#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:17:28 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180498 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/67/7216767.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_7216767
loop_
_publ_author_name
'Liao, Shengyun'
'Li, Tianhao'
'Tian, Jin-Lei'
'Yang, Linyan'
'Gu, Wen'
'Liu, Xin'
_publ_section_title
;
 Strong Antiferromagnetic Interaction in a 3D Copper-Organic Framework and
 Spin-glass-like Behaviour in a 1D Nickel Compound
;
_journal_name_full               'RSC Advances'
_journal_paper_doi               10.1039/c4ra02942a
_journal_year                    2014
_chemical_formula_sum            'C22 H36 N6 Ni3 O26'
_chemical_formula_weight         976.70
_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                82.523(10)
_cell_angle_beta                 82.286(10)
_cell_angle_gamma                71.561(9)
_cell_formula_units_Z            1
_cell_length_a                   6.958(2)
_cell_length_b                   10.909(4)
_cell_length_c                   11.877(4)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.96992
_cell_measurement_theta_min      6.202400
_cell_volume                     843.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5590
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.771
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5649
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             502
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         2951
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0611P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1298
_reflns_number_gt                2473
_reflns_number_total             2951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra02942a2.cif
_cod_data_source_block           c101124a2
_cod_original_cell_volume        843.9(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7216767
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
Ni1 Ni 0.5000 1.0000 0.5000 0.0244(2) Uani 1 2 d SD
Ni2 Ni 0.5000 0.5000 0.0000 0.0231(2) Uani 1 2 d SD
Ni3 Ni 0.0000 1.0000 1.0000 0.0269(2) Uani 1 2 d SD
O1 O 0.3877(5) 0.8474(3) 0.5239(3) 0.0279(8) Uani 1 1 d .
O9 O 0.8084(5) 0.4076(3) 0.0291(3) 0.0269(7) Uani 1 1 d D
O6 O 0.4561(5) 0.3191(3) 0.0111(3) 0.0277(7) Uani 1 1 d .
O11 O -0.2699(5) 0.9637(4) 1.0230(3) 0.0424(9) Uani 1 1 d D
O2 O 0.1084(5) 0.8960(3) 0.6468(3) 0.0360(9) Uani 1 1 d .
O4 O 0.1197(6) 0.2926(3) 0.7396(3) 0.0382(9) Uani 1 1 d .
O8 O 0.2467(6) 1.1026(3) 0.5950(3) 0.0448(10) Uani 1 1 d D
O10 O -0.0806(6) 1.1297(4) 0.8629(4) 0.0475(10) Uani 1 1 d D
O7 O 0.6706(6) 0.9357(4) 0.6410(3) 0.0419(9) Uani 1 1 d D
O5 O 0.3916(5) 0.1619(3) 0.1356(3) 0.0369(9) Uani 1 1 d .
O3 O 0.0534(5) 0.4544(3) 0.8466(3) 0.0309(8) Uani 1 1 d .
N1 N 0.3263(5) 0.4698(3) 0.3447(3) 0.0204(8) Uani 1 1 d .
N2 N 0.3846(5) 0.5435(3) 0.2551(3) 0.0239(9) Uani 1 1 d .
C1 C 0.2188(6) 0.6923(4) 0.5689(4) 0.0200(9) Uani 1 1 d .
C3 C 0.2725(6) 0.5194(4) 0.4541(4) 0.0208(10) Uani 1 1 d .
N3 N 0.4225(5) 0.4745(3) 0.1688(3) 0.0235(9) Uani 1 1 d .
C2 C 0.2746(7) 0.6437(4) 0.4634(4) 0.0229(10) Uani 1 1 d .
H2 H 0.311(7) 0.688(4) 0.409(4) 0.027 Uiso 1 1 d .
C6 C 0.1605(7) 0.6175(4) 0.6624(4) 0.0228(10) Uani 1 1 d .
H6 H 0.109(7) 0.655(4) 0.738(4) 0.027 Uiso 1 1 d .
C8 C 0.3902(6) 0.3577(4) 0.2015(4) 0.0220(10) Uani 1 1 d .
C4 C 0.2233(7) 0.4418(4) 0.5464(4) 0.0213(10) Uani 1 1 d .
