#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:29:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179751 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/47/7004770.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_7004770
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            'C40 H44 N12 Ni4 O18'
_chemical_formula_weight         1215.63
_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                 107.636(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.708(5)
_cell_length_b                   21.503(6)
_cell_length_c                   7.602(2)
_cell_measurement_reflns_used    2165
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.7944
_cell_measurement_theta_min      2.8570
_cell_volume                     2914.4(14)
_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      294(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7058
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    1.344
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2559
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0754P)²+6.7889P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1423
_reflns_number_gt                1879
_reflns_number_total             2559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812402g.txt
_cod_data_source_block           1
_cod_depositor_comments
;
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_sg_symbol_H-M      C2/c
_cod_database_code               7004770
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 -0.5000 0.08943(4) -0.7500 0.0220(3) Uani 1 2 d S . .
Ni2 Ni -0.5000 0.5000 -0.5000 0.0159(2) Uani 1 2 d S . .
O1W O -0.50105(19) 0.07983(18) -1.0222(5) 0.0354(9) Uani 1 1 d . . .
H1 H -0.5383 0.0600 -1.0796 0.043 Uiso 1 1 d R . .
H2 H -0.4702 0.0634 -1.0514 0.043 Uiso 1 1 d R . .
O1 O -0.11341(19) 0.41541(19) -0.3249(5) 0.0405(10) Uani 1 1 d . . .
O2 O -0.1021(2) 0.5201(2) -0.3293(6) 0.0447(10) Uani 1 1 d . . .
O3 O -0.52314(18) 0.41345(14) -0.6279(4) 0.0226(7) Uani 1 1 d . . .
O4 O -0.2972(18) 0.2165(13) -0.348(4) 0.279(13) Uiso 0.50 1 d PD . .
H4B H -0.3001 0.1840 -0.4063 0.419 Uiso 0.50 1 calc PR . .
N1 N -0.3815(2) 0.48701(18) -0.4421(5) 0.0237(9) Uani 1 1 d U . .
N2 N -0.5000 0.1845(3) -0.7500 0.0247(13) Uani 1 2 d SU . .
N3 N -0.5000 0.4525(3) -0.2500 0.0207(12) Uani 1 2 d SU . .
N4 N -0.5000 0.3969(3) -0.2500 0.0371(16) Uani 1 2 d SU . .
N5 N -0.5000 0.3432(4) -0.2500 0.078(3) Uani 1 2 d SU . .
C1 C -0.3375(3) 0.5378(2) -0.4381(7) 0.0288(12) Uani 1 1 d . . .
H1A H -0.3599 0.5769 -0.4572 0.035 Uiso 1 1 calc R . .
C2 C -0.2602(3) 0.5338(2) -0.4066(7) 0.0311(12) Uani 1 1 d . . .
H2A H -0.2321 0.5696 -0.4042 0.037 Uiso 1 1 calc R . .
C3 C -0.2251(3) 0.4754(2) -0.3785(6) 0.0251(11) Uani 1 1 d . . .
C4 C -0.2696(3) 0.4232(2) -0.3815(7) 0.0301(12) Uani 1 1 d . . .
H4A H -0.2484 0.3837 -0.3633 0.036 Uiso 1 1 calc R . .
C5 C -0.3467(3) 0.4312(2) -0.4125(7) 0.0285(12) Uani 1 1 d . . .
H5A H -0.3757 0.3960 -0.4126 0.034 Uiso 1 1 calc R . .
C6 C -0.1400(3) 0.4700(3) -0.3417(7) 0.0305(12) Uani 1 1 d . . .
C7 C -0.5459(3) 0.2176(2) -0.6781(8) 0.0355(13) Uani 1 1 d . . .
H7A H -0.5784 0.1959 -0.6288 0.043 Uiso 1 1 calc R . .
C8 C -0.5472(3) 0.2826(2) -0.6737(8) 0.0356(13) Uani 1 1 d . . .
