Novel stereochemistry, reactivity, and stability of an arsenic heterocycle in a metal-promoted asymmetric cycloaddition reaction.
Ma, Mengtao; Pullarkat, Sumod A.; Li, Yongxin; Leung, Pak-Hing; Inorganic chemistry 46 (2007) 9488–9494; doi:10.1021/ic701419j

data_4338969
_publ_section_title
;
 Novel stereochemistry, reactivity, and stability of an arsenic
 heterocycle in a metal-promoted asymmetric cycloaddition reaction.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9488
_journal_page_last               9494
_journal_paper_doi               10.1021/ic701419j
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C36.5 H40.5 As Cl2.5 N O4 P Pd'
_chemical_formula_weight         858.11
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.513(2)
_cell_angle_beta                 103.462(2)
_cell_angle_gamma                100.6610(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9874(3)
_cell_length_b                   10.4103(3)
_cell_length_c                   18.6414(7)
_cell_measurement_reflns_used    8762
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     1841.32(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  '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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50592
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    1.660
_exptl_absorpt_correction_T_max  0.8009
_exptl_absorpt_correction_T_min  0.5943
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.039
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         21041
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+0.3998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0656
_reflns_number_gt                20010
_reflns_number_total             21041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701419j2.cif
_cod_data_source_block           leung83a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1841.32(10)
_cod_original_sg_symbol_H-M      P1
_cod_original_formula_sum        'C36.50 H40.50 As Cl2.50 N O4 P Pd'
_cod_database_code               4338969