#------------------------------------------------------------------------------
#$Date: 2016-03-24 16:15:54 +0100 (jue 24 de mar de 2016) $
#$Revision: 179683 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/05/7000529.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_7000529
loop_
_publ_author_name
'Zheng, Yan-Zhen'
'Zhang, Yue-Biao'
'Tong, Ming-Liang'
'Xue, Wei'
'Chen, Xiao-Ming'
_publ_section_title
;
 Syntheses, structures and magnetic properties of a family of metal
 carboxylate polymers viain situ metal--ligand reactions of
 benzene-1,2,3-tricarboxylic acid
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1396
_journal_paper_doi               10.1039/b815843f
_journal_year                    2009
_chemical_formula_sum            'C19 H16 N2 Ni O8'
_chemical_formula_weight         459.05
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.315(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2803(10)
_cell_length_b                   8.4929(7)
_cell_length_c                   19.9649(17)
_cell_measurement_reflns_used    5141
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.615
_cell_volume                     1868.7(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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9958
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_T_max  0.8802
_exptl_absorpt_correction_T_min  0.6512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0713P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                3565
_reflns_number_total             4051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815843f.txt
_cod_data_source_block           11
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7000529
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 1.19792(2) 0.85119(3) 1.176162(12) 0.01868(12) Uani 1 1 d . . .
O1 O 1.20333(12) 0.61223(17) 1.19659(8) 0.0237(3) Uani 1 1 d . . .
O2 O 1.27417(13) 0.36995(15) 1.21970(7) 0.0234(3) Uani 1 1 d . . .
O3 O 1.15460(13) 0.81246(16) 1.06955(7) 0.0256(3) Uani 1 1 d . . .
O4 O 1.01296(14) 0.62641(17) 1.05131(8) 0.0315(4) Uani 1 1 d . . .
O5 O 1.07906(17) 0.6312(2) 0.90941(9) 0.0417(4) Uani 1 1 d . . .
O6 O 1.26232(18) 0.6864(2) 0.89396(10) 0.0523(5) Uani 1 1 d . . .
N1 N 1.38300(16) 0.84664(19) 1.17584(9) 0.0247(4) Uani 1 1 d . . .
N2 N 2.01107(16) 0.84659(18) 1.17675(9) 0.0228(4) Uani 1 1 d . . .
O1W O 1.19029(15) 1.08641(19) 1.15563(10) 0.0292(3) Uani 1 1 d . . .
H1WA H 1.221(3) 1.152(4) 1.1805(18) 0.061(12) Uiso 1 1 d . . .
H1WB H 1.181(3) 1.117(4) 1.117(2) 0.070(11) Uiso 1 1 d . . .
O2W O 1.1419(3) 1.1305(3) 1.02070(12) 0.0617(7) Uani 1 1 d . . .
H2WA H 1.091(4) 1.199(5) 0.995(2) 0.119(16) Uiso 1 1 d . . .
H2WB H 1.117(3) 1.043(4) 1.0119(17) 0.077(13) Uiso 1 1 d . . .
C1 C 1.21835(18) 0.5528(2) 1.05355(10) 0.0227(4) Uani 1 1 d . . .
C2 C 1.2545(2) 0.5316(2) 0.99110(10) 0.0267(4) Uani 1 1 d . . .
C3 C 1.3504(2) 0.4326(3) 0.98706(11) 0.0339(5) Uani 1 1 d . . .
H3 H 1.3744 0.4211 0.9456 0.041 Uiso 1 1 calc R . .
C4 C 1.4107(2) 0.3509(3) 1.04394(13) 0.0360(6) Uani 1 1 d . . .
H4 H 1.4744 0.2838 1.0408 0.043 Uiso 1 1 calc R . .
C5 C 1.3756(2) 0.3696(2) 1.10551(12) 0.0297(5) Uani 1 1 d . . .
H5 H 1.4158 0.3142 1.1438 0.036 Uiso 1 1 calc R . .
C6 C 1.28037(17) 0.4707(2) 1.11106(10) 0.0221(4) Uani 1 1 d . . .
C7 C 1.1991(2) 0.6216(3) 0.92753(12) 0.0334(5) Uani 1 1 d . . .
