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_4118850
_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, H2 O'
_chemical_formula_sum            'C23 H25 N4 O3 Pt'
_chemical_formula_weight         600.56
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_author_name               'Tanaka, R.'
_audit_creation_date             2010-02-02
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.978(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9464(14)
_cell_length_b                   15.361(2)
_cell_length_c                   14.300(2)
_cell_measurement_reflns_used    8790
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.1334
_cell_volume                     2163.7(5)
_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    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
scan:
    Number of images: 600
               Slice: -80.0000 - 100.000
         Image width: 0.3000
            Exp time: 15.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 35.1657
              2theta: 9.8218
scan:
    Number of images: 167
               Slice: -30.0000 - 20.1000
         Image width: 0.3000
            Exp time: 15.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 35.1657
              2theta: 9.8218
scan:
    Number of images: 167
               Slice: -30.0000 - 20.1000
         Image width: 0.3000
            Exp time: 15.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 35.1657
              2theta: 9.8218
scan:
    Number of images: 167
               Slice: -30.0000 - 20.1000
         Image width: 0.3000
            Exp time: 15.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 35.1657
              2theta: 9.8218

;
_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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21274
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.14
_diffrn_source_current           250.0000
_diffrn_source_power             15.0000
_diffrn_source_voltage           60.0000
_exptl_absorpt_coefficient_mu    6.518
_exptl_absorpt_correction_T_max  0.8807
_exptl_absorpt_correction_T_min  0.4414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1172
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 200(2) K'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.270
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4940
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.269
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0000P)^2^+5.0451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0764
_reflns_number_gt                4600
_reflns_number_total             4940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja308103g_si_004.cif
_cod_data_source_block           1(NN-Pt(NCN)-1)-H2O
_cod_database_code               4118850