#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:50:11 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178965 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/94/4119459.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_4119459
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, H2 O'
_chemical_formula_sum            'C15 H14 Cu N6 O3'
_chemical_formula_weight         389.9
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                75.320(5)
_cell_angle_beta                 73.151(6)
_cell_angle_gamma                68.201(4)
_cell_formula_units_Z            2
_cell_length_a                   8.8876(6)
_cell_length_b                   9.8698(7)
_cell_length_c                   11.3149(6)
_cell_measurement_temperature    295(2)
_cell_volume                     870.05(10)
_computing_cell_refinement       'TOPAS v.4.2 (Bruker AXS, 2009)'
_computing_data_reduction        'Fit 2D (Hammersley, 1996)'
_computing_molecular_graphics    'DIAMOND 3 (Brandenburg, 2005)'
_computing_publication_material  'Jana 2006 (Palatinus, 2007)'
_computing_structure_refinement  'Jana 2006 (Palatinus, 2007)'
_computing_structure_solution    'FOX (Favre-Nicolin, 2002)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'Imaging Plate'
_diffrn_detector_type            Mar345
_diffrn_measurement_device       'diffractometr at 1-BM line'
_diffrn_radiation_monochromator  'PSL DCM Si(111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.60505
_diffrn_source                   synchrotron
_diffrn_source_type              synchrotron
_exptl_absorpt_coefficient_mu    0.831
_exptl_crystal_density_diffrn    1.4877
_exptl_crystal_F_000             398
_pd_char_colour                  blue
_pd_char_particle_morphology     'samll crystalline powder'
_pd_instr_location
; 
1-BM-C line diffractometer, APS, Argonne National Lab (USA)
;
_pd_meas_2theta_range_inc        0.013
_pd_meas_2theta_range_max        25.993
_pd_meas_2theta_range_min        0.761
_pd_meas_number_of_points        1942
_pd_meas_scan_method             fixed
_pd_prep_cool_rate               180
_pd_prep_pressure                101.325
_pd_prep_temperature             295(2)
_pd_proc_2theta_range_inc        0.013
_pd_proc_2theta_range_max        25.824
_pd_proc_2theta_range_min        2.905
_pd_proc_ls_background_function  '12 Legendre polynoms'
_pd_proc_ls_pref_orient_corr     'Sasa & Uda'
_pd_proc_ls_profile_function     Pseudo-Voigt
_pd_proc_ls_prof_R_factor        0.0534
_pd_proc_ls_prof_wR_expected     0.0397
_pd_proc_ls_prof_wR_factor       0.0729
_pd_spec_mounting                'capton capillary with He exchange gas'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              10.0
_pd_spec_size_equat              0.9
_pd_spec_size_thick              0.9
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.31
_refine_ls_goodness_of_fit_all   1.830
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    125
_refine_ls_number_parameters     42
