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_1573660
_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             2023-05-15
_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                   16.168(2)
_cell_length_b                   10.9575(12)
_cell_length_c                   17.526(4)
_cell_measurement_reflns_used    1342
_cell_measurement_temperature    295.3(4)
_cell_measurement_theta_max      23.5910
_cell_measurement_theta_min      1.9630
_cell_volume                     3104.9(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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         450000
_diffrn_ambient_temperature      295.3(4)
_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 0.723
_diffrn_measured_fraction_theta_max 0.564
_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      -0.0205951765
_diffrn_orient_matrix_UB_12      0.0026452197
_diffrn_orient_matrix_UB_13      -0.0255761282
_diffrn_orient_matrix_UB_21      -0.0037449549
_diffrn_orient_matrix_UB_22      -0.0507445881
_diffrn_orient_matrix_UB_23      0.0004702167
_diffrn_orient_matrix_UB_31      -0.0275903959
_diffrn_orient_matrix_UB_32      0.0048684908
_diffrn_orient_matrix_UB_33      0.0190472492
_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  0.0783
_diffrn_reflns_av_unetI/netI     0.1466
_diffrn_reflns_Laue_measured_fraction_full 0.723
_diffrn_reflns_Laue_measured_fraction_max 0.564
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10035
_diffrn_reflns_point_group_measured_fraction_full 0.723
_diffrn_reflns_point_group_measured_fraction_max 0.564
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         25.495
_diffrn_reflns_theta_min         1.988
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    5.172
_exptl_absorpt_correction_T_max  0.08698
_exptl_absorpt_correction_T_min  0.06629
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.909
_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 0.45 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         0.637
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.106
_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         3319
_refine_ls_number_restraints     206
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.2449
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0312P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.1402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                921
_reflns_number_total             3319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03036b2.cif
_cod_data_source_block           appr4_0p45GPa
_cod_depositor_comments
'Adding full bibliography for 1573624--1573666.cif.'
_cod_original_cell_volume        3104.8(10)
_cod_database_code               1573660
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C14 H19 O P Au'
_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. Restrained distances
 C14-C15 \\sim C14-C15A
 with sigma of 0.02
 O1-C9 \\sim O1A-C9A
 with sigma of 0.02
 C6-C9 \\sim C6A-C9A
 with sigma of 0.04
 C8-C6 \\sim C8A-C6A
 with sigma of 0.04
 C2-C3 \\sim C2-C3A
 with sigma of 0.02
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 C7-C6 \\sim C7A-C6A
 with sigma of 0.02
 C8-C3 \\sim C8A-C3A
 with sigma of 0.02
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 C4-C6 \\sim C4A-C6A
 with sigma of 0.04
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 C5-C6 \\sim C5A-C6A
 with sigma of 0.02
 C8-C4 \\sim C8A-C4A
 with sigma of 0.04
 C6-O1 \\sim C6A-O1A
 with sigma of 0.02
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
 C5-O1 \\sim C5A-O1A
 with sigma of 0.04
 C2-C8 \\sim C2-C8A
 with sigma of 0.04
 C2-C4 \\sim C2-C4A
 with sigma of 0.04
 C7-C3 \\sim C7A-C3A
 with sigma of 0.04
 C7-C5 \\sim C7A-C5A
 with sigma of 0.04
 C7-O1 \\sim C7A-O1A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C9A \\sim C9: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C5A \\sim C5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C3 \\sim C3A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C11: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
1.7A
C7A \\sim C7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C4A \\sim C4: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
O1A \\sim O1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C8A \\sim C8: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C15 \\sim C15A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C6A \\sim C6: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C12: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
1.7A
C13: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
1.7A
Uanis(C3) = Uanis(C3A)
Uanis(C8) = Uanis(C8A)
Uanis(C4A) = Uanis(C4)
Uanis(C5) = Uanis(C5A)
4. Rigid body (RIGU) restrains
 C3, C4, C5, C6, C8, C7, O1, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3A, C4A, C5A, C6A, C7A, C8A, C9A, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C15, C15A, P1, C12, C13, C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(O1A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=
 Sof(C3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=1-FVAR(1)
 Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=
 Sof(C6)=Sof(O1)=Sof(H14A)=Sof(H14B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B), C14(H14C,H14D)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C4(H4), C5(H5), C7A(H7A), C8A(H8A), C4A(H4A), C5A(H5A)
6.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C15A(H15D,H15E,
 H15F), C11(H11A,H11B,H11C), C9A(H9AA,H9AB,H9AC)
;
_shelx_res_checksum              61264
_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 2.758
_oxdiff_exptl_absorpt_empirical_full_min 0.681