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_7114586
_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 S2'
_chemical_formula_sum            'C64 H82 N4 Ni2 S2'
_chemical_formula_weight         1088.88
_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             2013-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                100.585(3)
_cell_angle_beta                 95.676(3)
_cell_angle_gamma                114.757(4)
_cell_formula_units_Z            2
_cell_length_a                   13.0231(5)
_cell_length_b                   14.2423(6)
_cell_length_c                   18.1147(5)
_cell_measurement_reflns_used    11760
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.6810
_cell_measurement_theta_min      3.7720
_cell_volume                     2940.4(2)
_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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.9908
_diffrn_measured_fraction_theta_max 0.9552
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0843600000
_diffrn_orient_matrix_UB_12      -0.0500490000
_diffrn_orient_matrix_UB_13      -0.0041758000
_diffrn_orient_matrix_UB_21      -0.0815799000
_diffrn_orient_matrix_UB_22      -0.0862048000
_diffrn_orient_matrix_UB_23      -0.0717429000
_diffrn_orient_matrix_UB_31      0.0623087000
_diffrn_orient_matrix_UB_32      0.0720489000
_diffrn_orient_matrix_UB_33      -0.0512135000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21454
_diffrn_reflns_theta_full        66.97
_diffrn_reflns_theta_max         73.66
_diffrn_reflns_theta_min         3.53
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87508
_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_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         11356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0348P)^2^+1.0071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                9816
_reflns_number_total             11356
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4cc02601b2.cif
_cod_data_source_block           6-S
_cod_original_cell_volume        2940.41(19)
_cod_database_code               7114586
_chemical_oxdiff_formula         'C64 H82 N4 Ni2 S2'
_reflns_odcompleteness_completeness 99.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.029) H3(0.028) H4(0.036) H5(0.034) H6(0.036) H7(0.039)
 H8(0.039) H11(0.035) H12(0.041) H13(0.036) H15(0.031) H16A(0.082) H16B(0.082)
 H16C(0.082) H17A(0.093) H17B(0.093) H17C(0.093) H18(0.031) H19A(0.051)
 H19B(0.051) H19C(0.051) H20A(0.057) H20B(0.057) H20C(0.057) H23(0.032)
 H24(0.038) H25(0.034) H27(0.028) H28A(0.047) H28B(0.047) H28C(0.047)
 H29A(0.054) H29B(0.054) H29C(0.054) H30(0.03) H31A(0.06) H31B(0.06) H31C(0.06)
 H32A(0.067) H32B(0.067) H32C(0.067) H34(0.027) H35(0.028) H36(0.035) H37(0.03)
 H38(0.03) H39(0.034) H40(0.036) H43(0.039) H44(0.047) H45(0.04) H47(0.035)
 H48A(0.055) H48B(0.055) H48C(0.055) H49A(0.066) H49B(0.066) H49C(0.066)
 H50(0.035) H51A(0.065) H51B(0.065) H51C(0.065) H52A(0.057) H52B(0.057)
 H52C(0.057) H55(0.044) H56(0.053) H57(0.046) H59(0.031) H60A(0.069)
 H60B(0.069) H60C(0.069) H61A(0.068) H61B(0.068) H61C(0.068) H62(0.039)
 H63A(0.072) H63B(0.072) H63C(0.072) H64A(0.072) H64B(0.072) H64C(0.072)
