#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:40:45 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179857 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/53/7015327.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_7015327
loop_
_publ_author_name
'Ou, Yong-Cong'
'Wang, Jing'
'Leng, Ji-Dong'
'Lin, Zhuo-Jia'
'Tong, Ming-Liang'
_publ_section_title
;
 Two new 1,2,4,5-cyclohexanetetracarboxylate-bridged frameworks with
 metal hydroxide subunits. Synthesis, structures, magnetism and
 adsorption.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3592
_journal_page_last               3600
_journal_paper_doi               10.1039/c0dt01497d
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C35 H56 N4 Ni4 O32'
_chemical_formula_weight         1279.68
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 97.060(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.1211(12)
_cell_length_b                   17.5536(10)
_cell_length_c                   7.0480(5)
_cell_measurement_temperature    150(2)
_cell_volume                     2716.0(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            7147
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_T_max  0.8107
_exptl_absorpt_correction_T_min  0.6852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2938
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.259
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0531
_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)+(0.0857P)²+12.1037P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1637
_reflns_number_gt                2548
_reflns_number_total             2938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01497d.txt
_cod_data_source_block           compound2
_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 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7015327
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'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Ni2 Ni 0.24423(3) 0.0000 0.46905(10) 0.0168(2) Uani 1 2 d S . .
Ni1 Ni 0.11447(3) 0.0000 0.70499(11) 0.0205(2) Uani 1 2 d S . .
O1W O 0.0792(3) 0.0000 0.9667(8) 0.0485(14) Uani 1 2 d S A .
H1W H 0.0973 -0.0334 1.0403 0.058 Uiso 1 1 d RD . .
O1 O 0.14990(18) 0.0000 0.4517(6) 0.0194(8) Uani 1 2 d S A .
H1O H 0.1360 -0.0381 0.3857 0.023 Uiso 0.50 1 d PR . .
O2 O 0.16783(15) -0.0873(2) 0.8081(5) 0.0357(8) Uani 1 1 d . A .
O3 O 0.25393(15) -0.08285(18) 0.6725(5) 0.0330(8) Uani 1 1 d . A .
O4 O 0.24003(14) -0.08344(17) 1.2586(5) 0.0278(7) Uani 1 1 d . . .
O5 O 0.14284(15) -0.11886(18) 1.2431(5) 0.0325(8) Uani 1 1 d . . .
H5O H 0.1226 -0.1600 1.2282 0.039 Uiso 1 1 d R . .
C1 C 0.2487(2) -0.1720(2) 0.9207(6) 0.0220(8) Uani 1 1 d . . .
H1 H 0.2887 -0.1536 0.9861 0.026 Uiso 1 1 calc R . .
C2 C 0.20876(18) -0.1940(2) 1.0742(6) 0.0206(8) Uani 1 1 d . . .
H2 H 0.1689 -0.2132 1.0098 0.025 Uiso 1 1 calc R . .
C3 C 0.2393(2) -0.2577(2) 1.2010(6) 0.0237(8) Uani 1 1 d . . .
H3A H 0.2126 -0.2724 1.2979 0.028 Uiso 1 1 calc R . .
H3B H 0.2783 -0.2390 1.2689 0.028 Uiso 1 1 calc R . .
C4 C 0.22078(19) -0.1085(2) 0.7896(6) 0.0208(8) Uani 1 1 d . . .
C5 C 0.1966(2) -0.1265(2) 1.2011(6) 0.0230(8) Uani 1 1 d . . .
O6 O 0.04692(14) 0.07676(17) 0.5904(5) 0.0259(7) Uani 0.50 1 d P A 1
N1 N 0.04692(14) 0.07676(17) 0.5904(5) 0.0259(7) Uani 0.50 1 d PD . 2
C6 C 0.0000 0.0433(3) 0.5000 0.0216(11) Uani 1 2 d SD . 2
C7 C 0.0474(4) 0.1539(5) 0.5898(18) 0.047(3) Uani 0.50 1 d PD . 2
H7 H 0.0816 0.1801 0.6535 0.057 Uiso 0.50 1 calc PR . 2
C8 C 0.0000 0.1944(7) 0.5000 0.063(6) Uani 0.50 2 d SPD . 2
H8 H 0.0000 0.2485 0.5000 0.075 Uiso 0.50 2 calc SPR . 2
N2 N 0.3382(2) 0.0000 0.4756(8) 0.0262(11) Uani 1 2 d S . .
