Assembly of the Audiphosphine helical cage molecules via alkynyl?4-methylydine ligand transformation (C152 H142 Au8 F12 N2 O5 P10 and C155 H112 Au8 Cl6 F12 O2 P10)
Igor Koshevoy; Matti Haukka; Stanislav Selivanov; Sergey Tunik; Tapani Pakkanen; Chem.Commun. 46 (2010) 8926–; doi:10.1039/c0cc03953e

data_7105710
_publ_section_title
;
Assembly of the Au&#x0096;diphosphine helical cage molecules via 
alkynyl&#x0096;?4-methylydine ligand transformation 
(C152 H142 Au8 F12 N2 O5 P10 and C155 H112 Au8 Cl6 F12 O2 P10)
;
_journal_name_full               Chem.Commun.
_journal_page_first              8926
_journal_paper_doi               10.1039/c0cc03953e
_journal_volume                  46
_journal_year                    2010
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C136 H106 Au8 O2 P8, 3(C4 H10 O), 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C152 H142 Au8 F12 N2 O5 P10'
_chemical_formula_weight         4190.11
_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                69.282(7)
_cell_angle_beta                 75.031(7)
_cell_angle_gamma                63.004(6)
_cell_formula_units_Z            1
_cell_length_a                   15.7044(2)
_cell_length_b                   15.9465(2)
_cell_length_c                   17.4245(2)
_cell_measurement_reflns_used    55741
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.00
_cell_volume                     3611.6(2)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2008)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond v.3.2e (Brandenburg, 2010)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            73258
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    8.272
_exptl_absorpt_correction_T_max  0.1933
_exptl_absorpt_correction_T_min  0.1230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1998
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.099
_refine_diff_density_min         -2.447
_refine_diff_density_rms         0.191
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.367(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1711
_refine_ls_number_reflns         38565
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0174P)^2^+1.6079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0575
_reflns_number_gt                35982
_reflns_number_total             38565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC03953E.TXT
_cod_data_source_block           1
_cod_database_code               7105710