Resolution and Improved Synthesis of (±)-Arsenicin A: A Natural Adamantane-Type Tetraarsenical Possessing Strong Anti-Acute Promelocytic Leukemia Cell Line Activity
Lu, Di; Coote, Michelle L.; Ho, Junming; Kilah, Nathan L.; Lin, Ching-Yeh; Salem, Geoff; Weir, Michelle L.; Willis, Anthony C.; Wild, S. Bruce; Dilda, Pierre J.; Organometallics 31 (2012) 1808–; doi:10.1021/om201180d

data_4076410
_publ_section_title
;
 Resolution and Improved Synthesis of (+-)-Arsenicin A: A Natural
 Adamantane-Type Tetraarsenical Possessing Strong Anti-Acute Promelocytic
 Leukemia Cell Line Activity
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1808
_journal_paper_doi               10.1021/om201180d
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_compound_source        local
_chemical_formula_moiety         'C3 H6 As4 O3'
_chemical_formula_sum            'C3 H6 As4 O3'
_chemical_formula_weight         389.77
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-01-14
_audit_creation_method           CRYSTALS_ver_12.87
_audit_update_record
;
2010-01-14 - Report on (-) C3 H6 As4 O3
             by Anthony C. Willis
             for   Di Lu and S. Bruce Wild and Geoff Salem

2010-01-141 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8594(3)
_cell_length_b                   9.8038(5)
_cell_length_c                   12.3203(6)
_cell_measurement_reflns_used    39340
_cell_measurement_temperature    150
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2.6
_cell_volume                     828.52(7)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9310
_diffrn_reflns_theta_full        28.524
_diffrn_reflns_theta_max         30.025
_diffrn_reflns_theta_min         2.655
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.940
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.188
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.08
_refine_diff_density_min         -1.24
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       18(3)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0708
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2365
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.0006574
_refine_ls_shift/su_mean         0.5303434
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 1.45P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0835
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0835
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                2140
_reflns_number_total             2365
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.02
_oxford_diffrn_Wilson_scale      7.35
_oxford_refine_ls_r_factor_ref   0.0414
_oxford_refine_ls_scale          0.4652(10)
_oxford_reflns_number_all        2365
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '1131631 wil1002'
_cod_data_source_file            om201180d_si_002.cif
_cod_data_source_block           wil1002
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4076410