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_4327967
_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            'C80 H78 Co2 N2 O2 P6'
_chemical_formula_weight         1403.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.4370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1309(8)
_cell_length_b                   21.1279(10)
_cell_length_c                   19.9712(9)
_cell_measurement_reflns_used    850
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     6786.0(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.1296
_diffrn_reflns_av_sigmaI/netI    0.1102
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57210
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.9475
_exptl_absorpt_correction_T_min  0.8218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       plate
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         13284
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1202
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0366P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1075
_reflns_number_gt                8065
_reflns_number_total             13284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201617p_si_002_2.cif
_cod_data_source_block           copn7m
_cod_database_code               4327967