Synthesis, Structures, and Catalytic Properties of Late-Transition-Metal 2,6-Bis(2-phosphaethenyl)pyridine Complexes
Hayashi, Akito; Okazaki, Masaaki; Ozawa, Fumiyuki; Tanaka, Rika; Organometallics 26 (2007) 5246–; doi:10.1021/om700488y

data_4073594
_publ_section_title
;
 Synthesis, Structures, and Catalytic Properties of Late-Transition-Metal
 2,6-Bis(2-phosphaethenyl)pyridine Complexes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5246
_journal_paper_doi               10.1021/om700488y
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C44 H65 Ag F3 N O4 P2 S'
_chemical_formula_sum            'C44 H65 Ag F3 N O4 P2 S'
_chemical_formula_weight         930.87
_chemical_melting_point          492
_chemical_name_common            'complex 4'
_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'
_cell_angle_alpha                79.143(6)
_cell_angle_beta                 74.963(5)
_cell_angle_gamma                85.396(7)
_cell_formula_units_Z            2
_cell_length_a                   10.953(1)
_cell_length_b                   14.836(2)
_cell_length_c                   15.422(1)
_cell_measurement_reflns_used    9721
_cell_measurement_temperature    223.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2375.6(4)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 14.62
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23463
_diffrn_reflns_theta_max         27.48
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_recrystallization_method
'From CH2Cl2/pentane at room temperature'
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.54
_refine_ls_extinction_coef       0.0000
_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   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     688
_refine_ls_number_reflns         8845
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          -0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0510P)^2^+1.8628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                8845
_reflns_number_total             10655
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            om700488y-file005.cif
_cod_data_source_block           HAY-3-033
_cod_database_code               4073594