Nickel Phosphanido Hydride Complex: An Intermediate in the Hydrophosphination of Unactivated Alkenes by Primary Phosphine
Ganushevich, Yulia S.; Miluykov, Vasily A.; Polyancev, Fedor M.; Latypov, Shamil K.; Lönnecke, Peter; Hey-Hawkins, Evamarie; Yakhvarov, Dmitry G.; Sinyashin, Oleg G.; Organometallics 32 (2013) 3914–; doi:10.1021/om400408e

data_4081068
_publ_section_title
;
 Nickel Phosphanido Hydride Complex: An Intermediate in the
 Hydrophosphination of Unactivated Alkenes by Primary Phosphine
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3914
_journal_paper_doi               10.1021/om400408e
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C42 H67 Ni P3'
_chemical_formula_weight         723.58
_chemical_name_systematic
;
 ?
;
_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      2.4
_audit_creation_date             2012-01-02T13:07:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 117.066(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8063(5)
_cell_length_b                   35.6291(13)
_cell_length_c                   11.6308(5)
_cell_measurement_reflns_used    4041
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.1214
_cell_measurement_theta_min      2.5952
_cell_volume                     3987.7(3)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_molecular_graphics    'ORTEP3 for Windows (L. J. Farrugia, 1997)'
_computing_publication_material  'WINGX  (L.J. Farrugia,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo 1993)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'ccd Xcalibur S'
_diffrn_measurement_method       '\w- amd \f-scans'
_diffrn_orient_matrix_UB_11      0.0337423789
_diffrn_orient_matrix_UB_12      0.0108692911
_diffrn_orient_matrix_UB_13      0.0568842444
_diffrn_orient_matrix_UB_21      0.012413397
_diffrn_orient_matrix_UB_22      0.0142878467
_diffrn_orient_matrix_UB_23      -0.0356275856
_diffrn_orient_matrix_UB_31      -0.0641495523
_diffrn_orient_matrix_UB_32      0.0084579611
_diffrn_orient_matrix_UB_33      -0.0126427351
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.1522
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18266
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.99057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'deep yellow'
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism (rhombus)'
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         5681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0269P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.078
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                3217
_reflns_number_total             5681
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400408e_si_001.cif
_cod_data_source_block           x0621fin
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3987.6(3)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4081068