_refine_ls_number_restraints     0
_refine_ls_R_I_factor            0.0515
_refine_ls_shift/su_max          0.0154
_refine_ls_shift/su_mean         0.0008
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            ja312347p_si_006.cif
_cod_data_source_block           I
_cod_original_cell_volume        870.04(10)
_cod_database_code               4119459
_cod_database_fobs_code          4119459
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -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_adp_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0 0 0 Uiso 0.036(3) 2 1 d S
Cu2 Cu 0 0 0.5 Uiso 0.036(3) 2 1 d S
O1 O -0.105453 -0.112276 -0.098469 Uiso 0.048(4) 1 1 d G
O2 O -0.095376 -0.103909 -0.299619 Uiso 0.048(4) 1 1 d G
C1 C -0.081471 -0.059938 -0.212402 Uiso 0.048(4) 1 1 d G
C2 C -0.025231 0.067174 -0.24884 Uiso 0.048(4) 1 1 d G
N1 N 0.004028 0.12768 -0.169374 Uiso 0.048(4) 1 1 d G
N2 N 0.06062 0.233465 -0.238431 Uiso 0.048(4) 1 1 d G
N3 N 0.066588 0.239611 -0.361904 Uiso 0.048(4) 1 1 d G
N4 N 0.013877 0.137394 -0.367008 Uiso 0.048(4) 1 1 d G
N11 N -0.223807 0.134475 0.05717 Uiso 0.048(4) 1 1 d G
N12 N -0.215299 0.129309 0.472991 Uiso 0.048(4) 1 1 d G
C11 C -0.357885 0.092418 0.103892 Uiso 0.048(4) 1 1 d G
C12 C -0.51305 0.187962 0.150273 Uiso 0.048(4) 1 1 d G
C13 C -0.535816 0.333117 0.153245 Uiso 0.048(4) 1 1 d G
C14 C -0.398488 0.374244 0.106153 Uiso 0.048(4) 1 1 d G
C15 C -0.246468 0.27392 0.059584 Uiso 0.048(4) 1 1 d G
C16 C -0.707403 0.439868 0.202262 Uiso 0.048(4) 1 1 d G
C17 C -0.780322 0.402509 0.342965 Uiso 0.048(4) 1 1 d G
C18 C -0.70466 0.437206 0.429825 Uiso 0.048(4) 1 1 d G
C19 C -0.531961 0.32968 0.443223 Uiso 0.048(4) 1 1 d G
C20 C -0.507825 0.187243 0.508537 Uiso 0.048(4) 1 1 d G
C21 C -0.352491 0.092578 0.521681 Uiso 0.048(4) 1 1 d G
C22 C -0.237873 0.267973 0.410284 Uiso 0.048(4) 1 1 d G
C23 C -0.390972 0.369277 0.394006 Uiso 0.048(4) 1 1 d G
O1w O 0.195(3) 0.391(3) 0.894(2) Uiso 0.048(4) 1 1 d .
H1c11 H -0.347184 -0.008484 0.105722 Uiso 0.0573 1 1 d R
H1c12 H -0.606313 0.152102 0.180877 Uiso 0.0573 1 1 d R
H1c14 H -0.405594 0.474093 0.1047 Uiso 0.0573 1 1 d R
H1c15 H -0.152205 0.308315 0.027194 Uiso 0.0573 1 1 d R
H1c16 H -0.78388 0.445214 0.154933 Uiso 0.0573 1 1 d R
H2c16 H -0.702592 0.538831 0.183524 Uiso 0.0573 1 1 d R
H1c17 H -0.898091 0.451738 0.360109 Uiso 0.0573 1 1 d R
H2c17 H -0.772588 0.299955 0.363643 Uiso 0.0573 1 1 d R
H1c18 H -0.778219 0.440853 0.510886 Uiso 0.0573 1 1 d R
H2c18 H -0.699698 0.536127 0.402702 Uiso 0.0573 1 1 d R
H1c20 H -0.602049 0.153455 0.545746 Uiso 0.0573 1 1 d R
H1c21 H -0.342878 -0.004998 0.568452 Uiso 0.0573 1 1 d R
H1c22 H -0.14166 0.299135 0.374294 Uiso 0.0573 1 1 d R
H1c23 H -0.398192 0.466974 0.348342 Uiso 0.0573 1 1 d R
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0020 0.0012 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Cu 0.3365 0.9562 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0043 0.0024 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0076 0.0044 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 Cu1 N1 . 2_555 180
