#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:50:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179396 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/93/4329345.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_4329345
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, 2.125(H2 O)'
_chemical_formula_sum            'C20 H20.25 N6 O6.125 Zn'
_chemical_formula_weight         508.04
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           104
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      104
_symmetry_space_group_name_Hall  'P 4 -2n'
_symmetry_space_group_name_H-M   'P 4 n c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5956(16)
_cell_length_b                   14.5956(16)
_cell_length_c                   12.8842(14)
_cell_measurement_reflns_used    5649
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      1.90
_cell_volume                     2744.7(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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7131
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.90
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  0.6520
_exptl_absorpt_correction_T_min  0.6520
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       block
_exptl_crystal_F_000             1045
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3019
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0541
_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)+(0.1118P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1582
_reflns_number_gt                1901
_reflns_number_total             3019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300235s_si_002_8.cif
_cod_data_source_block           compound_5
_cod_database_code               4329345
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, z+1/2'
'-x, -y, z'
'x+1/2, -y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y, -x, z'
'-y, x, z'
'y+1/2, x+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 0.6647(3) 0.9198(3) 0.0555(4) 0.0400(10) Uani 1 1 d .
C2 C 0.7266(3) 0.8711(3) 0.1301(3) 0.0409(10) Uani 1 1 d .
C3 C 0.7977(4) 0.8158(4) 0.0934(4) 0.0534(14) Uani 1 1 d .
H3 H 0.8083 0.8114 0.0216 0.064 Uiso 1 1 calc R
C4 C 0.8535(4) 0.7667(4) 0.1624(4) 0.0557(14) Uani 1 1 d .
H4 H 0.9015 0.7297 0.1380 0.067 Uiso 1 1 calc R
C5 C 0.8358(3) 0.7744(4) 0.2677(4) 0.0456(11) Uani 1 1 d .
C6 C 0.7663(4) 0.8272(4) 0.3050(4) 0.0493(12) Uani 1 1 d .
H6 H 0.7563 0.8312 0.3769 0.059 Uiso 1 1 calc R
C7 C 0.7109(4) 0.8746(4) 0.2375(4) 0.0490(12) Uani 1 1 d .
H7 H 0.6620 0.9096 0.2635 0.059 Uiso 1 1 calc R
C8 C 0.9393(5) 0.7583(4) 0.4212(5) 0.0653(16) Uani 1 1 d .
H8 H 0.9422 0.8212 0.4364 0.078 Uiso 1 1 calc R
C9 C 0.9053(3) 0.6305(3) 0.3447(4) 0.0395(10) Uani 1 1 d .
C10 C 0.8654(4) 0.5630(4) 0.2734(4) 0.0546(13) Uani 1 1 d .
H10A H 0.9043 0.5570 0.2127 0.082 Uiso 1 1 calc R
H10B H 0.8049 0.5832 0.2522 0.082 Uiso 1 1 calc R
H10C H 0.8606 0.5042 0.3081 0.082 Uiso 1 1 calc R
N2 N 0.9802(3) 0.6952(3) 0.4760(3) 0.0576(12) Uani 1 1 d .
N1 N 0.9583(3) 0.6138(3) 0.4260(3) 0.0416(9) Uani 1 1 d .
N3 N 0.8917(3) 0.7225(3) 0.3395(3) 0.0456(10) Uani 1 1 d .
O1 O 0.5957(2) 0.9599(3) 0.0973(3) 0.0461(8) Uani 1 1 d .
O2 O 0.6819(3) 0.9200(3) -0.0392(3) 0.0595(10) Uani 1 1 d .
O3 O 1.0000 1.0000 0.270(3) 0.063(8) Uani 0.25 4 d SP
O4 O 0.8368(8) 0.8925(12) 0.8326(10) 0.125(5) Uani 0.50 1 d P
O5 O 0.8262(8) 0.9172(10) 0.6106(9) 0.110(4) Uani 0.50 1 d P
ZN2 Zn 0.5000 1.0000 0.0000(2) 0.03534(18) Uani 1 2 d S
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 124.5(5) . .
O2 C1 C2 120.6(4) . .
O1 C1 C2 114.9(4) . .
C3 C2 C7 118.4(4) . .
C3 C2 C1 120.3(4) . .
C7 C2 C1 121.1(4) . .
C2 C3 C4 120.7(5) . .
C2 C3 H3 119.6 . .
C4 C3 H3 119.6 . .
C5 C4 C3 118.2(5) . .
C5 C4 H4 120.9 . .
C3 C4 H4 120.9 . .
C6 C5 C4 122.0(5) . .
C6 C5 N3 119.4(4) . .
C4 C5 N3 118.6(5) . .
C5 C6 C7 120.0(5) . .
C5 C6 H6 120.0 . .
C7 C6 H6 120.0 . .
C6 C7 C2 120.6(5) . .
C6 C7 H7 119.7 . .
C2 C7 H7 119.7 . .
N2 C8 N3 112.4(5) . .
N2 C8 H8 123.8 . .
N3 C8 H8 123.8 . .
N1 C9 N3 107.9(4) . .
N1 C9 C10 127.1(4) . .
N3 C9 C10 125.0(4) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C8 N2 N1 104.3(4) . .
C9 N1 N2 110.1(4) . .
C9 N1 ZN2 134.8(3) . 2_645
N2 N1 ZN2 114.7(3) . 2_645
C9 N3 C8 105.4(4) . .
C9 N3 C5 129.1(4) . .
C8 N3 C5 125.5(4) . .
C1 O1 ZN2 115.3(3) . .
O1 ZN2 O1 100.8(2) 3_675 .
O1 ZN2 N1 105.75(16) 3_675 2_654
O1 ZN2 N1 109.48(17) . 2_654
O1 ZN2 N1 109.48(17) 3_675 4_464
O1 ZN2 N1 105.75(16) . 4_464
N1 ZN2 N1 123.3(3) 2_654 4_464
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.246(6) .
C1 O1 1.283(6) .
C1 C2 1.498(6) .
C2 C3 1.397(7) .
C2 C7 1.404(7) .
C3 C4 1.402(7) .
C3 H3 0.9400 .
C4 C5 1.385(7) .
C4 H4 0.9400 .
C5 C6 1.361(7) .
C5 N3 1.448(6) .
C6 C7 1.374(7) .
C6 H6 0.9400 .
C7 H7 0.9400 .
C8 N2 1.305(7) .
C8 N3 1.365(7) .
C8 H8 0.9400 .
C9 N1 1.325(6) .
C9 N3 1.359(6) .
C9 C10 1.469(7) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C10 H10C 0.9700 .
N2 N1 1.389(6) .
N1 ZN2 2.009(4) 2_645
O1 ZN2 1.966(4) .
ZN2 O1 1.966(4) 3_675
ZN2 N1 2.009(4) 2_654
ZN2 N1 2.009(4) 4_464
