#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:50:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179396 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/93/4329346.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_4329346
loop_
_publ_author_name
'Daniel Lässig'
'Jörg Lincke'
'Renata Gerhardt'
'Harald Krautscheid'
_publ_contact_author_address
;
Universität Leipzig
Fakultät für Chemie und Mineralogie
Institut für Anorganische  Chemie
Johannisallee 29
D-04103 Leipzig
Germany
;
_publ_contact_author_email       Krautscheid@rz.uni-leipzig.de
_publ_contact_author_fax         00493419736199
_publ_contact_author_name
;
Harald Krautscheid
;
_publ_contact_author_phone       00493419736172
_publ_section_title
;
 Solid-State Syntheses of Coordination Polymers by Thermal Conversion of
 Molecular Building Blocks and Polymeric Precursors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6180
_journal_page_last               6189
_journal_paper_doi               10.1021/ic300235s
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C20 H16 N6 O4 Zn'
_chemical_formula_sum            'C20 H16 N6 O4 Zn'
_chemical_formula_weight         469.76
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 98.544(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6474(9)
_cell_length_b                   19.167(2)
_cell_length_c                   15.366(3)
_cell_measurement_reflns_used    8278
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.90
_cell_volume                     1936.1(5)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA, STOE X-RED'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement
'SHELXL-97 Sheldrick, G. M. (2008) Acta Cryst.'
_computing_structure_solution
'SHELXS-97 Sheldrick, G. M. (2008) Acta Cryst.'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'STOE IPDS-I'
_diffrn_measurement_method       'ω 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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4644
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         1.90
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       needle
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3291
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0280
_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)+(0.0502P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                3141
_reflns_number_total             3291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300235s_si_002_9.cif
_cod_data_source_block           compound_6
_cod_original_cell_volume        1936.0(5)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4329346
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'
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
C1 C 0.0922(5) 0.41818(14) 0.3584(2) 0.0334(7) Uani 1 1 d .
C2 C 0.2246(5) 0.45432(15) 0.2990(2) 0.0307(6) Uani 1 1 d .
C3 C 0.4217(6) 0.47585(15) 0.3306(2) 0.0334(6) Uani 1 1 d .
H3 H 0.4706 0.4731 0.3911 0.040 Uiso 1 1 calc R
C4 C 0.5469(5) 0.50152(16) 0.2729(2) 0.0345(7) Uani 1 1 d .
H4 H 0.6811 0.5154 0.2937 0.041 Uiso 1 1 calc R
C5 C 0.4692(5) 0.50621(14) 0.1838(2) 0.0324(7) Uani 1 1 d .
C6 C 0.2693(5) 0.48871(17) 0.1518(2) 0.0389(7) Uani 1 1 d .
H6 H 0.2176 0.4945 0.0919 0.047 Uiso 1 1 calc R
C7 C 0.1464(5) 0.46230(17) 0.2102(2) 0.0374(7) Uani 1 1 d .
H7 H 0.0108 0.4499 0.1897 0.045 Uiso 1 1 calc R
C8 C 0.6316(9) 0.40174(19) 0.0628(4) 0.0670(14) Uani 1 1 d .
H8A H 0.4948 0.3947 0.0321 0.100 Uiso 1 1 calc R
H8B H 0.6408 0.3839 0.1224 0.100 Uiso 1 1 calc R
H8C H 0.7277 0.3772 0.0322 0.100 Uiso 1 1 calc R
C9 C 0.6799(5) 0.47757(15) 0.0657(2) 0.0330(6) Uani 1 1 d .
C10 C 0.6976(6) 0.58512(14) 0.1081(2) 0.0380(7) Uani 1 1 d .
H10 H 0.6790 0.6269 0.1380 0.046 Uiso 1 1 calc R
C11 C 0.2971(5) 0.27622(16) 0.5960(2) 0.0297(6) Uani 1 1 d .
C12 C 0.4709(5) 0.26263(14) 0.66979(19) 0.0271(6) Uani 1 1 d .
C13 C 0.4729(5) 0.29268(16) 0.75294(19) 0.0304(6) Uani 1 1 d .
