#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:50:11 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178965 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/94/4119456.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_4119456
loop_
_publ_author_name
'Mario Wriedt'
'Andrey A. Yakovenko'
'Gregory J. Halder'
'Andrey V. Prosvirin'
'Kim R. Dunbar'
'Hong-Cai Zhou'
_publ_section_title
;
 Reversible Switching from Antiferro- to Ferromagnetic Behavior by
 Solvent-Mediated, Thermally-Induced Phase Transitions in a Trimorphic
 MOF-Based Magnetic Sponge System
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4040
_journal_page_last               4050
_journal_paper_doi               10.1021/ja312347p
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C15 H14 Cu N6 O2'
_chemical_formula_sum            'C15 H14 Cu N6 O2'
_chemical_formula_weight         373.86
_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                 108.276(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.529(9)
_cell_length_b                   10.884(4)
_cell_length_c                   19.479(7)
_cell_measurement_reflns_used    3768
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.18
_cell_measurement_theta_min      2.20
_cell_volume                     3931(3)
_computing_cell_refinement       'SAINT+ ver. (Bruker, 2001)'
_computing_data_collection       'APEX2  (Bruker, 2008)'
_computing_data_reduction        'SAINT+ ver. (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX II 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  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21459
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_T_max  0.8058
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       prism
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4265
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0394
_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)+(0.0300P)²+4.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                3292
_reflns_number_total             4265
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja312347p_si_003.cif
_cod_data_source_block           mw71_sq
_cod_original_cell_volume        3932(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4119456
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_group
Cu1 Cu 0.0000 0.0000 0.0000 0.03646(14) Uani 1 2 d S .
Cu2 Cu 0.2500 0.2500 0.0000 0.02762(12) Uani 1 2 d S .
O1 O -0.02677(10) -0.1842(3) 0.03516(14) 0.0367(6) Uani 0.75 1 d PD 1
O2 O -0.12223(13) -0.2864(2) 0.04087(14) 0.0331(5) Uani 0.75 1 d PD 1
N1 N -0.11171(13) 0.0311(2) 0.00348(14) 0.0336(7) Uani 0.75 1 d PD 1
N2 N -0.16789(15) 0.1042(2) -0.01262(15) 0.0401(8) Uani 0.75 1 d PD 1
N3 N -0.22746(15) 0.0375(2) -0.01415(17) 0.0355(8) Uani 0.75 1 d PD 1
N4 N -0.20678(10) -0.0766(2) 0.00127(12) 0.0250(5) Uani 0.75 1 d PD 1
C1 C -0.09092(10) -0.19304(18) 0.03092(15) 0.0259(6) Uani 0.75 1 d PD 1
C2 C -0.13594(11) -0.0810(2) 0.0115(3) 0.0201(7) Uani 0.75 1 d PD 1
O1' O -0.1340(4) 0.0899(7) -0.0116(6) 0.0367(6) Uani 0.25 1 d PD 2
O2' O -0.2323(4) -0.0100(9) -0.0133(6) 0.0331(5) Uani 0.25 1 d PD 2
N1' N -0.0516(4) -0.1232(7) 0.0280(4) 0.0336(7) Uani 0.25 1 d PD 2
N2' N -0.0337(5) -0.2368(7) 0.0478(5) 0.0401(8) Uani 0.25 1 d PD 2
N3' N -0.0935(4) -0.3003(9) 0.0491(6) 0.0355(8) Uani 0.25 1 d PD 2
N4' N -0.1473(4) -0.2224(7) 0.0315(4) 0.0250(5) Uani 0.25 1 d PD 2
C1' C -0.1672(3) -0.0026(7) -0.0042(4) 0.0259(6) Uani 0.25 1 d PD 2
C2' C -0.1219(4) -0.1133(8) 0.0196(11) 0.0201(7) Uani 0.25 1 d PD 2
N11 N 0.04125(10) 0.0514(2) 0.10407(10) 0.0369(5) Uani 1 1 d . .
N12 N 0.24803(11) 0.27086(18) 0.10171(10) 0.0294(5) Uani 1 1 d . .
