#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:29:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179751 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/47/7004771.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_7004771
loop_
_publ_author_name
'Hu, Bo-Wen'
'Zhao, Jiong-Peng'
'Sañudo, E. C.'
'Liu, Fu-Chen'
'Zeng, Yong-Fei'
'Bu, Xian-He'
_publ_section_title
;
 Nickel(ii)--azido ferromagnetic chains in a 3D porous metal--organic
 framework with breathing guest molecules
;
_journal_issue                   41
_journal_name_full               'Dalton Transactions'
_journal_page_first              5556
_journal_page_last               5559
_journal_paper_doi               10.1039/b812402g
_journal_year                    2008
_chemical_formula_sum            'C9 H8 N3 Ni O4'
_chemical_formula_weight         280.89
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.502(4)
_cell_length_b                   21.177(4)
_cell_length_c                   7.4933(15)
_cell_measurement_temperature    293(2)
_cell_volume                     2801.8(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω 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  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14484
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0437
_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)+(0.0427P)²+5.1793P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                2796
_reflns_number_total             3210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812402g.txt
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2801.8(10)
_cod_original_sg_symbol_H-M      'C2/c '
_cod_database_code               7004771
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.41123(2) 0.2500 0.02076(15) Uani 1 2 d S . .
Ni2 Ni 0.5000 0.5000 0.5000 0.01539(14) Uani 1 2 d S . .
O3 O 0.47742(12) 0.58685(8) 0.3736(3) 0.0230(4) Uani 1 1 d . . .
N1 N 0.38119(13) 0.48736(11) 0.4413(3) 0.0223(5) Uani 1 1 d . . .
C4 C 0.26964(17) 0.42362(14) 0.3848(5) 0.0310(7) Uani 1 1 d . . .
H4A H 0.2482 0.3835 0.3690 0.037 Uiso 1 1 calc R . .
O1W O -0.00096(16) 0.42108(12) -0.0209(4) 0.0334(5) Uani 1 1 d . . .
C3 C 0.22475(16) 0.47667(15) 0.3782(4) 0.0250(6) Uani 1 1 d . . .
C5 C 0.34668(17) 0.43127(14) 0.4153(5) 0.0290(7) Uani 1 1 d . . .
H5A H 0.3760 0.3954 0.4177 0.035 Uiso 1 1 calc R . .
C6 C 0.14037(17) 0.47145(16) 0.3413(4) 0.0309(7) Uani 1 1 d . . .
O2 O 0.10234(13) 0.52113(12) 0.3293(4) 0.0424(6) Uani 1 1 d . . .
C2 C 0.25985(17) 0.53453(15) 0.4043(5) 0.0312(7) Uani 1 1 d . . .
H2A H 0.2317 0.5712 0.4007 0.037 Uiso 1 1 calc R . .
C1 C 0.33757(17) 0.53796(14) 0.4362(5) 0.0300(7) Uani 1 1 d . . .
H1A H 0.3604 0.5775 0.4548 0.036 Uiso 1 1 calc R . .
O1 O 0.11306(13) 0.41619(12) 0.3239(4) 0.0408(6) Uani 1 1 d . . .
N3 N 0.5000 0.54645(15) 0.7500 0.0206(7) Uani 1 2 d S . .
N4 N 0.5000 0.60234(18) 0.7500 0.0487(13) Uani 1 2 d S . .
N5 N 0.5000 0.6563(2) 0.7500 0.142(4) Uani 1 2 d S . .
C11 C 0.5000 0.61314(17) 0.2500 0.0176(7) Uani 1 2 d S . .
C9 C 0.5000 0.68426(17) 0.2500 0.0215(8) Uani 1 2 d S . .
N2 N 0.5000 0.81582(15) 0.2500 0.0245(7) Uani 1 2 d S . .
C10 C 0.5430(2) 0.78302(15) 0.1679(6) 0.0436(10) Uani 1 1 d . . .
H10A H 0.572(2) 0.8089(19) 0.116(6) 0.052 Uiso 1 1 d . . .
H1WB H 0.035(2) 0.441(2) -0.060(6) 0.054(12) Uiso 1 1 d . . .
H1WA H -0.033(2) 0.430(2) -0.092(6) 0.041(13) Uiso 1 1 d . . .
C8 C 0.5441(2) 0.71804(14) 0.1632(6) 0.0412(9) Uani 1 1 d . . .
H8A H 0.5742 0.6971 0.1024 0.049 Uiso 1 1 calc R . .
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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
O1 Ni1 O1 173.98(14) 2 . ?
O1 Ni1 N2 93.01(7) 2 3_445 ?
O1 Ni1 N2 93.01(7) . 3_445 ?
O1 Ni1 O1W 88.14(11) 2 2 ?