H13 H 0.3567 0.3162 0.7657 0.037 Uiso 1 1 calc R
C14 C 0.6445(5) 0.28836(16) 0.8174(2) 0.0312(6) Uani 1 1 d .
H14 H 0.6431 0.3076 0.8736 0.037 Uiso 1 1 calc R
C15 C 0.8177(5) 0.25504(14) 0.79685(19) 0.0260(6) Uani 1 1 d .
C16 C 0.8171(5) 0.22292(16) 0.7151(2) 0.0316(6) Uani 1 1 d .
H16 H 0.9337 0.1997 0.7024 0.038 Uiso 1 1 calc R
C17 C 0.6432(5) 0.22560(15) 0.6528(2) 0.0316(6) Uani 1 1 d .
H17 H 0.6407 0.2024 0.5988 0.038 Uiso 1 1 calc R
C18 C 1.0471(7) 0.38557(15) 0.8839(3) 0.0474(9) Uani 1 1 d .
H18A H 0.9349 0.3959 0.9156 0.071 Uiso 1 1 calc R
H18B H 1.0047 0.3932 0.8215 0.071 Uiso 1 1 calc R
H18C H 1.1610 0.4159 0.9047 0.071 Uiso 1 1 calc R
C19 C 1.1099(5) 0.31120(14) 0.89921(19) 0.0280(6) Uani 1 1 d .
C20 C 1.1187(5) 0.19898(15) 0.8879(2) 0.0310(6) Uani 1 1 d .
H20 H 1.0859 0.1526 0.8718 0.037 Uiso 1 1 calc R
N1 N 0.8154(5) 0.57803(12) 0.04816(19) 0.0306(6) Uani 1 1 d .
N2 N 0.8043(4) 0.50923(12) 0.02018(17) 0.0332(5) Uani 1 1 d .
N3 N 0.6053(4) 0.52343(12) 0.12143(18) 0.0319(6) Uani 1 1 d .
N4 N 1.2820(4) 0.21786(11) 0.94150(17) 0.0284(5) Uani 1 1 d .
N5 N 1.2767(4) 0.29063(11) 0.94903(16) 0.0283(5) Uani 1 1 d .
N6 N 1.0028(4) 0.25520(12) 0.85878(16) 0.0269(5) Uani 1 1 d .
O1 O 0.1844(4) 0.40132(13) 0.43602(17) 0.0401(6) Uani 1 1 d .
O2 O -0.0884(4) 0.40582(13) 0.33056(18) 0.0482(6) Uani 1 1 d .
O3 O 0.1586(4) 0.31802(12) 0.61360(15) 0.0375(5) Uani 1 1 d .
O4 O 0.2997(4) 0.24980(13) 0.52260(16) 0.0437(6) Uani 1 1 d .
Zn1 Zn 0.00000(3) 0.348070(13) 0.50000(2) 0.02514(9) Uani 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
O2 C1 O1 124.9(3) . .
O2 C1 C2 119.8(3) . .
O1 C1 C2 115.3(3) . .
C3 C2 C7 120.3(3) . .
C3 C2 C1 121.5(3) . .
C7 C2 C1 118.1(3) . .
C2 C3 C4 120.2(3) . .
C2 C3 H3 119.9 . .
C4 C3 H3 119.9 . .
C3 C4 C5 118.6(3) . .
C3 C4 H4 120.7 . .
C5 C4 H4 120.7 . .
C6 C5 C4 121.9(3) . .
C6 C5 N3 118.7(3) . .
C4 C5 N3 119.2(3) . .
C5 C6 C7 118.7(3) . .
C5 C6 H6 120.6 . .
C7 C6 H6 120.6 . .
C2 C7 C6 120.1(3) . .
C2 C7 H7 120.0 . .
C6 C7 H7 120.0 . .
C9 C8 H8A 109.5 . .
C9 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C9 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N2 C9 N3 110.6(2) . .
N2 C9 C8 126.0(3) . .
N3 C9 C8 123.3(3) . .
N1 C10 N3 110.3(3) . .
N1 C10 H10 124.8 . .
N3 C10 H10 124.8 . .
O4 C11 O3 123.8(3) . .