C9 C 0.3693(2) 0.0645(3) 0.4806(11) 0.0506(16) Uani 1 1 d . . .
H9 H 0.3475 0.1112 0.4767 0.061 Uiso 1 1 calc R . .
C10 C 0.4328(3) 0.0670(3) 0.4914(14) 0.061(2) Uani 1 1 d . . .
H10 H 0.4532 0.1148 0.4953 0.073 Uiso 1 1 calc R . .
C11 C 0.4663(3) 0.0000 0.4966(12) 0.0357(15) Uani 1 2 d S . .
O2W O 0.3422(5) 0.0000 1.0017(14) 0.101(3) Uani 1 2 d S . .
O3W O 0.4121(6) 0.1369(8) 1.015(2) 0.094(4) Uiso 0.50 1 d P . .
O4W O 0.0818(7) -0.2577(8) 1.296(2) 0.102(4) Uiso 0.50 1 d P . .
O4W' O 0.0441(15) -0.2138(19) 1.160(5) 0.115(10) Uiso 0.25 1 d P . .
O5W O 0.0882(12) -0.2433(13) 1.686(5) 0.176(9) Uiso 0.50 1 d P . .
O6W O 0.478(4) 0.0000 0.984(16) 0.35(4) Uiso 0.50 2 d SP . .
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
O3 Ni2 O3 91.2(2) 6 . ?
O3 Ni2 N2 88.04(14) 6 . ?
O3 Ni2 N2 88.04(14) . . ?
O3 Ni2 O1 93.42(12) 6 . ?
O3 Ni2 O1 93.42(12) . . ?
N2 Ni2 O1 177.91(19) . . ?
O3 Ni2 O4 176.38(12) 6 1_554 ?
O3 Ni2 O4 89.47(15) . 1_554 ?
N2 Ni2 O4 88.43(14) . 1_554 ?
O1 Ni2 O4 90.09(12) . 1_554 ?
O3 Ni2 O4 89.47(15) 6 6_554 ?
O3 Ni2 O4 176.38(12) . 6_554 ?
N2 Ni2 O4 88.43(14) . 6_554 ?
O1 Ni2 O4 90.09(12) . 6_554 ?
O4 Ni2 O4 89.62(19) 1_554 6_554 ?
O2 Ni1 O2 99.0(2) 6 . ?
O2 Ni1 O1 92.55(12) 6 . ?
O2 Ni1 O1 92.55(12) . . ?
O2 Ni1 O1W 86.97(15) 6 . ?
O2 Ni1 O1W 86.97(15) . . ?
O1 Ni1 O1W 179.3(2) . . ?
O2 Ni1 N1 170.10(14) 6 6 ?
O2 Ni1 N1 90.49(14) . 6 ?
O1 Ni1 N1 89.72(14) . 6 ?
O1W Ni1 N1 90.83(16) . 6 ?
O2 Ni1 O6 170.10(14) 6 6 ?
O2 Ni1 O6 90.49(14) . 6 ?
O1 Ni1 O6 89.72(14) . 6 ?
O1W Ni1 O6 90.83(16) . 6 ?
N1 Ni1 O6 0.00(18) 6 6 ?
O2 Ni1 O6 90.49(14) 6 . ?
O2 Ni1 O6 170.10(14) . . ?
O1 Ni1 O6 89.72(14) . . ?
O1W Ni1 O6 90.83(16) . . ?
N1 Ni1 O6 79.89(17) 6 . ?
O6 Ni1 O6 79.89(17) 6 . ?
Ni1 O1W H1W 109.9 . . ?
Ni1 O1 Ni2 116.18(19) . . ?
Ni1 O1 H1O 109.1 . . ?
Ni2 O1 H1O 109.1 . . ?
C4 O2 Ni1 134.7(3) . . ?
C4 O3 Ni2 134.5(3) . . ?
C5 O4 Ni2 128.5(3) . 1_556 ?
C5 O5 H5O 112.1 . . ?
C2 C1 C4 112.7(3) . . ?
C2 C1 C3 110.3(3) . 7_547 ?
C4 C1 C3 109.4(3) . 7_547 ?
