#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:47:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179424 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/21/4332161.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_4332161
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            'C18 H12 N8 Ni'
_chemical_formula_weight         399.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.926(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8725(4)
_cell_length_b                   15.3131(7)
_cell_length_c                   12.8028(6)
_cell_measurement_reflns_used    8042
_cell_measurement_temperature    293(2)
_cell_volume                     1735.38(14)
_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 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22425
_diffrn_reflns_theta_full        32.99
_diffrn_reflns_theta_max         32.99
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  0.8754
_exptl_absorpt_correction_T_min  0.6714
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            sky-blue
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallepiped
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.065
_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     244
_refine_ls_number_reflns         6249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0334
_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/[σ²(Fo²)+(0.0633P)²+0.1512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                4776
_reflns_number_total             6249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060044usup11.cif
_cod_data_source_block           2
_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)/n
_cod_database_code               4332161
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.25646(2) 0.967016(11) 0.787918(14) 0.03335(7) Uani 1 1 d .
N1 N 0.44538(14) 0.89959(8) 0.73310(10) 0.0369(3) Uani 1 1 d .
N2 N 0.24652(15) 1.00787(10) 0.62805(10) 0.0404(3) Uani 1 1 d .
C1 C 0.5561(2) 0.85545(11) 0.78509(16) 0.0496(4) Uani 1 1 d .
C2 C 0.6432(3) 0.79420(14) 0.7308(2) 0.0762(7) Uani 1 1 d .
H2 H 0.7193 0.7628 0.7676 0.091 Uiso 1 1 calc R
C3 C 0.6173(3) 0.78102(14) 0.6270(2) 0.0817(8) Uani 1 1 d .
H3 H 0.6731 0.7395 0.5933 0.098 Uiso 1 1 calc R
C4 C 0.5066(2) 0.82972(13) 0.57011(18) 0.0625(6) Uani 1 1 d .
C5 C 0.4792(4) 0.82515(19) 0.4580(2) 0.0891(10) Uani 1 1 d .
H5 H 0.5282 0.7828 0.4207 0.107 Uiso 1 1 calc R
C6 C 0.3834(4) 0.8814(2) 0.4060(2) 0.0893(10) Uani 1 1 d .
H6 H 0.3694 0.8780 0.3335 0.107 Uiso 1 1 calc R
C7 C 0.3035(3) 0.94568(17) 0.46075(15) 0.0664(6) Uani 1 1 d .
C8 C 0.2101(3) 1.0099(2) 0.41073(18) 0.0847(9) Uani 1 1 d .
H8 H 0.1917 1.0093 0.3383 0.102 Uiso 1 1 calc R
C9 C 0.1476(3) 1.0720(2) 0.4683(2) 0.0840(9) Uani 1 1 d .
H9 H 0.0906 1.1161 0.4349 0.101 Uiso 1 1 calc R
C10 C 0.1671(2) 1.07132(14) 0.57777(17) 0.0578(5) Uani 1 1 d .
C11 C 0.3195(2) 0.94774(12) 0.57104(12) 0.0443(4) Uani 1 1 d .
C12 C 0.42386(18) 0.88995(10) 0.62688(13) 0.0427(3) Uani 1 1 d .
C13 C 0.5887(2) 0.87159(15) 0.89963(17) 0.0657(6) Uani 1 1 d .
H13A H 0.5237 0.9170 0.9221 0.099 Uiso 1 1 calc R
H13B H 0.6922 0.8891 0.9125 0.099 Uiso 1 1 calc R
H13C H 0.5710 0.8190 0.9378 0.099 Uiso 1 1 calc R
C14 C 0.1033(3) 1.14542(14) 0.6383(2) 0.0764(7) Uani 1 1 d .
H14A H 0.1300 1.1376 0.7117 0.115 Uiso 1 1 calc R
H14B H -0.0047 1.1462 0.6264 0.115 Uiso 1 1 calc R
H14C H 0.1440 1.1997 0.6155 0.115 Uiso 1 1 calc R
N3 N 0.13266(16) 0.85499(8) 0.73812(11) 0.0442(3) Uani 1 1 d .
C15 C 0.08305(17) 0.79100(9) 0.70480(12) 0.0372(3) Uani 1 1 d .
N4 N 0.01091(19) 0.72332(9) 0.66400(14) 0.0621(5) Uani 1 1 d .
C16 C 0.07491(18) 0.64683(9) 0.66839(12) 0.0394(3) Uani 1 1 d .
N5 N 0.12111(18) 0.57695(8) 0.66894(11) 0.0457(3) Uani 1 1 d .
