Synthesis and structures of dinickel(II) complexes with a binucleating ligand, N,N'-bis[3-(N,N-dimethyl)aminopropyl]-N,N'-dimethyl-1,3-diamino-2-hydroxypropane (HL1), and investigation of carboxylic acid capture assisted by intramolecular hydrogen bonding
Mochizuki, Katsura; Takahashi, Junpei; Inorganica Chimica Acta 414 (2014) 27–32; doi:10.1016/j.ica.2014.01.031

data_1513904
_publ_section_title
;
 Synthesis and structures of dinickel(II) complexes with a binucleating
 ligand,
 N,N'-bis[3-(N,N-dimethyl)aminopropyl]-N,N'-dimethyl-1,3-diamino-2-hydroxypropane
 (HL1), and investigation of carboxylic acid capture assisted by
 intramolecular hydrogen bonding
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              27
_journal_page_last               32
_journal_paper_doi               10.1016/j.ica.2014.01.031
_journal_volume                  414
_journal_year                    2014
_chemical_formula_moiety         'C21 H44 N3 Ni2 O9, C24 H20 B'
_chemical_formula_sum            'C45 H64 B N3 Ni2 O9'
_chemical_formula_weight         919.23
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                105.908(8)
_cell_angle_beta                 90.358(4)
_cell_angle_gamma                106.792(5)
_cell_formula_units_Z            2
_cell_length_a                   9.981(5)
_cell_length_b                   14.789(8)
_cell_length_c                   16.927(8)
_cell_measurement_reflns_used    6177
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.45
_cell_volume                     2291(2)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r1'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r1'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 13.653
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23177
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             976.00
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.280
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.700
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     544
_refine_ls_number_reflns         10413
_refine_ls_number_restraints     16
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.9158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1269
_reflns_number_gt                9145
_reflns_number_total             10413
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            Complex_6.cif
_cod_data_source_block           NiL3pn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2290.6(19)
_cod_database_code               1513904