The Intramolecular Rearrangement of Phosphinohydrazides [R'2P-NR-NR-M] → [RN=PR'2-NR-M]: General Rules and Exceptions. Transformations of Bulky Phosphinohydrazines (R-NH-N(PPh2)2, R =tBu, Ph2P)
Alexander N. Kornev; Vyacheslav V. Sushev; Yulia S. Panova; Natalia V. Belina; Olga V. Lukoyanova; Georgy K. Fukin; Sergey Y. Ketkov; Gleb A. Abakumov; Peter Lönnecke; Evamarie Hey-Hawkins; Inorganic Chemistry 51 (2012) 874–881; doi:10.1021/ic201617p

data_4327966
_publ_contact_author             G.K.Fukin
_publ_contact_author_email       gera@iomc.ras.ru
_publ_section_title
;
 The Intramolecular Rearrangement of Phosphinohydrazides [R'2P-NR-NR-M]
 \\rightarrow [RN=PR'2-NR-M]: General Rules and Exceptions.
 Transformations of Bulky Phosphinohydrazines (R-NH-N(PPh2)2, R =tBu,
 Ph2P)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              874
_journal_page_last               881
_journal_paper_doi               10.1021/ic201617p
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C28 H30 N2 P2'
_chemical_formula_weight         456.48
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-10-15T17:23:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.036(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.2853(2)
_cell_length_b                   31.6711(5)
_cell_length_c                   12.8947(3)
_cell_measurement_reflns_used    39261
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.2339
_cell_measurement_theta_min      2.6158
_cell_volume                     5017.18(16)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_molecular_graphics    'ORTEP3 for Windows (L. J. Farrugia, 1997)'
_computing_publication_material  'WINGX  (L.J. Farrugia,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ccd Xcalibur S'
_diffrn_measurement_method       '\w- amd \f-scans'
_diffrn_orient_matrix_UB_11      0.0535689586
_diffrn_orient_matrix_UB_12      -0.004142728
_diffrn_orient_matrix_UB_13      0.0081809259
_diffrn_orient_matrix_UB_21      0.0016751117
_diffrn_orient_matrix_UB_22      -0.05290786
_diffrn_orient_matrix_UB_23      -0.0060362859
_diffrn_orient_matrix_UB_31      0.0215032363
_diffrn_orient_matrix_UB_32      0.0143532555
_diffrn_orient_matrix_UB_33      -0.0199390389
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            117371
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       prism
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.19
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         15318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.19
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+7.8649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1559
_reflns_number_gt                11330
_reflns_number_total             15318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201617p_si_002_1.cif
_cod_data_source_block           x0316fin
_cod_database_code               4327966