Synthesis and Structural Properties of the First Macrocyclic Selenoether Complex of Arsenic(III): A Rare Example of Exo and Endo Coordination in a Single Species
Andrew J. Barton; Nicholas J. Hill; William Levason; Gillian Reid; Journal of the American Chemical Society 123 (2001) 11801–11802; doi:10.1021/ja0110527

data_4115787
_publ_contact_author_address
;
    Department of Chemistry,
    University of Southampton,
    Highfield,
    Southampton SO17 1BJ,
    UK
;
_publ_contact_author_email       ' gr@soton.ac.uk '
_publ_contact_author_fax         ' 023 80 593781 '
_publ_contact_author_name        ' Dr Gillian Reid'
_publ_contact_author_phone       ' 023 80 593609 '
_publ_section_title
;
 Synthesis and Structural Properties of the First Macrocyclic Selenoether
 Complex of Arsenic(III): A Rare Example of Exo and Endo Coordination in a
 Single Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11801
_journal_page_last               11802
_journal_paper_doi               10.1021/ja0110527
_journal_volume                  123
_journal_year                    2001
_chemical_formula_moiety         '[(AsCl3)4([24]aneSe6)]'
_chemical_formula_sum            'C18 H36 As4 Cl12 Se6'
_chemical_formula_weight         1451.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 95.71(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.227(4)
_cell_length_b                   25.656(11)
_cell_length_c                   9.808(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      12.6
_cell_volume                     2059.9(16)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction
'teXsan for Windows version 1.06 (MSC, 1997-1999)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  Shelxl-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
DIRDIF Patty (Beurskens, 1994)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'scintillation counter Rigaky AFC7S '
_diffrn_measurement_method       \w-2\q
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3899
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        -2.35
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.311
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.302
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.340
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.976
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                2449
_reflns_number_total             3635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0110527.cif
_cod_data_source_block           '_asclse6__AsCl3_+_24aneSe6'
_cod_original_cell_volume        2059.9(15)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4115787