The First Structurally Characterized Metal (κ^2^N,P)-Phosphinohydrazides: The Key to Understanding the Intramolecular Rearrangement R~2~P‒NR'‒NR'‒M → R'N=PR~2~‒NR'‒M. Metalloderivatives of Diisopropylphosphinohydrazines: Synthesis and Properties
Kornev, Alexander N.; Belina, Natalia V.; Sushev, Vyacheslav V.; Fukin, Georgy K.; Baranov, Evgenii V.; Kurskiy, Yuriy A.; Poddelskii, Andrei I.; Abakumov, Gleb A.; Lönnecke, Peter; Hey-Hawkins, Evamarie; Inorganic chemistry 48 (2009) 5574–5583; doi:10.1021/ic900135b

data_4338597
_publ_section_title
;
 The First Structurally Characterized Metal (\k^2^N,P)-Phosphinohydrazides:
 The Key to Understanding the Intramolecular Rearrangement
 R~2~P--NR'--NR'--M \\rightarrow  R'N=PR~2~--NR'--M.
 Metalloderivatives of Diisopropylphosphinohydrazines:
 Synthesis and Properties
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5574
_journal_page_last               5583
_journal_paper_doi               10.1021/ic900135b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C13 H32 Cl2 Co N2 P2'
_chemical_formula_weight         408.18
_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   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
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_audit_creation_date             2007-11-13T18:29:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.8870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.32830(10)
_cell_length_b                   16.0842(2)
_cell_length_c                   14.3787(2)
_cell_measurement_reflns_used    16556
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.2696
_cell_measurement_theta_min      2.743
_cell_volume                     1925.04(4)
_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 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'ccd Xcalibur S'
_diffrn_measurement_method       '\w- amd \f-scans'
_diffrn_orient_matrix_UB_11      0.0200532589
_diffrn_orient_matrix_UB_12      0.0216297906
_diffrn_orient_matrix_UB_13      0.0417065217
_diffrn_orient_matrix_UB_21      0.0314574771
_diffrn_orient_matrix_UB_22      0.0332064804
_diffrn_orient_matrix_UB_23      -0.026263536
_diffrn_orient_matrix_UB_31      -0.0764789207
_diffrn_orient_matrix_UB_32      0.0193080628
_diffrn_orient_matrix_UB_33      -0.0016657444
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47043
_diffrn_reflns_theta_full        30.5
_diffrn_reflns_theta_max         30.5
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.83289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.046
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0581
_reflns_number_gt                4367
_reflns_number_total             5863
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900135b_si_001.cif
_cod_data_source_block           710342
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4338597