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_1573666
_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             2024-02-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_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                   16.215(3)
_cell_length_b                   11.0942(12)
_cell_length_c                   17.732(4)
_cell_measurement_reflns_used    1269
_cell_measurement_temperature    295.40(16)
_cell_measurement_theta_max      24.6000
_cell_measurement_theta_min      2.4440
_cell_volume                     3189.9(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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      'Diamond Anvil Cell filled with silicone oil'
_diffrn_ambient_pressure         320000
_diffrn_ambient_temperature      295.40(16)
_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 0.703
_diffrn_measured_fraction_theta_max 0.688
_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      6.00  42.00   1.00   90.00    --   22.04 -39.00-167.00   36
  2  \w     10.00  36.00   1.00   90.00    --   22.04 -81.00-151.00   26
  3  \w    -27.00  10.00   1.00   90.00    --   22.04  39.00 167.00   37
  4  \w     10.00  35.00   1.00   90.00    --   22.04 -77.00  30.00   25
  5  \w    -18.00  22.00   1.00   90.00    --   22.04 -53.00-162.00   40
  6  \w    -41.00  -6.00   1.00   90.00    --   22.04 114.00 -45.00   35
  7  \w    -56.00 -31.00   1.00   90.00    --  -22.19 150.00 -64.00   25
  8  \w    -58.00 -25.00   1.00   90.00    --  -22.19 135.00 123.00   33
  9  \w   -107.00 -81.00   1.00   90.00    --  -22.19-160.00-120.00   26
;
_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 deg.'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0205790101
_diffrn_orient_matrix_UB_12      -0.0027264149
_diffrn_orient_matrix_UB_13      0.0252727070
_diffrn_orient_matrix_UB_21      -0.0037463354
_diffrn_orient_matrix_UB_22      0.0500986059
_diffrn_orient_matrix_UB_23      -0.0005056057
_diffrn_orient_matrix_UB_31      -0.0274023848
_diffrn_orient_matrix_UB_32      -0.0048782065
_diffrn_orient_matrix_UB_33      -0.0189292525
_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  0.0837
_diffrn_reflns_av_unetI/netI     0.1092
_diffrn_reflns_Laue_measured_fraction_full 0.703
_diffrn_reflns_Laue_measured_fraction_max 0.688
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8296
_diffrn_reflns_point_group_measured_fraction_full 0.703
_diffrn_reflns_point_group_measured_fraction_max 0.688
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.514
_diffrn_reflns_theta_min         1.975
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    5.034
_exptl_absorpt_correction_T_max  0.64452
_exptl_absorpt_correction_T_min  0.63711
_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    1.858
_exptl_crystal_description       sphere
_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 0.32 GPa and left to stabilize over ? hours.'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane/dichloromethane'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2239
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.1764
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0161P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                807
_reflns_number_total             2239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03036b2.cif
_cod_data_source_block           appr4_0p32GPa
_cod_depositor_comments
'Adding full bibliography for 1573624--1573666.cif.'
_cod_database_code               1573666
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O1A \\sim O1 \\sim C9A \\sim C9: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C3 \\sim C3A \\sim C4A \\sim C4 \\sim C5A \\sim C5 \\sim C6A \\sim C6 \\sim C7A
\\sim C7 \\sim C8A \\sim C8: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
C8 \\sim C7 \\sim C4 \\sim C13 \\sim C3 \\sim C11 \\sim C5 \\sim C10 \\sim C1:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C2 \\sim O1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C11 \\sim C10 \\sim P1 \\sim C13 \\sim C12 \\sim C15 \\sim C14 \\sim C15A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
3. Others
 Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(O1A)=Sof(C3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=1-FVAR(1)
 Sof(C3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=Sof(H7)=Sof(C8)=
 Sof(H8)=Sof(O1)=Sof(H14A)=Sof(H14B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C15)=Sof(H15D)=Sof(H15E)=Sof(H15F)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C10(H10A,H10B), C14(H14C,H14D), C14(H14A,H14B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C4A(H4A), C5A(H5A), C7A(H7A), C8A(H8A)
4.c Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8), C3A(C4A,C5A,C6A,C7A,C8A)
4.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C15A(H15A,H15B,H15C), C9(H9A,H9B,
 H9C), C9A(H9AA,H9AB,H9AC), C15(H15D,H15E,H15F)
;
_shelx_res_checksum              55680
_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 1.874
_oxdiff_exptl_absorpt_empirical_full_min 0.525