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_4076409
_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_compound_source        local
_chemical_formula_moiety         'C3 H6 As4 I6'
_chemical_formula_sum            'C3 H6 As4 I6'
_chemical_formula_weight         1103.20
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-06-24
_audit_creation_method           CRYSTALS_ver_12.87
_audit_update_record
;
2010-06-25 - Report on C3 H6 As4 I6
             by Anthony C. Willis
             for   Di Lu and S. Bruce Wild and Geoff Salem

2010-06-25 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 94.8205(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3774(2)
_cell_length_b                   19.0852(3)
_cell_length_c                   10.0191(2)
_cell_measurement_reflns_used    89976
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     1786.77(6)
_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
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_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      200
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.074
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            35577
_diffrn_reflns_theta_full        27.403
_diffrn_reflns_theta_max         27.403
_diffrn_reflns_theta_min         2.953
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.752
_exptl_absorpt_correction_T_max  0.591
_exptl_absorpt_correction_T_min  0.166
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.101
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.30
_refine_diff_density_min         -1.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9534
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         4043
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.0010049
_refine_ls_shift/su_mean         0.00007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 165. 278. 175. 75.0 17.6 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0831
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0831
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                3585
_reflns_number_total             4044
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.86
_oxford_diffrn_Wilson_scale      35.76
_oxford_refine_ls_r_factor_ref   0.0376
_oxford_refine_ls_scale          0.24599(19)
_oxford_reflns_number_all        4043
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '6241138 sal1006'
_cod_data_source_file            om201180d_si_001.cif
_cod_data_source_block           sal1006a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 1 21/c 1 '
_cod_database_code               4076409