#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:05:36 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179612 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/76/4507616.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_4507616
loop_
_publ_author_name
'Hou, Juan-Juan'
'Zhang, Rong'
'Qin, Ying-Lian'
'Zhang, Xian-Ming'
_publ_section_title
;
 From (3,6)-Connectedkgd,chiralanhto (3,8)-connectedtfz-dNets in Low
 Nuclear Metal Cluster-Based Networks with Triangular
 Pyridinedicarboxylate Ligand
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1618
_journal_paper_doi               10.1021/cg301827p
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C13 H11 N Ni O6'
_chemical_formula_weight         335.94
_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                74.359(6)
_cell_angle_beta                 83.755(6)
_cell_angle_gamma                83.938(5)
_cell_formula_units_Z            2
_cell_length_a                   6.3725(4)
_cell_length_b                   7.7363(5)
_cell_length_c                   12.7332(10)
_cell_measurement_temperature    293(2)
_cell_volume                     599.00(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3431
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    1.650
_exptl_absorpt_correction_T_max  0.8793
_exptl_absorpt_correction_T_min  0.8524
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.248
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0367
_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)+(0.0420P)²+0.7728P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                2272
_reflns_number_total             2562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301827p_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4507616
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
Ni1 Ni 0.52420(6) 0.66740(6) 0.89139(3) 0.01718(15) Uani 1 1 d
N1 N -0.2231(4) 0.5243(4) 0.8239(2) 0.0185(6) Uani 1 1 d
O1 O 0.4319(4) 0.1835(4) 0.8883(2) 0.0325(7) Uani 1 1 d
O2 O 0.3593(4) 0.4266(3) 0.95321(19) 0.0187(5) Uani 1 1 d
O3 O -0.4096(4) 0.2649(4) 0.2580(2) 0.0295(6) Uani 1 1 d
O4 O -0.0946(4) 0.1179(4) 0.2391(2) 0.0275(6) Uani 1 1 d
O1W O 0.6961(4) 0.8916(4) 0.8561(3) 0.0332(7) Uani 1 1 d
O2W O 0.2681(4) 0.8092(3) 0.9527(2) 0.0249(5) Uani 1 1 d
C1 C -0.0350(5) 0.4894(5) 0.8664(3) 0.0186(7) Uani 1 1 d
C2 C 0.1237(5) 0.3717(4) 0.8360(3) 0.0173(7) Uani 1 1 d
C3 C 0.0913(5) 0.2938(4) 0.7527(3) 0.0183(7) Uani 1 1 d
C4 C -0.0960(5) 0.3389(5) 0.7011(3) 0.0200(7) Uani 1 1 d
C5 C -0.2502(5) 0.4517(5) 0.7416(3) 0.0209(7) Uani 1 1 d
C6 C -0.1312(5) 0.2814(5) 0.6013(3) 0.0206(7) Uani 1 1 d
C7 C 0.0389(6) 0.2501(5) 0.5297(3) 0.0252(8) Uani 1 1 d
C8 C 0.0091(6) 0.2135(5) 0.4318(3) 0.0233(7) Uani 1 1 d
C9 C -0.1945(5) 0.2146(4) 0.4023(3) 0.0206(7) Uani 1 1 d
C10 C -0.3639(6) 0.2413(6) 0.4750(4) 0.0346(10) Uani 1 1 d
C11 C -0.3329(6) 0.2714(7) 0.5744(3) 0.0343(10) Uani 1 1 d
C12 C 0.3212(5) 0.3203(4) 0.8959(3) 0.0173(7) Uani 1 1 d
C13 C -0.2336(5) 0.1960(5) 0.2910(3) 0.0198(7) Uani 1 1 d
H1A H -0.013(6) 0.555(5) 0.918(3) 0.016(9) Uiso 1 1 d
H3A H 0.198(6) 0.203(5) 0.732(3) 0.029(11) Uiso 1 1 d
H8A H 0.125(7) 0.203(5) 0.382(3) 0.028(11) Uiso 1 1 d
H5A H -0.387(6) 0.491(5) 0.707(3) 0.027(10) Uiso 1 1 d
H11A H -0.438(8) 0.281(7) 0.619(4) 0.052(15) Uiso 1 1 d
H7A H 0.171(7) 0.255(6) 0.548(4) 0.034(12) Uiso 1 1 d
H10A H -0.495(8) 0.244(6) 0.454(4) 0.042(13) Uiso 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'
Ni Ni 0.3393 1.1124 '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
O3 Ni1 O2W 90.96(10) 2_566 .
