Crystal structure, configurational and density functional theory analysis of nickel(II) complexes with pentadentate 1,3-pd3a-type ligands
Svetlana Belosevic; Marina Cendic; Maja Djukic; Miorad Vasojevic; Auke Meetsma; Zoran D. Matovic; Inorganica Chimica Acta 399 (2013) 146–153; doi:

data_1516874
_publ_section_title
;
 Crystal structure, configurational and density functional theory analysis
 of nickel(II) complexes with pentadentate 1,3-pd3a-type ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              146
_journal_page_last               153
_journal_volume                  399
_journal_year                    2013
_chemical_compound_source        'see text'
_chemical_formula_moiety         'K , C9 H15 N2 Ni O7, 3(H2 O)'
_chemical_formula_sum            'C9 H21 K N2 Ni O10'
_chemical_formula_weight         415.06
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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   direct
_cell_angle_alpha                86.982(1)
_cell_angle_beta                 78.640(1)
_cell_angle_gamma                63.532(1)
_cell_formula_units_Z            2
_cell_length_a                   7.2681(5)
_cell_length_b                   7.9578(6)
_cell_length_c                   15.377(1)
_cell_measurement_reflns_used    5929
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      29.70
_cell_measurement_theta_min      2.70
_cell_volume                     779.93(9)
_computing_cell_refinement       'SAINTPLUS, (Bruker, 2001)'
_computing_data_collection       'SMART,(Bruker, 2001)'
_computing_data_reduction        'XPREP, (Bruker, 2001)'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 2005) 
 PLATON (Spek, 2003)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 SIR2004 (Burla et al., 2005)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type
;
  Bruker Smart Apex; CCD area detector 
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_detector
;
  CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0122
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7144
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001)
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.564
_exptl_absorpt_correction_T_max  0.5406
_exptl_absorpt_correction_T_min  0.4894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, (Bruker, 2001))'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.7492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0626
_reflns_number_gt                3596
_reflns_number_total             3710
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ICA-2013-399-146-153.cif
_cod_data_source_block           Q1087
_cod_database_code               1516874