Aurophilicity under pressure: a combined crystallographic and in situ spectroscopic study.
O'Connor, Alice E; Mirzadeh, Nedaossadat; Bhargava, Suresh K.; Easun, Timothy L.; Schröder, Martin; Blake, Alexander J.; Chemical communications (Cambridge, England) 52 (2016) 6769–6772; doi:10.1039/c6cc00923a

data_7118884
_publ_section_title
;
 Aurophilicity under pressure: a combined crystallographic and in situ
 spectroscopic study.
;
_journal_issue                   41
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6769
_journal_page_last               6772
_journal_paper_doi               10.1039/c6cc00923a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         '0.5(C60 H48 Au4 Cl4 P4)'
_chemical_formula_sum            'C30 H24 Au2 Cl2 P2'
_chemical_formula_weight         911.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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
_audit_creation_date             2014-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.25 svn.r3098 for OlexSys, GUI svn.r4951)
;
_audit_update_record
;
2015-10-06 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.564(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1185(6)
_cell_length_b                   12.5191(7)
_cell_length_c                   10.6485(6)
_cell_measurement_reflns_used    4223
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      27.3130
_cell_measurement_theta_min      2.0680
_cell_volume                     2079.71(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 16.1592
_diffrn_detector_type            'Agilent Diffraction Eos detector'
_diffrn_measured_fraction_theta_full 0.508
_diffrn_measured_fraction_theta_max 0.469
_diffrn_measurement_details
;
  1 omega    4.00   70.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870    0.0000  150.0000 66

  2 omega   -4.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870  -53.0000   17.0000 61

  3 omega  -49.00  -17.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870  134.0000  123.0000 32

  4 omega  -30.00   26.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870   39.0000  -12.0000 56

  5 omega  -25.00   33.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870   13.0000   -3.0000 58

  6 omega   13.00   74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4874  -97.0000 -143.0000 61

  7 omega  -28.00    2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870   97.0000  -35.0000 30

  8 omega  -57.00    4.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500   53.0000  -17.0000 61

  9 omega  -12.00   15.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500  -81.0000   29.0000 27

 10 omega   -5.00   26.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500  -97.0000   35.0000 31

 11 omega  -21.00   13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500  -53.0000   17.0000 34

 12 omega   -6.00   27.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500  -97.0000 -143.0000 33

 13 omega  -20.00   11.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870   81.0000  151.0000 31

 14 omega   -5.00   62.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870  -37.0000 -180.0000 67

 15 omega  -29.00    3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870   97.0000  -35.0000 32

 16 omega   16.00   70.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870 -114.0000   44.0000 54

 17 omega  -52.00   16.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500   39.0000  167.0000 68

 18 omega  -25.00   29.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500  -39.0000   12.0000 54

 19 omega  -28.00   28.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500  -39.0000 -167.0000 56

 20 omega    4.00   37.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500 -114.0000   44.0000 33
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0143119000
_diffrn_orient_matrix_UB_12      0.0352099000
_diffrn_orient_matrix_UB_13      0.0423941000
_diffrn_orient_matrix_UB_21      0.0156590000
_diffrn_orient_matrix_UB_22      -0.0356686000
_diffrn_orient_matrix_UB_23      0.0523138000
_diffrn_orient_matrix_UB_31      0.0402121000
_diffrn_orient_matrix_UB_32      0.0264009000
_diffrn_orient_matrix_UB_33      0.0142009000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.508
_diffrn_reflns_Laue_measured_fraction_max 0.469
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8884
_diffrn_reflns_point_group_measured_fraction_full 0.508
_diffrn_reflns_point_group_measured_fraction_max 0.469
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         2.086
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    14.528
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.0646 before and 0.0553 after correction. 
The Ratio of minimum to maximum transmission is 0.8790. 
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.910
_exptl_crystal_description       plate
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.073
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1124
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+16.0958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1019
_reflns_number_total             1124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc00923a2.cif
_cod_data_source_block           74-2kbar
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7118875--7118888.cif.
;
_cod_database_code               7118884
_chemical_oxdiff_formula         C30H24Au2Cl2P2
_chemical_oxdiff_usercomment
'digold-dichloride-PTM MeOH/EtOH-starting pressure 74 '
_reflns_odcompleteness_completeness 48.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C15-C13 = C14-C13
 1.39 with sigma of 0.01
 C12-C7 \\sim C11-C12 \\sim C11-C10 \\sim C10-C9 \\sim C8-C9 \\sim C8-C7
 with sigma of 0.02
 C2-C1 \\sim C6-C1 \\sim C5-C6 \\sim C5-C4 \\sim C3-C4 \\sim C3-C2
 with sigma of 0.02
 C13-C15 \\sim C14-C13 \\sim C14-C15_$1 \\sim C13_$1-C15_$1 \\sim C14_$1-C13_$1
\\sim C14_$1-C15
 with sigma of 0.02
 C8-C7 \\sim C9-C8 \\sim C10-C9 \\sim C11-C10 \\sim C12-C11 \\sim C12-C7
 with sigma of 0.02
 C2-C1 \\sim C3-C2 \\sim C3-C4 \\sim C5-C4 \\sim C6-C5 \\sim C1-C6
 with sigma of 0.02
 C15-C13 \\sim C14-C13
 with sigma of 0.02
 C15-C14_$1 \\sim C15-C13
 with sigma of 0.02
 C15-C14_$1 \\sim C14_$1-C13_$1
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C9(H9), C14(H14), C2(H2), C6(H6), C12(H12), C10(H10), C4(H4),
 C8(H8), C3(H3), C5(H5), C11(H11)
;
_shelx_res_checksum              36499
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'