#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/87/2238712.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2238712
loop_
_publ_author_name
'Sim, Jaeung'
'Kim, Taemin'
'Yang, Jin Kuk'
_publ_section_title
;
 Poly[(μ₆-benzene-1,3,5-tricarboxylato-κ⁶O¹:O^1'^:O³:O^3'^:O⁵:O^5'^)tris(N,N-dimethylformamide-κO)tris(μ₃-formato-κ³O:O:O')trizinc(II)]
;
_journal_coeditor_code           CV5429
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m619
_journal_paper_doi               10.1107/S1600536813028687
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Zn3 (H C O2)3 (C9 H3 O6) (C3 H7 N O)3]'
_chemical_formula_moiety         'C21 H27 N3 O15 Zn3'
_chemical_formula_sum            'C21 H27 N3 O15 Zn3'
_chemical_formula_weight         757.56
_chemical_name_systematic
Poly[(μ₆-benzene-1,3,5-tricarboxylato-κ⁶O¹:O^1'^:O³:O^3'^:O⁵:O^5'^)tris(N,N-dimethylformamide-κO)tris(μ₃-formato-κ³O:O:O')trizinc(II)]
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.8594(17)
_cell_length_b                   13.8594(17)
_cell_length_c                   8.0100(14)
_cell_measurement_reflns_used    2269
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.209
_cell_measurement_theta_min      2.365
_cell_volume                     1332.5(3)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'CrystalMaker (CrystalMaker, 2013)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_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  0.1533
_diffrn_reflns_av_sigmaI/netI    0.0991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.543
_diffrn_reflns_theta_min         1.697
_exptl_absorpt_coefficient_mu    2.760
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_description       column
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.792
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.809
_refine_ls_goodness_of_fit_ref   0.809
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.809
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0317P)²+0.1686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                1563
_reflns_number_total             2027
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cv5429.cif
_cod_data_source_block           I
_cod_original_cell_volume        1332.5(4)
_cod_database_code               2238712
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Zn Zn1 0.01272(3) 0.23313(3) 0.39911(5) 0.01217(12) Uani d 1
O O1 -0.25265(17) 0.12229(17) 0.4805(3) 0.0160(5) Uani d 1
O O2 -0.10070(17) 0.28429(17) 0.4230(3) 0.0149(5) Uani d 1
O O3 -0.05005(17) 0.13366(17) 0.6162(3) 0.0140(5) Uani d 1
O O4 0.10436(18) 0.19215(19) 0.7680(3) 0.0162(5) Uani d 1
C C1 -0.2019(3) 0.2249(2) 0.4582(4) 0.0115(6) Uani d 1
C C2 -0.2697(3) 0.2816(2) 0.4691(4) 0.0113(6) Uani d 1
C C3 -0.3856(3) 0.2180(3) 0.4700(3) 0.0130(7) Uani d 1
H H3 -0.4213 0.1390 0.4712 0.016 Uiso calc 1
C C4 0.0026(3) 0.1477(3) 0.7513(4) 0.0140(7) Uani d 1
H H4 -0.0408 0.1214 0.8502 0.017 Uiso calc 1
