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_4087057
_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         'C32 H37 Cl2 N P Rh, C H2 Cl2'
_chemical_formula_sum            'C33 H39 Cl4 N P Rh'
_chemical_formula_weight         725.33
_chemical_name_systematic
;
 ((N-methyl)phenylimidoyl)di(3-methylphenyl)phosphanyl)-
(pentamethylcyclopentadienyl) Rhodium(III) dichloride
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
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_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.980(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   23.6047(3)
_cell_length_c                   16.0910(2)
_cell_measurement_reflns_used    11582
_cell_measurement_temperature    120(2)
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_cell_measurement_theta_min      4.6
_cell_volume                     3278.83(7)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Agilent, SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'rotation in \w, 1\%'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.836
_diffrn_reflns_theta_min         3.404
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.845
_exptl_absorpt_correction_T_max  0.895
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       rods
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.477
_refine_diff_density_min         -1.838
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0379P)^2^+4.7820P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6296
_reflns_number_total             6858
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00057_si_002.cif
_cod_data_source_block           jcs018_2_compound_4e
_cod_depositor_comments
'Adding full bibliography for 4087056--4087059.cif.'
_cod_database_code               4087057
_shelx_estimated_absorpt_t_min   0.290
_shelx_estimated_absorpt_t_max   0.891
_shelxl_version_number           2013-2
_shelx_res_checksum              40327
_shelx_hkl_checksum              5975