Selective formation of gold(i) bis-phospholane macrocycles, polymeric chains, and nanotubes.
Streitberger, Markus; Schmied, Andy; Hey-Hawkins, Evamarie; Inorganic chemistry 53 (2014) 6794–6804; doi:10.1021/ic5006055

data_4340020
_publ_section_title
;
 Selective formation of gold(i) bis-phospholane macrocycles, polymeric
 chains, and nanotubes.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6794
_journal_page_last               6804
_journal_paper_doi               10.1021/ic5006055
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C35.75 H71.5 Au2 Cl5.5 P4'
_chemical_formula_weight         1214.22
_space_group_IT_number           2
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-29T15:23:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                104.162(3)
_cell_angle_beta                 100.406(2)
_cell_angle_gamma                96.329(2)
_cell_formula_units_Z            4
_cell_length_a                   12.5845(3)
_cell_length_b                   19.8177(6)
_cell_length_c                   20.1551(6)
_cell_measurement_reflns_used    15998
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.4549
_cell_measurement_theta_min      2.9195
_cell_volume                     4730.4(2)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'ORTEP3 for Windows (L. J. Farrugia, 1997)'
_computing_publication_material  'WINGX  (L.J. Farrugia,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo 1993)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0571793
_diffrn_orient_matrix_UB_12      0.0109852
_diffrn_orient_matrix_UB_13      0.0052342
_diffrn_orient_matrix_UB_21      0.0084326
_diffrn_orient_matrix_UB_22      -0.0355203
_diffrn_orient_matrix_UB_23      -0.0047513
_diffrn_orient_matrix_UB_31      -0.0056379
_diffrn_orient_matrix_UB_32      -0.0041112
_diffrn_orient_matrix_UB_33      -0.0364892
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38840
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    6.665
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.5859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             2390
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Based on the total SQUEEZE electron count of 359 removed electrons, 4 missing
and unresolved chloride anions (68 electrons) and 7 dichlormethane solvent
molecules (294 electrons) had been removed with the SQUEEZE routine
implemented in PLATON (68 + 294 = 362 electrons). For each non-hydrogen atom
a volume of 41A^3^ can be deduced from the total void volume calculated by
SQUEEZE. This value is relatively high, but acceptable for loosly packed
solvent moieties.
;
_refine_diff_density_max         1.455
_refine_diff_density_min         -2.38
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         19316
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+27.0683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                15588
_reflns_number_total             19316
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5006055_si_003.cif
_cod_data_source_block           x1487fin
_cod_depositor_comments
'Adding full bibliography for 4340012--4340022.cif.'
_cod_original_sg_symbol_H-M      p-1
_cod_original_formula_sum        'C35.75 H71.50 Au2 Cl5.50 P4'
_cod_database_code               4340020