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_1573663
_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     dual
_audit_creation_date             2023-05-24
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_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                   16.7686(6)
_cell_length_b                   9.8173(2)
_cell_length_c                   16.1828(17)
_cell_measurement_reflns_used    3467
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.1170
_cell_measurement_theta_min      1.9110
_cell_volume                     2664.1(3)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment
'Diamond Anvil Cell filled with n-pentane/i-pentane 1:1 mixture'
_diffrn_ambient_pressure         2590000
_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 0.639
_diffrn_measured_fraction_theta_max 0.532
_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    -54.00 -18.00   1.00  150.00    --   22.11 135.00 -57.00   36
  2  \w    -75.00 -11.00   1.00  150.00    --  -22.19  97.00 143.00   64
  3  \w    -60.00  16.00   1.00  150.00    --  -22.19  67.00 -23.00   76
  4  \w    -16.00  33.00   1.00  150.00    --  -22.19 -38.00-180.00   49
  5  \w    -97.00 -26.00   1.00  150.00    --  -22.19 135.00 -57.00   71
  6  \w    -38.00  -9.00   1.00  150.00    --  -22.19  77.00 -30.00   29
  7  \w    -56.00 -25.00   1.00  150.00    --  -22.19  38.00-180.00   31
;
_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 37 deg.'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0118128429
_diffrn_orient_matrix_UB_12      -0.0117365286
_diffrn_orient_matrix_UB_13      -0.0315376518
_diffrn_orient_matrix_UB_21      -0.0312109398
_diffrn_orient_matrix_UB_22      0.0053906853
_diffrn_orient_matrix_UB_23      0.0117829221
_diffrn_orient_matrix_UB_31      0.0005336756
_diffrn_orient_matrix_UB_32      0.0554866469
_diffrn_orient_matrix_UB_33      -0.0078033795
_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  0.1009
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.639
_diffrn_reflns_Laue_measured_fraction_max 0.532
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11137
_diffrn_reflns_point_group_measured_fraction_full 0.639
_diffrn_reflns_point_group_measured_fraction_max 0.532
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         25.688
_diffrn_reflns_theta_min         1.917
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    6.027
_exptl_absorpt_correction_T_max  0.58955
_exptl_absorpt_correction_T_min  0.58080
_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_density_diffrn    2.225
_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 2.59 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         1.166
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2732
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0174P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1526
_reflns_number_total             2732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03036b2.cif
_cod_data_source_block           appr6_2p59GPa
_cod_depositor_comments
'Adding full bibliography for 1573624--1573666.cif.'
_cod_database_code               1573663
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H22 O P Au'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_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. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C4(H4), C5(H5)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              28655
_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 1.147
_oxdiff_exptl_absorpt_empirical_full_min 0.864