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_7009837
_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
'C32 H48 As6 Co 3+, (F6 P -)3, C3 H6 O, 0.31(H2 O)'
_chemical_formula_sum            'C35 H54.62 As6 Co F18 O1.31 P3'
_chemical_formula_weight         1439.75
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_date             1999-03-10
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
2000-05-19  acw edits cif
2000-05-19  passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.080(3)
_cell_length_b                   24.057(4)
_cell_length_c                   31.300(4)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    193.2
_cell_measurement_theta_max      54.8
_cell_measurement_theta_min      53.1
_cell_volume                     9849(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      193.2
_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_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00796
_diffrn_orient_matrix_UB_12      0.03899
_diffrn_orient_matrix_UB_13      -0.01057
_diffrn_orient_matrix_UB_21      -0.04967
_diffrn_orient_matrix_UB_22      0.01314
_diffrn_orient_matrix_UB_23      0.02209
_diffrn_orient_matrix_UB_31      0.05758
_diffrn_orient_matrix_UB_32      0.00594
_diffrn_orient_matrix_UB_33      0.02052
_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  0.00000
_diffrn_reflns_av_sigmaI/netI    0.070
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8059
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.05
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        -1.47
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.047
_exptl_absorpt_correction_T_max  0.344
_exptl_absorpt_correction_T_min  0.232
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
analytical (de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_meas      ?
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             5656.80
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.15
_refine_diff_density_min         -0.92
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.908
_refine_ls_goodness_of_fit_ref   2.133
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     581
_refine_ls_number_reflns         5385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.0590
_refine_ls_shift/su_mean         0.0060
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0574
_refine_ls_wR_factor_ref         0.0542
_reflns_number_gt                5385
_reflns_number_total             7312
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            b003981k.txt
_cod_data_source_block           rxd12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00010|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P b c a    '
_cod_original_formula_sum        'C35 H54.62 As6 Co F18 O1.31 P3 '
_cod_database_code               7009837