#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:57:10 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180457 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/26/7212606.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_7212606
loop_
_publ_author_name
'Pan, Qinhe'
'Chen, Qiang'
'Song, Wei-Chao'
'Hu, Tong-Liang'
'Bu, Xian-He'
_publ_section_title
;
 Template-directed synthesis of three new open-framework metal(ii)
 oxalates using Co(iii) complex as template
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              4198
_journal_paper_doi               10.1039/c002658a
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C13 H34 Co N6 O19 Zn2'
_chemical_formula_weight         768.13
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.92(3)
_cell_angle_beta                 92.14(3)
_cell_angle_gamma                109.46(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9116(18)
_cell_length_b                   9.2445(18)
_cell_length_c                   18.724(4)
_cell_measurement_reflns_used    11268
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      3.1
_cell_volume                     1400.0(6)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  SHELXL
_computing_structure_solution    DirectMethod
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  SCX-MINI
_diffrn_measurement_method       multi-scan
_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  0.0760
_diffrn_reflns_av_sigmaI/netI    0.1099
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14301
_diffrn_reflns_theta_full        27.37
_diffrn_reflns_theta_max         27.37
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    2.377
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1445
_refine_ls_R_factor_gt           0.0811
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0381P)²+3.1723P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1491
_reflns_number_gt                3833
_reflns_number_total             6251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002658a.txt
_cod_data_source_block           Zn-1
_cod_original_cell_volume        1400.0(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7212606
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Zn1 Zn -0.51378(12) -0.21685(10) -0.42054(5) 0.0552(3) Uani 1 1 d
Zn2 Zn -0.41462(9) -0.15923(8) -0.12418(4) 0.0310(2) Uani 1 1 d
Co1 Co -0.09870(10) -0.31274(10) 0.22581(5) 0.0337(2) Uani 1 1 d
O1 O -0.6286(7) -0.6392(6) -0.5777(3) 0.0672(16) Uani 1 1 d
O2 O -0.6464(7) -0.4125(6) -0.5077(3) 0.0687(17) Uani 1 1 d
O3 O -0.6437(6) -0.0798(6) -0.4443(3) 0.0568(14) Uani 1 1 d
O4 O -0.6383(7) 0.0941(6) -0.5109(3) 0.0616(15) Uani 1 1 d
O5 O -0.6495(6) -0.2844(5) -0.3359(3) 0.0526(13) Uani 1 1 d
O6 O -0.6198(5) -0.2333(5) -0.2119(2) 0.0385(11) Uani 1 1 d
O7 O -0.3554(6) -0.0593(5) -0.3260(3) 0.0534(14) Uani 1 1 d
O8 O -0.3046(5) -0.0633(5) -0.2088(2) 0.0411(11) Uani 1 1 d
O9 O -0.4381(5) -0.3987(5) -0.1725(2) 0.0409(11) Uani 1 1 d
O10 O -0.2901(6) -0.5555(6) -0.1870(3) 0.0727(18) Uani 1 1 d
