Structure-property relationship of a complex photoluminescent arylacetylide-gold(I) compound. I: a pressure-induced phase transformation caught in the act.
Jastrzębska, Róża; Poręba, Tomasz; Cova, Federico; Tchoń, Daniel M; Makal, Anna; IUCrJ 11 (2024) –; doi:10.1107/S2052252524007681

data_1572397
_publ_section_title
;
 Structure-property relationship of a complex photoluminescent
 arylacetylide-gold(I) compound. I: a pressure-induced phase
 transformation caught in the act.
;
_journal_issue                   5
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524007681
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety         'C25 H24 Au O P'
_chemical_formula_sum            'C25 H24 Au O P'
_chemical_formula_weight         568.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2023-11-01
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.08.24 svn.re1ec141 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.93(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.13(4)
_cell_length_b                   6.7304(9)
_cell_length_c                   18.096(3)
_cell_measurement_reflns_used    3884
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.475
_cell_measurement_theta_min      1.971
_cell_volume                     1946(5)
_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-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment
'Membrane Diamond Anvil Cell filled with helium'
_diffrn_ambient_pressure         800000
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.306
_diffrn_measured_fraction_theta_max 0.173
_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    -32.00  32.00   0.50    0.50    --    0.00   0.00   0.00  128
;
_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
'Membrane Diamond Anvil Cell with stainless steel gasket 0.1 mm thick, effective opening angle of 35 deg.'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0256942000
_diffrn_orient_matrix_UB_12      0.0003110000
_diffrn_orient_matrix_UB_13      0.0033389000
_diffrn_orient_matrix_UB_21      -0.0002277000
_diffrn_orient_matrix_UB_22      0.0240754000
_diffrn_orient_matrix_UB_23      0.0207591000
_diffrn_orient_matrix_UB_31      -0.0002069000
_diffrn_orient_matrix_UB_32      -0.0559577000
_diffrn_orient_matrix_UB_33      0.0089403000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41004
_diffrn_reflns_av_R_equivalents  0.1625
_diffrn_reflns_av_unetI/netI     0.2750
_diffrn_reflns_Laue_measured_fraction_full 0.306
_diffrn_reflns_Laue_measured_fraction_max 0.173
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            3884
_diffrn_reflns_point_group_measured_fraction_full 0.306
_diffrn_reflns_point_group_measured_fraction_max 0.173
_diffrn_reflns_theta_full        14.242
_diffrn_reflns_theta_max         21.475
_diffrn_reflns_theta_min         1.971
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.869
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12939
_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            yellow
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_description       prism
_exptl_crystal_F_000             1104
_exptl_crystal_preparation
'Mounted in a Membrane Diamond-Anvil Cell with using helium as pressure medium.'
_exptl_crystal_pressure_history
'Pressurized to 0.8 GPa and left to stabilize over 0.5 hours.'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.145
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2004
_refine_ls_number_restraints     632
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.4117
_refine_ls_R_factor_gt           0.1721
_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^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3743
_refine_ls_wR_factor_ref         0.4834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                432
_reflns_number_total             2004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5070.cif
_cod_data_source_block           crystal_4b
_cod_original_cell_volume        1945(5)
_cod_database_code               1572397
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C25 H24 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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C19-C18 = O1-C17
 1.2 with sigma of 0.05
 C18-Au1
 3.3 with sigma of 0.05
 C19-C17
 2.3 with sigma of 0.05
 C1-C13 \\sim C1-C15 \\sim C12-C14 \\sim C12-C2 \\sim C13-C15 \\sim C14-C2
\\sim C11-C9 \\sim C11-C15 ~
 C16-C10 \\sim C10-C12 \\sim C12-C16 \\sim C9-C15 \\sim C9-C7 \\sim C9-C5 \\sim
C7-C5 \\sim C8-C6 \\sim C8-C16
 \\sim C6-C16 \\sim C4-C2 \\sim C4-C16 \\sim C2-C16 \\sim C3-C15 \\sim C5-C15
\\sim C5-C3
 with sigma of 0.04
 C21-C20 \\sim C23-C22 \\sim C25-C24
 with sigma of 0.02
 P1-C20 \\sim P1-C22 \\sim P1-C24
 with sigma of 0.02
3. Restrained planarity
 C1, C14, C13, C12, C11, C10, C9, C8, C7, C6, C5, C4, C3, C2, C15, C16
 with sigma of 0.05
4. Uiso/Uaniso restraints and constraints
Au1 \\sim Au2: within 3A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 3A
Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(O1)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C25, C24, P1, C20, C21, C22, C23
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C14, C13, C12, C11, C10, C9, C8, C7, C6, C5, C16, C15, C2, C3, C4, C1, C17,
 O1, C18, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C22(H22A,H22B), C24(H24A,H24B)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C4(H4), C3(H3), C13(H13), C14(H14), C6(H6), C7(H7), C8(H8)
6.c Fitted hexagon refined as free rotating group:
 C15(C12,C13,C14,C1,C2), C16(C5,C6,C7,C8,C9)
6.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C)
;
_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 4.177
_oxdiff_exptl_absorpt_empirical_full_min 0.249