C11 C 0.07894(13) -0.0267(3) 0.15510(14) 0.0418(7) Uani 1 1 d . .
H11A H 0.0858 -0.1085 0.1416 0.050 Uiso 1 1 calc R .
C12 C 0.10818(14) 0.0077(3) 0.22679(14) 0.0431(7) Uani 1 1 d . .
H12A H 0.1346 -0.0502 0.2615 0.052 Uiso 1 1 calc R .
C13 C 0.09887(13) 0.1266(3) 0.24789(13) 0.0385(6) Uani 1 1 d . .
C14 C 0.05885(13) 0.2063(3) 0.19487(14) 0.0410(7) Uani 1 1 d . .
H14A H 0.0504 0.2882 0.2070 0.049 Uiso 1 1 calc R .
C15 C 0.03129(13) 0.1656(3) 0.12410(14) 0.0388(6) Uani 1 1 d . .
H15A H 0.0042 0.2214 0.0883 0.047 Uiso 1 1 calc R .
C16 C 0.13084(14) 0.1669(3) 0.32549(13) 0.0440(7) Uani 1 1 d . .
H16A H 0.1213 0.1022 0.3571 0.053 Uiso 1 1 calc R .
H16B H 0.1056 0.2422 0.3328 0.053 Uiso 1 1 calc R .
C17 C 0.21154(13) 0.1926(3) 0.34964(12) 0.0331(6) Uani 1 1 d . .
H17A H 0.2285 0.2008 0.4029 0.040 Uiso 1 1 calc R .
H17B H 0.2362 0.1205 0.3372 0.040 Uiso 1 1 calc R .
C18 C 0.23484(17) 0.3059(3) 0.31766(14) 0.0432(7) Uani 1 1 d . .
H18A H 0.2830 0.3310 0.3497 0.052 Uiso 1 1 calc R .
H18B H 0.2008 0.3733 0.3178 0.052 Uiso 1 1 calc R .
C19 C 0.20553(13) 0.3548(2) 0.11785(13) 0.0320(6) Uani 1 1 d . .
H19A H 0.1783 0.4080 0.0806 0.038 Uiso 1 1 calc R .
C20 C 0.19935(14) 0.3677(2) 0.18619(13) 0.0354(6) Uani 1 1 d . .
H20A H 0.1680 0.4280 0.1950 0.042 Uiso 1 1 calc R .
C21 C 0.23879(14) 0.2928(2) 0.24158(13) 0.0341(6) Uani 1 1 d . .
C22 C 0.28436(14) 0.2069(2) 0.22553(13) 0.0347(6) Uani 1 1 d . .
H22A H 0.3131 0.1545 0.2624 0.042 Uiso 1 1 calc R .
C23 C 0.28762(13) 0.1979(2) 0.15583(13) 0.0324(5) Uani 1 1 d . .
H23A H 0.3187 0.1386 0.1456 0.039 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'
Cu Cu 0.3201 1.2651 '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
N1' Cu1 N1' 179.999(1) . 5
N1' Cu1 N11 89.3(3) . .
N1' Cu1 N11 90.7(3) 5 .
N1' Cu1 N11 90.7(3) . 5
N1' Cu1 N11 89.3(3) 5 5
N11 Cu1 N11 180.0 . 5
N1' Cu1 N1 58.3(2) . .
N1' Cu1 N1 121.7(2) 5 .
N11 Cu1 N1 90.78(9) . .
N11 Cu1 N1 89.22(9) 5 .
N1' Cu1 N1 121.7(2) . 5
N1' Cu1 N1 58.3(2) 5 5
N11 Cu1 N1 89.22(9) . 5
N11 Cu1 N1 90.78(9) 5 5
N1 Cu1 N1 180.0 . 5
N1' Cu1 O1 159.8(2) . 5
N1' Cu1 O1 20.2(2) 5 5
N11 Cu1 O1 90.08(9) . 5
N11 Cu1 O1 89.92(9) 5 5
N1 Cu1 O1 101.46(7) . 5
N1 Cu1 O1 78.54(7) 5 5
N1' Cu1 O1 20.2(2) . .