O11 O -0.1978(5) -0.1611(5) -0.0803(3) 0.0483(13) Uani 1 1 d
O12 O -0.0292(6) -0.2953(6) -0.1089(3) 0.0614(15) Uani 1 1 d
O13 O -0.3816(5) 0.0760(5) -0.0647(2) 0.0370(11) Uani 1 1 d
O14 O -0.4411(5) 0.2059(5) 0.0419(2) 0.0367(11) Uani 1 1 d
N1 N -0.2893(7) -0.3632(7) 0.2801(3) 0.0527(16) Uani 1 1 d
H1A H -0.3710 -0.4458 0.2510 0.080 Uiso 1 1 calc
H1B H -0.2654 -0.3900 0.3210 0.080 Uiso 1 1 calc
N2 N -0.1428(7) -0.1189(7) 0.2226(4) 0.0565(17) Uani 1 1 d
H2A H -0.0683 -0.0333 0.2540 0.080 Uiso 1 1 calc
H2B H -0.1375 -0.1060 0.1765 0.080 Uiso 1 1 calc
N3 N -0.2307(7) -0.4358(7) 0.1297(3) 0.0486(16) Uani 1 1 d
H3A H -0.2871 -0.5352 0.1319 0.080 Uiso 1 1 calc
H3B H -0.3007 -0.3898 0.1199 0.080 Uiso 1 1 calc
N4 N 0.0813(6) -0.2631(6) 0.1676(3) 0.0427(14) Uani 1 1 d
H4A H 0.1449 -0.1603 0.1856 0.080 Uiso 1 1 calc
H4B H 0.1402 -0.3241 0.1710 0.080 Uiso 1 1 calc
N5 N 0.0480(6) -0.2033(6) 0.3205(3) 0.0442(14) Uani 1 1 d
H5A H 0.1166 -0.1087 0.3177 0.080 Uiso 1 1 calc
H5B H -0.0092 -0.1856 0.3581 0.080 Uiso 1 1 calc
N6 N -0.0600(6) -0.5057(6) 0.2374(3) 0.0437(15) Uani 1 1 d
H6A H -0.1543 -0.5866 0.2310 0.080 Uiso 1 1 calc
H6B H -0.0008 -0.5346 0.2026 0.080 Uiso 1 1 calc
C1 C -0.3369(10) -0.2179(12) 0.3013(5) 0.077(3) Uani 1 1 d
H1C H -0.4497 -0.2500 0.3077 0.080 Uiso 1 1 calc
H1D H -0.2755 -0.1482 0.3481 0.080 Uiso 1 1 calc
C2 C -0.3079(13) -0.1321(13) 0.2442(7) 0.098(4) Uani 1 1 d
H2C H -0.3131 -0.0268 0.2631 0.080 Uiso 1 1 calc
H2D H -0.3886 -0.1891 0.2013 0.080 Uiso 1 1 calc
C3 C -0.1271(9) -0.4435(9) 0.0688(4) 0.052(2) Uani 1 1 d
H3C H -0.0939 -0.5350 0.0635 0.080 Uiso 1 1 calc
H3D H -0.1868 -0.4548 0.0221 0.080 Uiso 1 1 calc
C4 C 0.0172(9) -0.2939(9) 0.0873(4) 0.0507(19) Uani 1 1 d
H4C H -0.0121 -0.2056 0.0805 0.080 Uiso 1 1 calc
H4D H 0.0979 -0.3064 0.0555 0.080 Uiso 1 1 calc
C5 C 0.1387(9) -0.3035(9) 0.3347(4) 0.0517(19) Uani 1 1 d
H5C H 0.1815 -0.2712 0.3867 0.080 Uiso 1 1 calc
H5D H 0.2276 -0.2920 0.3055 0.080 Uiso 1 1 calc
C6 C 0.0268(10) -0.4727(9) 0.3136(4) 0.060(2) Uani 1 1 d
H6C H -0.0494 -0.4893 0.3491 0.080 Uiso 1 1 calc
H6D H 0.0864 -0.5436 0.3129 0.080 Uiso 1 1 calc
C7 C -0.5807(11) -0.5150(9) -0.5239(4) 0.061(2) Uani 1 1 d
C8 C -0.5810(9) 0.0043(8) -0.4871(4) 0.0491(19) Uani 1 1 d
C9 C -0.5717(8) -0.2201(7) -0.2727(4) 0.0348(15) Uani 1 1 d
C10 C -0.3937(8) -0.1036(7) -0.2685(4) 0.0357(16) Uani 1 1 d
C11 C -0.3096(8) -0.4273(7) -0.1619(4) 0.0386(16) Uani 1 1 d
C12 C -0.1653(8) -0.2827(8) -0.1130(4) 0.0425(17) Uani 1 1 d
C13 C -0.4488(7) 0.0815(7) -0.0071(4) 0.0317(15) Uani 1 1 d
O1W O -0.9677(12) -0.3535(15) -0.4751(6) 0.190(5) Uani 1 1 d
O2W O -0.4904(11) -0.3736(14) 0.0588(6) 0.188(5) Uani 1 1 d
O3W O -0.1226(11) -0.2059(12) -0.5465(4) 0.151(4) Uani 1 1 d
O4W O -0.0406(11) -0.1623(9) -0.3507(4) 0.137(3) Uani 1 1 d
O5W O 0.1942(6) 0.0243(6) -0.0759(3) 0.0572(14) 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'
Co Co 0.3494 0.9721 '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 Zn1 O3 92.4(2) . .
