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_7114590
_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         'C64 H82 N4 Ni2 Se3'
_chemical_formula_sum            'C64 H82 N4 Ni2 Se3'
_chemical_formula_weight         1261.63
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_date             2014-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.196(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.8208(6)
_cell_length_b                   18.4669(10)
_cell_length_c                   39.0547(10)
_cell_measurement_reflns_used    15684
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.2610
_cell_measurement_theta_min      3.5170
_cell_volume                     12060.6(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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2013 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0461342000
_diffrn_orient_matrix_UB_12      0.0412242000
_diffrn_orient_matrix_UB_13      -0.0301845000
_diffrn_orient_matrix_UB_21      -0.0418310000
_diffrn_orient_matrix_UB_22      -0.0708341000
_diffrn_orient_matrix_UB_23      -0.0126389000
_diffrn_orient_matrix_UB_31      -0.0677460000
_diffrn_orient_matrix_UB_32      0.0156714000
_diffrn_orient_matrix_UB_33      0.0225073000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            43761
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.985
_diffrn_reflns_theta_min         3.566
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.152
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89919
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       block
_exptl_crystal_F_000             5216
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.756
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1315
_refine_ls_number_reflns         23312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+12.6020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19930
_reflns_number_total             23312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc02601b2.cif
_cod_data_source_block           7-Se
_cod_database_code               7114590
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C64 H82 N4 Ni2 Se'
_reflns_odcompleteness_completeness 98.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.034) H3(0.033) H4(0.04) H5(0.041) H6(0.04) H7(0.041)
 H8(0.042) H11(0.044) H12(0.045) H13(0.037) H15(0.042) H16A(0.067) H16B(0.067)
 H16C(0.067) H17A(0.075) H17B(0.075) H17C(0.075) H18(0.033) H19A(0.054)
 H19B(0.054) H19C(0.054) H20A(0.058) H20B(0.058) H20C(0.058) H23(0.064)
 H24(0.069) H25(0.058) H27(0.061) H28A(0.101) H28B(0.101) H28C(0.101)
