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_7049168
_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         'C84 H124 Au4 P4'
_chemical_formula_sum            'C84 H124 Au4 P4'
_chemical_formula_weight         2045.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-13 deposited with the CCDC.    2019-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                117.469(11)
_cell_angle_beta                 97.066(10)
_cell_angle_gamma                96.219(10)
_cell_formula_units_Z            1
_cell_length_a                   11.2609(13)
_cell_length_b                   14.3119(17)
_cell_length_c                   14.3796(12)
_cell_measurement_reflns_used    3196
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.7930
_cell_measurement_theta_min      3.5040
_cell_volume                     2004.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.978
_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    -91.00 -15.00   1.00   27.61    --  -42.08 -57.00  90.00   76
  2  \w   -118.00  -5.00   1.00   27.61    --  -42.08 -19.00 150.00  113
  3  \w    -51.00  29.00   1.00   27.61    --  -42.08  38.00 -30.00   80
  4  \w     84.00 125.00   1.00   27.61    --   42.08-178.00 -30.00   41
  5  \w     58.00 123.00   1.00   27.61    --   42.08 178.00 120.00   65
  6  \w     72.00 114.00   1.00   90.00    --  108.91 -45.00  90.00   42
  7  \w     85.00 178.00   1.00   90.00    --  108.91  30.00 -90.00   93
  8  \w     45.00 134.00   1.00   90.00    --  108.91 -61.00-180.00   89
  9  \w     28.00 103.00   1.00   90.00    --  108.91 -94.00 150.00   75
 10  \w     53.00 121.00   1.00   90.00    --  108.91-125.00  30.00   68
 11  \w     94.00 173.00   1.00   90.00    --  108.91 125.00-180.00   79
 12  \w    106.00 131.00   1.00   90.00    --  108.91 125.00  60.00   25
 13  \w    150.00 175.00   1.00   90.00    --  108.91 125.00  60.00   25
 14  \w     78.00 154.00   1.00   90.00    --  108.91  77.00   0.00   76
 15  \w     93.00 120.00   1.00   90.00    --  108.91-125.00-120.00   27
 16  \w     86.00 163.00   1.00   90.00    --  108.91  61.00 150.00   77
 17  \w     94.00 142.00   1.00   90.00    --  108.91 125.00  90.00   48
 18  \w    109.00 178.00   1.00   90.00    --  108.91 125.00-150.00   69
;
_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      -0.0430372000
_diffrn_orient_matrix_UB_12      -0.0692502000
_diffrn_orient_matrix_UB_13      0.0500057000
_diffrn_orient_matrix_UB_21      0.1293987000
_diffrn_orient_matrix_UB_22      0.0273346000
_diffrn_orient_matrix_UB_23      0.0661521000
_diffrn_orient_matrix_UB_31      -0.0331592000
_diffrn_orient_matrix_UB_32      0.0985478000
_diffrn_orient_matrix_UB_33      0.0910319000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_unetI/netI     0.1191
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13679
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.104
_diffrn_reflns_theta_min         3.533
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.506
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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    1.695
_exptl_crystal_description       needle
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.044
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.016
_refine_diff_density_max         3.634
_refine_diff_density_min         -4.846
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         7736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0746P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5119
_reflns_number_total             7736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04783a2.cif
_cod_data_source_block           compound_5
_cod_depositor_comments
'Adding full bibliography for 7049167--7049169.cif.'
_cod_database_code               7049168
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C48 H99 Au2'
_reflns_odcompleteness_completeness 97.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.20
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B),
  C37(H37A,H37B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C34(H34A,H34B,
 H34C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              56868
_shelx_hkl_checksum              12283
_olex2_date_sample_data_collection 2018-01-16
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.765
_oxdiff_exptl_absorpt_empirical_full_min 0.622