N6 N 0.05348(19) 1.02360(10) 0.82294(13) 0.0522(4) Uani 1 1 d .
C17 C -0.0604(2) 1.04194(9) 0.85393(13) 0.0411(3) Uani 1 1 d .
N7 N -0.19694(17) 1.06315(12) 0.87682(11) 0.0531(4) Uani 1 1 d .
C18 C -0.22632(18) 1.07069(10) 0.97489(13) 0.0401(3) Uani 1 1 d .
N8 N -0.26388(18) 1.07966(11) 1.05797(11) 0.0506(3) 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
N5 Ni1 N6 92.89(6) 2_556 .
N5 Ni1 N8 92.54(6) 2_556 3_577
N6 Ni1 N8 84.88(6) . 3_577
N5 Ni1 N3 177.97(6) 2_556 .
N6 Ni1 N3 87.89(6) . .
N8 Ni1 N3 89.39(6) 3_577 .
N5 Ni1 N1 94.14(5) 2_556 .
N6 Ni1 N1 171.36(6) . .
N8 Ni1 N1 99.81(6) 3_577 .
N3 Ni1 N1 84.92(5) . .
N5 Ni1 N2 90.23(6) 2_556 .
N6 Ni1 N2 96.04(6) . .
N8 Ni1 N2 177.04(6) 3_577 .
N3 Ni1 N2 87.83(6) . .
N1 Ni1 N2 78.92(5) . .
C1 N1 C12 119.33(14) . .
C1 N1 Ni1 130.66(12) . .
C12 N1 Ni1 108.71(10) . .
C10 N2 C11 119.04(16) . .
C10 N2 Ni1 131.23(14) . .
C11 N2 Ni1 108.94(10) . .
N1 C1 C2 119.7(2) . .
N1 C1 C13 119.51(17) . .
C2 C1 C13 120.76(19) . .
C3 C2 C1 121.1(2) . .
C2 C3 C4 120.02(19) . .
C3 C4 C12 116.9(2) . .
C3 C4 C5 123.9(2) . .
C12 C4 C5 119.1(2) . .
C6 C5 C4 121.1(2) . .
C5 C6 C7 121.0(2) . .
C11 C7 C8 117.1(2) . .
C11 C7 C6 119.2(3) . .
C8 C7 C6 123.7(2) . .
C9 C8 C7 119.7(2) . .
C8 C9 C10 121.0(2) . .
N2 C10 C9 120.8(2) . .
N2 C10 C14 120.21(19) . .
C9 C10 C14 119.0(2) . .
N2 C11 C7 122.10(19) . .
N2 C11 C12 117.57(14) . .
C7 C11 C12 120.16(19) . .
N1 C12 C4 122.71(18) . .
N1 C12 C11 118.02(14) . .
C4 C12 C11 119.14(18) . .
C15 N3 Ni1 170.64(14) . .
N3 C15 N4 172.89(17) . .
C16 N4 C15 119.72(14) . .
N5 C16 N4 174.78(18) . .
C16 N5 Ni1 161.35(14) . 2_546
C17 N6 Ni1 167.54(15) . .
N6 C17 N7 172.71(19) . .
C18 N7 C17 119.15(15) . .
N8 C18 N7 174.26(19) . .
C18 N8 Ni1 147.34(14) . 3_577
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N5 2.0584(14) 2_556
Ni1 N6 2.0750(16) .
Ni1 N8 2.0953(15) 3_577
Ni1 N3 2.1119(13) .
Ni1 N1 2.1282(12) .
Ni1 N2 2.1362(13) .
N1 C1 1.332(2) .
N1 C12 1.368(2) .
N2 C10 1.339(2) .
N2 C11 1.366(2) .
C1 C2 1.426(3) .
C1 C13 1.496(3) .
C2 C3 1.348(4) .
C3 C4 1.398(4) .
C4 C12 1.411(2) .
C4 C5 1.441(4) .
C5 C6 1.353(4) .
C6 C7 1.425(4) .
C7 C11 1.410(2) .
C7 C8 1.411(4) .
C8 C9 1.346(5) .
C9 C10 1.400(3) .
C10 C14 1.506(3) .
C11 C12 1.435(3) .
N3 C15 1.1447(19) .
C15 N4 1.308(2) .
N4 C16 1.301(2) .
C16 N5 1.1457(19) .
N5 Ni1 2.0584(14) 2_546
N6 C17 1.146(2) .
C17 N7 1.307(2) .
N7 C18 1.305(2) .
C18 N8 1.144(2) .
N8 Ni1 2.0953(15) 3_577