H8A H -0.5792 0.3032 -0.6205 0.043 Uiso 1 1 calc R . .
C9 C -0.5000 0.3162(3) -0.7500 0.0205(14) Uani 1 2 d S . .
C10 C -0.5000 0.3872(3) -0.7500 0.0192(14) Uani 1 2 d S . .
C11 C -0.3541(16) 0.2161(13) -0.247(4) 0.157(10) Uiso 0.50 1 d P . .
H11A H -0.3456 0.1810 -0.1627 0.188 Uiso 0.50 1 calc PR . .
H11B H -0.4042 0.2125 -0.3332 0.188 Uiso 0.50 1 calc PR . .
C12 C -0.3470(16) 0.2733(14) -0.146(4) 0.172(12) Uiso 0.50 1 d PD . .
H12A H -0.3830 0.2741 -0.0787 0.258 Uiso 0.50 1 calc PR . .
H12B H -0.3558 0.3077 -0.2301 0.258 Uiso 0.50 1 calc PR . .
H12C H -0.2973 0.2763 -0.0607 0.258 Uiso 0.50 1 calc PR . .
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'
O O 0.0106 0.0060 '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 174.1(2) 7_454 8_455 ?
O1 Ni1 N2 92.94(12) 7_454 . ?
O1 Ni1 N2 92.94(12) 8_455 . ?
O1 Ni1 O1W 88.17(14) 7_454 . ?
O1 Ni1 O1W 91.25(14) 8_455 . ?
N2 Ni1 O1W 95.71(11) . . ?
O1 Ni1 O1W 91.25(14) 7_454 2_453 ?
O1 Ni1 O1W 88.17(14) 8_455 2_453 ?
N2 Ni1 O1W 95.71(11) . 2_453 ?
O1W Ni1 O1W 168.6(2) . 2_453 ?
O3 Ni2 O3 180.00(8) 5_464 . ?
O3 Ni2 N1 92.01(14) 5_464 5_464 ?
O3 Ni2 N1 87.99(14) . 5_464 ?
O3 Ni2 N1 87.99(14) 5_464 . ?
O3 Ni2 N1 92.01(14) . . ?
N1 Ni2 N1 180.00(5) 5_464 . ?
O3 Ni2 N3 86.14(15) 5_464 5_464 ?
O3 Ni2 N3 93.86(15) . 5_464 ?
N1 Ni2 N3 91.93(10) 5_464 5_464 ?
N1 Ni2 N3 88.07(10) . 5_464 ?
O3 Ni2 N3 93.86(15) 5_464 . ?
O3 Ni2 N3 86.14(15) . . ?
N1 Ni2 N3 88.07(10) 5_464 . ?
N1 Ni2 N3 91.93(10) . . ?
N3 Ni2 N3 180.000(1) 5_464 . ?
Ni1 O1W H1 109.4 . . ?
Ni1 O1W H2 123.8 . . ?
H1 O1W H2 101.5 . . ?
C6 O1 Ni1 115.0(3) . 7_454 ?
C10 O3 Ni2 132.0(3) . . ?
C11 O4 H4B 109.5 . . ?
C5 N1 C1 116.8(4) . . ?
C5 N1 Ni2 124.4(3) . . ?
C1 N1 Ni2 118.7(3) . . ?
C7 N2 C7 116.6(6) 2_453 . ?
C7 N2 Ni1 121.7(3) 2_453 . ?
C7 N2 Ni1 121.7(3) . . ?
N4 N3 Ni2 118.24(13) . 2_454 ?
N4 N3 Ni2 118.24(13) . . ?
Ni2 N3 Ni2 123.5(3) 2_454 . ?
N5 N4 N3 180.000(1) . . ?
N1 C1 C2 122.8(5) . . ?
N1 C1 H1A 118.6 . . ?
C2 C1 H1A 118.6 . . ?
C1 C2 C3 119.7(5) . . ?
