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_1572398
_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         568.409
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2024-06-05
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.886(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0966(4)
_cell_length_b                   6.62840(13)
_cell_length_c                   17.9473(14)
_cell_measurement_reflns_used    597
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.6480
_cell_measurement_theta_min      2.0660
_cell_volume                     1896.77(16)
_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  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_environment
'Merill-Basset DAC with helium gas Paratone oil used as a pressure medium'
_diffrn_ambient_pressure         1100000(50000)
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.7095
_diffrn_measured_fraction_theta_max 0.5420
_diffrn_measurement_details
;
  1 phi    142.00  218.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
   0.0000    0.0000    0.0000     -     152
;
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       '\p scans'
_diffrn_measurement_specimen_support 'DAC, effective opening angle of 30 deg.'
_diffrn_orient_matrix_UB_11      0.0040118000
_diffrn_orient_matrix_UB_12      0.0461855000
_diffrn_orient_matrix_UB_13      0.0155586000
_diffrn_orient_matrix_UB_21      -0.0197822000
_diffrn_orient_matrix_UB_22      0.0312129000
_diffrn_orient_matrix_UB_23      -0.0114588000
_diffrn_orient_matrix_UB_31      -0.0160114000
_diffrn_orient_matrix_UB_32      -0.0275491000
_diffrn_orient_matrix_UB_33      0.0129229000
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41097
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.7095
_diffrn_reflns_Laue_measured_fraction_max 0.5420
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3932
_diffrn_reflns_point_group_measured_fraction_full 0.7095
_diffrn_reflns_point_group_measured_fraction_max 0.5420
_diffrn_reflns_theta_full        14.2753
_diffrn_reflns_theta_max         18.14
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.990
_exptl_crystal_description       block
_exptl_crystal_F_000             1102.600
_exptl_crystal_preparation
'3 pieces from the same block mounted in a Merill-Basset Diamond-Anvil Cell using Paratone oil as pressure medium.'
_exptl_crystal_pressure_history
'pressurized to 1.1 GPa and left to stabilize over 20 min.'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.3421
_refine_diff_density_min         -2.1037
_refine_diff_density_rms         0.2554
_refine_ls_d_res_high            0.6602
_refine_ls_d_res_low             6.2107
_refine_ls_goodness_of_fit_ref   1.0247
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    39
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0247
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1273P)^2^+1.6491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.2290
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                1955
_reflns_number_total             3740
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            lt5070.cif
_cod_data_source_block           crystal_5
_cod_database_code               1572398
_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.a Secondary CH2 refined with riding coordinates:
 C20(H20a,H20b), C22(H22a,H22b), C24(H24a,H24b)
2.b Me refined with riding coordinates:
 C21(H21a,H21b,H21c), C23(H23a,H23b,H23c), C25(H25a,H25b,H25c)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C10(H10), C11(H11), C13(H13), C14(H14), C6(H6), C7(H7), C8(H8)
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         R2SCAN
   BASIS SET:      x2c-TZVP
   CHARGE:         0
   MULTIPLICITY:   1
   RELATIVISTIC:   DKH2
   DATE:           2024-05-19_19-46-48
;
_olex2_submission_special_instructions 'No special instructions were received'