Pressure-induced phase transitions in a new luminescent gold(I)-arylacetylide.
Dziewiątkowska, Róża; Krzeszczakowska, Joanna; Głodek, Marta; Łomzik, Michał; Plażuk, Damian; Makal, Anna; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3362–3374; doi:10.1039/d4dt03036b

data_1573654
_publ_section_title
;
 Pressure-induced phase transitions in a new luminescent
 gold(I)-arylacetylide.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3362
_journal_page_last               3374
_journal_paper_doi               10.1039/d4dt03036b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C15 H22 Au O P'
_chemical_formula_sum            'C15 H22 Au O P'
_chemical_formula_weight         446.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-02-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-07-24 deposited with the CCDC.	2025-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.0628(9)
_cell_length_b                   11.0945(4)
_cell_length_c                   17.7070(6)
_cell_measurement_reflns_used    5564
_cell_measurement_temperature    295.5(3)
_cell_measurement_theta_max      24.5360
_cell_measurement_theta_min      2.0580
_cell_volume                     3155.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      'Diamond Anvil Cell filled with silicone oil'
_diffrn_ambient_pressure         330000
_diffrn_ambient_temperature      295.5(3)
_diffrn_crystal_treatment
'pressurized rapidly in silicone oil as a hydrostatic medium'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0128
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.914
_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     10.00  35.00   1.00   60.00    --   22.04  53.00 -17.00   25
  2  \w    -20.00  51.00   1.00   90.00    --   22.04 -53.00  17.00   71
  3  \w    -27.00  51.00   1.00   90.00    --   22.04 -39.00-167.00   78
  4  \w    -50.00  45.00   1.00   90.00    --   22.04  26.00  -8.00   95
  5  \w    -13.00  17.00   1.00   90.00    --   22.04  97.00 143.00   30
  6  \w    -20.00   7.00   1.00   90.00    --   22.04 114.00 -45.00   27
  7  \w    -32.00  -6.00   1.00   90.00    --   22.04  39.00 167.00   26
  8  \w    -67.00 -13.00   1.00   90.00    --  -22.19 135.00 123.00   54
  9  \w    -23.00  28.00   1.00   90.00    --  -22.19  39.00 -12.00   51
 10  \w    -85.00   1.00   1.00   90.00    --  -22.19 114.00 -45.00   86
 11  \w    -45.00  48.00   1.00   90.00    --  -22.19 -26.00   8.00   93
 12  \w    -34.00  29.00   1.00   90.00    --  -22.19  53.00 162.00   63
 13  \w    -17.00  21.00   1.00   90.00    --  -22.19 -97.00-143.00   38
 14  \w    -16.00  21.00   1.00   90.00    --  -22.19 -97.00  35.00   37
 15  \w    -50.00  45.00   1.00   15.00    --   22.04  26.00  -8.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support
'Diamond Anvil Cell, effective opening angle 51 deg.'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0280698018
_diffrn_orient_matrix_UB_12      0.0291718516
_diffrn_orient_matrix_UB_13      0.0039395935
_diffrn_orient_matrix_UB_21      0.0085926994
_diffrn_orient_matrix_UB_22      -0.0262371656
_diffrn_orient_matrix_UB_23      0.0258332096
_diffrn_orient_matrix_UB_31      0.0187233879
_diffrn_orient_matrix_UB_32      -0.0316895172
_diffrn_orient_matrix_UB_33      -0.0177534866
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.919
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35162
_diffrn_reflns_point_group_measured_fraction_full 0.919
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.510
_diffrn_reflns_theta_min         1.815
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    5.089
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.36a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_description       needle
_exptl_crystal_F_000             1712
_exptl_crystal_preparation
'Mounted in a Diamond-Anvil Cell using silicone oil as pressure medium.,Luminescent'
_exptl_crystal_pressure_history
'Pressurized to 0.33 GPa and left to stabilize over ? hours.'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane/dichloromethane'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.075
_refine_diff_density_min         -1.755
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2939
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0739P)^2^+10.8659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1505
_reflns_number_total             2939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03036b2.cif
_cod_data_source_block           appr5_0p33GPa
_cod_depositor_comments
'Adding full bibliography for 1573624--1573666.cif.'
_cod_database_code               1573654
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H22 O P Au'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C3A \\sim C3 \\sim C8A \\sim C8 \\sim C7A \\sim C7 \\sim C6A \\sim C6 \\sim C5A
\\sim C5 \\sim C4A \\sim C4: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
C9A \\sim C9 \\sim O1A \\sim O1: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
3. Others
 Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(O1A)=Sof(C3A)=Sof(C8A)=Sof(H8A)=Sof(C7A)=
 Sof(H7A)=Sof(C6A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=1-FVAR(1)
 Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=
 Sof(C6)=Sof(O1)=Sof(H14A)=Sof(H14B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C15)=Sof(H15D)=Sof(H15E)=Sof(H15F)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C10(H10A,H10B), C14(H14C,H14D), C14(H14A,H14B)
4.b Me refined with riding coordinates:
 C15A(H15A,H15B,H15C)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C4(H4), C5(H5), C8A(H8A), C7A(H7A), C5A(H5A), C4A(H4A)
4.d Fitted hexagon refined as free rotating group:
 C3A(C8A,C7A,C6A,C5A,C4A)
4.e Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,
 H9AC), C15(H15D,H15E,H15F)
;
_shelx_res_checksum              87868
_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 2.051
_oxdiff_exptl_absorpt_empirical_full_min 0.763