A novel linkage isomeric pair of mixed ligand Ni(ii) complexes with IM2py-κ2N,O and IM2py-κ2N,N modes in [Ni(acac)(tmen)(IM2py)]+; synthesis and X-ray structure
Tsukahara, Yasunori; Kamatani, Takayuki; Suzuki, Takayoshi; Kaizaki, Sumio; Dalton Transactions  (2003) 1276–; doi:10.1039/b301530k

data_7012814
_publ_section_title
;
 A novel linkage isomeric pair of mixed ligand Ni(ii) complexes with
 IM2py-\k2N,O and IM2py-\k2N,N modes in [Ni(acac)(tmen)(IM2py)]+;
 synthesis and X-ray structure
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              1276
_journal_paper_doi               10.1039/b301530k
_journal_year                    2003
_chemical_formula_moiety
'(Ni (C6 H16 N2) (C5 H7 O2) (C12 H16 N3 O) 1+), (P F6 1-)'
_chemical_formula_sum            'C23 H39 F6 N5 Ni O3 P'
_chemical_formula_weight         637.27
_chemical_name_common
;
(2,5-Dimethyl-2,5-diazahexane)(pentane-2,4-dionato)(2-(2'-
pyridyl)-4,4,5,5-tetramethyl-4,5-dihydro-1H-imidazol-1-oxy)nickel(ii)
Hexafluorophosphate
;
_chemical_name_systematic
; 
(2,5-Dimethyl-2,5-diazahexane)(pentane-2,4-dionato)(2-(2'-pyridyl)-4,4,5,5-
tetramethyl-4,5-dihydro-1H-imidazol-1-oxy)nickel(II) Hexafluorophosphate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.377(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3779(16)
_cell_length_b                   13.3309(18)
_cell_length_c                   16.5597(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.9
_cell_volume                     3041.3(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  SHELXL97
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  AFC5R
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.1475
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7249
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0.26
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Coppens numerical'
_exptl_crystal_colour            green-red
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.2131
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.115
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1560P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.2455
_reflns_number_gt                2677
_reflns_number_total             6986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            b301530k.txt
_cod_data_source_block           kama1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7012814