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_7114594
_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         'C26 H29 N2 Ni'
_chemical_formula_sum            'C26 H29 N2 Ni'
_chemical_formula_weight         428.22
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.89090(10)
_cell_length_b                   11.10740(10)
_cell_length_c                   9.03710(10)
_cell_measurement_reflns_used    31289
_cell_measurement_temperature    123.1(4)
_cell_measurement_theta_max      66.9240
_cell_measurement_theta_min      5.2430
_cell_volume                     2297.76(3)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.1(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1169996000
_diffrn_orient_matrix_UB_12      0.0926894000
_diffrn_orient_matrix_UB_13      0.0192892000
_diffrn_orient_matrix_UB_21      0.0591175000
_diffrn_orient_matrix_UB_22      0.0897542000
_diffrn_orient_matrix_UB_23      -0.0456906000
_diffrn_orient_matrix_UB_31      -0.1088984000
_diffrn_orient_matrix_UB_32      -0.0509322000
_diffrn_orient_matrix_UB_33      -0.0455121000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0112
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            49162
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.034
_diffrn_reflns_theta_min         3.862
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2165
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+1.0664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2072
_reflns_number_total             2165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc02601b2.cif
_cod_data_source_block           2
_cod_database_code               7114594
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C26 H41 N2 Ni'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed U12: C1(0) C2(0) C3(0) C6(0) C7(0) C10(0) C12(0) C13(0) C16(0) C18(0)
 N1(0) N2(0) Ni1(0)
 Fixed U23: C1(0) C2(0) C3(0) C6(0) C7(0) C10(0) C12(0) C13(0) C16(0) C18(0)
 N1(0) N2(0) Ni1(0)
 Fixed Uiso: H2(0.028) H3(0.029) H4(0.038) H5(0.033) H6(0.03) H9(0.031)
 H11A(0.05) H11B(0.05) H11C(0.05) H15(0.026) H17A(0.045) H17B(0.045) H17C(0.045)
 Fixed X: H2(0.3765) H3(0.2763) H4(0.4627) H5(0.3591) H6(0.2957) H9(0.5741)
 H11A(0.435) H11B(0.4877) H11C(0.4379) H15(0.1751) H17A(0.307) H17B(0.2455)
 H17C(0.2662)
 Fixed Y: C1(0.25) C2(0.25) H2(0.25) C3(0.25) H3(0.25) H4(0.1366) H5(0.4325)
 C6(0.25) H6(0.25) C7(0.25) H9(0.43) C10(0.25) H11A(0.4757) H11B(0.5421)
 H11C(0.4867) C12(0.25) C13(0.25) H15(0.0698) C16(0.25) H17A(0.0187) H17B(-
 0.0428) H17C(0.0175) C18(0.25) N1(0.25) N2(0.25) Ni1(0.25) H18B(0.25)
 H12A(0.25)
 Fixed Z: H2(0.872) H3(0.777) H4(0.1096) H5(0.1336) H6(0.1551) H9(0.7046)
 H11A(0.5838) H11B(0.6588) H11C(0.7566) H15(0.3061) H17A(0.4436) H17B(0.435)
 H17C(0.5828)
;
_shelx_res_checksum              93627
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'