C1 C2 H2A 120.2 . . ?
C3 C2 H2A 120.2 . . ?
C4 C3 C2 118.0(4) . . ?
C4 C3 C6 121.5(5) . . ?
C2 C3 C6 120.6(5) . . ?
C3 C4 C5 118.9(5) . . ?
C3 C4 H4A 120.6 . . ?
C5 C4 H4A 120.6 . . ?
N1 C5 C4 123.8(5) . . ?
N1 C5 H5A 118.1 . . ?
C4 C5 H5A 118.1 . . ?
O1 C6 O2 125.5(5) . . ?
O1 C6 C3 116.4(5) . . ?
O2 C6 C3 118.2(5) . . ?
N2 C7 C8 123.6(5) . . ?
N2 C7 H7A 118.2 . . ?
C8 C7 H7A 118.2 . . ?
C9 C8 C7 119.3(5) . . ?
C9 C8 H8A 120.3 . . ?
C7 C8 H8A 120.3 . . ?
C8 C9 C8 117.6(6) 2_453 . ?
C8 C9 C10 121.2(3) 2_453 . ?
C8 C9 C10 121.2(3) . . ?
O3 C10 O3 127.2(6) . 2_453 ?
O3 C10 C9 116.4(3) . . ?
O3 C10 C9 116.4(3) 2_453 . ?
O4 C11 C12 108(2) . . ?
O4 C11 H11A 110.1 . . ?
C12 C11 H11A 110.1 . . ?
O4 C11 H11B 110.2 . . ?
C12 C11 H11B 110.1 . . ?
H11A C11 H11B 108.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
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 2.026(3) 7_454 ?
Ni1 O1 2.026(3) 8_455 ?
Ni1 N2 2.045(6) . ?
Ni1 O1W 2.073(3) . ?
Ni1 O1W 2.073(3) 2_453 ?
Ni2 O3 2.083(3) 5_464 ?
Ni2 O3 2.083(3) . ?
Ni2 N1 2.144(4) 5_464 ?
Ni2 N1 2.144(4) . ?
Ni2 N3 2.157(3) 5_464 ?
Ni2 N3 2.157(3) . ?
O1W H1 0.8200 . ?
O1W H2 0.7647 . ?
O1 C6 1.266(6) . ?
O1 Ni1 2.026(3) 7_454 ?
O2 C6 1.278(7) . ?
O3 C10 1.270(4) . ?
O4 C11 1.49(3) . ?
O4 H4B 0.8200 . ?
N1 C5 1.352(6) . ?
N1 C1 1.363(6) . ?
N2 C7 1.352(6) 2_453 ?
N2 C7 1.352(6) . ?
N3 N4 1.196(8) . ?
N3 Ni2 2.157(3) 2_454 ?
N4 N5 1.155(9) . ?
C1 C2 1.394(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.403(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.395(7) . ?
C3 C6 1.534(6) . ?
C4 C5 1.401(7) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C7 C8 1.398(7) . ?
C7 H7A 0.9300 . ?
C8 C9 1.397(6) . ?
C8 H8A 0.9300 . ?
C9 C8 1.397(6) 2_453 ?
C9 C10 1.526(9) . ?
C10 O3 1.270(4) 2_453 ?
C11 C12 1.44(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
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 C10 -35(100) 5_464 . . . ?
N1 Ni2 O3 C10 131.5(3) 5_464 . . . ?
N1 Ni2 O3 C10 -48.5(3) . . . . ?
N3 Ni2 O3 C10 39.7(3) 5_464 . . . ?
N3 Ni2 O3 C10 -140.3(3) . . . . ?
O3 Ni2 N1 C5 150.0(4) 5_464 . . . ?
O3 Ni2 N1 C5 -30.0(4) . . . . ?
N1 Ni2 N1 C5 -128(100) 5_464 . . . ?
N3 Ni2 N1 C5 -123.7(4) 5_464 . . . ?
