Aurophilicity in action: stepwise formation of dinuclear Au(i) macrocycles with rigid 1,8-dialkynylanthracenes.
Niermeier, Philipp; Wickemeyer, Lucas; Neumann, Beate; Stammler, Hans-Georg; Goett-Zink, Lukas; Kottke, Tilman; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4109–4113; doi:10.1039/c8dt04783a

data_7049167
_publ_section_title
;
 Aurophilicity in action: stepwise formation of dinuclear Au(i)
 macrocycles with rigid 1,8-dialkynylanthracenes.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4109
_journal_page_last               4113
_journal_paper_doi               10.1039/c8dt04783a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C60 H50 Au2 P2'
_chemical_formula_sum            'C60 H50 Au2 P2'
_chemical_formula_weight         1226.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-04-25
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2018-11-13 deposited with the CCDC.    2019-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.7936(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6517(2)
_cell_length_b                   12.1844(2)
_cell_length_c                   26.4203(5)
_cell_measurement_reflns_used    45914
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.7290
_cell_measurement_theta_min      2.8540
_cell_volume                     4991.98(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9886
_diffrn_measured_fraction_theta_max 0.9796
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -63.00  32.00   1.00    5.00    --  -40.83  38.00-120.00   95
  2  \w    -67.00  29.00   1.00    5.00    --  -40.83  57.00  90.00   96
  3  \w   -111.00 -14.00   1.00    5.00    --  -40.83 -57.00 -60.00   97
  4  \w      4.00 119.00   1.00    5.00    --   40.83  19.00 -30.00  115
  5  \w     57.00 128.00   1.00    5.00    --   40.83 178.00  30.00   71
  6  \w     57.00 128.00   1.00    5.00    --   40.83 178.00-120.00   71
  7  \w     30.00 109.00   1.00   27.50    --  111.00 -94.00 -90.00   79
  8  \w     41.00 139.00   1.00   27.50    --  111.00 -61.00  60.00   98
  9  \w     87.00 178.00   1.00   27.50    --  111.00  30.00  30.00   91
 10  \w     36.00 135.00   1.00   27.50    --  111.00 -30.00 120.00   99
 11  \w     39.00 121.00   1.00   27.50    --  111.00-125.00-150.00   82
 12  \w     36.00 135.00   1.00   27.50    --  111.00 -30.00-150.00   99
 13  \w     41.00 139.00   1.00   27.50    --  111.00 -61.00 -60.00   98
 14  \w     39.00 121.00   1.00   27.50    --  111.00-125.00  90.00   82
 15  \w     31.00 156.00   1.00   27.50    --  111.00 -15.00   0.00  125
 16  \w     30.00 109.00   1.00   27.50    --  111.00 -94.00  60.00   79
 17  \w     30.00 109.00   1.00   27.50    --  111.00 -94.00-150.00   79
 18  \w   -115.00  -9.00   1.00    5.00    --  -40.83 -77.00  90.00  106
 19  \w    -67.00  29.00   1.00    5.00    --  -40.83  57.00   0.00   96
 20  \w   -111.00 -14.00   1.00    5.00    --  -40.83 -57.00 120.00   97
 21  \w   -111.00 -14.00   1.00    5.00    --  -40.83 -57.00-150.00   97
 22  \w   -111.00 -14.00   1.00    5.00    --  -40.83 -57.00  30.00   97
 23  \w     66.00 178.00   1.00   27.50    --  111.00  15.00 120.00  112
 24  \w     83.00 178.00   1.00   27.50    --  111.00  61.00 -90.00   95
 25  \w     87.00 178.00   1.00   27.50    --  111.00  30.00-180.00   91
 26  \w     83.00 178.00   1.00   27.50    --  111.00  61.00 120.00   95
 27  \w     83.00 178.00   1.00   27.50    --  111.00  61.00 -30.00   95
 28  \w     83.00 178.00   1.00   27.50    --  111.00  61.00 -60.00   95
 29  \w     83.00 178.00   1.00   27.50    --  111.00  61.00-180.00   95
 30  \w     83.00 178.00   1.00   27.50    --  111.00  61.00  30.00   95
 31  \w     83.00 178.00   1.00   27.50    --  111.00  61.00-120.00   95
 32  \w     66.00 178.00   1.00   27.50    --  111.00  15.00 -90.00  112
 33  \w   -115.00  -9.00   1.00    5.00    --  -40.83 -77.00 -30.00  106
 34  \w   -115.00  -9.00   1.00    5.00    --  -40.83 -77.00-180.00  106
 35  \w   -115.00  -9.00   1.00    5.00    --  -40.83 -77.00-120.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0139661000
_diffrn_orient_matrix_UB_12      -0.0041804000
_diffrn_orient_matrix_UB_13      0.0588521000
_diffrn_orient_matrix_UB_21      -0.0973687000
_diffrn_orient_matrix_UB_22      0.0169783000
_diffrn_orient_matrix_UB_23      0.0005629000
_diffrn_orient_matrix_UB_31      -0.0136189000
_diffrn_orient_matrix_UB_32      -0.1252023000
_diffrn_orient_matrix_UB_33      -0.0019186000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            84443
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.344
_diffrn_reflns_theta_min         2.850
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.778
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.310
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       plate
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.023
_refine_diff_density_max         2.740
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         9736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+53.1471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9463
_reflns_number_total             9736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04783a2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 7049167--7049169.cif.'
_cod_original_cell_volume        4991.99(15)
_cod_database_code               7049167
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C60 H50 Au2 P2'
_reflns_odcompleteness_completeness 98.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelx_res_checksum              19203
_shelx_hkl_checksum              67635
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.144