#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/47/2214719.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2214719
loop_
_publ_author_name
'Hu, Xiang-Yang'
'Ren, Yan-Ping'
'Ng, Seik Weng'
_publ_section_title
;Poly[[({μ}₄-iminiodiacetato)bis({μ}₃-iminodiacetato)lanthanum(III)nickel(II)]
 monohydrate]
;
_journal_coeditor_code           HJ3046
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2124
_journal_page_last               m2125
_journal_paper_doi               10.1107/S1600536807032904
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[La Ni (C4 H5 N O4)2 (C4 H6 N O4)], H2 O'
_chemical_formula_moiety         'C12 H16 La N3 Ni O12, H2 O'
_chemical_formula_sum            'C12 H18 La N3 Ni O13'
_chemical_formula_weight         609.91
_chemical_name_systematic
;Poly[[(μ₄-iminiodiacetato)bis(μ₃-iminodiacetato)lanthanum(III)nickel(II)]
monohydrate]
;
_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                 114.7320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7390(4)
_cell_length_b                   23.8590(10)
_cell_length_c                   8.5312(4)
_cell_measurement_reflns_used    6635
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.5
_cell_volume                     1800.50(14)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Bruker APEX area-detector diffractometer'
_diffrn_measurement_method       'φ and 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  0.020
_diffrn_reflns_av_sigmaI/netI    0.018
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7464
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.7
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.466
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    2.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Column
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.07
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.25
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2049
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.26
_refine_ls_R_factor_all          0.024
_refine_ls_R_factor_gt           0.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0250P)²+7.2608P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.062
_refine_ls_wR_factor_ref         0.062
_reflns_number_gt                2046
_reflns_number_total             2049
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hj3046.cif
_cod_data_source_block           I
_cod_original_cell_volume        1800.50(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2214719
_cod_database_fobs_code          2214719
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La La1 0.5000 0.506465(9) 0.7500 0.01011(8) Uani d S 1 . .
Ni Ni1 0.5000 0.66141(2) 0.7500 0.01438(12) Uani d S 1 . .
O O1 0.3730(3) 0.58240(9) 1.0855(3) 0.0192(5) Uani d . 1 . .
O O2 0.4288(2) 0.59806(9) 0.8602(3) 0.0160(4) Uani d . 1 . .
O O3 0.2951(3) 0.66506(9) 0.5435(3) 0.0201(5) Uani d . 1 . .
O O4 0.0546(3) 0.68604(11) 0.4774(4) 0.0313(6) Uani d . 1 . .
O O5 0.6443(2) 0.47668(9) 0.5902(3) 0.0148(4) Uani d . 1 . .
O O6 0.7921(2) 0.45955(9) 0.4593(3) 0.0175(4) Uani d . 1 . .
O O1w 0.958(3) 0.4153(7) 0.255(4) 0.175(8) Uani d PU 0.50 A -1
H H1w1 0.9572 0.4361 0.3381 0.262 Uiso d P 0.50 B -1
H H1w2 1.0410 0.4162 0.2436 0.262 Uiso d P 0.50 C -1
N N1 0.3913(3) 0.71032(10) 0.8677(3) 0.0166(5) Uani d . 1 . .
H H1n 0.4419 0.7416 0.9068 0.020 Uiso calc R 1 . .
N N2 1.0000 0.40180(15) 0.7500 0.0144(7) Uani d S 1 . .
H H2n1 0.9617 0.3800 0.6587 0.017 Uiso calc PR 0.50 . .
H H2n2 1.0383 0.3800 0.8413 0.017 Uiso calc PR 0.50 . .
C C1 0.3964(3) 0.61346(12) 0.9834(4) 0.0151(5) Uani d . 1 . .
C C2 0.3938(4) 0.67636(13) 1.0123(4) 0.0224(7) Uani d . 1 . .
H H2A 0.3035 0.6855 1.0327 0.027 Uiso calc R 1 . .
H H2B 0.4842 0.6866 1.1176 0.027 Uiso calc R 1 . .
C C3 0.2385(4) 0.72313(14) 0.7375(4) 0.0217(6) Uani d . 1 . .
H H3A 0.2335 0.7633 0.7064 0.026 Uiso calc R 1 . .
H H3B 0.1652 0.7167 0.7883 0.026 Uiso calc R 1 . .
C C4 0.1924(4) 0.68802(13) 0.5741(4) 0.0200(6) Uani d . 1 . .
C C5 0.7663(3) 0.45831(12) 0.5895(4) 0.0137(5) Uani d . 1 . .
