Luminescence behaviour of Au(I)-Cu(I) heterobimetallic coordination polymers based on alkynyl-tris(2-pyridyl)phosphine Au(I) complexes.
Petrovskii, Stanislav K.; Paderina, Aleksandra V.; Sizova, Anastasia A.; Baranov, Andrey Yu; Artem'ev, Alexander A.; Sizov, Vladimir V.; Grachova, Elena V.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13430–13439; doi:10.1039/d0dt02583f

data_7705340
_publ_section_title
;
 Luminescence behaviour of Au(I)-Cu(I) heterobimetallic coordination
 polymers based on alkynyl-tris(2-pyridyl)phosphine Au(I) complexes.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13430
_journal_page_last               13439
_journal_paper_doi               10.1039/d0dt02583f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'2(C69 H51 Au3 Cu3 N9 P3), 6(B F4), 6(C H1.50 N0.50)'
_chemical_formula_sum            'C144 H111 Au6 B6 Cu6 F24 N21 P6'
_chemical_formula_weight         4405.34
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc25k7jj
_audit_creation_date             2020-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-27 deposited with the CCDC.	2020-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   15.2140(2)
_cell_length_b                   15.2140(2)
_cell_length_c                   19.3663(2)
_cell_measurement_reflns_used    23100
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      75.9760
_cell_measurement_theta_min      4.0160
_cell_volume                     3882.08(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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    -67.00  25.00   1.00    1.72    --  -40.38  38.00 -90.00   92
  2  \w     53.00  81.00   1.00    1.72    --   40.38 -99.00  60.00   28
  3  \w     32.00  86.00   1.00    6.88    --  113.00 -95.00  60.00   54
  4  \w     56.00 104.00   1.00    6.88    --  113.00 -95.00 120.00   48
  5  \w     86.00 175.00   1.00    6.88    --  113.00  45.00 150.00   89
  6  \w    102.00 176.00   1.00    6.88    --  113.00 112.00  90.00   74
  7  \w    102.00 127.00   1.00    6.88    --  113.00 112.00  30.00   25
  8  \w     88.00 116.00   1.00    1.72    --   40.38 178.00 -30.00   28
  9  \w     92.00 177.00   1.00    6.88    --  113.00  77.00-120.00   85
 10  \w    101.00 127.00   1.00    6.88    --  113.00 112.00-180.00   26
 11  \w     77.00 142.00   1.00    6.88    --  113.00 -77.00-180.00   65
 12  \w     36.00 115.00   1.00    6.88    --  113.00-112.00-150.00   79
 13  \w     31.00  60.00   1.00    6.88    --  113.00 -95.00-150.00   29
 14  \w   -116.00 -14.00   1.00    1.72    --  -40.38 -38.00  90.00  102
 15  \w    -71.00 -45.00   1.00    1.72    --  -40.38 -38.00-150.00   26
 16  \w   -124.00 -35.00   1.00    1.72    --  -40.38-178.00-120.00   89
 17  \w   -112.00 -82.00   1.00    1.72    --  -40.38 -38.00-150.00   30
 18  \w    -72.00 -35.00   1.00    1.72    --  -40.38-178.00  60.00   37
 19  \w      2.00  75.00   1.00    1.72    --   40.38 -99.00 150.00   73
 20  \w    109.00 166.00   1.00    6.88    --  113.00 112.00-150.00   57
 21  \w     41.00 115.00   1.00    6.88    --  113.00-112.00  30.00   74
 22  \w    115.00 167.00   1.00    6.88    --  113.00 112.00 -30.00   52
 23  \w     89.00 115.00   1.00    6.88    --  113.00-112.00 -60.00   26
 24  \w     45.00  72.00   1.00    6.88    --  113.00-112.00  60.00   27
 25  \w     96.00 122.00   1.00    6.88    --  113.00  61.00  60.00   26
 26  \w     75.00 101.00   1.00    6.88    --  113.00 -95.00 -60.00   26
 27  \w    153.00 178.00   1.00    6.88    --  113.00 112.00 -90.00   25
 28  \w     82.00 177.00   1.00    6.88    --  113.00  30.00 -30.00   95
 29  \w     82.00 109.00   1.00    6.88    --  113.00 -95.00  60.00   27
 30  \w     95.00 135.00   1.00    6.88    --  113.00 -45.00  30.00   40
 31  \w     39.00 101.00   1.00    6.88    --  113.00 -45.00-180.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0559297000
_diffrn_orient_matrix_UB_12      0.1162590000
_diffrn_orient_matrix_UB_13      -0.0075407000
_diffrn_orient_matrix_UB_21      -0.0815093000
_diffrn_orient_matrix_UB_22      0.0042464000
_diffrn_orient_matrix_UB_23      0.0447919000
_diffrn_orient_matrix_UB_31      0.0624226000
_diffrn_orient_matrix_UB_32      0.0105938000
_diffrn_orient_matrix_UB_33      0.0653498000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36133
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.498
_diffrn_reflns_theta_min         3.354
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.535
_exptl_absorpt_correction_T_max  0.155
_exptl_absorpt_correction_T_min  0.092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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    1.901
_exptl_crystal_description       block
_exptl_crystal_F_000             2127
_exptl_crystal_recrystallization_method 'acetonitrile-diethyl ether'
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.306
_exptl_crystal_size_min          0.237
_refine_diff_density_max         2.419
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details
;
 Flack x determined using 2186 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.032(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5133
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0686P)^2^+2.2093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0922
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5008
_reflns_number_total             5133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02583f3.cif
_cod_data_source_block           3ver0-11226-ps003_1
_cod_depositor_comments
'Adding full bibliography for 7705338--7705340.cif.'
_cod_original_cell_volume        3882.07(11)
_cod_database_code               7705340
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C46 H34 N6 P2 Au2 Cu1 B1 F4'
_shelx_estimated_absorpt_t_max   0.155
_shelx_estimated_absorpt_t_min   0.092
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N4-C24
 1.16 with sigma of 0.01
 C24-C25
 1.468 with sigma of 0.01
 C22-C21 \\sim C20-C19 \\sim C18-C23
 with sigma of 0.02
 C23-C20A \\sim C21A-C22A \\sim C23A-C18A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C18) = Uanis(C23)
Uanis(C21) = Uanis(C20)
Uanis(C22) = Uanis(C19A)
Uanis(C18) = Uanis(C19A)
Uanis(C18A) = Uanis(C19A)
Uanis(C22) = Uanis(C21)
4. Others
 Fixed Sof: C17(0.5) C17A(0.5) C18(0.5) C18A(0.5) C19(0.5) H19(0.5) C19A(0.5)
 H19A(0.5) C20(0.5) H20(0.5) C20A(0.5) H20A(0.5) C21(0.5) H21(0.5) C21A(0.5)
 H21A(0.5) C22(0.5) H22(0.5) C22A(0.5) H22A(0.5) C23(0.5) H23(0.5) C23A(0.5)
 H23A(0.5) N4(0.5) C24(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
 Fixed Uiso: H25A(0.06129)
5.a Free rotating group:
 N4(C24,C25,H25A,H25B,H25C)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11),
 C12(H12), C13(H13), C14(H14), C19(H19), C19A(H19A), C20(H20), C20A(H20A),
 C21(H21), C21A(H21A), C22(H22), C22A(H22A), C23(H23), C23A(H23A)
;
_shelx_res_checksum              9502
_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 1.599
_oxdiff_exptl_absorpt_empirical_full_min 0.660