<i>cis</i>-Bis(tricyanomethanido-κ<i>N</i>)[tris(2-aminoethyl)amine-κ^4^<i>N</i>]nickel(II)
Potočňák, Ivan; Lancz, Gábor; R°užička, Aleš; Jäger, Lothar; Acta Crystallographica Section E 63 (2007) m2072–m2073; doi:10.1107/S1600536807031807

data_2214839
_publ_section_title
<i>cis</i>-Bis(tricyanomethanido-\k<i>N</i>)[tris(2-aminoethyl)amine-\k^4^<i>N</i>]nickel(II)
_journal_coeditor_code           RK2024
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2072
_journal_page_last               m2073
_journal_paper_doi               10.1107/S1600536807031807
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni (C4 N3)2 (C6 H18 N4)]'
_chemical_formula_moiety         'C14 H18 N10 Ni'
_chemical_formula_sum            'C14 H18 N10 Ni'
_chemical_formula_weight         385.07
_chemical_name_systematic
;
cis-Bis(tricyanomethanido-\kN)[tris(2-aminoethyl)amine-\k^4^N]nickel(II))
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   14.4376(11)
_cell_length_b                   15.2861(12)
_cell_length_c                   8.0888(6)
_cell_measurement_reflns_used    13020
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1
_cell_volume                     1785.2(2)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
;
COLLECT (Nonius, 1998) and DENZO (Otwinowski & Minor, 1997)
;
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2000)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_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  0.0770
_diffrn_reflns_av_sigmaI/netI    0.0664
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12191
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  0.672
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   'Gaussian integration'
_exptl_absorpt_process_details   '(Coppens, 1970)'
_exptl_crystal_colour            red-violet
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.467
_exptl_crystal_size_mid          0.439
_exptl_crystal_size_min          0.392
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.655
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   -0.005(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.6801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                2761
_reflns_number_total             3504
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2024.cif
_cod_data_source_block           I
_cod_database_code               2214839
_cod_database_fobs_code          2214839