 H29A(0.098) H29B(0.098) H29C(0.098) H30(0.045) H31A(0.065) H31B(0.065)
 H31C(0.065) H32A(0.076) H32B(0.076) H32C(0.076) H34(0.033) H35(0.033)
 H36(0.047) H37(0.048) H38(0.043) H39(0.045) H40(0.047) H43(0.052) H44(0.059)
 H45(0.054) H47(0.044) H48A(0.085) H48B(0.085) H48C(0.085) H49A(0.065)
 H49B(0.065) H49C(0.065) H50(0.046) H51A(0.076) H51B(0.076) H51C(0.076)
 H52A(0.079) H52B(0.079) H52C(0.079) H55(0.044) H56(0.047) H57(0.042)
 H59(0.042) H60A(0.069) H60B(0.069) H60C(0.069) H61A(0.067) H61B(0.067)
 H61C(0.067) H62(0.039) H63A(0.099) H63B(0.099) H63C(0.099) H64A(0.089)
 H64B(0.089) H64C(0.089) H66(0.036) H67(0.036) H68(0.041) H69(0.042) H70(0.048)
 H71(0.051) H72(0.048) H75(0.05) H76(0.055) H77(0.047) H79(0.045) H80A(0.077)
 H80B(0.077) H80C(0.077) H81A(0.069) H81B(0.069) H81C(0.069) H82(0.038)
 H83A(0.067) H83B(0.067) H83C(0.067) H84A(0.059) H84B(0.059) H84C(0.059)
 H87(0.05) H88(0.053) H89(0.045) H91(0.04) H92A(0.065) H92B(0.065) H92C(0.065)
 H93A(0.074) H93B(0.074) H93C(0.074) H94(0.048) H95A(0.07) H95B(0.07)
 H95C(0.07) H96A(0.089) H96B(0.089) H96C(0.089) H98(0.046) H99(0.05)
 H100(0.046) H101(0.049) H102(0.044) H103(0.043) H104(0.042) H107(0.056)
 H108(0.059) H109(0.05) H111(0.056) H11A(0.103) H11B(0.103) H11C(0.103)
 H11D(0.098) H11E(0.098) H11F(0.098) H114(0.04) H11G(0.077) H11H(0.077)
 H11I(0.077) H11J(0.08) H11K(0.08) H11L(0.08) H119(0.065) H120(0.075)
 H121(0.067) H123(0.053) H12A(0.077) H12B(0.077) H12C(0.077) H12D(0.077)
 H12E(0.077) H12F(0.077) H126(0.062) H12G(0.12) H12H(0.12) H12I(0.12)
 H12J(0.105) H12K(0.105) H12L(0.105)
 Fixed X: H2(1.0711) H3(1.1217) H4(1.086) H5(0.9609) H6(0.8532) H7(0.9176)
 H8(1.0625) H11(1.0126) H12(0.8925) H13(0.8239) H15(1.1066) H16A(1.169)
 H16B(1.1116) H16C(1.0774) H17A(1.2196) H17B(1.1622) H17C(1.164) H18(0.8759)
 H19A(0.7453) H19B(0.7538) H19C(0.753) H20A(0.8591) H20B(0.8747) H20C(0.9435)
 H23(1.2379) H24(1.16) H25(1.0346) H27(1.1823) H28A(1.282) H28B(1.2052)
 H28C(1.279) H29A(1.3161) H29B(1.3147) H29C(1.2618) H30(0.9293) H31A(0.9156)
 H31B(0.9977) H31C(0.9944) H32A(0.849) H32B(0.9227) H32C(0.8885) H34(0.5752)
 H35(0.5684) H36(0.5165) H37(0.622) H38(0.5878) H39(0.456) H40(0.4203)
 H43(0.4533) H44(0.5665) H45(0.6829) H47(0.439) H48A(0.3149) H48B(0.3826)
 H48C(0.347) H49A(0.3406) H49B(0.3755) H49C(0.4261) H50(0.7157) H51A(0.7737)
 H51B(0.6802) H51C(0.7263) H52A(0.8403) H52B(0.7981) H52C(0.7904) H55(0.4065)
 H56(0.5065) H57(0.6346) H59(0.4236) H60A(0.2886) H60B(0.311) H60C(0.3386)
 H61A(0.3478) H61B(0.4376) H61C(0.3746) H62(0.697) H63A(0.7145) H63B(0.7958)
 H63C(0.7496) H64A(0.7997) H64B(0.7207) H64C(0.7493) H66(0.9936) H67(1.0215)
