#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:31:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179505 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/02/4340224.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_4340224
loop_
_publ_author_name
'Ke, Yanxiong'
'Collins, David J.'
'Sun, Daofeng'
'Zhou, Hong-Cai'
_publ_section_title
;
 (10,3)-a Noninterpenetrated network built from a Piedfort ligand pair.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1897
_journal_page_last               1899
_journal_paper_doi               10.1021/ic051900p
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'Zn3 2(C27 H12 N7 O6) 2(H2O)'
_chemical_formula_sum            'C54 H28 N14 O14 Zn3'
_chemical_formula_weight         1293.01
_chemical_melting_point          ?
_chemical_name_common            'Zn3 (HTB)2 (H2O)2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           212
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 4acd 2ab 3'
_symmetry_space_group_name_H-M   'P 43 3 2'
_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                   29.497(2)
_cell_length_b                   29.497(2)
_cell_length_c                   29.497(2)
_cell_measurement_reflns_used    7638
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.87
_cell_measurement_theta_min      2.18
_cell_volume                     25665(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1164
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            62706
_diffrn_reflns_theta_full        17.21
_diffrn_reflns_theta_max         17.21
_diffrn_reflns_theta_min         0.98
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.335
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.70
_refine_diff_density_max         0.053
_refine_diff_density_min         -0.092
_refine_diff_density_rms         0.014
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.117(18)
_refine_ls_extinction_coef       0.000023(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.844
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.844
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0359P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                1660
_reflns_number_total             2610
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051900psi20060117_072953.cif
_cod_data_source_block           xamd333
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Cubic' changed to 'cubic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        25666(3)
_cod_original_sg_symbol_H-M      P4(3)32
_cod_database_code               4340224
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'y+3/4, -x+3/4, z+1/4'
'-y+3/4, x+1/4, z+3/4'
'x+1/4, z+3/4, -y+3/4'
'-x+3/4, z+1/4, y+3/4'
'-x+1/4, -z+1/4, -y+1/4'
'x+3/4, -z+3/4, y+1/4'
'z+1/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+1/4'
'-z+3/4, y+1/4, x+3/4'
'-z+1/4, -y+1/4, -x+1/4'
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 0.5123(3) 0.8372(2) 0.6132(4) 0.192(3) Uani 1 1 d .
C2 C 0.5478(4) 0.8258(3) 0.5826(3) 0.217(3) Uani 1 1 d .
H2 H 0.5507 0.8410 0.5551 0.261 Uiso 1 1 calc R
C3 C 0.5781(3) 0.7915(4) 0.5943(4) 0.220(3) Uani 1 1 d .
H3 H 0.6028 0.7849 0.5759 0.264 Uiso 1 1 calc R
C4 C 0.5702(4) 0.7654(2) 0.6374(5) 0.224(4) Uani 1 1 d .
C5 C 0.5363(4) 0.7781(4) 0.6651(3) 0.208(3) Uani 1 1 d .
H5 H 0.5320 0.7634 0.6926 0.249 Uiso 1 1 calc R
C6 C 0.5091(3) 0.8120(4) 0.6531(3) 0.195(2) Uani 1 1 d .
H6 H 0.4859 0.8195 0.6730 0.234 Uiso 1 1 calc R
C7 C 0.4769(3) 0.8723(3) 0.6035(3) 0.303(7) Uani 1 1 d .
C8 C 0.6042(3) 0.7236(4) 0.6445(5) 0.242(6) Uani 1 1 d .
C9 C 0.6649(5) 0.6839(3) 0.6249(3) 0.196(3) Uani 1 1 d .
N1 N 0.6385(3) 0.7205(3) 0.6143(2) 0.202(2) Uani 1 1 d .
N2 N 0.59461(17) 0.6998(4) 0.6796(3) 0.196(2) Uani 1 1 d .
N3 N 0.65757(14) 0.65757(14) 0.65757(14) 0.165(3) Uani 1 3 d S
O1 O 0.48427(12) 0.89606(13) 0.56887(13) 0.2213(16) Uani 1 1 d .
O2 O 0.43765(13) 0.87382(19) 0.62913(16) 0.255(2) Uani 1 1 d .