O3 Ni1 O1W 93.47(12) 2_566 .
O2W Ni1 O1W 90.02(10) . .
O3 Ni1 N1 86.84(10) 2_566 1_655
O2W Ni1 N1 177.73(10) . 1_655
O1W Ni1 N1 90.68(11) . 1_655
O3 Ni1 O2 174.97(10) 2_566 2_667
O2W Ni1 O2 91.43(10) . 2_667
O1W Ni1 O2 90.95(11) . 2_667
N1 Ni1 O2 90.72(10) 1_655 2_667
O3 Ni1 O2 95.23(11) 2_566 .
O2W Ni1 O2 88.77(9) . .
O1W Ni1 O2 171.23(11) . .
N1 Ni1 O2 90.86(10) 1_655 .
O2 Ni1 O2 80.40(9) 2_667 .
C1 N1 C5 117.7(3) . .
C1 N1 Ni1 121.4(2) . 1_455
C5 N1 Ni1 120.7(2) . 1_455
C12 O2 Ni1 123.0(2) . 2_667
C12 O2 Ni1 125.2(2) . .
Ni1 O2 Ni1 99.60(9) 2_667 .
C13 O3 Ni1 132.8(2) . 2_566
N1 C1 C2 123.0(3) . .
C1 C2 C3 118.5(3) . .
C1 C2 C12 120.7(3) . .
C3 C2 C12 120.7(3) . .
C4 C3 C2 119.7(3) . .
C3 C4 C5 117.3(3) . .
C3 C4 C6 123.0(3) . .
C5 C4 C6 119.6(3) . .
N1 C5 C4 123.6(3) . .
C11 C6 C7 118.4(3) . .
C11 C6 C4 121.2(3) . .
C7 C6 C4 120.2(3) . .
C6 C7 C8 121.3(3) . .
C7 C8 C9 119.9(3) . .
C10 C9 C8 118.7(3) . .
C10 C9 C13 119.7(3) . .
C8 C9 C13 121.5(3) . .
C9 C10 C11 121.0(3) . .
C6 C11 C10 120.5(3) . .
O1 C12 O2 125.0(3) . .
O1 C12 C2 119.2(3) . .
O2 C12 C2 115.7(3) . .
O4 C13 O3 125.1(3) . .
O4 C13 C9 120.0(3) . .
O3 C13 C9 114.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O3 2.027(3) 2_566
Ni1 O2W 2.069(2) .
Ni1 O1W 2.070(3) .
Ni1 N1 2.096(3) 1_655
Ni1 O2 2.104(2) 2_667
Ni1 O2 2.154(2) .
N1 C1 1.340(4) .
N1 C5 1.350(4) .
N1 Ni1 2.096(3) 1_455
O1 C12 1.229(4) .
O2 C12 1.293(4) .
O2 Ni1 2.104(2) 2_667
O3 C13 1.255(4) .
O3 Ni1 2.027(3) 2_566
O4 C13 1.249(4) .
C1 C2 1.382(5) .
C2 C3 1.397(4) .
C2 C12 1.504(4) .
C3 C4 1.392(5) .
C4 C5 1.394(5) .
C4 C6 1.500(5) .
C6 C11 1.381(5) .
C6 C7 1.383(5) .
C7 C8 1.386(5) .
C8 C9 1.388(5) .
C9 C10 1.380(5) .
C9 C13 1.512(5) .
C10 C11 1.386(5) .
