Chromic triboluminescence of self-assembled platinum(II) complexes.
Sasaki, Kono; Saito, Daisuke; Yoshida, Masaki; Tanaka, Fuka; Kobayashi, Atsushi; Sada, Kazuki; Kato, Masako; Chemical communications (Cambridge, England) 59 (2023) 6745–6748; doi:10.1039/d3cc01525d

data_7131623
_publ_section_title
;
 Chromic triboluminescence of self-assembled platinum(II) complexes.
;
_journal_issue                   44
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6745
_journal_page_last               6748
_journal_paper_doi               10.1039/d3cc01525d
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C13 H13 N5 Pt'
_chemical_formula_sum            'C13 H13 N5 Pt'
_chemical_formula_weight         434.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-19 deposited with the CCDC.	2023-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   13.75090(10)
_cell_length_b                   17.88980(10)
_cell_length_c                   21.4801(2)
_cell_measurement_reflns_used    15004
_cell_measurement_temperature    150
_cell_measurement_theta_max      77.4220
_cell_measurement_theta_min      3.1900
_cell_volume                     5284.12(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.962
_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     28.00  96.00   0.50    6.85    --   46.37   8.00-147.00  136
  2  \w     33.00  76.00   0.50    7.11    --  108.56 -19.00-180.00   86
  3  \w     42.00 109.00   0.50    7.11    --  108.56 -99.00-150.00  134
  4  \w     44.00  88.00   0.50    7.11    --  108.56-125.00-140.00   88
  5  \w     41.00 101.00   0.50    7.11    --  108.56 -99.00 -60.00  120
  6  \w     34.00 115.00   0.50    7.11    --  108.56  -8.00  38.00  162
  7  \w     37.00  93.00   0.50    7.11    --  108.56 -99.00 120.00  112
  8  \w     35.00  60.00   0.50    7.11    --  108.56 -37.00  90.00   50
  9  \w    -27.00  60.00   0.50    6.85    --   46.37 -37.00   0.00  174
 10  \w     92.00 117.00   0.50    6.85    --   46.37 145.00 104.00   50
 11  \w   -100.00 -74.00   0.50    7.11    --  -84.50-146.00 143.00   52
 12  \w   -145.00-119.00   0.50    7.11    --  -84.50-146.00 143.00   52
 13  \w   -116.00 -87.00   0.50    6.85    --  -46.37-125.00   0.00   58
;
_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  0.0398
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21810
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.616
_diffrn_reflns_theta_min         3.215
_exptl_absorpt_coefficient_mu    19.816
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.184
_exptl_crystal_description       needle
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.221
_refine_diff_density_min         -1.930
_refine_diff_density_rms         0.276
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.34(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         10146
_refine_ls_number_restraints     471
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0966P)^2^+29.1099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.700
_reflns_Friedel_fraction_full    0.913
_reflns_Friedel_fraction_max     0.824
_reflns_number_gt                9581
_reflns_number_total             10146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01525d6.cif
_cod_data_source_block           0315_et_et2o
_cod_depositor_comments
'Adding full bibliography for 7131620--7131623.cif.'
_cod_database_code               7131623
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.693
_shelx_estimated_absorpt_t_min   0.061
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.66(3)
 0.34(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N5B-C12B \\sim N5B-C14B
 with sigma of 0.02
 N5B-C13B \\sim N5B-C15B
 with sigma of 0.04
 C12B-C13B \\sim C14B-C15B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
5. Rigid body (RIGU) restrains
 C12B, C13B, C15B, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12B, C15B, C14B, C13B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2A, C1A, N2A, N1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H12E)=Sof(H12F)=Sof(C15B)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C14B)=
 Sof(H14A)=Sof(H14B)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(H14E)=1-FVAR(1)
 Sof(C12B)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(H12D)=Sof(C13B)=Sof(H13A)=
 Sof(H13B)=Sof(H13C)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C12D(H12I,H12J), C12B(H12A,H12B), C12C(H12G,H12H), C12A(H12E,H12F), C12A(H12C,
 H12D), C14B(H14A,H14B)
7.b Aromatic/amide H refined with riding coordinates:
 C10C(H10C), C3D(H3D), C7D(H7D), C7A(H7A), C10A(H10A), C10B(H10B), C11D(H11D),
 C3C(H3C), C3B(H3B), C11A(H11A), C7C(H7C), C11B(H11B), C7B(H7B), C4B(H4B),
 C4D(H4D), C11C(H11C), C3A(H3A), C4A(H4A), C4C(H4C), C10D(H10D)
7.c Idealised Me refined as rotating group:
 C6C(H6CA,H6CB,H6CC), C13C(H13G,H13H,H13I), C6A(H6AA,H6AB,H6AC), C6B(H6BA,H6BB,
 H6BC), C6D(H6DA,H6DB,H6DC), C13D(H13J,H13K,H13L), C13B(H13A,H13B,H13C),
 C15B(H15A,H15B,H15C), C13A(H13D,H13E,H13F), C14A(H14C,H14D,H14E)
;
_shelx_res_checksum              91315
_shelx_hkl_checksum              42976
_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
- Detector area scaling
;