N1' Cu1 O1 159.8(2) 5 .
N11 Cu1 O1 89.92(9) . .
N11 Cu1 O1 90.08(9) 5 .
N1 Cu1 O1 78.54(7) . .
N1 Cu1 O1 101.46(7) 5 .
O1 Cu1 O1 180.0 5 .
N4' Cu2 N4' 180.00(15) 5 3
N4' Cu2 N12 89.5(2) 5 .
N4' Cu2 N12 90.5(2) 3 .
N4' Cu2 N12 90.5(2) 5 7
N4' Cu2 N12 89.5(2) 3 7
N12 Cu2 N12 180.0 . 7
N4' Cu2 N4 121.8(2) 5 3
N4' Cu2 N4 58.2(2) 3 3
N12 Cu2 N4 91.09(8) . 3
N12 Cu2 N4 88.91(8) 7 3
N4' Cu2 N4 58.2(2) 5 5
N4' Cu2 N4 121.8(2) 3 5
N12 Cu2 N4 88.91(8) . 5
N12 Cu2 N4 91.09(8) 7 5
N4 Cu2 N4 180.00(13) 3 5
N4' Cu2 O2 161.5(2) 5 3
N4' Cu2 O2 18.5(2) 3 3
N12 Cu2 O2 91.77(9) . 3
N12 Cu2 O2 88.23(9) 7 3
N4 Cu2 O2 76.62(7) 3 3
N4 Cu2 O2 103.38(7) 5 3
N4' Cu2 O2 18.5(2) 5 5
N4' Cu2 O2 161.5(2) 3 5
N12 Cu2 O2 88.23(9) . 5
N12 Cu2 O2 91.77(9) 7 5
N4 Cu2 O2 103.38(7) 3 5
N4 Cu2 O2 76.62(7) 5 5
O2 Cu2 O2 180.00(4) 3 5
C1 O1 Cu1 112.4(2) . .
C1 O2 Cu2 109.09(17) . 3_445
N2 N1 C2 106.4(2) . .
N2 N1 Cu1 146.93(19) . .
C2 N1 Cu1 104.53(17) . .
N1 N2 N3 109.1(2) . .
N4 N3 N2 107.4(2) . .
N3 N4 C2 107.4(2) . .
N3 N4 Cu2 140.14(19) . 3_445
C2 N4 Cu2 111.66(16) . 3_445
O2 C1 O1 126.7(2) . .
O2 C1 C2 115.8(2) . .
O1 C1 C2 117.5(2) . .
N4 C2 N1 109.74(19) . .
N4 C2 C1 124.91(19) . .
N1 C2 C1 125.3(2) . .
N2' N1' C2' 106.3(7) . .
N2' N1' Cu1 130.4(7) . .
C2' N1' Cu1 122.5(5) . .
N1' N2' N3' 109.5(9) . .
N4' N3' N2' 106.8(8) . .
N3' N4' C2' 108.0(7) . .
N3' N4' Cu2 130.7(6) . 3_445
C2' N4' Cu2 119.4(6) . 3_445
O2' C1' O1' 126.5(8) . .
O2' C1' C2' 118.8(8) . .
O1' C1' C2' 114.7(7) . .
N4' C2' N1' 109.4(6) . .
N4' C2' C1' 124.0(7) . .
N1' C2' C1' 126.5(6) . .
C15 N11 C11 118.1(2) . .
C15 N11 Cu1 120.26(18) . .
C11 N11 Cu1 121.7(2) . .
C19 N12 C23 117.6(2) . .
C19 N12 Cu2 121.02(17) . .
C23 N12 Cu2 121.34(17) . .
N11 C11 C12 122.3(3) . .
N11 C11 H11A 118.9 . .
C12 C11 H11A 118.9 . .
C11 C12 C13 120.0(3) . .
C11 C12 H12A 120.0 . .
C13 C12 H12A 120.0 . .
C12 C13 C14 117.3(2) . .
C12 C13 C16 121.1(3) . .
