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_7715704
_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         'C19 H12 F N3 O2 Pt'
_chemical_formula_sum            'C19 H12 F N3 O2 Pt'
_chemical_formula_weight         528.41
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-20
_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                120
_cell_formula_units_Z            18
_cell_length_a                   30.5683(10)
_cell_length_b                   30.5683(10)
_cell_length_c                   9.9905(4)
_cell_measurement_reflns_used    9770
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.2780
_cell_measurement_theta_min      2.2700
_cell_volume                     8084.6(5)
_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 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                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.837
_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     44.00  81.00   0.50  100.13    --   -8.80  37.00  60.00   74
  2  \w    -93.00 -56.00   0.50  100.13    --   -8.80  28.00-180.00   74
  3  \w    -39.00  80.00   0.50  100.13    --   -8.80  28.00-180.00  238
  4  \w    -57.00   2.00   0.50  100.13    --   -8.80  37.00  60.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0241896000
_diffrn_orient_matrix_UB_12      0.0132603000
_diffrn_orient_matrix_UB_13      -0.0306822000
_diffrn_orient_matrix_UB_21      0.0018817000
_diffrn_orient_matrix_UB_22      -0.0222152000
_diffrn_orient_matrix_UB_23      0.0021222000
_diffrn_orient_matrix_UB_31      -0.0113558000
_diffrn_orient_matrix_UB_32      -0.0070296000
_diffrn_orient_matrix_UB_33      -0.0639315000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20529
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.477
_diffrn_reflns_theta_min         2.179
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    7.837
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50268
_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_colour_primary    red
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_description       needle
_exptl_crystal_F_000             4500
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.017
_exptl_crystal_size_min          0.013
_refine_diff_density_max         3.112
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0384P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3702
_reflns_number_total             4582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00713a2.cif
_cod_data_source_block           Pt-Fpy
_cod_depositor_comments
'Adding full bibliography for 7715702--7715704.cif.'
_cod_original_cell_volume        8084.6(6)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7715704
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         PtC19N3O2FH12
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C12(H12), C16(H16), C17(H17), C14(H14), C9(H9), C2(H2A), C3(H3),
 C5(H5), C11(H11), C4(H4), C10(H10)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              66025
_shelx_fab_checksum              10534
_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 1.797
_oxdiff_exptl_absorpt_empirical_full_min 0.717