(Ar-CO-C[triple bond, length as m-dash]C)(PEt<sub>3</sub>)Au and (Ar-C[triple bond, length as m-dash]C)(PEt<sub>3</sub>)Au complexes bearing pyrenyl and ferrocenyl groups: synthesis, structure, and luminescence properties.
Głodek, Marta; Makal, Anna; Paluch, Piotr; Kadziołka-Gaweł, Mariola; Kobayashi, Yasuhiro; Zakrzewski, Janusz; Plażuk, Damian; Dalton transactions (Cambridge, England : 2003) 47 (2018) 6702–6712; doi:10.1039/c8dt01061g

data_7046029
_publ_section_title
;
 (Ar-CO-C[triple bond, length as m-dash]C)(PEt<sub>3</sub>)Au and
 (Ar-C[triple bond, length as m-dash]C)(PEt<sub>3</sub>)Au complexes
 bearing pyrenyl and ferrocenyl groups: synthesis, structure, and
 luminescence properties.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6702
_journal_page_last               6712
_journal_paper_doi               10.1039/c8dt01061g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.5(C100 H96 Au4 O4 P4)'
_chemical_formula_sum            'C50 H48 Au2 O2 P2'
_chemical_formula_weight         1136.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-11-21
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-21 deposited with the CCDC.
2018-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                86.4576(6)
_cell_angle_beta                 81.5703(6)
_cell_angle_gamma                69.9495(8)
_cell_formula_units_Z            4
_cell_length_a                   9.97212(8)
_cell_length_b                   13.96926(13)
_cell_length_c                   32.1775(2)
_cell_measurement_reflns_used    82395
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      47.7780
_cell_measurement_theta_min      1.9900
_cell_volume                     4164.94(6)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0026
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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 -77.00 43.00 0.50 7.50 -- 0.71 -57.00 90.00 240 2 \w -94.00 -49.00 0.50 7.50 -- 0.71-160.00-120.00 90 3 \w -86.00 64.00 0.50 7.50 -- -1.03 -37.00 -30.00 300 4 \w -58.00 -1.00 0.50 7.50 -- 12.00 124.00 145.19 114 5 \w -51.00 -2.00 0.50 7.50 -- 20.00 125.00-133.22 98 6 \w -43.00 -2.00 0.50 30.00 -- 28.00 125.00 -36.45 82 7 \w -3.00 33.00 0.50 30.00 -- 48.84 89.00 1.17 72 8 \w 3.00 137.00 0.50 30.00 -- 48.84 77.00 120.00 268 9 \w 8.00 128.00 0.50 30.00 -- 48.84 61.00 -60.00 240 10 \w -30.00 90.00 0.50 30.00 -- 48.84 -61.00 -60.00 240 11 \w 8.00 128.00 0.50 30.00 -- 48.84 61.00 0.00 240 12 \w -2.00 131.00 0.50 30.00 -- 48.84 45.00 90.00 266 13 \w -106.00 -41.00 0.50 7.50 -- -24.45 -47.00-119.00 130 14 \w -78.00 -51.00 0.50 25.00 -- -72.58 -47.00-119.00 54 15 \w 21.00 92.00 0.50 7.50 -- 23.83 57.00-150.00 142 16 \w -93.00 -49.00 0.50 7.50 -- -24.45-160.00 -30.00 88 17 \w -117.00 -33.00 0.50 7.50 -- -24.45 160.00 60.00 168 18 \w -116.00 -53.00 0.50 7.50 -- -24.45-160.00 120.00 126 19 \w -5.00 20.00 0.50 25.00 -- 52.00 98.00 33.84 50 20 \w -4.00 21.00 0.50 25.00 -- 52.00 98.00-132.07 50 21 \w 2.00 27.00 0.50 25.00 -- 56.00 92.00 -10.31 50 22 \w 2.00 28.00 0.50 25.00 -- 56.00 92.00 150.85 52 23 \w 2.00 27.00 0.50 25.00 -- 56.00 92.00-145.38 50 24 \w 2.00 27.00 0.50 25.00 -- 56.00 92.00 101.93 50 25 \w 3.00 28.00 0.50 25.00 -- 56.00 91.00 -63.46 50 26 \w 11.00 36.00 0.50 25.00 -- 60.00 84.00 -74.58 50 27 \w 21.00 46.00 0.50 25.00 -- 68.00 79.00 -38.18 50 28 \w 20.00 45.00 0.50 25.00 -- 68.00 81.00 17.34 50 29 \w 93.00 155.00 0.50 25.00 -- 71.95 160.00 30.00 124 30 \w 91.00 158.00 0.50 25.00 -- 71.95 160.00-150.00 134 31 \w 49.00 75.00 0.50 25.00 -- 71.95 160.00-150.00 52 32 \w -18.00 125.00 0.50 25.00 -- 71.95 -91.00 120.00 286 33 \w -66.00 -27.00 0.50 25.00 -- -72.58 -77.00 9.37 78 34 \w -159.00 -89.00 0.50 25.00 -- -72.58 -77.00 9.37 140 35 \w
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0315169000
_diffrn_orient_matrix_UB_12      0.0384310000
_diffrn_orient_matrix_UB_13      0.0000813000
_diffrn_orient_matrix_UB_21      -0.0103317000
_diffrn_orient_matrix_UB_22      0.0119351000
_diffrn_orient_matrix_UB_23      -0.0213033000
_diffrn_orient_matrix_UB_31      -0.0688297000
_diffrn_orient_matrix_UB_32      0.0360924000
_diffrn_orient_matrix_UB_33      0.0065440000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71072
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            99159
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.920
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.154
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_correction_T_min  0.381
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model 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    1.813
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.109
_refine_diff_density_max         2.655
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1017
_refine_ls_number_reflns         24186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0206
_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^)+(0.0077P)^2^+5.8115P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0428
_refine_ls_wR_factor_ref         0.0436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22638
_reflns_number_total             24186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01061g2.cif
_cod_data_source_block           pircoccaupet3_2
_cod_depositor_comments
'Adding full bibliography for 7046025--7046029.cif.'
_cod_database_code               7046029
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C25 H24 O P Au'
_reflns_odcompleteness_completeness 89.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     47.63
_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. Others
 Fixed Z: Au1(0.75221) Au2(0.75173) Au3(0.74801) Au4(0.752399)
3.a Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B), C83(H83A,H83B), C85(H85A,H85B), C91(H91A,H91B), C93(H93A,
 H93B), C95(H95A,H95B), C101(H10A,H10B), C103(H10F,H10G), C105(H10K,H10L),
 C111(H11A,H11B), C113(H11F,H11G), C115(H11K,H11L)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31),
  C33(H33), C34(H34), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48),
 C50(H50), C51(H51), C53(H53), C54(H54), C63(H63), C64(H64), C66(H66), C67(H67),
  C68(H68), C70(H70), C71(H71), C73(H73), C74(H74)
3.c Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C92(H92A,H92B,
 H92C), C94(H94A,H94B,H94C), C96(H96A,H96B,H96C), C102(H10C,H10D,H10E),
 C104(H10H,H10I,H10J), C106(H10M,H10N,H10O), C112(H11C,H11D,H11E), C114(H11H,
 H11I,H11J), C116(H11M,H11N,H11O)
;
_olex2_date_sample_data_collection 2017-10-27
_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 1.297
_oxdiff_exptl_absorpt_empirical_full_min 0.828