 
data_MOF-2
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C23 H14 N2 O5 Zn'
_chemical_formula_sum
 'C23 H14 N2 O5 Zn'
_chemical_formula_weight          463.75
 
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'
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    'C 2/c'
_symmetry_space_group_name_Hall   '-C 2yc'
 
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'
 
_cell_length_a                    29.971(8)
_cell_length_b                    16.271(4)
_cell_length_c                    15.804(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  115.749(7)
_cell_angle_gamma                 90.00
_cell_volume                      6942(3)
_cell_formula_units_Z             8
_cell_measurement_temperature     90(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        'Needles'
_exptl_crystal_colour             'colorless'
_exptl_crystal_size_max           0.40
_exptl_crystal_size_mid           0.23
_exptl_crystal_size_min           0.21
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     0.887
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1888.0
_exptl_absorpt_coefficient_mu     0.730
_exptl_absorpt_correction_type    'EMPIRICAL'
_exptl_absorpt_correction_T_min   0.818
_exptl_absorpt_correction_T_max   0.858
_exptl_absorpt_process_details    'SADABS'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       90(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'CCD area detector'
_diffrn_measurement_method        'phi and omega scan'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             76513
_diffrn_reflns_av_R_equivalents   0.0859
_diffrn_reflns_av_sigmaI/netI     0.0481
_diffrn_reflns_limit_h_min        -37
_diffrn_reflns_limit_h_max        37
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          3.13
_diffrn_reflns_theta_max          26.37
_reflns_number_total              7085
_reflns_number_gt                 4780
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        'Bruker kappa apex ccd'
_computing_cell_refinement        'Bruker kappa apex ccd'
_computing_data_reduction         'Bruker saint'
_computing_structure_solution     'shelxs-97'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   'WinGX1.80.05'
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          7085
_refine_ls_number_parameters      280
_refine_ls_number_restraints      14
_refine_ls_R_factor_all           0.1319
_refine_ls_R_factor_gt            0.1051
_refine_ls_wR_factor_ref          0.3192
_refine_ls_wR_factor_gt           0.3014
_refine_ls_goodness_of_fit_ref    1.215
_refine_ls_restrained_S_all       1.222
_refine_ls_shift/su_max           0.002
_refine_ls_shift/su_mean          0.000
 
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 0.24686(2) 0.21143(3) 0.37151(3) 0.0405(3) Uani 1 1 d . . .
O4 O 0.24791(13) 0.3364(2) 0.3746(2) 0.0486(9) Uani 1 1 d . . .
O1 O 0.25047(16) 0.20610(19) 0.2394(3) 0.0530(10) Uani 1 1 d . . .
N2 N 0.3262(2) 0.2079(3) 0.4458(4) 0.0600(13) Uani 1 1 d . . .
N1 N 0.1672(2) 0.2139(3) 0.2957(4) 0.0607(13) Uani 1 1 d . . .
C13 C 0.2539(2) 0.3747(3) 0.4477(3) 0.0441(12) Uani 1 1 d . . .
C10 C 0.2468(2) 0.0885(3) 0.1476(3) 0.0500(14) Uani 1 1 d . . .
C11 C 0.2497(2) 0.1307(3) 0.2350(4) 0.0491(13) Uani 1 1 d . . .
C3 C 0.0635(4) 0.2166(8) 0.1868(11) 0.136(5) Uani 1 1 d . . .
C2 C 0.0980(5) 0.2856(9) 0.1812(14) 0.213(10) Uani 1 1 d D . .
H2 H 0.0854 0.3305 0.1414 0.256 Uiso 1 1 calc R . .
C6 C 0.3512(4) 0.1570(8) 0.5125(12) 0.173(6) Uani 1 1 d . . .
H6 H 0.3337 0.1184 0.5297 0.208 Uiso 1 1 calc R . .