 Fixed X: H2(0.8044) H3(0.6422) H4(0.4591) H5(0.3736) H6(0.5366) H7(0.7193)
 H8(0.669) H11(0.8301) H12(0.9813) H13(1.0128) H15(0.6104) H16A(0.5508)
 H16B(0.6667) H16C(0.5783) H17A(0.655) H17B(0.7455) H17C(0.7766) H18(0.8357)
 H19A(0.945) H19B(0.8647) H19C(0.9961) H20A(1.0209) H20B(1.0728) H20C(0.9873)
 H23(0.2349) H24(0.2207) H25(0.3529) H27(0.4452) H28A(0.2757) H28B(0.2528)
 H28C(0.2111) H29A(0.4222) H29B(0.3633) H29C(0.4939) H30(0.5719) H31A(0.5561)
 H31B(0.4655) H31C(0.4354) H32A(0.7036) H32B(0.6837) H32C(0.6246) H34(0.0057)
 H35(-0.1549) H36(-0.0533) H37(0.1327) H38(0.2936) H39(0.2052) H40(-0.0074)
 H43(0.4207) H44(0.4392) H45(0.3012) H47(0.2) H48A(0.364) H48B(0.3904)
 H48C(0.4358) H49A(0.2256) H49B(0.2894) H49C(0.158) H50(0.0698) H51A(0.0763)
 H51B(0.1716) H51C(0.1987) H52A(-0.0602) H52B(-0.0314) H52C(0.0264) H55(-
 0.2047) H56(-0.3491) H57(-0.3631) H59(0.0313) H60A(0.0847) H60B(-0.0345)
 H60C(0.0539) H61A(-0.1036) H61B(-0.1283) H61C(-0.007) H62(-0.163) H63A(-
 0.2683) H63B(-0.2006) H63C(-0.3332) H64A(-0.3356) H64B(-0.4032) H64C(-0.3113)
 Fixed Y: H2(0.4191) H3(0.4637) H4(0.161) H5(-0.0182) H6(-0.0513) H7(0.1134)
 H8(0.2502) H11(0.051) H12(0.1225) H13(0.272) H15(0.1343) H16A(-0.0341) H16B(-
 0.0345) H16C(-0.0365) H17A(0.1311) H17B(0.2355) H17C(0.1415) H18(0.4074)
 H19A(0.451) H19B(0.3278) H19C(0.3721) H20A(0.5531) H20B(0.4771) H20C(0.498)
 H23(0.3359) H24(0.4063) H25(0.4317) H27(0.2478) H28A(0.1475) H28B(0.1246)
 H28C(0.2004) H29A(0.3207) H29B(0.3814) H29C(0.4124) H30(0.3499) H31A(0.4091)
 H31B(0.4457) H31C(0.3241) H32A(0.5231) H32B(0.5138) H32C(0.5679) H34(-0.4446)
 H35(-0.4314) H36(0.0043) H37(0.1225) H38(0.1459) H39(0.0543) H40(-0.0502) H43(-
 0.2865) H44(-0.2262) H45(-0.1862) H47(-0.3112) H48A(-0.2858) H48B(-0.1843)
 H48C(-0.2659) H49A(-0.4638) H49B(-0.4515) H49C(-0.4793) H50(-0.1735) H51A(-
 0.1223) H51B(-0.1595) H51C(-0.0621) H52A(-0.2993) H52B(-0.3566) H52C(-0.3481)
 H55(-0.1407) H56(-0.1455) H57(-0.2036) H59(-0.1899) H60A(-0.0772) H60B(-
 0.0737) H60C(-0.0228) H61A(-0.3443) H61B(-0.2738) H61C(-0.2731) H62(-0.273)
 H63A(-0.2312) H63B(-0.1322) H63C(-0.2026) H64A(-0.4128) H64B(-0.3938) H64C(-
 0.4353)
 Fixed Z: H2(0.4913) H3(0.4795) H4(0.1218) H5(0.1507) H6(0.2072) H7(0.2251)
 H8(0.182) H11(0.4198) H12(0.359) H13(0.3154) H15(0.4409) H16A(0.4645)
 H16B(0.4484) H16C(0.382) H17A(0.5692) H17B(0.5526) H17C(0.5574) H18(0.322)
 H19A(0.2272) H19B(0.206) H19C(0.2405) H20A(0.361) H20B(0.3802) H20C(0.4282)
 H23(0.4203) H24(0.3177) H25(0.2388) H27(0.4718) H28A(0.5127) H28B(0.4231)
 H28C(0.4712) H29A(0.5924) H29B(0.5552) H29C(0.5553) H30(0.2446) H31A(0.1338)
 H31B(0.1618) H31C(0.141) H32A(0.246) H32B(0.3288) H32C(0.2836) H34(0.1053)
 H35(0.1585) H36(0.2022) H37(0.2925) H38(0.2197) H39(0.0817) H40(0.0737)
 H43(0.1239) H44(0.0143) H45(-0.0413) H47(0.2316) H48A(0.3152) H48B(0.2838)
 H48C(0.2503) H49A(0.2378) H49B(0.1686) H49C(0.1565) H50(0.0329) H51A(-0.083)
 H51B(-0.098) H51C(-0.0295) H52A(-0.077) H52B(-0.0178) H52C(-0.0898) H55(0.362)
 H56(0.2755) H57(0.1465) H59(0.3177) H60A(0.4403) H60B(0.4305) H60C(0.3796)
 H61A(0.3451) H61B(0.4114) H61C(0.4178) H62(0.0586) H63A(-0.0315) H63B(0.0386)
 H63C(0.0306) H64A(-0.0167) H64B(0.0468) H64C(0.0631)
;