O O5 0.07684(19) 0.32946(18) 0.1759(3) 0.0198(5) Uani d 1
N N1 0.0391(2) 0.3985(2) -0.0540(3) 0.0204(6) Uani d 1
C C5 0.0119(3) 0.3253(3) 0.0664(4) 0.0203(8) Uani d 1
H H5 -0.0626 0.2651 0.0699 0.024 Uiso calc 1
C C6 0.1529(3) 0.4921(3) -0.0652(5) 0.0286(9) Uani d 1
H H6A 0.1890 0.5051 0.0442 0.043 Uiso calc 1
H H6B 0.1514 0.5590 -0.1003 0.043 Uiso calc 1
H H6C 0.1948 0.4749 -0.1470 0.043 Uiso calc 1
C C7 -0.0372(3) 0.3837(3) -0.1897(4) 0.0294(9) Uani d 1
H H7A -0.1092 0.3163 -0.1697 0.044 Uiso calc 1
H H7B -0.0061 0.3762 -0.2956 0.044 Uiso calc 1
H H7C -0.0477 0.4485 -0.1951 0.044 Uiso calc 1
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Zn1 O2 5_556 . 87.25(9)
O1 Zn1 O4 5_556 6_556 168.88(9)
O2 Zn1 O4 . 6_556 93.23(9)
O1 Zn1 O3 5_556 5_556 90.61(8)
O2 Zn1 O3 . 5_556 177.54(9)
O4 Zn1 O3 6_556 5_556 89.09(8)
O1 Zn1 O3 5_556 . 96.06(9)
O2 Zn1 O3 . . 90.70(8)
O4 Zn1 O3 6_556 . 95.05(8)
O3 Zn1 O3 5_556 . 88.32(10)
O1 Zn1 O5 5_556 . 85.20(9)
O2 Zn1 O5 . . 90.77(9)
O4 Zn1 O5 6_556 . 83.68(8)
O3 Zn1 O5 5_556 . 90.26(9)
O3 Zn1 O5 . . 178.11(9)
C1 O1 Zn1 . 6_556 135.5(2)
C1 O2 Zn1 . . 126.83(19)
C4 O3 Zn1 . 6_556 120.2(2)
C4 O3 Zn1 . . 125.8(2)
Zn1 O3 Zn1 6_556 . 113.73(10)
C4 O4 Zn1 . 5_556 132.5(2)
O1 C1 O2 . . 126.2(3)
O1 C1 C2 . . 116.5(3)
O2 C1 C2 . . 117.3(3)
C3 C2 C3 2_565 . 119.9(3)
C3 C2 C1 2_565 . 120.3(3)
C3 C2 C1 . . 119.7(3)
C2 C3 C2 3_455 . 120.1(3)
C2 C3 H3 3_455 . 120.0
C2 C3 H3 . . 120.0
O4 C4 O3 . . 126.7(3)
O4 C4 H4 . . 116.6
O3 C4 H4 . . 116.6
C5 O5 Zn1 . . 119.8(2)
C5 N1 C7 . . 122.1(3)
C5 N1 C6 . . 119.8(3)
C7 N1 C6 . . 117.7(3)
O5 C5 N1 . . 124.4(3)
O5 C5 H5 . . 117.8
N1 C5 H5 . . 117.8
N1 C6 H6A . . 109.5
N1 C6 H6B . . 109.5
H6A C6 H6B . . 109.5
N1 C6 H6C . . 109.5
H6A C6 H6C . . 109.5
H6B C6 H6C . . 109.5
N1 C7 H7A . . 109.5
N1 C7 H7B . . 109.5
H7A C7 H7B . . 109.5
N1 C7 H7C . . 109.5
H7A C7 H7C . . 109.5
H7B C7 H7C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Zn1 O1 5_556 2.028(2)
Zn1 O2 . 2.031(2)
Zn1 O4 6_556 2.105(2)
Zn1 O3 5_556 2.108(2)
Zn1 O3 . 2.117(2)
Zn1 O5 . 2.140(2)
O1 C1 . 1.245(3)
O1 Zn1 6_556 2.028(2)
O2 C1 . 1.253(4)
O3 C4 . 1.265(4)
O3 Zn1 6_556 2.108(2)
O4 C4 . 1.232(4)
O4 Zn1 5_556 2.105(2)
C1 C2 . 1.499(4)
C2 C3 2_565 1.380(4)
C2 C3 . 1.394(4)
C3 C2 3_455 1.380(4)
C3 H3 . 0.9500
C4 H4 . 0.9500
O5 C5 . 1.237(4)
N1 C5 . 1.311(4)
N1 C7 . 1.458(4)
N1 C6 . 1.460(5)
C5 H5 . 0.9500
C6 H6A . 0.9800
C6 H6B . 0.9800
C6 H6C . 0.9800
C7 H7A . 0.9800
C7 H7B . 0.9800
C7 H7C . 0.9800
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
Zn1 O1 C1 O2 6_556 . 42.6(5)
Zn1 O1 C1 C2 6_556 . -139.5(2)
Zn1 O2 C1 O1 . . -2.2(5)
Zn1 O2 C1 C2 . . 179.99(19)
O1 C1 C2 C3 . 2_565 170.7(3)
O2 C1 C2 C3 . 2_565 -11.3(4)
O1 C1 C2 C3 . . -12.5(4)
O2 C1 C2 C3 . . 165.5(3)
C3 C2 C3 C2 2_565 3_455 1.0(6)
C1 C2 C3 C2 . 3_455 -175.8(2)
Zn1 O4 C4 O3 5_556 . -21.4(5)
Zn1 O3 C4 O4 6_556 . 159.8(3)
Zn1 O3 C4 O4 . . -26.7(4)
Zn1 O5 C5 N1 . . 163.2(2)
C7 N1 C5 O5 . . 173.5(3)
C6 N1 C5 O5 . . 0.5(5)
