#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:44:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179391 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/88/4328868.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_4328868
loop_
_publ_author_name
'Eugenio Coronado'
'Mónica Giménez-Marqués'
'Guillermo Mínguez Espallargas'
_publ_section_title
;
 Combination of Magnetic Susceptibility and Electron Paramagnetic
 Resonance to Monitor the 1D to 2D Solid State Transformation in Flexible
 Metal-Organic Frameworks of Co(II) and Zn(II) with
 1,4-Bis(triazol-1-ylmethyl)benzene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4403
_journal_page_last               4410
_journal_paper_doi               10.1021/ic300276q
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C24 H24 N14 O6 Zn'
_chemical_formula_sum            'C24 H24 N14 O6 Zn'
_chemical_formula_weight         669.94
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 105.358(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1968(3)
_cell_length_b                   20.7210(9)
_cell_length_c                   8.4639(3)
_cell_measurement_reflns_used    2522
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4378
_cell_measurement_theta_min      1.9617
_cell_volume                     1386.22(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9927
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.955
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0422
_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)+(0.0242P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                2332
_reflns_number_total             3172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300276q_si_002_4.cif
_cod_data_source_block           5
_cod_original_cell_volume        1386.22(9)
_cod_database_code               4328868
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Zn1 Zn 0.5000 0.5000 0.5000 0.01833(12) Uani 1 2 d S . .
N1 N 0.4233(3) 0.59068(10) 0.5788(2) 0.0235(5) Uani 1 1 d . A .
C2 C 0.2997(3) 0.60092(12) 0.6510(3) 0.0227(6) Uani 1 1 d . . .
H2 H 0.2204 0.5693 0.6641 0.027 Uiso 1 1 calc R A .
N3 N 0.3033(3) 0.66146(10) 0.7020(2) 0.0226(5) Uani 1 1 d . A .
N4 N 0.4332(3) 0.69397(10) 0.6652(3) 0.0296(5) Uani 1 1 d . . .
C5 C 0.5000(3) 0.64940(13) 0.5910(3) 0.0278(6) Uani 1 1 d . A .
H5 H 0.5947 0.6576 0.5491 0.033 Uiso 1 1 calc R . .
C6 C 0.2019(3) 0.69056(12) 0.8014(3) 0.0290(6) Uani 1 1 d . . .
H6A H 0.2786 0.7071 0.9042 0.043 Uiso 1 1 calc R A .
H6B H 0.1297 0.6568 0.8310 0.043 Uiso 1 1 calc R . .
C7 C 0.0908(3) 0.74501(12) 0.7163(3) 0.0261(6) Uani 1 1 d . A .
C8 C 0.1307(3) 0.80766(12) 0.7625(3) 0.0317(7) Uani 1 1 d . . .
H8 H 0.2321 0.8167 0.8446 0.038 Uiso 1 1 calc R A .
C9 C 0.0260(3) 0.85795(13) 0.6918(3) 0.0311(7) Uani 1 1 d . A .
H9 H 0.0574 0.9010 0.7247 0.037 Uiso 1 1 calc R . .
C10 C -0.1226(3) 0.84655(13) 0.5746(3) 0.0287(6) Uani 1 1 d . . .
C11 C -0.1621(4) 0.78391(15) 0.5245(4) 0.0513(10) Uani 1 1 d . A .
H11 H -0.2625 0.7751 0.4409 0.062 Uiso 1 1 calc R . .
C12 C -0.0563(4) 0.73376(14) 0.5954(4) 0.0501(9) Uani 1 1 d . . .
H12 H -0.0855 0.6908 0.5601 0.060 Uiso 1 1 calc R A .
C13 C -0.2357(3) 0.90218(15) 0.5004(3) 0.0349(7) Uani 1 1 d . A .
H13A H -0.1649 0.9402 0.4934 0.052 Uiso 1 1 calc R . .
H13B H -0.3002 0.8906 0.3877 0.052 Uiso 1 1 calc R . .
N14 N -0.3546(3) 0.91908(10) 0.5968(2) 0.0249(5) Uani 1 1 d . . .