O1 Ni1 O1W 91.25(11) . 2 ?
N2 Ni1 O1W 95.88(7) 3_445 2 ?
O1 Ni1 O1W 91.25(11) 2 . ?
O1 Ni1 O1W 88.14(11) . . ?
N2 Ni1 O1W 95.88(7) 3_445 . ?
O1W Ni1 O1W 168.24(15) 2 . ?
O3 Ni2 O3 180.000(1) 5_666 . ?
O3 Ni2 N3 86.46(9) 5_666 5_666 ?
O3 Ni2 N3 93.54(9) . 5_666 ?
O3 Ni2 N3 93.54(9) 5_666 . ?
O3 Ni2 N3 86.46(9) . . ?
N3 Ni2 N3 180.0 5_666 . ?
O3 Ni2 N1 92.16(9) 5_666 . ?
O3 Ni2 N1 87.84(9) . . ?
N3 Ni2 N1 91.83(7) 5_666 . ?
N3 Ni2 N1 88.17(7) . . ?
O3 Ni2 N1 87.84(9) 5_666 5_666 ?
O3 Ni2 N1 92.16(9) . 5_666 ?
N3 Ni2 N1 88.17(7) 5_666 5_666 ?
N3 Ni2 N1 91.83(7) . 5_666 ?
N1 Ni2 N1 180.00(3) . 5_666 ?
C11 O3 Ni2 132.18(19) . . ?
C5 N1 C1 116.8(3) . . ?
C5 N1 Ni2 124.2(2) . . ?
C1 N1 Ni2 118.93(19) . . ?
C5 C4 C3 119.1(3) . . ?
C5 C4 H4A 120.4 . . ?
C3 C4 H4A 120.4 . . ?
Ni1 O1W H1WB 125(3) . . ?
Ni1 O1W H1WA 123(3) . . ?
H1WB O1W H1WA 99(4) . . ?
C2 C3 C4 117.7(3) . . ?
C2 C3 C6 120.8(3) . . ?
C4 C3 C6 121.5(3) . . ?
N1 C5 C4 123.5(3) . . ?
N1 C5 H5A 118.2 . . ?
C4 C5 H5A 118.2 . . ?
O2 C6 O1 124.8(3) . . ?
O2 C6 C3 118.7(3) . . ?
O1 C6 C3 116.5(3) . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
N1 C1 C2 123.3(3) . . ?
N1 C1 H1A 118.3 . . ?
C2 C1 H1A 118.3 . . ?
C6 O1 Ni1 115.4(2) . . ?
N4 N3 Ni2 117.70(8) . . ?
N4 N3 Ni2 117.70(8) . 2_656 ?
Ni2 N3 Ni2 124.60(15) . 2_656 ?
N5 N4 N3 180.000(1) . . ?
O3 C11 O3 127.3(3) . 2_655 ?
O3 C11 C9 116.36(17) . . ?
O3 C11 C9 116.36(17) 2_655 . ?
C8 C9 C8 117.8(4) 2_655 . ?
C8 C9 C11 121.08(18) 2_655 . ?
C8 C9 C11 121.08(18) . . ?
C10 N2 C10 117.4(4) 2_655 . ?
C10 N2 Ni1 121.32(18) 2_655 3 ?
C10 N2 Ni1 121.32(18) . 3 ?
N2 C10 C8 123.2(3) . . ?
N2 C10 H10A 113(2) . . ?
C8 C10 H10A 124(2) . . ?
C10 C8 C9 119.2(3) . . ?
C10 C8 H8A 120.4 . . ?
C9 C8 H8A 120.4 . . ?
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 O1 2.000(2) 2 ?
Ni1 O1 2.000(2) . ?
Ni1 N2 2.020(3) 3_445 ?
Ni1 O1W 2.035(2) 2 ?
Ni1 O1W 2.035(2) . ?
Ni2 O3 2.0537(18) 5_666 ?
Ni2 O3 2.0537(18) . ?
Ni2 N3 2.1159(15) 5_666 ?
Ni2 N3 2.1159(15) . ?
Ni2 N1 2.126(2) . ?
Ni2 N1 2.126(2) 5_666 ?
O3 C11 1.254(2) . ?
N1 C5 1.335(4) . ?
N1 C1 1.335(4) . ?
C4 C5 1.384(4) . ?
C4 C3 1.389(4) . ?
C4 H4A 0.9300 . ?
O1W H1WB 0.92(4) . ?
O1W H1WA 0.70(4) . ?
C3 C2 1.373(4) . ?
C3 C6 1.506(4) . ?
C5 H5A 0.9300 . ?
C6 O2 1.254(4) . ?
C6 O1 1.266(4) . ?
C2 C1 1.387(4) . ?
C2 H2A 0.9300 . ?
C1 H1A 0.9300 . ?
