#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:47:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179424 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/21/4332164.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332164
loop_
_publ_author_name
'Armentano, Donatella'
'De Munno, Giovanni'
'Guerra, Francesca'
'Julve, Miguel'
'Lloret, Francesc'
_publ_section_title
;
 Ligand Effects on the Structures of Extended Networks of
 Dicyanamide-Containing Transition-Metal Ions
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4626
_journal_page_last               4636
_journal_paper_doi               10.1021/ic060044u
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C16 H8 N8 Ni'
_chemical_formula_weight         371.01
_chemical_name_systematic
; 
 ? 
;
_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                 101.3840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0591(2)
_cell_length_b                   10.9889(2)
_cell_length_c                   14.0219(3)
_cell_measurement_reflns_used    7833
_cell_measurement_temperature    293(2)
_cell_volume                     1519.47(5)
_computing_cell_refinement       'Bruker-Nonius SAINT'
_computing_data_collection       'Bruker-Nonius SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40975
_diffrn_reflns_theta_full        31.72
_diffrn_reflns_theta_max         31.72
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_T_max  0.8396
_exptl_absorpt_correction_T_min  0.6975
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            light-blue
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         5089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0533P)²+0.1845P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                3838
_reflns_number_total             5089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060044usup3.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4332164
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.162006(18) 0.116315(19) 0.736656(12) 0.04251(8) Uani 1 1 d .
N1 N 0.25844(12) -0.04489(12) 0.78973(9) 0.0449(3) Uani 1 1 d .
N2 N 0.34584(12) 0.18491(13) 0.80980(8) 0.0439(3) Uani 1 1 d .
C1 C 0.21276(18) -0.15815(17) 0.77776(13) 0.0552(4) Uani 1 1 d .
H1 H 0.1233 -0.1711 0.7466 0.066 Uiso 1 1 calc R
C2 C 0.2944(2) -0.25903(18) 0.81034(15) 0.0652(5) Uani 1 1 d .
H2 H 0.2592 -0.3373 0.8008 0.078 Uiso 1 1 calc R
C3 C 0.4261(2) -0.24165(19) 0.85622(14) 0.0636(5) Uani 1 1 d .
H3 H 0.4811 -0.3079 0.8786 0.076 Uiso 1 1 calc R
C4 C 0.47745(18) -0.12322(16) 0.86914(12) 0.0521(4) Uani 1 1 d .
C5 C 0.61316(19) -0.0954(2) 0.91730(14) 0.0637(5) Uani 1 1 d .
H5 H 0.6724 -0.1584 0.9406 0.076 Uiso 1 1 calc R
C6 C 0.65646(17) 0.0203(2) 0.92946(13) 0.0650(5) Uani 1 1 d .
H6 H 0.7452 0.0357 0.9611 0.078 Uiso 1 1 calc R
C7 C 0.56916(16) 0.12072(17) 0.89488(12) 0.0533(4) Uani 1 1 d .
C8 C 0.60538(19) 0.2441(2) 0.90836(13) 0.0662(5) Uani 1 1 d .
H8 H 0.6923 0.2651 0.9405 0.079 Uiso 1 1 calc R
C9 C 0.5143(2) 0.3324(2) 0.87467(15) 0.0672(5) Uani 1 1 d .
H9 H 0.5375 0.4140 0.8848 0.081 Uiso 1 1 calc R
C10 C 0.38400(19) 0.29966(17) 0.82410(12) 0.0554(4) Uani 1 1 d .
H10 H 0.3227 0.3609 0.7999 0.066 Uiso 1 1 calc R
C11 C 0.43576(15) 0.09605(15) 0.84590(10) 0.0437(3) Uani 1 1 d .
C12 C 0.38997(14) -0.02731(15) 0.83433(10) 0.0438(3) Uani 1 1 d .
N3 N 0.09272(15) 0.28198(16) 0.66901(10) 0.0602(4) Uani 1 1 d .
C13 C 0.04522(16) 0.30968(17) 0.59050(12) 0.0514(4) Uani 1 1 d .
N4 N -0.02035(16) 0.3407(2) 0.50464(12) 0.0786(5) Uani 1 1 d .
C14 C 0.03786(15) 0.34759(17) 0.42962(11) 0.0483(3) Uani 1 1 d .
N5 N 0.07704(14) 0.35544(14) 0.35840(10) 0.0514(3) Uani 1 1 d .
