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_7114587
_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 Se2, C6 H14'
_chemical_formula_sum            'C70 H96 N4 Ni2 Se2'
_chemical_formula_weight         1268.84
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.1920(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5580(3)
_cell_length_b                   20.1611(2)
_cell_length_c                   16.7962(2)
_cell_measurement_reflns_used    18301
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.4600
_cell_measurement_theta_min      3.1520
_cell_volume                     6584.29(14)
_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 0.9918
_diffrn_measured_fraction_theta_max 0.9636
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0762822000
_diffrn_orient_matrix_UB_12      0.0415948000
_diffrn_orient_matrix_UB_13      0.0040683000
_diffrn_orient_matrix_UB_21      0.0395762000
_diffrn_orient_matrix_UB_22      0.0589568000
_diffrn_orient_matrix_UB_23      -0.0333559000
_diffrn_orient_matrix_UB_31      -0.0336252000
_diffrn_orient_matrix_UB_32      -0.0252191000
_diffrn_orient_matrix_UB_33      -0.0716979000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32467
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.481
_diffrn_reflns_theta_min         3.158
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.282
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65750
_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    1.280
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         12810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+3.4382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10916
_reflns_number_total             12810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc02601b2.cif
_cod_data_source_block           6-Se
_cod_original_cell_volume        6584.28(14)
_cod_database_code               7114587
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C64 H82 N4 Ni2 Se2'
_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.023) H3(0.022) H4(0.029) H5(0.029) H6(0.03) H7(0.029)
 H8(0.03) H11(0.027) H12(0.028) H13(0.026) H15(0.025) H16A(0.041) H16B(0.041)
 H16C(0.041) H17A(0.046) H17B(0.046) H17C(0.046) H18(0.027) H19A(0.045)
 H19B(0.045) H19C(0.045) H20A(0.052) H20B(0.052) H20C(0.052) H23(0.027)
 H24(0.031) H25(0.028) H27(0.029) H28A(0.055) H28B(0.055) H28C(0.055)
 H29A(0.05) H29B(0.05) H29C(0.05) H30(0.024) H31A(0.044) H31B(0.044)
 H31C(0.044) H32A(0.04) H32B(0.04) H32C(0.04) H34(0.028) H35(0.026) H36(0.028)
 H37(0.03) H38(0.027) H39(0.027) H40(0.028) H43(0.034) H44(0.038) H45(0.035)
 H47(0.034) H48A(0.072) H48B(0.072) H48C(0.072) H49A(0.066) H49B(0.066)
 H49C(0.066) H50(0.034) H51A(0.059) H51B(0.059) H51C(0.059) H52A(0.064)
 H52B(0.064) H52C(0.064) H55(0.036) H56(0.041) H57(0.038) H59(0.033)
 H60A(0.054) H60B(0.054) H60C(0.054) H61A(0.072) H61B(0.072) H61C(0.072)
 H62(0.041) H63A(0.079) H63B(0.079) H63C(0.079) H64A(0.072) H64B(0.072)
 H64C(0.072) H10A(0.11) H10B(0.11) H10C(0.11) H10D(0.072) H10E(0.072)
 H10F(0.071) H10G(0.071) H10H(0.077) H10I(0.077) H10J(0.11) H10K(0.11)
 H10L(0.157) H10M(0.157) H10N(0.157)
 Fixed X: H2(0.8183) H3(0.764) H4(0.9349) H5(0.8451) H6(0.8135) H7(0.891)
 H8(0.9579) H11(0.8716) H12(0.9882) H13(1.0347) H15(0.7467) H16A(0.7002)
 H16B(0.7706) H16C(0.7649) H17A(0.6925) H17B(0.751) H17C(0.7633) H18(0.9448)
 H19A(1.0631) H19B(1.0387) H19C(1.0784) H20A(1.0085) H20B(1.0194) H20C(0.9455)
