#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/21/2222191.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_2222191
loop_
_publ_author_name
'Hsu, Shih-Chen'
'Chiang, Pei-Hsuan'
'Chang, Chih-Hsien'
'Lin, Chia-Her'
_publ_section_title
catena-Poly[[tetraaquanickel(II)]-μ₃-benzene-1,3,5-tricarboxylato-3':1:2-κ⁴O¹:O³,O^3'^:O⁵-[tetraaquanickel(II)]-μ₂-benzene-1,3,5-tricarboxylato-2:3κ²O¹:O³-[tetraaquanickel(II)]]
_journal_coeditor_code           ZL2190
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m625
_journal_page_last               m626
_journal_paper_doi               10.1107/S1600536809016729
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni3 (C9 H3 O6)2 (H2 O)12]'
_chemical_formula_moiety         'C18 H30 Ni3 O24'
_chemical_formula_sum            'C18 H30 Ni3 O24'
_chemical_formula_weight         806.49
_chemical_name_systematic
;
catena-Poly[[tetraaquanickel(II)]-μ₃-benzene-1,3,5-tricarboxylato-
3':1:2-κ⁴O¹:O³,O^3'^:O⁵-
[tetraaquanickel(II)]-\\m₂-benzene-1,3,5-tricarboxylato-
2:3κ²O¹:O³-[tetraaquanickel(II)]]
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 111.609(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.3394(10)
_cell_length_b                   12.8724(7)
_cell_length_c                   6.5462(3)
_cell_measurement_reflns_used    4802
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.294
_cell_measurement_theta_min      2.527
_cell_volume                     1358.42(13)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6798
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    2.167
_exptl_absorpt_correction_T_max  0.7370
_exptl_absorpt_correction_T_min  0.6134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            light-blue
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.382
_refine_ls_abs_structure_details 'Flack (1983), 1531 Friedel pairs'
_refine_ls_abs_structure_Flack   0.549(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3299
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ\^2\^(Fo\^2\^)+(0.0363P)\^2\^] where P=(Fo\^2\^+2Fc\^2\^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0684
_reflns_number_gt                3156
_reflns_number_total             3299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zl2190.cif
_cod_data_source_block           I
_cod_original_cell_volume        1358.42(12)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               2222191
_cod_database_fobs_code          2222191
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
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
Ni Ni1 0.5000 0.68238(4) 0.0000 0.02554(13) Uani d S 1 . .
Ni Ni2 0.757745(18) -0.02765(2) 0.22999(5) 0.01825(9) Uani d . 1 . .
O O1 0.56460(12) 0.54287(15) 0.1157(3) 0.0269(4) Uani d . 1 . .
O O2 0.58008(19) 0.7828(2) 0.1959(5) 0.0659(10) Uani d . 1 . .
H H2A 0.5729 0.8177 0.2978 0.079 Uiso d R 1 . .
H H2B 0.6113 0.8141 0.1460 0.079 Uiso d R 1 . .
O O3 0.44433(15) 0.68727(18) 0.2333(4) 0.0396(5) Uani d . 1 . .
H H3A 0.4101 0.6382 0.2657 0.047 Uiso d R 1 . .
H H3B 0.4382 0.7546 0.2822 0.047 Uiso d R 1 . .
O O4 0.83989(12) 0.08047(16) 0.4286(3) 0.0259(4) Uani d . 1 . .
H H4B 0.8029 0.1274 0.4439 0.031 Uiso d R 1 . .
H H4C 0.8708 0.0577 0.5683 0.031 Uiso d R 1 . .
O O5 0.67707(12) -0.13068(15) 0.0142(3) 0.0229(4) Uani d . 1 . .
H H5A 0.7035 -0.1838 0.0246 0.028 Uiso d R 1 . .
H H5B 0.6543 -0.1191 -0.1354 0.028 Uiso d R 1 . .
O O6 0.77890(12) 0.03467(16) -0.0377(3) 0.0316(5) Uani d . 1 . .
H H6A 0.7595 0.0949 -0.0829 0.038 Uiso d R 1 . .
H H6B 0.8290 0.0322 -0.0698 0.038 Uiso d R 1 . .
O O7 0.85264(11) -0.12996(14) 0.3010(3) 0.0223(4) Uani d . 1 . .
O O8 0.65774(12) 0.06587(15) 0.1685(3) 0.0237(4) Uani d . 1 . .
O O9 0.73419(13) -0.09194(17) 0.4944(3) 0.0299(5) Uani d . 1 . .
H H9A 0.6945 -0.0832 0.5292 0.036 Uiso d R 1 . .
H H9B 0.7453 -0.1563 0.5346 0.036 Uiso d R 1 . .
O O10 0.71601(12) 0.21051(15) 0.3445(3) 0.0271(4) Uani d . 1 . .
O O11 0.78560(12) -0.27492(14) 0.1508(3) 0.0253(4) Uani d . 1 . .
O O12 0.93126(13) -0.61400(16) 0.4291(4) 0.0333(5) Uani d . 1 . .
C C1 0.92709(16) -0.3961(2) 0.3927(4) 0.0156(5) Uani d . 1 . .