N15 N -0.5246(3) 0.91719(12) 0.5289(3) 0.0360(6) Uani 1 1 d . A .
C16 C -0.5847(3) 0.93925(13) 0.6471(3) 0.0317(7) Uani 1 1 d . . .
H16 H -0.7025 0.9439 0.6363 0.038 Uiso 1 1 calc R A .
N17 N -0.4650(2) 0.95502(9) 0.7865(2) 0.0200(5) Uani 1 1 d . . .
C18 C -0.3226(3) 0.94148(12) 0.7485(3) 0.0220(6) Uani 1 1 d . A .
H18 H -0.2127 0.9470 0.8199 0.026 Uiso 1 1 calc R . .
N1N N 0.1102(3) 0.46670(10) 0.3254(3) 0.0246(5) Uani 1 1 d . . .
O1N O 0.2334(4) 0.50520(19) 0.3625(4) 0.0213(9) Uani 0.512(4) 1 d P A -1
O2N O -0.017(3) 0.4770(8) 0.207(3) 0.020(2) Uani 0.512(4) 1 d P A -1
O3N O 0.1362(4) 0.40916(16) 0.3836(4) 0.0281(11) Uani 0.512(4) 1 d P A -1
O1N' O 0.2565(4) 0.4597(2) 0.3507(4) 0.0269(11) Uani 0.488(4) 1 d P A -2
O2N' O 0.003(3) 0.4600(8) 0.201(3) 0.027(3) Uani 0.488(4) 1 d P A -2
O3N' O 0.0526(4) 0.49180(18) 0.4493(4) 0.0314(12) Uani 0.488(4) 1 d P A -2
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'
Zn Zn 0.2839 1.4301 '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
N17 Zn1 N17 180.00(9) 4_675 2_546
N17 Zn1 N1 90.18(7) 4_675 3_666
N17 Zn1 N1 89.82(7) 2_546 3_666
N17 Zn1 N1 89.82(7) 4_675 .
N17 Zn1 N1 90.18(7) 2_546 .
N1 Zn1 N1 180.000(1) 3_666 .
N17 Zn1 O1N 82.33(10) 4_675 .
N17 Zn1 O1N 97.67(10) 2_546 .
N1 Zn1 O1N 102.22(12) 3_666 .
N1 Zn1 O1N 77.78(12) . .
N17 Zn1 O1N 97.67(10) 4_675 3_666
N17 Zn1 O1N 82.33(10) 2_546 3_666
N1 Zn1 O1N 77.78(12) 3_666 3_666
N1 Zn1 O1N 102.22(12) . 3_666
O1N Zn1 O1N 180.0 . 3_666
N17 Zn1 O1N' 89.10(12) 4_675 .
N17 Zn1 O1N' 90.90(12) 2_546 .
N1 Zn1 O1N' 77.71(13) 3_666 .
N1 Zn1 O1N' 102.29(13) . .
O1N Zn1 O1N' 25.43(11) . .
O1N Zn1 O1N' 154.57(11) 3_666 .
N17 Zn1 O1N' 90.90(12) 4_675 3_666
N17 Zn1 O1N' 89.10(12) 2_546 3_666
N1 Zn1 O1N' 102.29(13) 3_666 3_666
N1 Zn1 O1N' 77.71(13) . 3_666
O1N Zn1 O1N' 154.57(11) . 3_666
O1N Zn1 O1N' 25.43(11) 3_666 3_666
O1N' Zn1 O1N' 180.0(2) . 3_666
C2 N1 C5 102.4(2) . .
C2 N1 Zn1 127.18(17) . .
C5 N1 Zn1 129.77(17) . .
N3 C2 N1 110.3(2) . .
N3 C2 H2 124.8 . .
N1 C2 H2 124.8 . .
C2 N3 N4 110.1(2) . .
C2 N3 C6 127.8(2) . .
N4 N3 C6 121.7(2) . .
C5 N4 N3 102.2(2) . .
N4 C5 N1 114.9(2) . .
N4 C5 H5 122.5 . .
N1 C5 H5 122.5 . .
N3 C6 C7 113.4(2) . .
N3 C6 H6A 108.9 . .
