Synthesis of a Rhodium Carbonyl Phosphaalkenyl‒Phosphido Complex: A Phosphorus Congener of Schiff Base Type N,N′-Chelating Monoanionic Ligands
Matsumoto, Teruyuki; Sasamori, Takahiro; Miyake, Hideaki; Tokitoh, Norihiro; Organometallics 33 (2014) 1341–; doi:10.1021/om500065n

data_4082756
_publ_section_title
;
 Synthesis of a Rhodium Carbonyl Phosphaalkenyl--Phosphido Complex: A
 Phosphorus Congener of Schiff Base Type N,N&#x2032;-Chelating Monoanionic
 Ligands
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1341
_journal_paper_doi               10.1021/om500065n
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C45 H63 O2 P2 Rh, 0.5(C6 H6), 0.5(C6 H14),'
_chemical_formula_sum            'C51 H73 O2 P2 Rh'
_chemical_formula_weight         882.94
_chemical_name_systematic
; 
 ? 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.9108(12)
_cell_angle_beta                 93.5674(12)
_cell_angle_gamma                106.4291(16)
_cell_formula_units_Z            2
_cell_length_a                   9.6326(2)
_cell_length_b                   15.2660(4)
_cell_length_c                   18.9224(6)
_cell_measurement_temperature    103(2)
_cell_volume                     2431.76(12)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics
'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_publication_material
'Yadokari-XG 2011 (Wakita,Nemoto et al., 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Rigaku_Mercury_CCD
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0707
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21712
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.9865
_exptl_absorpt_correction_T_min  0.9561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 MULABS - Empirical Correction for Absorption Anisotropy.
 Blessing, R. H., Acta Cryst., A51, 33-38 (1995).
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         8996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                6602
_reflns_number_total             8996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500065n_si_003.cif
_cod_data_source_block           compound6
_cod_original_cell_volume        2431.76(11)
_cod_original_sg_symbol_Hall     ' -P 1 '
_cod_database_code               4082756