H H1A 0.8781 -0.4324 0.3216 0.019 Uiso calc R 1 . .
C C2 0.5000 0.1625(3) 0.0000 0.0159(7) Uani d S 1 . .
H H2C 0.5000 0.0903 0.0000 0.019 Uiso calc SR 1 . .
C C3 1.0000 -0.4499(3) 0.5000 0.0157(7) Uani d S 1 . .
C C4 1.0000 -0.2341(3) 0.5000 0.0158(6) Uani d S 1 . .
H H4A 1.0000 -0.1618 0.5000 0.019 Uiso calc SR 1 . .
C C5 0.92667(15) -0.28782(19) 0.3907(4) 0.0149(5) Uani d . 1 . .
C C6 0.65536(16) 0.1604(2) 0.2156(4) 0.0178(5) Uani d . 1 . .
C C7 0.5000 0.3778(3) 0.0000 0.0163(7) Uani d S 1 . .
C C8 0.84852(15) -0.2270(2) 0.2722(4) 0.0159(5) Uani d . 1 . .
C C9 0.57403(16) 0.2158(2) 0.1077(4) 0.0159(5) Uani d . 1 . .
C C10 0.57306(15) 0.3237(2) 0.1084(4) 0.0167(5) Uani d . 1 . .
H H10A 0.6218 0.3601 0.1821 0.020 Uiso calc R 1 . .
C C11 0.5000 0.4925(3) 0.0000 0.0204(8) Uani d S 1 . .
C C12 1.0000 -0.5673(3) 0.5000 0.0211(8) Uani d S 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Ni1 O2 2_655 . 98.7(2) ?
O2 Ni1 O3 2_655 2_655 84.80(10) ?
O2 Ni1 O3 . 2_655 92.94(10) ?
O2 Ni1 O3 2_655 . 92.94(10) ?
O2 Ni1 O3 . . 84.80(10) ?
O3 Ni1 O3 2_655 . 176.54(13) ?
O2 Ni1 O1 2_655 2_655 99.80(12) ?
O2 Ni1 O1 . 2_655 160.42(11) ?
O3 Ni1 O1 2_655 2_655 95.20(9) ?
O3 Ni1 O1 . 2_655 87.75(9) ?
O2 Ni1 O1 2_655 . 160.42(11) ?
O2 Ni1 O1 . . 99.80(12) ?
O3 Ni1 O1 2_655 . 87.75(9) ?
O3 Ni1 O1 . . 95.20(9) ?
O1 Ni1 O1 2_655 . 62.84(10) ?
O2 Ni1 C11 2_655 . 130.67(11) ?
O2 Ni1 C11 . . 130.67(11) ?
O3 Ni1 C11 2_655 . 91.73(7) ?
O3 Ni1 C11 . . 91.73(7) ?
O1 Ni1 C11 2_655 . 31.42(5) ?
O1 Ni1 C11 . . 31.42(5) ?
O7 Ni2 O8 . . 175.21(9) ?
O7 Ni2 O5 . . 91.60(7) ?
O8 Ni2 O5 . . 86.05(8) ?
O7 Ni2 O4 . . 88.86(8) ?
O8 Ni2 O4 . . 93.77(8) ?
O5 Ni2 O4 . . 176.11(9) ?
O7 Ni2 O6 . . 93.66(8) ?
O8 Ni2 O6 . . 90.41(8) ?
O5 Ni2 O6 . . 87.51(8) ?
O4 Ni2 O6 . . 88.61(8) ?
O7 Ni2 O9 . . 86.70(8) ?
O8 Ni2 O9 . . 89.18(8) ?
O5 Ni2 O9 . . 91.29(8) ?
O4 Ni2 O9 . . 92.59(8) ?
O6 Ni2 O9 . . 178.76(9) ?
C11 O1 Ni1 . . 89.19(17) ?
Ni1 O2 H2A . . 125.6 ?
Ni1 O2 H2B . . 117.6 ?
H2A O2 H2B . . 110.8 ?
Ni1 O3 H3A . . 130.1 ?
Ni1 O3 H3B . . 114.6 ?
H3A O3 H3B . . 112.3 ?
Ni2 O4 H4B . . 99.5 ?
Ni2 O4 H4C . . 115.0 ?
H4B O4 H4C . . 106.1 ?
Ni2 O5 H5A . . 105.4 ?
Ni2 O5 H5B . . 122.7 ?
H5A O5 H5B . . 103.5 ?
Ni2 O6 H6A . . 118.3 ?
Ni2 O6 H6B . . 128.5 ?
H6A O6 H6B . . 103.1 ?
C8 O7 Ni2 . . 127.85(17) ?
C6 O8 Ni2 . . 128.92(18) ?
Ni2 O9 H9A . . 128.6 ?
Ni2 O9 H9B . . 122.6 ?
H9A O9 H9B . . 99.5 ?
C3 C1 C5 . . 120.4(2) ?
C3 C1 H1A . . 119.8 ?
C5 C1 H1A . . 119.8 ?
C9 C2 C9 . 2_655 121.2(3) ?
C9 C2 H2C . . 119.4 ?