C7 C6 H6A 108.9 . .
N3 C6 H6B 108.9 . .
C7 C6 H6B 108.9 . .
H6A C6 H6B 107.7 . .
C8 C7 C12 117.9(3) . .
C8 C7 C6 120.3(2) . .
C12 C7 C6 121.8(2) . .
C7 C8 C9 121.1(2) . .
C7 C8 H8 119.4 . .
C9 C8 H8 119.4 . .
C10 C9 C8 120.9(2) . .
C10 C9 H9 119.5 . .
C8 C9 H9 119.5 . .
C9 C10 C11 118.4(3) . .
C9 C10 C13 120.0(2) . .
C11 C10 C13 121.6(2) . .
C10 C11 C12 120.3(3) . .
C10 C11 H11 119.9 . .
C12 C11 H11 119.9 . .
C7 C12 C11 121.3(3) . .
C7 C12 H12 119.4 . .
C11 C12 H12 119.4 . .
N14 C13 C10 112.1(2) . .
N14 C13 H13A 109.2 . .
C10 C13 H13A 109.2 . .
N14 C13 H13B 109.2 . .
C10 C13 H13B 109.2 . .
H13A C13 H13B 107.9 . .
C18 N14 N15 109.7(2) . .
C18 N14 C13 129.2(2) . .
N15 N14 C13 121.0(2) . .
C16 N15 N14 102.6(2) . .
N15 C16 N17 114.6(2) . .
N15 C16 H16 122.7 . .
N17 C16 H16 122.7 . .
C18 N17 C16 102.6(2) . .
C18 N17 Zn1 128.99(16) . 2_556
C16 N17 Zn1 128.07(17) . 2_556
N17 C18 N14 110.5(2) . .
N17 C18 H18 124.8 . .
N14 C18 H18 124.8 . .
O1N' N1N O2N' 129.0(10) . .
O1N' N1N O2N 139.4(10) . .
O1N' N1N O1N 47.0(2) . .
O2N' N1N O1N 130.6(12) . .
O2N N1N O1N 122.1(10) . .
O1N' N1N O3N 76.0(3) . .
O2N' N1N O3N 103.9(9) . .
O2N N1N O3N 118.7(9) . .
O1N N1N O3N 116.8(3) . .
O1N' N1N O3N' 117.0(3) . .
O2N' N1N O3N' 113.6(9) . .
O2N N1N O3N' 99.6(8) . .
O1N N1N O3N' 89.1(3) . .
O3N N1N O3N' 96.6(3) . .
N1N O1N Zn1 136.3(3) . .
N1N O1N' Zn1 141.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N17 2.1188(19) 4_675
Zn1 N17 2.1188(19) 2_546
Zn1 N1 2.143(2) 3_666
Zn1 N1 2.143(2) .
Zn1 O1N 2.190(3) .
Zn1 O1N 2.190(3) 3_666
Zn1 O1N' 2.223(4) .
Zn1 O1N' 2.223(4) 3_666
N1 C2 1.331(3) .
N1 C5 1.361(3) .
C2 N3 1.325(3) .
C2 H2 0.9500 .
N3 N4 1.364(3) .
N3 C6 1.460(3) .
N4 C5 1.315(3) .
C5 H5 0.9500 .
C6 C7 1.508(3) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.370(3) .
C7 C12 1.379(4) .
C8 C9 1.381(3) .
C8 H8 0.9500 .
C9 C10 1.373(3) .
C9 H9 0.9500 .
C10 C11 1.377(4) .
C10 C13 1.508(4) .
C11 C12 1.385(4) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 N14 1.469(3) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
N14 C18 1.325(3) .
N14 N15 1.360(3) .
N15 C16 1.309(3) .
C16 N17 1.360(3) .
C16 H16 0.9500 .
N17 C18 1.321(3) .
N17 Zn1 2.1188(19) 2_556
C18 H18 0.9500 .
N1N O1N' 1.169(4) .
N1N O2N' 1.19(2) .
N1N O2N 1.26(2) .
N1N O1N 1.259(4) .
N1N O3N 1.286(4) .
N1N O3N' 1.362(4) .
