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_1572396
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-11-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                109.591(15)
_cell_angle_beta                 98.20(2)
_cell_angle_gamma                86.14(3)
_cell_formula_units_Z            4
_cell_length_a                   15.906(7)
_cell_length_b                   13.677(2)
_cell_length_c                   9.7733(14)
_cell_measurement_reflns_used    4078
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.384
_cell_measurement_theta_min      2.430
_cell_volume                     1982.2(10)
_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)'
_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 0.254
_diffrn_measured_fraction_theta_max 0.134
_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      -0.0258876000
_diffrn_orient_matrix_UB_12      0.0001834000
_diffrn_orient_matrix_UB_13      -0.0032837000
_diffrn_orient_matrix_UB_21      0.0000818000
_diffrn_orient_matrix_UB_22      0.0239816000
_diffrn_orient_matrix_UB_23      -0.0211926000
_diffrn_orient_matrix_UB_31      -0.0000805000
_diffrn_orient_matrix_UB_32      -0.0576522000
_diffrn_orient_matrix_UB_33      -0.0088302000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41004
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.1993
_diffrn_reflns_Laue_measured_fraction_full 0.254
_diffrn_reflns_Laue_measured_fraction_max 0.134
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4078
_diffrn_reflns_point_group_measured_fraction_full 0.254
_diffrn_reflns_point_group_measured_fraction_max 0.134
_diffrn_reflns_theta_full        14.242
_diffrn_reflns_theta_max         21.384
_diffrn_reflns_theta_min         2.430
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.835
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36244
_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    1.905
_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 measured without additional time for stabilization.'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.088
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3120
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.3242
_refine_ls_R_factor_gt           0.1229
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1727P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2712
_refine_ls_wR_factor_ref         0.3677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                886
_reflns_number_total             3120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5070.cif
_cod_data_source_block           crystal_4a
_cod_database_code               1572396
_shelx_shelxl_version_number     2018/3
_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
 C37-C21 = C17-C1
 1.45 with sigma of 0.04
 O2-C37 = O1-C17
 1.2 with sigma of 0.04
 C39-C38 = C19-C18
 1.18 with sigma of 0.1
 C112-C111 = C116-C115 = C114-C113 = C86-C85 = C82-C81 = C84-C83
 1.5 with sigma of 0.1
 P1-C85 = P1-C81 = P1-C83 = P4-C111 = P4-C115 = P4-C113
 1.75 with sigma of 0.1
 C19-C17 = C37-C39
 2.6 with sigma of 0.04
 Au1-C18 = C38-Au1
 3.2 with sigma of 0.1
 O1-C18 = O2-C38
 2.3 with sigma of 0.04
 O2-C21 = C1-O1
 2.4 with sigma of 0.1
 C18-C1
 2.41 with sigma of 0.04
 C5-C4 \\sim C4-C3 \\sim C3-C2 \\sim C2-C15 \\sim C16-C15 \\sim C5-C16 \\sim
C9-C16 \\sim C9-C10 \\sim C11-C10
 \\sim C12-C11 \\sim C15-C12
 with sigma of 0.02
 C32-C31 \\sim C31-C30 \\sim C30-C29 \\sim C36-C29 \\sim C36-C35 \\sim C35-C32
\\sim C35-C22 \\sim C23-C22
 \\sim C24-C23 \\sim C25-C24 \\sim C36-C25
 with sigma of 0.02
3. Restrained planarity
 C1, C3, C14, C2, C12, C15, C13, C4, C5, C16, C11, C10, C7, C9, C8, C6
 with sigma of 0.1
 C34, C22, C23, C21, C32, C36, C25, C24, C35, C33, C26, C29, C31, C27, C30, C28
 with sigma of 0.1
 C17, O1, C18, C19
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C115 \\sim C116 \\sim C111 \\sim C112 \\sim C113 \\sim C114: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C12 \\sim C15: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(C115) \\sim Ueq, Uanis(C116) \\sim Ueq, Uanis(C111) \\sim Ueq,
Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(C82)
\\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq: with sigma of 0.05 and
sigma for terminal atoms of 0.1
5. Rigid body (RIGU) restrains
 C86, C85, P1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C82, C81, P1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C84, C83, P1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C116, C115, P4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P4, C113, C114
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P4, C111, C112
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Au4(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C85(H85A,H85B), C81(H81A,H81B), C83(H83A,H83B), C113(H11A,H11B), C111(H11I,
 H11J), C115(H11K,H11L)
7.b Me refined with riding coordinates:
 C82(H82A,H82B,H82C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C114(H11C,H11D,
 H11E), C112(H11F,H11G,H11H), C116(H11M,H11N,H11O)
7.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C33(H33), C13(H13), C14(H14), C23(H23), C3(H3), C26(H26), C27(H27),
 C28(H28), C24(H24), C31(H31), C30(H30), C4(H4), C6(H6), C7(H7), C8(H8),
 C11(H11), C10(H10)
7.d Fitted hexagon refined as free rotating group:
 C34(C21,C22,C35,C32,C33), C1(C2,C15,C12,C13,C14), C36(C25,C26,C27,C28,C29),
 C5(C6,C7,C8,C9,C16)
;
_shelx_res_checksum              68376
_shelx_hkl_checksum              45793