Crystal structure and thermal properties of a square-planar Ni^II^ complex of cyanide and a tricyclic bis-amidine ligand formed <i>in situ</i> under solvothermal conditions
Stolárová, Monika; Černák, Juraj; Tomás, Milagros; Falvello, Larry R.; Acta Crystallographica Section C 69 (2013) 565–568; doi:10.1107/S0108270113010585

data_2018964
_publ_section_title
;
 Crystal structure and thermal properties of a square-planar Ni^II^
 complex of cyanide and a tricyclic bis-amidine ligand formed <i>in
 situ</i> under solvothermal conditions
;
_journal_coeditor_code           KU3094
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              565
_journal_page_last               568
_journal_paper_doi               10.1107/S0108270113010585
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Ni (C N)2 (C10 H16 N4)] , 0.5H2 O'
_chemical_formula_moiety         'C12 H16 N6 Ni, 0.5(H2 O)'
_chemical_formula_sum            'C12 H17 N6 Ni O0.5'
_chemical_formula_weight         312.03
_chemical_name_systematic
'Dicyanido(2,3,4,6,7,9,10,11-octahydropyrimido[2',1':3,4]pyrazino[1,2-<i>a</i>]pyrimidine)nickel(II) hemihydrate'
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.4120(4)
_cell_length_b                   7.1730(2)
_cell_length_c                   17.8858(4)
_cell_measurement_reflns_used    8937
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      28.8415
_cell_measurement_theta_min      4.1199
_cell_volume                     2618.75(11)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42018
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.13
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.288
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0357P)^2^+3.9675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                2304
_reflns_number_total             2994
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ku3094.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C12 H17 N6 Ni O0.50'
_cod_database_code               2018964
_cod_database_fobs_code          2018964