Modulation of Intersystem Crossing Rate by Minor Ligand Modifications in Cyclometalated Platinum(II) Complexes.
Shafikov, Marsel Z.; Kozhevnikov, Dmitry N.; Bodensteiner, Michael; Brandl, Fabian; Czerwieniec, Rafał; Inorganic chemistry 55 (2016) 7457–7466; doi:10.1021/acs.inorgchem.6b00704

data_4347851
_publ_section_title
;
 Modulation of Intersystem Crossing Rate by Minor Ligand Modifications in
 Cyclometalated Platinum(II) Complexes.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7457
_journal_page_last               7466
_journal_paper_doi               10.1021/acs.inorgchem.6b00704
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H22 F N O2 Pt S2'
_chemical_formula_sum            'C26 H22 F N O2 Pt S2'
_chemical_formula_weight         658.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-27
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.512(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9809(4)
_cell_length_b                   11.5439(3)
_cell_length_c                   11.9873(5)
_cell_measurement_reflns_used    3355
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      70.0570
_cell_measurement_theta_min      5.2630
_cell_volume                     1156.21(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.848
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measurement_details
;
  1 omega  -29.00   23.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0561   37.0000 -120.0000 52

  2 omega   27.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0561 -125.0000 -120.0000 69

  3 omega   25.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      101.0432  -30.0000  150.0000 44

  4 omega   30.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      101.0432  -45.0000 -150.0000 47

  5 omega   73.00  151.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      101.0432  125.0000 -120.0000 78

  6 omega   71.00  148.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      101.0432   77.0000   30.0000 77

  7 omega -117.00   -8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0561  -77.0000 -180.0000 109

  8 omega -113.00  -13.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0561  -57.0000  -60.0000 100

  9 omega   25.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      101.0432  -30.0000  -30.0000 44

 10 omega   28.00   59.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      101.0432 -125.0000 -150.0000 31

 11 omega   28.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      101.0432  -45.0000  -90.0000 49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0089549000
_diffrn_orient_matrix_UB_12      -0.1283495000
_diffrn_orient_matrix_UB_13      -0.0320518000
_diffrn_orient_matrix_UB_21      -0.0733495000
_diffrn_orient_matrix_UB_22      -0.0353786000
_diffrn_orient_matrix_UB_23      0.0927805000
_diffrn_orient_matrix_UB_31      -0.1689204000
_diffrn_orient_matrix_UB_32      0.0086043000
_diffrn_orient_matrix_UB_33      -0.0972262000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.848
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4569
_diffrn_reflns_point_group_measured_fraction_full 0.729
_diffrn_reflns_point_group_measured_fraction_max 0.695
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         70.458
_diffrn_reflns_theta_min         3.964
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.314
_exptl_absorpt_correction_T_max  0.537
_exptl_absorpt_correction_T_min  0.111
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.4211
_exptl_crystal_size_mid          0.0866
_exptl_crystal_size_min          0.0705
_refine_diff_density_max         1.899
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Flack x determined using 1122 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).

 Distance and displacement parameters were used for the refinement of the 
 disordered minor position.
;
_refine_ls_abs_structure_Flack   -0.036(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         3076
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0549P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.620
_reflns_Friedel_fraction_full    0.597
_reflns_Friedel_fraction_max     0.562
_reflns_number_gt                3003
_reflns_number_total             3076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00704_si_002.cif
_cod_data_source_block           n010
_cod_original_cell_volume        1156.20(8)
_cod_database_code               4347851
_chemical_oxdiff_formula         'Pt S2 O2 N F C26 H22'
_reflns_odcompleteness_completeness 84.68
_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 C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S2B-C19B \\sim S2B-C16B \\sim S2A-C16A \\sim S2A-C19A
 with sigma of 0.01
 C16B-C17B \\sim C18B-C19B
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
S2A \\sim C20A \\sim C19A \\sim C18A \\sim C16A \\sim C21A \\sim C17A \\sim
C16B \\sim C17B \\sim C18B \\sim C19B \\sim S2B \\sim C20B \\sim C21B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: S2A(0.82364) C20A(0.82364) H20A(0.82364) H20B(0.82364)
 C19A(0.82364) C18A(0.82364) H18A(0.82364) C16A(0.82364) C21A(0.82364)
 H21A(0.82364) H21B(0.82364) H21C(0.82364) C17A(0.82364) H17A(0.82364)
 C16B(0.17636) C17B(0.17636) H17B(0.17636) C18B(0.17636) H18B(0.17636)
 C19B(0.17636) S2B(0.17636) C20B(0.17636) H20C(0.17636) H20D(0.17636)
 C21B(0.17636) H21D(0.17636) H21E(0.17636) H21F(0.17636)
5.a Secondary CH2 refined with riding coordinates:
 C20A(H20A,H20B), C20B(H20C,H20D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C14(H14), C10(H10), C6(H6), C18A(H18A), C5(H5), C9(H9), C8(H8),
 C3(H3), C24(H24), C17A(H17A), C17B(H17B), C18B(H18B)
5.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C22(H22A,H22B,H22C), C21A(H21A,H21B,H21C), C21B(H21D,
 H21E,H21F)
;
_shelx_res_checksum              89288
_shelx_hkl_checksum              28287
_shelx_shelxl_version_number     2014/7
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_diffrn_ambient_temperature_device 'CryoStream 700, Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder with inert oil'
_olex2_submission_special_instructions 'No special instructions were received'