Iminophosphorane-based [P2N2] rhodium complexes: synthesis, reactivity, and application in catalysed transfer hydrogenation of polar bonds
Buchard, Antoine; Payet, Elina; Auffrant, Audrey; Goff, Xavier Le; Floch, Pascal Le; New Journal of Chemistry 34 (2010) 2943–; doi:10.1039/c0nj00299b

data_7053615
_publ_section_title
;
 Iminophosphorane-based [P2N2] rhodium complexes: synthesis, reactivity,
 and application in catalysed transfer hydrogenation of polar bonds
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2943
_journal_paper_doi               10.1039/c0nj00299b
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         'C52 H48 N2 P4 Rh, 4(C H2 Cl2), Cl'
_chemical_formula_sum            'C56 H56 Cl9 N2 P4 Rh'
_chemical_formula_weight         1302.87
_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                 91.563(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.715(1)
_cell_length_b                   21.218(1)
_cell_length_c                   23.598(1)
_cell_measurement_reflns_used    12206
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     5863.5(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13346
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.9832
_exptl_absorpt_correction_T_min  0.8352
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
An highly disordered CH2Cl2 molecule was accounted for using the
Platon SQUEEZE function.
;
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         13346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0402P)^2^+7.7966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                10863
_reflns_number_total             13346
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00299b.txt
_cod_data_source_block           ab982
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P21/c '
_cod_database_code               7053615