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_1573629
_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                   17.0137(3)
_cell_length_b                   9.85586(8)
_cell_length_c                   16.7032(5)
_cell_measurement_reflns_used    5174
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.3650
_cell_measurement_theta_min      1.8220
_cell_volume                     2800.87(10)
_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 daphne-7575'
_diffrn_ambient_pressure         1620000
_diffrn_ambient_temperature      293(2)
_diffrn_crystal_treatment
'pressurized rapidly in daphne-7575 as a hydrostatic medium'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.632
_diffrn_measured_fraction_theta_max 0.435
_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    -39.00  39.00   0.50    1.00    --    0.00   0.00   0.00  156
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_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      0.0117108874
_diffrn_orient_matrix_UB_12      -0.0030876521
_diffrn_orient_matrix_UB_13      -0.0213859222
_diffrn_orient_matrix_UB_21      -0.0033333933
_diffrn_orient_matrix_UB_22      0.0406520124
_diffrn_orient_matrix_UB_23      -0.0039353957
_diffrn_orient_matrix_UB_31      0.0207943559
_diffrn_orient_matrix_UB_32      0.0082452335
_diffrn_orient_matrix_UB_33      0.0113966510
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.410
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.632
_diffrn_reflns_Laue_measured_fraction_max 0.435
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10054
_diffrn_reflns_point_group_measured_fraction_full 0.579
_diffrn_reflns_point_group_measured_fraction_max 0.364
_diffrn_reflns_theta_full        14.241
_diffrn_reflns_theta_max         21.717
_diffrn_reflns_theta_min         1.547
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    2.580
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_description       needle
_exptl_crystal_F_000             1712
_exptl_crystal_preparation
'Mounted in a Diamond-Anvil Cell using daphne-7575 as pressure medium.,Luminescent'
_exptl_crystal_pressure_history
'Pressurized to 1.62 GPa and left to stabilize over ? hours.'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane/dichloromethane'
_exptl_crystal_size_max          0.0025
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.0015
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.94(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6267
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0379P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.604
_reflns_Friedel_fraction_full    0.519
_reflns_Friedel_fraction_max     0.286
_reflns_number_gt                5654
_reflns_number_total             6267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03036b3.cif
_cod_data_source_block           0004_1p62GPa
_cod_depositor_comments
'Adding full bibliography for 1573624--1573666.cif.'
_cod_original_cell_volume        2800.87(9)
_cod_database_code               1573629
_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. Twinned data refinement
 Scales: 0.06(3)
 0.94(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(HB,HC), C30(H30A,H30B), C32(H32A,H32B), C12(HH,HI), C14(HJ,HK), C34(H34A,
 H34B)
3.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C24(H24), C28(H28), C25(H25), C7(H), C8(HA), C4(HG), C5(HO)
3.c Idealised Me refined as rotating group:
 C11(HD,HE,HF), C31(H31A,H31B,H31C), C9(HL,HM,HN), C35(H35A,H35B,H35C),
 C33(H33A,H33B,H33C), C15(HP,HQ,HR), C13(HS,HT,HU), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              63714
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.288
_oxdiff_exptl_absorpt_empirical_full_min 0.860