#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/46/7214628.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_7214628
loop_
_publ_author_name
'Duan, Chunmei'
'Luo, Daibing'
'Zeng, Hongmei'
'Kang, Maoping'
'Lin, Zhien'
_publ_section_title
;
 Solvent-free synthesis of new open-framework oxalate structures
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              5734
_journal_paper_doi               10.1039/c2ce25856k
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C8 H12.8 N2 O7.4 Zn'
_chemical_formula_weight         320.77
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 114.50(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.884(3)
_cell_length_b                   12.146(2)
_cell_length_c                   16.327(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2505.4(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Eos'
_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    0.0289
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9114
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.992
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0362
_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)+(0.0526P)²+2.8353P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                1855
_reflns_number_total             2197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25856k.txt
_cod_data_source_block           4
_cod_original_cell_volume        2505.3(9)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C8 H12.80 N2 O7.40 Zn'
_cod_database_code               7214628
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'
'-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
Zn1 Zn 0.42955(3) 0.20855(3) 0.47951(3) 0.04322(18) Uani 1 1 d .
O1 O 0.46661(18) 0.08792(17) 0.40780(15) 0.0435(5) Uani 1 1 d .
O2 O 0.5127(2) -0.08829(18) 0.42142(15) 0.0495(6) Uani 1 1 d .
O3 O 0.3775(2) 0.29959(18) 0.56128(17) 0.0490(6) Uani 1 1 d .
O4 O 0.22838(19) 0.3385(2) 0.57417(17) 0.0519(6) Uani 1 1 d .
O5 O 0.56533(18) 0.30080(19) 0.51829(17) 0.0533(7) Uani 1 1 d .
O6 O 0.3887(2) 0.3257(2) 0.36883(17) 0.0559(6) Uani 1 1 d .
O7 O 0.6266(2) 0.4591(2) 0.4910(2) 0.0712(8) Uani 1 1 d .
N1 N 0.4466(3) 0.4917(3) 0.3445(2) 0.0630(9) Uani 1 1 d .
H1A H 0.4977 0.5384 0.3639 0.076 Uiso 1 1 calc R
N2 N 0.2309(2) 0.5722(3) 0.3352(2) 0.0618(9) Uani 1 1 d .
H2A H 0.2829 0.5589 0.3908 0.074 Uiso 1 1 calc R
C1 C 0.4939(2) -0.0003(3) 0.4510(2) 0.0364(7) Uani 1 1 d .
C2 C 0.2804(3) 0.2898(2) 0.5392(2) 0.0407(8) Uani 1 1 d .
C3 C 0.5593(3) 0.3858(3) 0.4733(3) 0.0498(9) Uani 1 1 d .
C4 C 0.4563(3) 0.3995(3) 0.3896(3) 0.0495(9) Uani 1 1 d .
C5 C 0.3531(4) 0.5181(4) 0.2631(3) 0.0738(13) Uani 1 1 d .
H5A H 0.3119 0.4515 0.2411 0.089 Uiso 1 1 calc R
H5B H 0.3757 0.5429 0.2174 0.089 Uiso 1 1 calc R
C6 C 0.2832(3) 0.6046(4) 0.2756(3) 0.0674(12) Uani 1 1 d .
H6A H 0.3254 0.6700 0.3003 0.081 Uiso 1 1 calc R
H6B H 0.2289 0.6239 0.2169 0.081 Uiso 1 1 calc R
C7 C 0.1680(4) 0.6677(5) 0.3436(4) 0.101(2) Uani 1 1 d .
H7A H 0.1340 0.6481 0.3821 0.152 Uiso 1 1 calc R
H7B H 0.1154 0.6872 0.2852 0.152 Uiso 1 1 calc R
H7C H 0.2142 0.7293 0.3690 0.152 Uiso 1 1 calc R
C8 C 0.1655(3) 0.4704(4) 0.3059(4) 0.0870(15) Uani 1 1 d .
