Synthesis and Resolution of (R*,R*)-(\±)-1,1,4,7,10,10-Hexaphenyl-1,10-diarsa-4,7-diphosphadecane: New Ligand for the Stereoselective Self-Assembly of Dicopper(I), Disilver(I), and Digold(I) Helicates
Vernon C. Cook; Anthony C. Willis; Johann Zank; S. Bruce Wild; Inorganic Chemistry 41 (2002) 1897–1906; doi:10.1021/ic010988d

data_4317782
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       ' sbw@rsc.anu.edu.au '
_publ_contact_author_fax         ' 61 2 6125 0750 '
_publ_contact_author_name        '  S. Bruce Wild  '
_publ_contact_author_phone       ' 61 2 6125 4236 '
_publ_section_title
;
 Synthesis and Resolution of
 (R*,R*)-(\+-)-1,1,4,7,10,10-Hexaphenyl-1,10-diarsa-4,7-diphosphadecane:
 New Ligand for the Stereoselective Self-Assembly of Dicopper(I),
 Disilver(I), and Digold(I) Helicates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1897
_journal_page_last               1906
_journal_paper_doi               10.1021/ic010988d
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C84 H84 As4 Au2 P4 2+, 2(F6 P -) '
_chemical_formula_sum            'C84 H84 As4 Au2 F12 P6'
_chemical_formula_weight         2201.03
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             1997-10-02
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
2001-08-28  amend cif to match report
2001-08-28  passes checkcif with minor warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.199(4)
_cell_length_b                   18.373(4)
_cell_length_c                   29.347(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      54.5
_cell_measurement_theta_min      51.0
_cell_volume                     8734(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      296.2
_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      0.00047
_diffrn_orient_matrix_UB_12      0.05338
_diffrn_orient_matrix_UB_13      -0.00665
_diffrn_orient_matrix_UB_21      -0.00266
_diffrn_orient_matrix_UB_22      0.01063
_diffrn_orient_matrix_UB_23      0.03339
_diffrn_orient_matrix_UB_31      0.06167
_diffrn_orient_matrix_UB_32      0.00005
_diffrn_orient_matrix_UB_33      0.00149
_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    0.060
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7142
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.07
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        -4.52
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.643
_exptl_absorpt_correction_T_max  0.307
_exptl_absorpt_correction_T_min  0.180
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
analytical (de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4304.00
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.11
_refine_diff_density_min         -0.47
_refine_ls_abs_structure_details
;
The absolute structure has been established by refining the structure
with coordinates transformed by the operation (-x,-y,-z);
the final agreement factors for that hand were R = 0.057
and Rw = 0.069.

;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.600
_refine_ls_goodness_of_fit_ref   1.666
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    17
_refine_ls_number_parameters     962
_refine_ls_number_reflns         6272
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.0280
_refine_ls_shift/su_mean         0.0170
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0426
_refine_ls_wR_factor_ref         0.0413
_reflns_number_gt                6272
_reflns_number_total             7142
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ic010988d_2.cif
_cod_data_source_block           Vcc3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C84 H84 As4 Au2 F12 P6 '
_cod_database_code               4317782