 H23(0.8296) H24(0.7155) H25(0.6316) H27(0.8963) H28A(0.9854) H28B(0.9345)
 H28C(0.9252) H29A(0.963) H29B(0.8885) H29C(0.9089) H30(0.6561) H31A(0.5426)
 H31B(0.5939) H31C(0.5574) H32A(0.5732) H32B(0.5912) H32C(0.6458) H34(0.5598)
 H35(0.6816) H36(0.7196) H37(0.5905) H38(0.5604) H39(0.6705) H40(0.7699)
 H43(0.3825) H44(0.3485) H45(0.4228) H47(0.5477) H48A(0.4874) H48B(0.493)
 H48C(0.424) H49A(0.4851) H49B(0.4225) H49C(0.4915) H50(0.599) H51A(0.5842)
 H51B(0.5071) H51C(0.5659) H52A(0.5699) H52B(0.5417) H52C(0.4917) H55(0.8789)
 H56(0.9524) H57(0.9108) H59(0.6956) H60A(0.73) H60B(0.8075) H60C(0.7614)
 H61A(0.7085) H61B(0.7229) H61C(0.7844) H62(0.7362) H63A(0.8055) H63B(0.8255)
 H63C(0.8717) H64A(0.762) H64B(0.8242) H64C(0.7488) H10A(0.5983) H10B(0.6341)
 H10C(0.632) H10D(0.7045) H10E(0.7023) H10F(0.7647) H10G(0.7604) H10H(0.8331)
 H10I(0.8346) H10J(0.8896) H10K(0.8923) H10L(0.9987) H10M(0.9668) H10N(0.9642)
 Fixed Y: H2(-0.2749) H3(-0.2802) H4(-0.0187) H5(0.0684) H6(0.0848) H7(0.0137)
 H8(-0.0585) H11(-0.0731) H12(-0.0899) H13(-0.1487) H15(-0.1206) H16A(-0.0352)
 H16B(-0.0268) H16C(-0.0093) H17A(-0.153) H17B(-0.2031) H17C(-0.1502) H18(-
 0.2037) H19A(-0.2019) H19B(-0.1307) H19C(-0.1752) H20A(-0.3008) H20B(-0.2783)
 H20C(-0.2963) H23(-0.1417) H24(-0.1463) H25(-0.1617) H27(-0.1448) H28A(-
 0.1237) H28B(-0.1332) H28C(-0.0731) H29A(-0.2356) H29B(-0.2583) H29C(-0.2514)
 H30(-0.1787) H31A(-0.1432) H31B(-0.0883) H31C(-0.1345) H32A(-0.2611) H32B(-
 0.2576) H32C(-0.284) H34(0.2589) H35(0.2475) H36(0.092) H37(0.1039)
 H38(0.2184) H39(0.2766) H40(0.2026) H43(0.135) H44(0.2363) H45(0.325)
 H47(0.0957) H48A(-0.0028) H48B(0.0388) H48C(0.0379) H49A(0.052) H49B(0.0974)
 H49C(0.1292) H50(0.3203) H51A(0.4078) H51B(0.3875) H51C(0.3399) H52A(0.4248)
 H52B(0.3686) H52C(0.4057) H55(0.0911) H56(0.1638) H57(0.2534) H59(0.094) H60A(-
 0.0125) H60B(0.0082) H60C(0.0041) H61A(0.075) H61B(0.1497) H61C(0.1011)
 H62(0.2917) H63A(0.3645) H63B(0.2911) H63C(0.3329) H64A(0.3951) H64B(0.3631)
 H64C(0.3417) H10A(-0.0312) H10B(-0.1003) H10C(-0.0495) H10D(-0.0292)
 H10E(0.0216) H10F(-0.103) H10G(-0.0546) H10H(0.018) H10I(-0.0264) H10J(-
 0.0645) H10K(-0.1075) H10L(-0.057) H10M(-0.0297) H10N(0.0133)
 Fixed Z: H2(-0.02) H3(0.1049) H4(-0.0184) H5(-0.0222) H6(0.1183) H7(0.2106)
 H8(0.1248) H11(-0.2213) H12(-0.1985) H13(-0.0881) H15(-0.0928) H16A(-0.1762)
 H16B(-0.2118) H16C(-0.1218) H17A(-0.2186) H17B(-0.1888) H17C(-0.2542)
 H18(0.0729) H19A(0.1154) H19B(0.0877) H19C(0.0315) H20A(0.0552) H20B(-0.0318)
 H20C(-0.0107) H23(0.3759) H24(0.3983) H25(0.2936) H27(0.1897) H28A(0.2912)
 H28B(0.3563) H28C(0.2969) H29A(0.2393) H29B(0.2067) H29C(0.2992) H30(0.0878)
 H31A(0.0947) H31B(0.1302) H31C(0.1877) H32A(0.1044) H32B(0.1976) H32C(0.1435)
 H34(0.3008) H35(0.3506) H36(-0.0425) H37(-0.0669) H38(-0.0289) H39(0.0238)
 H40(-0.0014) H43(0.0931) H44(0.0401) H45(0.0488) H47(0.1906) H48A(0.1595)
 H48B(0.0816) H48C(0.121) H49A(0.2902) H49B(0.2602) H49C(0.2983) H50(0.1297)
 H51A(0.0369) H51B(0.0153) H51C(-0.0058) H52A(0.1771) H52B(0.2293) H52C(0.1649)
 H55(0.3392) H56(0.2871) H57(0.2128) H59(0.304) H60A(0.3478) H60B(0.3503)
 H60C(0.2681) H61A(0.4432) H61B(0.4251) H61C(0.4487) H62(0.155) H63A(0.0914)
 H63B(0.0738) H63C(0.1373) H64A(0.2162) H64B(0.2694) H64C(0.2806) H10A(0.5734)
 H10B(0.5666) H10C(0.4957) H10D(0.6463) H10E(0.5757) H10F(0.5764) H10G(0.5034)
 H10H(0.5739) H10I(0.6504) H10J(0.5114) H10K(0.5892) H10L(0.5822) H10M(0.6574)
 H10N(0.5794)
;
_shelx_res_checksum              88440