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_1573655
_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      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2a'
_space_group_name_H-M_alt        'P 1 1 a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2023-05-31
_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                93.865(3)
_cell_formula_units_Z            8
_cell_length_a                   16.7021(6)
_cell_length_b                   9.8830(3)
_cell_length_c                   16.8029(4)
_cell_measurement_reflns_used    8058
_cell_measurement_temperature    294.7(3)
_cell_measurement_theta_max      19.6880
_cell_measurement_theta_min      2.4260
_cell_volume                     2767.29(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_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 silicone oil'
_diffrn_ambient_pressure         2130000
_diffrn_ambient_temperature      294.7(3)
_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 0.651
_diffrn_measured_fraction_theta_max 0.604
_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     10.00  35.00   1.00   60.00    --   22.04  53.00 -17.00   25
  2  \w    -20.00  51.00   1.00   95.00    --   22.04 -53.00  17.00   71
  3  \w    -27.00  51.00   1.00   95.00    --   22.04 -39.00-167.00   78
  4  \w    -50.00  45.00   1.00   95.00    --   22.04  26.00  -8.00   95
  5  \w    -13.00  17.00   1.00   95.00    --   22.04  97.00 143.00   30
  6  \w    -20.00   7.00   1.00   95.00    --   22.04 114.00 -45.00   27
  7  \w    -32.00  -6.00   1.00   95.00    --   22.04  39.00 167.00   26
  8  \w    -67.00 -13.00   1.00   95.00    --  -22.19 135.00 123.00   54
  9  \w    -23.00  28.00   1.00   95.00    --  -22.19  39.00 -12.00   51
 10  \w    -85.00   1.00   1.00   95.00    --  -22.19 114.00 -45.00   86
 11  \w    -45.00  48.00   1.00   95.00    --  -22.19 -26.00   8.00   93
 12  \w    -34.00  29.00   1.00   95.00    --  -22.19  53.00 162.00   63
 13  \w    -17.00  21.00   1.00   95.00    --  -22.19 -97.00-143.00   38
 14  \w    -16.00  21.00   1.00   95.00    --  -22.19 -97.00  35.00   37
 15  \w    -50.00  45.00   1.00   60.00    --   22.04  26.00  -8.00   95
;
_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 51 deg.'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0260618715
_diffrn_orient_matrix_UB_12      -0.0379671868
_diffrn_orient_matrix_UB_13      0.0040788950
_diffrn_orient_matrix_UB_21      -0.0089981972
_diffrn_orient_matrix_UB_22      0.0272505665
_diffrn_orient_matrix_UB_23      0.0274262832
_diffrn_orient_matrix_UB_31      -0.0191501385
_diffrn_orient_matrix_UB_32      0.0321626829
_diffrn_orient_matrix_UB_33      -0.0184265919
_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  0.0547
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_Laue_measured_fraction_full 0.651
_diffrn_reflns_Laue_measured_fraction_max 0.604
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22719
_diffrn_reflns_point_group_measured_fraction_full 0.643
_diffrn_reflns_point_group_measured_fraction_max 0.583
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.977
_diffrn_reflns_theta_min         2.513
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    5.803
_exptl_absorpt_correction_T_max  0.20757
_exptl_absorpt_correction_T_min  0.19601
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.36a (Rigaku Oxford Diffraction, 2021)
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    2.142
_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 2.13 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          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         7038
_refine_ls_number_restraints     410
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0258P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    0.636
_reflns_Friedel_fraction_max     0.562
_reflns_number_gt                5324
_reflns_number_total             7038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03036b2.cif
_cod_data_source_block           appr5_2p13GPa
_cod_depositor_comments
'Adding full bibliography for 1573624--1573666.cif.'
_cod_original_cell_volume        2767.29(14)
_cod_original_sg_symbol_H-M      'P 1 1 a'
_cod_database_code               1573655
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H22 O P Au'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.94(3)
 0.06(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. Uiso/Uaniso restraints and constraints
C49 \\sim O3 \\sim C46 \\sim C47 \\sim C45 \\sim C44 \\sim C48 \\sim C43 \\sim
C42 \\sim C41: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C34 \\sim C35 \\sim C31 \\sim C30 \\sim C33 \\sim C32 \\sim P2: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C21 \\sim C22 \\sim C23 \\sim C28 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim
O2 \\sim C29: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C15 \\sim C14 \\sim C11 \\sim C10 \\sim C13 \\sim C12 \\sim P1: within 2A with
sigma of 0.03 and sigma for terminal atoms of 0.06 within 2A
C51 \\sim C50 \\sim C53 \\sim C52 \\sim C55 \\sim C54 \\sim P3: within 2A with
sigma of 0.03 and sigma for terminal atoms of 0.06 within 2A
C9 \\sim O1 \\sim C6 \\sim C5 \\sim C7 \\sim C4 \\sim C8 \\sim C3 \\sim C2
\\sim C1: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 1.7A
C75 \\sim C74 \\sim C73 \\sim C72 \\sim C70 \\sim C71 \\sim P4: within 2A with
sigma of 0.03 and sigma for terminal atoms of 0.06 within 2A
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C68 \\sim C65 \\sim C67 \\sim C66 \\sim
O4 \\sim C69: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
Uanis(C29) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C54)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C30(H30A,H30B), C34(H34A,H34B), C70(H70A,H70B), C32(H32A,
 H32B), C52(H52A,H52B), C54(H54A,H54B), C50(H50A,H50B), C72(H72A,H72B),
 C14(H14A,H14B), C10(H10A,H10B), C12(H12A,H12B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C44(H44), C24(H24), C8(H8), C65(H65), C64(H64), C48(H48),
 C67(H67), C68(H68), C28(H28), C4(H4), C27(H27), C25(H25), C45(H45), C47(H47)
4.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C53(H53A,H53B,H53C), C31(H31A,H31B,H31C), C71(H71A,H71B,
 H71C), C51(H51A,H51B,H51C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C15(H15A,
 H15B,H15C), C33(H33A,H33B,H33C), C13(H13A,H13B,H13C), C69(H69A,H69B,H69C),
 C29(H29A,H29B,H29C), C49(H49A,H49B,H49C), C75(H75A,H75B,H75C), C73(H73A,H73B,
 H73C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              54563
_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 1.599
_oxdiff_exptl_absorpt_empirical_full_min 0.802