#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:44:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179260 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/80/4318081.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_4318081
loop_
_publ_author_name
'Chuan-De Wu'
'Can-Zhong Lu'
'Wen-Bin Yang'
'Hong-Hui Zhuang'
'Jin-Shun Huang'
_publ_contact_author_address
;
   The State Key Laboratory of Structural Chemistry,
   Fujian Institute of Research on the Structure of Matter,
   the Chinese Academy of Sciences,
   Fuzhou, Fujian 350002,
   P. R. China
;
_publ_contact_author_email       czlu@ms.fjirsm.ac.cn
_publ_contact_author_fax         86-591-3714946
_publ_contact_author_name        'Can-Zhong Lu'
_publ_contact_author_phone       86-591-3705834
_publ_section_title
;
 Hydrothermal Synthesis, Structures, and Magnetic Properties of Three
 Novel 5-Aminoisophthalic Acid Ligand Bridged Transition Metal Cation
 Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3302
_journal_page_last               3307
_journal_paper_doi               10.1021/ic011182g
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C8 H9 N Ni O6'
_chemical_formula_weight         273.87
_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                113.09(3)
_cell_angle_beta                 99.64(3)
_cell_angle_gamma                98.90(3)
_cell_formula_units_Z            2
_cell_length_a                   6.425(1)
_cell_length_b                   8.115(2)
_cell_length_c                   10.146(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.75
_cell_measurement_theta_min      14.43
_cell_volume                     465.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0653
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2859
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    2.098
_exptl_absorpt_correction_T_max  0.9942
_exptl_absorpt_correction_T_min  0.4872
_exptl_crystal_colour            'Deep Green'
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.792
_refine_diff_density_min         -2.274
_refine_diff_density_rms         0.224
_refine_ls_extinction_coef       0.000(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2718
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          2.068
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1321P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1826
_reflns_number_gt                2128
_reflns_number_total             2718
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011182g_2.cif
_cod_data_source_block           NiAIP
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318081
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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.20251(9) 1.25121(8) 1.30491(5) 0.0135(2) Uani 1 1 d . . .
O1 O 0.1660(5) 1.2487(5) 1.0954(3) 0.0200(7) Uani 1 1 d . . .
O2 O 0.4905(5) 1.2851(5) 1.2262(3) 0.0183(6) Uani 1 1 d . . .
O3 O 0.0500(6) 1.2507(6) 0.6039(4) 0.0295(9) Uani 1 1 d . . .
O4 O 0.3344(5) 1.2578(5) 0.5038(3) 0.0175(6) Uani 1 1 d . . .
O5 O 0.2463(6) 1.5317(5) 1.4059(4) 0.0218(7) Uani 1 1 d D . .
HA5 H 0.374(4) 1.595(6) 1.425(6) 0.007(12) Uiso 1 1 d D . .
HB5 H 0.162(8) 1.584(11) 1.374(11) 0.09(4) Uiso 1 1 d D . .
O6 O -0.1140(6) 1.2098(6) 1.3204(4) 0.0235(7) Uani 1 1 d D . .
HA6 H -0.188(10) 1.099(4) 1.288(11) 0.09(4) Uiso 1 1 d D . .
HB6 H -0.204(8) 1.271(7) 1.307(7) 0.027(16) Uiso 1 1 d D . .
N1 N 0.8599(6) 1.0405(5) 0.7919(4) 0.0145(7) Uani 1 1 d . . .
HA1 H 0.916(9) 1.066(7) 0.728(6) 0.015(13) Uiso 1 1 d . . .
HA2 H 0.953(9) 1.072(8) 0.874(6) 0.016(13) Uiso 1 1 d . . .
C1 C 0.3675(7) 1.2659(6) 1.1084(4) 0.0136(7) Uani 1 1 d . . .
C2 C 0.4490(7) 1.2448(6) 0.9746(4) 0.0146(8) Uani 1 1 d . . .
C3 C 0.3304(7) 1.2793(6) 0.8645(4) 0.0152(8) Uani 1 1 d . . .
H3A H 0.2137 1.3328 0.8812 0.018 Uiso 1 1 calc R . .
