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_1573651
_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
_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                   17.1407(10)
_cell_length_b                   9.8864(4)
_cell_length_c                   16.8388(12)
_cell_measurement_reflns_used    11118
_cell_measurement_temperature    295.5(5)
_cell_measurement_theta_max      22.7830
_cell_measurement_theta_min      2.0840
_cell_volume                     2853.5(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)'
_diffrn_ambient_environment      'Diamond Anvil Cell filled with silicone oil'
_diffrn_ambient_pressure         1120000
_diffrn_ambient_temperature      295.5(5)
_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 0.914
_diffrn_measured_fraction_theta_max 0.885
_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    -88.00   5.00   1.00   90.00    --  -25.00 114.00 -45.00   93
  2  \w    -37.00  29.00   1.00   90.00    --  -25.00 -39.00-167.00   66
  3  \w    -26.00  10.00   1.00   90.00    --  -25.00  67.00 -23.00   36
  4  \w    -14.00  18.00   1.00   90.00    --  -25.00 -97.00  35.00   32
  5  \w    -14.00  21.00   1.00   90.00    --  -25.00 -97.00-143.00   35
  6  \w      2.00  43.00   1.00   90.00    --  -25.00 -26.00   8.00   41
  7  \w    -97.00 -14.00   1.00   90.00    --  -25.00 135.00 123.00   83
  8  \w    -64.00  28.00   1.00   90.00    --  -25.00  53.00 162.00   92
  9  \w    -29.00  37.00   1.00   90.00    --   25.08  39.00 167.00   66
 10  \w    -20.00  60.00   1.00   90.00    --   25.08 -67.00  23.00   80
 11  \w    -12.00  14.00   1.00   90.00    --   25.08  97.00 143.00   26
 12  \w    -28.00  62.00   1.00   90.00    --   25.08 -39.00-167.00   90
 13  \w    -54.00  42.00   1.00   90.00    --   25.08  26.00  -8.00   96
 14  \w    -16.00  14.00   1.00   90.00    --   25.08  97.00 -35.00   30
;
_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 52 deg.'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0198248000
_diffrn_orient_matrix_UB_12      0.0263518000
_diffrn_orient_matrix_UB_13      0.0031499000
_diffrn_orient_matrix_UB_21      0.0167071000
_diffrn_orient_matrix_UB_22      -0.0148102000
_diffrn_orient_matrix_UB_23      0.0415346000
_diffrn_orient_matrix_UB_31      0.0197816000
_diffrn_orient_matrix_UB_32      -0.0138687000
_diffrn_orient_matrix_UB_33      -0.0382694000
_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  0.0873
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.914
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40946
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.002
_diffrn_reflns_theta_min         1.875
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    5.627
_exptl_absorpt_correction_T_max  0.61198
_exptl_absorpt_correction_T_min  0.60373
_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    2.078
_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 1.12 GPa and left to stabilize over ? hours.'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane/dichloromethane'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.981
_refine_diff_density_min         -1.439
_refine_diff_density_rms         0.179
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.54(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7156
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0414P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_full    0.921
_reflns_Friedel_fraction_max     0.882
_reflns_number_gt                5364
_reflns_number_total             7156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03036b2.cif
_cod_data_source_block           appr2_1p12GPa
_cod_depositor_comments
'Adding full bibliography for 1573624--1573666.cif.'
_cod_database_code               1573651
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H22 O P Au'
_shelx_estimated_absorpt_t_max   0.631
_shelx_estimated_absorpt_t_min   0.431
_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: 0.46(3)
 0.54(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.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)
3.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C24(H24), C28(H28), C25(H25), C7(H7), C8(H8), C4(H4), C5(H5)
3.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              498
_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 3.120
_oxdiff_exptl_absorpt_empirical_full_min 0.601