A Convenient Method for the Synthesis of Protic 2-(Tertiary phosphino)-1-amines and Their Cp*RuCl Complexes
Ito, Masato; Osaku, Akihide; Kobayashi, Chika; Shiibashi, Akira; Ikariya, Takao; Organometallics 28 (2009) 390–393; doi:10.1021/om801042b

data_4063501
_publ_section_title
;
 A Convenient Method for the Synthesis of Protic 2-(Tertiary
 phosphino)-1-amines and Their Cp*RuCl Complexes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              390
_journal_page_last               393
_journal_paper_doi               10.1021/om801042b
_journal_volume                  28
_journal_year                    2009
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C28 H37 Cl N P Ru '
_chemical_formula_sum            'C28 H37 Cl N P Ru'
_chemical_formula_weight         555.10
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 110.884(12)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   9.804(9)
_cell_length_b                   12.792(11)
_cell_length_c                   11.427(11)
_cell_measurement_reflns_used    4681
_cell_measurement_temperature    193.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.4
_cell_volume                     1339(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10680
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.23
_refine_diff_density_min         -2.17
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2701 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_coef       71(15)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     328
_refine_ls_number_reflns         10680
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0005Fo^2^ + 0.9000\s(Fo^2^) + 0.3300]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                7774
_reflns_number_total             10680
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om801042b_si_004.cif
_cod_data_source_block           '__CpRuClPN2'
_cod_original_formula_sum        'C28 H37 Cl N P Ru '
_cod_database_code               4063501