O2 Zn1 O7 165.7(2) . .
O3 Zn1 O7 101.7(2) . .
O2 Zn1 O5 97.3(2) . .
O3 Zn1 O5 94.2(2) . .
O7 Zn1 O5 79.98(18) . .
O2 Zn1 O1 80.3(2) . 2_444
O3 Zn1 O1 166.67(19) . 2_444
O7 Zn1 O1 86.1(2) . 2_444
O5 Zn1 O1 97.7(2) . 2_444
O2 Zn1 O4 94.9(2) . 2_454
O3 Zn1 O4 79.9(2) . 2_454
O7 Zn1 O4 89.4(2) . 2_454
O5 Zn1 O4 166.64(19) . 2_454
O1 Zn1 O4 89.6(2) 2_444 2_454
O14 Zn2 O11 102.32(19) 2_455 .
O14 Zn2 O13 80.56(16) 2_455 .
O11 Zn2 O13 96.11(18) . .
O14 Zn2 O8 162.60(17) 2_455 .
O11 Zn2 O8 91.12(19) . .
O13 Zn2 O8 87.13(16) . .
O14 Zn2 O9 95.92(17) 2_455 .
O11 Zn2 O9 79.26(18) . .
O13 Zn2 O9 173.53(18) . .
O8 Zn2 O9 97.43(17) . .
O14 Zn2 O6 94.11(16) 2_455 .
O11 Zn2 O6 153.96(17) . .
O13 Zn2 O6 106.51(17) . .
O8 Zn2 O6 77.58(16) . .
O9 Zn2 O6 79.06(17) . .
N4 Co1 N3 85.5(2) . .
N4 Co1 N2 92.6(2) . .
N3 Co1 N2 92.7(3) . .
N4 Co1 N6 91.4(2) . .
N3 Co1 N6 90.2(2) . .
N2 Co1 N6 175.3(3) . .
N4 Co1 N5 91.4(2) . .
N3 Co1 N5 174.0(2) . .
N2 Co1 N5 92.6(2) . .
N6 Co1 N5 84.7(2) . .
N4 Co1 N1 176.8(3) . .
N3 Co1 N1 91.8(2) . .
N2 Co1 N1 85.8(3) . .
N6 Co1 N1 90.4(2) . .
N5 Co1 N1 91.5(2) . .
C7 O1 Zn1 112.6(5) . 2_444
C7 O2 Zn1 112.8(5) . .
C8 O3 Zn1 113.7(5) . .
C8 O4 Zn1 112.1(5) . 2_454
C9 O5 Zn1 112.5(4) . .
C9 O6 Zn2 110.8(4) . .
C10 O7 Zn1 110.9(4) . .
C10 O8 Zn2 114.8(4) . .
C11 O9 Zn2 113.5(4) . .
C12 O11 Zn2 113.5(4) . .
C13 O13 Zn2 112.3(4) . .
C13 O14 Zn2 113.3(4) . 2_455
C1 N1 Co1 108.4(5) . .
C1 N1 H1A 110.0 . .
Co1 N1 H1A 110.0 . .
C1 N1 H1B 110.0 . .
Co1 N1 H1B 110.0 . .
