#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:33:06 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179066 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/28/4302819.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4302819
loop_
_publ_author_name
'Ru-Yin Li'
'Bing-Wu Wang'
'Xin-Yi Wang'
'Xiu-Teng Wang'
'Zhe-Ming Wang'
'Song Gao'
_publ_section_title
;
Two EE-Azido-Bridged Nickel(II) Layered Compounds: Vigorous Twisted Torsion
Angle Ni-N3-Ni Results in Ferromagnetic Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7174
_journal_page_last               7180
_journal_paper_doi               10.1021/ic9003092
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C4 H6 N14 Ni'
_chemical_formula_weight         308.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.70(3)
_cell_angle_beta                 87.86(3)
_cell_angle_gamma                70.23(3)
_cell_formula_units_Z            2
_cell_length_a                   6.5631(13)
_cell_length_b                   9.0899(18)
_cell_length_c                   9.4638(19)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.75
_cell_volume                     511.6(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'NONIUS KappaCCD Diffractometer'
_diffrn_measurement_method       CCD
_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  0.0745
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10254
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.75
_exptl_absorpt_coefficient_mu    1.913
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0312
_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/[σ²(Fo²)+(0.0334P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0684
_reflns_number_gt                1706
_reflns_number_total             2349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9003092_si_001_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        511.65(18)
_cod_database_code               4302819
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.0000 0.0000 0.02340(12) Uani 1 2 d S . .
Ni2 Ni 0.5000 0.0000 -0.5000 0.02416(13) Uani 1 2 d S . .
N2 N 0.2321(3) 0.1119(2) -0.7859(2) 0.0261(4) Uani 1 1 d . . .
N5 N 0.1926(3) 0.1142(2) -0.2880(2) 0.0274(4) Uani 1 1 d . . .
N14 N 0.5879(3) -0.3879(2) 0.1300(2) 0.0247(4) Uani 1 1 d . . .
N7 N 0.3653(3) -0.1784(2) -0.4881(2) 0.0286(4) Uani 1 1 d . . .
N11 N 0.2711(3) -0.2100(2) 0.0650(2) 0.0262(4) Uani 1 1 d . . .
N3 N 0.3717(3) 0.1186(2) -0.7168(2) 0.0343(5) Uani 1 1 d . . .
N10 N 0.2181(3) -0.3606(2) -0.4087(2) 0.0267(4) Uani 1 1 d . . .
N9 N 0.2828(3) -0.3691(3) -0.5437(2) 0.0392(5) Uani 1 1 d . . .
C4 C 0.4788(3) -0.2311(3) 0.0791(2) 0.0263(5) Uani 1 1 d . . .
H4 H 0.538(3) -0.153(3) 0.062(2) 0.017(5) Uiso 1 1 d . . .
C3 C 0.8212(3) -0.4755(3) 0.1623(3) 0.0272(5) Uani 1 1 d . . .
H3A H 0.887(4) -0.400(3) 0.112(3) 0.033(7) Uiso 1 1 d . . .
H3B H 0.855(3) -0.565(3) 0.125(2) 0.024(6) Uiso 1 1 d . . .
N8 N 0.3716(3) -0.2596(3) -0.5910(2) 0.0397(5) Uani 1 1 d . . .
N4 N 0.2148(3) 0.1329(3) -0.4145(2) 0.0348(5) Uani 1 1 d . . .
N13 N 0.4455(3) -0.4685(2) 0.1478(2) 0.0318(5) Uani 1 1 d . . .
N12 N 0.2555(3) -0.3604(2) 0.1091(2) 0.0318(5) Uani 1 1 d . . .
N6 N 0.1732(3) 0.1018(2) -0.1609(2) 0.0340(5) Uani 1 1 d . . .
C1 C 0.2687(4) -0.2427(3) -0.3778(3) 0.0305(5) Uani 1 1 d . . .
H1 H 0.243(4) -0.216(3) -0.291(3) 0.050(8) Uiso 1 1 d . . .
C2 C 0.1132(4) -0.4721(3) -0.3232(3) 0.0309(5) Uani 1 1 d . . .
H2A H 0.162(4) -0.566(3) -0.368(3) 0.036(7) Uiso 1 1 d . . .
H2B H -0.039(4) -0.420(3) -0.334(2) 0.028(6) Uiso 1 1 d . . .
N1 N 0.0874(3) 0.1159(3) 0.1425(2) 0.0376(5) 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
Ni Ni 0.3393 1.1124 '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'
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'
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
_geom_angle_publ_flag
N6 Ni1 N6 180.00(17) 2 . ?
N6 Ni1 N11 89.80(8) 2 . ?
N6 Ni1 N11 90.20(8) . . ?
N6 Ni1 N11 90.20(8) 2 2 ?
N6 Ni1 N11 89.80(8) . 2 ?
N11 Ni1 N11 180.00(14) . 2 ?
N6 Ni1 N1 91.14(8) 2 . ?
N6 Ni1 N1 88.86(8) . . ?
N11 Ni1 N1 93.94(8) . . ?
N11 Ni1 N1 86.06(8) 2 . ?
