NCN Pincer-Pt Complexes Coordinated by (Nitronyl Nitroxide)-2-ide Radical Anion
Xun Zhang; Shuichi Suzuki; Masatoshi Kozaki; Keiji Okada; Journal of the American Chemical Society 134 (2012) 17866–17868; doi:10.1021/ja308103g

data_4118849
_publ_contact_author_address
;
Department of Chemistry, Graduate School of Science, Osaka City University, 
Sumiyoshi-ku, Osaka 558-8585, Japan
;
_publ_contact_author_email       okadak@sci.osaka-cu.ac.jp
_publ_contact_author_fax         +81-666902709
_publ_contact_author_name        'Okada, K.'
_publ_contact_author_phone       +81-66052568
_publ_section_title
;
 NCN Pincer-Pt Complexes Coordinated by (Nitronyl Nitroxide)-2-ide Radical
 Anion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17866
_journal_page_last               17868
_journal_paper_doi               10.1021/ja308103g
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C23 H23 N4 O2 Pt, 2(C2 H6 O)'
_chemical_formula_sum            'C27 H35 N4 O4 Pt'
_chemical_formula_weight         674.68
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_author_name               'Tanaka, R.'
_audit_creation_date             2010-11-18
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.251(17)
_cell_angle_beta                 75.385(17)
_cell_angle_gamma                66.316(13)
_cell_formula_units_Z            2
_cell_length_a                   8.8562(13)
_cell_length_b                   10.4837(19)
_cell_length_c                   16.091(3)
_cell_measurement_reflns_used    5751
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0033
_cell_volume                     1321.7(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -80.0000 - 100.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 35.1993
              2theta: 9.8495
scan:
    Number of images: 100
               Slice: -30.0000 - 20.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 35.1993
              2theta: 9.8495
scan:
    Number of images: 100
               Slice: -30.0000 - 20.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 35.1993
              2theta: 9.8495
scan:
    Number of images: 100
               Slice: -30.0000 - 20.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 35.1993
              2theta: 9.8495

;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details 'AFC7: Eulerian 3-circle'
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\w or \f'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0720
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12972
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.00
_diffrn_source_current           280.0000
_diffrn_source_power             16.8000
_diffrn_source_voltage           60.0000
_exptl_absorpt_coefficient_mu    5.348
_exptl_absorpt_correction_T_max  0.8560
_exptl_absorpt_correction_T_min  0.1287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       Needle
_exptl_crystal_F_000             670
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 120(2) K'
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.795
_refine_diff_density_min         -2.335
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5919
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+23.5520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                5316
_reflns_number_total             5919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja308103g_si_003.cif
_cod_data_source_block           1(NN-Pt(NCN)-1)-EtOH
_cod_database_code               4118849