N1 Cu1 N11 . . 88.2287
N1 Cu1 N11 . 2_555 91.7713
N1 Cu1 N11 2_555 . 91.7713
N1 Cu1 N11 2_555 2_555 88.2287
N11 Cu1 N11 . 2_555 180
N12 Cu2 N12 . 2_556 180
O1 C1 O2 . . 128.8739
O1 C1 C2 . . 116.5747
O2 C1 C2 . . 114.5266
C1 C2 N1 . . 123.8215
C1 C2 N4 . . 126.2372
N1 C2 N4 . . 109.8542
Cu1 N1 C2 . . 111.3744
Cu1 N1 N2 . . 141.0125
C2 N1 N2 . . 105.2911
N1 N2 N3 . . 110.1769
N2 N3 N4 . . 106.9028
C2 N4 N3 . . 107.7748
Cu1 N11 C11 . . 124.0683
Cu1 N11 C15 . . 120.2977
C11 N11 C15 . . 115.4447
Cu2 N12 C21 . . 122.9695
Cu2 N12 C22 . . 121.6039
C21 N12 C22 . . 115.2628
N11 C11 C12 . . 122.9299
N11 C11 H1c11 . . 118.535
C12 C11 H1c11 . . 118.5352
C11 C12 C13 . . 121.3777
C11 C12 H1c12 . . 119.3109
C13 C12 H1c12 . . 119.3114
C12 C13 C14 . . 115.0982
C12 C13 C16 . . 121.6194
C14 C13 C16 . . 123.2411
C13 C14 C15 . . 120.9666
C13 C14 H1c14 . . 119.5168
C15 C14 H1c14 . . 119.5166
N11 C15 C14 . . 124.1656
N11 C15 H1c15 . . 117.9168
C14 C15 H1c15 . . 117.9176
C13 C16 C17 . . 115.1156
C13 C16 H1c16 . . 109.4713
C13 C16 H2c16 . . 109.471
C17 C16 H1c16 . . 109.4712
C17 C16 H2c16 . . 109.471
H1c16 C16 H2c16 . . 103.168
C16 C17 C18 . . 115.5889
C16 C17 H1c17 . . 109.4707
C16 C17 H2c17 . . 109.4708
C18 C17 H1c17 . . 109.4712
C18 C17 H2c17 . . 109.4718
H1c17 C17 H2c17 . . 102.5714
C17 C18 C19 . . 114.72
C17 C18 H1c18 . . 109.4713
C17 C18 H2c18 . . 109.4714
C19 C18 H1c18 . . 109.4716
C19 C18 H2c18 . . 109.4708
H1c18 C18 H2c18 . . 103.6568
C18 C19 C20 . . 122.3353
C18 C19 C23 . . 122.3561
C20 C19 C23 . . 115.288
C19 C20 C21 . . 121.7929
C19 C20 H1c20 . . 119.1032
C21 C20 H1c20 . . 119.104
N12 C21 C20 . . 123.3048
N12 C21 H1c21 . . 118.3479
C20 C21 H1c21 . . 118.3474
N12 C22 C23 . . 124.3959
N12 C22 H1c22 . . 117.8022
C23 C22 H1c22 . . 117.8019
C19 C23 C22 . . 119.9467
C19 C23 H1c23 . . 120.0262
C22 C23 H1c23 . . 120.0271
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cu1 N1 . 2.0079
Cu1 N1 2_555 2.0079
Cu1 N11 . 1.966
Cu1 N11 2_555 1.966
Cu2 N12 . 1.9264
Cu2 N12 2_556 1.9264
O1 C1 . 1.2486
O2 C1 . 1.2268
C1 C2 . 1.4415
C2 N1 . 1.325
C2 N4 . 1.3523
N1 N2 . 1.3047
N2 N3 . 1.3692
N3 N4 . 1.2794
N11 C11 . 1.3277
N11 C15 . 1.3212
N12 C21 . 1.3264
N12 C22 . 1.3428
C11 C12 . 1.3899
C11 H1c11 . 0.96
C12 C13 . 1.3783
C12 H1c12 . 0.96
C13 C14 . 1.349
C13 C16 . 1.5349
C14 C15 . 1.3934
C14 H1c14 . 0.96
C15 H1c15 . 0.96
C16 C17 . 1.5403
C16 H1c16 . 0.96
C16 H2c16 . 0.96
C17 C18 . 1.5034
C17 H1c17 . 0.96
C17 H2c17 . 0.96
C18 C19 . 1.5325
C18 H1c18 . 0.96
C18 H2c18 . 0.96
C19 C20 . 1.382
C19 C23 . 1.3718
C20 C21 . 1.3753
C20 H1c20 . 0.96
C21 H1c21 . 0.96
C22 C23 . 1.388
C22 H1c22 . 0.96
C23 H1c23 . 0.96
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C22 H1c22 O2 2_555 0.96 2.38 2.8771 112.06
loop_
_pd_proc_info_excluded_regions
'from 0.76 to 2.900'
'from 25.83 to 26.019'