H8A H 0.1352 0.4539 0.3477 0.130 Uiso 1 1 calc R
H8B H 0.2093 0.4101 0.3041 0.130 Uiso 1 1 calc R
H8C H 0.1100 0.4816 0.2471 0.130 Uiso 1 1 calc R
OW1 O 0.5000 0.2960(10) 0.7500 0.101(4) Uani 0.50 2 d SP
OW2 O 0.2817(16) 0.8984(17) 0.4190(15) 0.080(6) Uani 0.15 1 d P
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
O5 Zn1 O1 98.56(10) . .
O5 Zn1 O4 162.53(10) . 7_556
O1 Zn1 O4 91.91(9) . 7_556
O5 Zn1 O2 97.75(10) . 5_656
O1 Zn1 O2 80.58(9) . 5_656
O4 Zn1 O2 97.73(11) 7_556 5_656
O5 Zn1 O3 91.77(10) . .
O1 Zn1 O3 166.80(9) . .
O4 Zn1 O3 80.21(9) 7_556 .
O2 Zn1 O3 89.93(9) 5_656 .
O5 Zn1 O6 77.85(10) . .
O1 Zn1 O6 91.89(10) . .
O4 Zn1 O6 87.91(11) 7_556 .
O2 Zn1 O6 170.70(10) 5_656 .
O3 Zn1 O6 98.34(10) . .
C1 O1 Zn1 112.04(19) . .
C1 O2 Zn1 112.2(2) . 5_656
C2 O3 Zn1 112.6(2) . .
C2 O4 Zn1 112.9(2) . 7_556
C3 O5 Zn1 116.1(2) . .
C4 O6 Zn1 109.7(2) . .
C4 N1 C5 123.0(4) . .
C4 N1 H1A 118.5 . .
C5 N1 H1A 118.5 . .
C6 N2 C8 114.0(4) . .
C6 N2 C7 108.5(3) . .
C8 N2 C7 111.9(4) . .
C6 N2 H2A 107.4 . .
C8 N2 H2A 107.4 . .
C7 N2 H2A 107.4 . .
O2 C1 O1 125.4(3) . .
O2 C1 C1 117.2(3) . 5_656
O1 C1 C1 117.3(3) . 5_656
O4 C2 O3 125.9(3) . .
O4 C2 C2 117.2(4) . 7_556
O3 C2 C2 116.9(4) . 7_556
O7 C3 O5 126.7(4) . .
O7 C3 C4 117.9(3) . .
O5 C3 C4 115.3(3) . .
O6 C4 N1 124.9(4) . .
O6 C4 C3 119.3(3) . .
N1 C4 C3 115.9(3) . .
N1 C5 C6 114.4(4) . .
N1 C5 H5A 108.7 . .
C6 C5 H5A 108.7 . .
N1 C5 H5B 108.7 . .
C6 C5 H5B 108.7 . .
H5A C5 H5B 107.6 . .
N2 C6 C5 114.9(3) . .
N2 C6 H6A 108.5 . .
C5 C6 H6A 108.5 . .
N2 C6 H6B 108.5 . .
C5 C6 H6B 108.5 . .
H6A C6 H6B 107.5 . .
N2 C7 H7A 109.5 . .
N2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N2 C8 H8A 109.5 . .
N2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
N2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O5 2.054(2) .
Zn1 O1 2.069(2) .
Zn1 O4 2.075(3) 7_556
Zn1 O2 2.078(2) 5_656
Zn1 O3 2.080(2) .
Zn1 O6 2.182(2) .
O1 C1 1.252(4) .
O2 C1 1.244(4) .
O2 Zn1 2.078(2) 5_656
O3 C2 1.249(4) .
O4 C2 1.241(4) .
O4 Zn1 2.075(3) 7_556
O5 C3 1.249(4) .
O6 C4 1.240(4) .
O7 C3 1.235(4) .
N1 C4 1.316(5) .
N1 C5 1.456(5) .
N1 H1A 0.8600 .
N2 C6 1.490(5) .
N2 C8 1.491(6) .
N2 C7 1.493(6) .
N2 H2A 0.9100 .
C1 C1 1.537(6) 5_656
C2 C2 1.545(6) 7_556
C3 C4 1.522(5) .
C5 C6 1.500(6) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