O3 O 0.48549(10) 0.98549(10) 0.51451(10) 0.281(2) Uani 1 3 d S
Zn1 Zn 0.3750 0.8750 0.6250 0.1728(5) Uani 1 6 d S
Zn2 Zn 0.444937(18) 0.944937(18) 0.555063(18) 0.1970(5) Uani 1 3 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
C6 C1 C2 117.4(8) . .
C6 C1 C7 118.8(12) . .
C2 C1 C7 123.6(10) . .
C3 C2 C1 118.9(9) . .
C3 C2 H2 120.5 . .
C1 C2 H2 120.5 . .
C2 C3 C4 118.9(9) . .
C2 C3 H3 120.6 . .
C4 C3 H3 120.6 . .
C5 C4 C3 119.0(9) . .
C5 C4 C8 127.0(16) . .
C3 C4 C8 114.0(15) . .
C6 C5 C4 119.7(10) . .
C6 C5 H5 120.1 . .
C4 C5 H5 120.1 . .
C5 C6 C1 125.8(9) . .
C5 C6 H6 117.1 . .
C1 C6 H6 117.1 . .
O1 C7 O2 124.8(9) . .
O1 C7 C1 114.8(9) . .
O2 C7 C1 120.0(8) . .
N2 C8 N1 131.3(11) . .
N2 C8 C4 112.8(13) . .
N1 C8 C4 115.8(15) . .
N3 C9 N1 124.4(10) . .
N3 C9 N2 124.9(10) . 9
N1 C9 N2 110.6(9) . 9
C8 N1 C9 109.2(11) . .
C8 N2 C9 110.1(9) . 5
C9 N3 C9 119.984(18) 5 .
C9 N3 C9 119.984(18) 5 9
C9 N3 C9 119.984(18) . 9
C7 O1 Zn2 119.5(6) . .
C7 O2 Zn1 143.1(5) . .
O2 Zn1 O2 82.5(3) 8_656 18_554
O2 Zn1 O2 88.1(3) 8_656 22_465
O2 Zn1 O2 94.8(2) 18_554 22_465
O2 Zn1 O2 94.8(2) 8_656 .
O2 Zn1 O2 176.2(3) 18_554 .
O2 Zn1 O2 82.5(3) 22_465 .
O2 Zn1 O2 94.8(2) 8_656 11_466
O2 Zn1 O2 88.1(3) 18_554 11_466
O2 Zn1 O2 176.2(3) 22_465 11_466
O2 Zn1 O2 94.8(2) . 11_466
O2 Zn1 O2 176.2(3) 8_656 14_666
O2 Zn1 O2 94.8(2) 18_554 14_666
O2 Zn1 O2 94.8(2) 22_465 14_666
O2 Zn1 O2 88.1(3) . 14_666
O2 Zn1 O2 82.5(3) 11_466 14_666
O1 Zn2 O1 115.72(8) 8_656 .
O1 Zn2 O1 115.72(8) 8_656 11_466
O1 Zn2 O1 115.72(8) . 11_466
O1 Zn2 O3 102.12(11) 8_656 .
O1 Zn2 O3 102.12(12) . .
O1 Zn2 O3 102.12(11) 11_466 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.394(6) .
C1 C2 1.423(6) .
C1 C7 1.500(10) .
C2 C3 1.394(7) .
C2 H2 0.9300 .
C3 C4 1.504(9) .
C3 H3 0.9300 .
C4 C5 1.345(10) .
C4 C8 1.602(11) .
C5 C6 1.330(7) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 O1 1.257(8) .
C7 O2 1.383(11) .
C8 N2 1.283(9) .
C8 N1 1.350(8) .
C9 N3 1.256(8) .
C9 N1 1.369(6) .
C9 N2 1.369(7) 9
N2 C9 1.369(7) 5
N3 C9 1.256(8) 5
N3 C9 1.256(8) 9
O1 Zn2 1.895(4) .
O2 Zn1 1.852(4) .
O3 Zn2 2.072(5) .
Zn1 O2 1.852(4) 8_656
Zn1 O2 1.852(4) 18_554
Zn1 O2 1.852(4) 22_465
Zn1 O2 1.852(4) 11_466
Zn1 O2 1.852(4) 14_666
Zn2 O1 1.895(4) 8_656
Zn2 O1 1.895(4) 11_466
