Controlled crystallisation of porous crystals of luminescent platinum(II) complexes by electronic tuning of ancillary ligands.
Mochizuki, Takanari; Yoshida, Masaki; Kobayashi, Atsushi; Kato, Masako; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12064–12072; doi:10.1039/d4dt00713a

data_7715703
_publ_section_title
;
 Controlled crystallisation of porous crystals of luminescent platinum(II)
 complexes by electronic tuning of ancillary ligands.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12064
_journal_page_last               12072
_journal_paper_doi               10.1039/d4dt00713a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C17 H11 N3 O3 Pt'
_chemical_formula_sum            'C17 H11 N3 O3 Pt'
_chemical_formula_weight         500.38
_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             2023-07-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-02-20 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7698(5)
_cell_length_b                   15.2043(3)
_cell_length_c                   5.06530(10)
_cell_measurement_reflns_used    3070
_cell_measurement_temperature    150
_cell_measurement_theta_max      76.0850
_cell_measurement_theta_min      3.6990
_cell_volume                     1445.54(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_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    -55.00  23.00   0.50    0.83    --  -46.37  20.00 176.00  156
  2  \w    -85.00 -41.00   0.50    0.96    --  -84.50 107.00 -11.00   88
  3  \w     33.00  73.00   0.50    0.96    --  108.56 -20.00   9.00   80
  4  \w     77.00 103.00   0.50    0.96    --  108.56-120.00 165.00   52
  5  \w     38.00  74.00   0.50    0.96    --  108.56-120.00 165.00   72
  6  \w    -27.00  46.00   0.50    0.83    --   46.37 -37.00 -30.00  146
  7  \w   -118.00 -92.00   0.50    0.96    --  -84.50 -20.00   9.00   52
  8  \w     35.00  65.00   0.50    0.96    --  108.56 -37.00  60.00   60
  9  \w     40.00  66.00   0.50    0.96    --  108.56 -37.00-180.00   52
 10  \w     42.00 110.00   0.50    0.96    --  108.56-125.00   0.00  136
 11  \w     34.00  71.00   0.50    0.96    --  108.56 -19.00 -30.00   74
 12  \w     35.00  61.00   0.50    0.96    --  108.56 -37.00-150.00   52
;
_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      0.0724249000
_diffrn_orient_matrix_UB_12      0.0476377000
_diffrn_orient_matrix_UB_13      -0.0043844000
_diffrn_orient_matrix_UB_21      0.0375713000
_diffrn_orient_matrix_UB_22      -0.0859606000
_diffrn_orient_matrix_UB_23      0.0807864000
_diffrn_orient_matrix_UB_31      0.0092328000
_diffrn_orient_matrix_UB_32      -0.0244356000
_diffrn_orient_matrix_UB_33      -0.2932196000
_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  0.0327
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       2
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5136
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.400
_diffrn_reflns_theta_min         3.741
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.364
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.299
_exptl_crystal_description       needle
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.043
_refine_diff_density_max         3.167
_refine_diff_density_min         -2.374
_refine_diff_density_rms         0.273
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.35(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0500
_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^)+(0.1113P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1485
_reflns_Friedel_coverage         0.554
_reflns_Friedel_fraction_full    0.876
_reflns_Friedel_fraction_max     0.765
_reflns_number_gt                2440
_reflns_number_total             2700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00713a2.cif
_cod_data_source_block           Pt-ox
_cod_depositor_comments
'Adding full bibliography for 7715702--7715704.cif.'
_cod_database_code               7715703
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pt C O N H'
_chemical_oxdiff_usercomment     '150 K'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.65(4)
 0.35(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C11(H11), C5(H5), N2(H2), C12(H12), C2(H2A), C9(H9), C15(H15),
 C4(H4), C3(H3), C10(H10)
;
_shelx_res_checksum              70364
_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 2.595
_oxdiff_exptl_absorpt_empirical_full_min 0.608