#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:50:55 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178919 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/48/4114847.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_4114847
loop_
_publ_author_name
'Juan C. Noveron'
'Myoung Soo Lah'
'Rico E. Del Sesto'
'Atta M. Arif'
'Joel S. Miller'
'Peter J. Stang'
_publ_section_title
;
 Engineering the Structure and Magnetic Properties of Crystalline Solids
 via the Metal-Directed Self-Assembly of a Versatile Molecular Building
 Unit
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6613
_journal_page_last               6625
_journal_paper_doi               10.1021/ja0200241
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C26 H28 N6 O10 Zn'
_chemical_formula_weight         649.91
_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                 97.9708(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.4389(3)
_cell_length_b                   12.6873(2)
_cell_length_c                   14.7479(5)
_cell_measurement_reflns_used    12222
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     1378.45(8)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius COLLECT'
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      200(1)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi plus Omega scan'
_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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5788
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.50
_diffrn_standards_decay_%        <2.0
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.9101
_exptl_absorpt_correction_T_min  0.8311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0334
_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)+(0.0334P)²+0.6347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                2465
_reflns_number_total             3110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0200241_09.cif
_cod_data_source_block           Zn_complex9
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4114847
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
Zn1 Zn 1.0000 0.0000 0.0000 0.02153(11) Uani 1 2 d S
O1 O 0.7979(2) -0.14975(10) 0.43987(9) 0.0338(4) Uani 1 1 d .
O2 O 1.1832(2) 0.12912(11) 0.04126(10) 0.0285(3) Uani 1 1 d .
O3 O 0.76700(19) 0.09405(10) -0.05471(9) 0.0282(3) Uani 1 1 d .
O4 O 0.8858(2) 0.25128(11) -0.04670(11) 0.0380(4) Uani 1 1 d .
O5 O 0.6185(2) 0.22571(12) -0.12102(11) 0.0428(4) Uani 1 1 d .
N1 N 0.9100(2) 0.00489(11) 0.12737(11) 0.0223(3) Uani 1 1 d .
N2 N 0.7926(2) 0.02186(13) 0.39718(11) 0.0236(4) Uani 1 1 d .
N3 N 0.7566(2) 0.19121(12) -0.07450(11) 0.0259(4) Uani 1 1 d .
C1 C 0.9010(3) -0.08247(16) 0.17741(13) 0.0274(4) Uani 1 1 d .
C2 C 0.8613(3) -0.08401(15) 0.26586(13) 0.0275(4) Uani 1 1 d .
C3 C 0.8277(3) 0.01097(14) 0.30757(12) 0.0212(4) Uani 1 1 d .
C4 C 0.8302(3) 0.10216(15) 0.25462(13) 0.0270(4) Uani 1 1 d .
C5 C 0.8716(3) 0.09595(15) 0.16722(13) 0.0266(4) Uani 1 1 d .
C6 C 0.7769(3) -0.05739(14) 0.45897(13) 0.0220(4) Uani 1 1 d .
C7 C 0.7318(3) -0.02551(15) 0.55080(13) 0.0226(4) Uani 1 1 d .
C8 C 0.7287(3) -0.10531(18) 0.61551(15) 0.0358(5) Uani 1 1 d .
C9 C 0.6847(3) -0.0828(2) 0.70131(15) 0.0410(6) Uani 1 1 d .
C10 C 0.6442(3) 0.01864(19) 0.72472(14) 0.0353(5) Uani 1 1 d .
C11 C 0.6454(3) 0.09808(19) 0.66075(15) 0.0376(5) Uani 1 1 d .
C12 C 0.6883(3) 0.07634(17) 0.57422(14) 0.0326(5) Uani 1 1 d .
C13 C 1.3755(3) 0.12920(19) 0.0414(2) 0.0377(5) Uani 1 1 d .
H2O H 1.149(3) 0.186(2) 0.0346(17) 0.045(8) Uiso 1 1 d .
H2N H 0.781(3) 0.0827(19) 0.4131(15) 0.030(6) Uiso 1 1 d .
H1 H 0.926(3) -0.1488(18) 0.1487(15) 0.035(6) Uiso 1 1 d .
H2 H 0.857(3) -0.1472(18) 0.2957(15) 0.039(6) Uiso 1 1 d .
H4 H 0.806(3) 0.1636(17) 0.2791(14) 0.028(6) Uiso 1 1 d .
H5 H 0.881(3) 0.1573(17) 0.1319(14) 0.028(5) Uiso 1 1 d .
H8 H 0.757(3) -0.175(2) 0.6000(16) 0.049(7) Uiso 1 1 d .
H9 H 0.684(4) -0.132(2) 0.744(2) 0.066(9) Uiso 1 1 d .
H10 H 0.612(3) 0.0336(18) 0.7828(16) 0.033(6) Uiso 1 1 d .
H11 H 0.611(3) 0.165(2) 0.6745(17) 0.052(7) Uiso 1 1 d .
H12 H 0.688(3) 0.1294(18) 0.5298(16) 0.042(7) Uiso 1 1 d .
H13A H 1.432(5) 0.191(3) 0.070(2) 0.096(12) Uiso 1 1 d .
