Elastic deformability and luminescence of crystals of polyhalogenated platinum(ii)‒bipyridine complexes
Yoshida, Masaki; Makino, Yusuke; Sasaki, Toshiyuki; Sakamoto, Shunichi; Takamizawa, Satoshi; Kobayashi, Atsushi; Kato, Masako; CrystEngComm 23 (2021) 5891–5898; doi:10.1039/D1CE00459J

data_7243022
_publ_section_title
;
 Elastic deformability and luminescence of crystals of polyhalogenated
 platinum(ii)--bipyridine complexes
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              5891
_journal_page_last               5898
_journal_paper_doi               10.1039/D1CE00459J
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C10 H6 Cl4 N2 Pt, 0.333(C H4 O)'
_chemical_formula_sum            'C10.33 H7.33 Cl4 N2 O0.33 Pt'
_chemical_formula_weight         501.74
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-03-28 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                99.217(2)
_cell_angle_beta                 97.693(2)
_cell_angle_gamma                94.038(2)
_cell_formula_units_Z            6
_cell_length_a                   7.3163(2)
_cell_length_b                   12.5322(4)
_cell_length_c                   22.0934(3)
_cell_measurement_reflns_used    9690
_cell_measurement_temperature    150
_cell_measurement_theta_max      76.1560
_cell_measurement_theta_min      3.5760
_cell_volume                     1972.82(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.959
_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    -62.00 -37.00   0.50    3.69    --  -46.37  60.00 106.00   50
  2  \w     -5.00  24.00   0.50    3.69    --  -46.37  60.00 106.00   58
  3  \w     30.00 118.00   0.50    3.69    --   46.37  60.00 106.00  176
  4  \w     93.00 177.00   0.50    4.14    --  108.56  60.00 106.00  168
  5  \w    135.00 170.00   0.50    4.14    --  108.56  19.00  60.00   70
  6  \w     98.00 125.00   0.50    4.14    --  108.56  19.00  60.00   54
  7  \w     96.00 178.00   0.50    4.14    --  108.56  37.00   0.00  164
  8  \w     88.00 130.00   0.50    4.14    --  108.56 -77.00 120.00   84
  9  \w     60.00 109.00   0.50    4.14    --  108.56 -60.00 -33.00   98
 10  \w     77.00 116.00   0.50    4.14    --  108.56-125.00 -60.00   78
 11  \w     56.00 116.00   0.50    4.14    --  108.56-125.00 -30.00  120
 12  \w     35.00  68.00   0.50    4.14    --  108.56 -37.00  90.00   66
 13  \w     42.00  70.00   0.50    4.14    --  108.56 -19.00 120.00   56
 14  \w     38.00  63.00   0.50    4.14    --  108.56 -37.00 150.00   50
 15  \w     35.00  76.00   0.50    4.14    --  108.56 -19.00  90.00   82
 16  \w     35.00  63.00   0.50    4.14    --  108.56 -19.00  30.00   56
 17  \w     42.00  69.00   0.50    4.14    --  108.56 -37.00   0.00   54
 18  \w     37.00 105.00   0.50    4.14    --  108.56 -99.00 -30.00  136
 19  \w     36.00  67.00   0.50    4.14    --  108.56 -37.00-120.00   62
 20  \w     36.00  68.00   0.50    4.14    --  108.56 -37.00-150.00   64
 21  \w     43.00  69.00   0.50    4.14    --  108.56 -19.00-150.00   52
 22  \w     33.00  58.00   0.50    4.14    --  108.56 -19.00-180.00   50
 23  \w     27.00  63.00   0.50    3.69    --   46.37 -60.00 -33.00   72
 24  \w     41.00  71.00   0.50    4.14    --  108.56-125.00 -60.00   60
 25  \w     41.00 115.00   0.50    4.14    --  108.56-125.00 -90.00  148
 26  \w     39.00 104.00   0.50    4.14    --  108.56 -99.00  30.00  130
 27  \w     58.00 100.00   0.50    4.14    --  108.56 -99.00 120.00   84
 28  \w     54.00 116.00   0.50    4.14    --  108.56-125.00 120.00  124
 29  \w     38.00  99.00   0.50    4.14    --  108.56 -99.00 150.00  122
 30  \w     38.00  65.00   0.50    4.14    --  108.56 -37.00 120.00   54
 31  \w    -21.00  10.00   0.50    3.69    --   46.37 -60.00 -33.00   62
 32  \w    -61.00 -33.00   0.50    3.69    --  -46.37  57.00-150.00   56
 33  \w    -20.00  26.00   0.50    3.69    --  -46.37  57.00-150.00   92
 34  \w     71.00 115.00   0.50    3.69    --   46.37 125.00 -30.00   88
 35  \w    -65.00 -27.00   0.50    4.14    --  -84.50 125.00 -60.00   76
 36  \w    -94.00 -10.00   0.50    3.69    --  -46.37 125.00  60.00  168
 37  \w    -99.00 -11.00   0.50    4.14    --  -84.50  60.00 106.00  176
 38  \w   -109.00 -30.00   0.50    3.69    --  -46.37 -60.00 -33.00  158
 39  \w   -118.00 -91.00   0.50    4.14    --  -84.50-125.00  90.00   54
 40  \w   -153.00-100.00   0.50    4.14    --  -84.50 -60.00 -33.00  106
 41  \w   -155.00-126.00   0.50    4.14    --  -84.50-125.00  90.00   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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0034186000
_diffrn_orient_matrix_UB_12      0.1123917000
_diffrn_orient_matrix_UB_13      0.0405961000
_diffrn_orient_matrix_UB_21      0.1989856000
_diffrn_orient_matrix_UB_22      -0.0102307000
_diffrn_orient_matrix_UB_23      0.0301366000
_diffrn_orient_matrix_UB_31      0.0770817000
_diffrn_orient_matrix_UB_32      0.0539505000
_diffrn_orient_matrix_UB_33      -0.0504462000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24125
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.744
_diffrn_reflns_theta_min         2.048
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    27.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45h (Rigaku Oxford Diffraction, 2018)
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    2.534
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.378
_refine_diff_density_min         -1.566
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0705P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7050
_reflns_number_total             8060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00459j3.cif
_cod_data_source_block           1-MeOH
_cod_depositor_comments
'Adding full bibliography for 7243022--7243026.cif.'
_cod_database_code               7243022
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C10H6N2PtCl4
_shelx_estimated_absorpt_t_max   0.171
_shelx_estimated_absorpt_t_min   0.045
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9B(H9B), C10B(H10B), C9A(H9A), C1B(H1B), C7C(H7C), C10A(H10A), C4A(H4A),
 C7B(H7B), C1A(H1A), C4C(H4C), C7A(H7A), C9C(H9C), C4B(H4B), C1C(H1C),
 C10C(H10C), C2A(H2A), C2B(H2B), C2C(H2C)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              69102
_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 1.535
_oxdiff_exptl_absorpt_empirical_full_min 0.568