C8 C 1.11971(19) 0.6708(2) 1.05885(10) 0.0230(4) Uani 1 1 d . . .
C9 C 1.24940(17) 0.4875(2) 1.18044(9) 0.0188(4) Uani 1 1 d . . .
C10 C 1.4240(2) 0.8960(3) 1.12099(12) 0.0355(5) Uani 1 1 d . . .
H10 H 1.3683 0.9330 1.0830 0.043 Uiso 1 1 calc R . .
C11 C 1.5455(2) 0.8939(3) 1.11881(12) 0.0375(5) Uani 1 1 d . . .
H11 H 1.5701 0.9285 1.0797 0.045 Uiso 1 1 calc R . .
C12 C 1.6311(2) 0.8403(2) 1.17484(12) 0.0270(5) Uani 1 1 d . . .
C13 C 1.5873(2) 0.7897(3) 1.23143(12) 0.0345(5) Uani 1 1 d . . .
H13 H 1.6407 0.7522 1.2702 0.041 Uiso 1 1 calc R . .
C14 C 1.4652(2) 0.7954(3) 1.22972(11) 0.0330(5) Uani 1 1 d . . .
H14 H 1.4382 0.7618 1.2682 0.040 Uiso 1 1 calc R . .
C15 C 1.7619(2) 0.8398(2) 1.17533(12) 0.0269(5) Uani 1 1 d . . .
C16 C 1.8401(2) 0.7242(3) 1.20815(13) 0.0395(6) Uani 1 1 d . . .
H16 H 1.8103 0.6421 1.2306 0.047 Uiso 1 1 calc R . .
C17 C 1.9613(2) 0.7309(3) 1.20742(13) 0.0352(5) Uani 1 1 d . . .
H17 H 2.0116 0.6512 1.2293 0.042 Uiso 1 1 calc R . .
C18 C 1.81325(19) 0.9581(3) 1.14295(12) 0.0322(5) Uani 1 1 d . . .
H18 H 1.7648 1.0376 1.1195 0.039 Uiso 1 1 calc R . .
C19 C 1.93589(19) 0.9576(3) 1.14564(11) 0.0305(5) Uani 1 1 d . . .
H19 H 1.9683 1.0397 1.1245 0.037 Uiso 1 1 calc R . .
H5A H 1.048(3) 0.541(4) 0.9291(18) 0.092(12) 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
_geom_angle_publ_flag
O1W Ni1 O2 96.84(6) . 2_757 ?
O1W Ni1 O1 179.28(6) . . ?
O2 Ni1 O1 83.34(5) 2_757 . ?
O1W Ni1 N1 90.97(7) . . ?
O2 Ni1 N1 93.86(7) 2_757 . ?
O1 Ni1 N1 89.71(6) . . ?
O1W Ni1 O3 87.65(7) . . ?
O2 Ni1 O3 173.60(5) 2_757 . ?
O1 Ni1 O3 92.11(6) . . ?
N1 Ni1 O3 90.61(6) . . ?
O1W Ni1 N2 91.14(6) . 1_455 ?
O2 Ni1 N2 86.16(6) 2_757 1_455 ?
O1 Ni1 N2 88.18(6) . 1_455 ?
N1 Ni1 N2 177.88(6) . 1_455 ?
O3 Ni1 N2 89.20(6) . 1_455 ?
C9 O1 Ni1 140.87(13) . . ?
C9 O2 Ni1 131.24(12) . 2_747 ?
C8 O3 Ni1 108.35(12) . . ?
C7 O5 H5A 106(2) . . ?
C14 N1 C10 117.27(19) . . ?
C14 N1 Ni1 121.76(14) . . ?
C10 N1 Ni1 120.97(15) . . ?
C19 N2 C17 116.40(18) . . ?
C19 N2 Ni1 121.49(13) . 1_655 ?
C17 N2 Ni1 122.10(14) . 1_655 ?
Ni1 O1W H1WA 126(2) . . ?
Ni1 O1W H1WB 120(2) . . ?
H1WA O1W H1WB 109(3) . . ?
H2WA O2W H2WB 109(4) . . ?
C6 C1 C2 118.47(18) . . ?
C6 C1 C8 121.21(17) . . ?