C2 C1 H1 108.1 . . ?
C4 C1 H1 108.1 . . ?
C3 C1 H1 108.1 7_547 . ?
C1 C2 C5 112.2(3) . . ?
C1 C2 C3 110.2(3) . . ?
C5 C2 C3 108.7(3) . . ?
C1 C2 H2 108.6 . . ?
C5 C2 H2 108.6 . . ?
C3 C2 H2 108.6 . . ?
C2 C3 C1 110.6(3) . 7_547 ?
C2 C3 H3A 109.5 . . ?
C1 C3 H3A 109.5 7_547 . ?
C2 C3 H3B 109.5 . . ?
C1 C3 H3B 109.5 7_547 . ?
H3A C3 H3B 108.1 . . ?
O2 C4 O3 126.4(4) . . ?
O2 C4 C1 117.9(4) . . ?
O3 C4 C1 115.7(4) . . ?
O4 C5 O5 124.4(4) . . ?
O4 C5 C2 118.4(4) . . ?
O5 C5 C2 117.1(4) . . ?
N1 C6 C6 117.1(2) 2_556 5_556 ?
C8 C7 O5W 92.3(10) . 6_554 ?
C8 C7 H7 119.4 . . ?
O5W C7 H7 27.4 6_554 . ?
C7 C8 C7 116.8(10) 2_556 . ?
C7 C8 H8 121.6 2_556 . ?
C7 C8 H8 121.6 . . ?
C9 N2 C9 117.7(6) . 6 ?
C9 N2 Ni2 121.1(3) . . ?
C9 N2 Ni2 121.1(3) 6 . ?
N2 C9 C10 123.0(5) . . ?
N2 C9 H9 118.5 . . ?
C10 C9 H9 118.5 . . ?
C11 C10 C9 120.2(5) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C10 115.9(7) 6 . ?
C10 C11 C11 122.0(3) 6 5_656 ?
C10 C11 C11 122.0(3) . 5_656 ?
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
Ni2 O3 2.035(3) 6 ?
Ni2 O3 2.035(3) . ?
Ni2 N2 2.074(5) . ?
Ni2 O1 2.075(4) . ?
Ni2 O4 2.078(3) 1_554 ?
Ni2 O4 2.078(3) 6_554 ?
Ni1 O2 2.014(3) 6 ?
Ni1 O2 2.014(3) . ?
Ni1 O1 2.036(4) . ?
Ni1 O1W 2.089(6) . ?
Ni1 N1 2.099(3) 6 ?
Ni1 O6 2.099(3) 6 ?
Ni1 O6 2.099(3) . ?
O1W H1W 0.8500 . ?
O1 H1O 0.8501 . ?
O2 C4 1.251(5) . ?
O3 C4 1.253(5) . ?
O4 C5 1.250(5) . ?
O4 Ni2 2.078(3) 1_556 ?
O5 C5 1.268(5) . ?
O5 H5O 0.8500 . ?
C1 C2 1.527(5) . ?
C1 C4 1.529(5) . ?
C1 C3 1.543(5) 7_547 ?
C1 H1 1.0000 . ?
C2 C5 1.527(5) . ?
C2 C3 1.536(5) . ?
C2 H2 1.0000 . ?
C3 C1 1.543(5) 7_547 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C6 N1 1.291(4) 2_556 ?
C6 C6 1.519(10) 5_556 ?
C7 C8 1.358(10) . ?
C7 O5W 1.89(3) 6_554 ?
C7 H7 0.9500 . ?
C8 C7 1.358(10) 2_556 ?
C8 H8 0.9500 . ?
N2 C9 1.323(6) . ?
N2 C9 1.323(6) 6 ?
C9 C10 1.399(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(7) . ?
C10 H10 0.9500 . ?
C11 C10 1.388(7) 6 ?
C11 C11 1.486(14) 5_656 ?
O4W O4W' 1.42(4) . ?
O5W C7 1.89(3) 6_556 ?
O6W O6W 0.99(15) 5_657 ?
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 H1W O5 0.85 2.23 3.074(6) 177.6 .
O1 H1O O5 0.85 1.76 2.546(4) 153.8 1_554
O5 H5O O4W' 0.85 1.98 2.75(3) 150.1 .
