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_7105711
_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_formula_moiety         'C152 H106 Au8 O2 P8, 3(C H2 Cl2), 2(F6 P)'
_chemical_formula_sum            'C155 H112 Au8 Cl6 F12 O2 P10'
_chemical_formula_weight         4332.58
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.8480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.8064(4)
_cell_length_b                   20.5555(5)
_cell_length_c                   36.4529(9)
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.60
_cell_volume                     15582.3(6)
_computing_cell_refinement       'SAINT (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_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 16
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '62mm x 62mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II DUO CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'curved graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            82208
_diffrn_reflns_theta_full        29.62
_diffrn_reflns_theta_max         29.62
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    7.770
_exptl_absorpt_correction_T_max  0.3417
_exptl_absorpt_correction_T_min  0.1793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8200
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.050
_refine_diff_density_min         -1.814
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     921
_refine_ls_number_reflns         21720
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+194.1387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                16650
_reflns_number_total             21720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC03953E.TXT
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7105711