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_4081066
_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            'C24 H27 P'
_chemical_formula_weight         346.43
_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             2010-12-05T18:43:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.187(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.7356(2)
_cell_length_b                   13.0017(2)
_cell_length_c                   35.9118(6)
_cell_measurement_reflns_used    14827
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.956
_cell_measurement_theta_min      2.8214
_cell_volume                     4055.02(13)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
        (compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
        (compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
        (compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics
;
 ORTEP3 for Windows
 L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_publication_material
;
 WINGX
 L.J. Farrugia,
 J. Appl. Cryst., 1999, 32, 837-838.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
 SHELXS-97
 Program for Crystal Structure Analysis (Release 97-2)
 G. M. Sheldrick, Instit\"ut f\"ur Anorganische Chemie der Universit\"at,
 Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998.
;
_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  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0185269
_diffrn_orient_matrix_UB_12      0.0475541
_diffrn_orient_matrix_UB_13      0.0090725
_diffrn_orient_matrix_UB_21      0.0405868
_diffrn_orient_matrix_UB_22      -0.0265782
_diffrn_orient_matrix_UB_23      0.0152461
_diffrn_orient_matrix_UB_31      0.0684275
_diffrn_orient_matrix_UB_32      0.0029186
_diffrn_orient_matrix_UB_33      -0.0089337
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            33068
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.97461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
        (compiled Oct 25 2010,18:11:34)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         8283
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0652P)^2^+1.8476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.13
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                6823
_reflns_number_total             8283
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400408e_si_001.cif
_cod_data_source_block           x1162fin
_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_sg_symbol_H-M      P2(1)/c
_cod_database_code               4081066