Selective P4 activation by an organometallic nickel(I) radical: formation of a dinuclear nickel(II) tetraphosphide and related di- and trichalcogenides
Stefan Pelties; Dirk Herrmann; Bas de Bruin; Frantisek Hartl; Robert Wolf; Chem.Commun. 50 (2014) 7014–; doi:10.1039/C4CC02601B

data_7114592
_publ_section_title
;
 Selective P4 activation by an organometallic nickel(I) radical: formation
 of a dinuclear nickel(II) tetraphosphide and related di- and
 trichalcogenides
;
_journal_name_full               Chem.Commun.
_journal_page_first              7014
_journal_paper_doi               10.1039/C4CC02601B
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C32 H41 N2 Ni'
_chemical_formula_sum            'C32 H41 N2 Ni'
_chemical_formula_weight         512.38
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-06
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                92.783(2)
_cell_angle_beta                 90.158(2)
_cell_angle_gamma                116.159(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1771(3)
_cell_length_b                   9.3242(3)
_cell_length_c                   18.2253(5)
_cell_measurement_reflns_used    12154
_cell_measurement_temperature    123.00(16)
_cell_measurement_theta_max      76.5000
_cell_measurement_theta_min      4.8480
_cell_volume                     1397.63(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.00(16)
_diffrn_detector_area_resol_mean 5.1773
_diffrn_measured_fraction_theta_full 0.9922
_diffrn_measured_fraction_theta_max 0.9677
_diffrn_measurement_details
;
  1 omega  -27.00   67.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064  -37.0000 -150.0000 94

  2 omega   17.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   37.0000   30.0000 93

  3 omega    4.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064 -125.0000  150.0000 94

  4 omega  -77.00  -15.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   45.0000 -120.0000 62

  5 omega   76.00  113.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000   60.0000 37

  6 omega   40.00   85.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  150.0000 45

  7 omega   35.00   65.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   60.0000 30

  8 omega   87.00  155.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000  -60.0000 68

  9 omega   42.00   68.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000   60.0000 26

 10 omega   36.00  116.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  -30.0000 80

 11 omega   40.00   77.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -90.0000 37

 12 omega   52.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  150.0000 62

 13 omega   35.00   60.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   90.0000 25

 14 omega   39.00  143.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -30.0000 104

 15 omega   41.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  120.0000 28

 16 omega  113.00  147.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  150.0000 34

 17 omega   35.00  116.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -120.0000 81

 18 omega   39.00   65.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -180.0000 26

 19 omega   27.00  154.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000    0.0000   90.0000 127

 20 omega  -71.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064   57.0000   30.0000 104

 21 omega   12.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   57.0000   90.0000 103

 22 omega   15.00  117.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   37.0000 -150.0000 102

 23 omega   12.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   57.0000  -90.0000 103

 24 omega   85.00  158.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  120.0000 73

 25 omega   83.00  158.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -120.0000 75

 26 omega   82.00  158.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -150.0000 76

 27 omega   79.00  158.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   60.0000 79

 28 omega   35.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -60.0000 34
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0584908000
_diffrn_orient_matrix_UB_12      -0.0263555000
_diffrn_orient_matrix_UB_13      0.0752293000
_diffrn_orient_matrix_UB_21      -0.1294080000
_diffrn_orient_matrix_UB_22      -0.1757536000
_diffrn_orient_matrix_UB_23      -0.0054795000
_diffrn_orient_matrix_UB_31      0.1218082000
_diffrn_orient_matrix_UB_32      -0.0490350000
_diffrn_orient_matrix_UB_33      -0.0384411000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14839
_diffrn_reflns_theta_full        70.93
_diffrn_reflns_theta_max         76.68
_diffrn_reflns_theta_min         4.86
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.0014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0319P)^2^+0.6198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0745
_reflns_number_gt                5475
_reflns_number_total             5715
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4cc02601b2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1397.63(7)
_cod_database_code               7114592
_chemical_oxdiff_formula         'C32 H41 N2 Ni'
_reflns_odcompleteness_completeness 99.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     70.93
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C121(H121), C161(H161), C221(H221), C261(H261)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14),
 C15(H15), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C122(H12a,H12b,H12c), C123(H12d,H12e,H12f), C162(H16a,H16b,H16c), C163(H16d,
 H16e,H16f), C222(H22a,H22b,H22c), C223(H22d,H22e,H22f), C262(H26a,H26b,H26c),
 C263(H26d,H26e,H26f)
;