N6 N 0.25023(16) 0.08624(17) 0.61037(11) 0.0592(4) Uani 1 1 d .
C15 C 0.23086(13) 0.05355(14) 0.53219(11) 0.0428(3) Uani 1 1 d .
N7 N 0.22379(15) 0.0139(2) 0.44434(12) 0.0780(6) Uani 1 1 d .
C16 C 0.10626(16) -0.00705(18) 0.38896(11) 0.0518(4) Uani 1 1 d .
N8 N 0.01081(15) -0.03066(16) 0.33377(11) 0.0609(4) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N8 Ni1 N2 173.99(6) 3_556 .
N8 Ni1 N5 90.98(6) 3_556 4_566
N2 Ni1 N5 90.61(5) . 4_566
N8 Ni1 N1 94.15(6) 3_556 .
N2 Ni1 N1 79.95(5) . .
N5 Ni1 N1 94.10(6) 4_566 .
N8 Ni1 N3 90.35(7) 3_556 .
N2 Ni1 N3 95.29(6) . .
N5 Ni1 N3 95.03(6) 4_566 .
N1 Ni1 N3 169.74(5) . .
N8 Ni1 N6 88.93(6) 3_556 .
N2 Ni1 N6 89.46(5) . .
N5 Ni1 N6 179.78(6) 4_566 .
N1 Ni1 N6 85.70(6) . .
N3 Ni1 N6 85.18(6) . .
C1 N1 C12 118.20(15) . .
C1 N1 Ni1 128.84(11) . .
C12 N1 Ni1 112.64(11) . .
C10 N2 C11 118.48(14) . .
C10 N2 Ni1 128.79(12) . .
C11 N2 Ni1 112.73(10) . .
N1 C1 C2 122.35(17) . .
C3 C2 C1 119.61(18) . .
C2 C3 C4 119.31(18) . .
C12 C4 C3 117.75(16) . .
C12 C4 C5 118.65(17) . .
C3 C4 C5 123.59(17) . .
C6 C5 C4 121.15(17) . .
C5 C6 C7 121.56(16) . .
C8 C7 C11 116.60(17) . .
C8 C7 C6 124.82(16) . .
C11 C7 C6 118.56(17) . .
C9 C8 C7 120.27(16) . .
C8 C9 C10 119.42(19) . .
N2 C10 C9 122.26(19) . .
N2 C11 C7 122.92(16) . .
N2 C11 C12 117.57(13) . .
C7 C11 C12 119.50(15) . .
N1 C12 C4 122.78(16) . .
N1 C12 C11 116.66(14) . .
C4 C12 C11 120.56(14) . .
C13 N3 Ni1 134.19(16) . .
N3 C13 N4 174.11(17) . .
C13 N4 C14 122.45(15) . .
N5 C14 N4 173.51(17) . .
C14 N5 Ni1 173.94(15) . 4_565
C15 N6 Ni1 145.35(14) . .
N6 C15 N7 173.32(17) . .
C15 N7 C16 120.01(15) . .
N8 C16 N7 172.77(18) . .
C16 N8 Ni1 162.45(17) . 3_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N8 2.0508(14) 3_556
Ni1 N2 2.0715(12) .
Ni1 N5 2.0777(14) 4_566
Ni1 N1 2.0851(14) .
Ni1 N3 2.1068(16) .
Ni1 N6 2.1570(15) .
N1 C1 1.326(2) .
N1 C12 1.3610(18) .
N2 C10 1.322(2) .
N2 C11 1.359(2) .
C1 C2 1.402(3) .
C2 C3 1.367(3) .
C3 C4 1.399(3) .
C4 C12 1.398(2) .
C4 C5 1.432(3) .
C5 C6 1.344(3) .
C6 C7 1.433(3) .
C7 C8 1.407(3) .
C7 C11 1.408(2) .
C8 C9 1.354(3) .
C9 C10 1.408(3) .
C11 C12 1.431(2) .
N3 C13 1.151(2) .
C13 N4 1.299(2) .
N4 C14 1.303(2) .
C14 N5 1.147(2) .
N5 Ni1 2.0777(14) 4_565
N6 C15 1.133(2) .
C15 N7 1.295(2) .
N7 C16 1.301(2) .
C16 N8 1.138(2) .
N8 Ni1 2.0508(14) 3_556