 H68(0.959) H69(0.8809) H70(0.967) H71(1.0921) H72(1.0946) H75(0.7793)
 H76(0.8693) H77(1.0022) H79(0.8205) H80A(0.6829) H80B(0.695) H80C(0.7245)
 H81A(0.749) H81B(0.8371) H81C(0.7672) H82(1.0968) H83A(1.1935) H83B(1.129)
 H83C(1.1274) H84A(1.1581) H84B(1.0892) H84C(1.0709) H87(0.9188) H88(1.0425)
 H89(1.1451) H91(0.852) H92A(0.7437) H92B(0.7903) H92C(0.8021) H93A(0.8124)
 H93B(0.8755) H93C(0.9039) H94(1.1309) H95A(1.2454) H95B(1.2234) H95C(1.1693)
 H96A(1.2481) H96B(1.1724) H96C(1.2227) H98(0.5045) H99(0.458) H100(0.6213)
 H101(0.4766) H102(0.4362) H103(0.5509) H104(0.6687) H107(0.6976) H108(0.6183)
 H109(0.5032) H111(0.6708) H11A(0.7029) H11B(0.6147) H11C(0.6826) H11D(0.8046)
 H11E(0.7893) H11F(0.7843) H114(0.4389) H11G(0.3562) H11H(0.4459) H11I(0.4008)
 H11J(0.319) H11K(0.3641) H11L(0.3841) H119(0.5147) H120(0.3859) H121(0.3056)
 H123(0.6194) H12A(0.6504) H12B(0.5755) H12C(0.5642) H12D(0.7097) H12E(0.6612)
 H12F(0.6394) H126(0.3657) H12G(0.2452) H12H(0.3128) H12I(0.2475) H12J(0.2475)
 H12K(0.2476) H12L(0.3147)
 Fixed Y: H2(0.5176) H3(0.5214) H4(0.2305) H5(0.1876) H6(0.1844) H7(0.2062)
 H8(0.2302) H11(0.3026) H12(0.3499) H13(0.4293) H15(0.3266) H16A(0.2319)
 H16B(0.2435) H16C(0.2159) H17A(0.355) H17B(0.4219) H17C(0.3745) H18(0.478)
 H19A(0.5156) H19B(0.4323) H19C(0.4868) H20A(0.5979) H20B(0.5726) H20C(0.5683)
 H23(0.336) H24(0.3531) H25(0.4009) H27(0.3733) H28A(0.2837) H28B(0.2538)
 H28C(0.2782) H29A(0.4124) H29B(0.4136) H29C(0.4682) H30(0.4363) H31A(0.5596)
 H31B(0.5451) H31C(0.556) H32A(0.4655) H32B(0.4573) H32C(0.3894) H34(-0.0336)
 H35(0.0125) H36(0.3108) H37(0.3705) H38(0.3519) H39(0.2891) H40(0.2507)
 H43(0.08) H44(0.0491) H45(0.0261) H47(0.1302) H48A(0.1452) H48B(0.1804)
 H48C(0.105) H49A(0.0412) H49B(-0.0046) H49C(0.0071) H50(0.0413) H51A(-0.0727)
 H51B(-0.0788) H51C(-0.0761) H52A(0.0418) H52B(0.0413) H52C(0.1091) H55(0.2051)
 H56(0.2704) H57(0.2666) H59(0.1002) H60A(0.1293) H60B(0.1763) H60C(0.2005)
 H61A(0.0212) H61B(0.02) H61C(0.0636) H62(0.1943) H63A(0.0884) H63B(0.1295)
 H63C(0.1341) H64A(0.2602) H64B(0.3059) H64C(0.268) H66(-0.0117) H67(-0.0459)
 H68(0.3411) H69(0.3415) H70(0.2833) H71(0.2389) H72(0.2914) H75(0.1944)
 H76(0.2375) H77(0.2071) H79(0.1196) H80A(0.1282) H80B(0.1442) H80C(0.2002)
 H81A(0.0132) H81B(0.0067) H81C(0.0222) H82(0.113) H83A(0.182) H83B(0.2338)
 H83C(0.2159) H84A(0.0607) H84B(0.0902) H84C(0.0307) H87(0.0328) H88(0.0636)
 H89(0.0901) H91(0.0412) H92A(0.0186) H92B(0.0874) H92C(0.0132) H93A(-0.0801)
 H93B(-0.0894) H93C(-0.076) H94(0.1012) H95A(0.165) H95B(0.152) H95C(0.2018)
 H96A(0.0329) H96B(-0.0148) H96C(0.0162) H98(0.482) H99(0.5156) H100(0.2242)
