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_4073593
_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         'C45 H66 Cu F6 N2 P3'
_chemical_formula_sum            'C45 H66 Cu F6 N2 P3'
_chemical_formula_weight         905.49
_chemical_melting_point          190
_chemical_name_common            'complex 3'
_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                95.400(5)
_cell_angle_beta                 95.810(4)
_cell_angle_gamma                110.560(5)
_cell_formula_units_Z            2
_cell_length_a                   11.730(3)
_cell_length_b                   13.310(3)
_cell_length_c                   18.690(5)
_cell_measurement_reflns_used    9521
_cell_measurement_temperature    223.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2691.6(12)
_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       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26429
_diffrn_reflns_theta_max         27.49
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_recrystallization_method 'From CH2Cl2/Et2O at room temperature'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.20
_refine_diff_density_min         -0.44
_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   1.742
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     541
_refine_ls_number_reflns         9166
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          -0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0000P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                9166
_reflns_number_total             12076
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            om700488y-file004.cif
_cod_data_source_block           HAY-3-020
_cod_original_cell_volume        2691(1)
_cod_database_code               4073593