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_1513901
_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_sum            'C48 H71 B N4 Ni2 O7'
_chemical_formula_weight         944.32
_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                72.14(3)
_cell_angle_beta                 76.146(15)
_cell_angle_gamma                82.73(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9320(14)
_cell_length_b                   13.070(6)
_cell_length_c                   18.723(5)
_cell_measurement_reflns_used    47
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      17.46
_cell_measurement_theta_min      15.04
_cell_volume                     2468.1(14)
_computing_cell_refinement       'MXC (MAC Science) '
_computing_data_collection       'MXC (MAC Science) '
_computing_data_reduction        'MXC (MAC Science) '
_computing_molecular_graphics    Ortep-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir-92 in maxus'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Mac Science MXC3K'
_diffrn_measurement_method       2theta-Omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11818
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
psi-scan (North, Philips & Mathews, 1968)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular Solid'
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         11317
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0859P)^2^+1.7820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1906
_reflns_number_gt                6524
_reflns_number_total             11317
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Complex_3.cif
_cod_data_source_block           NiLpro
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_H-M      'P -1          '
_cod_database_code               1513901