
_cell_length_b                   15.7895(9)
_cell_length_c                   27.0054(15)
_cell_measurement_reflns_used    2741
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.92
_cell_measurement_theta_min      2.22
_cell_volume                     4798.5(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0901
_diffrn_reflns_av_sigmaI/netI    0.1672
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            30048
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        0.02
_diffrn_standards_number         89
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.9799
_exptl_absorpt_correction_T_min  0.9229
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.762
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.762
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                4575
_reflns_number_total             9438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048937esi20040803_053427_4.cif
_cod_data_source_block           compound_2_
_cod_database_code               4309021