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_4118847
_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 F6 N4 O2 P Pt, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C23.5 H24 Cl F6 N4 O2 P Pt'
_chemical_formula_weight         769.98
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_audit_author_name               'Tanaka, R.'
_audit_creation_date             2011-07-25
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.7963(16)
_cell_length_b                   8.4080(5)
_cell_length_c                   21.7444(11)
_cell_measurement_reflns_used    16676
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.1001
_cell_volume                     5447.6(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      150(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;

scan:

    Number of images: 1800

               Slice: -80.0000 - 100.0000

         Image width: 0.1000

            Exp time: 15.0000

       Rotation axis: Phi

               Omega: 0.0000

                 Chi: 0.0000

                 Phi: 0.0000

                 XTD: 55.2589

              2theta: 24.8080

scan:

    Number of images: 600

               Slice: -15.0000 - 45.0000

         Image width: 0.1000

            Exp time: 15.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 90.0000

                 Phi: 0.0000

                 XTD: 55.2589

              2theta: 24.8080

scan:

    Number of images: 600

               Slice: -15.0000 - 45.0000

         Image width: 0.1000

            Exp time: 15.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 90.0000

                 Phi: 90.0000

                 XTD: 55.2589

              2theta: 24.8080

scan:

    Number of images: 600

               Slice: -15.0000 - 45.0000

         Image width: 0.1000

            Exp time: 15.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 90.0000

                 Phi: 180.0000

                 XTD: 55.2589

              2theta: 24.8080

scan:

    Number of images: 600

               Slice: -15.0000 - 45.0000

         Image width: 0.1000

            Exp time: 15.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 90.0000

                 Phi: 270.0000

                 XTD: 55.2589

              2theta: 24.8080

;
_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  0.0797
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40012
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         4.10
_diffrn_source_current           250.0000
_diffrn_source_power             15.0000
_diffrn_source_voltage           60.0000
_exptl_absorpt_coefficient_mu    5.379
_exptl_absorpt_correction_T_max  0.8553
_exptl_absorpt_correction_T_min  0.6153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            'Dark Orange'
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2984
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 150(2) K'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.897
_refine_diff_density_min         -1.727
_refine_diff_density_rms         0.187
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.389(13)
_refine_ls_extinction_coef       0.00037(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         11774
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0236P)^2^+71.1928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1345
_reflns_number_gt                9675
_reflns_number_total             11774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja308103g_si_001.cif
_cod_data_source_block           1+(NN+-Pt(NCN)-1)
_cod_original_formula_sum        'C23.50 H24 Cl F6 N4 O2 P Pt'
_cod_database_code               4118847