A New Class of Rhodium(I) κ1-Pand κ2-P,NComplexes with Rigid PTN(R) Ligands (PTN = 7-Phospha-3-methyl-1,3,5-triazabicyclo[3.3.1]nonane)
Phillips, Andrew D.; Bolaño, Sandra; Bosquain, Sylvain S.; Daran, Jean-Claude; Malacea, Raluca; Peruzzini, Maurizio; Poli, Rinaldo; Gonsalvi, Luca; Organometallics 25 (2006) 2189–; doi:10.1021/om051099r

data_4075027
_publ_section_title
;
 A New Class of Rhodium(I) \k1-Pand \k2-P,NComplexes with Rigid PTN(R)
 Ligands (PTN = 7-Phospha-3-methyl-1,3,5-triazabicyclo[3.3.1]nonane)
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2189
_journal_paper_doi               10.1021/om051099r
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C8 H16 I N3 O P Rh'
_chemical_formula_sum            'C8 H16 I N3 O P Rh'
_chemical_formula_weight         431.02
_chemical_name_common            RhIPTN(Me)CO
_chemical_name_systematic
;
 ?
;
_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'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.5944(12)
_cell_length_b                   12.1571(9)
_cell_length_c                   17.0443(14)
_cell_measurement_reflns_used    2500
_cell_measurement_temperature    73(2)
_cell_measurement_theta_max      31.4590
_cell_measurement_theta_min      3.9249
_cell_volume                     2609.7(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.pre23_10 beta (release 21.06.2004 CrysAlis171 .NET)
(compiled Jun 21 2004,12:00:08)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.pre23_10 beta (release 21.06.2004 CrysAlis171 .NET)
(compiled Jun 21 2004,12:00:08)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.pre23_10 beta (release 21.06.2004 CrysAlis171 .NET)
(compiled Jun 21 2004,12:00:08)
;
_computing_molecular_graphics    'ORTEPIII for Windows (Farrugia, 1997)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      73(2)
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega -103.53   47.47   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -28.0000    0.0000   90.0000    0.0000    0.0000 151

;
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      0.0406803436
_diffrn_orient_matrix_UB_12      -0.0092238758
_diffrn_orient_matrix_UB_13      -0.0290630593
_diffrn_orient_matrix_UB_21      -0.0100977963
_diffrn_orient_matrix_UB_22      0.0510245482
_diffrn_orient_matrix_UB_23      -0.0161050719
_diffrn_orient_matrix_UB_31      0.0405863142
_diffrn_orient_matrix_UB_32      0.0219822656
_diffrn_orient_matrix_UB_33      0.0250556123
_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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6852
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.778
_exptl_absorpt_correction_T_max  0.9455
_exptl_absorpt_correction_T_min  0.8636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0435P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                2446
_reflns_number_total             2952
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            om051099rsi20051229_074424.cif
_cod_data_source_block           adp147
_cod_database_code               4075027