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_4073592
_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         'C51 H83 Cl N O2 P2 Rh'
_chemical_formula_sum            'C51 H83 Cl N O2 P2 Rh'
_chemical_formula_weight         942.53
_chemical_melting_point          468
_chemical_name_common            'complex 1a'
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.980(1)
_cell_length_b                   33.843(2)
_cell_length_c                   18.534(1)
_cell_measurement_reflns_used    20586
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     10650.6(11)
_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      296
_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       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            83158
_diffrn_reflns_theta_max         27.49
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Dark_Green
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_recrystallization_method 'From Et2O at 203 K'
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.96
_refine_diff_density_min         -0.77
_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   1.032
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     523
_refine_ls_number_reflns         8039
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          -0.0050
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1831
_reflns_number_gt                8039
_reflns_number_total             12156
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            om700488y-file003.cif
_cod_data_source_block           PNP-Rh-Cl
_cod_original_cell_volume        10651(1)
_cod_database_code               4073592