Asymmetric Hydrogenation. Dimerization of Solvate Complexes: Synthesis and Characterization of Dimeric [Rh(DIPAMP)]22+, a Valuable Catalyst Precursor
Preetz, Angelika; Baumann, Wolfgang; Fischer, Christian; Drexler, Hans-Joachim; Schmidt, Thomas; Thede, Richard; Heller, Detlef; Organometallics 28 (2009) 3673–; doi:10.1021/om801199q

data_4069006
_publ_section_title
;
 Asymmetric Hydrogenation. Dimerization of Solvate Complexes: Synthesis
 and Characterization of Dimeric [Rh(DIPAMP)]22+, a Valuable Catalyst
 Precursor
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3673
_journal_paper_doi               10.1021/om801199q
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C52 H48 B2 F8 P4 Rh2'
_chemical_formula_weight         1176.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.608(2)
_cell_length_b                   14.618(3)
_cell_length_c                   14.631(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     2479.8(8)
_computing_cell_refinement       STOE-CELL
_computing_data_collection       STOE-EXPOSE
_computing_data_reduction        STOE-INTEGRATE
_computing_molecular_graphics    'XP (Siemens)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'laser scanned imaging plate'
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13052
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.97
_diffrn_standards_interval_time  360
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    0.861
_exptl_absorpt_correction_type   'mean imaging plate intensity method'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         3739
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.349
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.240
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.3261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                3064
_reflns_number_total             3739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801199q_si_002.cif
_cod_data_source_block           ks331a
_cod_original_cell_volume        2479.8(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4069006