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_7053618
_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 Cl2 N2 P4 Rh, Cl, 3(C2 H3 N)'
_chemical_formula_sum            'C58 H57 Cl6 N2 P4 Rh'
_chemical_formula_weight         1221.55
_chemical_name_systematic
;
?
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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            4
_cell_length_a                   19.416(1)
_cell_length_b                   24.922(1)
_cell_length_c                   10.803(1)
_cell_measurement_reflns_used    7935
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      0.998
_cell_volume                     5227.4(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1246
_diffrn_reflns_av_sigmaI/netI    0.1842
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8882
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.9687
_exptl_absorpt_correction_T_min  0.7841
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
Three highly disordered CH3CN molecule were accounted
by using Squeeze Platon's function.
;
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.10(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         8882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0595P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                5203
_reflns_number_total             8882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00299b.txt
_cod_data_source_block           ab1009
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'Orthorombic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P21212 '
_cod_database_code               7053618