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_7114593
_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 H42 N2 Ni'
_chemical_formula_sum            'C32 H42 N2 Ni'
_chemical_formula_weight         513.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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_creation_date             2013-07-03
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.223(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.4764(4)
_cell_length_b                   36.2568(10)
_cell_length_c                   12.7163(4)
_cell_measurement_reflns_used    11451
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      31.0410
_cell_measurement_theta_min      3.5990
_cell_volume                     5752.2(3)
_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(10)
_diffrn_detector                 ATLAS
_diffrn_detector_area_resol_mean 7.9851
_diffrn_detector_type            CCD
_diffrn_measured_fraction_theta_full 0.9851
_diffrn_measured_fraction_theta_max 0.9076
_diffrn_measurement_details
;
  1 omega  -46.00   54.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       33.5453  -38.0000 -150.0000 200

  2 omega   13.00  108.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       33.5453   57.0000    0.0000 190

  3 omega -120.00  -64.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.8578  178.0000  -90.0000 112

  4 omega  -38.00   11.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.8578   57.0000   90.0000 98

  5 omega -109.00  -84.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.8578  -54.0000 -176.0000 50
;
_diffrn_measurement_device       SuperNova
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0093226000
_diffrn_orient_matrix_UB_12      0.0189521000
_diffrn_orient_matrix_UB_13      0.0104154000
_diffrn_orient_matrix_UB_21      0.0359143000
_diffrn_orient_matrix_UB_22      -0.0048358000
_diffrn_orient_matrix_UB_23      0.0411158000
_diffrn_orient_matrix_UB_31      0.0431200000
_diffrn_orient_matrix_UB_32      -0.0000779000
_diffrn_orient_matrix_UB_33      -0.0361899000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27792
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.20
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_target            'microfocus sealed X-ray tube'
_diffrn_source_type              'Agilent microfocus 1st generation'
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96541
_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 ? red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         11247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+30.8404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.1771
_reflns_number_gt                10004
_reflns_number_total             11247
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4cc02601b2.cif
_cod_data_source_block           1-H
_cod_database_code               7114593
_chemical_oxdiff_formula         'C32 H42 N2 Ni'
_reflns_odcompleteness_completeness 98.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2A(0.028) H3(0.028) H4(0.035) H5(0.036) H6(0.037) H7(0.035)
 H8(0.032) H12(0.039) H13(0.042) H14(0.034) H22(0.037) H23(0.04) H24(0.036)
 H31(0.031) H32(0.032) H33(0.063) H34(0.058) H35(0.053) H36(0.051) H37(0.048)
 H42(0.041) H43(0.04) H44(0.036) H52(0.041) H53(0.041) H54(0.042) H111(0.039)
 H11A(0.09) H11B(0.09) H11C(0.09) H11D(0.112) H11E(0.112) H11F(0.112)
 H151(0.033) H15A(0.118) H15B(0.118) H15C(0.118) H15D(0.083) H15E(0.083)
 H15F(0.083) H211(0.035) H21A(0.079) H21B(0.079) H21C(0.079) H21D(0.073)
