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_4317783
_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 Ag2 As4 P4 2+, 2(F6 P -)  '
_chemical_formula_sum            'C84 H84 Ag2 As4 F12 P6'
_chemical_formula_weight         2022.83
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_audit_creation_date             99-11-29
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_audit_update_record
;
2001-08-28  amend cif to match report
2001-08-28  passes checkcif with minor warnings

;
_cell_angle_alpha                92.057(18)
_cell_angle_beta                 95.188(14)
_cell_angle_gamma                98.234(17)
_cell_formula_units_Z            2
_cell_length_a                   12.487(2)
_cell_length_b                   12.695(4)
_cell_length_c                   27.242(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      34.23
_cell_measurement_theta_min      24.14
_cell_volume                     4251.2(16)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        xtal_DIFDAT_ABSORB_SORTRF_ADDREF
_computing_molecular_graphics    xtal
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    xtal
_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_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  .032
_diffrn_reflns_av_sigmaI/netI    .044
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12874
_diffrn_reflns_reduction_process equatorial_monochr_Lp
_diffrn_reflns_theta_max         60.25
_diffrn_reflns_theta_min         3.52
_diffrn_standards_decay_%        -20
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.07
_exptl_absorpt_correction_T_max  .84
_exptl_absorpt_correction_T_min  .44
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
analytical (de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.58
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .10
_exptl_crystal_size_min          .02
_refine_diff_density_max         .851
_refine_diff_density_min         -1.16
_refine_ls_abs_structure_details
;
Refinement of a model with coordinates transformed by (-x, -y, -z) 
yielded significantly inferior agreement factors (R = 0.069, Rw = 
0.090, GOF = 1.91) establishing that the original model shows the 
absolute configuration.  It is also in agreement with the known 
chirality of the ligand.
;
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.556
_refine_ls_goodness_of_fit_ref   1.704
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     819
_refine_ls_number_reflns         9216
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          .085
_refine_ls_R_factor_gt           .062
_refine_ls_shift/su_max          .113
_refine_ls_shift/su_mean         .008
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.0009|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .087
_refine_ls_wR_factor_ref         .08
_reflns_d_resolution_high        .888
_reflns_d_resolution_low         12.549
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              0
_reflns_limit_k_min              -14
_reflns_limit_l_max              30
_reflns_limit_l_min              -30
_reflns_number_gt                9216
_reflns_number_total             12601
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ic010988d_3.cif
_cod_data_source_block           vcc4
_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_cell_volume        4251.3(16)
_cod_original_sg_symbol_Hall     p_1
_cod_original_formula_sum        'C84 H84 Ag2 As4 F12 P6 '
_cod_database_code               4317783