C C6 0.8756(3) 0.43440(13) 0.7608(4) 0.0169(6) Uani d . 1 . .
H H6A 0.9192 0.4656 0.8434 0.020 Uiso calc R 1 . .
H H6B 0.8191 0.4100 0.8070 0.020 Uiso calc R 1 . .
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'
La La -0.2871 2.4523 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O5 La1 O5 2_656 . 146.10(10)
O5 La1 O1 2_656 6_565 78.79(7)
O5 La1 O1 . 6_565 73.20(7)
O5 La1 O1 2_656 5_667 73.20(7)
O5 La1 O1 . 5_667 78.79(7)
O1 La1 O1 6_565 5_667 68.03(11)
O5 La1 O2 2_656 . 74.83(7)
O5 La1 O2 . . 138.99(7)
O1 La1 O2 6_565 . 139.33(7)
O1 La1 O2 5_667 . 130.01(7)
O5 La1 O2 2_656 2_656 138.99(7)
O5 La1 O2 . 2_656 74.83(7)
O1 La1 O2 6_565 2_656 130.01(7)
O1 La1 O2 5_667 2_656 139.33(7)
O2 La1 O2 . 2_656 64.59(9)
O5 La1 O5 2_656 5_666 119.13(8)
O5 La1 O5 . 5_666 66.48(8)
O1 La1 O5 6_565 5_666 67.37(7)
O1 La1 O5 5_667 5_666 129.37(7)
O2 La1 O5 . 5_666 99.69(6)
O2 La1 O5 2_656 5_666 65.00(7)
O5 La1 O5 2_656 6_566 66.48(8)
O5 La1 O5 . 6_566 119.13(8)
O1 La1 O5 6_565 6_566 129.37(7)
O1 La1 O5 5_667 6_566 67.37(7)
O2 La1 O5 . 6_566 65.00(7)
O2 La1 O5 2_656 6_566 99.69(7)
O5 La1 O5 5_666 6_566 162.69(9)
O5 La1 O6 2_656 6_566 113.67(6)
O5 La1 O6 . 6_566 76.65(7)
O1 La1 O6 6_565 6_566 136.56(7)
O1 La1 O6 5_667 6_566 76.04(7)
O2 La1 O6 . 6_566 82.97(7)
O2 La1 O6 2_656 6_566 68.16(7)
O5 La1 O6 5_666 6_566 125.93(6)
O5 La1 O6 6_566 6_566 47.57(6)
O5 La1 O6 2_656 5_666 76.65(7)
O5 La1 O6 . 5_666 113.67(6)
O1 La1 O6 6_565 5_666 76.04(7)
O1 La1 O6 5_667 5_666 136.56(7)
O2 La1 O6 . 5_666 68.16(7)
O2 La1 O6 2_656 5_666 82.97(7)
O5 La1 O6 5_666 5_666 47.57(6)
O5 La1 O6 6_566 5_666 125.93(6)
O6 La1 O6 6_566 5_666 145.99(9)
O3 Ni1 O3 . 2_656 175.11(13)
O3 Ni1 O2 . 2_656 91.83(9)
O3 Ni1 O2 2_656 2_656 91.78(9)
O3 Ni1 O2 . . 91.78(9)
O3 Ni1 O2 2_656 . 91.83(9)
O2 Ni1 O2 2_656 . 84.85(12)
O3 Ni1 N1 . . 83.21(10)
O3 Ni1 N1 2_656 . 94.06(10)
O2 Ni1 N1 2_656 . 165.47(10)
O2 Ni1 N1 . . 81.68(9)
O3 Ni1 N1 . 2_656 94.06(10)
O3 Ni1 N1 2_656 2_656 83.21(10)