 H21E(0.073) H21F(0.073) H251(0.039) H25A(0.068) H25B(0.068) H25C(0.068)
 H25D(0.081) H25E(0.081) H25F(0.081) H411(0.042) H41A(0.121) H41B(0.121)
 H41C(0.121) H41D(0.103) H41E(0.103) H41F(0.103) H451(0.039) H45A(0.095)
 H45B(0.095) H45C(0.095) H45D(0.117) H45E(0.117) H45F(0.117) H511(0.043)
 H51A(0.101) H51B(0.101) H51C(0.101) H51D(0.102) H51E(0.102) H51F(0.102)
 H551(0.055) H55A(0.103) H55B(0.103) H55C(0.103) H55D(0.132) H55E(0.132)
 H55F(0.132)
 Fixed X: H2A(0.7767) H3(0.6053) H4(0.6459) H5(0.5692) H6(0.7159) H7(0.8853)
 H8(0.8391) H12(1.0968) H13(1.1001) H14(0.9623) H22(0.4292) H23(0.2771)
 H24(0.2782) H31(0.7065) H32(0.7946) H33(0.9168) H34(0.7594) H35(0.6294)
 H36(0.7178) H37(0.8897) H42(0.7423) H43(0.9243) H44(1.0402) H52(0.3886)
 H53(0.4686) H54(0.6514) H111(0.876) H11A(0.9616) H11B(1.0736) H11C(0.9965)
 H11D(0.98) H11E(1.0078) H11F(1.0849) H151(0.7416) H15A(0.8708) H15B(0.8488)
 H15C(0.7592) H15D(0.668) H15E(0.6337) H15F(0.7235) H211(0.6825) H21A(0.7196)
 H21B(0.5997) H21C(0.6724) H21D(0.5852) H21E(0.5506) H21F(0.6713) H251(0.5028)
 H25A(0.3955) H25B(0.4448) H25C(0.3249) H25D(0.3557) H25E(0.2852) H25F(0.3825)
 H411(0.6086) H41A(0.581) H41B(0.5712) H41C(0.4848) H41D(0.516) H41E(0.6103)
 H41F(0.6287) H451(0.9653) H45A(1.0458) H45B(1.1299) H45C(1.1285) H45D(1.1156)
 H45E(1.0162) H45F(1.1054) H511(0.5263) H51A(0.3539) H51B(0.331) H51C(0.4172)
 H51D(0.391) H51E(0.482) H51F(0.3734) H551(0.8387) H55A(0.9165) H55B(0.8074)
 H55C(0.8168) H55D(0.924) H55E(0.8283) H55F(0.8155)
 Fixed Y: H2A(0.118) H3(0.1093) H4(0.286) H5(0.3004) H6(0.2934) H7(0.2793)
 H8(0.2698) H12(0.2171) H13(0.2405) H14(0.2293) H22(0.1642) H23(0.1859)
 H24(0.1983) H31(0.3639) H32(0.3562) H33(0.5143) H34(0.5509) H35(0.5551)
 H36(0.5289) H37(0.5006) H42(0.4419) H43(0.4467) H44(0.4321) H52(0.4476)
 H53(0.4709) H54(0.4712) H111(0.17) H11A(0.2224) H11B(0.2044) H11C(0.1872)
 H11D(0.1237) H11E(0.1268) H11F(0.1439) H151(0.17) H15A(0.1655) H15B(0.2066)
 H15C(0.1768) H15D(0.2271) H15E(0.215) H15F(0.2448) H211(0.1483) H21A(0.1623)
 H21B(0.1736) H21C(0.1969) H21D(0.0939) H21E(0.1081) H21F(0.0992) H251(0.1887)
 H25A(0.2354) H25B(0.2482) H25C(0.2354) H25D(0.17) H25E(0.1667) H25F(0.14)
 H411(0.4268) H41A(0.4743) H41B(0.4452) H41C(0.4465) H41D(0.3808) H41E(0.378)
 H41F(0.3666) H451(0.4118) H45A(0.4688) H45B(0.4413) H45C(0.4493) H45D(0.3746)
 H45E(0.359) H45F(0.3808) H511(0.4131) H51A(0.4301) H51B(0.4463) H51C(0.4648)
 H51D(0.3682) H51E(0.363) H51F(0.3817) H551(0.4413) H55A(0.4206) H55B(0.4267)
 H55C(0.3963) H55D(0.4869) H55E(0.5044) H55F(0.4952)
 Fixed Z: H2A(0.1453) H3(0.2339) H4(0.1339) H5(0.3098) H6(0.4428) H7(0.3473)
 H8(0.1582) H12(0.2367) H13(0.0696) H14(-0.0457) H22(0.5719) H23(0.49)
 H24(0.3122) H31(0.1211) H32(0.2915) H33(0.213) H34(0.1487) H35(0.2984)
 H36(0.4582) H37(0.4037) H42(0.6463) H43(0.6707) H44(0.5367) H52(0.0069) H53(-
 0.1412) H54(-0.1564) H111(0.3565) H11A(0.4252) H11B(0.4041) H11C(0.4879)
 H11D(0.2777) H11E(0.3977) H11F(0.3138) H151(0.0025) H15A(-0.1282) H15B(-
 0.1602) H15C(-0.1753) H15D(0.0458) H15E(-0.0678) H15F(-0.0525) H211(0.4484)
 H21A(0.624) H21B(0.6412) H21C(0.5661) H21D(0.4758) H21E(0.5871) H21F(0.5646)
 H251(0.1401) H25A(0.0696) H25B(0.1771) H25C(0.1713) H25D(0.0367) H25E(0.1381)
 H25F(0.1218) H411(0.4044) H41A(0.5258) H41B(0.6164) H41C(0.5266) H41D(0.4948)
 H41E(0.5763) H41F(0.4588) H451(0.2718) H45A(0.3086) H45B(0.2619) H45C(0.383)
 H45D(0.3004) H45E(0.3608) H45F(0.4219) H511(0.2341) H51A(0.2861) H51B(0.1739)
 H51C(0.2468) H51D(0.2113) H51E(0.1278) H51F(0.0953) H551(0.0404) H55A(-0.1171)
 H55B(-0.1763) H55C(-0.0891) H55D(-0.0623) H55E(-0.0003) H55F(-0.1202)
;