Synthesis of cyclo-2,4,6-Triarsa-1,3,5-triazanes from cyclo-2,4-Diarsa-1,3-diazanes Demonstrating the General Influence of Substituent Steric Strain on the Relative Stability of Pnictazane Oligomers
Neil Burford; Jeff C. Landry; Michael J. Ferguson; Robert McDonald; Inorganic Chemistry 44 (2005) 5897–5902; doi:10.1021/ic050532m

data_4309356
_publ_contact_author_address
;Department of Chemistry
Dalhousie University
Halifax, NS
CANADA
B3H 4J3
;
_publ_contact_author_email       neil.burford@dal.ca
_publ_contact_author_fax         902-494-1310
_publ_contact_author_name        'Neil Burford'
_publ_contact_author_phone       902-494-3190
_publ_section_title
;
Synthesis of cyclo-2,4,6-Triarsa-1,3,5-triazanes
from cyclo-2,4-Diarsa-1,3-diazanes Demonstrating the General Influence of
Substituent Steric Strain on the Relative Stability of Pnictazane Oligomers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5897
_journal_page_last               5902
_journal_paper_doi               10.1021/ic050532m
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C36 H51 As3 Cl3 N3'
_chemical_formula_sum            'C36 H51 As3 Cl3 N3'
_chemical_formula_weight         856.91
_chemical_melting_point          418.5(15)
_chemical_name_common            'DippNAsCl trimer'
_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                 111.852(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2049(14)
_cell_length_b                   21.386(2)
_cell_length_c                   16.3283(19)
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.364
_cell_measurement_theta_min      2.332
_cell_volume                     3955.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30028
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.65
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.750
_exptl_absorpt_correction_T_max  0.8100
_exptl_absorpt_correction_T_min  0.4059
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   emperical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+0.7467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0752
_reflns_number_gt                6329
_reflns_number_total             8104
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050532msi20050407_085836_5.cif
_cod_data_source_block           dal04g2
_cod_depositor_comments
;
The following automatic conversions were performed:
_chemical_melting_point value '417-420' changed to '418.5(15)' - took
average value and fixed precision.
Automatic conversion script
Id: cif_fix_values 1391 2010-09-07 12:51:13Z saulius 
;
_cod_original_cell_volume        3955.7(8)
_cod_database_code               4309356