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_1573650
_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                   17.2929(5)
_cell_length_b                   9.9154(4)
_cell_length_c                   16.8744(7)
_cell_measurement_reflns_used    4410
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.6220
_cell_measurement_theta_min      2.4550
_cell_volume                     2893.39(19)
_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         940000
_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 0.741
_diffrn_measured_fraction_theta_max 0.666
_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    -84.00 -13.00   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 39 deg.'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0038224658
_diffrn_orient_matrix_UB_12      0.0345569737
_diffrn_orient_matrix_UB_13      0.0259294213
_diffrn_orient_matrix_UB_21      -0.0321104269
_diffrn_orient_matrix_UB_22      -0.0046923637
_diffrn_orient_matrix_UB_23      -0.0027720715
_diffrn_orient_matrix_UB_31      0.0004467100
_diffrn_orient_matrix_UB_32      -0.0443697163
_diffrn_orient_matrix_UB_33      0.0204678075
_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  0.0479
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 0.741
_diffrn_reflns_Laue_measured_fraction_max 0.666
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12415
_diffrn_reflns_point_group_measured_fraction_full 0.612
_diffrn_reflns_point_group_measured_fraction_max 0.534
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         21.101
_diffrn_reflns_theta_min         2.466
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    5.550
_exptl_absorpt_correction_T_max  0.66606
_exptl_absorpt_correction_T_min  0.65910
_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    2.049
_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 0.94 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         0.871
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.69(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3426
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0148P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0524
_reflns_Friedel_coverage         0.513
_reflns_Friedel_fraction_full    0.464
_reflns_Friedel_fraction_max     0.385
_reflns_number_gt                2335
_reflns_number_total             3426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03036b2.cif
_cod_data_source_block           appr6_0p94GPa
_cod_depositor_comments
'Adding full bibliography for 1573624--1573666.cif.'
_cod_original_cell_volume        2893.39(17)
_cod_database_code               1573650
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C15H22OPAu
_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: 0.31(4)
 0.69(4)
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
C23 \\sim C28 \\sim C27 \\sim C26 \\sim C25 \\sim C24: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
C11 \\sim C10: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
4. Rigid body (RIGU) restrains
 C3, C8, C7, C6, C5, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C27, C28, C23, C24, C25
 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              96137
_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 1.313
_oxdiff_exptl_absorpt_empirical_full_min 0.700