H1A N1 H1B 108.4 . .
C2 N2 Co1 110.1(5) . .
C2 N2 H2A 109.6 . .
Co1 N2 H2A 109.6 . .
C2 N2 H2B 109.6 . .
Co1 N2 H2B 109.6 . .
H2A N2 H2B 108.2 . .
C3 N3 Co1 110.6(4) . .
C3 N3 H3A 109.5 . .
Co1 N3 H3A 109.5 . .
C3 N3 H3B 109.5 . .
Co1 N3 H3B 109.5 . .
H3A N3 H3B 108.1 . .
C4 N4 Co1 109.4(4) . .
C4 N4 H4A 109.8 . .
Co1 N4 H4A 109.8 . .
C4 N4 H4B 109.8 . .
Co1 N4 H4B 109.8 . .
H4A N4 H4B 108.2 . .
C5 N5 Co1 109.6(4) . .
C5 N5 H5A 109.8 . .
Co1 N5 H5A 109.8 . .
C5 N5 H5B 109.8 . .
Co1 N5 H5B 109.8 . .
H5A N5 H5B 108.2 . .
C6 N6 Co1 110.1(4) . .
C6 N6 H6A 109.6 . .
Co1 N6 H6A 109.6 . .
C6 N6 H6B 109.6 . .
Co1 N6 H6B 109.6 . .
H6A N6 H6B 108.2 . .
C2 C1 N1 110.6(7) . .
C2 C1 H1C 109.5 . .
N1 C1 H1C 109.5 . .
C2 C1 H1D 109.5 . .
N1 C1 H1D 109.5 . .
H1C C1 H1D 108.1 . .
C1 C2 N2 108.0(7) . .
C1 C2 H2C 110.1 . .
N2 C2 H2C 110.1 . .
C1 C2 H2D 110.1 . .
N2 C2 H2D 110.1 . .
H2C C2 H2D 108.4 . .
C4 C3 N3 108.9(6) . .
C4 C3 H3C 109.9 . .
N3 C3 H3C 109.9 . .
C4 C3 H3D 109.9 . .
N3 C3 H3D 109.9 . .
H3C C3 H3D 108.3 . .
C3 C4 N4 107.0(6) . .
C3 C4 H4C 110.3 . .
N4 C4 H4C 110.3 . .
C3 C4 H4D 110.3 . .
N4 C4 H4D 110.3 . .
H4C C4 H4D 108.6 . .
N5 C5 C6 108.1(6) . .
N5 C5 H5C 110.1 . .
C6 C5 H5C 110.1 . .
N5 C5 H5D 110.1 . .
C6 C5 H5D 110.1 . .
H5C C5 H5D 108.4 . .
C5 C6 N6 107.4(6) . .
C5 C6 H6C 110.2 . .
N6 C6 H6C 110.2 . .
C5 C6 H6D 110.2 . .
N6 C6 H6D 110.2 . .
H6C C6 H6D 108.5 . .
O2 C7 O1 126.1(8) . .
O2 C7 C7 118.1(8) . 2_444
O1 C7 C7 115.7(10) . 2_444
O4 C8 O3 125.7(7) . .
O4 C8 C8 117.2(8) . 2_454
O3 C8 C8 117.1(9) . 2_454
O5 C9 O6 127.6(6) . .
O5 C9 C10 116.5(6) . .
O6 C9 C10 115.9(6) . .
O8 C10 O7 126.1(6) . .
O8 C10 C9 117.3(5) . .
O7 C10 C9 116.6(6) . .
O10 C11 O9 126.1(6) . .
O10 C11 C12 118.7(6) . .
O9 C11 C12 115.2(5) . .
O12 C12 O11 125.6(6) . .
O12 C12 C11 118.5(6) . .
O11 C12 C11 115.9(6) . .
O13 C13 O14 126.6(6) . .