C9 C2 H2C 2_655 . 119.4 ?
C1 C3 C1 2_756 . 119.9(3) ?
C1 C3 C12 2_756 . 120.03(16) ?
C1 C3 C12 . . 120.03(16) ?
C5 C4 C5 . 2_756 120.4(3) ?
C5 C4 H4A . . 119.8 ?
C5 C4 H4A 2_756 . 119.8 ?
C4 C5 C1 . . 119.4(2) ?
C4 C5 C8 . . 118.9(2) ?
C1 C5 C8 . . 121.6(2) ?
O10 C6 O8 . . 124.4(2) ?
O10 C6 C9 . . 118.7(2) ?
O8 C6 C9 . . 116.9(2) ?
C10 C7 C10 . 2_655 119.9(3) ?
C10 C7 C11 . . 120.07(17) ?
C10 C7 C11 2_655 . 120.07(17) ?
O11 C8 O7 . . 124.9(2) ?
O11 C8 C5 . . 118.6(2) ?
O7 C8 C5 . . 116.5(2) ?
C10 C9 C2 . . 118.9(2) ?
C10 C9 C6 . . 118.9(2) ?
C2 C9 C6 . . 122.2(2) ?
C9 C10 C7 . . 120.6(3) ?
C9 C10 H10A . . 119.7 ?
C7 C10 H10A . . 119.7 ?
O1 C11 O1 . 2_655 118.8(3) ?
O1 C11 C7 . . 120.61(16) ?
O1 C11 C7 2_655 . 120.61(16) ?
O1 C11 Ni1 . . 59.39(16) ?
O1 C11 Ni1 2_655 . 59.39(16) ?
C7 C11 Ni1 . . 180.0 ?
O12 C12 O12 2_756 . 123.1(4) ?
O12 C12 C3 2_756 . 118.45(18) ?
O12 C12 C3 . . 118.45(18) ?
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
Ni1 O2 2_655 1.983(3) ?
Ni1 O2 . 1.983(3) ?
Ni1 O3 2_655 2.087(2) ?
Ni1 O3 . 2.087(2) ?
Ni1 O1 2_655 2.1043(19) ?
Ni1 O1 . 2.1043(19) ?
Ni1 C11 . 2.445(4) ?
Ni2 O7 . 2.0235(18) ?
Ni2 O8 . 2.026(2) ?
Ni2 O5 . 2.0630(19) ?
Ni2 O4 . 2.0716(19) ?
Ni2 O6 . 2.0787(19) ?
Ni2 O9 . 2.090(2) ?
O1 C11 . 1.275(3) ?
O2 H2A . 0.8508 ?
O2 H2B . 0.8329 ?
O3 H3A . 0.9431 ?
O3 H3B . 0.9439 ?
O4 H4B . 0.9132 ?
O4 H4C . 0.9216 ?
O5 H5A . 0.8116 ?
O5 H5B . 0.9233 ?
O6 H6A . 0.8533 ?
O6 H6B . 0.9664 ?
O7 C8 . 1.261(3) ?
O8 C6 . 1.260(3) ?
O9 H9A . 0.8087 ?
O9 H9B . 0.8686 ?
O10 C6 . 1.257(3) ?
O11 C8 . 1.250(3) ?
O12 C12 . 1.261(3) ?
C1 C3 . 1.385(3) ?
C1 C5 . 1.393(4) ?
C1 H1A . 0.9300 ?
C2 C9 . 1.396(3) ?
C2 C9 2_655 1.396(3) ?
C2 H2C . 0.9300 ?
C3 C1 2_756 1.385(3) ?
C3 C12 . 1.512(5) ?
C4 C5 . 1.392(3) ?
C4 C5 2_756 1.392(3) ?
C4 H4A . 0.9300 ?
C5 C8 . 1.509(3) ?
C6 C9 . 1.504(3) ?
C7 C10 . 1.390(3) ?
C7 C10 2_655 1.390(3) ?
C7 C11 . 1.476(5) ?
C9 C10 . 1.390(3) ?
C10 H10A . 0.9300 ?
C11 O1 2_655 1.275(3) ?
C12 O12 2_756 1.261(3) ?
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
O9 H9B O10 4_646 0.87 1.90 2.767(3) 171.5
O9 H9A O12 4_656 0.81 2.33 3.102(3) 160.0
O6 H6B O1 4_645 0.97 1.98 2.942(3) 173.1
O6 H6A O11 4_655 0.85 1.83 2.683(3) 173.1
O5 H5B O12 4_655 0.92 1.95 2.825(3) 157.6
O5 H5A O11 . 0.81 1.79 2.559(3) 156.4
O4 H4C O1 4_646 0.92 1.97 2.870(3) 166.7
O4 H4B O10 . 0.91 1.77 2.617(3) 154.0
O3 H3B O12 3_465 0.94 1.97 2.907(3) 171.3
O3 H3A O4 3_455 0.94 2.03 2.917(3) 155.8
O2 H2B O5 1_565 0.83 1.81 2.638(3) 173.0
O2 H2A O12 4_666 0.85 2.02 2.861(4) 171.3