C4 C 0.0870(4) 0.1532(8) 0.2365(10) 0.149(5) Uani 1 1 d . . .
H4 H 0.0692 0.1062 0.2359 0.178 Uiso 1 1 calc R . .
C1 C 0.1464(4) 0.2778(7) 0.2360(12) 0.167(7) Uani 1 1 d . . .
H1 H 0.1674 0.3187 0.2331 0.200 Uiso 1 1 calc R . .
C5 C 0.1371(4) 0.1541(6) 0.2896(8) 0.117(3) Uani 1 1 d . . .
H5 H 0.1511 0.1073 0.3249 0.141 Uiso 1 1 calc R . .
C14 C 0.3526(4) 0.2647(9) 0.4256(10) 0.149(5) Uani 1 1 d . . .
H14 H 0.3361 0.3043 0.3804 0.179 Uiso 1 1 calc R . .
C8 C 0.4306(4) 0.2102(7) 0.5409(10) 0.123(4) Uani 1 1 d . . .
C9 C 0.4038(5) 0.2655(12) 0.4705(15) 0.207(9) Uani 1 1 d . . .
H9 H 0.4209 0.3045 0.4527 0.249 Uiso 1 1 calc R . .
C7 C 0.4043(6) 0.1565(10) 0.5616(16) 0.240(11) Uani 1 1 d . . .
H7 H 0.4202 0.1178 0.6085 0.288 Uiso 1 1 calc R . .
O3 O 0.24794(17) 0.0862(2) 0.2998(3) 0.0627(11) Uani 1 1 d . . .
C15 C 0.2559(2) 0.4661(3) 0.4386(3) 0.0438(12) Uani 1 1 d . . .
C17 C 0.25269(17) 0.5049(3) 0.3592(3) 0.0425(12) Uani 1 1 d . . .
H17 H 0.2501 0.4732 0.3082 0.051 Uiso 1 1 calc R . .
C18 C 0.2598(3) 0.5146(3) 0.5165(4) 0.076(2) Uani 1 1 d . . .
H18 H 0.2618 0.4899 0.5711 0.091 Uiso 1 1 calc R . .
C19 C 0.2605(4) 0.5997(4) 0.5092(5) 0.098(3) Uani 1 1 d . . .
C20 C 0.2429(4) 0.1382(3) 0.0729(5) 0.089(3) Uani 1 1 d . . .
H20 H 0.2424 0.1952 0.0772 0.107 Uiso 1 1 calc R . .
O2 O 0.2612(2) 0.3457(2) 0.5237(3) 0.0752(14) Uani 1 1 d . . .
O5 O 0.2663(3) 0.6534(2) 0.5829(4) 0.140(3) Uani 1 1 d . . .
C24 C 0.2811(6) 0.6190(6) 0.6757(6) 0.153(6) Uani 1 1 d D . .
H24A H 0.2620 0.5697 0.6711 0.184 Uiso 1 1 calc R . .
H24B H 0.2742 0.6582 0.7148 0.184 Uiso 1 1 calc R . .
C25 C 0.3397(9) 0.5967(8) 0.7241(12) 0.180(8) Uani 1 1 d DU . .
C26 C 0.3873(14) 0.5783(18) 0.7732(17) 0.336(19) Uani 1 1 d U . .
H26 H 0.4206 0.5654 0.8075 0.403 Uiso 1 1 calc R . .
C2B C 0.4673(4) 0.2897(5) 0.6357(7) 0.037(2) Uiso 0.48 1 d P . .
C1B C 0.0236(4) 0.2830(6) 0.1114(9) 0.054(3) Uiso 0.52 1 d PD . .
C1A C 0.0056(7) 0.2172(10) 0.1240(14) 0.092(5) Uiso 0.48 1 d P . .
C2A C 0.4832(7) 0.2049(9) 0.5910(13) 0.092(5) Uiso 0.52 1 d P . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
 
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
Zn1 O2 2.004(4) 7_556 ?
