Do Spiroarsoranes Exhibit Polytopal Equilibrium in Solution?
Antonio R. Tapia-Benavides; Luis H. Mendoza-Huizar; Francisco Pérez-García; Hugo Tlahuext; Alejandro Alvarez; Margarita Tlahuextl; Inorganic Chemistry 49 (2010) 1496–1502; doi:10.1021/ic901740d

data_4314766
_publ_contact_author_email       tromero@uaeh.edu.mx
_publ_contact_author_name        'Margarita Tlahuextl'
_publ_section_title
;
 Do Spiroarsoranes Exhibit Polytopal Equilibrium in Solution?
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1496
_journal_page_last               1502
_journal_paper_doi               10.1021/ic901740d
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C24 H27 As N2 O2'
_chemical_formula_sum            'C24 H27 As N2 O2'
_chemical_formula_weight         450.40
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2009-08-29 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.499(2)
_cell_length_b                   5.9685(12)
_cell_length_c                   17.833(4)
_cell_measurement_reflns_used    3838
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      3.61
_cell_volume                     1117.4(4)
_computing_cell_refinement       'SAINT-Plus NT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus NT'
_computing_molecular_graphics    SHELXTL-NT
_computing_structure_refinement  SHELXTL-NT
_computing_structure_solution    'SHELXTL-NT (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6883
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.14
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.542
_exptl_absorpt_correction_T_max  0.8365
_exptl_absorpt_correction_T_min  0.4953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
; 
The absolute configuration was assigned to agree with the known
chirality at C4 and C5 arising from its precursor (+)-Norephedrine
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3838
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0486
_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^)+(0.1004P)^2^+0.3138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1527
_reflns_number_gt                2183
_reflns_number_total             3838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901740d_si_002.cif
_cod_data_source_block           pefpacom
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1117.3(4)
_cod_database_code               4314766