Solution versus solid-state dual emission of the Au(i)-alkynyl diphosphine complexes via modification of polyaromatic spacers
Belyaev, Andrey; Kolesnikov, Ilya; Melnikov, Alexei S.; Gurzhiy, Vladislav V.; Tunik, Sergey P.; Koshevoy, Igor O.; New Journal of Chemistry 43 (2019) 13741–; doi:10.1039/C9NJ03426A

data_7058743
_publ_section_title
;
 Solution versus solid-state dual emission of the Au(i)-alkynyl
 diphosphine complexes via modification of polyaromatic spacers
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13741
_journal_paper_doi               10.1039/C9NJ03426A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C48 H42 Au2 O2 P2, 0.18(C H2 Cl2)'
_chemical_formula_sum            'C48.18 H42.36 Au2 Cl0.36 O2 P2'
_chemical_formula_weight         1121.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.12 svn.r2899 for OlexSys, GUI svn.r4796)
;
_audit_update_record
;
2015-03-17 deposited with the CCDC.    2019-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.243(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0271(2)
_cell_length_b                   15.4167(3)
_cell_length_c                   33.6004(7)
_cell_measurement_reflns_used    18436
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.6164
_cell_measurement_theta_min      2.8639
_cell_volume                     4676.06(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega  -44.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0037   38.0000  120.0000 32

  2 omega   -8.00   35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0037   38.0000  120.0000 43

  3 omega  -96.00  -44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0037  126.0000  -90.0000 52

  4 omega  -41.00  -16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0037  -38.0000 -180.0000 25

  5 omega -114.00  -11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0037  -57.0000  -30.0000 103

  6 omega   13.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0037   57.0000  -90.0000 31

  7 omega   58.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  150.0000 27

  8 omega   35.00   60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -60.0000 25

  9 omega   48.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -24.0000  114.6368 39

 10 omega  113.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  150.0000 27

 11 omega   45.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -60.0000 36

 12 omega   40.00   97.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -30.0000 57

 13 omega   87.00  150.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   90.0000 63

 14 omega   75.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000 -180.0000 34

 15 omega   57.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  150.0000 44

 16 omega   44.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -180.0000 27

 17 omega  123.00  150.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000    0.0000 27

 18 omega   82.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000    0.0000 39

 19 omega   87.00  172.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   90.0000 85

 20 omega   35.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000    0.0000 56

 21 omega   61.00  110.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  150.0000 49

 22 omega   57.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000 -120.0000 52

 23 omega  111.00  136.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -180.0000 25

 24 omega   96.00  145.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   60.0000 49

 25 omega   55.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -180.0000 37

 26 omega   93.00  120.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000  -60.0000 27

 27 omega   39.00   64.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   90.0000 25

 28 omega   56.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  -60.0000 28

 29 omega  113.00  144.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  -60.0000 31

 30 omega   54.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  150.0000 45

 31 omega   59.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000  -60.0000 33

 32 omega   90.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -180.0000 25

 33 omega   72.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000    0.0000 27

 34 omega   60.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  120.0000 33

 35 omega  107.00  136.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000  150.0000 29

 36 omega  148.00  173.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000  150.0000 25

 37 omega   46.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -30.0000 60

 38 omega   70.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  150.0000 28

 39 omega   81.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000   30.0000 27

 40 omega   96.00  123.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -30.0000 27

 41 omega   78.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -67.0000  -87.7213 25

 42 omega  104.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -85.0000  139.2674 35
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1635675000
_diffrn_orient_matrix_UB_12      0.0283463000
_diffrn_orient_matrix_UB_13      -0.0016461000
_diffrn_orient_matrix_UB_21      0.0056770000
_diffrn_orient_matrix_UB_22      0.0027738000
_diffrn_orient_matrix_UB_23      0.0458101000
_diffrn_orient_matrix_UB_31      0.0487508000
_diffrn_orient_matrix_UB_32      -0.0957211000
_diffrn_orient_matrix_UB_33      0.0008666000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            38843
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.475
_diffrn_reflns_theta_min         4.881
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.726
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lamina
_exptl_crystal_F_000             2166
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.880
_refine_diff_density_min         -3.112
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         8344
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0603
_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^)+(0.1077P)^2^+22.7186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7408
_reflns_number_total             8344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03426a2.cif
_cod_data_source_block           Complex_3
_cod_depositor_comments
'Adding full bibliography for 7058741--7058748.cif.'
_cod_original_cell_volume        4676.04(18)
_cod_database_code               7058743
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 95.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95
_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, All O(H) groups
2. Restrained distances
 O2B-C47B
 2.5 with sigma of 0.02
 O2A-O2B
 0.4 with sigma of 0.02
 H2B-O1_$1
 2.1 with sigma of 0.02
 C49-Cl2
 1.8 with sigma of 0.02
 Cl1-Cl2
 2.7 with sigma of 0.02
 C49-Cl1
 1.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C27A) = Uanis(C32A) = Uanis(C31A) = Uanis(C30A) = Uanis(C31B) =
Uanis(C30B) = Uanis(C29B) = Uanis(C28B) = Uanis(C29A) = Uanis(C28A) =
Uanis(C32B) = Uanis(C27B)
Uanis(C45) = Uanis(C44)
Uanis(C48A) = Uanis(C48B) = Uanis(C47B) = Uanis(C47A) = Uanis(O2A) = Uanis(O2B)
= Uanis(C39A) = Uanis(C39B) = Uanis(C40A) = Uanis(C40B) = Uanis(C46A) =
Uanis(C46B)
Uanis(Cl1) = Uanis(C49) = Uanis(Cl2)
4. Others
 Sof(Au2B)=Sof(O2B)=Sof(H2B)=Sof(C27B)=Sof(C32B)=Sof(H32B)=Sof(C31B)=Sof(H31B)=
 Sof(C30B)=Sof(H30B)=Sof(C29B)=Sof(H29B)=Sof(C28B)=Sof(H28B)=Sof(C39B)=
 Sof(C40B)=Sof(C46B)=Sof(C47B)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(C48B)=
 Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(1)
 Sof(Au2A)=Sof(O2A)=Sof(H2A)=Sof(C27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=
 Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C39A)=
 Sof(C40A)=Sof(C46A)=Sof(C47A)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48A)=
 Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(1)
 Fixed Sof: Cl1(0.18) Cl2(0.18) C49(0.18) H49A(0.18) H49B(0.18)
5.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B)
5.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C19(H19), C18(H18), C17(H17), C16(H16), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C13(H13), C12(H12), C11(H11), C10(H10), C6(H6),
 C5(H5), C4(H4), C3(H3), C38(H38), C37(H37), C36(H36), C35(H35), C34(H34),
 C28A(H28A), C29A(H29A), C30A(H30A), C31A(H31A), C32A(H32A), C32B(H32B),
 C31B(H31B), C30B(H30B), C29B(H29B), C28B(H28B)
5.c Fitted hexagon refined as free rotating group:
 C27A(C28A,C29A,C30A,C31A,C32A), C27B(C32B,C31B,C30B,C29B,C28B)
5.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47A(H47A,H47B,H47C), C48A(H48A,
 H48B,H48C), C47B(H47D,H47E,H47F), C48B(H48D,H48E,H48F)
5.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2A(H2A), O2B(H2B)
;