H13B H 1.428(4) 0.070(3) 0.074(2) 0.076(10) Uiso 1 1 d .
H13C H 1.403(5) 0.130(3) -0.019(3) 0.109(13) Uiso 1 1 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'
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
N1 Zn1 N1 180.00(8) 3_755 .
N1 Zn1 O2 89.57(6) 3_755 3_755
N1 Zn1 O2 90.43(6) . 3_755
N1 Zn1 O2 90.43(6) 3_755 .
N1 Zn1 O2 89.57(6) . .
O2 Zn1 O2 180.00(5) 3_755 .
N1 Zn1 O3 88.78(6) 3_755 3_755
N1 Zn1 O3 91.22(6) . 3_755
O2 Zn1 O3 97.35(5) 3_755 3_755
O2 Zn1 O3 82.65(5) . 3_755
N1 Zn1 O3 91.22(6) 3_755 .
N1 Zn1 O3 88.78(6) . .
O2 Zn1 O3 82.65(5) 3_755 .
O2 Zn1 O3 97.35(5) . .
O3 Zn1 O3 180.00(7) 3_755 .
C13 O2 Zn1 126.28(13) . .
C13 O2 H2O 107.9(19) . .
Zn1 O2 H2O 119.8(19) . .
N3 O3 Zn1 129.96(13) . .
C1 N1 C5 116.15(16) . .
C1 N1 Zn1 121.33(12) . .
C5 N1 Zn1 122.31(12) . .
C6 N2 C3 127.10(17) . .
C6 N2 H2N 118.7(15) . .
C3 N2 H2N 114.2(15) . .
O5 N3 O4 120.60(16) . .
O5 N3 O3 119.54(17) . .
O4 N3 O3 119.86(17) . .
N1 C1 C2 124.60(18) . .
N1 C1 H1 116.7(13) . .
C2 C1 H1 118.7(13) . .
C1 C2 C3 118.81(18) . .
C1 C2 H2 119.6(15) . .
C3 C2 H2 121.6(15) . .
N2 C3 C2 125.16(17) . .
N2 C3 C4 117.92(16) . .
C2 C3 C4 116.92(17) . .
C5 C4 C3 120.07(18) . .
C5 C4 H4 121.2(14) . .
C3 C4 H4 118.7(13) . .
N1 C5 C4 123.38(18) . .
N1 C5 H5 115.5(13) . .
C4 C5 H5 121.1(13) . .
O1 C6 N2 121.65(17) . .
O1 C6 C7 121.38(17) . .
N2 C6 C7 116.97(16) . .
C12 C7 C8 118.66(19) . .
C12 C7 C6 124.52(17) . .
C8 C7 C6 116.79(18) . .
C9 C8 C7 120.4(2) . .
C9 C8 H8 120.3(15) . .
C7 C8 H8 119.3(15) . .
C10 C9 C8 120.7(2) . .
C10 C9 H9 116.9(19) . .
C8 C9 H9 122.3(19) . .
C9 C10 C11 119.3(2) . .
C9 C10 H10 120.7(14) . .
C11 C10 H10 120.0(14) . .
C10 C11 C12 120.5(2) . .
C10 C11 H11 119.8(16) . .
C12 C11 H11 119.6(16) . .
C11 C12 C7 120.4(2) . .
C11 C12 H12 121.5(14) . .
C7 C12 H12 118.1(14) . .
O2 C13 H13A 112(2) . .
O2 C13 H13B 110.1(18) . .
H13A C13 H13B 108(3) . .
O2 C13 H13C 110(2) . .
H13A C13 H13C 105(3) . .
H13B C13 H13C 111(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 2.0809(15) 3_755
Zn1 N1 2.0809(15) .
Zn1 O2 2.1636(14) 3_755
Zn1 O2 2.1636(14) .
Zn1 O3 2.1659(13) 3_755
Zn1 O3 2.1659(13) .
O1 C6 1.220(2) .
O2 C13 1.431(3) .
O2 H2O 0.77(3) .
O3 N3 1.267(2) .
O4 N3 1.250(2) .
O5 N3 1.234(2) .
N1 C1 1.338(2) .
N1 C5 1.345(2) .
N2 C6 1.373(2) .
N2 C3 1.389(2) .
N2 H2N 0.81(2) .
C1 C2 1.377(3) .
C1 H1 0.97(2) .
C2 C3 1.391(3) .
C2 H2 0.92(2) .
C3 C4 1.398(3) .
C4 C5 1.368(3) .
C4 H4 0.89(2) .
C5 H5 0.94(2) .
C6 C7 1.495(3) .
C7 C12 1.387(3) .
C7 C8 1.394(3) .
C8 C9 1.380(3) .
C8 H8 0.95(3) .
C9 C10 1.377(3) .
C9 H9 0.89(3) .
C10 C11 1.381(3) .
C10 H10 0.94(2) .
C11 C12 1.385(3) .
C11 H11 0.92(3) .
C12 H12 0.94(2) .
C13 H13A 0.96(4) .
C13 H13B 0.95(3) .
C13 H13C 0.95(4) .