C4 C 0.3849(7) 1.2347(6) 0.7299(4) 0.0144(8) Uani 1 1 d . . .
C5 C 0.2444(7) 1.2522(6) 0.6050(4) 0.0173(8) Uani 1 1 d . . .
C6 C 0.5638(7) 1.1586(6) 0.7085(4) 0.0145(8) Uani 1 1 d . . .
H6A H 0.6028 1.1291 0.6192 0.017 Uiso 1 1 calc R . .
C7 C 0.6840(7) 1.1266(6) 0.8189(4) 0.0132(7) Uani 1 1 d . . .
C8 C 0.6290(7) 1.1717(6) 0.9532(4) 0.0149(8) Uani 1 1 d . . .
H8A H 0.7119 1.1532 1.0283 0.018 Uiso 1 1 calc R . .
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
O4 Ni O5 89.13(14) 1_556 . ?
O4 Ni O6 96.01(14) 1_556 . ?
O5 Ni O6 91.48(15) . . ?
O4 Ni O1 162.26(14) 1_556 . ?
O5 Ni O1 92.15(15) . . ?
O6 Ni O1 101.64(14) . . ?
O4 Ni N1 89.54(14) 1_556 2_677 ?
O5 Ni N1 176.03(15) . 2_677 ?
O6 Ni N1 84.94(16) . 2_677 ?
O1 Ni N1 90.26(14) . 2_677 ?
O4 Ni O2 100.43(13) 1_556 . ?
O5 Ni O2 90.16(14) . . ?
O6 Ni O2 163.50(13) . . ?
O1 Ni O2 61.89(12) . . ?
N1 Ni O2 93.76(14) 2_677 . ?
O4 Ni C1 131.26(14) 1_556 . ?
O5 Ni C1 92.37(15) . . ?
O6 Ni C1 132.60(14) . . ?
O1 Ni C1 31.01(13) . . ?
N1 Ni C1 91.32(15) 2_677 . ?
O2 Ni C1 30.91(12) . . ?
C1 O1 Ni 90.2(2) . . ?
C1 O2 Ni 87.3(3) . . ?
C5 O4 Ni 129.8(3) . 1_554 ?
C7 N1 Ni 119.4(3) . 2_677 ?
O2 C1 O1 120.5(4) . . ?
O2 C1 C2 121.8(4) . . ?
O1 C1 C2 117.4(4) . . ?
O2 C1 Ni 61.8(2) . . ?
O1 C1 Ni 58.8(2) . . ?
C2 C1 Ni 171.2(3) . . ?
C8 C2 C3 120.2(4) . . ?
C8 C2 C1 119.8(4) . . ?
C3 C2 C1 119.6(4) . . ?
C4 C3 C2 120.5(4) . . ?
C3 C4 C6 118.8(4) . . ?
C3 C4 C5 120.9(4) . . ?
C6 C4 C5 120.0(4) . . ?
O3 C5 O4 125.5(4) . . ?
O3 C5 C4 118.7(4) . . ?
O4 C5 C4 115.7(4) . . ?
C7 C6 C4 120.6(4) . . ?
C6 C7 C8 120.3(4) . . ?
C6 C7 N1 119.6(4) . . ?
C8 C7 N1 120.0(3) . . ?
C7 C8 C2 119.4(4) . . ?
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
Ni O4 2.030(3) 1_556 ?
Ni O5 2.046(3) . ?
Ni O6 2.052(4) . ?
Ni O1 2.091(3) . ?
Ni N1 2.117(4) 2_677 ?
Ni O2 2.156(3) . ?
Ni C1 2.443(4) . ?
O1 C1 1.259(5) . ?
O2 C1 1.256(5) . ?
O3 C5 1.245(6) . ?
O4 C5 1.272(5) . ?
O4 Ni 2.030(3) 1_554 ?
N1 C7 1.428(5) . ?
N1 Ni 2.117(4) 2_677 ?
C1 C2 1.493(6) . ?
C2 C8 1.390(6) . ?
C2 C3 1.390(5) . ?
C3 C4 1.389(6) . ?
C4 C6 1.396(6) . ?
C4 C5 1.496(5) . ?
C6 C7 1.385(5) . ?
C7 C8 1.387(5) . ?
