Synthesis of chiral multidentate tertiary arsines with As4 or As6 donor atoms
Doyle, Roy J.; Habermehl, Nicole; Salem, Geoffrey; Willis, Anthony C.; Journal of the Chemical Society, Dalton Transactions  (2000) 3603–; doi:10.1039/b003981k

data_7009835
_publ_section_title
;
 Synthesis of chiral multidentate tertiary arsines with As4 or As6
 donor atoms
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3603
_journal_paper_doi               10.1039/b003981k
_journal_year                    2000
_chemical_formula_moiety
' C22 H32 As4 Cl2 Co +, F6 P -, 0.3333(C4 H10 O), 0.3333(H2 O) '
_chemical_formula_sum            'C23.333 H36 As4 Cl2 Co F6 O0.666 P'
_chemical_formula_weight         901.70
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_audit_creation_date             98-11-02
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_audit_update_record
;
2000-05-19  acw edits default cif
2000-05-19  passes checkcif tests with minor warnings
;
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                120.000
_cell_formula_units_Z            9
_cell_length_a                   21.231(2)
_cell_length_b                   21.231(2)
_cell_length_c                   18.627(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      53.28
_cell_measurement_theta_min      47.34
_cell_volume                     7271.3(15)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        xtal
_computing_molecular_graphics    xtal
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    xtal
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Rigaku AFC6R'
_diffrn_measurement_device_details
;
Rigaku AFC6R diffractometer with extended arm and
evacuated collimator and beam tunnel.
Data cannot be collected beyond \y 60 deg in this configuration.
;
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  .048
_diffrn_reflns_av_sigmaI/netI    .047
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            7345
_diffrn_reflns_reduction_process equatorial_monochr_Lp
_diffrn_reflns_theta_max         60.01
_diffrn_reflns_theta_min         3.38
_diffrn_standards_decay_%        0.
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.17
_exptl_absorpt_correction_T_max  .564
_exptl_absorpt_correction_T_min  .222
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
analytical (de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3990
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         .534
_refine_diff_density_min         -.481
_refine_ls_abs_structure_details
;
Absolute structure determined by comparative refinement.
Refinement of a model with coordinates transformed by (-x,-y,-z)
yielded R = 0.041, wR = 0.042, S = 1.518.
;
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.332
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     346
_refine_ls_number_reflns         2104
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          .043
_refine_ls_R_factor_gt           .035
_refine_ls_shift/su_max          .064
_refine_ls_shift/su_mean         .004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .04
_refine_ls_wR_factor_ref         .036
_reflns_d_resolution_high        .89
_reflns_d_resolution_low         13.051
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                2105
_reflns_number_total             2406
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            b003981k.txt
_cod_data_source_block           rxd10
_cod_original_cell_volume        7271.3(18)
_cod_original_sg_symbol_Hall     r_3
_cod_original_sg_symbol_H-M      r_3:h
_cod_original_formula_sum        ' C23.333 H36 As4 Cl2 Co F6 O0.666 P  '
_cod_database_code               7009835