Liquid-liquid interface-promoted formation of a porous molecular crystal based on a luminescent platinum(II) complex.
Kimura, Mari; Yoshida, Masaki; Fujii, Sho; Miura, Atsushi; Ueno, Kosei; Shigeta, Yasuhiro; Kobayashi, Atsushi; Kato, Masako; Chemical communications (Cambridge, England) 56 (2020) 12989–12992; doi:10.1039/d0cc04164e

data_7127314
_publ_section_title
;
 Liquid-liquid interface-promoted formation of a porous molecular crystal
 based on a luminescent platinum(II) complex.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12989
_journal_page_last               12992
_journal_paper_doi               10.1039/d0cc04164e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C19 H13 N3 O2 Pt'
_chemical_formula_sum            'C19 H13 N3 O2 Pt'
_chemical_formula_weight         510.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-14 deposited with the CCDC.	2020-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.4350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.00340(10)
_cell_length_b                   12.65020(10)
_cell_length_c                   23.9841(2)
_cell_measurement_reflns_used    20215
_cell_measurement_temperature    150
_cell_measurement_theta_max      77.4810
_cell_measurement_theta_min      3.9300
_cell_volume                     3302.36(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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -65.00 -38.00   0.50    0.89    --  -46.37 125.00 -78.00   54
  2  \w   -106.00 -81.00   0.50    0.89    --  -46.37-125.00-156.00   50
  3  \w    -81.00 -56.00   0.50    0.89    --  -46.37-146.00  37.00   50
  4  \w     13.00  95.00   0.50    0.89    --   46.37-125.00-156.00  164
  5  \w     56.00  88.00   0.50    0.89    --   46.37 146.00  88.00   64
  6  \w    -88.00 -63.00   0.50    0.95    --  -84.50 125.00 -78.00   50
  7  \w   -131.00-106.00   0.50    0.95    --  -84.50-146.00  37.00   50
  8  \w     52.00  77.00   0.50    0.95    --  108.56-125.00-156.00   50
  9  \w    100.00 125.00   0.50    0.95    --  108.56 125.00 -78.00   50
 10  \w     83.00 126.00   0.50    0.95    --  108.56-146.00  37.00   86
 11  \w     63.00 125.00   0.50    0.95    --  108.56 146.00  88.00  124
 12  \w   -105.00 -74.00   0.50    0.89    --  -46.37-125.00 -90.00   62
 13  \w     24.00 117.00   0.50    0.89    --   46.37  77.00 -90.00  186
 14  \w     55.00 114.00   0.50    0.89    --   46.37  57.00-180.00  118
 15  \w    -65.00 -27.00   0.50    0.95    --  -84.50  37.00 120.00   76
 16  \w     49.00 107.00   0.50    0.95    --  108.56 -99.00  60.00  116
 17  \w     35.00  69.00   0.50    0.95    --  108.56 -37.00  30.00   68
 18  \w     70.00 122.00   0.50    0.95    --  108.56 -57.00   0.00  104
 19  \w     37.00  68.00   0.50    0.95    --  108.56 -37.00  60.00   62
 20  \w     42.00 108.00   0.50    0.95    --  108.56 -99.00   0.00  132
 21  \w     41.00  66.00   0.50    0.95    --  108.56 -37.00   0.00   50
 22  \w     37.00  62.00   0.50    0.95    --  108.56 -37.00-180.00   50
 23  \w     71.00 178.00   0.50    0.95    --  108.56 125.00 -60.00  214
 24  \w     37.00  63.00   0.50    0.95    --  108.56 -37.00-150.00   52
 25  \w     36.00  61.00   0.50    0.95    --  108.56 -19.00-180.00   50
 26  \w     47.00  72.00   0.50    0.95    --  108.56 -99.00-180.00   50
 27  \w     34.00  74.00   0.50    0.95    --  108.56 -19.00-150.00   80
 28  \w     76.00 107.00   0.50    0.95    --  108.56 -99.00-180.00   62
 29  \w     42.00  74.00   0.50    0.95    --  108.56 -19.00 -60.00   64
;
_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      0.0816344000
_diffrn_orient_matrix_UB_12      0.0560809000
_diffrn_orient_matrix_UB_13      -0.0378655000
_diffrn_orient_matrix_UB_21      -0.0514945000
_diffrn_orient_matrix_UB_22      0.1076578000
_diffrn_orient_matrix_UB_23      0.0152896000
_diffrn_orient_matrix_UB_31      0.1035926000
_diffrn_orient_matrix_UB_32      0.0094355000
_diffrn_orient_matrix_UB_33      0.0504796000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24028
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.726
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.048
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45272
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.205
_refine_diff_density_min         -2.098
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0375P)^2^+7.4059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5662
_reflns_number_total             5890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04164e2.cif
_cod_data_source_block           1N
_cod_depositor_comments
'Adding full bibliography for 7127314--7127318.cif.'
_cod_database_code               7127314
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C19H13N3O2Pt
_chemical_oxdiff_usercomment     150K
_shelx_estimated_absorpt_t_max   0.501
_shelx_estimated_absorpt_t_min   0.297
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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), N5(H5), C2(H2A), C28(H28), C3(H3), C31(H31), C14(H14), C15(H15),
 C9(H9), C33(H33), C24(H24), C17(H17), C10(H10), C4(H4), C22(H22), C34(H34),
 C5(H5A), C12(H12), C21(H21), C30(H30), C16(H16), C36(H36), C11(H11), C29(H29),
 C35(H35), C23(H23)
;
_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 1.878
_oxdiff_exptl_absorpt_empirical_full_min 0.716