Synthesis, Characterization, and Reactivity toward MeI of Carbonyl Rh(I) Complexes Containing a PNO Hydrazonic Ligand
Pelagatti, Paolo; Bacchi, Alessia; Bobbio, Carla; Carcelli, Mauro; Costa, Mirco; Pelizzi, Corrado; Vivorio, Cristiano; Organometallics 19 (2000) 5440–; doi:10.1021/om000562r

data_4077596
_publ_section_title
;
 Synthesis, Characterization, and Reactivity toward MeI of Carbonyl Rh(I)
 Complexes Containing a PNO Hydrazonic Ligand
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5440
_journal_paper_doi               10.1021/om000562r
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C36 H39 I N2 O4 P Rh'
_chemical_formula_weight         824.54
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.98(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.746(4)
_cell_length_b                   9.576(4)
_cell_length_c                   37.366(9)
_cell_measurement_temperature    293(2)
_cell_volume                     3483(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Siemens AED diffractometer'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            10314
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         3.05
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.453
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.288
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         10182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1177P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1893
_reflns_number_gt                4501
_reflns_number_total             10182
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000562r.cif
_cod_data_source_block           compound_9
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4077596