Zn1 O4 2.033(4) . ?
Zn1 N2 2.146(6) . ?
Zn1 O1 2.139(4) . ?
Zn1 N1 2.157(5) . ?
Zn1 O3 2.339(4) . ?
Zn1 C11 2.558(5) . ?
O4 C13 1.256(5) . ?
O1 C11 1.229(6) . ?
N2 C6 1.294(13) . ?
N2 C14 1.342(12) . ?
N1 C5 1.303(10) . ?
N1 C1 1.359(12) . ?
C13 O2 1.218(6) . ?
C13 C15 1.498(6) . ?
C10 C17 1.365(7) 4_545 ?
C10 C20 1.393(7) . ?
C10 C11 1.512(7) . ?
C11 O3 1.273(6) . ?
C3 C4 1.302(15) . ?
C3 C2 1.556(19) . ?
C3 C1A 1.58(2) . ?
C3 C1B 1.667(17) . ?
C2 C1 1.335(16) . ?
C2 C1B 2.013(17) . ?
C6 C7 1.438(17) . ?
C4 C5 1.365(14) . ?
C14 C9 1.385(16) . ?
C8 C7 1.31(2) . ?
C8 C9 1.385(19) . ?
C8 C2A 1.43(2) . ?
C8 C2B 1.922(15) . ?
C15 C17 1.370(6) . ?
C15 C18 1.423(7) . ?
C17 C10 1.365(7) 4 ?
C18 C19 1.391(8) . ?
C19 O5 1.406(7) . ?
C19 C20 1.404(8) 4 ?
C20 C19 1.404(8) 4_545 ?
O2 Zn1 2.004(4) 7_556 ?
O5 C24 1.448(10) . ?
C24 C25 1.62(2) . ?
C25 C26 1.33(3) . ?
C2B C1A 1.24(2) 8_556 ?
C2B C2A 1.710(19) . ?
C1B C2A 1.13(2) 8_455 ?
C1B C1A 1.254(19) . ?
C1A C2B 1.24(2) 8_455 ?
C1A C2A 1.42(2) 8_455 ?
C2A C1B 1.13(2) 8_556 ?
C2A C1A 1.42(2) 8_556 ?
 
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
O2 Zn1 O4 116.73(13) 7_556 . ?
O2 Zn1 N2 92.2(2) 7_556 . ?
O4 Zn1 N2 90.66(16) . . ?
O2 Zn1 O1 149.74(13) 7_556 . ?
O4 Zn1 O1 93.29(12) . . ?
N2 Zn1 O1 91.11(19) . . ?
O2 Zn1 N1 88.1(2) 7_556 . ?
O4 Zn1 N1 89.78(16) . . ?
N2 Zn1 N1 179.32(19) . . ?
O1 Zn1 N1 88.35(19) . . ?
O2 Zn1 O3 91.66(14) 7_556 . ?
O4 Zn1 O3 151.57(12) . . ?
N2 Zn1 O3 89.82(17) . . ?
O1 Zn1 O3 58.28(12) . . ?
N1 Zn1 O3 89.55(18) . . ?
O2 Zn1 C11 121.27(17) 7_556 . ?
O4 Zn1 C11 121.88(15) . . ?
N2 Zn1 C11 90.74(19) . . ?
O1 Zn1 C11 28.58(15) . . ?
N1 Zn1 C11 88.6(2) . . ?
O3 Zn1 C11 29.69(15) . . ?
C13 O4 Zn1 120.9(3) . . ?
C11 O1 Zn1 95.0(3) . . ?
C6 N2 C14 116.2(9) . . ?
C6 N2 Zn1 125.1(7) . . ?
C14 N2 Zn1 118.6(6) . . ?
C5 N1 C1 115.2(8) . . ?
C5 N1 Zn1 126.3(6) . . ?
C1 N1 Zn1 117.6(5) . . ?
