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_1513899
_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            'C45 H65 B N4 Ni2 O7'
_chemical_formula_weight         902.24
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.47(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.569(10)
_cell_length_b                   9.687(4)
_cell_length_c                   33.624(4)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      14.85
_cell_measurement_theta_min      13.15
_cell_volume                     4551(4)
_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    'DIRdif in MAXUS'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Mac Science MXCk3'
_diffrn_measurement_method       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  0.1677
_diffrn_reflns_av_sigmaI/netI    0.1066
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            10631
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        15.305
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
psi-scan (North, Philips & Mathews, 1968)
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         10451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1769
_refine_ls_R_factor_gt           0.0840
_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^)+(0.1076P)^2^+12.7044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2161
_refine_ls_wR_factor_ref         0.2752
_reflns_number_gt                5113
_reflns_number_total             10451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Complex_1.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Psi-Scan'
changed to 'psi-scan' 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 21/c'
_cod_database_code               1513899