O4 C11 C12 119.9(3) . .
O3 C11 C12 116.2(3) . .
C13 C12 C17 118.7(3) . .
C13 C12 C11 121.0(3) . .
C17 C12 C11 120.0(3) . .
C14 C13 C12 121.3(3) . .
C14 C13 H13 119.4 . .
C12 C13 H13 119.4 . .
C15 C14 C13 118.8(3) . .
C15 C14 H14 120.6 . .
C13 C14 H14 120.6 . .
C14 C15 C16 120.9(3) . .
C14 C15 N6 120.2(3) . .
C16 C15 N6 118.9(3) . .
C17 C16 C15 119.6(3) . .
C17 C16 H16 120.2 . .
C15 C16 H16 120.2 . .
C16 C17 C12 120.6(3) . .
C16 C17 H17 119.7 . .
C12 C17 H17 119.7 . .
C19 C18 H18A 109.5 . .
C19 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C19 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
N5 C19 N6 111.3(2) . .
N5 C19 C18 124.8(3) . .
N6 C19 C18 123.8(3) . .
N4 C20 N6 111.3(3) . .
N4 C20 H20 124.4 . .
N6 C20 H20 124.4 . .
C10 N1 N2 108.0(2) . .
C10 N1 Zn1 129.0(2) . 2_664
N2 N1 Zn1 122.99(19) . 2_664
C9 N2 N1 106.5(2) . .
C10 N3 C9 104.5(2) . .
C10 N3 C5 129.5(3) . .
C9 N3 C5 125.9(2) . .
C20 N4 N5 107.3(2) . .
C20 N4 Zn1 125.17(19) . 4_655
N5 N4 Zn1 127.5(2) . 4_655
C19 N5 N4 106.3(2) . .
C20 N6 C19 103.8(3) . .
C20 N6 C15 127.0(3) . .
C19 N6 C15 129.1(2) . .
C1 O1 Zn1 110.1(2) . .
C11 O3 Zn1 107.5(2) . .
O1 Zn1 O3 107.51(11) . .
O1 Zn1 N4 123.97(11) . 4_354
O3 Zn1 N4 117.36(10) . 4_354
O1 Zn1 N1 105.60(10) . 2_465
O3 Zn1 N1 98.56(11) . 2_465
N4 Zn1 N1 99.29(11) 4_354 2_465
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.236(4) .
C1 O1 1.298(4) .
C1 C2 1.525(4) .
C2 C3 1.391(5) .
C2 C7 1.393(5) .
C3 C4 1.393(5) .
C3 H3 0.9400 .
C4 C5 1.393(5) .
C4 H4 0.9400 .
C5 C6 1.388(5) .
C5 N3 1.450(4) .
C6 C7 1.396(4) .
C6 H6 0.9400 .
C7 H7 0.9400 .
C8 C9 1.488(4) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 H8C 0.9700 .
C9 N2 1.309(4) .
C9 N3 1.371(4) .
C10 N1 1.302(4) .
C10 N3 1.361(4) .
C10 H10 0.9400 .
C11 O4 1.238(4) .
C11 O3 1.280(4) .
C11 C12 1.517(4) .
C12 C13 1.400(4) .
C12 C17 1.405(4) .
C13 C14 1.397(4) .
C13 H13 0.9400 .
C14 C15 1.393(4) .
C14 H14 0.9400 .
C15 C16 1.399(4) .
C15 N6 1.440(4) .
C16 C17 1.387(5) .
C16 H16 0.9400 .
C17 H17 0.9400 .
C18 C19 1.494(4) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C18 H18C 0.9700 .
C19 N5 1.311(4) .
C19 N6 1.383(4) .
C20 N4 1.312(4) .
C20 N6 1.361(4) .
C20 H20 0.9400 .
N1 N2 1.385(3) .
N1 Zn1 2.081(3) 2_664
N4 N5 1.400(3) .
N4 Zn1 2.029(3) 4_655
O1 Zn1 1.967(2) .
O3 Zn1 1.986(2) .
Zn1 N4 2.029(3) 4_354
Zn1 N1 2.081(3) 2_465
