Iminophosphanes: Synthesis, Rhodium Complexes, and Ruthenium(II)-Catalyzed Hydration of Nitriles.
Rong, Mark K.; van Duin, Koen; van Dijk, Tom; de Pater, Jeroen J. M.; Deelman, Berth-Jan; Nieger, Martin; Ehlers, A. W.; Slootweg, J. Chris; Lammertsma, Koop; Organometallics 36 (2017) 1079–1090; doi:10.1021/acs.organomet.7b00057

data_4087058
_publ_section_title
;
 Iminophosphanes: Synthesis, Rhodium Complexes, and
 Ruthenium(II)-Catalyzed Hydration of Nitriles.
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1079
_journal_page_last               1090
_journal_paper_doi               10.1021/acs.organomet.7b00057
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C30 H33 Cl N P Rh, C F3 O3 S'
_chemical_formula_sum            'C31 H33 Cl F3 N O3 P Rh S'
_chemical_formula_weight         725.97
_chemical_name_systematic
;
 Chloro (((N-methyl)phenylimidoyl)diphenylphosphanyl)(pentamethyl-
cyclopentadienyl) Rhodium(III) trifluoromethylsulfonate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4195(3)
_cell_length_b                   14.5992(3)
_cell_length_c                   15.1828(3)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.4
_cell_volume                     3196.18(11)
_computing_cell_refinement       SAINT
_computing_data_collection       APEXII
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  publCIF
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       'rotation in \f and \w, 0.5\%'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25974
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.682
_diffrn_reflns_theta_min         1.935
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       plates
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 2963 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.037(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7166
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+2.9625P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.853
_reflns_Friedel_fraction_full    0.932
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                6737
_reflns_number_total             7166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00057_si_002.cif
_cod_data_source_block           jcs019_compound_6a
_cod_depositor_comments
'Adding full bibliography for 4087056--4087059.cif.'
_cod_database_code               4087058
_shelx_estimated_absorpt_t_min   0.799
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2013-2
_shelx_res_checksum              73447
_shelx_hkl_checksum              4715