O2 Ni1 N1 2_656 2_656 81.68(9)
O2 Ni1 N1 . 2_656 165.47(9)
N1 Ni1 N1 . 2_656 112.22(14)
C1 O1 La1 . 5_667 134.0(2)
C1 O2 Ni1 . . 114.52(19)
C1 O2 La1 . . 137.87(19)
Ni1 O2 La1 . . 105.28(8)
C4 O3 Ni1 . . 114.5(2)
C5 O5 La1 . . 149.69(19)
C5 O5 La1 . 5_666 96.62(17)
La1 O5 La1 . 5_666 113.52(8)
C5 O6 La1 . 5_666 92.63(17)
H1w1 O1w H1w2 . . 114
C2 N1 C3 . . 113.9(3)
C2 N1 Ni1 . . 105.16(18)
C3 N1 Ni1 . . 108.01(19)
C2 N1 H1n . . 109.9
C3 N1 H1n . . 109.9
Ni1 N1 H1n . . 109.9
C6 N2 C6 . 2_756 116.3(3)
C6 N2 H2n1 . . 108.2
C6 N2 H2n1 2_756 . 108.2
C6 N2 H2n2 . . 108.2
C6 N2 H2n2 2_756 . 108.2
H2n1 N2 H2n2 . . 107.4
O1 C1 O2 . . 126.3(3)
O1 C1 C2 . . 117.2(3)
O2 C1 C2 . . 116.4(3)
N1 C2 C1 . . 113.8(3)
N1 C2 H2A . . 108.8
C1 C2 H2A . . 108.8
N1 C2 H2B . . 108.8
C1 C2 H2B . . 108.8
H2A C2 H2B . . 107.7
N1 C3 C4 . . 113.3(3)
N1 C3 H3A . . 108.9
C4 C3 H3A . . 108.9
N1 C3 H3B . . 108.9
C4 C3 H3B . . 108.9
H3A C3 H3B . . 107.7
O4 C4 O3 . . 125.0(3)
O4 C4 C3 . . 116.7(3)
O3 C4 C3 . . 118.2(3)
O6 C5 O5 . . 122.5(3)
O6 C5 C6 . . 123.4(3)
O5 C5 C6 . . 114.1(2)
N2 C6 C5 . . 113.8(2)
N2 C6 H6A . . 108.8
C5 C6 H6A . . 108.8
N2 C6 H6B . . 108.8
C5 C6 H6B . . 108.8
H6A C6 H6B . . 107.7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
La1 O1 5_667 2.558(2) yes
La1 O1 6_565 2.558(2) yes
La1 O2 . 2.585(2) yes
La1 O2 2_656 2.585(2) yes
La1 O5 . 2.438(2) yes
La1 O5 2_656 2.438(2) yes
La1 O5 5_666 2.673(2) yes
La1 O5 6_566 2.673(2) yes
La1 O6 5_666 2.773(2) yes
La1 O6 6_566 2.773(2) yes
Ni1 O2 . 2.048(2) yes
Ni1 O2 2_656 2.048(2) ?
Ni1 O3 . 2.038(2) yes
Ni1 O3 2_656 2.038(2) ?
Ni1 N1 . 2.093(3) yes
Ni1 N1 2_656 2.093(3) ?
O1 C1 . 1.235(4) ?
O1 La1 5_667 2.558(2) ?
O2 C1 . 1.272(4) ?
O3 C4 . 1.260(4) ?
O4 C4 . 1.248(4) ?
O5 C5 . 1.269(3) ?
O5 La1 5_666 2.673(2) ?
O6 C5 . 1.238(4) ?
O6 La1 5_666 2.773(2) ?
O1w H1w1 . 0.87 ?
O1w H1w2 . 0.856 ?
N1 C2 . 1.468(4) ?
N1 C3 . 1.469(4) ?
N1 H1n . 0.8800 ?
N2 C6 . 1.475(3) ?
N2 C6 2_756 1.475(3) ?
N2 H2n1 . 0.8800 ?
N2 H2n2 . 0.8800 ?