C14 C13 C16 121.6(3) . .
C15 C14 C13 119.6(3) . .
C15 C14 H14A 120.2 . .
C13 C14 H14A 120.2 . .
N11 C15 C14 122.8(3) . .
N11 C15 H15A 118.6 . .
C14 C15 H15A 118.6 . .
C13 C16 C17 115.2(2) . .
C13 C16 H16A 108.5 . .
C17 C16 H16A 108.5 . .
C13 C16 H16B 108.5 . .
C17 C16 H16B 108.5 . .
H16A C16 H16B 107.5 . .
C18 C17 C16 116.0(2) . .
C18 C17 H17A 108.3 . .
C16 C17 H17A 108.3 . .
C18 C17 H17B 108.3 . .
C16 C17 H17B 108.3 . .
H17A C17 H17B 107.4 . .
C17 C18 C21 116.1(2) . .
C17 C18 H18A 108.3 . .
C21 C18 H18A 108.3 . .
C17 C18 H18B 108.3 . .
C21 C18 H18B 108.3 . .
H18A C18 H18B 107.4 . .
N12 C19 C20 123.0(2) . .
N12 C19 H19A 118.5 . .
C20 C19 H19A 118.5 . .
C21 C20 C19 119.9(2) . .
C21 C20 H20A 120.1 . .
C19 C20 H20A 120.1 . .
C20 C21 C22 117.4(2) . .
C20 C21 C18 121.5(2) . .
C22 C21 C18 121.0(2) . .
C23 C22 C21 119.8(2) . .
C23 C22 H22A 120.1 . .
C21 C22 H22A 120.1 . .
N12 C23 C22 122.2(2) . .
N12 C23 H23A 118.9 . .
C22 C23 H23A 118.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1' 1.859(7) .
Cu1 N1' 1.859(7) 5
Cu1 N11 2.012(2) .
Cu1 N11 2.012(2) 5
Cu1 N1 2.230(3) .
Cu1 N1 2.230(3) 5
Cu1 O1 2.233(3) 5
Cu1 O1 2.233(3) .
Cu2 N4' 1.927(7) 5
Cu2 N4' 1.927(7) 3
Cu2 N12 2.0064(19) .
Cu2 N12 2.0065(19) 7
Cu2 N4 2.065(2) 3
Cu2 N4 2.065(2) 5
Cu2 O2 2.402(3) 3
Cu2 O2 2.402(3) 5
O1 C1 1.2332(11) .
O2 C1 1.2323(10) .
O2 Cu2 2.402(3) 3_445
N1 N2 1.3112(11) .
N1 C2 1.3355(11) .
N2 N3 1.3634(11) .
N3 N4 1.3115(11) .
N4 C2 1.3352(12) .
N4 Cu2 2.065(2) 3_445
C1 C2 1.4811(11) .
O1' C1' 1.2302(11) .
O2' C1' 1.2301(12) .
N1' N2' 1.3095(11) .
N1' C2' 1.3353(12) .
N2' N3' 1.3643(11) .
N3' N4' 1.3094(11) .
N4' C2' 1.3352(11) .
N4' Cu2 1.927(7) 3_445
C1' C2' 1.4804(11) .
N11 C15 1.336(4) .
N11 C11 1.339(4) .
N12 C19 1.336(3) .
N12 C23 1.352(3) .
C11 C12 1.384(3) .
C11 H11A 0.9500 .
C12 C13 1.387(4) .
C12 H12A 0.9500 .
C13 C14 1.387(4) .
C13 C16 1.508(3) .
C14 C15 1.386(3) .
C14 H14A 0.9500 .
C15 H15A 0.9500 .
C16 C17 1.523(3) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.515(4) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 C21 1.515(3) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 C20 1.381(3) .
C19 H19A 0.9500 .
C20 C21 1.379(4) .
C20 H20A 0.9500 .
C21 C22 1.393(4) .
C22 C23 1.382(3) .
C22 H22A 0.9500 .
C23 H23A 0.9500 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.243 500 180 ' '
2 0.000 0.500 0.766 500 180 ' '
