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_7114588
_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 Te2, C6 H14'
_chemical_formula_sum            'C70 H96 N4 Ni2 Te2'
_chemical_formula_weight         1366.12
_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             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                 98.0580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.69630(10)
_cell_length_b                   20.47330(10)
_cell_length_c                   16.93030(10)
_cell_measurement_reflns_used    45790
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.5530
_cell_measurement_theta_min      3.8400
_cell_volume                     6759.71(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0059040000
_diffrn_orient_matrix_UB_12      -0.0618503000
_diffrn_orient_matrix_UB_13      0.0448797000
_diffrn_orient_matrix_UB_21      -0.0079702000
_diffrn_orient_matrix_UB_22      0.0421157000
_diffrn_orient_matrix_UB_23      0.0635014000
_diffrn_orient_matrix_UB_31      -0.0914252000
_diffrn_orient_matrix_UB_32      -0.0076789000
_diffrn_orient_matrix_UB_33      -0.0138185000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            88776
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.632
_diffrn_reflns_theta_min         3.129
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_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 brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.469
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         13479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+5.4258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12622
_reflns_number_total             13479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc02601b2.cif
_cod_data_source_block           6-Te
_cod_database_code               7114588
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C64 H82 N4 Ni2 Te2'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.027) H3(0.03) H4(0.029) H5(0.028) H6(0.027) H7(0.028)
 H8(0.03) H11(0.037) H12(0.042) H13(0.037) H15(0.037) H16A(0.071) H16B(0.071)
 H16C(0.071) H17A(0.065) H17B(0.065) H17C(0.065) H18(0.033) H19A(0.056)
 H19B(0.056) H19C(0.056) H20A(0.068) H20B(0.068) H20C(0.068) H23(0.035)
 H24(0.039) H25(0.035) H27(0.035) H28A(0.063) H28B(0.063) H28C(0.063)
 H29A(0.065) H29B(0.065) H29C(0.065) H30(0.033) H31A(0.057) H31B(0.057)
 H31C(0.057) H32A(0.061) H32B(0.061) H32C(0.061) H34(0.024) H35(0.025)
 H36(0.032) H37(0.032) H38(0.032) H39(0.032) H40(0.033) H43(0.029) H44(0.034)
 H45(0.031) H47(0.03) H48A(0.053) H48B(0.053) H48C(0.053) H49A(0.055)
 H49B(0.055) H49C(0.055) H50(0.026) H51A(0.044) H51B(0.044) H51C(0.044)
 H52A(0.048) H52B(0.048) H52C(0.048) H55(0.028) H56(0.03) H57(0.027) H59(0.029)
 H60A(0.059) H60B(0.059) H60C(0.059) H61A(0.048) H61B(0.048) H61C(0.048)
 H62(0.026) H63A(0.049) H63B(0.049) H63C(0.049) H64A(0.045) H64B(0.045)
 H64C(0.045) H10A(0.126) H10B(0.126) H10C(0.126) H10D(0.101) H10E(0.101)
 H10F(0.102) H10G(0.102) H10H(0.104) H10I(0.104) H10J(0.156) H10K(0.156)
 H10L(0.165) H10M(0.165) H10N(0.165)
 Fixed X: H2(0.3112) H3(0.4346) H4(0.2737) H5(0.228) H6(0.3297) H7(0.4371)
 H8(0.403) H11(0.0955) H12(0.0443) H13(0.107) H15(0.273) H16A(0.2136)
 H16B(0.1434) H16C(0.1921) H17A(0.2478) H17B(0.2523) H17C(0.1806) H18(0.2884)
 H19A(0.244) H19B(0.2225) H19C(0.1694) H20A(0.2592) H20B(0.1862) H20C(0.2513)
 H23(0.5765) H24(0.652) H25(0.6186) H27(0.4) H28A(0.4179) H28B(0.4382)