H4 H 0.231(7) 0.364(4) 0.549(4) 0.026 Uiso 1 1 d .
C5 C 0.1669(6) 0.4898(4) 0.6522(4) 0.0200(10) Uani 1 1 d .
C11 C 0.4154(7) 0.2705(4) 0.1109(4) 0.0258(10) Uani 1 1 d .
C7 C 0.3285(7) 0.3546(4) 0.3152(4) 0.0219(10) Uani 1 1 d .
H7 H 0.301(7) 0.288(4) 0.368(4) 0.026 Uiso 1 1 d .
O12 O 0.1128(6) 0.8569(4) 0.8904(3) 0.0405(9) Uani 1 1 d D
C9 C 0.2377(7) 0.8242(4) 0.5804(4) 0.0248(10) Uani 1 1 d .
C10 C 0.1109(6) 0.4056(4) 0.7541(4) 0.0227(10) Uani 1 1 d .
O13 O 0.4578(8) 0.8297(5) 0.1884(6) 0.0946(19) Uani 1 1 d D
H9A H 0.821(8) 0.460(6) 0.072(5) 0.142 Uiso 1 1 d D
H9B H 0.862(8) 0.422(7) -0.038(2) 0.142 Uiso 1 1 d D
H11A H -0.368(6) 0.999(7) 1.071(6) 0.142 Uiso 1 1 d D
H11B H -0.301(6) 0.914(7) 0.985(6) 0.142 Uiso 1 1 d D
H8A H 0.158(9) 1.066(5) 0.625(6) 0.142 Uiso 1 1 d D
H8B H 0.252(7) 1.158(6) 0.638(5) 0.142 Uiso 1 1 d D
H10A H -0.203(4) 1.156(6) 0.848(6) 0.142 Uiso 1 1 d D
H10B H -0.030(9) 1.192(5) 0.847(7) 0.142 Uiso 1 1 d D
H7A H 0.625(5) 0.913(9) 0.707(2) 0.142 Uiso 1 1 d D
H7B H 0.794(4) 0.932(8) 0.640(3) 0.142 Uiso 1 1 d D
H13A H 0.554(8) 0.863(6) 0.187(9) 0.142 Uiso 1 1 d D
H13B H 0.506(11) 0.7478(16) 0.204(9) 0.142 Uiso 1 1 d D
H12A H 0.099(8) 0.877(5) 0.8196(14) 0.045(17) Uiso 1 1 d D
H12B H 0.136(10) 0.7766(19) 0.911(6) 0.08(2) Uiso 1 1 d 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'
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
O1 Ni1 O1 180.000(1) 2_676 .
O1 Ni1 O8 91.35(13) 2_676 .
O1 Ni1 O8 88.65(13) . .
O1 Ni1 O8 88.65(13) 2_676 2_676
O1 Ni1 O8 91.35(13) . 2_676
O8 Ni1 O8 180.000(1) . 2_676
O1 Ni1 O7 93.44(14) 2_676 2_676
O1 Ni1 O7 86.56(14) . 2_676
O8 Ni1 O7 86.63(17) . 2_676
O8 Ni1 O7 93.37(17) 2_676 2_676
O1 Ni1 O7 86.56(14) 2_676 .
O1 Ni1 O7 93.44(14) . .
O8 Ni1 O7 93.37(17) . .
O8 Ni1 O7 86.63(17) 2_676 .
O7 Ni1 O7 180.000(1) 2_676 .
N3 Ni2 N3 180.0(2) 2_665 .
N3 Ni2 O6 100.07(13) 2_665 .
N3 Ni2 O6 79.93(13) . .
N3 Ni2 O6 79.93(13) 2_665 2_665
N3 Ni2 O6 100.07(13) . 2_665
O6 Ni2 O6 180.0 . 2_665
N3 Ni2 O9 91.03(14) 2_665 .
N3 Ni2 O9 88.97(14) . .
O6 Ni2 O9 89.27(12) . .
O6 Ni2 O9 90.73(12) 2_665 .