 H101(0.2514) H102(0.2069) H103(0.1359) H104(0.1565) H107(0.3331) H108(0.2401)
 H109(0.2104) H111(0.4401) H11A(0.529) H11B(0.5027) H11C(0.4746) H11D(0.448)
 H11E(0.3915) H11F(0.3675) H114(0.281) H11G(0.1851) H11H(0.1606) H11I(0.1798)
 H11J(0.3109) H11K(0.3137) H11L(0.3704) H119(0.4091) H120(0.3697) H121(0.3548)
 H123(0.4327) H12A(0.5489) H12B(0.5465) H12C(0.5472) H12D(0.44) H12E(0.3675)
 H12F(0.4322) H126(0.37) H12G(0.4345) H12H(0.4826) H12I(0.448) H12J(0.3034)
 H12K(0.3077) H12L(0.2642)
 Fixed Z: H2(0.8166) H3(0.8779) H4(0.8526) H5(0.8177) H6(0.8575) H7(0.9181)
 H8(0.9155) H11(0.7301) H12(0.7078) H13(0.7394) H15(0.8148) H16A(0.7883)
 H16B(0.7544) H16C(0.7878) H17A(0.7867) H17B(0.7864) H17C(0.7532) H18(0.8264)
 H19A(0.8086) H19B(0.8021) H19C(0.7713) H20A(0.8063) H20B(0.7693) H20C(0.7997)
 H23(0.9613) H24(1.0048) H25(0.9943) H27(0.8724) H28A(0.876) H28B(0.8906)
 H28C(0.9159) H29A(0.8796) H29B(0.9196) H29C(0.8964) H30(0.9139) H31A(0.9271)
 H31B(0.9127) H31C(0.9524) H32A(0.9573) H32B(0.9853) H32C(0.9646) H34(0.8559)
 H35(0.797) H36(0.8078) H37(0.8474) H38(0.9084) H39(0.9058) H40(0.8446)
 H43(0.9667) H44(1.001) H45(0.9779) H47(0.88) H48A(0.9012) H48B(0.9266)
 H48C(0.9353) H49A(0.8664) H49B(0.8984) H49C(0.8674) H50(0.8898) H51A(0.9046)
 H51B(0.8999) H51C(0.937) H52A(0.9231) H52B(0.957) H52C(0.9328) H55(0.7317)
 H56(0.7104) H57(0.7376) H59(0.8084) H60A(0.7938) H60B(0.7628) H60C(0.8006)
 H61A(0.7705) H61B(0.7633) H61C(0.7389) H62(0.8184) H63A(0.7874) H63B(0.7957)
 H63C(0.7587) H64A(0.7979) H64B(0.7943) H64C(0.7619) H66(1.0612) H67(1.1221)
 H68(1.159) H69(1.0995) H70(1.0592) H71(1.0947) H72(1.154) H75(1.0072)
 H76(0.9718) H77(0.9818) H79(1.088) H80A(1.0742) H80B(1.0356) H80C(1.0644)
 H81A(1.073) H81B(1.0637) H81C(1.0347) H82(1.0545) H83A(1.0303) H83B(1.043)
 H83C(1.0037) H84A(1.009) H84B(0.9824) H84C(1.0091) H87(1.2381) H88(1.2641)
 H89(1.2318) H91(1.1495) H92A(1.1813) H92B(1.1959) H92C(1.2153) H93A(1.155)
 H93B(1.1873) H93C(1.1509) H94(1.1403) H95A(1.1631) H95B(1.2006) H95C(1.1752)
 H96A(1.1535) H96B(1.1572) H96C(1.1901) H98(1.0423) H99(1.0974) H100(1.1861)
 H101(1.1717) H102(1.1114) H103(1.0921) H104(1.1358) H107(0.9839) H108(0.962)
 H109(0.9864) H111(1.0573) H11A(1.0177) H11B(1.0083) H11C(0.9872) H11D(1.0463)
 H11E(1.0164) H11F(1.0546) H114(1.0617) H11G(1.0413) H11H(1.0443) H11I(1.0082)
 H11J(1.0284) H11K(0.9954) H11L(1.0249) H119(1.2291) H120(1.229) H121(1.1784)
 H123(1.1555) H12A(1.1772) H12B(1.1978) H12C(1.1574) H12D(1.205) H12E(1.2049)
 H12F(1.2281) H126(1.0941) H12G(1.0849) H12H(1.104) H12I(1.1247) H12J(1.0907)
 H12K(1.1308) H12L(1.1148)
;
_shelx_res_checksum              61416