 H28C(0.4954) H29A(0.4271) H29B(0.505) H29C(0.4524) H30(0.4528) H31A(0.5159)
 H31B(0.5787) H31C(0.5108) H32A(0.5149) H32B(0.5068) H32C(0.5765) H34(0.2355)
 H35(0.1805) H36(0.0398) H37(0.1079) H38(0.1851) H39(0.1511) H40(0.0611)
 H43(0.1758) H44(0.2906) H45(0.3719) H47(0.1042) H48A(0.0395) H48B(0.0952)
 H48C(0.1132) H49A(0.0177) H49B(0.0774) H49C(0.0704) H50(0.3439) H51A(0.4215)
 H51B(0.3479) H51C(0.404) H52A(0.4594) H52B(0.4458) H52C(0.4122) H55(-0.0359)
 H56(0.0103) H57(0.1271) H59(0.0534) H60A(-0.0106) H60B(0.0523) H60C(-0.0212)
 H61A(-0.0645) H61B(-0.0795) H61C(-0.0393) H62(0.2516) H63A(0.3044)
 H63B(0.2335) H63C(0.2453) H64A(0.2997) H64B(0.2361) H64C(0.2294) H10A(0.4026)
 H10B(0.3698) H10C(0.3699) H10D(0.3001) H10E(0.3002) H10F(0.2415) H10G(0.2438)
 H10H(0.1685) H10I(0.1702) H10J(0.1127) H10K(0.1148) H10L(0.006) H10M(0.0381)
 H10N(0.036)
 Fixed Y: H2(-0.2442) H3(-0.2514) H4(-0.1104) H5(-0.2193) H6(-0.2893) H7(-
 0.2307) H8(-0.1191) H11(-0.2694) H12(-0.1762) H13(-0.1002) H15(-0.3035) H16A(-
 0.3861) H16B(-0.3549) H16C(-0.3176) H17A(-0.3998) H17B(-0.3403) H17C(-0.3678)
 H18(-0.0976) H19A(0.0051) H19B(-0.0119) H19C(-0.0192) H20A(-0.0817) H20B(-
 0.111) H20C(-0.1555) H23(-0.326) H24(-0.2398) H25(-0.1401) H27(-0.3203) H28A(-
 0.4106) H28B(-0.3459) H28C(-0.3914) H29A(-0.4205) H29B(-0.4014) H29C(-0.3622)
 H30(-0.0988) H31A(-0.0029) H31B(-0.0443) H31C(-0.0433) H32A(-0.058) H32B(-
 0.134) H32C(-0.1037) H34(0.2794) H35(0.2742) H36(0.0604) H37(-0.0111) H38(-
 0.0799) H39(-0.0626) H40(0.0228) H43(0.1356) H44(0.138) H45(0.159) H47(0.1437)
 H48A(0.2337) H48B(0.2488) H48C(0.2558) H49A(0.1241) H49B(0.0737) H49C(0.1332)
 H50(0.1819) H51A(0.2674) H51B(0.2854) H51C(0.2617) H52A(0.1538) H52B(0.1434)
 H52C(0.0964) H55(0.1488) H56(0.0908) H57(0.0755) H59(0.2031) H60A(0.2984)
 H60B(0.2945) H60C(0.2765) H61A(0.2001) H61B(0.1739) H61C(0.1304) H62(0.1221)
 H63A(0.1621) H63B(0.1608) H63C(0.2089) H64A(0.0437) H64B(0.0142) H64C(0.0366)
 H10A(0.0319) H10B(0.0492) H10C(0.101) H10D(-0.0153) H10E(0.0362) H10F(0.1076)
 H10G(0.0587) H10H(0.0391) H10I(-0.009) H10J(0.1132) H10K(0.0655) H10L(0.0651)
 H10M(-0.0046) H10N(0.0436)
 Fixed Z: H2(0.1301) H3(0.1763) H4(0.5239) H5(0.4743) H6(0.4553) H7(0.5172)
 H8(0.5558) H11(0.2887) H12(0.2323) H13(0.1745) H15(0.3218) H16A(0.3789)
 H16B(0.3426) H16C(0.4088) H17A(0.248) H17B(0.1907) H17C(0.2043) H18(0.1819)
 H19A(0.1401) H19B(0.2234) H19C(0.1457) H20A(0.0434) H20B(0.0474) H20C(0.065)
 H23(0.4306) H24(0.4401) H25(0.3846) H27(0.3486) H28A(0.4341) H28B(0.4812)
 H28C(0.4558) H29A(0.2931) H29B(0.305) H29C(0.2447) H30(0.2867) H31A(0.3181)
 H31B(0.3573) H31C(0.3957) H32A(0.1886) H32B(0.1812) H32C(0.2203) H34(0.4071)
 H35(0.5279) H36(0.3758) H37(0.2948) H38(0.3921) H39(0.5292) H40(0.5185)
 H43(0.1361) H44(0.1219) H45(0.2301) H47(0.3141) H48A(0.26) H48B(0.2049)
 H48C(0.2977) H49A(0.2072) H49B(0.2056) H49C(0.1467) H50(0.4307) H51A(0.4153)
 H51B(0.3729) H51C(0.3223) H52A(0.43) H52B(0.3374) H52C(0.3939) H55(0.5864)
 H56(0.6974) H57(0.7254) H59(0.4302) H60A(0.4445) H60B(0.5122) H60C(0.5307)
 H61A(0.3834) H61B(0.4662) H61C(0.4123) H62(0.6028) H63A(0.7268) H63B(0.7589)
 H63C(0.69) H64A(0.6952) H64B(0.6408) H64C(0.728) H10A(-0.0594) H10B(0.0171)
 H10C(-0.0511) H10D(-0.0659) H10E(-0.134) H10F(-0.0666) H10G(0.0042) H10H(-
 0.1444) H10I(-0.0727) H10J(-0.079) H10K(-0.0069) H10L(-0.0799) H10M(-0.0845)
 H10N(-0.1568)
;
_shelx_res_checksum              27842