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_1572395
_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_coeditor_code           LT5070
_journal_issue                   5
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524007681
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety         '0.25(C100 H96 Au4 O4 P4)'
_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             2024-04-17
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb for OlexSys, GUI svn.r6869)
;
_cell_angle_alpha                109.816(4)
_cell_angle_beta                 98.398(2)
_cell_angle_gamma                85.874(3)
_cell_formula_units_Z            4
_cell_length_a                   16.0839(5)
_cell_length_b                   14.2240(7)
_cell_length_c                   10.1393(3)
_cell_measurement_reflns_used    11269
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9040
_cell_measurement_theta_min      3.1020
_cell_volume                     2158.26(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.0013
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -34.00  -3.00   1.00   20.00    --   33.59 126.00-143.71   31
  2  \w     49.00 116.00   1.00   20.00    --   33.59 160.00-150.00   67
  3  \w    -19.00  86.00   1.00   20.00    --   33.59 -99.00 -30.00  105
  4  \w    -43.00  68.00   1.00   20.00    --   33.59 -37.00 -30.00  111
  5  \w   -107.00  -1.00   1.00   20.00    --  -33.91 -57.00-150.00  106
  6  \w   -108.00  -2.00   1.00   20.00    --  -33.91 -57.00 -30.00  106
  7  \w    -40.00  39.00   1.00   20.00    --  -33.91  57.00-180.00   79
  8  \w   -108.00  -3.00   1.00   20.00    --  -33.91 -57.00 -90.00  105
  9  \w    -70.00  43.00   1.00   20.00    --  -33.91  77.00-120.00  113
 10  \w   -105.00  -1.00   1.00   20.00    --  -33.91 -57.00 120.00  104
 11  \w   -107.00 -82.00   1.00   20.00    --  -33.91 -77.00  60.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            42542
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.117
_exptl_absorpt_coefficient_mu    6.903
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.011
_refine_diff_density_min         -1.472
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         13173
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+1.6049P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9022
_reflns_number_total             13173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5070.cif
_cod_data_source_block           crystal_1
_cod_database_code               1572395
_shelxl_version_number           2013-2
_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
 C204-C203 = C104-C103
 1.5 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C204 \\sim C104 \\sim C203 \\sim C103: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
4. Others
 Sof(C203)=Sof(H20A)=Sof(H20B)=Sof(C204)=Sof(H20C)=Sof(H20D)=Sof(H20E)=0.5*(1-
 FVAR(2))
 Sof(C104)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C103)=Sof(H10D)=Sof(H10E)=0.5*
 FVAR(2)
 Fixed Sof: Au4(0.5) P3(0.5) P4(0.5) C113(0.5) H11A(0.5) H11B(0.5) C114(0.5)
 H11C(0.5) H11D(0.5) H11E(0.5) C112(0.5) H11F(0.5) H11G(0.5) H11H(0.5)
 C111(0.5) H11I(0.5) H11J(0.5) C115(0.5) H11K(0.5) H11L(0.5) C116(0.5)
 H11M(0.5) H11N(0.5) H11O(0.5) C102(0.5) H10F(0.5) H10G(0.5) H10H(0.5)
 C101(0.5) H10I(0.5) H10J(0.5) C105(0.5) H10K(0.5) H10L(0.5) C106(0.5)
 H10M(0.5) H10N(0.5) H10O(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C85(H85A,H85B), C81(H81A,H81B), C83(H83A,H83B), C113(H11A,H11B), C103(H10D,
 H10E), C111(H11I,H11J), C115(H11K,H11L), C101(H10I,H10J), C105(H10K,H10L),
 C203(H20A,H20B)
5.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C23(H23), C3(H3), C24(H24), C14(H14), C33(H33), C26(H26), C31(H31),
 C13(H13), C27(H27), C30(H30), C4(H4), C28(H28), C11(H11), C10(H10), C7(H7),
 C8(H8), C6(H6)
5.c Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C104(H10A,H10B,
 H10C), C114(H11C,H11D,H11E), C112(H11F,H11G,H11H), C116(H11M,H11N,H11O),
 C102(H10F,H10G,H10H), C106(H10M,H10N,H10O), C204(H20C,H20D,H20E)
;
_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
;