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_7243026
_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 Br2 Cl2 N2 Pt, 0.333(C H4 O)'
_chemical_formula_sum            'C10.33 H7.33 Br2 Cl2 N2 O0.33 Pt'
_chemical_formula_weight         590.66
_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                99.6290(10)
_cell_angle_beta                 98.1860(10)
_cell_angle_gamma                94.7940(10)
_cell_formula_units_Z            6
_cell_length_a                   7.45320(10)
_cell_length_b                   12.7323(2)
_cell_length_c                   22.1827(3)
_cell_measurement_reflns_used    10666
_cell_measurement_temperature    150
_cell_measurement_theta_max      76.5520
_cell_measurement_theta_min      3.5570
_cell_volume                     2041.78(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.951
_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    -90.00 -64.00   0.50    1.29    --  -46.37-151.00-106.00   52
  2  \w   -120.00 -94.00   0.50    5.22    --  -84.50-151.00-106.00   52
  3  \w   -134.00-107.00   0.50    5.22    --  -84.50-121.00  54.00   54
  4  \w    -76.00 -46.00   0.50    5.22    --  -84.50  19.00   0.00   60
  5  \w    -59.00 -10.00   0.50    5.22    --  -84.50  37.00   0.00   98
  6  \w    -88.00  -8.00   0.50    1.29    --  -46.37 121.00 136.00  160
  7  \w    -80.00 -55.00   0.50    1.29    --  -46.37 151.00 -62.00   50
  8  \w   -103.00 -78.00   0.50    5.22    --  -84.50 151.00 -62.00   50
  9  \w   -107.00 -82.00   0.50    5.22    --  -84.50 121.00 136.00   50
 10  \w    -29.00  62.00   0.50    1.29    --   46.37 -19.00 -30.00  182
 11  \w     89.00 116.00   0.50    1.29    --   46.37  77.00-150.00   54
 12  \w     58.00  89.00   0.50    1.29    --   46.37 151.00 -62.00   62
 13  \w     87.00 113.00   0.50    5.22    --  108.56 151.00 -62.00   52
 14  \w    143.00 176.00   0.50    5.22    --  108.56 125.00 -90.00   66
 15  \w     96.00 166.00   0.50    5.22    --  108.56  37.00  60.00  140
 16  \w    125.00 150.00   0.50    5.22    --  108.56 121.00 136.00   50
 17  \w     38.00  68.00   0.50    5.22    --  108.56 -37.00  90.00   60
 18  \w     38.00  68.00   0.50    5.22    --  108.56 -19.00  60.00   60
 19  \w     41.00  66.00   0.50    5.22    --  108.56 -57.00   0.00   50
 20  \w     83.00 118.00   0.50    5.22    --  108.56 -57.00   0.00   70
 21  \w     77.00 103.00   0.50    5.22    --  108.56 -99.00 -60.00   52
 22  \w     80.00 125.00   0.50    5.22    --  108.56-151.00-106.00   90
 23  \w     57.00 100.00   0.50    1.29    --   46.37-151.00-106.00   86
 24  \w     82.00 125.00   0.50    5.22    --  108.56 -57.00-150.00   86
 25  \w     43.00  90.00   0.50    5.22    --  108.56 -99.00 -90.00   94
 26  \w     35.00  68.00   0.50    5.22    --  108.56 -37.00 -60.00   66
 27  \w     38.00  66.00   0.50    5.22    --  108.56 -37.00   0.00   56
 28  \w     35.00  64.00   0.50    5.22    --  108.56 -37.00  60.00   58
 29  \w     44.00 122.00   0.50    5.22    --  108.56 -77.00   0.00  156
 30  \w     65.00 109.00   0.50    5.22    --  108.56-121.00  54.00   88
 31  \w     67.00  98.00   0.50    5.22    --  108.56 -99.00 120.00   62
 32  \w     38.00  76.00   0.50    5.22    --  108.56 -19.00  90.00   76
 33  \w     35.00  69.00   0.50    5.22    --  108.56 -37.00 150.00   68
 34  \w     39.00  70.00   0.50    5.22    --  108.56 -19.00 150.00   62
 35  \w     41.00  66.00   0.50    5.22    --  108.56 -37.00  30.00   50
 36  \w     36.00  61.00   0.50    5.22    --  108.56 -19.00   0.00   50
 37  \w     44.00  70.00   0.50    5.22    --  108.56 -19.00 -60.00   52
 38  \w     37.00  67.00   0.50    5.22    --  108.56 -57.00-150.00   60
 39  \w     46.00 107.00   0.50    5.22    --  108.56 -99.00-150.00  122
 40  \w     49.00  74.00   0.50    5.22    --  108.56 -19.00-150.00   50
 41  \w     39.00  68.00   0.50    5.22    --  108.56 -37.00-150.00   58
 42  \w     24.00  51.00   0.50    1.29    --   46.37  77.00-150.00   54
 43  \w     75.00 102.00   0.50    5.22    --  108.56 125.00 -90.00   54
 44  \w    -29.00  61.00   0.50    1.29    --   46.37 -19.00-120.00  180
 45  \w     36.00 112.00   0.50    5.22    --  108.56-125.00   0.00  152
 46  \w     27.00  54.00   0.50    1.29    --   46.37-121.00  54.00   54
;
_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      -0.0361791000
_diffrn_orient_matrix_UB_12      -0.1180978000
_diffrn_orient_matrix_UB_13      0.0066553000
_diffrn_orient_matrix_UB_21      -0.0149523000
_diffrn_orient_matrix_UB_22      -0.0347976000
_diffrn_orient_matrix_UB_23      -0.0706311000
_diffrn_orient_matrix_UB_31      0.2064217000
_diffrn_orient_matrix_UB_32      -0.0093887000
_diffrn_orient_matrix_UB_33      0.0076086000
_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  0.0460
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24010
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.849
_diffrn_reflns_theta_min         2.046
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    29.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69064
_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 yellow'
_exptl_crystal_density_diffrn    2.882
_exptl_crystal_description       needle
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.458
_refine_diff_density_min         -1.927
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0482P)^2^+15.1791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7265
_reflns_number_total             8301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00459j3.cif
_cod_data_source_block           2-MeOH
_cod_depositor_comments
'Adding full bibliography for 7243022--7243026.cif.'
_cod_database_code               7243026
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C10H6N2Br2Cl2Pt
_reflns_odcompleteness_completeness 99.93
_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:
 C1B(H1B), C1C(H1C), C7C(H7C), C4B(H4B), C1A(H1A), C4C(H4C), C10A(H10A),
 C9C(H9C), C7A(H7A), C2A(H2A), C10C(H10C), C2B(H2B), C9A(H9A), C10B(H10B),
 C7B(H7B), C2C(H2C), C4A(H4A), C9B(H9B)
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              91481
_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 1.981
_oxdiff_exptl_absorpt_empirical_full_min 0.529