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_7114596
_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_absolute_configuration unk
_chemical_formula_moiety         'C36 H49 N2 Ni O, F6 P'
_chemical_formula_sum            'C36 H49 F6 N2 Ni O P'
_chemical_formula_weight         729.45
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-21
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.4860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7889(2)
_cell_length_b                   16.8666(3)
_cell_length_c                   16.4852(3)
_cell_measurement_reflns_used    13554
_cell_measurement_temperature    122.96(18)
_cell_measurement_theta_max      73.1390
_cell_measurement_theta_min      4.2980
_cell_volume                     3545.05(11)
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      122.96(18)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9840
_diffrn_measurement_details
;
  1 omega   22.00  111.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   37.0000  -60.0000 178

  2 omega   27.00  117.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   37.0000 -150.0000 180

  3 omega   32.00   74.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  -30.0000 84

  4 omega   36.00   64.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000    0.0000 56

  5 omega   38.00  109.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000    0.0000 142

  6 omega   31.00   68.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -150.0000 74

  7 omega   76.00  158.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  120.0000 164

  8 omega   29.00   69.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000   30.0000 80

  9 omega   35.00   86.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000 -120.0000 102

 10 omega   26.00   82.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000 -180.0000 112

 11 omega  -98.00   -2.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  125.0000  -60.0000 192

 12 omega  -33.00   71.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064  -57.0000  150.0000 208

 13 omega   15.00  117.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   37.0000   90.0000 204

 14 omega   79.00  158.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000   90.0000 158

 15 omega   76.00  158.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000 -150.0000 164

 16 omega   77.00  158.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  -90.0000 162

 17 omega   29.00   69.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -180.0000 80

 18 omega   32.00  121.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000 -180.0000 178

 19 omega   46.00  158.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   15.0000   30.0000 224

 20 omega -120.00   -8.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -77.0000  150.0000 224

 21 omega    8.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   77.0000   90.0000 224

 22 omega   12.00  115.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   57.0000  -30.0000 206

 23 omega -162.00  -49.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000  -50.7416 226

 24 omega -162.00  -49.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000   30.0000 226

 25 omega   73.00  158.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000 -150.0000 170

 26 omega   32.00   76.50   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  150.0000 89
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0229755000
_diffrn_orient_matrix_UB_12      0.0203420000
_diffrn_orient_matrix_UB_13      0.0879466000
_diffrn_orient_matrix_UB_21      -0.1068947000
_diffrn_orient_matrix_UB_22      0.0351564000
_diffrn_orient_matrix_UB_23      -0.0312645000
_diffrn_orient_matrix_UB_31      -0.0516670000
_diffrn_orient_matrix_UB_32      -0.0817579000
_diffrn_orient_matrix_UB_33      0.0083566000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20803
_diffrn_reflns_theta_full        66.97
_diffrn_reflns_theta_max         73.66
_diffrn_reflns_theta_min         4.35
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.754
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80138
_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 light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.1974
_exptl_crystal_size_mid          0.0705
_exptl_crystal_size_min          0.0462
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6714
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0324P)^2^+0.6977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                6549
_reflns_number_total             6714
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4cc02601b2.cif
_cod_data_source_block           mccc
_cod_database_code               7114596
_chemical_oxdiff_formula         'C32 H41 N2 Ni P F6'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C27(H27), C30(H30)
2.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
2.c Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C)
2.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12),
 C13(H13), C23(H23), C24(H24), C25(H25)
;