N3 N4 1.184(5) . ?
N3 Ni2 2.1159(15) 2_656 ?
N4 N5 1.142(6) . ?
C11 O3 1.254(2) 2_655 ?
C11 C9 1.506(5) . ?
C9 C8 1.385(4) 2_655 ?
C9 C8 1.385(4) . ?
N2 C10 1.336(4) 2_655 ?
N2 C10 1.336(4) . ?
N2 Ni1 2.020(3) 3 ?
C10 C8 1.377(4) . ?
C10 H10A 0.93(4) . ?
C8 H8A 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Ni2 O3 C11 36(11) 5_666 . . . ?
N3 Ni2 O3 C11 -38.8(2) 5_666 . . . ?
N3 Ni2 O3 C11 141.2(2) . . . . ?
N1 Ni2 O3 C11 -130.5(2) . . . . ?
N1 Ni2 O3 C11 49.5(2) 5_666 . . . ?
O3 Ni2 N1 C5 -28.2(2) 5_666 . . . ?
O3 Ni2 N1 C5 151.8(2) . . . . ?
N3 Ni2 N1 C5 58.3(3) 5_666 . . . ?
N3 Ni2 N1 C5 -121.7(3) . . . . ?
N1 Ni2 N1 C5 113(100) 5_666 . . . ?
O3 Ni2 N1 C1 149.3(2) 5_666 . . . ?
O3 Ni2 N1 C1 -30.7(2) . . . . ?
N3 Ni2 N1 C1 -124.2(2) 5_666 . . . ?
N3 Ni2 N1 C1 55.8(2) . . . . ?
N1 Ni2 N1 C1 -70(100) 5_666 . . . ?
C5 C4 C3 C2 -0.6(5) . . . . ?
C5 C4 C3 C6 178.6(3) . . . . ?
C1 N1 C5 C4 -0.3(5) . . . . ?
Ni2 N1 C5 C4 177.2(2) . . . . ?
C3 C4 C5 N1 0.8(5) . . . . ?
C2 C3 C6 O2 2.1(4) . . . . ?
C4 C3 C6 O2 -177.1(3) . . . . ?
C2 C3 C6 O1 -178.2(3) . . . . ?
C4 C3 C6 O1 2.6(4) . . . . ?
C4 C3 C2 C1 -0.1(5) . . . . ?
C6 C3 C2 C1 -179.3(3) . . . . ?
C5 N1 C1 C2 -0.4(5) . . . . ?
Ni2 N1 C1 C2 -178.1(2) . . . . ?
C3 C2 C1 N1 0.6(5) . . . . ?
O2 C6 O1 Ni1 5.5(4) . . . . ?
C3 C6 O1 Ni1 -174.16(19) . . . . ?
O1 Ni1 O1 C6 -0.2(2) 2 . . . ?
N2 Ni1 O1 C6 179.8(2) 3_445 . . . ?
O1W Ni1 O1 C6 -84.2(2) 2 . . . ?
O1W Ni1 O1 C6 84.0(2) . . . . ?
O3 Ni2 N3 N4 168.79(6) 5_666 . . . ?
O3 Ni2 N3 N4 -11.21(6) . . . . ?
N3 Ni2 N3 N4 -98(100) 5_666 . . . ?
N1 Ni2 N3 N4 -99.16(7) . . . . ?
N1 Ni2 N3 N4 80.84(7) 5_666 . . . ?
O3 Ni2 N3 Ni2 -11.21(6) 5_666 . . 2_656 ?
O3 Ni2 N3 Ni2 168.79(6) . . . 2_656 ?
N3 Ni2 N3 Ni2 82(100) 5_666 . . 2_656 ?
N1 Ni2 N3 Ni2 80.84(7) . . . 2_656 ?
N1 Ni2 N3 Ni2 -99.16(7) 5_666 . . 2_656 ?
Ni2 N3 N4 N5 107(100) . . . . ?
Ni2 N3 N4 N5 -73(100) 2_656 . . . ?
Ni2 O3 C11 O3 25.88(14) . . . 2_655 ?
Ni2 O3 C11 C9 -154.12(14) . . . . ?
O3 C11 C9 C8 -20.3(2) . . . 2_655 ?
O3 C11 C9 C8 159.7(2) 2_655 . . 2_655 ?
O3 C11 C9 C8 159.7(2) . . . . ?
O3 C11 C9 C8 -20.3(2) 2_655 . . . ?
C10 N2 C10 C8 0.6(3) 2_655 . . . ?
Ni1 N2 C10 C8 -179.4(3) 3 . . . ?
N2 C10 C8 C9 -1.2(6) . . . . ?
C8 C9 C8 C10 0.6(3) 2_655 . . . ?
C11 C9 C8 C10 -179.4(3) . . . . ?