O13 C13 C13 117.3(7) . 2_455
O14 C13 C13 116.2(7) . 2_455
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O2 2.084(5) .
Zn1 O3 2.087(5) .
Zn1 O7 2.110(5) .
Zn1 O5 2.116(5) .
Zn1 O1 2.119(6) 2_444
Zn1 O4 2.140(5) 2_454
Zn2 O14 2.076(4) 2_455
Zn2 O11 2.078(4) .
Zn2 O13 2.107(4) .
Zn2 O8 2.115(4) .
Zn2 O9 2.116(4) .
Zn2 O6 2.215(4) .
Co1 N4 1.963(5) .
Co1 N3 1.971(6) .
Co1 N2 1.972(6) .
Co1 N6 1.984(6) .
Co1 N5 1.990(6) .
Co1 N1 1.991(6) .
O1 C7 1.264(8) .
O1 Zn1 2.119(6) 2_444
O2 C7 1.256(9) .
O3 C8 1.266(8) .
O4 C8 1.262(9) .
O4 Zn1 2.140(5) 2_454
O5 C9 1.250(7) .
O6 C9 1.251(7) .
O7 C10 1.261(7) .
O8 C10 1.246(7) .
O9 C11 1.277(7) .
O10 C11 1.237(7) .
O11 C12 1.274(7) .
O12 C12 1.257(8) .
O13 C13 1.252(7) .
O14 C13 1.267(7) .
O14 Zn2 2.076(4) 2_455
N1 C1 1.509(10) .
N1 H1A 0.9000 .
N1 H1B 0.9000 .
N2 C2 1.514(11) .
N2 H2A 0.9000 .
N2 H2B 0.9000 .
N3 C3 1.497(9) .
N3 H3A 0.9000 .
N3 H3B 0.9000 .
N4 C4 1.512(9) .
N4 H4A 0.9000 .
N4 H4B 0.9000 .
N5 C5 1.477(9) .
N5 H5A 0.9000 .
N5 H5B 0.9000 .
N6 C6 1.510(9) .
N6 H6A 0.9000 .
N6 H6B 0.9000 .
C1 C2 1.460(13) .
C1 H1C 0.9700 .
C1 H1D 0.9700 .
C2 H2C 0.9700 .
C2 H2D 0.9700 .
C3 C4 1.495(10) .
C3 H3C 0.9700 .
C3 H3D 0.9700 .
C4 H4C 0.9700 .
C4 H4D 0.9700 .
C5 C6 1.493(10) .
C5 H5C 0.9700 .
C5 H5D 0.9700 .
C6 H6C 0.9700 .
C6 H6D 0.9700 .
C7 C7 1.570(17) 2_444
C8 C8 1.560(15) 2_454
C9 C10 1.579(9) .
C11 C12 1.567(9) .
C13 C13 1.571(12) 2_455
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O9 0.90 2.07 2.956(7) 168.0 2_445
N1 H1B O3W 0.90 2.64 3.285(11) 129.6 1_556
N2 H2A O4W 0.90 2.15 3.010(9) 160.1 2
N2 H2B O5W 0.90 2.29 3.137(8) 157.1 2
N3 H3A O14 0.90 2.48 3.193(7) 136.5 1_545
N3 H3A O9 0.90 2.51 3.075(7) 121.0 2_445
N3 H3B O2W 0.90 2.07 2.911(10) 154.5 .
N4 H4A O8 0.90 2.01 2.902(7) 169.7 2
N4 H4B O10 0.90 2.06 2.955(7) 174.2 2_545
N5 H5A O7 0.90 2.15 2.973(7) 151.6 2
N5 H5B O3W 0.90 2.10 2.966(9) 160.9 1_556
N6 H6A O6 0.90 2.09 2.992(7) 176.1 2_445
N6 H6B O12 0.90 2.15 2.965(7) 150.7 2_545
N6 H6B O10 0.90 2.50 3.201(7) 135.4 2_545
