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_7000435
_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         'C23 H43 Cl N Ni P2, B F4'
_chemical_formula_sum            'C23 H43 B Cl F4 N Ni P2'
_chemical_formula_weight         576.49
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.5826(5)
_cell_angle_beta                 75.8775(6)
_cell_angle_gamma                87.7751(8)
_cell_formula_units_Z            2
_cell_length_a                   8.3356(1)
_cell_length_b                   12.2538(1)
_cell_length_c                   14.6565(2)
_cell_measurement_reflns_used    29114
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     1391.88(3)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'HKL2000, denzox, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34132
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         6356
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.6447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0659
_reflns_number_gt                5719
_reflns_number_total             6356
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            B814806F.txt
_cod_data_source_block           s3897a
_cod_original_cell_volume        1391.89(3)
_cod_database_code               7000435