C1 C2 . 1.523(4) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 C4 . 1.524(4) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C5 C6 . 1.514(4) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1n O4 8_566 0.88 2.00 2.877(4) 176 no
N2 H2n1 O4 5_666 0.88 1.92 2.752(4) 156 no
N2 H2n2 O4 6_666 0.88 1.92 2.752(4) 156 no
O1w H1w1 O6 . 0.87 2.31 3.01(2) 138 no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O3 Ni1 O2 C1 . . -102.5(2)
O3 Ni1 O2 C1 2_656 . 74.2(2)
O2 Ni1 O2 C1 2_656 . 165.8(2)
N1 Ni1 O2 C1 . . -19.6(2)
N1 Ni1 O2 C1 2_656 . 143.8(3)
O3 Ni1 O2 La1 . . 91.68(9)
O3 Ni1 O2 La1 2_656 . -91.62(9)
O2 Ni1 O2 La1 2_656 . 0.0
N1 Ni1 O2 La1 . . 174.55(10)
N1 Ni1 O2 La1 2_656 . -22.0(4)
O5 La1 O2 C1 2_656 . 25.4(3)
O5 La1 O2 C1 . . -151.7(3)
O1 La1 O2 C1 6_565 . 76.8(3)
O1 La1 O2 C1 5_667 . -26.4(3)
O2 La1 O2 C1 2_656 . -160.6(3)
O5 La1 O2 C1 5_666 . 143.2(3)
O5 La1 O2 C1 6_566 . -45.3(3)
O6 La1 O2 C1 6_566 . -91.5(3)
O6 La1 O2 C1 5_666 . 106.9(3)
O5 La1 O2 Ni1 2_656 . -173.97(10)
O5 La1 O2 Ni1 . . 8.89(15)
O1 La1 O2 Ni1 6_565 . -122.63(10)
O1 La1 O2 Ni1 5_667 . 134.23(9)
O2 La1 O2 Ni1 2_656 . 0.0
O5 La1 O2 Ni1 5_666 . -56.24(9)
O5 La1 O2 Ni1 6_566 . 115.28(10)
O6 La1 O2 Ni1 6_566 . 69.12(9)
O6 La1 O2 Ni1 5_666 . -92.54(9)
O2 Ni1 O3 C4 2_656 . 159.8(2)
O2 Ni1 O3 C4 . . 74.9(2)
N1 Ni1 O3 C4 . . -6.5(2)
N1 Ni1 O3 C4 2_656 . -118.5(2)
O5 La1 O5 C5 2_656 . -78.8(4)
O1 La1 O5 C5 6_565 . -114.4(4)
O1 La1 O5 C5 5_667 . -44.2(4)
O2 La1 O5 C5 . . 96.2(4)
O2 La1 O5 C5 2_656 . 104.6(4)
O5 La1 O5 C5 5_666 . 173.5(4)
O5 La1 O5 C5 6_566 . 11.8(4)
O6 La1 O5 C5 6_566 . 33.9(4)
O6 La1 O5 C5 5_666 . 179.6(4)
C5 La1 O5 C5 6_566 . 25.2(4)
C5 La1 O5 C5 5_666 . 174.8(3)
O5 La1 O5 La1 2_656 5_666 107.71(8)
O1 La1 O5 La1 6_565 5_666 72.12(9)
O1 La1 O5 La1 5_667 5_666 142.32(10)
O2 La1 O5 La1 . 5_666 -77.24(12)
O2 La1 O5 La1 2_656 5_666 -68.93(8)
O5 La1 O5 La1 5_666 5_666 0.0
O5 La1 O5 La1 6_566 5_666 -161.70(9)
O6 La1 O5 La1 6_566 5_666 -139.55(9)
O6 La1 O5 La1 5_666 5_666 6.16(11)
O3 Ni1 N1 C2 . . 117.8(2)
O3 Ni1 N1 C2 2_656 . -66.3(2)
O2 Ni1 N1 C2 2_656 . 47.2(5)
O2 Ni1 N1 C2 . . 25.0(2)
N1 Ni1 N1 C2 2_656 . -150.6(2)
O3 Ni1 N1 C3 . . -4.2(2)
O3 Ni1 N1 C3 2_656 . 171.7(2)
O2 Ni1 N1 C3 2_656 . -74.9(4)
O2 Ni1 N1 C3 . . -97.0(2)
N1 Ni1 N1 C3 2_656 . 87.4(2)
La1 O1 C1 O2 5_667 . 42.4(5)
La1 O1 C1 C2 5_667 . -134.4(3)
Ni1 O2 C1 O1 . . -168.5(2)
La1 O2 C1 O1 . . -9.1(5)
Ni1 O2 C1 C2 . . 8.3(3)
La1 O2 C1 C2 . . 167.7(2)
C3 N1 C2 C1 . . 89.9(3)
Ni1 N1 C2 C1 . . -28.2(3)
O1 C1 C2 N1 . . -168.1(3)
O2 C1 C2 N1 . . 14.7(4)
C2 N1 C3 C4 . . -103.8(3)
Ni1 N1 C3 C4 . . 12.7(3)
Ni1 O3 C4 O4 . . -166.8(3)
Ni1 O3 C4 C3 . . 16.0(4)
N1 C3 C4 O4 . . 162.7(3)
N1 C3 C4 O3 . . -19.9(4)
La1 O6 C5 O5 5_666 . -8.2(3)
La1 O6 C5 C6 5_666 . 171.1(3)
La1 O5 C5 O6 . . -165.4(3)
La1 O5 C5 O6 5_666 . 8.6(3)
La1 O5 C5 C6 . . 15.2(5)
La1 O5 C5 C6 5_666 . -170.8(2)
C6 N2 C6 C5 2_756 . 77.8(2)
O6 C5 C6 N2 . . -12.6(4)
O5 C5 C6 N2 . . 166.8(3)