N3 Ni2 N1 C5 56.3(4) . . . . ?
O3 Ni2 N1 C1 -31.4(4) 5_464 . . . ?
O3 Ni2 N1 C1 148.6(4) . . . . ?
N1 Ni2 N1 C1 51(100) 5_464 . . . ?
N3 Ni2 N1 C1 54.9(4) 5_464 . . . ?
N3 Ni2 N1 C1 -125.2(4) . . . . ?
O1 Ni1 N2 C7 42.5(3) 7_454 . . 2_453 ?
O1 Ni1 N2 C7 -137.5(3) 8_455 . . 2_453 ?
O1W Ni1 N2 C7 -45.9(3) . . . 2_453 ?
O1W Ni1 N2 C7 134.1(3) 2_453 . . 2_453 ?
O1 Ni1 N2 C7 -137.5(3) 7_454 . . . ?
O1 Ni1 N2 C7 42.5(3) 8_455 . . . ?
O1W Ni1 N2 C7 134.1(3) . . . . ?
O1W Ni1 N2 C7 -45.9(3) 2_453 . . . ?
O3 Ni2 N3 N4 -168.55(9) 5_464 . . . ?
O3 Ni2 N3 N4 11.45(9) . . . . ?
N1 Ni2 N3 N4 99.56(11) 5_464 . . . ?
N1 Ni2 N3 N4 -80.44(11) . . . . ?
N3 Ni2 N3 N4 -21(100) 5_464 . . . ?
O3 Ni2 N3 Ni2 11.45(9) 5_464 . . 2_454 ?
O3 Ni2 N3 Ni2 -168.55(9) . . . 2_454 ?
N1 Ni2 N3 Ni2 -80.44(11) 5_464 . . 2_454 ?
N1 Ni2 N3 Ni2 99.56(11) . . . 2_454 ?
N3 Ni2 N3 Ni2 159(100) 5_464 . . 2_454 ?
Ni2 N3 N4 N5 0(100) 2_454 . . . ?
Ni2 N3 N4 N5 0(100) . . . . ?
C5 N1 C1 C2 0.5(7) . . . . ?
Ni2 N1 C1 C2 -178.2(4) . . . . ?
N1 C1 C2 C3 0.4(8) . . . . ?
C1 C2 C3 C4 -0.6(7) . . . . ?
C1 C2 C3 C6 -179.4(4) . . . . ?
C2 C3 C4 C5 0.1(7) . . . . ?
C6 C3 C4 C5 178.8(4) . . . . ?
C1 N1 C5 C4 -1.1(7) . . . . ?
Ni2 N1 C5 C4 177.6(4) . . . . ?
C3 C4 C5 N1 0.8(8) . . . . ?
Ni1 O1 C6 O2 5.6(7) 7_454 . . . ?
Ni1 O1 C6 C3 -173.9(3) 7_454 . . . ?
C4 C3 C6 O1 3.9(7) . . . . ?
C2 C3 C6 O1 -177.4(5) . . . . ?
C4 C3 C6 O2 -175.6(5) . . . . ?
C2 C3 C6 O2 3.1(7) . . . . ?
C7 N2 C7 C8 -0.6(4) 2_453 . . . ?
Ni1 N2 C7 C8 179.4(4) . . . . ?
N2 C7 C8 C9 1.2(8) . . . . ?
C7 C8 C9 C8 -0.6(4) . . . 2_453 ?
C7 C8 C9 C10 179.4(4) . . . . ?
Ni2 O3 C10 O3 -26.5(2) . . . 2_453 ?
Ni2 O3 C10 C9 153.5(2) . . . . ?
C8 C9 C10 O3 -156.5(3) 2_453 . . . ?
C8 C9 C10 O3 23.5(3) . . . . ?
C8 C9 C10 O3 23.5(3) 2_453 . . 2_453 ?
C8 C9 C10 O3 -156.5(3) . . . 2_453 ?
