Synthesis, Structures, and Reactivity of Ruthenium Complexes with PNP-pincer Type Phosphaalkene Ligands
Nakajima, Yumiko; Okamoto, Yuki; Chang, Yung-Hung; Ozawa, Fumiyuki; Organometallics 32 (2013) 2918–; doi:10.1021/om400126v

data_4080718
_publ_section_title
;
 Synthesis, Structures, and Reactivity of Ruthenium Complexes with
 PNP-pincer Type Phosphaalkene Ligands
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2918
_journal_paper_doi               10.1021/om400126v
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C57 H71 N O2 P2 Ru'
_chemical_formula_weight         965.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.543(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6958(9)
_cell_length_b                   9.8210(7)
_cell_length_c                   18.2435(14)
_cell_measurement_temperature    103(2)
_cell_volume                     2570.2(3)
_computing_cell_refinement       'Nonius CAD4 software'
_computing_data_collection       'Nonius CAD4 software'
_computing_data_reduction        'Nonius CAD4 software'
_computing_molecular_graphics    'ORTEP3 for windows'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  ' CCD area detector '
_diffrn_measurement_method       ' phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1851
_diffrn_reflns_av_sigmaI/netI    0.2269
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20008
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.9603
_exptl_absorpt_correction_T_min  0.9228
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         8752
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.2128
_refine_ls_R_factor_gt           0.1126
_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^)+(0.0000P)^2^+16.9218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.2276
_reflns_number_gt                4832
_reflns_number_total             8752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400126v_si_002.cif
_cod_data_source_block           complex1
_cod_original_sg_symbol_H-M      P21
_cod_database_code               4080718