C2 C1 C8 120.19(18) . . ?
C3 C2 C1 120.52(19) . . ?
C3 C2 C7 116.70(19) . . ?
C1 C2 C7 122.63(19) . . ?
C4 C3 C2 120.7(2) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 C3 119.4(2) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.9(2) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 120.00(18) . . ?
C1 C6 C9 122.35(17) . . ?
C5 C6 C9 117.66(18) . . ?
O6 C7 O5 120.6(2) . . ?
O6 C7 C2 120.8(2) . . ?
O5 C7 C2 118.6(2) . . ?
O4 C8 O3 124.51(19) . . ?
O4 C8 C1 119.89(18) . . ?
O3 C8 C1 115.58(18) . . ?
O1 C9 O2 123.92(18) . . ?
O1 C9 C6 120.50(17) . . ?
O2 C9 C6 115.58(16) . . ?
N1 C10 C11 122.6(2) . . ?
N1 C10 H10 118.7 . . ?
C11 C10 H10 118.7 . . ?
C10 C11 C12 120.2(2) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 116.6(2) . . ?
C11 C12 C15 122.0(2) . . ?
C13 C12 C15 121.4(2) . . ?
C14 C13 C12 119.8(2) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
N1 C14 C13 123.6(2) . . ?
N1 C14 H14 118.2 . . ?
C13 C14 H14 118.2 . . ?
C18 C15 C16 116.5(2) . . ?
C18 C15 C12 120.81(19) . . ?
C16 C15 C12 122.67(19) . . ?
C17 C16 C15 120.0(2) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
N2 C17 C16 123.4(2) . . ?
N2 C17 H17 118.3 . . ?
C16 C17 H17 118.3 . . ?
C19 C18 C15 119.8(2) . . ?
C19 C18 H18 120.1 . . ?
C15 C18 H18 120.1 . . ?
N2 C19 C18 123.9(2) . . ?
N2 C19 H19 118.1 . . ?
C18 C19 H19 118.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1W 2.0375(16) . ?
Ni1 O2 2.0416(14) 2_757 ?
Ni1 O1 2.0683(15) . ?
Ni1 N1 2.0895(19) . ?
Ni1 O3 2.1058(14) . ?
Ni1 N2 2.1105(18) 1_455 ?
O1 C9 1.252(2) . ?
O2 C9 1.263(2) . ?
O2 Ni1 2.0416(14) 2_747 ?
O3 C8 1.270(2) . ?
O4 C8 1.240(3) . ?
O5 C7 1.327(3) . ?
O5 H5A 0.96(4) . ?
O6 C7 1.210(3) . ?
N1 C14 1.334(3) . ?
N1 C10 1.343(3) . ?
N2 C19 1.330(3) . ?
N2 C17 1.342(3) . ?
N2 Ni1 2.1105(17) 1_655 ?
O1W H1WA 0.78(4) . ?
O1W H1WB 0.81(4) . ?
O2W H2WA 0.89(5) . ?
O2W H2WB 0.80(4) . ?
C1 C6 1.397(3) . ?
C1 C2 1.403(3) . ?
C1 C8 1.518(3) . ?
C2 C3 1.386(3) . ?
C2 C7 1.499(3) . ?
C3 C4 1.380(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.378(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.398(3) . ?
C5 H5 0.9300 . ?
C6 C9 1.506(2) . ?
C10 C11 1.381(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.389(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.394(3) . ?
C12 C15 1.473(3) . ?
C13 C14 1.371(3) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C18 1.386(3) . ?
C15 C16 1.388(3) . ?
C16 C17 1.372(3) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.373(3) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
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
O1W H1WA O2 0.78(4) 2.05(3) 2.795(2) 161(3) 1_565
O1W H1WA O1 0.78(4) 2.44(3) 2.947(2) 124(3) 2_757
O1W H1WB O2W 0.81(4) 1.88(4) 2.659(3) 163(3) .
O2W H2WA O4 0.89(5) 2.00(5) 2.883(3) 172(4) 3_777
O2W H2WB O3 0.80(4) 2.26(4) 2.865(3) 132(3) .
O5 H5A O4 0.96(4) 1.67(4) 2.613(2) 170(3) 3_767