N6 Ni1 N1 88.86(8) 2 2 ?
N6 Ni1 N1 91.14(8) . 2 ?
N11 Ni1 N1 86.06(8) . 2 ?
N11 Ni1 N1 93.94(8) 2 2 ?
N1 Ni1 N1 180.00(7) . 2 ?
N7 Ni2 N7 180.0 . 2_654 ?
N7 Ni2 N3 88.41(8) . 2_654 ?
N7 Ni2 N3 91.59(8) 2_654 2_654 ?
N7 Ni2 N3 91.59(8) . . ?
N7 Ni2 N3 88.41(8) 2_654 . ?
N3 Ni2 N3 180.0 2_654 . ?
N7 Ni2 N4 88.59(8) . . ?
N7 Ni2 N4 91.41(8) 2_654 . ?
N3 Ni2 N4 88.54(8) 2_654 . ?
N3 Ni2 N4 91.46(8) . . ?
N7 Ni2 N4 91.41(8) . 2_654 ?
N7 Ni2 N4 88.59(8) 2_654 2_654 ?
N3 Ni2 N4 91.46(8) 2_654 2_654 ?
N3 Ni2 N4 88.54(8) . 2_654 ?
N4 Ni2 N4 180.0 . 2_654 ?
N1 N2 N3 175.7(2) 1_554 . ?
N4 N5 N6 176.8(2) . . ?
C4 N14 N13 108.29(17) . . ?
C4 N14 C3 130.8(2) . . ?
N13 N14 C3 120.94(18) . . ?
C1 N7 N8 105.98(19) . . ?
C1 N7 Ni2 127.43(16) . . ?
N8 N7 Ni2 126.47(15) . . ?
C4 N11 N12 106.00(17) . . ?
C4 N11 Ni1 131.49(16) . . ?
N12 N11 Ni1 122.45(13) . . ?
N2 N3 Ni2 132.58(17) . . ?
C1 N10 N9 107.9(2) . . ?
C1 N10 C2 131.5(2) . . ?
N9 N10 C2 120.61(19) . . ?
N8 N9 N10 107.03(18) . . ?
N11 C4 N14 108.9(2) . . ?
N11 C4 H4 126.3(13) . . ?
N14 C4 H4 124.7(13) . . ?
N14 C3 C2 113.38(19) . 2_645 ?
N14 C3 H3A 104.2(13) . . ?
C2 C3 H3A 109.7(14) 2_645 . ?
N14 C3 H3B 106.5(13) . . ?
C2 C3 H3B 110.6(14) 2_645 . ?
H3A C3 H3B 112.3(19) . . ?
N9 N8 N7 109.83(19) . . ?
N5 N4 Ni2 122.62(16) . . ?
N12 N13 N14 106.66(17) . . ?
N13 N12 N11 110.14(17) . . ?
N5 N6 Ni1 135.99(17) . . ?
N7 C1 N10 109.2(2) . . ?
N7 C1 H1 126.9(18) . . ?
N10 C1 H1 123.9(18) . . ?
N10 C2 C3 112.58(19) . 2_645 ?
N10 C2 H2A 103.4(14) . . ?
C3 C2 H2A 111.7(14) 2_645 . ?
N10 C2 H2B 109.3(14) . . ?
C3 C2 H2B 108.0(14) 2_645 . ?
H2A C2 H2B 111.8(19) . . ?
N2 N1 Ni1 143.32(16) 1_556 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N6 2.075(2) 2 ?
Ni1 N6 2.075(2) . ?
Ni1 N11 2.0860(19) . ?
Ni1 N11 2.0861(19) 2 ?
Ni1 N1 2.115(2) . ?
Ni1 N1 2.115(2) 2 ?
Ni2 N7 2.0713(19) . ?
Ni2 N7 2.0713(19) 2_654 ?
Ni2 N3 2.104(2) 2_654 ?
Ni2 N3 2.104(2) . ?
Ni2 N4 2.119(2) . ?
Ni2 N4 2.119(2) 2_654 ?
N2 N1 1.172(3) 1_554 ?
N2 N3 1.172(2) . ?
N5 N4 1.175(3) . ?
N5 N6 1.184(3) . ?
N14 C4 1.322(3) . ?
N14 N13 1.351(3) . ?
N14 C3 1.468(3) . ?
N7 C1 1.309(3) . ?
N7 N8 1.361(3) . ?
N11 C4 1.317(3) . ?
N11 N12 1.358(3) . ?
N10 C1 1.326(3) . ?
N10 N9 1.345(3) . ?
N10 C2 1.467(3) . ?
N9 N8 1.292(3) . ?
C4 H4 0.90(2) . ?
C3 C2 1.503(3) 2_645 ?
C3 H3A 0.94(3) . ?
C3 H3B 0.93(2) . ?
N13 N12 1.293(3) . ?
C1 H1 0.91(3) . ?
C2 C3 1.503(3) 2_645 ?
C2 H2A 1.01(2) . ?
C2 H2B 0.94(2) . ?
N1 N2 1.172(3) 1_556 ?