N3 Ni2 O9 88.97(14) 2_665 2_665
N3 Ni2 O9 91.03(14) . 2_665
O6 Ni2 O9 90.73(12) . 2_665
O6 Ni2 O9 89.27(12) 2_665 2_665
O9 Ni2 O9 180.00(18) . 2_665
O11 Ni3 O11 180.0(3) 2_577 .
O11 Ni3 O10 87.21(16) 2_577 .
O11 Ni3 O10 92.79(16) . .
O11 Ni3 O10 92.79(16) 2_577 2_577
O11 Ni3 O10 87.21(16) . 2_577
O10 Ni3 O10 180.000(1) . 2_577
O11 Ni3 O12 89.82(15) 2_577 .
O11 Ni3 O12 90.18(15) . .
O10 Ni3 O12 88.40(17) . .
O10 Ni3 O12 91.60(17) 2_577 .
O11 Ni3 O12 90.18(15) 2_577 2_577
O11 Ni3 O12 89.82(15) . 2_577
O10 Ni3 O12 91.60(17) . 2_577
O10 Ni3 O12 88.40(17) 2_577 2_577
O12 Ni3 O12 180.00(16) . 2_577
C9 O1 Ni1 134.9(3) . .
C11 O6 Ni2 115.9(3) . .
C7 N1 N2 111.8(4) . .
C7 N1 C3 128.9(4) . .
N2 N1 C3 119.2(3) . .
N3 N2 N1 105.5(3) . .
C2 C1 C6 120.3(4) . .
C2 C1 C9 118.2(4) . .
C6 C1 C9 121.4(4) . .
C4 C3 C2 122.1(4) . .
C4 C3 N1 119.2(4) . .
C2 C3 N1 118.7(4) . .
N2 N3 C8 110.6(4) . .
N2 N3 Ni2 136.6(3) . .
C8 N3 Ni2 112.7(3) . .
C3 C2 C1 118.6(4) . .
C1 C6 C5 120.3(4) . .
C7 C8 N3 107.3(4) . .
C7 C8 C11 135.4(4) . .
N3 C8 C11 117.2(4) . .
C3 C4 C5 119.6(4) . .
C4 C5 C6 119.1(4) . .
C4 C5 C10 120.0(4) . .
C6 C5 C10 120.9(4) . .
O5 C11 O6 125.6(4) . .
O5 C11 C8 120.2(4) . .
O6 C11 C8 114.1(4) . .
N1 C7 C8 104.7(4) . .
O1 C9 O2 126.9(4) . .
O1 C9 C1 114.6(4) . .
O2 C9 C1 118.4(4) . .
O3 C10 O4 124.2(4) . .
O3 C10 C5 117.9(4) . .
O4 C10 C5 117.9(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.026(3) 2_676
Ni1 O1 2.026(3) .
Ni1 O8 2.045(3) .
Ni1 O8 2.045(3) 2_676
Ni1 O7 2.099(4) 2_676
Ni1 O7 2.099(4) .
Ni2 N3 2.011(4) 2_665
Ni2 N3 2.011(4) .
Ni2 O6 2.076(3) .
Ni2 O6 2.076(3) 2_665
Ni2 O9 2.117(3) .
Ni2 O9 2.117(3) 2_665
Ni3 O11 2.016(3) 2_577
Ni3 O11 2.016(3) .
Ni3 O10 2.028(4) .
Ni3 O10 2.028(4) 2_577
Ni3 O12 2.056(4) .
Ni3 O12 2.056(4) 2_577
O1 C9 1.241(5) .
O6 C11 1.267(5) .
O2 C9 1.253(5) .
O4 C10 1.249(5) .
O5 C11 1.241(5) .
O3 C10 1.244(5) .
N1 C7 1.343(5) .
N1 N2 1.345(5) .
N1 C3 1.430(5) .
N2 N3 1.300(5) .
C1 C2 1.383(6) .
C1 C6 1.384(6) .
C1 C9 1.510(6) .
C3 C4 1.370(6) .
C3 C2 1.380(6) .
N3 C8 1.362(5) .
C6 C5 1.400(6) .
C8 C7 1.360(6) .
C8 C11 1.484(6) .
C4 C5 1.385(6) .
C5 C10 1.507(6) .
