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_1573652
_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           29
_space_group_name_Hall           'P -2a -2ab'
_space_group_name_H-M_alt        'P b 21 a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-05-06
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_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                   16.9003(5)
_cell_length_b                   9.8370(4)
_cell_length_c                   16.6364(10)
_cell_measurement_reflns_used    5663
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7690
_cell_measurement_theta_min      2.1090
_cell_volume                     2765.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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 n-pentane/i-pentane 1:1 mixture'
_diffrn_ambient_pressure         1940000
_diffrn_ambient_temperature      293(2)
_diffrn_crystal_treatment
'pressurized rapidly in n-pentane/i-pentane 1:1 mixture as a hydrostatic medium'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0128
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.724
_diffrn_measured_fraction_theta_max 0.594
_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    -28.00   3.00   1.00  120.00    --   22.04  39.00 167.00   31
  2  \w    -42.00  32.00   1.00  120.00    --   22.04  26.00  -8.00   74
  3  \w     59.00  86.00   1.00  120.00    --   22.04-160.00  60.00   27
  4  \w     20.00  56.00   1.00  120.00    --   22.04-114.00  45.00   36
  5  \w     -8.00  36.00   1.00  120.00    --   22.04 -67.00-157.00   44
  6  \w    -30.00  12.00   1.00  120.00    --  -22.19  67.00 157.00   42
  7  \w    -39.00 -14.00   1.00  120.00    --  -22.19  97.00 -35.00   25
  8  \w    -82.00 -11.00   1.00  120.00    --  -22.19 114.00 135.00   71
  9  \w    -59.00  11.00   1.00  120.00    --  -22.19  67.00 -23.00   70
 10  \w    -70.00 -43.00   1.00  120.00    --  -22.19 137.00 114.00   27
 11  \w    -32.00  20.00   1.00  120.00    --  -22.19 -26.00   8.00   52
 12  \w   -108.00 -73.00   1.00  120.00    --  -22.19-160.00-120.00   35
 13  \w    -43.00 -16.00   1.00  120.00    --  -22.19 114.00 -45.00   27
 14  \w    -13.00  14.00   1.00  120.00    --  -22.19  39.00 167.00   27
 15  \w    -23.00   2.00   1.00  120.00    --  -22.19   0.00-150.00   25
;
_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 38.5 deg.'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0041292330
_diffrn_orient_matrix_UB_12      0.0335712297
_diffrn_orient_matrix_UB_13      0.0268301426
_diffrn_orient_matrix_UB_21      -0.0328365506
_diffrn_orient_matrix_UB_22      -0.0044038301
_diffrn_orient_matrix_UB_23      -0.0032563803
_diffrn_orient_matrix_UB_31      0.0001498909
_diffrn_orient_matrix_UB_32      -0.0456843100
_diffrn_orient_matrix_UB_33      0.0200180236
_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  0.0652
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_Laue_measured_fraction_full 0.724
_diffrn_reflns_Laue_measured_fraction_max 0.594
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17169
_diffrn_reflns_point_group_measured_fraction_full 0.653
_diffrn_reflns_point_group_measured_fraction_max 0.490
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         25.609
_diffrn_reflns_theta_min         1.902
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    5.806
_exptl_absorpt_correction_T_max  0.65468
_exptl_absorpt_correction_T_min  0.64727
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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    2.143
_exptl_crystal_description       needle
_exptl_crystal_F_000             1712
_exptl_crystal_preparation
'Mounted in a Diamond-Anvil Cell using n-pentane/i-pentane 1:1 mixture as pressure medium.,Luminescent'
_exptl_crystal_pressure_history
'Pressurized to 1.94 GPa and left to stabilize over ? hours.'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane/dichloromethane'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.70(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5195
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0164P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0626
_reflns_Friedel_coverage         0.569
_reflns_Friedel_fraction_full    0.572
_reflns_Friedel_fraction_max     0.375
_reflns_number_gt                3275
_reflns_number_total             5195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03036b2.cif
_cod_data_source_block           appr6_1p94GPa
_cod_depositor_comments
'Adding full bibliography for 1573624--1573666.cif.'
_cod_database_code               1573652
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C15H25OPAu
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.30(3)
 0.70(3)
2. 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
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim C28 \\sim C24 \\sim C25 \\sim C27 \\sim C26 \\sim
O2 \\sim C29: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C1 \\sim C2 \\sim C3 \\sim C8 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim O1
\\sim C9: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 1.7A
C15 \\sim C14 \\sim P1 \\sim C10 \\sim C11 \\sim C12 \\sim C13: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C28, C27, C26, C23, C24, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C4, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C30(H30A,H30B), C32(H32A,H32B), C12(H12A,H12B), C14(H14A,
 H14B), C34(H34A,H34B)
5.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C24(H24), C28(H28), C25(H25), C7(H7), C8(H8), C4(H4), C5(H5)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C31(H31A,H31B,H31C), C9(H9A,H9B,H9C), C35(H35A,H35B,
 H35C), C33(H33A,H33B,H33C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C29(H29A,
 H29B,H29C)
;
_shelx_res_checksum              8757
_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 1.241
_oxdiff_exptl_absorpt_empirical_full_min 0.790