Bis(dicyanamido-κ<i>N</i>)[tris(3-aminopropyl)amine-κ^4^<i>N</i>]nickel(II)
Luo, Jun; Zhang, Xin-Rong; Qiu, Li-Juan; Yang, Feng; Liu, Bao-Shu; Acta Crystallographica Section E 69 (2013) m385–m386; doi:10.1107/S1600536813015651

data_2238127
_publ_section_title
;
 Bis(dicyanamido-\k<i>N</i>)[tris(3-aminopropyl)amine-\k^4^<i>N</i>]nickel(II)
;
_journal_coeditor_code           BG2508
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m385
_journal_page_last               m386
_journal_paper_doi               10.1107/S1600536813015651
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Ni (C2 N3)2 (C9 H24 N4)]'
_chemical_formula_moiety         'C13 H24 N10 Ni'
_chemical_formula_sum            'C13 H24 N10 Ni'
_chemical_formula_weight         379.13
_chemical_name_systematic
;
Bis(dicyanamido-\k<i>N</i>)[tris(3-aminopropyl)amine-\k^4^<i>N</i>]nickel(II)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 105.660(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1710(10)
_cell_length_b                   11.3960(11)
_cell_length_c                   15.5305(15)
_cell_measurement_reflns_used    5066
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      2.25
_cell_volume                     1733.3(3)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART  (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12722
_diffrn_reflns_theta_full        27.75
_diffrn_reflns_theta_max         27.75
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        3.85
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_T_max  0.9453
_exptl_absorpt_correction_T_min  0.8301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4056
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.0784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0789
_reflns_number_gt                3403
_reflns_number_total             4056
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg2508.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2238127
_cod_database_fobs_code          2238127