O2 C13 O4 127.3(4) . . ?
O2 C13 C15 118.9(4) . . ?
O4 C13 C15 113.6(4) . . ?
C17 C10 C20 120.8(4) 4_545 . ?
C17 C10 C11 121.7(4) 4_545 . ?
C20 C10 C11 117.5(4) . . ?
O1 C11 O3 121.9(5) . . ?
O1 C11 C10 119.8(5) . . ?
O3 C11 C10 118.1(4) . . ?
O1 C11 Zn1 56.4(3) . . ?
O3 C11 Zn1 65.5(3) . . ?
C10 C11 Zn1 173.9(4) . . ?
C4 C3 C2 114.0(10) . . ?
C4 C3 C1A 122.9(12) . . ?
C2 C3 C1A 122.4(12) . . ?
C4 C3 C1B 167.6(11) . . ?
C2 C3 C1B 77.2(9) . . ?
C1A C3 C1B 45.3(7) . . ?
C1 C2 C3 117.2(11) . . ?
C1 C2 C1B 170.8(14) . . ?
C3 C2 C1B 53.9(7) . . ?
N2 C6 C7 123.8(13) . . ?
C3 C4 C5 121.6(11) . . ?
N1 C1 C2 124.4(10) . . ?
N1 C5 C4 126.6(9) . . ?
N2 C14 C9 121.5(11) . . ?
C7 C8 C9 115.7(11) . . ?
C7 C8 C2A 117.5(13) . . ?
C9 C8 C2A 126.8(14) . . ?
C7 C8 C2B 117.2(15) . . ?
C9 C8 C2B 97.1(11) . . ?
C2A C8 C2B 59.2(8) . . ?
C8 C9 C14 122.1(13) . . ?
C8 C7 C6 120.5(14) . . ?
C11 O3 Zn1 84.8(3) . . ?
C17 C15 C18 119.0(4) . . ?
C17 C15 C13 123.7(4) . . ?
C18 C15 C13 117.3(4) . . ?
C10 C17 C15 122.1(4) 4 . ?
C19 C18 C15 118.6(5) . . ?
O5 C19 C18 123.4(6) . . ?
O5 C19 C20 114.9(5) . 4 ?
C18 C19 C20 121.6(5) . 4 ?
C10 C20 C19 118.0(5) . 4_545 ?
C13 O2 Zn1 163.8(5) . 7_556 ?
C19 O5 C24 118.2(5) . . ?
O5 C24 C25 110.9(11) . . ?
C26 C25 C24 173(2) . . ?
C1A C2B C2A 54.8(10) 8_556 . ?
C1A C2B C8 94.3(11) 8_556 . ?
C2A C2B C8 45.8(7) . . ?
C2A C1B C1A 73.1(12) 8_455 . ?
C2A C1B C3 131.7(14) 8_455 . ?
C1A C1B C3 63.7(11) . . ?
C2A C1B C2 161.7(14) 8_455 . ?
C1A C1B C2 112.5(13) . . ?
C3 C1B C2 48.9(6) . . ?
C1B C1A C2B 126.2(16) . 8_455 ?
C1B C1A C2A 49.3(10) . 8_455 ?
C2B C1A C2A 79.5(15) 8_455 8_455 ?
C1B C1A C3 70.9(12) . . ?
C2B C1A C3 137.5(17) 8_455 . ?
C2A C1A C3 116.7(15) 8_455 . ?
C1B C2A C1A 57.6(12) 8_556 8_556 ?
C1B C2A C8 160.0(17) 8_556 . ?
C1A C2A C8 112.4(15) 8_556 . ?
C1B C2A C2B 101.5(12) 8_556 . ?
C1A C2A C2B 45.7(10) 8_556 . ?
C8 C2A C2B 75.0(10) . . ?
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              26.37
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    2.514
_refine_diff_density_min   -0.918
_refine_diff_density_rms    0.140
