Cationic and neutral NiII complexes containing a non-innocent PNP ligand: formation of alkyl and thiolate species
van der Vlugt, Jarl Ivar; Lutz, Martin; Pidko, Evgeny A.; Vogt, Dieter; Spek, Anthony L.; Dalton Transactions  (2009) 1016–1023; doi:10.1039/b814806f

data_7000433
_publ_section_title
;
 Cationic and neutral NiII complexes containing a non-innocent PNP
 ligand: formation of alkyl and thiolate species
;
_journal_coden_ASTM              DTARAF
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1016
_journal_page_last               1023
_journal_paper_doi               10.1039/b814806f
_journal_year                    2009
_chemical_formula_moiety         'C30 H50 N Ni P2 S, B F4'
_chemical_formula_sum            'C30 H50 B F4 N Ni P2 S'
_chemical_formula_weight         664.23
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                94.763(1)
_cell_angle_beta                 90.893(2)
_cell_angle_gamma                101.983(1)
_cell_formula_units_Z            2
_cell_length_a                   8.7077(2)
_cell_length_b                   11.0192(3)
_cell_length_c                   17.2498(4)
_cell_measurement_reflns_used    21908
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.90
_cell_volume                     1612.58(7)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Pixel15, Twinabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0078
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26222
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.971
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         7366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+1.7924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                6765
_reflns_number_total             7366
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            B814806F.txt
_cod_data_source_block           s4098a
_cod_database_code               7000433