O5 H5O O4W 0.85 2.02 2.832(15) 159.3 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ni1 O1 Ni2 49.58(11) 6 . . . ?
O2 Ni1 O1 Ni2 -49.58(11) . . . . ?
O1W Ni1 O1 Ni2 0.000(19) . . . . ?
N1 Ni1 O1 Ni2 -140.06(8) 6 . . . ?
O6 Ni1 O1 Ni2 -140.06(8) 6 . . . ?
O6 Ni1 O1 Ni2 140.06(8) . . . . ?
O3 Ni2 O1 Ni1 -45.71(11) 6 . . . ?
O3 Ni2 O1 Ni1 45.71(11) . . . . ?
N2 Ni2 O1 Ni1 180.000(6) . . . . ?
O4 Ni2 O1 Ni1 135.19(9) 1_554 . . . ?
O4 Ni2 O1 Ni1 -135.19(9) 6_554 . . . ?
O2 Ni1 O2 C4 -59.0(5) 6 . . . ?
O1 Ni1 O2 C4 34.0(5) . . . . ?
O1W Ni1 O2 C4 -145.5(5) . . . . ?
N1 Ni1 O2 C4 123.7(5) 6 . . . ?
O6 Ni1 O2 C4 123.7(5) 6 . . . ?
O6 Ni1 O2 C4 137.1(8) . . . . ?
O3 Ni2 O3 C4 73.5(5) 6 . . . ?
N2 Ni2 O3 C4 161.4(5) . . . . ?
O1 Ni2 O3 C4 -20.0(5) . . . . ?
O4 Ni2 O3 C4 -110.1(5) 1_554 . . . ?
O4 Ni2 O3 C4 174(2) 6_554 . . . ?
C4 C1 C2 C5 -58.6(5) . . . . ?
C3 C1 C2 C5 178.8(3) 7_547 . . . ?
C4 C1 C2 C3 -179.9(3) . . . . ?
C3 C1 C2 C3 57.6(5) 7_547 . . . ?
C1 C2 C3 C1 -57.8(5) . . . 7_547 ?
C5 C2 C3 C1 178.9(3) . . . 7_547 ?
Ni1 O2 C4 O3 -10.2(8) . . . . ?
Ni1 O2 C4 C1 170.1(3) . . . . ?
Ni2 O3 C4 O2 1.3(7) . . . . ?
Ni2 O3 C4 C1 -179.0(3) . . . . ?
C2 C1 C4 O2 -6.9(5) . . . . ?
C3 C1 C4 O2 116.2(4) 7_547 . . . ?
C2 C1 C4 O3 173.4(4) . . . . ?
C3 C1 C4 O3 -63.6(5) 7_547 . . . ?
Ni2 O4 C5 O5 11.3(7) 1_556 . . . ?
Ni2 O4 C5 C2 -167.7(3) 1_556 . . . ?
C1 C2 C5 O4 -43.5(5) . . . . ?
C3 C2 C5 O4 78.5(5) . . . . ?
C1 C2 C5 O5 137.4(4) . . . . ?
C3 C2 C5 O5 -100.5(4) . . . . ?
O5W C7 C8 C7 -176.3(12) 6_554 . . 2_556 ?
O3 Ni2 N2 C9 -43.3(6) 6 . . . ?
O3 Ni2 N2 C9 -134.6(6) . . . . ?
O1 Ni2 N2 C9 91.0(6) . . . . ?
O4 Ni2 N2 C9 135.9(6) 1_554 . . . ?
O4 Ni2 N2 C9 46.2(6) 6_554 . . . ?
O3 Ni2 N2 C9 134.6(6) 6 . . 6 ?
O3 Ni2 N2 C9 43.3(6) . . . 6 ?
O1 Ni2 N2 C9 -91.0(6) . . . 6 ?
O4 Ni2 N2 C9 -46.2(6) 1_554 . . 6 ?
O4 Ni2 N2 C9 -135.9(6) 6_554 . . 6 ?
C9 N2 C9 C10 -0.2(13) 6 . . . ?
Ni2 N2 C9 C10 177.8(6) . . . . ?
N2 C9 C10 C11 0.3(13) . . . . ?
C9 C10 C11 C10 -0.3(15) . . . 6 ?
C9 C10 C11 C11 178.5(10) . . . 5_656 ?
