Neutral and Cationic NCN Pincer Platinum(II) Complexes with 1,3-Bis(benzimidazol-2′-yl)benzene Ligands: Synthesis, Structures, and Their Photophysical Properties
Wang, Zhao; Sun, Zheming; Hao, Xin-Qi; Niu, Jun-Long; Wei, Donghui; Tu, Tao; Gong, Jun-Fang; Song, Mao-Ping; Organometallics 33 (2014) 1563–; doi:10.1021/om400946n

data_4082860
_publ_section_title
;
 Neutral and Cationic NCN Pincer Platinum(II) Complexes with
 1,3-Bis(benzimidazol-2&#x2032;-yl)benzene Ligands: Synthesis, Structures,
 and Their Photophysical Properties
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1563
_journal_paper_doi               10.1021/om400946n
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety
'0.5(C39 H47 N6 O Pt), 0.5(C39 H41 N6 O Pt), C F3 O3 S'
_chemical_formula_sum            'C40 H47 F3 N6 O4 Pt S'
_chemical_formula_weight         959.99
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-28
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.9563(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.9700(3)
_cell_length_b                   27.9808(6)
_cell_length_c                   19.4140(3)
_cell_measurement_reflns_used    11673
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      65.8510
_cell_measurement_theta_min      3.1790
_cell_volume                     8642.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9997
_diffrn_measurement_details
;
  1 omega  -47.00  -21.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 26

  2 omega  -19.00    8.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 27

  3 omega   42.00   68.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000  -60.0000 26

  4 omega  -38.00   23.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000  -60.0000 61

  5 omega  -10.00   17.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -150.0000 27

  6 omega -115.00   30.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000    0.0000  120.0000 145

  7 omega  -47.00   23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   37.0000 -180.0000 70

  8 omega -118.00  -92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000    0.0000 26

  9 omega  -60.00    7.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   57.0000   30.0000 67

 10 omega -103.00  -51.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000  -90.0000 52

 11 omega  -70.00  -40.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000    0.0000 30

 12 omega  -14.00   26.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   61.0000  -60.0000 40

 13 omega  -13.00   57.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -77.0000  -90.0000 70

 14 omega   25.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000  120.0000 88

 15 omega   16.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000  150.0000 59

 16 omega  134.00  161.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000   60.0000 27

 17 omega   45.00  103.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -30.0000 58

 18 omega   41.00   93.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   60.0000 52

 19 omega   73.00  104.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   90.0000 31

 20 omega   66.00  116.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -150.0000 50

 21 omega   46.00  146.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -15.0000   90.0000 100

 22 omega   91.00  176.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  120.0000 85

 23 omega   94.00  173.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -60.0000 79

 24 omega  125.00  151.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000   60.0000 26

 25 omega   41.00   90.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -180.0000 49

 26 omega   43.00   77.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -30.0000 34

 27 omega   45.00  134.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000 -180.0000 89

 28 omega   43.00   88.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  120.0000 45

 29 omega   43.00   70.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000    0.0000 27

 30 omega   42.00   92.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -90.0000 50

 31 omega   44.00   76.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 32

 32 omega  125.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  -90.0000 53

 33 omega   51.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   30.0000 47

 34 omega  101.00  127.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -140.0000   81.0000 26

 35 omega   61.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -140.0000   81.0000 30

 36 omega  -70.00   26.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000   30.0000 96

 37 omega  -77.00  -52.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000 -150.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0893900000
_diffrn_orient_matrix_UB_12      -0.0201143000
_diffrn_orient_matrix_UB_13      -0.0033073000
_diffrn_orient_matrix_UB_21      0.0345093000
_diffrn_orient_matrix_UB_22      0.0512065000
_diffrn_orient_matrix_UB_23      -0.0048019000
_diffrn_orient_matrix_UB_31      0.0141951000
_diffrn_orient_matrix_UB_32      0.0022723000
_diffrn_orient_matrix_UB_33      0.0794457000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15415
_diffrn_reflns_theta_full        67.06
_diffrn_reflns_theta_max         67.06
_diffrn_reflns_theta_min         3.16
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.011
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.184
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         15415
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                10683
_reflns_number_total             15415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400946n_si_002.cif
_cod_data_source_block           complex-12
_cod_depositor_comments          'Adding full bibliography for 4082860.cif.'
_cod_database_code               4082860
_chemical_oxdiff_formula         C20H20N4OPt1
_reflns_odcompleteness_completeness 99.97
_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
 C9'-C10'
 1.52 with sigma of 0.02
 C10'-C11'
 1.52 with sigma of 0.02
 O1'-C9'
 1.52 with sigma of 0.02
 C9'-C10'
 1.52 with sigma of 0.02
 C10'-C11'
 1.52 with sigma of 0.02
 S1'-C40'
 1.75 with sigma of 0.02
 C40'-F1'
 1.3 with sigma of 0.02
 C40'-F2'A
 1.3 with sigma of 0.02
 C40'-F2'
 1.3 with sigma of 0.02
 C40'-F1'A
 1.3 with sigma of 0.02
 C40'-F3'
 1.3 with sigma of 0.02
 C40'-F3'A
 1.3 with sigma of 0.02
 C12-C11
 1.5 with sigma of 0.02
 C31'-C32'
 1.5 with sigma of 0.02
 C12'-C11'
 1.5 with sigma of 0.02
 C11'-C9'
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22') \\sim Ueq, Uanis(C21') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31') \\sim Ueq, Uanis(C32') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32') \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uiso(F2') = Uiso(F2'A)
Uiso(F1') = Uiso(F1'A)
Uiso(F3') = Uiso(F3'A)
Uiso(C12') = Uiso(C11')
4. Others
 Sof(F1'A)=Sof(F2'A)=Sof(F3'A)=1-FVAR(1)
 Sof(F1')=Sof(F2')=Sof(F3')=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C9'(H9'A,H9'B), C10(H10A,H10B), C10'(H10C,H10D), C11(H11A,H11B),
 C11'(H11C,H11D), C19(H19A,H19B), C19'(H19C,H19D), C20(H20A,H20B), C20'(H20C,
 H20D), C21(H21A,H21B), C21'(H21C,H21D), C29(H29A,H29B), C29'(H29C,H29D),
 C30(H30A,H30B), C30'(H30C,H30D), C31(H31A,H31B), C31'(H31C,H31D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C3'(H3'), C5(H5), C5'(H5'), C15(H15), C15'(H15'), C16(H16),
 C16'(H16'), C17(H17), C17'(H17'), C18(H18), C18'(H18'), C25(H25), C25'(H25'),
 C26(H26), C26'(H26'), C27(H27), C27'(H27'), C28(H28), C28'(H28'), C33(H33),
 C33'(H33'), C34(H34), C34'(H34'), C36(H36), C36'(H36'), C37(H37), C37'(H37')
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C22'(H22D,H22E,H22F), C32(H32A,H32B,
 H32C), C38(H38A,H38B,H38C), C38'(H38D,H38E,H38F), C39(H39A,H39B,H39C),
 C39'(H39D,H39E,H39F)
;