Cooperative phenomenon of vapochromism and proton conduction of luminescent Pt(ii) complexes for the visualisation of proton conductivity.
Kobayashi, Atsushi; Imada, Shin-Ichiro; Wang, Dongjin; Nagao, Yuki; Yoshida, Masaki; Kato, Masako; Faraday discussions 225 (2021) 184–196; doi:10.1039/d0fd00001a

data_1557793
_publ_section_title
;
 Cooperative phenomenon of vapochromism and proton conduction of
 luminescent Pt(ii) complexes for the visualisation of proton
 conductivity.
;
_journal_name_full               'Faraday discussions'
_journal_page_first              184
_journal_page_last               196
_journal_paper_doi               10.1039/d0fd00001a
_journal_volume                  225
_journal_year                    2021
_chemical_formula_moiety         '2(C20 H15 Cl N4 Pt), 4.5(Cl), 4(O), 2(H2 O)'
_chemical_formula_sum            'C40 H34 Cl6.5 N8 O6 Pt2'
_chemical_formula_weight         1343.35
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-06 deposited with the CCDC.	2020-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                99.605(2)
_cell_angle_beta                 101.408(2)
_cell_angle_gamma                117.546(3)
_cell_formula_units_Z            2
_cell_length_a                   13.5911(4)
_cell_length_b                   14.4864(5)
_cell_length_c                   14.6981(4)
_cell_measurement_reflns_used    11626
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.9280
_cell_measurement_theta_min      3.2210
_cell_volume                     2401.45(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_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     15.00  58.00   0.50    1.47    --   46.37 -33.00  63.00   86
  2  \w     38.00  63.00   0.50    1.08    --  108.56 -33.00  63.00   50
  3  \w     37.00  69.00   0.50    1.08    --  108.56 -37.00 120.00   64
  4  \w     61.00 126.00   0.50    1.08    --  108.56 -77.00 150.00  130
  5  \w     69.00 108.00   0.50    1.08    --  108.56 -99.00  60.00   78
  6  \w     75.00 101.00   0.50    1.08    --  108.56 -77.00  30.00   52
  7  \w     60.00  86.00   0.50    1.08    --  108.56 -99.00   0.00   52
  8  \w     59.00 109.00   0.50    1.08    --  108.56 -99.00 -60.00  100
  9  \w     88.00 116.00   0.50    1.08    --  108.56-125.00-120.00   56
 10  \w     57.00  82.00   0.50    1.47    --   46.37-125.00-180.00   50
 11  \w     35.00  67.00   0.50    1.08    --  108.56 -37.00 -90.00   64
 12  \w     39.00  68.00   0.50    1.08    --  108.56 -37.00 -30.00   58
 13  \w     38.00  63.00   0.50    1.08    --  108.56 -19.00 -30.00   50
 14  \w     34.00  73.00   0.50    1.08    --  108.56 -19.00 -60.00   78
 15  \w     94.00 130.00   0.50    1.08    --  108.56  33.00-138.00   72
 16  \w    134.00 177.00   0.50    1.08    --  108.56  33.00-138.00   86
 17  \w     94.00 156.00   0.50    1.08    --  108.56 125.00  30.00  124
 18  \w     81.00 115.00   0.50    1.47    --   46.37 125.00 150.00   68
 19  \w     38.00  75.00   0.50    1.08    --  108.56 -19.00  90.00   74
 20  \w     33.00  69.00   0.50    1.08    --  108.56 -19.00  60.00   72
 21  \w     39.00  69.00   0.50    1.08    --  108.56 -37.00  90.00   60
 22  \w     46.00  71.00   0.50    1.08    --  108.56 -77.00  30.00   50
 23  \w     64.00  93.00   0.50    1.08    --  108.56 -99.00  30.00   58
 24  \w     36.00  98.00   0.50    1.08    --  108.56 -99.00 120.00  124
 25  \w     65.00 109.00   0.50    1.08    --  108.56 -99.00 150.00   88
 26  \w     35.00  66.00   0.50    1.08    --  108.56 -37.00 150.00   62
 27  \w     35.00  60.00   0.50    1.08    --  108.56 -37.00  60.00   50
 28  \w     36.00  69.00   0.50    1.08    --  108.56 -37.00  30.00   66
 29  \w     36.00 107.00   0.50    1.08    --  108.56 -99.00 -30.00  142
 30  \w     37.00  66.00   0.50    1.08    --  108.56 -37.00-120.00   58
 31  \w     37.00  62.00   0.50    1.08    --  108.56 -37.00-180.00   50
 32  \w     37.00  66.00   0.50    1.08    --  108.56 -37.00-150.00   58
 33  \w     44.00 105.00   0.50    1.08    --  108.56 -99.00-120.00  122
 34  \w     35.00  69.00   0.50    1.08    --  108.56 -37.00 -60.00   68
 35  \w     33.00  72.00   0.50    1.08    --  108.56 -19.00   0.00   78
 36  \w     33.00 121.00   0.50    1.47    --   46.37  33.00-138.00  176
 37  \w    -21.00  12.00   0.50    1.47    --   46.37 -33.00  63.00   66
 38  \w    -61.00  27.00   0.50    1.47    --  -46.37  19.00  30.00  176
 39  \w    -63.00 -38.00   0.50    1.08    --  -84.50  33.00-138.00   50
 40  \w    -41.00 -16.00   0.50    1.47    --  -46.37  33.00-138.00   50
 41  \w    -67.00 -14.00   0.50    1.08    --  -84.50  37.00 -30.00  106
 42  \w    -45.00 -11.00   0.50    1.47    --  -46.37 125.00-150.00   68
 43  \w    -94.00 -52.00   0.50    1.47    --  -46.37 125.00-150.00   84
 44  \w    -68.00 -19.00   0.50    1.08    --  -84.50  77.00   0.00   98
 45  \w   -121.00 -35.00   0.50    1.47    --  -46.37 -33.00  63.00  172
 46  \w   -154.00 -94.00   0.50    1.08    --  -84.50 -33.00  63.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27916
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         3.213
_exptl_absorpt_coefficient_mu    14.507
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_description       needle
_exptl_crystal_F_000             1289
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.118
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         8585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0801P)^2^+13.0867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1356
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7294
_reflns_number_total             8585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0fd00001a2.cif
_cod_data_source_block           o-Pt-HCl
_cod_depositor_comments
'Adding full bibliography for 1557791--1557793.cif.'
_cod_original_cell_volume        2401.44(14)
_cod_original_formula_sum        'C40 H34 Cl6.50 N8 O6 Pt2'
_cod_database_code               1557793
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: Cl7(0.5)
3.a Free rotating group:
 O3(H3A,H3B), O4(H4B,H4C)
3.b Aromatic/amide H refined with riding coordinates:
 N8(H8), C21(H21), C27(H27), C37(H37), C33(H33), C40(H40), C23(H23), C22(H22),
 C24(H24), C38(H38), C39(H39), C35(H35), C32(H32), C34(H34), C29(H29), N4(H4),
 C19(H19), C7(H7), C3(H3), C17(H17), C9(H9), C1(H1), C15(H15), C13(H13),
 C14(H14), C18(H18), C2(H2), C20(H20), C12(H12), C4(H4A)
;
_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
;