Cyclic Trinuclear Rh2M Complexes (M = Rh, Pt, Pd, Ni) Supported bymeso-1,3-Bis[(diphenylphosphinomethyl)phenylphosphino]propane
Nakajima, Takayuki; Kurai, Sachi; Noda, Sayo; Zouda, Maki; Kure, Bunsho; Tanase, Tomoaki; Organometallics 31 (2012) 4283–; doi:10.1021/om300278k

data_4078504
_publ_section_title
;
 Cyclic Trinuclear Rh2M Complexes (M = Rh, Pt, Pd, Ni) Supported
 bymeso-1,3-Bis[(diphenylphosphinomethyl)phenylphosphino]propane
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              4283
_journal_paper_doi               10.1021/om300278k
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C62.50 H59 Br2 Cl9 F6 Hg N2 P5 Rh3'
_chemical_formula_sum            'C62.5 H59 Br2 Cl9 F6 Hg N2 P5 Rh3'
_chemical_formula_weight         2095.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.263(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.164(7)
_cell_length_b                   40.57(3)
_cell_length_c                   18.108(13)
_cell_measurement_reflns_used    14889
_cell_measurement_temperature    153
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.05
_cell_volume                     7467(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      153
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54178
_diffrn_reflns_theta_full        27.32
_diffrn_reflns_theta_max         27.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.262
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4060.00
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.068
_refine_diff_density_max         5.400
_refine_diff_density_min         -2.790
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     824
_refine_ls_number_reflns         15196
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1056P)^2^+19.5267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1919
_reflns_number_gt                11408
_reflns_number_total             15196
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om300278k_si_002.cif
_cod_data_source_block           '[Rh3(HgBr)Cl2Br(dpmppp)(XylNC)2]PF6(8b)'
_cod_original_cell_volume        7466(9)
_cod_original_formula_sum        'C62.50 H59 Br2 Cl9 F6 Hg N2 P5 Rh3'
_cod_database_code               4078504